#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:08:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180413 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/82/7208298.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7208298
loop_
_publ_author_name
'Fu, Jie'
'Sun, Haixia'
'Xu, Yan'
'Wang, Congling'
'Zhu, Dunru'
'Sun, Qi'
'Liu, Hongke'
_publ_section_title
;
 [Ni(C17H20N4)4][H5PMoVI8VIV4O40(VIVO)2]·8H2O: confinement of
 heteropoly anions in Ni-containing rigid concave surfaces with high
 catalytic activity in the oxidation of styrene
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              5148
_journal_paper_doi               10.1039/c2ce25419k
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C68 H101 Mo8 N16 Ni O50 P V6'
_chemical_formula_weight         3105.49
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.7780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.688(4)
_cell_length_b                   15.4772(18)
_cell_length_c                   25.663(3)
_cell_measurement_temperature    296(2)
_cell_volume                     10235(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35327
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.757
_exptl_absorpt_correction_T_max  0.8439
_exptl_absorpt_correction_T_min  0.7663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             6152
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         9027
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0670P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                6340
_reflns_number_total             9027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25419k.txt
_cod_data_source_block           fj-11
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C2/c '
_cod_database_code               7208298
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Mo1 Mo 0.549300(14) 1.77779(3) -0.131071(16) 0.02369(10) Uani 1 1 d .
Mo2 Mo 0.593768(13) 1.77734(3) -0.238702(17) 0.02461(10) Uani 1 1 d .
Mo3 Mo 0.542143(14) 1.47042(3) -0.130981(16) 0.02381(10) Uani 1 1 d .
Mo4 Mo 0.590231(13) 1.47022(3) -0.247263(16) 0.02400(10) Uani 1 1 d .
P1 P 0.5000 1.62453(10) -0.2500 0.0190(4) Uani 1 2 d S
Ni1 Ni 0.5000 1.12435(5) -0.2500 0.0237(2) Uani 1 2 d S
V1 V 0.54505(3) 1.61850(5) -0.35790(3) 0.02279(19) Uani 1 1 d .
V2 V 0.63336(3) 1.63038(5) -0.12841(3) 0.0221(2) Uani 1 1 d .
V3 V 0.5000 1.36557(7) -0.2500 0.0221(3) Uani 1 2 d S
V4 V 0.5000 1.88353(7) -0.2500 0.0221(3) Uani 1 2 d S
O1 O 0.56470(12) 1.6351(2) -0.40512(14) 0.0395(9) Uani 1 1 d .
O2 O 0.69085(12) 1.6112(2) -0.07570(14) 0.0389(10) Uani 1 1 d .
O3 O 0.63327(11) 1.3896(2) -0.23408(14) 0.0332(9) Uani 1 1 d .
O4 O 0.57202(11) 1.39069(19) -0.07951(13) 0.0322(9) Uani 1 1 d D
O5 O 0.51580(10) 1.56774(18) -0.28730(12) 0.0229(8) Uani 1 1 d .
O6 O 0.58578(10) 1.69930(19) -0.29429(13) 0.0301(8) Uani 1 1 d .
O7 O 0.51211(10) 1.69940(19) -0.11756(12) 0.0278(8) Uani 1 1 d .
O8 O 0.52263(9) 1.40622(19) -0.30638(12) 0.0236(8) Uani 1 1 d .
O9 O 0.62797(11) 1.8589(2) -0.24679(14) 0.0363(9) Uani 1 1 d .
O10 O 0.62565(10) 1.54872(19) -0.18986(12) 0.0286(8) Uani 1 1 d .
O11 O 0.59279(11) 1.5490(2) -0.11106(12) 0.0301(9) Uani 1 1 d D
O12 O 0.50559(10) 1.52480(19) -0.10213(12) 0.0286(8) Uani 1 1 d .
O13 O 0.61208(10) 1.7228(2) -0.09355(12) 0.0299(9) Uani 1 1 d .
O14 O 0.64337(10) 1.7231(2) -0.17220(12) 0.0284(8) Uani 1 1 d .
O15 O 0.55883(12) 1.8579(2) -0.08198(13) 0.0333(9) Uani 1 1 d .
O16 O 0.59074(10) 1.52406(19) -0.31047(12) 0.0278(8) Uani 1 1 d .
O17 O 0.54635(10) 1.68134(18) -0.20760(12) 0.0226(8) Uani 1 1 d .
O18 O 0.51979(10) 1.82082(19) -0.29887(12) 0.0258(8) Uani 1 1 d .
O19 O 0.5000 1.9883(3) -0.2500 0.0290(12) Uani 1 2 d S
O20 O 0.56017(10) 1.42740(19) -0.19536(11) 0.0233(8) Uani 1 1 d .
O21 O 0.5000 1.2608(3) -0.2500 0.0284(12) Uani 1 2 d S
O22 O 0.56917(10) 1.8438(2) -0.18664(12) 0.0251(8) Uani 1 1 d D
C1 C 0.3379(2) 1.1824(4) -0.1107(3) 0.0711(17) Uani 1 1 d U
C2 C 0.3506(2) 1.1277(4) -0.1438(3) 0.0654(18) Uani 1 1 d U
C3 C 0.31132(19) 1.0940(4) -0.1997(3) 0.0629(16) Uani 1 1 d U
C4 C 0.2590(2) 1.1138(4) -0.2190(3) 0.0690(17) Uani 1 1 d U
C5 C 0.2471(2) 1.1672(5) -0.1854(3) 0.084(2) Uani 1 1 d .
H5A H 0.2125 1.1800 -0.1985 0.101 Uiso 1 1 calc R
C6 C 0.2853(2) 1.2029(4) -0.1323(3) 0.0774(18) Uani 1 1 d U
C7 C 0.2155(2) 1.0826(5) -0.2785(3) 0.097(3) Uani 1 1 d .
H7A H 0.1830 1.1028 -0.2837 0.145 Uiso 1 1 calc R
H7B H 0.2155 1.0206 -0.2793 0.145 Uiso 1 1 calc R
H7C H 0.2204 1.1046 -0.3103 0.145 Uiso 1 1 calc R
C8 C 0.4069(2) 1.1049(5) -0.1220(3) 0.091(3) Uani 1 1 d .
H8A H 0.4286 1.1321 -0.0839 0.137 Uiso 1 1 calc R
H8B H 0.4165 1.1248 -0.1506 0.137 Uiso 1 1 calc R
H8C H 0.4113 1.0434 -0.1176 0.137 Uiso 1 1 calc R
C9 C 0.2674(3) 1.2696(5) -0.1016(4) 0.121(3) Uani 1 1 d U
H9A H 0.2969 1.2894 -0.0651 0.181 Uiso 1 1 calc R
H9B H 0.2429 1.2432 -0.0926 0.181 Uiso 1 1 calc R
H9C H 0.2514 1.3178 -0.1281 0.181 Uiso 1 1 calc R
C10 C 0.3783(3) 1.2217(4) -0.0541(3) 0.087(2) Uani 1 1 d U
H10A H 0.3639 1.2321 -0.0280 0.104 Uiso 1 1 calc R
H10B H 0.4068 1.1813 -0.0339 0.104 Uiso 1 1 calc R
C11 C 0.3252(2) 1.0415(4) -0.2376(3) 0.078(2) Uani 1 1 d .
H11A H 0.3436 0.9902 -0.2156 0.093 Uiso 1 1 calc R
H11B H 0.2937 1.0231 -0.2732 0.093 Uiso 1 1 calc R
C12 C 0.4331(3) 1.4360(6) -0.0458(3) 0.130(3) Uani 1 1 d DU
H12A H 0.4476 1.4886 -0.0278 0.155 Uiso 1 1 calc R
C13 C 0.4271(3) 1.3621(5) -0.0190(4) 0.120(2) Uani 1 1 d DU
H13A H 0.4401 1.3537 0.0219 0.144 Uiso 1 1 calc R
C14 C 0.3889(3) 1.3384(5) -0.1146(3) 0.092(2) Uani 1 1 d U
H14A H 0.3681 1.3134 -0.1520 0.110 Uiso 1 1 calc R
C15 C 0.3514(2) 1.1729(4) -0.2730(3) 0.0575(18) Uani 1 1 d .
H15A H 0.3245 1.2095 -0.2789 0.069 Uiso 1 1 calc R
C16 C 0.39224(18) 1.1928(4) -0.2800(2) 0.0458(16) Uani 1 1 d .
H16A H 0.3979 1.2465 -0.2919 0.055 Uiso 1 1 calc R
C17 C 0.40223(17) 1.0636(3) -0.2530(2) 0.0484(16) Uani 1 1 d .
H17A H 0.4159 1.0083 -0.2420 0.058 Uiso 1 1 calc R
C18 C 0.1760(3) 1.2110(6) -0.5758(3) 0.097(3) Uani 1 1 d .
H18A H 0.1493 1.2281 -0.5689 0.116 Uiso 1 1 calc R
C19 C 0.1821(2) 1.1306(6) -0.5895(3) 0.089(3) Uani 1 1 d .
H19A H 0.1618 1.0828 -0.5931 0.107 Uiso 1 1 calc R
C20 C 0.2419(2) 1.2144(4) -0.5868(3) 0.0657(19) Uani 1 1 d U
H20A H 0.2707 1.2333 -0.5889 0.079 Uiso 1 1 calc R
C21 C 0.30463(19) 1.1275(3) -0.6497(2) 0.0433(16) Uani 1 1 d .
C22 C 0.35389(19) 1.1474(3) -0.6371(2) 0.0408(15) Uani 1 1 d .
H22A H 0.3579 1.1814 -0.6645 0.049 Uiso 1 1 calc R
C23 C 0.39823(18) 1.1197(3) -0.5858(2) 0.0344(13) Uani 1 1 d .
C24 C 0.39093(16) 1.0718(3) -0.54418(18) 0.0272(12) Uani 1 1 d .
C25 C 0.34127(17) 1.0533(3) -0.5544(2) 0.0336(13) Uani 1 1 d .
C26 C 0.29785(18) 1.0812(4) -0.6079(2) 0.0427(15) Uani 1 1 d .
C27 C 0.45157(18) 1.1412(4) -0.5770(2) 0.0514(17) Uani 1 1 d .
H27A H 0.4778 1.1173 -0.5397 0.077 Uiso 1 1 calc R
H27B H 0.4557 1.2028 -0.5763 0.077 Uiso 1 1 calc R
H27C H 0.4549 1.1172 -0.6095 0.077 Uiso 1 1 calc R
C28 C 0.3340(2) 1.0023(4) -0.5089(2) 0.0575(18) Uani 1 1 d .
H28A H 0.3673 0.9877 -0.4754 0.086 Uiso 1 1 calc R
H28B H 0.3150 0.9503 -0.5272 0.086 Uiso 1 1 calc R
H28C H 0.3150 1.0364 -0.4951 0.086 Uiso 1 1 calc R
C29 C 0.2600(2) 1.1614(5) -0.7086(3) 0.079(3) Uani 1 1 d .
H29A H 0.2737 1.1909 -0.7306 0.118 Uiso 1 1 calc R
H29B H 0.2394 1.2008 -0.7003 0.118 Uiso 1 1 calc R
H29C H 0.2388 1.1140 -0.7320 0.118 Uiso 1 1 calc R
C30 C 0.24399(19) 1.0621(4) -0.6191(3) 0.0578(19) Uani 1 1 d .
H30A H 0.2208 1.0541 -0.6618 0.069 Uiso 1 1 calc R
H30B H 0.2445 1.0090 -0.5988 0.069 Uiso 1 1 calc R
C31 C 0.43792(16) 1.0386(3) -0.48808(18) 0.0308(13) Uani 1 1 d .
H31A H 0.4313 0.9799 -0.4804 0.037 Uiso 1 1 calc R
H31B H 0.4674 1.0373 -0.4946 0.037 Uiso 1 1 calc R
C32 C 0.4712(2) 1.2012(4) -0.3741(2) 0.0583(19) Uani 1 1 d .
H32A H 0.4779 1.2571 -0.3588 0.070 Uiso 1 1 calc R
C33 C 0.4554(2) 1.1795(3) -0.4318(2) 0.0546(18) Uani 1 1 d .
H33A H 0.4490 1.2172 -0.4629 0.066 Uiso 1 1 calc R
C34 C 0.46426(16) 1.0640(3) -0.37913(19) 0.0308(13) Uani 1 1 d .
H34A H 0.4652 1.0063 -0.3686 0.037 Uiso 1 1 calc R
N1 N 0.4127(2) 1.4131(5) -0.1059(2) 0.1052(19) Uani 1 1 d DU
N2 N 0.3984(2) 1.3040(4) -0.0637(2) 0.0865(17) Uani 1 1 d U
N3 N 0.35746(15) 1.0887(3) -0.2556(2) 0.0529(14) Uani 1 1 d .
N4 N 0.42376(13) 1.1237(2) -0.26710(17) 0.0312(11) Uani 1 1 d .
N5 N 0.47575(14) 1.1284(2) -0.34193(16) 0.0330(11) Uani 1 1 d .
N6 N 0.45073(14) 1.0920(3) -0.43545(16) 0.0309(11) Uani 1 1 d .
N7 N 0.22461(16) 1.1328(3) -0.5974(2) 0.0551(15) Uani 1 1 d U
N8 N 0.2134(2) 1.2654(4) -0.5729(2) 0.089(2) Uani 1 1 d .
O1W O 0.7116(5) 1.8121(9) -0.0210(5) 0.166(5) Uani 0.50 1 d PU
H1WA H 0.6837 1.8079 -0.0221 0.249 Uiso 0.50 1 d PR
H1WB H 0.7143 1.8484 -0.0429 0.249 Uiso 0.50 1 d PRD
O2W O 0.6746(4) 1.5147(6) 0.0248(4) 0.101(4) Uani 0.50 1 d PD
H2WA H 0.6505(11) 1.5612(13) 0.0018(9) 0.151 Uiso 0.50 1 d PD
H2WB H 0.6616(16) 1.4844(17) -0.0132(7) 0.151 Uiso 0.50 1 d PD
O3W O 0.6672(3) 1.9320(5) -0.1148(3) 0.189(3) Uiso 1 1 d D
H3WA H 0.6339(5) 1.9538(13) -0.130(2) 0.283 Uiso 1 1 d D
H3WB H 0.6590(7) 1.8807(10) -0.1355(8) 0.283 Uiso 1 1 d D
O4W O 0.2323(3) 1.4357(5) -0.5676(3) 0.182(4) Uani 1 1 d .
H4WA H 0.2547 1.4365 -0.5781 0.273 Uiso 1 1 d R
H4WB H 0.2340 1.4755 -0.5455 0.273 Uiso 1 1 d R
O5W O 0.6385(2) 1.3435(5) 0.0481(2) 0.139(3) Uani 1 1 d D
H5WA H 0.6132(7) 1.3864(14) 0.0296(8) 0.208 Uiso 1 1 d D
H5WB H 0.6368(9) 1.324(2) 0.0130(7) 0.208 Uiso 1 1 d D
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O15 Mo1 O7 104.17(15) . .
O15 Mo1 O13 101.50(14) . .
O7 Mo1 O13 98.54(13) . .
O15 Mo1 O18 98.02(13) . 2_654
O7 Mo1 O18 86.87(12) . 2_654
O13 Mo1 O18 157.74(13) . 2_654
O15 Mo1 O22 98.77(14) . .
O7 Mo1 O22 152.42(11) . .
O13 Mo1 O22 91.59(13) . .
O18 Mo1 O22 74.85(11) 2_654 .
O15 Mo1 O17 168.01(14) . .
O7 Mo1 O17 87.82(12) . .
O13 Mo1 O17 76.01(11) . .
O18 Mo1 O17 82.67(10) 2_654 .
O22 Mo1 O17 69.77(11) . .
O15 Mo1 V4 99.69(10) . .
O7 Mo1 V4 120.81(8) . .
O13 Mo1 V4 128.37(10) . .
O18 Mo1 V4 36.19(9) 2_654 .
O22 Mo1 V4 38.68(7) . .
O17 Mo1 V4 73.76(7) . .
O9 Mo2 O6 104.76(16) . .
O9 Mo2 O14 101.78(14) . .
O6 Mo2 O14 99.30(13) . .
O9 Mo2 O18 98.30(13) . .
O6 Mo2 O18 87.33(12) . .
O14 Mo2 O18 156.41(13) . .
O9 Mo2 O22 97.62(14) . .
O6 Mo2 O22 153.18(12) . .
O14 Mo2 O22 90.26(12) . .
O18 Mo2 O22 74.83(11) . .
O9 Mo2 O17 166.36(13) . .
O6 Mo2 O17 88.87(13) . .
O14 Mo2 O17 74.97(11) . .
O18 Mo2 O17 82.60(11) . .
O22 Mo2 O17 69.38(11) . .
O9 Mo2 V4 99.04(11) . .
O6 Mo2 V4 121.44(9) . .
O14 Mo2 V4 126.97(10) . .
O18 Mo2 V4 36.19(8) . .
O22 Mo2 V4 38.67(7) . .
O17 Mo2 V4 73.61(7) . .
O4 Mo3 O12 102.04(15) . .
O4 Mo3 O11 103.29(13) . .
O12 Mo3 O11 99.01(14) . .
O4 Mo3 O8 100.47(13) . 2_654
O12 Mo3 O8 91.54(12) . 2_654
O11 Mo3 O8 151.26(13) . 2_654
O4 Mo3 O20 98.27(14) . .
O12 Mo3 O20 157.19(11) . .
O11 Mo3 O20 86.21(13) . .
O8 Mo3 O20 74.54(11) 2_654 .
O4 Mo3 O5 168.99(12) . 2_654
O12 Mo3 O5 75.80(11) . 2_654
O11 Mo3 O5 87.71(11) . 2_654
O8 Mo3 O5 68.99(10) 2_654 2_654
O20 Mo3 O5 82.29(10) . 2_654
O4 Mo3 V3 100.60(10) . .
O12 Mo3 V3 128.03(8) . .
O11 Mo3 V3 120.14(10) . .
O8 Mo3 V3 38.36(9) 2_654 .
O20 Mo3 V3 36.21(7) . .
O5 Mo3 V3 73.32(7) 2_654 .
O3 Mo4 O10 104.98(13) . .
O3 Mo4 O16 100.06(15) . .
O10 Mo4 O16 99.21(13) . .
O3 Mo4 O20 99.25(14) . .
O10 Mo4 O20 87.25(13) . .
O16 Mo4 O20 157.25(11) . .
O3 Mo4 O8 98.88(13) . .
O10 Mo4 O8 152.37(13) . .
O16 Mo4 O8 90.00(12) . .
O20 Mo4 O8 75.21(11) . .
O3 Mo4 O5 166.85(12) . .
O10 Mo4 O5 88.03(11) . .
O16 Mo4 O5 75.51(12) . .
O20 Mo4 O5 83.00(10) . .
O8 Mo4 O5 69.03(10) . .
O3 Mo4 V3 100.19(11) . .
O10 Mo4 V3 121.34(11) . .
O16 Mo4 V3 127.23(8) . .
O20 Mo4 V3 36.38(7) . .
O8 Mo4 V3 38.87(8) . .
O5 Mo4 V3 73.88(7) . .
O5 P1 O5 110.1(2) 2_654 .
O5 P1 O17 109.24(14) 2_654 .
O5 P1 O17 109.01(15) . .
O5 P1 O17 109.00(15) 2_654 2_654
O5 P1 O17 109.24(14) . 2_654
O17 P1 O17 110.2(2) . 2_654
N4 Ni1 N4 179.4(2) . 2_654
N4 Ni1 N5 91.90(16) . .
N4 Ni1 N5 88.12(16) 2_654 .
N4 Ni1 N5 88.12(16) . 2_654
N4 Ni1 N5 91.90(16) 2_654 2_654
N5 Ni1 N5 176.6(2) . 2_654
N4 Ni1 O19 89.72(11) . 1_545
N4 Ni1 O19 89.71(11) 2_654 1_545
N5 Ni1 O19 91.71(10) . 1_545
N5 Ni1 O19 91.71(10) 2_654 1_545
N4 Ni1 O21 90.29(11) . .
N4 Ni1 O21 90.28(11) 2_654 .
N5 Ni1 O21 88.29(10) . .
N5 Ni1 O21 88.29(10) 2_654 .
O19 Ni1 O21 180.000(1) 1_545 .
O1 V1 O6 102.97(15) . .
O1 V1 O7 103.77(15) . 2_654
O6 V1 O7 86.34(12) . 2_654
O1 V1 O16 100.96(15) . .
O6 V1 O16 90.47(12) . .
O7 V1 O16 155.15(14) 2_654 .
O1 V1 O12 101.20(15) . 2_654
O6 V1 O12 155.78(14) . 2_654
O7 V1 O12 89.31(12) 2_654 2_654
O16 V1 O12 83.56(12) . 2_654
O2 V2 O14 102.85(15) . .
O2 V2 O11 102.10(15) . .
O14 V2 O11 155.02(11) . .
O2 V2 O10 102.28(15) . .
O14 V2 O10 90.06(13) . .
O11 V2 O10 85.86(13) . .
O2 V2 O13 101.63(15) . .
O14 V2 O13 84.30(14) . .
O11 V2 O13 89.51(14) . .
O10 V2 O13 156.09(11) . .
O21 V3 O20 120.36(9) . .
O21 V3 O20 120.36(9) . 2_654
O20 V3 O20 119.28(18) . 2_654
O21 V3 O8 108.57(9) . .
O20 V3 O8 80.94(12) . .
O20 V3 O8 80.54(12) 2_654 .
O21 V3 O8 108.57(9) . 2_654
O20 V3 O8 80.54(12) . 2_654
O20 V3 O8 80.94(12) 2_654 2_654
O8 V3 O8 142.87(18) . 2_654
O21 V3 Mo4 121.487(18) . 2_654
O20 V3 Mo4 103.85(10) . 2_654
O20 V3 Mo4 39.88(9) 2_654 2_654
O8 V3 Mo4 114.90(9) . 2_654
O8 V3 Mo4 41.10(7) 2_654 2_654
O21 V3 Mo4 121.487(18) . .
O20 V3 Mo4 39.88(9) . .
O20 V3 Mo4 103.85(10) 2_654 .
O8 V3 Mo4 41.10(7) . .
O8 V3 Mo4 114.90(9) 2_654 .
Mo4 V3 Mo4 117.03(4) 2_654 .
O21 V3 Mo3 121.345(18) . .
O20 V3 Mo3 40.53(9) . .
O20 V3 Mo3 103.55(9) 2_654 .
O8 V3 Mo3 115.74(9) . .
O8 V3 Mo3 40.05(7) 2_654 .
Mo4 V3 Mo3 70.875(17) 2_654 .
Mo4 V3 Mo3 77.54(2) . .
O21 V3 Mo3 121.345(18) . 2_654
O20 V3 Mo3 103.55(9) . 2_654
O20 V3 Mo3 40.53(9) 2_654 2_654
O8 V3 Mo3 40.05(7) . 2_654
O8 V3 Mo3 115.74(9) 2_654 2_654
Mo4 V3 Mo3 77.54(2) 2_654 2_654
Mo4 V3 Mo3 70.875(17) . 2_654
Mo3 V3 Mo3 117.31(4) . 2_654
O19 V4 O18 120.80(10) . .
O19 V4 O18 120.80(10) . 2_654
O18 V4 O18 118.39(19) . 2_654
O19 V4 O22 108.09(9) . 2_654
O18 V4 O22 80.41(12) . 2_654
O18 V4 O22 81.29(12) 2_654 2_654
O19 V4 O22 108.09(9) . .
O18 V4 O22 81.29(12) . .
O18 V4 O22 80.41(12) 2_654 .
O22 V4 O22 143.82(18) 2_654 .
O19 V4 Mo1 121.701(18) . 2_654
O18 V4 Mo1 39.79(8) . 2_654
O18 V4 Mo1 103.31(9) 2_654 2_654
O22 V4 Mo1 40.64(9) 2_654 2_654
O22 V4 Mo1 115.63(9) . 2_654
O19 V4 Mo1 121.701(18) . .
O18 V4 Mo1 103.31(9) . .
O18 V4 Mo1 39.79(8) 2_654 .
O22 V4 Mo1 115.63(9) 2_654 .
O22 V4 Mo1 40.64(9) . .
Mo1 V4 Mo1 116.60(4) 2_654 .
O19 V4 Mo2 121.790(18) . 2_654
O18 V4 Mo2 102.96(9) . 2_654
O18 V4 Mo2 40.20(7) 2_654 2_654
O22 V4 Mo2 41.12(9) 2_654 2_654
O22 V4 Mo2 115.23(9) . 2_654
Mo1 V4 Mo2 70.654(18) 2_654 2_654
Mo1 V4 Mo2 77.150(19) . 2_654
O19 V4 Mo2 121.790(18) . .
O18 V4 Mo2 40.20(7) . .
O18 V4 Mo2 102.96(9) 2_654 .
O22 V4 Mo2 115.23(9) 2_654 .
O22 V4 Mo2 41.12(9) . .
Mo1 V4 Mo2 77.150(19) 2_654 .
Mo1 V4 Mo2 70.654(18) . .
Mo2 V4 Mo2 116.42(4) 2_654 .
P1 O5 Mo4 125.78(14) . .
P1 O5 Mo3 125.59(14) . 2_654
Mo4 O5 Mo3 94.81(10) . 2_654
Mo2 O6 V1 152.70(18) . .
Mo1 O7 V1 153.95(16) . 2_654
V3 O8 Mo3 101.59(13) . 2_654
V3 O8 Mo4 100.03(12) . .
Mo3 O8 Mo4 122.24(15) 2_654 .
Mo4 O10 V2 153.14(18) . .
Mo3 O11 V2 154.09(17) . .
Mo3 O12 V1 126.19(16) . 2_654
Mo1 O13 V2 125.26(14) . .
Mo2 O14 V2 127.07(15) . .
Mo4 O16 V1 125.72(17) . .
P1 O17 Mo1 125.65(16) . .
P1 O17 Mo2 125.19(15) . .
Mo1 O17 Mo2 95.46(10) . .
V4 O18 Mo1 104.02(13) . 2_654
V4 O18 Mo2 103.62(12) . .
Mo1 O18 Mo2 140.81(16) 2_654 .
V4 O19 Ni1 180.000(2) . 1_565
V3 O20 Mo4 103.74(12) . .
V3 O20 Mo3 103.26(13) . .
Mo4 O20 Mo3 141.21(15) . .
V3 O21 Ni1 180.000(1) . .
V4 O22 Mo1 100.68(13) . .
V4 O22 Mo2 100.22(12) . .
Mo1 O22 Mo2 120.66(15) . .
C2 C1 C6 118.9(6) . .
C2 C1 C10 121.5(6) . .
C6 C1 C10 119.5(7) . .
C1 C2 C3 120.6(5) . .
C1 C2 C8 120.2(6) . .
C3 C2 C8 119.2(6) . .
C4 C3 C2 118.9(6) . .
C4 C3 C11 120.5(5) . .
C2 C3 C11 120.6(5) . .
C5 C4 C3 119.7(6) . .
C5 C4 C7 118.4(6) . .
C3 C4 C7 121.8(7) . .
C4 C5 C6 121.6(6) . .
C4 C5 H5A 119.2 . .
C6 C5 H5A 119.2 . .
C5 C6 C1 120.2(7) . .
C5 C6 C9 116.8(6) . .
C1 C6 C9 122.9(6) . .
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C2 C8 H8A 109.5 . .
C2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N2 C10 C1 112.8(5) . .
N2 C10 H10A 109.0 . .
C1 C10 H10A 109.0 . .
N2 C10 H10B 109.0 . .
C1 C10 H10B 109.0 . .
H10A C10 H10B 107.8 . .
N3 C11 C3 112.2(5) . .
N3 C11 H11A 109.2 . .
C3 C11 H11A 109.2 . .
N3 C11 H11B 109.2 . .
C3 C11 H11B 109.2 . .
H11A C11 H11B 107.9 . .
N1 C12 C13 104.2(7) . .
N1 C12 H12A 127.9 . .
C13 C12 H12A 127.9 . .
N2 C13 C12 107.7(7) . .
N2 C13 H13A 126.2 . .
C12 C13 H13A 126.2 . .
N2 C14 N1 111.0(6) . .
N2 C14 H14A 124.5 . .
N1 C14 H14A 124.5 . .
C16 C15 N3 106.5(5) . .
C16 C15 H15A 126.8 . .
N3 C15 H15A 126.8 . .
C15 C16 N4 110.3(5) . .
C15 C16 H16A 124.9 . .
N4 C16 H16A 124.9 . .
N4 C17 N3 113.2(5) . .
N4 C17 H17A 123.4 . .
N3 C17 H17A 123.4 . .
C19 C18 N8 112.0(7) . .
C19 C18 H18A 124.0 . .
N8 C18 H18A 124.0 . .
C18 C19 N7 105.8(7) . .
C18 C19 H19A 127.1 . .
N7 C19 H19A 127.1 . .
N8 C20 N7 112.5(6) . .
N8 C20 H20A 123.7 . .
N7 C20 H20A 123.7 . .
C22 C21 C26 119.0(4) . .
C22 C21 C29 117.1(5) . .
C26 C21 C29 123.8(5) . .
C21 C22 C23 123.5(5) . .
C21 C22 H22A 118.2 . .
C23 C22 H22A 118.2 . .
C22 C23 C24 117.0(5) . .
C22 C23 C27 119.9(5) . .
C24 C23 C27 123.1(4) . .
C25 C24 C23 120.9(4) . .
C25 C24 C31 120.0(4) . .
C23 C24 C31 119.1(4) . .
C24 C25 C26 119.6(5) . .
C24 C25 C28 120.4(4) . .
C26 C25 C28 120.0(5) . .
C21 C26 C25 119.9(5) . .
C21 C26 C30 120.1(4) . .
C25 C26 C30 119.9(5) . .
C23 C27 H27A 109.5 . .
C23 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C23 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C25 C28 H28A 109.5 . .
C25 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C25 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C21 C29 H29A 109.5 . .
C21 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C21 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
N7 C30 C26 111.1(5) . .
N7 C30 H30A 109.4 . .
C26 C30 H30A 109.4 . .
N7 C30 H30B 109.4 . .
C26 C30 H30B 109.4 . .
H30A C30 H30B 108.0 . .
N6 C31 C24 112.4(4) . .
N6 C31 H31A 109.1 . .
C24 C31 H31A 109.1 . .
N6 C31 H31B 109.1 . .
C24 C31 H31B 109.1 . .
H31A C31 H31B 107.9 . .
C33 C32 N5 109.4(5) . .
C33 C32 H32A 125.3 . .
N5 C32 H32A 125.3 . .
C32 C33 N6 106.9(5) . .
C32 C33 H33A 126.5 . .
N6 C33 H33A 126.5 . .
N5 C34 N6 111.5(4) . .
N5 C34 H34A 124.3 . .
N6 C34 H34A 124.3 . .
C14 N1 C12 108.3(6) . .
C14 N2 C13 107.8(6) . .
C14 N2 C10 127.9(6) . .
C13 N2 C10 124.1(6) . .
C17 N3 C15 104.8(5) . .
C17 N3 C11 128.9(5) . .
C15 N3 C11 126.0(5) . .
C17 N4 C16 105.2(4) . .
C17 N4 Ni1 126.0(3) . .
C16 N4 Ni1 126.6(3) . .
C34 N5 C32 106.1(4) . .
C34 N5 Ni1 128.3(3) . .
C32 N5 Ni1 125.5(3) . .
C33 N6 C34 106.0(4) . .
C33 N6 C31 126.7(4) . .
C34 N6 C31 127.1(4) . .
C20 N7 C19 106.4(6) . .
C20 N7 C30 126.5(5) . .
C19 N7 C30 126.8(6) . .
C20 N8 C18 103.2(7) . .
H1WA O1W H1WB 117.9 . .
H2WA O2W H2WB 86.8(15) . .
H3WA O3W H3WB 98.3(16) . .
H4WA O4W H4WB 115.3 . .
H5WA O5W H5WB 95.6(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O15 1.688(3) .
Mo1 O7 1.786(3) .
Mo1 O13 1.828(3) .
Mo1 O18 2.054(2) 2_654
Mo1 O22 2.064(3) .
Mo1 O17 2.434(3) .
Mo1 V4 3.1142(7) .
Mo2 O9 1.697(3) .
Mo2 O6 1.793(3) .
Mo2 O14 1.814(3) .
Mo2 O18 2.072(3) .
Mo2 O22 2.085(3) .
Mo2 O17 2.438(3) .
Mo2 V4 3.1197(7) .
Mo3 O4 1.700(3) .
Mo3 O12 1.798(3) .
Mo3 O11 1.800(3) .
Mo3 O8 2.049(2) 2_654
Mo3 O20 2.083(3) .
Mo3 O5 2.458(3) 2_654
Mo3 V3 3.1197(7) .
Mo4 O3 1.696(3) .
Mo4 O10 1.793(3) .
Mo4 O16 1.830(3) .
Mo4 O20 2.047(3) .
Mo4 O8 2.070(2) .
Mo4 O5 2.442(3) .
Mo4 V3 3.1012(7) .
P1 O5 1.534(3) 2_654
P1 O5 1.534(3) .
P1 O17 1.537(3) .
P1 O17 1.537(3) 2_654
Ni1 N4 2.081(4) .
Ni1 N4 2.081(4) 2_654
Ni1 N5 2.098(4) .
Ni1 N5 2.098(4) 2_654
Ni1 O19 2.106(4) 1_545
Ni1 O21 2.112(4) .
V1 O1 1.605(4) .
V1 O6 1.931(3) .
V1 O7 1.945(3) 2_654
V1 O16 1.954(3) .
V1 O12 1.971(3) 2_654
V2 O2 1.593(3) .
V2 O14 1.934(3) .
V2 O11 1.941(3) .
V2 O10 1.944(3) .
V2 O13 1.951(3) .
V3 O21 1.621(4) .
V3 O20 1.893(3) .
V3 O20 1.893(3) 2_654
V3 O8 1.976(3) .
V3 O8 1.976(3) 2_654
V3 Mo4 3.1012(7) 2_654
V3 Mo3 3.1197(7) 2_654
V4 O19 1.622(4) .
V4 O18 1.895(3) .
V4 O18 1.895(3) 2_654
V4 O22 1.981(2) 2_654
V4 O22 1.981(2) .
V4 Mo1 3.1142(7) 2_654
V4 Mo2 3.1197(7) 2_654
O5 Mo3 2.458(3) 2_654
O7 V1 1.945(3) 2_654
O8 Mo3 2.049(3) 2_654
O12 V1 1.971(3) 2_654
O18 Mo1 2.054(2) 2_654
O19 Ni1 2.106(4) 1_565
C1 C2 1.378(10) .
C1 C6 1.411(8) .
C1 C10 1.479(8) .
C2 C3 1.423(8) .
C2 C8 1.518(8) .
C3 C4 1.410(8) .
C3 C11 1.475(9) .
C4 C5 1.361(10) .
C4 C7 1.507(9) .
C5 C6 1.382(9) .
C5 H5A 0.9300 .
C6 C9 1.543(11) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 N2 1.479(8) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 N3 1.449(8) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 N1 1.393(9) .
C12 C13 1.392(10) .
C12 H12A 0.9300 .
C13 N2 1.371(9) .
C13 H13A 0.9300 .
C14 N2 1.306(8) .
C14 N1 1.314(9) .
C14 H14A 0.9300 .
C15 C16 1.345(8) .
C15 N3 1.361(7) .
C15 H15A 0.9300 .
C16 N4 1.350(6) .
C16 H16A 0.9300 .
C17 N4 1.278(7) .
C17 N3 1.354(6) .
C17 H17A 0.9300 .
C18 C19 1.330(11) .
C18 N8 1.368(10) .
C18 H18A 0.9300 .
C19 N7 1.372(9) .
C19 H19A 0.9300 .
C20 N8 1.328(9) .
C20 N7 1.339(8) .
C20 H20A 0.9300 .
C21 C22 1.368(7) .
C21 C26 1.385(8) .
C21 C29 1.526(7) .
C22 C23 1.389(6) .
C22 H22A 0.9300 .
C23 C24 1.403(7) .
C23 C27 1.522(7) .
C24 C25 1.392(7) .
C24 C31 1.513(5) .
C25 C26 1.404(6) .
C25 C28 1.514(7) .
C26 C30 1.506(7) .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C30 N7 1.469(8) .
C30 H30A 0.9700 .
C30 H30B 0.9700 .
C31 N6 1.464(6) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 C33 1.355(7) .
C32 N5 1.364(6) .
C32 H32A 0.9300 .
C33 N6 1.360(6) .
C33 H33A 0.9300 .
C34 N5 1.302(6) .
C34 N6 1.364(6) .
C34 H34A 0.9300 .
O1W H1WA 0.8187 .
O1W H1WB 0.8249 .
O2W H2WA 0.977(16) .
O2W H2WB 0.973(16) .
O3W H3WA 0.925(14) .
O3W H3WB 0.919(15) .
O4W H4WA 0.8325 .
O4W H4WB 0.8225 .
O5W H5WA 0.936(15) .
O5W H5WB 0.928(15) .
