Intrinsic Structural Distortions in Five-Coordinate (Nitrosyl)iron(II) Porphyrinate Derivatives
W. Robert Scheidt; Hugues F. Duval; Teresa J. Neal; Mary K. Ellison; Journal of the American Chemical Society 122 (2000) 4651–4659; doi:10.1021/ja993995y

data_4116007
_publ_section_title
;
 Intrinsic Structural Distortions in Five-Coordinate (Nitrosyl)iron(II)
 Porphyrinate Derivatives
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4651
_journal_page_last               4659
_journal_paper_doi               10.1021/ja993995y
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C45.5 H24 Br4 Cl4.5 Fe N5 O'
_chemical_formula_weight         1191.71
_chemical_name_common            '[Fe(TPPBr4)(NO)]'
_chemical_name_systematic
;
Nitrosyl-iron(II)-2,3,12,13-tetrabromo-5,10,15,20-tetraphenylporphyrin
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.750(3)
_cell_length_b                   15.293(3)
_cell_length_c                   17.608(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     4295.2(17)
_computing_cell_refinement       Madnes
_computing_data_collection       Madnes
_computing_data_reduction        'Madnes (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'OrtepIII (Burnett, Johnson, 1996)'
_computing_publication_material  Shelxl-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.842
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'Enraf-Nonius fast area detector'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1095
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31981
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    4.397
_exptl_absorpt_correction_T_max  0.506
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_type   difabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_description       needle
_exptl_crystal_F_000             2330
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max
;
1.145 NEAREST ATOM IS 1Br(b4) AT 1.16 \%A
;
_refine_diff_density_min
;
-1.025 NEAREST ATOM IS 2Br(b1) AT 0.85 \%A
;
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         10958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+13.2065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.2321
_reflns_number_gt                6661
_reflns_number_total             10958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993995y_4.cif
_cod_data_source_block           sd:[Fe(TPPBr4)(NO)](A'&A")
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+13.2065P] 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^)+(0.1135P)^2^+13.2065P] 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        4294.9(15)
_cod_original_formula_sum        'C45.50 H24 Br4 Cl4.50 Fe N5 O'
_cod_database_code               4116007