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_4304890
_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         'C72 H76 Fe N12 O4, C4 H6 N2'
_chemical_formula_sum            'C76 H82 Fe N14 O4'
_chemical_formula_weight         1311.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 103.7820(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2358(3)
_cell_length_b                   19.2487(5)
_cell_length_c                   27.4149(6)
_cell_measurement_reflns_used    9599
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.19
_cell_volume                     6783.5(3)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2005; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker x8-ApexII 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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            69821
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.9506
_exptl_absorpt_correction_T_min  0.9146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2004) SADABS, University of G\"ottingen, Germany'
_exptl_crystal_colour            'translucent red'
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.898
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         16877
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0764P)^2^+6.6032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                12814
_reflns_number_total             16877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702498c-file012_1.cif
_cod_data_source_block           '[Fe(TpivPP))(1-MeIm)2]'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4304890