Trinuclear M3S4 cluster complexes with hemilabile phosphino-thioether ligands: Some experimental and theoretical aspects
Gushchin, Artem L.; Shmelev, Nikita Y.; Malysheva, Svetlana F.; Artem'ev, Alexander V.; Belogorlova, Nataliya A.; Abramov, Pavel A.; Laricheva, Yuliya A.; Fomenko, Iakov S.; Piryazev, Dmitriy A.; Sheven, Dmitriy G.; Sokolov, Maxim N.; Inorganica Chimica Acta 508 (2020) 119645–; doi:10.1016/j.ica.2020.119645

data_1564589
_publ_section_title
;
 Trinuclear M3S4 cluster complexes with hemilabile phosphino-thioether
 ligands: Some experimental and theoretical aspects
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119645
_journal_paper_doi               10.1016/j.ica.2020.119645
_journal_volume                  508
_journal_year                    2020
_chemical_formula_sum            'C69 H99 Cl3 F6 P4 S7 W3'
_chemical_formula_weight         2048.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                89.934(2)
_cell_angle_beta                 72.574(2)
_cell_angle_gamma                78.179(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2529(8)
_cell_length_b                   17.4818(9)
_cell_length_c                   17.8346(9)
_cell_measurement_reflns_used    7497
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.3565
_cell_measurement_theta_min      2.3170
_cell_volume                     4141.3(4)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30162
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.464
_diffrn_reflns_theta_min         1.632
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.557
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.036
_refine_diff_density_max         2.605
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         16214
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11679
_reflns_number_total             16214
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2020-508-119641.cif
_cod_data_source_block           2
_cod_database_code               1564589
_shelx_estimated_absorpt_t_min   0.370
_shelx_estimated_absorpt_t_max   0.853