Steric and Electronic Effects of Carbene Substitution in Grubbs First-Generation Catalysts
Lane, David R.; Beavers, Christine M.; Olmstead, Marilyn M.; Schore, Neil E.; Organometallics 28 (2009) 6789–; doi:10.1021/om900762n

data_4070377
_publ_section_title
;
 Steric and Electronic Effects of Carbene Substitution in Grubbs
 First-Generation Catalysts
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6789
_journal_paper_doi               10.1021/om900762n
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C43 H71 Br Cl2 P2 Ru, C6 H6'
_chemical_formula_sum            'C49 H77 Br Cl2 P2 Ru'
_chemical_formula_weight         979.93
_chemical_name_systematic
; 
 bis(tricyclohexylphosphino)dichloro[(4-bromophenyl)methylidene]ruthenium(II) 
benzene solvate   
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.320(2)
_cell_angle_beta                 80.179(2)
_cell_angle_gamma                69.200(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8233(6)
_cell_length_b                   12.6850(8)
_cell_length_c                   20.9842(12)
_cell_measurement_reflns_used    4958
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.69
_cell_volume                     2345.3(2)
_computing_cell_refinement       'SAINT 7.16 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28758
_diffrn_reflns_theta_full        26.85
_diffrn_reflns_theta_max         26.85
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.9083
_exptl_absorpt_correction_T_min  0.7209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/4 (Bruker-AXS, 2007)'
_exptl_crystal_colour            purple-red
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         10073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.0080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                7298
_reflns_number_total             10073
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900762n_si_001.cif
_cod_data_source_block           cb103
_cod_database_code               4070377