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_4116008
_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            'C44 H24 Br4 Fe N5 O'
_chemical_formula_weight         1014.17
_chemical_name_common            '[FE(II)(TPPBr4)(NO)]'
_chemical_name_systematic
;
Nitrosyl-iron(II)-2,3,12,13-tetrabromo-5,10,15,20-tetraphenylporphyrin
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 90.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.623(4)
_cell_length_b                   10.522(2)
_cell_length_c                   19.457(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20,5
_cell_volume                     3607.6(13)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.418
_diffrn_measured_fraction_theta_max 0.418
_diffrn_measurement_device_type  '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  0.1056
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10550
_diffrn_reflns_theta_full        30.47
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    4.894
_exptl_absorpt_correction_T_max  0.17
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   DIFFAST
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_meas      ?
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.893
_refine_diff_density_min
;
-1.512 NEAREST ATOM IS BR1 AT 0.73 \%A
;
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       SHELXL
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1912P)^2^+0.8899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2538
_refine_ls_wR_factor_ref         0.3373
_reflns_number_gt                2335
_reflns_number_total             4817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993995y_5.cif
_cod_data_source_block           sd:[Fe(TPPBr4)(NO)](B)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_cell_measurement_temperature' value 'AMBIENT TEMPERATURE' was
changed to '295(2)' - the room/ambient temperature average [293;298]
in Kelvins(K) was taken.

'_diffrn_ambient_temperature' value
'AMBIENT TEMPERATURE' was changed to '295(2)' - the room/ambient
temperature average [293;298] in Kelvins(K) was taken.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1912P)^2^+0.8899P] 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^)+(0.1912P)^2^+0.8899P] 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        3607.6(12)
_cod_database_code               4116008