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_4307135
_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            'C69.5 H138 Cl Fe7 N3 O30'
_chemical_formula_weight         1922.23
_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                 115.078(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   63.351(3)
_cell_length_b                   10.4329(5)
_cell_length_c                   31.4090(16)
_cell_measurement_reflns_used    15332
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.23
_cell_volume                     18802.4(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.938
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -83
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46786
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8120
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1044
_refine_ls_number_reflns         21285
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                14323
_reflns_number_total             21285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061650ssi20060831_091622_2.cif
_cod_data_source_block           188cx
_cod_original_cell_volume        18802.3(16)
_cod_database_code               4307135