# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C14 H10 N2 O5 V), H14 Li2 O7, 2(H2 O)'
_chemical_formula_sum            'C28 H38 Li2 N4 O19 V2'
_chemical_formula_weight         850.38

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'
Li Li -0.0003 0.0001 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   6.8227(2)
_cell_length_b                   15.4441(6)
_cell_length_c                   18.3454(7)
_cell_angle_alpha                67.969(2)
_cell_angle_beta                 80.954(2)
_cell_angle_gamma                89.346(2)
_cell_volume                     1767.24(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    321
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             876
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_T_max  0.9132

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24488
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         28.47
_reflns_number_total             8797
_reflns_number_gt                7372
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'

_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 > 2σ(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)+(0.0541P)²+0.9492P] 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         8797
_refine_ls_number_parameters     498
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.92923(4) 0.20359(2) 0.816343(17) 0.01206(8) Uani 1 1 d . . .
O1 O 0.6644(2) 0.19538(10) 0.55069(7) 0.0225(3) Uani 1 1 d . . .
H1O H 0.7569 0.2110 0.5693 0.034 Uiso 1 1 calc R . .
O2 O 0.70275(18) 0.14577(9) 0.78994(7) 0.0150(2) Uani 1 1 d . . .
O3 O 1.17003(19) 0.27650(10) 0.79727(7) 0.0206(3) Uani 1 1 d . . .
O4 O 0.99026(19) 0.10443(9) 0.87948(8) 0.0187(3) Uani 1 1 d . . .
O5 O 0.79021(19) 0.25558(9) 0.86607(8) 0.0197(3) Uani 1 1 d . . .
N1 N 0.8427(2) 0.21143(10) 0.65858(9) 0.0137(3) Uani 1 1 d . . .
N2 N 0.9851(2) 0.24321(10) 0.69128(8) 0.0122(3) Uani 1 1 d . . .
C1 C 0.5225(3) 0.14326(12) 0.61124(10) 0.0150(3) Uani 1 1 d . . .
C2 C 0.3599(3) 0.10884(12) 0.59118(11) 0.0178(4) Uani 1 1 d . . .
H2 H 0.3522 0.1228 0.5367 0.021 Uiso 1 1 calc R . .
C3 C 0.2096(3) 0.05454(12) 0.64983(11) 0.0179(4) Uani 1 1 d . . .
H3 H 0.1000 0.0308 0.6355 0.021 Uiso 1 1 calc R . .
C4 C 0.2183(3) 0.03442(13) 0.72980(11) 0.0176(4) Uani 1 1 d . . .
H4 H 0.1150 -0.0030 0.7701 0.021 Uiso 1 1 calc R . .
C5 C 0.3784(3) 0.06932(12) 0.75022(10) 0.0150(3) Uani 1 1 d . . .
H5 H 0.3834 0.0557 0.8048 0.018 Uiso 1 1 calc R . .
C6 C 0.5330(2) 0.12429(11) 0.69185(10) 0.0127(3) Uani 1 1 d . . .
C7 C 0.7004(2) 0.16211(11) 0.71455(10) 0.0128(3) Uani 1 1 d . . .
C8 C 1.1351(2) 0.29040(11) 0.63895(10) 0.0134(3) Uani 1 1 d . . .
H8 H 1.1359 0.2990 0.5848 0.016 Uiso 1 1 calc R . .
C9 C 1.2995(2) 0.33024(11) 0.65754(10) 0.0132(3) Uani 1 1 d . . .
C10 C 1.4534(3) 0.37992(12) 0.59471(11) 0.0158(3) Uani 1 1 d . . .
H10 H 1.4454 0.3858 0.5418 0.019 Uiso 1 1 calc R . .
C11 C 1.6143(3) 0.41985(12) 0.60908(11) 0.0177(4) Uani 1 1 d . . .
H11 H 1.7165 0.4537 0.5664 0.021 Uiso 1 1 calc R . .
C12 C 1.6265(3) 0.41028(12) 0.68715(11) 0.0170(3) Uani 1 1 d . . .
H12 H 1.7389 0.4370 0.6973 0.020 Uiso 1 1 calc R . .
C13 C 1.4777(3) 0.36254(12) 0.74959(11) 0.0161(3) Uani 1 1 d . . .
H13 H 1.4878 0.3573 0.8021 0.019 Uiso 1 1 calc R . .
C14 C 1.3118(2) 0.32184(12) 0.73593(10) 0.0141(3) Uani 1 1 d . . .
V2 V 0.72014(4) 0.29884(2) 0.189591(17) 0.01243(8) Uani 1 1 d . . .
O6 O 0.2273(2) 0.31362(10) 0.45174(8) 0.0231(3) Uani 1 1 d . . .
H6O H 0.3353 0.2960 0.4343 0.035 Uiso 1 1 calc R . .
O7 O 0.46819(18) 0.35422(9) 0.21455(7) 0.0164(3) Uani 1 1 d . . .
O8 O 0.9603(2) 0.23585(10) 0.20961(8) 0.0246(3) Uani 1 1 d . . .
O9 O 0.63524(19) 0.23709(10) 0.14520(8) 0.0228(3) Uani 1 1 d . . .
O10 O 0.8204(2) 0.39739(9) 0.12162(8) 0.0232(3) Uani 1 1 d . . .
N3 N 0.4935(2) 0.28877(10) 0.34650(8) 0.0133(3) Uani 1 1 d . . .
N4 N 0.6675(2) 0.25763(10) 0.31506(8) 0.0122(3) Uani 1 1 d . . .
C15 C 0.1324(3) 0.36150(12) 0.39010(10) 0.0152(3) Uani 1 1 d . . .
C16 C -0.0487(3) 0.39738(12) 0.40806(11) 0.0186(4) Uani 1 1 d . . .
H16 H -0.1013 0.3870 0.4619 0.022 Uiso 1 1 calc R . .
C17 C -0.1527(3) 0.44797(12) 0.34817(11) 0.0184(4) Uani 1 1 d . . .
H17 H -0.2756 0.4726 0.3611 0.022 Uiso 1 1 calc R . .
C18 C -0.0783(3) 0.46305(12) 0.26882(11) 0.0175(4) Uani 1 1 d . . .
H18 H -0.1497 0.4979 0.2276 0.021 Uiso 1 1 calc R . .
C19 C 0.1005(3) 0.42662(12) 0.25084(11) 0.0153(3) Uani 1 1 d . . .
H19 H 0.1506 0.4363 0.1969 0.018 Uiso 1 1 calc R . .
C20 C 0.2094(2) 0.37568(11) 0.31043(10) 0.0133(3) Uani 1 1 d . . .
C21 C 0.3993(2) 0.33795(11) 0.28941(10) 0.0124(3) Uani 1 1 d . . .
C22 C 0.7720(2) 0.20884(12) 0.36822(10) 0.0138(3) Uani 1 1 d . . .
H22 H 0.7239 0.1989 0.4224 0.017 Uiso 1 1 calc R . .
C23 C 0.9550(2) 0.16898(11) 0.35070(10) 0.0126(3) Uani 1 1 d . . .
C24 C 1.0504(3) 0.11477(12) 0.41466(11) 0.0158(3) Uani 1 1 d . . .
H24 H 0.9929 0.1061 0.4677 0.019 Uiso 1 1 calc R . .
C25 C 1.2263(3) 0.07433(12) 0.40088(11) 0.0173(3) Uani 1 1 d . . .
H25 H 1.2894 0.0374 0.4441 0.021 Uiso 1 1 calc R . .
C26 C 1.3107(3) 0.08839(12) 0.32248(11) 0.0169(3) Uani 1 1 d . . .
H26 H 1.4326 0.0612 0.3126 0.020 Uiso 1 1 calc R . .
C27 C 1.2198(3) 0.14108(13) 0.25928(11) 0.0177(4) Uani 1 1 d . . .
H27 H 1.2788 0.1492 0.2065 0.021 Uiso 1 1 calc R . .
C28 C 1.0413(3) 0.18271(12) 0.27214(10) 0.0154(3) Uani 1 1 d . . .
Li1 Li 0.3463(5) 0.3447(2) -0.0190(2) 0.0247(7) Uani 1 1 d . . .
Li2 Li 0.4925(5) 0.1179(2) 0.0146(2) 0.0254(7) Uani 1 1 d . . .
O1W O 0.5470(2) 0.24907(9) 0.00272(8) 0.0209(3) Uani 1 1 d . . .
H1W1 H 0.5913 0.2456 0.0416 0.031 Uiso 1 1 d R . .
H1W2 H 0.6403 0.2616 -0.0324 0.031 Uiso 1 1 d R . .
O2W O 0.1200(2) 0.31329(10) -0.05800(9) 0.0256(3) Uani 1 1 d . . .
H2W1 H 0.1266 0.3063 -0.0993 0.038 Uiso 1 1 d R . .
H2W2 H 0.0682 0.2660 -0.0245 0.038 Uiso 1 1 d R . .
O3W O 0.4947(2) 0.45160(10) -0.09347(9) 0.0291(3) Uani 1 1 d . . .
H3W1 H 0.4633 0.5023 -0.1201 0.044 Uiso 1 1 d R . .
H3W2 H 0.5973 0.4603 -0.0808 0.044 Uiso 1 1 d R . .
O4W O 0.2456(2) 0.35159(14) 0.08121(11) 0.0466(5) Uani 1 1 d . . .
H4W1 H 0.1492 0.3224 0.1105 0.070 Uiso 1 1 d R . .
H4W2 H 0.3217 0.3530 0.1097 0.070 Uiso 1 1 d R . .
O5W O 0.3090(2) 0.05313(10) 0.10680(8) 0.0262(3) Uani 1 1 d . . .
H5W1 H 0.1978 0.0699 0.1027 0.039 Uiso 1 1 d R . .
H5W2 H 0.2940 -0.0005 0.1372 0.039 Uiso 1 1 d R . .
O6W O 0.3927(2) 0.13234(10) -0.08153(9) 0.0267(3) Uani 1 1 d . . .
H6W1 H 0.4757 0.1433 -0.1206 0.040 Uiso 1 1 d R . .
H6W2 H 0.2943 0.1538 -0.0985 0.040 Uiso 1 1 d R . .
O7W O 0.7436(2) 0.05722(10) 0.02347(9) 0.0289(3) Uani 1 1 d . . .
H7W1 H 0.8235 0.0721 -0.0168 0.043 Uiso 1 1 d R . .
H7W2 H 0.7251 0.0018 0.0373 0.043 Uiso 1 1 d R . .
O8W O 0.9785(2) 0.15478(10) 0.07933(9) 0.0322(4) Uani 1 1 d . . .
H8W1 H 0.9159 0.1701 0.1127 0.048 Uiso 1 1 d R . .
H8W2 H 0.9023 0.1232 0.0694 0.048 Uiso 1 1 d R . .
O9W O 0.8567(2) 0.44636(10) -0.04146(9) 0.0285(3) Uani 1 1 d . . .
H9W1 H 0.8432 0.4318 0.0059 0.043 Uiso 1 1 d R . .
H9W2 H 0.9267 0.4085 -0.0506 0.043 Uiso 1 1 d R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O5 1.6238(13) . ?
V1 O4 1.6330(13) . ?
V1 O3 1.9119(13) . ?
V1 O2 2.0028(12) . ?
V1 N2 2.1121(14) . ?
O1 C1 1.352(2) . ?
O1 H1O 0.8400 . ?
O2 C7 1.312(2) . ?
O3 C14 1.332(2) . ?
N1 C7 1.302(2) . ?
N1 N2 1.3994(19) . ?
N2 C8 1.298(2) . ?
C1 C2 1.392(2) . ?
C1 C6 1.409(2) . ?
C2 C3 1.381(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.392(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.471(2) . ?
C8 C9 1.430(2) . ?
C8 H8 0.9500 . ?
C9 C14 1.410(2) . ?
C9 C10 1.412(2) . ?
C10 C11 1.372(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.399(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.380(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.401(2) . ?
C13 H13 0.9500 . ?
V2 O9 1.6284(13) . ?
V2 O10 1.6343(13) . ?
V2 O8 1.9109(13) . ?
V2 O7 1.9771(12) . ?
V2 N4 2.1163(14) . ?
O6 C15 1.355(2) . ?
O6 H6O 0.8400 . ?
O7 C21 1.308(2) . ?
O8 C28 1.333(2) . ?
N3 C21 1.301(2) . ?
N3 N4 1.3975(19) . ?
N4 C22 1.297(2) . ?
C15 C16 1.391(2) . ?
C15 C20 1.407(2) . ?
C16 C17 1.382(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.395(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.382(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.401(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.470(2) . ?
C22 C23 1.430(2) . ?
C22 H22 0.9500 . ?
C23 C28 1.405(2) . ?
C23 C24 1.412(2) . ?
C24 C25 1.378(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.398(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.378(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.399(2) . ?
C27 H27 0.9500 . ?
Li1 O3W 1.879(4) . ?
Li1 O4W 1.900(4) . ?
Li1 O2W 1.938(4) . ?
Li1 O1W 1.974(4) . ?
Li1 Li2 3.484(5) . ?
Li1 H2W2 2.3009 . ?
Li1 H3W2 2.3132 . ?
Li2 O5W 1.877(4) . ?
Li2 O6W 1.923(4) . ?
Li2 O7W 1.943(4) . ?
Li2 O1W 1.988(4) . ?
Li2 H1W1 2.3362 . ?
Li2 H1W2 2.2429 . ?
Li2 H5W1 2.3064 . ?
O1W H1W1 0.8006 . ?
O1W H1W2 0.7990 . ?
O2W H2W1 0.7978 . ?
O2W H2W2 0.7982 . ?
O3W H3W1 0.7996 . ?
O3W H3W2 0.7999 . ?
O4W H4W1 0.7993 . ?
O4W H4W2 0.7978 . ?
O5W H5W1 0.8045 . ?
O5W H5W2 0.8037 . ?
O6W H6W1 0.8033 . ?
O6W H6W2 0.7999 . ?
O7W H7W1 0.8034 . ?
O7W H7W2 0.8010 . ?
O8W H8W1 0.7984 . ?
O8W H8W2 0.8029 . ?
O9W H9W1 0.8009 . ?
O9W H9W2 0.8005 . ?

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
O5 V1 O4 108.37(7) . . ?
O5 V1 O3 97.45(6) . . ?
O4 V1 O3 99.26(6) . . ?
O5 V1 O2 95.27(6) . . ?
O4 V1 O2 94.16(6) . . ?
O3 V1 O2 157.54(5) . . ?
O5 V1 N2 126.73(6) . . ?
O4 V1 N2 124.16(6) . . ?
O3 V1 N2 83.30(5) . . ?
O2 V1 N2 74.26(5) . . ?
C1 O1 H1O 109.5 . . ?
C7 O2 V1 117.66(10) . . ?
C14 O3 V1 137.77(11) . . ?
C7 N1 N2 110.31(14) . . ?
C8 N2 N1 113.61(14) . . ?
C8 N2 V1 130.34(12) . . ?
N1 N2 V1 116.01(10) . . ?
O1 C1 C2 117.23(15) . . ?
O1 C1 C6 122.73(16) . . ?
C2 C1 C6 120.04(16) . . ?
C3 C2 C1 120.53(16) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.26(17) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.58(17) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.26(16) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 118.33(15) . . ?
C5 C6 C7 120.53(15) . . ?
C1 C6 C7 121.13(15) . . ?
N1 C7 O2 121.73(15) . . ?
N1 C7 C6 118.56(15) . . ?
O2 C7 C6 119.71(15) . . ?
N2 C8 C9 124.18(16) . . ?
N2 C8 H8 117.9 . . ?
C9 C8 H8 117.9 . . ?
C14 C9 C10 119.39(16) . . ?
C14 C9 C8 122.27(15) . . ?
C10 C9 C8 118.33(15) . . ?
C11 C10 C9 120.82(16) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 119.46(17) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 120.92(17) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 120.38(17) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
O3 C14 C13 119.08(16) . . ?
O3 C14 C9 121.89(15) . . ?
C13 C14 C9 119.03(16) . . ?
O9 V2 O10 108.46(7) . . ?
O9 V2 O8 97.56(7) . . ?
O10 V2 O8 97.62(7) . . ?
O9 V2 O7 97.61(6) . . ?
O10 V2 O7 93.91(6) . . ?
O8 V2 O7 156.95(5) . . ?
O9 V2 N4 122.36(6) . . ?
O10 V2 N4 128.77(7) . . ?
O8 V2 N4 82.71(5) . . ?
O7 V2 N4 74.52(5) . . ?
C15 O6 H6O 109.5 . . ?
C21 O7 V2 118.02(11) . . ?
C28 O8 V2 138.20(11) . . ?
C21 N3 N4 110.05(13) . . ?
C22 N4 N3 113.98(14) . . ?
C22 N4 V2 130.59(11) . . ?
N3 N4 V2 115.42(10) . . ?
O6 C15 C16 117.32(15) . . ?
O6 C15 C20 122.85(15) . . ?
C16 C15 C20 119.83(16) . . ?
C17 C16 C15 120.56(17) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 120.40(16) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 119.21(17) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 121.45(16) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C19 C20 C15 118.55(15) . . ?
C19 C20 C21 120.17(15) . . ?
C15 C20 C21 121.28(15) . . ?
N3 C21 O7 121.97(15) . . ?
N3 C21 C20 118.47(15) . . ?
O7 C21 C20 119.56(15) . . ?
N4 C22 C23 124.31(15) . . ?
N4 C22 H22 117.8 . . ?
C23 C22 H22 117.8 . . ?
C28 C23 C24 119.67(15) . . ?
C28 C23 C22 121.87(16) . . ?
C24 C23 C22 118.46(15) . . ?
C25 C24 C23 120.65(16) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 119.19(17) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C27 C26 C25 121.01(16) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C28 120.58(17) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
O8 C28 C27 119.17(16) . . ?
O8 C28 C23 121.91(15) . . ?
C27 C28 C23 118.90(16) . . ?
O3W Li1 O4W 115.18(19) . . ?
O3W Li1 O2W 112.54(19) . . ?
O4W Li1 O2W 106.38(17) . . ?
O3W Li1 O1W 102.67(16) . . ?
O4W Li1 O1W 105.51(19) . . ?
O2W Li1 O1W 114.58(18) . . ?
O3W Li1 Li2 123.10(15) . . ?
O4W Li1 Li2 108.22(16) . . ?
O2W Li1 Li2 87.11(13) . . ?
O1W Li1 Li2 28.55(9) . . ?
O3W Li1 H2W2 131.9 . . ?
O4W Li1 H2W2 95.1 . . ?
O2W Li1 H2W2 19.4 . . ?
O1W Li1 H2W2 104.0 . . ?
Li2 Li1 H2W2 75.4 . . ?
O3W Li1 H3W2 18.5 . . ?
O4W Li1 H3W2 106.9 . . ?
O2W Li1 H3W2 130.8 . . ?
O1W Li1 H3W2 89.8 . . ?
Li2 Li1 H3W2 115.0 . . ?
H2W2 Li1 H3W2 150.0 . . ?
O5W Li2 O6W 112.49(19) . . ?
O5W Li2 O7W 108.69(19) . . ?
O6W Li2 O7W 113.85(18) . . ?
O5W Li2 O1W 111.76(18) . . ?
O6W Li2 O1W 103.16(17) . . ?
O7W Li2 O1W 106.69(17) . . ?
O5W Li2 Li1 99.01(14) . . ?
O6W Li2 Li1 85.81(14) . . ?
O7W Li2 Li1 134.83(16) . . ?
O1W Li2 Li1 28.34(9) . . ?
O5W Li2 H1W1 101.4 . . ?
O6W Li2 H1W1 122.4 . . ?
O7W Li2 H1W1 96.1 . . ?
O1W Li2 H1W1 19.3 . . ?
Li1 Li2 H1W1 42.6 . . ?
O5W Li2 H1W2 131.9 . . ?
O6W Li2 H1W2 95.5 . . ?
O7W Li2 H1W2 93.0 . . ?
O1W Li2 H1W2 20.7 . . ?
Li1 Li2 H1W2 43.1 . . ?
H1W1 Li2 H1W2 32.2 . . ?
O5W Li2 H5W1 18.8 . . ?
O6W Li2 H5W1 98.3 . . ?
O7W Li2 H5W1 127.2 . . ?
O1W Li2 H5W1 105.1 . . ?
Li1 Li2 H5W1 85.9 . . ?
H1W1 Li2 H5W1 100.6 . . ?
H1W2 Li2 H5W1 125.6 . . ?
Li1 O1W Li2 123.11(16) . . ?
Li1 O1W H1W1 110.0 . . ?
Li2 O1W H1W1 105.8 . . ?
Li1 O1W H1W2 112.7 . . ?
Li2 O1W H1W2 98.0 . . ?
H1W1 O1W H1W2 105.6 . . ?
Li1 O2W H2W1 124.3 . . ?
Li1 O2W H2W2 106.9 . . ?
H2W1 O2W H2W2 105.8 . . ?
Li1 O3W H3W1 132.4 . . ?
Li1 O3W H3W2 113.1 . . ?
H3W1 O3W H3W2 105.4 . . ?
Li1 O4W H4W1 124.4 . . ?
Li1 O4W H4W2 119.1 . . ?
H4W1 O4W H4W2 105.2 . . ?
Li2 O5W H5W1 112.4 . . ?
Li2 O5W H5W2 133.7 . . ?
H5W1 O5W H5W2 104.3 . . ?
Li2 O6W H6W1 115.4 . . ?
Li2 O6W H6W2 133.0 . . ?
H6W1 O6W H6W2 104.5 . . ?
Li2 O7W H7W1 116.1 . . ?
Li2 O7W H7W2 110.1 . . ?
H7W1 O7W H7W2 104.6 . . ?
H8W1 O8W H8W2 105.4 . . ?
H9W1 O9W H9W2 105.1 . . ?

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
O5 V1 O2 C7 125.15(12) . . . . ?
O4 V1 O2 C7 -125.94(12) . . . . ?
O3 V1 O2 C7 0.8(2) . . . . ?
N2 V1 O2 C7 -1.57(11) . . . . ?
O5 V1 O3 C14 -132.05(18) . . . . ?
O4 V1 O3 C14 117.86(18) . . . . ?
O2 V1 O3 C14 -8.1(3) . . . . ?
N2 V1 O3 C14 -5.76(17) . . . . ?
C7 N1 N2 C8 177.80(14) . . . . ?
C7 N1 N2 V1 -0.05(17) . . . . ?
O5 V1 N2 C8 98.68(16) . . . . ?
O4 V1 N2 C8 -92.32(16) . . . . ?
O3 V1 N2 C8 4.36(15) . . . . ?
O2 V1 N2 C8 -176.56(16) . . . . ?
O5 V1 N2 N1 -83.91(13) . . . . ?
O4 V1 N2 N1 85.10(12) . . . . ?
O3 V1 N2 N1 -178.23(12) . . . . ?
O2 V1 N2 N1 0.86(10) . . . . ?
O1 C1 C2 C3 179.58(16) . . . . ?
C6 C1 C2 C3 -1.2(3) . . . . ?
C1 C2 C3 C4 0.7(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C4 C5 C6 C1 -0.2(2) . . . . ?
C4 C5 C6 C7 178.97(15) . . . . ?
O1 C1 C6 C5 -179.88(16) . . . . ?
C2 C1 C6 C5 0.9(2) . . . . ?
O1 C1 C6 C7 1.0(3) . . . . ?
C2 C1 C6 C7 -178.20(15) . . . . ?
N2 N1 C7 O2 -1.4(2) . . . . ?
N2 N1 C7 C6 178.46(13) . . . . ?
V1 O2 C7 N1 2.3(2) . . . . ?
V1 O2 C7 C6 -177.58(11) . . . . ?
C5 C6 C7 N1 178.79(15) . . . . ?
C1 C6 C7 N1 -2.1(2) . . . . ?
C5 C6 C7 O2 -1.4(2) . . . . ?
C1 C6 C7 O2 177.76(15) . . . . ?
N1 N2 C8 C9 179.92(15) . . . . ?
V1 N2 C8 C9 -2.6(2) . . . . ?
N2 C8 C9 C14 -0.4(3) . . . . ?
N2 C8 C9 C10 179.92(16) . . . . ?
C14 C9 C10 C11 0.1(2) . . . . ?
C8 C9 C10 C11 179.79(16) . . . . ?
C9 C10 C11 C12 0.7(3) . . . . ?
C10 C11 C12 C13 -1.0(3) . . . . ?
C11 C12 C13 C14 0.6(3) . . . . ?
V1 O3 C14 C13 -175.19(13) . . . . ?
V1 O3 C14 C9 5.0(3) . . . . ?
C12 C13 C14 O3 -179.74(16) . . . . ?
C12 C13 C14 C9 0.1(2) . . . . ?
C10 C9 C14 O3 179.38(15) . . . . ?
C8 C9 C14 O3 -0.3(3) . . . . ?
C10 C9 C14 C13 -0.5(2) . . . . ?
C8 C9 C14 C13 179.83(15) . . . . ?
O9 V2 O7 C21 120.52(13) . . . . ?
O10 V2 O7 C21 -130.25(13) . . . . ?
O8 V2 O7 C21 -10.3(2) . . . . ?
N4 V2 O7 C21 -1.03(12) . . . . ?
O9 V2 O8 C28 -114.5(2) . . . . ?
O10 V2 O8 C28 135.7(2) . . . . ?
O7 V2 O8 C28 16.3(3) . . . . ?
N4 V2 O8 C28 7.36(19) . . . . ?
C21 N3 N4 C22 179.15(14) . . . . ?
C21 N3 N4 V2 0.03(17) . . . . ?
O9 V2 N4 C22 92.32(16) . . . . ?
O10 V2 N4 C22 -95.98(16) . . . . ?
O8 V2 N4 C22 -2.04(16) . . . . ?
O7 V2 N4 C22 -178.41(16) . . . . ?
O9 V2 N4 N3 -88.74(12) . . . . ?
O10 V2 N4 N3 82.95(13) . . . . ?
O8 V2 N4 N3 176.90(12) . . . . ?
O7 V2 N4 N3 0.52(10) . . . . ?
O6 C15 C16 C17 179.18(16) . . . . ?
C20 C15 C16 C17 -0.9(3) . . . . ?
C15 C16 C17 C18 0.6(3) . . . . ?
C16 C17 C18 C19 0.1(3) . . . . ?
C17 C18 C19 C20 -0.6(3) . . . . ?
C18 C19 C20 C15 0.3(3) . . . . ?
C18 C19 C20 C21 -179.90(16) . . . . ?
O6 C15 C20 C19 -179.65(16) . . . . ?
C16 C15 C20 C19 0.4(3) . . . . ?
O6 C15 C20 C21 0.6(3) . . . . ?
C16 C15 C20 C21 -179.37(16) . . . . ?
N4 N3 C21 O7 -1.0(2) . . . . ?
N4 N3 C21 C20 178.79(14) . . . . ?
V2 O7 C21 N3 1.5(2) . . . . ?
V2 O7 C21 C20 -178.22(11) . . . . ?
C19 C20 C21 N3 -178.08(15) . . . . ?
C15 C20 C21 N3 1.7(2) . . . . ?
C19 C20 C21 O7 1.7(2) . . . . ?
C15 C20 C21 O7 -178.57(15) . . . . ?
N3 N4 C22 C23 179.59(15) . . . . ?
V2 N4 C22 C23 -1.5(3) . . . . ?
N4 C22 C23 C28 2.3(3) . . . . ?
N4 C22 C23 C24 -177.97(16) . . . . ?
C28 C23 C24 C25 -0.7(3) . . . . ?
C22 C23 C24 C25 179.55(16) . . . . ?
C23 C24 C25 C26 0.7(3) . . . . ?
C24 C25 C26 C27 -0.6(3) . . . . ?
C25 C26 C27 C28 0.7(3) . . . . ?
V2 O8 C28 C27 172.99(14) . . . . ?
V2 O8 C28 C23 -8.5(3) . . . . ?
C26 C27 C28 O8 177.77(17) . . . . ?
C26 C27 C28 C23 -0.8(3) . . . . ?
C24 C23 C28 O8 -177.73(16) . . . . ?
C22 C23 C28 O8 2.0(3) . . . . ?
C24 C23 C28 C27 0.8(3) . . . . ?
C22 C23 C28 C27 -179.52(16) . . . . ?
O3W Li1 Li2 O5W 169.22(19) . . . . ?
O4W Li1 Li2 O5W 30.7(2) . . . . ?
O2W Li1 Li2 O5W -75.61(17) . . . . ?
O1W Li1 Li2 O5W 119.8(2) . . . . ?
O3W Li1 Li2 O6W -78.7(2) . . . . ?
O4W Li1 Li2 O6W 142.82(17) . . . . ?
O2W Li1 Li2 O6W 36.52(15) . . . . ?
O1W Li1 Li2 O6W -128.1(2) . . . . ?
O3W Li1 Li2 O7W 41.3(3) . . . . ?
O4W Li1 Li2 O7W -97.3(3) . . . . ?
O2W Li1 Li2 O7W 156.4(2) . . . . ?
O1W Li1 Li2 O7W -8.2(2) . . . . ?
O3W Li1 Li2 O1W 49.4(2) . . . . ?
O4W Li1 Li2 O1W -89.1(2) . . . . ?
O2W Li1 Li2 O1W 164.6(2) . . . . ?
O3W Li1 O1W Li2 -139.29(17) . . . . ?
O4W Li1 O1W Li2 99.7(2) . . . . ?
O2W Li1 O1W Li2 -17.0(3) . . . . ?
O5W Li2 O1W Li1 -67.4(3) . . . . ?
O6W Li2 O1W Li1 53.7(2) . . . . ?
O7W Li2 O1W Li1 173.96(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.070
_database_code_depnum_ccdc_archive 'CCDC 991925'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N2 O4 V, H2 O, Cs'
_chemical_formula_sum            'C15 H14 Cs N2 O5 V'
_chemical_formula_weight         486.13

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   15.430(2)
_cell_length_b                   7.1128(10)
_cell_length_c                   30.505(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.682(8)
_cell_angle_gamma                90.00
_cell_volume                     3309.5(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    228
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    2.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.4877
_exptl_absorpt_correction_T_max  0.8964

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            107431
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         28.43
_reflns_number_total             8117
_reflns_number_gt                6866
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (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 > 2σ(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)+(0.0186P)²+5.7119P] 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         8117
_refine_ls_number_parameters     447
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0594
_refine_ls_wR_factor_gt          0.0540
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.128
_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 0.31421(3) 0.50616(6) 0.419472(15) 0.01389(10) Uani 1 1 d . . .
O1 O 0.22169(13) 0.6833(3) 0.41094(6) 0.0190(4) Uani 1 1 d . . .
O2 O 0.36688(13) 0.2759(3) 0.39947(6) 0.0169(4) Uani 1 1 d . . .
O3 O 0.27466(14) 0.3941(3) 0.45887(6) 0.0207(4) Uani 1 1 d . . .
O4 O 0.40053(14) 0.6258(3) 0.44121(7) 0.0237(5) Uani 1 1 d . . .
N1 N 0.30898(15) 0.5391(3) 0.34910(7) 0.0142(5) Uani 1 1 d . . .
N2 N 0.35430(15) 0.4004(3) 0.32924(7) 0.0156(5) Uani 1 1 d . . .
C1 C 0.20533(18) 0.8290(4) 0.38309(9) 0.0155(6) Uani 1 1 d . . .
C2 C 0.15969(19) 0.9826(4) 0.39728(10) 0.0194(6) Uani 1 1 d . . .
H2 H 0.1411 0.9785 0.4256 0.023 Uiso 1 1 calc R . .
C3 C 0.14130(19) 1.1395(4) 0.37095(10) 0.0209(6) Uani 1 1 d . . .
H3 H 0.1109 1.2428 0.3812 0.025 Uiso 1 1 calc R . .
C4 C 0.1675(2) 1.1457(4) 0.32929(10) 0.0235(7) Uani 1 1 d . . .
H4 H 0.1557 1.2537 0.3111 0.028 Uiso 1 1 calc R . .
C5 C 0.21059(19) 0.9950(4) 0.31479(10) 0.0195(6) Uani 1 1 d . . .
H5 H 0.2270 1.0002 0.2860 0.023 Uiso 1 1 calc R . .
C6 C 0.23163(18) 0.8326(4) 0.34069(9) 0.0150(5) Uani 1 1 d . . .
C7 C 0.27789(18) 0.6772(4) 0.32321(9) 0.0151(6) Uani 1 1 d . . .
C8 C 0.2910(2) 0.6825(4) 0.27542(9) 0.0213(6) Uani 1 1 d . . .
H8A H 0.3326 0.7825 0.2712 0.032 Uiso 1 1 calc R . .
H8B H 0.2347 0.7072 0.2567 0.032 Uiso 1 1 calc R . .
H8C H 0.3141 0.5613 0.2672 0.032 Uiso 1 1 calc R . .
C9 C 0.38241(18) 0.2728(4) 0.35834(9) 0.0143(5) Uani 1 1 d . . .
C10 C 0.43278(18) 0.1128(4) 0.34391(9) 0.0146(5) Uani 1 1 d . . .
C11 C 0.45522(19) 0.1110(4) 0.30116(9) 0.0185(6) Uani 1 1 d . . .
H11 H 0.4378 0.2122 0.2815 0.022 Uiso 1 1 calc R . .
C12 C 0.5025(2) -0.0370(4) 0.28745(10) 0.0233(7) Uani 1 1 d . . .
H12 H 0.5179 -0.0363 0.2584 0.028 Uiso 1 1 calc R . .
C13 C 0.5278(2) -0.1865(4) 0.31567(10) 0.0216(6) Uani 1 1 d . . .
H13 H 0.5604 -0.2879 0.3061 0.026 Uiso 1 1 calc R . .
C14 C 0.50511(19) -0.1869(4) 0.35796(10) 0.0208(6) Uani 1 1 d . . .
H14 H 0.5214 -0.2898 0.3773 0.025 Uiso 1 1 calc R . .
C15 C 0.45868(19) -0.0376(4) 0.37204(10) 0.0189(6) Uani 1 1 d . . .
H15 H 0.4444 -0.0378 0.4013 0.023 Uiso 1 1 calc R . .
V2 V 0.15908(3) 0.09752(6) 0.566620(14) 0.01348(10) Uani 1 1 d . . .
N3 N 0.19496(15) 0.1316(3) 0.63745(7) 0.0136(5) Uani 1 1 d . . .
N4 N 0.16121(15) -0.0046(3) 0.66347(7) 0.0153(5) Uani 1 1 d . . .
O5 O 0.26326(13) 0.2350(3) 0.56633(6) 0.0181(4) Uani 1 1 d . . .
O6 O 0.11633(13) -0.1270(3) 0.59407(6) 0.0154(4) Uani 1 1 d . . .
O7 O 0.16170(13) -0.0148(3) 0.51938(6) 0.0184(4) Uani 1 1 d . . .
O8 O 0.07911(13) 0.2468(3) 0.55854(6) 0.0199(4) Uani 1 1 d . . .
C16 C 0.28867(18) 0.3913(4) 0.58953(9) 0.0147(5) Uani 1 1 d . . .
C17 C 0.3348(2) 0.5273(4) 0.56900(9) 0.0194(6) Uani 1 1 d . . .
H17 H 0.3476 0.5054 0.5399 0.023 Uiso 1 1 calc R . .
C18 C 0.3619(2) 0.6925(4) 0.59053(10) 0.0212(6) Uani 1 1 d . . .
H18 H 0.3934 0.7828 0.5763 0.025 Uiso 1 1 calc R . .
C19 C 0.3431(2) 0.7274(4) 0.63297(10) 0.0209(6) Uani 1 1 d . . .
H19 H 0.3597 0.8432 0.6474 0.025 Uiso 1 1 calc R . .
C20 C 0.30033(19) 0.5924(4) 0.65391(9) 0.0177(6) Uani 1 1 d . . .
H20 H 0.2892 0.6158 0.6832 0.021 Uiso 1 1 calc R . .
C21 C 0.27242(18) 0.4203(4) 0.63340(9) 0.0151(5) Uani 1 1 d . . .
C22 C 0.23259(18) 0.2766(4) 0.65813(9) 0.0142(5) Uani 1 1 d . . .
C23 C 0.2344(2) 0.3007(4) 0.70726(9) 0.0202(6) Uani 1 1 d . . .
H23A H 0.1908 0.3948 0.7126 0.030 Uiso 1 1 calc R . .
H23B H 0.2928 0.3425 0.7209 0.030 Uiso 1 1 calc R . .
H23C H 0.2207 0.1804 0.7203 0.030 Uiso 1 1 calc R . .
C24 C 0.12070(18) -0.1309(4) 0.63748(9) 0.0136(5) Uani 1 1 d . . .
C25 C 0.07765(18) -0.2914(4) 0.65664(9) 0.0145(5) Uani 1 1 d . . .
C26 C 0.06005(19) -0.2855(4) 0.70019(9) 0.0176(6) Uani 1 1 d . . .
H26 H 0.0784 -0.1805 0.7185 0.021 Uiso 1 1 calc R . .
C27 C 0.0157(2) -0.4331(4) 0.71673(10) 0.0203(6) Uani 1 1 d . . .
H27 H 0.0040 -0.4286 0.7464 0.024 Uiso 1 1 calc R . .
C28 C -0.0115(2) -0.5874(4) 0.69023(10) 0.0210(6) Uani 1 1 d . . .
H28 H -0.0430 -0.6866 0.7015 0.025 Uiso 1 1 calc R . .
C29 C 0.00748(19) -0.5958(4) 0.64716(9) 0.0178(6) Uani 1 1 d . . .
H29 H -0.0099 -0.7021 0.6291 0.021 Uiso 1 1 calc R . .
C30 C 0.05176(18) -0.4488(4) 0.63066(9) 0.0161(6) Uani 1 1 d . . .
H30 H 0.0647 -0.4553 0.6012 0.019 Uiso 1 1 calc R . .
Cs1 Cs 0.334800(12) 0.01514(2) 0.485145(6) 0.01687(5) Uani 1 1 d . . .
Cs2 Cs 0.123036(12) -0.41337(2) 0.492030(6) 0.01960(5) Uani 1 1 d . . .
O1W O 0.50006(15) 0.2458(3) 0.48336(7) 0.0244(5) Uani 1 1 d D . .
H1W1 H 0.472(2) 0.324(3) 0.4663(8) 0.037 Uiso 1 1 d D . .
H1W2 H 0.529(2) 0.299(4) 0.5056(7) 0.037 Uiso 1 1 d D . .
O2W O 0.03509(14) -0.7693(3) 0.46180(7) 0.0223(5) Uani 1 1 d D . .
H2W1 H -0.0043(16) -0.825(4) 0.4442(9) 0.033 Uiso 1 1 d D . .
H2W2 H 0.0660(18) -0.848(3) 0.4780(9) 0.033 Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 1.634(2) . ?
V1 O3 1.6352(19) . ?
V1 O1 1.892(2) . ?
V1 O2 1.9656(19) . ?
V1 N1 2.149(2) . ?
V1 Cs2 3.9873(7) 1_565 ?
V1 Cs1 4.0150(7) . ?
V1 Cs1 4.1266(7) 1_565 ?
O1 C1 1.340(3) . ?
O1 Cs2 3.1694(19) 1_565 ?
O1 Cs1 3.542(2) 1_565 ?
O2 C9 1.313(3) . ?
O2 Cs1 3.3026(18) . ?
O3 Cs1 2.923(2) . ?
O3 Cs2 3.014(2) 1_565 ?
O4 Cs1 3.302(2) 1_565 ?
N1 C7 1.305(4) . ?
N1 N2 1.399(3) . ?
N2 C9 1.298(4) . ?
C1 C2 1.403(4) . ?
C1 C6 1.413(4) . ?
C1 Cs1 3.682(3) 1_565 ?
C2 C3 1.379(4) . ?
C2 Cs1 3.514(3) 1_565 ?
C2 H2 0.9500 . ?
C3 C4 1.392(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.410(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.459(4) . ?
C7 C8 1.502(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.482(4) . ?
C10 C15 1.392(4) . ?
C10 C11 1.399(4) . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
V2 O8 1.618(2) . ?
V2 O7 1.6534(19) . ?
V2 O5 1.883(2) . ?
V2 O6 1.9631(19) . ?
V2 N3 2.162(2) . ?
V2 Cs1 3.9883(7) . ?
V2 Cs2 4.1482(7) 1_565 ?
V2 Cs2 4.2790(7) . ?
N3 C22 1.299(3) . ?
N3 N4 1.402(3) . ?
N4 C24 1.295(4) . ?
O5 C16 1.344(3) . ?
O5 Cs1 3.2591(19) . ?
O6 C24 1.316(3) . ?
O6 Cs2 3.7344(19) . ?
O7 Cs2 2.9900(19) . ?
O7 Cs1 3.019(2) . ?
O8 Cs2 3.292(2) 1_565 ?
O8 Cs2 3.473(2) 3_556 ?
C16 C17 1.404(4) . ?
C16 C21 1.413(4) . ?
C16 Cs2 3.875(3) 1_565 ?
C17 C18 1.379(4) . ?
C17 Cs2 3.749(3) 1_565 ?
C17 H17 0.9500 . ?
C18 C19 1.391(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.376(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.412(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.460(4) . ?
C22 C23 1.505(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.484(4) . ?
C25 C30 1.395(4) . ?
C25 C26 1.396(4) . ?
C26 C27 1.389(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.385(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
Cs1 O1W 3.039(2) . ?
Cs1 O1W 3.181(2) 3_656 ?
Cs1 O4 3.302(2) 1_545 ?
Cs1 C2 3.514(3) 1_545 ?
Cs1 O1 3.542(2) 1_545 ?
Cs1 C1 3.682(3) 1_545 ?
Cs1 H1W1 3.17(3) . ?
Cs2 O2W 2.953(2) . ?
Cs2 O3 3.014(2) 1_545 ?
Cs2 O1 3.1694(19) 1_545 ?
Cs2 O2W 3.265(2) 3_546 ?
Cs2 O8 3.292(2) 1_545 ?
Cs2 O8 3.473(2) 3_556 ?
Cs2 C17 3.749(3) 1_545 ?
Cs2 C16 3.875(3) 1_545 ?
Cs2 V1 3.9873(7) 1_545 ?
Cs2 Cs2 4.0900(7) 3_546 ?
Cs2 H2W2 3.22(3) . ?
O1W Cs1 3.181(2) 3_656 ?
O1W H1W1 0.837(10) . ?
O1W H1W2 0.844(10) . ?
O2W Cs2 3.265(2) 3_546 ?
O2W H2W1 0.847(10) . ?
O2W H2W2 0.845(10) . ?

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
O4 V1 O3 109.10(11) . . ?
O4 V1 O1 105.12(10) . . ?
O3 V1 O1 93.91(9) . . ?
O4 V1 O2 102.11(10) . . ?
O3 V1 O2 92.28(9) . . ?
O1 V1 O2 148.28(9) . . ?
O4 V1 N1 104.71(10) . . ?
O3 V1 N1 145.65(10) . . ?
O1 V1 N1 82.89(8) . . ?
O2 V1 N1 74.68(8) . . ?
O4 V1 Cs2 109.02(8) . 1_565 ?
O3 V1 Cs2 43.32(7) . 1_565 ?
O1 V1 Cs2 51.30(6) . 1_565 ?
O2 V1 Cs2 131.84(6) . 1_565 ?
N1 V1 Cs2 128.28(6) . 1_565 ?
O4 V1 Cs1 104.61(8) . . ?
O3 V1 Cs1 38.69(7) . . ?
O1 V1 Cs1 130.47(6) . . ?
O2 V1 Cs1 54.90(5) . . ?
N1 V1 Cs1 125.57(6) . . ?
Cs2 V1 Cs1 81.798(11) 1_565 . ?
O4 V1 Cs1 49.31(8) . 1_565 ?
O3 V1 Cs1 94.63(7) . 1_565 ?
O1 V1 Cs1 58.93(7) . 1_565 ?
O2 V1 Cs1 151.21(6) . 1_565 ?
N1 V1 Cs1 112.20(6) . 1_565 ?
Cs2 V1 Cs1 67.280(9) 1_565 1_565 ?
Cs1 V1 Cs1 121.763(15) . 1_565 ?
C1 O1 V1 131.94(18) . . ?
C1 O1 Cs2 126.58(16) . 1_565 ?
V1 O1 Cs2 100.92(7) . 1_565 ?
C1 O1 Cs1 85.24(15) . 1_565 ?
V1 O1 Cs1 93.85(8) . 1_565 ?
Cs2 O1 Cs1 83.92(4) 1_565 1_565 ?
C9 O2 V1 117.05(17) . . ?
C9 O2 Cs1 144.84(16) . . ?
V1 O2 Cs1 95.97(6) . . ?
V1 O3 Cs1 120.85(9) . . ?
V1 O3 Cs2 114.83(9) . 1_565 ?
Cs1 O3 Cs2 123.87(7) . 1_565 ?
V1 O4 Cs1 108.65(10) . 1_565 ?
C7 N1 N2 115.5(2) . . ?
C7 N1 V1 129.89(19) . . ?
N2 N1 V1 114.18(16) . . ?
C9 N2 N1 109.6(2) . . ?
O1 C1 C2 117.5(2) . . ?
O1 C1 C6 122.8(2) . . ?
C2 C1 C6 119.7(3) . . ?
O1 C1 Cs1 73.49(14) . 1_565 ?
C2 C1 Cs1 72.11(16) . 1_565 ?
C6 C1 Cs1 124.99(18) . 1_565 ?
C3 C2 C1 121.3(3) . . ?
C3 C2 Cs1 117.3(2) . 1_565 ?
C1 C2 Cs1 85.56(17) . 1_565 ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
Cs1 C2 H2 67.2 1_565 . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 122.8(3) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C5 C6 C1 117.0(3) . . ?
C5 C6 C7 120.0(2) . . ?
C1 C6 C7 123.0(2) . . ?
N1 C7 C6 120.3(2) . . ?
N1 C7 C8 121.0(3) . . ?
C6 C7 C8 118.7(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 O2 123.5(2) . . ?
N2 C9 C10 118.0(2) . . ?
O2 C9 C10 118.5(2) . . ?
C15 C10 C11 118.6(3) . . ?
C15 C10 C9 121.4(2) . . ?
C11 C10 C9 119.9(2) . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.5(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.5(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C10 120.8(3) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
O8 V2 O7 107.61(10) . . ?
O8 V2 O5 106.90(10) . . ?
O7 V2 O5 96.52(9) . . ?
O8 V2 O6 107.53(10) . . ?
O7 V2 O6 91.88(9) . . ?
O5 V2 O6 140.05(9) . . ?
O8 V2 N3 98.81(9) . . ?
O7 V2 N3 152.76(10) . . ?
O5 V2 N3 81.75(9) . . ?
O6 V2 N3 73.55(8) . . ?
O8 V2 Cs1 125.16(7) . . ?
O7 V2 Cs1 43.74(7) . . ?
O5 V2 Cs1 53.99(6) . . ?
O6 V2 Cs1 116.75(6) . . ?
N3 V2 Cs1 122.94(6) . . ?
O8 V2 Cs2 47.95(7) . 1_565 ?
O7 V2 Cs2 86.90(7) . 1_565 ?
O5 V2 Cs2 66.78(6) . 1_565 ?
O6 V2 Cs2 152.93(6) . 1_565 ?
N3 V2 Cs2 116.56(6) . 1_565 ?
Cs1 V2 Cs2 80.145(11) . 1_565 ?
O8 V2 Cs2 116.18(8) . . ?
O7 V2 Cs2 31.20(7) . . ?
O5 V2 Cs2 118.75(6) . . ?
O6 V2 Cs2 60.71(5) . . ?
N3 V2 Cs2 128.31(6) . . ?
Cs1 V2 Cs2 65.786(9) . . ?
Cs2 V2 Cs2 115.127(15) 1_565 . ?
C22 N3 N4 116.8(2) . . ?
C22 N3 V2 127.06(18) . . ?
N4 N3 V2 115.30(16) . . ?
C24 N4 N3 108.6(2) . . ?
C16 O5 V2 127.47(17) . . ?
C16 O5 Cs1 133.75(16) . . ?
V2 O5 Cs1 98.16(7) . . ?
C24 O6 V2 118.47(17) . . ?
C24 O6 Cs2 145.45(16) . . ?
V2 O6 Cs2 92.00(6) . . ?
V2 O7 Cs2 132.16(9) . . ?
V2 O7 Cs1 114.01(9) . . ?
Cs2 O7 Cs1 96.89(5) . . ?
V2 O8 Cs2 110.64(9) . 1_565 ?
V2 O8 Cs2 154.78(10) . 3_556 ?
Cs2 O8 Cs2 74.35(4) 1_565 3_556 ?
O5 C16 C17 117.6(2) . . ?
O5 C16 C21 122.7(2) . . ?
C17 C16 C21 119.7(3) . . ?
O5 C16 Cs2 77.66(14) . 1_565 ?
C17 C16 Cs2 74.37(16) . 1_565 ?
C21 C16 Cs2 118.92(18) . 1_565 ?
C18 C17 C16 120.8(3) . . ?
C18 C17 Cs2 112.02(19) . 1_565 ?
C16 C17 Cs2 84.49(17) . 1_565 ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
Cs2 C17 H17 73.6 1_565 . ?
C17 C18 C19 120.3(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C20 C19 C18 119.3(3) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C21 122.3(3) . . ?
C19 C20 H20 118.8 . . ?
C21 C20 H20 118.8 . . ?
C20 C21 C16 117.4(2) . . ?
C20 C21 C22 120.1(2) . . ?
C16 C21 C22 122.4(2) . . ?
N3 C22 C21 119.8(2) . . ?
N3 C22 C23 120.9(2) . . ?
C21 C22 C23 119.3(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 O6 123.2(2) . . ?
N4 C24 C25 119.7(2) . . ?
O6 C24 C25 117.0(2) . . ?
C30 C25 C26 119.0(3) . . ?
C30 C25 C24 120.0(2) . . ?
C26 C25 C24 121.0(2) . . ?
C27 C26 C25 120.0(3) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.5(3) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C29 119.7(3) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 119.8(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C25 120.9(3) . . ?
C29 C30 H30 119.5 . . ?
C25 C30 H30 119.5 . . ?
O3 Cs1 O7 84.20(5) . . ?
O3 Cs1 O1W 74.33(6) . . ?
O7 Cs1 O1W 146.38(6) . . ?
O3 Cs1 O1W 145.83(6) . 3_656 ?
O7 Cs1 O1W 124.37(6) . 3_656 ?
O1W Cs1 O1W 71.60(6) . 3_656 ?
O3 Cs1 O5 68.65(5) . . ?
O7 Cs1 O5 49.61(5) . . ?
O1W Cs1 O5 97.81(6) . . ?
O1W Cs1 O5 113.46(5) 3_656 . ?
O3 Cs1 O4 140.02(5) . 1_545 ?
O7 Cs1 O4 115.05(5) . 1_545 ?
O1W Cs1 O4 97.79(6) . 1_545 ?
O1W Cs1 O4 49.63(5) 3_656 1_545 ?
O5 Cs1 O4 150.55(5) . 1_545 ?
O3 Cs1 O2 49.03(5) . . ?
O7 Cs1 O2 124.02(5) . . ?
O1W Cs1 O2 57.06(5) . . ?
O1W Cs1 O2 110.96(5) 3_656 . ?
O5 Cs1 O2 116.12(5) . . ?
O4 Cs1 O2 93.32(5) 1_545 . ?
O3 Cs1 C2 71.09(6) . 1_545 ?
O7 Cs1 C2 68.94(6) . 1_545 ?
O1W Cs1 C2 124.91(6) . 1_545 ?
O1W Cs1 C2 132.88(6) 3_656 1_545 ?
O5 Cs1 C2 107.55(6) . 1_545 ?
O4 Cs1 C2 83.29(6) 1_545 1_545 ?
O2 Cs1 C2 67.87(6) . 1_545 ?
O3 Cs1 O1 109.50(5) . 1_545 ?
O7 Cs1 O1 78.34(5) . 1_545 ?
O1W Cs1 O1 133.00(5) . 1_545 ?
O1W Cs1 O1 95.69(5) 3_656 1_545 ?
O5 Cs1 O1 127.92(5) . 1_545 ?
O4 Cs1 O1 48.22(5) 1_545 1_545 ?
O2 Cs1 O1 89.25(5) . 1_545 ?
C2 Cs1 O1 38.82(6) 1_545 1_545 ?
O3 Cs1 C1 89.45(6) . 1_545 ?
O7 Cs1 C1 82.63(6) . 1_545 ?
O1W Cs1 C1 121.90(6) . 1_545 ?
O1W Cs1 C1 110.68(6) 3_656 1_545 ?
O5 Cs1 C1 127.75(6) . 1_545 ?
O4 Cs1 C1 61.05(6) 1_545 1_545 ?
O2 Cs1 C1 70.12(6) . 1_545 ?
C2 Cs1 C1 22.33(6) 1_545 1_545 ?
O1 Cs1 C1 21.26(5) 1_545 1_545 ?
O3 Cs1 V2 79.50(4) . . ?
O7 Cs1 V2 22.25(4) . . ?
O1W Cs1 V2 125.66(4) . . ?
O1W Cs1 V2 119.10(4) 3_656 . ?
O5 Cs1 V2 27.86(3) . . ?
O4 Cs1 V2 130.96(4) 1_545 . ?
O2 Cs1 V2 127.43(3) . . ?
C2 Cs1 V2 88.18(5) 1_545 . ?
O1 Cs1 V2 100.39(3) 1_545 . ?
C1 Cs1 V2 104.28(4) 1_545 . ?
O3 Cs1 V1 20.47(4) . . ?
O7 Cs1 V1 103.09(4) . . ?
O1W Cs1 V1 61.64(4) . . ?
O1W Cs1 V1 131.12(4) 3_656 . ?
O5 Cs1 V1 87.22(4) . . ?
O4 Cs1 V1 122.21(4) 1_545 . ?
O2 Cs1 V1 29.14(3) . . ?
C2 Cs1 V1 71.51(5) 1_545 . ?
O1 Cs1 V1 105.46(3) 1_545 . ?
C1 Cs1 V1 84.20(4) 1_545 . ?
V2 Cs1 V1 99.969(12) . . ?
O3 Cs1 H1W1 60.2(4) . . ?
O7 Cs1 H1W1 139.8(5) . . ?
O1W Cs1 H1W1 15.3(2) . . ?
O1W Cs1 H1W1 86.1(3) 3_656 . ?
O5 Cs1 H1W1 96.8(6) . . ?
O4 Cs1 H1W1 104.7(6) 1_545 . ?
O2 Cs1 H1W1 44.1(3) . . ?
C2 Cs1 H1W1 111.5(3) 1_545 . ?
O1 Cs1 H1W1 128.7(5) 1_545 . ?
C1 Cs1 H1W1 112.9(4) 1_545 . ?
V2 Cs1 H1W1 123.2(6) . . ?
V1 Cs1 H1W1 46.4(3) . . ?
O2W Cs2 O7 164.33(6) . . ?
O2W Cs2 O3 81.32(6) . 1_545 ?
O7 Cs2 O3 113.09(6) . 1_545 ?
O2W Cs2 O1 101.21(6) . 1_545 ?
O7 Cs2 O1 85.01(5) . 1_545 ?
O3 Cs2 O1 49.32(5) 1_545 1_545 ?
O2W Cs2 O2W 97.92(5) . 3_546 ?
O7 Cs2 O2W 68.47(5) . 3_546 ?
O3 Cs2 O2W 173.63(5) 1_545 3_546 ?
O1 Cs2 O2W 136.76(5) 1_545 3_546 ?
O2W Cs2 O8 55.62(5) . 1_545 ?
O7 Cs2 O8 125.12(5) . 1_545 ?
O3 Cs2 O8 96.64(5) 1_545 1_545 ?
O1 Cs2 O8 143.92(5) 1_545 1_545 ?
O2W Cs2 O8 77.85(5) 3_546 1_545 ?
O2W Cs2 O8 79.30(6) . 3_556 ?
O7 Cs2 O8 85.89(5) . 3_556 ?
O3 Cs2 O8 134.15(5) 1_545 3_556 ?
O1 Cs2 O8 94.83(5) 1_545 3_556 ?
O2W Cs2 O8 51.42(5) 3_546 3_556 ?
O8 Cs2 O8 105.65(4) 1_545 3_556 ?
O2W Cs2 O6 131.19(5) . . ?
O7 Cs2 O6 43.92(5) . . ?
O3 Cs2 O6 130.39(5) 1_545 . ?
O1 Cs2 O6 127.54(5) 1_545 . ?
O2W Cs2 O6 46.13(5) 3_546 . ?
O8 Cs2 O6 81.52(5) 1_545 . ?
O8 Cs2 O6 92.76(4) 3_556 . ?
O2W Cs2 C17 114.53(6) . 1_545 ?
O7 Cs2 C17 79.26(6) . 1_545 ?
O3 Cs2 C17 60.77(6) 1_545 1_545 ?
O1 Cs2 C17 92.14(6) 1_545 1_545 ?
O2W Cs2 C17 114.34(6) 3_546 1_545 ?
O8 Cs2 C17 76.85(6) 1_545 1_545 ?
O8 Cs2 C17 162.98(6) 3_556 1_545 ?
O6 Cs2 C17 70.76(5) . 1_545 ?
O2W Cs2 C16 98.69(6) . 1_545 ?
O7 Cs2 C16 92.59(6) . 1_545 ?
O3 Cs2 C16 68.85(6) 1_545 1_545 ?
O1 Cs2 C16 109.76(5) 1_545 1_545 ?
O2W Cs2 C16 105.12(6) 3_546 1_545 ?
O8 Cs2 C16 55.73(5) 1_545 1_545 ?
O8 Cs2 C16 155.15(5) 3_556 1_545 ?
O6 Cs2 C16 69.75(5) . 1_545 ?
C17 Cs2 C16 21.14(6) 1_545 1_545 ?
O2W Cs2 V1 92.70(4) . 1_545 ?
O7 Cs2 V1 99.08(4) . 1_545 ?
O3 Cs2 V1 21.85(4) 1_545 1_545 ?
O1 Cs2 V1 27.77(4) 1_545 1_545 ?
O2W Cs2 V1 163.76(4) 3_546 1_545 ?
O8 Cs2 V1 118.37(4) 1_545 1_545 ?
O8 Cs2 V1 119.51(3) 3_556 1_545 ?
O6 Cs2 V1 131.06(3) . 1_545 ?
C17 Cs2 V1 71.55(5) 1_545 1_545 ?
C16 Cs2 V1 85.25(4) 1_545 1_545 ?
O2W Cs2 Cs2 52.25(4) . 3_546 ?
O7 Cs2 Cs2 113.72(4) . 3_546 ?
O3 Cs2 Cs2 133.19(4) 1_545 3_546 ?
O1 Cs2 Cs2 136.22(4) 1_545 3_546 ?
O2W Cs2 Cs2 45.66(4) 3_546 3_546 ?
O8 Cs2 Cs2 54.84(4) 1_545 3_546 ?
O8 Cs2 Cs2 50.80(3) 3_556 3_546 ?
O6 Cs2 Cs2 85.54(3) . 3_546 ?
C17 Cs2 Cs2 128.96(5) 1_545 3_546 ?
C16 Cs2 Cs2 108.50(4) 1_545 3_546 ?
V1 Cs2 Cs2 143.183(11) 1_545 3_546 ?
O2W Cs2 H2W2 14.9(3) . . ?
O7 Cs2 H2W2 170.0(6) . . ?
O3 Cs2 H2W2 74.3(6) 1_545 . ?
O1 Cs2 H2W2 105.0(6) 1_545 . ?
O2W Cs2 H2W2 103.4(6) 3_546 . ?
O8 Cs2 H2W2 45.6(5) 1_545 . ?
O8 Cs2 H2W2 93.4(3) 3_556 . ?
O6 Cs2 H2W2 126.3(6) . . ?
C17 Cs2 H2W2 99.8(3) 1_545 . ?
C16 Cs2 H2W2 83.9(3) 1_545 . ?
V1 Cs2 H2W2 89.9(6) 1_545 . ?
Cs2 Cs2 H2W2 59.2(6) 3_546 . ?
Cs1 O1W Cs1 108.40(6) . 3_656 ?
Cs1 O1W H1W1 91(2) . . ?
Cs1 O1W H1W1 153(3) 3_656 . ?
Cs1 O1W H1W2 125(3) . . ?
Cs1 O1W H1W2 74(2) 3_656 . ?
H1W1 O1W H1W2 110.9(17) . . ?
Cs2 O2W Cs2 82.08(5) . 3_546 ?
Cs2 O2W H2W1 149(2) . . ?
Cs2 O2W H2W1 87(2) 3_546 . ?
Cs2 O2W H2W2 101(2) . . ?
Cs2 O2W H2W2 114(2) 3_546 . ?
H2W1 O2W H2W2 110.3(16) . . ?

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
O4 V1 O1 C1 69.1(3) . . . . ?
O3 V1 O1 C1 -179.9(2) . . . . ?
O2 V1 O1 C1 -79.2(3) . . . . ?
N1 V1 O1 C1 -34.3(2) . . . . ?
Cs2 V1 O1 C1 171.6(3) 1_565 . . . ?
Cs1 V1 O1 C1 -165.9(2) . . . . ?
Cs1 V1 O1 C1 87.1(2) 1_565 . . . ?
O4 V1 O1 Cs2 -102.48(9) . . . 1_565 ?
O3 V1 O1 Cs2 8.51(9) . . . 1_565 ?
O2 V1 O1 Cs2 109.25(14) . . . 1_565 ?
N1 V1 O1 Cs2 154.15(9) . . . 1_565 ?
Cs1 V1 O1 Cs2 22.54(10) . . . 1_565 ?
Cs1 V1 O1 Cs2 -84.54(6) 1_565 . . 1_565 ?
O4 V1 O1 Cs1 -17.94(9) . . . 1_565 ?
O3 V1 O1 Cs1 93.05(8) . . . 1_565 ?
O2 V1 O1 Cs1 -166.21(13) . . . 1_565 ?
N1 V1 O1 Cs1 -121.31(7) . . . 1_565 ?
Cs2 V1 O1 Cs1 84.54(6) 1_565 . . 1_565 ?
Cs1 V1 O1 Cs1 107.08(6) . . . 1_565 ?
O4 V1 O2 C9 -93.0(2) . . . . ?
O3 V1 O2 C9 156.9(2) . . . . ?
O1 V1 O2 C9 55.7(3) . . . . ?
N1 V1 O2 C9 9.11(19) . . . . ?
Cs2 V1 O2 C9 137.20(17) 1_565 . . . ?
Cs1 V1 O2 C9 167.5(2) . . . . ?
Cs1 V1 O2 C9 -99.2(2) 1_565 . . . ?
O4 V1 O2 Cs1 99.46(9) . . . . ?
O3 V1 O2 Cs1 -10.63(9) . . . . ?
O1 V1 O2 Cs1 -111.82(14) . . . . ?
N1 V1 O2 Cs1 -158.39(9) . . . . ?
Cs2 V1 O2 Cs1 -30.29(9) 1_565 . . . ?
Cs1 V1 O2 Cs1 93.26(11) 1_565 . . . ?
O4 V1 O3 Cs1 -89.68(13) . . . . ?
O1 V1 O3 Cs1 162.84(11) . . . . ?
O2 V1 O3 Cs1 13.97(12) . . . . ?
N1 V1 O3 Cs1 79.74(19) . . . . ?
Cs2 V1 O3 Cs1 172.53(18) 1_565 . . . ?
Cs1 V1 O3 Cs1 -138.06(9) 1_565 . . . ?
O4 V1 O3 Cs2 97.79(12) . . . 1_565 ?
O1 V1 O3 Cs2 -9.69(11) . . . 1_565 ?
O2 V1 O3 Cs2 -158.56(10) . . . 1_565 ?
N1 V1 O3 Cs2 -92.79(17) . . . 1_565 ?
Cs1 V1 O3 Cs2 -172.53(18) . . . 1_565 ?
Cs1 V1 O3 Cs2 49.41(9) 1_565 . . 1_565 ?
O3 V1 O4 Cs1 -79.33(11) . . . 1_565 ?
O1 V1 O4 Cs1 20.36(10) . . . 1_565 ?
O2 V1 O4 Cs1 -176.07(7) . . . 1_565 ?
N1 V1 O4 Cs1 106.82(9) . . . 1_565 ?
Cs2 V1 O4 Cs1 -33.35(9) 1_565 . . 1_565 ?
Cs1 V1 O4 Cs1 -119.56(6) . . . 1_565 ?
O4 V1 N1 C7 -81.7(3) . . . . ?
O3 V1 N1 C7 108.6(3) . . . . ?
O1 V1 N1 C7 22.1(2) . . . . ?
O2 V1 N1 C7 179.5(3) . . . . ?
Cs2 V1 N1 C7 47.8(3) 1_565 . . . ?
Cs1 V1 N1 C7 157.7(2) . . . . ?
Cs1 V1 N1 C7 -30.1(3) 1_565 . . . ?
O4 V1 N1 N2 90.57(19) . . . . ?
O3 V1 N1 N2 -79.1(2) . . . . ?
O1 V1 N1 N2 -165.60(19) . . . . ?
O2 V1 N1 N2 -8.23(17) . . . . ?
Cs2 V1 N1 N2 -139.91(15) 1_565 . . . ?
Cs1 V1 N1 N2 -30.0(2) . . . . ?
Cs1 V1 N1 N2 142.18(15) 1_565 . . . ?
C7 N1 N2 C9 179.4(2) . . . . ?
V1 N1 N2 C9 6.0(3) . . . . ?
V1 O1 C1 C2 -149.9(2) . . . . ?
Cs2 O1 C1 C2 19.9(3) 1_565 . . . ?
Cs1 O1 C1 C2 -59.0(2) 1_565 . . . ?
V1 O1 C1 C6 30.5(4) . . . . ?
Cs2 O1 C1 C6 -159.8(2) 1_565 . . . ?
Cs1 O1 C1 C6 121.4(3) 1_565 . . . ?
V1 O1 C1 Cs1 -90.9(2) . . . 1_565 ?
Cs2 O1 C1 Cs1 78.81(14) 1_565 . . 1_565 ?
O1 C1 C2 C3 179.0(3) . . . . ?
C6 C1 C2 C3 -1.3(4) . . . . ?
Cs1 C1 C2 C3 119.4(3) 1_565 . . . ?
O1 C1 C2 Cs1 59.7(2) . . . 1_565 ?
C6 C1 C2 Cs1 -120.6(2) . . . 1_565 ?
C1 C2 C3 C4 0.7(5) . . . . ?
Cs1 C2 C3 C4 102.8(3) 1_565 . . . ?
C2 C3 C4 C5 0.6(5) . . . . ?
C3 C4 C5 C6 -1.3(5) . . . . ?
C4 C5 C6 C1 0.7(4) . . . . ?
C4 C5 C6 C7 -179.8(3) . . . . ?
O1 C1 C6 C5 -179.7(3) . . . . ?
C2 C1 C6 C5 0.6(4) . . . . ?
Cs1 C1 C6 C5 -87.5(3) 1_565 . . . ?
O1 C1 C6 C7 0.8(4) . . . . ?
C2 C1 C6 C7 -178.9(3) . . . . ?
Cs1 C1 C6 C7 93.0(3) 1_565 . . . ?
N2 N1 C7 C6 -178.2(2) . . . . ?
V1 N1 C7 C6 -6.0(4) . . . . ?
N2 N1 C7 C8 0.1(4) . . . . ?
V1 N1 C7 C8 172.3(2) . . . . ?
C5 C6 C7 N1 169.8(3) . . . . ?
C1 C6 C7 N1 -10.7(4) . . . . ?
C5 C6 C7 C8 -8.5(4) . . . . ?
C1 C6 C7 C8 171.0(3) . . . . ?
N1 N2 C9 O2 1.9(4) . . . . ?
N1 N2 C9 C10 -179.7(2) . . . . ?
V1 O2 C9 N2 -9.7(4) . . . . ?
Cs1 O2 C9 N2 148.3(2) . . . . ?
V1 O2 C9 C10 171.88(19) . . . . ?
Cs1 O2 C9 C10 -30.1(4) . . . . ?
N2 C9 C10 C15 -174.5(3) . . . . ?
O2 C9 C10 C15 4.0(4) . . . . ?
N2 C9 C10 C11 5.5(4) . . . . ?
O2 C9 C10 C11 -176.0(3) . . . . ?
C15 C10 C11 C12 -0.3(4) . . . . ?
C9 C10 C11 C12 179.7(3) . . . . ?
C10 C11 C12 C13 0.6(5) . . . . ?
C11 C12 C13 C14 0.1(5) . . . . ?
C12 C13 C14 C15 -0.9(5) . . . . ?
C13 C14 C15 C10 1.2(5) . . . . ?
C11 C10 C15 C14 -0.5(4) . . . . ?
C9 C10 C15 C14 179.4(3) . . . . ?
O8 V2 N3 C22 -70.4(2) . . . . ?
O7 V2 N3 C22 123.7(3) . . . . ?
O5 V2 N3 C22 35.5(2) . . . . ?
O6 V2 N3 C22 -176.2(2) . . . . ?
Cs1 V2 N3 C22 72.2(2) . . . . ?
Cs2 V2 N3 C22 -23.3(2) 1_565 . . . ?
Cs2 V2 N3 C22 155.8(2) . . . . ?
O8 V2 N3 N4 98.66(18) . . . . ?
O7 V2 N3 N4 -67.2(3) . . . . ?
O5 V2 N3 N4 -155.40(19) . . . . ?
O6 V2 N3 N4 -7.13(17) . . . . ?
Cs1 V2 N3 N4 -118.71(16) . . . . ?
Cs2 V2 N3 N4 145.79(15) 1_565 . . . ?
Cs2 V2 N3 N4 -35.1(2) . . . . ?
C22 N3 N4 C24 175.3(2) . . . . ?
V2 N3 N4 C24 5.1(3) . . . . ?
O8 V2 O5 C16 50.4(2) . . . . ?
O7 V2 O5 C16 161.1(2) . . . . ?
O6 V2 O5 C16 -98.1(2) . . . . ?
N3 V2 O5 C16 -46.4(2) . . . . ?
Cs1 V2 O5 C16 171.9(3) . . . . ?
Cs2 V2 O5 C16 77.3(2) 1_565 . . . ?
Cs2 V2 O5 C16 -175.78(19) . . . . ?
O8 V2 O5 Cs1 -121.55(8) . . . . ?
O7 V2 O5 Cs1 -10.89(9) . . . . ?
O6 V2 O5 Cs1 89.93(12) . . . . ?
N3 V2 O5 Cs1 141.69(8) . . . . ?
Cs2 V2 O5 Cs1 -94.68(5) 1_565 . . . ?
Cs2 V2 O5 Cs1 12.28(8) . . . . ?
O8 V2 O6 C24 -86.3(2) . . . . ?
O7 V2 O6 C24 164.6(2) . . . . ?
O5 V2 O6 C24 62.1(2) . . . . ?
N3 V2 O6 C24 7.98(19) . . . . ?
Cs1 V2 O6 C24 127.06(17) . . . . ?
Cs2 V2 O6 C24 -108.55(19) 1_565 . . . ?
Cs2 V2 O6 C24 163.0(2) . . . . ?
O8 V2 O6 Cs2 110.69(8) . . . . ?
O7 V2 O6 Cs2 1.56(8) . . . . ?
O5 V2 O6 Cs2 -100.91(11) . . . . ?
N3 V2 O6 Cs2 -155.06(8) . . . . ?
Cs1 V2 O6 Cs2 -35.98(6) . . . . ?
Cs2 V2 O6 Cs2 88.42(12) 1_565 . . . ?
O8 V2 O7 Cs2 -111.69(14) . . . . ?
O5 V2 O7 Cs2 138.24(13) . . . . ?
O6 V2 O7 Cs2 -2.63(14) . . . . ?
N3 V2 O7 Cs2 53.6(3) . . . . ?
Cs1 V2 O7 Cs2 125.47(17) . . . . ?
Cs2 V2 O7 Cs2 -155.56(12) 1_565 . . . ?
O8 V2 O7 Cs1 122.84(10) . . . . ?
O5 V2 O7 Cs1 12.77(10) . . . . ?
O6 V2 O7 Cs1 -128.10(9) . . . . ?
N3 V2 O7 Cs1 -71.8(2) . . . . ?
Cs2 V2 O7 Cs1 78.97(7) 1_565 . . . ?
Cs2 V2 O7 Cs1 -125.47(17) . . . . ?
O7 V2 O8 Cs2 -68.74(11) . . . 1_565 ?
O5 V2 O8 Cs2 34.02(10) . . . 1_565 ?
O6 V2 O8 Cs2 -166.57(7) . . . 1_565 ?
N3 V2 O8 Cs2 118.01(8) . . . 1_565 ?
Cs1 V2 O8 Cs2 -23.46(12) . . . 1_565 ?
Cs2 V2 O8 Cs2 -101.17(7) . . . 1_565 ?
O7 V2 O8 Cs2 28.3(3) . . . 3_556 ?
O5 V2 O8 Cs2 131.1(2) . . . 3_556 ?
O6 V2 O8 Cs2 -69.5(2) . . . 3_556 ?
N3 V2 O8 Cs2 -144.9(2) . . . 3_556 ?
Cs1 V2 O8 Cs2 73.6(2) . . . 3_556 ?
Cs2 V2 O8 Cs2 97.1(2) 1_565 . . 3_556 ?
Cs2 V2 O8 Cs2 -4.1(3) . . . 3_556 ?
V2 O5 C16 C17 -144.1(2) . . . . ?
Cs1 O5 C16 C17 24.9(4) . . . . ?
V2 O5 C16 C21 37.4(4) . . . . ?
Cs1 O5 C16 C21 -153.7(2) . . . . ?
V2 O5 C16 Cs2 -79.23(17) . . . 1_565 ?
Cs1 O5 C16 Cs2 89.70(18) . . . 1_565 ?
O5 C16 C17 C18 179.1(3) . . . . ?
C21 C16 C17 C18 -2.4(4) . . . . ?
Cs2 C16 C17 C18 112.4(3) 1_565 . . . ?
O5 C16 C17 Cs2 66.7(2) . . . 1_565 ?
C21 C16 C17 Cs2 -114.7(2) . . . 1_565 ?
C16 C17 C18 C19 -0.5(5) . . . . ?
Cs2 C17 C18 C19 96.4(3) 1_565 . . . ?
C17 C18 C19 C20 2.5(5) . . . . ?
C18 C19 C20 C21 -1.7(5) . . . . ?
C19 C20 C21 C16 -1.1(4) . . . . ?
C19 C20 C21 C22 175.8(3) . . . . ?
O5 C16 C21 C20 -178.4(3) . . . . ?
C17 C16 C21 C20 3.1(4) . . . . ?
Cs2 C16 C21 C20 -84.7(3) 1_565 . . . ?
O5 C16 C21 C22 4.7(4) . . . . ?
C17 C16 C21 C22 -173.8(3) . . . . ?
Cs2 C16 C21 C22 98.4(3) 1_565 . . . ?
N4 N3 C22 C21 177.5(2) . . . . ?
V2 N3 C22 C21 -13.6(4) . . . . ?
N4 N3 C22 C23 -3.6(4) . . . . ?
V2 N3 C22 C23 165.3(2) . . . . ?
C20 C21 C22 N3 169.4(3) . . . . ?
C16 C21 C22 N3 -13.8(4) . . . . ?
C20 C21 C22 C23 -9.4(4) . . . . ?
C16 C21 C22 C23 167.3(3) . . . . ?
N3 N4 C24 O6 1.7(4) . . . . ?
N3 N4 C24 C25 -179.3(2) . . . . ?
V2 O6 C24 N4 -8.6(3) . . . . ?
Cs2 O6 C24 N4 140.4(2) . . . . ?
V2 O6 C24 C25 172.40(18) . . . . ?
Cs2 O6 C24 C25 -38.6(4) . . . . ?
N4 C24 C25 C30 -165.2(3) . . . . ?
O6 C24 C25 C30 13.8(4) . . . . ?
N4 C24 C25 C26 16.7(4) . . . . ?
O6 C24 C25 C26 -164.3(3) . . . . ?
C30 C25 C26 C27 -1.4(4) . . . . ?
C24 C25 C26 C27 176.7(3) . . . . ?
C25 C26 C27 C28 -0.1(4) . . . . ?
C26 C27 C28 C29 1.5(5) . . . . ?
C27 C28 C29 C30 -1.4(4) . . . . ?
C28 C29 C30 C25 -0.1(4) . . . . ?
C26 C25 C30 C29 1.5(4) . . . . ?
C24 C25 C30 C29 -176.7(3) . . . . ?
V1 O3 Cs1 O7 -157.36(13) . . . . ?
Cs2 O3 Cs1 O7 14.47(8) 1_565 . . . ?
V1 O3 Cs1 O1W 48.76(12) . . . . ?
Cs2 O3 Cs1 O1W -139.41(10) 1_565 . . . ?
V1 O3 Cs1 O1W 53.22(17) . . . 3_656 ?
Cs2 O3 Cs1 O1W -134.95(9) 1_565 . . 3_656 ?
V1 O3 Cs1 O5 153.91(14) . . . . ?
Cs2 O3 Cs1 O5 -34.27(7) 1_565 . . . ?
V1 O3 Cs1 O4 -34.60(17) . . . 1_545 ?
Cs2 O3 Cs1 O4 137.23(8) 1_565 . . 1_545 ?
V1 O3 Cs1 O2 -10.96(9) . . . . ?
Cs2 O3 Cs1 O2 160.87(12) 1_565 . . . ?
V1 O3 Cs1 C2 -87.67(13) . . . 1_545 ?
Cs2 O3 Cs1 C2 84.16(9) 1_565 . . 1_545 ?
V1 O3 Cs1 O1 -81.93(12) . . . 1_545 ?
Cs2 O3 Cs1 O1 89.90(8) 1_565 . . 1_545 ?
V1 O3 Cs1 C1 -74.71(12) . . . 1_545 ?
Cs2 O3 Cs1 C1 97.11(9) 1_565 . . 1_545 ?
V1 O3 Cs1 V2 -179.34(12) . . . . ?
Cs2 O3 Cs1 V2 -7.52(7) 1_565 . . . ?
Cs2 O3 Cs1 V1 171.83(19) 1_565 . . . ?
V2 O7 Cs1 O3 -76.39(10) . . . . ?
Cs2 O7 Cs1 O3 141.07(6) . . . . ?
V2 O7 Cs1 O1W -26.41(16) . . . . ?
Cs2 O7 Cs1 O1W -168.96(7) . . . . ?
V2 O7 Cs1 O1W 83.36(11) . . . 3_656 ?
Cs2 O7 Cs1 O1W -59.19(8) . . . 3_656 ?
V2 O7 Cs1 O5 -9.59(8) . . . . ?
Cs2 O7 Cs1 O5 -152.14(9) . . . . ?
V2 O7 Cs1 O4 140.22(9) . . . 1_545 ?
Cs2 O7 Cs1 O4 -2.33(7) . . . 1_545 ?
V2 O7 Cs1 O2 -106.66(10) . . . . ?
Cs2 O7 Cs1 O2 110.79(6) . . . . ?
V2 O7 Cs1 C2 -148.33(12) . . . 1_545 ?
Cs2 O7 Cs1 C2 69.12(6) . . . 1_545 ?
V2 O7 Cs1 O1 172.29(11) . . . 1_545 ?
Cs2 O7 Cs1 O1 29.74(5) . . . 1_545 ?
V2 O7 Cs1 C1 -166.59(11) . . . 1_545 ?
Cs2 O7 Cs1 C1 50.87(6) . . . 1_545 ?
Cs2 O7 Cs1 V2 -142.55(13) . . . . ?
V2 O7 Cs1 V1 -84.33(10) . . . . ?
Cs2 O7 Cs1 V1 133.12(4) . . . . ?
C16 O5 Cs1 O3 -62.4(2) . . . . ?
V2 O5 Cs1 O3 108.71(9) . . . . ?
C16 O5 Cs1 O7 -163.4(3) . . . . ?
V2 O5 Cs1 O7 7.76(6) . . . . ?
C16 O5 Cs1 O1W 7.3(2) . . . . ?
V2 O5 Cs1 O1W 178.45(8) . . . . ?
C16 O5 Cs1 O1W 80.6(2) . . . 3_656 ?
V2 O5 Cs1 O1W -108.27(8) . . . 3_656 ?
C16 O5 Cs1 O4 128.7(2) . . . 1_545 ?
V2 O5 Cs1 O4 -60.14(14) . . . 1_545 ?
C16 O5 Cs1 O2 -49.7(2) . . . . ?
V2 O5 Cs1 O2 121.40(7) . . . . ?
C16 O5 Cs1 C2 -123.2(2) . . . 1_545 ?
V2 O5 Cs1 C2 47.96(9) . . . 1_545 ?
C16 O5 Cs1 O1 -161.1(2) . . . 1_545 ?
V2 O5 Cs1 O1 10.09(10) . . . 1_545 ?
C16 O5 Cs1 C1 -134.0(2) . . . 1_545 ?
V2 O5 Cs1 C1 37.10(11) . . . 1_545 ?
C16 O5 Cs1 V2 -171.1(3) . . . . ?
C16 O5 Cs1 V1 -53.6(2) . . . . ?
V2 O5 Cs1 V1 117.57(7) . . . . ?
C9 O2 Cs1 O3 -152.6(3) . . . . ?
V1 O2 Cs1 O3 7.84(7) . . . . ?
C9 O2 Cs1 O7 -111.0(3) . . . . ?
V1 O2 Cs1 O7 49.46(9) . . . . ?
C9 O2 Cs1 O1W 109.6(3) . . . . ?
V1 O2 Cs1 O1W -89.98(9) . . . . ?
C9 O2 Cs1 O1W 60.2(3) . . . 3_656 ?
V1 O2 Cs1 O1W -139.38(7) . . . 3_656 ?
C9 O2 Cs1 O5 -168.3(3) . . . . ?
V1 O2 Cs1 O5 -7.87(9) . . . . ?
C9 O2 Cs1 O4 12.5(3) . . . 1_545 ?
V1 O2 Cs1 O4 172.89(7) . . . 1_545 ?
C9 O2 Cs1 C2 -68.9(3) . . . 1_545 ?
V1 O2 Cs1 C2 91.51(8) . . . 1_545 ?
C9 O2 Cs1 O1 -35.6(3) . . . 1_545 ?
V1 O2 Cs1 O1 124.82(7) . . . 1_545 ?
C9 O2 Cs1 C1 -45.1(3) . . . 1_545 ?
V1 O2 Cs1 C1 115.34(9) . . . 1_545 ?
C9 O2 Cs1 V2 -138.2(3) . . . . ?
V1 O2 Cs1 V2 22.28(9) . . . . ?
C9 O2 Cs1 V1 -160.4(3) . . . . ?
O8 V2 Cs1 O3 22.05(10) . . . . ?
O7 V2 Cs1 O3 100.46(11) . . . . ?
O5 V2 Cs1 O3 -63.79(9) . . . . ?
O6 V2 Cs1 O3 162.19(8) . . . . ?
N3 V2 Cs1 O3 -110.76(8) . . . . ?
Cs2 V2 Cs1 O3 4.59(4) 1_565 . . . ?
Cs2 V2 Cs1 O3 128.01(4) . . . . ?
O8 V2 Cs1 O7 -78.41(14) . . . . ?
O5 V2 Cs1 O7 -164.25(13) . . . . ?
O6 V2 Cs1 O7 61.73(12) . . . . ?
N3 V2 Cs1 O7 148.78(13) . . . . ?
Cs2 V2 Cs1 O7 -95.86(10) 1_565 . . . ?
Cs2 V2 Cs1 O7 27.55(10) . . . . ?
O8 V2 Cs1 O1W 83.95(10) . . . . ?
O7 V2 Cs1 O1W 162.35(11) . . . . ?
O5 V2 Cs1 O1W -1.89(9) . . . . ?
O6 V2 Cs1 O1W -135.92(8) . . . . ?
N3 V2 Cs1 O1W -48.86(9) . . . . ?
Cs2 V2 Cs1 O1W 66.49(5) 1_565 . . . ?
Cs2 V2 Cs1 O1W -170.10(5) . . . . ?
O8 V2 Cs1 O1W 171.36(10) . . . 3_656 ?
O7 V2 Cs1 O1W -110.23(11) . . . 3_656 ?
O5 V2 Cs1 O1W 85.52(9) . . . 3_656 ?
O6 V2 Cs1 O1W -48.50(8) . . . 3_656 ?
N3 V2 Cs1 O1W 38.55(9) . . . 3_656 ?
Cs2 V2 Cs1 O1W 153.90(5) 1_565 . . 3_656 ?
Cs2 V2 Cs1 O1W -82.68(5) . . . 3_656 ?
O8 V2 Cs1 O5 85.84(12) . . . . ?
O7 V2 Cs1 O5 164.25(13) . . . . ?
O6 V2 Cs1 O5 -134.02(10) . . . . ?
N3 V2 Cs1 O5 -46.97(11) . . . . ?
Cs2 V2 Cs1 O5 68.38(8) 1_565 . . . ?
Cs2 V2 Cs1 O5 -168.20(8) . . . . ?
O8 V2 Cs1 O4 -128.54(10) . . . 1_545 ?
O7 V2 Cs1 O4 -50.13(11) . . . 1_545 ?
O5 V2 Cs1 O4 145.62(9) . . . 1_545 ?
O6 V2 Cs1 O4 11.60(8) . . . 1_545 ?
N3 V2 Cs1 O4 98.65(9) . . . 1_545 ?
Cs2 V2 Cs1 O4 -146.00(5) 1_565 . . 1_545 ?
Cs2 V2 Cs1 O4 -22.58(5) . . . 1_545 ?
O8 V2 Cs1 O2 11.02(10) . . . . ?
O7 V2 Cs1 O2 89.42(11) . . . . ?
O5 V2 Cs1 O2 -74.82(9) . . . . ?
O6 V2 Cs1 O2 151.15(8) . . . . ?
N3 V2 Cs1 O2 -121.79(8) . . . . ?
Cs2 V2 Cs1 O2 -6.44(5) 1_565 . . . ?
Cs2 V2 Cs1 O2 116.97(5) . . . . ?
O8 V2 Cs1 C2 -49.05(10) . . . 1_545 ?
O7 V2 Cs1 C2 29.36(11) . . . 1_545 ?
O5 V2 Cs1 C2 -134.89(9) . . . 1_545 ?
O6 V2 Cs1 C2 91.09(8) . . . 1_545 ?
N3 V2 Cs1 C2 178.14(9) . . . 1_545 ?
Cs2 V2 Cs1 C2 -66.51(5) 1_565 . . 1_545 ?
Cs2 V2 Cs1 C2 56.91(5) . . . 1_545 ?
O8 V2 Cs1 O1 -86.08(10) . . . 1_545 ?
O7 V2 Cs1 O1 -7.67(11) . . . 1_545 ?
O5 V2 Cs1 O1 -171.92(8) . . . 1_545 ?
O6 V2 Cs1 O1 54.06(7) . . . 1_545 ?
N3 V2 Cs1 O1 141.11(8) . . . 1_545 ?
Cs2 V2 Cs1 O1 -103.54(3) 1_565 . . 1_545 ?
Cs2 V2 Cs1 O1 19.88(3) . . . 1_545 ?
O8 V2 Cs1 C1 -64.67(10) . . . 1_545 ?
O7 V2 Cs1 C1 13.73(11) . . . 1_545 ?
O5 V2 Cs1 C1 -150.51(9) . . . 1_545 ?
O6 V2 Cs1 C1 75.46(8) . . . 1_545 ?
N3 V2 Cs1 C1 162.52(8) . . . 1_545 ?
Cs2 V2 Cs1 C1 -82.13(5) 1_565 . . 1_545 ?
Cs2 V2 Cs1 C1 41.28(4) . . . 1_545 ?
O8 V2 Cs1 V1 21.82(9) . . . . ?
O7 V2 Cs1 V1 100.23(10) . . . . ?
O5 V2 Cs1 V1 -64.02(8) . . . . ?
O6 V2 Cs1 V1 161.96(6) . . . . ?
N3 V2 Cs1 V1 -110.99(7) . . . . ?
Cs2 V2 Cs1 V1 4.362(10) 1_565 . . . ?
Cs2 V2 Cs1 V1 127.776(12) . . . . ?
O4 V1 Cs1 O3 102.45(15) . . . . ?
O1 V1 Cs1 O3 -22.77(15) . . . . ?
O2 V1 Cs1 O3 -162.86(15) . . . . ?
N1 V1 Cs1 O3 -136.96(15) . . . . ?
Cs2 V1 Cs1 O3 -5.17(12) 1_565 . . . ?
Cs1 V1 Cs1 O3 51.58(12) 1_565 . . . ?
O4 V1 Cs1 O7 125.60(9) . . . . ?
O3 V1 Cs1 O7 23.15(13) . . . . ?
O1 V1 Cs1 O7 0.38(9) . . . . ?
O2 V1 Cs1 O7 -139.71(8) . . . . ?
N1 V1 Cs1 O7 -113.81(9) . . . . ?
Cs2 V1 Cs1 O7 17.98(4) 1_565 . . . ?
Cs1 V1 Cs1 O7 74.73(4) 1_565 . . . ?
O4 V1 Cs1 O1W -22.18(9) . . . . ?
O3 V1 Cs1 O1W -124.63(13) . . . . ?
O1 V1 Cs1 O1W -147.40(10) . . . . ?
O2 V1 Cs1 O1W 72.51(9) . . . . ?
N1 V1 Cs1 O1W 98.40(9) . . . . ?
Cs2 V1 Cs1 O1W -129.81(5) 1_565 . . . ?
Cs1 V1 Cs1 O1W -73.05(5) 1_565 . . . ?
O4 V1 Cs1 O1W -40.89(9) . . . 3_656 ?
O3 V1 Cs1 O1W -143.34(13) . . . 3_656 ?
O1 V1 Cs1 O1W -166.10(10) . . . 3_656 ?
O2 V1 Cs1 O1W 53.81(9) . . . 3_656 ?
N1 V1 Cs1 O1W 79.70(10) . . . 3_656 ?
Cs2 V1 Cs1 O1W -148.51(5) 1_565 . . 3_656 ?
Cs1 V1 Cs1 O1W -91.75(6) 1_565 . . 3_656 ?
O4 V1 Cs1 O5 78.24(8) . . . . ?
O3 V1 Cs1 O5 -24.21(13) . . . . ?
O1 V1 Cs1 O5 -46.98(9) . . . . ?
O2 V1 Cs1 O5 172.93(8) . . . . ?
N1 V1 Cs1 O5 -161.18(9) . . . . ?
Cs2 V1 Cs1 O5 -29.39(4) 1_565 . . . ?
Cs1 V1 Cs1 O5 27.37(4) 1_565 . . . ?
O4 V1 Cs1 O4 -103.09(10) . . . 1_545 ?
O3 V1 Cs1 O4 154.46(13) . . . 1_545 ?
O1 V1 Cs1 O4 131.69(9) . . . 1_545 ?
O2 V1 Cs1 O4 -8.40(9) . . . 1_545 ?
N1 V1 Cs1 O4 17.50(9) . . . 1_545 ?
Cs2 V1 Cs1 O4 149.29(4) 1_565 . . 1_545 ?
Cs1 V1 Cs1 O4 -153.96(4) 1_565 . . 1_545 ?
O4 V1 Cs1 O2 -94.69(11) . . . . ?
O3 V1 Cs1 O2 162.86(15) . . . . ?
O1 V1 Cs1 O2 140.09(11) . . . . ?
N1 V1 Cs1 O2 25.89(11) . . . . ?
Cs2 V1 Cs1 O2 157.69(8) 1_565 . . . ?
Cs1 V1 Cs1 O2 -145.56(8) 1_565 . . . ?
O4 V1 Cs1 C2 -172.22(9) . . . 1_545 ?
O3 V1 Cs1 C2 85.33(13) . . . 1_545 ?
O1 V1 Cs1 C2 62.56(10) . . . 1_545 ?
O2 V1 Cs1 C2 -77.53(9) . . . 1_545 ?
N1 V1 Cs1 C2 -51.63(9) . . . 1_545 ?
Cs2 V1 Cs1 C2 80.16(5) 1_565 . . 1_545 ?
Cs1 V1 Cs1 C2 136.91(5) 1_565 . . 1_545 ?
O4 V1 Cs1 O1 -153.09(8) . . . 1_545 ?
O3 V1 Cs1 O1 104.46(13) . . . 1_545 ?
O1 V1 Cs1 O1 81.70(9) . . . 1_545 ?
O2 V1 Cs1 O1 -58.40(8) . . . 1_545 ?
N1 V1 Cs1 O1 -32.50(8) . . . 1_545 ?
Cs2 V1 Cs1 O1 99.29(3) 1_565 . . 1_545 ?
Cs1 V1 Cs1 O1 156.05(3) 1_565 . . 1_545 ?
O4 V1 Cs1 C1 -153.37(9) . . . 1_545 ?
O3 V1 Cs1 C1 104.18(13) . . . 1_545 ?
O1 V1 Cs1 C1 81.41(9) . . . 1_545 ?
O2 V1 Cs1 C1 -58.68(9) . . . 1_545 ?
N1 V1 Cs1 C1 -32.79(9) . . . 1_545 ?
Cs2 V1 Cs1 C1 99.00(4) 1_565 . . 1_545 ?
Cs1 V1 Cs1 C1 155.76(5) 1_565 . . 1_545 ?
O4 V1 Cs1 V2 103.10(8) . . . . ?
O3 V1 Cs1 V2 0.65(12) . . . . ?
O1 V1 Cs1 V2 -22.11(8) . . . . ?
O2 V1 Cs1 V2 -162.20(7) . . . . ?
N1 V1 Cs1 V2 -136.31(8) . . . . ?
Cs2 V1 Cs1 V2 -4.517(10) 1_565 . . . ?
Cs1 V1 Cs1 V2 52.239(18) 1_565 . . . ?
V2 O7 Cs2 O2W 81.2(3) . . . . ?
Cs1 O7 Cs2 O2W -147.31(18) . . . . ?
V2 O7 Cs2 O3 -122.96(13) . . . 1_545 ?
Cs1 O7 Cs2 O3 8.50(7) . . . 1_545 ?
V2 O7 Cs2 O1 -164.50(14) . . . 1_545 ?
Cs1 O7 Cs2 O1 -33.03(5) . . . 1_545 ?
V2 O7 Cs2 O2W 50.36(13) . . . 3_546 ?
Cs1 O7 Cs2 O2W -178.18(7) . . . 3_546 ?
V2 O7 Cs2 O8 -5.99(17) . . . 1_545 ?
Cs1 O7 Cs2 O8 125.48(6) . . . 1_545 ?
V2 O7 Cs2 O8 100.28(14) . . . 3_556 ?
Cs1 O7 Cs2 O8 -128.26(5) . . . 3_556 ?
V2 O7 Cs2 O6 1.99(10) . . . . ?
Cs1 O7 Cs2 O6 133.46(9) . . . . ?
V2 O7 Cs2 C17 -71.37(14) . . . 1_545 ?
Cs1 O7 Cs2 C17 60.10(6) . . . 1_545 ?
V2 O7 Cs2 C16 -54.88(14) . . . 1_545 ?
Cs1 O7 Cs2 C16 76.58(6) . . . 1_545 ?
V2 O7 Cs2 V1 -140.48(13) . . . 1_545 ?
Cs1 O7 Cs2 V1 -9.01(5) . . . 1_545 ?
V2 O7 Cs2 Cs2 56.63(15) . . . 3_546 ?
Cs1 O7 Cs2 Cs2 -171.90(3) . . . 3_546 ?
C24 O6 Cs2 O2W 46.3(3) . . . . ?
V2 O6 Cs2 O2W -160.59(7) . . . . ?
C24 O6 Cs2 O7 -154.3(3) . . . . ?
V2 O6 Cs2 O7 -1.24(7) . . . . ?
C24 O6 Cs2 O3 -72.5(3) . . . 1_545 ?
V2 O6 Cs2 O3 80.64(8) . . . 1_545 ?
C24 O6 Cs2 O1 -137.3(3) . . . 1_545 ?
V2 O6 Cs2 O1 15.82(9) . . . 1_545 ?
C24 O6 Cs2 O2W 100.3(3) . . . 3_546 ?
V2 O6 Cs2 O2W -106.57(9) . . . 3_546 ?
C24 O6 Cs2 O8 19.1(3) . . . 1_545 ?
V2 O6 Cs2 O8 172.17(7) . . . 1_545 ?
C24 O6 Cs2 O8 124.5(3) . . . 3_556 ?
V2 O6 Cs2 O8 -82.42(7) . . . 3_556 ?
C24 O6 Cs2 C17 -59.9(3) . . . 1_545 ?
V2 O6 Cs2 C17 93.21(8) . . . 1_545 ?
C24 O6 Cs2 C16 -37.4(3) . . . 1_545 ?
V2 O6 Cs2 C16 115.66(8) . . . 1_545 ?
C24 O6 Cs2 V1 -101.4(3) . . . 1_545 ?
V2 O6 Cs2 V1 51.68(8) . . . 1_545 ?
C24 O6 Cs2 Cs2 74.2(3) . . . 3_546 ?
V2 O6 Cs2 Cs2 -132.74(6) . . . 3_546 ?
O3 Cs1 O1W Cs1 177.36(8) . . . 3_656 ?
O7 Cs1 O1W Cs1 125.06(9) . . . 3_656 ?
O1W Cs1 O1W Cs1 0.0 3_656 . . 3_656 ?
O5 Cs1 O1W Cs1 112.20(7) . . . 3_656 ?
O4 Cs1 O1W Cs1 -42.74(7) 1_545 . . 3_656 ?
O2 Cs1 O1W Cs1 -131.65(9) . . . 3_656 ?
C2 Cs1 O1W Cs1 -129.97(7) 1_545 . . 3_656 ?
O1 Cs1 O1W Cs1 -80.37(8) 1_545 . . 3_656 ?
C1 Cs1 O1W Cs1 -103.38(7) 1_545 . . 3_656 ?
V2 Cs1 O1W Cs1 113.10(5) . . . 3_656 ?
V1 Cs1 O1W Cs1 -165.25(8) . . . 3_656 ?
O7 Cs2 O2W Cs2 -28.8(2) . . . 3_546 ?
O3 Cs2 O2W Cs2 173.60(5) 1_545 . . 3_546 ?
O1 Cs2 O2W Cs2 -141.02(5) 1_545 . . 3_546 ?
O2W Cs2 O2W Cs2 0.0 3_546 . . 3_546 ?
O8 Cs2 O2W Cs2 69.35(6) 1_545 . . 3_546 ?
O8 Cs2 O2W Cs2 -48.16(4) 3_556 . . 3_546 ?
O6 Cs2 O2W Cs2 36.08(8) . . . 3_546 ?
C17 Cs2 O2W Cs2 121.38(6) 1_545 . . 3_546 ?
C16 Cs2 O2W Cs2 106.71(5) 1_545 . . 3_546 ?
V1 Cs2 O2W Cs2 -167.69(3) 1_545 . . 3_546 ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.108
_database_code_depnum_ccdc_archive 'CCDC 991926'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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#
data_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H11 N3 O4 V, 2(H2 O), K '
_chemical_formula_sum            'C14 H15 K N3 O6 V'
_chemical_formula_weight         411.33

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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   ' P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   11.6880(4)
_cell_length_b                   8.2858(2)
_cell_length_c                   34.9484(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3384.56(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8003
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      24.11

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1680
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7686
_exptl_absorpt_correction_T_max  0.9711

_exptl_special_details           
;
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            63472
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         30.55
_reflns_number_total             5179
_reflns_number_gt                3225
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'

_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 > 2σ(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)+(0.0401P)²+1.9983P] 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         5179
_refine_ls_number_parameters     239
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1090
_refine_ls_wR_factor_gt          0.0924
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001

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
V V 0.48516(3) 0.20419(5) 0.123035(11) 0.02644(11) Uani 1 1 d . . .
O1 O 0.56527(14) 0.0731(2) 0.08452(5) 0.0348(4) Uani 1 1 d . . .
O2 O 0.47696(14) 0.3955(2) 0.15249(5) 0.0377(4) Uani 1 1 d . . .
O3 O 0.42947(15) 0.0673(2) 0.15027(5) 0.0418(4) Uani 1 1 d . . .
O4 O 0.38958(14) 0.2621(2) 0.09175(4) 0.0352(4) Uani 1 1 d . . .
N1 N 0.8444(2) -0.1797(3) -0.00590(6) 0.0483(6) Uani 1 1 d . . .
N2 N 0.73864(16) 0.1497(2) 0.10956(5) 0.0293(4) Uani 1 1 d . . .
N3 N 0.66497(16) 0.2287(2) 0.13541(5) 0.0266(4) Uani 1 1 d . . .
C1 C 0.9027(2) -0.1188(3) 0.02332(8) 0.0458(7) Uani 1 1 d . . .
H1 H 0.9816 -0.1332 0.0236 0.055 Uiso 1 1 calc R . .
C2 C 0.8537(2) -0.0355(3) 0.05344(7) 0.0363(6) Uani 1 1 d . . .
H2 H 0.8988 0.0069 0.0729 0.044 Uiso 1 1 calc R . .
C3 C 0.7355(2) -0.0165(3) 0.05391(6) 0.0299(5) Uani 1 1 d . . .
C4 C 0.6735(2) -0.0814(3) 0.02387(7) 0.0391(6) Uani 1 1 d . . .
H4 H 0.5942 -0.0724 0.0233 0.047 Uiso 1 1 calc R . .
C5 C 0.7309(3) -0.1598(3) -0.00530(7) 0.0483(7) Uani 1 1 d . . .
H5 H 0.6883 -0.2008 -0.0256 0.058 Uiso 1 1 calc R . .
C6 C 0.67704(19) 0.0729(3) 0.08490(6) 0.0275(5) Uani 1 1 d . . .
C7 C 0.71566(19) 0.3072(3) 0.16305(6) 0.0268(5) Uani 1 1 d . . .
C7' C 0.8432(2) 0.3128(3) 0.16622(7) 0.0361(6) Uani 1 1 d . . .
H71 H 0.8767 0.2812 0.1423 0.054 Uiso 1 1 calc R . .
H72 H 0.8679 0.2403 0.1860 0.054 Uiso 1 1 calc R . .
H73 H 0.8669 0.4207 0.1724 0.054 Uiso 1 1 calc R . .
C8 C 0.6460(2) 0.3906(3) 0.19168(6) 0.0291(5) Uani 1 1 d . . .
C9 C 0.6948(2) 0.4396(3) 0.22655(7) 0.0397(6) Uani 1 1 d . . .
H9 H 0.7713 0.4159 0.2313 0.048 Uiso 1 1 calc R . .
C10 C 0.6337(3) 0.5208(3) 0.25368(7) 0.0498(7) Uani 1 1 d . . .
H10 H 0.6686 0.5514 0.2765 0.060 Uiso 1 1 calc R . .
C11 C 0.5198(3) 0.5574(3) 0.24723(8) 0.0479(7) Uani 1 1 d . . .
H11 H 0.4778 0.6126 0.2657 0.058 Uiso 1 1 calc R . .
C12 C 0.4696(2) 0.5121(3) 0.21366(7) 0.0403(6) Uani 1 1 d . . .
H12 H 0.3930 0.5370 0.2095 0.048 Uiso 1 1 calc R . .
C13 C 0.5303(2) 0.4290(3) 0.18534(7) 0.0305(5) Uani 1 1 d . . .
K K 0.20850(5) 0.04886(7) 0.110415(19) 0.04901(18) Uani 1 1 d . . .
O1W O 0.1106(2) 0.3228(3) 0.07737(6) 0.0735(7) Uani 1 1 d D . .
H1W1 H 0.051(2) 0.378(5) 0.0818(9) 0.110 Uiso 1 1 d D . .
H1W2 H 0.112(3) 0.293(5) 0.0545(4) 0.110 Uiso 1 1 d D . .
O2W O 0.2029(3) 0.2865(4) 0.16658(8) 0.0885(8) Uani 1 1 d D . .
H2W1 H 0.216(3) 0.304(6) 0.1903(5) 0.133 Uiso 1 1 d D . .
H2W2 H 0.1297(11) 0.291(6) 0.1635(11) 0.133 Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
V O3 1.6174(17) . ?
V O4 1.6350(16) . ?
V O2 1.8926(16) . ?
V O1 1.9668(16) . ?
V N3 2.1552(19) . ?
V K 3.5082(7) . ?
V K 3.6707(7) 8_665 ?
O1 C6 1.306(3) . ?
O2 C13 1.336(3) . ?
O2 K 2.9112(17) 8_665 ?
O3 K 2.9383(19) . ?
O4 K 2.7178(17) 8_665 ?
O4 K 2.8330(18) . ?
N1 C1 1.327(4) . ?
N1 C5 1.337(4) . ?
N2 C6 1.291(3) . ?
N2 N3 1.409(2) . ?
N3 C7 1.306(3) . ?
C1 C2 1.383(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.391(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.384(3) . ?
C3 C6 1.479(3) . ?
C4 C5 1.382(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C7 C8 1.464(3) . ?
C7 C7' 1.495(3) . ?
C7' H71 0.9600 . ?
C7' H72 0.9600 . ?
C7' H73 0.9600 . ?
C8 C9 1.405(3) . ?
C8 C13 1.407(3) . ?
C9 C10 1.364(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.364(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.399(3) . ?
C12 H12 0.9300 . ?
K O4 2.7178(17) 8_655 ?
K O2W 2.781(3) . ?
K O1W 2.792(2) . ?
K O2 2.9112(17) 8_655 ?
K O1W 3.052(3) 8_655 ?
K O2W 3.106(3) 8_655 ?
K V 3.6707(7) 8_655 ?
O1W K 3.052(3) 8_665 ?
O1W H1W1 0.843(10) . ?
O1W H1W2 0.836(10) . ?
O2W K 3.106(3) 8_665 ?
O2W H2W1 0.857(10) . ?
O2W H2W2 0.863(10) . ?

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
O3 V O4 108.92(9) . . ?
O3 V O2 104.30(9) . . ?
O4 V O2 94.79(8) . . ?
O3 V O1 101.95(8) . . ?
O4 V O1 91.69(8) . . ?
O2 V O1 149.19(8) . . ?
O3 V N3 109.90(8) . . ?
O4 V N3 140.61(8) . . ?
O2 V N3 82.03(7) . . ?
O1 V N3 74.05(7) . . ?
O3 V K 56.34(7) . . ?
O4 V K 52.68(6) . . ?
O2 V K 109.21(5) . . ?
O1 V K 98.64(5) . . ?
N3 V K 163.45(5) . . ?
O3 V K 111.60(7) . 8_665 ?
O4 V K 43.13(6) . 8_665 ?
O2 V K 51.86(5) . 8_665 ?
O1 V K 129.86(5) . 8_665 ?
N3 V K 123.51(5) . 8_665 ?
K V K 72.659(9) . 8_665 ?
C6 O1 V 118.02(14) . . ?
C13 O2 V 128.17(15) . . ?
C13 O2 K 133.71(14) . 8_665 ?
V O2 K 97.39(6) . 8_665 ?
V O3 K 96.39(8) . . ?
V O4 K 112.59(8) . 8_665 ?
V O4 K 100.00(8) . . ?
K O4 K 100.07(5) 8_665 . ?
C1 N1 C5 116.8(2) . . ?
C6 N2 N3 108.43(19) . . ?
C7 N3 N2 115.34(19) . . ?
C7 N3 V 129.61(15) . . ?
N2 N3 V 115.05(13) . . ?
N1 C1 C2 124.3(3) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C1 C2 C3 118.5(2) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 117.9(2) . . ?
C4 C3 C6 120.5(2) . . ?
C2 C3 C6 121.6(2) . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 123.4(3) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
N2 C6 O1 124.3(2) . . ?
N2 C6 C3 118.6(2) . . ?
O1 C6 C3 117.1(2) . . ?
N3 C7 C8 119.2(2) . . ?
N3 C7 C7' 121.5(2) . . ?
C8 C7 C7' 119.3(2) . . ?
C7 C7' H71 109.5 . . ?
C7 C7' H72 109.5 . . ?
H71 C7' H72 109.5 . . ?
C7 C7' H73 109.5 . . ?
H71 C7' H73 109.5 . . ?
H72 C7' H73 109.5 . . ?
C9 C8 C13 117.5(2) . . ?
C9 C8 C7 120.2(2) . . ?
C13 C8 C7 122.2(2) . . ?
C10 C9 C8 122.2(3) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C9 C10 C11 119.9(2) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 119.6(2) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 121.7(3) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
O2 C13 C12 118.3(2) . . ?
O2 C13 C8 122.5(2) . . ?
C12 C13 C8 119.2(2) . . ?
O4 K O2W 141.13(7) 8_655 . ?
O4 K O1W 116.02(7) 8_655 . ?
O2W K O1W 72.95(8) . . ?
O4 K O4 143.62(6) 8_655 . ?
O2W K O4 74.84(7) . . ?
O1W K O4 72.78(7) . . ?
O4 K O2 54.94(5) 8_655 8_655 ?
O2W K O2 86.28(7) . 8_655 ?
O1W K O2 104.99(7) . 8_655 ?
O4 K O2 160.86(5) . 8_655 ?
O4 K O3 122.00(6) 8_655 . ?
O2W K O3 69.46(7) . . ?
O1W K O3 120.93(7) . . ?
O4 K O3 54.55(5) . . ?
O2 K O3 115.96(5) 8_655 . ?
O4 K O1W 70.41(5) 8_655 8_655 ?
O2W K O1W 135.88(8) . 8_655 ?
O1W K O1W 128.79(9) . 8_655 ?
O4 K O1W 77.18(5) . 8_655 ?
O2 K O1W 116.04(6) 8_655 8_655 ?
O3 K O1W 66.56(5) . 8_655 ?
O4 K O2W 71.36(6) 8_655 8_655 ?
O2W K O2W 93.28(9) . 8_655 ?
O1W K O2W 165.20(8) . 8_655 ?
O4 K O2W 109.44(7) . 8_655 ?
O2 K O2W 67.89(7) 8_655 8_655 ?
O3 K O2W 56.22(6) . 8_655 ?
O1W K O2W 65.08(8) 8_655 8_655 ?
O4 K V 137.71(4) 8_655 . ?
O2W K V 70.92(6) . . ?
O1W K V 97.56(6) . . ?
O4 K V 27.32(3) . . ?
O2 K V 141.53(4) 8_655 . ?
O3 K V 27.27(3) . . ?
O1W K V 68.54(4) 8_655 . ?
O2W K V 82.54(6) 8_655 . ?
O4 K V 24.28(3) 8_655 8_655 ?
O2W K V 116.85(7) . 8_655 ?
O1W K V 115.43(6) . 8_655 ?
O4 K V 166.78(4) . 8_655 ?
O2 K V 30.75(3) 8_655 8_655 ?
O3 K V 121.70(4) . 8_655 ?
O1W K V 89.72(4) 8_655 8_655 ?
O2W K V 65.49(5) 8_655 8_655 ?
V K V 147.00(2) . 8_655 ?
O4 K K 161.35(4) 8_655 8_665 ?
O2W K K 46.84(6) . 8_665 ?
O1W K K 45.72(6) . 8_665 ?
O4 K K 38.97(4) . 8_665 ?
O2 K K 126.49(4) 8_655 8_665 ?
O3 K K 75.46(4) . 8_665 ?
O1W K K 116.09(5) 8_655 8_665 ?
O2W K K 127.25(5) 8_655 8_665 ?
V K K 55.433(16) . 8_665 ?
V K K 153.91(2) 8_655 8_665 ?
O4 K K 40.96(4) 8_655 8_655 ?
O2W K K 134.01(7) . 8_655 ?
O1W K K 152.25(5) . 8_655 ?
O4 K K 115.90(4) . 8_655 ?
O2 K K 75.22(4) 8_655 8_655 ?
O3 K K 81.38(4) . 8_655 ?
O1W K K 40.92(5) 8_655 8_655 ?
O2W K K 40.77(5) 8_655 8_655 ?
V K K 98.46(2) . 8_655 ?
V K K 51.908(12) 8_655 8_655 ?
K K K 153.64(3) 8_665 8_655 ?
O4 K H1W2 105.8(7) 8_655 . ?
O2W K H1W2 88.5(4) . . ?
O1W K H1W2 15.9(3) . . ?
O4 K H1W2 73.3(8) . . ?
O2 K H1W2 109.9(7) 8_655 . ?
O3 K H1W2 126.7(8) . . ?
O1W K H1W2 115.0(4) 8_655 . ?
O2W K H1W2 177.0(7) 8_655 . ?
V K H1W2 100.3(8) . . ?
V K H1W2 111.6(8) 8_655 . ?
K K H1W2 55.6(7) 8_665 . ?
K K H1W2 137.3(4) 8_655 . ?
K O1W K 93.36(6) . 8_665 ?
K O1W H1W1 134(3) . . ?
K O1W H1W1 100(3) 8_665 . ?
K O1W H1W2 98(3) . . ?
K O1W H1W2 122(3) 8_665 . ?
H1W1 O1W H1W2 110.8(17) . . ?
K O2W K 92.39(8) . 8_665 ?
K O2W H2W1 143(3) . . ?
K O2W H2W1 115(3) 8_665 . ?
K O2W H2W2 88(3) . . ?
K O2W H2W2 103(3) 8_665 . ?
H2W1 O2W H2W2 107.2(16) . . ?

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
O3 V O1 C6 -110.21(17) . . . . ?
O4 V O1 C6 140.05(17) . . . . ?
O2 V O1 C6 37.8(2) . . . . ?
N3 V O1 C6 -2.67(15) . . . . ?
K V O1 C6 -167.46(15) . . . . ?
K V O1 C6 117.96(15) 8_665 . . . ?
O3 V O2 C13 64.8(2) . . . . ?
O4 V O2 C13 175.7(2) . . . . ?
O1 V O2 C13 -82.9(2) . . . . ?
N3 V O2 C13 -43.82(19) . . . . ?
K V O2 C13 123.66(18) . . . . ?
K V O2 C13 171.2(2) 8_665 . . . ?
O3 V O2 K -106.43(8) . . . 8_665 ?
O4 V O2 K 4.48(8) . . . 8_665 ?
O1 V O2 K 105.92(13) . . . 8_665 ?
N3 V O2 K 144.96(7) . . . 8_665 ?
K V O2 K -47.56(6) . . . 8_665 ?
O4 V O3 K 3.50(9) . . . . ?
O2 V O3 K 103.78(7) . . . . ?
O1 V O3 K -92.49(7) . . . . ?
N3 V O3 K -169.66(6) . . . . ?
K V O3 K 49.55(6) 8_665 . . . ?
O3 V O4 K 101.74(10) . . . 8_665 ?
O2 V O4 K -5.16(9) . . . 8_665 ?
O1 V O4 K -155.01(8) . . . 8_665 ?
N3 V O4 K -88.42(12) . . . 8_665 ?
K V O4 K 105.41(9) . . . 8_665 ?
O3 V O4 K -3.67(9) . . . . ?
O2 V O4 K -110.57(7) . . . . ?
O1 V O4 K 99.58(7) . . . . ?
N3 V O4 K 166.17(8) . . . . ?
K V O4 K -105.41(9) 8_665 . . . ?
C6 N2 N3 C7 177.63(19) . . . . ?
C6 N2 N3 V -3.1(2) . . . . ?
O3 V N3 C7 -80.4(2) . . . . ?
O4 V N3 C7 109.8(2) . . . . ?
O2 V N3 C7 21.95(19) . . . . ?
O1 V N3 C7 -177.7(2) . . . . ?
K V N3 C7 -112.1(2) . . . . ?
K V N3 C7 54.7(2) 8_665 . . . ?
O3 V N3 N2 100.37(15) . . . . ?
O4 V N3 N2 -69.41(19) . . . . ?
O2 V N3 N2 -157.24(15) . . . . ?
O1 V N3 N2 3.15(14) . . . . ?
K V N3 N2 68.7(2) . . . . ?
K V N3 N2 -124.45(12) 8_665 . . . ?
C5 N1 C1 C2 -1.0(4) . . . . ?
N1 C1 C2 C3 1.5(4) . . . . ?
C1 C2 C3 C4 -0.5(4) . . . . ?
C1 C2 C3 C6 -179.2(2) . . . . ?
C2 C3 C4 C5 -0.8(4) . . . . ?
C6 C3 C4 C5 177.9(2) . . . . ?
C1 N1 C5 C4 -0.4(4) . . . . ?
C3 C4 C5 N1 1.4(4) . . . . ?
N3 N2 C6 O1 0.9(3) . . . . ?
N3 N2 C6 C3 178.35(18) . . . . ?
V O1 C6 N2 2.0(3) . . . . ?
V O1 C6 C3 -175.50(14) . . . . ?
C4 C3 C6 N2 -170.9(2) . . . . ?
C2 C3 C6 N2 7.8(3) . . . . ?
C4 C3 C6 O1 6.7(3) . . . . ?
C2 C3 C6 O1 -174.6(2) . . . . ?
N2 N3 C7 C8 -178.94(18) . . . . ?
V N3 C7 C8 1.9(3) . . . . ?
N2 N3 C7 C7' 0.7(3) . . . . ?
V N3 C7 C7' -178.49(16) . . . . ?
N3 C7 C8 C9 163.5(2) . . . . ?
C7' C7 C8 C9 -16.1(3) . . . . ?
N3 C7 C8 C13 -18.3(3) . . . . ?
C7' C7 C8 C13 162.0(2) . . . . ?
C13 C8 C9 C10 0.3(4) . . . . ?
C7 C8 C9 C10 178.6(2) . . . . ?
C8 C9 C10 C11 0.0(4) . . . . ?
C9 C10 C11 C12 -0.1(4) . . . . ?
C10 C11 C12 C13 0.0(4) . . . . ?
V O2 C13 C12 -139.93(19) . . . . ?
K O2 C13 C12 28.0(3) 8_665 . . . ?
V O2 C13 C8 43.1(3) . . . . ?
K O2 C13 C8 -149.04(17) 8_665 . . . ?
C11 C12 C13 O2 -176.8(2) . . . . ?
C11 C12 C13 C8 0.3(4) . . . . ?
C9 C8 C13 O2 176.6(2) . . . . ?
C7 C8 C13 O2 -1.6(3) . . . . ?
C9 C8 C13 C12 -0.4(3) . . . . ?
C7 C8 C13 C12 -178.6(2) . . . . ?
V O4 K O4 -95.15(12) . . . 8_655 ?
K O4 K O4 149.54(7) 8_665 . . 8_655 ?
V O4 K O2W 77.68(9) . . . . ?
K O4 K O2W -37.63(8) 8_665 . . . ?
V O4 K O1W 154.14(9) . . . . ?
K O4 K O1W 38.83(6) 8_665 . . . ?
V O4 K O2 67.99(19) . . . 8_655 ?
K O4 K O2 -47.32(19) 8_665 . . 8_655 ?
V O4 K O3 2.34(6) . . . . ?
K O4 K O3 -112.96(7) 8_665 . . . ?
V O4 K O1W -67.86(8) . . . 8_655 ?
K O4 K O1W 176.83(7) 8_665 . . 8_655 ?
V O4 K O2W -10.45(10) . . . 8_655 ?
K O4 K O2W -125.76(7) 8_665 . . 8_655 ?
K O4 K V -115.31(9) 8_665 . . . ?
V O4 K V -75.54(19) . . . 8_655 ?
K O4 K V 169.15(14) 8_665 . . 8_655 ?
V O4 K K 115.31(9) . . . 8_665 ?
V O4 K K -54.28(7) . . . 8_655 ?
K O4 K K -169.59(3) 8_665 . . 8_655 ?
V O3 K O4 133.75(7) . . . 8_655 ?
V O3 K O2W -87.98(10) . . . . ?
V O3 K O1W -34.11(10) . . . . ?
V O3 K O4 -2.35(6) . . . . ?
V O3 K O2 -162.94(7) . . . 8_655 ?
V O3 K O1W 88.32(8) . . . 8_655 ?
V O3 K O2W 163.10(11) . . . 8_655 ?
V O3 K V 162.42(5) . . . 8_655 ?
V O3 K K -39.09(6) . . . 8_665 ?
V O3 K K 128.21(7) . . . 8_655 ?
O3 V K O4 -65.56(10) . . . 8_655 ?
O4 V K O4 118.61(11) . . . 8_655 ?
O2 V K O4 -160.28(8) . . . 8_655 ?
O1 V K O4 33.10(8) . . . 8_655 ?
N3 V K O4 -29.21(19) . . . 8_655 ?
K V K O4 162.27(6) 8_665 . . 8_655 ?
O3 V K O2W 82.01(10) . . . . ?
O4 V K O2W -93.82(10) . . . . ?
O2 V K O2W -12.71(9) . . . . ?
O1 V K O2W -179.33(9) . . . . ?
N3 V K O2W 118.36(19) . . . . ?
K V K O2W -50.16(7) 8_665 . . . ?
O3 V K O1W 150.97(9) . . . . ?
O4 V K O1W -24.86(8) . . . . ?
O2 V K O1W 56.26(8) . . . . ?
O1 V K O1W -110.37(7) . . . . ?
N3 V K O1W -172.68(18) . . . . ?
K V K O1W 18.81(5) 8_665 . . . ?
O3 V K O4 175.83(11) . . . . ?
O2 V K O4 81.11(9) . . . . ?
O1 V K O4 -85.51(9) . . . . ?
N3 V K O4 -147.82(19) . . . . ?
K V K O4 43.66(7) 8_665 . . . ?
O3 V K O2 25.08(10) . . . 8_655 ?
O4 V K O2 -150.75(10) . . . 8_655 ?
O2 V K O2 -69.63(7) . . . 8_655 ?
O1 V K O2 123.74(8) . . . 8_655 ?
N3 V K O2 61.43(19) . . . 8_655 ?
K V K O2 -107.09(6) 8_665 . . 8_655 ?
O4 V K O3 -175.83(11) . . . . ?
O2 V K O3 -94.72(10) . . . . ?
O1 V K O3 98.66(9) . . . . ?
N3 V K O3 36.35(19) . . . . ?
K V K O3 -132.17(8) 8_665 . . . ?
O3 V K O1W -80.20(9) . . . 8_655 ?
O4 V K O1W 103.97(9) . . . 8_655 ?
O2 V K O1W -174.92(8) . . . 8_655 ?
O1 V K O1W 18.45(7) . . . 8_655 ?
N3 V K O1W -43.86(19) . . . 8_655 ?
K V K O1W 147.63(5) 8_665 . . 8_655 ?
O3 V K O2W -14.10(9) . . . 8_655 ?
O4 V K O2W 170.07(9) . . . 8_655 ?
O2 V K O2W -108.82(8) . . . 8_655 ?
O1 V K O2W 84.56(8) . . . 8_655 ?
N3 V K O2W 22.25(19) . . . 8_655 ?
K V K O2W -146.27(6) 8_665 . . 8_655 ?
O3 V K V -28.16(9) . . . 8_655 ?
O4 V K V 156.01(8) . . . 8_655 ?
O2 V K V -122.88(7) . . . 8_655 ?
O1 V K V 70.50(7) . . . 8_655 ?
N3 V K V 8.2(2) . . . 8_655 ?
K V K V -160.33(3) 8_665 . . 8_655 ?
O3 V K K 132.17(8) . . . 8_665 ?
O4 V K K -43.66(7) . . . 8_665 ?
O2 V K K 37.45(6) . . . 8_665 ?
O1 V K K -129.17(5) . . . 8_665 ?
N3 V K K 168.52(18) . . . 8_665 ?
O3 V K K -51.76(8) . . . 8_655 ?
O4 V K K 132.41(7) . . . 8_655 ?
O2 V K K -146.48(6) . . . 8_655 ?
O1 V K K 46.90(5) . . . 8_655 ?
N3 V K K -15.41(18) . . . 8_655 ?
K V K K 176.070(8) 8_665 . . 8_655 ?
O4 K O1W K -175.29(5) 8_655 . . 8_665 ?
O2W K O1W K 45.55(8) . . . 8_665 ?
O4 K O1W K -33.42(6) . . . 8_665 ?
O2 K O1W K 126.79(5) 8_655 . . 8_665 ?
O3 K O1W K -6.74(9) . . . 8_665 ?
O1W K O1W K -90.24(10) 8_655 . . 8_665 ?
O2W K O1W K 67.6(3) 8_655 . . 8_665 ?
V K O1W K -21.76(6) . . . 8_665 ?
V K O1W K 157.72(3) 8_655 . . 8_665 ?
K K O1W K -146.57(9) 8_655 . . 8_665 ?
O4 K O2W K -155.01(8) 8_655 . . 8_665 ?
O1W K O2W K -44.49(8) . . . 8_665 ?
O4 K O2W K 31.76(6) . . . 8_665 ?
O2 K O2W K -151.41(8) 8_655 . . 8_665 ?
O3 K O2W K 89.07(7) . . . 8_665 ?
O1W K O2W K 84.19(12) 8_655 . . 8_665 ?
O2W K O2W K 141.03(12) 8_655 . . 8_665 ?
V K O2W K 60.09(5) . . . 8_665 ?
V K O2W K -154.87(4) 8_655 . . 8_665 ?
K K O2W K 143.32(6) 8_655 . . 8_665 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.55
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.070
_database_code_depnum_ccdc_archive 'CCDC 991927'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H9 N3 O4 V, 4(H2 O), Na'
_chemical_formula_sum            'C13 H17 N3 Na O8 V'
_chemical_formula_weight         417.23

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'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   7.7429(8)
_cell_length_b                   10.3131(10)
_cell_length_c                   12.0373(13)
_cell_angle_alpha                109.590(6)
_cell_angle_beta                 104.363(5)
_cell_angle_gamma                92.983(5)
_cell_volume                     867.59(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5267
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.59

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             428
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8453
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'

_exptl_special_details           
;
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17852
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         30.65
_reflns_number_total             5283
_reflns_number_gt                4107
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'

_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 > 2σ(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)+(0.0570P)²+0.0946P] 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         5283
_refine_ls_number_parameters     259
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1106
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V V 0.62993(4) 0.19701(3) 0.87665(2) 0.02659(9) Uani 1 1 d . . .
O1 O 0.75471(19) 0.33177(12) 1.04443(11) 0.0389(3) Uani 1 1 d . . .
O2 O 0.4838(2) 0.14043(13) 0.71122(12) 0.0472(4) Uani 1 1 d . . .
O3 O 0.79476(19) 0.10878(16) 0.86069(12) 0.0501(4) Uani 1 1 d . . .
O4 O 0.49775(19) 0.11493(14) 0.92524(12) 0.0458(4) Uani 1 1 d . . .
N1 N 1.0736(2) 0.74801(18) 1.41745(14) 0.0436(4) Uani 1 1 d . . .
N2 N 0.7271(2) 0.50991(14) 0.97139(12) 0.0337(3) Uani 1 1 d . . .
N3 N 0.63428(19) 0.39756(14) 0.86394(12) 0.0286(3) Uani 1 1 d . . .
C1 C 0.9896(3) 0.7917(2) 1.32921(18) 0.0447(5) Uani 1 1 d . . .
H1 H 0.9943 0.8871 1.3478 0.054 Uiso 1 1 calc R . .
C2 C 0.8959(3) 0.70489(19) 1.21203(16) 0.0384(4) Uani 1 1 d . . .
H2 H 0.8408 0.7412 1.1534 0.046 Uiso 1 1 calc R . .
C3 C 0.8854(2) 0.56252(17) 1.18315(15) 0.0297(4) Uani 1 1 d . . .
C4 C 0.9711(3) 0.5148(2) 1.27441(16) 0.0416(5) Uani 1 1 d . . .
H4 H 0.9671 0.4200 1.2590 0.050 Uiso 1 1 calc R . .
C5 C 1.0626(3) 0.6115(2) 1.38882(18) 0.0479(5) Uani 1 1 d . . .
H5 H 1.1201 0.5786 1.4494 0.058 Uiso 1 1 calc R . .
C6 C 0.7838(2) 0.46334(16) 1.05892(15) 0.0283(3) Uani 1 1 d . . .
C7 C 0.5616(2) 0.43396(17) 0.77208(15) 0.0305(4) Uani 1 1 d . . .
H7 H 0.5739 0.5285 0.7849 0.037 Uiso 1 1 calc R . .
C8 C 0.4636(2) 0.33936(18) 0.65210(15) 0.0302(4) Uani 1 1 d . . .
C9 C 0.3996(3) 0.3917(2) 0.55891(17) 0.0440(5) Uani 1 1 d . . .
H9 H 0.4161 0.4874 0.5777 0.053 Uiso 1 1 calc R . .
C10 C 0.3131(3) 0.3057(2) 0.44041(18) 0.0507(6) Uani 1 1 d . . .
H10 H 0.2725 0.3420 0.3791 0.061 Uiso 1 1 calc R . .
C11 C 0.2875(3) 0.1626(2) 0.41440(17) 0.0441(5) Uani 1 1 d . . .
H11 H 0.2305 0.1028 0.3344 0.053 Uiso 1 1 calc R . .
C12 C 0.3445(3) 0.1083(2) 0.50402(16) 0.0380(4) Uani 1 1 d . . .
H12 H 0.3239 0.0126 0.4846 0.046 Uiso 1 1 calc R . .
C13 C 0.4339(2) 0.19564(18) 0.62521(15) 0.0310(4) Uani 1 1 d . . .
Na Na 0.32872(10) 0.08539(8) 1.05851(7) 0.04001(19) Uani 1 1 d . . .
O1W O 0.5736(2) 0.25076(16) 1.20731(14) 0.0489(4) Uani 1 1 d D . .
H1W1 H 0.642(3) 0.276(3) 1.173(2) 0.073 Uiso 1 1 d D . .
H1W2 H 0.639(3) 0.218(3) 1.254(2) 0.073 Uiso 1 1 d D . .
O2W O 0.0996(2) -0.04044(17) 0.87506(14) 0.0507(4) Uani 1 1 d D . .
H2W1 H 0.025(3) 0.014(2) 0.866(3) 0.076 Uiso 1 1 d D . .
H2W2 H 0.134(4) -0.052(3) 0.8126(17) 0.076 Uiso 1 1 d D . .
O3W O 0.1474(2) 0.25421(17) 1.09545(18) 0.0573(4) Uani 1 1 d D . .
H3W1 H 0.062(3) 0.216(3) 1.108(3) 0.086 Uiso 1 1 d D . .
H3W2 H 0.141(4) 0.311(3) 1.060(3) 0.086 Uiso 1 1 d D . .
O4W O 0.2303(2) -0.09714(15) 0.66829(12) 0.0472(4) Uani 1 1 d D . .
H4W1 H 0.175(3) -0.138(2) 0.5946(11) 0.071 Uiso 1 1 d D . .
H4W2 H 0.314(3) -0.038(2) 0.676(2) 0.071 Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
V O3 1.6183(14) . ?
V O4 1.6263(14) . ?
V O2 1.9027(13) . ?
V O1 1.9884(12) . ?
V N3 2.1236(14) . ?
V Na 3.2698(8) 2_657 ?
O1 C6 1.309(2) . ?
O2 C13 1.329(2) . ?
O3 Na 2.7274(19) 2_657 ?
O4 Na 2.3889(16) . ?
O4 Na 2.5576(18) 2_657 ?
N1 C5 1.325(3) . ?
N1 C1 1.328(3) . ?
N2 C6 1.291(2) . ?
N2 N3 1.4067(18) . ?
N3 C7 1.293(2) . ?
C1 C2 1.377(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.384(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(3) . ?
C3 C6 1.486(2) . ?
C4 C5 1.384(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C7 C8 1.431(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.397(2) . ?
C8 C13 1.400(2) . ?
C9 C10 1.373(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.395(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.366(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.404(2) . ?
C12 H12 0.9300 . ?
Na O3W 2.2904(18) . ?
Na O2W 2.3668(17) . ?
Na O1W 2.3751(18) . ?
Na O4 2.5576(18) 2_657 ?
Na O3 2.7274(19) 2_657 ?
Na V 3.2698(8) 2_657 ?
Na Na 3.5773(16) 2_657 ?
Na H3W1 2.61(3) . ?
O1W H1W1 0.828(10) . ?
O1W H1W2 0.829(10) . ?
O2W H2W1 0.839(10) . ?
O2W H2W2 0.830(10) . ?
O3W H3W1 0.823(10) . ?
O3W H3W2 0.832(10) . ?
O4W H4W1 0.831(10) . ?
O4W H4W2 0.835(10) . ?

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
O3 V O4 106.57(9) . . ?
O3 V O2 101.49(7) . . ?
O4 V O2 97.17(7) . . ?
O3 V O1 96.32(7) . . ?
O4 V O1 93.44(6) . . ?
O2 V O1 155.67(6) . . ?
O3 V N3 121.76(8) . . ?
O4 V N3 130.78(7) . . ?
O2 V N3 82.79(5) . . ?
O1 V N3 73.74(5) . . ?
O3 V Na 56.30(6) . 2_657 ?
O4 V Na 50.29(6) . 2_657 ?
O2 V Na 106.76(4) . 2_657 ?
O1 V Na 96.87(4) . 2_657 ?
N3 V Na 170.41(4) . 2_657 ?
C6 O1 V 117.88(10) . . ?
C13 O2 V 138.21(11) . . ?
V O3 Na 94.12(7) . 2_657 ?
V O4 Na 156.91(8) . . ?
V O4 Na 100.42(7) . 2_657 ?
Na O4 Na 92.58(5) . 2_657 ?
C5 N1 C1 116.52(16) . . ?
C6 N2 N3 108.75(13) . . ?
C7 N3 N2 113.84(13) . . ?
C7 N3 V 129.88(11) . . ?
N2 N3 V 116.28(10) . . ?
N1 C1 C2 124.28(18) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C1 C2 C3 118.69(18) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C2 C3 C4 117.89(16) . . ?
C2 C3 C6 121.29(16) . . ?
C4 C3 C6 120.82(16) . . ?
C5 C4 C3 118.53(18) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N1 C5 C4 124.07(19) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
N2 C6 O1 123.14(14) . . ?
N2 C6 C3 119.26(15) . . ?
O1 C6 C3 117.59(14) . . ?
N3 C7 C8 124.73(15) . . ?
N3 C7 H7 117.6 . . ?
C8 C7 H7 117.6 . . ?
C9 C8 C13 119.29(16) . . ?
C9 C8 C7 119.06(16) . . ?
C13 C8 C7 121.64(15) . . ?
C10 C9 C8 121.84(19) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C9 C10 C11 118.24(19) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C12 C11 C10 121.36(17) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 120.64(18) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
O2 C13 C8 122.00(15) . . ?
O2 C13 C12 119.40(16) . . ?
C8 C13 C12 118.59(16) . . ?
O3W Na O2W 87.63(7) . . ?
O3W Na O1W 88.20(6) . . ?
O2W Na O1W 163.04(7) . . ?
O3W Na O4 110.65(7) . . ?
O2W Na O4 85.12(6) . . ?
O1W Na O4 80.99(6) . . ?
O3W Na O4 161.51(7) . 2_657 ?
O2W Na O4 98.14(6) . 2_657 ?
O1W Na O4 90.96(6) . 2_657 ?
O4 Na O4 87.42(5) . 2_657 ?
O3W Na O3 104.80(6) . 2_657 ?
O2W Na O3 83.40(6) . 2_657 ?
O1W Na O3 113.56(6) . 2_657 ?
O4 Na O3 142.12(5) . 2_657 ?
O4 Na O3 58.86(5) 2_657 2_657 ?
O3W Na V 133.97(6) . 2_657 ?
O2W Na V 90.42(5) . 2_657 ?
O1W Na V 104.23(5) . 2_657 ?
O4 Na V 114.99(5) . 2_657 ?
O4 Na V 29.29(3) 2_657 2_657 ?
O3 Na V 29.58(3) 2_657 2_657 ?
O3W Na Na 156.00(6) . 2_657 ?
O2W Na Na 92.54(5) . 2_657 ?
O1W Na Na 84.69(5) . 2_657 ?
O4 Na Na 45.58(4) . 2_657 ?
O4 Na Na 41.84(4) 2_657 2_657 ?
O3 Na Na 99.05(4) 2_657 2_657 ?
V Na Na 70.03(2) 2_657 2_657 ?
O3W Na H3W1 17.9(4) . . ?
O2W Na H3W1 80.9(7) . . ?
O1W Na H3W1 99.5(6) . . ?
O4 Na H3W1 125.9(5) . . ?
O4 Na H3W1 146.1(4) 2_657 . ?
O3 Na H3W1 87.5(4) 2_657 . ?
V Na H3W1 117.0(4) 2_657 . ?
Na Na H3W1 170.1(6) 2_657 . ?
Na O1W H1W1 110(2) . . ?
Na O1W H1W2 113(2) . . ?
H1W1 O1W H1W2 104(3) . . ?
Na O2W H2W1 106(2) . . ?
Na O2W H2W2 113(2) . . ?
H2W1 O2W H2W2 100(2) . . ?
Na O3W H3W1 103(2) . . ?
Na O3W H3W2 121(2) . . ?
H3W1 O3W H3W2 125(3) . . ?
H4W1 O4W H4W2 111(2) . . ?

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
O3 V O1 C6 117.35(15) . . . . ?
O4 V O1 C6 -135.55(14) . . . . ?
O2 V O1 C6 -19.7(2) . . . . ?
N3 V O1 C6 -3.94(13) . . . . ?
Na V O1 C6 174.05(13) 2_657 . . . ?
O3 V O2 C13 -111.7(2) . . . . ?
O4 V O2 C13 139.7(2) . . . . ?
O1 V O2 C13 24.5(3) . . . . ?
N3 V O2 C13 9.3(2) . . . . ?
Na V O2 C13 -169.70(19) 2_657 . . . ?
O4 V O3 Na -1.44(7) . . . 2_657 ?
O2 V O3 Na -102.59(6) . . . 2_657 ?
O1 V O3 Na 94.06(5) . . . 2_657 ?
N3 V O3 Na 168.83(5) . . . 2_657 ?
O3 V O4 Na 124.8(2) . . . . ?
O2 V O4 Na -130.9(2) . . . . ?
O1 V O4 Na 27.2(2) . . . . ?
N3 V O4 Na -44.3(3) . . . . ?
Na V O4 Na 123.2(2) 2_657 . . . ?
O3 V O4 Na 1.56(7) . . . 2_657 ?
O2 V O4 Na 105.86(6) . . . 2_657 ?
O1 V O4 Na -96.07(6) . . . 2_657 ?
N3 V O4 Na -167.50(5) . . . 2_657 ?
C6 N2 N3 C7 175.86(16) . . . . ?
C6 N2 N3 V -3.10(19) . . . . ?
O3 V N3 C7 97.70(17) . . . . ?
O4 V N3 C7 -94.65(18) . . . . ?
O2 V N3 C7 -1.38(17) . . . . ?
O1 V N3 C7 -174.92(18) . . . . ?
Na V N3 C7 173.03(19) 2_657 . . . ?
O3 V N3 N2 -83.54(13) . . . . ?
O4 V N3 N2 84.12(14) . . . . ?
O2 V N3 N2 177.38(13) . . . . ?
O1 V N3 N2 3.84(11) . . . . ?
Na V N3 N2 -8.2(4) 2_657 . . . ?
C5 N1 C1 C2 -0.9(3) . . . . ?
N1 C1 C2 C3 0.9(3) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C3 C6 179.00(18) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C6 C3 C4 C5 -179.49(18) . . . . ?
C1 N1 C5 C4 0.3(3) . . . . ?
C3 C4 C5 N1 0.2(4) . . . . ?
N3 N2 C6 O1 -0.3(2) . . . . ?
N3 N2 C6 C3 -179.49(14) . . . . ?
V O1 C6 N2 3.9(2) . . . . ?
V O1 C6 C3 -176.95(12) . . . . ?
C2 C3 C6 N2 10.3(3) . . . . ?
C4 C3 C6 N2 -170.43(18) . . . . ?
C2 C3 C6 O1 -168.93(17) . . . . ?
C4 C3 C6 O1 10.3(3) . . . . ?
N2 N3 C7 C8 178.54(16) . . . . ?
V N3 C7 C8 -2.7(3) . . . . ?
N3 C7 C8 C9 -176.70(19) . . . . ?
N3 C7 C8 C13 1.8(3) . . . . ?
C13 C8 C9 C10 -2.1(3) . . . . ?
C7 C8 C9 C10 176.5(2) . . . . ?
C8 C9 C10 C11 0.8(4) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 C13 -1.2(3) . . . . ?
V O2 C13 C8 -12.4(3) . . . . ?
V O2 C13 C12 169.21(16) . . . . ?
C9 C8 C13 O2 -176.71(18) . . . . ?
C7 C8 C13 O2 4.8(3) . . . . ?
C9 C8 C13 C12 1.7(3) . . . . ?
C7 C8 C13 C12 -176.83(17) . . . . ?
C11 C12 C13 O2 178.32(19) . . . . ?
C11 C12 C13 C8 -0.1(3) . . . . ?
V O4 Na O3W 51.4(2) . . . . ?
Na O4 Na O3W 175.99(7) 2_657 . . . ?
V O4 Na O2W 137.0(2) . . . . ?
Na O4 Na O2W -98.40(6) 2_657 . . . ?
V O4 Na O1W -33.2(2) . . . . ?
Na O4 Na O1W 91.38(6) 2_657 . . . ?
V O4 Na O4 -124.6(2) . . . 2_657 ?
Na O4 Na O4 0.0 2_657 . . 2_657 ?
V O4 Na O3 -150.3(2) . . . 2_657 ?
Na O4 Na O3 -25.71(9) 2_657 . . 2_657 ?
V O4 Na V -134.8(2) . . . 2_657 ?
Na O4 Na V -10.21(4) 2_657 . . 2_657 ?
V O4 Na Na -124.6(2) . . . 2_657 ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        30.65
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.066
_database_code_depnum_ccdc_archive 'CCDC 991928'
