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_1564477
_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 Ge4 In N8 O S13'
_chemical_formula_sum            'C12 Ge4 In N8 O S13'
_chemical_formula_weight         1094.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2157(9)
_cell_length_b                   11.3247(5)
_cell_length_c                   15.6853(7)
_cell_measurement_reflns_used    2387
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.0910
_cell_measurement_theta_min      3.2240
_cell_volume                     3768.6(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0876
_diffrn_reflns_av_unetI/netI     0.1196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.769
_exptl_absorpt_coefficient_mu    4.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.891
_refine_diff_density_min         -2.202
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         4302
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.450
_refine_ls_R_factor_all          0.1603
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1156P)^2^+15.2135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2747
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2243
_reflns_number_total             4302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA_2020-509-119698.cif
_cod_data_source_block           compound-3
_cod_database_code               1564477
_shelx_res_checksum              84471
_shelx_hkl_checksum              93559