data_pale_g1
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'As0.25 Ca3 Mn2 Na0.25 O12 Si0.25 V3'
_chemical_formula_weight          606.44
 
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'
 'Ca'  'Ca'   0.2262   0.3064
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'V'  'V'   0.3005   0.5294
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mn'  'Mn'   0.3368   0.7283
 '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'
 'As'  'As'   0.0499   2.0058
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0817   0.0704
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            ?
_symmetry_space_group_name_H-M    ?
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 'z, x, y'
 'z+1/2, -x+1/2, -y'
 '-z+1/2, -x, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y, z, x'
 '-y, z+1/2, -x+1/2'
 'y+1/2, -z+1/2, -x'
 '-y+1/2, -z, x+1/2'
 'y+3/4, x+1/4, -z+1/4'
 '-y+3/4, -x+3/4, -z+3/4'
 'y+1/4, -x+1/4, z+3/4'
 '-y+1/4, x+3/4, z+1/4'
 'x+3/4, z+1/4, -y+1/4'
 '-x+1/4, z+3/4, y+1/4'
 '-x+3/4, -z+3/4, -y+3/4'
 'x+1/4, -z+1/4, y+3/4'
 'z+3/4, y+1/4, -x+1/4'
 'z+1/4, -y+1/4, x+3/4'
 '-z+1/4, y+3/4, x+1/4'
 '-z+3/4, -y+3/4, -x+3/4'
 'x+1/2, y+1/2, z+1/2'
 '-x+1, -y+1/2, z+1'
 '-x+1/2, y+1, -z+1'
 'x+1, -y+1, -z+1/2'
 'z+1/2, x+1/2, y+1/2'
 'z+1, -x+1, -y+1/2'
 '-z+1, -x+1/2, y+1'
 '-z+1/2, x+1, -y+1'
 'y+1/2, z+1/2, x+1/2'
 '-y+1/2, z+1, -x+1'
 'y+1, -z+1, -x+1/2'
 '-y+1, -z+1/2, x+1'
 'y+5/4, x+3/4, -z+3/4'
 '-y+5/4, -x+5/4, -z+5/4'
 'y+3/4, -x+3/4, z+5/4'
 '-y+3/4, x+5/4, z+3/4'
 'x+5/4, z+3/4, -y+3/4'
 '-x+3/4, z+5/4, y+3/4'
 '-x+5/4, -z+5/4, -y+5/4'
 'x+3/4, -z+3/4, y+5/4'
 'z+5/4, y+3/4, -x+3/4'
 'z+3/4, -y+3/4, x+5/4'
 '-z+3/4, y+5/4, x+3/4'
 '-z+5/4, -y+5/4, -x+5/4'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 '-z, -x, -y'
 '-z-1/2, x-1/2, y'
 'z-1/2, x, -y-1/2'
 'z, -x-1/2, y-1/2'
 '-y, -z, -x'
 'y, -z-1/2, x-1/2'
 '-y-1/2, z-1/2, x'
 'y-1/2, z, -x-1/2'
 '-y-3/4, -x-1/4, z-1/4'
 'y-3/4, x-3/4, z-3/4'
 '-y-1/4, x-1/4, -z-3/4'
 'y-1/4, -x-3/4, -z-1/4'
 '-x-3/4, -z-1/4, y-1/4'
 'x-1/4, -z-3/4, -y-1/4'
 'x-3/4, z-3/4, y-3/4'
 '-x-1/4, z-1/4, -y-3/4'
 '-z-3/4, -y-1/4, x-1/4'
 '-z-1/4, y-1/4, -x-3/4'
 'z-1/4, -y-3/4, -x-1/4'
 'z-3/4, y-3/4, x-3/4'
 '-x+1/2, -y+1/2, -z+1/2'
 'x, y+1/2, -z'
 'x+1/2, -y, z'
 '-x, y, z+1/2'
 '-z+1/2, -x+1/2, -y+1/2'
 '-z, x, y+1/2'
 'z, x+1/2, -y'
 'z+1/2, -x, y'
 '-y+1/2, -z+1/2, -x+1/2'
 'y+1/2, -z, x'
 '-y, z, x+1/2'
 'y, z+1/2, -x'
 '-y-1/4, -x+1/4, z+1/4'
 'y-1/4, x-1/4, z-1/4'
 '-y+1/4, x+1/4, -z-1/4'
 'y+1/4, -x-1/4, -z+1/4'
 '-x-1/4, -z+1/4, y+1/4'
 'x+1/4, -z-1/4, -y+1/4'
 'x-1/4, z-1/4, y-1/4'
 '-x+1/4, z+1/4, -y-1/4'
 '-z-1/4, -y+1/4, x+1/4'
 '-z+1/4, y+1/4, -x-1/4'
 'z+1/4, -y-1/4, -x+1/4'
 'z-1/4, y-1/4, x-1/4'
 
_cell_length_a                    12.5359(2)
_cell_length_b                    12.5359(2)
_cell_length_c                    12.5359(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1970.00(5)
_cell_formula_units_Z             8
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           0.05
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     4.089
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2316
_exptl_absorpt_coefficient_mu     7.741
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   0.7221
_exptl_absorpt_correction_T_max   0.9266
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             9095
_diffrn_reflns_av_R_equivalents   0.0404
_diffrn_reflns_av_sigmaI/netI     0.0183
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          3.98
_diffrn_reflns_theta_max          36.29
_reflns_number_total              406
_reflns_number_gt                 281
_reflns_threshold_expression      >2\s(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.2720P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          406
_refine_ls_number_parameters      19
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0396
_refine_ls_R_factor_gt            0.0242
_refine_ls_wR_factor_ref          0.0605
_refine_ls_wR_factor_gt           0.0548
_refine_ls_goodness_of_fit_ref    1.051
_refine_ls_restrained_S_all       1.051
_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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ca Ca 0.1250 0.0000 0.2500 0.01117(18) Uani 0.73 4 d SP . .
Na Na 0.1250 0.0000 0.2500 0.01117(18) Uani 0.27 4 d SP . .
V V 0.3750 0.0000 0.2500 0.00635(13) Uani 0.900(5) 4 d SP . .
As As 0.3750 0.0000 0.2500 0.00635(13) Uani 0.044(5) 4 d SP . .
Si Si 0.3750 0.0000 0.2500 0.00635(13) Uani 0.06 4 d SP . .
Mn Mn 0.0000 0.0000 0.0000 0.00949(16) Uani 0.989(3) 6 d SP . .
O O 0.03924(7) 0.05418(7) 0.65829(6) 0.0118(2) Uani 1 1 d . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Ca 0.0087(3) 0.0124(2) 0.0124(2) 0.00158(19) 0.000 0.000
Na 0.0087(3) 0.0124(2) 0.0124(2) 0.00158(19) 0.000 0.000
V 0.0056(2) 0.00672(15) 0.00672(15) 0.000 0.000 0.000
As 0.0056(2) 0.00672(15) 0.00672(15) 0.000 0.000 0.000
Si 0.0056(2) 0.00672(15) 0.00672(15) 0.000 0.000 0.000
Mn 0.00949(16) 0.00949(16) 0.00949(16) -0.00060(9) -0.00060(9) -0.00060(9)
O 0.0126(5) 0.0126(4) 0.0104(4) -0.0006(3) -0.0006(3) -0.0001(3)
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O 2.4540(9) 76_554 ?
Ca O 2.4540(9) 49_556 ?
Ca O 2.4540(9) 67_656 ?
Ca O 2.4540(9) 90_565 ?
Ca O 2.5381(8) 70_656 ?
Ca O 2.5381(8) 55_556 ?
Ca O 2.5381(8) 80_455 ?
Ca O 2.5381(8) 93_655 ?
Ca V 3.1340 . ?
Ca Si 3.1340 50_556 ?
V O 1.7143(8) 27_545 ?
V O 1.7143(8) 90_565 ?
V O 1.7143(8) 2_554 ?
V O 1.7143(8) 67_656 ?
V Na 3.1340 50_656 ?
V Ca 3.1340 50_656 ?
Mn O 2.1542(8) 36_454 ?
Mn O 2.1542(8) 32_544 ?
Mn O 2.1542(8) 28_445 ?
Mn O 2.1542(8) 84_545 ?
Mn O 2.1542(8) 80_455 ?
Mn O 2.1542(8) 76_554 ?
Mn Ca 3.5039 5 ?
Mn Ca 3.5039 57 ?
Mn Na 3.5039 49 ?
Mn Na 3.5039 5 ?
Mn Na 3.5039 53 ?
Mn Na 3.5039 9 ?
O Si 1.7143(8) 2 ?
O As 1.7143(8) 2 ?
O V 1.7143(8) 2 ?
O Mn 2.1542(8) 28_445 ?
O Ca 2.4540(9) 49_556 ?
O Na 2.4540(9) 49_556 ?
O Na 2.5381(8) 58_566 ?
O Ca 2.5381(8) 58_566 ?
 
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
O Ca O 65.93(4) 76_554 49_556 ?
O Ca O 164.42(4) 76_554 67_656 ?
O Ca O 116.40(4) 49_556 67_656 ?
O Ca O 116.40(4) 76_554 90_565 ?
O Ca O 164.42(4) 49_556 90_565 ?
O Ca O 65.93(4) 67_656 90_565 ?
O Ca O 92.23(2) 76_554 70_656 ?
O Ca O 71.65(3) 49_556 70_656 ?
O Ca O 74.84(4) 67_656 70_656 ?
O Ca O 122.507(18) 90_565 70_656 ?
O Ca O 122.507(18) 76_554 55_556 ?
O Ca O 74.84(4) 49_556 55_556 ?
O Ca O 71.65(3) 67_656 55_556 ?
O Ca O 92.23(2) 90_565 55_556 ?
O Ca O 113.70(4) 70_656 55_556 ?
O Ca O 74.84(4) 76_554 80_455 ?
O Ca O 122.507(18) 49_556 80_455 ?
O Ca O 92.23(2) 67_656 80_455 ?
O Ca O 71.65(3) 90_565 80_455 ?
O Ca O 69.64(4) 70_656 80_455 ?
O Ca O 161.07(4) 55_556 80_455 ?
O Ca O 71.65(3) 76_554 93_655 ?
O Ca O 92.23(2) 49_556 93_655 ?
O Ca O 122.507(18) 67_656 93_655 ?
O Ca O 74.84(4) 90_565 93_655 ?
O Ca O 161.07(4) 70_656 93_655 ?
O Ca O 69.64(4) 55_556 93_655 ?
O Ca O 113.70(4) 80_455 93_655 ?
O Ca V 147.035(19) 76_554 . ?
O Ca V 147.035(19) 49_556 . ?
O Ca V 32.965(19) 67_656 . ?
O Ca V 32.965(19) 90_565 . ?
O Ca V 99.463(18) 70_656 . ?
O Ca V 80.537(18) 55_556 . ?
O Ca V 80.537(18) 80_455 . ?
O Ca V 99.463(18) 93_655 . ?
O Ca Si 32.965(19) 76_554 50_556 ?
O Ca Si 32.965(19) 49_556 50_556 ?
O Ca Si 147.035(19) 67_656 50_556 ?
O Ca Si 147.035(19) 90_565 50_556 ?
O Ca Si 80.537(18) 70_656 50_556 ?
O Ca Si 99.463(18) 55_556 50_556 ?
O Ca Si 99.463(18) 80_455 50_556 ?
O Ca Si 80.537(18) 93_655 50_556 ?
V Ca Si 180.0 . 50_556 ?
O V O 113.16(3) 27_545 90_565 ?
O V O 102.33(6) 27_545 2_554 ?
O V O 113.16(3) 90_565 2_554 ?
O V O 113.16(3) 27_545 67_656 ?
O V O 102.33(6) 90_565 67_656 ?
O V O 113.16(3) 2_554 67_656 ?
O V Na 51.16(3) 27_545 50_656 ?
O V Na 128.84(3) 90_565 50_656 ?
O V Na 51.16(3) 2_554 50_656 ?
O V Na 128.84(3) 67_656 50_656 ?
O V Ca 51.16(3) 27_545 50_656 ?
O V Ca 128.84(3) 90_565 50_656 ?
O V Ca 51.16(3) 2_554 50_656 ?
O V Ca 128.84(3) 67_656 50_656 ?
Na V Ca 0.0 50_656 50_656 ?
O V Ca 128.84(3) 27_545 . ?
O V Ca 51.16(3) 90_565 . ?
O V Ca 128.84(3) 2_554 . ?
O V Ca 51.16(3) 67_656 . ?
Na V Ca 180.0 50_656 . ?
Ca V Ca 180.0 50_656 . ?
O Mn O 89.54(3) 36_454 32_544 ?
O Mn O 89.54(3) 36_454 28_445 ?
O Mn O 89.54(3) 32_544 28_445 ?
O Mn O 180.00(5) 36_454 84_545 ?
O Mn O 90.46(3) 32_544 84_545 ?
O Mn O 90.46(3) 28_445 84_545 ?
O Mn O 90.46(3) 36_454 80_455 ?
O Mn O 180.00(7) 32_544 80_455 ?
O Mn O 90.46(3) 28_445 80_455 ?
O Mn O 89.54(3) 84_545 80_455 ?
O Mn O 90.46(3) 36_454 76_554 ?
O Mn O 90.46(3) 32_544 76_554 ?
O Mn O 180.00(5) 28_445 76_554 ?
O Mn O 89.54(3) 84_545 76_554 ?
O Mn O 89.54(3) 80_455 76_554 ?
O Mn Ca 133.94(2) 36_454 5 ?
O Mn Ca 136.20(2) 32_544 5 ?
O Mn Ca 86.37(2) 28_445 5 ?
O Mn Ca 46.06(2) 84_545 5 ?
O Mn Ca 43.80(2) 80_455 5 ?
O Mn Ca 93.63(2) 76_554 5 ?
O Mn Ca 43.80(2) 36_454 57 ?
O Mn Ca 93.63(2) 32_544 57 ?
O Mn Ca 46.06(2) 28_445 57 ?
O Mn Ca 136.20(2) 84_545 57 ?
O Mn Ca 86.37(2) 80_455 57 ?
O Mn Ca 133.94(2) 76_554 57 ?
Ca Mn Ca 113.6 5 57 ?
O Mn Na 93.63(2) 36_454 49 ?
O Mn Na 46.06(2) 32_544 49 ?
O Mn Na 43.80(2) 28_445 49 ?
O Mn Na 86.37(2) 84_545 49 ?
O Mn Na 133.94(2) 80_455 49 ?
O Mn Na 136.20(2) 76_554 49 ?
Ca Mn Na 113.6 5 49 ?
Ca Mn Na 66.4 57 49 ?
O Mn Na 133.94(2) 36_454 5 ?
O Mn Na 136.20(2) 32_544 5 ?
O Mn Na 86.37(2) 28_445 5 ?
O Mn Na 46.06(2) 84_545 5 ?
O Mn Na 43.80(2) 80_455 5 ?
O Mn Na 93.63(2) 76_554 5 ?
Ca Mn Na 0.0 5 5 ?
Ca Mn Na 113.6 57 5 ?
Na Mn Na 113.6 49 5 ?
O Mn Na 46.06(2) 36_454 53 ?
O Mn Na 43.80(2) 32_544 53 ?
O Mn Na 93.63(2) 28_445 53 ?
O Mn Na 133.94(2) 84_545 53 ?
O Mn Na 136.20(2) 80_455 53 ?
O Mn Na 86.37(2) 76_554 53 ?
Ca Mn Na 180.0 5 53 ?
Ca Mn Na 66.4 57 53 ?
Na Mn Na 66.4 49 53 ?
Na Mn Na 180.0 5 53 ?
O Mn Na 136.20(2) 36_454 9 ?
O Mn Na 86.37(2) 32_544 9 ?
O Mn Na 133.94(2) 28_445 9 ?
O Mn Na 43.80(2) 84_545 9 ?
O Mn Na 93.63(2) 80_455 9 ?
O Mn Na 46.06(2) 76_554 9 ?
Ca Mn Na 66.4 5 9 ?
Ca Mn Na 180.0 57 9 ?
Na Mn Na 113.6 49 9 ?
Na Mn Na 66.4 5 9 ?
Na Mn Na 113.6 53 9 ?
Si O As 0.0 2 2 ?
Si O V 0.0 2 2 ?
As O V 0.0 2 2 ?
Si O Mn 129.50(4) 2 28_445 ?
As O Mn 129.50(4) 2 28_445 ?
V O Mn 129.50(4) 2 28_445 ?
Si O Ca 95.87(4) 2 49_556 ?
As O Ca 95.87(4) 2 49_556 ?
V O Ca 95.87(4) 2 49_556 ?
Mn O Ca 98.78(3) 28_445 49_556 ?
Si O Na 95.87(4) 2 49_556 ?
As O Na 95.87(4) 2 49_556 ?
V O Na 95.87(4) 2 49_556 ?
Mn O Na 98.78(3) 28_445 49_556 ?
Ca O Na 0.0 49_556 49_556 ?
Si O Na 127.95(4) 2 58_566 ?
As O Na 127.95(4) 2 58_566 ?
V O Na 127.95(4) 2 58_566 ?
Mn O Na 96.27(3) 28_445 58_566 ?
Ca O Na 100.49(3) 49_556 58_566 ?
Na O Na 100.49(3) 49_556 58_566 ?
Si O Ca 127.95(4) 2 58_566 ?
As O Ca 127.95(4) 2 58_566 ?
V O Ca 127.95(4) 2 58_566 ?
Mn O Ca 96.27(3) 28_445 58_566 ?
Ca O Ca 100.49(3) 49_556 58_566 ?
Na O Ca 100.49(3) 49_556 58_566 ?
Na O Ca 0.0 58_566 58_566 ?
 
_diffrn_measured_fraction_theta_max    1.000
_diffrn_reflns_theta_full              36.29
_diffrn_measured_fraction_theta_full   1.000
_refine_diff_density_max    0.338
_refine_diff_density_min   -0.812
_refine_diff_density_rms    0.126