Facile Nitrite Reduction in a Non-heme Iron System: Formation of an Iron(III)-Oxo.
Matson, Ellen M.; Park, Yun Ji; Fout, Alison R.; Journal of the American Chemical Society  (2014) 141203122255000–; doi:10.1021/ja510615p

data_4123021
_publ_contact_author
; 
Alison R. Fout 
University of Illinois 
A406 CLSL, Box 54-6 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Facile Nitrite Reduction in a Non-heme Iron System: Formation of an
 Iron(III)-Oxo.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141203122255000
_journal_paper_doi               10.1021/ja510615p
_journal_year                    2014
_chemical_formula_moiety         'C36 H51 Fe N7 O, C F3 O3 S'
_chemical_formula_sum            'C37 H51 F3 Fe N7 O4 S'
_chemical_formula_weight         802.75
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_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
; 
? 
;
_cell_angle_alpha                63.7660(10)
_cell_angle_beta                 74.697(2)
_cell_angle_gamma                64.8870(10)
_cell_formula_units_Z            2
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_cell_length_b                   13.4483(5)
_cell_length_c                   13.7997(5)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.30
_cell_volume                     1917.20(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics
; 
SHELXTL v2013-4 (Bruker, 2013), CrystalMaker v2.7.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2013-1 (Bruker, 2013)'
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_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
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_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_Laue_measured_fraction_max 0.995
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_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_theta_min         2.304
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_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             846
_exptl_crystal_id                cd13eas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1, 2, 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     515
_refine_ls_number_reflns         11731
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.0006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9397
_reflns_number_total             11731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja510615p_si_002.cif
_cod_data_source_block           cd13eas_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

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 
;
_cod_original_cell_volume        1917.21(13)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4123021
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.970
_shelxl_version_number           2014-3
_shelx_res_checksum              83332
_shelx_hkl_checksum              31131