data_I 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 Bis(nickel hexahydrate ) diammonium decavanadate tetrahydrate 
; 
# PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic     ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?
_journal_coeditor_code            ?
#==============================================================================
# SUBMISSION DETAILS
_publ_contact_author_name            'Chun-An Ma' 
_publ_contact_author_address          
;
State Key Laboratory Breeding Base of Green 
Chemistry-Synthesis Technology, College of Chemical 
Engineering and Materials Science
Zhejiang  University of Technology 
Hangzhou
320014
People's Republic of  china
;                
_publ_contact_author_email           'science@zjut.edu.cn, srsyxieaili@163.com' 
_publ_contact_author_fax             '+86-571-88320830'  
_publ_contact_author_phone           '+86-571-88320830'  
_publ_contact_letter
;
   We are grateful if this CIF submission will be considered for 
publication in Acta Crystallographica, Section E. 
;
    
_publ_requested_journal              'Acta Crystallographica Section E' 
_publ_requested_category               EI
_publ_requested_coeditor_name       '?'    
#==============================================================================
# TITLE AND AUTHOR LIST
_publ_section_title
;
Bis(nickel hexahydrate ) diammonium decavanadate tetrahydrate,
[Ni(H~2~O)~6~]~2~(NH~4~)~2~V~10~O~28~.4H~2~O  
;
loop_
_publ_author_name
_publ_author_address
'Ai-Li Xie'
;
1.Department of chemistry 
Shangrao Normal College 
Shangrao
334001
People's Republic of  China
2.State Key Laboratory Breeding Base of Green 
Chemistry-Synthesis Technology, College of Chemical 
Engineering and Materials Science 
Zhejiang University of Technology 
Hangzhou
320014
People's Republic of  China
;
'Chun-An Ma'
; 
State Key Laboratory Breeding Base of Green 
Chemistry-Synthesis Technology, College of Chemical 
Engineering and Materials Science
Zhejiang University of Technology 
Hangzhou 
320014
People's Republic of  China
;
'Lian-Bang Wang'
;
State Key Laboratory Breeding Base of Green 
Chemistry-Synthesis Technology, College of Chemical 
Engineering and Materials Science 
Zhejiang University of Technology 
Hangzhou
320014
People's Republic of  China
;
#==============================================================================
# TEXT
_publ_section_abstract
;
The crystal structure of the novel title compound, 
[Ni(H~2~O)~6~]~2~(NH~4~)~2~ V~10~O~28~.4H~2~O, 
contains centrosymmetric [V~10~O~28~]^6-^ anions 
separated by the ammonium and nickel hexahydrate 
cations, and water molecules, in the bc plane structure.
;
_publ_section_comment
;
Recently, the decavanadate salt of nickel metal and double 
salts of nickel metal with alkali metal have been reported, viz.
[Ni(H~2~O)~6~]~2~[Na(H~2~O)~3~]~2~[V~10~O~28~].4H~2~O
(Higami et al, 2002), NiNa~4~[HV~10~O~28~].23H~2~O(Sum et al, 
2002), [K(H~2~O)~2~ Ni(H~2~O)~6~]~2~[V~10~O~28~]
(Li et al, 2004). However, no nickel metal double salt with 
ammonium has yet been reported. We present here the crystal 
structure of a novel decavanadate, bis(nickel hexahydrate) 
diammonium decavanadate tetrahydrate (I), consists of a polyanions 
 [V~10~O~28~]^6-^, two nickel hexahydrate [Ni(H~2~O)~6~]^2+^, 
two ammonium [NH~4~]^+^ and four lattice water (Fig. 1).
In the compound (I),  the centrosymmetric polyanion is composed of 
ten VO~6~ octahedra combined via shared edges and shared corners, 
the array of O and V atoms in the polyanion is the same as those 
in the [Li~6~(H~2~O)~16~V~10~O~28~]~n~(Xie & Ma, 2005) and 
{[LiNa~2~(H~2~O)~9~]~2~[V~10~O~28~]}~n~(Ma et al, 2005) reported 
previously. however, [Ni(H~2~O)~6~]^2+^ cations in the (I) are 
octahedrally coordinated by six water molecules.
In the [V~10~O~28~]^6-^ polyanion structure, The V...V distances 
are in the range 3.0537(14)-3.1155(8)\%A; the V-O distance is in 
the range of 1.5985(9)-1.6136(18)\%A; the V-O-\m~2~ distance is in 
the range of 1.6840(19)-2.0214(19)\%A; the V-O-\m~3~ distance is in 
the range of 1.9069(17)-1.9965(18)\%A; the V-O-\m~6~ distance is in 
the range of 2.1057(19)-2.3410(19)\%A. The bond lengths and angles 
of the [V~10~O~28~]^6-^ polyanion show a similar trend to those found 
in the literature (Kamenar et al., 1996; Choi et al., 2003; Xie & Ma, 
2005; Ma et al., 2005). However, All O atoms on the surface of the 
decavanadate don't form chemical bonds with atoms in other molecules 
on comparison with the [Li~6~(H~2~O)~16~V~10~O~28~]~n~(Xie & Ma, 
2005) and {[LiNa~2~(H~2~O)~9~]~2~[V~10~O~28~]}~n~(Ma et al, 2005). 
The Ni^2+^ cations in (I) are octahedrally coordinated by six water 
molecules. The NiO~6~ is better regular octahedron. In the octahedron, 
the lengths of the Ni---O bonds are in the range of 2.047(2)-2.0848(19)\%A,
the angles of cis-O-Ni-O are in the range of 84.79(7)-95.55(9)\% and 
the angles of trans-O-Ni-O are in the range of 172.97(8)-175.84(7)\%. 
The normal bond lengths and angles of the compound are listed in Table 1.
The compound composed of centrosymmetric [V~10~O~28~]^6-^
polyanions linked by [Ni(H~2~O)~6~]^2+^ and [NH~4~]^+^ cations 
via Ni---O-water---H...O-polyanion, O-water---H...O-polyanion, 
N---H...O-water and N-H...O-polyanion hydrogen bonds, with 
O-water---H...O-polyanion bond lengths of 2.671(3)-3.300(3)\%A,  
N---H...O-polyanion bond lengths of 2.957(3)\%A and 
N---H...O-water bond lengths of 2.825(3)-3.195(3)\%A. In the water 
molecules, as can be seen in the large bond angles of 118.4\% and 
117.9\% for H(19A)---O(19)---H(19B) and H(20A)---O(20)---H(20B), 
and 115.7\% for H(23B)---N---H(23C) and H(23B)---N---H(23D), 
the opening of these angles may be caused by the hydrogen bonds 
formed (shown in Fig.2 ).
The hydrogen-bonds occur between the ployanion,  hydration cations, 
ammonium ions and lattice H~2~O molecules in the compound. All the
 water molecules and ammonium ion form hydrogen bonds with O atoms 
on the surface of the decavanadate(except the O13 atom), and there are also 
Ow---H...Ow hydrogen-bond interactions. Hydrogen-bonds with a distance 
less than 3.300(3)\%A are listed in Table 2. The ployanions, hydration ions, 
ammonium ions and lattice H~2~O molecules (shown in Fig. 3) are then linked
by hydrogen bonds into a three-dimensional framework, the hydrogen bonds 
stabilize the structure. 
;
_publ_section_references
;
Choi H., & Chang Y. Y.(2003). Chem. Mater. 15, 3261-3267.
Higami T., Hashimoto M. & Okeye S.(2002). Acta Cryst. C58, 
i144-i146
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
Kamenar B., Clndric M. & Strukan N. (1996). Acta Cryst.C52, 
1338-1341.
Li D. H., Liu S. X., Peng J., Shao K. Z., Xu H. B., Zhai H. J. & Wang 
E. B.(2004). Chinese Journal of Inorganic Chemistry20(9), 1076-1080
Rigaku, Corporation (1998), 3-9-12 Akishima, Tokyo 196-8666, Japan. 
Rigaku, Corporation (2002), 3-9-12 Akishima, Tokyo 196-8666, Japan. 
Rigaku/MSC(2004). 9009 New Trails Dr. The Woodlands TX, USA 
77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. 
Ma C. A., Xie A. L. & Wang L. B.(2005). Acta Cryst. E61, i185--i187.
Sheldrick G. M.(1990). SHELXL-97. Acta Cryst. A46, 467-473. 
Sheldrick G. M.(1997). SHELXL-97. University of G\"ottingen, 
Germany.
Sum Z. G., Long L. S., Ren Y. P., Huang R. B. & Zheng L. S.(2002). 
Acta Cryst. C58(5), i34-i36
Watkin D. J., Prout, C. K., Carruthers, J. R. & Betteridge, P. W.
(1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, 
Oxford, UK.
Xie A. L. & Ma C. A., (2005). Acta Cryst. C61, i67-i68.
;
_publ_section_figure_captions
;
Figure 1 
The structure of (I), with 40% probability displacement ellipsoids, 
showing the labeling of the atoms [Symmetry codes:(i) x-1, y, z]. 
   
Figure 2
The unit-cell packing and interactions of O atoms between the ployanion,  
hydration cations, ammonium ions and lattice H~2~O molecules in (I).
A part of  hydrogen bond is shown as a broken line  [Symmetry codes: 
(i) x-1, y, z].
Figure 3
The structure of  (I) shown in the bc plane.  The hydrogen bond
is shown as a broken line.
;
_publ_section_exptl_prep
;
The compound was prepared by hydrothermal treatment of
NH~4~VO~3~ and Ni(Ac)~2~.4H~2~O(in a 1:0.2 molar ratio)
acidified to pH 5 .The reaction mixture was heated for 10 h at
398 K. The filtrate was kept at room temperature and orange 
single crystals formed after 20 d.
;     
_publ_section_exptl_refinement
;
All hydrogen atoms and other atoms were found in a difference 
Fourier map, and H atoms were included in the final cycles of
refinement in the riding-motion approximation, with the O-H 
distances fixed at the chemically reasonable distances found in 
the difference map and U(iso)(H)=1.2U~eq~ of the carrier atom.
;
_publ_section_acknowledgement
;
The work at Hangzhou was supported by the National Science 
Foundation through grant No.20476097.
;
  
#==============================================================================
data__XAL-132
#==============================================================================
# CHEMICAL DATA
_chemical_formula_sum                  'H40 N2 Ni2 O44 V10 '
_chemical_formula_moiety               'O28 V10, 2(H12 Ni O6), 2(H4 N), 4(H2 O)'
_chemical_formula_structural        '[Ni(H2O)6NH4(H2O)2]2V10O28'
_chemical_formula_IUPAC             'Ni2(NH4)2(H2 O)16V10O28'
_chemical_formula_weight               1399.12
_chemical_melting_point                ?
#==============================================================================
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'H'  'H'   0.0000   0.0000 
 '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' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'V'  'V'   0.3005   0.5294 
 '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' 
 
_symmetry_cell_setting            triclinic 
_symmetry_space_group_name_H-M    'P -1'
_symmetry_space_group_name_Hall       '-P 1'
_symmetry_Int_Tables_number            2  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    8.7728(18) 
_cell_length_b                    10.923(2) 
_cell_length_c                    11.114(2) 
_cell_angle_alpha                 65.18(3) 
_cell_angle_beta                  73.12(3) 
_cell_angle_gamma                 70.64(3) 
_cell_volume                      897.6(4) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     7874 
_cell_measurement_theta_min       3.44 
_cell_measurement_theta_max       27.46 
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'yellow' 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.588 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              692 
_exptl_absorpt_coefficient_mu     3.636 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.471 
_exptl_absorpt_correction_T_max   0.483 
_exptl_absorpt_process_details    '(ABSCOR; Higashi, 1995)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku RAXIS-RAPID' 
_diffrn_measurement_method        \w 
_diffrn_detector_area_resol_mean  10.00 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         no
_diffrn_reflns_number             8845 
_diffrn_reflns_av_R_equivalents   0.0205 
_diffrn_reflns_av_sigmaI/netI     0.0267 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.44 
_diffrn_reflns_theta_max          27.47 
_reflns_number_total              4056 
_reflns_number_gt                 3602 
_reflns_threshold_expression      I>2\s(I) 
 
_computing_data_collection        'PROCESS-AUTO (Rigaku, 1998)' 
_computing_cell_refinement        'PROCESS-AUTO (Rigaku, 2002)' 
_computing_data_reduction         'CrystalStructure(Rigaku/MSC, 2004)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXL-97 (Sheldrick, 1997)' 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+1.7228P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4056 
_refine_ls_number_parameters      262 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0293 
_refine_ls_R_factor_gt            0.0239 
_refine_ls_wR_factor_ref          0.0598 
_refine_ls_wR_factor_gt           0.0536 
_refine_ls_goodness_of_fit_ref    1.085 
_refine_ls_restrained_S_all       1.085 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
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 
Ni Ni 0.77935(4) 0.73559(3) 0.78156(3) 0.00754(8) Uani 1 1 d . . . 
V1 V 0.69104(5) 0.73612(4) 0.23549(4) 0.00725(9) Uani 1 1 d . . . 
V2 V 0.38279(5) 0.77454(4) 0.44976(4) 0.00630(9) Uani 1 1 d . . . 
V3 V 0.36396(5) 0.71898(4) 0.20208(4) 0.00716(9) Uani 1 1 d . . . 
V4 V 0.32299(5) 0.49313(4) 0.48397(4) 0.00576(9) Uani 1 1 d . . . 
V5 V 0.35210(5) 0.54994(4) 0.72996(4) 0.00609(9) Uani 1 1 d . . . 
O1 O 0.8279(2) 0.82194(19) 0.14635(18) 0.0116(4) Uani 1 1 d . . . 
O2 O 0.2878(2) 0.88984(18) 0.51839(18) 0.0099(3) Uani 1 1 d . . . 
O3 O 0.2513(2) 0.79399(19) 0.08874(18) 0.0118(4) Uani 1 1 d . . . 
O4 O 0.2035(2) 0.38655(18) 0.59565(17) 0.0085(3) Uani 1 1 d . . . 
O5 O 0.2202(2) 0.42913(17) 0.80454(17) 0.0076(3) Uani 1 1 d . . . 
O6 O 0.4792(2) 0.35668(17) 0.41068(17) 0.0067(3) Uani 1 1 d . . . 
O7 O 0.2524(2) 0.66600(18) 0.79654(18) 0.0097(3) Uani 1 1 d . . . 
O8 O 0.5082(2) 0.44277(17) 0.83646(17) 0.0077(3) Uani 1 1 d . . . 
O9 O 0.5624(2) 0.83814(17) 0.34111(17) 0.0076(3) Uani 1 1 d . . . 
O10 O 0.5403(2) 0.79892(18) 0.12541(17) 0.0088(3) Uani 1 1 d . . . 
O11 O 0.2762(2) 0.82728(17) 0.31027(17) 0.0082(3) Uani 1 1 d . . . 
O12 O 0.2309(2) 0.58745(18) 0.34623(17) 0.0077(3) Uani 1 1 d . . . 
O13 O 0.4863(2) 0.40223(17) 0.62168(16) 0.0065(3) Uani 1 1 d . . . 
O14 O 0.2559(2) 0.63212(17) 0.56256(17) 0.0065(3) Uani 1 1 d . . . 
O15 O 0.9447(3) 0.8545(2) 0.6688(2) 0.0228(4) Uani 1 1 d . . . 
O16 O 0.6622(2) 0.81476(19) 0.61938(18) 0.0121(4) Uani 1 1 d . . . 
O17 O 0.9093(2) 0.5669(2) 0.7265(2) 0.0192(4) Uani 1 1 d . . . 
O18 O 0.5903(2) 0.63802(18) 0.89135(17) 0.0102(3) Uani 1 1 d . . . 
O19 O 0.9122(2) 0.6542(2) 0.93409(18) 0.0144(4) Uani 1 1 d . . . 
O20 O 0.6350(2) 0.89580(18) 0.85052(18) 0.0111(4) Uani 1 1 d . . . 
O21 O -0.0096(2) 0.9454(2) 0.87664(19) 0.0167(4) Uani 1 1 d . . . 
O22 O 0.9237(2) 0.8325(2) 0.3987(2) 0.0156(4) Uani 1 1 d . . . 
N N 0.3278(3) 0.9151(2) 0.7615(2) 0.0112(4) Uani 1 1 d . . . 
H15A H 0.9685 0.8916 0.7168 0.050 Uiso 1 1 d . . . 
H15B H 1.0487 0.8167 0.6261 0.050 Uiso 1 1 d . . . 
H16A H 0.7339 0.8371 0.5421 0.050 Uiso 1 1 d . . . 
H16B H 0.6107 0.7563 0.6146 0.050 Uiso 1 1 d . . . 
H17A H 0.8746 0.5193 0.6981 0.050 Uiso 1 1 d . . . 
H17B H 1.0128 0.5222 0.7384 0.050 Uiso 1 1 d . . . 
H18A H 0.5579 0.6109 0.9756 0.050 Uiso 1 1 d . . . 
H18B H 0.5825 0.5766 0.8655 0.050 Uiso 1 1 d . . . 
H19A H 0.8731 0.6268 1.0198 0.050 Uiso 1 1 d . . . 
H19B H 1.0085 0.6662 0.9084 0.050 Uiso 1 1 d . . . 
H20A H 0.6063 0.8735 0.9323 0.050 Uiso 1 1 d . . . 
H20B H 0.6561 0.9732 0.8074 0.050 Uiso 1 1 d . . . 
H21A H -0.0576 1.0296 0.8712 0.050 Uiso 1 1 d . . . 
H21B H -0.0455 0.9007 0.9577 0.050 Uiso 1 1 d . . . 
H22A H 1.0249 0.8305 0.3806 0.050 Uiso 1 1 d . . . 
H22B H 0.9294 0.7555 0.3794 0.050 Uiso 1 1 d . . . 
H23A H 0.3216 0.9019 0.6803 0.050 Uiso 1 1 d . . . 
H23B H 0.2190 0.9262 0.8164 0.050 Uiso 1 1 d . . . 
H23C H 0.4130 0.8364 0.8055 0.050 Uiso 1 1 d . . . 
H23D H 0.3681 0.9921 0.7208 0.050 Uiso 1 1 d . . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Ni 0.00774(15) 0.00808(15) 0.00719(15) -0.00314(12) -0.00112(11) -0.00203(12) 
V1 0.0087(2) 0.00641(19) 0.00648(19) -0.00194(16) -0.00033(15) -0.00295(15) 
V2 0.00814(19) 0.00496(19) 0.00538(19) -0.00206(16) -0.00092(15) -0.00100(15) 
V3 0.0090(2) 0.00638(19) 0.00564(19) -0.00178(16) -0.00227(15) -0.00099(15) 
V4 0.00600(19) 0.00594(19) 0.00592(19) -0.00244(16) -0.00110(15) -0.00169(15) 
V5 0.00729(19) 0.00537(19) 0.00574(19) -0.00238(16) -0.00086(15) -0.00144(15) 
O1 0.0141(9) 0.0122(9) 0.0091(8) -0.0047(7) 0.0019(7) -0.0065(7) 
O2 0.0122(9) 0.0079(8) 0.0094(8) -0.0040(7) -0.0025(7) -0.0006(7) 
O3 0.0155(9) 0.0106(9) 0.0100(9) -0.0037(7) -0.0060(7) -0.0008(7) 
O4 0.0085(8) 0.0080(8) 0.0097(8) -0.0033(7) -0.0019(7) -0.0024(7) 
O5 0.0094(8) 0.0079(8) 0.0056(8) -0.0025(7) 0.0005(6) -0.0036(7) 
O6 0.0074(8) 0.0052(8) 0.0078(8) -0.0026(7) -0.0023(6) -0.0006(6) 
O7 0.0106(8) 0.0087(8) 0.0115(9) -0.0044(7) -0.0026(7) -0.0027(7) 
O8 0.0100(8) 0.0076(8) 0.0064(8) -0.0034(7) -0.0015(6) -0.0023(7) 
O9 0.0098(8) 0.0065(8) 0.0058(8) -0.0019(7) 0.0003(6) -0.0029(7) 
O10 0.0108(8) 0.0071(8) 0.0080(8) -0.0027(7) -0.0017(7) -0.0015(7) 
O11 0.0087(8) 0.0070(8) 0.0073(8) -0.0015(7) -0.0020(7) -0.0007(7) 
O12 0.0069(8) 0.0085(8) 0.0084(8) -0.0040(7) -0.0017(6) -0.0012(6) 
O13 0.0076(8) 0.0058(8) 0.0061(8) -0.0021(7) -0.0013(6) -0.0014(6) 
O14 0.0068(8) 0.0060(8) 0.0068(8) -0.0018(7) -0.0023(6) -0.0012(6) 
O15 0.0177(10) 0.0261(11) 0.0231(11) -0.0054(9) -0.0038(8) -0.0077(9) 
O16 0.0141(9) 0.0130(9) 0.0104(9) -0.0030(7) -0.0034(7) -0.0053(7) 
O17 0.0120(9) 0.0201(10) 0.0352(12) -0.0202(10) -0.0086(8) 0.0016(8) 
O18 0.0140(9) 0.0100(8) 0.0084(8) -0.0031(7) -0.0012(7) -0.0059(7) 
O19 0.0106(9) 0.0225(10) 0.0068(8) -0.0022(8) -0.0011(7) -0.0042(8) 
O20 0.0160(9) 0.0079(8) 0.0095(9) -0.0027(7) -0.0033(7) -0.0028(7) 
O21 0.0153(10) 0.0141(9) 0.0146(9) -0.0013(8) 0.0008(8) -0.0040(8) 
O22 0.0133(9) 0.0176(10) 0.0177(10) -0.0090(8) -0.0003(8) -0.0045(8) 
N 0.0137(10) 0.0081(10) 0.0143(11) -0.0041(9) -0.0048(9) -0.0038(8) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Ni O15 2.047(2) . y 
Ni O19 2.054(2) . y 
Ni O17 2.054(2) . y 
Ni O16 2.057(2) . y 
Ni O18 2.0688(19) . y 
Ni O20 2.0848(19) . y 
V1 O1 1.6054(19) . ? 
V1 O10 1.8303(19) . ? 
V1 O9 1.8407(18) . ? 
V1 O5 1.8982(18) 2_666 ? 
V1 O4 2.061(2) 2_666 ? 
V1 O13 2.3093(19) 2_666 ? 
V1 V4 3.0713(14) 2_666 ? 
V1 V3 3.0725(8) . ? 
V1 V2 3.0832(13) . ? 
V2 O2 1.6136(18) . ? 
V2 O9 1.8276(18) . ? 
V2 O11 1.8291(18) . ? 
V2 O14 1.9825(19) . ? 
V2 O6 1.9997(19) 2_666 ? 
V2 O13 2.2282(18) 2_666 ? 
V2 V5 3.0537(14) . ? 
V2 V3 3.1155(8) . ? 
V3 O3 1.5985(19) . ? 
V3 O10 1.8404(19) . ? 
V3 O11 1.8682(18) . ? 
V3 O8 1.8987(18) 2_666 ? 
V3 O12 2.0214(19) . ? 
V3 O13 2.3410(19) 2_666 ? 
V3 V4 3.0782(14) . ? 
V4 O4 1.6840(19) . ? 
V4 O12 1.7027(19) . ? 
V4 O14 1.9069(17) . ? 
V4 O6 1.9442(18) . ? 
V4 O13 2.1057(19) . ? 
V4 O13 2.1180(18) 2_666 ? 
V4 V1 3.0713(14) 2_666 ? 
V5 O7 1.6112(18) . ? 
V5 O5 1.8179(18) . ? 
V5 O8 1.8337(19) . ? 
V5 O14 1.9965(18) . ? 
V5 O6 1.9979(19) 2_666 ? 
V5 O13 2.2328(18) . ? 
O4 V1 2.061(2) 2_666 ? 
O5 V1 1.8982(18) 2_666 ? 
O6 V5 1.9979(19) 2_666 ? 
O6 V2 1.9997(19) 2_666 ? 
O8 V3 1.8987(18) 2_666 ? 
O13 V4 2.1180(18) 2_666 ? 
O13 V2 2.2282(18) 2_666 ? 
O13 V1 2.3093(19) 2_666 ? 
O13 V3 2.3410(19) 2_666 ? 
O15 H15A 0.8909 . ? 
O15 H15B 0.9442 . ? 
O16 H16A 0.8974 . ? 
O16 H16B 0.9209 . ? 
O17 H17A 0.8725 . ? 
O17 H17B 0.8954 . ? 
O18 H18A 0.8448 . ? 
O18 H18B 0.8609 . ? 
O19 H19A 0.8680 . ? 
O19 H19B 0.8453 . ? 
O20 H20A 0.8190 . ? 
O20 H20B 0.8313 . ? 
O21 H21A 0.8592 . ? 
O21 H21B 0.8469 . ? 
O22 H22A 0.8460 . ? 
O22 H22B 0.9345 . ? 
N H23A 0.9903 . y 
N H23B 0.9723 . y 
N H23C 0.9850 . y 
N H23D 0.9065 . y 
 
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_3 
 _geom_angle_publ_flag 
O15 Ni O19 87.70(8) . . y 
O15 Ni O17 95.55(9) . . y 
O19 Ni O17 87.93(8) . . y 
O15 Ni O16 89.45(8) . . y 
O19 Ni O16 175.84(7) . . y 
O17 Ni O16 89.33(8) . . y
O15 Ni O18 172.97(8) . . y 
O19 Ni O18 96.18(8) . . y
O17 Ni O18 90.46(8) . . y 
O16 Ni O18 86.97(8) . . y 
O15 Ni O20 89.29(8) . . y 
O19 Ni O20 91.17(8) . . y 
O17 Ni O20 175.04(8) . . y 
O16 Ni O20 91.83(8) . . y
O18 Ni O20 84.79(7) . . y 
O1 V1 O10 103.45(9) . . ? 
O1 V1 O9 102.66(9) . . ? 
O10 V1 O9 93.55(8) . . ? 
O1 V1 O5 101.28(9) . 2_666 ? 
O10 V1 O5 91.02(8) . 2_666 ? 
O9 V1 O5 153.82(8) . 2_666 ? 
O1 V1 O4 99.85(9) . 2_666 ? 
O10 V1 O4 156.59(8) . 2_666 ? 
O9 V1 O4 83.54(8) . 2_666 ? 
O5 V1 O4 82.11(8) 2_666 2_666 ? 
O1 V1 O13 174.03(8) . 2_666 ? 
O10 V1 O13 82.34(7) . 2_666 ? 
O9 V1 O13 78.15(7) . 2_666 ? 
O5 V1 O13 76.95(7) 2_666 2_666 ? 
O4 V1 O13 74.31(7) 2_666 2_666 ? 
O1 V1 V4 130.90(7) . 2_666 ? 
O10 V1 V4 125.56(6) . 2_666 ? 
O9 V1 V4 79.19(6) . 2_666 ? 
O5 V1 V4 77.22(6) 2_666 2_666 ? 
O4 V1 V4 31.06(5) 2_666 2_666 ? 
O13 V1 V4 43.25(5) 2_666 2_666 ? 
O1 V1 V3 136.72(7) . . ? 
O10 V1 V3 33.28(6) . . ? 
O9 V1 V3 85.12(6) . . ? 
O5 V1 V3 84.68(6) 2_666 . ? 
O4 V1 V3 123.40(6) 2_666 . ? 
O13 V1 V3 49.09(5) 2_666 . ? 
V4 V1 V3 92.34(4) 2_666 . ? 
O1 V1 V2 135.24(7) . . ? 
O10 V1 V2 83.20(6) . . ? 
O9 V1 V2 32.67(5) . . ? 
O5 V1 V2 123.04(6) 2_666 . ? 
O4 V1 V2 81.94(6) 2_666 . ? 
O13 V1 V2 46.10(5) 2_666 . ? 
V4 V1 V2 61.99(3) 2_666 . ? 
V3 V1 V2 60.81(2) . . ? 
O2 V2 O9 103.10(9) . . ? 
O2 V2 O11 103.60(9) . . ? 
O9 V2 O11 94.15(8) . . ? 
O2 V2 O14 98.91(8) . . ? 
O9 V2 O14 155.58(7) . . ? 
O11 V2 O14 90.83(8) . . ? 
O2 V2 O6 98.49(8) . 2_666 ? 
O9 V2 O6 89.49(8) . 2_666 ? 
O11 V2 O6 156.15(7) . 2_666 ? 
O14 V2 O6 76.82(7) . 2_666 ? 
O2 V2 O13 173.59(8) . 2_666 ? 
O9 V2 O13 80.61(7) . 2_666 ? 
O11 V2 O13 81.17(7) . 2_666 ? 
O14 V2 O13 76.56(7) . 2_666 ? 
O6 V2 O13 76.17(7) 2_666 2_666 ? 
O2 V2 V5 88.57(7) . . ? 
O9 V2 V5 129.65(6) . . ? 
O11 V2 V5 130.87(6) . . ? 
O14 V2 V5 40.04(5) . . ? 
O6 V2 V5 40.17(5) 2_666 . ? 
O13 V2 V5 85.05(5) 2_666 . ? 
O2 V2 V1 135.89(7) . . ? 
O9 V2 V1 32.94(5) . . ? 
O11 V2 V1 82.93(6) . . ? 
O14 V2 V1 124.85(6) . . ? 
O6 V2 V1 87.51(6) 2_666 . ? 
O13 V2 V1 48.31(5) 2_666 . ? 
V5 V2 V1 120.23(4) . . ? 
O2 V2 V3 136.51(7) . . ? 
O9 V2 V3 84.05(6) . . ? 
O11 V2 V3 32.97(5) . . ? 
O14 V2 V3 87.27(6) . . ? 
O6 V2 V3 124.69(5) 2_666 . ? 
O13 V2 V3 48.55(5) 2_666 . ? 
V5 V2 V3 119.90(2) . . ? 
V1 V2 V3 59.42(2) . . ? 
O3 V3 O10 103.42(9) . . ? 
O3 V3 O11 102.69(9) . . ? 
O10 V3 O11 90.86(8) . . ? 
O3 V3 O8 102.04(9) . 2_666 ? 
O10 V3 O8 90.32(8) . 2_666 ? 
O11 V3 O8 154.24(8) . 2_666 ? 
O3 V3 O12 100.88(9) . . ? 
O10 V3 O12 155.68(8) . . ? 
O11 V3 O12 84.84(7) . . ? 
O8 V3 O12 83.57(8) 2_666 . ? 
O3 V3 O13 175.32(8) . 2_666 ? 
O10 V3 O13 81.25(7) . 2_666 ? 
O11 V3 O13 77.38(7) . 2_666 ? 
O8 V3 O13 77.38(7) 2_666 2_666 ? 
O12 V3 O13 74.45(7) . 2_666 ? 
O3 V3 V1 136.47(7) . . ? 
O10 V3 V1 33.07(6) . . ? 
O11 V3 V1 82.66(6) . . ? 
O8 V3 V1 84.38(6) 2_666 . ? 
O12 V3 V1 122.65(6) . . ? 
O13 V3 V1 48.21(5) 2_666 . ? 
O3 V3 V4 131.92(7) . . ? 
O10 V3 V4 124.66(6) . . ? 
O11 V3 V4 78.98(6) . . ? 
O8 V3 V4 79.23(6) 2_666 . ? 
O12 V3 V4 31.05(5) . . ? 
O13 V3 V4 43.41(5) 2_666 . ? 
V1 V3 V4 91.61(4) . . ? 
O3 V3 V2 134.85(7) . . ? 
O10 V3 V2 82.12(6) . . ? 
O11 V3 V2 32.20(6) . . ? 
O8 V3 V2 122.89(6) 2_666 . ? 
O12 V3 V2 81.57(5) . . ? 
O13 V3 V2 45.51(4) 2_666 . ? 
V1 V3 V2 59.77(3) . . ? 
V4 V3 V2 60.85(2) . . ? 
O4 V4 O12 107.01(9) . . ? 
O4 V4 O14 98.62(8) . . ? 
O12 V4 O14 97.91(8) . . ? 
O4 V4 O6 96.32(8) . . ? 
O12 V4 O6 95.91(8) . . ? 
O14 V4 O6 155.69(7) . . ? 
O4 V4 O13 87.89(8) . . ? 
O12 V4 O13 164.99(8) . . ? 
O14 V4 O13 81.20(7) . . ? 
O6 V4 O13 80.30(7) . . ? 
O4 V4 O13 165.69(8) . 2_666 ? 
O12 V4 O13 87.17(8) . 2_666 ? 
O14 V4 O13 80.87(7) . 2_666 ? 
O6 V4 O13 79.93(7) . 2_666 ? 
O13 V4 O13 77.89(8) . 2_666 ? 
O4 V4 V1 39.17(6) . 2_666 ? 
O12 V4 V1 146.16(6) . 2_666 ? 
O14 V4 V1 90.73(6) . 2_666 ? 
O6 V4 V1 88.83(6) . 2_666 ? 
O13 V4 V1 48.72(5) . 2_666 ? 
O13 V4 V1 126.59(6) 2_666 2_666 ? 
O4 V4 V3 144.76(7) . . ? 
O12 V4 V3 37.75(6) . . ? 
O14 V4 V3 89.69(6) . . ? 
O6 V4 V3 89.08(6) . . ? 
O13 V4 V3 127.31(5) . . ? 
O13 V4 V3 49.43(5) 2_666 . ? 
V1 V4 V3 175.832(18) 2_666 . ? 
O7 V5 O5 101.40(9) . . ? 
O7 V5 O8 102.33(9) . . ? 
O5 V5 O8 95.86(8) . . ? 
O7 V5 O14 99.59(9) . . ? 
O5 V5 O14 89.38(8) . . ? 
O8 V5 O14 155.94(7) . . ? 
O7 V5 O6 101.32(8) . 2_666 ? 
O5 V5 O6 154.95(7) . 2_666 ? 
O8 V5 O6 89.48(8) . 2_666 ? 
O14 V5 O6 76.54(7) . 2_666 ? 
O7 V5 O13 175.39(8) . . ? 
O5 V5 O13 80.54(7) . . ? 
O8 V5 O13 81.54(7) . . ? 
O14 V5 O13 76.18(7) . . ? 
O6 V5 O13 76.05(7) 2_666 . ? 
O7 V5 V2 90.87(7) . . ? 
O5 V5 V2 129.08(6) . . ? 
O8 V5 V2 129.69(6) . . ? 
O14 V5 V2 39.71(5) . . ? 
O6 V5 V2 40.21(5) 2_666 . ? 
O13 V5 V2 84.69(5) . . ? 
V4 O4 V1 109.77(9) . 2_666 ? 
V5 O5 V1 114.28(9) . 2_666 ? 
V4 O6 V5 107.54(8) . 2_666 ? 
V4 O6 V2 106.95(8) . 2_666 ? 
V5 O6 V2 99.62(8) 2_666 2_666 ? 
V5 O8 V3 113.84(9) . 2_666 ? 
V2 O9 V1 114.39(9) . . ? 
V1 O10 V3 113.65(10) . . ? 
V2 O11 V3 114.83(9) . . ? 
V4 O12 V3 111.20(9) . . ? 
V4 O13 V4 102.11(8) . 2_666 ? 
V4 O13 V2 93.95(7) . 2_666 ? 
V4 O13 V2 92.37(7) 2_666 2_666 ? 
V4 O13 V5 92.68(7) . . ? 
V4 O13 V5 93.89(7) 2_666 . ? 
V2 O13 V5 169.74(9) 2_666 . ? 
V4 O13 V1 88.03(7) . 2_666 ? 
V4 O13 V1 169.77(9) 2_666 2_666 ? 
V2 O13 V1 85.59(6) 2_666 2_666 ? 
V5 O13 V1 86.82(6) . 2_666 ? 
V4 O13 V3 170.72(8) . 2_666 ? 
V4 O13 V3 87.16(7) 2_666 2_666 ? 
V2 O13 V3 85.94(6) 2_666 2_666 ? 
V5 O13 V3 86.25(6) . 2_666 ? 
V1 O13 V3 82.70(6) 2_666 2_666 ? 
V4 O14 V2 107.50(8) . . ? 
V4 O14 V5 107.08(8) . . ? 
V2 O14 V5 100.25(8) . . ? 
Ni O15 H15A 111.6 . . ? 
Ni O15 H15B 121.2 . . ? 
H15A O15 H15B 103.5 . . ? 
Ni O16 H16A 110.3 . . ? 
Ni O16 H16B 115.4 . . ? 
H16A O16 H16B 106.6 . . ? 
Ni O17 H17A 128.7 . . ? 
Ni O17 H17B 123.7 . . ? 
H17A O17 H17B 107.2 . . ? 
Ni O18 H18A 127.8 . . ? 
Ni O18 H18B 115.6 . . ? 
H18A O18 H18B 106.3 . . ? 
Ni O19 H19A 126.2 . . ? 
Ni O19 H19B 114.0 . . ? 
H19A O19 H19B 118.4 . . ? 
Ni O20 H20A 115.8 . . ? 
Ni O20 H20B 116.3 . . ? 
H20A O20 H20B 117.9 . . ? 
H21A O21 H21B 101.4 . . ? 
H22A O22 H22B 99.3 . . ? 
H23A N H23B 109.1 . . ? 
H23A N H23C 107.0 . . y 
H23B N H23C 115.7 . . y 
H23A N H23D 99.1 . . y
H23B N H23D 115.7 . . y 
H23C N H23D 108.6 . . y 
 
_diffrn_measured_fraction_theta_max    0.987 
_diffrn_reflns_theta_full              27.47 
_diffrn_measured_fraction_theta_full   0.987 
_refine_diff_density_max    0.473 
_refine_diff_density_min   -0.432 
_refine_diff_density_rms    0.105 
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
 O15 H15A O21 . . 1_655 3.035(3) 0.891 2.166 165.0 y    
 O15 H15B O2 . . 1_655 3.050(3) 0.944 2.306 135.3 y 
 O15 H15B O14 . . 1_655 3.300(3) 0.944 2.426 153.8 y
 O16 H16A O22 . . . 2.819(3) 0.897 1.947 163.9 y
 O16 H16B O6 . . 2_666 2.731(2) 0.920 1.814 174.5 y
 O17 H17A O12 . . 2_666 2.847((3) 0.872 1.980 172.0 y
 O17 H17B O5 . . 1_655 2.830(2) 0.895 1.951 166.9 y
 O17 H17B O4 . . 1_655 3.083(6) 0.895 2.510 122.4 y
 O18 H18A O8 . . 2_667 2.726(1) 0.846 1.881 176.8 y
 O18 H18B O8 . . .  2.794(3) 0.861 1.954 165.0 y
 O19 H19A O5 . . 2_667 2.671(3) 0.868 1.805 176.4 y
 O19 H19B O7 . . 1_655 2.951(3) 0.845 2.140 160.5 y
 O20 H20A O10 . . 1_556 2.746(3) 0.820 1.931 173.0 y 
 O21 H21A O3 . . 2_576 3.030(3) 0.858  2.215 158.6  y
 O21 H21B O1 . . 1_456 2.869(3) 0.847  2.034 169.0  y
 O22 H22A O11 . . 1_655 2.948(3) 0.846 2.108 172.5 y
 O22 H22B O4 . . 2_666 2.928(3) 0.934 2.120 144.2 y
 N H23A O2 . . . 2.957(3) 0.991 1.969 174.1 y
 N H23B O21 . . . 2.835(3) 0.975 1.891 162.1 y
 N H23C O18 . . . 3.195(3) 0.987 2.217 170.2 y
 N H23C O20 . . . 3.044(3) 0.987 2.478 116.1 y
 N H23D O9 . . 2_676 2.828(3) 0.907 1.928 171.3 y