Synthetic and Mechanistic Aspects of a New Method for Ruthenium-Metalation of Porphyrins and Schiff-Bases
Júlio S. Rebouças; Elizabeth L. S. Cheu; Caroline J. Ware; Brian R. James; Kirsten A. Skov; Inorganic Chemistry 47 (2008) 7894–7907; doi:10.1021/ic800616q

data_4305636
_publ_section_title
;
Synthetic and Mechanistic Aspects of a New Method for Ruthenium-Metalation
of Porphyrins and Schiff-Bases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7894
_journal_page_last               7907
_journal_paper_doi               10.1021/ic800616q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C41 H52 N4 O2 Ru '
_chemical_formula_sum            'C41 H52 N4 O2 Ru'
_chemical_formula_weight         733.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             1998-05-25
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                90
_cell_angle_beta                 99.5847(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4420(8)
_cell_length_b                   32.418(2)
_cell_length_c                   10.7811(2)
_cell_measurement_reflns_used    15440
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     3598.6(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
'DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      150.2
_diffrn_measured_fraction_theta_full 0.869
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Quantum CCD'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.05721
_diffrn_reflns_av_sigmaI/netI    0.120
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            33364
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1544.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.07
_refine_diff_density_min         -2.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.206
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9166
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.0100
_refine_ls_shift/su_mean         0.0120
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0770
_refine_ls_wR_factor_ref         0.034
_reflns_number_gt                4171
_reflns_number_total             9166
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic800616q-file004.cif
_cod_data_source_block           bj260/RuOEP(CO)(THF)
_cod_original_cell_volume        3598.6(3)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C41 H52 N4 O2 Ru '
_cod_database_code               4305636