# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_exp_5500
_database_code_depnum_ccdc_archive 'CCDC 1984644'
loop_
_audit_author_name
_audit_author_address
'Zhuang Li'
;Technical Institute of Physics and Chemistry, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_audit_creation_date             2019-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cd3 Cu P S6'
_chemical_formula_sum            'Cd3 Cu P S6'
_chemical_formula_weight         624.07
_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
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
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                   12.0326(11)
_cell_length_b                   6.9383(3)
_cell_length_c                   13.8825(13)
_cell_angle_alpha                90
_cell_angle_beta                 125.005(14)
_cell_angle_gamma                90
_cell_volume                     949.33(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5108
_cell_measurement_temperature    295.39(10)
_cell_measurement_theta_max      26.3380
_cell_measurement_theta_min      3.4090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    4.366
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5770
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.443
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.39(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.00  68.00   0.50    0.74    --    9.62  77.00-150.00  132
  2  ω     -2.00  71.00   0.50    0.74    --    9.62  77.00 -30.00  146
  3  ω     16.00  50.00   0.50    0.74    --   -8.52  77.00 -90.00   68
  4  ω    -29.00  12.00   0.50    0.74    --   -8.52  77.00 -90.00   82
  5  ω      5.00  74.00   0.50    0.74    --    9.62  77.00  30.00  138
  6  ω     -7.00  76.00   0.50    0.74    --    9.62  77.00  90.00  166
  7  ω    -24.00  58.00   0.50    0.74    --   -8.52  77.00 150.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0058456520
_diffrn_orient_matrix_UB_12      -0.0703257520
_diffrn_orient_matrix_UB_13      -0.0397629040
_diffrn_orient_matrix_UB_21      0.0437000996
_diffrn_orient_matrix_UB_22      0.0551351996
_diffrn_orient_matrix_UB_23      -0.0080748008
_diffrn_orient_matrix_UB_31      0.0568525024
_diffrn_orient_matrix_UB_32      -0.0496693976
_diffrn_orient_matrix_UB_33      0.0473763047
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                1820
_reflns_number_total             1830
_reflns_odcompleteness_completeness 81.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.417
_refine_diff_density_min         -1.853
_refine_diff_density_rms         0.374
_refine_ls_abs_structure_details 
;
 Flack x determined using 821 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1830
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0427
_refine_ls_restrained_S_all      1.252
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0439P)²+55.3491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1186
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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
Cd1 Cd 0.75965(18) 0.4308(3) 0.42682(16) 0.0273(5) Uani 1 1 d . . . . .
Cd2 Cd 0.89961(16) 0.3791(3) 0.75607(14) 0.0204(4) Uani 1 1 d . . . . .
Cd3 Cd 0.68533(18) 0.8415(2) 0.56008(15) 0.0195(4) Uani 1 1 d . . . . .
Cu1 Cu 0.5257(3) 0.3104(5) 0.5652(3) 0.0220(7) Uani 1 1 d . . . . .
S1 S 0.6982(6) 0.4869(7) 0.5658(5) 0.0112(10) Uani 1 1 d . . . . .
S2 S 0.3356(5) 0.5077(7) 0.4972(4) 0.0096(10) Uani 1 1 d . . . . .
S3 S 0.3521(6) 0.4992(7) 0.2667(5) 0.0114(10) Uani 1 1 d . . . . .
S4 S 0.1058(6) 0.2404(8) 0.2632(4) 0.0124(10) Uani 1 1 d . . . . .
S5 S 0.0993(5) 0.7196(7) 0.2434(4) 0.0101(10) Uani 1 1 d . . . . .
S6 S 0.4732(6) 0.0323(8) 0.4558(5) 0.0140(10) Uani 1 1 d . . . . .
P1 P 0.2221(5) 0.4802(7) 0.3170(4) 0.0062(10) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0278(10) 0.0352(11) 0.0297(10) -0.0178(8) 0.0227(9) -0.0157(8)
Cd2 0.0170(9) 0.0284(9) 0.0148(8) 0.0006(7) 0.0084(7) 0.0023(8)
Cd3 0.0203(9) 0.0157(8) 0.0208(9) 0.0011(7) 0.0107(7) 0.0047(7)
Cu1 0.0201(16) 0.0210(15) 0.0186(15) 0.0008(12) 0.0074(13) 0.0027(12)
S1 0.013(3) 0.012(2) 0.012(2) 0.000(2) 0.010(2) 0.001(2)
S2 0.013(3) 0.012(2) 0.003(2) 0.0001(16) 0.004(2) 0.0011(17)
S3 0.013(3) 0.015(2) 0.015(3) 0.0020(19) 0.013(2) 0.0009(19)
S4 0.014(3) 0.013(2) 0.008(2) -0.0040(18) 0.006(2) -0.006(2)
S5 0.009(2) 0.009(2) 0.009(2) 0.0038(18) 0.004(2) 0.0030(18)
S6 0.011(3) 0.017(2) 0.013(2) 0.002(2) 0.006(2) 0.001(2)
P1 0.006(3) 0.007(2) 0.004(2) 0.0005(17) 0.001(2) 0.0002(18)

_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 S1 2.461(5) . ?
Cd1 S4 2.895(6) 3 ?
Cd1 S5 2.592(5) 3_545 ?
Cd1 S6 2.465(6) 3 ?
Cd2 S1 2.462(6) . ?
Cd2 S3 2.709(6) 4 ?
Cd2 S5 2.599(5) 2_665 ?
Cd2 S6 2.456(6) 4 ?
Cd3 S1 2.464(5) . ?
Cd3 S2 2.679(6) 3 ?
Cd3 S3 2.622(6) 4_565 ?
Cd3 S6 2.474(6) 1_565 ?
Cu1 S1 2.406(6) . ?
Cu1 S2 2.349(6) . ?
Cu1 S4 2.360(5) 4 ?
Cu1 S6 2.309(6) . ?
S2 Cd3 2.679(6) 3_445 ?
S2 P1 2.059(7) . ?
S3 Cd2 2.709(6) 4_454 ?
S3 Cd3 2.622(6) 4_464 ?
S3 P1 2.050(7) . ?
S4 Cd1 2.895(6) 3_445 ?
S4 Cu1 2.360(5) 4_454 ?
S4 P1 2.022(7) . ?
S5 Cd1 2.592(5) 3_455 ?
S5 Cd2 2.599(5) 2_464 ?
S5 P1 2.063(7) . ?
S6 Cd1 2.465(6) 3_445 ?
S6 Cd2 2.456(6) 4_454 ?
S6 Cd3 2.474(6) 1_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
S1 Cd1 S4 98.82(17) . 3 ?
S1 Cd1 S5 118.06(18) . 3_545 ?
S1 Cd1 S6 125.5(2) . 3 ?
S5 Cd1 S4 82.41(17) 3_545 3 ?
S6 Cd1 S4 93.07(18) 3 3 ?
S6 Cd1 S5 116.15(18) 3 3_545 ?
S1 Cd2 S3 104.13(19) . 4 ?
S1 Cd2 S5 112.73(18) . 2_665 ?
S5 Cd2 S3 88.88(16) 2_665 4 ?
S6 Cd2 S1 129.09(19) 4 . ?
S6 Cd2 S3 97.57(19) 4 4 ?
S6 Cd2 S5 113.18(18) 4 2_665 ?
S1 Cd3 S2 113.48(18) . 3 ?
S1 Cd3 S3 113.01(19) . 4_565 ?
S1 Cd3 S6 125.3(2) . 1_565 ?
S3 Cd3 S2 86.52(16) 4_565 3 ?
S6 Cd3 S2 103.99(18) 1_565 3 ?
S6 Cd3 S3 107.47(19) 1_565 4_565 ?
S2 Cu1 S1 110.1(2) . . ?
S2 Cu1 S4 102.0(2) . 4 ?
S4 Cu1 S1 107.3(2) 4 . ?
S6 Cu1 S1 109.7(2) . . ?
S6 Cu1 S2 112.8(2) . . ?
S6 Cu1 S4 114.6(2) . 4 ?
Cd1 S1 Cd3 100.04(19) . . ?
Cd2 S1 Cd1 103.9(2) . . ?
Cd2 S1 Cd3 110.0(2) . . ?
Cu1 S1 Cd1 124.3(2) . . ?
Cu1 S1 Cd2 99.5(2) . . ?
Cu1 S1 Cd3 118.0(2) . . ?
Cu1 S2 Cd3 107.6(2) . 3_445 ?
P1 S2 Cd3 104.8(3) . 3_445 ?
P1 S2 Cu1 104.4(3) . . ?
Cd3 S3 Cd2 113.7(2) 4_464 4_454 ?
P1 S3 Cd2 100.5(2) . 4_454 ?
P1 S3 Cd3 98.3(3) . 4_464 ?
Cu1 S4 Cd1 116.9(2) 4_454 3_445 ?
P1 S4 Cd1 109.0(3) . 3_445 ?
P1 S4 Cu1 106.7(3) . 4_454 ?
Cd1 S5 Cd2 106.19(19) 3_455 2_464 ?
P1 S5 Cd1 92.9(2) . 3_455 ?
P1 S5 Cd2 100.5(2) . 2_464 ?
Cd1 S6 Cd3 124.9(2) 3_445 1_545 ?
Cd2 S6 Cd1 102.7(2) 4_454 3_445 ?
Cd2 S6 Cd3 112.2(2) 4_454 1_545 ?
Cu1 S6 Cd1 102.2(2) . 3_445 ?
Cu1 S6 Cd2 108.6(2) . 4_454 ?
Cu1 S6 Cd3 105.1(2) . 1_545 ?
S2 P1 S5 108.3(3) . . ?
S3 P1 S2 107.7(3) . . ?
S3 P1 S5 104.4(3) . . ?
S4 P1 S2 111.2(3) . . ?
S4 P1 S3 115.4(3) . . ?
S4 P1 S5 109.4(3) . . ?

_shelx_res_file                  
;
    exp_5500.res created by SHELXL-2014/7

TITL exp_5500_a.res in Cc
REM Old TITL exp_5500 in Cc
REM SHELXT solution in Cc
REM R1 0.072, Rweak 0.036, Alpha 0.001, Orientation as input
REM Flack x = 0.409 ( 0.040 ) from Parsons' quotients
REM Formula found by SHELXT: Cu Cd3 P S6
CELL 0.71073 12.0326 6.9383 13.8825 90 125.005 90
ZERR 4 0.0011 0.0003 0.0013 0 0.014 0
LATT -7
SYMM +X,-Y,0.5+Z
SFAC Cd Cu P S
UNIT 12 4 4 24

L.S. 4 0 0
PLAN  20
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\exp_5500.hkl">
REM </olex2.extras>

WGHT    0.043900   55.349098
FVAR       0.22360
CD1   1    0.759652    0.430765    0.426823    11.00000    0.02777    0.03522 =
         0.02966   -0.01776    0.02274   -0.01574
CD2   1    0.899613    0.379143    0.756074    11.00000    0.01695    0.02840 =
         0.01476    0.00062    0.00837    0.00233
CD3   1    0.685328    0.841548    0.560083    11.00000    0.02027    0.01568 =
         0.02081    0.00107    0.01071    0.00474
CU1   2    0.525685    0.310421    0.565198    11.00000    0.02007    0.02098 =
         0.01860    0.00082    0.00741    0.00270
S1    4    0.698240    0.486866    0.565816    11.00000    0.01327    0.01187 =
         0.01241   -0.00008    0.00964    0.00074
S2    4    0.335636    0.507698    0.497182    11.00000    0.01268    0.01198 =
         0.00270    0.00012    0.00357    0.00110
S3    4    0.352096    0.499248    0.266739    11.00000    0.01281    0.01520 =
         0.01462    0.00201    0.01277    0.00090
S4    4    0.105758    0.240424    0.263185    11.00000    0.01447    0.01285 =
         0.00838   -0.00398    0.00560   -0.00631
S5    4    0.099275    0.719599    0.243417    11.00000    0.00930    0.00922 =
         0.00932    0.00378    0.00386    0.00304
S6    4    0.473190    0.032254    0.455754    11.00000    0.01115    0.01717 =
         0.01257    0.00234    0.00607    0.00131
P1    3    0.222135    0.480244    0.317014    11.00000    0.00558    0.00744 =
         0.00359    0.00049    0.00141    0.00022
HKLF 4

REM  exp_5500_a.res in Cc
REM R1 =  0.0427 for    1820 Fo > 4sig(Fo)  and  0.0430 for all    1830 data
REM    100 parameters refined using      2 restraints

END

WGHT      0.0440     55.1274

REM Highest difference peak  2.417,  deepest hole -1.853,  1-sigma level  0.374
Q1    1   0.6848  1.1601  0.5580  11.00000  0.05    2.42
Q2    1   0.9038  0.6195  0.7550  11.00000  0.05    2.15
Q3    1   0.7542  0.5808  0.4265  11.00000  0.05    1.79
Q4    1   0.5248  0.6987  0.5630  11.00000  0.05    1.42
Q5    1   0.2003  0.4000  0.2027  11.00000  0.05    1.37
Q6    1   0.6714  0.5256  0.3221  11.00000  0.05    1.19
Q7    1   0.8656  0.6137  0.5342  11.00000  0.05    1.08
Q8    1   0.2801  0.3589  0.1229  11.00000  0.05    1.07
Q9    1   0.5113  0.7036  0.4032  11.00000  0.05    1.03
Q10   1   0.8189  0.5038  0.6750  11.00000  0.05    1.02
Q11   1   1.0045  0.5157  0.8264  11.00000  0.05    1.01
Q12   1   0.1473  0.4987  0.4003  11.00000  0.05    0.98
Q13   1   0.1957  0.5989  0.2027  11.00000  0.05    0.95
Q14   1   0.5308  0.7593  0.4827  11.00000  0.05    0.95
Q15   1   0.6013  0.0431  0.5422  11.00000  0.05    0.94
Q16   1   0.2031  0.5003  0.4882  11.00000  0.05    0.94
Q17   1   0.6414  0.4988  0.4422  11.00000  0.05    0.93
Q18   1   0.1823  0.5625  0.3174  11.00000  0.05    0.93
Q19   1   0.7792  0.6248  0.5380  11.00000  0.05    0.93
Q20   1   0.1193  0.7111  0.3942  11.00000  0.05    0.92
;
_shelx_res_checksum              55877
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.968
_oxdiff_exptl_absorpt_empirical_full_min 0.633
