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_4070379
_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 H72 Cl2 P2 Ru, 1.5(C6 H6)'
_chemical_formula_sum            'C52 H81 Cl2 P2 Ru'
_chemical_formula_weight         940.08
_chemical_name_systematic
; 
 bis(tricyclohexylphosphino)dichloro[(benzylidene)]ruthenium(II) 
 benzene sesquisolvate    
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.559(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6923(3)
_cell_length_b                   13.4885(5)
_cell_length_c                   37.6549(13)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.7
_cell_volume                     4917.9(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            69823
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/4 (Bruker-AXS, 2007)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         13235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+6.4234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                10367
_reflns_number_total             13235
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900762n_si_001.cif
_cod_data_source_block           cb105
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4070379