Iron(II) Cage Complexes of N-Heterocyclic Amide and Bis(trimethylsilyl)amide Ligands: Synthesis, Structure, and Magnetic Properties
Scott A. Sulway; David Collison; Joseph J. W. McDouall; Floriana Tuna; Richard A. Layfield; Inorganic Chemistry 50 (2011) 2521–2526; doi:10.1021/ic102341a

data_4324664
_publ_section_title
;
 Iron(II) Cage Complexes of N-Heterocyclic Amide and
 Bis(trimethylsilyl)amide Ligands: Synthesis, Structure, and Magnetic
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2521
_journal_page_last               2526
_journal_paper_doi               10.1021/ic102341a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'Fe2 Li2 Si8 N10 C36 H80'
_chemical_formula_sum            'C18 H40 Fe Li N5 Si4'
_chemical_formula_weight         501.6795
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.276(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0458(7)
_cell_length_b                   8.5059(3)
_cell_length_c                   18.7423(7)
_cell_measurement_reflns_used    4446
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4491
_cell_measurement_theta_min      2.7838
_cell_volume                     2821.33(19)
_computing_cell_refinement       'SHELXS-97 (Sheldrick, 1990)'
_computing_data_collection       'SHELXS-97 (Sheldrick, 1990)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire2 (large Be window)'
_diffrn_measurement_method
'Goniometer KM4/Xcalibur, detector: Sapphire2 (large Be window)'
_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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.1067
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10747
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         2.79
_diffrn_standards_number         11222
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1072.0
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         7065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.836
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                3850
_reflns_number_total             7065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102341a_si_002_2.cif
_cod_data_source_block           oral65
_cod_original_cell_volume        2821.34(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C18 H40 Fe1 Li1 N5 Si4'
_cod_database_code               4324664