#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/31/4303165.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4303165
loop_
_publ_author_name
'Yukinari Sunatsuki'
'Ryohei Kawamoto'
'Kunihiro Fujita'
'Hisashi Maruyama'
'Takayoshi Suzuki'
'Hiroyuki Ishida'
'Masaaki Kojima'
'Seiichiro Iijima'
'Naohide Matsumoto'
_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         'C30 H36 Cl4 Fe2 N18 O16 '
_chemical_formula_sum            'C30 H36 Cl4 Fe2 N18 O16'
_chemical_formula_weight         1158.23
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            2
_cell_length_a                   10.031(2)
_cell_length_b                   10.031(2)
_cell_length_c                   24.859(6)
_cell_measurement_reflns_used    15265
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     2166.2(8)
_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       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19650
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1180.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1661
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0625P)²+2.1115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                1397
_reflns_number_total             1661
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic900977m_si_002_6.cif
_cod_data_source_block           '_2Me.ClO4'
_cod_original_cell_volume        2166.2(9)
_cod_original_formula_sum        'C30 H36 Cl4 Fe2 N18 O16 '
_cod_database_code               4303165
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -Y,+X-Y,+Z
3 -X+Y,-X,+Z
4 -X+Y,+Y,1/2+Z
5 +X,+X-Y,1/2+Z
6 -Y,-X,1/2+Z
7 -X,-Y,-Z
8 +Y,-X+Y,-Z
9 +X-Y,+X,-Z
10 +X-Y,-Y,1/2-Z
11 -X,-X+Y,1/2-Z
12 +Y,+X,1/2-Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe(1) Fe 0.0000 1.0000 0.17992(2) 0.02003(17) Uani 1.00 3 d S . .
Cl(1) Cl 0.3333 0.6667 -0.00751(4) 0.0344(2) Uani 1.00 3 d S . .
Cl(2) Cl 0.3333 0.6667 0.19277(5) 0.0371(2) Uani 1.00 3 d S . .
O(1) O 0.3669(3) 0.8159(3) -0.02100(16) 0.0966(11) Uani 1.00 1 d . . .
O(2) O 0.3333 0.6667 0.0496(2) 0.117(2) Uani 1.00 3 d S . .
O(3) O 0.2079(2) 0.6859(3) 0.17459(9) 0.0585(6) Uani 1.00 1 d . . .
O(4) O 0.3333 0.6667 0.25134(14) 0.0466(9) Uani 1.00 3 d S . .
N(1) N 0.3497(2) 0.9850(2) 0.09443(9) 0.0406(5) Uani 1.00 1 d . . .
N(2) N 0.1710(2) 0.9984(2) 0.13996(7) 0.0247(4) Uani 1.00 1 d . . .
N(3) N 0.1727(2) 1.1388(2) 0.22435(7) 0.0232(3) Uani 1.00 1 d . . .
C(1) C 0.0815(3) 0.8136(3) 0.06262(11) 0.0441(6) Uani 1.00 1 d . . .
C(2) C 0.1966(2) 0.9308(2) 0.09868(9) 0.0303(5) Uani 1.00 1 d . . .
C(3) C 0.4246(3) 1.0866(3) 0.13454(11) 0.0418(6) Uani 1.00 1 d . . .
C(4) C 0.3141(2) 1.0963(3) 0.16271(9) 0.0306(5) Uani 1.00 1 d . . .
C(5) C 0.3106(2) 1.1707(2) 0.21220(9) 0.0294(5) Uani 1.00 1 d . . .
H(1) H 0.1268 0.8232 0.0269 0.053 Uiso 1.00 1 c R . .
H(2) H -0.0077 0.8285 0.0598 0.053 Uiso 1.00 1 c R . .
H(3) H 0.0486 0.7109 0.0771 0.053 Uiso 1.00 1 c R . .
H(4) H 0.3939 0.9583 0.0694 0.049 Uiso 1.00 1 c R . .
H(5) H 0.5322 1.1400 0.1415 0.050 Uiso 1.00 1 c R . .
H(6) H 0.3991 1.2350 0.2332 0.035 Uiso 1.00 1 c R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.346 0.844
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.148 0.159
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
N(2) Fe(1) N(2) 97.23(9) yes . . 2_675
N(2) Fe(1) N(2) 97.23(8) yes . . 3_465
N(2) Fe(1) N(3) 79.94(8) yes . . .
N(2) Fe(1) N(3) 170.11(6) yes . . 2_675
N(2) Fe(1) N(3) 92.54(9) yes . . 3_465
N(2) Fe(1) N(2) 97.23(8) yes 2_675 . 3_465
N(2) Fe(1) N(3) 92.54(8) yes 2_675 . .
N(2) Fe(1) N(3) 79.94(8) yes 2_675 . 2_675
N(2) Fe(1) N(3) 170.11(9) yes 2_675 . 3_465
N(2) Fe(1) N(3) 170.11(9) yes 3_465 . .
N(2) Fe(1) N(3) 92.54(8) yes 3_465 . 2_675
N(2) Fe(1) N(3) 79.94(7) yes 3_465 . 3_465
N(3) Fe(1) N(3) 90.67(8) yes . . 2_675
N(3) Fe(1) N(3) 90.67(7) yes . . 3_465
N(3) Fe(1) N(3) 90.67(9) yes 2_675 . 3_465
O(1) Cl(1) O(1) 114.5(2) yes . . 2_665
O(1) Cl(1) O(1) 114.45(19) yes . . 3_565
O(1) Cl(1) O(2) 103.85(16) yes . . .
O(1) Cl(1) O(1) 114.4(2) yes 2_665 . 3_565
O(1) Cl(1) O(2) 103.85(16) yes 2_665 . .
O(1) Cl(1) O(2) 103.85(16) yes 3_565 . .
O(3) Cl(2) O(3) 110.61(15) yes . . 2_665
O(3) Cl(2) O(3) 110.63(16) yes . . 3_565
O(3) Cl(2) O(4) 108.32(10) yes . . .
O(3) Cl(2) O(3) 110.57(16) yes 2_665 . 3_565
O(3) Cl(2) O(4) 108.31(10) yes 2_665 . .
O(3) Cl(2) O(4) 108.31(10) yes 3_565 . .
C(2) N(1) C(3) 109.7(2) yes . . .
Fe(1) N(2) C(2) 141.25(15) yes . . .
Fe(1) N(2) C(4) 112.40(16) yes . . .
C(2) N(2) C(4) 106.3(2) yes . . .
Fe(1) N(3) N(3) 117.00(13) yes . . 12_465
Fe(1) N(3) C(5) 120.52(16) yes . . .
N(3) N(3) C(5) 120.79(17) yes 12_465 . .
N(1) C(2) N(2) 109.06(19) yes . . .
N(1) C(2) C(1) 123.6(2) yes . . .
N(2) C(2) C(1) 127.3(2) yes . . .
N(1) C(3) C(4) 105.6(2) yes . . .
N(2) C(4) C(3) 109.4(2) yes . . .
N(2) C(4) C(5) 115.3(2) yes . . .
C(3) C(4) C(5) 135.0(2) yes . . .
N(3) C(5) C(4) 111.71(19) yes . . .
C(2) N(1) H(4) 125.2 no . . .
C(3) N(1) H(4) 125.2 no . . .
C(2) C(1) H(1) 109.5 no . . .
C(2) C(1) H(2) 109.5 no . . .
C(2) C(1) H(3) 109.5 no . . .
H(1) C(1) H(2) 109.5 no . . .
H(1) C(1) H(3) 109.5 no . . .
H(2) C(1) H(3) 109.5 no . . .
N(1) C(3) H(5) 127.2 no . . .
C(4) C(3) H(5) 127.2 no . . .
N(3) C(5) H(6) 124.1 no . . .
C(4) C(5) H(6) 124.1 no . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Fe(1) N(2) 1.989(2) yes . .
Fe(1) N(2) 1.989(2) yes . 2_675
Fe(1) N(2) 1.9890(16) yes . 3_465
Fe(1) N(3) 1.9358(16) yes . .
Fe(1) N(3) 1.936(2) yes . 2_675
Fe(1) N(3) 1.936(2) yes . 3_465
Cl(1) O(1) 1.400(3) yes . .
Cl(1) O(1) 1.401(2) yes . 2_665
Cl(1) O(1) 1.401(4) yes . 3_565
Cl(1) O(2) 1.420(5) yes . .
Cl(2) O(3) 1.438(3) yes . .
Cl(2) O(3) 1.439(3) yes . 2_665
Cl(2) O(3) 1.438(2) yes . 3_565
Cl(2) O(4) 1.456(3) yes . .
N(1) C(2) 1.353(3) yes . .
N(1) C(3) 1.353(3) yes . .
N(2) C(2) 1.324(3) yes . .
N(2) C(4) 1.391(2) yes . .
N(3) N(3) 1.405(2) yes . 12_465
N(3) C(5) 1.291(3) yes . .
C(1) C(2) 1.470(3) yes . .
C(3) C(4) 1.355(4) yes . .
C(4) C(5) 1.448(3) yes . .
N(1) H(4) 0.880 no . .
C(1) H(1) 0.980 no . .
C(1) H(2) 0.980 no . .
C(1) H(3) 0.980 no . .
C(3) H(5) 0.950 no . .
C(5) H(6) 0.950 no . .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
Fe(1) Fe(1) 3.4842(7) ? . 10_675
Fe(1) N(3) 2.862(2) ? . 10_675
Fe(1) N(3) 2.8619(19) ? . 11_555
Cl(2) O(2) 3.559(5) ? . .
O(1) O(1) 3.464(3) ? . 7_675
O(1) N(1) 3.382(4) ? . .
O(1) N(1) 3.118(3) ? . 7_675
O(1) C(1) 3.529(5) ? . .
O(1) C(1) 3.435(5) ? . 9_665
O(1) C(3) 3.354(4) ? . 7_675
O(2) Cl(2) 3.559(5) ? . .
O(2) O(3) 3.394(5) ? . .
O(2) O(3) 3.394(5) ? . 2_665
O(2) O(3) 3.394(5) ? . 3_565
O(2) N(1) 3.308(3) ? . .
O(2) N(1) 3.308(2) ? . 2_665
O(2) N(1) 3.309(3) ? . 3_565
O(2) C(1) 3.518(4) ? . .
O(2) C(1) 3.519(3) ? . 2_665
O(2) C(1) 3.519(2) ? . 3_565
O(3) O(2) 3.394(5) ? . .
O(3) N(1) 3.276(3) ? . .
O(3) N(1) 3.444(3) ? . 2_665
O(3) N(2) 3.445(4) ? . .
O(3) N(3) 3.587(4) ? . 3_465
O(3) C(1) 3.552(4) ? . .
O(3) C(2) 3.144(4) ? . .
O(3) C(3) 3.404(3) ? . 2_665
O(3) C(5) 3.381(3) ? . 10_675
O(4) C(5) 3.226(3) ? . 10_675
O(4) C(5) 3.227(2) ? . 11_655
O(4) C(5) 3.227(2) ? . 12_455
N(1) O(1) 3.382(4) ? . .
N(1) O(1) 3.118(3) ? . 7_675
N(1) O(2) 3.308(3) ? . .
N(1) O(3) 3.276(3) ? . .
N(1) O(3) 3.444(4) ? . 3_565
N(2) O(3) 3.445(4) ? . .
N(3) Fe(1) 2.8619(17) ? . 10_675
N(3) O(3) 3.587(3) ? . 2_675
N(3) N(3) 2.728(2) ? . 10_675
N(3) N(3) 3.260(2) ? . 11_555
N(3) C(5) 3.348(3) ? . 10_675
C(1) O(1) 3.529(5) ? . .
C(1) O(1) 3.435(3) ? . 8_455
C(1) O(2) 3.518(4) ? . .
C(1) O(3) 3.552(4) ? . .
C(2) O(3) 3.144(4) ? . .
C(3) O(1) 3.354(4) ? . 7_675
C(3) O(3) 3.404(5) ? . 3_565
C(5) O(3) 3.381(3) ? . 10_675
C(5) O(4) 3.226(2) ? . 10_675
C(5) N(3) 3.348(2) ? . 10_675
C(5) C(5) 3.511(3) ? . 10_675
Cl(1) H(1) 3.277 ? . .
Cl(1) H(1) 3.278 ? . 2_665
Cl(1) H(1) 3.278 ? . 3_565
Cl(1) H(4) 3.287 ? . .
Cl(1) H(4) 3.287 ? . 2_665
Cl(1) H(4) 3.288 ? . 3_565
Cl(2) H(6) 2.986 ? . 10_675
Cl(2) H(6) 2.987 ? . 11_655
Cl(2) H(6) 2.987 ? . 12_455
O(1) H(1) 2.721 ? . .
O(1) H(1) 3.283 ? . 3_565
O(1) H(1) 3.483 ? . 9_665
O(1) H(2) 3.437 ? . 9_665
O(1) H(3) 3.543 ? . 3_565
O(1) H(3) 2.857 ? . 9_665
O(1) H(4) 2.603 ? . .
O(1) H(4) 2.627 ? . 7_675
O(1) H(5) 3.122 ? . 7_675
O(2) H(1) 3.214 ? . .
O(2) H(1) 3.215 ? . 2_665
O(2) H(1) 3.214 ? . 3_565
O(2) H(3) 3.176 ? . .
O(2) H(3) 3.177 ? . 2_665
O(2) H(3) 3.177 ? . 3_565
O(2) H(4) 2.718 ? . .
O(2) H(4) 2.719 ? . 2_665
O(2) H(4) 2.719 ? . 3_565
O(3) H(3) 2.981 ? . .
O(3) H(4) 3.562 ? . .
O(3) H(4) 3.426 ? . 2_665
O(3) H(5) 3.355 ? . 2_665
O(3) H(6) 2.536 ? . 10_675
O(4) H(5) 3.172 ? . 10_675
O(4) H(5) 3.172 ? . 11_655
O(4) H(5) 3.172 ? . 12_455
O(4) H(6) 2.382 ? . 10_675
O(4) H(6) 2.383 ? . 11_655
O(4) H(6) 2.383 ? . 12_455
N(1) H(1) 3.463 ? . 9_665
N(1) H(3) 3.345 ? . 3_565
C(1) H(1) 3.162 ? . 8_455
C(1) H(1) 3.576 ? . 9_665
C(1) H(2) 3.417 ? . 9_665
C(2) H(1) 3.557 ? . 9_665
C(3) H(3) 3.577 ? . 3_565
C(3) H(5) 3.317 ? . 3_575
C(4) H(5) 3.445 ? . 3_575
C(5) H(5) 3.461 ? . 3_575
H(1) Cl(1) 3.277 ? . .
H(1) O(1) 2.721 ? . .
H(1) O(1) 3.283 ? . 2_665
H(1) O(1) 3.483 ? . 8_455
H(1) O(2) 3.214 ? . .
H(1) N(1) 3.463 ? . 8_455
H(1) C(1) 3.576 ? . 8_455
H(1) C(1) 3.162 ? . 9_665
H(1) C(2) 3.557 ? . 8_455
H(1) H(1) 2.967 ? . 8_455
H(1) H(1) 2.967 ? . 9_665
H(1) H(2) 2.651 ? . 9_665
H(1) H(3) 3.390 ? . 9_665
H(1) H(4) 3.308 ? . 8_455
H(2) O(1) 3.437 ? . 8_455
H(2) C(1) 3.417 ? . 8_455
H(2) H(1) 2.651 ? . 8_455
H(2) H(2) 3.416 ? . 8_455
H(2) H(2) 3.416 ? . 9_665
H(3) O(1) 3.543 ? . 2_665
H(3) O(1) 2.857 ? . 8_455
H(3) O(2) 3.176 ? . .
H(3) O(3) 2.981 ? . .
H(3) N(1) 3.345 ? . 2_665
H(3) C(3) 3.577 ? . 2_665
H(3) H(1) 3.390 ? . 8_455
H(3) H(4) 2.734 ? . 2_665
H(3) H(5) 3.211 ? . 2_665
H(4) Cl(1) 3.287 ? . .
H(4) O(1) 2.603 ? . .
H(4) O(1) 2.627 ? . 7_675
H(4) O(2) 2.718 ? . .
H(4) O(3) 3.562 ? . .
H(4) O(3) 3.426 ? . 3_565
H(4) H(1) 3.308 ? . 9_665
H(4) H(3) 2.734 ? . 3_565
H(5) O(1) 3.122 ? . 7_675
H(5) O(3) 3.355 ? . 3_565
H(5) O(4) 3.172 ? . 10_675
H(5) C(3) 3.317 ? . 2_775
H(5) C(4) 3.445 ? . 2_775
H(5) C(5) 3.461 ? . 2_775
H(5) H(3) 3.211 ? . 3_565
H(5) H(5) 2.982 ? . 2_775
H(5) H(5) 2.982 ? . 3_575
H(5) H(6) 3.185 ? . 2_775
H(6) Cl(2) 2.986 ? . 10_675
H(6) O(3) 2.536 ? . 10_675
H(6) O(4) 2.382 ? . 10_675
H(6) H(5) 3.185 ? . 3_575
