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_1567871
_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         'C35 H44 Cl2 N2 O3 Ru'
_chemical_formula_sum            'C35 H44 Cl2 N2 O3 Ru'
_chemical_formula_weight         712.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.7486(6)
_cell_length_b                   19.3141(12)
_cell_length_c                   43.739(3)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.6158
_cell_measurement_theta_min      2.3282
_cell_measurement_wavelength     0.710730
_cell_volume                     7390.6(9)
_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 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0571118
_diffrn_orient_matrix_UB_12      -0.0119883
_diffrn_orient_matrix_UB_13      -0.0190837
_diffrn_orient_matrix_UB_21      0.0913655
_diffrn_orient_matrix_UB_22      0.0128463
_diffrn_orient_matrix_UB_23      -0.0125125
_diffrn_orient_matrix_UB_31      0.0381576
_diffrn_orient_matrix_UB_32      -0.0487028
_diffrn_orient_matrix_UB_33      0.0013971
_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  0.0749
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            52972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.654
_diffrn_reflns_theta_min         2.109
_diffrn_source_current           1.0
_diffrn_source_power             50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.735
_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    1.281
_exptl_crystal_description       plate
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.124
_refine_diff_density_min         -1.846
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details
;
Flack x determined using 4202 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         16456
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+70.8688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    0.957
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                12661
_reflns_number_total             16456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2cy01795d2.cif
_cod_data_source_block           JM3542
_cod_depositor_comments
'Adding full bibliography for 1567867--1567872.cif.'
_cod_original_cell_volume        7390.7(8)
_cod_database_code               1567871
_shelx_res_checksum              53320
_shelx_fab_checksum              15955