Synthesis and Characterization of anti-bisFe(III) Porphyrins, syn-bisFe(III)-μ-oxo Porphyrin, and syn-bisFe(III)-μ-oxo Porphyrin Cation Radical
Sudip Kumar Ghosh; Ranjan Patra; Sankar Prasad Rath; Inorganic Chemistry 49 (2010) 3449–3460; doi:10.1021/ic100002c

data_4315212
_publ_contact_author_address
;Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur-208016, INDIA
;
_publ_contact_author_email       sprath@iitk.ac.in
_publ_contact_author_fax         91-512-2597436
_publ_contact_author_name        'Dr. Sankar Prasad Rath'
_publ_contact_author_phone       91-512-2597251
_publ_section_title
;
 Synthesis and Characterization of anti-bisFe(III) Porphyrins,
 syn-bisFe(III)-\m-oxo Porphyrin, and syn-bisFe(III)-\m-oxo Porphyrin
 Cation Radical
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3449
_journal_page_last               3460
_journal_paper_doi               10.1021/ic100002c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C74 H90 Cl2 Fe2 N8 O8, H2 O'
_chemical_formula_sum            'C74 H92 Cl2 Fe2 N8 O9'
_chemical_formula_weight         1420.16
_chemical_name_common            'Bis Fe(III)porphyrin perchlorato, 2c'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 99.118(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.485(4)
_cell_length_b                   20.610(8)
_cell_length_c                   14.784(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.4
_cell_volume                     3455(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       \w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1029
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7700
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         7700
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0912
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+6.9955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2107
_refine_ls_wR_factor_ref         0.2421
_reflns_number_gt                5206
_reflns_number_total             7700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100002c_si_001.cif
_cod_data_source_block           15sepam
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315212