K₂[Mo₂O₄(C₂O₄)₂(H₂O)₂]·3H₂O

The crystal and molecular structure of dipotassium di-μ-oxo-bis[aqua(oxalato-O¹,O²)oxomolybdenum(III)] trihydrate, K₂­[Mo₂O₄(C₂O₄)₂(H₂O)₂]·3H₂O, has been determined from X-ray diffraction data. In the dimeric anion, which has approximate twofold symmetry, each Mo atom is in a distorted octahedral coordination, being bonded to one terminal oxo-O atom, two bridging O atoms, two O atoms from the oxalato ligand and one from the water mol­ecule. Bond lengths trans to the multiple-bonded terminal oxo ligand are larger than those in the cis position, confirming the trans influence as a generally valid rule.

Computing details

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLUTON (Spek, 1982) and ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

dipotassium di-µ-oxo-bis[aqua(oxalato-O¹,O²)oxomolybdenum(III)] trihydrate

Crystal data

K2[Mo2O4(C2O4)2(H2O)2]·3H2O	Z = 8
Mr = 600.20	F(000) = 2336
Triclinic, P1	Dx = 2.523 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71069 Å
a = 12.2683 (10) Å	Cell parameters from 30 reflections
b = 15.0622 (17) Å	θ = 8–17°
c = 18.2824 (17) Å	µ = 2.20 mm^−1
α = 81.818 (9)°	T = 293 K
β = 71.050 (7)°	Prism, red
γ = 85.001 (9)°	0.30 × 0.27 × 0.25 mm
V = 3159.7 (5) Å^3

Data collection

Philips PW1100 updated by Stoe diffractometer	θmax = 30.1°, θmin = 2.3°
Radiation source: fine-focus sealed tube	h = −16→17
Graphite monochromator	k = −20→21
ω/θ scans	l = 0→25
18345 measured reflections	3 standard reflections every 90 min
18254 independent reflections	intensity decay: 24.2%
7507 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: heavy-atom method
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.049	Hydrogen site location: difference Fourier map
wR(F^2) = 0.106	H-atom parameters not refined
S = 0.93	Calculated w = 1/[σ^2(Fo^2) + (0.065P)^2] where P = (Fo^2 + 2Fc^2)/3
18254 reflections	(Δ/σ)max = 0.003
907 parameters	Δρmax = 1.51 e Å^−3
0 restraints	Δρmin = −1.14 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Mo11	0.64581 (5)	0.36223 (4)	0.56566 (4)	0.02044 (16)
Mo12	0.62107 (5)	0.36345 (4)	0.43129 (4)	0.02111 (16)
O11	0.6331 (4)	0.4726 (3)	0.5737 (3)	0.0323 (13)
O12	0.6171 (4)	0.4735 (3)	0.4010 (3)	0.0326 (13)
O13	0.6479 (4)	0.2133 (3)	0.5969 (3)	0.0286 (12)
O14	0.6385 (4)	0.2169 (3)	0.4263 (3)	0.0303 (13)
O15	0.5452 (4)	0.3336 (4)	0.6866 (3)	0.0270 (12)
O16	0.7263 (4)	0.3420 (4)	0.3152 (3)	0.0303 (13)
O17	0.7556 (4)	0.3432 (3)	0.4662 (3)	0.0264 (13)
O18	0.5133 (4)	0.3401 (3)	0.5344 (3)	0.0248 (12)
O19	0.5773 (5)	0.1004 (4)	0.6888 (3)	0.0420 (15)
O110	0.4993 (4)	0.2306 (4)	0.7913 (3)	0.0314 (13)
O111	0.8072 (4)	0.2416 (4)	0.2322 (3)	0.0360 (14)
O112	0.7366 (5)	0.1077 (4)	0.3570 (3)	0.0424 (15)
O113	0.4832 (4)	0.3465 (4)	0.3871 (3)	0.0292 (13)
H11	0.4250	0.3543	0.4036	0.035*
H12	0.4967	0.3063	0.3503	0.035*
O114	0.7901 (4)	0.3414 (4)	0.6064 (3)	0.0345 (14)
H13	0.7813	0.3143	0.6528	0.041*
H14	0.8616	0.3587	0.5826	0.041*
C11	0.5930 (6)	0.1810 (5)	0.6644 (4)	0.0244 (16)
C12	0.5408 (6)	0.2523 (5)	0.7203 (4)	0.0234 (18)
C13	0.7066 (6)	0.1873 (5)	0.3646 (5)	0.0265 (17)
C14	0.7503 (6)	0.2631 (6)	0.2978 (4)	0.0262 (18)
Mo21	0.14510 (5)	0.36083 (4)	0.56520 (4)	0.01970 (16)
Mo22	0.12443 (5)	0.36243 (4)	0.42996 (4)	0.01974 (15)
O21	0.1350 (4)	0.4707 (3)	0.5722 (3)	0.0323 (13)
O22	0.1254 (4)	0.4732 (3)	0.3981 (3)	0.0310 (13)
O23	0.1598 (4)	0.2114 (3)	0.5974 (3)	0.0280 (12)
O24	0.1210 (4)	0.2174 (3)	0.4285 (3)	0.0243 (11)
O25	0.0402 (4)	0.3304 (3)	0.6839 (3)	0.0259 (12)
O26	0.2332 (4)	0.3312 (3)	0.3170 (3)	0.0267 (12)
O27	0.2572 (4)	0.3383 (3)	0.4661 (3)	0.0228 (11)
O28	0.0133 (4)	0.3417 (3)	0.5322 (3)	0.0239 (12)
O29	0.1169 (4)	0.1009 (3)	0.6968 (3)	0.0308 (12)
O210	−0.0008 (4)	0.2296 (3)	0.7911 (3)	0.0285 (13)
O211	0.1885 (5)	0.1015 (4)	0.3617 (3)	0.0377 (14)
O212	0.2996 (4)	0.2273 (4)	0.2365 (3)	0.0313 (13)
O213	−0.0155 (4)	0.3567 (3)	0.3815 (3)	0.0283 (13)
H21	−0.0805	0.3590	0.4030	0.034*
H22	−0.0024	0.3053	0.3520	0.034*
O214	0.2860 (4)	0.3475 (4)	0.6116 (3)	0.0336 (14)
H23	0.2754	0.3086	0.6554	0.040*
H24	0.3537	0.3611	0.5801	0.040*
C21	0.1121 (6)	0.1802 (5)	0.6688 (4)	0.0225 (16)
C22	0.0444 (6)	0.2523 (5)	0.7199 (5)	0.0243 (18)
C23	0.1815 (7)	0.1816 (5)	0.3688 (4)	0.0255 (17)
C24	0.2456 (6)	0.2511 (5)	0.3010 (5)	0.0267 (18)
Mo31	0.56900 (5)	0.35719 (4)	1.06688 (4)	0.02159 (16)
Mo32	0.72350 (5)	0.35992 (4)	0.93278 (4)	0.02157 (16)
O31	0.5482 (4)	0.4672 (4)	1.0751 (3)	0.0339 (14)
O32	0.7311 (4)	0.4701 (4)	0.9032 (3)	0.0324 (13)
O33	0.5617 (4)	0.2076 (3)	1.0972 (3)	0.0305 (13)
O34	0.7506 (4)	0.2128 (3)	0.9289 (3)	0.0301 (13)
O35	0.5601 (4)	0.3273 (4)	1.1871 (3)	0.0290 (13)
O36	0.7364 (4)	0.3353 (4)	0.8182 (3)	0.0309 (13)
O37	0.7358 (4)	0.3372 (3)	1.0357 (3)	0.0262 (12)
O38	0.5604 (4)	0.3386 (3)	0.9659 (3)	0.0253 (12)
O39	0.5393 (5)	0.0955 (4)	1.1947 (3)	0.0399 (14)
O310	0.5263 (5)	0.2252 (4)	1.2912 (3)	0.0319 (13)
O311	0.7741 (4)	0.2360 (4)	0.7324 (3)	0.0319 (13)
O312	0.7740 (5)	0.1029 (4)	0.8558 (3)	0.0431 (15)
O313	0.9104 (4)	0.3479 (4)	0.8863 (3)	0.0355 (14)
H31	0.9188	0.3317	0.9364	0.043*
H32	0.9432	0.4260	0.8593	0.043*
O314	0.3881 (4)	0.3384 (4)	1.1100 (3)	0.0360 (15)
H33	0.3299	0.3452	1.0939	0.043*
H34	0.3600	0.3103	1.1609	0.043*
C31	0.5488 (6)	0.1751 (5)	1.1692 (5)	0.0293 (19)
C32	0.5450 (6)	0.2486 (5)	1.2215 (4)	0.0231 (17)
C33	0.7610 (6)	0.1805 (6)	0.8647 (4)	0.0255 (18)
C34	0.7568 (6)	0.2554 (5)	0.7991 (5)	0.0247 (18)
Mo41	1.07590 (5)	0.36453 (4)	1.06078 (4)	0.02022 (15)
Mo42	1.23165 (5)	0.36446 (4)	0.92694 (4)	0.02041 (15)
O41	1.0559 (4)	0.4752 (3)	1.0669 (3)	0.0303 (13)
O42	1.2380 (4)	0.4752 (3)	0.8945 (3)	0.0292 (12)
O43	1.0781 (5)	0.2151 (3)	1.0911 (3)	0.0308 (13)
O44	1.2559 (4)	0.2168 (3)	0.9279 (3)	0.0271 (12)
O45	1.0650 (4)	0.3363 (3)	1.1824 (3)	0.0243 (12)
O46	1.2491 (4)	0.3355 (3)	0.8112 (3)	0.0274 (12)
O47	1.2435 (4)	0.3461 (3)	1.0308 (3)	0.0221 (11)
O48	1.0680 (4)	0.3424 (3)	0.9607 (3)	0.0250 (12)
O49	1.0795 (5)	0.1033 (4)	1.1872 (3)	0.0393 (14)
O410	1.0211 (4)	0.2347 (4)	1.2870 (3)	0.0295 (13)
O411	1.2459 (6)	0.1038 (4)	0.8631 (3)	0.0473 (16)
O412	1.2813 (5)	0.2295 (4)	0.7318 (3)	0.0364 (14)
O413	1.4165 (4)	0.3518 (4)	0.8844 (3)	0.0297 (13)
H41	1.4364	0.3203	0.8498	0.036*
H42	1.4406	0.3546	0.9183	0.036*
O414	0.8970 (5)	0.3430 (4)	1.1023 (3)	0.0352 (16)
H43	0.873	0.322	1.143	0.042*
H44	0.858	0.357	1.076	0.042*
C41	1.0711 (6)	0.1827 (5)	1.1602 (4)	0.0211 (15)
C42	1.0505 (6)	0.2566 (5)	1.2158 (4)	0.0258 (18)
C43	1.2545 (7)	0.1834 (6)	0.8691 (5)	0.032 (2)
C44	1.2616 (6)	0.2545 (5)	0.7968 (5)	0.0251 (19)
K1	0.9118 (2)	0.49703 (16)	0.75164 (13)	0.0592 (6)
K2	0.5704 (2)	0.49875 (16)	0.25073 (14)	0.0620 (7)
K3	0.03505 (14)	−0.05368 (12)	0.65508 (11)	0.0378 (4)
K4	0.70006 (18)	−0.03065 (14)	0.78047 (12)	0.0494 (5)
K5	0.34568 (17)	0.03380 (14)	0.71462 (12)	0.0476 (5)
K6	0.00855 (18)	0.05198 (14)	0.85836 (13)	0.0525 (5)
K7	0.6658 (2)	0.05955 (16)	0.52713 (15)	0.0827 (9)
K8	0.3486 (4)	−0.0496 (2)	0.9773 (3)	0.174 (2)
OW1	0.8501 (6)	−0.0525 (4)	0.4737 (3)	0.0540 (18)
H1A	0.8565	−0.0829	0.4150	0.081*
H1B	0.9026	−0.0881	0.5024	0.081*
OW2	1.1260 (7)	0.4977 (5)	0.7505 (5)	0.079 (2)
H2A	1.1828	0.4556	0.7292	0.119*
H2B	1.1635	0.5430	0.7691	0.119*
OW3	0.8688 (5)	0.0832 (4)	0.6621 (4)	0.0609 (19)
H3A	0.8176	0.1271	0.7070	0.091*
H3B	0.8393	0.0110	0.6459	0.091*
OW4	0.3562 (7)	0.4953 (6)	0.2460 (5)	0.089 (3)
H4A	0.3166	0.4492	0.2997	0.133*
H4B	0.4050	0.5575	0.2521	0.133*
OW5	−0.1130 (5)	0.1575 (4)	0.4920 (4)	0.0580 (19)
H5A	−0.1964	0.1844	0.4700	0.087*
H5B	−0.1358	0.1048	0.5542	0.087*
OW6	0.4100 (5)	0.1491 (5)	0.5552 (4)	0.0587 (18)
H6A	0.3345	0.1723	0.5700	0.088*
H6B	0.4590	0.2021	0.5594	0.088*
OW7	0.3686 (7)	0.1411 (5)	1.0538 (4)	0.072 (2)
H7A	0.4383	0.1451	0.9985	0.108*
H7B	0.2950	0.1673	1.0394	0.108*
OW8	0.1824 (6)	−0.0814 (5)	0.8307 (5)	0.090 (3)
H8A	0.1451	−0.1164	0.8759	0.135*
H8B	0.2243	−0.0216	0.8358	0.135*
OW9	0.5367 (7)	−0.0753 (5)	0.5983 (5)	0.095 (3)
H9A	0.5409	−0.1494	0.6109	0.142*
H9B	0.5406	−0.0420	0.6463	0.142*
OW10	0.5078 (7)	0.0664 (6)	0.8922 (7)	0.139 (5)
H10A	0.5319	0.1025	0.8452	0.209*
H10B	0.4173	0.0818	0.9246	0.209*
OW11	0.9308 (9)	0.1534 (6)	1.0016 (6)	0.116 (4)
H11A	0.9535	0.1236	1.0598	0.173*
H11B	0.9325	0.1059	0.9612	0.173*
OW12	−0.1459 (13)	−0.0442 (6)	0.9793 (6)	0.173 (6)
H12A	−0.1580	−0.0922	1.0260	0.259*
H12B	−0.0956	−0.0898	0.9249	0.259*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo11	0.0155 (3)	0.0225 (4)	0.0224 (4)	−0.0014 (3)	−0.0032 (3)	−0.0060 (3)
Mo12	0.0162 (3)	0.0240 (4)	0.0222 (4)	−0.0015 (3)	−0.0039 (3)	−0.0044 (3)
O11	0.032 (3)	0.034 (3)	0.034 (3)	0.000 (3)	−0.009 (2)	−0.017 (3)
O12	0.027 (3)	0.029 (3)	0.035 (3)	0.005 (2)	−0.004 (2)	−0.002 (3)
O13	0.029 (3)	0.027 (3)	0.024 (3)	0.002 (2)	0.001 (2)	−0.006 (2)
O14	0.033 (3)	0.028 (3)	0.029 (3)	−0.007 (2)	−0.004 (2)	−0.011 (2)
O15	0.023 (3)	0.030 (3)	0.025 (3)	0.001 (2)	−0.003 (2)	−0.010 (2)
O16	0.023 (3)	0.036 (3)	0.028 (3)	−0.002 (2)	0.000 (2)	−0.010 (3)
O17	0.017 (3)	0.034 (3)	0.025 (3)	−0.003 (2)	0.000 (2)	−0.006 (2)
O18	0.011 (2)	0.028 (3)	0.035 (3)	−0.003 (2)	−0.005 (2)	−0.007 (2)
O19	0.047 (4)	0.026 (3)	0.048 (4)	−0.006 (3)	−0.008 (3)	0.000 (3)
O110	0.027 (3)	0.040 (3)	0.026 (3)	−0.002 (3)	−0.005 (2)	−0.006 (3)
O111	0.034 (3)	0.045 (4)	0.026 (3)	0.000 (3)	−0.003 (2)	−0.011 (3)
O112	0.040 (3)	0.029 (3)	0.052 (4)	0.007 (3)	−0.006 (3)	−0.013 (3)
O113	0.015 (2)	0.046 (3)	0.033 (3)	0.003 (2)	−0.011 (2)	−0.020 (3)
O114	0.020 (3)	0.056 (4)	0.028 (3)	−0.008 (3)	−0.011 (2)	0.005 (3)
C11	0.023 (4)	0.027 (4)	0.024 (4)	−0.006 (3)	−0.005 (3)	−0.007 (3)
C12	0.017 (4)	0.036 (5)	0.015 (4)	−0.008 (3)	0.002 (3)	−0.006 (4)
C13	0.016 (3)	0.030 (4)	0.032 (4)	0.002 (3)	−0.004 (3)	−0.010 (3)
C14	0.013 (3)	0.042 (5)	0.023 (4)	0.003 (3)	−0.002 (3)	−0.013 (4)
Mo21	0.0163 (3)	0.0218 (4)	0.0202 (3)	−0.0012 (3)	−0.0034 (3)	−0.0055 (3)
Mo22	0.0177 (3)	0.0208 (4)	0.0199 (3)	−0.0019 (3)	−0.0037 (3)	−0.0048 (3)
O21	0.032 (3)	0.028 (3)	0.035 (3)	0.000 (2)	−0.007 (2)	−0.008 (3)
O22	0.034 (3)	0.025 (3)	0.036 (3)	−0.006 (2)	−0.012 (2)	−0.001 (2)
O23	0.037 (3)	0.026 (3)	0.021 (3)	−0.001 (2)	−0.008 (2)	−0.004 (2)
O24	0.025 (3)	0.023 (3)	0.020 (3)	−0.003 (2)	0.000 (2)	−0.003 (2)
O25	0.030 (3)	0.022 (3)	0.022 (3)	0.001 (2)	−0.003 (2)	−0.007 (2)
O26	0.029 (3)	0.024 (3)	0.026 (3)	−0.007 (2)	−0.004 (2)	−0.005 (2)
O27	0.014 (2)	0.029 (3)	0.026 (3)	0.001 (2)	−0.004 (2)	−0.009 (2)
O28	0.017 (3)	0.031 (3)	0.026 (3)	0.001 (2)	−0.008 (2)	−0.010 (2)
O29	0.034 (3)	0.024 (3)	0.034 (3)	−0.001 (2)	−0.010 (2)	−0.001 (2)
O210	0.031 (3)	0.031 (3)	0.018 (3)	0.001 (2)	−0.001 (2)	−0.004 (2)
O211	0.050 (4)	0.025 (3)	0.035 (3)	0.000 (3)	−0.008 (3)	−0.010 (2)
O212	0.028 (3)	0.036 (3)	0.026 (3)	−0.002 (2)	−0.003 (2)	−0.005 (3)
O213	0.023 (3)	0.026 (3)	0.035 (3)	0.005 (2)	−0.006 (2)	−0.010 (2)
O214	0.016 (3)	0.045 (3)	0.039 (3)	−0.007 (2)	−0.010 (2)	0.002 (3)
C21	0.022 (3)	0.023 (4)	0.024 (4)	0.000 (3)	−0.009 (3)	−0.004 (3)
C22	0.020 (4)	0.022 (4)	0.034 (5)	0.005 (3)	−0.010 (3)	−0.011 (4)
C23	0.029 (4)	0.027 (4)	0.021 (4)	−0.004 (3)	−0.012 (3)	0.004 (3)
C24	0.022 (4)	0.031 (4)	0.027 (4)	0.003 (3)	−0.009 (3)	−0.006 (4)
Mo31	0.0188 (3)	0.0269 (4)	0.0212 (4)	−0.0019 (3)	−0.0083 (3)	−0.0045 (3)
Mo32	0.0188 (3)	0.0265 (4)	0.0215 (4)	−0.0003 (3)	−0.0077 (3)	−0.0068 (3)
O31	0.034 (3)	0.030 (3)	0.037 (3)	0.001 (3)	−0.010 (3)	−0.007 (3)
O32	0.029 (3)	0.036 (3)	0.029 (3)	−0.005 (2)	−0.006 (2)	0.000 (3)
O33	0.033 (3)	0.026 (3)	0.032 (3)	−0.002 (2)	−0.009 (2)	−0.007 (2)
O34	0.032 (3)	0.027 (3)	0.031 (3)	0.005 (2)	−0.014 (3)	0.001 (3)
O35	0.037 (3)	0.030 (3)	0.023 (3)	−0.002 (2)	−0.009 (2)	−0.010 (2)
O36	0.028 (3)	0.036 (3)	0.027 (3)	0.003 (2)	−0.010 (2)	0.003 (3)
O37	0.020 (3)	0.035 (3)	0.023 (3)	0.001 (2)	−0.006 (2)	−0.007 (2)
O38	0.023 (3)	0.037 (3)	0.021 (3)	−0.001 (2)	−0.011 (2)	−0.009 (2)
O39	0.051 (4)	0.030 (3)	0.042 (3)	−0.003 (3)	−0.019 (3)	−0.003 (3)
O310	0.043 (3)	0.035 (3)	0.020 (3)	−0.005 (3)	−0.012 (2)	−0.004 (2)
O311	0.038 (3)	0.043 (3)	0.020 (3)	0.009 (3)	−0.012 (2)	−0.020 (3)
O312	0.053 (4)	0.024 (3)	0.048 (4)	−0.003 (3)	−0.009 (3)	−0.008 (3)
O313	0.027 (3)	0.043 (4)	0.036 (3)	−0.003 (3)	−0.008 (3)	−0.008 (3)
O314	0.017 (3)	0.061 (4)	0.028 (3)	−0.007 (3)	−0.009 (2)	0.006 (3)
C31	0.023 (4)	0.025 (4)	0.035 (5)	−0.005 (3)	−0.001 (3)	−0.002 (4)
C32	0.015 (3)	0.032 (4)	0.027 (4)	0.003 (3)	−0.010 (3)	−0.010 (4)
C33	0.020 (4)	0.034 (5)	0.024 (4)	−0.008 (3)	−0.005 (3)	−0.006 (4)
C34	0.021 (4)	0.029 (5)	0.028 (5)	0.011 (3)	−0.014 (3)	−0.009 (4)
Mo41	0.0192 (3)	0.0233 (4)	0.0203 (3)	0.0006 (3)	−0.0087 (3)	−0.0046 (3)
Mo42	0.0196 (3)	0.0232 (4)	0.0200 (3)	−0.0002 (3)	−0.0081 (3)	−0.0041 (3)
O41	0.027 (3)	0.028 (3)	0.039 (3)	0.005 (2)	−0.013 (2)	−0.011 (3)
O42	0.035 (3)	0.019 (3)	0.037 (3)	−0.004 (2)	−0.014 (2)	−0.003 (2)
O43	0.050 (3)	0.024 (3)	0.022 (3)	−0.004 (2)	−0.014 (2)	−0.007 (2)
O44	0.035 (3)	0.022 (3)	0.026 (3)	0.003 (2)	−0.012 (2)	−0.007 (2)
O45	0.030 (3)	0.023 (3)	0.024 (3)	−0.001 (2)	−0.014 (2)	−0.004 (2)
O46	0.041 (3)	0.025 (3)	0.017 (3)	−0.004 (2)	−0.009 (2)	−0.006 (2)
O47	0.020 (2)	0.034 (3)	0.017 (3)	0.001 (2)	−0.008 (2)	−0.010 (2)
O48	0.020 (3)	0.033 (3)	0.027 (3)	0.002 (2)	−0.014 (2)	−0.007 (2)
O49	0.055 (4)	0.027 (3)	0.038 (3)	0.003 (3)	−0.019 (3)	−0.002 (3)
O410	0.033 (3)	0.036 (3)	0.022 (3)	−0.003 (2)	−0.011 (2)	−0.006 (2)
O411	0.077 (5)	0.028 (3)	0.040 (4)	−0.011 (3)	−0.020 (3)	−0.006 (3)
O412	0.042 (3)	0.046 (4)	0.027 (3)	−0.006 (3)	−0.015 (3)	−0.011 (3)
O413	0.019 (3)	0.048 (3)	0.031 (3)	0.001 (2)	−0.011 (2)	−0.026 (3)
O414	0.021 (3)	0.058 (4)	0.028 (3)	−0.005 (3)	−0.013 (2)	0.006 (3)
C41	0.018 (3)	0.029 (4)	0.015 (3)	0.003 (3)	−0.003 (3)	−0.010 (3)
C42	0.027 (4)	0.029 (4)	0.020 (4)	−0.001 (3)	−0.005 (3)	−0.003 (3)
C43	0.031 (4)	0.029 (5)	0.030 (5)	0.001 (4)	0.000 (4)	−0.010 (4)
C44	0.016 (4)	0.034 (5)	0.028 (5)	−0.007 (3)	−0.008 (3)	−0.008 (4)
K1	0.0679 (15)	0.0556 (15)	0.0459 (13)	−0.0074 (12)	−0.0130 (11)	0.0115 (11)
K2	0.0819 (17)	0.0491 (14)	0.0478 (13)	−0.0064 (12)	−0.0144 (12)	0.0047 (11)
K3	0.0321 (9)	0.0302 (9)	0.0449 (11)	−0.0019 (7)	−0.0060 (8)	0.0014 (8)
K4	0.0546 (12)	0.0398 (11)	0.0539 (13)	0.0022 (9)	−0.0149 (10)	−0.0140 (10)
K5	0.0437 (11)	0.0440 (12)	0.0543 (13)	−0.0025 (9)	−0.0135 (9)	−0.0075 (10)
K6	0.0489 (12)	0.0412 (11)	0.0569 (14)	0.0016 (9)	−0.0072 (10)	0.0026 (10)
K7	0.101 (2)	0.0383 (13)	0.0671 (16)	−0.0098 (13)	0.0332 (14)	−0.0096 (12)
K8	0.157 (3)	0.060 (2)	0.193 (4)	−0.019 (2)	0.102 (3)	−0.013 (2)
OW1	0.092 (5)	0.032 (4)	0.035 (4)	0.007 (3)	−0.023 (3)	0.005 (3)
OW2	0.084 (6)	0.056 (5)	0.107 (6)	0.001 (4)	−0.041 (5)	−0.015 (4)
OW3	0.054 (4)	0.048 (4)	0.089 (5)	0.009 (3)	−0.026 (4)	−0.031 (4)
OW4	0.095 (6)	0.072 (6)	0.089 (6)	−0.018 (5)	−0.029 (5)	0.029 (5)
OW5	0.038 (3)	0.043 (4)	0.090 (5)	−0.001 (3)	−0.010 (3)	−0.025 (4)
OW6	0.045 (4)	0.063 (5)	0.059 (5)	0.004 (3)	−0.003 (3)	−0.017 (4)
OW7	0.086 (6)	0.063 (5)	0.083 (6)	0.000 (4)	−0.047 (5)	−0.010 (4)
OW8	0.054 (5)	0.054 (5)	0.165 (9)	−0.007 (4)	−0.021 (5)	−0.052 (5)
OW9	0.082 (6)	0.060 (5)	0.133 (8)	−0.032 (5)	−0.026 (5)	0.018 (5)
OW10	0.058 (5)	0.094 (7)	0.213 (11)	−0.008 (5)	−0.019 (6)	0.098 (7)
OW11	0.172 (10)	0.075 (6)	0.137 (9)	0.022 (6)	−0.101 (8)	−0.027 (6)
OW12	0.313 (17)	0.059 (7)	0.096 (8)	−0.066 (9)	0.016 (9)	−0.007 (6)

Geometric parameters (Å, º)

Mo11—O11	1.679 (5)	O33—C31	1.301 (9)
Mo11—O17	1.922 (5)	O34—C33	1.298 (9)
Mo11—O18	1.958 (4)	O35—C32	1.259 (9)
Mo11—O114	2.117 (5)	O36—C34	1.282 (9)
Mo11—O15	2.155 (5)	O39—C31	1.225 (9)
Mo11—O13	2.235 (5)	O310—C32	1.223 (8)
Mo11—Mo12	2.5686 (10)	O311—C34	1.241 (8)
Mo12—O12	1.674 (5)	O312—C33	1.192 (9)
Mo12—O18	1.924 (5)	O313—H31	0.951
Mo12—O17	1.941 (5)	O313—H32	1.255
Mo12—O113	2.145 (4)	O314—H33	0.850
Mo12—O16	2.148 (5)	O314—H34	0.932
Mo12—O14	2.212 (5)	C31—C32	1.551 (10)
O13—C11	1.248 (8)	C33—C34	1.537 (10)
O14—C13	1.278 (8)	Mo41—O41	1.678 (5)
O15—C12	1.286 (9)	Mo41—O48	1.939 (5)
O16—C14	1.259 (9)	Mo41—O47	1.953 (5)
O19—C11	1.241 (9)	Mo41—O414	2.115 (5)
O110—C12	1.237 (8)	Mo41—O45	2.166 (5)
O111—C14	1.248 (8)	Mo41—O43	2.241 (5)
O112—C13	1.236 (9)	Mo41—Mo42	2.5695 (10)
O113—H11	0.686	Mo42—O42	1.688 (5)
O113—H12	0.935	Mo42—O47	1.930 (4)
O114—H13	0.864	Mo42—O48	1.943 (4)
O114—H14	0.886	Mo42—O413	2.146 (5)
C11—C12	1.541 (10)	Mo42—O46	2.160 (5)
C13—O112	1.236 (9)	Mo42—O44	2.217 (5)
C13—C14	1.539 (10)	O43—C41	1.266 (8)
Mo21—O21	1.669 (5)	O44—C43	1.254 (9)
Mo21—O27	1.940 (5)	O45—C42	1.266 (8)
Mo21—O28	1.955 (4)	O46—C44	1.271 (9)
Mo21—O25	2.140 (5)	O49—C41	1.236 (8)
Mo21—O214	2.142 (5)	O410—C42	1.236 (8)
Mo21—O23	2.250 (5)	O411—C43	1.235 (9)
Mo21—Mo22	2.5627 (9)	O412—C44	1.240 (8)
Mo22—O22	1.686 (5)	O413—H41	0.806
Mo22—O28	1.924 (5)	O413—H42	0.775
Mo22—O27	1.936 (4)	O414—H43	0.75
Mo22—O26	2.155 (5)	O414—H44	0.78
Mo22—O213	2.185 (5)	C41—C42	1.562 (10)
Mo22—O24	2.192 (5)	C42—O410	1.236 (8)
O23—C21	1.282 (8)	C43—C44	1.563 (11)
O24—C23	1.267 (9)	C44—C43	1.563 (11)
O25—C22	1.270 (8)	OW1—H1A	1.203
O26—C24	1.266 (9)	OW1—H1B	1.028
O29—C21	1.235 (8)	OW2—H2A	0.925
O210—C22	1.247 (8)	OW2—H2B	1.008
O211—C23	1.225 (9)	OW3—H3A	1.120
O212—C24	1.237 (9)	OW3—H3B	1.277
O213—H21	0.766	OW4—H4A	1.112
O213—H22	0.979	OW4—H4B	1.193
O214—H23	0.902	OW5—H5A	1.233
O214—H24	0.866	OW5—H5B	1.256
C21—C22	1.540 (10)	OW6—H6A	0.928
C23—C24	1.546 (10)	OW6—H6B	1.066
Mo31—O31	1.675 (5)	OW7—H7A	1.090
Mo31—O38	1.944 (5)	OW7—H7B	1.050
Mo31—O37	1.946 (5)	OW8—H8A	0.918
Mo31—O314	2.129 (5)	OW8—H8B	1.105
Mo31—O35	2.149 (5)	OW9—H9A	1.107
Mo31—O33	2.245 (5)	OW9—H9B	1.087
Mo31—Mo32	2.5635 (10)	OW10—H10A	0.923
Mo32—O32	1.672 (5)	OW10—H10B	1.097
Mo32—O37	1.916 (5)	OW11—H11A	1.202
Mo32—O38	1.935 (5)	OW11—H11B	1.094
Mo32—O36	2.132 (5)	OW12—H12A	1.017
Mo32—O313	2.172 (5)	OW12—H12B	1.250
Mo32—O34	2.220 (5)
K1···OW2	2.622 (8)	K4···O19	3.025 (7)
K1···O22^i	2.887 (6)	K4···O312	2.947 (7)
K1···O45^ii	3.008 (6)	K5···OW8	2.885 (8)
K1···O25	3.040 (6)	K5···O411	2.901 (6)
K1···O213^i	3.057 (5)	K5···O39^v	2.941 (6)
K1···OW4^i	3.265 (9)	K5···OW6	3.072 (7)
K1···O26^i	3.341 (6)	K5···OW9	3.131 (9)
K1···O32	2.933 (5)	K5···O19	2.966 (7)
K1···O36	3.227 (6)	K5···O112	3.050 (7)
K1···O313	3.083 (6)	K5···O29	3.002 (6)
K2···OW4	2.663 (9)	K5···O412	3.018 (6)
K2···O42^iii	2.923 (6)	K6···OW12	2.724 (10)
K2···O15^i	2.975 (6)	K6···OW8	2.772 (8)
K2···O35^iv	3.008 (6)	K6···O312	2.926 (7)
K2···O413^iii	3.069 (6)	K6···O49^v	2.986 (6)
K2···O46^i	3.309 (5)	K6···OW11	3.060 (10)
K2···O31^iv	3.412 (6)	K6···O411	3.111 (7)
K2···O11^i	3.424 (6)	K6···O29	2.834 (5)
K2···O12	2.951 (7)	K6···O210	2.789 (5)
K2···O16	3.242 (6)	K7···OW9	2.607 (7)
K2···O113	3.112 (5)	K7···OW1	2.699 (7)
K3···OW1	2.693 (6)	K7···O112	2.945 (6)
K3···OW3	2.757 (7)	K7···OW5	3.042 (7)
K3···O49^v	2.790 (6)	K7···OW6	3.216 (7)
K3···O410^vi	2.839 (6)	K7···O13	2.758 (6)
K3···O211^vi	3.015 (6)	K7···O14	2.854 (6)
K3···OW5^vi	3.140 (7)	K7···O19	2.935 (7)
K3···O112	2.795 (6)	K8···OW10	2.671 (8)
K3···029	2.901 (6)	K8···OW12^viii	2.690 (16)
K4···O211	2.826 (6)	K8···O33^v	2.866 (6)
K4···OW3	2.927 (7)	K8···O34^v	2.902 (6)
K4···OW10	2.998 (11)	K8···O312^v	2.958 (7)
K4···O212	3.021 (6)	K8···O39^v	3.147 (7)
K4···O49^vii	3.033 (6)	K8···O411	3.334 (8)
K4···O39^v	3.049 (6)	K8···OW10^v	3.368 (13)
K4···OW7^v	3.132 (8)	K8···OW7	3.429 (8)
O11—Mo11—O17	108.7 (2)	O31—Mo31—O35	91.2 (2)
O11—Mo11—O18	104.2 (2)	O38—Mo31—O35	158.8 (2)
O17—Mo11—O18	93.6 (2)	O37—Mo31—O35	89.9 (2)
O11—Mo11—O114	93.4 (2)	O314—Mo31—O35	84.5 (2)
O17—Mo11—O114	84.8 (2)	O31—Mo31—O33	161.2 (2)
O18—Mo11—O114	161.9 (2)	O38—Mo31—O33	86.8 (2)
O11—Mo11—O15	90.5 (2)	O37—Mo31—O33	85.8 (2)
O17—Mo11—O15	158.7 (2)	O314—Mo31—O33	77.8 (2)
O18—Mo11—O15	90.31 (19)	O35—Mo31—O33	72.6 (2)
O114—Mo11—O15	85.05 (19)	O32—Mo32—O37	109.2 (2)
O11—Mo11—O13	161.3 (2)	O32—Mo32—O38	104.3 (2)
O17—Mo11—O13	87.8 (2)	O37—Mo32—O38	94.8 (2)
O18—Mo11—O13	82.8 (2)	O32—Mo32—O36	90.1 (2)
O114—Mo11—O13	79.1 (2)	O37—Mo32—O36	158.6 (2)
O15—Mo11—O13	71.98 (19)	O38—Mo32—O36	89.27 (19)
O12—Mo12—O18	109.4 (2)	O32—Mo32—O313	88.6 (2)
O12—Mo12—O17	104.9 (2)	O37—Mo32—O313	88.8 (2)
O18—Mo12—O17	94.07 (19)	O38—Mo32—O313	164.6 (2)
O12—Mo12—O113	89.8 (2)	O36—Mo32—O313	82.2 (2)
O18—Mo12—O113	87.68 (19)	O32—Mo32—O34	159.9 (2)
O17—Mo12—O113	163.6 (2)	O37—Mo32—O34	86.7 (2)
O12—Mo12—O16	88.6 (2)	O38—Mo32—O34	85.9 (2)
O18—Mo12—O16	159.7 (2)	O36—Mo32—O34	72.6 (2)
O17—Mo12—O16	90.16 (19)	O313—Mo32—O34	79.2 (2)
O113—Mo12—O16	82.86 (18)	C31—O33—Mo31	117.6 (5)
O12—Mo12—O14	159.4 (2)	C33—O34—Mo32	119.3 (5)
O18—Mo12—O14	88.0 (2)	C32—O35—Mo31	121.0 (5)
O17—Mo12—O14	84.1 (2)	C34—O36—Mo32	120.4 (5)
O113—Mo12—O14	79.7 (2)	Mo32—O37—Mo31	83.17 (19)
O16—Mo12—O14	72.7 (2)	Mo32—O38—Mo31	82.73 (18)
C11—O13—Mo11	119.2 (5)	Mo32—O313—H31	93.1
C13—O14—Mo12	118.6 (5)	Mo32—O313—H32	106.0
C12—O15—Mo11	119.9 (5)	H31—O313—H32	110.7
C14—O16—Mo12	119.6 (5)	Mo31—O314—H33	139.4
Mo11—O17—Mo12	83.36 (18)	Mo31—O314—H34	115.9
Mo12—O18—Mo11	82.86 (16)	H33—O314—H34	104.5
Mo12—O113—H11	129.2	O39—C31—O33	124.8 (8)
Mo12—O113—H12	117.5	O39—C31—C32	122.3 (8)
H11—O113—H12	109.8	O33—C31—C32	112.9 (7)
Mo11—O114—H13	119.0	O310—C32—O35	126.8 (7)
Mo11—O114—H14	128.6	O310—C32—C31	117.6 (7)
H13—O114—H14	112.3	O35—C32—C31	115.6 (7)
O19—C11—O13	126.9 (8)	O312—C33—O34	125.6 (8)
O19—C11—C12	119.4 (7)	O312—C33—C34	122.9 (7)
O13—C11—C12	113.7 (6)	O34—C33—C34	111.5 (7)
O110—C12—O15	124.7 (7)	O311—C34—O36	124.7 (7)
O110—C12—C11	121.0 (7)	O311—C34—C33	119.3 (7)
O15—C12—C11	114.3 (6)	O36—C34—C33	116.0 (7)
O112—C13—O14	125.9 (7)	O41—Mo41—O48	108.6 (2)
O112—C13—C14	121.9 (7)	O41—Mo41—O47	103.1 (2)
O14—C13—C14	112.2 (7)	O48—Mo41—O47	94.05 (19)
O111—C14—O16	125.9 (7)	O41—Mo41—O414	93.1 (2)
O111—C14—C13	117.9 (7)	O48—Mo41—O414	85.4 (2)
O16—C14—C13	116.2 (7)	O47—Mo41—O414	163.0 (2)
O21—Mo21—O27	109.2 (2)	O41—Mo41—O45	91.6 (2)
O21—Mo21—O28	103.7 (2)	O48—Mo41—O45	157.9 (2)
O27—Mo21—O28	93.54 (19)	O47—Mo41—O45	89.93 (18)
O21—Mo21—O25	92.2 (2)	O414—Mo41—O45	84.5 (2)
O27—Mo21—O25	157.0 (2)	O41—Mo41—O43	162.9 (2)
O28—Mo21—O25	89.11 (19)	O48—Mo41—O43	86.3 (2)
O21—Mo21—O214	89.2 (2)	O47—Mo41—O43	83.5 (2)
O27—Mo21—O214	87.17 (19)	O414—Mo41—O43	79.5 (2)
O28—Mo21—O214	165.9 (2)	O45—Mo41—O43	72.47 (18)
O25—Mo21—O214	84.91 (19)	O42—Mo42—O47	109.0 (2)
O21—Mo21—O23	160.4 (2)	O42—Mo42—O48	104.0 (2)
O27—Mo21—O23	85.06 (19)	O47—Mo42—O48	94.65 (19)
O28—Mo21—O23	88.2 (2)	O42—Mo42—O413	89.6 (2)
O25—Mo21—O23	72.22 (19)	O47—Mo42—O413	87.38 (19)
O214—Mo21—O23	77.87 (19)	O48—Mo42—O413	164.6 (2)
O22—Mo22—O28	109.6 (2)	O42—Mo42—O46	89.8 (2)
O22—Mo22—O27	105.1 (2)	O47—Mo42—O46	158.5 (2)
O28—Mo22—O27	94.65 (19)	O48—Mo42—O46	90.5 (2)
O22—Mo22—O26	91.4 (2)	O413—Mo42—O46	82.36 (19)
O28—Mo22—O26	157.2 (2)	O42—Mo42—O44	160.8 (2)
O27—Mo22—O26	88.24 (19)	O47—Mo42—O44	86.8 (2)
O22—Mo22—O213	86.6 (2)	O48—Mo42—O44	84.9 (2)
O28—Mo22—O213	88.17 (19)	O413—Mo42—O44	80.0 (2)
O27—Mo22—O213	166.15 (19)	O46—Mo42—O44	72.87 (19)
O26—Mo22—O213	84.03 (18)	C41—O43—Mo41	118.7 (5)
O22—Mo22—O24	159.2 (2)	C43—O44—Mo42	118.4 (5)
O28—Mo22—O24	85.15 (19)	C42—O45—Mo41	119.2 (5)
O27—Mo22—O24	87.68 (19)	C44—O46—Mo42	119.6 (5)
O26—Mo22—O24	72.32 (18)	Mo42—O47—Mo41	82.84 (17)
O213—Mo22—O24	79.04 (19)	Mo41—O48—Mo42	82.89 (17)
C21—O23—Mo21	117.6 (5)	Mo42—O413—H41	109.6
C23—O24—Mo22	119.9 (4)	Mo42—O413—H42	109.1
C22—O25—Mo21	120.7 (5)	H41—O413—H42	130.8
C24—O26—Mo22	120.2 (5)	Mo41—O414—H43	117
Mo22—O27—Mo21	82.78 (17)	Mo41—O414—H44	122
Mo22—O28—Mo21	82.68 (17)	H43—O414—H44	122
Mo22—O213—H21	127.6	O49—C41—O43	128.9 (7)
Mo22—O213—H22	110.3	O49—C41—C42	118.4 (6)
H21—O213—H22	105.3	O43—C41—C42	112.7 (6)
Mo21—O214—H23	114.7	O410—C42—O45	125.0 (8)
Mo21—O214—H24	118.0	O410—C42—C41	119.6 (7)
H23—O214—H24	122.7	O45—C42—C41	115.4 (6)
O29—C21—O23	125.8 (7)	O411—C43—O44	128.2 (8)
O29—C21—C22	120.8 (7)	O411—C43—C44	118.3 (8)
O23—C21—C22	113.3 (6)	O44—C43—C44	113.5 (7)
O210—C22—O25	126.4 (7)	O412—C44—O46	125.7 (7)
O210—C22—C21	118.4 (7)	O412—C44—C43	119.8 (7)
O25—C22—C21	115.2 (7)	O46—C44—C43	114.5 (7)
O211—C23—O24	125.9 (7)	H1A—OW1—H1B	111.8
O211—C23—C24	121.3 (7)	H2A—OW2—H2B	107.4
O24—C23—C24	112.8 (7)	H3A—OW3—H3B	128.3
O212—C24—O26	125.1 (7)	H4A—OW4—H4B	117.5
O212—C24—C23	120.2 (7)	H5A—OW5—H5B	115.3
O26—C24—C23	114.7 (7)	H6A—OW6—H6B	104.0
O31—Mo31—O38	108.2 (2)	H7A—OW7—H7B	104.9
O31—Mo31—O37	104.2 (2)	H8A—OW8—H8B	117.5
O38—Mo31—O37	93.5 (2)	H9A—OW9—H9B	112.6
O31—Mo31—O314	91.5 (2)	H10A—OW10—H10B	111.7
O38—Mo31—O314	86.4 (2)	H11A—OW11—H11B	117.1
O37—Mo31—O314	163.5 (2)	H12A—OW12—H12B	100.7

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+2, −y+1, −z+2; (iii) −x+2, −y+1, −z+1; (iv) x, y, z−1; (v) −x+1, −y, −z+2; (vi) −x, −y, −z+1; (vii) −x+2, −y, −z+2; (viii) −x, −y, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O113—H11···O27	0.686	2.021	2.683 (6)	162.7
O113—H12···O310^iv	0.935	1.684	2.615 (7)	173.4
O114—H13···O311	0.864	1.722	2.566 (7)	165.0
O114—H14···O28^ix	0.886	1.803	2.632 (7)	154.8
O213—H21···O17^x	0.766	1.982	2.740 (6)	170.1
O213—H22···O410^xi	0.979	1.646	2.612 (7)	168.2
O214—H23···O412^x	0.902	1.718	2.610 (8)	169.7
O214—H24···O18	0.866	1.880	2.686 (6)	154.2
O313—H31···O48	0.951	2.043	2.692 (7)	124.0
O313—H31···O37	0.951	2.388	2.865 (7)	110.6
O313—H32···O41^ii	1.255	2.149	3.012 (8)	122.2
O314—H33···O47^x	0.850	1.801	2.616 (7)	160.1
O314—H34···O212^xii	0.932	1.740	2.630 (7)	158.4
O413—H41···O110^ix	0.806	1.806	2.589 (7)	163.6
O413—H42···O38^ix	0.775	1.919	2.633 (6)	152.9
O414—H43···O111^xii	0.75	1.87	2.598 (8)	163
O414—H44···O37	0.78	1.93	2.650 (7)	153
OW1—H1A···O23^xiii	1.203	2.016	2.912 (8)	127.7
OW1—H1A···O29^xiii	1.203	2.017	3.192 (8)	164.5
OW1—H1B···O24^xiii	1.028	2.152	2.913 (7)	129.2
OW1—H1B···O211^xiii	1.028	2.358	2.886 (8)	110.7
OW2—H2A···O46	0.925	2.438	3.025 (10)	121.4
OW2—H2B···O16^iii	1.008	2.345	3.013 (9)	122.9
OW3—H3A···O311	1.120	1.758	2.775 (8)	148.5
OW3—H3B···O211^xiii	1.277	1.790	3.050 (8)	167.8
OW4—H4A···O26	1.112	2.062	2.921 (9)	131.6
OW4—H4A···O22	1.112	2.483	3.263 (10)	126.0
OW4—H4B···O15^i	1.193	2.338	3.472 (10)	157.8
OW5—H5A···O17^x	1.233	2.409	3.158 (8)	116.4
OW5—H5B···OW3^x	1.256	1.971	3.094 (10)	146.1
OW6—H6A···O23	0.928	2.088	3.011 (8)	173.0
OW6—H6B···O18	1.066	2.179	3.168 (8)	153.5
OW7—H7A···OW10	1.090	2.306	3.201 (15)	138.2
OW7—H7B···O44^x	1.050	2.255	3.092 (8)	135.4
OW8—H8A···OW11^v	0.918	2.139	3.009 (14)	158.0
OW8—H8B···O411^x	1.105	2.081	3.145 (9)	160.8
OW9—H9A···O310^v	1.107	1.952	2.786 (9)	129.2
OW9—H9B···O19	1.087	2.506	3.465 (11)	146.6
OW10—H10A···O110	0.923	2.105	2.883 (9)	141.2
OW10—H10B···OW7	1.097	2.515	3.201 (15)	119.5
OW11—H11A···OW8^v	1.202	2.202	3.009 (14)	121.5
OW11—H11A···O43	1.202	2.392	3.074 (10)	113.4
OW11—H11B···OW12^ix	1.094	2.471	3.316 (13)	133.1
OW12—H12A···O411^v	1.017	1.953	2.788 (12)	137.3
OW12—H12A···O44^v	1.017	2.227	3.054 (10)	137.4
OW12—H12B···O43^v	1.250	1.933	2.975 (11)	137.2
OW12—H12B···O49^v	1.250	2.033	3.124 (12)	143.1

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+2, −y+1, −z+2; (iii) −x+2, −y+1, −z+1; (iv) x, y, z−1; (v) −x+1, −y, −z+2; (ix) x+1, y, z; (x) x−1, y, z; (xi) x−1, y, z−1; (xii) x, y, z+1; (xiii) −x+1, −y, −z+1.