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_4317761
_publ_section_title
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 Five-Coordinate Iron(III) Porphycenes: 1H NMR, Magnetic, and Structural
 Studies
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_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_sum            'C32 H36 Cl Fe N4'
_chemical_formula_weight         567.95
_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                112.22(3)
_cell_angle_beta                 97.85(3)
_cell_angle_gamma                96.76(3)
_cell_formula_units_Z            2
_cell_length_a                   9.496(2)
_cell_length_b                   12.281(2)
_cell_length_c                   13.338(3)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      2.92
_cell_volume                     1401.9(6)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.875
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10413
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.9614
_exptl_absorpt_correction_T_min  0.8791
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                4574
_reflns_number_total             6514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010725j_1.cif
_cod_data_source_block           compound_1_C32H36ClFeN4
_cod_depositor_comments
;
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^)+(0.0499P)^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^)+(0.0499P)^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 
;
_cod_original_cell_volume        1401.9(5)
_cod_database_code               4317761