Coordination Studies of Bis-Strapped-Hanging-Carboxylate Porphyrins. X-ray Characterization of a Five-Coordinate Iron(II) Complex with a Built-in Axial Base
Ismail Hijazi; Thierry Roisnel; Marc Fourmigué; Jean Weiss; Bernard Boitrel; Inorganic Chemistry 49 (2010) 3098–3100; doi:10.1021/ic1001072

data_4315257
_publ_section_title
;
 Coordination Studies of Bis-Strapped-Hanging-Carboxylate Porphyrins.
 X-ray Characterization of a Five-Coordinate Iron(II) Complex with a
 Built-in Axial Base
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3098
_journal_page_last               3100
_journal_paper_doi               10.1021/ic1001072
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C89 H68 Fe N10 O8, C6 H6'
_chemical_formula_sum            'C95 H74 Fe N10 O8'
_chemical_formula_weight         1539.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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             2009-10-02T16:22:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 111.745(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   58.753(14)
_cell_length_b                   12.399(3)
_cell_length_c                   23.190(6)
_cell_measurement_reflns_used    6710
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.27
_cell_measurement_wavelength     0.71073
_cell_volume                     15691(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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 0.973
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_limit_h_max       75
_diffrn_reflns_limit_h_min       -75
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            68315
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.6
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6432
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
;
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         17723
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.1239
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+195.5199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2823
_refine_ls_wR_factor_ref         0.3037
_reflns_number_gt                12032
_reflns_number_total             17723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1001072_si_001.cif
_cod_data_source_block           sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4315257