# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_181
_database_code_depnum_ccdc_archive 'CCDC 1909605'
loop_
_audit_author_name
_audit_author_address
'Guangmao Li'
;Harbin Institute of Technology
China
;
_audit_update_record             
;
2019-04-11 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cd Li2 S4 Si'
_chemical_formula_weight         282.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pmn2(1) '

loop_
_symmetry_equiv_pos_as_xyz
" 'x, y, z' "
" '-x+1/2, -y, z+1/2' "
" 'x+1/2, -y, z+1/2' "
" '-x, y, z' "

_cell_length_a                   7.611(3)
_cell_length_b                   6.793(2)
_cell_length_c                   6.304(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     325.90(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1271
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.41

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             264
_exptl_absorpt_coefficient_mu    4.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8829
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1899
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.45
_reflns_number_total             606
_reflns_number_gt                597
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
" goodness of fit S are based on F², conventional R-factors R are based "
" on F, with F set to zero for negative F². The threshold expression of "
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
" on F² are statistically about twice as large as those based on F, and R- "
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0131P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
" 'Flack H D (1983), Acta Cryst. A39, 876-881' "
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_number_reflns         606
_refine_ls_number_parameters     44
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0149
_refine_ls_R_factor_gt           0.0145
_refine_ls_wR_factor_ref         0.0302
_refine_ls_wR_factor_gt          0.0300
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 -0.14354(4) 0.86817(4) 0.01809(11) Uani 1 2 d S . .
Si1 Si 0.0000 0.17581(13) 0.3708(4) 0.0105(2) Uani 1 2 d S . .
S1 S 0.0000 -0.12244(15) 0.2712(2) 0.0144(2) Uani 1 2 d S . .
S2 S 0.0000 0.19481(18) 0.7053(2) 0.0150(3) Uani 1 2 d S . .
S3 S -0.22384(11) 0.32831(10) 0.25185(14) 0.01406(18) Uani 1 1 d . . .
Li1 Li -0.2547(7) 0.3296(6) 0.869(3) 0.0219(11) 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 0.01868(18) 0.01877(16) 0.01682(17) 0.00032(19) 0.000 0.000
Si1 0.0115(5) 0.0107(5) 0.0094(5) -0.0005(9) 0.000 0.000
S1 0.0185(6) 0.0111(5) 0.0136(6) -0.0007(5) 0.000 0.000
S2 0.0187(7) 0.0153(5) 0.0111(6) -0.0005(5) 0.000 0.000
S3 0.0130(4) 0.0143(4) 0.0149(4) 0.0017(3) -0.0020(4) 0.0023(3)
Li1 0.023(3) 0.021(3) 0.022(2) 0.005(5) 0.001(3) -0.0016(19)

_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 S2 2.5174(15) . ?
Cd1 S1 2.5447(17) 1_556 ?
Cd1 S3 2.5555(11) 3 ?
Cd1 S3 2.5555(11) 2_455 ?
Si1 S2 2.113(3) . ?
Si1 S1 2.1210(17) . ?
Si1 S3 2.1301(14) 4 ?
Si1 S3 2.1301(14) . ?
S1 Li1 2.418(7) 3_554 ?
S1 Li1 2.418(7) 2_454 ?
S1 Cd1 2.5447(17) 1_554 ?
S2 Li1 2.380(10) 4 ?
S2 Li1 2.380(10) . ?
S3 Li1 2.42(2) 1_554 ?
S3 Li1 2.444(8) 2_464 ?
S3 Cd1 2.5555(11) 2_454 ?
Li1 S1 2.418(7) 2_455 ?
Li1 S3 2.42(2) 1_556 ?
Li1 S3 2.444(8) 2_465 ?

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
S2 Cd1 S1 110.84(4) . 1_556 ?
S2 Cd1 S3 109.36(3) . 3 ?
S1 Cd1 S3 108.31(3) 1_556 3 ?
S2 Cd1 S3 109.36(3) . 2_455 ?
S1 Cd1 S3 108.31(3) 1_556 2_455 ?
S3 Cd1 S3 110.66(4) 3 2_455 ?
S2 Si1 S1 110.71(10) . . ?
S2 Si1 S3 108.76(7) . 4 ?
S1 Si1 S3 111.13(7) . 4 ?
S2 Si1 S3 108.76(7) . . ?
S1 Si1 S3 111.13(7) . . ?
S3 Si1 S3 106.21(9) 4 . ?
Si1 S1 Li1 118.7(2) . 3_554 ?
Si1 S1 Li1 118.7(2) . 2_454 ?
Li1 S1 Li1 101.1(4) 3_554 2_454 ?
Si1 S1 Cd1 110.44(9) . 1_554 ?
Li1 S1 Cd1 102.8(5) 3_554 1_554 ?
Li1 S1 Cd1 102.8(5) 2_454 1_554 ?
Si1 S2 Li1 117.2(5) . 4 ?
Si1 S2 Li1 117.2(5) . . ?
Li1 S2 Li1 109.1(6) 4 . ?
Si1 S2 Cd1 110.56(6) . . ?
Li1 S2 Cd1 100.0(3) 4 . ?
Li1 S2 Cd1 100.0(3) . . ?
Si1 S3 Li1 115.44(13) . 1_554 ?
Si1 S3 Li1 114.2(3) . 2_464 ?
Li1 S3 Li1 106.9(5) 1_554 2_464 ?
Si1 S3 Cd1 108.53(5) . 2_454 ?
Li1 S3 Cd1 101.99(13) 1_554 2_454 ?
Li1 S3 Cd1 109.0(2) 2_464 2_454 ?
S2 Li1 S1 107.1(5) . 2_455 ?
S2 Li1 S3 110.6(4) . 1_556 ?
S1 Li1 S3 109.1(5) 2_455 1_556 ?
S2 Li1 S3 106.8(5) . 2_465 ?
S1 Li1 S3 115.1(5) 2_455 2_465 ?
S3 Li1 S3 108.1(5) 1_556 2_465 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.098
