Solid-State NMR, Mössbauer, Crystallographic, and Density Functional Theory Investigation of Fe-O2 and Fe-O2 Analogue Metalloporphyrins and Metalloproteins
Nathalie Godbout; Lori K. Sanders; Renzo Salzmann; Robert H. Havlin; Mark Wojdelski; Eric Oldfield; Journal of the American Chemical Society 121 (1999) 3829–3844; doi:10.1021/ja9832820

data_4116366
_publ_contact_author
; 
Eric Oldfield 
University of Illinois at Urbana-Champaign 
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, M\"ossbauer, Crystallographic, and Density Functional
 Theory Investigation of Fe-O2 and Fe-O2 Analogue Metalloporphyrins and
 Metalloproteins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3829
_journal_page_last               3844
_journal_paper_doi               10.1021/ja9832820
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C64 H51 Fe N7 O'
_chemical_formula_weight         989.97
_chemical_name_systematic
; 
Fe(TPP)(NODMA)(py)
;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_audit_update_record
; 
31-08-1998 (srw/lks) 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.823(2)
_cell_length_b                   12.3148(8)
_cell_length_c                   21.4172(13)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_volume                     10239.5(11)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXTL (Bruker, 1998)'
_diffrn_ambient_temperature      198(2)
_diffrn_measurement_device       'Siemens Platform/CCD'
_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_refln_elapsed_time       0.1667
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_sigmaI/netI    0.1468
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26755
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_time  360
_diffrn_standards_number         446
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_correction_T_min  0.8977
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tabular
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.300
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8413
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.297
_refine_ls_R_factor_all          0.1429
_refine_ls_R_factor_obs          0.0624
_refine_ls_shift/esd_max         0.056
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1458
_refine_ls_wR_factor_obs         0.1270
_reflns_number_observed          4388
_reflns_number_total             8413
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9832820_2.cif
_cod_data_source_block           w19zia_Fe(TPP)(NODMA)(py)
_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^)+(0.0550P)^2^+0.0000P] 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^)+(0.0550P)^2^+0.0000P] 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        10239.6(11)
_cod_database_code               4116366