Hemilability of phosphine-thioether ligands coordinated to trinuclear Mo3S4 cluster and its effect on hydrogenation catalysis
Gushchin, Artem L.; Shmelev, Nikita Y.; Malysheva, Svetlana F.; Artem’ev, Alexander V.; Belogorlova, Nataliya A.; Abramov, Pavel A.; Kompan’kov, Nikolay B.; Manoury, Eric; Poli, Rinaldo; Sheven, Dmitriy G.; Llusar, Rosa; Sokolov, Maxim N.; New Journal of Chemistry 42 (2018) 17708–; doi:10.1039/C8NJ03720E

data_7057785
_publ_section_title
;
 Hemilability of phosphine-thioether ligands coordinated to trinuclear
 Mo3S4 cluster and its effect on hydrogenation catalysis
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17708
_journal_paper_doi               10.1039/C8NJ03720E
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C73.55 H84.1 Cl7.1 Mo3 P3 S7'
_chemical_formula_weight         1824.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-01-13 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.229(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.9893(15)
_cell_length_b                   16.6109(4)
_cell_length_c                   24.8560(9)
_cell_measurement_reflns_used    6333
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      3.59
_cell_volume                     16429.8(9)
_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-2017 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker X8Apex'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.1145
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45845
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         3.085
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.5453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             7433
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.202
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         18801
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0751
_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^)+(0.1078P)^2^+127.8200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.2219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11618
_reflns_number_total             18801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03720e2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7057783--7057785.cif.'
_cod_original_formula_sum        'C73.55 H84.10 Cl7.10 Mo3 P3 S7'
_cod_database_code               7057785
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              17544