Cyclic(alkyl)(amino)carbene ruthenium complexes for Z-stereoselective (asymmetric) olefin metathesis
Morvan, Jennifer; Vermersch, François; Lorkowski, Jan; Talcik, Jakub; Vives, Thomas; Roisnel, Thierry; Crévisy, Christophe; Vanthuyne, Nicolas; Bertrand, Guy; Jazzar, Rodolphe; Mauduit, Marc; Catalysis Science & Technology 13 (2023) 381–388; doi:10.1039/D2CY01795D

data_1567872
_publ_section_title
;
 Cyclic(alkyl)(amino)carbene ruthenium complexes for Z-stereoselective
 (asymmetric) olefin metathesis
;
_journal_issue                   2
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              381
_journal_page_last               388
_journal_paper_doi               10.1039/D2CY01795D
_journal_volume                  13
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H40 Cl2 N2 O3 Ru'
_chemical_formula_sum            'C33 H40 Cl2 N2 O3 Ru'
_chemical_formula_weight         684.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-04-06 deposited with the CCDC.	2022-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.407(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3665(11)
_cell_length_b                   11.5707(6)
_cell_length_c                   17.4342(11)
_cell_measurement_reflns_used    9753
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5827
_cell_measurement_theta_min      2.3523
_cell_measurement_wavelength     0.71073
_cell_volume                     3164.4(3)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0575918
_diffrn_orient_matrix_UB_12      0.0030360
_diffrn_orient_matrix_UB_13      -0.0001052
_diffrn_orient_matrix_UB_21      -0.0270133
_diffrn_orient_matrix_UB_22      -0.0194072
_diffrn_orient_matrix_UB_23      -0.0618771
_diffrn_orient_matrix_UB_31      0.0041515
_diffrn_orient_matrix_UB_32      -0.0841634
_diffrn_orient_matrix_UB_33      0.0142644
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47232
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.184
_diffrn_source_current           1.0
_diffrn_source_power             50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         13184
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0041P)^2^+1.8389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    0.822
_reflns_Friedel_fraction_max     0.805
_reflns_number_gt                12201
_reflns_number_total             13184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2cy01795d2.cif
_cod_data_source_block           JM287
_cod_depositor_comments
'Adding full bibliography for 1567867--1567872.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1567872
_shelx_res_checksum              49641