Pentacoordinate Ruthenium(II) Catecholthiolate and Mercaptophenolate Catalysts for Olefin Metathesis: Anionic Ligand Exchange and Ease of Initiation
Mikus, Malte S.; Torker, Sebastian; Xu, Chaofan; Li, Bo; Hoveyda, Amir H.; Organometallics 35 (2016) 3878–; doi:10.1021/acs.organomet.6b00773

data_4089151
_publ_section_title
;
 Pentacoordinate Ruthenium(II) Catecholthiolate and Mercaptophenolate
 Catalysts for Olefin Metathesis: Anionic Ligand Exchange and Ease of
 Initiation
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              3878
_journal_paper_doi               10.1021/acs.organomet.6b00773
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C37 H37 N3 Ru S2, 3(C H2 Cl2)'
_chemical_formula_sum            'C40 H43 Cl6 N3 Ru S2'
_chemical_formula_weight         943.66
_chemical_name_systematic
;
 Ru-4i
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7231(7)
_cell_length_b                   16.3731(6)
_cell_length_c                   26.6239(9)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      4.83
_cell_volume                     8597.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa DUO CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            128177
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.315
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\uS'
_exptl_absorpt_coefficient_mu    7.539
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. (2013). SADABS. Bruker AXS Inc. Madison, WI USA.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.111
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7797
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0953P)^2^+24.6180P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7742
_reflns_number_total             7797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00773_si_001.cif
_cod_data_source_block           C37H37N3RuS2(CH2Cl2)3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4089151
_shelx_estimated_absorpt_t_min   0.129
_shelx_estimated_absorpt_t_max   0.314
_shelxl_version_number           2013-2
_shelx_res_checksum              44780
_shelx_hkl_checksum              47215