Origins of initiation rate differences in ruthenium olefin metathesis catalysts containing chelating benzylidenes.
Engle, Keary M.; Lu, Gang; Luo, Shao-Xiong; Henling, Lawrence M.; Takase, Michael K.; Liu, Peng; Houk, K. N.; Grubbs, Robert H.; Journal of the American Chemical Society 137 (2015) 5782–5792; doi:10.1021/jacs.5b01144

data_4129360
_publ_section_title
;
 Origins of initiation rate differences in ruthenium olefin metathesis
 catalysts containing chelating benzylidenes.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5782
_journal_page_last               5792
_journal_paper_doi               10.1021/jacs.5b01144
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C34 H44 Cl4 N2 O Ru'
_chemical_formula_weight         739.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6691(6)
_cell_length_b                   14.3203(7)
_cell_length_c                   21.4702(11)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.41
_cell_measurement_theta_min      2.63
_cell_volume                     3504.8(3)
_computing_cell_refinement       'SAINT v8.32B (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT v8.32B (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            329568
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.469
_diffrn_reflns_theta_min         1.722
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.490
_exptl_crystal_size_min          0.450
_refine_diff_density_max         0.873
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         17149
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+2.7904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15558
_reflns_number_total             17149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b01144_si_004.cif
_cod_data_source_block           A14086
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129360
_shelx_estimated_absorpt_t_min   0.652
_shelx_estimated_absorpt_t_max   0.720
_shelxl_version_number           2013-4
_shelx_res_checksum              98292
_shelx_hkl_checksum              71845