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_4116006
_publ_section_title
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 Intrinsic Structural Distortions in Five-Coordinate (Nitrosyl)iron(II)
 Porphyrinate Derivatives
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_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            'C37 H45 Cl3 Fe N5 O2'
_chemical_formula_weight         753.98
_chemical_name_common            '[Fe(oxoOEC)(NO)]'
_chemical_name_systematic
;
NITROSYL-IRON(II)-3,3,7,8,12,13,17,18-OCTAETHYL-3(H)-PORPHIN-2-ONATO(2-)
;
_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                69.946(12)
_cell_angle_beta                 83.063(7)
_cell_angle_gamma                86.647(11)
_cell_formula_units_Z            2
_cell_length_a                   8.8435(6)
_cell_length_b                   14.1716(13)
_cell_length_c                   15.6651(18)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     1830.4(3)
_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-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 0.838
_diffrn_measured_fraction_theta_max 0.838
_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  0.0842
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            53891
_diffrn_reflns_theta_full        45.54
_diffrn_reflns_theta_max         45.54
_diffrn_reflns_theta_min         2.32
_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    0.671
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   diffast
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       'asymmetrical block'
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max
;
1.492 Extremely high resolution data.  0.72 Angstroms from N(5)
;
_refine_diff_density_min
;
-2.004  Extremely high resolution data.  0.57 Angstroms away from Fe
;
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment
;
Idealized with riding model, Aromatic C-H = 0.95\%A, Aliphatic C-H = 0.99\%A.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         26043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+1.5026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2351
_reflns_number_gt                18419
_reflns_number_total             26043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993995y_3.cif
_cod_data_source_block           sd:[Fe(oxoOEC)(NO)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+1.5026P] 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^)+(0.1109P)^2^+1.5026P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4116006