#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/33/2213369.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_2213369
loop_
_publ_author_name
'Zhang, Guo-Fang'
'Zhao, Shu-Min'
'She, Jiang-Bo'
'Ng, Seik Weng'
_publ_section_title
;
 Hexaaquahexakis(μ₂-3,5-diamino-1,2,4-triazole)trinickel(II)
 trisulfate octadecahydrate
;
_journal_coeditor_code           HB2392
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1517
_journal_page_last               m1518
_journal_paper_doi               10.1107/S160053680702051X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni3 (C2 H5 N5)6 (H2 O)6] (S O4)3, 18H2 O'
_chemical_formula_moiety
'[(C2 H5 N5)6 (H2 O)6 Ni3] 6+, 3[S O4] 2-, 18(H2 O)'
_chemical_formula_sum            'C12 H78 N30 Ni3 O36 S3'
_chemical_formula_weight         1491.35
_chemical_name_systematic
;
Hexaaquahexakis(μ₂-3,5-diamino-1,2,4-triazole)trinickel(II) trisulfate
octadecahydrate
;
_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                   12.664(2)
_cell_length_b                   12.664
_cell_length_c                   63.653(6)
_cell_measurement_reflns_used    7201
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      3.2
_cell_volume                     8840.8(16)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Bruker APEX CCD'
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.012
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -82
_diffrn_reflns_number            24396
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.33
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.35
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1P)²+10P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.170
_refine_ls_wR_factor_ref         0.180
_reflns_number_gt                1868
_reflns_number_total             2269
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2392.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        8841(2)
_cod_original_sg_symbol_H-M      'R -3c'
_cod_database_code               2213369
_cod_database_fobs_code          2213369
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, 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'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+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'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x-y, -y, -z-1/2'
'-x, -x+y, -z-1/2'
'y, x, -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'
'x-y+2/3, -y+1/3, -z-1/6'
'-x+2/3, -x+y+1/3, -z-1/6'
'y+2/3, x+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'
'x-y+1/3, -y+2/3, -z+1/6'
'-x+1/3, -x+y+2/3, -z+1/6'
'y+1/3, x+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 0.0833 0.0208(3) Uani d S 1 . .
Ni Ni2 0.6667 0.3333 0.025169(9) 0.0238(2) Uani d S 1 . .
S S1 1.0000 0.0000 0.0000 0.0730(9) Uani d SD 1 . .
S S2 0.6667 0.3333 -0.08615(2) 0.0328(3) Uani d SD 1 . .
O O1 1.0719(19) 0.068(2) 0.0183(3) 0.118(14) Uani d PDU 0.1666667 A -1
O O2 0.8739(9) -0.0434(17) 0.0039(3) 0.071(7) Uani d PDU 0.1666667 B -1
O O3 1.040(2) 0.0874(19) -0.0174(3) 0.098(11) Uani d PDU 0.1666667 C -1
O O4 1.0253(16) -0.0949(13) -0.0048(3) 0.065(6) Uani d PDU 0.1666667 B -1
O O5 0.6667 0.3333 -0.06391(8) 0.107(3) Uani d SDU 1 . .
O O6 0.6948(4) 0.4519(3) -0.09445(7) 0.0967(12) Uani d DU 1 . .
O O1w 0.8185(2) 0.3878(2) 0.00548(3) 0.0359(5) Uani d D 1 . .
H H1w1 0.875(2) 0.390(3) 0.0128(4) 0.043 Uiso d D 1 . .
H H1w2 0.812(3) 0.352(3) -0.0060(3) 0.043 Uiso d D 1 . .
O O2W 1.0048(2) 0.4140(3) 0.03031(5) 0.0591(8) Uani d D 1 . .
H H2w1 1.060(3) 0.4875(15) 0.0326(8) 0.071 Uiso d D 1 . .
H H2w2 1.038(3) 0.370(3) 0.0293(8) 0.071 Uiso d D 1 . .
O O3w 0.8269(3) 0.3208(3) -0.03537(4) 0.0596(7) Uani d D 1 . .
H H3w1 0.781(4) 0.314(3) -0.0456(5) 0.072 Uiso d D 1 . .
H H3w2 0.818(4) 0.251(2) -0.0324(6) 0.072 Uiso d D 1 . .
O O4w 1.1016(4) 0.2587(4) 0.03766(9) 0.0919(12) Uani d D 1 . .
H H4w1 1.099(6) 0.229(6) 0.0495(4) 0.110 Uiso d D 1 . .
H H4w2 1.111(7) 0.220(5) 0.0278(6) 0.110 Uiso d D 1 . .
N N1 0.3477(3) 0.1713(3) 0.08987(5) 0.0489(9) Uani d D 1 . .
H H1n1 0.394(3) 0.157(4) 0.0974(6) 0.059 Uiso d D 1 . .
H H1n2 0.2696(11) 0.134(3) 0.0909(8) 0.059 Uiso d D 1 . .
N N2 0.5086(2) 0.2574(2) 0.06450(3) 0.0265(5) Uani d . 1 . .
N N3 0.5114(2) 0.2826(2) 0.04272(3) 0.0255(5) Uani d . 1 . .
N N4 0.3585(3) 0.2501(3) 0.01736(4) 0.0492(8) Uani d D 1 . .
H H4n1 0.404(3) 0.290(3) 0.0070(4) 0.059 Uiso d D 1 . .
H H4n2 0.292(2) 0.194(3) 0.0123(6) 0.059 Uiso d D 1 . .
N N5 0.3218(2) 0.1958(3) 0.05358(4) 0.0348(6) Uani d D 1 . .
H H5n 0.2477(13) 0.177(3) 0.0544(6) 0.042 Uiso d D 1 . .
C C1 0.3940(3) 0.2063(3) 0.07033(5) 0.0307(6) Uani d . 1 . .
C C2 0.3987(2) 0.2440(3) 0.03683(4) 0.0308(6) 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'
S S 0.1246 0.1234 '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
N2 Ni1 N2 34 35_655 90.85(8)
N2 Ni1 N2 34 36_545 90.85(8)
N2 Ni1 N2 35_655 36_545 90.85(8)
N2 Ni1 N2 34 2_655 177.85(11)
N2 Ni1 N2 35_655 2_655 90.70(12)
N2 Ni1 N2 36_545 2_655 87.63(12)
N2 Ni1 N2 34 . 87.64(12)
N2 Ni1 N2 35_655 . 177.85(11)
N2 Ni1 N2 36_545 . 90.70(12)
N2 Ni1 N2 2_655 . 90.85(8)
N2 Ni1 N2 34 3_665 90.70(12)
N2 Ni1 N2 35_655 3_665 87.64(12)
N2 Ni1 N2 36_545 3_665 177.85(11)
N2 Ni1 N2 2_655 3_665 90.85(8)
N2 Ni1 N2 . 3_665 90.85(8)
N3 Ni2 N3 2_655 3_665 93.50(8)
N3 Ni2 N3 2_655 . 93.50(8)
N3 Ni2 N3 3_665 . 93.50(8)
N3 Ni2 O1w 2_655 . 90.39(9)
N3 Ni2 O1w 3_665 . 87.94(9)
N3 Ni2 O1w . . 175.77(8)
N3 Ni2 O1w 2_655 3_665 87.94(9)
N3 Ni2 O1w 3_665 3_665 175.77(8)
N3 Ni2 O1w . 3_665 90.39(9)
O1w Ni2 O1w . 3_665 88.07(9)
N3 Ni2 O1w 2_655 2_655 175.77(8)
N3 Ni2 O1w 3_665 2_655 90.39(9)
N3 Ni2 O1w . 2_655 87.94(9)
O1w Ni2 O1w . 2_655 88.07(9)
O1w Ni2 O1w 3_665 2_655 88.07(9)
O4 S1 O4 20_665 21_545 115.6(5)
O4 S1 O4 20_665 19_755 115.6(5)
O4 S1 O4 . 2_645 115.6(5)
O4 S1 O4 . 3_765 115.6(5)
O4 S1 O4 2_645 3_765 115.6(5)
O4 S1 O2 21_545 21_545 113.1(8)
O4 S1 O2 3_765 3_765 113.1(8)
O4 S1 O2 . . 113.1(8)
O2 S1 O2 3_765 . 117.0(4)
O4 S1 O2 19_755 19_755 113.1(8)
O2 S1 O2 21_545 19_755 117.0(4)
O4 S1 O2 20_665 20_665 113.1(8)
O2 S1 O2 21_545 20_665 117.0(4)
O2 S1 O2 19_755 20_665 117.0(4)
O4 S1 O2 2_645 2_645 113.1(8)
O2 S1 O2 3_765 2_645 117.0(4)
O2 S1 O2 . 2_645 117.0(4)
O5 S2 O6 . 3_665 111.26(18)
O5 S2 O6 . 2_655 111.26(19)
O6 S2 O6 3_665 2_655 107.6(2)
O5 S2 O6 . . 111.26(18)
O6 S2 O6 3_665 . 107.6(2)
O6 S2 O6 2_655 . 107.6(2)
Ni2 O1w H1w1 . . 108(2)
Ni2 O1w H1w2 . . 121(2)
H1w1 O1w H1w2 . . 110.9(17)
H2w1 O2W H2w2 . . 108.3(17)
H3w1 O3w H3w2 . . 109.4(18)
H4w1 O4w H4w2 . . 113(2)
C1 N1 H1n1 . . 111(3)
C1 N1 H1n2 . . 116(3)
H1n1 N1 H1n2 . . 125(4)
C1 N2 N3 . . 106.5(2)
C1 N2 Ni1 . . 128.87(19)
N3 N2 Ni1 . . 122.82(17)
C2 N3 N2 . . 107.2(2)
C2 N3 Ni2 . . 130.62(18)
N2 N3 Ni2 . . 120.73(16)
C2 N4 H4n1 . . 125(3)
C2 N4 H4n2 . . 123(3)
H4n1 N4 H4n2 . . 107(4)
C2 N5 C1 . . 105.8(2)
C2 N5 H5n . . 128(2)
C1 N5 H5n . . 125(2)
N2 C1 N1 . . 127.9(3)
N2 C1 N5 . . 110.4(3)
N1 C1 N5 . . 121.7(3)
N3 C2 N4 . . 127.6(3)
N3 C2 N5 . . 110.1(2)
N4 C2 N5 . . 122.3(3)
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 N2 . 2.108(2) yes
Ni1 N2 2_655 2.108(2) n
Ni1 N2 3_665 2.108(2) n
Ni1 N2 34 2.108(2) n
Ni1 N2 35_655 2.108(2) n
Ni1 N2 36_545 2.108(2) n
Ni2 N3 . 2.065(2) yes
Ni2 N3 2_655 2.065(2) n
Ni2 N3 3_665 2.065(2) n
Ni2 O1w . 2.101(2) yes
Ni2 O1w 2_655 2.101(2) n
Ni2 O1w 3_665 2.101(2) n
S1 O4 20_665 1.422(8) ?
S1 O4 21_545 1.422(8) ?
S1 O4 19_755 1.422(8) ?
S1 O4 . 1.422(8) ?
S1 O4 2_645 1.422(8) ?
S1 O4 3_765 1.422(8) ?
S1 O2 21_545 1.427(9) ?
S1 O2 3_765 1.427(9) ?
S1 O2 . 1.427(9) ?
S1 O2 19_755 1.427(9) ?
S1 O2 20_665 1.427(9) ?
S1 O2 2_645 1.427(9) ?
S2 O5 . 1.415(5) ?
S2 O6 3_665 1.458(3) ?
S2 O6 2_655 1.458(3) ?
S2 O6 . 1.458(3) ?
O1w H1w1 . 0.838(10) ?
O1w H1w2 . 0.841(10) ?
O2W H2w1 . 0.853(10) ?
O2W H2w2 . 0.852(10) ?
O3w H3w1 . 0.848(10) ?
O3w H3w2 . 0.852(10) ?
O4w H4w1 . 0.838(10) ?
O4w H4w2 . 0.845(10) ?
N1 C1 . 1.352(4) ?
N1 H1n1 . 0.846(10) ?
N1 H1n2 . 0.859(11) ?
N2 C1 . 1.313(4) ?
N2 N3 . 1.419(3) ?
N3 C2 . 1.311(3) ?
N4 C2 . 1.357(4) ?
N4 H4n1 . 0.855(10) ?
N4 H4n2 . 0.846(10) ?
N5 C2 . 1.365(4) ?
N5 C1 . 1.367(4) ?
N5 H5n . 0.847(10) ?
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
O1w H1w1 O2w . 0.840(10) 1.890(10) 2.719(4) 173(3) yes
O1w H1w2 O3w . 0.840(10) 1.94(2) 2.754(3) 162(4) yes
N4 H4n1 O1w 2_655 0.860(10) 2.33(3) 2.962(4) 131(4) yes
N4 H4n2 O2 3_665 0.850(10) 2.41(3) 3.15(2) 147(4) yes
N5 H5n O6 16_544 0.850(10) 2.08(2) 2.843(5) 150(3) yes
O2W H2w1 O3w 19_765 0.850(10) 2.120(10) 2.962(4) 168(4) yes
O2W H2w2 O4w . 0.850(10) 2.01(2) 2.828(5) 160(5) yes
O3w H3w1 O5 . 0.850(10) 1.97(2) 2.787(5) 162(4) yes
O3w H3w2 O4w 21_545 0.850(10) 2.10(2) 2.885(5) 154(5) yes
O4w H4w1 O6 16_644 0.840(10) 1.98(2) 2.786(6) 163(6) yes
O4w H4w2 O1 . 0.850(10) 1.83(4) 2.57(2) 145(6) yes
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
N2 Ni1 N2 C1 34 -41.1(2)
N2 Ni1 N2 C1 36_545 49.7(2)
N2 Ni1 N2 C1 2_655 137.3(3)
N2 Ni1 N2 C1 3_665 -131.8(3)
N2 Ni1 N2 N3 34 121.4(2)
N2 Ni1 N2 N3 36_545 -147.8(2)
N2 Ni1 N2 N3 2_655 -60.12(14)
N2 Ni1 N2 N3 3_665 30.75(16)
C1 N2 N3 C2 . -0.7(3)
Ni1 N2 N3 C2 . -166.61(18)
C1 N2 N3 Ni2 . -168.31(18)
Ni1 N2 N3 Ni2 . 25.8(3)
N3 Ni2 N3 C2 2_655 -131.8(3)
N3 Ni2 N3 C2 3_665 134.5(3)
O1w Ni2 N3 C2 3_665 -43.8(3)
O1w Ni2 N3 C2 2_655 44.2(3)
N3 Ni2 N3 N2 2_655 32.54(16)
N3 Ni2 N3 N2 3_665 -61.19(14)
O1w Ni2 N3 N2 3_665 120.50(19)
O1w Ni2 N3 N2 2_655 -151.45(19)
N3 N2 C1 N1 . -176.9(3)
Ni1 N2 C1 N1 . -12.1(4)
N3 N2 C1 N5 . 0.5(3)
Ni1 N2 C1 N5 . 165.2(2)
C2 N5 C1 N2 . -0.1(3)
C2 N5 C1 N1 . 177.4(3)
N2 N3 C2 N4 . 179.5(3)
Ni2 N3 C2 N4 . -14.5(5)
N2 N3 C2 N5 . 0.7(3)
Ni2 N3 C2 N5 . 166.6(2)
C1 N5 C2 N3 . -0.4(3)
C1 N5 C2 N4 . -179.3(3)
