Primary and Secondary Phosphine Complexes of Iron Porphyrins and Ruthenium Phthalocyanine: Synthesis, Structure, and P-H Bond Functionalization
Jie-Sheng Huang; Guang-Ao Yu; Jin Xie; Kwok-Ming Wong; Nianyong Zhu; Chi-Ming Che; Inorganic Chemistry 47 (2008) 9166–9181; doi:10.1021/ic800484k

data_4305491
_publ_section_title
;
Primary and Secondary Phosphine Complexes of Iron Porphyrins and Ruthenium
Phthalocyanine: Synthesis, Structure, and P-H Bond Functionalization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9166
_journal_page_last               9181
_journal_paper_doi               10.1021/ic800484k
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C70 H44 Cl12 Fe N4 P2'
_chemical_formula_sum            'C70 H44 Cl12 Fe N4 P2'
_chemical_formula_weight         1484.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                91.57(3)
_cell_angle_beta                 107.00(3)
_cell_angle_gamma                117.49(3)
_cell_formula_units_Z            1
_cell_length_a                   12.279(4)
_cell_length_b                   12.517(4)
_cell_length_c                   12.727(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1628.7(11)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0991
_diffrn_reflns_av_sigmaI/netI    0.1206
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14231
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    ride-on
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1692
_refine_ls_R_factor_gt           0.0933
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+6.8431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2485
_reflns_number_gt                4129
_reflns_number_total             7232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800484k_si_001_2.cif
_cod_data_source_block           complex_2b
_cod_original_cell_volume        1628.7(9)
_cod_database_code               4305491