Synthesis, Structure, and Activity of Enhanced Initiators for Olefin Metathesis
Jennifer A. Love; Melanie S. Sanford; Michael W. Day; Robert H. Grubbs; Journal of the American Chemical Society 125 (2003) 10103–10109; doi:10.1021/ja027472t

data_4114060
_publ_section_title
;
 Synthesis, Structure, and Activity of Enhanced Initiators for Olefin
 Metathesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10103
_journal_page_last               10109
_journal_paper_doi               10.1021/ja027472t
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C46 H65 Cl2 N2 P Ru, C6 H6, 0.5(C5 H12)'
_chemical_formula_sum            'C54.5 H77 Cl2 N2 P Ru'
_chemical_formula_weight         963.17
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.601(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2949(7)
_cell_length_b                   14.9666(8)
_cell_length_c                   27.1432(15)
_cell_measurement_reflns_used    7485
_cell_measurement_temperature    98
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.4
_cell_volume                     4950.8(5)
_computing_cell_refinement       'Bruker SMART v5.606, Bruker SAINT v6.02'
_computing_data_collection       'Bruker SMART v5.054'
_computing_data_reduction        'Bruker SAINT v6.02'
_computing_molecular_graphics    'Diamond, Bruker SHELXTL v5.1'
_computing_publication_material  'Bruker SHELXTL v5.1'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      98
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker SMART 1000 ccd'
_diffrn_measurement_method       '\w scans at 6 fixed \f values'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            87057
_diffrn_reflns_theta_full        28.54
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  'first 75 scans recollected at end of runs'
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.9093
_exptl_absorpt_correction_T_min  0.8631
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            burgundy
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.990
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.658
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         11892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.658
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/\s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                10104
_reflns_number_total             11892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027472tsi20030515_033334_1.cif
_cod_data_source_block           mss26
_cod_original_formula_sum        'C54.50 H77 Cl2 N2 P Ru'
_cod_database_code               4114060