Preparation of Iron Amido Complexes via Putative Fe(IV) Imido Intermediates
Robie L. Lucas; Douglas R. Powell; A. S. Borovik; Journal of the American Chemical Society 127 (2005) 11596–11597; doi:10.1021/ja052952g

data_4111873
_publ_contact_author
; 
   Prof. Andrew S. Borovik 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
;
_publ_contact_author_email       aborovik@ku.edu
_publ_contact_author_fax         1(785)8645396
_publ_contact_author_phone       1(785)8644067
_publ_section_title
;
 Preparation of Iron Amido Complexes via Putative Fe(IV) Imido
 Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11596
_journal_page_last               11597
_journal_paper_doi               10.1021/ja052952g
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'K 1+, (C26 H45 Fe N7 O3) 1-'
_chemical_formula_sum            'C26 H45 Fe K N7 O3'
_chemical_formula_weight         598.64
_chemical_name_systematic
; 
 ? 
;
_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                108.008(5)
_cell_angle_beta                 100.887(6)
_cell_angle_gamma                100.453(6)
_cell_formula_units_Z            2
_cell_length_a                   10.256(3)
_cell_length_b                   11.650(4)
_cell_length_c                   14.419(5)
_cell_measurement_reflns_used    2586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.90
_cell_measurement_theta_min      2.25
_cell_volume                     1555.0(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w 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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13829
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       plate
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1000P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1904
_reflns_number_gt                4115
_reflns_number_total             6329
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja052952gsi20050513_055955.cif
_cod_data_source_block           compound_K[Fe^III^H~2~2(NHTol)]_
_cod_database_code               4111873