# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2011


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Yan Xu'
_publ_contact_author_email       yanxu@njut.edu.cn

_publ_section_title              
;
{[VIV14VV4O42(H2O)][Ni(C4N3H13)(C4N3H14)]4(H5O2)4}8+:
A novel nanosized calix-type polyoxovanadate cation

;
loop_
_publ_author_name
'Yan Xu'
'Zhibin Zhang'
'Lei Zheng'
'Dunru Zhu'
'You SONG'

data_zzb4
_database_code_depnum_ccdc_archive 'CCDC 793076'
#TrackingRef '- ZZB4.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H167 N30 Ni4 O101 P V36'
_chemical_formula_weight         4784.69

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'
P P 0.1023 0.0942 '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   P4/n

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

_cell_length_a                   18.9721(7)
_cell_length_b                   18.9721(7)
_cell_length_c                   20.2105(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7274.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    60
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      24.36

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4760
_exptl_absorpt_coefficient_mu    2.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6941
_exptl_absorpt_correction_T_max  0.7289
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53134
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_av_sigmaI/netI    0.0664
_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       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.01
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6791
_reflns_number_gt                4550
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_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^)+(0.1520P)^2^+0.0000P] 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    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6791
_refine_ls_number_parameters     515
_refine_ls_number_restraints     148
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.2342
_refine_ls_wR_factor_gt          0.2159
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.002

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
Ni1 Ni 0.35559(3) 0.95704(3) 0.15770(3) 0.02581(15) Uani 1 1 d . . .
V1 V 0.29578(4) 1.12221(3) 0.09146(3) 0.02051(18) Uani 1 1 d . . .
V2 V 0.2500 1.2500 0.15458(7) 0.0311(4) Uani 1 4 d S . .
V3 V 0.16606(4) 1.07110(4) -0.02983(4) 0.0301(2) Uani 1 1 d . . .
V4 V 0.31693(5) 1.06438(4) -0.04631(4) 0.0385(2) Uani 1 1 d . . .
V5 V 0.19072(5) 1.12513(4) -0.16805(4) 0.0356(2) Uani 1 1 d . . .
V6 V 0.2500 1.2500 -0.22991(8) 0.0472(5) Uani 1 4 d S . .
V7 V 0.2500 0.7500 0.30643(5) 0.0330(3) Uani 1 2 d S . .
V8 V 0.42497(4) 0.86058(5) 0.50277(4) 0.0360(2) Uani 1 1 d . . .
V9 V 0.28870(5) 0.93497(4) 0.49623(4) 0.0331(2) Uani 1 1 d . . .
V10 V 0.35941(4) 0.82693(4) 0.37440(4) 0.0305(2) Uani 1 1 d . . .
V11 V 0.17953(4) 0.86522(4) 0.37376(4) 0.0300(2) Uani 1 1 d . . .
P1 P 0.2500 0.7500 0.5000 0.0217(5) Uani 1 4 d S . .
O1 O 0.2500 1.2500 -0.3093(3) 0.080(3) Uani 1 4 d S . .
O2 O 0.24630(16) 1.06887(17) 0.02450(15) 0.0339(9) Uani 1 1 d . . .
O3 O 0.21012(15) 1.16458(15) 0.12175(15) 0.0307(9) Uani 1 1 d . . .
O4 O 0.31649(15) 1.06326(14) 0.14637(14) 0.0244(8) Uani 1 1 d . . .
O5 O 0.11762(16) 1.12500(16) -0.09988(14) 0.0318(8) Uani 1 1 d . . .
O6 O 0.36859(15) 1.11330(16) 0.02441(14) 0.0290(8) Uani 1 1 d . . .
O7 O 0.1658(2) 1.0691(2) -0.22311(18) 0.0529(11) Uani 1 1 d . . .
O8 O 0.35268(18) 0.89193(16) 0.55935(14) 0.0359(9) Uani 1 1 d . . .
O9 O 0.26463(17) 0.81438(17) 0.45627(15) 0.0366(9) Uani 1 1 d . . .
O10 O 0.36369(17) 0.90725(17) 0.43641(15) 0.0371(9) Uani 1 1 d . . .
O11 O 0.42150(17) 0.78659(17) 0.44120(15) 0.0361(9) Uani 1 1 d . . .
O12 O 0.2500 1.2500 0.2341(3) 0.052(2) Uani 1 4 d S . .
O13 O 0.33744(16) 0.73115(16) 0.34516(15) 0.0322(9) Uani 1 1 d . . .
O14 O 0.26921(17) 0.84693(17) 0.33144(14) 0.0350(9) Uani 1 1 d . . .
O15 O 0.33944(18) 1.28241(18) -0.19663(16) 0.0423(10) Uani 1 1 d . . .
O16 O 0.34453(18) 0.98423(17) -0.04812(17) 0.0424(10) Uani 1 1 d . . .
O17 O 0.21610(18) 0.93879(17) 0.43021(16) 0.0399(10) Uani 1 1 d . . .
O18 O 0.13037(18) 0.99545(17) -0.02469(18) 0.0443(10) Uani 1 1 d . . .
O19 O 0.41345(18) 0.85394(18) 0.31820(15) 0.0413(10) Uani 1 1 d . . .
O20 O 0.13963(19) 0.90981(19) 0.31770(16) 0.0452(10) Uani 1 1 d . . .
O21 O 0.3068(2) 1.01763(19) 0.50402(17) 0.0507(12) Uani 1 1 d . . .
O22 O 0.23759(17) 1.06862(17) -0.10052(15) 0.0385(9) Uani 1 1 d . . .
O23 O 0.4979(2) 0.9069(2) 0.50337(17) 0.0546(12) Uani 1 1 d . . .
O24 O 0.2500 0.7500 0.2264(2) 0.0562(18) Uani 1 2 d S . .
C1 C 0.2055(3) 0.9395(4) 0.1698(3) 0.072(2) Uani 1 1 d U . .
H1A H 0.1918 0.9872 0.1585 0.087 Uiso 1 1 calc R . .
H1B H 0.1659 0.9175 0.1923 0.087 Uiso 1 1 calc R . .
C2 C 0.2204(3) 0.9007(4) 0.1095(3) 0.067(2) Uani 1 1 d . . .
H2A H 0.1854 0.9128 0.0764 0.081 Uiso 1 1 calc R . .
H2B H 0.2164 0.8506 0.1183 0.081 Uiso 1 1 calc R . .
C3 C 0.3258(3) 0.8534(3) 0.0572(3) 0.0451(15) Uani 1 1 d . . .
H3A H 0.3628 0.8677 0.0269 0.054 Uiso 1 1 calc R . .
H3B H 0.2920 0.8255 0.0325 0.054 Uiso 1 1 calc R . .
C4 C 0.3567(3) 0.8097(3) 0.1104(3) 0.0488(16) Uani 1 1 d . . .
H4A H 0.3195 0.7836 0.1323 0.059 Uiso 1 1 calc R . .
H4B H 0.3892 0.7760 0.0912 0.059 Uiso 1 1 calc R . .
C5 C 0.4731(3) 1.0393(3) 0.2066(3) 0.0553(18) Uani 1 1 d . . .
H5A H 0.5132 1.0445 0.2360 0.066 Uiso 1 1 calc R . .
H5B H 0.4522 1.0854 0.2002 0.066 Uiso 1 1 calc R . .
C6 C 0.4976(3) 1.0112(4) 0.1415(3) 0.066(2) Uani 1 1 d . . .
H6A H 0.5267 1.0463 0.1199 0.080 Uiso 1 1 calc R . .
H6B H 0.5262 0.9696 0.1489 0.080 Uiso 1 1 calc R . .
C7 C 0.4249(4) 1.0559(4) 0.3462(3) 0.095(2) Uani 1 1 d DU . .
H7A H 0.4627 1.0837 0.3272 0.114 Uiso 1 1 calc R . .
H7B H 0.3942 1.0878 0.3702 0.114 Uiso 1 1 calc R . .
C8 C 0.3849(3) 1.0243(3) 0.2927(3) 0.0555(18) Uani 1 1 d . . .
H8A H 0.3536 1.0603 0.2753 0.067 Uiso 1 1 calc R . .
H8B H 0.3553 0.9879 0.3118 0.067 Uiso 1 1 calc R . .
N1 N 0.26406(19) 0.9419(2) 0.21380(19) 0.0367(11) Uani 1 1 d . . .
H1C H 0.2671 0.9013 0.2367 0.044 Uiso 1 1 calc R . .
H1D H 0.2587 0.9775 0.2428 0.044 Uiso 1 1 calc R . .
N2 N 0.29118(19) 0.9154(2) 0.08271(18) 0.0303(10) Uani 1 1 d . . .
H2C H 0.2873 0.9478 0.0497 0.036 Uiso 1 1 calc R . .
N3 N 0.3942(2) 0.8528(2) 0.1593(2) 0.0417(12) Uani 1 1 d . . .
H3C H 0.4406 0.8528 0.1501 0.050 Uiso 1 1 calc R . .
H3D H 0.3882 0.8343 0.1999 0.050 Uiso 1 1 calc R . .
N4 N 0.4390(2) 0.99310(19) 0.09850(19) 0.0332(11) Uani 1 1 d . . .
H4C H 0.4520 0.9593 0.0698 0.040 Uiso 1 1 calc R . .
H4D H 0.4253 1.0312 0.0753 0.040 Uiso 1 1 calc R . .
N5 N 0.4223(2) 0.9930(2) 0.23639(19) 0.0379(12) Uani 1 1 d . . .
H5C H 0.4462 0.9548 0.2519 0.046 Uiso 1 1 calc R . .
O1W O 0.2500 1.2500 -0.0343(5) 0.071(3) Uani 1 4 d S . .
O2W O 0.4041(4) 1.2040(4) 0.2613(3) 0.166(3) Uani 1 1 d DU . .
O3W O 0.4170(5) 1.2308(5) 0.3833(4) 0.208(3) Uani 1 1 d DU . .
O4W O 0.0538(6) 1.0795(6) -0.3270(5) 0.258(4) Uani 1 1 d U . .
N6 N 0.4544(4) 1.0078(3) 0.3916(3) 0.119(2) Uani 1 1 d DU . .
H6C H 0.4764 1.0314 0.4235 0.179 Uiso 1 1 calc R . .
H6D H 0.4850 0.9801 0.3707 0.179 Uiso 1 1 calc R . .
H6E H 0.4203 0.9816 0.4091 0.179 Uiso 1 1 calc R . .
N7 N 0.19123(12) 1.18401(14) -0.52066(8) 0.259(4) Uani 0.50 1 d PDU . .
H7C H 0.1573 1.2026 -0.5456 0.389 Uiso 0.50 1 d PR . .
H7D H 0.2150 1.1521 -0.5440 0.389 Uiso 0.50 1 d PR . .
N8 N 0.24824(4) 1.08730(8) -0.37397(11) 0.193(3) Uani 0.50 1 d PDU . .
H8C H 0.2740 1.0863 -0.4114 0.232 Uiso 0.50 1 calc PR . .
H8D H 0.2636 1.1250 -0.3511 0.232 Uiso 0.25 1 calc PR . .
N9 N 0.3185(3) 0.9561(3) -0.20733(9) 0.145(4) Uani 0.50 1 d PDU . .
H9C H 0.3245 0.9097 -0.2039 0.217 Uiso 0.50 1 calc PR . .
H9D H 0.2845 0.9698 -0.1798 0.217 Uiso 0.50 1 calc PR . .
H9E H 0.3585 0.9780 -0.1969 0.217 Uiso 0.50 1 calc PR . .
C9 C 0.15850(15) 1.15142(8) -0.45860(6) 0.207(3) Uani 0.50 1 d PDU . .
H9A H 0.1197 1.1252 -0.4779 0.249 Uiso 0.50 1 calc PR . .
H9B H 0.1364 1.1925 -0.4389 0.249 Uiso 0.50 1 calc PR . .
C10 C 0.17339(5) 1.10689(11) -0.39644(8) 0.199(3) Uani 0.50 1 d PDU . .
H10A H 0.1514 1.1312 -0.3596 0.239 Uiso 0.50 1 calc PR . .
H10B H 0.1480 1.0629 -0.4020 0.239 Uiso 0.50 1 calc PR . .
C11 C 0.27315(17) 1.02344(9) -0.33406(10) 0.167(3) Uani 0.50 1 d PDU . .
H11A H 0.2354 0.9927 -0.3487 0.201 Uiso 0.50 1 calc PR . .
H11B H 0.3116 1.0118 -0.3638 0.201 Uiso 0.50 1 calc PR . .
C12 C 0.2978(2) 0.97471(15) -0.27839(9) 0.158(4) Uani 0.50 1 d PDU . .
H12A H 0.3397 0.9566 -0.3001 0.190 Uiso 0.50 1 calc PR . .
H12B H 0.2633 0.9376 -0.2849 0.190 Uiso 0.50 1 calc PR . .

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
Ni1 0.0275(3) 0.0223(3) 0.0276(3) 0.0006(2) -0.0007(2) 0.0013(2)
V1 0.0197(3) 0.0168(3) 0.0250(4) 0.0003(3) 0.0013(3) 0.0015(3)
V2 0.0344(5) 0.0344(5) 0.0244(7) 0.000 0.000 0.000
V3 0.0272(4) 0.0256(4) 0.0376(4) -0.0043(3) -0.0031(4) -0.0052(3)
V4 0.0397(5) 0.0346(4) 0.0412(5) -0.0027(4) 0.0061(4) 0.0036(4)
V5 0.0394(4) 0.0389(5) 0.0285(4) -0.0080(4) -0.0027(4) -0.0002(4)
V6 0.0579(7) 0.0579(7) 0.0257(8) 0.000 0.000 0.000
V7 0.0410(6) 0.0396(6) 0.0184(5) 0.000 0.000 -0.0017(5)
V8 0.0326(4) 0.0427(5) 0.0328(4) -0.0045(4) -0.0012(4) -0.0124(4)
V9 0.0417(5) 0.0283(4) 0.0293(4) 0.0012(3) 0.0022(4) -0.0029(4)
V10 0.0321(4) 0.0364(4) 0.0229(4) 0.0026(3) 0.0014(3) -0.0079(3)
V11 0.0355(4) 0.0306(4) 0.0237(4) 0.0058(3) 0.0009(3) 0.0022(3)
P1 0.0226(6) 0.0226(6) 0.0199(10) 0.000 0.000 0.000
O1 0.110(4) 0.110(4) 0.020(4) 0.000 0.000 0.000
O2 0.0270(16) 0.0413(18) 0.0334(16) -0.0067(15) -0.0036(14) 0.0004(15)
O3 0.0201(14) 0.0294(16) 0.0427(18) 0.0010(14) 0.0019(14) 0.0038(13)
O4 0.0277(15) 0.0162(14) 0.0293(15) 0.0007(12) 0.0035(13) 0.0006(12)
O5 0.0311(16) 0.0305(16) 0.0339(16) -0.0019(14) -0.0012(14) 0.0030(14)
O6 0.0231(15) 0.0309(16) 0.0331(16) -0.0005(14) 0.0085(13) -0.0007(13)
O7 0.059(2) 0.056(2) 0.044(2) -0.0188(18) -0.0105(19) -0.0041(19)
O8 0.053(2) 0.0328(17) 0.0215(15) 0.0008(14) -0.0014(15) -0.0007(16)
O9 0.0354(17) 0.0411(18) 0.0334(17) 0.0066(15) 0.0016(15) -0.0040(15)
O10 0.0413(18) 0.0399(18) 0.0303(16) -0.0033(15) 0.0052(15) -0.0120(16)
O11 0.0417(18) 0.0383(18) 0.0283(16) 0.0014(15) -0.0036(15) -0.0061(15)
O12 0.062(3) 0.062(3) 0.032(4) 0.000 0.000 0.000
O13 0.0287(16) 0.0326(17) 0.0353(17) 0.0012(14) -0.0024(14) 0.0025(14)
O14 0.0360(17) 0.0415(18) 0.0274(16) 0.0068(14) -0.0002(14) 0.0056(15)
O15 0.0418(19) 0.048(2) 0.0365(18) 0.0028(16) 0.0117(16) -0.0055(17)
O16 0.047(2) 0.0344(18) 0.046(2) -0.0044(16) 0.0026(17) 0.0035(16)
O17 0.050(2) 0.0332(17) 0.0365(18) 0.0021(15) -0.0032(16) -0.0001(16)
O18 0.0417(19) 0.0295(17) 0.062(2) -0.0093(17) -0.0076(18) -0.0123(15)
O19 0.0471(19) 0.049(2) 0.0276(16) 0.0074(16) 0.0088(16) -0.0106(17)
O20 0.051(2) 0.052(2) 0.0325(18) 0.0081(17) 0.0012(17) 0.0141(18)
O21 0.077(3) 0.0339(19) 0.041(2) -0.0034(16) -0.0068(19) -0.0127(19)
O22 0.0376(18) 0.0464(19) 0.0314(16) -0.0028(15) -0.0010(15) 0.0097(16)
O23 0.046(2) 0.071(3) 0.046(2) -0.0097(19) -0.0012(17) -0.0299(19)
O24 0.079(4) 0.069(4) 0.020(2) 0.000 0.000 -0.009(3)
C1 0.057(3) 0.101(4) 0.060(3) -0.003(3) 0.012(3) -0.012(3)
C2 0.042(3) 0.092(5) 0.068(4) -0.028(4) 0.009(3) -0.017(3)
C3 0.046(3) 0.036(3) 0.054(3) -0.007(3) 0.012(3) -0.011(2)
C4 0.046(3) 0.035(3) 0.066(3) -0.007(3) 0.016(3) -0.004(3)
C5 0.052(3) 0.068(4) 0.046(3) 0.000(3) -0.007(3) -0.014(3)
C6 0.041(3) 0.078(4) 0.080(4) -0.014(4) 0.005(3) -0.017(3)
C7 0.098(4) 0.092(4) 0.095(4) 0.004(3) -0.015(3) -0.038(3)
C8 0.063(4) 0.065(4) 0.039(3) -0.010(3) -0.011(3) -0.017(3)
N1 0.032(2) 0.041(2) 0.037(2) 0.0121(19) 0.0011(18) -0.0005(18)
N2 0.031(2) 0.033(2) 0.0269(19) -0.0027(17) 0.0051(16) -0.0017(17)
N3 0.048(2) 0.026(2) 0.051(3) 0.0048(19) 0.004(2) 0.0122(19)
N4 0.039(2) 0.0242(19) 0.036(2) 0.0007(17) 0.0015(18) 0.0107(17)
N5 0.034(2) 0.040(2) 0.040(2) 0.0048(19) -0.0003(19) -0.0045(19)
O1W 0.047(3) 0.047(3) 0.119(7) 0.000 0.000 0.000
O2W 0.172(5) 0.161(5) 0.164(5) 0.026(4) 0.002(4) -0.009(4)
O3W 0.196(5) 0.222(6) 0.207(5) -0.004(5) -0.031(5) 0.000(5)
O4W 0.257(6) 0.264(6) 0.254(6) -0.020(5) -0.019(5) 0.000(5)
N6 0.128(4) 0.112(4) 0.118(4) 0.018(4) -0.038(4) -0.050(3)
N7 0.258(6) 0.260(7) 0.260(7) -0.001(5) -0.003(5) 0.002(5)
N8 0.195(5) 0.197(5) 0.187(5) -0.012(4) 0.011(4) 0.007(4)
N9 0.141(6) 0.147(6) 0.146(6) 0.003(5) 0.003(5) 0.008(5)
C9 0.206(5) 0.210(5) 0.206(5) -0.005(5) 0.000(5) 0.005(5)
C10 0.200(5) 0.201(5) 0.196(5) -0.011(4) 0.005(4) 0.002(4)
C11 0.170(5) 0.170(5) 0.163(5) -0.014(4) 0.008(4) 0.003(4)
C12 0.155(6) 0.157(6) 0.163(6) -0.017(5) 0.013(5) -0.001(5)

_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
Ni1 N1 2.094(4) . ?
Ni1 N4 2.098(4) . ?
Ni1 N2 2.101(4) . ?
Ni1 N3 2.109(4) . ?
Ni1 N5 2.144(4) . ?
Ni1 O4 2.160(3) . ?
V1 O4 1.624(3) . ?
V1 O3 1.914(3) . ?
V1 O3 1.929(3) 3_665 ?
V1 O2 1.933(3) . ?
V1 O6 1.942(3) . ?
V1 V2 2.8741(9) . ?
V1 V4 3.0194(11) . ?
V2 O12 1.606(7) . ?
V2 O3 1.908(3) 4_465 ?
V2 O3 1.908(3) . ?
V2 O3 1.908(3) 2_575 ?
V2 O3 1.908(3) 3_665 ?
V2 V1 2.8741(10) 4_465 ?
V2 V1 2.8741(9) 2_575 ?
V2 V1 2.8741(10) 3_665 ?
V3 O18 1.590(3) . ?
V3 O6 1.874(3) 4_465 ?
V3 O2 1.877(3) . ?
V3 O22 1.971(3) . ?
V3 O5 1.974(3) . ?
V3 V4 2.8843(12) . ?
V3 V4 2.8888(12) 4_465 ?
V3 V5 3.0122(12) . ?
V4 O16 1.609(3) . ?
V4 O5 1.846(3) 3_665 ?
V4 O22 1.864(3) . ?
V4 O2 1.962(3) . ?
V4 O6 1.966(3) . ?
V4 V3 2.8888(12) 3_665 ?
V5 O7 1.610(4) . ?
V5 O15 1.933(3) 2_575 ?
V5 O22 1.950(3) . ?
V5 O15 1.952(3) 4_465 ?
V5 O5 1.955(3) . ?
V5 V6 2.9052(11) . ?
V6 O1 1.604(7) . ?
V6 O15 1.926(3) 2_575 ?
V6 O15 1.926(3) 3_665 ?
V6 O15 1.926(3) . ?
V6 O15 1.926(3) 4_465 ?
V6 V5 2.9052(11) 4_465 ?
V6 V5 2.9052(11) 2_575 ?
V6 V5 2.9052(11) 3_665 ?
V7 O24 1.617(5) . ?
V7 O13 1.869(3) 2_565 ?
V7 O13 1.869(3) . ?
V7 O14 1.942(3) 2_565 ?
V7 O14 1.942(3) . ?
V7 V10 2.8855(9) . ?
V7 V10 2.8855(9) 2_565 ?
V7 V11 2.9012(9) 2_565 ?
V7 V11 2.9012(9) . ?
V8 O23 1.639(4) . ?
V8 O11 1.877(3) . ?
V8 O8 1.882(3) . ?
V8 O10 1.983(3) . ?
V8 O17 2.005(3) 7_566 ?
V8 V9 2.8386(13) 7_566 ?
V8 V11 2.8445(11) 7_566 ?
V8 V10 2.9471(11) . ?
V8 V9 2.9484(12) . ?
V9 O21 1.613(4) . ?
V9 O17 1.919(3) . ?
V9 O11 1.925(3) 8_666 ?
V9 O10 1.940(3) . ?
V9 O8 1.941(3) . ?
V9 O9 2.469(3) . ?
V9 V8 2.8386(13) 8_666 ?
V10 O19 1.614(3) . ?
V10 O11 1.948(3) . ?
V10 O13 1.956(3) . ?
V10 O14 1.956(3) . ?
V10 O10 1.975(3) . ?
V10 O9 2.455(3) . ?
V11 O20 1.604(3) . ?
V11 O8 1.929(3) 8_666 ?
V11 O17 1.931(3) . ?
V11 O14 1.936(3) . ?
V11 O13 1.944(3) 2_565 ?
V11 V8 2.8445(11) 8_666 ?
P1 O9 1.533(3) 8_666 ?
P1 O9 1.533(3) 7_566 ?
P1 O9 1.533(3) . ?
P1 O9 1.533(3) 2_565 ?
O3 V1 1.929(3) 4_465 ?
O5 V4 1.846(3) 4_465 ?
O6 V3 1.874(3) 3_665 ?
O8 V11 1.929(3) 7_566 ?
O11 V9 1.925(3) 7_566 ?
O13 V11 1.944(3) 2_565 ?
O15 V5 1.933(3) 2_575 ?
O15 V5 1.952(3) 3_665 ?
O17 V8 2.005(3) 8_666 ?
C1 N1 1.424(7) . ?
C1 C2 1.453(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.474(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.443(6) . ?
C3 C4 1.480(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N3 1.466(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N5 1.436(7) . ?
C5 C6 1.493(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N4 1.452(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N6 1.409(8) . ?
C7 C8 1.450(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N5 1.467(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N2 H2C 0.9100 . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
N5 H5C 0.9100 . ?
N6 H6C 0.8900 . ?
N6 H6D 0.8900 . ?
N6 H6E 0.8900 . ?
N7 C9 1.5301(14) . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8899 . ?
N8 C11 1.5303(16) . ?
N8 C10 1.5365(10) . ?
N8 H8C 0.9000 . ?
N8 H8D 0.9000 . ?
N9 C12 1.5300(18) . ?
N9 H9C 0.8900 . ?
N9 H9D 0.8900 . ?
N9 H9E 0.8900 . ?
C9 C10 1.5399(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.5296(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?

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
N1 Ni1 N4 168.22(15) . . ?
N1 Ni1 N2 81.76(15) . . ?
N4 Ni1 N2 98.61(14) . . ?
N1 Ni1 N3 98.68(16) . . ?
N4 Ni1 N3 93.02(16) . . ?
N2 Ni1 N3 81.97(16) . . ?
N1 Ni1 N5 97.56(15) . . ?
N4 Ni1 N5 82.77(15) . . ?
N2 Ni1 N5 176.46(15) . . ?
N3 Ni1 N5 94.73(16) . . ?
N1 Ni1 O4 84.30(13) . . ?
N4 Ni1 O4 83.93(13) . . ?
N2 Ni1 O4 94.27(13) . . ?
N3 Ni1 O4 174.78(14) . . ?
N5 Ni1 O4 89.10(13) . . ?
O4 V1 O3 106.03(14) . . ?
O4 V1 O3 106.51(14) . 3_665 ?
O3 V1 O3 82.32(18) . 3_665 ?
O4 V1 O2 103.62(14) . . ?
O3 V1 O2 91.80(13) . . ?
O3 V1 O2 149.77(13) 3_665 . ?
O4 V1 O6 104.17(14) . . ?
O3 V1 O6 149.73(13) . . ?
O3 V1 O6 91.12(13) 3_665 . ?
O2 V1 O6 79.13(13) . . ?
O4 V1 V2 110.53(11) . . ?
O3 V1 V2 41.15(9) . . ?
O3 V1 V2 41.21(9) 3_665 . ?
O2 V1 V2 127.27(10) . . ?
O6 V1 V2 126.73(9) . . ?
O4 V1 V4 110.36(10) . . ?
O3 V1 V4 124.09(10) . . ?
O3 V1 V4 123.71(10) 3_665 . ?
O2 V1 V4 39.53(9) . . ?
O6 V1 V4 39.70(9) . . ?
V2 V1 V4 139.11(4) . . ?
O12 V2 O3 110.35(10) . 4_465 ?
O12 V2 O3 110.35(10) . . ?
O3 V2 O3 83.05(7) 4_465 . ?
O12 V2 O3 110.35(10) . 2_575 ?
O3 V2 O3 83.05(7) 4_465 2_575 ?
O3 V2 O3 139.3(2) . 2_575 ?
O12 V2 O3 110.35(10) . 3_665 ?
O3 V2 O3 139.3(2) 4_465 3_665 ?
O3 V2 O3 83.05(7) . 3_665 ?
O3 V2 O3 83.05(7) 2_575 3_665 ?
O12 V2 V1 116.35(3) . 4_465 ?
O3 V2 V1 41.31(9) 4_465 4_465 ?
O3 V2 V1 41.78(9) . 4_465 ?
O3 V2 V1 115.91(10) 2_575 4_465 ?
O3 V2 V1 116.26(10) 3_665 4_465 ?
O12 V2 V1 116.35(3) . . ?
O3 V2 V1 115.91(10) 4_465 . ?
O3 V2 V1 41.31(9) . . ?
O3 V2 V1 116.26(10) 2_575 . ?
O3 V2 V1 41.78(9) 3_665 . ?
V1 V2 V1 78.64(2) 4_465 . ?
O12 V2 V1 116.35(3) . 2_575 ?
O3 V2 V1 41.78(9) 4_465 2_575 ?
O3 V2 V1 116.26(10) . 2_575 ?
O3 V2 V1 41.31(9) 2_575 2_575 ?
O3 V2 V1 115.91(10) 3_665 2_575 ?
V1 V2 V1 78.64(2) 4_465 2_575 ?
V1 V2 V1 127.30(6) . 2_575 ?
O12 V2 V1 116.35(3) . 3_665 ?
O3 V2 V1 116.26(10) 4_465 3_665 ?
O3 V2 V1 115.91(10) . 3_665 ?
O3 V2 V1 41.78(9) 2_575 3_665 ?
O3 V2 V1 41.31(9) 3_665 3_665 ?
V1 V2 V1 127.30(6) 4_465 3_665 ?
V1 V2 V1 78.64(2) . 3_665 ?
V1 V2 V1 78.64(2) 2_575 3_665 ?
O18 V3 O6 106.58(16) . 4_465 ?
O18 V3 O2 106.66(17) . . ?
O6 V3 O2 96.01(14) 4_465 . ?
O18 V3 O22 108.60(17) . . ?
O6 V3 O22 143.73(14) 4_465 . ?
O2 V3 O22 82.25(13) . . ?
O18 V3 O5 108.43(16) . . ?
O6 V3 O5 81.64(13) 4_465 . ?
O2 V3 O5 143.98(14) . . ?
O22 V3 O5 79.22(13) . . ?
O18 V3 V4 112.96(13) . . ?
O6 V3 V4 128.64(10) 4_465 . ?
O2 V3 V4 42.43(10) . . ?
O22 V3 V4 39.83(9) . . ?
O5 V3 V4 113.71(10) . . ?
O18 V3 V4 112.76(13) . 4_465 ?
O6 V3 V4 42.42(9) 4_465 4_465 ?
O2 V3 V4 128.71(10) . 4_465 ?
O22 V3 V4 113.19(10) . 4_465 ?
O5 V3 V4 39.22(9) . 4_465 ?
V4 V3 V4 132.99(4) . 4_465 ?
O18 V3 V5 115.71(14) . . ?
O6 V3 V5 114.68(10) 4_465 . ?
O2 V3 V5 115.09(10) . . ?
O22 V3 V5 39.55(10) . . ?
O5 V3 V5 39.71(9) . . ?
V4 V3 V5 75.75(3) . . ?
V4 V3 V5 75.32(3) 4_465 . ?
O16 V4 O5 108.03(16) . 3_665 ?
O16 V4 O22 106.88(17) . . ?
O5 V4 O22 96.52(14) 3_665 . ?
O16 V4 O2 106.26(16) . . ?
O5 V4 O2 144.27(14) 3_665 . ?
O22 V4 O2 82.84(14) . . ?
O16 V4 O6 107.49(16) . . ?
O5 V4 O6 82.56(13) 3_665 . ?
O22 V4 O6 144.08(14) . . ?
O2 V4 O6 77.87(12) . . ?
O16 V4 V3 111.56(13) . . ?
O5 V4 V3 129.49(10) 3_665 . ?
O22 V4 V3 42.64(10) . . ?
O2 V4 V3 40.21(9) . . ?
O6 V4 V3 112.95(9) . . ?
O16 V4 V3 113.23(13) . 3_665 ?
O5 V4 V3 42.54(9) 3_665 3_665 ?
O22 V4 V3 129.27(11) . 3_665 ?
O2 V4 V3 112.90(10) . 3_665 ?
O6 V4 V3 40.03(9) . 3_665 ?
V3 V4 V3 133.39(4) . 3_665 ?
O16 V4 V1 114.06(13) . . ?
O5 V4 V1 114.93(10) 3_665 . ?
O22 V4 V1 114.78(10) . . ?
O2 V4 V1 38.84(9) . . ?
O6 V4 V1 39.13(8) . . ?
V3 V4 V1 75.27(3) . . ?
V3 V4 V1 75.45(3) 3_665 . ?
O7 V5 O15 107.79(17) . 2_575 ?
O7 V5 O22 104.76(17) . . ?
O15 V5 O22 147.44(14) 2_575 . ?
O7 V5 O15 106.56(17) . 4_465 ?
O15 V5 O15 82.1(2) 2_575 4_465 ?
O22 V5 O15 89.43(14) . 4_465 ?
O7 V5 O5 106.11(17) . . ?
O15 V5 O5 90.10(14) 2_575 . ?
O22 V5 O5 80.18(13) . . ?
O15 V5 O5 147.25(14) 4_465 . ?
O7 V5 V6 110.79(14) . . ?
O15 V5 V6 41.08(10) 2_575 . ?
O22 V5 V6 124.96(11) . . ?
O15 V5 V6 41.15(10) 4_465 . ?
O5 V5 V6 125.37(10) . . ?
O7 V5 V3 111.75(14) . . ?
O15 V5 V3 122.67(11) 2_575 . ?
O22 V5 V3 40.06(10) . . ?
O15 V5 V3 122.00(10) 4_465 . ?
O5 V5 V3 40.16(9) . . ?
V6 V5 V3 137.45(4) . . ?
O1 V6 O15 110.44(11) . 2_575 ?
O1 V6 O15 110.44(11) . 3_665 ?
O15 V6 O15 83.00(7) 2_575 3_665 ?
O1 V6 O15 110.44(11) . . ?
O15 V6 O15 139.1(2) 2_575 . ?
O15 V6 O15 83.00(7) 3_665 . ?
O1 V6 O15 110.44(11) . 4_465 ?
O15 V6 O15 83.00(7) 2_575 4_465 ?
O15 V6 O15 139.1(2) 3_665 4_465 ?
O15 V6 O15 83.00(7) . 4_465 ?
O1 V6 V5 115.49(3) . 4_465 ?
O15 V6 V5 41.83(10) 2_575 4_465 ?
O15 V6 V5 41.27(10) 3_665 4_465 ?
O15 V6 V5 116.40(11) . 4_465 ?
O15 V6 V5 116.81(11) 4_465 4_465 ?
O1 V6 V5 115.49(3) . 2_575 ?
O15 V6 V5 116.81(11) 2_575 2_575 ?
O15 V6 V5 41.83(10) 3_665 2_575 ?
O15 V6 V5 41.27(10) . 2_575 ?
O15 V6 V5 116.40(11) 4_465 2_575 ?
V5 V6 V5 79.33(3) 4_465 2_575 ?
O1 V6 V5 115.49(3) . . ?
O15 V6 V5 41.27(10) 2_575 . ?
O15 V6 V5 116.40(11) 3_665 . ?
O15 V6 V5 116.81(11) . . ?
O15 V6 V5 41.83(10) 4_465 . ?
V5 V6 V5 79.33(3) 4_465 . ?
V5 V6 V5 129.03(7) 2_575 . ?
O1 V6 V5 115.49(3) . 3_665 ?
O15 V6 V5 116.40(11) 2_575 3_665 ?
O15 V6 V5 116.81(11) 3_665 3_665 ?
O15 V6 V5 41.83(10) . 3_665 ?
O15 V6 V5 41.27(10) 4_465 3_665 ?
V5 V6 V5 129.03(7) 4_465 3_665 ?
V5 V6 V5 79.33(3) 2_575 3_665 ?
V5 V6 V5 79.33(3) . 3_665 ?
O24 V7 O13 114.76(10) . 2_565 ?
O24 V7 O13 114.76(10) . . ?
O13 V7 O13 130.48(19) 2_565 . ?
O24 V7 O14 105.09(9) . 2_565 ?
O13 V7 O14 84.59(13) 2_565 2_565 ?
O13 V7 O14 82.90(13) . 2_565 ?
O24 V7 O14 105.09(9) . . ?
O13 V7 O14 82.90(13) 2_565 . ?
O13 V7 O14 84.59(13) . . ?
O14 V7 O14 149.83(18) 2_565 . ?
O24 V7 V10 118.43(2) . . ?
O13 V7 V10 110.02(10) 2_565 . ?
O13 V7 V10 42.17(10) . . ?
O14 V7 V10 119.35(10) 2_565 . ?
O14 V7 V10 42.44(9) . . ?
O24 V7 V10 118.43(2) . 2_565 ?
O13 V7 V10 42.17(10) 2_565 2_565 ?
O13 V7 V10 110.02(10) . 2_565 ?
O14 V7 V10 42.44(9) 2_565 2_565 ?
O14 V7 V10 119.35(10) . 2_565 ?
V10 V7 V10 123.14(5) . 2_565 ?
O24 V7 V11 117.97(2) . 2_565 ?
O13 V7 V11 110.90(10) 2_565 2_565 ?
O13 V7 V11 41.44(10) . 2_565 ?
O14 V7 V11 41.48(9) 2_565 2_565 ?
O14 V7 V11 120.34(10) . 2_565 ?
V10 V7 V11 80.00(3) . 2_565 ?
V10 V7 V11 74.16(3) 2_565 2_565 ?
O24 V7 V11 117.97(2) . . ?
O13 V7 V11 41.44(10) 2_565 . ?
O13 V7 V11 110.90(10) . . ?
O14 V7 V11 120.34(10) 2_565 . ?
O14 V7 V11 41.48(9) . . ?
V10 V7 V11 74.16(3) . . ?
V10 V7 V11 80.00(3) 2_565 . ?
V11 V7 V11 124.06(5) 2_565 . ?
O23 V8 O11 115.79(17) . . ?
O23 V8 O8 116.20(17) . . ?
O11 V8 O8 127.85(15) . . ?
O23 V8 O10 105.11(17) . . ?
O11 V8 O10 82.25(14) . . ?
O8 V8 O10 80.95(13) . . ?
O23 V8 O17 105.86(17) . 7_566 ?
O11 V8 O17 84.82(14) . 7_566 ?
O8 V8 O17 85.07(13) . 7_566 ?
O10 V8 O17 149.02(14) . 7_566 ?
O23 V8 V9 118.56(15) . 7_566 ?
O11 V8 V9 42.34(10) . 7_566 ?
O8 V8 V9 111.08(10) . 7_566 ?
O10 V8 V9 119.30(10) . 7_566 ?
O17 V8 V9 42.48(10) 7_566 7_566 ?
O23 V8 V11 118.25(13) . 7_566 ?
O11 V8 V11 111.56(10) . 7_566 ?
O8 V8 V11 42.36(9) . 7_566 ?
O10 V8 V11 118.62(10) . 7_566 ?
O17 V8 V11 42.72(9) 7_566 7_566 ?
V9 V8 V11 75.73(3) 7_566 7_566 ?
O23 V8 V10 118.61(13) . . ?
O11 V8 V10 40.51(10) . . ?
O8 V8 V10 107.21(10) . . ?
O10 V8 V10 41.76(9) . . ?
O17 V8 V10 119.52(10) 7_566 . ?
V9 V8 V10 79.53(3) 7_566 . ?
V11 V8 V10 123.10(4) 7_566 . ?
O23 V8 V9 118.96(15) . . ?
O11 V8 V9 107.31(11) . . ?
O8 V8 V9 40.27(10) . . ?
O10 V8 V9 40.72(9) . . ?
O17 V8 V9 119.49(10) 7_566 . ?
V9 V8 V9 122.45(4) 7_566 . ?
V11 V8 V9 79.51(3) 7_566 . ?
V10 V8 V9 72.19(3) . . ?
O21 V9 O17 100.62(17) . . ?
O21 V9 O11 102.90(17) . 8_666 ?
O17 V9 O11 85.94(14) . 8_666 ?
O21 V9 O10 99.68(17) . . ?
O17 V9 O10 95.93(14) . . ?
O11 V9 O10 156.61(14) 8_666 . ?
O21 V9 O8 102.21(17) . . ?
O17 V9 O8 157.17(14) . . ?
O11 V9 O8 88.65(14) 8_666 . ?
O10 V9 O8 80.61(14) . . ?
O21 V9 O9 166.46(15) . . ?
O17 V9 O9 71.02(12) . . ?
O11 V9 O9 87.40(13) 8_666 . ?
O10 V9 O9 71.36(12) . . ?
O8 V9 O9 86.60(12) . . ?
O21 V9 V8 106.08(15) . 8_666 ?
O17 V9 V8 44.88(10) . 8_666 ?
O11 V9 V8 41.06(10) 8_666 8_666 ?
O10 V9 V8 135.90(10) . 8_666 ?
O8 V9 V8 126.24(10) . 8_666 ?
O9 V9 V8 75.87(8) . 8_666 ?
O21 V9 V8 105.90(15) . . ?
O17 V9 V8 132.73(11) . . ?
O11 V9 V8 123.90(10) 8_666 . ?
O10 V9 V8 41.84(10) . . ?
O8 V9 V8 38.81(9) . . ?
O9 V9 V8 74.53(8) . . ?
V8 V9 V8 147.41(4) 8_666 . ?
O19 V10 O11 103.20(16) . . ?
O19 V10 O13 102.57(15) . . ?
O11 V10 O13 88.46(13) . . ?
O19 V10 O14 100.47(15) . . ?
O11 V10 O14 155.88(14) . . ?
O13 V10 O14 81.93(13) . . ?
O19 V10 O10 100.11(15) . . ?
O11 V10 O10 80.71(13) . . ?
O13 V10 O10 156.57(13) . . ?
O14 V10 O10 99.68(14) . . ?
O19 V10 O9 166.06(15) . . ?
O11 V10 O9 86.43(12) . . ?
O13 V10 O9 87.57(12) . . ?
O14 V10 O9 71.17(12) . . ?
O10 V10 O9 71.17(12) . . ?
O19 V10 V7 106.41(12) . . ?
O11 V10 V7 124.48(10) . . ?
O13 V10 V7 39.90(9) . . ?
O14 V10 V7 42.05(9) . . ?
O10 V10 V7 136.23(10) . . ?
O9 V10 V7 75.22(8) . . ?
O19 V10 V8 106.42(12) . . ?
O11 V10 V8 38.74(9) . . ?
O13 V10 V8 123.86(9) . . ?
O14 V10 V8 135.89(10) . . ?
O10 V10 V8 41.99(10) . . ?
O9 V10 V8 74.74(8) . . ?
V7 V10 V8 146.33(4) . . ?
O20 V11 O8 103.20(16) . 8_666 ?
O20 V11 O17 101.87(16) . . ?
O8 V11 O17 85.85(14) 8_666 . ?
O20 V11 O14 101.38(16) . . ?
O8 V11 O14 154.85(14) 8_666 . ?
O17 V11 O14 94.29(14) . . ?
O20 V11 O13 101.99(16) . 2_565 ?
O8 V11 O13 88.62(14) 8_666 2_565 ?
O17 V11 O13 156.14(14) . 2_565 ?
O14 V11 O13 81.12(13) . 2_565 ?
O20 V11 V8 106.45(13) . 8_666 ?
O8 V11 V8 41.10(10) 8_666 8_666 ?
O17 V11 V8 44.76(10) . 8_666 ?
O14 V11 V8 133.97(10) . 8_666 ?
O13 V11 V8 126.24(10) 2_565 8_666 ?
O20 V11 V7 106.48(13) . . ?
O8 V11 V7 124.02(11) 8_666 . ?
O17 V11 V7 130.99(11) . . ?
O14 V11 V7 41.64(10) . . ?
O13 V11 V7 39.50(9) 2_565 . ?
V8 V11 V7 146.62(4) 8_666 . ?
O9 P1 O9 109.6(2) 8_666 7_566 ?
O9 P1 O9 109.41(12) 8_666 . ?
O9 P1 O9 109.41(12) 7_566 . ?
O9 P1 O9 109.41(12) 8_666 2_565 ?
O9 P1 O9 109.41(12) 7_566 2_565 ?
O9 P1 O9 109.6(2) . 2_565 ?
V3 O2 V1 142.32(18) . . ?
V3 O2 V4 97.36(14) . . ?
V1 O2 V4 101.63(14) . . ?
V2 O3 V1 97.54(13) . . ?
V2 O3 V1 97.02(13) . 4_465 ?
V1 O3 V1 142.78(18) . 4_465 ?
V1 O4 Ni1 142.96(17) . . ?
V4 O5 V5 143.22(18) 4_465 . ?
V4 O5 V3 98.24(14) 4_465 . ?
V5 O5 V3 100.13(14) . . ?
V3 O6 V1 142.72(17) 3_665 . ?
V3 O6 V4 97.55(14) 3_665 . ?
V1 O6 V4 101.17(13) . . ?
V8 O8 V11 96.54(15) . 7_566 ?
V8 O8 V9 100.91(14) . . ?
V11 O8 V9 146.43(19) 7_566 . ?
P1 O9 V10 126.76(18) . . ?
P1 O9 V9 125.68(17) . . ?
V10 O9 V9 89.72(11) . . ?
V9 O10 V10 125.07(17) . . ?
V9 O10 V8 97.44(14) . . ?
V10 O10 V8 96.25(14) . . ?
V8 O11 V9 96.60(14) . 7_566 ?
V8 O11 V10 100.76(15) . . ?
V9 O11 V10 145.80(18) 7_566 . ?
V7 O13 V11 99.06(14) . 2_565 ?
V7 O13 V10 97.92(14) . . ?
V11 O13 V10 145.00(17) 2_565 . ?
V11 O14 V7 96.88(14) . . ?
V11 O14 V10 127.41(15) . . ?
V7 O14 V10 95.51(14) . . ?
V6 O15 V5 97.65(15) . 2_575 ?
V6 O15 V5 97.02(15) . 3_665 ?
V5 O15 V5 145.28(19) 2_575 3_665 ?
V9 O17 V11 129.88(18) . . ?
V9 O17 V8 92.64(14) . 8_666 ?
V11 O17 V8 92.52(14) . 8_666 ?
V4 O22 V5 143.47(19) . . ?
V4 O22 V3 97.52(14) . . ?
V5 O22 V3 100.39(15) . . ?
N1 C1 C2 112.8(5) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 N2 113.0(5) . . ?
C1 C2 H2A 109.0 . . ?
N2 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
N2 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 C4 112.2(4) . . ?
N2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N3 C4 C3 111.7(4) . . ?
N3 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N3 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
N5 C5 C6 111.1(5) . . ?
N5 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N5 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N4 C6 C5 111.9(5) . . ?
N4 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
N4 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N6 C7 C8 115.2(6) . . ?
N6 C7 H7A 108.5 . . ?
C8 C7 H7A 108.5 . . ?
N6 C7 H7B 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 N5 119.5(5) . . ?
C7 C8 H8A 107.5 . . ?
N5 C8 H8A 107.5 . . ?
C7 C8 H8B 107.5 . . ?
N5 C8 H8B 107.5 . . ?
H8A C8 H8B 107.0 . . ?
C1 N1 Ni1 108.3(3) . . ?
C1 N1 H1C 110.0 . . ?
Ni1 N1 H1C 110.0 . . ?
C1 N1 H1D 110.0 . . ?
Ni1 N1 H1D 110.0 . . ?
H1C N1 H1D 108.4 . . ?
C3 N2 C2 113.1(4) . . ?
C3 N2 Ni1 107.4(3) . . ?
C2 N2 Ni1 109.7(3) . . ?
C3 N2 H2C 108.9 . . ?
C2 N2 H2C 108.9 . . ?
Ni1 N2 H2C 108.9 . . ?
C4 N3 Ni1 110.2(3) . . ?
C4 N3 H3C 109.6 . . ?
Ni1 N3 H3C 109.6 . . ?
C4 N3 H3D 109.6 . . ?
Ni1 N3 H3D 109.6 . . ?
H3C N3 H3D 108.1 . . ?
C6 N4 Ni1 108.2(3) . . ?
C6 N4 H4C 110.1 . . ?
Ni1 N4 H4C 110.0 . . ?
C6 N4 H4D 110.0 . . ?
Ni1 N4 H4D 110.0 . . ?
H4C N4 H4D 108.4 . . ?
C5 N5 C8 113.7(4) . . ?
C5 N5 Ni1 106.2(3) . . ?
C8 N5 Ni1 114.7(3) . . ?
C5 N5 H5C 107.2 . . ?
C8 N5 H5C 107.2 . . ?
Ni1 N5 H5C 107.2 . . ?
C7 N6 H6C 109.5 . . ?
C7 N6 H6D 109.5 . . ?
H6C N6 H6D 109.5 . . ?
C7 N6 H6E 109.5 . . ?
H6C N6 H6E 109.5 . . ?
H6D N6 H6E 109.5 . . ?
C9 N7 H7C 109.3 . . ?
C9 N7 H7D 111.5 . . ?
H7C N7 H7D 109.5 . . ?
C11 N8 C10 129.26(17) . . ?
C11 N8 H8C 105.0 . . ?
C10 N8 H8C 105.0 . . ?
C11 N8 H8D 105.0 . . ?
C10 N8 H8D 105.0 . . ?
H8C N8 H8D 105.8 . . ?
C12 N9 H9C 109.5 . . ?
C12 N9 H9D 109.5 . . ?
H9C N9 H9D 109.5 . . ?
C12 N9 H9E 109.5 . . ?
H9C N9 H9E 109.5 . . ?
H9D N9 H9E 109.5 . . ?
N7 C9 C10 144.7(2) . . ?
N7 C9 H9A 100.7 . . ?
C10 C9 H9A 100.7 . . ?
N7 C9 H9B 100.7 . . ?
C10 C9 H9B 100.7 . . ?
H9A C9 H9B 104.4 . . ?
N8 C10 C9 122.91(16) . . ?
N8 C10 H10A 106.6 . . ?
C9 C10 H10A 106.6 . . ?
N8 C10 H10B 106.6 . . ?
C9 C10 H10B 106.6 . . ?
H10A C10 H10B 106.6 . . ?
C12 C11 N8 163.9(2) . . ?
C12 C11 H11A 95.0 . . ?
N8 C11 H11A 95.0 . . ?
C12 C11 H11B 95.0 . . ?
N8 C11 H11B 95.0 . . ?
H11A C11 H11B 103.2 . . ?
C11 C12 N9 155.3(3) . . ?
C11 C12 H12A 97.6 . . ?
N9 C12 H12A 97.6 . . ?
C11 C12 H12B 97.6 . . ?
N9 C12 H12B 97.6 . . ?
H12A C12 H12B 103.6 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         4.806
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.195


data_zzb-ce
_database_code_depnum_ccdc_archive 'CCDC 802909'
#TrackingRef '- ZZB-CE.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H155 N30 Ni4 O95 P V36'
_chemical_formula_weight         4676.59

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'
P P 0.1023 0.0942 '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   P4/n

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

_cell_length_a                   18.8231(7)
_cell_length_b                   18.8231(7)
_cell_length_c                   20.3320(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7203.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    196(2)
_cell_measurement_reflns_used    60
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      24.36

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4640
_exptl_absorpt_coefficient_mu    2.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7272
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      196(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  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35104
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6285
_reflns_number_gt                3849
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_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^)+(0.1000P)^2^+0.0000P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6285
_refine_ls_number_parameters     566
_refine_ls_number_restraints     257
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0698
_refine_ls_wR_factor_ref         0.2045
_refine_ls_wR_factor_gt          0.1932
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.002

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
Ni1 Ni 0.54384(3) 0.14297(3) 0.34175(3) 0.02666(17) Uani 1 1 d . . .
V1 V 0.31422(9) 0.43571(8) 0.54485(8) 0.0222(4) Uani 0.50 1 d P A 1
V1A V 0.32436(10) 0.46732(9) 0.60415(9) 0.0344(5) Uani 0.50 1 d PD A 2
V2 V 0.2500 0.2500 0.72355(10) 0.0546(6) Uani 1 4 d S . .
V3 V 0.2500 0.2500 0.34072(12) 0.0661(8) Uani 1 4 d S . .
V4 V 0.37496(5) 0.31064(5) 0.66554(4) 0.0339(3) Uani 1 1 d . A .
V5 V 0.42563(5) 0.33533(5) 0.52326(4) 0.0312(2) Uani 1 1 d . . .
V6 V 0.37658(4) 0.20633(4) 0.40658(4) 0.0224(2) Uani 1 1 d . . .
V7 V 0.43263(6) 0.79304(6) -0.00397(5) 0.0487(3) Uani 1 1 d . . .
V8 V 0.2500 0.7500 -0.19128(6) 0.0382(4) Uani 1 2 d S . .
V9 V 0.32623(5) 0.86152(5) -0.12247(5) 0.0420(3) Uani 1 1 d . . .
V10 V 0.36707(5) 0.68270(5) -0.12244(5) 0.0412(3) Uani 1 1 d . . .
V11 V 0.35907(9) 0.92696(8) 0.00000(7) 0.0847(5) Uani 1 1 d . . .
P1 P 0.2500 0.7500 0.0000 0.0251(6) Uani 1 4 d S . .
O1 O 0.34323(18) 0.51969(18) 0.54736(18) 0.0367(10) Uani 1 1 d D . .
O2 O 0.4336(2) 0.26692(18) 0.59676(17) 0.0388(11) Uani 1 1 d . A .
O3 O 0.50128(18) 0.37209(19) 0.51937(19) 0.0396(11) Uani 1 1 d . A .
O4 O 0.4286(2) 0.3370(2) 0.72157(18) 0.0508(12) Uani 1 1 d . . .
O5 O 0.28160(19) 0.3422(2) 0.69175(17) 0.0435(11) Uani 1 1 d . . .
O6 O 0.37657(19) 0.38282(19) 0.59702(16) 0.0376(11) Uani 1 1 d . A .
O7 O 0.38684(19) 0.13160(18) 0.47075(17) 0.0353(10) Uani 1 1 d . A .
O8 O 0.29187(17) 0.16449(18) 0.37317(17) 0.0332(10) Uani 1 1 d . A .
O9 O 0.4320(2) 0.25889(19) 0.47114(19) 0.0431(11) Uani 1 1 d . A .
O10 O 0.43717(16) 0.18495(17) 0.35336(16) 0.0263(9) Uani 1 1 d . A .
O11 O 0.2500 0.2500 0.8000(4) 0.079(3) Uani 1 4 d S . .
O12 O 0.2500 0.2500 0.2649(5) 0.088(4) Uani 1 4 d S . .
O13 O 0.5156(2) 0.8124(3) 0.0064(2) 0.0663(16) Uani 1 1 d . . .
O14 O 0.3482(2) 0.9183(2) -0.17911(18) 0.0520(13) Uani 1 1 d . . .
O15 O 0.2500 0.7500 -0.2702(3) 0.067(2) Uani 1 2 d S . .
O16 O 0.2708(2) 0.66375(19) -0.15221(16) 0.0408(11) Uani 1 1 d . . .
O17 O 0.3568(2) 0.6119(2) -0.05693(17) 0.0460(12) Uani 1 1 d . . .
O18 O 0.4119(2) 0.6414(2) -0.17895(18) 0.0545(13) Uani 1 1 d . . .
O19 O 0.4078(2) 0.8648(2) -0.06778(19) 0.0557(13) Uani 1 1 d . . .
O20 O 0.2837(2) 0.92087(19) -0.05727(17) 0.0443(12) Uani 1 1 d . . .
O21 O 0.4426(2) 0.7199(2) -0.0698(2) 0.0577(14) Uani 1 1 d . . .
O22 O 0.31439(18) 0.76534(18) -0.04301(15) 0.0302(9) Uani 1 1 d . . .
O23 O 0.34758(19) 0.7732(2) -0.16738(16) 0.0411(11) Uani 1 1 d . . .
O24 O 0.4029(3) 0.9998(3) 0.0005(2) 0.0861(19) Uani 1 1 d . . .
C1 C 0.5673(5) 0.2955(4) 0.3298(3) 0.083(3) Uani 1 1 d . . .
H1A H 0.5949 0.3319 0.3077 0.099 Uiso 1 1 calc R . .
H1B H 0.5205 0.3150 0.3386 0.099 Uiso 1 1 calc R . .
C2 C 0.6008(4) 0.2787(3) 0.3911(3) 0.057(2) Uani 1 1 d . . .
H2A H 0.5854 0.3131 0.4236 0.068 Uiso 1 1 d R . .
H2B H 0.6517 0.2842 0.3857 0.068 Uiso 1 1 d R . .
C3 C 0.6504(3) 0.1694(4) 0.4406(3) 0.0533(19) Uani 1 1 d . . .
H3A H 0.6800 0.2021 0.4651 0.064 Uiso 1 1 calc R . .
H3B H 0.6354 0.1321 0.4704 0.064 Uiso 1 1 calc R . .
C4 C 0.6924(3) 0.1380(3) 0.3879(3) 0.0477(18) Uani 1 1 d . . .
H4A H 0.7260 0.1046 0.4067 0.057 Uiso 1 1 calc R . .
H4B H 0.7193 0.1751 0.3661 0.057 Uiso 1 1 calc R . .
C5 C 0.4850(4) 0.0041(3) 0.3608(4) 0.080(2) Uani 1 1 d U . .
H5A H 0.5231 -0.0304 0.3575 0.096 Uiso 1 1 calc RD . .
H5B H 0.4452 -0.0193 0.3821 0.096 Uiso 1 1 calc R . .
C6 C 0.4639(3) 0.0232(4) 0.2963(3) 0.078(2) Uani 1 1 d U . .
H6A H 0.4150 0.0394 0.2978 0.093 Uiso 1 1 calc RD . .
H6B H 0.4652 -0.0190 0.2689 0.093 Uiso 1 1 calc RD . .
C7 C 0.4764(4) 0.1103(4) 0.2087(3) 0.0812(18) Uani 1 1 d DU . .
H7D H 0.5110 0.1432 0.1921 0.097 Uiso 1 1 d R B .
H7E H 0.4363 0.1375 0.2231 0.097 Uiso 1 1 d R . .
C8 C 0.4641(8) 0.0572(6) 0.1550(4) 0.078(2) Uani 0.50 1 d PDU B 1
H8A H 0.5068 0.0300 0.1465 0.094 Uiso 0.50 1 calc PR B 1
H8B H 0.4261 0.0248 0.1668 0.094 Uiso 0.50 1 calc PR B 1
C8A C 0.4425(6) 0.0737(7) 0.1512(5) 0.077(2) Uani 0.50 1 d PDU B 2
H8AA H 0.4066 0.0410 0.1674 0.093 Uiso 0.50 1 calc PR B 2
H8AB H 0.4188 0.1088 0.1241 0.093 Uiso 0.50 1 calc PR B 2
N1 N 0.5868(2) 0.2077(2) 0.4166(2) 0.0314(12) Uani 1 1 d . . .
H1C H 0.5548 0.2110 0.4500 0.038 Uiso 1 1 calc R . .
N2 N 0.5084(2) 0.0609(2) 0.4022(2) 0.0346(12) Uani 1 1 d . . .
H2C H 0.5438 0.0460 0.4285 0.041 Uiso 1 1 calc R . .
H2D H 0.4724 0.0762 0.4276 0.041 Uiso 1 1 calc R . .
N3 N 0.5059(3) 0.0772(2) 0.2653(2) 0.0449(15) Uani 1 1 d . B .
H3C H 0.5451 0.0541 0.2503 0.054 Uiso 1 1 calc R . .
N4 N 0.5599(2) 0.2342(2) 0.2859(2) 0.0349(12) Uani 1 1 d . . .
H4C H 0.5994 0.2294 0.2613 0.042 Uiso 1 1 calc R . .
H4D H 0.5228 0.2409 0.2586 0.042 Uiso 1 1 calc R . .
N5 N 0.6481(2) 0.1006(3) 0.3387(2) 0.0429(14) Uani 1 1 d . . .
H5C H 0.6469 0.0538 0.3477 0.051 Uiso 1 1 calc R . .
H5D H 0.6666 0.1064 0.2983 0.051 Uiso 1 1 calc R . .
N6A N 0.4937(5) 0.0341(6) 0.1104(5) 0.075(3) Uani 0.50 1 d PDU B 2
H6AA H 0.4711 0.0140 0.0768 0.113 Uiso 0.50 1 calc PR B 2
H6AB H 0.5145 0.0007 0.1346 0.113 Uiso 0.50 1 calc PR B 2
H6AC H 0.5266 0.0639 0.0951 0.113 Uiso 0.50 1 calc PR B 2
N6 N 0.4445(7) 0.0993(7) 0.0975(5) 0.095(3) Uani 0.50 1 d PDU B 1
H6C H 0.4395 0.0707 0.0628 0.143 Uiso 0.50 1 calc PR B 1
H6D H 0.4783 0.1311 0.0893 0.143 Uiso 0.50 1 calc PR B 1
H6E H 0.4037 0.1216 0.1052 0.143 Uiso 0.50 1 calc PR B 1
C9 C 0.3229(8) 0.5514(4) 0.7366(2) 0.157(2) Uani 0.50 1 d PDU C 1
H9A H 0.2877 0.5883 0.7299 0.189 Uiso 0.50 1 calc PR C 1
H9B H 0.3689 0.5741 0.7416 0.189 Uiso 0.50 1 calc PR C 1
C10 C 0.3061(4) 0.5123(3) 0.7960(3) 0.1555(17) Uani 0.50 1 d PDU C 1
H10A H 0.2867 0.4662 0.7845 0.187 Uiso 0.50 1 calc PRD C 1
H10B H 0.2705 0.5380 0.8210 0.187 Uiso 0.50 1 calc PR C 1
C11 C 0.3788(3) 0.42775(18) 0.8546(4) 0.1627(19) Uani 0.50 1 d PDU C 1
H11A H 0.3970 0.4091 0.8134 0.195 Uiso 0.50 1 calc PR C 1
H11B H 0.4207 0.4320 0.8822 0.195 Uiso 0.50 1 calc PR C 1
C12 C 0.34861(14) 0.3629(2) 0.8821(5) 0.1644(19) Uani 0.50 1 d PDU C 1
H12A H 0.3637 0.3222 0.8564 0.197 Uiso 0.50 1 calc PR C 1
H12B H 0.3649 0.3565 0.9269 0.197 Uiso 0.50 1 calc PR C 1
N7 N 0.3244(5) 0.5055(5) 0.6795(3) 0.100(3) Uani 0.50 1 d PDU C 1
H7A H 0.3219 0.5318 0.6432 0.150 Uiso 0.50 1 calc PR C 1
H7B H 0.2877 0.4758 0.6810 0.150 Uiso 0.50 1 calc PR C 1
H7C H 0.3647 0.4808 0.6793 0.150 Uiso 0.50 1 calc PR C 1
N8 N 0.3698(4) 0.5031(3) 0.8357(4) 0.1631(17) Uani 0.50 1 d PDU C 1
H8C H 0.3665 0.5301 0.8722 0.196 Uiso 0.50 1 calc PR C 1
H8D H 0.4080 0.5177 0.8128 0.196 Uiso 0.50 1 calc PR C 1
N9 N 0.27161(16) 0.3686(4) 0.8808(6) 0.175(3) Uani 0.50 1 d PDU C 1
H9C H 0.2526 0.3309 0.9005 0.263 Uiso 0.50 1 calc PR C 1
H9D H 0.2567 0.3706 0.8393 0.263 Uiso 0.50 1 calc PRD C 1
H9E H 0.2583 0.4078 0.9019 0.263 Uiso 0.50 1 calc PR C 1
O1W O 0.2500 0.2500 0.52985(12) 0.045(2) Uani 1 4 d SD . .
H1WA H 0.2593(7) 0.2637(5) 0.56610(19) 0.067 Uiso 0.25 1 d PD . .
H1WB H 0.2394(6) 0.2805(3) 0.5042(3) 0.067 Uiso 0.25 1 d PD . .
O2W O 0.2281(3) 0.3672(2) 0.16034(13) 0.066(3) Uani 0.50 1 d PDU D 1
H2WA H 0.231(3) 0.363(2) 0.1212(2) 0.119 Uiso 0.50 1 d PD E 1
H2WB H 0.2058(4) 0.3355(3) 0.1767(4) 0.119 Uiso 0.50 1 d PD F 1
O3W O 0.2426(3) 0.42782(19) 0.11187(16) 0.161(4) Uani 0.50 1 d PDU G 2
H3WA H 0.2588(4) 0.4541(4) 0.1389(3) 0.242 Uiso 0.50 1 d PD H 2
H3WB H 0.2239(4) 0.4471(5) 0.0813(3) 0.242 Uiso 0.50 1 d PD I 2
O4W O 0.2003(3) 0.40940(15) 0.24001(15) 0.110(4) Uani 0.50 1 d PD J 2
H4WA H 0.1840(5) 0.3701(2) 0.2378(5) 0.165 Uiso 0.50 1 d PD K 2
H4WB H 0.1944(5) 0.4280(3) 0.2750(2) 0.165 Uiso 0.50 1 d PD L 2

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
Ni1 0.0248(3) 0.0297(3) 0.0255(3) 0.0009(3) 0.0006(3) 0.0040(3)
V1 0.0237(8) 0.0174(8) 0.0256(8) -0.0019(7) -0.0042(7) -0.0027(7)
V1A 0.0308(10) 0.0313(10) 0.0412(10) -0.0116(8) -0.0074(8) -0.0015(9)
V2 0.0649(9) 0.0649(9) 0.0342(11) 0.000 0.000 0.000
V3 0.0676(10) 0.0676(10) 0.0632(15) 0.000 0.000 0.000
V4 0.0366(5) 0.0378(5) 0.0272(4) 0.0003(4) -0.0076(4) -0.0004(4)
V5 0.0276(5) 0.0338(5) 0.0324(5) 0.0009(4) -0.0086(4) -0.0081(4)
V6 0.0211(4) 0.0222(4) 0.0239(4) 0.0007(4) 0.0006(4) -0.0012(4)
V7 0.0391(6) 0.0741(8) 0.0330(5) 0.0040(5) 0.0023(5) -0.0068(6)
V8 0.0486(8) 0.0491(8) 0.0169(6) 0.000 0.000 0.0042(7)
V9 0.0514(6) 0.0454(6) 0.0290(5) 0.0061(4) 0.0082(5) -0.0029(5)
V10 0.0457(6) 0.0523(6) 0.0255(5) 0.0009(4) 0.0069(4) 0.0135(5)
V11 0.1016(11) 0.0838(10) 0.0687(9) 0.0005(8) -0.0032(8) -0.0249(9)
P1 0.0305(9) 0.0305(9) 0.0141(11) 0.000 0.000 0.000
O1 0.033(2) 0.0287(19) 0.048(2) -0.0047(17) -0.0045(17) -0.0028(17)
O2 0.051(2) 0.0285(19) 0.037(2) 0.0072(16) 0.0015(18) 0.0077(18)
O3 0.0234(19) 0.040(2) 0.055(2) -0.0063(19) -0.0063(17) -0.0045(18)
O4 0.064(3) 0.055(2) 0.033(2) -0.005(2) -0.015(2) -0.007(2)
O5 0.040(2) 0.057(2) 0.033(2) -0.0020(19) -0.0037(18) 0.005(2)
O6 0.043(2) 0.039(2) 0.0304(19) 0.0019(17) 0.0025(17) 0.0078(18)
O7 0.034(2) 0.035(2) 0.0364(19) 0.0146(17) -0.0032(17) -0.0060(17)
O8 0.0199(17) 0.040(2) 0.040(2) 0.0054(17) -0.0040(16) -0.0082(16)
O9 0.048(2) 0.0278(19) 0.053(2) -0.0166(18) -0.0235(19) 0.0024(18)
O10 0.0187(16) 0.0253(17) 0.0349(18) 0.0046(15) 0.0023(15) 0.0020(15)
O11 0.101(5) 0.101(5) 0.036(5) 0.000 0.000 0.000
O12 0.104(5) 0.104(5) 0.055(6) 0.000 0.000 0.000
O13 0.047(3) 0.102(4) 0.051(3) -0.005(3) -0.001(2) -0.018(3)
O14 0.074(3) 0.051(2) 0.032(2) 0.0114(19) 0.005(2) -0.008(2)
O15 0.097(5) 0.087(5) 0.018(3) 0.000 0.000 0.008(4)
O16 0.057(2) 0.045(2) 0.0206(18) 0.0005(17) 0.0024(17) 0.0109(19)
O17 0.061(2) 0.053(2) 0.0245(19) 0.0034(18) 0.0053(19) 0.012(2)
O18 0.061(3) 0.075(3) 0.028(2) 0.002(2) 0.0127(19) 0.029(2)
O19 0.052(2) 0.080(3) 0.035(2) 0.018(2) -0.0035(19) -0.028(2)
O20 0.069(3) 0.034(2) 0.030(2) -0.0009(17) 0.0047(19) -0.006(2)
O21 0.033(2) 0.095(3) 0.046(2) -0.016(2) 0.0036(19) 0.015(2)
O22 0.0328(19) 0.039(2) 0.0192(16) 0.0006(15) 0.0045(15) 0.0000(17)
O23 0.045(2) 0.056(2) 0.0217(18) 0.0021(17) 0.0105(17) 0.007(2)
O24 0.117(4) 0.066(3) 0.075(3) -0.006(3) -0.003(3) -0.040(3)
C1 0.160(8) 0.042(4) 0.046(4) 0.007(3) -0.011(5) -0.014(5)
C2 0.073(4) 0.045(4) 0.054(4) 0.000(3) -0.019(3) -0.023(3)
C3 0.051(4) 0.067(4) 0.041(3) 0.009(3) -0.016(3) -0.010(3)
C4 0.032(3) 0.046(3) 0.065(4) 0.017(3) 0.000(3) 0.008(3)
C5 0.099(5) 0.066(4) 0.074(4) 0.019(3) -0.018(4) -0.014(4)
C6 0.083(4) 0.094(4) 0.056(4) -0.010(4) 0.007(3) -0.030(4)
C7 0.087(3) 0.110(3) 0.047(3) -0.012(3) -0.006(3) -0.038(3)
C8 0.088(4) 0.106(4) 0.041(4) -0.005(4) -0.003(4) -0.050(4)
C8A 0.084(4) 0.106(4) 0.041(4) -0.006(4) -0.001(4) -0.049(4)
N1 0.024(2) 0.037(2) 0.032(2) 0.003(2) 0.0018(19) 0.001(2)
N2 0.032(2) 0.035(2) 0.037(2) 0.006(2) -0.009(2) 0.005(2)
N3 0.059(3) 0.032(3) 0.044(3) -0.005(2) 0.000(3) -0.005(2)
N4 0.039(3) 0.033(2) 0.032(2) 0.002(2) 0.011(2) -0.001(2)
N5 0.029(2) 0.050(3) 0.049(3) 0.008(2) 0.009(2) 0.006(2)
N6A 0.076(6) 0.104(6) 0.046(5) -0.011(5) 0.000(5) -0.041(6)
N6 0.100(5) 0.111(5) 0.074(5) 0.002(4) -0.016(4) -0.017(5)
C9 0.155(4) 0.159(4) 0.157(4) -0.010(3) -0.005(3) 0.002(3)
C10 0.156(3) 0.157(3) 0.153(3) -0.010(3) -0.003(3) 0.000(3)
C11 0.165(3) 0.163(3) 0.160(3) -0.010(3) -0.001(3) 0.000(3)
C12 0.165(3) 0.165(3) 0.163(3) -0.009(3) 0.000(3) -0.002(3)
N7 0.103(5) 0.106(5) 0.092(5) -0.016(4) -0.010(4) 0.008(4)
N8 0.163(3) 0.165(3) 0.161(3) -0.007(3) 0.000(3) -0.001(3)
N9 0.174(5) 0.180(5) 0.171(5) -0.011(4) 0.001(4) -0.005(4)
O1W 0.033(3) 0.033(3) 0.069(5) 0.000 0.000 0.000
O2W 0.059(4) 0.053(4) 0.087(5) -0.003(4) -0.006(4) 0.002(4)
O3W 0.148(7) 0.173(7) 0.162(7) 0.019(6) -0.007(6) 0.006(6)
O4W 0.125(8) 0.130(9) 0.076(6) 0.042(6) -0.060(6) 0.014(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.

Since there are 14 disorder atoms including V1, V1a, C8, C8a, N6,
N6a, C9, C10, C11, C12 N7, N8, N9, O2w, O3w and O4w, the organic amine can
not be refined steady. Also the anisotropic termal parameters are not
refined steady. Therefore all thermal parameters for half occupied atoms
(except V1 and V1a) and C-C, C-N distances related to half occupied C and N
are restrained. In addtion, all H-O bond distances and H-O-H angles are
restrained.
;

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
Ni1 N4 2.081(4) . ?
Ni1 N2 2.083(4) . ?
Ni1 N1 2.111(4) . ?
Ni1 N3 2.111(5) . ?
Ni1 N5 2.118(4) . ?
Ni1 O10 2.171(3) . ?
V1 O1 1.673(4) . ?
V1 O2 1.857(4) 3 ?
V1 O6 1.869(4) . ?
V1 O9 2.036(4) 3 ?
V1 O7 2.039(4) 3 ?
V1 V5 2.8553(18) 3 ?
V1 V5 2.8566(18) . ?
V1 V6 3.0482(18) 3 ?
V1A O1 1.559(4) . ?
V1A O2 1.838(4) 3 ?
V1A O6 1.875(4) . ?
V2 O11 1.555(9) . ?
V2 O5 1.945(4) 2 ?
V2 O5 1.945(4) 3 ?
V2 O5 1.945(4) . ?
V2 O5 1.945(4) 4 ?
V2 V4 2.8681(13) 2 ?
V2 V4 2.8681(13) . ?
V2 V4 2.8681(13) 4 ?
V2 V4 2.8681(13) 3 ?
V3 O12 1.541(10) . ?
V3 O8 1.910(3) 4 ?
V3 O8 1.910(3) 2 ?
V3 O8 1.910(3) . ?
V3 O8 1.910(3) 3 ?
V3 V6 2.8541(14) 4 ?
V3 V6 2.8541(14) 2 ?
V3 V6 2.8541(14) . ?
V3 V6 2.8541(14) 3 ?
V4 O4 1.602(4) . ?
V4 O5 1.918(4) 4 ?
V4 O5 1.930(4) . ?
V4 O6 1.946(4) . ?
V4 O2 1.963(4) . ?
V4 V5 3.0812(13) . ?
V5 O3 1.585(4) . ?
V5 O9 1.791(4) . ?
V5 O7 1.800(3) 3 ?
V5 O6 1.975(4) . ?
V5 O2 1.978(4) . ?
V5 V1 2.8553(18) 4 ?
V6 O10 1.623(3) . ?
V6 O8 1.904(3) . ?
V6 O8 1.911(3) 3 ?
V6 O7 1.928(3) . ?
V6 O9 1.947(4) . ?
V6 V1 3.0482(18) 4 ?
V7 O13 1.618(5) . ?
V7 O17 1.918(4) 8_665 ?
V7 O20 1.919(4) 7_565 ?
V7 O21 1.929(4) . ?
V7 O19 1.930(4) . ?
V7 O22 2.420(4) . ?
V7 V11 2.866(2) 7_565 ?
V7 V11 2.877(2) . ?
V8 O15 1.605(5) . ?
V8 O16 1.850(4) 2_565 ?
V8 O16 1.850(4) . ?
V8 O23 1.949(4) 2_565 ?
V8 O23 1.949(4) . ?
V8 V10 2.9017(11) 2_565 ?
V8 V10 2.9017(11) . ?
V8 V9 2.9021(12) . ?
V8 V9 2.9021(12) 2_565 ?
V9 O14 1.625(4) . ?
V9 O19 1.897(4) . ?
V9 O20 1.910(4) . ?
V9 O23 1.939(4) . ?
V9 O16 1.982(4) 2_565 ?
V9 O22 2.437(3) . ?
V9 V11 2.8461(17) . ?
V10 O18 1.624(4) . ?
V10 O17 1.894(4) . ?
V10 O21 1.912(4) . ?
V10 O16 1.943(4) . ?
V10 O23 1.967(4) . ?
V10 O22 2.452(3) . ?
V10 V11 2.8436(17) 7_565 ?
V11 O24 1.601(5) . ?
V11 O17 1.838(4) 8_665 ?
V11 O20 1.839(4) . ?
V11 O19 2.028(4) . ?
V11 O21 2.075(5) 8_665 ?
V11 V10 2.8436(17) 8_665 ?
V11 V7 2.866(2) 8_665 ?
P1 O22 1.522(3) 2_565 ?
P1 O22 1.522(3) 8_665 ?
P1 O22 1.522(3) 7_565 ?
P1 O22 1.522(3) . ?
O2 V1A 1.838(4) 4 ?
O2 V1 1.857(4) 4 ?
O5 V4 1.918(4) 3 ?
O7 V5 1.800(3) 4 ?
O7 V1 2.039(4) 4 ?
O8 V6 1.911(3) 4 ?
O9 V1 2.036(4) 4 ?
O16 V9 1.982(4) 2_565 ?
O17 V11 1.838(4) 7_565 ?
O17 V7 1.918(4) 7_565 ?
O20 V7 1.919(4) 8_665 ?
O21 V11 2.075(5) 7_565 ?
C1 C2 1.431(9) . ?
C1 N4 1.466(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.457(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.457(9) . ?
C3 N1 1.480(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N5 1.480(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.416(9) . ?
C5 N2 1.432(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N3 1.434(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.422(8) . ?
C7 C8 1.497(11) . ?
C7 C8A 1.499(11) . ?
C7 H7D 0.9601 . ?
C7 H7E 0.9599 . ?
C8 N6 1.459(13) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8A N6A 1.475(13) . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
N1 H1C 0.9100 . ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
N3 H3C 0.9100 . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
N5 H5C 0.9000 . ?
N5 H5D 0.9000 . ?
N6A H6AA 0.8900 . ?
N6A H6AB 0.8900 . ?
N6A H6AC 0.8900 . ?
N6 H6C 0.8900 . ?
N6 H6D 0.8900 . ?
N6 H6E 0.8900 . ?
C9 N7 1.445(8) . ?
C9 C10 1.449(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N8 1.457(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.458(4) . ?
C11 N8 1.480(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N9 1.454(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N7 H7C 0.8900 . ?
N8 H8C 0.9000 . ?
N8 H8D 0.9000 . ?
N9 H9C 0.8900 . ?
N9 H9D 0.8900 . ?
N9 H9E 0.8900 . ?
O1W H1WA 0.800(4) . ?
O1W H1WB 0.801(3) . ?
O2W H2WA 0.800(4) . ?
O2W H2WB 0.801(4) . ?
O3W H2WA 1.25(4) . ?
O3W H3WA 0.800(4) . ?
O3W H3WB 0.800(4) . ?
O4W H4WA 0.801(4) . ?
O4W H4WB 0.801(3) . ?

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
N4 Ni1 N2 168.57(16) . . ?
N4 Ni1 N1 82.03(16) . . ?
N2 Ni1 N1 97.23(16) . . ?
N4 Ni1 N3 97.51(17) . . ?
N2 Ni1 N3 83.77(17) . . ?
N1 Ni1 N3 177.22(18) . . ?
N4 Ni1 N5 99.21(17) . . ?
N2 Ni1 N5 92.01(17) . . ?
N1 Ni1 N5 83.32(17) . . ?
N3 Ni1 N5 94.06(19) . . ?
N4 Ni1 O10 83.87(14) . . ?
N2 Ni1 O10 84.80(15) . . ?
N1 Ni1 O10 93.77(14) . . ?
N3 Ni1 O10 88.90(16) . . ?
N5 Ni1 O10 175.39(16) . . ?
O1 V1 O2 105.73(18) . 3 ?
O1 V1 O6 106.32(18) . . ?
O2 V1 O6 100.52(17) 3 . ?
O1 V1 O9 105.99(18) . 3 ?
O2 V1 O9 82.05(16) 3 3 ?
O6 V1 O9 145.47(17) . 3 ?
O1 V1 O7 106.60(18) . 3 ?
O2 V1 O7 145.27(17) 3 3 ?
O6 V1 O7 82.24(15) . 3 ?
O9 V1 O7 77.21(15) 3 3 ?
O1 V1 V5 112.91(14) . 3 ?
O2 V1 V5 43.54(11) 3 3 ?
O6 V1 V5 132.13(13) . 3 ?
O9 V1 V5 38.57(11) 3 3 ?
O7 V1 V5 110.46(12) 3 3 ?
O1 V1 V5 112.96(14) . . ?
O2 V1 V5 132.61(14) 3 . ?
O6 V1 V5 43.44(11) . . ?
O9 V1 V5 111.12(12) 3 . ?
O7 V1 V5 38.81(10) 3 . ?
V5 V1 V5 131.00(7) 3 . ?
O1 V1 V6 114.49(14) . 3 ?
O2 V1 V6 114.33(13) 3 3 ?
O6 V1 V6 114.12(13) . 3 ?
O9 V1 V6 38.99(10) 3 3 ?
O7 V1 V6 38.48(10) 3 3 ?
V5 V1 V6 73.07(4) 3 3 ?
V5 V1 V6 73.14(4) . 3 ?
O1 V1A O2 111.8(2) . 3 ?
O1 V1A O6 111.08(19) . . ?
O2 V1A O6 101.00(18) 3 . ?
O11 V2 O5 109.41(12) . 2 ?
O11 V2 O5 109.41(12) . 3 ?
O5 V2 O5 83.66(8) 2 3 ?
O11 V2 O5 109.41(12) . . ?
O5 V2 O5 141.2(2) 2 . ?
O5 V2 O5 83.66(8) 3 . ?
O11 V2 O5 109.41(12) . 4 ?
O5 V2 O5 83.66(8) 2 4 ?
O5 V2 O5 141.2(2) 3 4 ?
O5 V2 O5 83.66(8) . 4 ?
O11 V2 V4 114.28(4) . 2 ?
O5 V2 V4 42.06(11) 2 2 ?
O5 V2 V4 41.70(11) 3 2 ?
O5 V2 V4 117.98(12) . 2 ?
O5 V2 V4 118.25(13) 4 2 ?
O11 V2 V4 114.28(4) . . ?
O5 V2 V4 117.98(12) 2 . ?
O5 V2 V4 118.25(13) 3 . ?
O5 V2 V4 42.06(11) . . ?
O5 V2 V4 41.70(11) 4 . ?
V4 V2 V4 131.44(8) 2 . ?
O11 V2 V4 114.28(4) . 4 ?
O5 V2 V4 41.70(11) 2 4 ?
O5 V2 V4 117.98(12) 3 4 ?
O5 V2 V4 118.25(13) . 4 ?
O5 V2 V4 42.06(11) 4 4 ?
V4 V2 V4 80.26(3) 2 4 ?
V4 V2 V4 80.26(3) . 4 ?
O11 V2 V4 114.28(4) . 3 ?
O5 V2 V4 118.25(13) 2 3 ?
O5 V2 V4 42.06(11) 3 3 ?
O5 V2 V4 41.70(11) . 3 ?
O5 V2 V4 117.98(12) 4 3 ?
V4 V2 V4 80.26(3) 2 3 ?
V4 V2 V4 80.26(3) . 3 ?
V4 V2 V4 131.44(8) 4 3 ?
O12 V3 O8 110.21(13) . 4 ?
O12 V3 O8 110.21(13) . 2 ?
O8 V3 O8 83.15(8) 4 2 ?
O12 V3 O8 110.21(13) . . ?
O8 V3 O8 83.15(8) 4 . ?
O8 V3 O8 139.6(3) 2 . ?
O12 V3 O8 110.21(13) . 3 ?
O8 V3 O8 139.6(3) 4 3 ?
O8 V3 O8 83.15(8) 2 3 ?
O8 V3 O8 83.15(8) . 3 ?
O12 V3 V6 117.98(5) . 4 ?
O8 V3 V6 41.47(10) 4 4 ?
O8 V3 V6 115.01(13) 2 4 ?
O8 V3 V6 41.68(10) . 4 ?
O8 V3 V6 115.17(13) 3 4 ?
O12 V3 V6 117.98(5) . 2 ?
O8 V3 V6 41.68(10) 4 2 ?
O8 V3 V6 41.47(10) 2 2 ?
O8 V3 V6 115.17(13) . 2 ?
O8 V3 V6 115.01(13) 3 2 ?
V6 V3 V6 77.29(4) 4 2 ?
O12 V3 V6 117.98(5) . . ?
O8 V3 V6 115.01(13) 4 . ?
O8 V3 V6 115.17(13) 2 . ?
O8 V3 V6 41.47(10) . . ?
O8 V3 V6 41.68(10) 3 . ?
V6 V3 V6 77.29(4) 4 . ?
V6 V3 V6 124.04(9) 2 . ?
O12 V3 V6 117.98(5) . 3 ?
O8 V3 V6 115.17(13) 4 3 ?
O8 V3 V6 41.68(10) 2 3 ?
O8 V3 V6 115.01(13) . 3 ?
O8 V3 V6 41.47(10) 3 3 ?
V6 V3 V6 124.04(9) 4 3 ?
V6 V3 V6 77.29(4) 2 3 ?
V6 V3 V6 77.29(4) . 3 ?
O4 V4 O5 106.62(19) . 4 ?
O4 V4 O5 106.40(19) . . ?
O5 V4 O5 84.8(2) 4 . ?
O4 V4 O6 106.42(18) . . ?
O5 V4 O6 146.71(16) 4 . ?
O5 V4 O6 89.82(16) . . ?
O4 V4 O2 106.38(19) . . ?
O5 V4 O2 89.96(15) 4 . ?
O5 V4 O2 146.93(16) . . ?
O6 V4 O2 76.94(15) . . ?
O4 V4 V2 110.38(15) . . ?
O5 V4 V2 42.43(12) 4 . ?
O5 V4 V2 42.46(12) . . ?
O6 V4 V2 125.80(12) . . ?
O2 V4 V2 125.98(11) . . ?
O4 V4 V5 115.20(15) . . ?
O5 V4 V5 119.80(11) 4 . ?
O5 V4 V5 119.65(11) . . ?
O6 V4 V5 38.54(10) . . ?
O2 V4 V5 38.75(10) . . ?
V2 V4 V5 134.42(5) . . ?
O3 V5 O9 105.14(19) . . ?
O3 V5 O7 105.83(18) . 3 ?
O9 V5 O7 97.00(17) . 3 ?
O3 V5 O6 105.09(18) . . ?
O9 V5 O6 147.58(17) . . ?
O7 V5 O6 85.80(15) 3 . ?
O3 V5 O2 104.69(18) . . ?
O9 V5 O2 85.35(16) . . ?
O7 V5 O2 147.58(16) 3 . ?
O6 V5 O2 75.91(15) . . ?
O3 V5 V1 112.23(14) . 4 ?
O9 V5 V1 45.13(13) . 4 ?
O7 V5 V1 131.45(12) 3 4 ?
O6 V5 V1 111.14(11) . 4 ?
O2 V5 V1 40.28(11) . 4 ?
O3 V5 V1 112.23(14) . . ?
O9 V5 V1 132.18(13) . . ?
O7 V5 V1 45.22(12) 3 . ?
O6 V5 V1 40.60(11) . . ?
O2 V5 V1 111.73(12) . . ?
V1 V5 V1 132.63(7) 4 . ?
O3 V5 V4 113.00(14) . . ?
O9 V5 V4 117.07(13) . . ?
O7 V5 V4 116.93(12) 3 . ?
O6 V5 V4 37.88(10) . . ?
O2 V5 V4 38.39(11) . . ?
V1 V5 V4 74.19(4) 4 . ?
V1 V5 V4 74.23(4) . . ?
O10 V6 O8 104.37(16) . . ?
O10 V6 O8 104.85(16) . 3 ?
O8 V6 O8 83.3(2) . 3 ?
O10 V6 O7 101.53(16) . . ?
O8 V6 O7 91.35(15) . . ?
O8 V6 O7 153.60(16) 3 . ?
O10 V6 O9 101.48(16) . . ?
O8 V6 O9 154.11(16) . . ?
O8 V6 O9 91.63(15) 3 . ?
O7 V6 O9 82.00(15) . . ?
O10 V6 V3 110.20(13) . . ?
O8 V6 V3 41.62(10) . . ?
O8 V6 V3 41.65(10) 3 . ?
O7 V6 V3 127.67(11) . . ?
O9 V6 V3 128.12(12) . . ?
O10 V6 V1 109.08(12) . 4 ?
O8 V6 V1 125.62(11) . 4 ?
O8 V6 V1 125.63(11) 3 4 ?
O7 V6 V1 41.14(11) . 4 ?
O9 V6 V1 41.15(12) . 4 ?
V3 V6 V1 140.72(6) . 4 ?
O13 V7 O17 101.4(2) . 8_665 ?
O13 V7 O20 101.3(2) . 7_565 ?
O17 V7 O20 90.10(16) 8_665 7_565 ?
O13 V7 O21 99.1(2) . . ?
O17 V7 O21 159.56(17) 8_665 . ?
O20 V7 O21 85.64(18) 7_565 . ?
O13 V7 O19 99.4(2) . . ?
O17 V7 O19 83.70(17) 8_665 . ?
O20 V7 O19 159.14(17) 7_565 . ?
O21 V7 O19 93.24(19) . . ?
O13 V7 O22 168.30(17) . . ?
O17 V7 O22 86.81(14) 8_665 . ?
O20 V7 O22 86.83(14) 7_565 . ?
O21 V7 O22 73.01(14) . . ?
O19 V7 O22 72.99(14) . . ?
O13 V7 V11 104.9(2) . 7_565 ?
O17 V7 V11 126.22(13) 8_665 7_565 ?
O20 V7 V11 39.28(12) 7_565 7_565 ?
O21 V7 V11 46.37(14) . 7_565 ?
O19 V7 V11 135.13(13) . 7_565 ?
O22 V7 V11 76.10(9) . 7_565 ?
O13 V7 V11 105.3(2) . . ?
O17 V7 V11 39.00(12) 8_665 . ?
O20 V7 V11 125.83(12) 7_565 . ?
O21 V7 V11 133.75(13) . . ?
O19 V7 V11 44.72(13) . . ?
O22 V7 V11 75.84(9) . . ?
V11 V7 V11 148.92(7) 7_565 . ?
O15 V8 O16 115.44(11) . 2_565 ?
O15 V8 O16 115.44(11) . . ?
O16 V8 O16 129.1(2) 2_565 . ?
O15 V8 O23 104.43(10) . 2_565 ?
O16 V8 O23 83.67(16) 2_565 2_565 ?
O16 V8 O23 84.04(16) . 2_565 ?
O15 V8 O23 104.43(10) . . ?
O16 V8 O23 84.04(16) 2_565 . ?
O16 V8 O23 83.67(16) . . ?
O23 V8 O23 151.1(2) 2_565 . ?
O15 V8 V10 118.84(3) . 2_565 ?
O16 V8 V10 41.29(12) 2_565 2_565 ?
O16 V8 V10 109.69(12) . 2_565 ?
O23 V8 V10 42.43(11) 2_565 2_565 ?
O23 V8 V10 119.84(11) . 2_565 ?
O15 V8 V10 118.84(3) . . ?
O16 V8 V10 109.69(12) 2_565 . ?
O16 V8 V10 41.29(12) . . ?
O23 V8 V10 119.84(11) 2_565 . ?
O23 V8 V10 42.43(11) . . ?
V10 V8 V10 122.32(6) 2_565 . ?
O15 V8 V9 118.82(3) . . ?
O16 V8 V9 42.50(12) 2_565 . ?
O16 V8 V9 108.85(12) . . ?
O23 V8 V9 120.50(11) 2_565 . ?
O23 V8 V9 41.59(11) . . ?
V10 V8 V9 80.05(3) 2_565 . ?
V10 V8 V9 73.01(3) . . ?
O15 V8 V9 118.82(3) . 2_565 ?
O16 V8 V9 108.85(12) 2_565 2_565 ?
O16 V8 V9 42.50(12) . 2_565 ?
O23 V8 V9 41.59(11) 2_565 2_565 ?
O23 V8 V9 120.50(11) . 2_565 ?
V10 V8 V9 73.01(3) 2_565 2_565 ?
V10 V8 V9 80.05(3) . 2_565 ?
V9 V8 V9 122.35(6) . 2_565 ?
O14 V9 O19 100.83(19) . . ?
O14 V9 O20 102.36(18) . . ?
O19 V9 O20 85.06(18) . . ?
O14 V9 O23 100.22(18) . . ?
O19 V9 O23 97.81(17) . . ?
O20 V9 O23 156.27(16) . . ?
O14 V9 O16 100.18(18) . 2_565 ?
O19 V9 O16 158.85(16) . 2_565 ?
O20 V9 O16 88.02(16) . 2_565 ?
O23 V9 O16 80.89(16) . 2_565 ?
O14 V9 O22 169.10(18) . . ?
O19 V9 O22 73.10(15) . . ?
O20 V9 O22 86.33(14) . . ?
O23 V9 O22 72.19(13) . . ?
O16 V9 O22 86.54(13) 2_565 . ?
O14 V9 V11 106.26(15) . . ?
O19 V9 V11 45.36(13) . . ?
O20 V9 V11 39.70(12) . . ?
O23 V9 V11 137.57(12) . . ?
O16 V9 V11 124.81(11) 2_565 . ?
O22 V9 V11 76.19(9) . . ?
O14 V9 V8 105.08(15) . . ?
O19 V9 V8 134.92(14) . . ?
O20 V9 V8 123.39(13) . . ?
O23 V9 V8 41.86(11) . . ?
O16 V9 V8 39.08(11) 2_565 . ?
O22 V9 V8 74.75(8) . . ?
V11 V9 V8 147.38(5) . . ?
O18 V10 O17 102.33(19) . . ?
O18 V10 O21 100.69(19) . . ?
O17 V10 O21 86.51(18) . . ?
O18 V10 O16 100.16(18) . . ?
O17 V10 O16 89.71(16) . . ?
O21 V10 O16 159.14(16) . . ?
O18 V10 O23 100.55(18) . . ?
O17 V10 O23 156.45(16) . . ?
O21 V10 O23 94.69(18) . . ?
O16 V10 O23 80.82(16) . . ?
O18 V10 O22 168.55(18) . . ?
O17 V10 O22 86.66(14) . . ?
O21 V10 O22 72.50(15) . . ?
O16 V10 O22 86.82(13) . . ?
O23 V10 O22 71.41(13) . . ?
O18 V10 V11 106.31(15) . 7_565 ?
O17 V10 V11 39.65(12) . 7_565 ?
O21 V10 V11 46.87(14) . 7_565 ?
O16 V10 V11 126.26(11) . 7_565 ?
O23 V10 V11 136.05(12) . 7_565 ?
O22 V10 V11 76.06(8) . 7_565 ?
O18 V10 V8 105.23(14) . . ?
O17 V10 V8 124.69(13) . . ?
O21 V10 V8 132.43(14) . . ?
O16 V10 V8 38.91(11) . . ?
O23 V10 V8 41.96(11) . . ?
O22 V10 V8 74.55(8) . . ?
V11 V10 V8 147.57(5) 7_565 . ?
O24 V11 O17 117.3(2) . 8_665 ?
O24 V11 O20 117.1(2) . . ?
O17 V11 O20 125.65(19) 8_665 . ?
O24 V11 O19 105.4(2) . . ?
O17 V11 O19 83.05(17) 8_665 . ?
O20 V11 O19 83.28(17) . . ?
O24 V11 O21 104.1(2) . 8_665 ?
O17 V11 O21 83.34(17) 8_665 8_665 ?
O20 V11 O21 83.61(18) . 8_665 ?
O19 V11 O21 150.48(18) . 8_665 ?
O24 V11 V10 118.48(19) . 8_665 ?
O17 V11 V10 41.09(12) 8_665 8_665 ?
O20 V11 V10 108.43(13) . 8_665 ?
O19 V11 V10 119.42(13) . 8_665 ?
O21 V11 V10 42.25(12) 8_665 8_665 ?
O24 V11 V9 119.22(19) . . ?
O17 V11 V9 107.73(13) 8_665 . ?
O20 V11 V9 41.55(12) . . ?
O19 V11 V9 41.73(12) . . ?
O21 V11 V9 120.24(13) 8_665 . ?
V10 V11 V9 122.30(6) 8_665 . ?
O24 V11 V7 118.9(2) . 8_665 ?
O17 V11 V7 107.79(14) 8_665 8_665 ?
O20 V11 V7 41.35(12) . 8_665 ?
O19 V11 V7 119.51(13) . 8_665 ?
O21 V11 V7 42.27(12) 8_665 8_665 ?
V10 V11 V7 73.38(5) 8_665 8_665 ?
V9 V11 V7 79.85(5) . 8_665 ?
O24 V11 V7 120.2(2) . . ?
O17 V11 V7 41.04(12) 8_665 . ?
O20 V11 V7 107.40(13) . . ?
O19 V11 V7 42.04(12) . . ?
O21 V11 V7 119.20(12) 8_665 . ?
V10 V11 V7 79.07(5) 8_665 . ?
V9 V11 V7 72.59(5) . . ?
V7 V11 V7 120.94(7) 8_665 . ?
O22 P1 O22 109.27(12) 2_565 8_665 ?
O22 P1 O22 109.27(12) 2_565 7_565 ?
O22 P1 O22 109.9(2) 8_665 7_565 ?
O22 P1 O22 109.9(2) 2_565 . ?
O22 P1 O22 109.27(12) 8_665 . ?
O22 P1 O22 109.27(12) 7_565 . ?
V1A O1 V1 49.53(13) . . ?
V1A O2 V1 43.13(11) 4 4 ?
V1A O2 V4 121.87(19) 4 . ?
V1 O2 V4 139.6(2) 4 . ?
V1A O2 V5 134.2(2) 4 . ?
V1 O2 V5 96.18(17) 4 . ?
V4 O2 V5 102.86(16) . . ?
V4 O5 V4 147.8(2) 3 . ?
V4 O5 V2 95.88(17) 3 . ?
V4 O5 V2 95.48(17) . . ?
V1 O6 V1A 42.53(11) . . ?
V1 O6 V4 140.2(2) . . ?
V1A O6 V4 121.92(19) . . ?
V1 O6 V5 95.95(16) . . ?
V1A O6 V5 133.4(2) . . ?
V4 O6 V5 103.58(17) . . ?
V5 O7 V6 141.6(2) 4 . ?
V5 O7 V1 95.97(16) 4 4 ?
V6 O7 V1 100.38(16) . 4 ?
V6 O8 V3 96.91(15) . . ?
V6 O8 V6 138.3(2) . 4 ?
V3 O8 V6 96.67(15) . 4 ?
V5 O9 V6 140.5(2) . . ?
V5 O9 V1 96.30(18) . 4 ?
V6 O9 V1 99.86(16) . 4 ?
V6 O10 Ni1 144.38(19) . . ?
V8 O16 V10 99.80(18) . . ?
V8 O16 V9 98.41(17) . 2_565 ?
V10 O16 V9 143.94(18) . 2_565 ?
V11 O17 V10 99.26(19) 7_565 . ?
V11 O17 V7 99.96(17) 7_565 7_565 ?
V10 O17 V7 145.6(2) . 7_565 ?
V9 O19 V7 124.6(2) . . ?
V9 O19 V11 92.91(18) . . ?
V7 O19 V11 93.24(17) . . ?
V11 O20 V9 98.75(19) . . ?
V11 O20 V7 99.36(17) . 8_665 ?
V9 O20 V7 146.4(2) . 8_665 ?
V10 O21 V7 125.3(2) . . ?
V10 O21 V11 90.88(19) . 7_565 ?
V7 O21 V11 91.35(17) . 7_565 ?
P1 O22 V7 125.78(17) . . ?
P1 O22 V9 126.49(19) . . ?
V7 O22 V9 88.47(12) . . ?
P1 O22 V10 125.46(19) . . ?
V7 O22 V10 88.90(12) . . ?
V9 O22 V10 89.87(11) . . ?
V9 O23 V8 96.55(16) . . ?
V9 O23 V10 124.21(17) . . ?
V8 O23 V10 95.61(17) . . ?
C2 C1 N4 113.4(6) . . ?
C2 C1 H1A 108.9 . . ?
N4 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
N4 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 N1 115.6(5) . . ?
C1 C2 H2A 108.4 . . ?
N1 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
N1 C2 H2B 108.4 . . ?
H2A C2 H2B 107.4 . . ?
C4 C3 N1 113.2(5) . . ?
C4 C3 H3A 108.9 . . ?
N1 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
N1 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C3 C4 N5 112.5(5) . . ?
C3 C4 H4A 109.1 . . ?
N5 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
N5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 N2 116.1(5) . . ?
C6 C5 H5A 108.3 . . ?
N2 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
N2 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
C5 C6 N3 115.6(6) . . ?
C5 C6 H6A 108.4 . . ?
N3 C6 H6A 108.4 . . ?
C5 C6 H6B 108.4 . . ?
N3 C6 H6B 108.4 . . ?
H6A C6 H6B 107.4 . . ?
N3 C7 C8 111.1(7) . . ?
N3 C7 C8A 126.6(7) . . ?
C8 C7 C8A 19.9(7) . . ?
N3 C7 H7D 107.6 . . ?
C8 C7 H7D 106.3 . . ?
C8A C7 H7D 108.2 . . ?
N3 C7 H7E 107.0 . . ?
C8 C7 H7E 117.2 . . ?
C8A C7 H7E 98.5 . . ?
H7D C7 H7E 107.3 . . ?
N6 C8 C7 105.2(9) . . ?
N6 C8 H8A 110.7 . . ?
C7 C8 H8A 110.7 . . ?
N6 C8 H8B 110.7 . . ?
C7 C8 H8B 110.7 . . ?
H8A C8 H8B 108.8 . . ?
N6A C8A C7 113.0(9) . . ?
N6A C8A H8AA 109.0 . . ?
C7 C8A H8AA 109.0 . . ?
N6A C8A H8AB 109.0 . . ?
C7 C8A H8AB 109.0 . . ?
H8AA C8A H8AB 107.8 . . ?
C2 N1 C3 114.8(5) . . ?
C2 N1 Ni1 110.0(3) . . ?
C3 N1 Ni1 105.4(3) . . ?
C2 N1 H1C 108.8 . . ?
C3 N1 H1C 108.8 . . ?
Ni1 N1 H1C 108.8 . . ?
C5 N2 Ni1 107.8(4) . . ?
C5 N2 H2C 110.1 . . ?
Ni1 N2 H2C 110.1 . . ?
C5 N2 H2D 110.1 . . ?
Ni1 N2 H2D 110.1 . . ?
H2C N2 H2D 108.5 . . ?
C7 N3 C6 116.8(5) . . ?
C7 N3 Ni1 118.2(4) . . ?
C6 N3 Ni1 106.2(4) . . ?
C7 N3 H3C 104.7 . . ?
C6 N3 H3C 104.7 . . ?
Ni1 N3 H3C 104.7 . . ?
C1 N4 Ni1 109.3(3) . . ?
C1 N4 H4C 109.8 . . ?
Ni1 N4 H4C 109.8 . . ?
C1 N4 H4D 109.8 . . ?
Ni1 N4 H4D 109.8 . . ?
H4C N4 H4D 108.3 . . ?
C4 N5 Ni1 108.9(3) . . ?
C4 N5 H5C 109.9 . . ?
Ni1 N5 H5C 109.9 . . ?
C4 N5 H5D 109.9 . . ?
Ni1 N5 H5D 109.9 . . ?
H5C N5 H5D 108.3 . . ?
C8A N6A H6AA 109.5 . . ?
C8A N6A H6AB 109.5 . . ?
H6AA N6A H6AB 109.5 . . ?
C8A N6A H6AC 109.5 . . ?
H6AA N6A H6AC 109.5 . . ?
H6AB N6A H6AC 109.5 . . ?
C8 N6 H6C 109.5 . . ?
C8 N6 H6D 109.5 . . ?
H6C N6 H6D 109.5 . . ?
C8 N6 H6E 109.5 . . ?
H6C N6 H6E 109.5 . . ?
H6D N6 H6E 109.5 . . ?
N7 C9 C10 111.7(7) . . ?
N7 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
N7 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 N8 110.1(7) . . ?
C9 C10 H10A 109.6 . . ?
N8 C10 H10A 109.6 . . ?
C9 C10 H10B 109.7 . . ?
N8 C10 H10B 109.6 . . ?
H10A C10 H10B 108.2 . . ?
C12 C11 N8 149.0(5) . . ?
C12 C11 H11A 99.5 . . ?
N8 C11 H11A 99.5 . . ?
C12 C11 H11B 99.5 . . ?
N8 C11 H11B 99.5 . . ?
H11A C11 H11B 104.0 . . ?
N9 C12 C11 108.7(5) . . ?
N9 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
N9 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C9 N7 H7A 109.5 . . ?
C9 N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
C9 N7 H7C 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
C10 N8 C11 110.6(5) . . ?
C10 N8 H8C 109.5 . . ?
C11 N8 H8C 109.5 . . ?
C10 N8 H8D 109.5 . . ?
C11 N8 H8D 109.5 . . ?
H8C N8 H8D 108.1 . . ?
C12 N9 H9C 109.5 . . ?
C12 N9 H9D 109.5 . . ?
H9C N9 H9D 109.5 . . ?
C12 N9 H9E 109.5 . . ?
H9C N9 H9E 109.5 . . ?
H9D N9 H9E 109.5 . . ?
H1WA O1W H1WB 115.1(8) . . ?
H2WA O2W H2WB 112(4) . . ?
H2WA O3W H3WA 124.4(11) . . ?
H2WA O3W H3WB 118.7(17) . . ?
H3WA O3W H3WB 114.9(8) . . ?
H4WA O4W H4WB 113.6(8) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.993
_refine_diff_density_min         -1.731
_refine_diff_density_rms         0.182