 
data_#20010054
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Ca Fe0.50 O7 Pb Sb1.50' 
_chemical_formula_weight          569.82

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb'  'Sb'  -0.5866   1.5461
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.2262   0.3064
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            227
_space_group_name_H-M_alt         'F d -3 m'
_space_group_name_Hall            '-F 4vw 2vw 3'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+3/4, -y+1/4, z+1/2'
 '-x+1/4, y+1/2, -z+3/4'
 'x+1/2, -y+3/4, -z+1/4'
 'z, x, y'
 'z+1/2, -x+3/4, -y+1/4'
 '-z+3/4, -x+1/4, y+1/2'
 '-z+1/4, x+1/2, -y+3/4'
 'y, z, x'
 '-y+1/4, z+1/2, -x+3/4'
 'y+1/2, -z+3/4, -x+1/4'
 '-y+3/4, -z+1/4, x+1/2'
 'y+3/4, x+1/4, -z+1/2'
 '-y, -x, -z'
 'y+1/4, -x+1/2, z+3/4'
 '-y+1/2, x+3/4, z+1/4'
 'x+3/4, z+1/4, -y+1/2'
 '-x+1/2, z+3/4, y+1/4'
 '-x, -z, -y'
 'x+1/4, -z+1/2, y+3/4'
 'z+3/4, y+1/4, -x+1/2'
 'z+1/4, -y+1/2, x+3/4'
 '-z+1/2, y+3/4, x+1/4'
 '-z, -y, -x'
 'x, y+1/2, z+1/2'
 '-x+3/4, -y+3/4, z+1'
 '-x+1/4, y+1, -z+5/4'
 'x+1/2, -y+5/4, -z+3/4'
 'z, x+1/2, y+1/2'
 'z+1/2, -x+5/4, -y+3/4'
 '-z+3/4, -x+3/4, y+1'
 '-z+1/4, x+1, -y+5/4'
 'y, z+1/2, x+1/2'
 '-y+1/4, z+1, -x+5/4'
 'y+1/2, -z+5/4, -x+3/4'
 '-y+3/4, -z+3/4, x+1'
 'y+3/4, x+3/4, -z+1'
 '-y, -x+1/2, -z+1/2'
 'y+1/4, -x+1, z+5/4'
 '-y+1/2, x+5/4, z+3/4'
 'x+3/4, z+3/4, -y+1'
 '-x+1/2, z+5/4, y+3/4'
 '-x, -z+1/2, -y+1/2'
 'x+1/4, -z+1, y+5/4'
 'z+3/4, y+3/4, -x+1'
 'z+1/4, -y+1, x+5/4'
 '-z+1/2, y+5/4, x+3/4'
 '-z, -y+1/2, -x+1/2'
 'x+1/2, y, z+1/2'
 '-x+5/4, -y+1/4, z+1'
 '-x+3/4, y+1/2, -z+5/4'
 'x+1, -y+3/4, -z+3/4'
 'z+1/2, x, y+1/2'
 'z+1, -x+3/4, -y+3/4'
 '-z+5/4, -x+1/4, y+1'
 '-z+3/4, x+1/2, -y+5/4'
 'y+1/2, z, x+1/2'
 '-y+3/4, z+1/2, -x+5/4'
 'y+1, -z+3/4, -x+3/4'
 '-y+5/4, -z+1/4, x+1'
 'y+5/4, x+1/4, -z+1'
 '-y+1/2, -x, -z+1/2'
 'y+3/4, -x+1/2, z+5/4'
 '-y+1, x+3/4, z+3/4'
 'x+5/4, z+1/4, -y+1'
 '-x+1, z+3/4, y+3/4'
 '-x+1/2, -z, -y+1/2'
 'x+3/4, -z+1/2, y+5/4'
 'z+5/4, y+1/4, -x+1'
 'z+3/4, -y+1/2, x+5/4'
 '-z+1, y+3/4, x+3/4'
 '-z+1/2, -y, -x+1/2'
 'x+1/2, y+1/2, z'
 '-x+5/4, -y+3/4, z+1/2'
 '-x+3/4, y+1, -z+3/4'
 'x+1, -y+5/4, -z+1/4'
 'z+1/2, x+1/2, y'
 'z+1, -x+5/4, -y+1/4'
 '-z+5/4, -x+3/4, y+1/2'
 '-z+3/4, x+1, -y+3/4'
 'y+1/2, z+1/2, x'
 '-y+3/4, z+1, -x+3/4'
 'y+1, -z+5/4, -x+1/4'
 '-y+5/4, -z+3/4, x+1/2'
 'y+5/4, x+3/4, -z+1/2'
 '-y+1/2, -x+1/2, -z'
 'y+3/4, -x+1, z+3/4'
 '-y+1, x+5/4, z+1/4'
 'x+5/4, z+3/4, -y+1/2'
 '-x+1, z+5/4, y+1/4'
 '-x+1/2, -z+1/2, -y'
 'x+3/4, -z+1, y+3/4'
 'z+5/4, y+3/4, -x+1/2'
 'z+3/4, -y+1, x+3/4'
 '-z+1, y+5/4, x+1/4'
 '-z+1/2, -y+1/2, -x'
 '-x, -y, -z'
 'x-3/4, y-1/4, -z-1/2'
 'x-1/4, -y-1/2, z-3/4'
 '-x-1/2, y-3/4, z-1/4'
 '-z, -x, -y'
 '-z-1/2, x-3/4, y-1/4'
 'z-3/4, x-1/4, -y-1/2'
 'z-1/4, -x-1/2, y-3/4'
 '-y, -z, -x'
 'y-1/4, -z-1/2, x-3/4'
 '-y-1/2, z-3/4, x-1/4'
 'y-3/4, z-1/4, -x-1/2'
 '-y-3/4, -x-1/4, z-1/2'
 'y, x, z'
 '-y-1/4, x-1/2, -z-3/4'
 'y-1/2, -x-3/4, -z-1/4'
 '-x-3/4, -z-1/4, y-1/2'
 'x-1/2, -z-3/4, -y-1/4'
 'x, z, y'
 '-x-1/4, z-1/2, -y-3/4'
 '-z-3/4, -y-1/4, x-1/2'
 '-z-1/4, y-1/2, -x-3/4'
 'z-1/2, -y-3/4, -x-1/4'
 'z, y, x'
 '-x, -y+1/2, -z+1/2'
 'x-3/4, y+1/4, -z'
 'x-1/4, -y, z-1/4'
 '-x-1/2, y-1/4, z+1/4'
 '-z, -x+1/2, -y+1/2'
 '-z-1/2, x-1/4, y+1/4'
 'z-3/4, x+1/4, -y'
 'z-1/4, -x, y-1/4'
 '-y, -z+1/2, -x+1/2'
 'y-1/4, -z, x-1/4'
 '-y-1/2, z-1/4, x+1/4'
 'y-3/4, z+1/4, -x'
 '-y-3/4, -x+1/4, z'
 'y, x+1/2, z+1/2'
 '-y-1/4, x, -z-1/4'
 'y-1/2, -x-1/4, -z+1/4'
 '-x-3/4, -z+1/4, y'
 'x-1/2, -z-1/4, -y+1/4'
 'x, z+1/2, y+1/2'
 '-x-1/4, z, -y-1/4'
 '-z-3/4, -y+1/4, x'
 '-z-1/4, y, -x-1/4'
 'z-1/2, -y-1/4, -x+1/4'
 'z, y+1/2, x+1/2'
 '-x+1/2, -y, -z+1/2'
 'x-1/4, y-1/4, -z'
 'x+1/4, -y-1/2, z-1/4'
 '-x, y-3/4, z+1/4'
 '-z+1/2, -x, -y+1/2'
 '-z, x-3/4, y+1/4'
 'z-1/4, x-1/4, -y'
 'z+1/4, -x-1/2, y-1/4'
 '-y+1/2, -z, -x+1/2'
 'y+1/4, -z-1/2, x-1/4'
 '-y, z-3/4, x+1/4'
 'y-1/4, z-1/4, -x'
 '-y-1/4, -x-1/4, z'
 'y+1/2, x, z+1/2'
 '-y+1/4, x-1/2, -z-1/4'
 'y, -x-3/4, -z+1/4'
 '-x-1/4, -z-1/4, y'
 'x, -z-3/4, -y+1/4'
 'x+1/2, z, y+1/2'
 '-x+1/4, z-1/2, -y-1/4'
 '-z-1/4, -y-1/4, x'
 '-z+1/4, y-1/2, -x-1/4'
 'z, -y-3/4, -x+1/4'
 'z+1/2, y, x+1/2'
 '-x+1/2, -y+1/2, -z'
 'x-1/4, y+1/4, -z-1/2'
 'x+1/4, -y, z-3/4'
 '-x, y-1/4, z-1/4'
 '-z+1/2, -x+1/2, -y'
 '-z, x-1/4, y-1/4'
 'z-1/4, x+1/4, -y-1/2'
 'z+1/4, -x, y-3/4'
 '-y+1/2, -z+1/2, -x'
 'y+1/4, -z, x-3/4'
 '-y, z-1/4, x-1/4'
 'y-1/4, z+1/4, -x-1/2'
 '-y-1/4, -x+1/4, z-1/2'
 'y+1/2, x+1/2, z'
 '-y+1/4, x, -z-3/4'
 'y, -x-1/4, -z-1/4'
 '-x-1/4, -z+1/4, y-1/2'
 'x, -z-1/4, -y-1/4'
 'x+1/2, z+1/2, y'
 '-x+1/4, z, -y-3/4'
 '-z-1/4, -y+1/4, x-1/2'
 '-z+1/4, y, -x-3/4'
 'z, -y-1/4, -x-1/4'
 'z+1/2, y+1/2, x'
 
_cell_length_a                    10.4201(10)
_cell_length_b                    10.4201(10)
_cell_length_c                    10.4201(10)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1131.4(3)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     6.691          
_exptl_crystal_F_000              1980
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.170
_exptl_crystal_size_mid           0.160
_exptl_crystal_size_min           0.150
_exptl_absorpt_coefficient_mu     38.955
_shelx_estimated_absorpt_T_min    0.058
_shelx_estimated_absorpt_T_max    0.068
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             2115
_diffrn_reflns_av_unetI/netI      0.0151
_diffrn_reflns_av_R_equivalents   0.0319
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          3.386
_diffrn_reflns_theta_max          36.206
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.994
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              163
_reflns_number_gt                 134
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+88.8990P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00023(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          163
_refine_ls_number_parameters      13
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0311
_refine_ls_R_factor_gt            0.0259
_refine_ls_wR_factor_ref          0.0590
_refine_ls_wR_factor_gt           0.0576
_refine_ls_goodness_of_fit_ref    1.354
_refine_ls_restrained_S_all       1.354
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pb Pb 0.5000 0.5000 0.5000 0.0207(4) Uani 0.703(9) 12 d S T P . .
Ca Ca 0.5000 0.5000 0.5000 0.0207(4) Uani 0.297(9) 12 d S T P . .
Sb Sb 0.0000 0.0000 0.0000 0.0081(4) Uani 0.8077 12 d S T P . .
Fe Fe 0.0000 0.0000 0.0000 0.0081(4) Uani 0.1922 12 d S T P . .
O1 O 0.3217(7) 0.1250 0.1250 0.0114(12) Uani 1 4 d S T P . .
O2 O 0.3750 0.3750 0.3750 0.014(8) Uani 0.61(8) 24 d S T . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pb O2 2.2560(2) 97_666 ?
Pb O2 2.2560(2) . ?
Pb O1 2.616(5) 177_556 ?
Pb O1 2.616(5) 81 ?
Pb O1 2.616(5) 149_565 ?
Pb O1 2.616(5) 53 ?
Pb O1 2.616(5) 121_655 ?
Pb O1 2.616(5) 25 ?
Pb Pb 3.6841(4) 26_554 ?
Pb Ca 3.6841(4) 50_564 ?
Pb Ca 3.6841(4) 27_645 ?
Pb Ca 3.6841(4) 75_545 ?
Sb O1 1.988(3) 130 ?
Sb O1 1.988(3) 34_544 ?
Sb O1 1.988(3) 174 ?
Sb O1 1.988(3) 78_445 ?
Sb O1 1.988(3) 146 ?
Sb O1 1.988(3) 50_454 ?
Sb Ca 3.6841(4) 2_554 ?
Sb Ca 3.6841(4) 28_445 ?
Sb Ca 3.6841(4) 4_455 ?
Sb Ca 3.6841(4) 51_544 ?
Sb Ca 3.6841(4) 3_545 ?
Sb Ca 3.6841(4) 74_454 ?
O1 Fe 1.988(3) 27_544 ?
O1 Fe 1.988(3) 50_454 ?
O1 Sb 1.988(3) 27_544 ?
O1 Sb 1.988(3) 50_454 ?
O1 Pb 2.616(5) 52_455 ?
O1 Ca 2.616(5) 52_455 ?
O1 Pb 2.616(5) 25_544 ?
O1 Ca 2.616(5) 25_544 ?
O2 Ca 2.2560(2) 52_455 ?
O2 Pb 2.2560(2) 26_554 ?
O2 Pb 2.2560(2) 75_545 ?
O2 Pb 2.2560(2) 52_455 ?
O2 Ca 2.2560(2) 26_554 ?
O2 Ca 2.2560(2) 75_545 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O2 Pb O2 180.0 97_666 . ?
O2 Pb O1 99.49(12) 97_666 177_556 ?
O2 Pb O1 80.51(12) . 177_556 ?
O2 Pb O1 80.51(12) 97_666 81 ?
O2 Pb O1 99.49(12) . 81 ?
O1 Pb O1 180.0 177_556 81 ?
O2 Pb O1 99.49(12) 97_666 149_565 ?
O2 Pb O1 80.51(12) . 149_565 ?
O1 Pb O1 117.34(7) 177_556 149_565 ?
O1 Pb O1 62.66(6) 81 149_565 ?
O2 Pb O1 80.51(12) 97_666 53 ?
O2 Pb O1 99.49(12) . 53 ?
O1 Pb O1 62.66(6) 177_556 53 ?
O1 Pb O1 117.34(7) 81 53 ?
O1 Pb O1 180.0 149_565 53 ?
O2 Pb O1 99.49(12) 97_666 121_655 ?
O2 Pb O1 80.51(12) . 121_655 ?
O1 Pb O1 117.34(6) 177_556 121_655 ?
O1 Pb O1 62.66(6) 81 121_655 ?
O1 Pb O1 117.34(6) 149_565 121_655 ?
O1 Pb O1 62.66(6) 53 121_655 ?
O2 Pb O1 80.51(12) 97_666 25 ?
O2 Pb O1 99.49(12) . 25 ?
O1 Pb O1 62.66(6) 177_556 25 ?
O1 Pb O1 117.34(6) 81 25 ?
O1 Pb O1 62.66(6) 149_565 25 ?
O1 Pb O1 117.34(6) 53 25 ?
O1 Pb O1 180.0 121_655 25 ?
O2 Pb Pb 144.7 97_666 26_554 ?
O2 Pb Pb 35.3 . 26_554 ?
O1 Pb Pb 45.24(12) 177_556 26_554 ?
O1 Pb Pb 134.76(12) 81 26_554 ?
O1 Pb Pb 98.63(10) 149_565 26_554 ?
O1 Pb Pb 81.37(10) 53 26_554 ?
O1 Pb Pb 98.63(10) 121_655 26_554 ?
O1 Pb Pb 81.37(10) 25 26_554 ?
O2 Pb Ca 35.3 97_666 50_564 ?
O2 Pb Ca 144.7 . 50_564 ?
O1 Pb Ca 134.76(12) 177_556 50_564 ?
O1 Pb Ca 45.24(12) 81 50_564 ?
O1 Pb Ca 81.37(10) 149_565 50_564 ?
O1 Pb Ca 98.63(10) 53 50_564 ?
O1 Pb Ca 81.37(10) 121_655 50_564 ?
O1 Pb Ca 98.63(10) 25 50_564 ?
Pb Pb Ca 180.0 26_554 50_564 ?
O2 Pb Ca 35.3 97_666 27_645 ?
O2 Pb Ca 144.7 . 27_645 ?
O1 Pb Ca 81.37(10) 177_556 27_645 ?
O1 Pb Ca 98.63(10) 81 27_645 ?
O1 Pb Ca 134.76(12) 149_565 27_645 ?
O1 Pb Ca 45.24(12) 53 27_645 ?
O1 Pb Ca 81.37(10) 121_655 27_645 ?
O1 Pb Ca 98.63(10) 25 27_645 ?
Pb Pb Ca 120.0 26_554 27_645 ?
Ca Pb Ca 60.0 50_564 27_645 ?
O2 Pb Ca 144.7 97_666 75_545 ?
O2 Pb Ca 35.3 . 75_545 ?
O1 Pb Ca 98.63(10) 177_556 75_545 ?
O1 Pb Ca 81.37(10) 81 75_545 ?
O1 Pb Ca 45.24(12) 149_565 75_545 ?
O1 Pb Ca 134.76(12) 53 75_545 ?
O1 Pb Ca 98.63(10) 121_655 75_545 ?
O1 Pb Ca 81.37(10) 25 75_545 ?
Pb Pb Ca 60.0 26_554 75_545 ?
Ca Pb Ca 120.0 50_564 75_545 ?
Ca Pb Ca 180.0 27_645 75_545 ?
O1 Sb O1 180.0(4) 130 34_544 ?
O1 Sb O1 93.6(3) 130 174 ?
O1 Sb O1 86.4(3) 34_544 174 ?
O1 Sb O1 86.4(3) 130 78_445 ?
O1 Sb O1 93.6(3) 34_544 78_445 ?
O1 Sb O1 180.0(4) 174 78_445 ?
O1 Sb O1 93.6(3) 130 146 ?
O1 Sb O1 86.4(3) 34_544 146 ?
O1 Sb O1 93.6(3) 174 146 ?
O1 Sb O1 86.4(3) 78_445 146 ?
O1 Sb O1 86.4(3) 130 50_454 ?
O1 Sb O1 93.6(3) 34_544 50_454 ?
O1 Sb O1 86.4(3) 174 50_454 ?
O1 Sb O1 93.6(3) 78_445 50_454 ?
O1 Sb O1 180.0(4) 146 50_454 ?
O1 Sb Ca 90.0 130 2_554 ?
O1 Sb Ca 90.0 34_544 2_554 ?
O1 Sb Ca 136.82(14) 174 2_554 ?
O1 Sb Ca 43.18(14) 78_445 2_554 ?
O1 Sb Ca 43.18(14) 146 2_554 ?
O1 Sb Ca 136.82(14) 50_454 2_554 ?
O1 Sb Ca 43.18(14) 130 28_445 ?
O1 Sb Ca 136.82(14) 34_544 28_445 ?
O1 Sb Ca 136.82(14) 174 28_445 ?
O1 Sb Ca 43.18(14) 78_445 28_445 ?
O1 Sb Ca 90.0 146 28_445 ?
O1 Sb Ca 90.0 50_454 28_445 ?
Ca Sb Ca 60.0 2_554 28_445 ?
O1 Sb Ca 136.82(14) 130 4_455 ?
O1 Sb Ca 43.18(14) 34_544 4_455 ?
O1 Sb Ca 43.18(14) 174 4_455 ?
O1 Sb Ca 136.82(14) 78_445 4_455 ?
O1 Sb Ca 90.0 146 4_455 ?
O1 Sb Ca 90.0 50_454 4_455 ?
Ca Sb Ca 120.0 2_554 4_455 ?
Ca Sb Ca 180.0 28_445 4_455 ?
O1 Sb Ca 136.82(14) 130 51_544 ?
O1 Sb Ca 43.18(14) 34_544 51_544 ?
O1 Sb Ca 90.0 174 51_544 ?
O1 Sb Ca 90.0 78_445 51_544 ?
O1 Sb Ca 43.18(14) 146 51_544 ?
O1 Sb Ca 136.82(14) 50_454 51_544 ?
Ca Sb Ca 60.0 2_554 51_544 ?
Ca Sb Ca 120.0 28_445 51_544 ?
Ca Sb Ca 60.0 4_455 51_544 ?
O1 Sb Ca 43.18(14) 130 3_545 ?
O1 Sb Ca 136.82(14) 34_544 3_545 ?
O1 Sb Ca 90.0 174 3_545 ?
O1 Sb Ca 90.0 78_445 3_545 ?
O1 Sb Ca 136.82(14) 146 3_545 ?
O1 Sb Ca 43.18(14) 50_454 3_545 ?
Ca Sb Ca 120.0 2_554 3_545 ?
Ca Sb Ca 60.0 28_445 3_545 ?
Ca Sb Ca 120.0 4_455 3_545 ?
Ca Sb Ca 180.0 51_544 3_545 ?
O1 Sb Ca 90.0 130 74_454 ?
O1 Sb Ca 90.0 34_544 74_454 ?
O1 Sb Ca 43.18(14) 174 74_454 ?
O1 Sb Ca 136.82(14) 78_445 74_454 ?
O1 Sb Ca 136.82(14) 146 74_454 ?
O1 Sb Ca 43.18(14) 50_454 74_454 ?
Ca Sb Ca 180.0 2_554 74_454 ?
Ca Sb Ca 120.0 28_445 74_454 ?
Ca Sb Ca 60.0 4_455 74_454 ?
Ca Sb Ca 120.0 51_544 74_454 ?
Ca Sb Ca 60.0 3_545 74_454 ?
Fe O1 Fe 135.8(4) 27_544 50_454 ?
Fe O1 Sb 0.0 27_544 27_544 ?
Fe O1 Sb 135.8(4) 50_454 27_544 ?
Fe O1 Sb 135.8(4) 27_544 50_454 ?
Fe O1 Sb 0.0 50_454 50_454 ?
Sb O1 Sb 135.8(4) 27_544 50_454 ?
Fe O1 Pb 105.48(11) 27_544 52_455 ?
Fe O1 Pb 105.48(11) 50_454 52_455 ?
Sb O1 Pb 105.48(11) 27_544 52_455 ?
Sb O1 Pb 105.48(11) 50_454 52_455 ?
Fe O1 Ca 105.48(11) 27_544 52_455 ?
Fe O1 Ca 105.48(11) 50_454 52_455 ?
Sb O1 Ca 105.48(11) 27_544 52_455 ?
Sb O1 Ca 105.48(11) 50_454 52_455 ?
Pb O1 Ca 0.0 52_455 52_455 ?
Fe O1 Pb 105.48(11) 27_544 25_544 ?
Fe O1 Pb 105.48(11) 50_454 25_544 ?
Sb O1 Pb 105.48(11) 27_544 25_544 ?
Sb O1 Pb 105.48(11) 50_454 25_544 ?
Pb O1 Pb 89.5(2) 52_455 25_544 ?
Ca O1 Pb 89.5(2) 52_455 25_544 ?
Fe O1 Ca 105.48(11) 27_544 25_544 ?
Fe O1 Ca 105.48(11) 50_454 25_544 ?
Sb O1 Ca 105.48(11) 27_544 25_544 ?
Sb O1 Ca 105.48(11) 50_454 25_544 ?
Pb O1 Ca 89.5(2) 52_455 25_544 ?
Ca O1 Ca 89.5(2) 52_455 25_544 ?
Pb O1 Ca 0.0 25_544 25_544 ?
Pb O2 Ca 109.471(1) . 52_455 ?
Pb O2 Pb 109.471(1) . 26_554 ?
Ca O2 Pb 109.5 52_455 26_554 ?
Pb O2 Pb 109.471(1) . 75_545 ?
Ca O2 Pb 109.5 52_455 75_545 ?
Pb O2 Pb 109.5 26_554 75_545 ?
Pb O2 Pb 109.471(1) . 52_455 ?
Ca O2 Pb 0.0 52_455 52_455 ?
Pb O2 Pb 109.5 26_554 52_455 ?
Pb O2 Pb 109.5 75_545 52_455 ?
Pb O2 Ca 109.471(1) . 26_554 ?
Ca O2 Ca 109.5 52_455 26_554 ?
Pb O2 Ca 0.0 26_554 26_554 ?
Pb O2 Ca 109.5 75_545 26_554 ?
Pb O2 Ca 109.5 52_455 26_554 ?
Pb O2 Ca 109.471(1) . 75_545 ?
Ca O2 Ca 109.5 52_455 75_545 ?
Pb O2 Ca 109.5 26_554 75_545 ?
Pb O2 Ca 0.0 75_545 75_545 ?
Pb O2 Ca 109.5 52_455 75_545 ?
Ca O2 Ca 109.5 26_554 75_545 ?
 
_refine_diff_density_max    1.105
_refine_diff_density_min   -0.937
_refine_diff_density_rms    0.243


 
data_#19332400
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Ca Fe0.12 O7 Pb Sb1.88' 
_chemical_formula_weight          594.53

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0080   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb'  'Sb'  -0.5866   1.5461
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.2262   0.3064
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            227
_space_group_name_H-M_alt         'F d -3 m'
_space_group_name_Hall            '-F 4vw 2vw 3'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+3/4, -y+1/4, z+1/2'
 '-x+1/4, y+1/2, -z+3/4'
 'x+1/2, -y+3/4, -z+1/4'
 'z, x, y'
 'z+1/2, -x+3/4, -y+1/4'
 '-z+3/4, -x+1/4, y+1/2'
 '-z+1/4, x+1/2, -y+3/4'
 'y, z, x'
 '-y+1/4, z+1/2, -x+3/4'
 'y+1/2, -z+3/4, -x+1/4'
 '-y+3/4, -z+1/4, x+1/2'
 'y+3/4, x+1/4, -z+1/2'
 '-y, -x, -z'
 'y+1/4, -x+1/2, z+3/4'
 '-y+1/2, x+3/4, z+1/4'
 'x+3/4, z+1/4, -y+1/2'
 '-x+1/2, z+3/4, y+1/4'
 '-x, -z, -y'
 'x+1/4, -z+1/2, y+3/4'
 'z+3/4, y+1/4, -x+1/2'
 'z+1/4, -y+1/2, x+3/4'
 '-z+1/2, y+3/4, x+1/4'
 '-z, -y, -x'
 'x, y+1/2, z+1/2'
 '-x+3/4, -y+3/4, z+1'
 '-x+1/4, y+1, -z+5/4'
 'x+1/2, -y+5/4, -z+3/4'
 'z, x+1/2, y+1/2'
 'z+1/2, -x+5/4, -y+3/4'
 '-z+3/4, -x+3/4, y+1'
 '-z+1/4, x+1, -y+5/4'
 'y, z+1/2, x+1/2'
 '-y+1/4, z+1, -x+5/4'
 'y+1/2, -z+5/4, -x+3/4'
 '-y+3/4, -z+3/4, x+1'
 'y+3/4, x+3/4, -z+1'
 '-y, -x+1/2, -z+1/2'
 'y+1/4, -x+1, z+5/4'
 '-y+1/2, x+5/4, z+3/4'
 'x+3/4, z+3/4, -y+1'
 '-x+1/2, z+5/4, y+3/4'
 '-x, -z+1/2, -y+1/2'
 'x+1/4, -z+1, y+5/4'
 'z+3/4, y+3/4, -x+1'
 'z+1/4, -y+1, x+5/4'
 '-z+1/2, y+5/4, x+3/4'
 '-z, -y+1/2, -x+1/2'
 'x+1/2, y, z+1/2'
 '-x+5/4, -y+1/4, z+1'
 '-x+3/4, y+1/2, -z+5/4'
 'x+1, -y+3/4, -z+3/4'
 'z+1/2, x, y+1/2'
 'z+1, -x+3/4, -y+3/4'
 '-z+5/4, -x+1/4, y+1'
 '-z+3/4, x+1/2, -y+5/4'
 'y+1/2, z, x+1/2'
 '-y+3/4, z+1/2, -x+5/4'
 'y+1, -z+3/4, -x+3/4'
 '-y+5/4, -z+1/4, x+1'
 'y+5/4, x+1/4, -z+1'
 '-y+1/2, -x, -z+1/2'
 'y+3/4, -x+1/2, z+5/4'
 '-y+1, x+3/4, z+3/4'
 'x+5/4, z+1/4, -y+1'
 '-x+1, z+3/4, y+3/4'
 '-x+1/2, -z, -y+1/2'
 'x+3/4, -z+1/2, y+5/4'
 'z+5/4, y+1/4, -x+1'
 'z+3/4, -y+1/2, x+5/4'
 '-z+1, y+3/4, x+3/4'
 '-z+1/2, -y, -x+1/2'
 'x+1/2, y+1/2, z'
 '-x+5/4, -y+3/4, z+1/2'
 '-x+3/4, y+1, -z+3/4'
 'x+1, -y+5/4, -z+1/4'
 'z+1/2, x+1/2, y'
 'z+1, -x+5/4, -y+1/4'
 '-z+5/4, -x+3/4, y+1/2'
 '-z+3/4, x+1, -y+3/4'
 'y+1/2, z+1/2, x'
 '-y+3/4, z+1, -x+3/4'
 'y+1, -z+5/4, -x+1/4'
 '-y+5/4, -z+3/4, x+1/2'
 'y+5/4, x+3/4, -z+1/2'
 '-y+1/2, -x+1/2, -z'
 'y+3/4, -x+1, z+3/4'
 '-y+1, x+5/4, z+1/4'
 'x+5/4, z+3/4, -y+1/2'
 '-x+1, z+5/4, y+1/4'
 '-x+1/2, -z+1/2, -y'
 'x+3/4, -z+1, y+3/4'
 'z+5/4, y+3/4, -x+1/2'
 'z+3/4, -y+1, x+3/4'
 '-z+1, y+5/4, x+1/4'
 '-z+1/2, -y+1/2, -x'
 '-x, -y, -z'
 'x-3/4, y-1/4, -z-1/2'
 'x-1/4, -y-1/2, z-3/4'
 '-x-1/2, y-3/4, z-1/4'
 '-z, -x, -y'
 '-z-1/2, x-3/4, y-1/4'
 'z-3/4, x-1/4, -y-1/2'
 'z-1/4, -x-1/2, y-3/4'
 '-y, -z, -x'
 'y-1/4, -z-1/2, x-3/4'
 '-y-1/2, z-3/4, x-1/4'
 'y-3/4, z-1/4, -x-1/2'
 '-y-3/4, -x-1/4, z-1/2'
 'y, x, z'
 '-y-1/4, x-1/2, -z-3/4'
 'y-1/2, -x-3/4, -z-1/4'
 '-x-3/4, -z-1/4, y-1/2'
 'x-1/2, -z-3/4, -y-1/4'
 'x, z, y'
 '-x-1/4, z-1/2, -y-3/4'
 '-z-3/4, -y-1/4, x-1/2'
 '-z-1/4, y-1/2, -x-3/4'
 'z-1/2, -y-3/4, -x-1/4'
 'z, y, x'
 '-x, -y+1/2, -z+1/2'
 'x-3/4, y+1/4, -z'
 'x-1/4, -y, z-1/4'
 '-x-1/2, y-1/4, z+1/4'
 '-z, -x+1/2, -y+1/2'
 '-z-1/2, x-1/4, y+1/4'
 'z-3/4, x+1/4, -y'
 'z-1/4, -x, y-1/4'
 '-y, -z+1/2, -x+1/2'
 'y-1/4, -z, x-1/4'
 '-y-1/2, z-1/4, x+1/4'
 'y-3/4, z+1/4, -x'
 '-y-3/4, -x+1/4, z'
 'y, x+1/2, z+1/2'
 '-y-1/4, x, -z-1/4'
 'y-1/2, -x-1/4, -z+1/4'
 '-x-3/4, -z+1/4, y'
 'x-1/2, -z-1/4, -y+1/4'
 'x, z+1/2, y+1/2'
 '-x-1/4, z, -y-1/4'
 '-z-3/4, -y+1/4, x'
 '-z-1/4, y, -x-1/4'
 'z-1/2, -y-1/4, -x+1/4'
 'z, y+1/2, x+1/2'
 '-x+1/2, -y, -z+1/2'
 'x-1/4, y-1/4, -z'
 'x+1/4, -y-1/2, z-1/4'
 '-x, y-3/4, z+1/4'
 '-z+1/2, -x, -y+1/2'
 '-z, x-3/4, y+1/4'
 'z-1/4, x-1/4, -y'
 'z+1/4, -x-1/2, y-1/4'
 '-y+1/2, -z, -x+1/2'
 'y+1/4, -z-1/2, x-1/4'
 '-y, z-3/4, x+1/4'
 'y-1/4, z-1/4, -x'
 '-y-1/4, -x-1/4, z'
 'y+1/2, x, z+1/2'
 '-y+1/4, x-1/2, -z-1/4'
 'y, -x-3/4, -z+1/4'
 '-x-1/4, -z-1/4, y'
 'x, -z-3/4, -y+1/4'
 'x+1/2, z, y+1/2'
 '-x+1/4, z-1/2, -y-1/4'
 '-z-1/4, -y-1/4, x'
 '-z+1/4, y-1/2, -x-1/4'
 'z, -y-3/4, -x+1/4'
 'z+1/2, y, x+1/2'
 '-x+1/2, -y+1/2, -z'
 'x-1/4, y+1/4, -z-1/2'
 'x+1/4, -y, z-3/4'
 '-x, y-1/4, z-1/4'
 '-z+1/2, -x+1/2, -y'
 '-z, x-1/4, y-1/4'
 'z-1/4, x+1/4, -y-1/2'
 'z+1/4, -x, y-3/4'
 '-y+1/2, -z+1/2, -x'
 'y+1/4, -z, x-3/4'
 '-y, z-1/4, x-1/4'
 'y-1/4, z+1/4, -x-1/2'
 '-y-1/4, -x+1/4, z-1/2'
 'y+1/2, x+1/2, z'
 '-y+1/4, x, -z-3/4'
 'y, -x-1/4, -z-1/4'
 '-x-1/4, -z+1/4, y-1/2'
 'x, -z-1/4, -y-1/4'
 'x+1/2, z+1/2, y'
 '-x+1/4, z, -y-3/4'
 '-z-1/4, -y+1/4, x-1/2'
 '-z+1/4, y, -x-3/4'
 'z, -y-1/4, -x-1/4'
 'z+1/2, y+1/2, x'
 
_cell_length_a                    10.3907(5)
_cell_length_b                    10.3907(5)
_cell_length_c                    10.3907(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1121.85(16)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     7.040          
_exptl_crystal_F_000              2167
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.200
_exptl_crystal_size_mid           0.180
_exptl_crystal_size_min           0.140
_exptl_absorpt_coefficient_mu     40.411
_shelx_estimated_absorpt_T_min    0.046
_shelx_estimated_absorpt_T_max    0.070
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             2345
_diffrn_reflns_av_unetI/netI      0.0205
_diffrn_reflns_av_R_equivalents   0.0437
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.396
_diffrn_reflns_theta_max          36.325
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.994
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              163
_reflns_number_gt                 160
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0331P)²+69.2246P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00114(17)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          163
_refine_ls_number_parameters      12
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0404
_refine_ls_R_factor_gt            0.0397
_refine_ls_wR_factor_ref          0.1140
_refine_ls_wR_factor_gt           0.1134
_refine_ls_goodness_of_fit_ref    1.286
_refine_ls_restrained_S_all       1.286
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pb Pb 0.5000 0.5000 0.5000 0.0221(6) Uani 0.561(8) 12 d S T P . .
Ca Ca 0.5000 0.5000 0.5000 0.0221(6) Uani 0.439(8) 12 d S T P . .
Sb Sb 0.0000 0.0000 0.0000 0.0100(5) Uani 0.8132 12 d S T P . .
Fe Fe 0.0000 0.0000 0.0000 0.0100(5) Uani 0.1868 12 d S T P . .
O1 O 0.3224(7) 0.1250 0.1250 0.0119(12) Uani 1 4 d S T P . .
O2 O 0.3750 0.3750 0.3750 0.015(5) Uani 0.5976 24 d S T P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pb O2 2.24965(11) 97_666 ?
Pb O2 2.24965(10) . ?
Pb O1 2.603(5) 177_556 ?
Pb O1 2.603(5) 81 ?
Pb O1 2.603(5) 149_565 ?
Pb O1 2.603(5) 53 ?
Pb O1 2.603(5) 121_655 ?
Pb O1 2.603(5) 25 ?
Pb Pb 3.67367(18) 26_554 ?
Pb Ca 3.67367(18) 50_564 ?
Pb Ca 3.67367(18) 27_645 ?
Pb Ca 3.67367(18) 75_545 ?
Sb O1 1.985(3) 130 ?
Sb O1 1.985(3) 34_544 ?
Sb O1 1.985(3) 174 ?
Sb O1 1.985(3) 78_445 ?
Sb O1 1.985(3) 146 ?
Sb O1 1.985(3) 50_454 ?
Sb Ca 3.67367(18) 2_554 ?
Sb Ca 3.67367(18) 28_445 ?
Sb Ca 3.67367(18) 4_455 ?
Sb Ca 3.67367(18) 51_544 ?
Sb Ca 3.67367(18) 3_545 ?
Sb Ca 3.67367(18) 74_454 ?
O1 Fe 1.985(3) 27_544 ?
O1 Fe 1.985(3) 50_454 ?
O1 Sb 1.985(3) 27_544 ?
O1 Sb 1.985(3) 50_454 ?
O1 Pb 2.603(5) 52_455 ?
O1 Ca 2.603(5) 52_455 ?
O1 Pb 2.603(5) 25_544 ?
O1 Ca 2.603(5) 25_544 ?
O2 Ca 2.24965(11) 52_455 ?
O2 Pb 2.24965(11) 26_554 ?
O2 Pb 2.24965(11) 75_545 ?
O2 Pb 2.24965(11) 52_455 ?
O2 Ca 2.24965(11) 26_554 ?
O2 Ca 2.24965(11) 75_545 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O2 Pb O2 180.0 97_666 . ?
O2 Pb O1 99.61(11) 97_666 177_556 ?
O2 Pb O1 80.39(11) . 177_556 ?
O2 Pb O1 80.39(11) 97_666 81 ?
O2 Pb O1 99.61(11) . 81 ?
O1 Pb O1 180.0 177_556 81 ?
O2 Pb O1 99.61(11) 97_666 149_565 ?
O2 Pb O1 80.39(11) . 149_565 ?
O1 Pb O1 117.27(6) 177_556 149_565 ?
O1 Pb O1 62.73(6) 81 149_565 ?
O2 Pb O1 80.39(11) 97_666 53 ?
O2 Pb O1 99.61(11) . 53 ?
O1 Pb O1 62.73(6) 177_556 53 ?
O1 Pb O1 117.27(6) 81 53 ?
O1 Pb O1 180.0 149_565 53 ?
O2 Pb O1 99.61(11) 97_666 121_655 ?
O2 Pb O1 80.39(11) . 121_655 ?
O1 Pb O1 117.27(6) 177_556 121_655 ?
O1 Pb O1 62.73(6) 81 121_655 ?
O1 Pb O1 117.27(6) 149_565 121_655 ?
O1 Pb O1 62.73(6) 53 121_655 ?
O2 Pb O1 80.39(11) 97_666 25 ?
O2 Pb O1 99.61(11) . 25 ?
O1 Pb O1 62.73(6) 177_556 25 ?
O1 Pb O1 117.27(6) 81 25 ?
O1 Pb O1 62.73(6) 149_565 25 ?
O1 Pb O1 117.27(6) 53 25 ?
O1 Pb O1 180.0 121_655 25 ?
O2 Pb Pb 144.7 97_666 26_554 ?
O2 Pb Pb 35.3 . 26_554 ?
O1 Pb Pb 45.13(11) 177_556 26_554 ?
O1 Pb Pb 134.87(11) 81 26_554 ?
O1 Pb Pb 98.53(9) 149_565 26_554 ?
O1 Pb Pb 81.47(9) 53 26_554 ?
O1 Pb Pb 98.53(9) 121_655 26_554 ?
O1 Pb Pb 81.47(9) 25 26_554 ?
O2 Pb Ca 35.3 97_666 50_564 ?
O2 Pb Ca 144.7 . 50_564 ?
O1 Pb Ca 134.87(11) 177_556 50_564 ?
O1 Pb Ca 45.13(11) 81 50_564 ?
O1 Pb Ca 81.47(9) 149_565 50_564 ?
O1 Pb Ca 98.53(9) 53 50_564 ?
O1 Pb Ca 81.47(9) 121_655 50_564 ?
O1 Pb Ca 98.53(9) 25 50_564 ?
Pb Pb Ca 180.0 26_554 50_564 ?
O2 Pb Ca 35.3 97_666 27_645 ?
O2 Pb Ca 144.7 . 27_645 ?
O1 Pb Ca 81.47(9) 177_556 27_645 ?
O1 Pb Ca 98.53(9) 81 27_645 ?
O1 Pb Ca 134.87(11) 149_565 27_645 ?
O1 Pb Ca 45.13(11) 53 27_645 ?
O1 Pb Ca 81.47(9) 121_655 27_645 ?
O1 Pb Ca 98.53(9) 25 27_645 ?
Pb Pb Ca 120.0 26_554 27_645 ?
Ca Pb Ca 60.0 50_564 27_645 ?
O2 Pb Ca 144.7 97_666 75_545 ?
O2 Pb Ca 35.3 . 75_545 ?
O1 Pb Ca 98.53(9) 177_556 75_545 ?
O1 Pb Ca 81.47(9) 81 75_545 ?
O1 Pb Ca 45.13(11) 149_565 75_545 ?
O1 Pb Ca 134.87(11) 53 75_545 ?
O1 Pb Ca 98.53(9) 121_655 75_545 ?
O1 Pb Ca 81.47(9) 25 75_545 ?
Pb Pb Ca 60.0 26_554 75_545 ?
Ca Pb Ca 120.0 50_564 75_545 ?
Ca Pb Ca 180.0 27_645 75_545 ?
O1 Sb O1 180.0(4) 130 34_544 ?
O1 Sb O1 93.9(2) 130 174 ?
O1 Sb O1 86.1(2) 34_544 174 ?
O1 Sb O1 86.1(2) 130 78_445 ?
O1 Sb O1 93.9(2) 34_544 78_445 ?
O1 Sb O1 180.0(4) 174 78_445 ?
O1 Sb O1 93.9(2) 130 146 ?
O1 Sb O1 86.1(2) 34_544 146 ?
O1 Sb O1 93.9(2) 174 146 ?
O1 Sb O1 86.1(2) 78_445 146 ?
O1 Sb O1 86.1(2) 130 50_454 ?
O1 Sb O1 93.9(2) 34_544 50_454 ?
O1 Sb O1 86.1(2) 174 50_454 ?
O1 Sb O1 93.9(2) 78_445 50_454 ?
O1 Sb O1 180.0(4) 146 50_454 ?
O1 Sb Ca 90.0 130 2_554 ?
O1 Sb Ca 90.0 34_544 2_554 ?
O1 Sb Ca 136.95(12) 174 2_554 ?
O1 Sb Ca 43.05(12) 78_445 2_554 ?
O1 Sb Ca 43.05(12) 146 2_554 ?
O1 Sb Ca 136.95(12) 50_454 2_554 ?
O1 Sb Ca 43.05(12) 130 28_445 ?
O1 Sb Ca 136.95(12) 34_544 28_445 ?
O1 Sb Ca 136.95(12) 174 28_445 ?
O1 Sb Ca 43.05(12) 78_445 28_445 ?
O1 Sb Ca 90.0 146 28_445 ?
O1 Sb Ca 90.0 50_454 28_445 ?
Ca Sb Ca 60.0 2_554 28_445 ?
O1 Sb Ca 136.95(12) 130 4_455 ?
O1 Sb Ca 43.05(12) 34_544 4_455 ?
O1 Sb Ca 43.05(12) 174 4_455 ?
O1 Sb Ca 136.95(12) 78_445 4_455 ?
O1 Sb Ca 90.0 146 4_455 ?
O1 Sb Ca 90.0 50_454 4_455 ?
Ca Sb Ca 120.0 2_554 4_455 ?
Ca Sb Ca 180.0 28_445 4_455 ?
O1 Sb Ca 136.95(12) 130 51_544 ?
O1 Sb Ca 43.05(12) 34_544 51_544 ?
O1 Sb Ca 90.0 174 51_544 ?
O1 Sb Ca 90.0 78_445 51_544 ?
O1 Sb Ca 43.05(12) 146 51_544 ?
O1 Sb Ca 136.95(12) 50_454 51_544 ?
Ca Sb Ca 60.0 2_554 51_544 ?
Ca Sb Ca 120.0 28_445 51_544 ?
Ca Sb Ca 60.0 4_455 51_544 ?
O1 Sb Ca 43.05(12) 130 3_545 ?
O1 Sb Ca 136.95(12) 34_544 3_545 ?
O1 Sb Ca 90.0 174 3_545 ?
O1 Sb Ca 90.0 78_445 3_545 ?
O1 Sb Ca 136.95(12) 146 3_545 ?
O1 Sb Ca 43.05(12) 50_454 3_545 ?
Ca Sb Ca 120.0 2_554 3_545 ?
Ca Sb Ca 60.0 28_445 3_545 ?
Ca Sb Ca 120.0 4_455 3_545 ?
Ca Sb Ca 180.0 51_544 3_545 ?
O1 Sb Ca 90.0 130 74_454 ?
O1 Sb Ca 90.0 34_544 74_454 ?
O1 Sb Ca 43.05(12) 174 74_454 ?
O1 Sb Ca 136.95(12) 78_445 74_454 ?
O1 Sb Ca 136.95(12) 146 74_454 ?
O1 Sb Ca 43.05(12) 50_454 74_454 ?
Ca Sb Ca 180.0 2_554 74_454 ?
Ca Sb Ca 120.0 28_445 74_454 ?
Ca Sb Ca 60.0 4_455 74_454 ?
Ca Sb Ca 120.0 51_544 74_454 ?
Ca Sb Ca 60.0 3_545 74_454 ?
Fe O1 Fe 135.4(4) 27_544 50_454 ?
Fe O1 Sb 0.0 27_544 27_544 ?
Fe O1 Sb 135.4(4) 50_454 27_544 ?
Fe O1 Sb 135.4(4) 27_544 50_454 ?
Fe O1 Sb 0.0 50_454 50_454 ?
Sb O1 Sb 135.4(4) 27_544 50_454 ?
Fe O1 Pb 105.59(9) 27_544 52_455 ?
Fe O1 Pb 105.59(9) 50_454 52_455 ?
Sb O1 Pb 105.59(9) 27_544 52_455 ?
Sb O1 Pb 105.59(9) 50_454 52_455 ?
Fe O1 Ca 105.59(9) 27_544 52_455 ?
Fe O1 Ca 105.59(9) 50_454 52_455 ?
Sb O1 Ca 105.59(9) 27_544 52_455 ?
Sb O1 Ca 105.59(9) 50_454 52_455 ?
Pb O1 Ca 0.0 52_455 52_455 ?
Fe O1 Pb 105.59(9) 27_544 25_544 ?
Fe O1 Pb 105.59(9) 50_454 25_544 ?
Sb O1 Pb 105.59(9) 27_544 25_544 ?
Sb O1 Pb 105.59(9) 50_454 25_544 ?
Pb O1 Pb 89.7(2) 52_455 25_544 ?
Ca O1 Pb 89.7(2) 52_455 25_544 ?
Fe O1 Ca 105.59(9) 27_544 25_544 ?
Fe O1 Ca 105.59(9) 50_454 25_544 ?
Sb O1 Ca 105.59(9) 27_544 25_544 ?
Sb O1 Ca 105.59(9) 50_454 25_544 ?
Pb O1 Ca 89.7(2) 52_455 25_544 ?
Ca O1 Ca 89.7(2) 52_455 25_544 ?
Pb O1 Ca 0.0 25_544 25_544 ?
Pb O2 Ca 109.471(1) . 52_455 ?
Pb O2 Pb 109.471(1) . 26_554 ?
Ca O2 Pb 109.5 52_455 26_554 ?
Pb O2 Pb 109.471(1) . 75_545 ?
Ca O2 Pb 109.5 52_455 75_545 ?
Pb O2 Pb 109.5 26_554 75_545 ?
Pb O2 Pb 109.471(1) . 52_455 ?
Ca O2 Pb 0.0 52_455 52_455 ?
Pb O2 Pb 109.5 26_554 52_455 ?
Pb O2 Pb 109.5 75_545 52_455 ?
Pb O2 Ca 109.471(1) . 26_554 ?
Ca O2 Ca 109.5 52_455 26_554 ?
Pb O2 Ca 0.0 26_554 26_554 ?
Pb O2 Ca 109.5 75_545 26_554 ?
Pb O2 Ca 109.5 52_455 26_554 ?
Pb O2 Ca 109.471(1) . 75_545 ?
Ca O2 Ca 109.5 52_455 75_545 ?
Pb O2 Ca 109.5 26_554 75_545 ?
Pb O2 Ca 0.0 75_545 75_545 ?
Pb O2 Ca 109.5 52_455 75_545 ?
Ca O2 Ca 109.5 26_554 75_545 ?
 
_refine_diff_density_max    1.715
_refine_diff_density_min   -1.276
_refine_diff_density_rms    0.297


 
data_#g31041
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Ca Fe0.12 O7 Pb Sb1.88' 
_chemical_formula_weight          594.53

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0080   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb'  'Sb'  -0.5866   1.5461
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.2262   0.3064
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            227
_space_group_name_H-M_alt         'F d -3 m'
_space_group_name_Hall            '-F 4vw 2vw 3'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+3/4, -y+1/4, z+1/2'
 '-x+1/4, y+1/2, -z+3/4'
 'x+1/2, -y+3/4, -z+1/4'
 'z, x, y'
 'z+1/2, -x+3/4, -y+1/4'
 '-z+3/4, -x+1/4, y+1/2'
 '-z+1/4, x+1/2, -y+3/4'
 'y, z, x'
 '-y+1/4, z+1/2, -x+3/4'
 'y+1/2, -z+3/4, -x+1/4'
 '-y+3/4, -z+1/4, x+1/2'
 'y+3/4, x+1/4, -z+1/2'
 '-y, -x, -z'
 'y+1/4, -x+1/2, z+3/4'
 '-y+1/2, x+3/4, z+1/4'
 'x+3/4, z+1/4, -y+1/2'
 '-x+1/2, z+3/4, y+1/4'
 '-x, -z, -y'
 'x+1/4, -z+1/2, y+3/4'
 'z+3/4, y+1/4, -x+1/2'
 'z+1/4, -y+1/2, x+3/4'
 '-z+1/2, y+3/4, x+1/4'
 '-z, -y, -x'
 'x, y+1/2, z+1/2'
 '-x+3/4, -y+3/4, z+1'
 '-x+1/4, y+1, -z+5/4'
 'x+1/2, -y+5/4, -z+3/4'
 'z, x+1/2, y+1/2'
 'z+1/2, -x+5/4, -y+3/4'
 '-z+3/4, -x+3/4, y+1'
 '-z+1/4, x+1, -y+5/4'
 'y, z+1/2, x+1/2'
 '-y+1/4, z+1, -x+5/4'
 'y+1/2, -z+5/4, -x+3/4'
 '-y+3/4, -z+3/4, x+1'
 'y+3/4, x+3/4, -z+1'
 '-y, -x+1/2, -z+1/2'
 'y+1/4, -x+1, z+5/4'
 '-y+1/2, x+5/4, z+3/4'
 'x+3/4, z+3/4, -y+1'
 '-x+1/2, z+5/4, y+3/4'
 '-x, -z+1/2, -y+1/2'
 'x+1/4, -z+1, y+5/4'
 'z+3/4, y+3/4, -x+1'
 'z+1/4, -y+1, x+5/4'
 '-z+1/2, y+5/4, x+3/4'
 '-z, -y+1/2, -x+1/2'
 'x+1/2, y, z+1/2'
 '-x+5/4, -y+1/4, z+1'
 '-x+3/4, y+1/2, -z+5/4'
 'x+1, -y+3/4, -z+3/4'
 'z+1/2, x, y+1/2'
 'z+1, -x+3/4, -y+3/4'
 '-z+5/4, -x+1/4, y+1'
 '-z+3/4, x+1/2, -y+5/4'
 'y+1/2, z, x+1/2'
 '-y+3/4, z+1/2, -x+5/4'
 'y+1, -z+3/4, -x+3/4'
 '-y+5/4, -z+1/4, x+1'
 'y+5/4, x+1/4, -z+1'
 '-y+1/2, -x, -z+1/2'
 'y+3/4, -x+1/2, z+5/4'
 '-y+1, x+3/4, z+3/4'
 'x+5/4, z+1/4, -y+1'
 '-x+1, z+3/4, y+3/4'
 '-x+1/2, -z, -y+1/2'
 'x+3/4, -z+1/2, y+5/4'
 'z+5/4, y+1/4, -x+1'
 'z+3/4, -y+1/2, x+5/4'
 '-z+1, y+3/4, x+3/4'
 '-z+1/2, -y, -x+1/2'
 'x+1/2, y+1/2, z'
 '-x+5/4, -y+3/4, z+1/2'
 '-x+3/4, y+1, -z+3/4'
 'x+1, -y+5/4, -z+1/4'
 'z+1/2, x+1/2, y'
 'z+1, -x+5/4, -y+1/4'
 '-z+5/4, -x+3/4, y+1/2'
 '-z+3/4, x+1, -y+3/4'
 'y+1/2, z+1/2, x'
 '-y+3/4, z+1, -x+3/4'
 'y+1, -z+5/4, -x+1/4'
 '-y+5/4, -z+3/4, x+1/2'
 'y+5/4, x+3/4, -z+1/2'
 '-y+1/2, -x+1/2, -z'
 'y+3/4, -x+1, z+3/4'
 '-y+1, x+5/4, z+1/4'
 'x+5/4, z+3/4, -y+1/2'
 '-x+1, z+5/4, y+1/4'
 '-x+1/2, -z+1/2, -y'
 'x+3/4, -z+1, y+3/4'
 'z+5/4, y+3/4, -x+1/2'
 'z+3/4, -y+1, x+3/4'
 '-z+1, y+5/4, x+1/4'
 '-z+1/2, -y+1/2, -x'
 '-x, -y, -z'
 'x-3/4, y-1/4, -z-1/2'
 'x-1/4, -y-1/2, z-3/4'
 '-x-1/2, y-3/4, z-1/4'
 '-z, -x, -y'
 '-z-1/2, x-3/4, y-1/4'
 'z-3/4, x-1/4, -y-1/2'
 'z-1/4, -x-1/2, y-3/4'
 '-y, -z, -x'
 'y-1/4, -z-1/2, x-3/4'
 '-y-1/2, z-3/4, x-1/4'
 'y-3/4, z-1/4, -x-1/2'
 '-y-3/4, -x-1/4, z-1/2'
 'y, x, z'
 '-y-1/4, x-1/2, -z-3/4'
 'y-1/2, -x-3/4, -z-1/4'
 '-x-3/4, -z-1/4, y-1/2'
 'x-1/2, -z-3/4, -y-1/4'
 'x, z, y'
 '-x-1/4, z-1/2, -y-3/4'
 '-z-3/4, -y-1/4, x-1/2'
 '-z-1/4, y-1/2, -x-3/4'
 'z-1/2, -y-3/4, -x-1/4'
 'z, y, x'
 '-x, -y+1/2, -z+1/2'
 'x-3/4, y+1/4, -z'
 'x-1/4, -y, z-1/4'
 '-x-1/2, y-1/4, z+1/4'
 '-z, -x+1/2, -y+1/2'
 '-z-1/2, x-1/4, y+1/4'
 'z-3/4, x+1/4, -y'
 'z-1/4, -x, y-1/4'
 '-y, -z+1/2, -x+1/2'
 'y-1/4, -z, x-1/4'
 '-y-1/2, z-1/4, x+1/4'
 'y-3/4, z+1/4, -x'
 '-y-3/4, -x+1/4, z'
 'y, x+1/2, z+1/2'
 '-y-1/4, x, -z-1/4'
 'y-1/2, -x-1/4, -z+1/4'
 '-x-3/4, -z+1/4, y'
 'x-1/2, -z-1/4, -y+1/4'
 'x, z+1/2, y+1/2'
 '-x-1/4, z, -y-1/4'
 '-z-3/4, -y+1/4, x'
 '-z-1/4, y, -x-1/4'
 'z-1/2, -y-1/4, -x+1/4'
 'z, y+1/2, x+1/2'
 '-x+1/2, -y, -z+1/2'
 'x-1/4, y-1/4, -z'
 'x+1/4, -y-1/2, z-1/4'
 '-x, y-3/4, z+1/4'
 '-z+1/2, -x, -y+1/2'
 '-z, x-3/4, y+1/4'
 'z-1/4, x-1/4, -y'
 'z+1/4, -x-1/2, y-1/4'
 '-y+1/2, -z, -x+1/2'
 'y+1/4, -z-1/2, x-1/4'
 '-y, z-3/4, x+1/4'
 'y-1/4, z-1/4, -x'
 '-y-1/4, -x-1/4, z'
 'y+1/2, x, z+1/2'
 '-y+1/4, x-1/2, -z-1/4'
 'y, -x-3/4, -z+1/4'
 '-x-1/4, -z-1/4, y'
 'x, -z-3/4, -y+1/4'
 'x+1/2, z, y+1/2'
 '-x+1/4, z-1/2, -y-1/4'
 '-z-1/4, -y-1/4, x'
 '-z+1/4, y-1/2, -x-1/4'
 'z, -y-3/4, -x+1/4'
 'z+1/2, y, x+1/2'
 '-x+1/2, -y+1/2, -z'
 'x-1/4, y+1/4, -z-1/2'
 'x+1/4, -y, z-3/4'
 '-x, y-1/4, z-1/4'
 '-z+1/2, -x+1/2, -y'
 '-z, x-1/4, y-1/4'
 'z-1/4, x+1/4, -y-1/2'
 'z+1/4, -x, y-3/4'
 '-y+1/2, -z+1/2, -x'
 'y+1/4, -z, x-3/4'
 '-y, z-1/4, x-1/4'
 'y-1/4, z+1/4, -x-1/2'
 '-y-1/4, -x+1/4, z-1/2'
 'y+1/2, x+1/2, z'
 '-y+1/4, x, -z-3/4'
 'y, -x-1/4, -z-1/4'
 '-x-1/4, -z+1/4, y-1/2'
 'x, -z-1/4, -y-1/4'
 'x+1/2, z+1/2, y'
 '-x+1/4, z, -y-3/4'
 '-z-1/4, -y+1/4, x-1/2'
 '-z+1/4, y, -x-3/4'
 'z, -y-1/4, -x-1/4'
 'z+1/2, y+1/2, x'
 
_cell_length_a                    10.3863(5)
_cell_length_b                    10.3863(5)
_cell_length_c                    10.3863(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1120.42(16)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     7.049          
_exptl_crystal_F_000              2167
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.120
_exptl_crystal_size_mid           0.110
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     40.462
_shelx_estimated_absorpt_T_min    0.085
_shelx_estimated_absorpt_T_max    0.107
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             2254
_diffrn_reflns_av_unetI/netI      0.0079
_diffrn_reflns_av_R_equivalents   0.0161
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.397
_diffrn_reflns_theta_max          36.343
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.994
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              163
_reflns_number_gt                 156
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0155P)²+21.9663P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00070(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          163
_refine_ls_number_parameters      13
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0232
_refine_ls_R_factor_gt            0.0218
_refine_ls_wR_factor_ref          0.0545
_refine_ls_wR_factor_gt           0.0538
_refine_ls_goodness_of_fit_ref    1.325
_refine_ls_restrained_S_all       1.325
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pb Pb 0.5000 0.5000 0.5000 0.0181(3) Uani 0.485(4) 12 d S T P . .
Ca Ca 0.5000 0.5000 0.5000 0.0181(3) Uani 0.515(4) 12 d S T P . .
Sb Sb 0.0000 0.0000 0.0000 0.0069(2) Uani 0.8594 12 d S T P . .
Fe Fe 0.0000 0.0000 0.0000 0.0069(2) Uani 0.1405 12 d S T P . .
O1 O 0.3224(4) 0.1250 0.1250 0.0095(7) Uani 1 4 d S T P . .
O2 O 0.3750 0.3750 0.3750 0.017(3) Uani 0.74(3) 24 d S T . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pb O2 2.24870(10) 97_666 ?
Pb O2 2.24870(11) . ?
Pb O1 2.602(3) 177_556 ?
Pb O1 2.602(3) 81 ?
Pb O1 2.602(3) 149_565 ?
Pb O1 2.602(3) 53 ?
Pb O1 2.602(3) 121_655 ?
Pb O1 2.602(3) 25 ?
Pb Pb 3.67211(18) 26_554 ?
Pb Ca 3.67211(17) 50_564 ?
Pb Ca 3.67211(17) 27_645 ?
Pb Ca 3.67211(18) 75_545 ?
Sb O1 1.9842(15) 174 ?
Sb O1 1.9842(15) 78_445 ?
Sb O1 1.9842(15) 146 ?
Sb O1 1.9842(15) 50_454 ?
Sb O1 1.9842(15) 130 ?
Sb O1 1.9842(15) 34_544 ?
Sb Ca 3.67211(18) 4_455 ?
Sb Ca 3.67211(18) 51_544 ?
Sb Ca 3.67211(18) 3_545 ?
Sb Ca 3.67211(18) 74_454 ?
Sb Ca 3.67211(18) 2_554 ?
Sb Ca 3.67211(18) 28_445 ?
O1 Fe 1.9842(15) 27_544 ?
O1 Sb 1.9842(15) 27_544 ?
O1 Fe 1.9842(15) 50_454 ?
O1 Sb 1.9842(15) 50_454 ?
O1 Pb 2.602(3) 52_455 ?
O1 Ca 2.602(3) 52_455 ?
O1 Pb 2.602(3) 25_544 ?
O1 Ca 2.602(3) 25_544 ?
O2 Ca 2.24870(11) 52_455 ?
O2 Pb 2.24870(11) 26_554 ?
O2 Pb 2.24870(11) 75_545 ?
O2 Pb 2.24870(11) 52_455 ?
O2 Ca 2.24870(11) 26_554 ?
O2 Ca 2.24870(11) 75_545 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O2 Pb O2 180.0 97_666 . ?
O2 Pb O1 99.61(6) 97_666 177_556 ?
O2 Pb O1 80.39(6) . 177_556 ?
O2 Pb O1 80.39(6) 97_666 81 ?
O2 Pb O1 99.61(6) . 81 ?
O1 Pb O1 180.0 177_556 81 ?
O2 Pb O1 99.61(6) 97_666 149_565 ?
O2 Pb O1 80.39(6) . 149_565 ?
O1 Pb O1 117.27(3) 177_556 149_565 ?
O1 Pb O1 62.73(3) 81 149_565 ?
O2 Pb O1 80.39(6) 97_666 53 ?
O2 Pb O1 99.61(6) . 53 ?
O1 Pb O1 62.73(3) 177_556 53 ?
O1 Pb O1 117.27(3) 81 53 ?
O1 Pb O1 180.0 149_565 53 ?
O2 Pb O1 99.61(6) 97_666 121_655 ?
O2 Pb O1 80.39(6) . 121_655 ?
O1 Pb O1 117.27(3) 177_556 121_655 ?
O1 Pb O1 62.73(3) 81 121_655 ?
O1 Pb O1 117.27(3) 149_565 121_655 ?
O1 Pb O1 62.73(3) 53 121_655 ?
O2 Pb O1 80.39(6) 97_666 25 ?
O2 Pb O1 99.61(6) . 25 ?
O1 Pb O1 62.73(3) 177_556 25 ?
O1 Pb O1 117.27(3) 81 25 ?
O1 Pb O1 62.73(3) 149_565 25 ?
O1 Pb O1 117.27(3) 53 25 ?
O1 Pb O1 180.0 121_655 25 ?
O2 Pb Pb 144.7 97_666 26_554 ?
O2 Pb Pb 35.3 . 26_554 ?
O1 Pb Pb 45.13(6) 177_556 26_554 ?
O1 Pb Pb 134.87(6) 81 26_554 ?
O1 Pb Pb 98.53(5) 149_565 26_554 ?
O1 Pb Pb 81.47(5) 53 26_554 ?
O1 Pb Pb 98.53(5) 121_655 26_554 ?
O1 Pb Pb 81.47(5) 25 26_554 ?
O2 Pb Ca 35.3 97_666 50_564 ?
O2 Pb Ca 144.7 . 50_564 ?
O1 Pb Ca 134.87(6) 177_556 50_564 ?
O1 Pb Ca 45.13(6) 81 50_564 ?
O1 Pb Ca 81.47(5) 149_565 50_564 ?
O1 Pb Ca 98.53(5) 53 50_564 ?
O1 Pb Ca 81.47(5) 121_655 50_564 ?
O1 Pb Ca 98.53(5) 25 50_564 ?
Pb Pb Ca 180.0 26_554 50_564 ?
O2 Pb Ca 35.3 97_666 27_645 ?
O2 Pb Ca 144.7 . 27_645 ?
O1 Pb Ca 81.47(5) 177_556 27_645 ?
O1 Pb Ca 98.53(5) 81 27_645 ?
O1 Pb Ca 134.87(6) 149_565 27_645 ?
O1 Pb Ca 45.13(6) 53 27_645 ?
O1 Pb Ca 81.47(5) 121_655 27_645 ?
O1 Pb Ca 98.53(5) 25 27_645 ?
Pb Pb Ca 120.0 26_554 27_645 ?
Ca Pb Ca 60.0 50_564 27_645 ?
O2 Pb Ca 144.7 97_666 75_545 ?
O2 Pb Ca 35.3 . 75_545 ?
O1 Pb Ca 98.53(5) 177_556 75_545 ?
O1 Pb Ca 81.47(5) 81 75_545 ?
O1 Pb Ca 45.13(6) 149_565 75_545 ?
O1 Pb Ca 134.87(6) 53 75_545 ?
O1 Pb Ca 98.53(5) 121_655 75_545 ?
O1 Pb Ca 81.47(5) 25 75_545 ?
Pb Pb Ca 60.0 26_554 75_545 ?
Ca Pb Ca 120.0 50_564 75_545 ?
Ca Pb Ca 180.0 27_645 75_545 ?
O1 Sb O1 180.0(2) 174 78_445 ?
O1 Sb O1 93.90(14) 174 146 ?
O1 Sb O1 86.10(14) 78_445 146 ?
O1 Sb O1 86.10(14) 174 50_454 ?
O1 Sb O1 93.90(14) 78_445 50_454 ?
O1 Sb O1 180.0(2) 146 50_454 ?
O1 Sb O1 93.90(14) 174 130 ?
O1 Sb O1 86.10(14) 78_445 130 ?
O1 Sb O1 93.90(14) 146 130 ?
O1 Sb O1 86.10(14) 50_454 130 ?
O1 Sb O1 86.10(14) 174 34_544 ?
O1 Sb O1 93.90(14) 78_445 34_544 ?
O1 Sb O1 86.10(14) 146 34_544 ?
O1 Sb O1 93.90(14) 50_454 34_544 ?
O1 Sb O1 180.0(2) 130 34_544 ?
O1 Sb Ca 43.05(7) 174 4_455 ?
O1 Sb Ca 136.95(7) 78_445 4_455 ?
O1 Sb Ca 90.0 146 4_455 ?
O1 Sb Ca 90.0 50_454 4_455 ?
O1 Sb Ca 136.95(7) 130 4_455 ?
O1 Sb Ca 43.05(7) 34_544 4_455 ?
O1 Sb Ca 90.0 174 51_544 ?
O1 Sb Ca 90.0 78_445 51_544 ?
O1 Sb Ca 43.05(7) 146 51_544 ?
O1 Sb Ca 136.95(7) 50_454 51_544 ?
O1 Sb Ca 136.95(7) 130 51_544 ?
O1 Sb Ca 43.05(7) 34_544 51_544 ?
Ca Sb Ca 60.0 4_455 51_544 ?
O1 Sb Ca 90.0 174 3_545 ?
O1 Sb Ca 90.0 78_445 3_545 ?
O1 Sb Ca 136.95(7) 146 3_545 ?
O1 Sb Ca 43.05(7) 50_454 3_545 ?
O1 Sb Ca 43.05(7) 130 3_545 ?
O1 Sb Ca 136.95(7) 34_544 3_545 ?
Ca Sb Ca 120.0 4_455 3_545 ?
Ca Sb Ca 180.0 51_544 3_545 ?
O1 Sb Ca 43.05(7) 174 74_454 ?
O1 Sb Ca 136.95(7) 78_445 74_454 ?
O1 Sb Ca 136.95(7) 146 74_454 ?
O1 Sb Ca 43.05(7) 50_454 74_454 ?
O1 Sb Ca 90.0 130 74_454 ?
O1 Sb Ca 90.0 34_544 74_454 ?
Ca Sb Ca 60.0 4_455 74_454 ?
Ca Sb Ca 120.0 51_544 74_454 ?
Ca Sb Ca 60.0 3_545 74_454 ?
O1 Sb Ca 136.95(7) 174 2_554 ?
O1 Sb Ca 43.05(7) 78_445 2_554 ?
O1 Sb Ca 43.05(7) 146 2_554 ?
O1 Sb Ca 136.95(7) 50_454 2_554 ?
O1 Sb Ca 90.0 130 2_554 ?
O1 Sb Ca 90.0 34_544 2_554 ?
Ca Sb Ca 120.0 4_455 2_554 ?
Ca Sb Ca 60.0 51_544 2_554 ?
Ca Sb Ca 120.0 3_545 2_554 ?
Ca Sb Ca 180.0 74_454 2_554 ?
O1 Sb Ca 136.95(7) 174 28_445 ?
O1 Sb Ca 43.05(7) 78_445 28_445 ?
O1 Sb Ca 90.0 146 28_445 ?
O1 Sb Ca 90.0 50_454 28_445 ?
O1 Sb Ca 43.05(7) 130 28_445 ?
O1 Sb Ca 136.95(7) 34_544 28_445 ?
Ca Sb Ca 180.0 4_455 28_445 ?
Ca Sb Ca 120.0 51_544 28_445 ?
Ca Sb Ca 60.0 3_545 28_445 ?
Ca Sb Ca 120.0 74_454 28_445 ?
Ca Sb Ca 60.0 2_554 28_445 ?
Fe O1 Sb 0.0 27_544 27_544 ?
Fe O1 Fe 135.4(2) 27_544 50_454 ?
Sb O1 Fe 135.4(2) 27_544 50_454 ?
Fe O1 Sb 135.4(2) 27_544 50_454 ?
Sb O1 Sb 135.4(2) 27_544 50_454 ?
Fe O1 Sb 0.0 50_454 50_454 ?
Fe O1 Pb 105.59(5) 27_544 52_455 ?
Sb O1 Pb 105.59(5) 27_544 52_455 ?
Fe O1 Pb 105.59(5) 50_454 52_455 ?
Sb O1 Pb 105.59(5) 50_454 52_455 ?
Fe O1 Ca 105.59(5) 27_544 52_455 ?
Sb O1 Ca 105.59(5) 27_544 52_455 ?
Fe O1 Ca 105.59(5) 50_454 52_455 ?
Sb O1 Ca 105.59(5) 50_454 52_455 ?
Pb O1 Ca 0.0 52_455 52_455 ?
Fe O1 Pb 105.59(5) 27_544 25_544 ?
Sb O1 Pb 105.59(5) 27_544 25_544 ?
Fe O1 Pb 105.59(5) 50_454 25_544 ?
Sb O1 Pb 105.59(5) 50_454 25_544 ?
Pb O1 Pb 89.74(12) 52_455 25_544 ?
Ca O1 Pb 89.74(12) 52_455 25_544 ?
Fe O1 Ca 105.59(5) 27_544 25_544 ?
Sb O1 Ca 105.59(5) 27_544 25_544 ?
Fe O1 Ca 105.59(5) 50_454 25_544 ?
Sb O1 Ca 105.59(5) 50_454 25_544 ?
Pb O1 Ca 89.74(12) 52_455 25_544 ?
Ca O1 Ca 89.74(12) 52_455 25_544 ?
Pb O1 Ca 0.0 25_544 25_544 ?
Pb O2 Ca 109.5 . 52_455 ?
Pb O2 Pb 109.5 . 26_554 ?
Ca O2 Pb 109.5 52_455 26_554 ?
Pb O2 Pb 109.5 . 75_545 ?
Ca O2 Pb 109.5 52_455 75_545 ?
Pb O2 Pb 109.5 26_554 75_545 ?
Pb O2 Pb 109.5 . 52_455 ?
Ca O2 Pb 0.0 52_455 52_455 ?
Pb O2 Pb 109.5 26_554 52_455 ?
Pb O2 Pb 109.5 75_545 52_455 ?
Pb O2 Ca 109.5 . 26_554 ?
Ca O2 Ca 109.5 52_455 26_554 ?
Pb O2 Ca 0.0 26_554 26_554 ?
Pb O2 Ca 109.5 75_545 26_554 ?
Pb O2 Ca 109.5 52_455 26_554 ?
Pb O2 Ca 109.5 . 75_545 ?
Ca O2 Ca 109.5 52_455 75_545 ?
Pb O2 Ca 109.5 26_554 75_545 ?
Pb O2 Ca 0.0 75_545 75_545 ?
Pb O2 Ca 109.5 52_455 75_545 ?
Ca O2 Ca 109.5 26_554 75_545 ?
 
_refine_diff_density_max    0.656
_refine_diff_density_min   -1.023
_refine_diff_density_rms    0.167


 
data_#20140122
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Ca F Na O6 Sb2' 
_chemical_formula_weight          421.57

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na'  'Na'   0.0362   0.0249
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb'  'Sb'  -0.5866   1.5461
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.2262   0.3064
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            227
_space_group_name_H-M_alt         'F d -3 m'
_space_group_name_Hall            '-F 4vw 2vw 3'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+3/4, -y+1/4, z+1/2'
 '-x+1/4, y+1/2, -z+3/4'
 'x+1/2, -y+3/4, -z+1/4'
 'z, x, y'
 'z+1/2, -x+3/4, -y+1/4'
 '-z+3/4, -x+1/4, y+1/2'
 '-z+1/4, x+1/2, -y+3/4'
 'y, z, x'
 '-y+1/4, z+1/2, -x+3/4'
 'y+1/2, -z+3/4, -x+1/4'
 '-y+3/4, -z+1/4, x+1/2'
 'y+3/4, x+1/4, -z+1/2'
 '-y, -x, -z'
 'y+1/4, -x+1/2, z+3/4'
 '-y+1/2, x+3/4, z+1/4'
 'x+3/4, z+1/4, -y+1/2'
 '-x+1/2, z+3/4, y+1/4'
 '-x, -z, -y'
 'x+1/4, -z+1/2, y+3/4'
 'z+3/4, y+1/4, -x+1/2'
 'z+1/4, -y+1/2, x+3/4'
 '-z+1/2, y+3/4, x+1/4'
 '-z, -y, -x'
 'x, y+1/2, z+1/2'
 '-x+3/4, -y+3/4, z+1'
 '-x+1/4, y+1, -z+5/4'
 'x+1/2, -y+5/4, -z+3/4'
 'z, x+1/2, y+1/2'
 'z+1/2, -x+5/4, -y+3/4'
 '-z+3/4, -x+3/4, y+1'
 '-z+1/4, x+1, -y+5/4'
 'y, z+1/2, x+1/2'
 '-y+1/4, z+1, -x+5/4'
 'y+1/2, -z+5/4, -x+3/4'
 '-y+3/4, -z+3/4, x+1'
 'y+3/4, x+3/4, -z+1'
 '-y, -x+1/2, -z+1/2'
 'y+1/4, -x+1, z+5/4'
 '-y+1/2, x+5/4, z+3/4'
 'x+3/4, z+3/4, -y+1'
 '-x+1/2, z+5/4, y+3/4'
 '-x, -z+1/2, -y+1/2'
 'x+1/4, -z+1, y+5/4'
 'z+3/4, y+3/4, -x+1'
 'z+1/4, -y+1, x+5/4'
 '-z+1/2, y+5/4, x+3/4'
 '-z, -y+1/2, -x+1/2'
 'x+1/2, y, z+1/2'
 '-x+5/4, -y+1/4, z+1'
 '-x+3/4, y+1/2, -z+5/4'
 'x+1, -y+3/4, -z+3/4'
 'z+1/2, x, y+1/2'
 'z+1, -x+3/4, -y+3/4'
 '-z+5/4, -x+1/4, y+1'
 '-z+3/4, x+1/2, -y+5/4'
 'y+1/2, z, x+1/2'
 '-y+3/4, z+1/2, -x+5/4'
 'y+1, -z+3/4, -x+3/4'
 '-y+5/4, -z+1/4, x+1'
 'y+5/4, x+1/4, -z+1'
 '-y+1/2, -x, -z+1/2'
 'y+3/4, -x+1/2, z+5/4'
 '-y+1, x+3/4, z+3/4'
 'x+5/4, z+1/4, -y+1'
 '-x+1, z+3/4, y+3/4'
 '-x+1/2, -z, -y+1/2'
 'x+3/4, -z+1/2, y+5/4'
 'z+5/4, y+1/4, -x+1'
 'z+3/4, -y+1/2, x+5/4'
 '-z+1, y+3/4, x+3/4'
 '-z+1/2, -y, -x+1/2'
 'x+1/2, y+1/2, z'
 '-x+5/4, -y+3/4, z+1/2'
 '-x+3/4, y+1, -z+3/4'
 'x+1, -y+5/4, -z+1/4'
 'z+1/2, x+1/2, y'
 'z+1, -x+5/4, -y+1/4'
 '-z+5/4, -x+3/4, y+1/2'
 '-z+3/4, x+1, -y+3/4'
 'y+1/2, z+1/2, x'
 '-y+3/4, z+1, -x+3/4'
 'y+1, -z+5/4, -x+1/4'
 '-y+5/4, -z+3/4, x+1/2'
 'y+5/4, x+3/4, -z+1/2'
 '-y+1/2, -x+1/2, -z'
 'y+3/4, -x+1, z+3/4'
 '-y+1, x+5/4, z+1/4'
 'x+5/4, z+3/4, -y+1/2'
 '-x+1, z+5/4, y+1/4'
 '-x+1/2, -z+1/2, -y'
 'x+3/4, -z+1, y+3/4'
 'z+5/4, y+3/4, -x+1/2'
 'z+3/4, -y+1, x+3/4'
 '-z+1, y+5/4, x+1/4'
 '-z+1/2, -y+1/2, -x'
 '-x, -y, -z'
 'x-3/4, y-1/4, -z-1/2'
 'x-1/4, -y-1/2, z-3/4'
 '-x-1/2, y-3/4, z-1/4'
 '-z, -x, -y'
 '-z-1/2, x-3/4, y-1/4'
 'z-3/4, x-1/4, -y-1/2'
 'z-1/4, -x-1/2, y-3/4'
 '-y, -z, -x'
 'y-1/4, -z-1/2, x-3/4'
 '-y-1/2, z-3/4, x-1/4'
 'y-3/4, z-1/4, -x-1/2'
 '-y-3/4, -x-1/4, z-1/2'
 'y, x, z'
 '-y-1/4, x-1/2, -z-3/4'
 'y-1/2, -x-3/4, -z-1/4'
 '-x-3/4, -z-1/4, y-1/2'
 'x-1/2, -z-3/4, -y-1/4'
 'x, z, y'
 '-x-1/4, z-1/2, -y-3/4'
 '-z-3/4, -y-1/4, x-1/2'
 '-z-1/4, y-1/2, -x-3/4'
 'z-1/2, -y-3/4, -x-1/4'
 'z, y, x'
 '-x, -y+1/2, -z+1/2'
 'x-3/4, y+1/4, -z'
 'x-1/4, -y, z-1/4'
 '-x-1/2, y-1/4, z+1/4'
 '-z, -x+1/2, -y+1/2'
 '-z-1/2, x-1/4, y+1/4'
 'z-3/4, x+1/4, -y'
 'z-1/4, -x, y-1/4'
 '-y, -z+1/2, -x+1/2'
 'y-1/4, -z, x-1/4'
 '-y-1/2, z-1/4, x+1/4'
 'y-3/4, z+1/4, -x'
 '-y-3/4, -x+1/4, z'
 'y, x+1/2, z+1/2'
 '-y-1/4, x, -z-1/4'
 'y-1/2, -x-1/4, -z+1/4'
 '-x-3/4, -z+1/4, y'
 'x-1/2, -z-1/4, -y+1/4'
 'x, z+1/2, y+1/2'
 '-x-1/4, z, -y-1/4'
 '-z-3/4, -y+1/4, x'
 '-z-1/4, y, -x-1/4'
 'z-1/2, -y-1/4, -x+1/4'
 'z, y+1/2, x+1/2'
 '-x+1/2, -y, -z+1/2'
 'x-1/4, y-1/4, -z'
 'x+1/4, -y-1/2, z-1/4'
 '-x, y-3/4, z+1/4'
 '-z+1/2, -x, -y+1/2'
 '-z, x-3/4, y+1/4'
 'z-1/4, x-1/4, -y'
 'z+1/4, -x-1/2, y-1/4'
 '-y+1/2, -z, -x+1/2'
 'y+1/4, -z-1/2, x-1/4'
 '-y, z-3/4, x+1/4'
 'y-1/4, z-1/4, -x'
 '-y-1/4, -x-1/4, z'
 'y+1/2, x, z+1/2'
 '-y+1/4, x-1/2, -z-1/4'
 'y, -x-3/4, -z+1/4'
 '-x-1/4, -z-1/4, y'
 'x, -z-3/4, -y+1/4'
 'x+1/2, z, y+1/2'
 '-x+1/4, z-1/2, -y-1/4'
 '-z-1/4, -y-1/4, x'
 '-z+1/4, y-1/2, -x-1/4'
 'z, -y-3/4, -x+1/4'
 'z+1/2, y, x+1/2'
 '-x+1/2, -y+1/2, -z'
 'x-1/4, y+1/4, -z-1/2'
 'x+1/4, -y, z-3/4'
 '-x, y-1/4, z-1/4'
 '-z+1/2, -x+1/2, -y'
 '-z, x-1/4, y-1/4'
 'z-1/4, x+1/4, -y-1/2'
 'z+1/4, -x, y-3/4'
 '-y+1/2, -z+1/2, -x'
 'y+1/4, -z, x-3/4'
 '-y, z-1/4, x-1/4'
 'y-1/4, z+1/4, -x-1/2'
 '-y-1/4, -x+1/4, z-1/2'
 'y+1/2, x+1/2, z'
 '-y+1/4, x, -z-3/4'
 'y, -x-1/4, -z-1/4'
 '-x-1/4, -z+1/4, y-1/2'
 'x, -z-1/4, -y-1/4'
 'x+1/2, z+1/2, y'
 '-x+1/4, z, -y-3/4'
 '-z-1/4, -y+1/4, x-1/2'
 '-z+1/4, y, -x-3/4'
 'z, -y-1/4, -x-1/4'
 'z+1/2, y+1/2, x'
 
_cell_length_a                    10.3157(2)
_cell_length_b                    10.3157(2)
_cell_length_c                    10.3157(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1097.73(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     5.102          
_exptl_crystal_F_000              1520
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.140
_exptl_crystal_size_mid           0.130
_exptl_crystal_size_min           0.120
_exptl_absorpt_coefficient_mu     10.853
_shelx_estimated_absorpt_T_min    0.312
_shelx_estimated_absorpt_T_max    0.356
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?                       
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             2284
_diffrn_reflns_av_unetI/netI      0.0059
_diffrn_reflns_av_R_equivalents   0.0132
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          3.421
_diffrn_reflns_theta_max          36.632
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.970
_diffrn_measured_fraction_theta_full  0.985
_diffrn_reflns_Laue_measured_fraction_max    0.970
_diffrn_reflns_Laue_measured_fraction_full   0.985
_diffrn_reflns_point_group_measured_fraction_max   0.970
_diffrn_reflns_point_group_measured_fraction_full  0.985
_reflns_number_total              159
_reflns_number_gt                 148
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0055P)²+11.7845P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00081(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          159
_refine_ls_number_parameters      13
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0137
_refine_ls_R_factor_gt            0.0121
_refine_ls_wR_factor_ref          0.0281
_refine_ls_wR_factor_gt           0.0272
_refine_ls_goodness_of_fit_ref    1.339
_refine_ls_restrained_S_all       1.339
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ca Ca 0.5000 0.5000 0.5000 0.0151(6) Uani 0.65(3) 12 d S T P . .
Na Na 0.5000 0.5000 0.5000 0.0151(6) Uani 0.35(3) 12 d S T P . .
Sb Sb 0.0000 0.0000 0.0000 0.00473(12) Uani 0.968(9) 12 d S T . . .
O1 O 0.3235(2) 0.1250 0.1250 0.0108(5) Uani 1 4 d S T P . .
F2 F 0.3750 0.3750 0.3750 0.0167(10) Uani 1 24 d S T P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ca F2 2.23342(4) 97_666 ?
Ca F2 2.23342(4) . ?
Ca O1 2.5771(16) 177_556 ?
Ca O1 2.5771(16) 81 ?
Ca O1 2.5771(16) 149_565 ?
Ca O1 2.5771(16) 53 ?
Ca O1 2.5771(16) 121_655 ?
Ca O1 2.5771(16) 25 ?
Ca Ca 3.64715(7) 26_554 ?
Ca Na 3.64715(8) 50_564 ?
Ca Na 3.64715(8) 27_645 ?
Ca Na 3.64715(7) 75_545 ?
Sb O1 1.9748(9) 174 ?
Sb O1 1.9748(9) 78_445 ?
Sb O1 1.9748(9) 130 ?
Sb O1 1.9748(9) 34_544 ?
Sb O1 1.9748(9) 146 ?
Sb O1 1.9748(9) 50_454 ?
Sb Ca 3.64715(7) 3_545 ?
Sb Na 3.64715(7) 2_554 ?
Sb Na 3.64715(7) 74_454 ?
Sb Na 3.64715(7) 3_545 ?
Sb Na 3.64715(7) 51_544 ?
Sb Na 3.64715(7) 4_455 ?
O1 Sb 1.9748(9) 27_544 ?
O1 Sb 1.9748(9) 50_454 ?
O1 Ca 2.5771(16) 52_455 ?
O1 Na 2.5771(16) 52_455 ?
O1 Ca 2.5771(16) 25_544 ?
O1 Na 2.5771(16) 25_544 ?
F2 Na 2.23341(4) 52_455 ?
F2 Ca 2.23341(4) 26_554 ?
F2 Ca 2.23341(4) 75_545 ?
F2 Ca 2.23341(4) 52_455 ?
F2 Na 2.23341(4) 26_554 ?
F2 Na 2.23341(4) 75_545 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
F2 Ca F2 180.0 97_666 . ?
F2 Ca O1 99.78(3) 97_666 177_556 ?
F2 Ca O1 80.22(4) . 177_556 ?
F2 Ca O1 80.22(4) 97_666 81 ?
F2 Ca O1 99.78(3) . 81 ?
O1 Ca O1 180.0 177_556 81 ?
F2 Ca O1 99.78(4) 97_666 149_565 ?
F2 Ca O1 80.22(4) . 149_565 ?
O1 Ca O1 117.18(2) 177_556 149_565 ?
O1 Ca O1 62.82(2) 81 149_565 ?
F2 Ca O1 80.22(4) 97_666 53 ?
F2 Ca O1 99.78(4) . 53 ?
O1 Ca O1 62.82(2) 177_556 53 ?
O1 Ca O1 117.18(2) 81 53 ?
O1 Ca O1 180.0 149_565 53 ?
F2 Ca O1 99.78(4) 97_666 121_655 ?
F2 Ca O1 80.22(4) . 121_655 ?
O1 Ca O1 117.18(2) 177_556 121_655 ?
O1 Ca O1 62.82(2) 81 121_655 ?
O1 Ca O1 117.18(2) 149_565 121_655 ?
O1 Ca O1 62.82(2) 53 121_655 ?
F2 Ca O1 80.22(4) 97_666 25 ?
F2 Ca O1 99.78(4) . 25 ?
O1 Ca O1 62.82(2) 177_556 25 ?
O1 Ca O1 117.18(2) 81 25 ?
O1 Ca O1 62.82(2) 149_565 25 ?
O1 Ca O1 117.18(2) 53 25 ?
O1 Ca O1 180.0 121_655 25 ?
F2 Ca Ca 144.7 97_666 26_554 ?
F2 Ca Ca 35.3 . 26_554 ?
O1 Ca Ca 44.96(4) 177_556 26_554 ?
O1 Ca Ca 135.04(4) 81 26_554 ?
O1 Ca Ca 98.39(3) 149_565 26_554 ?
O1 Ca Ca 81.61(3) 53 26_554 ?
O1 Ca Ca 98.39(3) 121_655 26_554 ?
O1 Ca Ca 81.61(3) 25 26_554 ?
F2 Ca Na 35.3 97_666 50_564 ?
F2 Ca Na 144.7 . 50_564 ?
O1 Ca Na 135.04(4) 177_556 50_564 ?
O1 Ca Na 44.96(4) 81 50_564 ?
O1 Ca Na 81.61(3) 149_565 50_564 ?
O1 Ca Na 98.39(3) 53 50_564 ?
O1 Ca Na 81.61(3) 121_655 50_564 ?
O1 Ca Na 98.39(3) 25 50_564 ?
Ca Ca Na 180.0 26_554 50_564 ?
F2 Ca Na 35.3 97_666 27_645 ?
F2 Ca Na 144.7 . 27_645 ?
O1 Ca Na 81.61(3) 177_556 27_645 ?
O1 Ca Na 98.39(3) 81 27_645 ?
O1 Ca Na 135.04(4) 149_565 27_645 ?
O1 Ca Na 44.96(4) 53 27_645 ?
O1 Ca Na 81.61(3) 121_655 27_645 ?
O1 Ca Na 98.39(3) 25 27_645 ?
Ca Ca Na 120.0 26_554 27_645 ?
Na Ca Na 60.0 50_564 27_645 ?
F2 Ca Na 144.7 97_666 75_545 ?
F2 Ca Na 35.3 . 75_545 ?
O1 Ca Na 98.39(3) 177_556 75_545 ?
O1 Ca Na 81.61(3) 81 75_545 ?
O1 Ca Na 44.96(4) 149_565 75_545 ?
O1 Ca Na 135.04(4) 53 75_545 ?
O1 Ca Na 98.39(3) 121_655 75_545 ?
O1 Ca Na 81.61(3) 25 75_545 ?
Ca Ca Na 60.0 26_554 75_545 ?
Na Ca Na 120.0 50_564 75_545 ?
Na Ca Na 180.0 27_645 75_545 ?
O1 Sb O1 180.00(12) 174 78_445 ?
O1 Sb O1 94.29(8) 174 130 ?
O1 Sb O1 85.71(8) 78_445 130 ?
O1 Sb O1 85.71(8) 174 34_544 ?
O1 Sb O1 94.29(8) 78_445 34_544 ?
O1 Sb O1 180.00(12) 130 34_544 ?
O1 Sb O1 94.29(8) 174 146 ?
O1 Sb O1 85.71(8) 78_445 146 ?
O1 Sb O1 94.29(8) 130 146 ?
O1 Sb O1 85.71(8) 34_544 146 ?
O1 Sb O1 85.71(8) 174 50_454 ?
O1 Sb O1 94.29(8) 78_445 50_454 ?
O1 Sb O1 85.71(8) 130 50_454 ?
O1 Sb O1 94.29(8) 34_544 50_454 ?
O1 Sb O1 180.00(12) 146 50_454 ?
O1 Sb Ca 90.0 174 3_545 ?
O1 Sb Ca 90.0 78_445 3_545 ?
O1 Sb Ca 42.85(4) 130 3_545 ?
O1 Sb Ca 137.15(4) 34_544 3_545 ?
O1 Sb Ca 137.15(4) 146 3_545 ?
O1 Sb Ca 42.85(4) 50_454 3_545 ?
O1 Sb Na 137.15(4) 174 2_554 ?
O1 Sb Na 42.85(4) 78_445 2_554 ?
O1 Sb Na 90.0 130 2_554 ?
O1 Sb Na 90.0 34_544 2_554 ?
O1 Sb Na 42.85(4) 146 2_554 ?
O1 Sb Na 137.15(4) 50_454 2_554 ?
Ca Sb Na 120.0 3_545 2_554 ?
O1 Sb Na 42.85(4) 174 74_454 ?
O1 Sb Na 137.15(4) 78_445 74_454 ?
O1 Sb Na 90.0 130 74_454 ?
O1 Sb Na 90.0 34_544 74_454 ?
O1 Sb Na 137.15(4) 146 74_454 ?
O1 Sb Na 42.85(4) 50_454 74_454 ?
Ca Sb Na 60.0 3_545 74_454 ?
Na Sb Na 180.0 2_554 74_454 ?
O1 Sb Na 90.0 174 3_545 ?
O1 Sb Na 90.0 78_445 3_545 ?
O1 Sb Na 42.85(4) 130 3_545 ?
O1 Sb Na 137.15(4) 34_544 3_545 ?
O1 Sb Na 137.15(4) 146 3_545 ?
O1 Sb Na 42.85(4) 50_454 3_545 ?
Ca Sb Na 0.0 3_545 3_545 ?
Na Sb Na 120.0 2_554 3_545 ?
Na Sb Na 60.0 74_454 3_545 ?
O1 Sb Na 90.0 174 51_544 ?
O1 Sb Na 90.0 78_445 51_544 ?
O1 Sb Na 137.15(4) 130 51_544 ?
O1 Sb Na 42.85(4) 34_544 51_544 ?
O1 Sb Na 42.85(4) 146 51_544 ?
O1 Sb Na 137.15(4) 50_454 51_544 ?
Ca Sb Na 180.0 3_545 51_544 ?
Na Sb Na 60.0 2_554 51_544 ?
Na Sb Na 120.0 74_454 51_544 ?
Na Sb Na 180.0 3_545 51_544 ?
O1 Sb Na 42.85(4) 174 4_455 ?
O1 Sb Na 137.15(4) 78_445 4_455 ?
O1 Sb Na 137.15(4) 130 4_455 ?
O1 Sb Na 42.85(4) 34_544 4_455 ?
O1 Sb Na 90.0 146 4_455 ?
O1 Sb Na 90.0 50_454 4_455 ?
Ca Sb Na 120.0 3_545 4_455 ?
Na Sb Na 120.0 2_554 4_455 ?
Na Sb Na 60.0 74_454 4_455 ?
Na Sb Na 120.0 3_545 4_455 ?
Na Sb Na 60.0 51_544 4_455 ?
Sb O1 Sb 134.86(12) 27_544 50_454 ?
Sb O1 Ca 105.74(3) 27_544 52_455 ?
Sb O1 Ca 105.74(3) 50_454 52_455 ?
Sb O1 Na 105.74(3) 27_544 52_455 ?
Sb O1 Na 105.74(3) 50_454 52_455 ?
Ca O1 Na 0.0 52_455 52_455 ?
Sb O1 Ca 105.74(3) 27_544 25_544 ?
Sb O1 Ca 105.74(3) 50_454 25_544 ?
Ca O1 Ca 90.08(7) 52_455 25_544 ?
Na O1 Ca 90.08(7) 52_455 25_544 ?
Sb O1 Na 105.74(3) 27_544 25_544 ?
Sb O1 Na 105.74(3) 50_454 25_544 ?
Ca O1 Na 90.08(7) 52_455 25_544 ?
Na O1 Na 90.08(7) 52_455 25_544 ?
Ca O1 Na 0.0 25_544 25_544 ?
Ca F2 Na 109.5 . 52_455 ?
Ca F2 Ca 109.5 . 26_554 ?
Na F2 Ca 109.5 52_455 26_554 ?
Ca F2 Ca 109.5 . 75_545 ?
Na F2 Ca 109.5 52_455 75_545 ?
Ca F2 Ca 109.5 26_554 75_545 ?
Ca F2 Ca 109.5 . 52_455 ?
Na F2 Ca 0.0 52_455 52_455 ?
Ca F2 Ca 109.5 26_554 52_455 ?
Ca F2 Ca 109.5 75_545 52_455 ?
Ca F2 Na 109.5 . 26_554 ?
Na F2 Na 109.5 52_455 26_554 ?
Ca F2 Na 0.0 26_554 26_554 ?
Ca F2 Na 109.5 75_545 26_554 ?
Ca F2 Na 109.5 52_455 26_554 ?
Ca F2 Na 109.5 . 75_545 ?
Na F2 Na 109.5 52_455 75_545 ?
Ca F2 Na 109.5 26_554 75_545 ?
Ca F2 Na 0.0 75_545 75_545 ?
Ca F2 Na 109.5 52_455 75_545 ?
Na F2 Na 109.5 26_554 75_545 ?
 
_refine_diff_density_max    0.444
_refine_diff_density_min   -0.444
_refine_diff_density_rms    0.104



