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_4116004
_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            'C36 H44 Fe N5 O'
_chemical_formula_weight         618.61
_chemical_name_common            '[FE(II)(OEP)(NO)]'
_chemical_name_systematic
;
NITROSYL-IRON(II)-2,3,7,8,12,13,17,18-OCTAETHYLPORPHYRIN
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.854(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.950(2)
_cell_length_b                   22.361(2)
_cell_length_c                   9.6966(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     3133.2(5)
_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-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       '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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22655
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        'no measurable crystal decay'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.283
_refine_ls_goodness_of_fit_obs   1.332
_refine_ls_hydrogen_treatment
;
Idealized with riding model, aromatic C-H = 0.95\%A, aliphatic C-H = 0.99\%A,
methyl C-H = 0.98\%A.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.284
_refine_ls_restrained_S_obs      1.332
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_obs          0.0421
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+5.6017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1561
_refine_ls_wR_factor_obs         0.1515
_reflns_number_observed          6949
_reflns_number_total             7890
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja993995y_1.cif
_cod_data_source_block           sd:[FE(II)(OEP)(NO)](A)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+5.6017P] 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^)+(0.0525P)^2^+5.6017P] 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        3133.3(4)
_cod_database_code               4116004