Relative Axial Ligand Orientation in Bis(imidazole)iron(II) Porphyrinates: Are "Picket Fence" Derivatives Different?
Jianfeng Li; Smitha M. Nair; Bruce C. Noll; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 47 (2008) 3841–3850; doi:10.1021/ic702498c

data_4304892
_publ_section_title
;
Relative Axial Ligand Orientation in Bis(imidazole)iron(II) Porphyrinates:
Are "Picket Fence" Derivatives Different?
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3841
_journal_page_last               3850
_journal_paper_doi               10.1021/ic702498c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C74 H76 Fe N12 O4, 2(C7 H8)'
_chemical_formula_sum            'C88 H92 Fe N12 O4'
_chemical_formula_weight         1437.59
_chemical_name_common            '[Fe(TpivPP)(1-vinylIm)2]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 106.108(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4924(4)
_cell_length_b                   28.2916(9)
_cell_length_c                   20.2542(6)
_cell_measurement_reflns_used    6513
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.8737
_cell_measurement_theta_min      2.3545
_cell_volume                     7427.9(4)
_computing_cell_refinement       'Brucker APEX2/SAINT'
_computing_data_collection       'Brucker APEX2'
_computing_data_reduction        'Brucker SAINT/SHELXTL'
_computing_molecular_graphics    Ortep3
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       '\f and \w 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  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            116392
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.9689
_exptl_absorpt_correction_T_min  0.9294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'translucent red'
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         16202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0710P)^2^+5.9060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                12203
_reflns_number_total             16202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702498c-file012_3.cif
_cod_data_source_block           '[Fe(TpivPP))(1-VinylIm)2]'
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_database_code               4304892