#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/85/2218529.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2218529
loop_
_publ_author_name
'Wu, Li-Ping'
'Zhao, Shu-Ming'
'Zhang, Guo-Fang'
'Ng, Seik Weng'
_publ_section_title
;
 Hexaaquahexakis(μ₂-3,5-diamino-4H-1,2,4-triazole)trinickel(II)
 tris(hexafluoridosilicate) icosahydrate
;
_journal_coeditor_code           SI2084
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m802
_journal_paper_doi               10.1107/S1600536808013329
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni3 (C2 H5 N5)6 (H2 O)6] [Si F6]3, 20H2 O'
_chemical_formula_moiety         'C12 H42 N30 Ni3 O6 6+, 3(Si F6 2-), 20 H2 O'
_chemical_formula_sum            'C12 H82 F18 N30 Ni3 O26 Si3'
_chemical_formula_weight         1665.48
_chemical_name_systematic
;
Hexaaquahexakis(μ₂-3,5-diamino-4H-1,2,4-triazole)trinickel(II)
tris(hexafluoridosilicate) icosahydrate
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.0240(10)
_cell_length_b                   13.024
_cell_length_c                   64.462(5)
_cell_measurement_reflns_used    5839
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      3.1
_cell_volume                     9469.4(10)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0098
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            25347
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2420
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0612P)²+17.0807P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                2093
_reflns_number_total             2420
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            si2084.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        9469.8(9)
_cod_original_sg_symbol_H-M      'R -3c'
_cod_database_code               2218529
_cod_database_fobs_code          2218529
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.6667 0.3333 0.140787(6) 0.02689(14) Uani d S 1 . .
Ni Ni2 0.6667 0.3333 0.0833 0.02377(16) Uani d S 1 . .
Si Si1 1.0000 0.0000 0.083802(16) 0.0331(2) Uani d S 1 . .
Si Si2 0.3333 -0.3333 0.1667 0.0552(5) Uani d S 1 . .
F F1 0.89685(14) 0.00226(15) 0.09960(2) 0.0623(4) Uani d . 1 . .
F F2 1.00168(16) 0.10635(14) 0.06943(3) 0.0648(4) Uani d . 1 . .
F F3 0.3983(3) -0.3868(3) 0.15169(5) 0.1399(12) Uani d . 1 . .
O O1 0.72286(15) 0.24063(14) 0.16010(2) 0.0398(3) Uani d D 1 . .
H H11 0.723(3) 0.1843(18) 0.1533(3) 0.060 Uiso d D 1 . .
H H12 0.699(3) 0.217(2) 0.1724(2) 0.060 Uiso d D 1 . .
O O2 0.7536(2) 0.0854(2) 0.13625(4) 0.0660(5) Uani d D 1 . .
H H21 0.713(2) 0.0108(10) 0.1358(6) 0.099 Uiso d D 1 . .
H H22 0.8267(10) 0.108(3) 0.1361(7) 0.099 Uiso d D 1 . .
O O3 0.65459(19) 0.15616(17) 0.19955(3) 0.0599(5) Uani d D 1 . .
H H31 0.5874(17) 0.094(2) 0.1978(5) 0.090 Uiso d D 1 . .
H H32 0.650(3) 0.197(2) 0.2092(4) 0.090 Uiso d D 1 . .
O O4 0.6041(2) -0.1661(3) 0.12859(4) 0.0796(6) Uani d D 1 . .
H H41 0.576(3) -0.184(4) 0.1164(3) 0.119 Uiso d D 1 . .
H H42 0.551(3) -0.182(4) 0.1374(4) 0.119 Uiso d D 1 . .
O O5 0.664(3) -0.1549(17) 0.0893(3) 0.185(7) Uani d PU 0.3333 A -1
H H51 0.7382 -0.1072 0.0905 0.278 Uiso d PR 0.3333 A -1
H H52 0.6338 -0.1239 0.0816 0.278 Uiso d PR 0.3333 A -1
N N1 0.61588(14) 0.43372(14) 0.12352(2) 0.0290(3) Uani d . 1 . .
N N2 0.59282(14) 0.41343(14) 0.10195(2) 0.0293(3) Uani d . 1 . .
N N3 0.52872(17) 0.53100(17) 0.11289(3) 0.0381(4) Uani d D 1 . .
H H3 0.500(2) 0.576(2) 0.1117(4) 0.057 Uiso d D 1 . .
N N4 0.5100(2) 0.4865(2) 0.07683(3) 0.0508(5) Uani d D 1 . .
H H4A 0.514(3) 0.449(3) 0.0663(4) 0.076 Uiso d D 1 . .
H H4B 0.468(2) 0.517(3) 0.0744(6) 0.076 Uiso d D 1 . .
N N5 0.5810(2) 0.5478(2) 0.14862(3) 0.0556(6) Uani d D 1 . .
H H5A 0.625(3) 0.540(3) 0.1574(4) 0.083 Uiso d D 1 . .
H H5B 0.535(3) 0.575(3) 0.1509(5) 0.083 Uiso d D 1 . .
C C1 0.57611(18) 0.50413(18) 0.12943(3) 0.0343(4) Uani d . 1 . .
C C2 0.54160(17) 0.47436(17) 0.09630(3) 0.0336(4) Uani d . 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Ni1 N1 3_665 2_655 93.61(6)
N1 Ni1 N1 3_665 . 93.61(6)
N1 Ni1 N1 2_655 . 93.61(6)
N1 Ni1 O1 3_665 . 87.31(6)
N1 Ni1 O1 2_655 . 90.45(6)
N1 Ni1 O1 . . 175.77(6)
N1 Ni1 O1 3_665 2_655 90.45(6)
N1 Ni1 O1 2_655 2_655 175.77(6)
N1 Ni1 O1 . 2_655 87.31(6)
O1 Ni1 O1 . 2_655 88.56(6)
N1 Ni1 O1 3_665 3_665 175.78(6)
N1 Ni1 O1 2_655 3_665 87.31(6)
N1 Ni1 O1 . 3_665 90.45(6)
O1 Ni1 O1 . 3_665 88.56(6)
O1 Ni1 O1 2_655 3_665 88.56(6)
N2 Ni2 N2 16_544 17_554 90.87(6)
N2 Ni2 N2 16_544 18_654 90.87(6)
N2 Ni2 N2 17_554 18_654 90.87(6)
N2 Ni2 N2 16_544 3_665 87.57(8)
N2 Ni2 N2 17_554 3_665 177.79(8)
N2 Ni2 N2 18_654 3_665 90.72(8)
N2 Ni2 N2 16_544 2_655 90.72(8)
N2 Ni2 N2 17_554 2_655 87.57(8)
N2 Ni2 N2 18_654 2_655 177.79(8)
N2 Ni2 N2 3_665 2_655 90.88(6)
N2 Ni2 N2 16_544 . 177.79(8)
N2 Ni2 N2 17_554 . 90.72(8)
N2 Ni2 N2 18_654 . 87.57(8)
N2 Ni2 N2 3_665 . 90.88(6)
N2 Ni2 N2 2_655 . 90.88(6)
F2 Si1 F2 . 2_645 91.80(9)
F2 Si1 F2 . 3_765 91.80(9)
F2 Si1 F2 2_645 3_765 91.80(9)
F2 Si1 F1 . 3_765 90.36(8)
F2 Si1 F1 2_645 3_765 177.12(10)
F2 Si1 F1 3_765 3_765 90.03(8)
F2 Si1 F1 . 2_645 177.12(10)
F2 Si1 F1 2_645 2_645 90.03(8)
F2 Si1 F1 3_765 2_645 90.36(8)
F1 Si1 F1 3_765 2_645 87.74(9)
F2 Si1 F1 . . 90.03(8)
F2 Si1 F1 2_645 . 90.36(8)
F2 Si1 F1 3_765 . 177.12(10)
F1 Si1 F1 3_765 . 87.74(9)
F1 Si1 F1 2_645 . 87.74(9)
F3 Si2 F3 25_545 27_445 89.21(17)
F3 Si2 F3 25_545 26 89.21(17)
F3 Si2 F3 27_445 26 89.21(17)
F3 Si2 F3 25_545 2_545 90.79(17)
F3 Si2 F3 27_445 2_545 90.79(17)
F3 Si2 F3 26 2_545 179.9950(10)
F3 Si2 F3 25_545 3_655 90.79(17)
F3 Si2 F3 27_445 3_655 179.9950(10)
F3 Si2 F3 26 3_655 90.79(17)
F3 Si2 F3 2_545 3_655 89.21(17)
F3 Si2 F3 25_545 . 179.9970(10)
F3 Si2 F3 27_445 . 90.79(17)
F3 Si2 F3 26 . 90.79(17)
F3 Si2 F3 2_545 . 89.21(17)
F3 Si2 F3 3_655 . 89.21(17)
Ni1 O1 H11 . . 110(2)
Ni1 O1 H12 . . 126(2)
H11 O1 H12 . . 109(2)
H21 O2 H22 . . 111(2)
H31 O3 H32 . . 110(2)
H41 O4 H42 . . 111(2)
H51 O5 H52 . . 109.4
C1 N1 N2 . . 107.04(15)
C1 N1 Ni1 . . 130.48(12)
N2 N1 Ni1 . . 121.05(11)
C2 N2 N1 . . 106.38(15)
C2 N2 Ni2 . . 129.31(13)
N1 N2 Ni2 . . 122.87(12)
C2 N3 C1 . . 106.38(16)
C2 N3 H3 . . 122(2)
C1 N3 H3 . . 132(2)
C2 N4 H4A . . 125(2)
C2 N4 H4B . . 122(3)
H4A N4 H4B . . 111(3)
C1 N5 H5A . . 117(2)
C1 N5 H5B . . 116(2)
H5A N5 H5B . . 126(3)
N1 C1 N5 . . 127.37(19)
N1 C1 N3 . . 109.86(16)
N5 C1 N3 . . 122.76(18)
N2 C2 N4 . . 126.92(19)
N2 C2 N3 . . 110.33(17)
N4 C2 N3 . . 122.67(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 . 2.062(2) yes
Ni1 N1 2_655 2.062(2) ?
Ni1 N1 3_665 2.062(2) ?
Ni1 O1 . 2.104(2) yes
Ni1 O1 2_655 2.104(2) ?
Ni1 O1 3_665 2.104(2) ?
Ni2 N2 16_544 2.111(2) ?
Ni2 N2 17_554 2.111(2) ?
Ni2 N2 18_654 2.111(2) ?
Ni2 N2 3_665 2.111(2) ?
Ni2 N2 2_655 2.111(2) ?
Ni2 N2 . 2.111(2) yes
Si1 F2 . 1.6574(15) ?
Si1 F2 2_645 1.6574(15) ?
Si1 F2 3_765 1.6574(15) ?
Si1 F1 3_765 1.6976(15) ?
Si1 F1 2_645 1.6976(15) ?
Si1 F1 . 1.6976(15) ?
Si2 F3 25_545 1.649(3) ?
Si2 F3 27_445 1.649(3) ?
Si2 F3 26 1.649(3) ?
Si2 F3 2_545 1.649(3) ?
Si2 F3 3_655 1.649(3) ?
Si2 F3 . 1.649(3) ?
O1 H11 . 0.86(3) ?
O1 H12 . 0.85(3) ?
O2 H21 . 0.84(3) ?
O2 H22 . 0.84(3) ?
O3 H31 . 0.85(3) ?
O3 H32 . 0.84(3) ?
O4 H41 . 0.85(3) ?
O4 H42 . 0.84(3) ?
O5 H51 . 0.85 ?
O5 H52 . 0.85 ?
N1 C1 . 1.315(2) ?
N1 N2 . 1.419(2) ?
N2 C2 . 1.318(3) ?
N3 C2 . 1.356(3) ?
N3 C1 . 1.362(3) ?
N3 H3 . 0.850(10) ?
N4 C2 . 1.354(3) ?
N4 H4A . 0.85(3) ?
N4 H4B . 0.84(3) ?
N5 C1 . 1.350(3) ?
N5 H5A . 0.84(3) ?
N5 H5B . 0.85(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H11 O2 . 0.86(3) 1.88(3) 2.724(3) 168(3) no
O1 H12 O3 . 0.85(3) 1.89(3) 2.737(2) 174(3) no
O2 H21 O4 . 0.84(3) 2.07(3) 2.896(4) 168(4) no
O2 H22 O3 25_655 0.84(3) 2.12(3) 2.961(3) 175(4) no
O3 H31 O4 27_445 0.85(3) 2.05(3) 2.861(3) 159(3) no
O3 H32 F1 27_445 0.84(3) 2.13(3) 2.904(2) 153(3) no
O4 H41 F2 16_534 0.85(3) 2.23(3) 2.950(3) 143(4) no
O4 H42 F3 2_545 0.84(3) 2.16(3) 2.973(4) 162(4) no
O4 H41 O5 . 0.85(3) 2.03(3) 2.64(2) 128(4) no
O5 H51 F1 . 0.85 1.92 2.76(3) 167 no
N3 H3 F2 16_544 0.85(3) 1.97(3) 2.764(2) 157(3) no
N4 H4b F1 16_544 0.84(3) 2.14(3) 2.974(3) 170(3) no
N5 H5a O1 2_655 0.84(3) 2.23(3) 2.942(3) 142(3) no
N5 H5b F3 1_565 0.85(3) 2.08(3) 2.909(3) 167(3) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
N1 Ni1 N1 C1 3_665 -135.1(2)
N1 Ni1 N1 C1 2_655 131.1(2)
O1 Ni1 N1 C1 2_655 -44.81(19)
O1 Ni1 N1 C1 3_665 43.72(19)
N1 Ni1 N1 N2 3_665 60.39(10)
N1 Ni1 N1 N2 2_655 -33.46(12)
O1 Ni1 N1 N2 2_655 150.67(13)
O1 Ni1 N1 N2 3_665 -120.79(13)
C1 N1 N2 C2 . 0.6(2)
Ni1 N1 N2 C2 . 168.37(13)
C1 N1 N2 Ni2 . 168.09(13)
Ni1 N1 N2 Ni2 . -24.17(18)
N2 Ni2 N2 C2 17_554 -48.86(15)
N2 Ni2 N2 C2 18_654 41.98(14)
N2 Ni2 N2 C2 3_665 132.67(18)
N2 Ni2 N2 C2 2_655 -136.44(18)
N2 Ni2 N2 N1 17_554 146.76(16)
N2 Ni2 N2 N1 18_654 -122.40(15)
N2 Ni2 N2 N1 3_665 -31.71(12)
N2 Ni2 N2 N1 2_655 59.18(10)
N2 N1 C1 N5 . -179.0(2)
Ni1 N1 C1 N5 . 14.9(3)
N2 N1 C1 N3 . -0.1(2)
Ni1 N1 C1 N3 . -166.30(14)
C2 N3 C1 N1 . -0.4(2)
C2 N3 C1 N5 . 178.5(2)
N1 N2 C2 N4 . 176.0(2)
Ni2 N2 C2 N4 . 9.6(3)
N1 N2 C2 N3 . -0.9(2)
Ni2 N2 C2 N3 . -167.25(14)
C1 N3 C2 N2 . 0.8(2)
C1 N3 C2 N4 . -176.2(2)
