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_4116361
_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         'C41 H50 N6 O Fe, C3 F7'
_chemical_formula_sum            'C44 H57 Fe N6 O'
_chemical_formula_weight         741.81
_chemical_name_systematic
; 
Fe(OEP)(1-MeIm)(CO) 
;
_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
; 
02-22-98 (lks) 
;
_cell_angle_alpha                84.19(3)
_cell_angle_beta                 69.72(3)
_cell_angle_gamma                69.85(3)
_cell_formula_units_Z            2
_cell_length_a                   11.872(2)
_cell_length_b                   13.192(3)
_cell_length_c                   14.305(3)
_cell_measurement_reflns_used    2783
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_volume                     1972.5(9)
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10326
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        4.2
_diffrn_standards_interval_time  360
_diffrn_standards_number         145
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.9295
_exptl_absorpt_correction_T_min  0.8470
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         .665
_refine_diff_density_min         -.592
_refine_diff_density_rms         .062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6519
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_obs          0.0594
_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^)+(0.0610P)^2^+0.9241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1673
_refine_ls_wR_factor_obs         0.1283
_reflns_number_observed          3873
_reflns_number_total             6785
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9832818_1.cif
_cod_data_source_block           h46c_Fe(OEP)(CO)(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^)+(0.0610P)^2^+0.9241P] 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^)+(0.0610P)^2^+0.9241P] 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        1972.5(7)
_cod_database_code               4116361