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_4116363
_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         'C42 H52 N6 O Cl2 Os '
_chemical_formula_sum            'C42 H52 Cl2 N6 O Os'
_chemical_formula_weight         918.00
_chemical_name_systematic
; 
Os(OEP)(CO)(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
; 
09-10-97(lks) 
;
_cell_angle_alpha                80.6350(10)
_cell_angle_beta                 76.7310(10)
_cell_angle_gamma                72.2190(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3677(3)
_cell_length_b                   12.9871(4)
_cell_length_c                   15.9564(5)
_cell_measurement_reflns_used    3856
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_volume                     1981.25(11)
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.1037
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10705
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  360
_diffrn_standards_number         185
_exptl_absorpt_coefficient_mu    3.394
_exptl_absorpt_correction_T_max  0.9307
_exptl_absorpt_correction_T_min  0.7516
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.316
_refine_diff_density_min         -1.525
_refine_diff_density_rms         .189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.147
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6914
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.148
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_obs          0.0653
_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^)+(0.0249P)^2^+17.0365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1449
_refine_ls_wR_factor_obs         0.1228
_reflns_number_observed          5297
_reflns_number_total             6916
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9832818_3.cif
_cod_data_source_block           h82b_Os(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^)+(0.0249P)^2^+17.0365P] 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^)+(0.0249P)^2^+17.0365P] 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        1981.25(10)
_cod_database_code               4116363