Oxidative Group Transfer to a Triiron Complex to Form a Nucleophilic μ3-Nitride, [Fe3(μ3-N)]-
Tamara M. Powers; Alison R. Fout; Shao-Liang Zheng; Theodore A. Betley; Journal of the American Chemical Society 133 (2011) 3336–3338; doi:10.1021/ja2003445

data_4105764
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
Harvard University
Mallinckrodt 306E
12 Oxford Street
Cambridge, MA 02138
;
_publ_contact_author_email       betley@chemistry.harvard.edu
_publ_contact_author_name        'Professor Theodore A. Betley'
_publ_contact_author_phone       617-496-9944
_publ_section_title
;
 Oxidative Group Transfer to a Triiron Complex to Form a Nucleophilic
 \m3-Nitride, [Fe3(\m3-N)]-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3336
_journal_page_last               3338
_journal_paper_doi               10.1021/ja2003445
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C49 H81 Fe3 N6 O Si3'
_chemical_formula_weight         1022.02
_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-97
_cell_angle_alpha                84.540(2)
_cell_angle_beta                 83.122(2)
_cell_angle_gamma                75.734(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6174(10)
_cell_length_b                   10.8500(10)
_cell_length_c                   23.503(2)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.719
_cell_measurement_theta_min      2.251
_cell_volume                     2599.1(4)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22864
_diffrn_reflns_theta_full        25.77
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.8135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9811
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+1.2488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                7729
_reflns_number_total             9811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2003445_si_002_1.cif
_cod_data_source_block           tbsLFe3thf
_cod_database_code               4105764