Latent, Yet Highly Active Photoswitchable Olefin Metathesis Precatalysts Bearing Cyclic Alkyl Amino Carbene (CAAC)/Phosphite Ligands
Eivgi, Or; Vaisman, Anna; Lemcoff, N. Gabriel; ACS Catalysis  (2020) 703–709; doi:10.1021/acscatal.0c04909

data_4518384
_publ_section_title
;
 Latent, Yet Highly Active Photoswitchable Olefin Metathesis Precatalysts
 Bearing Cyclic Alkyl Amino Carbene (CAAC)/Phosphite Ligands
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              703
_journal_page_last               709
_journal_paper_doi               10.1021/acscatal.0c04909
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C44 H54 Cl2 N O3 P Ru'
_chemical_formula_sum            'C44 H54 Cl2 N O3 P Ru'
_chemical_formula_weight         847.82
_chemical_name_common            'Keinan182b (Ofer)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.187(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.577(4)
_cell_length_b                   15.944(4)
_cell_length_c                   15.596(4)
_cell_measurement_reflns_used    5979
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.146
_cell_measurement_theta_min      1.783
_cell_volume                     4069.2(18)
_computing_cell_refinement       'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'APEX2 (Bruker AXS)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_av_unetI/netI     0.1497
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11334
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.146
_diffrn_reflns_theta_max         25.146
_diffrn_reflns_theta_min         1.783
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       needle
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5979
_refine_ls_number_restraints     514
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0723
_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^)+(0.0936P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3704
_reflns_number_total             5979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c04909_si_002.cif
_cod_data_source_block           Keinan182b
_cod_original_cell_volume        4069.2(16)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4518384
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              28527
_shelx_hkl_checksum              96525