#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322679.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_4322679
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 F12 Fe N18 Ni3 P2'
_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 11:16:43 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                   14.588(1)
_cell_length_b                   14.5879
_cell_length_c                   17.050(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      29.03
_cell_volume                     3142.3(4)
_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    SIR88
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.00120
_diffrn_orient_matrix_UB_12      -0.00979
_diffrn_orient_matrix_UB_13      0.05797
_diffrn_orient_matrix_UB_21      0.07904
_diffrn_orient_matrix_UB_22      0.04314
_diffrn_orient_matrix_UB_23      -0.00042
_diffrn_orient_matrix_UB_31      -0.00404
_diffrn_orient_matrix_UB_32      0.06564
_diffrn_orient_matrix_UB_33      0.00892
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  1.34
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1354
_diffrn_reflns_theta_max         25.0016
_diffrn_standards_decay_%        16.89
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 18.429
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1734.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         -0.26420
_refine_diff_density_min         0.17600
_refine_ls_extinction_coef       4.80857
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.190
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1130
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0190
_refine_ls_shift/esd_max         0.2690
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0190
_cod_data_source_file            ic9711168_2.cif
_cod_data_source_block           '[Ni(tn)2]3[Fe(CN)6](PF6)2'
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C24 H60 N18 P2 F12 Ni3 Fe'
_cod_database_code               4322679
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
Ni1 1.1667 0.3333 0.8333 0.0198 Uij ? ?
Fe1 1.0000 0.0000 1.0000 0.0152 Uij ? ?
P1 1.0000 0.0000 0.64026(6) 0.0267 Uij ? ?
F1 1.0812(1) 0.09619(10) 0.58795(8) 0.0498 Uij ? ?
F2 1.09598(10) 0.0154(1) 0.69512(8) 0.0483 Uij ? ?
N1 1.1429(1) 0.1951(1) 0.89702(9) 0.0275 Uij ? ?
N2 1.0028(1) 0.2459(1) 0.8087(1) 0.0295 Uij ? ?
N3 1.1297(2) 0.3821(2) 0.9394(1) 0.0291 Uij ? ?
C1 1.0912(1) 0.1205(1) 0.9351(1) 0.0196 Uij ? ?
C2 0.9365(2) 0.2938(2) 0.8263(1) 0.0357 Uij ? ?
C3 0.9426(2) 0.3233(2) 0.9115(1) 0.0394 Uij ? ?
C4 1.0482(2) 0.4131(2) 0.9374(1) 0.0326 Uij ? ?
H1 0.983(2) 0.192(2) 0.836(1) 0.041(7) Uij ? ?
H2 0.995(2) 0.228(2) 0.759(1) 0.040(7) Uij ? ?
H3 0.965(2) 0.359(2) 0.792(1) 0.042(6) Uij ? ?
H4 0.863(2) 0.245(2) 0.812(1) 0.047(7) Uij ? ?
H5 0.891(2) 0.343(2) 0.921(1) 0.042(6) Uij ? ?
H6 0.925(2) 0.262(2) 0.944(1) 0.042(6) Uij ? ?
H7 1.042(2) 0.442(2) 0.987(1) 0.034(6) Uij ? ?
H8 1.072(1) 0.471(2) 0.902(1) 0.026(5) Uij ? ?
H9 1.109(2) 0.327(2) 0.970(1) 0.047(7) Uij ? ?
H10 1.182(2) 0.431(2) 0.957(1) 0.034(7) 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'
P 0 6 0.102 0.094 'International Tables'
F 0 36 0.017 0.010 'International Tables'
Fe 0 3 0.346 0.844 'International Tables'
Ni 0 9 0.339 1.112 '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(1) N(1) 179.9626 ? ? ? yes
N(1) Ni(1) N(2) 86.08(7) ? ? ? yes
N(1) Ni(1) N(2) 93.93(7) ? ? ? yes
N(1) Ni(1) N(3) 86.26(7) ? ? ? yes
N(1) Ni(1) N(3) 93.75(7) ? ? ? yes
N(1) Ni(1) N(2) 93.94(7) ? ? ? yes
N(1) Ni(1) N(2) 86.06(7) ? ? ? yes
N(1) Ni(1) N(3) 93.71(7) ? ? ? yes
N(1) Ni(1) N(3) 86.29(7) ? ? ? yes
N(2) Ni(1) N(2) 179.9661 ? ? ? yes
N(2) Ni(1) N(3) 88.35(7) ? ? ? yes
N(2) Ni(1) N(3) 91.67(7) ? ? ? yes
N(2) Ni(1) N(3) 91.62(7) ? ? ? yes
N(2) Ni(1) N(3) 88.37(7) ? ? ? yes
N(3) Ni(1) N(3) 179.9806 ? ? ? yes
C(1) Fe(1) C(1) 89.46(7) ? ? ? yes
C(1) Fe(1) C(1) 90.54(7) ? ? ? yes
C(1) Fe(1) C(1) 89.46(7) ? ? ? yes
C(1) Fe(1) C(1) 180.0000 ? ? ? yes
C(1) Fe(1) C(1) 90.54(7) ? ? ? yes
C(1) Fe(1) C(1) 89.46(7) ? ? ? yes
C(1) Fe(1) C(1) 90.54(7) ? ? ? yes
C(1) Fe(1) C(1) 90.54(7) ? ? ? yes
C(1) Fe(1) C(1) 180.0000 ? ? ? yes
C(1) Fe(1) C(1) 180.0000 ? ? ? yes
C(1) Fe(1) C(1) 89.46(7) ? ? ? yes
C(1) Fe(1) C(1) 90.54(7) ? ? ? yes
C(1) Fe(1) C(1) 90.54(7) ? ? ? yes
C(1) Fe(1) C(1) 89.46(7) ? ? ? yes
C(1) Fe(1) C(1) 89.46(7) ? ? ? yes
F(1) P(1) F(1) 91.36(8) ? ? ? yes
F(1) P(1) F(1) 91.36(8) ? ? ? yes
F(1) P(1) F(2) 89.46(7) ? ? ? yes
F(1) P(1) F(2) 89.75(7) ? ? ? yes
F(1) P(1) F(2) 178.60(9) ? ? ? yes
F(1) P(1) F(1) 91.36(8) ? ? ? yes
F(1) P(1) F(2) 178.60(9) ? ? ? yes
F(1) P(1) F(2) 89.46(7) ? ? ? yes
F(1) P(1) F(2) 89.75(7) ? ? ? yes
F(1) P(1) F(2) 89.75(7) ? ? ? yes
F(1) P(1) F(2) 178.60(9) ? ? ? yes
F(1) P(1) F(2) 89.46(7) ? ? ? yes
F(2) P(1) F(2) 89.41(8) ? ? ? yes
F(2) P(1) F(2) 89.41(8) ? ? ? yes
F(2) P(1) F(2) 89.41(8) ? ? ? yes
Ni(1) N(1) Ni(1) 0.0374 ? ? ? yes
Ni(1) N(1) C(1) 151.7(1) ? ? ? yes
Ni(1) N(1) C(1) 151.7(1) ? ? ? yes
Ni(1) N(2) Ni(1) 0.0339 ? ? ? yes
Ni(1) N(2) C(2) 118.9(1) ? ? ? yes
Ni(1) N(2) H(1) 102(1) ? ? ? no
Ni(1) N(2) H(2) 108(1) ? ? ? no
Ni(1) N(2) C(2) 118.9(1) ? ? ? yes
Ni(1) N(2) H(1) 102(1) ? ? ? no
Ni(1) N(2) H(2) 108(1) ? ? ? no
C(2) N(2) H(1) 108(1) ? ? ? no
C(2) N(2) H(2) 108(1) ? ? ? no
H(1) N(2) H(2) 109(2) ? ? ? no
Ni(1) N(3) Ni(1) 0.0194 ? ? ? yes
Ni(1) N(3) C(4) 117.9(1) ? ? ? yes
Ni(1) N(3) H(9) 102(1) ? ? ? no
Ni(1) N(3) H(10) 109(1) ? ? ? no
Ni(1) N(3) C(4) 117.9(1) ? ? ? yes
Ni(1) N(3) H(9) 102(1) ? ? ? no
Ni(1) N(3) H(10) 109(1) ? ? ? no
C(4) N(3) H(9) 109(1) ? ? ? no
C(4) N(3) H(10) 107(1) ? ? ? no
H(9) N(3) H(10) 109(1) ? ? ? no
Fe(1) C(1) N(1) 176.6(2) ? ? ? yes
N(2) C(2) C(3) 111.9(2) ? ? ? yes
N(2) C(2) H(3) 105(1) ? ? ? no
N(2) C(2) H(4) 110(1) ? ? ? no
C(3) C(2) H(3) 110(1) ? ? ? no
C(3) C(2) H(4) 109(1) ? ? ? no
H(3) C(2) H(4) 108(1) ? ? ? no
C(2) C(3) C(4) 114.8(2) ? ? ? yes
C(2) C(3) H(5) 107(1) ? ? ? no
C(2) C(3) H(6) 109(1) ? ? ? no
C(4) C(3) H(5) 108(1) ? ? ? no
C(4) C(3) H(6) 109(1) ? ? ? no
H(5) C(3) H(6) 107(1) ? ? ? no
N(3) C(4) C(3) 111.9(2) ? ? ? yes
N(3) C(4) H(7) 112(1) ? ? ? no
N(3) C(4) H(8) 107(1) ? ? ? no
C(3) C(4) H(7) 110(1) ? ? ? no
C(3) C(4) H(8) 110(1) ? ? ? no
H(7) C(4) H(8) 103(1) ? ? ? 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(1) N(1) 2.160(2) ? ? yes
Ni(1) N(1) 2.160(2) ? ? yes
Ni(1) N(2) 2.114(2) ? ? yes
Ni(1) N(2) 2.115(2) ? ? yes
Ni(1) N(3) 2.109(2) ? ? yes
Ni(1) N(3) 2.108(2) ? ? yes
Fe(1) C(1) 1.936(2) ? ? yes
Fe(1) C(1) 1.936(2) ? ? yes
Fe(1) C(1) 1.936(2) ? ? yes
Fe(1) C(1) 1.936(2) ? ? yes
Fe(1) C(1) 1.936(2) ? ? yes
Fe(1) C(1) 1.936(2) ? ? yes
P(1) F(1) 1.583(1) ? ? yes
P(1) F(1) 1.583(1) ? ? yes
P(1) F(1) 1.583(1) ? ? yes
P(1) F(2) 1.604(1) ? ? yes
P(1) F(2) 1.604(1) ? ? yes
P(1) F(2) 1.604(1) ? ? yes
N(1) C(1) 1.163(2) ? ? yes
N(2) C(2) 1.479(3) ? ? yes
N(2) H(1) 0.83(2) ? ? no
N(2) H(2) 0.88(2) ? ? no
N(3) C(4) 1.469(3) ? ? yes
N(3) H(9) 0.88(2) ? ? no
N(3) H(10) 0.80(2) ? ? no
C(2) C(3) 1.505(3) ? ? yes
C(2) H(3) 1.01(2) ? ? no
C(2) H(4) 0.98(2) ? ? no
C(3) C(4) 1.506(3) ? ? yes
C(3) H(5) 0.95(2) ? ? no
C(3) H(6) 0.96(2) ? ? no
C(4) H(7) 0.97(2) ? ? no
C(4) H(8) 0.95(2) ? ? no
