Structural Characterization of Zinc and Iron (II/III) Complexes of a Porphyrin Bearing Two Built-in Nitrogen Bases. An Example of High-Spin Diaqua-Iron(III) Bromo Complex
Hijazi, Ismail; Roisnel, Thierry; Even-Hernandez, Pascale; Geneste, Florence; Cador, Olivier; Guizouarn, Thierry; Boitrel, Bernard; Inorganic Chemistry 49 (2010) 7536–7544; doi:10.1021/ic1009384

data_4333246
_publ_section_title
;
 Structural Characterization of Zinc and Iron (II/III) Complexes of a
 Porphyrin Bearing Two Built-in Nitrogen Bases. An Example of High-Spin
 Diaqua-Iron(III) Bromo Complex
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   16
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7536
_journal_page_last               7544
_journal_paper_doi               10.1021/ic1009384
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C88 H64 N12 O4 Zn'
_chemical_formula_sum            'C88 H64 N12 O4 Zn'
_chemical_formula_weight         1418.88
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-11-25T14:25:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.704(4)
_cell_length_b                   23.194(4)
_cell_length_c                   35.517(7)
_cell_measurement_reflns_used    2949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.6
_cell_measurement_theta_min      2.46
_cell_measurement_wavelength     0.71073
_cell_volume                     16232(5)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SAINT (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1602
_diffrn_reflns_av_unetI/netI     0.3721
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            69146
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             5904
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.869
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.34(2)
_refine_ls_extinction_coef       0.00460(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         32443
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.2359
_refine_ls_R_factor_gt           0.1041
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2555
_reflns_number_gt                11540
_reflns_number_total             32443
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4316282
_cod_data_source_file            ic1009384sup1.cif
_cod_data_source_block           dipyZn
_cod_database_code               4333246