Double Cleavage of sp2 C-H and sp3 C-H Bonds on One Metal Center: DMF-Appended Cyclometalated Platinum(II) and -(IV) Porphyrins
Shigeru Yamaguchi; Hiroshi Shinokubo; Atsuhiro Osuka; Inorganic Chemistry 48 (2009) 795–797; doi:10.1021/ic8019149

data_4301343
_publ_section_title
;
Double Cleavage of sp2 C-H and sp3 C-H Bonds on One Metal Center:
DMF-Appended Cyclometalated Platinum(II) and -(IV) Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              795
_journal_page_last               797
_journal_paper_doi               10.1021/ic8019149
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C73 H87 N6 O2 Pt Zn, C3 H8 O, 2(C H Cl3)'
_chemical_formula_sum            'C78 H97 Cl6 N6 O3 Pt Zn'
_chemical_formula_weight         1639.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.391(9)
_cell_angle_beta                 81.968(11)
_cell_angle_gamma                78.623(12)
_cell_formula_units_Z            2
_cell_length_a                   11.446(4)
_cell_length_b                   14.031(4)
_cell_length_c                   25.134(6)
_cell_measurement_reflns_used    3.0
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      123.1
_cell_measurement_theta_min      27.5
_cell_volume                     3895(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37879
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.6500
_exptl_absorpt_correction_T_min  0.3321
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1682
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.543
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1265
_refine_ls_number_reflns         17525
_refine_ls_number_restraints     1332
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+9.2413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                14345
_reflns_number_total             17525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8019149_si_002_5.cif
_cod_data_source_block           5Zn
_cod_database_code               4301343