Using thiol-amine solvent mixture to prepare main group heterometallic chalcogenides
Yu, Ji-Ming; Cai, Ting; Ma, Zhong-Jie; Wang, Fei; Wang, Huan; Yu, Ji-Peng; Xiao, Lu-Lu; Cheng, Fang-Fang; Xiong, Wei-Wei; Inorganica Chimica Acta 509 (2020) 119698–; doi:10.1016/j.ica.2020.119698

data_1564476
_publ_section_title
;
 Using thiol-amine solvent mixture to prepare main group heterometallic
 chalcogenides
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119698
_journal_paper_doi               10.1016/j.ica.2020.119698
_journal_volume                  509
_journal_year                    2020
_chemical_formula_moiety         'C12.20 H0 In2.80 N3.80 S2 Se6 Sn1.20'
_chemical_formula_sum            'C12.2 H0 In2.8 N3.8 S2 Se6 Sn1.2'
_chemical_formula_weight         1201.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3741(14)
_cell_length_b                   28.778(2)
_cell_length_c                   8.0083(7)
_cell_measurement_reflns_used    1946
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1110
_cell_measurement_theta_min      4.0800
_cell_volume                     3082.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_unetI/netI     0.1560
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19549
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.628
_diffrn_reflns_theta_min         3.314
_exptl_absorpt_coefficient_mu    10.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14136
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.589
_exptl_crystal_description       needle
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.545
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.278
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.50(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         6722
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+5.9364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                3463
_reflns_number_total             6722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA_2020-509-119698.cif
_cod_data_source_block           compound-2
_cod_original_formula_sum        'C12.20 H0 In2.80 N3.80 S2 Se6 Sn1.20'
_cod_database_code               1564476
_shelx_res_checksum              72446
_shelx_hkl_checksum              84361