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_4303163
_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         '5(C20 H24 Fe N12), 8(C2 H3 N), 10(Cl O4) '
_chemical_formula_sum            'C116 H144 Cl10 Fe5 N68 O40'
_chemical_formula_weight         3764.61
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   22.8537(12)
_cell_length_b                   22.8537(11)
_cell_length_c                   31.4028(15)
_cell_measurement_reflns_used    92429
_cell_measurement_temperature    200.1
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.1
_cell_volume                     16401.4(14)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.063
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            144564
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.780
_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    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7744.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     594
_refine_ls_number_reflns         9404
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1031P)^2^+49.3829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2060
_reflns_number_gt                7333
_reflns_number_total             9404
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic900977m_si_002_4.cif
_cod_data_source_block           '_1Me.ClO4'
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C116 H144 Cl10 Fe5 N68 O40 '
_cod_database_code               4303163