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_7129151
_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         'C34 H32 Mo O2 P2 S3, C H2 Cl2'
_chemical_formula_sum            'C35 H34 Cl2 Mo O2 P2 S3'
_chemical_formula_weight         811.58
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_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                 90.96(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8426(18)
_cell_length_b                   10.239(2)
_cell_length_c                   19.000(4)
_cell_measurement_reflns_used    19323
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      58.9
_cell_measurement_theta_min      4.0
_cell_volume                     1720.0(6)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2010).'
_computing_data_collection       'X-Area (Stoe & Cie, 2010).'
_computing_data_reduction        'X-Area (Stoe & Cie, 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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19308
_diffrn_reflns_point_group_measured_fraction_full 0.913
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.445
_diffrn_reflns_theta_min         2.144
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.9655
_exptl_absorpt_correction_T_min  0.8128
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       needles
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.209
_refine_diff_density_min         -2.179
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 2836 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8475
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0837P)^2^+3.0709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_full    0.814
_reflns_Friedel_fraction_max     0.766
_reflns_number_gt                7624
_reflns_number_total             8475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05335c2.cif
_cod_data_source_block           BE7-351-1
_cod_original_cell_volume        1720.1(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7129151
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.687
_shelx_estimated_absorpt_t_max   0.968
_exptl_absorpt_special_details
;
programs X-Red32 and X-Shape by STOE & Cie GmbH 2010
;
_shelx_res_checksum              26810
_shelx_hkl_checksum              10255