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_4116365
_publ_contact_author
; 
Eric Oldfield 
University of Illinois 
School of Chemical Sciences, Box 23.6 
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_moiety         'C55 H38 Fe N6 O'
_chemical_formula_sum            'C58.5 H42 Fe N6 O'
_chemical_formula_weight         900.83
_chemical_name_systematic
; 
Fe-TPP-PhNO-py 
;
_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
; 
99-01-18 revised sw 
;
_cell_angle_alpha                87.525(2)
_cell_angle_beta                 70.489(2)
_cell_angle_gamma                70.556(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9040(11)
_cell_length_b                   13.2592(12)
_cell_length_c                   16.4523(15)
_cell_measurement_reflns_used    2449
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      4
_cell_volume                     2301.3(4)
_computing_cell_refinement       'SAINT V5 (Bruker, 1998)'
_computing_data_collection       'SMART V5 (Bruker, 1998)'
_computing_data_reduction        'SAINT V5 (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL V5 (Bruker, 1998)'
_computing_publication_material  'CIFTAB (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL V5 (Bruker, 1998)'
_computing_structure_solution    'SHELXTL V5 (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       0.25
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.2177
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13404
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_time  720
_diffrn_standards_number         123
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.9398
_exptl_absorpt_correction_T_min  0.8489
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'black '
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'tabular '
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.939
_refine_ls_goodness_of_fit_obs   1.217
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         8850
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      0.942
_refine_ls_restrained_S_obs      1.198
_refine_ls_R_factor_all          0.1873
_refine_ls_R_factor_obs          0.0630
_refine_ls_shift/esd_max         -0.024
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1009
_refine_ls_wR_factor_obs         0.0801
_reflns_number_observed          3761
_reflns_number_total             8879
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9832820_1.cif
_cod_data_source_block           w27ye_Fe(TPP)(PhNO)(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^)+(0.0100P)^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^)+(0.0100P)^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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C58.50 H42 Fe N6 O'
_cod_database_code               4116365