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_1547473
_publ_section_title
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 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 H51 N3 O4 Ru'
_chemical_formula_sum            'C37 H51 N3 O4 Ru'
_chemical_formula_weight         702.87
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 104.291(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0174(7)
_cell_length_b                   10.8674(5)
_cell_length_c                   20.3090(9)
_cell_measurement_reflns_used    9476
_cell_measurement_temperature    100
_cell_measurement_theta_max      39.74
_cell_measurement_theta_min      2.64
_cell_volume                     3425.7(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2014.1-1 (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-2014/2 (Sheldrick, 2014)'
_computing_structure_solution    'XT-2014/1 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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  0.0959
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            238162
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         44.145
_diffrn_reflns_theta_min         1.861
_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    0.500
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0670 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.9294.
The \l/2 correction factor is 0.0015.
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_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.378
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         26425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.003
_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          0.0798
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17928
_reflns_number_total             26425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc01541j2-1.cif
_cod_data_source_block           a14093
_cod_database_code               1547473
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.873
_olex2_refinement_description
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1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C35A)=Sof(H35A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37A)=Sof(H37D)=
 Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(C35)=Sof(H35)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=FVAR(1)
3.a Idealised Me refined as rotating group:
 C36(H36D,H36E,H36F), C37A(H37D,H37E,H37F)
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