Syntheses, crystal structure, and photoelectric properties of two Zn-based chalcogenidoantimonates Zn-Sb-Q (Q = S, Se).
Zhang, Lirong; Zhao, Huiling; Liu, Xin; Teri, Gele; Baiyin, Menghe; Physical chemistry chemical physics : PCCP 25 (2023) 29709–29717; doi:10.1039/d3cp04074g

data_7247587
_publ_section_title
;
 Syntheses, crystal structure, and photoelectric properties of two
 Zn-based chalcogenidoantimonates Zn-Sb-Q (Q = S, Se).
;
_journal_issue                   43
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              29709
_journal_page_last               29717
_journal_paper_doi               10.1039/d3cp04074g
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C16 H48 N10 S6 Sb2 Zn2'
_chemical_formula_sum            'C16 H48 N10 S6 Sb2 Zn2'
_chemical_formula_weight         947.24
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-09 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9513(11)
_cell_length_b                   25.9513(11)
_cell_length_c                   9.8863(7)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.50
_cell_volume                     6658.1(6)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            71281
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.120
_diffrn_reflns_theta_min         3.129
_exptl_absorpt_coefficient_mu    3.432
_exptl_absorpt_correction_T_max  0.165
_exptl_absorpt_correction_T_min  0.143
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       block
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.751
_refine_diff_density_min         -3.424
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3679
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0472
_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/[\s^2^(Fo^2^)+(0.0476P)^2^+111.8368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3135
_reflns_number_total             3679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp04074g2.cif
_cod_data_source_block           230426c_0m_pl
_cod_depositor_comments
'Adding full bibliography for 7247586--7247587.cif.'
_cod_original_cell_volume        6658.1(7)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7247587
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.279
_shelx_estimated_absorpt_t_min   0.279
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Rigid bond restraints
 S1, S3, Sb1, S2, S2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
3. Uiso/Uaniso restraints and constraints
Uanis(Zn1) = Uanis(S3)
4.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3), N5(H5)
4.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), C1(H1D,H1E), C4(H4C,H4D), C6(H6A,H6B), C8(H8A,H8B), C2(H2A,H2B),
 C5(H5A,H5B), C3(H3A,H3B), C7(H7A,H7B)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'