Synthesis, Molecular Structures, and Properties of Six-Coordinate [Fe(OEP)(L)(NO)]+ Derivatives: Elusive Nitrosyl Ferric Porphyrins
Mary K. Ellison; W. Robert Scheidt; Journal of the American Chemical Society 121 (1999) 5210–5219; doi:10.1021/ja984308q

data_4116413
_publ_section_title
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 Synthesis, Molecular Structures, and Properties of Six-Coordinate
 [Fe(OEP)(L)(NO)]+ Derivatives: Elusive Nitrosyl Ferric Porphyrins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5210
_journal_page_last               5219
_journal_paper_doi               10.1021/ja984308q
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C40 H48 Cl Fe N7 O5.4'
_chemical_formula_weight         804.55
_chemical_name_systematic
;
 ?
;
_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                83.267(16)
_cell_angle_beta                 81.528(7)
_cell_angle_gamma                76.541(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4276(12)
_cell_length_b                   10.597(2)
_cell_length_c                   18.353(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     1943.5(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-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 0.881
_diffrn_measured_fraction_theta_max 0.881
_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  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18726
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        'no measurable crystal decay'
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.9365
_exptl_absorpt_correction_T_min  0.8617
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0055(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         9960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.1056
_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^)+(0.1174P)^2^+6.0148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2584
_refine_ls_wR_factor_ref         0.3065
_reflns_number_gt                5579
_reflns_number_total             9960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja984308q_5.cif
_cod_data_source_block           sd:feoepnoprzmonclo4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1174P)^2^+6.0148P] 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^)+(0.1174P)^2^+6.0148P] 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        1943.6(5)
_cod_original_formula_sum        'C40 H48 Cl Fe N7 O5.40'
_cod_database_code               4116413