data_calcioancylite-(La)

_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number       '2018/3'
_chemical_name_common              'calcioancylite-(La)'
_chemical_compound_source         'Gejiu, China'
_chemical_formula_moiety           'C2 Ca0.677 La1.323 O8'
_chemical_formula_sum              'C2 Ca0.67 La1.32 O8'
_chemical_formula_weight           363.13
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca' 'Ca' 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'La' 'La' -1.4094 9.0376
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'orthorhombic'
_space_group_IT_number             62
_space_group_name_H-M_alt          'P m c n'
_space_group_name_Hall             '-P 2n 2a'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y, -z'
 '-x+1/2, -y+1/2, z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y, z'
 'x-1/2, y-1/2, -z-1/2'

_cell_length_a                     5.0253(3)
_cell_length_b                     8.5152(6)
_cell_length_c                     7.2717(6)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       311.17(4)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      663
_cell_measurement_temperature      296.15
_cell_measurement_theta_max        76.5810
_cell_measurement_theta_min        5.2190
_shelx_estimated_absorpt_T_max     0.050
_shelx_estimated_absorpt_T_min     0.050
_exptl_absorpt_coefficient_mu      74.967
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.37165
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     ?
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      3.876
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description        plate
_exptl_crystal_F_000               330
_exptl_crystal_size_max            0.016
_exptl_crystal_size_mid            0.007
_exptl_crystal_size_min            0.005
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0526
_diffrn_reflns_av_unetI/netI       0.0494
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.973
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -6
_diffrn_reflns_limit_k_max         10
_diffrn_reflns_limit_k_min         -10
_diffrn_reflns_limit_l_max         7
_diffrn_reflns_limit_l_min         -9
_diffrn_reflns_number              1054
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.973
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           76.790
_diffrn_reflns_theta_min           8.014
_diffrn_ambient_temperature        296.15
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.973
_diffrn_measurement_device_type    'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  347
_reflns_number_total               360
_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.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection         'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction          'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics      'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      ?
_refine_diff_density_max           1.990
_refine_diff_density_min           -1.802
_refine_diff_density_rms           0.368
_refine_ls_extinction_coef         0.0055(15)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.259
_refine_ls_hydrogen_treatment      undef
_refine_ls_matrix_type             full
_refine_ls_number_parameters       36
_refine_ls_number_reflns           360
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0679
_refine_ls_R_factor_gt             0.0652
_refine_ls_restrained_S_all        1.259
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0434P)²+16.7795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1535
_refine_ls_wR_factor_ref           0.1551
_refine_special_details            ?
_olex2_refinement_description
;
1. Shared sites
{Ca, La}
2. Uiso/Uaniso restraints and constraints
Uanis(La) = Uanis(Ca)
Uanis(Ca) = Uanis(La)
3. Others
 Sof(La)=0.5*(1-FVAR(2))
 Sof(Ca)=0.5*FVAR(2)
;
_atom_sites_solution_hydrogens     .
_atom_sites_solution_primary       ?
_atom_sites_solution_secondary     ?
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
 La La 0.750000 0.66003(18) 0.8522(2) 0.0174(7) Uani 0.66(4) 2 d S T P A 8
 Ca Ca 0.750000 0.66003(18) 0.8522(2) 0.0174(7) Uani 0.34(4) 2 d S T P A 7
 C C 0.250000 0.811(2) 0.687(3) 0.016(4) Uani 1 2 d S T P A .
 O1 O 0.250000 0.681(2) 0.777(3) 0.032(4) Uani 1 2 d S T P . .
 O2 O 0.472(3) 0.8784(13) 0.6465(15) 0.029(3) Uani 1 1 d . . . . .
 O3 O 0.750000 0.586(2) 0.524(2) 0.036(5) Uani 1 2 d S T P . .

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
 La 0.0137(9) 0.0210(10) 0.0175(9) -0.0009(6) 0.000 0.000
 Ca 0.0137(9) 0.0210(10) 0.0175(9) -0.0009(6) 0.000 0.000
 C 0.010(8) 0.015(9) 0.022(10) 0.004(8) 0.000 0.000
 O1 0.028(9) 0.033(9) 0.036(10) 0.012(8) 0.000 0.000
 O2 0.029(6) 0.035(6) 0.022(6) -0.005(5) 0.002(5) -0.004(5)
 O3 0.049(11) 0.042(10) 0.018(8) 0.017(7) 0.000 0.000

_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
 La O1 2.577(4) . ?
 La O1 2.577(4) 1_655 ?
 La O2 2.576(11) 4_665 ?
 La O2 2.576(11) 6_576 ?
 La O2 2.765(12) 7_755 ?
 La O2 2.765(12) . ?
 La O2 2.645(12) 8_657 ?
 La O2 2.645(12) 2_646 ?
 La O3 2.496(17) 6_576 ?
 La O3 2.465(17) . ?
 Ca O1 2.577(4) . ?
 Ca O1 2.577(4) 1_655 ?
 Ca O2 2.576(11) 4_665 ?
 Ca O2 2.765(12) . ?
 Ca O2 2.765(12) 7_755 ?
 Ca O2 2.576(11) 6_576 ?
 Ca O2 2.645(12) 2_646 ?
 Ca O2 2.645(12) 8_657 ?
 Ca O3 2.465(17) . ?
 Ca O3 2.496(17) 6_576 ?
 C O1 1.28(3) . ?
 C O2 1.290(15) . ?
 C O2 1.290(15) 7_655 ?

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
 O1 La O1 154.3(8) . 1_655 ?
 O1 La O2 109.3(4) . 7_755 ?
 O1 La O2 49.2(4) . . ?
 O1 La O2 69.7(5) . 2_646 ?
 O1 La O2 49.2(4) 1_655 7_755 ?
 O1 La O2 118.4(5) 1_655 2_646 ?
 O1 La O2 109.3(5) 1_655 . ?
 O1 La O2 118.4(5) . 8_657 ?
 O1 La O2 69.7(5) 1_655 8_657 ?
 O2 La O1 69.9(5) 6_576 . ?
 O2 La O1 135.5(5) 4_665 . ?
 O2 La O1 69.9(5) 4_665 1_655 ?
 O2 La O1 135.5(5) 6_576 1_655 ?
 O2 La O2 113.49(12) 2_646 . ?
 O2 La O2 145.6(2) 2_646 7_755 ?
 O2 La O2 144.0(2) 4_665 . ?
 O2 La O2 96.3(3) 4_665 2_646 ?
 O2 La O2 144.0(2) 6_576 7_755 ?
 O2 La O2 69.7(4) 6_576 2_646 ?
 O2 La O2 65.6(5) 4_665 6_576 ?
 O2 La O2 69.7(4) 4_665 8_657 ?
 O2 La O2 113.49(13) 8_657 7_755 ?
 O2 La O2 96.3(3) 6_576 8_657 ?
 O2 La O2 105.1(4) 6_576 . ?
 O2 La O2 60.7(5) 7_755 . ?
 O2 La O2 145.6(2) 8_657 . ?
 O2 La O2 105.1(4) 4_665 7_755 ?
 O2 La O2 49.9(5) 2_646 8_657 ?
 O3 La O1 92.6(4) 6_576 1_655 ?
 O3 La O1 79.2(4) . . ?
 O3 La O1 92.6(4) 6_576 . ?
 O3 La O1 79.2(4) . 1_655 ?
 O3 La O2 141.5(4) 6_576 2_646 ?
 O3 La O2 140.4(3) . 4_665 ?
 O3 La O2 71.9(4) 6_576 7_755 ?
 O3 La O2 72.1(4) 6_576 4_665 ?
 O3 La O2 140.4(4) . 6_576 ?
 O3 La O2 141.5(4) 6_576 8_657 ?
 O3 La O2 76.9(4) . 8_657 ?
 O3 La O2 76.9(4) . 2_646 ?
 O3 La O2 69.4(4) . 7_755 ?
 O3 La O2 69.4(4) . . ?
 O3 La O2 71.9(4) 6_576 . ?
 O3 La O2 72.1(4) 6_576 6_576 ?
 O3 La O3 134.8(4) . 6_576 ?
 O1 Ca O1 154.3(8) . 1_655 ?
 O1 Ca O2 49.2(4) 1_655 7_755 ?
 O1 Ca O2 109.3(5) 1_655 . ?
 O1 Ca O2 69.7(5) . 2_646 ?
 O1 Ca O2 118.4(5) 1_655 2_646 ?
 O1 Ca O2 49.2(4) . . ?
 O1 Ca O2 118.4(5) . 8_657 ?
 O1 Ca O2 69.7(5) 1_655 8_657 ?
 O1 Ca O2 109.3(4) . 7_755 ?
 O2 Ca O1 69.9(5) 4_665 1_655 ?
 O2 Ca O1 135.5(5) 4_665 . ?
 O2 Ca O1 135.5(5) 6_576 1_655 ?
 O2 Ca O1 69.9(5) 6_576 . ?
 O2 Ca O2 113.49(12) 2_646 . ?
 O2 Ca O2 144.0(2) 4_665 . ?
 O2 Ca O2 145.6(2) 2_646 7_755 ?
 O2 Ca O2 69.7(4) 6_576 2_646 ?
 O2 Ca O2 60.7(5) 7_755 . ?
 O2 Ca O2 96.3(3) 4_665 2_646 ?
 O2 Ca O2 113.49(13) 8_657 7_755 ?
 O2 Ca O2 96.3(3) 6_576 8_657 ?
 O2 Ca O2 105.1(4) 6_576 . ?
 O2 Ca O2 65.6(5) 4_665 6_576 ?
 O2 Ca O2 69.7(4) 4_665 8_657 ?
 O2 Ca O2 105.1(4) 4_665 7_755 ?
 O2 Ca O2 145.6(2) 8_657 . ?
 O2 Ca O2 144.0(2) 6_576 7_755 ?
 O2 Ca O2 49.9(5) 2_646 8_657 ?
 O3 Ca O1 92.6(4) 6_576 . ?
 O3 Ca O1 92.6(4) 6_576 1_655 ?
 O3 Ca O1 79.2(4) . 1_655 ?
 O3 Ca O1 79.2(4) . . ?
 O3 Ca O2 76.9(4) . 8_657 ?
 O3 Ca O2 140.4(3) . 4_665 ?
 O3 Ca O2 72.1(4) 6_576 6_576 ?
 O3 Ca O2 141.5(4) 6_576 8_657 ?
 O3 Ca O2 141.5(4) 6_576 2_646 ?
 O3 Ca O2 72.1(4) 6_576 4_665 ?
 O3 Ca O2 140.4(4) . 6_576 ?
 O3 Ca O2 71.9(4) 6_576 7_755 ?
 O3 Ca O2 76.9(4) . 2_646 ?
 O3 Ca O2 69.4(4) . . ?
 O3 Ca O2 71.9(4) 6_576 . ?
 O3 Ca O2 69.4(4) . 7_755 ?
 O3 Ca O3 134.8(4) . 6_576 ?
 O1 C O2 120.0(9) . . ?
 O1 C O2 120.0(9) . 7_655 ?
 O2 C O2 119.9(18) . 7_655 ?
 C O1 La 167.9(14) . 5_667 ?
 C O1 La 99.7(4) . . ?
 C O1 La 99.7(4) . 1_455 ?
 C O1 Ca 99.7(4) . . ?
 La O2 La 145.2(4) 2_656 . ?
 La O2 La 95.2(4) 6_575 . ?
 C O2 La 127.0(12) . 6_575 ?
 C O2 La 90.8(9) . . ?
 C O2 La 92.2(10) . 2_656 ?
 C O2 Ca 90.8(9) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O1 C O2 La -151.1(18) . . . 2_656 ?
 O1 C O2 La 91(2) . . . 6_575 ?
 O1 C O2 La -5.8(19) . . . . ?
 O1 C O2 Ca -5.8(19) . . . . ?
 O2 C O1 La -169.4(16) 7_655 . . . ?
 O2 C O1 La 6(2) . . . . ?
 O2 C O1 La 169.4(16) . . . 1_455 ?
 O2 C O1 La -6(2) 7_655 . . 1_455 ?
 O2 C O1 La 87.9(18) . . . 5_667 ?
 O2 C O1 La -87.9(18) 7_655 . . 5_667 ?
 O2 C O1 Ca 6(2) . . . . ?
 O2 C O1 Ca -169.4(16) 7_655 . . . ?
 O2 C O2 La -93(2) 7_655 . . 6_575 ?
 O2 C O2 La 25(2) 7_655 . . 2_656 ?
 O2 C O2 La 169.9(17) 7_655 . . . ?
 O2 C O2 Ca 169.9(17) 7_655 . . . ?


