Reduction induced S-nucleophilicity in mono-dithiolene molybdenum complexes - in situ generation of sulfonium ligands
Elvers, Benedict Josua; Krewald, Vera; Schulzke, Carola; Fischer, Christian; Chemical Communications  (2021) –; doi:10.1039/D1CC05335C

data_7129149
_publ_section_title
;
 Reduction induced S-nucleophilicity in mono-dithiolene molybdenum
 complexes - in situ generation of sulfonium ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05335C
_journal_year                    2021
_chemical_formula_moiety         'C35 H34 Mo O2 P2 S2, C H2 Cl2'
_chemical_formula_sum            'C36 H36 Cl2 Mo O2 P2 S2'
_chemical_formula_weight         793.55
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-05 deposited with the CCDC.	2021-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.12(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8543(18)
_cell_length_b                   10.246(2)
_cell_length_c                   19.033(4)
_cell_measurement_reflns_used    18464
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      59.3
_cell_measurement_theta_min      6.3
_cell_volume                     1726.4(6)
_computing_cell_refinement       'X-Area by STOE & Cie GmbH 2010'
_computing_data_collection       'X-Area by STOE & Cie GmbH 2010'
_computing_data_reduction        'X-Area by STOE & Cie GmbH 2010'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.1157
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13582
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_min         3.041
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7685
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.237
_refine_diff_density_max         1.052
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(11)
_refine_ls_extinction_coef       0.022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6881
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+3.4094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                4773
_reflns_number_total             6881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05335c2.cif
_cod_data_source_block           BE-82-1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7129149
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.837
_exptl_absorpt_special_details
;
programs X-Red32 and X-Shape by STOE & Cie GmbH 2010
;
_shelx_res_checksum              86033
_shelx_hkl_checksum              11862