Isocyanide-Promoted Ylidene Transfer to Phosphorus: Rearrangement in the First-Generation Grubbs Complex
Galan, Brandon R.; Pitak, Mateusz; Keister, Jerome B.; Diver, Steven T.; Organometallics 27 (2008) 3630–; doi:10.1021/om8003652

data_4071761
_publ_section_title
;
 Isocyanide-Promoted Ylidene Transfer to Phosphorus: Rearrangement in the
 First-Generation Grubbs Complex
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3630
_journal_paper_doi               10.1021/om8003652
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C39 H45 Cl5 N3 P Ru, C H Cl3, 0.5 (C5 H12)'
_chemical_formula_sum            'C42.5 H52 Cl8 N3 P Ru'
_chemical_formula_weight         1020.51
_chemical_name_systematic
;
 ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.0610(10)
_cell_angle_beta                 78.1500(10)
_cell_angle_gamma                89.3380(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2488(2)
_cell_length_b                   15.0628(2)
_cell_length_c                   15.3236(2)
_cell_measurement_temperature    90(1)
_cell_volume                     2315.00(6)
_computing_cell_refinement       'Bruker Saint v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'Bruker Saint v7.23A (Bruker, 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(1)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48261
_diffrn_reflns_theta_full        29.14
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         1.48
_diffrn_source_type              'RIGAKU RU-2000BEH'
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_correction_T_min  0.8455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2004/1 Bruker 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1034
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         12485
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0368P)^2^+1.8602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                11165
_reflns_number_total             12485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8003652-file005.cif
_cod_data_source_block           Keister011908
_cod_original_formula_sum        'C42.50 H52 Cl8 N3 P Ru'
_cod_database_code               4071761