Air-Stable, Electron-Deficient Fe(II) Catalytic Porphyrins. Characterization and Molecular Structures of Rare High Spin Fe(II) Hexacoordinated Porphyrins
Kathleen M. Barkigia; Magali Palacio; Yu Sun; Marc Nogues; Mark W. Renner; François Varret; Pierrette Battioni; Daniel Mansuy; Jack Fajer; Inorganic Chemistry 41 (2002) 5647–5649; doi:10.1021/ic025869s

data_4318798
_publ_contact_author
;
 K.M. Barkigia (regarding the crystallographic data and cif)
 Materials Science Dept.
 Molecular Materials Division
 Bldg. 555
 Brookhaven National Laboratory
 Upton, NY 11973 USA
;
_publ_contact_author_email       barkigia@bnl.gov
_publ_contact_author_fax         631-344-5815
_publ_contact_author_phone       631-344-7661
_publ_section_title
;
 Air-Stable, Electron-Deficient Fe(II) Catalytic Porphyrins.
 Characterization and Molecular Structures of Rare High Spin Fe(II)
 Hexacoordinated Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5647
_journal_page_last               5649
_journal_paper_doi               10.1021/ic025869s
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        acetone/hexane
_chemical_formula_structural     'C44 H12 Cl8 Fe N12 O16, 2(H2 O), 2(C3 H6 O)'
_chemical_formula_sum            'C50 H28 Cl8 Fe N12 O20'
_chemical_formula_weight         1456.29
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 112.21(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.244(2)
_cell_length_b                   27.055(4)
_cell_length_c                   13.712(1)
_cell_measurement_reflns_used    36561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.18
_cell_measurement_theta_min      2.37
_cell_volume                     5922.5(13)
_computing_cell_refinement       Denzo/Scalepack
_computing_data_collection
;
 The software provided with the MAR345 image plate detector was used to
 collect the data.
;
_computing_data_reduction        Denzo
_computing_molecular_graphics    'SHELXTL and other in-house programs'
_computing_publication_material  'CIFTAB provided with SHELXL-86'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Burla et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'MAR345 image plate detector'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'X-rays from beamline X7B at the NSLS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.93850
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36561
_diffrn_reflns_theta_max         31.18
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         3168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+88.4319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1648
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                2608
_reflns_number_total             3168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025869s_s2_3.cif
_cod_data_source_block           1(H20)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5922.5(12)
_cod_database_code               4318798