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By the reaction of ammonium perchlorate with anion-incorporated bowl-type dodeca­vanadates, viz. [V12O32(X)]5− [X = N3 (1), OCN and NO3], tube-type tetra­deca­vanadates, viz. (NH4)7[V14O38(X)] [X = N3 (2), OCN (3) and NO3 (4)] were synthesized. The crystal structures of penta­­(tetra­ethyl­ammonium) azido­dodeca­vanadate nitro­methane monosolvate, (C8H20N)5[V12O32(N3)]·CH3NO2, 1, hepta­ammonium azido­tetra­deca­vanadate dimethyl sulfoxide hexa­solvate, (NH4)7[V14O38(N3)]·6C2H6OS, 2, hepta­ammonium cyanato­tetra­deca­vanadate dimethyl sulfoxide hexa­solvate, (NH4)7[V14O38(OCN)]·6C2H6OS, 3, and hepta­ammonium nitrato­tetra­deca­vanadate dimethyl sulfoxide hexa­solvate, (NH4)7[V14O38(NO3)]·6C2H6OS, 4, were determined. The tube consists of two layers of V7 rings with a guest anion at the centre. The distances between the incorporated anions and the nearest V atoms are 3.058 (3), 3.039 (6) and 2.811 (9) Å for 2, 3 and 4, respectively, showing that the incorporated anions are stabilized via noncovalent inter­actions. Two ammonium cations cap both ends of the tube to stabilize the structures via hydrogen-bonding inter­actions. Linear OCN and N3 anions sit on the twofold rotation axes of the tube frameworks and the triangular plane of the NO3 anion deviates from the equatorial plane of the tube by ca 30°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618008914/jr3005sup1.cif
Contains datablocks 1, 2, 3, 4, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618008914/jr30051sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618008914/jr30052sup3.hkl
Contains datablock 2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618008914/jr30053sup4.hkl
Contains datablock 3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618008914/jr30054sup5.hkl
Contains datablock 4

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618008914/jr3005sup6.pdf
NMR and IR spectra

CCDC references: 1850101; 1850100; 1850099; 1850098

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2006) for (1), (2), (3); SMART (Bruker, 2015) for (4). Cell refinement: CrystalClear (Rigaku/MSC, 2006) for (1), (2), (3); SAINT (Bruker, 2015) for (4). Data reduction: CrystalClear (Rigaku/MSC, 2006) for (1), (2), (3); SAINT (Bruker, 2015) for (4). For all structures, program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b).

Pentakis(tetraethylammonium) azidododecavanadate nitromethane monosolvate (1) top
Crystal data top
(C8H20N)5[V12O32(N3)]·CH3NO2Dx = 1.751 Mg m3
Mr = 1877.60Mo Kα radiation, λ = 0.7107 Å
Orthorhombic, Pna21Cell parameters from 31221 reflections
a = 26.3672 (11) Åθ = 3.1–27.5°
b = 13.0801 (5) ŵ = 1.59 mm1
c = 20.6502 (8) ÅT = 83 K
V = 7122.0 (5) Å3Prism, brown
Z = 40.24 × 0.24 × 0.14 mm
F(000) = 3840
Data collection top
Rigaku Mercury70
diffractometer
15235 reflections with I > 2σ(I)
Detector resolution: 7.314 pixels mm-1Rint = 0.046
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: numerical
(NUMABS; Rigaku, 1999)
h = 3433
Tmin = 0.680, Tmax = 0.796k = 1416
76477 measured reflectionsl = 2626
16085 independent reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.037 w = 1/[σ2(Fo2) + (0.0378P)2 + 4.2487P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.088(Δ/σ)max = 0.001
S = 1.12Δρmax = 0.71 e Å3
16085 reflectionsΔρmin = 0.43 e Å3
949 parametersAbsolute structure: Flack x determined using 6803 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
7 restraintsAbsolute structure parameter: 0.022 (6)
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C1010.5092 (2)0.5559 (5)0.1721 (3)0.0320 (12)
H10A0.53430.60390.19070.038*
H10B0.50430.50000.20380.038*
C1020.4592 (3)0.6120 (5)0.1639 (3)0.0440 (16)
H10C0.44800.63830.20590.066*
H10D0.46370.66900.13360.066*
H10E0.43360.56480.14670.066*
C1030.5793 (2)0.4550 (6)0.1315 (3)0.0400 (15)
H10F0.60270.50550.15100.048*
H10G0.57020.40520.16560.048*
C1040.6070 (3)0.3994 (8)0.0791 (4)0.073 (3)
H10H0.63720.36630.09740.109*
H10I0.58480.34750.06010.109*
H10J0.61740.44800.04550.109*
C1050.4941 (2)0.4375 (4)0.0788 (3)0.0296 (12)
H10K0.46380.47680.06550.035*
H10L0.50990.40980.03900.035*
C1060.4771 (3)0.3488 (5)0.1204 (3)0.0435 (15)
H10M0.45330.30620.09590.065*
H10N0.50660.30780.13280.065*
H10O0.46030.37490.15940.065*
C1070.5429 (2)0.5918 (5)0.0611 (3)0.0316 (12)
H10P0.51040.62120.04590.038*
H10Q0.55940.55890.02340.038*
C1080.5766 (2)0.6785 (5)0.0843 (3)0.0394 (14)
H10R0.58190.72730.04890.059*
H10S0.56030.71340.12080.059*
H10T0.60940.65090.09820.059*
C2010.85630 (19)0.4283 (4)0.3478 (3)0.0278 (11)
H20A0.83130.48050.36150.033*
H20B0.83980.38510.31460.033*
C2020.8685 (2)0.3618 (5)0.4056 (3)0.0399 (14)
H20C0.83730.33040.42200.060*
H20D0.89240.30800.39260.060*
H20E0.88390.40370.43970.060*
C2030.8779 (2)0.5532 (4)0.2660 (3)0.0310 (12)
H20F0.85310.59870.28760.037*
H20G0.85900.51100.23420.037*
C2040.9158 (3)0.6188 (6)0.2296 (4)0.0476 (17)
H20H0.89790.66160.19810.071*
H20I0.93410.66240.26030.071*
H20J0.94000.57460.20690.071*
C2050.9309 (2)0.5428 (5)0.3667 (3)0.0417 (15)
H20K0.94540.49360.39810.050*
H20L0.95960.57710.34470.050*
C2060.9012 (2)0.6228 (5)0.4040 (4)0.0502 (19)
H20M0.92360.65680.43510.075*
H20N0.88750.67350.37380.075*
H20O0.87320.58980.42730.075*
C2070.9379 (2)0.4072 (5)0.2877 (3)0.0400 (15)
H20P0.96850.44490.27350.048*
H20Q0.94850.35940.32230.048*
C2080.9190 (3)0.3461 (6)0.2320 (4)0.0490 (17)
H20R0.94570.29960.21710.074*
H20S0.88930.30630.24550.074*
H20T0.90940.39210.19660.074*
C3010.5703 (4)0.9542 (7)0.5351 (4)0.033 (2)0.633 (8)
H30A0.59730.90680.54960.039*0.633 (8)
H30B0.55800.99100.57390.039*0.633 (8)
C3510.5589 (6)0.9480 (11)0.4658 (7)0.031 (4)0.367 (8)
H35A0.53620.97990.43330.037*0.367 (8)
H35B0.58020.89790.44220.037*0.367 (8)
C3020.5274 (3)0.8911 (5)0.5095 (4)0.0433 (16)
H30C0.51560.84430.54330.065*0.633 (8)
H30D0.49950.93610.49640.065*0.633 (8)
H30E0.53900.85160.47200.065*0.633 (8)
H35C0.50740.84100.48500.065*0.367 (8)
H35D0.54870.85550.54110.065*0.367 (8)
H35E0.50450.93800.53220.065*0.367 (8)
C3030.6235 (3)0.9692 (6)0.4361 (4)0.0252 (18)0.633 (8)
H30F0.65110.93010.45700.030*0.633 (8)
H30G0.59970.91890.41710.030*0.633 (8)
C3530.6169 (7)1.0892 (12)0.4372 (7)0.033 (4)0.367 (8)
H35F0.64121.13890.45580.040*0.367 (8)
H35G0.58971.12900.41580.040*0.367 (8)
C3040.6445 (2)1.0274 (5)0.3853 (3)0.0365 (13)
H30H0.66160.98170.35460.055*0.633 (8)
H30I0.61751.06480.36300.055*0.633 (8)
H30J0.66911.07600.40310.055*0.633 (8)
H35H0.65811.07380.35230.055*0.367 (8)
H35I0.67250.98930.40530.055*0.367 (8)
H35J0.62080.97930.36510.055*0.367 (8)
C3050.5551 (4)1.0956 (7)0.4559 (5)0.034 (2)0.633 (8)
H30K0.53721.05160.42420.040*0.633 (8)
H30L0.57291.14950.43110.040*0.633 (8)
C3550.5609 (7)1.1099 (12)0.5307 (9)0.038 (4)0.367 (8)
H35K0.55111.07690.57200.045*0.367 (8)
H35L0.58241.16960.54160.045*0.367 (8)
C3060.5156 (2)1.1465 (5)0.4994 (3)0.0379 (14)
H30M0.49201.18620.47270.057*0.633 (8)
H30N0.49681.09390.52320.057*0.633 (8)
H30O0.53271.19210.53010.057*0.633 (8)
H35M0.49791.19420.52820.057*0.367 (8)
H35N0.52471.18160.45910.057*0.367 (8)
H35O0.49331.08860.48950.057*0.367 (8)
C3070.6307 (4)1.0988 (7)0.5250 (5)0.035 (2)0.633 (8)
H30P0.61131.14040.55650.042*0.633 (8)
H30Q0.64521.14660.49290.042*0.633 (8)
C3570.6315 (7)0.9844 (12)0.5373 (8)0.037 (4)0.367 (8)
H35P0.61240.96010.57560.045*0.367 (8)
H35Q0.64650.92350.51630.045*0.367 (8)
C3080.6737 (3)1.0504 (6)0.5605 (4)0.0549 (19)
H30R0.69451.10360.58080.082*0.633 (8)
H30S0.66031.00470.59410.082*0.633 (8)
H30T0.69451.01100.53010.082*0.633 (8)
H35R0.69521.01140.59040.082*0.367 (8)
H35S0.69391.07320.52350.082*0.367 (8)
H35T0.65971.11000.58310.082*0.367 (8)
C4010.3433 (2)0.5922 (4)0.3322 (3)0.0310 (12)
H40A0.35940.64040.36290.037*
H40B0.37070.55240.31130.037*
C4020.3164 (2)0.6529 (5)0.2810 (3)0.0360 (13)
H40C0.34070.69780.25900.054*
H40D0.30110.60620.24940.054*
H40E0.28970.69440.30110.054*
C4030.3446 (2)0.4705 (4)0.4203 (3)0.0328 (12)
H40F0.37070.42990.39740.039*
H40G0.36220.52550.44430.039*
C4040.3179 (3)0.4018 (5)0.4685 (3)0.0448 (16)
H40H0.34280.37370.49890.067*
H40I0.29260.44150.49240.067*
H40J0.30110.34580.44540.067*
C4050.2872 (2)0.4375 (4)0.3271 (3)0.0345 (13)
H40K0.26540.39300.35410.041*
H40L0.26510.47140.29490.041*
C4060.3246 (3)0.3710 (5)0.2915 (3)0.0441 (16)
H40M0.30610.32100.26510.066*
H40N0.34580.41360.26340.066*
H40O0.34610.33500.32280.066*
C4070.2661 (2)0.5740 (5)0.4017 (3)0.0360 (13)
H40P0.24410.52250.42290.043*
H40Q0.24580.60720.36730.043*
C4080.2803 (3)0.6546 (5)0.4517 (3)0.0465 (16)
H40R0.24940.68570.46920.070*
H40S0.29950.62250.48680.070*
H40T0.30120.70750.43110.070*
C5010.7064 (2)0.4383 (4)0.5442 (3)0.0298 (12)
H50A0.68240.48510.52230.036*
H50B0.72440.39920.51020.036*
C5020.6763 (3)0.3643 (5)0.5852 (3)0.0421 (15)
H50C0.65250.32660.55770.063*
H50D0.69960.31610.60630.063*
H50E0.65750.40220.61830.063*
C5030.7192 (2)0.5698 (4)0.6312 (3)0.0324 (13)
H50F0.74570.60890.65440.039*
H50G0.70210.52540.66340.039*
C5040.6801 (3)0.6454 (5)0.6043 (3)0.0424 (15)
H50H0.66570.68550.64000.064*
H50I0.69660.69150.57340.064*
H50J0.65290.60770.58240.064*
C5050.7813 (2)0.4336 (4)0.6180 (3)0.0305 (12)
H50K0.80470.47740.64330.037*
H50L0.76170.39200.64920.037*
C5060.8120 (3)0.3636 (5)0.5766 (3)0.0414 (15)
H50M0.83440.32240.60400.062*
H50N0.78930.31850.55220.062*
H50O0.83240.40410.54630.062*
C5070.7716 (2)0.5660 (4)0.5306 (3)0.0296 (12)
H50P0.78730.51950.49860.036*
H50Q0.74580.60730.50750.036*
C5080.8119 (3)0.6368 (5)0.5563 (3)0.0416 (15)
H50R0.82700.67500.52030.062*
H50S0.79660.68480.58710.062*
H50T0.83820.59680.57810.062*
C6010.5839 (2)0.0030 (4)0.2003 (3)0.0319 (12)
H60A0.56240.00210.23890.048*0.63 (3)
H60B0.59780.07220.19710.048*0.63 (3)
H60C0.61170.04640.20360.048*0.63 (3)
H65A0.61930.01080.18900.048*0.37 (3)
H65B0.56850.05910.21830.048*0.37 (3)
H65C0.58240.05780.23260.048*0.37 (3)
N6010.5537 (5)0.0192 (19)0.1428 (7)0.052 (5)0.63 (3)
O6010.5726 (5)0.017 (2)0.0892 (7)0.082 (6)0.63 (3)
O6020.5096 (3)0.046 (2)0.1532 (5)0.091 (8)0.63 (3)
N6510.5577 (10)0.032 (2)0.1457 (13)0.039 (5)0.37 (3)
O6510.5817 (9)0.039 (2)0.0950 (12)0.054 (6)0.37 (3)
O6520.5130 (7)0.053 (3)0.1481 (8)0.082 (12)0.37 (3)
N1A0.61625 (15)0.5047 (3)0.29278 (19)0.0201 (8)
N2A0.5743 (8)0.5371 (13)0.3026 (16)0.020 (4)0.40 (7)
N3A0.6583 (8)0.4747 (19)0.2904 (15)0.029 (4)0.40 (7)
N2B0.5863 (10)0.5348 (9)0.3279 (19)0.034 (6)0.60 (7)
N3B0.6510 (9)0.4690 (10)0.264 (2)0.042 (7)0.60 (7)
N1010.53142 (17)0.5106 (3)0.1106 (2)0.0279 (10)
N2010.90081 (16)0.4831 (3)0.3163 (3)0.0306 (10)
N3010.59417 (17)1.0316 (3)0.4906 (2)0.0280 (10)
N4010.31002 (16)0.5191 (3)0.3703 (2)0.0280 (9)
N5010.74488 (18)0.5019 (3)0.5812 (2)0.0272 (10)
O10.44686 (12)0.6421 (3)0.41852 (18)0.0246 (7)
O20.54199 (12)0.8770 (3)0.33350 (17)0.0234 (7)
O30.67574 (13)0.8658 (3)0.25573 (18)0.0252 (7)
O40.77593 (14)0.6810 (3)0.18415 (18)0.0269 (8)
O50.79632 (13)0.3648 (3)0.19207 (18)0.0269 (8)
O60.68581 (13)0.1277 (3)0.23276 (17)0.0228 (7)
O70.55089 (13)0.1453 (3)0.31229 (17)0.0231 (7)
O80.44961 (12)0.3237 (3)0.37863 (19)0.0266 (8)
O90.62889 (13)0.7450 (2)0.48184 (17)0.0212 (7)
O100.78154 (13)0.6233 (3)0.38230 (17)0.0230 (7)
O110.72157 (13)0.2435 (3)0.41231 (17)0.0229 (7)
O120.57042 (13)0.3630 (3)0.50779 (16)0.0218 (7)
O130.49647 (12)0.6963 (3)0.30613 (17)0.0225 (7)
O140.58624 (13)0.7592 (3)0.24087 (17)0.0221 (7)
O150.67165 (14)0.6857 (3)0.18654 (17)0.0254 (8)
O160.72513 (13)0.5059 (3)0.15671 (17)0.0235 (7)
O170.69613 (14)0.3123 (3)0.17387 (17)0.0235 (7)
O180.60098 (13)0.2491 (3)0.21917 (16)0.0212 (7)
O190.51500 (13)0.3312 (3)0.27384 (17)0.0247 (7)
O200.46441 (12)0.5060 (2)0.32053 (16)0.0205 (7)
O210.54895 (12)0.6861 (2)0.40239 (16)0.0189 (7)
O220.62604 (12)0.7415 (2)0.34636 (16)0.0185 (7)
O230.71085 (12)0.6751 (2)0.29239 (15)0.0191 (7)
O240.75416 (12)0.5137 (2)0.26934 (16)0.0202 (7)
O250.72402 (12)0.3135 (3)0.28536 (16)0.0203 (7)
O260.64061 (12)0.2612 (2)0.32529 (16)0.0185 (7)
O270.55636 (12)0.3279 (2)0.37858 (16)0.0189 (7)
O280.51764 (12)0.4862 (2)0.41649 (16)0.0191 (7)
O290.68303 (13)0.6097 (3)0.40567 (17)0.0221 (7)
O300.64398 (12)0.3843 (3)0.42254 (16)0.0217 (7)
O310.60099 (12)0.5527 (2)0.47046 (16)0.0193 (7)
O320.73551 (12)0.4380 (2)0.38378 (16)0.0190 (7)
V10.49275 (3)0.60404 (6)0.37400 (4)0.01834 (16)
V20.55565 (3)0.75935 (6)0.31894 (4)0.01749 (16)
V30.65369 (3)0.75203 (6)0.26184 (4)0.01827 (16)
V40.72825 (3)0.61615 (6)0.20811 (4)0.01968 (17)
V50.74101 (3)0.40263 (6)0.21281 (4)0.01995 (17)
V60.66843 (3)0.24481 (6)0.23926 (4)0.01739 (16)
V70.57096 (3)0.25781 (6)0.29802 (4)0.01776 (16)
V80.49418 (3)0.39189 (6)0.34844 (4)0.01821 (16)
V90.61793 (3)0.66140 (6)0.42709 (4)0.01673 (16)
V100.73046 (3)0.57422 (6)0.35346 (4)0.01784 (16)
V110.69676 (3)0.33332 (6)0.36960 (4)0.01648 (16)
V120.58328 (3)0.41967 (6)0.44091 (4)0.01761 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1010.037 (3)0.039 (3)0.019 (3)0.004 (3)0.005 (2)0.002 (2)
C1020.048 (4)0.057 (4)0.028 (3)0.018 (3)0.008 (3)0.009 (3)
C1030.032 (3)0.062 (4)0.027 (3)0.013 (3)0.003 (2)0.011 (3)
C1040.059 (5)0.121 (8)0.038 (4)0.054 (5)0.004 (4)0.019 (4)
C1050.037 (3)0.033 (3)0.019 (2)0.000 (2)0.003 (2)0.002 (2)
C1060.065 (4)0.033 (3)0.032 (3)0.008 (3)0.005 (3)0.004 (3)
C1070.031 (3)0.042 (3)0.022 (3)0.004 (2)0.005 (2)0.007 (2)
C1080.033 (3)0.051 (4)0.034 (3)0.012 (3)0.006 (2)0.013 (3)
C2010.018 (2)0.027 (3)0.038 (3)0.002 (2)0.001 (2)0.003 (2)
C2020.039 (3)0.036 (3)0.044 (4)0.006 (3)0.009 (3)0.003 (3)
C2030.024 (2)0.029 (3)0.040 (3)0.001 (2)0.000 (2)0.010 (2)
C2040.037 (3)0.049 (4)0.056 (4)0.010 (3)0.004 (3)0.018 (3)
C2050.019 (2)0.055 (4)0.051 (4)0.004 (2)0.007 (3)0.005 (3)
C2060.028 (3)0.043 (4)0.079 (5)0.005 (3)0.016 (3)0.017 (4)
C2070.021 (3)0.052 (4)0.047 (4)0.014 (3)0.008 (3)0.002 (3)
C2080.040 (3)0.052 (4)0.055 (4)0.021 (3)0.008 (3)0.003 (3)
C3010.038 (5)0.032 (5)0.028 (5)0.005 (4)0.008 (4)0.005 (4)
C3510.037 (8)0.026 (7)0.029 (8)0.004 (6)0.012 (7)0.003 (6)
C3020.047 (4)0.031 (3)0.053 (4)0.003 (3)0.005 (3)0.006 (3)
C3030.018 (3)0.027 (4)0.031 (4)0.004 (3)0.005 (3)0.000 (3)
C3530.046 (9)0.028 (7)0.026 (8)0.003 (7)0.002 (7)0.003 (6)
C3040.032 (3)0.039 (3)0.038 (3)0.009 (3)0.001 (3)0.002 (3)
C3050.039 (5)0.029 (5)0.033 (5)0.000 (4)0.003 (4)0.006 (4)
C3550.051 (10)0.025 (7)0.038 (9)0.001 (7)0.002 (8)0.006 (7)
C3060.040 (3)0.031 (3)0.042 (3)0.000 (3)0.007 (3)0.001 (3)
C3070.038 (5)0.036 (5)0.030 (5)0.002 (4)0.005 (4)0.010 (4)
C3570.050 (10)0.032 (8)0.030 (8)0.003 (7)0.019 (7)0.009 (7)
C3080.052 (4)0.069 (5)0.044 (4)0.006 (4)0.019 (3)0.006 (4)
C4010.024 (3)0.029 (3)0.041 (3)0.003 (2)0.001 (2)0.001 (2)
C4020.035 (3)0.036 (3)0.038 (3)0.002 (3)0.002 (3)0.004 (2)
C4030.027 (3)0.026 (3)0.045 (3)0.002 (2)0.013 (2)0.003 (2)
C4040.050 (4)0.040 (3)0.045 (4)0.009 (3)0.015 (3)0.011 (3)
C4050.035 (3)0.035 (3)0.034 (3)0.011 (2)0.012 (3)0.000 (2)
C4060.058 (4)0.033 (3)0.041 (4)0.005 (3)0.011 (3)0.005 (3)
C4070.031 (3)0.041 (3)0.036 (3)0.003 (2)0.000 (2)0.003 (3)
C4080.053 (4)0.037 (3)0.049 (4)0.014 (3)0.009 (3)0.004 (3)
C5010.035 (3)0.031 (3)0.023 (3)0.001 (2)0.012 (2)0.002 (2)
C5020.044 (4)0.040 (3)0.042 (3)0.010 (3)0.022 (3)0.011 (3)
C5030.041 (3)0.037 (3)0.020 (3)0.006 (3)0.009 (2)0.008 (2)
C5040.052 (4)0.041 (3)0.034 (3)0.014 (3)0.011 (3)0.009 (3)
C5050.035 (3)0.035 (3)0.022 (3)0.004 (2)0.008 (2)0.002 (2)
C5060.046 (4)0.040 (3)0.038 (3)0.013 (3)0.003 (3)0.003 (3)
C5070.038 (3)0.032 (3)0.019 (2)0.006 (2)0.010 (2)0.000 (2)
C5080.047 (4)0.043 (3)0.035 (3)0.009 (3)0.007 (3)0.002 (3)
C6010.030 (3)0.029 (3)0.036 (3)0.005 (2)0.002 (2)0.003 (2)
N6010.027 (5)0.104 (14)0.027 (5)0.002 (8)0.003 (4)0.008 (9)
O6010.039 (5)0.174 (19)0.033 (5)0.015 (9)0.002 (4)0.018 (9)
O6020.027 (4)0.21 (2)0.036 (5)0.012 (7)0.001 (4)0.017 (8)
N6510.028 (9)0.052 (13)0.036 (10)0.008 (10)0.004 (7)0.004 (11)
O6510.043 (11)0.085 (15)0.036 (10)0.008 (9)0.004 (8)0.019 (10)
O6520.025 (8)0.17 (3)0.050 (9)0.041 (12)0.002 (6)0.003 (13)
N1A0.0189 (18)0.022 (2)0.0194 (19)0.0017 (15)0.0014 (15)0.0020 (16)
N2A0.012 (5)0.031 (7)0.016 (10)0.009 (5)0.009 (6)0.001 (6)
N3A0.023 (5)0.043 (9)0.020 (10)0.014 (6)0.003 (7)0.014 (7)
N2B0.027 (8)0.030 (5)0.044 (13)0.000 (4)0.015 (9)0.001 (5)
N3B0.036 (7)0.021 (5)0.069 (18)0.008 (4)0.035 (9)0.006 (7)
N1010.030 (2)0.037 (2)0.017 (2)0.0003 (19)0.0056 (18)0.0036 (19)
N2010.0128 (18)0.032 (2)0.047 (3)0.0040 (17)0.0004 (19)0.007 (2)
N3010.033 (2)0.026 (2)0.025 (2)0.0037 (19)0.0051 (19)0.0048 (18)
N4010.023 (2)0.029 (2)0.032 (2)0.0040 (17)0.0084 (19)0.0002 (19)
N5010.033 (2)0.030 (2)0.018 (2)0.0024 (19)0.0090 (18)0.0010 (17)
O10.0163 (15)0.0281 (18)0.0293 (19)0.0023 (14)0.0009 (14)0.0017 (15)
O20.0177 (16)0.0243 (17)0.0281 (19)0.0013 (13)0.0016 (14)0.0028 (14)
O30.0265 (18)0.0243 (17)0.0248 (18)0.0016 (15)0.0048 (15)0.0048 (15)
O40.0276 (19)0.0253 (18)0.0278 (19)0.0030 (15)0.0078 (15)0.0021 (15)
O50.0218 (17)0.0307 (19)0.0283 (19)0.0002 (15)0.0085 (15)0.0032 (16)
O60.0218 (16)0.0221 (16)0.0245 (18)0.0015 (14)0.0002 (14)0.0039 (14)
O70.0192 (16)0.0225 (17)0.0276 (18)0.0046 (14)0.0026 (14)0.0047 (15)
O80.0177 (16)0.0249 (17)0.037 (2)0.0032 (13)0.0014 (15)0.0006 (16)
O90.0228 (17)0.0222 (17)0.0187 (16)0.0016 (13)0.0006 (14)0.0031 (13)
O100.0195 (16)0.0232 (17)0.0264 (18)0.0008 (13)0.0054 (14)0.0031 (15)
O110.0235 (18)0.0231 (17)0.0223 (18)0.0028 (13)0.0045 (14)0.0019 (14)
O120.0242 (17)0.0229 (17)0.0183 (16)0.0007 (14)0.0014 (14)0.0007 (14)
O130.0207 (16)0.0261 (17)0.0207 (17)0.0017 (14)0.0051 (13)0.0027 (14)
O140.0178 (16)0.0307 (18)0.0179 (16)0.0033 (14)0.0011 (14)0.0001 (14)
O150.0268 (18)0.0333 (19)0.0162 (16)0.0053 (15)0.0006 (14)0.0008 (15)
O160.0254 (18)0.0226 (17)0.0223 (17)0.0020 (14)0.0041 (14)0.0008 (14)
O170.0265 (18)0.0242 (17)0.0197 (17)0.0048 (14)0.0014 (14)0.0040 (14)
O180.0202 (17)0.0278 (18)0.0155 (16)0.0005 (13)0.0026 (13)0.0023 (13)
O190.0202 (16)0.0316 (19)0.0221 (18)0.0046 (14)0.0058 (14)0.0068 (15)
O200.0171 (15)0.0212 (16)0.0231 (17)0.0011 (13)0.0027 (14)0.0015 (14)
O210.0168 (15)0.0218 (16)0.0182 (16)0.0013 (13)0.0015 (13)0.0001 (13)
O220.0143 (15)0.0253 (17)0.0158 (15)0.0002 (12)0.0004 (13)0.0022 (13)
O230.0154 (15)0.0245 (17)0.0174 (16)0.0019 (13)0.0017 (13)0.0001 (13)
O240.0196 (16)0.0199 (16)0.0211 (17)0.0005 (13)0.0042 (13)0.0004 (13)
O250.0164 (15)0.0232 (17)0.0213 (17)0.0000 (13)0.0012 (13)0.0026 (14)
O260.0159 (15)0.0228 (16)0.0168 (16)0.0013 (13)0.0007 (13)0.0015 (13)
O270.0180 (15)0.0196 (15)0.0190 (16)0.0001 (12)0.0009 (13)0.0022 (13)
O280.0168 (15)0.0188 (15)0.0217 (16)0.0012 (12)0.0021 (13)0.0003 (13)
O290.0198 (16)0.0247 (17)0.0217 (17)0.0055 (14)0.0005 (14)0.0011 (14)
O300.0195 (16)0.0270 (18)0.0186 (16)0.0020 (14)0.0012 (14)0.0064 (14)
O310.0197 (16)0.0205 (16)0.0176 (16)0.0001 (13)0.0014 (13)0.0001 (13)
O320.0149 (15)0.0197 (16)0.0225 (17)0.0006 (12)0.0013 (13)0.0006 (14)
V10.0137 (3)0.0206 (4)0.0207 (4)0.0005 (3)0.0002 (3)0.0012 (3)
V20.0138 (3)0.0217 (4)0.0170 (4)0.0013 (3)0.0005 (3)0.0011 (3)
V30.0168 (4)0.0209 (4)0.0172 (4)0.0017 (3)0.0013 (3)0.0008 (3)
V40.0184 (4)0.0221 (4)0.0186 (4)0.0003 (3)0.0038 (3)0.0002 (3)
V50.0177 (4)0.0217 (4)0.0205 (4)0.0014 (3)0.0044 (3)0.0022 (3)
V60.0155 (4)0.0203 (4)0.0163 (4)0.0010 (3)0.0010 (3)0.0022 (3)
V70.0138 (3)0.0221 (4)0.0174 (4)0.0007 (3)0.0001 (3)0.0019 (3)
V80.0130 (3)0.0215 (4)0.0202 (4)0.0010 (3)0.0005 (3)0.0014 (3)
V90.0148 (3)0.0195 (4)0.0158 (4)0.0007 (3)0.0007 (3)0.0010 (3)
V100.0131 (3)0.0220 (4)0.0184 (4)0.0009 (3)0.0011 (3)0.0014 (3)
V110.0139 (3)0.0190 (4)0.0165 (4)0.0010 (3)0.0008 (3)0.0001 (3)
V120.0160 (4)0.0221 (4)0.0147 (4)0.0005 (3)0.0007 (3)0.0003 (3)
Geometric parameters (Å, º) top
C101—N1011.517 (7)C405—H40K0.9900
C101—C1021.519 (8)C405—H40L0.9900
C101—H10A0.9900C406—H40M0.9800
C101—H10B0.9900C406—H40N0.9800
C102—H10C0.9800C406—H40O0.9800
C102—H10D0.9800C407—N4011.510 (7)
C102—H10E0.9800C407—C4081.522 (9)
C103—C1041.494 (10)C407—H40P0.9900
C103—N1011.519 (7)C407—H40Q0.9900
C103—H10F0.9900C408—H40R0.9800
C103—H10G0.9900C408—H40S0.9800
C104—H10H0.9800C408—H40T0.9800
C104—H10I0.9800C501—C5021.510 (8)
C104—H10J0.9800C501—N5011.518 (7)
C105—C1061.511 (8)C501—H50A0.9900
C105—N1011.521 (7)C501—H50B0.9900
C105—H10K0.9900C502—H50C0.9800
C105—H10L0.9900C502—H50D0.9800
C106—H10M0.9800C502—H50E0.9800
C106—H10N0.9800C503—N5011.522 (7)
C106—H10O0.9800C503—C5041.533 (8)
C107—N1011.506 (7)C503—H50F0.9900
C107—C1081.519 (8)C503—H50G0.9900
C107—H10P0.9900C504—H50H0.9800
C107—H10Q0.9900C504—H50I0.9800
C108—H10R0.9800C504—H50J0.9800
C108—H10S0.9800C505—C5061.492 (8)
C108—H10T0.9800C505—N5011.516 (7)
C201—C2021.513 (8)C505—H50K0.9900
C201—N2011.521 (7)C505—H50L0.9900
C201—H20A0.9900C506—H50M0.9800
C201—H20B0.9900C506—H50N0.9800
C202—H20C0.9800C506—H50O0.9800
C202—H20D0.9800C507—C5081.506 (8)
C202—H20E0.9800C507—N5011.513 (7)
C203—N2011.511 (7)C507—H50P0.9900
C203—C2041.516 (8)C507—H50Q0.9900
C203—H20F0.9900C508—H50R0.9800
C203—H20G0.9900C508—H50S0.9800
C204—H20H0.9800C508—H50T0.9800
C204—H20I0.9800C601—N6511.38 (3)
C204—H20J0.9800C601—N6011.459 (16)
C205—C2061.517 (9)C601—H60A0.9800
C205—N2011.524 (8)C601—H60B0.9800
C205—H20K0.9900C601—H60C0.9800
C205—H20L0.9900C601—H65A0.9800
C206—H20M0.9800C601—H65B0.9800
C206—H20N0.9800C601—H65C0.9800
C206—H20O0.9800N601—O6011.22 (2)
C207—C2081.487 (10)N601—O6021.234 (17)
C207—N2011.515 (7)N651—O6521.21 (3)
C207—H20P0.9900N651—O6511.23 (3)
C207—H20Q0.9900N1A—N2B1.142 (12)
C208—H20R0.9800N1A—N3A1.18 (2)
C208—H20S0.9800N1A—N3B1.187 (16)
C208—H20T0.9800N1A—N2A1.202 (17)
C301—C3021.497 (11)O1—V11.599 (3)
C301—N3011.504 (10)O2—V21.608 (3)
C301—H30A0.9900O3—V31.603 (4)
C301—H30B0.9900O4—V41.595 (4)
C351—C3021.436 (17)O5—V51.599 (3)
C351—N3011.523 (15)O6—V61.605 (3)
C351—H35A0.9900O7—V71.591 (3)
C351—H35B0.9900O8—V81.602 (3)
C302—H30C0.9800O9—V91.600 (3)
C302—H30D0.9800O10—V101.607 (3)
C302—H30E0.9800O11—V111.609 (3)
C302—H35C0.9800O12—V121.603 (3)
C302—H35D0.9800O13—V21.784 (3)
C302—H35E0.9800O13—V11.852 (3)
C303—C3041.409 (10)O14—V21.803 (4)
C303—N3011.591 (10)O14—V31.833 (3)
C303—H30F0.9900O15—V41.804 (4)
C303—H30G0.9900O15—V31.843 (4)
C353—N3011.463 (15)O16—V41.793 (3)
C353—C3041.528 (17)O16—V51.828 (4)
C353—H35F0.9900O17—V61.771 (4)
C353—H35G0.9900O17—V51.855 (3)
C304—H30H0.9800O18—V71.814 (3)
C304—H30I0.9800O18—V61.827 (3)
C304—H30J0.9800O19—V81.818 (4)
C304—H35H0.9800O19—V71.830 (3)
C304—H35I0.9800O20—V81.782 (3)
C304—H35J0.9800O20—V11.850 (3)
C305—N3011.509 (10)O21—V91.916 (3)
C305—C3061.528 (11)O21—V11.921 (3)
C305—H30K0.9900O21—V21.980 (3)
C305—H30L0.9900O22—V31.896 (3)
C355—C3061.441 (19)O22—V21.955 (3)
C355—N3011.583 (17)O22—V91.980 (3)
C355—H35K0.9900O23—V101.897 (3)
C355—H35L0.9900O23—V31.919 (3)
C306—H30M0.9800O23—V41.958 (3)
C306—H30N0.9800O24—V51.896 (3)
C306—H30O0.9800O24—V41.965 (3)
C306—H35M0.9800O24—V102.009 (3)
C306—H35N0.9800O25—V111.900 (3)
C306—H35O0.9800O25—V51.951 (3)
C307—N3011.486 (10)O25—V61.965 (3)
C307—C3081.491 (12)O26—V71.921 (3)
C307—H30P0.9900O26—V61.934 (3)
C307—H30Q0.9900O26—V111.979 (3)
C357—C3081.487 (18)O27—V121.898 (3)
C357—N3011.510 (16)O27—V71.938 (3)
C357—H35P0.9900O27—V81.943 (3)
C357—H35Q0.9900O28—V11.892 (3)
C308—H30R0.9800O28—V81.969 (3)
C308—H30S0.9800O28—V122.002 (3)
C308—H30T0.9800O29—V101.715 (3)
C308—H35R0.9800O29—V91.897 (3)
C308—H35S0.9800O30—V121.709 (3)
C308—H35T0.9800O30—V111.891 (3)
C401—C4021.501 (8)O31—V91.739 (3)
C401—N4011.517 (7)O31—V121.902 (3)
C401—H40A0.9900O32—V111.734 (3)
C401—H40B0.9900O32—V101.893 (3)
C402—H40C0.9800V1—V82.8249 (11)
C402—H40D0.9800V1—V22.8583 (11)
C402—H40E0.9800V2—V32.8429 (11)
C403—C4041.514 (9)V2—V93.0538 (11)
C403—N4011.517 (7)V3—V42.8732 (11)
C403—H40F0.9900V4—V52.8148 (11)
C403—H40G0.9900V4—V103.0516 (12)
C404—H40H0.9800V5—V62.8673 (11)
C404—H40I0.9800V6—V72.8470 (11)
C404—H40J0.9800V6—V113.0237 (11)
C405—C4061.507 (9)V7—V82.8738 (11)
C405—N4011.515 (7)V8—V123.0494 (11)
N101—C101—C102115.5 (4)C207—N201—C205105.5 (4)
N101—C101—H10A108.4C201—N201—C205110.5 (5)
C102—C101—H10A108.4C307—N301—C301112.1 (6)
N101—C101—H10B108.4C307—N301—C305110.0 (6)
C102—C101—H10B108.4C301—N301—C305112.2 (6)
H10A—C101—H10B107.5C353—N301—C357115.2 (11)
C101—C102—H10C109.5C353—N301—C351111.5 (9)
C101—C102—H10D109.5C357—N301—C351108.6 (9)
H10C—C102—H10D109.5C353—N301—C355106.7 (9)
C101—C102—H10E109.5C357—N301—C355106.9 (10)
H10C—C102—H10E109.5C351—N301—C355107.6 (9)
H10D—C102—H10E109.5C307—N301—C303109.1 (6)
C104—C103—N101115.8 (5)C301—N301—C303106.9 (5)
C104—C103—H10F108.3C305—N301—C303106.3 (5)
N101—C103—H10F108.3C407—N401—C405106.4 (4)
C104—C103—H10G108.3C407—N401—C401111.6 (4)
N101—C103—H10G108.3C405—N401—C401111.6 (4)
H10F—C103—H10G107.4C407—N401—C403111.6 (5)
C103—C104—H10H109.5C405—N401—C403110.1 (4)
C103—C104—H10I109.5C401—N401—C403105.6 (4)
H10H—C104—H10I109.5C507—N501—C505112.2 (4)
C103—C104—H10J109.5C507—N501—C501105.5 (4)
H10H—C104—H10J109.5C505—N501—C501110.7 (4)
H10I—C104—H10J109.5C507—N501—C503110.7 (4)
C106—C105—N101115.4 (5)C505—N501—C503106.5 (4)
C106—C105—H10K108.4C501—N501—C503111.3 (4)
N101—C105—H10K108.4V2—O13—V1103.61 (17)
C106—C105—H10L108.4V2—O14—V3102.88 (17)
N101—C105—H10L108.4V4—O15—V3103.98 (18)
H10K—C105—H10L107.5V4—O16—V5102.05 (18)
C105—C106—H10M109.5V6—O17—V5104.48 (17)
C105—C106—H10N109.5V7—O18—V6102.87 (17)
H10M—C106—H10N109.5V8—O19—V7103.97 (17)
C105—C106—H10O109.5V8—O20—V1102.10 (16)
H10M—C106—H10O109.5V9—O21—V1135.98 (18)
H10N—C106—H10O109.5V9—O21—V2103.21 (15)
N101—C107—C108115.4 (5)V1—O21—V294.22 (14)
N101—C107—H10P108.4V3—O22—V295.15 (15)
C108—C107—H10P108.4V3—O22—V9148.72 (19)
N101—C107—H10Q108.4V2—O22—V9101.80 (15)
C108—C107—H10Q108.4V10—O23—V3142.88 (18)
H10P—C107—H10Q107.5V10—O23—V4104.66 (15)
C107—C108—H10R109.5V3—O23—V495.65 (15)
C107—C108—H10S109.5V5—O24—V493.60 (15)
H10R—C108—H10S109.5V5—O24—V10141.04 (18)
C107—C108—H10T109.5V4—O24—V10100.34 (15)
H10R—C108—H10T109.5V11—O25—V5135.09 (19)
H10S—C108—H10T109.5V11—O25—V6102.93 (15)
C202—C201—N201116.4 (4)V5—O25—V694.15 (15)
C202—C201—H20A108.2V7—O26—V695.20 (15)
N201—C201—H20A108.2V7—O26—V11149.49 (18)
C202—C201—H20B108.2V6—O26—V11101.18 (15)
N201—C201—H20B108.2V12—O27—V7143.81 (18)
H20A—C201—H20B107.3V12—O27—V8105.10 (15)
C201—C202—H20C109.5V7—O27—V895.53 (15)
C201—C202—H20D109.5V1—O28—V894.03 (14)
H20C—C202—H20D109.5V1—O28—V12140.45 (18)
C201—C202—H20E109.5V8—O28—V12100.34 (14)
H20C—C202—H20E109.5V10—O29—V9154.5 (2)
H20D—C202—H20E109.5V12—O30—V11155.9 (2)
N201—C203—C204114.8 (5)V9—O31—V12130.24 (19)
N201—C203—H20F108.6V11—O32—V10130.24 (18)
C204—C203—H20F108.6O1—V1—O20104.68 (16)
N201—C203—H20G108.6O1—V1—O13105.80 (17)
C204—C203—H20G108.6O20—V1—O1391.23 (15)
H20F—C203—H20G107.5O1—V1—O28104.45 (17)
C203—C204—H20H109.5O20—V1—O2881.49 (14)
C203—C204—H20I109.5O13—V1—O28149.74 (15)
H20H—C204—H20I109.5O1—V1—O21103.55 (16)
C203—C204—H20J109.5O20—V1—O21151.75 (15)
H20H—C204—H20J109.5O13—V1—O2179.98 (14)
H20I—C204—H20J109.5O28—V1—O2192.64 (14)
C206—C205—N201115.6 (5)O1—V1—V8115.05 (13)
C206—C205—H20K108.4O20—V1—V838.09 (10)
N201—C205—H20K108.4O13—V1—V8119.87 (12)
C206—C205—H20L108.4O28—V1—V844.06 (10)
N201—C205—H20L108.4O21—V1—V8126.54 (10)
H20K—C205—H20L107.4O1—V1—V2116.52 (13)
C205—C206—H20M109.5O20—V1—V2119.31 (11)
C205—C206—H20N109.5O13—V1—V237.35 (10)
H20M—C206—H20N109.5O28—V1—V2124.23 (10)
C205—C206—H20O109.5O21—V1—V243.69 (10)
H20M—C206—H20O109.5V8—V1—V2128.03 (4)
H20N—C206—H20O109.5O2—V2—O13105.89 (17)
C208—C207—N201115.9 (5)O2—V2—O14105.56 (17)
C208—C207—H20P108.3O13—V2—O14104.97 (16)
N201—C207—H20P108.3O2—V2—O22105.83 (16)
C208—C207—H20Q108.3O13—V2—O22144.89 (15)
N201—C207—H20Q108.3O14—V2—O2280.45 (15)
H20P—C207—H20Q107.4O2—V2—O21106.29 (16)
C207—C208—H20R109.5O13—V2—O2180.06 (14)
C207—C208—H20S109.5O14—V2—O21144.87 (15)
H20R—C208—H20S109.5O22—V2—O2176.98 (13)
C207—C208—H20T109.5O2—V2—V3108.26 (13)
H20R—C208—H20T109.5O13—V2—V3135.90 (12)
H20S—C208—H20T109.5O14—V2—V338.94 (11)
C302—C301—N301118.1 (7)O22—V2—V341.64 (10)
C302—C301—H30A107.8O21—V2—V3115.20 (10)
N301—C301—H30A107.8O2—V2—V1118.40 (13)
C302—C301—H30B107.8O13—V2—V139.04 (11)
N301—C301—H30B107.8O14—V2—V1127.93 (12)
H30A—C301—H30B107.1O22—V2—V1110.54 (10)
C302—C351—N301120.9 (11)O21—V2—V142.10 (10)
C302—C351—H35A107.1V3—V2—V1131.96 (4)
N301—C351—H35A107.1O2—V2—V9112.65 (13)
C302—C351—H35B107.1O13—V2—V9112.63 (11)
N301—C351—H35B107.1O14—V2—V9114.39 (11)
H35A—C351—H35B106.8O22—V2—V939.41 (10)
C301—C302—H30C109.5O21—V2—V937.65 (9)
C301—C302—H30D109.5V3—V2—V978.47 (3)
H30C—C302—H30D109.5V1—V2—V973.92 (3)
C301—C302—H30E109.5O3—V3—O14106.61 (17)
H30C—C302—H30E109.5O3—V3—O15106.11 (18)
H30D—C302—H30E109.5O14—V3—O1594.24 (16)
C351—C302—H35C109.5O3—V3—O22106.23 (17)
C351—C302—H35D109.5O14—V3—O2281.28 (15)
H35C—C302—H35D109.5O15—V3—O22147.26 (16)
C351—C302—H35E109.5O3—V3—O23103.17 (17)
H35C—C302—H35E109.5O14—V3—O23150.07 (15)
H35D—C302—H35E109.5O15—V3—O2380.13 (15)
C304—C303—N301116.1 (6)O22—V3—O2387.78 (14)
C304—C303—H30F108.3O3—V3—V2109.35 (13)
N301—C303—H30F108.3O14—V3—V238.19 (11)
C304—C303—H30G108.3O15—V3—V2126.84 (12)
N301—C303—H30G108.3O22—V3—V243.22 (10)
H30F—C303—H30G107.4O23—V3—V2126.55 (10)
N301—C353—C304116.8 (10)O3—V3—V4107.20 (13)
N301—C353—H35F108.1O14—V3—V4127.18 (11)
C304—C353—H35F108.1O15—V3—V437.53 (11)
N301—C353—H35G108.1O22—V3—V4124.99 (10)
C304—C353—H35G108.1O23—V3—V442.70 (10)
H35F—C353—H35G107.3V2—V3—V4143.43 (4)
C303—C304—H30H109.5O4—V4—O16106.28 (17)
C303—C304—H30I109.5O4—V4—O15107.90 (18)
H30H—C304—H30I109.5O16—V4—O15102.80 (17)
C303—C304—H30J109.5O4—V4—O23104.54 (17)
H30H—C304—H30J109.5O16—V4—O23146.34 (15)
H30I—C304—H30J109.5O15—V4—O2380.04 (15)
C353—C304—H35H109.5O4—V4—O24106.74 (17)
C353—C304—H35I109.5O16—V4—O2481.27 (15)
H35H—C304—H35I109.5O15—V4—O24142.24 (15)
C353—C304—H35J109.5O23—V4—O2477.18 (14)
H35H—C304—H35J109.5O4—V4—V5116.36 (13)
H35I—C304—H35J109.5O16—V4—V539.43 (12)
N301—C305—C306115.3 (7)O15—V4—V5127.43 (12)
N301—C305—H30K108.4O23—V4—V5112.83 (10)
C306—C305—H30K108.4O24—V4—V542.23 (10)
N301—C305—H30L108.4O4—V4—V3109.28 (13)
C306—C305—H30L108.4O16—V4—V3134.03 (12)
H30K—C305—H30L107.5O15—V4—V338.49 (11)
C306—C355—N301116.0 (11)O23—V4—V341.65 (10)
C306—C355—H35K108.3O24—V4—V3114.29 (10)
N301—C355—H35K108.3V5—V4—V3133.02 (4)
C306—C355—H35L108.3O4—V4—V10112.68 (14)
N301—C355—H35L108.3O16—V4—V10116.01 (12)
H35K—C355—H35L107.4O15—V4—V10110.45 (12)
C305—C306—H30M109.5O23—V4—V1036.97 (10)
C305—C306—H30N109.5O24—V4—V1040.36 (10)
H30M—C306—H30N109.5V5—V4—V1077.61 (3)
C305—C306—H30O109.5V3—V4—V1075.19 (3)
H30M—C306—H30O109.5O5—V5—O16105.55 (18)
H30N—C306—H30O109.5O5—V5—O17105.57 (18)
C355—C306—H35M109.5O16—V5—O1792.84 (16)
C355—C306—H35N109.5O5—V5—O24103.62 (17)
H35M—C306—H35N109.5O16—V5—O2482.30 (15)
C355—C306—H35O109.5O17—V5—O24150.64 (15)
H35M—C306—H35O109.5O5—V5—O25103.29 (17)
H35N—C306—H35O109.5O16—V5—O25151.15 (15)
N301—C307—C308118.5 (7)O17—V5—O2578.80 (15)
N301—C307—H30P107.7O24—V5—O2591.56 (14)
C308—C307—H30P107.7O5—V5—V4114.03 (14)
N301—C307—H30Q107.7O16—V5—V438.53 (11)
C308—C307—H30Q107.7O17—V5—V4122.72 (12)
H30P—C307—H30Q107.1O24—V5—V444.17 (10)
C308—C357—N301117.1 (11)O25—V5—V4126.32 (10)
C308—C357—H35P108.0O5—V5—V6115.91 (14)
N301—C357—H35P108.0O16—V5—V6119.98 (12)
C308—C357—H35Q108.0O17—V5—V636.73 (11)
N301—C357—H35Q108.0O24—V5—V6123.82 (10)
H35P—C357—H35Q107.3O25—V5—V643.12 (10)
C307—C308—H30R109.5V4—V5—V6129.88 (4)
C307—C308—H30S109.5O6—V6—O17107.11 (17)
H30R—C308—H30S109.5O6—V6—O18106.74 (16)
C307—C308—H30T109.5O17—V6—O18102.32 (16)
H30R—C308—H30T109.5O6—V6—O26106.94 (16)
H30S—C308—H30T109.5O17—V6—O26143.26 (15)
C357—C308—H35R109.5O18—V6—O2680.56 (14)
C357—C308—H35S109.5O6—V6—O25105.28 (16)
H35R—C308—H35S109.5O17—V6—O2580.43 (15)
C357—C308—H35T109.5O18—V6—O25145.32 (15)
H35R—C308—H35T109.5O26—V6—O2577.71 (14)
H35S—C308—H35T109.5O6—V6—V7110.52 (13)
C402—C401—N401115.2 (5)O17—V6—V7131.88 (12)
C402—C401—H40A108.5O18—V6—V738.40 (11)
N401—C401—H40A108.5O26—V6—V742.23 (10)
C402—C401—H40B108.5O25—V6—V7116.08 (10)
N401—C401—H40B108.5O6—V6—V5118.72 (13)
H40A—C401—H40B107.5O17—V6—V538.79 (11)
C401—C402—H40C109.5O18—V6—V5125.77 (11)
C401—C402—H40D109.5O26—V6—V5110.37 (10)
H40C—C402—H40D109.5O25—V6—V542.73 (10)
C401—C402—H40E109.5V7—V6—V5129.84 (4)
H40C—C402—H40E109.5O6—V6—V11111.68 (13)
H40D—C402—H40E109.5O17—V6—V11112.70 (11)
C404—C403—N401114.7 (5)O18—V6—V11115.53 (11)
C404—C403—H40F108.6O26—V6—V1139.96 (10)
N401—C403—H40F108.6O25—V6—V1137.77 (10)
C404—C403—H40G108.6V7—V6—V1179.68 (3)
N401—C403—H40G108.6V5—V6—V1174.28 (3)
H40F—C403—H40G107.6O7—V7—O18104.66 (17)
C403—C404—H40H109.5O7—V7—O19105.52 (17)
C403—C404—H40I109.5O18—V7—O1998.05 (16)
H40H—C404—H40I109.5O7—V7—O26106.57 (16)
C403—C404—H40J109.5O18—V7—O2681.23 (15)
H40H—C404—H40J109.5O19—V7—O26146.97 (15)
H40I—C404—H40J109.5O7—V7—O27102.26 (16)
C406—C405—N401115.8 (5)O18—V7—O27152.50 (15)
C406—C405—H40K108.3O19—V7—O2779.97 (15)
N401—C405—H40K108.3O26—V7—O2785.82 (14)
C406—C405—H40L108.3O7—V7—V6108.90 (13)
N401—C405—H40L108.3O18—V7—V638.73 (11)
H40K—C405—H40L107.4O19—V7—V6130.00 (12)
C405—C406—H40M109.5O26—V7—V642.57 (10)
C405—C406—H40N109.5O27—V7—V6124.99 (10)
H40M—C406—H40N109.5O7—V7—V8105.24 (13)
C405—C406—H40O109.5O18—V7—V8132.15 (11)
H40M—C406—H40O109.5O19—V7—V837.87 (11)
H40N—C406—H40O109.5O26—V7—V8123.56 (10)
N401—C407—C408115.6 (5)O27—V7—V842.30 (10)
N401—C407—H40P108.4V6—V7—V8145.76 (4)
C408—C407—H40P108.4O8—V8—O20105.61 (17)
N401—C407—H40Q108.4O8—V8—O19107.97 (18)
C408—C407—H40Q108.4O20—V8—O19102.98 (16)
H40P—C407—H40Q107.5O8—V8—O27104.74 (16)
C407—C408—H40R109.5O20—V8—O27146.71 (14)
C407—C408—H40S109.5O19—V8—O2780.13 (15)
H40R—C408—H40S109.5O8—V8—O28107.54 (17)
C407—C408—H40T109.5O20—V8—O2881.07 (14)
H40R—C408—H40T109.5O19—V8—O28141.56 (15)
H40S—C408—H40T109.5O27—V8—O2877.06 (13)
C502—C501—N501114.8 (4)O8—V8—V1117.67 (13)
C502—C501—H50A108.6O20—V8—V139.81 (11)
N501—C501—H50A108.6O19—V8—V1126.25 (12)
C502—C501—H50B108.6O27—V8—V1111.99 (10)
N501—C501—H50B108.6O28—V8—V141.91 (9)
H50A—C501—H50B107.5O8—V8—V7108.55 (13)
C501—C502—H50C109.5O20—V8—V7134.77 (12)
C501—C502—H50D109.5O19—V8—V738.17 (11)
H50C—C502—H50D109.5O27—V8—V742.17 (10)
C501—C502—H50E109.5O28—V8—V7114.79 (10)
H50C—C502—H50E109.5V1—V8—V7132.58 (4)
H50D—C502—H50E109.5O8—V8—V12112.82 (14)
N501—C503—C504115.5 (4)O20—V8—V12116.24 (11)
N501—C503—H50F108.4O19—V8—V12110.49 (11)
C504—C503—H50F108.4O27—V8—V1236.93 (10)
N501—C503—H50G108.4O28—V8—V1240.22 (9)
C504—C503—H50G108.4V1—V8—V1277.07 (3)
H50F—C503—H50G107.5V7—V8—V1275.92 (3)
C503—C504—H50H109.5O9—V9—O31103.99 (17)
C503—C504—H50I109.5O9—V9—O29104.20 (17)
H50H—C504—H50I109.5O31—V9—O2993.49 (15)
C503—C504—H50J109.5O9—V9—O21104.14 (16)
H50H—C504—H50J109.5O31—V9—O2191.78 (15)
H50I—C504—H50J109.5O29—V9—O21148.95 (15)
C506—C505—N501114.6 (5)O9—V9—O22102.33 (16)
C506—C505—H50K108.6O31—V9—O22153.36 (15)
N501—C505—H50K108.6O29—V9—O2283.95 (14)
C506—C505—H50L108.6O21—V9—O2277.84 (14)
N501—C505—H50L108.6O9—V9—V2109.09 (13)
H50K—C505—H50L107.6O31—V9—V2125.57 (11)
C505—C506—H50M109.5O29—V9—V2117.75 (11)
C505—C506—H50N109.5O21—V9—V239.13 (10)
H50M—C506—H50N109.5O22—V9—V238.80 (9)
C505—C506—H50O109.5O10—V10—O29105.67 (18)
H50M—C506—H50O109.5O10—V10—O32101.21 (16)
H50N—C506—H50O109.5O29—V10—O3295.62 (15)
C508—C507—N501115.2 (4)O10—V10—O23101.36 (16)
C508—C507—H50P108.5O29—V10—O2391.78 (15)
N501—C507—H50P108.5O32—V10—O23153.34 (15)
C508—C507—H50Q108.5O10—V10—O24102.55 (16)
N501—C507—H50Q108.5O29—V10—O24151.30 (16)
H50P—C507—H50Q107.5O32—V10—O2483.88 (14)
C507—C508—H50R109.5O23—V10—O2477.53 (14)
C507—C508—H50S109.5O10—V10—V4107.99 (14)
H50R—C508—H50S109.5O29—V10—V4123.76 (12)
C507—C508—H50T109.5O32—V10—V4119.73 (11)
H50R—C508—H50T109.5O23—V10—V438.37 (10)
H50S—C508—H50T109.5O24—V10—V439.31 (10)
N601—C601—H60A109.5O11—V11—O32104.18 (17)
N601—C601—H60B109.5O11—V11—O30103.88 (17)
H60A—C601—H60B109.5O32—V11—O3093.31 (15)
N601—C601—H60C109.5O11—V11—O25104.37 (17)
H60A—C601—H60C109.5O32—V11—O2592.27 (15)
H60B—C601—H60C109.5O30—V11—O25148.86 (15)
N651—C601—H65A109.5O11—V11—O26102.10 (16)
N651—C601—H65B109.5O32—V11—O26153.53 (15)
H65A—C601—H65B109.5O30—V11—O2683.38 (14)
N651—C601—H65C109.5O25—V11—O2678.15 (14)
H65A—C601—H65C109.5O11—V11—V6107.98 (13)
H65B—C601—H65C109.5O32—V11—V6126.76 (12)
O601—N601—O602123.4 (14)O30—V11—V6117.89 (11)
O601—N601—C601120.9 (12)O25—V11—V639.30 (10)
O602—N601—C601115.4 (12)O26—V11—V638.86 (10)
O652—N651—O651121 (3)O12—V12—O30105.32 (17)
O652—N651—C601121 (2)O12—V12—O27102.29 (17)
O651—N651—C601117 (2)O30—V12—O2791.63 (15)
N2B—N1A—N3B170.5 (10)O12—V12—O31101.44 (16)
N3A—N1A—N2A172.6 (10)O30—V12—O3195.11 (15)
C107—N101—C101111.7 (4)O27—V12—O31152.62 (15)
C107—N101—C103111.3 (4)O12—V12—O28103.58 (16)
C101—N101—C103105.7 (4)O30—V12—O28150.66 (16)
C107—N101—C105106.2 (4)O27—V12—O2877.32 (13)
C101—N101—C105110.9 (4)O31—V12—O2884.01 (14)
C103—N101—C105111.0 (5)O12—V12—V8108.74 (13)
C203—N201—C207112.8 (5)O30—V12—V8123.39 (12)
C203—N201—C201105.7 (4)O27—V12—V837.97 (10)
C207—N201—C201110.9 (4)O31—V12—V8119.94 (10)
C203—N201—C205111.5 (5)O28—V12—V839.44 (9)
N301—C351_f—C302—C301_e14.8 (9)V3—O14—V2—O223.95 (16)
N301—C301—C302—C35114.5 (9)V3—O14—V2—O2154.4 (3)
N301—C303—C304—C3530.4 (9)V3—O14—V2—V1112.60 (14)
N301—C353—C304—C3030.4 (9)V3—O14—V2—V924.46 (19)
N301—C355—C306—C30516.4 (9)V2—O14—V3—O3100.4 (2)
N301—C305—C306—C35517.1 (9)V2—O14—V3—O15151.41 (17)
N301—C357—C308—C30711.8 (10)V2—O14—V3—O224.06 (16)
N301—C307—C308—C35712.1 (10)V2—O14—V3—O2373.9 (3)
N651—C601—N601—O60177 (3)V2—O14—V3—V4131.78 (11)
N651—C601—N601—O602108 (4)V4—O15—V3—O397.4 (2)
N601—C601—N651—O65291 (4)V4—O15—V3—O14153.93 (18)
N601—C601—N651—O65191 (4)V4—O15—V3—O2273.5 (3)
C108—C107—N101—C10154.3 (7)V4—O15—V3—O233.56 (17)
C108—C107—N101—C10363.6 (7)V4—O15—V3—V2132.24 (12)
C108—C107—N101—C105175.5 (5)V2—O22—V3—O3101.20 (17)
C102—C101—N101—C10761.4 (6)V9—O22—V3—O3135.9 (4)
C102—C101—N101—C103177.4 (5)V2—O22—V3—O143.67 (14)
C102—C101—N101—C10557.0 (6)V9—O22—V3—O14119.3 (4)
C104—C103—N101—C10761.2 (8)V2—O22—V3—O1587.9 (3)
C104—C103—N101—C101177.4 (7)V9—O22—V3—O1535.0 (5)
C104—C103—N101—C10557.0 (8)V2—O22—V3—O23155.73 (15)
C106—C105—N101—C107179.9 (5)V9—O22—V3—O2332.8 (4)
C106—C105—N101—C10158.3 (6)V9—O22—V3—V2122.9 (4)
C106—C105—N101—C10358.9 (6)V2—O22—V3—V4133.38 (9)
C204—C203—N201—C20760.6 (7)V9—O22—V3—V410.4 (4)
C204—C203—N201—C201178.1 (5)V5—O16—V4—O4111.91 (19)
C204—C203—N201—C20557.9 (7)V5—O16—V4—O15134.84 (17)
C208—C207—N201—C20352.0 (7)V5—O16—V4—O2343.6 (3)
C208—C207—N201—C20166.4 (7)V5—O16—V4—O246.92 (16)
C208—C207—N201—C205174.0 (6)V5—O16—V4—V3108.57 (16)
C202—C201—N201—C203173.3 (5)V5—O16—V4—V1014.20 (19)
C202—C201—N201—C20764.1 (7)V3—O15—V4—O498.7 (2)
C202—C201—N201—C20552.5 (6)V3—O15—V4—O16149.25 (17)
C206—C205—N201—C20358.8 (7)V3—O15—V4—O233.49 (16)
C206—C205—N201—C207178.4 (6)V3—O15—V4—O2457.0 (3)
C206—C205—N201—C20158.5 (7)V3—O15—V4—V5114.70 (15)
C304—C353—N301—C307119.8 (13)V3—O15—V4—V1024.87 (19)
C304—C353—N301—C30126 (5)V4—O16—V5—O5109.21 (19)
C304—C353—N301—C305122.8 (13)V4—O16—V5—O17143.76 (17)
C304—C353—N301—C35770.4 (14)V4—O16—V5—O247.15 (16)
C304—C353—N301—C35153.9 (15)V4—O16—V5—O2572.0 (4)
C304—C353—N301—C355171.1 (12)V4—O16—V5—V6117.62 (13)
C304—C353—N301—C3030.4 (9)V6—O17—V5—O5112.6 (2)
C308—C307—N301—C353116.1 (11)V6—O17—V5—O16140.36 (18)
C308—C307—N301—C30156.6 (10)V6—O17—V5—O2461.0 (4)
C308—C307—N301—C305177.8 (8)V6—O17—V5—O2511.79 (16)
C308—C307—N301—C35712.0 (10)V6—O17—V5—V4114.40 (14)
C308—C307—N301—C35132 (5)V4—O24—V5—O5110.60 (17)
C308—C307—N301—C355132.4 (11)V10—O24—V5—O5138.1 (3)
C308—C307—N301—C30361.6 (9)V4—O24—V5—O166.39 (15)
C302—C301—N301—C35345 (4)V10—O24—V5—O16117.7 (3)
C302—C301—N301—C307171.4 (7)V4—O24—V5—O1775.7 (3)
C302—C301—N301—C30547.1 (9)V10—O24—V5—O1735.7 (5)
C302—C301—N301—C357146.7 (10)V4—O24—V5—O25145.32 (14)
C302—C301—N301—C35114.0 (9)V10—O24—V5—O2534.0 (3)
C302—C301—N301—C355101.7 (9)V10—O24—V5—V4111.3 (3)
C302—C301—N301—C30369.1 (8)V4—O24—V5—V6114.70 (11)
C306—C305—N301—C353140.8 (10)V10—O24—V5—V63.4 (4)
C306—C305—N301—C30773.3 (8)V5—O17—V6—O6114.81 (19)
C306—C305—N301—C30152.2 (9)V5—O17—V6—O18133.12 (17)
C306—C305—N301—C35731 (4)V5—O17—V6—O2642.4 (3)
C306—C305—N301—C351101.1 (9)V5—O17—V6—O2511.64 (16)
C306—C305—N301—C35515.9 (9)V5—O17—V6—V7104.95 (16)
C306—C305—N301—C303168.7 (6)V5—O17—V6—V118.4 (2)
C308—C357—N301—C35346.3 (16)V7—O18—V6—O6102.11 (19)
C308—C357—N301—C30711.9 (10)V7—O18—V6—O17145.54 (16)
C308—C357—N301—C301146.8 (15)V7—O18—V6—O262.87 (15)
C308—C357—N301—C30558 (5)V7—O18—V6—O2554.6 (3)
C308—C357—N301—C351172.2 (12)V7—O18—V6—V5111.24 (14)
C308—C357—N301—C35572.0 (15)V7—O18—V6—V1122.73 (18)
C308—C357—N301—C303102.8 (13)V6—O18—V7—O7102.07 (19)
C302—C351—N301—C353171.6 (12)V6—O18—V7—O19149.48 (16)
C302—C351—N301—C30742 (5)V6—O18—V7—O262.88 (15)
C302—C351—N301—C30115.0 (9)V6—O18—V7—O2765.8 (4)
C302—C351—N301—C305109.6 (12)V6—O18—V7—V8130.82 (11)
C302—C351—N301—C35760.5 (15)V8—O19—V7—O795.0 (2)
C302—C351—N301—C35554.9 (14)V8—O19—V7—O18157.26 (17)
C302—C351—N301—C303139.4 (13)V8—O19—V7—O2671.0 (3)
C306—C355—N301—C35369.9 (14)V8—O19—V7—O275.05 (16)
C306—C355—N301—C307141.6 (13)V8—O19—V7—V6132.76 (12)
C306—C355—N301—C301103.1 (12)V1—O20—V8—O8114.70 (19)
C306—C355—N301—C30517.0 (9)V1—O20—V8—O19132.16 (17)
C306—C355—N301—C357166.4 (12)V1—O20—V8—O2740.4 (3)
C306—C355—N301—C35149.9 (14)V1—O20—V8—O288.87 (15)
C306—C355—N301—C30336 (4)V1—O20—V8—V7107.36 (16)
C304—C303—N301—C3530.4 (9)V1—O20—V8—V1211.22 (19)
C304—C303—N301—C30764.6 (8)V7—O19—V8—O897.4 (2)
C304—C303—N301—C301173.9 (6)V7—O19—V8—O20151.20 (17)
C304—C303—N301—C30553.9 (8)V7—O19—V8—O275.03 (16)
C304—C303—N301—C357121.8 (9)V7—O19—V8—O2859.2 (3)
C304—C303—N301—C351127.0 (9)V7—O19—V8—V1115.14 (14)
C304—C303—N301—C35537 (3)V7—O19—V8—V1226.42 (19)
C408—C407—N401—C405175.4 (5)V12—O31—V9—O9178.9 (2)
C408—C407—N401—C40162.6 (6)V12—O31—V9—O2973.4 (2)
C408—C407—N401—C40355.3 (6)V12—O31—V9—O2176.0 (2)
C406—C405—N401—C407178.8 (5)V12—O31—V9—O2210.1 (5)
C406—C405—N401—C40159.3 (6)V12—O31—V9—V254.7 (3)
C406—C405—N401—C40357.7 (6)V10—O29—V9—O9131.5 (5)
C402—C401—N401—C40756.3 (6)V10—O29—V9—O31123.1 (5)
C402—C401—N401—C40562.7 (6)V10—O29—V9—O2123.8 (7)
C402—C401—N401—C403177.7 (5)V10—O29—V9—O2230.2 (5)
C404—C403—N401—C40752.8 (6)V10—O29—V9—V210.5 (5)
C404—C403—N401—C40565.1 (6)V9—O29—V10—O10133.6 (5)
C404—C403—N401—C401174.2 (5)V9—O29—V10—O32123.1 (5)
C508—C507—N501—C50559.7 (6)V9—O29—V10—O2331.3 (5)
C508—C507—N501—C501179.6 (5)V9—O29—V10—O2435.6 (7)
C508—C507—N501—C50359.2 (6)V9—O29—V10—V48.6 (6)
C506—C505—N501—C50756.4 (6)V11—O32—V10—O10175.9 (2)
C506—C505—N501—C50161.2 (6)V11—O32—V10—O2976.8 (3)
C506—C505—N501—C503177.6 (5)V11—O32—V10—O2328.6 (5)
C502—C501—N501—C507177.6 (5)V11—O32—V10—O2474.3 (2)
C502—C501—N501—C50556.0 (6)V11—O32—V10—V457.5 (3)
C502—C501—N501—C50362.3 (6)V3—O23—V10—O10134.4 (3)
C504—C503—N501—C50758.1 (6)V4—O23—V10—O10104.69 (18)
C504—C503—N501—C505179.7 (5)V3—O23—V10—O2928.0 (3)
C504—C503—N501—C50158.9 (6)V4—O23—V10—O29148.94 (17)
V8—O20—V1—O1112.04 (18)V3—O23—V10—O3278.3 (4)
V8—O20—V1—O13141.27 (17)V4—O23—V10—O3242.7 (4)
V8—O20—V1—O289.23 (16)V3—O23—V10—O24125.1 (3)
V8—O20—V1—O2170.4 (4)V4—O23—V10—O244.18 (14)
V8—O20—V1—V2115.40 (13)V3—O23—V10—V4121.0 (4)
V2—O13—V1—O1113.21 (19)V10—O32—V11—O11177.7 (2)
V2—O13—V1—O20141.16 (18)V10—O32—V11—O3072.5 (3)
V2—O13—V1—O2866.1 (3)V10—O32—V11—O2576.9 (2)
V2—O13—V1—O2111.83 (16)V10—O32—V11—O269.3 (5)
V2—O13—V1—V8114.74 (14)V10—O32—V11—V656.4 (3)
V8—O28—V1—O1111.24 (17)V12—O30—V11—O11127.0 (5)
V12—O28—V1—O1137.2 (3)V12—O30—V11—O32127.5 (5)
V8—O28—V1—O208.18 (14)V12—O30—V11—O2527.6 (7)
V12—O28—V1—O20119.8 (3)V12—O30—V11—O2626.1 (5)
V8—O28—V1—O1369.5 (3)V12—O30—V11—V67.6 (6)
V12—O28—V1—O1342.1 (5)V11—O30—V12—O12129.4 (5)
V8—O28—V1—O21144.04 (14)V11—O30—V12—O2726.2 (5)
V12—O28—V1—O2132.5 (3)V11—O30—V12—O31127.2 (5)
V12—O28—V1—V8111.6 (3)V11—O30—V12—O2840.4 (7)
V8—O28—V1—V2111.62 (11)V11—O30—V12—V84.0 (6)
V12—O28—V1—V20.0 (3)V7—O27—V12—O12132.7 (3)
V1—O13—V2—O2115.72 (19)V8—O27—V12—O12104.80 (18)
V1—O13—V2—O14132.89 (17)V7—O27—V12—O3026.6 (3)
V1—O13—V2—O2238.2 (3)V8—O27—V12—O30149.14 (17)
V1—O13—V2—O2111.47 (16)V7—O27—V12—O3177.8 (4)
V1—O13—V2—V3104.66 (17)V8—O27—V12—O3144.7 (4)
V1—O13—V2—V97.82 (19)V7—O27—V12—O28126.0 (3)
V3—O14—V2—O299.95 (19)V8—O27—V12—O283.42 (15)
V3—O14—V2—O13148.41 (16)V7—O27—V12—V8122.5 (4)
Heptaammonium azidotetradecavanadate dimethyl sulfoxide hexasolvate (2) top
Crystal data top
(NH4)7[V14O38(N3)]·6C2H6OSF(000) = 3904
Mr = 1958.25Dx = 2.089 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71075 Å
a = 19.272 (3) ÅCell parameters from 13563 reflections
b = 24.785 (3) Åθ = 1.6–13.8°
c = 14.552 (4) ŵ = 2.30 mm1
β = 116.387 (15)°T = 83 K
V = 6227 (2) Å3Block, red
Z = 40.20 × 0.20 × 0.20 mm
Data collection top
Rigaku Mercury70
diffractometer
6292 reflections with I > 2σ(I)
Detector resolution: 14.629 pixels mm-1Rint = 0.034
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: numerical
(NUMABS; Rigaku, 1999)
h = 2520
Tmin = 0.501, Tmax = 0.631k = 3132
33352 measured reflectionsl = 1518
7051 independent reflections
Refinement top
Refinement on F214 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.036H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.098 w = 1/[σ2(Fo2) + (0.0513P)2 + 19.2144P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
7051 reflectionsΔρmax = 1.07 e Å3
446 parametersΔρmin = 0.91 e Å3
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C1010.28101 (19)0.96267 (16)0.8402 (3)0.0357 (8)
H10A0.22940.94700.80090.054*
H10B0.30970.94120.90230.054*
H10C0.27580.99980.85940.054*
C1020.2773 (2)1.01291 (13)0.6731 (3)0.0357 (8)
H10D0.22630.99840.62670.054*
H10E0.27071.04450.70910.054*
H10F0.30491.02360.63340.054*
C2010.18451 (19)0.69520 (15)0.9394 (3)0.0322 (7)
H20A0.18790.73210.91770.048*
H20B0.19600.69511.01210.048*
H20C0.22200.67230.92930.048*
C2020.04072 (18)0.70993 (13)0.9199 (2)0.0257 (6)
H20D0.03880.74750.89780.039*
H20E0.01210.69630.89690.039*
H20F0.06850.70800.99490.039*
C3010.3274 (2)0.40411 (18)0.5397 (3)0.0441 (9)
H30A0.31040.38020.57940.066*
H30B0.29170.43480.51390.066*
H30C0.32760.38410.48170.066*
C3020.4729 (2)0.36707 (14)0.6277 (3)0.0340 (7)
H30D0.46330.34150.67220.051*
H30E0.45530.35130.55920.051*
H30F0.52840.37480.65670.051*
N1A0.25489 (16)0.72352 (12)0.5701 (2)0.0315 (6)
N2A0.25000.75000.50000.0211 (7)
N10.55738 (14)0.75064 (10)0.90881 (19)0.0168 (5)
N20.52456 (15)0.55703 (12)0.6140 (2)0.0247 (5)
N30.00337 (15)0.57391 (10)0.9919 (2)0.0192 (5)
N40.00000.53901 (15)0.75000.0245 (8)
O10.39611 (11)0.84816 (8)0.84735 (15)0.0198 (4)
O20.40679 (12)0.69131 (8)0.91862 (15)0.0215 (4)
O30.36740 (11)0.54570 (8)0.65899 (15)0.0191 (4)
O40.13152 (11)0.92400 (8)0.61245 (15)0.0187 (4)
O50.15934 (12)0.80703 (8)0.80009 (15)0.0204 (4)
O60.12684 (11)0.61075 (8)0.70025 (15)0.0179 (4)
O80.40231 (10)0.75246 (8)0.76046 (14)0.0160 (4)
O90.40226 (11)0.63065 (8)0.56668 (14)0.0167 (4)
O100.35958 (10)0.84207 (8)0.64328 (15)0.0173 (4)
O110.37830 (11)0.64494 (8)0.73385 (15)0.0175 (4)
O120.28829 (11)0.76176 (7)0.79023 (14)0.0158 (4)
O130.26785 (10)0.60429 (7)0.47358 (14)0.0149 (4)
O140.26680 (11)0.65844 (7)0.78119 (14)0.0160 (4)
O150.24247 (10)0.84168 (7)0.68867 (14)0.0156 (4)
O160.23494 (10)0.60680 (7)0.61444 (14)0.0147 (4)
O170.14750 (11)0.71781 (8)0.68567 (15)0.0173 (4)
O180.12314 (11)0.55947 (8)0.42881 (16)0.0206 (4)
O190.10937 (10)0.81397 (8)0.59330 (15)0.0167 (4)
O200.11130 (10)0.65201 (7)0.52075 (14)0.0147 (4)
O1010.41072 (12)0.98792 (8)0.83454 (16)0.0222 (4)
O2010.08979 (13)0.61273 (8)0.90413 (17)0.0246 (4)
O3010.44037 (16)0.46371 (10)0.5490 (2)0.0369 (6)
S1010.33171 (4)0.96259 (3)0.76434 (5)0.02078 (15)
S2010.08981 (4)0.66995 (3)0.86548 (5)0.01940 (15)
S3010.42139 (5)0.42786 (3)0.61872 (7)0.03002 (18)
V10.34650 (2)0.81247 (2)0.74752 (3)0.01367 (10)
V20.34907 (3)0.69858 (2)0.79970 (3)0.01470 (11)
V30.33743 (3)0.60611 (2)0.62210 (3)0.01393 (10)
V40.15833 (3)0.87196 (2)0.57127 (3)0.01360 (10)
V50.18223 (3)0.78515 (2)0.71331 (3)0.01385 (10)
V60.17553 (3)0.65064 (2)0.66441 (3)0.01410 (10)
V70.16743 (2)0.61587 (2)0.46699 (3)0.01405 (10)
H10.568 (2)0.7245 (11)0.953 (2)0.023 (9)*
H20.5075 (11)0.7532 (15)0.869 (2)0.029 (10)*
H30.574 (2)0.7433 (15)0.865 (2)0.025 (9)*
H40.573 (2)0.7796 (11)0.945 (3)0.037 (11)*
H50.560 (3)0.557 (3)0.679 (2)0.11 (2)*
H60.542 (2)0.5576 (16)0.565 (2)0.031 (10)*
H70.4995 (16)0.5265 (9)0.604 (2)0.008 (7)*
H80.4920 (19)0.5847 (12)0.601 (3)0.035 (10)*
H90.0277 (16)0.5881 (13)0.969 (2)0.016 (8)*
H100.0206 (18)0.5560 (12)1.0481 (18)0.020 (8)*
H110.0323 (18)0.5986 (12)1.000 (3)0.027 (9)*
H120.0341 (17)0.5506 (11)0.947 (2)0.020 (8)*
H130.023 (2)0.5189 (14)0.778 (3)0.042 (11)*
H140.0347 (16)0.5591 (13)0.703 (2)0.026 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1010.0238 (16)0.053 (2)0.0320 (18)0.0039 (15)0.0142 (14)0.0093 (16)
C1020.0302 (17)0.0222 (16)0.0336 (19)0.0009 (13)0.0048 (14)0.0042 (13)
C2010.0220 (15)0.0392 (19)0.0316 (18)0.0092 (13)0.0085 (14)0.0036 (14)
C2020.0258 (15)0.0246 (15)0.0281 (16)0.0028 (12)0.0132 (13)0.0019 (12)
C3010.0329 (19)0.059 (3)0.044 (2)0.0061 (17)0.0198 (18)0.0176 (19)
C3020.0350 (18)0.0286 (17)0.040 (2)0.0031 (14)0.0183 (16)0.0058 (14)
N1A0.0254 (14)0.0400 (16)0.0239 (14)0.0094 (12)0.0062 (11)0.0020 (12)
N2A0.0119 (15)0.0240 (18)0.0213 (18)0.0038 (13)0.0019 (13)0.0082 (14)
N10.0148 (11)0.0147 (11)0.0192 (12)0.0006 (9)0.0061 (10)0.0026 (9)
N20.0212 (13)0.0280 (14)0.0228 (14)0.0018 (11)0.0080 (11)0.0064 (11)
N30.0199 (12)0.0170 (12)0.0212 (13)0.0013 (9)0.0096 (10)0.0022 (9)
N40.035 (2)0.0179 (18)0.024 (2)0.0000.0168 (18)0.000
O10.0209 (10)0.0177 (10)0.0166 (10)0.0030 (8)0.0045 (8)0.0014 (7)
O20.0228 (10)0.0212 (10)0.0151 (10)0.0004 (8)0.0034 (8)0.0002 (8)
O30.0210 (10)0.0140 (9)0.0222 (10)0.0038 (7)0.0095 (8)0.0019 (7)
O40.0195 (9)0.0150 (9)0.0238 (10)0.0016 (7)0.0116 (8)0.0019 (7)
O50.0233 (10)0.0217 (10)0.0208 (10)0.0035 (8)0.0140 (9)0.0011 (8)
O60.0196 (10)0.0152 (9)0.0214 (10)0.0008 (7)0.0114 (8)0.0009 (7)
O80.0126 (9)0.0152 (9)0.0199 (10)0.0002 (7)0.0068 (7)0.0003 (7)
O90.0144 (9)0.0182 (9)0.0170 (9)0.0009 (7)0.0064 (8)0.0004 (7)
O100.0128 (9)0.0209 (10)0.0171 (9)0.0007 (7)0.0058 (8)0.0009 (7)
O110.0167 (9)0.0171 (9)0.0182 (10)0.0016 (7)0.0073 (8)0.0006 (7)
O120.0169 (9)0.0148 (9)0.0171 (9)0.0006 (7)0.0087 (8)0.0004 (7)
O130.0132 (8)0.0154 (9)0.0153 (9)0.0007 (7)0.0055 (7)0.0002 (7)
O140.0174 (9)0.0150 (9)0.0162 (9)0.0004 (7)0.0079 (8)0.0003 (7)
O150.0146 (9)0.0142 (9)0.0179 (9)0.0007 (7)0.0072 (8)0.0001 (7)
O160.0136 (9)0.0153 (9)0.0153 (9)0.0019 (7)0.0064 (7)0.0002 (7)
O170.0155 (9)0.0154 (9)0.0229 (10)0.0005 (7)0.0102 (8)0.0014 (7)
O180.0209 (10)0.0187 (10)0.0245 (11)0.0053 (8)0.0123 (8)0.0037 (8)
O190.0143 (9)0.0163 (9)0.0185 (10)0.0010 (7)0.0064 (8)0.0003 (7)
O200.0124 (8)0.0151 (9)0.0158 (9)0.0005 (7)0.0055 (7)0.0001 (7)
O1010.0212 (10)0.0180 (10)0.0231 (11)0.0012 (8)0.0061 (8)0.0034 (8)
O2010.0323 (11)0.0190 (10)0.0292 (12)0.0017 (8)0.0197 (10)0.0001 (8)
O3010.0579 (16)0.0260 (12)0.0432 (14)0.0008 (11)0.0372 (13)0.0037 (10)
S1010.0234 (3)0.0148 (3)0.0213 (4)0.0001 (3)0.0073 (3)0.0001 (2)
S2010.0208 (3)0.0210 (3)0.0178 (3)0.0030 (3)0.0098 (3)0.0007 (3)
S3010.0369 (4)0.0244 (4)0.0368 (4)0.0036 (3)0.0236 (4)0.0004 (3)
V10.0127 (2)0.0132 (2)0.0137 (2)0.00062 (16)0.00454 (18)0.00080 (16)
V20.0148 (2)0.0135 (2)0.0144 (2)0.00056 (16)0.00518 (18)0.00008 (16)
V30.0141 (2)0.0119 (2)0.0155 (2)0.00181 (16)0.00641 (18)0.00042 (16)
V40.0134 (2)0.0120 (2)0.0160 (2)0.00060 (16)0.00710 (18)0.00085 (16)
V50.0150 (2)0.0127 (2)0.0159 (2)0.00051 (16)0.00876 (18)0.00093 (16)
V60.0148 (2)0.0125 (2)0.0165 (2)0.00062 (16)0.00837 (18)0.00031 (16)
V70.0132 (2)0.0133 (2)0.0160 (2)0.00094 (16)0.00679 (18)0.00065 (16)
Geometric parameters (Å, º) top
C101—S1011.770 (3)O5—V51.6057 (19)
C101—H10A0.9800O6—V61.6017 (19)
C101—H10B0.9800O8—V11.7958 (19)
C101—H10C0.9800O8—V21.9191 (19)
C102—S1011.783 (3)O9—V4i1.8205 (19)
C102—H10D0.9800O9—V31.8647 (19)
C102—H10E0.9800O10—V7i1.786 (2)
C102—H10F0.9800O10—V11.801 (2)
C201—S2011.770 (3)O11—V31.7472 (19)
C201—H20A0.9800O11—V21.8662 (19)
C201—H20B0.9800O12—V21.9235 (19)
C201—H20C0.9800O12—V51.9323 (19)
C202—S2011.780 (3)O12—V11.9607 (19)
C202—H20D0.9800O13—V4i1.9030 (19)
C202—H20E0.9800O13—V71.9162 (19)
C202—H20F0.9800O13—V31.9737 (19)
C301—S3011.761 (4)O14—V21.7878 (19)
C301—H30A0.9800O14—V61.8337 (19)
C301—H30B0.9800O15—V41.9103 (19)
C301—H30C0.9800O15—V11.9368 (19)
C302—S3011.776 (3)O15—V51.9519 (19)
C302—H30D0.9800O16—V31.9283 (18)
C302—H30E0.9800O16—V61.9393 (18)
C302—H30F0.9800O16—V71.9662 (19)
N1A—N2A1.181 (3)O17—V51.7766 (19)
N2A—N1Ai1.181 (3)O17—V61.8186 (19)
N1—H10.869 (18)O18—V71.603 (2)
N1—H20.877 (18)O19—V41.8243 (19)
N1—H30.850 (18)O19—V51.8309 (19)
N1—H40.863 (19)O20—V71.8267 (19)
N2—H50.89 (2)O20—V61.8983 (19)
N2—H60.908 (18)O101—S1011.541 (2)
N2—H70.875 (17)O201—S2011.526 (2)
N2—H80.890 (19)O301—S3011.511 (2)
N3—H90.877 (18)V1—V22.9179 (6)
N3—H100.861 (18)V1—V53.0542 (6)
N3—H110.869 (18)V3—V4i2.9025 (6)
N3—H120.876 (18)V3—V73.0517 (6)
N4—H130.878 (18)V4—O9i1.8205 (19)
N4—H140.869 (18)V4—O13i1.9029 (19)
O1—V11.6038 (19)V4—V52.8755 (6)
O2—V21.598 (2)V4—V3i2.9026 (6)
O3—V31.6089 (19)V6—V72.9365 (6)
O4—V41.6016 (19)V7—O10i1.786 (2)
S101—C101—H10A109.5O14—V2—O8153.89 (8)
S101—C101—H10B109.5O11—V2—O891.13 (8)
H10A—C101—H10B109.5O2—V2—O12106.14 (9)
S101—C101—H10C109.5O14—V2—O1288.35 (8)
H10A—C101—H10C109.5O11—V2—O12148.91 (9)
H10B—C101—H10C109.5O8—V2—O1278.54 (8)
S101—C102—H10D109.5O2—V2—V1108.30 (8)
S101—C102—H10E109.5O14—V2—V1126.00 (6)
H10D—C102—H10E109.5O11—V2—V1121.98 (6)
S101—C102—H10F109.5O8—V2—V136.76 (6)
H10D—C102—H10F109.5O12—V2—V141.79 (6)
H10E—C102—H10F109.5O3—V3—O11104.81 (10)
S201—C201—H20A109.5O3—V3—O9103.75 (9)
S201—C201—H20B109.5O11—V3—O996.40 (9)
H20A—C201—H20B109.5O3—V3—O16103.54 (9)
S201—C201—H20C109.5O11—V3—O1694.32 (9)
H20A—C201—H20C109.5O9—V3—O16146.95 (8)
H20B—C201—H20C109.5O3—V3—O13108.21 (9)
S201—C202—H20D109.5O11—V3—O13146.90 (9)
S201—C202—H20E109.5O9—V3—O1378.09 (8)
H20D—C202—H20E109.5O16—V3—O1375.93 (8)
S201—C202—H20F109.5O3—V3—V4i109.70 (7)
H20D—C202—H20F109.5O11—V3—V4i127.16 (7)
H20E—C202—H20F109.5O9—V3—V4i37.50 (6)
S301—C301—H30A109.5O16—V3—V4i114.32 (6)
S301—C301—H30B109.5O13—V3—V4i40.60 (5)
H30A—C301—H30B109.5O3—V3—V7115.39 (7)
S301—C301—H30C109.5O11—V3—V7122.44 (6)
H30A—C301—H30C109.5O9—V3—V7111.08 (6)
H30B—C301—H30C109.5O16—V3—V738.85 (6)
S301—C302—H30D109.5O13—V3—V737.66 (5)
S301—C302—H30E109.5V4i—V3—V775.618 (16)
H30D—C302—H30E109.5O4—V4—O9i106.60 (10)
S301—C302—H30F109.5O4—V4—O19106.89 (9)
H30D—C302—H30F109.5O9i—V4—O1992.14 (9)
H30E—C302—H30F109.5O4—V4—O13i107.10 (9)
N1Ai—N2A—N1A180.0O9i—V4—O13i81.01 (8)
H1—N1—H2112 (3)O19—V4—O13i145.88 (9)
H1—N1—H3111 (3)O4—V4—O15105.58 (9)
H2—N1—H3100 (3)O9i—V4—O15147.76 (9)
H1—N1—H4106 (4)O19—V4—O1580.39 (8)
H2—N1—H4109 (4)O13i—V4—O1587.79 (8)
H3—N1—H4119 (4)O4—V4—V5107.98 (7)
H5—N2—H6117 (5)O9i—V4—V5125.84 (6)
H5—N2—H7107 (5)O19—V4—V538.21 (6)
H6—N2—H7105 (3)O13i—V4—V5124.94 (6)
H5—N2—H8111 (5)O15—V4—V542.44 (6)
H6—N2—H8107 (3)O4—V4—V3i111.40 (7)
H7—N2—H8110 (3)O9i—V4—V3i38.58 (6)
H9—N3—H10113 (3)O19—V4—V3i123.89 (6)
H9—N3—H11111 (3)O13i—V4—V3i42.45 (6)
H10—N3—H11110 (3)O15—V4—V3i124.21 (6)
H9—N3—H12109 (3)V5—V4—V3i140.58 (2)
H10—N3—H12105 (3)O5—V5—O17106.73 (10)
H11—N3—H12108 (3)O5—V5—O19104.84 (10)
H13—N4—H14109 (3)O17—V5—O1995.65 (9)
V1—O8—V2103.48 (9)O5—V5—O12103.62 (9)
V4i—O9—V3103.92 (9)O17—V5—O1292.54 (8)
V7i—O10—V1154.23 (12)O19—V5—O12146.61 (8)
V3—O11—V2139.14 (11)O5—V5—O15107.21 (9)
V2—O12—V5137.69 (10)O17—V5—O15145.87 (9)
V2—O12—V197.39 (8)O19—V5—O1579.12 (8)
V5—O12—V1103.36 (9)O12—V5—O1576.08 (8)
V4i—O13—V7145.98 (11)O5—V5—V4107.49 (8)
V4i—O13—V396.94 (8)O17—V5—V4128.05 (7)
V7—O13—V3103.35 (9)O19—V5—V438.04 (6)
V2—O14—V6128.28 (11)O12—V5—V4115.54 (6)
V4—O15—V1147.44 (11)O15—V5—V441.33 (6)
V4—O15—V596.23 (8)O5—V5—V1115.10 (8)
V1—O15—V5103.52 (9)O17—V5—V1120.27 (6)
V3—O16—V6138.04 (10)O19—V5—V1111.65 (6)
V3—O16—V7103.18 (9)O12—V5—V138.65 (6)
V6—O16—V797.51 (8)O15—V5—V138.07 (5)
V5—O17—V6142.00 (11)V4—V5—V176.970 (16)
V4—O19—V5103.75 (9)O6—V6—O17104.39 (9)
V7—O20—V6104.04 (9)O6—V6—O14102.88 (9)
O101—S101—C101104.06 (14)O17—V6—O1488.91 (9)
O101—S101—C102106.84 (14)O6—V6—O20100.37 (9)
C101—S101—C10299.12 (19)O17—V6—O2094.21 (8)
O201—S201—C201105.88 (15)O14—V6—O20154.98 (8)
O201—S201—C202105.45 (14)O6—V6—O16107.77 (9)
C201—S201—C20298.11 (17)O17—V6—O16147.80 (8)
O301—S301—C301104.12 (17)O14—V6—O1685.61 (8)
O301—S301—C302104.75 (16)O20—V6—O1678.56 (8)
C301—S301—C30298.25 (19)O6—V6—V7110.69 (7)
O1—V1—O8105.88 (9)O17—V6—V7122.99 (7)
O1—V1—O10106.74 (10)O14—V6—V7123.34 (6)
O8—V1—O1097.13 (9)O20—V6—V737.12 (6)
O1—V1—O15106.12 (9)O16—V6—V741.59 (5)
O8—V1—O15144.10 (8)O18—V7—O10i107.45 (10)
O10—V1—O1588.86 (8)O18—V7—O20104.50 (9)
O1—V1—O12105.14 (9)O10i—V7—O2096.14 (9)
O8—V1—O1280.57 (8)O18—V7—O13104.90 (9)
O10—V1—O12147.37 (9)O10i—V7—O1390.97 (8)
O15—V1—O1275.77 (8)O20—V7—O13146.02 (8)
O1—V1—V2111.31 (7)O18—V7—O16105.71 (9)
O8—V1—V239.76 (6)O10i—V7—O16146.56 (8)
O10—V1—V2128.38 (7)O20—V7—O1679.58 (8)
O15—V1—V2111.79 (6)O13—V7—O1676.39 (8)
O12—V1—V240.82 (5)O18—V7—V6112.56 (7)
O1—V1—V5115.30 (8)O10i—V7—V6125.11 (7)
O8—V1—V5111.26 (6)O20—V7—V638.84 (6)
O10—V1—V5118.42 (6)O13—V7—V6112.44 (6)
O15—V1—V538.42 (6)O16—V7—V640.90 (5)
O12—V1—V537.99 (6)O18—V7—V3114.74 (8)
V2—V1—V574.005 (16)O10i—V7—V3119.95 (6)
O2—V2—O14104.14 (10)O20—V7—V3111.56 (6)
O2—V2—O11104.61 (10)O13—V7—V339.00 (6)
O14—V2—O1188.62 (9)O16—V7—V337.97 (5)
O2—V2—O8101.18 (10)V6—V7—V374.148 (16)
V2—O8—V1—O1104.41 (10)V5—O19—V4—O13i77.03 (17)
V2—O8—V1—O10145.87 (9)V5—O19—V4—O155.67 (9)
V2—O8—V1—O1547.89 (18)V5—O19—V4—V3i130.64 (6)
V2—O8—V1—O121.23 (8)V6—O17—V5—O5135.74 (19)
V2—O8—V1—V521.57 (10)V6—O17—V5—O19116.89 (19)
V7i—O10—V1—O197.0 (3)V6—O17—V5—O1230.70 (19)
V7i—O10—V1—O8154.0 (3)V6—O17—V5—O1538.0 (3)
V7i—O10—V1—O159.5 (3)V6—O17—V5—V494.94 (19)
V7i—O10—V1—O1270.3 (3)V6—O17—V5—V12.3 (2)
V7i—O10—V1—V2126.7 (2)V4—O19—V5—O599.54 (11)
V7i—O10—V1—V535.1 (3)V4—O19—V5—O17151.47 (10)
V6—O14—V2—O2176.45 (13)V4—O19—V5—O1248.11 (19)
V6—O14—V2—O1178.83 (14)V4—O19—V5—O155.58 (9)
V6—O14—V2—O810.9 (3)V4—O19—V5—V125.72 (10)
V6—O14—V2—O1270.22 (13)V5—O17—V6—O6152.04 (18)
V6—O14—V2—V150.77 (16)V5—O17—V6—O1449.03 (19)
V3—O11—V2—O2153.00 (17)V5—O17—V6—O20106.12 (19)
V3—O11—V2—O1448.74 (18)V5—O17—V6—O1631.0 (3)
V3—O11—V2—O8105.14 (18)V5—O17—V6—V780.99 (19)
V3—O11—V2—O1235.8 (3)V2—O14—V6—O6178.79 (13)
V3—O11—V2—V183.95 (18)V2—O14—V6—O1774.28 (14)
V2—O11—V3—O3134.58 (17)V2—O14—V6—O2023.4 (3)
V2—O11—V3—O9119.34 (17)V2—O14—V6—O1673.97 (13)
V2—O11—V3—O1629.34 (18)V2—O14—V6—V755.46 (15)
V2—O11—V3—O1341.4 (3)V7—O20—V6—O6110.70 (10)
V2—O11—V3—V4i95.79 (17)V7—O20—V6—O17143.83 (9)
V2—O11—V3—V70.7 (2)V7—O20—V6—O1447.4 (2)
V4i—O9—V3—O3104.55 (11)V7—O20—V6—O164.47 (8)
V4i—O9—V3—O11148.46 (10)V6—O20—V7—O18108.09 (10)
V4i—O9—V3—O1640.32 (19)V6—O20—V7—O10i142.08 (9)
V4i—O9—V3—O131.54 (9)V6—O20—V7—O1341.11 (18)
V4i—O9—V3—V720.01 (10)V6—O20—V7—O164.39 (8)
V5—O19—V4—O497.81 (11)V6—O20—V7—V316.46 (10)
V5—O19—V4—O9i154.12 (10)
Symmetry code: (i) x+1/2, y+3/2, z+1.
Heptaammonium cyanatotetradecavanadate dimethyl sulfoxide hexasolvate (3) top
Crystal data top
(NH4)7[V14O38(OCN)]·6C2H6OSF(000) = 3904
Mr = 1958.24Dx = 2.084 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71075 Å
a = 19.352 (6) ÅCell parameters from 12134 reflections
b = 24.753 (6) Åθ = 3.1–27.5°
c = 14.561 (5) ŵ = 2.30 mm1
β = 116.537 (6)°T = 83 K
V = 6240 (3) Å3Block, red
Z = 40.20 × 0.20 × 0.20 mm
Data collection top
Rigaku Mercury70
diffractometer
6028 reflections with I > 2σ(I)
Detector resolution: 14.629 pixels mm-1Rint = 0.058
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: numerical
(NUMABS; Rigaku, 1999)
h = 2524
Tmin = 0.656, Tmax = 0.892k = 3226
33228 measured reflectionsl = 1818
7133 independent reflections
Refinement top
Refinement on F234 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.052H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.146 w = 1/[σ2(Fo2) + (0.0965P)2 + 17.6756P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
7133 reflectionsΔρmax = 1.32 e Å3
446 parametersΔρmin = 1.19 e Å3
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
N1A0.7537 (2)0.7752 (2)0.5711 (4)0.0660 (13)0.5
C1A0.75000.75000.50000.0562 (18)
O1A0.7537 (2)0.7752 (2)0.5711 (4)0.0660 (13)0.5
C1010.8153 (3)0.6944 (2)0.0603 (4)0.0478 (13)
H10A0.81130.73130.08180.072*
H10B0.80390.69450.01240.072*
H10C0.77820.67120.07020.072*
C1020.9588 (3)0.7102 (2)0.0812 (4)0.0381 (10)
H10D0.96030.74780.10320.057*
H10E1.01170.69680.10480.057*
H10F0.93150.70830.00610.057*
C2010.6713 (3)0.5946 (3)0.0401 (5)0.0662 (18)
H20A0.68920.61820.07920.099*
H20B0.67140.61470.01790.099*
H20C0.70590.56340.01440.099*
C2020.5270 (3)0.6331 (2)0.1287 (5)0.0524 (13)
H20D0.53670.65860.17310.079*
H20E0.47150.62550.15790.079*
H20F0.54460.64890.06020.079*
C3010.7821 (3)0.4634 (3)0.3418 (4)0.0508 (13)
H30A0.73040.44810.30270.076*
H30B0.81070.44170.40360.076*
H30C0.77780.50060.36150.076*
C3020.7775 (3)0.5132 (2)0.1739 (4)0.0516 (14)
H30D0.72640.49880.12810.077*
H30E0.77160.54490.21020.077*
H30F0.80450.52370.13350.077*
N10.94349 (18)0.74946 (15)0.5919 (3)0.0259 (7)
N20.4759 (2)0.55728 (19)0.3866 (3)0.0380 (9)
N31.00367 (19)0.42590 (15)0.5084 (3)0.0274 (7)
N41.00000.5389 (2)0.25000.0346 (11)
O10.66049 (16)0.69295 (12)0.8013 (2)0.0300 (6)
O20.87290 (15)0.61142 (11)0.3006 (2)0.0270 (6)
O30.87722 (15)0.55917 (12)0.5708 (2)0.0296 (6)
O40.60313 (15)0.84766 (12)0.1513 (2)0.0294 (6)
O50.59304 (16)0.69119 (12)0.0826 (2)0.0318 (6)
O60.63351 (15)0.54545 (11)0.3417 (2)0.0283 (6)
O70.63247 (15)0.57562 (11)0.6132 (2)0.0279 (6)
O80.85230 (14)0.71827 (11)0.3140 (2)0.0257 (6)
O90.86041 (14)0.65714 (11)0.6444 (2)0.0259 (6)
O100.88852 (14)0.65233 (11)0.48018 (19)0.0227 (5)
O110.76523 (14)0.60696 (11)0.3862 (2)0.0245 (5)
O120.73314 (14)0.65834 (11)0.2187 (2)0.0247 (5)
O130.74289 (14)0.65810 (11)0.6895 (2)0.0235 (5)
O140.71148 (14)0.76181 (11)0.2096 (2)0.0241 (5)
O150.73272 (14)0.60444 (10)0.5274 (2)0.0223 (5)
O160.62192 (14)0.64481 (11)0.2666 (2)0.0261 (6)
O170.61009 (14)0.68530 (11)0.5944 (2)0.0245 (5)
O180.59830 (13)0.75254 (11)0.2409 (2)0.0243 (5)
O190.59836 (14)0.63028 (11)0.4341 (2)0.0259 (6)
O1010.91065 (18)0.61291 (12)0.0962 (2)0.0356 (7)
O2010.5582 (2)0.53720 (15)0.0507 (3)0.0532 (9)
O3010.91143 (16)0.48762 (12)0.3345 (2)0.0320 (6)
V10.68285 (3)0.71460 (3)0.71404 (5)0.02183 (15)
V20.82410 (3)0.65129 (3)0.33605 (5)0.02248 (16)
V30.83309 (3)0.61563 (3)0.53367 (5)0.02199 (15)
V40.65320 (3)0.81265 (3)0.25186 (5)0.02161 (15)
V50.65127 (3)0.69857 (3)0.20126 (5)0.02330 (16)
V60.66303 (3)0.60582 (3)0.37839 (5)0.02196 (15)
V70.65902 (3)0.62768 (3)0.57216 (5)0.02141 (15)
S1010.90979 (6)0.66979 (4)0.13455 (7)0.0296 (2)
S2010.57772 (8)0.57232 (5)0.11969 (11)0.0465 (3)
S3010.83194 (6)0.46290 (4)0.26469 (8)0.0312 (2)
H10.9935 (12)0.748 (2)0.630 (3)0.046 (15)*
H20.929 (3)0.7195 (14)0.556 (4)0.049 (16)*
H30.937 (2)0.7766 (12)0.551 (2)0.012 (9)*
H40.932 (4)0.759 (3)0.641 (4)0.08 (2)*
H50.509 (2)0.5849 (15)0.404 (4)0.045 (15)*
H60.440 (4)0.556 (4)0.322 (3)0.14 (4)*
H70.461 (3)0.555 (2)0.437 (3)0.031 (12)*
H80.4998 (19)0.5260 (10)0.393 (3)0.006 (8)*
H90.9744 (19)0.4097 (15)0.533 (3)0.013 (9)*
H101.032 (2)0.4004 (16)0.498 (4)0.041 (14)*
H110.978 (2)0.4426 (19)0.451 (2)0.040 (14)*
H121.032 (2)0.4496 (15)0.555 (3)0.028 (12)*
H130.965 (2)0.5581 (18)0.200 (3)0.035 (13)*
H140.977 (2)0.5161 (16)0.275 (4)0.036 (13)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N1A0.0324 (18)0.072 (3)0.076 (3)0.010 (2)0.008 (2)0.030 (2)
C1A0.021 (3)0.057 (5)0.073 (4)0.008 (3)0.006 (3)0.038 (3)
O1A0.0324 (18)0.072 (3)0.076 (3)0.010 (2)0.008 (2)0.030 (2)
C1010.031 (2)0.064 (4)0.043 (3)0.013 (2)0.011 (2)0.003 (2)
C1020.040 (2)0.038 (3)0.039 (2)0.0043 (19)0.020 (2)0.003 (2)
C2010.047 (3)0.091 (5)0.063 (4)0.017 (3)0.027 (3)0.027 (4)
C2020.055 (3)0.045 (3)0.063 (3)0.003 (2)0.031 (3)0.008 (3)
C3010.035 (2)0.071 (4)0.051 (3)0.001 (2)0.024 (2)0.011 (3)
C3020.037 (2)0.038 (3)0.051 (3)0.003 (2)0.006 (2)0.006 (2)
N10.0213 (15)0.0242 (18)0.0284 (18)0.0008 (13)0.0079 (13)0.0072 (14)
N20.0306 (19)0.048 (3)0.034 (2)0.0045 (17)0.0131 (17)0.0084 (18)
N30.0251 (16)0.0256 (18)0.0319 (19)0.0034 (13)0.0129 (14)0.0040 (15)
N40.048 (3)0.027 (3)0.033 (3)0.0000.022 (3)0.000
O10.0318 (14)0.0346 (16)0.0289 (15)0.0046 (12)0.0183 (12)0.0022 (12)
O20.0261 (13)0.0271 (15)0.0312 (14)0.0015 (11)0.0161 (11)0.0001 (11)
O30.0273 (13)0.0282 (15)0.0362 (15)0.0068 (11)0.0167 (12)0.0042 (12)
O40.0278 (13)0.0286 (15)0.0259 (14)0.0045 (11)0.0068 (11)0.0024 (11)
O50.0308 (14)0.0329 (16)0.0231 (14)0.0010 (12)0.0042 (11)0.0000 (12)
O60.0276 (13)0.0239 (14)0.0326 (15)0.0042 (11)0.0128 (12)0.0037 (11)
O70.0295 (13)0.0234 (14)0.0332 (15)0.0014 (11)0.0161 (12)0.0039 (11)
O80.0217 (12)0.0239 (14)0.0328 (14)0.0009 (10)0.0133 (11)0.0005 (11)
O90.0188 (11)0.0310 (15)0.0267 (13)0.0002 (10)0.0092 (10)0.0007 (11)
O100.0196 (11)0.0225 (14)0.0251 (13)0.0007 (10)0.0091 (10)0.0009 (10)
O110.0192 (12)0.0274 (14)0.0266 (14)0.0030 (10)0.0101 (10)0.0003 (11)
O120.0255 (12)0.0233 (14)0.0261 (14)0.0006 (10)0.0123 (11)0.0008 (11)
O130.0211 (12)0.0226 (13)0.0266 (13)0.0012 (10)0.0106 (10)0.0019 (11)
O140.0238 (12)0.0242 (14)0.0252 (13)0.0006 (10)0.0117 (10)0.0004 (11)
O150.0198 (11)0.0212 (13)0.0244 (13)0.0004 (10)0.0087 (10)0.0007 (10)
O160.0213 (12)0.0284 (15)0.0253 (13)0.0006 (10)0.0075 (10)0.0014 (11)
O170.0201 (11)0.0243 (14)0.0273 (14)0.0015 (10)0.0089 (10)0.0000 (11)
O180.0182 (11)0.0239 (14)0.0296 (14)0.0007 (10)0.0095 (10)0.0010 (11)
O190.0201 (12)0.0294 (15)0.0282 (14)0.0007 (10)0.0107 (11)0.0011 (11)
O1010.0430 (17)0.0298 (16)0.0413 (17)0.0022 (13)0.0253 (14)0.0008 (13)
O2010.076 (2)0.044 (2)0.060 (2)0.0023 (18)0.050 (2)0.0025 (17)
O3010.0291 (13)0.0279 (15)0.0337 (16)0.0015 (11)0.0093 (12)0.0036 (12)
V10.0213 (3)0.0224 (3)0.0243 (3)0.0007 (2)0.0125 (2)0.0016 (2)
V20.0212 (3)0.0218 (3)0.0258 (3)0.0011 (2)0.0118 (3)0.0010 (2)
V30.0184 (3)0.0227 (3)0.0246 (3)0.0013 (2)0.0094 (2)0.0007 (2)
V40.0181 (3)0.0226 (3)0.0215 (3)0.0010 (2)0.0066 (2)0.0017 (2)
V50.0212 (3)0.0231 (3)0.0236 (3)0.0004 (2)0.0082 (2)0.0002 (2)
V60.0201 (3)0.0207 (3)0.0244 (3)0.0024 (2)0.0093 (2)0.0004 (2)
V70.0190 (3)0.0210 (3)0.0245 (3)0.0010 (2)0.0101 (2)0.0016 (2)
S1010.0298 (5)0.0335 (6)0.0266 (5)0.0042 (4)0.0136 (4)0.0011 (4)
S2010.0530 (7)0.0419 (7)0.0565 (8)0.0053 (5)0.0352 (6)0.0001 (6)
S3010.0326 (5)0.0243 (5)0.0326 (5)0.0005 (4)0.0110 (4)0.0017 (4)
Geometric parameters (Å, º) top
N1A—C1A1.183 (6)O5—V51.597 (3)
C1A—O1Ai1.183 (6)O6—V61.604 (3)
C1A—N1Ai1.183 (6)O7—V71.599 (3)
C101—S1011.766 (5)O8—V1i1.773 (3)
C101—H10A0.9800O8—V21.818 (3)
C101—H10B0.9800O9—V31.781 (3)
C101—H10C0.9800O9—V4i1.808 (3)
C102—S1011.779 (4)O10—V31.825 (3)
C102—H10D0.9800O10—V21.903 (3)
C102—H10E0.9800O11—V61.930 (3)
C102—H10F0.9800O11—V21.944 (3)
C201—S2011.747 (6)O11—V31.965 (3)
C201—H20A0.9800O12—V51.791 (3)
C201—H20B0.9800O12—V21.833 (3)
C201—H20C0.9800O13—V71.908 (3)
C202—S2011.769 (5)O13—V4i1.940 (3)
C202—H20D0.9800O13—V11.951 (3)
C202—H20E0.9800O14—V51.923 (3)
C202—H20F0.9800O14—V1i1.931 (3)
C301—S3011.776 (5)O14—V41.964 (3)
C301—H30A0.9800O15—V71.903 (3)
C301—H30B0.9800O15—V31.923 (3)
C301—H30C0.9800O15—V61.978 (3)
C302—S3011.779 (5)O16—V61.748 (3)
C302—H30D0.9800O16—V51.866 (3)
C302—H30E0.9800O17—V71.819 (3)
C302—H30F0.9800O17—V11.831 (3)
N1—H10.88 (2)O18—V41.793 (3)
N1—H20.88 (2)O18—V51.923 (3)
N1—H30.867 (19)O19—V71.820 (3)
N1—H40.86 (2)O19—V61.871 (3)
N2—H50.89 (2)O101—S1011.517 (3)
N2—H60.88 (2)O201—S2011.499 (4)
N2—H70.903 (19)O301—S3011.542 (3)
N2—H80.884 (18)V1—O8i1.773 (3)
N3—H90.889 (18)V1—O14i1.931 (3)
N3—H100.886 (19)V1—V72.8736 (11)
N3—H110.867 (19)V1—V4i3.0594 (13)
N3—H120.877 (19)V2—V32.9396 (12)
N4—H130.881 (19)V3—V63.0582 (12)
N4—H140.884 (19)V4—O9i1.808 (3)
O1—V11.607 (3)V4—O13i1.940 (3)
O2—V21.602 (3)V4—V52.9144 (11)
O3—V31.601 (3)V4—V1i3.0594 (13)
O4—V41.602 (3)V6—V72.9077 (12)
N1A—C1A—O1Ai180.0 (6)O12—V2—V3123.57 (9)
N1A—C1A—N1Ai180.0 (6)O10—V2—V337.01 (8)
O1Ai—C1A—N1Ai0.0 (4)O11—V2—V341.51 (8)
S101—C101—H10A109.5O3—V3—O9107.45 (14)
S101—C101—H10B109.5O3—V3—O10104.62 (13)
H10A—C101—H10B109.5O9—V3—O1096.06 (12)
S101—C101—H10C109.5O3—V3—O15105.38 (13)
H10A—C101—H10C109.5O9—V3—O1590.65 (11)
H10B—C101—H10C109.5O10—V3—O15145.61 (12)
S101—C102—H10D109.5O3—V3—O11105.61 (13)
S101—C102—H10E109.5O9—V3—O11146.64 (12)
H10D—C102—H10E109.5O10—V3—O1179.70 (11)
S101—C102—H10F109.5O15—V3—O1176.39 (11)
H10D—C102—H10F109.5O3—V3—V2112.47 (10)
H10E—C102—H10F109.5O9—V3—V2125.20 (10)
S201—C201—H20A109.5O10—V3—V238.89 (8)
S201—C201—H20B109.5O15—V3—V2112.32 (8)
H20A—C201—H20B109.5O11—V3—V240.95 (8)
S201—C201—H20C109.5O3—V3—V6114.58 (11)
H20A—C201—H20C109.5O9—V3—V6120.08 (8)
H20B—C201—H20C109.5O10—V3—V6111.57 (9)
S201—C202—H20D109.5O15—V3—V639.02 (8)
S201—C202—H20E109.5O11—V3—V637.86 (7)
H20D—C202—H20E109.5V2—V3—V674.14 (3)
S201—C202—H20F109.5O4—V4—O18105.97 (13)
H20D—C202—H20F109.5O4—V4—O9i106.61 (14)
H20E—C202—H20F109.5O18—V4—O9i96.67 (12)
S301—C301—H30A109.5O4—V4—O13i106.56 (13)
S301—C301—H30B109.5O18—V4—O13i143.64 (12)
H30A—C301—H30B109.5O9i—V4—O13i89.26 (11)
S301—C301—H30C109.5O4—V4—O14104.91 (13)
H30A—C301—H30C109.5O18—V4—O1480.84 (11)
H30B—C301—H30C109.5O9i—V4—O14147.78 (12)
S301—C302—H30D109.5O13i—V4—O1475.50 (11)
S301—C302—H30E109.5O4—V4—V5111.03 (11)
H30D—C302—H30E109.5O18—V4—V539.95 (8)
S301—C302—H30F109.5O9i—V4—V5128.47 (9)
H30D—C302—H30F109.5O13i—V4—V5111.51 (8)
H30E—C302—H30F109.5O14—V4—V540.89 (8)
H1—N1—H2109 (5)O4—V4—V1i115.30 (11)
H1—N1—H3104 (4)O18—V4—V1i111.20 (8)
H2—N1—H3110 (4)O9i—V4—V1i118.91 (8)
H1—N1—H496 (6)O13i—V4—V1i38.27 (8)
H2—N1—H4127 (6)O14—V4—V1i37.84 (8)
H3—N1—H4109 (6)V5—V4—V1i73.90 (2)
H5—N2—H6117 (7)O5—V5—O12104.01 (14)
H5—N2—H7106 (5)O5—V5—O16104.01 (14)
H6—N2—H7118 (7)O12—V5—O1689.01 (12)
H5—N2—H8111 (4)O5—V5—O18101.01 (14)
H6—N2—H8102 (7)O12—V5—O18154.20 (12)
H7—N2—H8102 (4)O16—V5—O1891.02 (12)
H9—N3—H10107 (4)O5—V5—O14106.01 (14)
H9—N3—H11114 (4)O12—V5—O1488.34 (12)
H10—N3—H11108 (5)O16—V5—O14149.59 (12)
H9—N3—H12107 (4)O18—V5—O1478.74 (11)
H10—N3—H12112 (4)O5—V5—V4107.91 (11)
H11—N3—H12109 (5)O12—V5—V4126.32 (9)
H13—N4—H14109 (4)O16—V5—V4122.30 (9)
V1i—O8—V2141.34 (15)O18—V5—V436.80 (8)
V3—O9—V4i154.16 (16)O14—V5—V441.95 (8)
V3—O10—V2104.10 (12)O6—V6—O16104.96 (14)
V6—O11—V2138.02 (15)O6—V6—O19103.79 (13)
V6—O11—V3103.45 (12)O16—V6—O1996.36 (12)
V2—O11—V397.53 (11)O6—V6—O11103.67 (13)
V5—O12—V2127.28 (15)O16—V6—O1194.30 (12)
V7—O13—V4i147.26 (15)O19—V6—O11146.77 (12)
V7—O13—V196.26 (11)O6—V6—O15108.43 (13)
V4i—O13—V1103.70 (12)O16—V6—O15146.54 (12)
V5—O14—V1i137.61 (15)O19—V6—O1577.89 (11)
V5—O14—V497.16 (11)O11—V6—O1575.95 (11)
V1i—O14—V4103.55 (13)O6—V6—V7109.68 (10)
V7—O15—V3146.69 (15)O16—V6—V7127.02 (10)
V7—O15—V697.03 (11)O19—V6—V737.41 (8)
V3—O15—V6103.24 (12)O11—V6—V7114.28 (8)
V6—O16—V5138.84 (15)O15—V6—V740.51 (8)
V7—O17—V1103.87 (12)O6—V6—V3115.20 (10)
V4—O18—V5103.25 (12)O16—V6—V3122.43 (9)
V7—O19—V6103.96 (13)O19—V6—V3111.17 (9)
O1—V1—O8i106.48 (14)O11—V6—V338.68 (8)
O1—V1—O17104.85 (14)O15—V6—V337.75 (7)
O8i—V1—O1795.69 (12)V7—V6—V375.78 (3)
O1—V1—O14i103.62 (13)O7—V7—O17106.61 (13)
O8i—V1—O14i92.75 (12)O7—V7—O19106.53 (14)
O17—V1—O14i146.55 (11)O17—V7—O1992.21 (12)
O1—V1—O13107.39 (14)O7—V7—O15107.42 (13)
O8i—V1—O13145.95 (12)O17—V7—O15145.83 (12)
O17—V1—O1379.01 (11)O19—V7—O1581.07 (12)
O14i—V1—O1376.01 (11)O7—V7—O13105.69 (13)
O1—V1—V7107.79 (11)O17—V7—O1380.42 (11)
O8i—V1—V7127.90 (9)O19—V7—O13147.73 (12)
O17—V1—V737.92 (8)O15—V7—O1387.60 (11)
O14i—V1—V7115.42 (8)O7—V7—V1108.07 (11)
O13—V1—V741.31 (8)O17—V7—V138.21 (8)
O1—V1—V4i115.12 (11)O19—V7—V1125.77 (9)
O8i—V1—V4i120.49 (9)O15—V7—V1124.65 (8)
O17—V1—V4i111.59 (8)O13—V7—V142.43 (8)
O14i—V1—V4i38.60 (8)O7—V7—V6111.39 (11)
O13—V1—V4i38.03 (8)O17—V7—V6124.07 (9)
V7—V1—V4i76.90 (2)O19—V7—V638.64 (8)
O2—V2—O8103.78 (13)O15—V7—V642.46 (8)
O2—V2—O12102.55 (13)O13—V7—V6124.15 (8)
O8—V2—O1289.29 (12)V1—V7—V6140.50 (3)
O2—V2—O10100.00 (13)O101—S101—C101105.9 (2)
O8—V2—O1094.70 (12)O101—S101—C102105.4 (2)
O12—V2—O10155.45 (11)C101—S101—C10298.4 (3)
O2—V2—O11107.58 (13)O201—S201—C201103.6 (3)
O8—V2—O11148.60 (12)O201—S201—C202104.2 (2)
O12—V2—O1185.62 (12)C201—S201—C20299.0 (3)
O10—V2—O1178.39 (11)O301—S301—C301104.1 (2)
O2—V2—V3110.17 (10)O301—S301—C302107.3 (2)
O8—V2—V3123.74 (9)C301—S301—C30299.0 (3)
Symmetry code: (i) x+3/2, y+3/2, z+1.
Heptaammonium nitratotetradecavanadate dimethyl sulfoxide hexasolvate (4) top
Crystal data top
(NH4)7[V14O38(NO3)]·6C2H6OSF(000) = 3944
Mr = 1978.23Dx = 2.083 Mg m3
Monoclinic, C2/cCu Kα radiation, λ = 1.54178 Å
a = 19.3923 (7) ÅCell parameters from 9911 reflections
b = 24.9031 (9) Åθ = 3.6–72.8°
c = 14.5785 (5) ŵ = 19.38 mm1
β = 116.374 (1)°T = 90 K
V = 6307.6 (4) Å3Block, red
Z = 40.18 × 0.06 × 0.03 mm
Data collection top
Bruker D8 goniometer
diffractometer
6245 independent reflections
Radiation source: sealed tube5607 reflections with I > 2σ(I)
Detector resolution: 10.4167 pixels mm-1Rint = 0.065
ω scansθmax = 72.9°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2015)
h = 2224
Tmin = 0.32, Tmax = 0.64k = 3030
24260 measured reflectionsl = 1817
Refinement top
Refinement on F214 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.052H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.138 w = 1/[σ2(Fo2) + (0.0713P)2 + 26.5076P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.001
6245 reflectionsΔρmax = 2.47 e Å3
464 parametersΔρmin = 1.05 e Å3
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C1010.3159 (3)0.3072 (3)0.0605 (5)0.0561 (15)
H10A0.31110.27070.08210.084*
H10B0.27900.33080.06960.084*
H10C0.30520.30690.01180.084*
C1020.4595 (3)0.2899 (2)0.0828 (4)0.0417 (11)
H10D0.46020.25260.10490.063*
H10E0.43280.29170.00790.063*
H10F0.51240.30280.10670.063*
C2010.2816 (3)0.5353 (3)0.3433 (5)0.0603 (17)
H20A0.23040.55080.30380.090*
H20B0.27650.49850.36320.090*
H20C0.31010.55690.40490.090*
C2020.2782 (4)0.4849 (2)0.1758 (5)0.0644 (19)
H20D0.22760.49940.12950.097*
H20E0.30580.47450.13630.097*
H20F0.27150.45330.21130.097*
C3010.5296 (4)1.1335 (2)0.3742 (5)0.0490 (13)
H30A0.53851.15870.32900.073*
H30B0.47431.12630.34690.073*
H30C0.54841.14930.44270.073*
C3020.6745 (4)1.0962 (4)0.4612 (6)0.086 (3)
H30D0.69131.11990.42140.129*
H30E0.67441.11610.51910.129*
H30F0.70981.06560.48680.129*
N10.5548 (2)0.74974 (15)0.4071 (3)0.0274 (7)
N20.4757 (3)0.9443 (2)0.3871 (3)0.0419 (10)
N30.5046 (2)0.57496 (15)0.5062 (3)0.0283 (7)
N40.50000.4622 (3)0.25000.0467 (15)
O10.90631 (19)0.69409 (13)0.9141 (2)0.0367 (7)
O20.87044 (19)0.54839 (13)0.6644 (2)0.0352 (7)
O30.86960 (18)0.57370 (12)0.3869 (2)0.0333 (7)
O40.6582 (2)0.80429 (14)0.8013 (3)0.0380 (7)
O50.62811 (18)0.61269 (12)0.6961 (2)0.0310 (6)
O60.62730 (18)0.55657 (12)0.4347 (3)0.0344 (7)
O70.60536 (18)0.65166 (13)0.1488 (2)0.0340 (7)
O80.89874 (16)0.75564 (12)0.7546 (2)0.0287 (6)
O90.90382 (17)0.62897 (12)0.5638 (2)0.0298 (6)
O100.87858 (18)0.64925 (13)0.7290 (2)0.0332 (7)
O110.76996 (16)0.60089 (12)0.4722 (2)0.0265 (6)
O120.78633 (17)0.76324 (12)0.7863 (2)0.0278 (6)
O130.76742 (18)0.66031 (12)0.7779 (2)0.0306 (6)
O140.75892 (16)0.65484 (11)0.3061 (2)0.0262 (6)
O150.73774 (17)0.60987 (12)0.6126 (2)0.0284 (6)
O160.64799 (17)0.71894 (12)0.6797 (3)0.0324 (7)
O170.64201 (16)0.65165 (13)0.3519 (2)0.0317 (7)
O180.61448 (17)0.65276 (11)0.5163 (2)0.0275 (6)
O190.60790 (17)0.81703 (12)0.5968 (2)0.0305 (6)
O1010.4124 (2)0.38740 (13)0.0969 (3)0.0368 (7)
O2010.41004 (19)0.50976 (13)0.3374 (3)0.0394 (7)
O3010.5621 (3)1.03701 (16)0.4524 (3)0.0544 (10)
S1010.41029 (7)0.33103 (5)0.13547 (8)0.0332 (2)
S2010.33194 (7)0.53467 (4)0.26748 (9)0.0383 (3)
S3010.57964 (8)1.07230 (6)0.38166 (11)0.0477 (3)
V10.84840 (4)0.70103 (3)0.79648 (5)0.02557 (17)
V20.83987 (4)0.60764 (3)0.62123 (5)0.02597 (18)
V30.84201 (4)0.62556 (3)0.42602 (5)0.02467 (17)
V40.68084 (4)0.78623 (3)0.71250 (5)0.02388 (17)
V50.67594 (4)0.65262 (3)0.66017 (5)0.02548 (18)
V60.67051 (4)0.61344 (3)0.46614 (5)0.02427 (17)
V70.65552 (4)0.68437 (3)0.25099 (5)0.02345 (17)
N1A0.75000.75000.50000.0343 (12)
O1A0.7363 (6)0.7457 (6)0.5748 (9)0.070 (3)0.5
O2A0.7892 (6)0.7173 (6)0.4880 (14)0.085 (4)0.5
O3A0.7310 (7)0.7904 (4)0.4461 (10)0.081 (3)0.5
H10.572 (3)0.7217 (17)0.447 (4)0.049 (17)*
H20.577 (4)0.764 (3)0.373 (5)0.059 (19)*
H30.5060 (14)0.743 (2)0.369 (3)0.035 (14)*
H40.566 (4)0.772 (3)0.459 (4)0.07 (2)*
H50.507 (4)0.916 (2)0.408 (6)0.08 (3)*
H60.455 (3)0.944 (2)0.431 (3)0.040 (15)*
H70.504 (3)0.9734 (16)0.397 (5)0.053 (19)*
H80.444 (4)0.953 (3)0.323 (2)0.08 (2)*
H90.535 (3)0.600 (2)0.501 (6)0.07 (2)*
H100.536 (2)0.5509 (17)0.548 (3)0.033 (13)*
H110.477 (3)0.560 (2)0.447 (3)0.052 (17)*
H120.470 (3)0.588 (2)0.523 (4)0.045 (16)*
H130.477 (4)0.486 (2)0.273 (5)0.07 (2)*
H140.468 (3)0.441 (2)0.203 (3)0.046 (16)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1010.034 (3)0.074 (4)0.052 (3)0.012 (3)0.012 (3)0.010 (3)
C1020.051 (3)0.039 (3)0.038 (3)0.002 (2)0.022 (2)0.005 (2)
C2010.036 (3)0.092 (5)0.052 (4)0.002 (3)0.019 (3)0.015 (3)
C2020.049 (3)0.039 (3)0.060 (4)0.000 (3)0.017 (3)0.010 (3)
C3010.058 (3)0.044 (3)0.051 (3)0.006 (2)0.030 (3)0.006 (2)
C3020.054 (4)0.134 (8)0.073 (5)0.004 (4)0.031 (4)0.041 (5)
N10.0177 (16)0.0314 (18)0.0276 (19)0.0006 (15)0.0051 (15)0.0031 (15)
N20.035 (2)0.059 (3)0.031 (2)0.008 (2)0.014 (2)0.002 (2)
N30.0256 (18)0.0283 (18)0.031 (2)0.0001 (15)0.0124 (16)0.0016 (15)
N40.069 (5)0.037 (3)0.037 (4)0.0000.027 (4)0.000
O10.0374 (17)0.0406 (17)0.0241 (16)0.0015 (14)0.0064 (14)0.0002 (13)
O20.0380 (17)0.0327 (16)0.0325 (17)0.0094 (13)0.0135 (15)0.0064 (13)
O30.0351 (17)0.0328 (16)0.0340 (17)0.0043 (13)0.0171 (14)0.0033 (13)
O40.0396 (18)0.0493 (19)0.0343 (18)0.0060 (15)0.0248 (16)0.0016 (14)
O50.0326 (16)0.0301 (15)0.0311 (16)0.0040 (12)0.0149 (14)0.0002 (12)
O60.0346 (17)0.0319 (15)0.0407 (18)0.0085 (13)0.0204 (15)0.0049 (13)
O70.0346 (17)0.0369 (16)0.0201 (15)0.0053 (13)0.0027 (13)0.0004 (12)
O80.0228 (14)0.0325 (15)0.0301 (15)0.0040 (12)0.0112 (12)0.0039 (12)
O90.0233 (14)0.0370 (16)0.0270 (15)0.0001 (12)0.0094 (12)0.0002 (12)
O100.0280 (15)0.0395 (17)0.0276 (16)0.0011 (13)0.0082 (13)0.0065 (13)
O110.0252 (14)0.0305 (14)0.0238 (14)0.0009 (12)0.0108 (12)0.0013 (11)
O120.0262 (14)0.0301 (14)0.0283 (15)0.0012 (12)0.0130 (12)0.0010 (12)
O130.0322 (16)0.0316 (15)0.0284 (16)0.0013 (12)0.0140 (13)0.0006 (12)
O140.0249 (14)0.0275 (14)0.0260 (15)0.0007 (11)0.0111 (12)0.0009 (11)
O150.0261 (15)0.0333 (15)0.0258 (15)0.0031 (12)0.0116 (13)0.0008 (12)
O160.0273 (15)0.0249 (14)0.0464 (19)0.0041 (12)0.0177 (15)0.0054 (13)
O170.0206 (14)0.0474 (18)0.0255 (15)0.0048 (13)0.0089 (12)0.0108 (13)
O180.0277 (15)0.0281 (14)0.0283 (15)0.0026 (12)0.0138 (13)0.0032 (11)
O190.0256 (15)0.0325 (15)0.0336 (17)0.0008 (12)0.0134 (13)0.0010 (12)
O1010.050 (2)0.0317 (16)0.0411 (19)0.0010 (14)0.0317 (17)0.0001 (13)
O2010.0375 (18)0.0341 (17)0.0335 (17)0.0029 (14)0.0040 (15)0.0082 (13)
O3010.075 (3)0.052 (2)0.054 (2)0.002 (2)0.045 (2)0.0025 (18)
S1010.0355 (6)0.0392 (6)0.0282 (5)0.0030 (5)0.0172 (5)0.0017 (4)
S2010.0415 (6)0.0276 (5)0.0362 (6)0.0030 (4)0.0085 (5)0.0017 (4)
S3010.0570 (8)0.0513 (7)0.0468 (7)0.0111 (6)0.0340 (7)0.0053 (6)
V10.0226 (4)0.0298 (4)0.0205 (4)0.0003 (3)0.0062 (3)0.0003 (3)
V20.0256 (4)0.0275 (4)0.0227 (4)0.0054 (3)0.0088 (3)0.0030 (3)
V30.0219 (3)0.0277 (3)0.0241 (4)0.0025 (3)0.0100 (3)0.0004 (3)
V40.0232 (3)0.0276 (3)0.0246 (4)0.0002 (3)0.0140 (3)0.0011 (3)
V50.0260 (4)0.0246 (3)0.0287 (4)0.0025 (3)0.0147 (3)0.0020 (3)
V60.0235 (4)0.0257 (3)0.0245 (4)0.0018 (3)0.0114 (3)0.0013 (3)
V70.0219 (3)0.0267 (3)0.0186 (3)0.0004 (3)0.0062 (3)0.0015 (3)
N1A0.018 (2)0.036 (3)0.044 (3)0.001 (2)0.009 (2)0.009 (3)
O1A0.053 (6)0.098 (8)0.074 (7)0.030 (6)0.043 (6)0.041 (6)
O2A0.043 (5)0.087 (9)0.124 (12)0.001 (5)0.035 (7)0.057 (9)
O3A0.056 (6)0.053 (6)0.082 (8)0.005 (5)0.015 (6)0.014 (6)
Geometric parameters (Å, º) top
C101—S1011.767 (6)O10—V21.749 (3)
C101—H10A0.9800O10—V11.867 (3)
C101—H10B0.9800O11—V31.902 (3)
C101—H10C0.9800O11—V61.917 (3)
C102—S1011.789 (5)O11—V21.993 (3)
C102—H10D0.9800O12—V11.927 (3)
C102—H10E0.9800O12—V41.927 (3)
C102—H10F0.9800O12—V7i1.953 (3)
C201—S2011.770 (6)O13—V11.786 (3)
C201—H20A0.9800O13—V51.851 (3)
C201—H20B0.9800O14—V31.919 (3)
C201—H20C0.9800O14—V71.943 (3)
C202—S2011.781 (6)O14—V4i1.968 (3)
C202—H20D0.9800O15—V21.929 (3)
C202—H20E0.9800O15—V51.947 (3)
C202—H20F0.9800O15—V61.947 (3)
C301—S3011.785 (6)O16—V41.781 (3)
C301—H30A0.9800O16—V51.800 (3)
C301—H30B0.9800O17—V61.780 (3)
C301—H30C0.9800O17—V71.799 (3)
C302—S3011.785 (8)O18—V61.839 (3)
C302—H30D0.9800O18—V51.897 (3)
C302—H30E0.9800O19—V41.820 (3)
C302—H30F0.9800O19—V3i1.840 (3)
N1—H10.88 (2)O101—S1011.519 (3)
N1—H20.86 (2)O201—S2011.532 (4)
N1—H30.87 (2)O301—S3011.504 (4)
N1—H40.88 (2)V1—V7i2.9297 (10)
N2—H50.88 (2)V2—V32.8992 (10)
N2—H60.89 (2)V2—V63.0531 (10)
N2—H70.88 (2)V3—O19i1.840 (3)
N2—H80.88 (2)V3—V4i2.8816 (10)
N3—H90.88 (2)V4—O14i1.968 (3)
N3—H100.88 (2)V4—V3i2.8817 (10)
N3—H110.88 (2)V4—V7i3.0642 (9)
N3—H120.87 (2)V5—V62.9497 (10)
N4—H130.89 (2)V7—O8i1.808 (3)
N4—H140.88 (2)V7—O12i1.953 (3)
O1—V11.588 (3)V7—V1i2.9296 (10)
O2—V21.610 (3)V7—V4i3.0642 (9)
O3—V31.597 (3)N1A—O2Ai1.180 (9)
O4—V41.604 (3)N1A—O2A1.180 (9)
O5—V51.598 (3)N1A—O3A1.228 (12)
O6—V61.605 (3)N1A—O3Ai1.228 (12)
O7—V71.594 (3)N1A—O1Ai1.236 (10)
O8—V7i1.808 (3)N1A—O1A1.236 (10)
O8—V11.925 (3)O1A—O2Ai1.236 (19)
O9—V31.828 (3)O2A—O1Ai1.236 (19)
O9—V21.856 (3)
S101—C101—H10A109.5O2—V2—V6114.89 (13)
S101—C101—H10B109.5O10—V2—V6121.91 (11)
H10A—C101—H10B109.5O9—V2—V6111.53 (10)
S101—C101—H10C109.5O15—V2—V638.25 (9)
H10A—C101—H10C109.5O11—V2—V637.77 (8)
H10B—C101—H10C109.5V3—V2—V675.26 (2)
S101—C102—H10D109.5O3—V3—O9105.65 (15)
S101—C102—H10E109.5O3—V3—O19i106.05 (15)
H10D—C102—H10E109.5O9—V3—O19i91.24 (14)
S101—C102—H10F109.5O3—V3—O11106.27 (15)
H10D—C102—H10F109.5O9—V3—O1181.50 (13)
H10E—C102—H10F109.5O19i—V3—O11147.65 (13)
S201—C201—H20A109.5O3—V3—O14105.14 (15)
S201—C201—H20B109.5O9—V3—O14149.21 (13)
H20A—C201—H20B109.5O19i—V3—O1480.63 (13)
S201—C201—H20C109.5O11—V3—O1489.62 (12)
H20A—C201—H20C109.5O3—V3—V4i109.76 (12)
H20B—C201—H20C109.5O9—V3—V4i123.81 (10)
S201—C202—H20D109.5O19i—V3—V4i37.83 (10)
S201—C202—H20E109.5O11—V3—V4i125.85 (9)
H20D—C202—H20E109.5O14—V3—V4i42.81 (8)
S201—C202—H20F109.5O3—V3—V2112.27 (12)
H20D—C202—H20F109.5O9—V3—V238.42 (9)
H20E—C202—H20F109.5O19i—V3—V2122.42 (10)
S301—C301—H30A109.5O11—V3—V243.10 (9)
S301—C301—H30B109.5O14—V3—V2125.47 (9)
H30A—C301—H30B109.5V4i—V3—V2137.77 (3)
S301—C301—H30C109.5O4—V4—O16106.67 (17)
H30A—C301—H30C109.5O4—V4—O19104.53 (16)
H30B—C301—H30C109.5O16—V4—O1996.30 (15)
S301—C302—H30D109.5O4—V4—O12103.64 (15)
S301—C302—H30E109.5O16—V4—O1291.99 (14)
H30D—C302—H30E109.5O19—V4—O12146.87 (13)
S301—C302—H30F109.5O4—V4—O14i107.09 (16)
H30D—C302—H30F109.5O16—V4—O14i145.90 (13)
H30E—C302—H30F109.5O19—V4—O14i79.78 (13)
H1—N1—H2125 (6)O12—V4—O14i75.56 (12)
H1—N1—H3105 (5)O4—V4—V3i109.85 (13)
H2—N1—H3112 (6)O16—V4—V3i127.15 (12)
H1—N1—H493 (6)O19—V4—V3i38.31 (9)
H2—N1—H4104 (7)O12—V4—V3i114.34 (9)
H3—N1—H4117 (6)O14i—V4—V3i41.49 (9)
H5—N2—H6102 (6)O4—V4—V7i115.22 (13)
H5—N2—H7109 (7)O16—V4—V7i119.40 (10)
H6—N2—H7109 (6)O19—V4—V7i112.26 (10)
H5—N2—H8126 (7)O12—V4—V7i38.14 (9)
H6—N2—H8116 (6)O14i—V4—V7i38.14 (8)
H7—N2—H895 (6)V3i—V4—V7i76.38 (2)
H9—N3—H10105 (6)O5—V5—O16105.04 (15)
H9—N3—H11112 (6)O5—V5—O13102.54 (15)
H10—N3—H11109 (5)O16—V5—O1389.44 (14)
H9—N3—H12112 (6)O5—V5—O18101.08 (15)
H10—N3—H12116 (5)O16—V5—O1895.03 (14)
H11—N3—H12102 (5)O13—V5—O18153.90 (13)
H13—N4—H14114 (6)O5—V5—O15108.38 (14)
V7i—O8—V1103.35 (13)O16—V5—O15146.57 (14)
V3—O9—V2103.83 (15)O13—V5—O1584.21 (13)
V2—O10—V1140.61 (19)O18—V5—O1577.93 (12)
V3—O11—V6144.42 (17)O5—V5—V6109.25 (11)
V3—O11—V296.18 (13)O16—V5—V6124.77 (11)
V6—O11—V2102.69 (13)O13—V5—V6122.34 (10)
V1—O12—V4138.92 (17)O18—V5—V637.17 (9)
V1—O12—V7i98.07 (13)O15—V5—V640.77 (9)
V4—O12—V7i104.31 (14)O6—V6—O17107.40 (16)
V1—O13—V5127.96 (17)O6—V6—O18104.91 (14)
V3—O14—V7144.63 (16)O17—V6—O1895.45 (13)
V3—O14—V4i95.70 (13)O6—V6—O11104.86 (14)
V7—O14—V4i103.15 (13)O17—V6—O1191.03 (13)
V2—O15—V5140.29 (17)O18—V6—O11145.99 (13)
V2—O15—V6103.94 (13)O6—V6—O15106.43 (15)
V5—O15—V698.48 (13)O17—V6—O15145.96 (14)
V4—O16—V5143.98 (18)O18—V6—O1579.29 (13)
V6—O17—V7155.45 (18)O11—V6—O1576.84 (12)
V6—O18—V5104.28 (14)O6—V6—V5110.92 (12)
V4—O19—V3i103.86 (15)O17—V6—V5125.78 (11)
O101—S101—C101105.8 (3)O18—V6—V538.55 (9)
O101—S101—C102105.3 (2)O11—V6—V5113.78 (9)
C101—S101—C10298.4 (3)O15—V6—V540.75 (8)
O201—S201—C201104.2 (3)O6—V6—V2115.03 (13)
O201—S201—C202107.1 (2)O17—V6—V2120.20 (10)
C201—S201—C202100.0 (4)O18—V6—V2111.22 (10)
O301—S301—C301105.0 (2)O11—V6—V239.55 (9)
O301—S301—C302103.4 (3)O15—V6—V237.81 (8)
C301—S301—C30297.5 (4)V5—V6—V274.75 (2)
O1—V1—O13104.71 (16)O7—V7—O17106.40 (16)
O1—V1—O10104.90 (16)O7—V7—O8i106.19 (15)
O13—V1—O1089.34 (14)O17—V7—O8i96.75 (14)
O1—V1—O8101.82 (16)O7—V7—O14106.41 (15)
O13—V1—O8152.72 (14)O17—V7—O1489.35 (12)
O10—V1—O889.93 (14)O8i—V7—O14143.54 (13)
O1—V1—O12106.78 (16)O7—V7—O12i105.64 (15)
O13—V1—O1288.15 (13)O17—V7—O12i147.31 (14)
O10—V1—O12147.80 (14)O8i—V7—O12i80.33 (12)
O8—V1—O1278.17 (12)O14—V7—O12i75.55 (12)
O1—V1—V7i107.03 (13)O7—V7—V1i109.63 (12)
O13—V1—V7i126.05 (10)O17—V7—V1i129.51 (11)
O10—V1—V7i121.99 (11)O8i—V7—V1i39.74 (9)
O8—V1—V7i36.91 (9)O14—V7—V1i112.34 (9)
O12—V1—V7i41.30 (9)O12i—V7—V1i40.63 (8)
O2—V2—O10104.81 (16)O7—V7—V4i116.07 (12)
O2—V2—O9103.57 (15)O17—V7—V4i118.80 (10)
O10—V2—O997.43 (14)O8i—V7—V4i110.34 (10)
O2—V2—O15103.96 (15)O14—V7—V4i38.72 (8)
O10—V2—O1593.46 (14)O12i—V7—V4i37.55 (9)
O9—V2—O15146.61 (13)V1i—V7—V4i74.01 (2)
O2—V2—O11107.62 (15)O2Ai—N1A—O2A180.0
O10—V2—O11147.38 (14)O3A—N1A—O3Ai180.0
O9—V2—O1178.44 (12)O2Ai—N1A—O1Ai118.5 (9)
O15—V2—O1175.50 (12)O2A—N1A—O1Ai61.5 (9)
O2—V2—V3111.17 (12)O2Ai—N1A—O1A61.5 (9)
O10—V2—V3127.08 (11)O2A—N1A—O1A118.5 (9)
O9—V2—V337.74 (9)O1Ai—N1A—O1A180.0
O15—V2—V3113.17 (9)N1A—O1A—O2Ai57.0 (7)
O11—V2—V340.72 (8)N1A—O2A—O1Ai61.5 (8)
Symmetry code: (i) x+3/2, y+3/2, z+1.
 

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