Low-Coordinate Iron(II) Amido Complexes of β-Diketiminates: Synthesis, Structure, and Reactivity
Nathan A. Eckert; Jeremy M. Smith; Rene J. Lachicotte; Patrick L. Holland; Inorganic Chemistry 43 (2004) 3306–3321; doi:10.1021/ic035483x

data_4311028
_publ_section_title
;
 Low-Coordinate Iron(II) Amido Complexes of \b-Diketiminates: Synthesis,
 Structure, and Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3306
_journal_page_last               3321
_journal_paper_doi               10.1021/ic035483x
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C33 H50 Fe N2 O'
_chemical_formula_weight         546.60
_chemical_name_common            holne56
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0746(14)
_cell_length_b                   8.7561(7)
_cell_length_c                   21.0325(16)
_cell_measurement_reflns_used    6943
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3328.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28447
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8069
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          1.600
_refine_ls_shift/su_mean         0.255
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.5653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                5769
_reflns_number_total             8069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035483xsi20031224_095602_10.cif
_cod_data_source_block           L(Me)FeOtBu
_cod_database_code               4311028