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_7057784
_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            'C70.2 H100.8 Cl3 F6 Mo3 N0.6 O0 P4 S7'
_chemical_formula_weight         1809.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90.424(3)
_cell_angle_beta                 105.595(3)
_cell_angle_gamma                99.817(4)
_cell_formula_units_Z            2
_cell_length_a                   14.068(2)
_cell_length_b                   17.495(3)
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_cell_measurement_reflns_used    9135
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.1013
_cell_measurement_theta_min      2.4042
_cell_volume                     4108.9(12)
_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 0.947
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_limit_k_min       -22
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_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34957
_diffrn_reflns_point_group_measured_fraction_full 0.947
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_diffrn_source                   'sealed X-ray tube'
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_exptl_absorpt_correction_T_min  0.5654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       prism
_exptl_crystal_F_000             1858
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         4.321
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0933
_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^)+(0.0875P)^2^+81.7326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2243
_refine_ls_wR_factor_ref         0.2547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13909
_reflns_number_total             18768
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8nj03720e2.cif
_cod_data_source_block           sn25_a
_cod_depositor_comments
'Adding full bibliography for 7057783--7057785.cif.'
_cod_original_cell_volume        4108.9(10)
_cod_original_formula_sum        'C70.20 H100.80 Cl3 F6 Mo3 N0.60 O0 P4 S7'
_cod_database_code               7057784
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              50531