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_4127588
_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         'C64 H42 F20 N4 O3 Ru, C6 H14'
_chemical_formula_sum            'C70 H56 F20 N4 O3 Ru'
_chemical_formula_weight         1482.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.696(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1060(6)
_cell_length_b                   19.2811(11)
_cell_length_c                   25.7572(14)
_cell_measurement_reflns_used    217
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.8
_cell_volume                     6450.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX3 v2015.5-2 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      151(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE FIXED-CHI PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            67858
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.134
_diffrn_reflns_theta_max         25.134
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         11469
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0158P)^2^+8.4280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8928
_reflns_number_total             11469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03357_si_004.cif
_cod_data_source_block           mo_CHEM0440
_cod_database_code               4127588
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              42877
_shelx_hkl_checksum              72740