# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_Cd5P2SmCl7
_database_code_depnum_ccdc_archive 'CCDC 2235035'
loop_
_audit_author_name
_audit_author_address
'Zhi-Xin Qiu'
;Fujian Institute of Research on the Structure  of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-01-29 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelxl_version_number           2013-2
_chemical_name_common            Cd5P2SmCl7
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         Cd5P2SmCl7
_chemical_formula_sum            'Cd5 Cl7 P2 Sm'
_chemical_formula_weight         1022.50
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   13.350(4)
_cell_length_b                   13.350(4)
_cell_length_c                   7.308(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1128.0(9)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    1610
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.199
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.516
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_description       lamellar
_exptl_crystal_F_000             1353
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.074
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8267
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.298
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Pilatus CCD'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1045
_reflns_number_total             1325
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_refine_diff_density_max         2.377
_refine_diff_density_min         -2.265
_refine_diff_density_rms         0.312
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0611
_refine_ls_restrained_S_all      1.005
_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)+(0.0923P)²+34.0188P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1810
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Sof: Sm1(0.29) Sm1B(0.043333) Sm2(0.166667) Cl7(0.166667)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.3333 0.6667 0.0647(3) 0.0244(5) Uani 0.87 3 d S T P . .
Sm1B Sm 0.3333 0.6667 0.9648(18) 0.025(3) Uani 0.13 3 d S T P . .
Sm2 Sm 0.0000 0.0000 0.0610(3) 0.0277(7) Uani 0.5 3 d S T P . .
Cl3 Cl 0.4998(3) 0.3294(3) 0.1713(5) 0.0328(9) Uani 1 1 d . . . . .
Cl4 Cl 0.3378(4) 0.4785(4) 0.1751(6) 0.0488(11) Uani 1 1 d . . . . .
Cl5 Cl 0.1801(4) 0.1709(4) 0.1742(6) 0.0477(11) Uani 1 1 d . . . . .
Cl6 Cl 0.3333 0.6667 0.4412(15) 0.097(4) Uani 1 3 d S T P . .
Cl7 Cl 0.0000 0.0000 0.441(2) 0.101(8) Uani 0.5 3 d S T P . .
Cd8 Cd 0.01606(12) 0.34000(11) 0.03779(16) 0.0531(5) Uani 1 1 d . . . . .
Cd9 Cd 0.5000 0.0000 0.5000 0.0776(9) Uani 1 2 d S . P . .
Cd10 Cd 0.33360(18) 0.16453(13) 0.4902(2) 0.0750(7) Uani 1 1 d . . . . .
P11 P 0.0060(3) 0.3363(3) 0.3699(5) 0.0213(8) Uani 1 1 d . . . . .


_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
Sm1 Sm1B 0.730(11) 1_554 ?
Sm1 Cl3 2.798(4) 4_665 ?
Sm1 Cl3 2.798(4) 6 ?
Sm1 Cl3 2.798(4) 5_565 ?
Sm1 Cl4 2.668(4) 3_565 ?
Sm1 Cl4 2.668(4) . ?
Sm1 Cl4 2.668(4) 2_665 ?
Sm1 Cl6 2.751(11) . ?
Sm1B Sm1 0.730(11) 1_556 ?
Sm1B Cl3 2.417(6) 5_566 ?
Sm1B Cl3 2.417(6) 4_666 ?
Sm1B Cl3 2.417(6) 6_556 ?
Sm1B Cl4 2.971(8) 3_566 ?
Sm1B Cl4 2.971(8) 1_556 ?
Sm1B Cl4 2.971(8) 2_666 ?
Sm2 Sm2 0.891(5) 4 ?
Sm2 Cl5 2.908(5) 5 ?
Sm2 Cl5 2.487(5) . ?
Sm2 Cl5 2.908(5) 6 ?
Sm2 Cl5 2.487(5) 2 ?
Sm2 Cl5 2.487(5) 3 ?
Sm2 Cl5 2.908(5) 4 ?
Sm2 Cl7 2.774(18) . ?
Cl3 Sm1 2.798(4) 4_665 ?
Cl3 Sm1B 2.417(6) 4_666 ?
Cl3 Cd8 2.595(4) 5 ?
Cl4 Sm1B 2.971(8) 1_554 ?
Cl4 Cd8 2.596(5) 5 ?
Cl5 Sm2 2.908(5) 4 ?
Cl5 Cd8 2.601(5) 5 ?
Cl7 Cl7 0.87(3) 4_556 ?
Cd8 Cl3 2.595(4) 6 ?
Cd8 Cl4 2.596(5) 6 ?
Cd8 Cl5 2.601(5) 6 ?
Cd8 P11 2.430(4) . ?
Cd9 P11 2.422(3) 6_656 ?
Cd9 P11 2.422(3) 3 ?
Cd10 P11 2.420(3) 3 ?
Cd10 P11 2.421(3) 5_556 ?
P11 Cd9 2.422(3) 2 ?
P11 Cd10 2.420(3) 2 ?
P11 Cd10 2.421(3) 6_556 ?

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
Sm1B Sm1 Cl3 51.94(8) 1_554 6 ?
Sm1B Sm1 Cl3 51.94(8) 1_554 4_665 ?
Sm1B Sm1 Cl3 51.93(8) 1_554 5_565 ?
Sm1B Sm1 Cl4 107.61(11) 1_554 . ?
Sm1B Sm1 Cl4 107.61(11) 1_554 2_665 ?
Sm1B Sm1 Cl4 107.60(11) 1_554 3_565 ?
Sm1B Sm1 Cl6 180.0 1_554 . ?
Cl3 Sm1 Cl3 85.97(12) 5_565 6 ?
Cl3 Sm1 Cl3 85.97(12) 6 4_665 ?
Cl3 Sm1 Cl3 85.97(12) 5_565 4_665 ?
Cl4 Sm1 Cl3 79.11(13) 3_565 5_565 ?
Cl4 Sm1 Cl3 159.54(14) 2_665 6 ?
Cl4 Sm1 Cl3 79.11(13) 2_665 4_665 ?
Cl4 Sm1 Cl3 79.13(12) 2_665 5_565 ?
Cl4 Sm1 Cl3 159.54(14) 3_565 4_665 ?
Cl4 Sm1 Cl3 159.54(14) . 5_565 ?
Cl4 Sm1 Cl3 79.13(12) . 4_665 ?
Cl4 Sm1 Cl3 79.13(12) 3_565 6 ?
Cl4 Sm1 Cl3 79.11(13) . 6 ?
Cl4 Sm1 Cl4 111.27(10) 3_565 2_665 ?
Cl4 Sm1 Cl4 111.27(10) 3_565 . ?
Cl4 Sm1 Cl4 111.27(10) 2_665 . ?
Cl4 Sm1 Cl6 72.39(11) 2_665 . ?
Cl4 Sm1 Cl6 72.39(11) 3_565 . ?
Cl4 Sm1 Cl6 72.39(11) . . ?
Cl6 Sm1 Cl3 128.06(8) . 4_665 ?
Cl6 Sm1 Cl3 128.06(8) . 5_565 ?
Cl6 Sm1 Cl3 128.06(8) . 6 ?
Sm1 Sm1B Cl3 114.3(3) 1_556 6_556 ?
Sm1 Sm1B Cl3 114.3(3) 1_556 5_566 ?
Sm1 Sm1B Cl3 114.3(3) 1_556 4_666 ?
Sm1 Sm1B Cl4 58.8(2) 1_556 3_566 ?
Sm1 Sm1B Cl4 58.8(2) 1_556 1_556 ?
Sm1 Sm1B Cl4 58.8(2) 1_556 2_666 ?
Cl3 Sm1B Cl3 104.2(3) 5_566 4_666 ?
Cl3 Sm1B Cl3 104.2(3) 6_556 4_666 ?
Cl3 Sm1B Cl3 104.2(3) 5_566 6_556 ?
Cl3 Sm1B Cl4 79.82(14) 6_556 3_566 ?
Cl3 Sm1B Cl4 79.79(14) 5_566 3_566 ?
Cl3 Sm1B Cl4 173.1(5) 5_566 1_556 ?
Cl3 Sm1B Cl4 173.1(5) 4_666 3_566 ?
Cl3 Sm1B Cl4 79.82(13) 4_666 1_556 ?
Cl3 Sm1B Cl4 79.79(14) 6_556 1_556 ?
Cl3 Sm1B Cl4 79.82(14) 5_566 2_666 ?
Cl3 Sm1B Cl4 79.79(14) 4_666 2_666 ?
Cl3 Sm1B Cl4 173.1(5) 6_556 2_666 ?
Cl4 Sm1B Cl4 95.7(3) 3_566 1_556 ?
Cl4 Sm1B Cl4 95.7(3) 2_666 1_556 ?
Cl4 Sm1B Cl4 95.7(3) 3_566 2_666 ?
Sm2 Sm2 Cl5 109.42(11) 4 3 ?
Sm2 Sm2 Cl5 53.77(10) 4 5 ?
Sm2 Sm2 Cl5 53.77(10) 4 6 ?
Sm2 Sm2 Cl5 109.42(11) 4 . ?
Sm2 Sm2 Cl5 53.77(10) 4 4 ?
Sm2 Sm2 Cl5 109.42(11) 4 2 ?
Sm2 Sm2 Cl7 180.0 4 . ?
Cl5 Sm2 Cl5 109.52(11) 3 . ?
Cl5 Sm2 Cl5 88.63(14) 4 5 ?
Cl5 Sm2 Cl5 109.52(11) 3 2 ?
Cl5 Sm2 Cl5 163.20(10) 2 5 ?
Cl5 Sm2 Cl5 79.41(12) 3 4 ?
Cl5 Sm2 Cl5 109.52(11) 2 . ?
Cl5 Sm2 Cl5 79.41(12) 2 4 ?
Cl5 Sm2 Cl5 79.41(12) 3 5 ?
Cl5 Sm2 Cl5 163.20(10) . 4 ?
Cl5 Sm2 Cl5 79.41(12) . 5 ?
Cl5 Sm2 Cl5 163.20(10) 3 6 ?
Cl5 Sm2 Cl5 88.63(14) 6 5 ?
Cl5 Sm2 Cl5 79.41(12) 2 6 ?
Cl5 Sm2 Cl5 88.63(14) 4 6 ?
Cl5 Sm2 Cl5 79.41(12) . 6 ?
Cl5 Sm2 Cl7 70.58(11) . . ?
Cl5 Sm2 Cl7 70.58(11) 3 . ?
Cl5 Sm2 Cl7 70.58(11) 2 . ?
Cl7 Sm2 Cl5 126.23(10) . 5 ?
Cl7 Sm2 Cl5 126.23(10) . 4 ?
Cl7 Sm2 Cl5 126.23(10) . 6 ?
Sm1B Cl3 Sm1 13.8(3) 4_666 4_665 ?
Sm1B Cl3 Cd8 119.6(3) 4_666 5 ?
Cd8 Cl3 Sm1 105.86(13) 5 4_665 ?
Sm1 Cl4 Sm1B 13.55(18) . 1_554 ?
Cd8 Cl4 Sm1 125.56(17) 5 . ?
Cd8 Cl4 Sm1B 112.0(3) 5 1_554 ?
Sm2 Cl5 Sm2 16.80(10) . 4 ?
Sm2 Cl5 Cd8 124.03(17) . 5 ?
Cd8 Cl5 Sm2 107.23(15) 5 4 ?
Cl7 Cl7 Sm2 180.0 4_556 . ?
Cl3 Cd8 Cl4 87.73(13) 6 6 ?
Cl3 Cd8 Cl5 90.66(13) 6 6 ?
Cl4 Cd8 Cl5 86.34(14) 6 6 ?
P11 Cd8 Cl3 128.18(12) . 6 ?
P11 Cd8 Cl4 124.23(13) . 6 ?
P11 Cd8 Cl5 126.79(14) . 6 ?
P11 Cd9 P11 180.00(7) 6_656 3 ?
P11 Cd10 P11 176.31(9) 3 5_556 ?
Cd9 P11 Cd8 113.57(14) 2 . ?
Cd10 P11 Cd8 112.42(14) 6_556 . ?
Cd10 P11 Cd8 113.49(14) 2 . ?
Cd10 P11 Cd9 104.45(13) 2 2 ?
Cd10 P11 Cd9 106.45(13) 6_556 2 ?
Cd10 P11 Cd10 105.74(15) 2 6_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Cd5P2Br4
_database_code_depnum_ccdc_archive 'CCDC 2235036'
loop_
_audit_author_name
_audit_author_address
'Zhi-Xin Qiu'
;Fujian Institute of Research on the Structure  of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-02-01 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_audit_creation_date             2022-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelxl_version_number           2013-2
_chemical_name_common            Cd5P2Br4
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         Cd5P2Br4
_chemical_formula_sum            'Br4 Cd5 P2'
_chemical_formula_weight         943.58
_chemical_absolute_configuration ?
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   12.1965(8)
_cell_length_b                   13.6691(10)
_cell_length_c                   7.7077(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1284.99(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2830
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.0690
_cell_measurement_theta_min      3.0280
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.877
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.074
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4786
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.238
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku Pilatus CCD'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                1888
_reflns_number_total             2017
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_refine_diff_density_max         2.212
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.364
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.35(3)
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2017
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0451
_refine_ls_restrained_S_all      0.985
_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)+(0.0867P)²+19.6128P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1338
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.64748
 0.35252
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.77686(17) 0.75001(13) 0.9879(3) 0.0363(5) Uani 1 1 d . U . . .
Cd2 Cd 0.74807(13) 0.91344(19) 0.5069(4) 0.0489(6) Uani 1 1 d . U . . .
Cd3 Cd 0.5095(2) 0.54641(17) 0.8023(3) 0.0482(6) Uani 1 1 d . U . . .
Cd4 Cd 0.95013(17) 0.50237(17) 0.6538(3) 0.0455(6) Uani 1 1 d . U . . .
Cd5 Cd 0.9927(2) 0.24135(16) 0.8939(4) 0.0548(7) Uani 1 1 d . U . . .
Br6 Br 0.99832(18) 0.7725(2) 1.0001(4) 0.0401(6) Uani 1 1 d . U . . .
Br7 Br 0.7282(2) 0.92800(18) 0.9179(4) 0.0366(6) Uani 1 1 d . U . . .
Br8 Br 0.74912(17) 0.6277(2) 0.7411(4) 0.0372(6) Uani 1 1 d . U . . .
Br9 Br 0.74927(19) 0.6862(2) 0.2943(4) 0.0409(7) Uani 1 1 d . U . . .
P10 P 0.9458(4) 0.9158(4) 0.5089(8) 0.0240(11) Uani 1 1 d . U . . .
P11 P 0.9433(5) 0.4133(4) 0.9307(8) 0.0258(12) Uani 1 1 d . U . . .


_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
Cd1 Br6 2.720(3) . ?
Cd1 Br7 2.562(3) . ?
Cd1 Br8 2.555(3) . ?
Cd1 Br9 2.540(4) 1_556 ?
Cd2 P10 2.412(5) . ?
Cd2 P11 2.407(6) 4_654 ?
Cd3 Br6 2.910(4) 3_465 ?
Cd3 P10 2.446(7) 3_465 ?
Cd3 P10 2.454(6) 4_645 ?
Cd4 Br7 3.012(4) 4_644 ?
Cd4 Br8 3.066(3) . ?
Cd4 P11 2.444(6) 2_764 ?
Cd4 P11 2.458(6) . ?
Cd5 Br6 3.043(4) 2_764 ?
Cd5 P10 2.441(6) 2_765 ?
Cd5 P11 2.443(6) . ?
Br6 Cd3 2.910(4) 3_565 ?
Br6 Cd5 3.043(4) 2_765 ?
Br7 Cd4 3.012(4) 4_655 ?
Br9 Cd1 2.540(4) 1_554 ?
P10 Cd3 2.454(6) 4_654 ?
P10 Cd3 2.446(7) 3_565 ?
P10 Cd5 2.441(6) 2_764 ?
P11 Cd2 2.407(6) 4_645 ?
P11 Cd4 2.444(6) 2_765 ?

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
Br7 Cd1 Br6 97.47(11) . . ?
Br8 Cd1 Br6 103.37(11) . . ?
Br8 Cd1 Br7 115.71(12) . . ?
Br9 Cd1 Br6 97.95(11) 1_556 . ?
Br9 Cd1 Br7 119.41(13) 1_556 . ?
Br9 Cd1 Br8 116.77(13) 1_556 . ?
P11 Cd2 P10 166.2(3) 4_654 . ?
P10 Cd3 Br6 106.83(17) 4_645 3_465 ?
P10 Cd3 Br6 106.82(17) 3_465 3_465 ?
P10 Cd3 P10 145.51(17) 3_465 4_645 ?
Br7 Cd4 Br8 75.14(9) 4_644 . ?
P11 Cd4 Br7 96.80(16) 2_764 4_644 ?
P11 Cd4 Br7 109.42(17) . 4_644 ?
P11 Cd4 Br8 108.43(16) 2_764 . ?
P11 Cd4 Br8 93.39(16) . . ?
P11 Cd4 P11 149.57(14) 2_764 . ?
P10 Cd5 Br6 107.25(18) 2_765 2_764 ?
P10 Cd5 P11 151.6(2) 2_765 . ?
P11 Cd5 Br6 100.63(18) . 2_764 ?
Cd1 Br6 Cd3 97.17(10) . 3_565 ?
Cd1 Br6 Cd5 93.61(11) . 2_765 ?
Cd3 Br6 Cd5 125.00(13) 3_565 2_765 ?
Cd1 Br7 Cd4 111.15(11) . 4_655 ?
Cd1 Br8 Cd4 115.03(10) . . ?
Cd2 P10 Cd3 109.1(2) . 3_565 ?
Cd2 P10 Cd3 103.1(2) . 4_654 ?
Cd2 P10 Cd5 107.1(2) . 2_764 ?
Cd3 P10 Cd3 112.0(2) 3_565 4_654 ?
Cd5 P10 Cd3 109.6(3) 2_764 4_654 ?
Cd5 P10 Cd3 115.1(2) 2_764 3_565 ?
Cd2 P11 Cd4 110.1(3) 4_645 2_765 ?
Cd2 P11 Cd4 104.2(2) 4_645 . ?
Cd2 P11 Cd5 105.6(2) 4_645 . ?
Cd4 P11 Cd4 111.1(2) 2_765 . ?
Cd5 P11 Cd4 111.5(3) . . ?
Cd5 P11 Cd4 113.8(2) . 2_765 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.64748
2 0.35252

