Experimental and Theoretical Electron Density Distribution and Magnetic Properties of the Butterfly-like Complex [Fe4O2(O2CCMe3)8(NC5H4Me)2].2CH3CN
Jacob Overgaard; David E. Hibbs; Eva Rentschler; Grigore A. Timco; Finn K. Larsen; Inorganic Chemistry 42 (2003) 7593–7601; doi:10.1021/ic034062c

data_4312473
_publ_contact_author
; 
Finn Krebs Larsen
Department of Chemistry 
University of Aarhus
Langelandsgade 140 
DK-8000 Aarhus C
Denmark
;
_publ_contact_author_email       kre@chem.au.dk
_publ_contact_author_fax         '+45 8619 6199'
_publ_contact_author_phone       '+45 8942 3897'
_publ_section_title
;
 Experimental and Theoretical Electron Density Distribution and Magnetic
 Properties of the Butterfly-like Complex
 [Fe4O2(O2CCMe3)8(NC5H4Me)2].2CH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7593
_journal_page_last               7601
_journal_paper_doi               10.1021/ic034062c
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C56 H92 Fe4 N4 O18'
_chemical_formula_weight         1332.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                115.372(2)
_cell_angle_beta                 107.702(3)
_cell_angle_gamma                102.731(2)
_cell_formula_units_Z            1
_cell_length_a                   12.6926(7)
_cell_length_b                   12.9134(8)
_cell_length_c                   13.4732(8)
_cell_measurement_reflns_used    3775
_cell_measurement_temperature    16(5)
_cell_measurement_theta_max      39.856
_cell_measurement_theta_min      2.868
_cell_volume                     1735.95(19)
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT+ V5.01 (Bruker, 1998)'
_computing_molecular_graphics    'XD (Koritsanszky et al, 1995)'
_computing_publication_material  'XD (Koritsanszky et al, 1995)'
_computing_structure_refinement  'XD (Koritsanszky et al, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      16(5)
_diffrn_measured_fraction_theta_full 0.719
_diffrn_measured_fraction_theta_max 0.719
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       \phi-scans
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.643
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55130
_diffrn_reflns_theta_full        40.06
_diffrn_reflns_theta_max         40.06
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.89
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS, Sheldrick 1996)'
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.10
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         20963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.10
_refine_ls_R_factor_all          0.025
_refine_ls_R_factor_gt           0.024
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.029
_refine_ls_wR_factor_ref         0.029
_reflns_number_gt                17007
_reflns_number_total             20960
_reflns_threshold_expression     >1.5sigma(I)
_cod_data_source_file            ic034062csi20030120_075128.cif
_cod_data_source_block           butterfly
_cod_original_cell_volume        1735.95(18)
_cod_database_code               4312473