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
CCDC references: 1850101; 1850100; 1850099; 1850098
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)]·CH3NO2 | Dx = 1.751 Mg m−3 |
Mr = 1877.60 | Mo Kα radiation, λ = 0.7107 Å |
Orthorhombic, Pna21 | Cell parameters from 31221 reflections |
a = 26.3672 (11) Å | θ = 3.1–27.5° |
b = 13.0801 (5) Å | µ = 1.59 mm−1 |
c = 20.6502 (8) Å | T = 83 K |
V = 7122.0 (5) Å3 | Prism, brown |
Z = 4 | 0.24 × 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-1 | Rint = 0.046 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: numerical (NUMABS; Rigaku, 1999) | h = −34→33 |
Tmin = 0.680, Tmax = 0.796 | k = −14→16 |
76477 measured reflections | l = −26→26 |
16085 independent reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-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 = 1.12 | Δρmax = 0.71 e Å−3 |
16085 reflections | Δρmin = −0.43 e Å−3 |
949 parameters | Absolute structure: Flack x determined using 6803 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013) |
7 restraints | Absolute 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C101 | 0.5092 (2) | 0.5559 (5) | 0.1721 (3) | 0.0320 (12) | |
H10A | 0.5343 | 0.6039 | 0.1907 | 0.038* | |
H10B | 0.5043 | 0.5000 | 0.2038 | 0.038* | |
C102 | 0.4592 (3) | 0.6120 (5) | 0.1639 (3) | 0.0440 (16) | |
H10C | 0.4480 | 0.6383 | 0.2059 | 0.066* | |
H10D | 0.4637 | 0.6690 | 0.1336 | 0.066* | |
H10E | 0.4336 | 0.5648 | 0.1467 | 0.066* | |
C103 | 0.5793 (2) | 0.4550 (6) | 0.1315 (3) | 0.0400 (15) | |
H10F | 0.6027 | 0.5055 | 0.1510 | 0.048* | |
H10G | 0.5702 | 0.4052 | 0.1656 | 0.048* | |
C104 | 0.6070 (3) | 0.3994 (8) | 0.0791 (4) | 0.073 (3) | |
H10H | 0.6372 | 0.3663 | 0.0974 | 0.109* | |
H10I | 0.5848 | 0.3475 | 0.0601 | 0.109* | |
H10J | 0.6174 | 0.4480 | 0.0455 | 0.109* | |
C105 | 0.4941 (2) | 0.4375 (4) | 0.0788 (3) | 0.0296 (12) | |
H10K | 0.4638 | 0.4768 | 0.0655 | 0.035* | |
H10L | 0.5099 | 0.4098 | 0.0390 | 0.035* | |
C106 | 0.4771 (3) | 0.3488 (5) | 0.1204 (3) | 0.0435 (15) | |
H10M | 0.4533 | 0.3062 | 0.0959 | 0.065* | |
H10N | 0.5066 | 0.3078 | 0.1328 | 0.065* | |
H10O | 0.4603 | 0.3749 | 0.1594 | 0.065* | |
C107 | 0.5429 (2) | 0.5918 (5) | 0.0611 (3) | 0.0316 (12) | |
H10P | 0.5104 | 0.6212 | 0.0459 | 0.038* | |
H10Q | 0.5594 | 0.5589 | 0.0234 | 0.038* | |
C108 | 0.5766 (2) | 0.6785 (5) | 0.0843 (3) | 0.0394 (14) | |
H10R | 0.5819 | 0.7273 | 0.0489 | 0.059* | |
H10S | 0.5603 | 0.7134 | 0.1208 | 0.059* | |
H10T | 0.6094 | 0.6509 | 0.0982 | 0.059* | |
C201 | 0.85630 (19) | 0.4283 (4) | 0.3478 (3) | 0.0278 (11) | |
H20A | 0.8313 | 0.4805 | 0.3615 | 0.033* | |
H20B | 0.8398 | 0.3851 | 0.3146 | 0.033* | |
C202 | 0.8685 (2) | 0.3618 (5) | 0.4056 (3) | 0.0399 (14) | |
H20C | 0.8373 | 0.3304 | 0.4220 | 0.060* | |
H20D | 0.8924 | 0.3080 | 0.3926 | 0.060* | |
H20E | 0.8839 | 0.4037 | 0.4397 | 0.060* | |
C203 | 0.8779 (2) | 0.5532 (4) | 0.2660 (3) | 0.0310 (12) | |
H20F | 0.8531 | 0.5987 | 0.2876 | 0.037* | |
H20G | 0.8590 | 0.5110 | 0.2342 | 0.037* | |
C204 | 0.9158 (3) | 0.6188 (6) | 0.2296 (4) | 0.0476 (17) | |
H20H | 0.8979 | 0.6616 | 0.1981 | 0.071* | |
H20I | 0.9341 | 0.6624 | 0.2603 | 0.071* | |
H20J | 0.9400 | 0.5746 | 0.2069 | 0.071* | |
C205 | 0.9309 (2) | 0.5428 (5) | 0.3667 (3) | 0.0417 (15) | |
H20K | 0.9454 | 0.4936 | 0.3981 | 0.050* | |
H20L | 0.9596 | 0.5771 | 0.3447 | 0.050* | |
C206 | 0.9012 (2) | 0.6228 (5) | 0.4040 (4) | 0.0502 (19) | |
H20M | 0.9236 | 0.6568 | 0.4351 | 0.075* | |
H20N | 0.8875 | 0.6735 | 0.3738 | 0.075* | |
H20O | 0.8732 | 0.5898 | 0.4273 | 0.075* | |
C207 | 0.9379 (2) | 0.4072 (5) | 0.2877 (3) | 0.0400 (15) | |
H20P | 0.9685 | 0.4449 | 0.2735 | 0.048* | |
H20Q | 0.9485 | 0.3594 | 0.3223 | 0.048* | |
C208 | 0.9190 (3) | 0.3461 (6) | 0.2320 (4) | 0.0490 (17) | |
H20R | 0.9457 | 0.2996 | 0.2171 | 0.074* | |
H20S | 0.8893 | 0.3063 | 0.2455 | 0.074* | |
H20T | 0.9094 | 0.3921 | 0.1966 | 0.074* | |
C301 | 0.5703 (4) | 0.9542 (7) | 0.5351 (4) | 0.033 (2) | 0.633 (8) |
H30A | 0.5973 | 0.9068 | 0.5496 | 0.039* | 0.633 (8) |
H30B | 0.5580 | 0.9910 | 0.5739 | 0.039* | 0.633 (8) |
C351 | 0.5589 (6) | 0.9480 (11) | 0.4658 (7) | 0.031 (4) | 0.367 (8) |
H35A | 0.5362 | 0.9799 | 0.4333 | 0.037* | 0.367 (8) |
H35B | 0.5802 | 0.8979 | 0.4422 | 0.037* | 0.367 (8) |
C302 | 0.5274 (3) | 0.8911 (5) | 0.5095 (4) | 0.0433 (16) | |
H30C | 0.5156 | 0.8443 | 0.5433 | 0.065* | 0.633 (8) |
H30D | 0.4995 | 0.9361 | 0.4964 | 0.065* | 0.633 (8) |
H30E | 0.5390 | 0.8516 | 0.4720 | 0.065* | 0.633 (8) |
H35C | 0.5074 | 0.8410 | 0.4850 | 0.065* | 0.367 (8) |
H35D | 0.5487 | 0.8555 | 0.5411 | 0.065* | 0.367 (8) |
H35E | 0.5045 | 0.9380 | 0.5322 | 0.065* | 0.367 (8) |
C303 | 0.6235 (3) | 0.9692 (6) | 0.4361 (4) | 0.0252 (18) | 0.633 (8) |
H30F | 0.6511 | 0.9301 | 0.4570 | 0.030* | 0.633 (8) |
H30G | 0.5997 | 0.9189 | 0.4171 | 0.030* | 0.633 (8) |
C353 | 0.6169 (7) | 1.0892 (12) | 0.4372 (7) | 0.033 (4) | 0.367 (8) |
H35F | 0.6412 | 1.1389 | 0.4558 | 0.040* | 0.367 (8) |
H35G | 0.5897 | 1.1290 | 0.4158 | 0.040* | 0.367 (8) |
C304 | 0.6445 (2) | 1.0274 (5) | 0.3853 (3) | 0.0365 (13) | |
H30H | 0.6616 | 0.9817 | 0.3546 | 0.055* | 0.633 (8) |
H30I | 0.6175 | 1.0648 | 0.3630 | 0.055* | 0.633 (8) |
H30J | 0.6691 | 1.0760 | 0.4031 | 0.055* | 0.633 (8) |
H35H | 0.6581 | 1.0738 | 0.3523 | 0.055* | 0.367 (8) |
H35I | 0.6725 | 0.9893 | 0.4053 | 0.055* | 0.367 (8) |
H35J | 0.6208 | 0.9793 | 0.3651 | 0.055* | 0.367 (8) |
C305 | 0.5551 (4) | 1.0956 (7) | 0.4559 (5) | 0.034 (2) | 0.633 (8) |
H30K | 0.5372 | 1.0516 | 0.4242 | 0.040* | 0.633 (8) |
H30L | 0.5729 | 1.1495 | 0.4311 | 0.040* | 0.633 (8) |
C355 | 0.5609 (7) | 1.1099 (12) | 0.5307 (9) | 0.038 (4) | 0.367 (8) |
H35K | 0.5511 | 1.0769 | 0.5720 | 0.045* | 0.367 (8) |
H35L | 0.5824 | 1.1696 | 0.5416 | 0.045* | 0.367 (8) |
C306 | 0.5156 (2) | 1.1465 (5) | 0.4994 (3) | 0.0379 (14) | |
H30M | 0.4920 | 1.1862 | 0.4727 | 0.057* | 0.633 (8) |
H30N | 0.4968 | 1.0939 | 0.5232 | 0.057* | 0.633 (8) |
H30O | 0.5327 | 1.1921 | 0.5301 | 0.057* | 0.633 (8) |
H35M | 0.4979 | 1.1942 | 0.5282 | 0.057* | 0.367 (8) |
H35N | 0.5247 | 1.1816 | 0.4591 | 0.057* | 0.367 (8) |
H35O | 0.4933 | 1.0886 | 0.4895 | 0.057* | 0.367 (8) |
C307 | 0.6307 (4) | 1.0988 (7) | 0.5250 (5) | 0.035 (2) | 0.633 (8) |
H30P | 0.6113 | 1.1404 | 0.5565 | 0.042* | 0.633 (8) |
H30Q | 0.6452 | 1.1466 | 0.4929 | 0.042* | 0.633 (8) |
C357 | 0.6315 (7) | 0.9844 (12) | 0.5373 (8) | 0.037 (4) | 0.367 (8) |
H35P | 0.6124 | 0.9601 | 0.5756 | 0.045* | 0.367 (8) |
H35Q | 0.6465 | 0.9235 | 0.5163 | 0.045* | 0.367 (8) |
C308 | 0.6737 (3) | 1.0504 (6) | 0.5605 (4) | 0.0549 (19) | |
H30R | 0.6945 | 1.1036 | 0.5808 | 0.082* | 0.633 (8) |
H30S | 0.6603 | 1.0047 | 0.5941 | 0.082* | 0.633 (8) |
H30T | 0.6945 | 1.0110 | 0.5301 | 0.082* | 0.633 (8) |
H35R | 0.6952 | 1.0114 | 0.5904 | 0.082* | 0.367 (8) |
H35S | 0.6939 | 1.0732 | 0.5235 | 0.082* | 0.367 (8) |
H35T | 0.6597 | 1.1100 | 0.5831 | 0.082* | 0.367 (8) |
C401 | 0.3433 (2) | 0.5922 (4) | 0.3322 (3) | 0.0310 (12) | |
H40A | 0.3594 | 0.6404 | 0.3629 | 0.037* | |
H40B | 0.3707 | 0.5524 | 0.3113 | 0.037* | |
C402 | 0.3164 (2) | 0.6529 (5) | 0.2810 (3) | 0.0360 (13) | |
H40C | 0.3407 | 0.6978 | 0.2590 | 0.054* | |
H40D | 0.3011 | 0.6062 | 0.2494 | 0.054* | |
H40E | 0.2897 | 0.6944 | 0.3011 | 0.054* | |
C403 | 0.3446 (2) | 0.4705 (4) | 0.4203 (3) | 0.0328 (12) | |
H40F | 0.3707 | 0.4299 | 0.3974 | 0.039* | |
H40G | 0.3622 | 0.5255 | 0.4443 | 0.039* | |
C404 | 0.3179 (3) | 0.4018 (5) | 0.4685 (3) | 0.0448 (16) | |
H40H | 0.3428 | 0.3737 | 0.4989 | 0.067* | |
H40I | 0.2926 | 0.4415 | 0.4924 | 0.067* | |
H40J | 0.3011 | 0.3458 | 0.4454 | 0.067* | |
C405 | 0.2872 (2) | 0.4375 (4) | 0.3271 (3) | 0.0345 (13) | |
H40K | 0.2654 | 0.3930 | 0.3541 | 0.041* | |
H40L | 0.2651 | 0.4714 | 0.2949 | 0.041* | |
C406 | 0.3246 (3) | 0.3710 (5) | 0.2915 (3) | 0.0441 (16) | |
H40M | 0.3061 | 0.3210 | 0.2651 | 0.066* | |
H40N | 0.3458 | 0.4136 | 0.2634 | 0.066* | |
H40O | 0.3461 | 0.3350 | 0.3228 | 0.066* | |
C407 | 0.2661 (2) | 0.5740 (5) | 0.4017 (3) | 0.0360 (13) | |
H40P | 0.2441 | 0.5225 | 0.4229 | 0.043* | |
H40Q | 0.2458 | 0.6072 | 0.3673 | 0.043* | |
C408 | 0.2803 (3) | 0.6546 (5) | 0.4517 (3) | 0.0465 (16) | |
H40R | 0.2494 | 0.6857 | 0.4692 | 0.070* | |
H40S | 0.2995 | 0.6225 | 0.4868 | 0.070* | |
H40T | 0.3012 | 0.7075 | 0.4311 | 0.070* | |
C501 | 0.7064 (2) | 0.4383 (4) | 0.5442 (3) | 0.0298 (12) | |
H50A | 0.6824 | 0.4851 | 0.5223 | 0.036* | |
H50B | 0.7244 | 0.3992 | 0.5102 | 0.036* | |
C502 | 0.6763 (3) | 0.3643 (5) | 0.5852 (3) | 0.0421 (15) | |
H50C | 0.6525 | 0.3266 | 0.5577 | 0.063* | |
H50D | 0.6996 | 0.3161 | 0.6063 | 0.063* | |
H50E | 0.6575 | 0.4022 | 0.6183 | 0.063* | |
C503 | 0.7192 (2) | 0.5698 (4) | 0.6312 (3) | 0.0324 (13) | |
H50F | 0.7457 | 0.6089 | 0.6544 | 0.039* | |
H50G | 0.7021 | 0.5254 | 0.6634 | 0.039* | |
C504 | 0.6801 (3) | 0.6454 (5) | 0.6043 (3) | 0.0424 (15) | |
H50H | 0.6657 | 0.6855 | 0.6400 | 0.064* | |
H50I | 0.6966 | 0.6915 | 0.5734 | 0.064* | |
H50J | 0.6529 | 0.6077 | 0.5824 | 0.064* | |
C505 | 0.7813 (2) | 0.4336 (4) | 0.6180 (3) | 0.0305 (12) | |
H50K | 0.8047 | 0.4774 | 0.6433 | 0.037* | |
H50L | 0.7617 | 0.3920 | 0.6492 | 0.037* | |
C506 | 0.8120 (3) | 0.3636 (5) | 0.5766 (3) | 0.0414 (15) | |
H50M | 0.8344 | 0.3224 | 0.6040 | 0.062* | |
H50N | 0.7893 | 0.3185 | 0.5522 | 0.062* | |
H50O | 0.8324 | 0.4041 | 0.5463 | 0.062* | |
C507 | 0.7716 (2) | 0.5660 (4) | 0.5306 (3) | 0.0296 (12) | |
H50P | 0.7873 | 0.5195 | 0.4986 | 0.036* | |
H50Q | 0.7458 | 0.6073 | 0.5075 | 0.036* | |
C508 | 0.8119 (3) | 0.6368 (5) | 0.5563 (3) | 0.0416 (15) | |
H50R | 0.8270 | 0.6750 | 0.5203 | 0.062* | |
H50S | 0.7966 | 0.6848 | 0.5871 | 0.062* | |
H50T | 0.8382 | 0.5968 | 0.5781 | 0.062* | |
C601 | 0.5839 (2) | −0.0030 (4) | 0.2003 (3) | 0.0319 (12) | |
H60A | 0.5624 | 0.0021 | 0.2389 | 0.048* | 0.63 (3) |
H60B | 0.5978 | −0.0722 | 0.1971 | 0.048* | 0.63 (3) |
H60C | 0.6117 | 0.0464 | 0.2036 | 0.048* | 0.63 (3) |
H65A | 0.6193 | 0.0108 | 0.1890 | 0.048* | 0.37 (3) |
H65B | 0.5685 | 0.0591 | 0.2183 | 0.048* | 0.37 (3) |
H65C | 0.5824 | −0.0578 | 0.2326 | 0.048* | 0.37 (3) |
N601 | 0.5537 (5) | 0.0192 (19) | 0.1428 (7) | 0.052 (5) | 0.63 (3) |
O601 | 0.5726 (5) | 0.017 (2) | 0.0892 (7) | 0.082 (6) | 0.63 (3) |
O602 | 0.5096 (3) | 0.046 (2) | 0.1532 (5) | 0.091 (8) | 0.63 (3) |
N651 | 0.5577 (10) | −0.032 (2) | 0.1457 (13) | 0.039 (5) | 0.37 (3) |
O651 | 0.5817 (9) | −0.039 (2) | 0.0950 (12) | 0.054 (6) | 0.37 (3) |
O652 | 0.5130 (7) | −0.053 (3) | 0.1481 (8) | 0.082 (12) | 0.37 (3) |
N1A | 0.61625 (15) | 0.5047 (3) | 0.29278 (19) | 0.0201 (8) | |
N2A | 0.5743 (8) | 0.5371 (13) | 0.3026 (16) | 0.020 (4) | 0.40 (7) |
N3A | 0.6583 (8) | 0.4747 (19) | 0.2904 (15) | 0.029 (4) | 0.40 (7) |
N2B | 0.5863 (10) | 0.5348 (9) | 0.3279 (19) | 0.034 (6) | 0.60 (7) |
N3B | 0.6510 (9) | 0.4690 (10) | 0.264 (2) | 0.042 (7) | 0.60 (7) |
N101 | 0.53142 (17) | 0.5106 (3) | 0.1106 (2) | 0.0279 (10) | |
N201 | 0.90081 (16) | 0.4831 (3) | 0.3163 (3) | 0.0306 (10) | |
N301 | 0.59417 (17) | 1.0316 (3) | 0.4906 (2) | 0.0280 (10) | |
N401 | 0.31002 (16) | 0.5191 (3) | 0.3703 (2) | 0.0280 (9) | |
N501 | 0.74488 (18) | 0.5019 (3) | 0.5812 (2) | 0.0272 (10) | |
O1 | 0.44686 (12) | 0.6421 (3) | 0.41852 (18) | 0.0246 (7) | |
O2 | 0.54199 (12) | 0.8770 (3) | 0.33350 (17) | 0.0234 (7) | |
O3 | 0.67574 (13) | 0.8658 (3) | 0.25573 (18) | 0.0252 (7) | |
O4 | 0.77593 (14) | 0.6810 (3) | 0.18415 (18) | 0.0269 (8) | |
O5 | 0.79632 (13) | 0.3648 (3) | 0.19207 (18) | 0.0269 (8) | |
O6 | 0.68581 (13) | 0.1277 (3) | 0.23276 (17) | 0.0228 (7) | |
O7 | 0.55089 (13) | 0.1453 (3) | 0.31229 (17) | 0.0231 (7) | |
O8 | 0.44961 (12) | 0.3237 (3) | 0.37863 (19) | 0.0266 (8) | |
O9 | 0.62889 (13) | 0.7450 (2) | 0.48184 (17) | 0.0212 (7) | |
O10 | 0.78154 (13) | 0.6233 (3) | 0.38230 (17) | 0.0230 (7) | |
O11 | 0.72157 (13) | 0.2435 (3) | 0.41231 (17) | 0.0229 (7) | |
O12 | 0.57042 (13) | 0.3630 (3) | 0.50779 (16) | 0.0218 (7) | |
O13 | 0.49647 (12) | 0.6963 (3) | 0.30613 (17) | 0.0225 (7) | |
O14 | 0.58624 (13) | 0.7592 (3) | 0.24087 (17) | 0.0221 (7) | |
O15 | 0.67165 (14) | 0.6857 (3) | 0.18654 (17) | 0.0254 (8) | |
O16 | 0.72513 (13) | 0.5059 (3) | 0.15671 (17) | 0.0235 (7) | |
O17 | 0.69613 (14) | 0.3123 (3) | 0.17387 (17) | 0.0235 (7) | |
O18 | 0.60098 (13) | 0.2491 (3) | 0.21917 (16) | 0.0212 (7) | |
O19 | 0.51500 (13) | 0.3312 (3) | 0.27384 (17) | 0.0247 (7) | |
O20 | 0.46441 (12) | 0.5060 (2) | 0.32053 (16) | 0.0205 (7) | |
O21 | 0.54895 (12) | 0.6861 (2) | 0.40239 (16) | 0.0189 (7) | |
O22 | 0.62604 (12) | 0.7415 (2) | 0.34636 (16) | 0.0185 (7) | |
O23 | 0.71085 (12) | 0.6751 (2) | 0.29239 (15) | 0.0191 (7) | |
O24 | 0.75416 (12) | 0.5137 (2) | 0.26934 (16) | 0.0202 (7) | |
O25 | 0.72402 (12) | 0.3135 (3) | 0.28536 (16) | 0.0203 (7) | |
O26 | 0.64061 (12) | 0.2612 (2) | 0.32529 (16) | 0.0185 (7) | |
O27 | 0.55636 (12) | 0.3279 (2) | 0.37858 (16) | 0.0189 (7) | |
O28 | 0.51764 (12) | 0.4862 (2) | 0.41649 (16) | 0.0191 (7) | |
O29 | 0.68303 (13) | 0.6097 (3) | 0.40567 (17) | 0.0221 (7) | |
O30 | 0.64398 (12) | 0.3843 (3) | 0.42254 (16) | 0.0217 (7) | |
O31 | 0.60099 (12) | 0.5527 (2) | 0.47046 (16) | 0.0193 (7) | |
O32 | 0.73551 (12) | 0.4380 (2) | 0.38378 (16) | 0.0190 (7) | |
V1 | 0.49275 (3) | 0.60404 (6) | 0.37400 (4) | 0.01834 (16) | |
V2 | 0.55565 (3) | 0.75935 (6) | 0.31894 (4) | 0.01749 (16) | |
V3 | 0.65369 (3) | 0.75203 (6) | 0.26184 (4) | 0.01827 (16) | |
V4 | 0.72825 (3) | 0.61615 (6) | 0.20811 (4) | 0.01968 (17) | |
V5 | 0.74101 (3) | 0.40263 (6) | 0.21281 (4) | 0.01995 (17) | |
V6 | 0.66843 (3) | 0.24481 (6) | 0.23926 (4) | 0.01739 (16) | |
V7 | 0.57096 (3) | 0.25781 (6) | 0.29802 (4) | 0.01776 (16) | |
V8 | 0.49418 (3) | 0.39189 (6) | 0.34844 (4) | 0.01821 (16) | |
V9 | 0.61793 (3) | 0.66140 (6) | 0.42709 (4) | 0.01673 (16) | |
V10 | 0.73046 (3) | 0.57422 (6) | 0.35346 (4) | 0.01784 (16) | |
V11 | 0.69676 (3) | 0.33332 (6) | 0.36960 (4) | 0.01648 (16) | |
V12 | 0.58328 (3) | 0.41967 (6) | 0.44091 (4) | 0.01761 (16) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C101 | 0.037 (3) | 0.039 (3) | 0.019 (3) | −0.004 (3) | −0.005 (2) | 0.002 (2) |
C102 | 0.048 (4) | 0.057 (4) | 0.028 (3) | 0.018 (3) | −0.008 (3) | −0.009 (3) |
C103 | 0.032 (3) | 0.062 (4) | 0.027 (3) | 0.013 (3) | −0.003 (2) | 0.011 (3) |
C104 | 0.059 (5) | 0.121 (8) | 0.038 (4) | 0.054 (5) | 0.004 (4) | 0.019 (4) |
C105 | 0.037 (3) | 0.033 (3) | 0.019 (2) | 0.000 (2) | −0.003 (2) | −0.002 (2) |
C106 | 0.065 (4) | 0.033 (3) | 0.032 (3) | −0.008 (3) | −0.005 (3) | 0.004 (3) |
C107 | 0.031 (3) | 0.042 (3) | 0.022 (3) | −0.004 (2) | −0.005 (2) | 0.007 (2) |
C108 | 0.033 (3) | 0.051 (4) | 0.034 (3) | −0.012 (3) | −0.006 (2) | 0.013 (3) |
C201 | 0.018 (2) | 0.027 (3) | 0.038 (3) | 0.002 (2) | 0.001 (2) | 0.003 (2) |
C202 | 0.039 (3) | 0.036 (3) | 0.044 (4) | 0.006 (3) | 0.009 (3) | 0.003 (3) |
C203 | 0.024 (2) | 0.029 (3) | 0.040 (3) | 0.001 (2) | 0.000 (2) | 0.010 (2) |
C204 | 0.037 (3) | 0.049 (4) | 0.056 (4) | −0.010 (3) | 0.004 (3) | 0.018 (3) |
C205 | 0.019 (2) | 0.055 (4) | 0.051 (4) | −0.004 (2) | −0.007 (3) | −0.005 (3) |
C206 | 0.028 (3) | 0.043 (4) | 0.079 (5) | −0.005 (3) | −0.016 (3) | −0.017 (4) |
C207 | 0.021 (3) | 0.052 (4) | 0.047 (4) | 0.014 (3) | 0.008 (3) | 0.002 (3) |
C208 | 0.040 (3) | 0.052 (4) | 0.055 (4) | 0.021 (3) | 0.008 (3) | 0.003 (3) |
C301 | 0.038 (5) | 0.032 (5) | 0.028 (5) | 0.005 (4) | 0.008 (4) | 0.005 (4) |
C351 | 0.037 (8) | 0.026 (7) | 0.029 (8) | 0.004 (6) | −0.012 (7) | −0.003 (6) |
C302 | 0.047 (4) | 0.031 (3) | 0.053 (4) | −0.003 (3) | 0.005 (3) | 0.006 (3) |
C303 | 0.018 (3) | 0.027 (4) | 0.031 (4) | −0.004 (3) | −0.005 (3) | 0.000 (3) |
C353 | 0.046 (9) | 0.028 (7) | 0.026 (8) | −0.003 (7) | 0.002 (7) | 0.003 (6) |
C304 | 0.032 (3) | 0.039 (3) | 0.038 (3) | 0.009 (3) | −0.001 (3) | 0.002 (3) |
C305 | 0.039 (5) | 0.029 (5) | 0.033 (5) | 0.000 (4) | 0.003 (4) | 0.006 (4) |
C355 | 0.051 (10) | 0.025 (7) | 0.038 (9) | −0.001 (7) | 0.002 (8) | −0.006 (7) |
C306 | 0.040 (3) | 0.031 (3) | 0.042 (3) | 0.000 (3) | 0.007 (3) | 0.001 (3) |
C307 | 0.038 (5) | 0.036 (5) | 0.030 (5) | −0.002 (4) | −0.005 (4) | −0.010 (4) |
C357 | 0.050 (10) | 0.032 (8) | 0.030 (8) | 0.003 (7) | −0.019 (7) | −0.009 (7) |
C308 | 0.052 (4) | 0.069 (5) | 0.044 (4) | −0.006 (4) | −0.019 (3) | −0.006 (4) |
C401 | 0.024 (3) | 0.029 (3) | 0.041 (3) | −0.003 (2) | −0.001 (2) | −0.001 (2) |
C402 | 0.035 (3) | 0.036 (3) | 0.038 (3) | −0.002 (3) | −0.002 (3) | 0.004 (2) |
C403 | 0.027 (3) | 0.026 (3) | 0.045 (3) | −0.002 (2) | −0.013 (2) | 0.003 (2) |
C404 | 0.050 (4) | 0.040 (3) | 0.045 (4) | −0.009 (3) | −0.015 (3) | 0.011 (3) |
C405 | 0.035 (3) | 0.035 (3) | 0.034 (3) | −0.011 (2) | −0.012 (3) | 0.000 (2) |
C406 | 0.058 (4) | 0.033 (3) | 0.041 (4) | 0.005 (3) | −0.011 (3) | −0.005 (3) |
C407 | 0.031 (3) | 0.041 (3) | 0.036 (3) | 0.003 (2) | 0.000 (2) | 0.003 (3) |
C408 | 0.053 (4) | 0.037 (3) | 0.049 (4) | 0.014 (3) | 0.009 (3) | −0.004 (3) |
C501 | 0.035 (3) | 0.031 (3) | 0.023 (3) | 0.001 (2) | −0.012 (2) | −0.002 (2) |
C502 | 0.044 (4) | 0.040 (3) | 0.042 (3) | −0.010 (3) | −0.022 (3) | 0.011 (3) |
C503 | 0.041 (3) | 0.037 (3) | 0.020 (3) | 0.006 (3) | −0.009 (2) | −0.008 (2) |
C504 | 0.052 (4) | 0.041 (3) | 0.034 (3) | 0.014 (3) | −0.011 (3) | −0.009 (3) |
C505 | 0.035 (3) | 0.035 (3) | 0.022 (3) | 0.004 (2) | −0.008 (2) | 0.002 (2) |
C506 | 0.046 (4) | 0.040 (3) | 0.038 (3) | 0.013 (3) | 0.003 (3) | 0.003 (3) |
C507 | 0.038 (3) | 0.032 (3) | 0.019 (2) | 0.006 (2) | −0.010 (2) | 0.000 (2) |
C508 | 0.047 (4) | 0.043 (3) | 0.035 (3) | −0.009 (3) | −0.007 (3) | 0.002 (3) |
C601 | 0.030 (3) | 0.029 (3) | 0.036 (3) | 0.005 (2) | −0.002 (2) | 0.003 (2) |
N601 | 0.027 (5) | 0.104 (14) | 0.027 (5) | −0.002 (8) | −0.003 (4) | 0.008 (9) |
O601 | 0.039 (5) | 0.174 (19) | 0.033 (5) | 0.015 (9) | 0.002 (4) | 0.018 (9) |
O602 | 0.027 (4) | 0.21 (2) | 0.036 (5) | 0.012 (7) | 0.001 (4) | 0.017 (8) |
N651 | 0.028 (9) | 0.052 (13) | 0.036 (10) | −0.008 (10) | 0.004 (7) | 0.004 (11) |
O651 | 0.043 (11) | 0.085 (15) | 0.036 (10) | −0.008 (9) | 0.004 (8) | −0.019 (10) |
O652 | 0.025 (8) | 0.17 (3) | 0.050 (9) | −0.041 (12) | 0.002 (6) | −0.003 (13) |
N1A | 0.0189 (18) | 0.022 (2) | 0.0194 (19) | −0.0017 (15) | −0.0014 (15) | 0.0020 (16) |
N2A | 0.012 (5) | 0.031 (7) | 0.016 (10) | 0.009 (5) | −0.009 (6) | 0.001 (6) |
N3A | 0.023 (5) | 0.043 (9) | 0.020 (10) | 0.014 (6) | 0.003 (7) | −0.014 (7) |
N2B | 0.027 (8) | 0.030 (5) | 0.044 (13) | 0.000 (4) | 0.015 (9) | −0.001 (5) |
N3B | 0.036 (7) | 0.021 (5) | 0.069 (18) | −0.008 (4) | 0.035 (9) | −0.006 (7) |
N101 | 0.030 (2) | 0.037 (2) | 0.017 (2) | 0.0003 (19) | −0.0056 (18) | 0.0036 (19) |
N201 | 0.0128 (18) | 0.032 (2) | 0.047 (3) | 0.0040 (17) | 0.0004 (19) | 0.007 (2) |
N301 | 0.033 (2) | 0.026 (2) | 0.025 (2) | −0.0037 (19) | −0.0051 (19) | 0.0048 (18) |
N401 | 0.023 (2) | 0.029 (2) | 0.032 (2) | −0.0040 (17) | −0.0084 (19) | 0.0002 (19) |
N501 | 0.033 (2) | 0.030 (2) | 0.018 (2) | 0.0024 (19) | −0.0090 (18) | 0.0010 (17) |
O1 | 0.0163 (15) | 0.0281 (18) | 0.0293 (19) | 0.0023 (14) | 0.0009 (14) | −0.0017 (15) |
O2 | 0.0177 (16) | 0.0243 (17) | 0.0281 (19) | 0.0013 (13) | −0.0016 (14) | 0.0028 (14) |
O3 | 0.0265 (18) | 0.0243 (17) | 0.0248 (18) | −0.0016 (15) | 0.0048 (15) | 0.0048 (15) |
O4 | 0.0276 (19) | 0.0253 (18) | 0.0278 (19) | −0.0030 (15) | 0.0078 (15) | −0.0021 (15) |
O5 | 0.0218 (17) | 0.0307 (19) | 0.0283 (19) | −0.0002 (15) | 0.0085 (15) | −0.0032 (16) |
O6 | 0.0218 (16) | 0.0221 (16) | 0.0245 (18) | 0.0015 (14) | 0.0002 (14) | −0.0039 (14) |
O7 | 0.0192 (16) | 0.0225 (17) | 0.0276 (18) | −0.0046 (14) | 0.0026 (14) | −0.0047 (15) |
O8 | 0.0177 (16) | 0.0249 (17) | 0.037 (2) | −0.0032 (13) | 0.0014 (15) | −0.0006 (16) |
O9 | 0.0228 (17) | 0.0222 (17) | 0.0187 (16) | 0.0016 (13) | −0.0006 (14) | −0.0031 (13) |
O10 | 0.0195 (16) | 0.0232 (17) | 0.0264 (18) | 0.0008 (13) | −0.0054 (14) | −0.0031 (15) |
O11 | 0.0235 (18) | 0.0231 (17) | 0.0223 (18) | 0.0028 (13) | −0.0045 (14) | 0.0019 (14) |
O12 | 0.0242 (17) | 0.0229 (17) | 0.0183 (16) | 0.0007 (14) | 0.0014 (14) | 0.0007 (14) |
O13 | 0.0207 (16) | 0.0261 (17) | 0.0207 (17) | −0.0017 (14) | −0.0051 (13) | 0.0027 (14) |
O14 | 0.0178 (16) | 0.0307 (18) | 0.0179 (16) | 0.0033 (14) | −0.0011 (14) | 0.0001 (14) |
O15 | 0.0268 (18) | 0.0333 (19) | 0.0162 (16) | 0.0053 (15) | 0.0006 (14) | −0.0008 (15) |
O16 | 0.0254 (18) | 0.0226 (17) | 0.0223 (17) | −0.0020 (14) | 0.0041 (14) | −0.0008 (14) |
O17 | 0.0265 (18) | 0.0242 (17) | 0.0197 (17) | −0.0048 (14) | 0.0014 (14) | −0.0040 (14) |
O18 | 0.0202 (17) | 0.0278 (18) | 0.0155 (16) | 0.0005 (13) | −0.0026 (13) | −0.0023 (13) |
O19 | 0.0202 (16) | 0.0316 (19) | 0.0221 (18) | 0.0046 (14) | −0.0058 (14) | −0.0068 (15) |
O20 | 0.0171 (15) | 0.0212 (16) | 0.0231 (17) | 0.0011 (13) | −0.0027 (14) | −0.0015 (14) |
O21 | 0.0168 (15) | 0.0218 (16) | 0.0182 (16) | 0.0013 (13) | −0.0015 (13) | −0.0001 (13) |
O22 | 0.0143 (15) | 0.0253 (17) | 0.0158 (15) | 0.0002 (12) | 0.0004 (13) | 0.0022 (13) |
O23 | 0.0154 (15) | 0.0245 (17) | 0.0174 (16) | 0.0019 (13) | 0.0017 (13) | 0.0001 (13) |
O24 | 0.0196 (16) | 0.0199 (16) | 0.0211 (17) | −0.0005 (13) | 0.0042 (13) | 0.0004 (13) |
O25 | 0.0164 (15) | 0.0232 (17) | 0.0213 (17) | 0.0000 (13) | 0.0012 (13) | −0.0026 (14) |
O26 | 0.0159 (15) | 0.0228 (16) | 0.0168 (16) | −0.0013 (13) | 0.0007 (13) | −0.0015 (13) |
O27 | 0.0180 (15) | 0.0196 (15) | 0.0190 (16) | 0.0001 (12) | 0.0009 (13) | −0.0022 (13) |
O28 | 0.0168 (15) | 0.0188 (15) | 0.0217 (16) | 0.0012 (12) | −0.0021 (13) | 0.0003 (13) |
O29 | 0.0198 (16) | 0.0247 (17) | 0.0217 (17) | 0.0055 (14) | 0.0005 (14) | 0.0011 (14) |
O30 | 0.0195 (16) | 0.0270 (18) | 0.0186 (16) | 0.0020 (14) | −0.0012 (14) | −0.0064 (14) |
O31 | 0.0197 (16) | 0.0205 (16) | 0.0176 (16) | −0.0001 (13) | −0.0014 (13) | 0.0001 (13) |
O32 | 0.0149 (15) | 0.0197 (16) | 0.0225 (17) | 0.0006 (12) | −0.0013 (13) | −0.0006 (14) |
V1 | 0.0137 (3) | 0.0206 (4) | 0.0207 (4) | 0.0005 (3) | −0.0002 (3) | 0.0012 (3) |
V2 | 0.0138 (3) | 0.0217 (4) | 0.0170 (4) | 0.0013 (3) | −0.0005 (3) | 0.0011 (3) |
V3 | 0.0168 (4) | 0.0209 (4) | 0.0172 (4) | 0.0017 (3) | 0.0013 (3) | 0.0008 (3) |
V4 | 0.0184 (4) | 0.0221 (4) | 0.0186 (4) | 0.0003 (3) | 0.0038 (3) | −0.0002 (3) |
V5 | 0.0177 (4) | 0.0217 (4) | 0.0205 (4) | −0.0014 (3) | 0.0044 (3) | −0.0022 (3) |
V6 | 0.0155 (4) | 0.0203 (4) | 0.0163 (4) | −0.0010 (3) | 0.0010 (3) | −0.0022 (3) |
V7 | 0.0138 (3) | 0.0221 (4) | 0.0174 (4) | −0.0007 (3) | −0.0001 (3) | −0.0019 (3) |
V8 | 0.0130 (3) | 0.0215 (4) | 0.0202 (4) | −0.0010 (3) | −0.0005 (3) | −0.0014 (3) |
V9 | 0.0148 (3) | 0.0195 (4) | 0.0158 (4) | 0.0007 (3) | −0.0007 (3) | −0.0010 (3) |
V10 | 0.0131 (3) | 0.0220 (4) | 0.0184 (4) | 0.0009 (3) | −0.0011 (3) | −0.0014 (3) |
V11 | 0.0139 (3) | 0.0190 (4) | 0.0165 (4) | 0.0010 (3) | −0.0008 (3) | −0.0001 (3) |
V12 | 0.0160 (4) | 0.0221 (4) | 0.0147 (4) | 0.0005 (3) | 0.0007 (3) | −0.0003 (3) |
Geometric parameters (Å, º) top
C101—N101 | 1.517 (7) | C405—H40K | 0.9900 |
C101—C102 | 1.519 (8) | C405—H40L | 0.9900 |
C101—H10A | 0.9900 | C406—H40M | 0.9800 |
C101—H10B | 0.9900 | C406—H40N | 0.9800 |
C102—H10C | 0.9800 | C406—H40O | 0.9800 |
C102—H10D | 0.9800 | C407—N401 | 1.510 (7) |
C102—H10E | 0.9800 | C407—C408 | 1.522 (9) |
C103—C104 | 1.494 (10) | C407—H40P | 0.9900 |
C103—N101 | 1.519 (7) | C407—H40Q | 0.9900 |
C103—H10F | 0.9900 | C408—H40R | 0.9800 |
C103—H10G | 0.9900 | C408—H40S | 0.9800 |
C104—H10H | 0.9800 | C408—H40T | 0.9800 |
C104—H10I | 0.9800 | C501—C502 | 1.510 (8) |
C104—H10J | 0.9800 | C501—N501 | 1.518 (7) |
C105—C106 | 1.511 (8) | C501—H50A | 0.9900 |
C105—N101 | 1.521 (7) | C501—H50B | 0.9900 |
C105—H10K | 0.9900 | C502—H50C | 0.9800 |
C105—H10L | 0.9900 | C502—H50D | 0.9800 |
C106—H10M | 0.9800 | C502—H50E | 0.9800 |
C106—H10N | 0.9800 | C503—N501 | 1.522 (7) |
C106—H10O | 0.9800 | C503—C504 | 1.533 (8) |
C107—N101 | 1.506 (7) | C503—H50F | 0.9900 |
C107—C108 | 1.519 (8) | C503—H50G | 0.9900 |
C107—H10P | 0.9900 | C504—H50H | 0.9800 |
C107—H10Q | 0.9900 | C504—H50I | 0.9800 |
C108—H10R | 0.9800 | C504—H50J | 0.9800 |
C108—H10S | 0.9800 | C505—C506 | 1.492 (8) |
C108—H10T | 0.9800 | C505—N501 | 1.516 (7) |
C201—C202 | 1.513 (8) | C505—H50K | 0.9900 |
C201—N201 | 1.521 (7) | C505—H50L | 0.9900 |
C201—H20A | 0.9900 | C506—H50M | 0.9800 |
C201—H20B | 0.9900 | C506—H50N | 0.9800 |
C202—H20C | 0.9800 | C506—H50O | 0.9800 |
C202—H20D | 0.9800 | C507—C508 | 1.506 (8) |
C202—H20E | 0.9800 | C507—N501 | 1.513 (7) |
C203—N201 | 1.511 (7) | C507—H50P | 0.9900 |
C203—C204 | 1.516 (8) | C507—H50Q | 0.9900 |
C203—H20F | 0.9900 | C508—H50R | 0.9800 |
C203—H20G | 0.9900 | C508—H50S | 0.9800 |
C204—H20H | 0.9800 | C508—H50T | 0.9800 |
C204—H20I | 0.9800 | C601—N651 | 1.38 (3) |
C204—H20J | 0.9800 | C601—N601 | 1.459 (16) |
C205—C206 | 1.517 (9) | C601—H60A | 0.9800 |
C205—N201 | 1.524 (8) | C601—H60B | 0.9800 |
C205—H20K | 0.9900 | C601—H60C | 0.9800 |
C205—H20L | 0.9900 | C601—H65A | 0.9800 |
C206—H20M | 0.9800 | C601—H65B | 0.9800 |
C206—H20N | 0.9800 | C601—H65C | 0.9800 |
C206—H20O | 0.9800 | N601—O601 | 1.22 (2) |
C207—C208 | 1.487 (10) | N601—O602 | 1.234 (17) |
C207—N201 | 1.515 (7) | N651—O652 | 1.21 (3) |
C207—H20P | 0.9900 | N651—O651 | 1.23 (3) |
C207—H20Q | 0.9900 | N1A—N2B | 1.142 (12) |
C208—H20R | 0.9800 | N1A—N3A | 1.18 (2) |
C208—H20S | 0.9800 | N1A—N3B | 1.187 (16) |
C208—H20T | 0.9800 | N1A—N2A | 1.202 (17) |
C301—C302 | 1.497 (11) | O1—V1 | 1.599 (3) |
C301—N301 | 1.504 (10) | O2—V2 | 1.608 (3) |
C301—H30A | 0.9900 | O3—V3 | 1.603 (4) |
C301—H30B | 0.9900 | O4—V4 | 1.595 (4) |
C351—C302 | 1.436 (17) | O5—V5 | 1.599 (3) |
C351—N301 | 1.523 (15) | O6—V6 | 1.605 (3) |
C351—H35A | 0.9900 | O7—V7 | 1.591 (3) |
C351—H35B | 0.9900 | O8—V8 | 1.602 (3) |
C302—H30C | 0.9800 | O9—V9 | 1.600 (3) |
C302—H30D | 0.9800 | O10—V10 | 1.607 (3) |
C302—H30E | 0.9800 | O11—V11 | 1.609 (3) |
C302—H35C | 0.9800 | O12—V12 | 1.603 (3) |
C302—H35D | 0.9800 | O13—V2 | 1.784 (3) |
C302—H35E | 0.9800 | O13—V1 | 1.852 (3) |
C303—C304 | 1.409 (10) | O14—V2 | 1.803 (4) |
C303—N301 | 1.591 (10) | O14—V3 | 1.833 (3) |
C303—H30F | 0.9900 | O15—V4 | 1.804 (4) |
C303—H30G | 0.9900 | O15—V3 | 1.843 (4) |
C353—N301 | 1.463 (15) | O16—V4 | 1.793 (3) |
C353—C304 | 1.528 (17) | O16—V5 | 1.828 (4) |
C353—H35F | 0.9900 | O17—V6 | 1.771 (4) |
C353—H35G | 0.9900 | O17—V5 | 1.855 (3) |
C304—H30H | 0.9800 | O18—V7 | 1.814 (3) |
C304—H30I | 0.9800 | O18—V6 | 1.827 (3) |
C304—H30J | 0.9800 | O19—V8 | 1.818 (4) |
C304—H35H | 0.9800 | O19—V7 | 1.830 (3) |
C304—H35I | 0.9800 | O20—V8 | 1.782 (3) |
C304—H35J | 0.9800 | O20—V1 | 1.850 (3) |
C305—N301 | 1.509 (10) | O21—V9 | 1.916 (3) |
C305—C306 | 1.528 (11) | O21—V1 | 1.921 (3) |
C305—H30K | 0.9900 | O21—V2 | 1.980 (3) |
C305—H30L | 0.9900 | O22—V3 | 1.896 (3) |
C355—C306 | 1.441 (19) | O22—V2 | 1.955 (3) |
C355—N301 | 1.583 (17) | O22—V9 | 1.980 (3) |
C355—H35K | 0.9900 | O23—V10 | 1.897 (3) |
C355—H35L | 0.9900 | O23—V3 | 1.919 (3) |
C306—H30M | 0.9800 | O23—V4 | 1.958 (3) |
C306—H30N | 0.9800 | O24—V5 | 1.896 (3) |
C306—H30O | 0.9800 | O24—V4 | 1.965 (3) |
C306—H35M | 0.9800 | O24—V10 | 2.009 (3) |
C306—H35N | 0.9800 | O25—V11 | 1.900 (3) |
C306—H35O | 0.9800 | O25—V5 | 1.951 (3) |
C307—N301 | 1.486 (10) | O25—V6 | 1.965 (3) |
C307—C308 | 1.491 (12) | O26—V7 | 1.921 (3) |
C307—H30P | 0.9900 | O26—V6 | 1.934 (3) |
C307—H30Q | 0.9900 | O26—V11 | 1.979 (3) |
C357—C308 | 1.487 (18) | O27—V12 | 1.898 (3) |
C357—N301 | 1.510 (16) | O27—V7 | 1.938 (3) |
C357—H35P | 0.9900 | O27—V8 | 1.943 (3) |
C357—H35Q | 0.9900 | O28—V1 | 1.892 (3) |
C308—H30R | 0.9800 | O28—V8 | 1.969 (3) |
C308—H30S | 0.9800 | O28—V12 | 2.002 (3) |
C308—H30T | 0.9800 | O29—V10 | 1.715 (3) |
C308—H35R | 0.9800 | O29—V9 | 1.897 (3) |
C308—H35S | 0.9800 | O30—V12 | 1.709 (3) |
C308—H35T | 0.9800 | O30—V11 | 1.891 (3) |
C401—C402 | 1.501 (8) | O31—V9 | 1.739 (3) |
C401—N401 | 1.517 (7) | O31—V12 | 1.902 (3) |
C401—H40A | 0.9900 | O32—V11 | 1.734 (3) |
C401—H40B | 0.9900 | O32—V10 | 1.893 (3) |
C402—H40C | 0.9800 | V1—V8 | 2.8249 (11) |
C402—H40D | 0.9800 | V1—V2 | 2.8583 (11) |
C402—H40E | 0.9800 | V2—V3 | 2.8429 (11) |
C403—C404 | 1.514 (9) | V2—V9 | 3.0538 (11) |
C403—N401 | 1.517 (7) | V3—V4 | 2.8732 (11) |
C403—H40F | 0.9900 | V4—V5 | 2.8148 (11) |
C403—H40G | 0.9900 | V4—V10 | 3.0516 (12) |
C404—H40H | 0.9800 | V5—V6 | 2.8673 (11) |
C404—H40I | 0.9800 | V6—V7 | 2.8470 (11) |
C404—H40J | 0.9800 | V6—V11 | 3.0237 (11) |
C405—C406 | 1.507 (9) | V7—V8 | 2.8738 (11) |
C405—N401 | 1.515 (7) | V8—V12 | 3.0494 (11) |
| | | |
N101—C101—C102 | 115.5 (4) | C207—N201—C205 | 105.5 (4) |
N101—C101—H10A | 108.4 | C201—N201—C205 | 110.5 (5) |
C102—C101—H10A | 108.4 | C307—N301—C301 | 112.1 (6) |
N101—C101—H10B | 108.4 | C307—N301—C305 | 110.0 (6) |
C102—C101—H10B | 108.4 | C301—N301—C305 | 112.2 (6) |
H10A—C101—H10B | 107.5 | C353—N301—C357 | 115.2 (11) |
C101—C102—H10C | 109.5 | C353—N301—C351 | 111.5 (9) |
C101—C102—H10D | 109.5 | C357—N301—C351 | 108.6 (9) |
H10C—C102—H10D | 109.5 | C353—N301—C355 | 106.7 (9) |
C101—C102—H10E | 109.5 | C357—N301—C355 | 106.9 (10) |
H10C—C102—H10E | 109.5 | C351—N301—C355 | 107.6 (9) |
H10D—C102—H10E | 109.5 | C307—N301—C303 | 109.1 (6) |
C104—C103—N101 | 115.8 (5) | C301—N301—C303 | 106.9 (5) |
C104—C103—H10F | 108.3 | C305—N301—C303 | 106.3 (5) |
N101—C103—H10F | 108.3 | C407—N401—C405 | 106.4 (4) |
C104—C103—H10G | 108.3 | C407—N401—C401 | 111.6 (4) |
N101—C103—H10G | 108.3 | C405—N401—C401 | 111.6 (4) |
H10F—C103—H10G | 107.4 | C407—N401—C403 | 111.6 (5) |
C103—C104—H10H | 109.5 | C405—N401—C403 | 110.1 (4) |
C103—C104—H10I | 109.5 | C401—N401—C403 | 105.6 (4) |
H10H—C104—H10I | 109.5 | C507—N501—C505 | 112.2 (4) |
C103—C104—H10J | 109.5 | C507—N501—C501 | 105.5 (4) |
H10H—C104—H10J | 109.5 | C505—N501—C501 | 110.7 (4) |
H10I—C104—H10J | 109.5 | C507—N501—C503 | 110.7 (4) |
C106—C105—N101 | 115.4 (5) | C505—N501—C503 | 106.5 (4) |
C106—C105—H10K | 108.4 | C501—N501—C503 | 111.3 (4) |
N101—C105—H10K | 108.4 | V2—O13—V1 | 103.61 (17) |
C106—C105—H10L | 108.4 | V2—O14—V3 | 102.88 (17) |
N101—C105—H10L | 108.4 | V4—O15—V3 | 103.98 (18) |
H10K—C105—H10L | 107.5 | V4—O16—V5 | 102.05 (18) |
C105—C106—H10M | 109.5 | V6—O17—V5 | 104.48 (17) |
C105—C106—H10N | 109.5 | V7—O18—V6 | 102.87 (17) |
H10M—C106—H10N | 109.5 | V8—O19—V7 | 103.97 (17) |
C105—C106—H10O | 109.5 | V8—O20—V1 | 102.10 (16) |
H10M—C106—H10O | 109.5 | V9—O21—V1 | 135.98 (18) |
H10N—C106—H10O | 109.5 | V9—O21—V2 | 103.21 (15) |
N101—C107—C108 | 115.4 (5) | V1—O21—V2 | 94.22 (14) |
N101—C107—H10P | 108.4 | V3—O22—V2 | 95.15 (15) |
C108—C107—H10P | 108.4 | V3—O22—V9 | 148.72 (19) |
N101—C107—H10Q | 108.4 | V2—O22—V9 | 101.80 (15) |
C108—C107—H10Q | 108.4 | V10—O23—V3 | 142.88 (18) |
H10P—C107—H10Q | 107.5 | V10—O23—V4 | 104.66 (15) |
C107—C108—H10R | 109.5 | V3—O23—V4 | 95.65 (15) |
C107—C108—H10S | 109.5 | V5—O24—V4 | 93.60 (15) |
H10R—C108—H10S | 109.5 | V5—O24—V10 | 141.04 (18) |
C107—C108—H10T | 109.5 | V4—O24—V10 | 100.34 (15) |
H10R—C108—H10T | 109.5 | V11—O25—V5 | 135.09 (19) |
H10S—C108—H10T | 109.5 | V11—O25—V6 | 102.93 (15) |
C202—C201—N201 | 116.4 (4) | V5—O25—V6 | 94.15 (15) |
C202—C201—H20A | 108.2 | V7—O26—V6 | 95.20 (15) |
N201—C201—H20A | 108.2 | V7—O26—V11 | 149.49 (18) |
C202—C201—H20B | 108.2 | V6—O26—V11 | 101.18 (15) |
N201—C201—H20B | 108.2 | V12—O27—V7 | 143.81 (18) |
H20A—C201—H20B | 107.3 | V12—O27—V8 | 105.10 (15) |
C201—C202—H20C | 109.5 | V7—O27—V8 | 95.53 (15) |
C201—C202—H20D | 109.5 | V1—O28—V8 | 94.03 (14) |
H20C—C202—H20D | 109.5 | V1—O28—V12 | 140.45 (18) |
C201—C202—H20E | 109.5 | V8—O28—V12 | 100.34 (14) |
H20C—C202—H20E | 109.5 | V10—O29—V9 | 154.5 (2) |
H20D—C202—H20E | 109.5 | V12—O30—V11 | 155.9 (2) |
N201—C203—C204 | 114.8 (5) | V9—O31—V12 | 130.24 (19) |
N201—C203—H20F | 108.6 | V11—O32—V10 | 130.24 (18) |
C204—C203—H20F | 108.6 | O1—V1—O20 | 104.68 (16) |
N201—C203—H20G | 108.6 | O1—V1—O13 | 105.80 (17) |
C204—C203—H20G | 108.6 | O20—V1—O13 | 91.23 (15) |
H20F—C203—H20G | 107.5 | O1—V1—O28 | 104.45 (17) |
C203—C204—H20H | 109.5 | O20—V1—O28 | 81.49 (14) |
C203—C204—H20I | 109.5 | O13—V1—O28 | 149.74 (15) |
H20H—C204—H20I | 109.5 | O1—V1—O21 | 103.55 (16) |
C203—C204—H20J | 109.5 | O20—V1—O21 | 151.75 (15) |
H20H—C204—H20J | 109.5 | O13—V1—O21 | 79.98 (14) |
H20I—C204—H20J | 109.5 | O28—V1—O21 | 92.64 (14) |
C206—C205—N201 | 115.6 (5) | O1—V1—V8 | 115.05 (13) |
C206—C205—H20K | 108.4 | O20—V1—V8 | 38.09 (10) |
N201—C205—H20K | 108.4 | O13—V1—V8 | 119.87 (12) |
C206—C205—H20L | 108.4 | O28—V1—V8 | 44.06 (10) |
N201—C205—H20L | 108.4 | O21—V1—V8 | 126.54 (10) |
H20K—C205—H20L | 107.4 | O1—V1—V2 | 116.52 (13) |
C205—C206—H20M | 109.5 | O20—V1—V2 | 119.31 (11) |
C205—C206—H20N | 109.5 | O13—V1—V2 | 37.35 (10) |
H20M—C206—H20N | 109.5 | O28—V1—V2 | 124.23 (10) |
C205—C206—H20O | 109.5 | O21—V1—V2 | 43.69 (10) |
H20M—C206—H20O | 109.5 | V8—V1—V2 | 128.03 (4) |
H20N—C206—H20O | 109.5 | O2—V2—O13 | 105.89 (17) |
C208—C207—N201 | 115.9 (5) | O2—V2—O14 | 105.56 (17) |
C208—C207—H20P | 108.3 | O13—V2—O14 | 104.97 (16) |
N201—C207—H20P | 108.3 | O2—V2—O22 | 105.83 (16) |
C208—C207—H20Q | 108.3 | O13—V2—O22 | 144.89 (15) |
N201—C207—H20Q | 108.3 | O14—V2—O22 | 80.45 (15) |
H20P—C207—H20Q | 107.4 | O2—V2—O21 | 106.29 (16) |
C207—C208—H20R | 109.5 | O13—V2—O21 | 80.06 (14) |
C207—C208—H20S | 109.5 | O14—V2—O21 | 144.87 (15) |
H20R—C208—H20S | 109.5 | O22—V2—O21 | 76.98 (13) |
C207—C208—H20T | 109.5 | O2—V2—V3 | 108.26 (13) |
H20R—C208—H20T | 109.5 | O13—V2—V3 | 135.90 (12) |
H20S—C208—H20T | 109.5 | O14—V2—V3 | 38.94 (11) |
C302—C301—N301 | 118.1 (7) | O22—V2—V3 | 41.64 (10) |
C302—C301—H30A | 107.8 | O21—V2—V3 | 115.20 (10) |
N301—C301—H30A | 107.8 | O2—V2—V1 | 118.40 (13) |
C302—C301—H30B | 107.8 | O13—V2—V1 | 39.04 (11) |
N301—C301—H30B | 107.8 | O14—V2—V1 | 127.93 (12) |
H30A—C301—H30B | 107.1 | O22—V2—V1 | 110.54 (10) |
C302—C351—N301 | 120.9 (11) | O21—V2—V1 | 42.10 (10) |
C302—C351—H35A | 107.1 | V3—V2—V1 | 131.96 (4) |
N301—C351—H35A | 107.1 | O2—V2—V9 | 112.65 (13) |
C302—C351—H35B | 107.1 | O13—V2—V9 | 112.63 (11) |
N301—C351—H35B | 107.1 | O14—V2—V9 | 114.39 (11) |
H35A—C351—H35B | 106.8 | O22—V2—V9 | 39.41 (10) |
C301—C302—H30C | 109.5 | O21—V2—V9 | 37.65 (9) |
C301—C302—H30D | 109.5 | V3—V2—V9 | 78.47 (3) |
H30C—C302—H30D | 109.5 | V1—V2—V9 | 73.92 (3) |
C301—C302—H30E | 109.5 | O3—V3—O14 | 106.61 (17) |
H30C—C302—H30E | 109.5 | O3—V3—O15 | 106.11 (18) |
H30D—C302—H30E | 109.5 | O14—V3—O15 | 94.24 (16) |
C351—C302—H35C | 109.5 | O3—V3—O22 | 106.23 (17) |
C351—C302—H35D | 109.5 | O14—V3—O22 | 81.28 (15) |
H35C—C302—H35D | 109.5 | O15—V3—O22 | 147.26 (16) |
C351—C302—H35E | 109.5 | O3—V3—O23 | 103.17 (17) |
H35C—C302—H35E | 109.5 | O14—V3—O23 | 150.07 (15) |
H35D—C302—H35E | 109.5 | O15—V3—O23 | 80.13 (15) |
C304—C303—N301 | 116.1 (6) | O22—V3—O23 | 87.78 (14) |
C304—C303—H30F | 108.3 | O3—V3—V2 | 109.35 (13) |
N301—C303—H30F | 108.3 | O14—V3—V2 | 38.19 (11) |
C304—C303—H30G | 108.3 | O15—V3—V2 | 126.84 (12) |
N301—C303—H30G | 108.3 | O22—V3—V2 | 43.22 (10) |
H30F—C303—H30G | 107.4 | O23—V3—V2 | 126.55 (10) |
N301—C353—C304 | 116.8 (10) | O3—V3—V4 | 107.20 (13) |
N301—C353—H35F | 108.1 | O14—V3—V4 | 127.18 (11) |
C304—C353—H35F | 108.1 | O15—V3—V4 | 37.53 (11) |
N301—C353—H35G | 108.1 | O22—V3—V4 | 124.99 (10) |
C304—C353—H35G | 108.1 | O23—V3—V4 | 42.70 (10) |
H35F—C353—H35G | 107.3 | V2—V3—V4 | 143.43 (4) |
C303—C304—H30H | 109.5 | O4—V4—O16 | 106.28 (17) |
C303—C304—H30I | 109.5 | O4—V4—O15 | 107.90 (18) |
H30H—C304—H30I | 109.5 | O16—V4—O15 | 102.80 (17) |
C303—C304—H30J | 109.5 | O4—V4—O23 | 104.54 (17) |
H30H—C304—H30J | 109.5 | O16—V4—O23 | 146.34 (15) |
H30I—C304—H30J | 109.5 | O15—V4—O23 | 80.04 (15) |
C353—C304—H35H | 109.5 | O4—V4—O24 | 106.74 (17) |
C353—C304—H35I | 109.5 | O16—V4—O24 | 81.27 (15) |
H35H—C304—H35I | 109.5 | O15—V4—O24 | 142.24 (15) |
C353—C304—H35J | 109.5 | O23—V4—O24 | 77.18 (14) |
H35H—C304—H35J | 109.5 | O4—V4—V5 | 116.36 (13) |
H35I—C304—H35J | 109.5 | O16—V4—V5 | 39.43 (12) |
N301—C305—C306 | 115.3 (7) | O15—V4—V5 | 127.43 (12) |
N301—C305—H30K | 108.4 | O23—V4—V5 | 112.83 (10) |
C306—C305—H30K | 108.4 | O24—V4—V5 | 42.23 (10) |
N301—C305—H30L | 108.4 | O4—V4—V3 | 109.28 (13) |
C306—C305—H30L | 108.4 | O16—V4—V3 | 134.03 (12) |
H30K—C305—H30L | 107.5 | O15—V4—V3 | 38.49 (11) |
C306—C355—N301 | 116.0 (11) | O23—V4—V3 | 41.65 (10) |
C306—C355—H35K | 108.3 | O24—V4—V3 | 114.29 (10) |
N301—C355—H35K | 108.3 | V5—V4—V3 | 133.02 (4) |
C306—C355—H35L | 108.3 | O4—V4—V10 | 112.68 (14) |
N301—C355—H35L | 108.3 | O16—V4—V10 | 116.01 (12) |
H35K—C355—H35L | 107.4 | O15—V4—V10 | 110.45 (12) |
C305—C306—H30M | 109.5 | O23—V4—V10 | 36.97 (10) |
C305—C306—H30N | 109.5 | O24—V4—V10 | 40.36 (10) |
H30M—C306—H30N | 109.5 | V5—V4—V10 | 77.61 (3) |
C305—C306—H30O | 109.5 | V3—V4—V10 | 75.19 (3) |
H30M—C306—H30O | 109.5 | O5—V5—O16 | 105.55 (18) |
H30N—C306—H30O | 109.5 | O5—V5—O17 | 105.57 (18) |
C355—C306—H35M | 109.5 | O16—V5—O17 | 92.84 (16) |
C355—C306—H35N | 109.5 | O5—V5—O24 | 103.62 (17) |
H35M—C306—H35N | 109.5 | O16—V5—O24 | 82.30 (15) |
C355—C306—H35O | 109.5 | O17—V5—O24 | 150.64 (15) |
H35M—C306—H35O | 109.5 | O5—V5—O25 | 103.29 (17) |
H35N—C306—H35O | 109.5 | O16—V5—O25 | 151.15 (15) |
N301—C307—C308 | 118.5 (7) | O17—V5—O25 | 78.80 (15) |
N301—C307—H30P | 107.7 | O24—V5—O25 | 91.56 (14) |
C308—C307—H30P | 107.7 | O5—V5—V4 | 114.03 (14) |
N301—C307—H30Q | 107.7 | O16—V5—V4 | 38.53 (11) |
C308—C307—H30Q | 107.7 | O17—V5—V4 | 122.72 (12) |
H30P—C307—H30Q | 107.1 | O24—V5—V4 | 44.17 (10) |
C308—C357—N301 | 117.1 (11) | O25—V5—V4 | 126.32 (10) |
C308—C357—H35P | 108.0 | O5—V5—V6 | 115.91 (14) |
N301—C357—H35P | 108.0 | O16—V5—V6 | 119.98 (12) |
C308—C357—H35Q | 108.0 | O17—V5—V6 | 36.73 (11) |
N301—C357—H35Q | 108.0 | O24—V5—V6 | 123.82 (10) |
H35P—C357—H35Q | 107.3 | O25—V5—V6 | 43.12 (10) |
C307—C308—H30R | 109.5 | V4—V5—V6 | 129.88 (4) |
C307—C308—H30S | 109.5 | O6—V6—O17 | 107.11 (17) |
H30R—C308—H30S | 109.5 | O6—V6—O18 | 106.74 (16) |
C307—C308—H30T | 109.5 | O17—V6—O18 | 102.32 (16) |
H30R—C308—H30T | 109.5 | O6—V6—O26 | 106.94 (16) |
H30S—C308—H30T | 109.5 | O17—V6—O26 | 143.26 (15) |
C357—C308—H35R | 109.5 | O18—V6—O26 | 80.56 (14) |
C357—C308—H35S | 109.5 | O6—V6—O25 | 105.28 (16) |
H35R—C308—H35S | 109.5 | O17—V6—O25 | 80.43 (15) |
C357—C308—H35T | 109.5 | O18—V6—O25 | 145.32 (15) |
H35R—C308—H35T | 109.5 | O26—V6—O25 | 77.71 (14) |
H35S—C308—H35T | 109.5 | O6—V6—V7 | 110.52 (13) |
C402—C401—N401 | 115.2 (5) | O17—V6—V7 | 131.88 (12) |
C402—C401—H40A | 108.5 | O18—V6—V7 | 38.40 (11) |
N401—C401—H40A | 108.5 | O26—V6—V7 | 42.23 (10) |
C402—C401—H40B | 108.5 | O25—V6—V7 | 116.08 (10) |
N401—C401—H40B | 108.5 | O6—V6—V5 | 118.72 (13) |
H40A—C401—H40B | 107.5 | O17—V6—V5 | 38.79 (11) |
C401—C402—H40C | 109.5 | O18—V6—V5 | 125.77 (11) |
C401—C402—H40D | 109.5 | O26—V6—V5 | 110.37 (10) |
H40C—C402—H40D | 109.5 | O25—V6—V5 | 42.73 (10) |
C401—C402—H40E | 109.5 | V7—V6—V5 | 129.84 (4) |
H40C—C402—H40E | 109.5 | O6—V6—V11 | 111.68 (13) |
H40D—C402—H40E | 109.5 | O17—V6—V11 | 112.70 (11) |
C404—C403—N401 | 114.7 (5) | O18—V6—V11 | 115.53 (11) |
C404—C403—H40F | 108.6 | O26—V6—V11 | 39.96 (10) |
N401—C403—H40F | 108.6 | O25—V6—V11 | 37.77 (10) |
C404—C403—H40G | 108.6 | V7—V6—V11 | 79.68 (3) |
N401—C403—H40G | 108.6 | V5—V6—V11 | 74.28 (3) |
H40F—C403—H40G | 107.6 | O7—V7—O18 | 104.66 (17) |
C403—C404—H40H | 109.5 | O7—V7—O19 | 105.52 (17) |
C403—C404—H40I | 109.5 | O18—V7—O19 | 98.05 (16) |
H40H—C404—H40I | 109.5 | O7—V7—O26 | 106.57 (16) |
C403—C404—H40J | 109.5 | O18—V7—O26 | 81.23 (15) |
H40H—C404—H40J | 109.5 | O19—V7—O26 | 146.97 (15) |
H40I—C404—H40J | 109.5 | O7—V7—O27 | 102.26 (16) |
C406—C405—N401 | 115.8 (5) | O18—V7—O27 | 152.50 (15) |
C406—C405—H40K | 108.3 | O19—V7—O27 | 79.97 (15) |
N401—C405—H40K | 108.3 | O26—V7—O27 | 85.82 (14) |
C406—C405—H40L | 108.3 | O7—V7—V6 | 108.90 (13) |
N401—C405—H40L | 108.3 | O18—V7—V6 | 38.73 (11) |
H40K—C405—H40L | 107.4 | O19—V7—V6 | 130.00 (12) |
C405—C406—H40M | 109.5 | O26—V7—V6 | 42.57 (10) |
C405—C406—H40N | 109.5 | O27—V7—V6 | 124.99 (10) |
H40M—C406—H40N | 109.5 | O7—V7—V8 | 105.24 (13) |
C405—C406—H40O | 109.5 | O18—V7—V8 | 132.15 (11) |
H40M—C406—H40O | 109.5 | O19—V7—V8 | 37.87 (11) |
H40N—C406—H40O | 109.5 | O26—V7—V8 | 123.56 (10) |
N401—C407—C408 | 115.6 (5) | O27—V7—V8 | 42.30 (10) |
N401—C407—H40P | 108.4 | V6—V7—V8 | 145.76 (4) |
C408—C407—H40P | 108.4 | O8—V8—O20 | 105.61 (17) |
N401—C407—H40Q | 108.4 | O8—V8—O19 | 107.97 (18) |
C408—C407—H40Q | 108.4 | O20—V8—O19 | 102.98 (16) |
H40P—C407—H40Q | 107.5 | O8—V8—O27 | 104.74 (16) |
C407—C408—H40R | 109.5 | O20—V8—O27 | 146.71 (14) |
C407—C408—H40S | 109.5 | O19—V8—O27 | 80.13 (15) |
H40R—C408—H40S | 109.5 | O8—V8—O28 | 107.54 (17) |
C407—C408—H40T | 109.5 | O20—V8—O28 | 81.07 (14) |
H40R—C408—H40T | 109.5 | O19—V8—O28 | 141.56 (15) |
H40S—C408—H40T | 109.5 | O27—V8—O28 | 77.06 (13) |
C502—C501—N501 | 114.8 (4) | O8—V8—V1 | 117.67 (13) |
C502—C501—H50A | 108.6 | O20—V8—V1 | 39.81 (11) |
N501—C501—H50A | 108.6 | O19—V8—V1 | 126.25 (12) |
C502—C501—H50B | 108.6 | O27—V8—V1 | 111.99 (10) |
N501—C501—H50B | 108.6 | O28—V8—V1 | 41.91 (9) |
H50A—C501—H50B | 107.5 | O8—V8—V7 | 108.55 (13) |
C501—C502—H50C | 109.5 | O20—V8—V7 | 134.77 (12) |
C501—C502—H50D | 109.5 | O19—V8—V7 | 38.17 (11) |
H50C—C502—H50D | 109.5 | O27—V8—V7 | 42.17 (10) |
C501—C502—H50E | 109.5 | O28—V8—V7 | 114.79 (10) |
H50C—C502—H50E | 109.5 | V1—V8—V7 | 132.58 (4) |
H50D—C502—H50E | 109.5 | O8—V8—V12 | 112.82 (14) |
N501—C503—C504 | 115.5 (4) | O20—V8—V12 | 116.24 (11) |
N501—C503—H50F | 108.4 | O19—V8—V12 | 110.49 (11) |
C504—C503—H50F | 108.4 | O27—V8—V12 | 36.93 (10) |
N501—C503—H50G | 108.4 | O28—V8—V12 | 40.22 (9) |
C504—C503—H50G | 108.4 | V1—V8—V12 | 77.07 (3) |
H50F—C503—H50G | 107.5 | V7—V8—V12 | 75.92 (3) |
C503—C504—H50H | 109.5 | O9—V9—O31 | 103.99 (17) |
C503—C504—H50I | 109.5 | O9—V9—O29 | 104.20 (17) |
H50H—C504—H50I | 109.5 | O31—V9—O29 | 93.49 (15) |
C503—C504—H50J | 109.5 | O9—V9—O21 | 104.14 (16) |
H50H—C504—H50J | 109.5 | O31—V9—O21 | 91.78 (15) |
H50I—C504—H50J | 109.5 | O29—V9—O21 | 148.95 (15) |
C506—C505—N501 | 114.6 (5) | O9—V9—O22 | 102.33 (16) |
C506—C505—H50K | 108.6 | O31—V9—O22 | 153.36 (15) |
N501—C505—H50K | 108.6 | O29—V9—O22 | 83.95 (14) |
C506—C505—H50L | 108.6 | O21—V9—O22 | 77.84 (14) |
N501—C505—H50L | 108.6 | O9—V9—V2 | 109.09 (13) |
H50K—C505—H50L | 107.6 | O31—V9—V2 | 125.57 (11) |
C505—C506—H50M | 109.5 | O29—V9—V2 | 117.75 (11) |
C505—C506—H50N | 109.5 | O21—V9—V2 | 39.13 (10) |
H50M—C506—H50N | 109.5 | O22—V9—V2 | 38.80 (9) |
C505—C506—H50O | 109.5 | O10—V10—O29 | 105.67 (18) |
H50M—C506—H50O | 109.5 | O10—V10—O32 | 101.21 (16) |
H50N—C506—H50O | 109.5 | O29—V10—O32 | 95.62 (15) |
C508—C507—N501 | 115.2 (4) | O10—V10—O23 | 101.36 (16) |
C508—C507—H50P | 108.5 | O29—V10—O23 | 91.78 (15) |
N501—C507—H50P | 108.5 | O32—V10—O23 | 153.34 (15) |
C508—C507—H50Q | 108.5 | O10—V10—O24 | 102.55 (16) |
N501—C507—H50Q | 108.5 | O29—V10—O24 | 151.30 (16) |
H50P—C507—H50Q | 107.5 | O32—V10—O24 | 83.88 (14) |
C507—C508—H50R | 109.5 | O23—V10—O24 | 77.53 (14) |
C507—C508—H50S | 109.5 | O10—V10—V4 | 107.99 (14) |
H50R—C508—H50S | 109.5 | O29—V10—V4 | 123.76 (12) |
C507—C508—H50T | 109.5 | O32—V10—V4 | 119.73 (11) |
H50R—C508—H50T | 109.5 | O23—V10—V4 | 38.37 (10) |
H50S—C508—H50T | 109.5 | O24—V10—V4 | 39.31 (10) |
N601—C601—H60A | 109.5 | O11—V11—O32 | 104.18 (17) |
N601—C601—H60B | 109.5 | O11—V11—O30 | 103.88 (17) |
H60A—C601—H60B | 109.5 | O32—V11—O30 | 93.31 (15) |
N601—C601—H60C | 109.5 | O11—V11—O25 | 104.37 (17) |
H60A—C601—H60C | 109.5 | O32—V11—O25 | 92.27 (15) |
H60B—C601—H60C | 109.5 | O30—V11—O25 | 148.86 (15) |
N651—C601—H65A | 109.5 | O11—V11—O26 | 102.10 (16) |
N651—C601—H65B | 109.5 | O32—V11—O26 | 153.53 (15) |
H65A—C601—H65B | 109.5 | O30—V11—O26 | 83.38 (14) |
N651—C601—H65C | 109.5 | O25—V11—O26 | 78.15 (14) |
H65A—C601—H65C | 109.5 | O11—V11—V6 | 107.98 (13) |
H65B—C601—H65C | 109.5 | O32—V11—V6 | 126.76 (12) |
O601—N601—O602 | 123.4 (14) | O30—V11—V6 | 117.89 (11) |
O601—N601—C601 | 120.9 (12) | O25—V11—V6 | 39.30 (10) |
O602—N601—C601 | 115.4 (12) | O26—V11—V6 | 38.86 (10) |
O652—N651—O651 | 121 (3) | O12—V12—O30 | 105.32 (17) |
O652—N651—C601 | 121 (2) | O12—V12—O27 | 102.29 (17) |
O651—N651—C601 | 117 (2) | O30—V12—O27 | 91.63 (15) |
N2B—N1A—N3B | 170.5 (10) | O12—V12—O31 | 101.44 (16) |
N3A—N1A—N2A | 172.6 (10) | O30—V12—O31 | 95.11 (15) |
C107—N101—C101 | 111.7 (4) | O27—V12—O31 | 152.62 (15) |
C107—N101—C103 | 111.3 (4) | O12—V12—O28 | 103.58 (16) |
C101—N101—C103 | 105.7 (4) | O30—V12—O28 | 150.66 (16) |
C107—N101—C105 | 106.2 (4) | O27—V12—O28 | 77.32 (13) |
C101—N101—C105 | 110.9 (4) | O31—V12—O28 | 84.01 (14) |
C103—N101—C105 | 111.0 (5) | O12—V12—V8 | 108.74 (13) |
C203—N201—C207 | 112.8 (5) | O30—V12—V8 | 123.39 (12) |
C203—N201—C201 | 105.7 (4) | O27—V12—V8 | 37.97 (10) |
C207—N201—C201 | 110.9 (4) | O31—V12—V8 | 119.94 (10) |
C203—N201—C205 | 111.5 (5) | O28—V12—V8 | 39.44 (9) |
| | | |
N301—C351_f—C302—C301_e | −14.8 (9) | V3—O14—V2—O22 | −3.95 (16) |
N301—C301—C302—C351 | 14.5 (9) | V3—O14—V2—O21 | −54.4 (3) |
N301—C303—C304—C353 | 0.4 (9) | V3—O14—V2—V1 | −112.60 (14) |
N301—C353—C304—C303 | −0.4 (9) | V3—O14—V2—V9 | −24.46 (19) |
N301—C355—C306—C305 | −16.4 (9) | V2—O14—V3—O3 | −100.4 (2) |
N301—C305—C306—C355 | 17.1 (9) | V2—O14—V3—O15 | 151.41 (17) |
N301—C357—C308—C307 | 11.8 (10) | V2—O14—V3—O22 | 4.06 (16) |
N301—C307—C308—C357 | −12.1 (10) | V2—O14—V3—O23 | 73.9 (3) |
N651—C601—N601—O601 | −77 (3) | V2—O14—V3—V4 | 131.78 (11) |
N651—C601—N601—O602 | 108 (4) | V4—O15—V3—O3 | 97.4 (2) |
N601—C601—N651—O652 | −91 (4) | V4—O15—V3—O14 | −153.93 (18) |
N601—C601—N651—O651 | 91 (4) | V4—O15—V3—O22 | −73.5 (3) |
C108—C107—N101—C101 | 54.3 (7) | V4—O15—V3—O23 | −3.56 (17) |
C108—C107—N101—C103 | −63.6 (7) | V4—O15—V3—V2 | −132.24 (12) |
C108—C107—N101—C105 | 175.5 (5) | V2—O22—V3—O3 | 101.20 (17) |
C102—C101—N101—C107 | 61.4 (6) | V9—O22—V3—O3 | −135.9 (4) |
C102—C101—N101—C103 | −177.4 (5) | V2—O22—V3—O14 | −3.67 (14) |
C102—C101—N101—C105 | −57.0 (6) | V9—O22—V3—O14 | 119.3 (4) |
C104—C103—N101—C107 | −61.2 (8) | V2—O22—V3—O15 | −87.9 (3) |
C104—C103—N101—C101 | 177.4 (7) | V9—O22—V3—O15 | 35.0 (5) |
C104—C103—N101—C105 | 57.0 (8) | V2—O22—V3—O23 | −155.73 (15) |
C106—C105—N101—C107 | −179.9 (5) | V9—O22—V3—O23 | −32.8 (4) |
C106—C105—N101—C101 | −58.3 (6) | V9—O22—V3—V2 | 122.9 (4) |
C106—C105—N101—C103 | 58.9 (6) | V2—O22—V3—V4 | −133.38 (9) |
C204—C203—N201—C207 | −60.6 (7) | V9—O22—V3—V4 | −10.4 (4) |
C204—C203—N201—C201 | 178.1 (5) | V5—O16—V4—O4 | 111.91 (19) |
C204—C203—N201—C205 | 57.9 (7) | V5—O16—V4—O15 | −134.84 (17) |
C208—C207—N201—C203 | −52.0 (7) | V5—O16—V4—O23 | −43.6 (3) |
C208—C207—N201—C201 | 66.4 (7) | V5—O16—V4—O24 | 6.92 (16) |
C208—C207—N201—C205 | −174.0 (6) | V5—O16—V4—V3 | −108.57 (16) |
C202—C201—N201—C203 | −173.3 (5) | V5—O16—V4—V10 | −14.20 (19) |
C202—C201—N201—C207 | 64.1 (7) | V3—O15—V4—O4 | −98.7 (2) |
C202—C201—N201—C205 | −52.5 (6) | V3—O15—V4—O16 | 149.25 (17) |
C206—C205—N201—C203 | 58.8 (7) | V3—O15—V4—O23 | 3.49 (16) |
C206—C205—N201—C207 | −178.4 (6) | V3—O15—V4—O24 | 57.0 (3) |
C206—C205—N201—C201 | −58.5 (7) | V3—O15—V4—V5 | 114.70 (15) |
C304—C353—N301—C307 | 119.8 (13) | V3—O15—V4—V10 | 24.87 (19) |
C304—C353—N301—C301 | −26 (5) | V4—O16—V5—O5 | −109.21 (19) |
C304—C353—N301—C305 | −122.8 (13) | V4—O16—V5—O17 | 143.76 (17) |
C304—C353—N301—C357 | 70.4 (14) | V4—O16—V5—O24 | −7.15 (16) |
C304—C353—N301—C351 | −53.9 (15) | V4—O16—V5—O25 | 72.0 (4) |
C304—C353—N301—C355 | −171.1 (12) | V4—O16—V5—V6 | 117.62 (13) |
C304—C353—N301—C303 | 0.4 (9) | V6—O17—V5—O5 | 112.6 (2) |
C308—C307—N301—C353 | −116.1 (11) | V6—O17—V5—O16 | −140.36 (18) |
C308—C307—N301—C301 | 56.6 (10) | V6—O17—V5—O24 | −61.0 (4) |
C308—C307—N301—C305 | −177.8 (8) | V6—O17—V5—O25 | 11.79 (16) |
C308—C307—N301—C357 | 12.0 (10) | V6—O17—V5—V4 | −114.40 (14) |
C308—C307—N301—C351 | 32 (5) | V4—O24—V5—O5 | 110.60 (17) |
C308—C307—N301—C355 | 132.4 (11) | V10—O24—V5—O5 | −138.1 (3) |
C308—C307—N301—C303 | −61.6 (9) | V4—O24—V5—O16 | 6.39 (15) |
C302—C301—N301—C353 | −45 (4) | V10—O24—V5—O16 | 117.7 (3) |
C302—C301—N301—C307 | 171.4 (7) | V4—O24—V5—O17 | −75.7 (3) |
C302—C301—N301—C305 | 47.1 (9) | V10—O24—V5—O17 | 35.7 (5) |
C302—C301—N301—C357 | −146.7 (10) | V4—O24—V5—O25 | −145.32 (14) |
C302—C301—N301—C351 | −14.0 (9) | V10—O24—V5—O25 | −34.0 (3) |
C302—C301—N301—C355 | 101.7 (9) | V10—O24—V5—V4 | 111.3 (3) |
C302—C301—N301—C303 | −69.1 (8) | V4—O24—V5—V6 | −114.70 (11) |
C306—C305—N301—C353 | −140.8 (10) | V10—O24—V5—V6 | −3.4 (4) |
C306—C305—N301—C307 | −73.3 (8) | V5—O17—V6—O6 | −114.81 (19) |
C306—C305—N301—C301 | 52.2 (9) | V5—O17—V6—O18 | 133.12 (17) |
C306—C305—N301—C357 | −31 (4) | V5—O17—V6—O26 | 42.4 (3) |
C306—C305—N301—C351 | 101.1 (9) | V5—O17—V6—O25 | −11.64 (16) |
C306—C305—N301—C355 | −15.9 (9) | V5—O17—V6—V7 | 104.95 (16) |
C306—C305—N301—C303 | 168.7 (6) | V5—O17—V6—V11 | 8.4 (2) |
C308—C357—N301—C353 | 46.3 (16) | V7—O18—V6—O6 | 102.11 (19) |
C308—C357—N301—C307 | −11.9 (10) | V7—O18—V6—O17 | −145.54 (16) |
C308—C357—N301—C301 | −146.8 (15) | V7—O18—V6—O26 | −2.87 (15) |
C308—C357—N301—C305 | −58 (5) | V7—O18—V6—O25 | −54.6 (3) |
C308—C357—N301—C351 | 172.2 (12) | V7—O18—V6—V5 | −111.24 (14) |
C308—C357—N301—C355 | −72.0 (15) | V7—O18—V6—V11 | −22.73 (18) |
C308—C357—N301—C303 | 102.8 (13) | V6—O18—V7—O7 | −102.07 (19) |
C302—C351—N301—C353 | −171.6 (12) | V6—O18—V7—O19 | 149.48 (16) |
C302—C351—N301—C307 | 42 (5) | V6—O18—V7—O26 | 2.88 (15) |
C302—C351—N301—C301 | 15.0 (9) | V6—O18—V7—O27 | 65.8 (4) |
C302—C351—N301—C305 | −109.6 (12) | V6—O18—V7—V8 | 130.82 (11) |
C302—C351—N301—C357 | 60.5 (15) | V8—O19—V7—O7 | 95.0 (2) |
C302—C351—N301—C355 | −54.9 (14) | V8—O19—V7—O18 | −157.26 (17) |
C302—C351—N301—C303 | 139.4 (13) | V8—O19—V7—O26 | −71.0 (3) |
C306—C355—N301—C353 | 69.9 (14) | V8—O19—V7—O27 | −5.05 (16) |
C306—C355—N301—C307 | 141.6 (13) | V8—O19—V7—V6 | −132.76 (12) |
C306—C355—N301—C301 | −103.1 (12) | V1—O20—V8—O8 | 114.70 (19) |
C306—C355—N301—C305 | 17.0 (9) | V1—O20—V8—O19 | −132.16 (17) |
C306—C355—N301—C357 | −166.4 (12) | V1—O20—V8—O27 | −40.4 (3) |
C306—C355—N301—C351 | −49.9 (14) | V1—O20—V8—O28 | 8.87 (15) |
C306—C355—N301—C303 | 36 (4) | V1—O20—V8—V7 | −107.36 (16) |
C304—C303—N301—C353 | −0.4 (9) | V1—O20—V8—V12 | −11.22 (19) |
C304—C303—N301—C307 | −64.6 (8) | V7—O19—V8—O8 | −97.4 (2) |
C304—C303—N301—C301 | 173.9 (6) | V7—O19—V8—O20 | 151.20 (17) |
C304—C303—N301—C305 | 53.9 (8) | V7—O19—V8—O27 | 5.03 (16) |
C304—C303—N301—C357 | −121.8 (9) | V7—O19—V8—O28 | 59.2 (3) |
C304—C303—N301—C351 | 127.0 (9) | V7—O19—V8—V1 | 115.14 (14) |
C304—C303—N301—C355 | 37 (3) | V7—O19—V8—V12 | 26.42 (19) |
C408—C407—N401—C405 | 175.4 (5) | V12—O31—V9—O9 | −178.9 (2) |
C408—C407—N401—C401 | −62.6 (6) | V12—O31—V9—O29 | −73.4 (2) |
C408—C407—N401—C403 | 55.3 (6) | V12—O31—V9—O21 | 76.0 (2) |
C406—C405—N401—C407 | −178.8 (5) | V12—O31—V9—O22 | 10.1 (5) |
C406—C405—N401—C401 | 59.3 (6) | V12—O31—V9—V2 | 54.7 (3) |
C406—C405—N401—C403 | −57.7 (6) | V10—O29—V9—O9 | −131.5 (5) |
C402—C401—N401—C407 | −56.3 (6) | V10—O29—V9—O31 | 123.1 (5) |
C402—C401—N401—C405 | 62.7 (6) | V10—O29—V9—O21 | 23.8 (7) |
C402—C401—N401—C403 | −177.7 (5) | V10—O29—V9—O22 | −30.2 (5) |
C404—C403—N401—C407 | 52.8 (6) | V10—O29—V9—V2 | −10.5 (5) |
C404—C403—N401—C405 | −65.1 (6) | V9—O29—V10—O10 | 133.6 (5) |
C404—C403—N401—C401 | 174.2 (5) | V9—O29—V10—O32 | −123.1 (5) |
C508—C507—N501—C505 | −59.7 (6) | V9—O29—V10—O23 | 31.3 (5) |
C508—C507—N501—C501 | 179.6 (5) | V9—O29—V10—O24 | −35.6 (7) |
C508—C507—N501—C503 | 59.2 (6) | V9—O29—V10—V4 | 8.6 (6) |
C506—C505—N501—C507 | −56.4 (6) | V11—O32—V10—O10 | −175.9 (2) |
C506—C505—N501—C501 | 61.2 (6) | V11—O32—V10—O29 | 76.8 (3) |
C506—C505—N501—C503 | −177.6 (5) | V11—O32—V10—O23 | −28.6 (5) |
C502—C501—N501—C507 | 177.6 (5) | V11—O32—V10—O24 | −74.3 (2) |
C502—C501—N501—C505 | 56.0 (6) | V11—O32—V10—V4 | −57.5 (3) |
C502—C501—N501—C503 | −62.3 (6) | V3—O23—V10—O10 | −134.4 (3) |
C504—C503—N501—C507 | 58.1 (6) | V4—O23—V10—O10 | 104.69 (18) |
C504—C503—N501—C505 | −179.7 (5) | V3—O23—V10—O29 | −28.0 (3) |
C504—C503—N501—C501 | −58.9 (6) | V4—O23—V10—O29 | −148.94 (17) |
V8—O20—V1—O1 | −112.04 (18) | V3—O23—V10—O32 | 78.3 (4) |
V8—O20—V1—O13 | 141.27 (17) | V4—O23—V10—O32 | −42.7 (4) |
V8—O20—V1—O28 | −9.23 (16) | V3—O23—V10—O24 | 125.1 (3) |
V8—O20—V1—O21 | 70.4 (4) | V4—O23—V10—O24 | 4.18 (14) |
V8—O20—V1—V2 | 115.40 (13) | V3—O23—V10—V4 | 121.0 (4) |
V2—O13—V1—O1 | 113.21 (19) | V10—O32—V11—O11 | −177.7 (2) |
V2—O13—V1—O20 | −141.16 (18) | V10—O32—V11—O30 | −72.5 (3) |
V2—O13—V1—O28 | −66.1 (3) | V10—O32—V11—O25 | 76.9 (2) |
V2—O13—V1—O21 | 11.83 (16) | V10—O32—V11—O26 | 9.3 (5) |
V2—O13—V1—V8 | −114.74 (14) | V10—O32—V11—V6 | 56.4 (3) |
V8—O28—V1—O1 | 111.24 (17) | V12—O30—V11—O11 | −127.0 (5) |
V12—O28—V1—O1 | −137.2 (3) | V12—O30—V11—O32 | 127.5 (5) |
V8—O28—V1—O20 | 8.18 (14) | V12—O30—V11—O25 | 27.6 (7) |
V12—O28—V1—O20 | 119.8 (3) | V12—O30—V11—O26 | −26.1 (5) |
V8—O28—V1—O13 | −69.5 (3) | V12—O30—V11—V6 | −7.6 (6) |
V12—O28—V1—O13 | 42.1 (5) | V11—O30—V12—O12 | 129.4 (5) |
V8—O28—V1—O21 | −144.04 (14) | V11—O30—V12—O27 | 26.2 (5) |
V12—O28—V1—O21 | −32.5 (3) | V11—O30—V12—O31 | −127.2 (5) |
V12—O28—V1—V8 | 111.6 (3) | V11—O30—V12—O28 | −40.4 (7) |
V8—O28—V1—V2 | −111.62 (11) | V11—O30—V12—V8 | 4.0 (6) |
V12—O28—V1—V2 | 0.0 (3) | V7—O27—V12—O12 | −132.7 (3) |
V1—O13—V2—O2 | −115.72 (19) | V8—O27—V12—O12 | 104.80 (18) |
V1—O13—V2—O14 | 132.89 (17) | V7—O27—V12—O30 | −26.6 (3) |
V1—O13—V2—O22 | 38.2 (3) | V8—O27—V12—O30 | −149.14 (17) |
V1—O13—V2—O21 | −11.47 (16) | V7—O27—V12—O31 | 77.8 (4) |
V1—O13—V2—V3 | 104.66 (17) | V8—O27—V12—O31 | −44.7 (4) |
V1—O13—V2—V9 | 7.82 (19) | V7—O27—V12—O28 | 126.0 (3) |
V3—O14—V2—O2 | 99.95 (19) | V8—O27—V12—O28 | 3.42 (15) |
V3—O14—V2—O13 | −148.41 (16) | V7—O27—V12—V8 | 122.5 (4) |
Heptaammonium azidotetradecavanadate dimethyl sulfoxide hexasolvate (2)
top
Crystal data top
(NH4)7[V14O38(N3)]·6C2H6OS | F(000) = 3904 |
Mr = 1958.25 | Dx = 2.089 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71075 Å |
a = 19.272 (3) Å | Cell parameters from 13563 reflections |
b = 24.785 (3) Å | θ = 1.6–13.8° |
c = 14.552 (4) Å | µ = 2.30 mm−1 |
β = 116.387 (15)° | T = 83 K |
V = 6227 (2) Å3 | Block, red |
Z = 4 | 0.20 × 0.20 × 0.20 mm |
Data collection top
Rigaku Mercury70 diffractometer | 6292 reflections with I > 2σ(I) |
Detector resolution: 14.629 pixels mm-1 | Rint = 0.034 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: numerical (NUMABS; Rigaku, 1999) | h = −25→20 |
Tmin = 0.501, Tmax = 0.631 | k = −31→32 |
33352 measured reflections | l = −15→18 |
7051 independent reflections | |
Refinement top
Refinement on F2 | 14 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.036 | H 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 reflections | Δρmax = 1.07 e Å−3 |
446 parameters | Δρmin = −0.91 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
C101 | 0.28101 (19) | 0.96267 (16) | 0.8402 (3) | 0.0357 (8) | |
H10A | 0.2294 | 0.9470 | 0.8009 | 0.054* | |
H10B | 0.3097 | 0.9412 | 0.9023 | 0.054* | |
H10C | 0.2758 | 0.9998 | 0.8594 | 0.054* | |
C102 | 0.2773 (2) | 1.01291 (13) | 0.6731 (3) | 0.0357 (8) | |
H10D | 0.2263 | 0.9984 | 0.6267 | 0.054* | |
H10E | 0.2707 | 1.0445 | 0.7091 | 0.054* | |
H10F | 0.3049 | 1.0236 | 0.6334 | 0.054* | |
C201 | 0.18451 (19) | 0.69520 (15) | 0.9394 (3) | 0.0322 (7) | |
H20A | 0.1879 | 0.7321 | 0.9177 | 0.048* | |
H20B | 0.1960 | 0.6951 | 1.0121 | 0.048* | |
H20C | 0.2220 | 0.6723 | 0.9293 | 0.048* | |
C202 | 0.04072 (18) | 0.70993 (13) | 0.9199 (2) | 0.0257 (6) | |
H20D | 0.0388 | 0.7475 | 0.8978 | 0.039* | |
H20E | −0.0121 | 0.6963 | 0.8969 | 0.039* | |
H20F | 0.0685 | 0.7080 | 0.9949 | 0.039* | |
C301 | 0.3274 (2) | 0.40411 (18) | 0.5397 (3) | 0.0441 (9) | |
H30A | 0.3104 | 0.3802 | 0.5794 | 0.066* | |
H30B | 0.2917 | 0.4348 | 0.5139 | 0.066* | |
H30C | 0.3276 | 0.3841 | 0.4817 | 0.066* | |
C302 | 0.4729 (2) | 0.36707 (14) | 0.6277 (3) | 0.0340 (7) | |
H30D | 0.4633 | 0.3415 | 0.6722 | 0.051* | |
H30E | 0.4553 | 0.3513 | 0.5592 | 0.051* | |
H30F | 0.5284 | 0.3748 | 0.6567 | 0.051* | |
N1A | 0.25489 (16) | 0.72352 (12) | 0.5701 (2) | 0.0315 (6) | |
N2A | 0.2500 | 0.7500 | 0.5000 | 0.0211 (7) | |
N1 | 0.55738 (14) | 0.75064 (10) | 0.90881 (19) | 0.0168 (5) | |
N2 | 0.52456 (15) | 0.55703 (12) | 0.6140 (2) | 0.0247 (5) | |
N3 | −0.00337 (15) | 0.57391 (10) | 0.9919 (2) | 0.0192 (5) | |
N4 | 0.0000 | 0.53901 (15) | 0.7500 | 0.0245 (8) | |
O1 | 0.39611 (11) | 0.84816 (8) | 0.84735 (15) | 0.0198 (4) | |
O2 | 0.40679 (12) | 0.69131 (8) | 0.91862 (15) | 0.0215 (4) | |
O3 | 0.36740 (11) | 0.54570 (8) | 0.65899 (15) | 0.0191 (4) | |
O4 | 0.13152 (11) | 0.92400 (8) | 0.61245 (15) | 0.0187 (4) | |
O5 | 0.15934 (12) | 0.80703 (8) | 0.80009 (15) | 0.0204 (4) | |
O6 | 0.12684 (11) | 0.61075 (8) | 0.70025 (15) | 0.0179 (4) | |
O8 | 0.40231 (10) | 0.75246 (8) | 0.76046 (14) | 0.0160 (4) | |
O9 | 0.40226 (11) | 0.63065 (8) | 0.56668 (14) | 0.0167 (4) | |
O10 | 0.35958 (10) | 0.84207 (8) | 0.64328 (15) | 0.0173 (4) | |
O11 | 0.37830 (11) | 0.64494 (8) | 0.73385 (15) | 0.0175 (4) | |
O12 | 0.28829 (11) | 0.76176 (7) | 0.79023 (14) | 0.0158 (4) | |
O13 | 0.26785 (10) | 0.60429 (7) | 0.47358 (14) | 0.0149 (4) | |
O14 | 0.26680 (11) | 0.65844 (7) | 0.78119 (14) | 0.0160 (4) | |
O15 | 0.24247 (10) | 0.84168 (7) | 0.68867 (14) | 0.0156 (4) | |
O16 | 0.23494 (10) | 0.60680 (7) | 0.61444 (14) | 0.0147 (4) | |
O17 | 0.14750 (11) | 0.71781 (8) | 0.68567 (15) | 0.0173 (4) | |
O18 | 0.12314 (11) | 0.55947 (8) | 0.42881 (16) | 0.0206 (4) | |
O19 | 0.10937 (10) | 0.81397 (8) | 0.59330 (15) | 0.0167 (4) | |
O20 | 0.11130 (10) | 0.65201 (7) | 0.52075 (14) | 0.0147 (4) | |
O101 | 0.41072 (12) | 0.98792 (8) | 0.83454 (16) | 0.0222 (4) | |
O201 | 0.08979 (13) | 0.61273 (8) | 0.90413 (17) | 0.0246 (4) | |
O301 | 0.44037 (16) | 0.46371 (10) | 0.5490 (2) | 0.0369 (6) | |
S101 | 0.33171 (4) | 0.96259 (3) | 0.76434 (5) | 0.02078 (15) | |
S201 | 0.08981 (4) | 0.66995 (3) | 0.86548 (5) | 0.01940 (15) | |
S301 | 0.42139 (5) | 0.42786 (3) | 0.61872 (7) | 0.03002 (18) | |
V1 | 0.34650 (2) | 0.81247 (2) | 0.74752 (3) | 0.01367 (10) | |
V2 | 0.34907 (3) | 0.69858 (2) | 0.79970 (3) | 0.01470 (11) | |
V3 | 0.33743 (3) | 0.60611 (2) | 0.62210 (3) | 0.01393 (10) | |
V4 | 0.15833 (3) | 0.87196 (2) | 0.57127 (3) | 0.01360 (10) | |
V5 | 0.18223 (3) | 0.78515 (2) | 0.71331 (3) | 0.01385 (10) | |
V6 | 0.17553 (3) | 0.65064 (2) | 0.66441 (3) | 0.01410 (10) | |
V7 | 0.16743 (2) | 0.61587 (2) | 0.46699 (3) | 0.01405 (10) | |
H1 | 0.568 (2) | 0.7245 (11) | 0.953 (2) | 0.023 (9)* | |
H2 | 0.5075 (11) | 0.7532 (15) | 0.869 (2) | 0.029 (10)* | |
H3 | 0.574 (2) | 0.7433 (15) | 0.865 (2) | 0.025 (9)* | |
H4 | 0.573 (2) | 0.7796 (11) | 0.945 (3) | 0.037 (11)* | |
H5 | 0.560 (3) | 0.557 (3) | 0.679 (2) | 0.11 (2)* | |
H6 | 0.542 (2) | 0.5576 (16) | 0.565 (2) | 0.031 (10)* | |
H7 | 0.4995 (16) | 0.5265 (9) | 0.604 (2) | 0.008 (7)* | |
H8 | 0.4920 (19) | 0.5847 (12) | 0.601 (3) | 0.035 (10)* | |
H9 | 0.0277 (16) | 0.5881 (13) | 0.969 (2) | 0.016 (8)* | |
H10 | 0.0206 (18) | 0.5560 (12) | 1.0481 (18) | 0.020 (8)* | |
H11 | −0.0323 (18) | 0.5986 (12) | 1.000 (3) | 0.027 (9)* | |
H12 | −0.0341 (17) | 0.5506 (11) | 0.947 (2) | 0.020 (8)* | |
H13 | −0.023 (2) | 0.5189 (14) | 0.778 (3) | 0.042 (11)* | |
H14 | −0.0347 (16) | 0.5591 (13) | 0.703 (2) | 0.026 (9)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C101 | 0.0238 (16) | 0.053 (2) | 0.0320 (18) | −0.0039 (15) | 0.0142 (14) | −0.0093 (16) |
C102 | 0.0302 (17) | 0.0222 (16) | 0.0336 (19) | −0.0009 (13) | −0.0048 (14) | 0.0042 (13) |
C201 | 0.0220 (15) | 0.0392 (19) | 0.0316 (18) | −0.0092 (13) | 0.0085 (14) | 0.0036 (14) |
C202 | 0.0258 (15) | 0.0246 (15) | 0.0281 (16) | 0.0028 (12) | 0.0132 (13) | −0.0019 (12) |
C301 | 0.0329 (19) | 0.059 (3) | 0.044 (2) | 0.0061 (17) | 0.0198 (18) | 0.0176 (19) |
C302 | 0.0350 (18) | 0.0286 (17) | 0.040 (2) | 0.0031 (14) | 0.0183 (16) | −0.0058 (14) |
N1A | 0.0254 (14) | 0.0400 (16) | 0.0239 (14) | −0.0094 (12) | 0.0062 (11) | 0.0020 (12) |
N2A | 0.0119 (15) | 0.0240 (18) | 0.0213 (18) | −0.0038 (13) | 0.0019 (13) | −0.0082 (14) |
N1 | 0.0148 (11) | 0.0147 (11) | 0.0192 (12) | 0.0006 (9) | 0.0061 (10) | 0.0026 (9) |
N2 | 0.0212 (13) | 0.0280 (14) | 0.0228 (14) | 0.0018 (11) | 0.0080 (11) | −0.0064 (11) |
N3 | 0.0199 (12) | 0.0170 (12) | 0.0212 (13) | 0.0013 (9) | 0.0096 (10) | 0.0022 (9) |
N4 | 0.035 (2) | 0.0179 (18) | 0.024 (2) | 0.000 | 0.0168 (18) | 0.000 |
O1 | 0.0209 (10) | 0.0177 (10) | 0.0166 (10) | −0.0030 (8) | 0.0045 (8) | −0.0014 (7) |
O2 | 0.0228 (10) | 0.0212 (10) | 0.0151 (10) | 0.0004 (8) | 0.0034 (8) | 0.0002 (8) |
O3 | 0.0210 (10) | 0.0140 (9) | 0.0222 (10) | 0.0038 (7) | 0.0095 (8) | 0.0019 (7) |
O4 | 0.0195 (9) | 0.0150 (9) | 0.0238 (10) | 0.0016 (7) | 0.0116 (8) | −0.0019 (7) |
O5 | 0.0233 (10) | 0.0217 (10) | 0.0208 (10) | 0.0035 (8) | 0.0140 (9) | −0.0011 (8) |
O6 | 0.0196 (10) | 0.0152 (9) | 0.0214 (10) | −0.0008 (7) | 0.0114 (8) | 0.0009 (7) |
O8 | 0.0126 (9) | 0.0152 (9) | 0.0199 (10) | −0.0002 (7) | 0.0068 (7) | −0.0003 (7) |
O9 | 0.0144 (9) | 0.0182 (9) | 0.0170 (9) | −0.0009 (7) | 0.0064 (8) | −0.0004 (7) |
O10 | 0.0128 (9) | 0.0209 (10) | 0.0171 (9) | 0.0007 (7) | 0.0058 (8) | 0.0009 (7) |
O11 | 0.0167 (9) | 0.0171 (9) | 0.0182 (10) | 0.0016 (7) | 0.0073 (8) | −0.0006 (7) |
O12 | 0.0169 (9) | 0.0148 (9) | 0.0171 (9) | 0.0006 (7) | 0.0087 (8) | 0.0004 (7) |
O13 | 0.0132 (8) | 0.0154 (9) | 0.0153 (9) | 0.0007 (7) | 0.0055 (7) | −0.0002 (7) |
O14 | 0.0174 (9) | 0.0150 (9) | 0.0162 (9) | 0.0004 (7) | 0.0079 (8) | 0.0003 (7) |
O15 | 0.0146 (9) | 0.0142 (9) | 0.0179 (9) | −0.0007 (7) | 0.0072 (8) | −0.0001 (7) |
O16 | 0.0136 (9) | 0.0153 (9) | 0.0153 (9) | 0.0019 (7) | 0.0064 (7) | 0.0002 (7) |
O17 | 0.0155 (9) | 0.0154 (9) | 0.0229 (10) | −0.0005 (7) | 0.0102 (8) | −0.0014 (7) |
O18 | 0.0209 (10) | 0.0187 (10) | 0.0245 (11) | −0.0053 (8) | 0.0123 (8) | −0.0037 (8) |
O19 | 0.0143 (9) | 0.0163 (9) | 0.0185 (10) | −0.0010 (7) | 0.0064 (8) | 0.0003 (7) |
O20 | 0.0124 (8) | 0.0151 (9) | 0.0158 (9) | 0.0005 (7) | 0.0055 (7) | 0.0001 (7) |
O101 | 0.0212 (10) | 0.0180 (10) | 0.0231 (11) | −0.0012 (8) | 0.0061 (8) | 0.0034 (8) |
O201 | 0.0323 (11) | 0.0190 (10) | 0.0292 (12) | −0.0017 (8) | 0.0197 (10) | −0.0001 (8) |
O301 | 0.0579 (16) | 0.0260 (12) | 0.0432 (14) | −0.0008 (11) | 0.0372 (13) | −0.0037 (10) |
S101 | 0.0234 (3) | 0.0148 (3) | 0.0213 (4) | 0.0001 (3) | 0.0073 (3) | −0.0001 (2) |
S201 | 0.0208 (3) | 0.0210 (3) | 0.0178 (3) | −0.0030 (3) | 0.0098 (3) | −0.0007 (3) |
S301 | 0.0369 (4) | 0.0244 (4) | 0.0368 (4) | 0.0036 (3) | 0.0236 (4) | 0.0004 (3) |
V1 | 0.0127 (2) | 0.0132 (2) | 0.0137 (2) | −0.00062 (16) | 0.00454 (18) | −0.00080 (16) |
V2 | 0.0148 (2) | 0.0135 (2) | 0.0144 (2) | 0.00056 (16) | 0.00518 (18) | 0.00008 (16) |
V3 | 0.0141 (2) | 0.0119 (2) | 0.0155 (2) | 0.00181 (16) | 0.00641 (18) | 0.00042 (16) |
V4 | 0.0134 (2) | 0.0120 (2) | 0.0160 (2) | 0.00060 (16) | 0.00710 (18) | −0.00085 (16) |
V5 | 0.0150 (2) | 0.0127 (2) | 0.0159 (2) | 0.00051 (16) | 0.00876 (18) | −0.00093 (16) |
V6 | 0.0148 (2) | 0.0125 (2) | 0.0165 (2) | −0.00062 (16) | 0.00837 (18) | −0.00031 (16) |
V7 | 0.0132 (2) | 0.0133 (2) | 0.0160 (2) | −0.00094 (16) | 0.00679 (18) | −0.00065 (16) |
Geometric parameters (Å, º) top
C101—S101 | 1.770 (3) | O5—V5 | 1.6057 (19) |
C101—H10A | 0.9800 | O6—V6 | 1.6017 (19) |
C101—H10B | 0.9800 | O8—V1 | 1.7958 (19) |
C101—H10C | 0.9800 | O8—V2 | 1.9191 (19) |
C102—S101 | 1.783 (3) | O9—V4i | 1.8205 (19) |
C102—H10D | 0.9800 | O9—V3 | 1.8647 (19) |
C102—H10E | 0.9800 | O10—V7i | 1.786 (2) |
C102—H10F | 0.9800 | O10—V1 | 1.801 (2) |
C201—S201 | 1.770 (3) | O11—V3 | 1.7472 (19) |
C201—H20A | 0.9800 | O11—V2 | 1.8662 (19) |
C201—H20B | 0.9800 | O12—V2 | 1.9235 (19) |
C201—H20C | 0.9800 | O12—V5 | 1.9323 (19) |
C202—S201 | 1.780 (3) | O12—V1 | 1.9607 (19) |
C202—H20D | 0.9800 | O13—V4i | 1.9030 (19) |
C202—H20E | 0.9800 | O13—V7 | 1.9162 (19) |
C202—H20F | 0.9800 | O13—V3 | 1.9737 (19) |
C301—S301 | 1.761 (4) | O14—V2 | 1.7878 (19) |
C301—H30A | 0.9800 | O14—V6 | 1.8337 (19) |
C301—H30B | 0.9800 | O15—V4 | 1.9103 (19) |
C301—H30C | 0.9800 | O15—V1 | 1.9368 (19) |
C302—S301 | 1.776 (3) | O15—V5 | 1.9519 (19) |
C302—H30D | 0.9800 | O16—V3 | 1.9283 (18) |
C302—H30E | 0.9800 | O16—V6 | 1.9393 (18) |
C302—H30F | 0.9800 | O16—V7 | 1.9662 (19) |
N1A—N2A | 1.181 (3) | O17—V5 | 1.7766 (19) |
N2A—N1Ai | 1.181 (3) | O17—V6 | 1.8186 (19) |
N1—H1 | 0.869 (18) | O18—V7 | 1.603 (2) |
N1—H2 | 0.877 (18) | O19—V4 | 1.8243 (19) |
N1—H3 | 0.850 (18) | O19—V5 | 1.8309 (19) |
N1—H4 | 0.863 (19) | O20—V7 | 1.8267 (19) |
N2—H5 | 0.89 (2) | O20—V6 | 1.8983 (19) |
N2—H6 | 0.908 (18) | O101—S101 | 1.541 (2) |
N2—H7 | 0.875 (17) | O201—S201 | 1.526 (2) |
N2—H8 | 0.890 (19) | O301—S301 | 1.511 (2) |
N3—H9 | 0.877 (18) | V1—V2 | 2.9179 (6) |
N3—H10 | 0.861 (18) | V1—V5 | 3.0542 (6) |
N3—H11 | 0.869 (18) | V3—V4i | 2.9025 (6) |
N3—H12 | 0.876 (18) | V3—V7 | 3.0517 (6) |
N4—H13 | 0.878 (18) | V4—O9i | 1.8205 (19) |
N4—H14 | 0.869 (18) | V4—O13i | 1.9029 (19) |
O1—V1 | 1.6038 (19) | V4—V5 | 2.8755 (6) |
O2—V2 | 1.598 (2) | V4—V3i | 2.9026 (6) |
O3—V3 | 1.6089 (19) | V6—V7 | 2.9365 (6) |
O4—V4 | 1.6016 (19) | V7—O10i | 1.786 (2) |
| | | |
S101—C101—H10A | 109.5 | O14—V2—O8 | 153.89 (8) |
S101—C101—H10B | 109.5 | O11—V2—O8 | 91.13 (8) |
H10A—C101—H10B | 109.5 | O2—V2—O12 | 106.14 (9) |
S101—C101—H10C | 109.5 | O14—V2—O12 | 88.35 (8) |
H10A—C101—H10C | 109.5 | O11—V2—O12 | 148.91 (9) |
H10B—C101—H10C | 109.5 | O8—V2—O12 | 78.54 (8) |
S101—C102—H10D | 109.5 | O2—V2—V1 | 108.30 (8) |
S101—C102—H10E | 109.5 | O14—V2—V1 | 126.00 (6) |
H10D—C102—H10E | 109.5 | O11—V2—V1 | 121.98 (6) |
S101—C102—H10F | 109.5 | O8—V2—V1 | 36.76 (6) |
H10D—C102—H10F | 109.5 | O12—V2—V1 | 41.79 (6) |
H10E—C102—H10F | 109.5 | O3—V3—O11 | 104.81 (10) |
S201—C201—H20A | 109.5 | O3—V3—O9 | 103.75 (9) |
S201—C201—H20B | 109.5 | O11—V3—O9 | 96.40 (9) |
H20A—C201—H20B | 109.5 | O3—V3—O16 | 103.54 (9) |
S201—C201—H20C | 109.5 | O11—V3—O16 | 94.32 (9) |
H20A—C201—H20C | 109.5 | O9—V3—O16 | 146.95 (8) |
H20B—C201—H20C | 109.5 | O3—V3—O13 | 108.21 (9) |
S201—C202—H20D | 109.5 | O11—V3—O13 | 146.90 (9) |
S201—C202—H20E | 109.5 | O9—V3—O13 | 78.09 (8) |
H20D—C202—H20E | 109.5 | O16—V3—O13 | 75.93 (8) |
S201—C202—H20F | 109.5 | O3—V3—V4i | 109.70 (7) |
H20D—C202—H20F | 109.5 | O11—V3—V4i | 127.16 (7) |
H20E—C202—H20F | 109.5 | O9—V3—V4i | 37.50 (6) |
S301—C301—H30A | 109.5 | O16—V3—V4i | 114.32 (6) |
S301—C301—H30B | 109.5 | O13—V3—V4i | 40.60 (5) |
H30A—C301—H30B | 109.5 | O3—V3—V7 | 115.39 (7) |
S301—C301—H30C | 109.5 | O11—V3—V7 | 122.44 (6) |
H30A—C301—H30C | 109.5 | O9—V3—V7 | 111.08 (6) |
H30B—C301—H30C | 109.5 | O16—V3—V7 | 38.85 (6) |
S301—C302—H30D | 109.5 | O13—V3—V7 | 37.66 (5) |
S301—C302—H30E | 109.5 | V4i—V3—V7 | 75.618 (16) |
H30D—C302—H30E | 109.5 | O4—V4—O9i | 106.60 (10) |
S301—C302—H30F | 109.5 | O4—V4—O19 | 106.89 (9) |
H30D—C302—H30F | 109.5 | O9i—V4—O19 | 92.14 (9) |
H30E—C302—H30F | 109.5 | O4—V4—O13i | 107.10 (9) |
N1Ai—N2A—N1A | 180.0 | O9i—V4—O13i | 81.01 (8) |
H1—N1—H2 | 112 (3) | O19—V4—O13i | 145.88 (9) |
H1—N1—H3 | 111 (3) | O4—V4—O15 | 105.58 (9) |
H2—N1—H3 | 100 (3) | O9i—V4—O15 | 147.76 (9) |
H1—N1—H4 | 106 (4) | O19—V4—O15 | 80.39 (8) |
H2—N1—H4 | 109 (4) | O13i—V4—O15 | 87.79 (8) |
H3—N1—H4 | 119 (4) | O4—V4—V5 | 107.98 (7) |
H5—N2—H6 | 117 (5) | O9i—V4—V5 | 125.84 (6) |
H5—N2—H7 | 107 (5) | O19—V4—V5 | 38.21 (6) |
H6—N2—H7 | 105 (3) | O13i—V4—V5 | 124.94 (6) |
H5—N2—H8 | 111 (5) | O15—V4—V5 | 42.44 (6) |
H6—N2—H8 | 107 (3) | O4—V4—V3i | 111.40 (7) |
H7—N2—H8 | 110 (3) | O9i—V4—V3i | 38.58 (6) |
H9—N3—H10 | 113 (3) | O19—V4—V3i | 123.89 (6) |
H9—N3—H11 | 111 (3) | O13i—V4—V3i | 42.45 (6) |
H10—N3—H11 | 110 (3) | O15—V4—V3i | 124.21 (6) |
H9—N3—H12 | 109 (3) | V5—V4—V3i | 140.58 (2) |
H10—N3—H12 | 105 (3) | O5—V5—O17 | 106.73 (10) |
H11—N3—H12 | 108 (3) | O5—V5—O19 | 104.84 (10) |
H13—N4—H14 | 109 (3) | O17—V5—O19 | 95.65 (9) |
V1—O8—V2 | 103.48 (9) | O5—V5—O12 | 103.62 (9) |
V4i—O9—V3 | 103.92 (9) | O17—V5—O12 | 92.54 (8) |
V7i—O10—V1 | 154.23 (12) | O19—V5—O12 | 146.61 (8) |
V3—O11—V2 | 139.14 (11) | O5—V5—O15 | 107.21 (9) |
V2—O12—V5 | 137.69 (10) | O17—V5—O15 | 145.87 (9) |
V2—O12—V1 | 97.39 (8) | O19—V5—O15 | 79.12 (8) |
V5—O12—V1 | 103.36 (9) | O12—V5—O15 | 76.08 (8) |
V4i—O13—V7 | 145.98 (11) | O5—V5—V4 | 107.49 (8) |
V4i—O13—V3 | 96.94 (8) | O17—V5—V4 | 128.05 (7) |
V7—O13—V3 | 103.35 (9) | O19—V5—V4 | 38.04 (6) |
V2—O14—V6 | 128.28 (11) | O12—V5—V4 | 115.54 (6) |
V4—O15—V1 | 147.44 (11) | O15—V5—V4 | 41.33 (6) |
V4—O15—V5 | 96.23 (8) | O5—V5—V1 | 115.10 (8) |
V1—O15—V5 | 103.52 (9) | O17—V5—V1 | 120.27 (6) |
V3—O16—V6 | 138.04 (10) | O19—V5—V1 | 111.65 (6) |
V3—O16—V7 | 103.18 (9) | O12—V5—V1 | 38.65 (6) |
V6—O16—V7 | 97.51 (8) | O15—V5—V1 | 38.07 (5) |
V5—O17—V6 | 142.00 (11) | V4—V5—V1 | 76.970 (16) |
V4—O19—V5 | 103.75 (9) | O6—V6—O17 | 104.39 (9) |
V7—O20—V6 | 104.04 (9) | O6—V6—O14 | 102.88 (9) |
O101—S101—C101 | 104.06 (14) | O17—V6—O14 | 88.91 (9) |
O101—S101—C102 | 106.84 (14) | O6—V6—O20 | 100.37 (9) |
C101—S101—C102 | 99.12 (19) | O17—V6—O20 | 94.21 (8) |
O201—S201—C201 | 105.88 (15) | O14—V6—O20 | 154.98 (8) |
O201—S201—C202 | 105.45 (14) | O6—V6—O16 | 107.77 (9) |
C201—S201—C202 | 98.11 (17) | O17—V6—O16 | 147.80 (8) |
O301—S301—C301 | 104.12 (17) | O14—V6—O16 | 85.61 (8) |
O301—S301—C302 | 104.75 (16) | O20—V6—O16 | 78.56 (8) |
C301—S301—C302 | 98.25 (19) | O6—V6—V7 | 110.69 (7) |
O1—V1—O8 | 105.88 (9) | O17—V6—V7 | 122.99 (7) |
O1—V1—O10 | 106.74 (10) | O14—V6—V7 | 123.34 (6) |
O8—V1—O10 | 97.13 (9) | O20—V6—V7 | 37.12 (6) |
O1—V1—O15 | 106.12 (9) | O16—V6—V7 | 41.59 (5) |
O8—V1—O15 | 144.10 (8) | O18—V7—O10i | 107.45 (10) |
O10—V1—O15 | 88.86 (8) | O18—V7—O20 | 104.50 (9) |
O1—V1—O12 | 105.14 (9) | O10i—V7—O20 | 96.14 (9) |
O8—V1—O12 | 80.57 (8) | O18—V7—O13 | 104.90 (9) |
O10—V1—O12 | 147.37 (9) | O10i—V7—O13 | 90.97 (8) |
O15—V1—O12 | 75.77 (8) | O20—V7—O13 | 146.02 (8) |
O1—V1—V2 | 111.31 (7) | O18—V7—O16 | 105.71 (9) |
O8—V1—V2 | 39.76 (6) | O10i—V7—O16 | 146.56 (8) |
O10—V1—V2 | 128.38 (7) | O20—V7—O16 | 79.58 (8) |
O15—V1—V2 | 111.79 (6) | O13—V7—O16 | 76.39 (8) |
O12—V1—V2 | 40.82 (5) | O18—V7—V6 | 112.56 (7) |
O1—V1—V5 | 115.30 (8) | O10i—V7—V6 | 125.11 (7) |
O8—V1—V5 | 111.26 (6) | O20—V7—V6 | 38.84 (6) |
O10—V1—V5 | 118.42 (6) | O13—V7—V6 | 112.44 (6) |
O15—V1—V5 | 38.42 (6) | O16—V7—V6 | 40.90 (5) |
O12—V1—V5 | 37.99 (6) | O18—V7—V3 | 114.74 (8) |
V2—V1—V5 | 74.005 (16) | O10i—V7—V3 | 119.95 (6) |
O2—V2—O14 | 104.14 (10) | O20—V7—V3 | 111.56 (6) |
O2—V2—O11 | 104.61 (10) | O13—V7—V3 | 39.00 (6) |
O14—V2—O11 | 88.62 (9) | O16—V7—V3 | 37.97 (5) |
O2—V2—O8 | 101.18 (10) | V6—V7—V3 | 74.148 (16) |
| | | |
V2—O8—V1—O1 | 104.41 (10) | V5—O19—V4—O13i | 77.03 (17) |
V2—O8—V1—O10 | −145.87 (9) | V5—O19—V4—O15 | 5.67 (9) |
V2—O8—V1—O15 | −47.89 (18) | V5—O19—V4—V3i | 130.64 (6) |
V2—O8—V1—O12 | 1.23 (8) | V6—O17—V5—O5 | −135.74 (19) |
V2—O8—V1—V5 | −21.57 (10) | V6—O17—V5—O19 | 116.89 (19) |
V7i—O10—V1—O1 | −97.0 (3) | V6—O17—V5—O12 | −30.70 (19) |
V7i—O10—V1—O8 | 154.0 (3) | V6—O17—V5—O15 | 38.0 (3) |
V7i—O10—V1—O15 | 9.5 (3) | V6—O17—V5—V4 | 94.94 (19) |
V7i—O10—V1—O12 | 70.3 (3) | V6—O17—V5—V1 | −2.3 (2) |
V7i—O10—V1—V2 | 126.7 (2) | V4—O19—V5—O5 | 99.54 (11) |
V7i—O10—V1—V5 | 35.1 (3) | V4—O19—V5—O17 | −151.47 (10) |
V6—O14—V2—O2 | 176.45 (13) | V4—O19—V5—O12 | −48.11 (19) |
V6—O14—V2—O11 | −78.83 (14) | V4—O19—V5—O15 | −5.58 (9) |
V6—O14—V2—O8 | 10.9 (3) | V4—O19—V5—V1 | −25.72 (10) |
V6—O14—V2—O12 | 70.22 (13) | V5—O17—V6—O6 | 152.04 (18) |
V6—O14—V2—V1 | 50.77 (16) | V5—O17—V6—O14 | 49.03 (19) |
V3—O11—V2—O2 | 153.00 (17) | V5—O17—V6—O20 | −106.12 (19) |
V3—O11—V2—O14 | 48.74 (18) | V5—O17—V6—O16 | −31.0 (3) |
V3—O11—V2—O8 | −105.14 (18) | V5—O17—V6—V7 | −80.99 (19) |
V3—O11—V2—O12 | −35.8 (3) | V2—O14—V6—O6 | −178.79 (13) |
V3—O11—V2—V1 | −83.95 (18) | V2—O14—V6—O17 | −74.28 (14) |
V2—O11—V3—O3 | −134.58 (17) | V2—O14—V6—O20 | 23.4 (3) |
V2—O11—V3—O9 | 119.34 (17) | V2—O14—V6—O16 | 73.97 (13) |
V2—O11—V3—O16 | −29.34 (18) | V2—O14—V6—V7 | 55.46 (15) |
V2—O11—V3—O13 | 41.4 (3) | V7—O20—V6—O6 | −110.70 (10) |
V2—O11—V3—V4i | 95.79 (17) | V7—O20—V6—O17 | 143.83 (9) |
V2—O11—V3—V7 | −0.7 (2) | V7—O20—V6—O14 | 47.4 (2) |
V4i—O9—V3—O3 | 104.55 (11) | V7—O20—V6—O16 | −4.47 (8) |
V4i—O9—V3—O11 | −148.46 (10) | V6—O20—V7—O18 | 108.09 (10) |
V4i—O9—V3—O16 | −40.32 (19) | V6—O20—V7—O10i | −142.08 (9) |
V4i—O9—V3—O13 | −1.54 (9) | V6—O20—V7—O13 | −41.11 (18) |
V4i—O9—V3—V7 | −20.01 (10) | V6—O20—V7—O16 | 4.39 (8) |
V5—O19—V4—O4 | −97.81 (11) | V6—O20—V7—V3 | −16.46 (10) |
V5—O19—V4—O9i | 154.12 (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)]·6C2H6OS | F(000) = 3904 |
Mr = 1958.24 | Dx = 2.084 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71075 Å |
a = 19.352 (6) Å | Cell parameters from 12134 reflections |
b = 24.753 (6) Å | θ = 3.1–27.5° |
c = 14.561 (5) Å | µ = 2.30 mm−1 |
β = 116.537 (6)° | T = 83 K |
V = 6240 (3) Å3 | Block, red |
Z = 4 | 0.20 × 0.20 × 0.20 mm |
Data collection top
Rigaku Mercury70 diffractometer | 6028 reflections with I > 2σ(I) |
Detector resolution: 14.629 pixels mm-1 | Rint = 0.058 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: numerical (NUMABS; Rigaku, 1999) | h = −25→24 |
Tmin = 0.656, Tmax = 0.892 | k = −32→26 |
33228 measured reflections | l = −18→18 |
7133 independent reflections | |
Refinement top
Refinement on F2 | 34 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.052 | H 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 reflections | Δρmax = 1.32 e Å−3 |
446 parameters | Δρmin = −1.19 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
N1A | 0.7537 (2) | 0.7752 (2) | 0.5711 (4) | 0.0660 (13) | 0.5 |
C1A | 0.7500 | 0.7500 | 0.5000 | 0.0562 (18) | |
O1A | 0.7537 (2) | 0.7752 (2) | 0.5711 (4) | 0.0660 (13) | 0.5 |
C101 | 0.8153 (3) | 0.6944 (2) | 0.0603 (4) | 0.0478 (13) | |
H10A | 0.8113 | 0.7313 | 0.0818 | 0.072* | |
H10B | 0.8039 | 0.6945 | −0.0124 | 0.072* | |
H10C | 0.7782 | 0.6712 | 0.0702 | 0.072* | |
C102 | 0.9588 (3) | 0.7102 (2) | 0.0812 (4) | 0.0381 (10) | |
H10D | 0.9603 | 0.7478 | 0.1032 | 0.057* | |
H10E | 1.0117 | 0.6968 | 0.1048 | 0.057* | |
H10F | 0.9315 | 0.7083 | 0.0061 | 0.057* | |
C201 | 0.6713 (3) | 0.5946 (3) | −0.0401 (5) | 0.0662 (18) | |
H20A | 0.6892 | 0.6182 | −0.0792 | 0.099* | |
H20B | 0.6714 | 0.6147 | 0.0179 | 0.099* | |
H20C | 0.7059 | 0.5634 | −0.0144 | 0.099* | |
C202 | 0.5270 (3) | 0.6331 (2) | −0.1287 (5) | 0.0524 (13) | |
H20D | 0.5367 | 0.6586 | −0.1731 | 0.079* | |
H20E | 0.4715 | 0.6255 | −0.1579 | 0.079* | |
H20F | 0.5446 | 0.6489 | −0.0602 | 0.079* | |
C301 | 0.7821 (3) | 0.4634 (3) | 0.3418 (4) | 0.0508 (13) | |
H30A | 0.7304 | 0.4481 | 0.3027 | 0.076* | |
H30B | 0.8107 | 0.4417 | 0.4036 | 0.076* | |
H30C | 0.7778 | 0.5006 | 0.3615 | 0.076* | |
C302 | 0.7775 (3) | 0.5132 (2) | 0.1739 (4) | 0.0516 (14) | |
H30D | 0.7264 | 0.4988 | 0.1281 | 0.077* | |
H30E | 0.7716 | 0.5449 | 0.2102 | 0.077* | |
H30F | 0.8045 | 0.5237 | 0.1335 | 0.077* | |
N1 | 0.94349 (18) | 0.74946 (15) | 0.5919 (3) | 0.0259 (7) | |
N2 | 0.4759 (2) | 0.55728 (19) | 0.3866 (3) | 0.0380 (9) | |
N3 | 1.00367 (19) | 0.42590 (15) | 0.5084 (3) | 0.0274 (7) | |
N4 | 1.0000 | 0.5389 (2) | 0.2500 | 0.0346 (11) | |
O1 | 0.66049 (16) | 0.69295 (12) | 0.8013 (2) | 0.0300 (6) | |
O2 | 0.87290 (15) | 0.61142 (11) | 0.3006 (2) | 0.0270 (6) | |
O3 | 0.87722 (15) | 0.55917 (12) | 0.5708 (2) | 0.0296 (6) | |
O4 | 0.60313 (15) | 0.84766 (12) | 0.1513 (2) | 0.0294 (6) | |
O5 | 0.59304 (16) | 0.69119 (12) | 0.0826 (2) | 0.0318 (6) | |
O6 | 0.63351 (15) | 0.54545 (11) | 0.3417 (2) | 0.0283 (6) | |
O7 | 0.63247 (15) | 0.57562 (11) | 0.6132 (2) | 0.0279 (6) | |
O8 | 0.85230 (14) | 0.71827 (11) | 0.3140 (2) | 0.0257 (6) | |
O9 | 0.86041 (14) | 0.65714 (11) | 0.6444 (2) | 0.0259 (6) | |
O10 | 0.88852 (14) | 0.65233 (11) | 0.48018 (19) | 0.0227 (5) | |
O11 | 0.76523 (14) | 0.60696 (11) | 0.3862 (2) | 0.0245 (5) | |
O12 | 0.73314 (14) | 0.65834 (11) | 0.2187 (2) | 0.0247 (5) | |
O13 | 0.74289 (14) | 0.65810 (11) | 0.6895 (2) | 0.0235 (5) | |
O14 | 0.71148 (14) | 0.76181 (11) | 0.2096 (2) | 0.0241 (5) | |
O15 | 0.73272 (14) | 0.60444 (10) | 0.5274 (2) | 0.0223 (5) | |
O16 | 0.62192 (14) | 0.64481 (11) | 0.2666 (2) | 0.0261 (6) | |
O17 | 0.61009 (14) | 0.68530 (11) | 0.5944 (2) | 0.0245 (5) | |
O18 | 0.59830 (13) | 0.75254 (11) | 0.2409 (2) | 0.0243 (5) | |
O19 | 0.59836 (14) | 0.63028 (11) | 0.4341 (2) | 0.0259 (6) | |
O101 | 0.91065 (18) | 0.61291 (12) | 0.0962 (2) | 0.0356 (7) | |
O201 | 0.5582 (2) | 0.53720 (15) | −0.0507 (3) | 0.0532 (9) | |
O301 | 0.91143 (16) | 0.48762 (12) | 0.3345 (2) | 0.0320 (6) | |
V1 | 0.68285 (3) | 0.71460 (3) | 0.71404 (5) | 0.02183 (15) | |
V2 | 0.82410 (3) | 0.65129 (3) | 0.33605 (5) | 0.02248 (16) | |
V3 | 0.83309 (3) | 0.61563 (3) | 0.53367 (5) | 0.02199 (15) | |
V4 | 0.65320 (3) | 0.81265 (3) | 0.25186 (5) | 0.02161 (15) | |
V5 | 0.65127 (3) | 0.69857 (3) | 0.20126 (5) | 0.02330 (16) | |
V6 | 0.66303 (3) | 0.60582 (3) | 0.37839 (5) | 0.02196 (15) | |
V7 | 0.65902 (3) | 0.62768 (3) | 0.57216 (5) | 0.02141 (15) | |
S101 | 0.90979 (6) | 0.66979 (4) | 0.13455 (7) | 0.0296 (2) | |
S201 | 0.57772 (8) | 0.57232 (5) | −0.11969 (11) | 0.0465 (3) | |
S301 | 0.83194 (6) | 0.46290 (4) | 0.26469 (8) | 0.0312 (2) | |
H1 | 0.9935 (12) | 0.748 (2) | 0.630 (3) | 0.046 (15)* | |
H2 | 0.929 (3) | 0.7195 (14) | 0.556 (4) | 0.049 (16)* | |
H3 | 0.937 (2) | 0.7766 (12) | 0.551 (2) | 0.012 (9)* | |
H4 | 0.932 (4) | 0.759 (3) | 0.641 (4) | 0.08 (2)* | |
H5 | 0.509 (2) | 0.5849 (15) | 0.404 (4) | 0.045 (15)* | |
H6 | 0.440 (4) | 0.556 (4) | 0.322 (3) | 0.14 (4)* | |
H7 | 0.461 (3) | 0.555 (2) | 0.437 (3) | 0.031 (12)* | |
H8 | 0.4998 (19) | 0.5260 (10) | 0.393 (3) | 0.006 (8)* | |
H9 | 0.9744 (19) | 0.4097 (15) | 0.533 (3) | 0.013 (9)* | |
H10 | 1.032 (2) | 0.4004 (16) | 0.498 (4) | 0.041 (14)* | |
H11 | 0.978 (2) | 0.4426 (19) | 0.451 (2) | 0.040 (14)* | |
H12 | 1.032 (2) | 0.4496 (15) | 0.555 (3) | 0.028 (12)* | |
H13 | 0.965 (2) | 0.5581 (18) | 0.200 (3) | 0.035 (13)* | |
H14 | 0.977 (2) | 0.5161 (16) | 0.275 (4) | 0.036 (13)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
N1A | 0.0324 (18) | 0.072 (3) | 0.076 (3) | 0.010 (2) | 0.008 (2) | 0.030 (2) |
C1A | 0.021 (3) | 0.057 (5) | 0.073 (4) | 0.008 (3) | 0.006 (3) | 0.038 (3) |
O1A | 0.0324 (18) | 0.072 (3) | 0.076 (3) | 0.010 (2) | 0.008 (2) | 0.030 (2) |
C101 | 0.031 (2) | 0.064 (4) | 0.043 (3) | 0.013 (2) | 0.011 (2) | −0.003 (2) |
C102 | 0.040 (2) | 0.038 (3) | 0.039 (2) | −0.0043 (19) | 0.020 (2) | 0.003 (2) |
C201 | 0.047 (3) | 0.091 (5) | 0.063 (4) | 0.017 (3) | 0.027 (3) | 0.027 (4) |
C202 | 0.055 (3) | 0.045 (3) | 0.063 (3) | 0.003 (2) | 0.031 (3) | −0.008 (3) |
C301 | 0.035 (2) | 0.071 (4) | 0.051 (3) | −0.001 (2) | 0.024 (2) | −0.011 (3) |
C302 | 0.037 (2) | 0.038 (3) | 0.051 (3) | −0.003 (2) | −0.006 (2) | 0.006 (2) |
N1 | 0.0213 (15) | 0.0242 (18) | 0.0284 (18) | 0.0008 (13) | 0.0079 (13) | 0.0072 (14) |
N2 | 0.0306 (19) | 0.048 (3) | 0.034 (2) | −0.0045 (17) | 0.0131 (17) | 0.0084 (18) |
N3 | 0.0251 (16) | 0.0256 (18) | 0.0319 (19) | 0.0034 (13) | 0.0129 (14) | 0.0040 (15) |
N4 | 0.048 (3) | 0.027 (3) | 0.033 (3) | 0.000 | 0.022 (3) | 0.000 |
O1 | 0.0318 (14) | 0.0346 (16) | 0.0289 (15) | −0.0046 (12) | 0.0183 (12) | 0.0022 (12) |
O2 | 0.0261 (13) | 0.0271 (15) | 0.0312 (14) | 0.0015 (11) | 0.0161 (11) | 0.0001 (11) |
O3 | 0.0273 (13) | 0.0282 (15) | 0.0362 (15) | 0.0068 (11) | 0.0167 (12) | 0.0042 (12) |
O4 | 0.0278 (13) | 0.0286 (15) | 0.0259 (14) | 0.0045 (11) | 0.0068 (11) | 0.0024 (11) |
O5 | 0.0308 (14) | 0.0329 (16) | 0.0231 (14) | −0.0010 (12) | 0.0042 (11) | 0.0000 (12) |
O6 | 0.0276 (13) | 0.0239 (14) | 0.0326 (15) | −0.0042 (11) | 0.0128 (12) | −0.0037 (11) |
O7 | 0.0295 (13) | 0.0234 (14) | 0.0332 (15) | −0.0014 (11) | 0.0161 (12) | 0.0039 (11) |
O8 | 0.0217 (12) | 0.0239 (14) | 0.0328 (14) | 0.0009 (10) | 0.0133 (11) | 0.0005 (11) |
O9 | 0.0188 (11) | 0.0310 (15) | 0.0267 (13) | −0.0002 (10) | 0.0092 (10) | −0.0007 (11) |
O10 | 0.0196 (11) | 0.0225 (14) | 0.0251 (13) | −0.0007 (10) | 0.0091 (10) | −0.0009 (10) |
O11 | 0.0192 (12) | 0.0274 (14) | 0.0266 (14) | −0.0030 (10) | 0.0101 (10) | 0.0003 (11) |
O12 | 0.0255 (12) | 0.0233 (14) | 0.0261 (14) | −0.0006 (10) | 0.0123 (11) | 0.0008 (11) |
O13 | 0.0211 (12) | 0.0226 (13) | 0.0266 (13) | 0.0012 (10) | 0.0106 (10) | −0.0019 (11) |
O14 | 0.0238 (12) | 0.0242 (14) | 0.0252 (13) | 0.0006 (10) | 0.0117 (10) | 0.0004 (11) |
O15 | 0.0198 (11) | 0.0212 (13) | 0.0244 (13) | −0.0004 (10) | 0.0087 (10) | 0.0007 (10) |
O16 | 0.0213 (12) | 0.0284 (15) | 0.0253 (13) | −0.0006 (10) | 0.0075 (10) | 0.0014 (11) |
O17 | 0.0201 (11) | 0.0243 (14) | 0.0273 (14) | 0.0015 (10) | 0.0089 (10) | 0.0000 (11) |
O18 | 0.0182 (11) | 0.0239 (14) | 0.0296 (14) | 0.0007 (10) | 0.0095 (10) | −0.0010 (11) |
O19 | 0.0201 (12) | 0.0294 (15) | 0.0282 (14) | 0.0007 (10) | 0.0107 (11) | 0.0011 (11) |
O101 | 0.0430 (17) | 0.0298 (16) | 0.0413 (17) | 0.0022 (13) | 0.0253 (14) | 0.0008 (13) |
O201 | 0.076 (2) | 0.044 (2) | 0.060 (2) | 0.0023 (18) | 0.050 (2) | −0.0025 (17) |
O301 | 0.0291 (13) | 0.0279 (15) | 0.0337 (16) | −0.0015 (11) | 0.0093 (12) | 0.0036 (12) |
V1 | 0.0213 (3) | 0.0224 (3) | 0.0243 (3) | −0.0007 (2) | 0.0125 (2) | 0.0016 (2) |
V2 | 0.0212 (3) | 0.0218 (3) | 0.0258 (3) | 0.0011 (2) | 0.0118 (3) | 0.0010 (2) |
V3 | 0.0184 (3) | 0.0227 (3) | 0.0246 (3) | 0.0013 (2) | 0.0094 (2) | 0.0007 (2) |
V4 | 0.0181 (3) | 0.0226 (3) | 0.0215 (3) | 0.0010 (2) | 0.0066 (2) | 0.0017 (2) |
V5 | 0.0212 (3) | 0.0231 (3) | 0.0236 (3) | −0.0004 (2) | 0.0082 (2) | 0.0002 (2) |
V6 | 0.0201 (3) | 0.0207 (3) | 0.0244 (3) | −0.0024 (2) | 0.0093 (2) | −0.0004 (2) |
V7 | 0.0190 (3) | 0.0210 (3) | 0.0245 (3) | −0.0010 (2) | 0.0101 (2) | 0.0016 (2) |
S101 | 0.0298 (5) | 0.0335 (6) | 0.0266 (5) | 0.0042 (4) | 0.0136 (4) | 0.0011 (4) |
S201 | 0.0530 (7) | 0.0419 (7) | 0.0565 (8) | 0.0053 (5) | 0.0352 (6) | 0.0001 (6) |
S301 | 0.0326 (5) | 0.0243 (5) | 0.0326 (5) | −0.0005 (4) | 0.0110 (4) | −0.0017 (4) |
Geometric parameters (Å, º) top
N1A—C1A | 1.183 (6) | O5—V5 | 1.597 (3) |
C1A—O1Ai | 1.183 (6) | O6—V6 | 1.604 (3) |
C1A—N1Ai | 1.183 (6) | O7—V7 | 1.599 (3) |
C101—S101 | 1.766 (5) | O8—V1i | 1.773 (3) |
C101—H10A | 0.9800 | O8—V2 | 1.818 (3) |
C101—H10B | 0.9800 | O9—V3 | 1.781 (3) |
C101—H10C | 0.9800 | O9—V4i | 1.808 (3) |
C102—S101 | 1.779 (4) | O10—V3 | 1.825 (3) |
C102—H10D | 0.9800 | O10—V2 | 1.903 (3) |
C102—H10E | 0.9800 | O11—V6 | 1.930 (3) |
C102—H10F | 0.9800 | O11—V2 | 1.944 (3) |
C201—S201 | 1.747 (6) | O11—V3 | 1.965 (3) |
C201—H20A | 0.9800 | O12—V5 | 1.791 (3) |
C201—H20B | 0.9800 | O12—V2 | 1.833 (3) |
C201—H20C | 0.9800 | O13—V7 | 1.908 (3) |
C202—S201 | 1.769 (5) | O13—V4i | 1.940 (3) |
C202—H20D | 0.9800 | O13—V1 | 1.951 (3) |
C202—H20E | 0.9800 | O14—V5 | 1.923 (3) |
C202—H20F | 0.9800 | O14—V1i | 1.931 (3) |
C301—S301 | 1.776 (5) | O14—V4 | 1.964 (3) |
C301—H30A | 0.9800 | O15—V7 | 1.903 (3) |
C301—H30B | 0.9800 | O15—V3 | 1.923 (3) |
C301—H30C | 0.9800 | O15—V6 | 1.978 (3) |
C302—S301 | 1.779 (5) | O16—V6 | 1.748 (3) |
C302—H30D | 0.9800 | O16—V5 | 1.866 (3) |
C302—H30E | 0.9800 | O17—V7 | 1.819 (3) |
C302—H30F | 0.9800 | O17—V1 | 1.831 (3) |
N1—H1 | 0.88 (2) | O18—V4 | 1.793 (3) |
N1—H2 | 0.88 (2) | O18—V5 | 1.923 (3) |
N1—H3 | 0.867 (19) | O19—V7 | 1.820 (3) |
N1—H4 | 0.86 (2) | O19—V6 | 1.871 (3) |
N2—H5 | 0.89 (2) | O101—S101 | 1.517 (3) |
N2—H6 | 0.88 (2) | O201—S201 | 1.499 (4) |
N2—H7 | 0.903 (19) | O301—S301 | 1.542 (3) |
N2—H8 | 0.884 (18) | V1—O8i | 1.773 (3) |
N3—H9 | 0.889 (18) | V1—O14i | 1.931 (3) |
N3—H10 | 0.886 (19) | V1—V7 | 2.8736 (11) |
N3—H11 | 0.867 (19) | V1—V4i | 3.0594 (13) |
N3—H12 | 0.877 (19) | V2—V3 | 2.9396 (12) |
N4—H13 | 0.881 (19) | V3—V6 | 3.0582 (12) |
N4—H14 | 0.884 (19) | V4—O9i | 1.808 (3) |
O1—V1 | 1.607 (3) | V4—O13i | 1.940 (3) |
O2—V2 | 1.602 (3) | V4—V5 | 2.9144 (11) |
O3—V3 | 1.601 (3) | V4—V1i | 3.0594 (13) |
O4—V4 | 1.602 (3) | V6—V7 | 2.9077 (12) |
| | | |
N1A—C1A—O1Ai | 180.0 (6) | O12—V2—V3 | 123.57 (9) |
N1A—C1A—N1Ai | 180.0 (6) | O10—V2—V3 | 37.01 (8) |
O1Ai—C1A—N1Ai | 0.0 (4) | O11—V2—V3 | 41.51 (8) |
S101—C101—H10A | 109.5 | O3—V3—O9 | 107.45 (14) |
S101—C101—H10B | 109.5 | O3—V3—O10 | 104.62 (13) |
H10A—C101—H10B | 109.5 | O9—V3—O10 | 96.06 (12) |
S101—C101—H10C | 109.5 | O3—V3—O15 | 105.38 (13) |
H10A—C101—H10C | 109.5 | O9—V3—O15 | 90.65 (11) |
H10B—C101—H10C | 109.5 | O10—V3—O15 | 145.61 (12) |
S101—C102—H10D | 109.5 | O3—V3—O11 | 105.61 (13) |
S101—C102—H10E | 109.5 | O9—V3—O11 | 146.64 (12) |
H10D—C102—H10E | 109.5 | O10—V3—O11 | 79.70 (11) |
S101—C102—H10F | 109.5 | O15—V3—O11 | 76.39 (11) |
H10D—C102—H10F | 109.5 | O3—V3—V2 | 112.47 (10) |
H10E—C102—H10F | 109.5 | O9—V3—V2 | 125.20 (10) |
S201—C201—H20A | 109.5 | O10—V3—V2 | 38.89 (8) |
S201—C201—H20B | 109.5 | O15—V3—V2 | 112.32 (8) |
H20A—C201—H20B | 109.5 | O11—V3—V2 | 40.95 (8) |
S201—C201—H20C | 109.5 | O3—V3—V6 | 114.58 (11) |
H20A—C201—H20C | 109.5 | O9—V3—V6 | 120.08 (8) |
H20B—C201—H20C | 109.5 | O10—V3—V6 | 111.57 (9) |
S201—C202—H20D | 109.5 | O15—V3—V6 | 39.02 (8) |
S201—C202—H20E | 109.5 | O11—V3—V6 | 37.86 (7) |
H20D—C202—H20E | 109.5 | V2—V3—V6 | 74.14 (3) |
S201—C202—H20F | 109.5 | O4—V4—O18 | 105.97 (13) |
H20D—C202—H20F | 109.5 | O4—V4—O9i | 106.61 (14) |
H20E—C202—H20F | 109.5 | O18—V4—O9i | 96.67 (12) |
S301—C301—H30A | 109.5 | O4—V4—O13i | 106.56 (13) |
S301—C301—H30B | 109.5 | O18—V4—O13i | 143.64 (12) |
H30A—C301—H30B | 109.5 | O9i—V4—O13i | 89.26 (11) |
S301—C301—H30C | 109.5 | O4—V4—O14 | 104.91 (13) |
H30A—C301—H30C | 109.5 | O18—V4—O14 | 80.84 (11) |
H30B—C301—H30C | 109.5 | O9i—V4—O14 | 147.78 (12) |
S301—C302—H30D | 109.5 | O13i—V4—O14 | 75.50 (11) |
S301—C302—H30E | 109.5 | O4—V4—V5 | 111.03 (11) |
H30D—C302—H30E | 109.5 | O18—V4—V5 | 39.95 (8) |
S301—C302—H30F | 109.5 | O9i—V4—V5 | 128.47 (9) |
H30D—C302—H30F | 109.5 | O13i—V4—V5 | 111.51 (8) |
H30E—C302—H30F | 109.5 | O14—V4—V5 | 40.89 (8) |
H1—N1—H2 | 109 (5) | O4—V4—V1i | 115.30 (11) |
H1—N1—H3 | 104 (4) | O18—V4—V1i | 111.20 (8) |
H2—N1—H3 | 110 (4) | O9i—V4—V1i | 118.91 (8) |
H1—N1—H4 | 96 (6) | O13i—V4—V1i | 38.27 (8) |
H2—N1—H4 | 127 (6) | O14—V4—V1i | 37.84 (8) |
H3—N1—H4 | 109 (6) | V5—V4—V1i | 73.90 (2) |
H5—N2—H6 | 117 (7) | O5—V5—O12 | 104.01 (14) |
H5—N2—H7 | 106 (5) | O5—V5—O16 | 104.01 (14) |
H6—N2—H7 | 118 (7) | O12—V5—O16 | 89.01 (12) |
H5—N2—H8 | 111 (4) | O5—V5—O18 | 101.01 (14) |
H6—N2—H8 | 102 (7) | O12—V5—O18 | 154.20 (12) |
H7—N2—H8 | 102 (4) | O16—V5—O18 | 91.02 (12) |
H9—N3—H10 | 107 (4) | O5—V5—O14 | 106.01 (14) |
H9—N3—H11 | 114 (4) | O12—V5—O14 | 88.34 (12) |
H10—N3—H11 | 108 (5) | O16—V5—O14 | 149.59 (12) |
H9—N3—H12 | 107 (4) | O18—V5—O14 | 78.74 (11) |
H10—N3—H12 | 112 (4) | O5—V5—V4 | 107.91 (11) |
H11—N3—H12 | 109 (5) | O12—V5—V4 | 126.32 (9) |
H13—N4—H14 | 109 (4) | O16—V5—V4 | 122.30 (9) |
V1i—O8—V2 | 141.34 (15) | O18—V5—V4 | 36.80 (8) |
V3—O9—V4i | 154.16 (16) | O14—V5—V4 | 41.95 (8) |
V3—O10—V2 | 104.10 (12) | O6—V6—O16 | 104.96 (14) |
V6—O11—V2 | 138.02 (15) | O6—V6—O19 | 103.79 (13) |
V6—O11—V3 | 103.45 (12) | O16—V6—O19 | 96.36 (12) |
V2—O11—V3 | 97.53 (11) | O6—V6—O11 | 103.67 (13) |
V5—O12—V2 | 127.28 (15) | O16—V6—O11 | 94.30 (12) |
V7—O13—V4i | 147.26 (15) | O19—V6—O11 | 146.77 (12) |
V7—O13—V1 | 96.26 (11) | O6—V6—O15 | 108.43 (13) |
V4i—O13—V1 | 103.70 (12) | O16—V6—O15 | 146.54 (12) |
V5—O14—V1i | 137.61 (15) | O19—V6—O15 | 77.89 (11) |
V5—O14—V4 | 97.16 (11) | O11—V6—O15 | 75.95 (11) |
V1i—O14—V4 | 103.55 (13) | O6—V6—V7 | 109.68 (10) |
V7—O15—V3 | 146.69 (15) | O16—V6—V7 | 127.02 (10) |
V7—O15—V6 | 97.03 (11) | O19—V6—V7 | 37.41 (8) |
V3—O15—V6 | 103.24 (12) | O11—V6—V7 | 114.28 (8) |
V6—O16—V5 | 138.84 (15) | O15—V6—V7 | 40.51 (8) |
V7—O17—V1 | 103.87 (12) | O6—V6—V3 | 115.20 (10) |
V4—O18—V5 | 103.25 (12) | O16—V6—V3 | 122.43 (9) |
V7—O19—V6 | 103.96 (13) | O19—V6—V3 | 111.17 (9) |
O1—V1—O8i | 106.48 (14) | O11—V6—V3 | 38.68 (8) |
O1—V1—O17 | 104.85 (14) | O15—V6—V3 | 37.75 (7) |
O8i—V1—O17 | 95.69 (12) | V7—V6—V3 | 75.78 (3) |
O1—V1—O14i | 103.62 (13) | O7—V7—O17 | 106.61 (13) |
O8i—V1—O14i | 92.75 (12) | O7—V7—O19 | 106.53 (14) |
O17—V1—O14i | 146.55 (11) | O17—V7—O19 | 92.21 (12) |
O1—V1—O13 | 107.39 (14) | O7—V7—O15 | 107.42 (13) |
O8i—V1—O13 | 145.95 (12) | O17—V7—O15 | 145.83 (12) |
O17—V1—O13 | 79.01 (11) | O19—V7—O15 | 81.07 (12) |
O14i—V1—O13 | 76.01 (11) | O7—V7—O13 | 105.69 (13) |
O1—V1—V7 | 107.79 (11) | O17—V7—O13 | 80.42 (11) |
O8i—V1—V7 | 127.90 (9) | O19—V7—O13 | 147.73 (12) |
O17—V1—V7 | 37.92 (8) | O15—V7—O13 | 87.60 (11) |
O14i—V1—V7 | 115.42 (8) | O7—V7—V1 | 108.07 (11) |
O13—V1—V7 | 41.31 (8) | O17—V7—V1 | 38.21 (8) |
O1—V1—V4i | 115.12 (11) | O19—V7—V1 | 125.77 (9) |
O8i—V1—V4i | 120.49 (9) | O15—V7—V1 | 124.65 (8) |
O17—V1—V4i | 111.59 (8) | O13—V7—V1 | 42.43 (8) |
O14i—V1—V4i | 38.60 (8) | O7—V7—V6 | 111.39 (11) |
O13—V1—V4i | 38.03 (8) | O17—V7—V6 | 124.07 (9) |
V7—V1—V4i | 76.90 (2) | O19—V7—V6 | 38.64 (8) |
O2—V2—O8 | 103.78 (13) | O15—V7—V6 | 42.46 (8) |
O2—V2—O12 | 102.55 (13) | O13—V7—V6 | 124.15 (8) |
O8—V2—O12 | 89.29 (12) | V1—V7—V6 | 140.50 (3) |
O2—V2—O10 | 100.00 (13) | O101—S101—C101 | 105.9 (2) |
O8—V2—O10 | 94.70 (12) | O101—S101—C102 | 105.4 (2) |
O12—V2—O10 | 155.45 (11) | C101—S101—C102 | 98.4 (3) |
O2—V2—O11 | 107.58 (13) | O201—S201—C201 | 103.6 (3) |
O8—V2—O11 | 148.60 (12) | O201—S201—C202 | 104.2 (2) |
O12—V2—O11 | 85.62 (12) | C201—S201—C202 | 99.0 (3) |
O10—V2—O11 | 78.39 (11) | O301—S301—C301 | 104.1 (2) |
O2—V2—V3 | 110.17 (10) | O301—S301—C302 | 107.3 (2) |
O8—V2—V3 | 123.74 (9) | C301—S301—C302 | 99.0 (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)]·6C2H6OS | F(000) = 3944 |
Mr = 1978.23 | Dx = 2.083 Mg m−3 |
Monoclinic, C2/c | Cu Kα radiation, λ = 1.54178 Å |
a = 19.3923 (7) Å | Cell parameters from 9911 reflections |
b = 24.9031 (9) Å | θ = 3.6–72.8° |
c = 14.5785 (5) Å | µ = 19.38 mm−1 |
β = 116.374 (1)° | T = 90 K |
V = 6307.6 (4) Å3 | Block, red |
Z = 4 | 0.18 × 0.06 × 0.03 mm |
Data collection top
Bruker D8 goniometer diffractometer | 6245 independent reflections |
Radiation source: sealed tube | 5607 reflections with I > 2σ(I) |
Detector resolution: 10.4167 pixels mm-1 | Rint = 0.065 |
ω scans | θmax = 72.9°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2015) | h = −22→24 |
Tmin = 0.32, Tmax = 0.64 | k = −30→30 |
24260 measured reflections | l = −18→17 |
Refinement top
Refinement on F2 | 14 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.052 | H 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 reflections | Δρmax = 2.47 e Å−3 |
464 parameters | Δρmin = −1.05 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C101 | 0.3159 (3) | 0.3072 (3) | 0.0605 (5) | 0.0561 (15) | |
H10A | 0.3111 | 0.2707 | 0.0821 | 0.084* | |
H10B | 0.2790 | 0.3308 | 0.0696 | 0.084* | |
H10C | 0.3052 | 0.3069 | −0.0118 | 0.084* | |
C102 | 0.4595 (3) | 0.2899 (2) | 0.0828 (4) | 0.0417 (11) | |
H10D | 0.4602 | 0.2526 | 0.1049 | 0.063* | |
H10E | 0.4328 | 0.2917 | 0.0079 | 0.063* | |
H10F | 0.5124 | 0.3028 | 0.1067 | 0.063* | |
C201 | 0.2816 (3) | 0.5353 (3) | 0.3433 (5) | 0.0603 (17) | |
H20A | 0.2304 | 0.5508 | 0.3038 | 0.090* | |
H20B | 0.2765 | 0.4985 | 0.3632 | 0.090* | |
H20C | 0.3101 | 0.5569 | 0.4049 | 0.090* | |
C202 | 0.2782 (4) | 0.4849 (2) | 0.1758 (5) | 0.0644 (19) | |
H20D | 0.2276 | 0.4994 | 0.1295 | 0.097* | |
H20E | 0.3058 | 0.4745 | 0.1363 | 0.097* | |
H20F | 0.2715 | 0.4533 | 0.2113 | 0.097* | |
C301 | 0.5296 (4) | 1.1335 (2) | 0.3742 (5) | 0.0490 (13) | |
H30A | 0.5385 | 1.1587 | 0.3290 | 0.073* | |
H30B | 0.4743 | 1.1263 | 0.3469 | 0.073* | |
H30C | 0.5484 | 1.1493 | 0.4427 | 0.073* | |
C302 | 0.6745 (4) | 1.0962 (4) | 0.4612 (6) | 0.086 (3) | |
H30D | 0.6913 | 1.1199 | 0.4214 | 0.129* | |
H30E | 0.6744 | 1.1161 | 0.5191 | 0.129* | |
H30F | 0.7098 | 1.0656 | 0.4868 | 0.129* | |
N1 | 0.5548 (2) | 0.74974 (15) | 0.4071 (3) | 0.0274 (7) | |
N2 | 0.4757 (3) | 0.9443 (2) | 0.3871 (3) | 0.0419 (10) | |
N3 | 0.5046 (2) | 0.57496 (15) | 0.5062 (3) | 0.0283 (7) | |
N4 | 0.5000 | 0.4622 (3) | 0.2500 | 0.0467 (15) | |
O1 | 0.90631 (19) | 0.69409 (13) | 0.9141 (2) | 0.0367 (7) | |
O2 | 0.87044 (19) | 0.54839 (13) | 0.6644 (2) | 0.0352 (7) | |
O3 | 0.86960 (18) | 0.57370 (12) | 0.3869 (2) | 0.0333 (7) | |
O4 | 0.6582 (2) | 0.80429 (14) | 0.8013 (3) | 0.0380 (7) | |
O5 | 0.62811 (18) | 0.61269 (12) | 0.6961 (2) | 0.0310 (6) | |
O6 | 0.62730 (18) | 0.55657 (12) | 0.4347 (3) | 0.0344 (7) | |
O7 | 0.60536 (18) | 0.65166 (13) | 0.1488 (2) | 0.0340 (7) | |
O8 | 0.89874 (16) | 0.75564 (12) | 0.7546 (2) | 0.0287 (6) | |
O9 | 0.90382 (17) | 0.62897 (12) | 0.5638 (2) | 0.0298 (6) | |
O10 | 0.87858 (18) | 0.64925 (13) | 0.7290 (2) | 0.0332 (7) | |
O11 | 0.76996 (16) | 0.60089 (12) | 0.4722 (2) | 0.0265 (6) | |
O12 | 0.78633 (17) | 0.76324 (12) | 0.7863 (2) | 0.0278 (6) | |
O13 | 0.76742 (18) | 0.66031 (12) | 0.7779 (2) | 0.0306 (6) | |
O14 | 0.75892 (16) | 0.65484 (11) | 0.3061 (2) | 0.0262 (6) | |
O15 | 0.73774 (17) | 0.60987 (12) | 0.6126 (2) | 0.0284 (6) | |
O16 | 0.64799 (17) | 0.71894 (12) | 0.6797 (3) | 0.0324 (7) | |
O17 | 0.64201 (16) | 0.65165 (13) | 0.3519 (2) | 0.0317 (7) | |
O18 | 0.61448 (17) | 0.65276 (11) | 0.5163 (2) | 0.0275 (6) | |
O19 | 0.60790 (17) | 0.81703 (12) | 0.5968 (2) | 0.0305 (6) | |
O101 | 0.4124 (2) | 0.38740 (13) | 0.0969 (3) | 0.0368 (7) | |
O201 | 0.41004 (19) | 0.50976 (13) | 0.3374 (3) | 0.0394 (7) | |
O301 | 0.5621 (3) | 1.03701 (16) | 0.4524 (3) | 0.0544 (10) | |
S101 | 0.41029 (7) | 0.33103 (5) | 0.13547 (8) | 0.0332 (2) | |
S201 | 0.33194 (7) | 0.53467 (4) | 0.26748 (9) | 0.0383 (3) | |
S301 | 0.57964 (8) | 1.07230 (6) | 0.38166 (11) | 0.0477 (3) | |
V1 | 0.84840 (4) | 0.70103 (3) | 0.79648 (5) | 0.02557 (17) | |
V2 | 0.83987 (4) | 0.60764 (3) | 0.62123 (5) | 0.02597 (18) | |
V3 | 0.84201 (4) | 0.62556 (3) | 0.42602 (5) | 0.02467 (17) | |
V4 | 0.68084 (4) | 0.78623 (3) | 0.71250 (5) | 0.02388 (17) | |
V5 | 0.67594 (4) | 0.65262 (3) | 0.66017 (5) | 0.02548 (18) | |
V6 | 0.67051 (4) | 0.61344 (3) | 0.46614 (5) | 0.02427 (17) | |
V7 | 0.65552 (4) | 0.68437 (3) | 0.25099 (5) | 0.02345 (17) | |
N1A | 0.7500 | 0.7500 | 0.5000 | 0.0343 (12) | |
O1A | 0.7363 (6) | 0.7457 (6) | 0.5748 (9) | 0.070 (3) | 0.5 |
O2A | 0.7892 (6) | 0.7173 (6) | 0.4880 (14) | 0.085 (4) | 0.5 |
O3A | 0.7310 (7) | 0.7904 (4) | 0.4461 (10) | 0.081 (3) | 0.5 |
H1 | 0.572 (3) | 0.7217 (17) | 0.447 (4) | 0.049 (17)* | |
H2 | 0.577 (4) | 0.764 (3) | 0.373 (5) | 0.059 (19)* | |
H3 | 0.5060 (14) | 0.743 (2) | 0.369 (3) | 0.035 (14)* | |
H4 | 0.566 (4) | 0.772 (3) | 0.459 (4) | 0.07 (2)* | |
H5 | 0.507 (4) | 0.916 (2) | 0.408 (6) | 0.08 (3)* | |
H6 | 0.455 (3) | 0.944 (2) | 0.431 (3) | 0.040 (15)* | |
H7 | 0.504 (3) | 0.9734 (16) | 0.397 (5) | 0.053 (19)* | |
H8 | 0.444 (4) | 0.953 (3) | 0.323 (2) | 0.08 (2)* | |
H9 | 0.535 (3) | 0.600 (2) | 0.501 (6) | 0.07 (2)* | |
H10 | 0.536 (2) | 0.5509 (17) | 0.548 (3) | 0.033 (13)* | |
H11 | 0.477 (3) | 0.560 (2) | 0.447 (3) | 0.052 (17)* | |
H12 | 0.470 (3) | 0.588 (2) | 0.523 (4) | 0.045 (16)* | |
H13 | 0.477 (4) | 0.486 (2) | 0.273 (5) | 0.07 (2)* | |
H14 | 0.468 (3) | 0.441 (2) | 0.203 (3) | 0.046 (16)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C101 | 0.034 (3) | 0.074 (4) | 0.052 (3) | −0.012 (3) | 0.012 (3) | 0.010 (3) |
C102 | 0.051 (3) | 0.039 (3) | 0.038 (3) | 0.002 (2) | 0.022 (2) | −0.005 (2) |
C201 | 0.036 (3) | 0.092 (5) | 0.052 (4) | 0.002 (3) | 0.019 (3) | 0.015 (3) |
C202 | 0.049 (3) | 0.039 (3) | 0.060 (4) | 0.000 (3) | −0.017 (3) | −0.010 (3) |
C301 | 0.058 (3) | 0.044 (3) | 0.051 (3) | 0.006 (2) | 0.030 (3) | −0.006 (2) |
C302 | 0.054 (4) | 0.134 (8) | 0.073 (5) | 0.004 (4) | 0.031 (4) | 0.041 (5) |
N1 | 0.0177 (16) | 0.0314 (18) | 0.0276 (19) | 0.0006 (15) | 0.0051 (15) | −0.0031 (15) |
N2 | 0.035 (2) | 0.059 (3) | 0.031 (2) | 0.008 (2) | 0.014 (2) | −0.002 (2) |
N3 | 0.0256 (18) | 0.0283 (18) | 0.031 (2) | 0.0001 (15) | 0.0124 (16) | −0.0016 (15) |
N4 | 0.069 (5) | 0.037 (3) | 0.037 (4) | 0.000 | 0.027 (4) | 0.000 |
O1 | 0.0374 (17) | 0.0406 (17) | 0.0241 (16) | −0.0015 (14) | 0.0064 (14) | 0.0002 (13) |
O2 | 0.0380 (17) | 0.0327 (16) | 0.0325 (17) | 0.0094 (13) | 0.0135 (15) | 0.0064 (13) |
O3 | 0.0351 (17) | 0.0328 (16) | 0.0340 (17) | 0.0043 (13) | 0.0171 (14) | −0.0033 (13) |
O4 | 0.0396 (18) | 0.0493 (19) | 0.0343 (18) | 0.0060 (15) | 0.0248 (16) | −0.0016 (14) |
O5 | 0.0326 (16) | 0.0301 (15) | 0.0311 (16) | −0.0040 (12) | 0.0149 (14) | 0.0002 (12) |
O6 | 0.0346 (17) | 0.0319 (15) | 0.0407 (18) | −0.0085 (13) | 0.0204 (15) | −0.0049 (13) |
O7 | 0.0346 (17) | 0.0369 (16) | 0.0201 (15) | −0.0053 (13) | 0.0027 (13) | −0.0004 (12) |
O8 | 0.0228 (14) | 0.0325 (15) | 0.0301 (15) | 0.0040 (12) | 0.0112 (12) | 0.0039 (12) |
O9 | 0.0233 (14) | 0.0370 (16) | 0.0270 (15) | −0.0001 (12) | 0.0094 (12) | 0.0002 (12) |
O10 | 0.0280 (15) | 0.0395 (17) | 0.0276 (16) | 0.0011 (13) | 0.0082 (13) | −0.0065 (13) |
O11 | 0.0252 (14) | 0.0305 (14) | 0.0238 (14) | 0.0009 (12) | 0.0108 (12) | 0.0013 (11) |
O12 | 0.0262 (14) | 0.0301 (14) | 0.0283 (15) | 0.0012 (12) | 0.0130 (12) | 0.0010 (12) |
O13 | 0.0322 (16) | 0.0316 (15) | 0.0284 (16) | 0.0013 (12) | 0.0140 (13) | 0.0006 (12) |
O14 | 0.0249 (14) | 0.0275 (14) | 0.0260 (15) | −0.0007 (11) | 0.0111 (12) | 0.0009 (11) |
O15 | 0.0261 (15) | 0.0333 (15) | 0.0258 (15) | 0.0031 (12) | 0.0116 (13) | 0.0008 (12) |
O16 | 0.0273 (15) | 0.0249 (14) | 0.0464 (19) | −0.0041 (12) | 0.0177 (15) | −0.0054 (13) |
O17 | 0.0206 (14) | 0.0474 (18) | 0.0255 (15) | 0.0048 (13) | 0.0089 (12) | 0.0108 (13) |
O18 | 0.0277 (15) | 0.0281 (14) | 0.0283 (15) | 0.0026 (12) | 0.0138 (13) | 0.0032 (11) |
O19 | 0.0256 (15) | 0.0325 (15) | 0.0336 (17) | −0.0008 (12) | 0.0134 (13) | 0.0010 (12) |
O101 | 0.050 (2) | 0.0317 (16) | 0.0411 (19) | −0.0010 (14) | 0.0317 (17) | −0.0001 (13) |
O201 | 0.0375 (18) | 0.0341 (17) | 0.0335 (17) | −0.0029 (14) | 0.0040 (15) | −0.0082 (13) |
O301 | 0.075 (3) | 0.052 (2) | 0.054 (2) | 0.002 (2) | 0.045 (2) | −0.0025 (18) |
S101 | 0.0355 (6) | 0.0392 (6) | 0.0282 (5) | −0.0030 (5) | 0.0172 (5) | 0.0017 (4) |
S201 | 0.0415 (6) | 0.0276 (5) | 0.0362 (6) | −0.0030 (4) | 0.0085 (5) | −0.0017 (4) |
S301 | 0.0570 (8) | 0.0513 (7) | 0.0468 (7) | 0.0111 (6) | 0.0340 (7) | 0.0053 (6) |
V1 | 0.0226 (4) | 0.0298 (4) | 0.0205 (4) | 0.0003 (3) | 0.0062 (3) | 0.0003 (3) |
V2 | 0.0256 (4) | 0.0275 (4) | 0.0227 (4) | 0.0054 (3) | 0.0088 (3) | 0.0030 (3) |
V3 | 0.0219 (3) | 0.0277 (3) | 0.0241 (4) | 0.0025 (3) | 0.0100 (3) | 0.0004 (3) |
V4 | 0.0232 (3) | 0.0276 (3) | 0.0246 (4) | 0.0002 (3) | 0.0140 (3) | −0.0011 (3) |
V5 | 0.0260 (4) | 0.0246 (3) | 0.0287 (4) | −0.0025 (3) | 0.0147 (3) | −0.0020 (3) |
V6 | 0.0235 (4) | 0.0257 (3) | 0.0245 (4) | −0.0018 (3) | 0.0114 (3) | 0.0013 (3) |
V7 | 0.0219 (3) | 0.0267 (3) | 0.0186 (3) | −0.0004 (3) | 0.0062 (3) | 0.0015 (3) |
N1A | 0.018 (2) | 0.036 (3) | 0.044 (3) | 0.001 (2) | 0.009 (2) | −0.009 (3) |
O1A | 0.053 (6) | 0.098 (8) | 0.074 (7) | −0.030 (6) | 0.043 (6) | −0.041 (6) |
O2A | 0.043 (5) | 0.087 (9) | 0.124 (12) | −0.001 (5) | 0.035 (7) | −0.057 (9) |
O3A | 0.056 (6) | 0.053 (6) | 0.082 (8) | −0.005 (5) | −0.015 (6) | −0.014 (6) |
Geometric parameters (Å, º) top
C101—S101 | 1.767 (6) | O10—V2 | 1.749 (3) |
C101—H10A | 0.9800 | O10—V1 | 1.867 (3) |
C101—H10B | 0.9800 | O11—V3 | 1.902 (3) |
C101—H10C | 0.9800 | O11—V6 | 1.917 (3) |
C102—S101 | 1.789 (5) | O11—V2 | 1.993 (3) |
C102—H10D | 0.9800 | O12—V1 | 1.927 (3) |
C102—H10E | 0.9800 | O12—V4 | 1.927 (3) |
C102—H10F | 0.9800 | O12—V7i | 1.953 (3) |
C201—S201 | 1.770 (6) | O13—V1 | 1.786 (3) |
C201—H20A | 0.9800 | O13—V5 | 1.851 (3) |
C201—H20B | 0.9800 | O14—V3 | 1.919 (3) |
C201—H20C | 0.9800 | O14—V7 | 1.943 (3) |
C202—S201 | 1.781 (6) | O14—V4i | 1.968 (3) |
C202—H20D | 0.9800 | O15—V2 | 1.929 (3) |
C202—H20E | 0.9800 | O15—V5 | 1.947 (3) |
C202—H20F | 0.9800 | O15—V6 | 1.947 (3) |
C301—S301 | 1.785 (6) | O16—V4 | 1.781 (3) |
C301—H30A | 0.9800 | O16—V5 | 1.800 (3) |
C301—H30B | 0.9800 | O17—V6 | 1.780 (3) |
C301—H30C | 0.9800 | O17—V7 | 1.799 (3) |
C302—S301 | 1.785 (8) | O18—V6 | 1.839 (3) |
C302—H30D | 0.9800 | O18—V5 | 1.897 (3) |
C302—H30E | 0.9800 | O19—V4 | 1.820 (3) |
C302—H30F | 0.9800 | O19—V3i | 1.840 (3) |
N1—H1 | 0.88 (2) | O101—S101 | 1.519 (3) |
N1—H2 | 0.86 (2) | O201—S201 | 1.532 (4) |
N1—H3 | 0.87 (2) | O301—S301 | 1.504 (4) |
N1—H4 | 0.88 (2) | V1—V7i | 2.9297 (10) |
N2—H5 | 0.88 (2) | V2—V3 | 2.8992 (10) |
N2—H6 | 0.89 (2) | V2—V6 | 3.0531 (10) |
N2—H7 | 0.88 (2) | V3—O19i | 1.840 (3) |
N2—H8 | 0.88 (2) | V3—V4i | 2.8816 (10) |
N3—H9 | 0.88 (2) | V4—O14i | 1.968 (3) |
N3—H10 | 0.88 (2) | V4—V3i | 2.8817 (10) |
N3—H11 | 0.88 (2) | V4—V7i | 3.0642 (9) |
N3—H12 | 0.87 (2) | V5—V6 | 2.9497 (10) |
N4—H13 | 0.89 (2) | V7—O8i | 1.808 (3) |
N4—H14 | 0.88 (2) | V7—O12i | 1.953 (3) |
O1—V1 | 1.588 (3) | V7—V1i | 2.9296 (10) |
O2—V2 | 1.610 (3) | V7—V4i | 3.0642 (9) |
O3—V3 | 1.597 (3) | N1A—O2Ai | 1.180 (9) |
O4—V4 | 1.604 (3) | N1A—O2A | 1.180 (9) |
O5—V5 | 1.598 (3) | N1A—O3A | 1.228 (12) |
O6—V6 | 1.605 (3) | N1A—O3Ai | 1.228 (12) |
O7—V7 | 1.594 (3) | N1A—O1Ai | 1.236 (10) |
O8—V7i | 1.808 (3) | N1A—O1A | 1.236 (10) |
O8—V1 | 1.925 (3) | O1A—O2Ai | 1.236 (19) |
O9—V3 | 1.828 (3) | O2A—O1Ai | 1.236 (19) |
O9—V2 | 1.856 (3) | | |
| | | |
S101—C101—H10A | 109.5 | O2—V2—V6 | 114.89 (13) |
S101—C101—H10B | 109.5 | O10—V2—V6 | 121.91 (11) |
H10A—C101—H10B | 109.5 | O9—V2—V6 | 111.53 (10) |
S101—C101—H10C | 109.5 | O15—V2—V6 | 38.25 (9) |
H10A—C101—H10C | 109.5 | O11—V2—V6 | 37.77 (8) |
H10B—C101—H10C | 109.5 | V3—V2—V6 | 75.26 (2) |
S101—C102—H10D | 109.5 | O3—V3—O9 | 105.65 (15) |
S101—C102—H10E | 109.5 | O3—V3—O19i | 106.05 (15) |
H10D—C102—H10E | 109.5 | O9—V3—O19i | 91.24 (14) |
S101—C102—H10F | 109.5 | O3—V3—O11 | 106.27 (15) |
H10D—C102—H10F | 109.5 | O9—V3—O11 | 81.50 (13) |
H10E—C102—H10F | 109.5 | O19i—V3—O11 | 147.65 (13) |
S201—C201—H20A | 109.5 | O3—V3—O14 | 105.14 (15) |
S201—C201—H20B | 109.5 | O9—V3—O14 | 149.21 (13) |
H20A—C201—H20B | 109.5 | O19i—V3—O14 | 80.63 (13) |
S201—C201—H20C | 109.5 | O11—V3—O14 | 89.62 (12) |
H20A—C201—H20C | 109.5 | O3—V3—V4i | 109.76 (12) |
H20B—C201—H20C | 109.5 | O9—V3—V4i | 123.81 (10) |
S201—C202—H20D | 109.5 | O19i—V3—V4i | 37.83 (10) |
S201—C202—H20E | 109.5 | O11—V3—V4i | 125.85 (9) |
H20D—C202—H20E | 109.5 | O14—V3—V4i | 42.81 (8) |
S201—C202—H20F | 109.5 | O3—V3—V2 | 112.27 (12) |
H20D—C202—H20F | 109.5 | O9—V3—V2 | 38.42 (9) |
H20E—C202—H20F | 109.5 | O19i—V3—V2 | 122.42 (10) |
S301—C301—H30A | 109.5 | O11—V3—V2 | 43.10 (9) |
S301—C301—H30B | 109.5 | O14—V3—V2 | 125.47 (9) |
H30A—C301—H30B | 109.5 | V4i—V3—V2 | 137.77 (3) |
S301—C301—H30C | 109.5 | O4—V4—O16 | 106.67 (17) |
H30A—C301—H30C | 109.5 | O4—V4—O19 | 104.53 (16) |
H30B—C301—H30C | 109.5 | O16—V4—O19 | 96.30 (15) |
S301—C302—H30D | 109.5 | O4—V4—O12 | 103.64 (15) |
S301—C302—H30E | 109.5 | O16—V4—O12 | 91.99 (14) |
H30D—C302—H30E | 109.5 | O19—V4—O12 | 146.87 (13) |
S301—C302—H30F | 109.5 | O4—V4—O14i | 107.09 (16) |
H30D—C302—H30F | 109.5 | O16—V4—O14i | 145.90 (13) |
H30E—C302—H30F | 109.5 | O19—V4—O14i | 79.78 (13) |
H1—N1—H2 | 125 (6) | O12—V4—O14i | 75.56 (12) |
H1—N1—H3 | 105 (5) | O4—V4—V3i | 109.85 (13) |
H2—N1—H3 | 112 (6) | O16—V4—V3i | 127.15 (12) |
H1—N1—H4 | 93 (6) | O19—V4—V3i | 38.31 (9) |
H2—N1—H4 | 104 (7) | O12—V4—V3i | 114.34 (9) |
H3—N1—H4 | 117 (6) | O14i—V4—V3i | 41.49 (9) |
H5—N2—H6 | 102 (6) | O4—V4—V7i | 115.22 (13) |
H5—N2—H7 | 109 (7) | O16—V4—V7i | 119.40 (10) |
H6—N2—H7 | 109 (6) | O19—V4—V7i | 112.26 (10) |
H5—N2—H8 | 126 (7) | O12—V4—V7i | 38.14 (9) |
H6—N2—H8 | 116 (6) | O14i—V4—V7i | 38.14 (8) |
H7—N2—H8 | 95 (6) | V3i—V4—V7i | 76.38 (2) |
H9—N3—H10 | 105 (6) | O5—V5—O16 | 105.04 (15) |
H9—N3—H11 | 112 (6) | O5—V5—O13 | 102.54 (15) |
H10—N3—H11 | 109 (5) | O16—V5—O13 | 89.44 (14) |
H9—N3—H12 | 112 (6) | O5—V5—O18 | 101.08 (15) |
H10—N3—H12 | 116 (5) | O16—V5—O18 | 95.03 (14) |
H11—N3—H12 | 102 (5) | O13—V5—O18 | 153.90 (13) |
H13—N4—H14 | 114 (6) | O5—V5—O15 | 108.38 (14) |
V7i—O8—V1 | 103.35 (13) | O16—V5—O15 | 146.57 (14) |
V3—O9—V2 | 103.83 (15) | O13—V5—O15 | 84.21 (13) |
V2—O10—V1 | 140.61 (19) | O18—V5—O15 | 77.93 (12) |
V3—O11—V6 | 144.42 (17) | O5—V5—V6 | 109.25 (11) |
V3—O11—V2 | 96.18 (13) | O16—V5—V6 | 124.77 (11) |
V6—O11—V2 | 102.69 (13) | O13—V5—V6 | 122.34 (10) |
V1—O12—V4 | 138.92 (17) | O18—V5—V6 | 37.17 (9) |
V1—O12—V7i | 98.07 (13) | O15—V5—V6 | 40.77 (9) |
V4—O12—V7i | 104.31 (14) | O6—V6—O17 | 107.40 (16) |
V1—O13—V5 | 127.96 (17) | O6—V6—O18 | 104.91 (14) |
V3—O14—V7 | 144.63 (16) | O17—V6—O18 | 95.45 (13) |
V3—O14—V4i | 95.70 (13) | O6—V6—O11 | 104.86 (14) |
V7—O14—V4i | 103.15 (13) | O17—V6—O11 | 91.03 (13) |
V2—O15—V5 | 140.29 (17) | O18—V6—O11 | 145.99 (13) |
V2—O15—V6 | 103.94 (13) | O6—V6—O15 | 106.43 (15) |
V5—O15—V6 | 98.48 (13) | O17—V6—O15 | 145.96 (14) |
V4—O16—V5 | 143.98 (18) | O18—V6—O15 | 79.29 (13) |
V6—O17—V7 | 155.45 (18) | O11—V6—O15 | 76.84 (12) |
V6—O18—V5 | 104.28 (14) | O6—V6—V5 | 110.92 (12) |
V4—O19—V3i | 103.86 (15) | O17—V6—V5 | 125.78 (11) |
O101—S101—C101 | 105.8 (3) | O18—V6—V5 | 38.55 (9) |
O101—S101—C102 | 105.3 (2) | O11—V6—V5 | 113.78 (9) |
C101—S101—C102 | 98.4 (3) | O15—V6—V5 | 40.75 (8) |
O201—S201—C201 | 104.2 (3) | O6—V6—V2 | 115.03 (13) |
O201—S201—C202 | 107.1 (2) | O17—V6—V2 | 120.20 (10) |
C201—S201—C202 | 100.0 (4) | O18—V6—V2 | 111.22 (10) |
O301—S301—C301 | 105.0 (2) | O11—V6—V2 | 39.55 (9) |
O301—S301—C302 | 103.4 (3) | O15—V6—V2 | 37.81 (8) |
C301—S301—C302 | 97.5 (4) | V5—V6—V2 | 74.75 (2) |
O1—V1—O13 | 104.71 (16) | O7—V7—O17 | 106.40 (16) |
O1—V1—O10 | 104.90 (16) | O7—V7—O8i | 106.19 (15) |
O13—V1—O10 | 89.34 (14) | O17—V7—O8i | 96.75 (14) |
O1—V1—O8 | 101.82 (16) | O7—V7—O14 | 106.41 (15) |
O13—V1—O8 | 152.72 (14) | O17—V7—O14 | 89.35 (12) |
O10—V1—O8 | 89.93 (14) | O8i—V7—O14 | 143.54 (13) |
O1—V1—O12 | 106.78 (16) | O7—V7—O12i | 105.64 (15) |
O13—V1—O12 | 88.15 (13) | O17—V7—O12i | 147.31 (14) |
O10—V1—O12 | 147.80 (14) | O8i—V7—O12i | 80.33 (12) |
O8—V1—O12 | 78.17 (12) | O14—V7—O12i | 75.55 (12) |
O1—V1—V7i | 107.03 (13) | O7—V7—V1i | 109.63 (12) |
O13—V1—V7i | 126.05 (10) | O17—V7—V1i | 129.51 (11) |
O10—V1—V7i | 121.99 (11) | O8i—V7—V1i | 39.74 (9) |
O8—V1—V7i | 36.91 (9) | O14—V7—V1i | 112.34 (9) |
O12—V1—V7i | 41.30 (9) | O12i—V7—V1i | 40.63 (8) |
O2—V2—O10 | 104.81 (16) | O7—V7—V4i | 116.07 (12) |
O2—V2—O9 | 103.57 (15) | O17—V7—V4i | 118.80 (10) |
O10—V2—O9 | 97.43 (14) | O8i—V7—V4i | 110.34 (10) |
O2—V2—O15 | 103.96 (15) | O14—V7—V4i | 38.72 (8) |
O10—V2—O15 | 93.46 (14) | O12i—V7—V4i | 37.55 (9) |
O9—V2—O15 | 146.61 (13) | V1i—V7—V4i | 74.01 (2) |
O2—V2—O11 | 107.62 (15) | O2Ai—N1A—O2A | 180.0 |
O10—V2—O11 | 147.38 (14) | O3A—N1A—O3Ai | 180.0 |
O9—V2—O11 | 78.44 (12) | O2Ai—N1A—O1Ai | 118.5 (9) |
O15—V2—O11 | 75.50 (12) | O2A—N1A—O1Ai | 61.5 (9) |
O2—V2—V3 | 111.17 (12) | O2Ai—N1A—O1A | 61.5 (9) |
O10—V2—V3 | 127.08 (11) | O2A—N1A—O1A | 118.5 (9) |
O9—V2—V3 | 37.74 (9) | O1Ai—N1A—O1A | 180.0 |
O15—V2—V3 | 113.17 (9) | N1A—O1A—O2Ai | 57.0 (7) |
O11—V2—V3 | 40.72 (8) | N1A—O2A—O1Ai | 61.5 (8) |
Symmetry code: (i) −x+3/2, −y+3/2, −z+1. |