Structures and Spin States of Bis(tridentate)-Type Mononuclear and Triple Helicate Dinuclear Iron(II) Complexes of Imidazole-4-carbaldehyde azine
Yukinari Sunatsuki; Ryohei Kawamoto; Kunihiro Fujita; Hisashi Maruyama; Takayoshi Suzuki; Hiroyuki Ishida; Masaaki Kojima; Seiichiro Iijima; Naohide Matsumoto; Inorganic Chemistry 48 (2009) 8784–8795; doi:10.1021/ic900977m

data_4303160
_publ_contact_author_address
;
  Department of Chemistry, Faculty of Science,
  Okayama University, 
  3-1-1 Tsushima-naka, 
  Okayama 700-8530, 
  Japan.
;
_publ_contact_author_email       kojima@cc.okayama-u.ac.jp
_publ_contact_author_fax         +81-86-251-7842
_publ_contact_author_name        'Masaaki Kojima'
_publ_contact_author_phone       +81-86-251-7842
_publ_section_title
;
Structures and Spin States of Bis(tridentate)-Type Mononuclear and Triple
Helicate Dinuclear Iron(II) Complexes of Imidazole-4-carbaldehyde azine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8784
_journal_page_last               8795
_journal_paper_doi               10.1021/ic900977m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '2(C24 H24 Fe2 N18), 13(C H3 N O2), H2 O '
_chemical_formula_sum            'C61 H89 B8 F32 Fe4 N49 O27'
_chemical_formula_weight         2858.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                90.2947(18)
_cell_angle_beta                 90.2919(18)
_cell_angle_gamma                108.5083(18)
_cell_formula_units_Z            1
_cell_length_a                   11.5903(7)
_cell_length_b                   15.5367(10)
_cell_length_c                   17.4994(10)
_cell_measurement_reflns_used    18618
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.0
_cell_volume                     2988.1(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29514
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1446.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.27
_refine_diff_density_min         -0.91
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     979
_refine_ls_number_reflns         13599
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.0040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1302P)^2^+3.3210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2158
_reflns_number_gt                10286
_reflns_number_total             13599
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic900977m_si_002_1.cif
_cod_data_source_block           '_2H.BF4'
_cod_original_formula_sum        'C61 H89 B8 F32 Fe4 N49 O27 '
_cod_database_code               4303160