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_4301339
_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         'C70 H80 Cl2 N6 Ni O Pt, 3(C6 H5 Cl)'
_chemical_formula_sum            'C88 H95 Cl5 N6 Ni O Pt'
_chemical_formula_weight         1683.75
_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                89.353(12)
_cell_angle_beta                 78.992(11)
_cell_angle_gamma                85.740(12)
_cell_formula_units_Z            2
_cell_length_a                   14.277(4)
_cell_length_b                   16.450(5)
_cell_length_c                   17.619(4)
_cell_measurement_reflns_used    34824
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     4050.6(19)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39333
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    2.172
_exptl_absorpt_correction_T_max  0.7365
_exptl_absorpt_correction_T_min  0.4098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.750
_refine_diff_density_min         -2.533
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         18066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0663P)^2^+11.3539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                16140
_reflns_number_total             18066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8019149_si_002_1.cif
_cod_data_source_block           3Ni
_cod_original_cell_volume        4051(2)
_cod_database_code               4301339