Synthesis and Characterization of an Iron(IV) Ketimide Complex
Richard A. Lewis; Guang Wu; Trevor W. Hayton; Journal of the American Chemical Society 132 (2010) 12814–12816; doi:10.1021/ja104934n

data_4103056
_publ_section_title
;
 Synthesis and Characterization of an Iron(IV) Ketimide Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12814
_journal_page_last               12816
_journal_paper_doi               10.1021/ja104934n
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C40 H82 Fe Li N4 O2'
_chemical_formula_weight         713.89
_chemical_name_systematic
; 
 Lithium dimethoxyethane Iron(III) tetrakis(bistert-butyl ketimide) 
;
_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                87.016(3)
_cell_angle_beta                 81.074(3)
_cell_angle_gamma                69.225(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7816(17)
_cell_length_b                   11.8835(19)
_cell_length_c                   18.739(3)
_cell_measurement_reflns_used    154
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.275
_cell_measurement_theta_min      12.776
_cell_volume                     2217.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17931
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.562008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         8317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0467P)^2^+0.7723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                6106
_reflns_number_total             8317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104934n_si_002_2.cif
_cod_data_source_block           Complex_2
_cod_database_code               4103056