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_4324663
_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         'C40 H84 Fe3 N14 Si4, C7 H8'
_chemical_formula_sum            'C47 H92 Fe3 N14 Si4'
_chemical_formula_weight         1133.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                   22.522(4)
_cell_length_b                   14.455(3)
_cell_length_c                   17.979(3)
_cell_measurement_temperature    100
_cell_volume                     5853.2(19)
_computing_cell_refinement       'SHELXL-97 (Sheldrick, 1997)'
_computing_data_collection       'SHELXL-97 (Sheldrick, 1997)'
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       Synchrotron
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26727
_diffrn_reflns_theta_full        89.23
_diffrn_reflns_theta_max         89.23
_diffrn_reflns_theta_min         4.39
_exptl_absorpt_coefficient_mu    5.230
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       Needles
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+9.7840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                6040
_reflns_number_total             6621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102341a_si_002_1.cif
_cod_data_source_block           pccn
_cod_database_code               4324663