# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Dr Shuxia Liu'
_publ_contact_author_address     
;
Chemistry Department
Institute of Polyoxometalate Chemistry Department of Chemistry Northeast
Normal
Institute of Polyoxometalate Chemis
ChangChun
CHINA
;

_publ_contact_author_email       LIUSX@NENU.EDU.CN

_publ_section_title              
;
An organic-inorganic hybrid material constructed from
three-dimensional coordination complex cationic framework and entrained
hexadecavanadate clusters
;
loop_
_publ_author_name
'Shuxia Liu'
'Bo Gao'
'Dehui Li'
'Zhongmin Su'
'Chunyan Sun'
'Linhua Xie'
;
Chundan Zhang
;

data_niv16
_database_code_depnum_ccdc_archive 'CCDC 276944'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H52 Cl N10 Ni2 O44 V16'
_chemical_formula_weight         2464.93

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'
Cl Cl 0.1484 0.1585 '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           tetragonal
_symmetry_space_group_name_H-M   P-4n2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   17.074(2)
_cell_length_b                   17.074(2)
_cell_length_c                   14.606(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4257.8(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4871
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.46

_exptl_crystal_description       octahedron
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.182
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2430
_exptl_absorpt_coefficient_mu    2.220
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         4871
_diffrn_standards_interval_count 12.88
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            36280
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         27.46
_reflns_number_total             4871
_reflns_number_gt                4727
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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^)+(0.0564P)^2^+29.9503P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.59(5)
_refine_ls_number_reflns         4871
_refine_ls_number_parameters     280
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0664
_refine_ls_wR_factor_ref         0.1567
_refine_ls_wR_factor_gt          0.1553
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_restrained_S_all      1.230
_refine_ls_shift/su_max          1.458
_refine_ls_shift/su_mean         0.005

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
V1 V 0.88776(7) 0.12203(7) 0.12782(7) 0.0105(2) Uani 1 1 d . . .
V2 V 0.81542(7) 0.04842(7) -0.08916(10) 0.0152(3) Uani 1 1 d . . .
V3 V 0.81163(7) -0.03217(7) 0.08669(10) 0.0146(3) Uani 1 1 d . . .
V4 V 1.07144(9) 0.06536(9) 0.23017(8) 0.0293(3) Uani 1 1 d . . .
Cl1 Cl 0.0000 0.0000 0.0000 0.0318(8) Uani 1 4 d S . .
Ni1 Ni 0.75467(5) 0.25467(5) 0.2500 0.0086(2) Uani 1 2 d S . .
N1 N 0.6611(4) 0.2223(4) 0.1606(5) 0.0185(14) Uani 1 1 d . . .
N2 N 0.7859(4) 0.3489(4) 0.1598(4) 0.0137(12) Uani 1 1 d . . .
N3 N 0.0000 0.5000 0.0070(16) 0.021(4) Uiso 0.50 2 d SPDU . .
N4 N 0.0000 0.5000 -0.1547(16) 0.027(5) Uiso 0.25 2 d SPD . .
N5 N 0.0000 0.5000 0.151(3) 0.017(8) Uiso 0.25 2 d SPDU . .
C1 C 0.8042(6) 0.3359(5) 0.0734(7) 0.030(2) Uani 1 1 d . . .
H1 H 0.8151 0.2849 0.0552 0.037 Uiso 1 1 calc R . .
C2 C 0.8077(7) 0.3958(5) 0.0077(6) 0.033(2) Uani 1 1 d . . .
H2 H 0.8192 0.3840 -0.0530 0.039 Uiso 1 1 calc R . .
C3 C 0.7944(5) 0.4706(5) 0.0331(6) 0.0192(16) Uani 1 1 d . . .
C4 C 0.7751(6) 0.4847(5) 0.1249(7) 0.028(2) Uani 1 1 d . . .
H4 H 0.7641 0.5353 0.1445 0.034 Uiso 1 1 calc R . .
C5 C 0.7725(6) 0.4232(5) 0.1861(7) 0.0247(18) Uani 1 1 d . . .
H5 H 0.7613 0.4334 0.2472 0.030 Uiso 1 1 calc R . .
C6 C 0.5870(5) 0.2370(6) 0.1833(6) 0.0241(18) Uani 1 1 d . . .
H6 H 0.5771 0.2527 0.2431 0.029 Uiso 1 1 calc R . .
C7 C 0.5246(5) 0.2309(6) 0.1258(7) 0.030(2) Uani 1 1 d . . .
H7 H 0.4743 0.2407 0.1474 0.035 Uiso 1 1 calc R . .
C8 C 0.5360(5) 0.2099(5) 0.0343(7) 0.0244(19) Uani 1 1 d . . .
C9 C 0.6117(5) 0.1875(6) 0.0118(6) 0.0249(19) Uani 1 1 d . . .
H9 H 0.6222 0.1676 -0.0461 0.030 Uiso 1 1 calc R . .
C10 C 0.6712(5) 0.1946(5) 0.0740(6) 0.0206(17) Uani 1 1 d . . .
H10 H 0.7213 0.1796 0.0562 0.025 Uiso 1 1 calc R . .
C11 C 0.0000 0.5000 0.1926(14) 0.009(3) Uiso 0.50 2 d SPDU . .
C12 C -0.0006(11) 0.4326(10) 0.1470(14) 0.029(4) Uiso 0.50 1 d PDU . .
C13 C 0.0002(12) 0.4317(11) 0.0486(15) 0.034(4) Uiso 0.50 1 d PDU . .
C14 C 0.0434(14) 0.5512(14) -0.1992(15) 0.046(5) Uiso 0.50 1 d PD . .
C15 C 0.0000 0.5000 -0.1547(16) 0.027(5) Uiso 0.25 2 d SP . .
C16 C 0.0000 0.5000 -0.0434(18) 0.000(5) Uiso 0.25 2 d SPDU . .
C17 C -0.0056(18) 0.4282(13) 0.007(2) 0.012(5) Uiso 0.25 1 d PDU . .
C18 C -0.0047(14) 0.4322(13) 0.1052(19) 0.005(4) Uiso 0.25 1 d PDU . .
O1 O 0.8295(3) 0.1823(3) 0.1817(3) 0.0133(9) Uani 1 1 d . . .
O2 O 0.9910(3) 0.1298(3) 0.1819(4) 0.0146(11) Uani 1 1 d . . .
O3 O 0.9411(3) 0.1857(3) 0.0385(4) 0.0178(11) Uani 1 1 d . . .
O4 O 0.8711(3) 0.0199(3) 0.1816(4) 0.0169(11) Uani 1 1 d . . .
O5 O 0.8203(3) 0.0731(3) 0.0367(4) 0.0159(11) Uani 1 1 d . . .
O6 O 0.8798(3) 0.1329(3) -0.1227(3) 0.0216(11) Uani 1 1 d . . .
O7 O 0.7289(4) 0.0690(4) -0.1254(5) 0.0280(14) Uani 1 1 d . . .
O8 O 0.7240(3) -0.0429(4) 0.1224(4) 0.0255(13) Uani 1 1 d . . .
O9 O 1.1134(4) 0.1045(4) 0.3173(3) 0.0377(15) Uani 1 1 d . . .
O10 O 1.0000 0.0000 0.2832(4) 0.0232(14) Uani 1 2 d S . .
O1W O 1.0000 0.0000 0.473(3) 0.147(16) Uiso 0.50 2 d SP . .
O2W O 0.946(2) 0.073(2) 0.483(2) 0.144(11) Uiso 0.50 1 d P . .
O3W O 0.748(3) 0.731(3) 0.193(2) 0.22(2) Uiso 0.50 1 d P . .
O4W O 0.6753(17) 0.8247(17) 0.2500 0.111(12) Uiso 0.50 2 d SP . .

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
V1 0.0100(5) 0.0086(5) 0.0130(4) -0.0009(4) 0.0006(4) 0.0030(4)
V2 0.0120(6) 0.0161(6) 0.0174(6) 0.0002(5) -0.0017(5) -0.0004(4)
V3 0.0136(6) 0.0153(6) 0.0148(6) 0.0006(5) 0.0004(5) -0.0003(5)
V4 0.0364(9) 0.0330(8) 0.0185(5) -0.0085(6) -0.0112(6) 0.0196(6)
Cl1 0.0237(11) 0.0237(11) 0.048(2) 0.000 0.000 0.000
Ni1 0.0087(3) 0.0087(3) 0.0083(4) -0.0001(3) 0.0001(3) 0.0004(4)
N1 0.015(3) 0.018(3) 0.022(4) 0.002(3) 0.003(3) -0.001(2)
N2 0.021(3) 0.012(3) 0.008(3) 0.005(2) 0.005(2) 0.003(2)
C1 0.045(5) 0.017(4) 0.030(5) 0.005(4) 0.011(4) -0.001(4)
C2 0.064(7) 0.022(4) 0.012(4) 0.014(3) -0.005(4) 0.001(4)
C3 0.024(4) 0.019(4) 0.015(4) 0.002(3) -0.004(3) -0.001(3)
C4 0.045(5) 0.007(3) 0.033(5) 0.008(3) 0.002(4) 0.003(3)
C5 0.029(4) 0.023(4) 0.022(4) -0.005(3) 0.008(3) -0.005(3)
C6 0.015(4) 0.042(5) 0.016(4) -0.007(4) -0.001(3) -0.003(4)
C7 0.015(4) 0.041(5) 0.032(5) -0.020(4) 0.003(4) 0.001(4)
C8 0.023(4) 0.023(4) 0.027(5) -0.003(3) -0.012(3) 0.001(3)
C9 0.018(4) 0.039(5) 0.018(4) -0.013(4) 0.004(3) 0.007(4)
C10 0.016(3) 0.032(4) 0.014(4) -0.001(3) 0.003(3) 0.009(3)
O1 0.009(2) 0.018(3) 0.0125(18) -0.0033(19) -0.0008(18) 0.0030(17)
O2 0.011(2) 0.016(3) 0.016(3) 0.000(2) 0.0001(19) -0.0023(19)
O3 0.015(3) 0.019(3) 0.019(3) 0.001(2) 0.002(2) 0.003(2)
O4 0.021(3) 0.013(2) 0.017(3) 0.002(2) 0.002(2) 0.006(2)
O5 0.016(3) 0.022(3) 0.009(2) -0.002(2) -0.001(2) 0.007(2)
O6 0.016(3) 0.025(3) 0.024(2) 0.008(2) 0.001(2) -0.003(2)
O7 0.019(3) 0.026(3) 0.039(4) 0.008(3) -0.008(3) 0.000(2)
O8 0.015(3) 0.032(3) 0.029(3) 0.004(3) 0.008(2) -0.005(2)
O9 0.043(4) 0.049(4) 0.021(2) -0.006(3) -0.012(3) 0.008(3)
O10 0.018(4) 0.030(5) 0.021(3) 0.000 0.000 0.002(3)

_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
V1 O1 1.633(4) . ?
V1 O3 1.928(6) . ?
V1 O4 1.933(6) . ?
V1 O2 1.937(5) . ?
V1 O5 1.948(5) . ?
V1 V3 2.9969(18) . ?
V1 V2 2.9973(18) 3_665 ?
V2 O7 1.608(6) . ?
V2 O6 1.878(6) . ?
V2 O5 1.888(6) . ?
V2 O2 1.915(5) 4_645 ?
V2 O3 1.976(6) 4_645 ?
V2 V3 2.9145(17) . ?
V2 V4 2.922(2) 4_645 ?
V2 V1 2.9973(18) 4_645 ?
V3 O8 1.595(5) . ?
V3 O6 1.853(6) 4_645 ?
V3 O3 1.884(6) 4_645 ?
V3 O4 1.935(6) . ?
V3 O5 1.945(6) . ?
V3 V4 2.949(2) 2_755 ?
V4 O9 1.607(5) . ?
V4 O10 1.826(3) . ?
V4 O4 1.893(6) 2_755 ?
V4 O2 1.895(6) . ?
V4 O6 2.107(5) 3_665 ?
V4 V2 2.922(2) 3_665 ?
V4 V3 2.949(2) 2_755 ?
Ni1 O1 2.038(4) . ?
Ni1 O1 2.038(4) 7_545 ?
Ni1 N1 2.137(7) . ?
Ni1 N1 2.137(7) 7_545 ?
Ni1 N2 2.146(6) 7_545 ?
Ni1 N2 2.146(6) . ?
N1 C6 1.331(11) . ?
N1 C10 1.361(11) . ?
N2 C1 1.319(12) . ?
N2 C5 1.346(10) . ?
N3 C16 0.74(3) . ?
N3 C17 1.23(2) . ?
N3 C17 1.23(2) 2_565 ?
N3 C13 1.31(2) . ?
N3 C13 1.31(2) 2_565 ?
N3 C18 1.85(3) 2_565 ?
N3 C18 1.85(3) . ?
N4 C14 1.32(2) 2_565 ?
N4 C14 1.32(2) . ?
N4 C16 1.63(3) . ?
N5 C11 0.61(4) . ?
N5 C12 1.153(18) . ?
N5 C12 1.153(18) 2_565 ?
N5 C18 1.34(3) . ?
N5 C18 1.34(3) 2_565 ?
N5 C13 1.90(4) . ?
N5 C13 1.90(4) 2_565 ?
C1 C2 1.404(12) . ?
C2 C3 1.349(13) . ?
C3 C4 1.401(13) . ?
C3 C8 1.490(9) 4_655 ?
C4 C5 1.379(12) . ?
C6 C7 1.360(12) . ?
C7 C8 1.397(13) . ?
C8 C9 1.388(12) . ?
C8 C3 1.490(9) 3_565 ?
C9 C10 1.367(12) . ?
C11 C12 1.33(2) . ?
C11 C12 1.33(2) 2_565 ?
C11 C11 1.68(4) 7_455 ?
C11 C18 1.72(3) . ?
C11 C18 1.72(3) 2_565 ?
C12 C18 0.61(2) . ?
C12 C13 1.44(2) . ?
C13 C17 0.62(3) . ?
C13 C18 0.83(3) . ?
C13 C16 1.78(3) . ?
C14 C14 1.50(4) 7_454 ?
C16 C17 1.43(3) . ?
C16 C17 1.43(3) 2_565 ?
C16 C13 1.78(3) 2_565 ?
C17 C18 1.44(3) . ?
O2 V2 1.915(5) 3_665 ?
O3 V3 1.884(6) 3_665 ?
O3 V2 1.976(6) 3_665 ?
O4 V4 1.893(6) 2_755 ?
O6 V3 1.853(6) 3_665 ?
O6 V4 2.107(5) 4_645 ?
O10 V4 1.826(3) 2_755 ?
O1W O1W 0.80(8) 3_666 ?
O1W O2W 1.56(3) 2_755 ?
O1W O2W 1.56(3) . ?
O1W O2W 1.69(3) 3_666 ?
O1W O2W 1.69(3) 4_646 ?
O2W O1W 1.69(3) 3_666 ?
O3W O3W 1.74(7) 8_665 ?

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
O1 V1 O3 105.0(2) . . ?
O1 V1 O4 106.5(2) . . ?
O3 V1 O4 148.6(2) . . ?
O1 V1 O2 108.3(2) . . ?
O3 V1 O2 78.9(2) . . ?
O4 V1 O2 91.71(19) . . ?
O1 V1 O5 103.9(2) . . ?
O3 V1 O5 93.4(2) . . ?
O4 V1 O5 78.7(2) . . ?
O2 V1 O5 147.8(2) . . ?
O1 V1 V3 112.7(2) . . ?
O3 V1 V3 124.40(18) . . ?
O4 V1 V3 39.24(17) . . ?
O2 V1 V3 122.48(17) . . ?
O5 V1 V3 39.63(17) . . ?
O1 V1 V2 115.0(2) . 3_665 ?
O3 V1 V2 40.43(17) . 3_665 ?
O4 V1 V2 122.15(17) . 3_665 ?
O2 V1 V2 38.66(16) . 3_665 ?
O5 V1 V2 124.42(17) . 3_665 ?
V3 V1 V2 132.24(5) . 3_665 ?
O7 V2 O6 106.5(3) . . ?
O7 V2 O5 108.2(3) . . ?
O6 V2 O5 93.3(2) . . ?
O7 V2 O2 109.1(3) . 4_645 ?
O6 V2 O2 85.6(2) . 4_645 ?
O5 V2 O2 141.4(2) . 4_645 ?
O7 V2 O3 108.5(3) . 4_645 ?
O6 V2 O3 144.6(2) . 4_645 ?
O5 V2 O3 80.9(2) . 4_645 ?
O2 V2 O3 78.2(2) 4_645 4_645 ?
O7 V2 V3 111.9(2) . . ?
O6 V2 V3 127.24(16) . . ?
O5 V2 V3 41.24(17) . . ?
O2 V2 V3 113.13(16) 4_645 . ?
O3 V2 V3 39.81(17) 4_645 . ?
O7 V2 V4 112.2(3) . 4_645 ?
O6 V2 V4 45.99(16) . 4_645 ?
O5 V2 V4 128.73(17) . 4_645 ?
O2 V2 V4 39.68(16) 4_645 4_645 ?
O3 V2 V4 113.31(18) 4_645 4_645 ?
V3 V2 V4 134.43(6) . 4_645 ?
O7 V2 V1 117.7(2) . 4_645 ?
O6 V2 V1 116.42(16) . 4_645 ?
O5 V2 V1 111.83(17) . 4_645 ?
O2 V2 V1 39.18(16) 4_645 4_645 ?
O3 V2 V1 39.26(17) 4_645 4_645 ?
V3 V2 V1 75.04(4) . 4_645 ?
V4 V2 V1 75.06(5) 4_645 4_645 ?
O8 V3 O6 107.1(3) . 4_645 ?
O8 V3 O3 108.2(3) . 4_645 ?
O6 V3 O3 93.8(2) 4_645 4_645 ?
O8 V3 O4 108.1(3) . . ?
O6 V3 O4 84.3(2) 4_645 . ?
O3 V3 O4 142.5(2) 4_645 . ?
O8 V3 O5 107.5(3) . . ?
O6 V3 O5 144.8(2) 4_645 . ?
O3 V3 O5 81.8(2) 4_645 . ?
O4 V3 O5 78.7(2) . . ?
O8 V3 V2 111.3(2) . . ?
O6 V3 V2 128.43(16) 4_645 . ?
O3 V3 V2 42.16(17) 4_645 . ?
O4 V3 V2 113.73(17) . . ?
O5 V3 V2 39.79(16) . . ?
O8 V3 V4 112.4(2) . 2_755 ?
O6 V3 V4 45.28(16) 4_645 2_755 ?
O3 V3 V4 128.79(18) 4_645 2_755 ?
O4 V3 V4 39.10(16) . 2_755 ?
O5 V3 V4 113.12(16) . 2_755 ?
V2 V3 V4 134.57(6) . 2_755 ?
O8 V3 V1 116.2(2) . . ?
O6 V3 V1 115.71(17) 4_645 . ?
O3 V3 V1 113.36(18) 4_645 . ?
O4 V3 V1 39.18(16) . . ?
O5 V3 V1 39.70(16) . . ?
V2 V3 V1 75.66(4) . . ?
V4 V3 V1 74.50(5) 2_755 . ?
O9 V4 O10 102.5(3) . . ?
O9 V4 O4 112.7(4) . 2_755 ?
O10 V4 O4 92.0(2) . 2_755 ?
O9 V4 O2 112.1(3) . . ?
O10 V4 O2 91.66(19) . . ?
O4 V4 O2 133.02(18) 2_755 . ?
O9 V4 O6 100.6(3) . 3_665 ?
O10 V4 O6 156.9(2) . 3_665 ?
O4 V4 O6 78.7(2) 2_755 3_665 ?
O2 V4 O6 79.9(2) . 3_665 ?
O9 V4 V2 109.2(3) . 3_665 ?
O10 V4 V2 129.41(13) . 3_665 ?
O4 V4 V2 109.95(18) 2_755 3_665 ?
O2 V4 V2 40.18(16) . 3_665 ?
O6 V4 V2 39.87(16) 3_665 3_665 ?
O9 V4 V3 109.9(3) . 2_755 ?
O10 V4 V3 129.51(13) . 2_755 ?
O4 V4 V3 40.13(18) 2_755 2_755 ?
O2 V4 V3 109.73(17) . 2_755 ?
O6 V4 V3 38.66(16) 3_665 2_755 ?
V2 V4 V3 73.99(5) 3_665 2_755 ?
O1 Ni1 O1 178.3(3) . 7_545 ?
O1 Ni1 N1 90.8(2) . . ?
O1 Ni1 N1 90.5(2) 7_545 . ?
O1 Ni1 N1 90.5(2) . 7_545 ?
O1 Ni1 N1 90.8(2) 7_545 7_545 ?
N1 Ni1 N1 89.2(4) . 7_545 ?
O1 Ni1 N2 88.9(2) . 7_545 ?
O1 Ni1 N2 89.9(2) 7_545 7_545 ?
N1 Ni1 N2 179.4(3) . 7_545 ?
N1 Ni1 N2 90.3(2) 7_545 7_545 ?
O1 Ni1 N2 89.9(2) . . ?
O1 Ni1 N2 88.9(2) 7_545 . ?
N1 Ni1 N2 90.3(2) . . ?
N1 Ni1 N2 179.4(3) 7_545 . ?
N2 Ni1 N2 90.3(4) 7_545 . ?
C6 N1 C10 114.6(7) . . ?
C6 N1 Ni1 120.7(6) . . ?
C10 N1 Ni1 124.3(5) . . ?
C1 N2 C5 118.1(7) . . ?
C1 N2 Ni1 121.4(6) . . ?
C5 N2 Ni1 119.3(5) . . ?
C16 N3 C17 90(2) . . ?
C16 N3 C17 90(2) . 2_565 ?
C17 N3 C17 180(4) . 2_565 ?
C16 N3 C13 117.5(13) . . ?
C17 N3 C13 28.0(15) . . ?
C17 N3 C13 152(3) 2_565 . ?
C16 N3 C13 117.5(13) . 2_565 ?
C17 N3 C13 152(3) . 2_565 ?
C17 N3 C13 28.0(15) 2_565 2_565 ?
C13 N3 C13 125(3) . 2_565 ?
C16 N3 C18 141.0(8) . 2_565 ?
C17 N3 C18 129(3) . 2_565 ?
C17 N3 C18 51.1(17) 2_565 2_565 ?
C13 N3 C18 101.3(19) . 2_565 ?
C13 N3 C18 23.7(12) 2_565 2_565 ?
C16 N3 C18 141.0(8) . . ?
C17 N3 C18 51.1(17) . . ?
C17 N3 C18 129(3) 2_565 . ?
C13 N3 C18 23.7(12) . . ?
C13 N3 C18 101.3(19) 2_565 . ?
C18 N3 C18 77.9(17) 2_565 . ?
C14 N4 C14 121(3) 2_565 . ?
C14 N4 C16 119.6(14) 2_565 . ?
C14 N4 C16 119.6(14) . . ?
C11 N5 C12 93(2) . . ?
C11 N5 C12 93(2) . 2_565 ?
C12 N5 C12 174(5) . 2_565 ?
C11 N5 C18 120(2) . . ?
C12 N5 C18 27.3(12) . . ?
C12 N5 C18 147(4) 2_565 . ?
C11 N5 C18 120(2) . 2_565 ?
C12 N5 C18 147(4) . 2_565 ?
C12 N5 C18 27.3(12) 2_565 2_565 ?
C18 N5 C18 120(4) . 2_565 ?
C11 N5 C13 142.0(10) . . ?
C12 N5 C13 49.2(16) . . ?
C12 N5 C13 125(3) 2_565 . ?
C18 N5 C13 22.4(14) . . ?
C18 N5 C13 98(3) 2_565 . ?
C11 N5 C13 142.0(10) . 2_565 ?
C12 N5 C13 125(3) . 2_565 ?
C12 N5 C13 49.2(16) 2_565 2_565 ?
C18 N5 C13 98(3) . 2_565 ?
C18 N5 C13 22.4(14) 2_565 2_565 ?
C13 N5 C13 75.9(19) . 2_565 ?
N2 C1 C2 122.8(8) . . ?
C3 C2 C1 119.6(9) . . ?
C2 C3 C4 117.8(8) . . ?
C2 C3 C8 122.4(7) . 4_655 ?
C4 C3 C8 119.4(7) . 4_655 ?
C5 C4 C3 119.7(8) . . ?
N2 C5 C4 121.9(8) . . ?
N1 C6 C7 125.2(8) . . ?
C6 C7 C8 120.1(8) . . ?
C9 C8 C7 115.2(8) . . ?
C9 C8 C3 121.9(8) . 3_565 ?
C7 C8 C3 122.7(7) . 3_565 ?
C10 C9 C8 120.7(8) . . ?
N1 C10 C9 123.6(7) . . ?
N5 C11 C12 60.0(12) . . ?
N5 C11 C12 60.0(12) . 2_565 ?
C12 C11 C12 120(2) . 2_565 ?
N5 C11 C11 180.000(9) . 7_455 ?
C12 C11 C11 120.0(12) . 7_455 ?
C12 C11 C11 120.0(12) 2_565 7_455 ?
N5 C11 C18 42.3(10) . . ?
C12 C11 C18 17.9(11) . . ?
C12 C11 C18 102.2(19) 2_565 . ?
C11 C11 C18 137.7(10) 7_455 . ?
N5 C11 C18 42.3(10) . 2_565 ?
C12 C11 C18 102.2(19) . 2_565 ?
C12 C11 C18 17.9(11) 2_565 2_565 ?
C11 C11 C18 137.7(10) 7_455 2_565 ?
C18 C11 C18 85(2) . 2_565 ?
C18 C12 N5 93(4) . . ?
C18 C12 C11 120(3) . . ?
N5 C12 C11 27.2(19) . . ?
C18 C12 C13 7(3) . . ?
N5 C12 C13 93(3) . . ?
C11 C12 C13 120.6(18) . . ?
C17 C13 C18 164(5) . . ?
C17 C13 N3 68(3) . . ?
C18 C13 N3 117(3) . . ?
C17 C13 C12 169(4) . . ?
C18 C13 C12 5(2) . . ?
N3 C13 C12 117.0(19) . . ?
C17 C13 C16 47(3) . . ?
C18 C13 C16 138(3) . . ?
N3 C13 C16 21.5(11) . . ?
C12 C13 C16 138.5(16) . . ?
C17 C13 N5 146(3) . . ?
C18 C13 N5 38(2) . . ?
N3 C13 N5 79.6(15) . . ?
C12 C13 N5 37.4(12) . . ?
C16 C13 N5 101.1(13) . . ?
N4 C14 C14 118.7(14) . 7_454 ?
N3 C16 C17 59.2(16) . . ?
N3 C16 C17 59.2(16) . 2_565 ?
C17 C16 C17 118(3) . 2_565 ?
N3 C16 N4 180.000(6) . . ?
C17 C16 N4 120.8(16) . . ?
C17 C16 N4 120.8(16) 2_565 . ?
N3 C16 C13 41.0(8) . . ?
C17 C16 C13 18.5(13) . . ?
C17 C16 C13 100(2) 2_565 . ?
N4 C16 C13 139.0(8) . . ?
N3 C16 C13 41.0(8) . 2_565 ?
C17 C16 C13 100(2) . 2_565 ?
C17 C16 C13 18.5(13) 2_565 2_565 ?
N4 C16 C13 139.0(8) . 2_565 ?
C13 C16 C13 81.9(17) . 2_565 ?
C13 C17 N3 84(3) . . ?
C13 C17 C16 114(4) . . ?
N3 C17 C16 30.9(15) . . ?
C13 C17 C18 9(3) . . ?
N3 C17 C18 87(2) . . ?
C16 C17 C18 118(2) . . ?
C12 C18 C13 168(5) . . ?
C12 C18 N5 59(3) . . ?
C13 C18 N5 120(3) . . ?
C12 C18 C17 174(4) . . ?
C13 C18 C17 7(2) . . ?
N5 C18 C17 123(3) . . ?
C12 C18 C11 42(3) . . ?
C13 C18 C11 138(3) . . ?
N5 C18 C11 17.8(14) . . ?
C17 C18 C11 140.4(19) . . ?
C12 C18 N3 140(3) . . ?
C13 C18 N3 39(2) . . ?
N5 C18 N3 81(2) . . ?
C17 C18 N3 41.7(12) . . ?
C11 C18 N3 98.8(13) . . ?
V1 O1 Ni1 178.2(4) . . ?
V4 O2 V2 100.1(2) . 3_665 ?
V4 O2 V1 140.4(3) . . ?
V2 O2 V1 102.2(3) 3_665 . ?
V3 O3 V1 141.7(3) 3_665 . ?
V3 O3 V2 98.0(2) 3_665 3_665 ?
V1 O3 V2 100.3(3) . 3_665 ?
V4 O4 V1 140.4(3) 2_755 . ?
V4 O4 V3 100.8(3) 2_755 . ?
V1 O4 V3 101.6(3) . . ?
V2 O5 V3 99.0(3) . . ?
V2 O5 V1 141.9(3) . . ?
V3 O5 V1 100.7(2) . . ?
V3 O6 V2 142.5(3) 3_665 . ?
V3 O6 V4 96.1(2) 3_665 4_645 ?
V2 O6 V4 94.1(2) . 4_645 ?
V4 O10 V4 129.8(4) 2_755 . ?
O1W O1W O2W 85(2) 3_666 2_755 ?
O1W O1W O2W 85(2) 3_666 . ?
O2W O1W O2W 169(4) 2_755 . ?
O1W O1W O2W 67.2(16) 3_666 3_666 ?
O2W O1W O2W 87.9(9) 2_755 3_666 ?
O2W O1W O2W 87.9(9) . 3_666 ?
O1W O1W O2W 67.2(16) 3_666 4_646 ?
O2W O1W O2W 87.9(9) 2_755 4_646 ?
O2W O1W O2W 87.9(9) . 4_646 ?
O2W O1W O2W 134(3) 3_666 4_646 ?
O1W O2W O1W 28(3) . 3_666 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.300
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.161

data_niv16(squeezed)
_database_code_depnum_ccdc_archive 'CCDC 276945'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H52 Cl N10 Ni2 O44 V16'
_chemical_formula_weight         2464.93

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'
Cl Cl 0.1484 0.1585 '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           tetragonal
_symmetry_space_group_name_H-M   P-4n2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   17.074(2)
_cell_length_b                   17.074(2)
_cell_length_c                   14.606(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4257.8(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4871
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.46

_exptl_crystal_description       octahedron
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.182
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2430
_exptl_absorpt_coefficient_mu    2.220
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         4871
_diffrn_standards_interval_count 12.88
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            36276
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         27.46
_reflns_number_total             4870
_reflns_number_gt                4725
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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^)+(0.0725P)^2^+13.6372P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.56(4)
_refine_ls_number_reflns         4870
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1382
_refine_ls_wR_factor_gt          0.1365
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_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
V1 V 0.88775(5) 0.12199(5) 0.12781(5) 0.00985(18) Uani 1 1 d . . .
V2 V 0.81549(5) 0.04844(6) -0.08919(7) 0.0145(2) Uani 1 1 d . . .
V3 V 0.81166(5) -0.03214(5) 0.08662(7) 0.0140(2) Uani 1 1 d . . .
V4 V 1.07144(7) 0.06526(7) 0.23011(6) 0.0285(3) Uani 1 1 d . . .
Cl1 Cl 0.0000 0.0000 0.0000 0.0308(6) Uani 1 4 d S . .
Ni1 Ni 0.75463(4) 0.25463(4) 0.2500 0.00803(18) Uani 1 2 d S . .
N1 N 0.6611(3) 0.2220(3) 0.1607(4) 0.0168(10) Uani 1 1 d . . .
N2 N 0.7864(3) 0.3491(3) 0.1594(3) 0.0129(9) Uani 1 1 d . . .
C1 C 0.8039(5) 0.3357(4) 0.0730(6) 0.0332(18) Uani 1 1 d . . .
H1 H 0.8142 0.2844 0.0551 0.040 Uiso 1 1 calc R . .
C2 C 0.8078(6) 0.3960(4) 0.0056(5) 0.0356(19) Uani 1 1 d . . .
H2 H 0.8193 0.3846 -0.0552 0.043 Uiso 1 1 calc R . .
C3 C 0.7940(4) 0.4707(4) 0.0333(5) 0.0191(13) Uani 1 1 d . . .
C4 C 0.7745(5) 0.4853(3) 0.1249(5) 0.0268(15) Uani 1 1 d . . .
H4 H 0.7630 0.5358 0.1446 0.032 Uiso 1 1 calc R . .
C5 C 0.7729(4) 0.4236(4) 0.1845(5) 0.0228(14) Uani 1 1 d . . .
H5 H 0.7619 0.4338 0.2457 0.027 Uiso 1 1 calc R . .
C6 C 0.5872(4) 0.2359(5) 0.1842(5) 0.0244(14) Uani 1 1 d . . .
H6 H 0.5769 0.2504 0.2444 0.029 Uiso 1 1 calc R . .
C7 C 0.5252(4) 0.2299(5) 0.1249(5) 0.0308(17) Uani 1 1 d . . .
H7 H 0.4748 0.2398 0.1460 0.037 Uiso 1 1 calc R . .
C8 C 0.5363(4) 0.2093(4) 0.0337(5) 0.0228(14) Uani 1 1 d . . .
C9 C 0.6121(4) 0.1881(4) 0.0126(4) 0.0220(14) Uani 1 1 d . . .
H9 H 0.6228 0.1685 -0.0455 0.026 Uiso 1 1 calc R . .
C10 C 0.6711(3) 0.1947(4) 0.0730(4) 0.0167(12) Uani 1 1 d . . .
H10 H 0.7211 0.1801 0.0546 0.020 Uiso 1 1 calc R . .
O1 O 0.8295(2) 0.1824(2) 0.1818(2) 0.0117(7) Uani 1 1 d . . .
O2 O 0.9912(2) 0.1298(2) 0.1820(3) 0.0138(8) Uani 1 1 d . . .
O3 O 0.9411(2) 0.1858(3) 0.0384(3) 0.0171(8) Uani 1 1 d . . .
O4 O 0.8715(3) 0.0199(2) 0.1812(3) 0.0174(9) Uani 1 1 d . . .
O5 O 0.8203(2) 0.0731(2) 0.0367(3) 0.0147(8) Uani 1 1 d . . .
O6 O 0.8795(2) 0.1329(3) -0.1226(2) 0.0206(8) Uani 1 1 d . . .
O7 O 0.7288(3) 0.0690(3) -0.1249(4) 0.0276(11) Uani 1 1 d . . .
O8 O 0.7236(3) -0.0433(3) 0.1224(3) 0.0236(9) Uani 1 1 d . . .
O9 O 1.1131(3) 0.1047(4) 0.3176(3) 0.0376(12) Uani 1 1 d . . .
O10 O 1.0000 0.0000 0.2836(3) 0.0229(11) Uani 1 2 d S . .

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
V1 0.0095(4) 0.0077(4) 0.0123(3) -0.0010(3) 0.0009(3) 0.0029(3)
V2 0.0116(4) 0.0160(5) 0.0160(5) 0.0002(4) -0.0017(4) 0.0001(3)
V3 0.0130(4) 0.0148(4) 0.0144(5) 0.0008(4) 0.0001(4) 0.0004(4)
V4 0.0353(7) 0.0323(7) 0.0180(4) -0.0080(4) -0.0118(4) 0.0197(5)
Cl1 0.0217(8) 0.0217(8) 0.0491(16) 0.000 0.000 0.000
Ni1 0.0082(3) 0.0082(3) 0.0077(3) -0.0003(2) 0.0003(2) 0.0006(3)
N1 0.012(2) 0.017(2) 0.022(3) 0.001(2) 0.001(2) 0.0031(18)
N2 0.023(2) 0.009(2) 0.007(2) 0.0019(17) 0.0046(18) 0.0008(18)
C1 0.043(4) 0.016(3) 0.040(5) 0.008(3) 0.013(3) 0.002(3)
C2 0.070(6) 0.022(3) 0.015(3) 0.015(3) -0.006(3) 0.001(3)
C3 0.020(3) 0.015(3) 0.022(3) 0.001(2) -0.005(2) -0.002(2)
C4 0.045(4) 0.005(3) 0.030(4) 0.007(2) -0.001(3) 0.001(3)
C5 0.022(3) 0.023(3) 0.023(3) -0.006(3) 0.007(3) -0.003(3)
C6 0.014(3) 0.047(4) 0.013(3) -0.010(3) -0.003(2) -0.002(3)
C7 0.014(3) 0.046(4) 0.032(4) -0.023(4) -0.001(3) 0.001(3)
C8 0.025(3) 0.021(3) 0.023(4) -0.003(3) -0.014(3) 0.001(2)
C9 0.018(3) 0.039(4) 0.009(3) -0.010(3) 0.002(2) 0.008(3)
C10 0.013(3) 0.029(3) 0.008(3) -0.001(2) 0.003(2) 0.010(2)
O1 0.0067(17) 0.017(2) 0.0113(14) -0.0042(14) -0.0023(13) 0.0027(13)
O2 0.0131(19) 0.0111(18) 0.017(2) -0.0004(16) 0.0015(15) -0.0026(15)
O3 0.014(2) 0.018(2) 0.018(2) -0.0026(17) 0.0041(17) 0.0011(15)
O4 0.025(2) 0.0112(19) 0.016(2) 0.0003(15) 0.0030(17) 0.0064(17)
O5 0.016(2) 0.018(2) 0.0098(18) -0.0007(15) -0.0023(15) 0.0081(16)
O6 0.013(2) 0.026(2) 0.0221(17) 0.0051(17) 0.0001(16) -0.0036(16)
O7 0.017(2) 0.023(2) 0.042(3) 0.011(2) -0.006(2) 0.0012(17)
O8 0.017(2) 0.029(2) 0.025(2) 0.0035(19) 0.0065(18) -0.0059(18)
O9 0.041(3) 0.051(4) 0.0206(19) -0.008(2) -0.012(2) 0.010(2)
O10 0.019(3) 0.029(4) 0.021(2) 0.000 0.000 0.003(2)

_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
V1 O1 1.636(3) . ?
V1 O4 1.930(4) . ?
V1 O3 1.930(4) . ?
V1 O2 1.940(4) . ?
V1 O5 1.947(4) . ?
V1 V3 2.9958(14) . ?
V1 V2 2.9975(14) 3_665 ?
V2 O7 1.607(5) . ?
V2 O6 1.875(5) . ?
V2 O5 1.889(4) . ?
V2 O2 1.914(4) 4_645 ?
V2 O3 1.977(4) 4_645 ?
V2 V3 2.9140(13) . ?
V2 V4 2.9217(15) 4_645 ?
V2 V1 2.9975(14) 4_645 ?
V3 O8 1.604(4) . ?
V3 O6 1.856(4) 4_645 ?
V3 O3 1.882(5) 4_645 ?
V3 O4 1.934(5) . ?
V3 O5 1.945(4) . ?
V3 V4 2.9488(15) 2_755 ?
V4 O9 1.610(4) . ?
V4 O10 1.827(2) . ?
V4 O4 1.890(4) 2_755 ?
V4 O2 1.893(4) . ?
V4 O6 2.110(4) 3_665 ?
V4 V2 2.9217(15) 3_665 ?
V4 V3 2.9488(15) 2_755 ?
Ni1 O1 2.036(3) 7_545 ?
Ni1 O1 2.036(3) . ?
Ni1 N1 2.136(5) . ?
Ni1 N1 2.136(5) 7_545 ?
Ni1 N2 2.156(5) 7_545 ?
Ni1 N2 2.156(5) . ?
N1 C6 1.329(8) . ?
N1 C10 1.374(8) . ?
N2 C1 1.316(9) . ?
N2 C5 1.344(8) . ?
C1 C2 1.426(9) . ?
C2 C3 1.358(10) . ?
C3 C4 1.400(10) . ?
C3 C8 1.488(7) 4_655 ?
C4 C5 1.367(9) . ?
C6 C7 1.372(9) . ?
C7 C8 1.390(10) . ?
C8 C9 1.380(9) . ?
C8 C3 1.488(7) 3_565 ?
C9 C10 1.343(9) . ?
O2 V2 1.914(4) 3_665 ?
O3 V3 1.882(5) 3_665 ?
O3 V2 1.977(4) 3_665 ?
O4 V4 1.890(4) 2_755 ?
O6 V3 1.856(4) 3_665 ?
O6 V4 2.110(4) 4_645 ?
O10 V4 1.827(2) 2_755 ?

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
O1 V1 O4 106.70(19) . . ?
O1 V1 O3 104.90(19) . . ?
O4 V1 O3 148.40(18) . . ?
O1 V1 O2 108.29(18) . . ?
O4 V1 O2 91.60(15) . . ?
O3 V1 O2 78.89(18) . . ?
O1 V1 O5 103.89(18) . . ?
O4 V1 O5 78.70(19) . . ?
O3 V1 O5 93.38(16) . . ?
O2 V1 O5 147.81(17) . . ?
O1 V1 V3 112.79(16) . . ?
O4 V1 V3 39.23(13) . . ?
O3 V1 V3 124.40(13) . . ?
O2 V1 V3 122.47(13) . . ?
O5 V1 V3 39.65(12) . . ?
O1 V1 V2 115.00(16) . 3_665 ?
O4 V1 V2 121.97(14) . 3_665 ?
O3 V1 V2 40.47(13) . 3_665 ?
O2 V1 V2 38.64(12) . 3_665 ?
O5 V1 V2 124.42(13) . 3_665 ?
V3 V1 V2 132.22(4) . 3_665 ?
O7 V2 O6 106.5(2) . . ?
O7 V2 O5 107.9(2) . . ?
O6 V2 O5 93.24(18) . . ?
O7 V2 O2 109.3(2) . 4_645 ?
O6 V2 O2 85.62(17) . 4_645 ?
O5 V2 O2 141.43(18) . 4_645 ?
O7 V2 O3 108.3(2) . 4_645 ?
O6 V2 O3 144.84(18) . 4_645 ?
O5 V2 O3 80.89(18) . 4_645 ?
O2 V2 O3 78.36(18) 4_645 4_645 ?
O7 V2 V3 111.63(19) . . ?
O6 V2 V3 127.30(12) . . ?
O5 V2 V3 41.25(13) . . ?
O2 V2 V3 113.18(13) 4_645 . ?
O3 V2 V3 39.76(13) 4_645 . ?
O7 V2 V4 112.5(2) . 4_645 ?
O6 V2 V4 46.10(12) . 4_645 ?
O5 V2 V4 128.72(13) . 4_645 ?
O2 V2 V4 39.62(13) 4_645 4_645 ?
O3 V2 V4 113.40(14) 4_645 4_645 ?
V3 V2 V4 134.42(5) . 4_645 ?
O7 V2 V1 117.79(18) . 4_645 ?
O6 V2 V1 116.58(13) . 4_645 ?
O5 V2 V1 111.84(13) . 4_645 ?
O2 V2 V1 39.25(12) 4_645 4_645 ?
O3 V2 V1 39.33(13) 4_645 4_645 ?
V3 V2 V1 75.03(3) . 4_645 ?
V4 V2 V1 75.07(4) 4_645 4_645 ?
O8 V3 O6 106.8(2) . 4_645 ?
O8 V3 O3 108.0(2) . 4_645 ?
O6 V3 O3 93.82(18) 4_645 4_645 ?
O8 V3 O4 108.5(2) . . ?
O6 V3 O4 84.35(18) 4_645 . ?
O3 V3 O4 142.40(19) 4_645 . ?
O8 V3 O5 107.6(2) . . ?
O6 V3 O5 144.90(17) 4_645 . ?
O3 V3 O5 81.89(18) 4_645 . ?
O4 V3 O5 78.64(18) . . ?
O8 V3 V2 111.35(18) . . ?
O6 V3 V2 128.46(12) 4_645 . ?
O3 V3 V2 42.20(13) 4_645 . ?
O4 V3 V2 113.63(14) . . ?
O5 V3 V2 39.82(12) . . ?
O8 V3 V4 112.37(18) . 2_755 ?
O6 V3 V4 45.40(12) 4_645 2_755 ?
O3 V3 V4 128.87(14) 4_645 2_755 ?
O4 V3 V4 39.01(13) . 2_755 ?
O5 V3 V4 113.08(13) . 2_755 ?
V2 V3 V4 134.56(5) . 2_755 ?
O8 V3 V1 116.46(18) . . ?
O6 V3 V1 115.83(13) 4_645 . ?
O3 V3 V1 113.44(14) 4_645 . ?
O4 V3 V1 39.12(13) . . ?
O5 V3 V1 39.69(12) . . ?
V2 V3 V1 75.67(3) . . ?
V4 V3 V1 74.47(4) 2_755 . ?
O9 V4 O10 102.2(2) . . ?
O9 V4 O4 113.1(3) . 2_755 ?
O10 V4 O4 92.10(16) . 2_755 ?
O9 V4 O2 111.8(3) . . ?
O10 V4 O2 91.74(14) . . ?
O4 V4 O2 132.87(15) 2_755 . ?
O9 V4 O6 100.6(2) . 3_665 ?
O10 V4 O6 157.25(18) . 3_665 ?
O4 V4 O6 78.81(18) 2_755 3_665 ?
O2 V4 O6 79.87(17) . 3_665 ?
O9 V4 V2 109.1(2) . 3_665 ?
O10 V4 V2 129.52(10) . 3_665 ?
O4 V4 V2 109.83(14) 2_755 3_665 ?
O2 V4 V2 40.16(12) . 3_665 ?
O6 V4 V2 39.81(12) 3_665 3_665 ?
O9 V4 V3 110.2(2) . 2_755 ?
O10 V4 V3 129.69(10) . 2_755 ?
O4 V4 V3 40.10(14) 2_755 2_755 ?
O2 V4 V3 109.72(13) . 2_755 ?
O6 V4 V3 38.77(12) 3_665 2_755 ?
V2 V4 V3 73.97(4) 3_665 2_755 ?
O1 Ni1 O1 178.2(3) 7_545 . ?
O1 Ni1 N1 90.56(17) 7_545 . ?
O1 Ni1 N1 90.73(17) . . ?
O1 Ni1 N1 90.73(17) 7_545 7_545 ?
O1 Ni1 N1 90.56(17) . 7_545 ?
N1 Ni1 N1 89.0(3) . 7_545 ?
O1 Ni1 N2 89.69(17) 7_545 7_545 ?
O1 Ni1 N2 89.03(16) . 7_545 ?
N1 Ni1 N2 179.4(2) . 7_545 ?
N1 Ni1 N2 90.48(16) 7_545 7_545 ?
O1 Ni1 N2 89.03(16) 7_545 . ?
O1 Ni1 N2 89.69(17) . . ?
N1 Ni1 N2 90.48(16) . . ?
N1 Ni1 N2 179.4(2) 7_545 . ?
N2 Ni1 N2 90.1(3) 7_545 . ?
C6 N1 C10 114.8(5) . . ?
C6 N1 Ni1 120.4(4) . . ?
C10 N1 Ni1 124.4(4) . . ?
C1 N2 C5 117.7(5) . . ?
C1 N2 Ni1 121.0(4) . . ?
C5 N2 Ni1 119.9(4) . . ?
N2 C1 C2 123.1(7) . . ?
C3 C2 C1 117.7(7) . . ?
C2 C3 C4 119.5(6) . . ?
C2 C3 C8 121.1(6) . 4_655 ?
C4 C3 C8 119.0(5) . 4_655 ?
C5 C4 C3 118.4(6) . . ?
N2 C5 C4 123.5(6) . . ?
N1 C6 C7 123.8(6) . . ?
C6 C7 C8 121.3(6) . . ?
C9 C8 C7 114.1(6) . . ?
C9 C8 C3 123.3(6) . 3_565 ?
C7 C8 C3 122.5(6) . 3_565 ?
C10 C9 C8 122.3(6) . . ?
C9 C10 N1 123.2(5) . . ?
V1 O1 Ni1 178.1(3) . . ?
V4 O2 V2 100.22(19) . 3_665 ?
V4 O2 V1 140.4(2) . . ?
V2 O2 V1 102.10(19) 3_665 . ?
V3 O3 V1 141.6(2) 3_665 . ?
V3 O3 V2 98.05(19) 3_665 3_665 ?
V1 O3 V2 100.2(2) . 3_665 ?
V4 O4 V1 140.6(3) 2_755 . ?
V4 O4 V3 100.9(2) 2_755 . ?
V1 O4 V3 101.7(2) . . ?
V2 O5 V3 98.93(19) . . ?
V2 O5 V1 141.9(2) . . ?
V3 O5 V1 100.66(18) . . ?
V3 O6 V2 142.4(2) 3_665 . ?
V3 O6 V4 95.84(18) 3_665 4_645 ?
V2 O6 V4 94.10(19) . 4_645 ?
V4 O10 V4 129.4(3) 2_755 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.144