Ruthenium(II) Porphyrin Quinoid Carbene Complexes: Synthesis, Crystal Structure, and Reactivity toward Carbene Transfer and Hydrogen Atom Transfer Reactions.
Wang, Hai-Xu; Wan, Qingyun; Wu, Kai; Low, Kam-Hung; Yang, Chen; Zhou, Cong-Ying; Huang, Jie-Sheng; Che, Chi-Ming; Journal of the American Chemical Society 141 (2019) 9027–9046; doi:10.1021/jacs.9b03357

data_4127591
_publ_section_title
;
 Ruthenium(II) Porphyrin Quinoid Carbene Complexes: Synthesis, Crystal
 Structure, and Reactivity toward Carbene Transfer and Hydrogen Atom
 Transfer Reactions.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9027
_journal_page_last               9046
_journal_paper_doi               10.1021/jacs.9b03357
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C63 H58 Br2 N4 O2 Ru, C H4 O, C H2 Cl2'
_chemical_formula_sum            'C65 H64 Br2 Cl2 N4 O3 Ru'
_chemical_formula_weight         1280.99
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 95.902(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9947(17)
_cell_length_b                   19.257(2)
_cell_length_c                   19.861(2)
_cell_measurement_reflns_used    1170
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      3
_cell_volume                     6085.0(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX3 v2015.5-2 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 1024
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
'Bruker D8 VENTURE KAPPA goniometer PHOTON II CMOS'
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.1451
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            104807
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        52.980
_diffrn_reflns_theta_max         52.980
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'Excillum MetalJet D2'
_exptl_absorpt_coefficient_mu    3.211
_exptl_absorpt_correction_T_max  0.3057
_exptl_absorpt_correction_T_min  0.1075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       rod
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.560
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10672
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.1055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+87.3482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2264
_refine_ls_wR_factor_ref         0.2385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8400
_reflns_number_total             10672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03357_si_003.cif
_cod_data_source_block           chem0386_sq
_cod_original_cell_volume        6084.9(11)
_cod_database_code               4127591
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.370
_shelx_estimated_absorpt_t_max   0.859
_shelx_res_checksum              62908
_shelx_hkl_checksum              77608
_shelx_fab_checksum              17245