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_1564588
_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            'C72 H81 Cl3 F6 P4 S7 W3'
_chemical_formula_weight         2066.58
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.7212(7)
_cell_length_b                   15.7212(7)
_cell_length_c                   59.122(3)
_cell_measurement_reflns_used    8493
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      2.59
_cell_volume                     12654.7(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            29540
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.647
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.475
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             6072
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.064
_refine_diff_density_max         2.582
_refine_diff_density_min         -2.973
_refine_diff_density_rms         0.238
_refine_ls_abs_structure_details
;
 Flack x determined using 2414 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.054(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6392
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+599.1689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.970
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                5637
_reflns_number_total             6392
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2020-508-119641.cif
_cod_data_source_block           1
_cod_original_cell_volume        12654.6(13)
_cod_database_code               1564588
_shelx_estimated_absorpt_t_min   0.389
_shelx_estimated_absorpt_t_max   0.763