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_4318796
_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
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_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/pentane/ethanol
_chemical_formula_structural
;
 Fe N12 C44 H12 Cl8 O16, 2(C2 H5 OH), (C H2 Cl2)
;
_chemical_formula_sum            'C49 H26 Cl10 Fe N12 O18'
_chemical_formula_weight         1481.17
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                70.51(2)
_cell_angle_beta                 88.85(2)
_cell_angle_gamma                73.60(2)
_cell_formula_units_Z            1
_cell_length_a                   12.001(2)
_cell_length_b                   12.110(4)
_cell_length_c                   12.258(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      15
_cell_volume                     1605.7(8)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        'XCAD4VAX provided with SHELXL-93'
_computing_molecular_graphics    'SHELXTL and other in  house programs'
_computing_publication_material  'CIFTAB provided with SHELXS-86'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Burla et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4709
_diffrn_reflns_theta_max         58.00
_diffrn_reflns_theta_min         3.84
_diffrn_standards_decay_%        0.52
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_T_max  0.65779
_exptl_absorpt_correction_T_min  0.27857
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 Absorption corrections were made using the SHELXTL Version 5 software.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.409
_refine_ls_goodness_of_fit_ref   1.760
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.472
_refine_ls_restrained_S_obs      1.760
_refine_ls_R_factor_all          0.1971
_refine_ls_R_factor_gt           0.1093
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2861
_refine_ls_wR_factor_ref         0.2428
_reflns_number_gt                2405
_reflns_number_total             4456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025869s_s2_1.cif
_cod_data_source_block           1(EtOH)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        1605.7(7)
_cod_database_code               4318796