Olefin Metathesis Reactions with Vinyl Halides: Formation, Observation, Interception, and Fate of the Ruthenium-Monohalomethylidene Moiety
Marisa L. Macnaughtan; Marc J. A. Johnson; Jeff W. Kampf; Journal of the American Chemical Society 129 (2007) 7708–7709; doi:10.1021/ja0715952

data_4109569
_publ_section_title
;
 Olefin Metathesis Reactions with Vinyl Halides: Formation, Observation,
 Interception, and Fate of the Ruthenium-Monohalomethylidene Moiety
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7708
_journal_page_last               7709
_journal_paper_doi               10.1021/ja0715952
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C40 H60 Cl3 N2 P Ru, 0.33(C4 H8 O)'
_chemical_formula_sum            'C41.33 H62.67 Cl3 N2 O0.33 P Ru'
_chemical_formula_weight         831.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.7728(8)
_cell_length_b                   20.7728(8)
_cell_length_c                   18.1437(16)
_cell_measurement_reflns_used    6411
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      2.27
_cell_volume                     6780.3(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-1K'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1470
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            88175
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.9544
_exptl_absorpt_correction_T_min  0.7987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2.10) Bruker/Siemens area
  detector absorption and other corrections, University of
  Gottingen, Germany 2003.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       needle
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       0.0022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6506
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                5493
_reflns_number_total             6506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0715952si20070306_085922.cif
_cod_data_source_block           mm426
_cod_database_code               4109569