Solid-State NMR, Crystallographic and Density Functional Theory Investigation of Fe-CO and Fe-CO Analogue Metalloporphyrins and Metalloproteins
Renzo Salzmann; Michael T. McMahon; Nathalie Godbout; Lori K. Sanders; Mark Wojdelski; Eric Oldfield; Journal of the American Chemical Society 121 (1999) 3818–3828; doi:10.1021/ja9832818

data_4116364
_publ_contact_author
; 
Eric Oldfield 
University of Illinois 
Department of Chemistry Box 11.6 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       eo@chad.scs.uiuc.edu
_publ_contact_author_fax         '1  217 244 0997'
_publ_contact_author_phone       '1  217 333 3374'
_publ_section_title
;
 Solid-State NMR, Crystallographic and Density Functional Theory
 Investigation of Fe-CO and Fe-CO Analogue Metalloporphyrins and
 Metalloproteins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3818
_journal_page_last               3828
_journal_paper_doi               10.1021/ja9832818
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C52 H41 N7 Fe, C2.5 H6'
_chemical_formula_sum            'C54.5 H47 Fe N7'
_chemical_formula_weight         855.84
_chemical_name_systematic
; 
Fe(TPP)(iPrNC)(1-MeIm) 
;
_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
_audit_update_record
; 
11-2-97,rs 
;
_cell_angle_alpha                73.86
_cell_angle_beta                 78.0500(10)
_cell_angle_gamma                79.5640(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9981(7)
_cell_length_b                   13.2076(8)
_cell_length_c                   17.1650(11)
_cell_measurement_reflns_used    3532
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_volume                     2322.8(3)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXTL (Siemens, 1994)'
_computing_structure_solution    'SHELXTL (Siemens, 1994)'
_diffrn_ambient_temperature      198(2)
_diffrn_measurement_device       'Siemens Platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11376
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  360
_diffrn_standards_number         140
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.8249
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platy
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         .733
_refine_diff_density_min         -.348
_refine_diff_density_rms         .076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.149
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         7013
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.146
_refine_ls_restrained_S_obs      1.150
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_obs          0.0663
_refine_ls_shift/esd_max         0.016
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+3.9678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1988
_refine_ls_wR_factor_obs         0.1596
_reflns_number_observed          4739
_reflns_number_total             7147
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9832818_4.cif
_cod_data_source_block           h06a_Fe(TPP)(iPrNC)(1-MeIm)
_cod_depositor_comments
;
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^)+(0.0724P)^2^+3.9678P] 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^)+(0.0724P)^2^+3.9678P] 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        2322.9(3)
_cod_original_formula_sum        'C54.50 H47 Fe N7'
_cod_database_code               4116364