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_4307138
_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            'C61 H111 Fe8 N9 O27 S3'
_chemical_formula_weight         1945.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.000(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   55.495(2)
_cell_length_b                   15.4971(9)
_cell_length_c                   21.1361(9)
_cell_measurement_reflns_used    30393
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      1.57
_cell_volume                     16970.0(14)
_computing_cell_refinement       'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_data_collection       'WinXpose 1.05 (Stoe & Cie GmbH, 2000)'
_computing_data_reduction        'X-Area 1.09 (Stoe & Cie GmbH, 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      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       '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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56154
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.89
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 5.1 (Bruker AXS Inc., 1997)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8096
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         17443
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                11437
_reflns_number_total             17443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061650ssi20060831_091622_5.cif
_cod_data_source_block           189
_cod_original_cell_volume        16969.9(14)
_cod_database_code               4307138