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_4318797
_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, propanol'
_chemical_formula_structural
;
 C44 H12 Cl8 Fe N12 O16, 2(C3 H8 O), 2(C3 H6 O)
;
_chemical_formula_sum            'C56 H40 Cl8 Fe N12 O20'
_chemical_formula_weight         1540.45
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.36(1)
_cell_angle_beta                 91.51(1)
_cell_angle_gamma                104.58(1)
_cell_formula_units_Z            1
_cell_length_a                   11.346(1)
_cell_length_b                   11.655(1)
_cell_length_c                   12.766(1)
_cell_measurement_reflns_used    27261
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.49
_cell_measurement_theta_min      2.2
_cell_volume                     1567.6(3)
_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 Version 5.0 (Sheldrick, 1995) and other in-house programs.
;
_computing_publication_material  'CIFTAB provided with SHELXS-86'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_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     0.90350
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36733
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green-blue'
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         3822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.228
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+1.8234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0861
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                3717
_reflns_number_total             3826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025869s_s2_2.cif
_cod_data_source_block           1(PrOH)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        1567.6(2)
_cod_database_code               4318797