Ru-based Z-selective metathesis catalysts with modified cyclometalated carbene ligands
Bronner, Sarah M.; Herbert, Myles B.; Patel, Paresma R.; Marx, Vanessa M.; Grubbs, Robert H.; Chemical Science 5 (2014) 4091–4098; doi:10.1039/C4SC01541J

data_1547474
_publ_section_title
;
 Ru-based Z-selective metathesis catalysts with modified cyclometalated
 carbene ligands
;
_journal_name_full               'Chemical Science'
_journal_page_first              4091
_journal_page_last               4098
_journal_paper_doi               10.1039/C4SC01541J
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C37 H49 N3 O4 Ru'
_chemical_formula_sum            'C37 H49 N3 O4 Ru'
_chemical_formula_weight         700.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                74.516(3)
_cell_angle_beta                 85.839(3)
_cell_angle_gamma                64.889(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8243(8)
_cell_length_b                   11.4812(10)
_cell_length_c                   15.4419(13)
_cell_measurement_reflns_used    5015
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.36
_cell_volume                     1672.8(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2013.10-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/1 (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.819
_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  0.0881
_diffrn_reflns_av_unetI/netI     0.1739
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17576
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.093
_diffrn_reflns_theta_min         1.370
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9168
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dichroic colorless/blue'
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       'rhomboidal plate'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.744
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.744
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3640
_reflns_number_total             6036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc01541j2-2.cif
_cod_data_source_block           a14032
_cod_database_code               1547474
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.946
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C12(H12), C22(H22), C25(H25), C35(H35)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C)
;