Cyclometalated Z-Selective Ruthenium Metathesis Catalysts with Modified N-Chelating Groups
Herbert, Myles B.; Suslick, Benjamin A.; Liu, Peng; Zou, Lufeng; Dornan, Peter K.; Houk, K. N.; Grubbs, Robert H.; Organometallics 34 (2015) 2858–; doi:10.1021/acs.organomet.5b00185

data_4087493
_publ_section_title
;
 Cyclometalated Z-Selective Ruthenium Metathesis Catalysts with Modified
 N-Chelating Groups
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2858
_journal_paper_doi               10.1021/acs.organomet.5b00185
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C44.63 H64.76 N2 O3.69 Ru'
_chemical_formula_weight         789.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 116.382(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7033(5)
_cell_length_b                   32.0649(13)
_cell_length_c                   11.9810(5)
_cell_measurement_reflns_used    9034
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.32
_cell_volume                     4027.8(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-2014 (Sheldrick, 2014)'
_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 0.994
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49432
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.574
_diffrn_reflns_theta_min         2.001
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.855
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         12286
_refine_ls_number_restraints     424
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+3.0733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9320
_reflns_number_total             12286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00185_si_003.cif
_cod_data_source_block           A14161
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087493
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.979
_shelxl_version_number           2014-2
_shelx_res_checksum              21570
_shelx_hkl_checksum              64052