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_1547475
_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
_cell_angle_alpha                74.510(3)
_cell_angle_beta                 85.583(3)
_cell_angle_gamma                64.732(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8191(9)
_cell_length_b                   11.4795(10)
_cell_length_c                   15.4551(13)
_cell_measurement_reflns_used    8168
_cell_measurement_temperature    130
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.36
_cell_volume                     1671.3(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v4.2.0 RC20'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2012)'
_diffrn_ambient_temperature      130
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.959
_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       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15103
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.13
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS HB'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2012). SADABS v2012/1. Bruker AXS Inc. Madison, WI 53711,
USA.
;
_exptl_crystal_colour            'dichroic colorless/blue'
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.871
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5212
_reflns_number_total             6606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc01541j2-3.cif
_cod_data_source_block           p14032
_cod_original_cell_volume        1671.3(2)
_cod_database_code               1547475
_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)
;