Synthesis, Characterization, and Electrochemical Studies of β,β'-Fused Metallocenoporphyrins
Hong J. H. Wang; Laurent Jaquinod; Marilyn M. Olmstead; M. Graça H. Vicente; Karl M. Kadish; Zhongping Ou; Kevin M. Smith; Inorganic Chemistry 46 (2007) 2898–2913; doi:10.1021/ic062303l

data_4307812
_publ_section_title
;
Synthesis, Characterization, and Electrochemical Studies of \b,\b'-Fused
Metallocenoporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2898
_journal_page_last               2913
_journal_paper_doi               10.1021/ic062303l
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C232 H211 Fe2 N16 O13 Zn4'
_chemical_formula_weight         3804.35
_chemical_name_common
{Cp2Fe[ZnTPP(THF)]2}{Cp2Fe[ZnTPP(THF)ZnTPP(MeOH)]}.3MeOH.6THF
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 106.309(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.327(5)
_cell_length_b                   19.145(3)
_cell_length_c                   29.603(5)
_cell_measurement_reflns_used    904
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      2.3
_cell_volume                     18128(5)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.161
_diffrn_reflns_av_sigmaI/netI    0.155
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            170844
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.9564
_exptl_absorpt_correction_T_min  0.8525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7964
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.503
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         26022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1639
_refine_ls_R_factor_gt           0.0906
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1240P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2470
_reflns_number_gt                14016
_reflns_number_total             26022
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic062303lsi20061203_122117.cif
_cod_data_source_block           mn1291
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4307812