#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322680.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_4322680
loop_
_publ_author_name
'Nobuo Fukita'
'Masaaki Ohba'
'Hisashi Ōkawa'
'Kenji Matsuda'
'Hiizu Iwamura'
_publ_section_title
;
 Bimetallic Assemblies [Ni(L)2]3[Fe(CN)6]X2 (L = Ethylenediamine,
 Trimethylenediamine; X = PF6-, ClO4-) with a Three-Dimensional Network
 Extended through FeII-CN-NiII Linkages
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              842
_journal_page_last               848
_journal_paper_doi               10.1021/ic9711168
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C24 H60 Cl2 Fe N18 Ni3 O8'
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_date             'Thu Apr 17 11:12:07 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3.00
_cell_length_a                   14.337(2)
_cell_length_b                   14.3372
_cell_length_c                   17.294(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      29.14
_cell_volume                     3078.6(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_computing_structure_solution    SAPI91
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.04550
_diffrn_orient_matrix_UB_12      -0.08030
_diffrn_orient_matrix_UB_13      0.00027
_diffrn_orient_matrix_UB_21      -0.06603
_diffrn_orient_matrix_UB_22      0.00618
_diffrn_orient_matrix_UB_23      0.00636
_diffrn_orient_matrix_UB_31      -0.00752
_diffrn_orient_matrix_UB_32      0.00031
_diffrn_orient_matrix_UB_33      -0.05747
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.75
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1314
_diffrn_reflns_theta_max         24.9662
_diffrn_standards_decay_%        -0.21
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 18.982
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1614.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         -0.38210
_refine_diff_density_min         0.27120
_refine_ls_extinction_coef       0.57178
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   3.590
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1073
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0240
_refine_ls_shift/esd_max         0.1800
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0220
_cod_data_source_file            ic9711168_3.cif
_cod_data_source_block           '[Ni(tn)2]3[Fe(CN)6](ClO4)2'
_cod_original_cell_volume        3078(1)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C24 H60 N18 O8 Cl2 Ni3 Fe'
_cod_database_code               4322680
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
2/3+x,1/3+y,1/3+z
1/3+x,2/3+y,2/3+z
'   -y,   +x-y,   +z'
2/3-y,1/3+x-y,1/3+z
1/3-y,2/3+x-y,2/3+z
'   -x+y,   -x,   +z'
2/3-x+y,1/3-x,1/3+z
1/3-x+y,2/3-x,2/3+z
'   -x,   -y,   -z'
2/3-x,1/3-y,1/3-z
1/3-x,2/3-y,2/3-z
'   +y,   -x+y,   -z'
2/3+y,1/3-x+y,1/3-z
1/3+y,2/3-x+y,2/3-z
'   +x-y,   +x,   -z'
2/3+x-y,1/3+x,1/3-z
1/3+x-y,2/3+x,2/3-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Ni 0.5000 -0.5000 -0.5000 0.0244 Uij ? ?
Fe 0.6666 -0.6667 -0.6667 0.0166 Uij ? ?
Cl 1.0000 0.0000 -0.65428(10) 0.0553 Uij ? ?
O1 1.0000 0.0000 -0.5751(6) 0.1708 Uij ? ?
O2 0.9048(6) -0.0176(7) -0.6262(6) 0.1746 Uij ? ?
O3 1.0000 0.0000 -0.732(1) 0.3351 Uij ? ?
O4 1.0732(5) -0.0295(5) -0.6837(4) 0.0850 Uij ? ?
N1 0.5195(2) -0.6193(2) -0.5633(1) 0.0309 Uij ? ?
N2 0.5431(2) -0.4122(2) -0.6045(1) 0.0377 Uij ? ?
N3 0.6649(2) -0.4284(2) -0.4721(2) 0.0381 Uij ? ?
C1 0.5722(2) -0.6407(2) -0.6021(1) 0.0210 Uij ? ?
C2 0.6302(3) -0.2999(2) -0.6028(2) 0.0474 Uij ? ?
C3 0.7332(2) -0.3126(2) -0.4882(2) 0.0474 Uij ? ?
C4 0.7342(3) -0.2885(3) -0.5730(2) 0.0561 Uij ? ?
H1 0.563(3) -0.447(3) -0.637(2) 0.07(1) Uij ? ?
H2 0.487(2) -0.413(2) -0.626(2) 0.05(1) Uij ? ?
H3 0.637(2) -0.267(2) -0.657(2) 0.066(9) Uij ? ?
H4 0.602(2) -0.264(2) -0.570(2) 0.057(9) Uij ? ?
H5 0.791(3) -0.219(3) -0.584(2) 0.08(1) Uij ? ?
H6 0.753(2) -0.335(2) -0.604(2) 0.056(9) Uij ? ?
H7 0.804(2) -0.286(2) -0.467(2) 0.054(9) Uij ? ?
H8 0.704(2) -0.272(2) -0.455(1) 0.047(8) Uij ? ?
H9 0.672(2) -0.443(2) -0.425(2) 0.050(10) Uij ? ?
H10 0.691(2) -0.463(2) -0.498(2) 0.053(10) Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 72 0.003 0.002 'International Tables'
H 0 180 0.000 0.000 'International Tables'
N 0 54 0.006 0.003 'International Tables'
O 0 24 0.011 0.006 'International Tables'
Cl 0 6 0.148 0.159 'International Tables'
Ni 0 9 0.339 1.112 'International Tables'
Fe 0 3 0.346 0.844 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N(1) Ni N(1) 180.0000 ? ? ? yes
N(1) Ni N(2) 85.59(9) ? ? ? yes
N(1) Ni N(2) 94.41(9) ? ? ? yes
N(1) Ni N(3) 86.79(9) ? ? ? yes
N(1) Ni N(3) 93.21(9) ? ? ? yes
N(1) Ni N(2) 94.41(9) ? ? ? yes
N(1) Ni N(2) 85.59(9) ? ? ? yes
N(1) Ni N(3) 93.21(9) ? ? ? yes
N(1) Ni N(3) 86.79(9) ? ? ? yes
N(2) Ni N(2) 180.0000 ? ? ? yes
N(2) Ni N(3) 89.0(1) ? ? ? yes
N(2) Ni N(3) 91.0(1) ? ? ? yes
N(2) Ni N(3) 91.0(1) ? ? ? yes
N(2) Ni N(3) 89.0(1) ? ? ? yes
N(3) Ni N(3) 180.0000 ? ? ? yes
C(1) Fe C(1) 90.11(9) ? ? ? yes
C(1) Fe C(1) 89.88(9) ? ? ? yes
C(1) Fe C(1) 179.9653 ? ? ? yes
C(1) Fe C(1) 90.10(9) ? ? ? yes
C(1) Fe C(1) 89.86(9) ? ? ? yes
C(1) Fe C(1) 90.13(9) ? ? ? yes
C(1) Fe C(1) 89.92(9) ? ? ? yes
C(1) Fe C(1) 89.91(9) ? ? ? yes
C(1) Fe C(1) 179.9761 ? ? ? yes
C(1) Fe C(1) 90.12(9) ? ? ? yes
C(1) Fe C(1) 179.9579(1) ? ? ? yes
C(1) Fe C(1) 89.87(9) ? ? ? yes
C(1) Fe C(1) 89.90(9) ? ? ? yes
C(1) Fe C(1) 90.10(9) ? ? ? yes
C(1) Fe C(1) 90.09(9) ? ? ? yes
O(1) Cl O(2) 68.9(5) ? ? ? yes
O(1) Cl O(2) 68.9(5) ? ? ? yes
O(1) Cl O(2) 68.9(5) ? ? ? yes
O(1) Cl O(3) 180.0000 ? ? ? yes
O(1) Cl O(4) 111.2(3) ? ? ? yes
O(1) Cl O(4) 111.2(3) ? ? ? yes
O(1) Cl O(4) 111.2(3) ? ? ? yes
O(2) Cl O(2) 107.8(5) ? ? ? yes
O(2) Cl O(2) 107.8(5) ? ? ? yes
O(2) Cl O(3) 111.1(5) ? ? ? yes
O(2) Cl O(4) 155.6(4) ? ? ? yes
O(2) Cl O(4) 94.1(5) ? ? ? yes
O(2) Cl O(4) 53.7(4) ? ? ? yes
O(2) Cl O(2) 107.8(5) ? ? ? yes
O(2) Cl O(3) 111.1(5) ? ? ? yes
O(2) Cl O(4) 53.7(4) ? ? ? yes
O(2) Cl O(4) 155.6(4) ? ? ? yes
O(2) Cl O(4) 94.1(5) ? ? ? yes
O(2) Cl O(3) 111.1(5) ? ? ? yes
O(2) Cl O(4) 94.1(5) ? ? ? yes
O(2) Cl O(4) 53.7(4) ? ? ? yes
O(2) Cl O(4) 155.6(4) ? ? ? yes
O(3) Cl O(4) 68.8(3) ? ? ? yes
O(3) Cl O(4) 68.8(3) ? ? ? yes
O(3) Cl O(4) 68.8(3) ? ? ? yes
O(4) Cl O(4) 107.7(3) ? ? ? yes
O(4) Cl O(4) 107.7(3) ? ? ? yes
O(4) Cl O(4) 107.7(3) ? ? ? yes
Cl O(1) O(2) 54.9(5) ? ? ? yes
Cl O(1) O(2) 54.9(5) ? ? ? yes
Cl O(1) O(2) 54.9(5) ? ? ? yes
O(2) O(1) O(2) 90.2(7) ? ? ? yes
O(2) O(1) O(2) 90.2(7) ? ? ? yes
O(2) O(1) O(2) 90.2(7) ? ? ? yes
Cl O(2) O(1) 56.2(5) ? ? ? yes
Cl O(2) O(4) 65.6(5) ? ? ? yes
O(1) O(2) O(4) 110.4(7) ? ? ? yes
Cl O(3) O(4) 57.3(6) ? ? ? yes
Cl O(3) O(4) 57.3(6) ? ? ? yes
Cl O(3) O(4) 57.3(6) ? ? ? yes
O(4) O(3) O(4) 93.6(8) ? ? ? yes
O(4) O(3) O(4) 93.6(8) ? ? ? yes
O(4) O(3) O(4) 93.6(8) ? ? ? yes
Cl O(4) O(2) 60.7(4) ? ? ? yes
Cl O(4) O(3) 53.8(6) ? ? ? yes
O(2) O(4) O(3) 104.5(8) ? ? ? yes
Ni N(1) C(1) 149.3(2) ? ? ? yes
Ni N(2) C(2) 118.3(2) ? ? ? yes
Ni N(2) H(1) 106(2) ? ? ? no
Ni N(2) H(2) 111(1) ? ? ? no
C(2) N(2) H(1) 107(2) ? ? ? no
C(2) N(2) H(2) 107(1) ? ? ? no
H(1) N(2) H(2) 105(2) ? ? ? no
Ni N(3) C(3) 117.2(2) ? ? ? yes
Ni N(3) H(9) 110(1) ? ? ? no
Ni N(3) H(10) 107(1) ? ? ? no
C(3) N(3) H(9) 110(1) ? ? ? no
C(3) N(3) H(10) 107(1) ? ? ? no
H(9) N(3) H(10) 102(2) ? ? ? no
Fe C(1) Fe 0.0206 ? ? ? yes
Fe C(1) Fe 0.0347 ? ? ? yes
Fe C(1) Fe 0.0215 ? ? ? yes
Fe C(1) Fe 0.0179 ? ? ? yes
Fe C(1) N(1) 176.4(2) ? ? ? yes
Fe C(1) Fe 0.0215 ? ? ? yes
Fe C(1) Fe 0.0239 ? ? ? yes
Fe C(1) Fe 0.0128 ? ? ? yes
Fe C(1) N(1) 176.4(2) ? ? ? yes
Fe C(1) Fe 0.0206 ? ? ? yes
Fe C(1) Fe 0.0342 ? ? ? yes
Fe C(1) N(1) 176.4(2) ? ? ? yes
Fe C(1) Fe 0.0318 ? ? ? yes
Fe C(1) N(1) 176.4(2) ? ? ? yes
Fe C(1) N(1) 176.4(2) ? ? ? yes
N(2) C(2) C(4) 112.3(3) ? ? ? yes
N(2) C(2) H(3) 108(1) ? ? ? no
N(2) C(2) H(4) 103(1) ? ? ? no
C(4) C(2) H(3) 113(1) ? ? ? no
C(4) C(2) H(4) 112(1) ? ? ? no
H(3) C(2) H(4) 105(2) ? ? ? no
N(3) C(3) C(4) 111.5(3) ? ? ? yes
N(3) C(3) H(7) 110(1) ? ? ? no
N(3) C(3) H(8) 107(1) ? ? ? no
C(4) C(3) H(7) 113(1) ? ? ? no
C(4) C(3) H(8) 111(1) ? ? ? no
H(7) C(3) H(8) 101(2) ? ? ? no
C(2) C(4) C(3) 114.4(3) ? ? ? yes
C(2) C(4) H(5) 109(1) ? ? ? no
C(2) C(4) H(6) 108(1) ? ? ? no
C(3) C(4) H(5) 110(1) ? ? ? no
C(3) C(4) H(6) 110(1) ? ? ? no
H(5) C(4) H(6) 102(2) ? ? ? no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N(1) 2.164(2) ? ? yes
Ni N(1) 2.164(2) ? ? yes
Ni N(2) 2.110(2) ? ? yes
Ni N(2) 2.110(2) ? ? yes
Ni N(3) 2.109(2) ? ? yes
Ni N(3) 2.109(2) ? ? yes
Fe C(1) 1.930(2) ? ? yes
Fe C(1) 1.929(2) ? ? yes
Fe C(1) 1.930(2) ? ? yes
Fe C(1) 1.929(2) ? ? yes
Fe C(1) 1.929(2) ? ? yes
Fe C(1) 1.930(2) ? ? yes
Cl O(1) 1.37(1) ? ? yes
Cl O(2) 1.349(7) ? ? yes
Cl O(2) 1.349(7) ? ? yes
Cl O(2) 1.349(7) ? ? yes
Cl O(3) 1.35(2) ? ? yes
Cl O(4) 1.408(5) ? ? yes
Cl O(4) 1.408(5) ? ? yes
Cl O(4) 1.408(5) ? ? yes
O(1) O(2) 1.538(10) ? ? yes
O(1) O(2) 1.538(10) ? ? yes
O(1) O(2) 1.538(10) ? ? yes
O(2) O(4) 1.25(1) ? ? yes
O(3) O(4) 1.56(1) ? ? yes
O(3) O(4) 1.56(1) ? ? yes
O(3) O(4) 1.56(1) ? ? yes
N(1) C(1) 1.160(3) ? ? yes
N(2) C(2) 1.463(4) ? ? yes
N(2) H(1) 0.88(3) ? ? no
N(2) H(2) 0.88(3) ? ? no
N(3) C(3) 1.473(4) ? ? yes
N(3) H(9) 0.86(3) ? ? no
N(3) H(10) 0.88(3) ? ? no
C(2) C(4) 1.507(5) ? ? yes
C(2) H(3) 1.04(3) ? ? no
C(2) H(4) 0.97(3) ? ? no
C(3) C(4) 1.505(5) ? ? yes
C(3) H(7) 0.96(3) ? ? no
C(3) H(8) 1.04(3) ? ? no
C(4) H(5) 0.94(3) ? ? no
C(4) H(6) 0.99(3) ? ? no
