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_1567868
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H43 Cl2 N O Ru'
_chemical_formula_sum            'C31 H43 Cl2 N O Ru'
_chemical_formula_weight         617.63
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2022-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.479(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8604(9)
_cell_length_b                   17.881(2)
_cell_length_c                   18.3060(19)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4681
_cell_measurement_theta_min      2.2780
_cell_measurement_wavelength     0.710730
_cell_volume                     2887.0(5)
_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-2019_2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CMOS-PHOTON70
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0782971
_diffrn_orient_matrix_UB_12      -0.0375220
_diffrn_orient_matrix_UB_13      -0.0183742
_diffrn_orient_matrix_UB_21      0.0704136
_diffrn_orient_matrix_UB_22      -0.0414682
_diffrn_orient_matrix_UB_23      0.0171276
_diffrn_orient_matrix_UB_31      -0.0420287
_diffrn_orient_matrix_UB_32      0.0004266
_diffrn_orient_matrix_UB_33      0.0487911
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22225
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.235
_diffrn_source_current           1.00
_diffrn_source_power             50.0
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0255P)^2^+3.6957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                5625
_reflns_number_total             6584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2cy01795d2.cif
_cod_data_source_block           JM829
_cod_depositor_comments
'Adding full bibliography for 1567867--1567872.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1567868
_shelx_res_checksum              49756