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_4116005
_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           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
_cell_angle_alpha                79.830(5)
_cell_angle_beta                 89.585(4)
_cell_angle_gamma                80.264(4)
_cell_formula_units_Z            2
_cell_length_a                   10.42040(10)
_cell_length_b                   10.5562(7)
_cell_length_c                   14.0425(7)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     1498.10(13)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEP-III (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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44013
_diffrn_reflns_theta_max         44.50
_diffrn_reflns_theta_min         2.44
_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    0.542
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max
;
1.507  (The closest atom is N5 at 0.647 \%A)
;
_refine_diff_density_min
;
-1.026  (The closest atom is Fe1 at 0.587 \%A)
;
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment
;
Idealized with riding model, aromatic C-H = 0.95\%A, methylene 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         20575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_obs          0.0412
_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^)+(0.0585P)^2^+0.4066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1128
_refine_ls_wR_factor_obs         0.1059
_reflns_number_observed          17208
_reflns_number_total             20616
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja993995y_2.cif
_cod_data_source_block           sd:[FE(II)(OEP)(NO)](B)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.4066P] 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^)+(0.0585P)^2^+0.4066P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116005