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_4515735
_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         'C31 H37 Cl2 N Ru S, C H2 Cl2'
_chemical_formula_sum            'C32 H39 Cl4 N Ru S'
_chemical_formula_weight         712.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c 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                   19.8680(7)
_cell_length_b                   9.2131(3)
_cell_length_c                   17.5258(7)
_cell_measurement_reflns_used    6938
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.05
_cell_volume                     3208.0(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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17187
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.287
_diffrn_reflns_theta_min         2.050
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.722
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 2787 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7307
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.888
_reflns_Friedel_fraction_max     0.825
_reflns_number_gt                6938
_reflns_number_total             7307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02122_si_005.cif
_cod_data_source_block           lem41
_cod_database_code               4515735
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.861