# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1111
_database_code_depnum_ccdc_archive 'CCDC 1449084'
_audit_update_record             
;
2016-01-22 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'ammonium citrato-oxovanadate (IV)'
_chemical_name_common            CA-V(IV)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 N4 O18 V2'
_chemical_formula_weight         618.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3000 0.5290 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4098(10)
_cell_length_b                   10.0034(10)
_cell_length_c                   13.9777(14)
_cell_angle_alpha                76.368(3)
_cell_angle_beta                 84.054(3)
_cell_angle_gamma                66.078(3)
_cell_volume                     1168.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    288(2)
_cell_measurement_reflns_used    9890
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      28.29

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8509
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      288(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16967
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         28.30
_reflns_number_total             5784
_reflns_number_gt                5164
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2007)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0516P)²+1.0121P] where P=(Fo²+2Fc²)/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         5784
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0938
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.51761(3) 0.93727(3) 0.39911(2) 0.01543(8) Uani 1 1 d . . .
O5 O 0.64872(13) 0.95061(13) 0.49421(9) 0.0151(2) Uani 1 1 d . . .
O7 O 0.67893(15) 1.06769(16) 0.64267(10) 0.0243(3) Uani 1 1 d . . .
O8 O 0.91752(18) 1.05601(19) 0.63656(13) 0.0357(4) Uani 1 1 d . . .
O1 O 0.77322(18) 0.49747(16) 0.47373(13) 0.0347(4) Uani 1 1 d . . .
O4 O 0.75851(18) 0.62236(16) 0.68482(11) 0.0331(3) Uani 1 1 d . . .
O6 O 0.62697(17) 0.90349(17) 0.30380(10) 0.0281(3) Uani 1 1 d . . .
O2 O 0.57878(15) 0.71886(15) 0.46656(11) 0.0237(3) Uani 1 1 d . . .
O3 O 0.55607(16) 0.84027(15) 0.66564(10) 0.0242(3) Uani 1 1 d . . .
C3 C 0.76451(19) 0.81932(19) 0.54841(13) 0.0162(3) Uani 1 1 d . . .
C5 C 0.8874(2) 0.8640(2) 0.58029(15) 0.0214(4) Uani 1 1 d . . .
H5A H 0.9527 0.7815 0.6295 0.026 Uiso 1 1 calc R . .
H5B H 0.9530 0.8781 0.5238 0.026 Uiso 1 1 calc R . .
C6 C 0.8254(2) 1.0042(2) 0.62193(13) 0.0205(3) Uani 1 1 d . . .
C4 C 0.6892(2) 0.7533(2) 0.64044(13) 0.0195(3) Uani 1 1 d . . .
C2 C 0.8381(2) 0.6994(2) 0.48674(14) 0.0209(4) Uani 1 1 d . . .
H2A H 0.8680 0.7438 0.4226 0.025 Uiso 1 1 calc R . .
H2B H 0.9312 0.6213 0.5189 0.025 Uiso 1 1 calc R . .
C1 C 0.7255(2) 0.6318(2) 0.47393(14) 0.0209(4) Uani 1 1 d . . .
V2 V -0.03635(3) 0.35794(3) 1.06774(2) 0.01662(8) Uani 1 1 d . . .
O11 O -0.01781(19) 0.24982(17) 1.17479(11) 0.0319(3) Uani 1 1 d . . .
O15 O 0.19580(16) 0.24492(15) 1.04016(10) 0.0243(3) Uani 1 1 d . . .
O14 O 0.00530(14) 0.46610(13) 0.91799(9) 0.0159(2) Uani 1 1 d . . .
O9 O -0.46607(18) 0.5883(2) 1.16869(13) 0.0385(4) Uani 1 1 d . . .
O10 O -0.26692(16) 0.47781(17) 1.07678(10) 0.0249(3) Uani 1 1 d . . .
O13 O -0.1805(2) 0.2107(2) 0.85595(13) 0.0439(4) Uani 1 1 d . . .
O12 O -0.09183(18) 0.24144(17) 0.98533(11) 0.0280(3) Uani 1 1 d . . .
O16 O 0.33105(16) 0.11891(16) 0.92748(11) 0.0280(3) Uani 1 1 d . . .
C10 C 0.1160(2) 0.35346(19) 0.87260(13) 0.0164(3) Uani 1 1 d . . .
C11 C 0.2207(2) 0.4137(2) 0.79907(13) 0.0214(4) Uani 1 1 d . . .
H11A H 0.2828 0.3390 0.7616 0.026 Uiso 1 1 calc R . .
H11B H 0.1565 0.5026 0.7533 0.026 Uiso 1 1 calc R . .
C7 C -0.3266(2) 0.5484(2) 1.14740(14) 0.0212(4) Uani 1 1 d . . .
C9 C 0.0263(2) 0.2907(2) 0.82404(14) 0.0219(4) Uani 1 1 d . . .
H9A H 0.0995 0.2044 0.7999 0.026 Uiso 1 1 calc R . .
H9B H -0.0291 0.3657 0.7679 0.026 Uiso 1 1 calc R . .
C8 C -0.0897(2) 0.2444(2) 0.89330(15) 0.0226(4) Uani 1 1 d . . .
C12 C 0.2238(2) 0.2280(2) 0.95156(14) 0.0186(3) Uani 1 1 d . . .
N4 N 0.3626(2) 0.95084(19) 0.14577(12) 0.0253(3) Uani 1 1 d . . .
H4C H 0.3102 1.0447 0.1122 0.030 Uiso 1 1 d R . .
H4D H 0.3058 0.8968 0.1461 0.030 Uiso 1 1 d R . .
H4A H 0.4555 0.9099 0.1168 0.030 Uiso 1 1 d R . .
H4B H 0.3786 0.9520 0.2079 0.030 Uiso 1 1 d R . .
N3 N 0.3974(2) 0.4032(2) 0.12377(14) 0.0339(4) Uani 1 1 d . . .
H3C H 0.4452 0.4623 0.1302 0.041 Uiso 1 1 d R . .
H3D H 0.3442 0.3884 0.1798 0.041 Uiso 1 1 d R . .
H3A H 0.3312 0.4486 0.0729 0.041 Uiso 1 1 d R . .
H3B H 0.4688 0.3148 0.1138 0.041 Uiso 1 1 d R . .
N2 N 1.2247(2) 0.8721(2) 0.70097(17) 0.0404(5) Uani 1 1 d . . .
H2E H 1.1893 0.8143 0.7480 0.048 Uiso 1 1 d R . .
H2F H 1.3285 0.8383 0.7064 0.048 Uiso 1 1 d R . .
H2C H 1.1989 0.8721 0.6407 0.048 Uiso 1 1 d R . .
H2D H 1.1784 0.9686 0.7058 0.048 Uiso 1 1 d R . .
O17 O 0.6789(2) 0.1520(2) 0.10012(15) 0.0467(4) Uani 1 1 d . . .
H17A H 0.7486 0.1738 0.0645 0.056 Uiso 1 1 d R . .
H17B H 0.6805 0.0712 0.0894 0.056 Uiso 1 1 d R . .
O18 O 0.3827(2) 0.6283(2) 0.60664(15) 0.0491(5) Uani 1 1 d . . .
H18A H 0.3335 0.5926 0.5792 0.059 Uiso 1 1 d R . .
H18B H 0.4060 0.5759 0.6646 0.059 Uiso 1 1 d R . .
N1 N 0.6819(3) 0.3546(2) 0.66728(15) 0.0370(4) Uani 1 1 d . . .
H1C H 0.6160 0.3782 0.7179 0.044 Uiso 1 1 d R . .
H1D H 0.6856 0.2681 0.6563 0.044 Uiso 1 1 d R . .
H1A H 0.6478 0.4276 0.6131 0.044 Uiso 1 1 d R . .
H1B H 0.7773 0.3435 0.6824 0.044 Uiso 1 1 d R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O6 1.6106(14) . ?
V1 O5 1.9658(12) . ?
V1 O7 2.0188(13) 2_676 ?
V1 O2 2.0286(14) . ?
V1 O3 2.0449(14) 2_676 ?
V1 O5 2.1937(12) 2_676 ?
O5 C3 1.424(2) . ?
O5 V1 2.1937(12) 2_676 ?
O7 C6 1.297(2) . ?
O7 V1 2.0188(13) 2_676 ?
O8 C6 1.230(2) . ?
O1 C1 1.233(2) . ?
O4 C4 1.239(2) . ?
O2 C1 1.299(2) . ?
O3 C4 1.272(2) . ?
O3 V1 2.0449(14) 2_676 ?
C3 C2 1.533(2) . ?
C3 C5 1.535(2) . ?
C3 C4 1.544(2) . ?
C5 C6 1.515(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 C1 1.513(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
V2 O11 1.6054(15) . ?
V2 O14 1.9540(13) 2_567 ?
V2 O10 2.0164(14) . ?
V2 O12 2.0514(14) . ?
V2 O15 2.0559(14) . ?
V2 O14 2.1936(13) . ?
O15 C12 1.275(2) . ?
O14 C10 1.416(2) . ?
O14 V2 1.9540(12) 2_567 ?
O9 C7 1.233(2) . ?
O10 C7 1.297(2) . ?
O13 C8 1.235(2) . ?
O12 C8 1.278(2) . ?
O16 C12 1.238(2) . ?
C10 C9 1.522(2) . ?
C10 C12 1.539(2) . ?
C10 C11 1.539(2) . ?
C11 C7 1.514(3) 2_567 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C7 C11 1.514(3) 2_567 ?
C9 C8 1.524(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N4 H4C 0.8999 . ?
N4 H4D 0.9000 . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9001 . ?
N3 H3C 0.8998 . ?
N3 H3D 0.8999 . ?
N3 H3A 0.8999 . ?
N3 H3B 0.9000 . ?
N2 H2E 0.9000 . ?
N2 H2F 0.8999 . ?
N2 H2C 0.9002 . ?
N2 H2D 0.9000 . ?
O17 H17A 0.8499 . ?
O17 H17B 0.8501 . ?
O18 H18A 0.8500 . ?
O18 H18B 0.8500 . ?
N1 H1C 0.9000 . ?
N1 H1D 0.8999 . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?

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
O6 V1 O5 105.31(7) . . ?
O6 V1 O7 101.01(7) . 2_676 ?
O5 V1 O7 153.54(6) . 2_676 ?
O6 V1 O2 94.99(7) . . ?
O5 V1 O2 87.77(5) . . ?
O7 V1 O2 87.28(6) 2_676 . ?
O6 V1 O3 87.63(7) . 2_676 ?
O5 V1 O3 93.25(6) . 2_676 ?
O7 V1 O3 90.48(6) 2_676 2_676 ?
O2 V1 O3 176.84(5) . 2_676 ?
O6 V1 O5 163.61(6) . 2_676 ?
O5 V1 O5 75.90(5) . 2_676 ?
O7 V1 O5 79.65(5) 2_676 2_676 ?
O2 V1 O5 101.40(5) . 2_676 ?
O3 V1 O5 75.99(5) 2_676 2_676 ?
C3 O5 V1 120.89(10) . . ?
C3 O5 V1 107.43(10) . 2_676 ?
V1 O5 V1 104.10(5) . 2_676 ?
C6 O7 V1 134.55(12) . 2_676 ?
C1 O2 V1 118.61(12) . . ?
C4 O3 V1 117.50(12) . 2_676 ?
O5 C3 C2 111.15(14) . . ?
O5 C3 C5 107.98(14) . . ?
C2 C3 C5 111.02(14) . . ?
O5 C3 C4 109.35(13) . . ?
C2 C3 C4 107.78(14) . . ?
C5 C3 C4 109.54(15) . . ?
C6 C5 C3 115.85(15) . . ?
C6 C5 H5A 108.3 . . ?
C3 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
C3 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
O8 C6 O7 120.49(18) . . ?
O8 C6 C5 118.47(17) . . ?
O7 C6 C5 121.04(16) . . ?
O4 C4 O3 123.98(17) . . ?
O4 C4 C3 119.78(17) . . ?
O3 C4 C3 116.25(15) . . ?
C1 C2 C3 110.86(14) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O1 C1 O2 122.08(18) . . ?
O1 C1 C2 120.16(17) . . ?
O2 C1 C2 117.72(16) . . ?
O11 V2 O14 107.42(7) . 2_567 ?
O11 V2 O10 96.98(7) . . ?
O14 V2 O10 87.63(5) 2_567 . ?
O11 V2 O12 100.97(7) . . ?
O14 V2 O12 151.50(6) 2_567 . ?
O10 V2 O12 86.50(6) . . ?
O11 V2 O15 89.65(7) . . ?
O14 V2 O15 92.61(6) 2_567 . ?
O10 V2 O15 172.98(6) . . ?
O12 V2 O15 89.98(6) . . ?
O11 V2 O14 164.35(7) . . ?
O14 V2 O14 74.63(5) 2_567 . ?
O10 V2 O14 98.61(5) . . ?
O12 V2 O14 78.74(5) . . ?
O15 V2 O14 74.72(5) . . ?
C12 O15 V2 113.09(11) . . ?
C10 O14 V2 123.05(10) . 2_567 ?
C10 O14 V2 107.57(10) . . ?
V2 O14 V2 105.38(5) 2_567 . ?
C7 O10 V2 121.53(12) . . ?
C8 O12 V2 134.39(13) . . ?
O14 C10 C9 107.14(14) . . ?
O14 C10 C12 109.39(14) . . ?
C9 C10 C12 109.37(15) . . ?
O14 C10 C11 111.83(14) . . ?
C9 C10 C11 112.41(15) . . ?
C12 C10 C11 106.67(14) . . ?
C7 C11 C10 110.63(15) 2_567 . ?
C7 C11 H11A 109.5 2_567 . ?
C10 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 2_567 . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
O9 C7 O10 121.57(18) . . ?
O9 C7 C11 120.57(17) . 2_567 ?
O10 C7 C11 117.82(16) . 2_567 ?
C10 C9 C8 113.22(15) . . ?
C10 C9 H9A 108.9 . . ?
C8 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
C8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
O13 C8 O12 122.30(19) . . ?
O13 C8 C9 116.73(18) . . ?
O12 C8 C9 120.97(16) . . ?
O16 C12 O15 123.64(17) . . ?
O16 C12 C10 120.07(16) . . ?
O15 C12 C10 116.28(15) . . ?
H4C N4 H4D 108.4 . . ?
H4C N4 H4A 110.0 . . ?
H4D N4 H4A 110.0 . . ?
H4C N4 H4B 110.0 . . ?
H4D N4 H4B 110.0 . . ?
H4A N4 H4B 108.5 . . ?
H3C N3 H3D 108.1 . . ?
H3C N3 H3A 109.6 . . ?
H3D N3 H3A 109.6 . . ?
H3C N3 H3B 109.6 . . ?
H3D N3 H3B 109.6 . . ?
H3A N3 H3B 110.3 . . ?
H2E N2 H2F 108.9 . . ?
H2E N2 H2C 110.9 . . ?
H2F N2 H2C 110.9 . . ?
H2E N2 H2D 110.9 . . ?
H2F N2 H2D 110.9 . . ?
H2C N2 H2D 104.3 . . ?
H17A O17 H17B 108.5 . . ?
H18A O18 H18B 108.3 . . ?
H1C N1 H1D 108.2 . . ?
H1C N1 H1A 109.8 . . ?
H1D N1 H1A 109.8 . . ?
H1C N1 H1B 109.8 . . ?
H1D N1 H1B 109.8 . . ?
H1A N1 H1B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 V1 O5 C3 -76.23(13) . . . . ?
O7 V1 O5 C3 97.69(16) 2_676 . . . ?
O2 V1 O5 C3 18.33(12) . . . . ?
O3 V1 O5 C3 -164.66(12) 2_676 . . . ?
O5 V1 O5 C3 120.67(13) 2_676 . . . ?
O6 V1 O5 V1 163.10(7) . . . 2_676 ?
O7 V1 O5 V1 -22.98(14) 2_676 . . 2_676 ?
O2 V1 O5 V1 -102.34(6) . . . 2_676 ?
O3 V1 O5 V1 74.67(6) 2_676 . . 2_676 ?
O5 V1 O5 V1 0.0 2_676 . . 2_676 ?
O6 V1 O2 C1 49.09(15) . . . . ?
O5 V1 O2 C1 -56.09(14) . . . . ?
O7 V1 O2 C1 149.91(14) 2_676 . . . ?
O3 V1 O2 C1 -165.1(10) 2_676 . . . ?
O5 V1 O2 C1 -131.22(13) 2_676 . . . ?
V1 O5 C3 C2 34.42(17) . . . . ?
V1 O5 C3 C2 153.46(11) 2_676 . . . ?
V1 O5 C3 C5 156.42(11) . . . . ?
V1 O5 C3 C5 -84.54(13) 2_676 . . . ?
V1 O5 C3 C4 -84.46(15) . . . . ?
V1 O5 C3 C4 34.58(15) 2_676 . . . ?
O5 C3 C5 C6 45.0(2) . . . . ?
C2 C3 C5 C6 167.05(16) . . . . ?
C4 C3 C5 C6 -74.0(2) . . . . ?
V1 O7 C6 O8 160.30(15) 2_676 . . . ?
V1 O7 C6 C5 -20.3(3) 2_676 . . . ?
C3 C5 C6 O8 -170.62(18) . . . . ?
C3 C5 C6 O7 10.0(3) . . . . ?
V1 O3 C4 O4 167.56(16) 2_676 . . . ?
V1 O3 C4 C3 -12.6(2) 2_676 . . . ?
O5 C3 C4 O4 162.86(17) . . . . ?
C2 C3 C4 O4 41.9(2) . . . . ?
C5 C3 C4 O4 -79.0(2) . . . . ?
O5 C3 C4 O3 -17.0(2) . . . . ?
C2 C3 C4 O3 -137.92(17) . . . . ?
C5 C3 C4 O3 101.18(18) . . . . ?
O5 C3 C2 C1 -71.94(18) . . . . ?
C5 C3 C2 C1 167.85(15) . . . . ?
C4 C3 C2 C1 47.88(19) . . . . ?
V1 O2 C1 O1 -148.79(16) . . . . ?
V1 O2 C1 C2 33.4(2) . . . . ?
C3 C2 C1 O1 -143.30(19) . . . . ?
C3 C2 C1 O2 34.5(2) . . . . ?
O11 V2 O15 C12 141.90(14) . . . . ?
O14 V2 O15 C12 -110.67(13) 2_567 . . . ?
O10 V2 O15 C12 -18.9(5) . . . . ?
O12 V2 O15 C12 40.93(13) . . . . ?
O14 V2 O15 C12 -37.39(12) . . . . ?
O11 V2 O14 C10 33.1(3) . . . . ?
O14 V2 O14 C10 132.87(12) 2_567 . . . ?
O10 V2 O14 C10 -142.01(10) . . . . ?
O12 V2 O14 C10 -57.36(10) . . . . ?
O15 V2 O14 C10 35.74(10) . . . . ?
O11 V2 O14 V2 -99.8(2) . . . 2_567 ?
O14 V2 O14 V2 0.0 2_567 . . 2_567 ?
O10 V2 O14 V2 85.12(6) . . . 2_567 ?
O12 V2 O14 V2 169.77(7) . . . 2_567 ?
O15 V2 O14 V2 -97.13(6) . . . 2_567 ?
O11 V2 O10 C7 56.50(15) . . . . ?
O14 V2 O10 C7 -50.77(15) 2_567 . . . ?
O12 V2 O10 C7 157.14(15) . . . . ?
O15 V2 O10 C7 -142.9(4) . . . . ?
O14 V2 O10 C7 -124.82(14) . . . . ?
O11 V2 O12 C8 -161.96(19) . . . . ?
O14 V2 O12 C8 23.1(3) 2_567 . . . ?
O10 V2 O12 C8 101.60(19) . . . . ?
O15 V2 O12 C8 -72.32(19) . . . . ?
O14 V2 O12 C8 2.09(18) . . . . ?
V2 O14 C10 C9 -148.69(11) 2_567 . . . ?
V2 O14 C10 C9 88.78(13) . . . . ?
V2 O14 C10 C12 92.86(15) 2_567 . . . ?
V2 O14 C10 C12 -29.67(15) . . . . ?
V2 O14 C10 C11 -25.09(18) 2_567 . . . ?
V2 O14 C10 C11 -147.62(12) . . . . ?
O14 C10 C11 C7 68.61(19) . . . 2_567 ?
C9 C10 C11 C7 -170.82(15) . . . 2_567 ?
C12 C10 C11 C7 -50.95(19) . . . 2_567 ?
V2 O10 C7 O9 -160.81(16) . . . . ?
V2 O10 C7 C11 21.5(2) . . . 2_567 ?
O14 C10 C9 C8 -51.14(19) . . . . ?
C12 C10 C9 C8 67.33(19) . . . . ?
C11 C10 C9 C8 -174.39(15) . . . . ?
V2 O12 C8 O13 -150.63(18) . . . . ?
V2 O12 C8 C9 29.2(3) . . . . ?
C10 C9 C8 O13 170.95(18) . . . . ?
C10 C9 C8 O12 -8.9(3) . . . . ?
V2 O15 C12 O16 -148.28(16) . . . . ?
V2 O15 C12 C10 32.10(19) . . . . ?
O14 C10 C12 O16 -178.96(16) . . . . ?
C9 C10 C12 O16 64.0(2) . . . . ?
C11 C10 C12 O16 -57.8(2) . . . . ?
O14 C10 C12 O15 0.7(2) . . . . ?
C9 C10 C12 O15 -116.38(17) . . . . ?
C11 C10 C12 O15 121.81(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.084
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: water and ethanol'
