Synthesis and Catalytic Properties of Sulfur-Chelated Ruthenium Benzylidenes Bearing a Cyclic (Alkyl)(amino)carbene Ligand
Rozenberg, Illya; Eivgi, Or; Frenklah, Alexander; Butilkov, Danielle; Kozuch, Sebastian; Goldberg, Israel; Lemcoff, N. Gabriel; ACS Catalysis 8 (2018) 8182–; doi:10.1021/acscatal.8b02122

data_4515733
_publ_section_title
;
 Synthesis and Catalytic Properties of Sulfur-Chelated Ruthenium
 Benzylidenes Bearing a Cyclic (Alkyl)(amino)carbene Ligand
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              8182
_journal_paper_doi               10.1021/acscatal.8b02122
_journal_volume                  8
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H36 Cl2 F3 N Ru S'
_chemical_formula_sum            'C28 H36 Cl2 F3 N Ru S'
_chemical_formula_weight         647.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3382(7)
_cell_length_b                   16.5805(7)
_cell_length_c                   10.4655(5)
_cell_measurement_reflns_used    5184
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      2.30
_cell_volume                     2835.1(2)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. \f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13639
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.693
_diffrn_reflns_theta_min         2.301
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       needles
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 1868 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.043(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0196P)^2^+0.0068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0438
_reflns_Friedel_coverage         0.591
_reflns_Friedel_fraction_full    0.759
_reflns_Friedel_fraction_max     0.651
_reflns_number_gt                5184
_reflns_number_total             5509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02122_si_002.cif
_cod_data_source_block           lem37
_cod_database_code               4515733
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.943