Five-Coordinate Iron(III) Porphycenes: 1H NMR, Magnetic, and Structural Studies
Krystyna Rachlewicz; Lechosław Latos-Grażyński; Emanuel Vogel; Zbigniew Ciunik; Lucjan B. Jerzykiewicz; Inorganic Chemistry 41 (2002) 1979–1988; doi:10.1021/ic010725j

data_4317762
_publ_section_title
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 Five-Coordinate Iron(III) Porphycenes: 1H NMR, Magnetic, and Structural
 Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1979
_journal_page_last               1988
_journal_paper_doi               10.1021/ic010725j
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C32 H36 Fe N4'
_chemical_formula_sum            'C32 H36 Fe N4'
_chemical_formula_weight         532.50
_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-97
_cell_angle_alpha                81.17(3)
_cell_angle_beta                 84.85(3)
_cell_angle_gamma                89.29(3)
_cell_formula_units_Z            1
_cell_length_a                   5.196(1)
_cell_length_b                   9.857(2)
_cell_length_c                   12.506(3)
_cell_measurement_reflns_used    873
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     630.4(2)
_computing_cell_refinement       'Kuma CCDKM4 software, version 1.166'
_computing_data_collection       'Kuma CCDKM4 software, version 1.166'
_computing_data_reduction        'Kuma CCDKM4 software, version 1.166'
_computing_molecular_graphics    'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.838
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       '\w scan'
_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  0.1040
_diffrn_reflns_av_sigmaI/netI    0.2159
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4090
_diffrn_reflns_theta_full        28.53
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.9399
_exptl_absorpt_correction_T_min  0.8847
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'rhombic shape'
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       dark
_exptl_crystal_F_000             282
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1940
_refine_ls_R_factor_gt           0.0875
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2412
_reflns_number_gt                1106
_reflns_number_total             2674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010725j_2.cif
_cod_data_source_block           compound_2_C32H36FeN4
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4317762