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_1547477
_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 H51 N3 O4 Ru, C4 H10 O'
_chemical_formula_sum            'C41 H61 N3 O5 Ru'
_chemical_formula_weight         776.99
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                77.754(2)
_cell_angle_beta                 78.100(2)
_cell_angle_gamma                63.815(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5807(5)
_cell_length_b                   11.4363(6)
_cell_length_c                   18.2848(9)
_cell_measurement_reflns_used    9675
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.51
_cell_measurement_theta_min      2.16
_cell_volume                     1924.23(17)
_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 0.994
_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  0.0900
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            323089
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         45.967
_diffrn_reflns_theta_min         2.004
_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    0.454
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0710 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.9242.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.856
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         33181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                25302
_reflns_number_total             33181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc01541j2-5.cif
_cod_data_source_block           a14083
_cod_database_code               1547477
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.865
_olex2_refinement_description
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;