Synthesis and crystal structure of oktakis(dimethylsulphoxide-κ1 O)gadolinium(III) [tetrabromido-μ2-bromido-μ2-sulfido-di-μ3-sulfido-μ4-sulfido-tetracopper(I)-tungsten(VI)], C16H48O8S12Br5Cu4GdW
Ye, Yunfeng; Tang, Guodong; Qian, Jun; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 455–457; doi:10.1515/ncrs-2020-0591

data_8104858
_publ_section_title
;
 Synthesis and crystal structure of oktakis(dimethylsulphoxide-\k1
 O)gadolinium(III)
 [tetrabromido-\m2-bromido-\m2-sulfido-di-\m3-sulfido-\m4-sulfido-tetracopper(I)-tungsten(VI)],
 C16H48O8S12Br5Cu4GdW
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              455
_journal_page_last               457
_journal_paper_doi               10.1515/ncrs-2020-0591
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C16 H48 Gd O8 S8, Br5 Cu4 S4 W'
_chemical_formula_sum            'C16 H48 Br5 Cu4 Gd O8 S12 W'
_chemical_formula_weight         1748.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   geom
_cell_angle_alpha                90
_cell_angle_beta                 100.76(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.576(2)
_cell_length_b                   12.407(3)
_cell_length_c                   17.582(3)
_cell_measurement_reflns_used    6878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.335
_cell_measurement_theta_min      3.145
_cell_volume                     2480.8(9)
_computing_cell_refinement       'OLEX2 [1]'
_computing_data_collection       'OLEX2 [1]'
_computing_data_reduction        'OLEX2 [1]'
_computing_molecular_graphics    'PLATON [4]'
_computing_publication_material  'SHELXL-2014/7 [3]'
_computing_structure_refinement  'SHELXL-2014/7 [3]'
_computing_structure_solution    'SHELXT  [2]'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11490
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.335
_diffrn_reflns_theta_min         3.145
_exptl_absorpt_coefficient_mu    9.874
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.332
_exptl_crystal_description       block
_exptl_crystal_F_000             1646
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.169
_exptl_transmission_factor_min   0.131
_refine_diff_density_max         2.996
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.228
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.037(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         6878
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                5277
_reflns_number_total             6878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0591_suppl.cif
_cod_data_source_block           s
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               8104858
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.869