# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2132681'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.291 La0.709'
_chemical_formula_sum            'Bi3 Ca3.29 La0.71'
_chemical_formula_weight         857.43
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
La La -0.2871 2.4523 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.6653(6)
_cell_length_b                   9.6653(6)
_cell_length_c                   9.6653(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     902.91(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1003
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      30.10
_cell_measurement_theta_min      5.17
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    63.363
_exptl_absorpt_correction_T_max  0.2655
_exptl_absorpt_correction_T_min  0.0785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.2005 before and 0.0829 after correction.
The Ratio of minimum to maximum transmission is 0.2957.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.308
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1421
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.019
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1720
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.451
_diffrn_reflns_theta_min         5.167
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                218
_reflns_number_total             230
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.129
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.348
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_coef       0.0020(3)
_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   1.064
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0281
_refine_ls_restrained_S_all      1.064
_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)+(0.0279P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0623
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.95(4)
 0.05(4)
2. Shared sites
{Ca02, La02}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca02) = Uanis(La02)
4. Others
 Sof(La02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi01 Bi 0.375000 0.000000 0.250000 0.0087(4) Uani 1 4 d S T P . .
Ca02 Ca 0.0720(2) 0.0720(2) 0.0720(2) 0.0110(13) Uani 0.823(13) 3 d S T P . 1
La02 La 0.0720(2) 0.0720(2) 0.0720(2) 0.0110(13) Uani 0.177(13) 3 d S T P . 2


_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
Bi01 Ca02 3.230(2) 39_444 ?
Bi01 Ca02 3.468(2) 28_445 ?
Bi01 Ca02 3.468(2) 16_545 ?
Bi01 Ca02 3.468(2) 38_544 ?
Bi01 Ca02 3.230(2) 2 ?
Bi01 Ca02 3.468(2) . ?
Bi01 Ca02 3.230(2) 13 ?
Bi01 Ca02 3.230(2) 27_544 ?
Bi01 La02 3.468(2) . ?
Ca02 Ca02 3.712(2) 27_544 ?
Ca02 Ca02 4.1852(3) 37_444 ?
Ca02 Ca02 4.1852(3) 13 ?
Ca02 Ca02 3.712(2) 26_454 ?
Ca02 Ca02 3.712(2) 28_445 ?

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
Ca02 Bi01 Ca02 161.73(8) 39_444 13 ?
Ca02 Bi01 Ca02 87.27(6) 2 16_545 ?
Ca02 Bi01 Ca02 67.21(4) 2 28_445 ?
Ca02 Bi01 Ca02 130.95(4) 13 16_545 ?
Ca02 Bi01 Ca02 77.263(6) 39_444 28_445 ?
Ca02 Bi01 Ca02 135.520(3) 38_544 . ?
Ca02 Bi01 Ca02 67.21(4) 39_444 16_545 ?
Ca02 Bi01 Ca02 91.444(13) 39_444 2 ?
Ca02 Bi01 Ca02 64.724(4) 38_544 16_545 ?
Ca02 Bi01 Ca02 87.27(6) 39_444 . ?
Ca02 Bi01 Ca02 87.27(6) 13 28_445 ?
Ca02 Bi01 Ca02 91.444(13) 13 2 ?
Ca02 Bi01 Ca02 135.520(3) 28_445 16_545 ?
Ca02 Bi01 Ca02 135.520(3) 38_544 28_445 ?
Ca02 Bi01 Ca02 67.21(4) 13 38_544 ?
Ca02 Bi01 Ca02 91.444(13) 39_444 27_544 ?
Ca02 Bi01 Ca02 77.263(6) 2 38_544 ?
Ca02 Bi01 Ca02 77.263(6) 27_544 16_545 ?
Ca02 Bi01 Ca02 87.27(6) 27_544 38_544 ?
Ca02 Bi01 Ca02 91.444(13) 13 27_544 ?
Ca02 Bi01 Ca02 67.21(4) 27_544 . ?
Ca02 Bi01 Ca02 130.95(4) 2 . ?
Ca02 Bi01 Ca02 64.724(4) 28_445 . ?
Ca02 Bi01 Ca02 161.73(8) 2 27_544 ?
Ca02 Bi01 Ca02 130.95(4) 27_544 28_445 ?
Ca02 Bi01 Ca02 135.520(3) 16_545 . ?
Ca02 Bi01 Ca02 130.95(4) 39_444 38_544 ?
Ca02 Bi01 Ca02 77.263(6) 13 . ?
Bi01 Ca02 Bi01 88.83(7) 6_455 2_554 ?
Bi01 Ca02 Bi01 84.829(6) 2_554 5 ?
Bi01 Ca02 Bi01 162.29(3) 6_455 . ?
Bi01 Ca02 Bi01 81.36(6) 5 . ?
Bi01 Ca02 Bi01 162.29(3) 10_545 5 ?
Bi01 Ca02 Bi01 81.36(6) 5 9 ?
Bi01 Ca02 Bi01 84.829(6) 6_455 9 ?
Bi01 Ca02 Bi01 88.83(7) 6_455 10_545 ?
Bi01 Ca02 Bi01 107.511(7) 10_545 9 ?
Bi01 Ca02 Bi01 162.29(3) 2_554 9 ?
Bi01 Ca02 Bi01 81.36(6) . 9 ?
Bi01 Ca02 Bi01 88.83(7) 2_554 10_545 ?
Bi01 Ca02 Bi01 107.511(7) 2_554 . ?
Bi01 Ca02 Bi01 84.829(6) 10_545 . ?
Bi01 Ca02 Bi01 107.511(7) 6_455 5 ?
Bi01 Ca02 Ca02 144.35(9) 6_455 27_544 ?
Bi01 Ca02 Ca02 53.33(7) 5 26_454 ?
Bi01 Ca02 Ca02 144.35(9) 2_554 28_445 ?
Bi01 Ca02 Ca02 53.33(7) 9 28_445 ?
Bi01 Ca02 Ca02 57.638(2) 9 26_454 ?
Bi01 Ca02 Ca02 126.09(5) 2_554 13 ?
Bi01 Ca02 Ca02 120.16(10) 9 27_544 ?
Bi01 Ca02 Ca02 59.45(3) 2_554 27_544 ?
Bi01 Ca02 Ca02 120.16(10) . 26_454 ?
Bi01 Ca02 Ca02 131.18(4) 5 37_444 ?
Bi01 Ca02 Ca02 105.020(15) 6_455 28_445 ?
Bi01 Ca02 Ca02 48.82(4) 9 13 ?
Bi01 Ca02 Ca02 59.45(3) 10_545 28_445 ?
Bi01 Ca02 Ca02 57.638(2) 5 27_544 ?
Bi01 Ca02 Ca02 53.91(5) 6_455 37_444 ?
Bi01 Ca02 Ca02 53.91(5) 2_554 37_444 ?
Bi01 Ca02 Ca02 53.91(5) 10_545 37_444 ?
Bi01 Ca02 Ca02 53.33(7) . 27_544 ?
Bi01 Ca02 Ca02 131.18(4) . 37_444 ?
Bi01 Ca02 Ca02 131.18(4) 9 37_444 ?
Bi01 Ca02 Ca02 126.09(5) 6_455 13 ?
Bi01 Ca02 Ca02 59.45(3) 6_455 26_454 ?
Bi01 Ca02 Ca02 126.09(5) 10_545 13 ?
Bi01 Ca02 Ca02 48.82(4) 5 13 ?
Bi01 Ca02 Ca02 48.82(4) . 13 ?
Bi01 Ca02 Ca02 105.020(15) 2_554 26_454 ?
Bi01 Ca02 Ca02 120.16(10) 5 28_445 ?
Bi01 Ca02 Ca02 57.638(2) . 28_445 ?
Bi01 Ca02 Ca02 144.35(9) 10_545 26_454 ?
Bi01 Ca02 Ca02 105.020(15) 10_545 27_544 ?
Ca02 Ca02 Ca02 110.33(6) 27_544 28_445 ?
Ca02 Ca02 Ca02 108.60(6) 26_454 37_444 ?
Ca02 Ca02 Ca02 71.40(6) 28_445 13 ?
Ca02 Ca02 Ca02 108.60(6) 28_445 37_444 ?
Ca02 Ca02 Ca02 110.33(6) 27_544 26_454 ?
Ca02 Ca02 Ca02 71.40(6) 26_454 13 ?
Ca02 Ca02 Ca02 108.60(6) 27_544 37_444 ?
Ca02 Ca02 Ca02 110.33(6) 26_454 28_445 ?
Ca02 Ca02 Ca02 71.40(6) 27_544 13 ?
Ca02 Ca02 Ca02 180.0(2) 37_444 13 ?
Bi01 La02 Bi01 162.29(3) 2_554 9 ?
Bi01 La02 Bi01 81.36(6) 5 . ?
Bi01 La02 Bi01 107.511(7) 2_554 . ?
Bi01 La02 Bi01 81.36(6) 5 9 ?
Bi01 La02 Bi01 81.36(6) . 9 ?
Bi01 La02 Bi01 88.83(7) 2_554 10_545 ?
Bi01 La02 Bi01 107.511(7) 6_455 5 ?
Bi01 La02 Bi01 107.511(7) 10_545 9 ?
Bi01 La02 Bi01 84.829(6) 2_554 5 ?
Bi01 La02 Bi01 162.29(3) 10_545 5 ?
Bi01 La02 Bi01 88.83(7) 6_455 2_554 ?
Bi01 La02 Bi01 84.829(6) 6_455 9 ?
Bi01 La02 Bi01 88.83(7) 6_455 10_545 ?
Bi01 La02 Bi01 84.829(6) 10_545 . ?
Bi01 La02 Bi01 162.29(3) 6_455 . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.95(4)
2 0.05(4)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2132683'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.345 Pr0.655'
_chemical_formula_sum            'Bi3 Ca3.35 Pr0.65'
_chemical_formula_weight         853.30
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Pr Pr -0.2180 2.8214 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.6228(5)
_cell_length_b                   9.6228(5)
_cell_length_c                   9.6228(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     891.05(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    991
_cell_measurement_temperature    200.01
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      5.19
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    64.422
_exptl_absorpt_correction_T_max  0.2652
_exptl_absorpt_correction_T_min  0.1139
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1398 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.4295.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1418
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1728
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.242
_diffrn_reflns_theta_min         5.190
_diffrn_ambient_temperature      200.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                214
_reflns_number_total             224
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.233
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(3)
_refine_ls_extinction_coef       0.0032(3)
_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   1.080
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0193
_refine_ls_restrained_S_all      1.080
_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)+(0.0130P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0394
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.42(3)
 0.58(3)
2. Shared sites
{Ca02, Pr02}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca02) = Uanis(Pr02)
4. Others
 Sof(Pr02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi01 Bi 0.375000 0.000000 0.250000 0.0068(3) Uani 1 4 d S T P . .
Ca02 Ca 0.07209(14) 0.07209(14) 0.07209(14) 0.0067(9) Uani 0.836(8) 3 d S T P .
1
Pr02 Pr 0.07209(14) 0.07209(14) 0.07209(14) 0.0067(9) Uani 0.164(8) 3 d S T P .
2


_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
Bi01 Ca02 3.2166(14) 39_444 ?
Bi01 Ca02 3.4509(15) . ?
Bi01 Ca02 3.2166(14) 27_544 ?
Bi01 Ca02 3.4509(15) 38_544 ?
Bi01 Ca02 3.2166(14) 2 ?
Bi01 Ca02 3.4509(15) 28_445 ?
Bi01 Ca02 3.2166(14) 13 ?
Bi01 Ca02 3.4509(15) 16_545 ?
Bi01 Pr02 3.4509(15) . ?
Ca02 Ca02 3.6944(15) 26_454 ?
Ca02 Ca02 4.1668(2) 37_444 ?
Ca02 Ca02 3.6944(15) 28_445 ?
Ca02 Ca02 3.6944(15) 27_544 ?
Ca02 Ca02 4.1668(2) 13 ?

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
Ca02 Bi01 Ca02 161.78(6) 39_444 13 ?
Ca02 Bi01 Ca02 67.19(3) 2 28_445 ?
Ca02 Bi01 Ca02 130.93(3) 2 . ?
Ca02 Bi01 Ca02 87.31(4) 13 28_445 ?
Ca02 Bi01 Ca02 67.19(3) 39_444 16_545 ?
Ca02 Bi01 Ca02 77.267(4) 27_544 16_545 ?
Ca02 Bi01 Ca02 77.267(4) 39_444 28_445 ?
Ca02 Bi01 Ca02 91.436(9) 39_444 2 ?
Ca02 Bi01 Ca02 135.518(2) 38_544 28_445 ?
Ca02 Bi01 Ca02 64.727(3) . 28_445 ?
Ca02 Bi01 Ca02 77.267(4) 13 . ?
Ca02 Bi01 Ca02 91.436(9) 13 2 ?
Ca02 Bi01 Ca02 135.518(2) 38_544 . ?
Ca02 Bi01 Ca02 135.518(2) 28_445 16_545 ?
Ca02 Bi01 Ca02 67.19(3) 13 38_544 ?
Ca02 Bi01 Ca02 91.436(9) 39_444 27_544 ?
Ca02 Bi01 Ca02 77.267(4) 2 38_544 ?
Ca02 Bi01 Ca02 130.93(3) 27_544 28_445 ?
Ca02 Bi01 Ca02 87.31(4) 27_544 38_544 ?
Ca02 Bi01 Ca02 91.436(9) 13 27_544 ?
Ca02 Bi01 Ca02 87.31(4) 2 16_545 ?
Ca02 Bi01 Ca02 130.93(3) 13 16_545 ?
Ca02 Bi01 Ca02 64.727(3) 38_544 16_545 ?
Ca02 Bi01 Ca02 161.78(6) 2 27_544 ?
Ca02 Bi01 Ca02 67.19(3) 27_544 . ?
Ca02 Bi01 Ca02 135.518(2) . 16_545 ?
Ca02 Bi01 Ca02 130.93(3) 39_444 38_544 ?
Ca02 Bi01 Ca02 87.31(4) 39_444 . ?
Pr02 Bi01 Ca02 135.518(2) . 16_545 ?
Pr02 Bi01 Ca02 64.727(3) . 28_445 ?
Bi01 Ca02 Bi01 84.833(4) 10_545 . ?
Bi01 Ca02 Bi01 107.516(5) 2_554 . ?
Bi01 Ca02 Bi01 162.306(18) 6_455 . ?
Bi01 Ca02 Bi01 88.79(5) 10_545 6_455 ?
Bi01 Ca02 Bi01 84.833(4) 6_455 9 ?
Bi01 Ca02 Bi01 81.40(4) . 9 ?
Bi01 Ca02 Bi01 162.306(18) 10_545 5 ?
Bi01 Ca02 Bi01 81.40(4) . 5 ?
Bi01 Ca02 Bi01 84.833(4) 2_554 5 ?
Bi01 Ca02 Bi01 88.79(5) 10_545 2_554 ?
Bi01 Ca02 Bi01 81.40(4) 9 5 ?
Bi01 Ca02 Bi01 107.516(5) 6_455 5 ?
Bi01 Ca02 Bi01 107.516(5) 10_545 9 ?
Bi01 Ca02 Bi01 88.79(5) 6_455 2_554 ?
Bi01 Ca02 Bi01 162.306(18) 2_554 9 ?
Bi01 Ca02 Ca02 59.43(2) 10_545 28_445 ?
Bi01 Ca02 Ca02 120.23(7) . 26_454 ?
Bi01 Ca02 Ca02 144.30(6) 6_455 27_544 ?
Bi01 Ca02 Ca02 57.637(2) 5 27_544 ?
Bi01 Ca02 Ca02 53.38(5) 5 26_454 ?
Bi01 Ca02 Ca02 126.12(3) 6_455 13 ?
Bi01 Ca02 Ca02 53.38(5) 9 28_445 ?
Bi01 Ca02 Ca02 105.030(11) 6_455 28_445 ?
Bi01 Ca02 Ca02 57.637(2) 9 26_454 ?
Bi01 Ca02 Ca02 144.30(6) 2_554 28_445 ?
Bi01 Ca02 Ca02 105.030(11) 10_545 27_544 ?
Bi01 Ca02 Ca02 48.85(3) 5 13 ?
Bi01 Ca02 Ca02 59.43(2) 2_554 27_544 ?
Bi01 Ca02 Ca02 57.637(2) . 28_445 ?
Bi01 Ca02 Ca02 53.88(3) 10_545 37_444 ?
Bi01 Ca02 Ca02 53.88(3) 6_455 37_444 ?
Bi01 Ca02 Ca02 53.88(3) 2_554 37_444 ?
Bi01 Ca02 Ca02 120.23(7) 5 28_445 ?
Bi01 Ca02 Ca02 131.15(3) 9 37_444 ?
Bi01 Ca02 Ca02 131.15(3) 5 37_444 ?
Bi01 Ca02 Ca02 126.12(3) 10_545 13 ?
Bi01 Ca02 Ca02 144.30(6) 10_545 26_454 ?
Bi01 Ca02 Ca02 126.12(3) 2_554 13 ?
Bi01 Ca02 Ca02 48.85(3) . 13 ?
Bi01 Ca02 Ca02 48.85(3) 9 13 ?
Bi01 Ca02 Ca02 59.43(2) 6_455 26_454 ?
Bi01 Ca02 Ca02 53.38(5) . 27_544 ?
Bi01 Ca02 Ca02 120.23(7) 9 27_544 ?
Bi01 Ca02 Ca02 105.030(11) 2_554 26_454 ?
Bi01 Ca02 Ca02 131.15(3) . 37_444 ?
Ca02 Ca02 Ca02 110.37(4) 28_445 27_544 ?
Ca02 Ca02 Ca02 108.56(4) 26_454 37_444 ?
Ca02 Ca02 Ca02 71.44(4) 27_544 13 ?
Ca02 Ca02 Ca02 108.56(4) 27_544 37_444 ?
Ca02 Ca02 Ca02 110.37(4) 28_445 26_454 ?
Ca02 Ca02 Ca02 71.44(4) 26_454 13 ?
Ca02 Ca02 Ca02 108.56(4) 28_445 37_444 ?
Ca02 Ca02 Ca02 110.37(4) 26_454 27_544 ?
Ca02 Ca02 Ca02 71.44(4) 28_445 13 ?
Ca02 Ca02 Ca02 180.00(18) 37_444 13 ?
Bi01 Pr02 Bi01 107.516(5) 6_455 5 ?
Bi01 Pr02 Bi01 81.40(4) . 9 ?
Bi01 Pr02 Bi01 84.833(4) 6_455 9 ?
Bi01 Pr02 Bi01 81.40(4) . 5 ?
Bi01 Pr02 Bi01 81.40(4) 9 5 ?
Bi01 Pr02 Bi01 88.79(5) 6_455 2_554 ?
Bi01 Pr02 Bi01 84.833(4) 10_545 . ?
Bi01 Pr02 Bi01 84.833(4) 2_554 5 ?
Bi01 Pr02 Bi01 162.306(18) 6_455 . ?
Bi01 Pr02 Bi01 107.516(5) 2_554 . ?
Bi01 Pr02 Bi01 88.79(5) 10_545 6_455 ?
Bi01 Pr02 Bi01 162.306(18) 10_545 5 ?
Bi01 Pr02 Bi01 88.79(5) 10_545 2_554 ?
Bi01 Pr02 Bi01 162.306(18) 2_554 9 ?
Bi01 Pr02 Bi01 107.516(5) 10_545 9 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.42(3)
2 0.58(3)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_svib1662
_database_code_depnum_ccdc_archive 'CCDC 2132682'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.296 Ce0.704'
_chemical_formula_sum            'Bi3 Ca3.30 Ce0.70'
_chemical_formula_weight         857.79
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Ce Ce -0.2486 2.6331 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.6407(6)
_cell_length_b                   9.6407(6)
_cell_length_c                   9.6407(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     896.04(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    773
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      29.28
_cell_measurement_theta_min      5.18
_shelx_estimated_absorpt_T_max   0.250
_shelx_estimated_absorpt_T_min   0.076
_exptl_absorpt_coefficient_mu    64.049
_exptl_absorpt_correction_T_max  0.2655
_exptl_absorpt_correction_T_min  0.1331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2005 before and 0.0430 after correction.
The Ratio of minimum to maximum transmission is 0.5013.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1423
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7.00 -5.00 1.00 0.0110
0.00 -5.00 2.00 0.0140
7.00 -6.00 3.00 0.0170
3.00 1.00 0.00 0.0140
-3.00 7.00 -3.00 0.0110
-3.00 7.00 -7.00 0.0180
-2.00 -6.00 7.00 0.0110
3.00 4.00 -4.00 0.0160
3.00 1.00 -6.00 0.0290
-1.00 0.00 -2.00 0.0240

_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.537
_diffrn_reflns_theta_min         5.180
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.699
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                212
_reflns_number_total             226
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(2)
_refine_ls_extinction_coef       0.00078(8)
_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   1.011
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0203
_refine_ls_restrained_S_all      1.011
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0259
_refine_ls_wR_factor_ref         0.0264
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.59(2)
 0.41(2)
2. Shared sites
{Ca02, Ce02}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca02) = Uanis(Ce02)
4. Others
 Sof(Ce02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi01 Bi 0.375000 0.000000 0.250000 0.00913(19) Uani 1 4 d S T P . .
Ca02 Ca 0.07200(11) 0.07200(11) 0.07200(11) 0.0099(7) Uani 0.824(5) 3 d S T P .
1
Ce02 Ce 0.07200(11) 0.07200(11) 0.07200(11) 0.0099(7) Uani 0.176(5) 3 d S T P .
2


_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
Bi01 Ca02 3.2217(11) 39_444 ?
Bi01 Ca02 3.4583(12) . ?
Bi01 Ca02 3.4583(12) 16_545 ?
Bi01 Ca02 3.2217(11) 13 ?
Bi01 Ca02 3.4583(12) 28_445 ?
Bi01 Ca02 3.2217(11) 2 ?
Bi01 Ca02 3.2217(11) 27_544 ?
Bi01 Ca02 3.4583(12) 38_544 ?
Bi01 Ce02 3.4583(12) . ?
Ca02 Ca02 4.1746(3) 37_444 ?
Ca02 Ca02 3.7023(12) 27_544 ?
Ca02 Ca02 4.1745(3) 13 ?
Ca02 Ca02 3.7023(12) 28_445 ?
Ca02 Ca02 3.7023(12) 26_454 ?

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
Ca02 Bi01 Ca02 161.75(4) 39_444 13 ?
Ca02 Bi01 Ca02 87.28(3) 13 28_445 ?
Ca02 Bi01 Ca02 135.519(2) . 16_545 ?
Ca02 Bi01 Ca02 91.442(7) 39_444 2 ?
Ca02 Bi01 Ca02 67.21(2) 39_444 16_545 ?
Ca02 Bi01 Ca02 91.442(7) 13 2 ?
Ca02 Bi01 Ca02 135.519(2) . 38_544 ?
Ca02 Bi01 Ca02 91.442(7) 39_444 27_544 ?
Ca02 Bi01 Ca02 130.95(2) 27_544 28_445 ?
Ca02 Bi01 Ca02 91.442(7) 13 27_544 ?
Ca02 Bi01 Ca02 87.28(3) 2 16_545 ?
Ca02 Bi01 Ca02 161.75(5) 2 27_544 ?
Ca02 Bi01 Ca02 135.519(2) 28_445 16_545 ?
Ca02 Bi01 Ca02 87.28(3) 39_444 . ?
Ca02 Bi01 Ca02 77.264(3) 39_444 28_445 ?
Ca02 Bi01 Ca02 77.264(3) 13 . ?
Ca02 Bi01 Ca02 67.21(2) 2 28_445 ?
Ca02 Bi01 Ca02 130.95(2) 2 . ?
Ca02 Bi01 Ca02 64.725(2) . 28_445 ?
Ca02 Bi01 Ca02 67.21(2) 27_544 . ?
Ca02 Bi01 Ca02 130.95(2) 13 16_545 ?
Ca02 Bi01 Ca02 130.95(2) 39_444 38_544 ?
Ca02 Bi01 Ca02 77.264(4) 27_544 16_545 ?
Ca02 Bi01 Ca02 67.21(2) 13 38_544 ?
Ca02 Bi01 Ca02 64.725(2) 38_544 16_545 ?
Ca02 Bi01 Ca02 77.264(4) 2 38_544 ?
Ca02 Bi01 Ca02 87.28(3) 27_544 38_544 ?
Ca02 Bi01 Ca02 135.519(2) 38_544 28_445 ?
Ce02 Bi01 Ca02 135.519(2) . 16_545 ?
Ce02 Bi01 Ca02 135.519(2) . 38_544 ?
Ce02 Bi01 Ca02 64.725(2) . 28_445 ?
Bi01 Ca02 Bi01 88.82(4) 10_545 6_455 ?
Bi01 Ca02 Bi01 81.37(3) 5 9 ?
Bi01 Ca02 Bi01 107.513(4) 10_545 9 ?
Bi01 Ca02 Bi01 162.294(14) 2_554 9 ?
Bi01 Ca02 Bi01 84.830(4) 2_554 5 ?
Bi01 Ca02 Bi01 107.513(4) 6_455 5 ?
Bi01 Ca02 Bi01 88.82(4) 10_545 2_554 ?
Bi01 Ca02 Bi01 81.37(3) . 5 ?
Bi01 Ca02 Bi01 88.82(4) 6_455 2_554 ?
Bi01 Ca02 Bi01 84.830(4) 6_455 9 ?
Bi01 Ca02 Bi01 84.830(4) 10_545 . ?
Bi01 Ca02 Bi01 81.37(3) . 9 ?
Bi01 Ca02 Bi01 162.294(14) 6_455 . ?
Bi01 Ca02 Bi01 107.513(4) 2_554 . ?
Bi01 Ca02 Bi01 162.294(14) 10_545 5 ?
Bi01 Ca02 Ca02 59.448(18) 10_545 28_445 ?
Bi01 Ca02 Ca02 120.18(6) 9 27_544 ?
Bi01 Ca02 Ca02 53.91(3) 6_455 37_444 ?
Bi01 Ca02 Ca02 105.022(9) 6_455 28_445 ?
Bi01 Ca02 Ca02 48.83(2) . 13 ?
Bi01 Ca02 Ca02 144.34(5) 2_554 28_445 ?
Bi01 Ca02 Ca02 131.17(2) 9 37_444 ?
Bi01 Ca02 Ca02 57.638(1) . 28_445 ?
Bi01 Ca02 Ca02 126.09(3) 6_455 13 ?
Bi01 Ca02 Ca02 53.34(4) 9 28_445 ?
Bi01 Ca02 Ca02 48.83(2) 9 13 ?
Bi01 Ca02 Ca02 144.34(5) 10_545 26_454 ?
Bi01 Ca02 Ca02 131.17(2) . 37_444 ?
Bi01 Ca02 Ca02 59.448(18) 6_455 26_454 ?
Bi01 Ca02 Ca02 57.638(1) 5 27_544 ?
Bi01 Ca02 Ca02 105.022(9) 2_554 26_454 ?
Bi01 Ca02 Ca02 126.09(3) 10_545 13 ?
Bi01 Ca02 Ca02 120.18(6) . 26_454 ?
Bi01 Ca02 Ca02 126.09(3) 2_554 13 ?
Bi01 Ca02 Ca02 53.34(4) 5 26_454 ?
Bi01 Ca02 Ca02 48.83(2) 5 13 ?
Bi01 Ca02 Ca02 57.638(1) 9 26_454 ?
Bi01 Ca02 Ca02 53.91(3) 10_545 37_444 ?
Bi01 Ca02 Ca02 105.022(9) 10_545 27_544 ?
Bi01 Ca02 Ca02 53.91(3) 2_554 37_444 ?
Bi01 Ca02 Ca02 144.34(5) 6_455 27_544 ?
Bi01 Ca02 Ca02 131.17(2) 5 37_444 ?
Bi01 Ca02 Ca02 59.448(18) 2_554 27_544 ?
Bi01 Ca02 Ca02 53.34(4) . 27_544 ?
Bi01 Ca02 Ca02 120.18(6) 5 28_445 ?
Ca02 Ca02 Ca02 110.34(3) 28_445 27_544 ?
Ca02 Ca02 Ca02 71.41(3) 27_544 13 ?
Ca02 Ca02 Ca02 108.59(3) 26_454 37_444 ?
Ca02 Ca02 Ca02 110.34(3) 26_454 27_544 ?
Ca02 Ca02 Ca02 108.59(3) 28_445 37_444 ?
Ca02 Ca02 Ca02 110.34(3) 28_445 26_454 ?
Ca02 Ca02 Ca02 108.59(3) 27_544 37_444 ?
Ca02 Ca02 Ca02 71.41(3) 28_445 13 ?
Ca02 Ca02 Ca02 71.41(3) 26_454 13 ?
Ca02 Ca02 Ca02 180.00(12) 13 37_444 ?
Bi01 Ce02 Bi01 107.513(4) 10_545 9 ?
Bi01 Ce02 Bi01 84.830(4) 2_554 5 ?
Bi01 Ce02 Bi01 162.294(14) 10_545 5 ?
Bi01 Ce02 Bi01 162.294(14) 2_554 9 ?
Bi01 Ce02 Bi01 107.513(4) 2_554 . ?
Bi01 Ce02 Bi01 81.37(3) 5 9 ?
Bi01 Ce02 Bi01 107.513(4) 6_455 5 ?
Bi01 Ce02 Bi01 84.830(4) 10_545 . ?
Bi01 Ce02 Bi01 81.37(3) . 5 ?
Bi01 Ce02 Bi01 162.294(14) 6_455 . ?
Bi01 Ce02 Bi01 84.830(4) 6_455 9 ?
Bi01 Ce02 Bi01 88.82(4) 10_545 6_455 ?
Bi01 Ce02 Bi01 81.37(3) . 9 ?
Bi01 Ce02 Bi01 88.82(4) 10_545 2_554 ?
Bi01 Ce02 Bi01 88.82(4) 6_455 2_554 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.59(2)
2 0.41(2)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2132686'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.232 Gd0.768'
_chemical_formula_sum            'Bi3 Ca3.23 Gd0.77'
_chemical_formula_weight         877.19
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Gd Gd -0.1653 3.9035 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.5782(5)
_cell_length_b                   9.5782(5)
_cell_length_c                   9.5782(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     878.72(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1275
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      30.40
_cell_measurement_theta_min      3.01
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    67.407
_exptl_absorpt_correction_T_max  0.2656
_exptl_absorpt_correction_T_min  0.1112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1576 before and 0.0657 after correction.
The Ratio of minimum to maximum transmission is 0.4187.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.631
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1451
_exptl_crystal_size_max          0.058
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.027
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1702
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.398
_diffrn_reflns_theta_min         5.214
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                224
_reflns_number_total             228
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.53(3)
_refine_ls_extinction_coef       0.00136(16)
_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   1.149
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.149
_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)+(0.0067P)²+6.7835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0390
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.47(3)
 0.53(3)
2. Shared sites
{Ca02, Gd02}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca02) = Uanis(Gd02)
4. Others
 Sof(Gd02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi01 Bi 0.375000 0.000000 0.250000 0.0065(2) Uani 1 4 d S T P . .
Ca02 Ca 0.07227(11) 0.07227(11) 0.07227(11) 0.0073(7) Uani 0.808(7) 3 d S T P .
1
Gd02 Gd 0.07227(11) 0.07227(11) 0.07227(11) 0.0073(7) Uani 0.192(7) 3 d S T P .
2


_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
Bi01 Ca02 3.2034(11) 39_444 ?
Bi01 Ca02 3.4330(13) . ?
Bi01 Ca02 3.4330(13) 16_545 ?
Bi01 Ca02 3.2034(11) 13 ?
Bi01 Ca02 3.4330(13) 28_445 ?
Bi01 Ca02 3.2034(11) 2 ?
Bi01 Ca02 3.2034(11) 27_544 ?
Bi01 Ca02 3.4330(13) 38_544 ?
Bi01 Gd02 3.4330(13) . ?
Ca02 Ca02 4.1475(2) 37_444 ?
Ca02 Ca02 3.6754(12) 27_544 ?
Ca02 Ca02 4.1475(2) 13 ?
Ca02 Ca02 3.6754(12) 28_445 ?
Ca02 Ca02 3.6754(12) 26_454 ?

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
Ca02 Bi01 Ca02 161.86(5) 39_444 13 ?
Ca02 Bi01 Ca02 87.36(4) 13 28_445 ?
Ca02 Bi01 Ca02 135.516(2) . 16_545 ?
Ca02 Bi01 Ca02 91.425(7) 39_444 2 ?
Ca02 Bi01 Ca02 67.16(2) 39_444 16_545 ?
Ca02 Bi01 Ca02 91.425(7) 13 2 ?
Ca02 Bi01 Ca02 135.515(2) . 38_544 ?
Ca02 Bi01 Ca02 91.425(7) 39_444 27_544 ?
Ca02 Bi01 Ca02 130.89(3) 27_544 28_445 ?
Ca02 Bi01 Ca02 91.425(7) 13 27_544 ?
Ca02 Bi01 Ca02 87.36(4) 2 16_545 ?
Ca02 Bi01 Ca02 161.86(5) 2 27_544 ?
Ca02 Bi01 Ca02 135.515(2) 28_445 16_545 ?
Ca02 Bi01 Ca02 87.36(4) 39_444 . ?
Ca02 Bi01 Ca02 77.273(4) 39_444 28_445 ?
Ca02 Bi01 Ca02 77.272(4) 13 . ?
Ca02 Bi01 Ca02 67.16(2) 2 28_445 ?
Ca02 Bi01 Ca02 130.89(3) 2 . ?
Ca02 Bi01 Ca02 64.731(3) . 28_445 ?
Ca02 Bi01 Ca02 67.16(2) 27_544 . ?
Ca02 Bi01 Ca02 130.89(3) 13 16_545 ?
Ca02 Bi01 Ca02 130.89(3) 39_444 38_544 ?
Ca02 Bi01 Ca02 77.273(4) 27_544 16_545 ?
Ca02 Bi01 Ca02 67.16(2) 13 38_544 ?
Ca02 Bi01 Ca02 64.731(3) 38_544 16_545 ?
Ca02 Bi01 Ca02 77.273(4) 2 38_544 ?
Ca02 Bi01 Ca02 87.36(4) 27_544 38_544 ?
Ca02 Bi01 Ca02 135.515(2) 38_544 28_445 ?
Gd02 Bi01 Ca02 135.516(2) . 16_545 ?
Gd02 Bi01 Ca02 135.515(2) . 38_544 ?
Gd02 Bi01 Ca02 64.731(3) . 28_445 ?
Bi01 Ca02 Bi01 88.73(4) 10_545 6_455 ?
Bi01 Ca02 Bi01 81.46(4) 5 9 ?
Bi01 Ca02 Bi01 107.522(4) 10_545 9 ?
Bi01 Ca02 Bi01 162.329(14) 2_554 9 ?
Bi01 Ca02 Bi01 84.839(4) 2_554 5 ?
Bi01 Ca02 Bi01 107.522(4) 6_455 5 ?
Bi01 Ca02 Bi01 88.73(4) 10_545 2_554 ?
Bi01 Ca02 Bi01 81.46(4) . 5 ?
Bi01 Ca02 Bi01 88.73(4) 6_455 2_554 ?
Bi01 Ca02 Bi01 84.839(4) 6_455 9 ?
Bi01 Ca02 Bi01 84.839(4) 10_545 . ?
Bi01 Ca02 Bi01 81.46(4) . 9 ?
Bi01 Ca02 Bi01 162.329(14) 6_455 . ?
Bi01 Ca02 Bi01 107.522(4) 2_554 . ?
Bi01 Ca02 Bi01 162.329(14) 10_545 5 ?
Bi01 Ca02 Ca02 59.404(19) 10_545 28_445 ?
Bi01 Ca02 Ca02 120.33(6) 9 27_544 ?
Bi01 Ca02 Ca02 53.84(3) 6_455 37_444 ?
Bi01 Ca02 Ca02 105.043(9) 6_455 28_445 ?
Bi01 Ca02 Ca02 48.89(2) . 13 ?
Bi01 Ca02 Ca02 144.22(5) 2_554 28_445 ?
Bi01 Ca02 Ca02 131.11(2) 9 37_444 ?
Bi01 Ca02 Ca02 57.635(1) . 28_445 ?
Bi01 Ca02 Ca02 126.16(3) 6_455 13 ?
Bi01 Ca02 Ca02 53.44(4) 9 28_445 ?
Bi01 Ca02 Ca02 48.89(2) 9 13 ?
Bi01 Ca02 Ca02 144.22(5) 10_545 26_454 ?
Bi01 Ca02 Ca02 131.11(2) . 37_444 ?
Bi01 Ca02 Ca02 59.404(19) 6_455 26_454 ?
Bi01 Ca02 Ca02 57.635(1) 5 27_544 ?
Bi01 Ca02 Ca02 105.043(9) 2_554 26_454 ?
Bi01 Ca02 Ca02 126.16(3) 10_545 13 ?
Bi01 Ca02 Ca02 120.33(6) . 26_454 ?
Bi01 Ca02 Ca02 126.16(3) 2_554 13 ?
Bi01 Ca02 Ca02 53.44(4) 5 26_454 ?
Bi01 Ca02 Ca02 48.89(2) 5 13 ?
Bi01 Ca02 Ca02 57.635(1) 9 26_454 ?
Bi01 Ca02 Ca02 53.84(3) 10_545 37_444 ?
Bi01 Ca02 Ca02 105.043(9) 10_545 27_544 ?
Bi01 Ca02 Ca02 53.84(3) 2_554 37_444 ?
Bi01 Ca02 Ca02 144.22(5) 6_455 27_544 ?
Bi01 Ca02 Ca02 131.11(2) 5 37_444 ?
Bi01 Ca02 Ca02 59.404(19) 2_554 27_544 ?
Bi01 Ca02 Ca02 53.44(4) . 27_544 ?
Bi01 Ca02 Ca02 120.33(6) 5 28_445 ?
Ca02 Ca02 Ca02 110.42(3) 28_445 27_544 ?
Ca02 Ca02 Ca02 71.50(4) 27_544 13 ?
Ca02 Ca02 Ca02 108.50(4) 26_454 37_444 ?
Ca02 Ca02 Ca02 110.42(3) 26_454 27_544 ?
Ca02 Ca02 Ca02 108.50(4) 28_445 37_444 ?
Ca02 Ca02 Ca02 110.42(3) 28_445 26_454 ?
Ca02 Ca02 Ca02 108.50(4) 27_544 37_444 ?
Ca02 Ca02 Ca02 71.50(4) 28_445 13 ?
Ca02 Ca02 Ca02 71.50(4) 26_454 13 ?
Ca02 Ca02 Ca02 180.00(12) 13 37_444 ?
Bi01 Gd02 Bi01 107.522(4) 10_545 9 ?
Bi01 Gd02 Bi01 84.839(4) 2_554 5 ?
Bi01 Gd02 Bi01 162.329(14) 10_545 5 ?
Bi01 Gd02 Bi01 162.329(14) 2_554 9 ?
Bi01 Gd02 Bi01 107.522(4) 2_554 . ?
Bi01 Gd02 Bi01 81.46(4) 5 9 ?
Bi01 Gd02 Bi01 107.522(4) 6_455 5 ?
Bi01 Gd02 Bi01 84.839(4) 10_545 . ?
Bi01 Gd02 Bi01 81.46(4) . 5 ?
Bi01 Gd02 Bi01 162.329(14) 6_455 . ?
Bi01 Gd02 Bi01 84.839(4) 6_455 9 ?
Bi01 Gd02 Bi01 88.73(4) 10_545 6_455 ?
Bi01 Gd02 Bi01 81.46(4) . 9 ?
Bi01 Gd02 Bi01 88.73(4) 10_545 2_554 ?
Bi01 Gd02 Bi01 88.73(4) 6_455 2_554 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.47(3)
2 0.53(3)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2132685'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.229 Sm0.771'
_chemical_formula_sum            'Bi3 Ca3.23 Sm0.77'
_chemical_formula_weight         872.17
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Sm Sm -0.1638 3.4418 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.5895(5)
_cell_length_b                   9.5895(5)
_cell_length_c                   9.5895(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     881.84(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    899
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      30.36
_cell_measurement_theta_min      5.21
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    66.522
_exptl_absorpt_correction_T_max  0.2654
_exptl_absorpt_correction_T_min  0.1179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1433 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.4442.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.569
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1445
_exptl_crystal_size_max          0.0084
_exptl_crystal_size_mid          0.0061
_exptl_crystal_size_min          0.0058
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1707
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.358
_diffrn_reflns_theta_min         5.208
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                218
_reflns_number_total             228
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.789
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.212
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.53(2)
_refine_ls_extinction_coef       0.00088(10)
_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   1.111
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0182
_refine_ls_restrained_S_all      1.111
_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)+(0.0067P)²+5.8249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0317
_refine_ls_wR_factor_ref         0.0321
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.47(2)
 0.53(2)
2. Shared sites
{Ca02, Sm02}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca02) = Uanis(Sm02)
4. Others
 Sof(Sm02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi01 Bi 0.375000 0.000000 0.250000 0.0083(2) Uani 1 4 d S T P . .
Ca02 Ca 0.07186(13) 0.07186(13) 0.07186(13) 0.0087(7) Uani 0.807(6) 3 d S T P .
1
Sm02 Sm 0.07186(13) 0.07186(13) 0.07186(13) 0.0087(7) Uani 0.193(6) 3 d S T P .
2


_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
Bi01 Ca02 3.2033(12) 39_444 ?
Bi01 Ca02 3.4414(14) 38_544 ?
Bi01 Ca02 3.4414(14) . ?
Bi01 Ca02 3.2033(12) 13 ?
Bi01 Ca02 3.4414(14) 28_445 ?
Bi01 Ca02 3.2033(12) 2 ?
Bi01 Ca02 3.2033(12) 27_544 ?
Bi01 Ca02 3.4414(14) 16_545 ?
Bi01 Sm02 3.4414(14) . ?
Ca02 Ca02 4.1524(2) 13 ?
Ca02 Ca02 3.6841(13) 27_544 ?
Ca02 Ca02 4.1524(2) 37_444 ?
Ca02 Ca02 3.6841(13) 28_445 ?
Ca02 Ca02 3.6840(13) 26_454 ?

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
Ca02 Bi01 Ca02 161.69(5) 39_444 13 ?
Ca02 Bi01 Ca02 130.98(3) 13 16_545 ?
Ca02 Bi01 Ca02 135.521(2) 38_544 . ?
Ca02 Bi01 Ca02 91.450(8) 39_444 2 ?
Ca02 Bi01 Ca02 87.24(4) 39_444 . ?
Ca02 Bi01 Ca02 91.450(8) 13 2 ?
Ca02 Bi01 Ca02 135.521(2) 38_544 28_445 ?
Ca02 Bi01 Ca02 91.450(8) 39_444 27_544 ?
Ca02 Bi01 Ca02 77.260(4) 27_544 16_545 ?
Ca02 Bi01 Ca02 91.450(8) 13 27_544 ?
Ca02 Bi01 Ca02 130.98(3) 2 . ?
Ca02 Bi01 Ca02 161.69(5) 2 27_544 ?
Ca02 Bi01 Ca02 135.521(2) 16_545 . ?
Ca02 Bi01 Ca02 130.98(3) 39_444 38_544 ?
Ca02 Bi01 Ca02 67.23(2) 39_444 16_545 ?
Ca02 Bi01 Ca02 67.23(2) 13 38_544 ?
Ca02 Bi01 Ca02 87.24(4) 2 16_545 ?
Ca02 Bi01 Ca02 77.260(4) 2 38_544 ?
Ca02 Bi01 Ca02 64.722(3) 38_544 16_545 ?
Ca02 Bi01 Ca02 87.24(4) 27_544 38_544 ?
Ca02 Bi01 Ca02 77.260(4) 13 . ?
Ca02 Bi01 Ca02 77.260(4) 39_444 28_445 ?
Ca02 Bi01 Ca02 67.23(2) 27_544 . ?
Ca02 Bi01 Ca02 87.24(4) 13 28_445 ?
Ca02 Bi01 Ca02 64.722(3) 28_445 . ?
Ca02 Bi01 Ca02 67.23(2) 2 28_445 ?
Ca02 Bi01 Ca02 130.98(3) 27_544 28_445 ?
Ca02 Bi01 Ca02 135.521(2) 28_445 16_545 ?
Bi01 Ca02 Bi01 88.87(4) 2_554 10_545 ?
Bi01 Ca02 Bi01 81.33(4) . 5 ?
Bi01 Ca02 Bi01 81.33(4) . 9 ?
Bi01 Ca02 Bi01 88.87(4) 2_554 6_455 ?
Bi01 Ca02 Bi01 107.508(5) 10_545 9 ?
Bi01 Ca02 Bi01 88.87(4) 10_545 6_455 ?
Bi01 Ca02 Bi01 107.508(5) 6_455 5 ?
Bi01 Ca02 Bi01 107.508(5) 2_554 . ?
Bi01 Ca02 Bi01 162.277(16) 2_554 9 ?
Bi01 Ca02 Bi01 84.826(4) 10_545 . ?
Bi01 Ca02 Bi01 84.826(4) 6_455 9 ?
Bi01 Ca02 Bi01 162.277(16) 6_455 . ?
Bi01 Ca02 Bi01 81.33(4) 5 9 ?
Bi01 Ca02 Bi01 84.826(4) 2_554 5 ?
Bi01 Ca02 Bi01 162.277(16) 10_545 5 ?
Bi01 Ca02 Ca02 144.40(6) 2_554 28_445 ?
Bi01 Ca02 Ca02 120.11(7) 9 27_544 ?
Bi01 Ca02 Ca02 126.06(3) 10_545 13 ?
Bi01 Ca02 Ca02 59.47(2) 10_545 28_445 ?
Bi01 Ca02 Ca02 131.20(3) . 37_444 ?
Bi01 Ca02 Ca02 105.012(10) 6_455 28_445 ?
Bi01 Ca02 Ca02 48.80(3) 9 13 ?
Bi01 Ca02 Ca02 57.639(1) . 28_445 ?
Bi01 Ca02 Ca02 53.94(3) 10_545 37_444 ?
Bi01 Ca02 Ca02 120.11(7) 5 28_445 ?
Bi01 Ca02 Ca02 131.20(3) 9 37_444 ?
Bi01 Ca02 Ca02 105.012(10) 2_554 26_454 ?
Bi01 Ca02 Ca02 48.80(3) . 13 ?
Bi01 Ca02 Ca02 144.40(6) 10_545 26_454 ?
Bi01 Ca02 Ca02 57.639(1) 5 27_544 ?
Bi01 Ca02 Ca02 59.47(2) 6_455 26_454 ?
Bi01 Ca02 Ca02 53.94(3) 2_554 37_444 ?
Bi01 Ca02 Ca02 120.11(7) . 26_454 ?
Bi01 Ca02 Ca02 53.94(3) 6_455 37_444 ?
Bi01 Ca02 Ca02 53.30(4) 5 26_454 ?
Bi01 Ca02 Ca02 131.20(3) 5 37_444 ?
Bi01 Ca02 Ca02 57.639(1) 9 26_454 ?
Bi01 Ca02 Ca02 126.06(3) 2_554 13 ?
Bi01 Ca02 Ca02 59.47(2) 2_554 27_544 ?
Bi01 Ca02 Ca02 126.06(3) 6_455 13 ?
Bi01 Ca02 Ca02 105.012(10) 10_545 27_544 ?
Bi01 Ca02 Ca02 48.80(3) 5 13 ?
Bi01 Ca02 Ca02 144.40(6) 6_455 27_544 ?
Bi01 Ca02 Ca02 53.30(4) . 27_544 ?
Bi01 Ca02 Ca02 53.30(4) 9 28_445 ?
Ca02 Ca02 Ca02 110.30(4) 28_445 27_544 ?
Ca02 Ca02 Ca02 108.63(4) 27_544 37_444 ?
Ca02 Ca02 Ca02 71.37(4) 26_454 13 ?
Ca02 Ca02 Ca02 110.30(4) 26_454 27_544 ?
Ca02 Ca02 Ca02 71.37(4) 28_445 13 ?
Ca02 Ca02 Ca02 110.30(4) 28_445 26_454 ?
Ca02 Ca02 Ca02 71.37(4) 27_544 13 ?
Ca02 Ca02 Ca02 108.63(4) 28_445 37_444 ?
Ca02 Ca02 Ca02 108.63(4) 26_454 37_444 ?
Ca02 Ca02 Ca02 180.00(16) 37_444 13 ?
Bi01 Sm02 Bi01 162.277(16) 2_554 9 ?
Bi01 Sm02 Bi01 107.508(5) 6_455 5 ?
Bi01 Sm02 Bi01 84.826(4) 2_554 5 ?
Bi01 Sm02 Bi01 84.826(4) 6_455 9 ?
Bi01 Sm02 Bi01 162.277(16) 6_455 . ?
Bi01 Sm02 Bi01 81.33(4) 5 9 ?
Bi01 Sm02 Bi01 162.277(16) 10_545 5 ?
Bi01 Sm02 Bi01 107.508(5) 2_554 . ?
Bi01 Sm02 Bi01 81.33(4) . 5 ?
Bi01 Sm02 Bi01 84.826(4) 10_545 . ?
Bi01 Sm02 Bi01 107.508(5) 10_545 9 ?
Bi01 Sm02 Bi01 88.87(4) 2_554 10_545 ?
Bi01 Sm02 Bi01 81.33(4) . 9 ?
Bi01 Sm02 Bi01 88.87(4) 2_554 6_455 ?
Bi01 Sm02 Bi01 88.87(4) 10_545 6_455 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.47(2)
2 0.53(2)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2132684'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.331 Nd0.669'
_chemical_formula_sum            'Bi3 Ca3.33 Nd0.67'
_chemical_formula_weight         857.05
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Nd Nd -0.1943 3.0179 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.6091(7)
_cell_length_b                   9.6091(7)
_cell_length_c                   9.6091(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     887.25(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    727
_cell_measurement_temperature    200.01
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      5.20
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    65.012
_exptl_absorpt_correction_T_max  0.2653
_exptl_absorpt_correction_T_min  0.1193
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.416
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1423
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1699
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.289
_diffrn_reflns_theta_min         5.197
_diffrn_ambient_temperature      200.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.659
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                204
_reflns_number_total             219
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_coef       0.00008(7)
_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   1.059
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8
_refine_ls_number_reflns         219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0216
_refine_ls_restrained_S_all      1.059
_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)+(0.0034P)²+16.7149P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0326
_refine_ls_wR_factor_ref         0.0335
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.49(3)
 0.51(3)
2. Shared sites
{Ca02, Nd02}
3. Uiso/Uaniso restraints and constraints
Uiso(Ca02) = Uiso(Nd02)
4. Others
 Sof(Nd02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi01 Bi 0.250000 0.125000 0.500000 0.0084(2) Uani 1 4 d S T P . .
Ca02 Ca 0.32190(16) 0.17810(16) 0.82190(16) 0.0084(8) Uiso 0.833(6) 3 d S . P .
1
Nd02 Nd 0.32190(16) 0.17810(16) 0.82190(16) 0.0084(8) Uiso 0.167(6) 3 d S . P .
2


_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
Bi01 Ca02 3.2102(15) 27_545 ?
Bi01 Ca02 3.2102(15) 16_546 ?
Bi01 Ca02 3.2102(15) . ?
Bi01 Ca02 3.4480(17) 14_554 ?
Bi01 Ca02 3.4480(17) 28_446 ?
Bi01 Ca02 3.4480(17) 2_554 ?
Bi01 Ca02 3.4480(17) 39_455 ?
Bi01 Ca02 3.2102(15) 37_444 ?
Bi01 Nd02 3.2102(15) . ?
Ca02 Ca02 3.6911(17) 28_446 ?
Ca02 Ca02 3.6911(17) 26_554 ?
Ca02 Ca02 4.1609(3) 14_554 ?
Ca02 Ca02 3.6911(17) 27_546 ?
Ca02 Ca02 4.1609(3) 38_544 ?

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
Ca02 Bi01 Ca02 91.447(10) 27_545 37_444 ?
Ca02 Bi01 Ca02 87.25(5) 16_546 2_554 ?
Ca02 Bi01 Ca02 135.521(2) 14_554 28_446 ?
Ca02 Bi01 Ca02 130.97(3) 16_546 14_554 ?
Ca02 Bi01 Ca02 77.261(5) 27_545 39_455 ?
Ca02 Bi01 Ca02 67.22(3) 16_546 39_455 ?
Ca02 Bi01 Ca02 77.261(5) 37_444 2_554 ?
Ca02 Bi01 Ca02 67.22(3) 37_444 14_554 ?
Ca02 Bi01 Ca02 130.97(3) . 2_554 ?
Ca02 Bi01 Ca02 87.25(5) 37_444 28_446 ?
Ca02 Bi01 Ca02 91.447(10) 16_546 . ?
Ca02 Bi01 Ca02 64.723(3) 2_554 28_446 ?
Ca02 Bi01 Ca02 67.22(3) . 28_446 ?
Ca02 Bi01 Ca02 87.25(5) 27_545 14_554 ?
Ca02 Bi01 Ca02 161.71(6) 27_545 . ?
Ca02 Bi01 Ca02 91.447(10) 27_545 16_546 ?
Ca02 Bi01 Ca02 77.261(5) . 14_554 ?
Ca02 Bi01 Ca02 135.520(2) 2_554 14_554 ?
Ca02 Bi01 Ca02 91.448(10) 37_444 . ?
Ca02 Bi01 Ca02 130.97(3) 27_545 28_446 ?
Ca02 Bi01 Ca02 77.261(5) 16_546 28_446 ?
Ca02 Bi01 Ca02 130.97(3) 37_444 39_455 ?
Ca02 Bi01 Ca02 87.25(5) . 39_455 ?
Ca02 Bi01 Ca02 161.71(6) 37_444 16_546 ?
Ca02 Bi01 Ca02 67.22(3) 27_545 2_554 ?
Ca02 Bi01 Ca02 64.723(4) 39_455 14_554 ?
Ca02 Bi01 Ca02 135.521(2) 2_554 39_455 ?
Ca02 Bi01 Ca02 135.521(2) 39_455 28_446 ?
Nd02 Bi01 Ca02 77.261(5) . 14_554 ?
Nd02 Bi01 Ca02 67.22(3) . 28_446 ?
Nd02 Bi01 Ca02 87.25(5) . 39_455 ?
Bi01 Ca02 Bi01 162.28(2) 6_456 33_545 ?
Bi01 Ca02 Bi01 84.827(5) . 33_545 ?
Bi01 Ca02 Bi01 88.85(5) . 6_456 ?
Bi01 Ca02 Bi01 84.827(5) 6_456 2 ?
Bi01 Ca02 Bi01 162.28(2) . 5_556 ?
Bi01 Ca02 Bi01 107.509(6) 34_545 33_545 ?
Bi01 Ca02 Bi01 88.85(5) 34_545 6_456 ?
Bi01 Ca02 Bi01 81.34(5) 5_556 33_545 ?
Bi01 Ca02 Bi01 107.509(6) . 2 ?
Bi01 Ca02 Bi01 107.509(6) 6_456 5_556 ?
Bi01 Ca02 Bi01 84.827(5) 34_545 5_556 ?
Bi01 Ca02 Bi01 162.28(2) 34_545 2 ?
Bi01 Ca02 Bi01 88.85(5) . 34_545 ?
Bi01 Ca02 Bi01 81.34(5) 5_556 2 ?
Bi01 Ca02 Bi01 81.34(5) 2 33_545 ?
Bi01 Ca02 Ca02 59.46(3) . 28_446 ?
Bi01 Ca02 Ca02 57.639(2) 33_545 28_446 ?
Bi01 Ca02 Ca02 59.46(3) 34_545 26_554 ?
Bi01 Ca02 Ca02 57.639(2) 5_556 26_554 ?
Bi01 Ca02 Ca02 105.015(12) . 26_554 ?
Bi01 Ca02 Ca02 105.015(12) 34_545 27_546 ?
Bi01 Ca02 Ca02 48.81(3) 5_556 38_544 ?
Bi01 Ca02 Ca02 120.14(8) 33_545 27_546 ?
Bi01 Ca02 Ca02 48.81(3) 33_545 38_544 ?
Bi01 Ca02 Ca02 53.93(4) 34_545 14_554 ?
Bi01 Ca02 Ca02 131.19(3) 5_556 14_554 ?
Bi01 Ca02 Ca02 53.31(5) 2 28_446 ?
Bi01 Ca02 Ca02 57.639(2) 2 27_546 ?
Bi01 Ca02 Ca02 144.38(7) 34_545 28_446 ?
Bi01 Ca02 Ca02 126.07(4) 6_456 38_544 ?
Bi01 Ca02 Ca02 120.14(8) 2 26_554 ?
Bi01 Ca02 Ca02 48.81(3) 2 38_544 ?
Bi01 Ca02 Ca02 105.015(13) 6_456 28_446 ?
Bi01 Ca02 Ca02 53.93(4) . 14_554 ?
Bi01 Ca02 Ca02 144.38(7) . 27_546 ?
Bi01 Ca02 Ca02 53.93(4) 6_456 14_554 ?
Bi01 Ca02 Ca02 131.19(3) 33_545 14_554 ?
Bi01 Ca02 Ca02 131.19(3) 2 14_554 ?
Bi01 Ca02 Ca02 59.46(3) 6_456 27_546 ?
Bi01 Ca02 Ca02 53.31(5) 5_556 27_546 ?
Bi01 Ca02 Ca02 120.14(8) 5_556 28_446 ?
Bi01 Ca02 Ca02 144.38(7) 6_456 26_554 ?
Bi01 Ca02 Ca02 126.07(4) . 38_544 ?
Bi01 Ca02 Ca02 126.07(4) 34_545 38_544 ?
Bi01 Ca02 Ca02 53.31(5) 33_545 26_554 ?
Ca02 Ca02 Ca02 110.31(5) 28_446 27_546 ?
Ca02 Ca02 Ca02 108.62(5) 28_446 14_554 ?
Ca02 Ca02 Ca02 71.38(5) 28_446 38_544 ?
Ca02 Ca02 Ca02 71.38(5) 26_554 38_544 ?
Ca02 Ca02 Ca02 108.62(5) 26_554 14_554 ?
Ca02 Ca02 Ca02 108.62(5) 27_546 14_554 ?
Ca02 Ca02 Ca02 110.31(5) 26_554 27_546 ?
Ca02 Ca02 Ca02 71.38(5) 27_546 38_544 ?
Ca02 Ca02 Ca02 110.31(5) 28_446 26_554 ?
Ca02 Ca02 Ca02 180.00(7) 38_544 14_554 ?
Bi01 Nd02 Bi01 88.85(5) . 34_545 ?
Bi01 Nd02 Bi01 84.827(5) 34_545 5_556 ?
Bi01 Nd02 Bi01 162.28(2) . 5_556 ?
Bi01 Nd02 Bi01 88.85(5) . 6_456 ?
Bi01 Nd02 Bi01 88.85(5) 34_545 6_456 ?
Bi01 Nd02 Bi01 107.509(6) . 2 ?
Bi01 Nd02 Bi01 162.28(2) 6_456 33_545 ?
Bi01 Nd02 Bi01 81.34(5) 5_556 33_545 ?
Bi01 Nd02 Bi01 107.509(6) 6_456 5_556 ?
Bi01 Nd02 Bi01 81.34(5) 2 33_545 ?
Bi01 Nd02 Bi01 84.827(5) . 33_545 ?
Bi01 Nd02 Bi01 107.509(6) 34_545 33_545 ?
Bi01 Nd02 Bi01 84.827(5) 6_456 2 ?
Bi01 Nd02 Bi01 81.34(5) 5_556 2 ?
Bi01 Nd02 Bi01 162.28(2) 34_545 2 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.49(3)
2 0.51(3)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_svib1502_0m
_database_code_depnum_ccdc_archive 'CCDC 2132689'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.377 Ho0.623'
_chemical_formula_sum            'Bi3 Ca3.38 Ho0.62'
_chemical_formula_weight         865.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Ho Ho -0.2175 4.6783 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.5590(9)
_cell_length_b                   9.5590(9)
_cell_length_c                   9.5590(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     873.4(2)
_cell_formula_units_Z            3.99984
_cell_measurement_reflns_used    1154
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      3.01
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    67.730
_exptl_absorpt_correction_T_max  0.2656
_exptl_absorpt_correction_T_min  0.0490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.2072 before and 0.0729 after correction.
The Ratio of minimum to maximum transmission is 0.1845.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    6.578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1433
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4.00 -5.00 -1.00 0.0320
2.00 1.00 4.00 0.0300
-1.00 4.00 4.00 0.0400
-4.00 5.00 1.00 0.0480
-2.00 -1.00 -4.00 0.0510
-2.00 3.00 1.00 0.0470
3.00 -1.00 3.00 0.0280
1.00 -5.00 -5.00 0.0380
-1.00 -3.00 1.00 0.0320
1.00 3.00 -1.00 0.0460
-2.00 2.00 -5.00 0.0510
4.00 4.00 3.00 0.0400
-5.00 -2.00 3.00 0.0420
5.00 2.00 -3.00 0.0390
1.00 1.00 -5.00 0.0400
-4.00 -1.00 -2.00 0.0390
-1.00 -1.00 5.00 0.0350

_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.084
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1849
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.465
_diffrn_reflns_theta_min         5.225
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                222
_reflns_number_total             228
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_coef       0.00193(16)
_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   1.232
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0142
_refine_ls_restrained_S_all      1.232
_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)+(0.0113P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0300
_refine_ls_wR_factor_ref         0.0303
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.50(2)
 0.50(2)
2. Shared sites
{Ca, Ho}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca) = Uanis(Ho)
4. Others
 Sof(Ho)=0.33333*(1-FVAR(2))
 Sof(Ca)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_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
Bi Bi 0.375000 0.000000 0.250000 0.00970(19) Uani 1 4 d S T P . .
Ca Ca 0.07252(9) 0.07252(9) 0.07252(9) 0.0095(6) Uani 0.844(5) 3 d S T P . .
Ho Ho 0.07252(9) 0.07252(9) 0.07252(9) 0.0095(6) Uani 0.156(5) 3 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
Bi Ca 3.1994(9) 39_444 ?
Bi Ca 3.4234(10) 38_544 ?
Bi Ca 3.4234(10) 28_445 ?
Bi Ca 3.4234(10) . ?
Bi Ca 3.1994(9) 2 ?
Bi Ca 3.4234(10) 16_545 ?
Bi Ca 3.1994(9) 13 ?
Bi Ca 3.1994(9) 27_544 ?
Ca Ca 3.6655(10) 28_445 ?
Ca Ca 3.6655(10) 27_544 ?
Ca Ca 3.6654(10) 26_454 ?
Ca Ca 4.1392(4) 37_444 ?
Ca Ca 4.1391(4) 13 ?

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
Ca Bi Ca 161.96(4) 39_444 13 ?
Ca Bi Ca 67.111(17) 2 28_445 ?
Ca Bi Ca 77.280(3) 2 38_544 ?
Ca Bi Ca 87.44(3) 13 28_445 ?
Ca Bi Ca 130.833(19) 39_444 38_544 ?
Ca Bi Ca 135.512(1) . 16_545 ?
Ca Bi Ca 77.280(3) 39_444 28_445 ?
Ca Bi Ca 91.409(6) 39_444 2 ?
Ca Bi Ca 64.736(2) . 28_445 ?
Ca Bi Ca 67.111(17) 39_444 16_545 ?
Ca Bi Ca 67.111(17) 13 38_544 ?
Ca Bi Ca 91.409(6) 13 2 ?
Ca Bi Ca 135.512(1) 38_544 28_445 ?
Ca Bi Ca 135.511(1) . 38_544 ?
Ca Bi Ca 77.280(3) 13 . ?
Ca Bi Ca 91.409(6) 39_444 27_544 ?
Ca Bi Ca 130.833(19) 2 . ?
Ca Bi Ca 130.833(19) 27_544 28_445 ?
Ca Bi Ca 67.111(17) 27_544 . ?
Ca Bi Ca 91.409(6) 13 27_544 ?
Ca Bi Ca 77.280(3) 27_544 16_545 ?
Ca Bi Ca 87.44(3) 2 16_545 ?
Ca Bi Ca 64.736(2) 38_544 16_545 ?
Ca Bi Ca 161.96(4) 2 27_544 ?
Ca Bi Ca 87.44(3) 27_544 38_544 ?
Ca Bi Ca 135.512(1) 28_445 16_545 ?
Ca Bi Ca 87.44(3) 39_444 . ?
Ca Bi Ca 130.833(19) 13 16_545 ?
Bi Ca Bi 88.64(3) 10_545 6_455 ?
Bi Ca Bi 81.53(3) . 9 ?
Bi Ca Bi 81.53(3) 9 5 ?
Bi Ca Bi 162.360(11) 2_554 9 ?
Bi Ca Bi 107.531(3) 6_455 5 ?
Bi Ca Bi 84.846(3) 2_554 5 ?
Bi Ca Bi 84.846(3) 10_545 . ?
Bi Ca Bi 88.64(3) 10_545 2_554 ?
Bi Ca Bi 162.360(11) 6_455 . ?
Bi Ca Bi 162.360(11) 10_545 5 ?
Bi Ca Bi 107.531(3) 2_554 . ?
Bi Ca Bi 88.64(3) 6_455 2_554 ?
Bi Ca Bi 81.53(3) . 5 ?
Bi Ca Bi 84.846(3) 6_455 9 ?
Bi Ca Bi 107.531(3) 10_545 9 ?
Bi Ca Ca 59.363(15) 10_545 28_445 ?
Bi Ca Ca 126.22(2) 10_545 13 ?
Bi Ca Ca 105.062(7) 10_545 27_544 ?
Bi Ca Ca 120.46(5) 9 27_544 ?
Bi Ca Ca 57.632(1) 9 26_454 ?
Bi Ca Ca 53.78(2) 6_455 37_444 ?
Bi Ca Ca 57.632(1) 5 27_544 ?
Bi Ca Ca 105.062(7) 6_455 28_445 ?
Bi Ca Ca 126.22(2) 2_554 13 ?
Bi Ca Ca 48.938(19) . 13 ?
Bi Ca Ca 53.53(3) 5 26_454 ?
Bi Ca Ca 144.10(4) 2_554 28_445 ?
Bi Ca Ca 144.10(4) 6_455 27_544 ?
Bi Ca Ca 131.062(19) 5 37_444 ?
Bi Ca Ca 59.363(15) 6_455 26_454 ?
Bi Ca Ca 57.632(1) . 28_445 ?
Bi Ca Ca 105.062(7) 2_554 26_454 ?
Bi Ca Ca 126.22(2) 6_455 13 ?
Bi Ca Ca 48.938(19) 9 13 ?
Bi Ca Ca 53.53(3) 9 28_445 ?
Bi Ca Ca 53.78(2) 10_545 37_444 ?
Bi Ca Ca 48.938(19) 5 13 ?
Bi Ca Ca 53.78(2) 2_554 37_444 ?
Bi Ca Ca 120.46(5) 5 28_445 ?
Bi Ca Ca 131.062(19) 9 37_444 ?
Bi Ca Ca 131.062(19) . 37_444 ?
Bi Ca Ca 59.363(15) 2_554 27_544 ?
Bi Ca Ca 144.10(4) 10_545 26_454 ?
Bi Ca Ca 53.53(3) . 27_544 ?
Bi Ca Ca 120.46(5) . 26_454 ?
Ca Ca Ca 108.43(3) 27_544 37_444 ?
Ca Ca Ca 180.00(10) 13 37_444 ?
Ca Ca Ca 71.57(3) 27_544 13 ?
Ca Ca Ca 71.57(3) 28_445 13 ?
Ca Ca Ca 110.49(3) 28_445 26_454 ?
Ca Ca Ca 108.43(3) 28_445 37_444 ?
Ca Ca Ca 108.43(3) 26_454 37_444 ?
Ca Ca Ca 110.49(3) 26_454 27_544 ?
Ca Ca Ca 110.49(3) 28_445 27_544 ?
Ca Ca Ca 71.57(3) 26_454 13 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.50(2)
2 0.50(2)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_svib1478_0m
_database_code_depnum_ccdc_archive 'CCDC 2132691'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.253 Tm0.747'
_chemical_formula_sum            'Bi3 Ca3.25 Tm0.75'
_chemical_formula_weight         883.58
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Tm Tm -0.3139 5.2483 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.5378(18)
_cell_length_b                   9.5378
_cell_length_c                   9.5378
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     867.7(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    471
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      5.24
_shelx_estimated_absorpt_T_max   0.104
_shelx_estimated_absorpt_T_min   0.083
_exptl_absorpt_coefficient_mu    70.059
_exptl_absorpt_correction_T_max  0.2656
_exptl_absorpt_correction_T_min  0.1035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1925 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.3897.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    6.764
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1463
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 -1.00 4.00 0.0300
1.00 1.00 3.00 0.0370
4.00 4.00 -1.00 0.0400
1.00 1.00 -1.00 0.0370
0.00 0.00 -1.00 0.0340
-1.00 -1.00 -3.00 0.0390
-4.00 -4.00 -1.00 0.0300
-2.00 -2.00 3.00 0.0290
-1.00 -3.00 -3.00 0.0350
0.00 -4.00 1.00 0.0350
1.00 -1.00 4.00 0.0310
0.00 4.00 -1.00 0.0330
-1.00 3.00 -4.00 0.0450
4.00 0.00 1.00 0.0280
2.00 -1.00 -3.00 0.0250
-4.00 0.00 -1.00 0.0290

_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.059
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1834
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.540
_diffrn_reflns_theta_min         5.236
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                220
_reflns_number_total             228
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.398
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.281
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.53(4)
_refine_ls_extinction_coef       0.0011(2)
_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   1.097
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0242
_refine_ls_restrained_S_all      1.097
_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)+(0.0271P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0519
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.47(4)
 0.53(4)
2. Shared sites
{Ca, Tm}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca) = Uanis(Tm)
4. Others
 Sof(Tm)=0.33333*(1-FVAR(2))
 Sof(Ca)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi Bi 0.375000 0.000000 0.250000 0.0106(3) Uani 1 4 d S T P . .
Ca Ca 0.07252(14) 0.07252(14) 0.07252(14) 0.0091(9) Uani 0.813(7) 3 d S T P . .
Tm Tm 0.07252(14) 0.07252(14) 0.07252(14) 0.0091(9) Uani 0.187(7) 3 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
Bi Ca 3.1924(14) 39_444 ?
Bi Ca 3.4157(16) . ?
Bi Ca 3.4157(16) 16_545 ?
Bi Ca 3.1924(14) 13 ?
Bi Ca 3.4157(16) 38_544 ?
Bi Ca 3.1924(14) 2 ?
Bi Ca 3.1924(14) 27_544 ?
Bi Ca 3.4157(16) 28_445 ?
Ca Ca 3.6573(15) 28_445 ?
Ca Ca 4.1300(3) 37_444 ?
Ca Ca 4.1300(3) 13 ?
Ca Ca 3.6573(15) 26_454 ?
Ca Ca 3.6573(16) 27_544 ?

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
Ca Bi Ca 161.96(6) 39_444 13 ?
Ca Bi Ca 87.44(4) 13 28_445 ?
Ca Bi Ca 135.512(7) . 16_545 ?
Ca Bi Ca 91.409(9) 39_444 2 ?
Ca Bi Ca 67.11(3) 39_444 16_545 ?
Ca Bi Ca 91.409(9) 13 2 ?
Ca Bi Ca 135.511(7) . 38_544 ?
Ca Bi Ca 91.409(9) 39_444 27_544 ?
Ca Bi Ca 130.83(3) 27_544 28_445 ?
Ca Bi Ca 91.409(9) 13 27_544 ?
Ca Bi Ca 87.44(4) 2 16_545 ?
Ca Bi Ca 161.96(6) 2 27_544 ?
Ca Bi Ca 135.511(7) 28_445 16_545 ?
Ca Bi Ca 87.44(4) 39_444 . ?
Ca Bi Ca 77.280(4) 39_444 28_445 ?
Ca Bi Ca 77.280(5) 13 . ?
Ca Bi Ca 67.11(3) 2 28_445 ?
Ca Bi Ca 130.83(3) 2 . ?
Ca Bi Ca 64.737(10) . 28_445 ?
Ca Bi Ca 67.11(3) 27_544 . ?
Ca Bi Ca 130.83(3) 13 16_545 ?
Ca Bi Ca 130.83(3) 39_444 38_544 ?
Ca Bi Ca 77.280(4) 27_544 16_545 ?
Ca Bi Ca 67.11(3) 13 38_544 ?
Ca Bi Ca 64.737(11) 38_544 16_545 ?
Ca Bi Ca 77.280(4) 2 38_544 ?
Ca Bi Ca 87.44(4) 27_544 38_544 ?
Ca Bi Ca 135.511(7) 38_544 28_445 ?
Bi Ca Bi 88.64(5) 10_545 6_455 ?
Bi Ca Bi 162.361(17) 2_554 9 ?
Bi Ca Bi 84.846(5) 2_554 5 ?
Bi Ca Bi 88.64(5) 10_545 2_554 ?
Bi Ca Bi 162.361(17) 10_545 5 ?
Bi Ca Bi 88.64(5) 6_455 2_554 ?
Bi Ca Bi 84.846(6) 6_455 9 ?
Bi Ca Bi 84.846(6) 10_545 . ?
Bi Ca Bi 81.54(4) . 9 ?
Bi Ca Bi 162.361(17) 6_455 . ?
Bi Ca Bi 107.531(8) 6_455 5 ?
Bi Ca Bi 107.531(8) 2_554 . ?
Bi Ca Bi 81.54(4) 9 5 ?
Bi Ca Bi 107.531(5) 10_545 9 ?
Bi Ca Bi 81.54(4) . 5 ?
Bi Ca Ca 59.36(2) 10_545 28_445 ?
Bi Ca Ca 120.46(7) 9 27_544 ?
Bi Ca Ca 53.78(3) 6_455 37_444 ?
Bi Ca Ca 105.062(11) 6_455 28_445 ?
Bi Ca Ca 48.94(3) . 13 ?
Bi Ca Ca 144.10(6) 2_554 28_445 ?
Bi Ca Ca 131.06(3) 5 37_444 ?
Bi Ca Ca 57.632(5) . 28_445 ?
Bi Ca Ca 126.22(3) 6_455 13 ?
Bi Ca Ca 53.53(5) 9 28_445 ?
Bi Ca Ca 48.94(3) 5 13 ?
Bi Ca Ca 120.46(7) 5 28_445 ?
Bi Ca Ca 131.06(3) . 37_444 ?
Bi Ca Ca 144.10(6) 10_545 26_454 ?
Bi Ca Ca 53.53(5) . 27_544 ?
Bi Ca Ca 59.36(2) 6_455 26_454 ?
Bi Ca Ca 126.22(3) 10_545 13 ?
Bi Ca Ca 105.062(11) 2_554 26_454 ?
Bi Ca Ca 126.22(3) 2_554 13 ?
Bi Ca Ca 120.46(7) . 26_454 ?
Bi Ca Ca 48.94(3) 9 13 ?
Bi Ca Ca 57.632(2) 9 26_454 ?
Bi Ca Ca 53.78(3) 10_545 37_444 ?
Bi Ca Ca 53.53(5) 5 26_454 ?
Bi Ca Ca 53.78(3) 2_554 37_444 ?
Bi Ca Ca 105.062(11) 10_545 27_544 ?
Bi Ca Ca 131.06(3) 9 37_444 ?
Bi Ca Ca 144.10(6) 6_455 27_544 ?
Bi Ca Ca 59.36(2) 2_554 27_544 ?
Bi Ca Ca 57.632(4) 5 27_544 ?
Ca Ca Ca 108.42(4) 27_544 37_444 ?
Ca Ca Ca 71.58(4) 28_445 13 ?
Ca Ca Ca 108.42(4) 28_445 37_444 ?
Ca Ca Ca 110.50(4) 26_454 27_544 ?
Ca Ca Ca 71.58(4) 26_454 13 ?
Ca Ca Ca 110.50(4) 28_445 26_454 ?
Ca Ca Ca 71.58(4) 27_544 13 ?
Ca Ca Ca 108.42(4) 26_454 37_444 ?
Ca Ca Ca 180.00(15) 13 37_444 ?
Ca Ca Ca 110.50(4) 28_445 27_544 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.47(4)
2 0.53(4)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2132694'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-11-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'1.672(Bi), 0.267(Ca12), 0.067(Ho12), 1.328(Sb)'
_chemical_formula_sum            'Bi1.67 Ca3.20 Ho0.80 Sb1.33'
_chemical_formula_weight         771.12
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Ho Ho -0.2175 4.6783 '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'

_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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y+1/4, -x+3/4, -z+1/4'
'-x, -y+1/2, z'
'-y+1/4, x+1/4, -z+3/4'
'-x+1/4, z+1/4, -y+3/4'
'x, -y, -z+1/2'
'-x+3/4, -z+1/4, y+1/4'
'-z+3/4, -y+1/4, x+1/4'
'-x+1/2, y, -z'
'z+1/4, -y+3/4, -x+1/4'
'z, x, y'
'y, z, x'
'-y, -z+1/2, x'
'z, -x, -y+1/2'
'-y+1/2, z, -x'
'-z, -x+1/2, y'
'-z+1/2, x, -y'
'y, -z, -x+1/2'
'-y+3/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'
'x+1/4, -z+3/4, -y+1/4'
'x+1/4, z+1/4, y+1/4'
'-z+1/4, y+1/4, -x+3/4'
'z+1/4, y+1/4, x+1/4'
'x+1/2, y+1/2, z+1/2'
'y+3/4, -x+5/4, -z+3/4'
'-x+1/2, -y+1, z+1/2'
'-y+3/4, x+3/4, -z+5/4'
'-x+3/4, z+3/4, -y+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+5/4, -z+3/4, y+3/4'
'-z+5/4, -y+3/4, x+3/4'
'-x+1, y+1/2, -z+1/2'
'z+3/4, -y+5/4, -x+3/4'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1, x+1/2'
'z+1/2, -x+1/2, -y+1'
'-y+1, z+1/2, -x+1/2'
'-z+1/2, -x+1, y+1/2'
'-z+1, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1'
'-y+5/4, -x+3/4, z+3/4'
'y+3/4, x+3/4, z+3/4'
'x+3/4, -z+5/4, -y+3/4'
'x+3/4, z+3/4, y+3/4'
'-z+3/4, y+3/4, -x+5/4'
'z+3/4, y+3/4, x+3/4'

_cell_length_a                   9.4530(17)
_cell_length_b                   9.4530(17)
_cell_length_c                   9.4530(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     844.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    670
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      29.916
_cell_measurement_theta_min      5.284
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    48.148
_exptl_absorpt_correction_T_max  0.2656
_exptl_absorpt_correction_T_min  0.1604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1215 before and 0.0497 after correction.
The Ratio of minimum to maximum transmission is 0.6039.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.064
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.0092
_exptl_crystal_size_mid          0.0086
_exptl_crystal_size_min          0.0045
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1624
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.475
_diffrn_reflns_theta_min         5.283
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                211
_reflns_number_total             220
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.675
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.391
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8
_refine_ls_number_reflns         220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      1.139
_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)+(0.0236P)²+83.2837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0775
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.49(8)
 0.51(8)
2. Shared sites
{Ca1, Ho1}
{Bi2, Sb2}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca1) = Uanis(Ho1)
Uanis(Bi2) = Uanis(Sb2)
4. Others
 Sof(Sb2)=0.25*(1-FVAR(2))
 Sof(Bi2)=0.25*FVAR(2)
 Fixed Sof: Ca1(0.26667) Ho1(0.06667)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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
Bi2 Bi 0.000000 0.750000 0.125000 0.0094(4) Uani 0.56(4) 4 d S T P A 3
Ca1 Ca 0.0725(2) 1.0725(2) 0.0725(2) 0.0085(10) Uani 0.8 3 d S T P B 1
Ho1 Ho 0.0725(2) 1.0725(2) 0.0725(2) 0.0085(10) Uani 0.2 3 d S T P C 2
Sb2 Sb 0.000000 0.750000 0.125000 0.0094(4) Uani 0.44(4) 4 d S T P A 4


_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
Ca1 Ca1 3.625(2) 9 ?
Ca1 Ca1 3.625(2) 6_575 ?
Ca1 Ca1 3.625(2) 3_575 ?
Ca1 Ca1 4.0933(7) 20_465 ?
Ca1 Ca1 4.0933(7) 44_354 ?

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
Ca1 Ca1 Ca1 110.50(6) 9 3_575 ?
Ca1 Ca1 Ca1 180.0 44_354 20_465 ?
Ca1 Ca1 Ca1 71.58(6) 3_575 20_465 ?
Ca1 Ca1 Ca1 71.58(6) 6_575 20_465 ?
Ca1 Ca1 Ca1 110.50(6) 3_575 6_575 ?
Ca1 Ca1 Ca1 71.58(6) 9 20_465 ?
Ca1 Ca1 Ca1 108.42(6) 9 44_354 ?
Ca1 Ca1 Ca1 110.50(6) 9 6_575 ?
Ca1 Ca1 Ca1 108.42(6) 3_575 44_354 ?
Ca1 Ca1 Ca1 108.42(6) 6_575 44_354 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.49(8)
2 0.51(8)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 2132687'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-12-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.349 Tb0.651'
_chemical_formula_sum            'Bi3 Ca3.35 Tb0.65'
_chemical_formula_weight         864.80
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Tb Tb -0.1723 4.1537 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.5706(19)
_cell_length_b                   9.5706(19)
_cell_length_c                   9.5706(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     876.6(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    715
_cell_measurement_temperature    200.01
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      5.22
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    67.108
_exptl_absorpt_correction_T_max  0.2654
_exptl_absorpt_correction_T_min  0.0750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1302 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.2826.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.553
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1433
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1663
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.424
_diffrn_reflns_theta_min         5.218
_diffrn_ambient_temperature      200.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                208
_reflns_number_total             227
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.376
_refine_diff_density_min         -2.377
_refine_diff_density_rms         0.329
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(4)
_refine_ls_extinction_coef       0.0009(2)
_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   1.116
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8
_refine_ls_number_reflns         227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0285
_refine_ls_restrained_S_all      1.116
_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)+(0.0175P)²+34.0845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0580
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.67(5)
 0.33(5)
2. Shared sites
{Ca02, Tb02}
3. Uiso/Uaniso restraints and constraints
Uiso(Ca02) = Uiso(Tb02)
4. Others
 Sof(Tb02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi01 Bi 0.625000 0.500000 0.250000 0.0102(4) Uani 1 4 d S T P . .
Ca02 Ca 0.5725(2) 0.4275(2) -0.0725(2) 0.0110(12) Uiso 0.837(10) 3 d S . P . 1
Tb02 Tb 0.5725(2) 0.4275(2) -0.0725(2) 0.0110(12) Uiso 0.163(10) 3 d S . P . 2


_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
Bi01 Ca02 3.203(2) 28_455 ?
Bi01 Ca02 3.428(2) 38_554 ?
Bi01 Ca02 3.428(2) 2_665 ?
Bi01 Ca02 3.428(2) 16_545 ?
Bi01 Ca02 3.203(2) 39_454 ?
Bi01 Ca02 3.428(2) 27_644 ?
Bi01 Ca02 3.203(2) 13 ?
Bi01 Ca02 3.203(2) . ?
Bi01 Tb02 3.203(2) . ?
Ca02 Ca02 4.1442(8) 38_554 ?
Ca02 Ca02 4.1441(8) 14_654 ?
Ca02 Ca02 3.670(2) 26_554 ?
Ca02 Ca02 3.670(2) 28_454 ?
Ca02 Ca02 3.670(2) 27_644 ?

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
Ca02 Bi01 Ca02 91.410(13) 28_455 13 ?
Ca02 Bi01 Ca02 130.84(5) 39_454 38_554 ?
Ca02 Bi01 Ca02 67.11(4) 39_454 16_545 ?
Ca02 Bi01 Ca02 67.11(4) 13 38_554 ?
Ca02 Bi01 Ca02 87.43(7) 13 27_644 ?
Ca02 Bi01 Ca02 64.736(5) 2_665 27_644 ?
Ca02 Bi01 Ca02 87.43(7) 28_455 38_554 ?
Ca02 Bi01 Ca02 91.411(13) 28_455 39_454 ?
Ca02 Bi01 Ca02 64.736(5) 16_545 38_554 ?
Ca02 Bi01 Ca02 130.84(5) 28_455 27_644 ?
Ca02 Bi01 Ca02 130.84(5) 13 16_545 ?
Ca02 Bi01 Ca02 161.95(9) 13 39_454 ?
Ca02 Bi01 Ca02 135.512(3) 2_665 38_554 ?
Ca02 Bi01 Ca02 135.512(3) 2_665 16_545 ?
Ca02 Bi01 Ca02 77.280(6) 13 2_665 ?
Ca02 Bi01 Ca02 161.95(9) 28_455 . ?
Ca02 Bi01 Ca02 87.43(7) 39_454 2_665 ?
Ca02 Bi01 Ca02 77.280(6) . 38_554 ?
Ca02 Bi01 Ca02 130.84(5) . 2_665 ?
Ca02 Bi01 Ca02 91.411(13) 13 . ?
Ca02 Bi01 Ca02 67.11(4) . 27_644 ?
Ca02 Bi01 Ca02 77.280(6) 39_454 27_644 ?
Ca02 Bi01 Ca02 135.512(3) 16_545 27_644 ?
Ca02 Bi01 Ca02 91.410(13) 39_454 . ?
Ca02 Bi01 Ca02 87.43(7) . 16_545 ?
Ca02 Bi01 Ca02 135.512(3) 38_554 27_644 ?
Ca02 Bi01 Ca02 67.11(4) 28_455 2_665 ?
Ca02 Bi01 Ca02 77.280(6) 28_455 16_545 ?
Tb02 Bi01 Ca02 77.280(6) . 38_554 ?
Tb02 Bi01 Ca02 87.43(7) . 16_545 ?
Bi01 Ca02 Bi01 88.65(7) 30_455 . ?
Bi01 Ca02 Bi01 84.846(7) 30_455 9_554 ?
Bi01 Ca02 Bi01 107.530(7) 10_655 9_554 ?
Bi01 Ca02 Bi01 162.36(3) 30_455 2_664 ?
Bi01 Ca02 Bi01 162.36(3) . 9_554 ?
Bi01 Ca02 Bi01 107.530(7) 30_455 29_544 ?
Bi01 Ca02 Bi01 162.36(3) 10_655 29_544 ?
Bi01 Ca02 Bi01 81.53(7) 9_554 2_664 ?
Bi01 Ca02 Bi01 84.846(6) . 29_544 ?
Bi01 Ca02 Bi01 88.65(7) 10_655 30_455 ?
Bi01 Ca02 Bi01 81.53(7) 2_664 29_544 ?
Bi01 Ca02 Bi01 81.53(7) 9_554 29_544 ?
Bi01 Ca02 Bi01 84.846(6) 10_655 2_664 ?
Bi01 Ca02 Bi01 88.65(7) 10_655 . ?
Bi01 Ca02 Bi01 107.530(7) . 2_664 ?
Bi01 Ca02 Ca02 59.37(4) 10_655 28_454 ?
Bi01 Ca02 Ca02 57.633(3) 9_554 26_554 ?
Bi01 Ca02 Ca02 144.11(10) 30_455 27_644 ?
Bi01 Ca02 Ca02 57.633(3) 29_544 27_644 ?
Bi01 Ca02 Ca02 53.52(7) 29_544 26_554 ?
Bi01 Ca02 Ca02 53.79(5) 30_455 38_554 ?
Bi01 Ca02 Ca02 57.633(3) 2_664 28_454 ?
Bi01 Ca02 Ca02 105.060(16) 30_455 28_454 ?
Bi01 Ca02 Ca02 120.45(11) 2_664 26_554 ?
Bi01 Ca02 Ca02 144.11(10) . 28_454 ?
Bi01 Ca02 Ca02 105.060(16) 10_655 27_644 ?
Bi01 Ca02 Ca02 131.07(4) 29_544 38_554 ?
Bi01 Ca02 Ca02 59.37(4) . 27_644 ?
Bi01 Ca02 Ca02 53.52(7) 9_554 28_454 ?
Bi01 Ca02 Ca02 126.21(5) 10_655 14_654 ?
Bi01 Ca02 Ca02 126.21(5) 30_455 14_654 ?
Bi01 Ca02 Ca02 126.21(5) . 14_654 ?
Bi01 Ca02 Ca02 120.45(11) 29_544 28_454 ?
Bi01 Ca02 Ca02 48.93(4) 2_664 14_654 ?
Bi01 Ca02 Ca02 48.93(4) 29_544 14_654 ?
Bi01 Ca02 Ca02 53.79(5) 10_655 38_554 ?
Bi01 Ca02 Ca02 144.11(10) 10_655 26_554 ?
Bi01 Ca02 Ca02 53.79(5) . 38_554 ?
Bi01 Ca02 Ca02 131.07(4) 9_554 38_554 ?
Bi01 Ca02 Ca02 131.07(4) 2_664 38_554 ?
Bi01 Ca02 Ca02 59.37(4) 30_455 26_554 ?
Bi01 Ca02 Ca02 120.45(11) 9_554 27_644 ?
Bi01 Ca02 Ca02 53.52(7) 2_664 27_644 ?
Bi01 Ca02 Ca02 105.060(16) . 26_554 ?
Bi01 Ca02 Ca02 48.93(4) 9_554 14_654 ?
Ca02 Ca02 Ca02 110.49(6) 28_454 27_644 ?
Ca02 Ca02 Ca02 71.57(7) 26_554 14_654 ?
Ca02 Ca02 Ca02 108.43(7) 27_644 38_554 ?
Ca02 Ca02 Ca02 71.57(7) 27_644 14_654 ?
Ca02 Ca02 Ca02 110.49(6) 28_454 26_554 ?
Ca02 Ca02 Ca02 108.43(7) 26_554 38_554 ?
Ca02 Ca02 Ca02 71.57(7) 28_454 14_654 ?
Ca02 Ca02 Ca02 110.49(6) 26_554 27_644 ?
Ca02 Ca02 Ca02 108.43(7) 28_454 38_554 ?
Ca02 Ca02 Ca02 180.0 14_654 38_554 ?
Bi01 Tb02 Bi01 107.530(7) 30_455 29_544 ?
Bi01 Tb02 Bi01 81.53(7) 9_554 2_664 ?
Bi01 Tb02 Bi01 162.36(3) 30_455 2_664 ?
Bi01 Tb02 Bi01 81.53(7) 9_554 29_544 ?
Bi01 Tb02 Bi01 81.53(7) 2_664 29_544 ?
Bi01 Tb02 Bi01 88.65(7) 30_455 . ?
Bi01 Tb02 Bi01 107.530(7) 10_655 9_554 ?
Bi01 Tb02 Bi01 84.846(6) . 29_544 ?
Bi01 Tb02 Bi01 84.846(7) 30_455 9_554 ?
Bi01 Tb02 Bi01 162.36(3) . 9_554 ?
Bi01 Tb02 Bi01 88.65(7) 10_655 30_455 ?
Bi01 Tb02 Bi01 162.36(3) 10_655 29_544 ?
Bi01 Tb02 Bi01 88.65(7) 10_655 . ?
Bi01 Tb02 Bi01 107.530(7) . 2_664 ?
Bi01 Tb02 Bi01 84.846(6) 10_655 2_664 ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.67(5)
2 0.33(5)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_test_svib1485
_database_code_depnum_ccdc_archive 'CCDC 2132693'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.29 Y0.71'
_chemical_formula_sum            'Bi3 Ca3.29 Y0.71'
_chemical_formula_weight         821.93
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Y Y -2.7962 3.5667 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.573(2)
_cell_length_b                   9.573(2)
_cell_length_c                   9.573(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     877.2(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    432
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      5.22
_shelx_estimated_absorpt_T_max   0.104
_shelx_estimated_absorpt_T_min   0.076
_exptl_absorpt_coefficient_mu    66.480
_exptl_absorpt_correction_T_max  0.2654
_exptl_absorpt_correction_T_min  0.1035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1513 before and 0.0743 after correction.
The Ratio of minimum to maximum transmission is 0.3900.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    6.223
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1370
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5.00 3.00 2.00 0.0410
4.00 -1.00 1.00 0.0210
5.00 -4.00 -4.00 0.0360
3.00 -4.00 5.00 0.0280
0.00 -5.00 -2.00 0.0450
0.00 1.00 -5.00 0.0300
3.00 5.00 1.00 0.0270
0.00 1.00 1.00 0.0200
-3.00 1.00 -4.00 0.0380
-3.00 3.00 -2.00 0.0270
0.00 -1.00 -1.00 0.0430
3.00 -4.00 1.00 0.0390
1.00 0.00 -1.00 0.0240
6.00 2.00 1.00 0.0150
0.00 -1.00 4.00 0.0220
-2.00 -4.00 1.00 0.0330
-3.00 -5.00 -3.00 0.0360

_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.062
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.416
_diffrn_reflns_theta_min         5.217
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                214
_reflns_number_total             228
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.00106(14)
_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   1.029
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0211
_refine_ls_restrained_S_all      1.029
_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)+(0.0048P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0361
_refine_ls_wR_factor_ref         0.0369
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.98(4)
 0.02(4)
2. Shared sites
{Ca, Y}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca) = Uanis(Y)
4. Others
 Sof(Y)=0.33333*(1-FVAR(2))
 Sof(Ca)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_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
Bi Bi 0.375000 0.000000 0.250000 0.0096(2) Uani 1 4 d S T P . .
Ca Ca 0.07284(19) 0.07284(19) 0.07284(19) 0.0107(10) Uani 0.823(18) 3 d S T P .
.
Y Y 0.07284(19) 0.07284(19) 0.07284(19) 0.0107(10) Uani 0.177(18) 3 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
Bi Ca 3.207(2) 39_444 ?
Bi Ca 3.425(2) 38_544 ?
Bi Ca 3.425(2) 28_445 ?
Bi Ca 3.425(2) . ?
Bi Ca 3.207(2) 2 ?
Bi Ca 3.425(2) 16_545 ?
Bi Ca 3.207(2) 13 ?
Bi Ca 3.207(2) 27_544 ?
Ca Ca 3.667(2) 28_445 ?
Ca Ca 3.667(2) 27_544 ?
Ca Ca 3.667(2) 26_454 ?
Ca Ca 4.1452(10) 37_444 ?
Ca Ca 4.1451(10) 13 ?

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
Ca Bi Ca 162.08(8) 39_444 13 ?
Ca Bi Ca 67.05(3) 2 28_445 ?
Ca Bi Ca 77.290(5) 2 38_544 ?
Ca Bi Ca 87.54(6) 13 28_445 ?
Ca Bi Ca 130.76(4) 39_444 38_544 ?
Ca Bi Ca 135.507(3) . 16_545 ?
Ca Bi Ca 77.290(5) 39_444 28_445 ?
Ca Bi Ca 91.389(12) 39_444 2 ?
Ca Bi Ca 64.744(5) . 28_445 ?
Ca Bi Ca 67.05(3) 39_444 16_545 ?
Ca Bi Ca 67.05(3) 13 38_544 ?
Ca Bi Ca 91.389(12) 13 2 ?
Ca Bi Ca 135.507(3) 38_544 28_445 ?
Ca Bi Ca 135.506(3) . 38_544 ?
Ca Bi Ca 77.289(5) 13 . ?
Ca Bi Ca 91.389(12) 39_444 27_544 ?
Ca Bi Ca 130.76(4) 2 . ?
Ca Bi Ca 130.76(4) 27_544 28_445 ?
Ca Bi Ca 67.05(3) 27_544 . ?
Ca Bi Ca 91.389(12) 13 27_544 ?
Ca Bi Ca 77.290(6) 27_544 16_545 ?
Ca Bi Ca 87.54(6) 2 16_545 ?
Ca Bi Ca 64.744(5) 38_544 16_545 ?
Ca Bi Ca 162.08(8) 2 27_544 ?
Ca Bi Ca 87.54(6) 27_544 38_544 ?
Ca Bi Ca 135.507(3) 28_445 16_545 ?
Ca Bi Ca 87.54(6) 39_444 . ?
Ca Bi Ca 130.76(4) 13 16_545 ?
Bi Ca Bi 88.53(6) 10_545 6_455 ?
Bi Ca Bi 81.64(6) . 5 ?
Bi Ca Bi 81.64(6) 5 9 ?
Bi Ca Bi 84.856(6) 2_554 5 ?
Bi Ca Bi 84.856(6) 6_455 9 ?
Bi Ca Bi 162.40(2) 2_554 9 ?
Bi Ca Bi 84.856(6) 10_545 . ?
Bi Ca Bi 88.53(6) 10_545 2_554 ?
Bi Ca Bi 162.40(2) 6_455 . ?
Bi Ca Bi 107.542(6) 10_545 9 ?
Bi Ca Bi 107.542(6) 2_554 . ?
Bi Ca Bi 88.53(6) 6_455 2_554 ?
Bi Ca Bi 81.64(6) . 9 ?
Bi Ca Bi 107.542(6) 6_455 5 ?
Bi Ca Bi 162.40(2) 10_545 5 ?
Bi Ca Ca 59.31(3) 10_545 28_445 ?
Bi Ca Ca 126.30(4) 10_545 13 ?
Bi Ca Ca 105.086(14) 10_545 27_544 ?
Bi Ca Ca 57.628(2) 5 27_544 ?
Bi Ca Ca 53.64(7) 5 26_454 ?
Bi Ca Ca 53.70(4) 6_455 37_444 ?
Bi Ca Ca 120.63(10) 9 27_544 ?
Bi Ca Ca 105.086(14) 6_455 28_445 ?
Bi Ca Ca 126.30(4) 2_554 13 ?
Bi Ca Ca 49.01(4) . 13 ?
Bi Ca Ca 57.628(2) 9 26_454 ?
Bi Ca Ca 143.95(9) 2_554 28_445 ?
Bi Ca Ca 143.95(9) 6_455 27_544 ?
Bi Ca Ca 130.99(4) 9 37_444 ?
Bi Ca Ca 59.31(3) 6_455 26_454 ?
Bi Ca Ca 57.628(2) . 28_445 ?
Bi Ca Ca 105.086(14) 2_554 26_454 ?
Bi Ca Ca 126.30(4) 6_455 13 ?
Bi Ca Ca 49.01(4) 5 13 ?
Bi Ca Ca 120.63(10) 5 28_445 ?
Bi Ca Ca 53.70(4) 10_545 37_444 ?
Bi Ca Ca 49.01(4) 9 13 ?
Bi Ca Ca 53.70(4) 2_554 37_444 ?
Bi Ca Ca 53.64(7) 9 28_445 ?
Bi Ca Ca 130.99(4) 5 37_444 ?
Bi Ca Ca 130.99(4) . 37_444 ?
Bi Ca Ca 59.31(3) 2_554 27_544 ?
Bi Ca Ca 143.95(9) 10_545 26_454 ?
Bi Ca Ca 53.64(7) . 27_544 ?
Bi Ca Ca 120.63(10) . 26_454 ?
Ca Ca Ca 108.33(6) 27_544 37_444 ?
Ca Ca Ca 180.0(2) 13 37_444 ?
Ca Ca Ca 71.67(6) 27_544 13 ?
Ca Ca Ca 71.67(6) 28_445 13 ?
Ca Ca Ca 110.59(6) 28_445 26_454 ?
Ca Ca Ca 108.33(6) 28_445 37_444 ?
Ca Ca Ca 108.33(6) 26_454 37_444 ?
Ca Ca Ca 110.59(6) 26_454 27_544 ?
Ca Ca Ca 110.59(6) 28_445 27_544 ?
Ca Ca Ca 71.67(6) 26_454 13 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.98(4)
2 0.02(4)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 2132688'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.33 Dy0.669'
_chemical_formula_sum            'Bi3 Ca3.33 Dy0.67'
_chemical_formula_weight         869.28
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Dy Dy -0.1892 4.4098 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.5538(15)
_cell_length_b                   9.5538(15)
_cell_length_c                   9.5538(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     872.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    758
_cell_measurement_temperature    200.02
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      5.23
_shelx_estimated_absorpt_T_max   0.158
_shelx_estimated_absorpt_T_min   0.023
_exptl_absorpt_coefficient_mu    67.899
_exptl_absorpt_correction_T_max  0.2656
_exptl_absorpt_correction_T_min  0.1374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1772 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.5173.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    6.621
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1439
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4.00 8.00 -1.00 0.0260
-9.00 -4.00 3.00 0.0100
8.00 0.00 -3.00 0.0210
9.00 5.00 -3.00 0.0250
-3.00 5.00 -1.00 0.0250
-3.00 0.00 2.00 0.0160

_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.043
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1688
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.483
_diffrn_reflns_theta_min         5.228
_diffrn_ambient_temperature      200.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                212
_reflns_number_total             222
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.199
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(2)
_refine_ls_extinction_coef       0.00113(9)
_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   1.097
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0208
_refine_ls_restrained_S_all      1.097
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0281
_refine_ls_wR_factor_ref         0.0288
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.67(2)
 0.33(2)
2. Shared sites
{Ca02, Dy02}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca02) = Uanis(Dy02)
4. Others
 Sof(Dy02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi01 Bi 0.875000 0.500000 0.750000 0.0096(2) Uani 1 4 d S T P . .
Ca02 Ca 0.07242(13) 0.07242(13) 0.07242(13) 0.0090(7) Uani 0.833(4) 3 d S T P .
1
Dy02 Dy 0.07242(13) 0.07242(13) 0.07242(13) 0.0090(7) Uani 0.167(4) 3 d S T P .
2


_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
Bi01 Ca02 3.1968(13) 15 ?
Bi01 Ca02 3.4225(15) 14_655 ?
Bi01 Ca02 3.4225(15) 40_545 ?
Bi01 Ca02 3.1968(13) 37 ?
Bi01 Ca02 3.4225(15) 25 ?
Bi01 Ca02 3.1968(13) 26 ?
Bi01 Ca02 3.1968(13) 3_655 ?
Bi01 Ca02 3.4225(15) 4_556 ?
Ca02 Ca02 3.6644(14) 28_445 ?
Ca02 Ca02 4.1369(7) 37_444 ?
Ca02 Ca02 4.1369(7) 13 ?
Ca02 Ca02 3.6644(14) 26_454 ?
Ca02 Ca02 3.6644(14) 27_544 ?

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
Ca02 Bi01 Ca02 161.92(5) 15 37 ?
Ca02 Bi01 Ca02 87.41(4) 37 4_556 ?
Ca02 Bi01 Ca02 64.734(3) 14_655 40_545 ?
Ca02 Bi01 Ca02 91.415(8) 15 26 ?
Ca02 Bi01 Ca02 67.13(2) 15 40_545 ?
Ca02 Bi01 Ca02 91.415(8) 37 26 ?
Ca02 Bi01 Ca02 135.513(2) 14_655 25 ?
Ca02 Bi01 Ca02 91.415(8) 15 3_655 ?
Ca02 Bi01 Ca02 130.85(3) 3_655 4_556 ?
Ca02 Bi01 Ca02 91.415(8) 37 3_655 ?
Ca02 Bi01 Ca02 87.41(4) 26 40_545 ?
Ca02 Bi01 Ca02 161.92(5) 26 3_655 ?
Ca02 Bi01 Ca02 135.513(2) 4_556 40_545 ?
Ca02 Bi01 Ca02 130.85(3) 15 14_655 ?
Ca02 Bi01 Ca02 77.277(4) 15 4_556 ?
Ca02 Bi01 Ca02 67.13(2) 37 14_655 ?
Ca02 Bi01 Ca02 67.13(2) 26 4_556 ?
Ca02 Bi01 Ca02 77.277(4) 26 14_655 ?
Ca02 Bi01 Ca02 135.513(2) 14_655 4_556 ?
Ca02 Bi01 Ca02 87.41(4) 3_655 14_655 ?
Ca02 Bi01 Ca02 130.85(3) 37 40_545 ?
Ca02 Bi01 Ca02 87.41(4) 15 25 ?
Ca02 Bi01 Ca02 77.277(4) 3_655 40_545 ?
Ca02 Bi01 Ca02 77.277(4) 37 25 ?
Ca02 Bi01 Ca02 135.513(2) 25 40_545 ?
Ca02 Bi01 Ca02 130.85(3) 26 25 ?
Ca02 Bi01 Ca02 67.13(2) 3_655 25 ?
Ca02 Bi01 Ca02 64.734(3) 25 4_556 ?
Bi01 Ca02 Bi01 88.67(4) 30_355 34_535 ?
Bi01 Ca02 Bi01 81.51(4) 29_444 25_444 ?
Bi01 Ca02 Bi01 81.51(4) 29_444 33_444 ?
Bi01 Ca02 Bi01 88.67(4) 30_355 26_553 ?
Bi01 Ca02 Bi01 107.528(4) 34_535 33_444 ?
Bi01 Ca02 Bi01 88.67(4) 34_535 26_553 ?
Bi01 Ca02 Bi01 107.528(4) 26_553 25_444 ?
Bi01 Ca02 Bi01 107.528(4) 30_355 29_444 ?
Bi01 Ca02 Bi01 84.843(4) 30_355 33_444 ?
Bi01 Ca02 Bi01 162.349(16) 34_535 29_444 ?
Bi01 Ca02 Bi01 162.349(16) 26_553 33_444 ?
Bi01 Ca02 Bi01 84.843(4) 26_553 29_444 ?
Bi01 Ca02 Bi01 81.51(4) 25_444 33_444 ?
Bi01 Ca02 Bi01 162.349(16) 30_355 25_444 ?
Bi01 Ca02 Bi01 84.843(4) 34_535 25_444 ?
Bi01 Ca02 Ca02 105.055(10) 30_355 28_445 ?
Bi01 Ca02 Ca02 120.41(7) 33_444 27_544 ?
Bi01 Ca02 Ca02 53.80(3) 34_535 37_444 ?
Bi01 Ca02 Ca02 59.38(2) 34_535 28_445 ?
Bi01 Ca02 Ca02 48.92(3) 29_444 13 ?
Bi01 Ca02 Ca02 144.14(6) 26_553 28_445 ?
Bi01 Ca02 Ca02 131.08(3) 33_444 37_444 ?
Bi01 Ca02 Ca02 120.41(7) 29_444 28_445 ?
Bi01 Ca02 Ca02 126.20(3) 34_535 13 ?
Bi01 Ca02 Ca02 57.633(1) 25_444 28_445 ?
Bi01 Ca02 Ca02 48.92(3) 33_444 13 ?
Bi01 Ca02 Ca02 59.38(2) 30_355 26_454 ?
Bi01 Ca02 Ca02 131.08(3) 29_444 37_444 ?
Bi01 Ca02 Ca02 144.14(6) 34_535 26_454 ?
Bi01 Ca02 Ca02 53.49(4) 25_444 27_544 ?
Bi01 Ca02 Ca02 105.055(10) 26_553 26_454 ?
Bi01 Ca02 Ca02 126.20(3) 30_355 13 ?
Bi01 Ca02 Ca02 53.49(4) 29_444 26_454 ?
Bi01 Ca02 Ca02 126.20(3) 26_553 13 ?
Bi01 Ca02 Ca02 120.41(7) 25_444 26_454 ?
Bi01 Ca02 Ca02 48.92(3) 25_444 13 ?
Bi01 Ca02 Ca02 57.633(1) 33_444 26_454 ?
Bi01 Ca02 Ca02 53.80(3) 30_355 37_444 ?
Bi01 Ca02 Ca02 144.14(6) 30_355 27_544 ?
Bi01 Ca02 Ca02 53.80(3) 26_553 37_444 ?
Bi01 Ca02 Ca02 105.055(10) 34_535 27_544 ?
Bi01 Ca02 Ca02 131.08(3) 25_444 37_444 ?
Bi01 Ca02 Ca02 59.38(2) 26_553 27_544 ?
Bi01 Ca02 Ca02 57.633(1) 29_444 27_544 ?
Bi01 Ca02 Ca02 53.49(4) 33_444 28_445 ?
Ca02 Ca02 Ca02 110.47(4) 28_445 27_544 ?
Ca02 Ca02 Ca02 71.54(4) 27_544 13 ?
Ca02 Ca02 Ca02 108.46(4) 26_454 37_444 ?
Ca02 Ca02 Ca02 110.47(4) 26_454 27_544 ?
Ca02 Ca02 Ca02 108.46(4) 28_445 37_444 ?
Ca02 Ca02 Ca02 110.47(4) 28_445 26_454 ?
Ca02 Ca02 Ca02 108.46(4) 27_544 37_444 ?
Ca02 Ca02 Ca02 71.54(4) 28_445 13 ?
Ca02 Ca02 Ca02 71.54(4) 26_454 13 ?
Ca02 Ca02 Ca02 180.00(14) 13 37_444 ?
Bi01 Dy02 Bi01 84.843(4) 30_355 33_444 ?
Bi01 Dy02 Bi01 107.528(4) 26_553 25_444 ?
Bi01 Dy02 Bi01 162.349(16) 30_355 25_444 ?
Bi01 Dy02 Bi01 162.349(16) 26_553 33_444 ?
Bi01 Dy02 Bi01 84.843(4) 26_553 29_444 ?
Bi01 Dy02 Bi01 81.51(4) 25_444 33_444 ?
Bi01 Dy02 Bi01 84.843(4) 34_535 25_444 ?
Bi01 Dy02 Bi01 107.528(4) 30_355 29_444 ?
Bi01 Dy02 Bi01 81.51(4) 29_444 25_444 ?
Bi01 Dy02 Bi01 162.349(16) 34_535 29_444 ?
Bi01 Dy02 Bi01 107.528(4) 34_535 33_444 ?
Bi01 Dy02 Bi01 88.67(4) 30_355 34_535 ?
Bi01 Dy02 Bi01 81.51(4) 29_444 33_444 ?
Bi01 Dy02 Bi01 88.67(4) 30_355 26_553 ?
Bi01 Dy02 Bi01 88.67(4) 34_535 26_553 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.67(2)
2 0.33(2)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_test_svib1492
_database_code_depnum_ccdc_archive 'CCDC 2132690'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.401 Er0.599'
_chemical_formula_sum            'Bi3 Ca3.40 Er0.60'
_chemical_formula_weight         863.57
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Er Er -0.2586 4.9576 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.575(5)
_cell_length_b                   9.575(5)
_cell_length_c                   9.575(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     877.8(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    749
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      5.22
_shelx_estimated_absorpt_T_max   0.095
_shelx_estimated_absorpt_T_min   0.050
_exptl_absorpt_coefficient_mu    67.538
_exptl_absorpt_correction_T_max  0.0996
_exptl_absorpt_correction_T_min  0.0406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1436 before and 0.0577 after correction. The Ratio of minimum to maximum transmission is 0.4076. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    6.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1431
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3.00 2.00 -3.00 0.0090
-3.00 -5.00 -2.00 0.0450
-3.00 -2.00 3.00 0.0520
-1.00 1.00 4.00 0.0490
1.00 3.00 3.00 0.0470
-1.00 -7.00 -1.00 0.0520
-1.00 -5.00 -7.00 0.0490
0.00 1.00 -7.00 0.0270
1.00 6.00 -1.00 0.0290
0.00 -1.00 7.00 0.0520
5.00 -3.00 2.00 0.0300
-5.00 2.00 -3.00 0.0330
-3.00 5.00 2.00 0.0400
5.00 -1.00 4.00 0.0310
3.00 -5.00 -2.00 0.0420

_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.066
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1769
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.229
_diffrn_reflns_theta_min         5.216
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                213
_reflns_number_total             222
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.68(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8
_refine_ls_number_reflns         222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0170
_refine_ls_R_factor_gt           0.0158
_refine_ls_restrained_S_all      1.060
_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)+(0.0142P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0325
_refine_ls_wR_factor_ref         0.0329
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.32(2)
 0.68(2)
2. Shared sites
{Ca, Er}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca) = Uanis(Er)
4. Others
 Sof(Er)=0.33333*(1-FVAR(2))
 Sof(Ca)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
Bi Bi 0.375000 0.000000 0.250000 0.01406(16) Uani 1 4 d S T P . .
Ca Ca 0.07257(11) 0.07257(11) 0.07257(11) 0.0117(6) Uani 0.850(5) 3 d S T P . .
Er Er 0.07257(11) 0.07257(11) 0.07257(11) 0.0117(6) Uani 0.150(5) 3 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
Bi Ca 3.205(2) 39_444 ?
Bi Ca 3.428(2) 38_544 ?
Bi Ca 3.428(2) . ?
Bi Ca 3.205(2) 13 ?
Bi Ca 3.428(2) 28_445 ?
Bi Ca 3.205(2) 2 ?
Bi Ca 3.205(2) 27_544 ?
Bi Ca 3.428(2) 16_545 ?
Ca Ca 3.671(2) 28_445 ?
Ca Ca 4.146(2) 13 ?
Ca Ca 4.146(2) 37_444 ?
Ca Ca 3.671(2) 26_454 ?
Ca Ca 3.671(2) 27_544 ?

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
Ca Bi Ca 161.98(4) 39_444 13 ?
Ca Bi Ca 130.82(2) 13 16_545 ?
Ca Bi Ca 135.511(2) 38_544 . ?
Ca Bi Ca 91.406(7) 39_444 2 ?
Ca Bi Ca 87.45(3) 39_444 . ?
Ca Bi Ca 91.406(7) 13 2 ?
Ca Bi Ca 135.511(2) 38_544 28_445 ?
Ca Bi Ca 91.406(7) 39_444 27_544 ?
Ca Bi Ca 77.282(3) 27_544 16_545 ?
Ca Bi Ca 91.406(7) 13 27_544 ?
Ca Bi Ca 130.82(2) 2 . ?
Ca Bi Ca 161.98(4) 2 27_544 ?
Ca Bi Ca 135.511(2) 16_545 . ?
Ca Bi Ca 130.82(2) 39_444 38_544 ?
Ca Bi Ca 67.10(2) 39_444 16_545 ?
Ca Bi Ca 67.10(2) 13 38_544 ?
Ca Bi Ca 87.45(3) 2 16_545 ?
Ca Bi Ca 77.282(3) 2 38_544 ?
Ca Bi Ca 64.738(2) 38_544 16_545 ?
Ca Bi Ca 87.45(3) 27_544 38_544 ?
Ca Bi Ca 77.282(3) 13 . ?
Ca Bi Ca 77.282(3) 39_444 28_445 ?
Ca Bi Ca 67.10(2) 27_544 . ?
Ca Bi Ca 87.45(3) 13 28_445 ?
Ca Bi Ca 64.738(3) 28_445 . ?
Ca Bi Ca 67.10(2) 2 28_445 ?
Ca Bi Ca 130.82(2) 27_544 28_445 ?
Ca Bi Ca 135.511(2) 28_445 16_545 ?
Bi Ca Bi 88.62(4) 10_545 6_455 ?
Bi Ca Bi 107.533(4) 2_554 . ?
Bi Ca Bi 162.367(13) 2_554 9 ?
Bi Ca Bi 88.62(4) 10_545 2_554 ?
Bi Ca Bi 107.533(4) 10_545 9 ?
Bi Ca Bi 88.62(4) 6_455 2_554 ?
Bi Ca Bi 162.367(13) 6_455 . ?
Bi Ca Bi 162.367(13) 10_545 5 ?
Bi Ca Bi 81.55(3) 5 . ?
Bi Ca Bi 107.533(4) 6_455 5 ?
Bi Ca Bi 84.848(3) 6_455 9 ?
Bi Ca Bi 84.848(3) 2_554 5 ?
Bi Ca Bi 81.55(3) . 9 ?
Bi Ca Bi 84.848(3) 10_545 . ?
Bi Ca Bi 81.55(3) 5 9 ?
Bi Ca Ca 59.354(17) 10_545 28_445 ?
Bi Ca Ca 53.55(4) . 27_544 ?
Bi Ca Ca 126.23(3) 6_455 13 ?
Bi Ca Ca 105.066(8) 6_455 28_445 ?
Bi Ca Ca 131.05(2) 5 37_444 ?
Bi Ca Ca 144.08(5) 2_554 28_445 ?
Bi Ca Ca 48.95(2) 9 13 ?
Bi Ca Ca 120.49(6) 5 28_445 ?
Bi Ca Ca 53.77(3) 6_455 37_444 ?
Bi Ca Ca 57.631(1) . 28_445 ?
Bi Ca Ca 131.05(2) 9 37_444 ?
Bi Ca Ca 53.55(4) 9 28_445 ?
Bi Ca Ca 48.95(2) 5 13 ?
Bi Ca Ca 144.08(5) 10_545 26_454 ?
Bi Ca Ca 57.631(1) 5 27_544 ?
Bi Ca Ca 59.354(17) 6_455 26_454 ?
Bi Ca Ca 53.77(3) 10_545 37_444 ?
Bi Ca Ca 105.066(8) 2_554 26_454 ?
Bi Ca Ca 53.77(3) 2_554 37_444 ?
Bi Ca Ca 53.55(4) 5 26_454 ?
Bi Ca Ca 131.05(2) . 37_444 ?
Bi Ca Ca 120.49(6) . 26_454 ?
Bi Ca Ca 126.23(3) 10_545 13 ?
Bi Ca Ca 57.631(1) 9 26_454 ?
Bi Ca Ca 126.23(3) 2_554 13 ?
Bi Ca Ca 105.066(8) 10_545 27_544 ?
Bi Ca Ca 48.95(2) . 13 ?
Bi Ca Ca 144.08(5) 6_455 27_544 ?
Bi Ca Ca 59.354(17) 2_554 27_544 ?
Bi Ca Ca 120.49(6) 9 27_544 ?
Ca Ca Ca 71.59(3) 27_544 13 ?
Ca Ca Ca 108.41(3) 28_445 37_444 ?
Ca Ca Ca 71.59(3) 28_445 13 ?
Ca Ca Ca 110.51(3) 26_454 27_544 ?
Ca Ca Ca 108.41(3) 26_454 37_444 ?
Ca Ca Ca 110.51(3) 28_445 26_454 ?
Ca Ca Ca 108.41(3) 27_544 37_444 ?
Ca Ca Ca 71.59(3) 26_454 13 ?
Ca Ca Ca 180.00(11) 37_444 13 ?
Ca Ca Ca 110.51(3) 28_445 27_544 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.32(2)
2 0.68(2)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_svib1540_0m
_database_code_depnum_ccdc_archive 'CCDC 2132692'
loop_
_audit_author_name
_audit_author_address
'Svilen Bobev'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-01-05 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_audit_creation_date             2021-10-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 Ca3.461 Lu0.539'
_chemical_formula_sum            'Bi3 Ca3.47 Lu0.53'
_chemical_formula_weight         858.75
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 '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'
Lu Lu -0.4720 5.8584 '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      cubic
_space_group_IT_number           220
_space_group_name_H-M_alt        'I -4 3 d'
_space_group_name_Hall           'I -4bd 2c 3'
loop_
_space_group_symop_operation_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+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+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, 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+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+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, x+5/4'

_cell_length_a                   9.555(2)
_cell_length_b                   9.555(2)
_cell_length_c                   9.555(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     872.5(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    308
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      5.23
_shelx_estimated_absorpt_T_max   0.120
_shelx_estimated_absorpt_T_min   0.058
_exptl_absorpt_coefficient_mu    68.225
_exptl_absorpt_correction_T_max  0.2656
_exptl_absorpt_correction_T_min  0.1576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1238 before and 0.0438 after correction.
The Ratio of minimum to maximum transmission is 0.5934.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    6.538
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -2.00 -3.00 0.0180
1.00 0.00 0.00 0.0280
2.00 -2.00 -3.00 0.0270
0.00 1.00 0.00 0.0210
3.00 -3.00 2.00 0.0340
0.00 -1.00 0.00 0.0360
3.00 3.00 2.00 0.0200
3.00 1.00 1.00 0.0220
-2.00 1.00 3.00 0.0230
1.00 4.00 -4.00 0.0300
-2.00 1.00 -4.00 0.0200
-4.00 1.00 -2.00 0.0100

_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.054
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1873
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.478
_diffrn_reflns_theta_min         5.227
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                210
_reflns_number_total             228
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.232
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8
_refine_ls_number_reflns         228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0224P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0488
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.52(4)
 0.48(4)
2. Shared sites
{Ca02, Lu02}
3. Uiso/Uaniso restraints and constraints
Uanis(Ca02) = Uanis(Lu02)
4. Others
 Sof(Lu02)=0.33333*(1-FVAR(2))
 Sof(Ca02)=0.33333*FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_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
Bi01 Bi 0.125000 0.500000 0.250000 0.0142(2) Uani 1 4 d S T P . .
Ca02 Ca 0.17686(18) 0.82314(18) 0.32314(18) 0.0124(10) Uani 0.865(6) 3 d S T P
. 1
Lu02 Lu 0.17686(18) 0.82314(18) 0.32314(18) 0.0124(10) Uani 0.135(6) 3 d S T P
. 2


_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
Bi01 Ca02 3.2043(19) 39_354 ?
Bi01 Ca02 3.415(2) 40_545 ?
Bi01 Ca02 3.415(2) 3_545 ?
Bi01 Ca02 3.415(2) 26_464 ?
Bi01 Ca02 3.2044(19) . ?
Bi01 Ca02 3.415(2) 14_654 ?
Bi01 Ca02 3.2043(19) 13_455 ?
Bi01 Ca02 3.2044(19) 28_455 ?
Bi01 Lu02 3.2044(19) . ?
Ca02 Ca02 4.1376(9) 38_554 ?
Ca02 Ca02 4.1376(9) 14_654 ?
Ca02 Ca02 3.658(2) 26_464 ?
Ca02 Ca02 3.658(2) 28_465 ?
Ca02 Ca02 3.658(2) 27_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
Ca02 Bi01 Ca02 162.21(7) 39_354 13_455 ?
Ca02 Bi01 Ca02 87.63(6) . 40_545 ?
Ca02 Bi01 Ca02 66.99(3) . 26_464 ?
Ca02 Bi01 Ca02 66.99(3) 13_455 40_545 ?
Ca02 Bi01 Ca02 130.70(4) 13_455 14_654 ?
Ca02 Bi01 Ca02 135.502(3) 3_545 14_654 ?
Ca02 Bi01 Ca02 130.70(4) 39_354 40_545 ?
Ca02 Bi01 Ca02 91.370(11) 39_354 . ?
Ca02 Bi01 Ca02 135.501(3) 3_545 40_545 ?
Ca02 Bi01 Ca02 66.99(3) 39_354 14_654 ?
Ca02 Bi01 Ca02 77.299(5) 13_455 26_464 ?
Ca02 Bi01 Ca02 91.371(11) 13_455 . ?
Ca02 Bi01 Ca02 135.502(3) 26_464 40_545 ?
Ca02 Bi01 Ca02 64.751(4) 3_545 26_464 ?
Ca02 Bi01 Ca02 87.63(6) 13_455 3_545 ?
Ca02 Bi01 Ca02 91.371(11) 39_354 28_455 ?
Ca02 Bi01 Ca02 130.70(4) . 3_545 ?
Ca02 Bi01 Ca02 77.299(5) 28_455 40_545 ?
Ca02 Bi01 Ca02 66.99(3) 28_455 3_545 ?
Ca02 Bi01 Ca02 91.369(11) 13_455 28_455 ?
Ca02 Bi01 Ca02 87.63(5) 28_455 14_654 ?
Ca02 Bi01 Ca02 77.298(5) . 14_654 ?
Ca02 Bi01 Ca02 135.501(3) 26_464 14_654 ?
Ca02 Bi01 Ca02 162.21(7) . 28_455 ?
Ca02 Bi01 Ca02 130.70(4) 28_455 26_464 ?
Ca02 Bi01 Ca02 64.753(5) 40_545 14_654 ?
Ca02 Bi01 Ca02 77.299(5) 39_354 3_545 ?
Ca02 Bi01 Ca02 87.63(5) 39_354 26_464 ?
Lu02 Bi01 Ca02 77.298(5) . 14_654 ?
Lu02 Bi01 Ca02 87.63(6) . 40_545 ?
Bi01 Ca02 Bi01 81.73(6) 26_464 33_455 ?
Bi01 Ca02 Bi01 107.552(6) . 26_464 ?
Bi01 Ca02 Bi01 84.865(5) 30_455 26_464 ?
Bi01 Ca02 Bi01 162.44(2) . 5_565 ?
Bi01 Ca02 Bi01 162.44(2) 10_655 26_464 ?
Bi01 Ca02 Bi01 81.73(6) 5_565 33_455 ?
Bi01 Ca02 Bi01 162.44(2) 30_455 33_455 ?
Bi01 Ca02 Bi01 81.73(6) 26_464 5_565 ?
Bi01 Ca02 Bi01 107.552(6) 10_655 33_455 ?
Bi01 Ca02 Bi01 84.865(5) . 33_455 ?
Bi01 Ca02 Bi01 88.43(6) . 10_655 ?
Bi01 Ca02 Bi01 88.43(6) 30_455 . ?
Bi01 Ca02 Bi01 107.552(6) 30_455 5_565 ?
Bi01 Ca02 Bi01 88.43(6) 30_455 10_655 ?
Bi01 Ca02 Bi01 84.865(5) 10_655 5_565 ?
Bi01 Ca02 Ca02 59.26(3) 30_455 28_465 ?
Bi01 Ca02 Ca02 53.75(6) 26_464 26_464 ?
Bi01 Ca02 Ca02 105.109(13) . 27_545 ?
Bi01 Ca02 Ca02 53.75(6) 33_455 27_545 ?
Bi01 Ca02 Ca02 57.625(2) 33_455 26_464 ?
Bi01 Ca02 Ca02 126.37(4) . 38_554 ?
Bi01 Ca02 Ca02 53.75(6) 5_565 28_465 ?
Bi01 Ca02 Ca02 143.82(8) . 28_465 ?
Bi01 Ca02 Ca02 120.79(9) 5_565 26_464 ?
Bi01 Ca02 Ca02 105.109(13) 10_655 28_465 ?
Bi01 Ca02 Ca02 143.81(8) 30_455 27_545 ?
Bi01 Ca02 Ca02 49.07(4) 33_455 38_554 ?
Bi01 Ca02 Ca02 59.26(3) 10_655 27_545 ?
Bi01 Ca02 Ca02 57.624(2) 26_464 28_465 ?
Bi01 Ca02 Ca02 53.63(4) 30_455 14_654 ?
Bi01 Ca02 Ca02 53.63(4) . 14_654 ?
Bi01 Ca02 Ca02 53.63(4) 10_655 14_654 ?
Bi01 Ca02 Ca02 120.79(9) 33_455 28_465 ?
Bi01 Ca02 Ca02 130.93(4) 5_565 14_654 ?
Bi01 Ca02 Ca02 130.93(4) 33_455 14_654 ?
Bi01 Ca02 Ca02 126.37(4) 30_455 38_554 ?
Bi01 Ca02 Ca02 105.108(13) 30_455 26_464 ?
Bi01 Ca02 Ca02 126.37(4) 10_655 38_554 ?
Bi01 Ca02 Ca02 49.07(4) 26_464 38_554 ?
Bi01 Ca02 Ca02 49.07(4) 5_565 38_554 ?
Bi01 Ca02 Ca02 59.26(3) . 26_464 ?
Bi01 Ca02 Ca02 120.79(9) 26_464 27_545 ?
Bi01 Ca02 Ca02 57.624(2) 5_565 27_545 ?
Bi01 Ca02 Ca02 143.81(8) 10_655 26_464 ?
Bi01 Ca02 Ca02 130.93(4) 26_464 14_654 ?
Ca02 Ca02 Ca02 110.68(5) 28_465 27_545 ?
Ca02 Ca02 Ca02 108.23(5) 26_464 14_654 ?
Ca02 Ca02 Ca02 71.77(6) 27_545 38_554 ?
Ca02 Ca02 Ca02 108.23(5) 27_545 14_654 ?
Ca02 Ca02 Ca02 110.68(5) 28_465 26_464 ?
Ca02 Ca02 Ca02 71.77(6) 26_464 38_554 ?
Ca02 Ca02 Ca02 108.23(6) 28_465 14_654 ?
Ca02 Ca02 Ca02 110.68(5) 26_464 27_545 ?
Ca02 Ca02 Ca02 71.77(6) 28_465 38_554 ?
Ca02 Ca02 Ca02 180.0 14_654 38_554 ?
Bi01 Lu02 Bi01 84.865(5) . 33_455 ?
Bi01 Lu02 Bi01 81.73(6) 26_464 5_565 ?
Bi01 Lu02 Bi01 162.44(2) . 5_565 ?
Bi01 Lu02 Bi01 81.73(6) 26_464 33_455 ?
Bi01 Lu02 Bi01 81.73(6) 5_565 33_455 ?
Bi01 Lu02 Bi01 88.43(6) . 10_655 ?
Bi01 Lu02 Bi01 84.865(5) 30_455 26_464 ?
Bi01 Lu02 Bi01 107.552(6) 10_655 33_455 ?
Bi01 Lu02 Bi01 107.552(6) . 26_464 ?
Bi01 Lu02 Bi01 162.44(2) 10_655 26_464 ?
Bi01 Lu02 Bi01 88.43(6) 30_455 . ?
Bi01 Lu02 Bi01 162.44(2) 30_455 33_455 ?
Bi01 Lu02 Bi01 88.43(6) 30_455 10_655 ?
Bi01 Lu02 Bi01 84.865(5) 10_655 5_565 ?
Bi01 Lu02 Bi01 107.552(6) 30_455 5_565 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.52(4)
2 0.48(4)

