Odd-Numbered FeIII Complexes: Synthesis, Molecular Structure, Reactivity, and Magnetic Properties
Ayuk M. Ako; Oliver Waldmann; Valeriu Mereacre; Frederik Klöwer; Ian J. Hewitt; Christopher E. Anson; Hans U. Güdel; Annie K. Powell; Inorganic Chemistry 46 (2007) 756–766; doi:10.1021/ic061650s

data_4307134
_publ_contact_author
; 
'Annie K. Powell'
;
_publ_contact_author_email       powell@aoc.uni-karlsruhe.de
_publ_contact_author_phone       '+44 721 608 2135'
_publ_section_title
;
Odd-Numbered FeIII Complexes: Synthesis, Molecular Structure, Reactivity,
and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              756
_journal_page_last               766
_journal_paper_doi               10.1021/ic061650s
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C63 H126 Fe7 N3 O33'
_chemical_formula_weight         1844.62
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.5804(8)
_cell_length_b                   15.5804(8)
_cell_length_c                   20.8694(11)
_cell_measurement_reflns_used    11090
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.47
_cell_volume                     4387.3(4)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_computing_data_reduction        'SAINT+ 6.0 (Bruker AXS Inc., 2000)'
_computing_molecular_graphics    'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_publication_material  'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_refinement  'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_solution    'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16786
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1942
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5060
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                4823
_reflns_number_total             5060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061650ssi20060831_091622_1.cif
_cod_data_source_block           ako224
_cod_database_code               4307134