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_4304891
_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         '2(C74 H80 Fe N12 O4), C7 H7'
_chemical_formula_sum            'C155 H167 Fe2 N24 O8'
_chemical_formula_weight         2605.83
_chemical_name_common            '[Fe(TpivPP)(1-EtIm)2]'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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                75.5240(10)
_cell_angle_beta                 88.1680(10)
_cell_angle_gamma                65.3220(10)
_cell_formula_units_Z            1
_cell_length_a                   13.1799(3)
_cell_length_b                   13.3672(3)
_cell_length_c                   22.2734(5)
_cell_measurement_temperature    100(2)
_cell_volume                     3440.79(14)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61045
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         0.95
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9726
_exptl_absorpt_correction_T_min  0.9160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1381
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         13447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0557P)^2^+3.2313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                10433
_reflns_number_total             13447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702498c-file012_2.cif
_cod_data_source_block           '[Fe(TpivPP))(1-EIm)2]'
_cod_original_cell_volume        3440.79(13)
_cod_database_code               4304891