Porphyrin Pincer Complexes: Peripherally Cyclometalated Porphyrins and Their Catalytic Activities Controlled by Central Metals
Shigeru Yamaguchi; Taisuke Katoh; Hiroshi Shinokubo; Atsuhiro Osuka; Journal of the American Chemical Society 129 (2007) 6392–6393; doi:10.1021/ja072218s

data_4109439
_publ_section_title
;
 Porphyrin Pincer Complexes: Peripherally Cyclometalated Porphyrins and
 Their Catalytic Activities Controlled by Central Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6392
_journal_page_last               6393
_journal_paper_doi               10.1021/ja072218s
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety
'C72 H77 Cl N6 Ni Pd, C2.67 H2.51 Cl4 N0.84, 3(C Cl4), C2 H3 N'
_chemical_formula_sum            'C79.67 H82.51 Cl17 N7.84 Ni Pd'
_chemical_formula_weight         1917.58
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.498(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.698(3)
_cell_length_b                   19.250(3)
_cell_length_c                   33.159(6)
_cell_measurement_reflns_used    6630
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.12
_cell_volume                     8741(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43280
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.9077
_exptl_absorpt_correction_T_min  0.6380
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       prism
_exptl_crystal_F_000             3913
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.028
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         15262
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0998
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1105P)^2^+116.7033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2655
_refine_ls_wR_factor_ref         0.2816
_reflns_number_gt                12303
_reflns_number_total             15262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072218ssi20070329_083816.cif
_cod_data_source_block           70206yamaguchi
_cod_original_cell_volume        8740(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4109439