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_4123022
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 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 N8 O2 Zn, C F3 O3 S, C4 H10 O'
_chemical_formula_sum            'C41 H61 F3 N8 O6 S Zn'
_chemical_formula_weight         916.40
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4321(4)
_cell_length_b                   23.9090(6)
_cell_length_c                   25.8489(7)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.28
_cell_volume                     8919.3(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      104(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd75lsa
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            86080
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.079
_diffrn_reflns_theta_min         2.280
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.82065
_exptl_absorpt_correction_T_min  0.62247
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             3872
_exptl_crystal_id                cd75lsa
_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 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         8813
_refine_ls_number_restraints     1534
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+18.6240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6799
_reflns_number_total             8813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja510615p_si_002.cif
_cod_data_source_block           cd75lsa_5
_cod_database_code               4123022
_shelx_estimated_absorpt_t_min   0.721
_shelx_estimated_absorpt_t_max   0.879
_shelxl_version_number           2014/6
_shelx_res_checksum              49383
_shelx_hkl_checksum              78510