Bis[bis(12-crown-4)­potassium] hexa­iodo­tetra­cuprate(I)

From 12-crown-4, KI, and CuI in an acetone solution, the title compound, [K(C₁₆H₃₂O₈)₂]₂[Cu₄I₆], was obtained. It consists of sandwich-type [(12-crown-4)₂K]⁺ complex cations and polymeric [Cu₄I₆]^2- anions. The latter consist of CuI₄ tetrahedra, which share edges and faces to form infinite chains.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.027
• wR factor = 0.061
• Data-to-parameter ratio = 22.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) .....         10 Ang.
PLAT142_ALERT_4_C su on b - Axis Small or Missing (x 100000) .....         10 Ang.
PLAT145_ALERT_4_C su on beta     Small or Missing  (x 10000) .....          4 Deg.
PLAT146_ALERT_4_C su on gamma    Small or Missing  (x 10000) .....          4 Deg.
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        Cu3
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....         I5
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....         I6
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.64
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.23 Ratio

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: Nonius KappaCCD; cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: maXus (Mackay et al., 1997).

(I)

Crystal data

[K(C16H32O8)2]2[Cu4I6]	Z = 2
Mr = 1798.63	F(000) = 1712
Triclinic, P1	Dx = 2.210 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 14.5859 (1) Å	Cell parameters from 34261 reflections
b = 14.6371 (1) Å	θ = 4.1–27.5°
c = 15.6526 (2) Å	µ = 5.19 mm^−1
α = 67.4428 (5)°	T = 150 K
β = 69.0664 (4)°	Irregular, colourless
γ = 64.1181 (4)°	0.30 × 0.15 × 0.10 mm
V = 2703.11 (4) Å^3

Data collection

Nonius KappaCCD diffractometer	10176 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.034
φ and ω scans	θmax = 27.5°, θmin = 4.1°
Absorption correction: numerical (HABITUS; Herrendorf & Bärnighausen, 1997).	h = −18→18
Tmin = 0.463, Tmax = 0.745	k = −19→19
62318 measured reflections	l = −20→20
12337 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.027	H-atom parameters constrained
wR(F^2) = 0.061	w = 1/[σ^2(Fo^2) + (0.0183P)^2 + 5.5412P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.002
12337 reflections	Δρmax = 1.88 e Å^−3
541 parameters	Δρmin = −1.68 e Å^−3
0 restraints

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	Uiso*/Ueq
Cu1	0.47688 (4)	0.98223 (3)	0.09234 (3)	0.03212 (11)
Cu2	0.56173 (4)	0.79882 (3)	0.18644 (4)	0.03470 (12)
Cu3	0.43845 (4)	0.69282 (3)	0.30817 (4)	0.03554 (12)
Cu4	0.47587 (4)	0.48584 (3)	0.59160 (3)	0.03046 (11)
I1	0.388113 (17)	0.674660 (15)	0.500264 (14)	0.01976 (5)
I2	0.409845 (17)	0.529752 (16)	0.302763 (15)	0.02082 (5)
I3	0.587750 (17)	0.956789 (16)	0.204946 (15)	0.02238 (5)
I4	0.616610 (17)	0.828106 (15)	−0.008095 (14)	0.02062 (5)
I5	0.656526 (15)	0.622931 (15)	0.290508 (14)	0.01738 (5)
I6	0.347578 (16)	0.866911 (15)	0.199857 (14)	0.01794 (5)
K1	0.87845 (6)	0.26627 (6)	0.02007 (5)	0.02464 (16)
C11	1.1070 (3)	0.2811 (3)	−0.1752 (3)	0.0280 (8)
C12	1.0491 (3)	0.3885 (3)	−0.1573 (2)	0.0283 (8)
C13	1.0874 (3)	0.3586 (3)	−0.0104 (3)	0.0321 (8)
C14	1.0429 (3)	0.3262 (3)	0.0948 (3)	0.0355 (9)
C15	1.1006 (3)	0.1379 (3)	0.1309 (3)	0.0311 (8)
C16	1.0670 (3)	0.0546 (3)	0.1296 (3)	0.0304 (8)
C17	1.1260 (3)	0.0583 (3)	−0.0350 (3)	0.0340 (9)
C18	1.0867 (3)	0.1128 (3)	−0.1245 (3)	0.0350 (9)
O11	1.00921 (19)	0.38374 (19)	−0.05819 (17)	0.0255 (5)
O12	1.01417 (19)	0.23531 (19)	0.12376 (17)	0.0275 (5)
O13	1.03883 (19)	0.07813 (18)	0.04301 (17)	0.0259 (5)
O14	1.03594 (19)	0.22495 (19)	−0.13803 (17)	0.0266 (5)
C21	0.7201 (3)	0.5316 (3)	−0.0344 (3)	0.0320 (9)
C22	0.6853 (3)	0.5097 (3)	0.0733 (3)	0.0310 (8)
C23	0.7299 (3)	0.3705 (3)	0.2107 (2)	0.0308 (8)
C24	0.6659 (3)	0.3047 (3)	0.2275 (3)	0.0322 (9)
C25	0.6729 (3)	0.1694 (3)	0.1752 (3)	0.0288 (8)
C26	0.6238 (3)	0.2309 (3)	0.0904 (3)	0.0340 (9)
C27	0.6663 (3)	0.3273 (3)	−0.0708 (3)	0.0321 (9)
C28	0.6417 (3)	0.4372 (3)	−0.0635 (3)	0.0302 (8)
O21	0.7640 (2)	0.41800 (19)	0.11250 (17)	0.0276 (5)
O22	0.7307 (2)	0.21937 (17)	0.18654 (16)	0.0260 (5)
O23	0.7043 (2)	0.24662 (19)	0.00826 (17)	0.0289 (6)
O24	0.7359 (2)	0.44568 (19)	−0.06682 (17)	0.0285 (6)
K2	0.11831 (6)	0.22973 (6)	0.48454 (5)	0.02650 (16)
C31	0.3518 (3)	0.0376 (3)	0.5669 (3)	0.0342 (9)
C32	0.2927 (4)	−0.0246 (3)	0.5681 (3)	0.0368 (9)
C33	0.3126 (3)	0.0022 (3)	0.4027 (3)	0.0325 (9)
C34	0.2645 (3)	0.0823 (3)	0.3223 (3)	0.0316 (9)
C35	0.3355 (3)	0.2173 (3)	0.2773 (3)	0.0367 (9)
C36	0.3128 (4)	0.3165 (3)	0.3009 (3)	0.0369 (9)
C37	0.3715 (3)	0.2544 (3)	0.4442 (3)	0.0394 (10)
C38	0.3336 (4)	0.2139 (3)	0.5493 (3)	0.0404 (10)
O31	0.2431 (2)	0.02166 (19)	0.48992 (16)	0.0271 (5)
O32	0.2441 (2)	0.18831 (18)	0.31830 (17)	0.0264 (5)
O33	0.2846 (2)	0.30373 (18)	0.40119 (17)	0.0278 (5)
O34	0.2827 (2)	0.14026 (19)	0.57268 (17)	0.0286 (5)
C41	−0.0812 (3)	0.3261 (3)	0.6667 (2)	0.0308 (8)
C42	−0.1146 (3)	0.2381 (3)	0.6766 (3)	0.0305 (8)
C43	−0.0511 (3)	0.0877 (3)	0.6168 (3)	0.0279 (8)
C44	−0.0919 (3)	0.1341 (3)	0.5276 (3)	0.0292 (8)
C45	−0.0491 (4)	0.2343 (3)	0.3665 (3)	0.0351 (9)
C46	−0.1034 (3)	0.3466 (3)	0.3731 (3)	0.0346 (9)
C47	−0.0782 (3)	0.4726 (3)	0.4159 (3)	0.0290 (8)
C48	−0.1255 (3)	0.4497 (3)	0.5214 (3)	0.0296 (8)
O41	−0.02552 (19)	0.15975 (18)	0.63709 (17)	0.0255 (5)
O42	−0.01199 (19)	0.16256 (18)	0.44931 (16)	0.0259 (5)
O43	−0.03058 (19)	0.38011 (19)	0.38279 (17)	0.0259 (5)
O44	−0.04389 (19)	0.37664 (19)	0.56947 (16)	0.0254 (5)
H11A	1.1639	0.2432	−0.1435	0.034*
H11B	1.1339	0.2878	−0.2421	0.034*
H12A	0.9918	0.4233	−0.1883	0.034*
H12B	1.0963	0.4272	−0.1854	0.034*
H13A	1.1478	0.3014	−0.0290	0.039*
H13B	1.1066	0.4194	−0.0276	0.039*
H14A	0.9820	0.3845	0.1107	0.043*
H14B	1.0946	0.3120	0.1270	0.043*
H15A	1.1580	0.1465	0.0778	0.037*
H15B	1.1215	0.1189	0.1889	0.037*
H16A	1.0073	0.0508	0.1814	0.037*
H16B	1.1233	−0.0119	0.1388	0.037*
H17A	1.1758	0.0858	−0.0370	0.041*
H17B	1.1584	−0.0163	−0.0278	0.041*
H18A	1.0384	0.0830	−0.1219	0.042*
H18B	1.1456	0.0998	−0.1770	0.042*
H21A	0.7849	0.5438	−0.0533	0.038*
H21B	0.6682	0.5939	−0.0622	0.038*
H22A	0.6203	0.4971	0.0953	0.037*
H22B	0.6771	0.5676	0.0934	0.037*
H23A	0.7900	0.3248	0.2372	0.037*
H23B	0.6882	0.4246	0.2431	0.037*
H24A	0.6083	0.3472	0.1970	0.039*
H24B	0.6397	0.2780	0.2942	0.039*
H25A	0.7192	0.1014	0.1660	0.035*
H25B	0.6181	0.1610	0.2310	0.035*
H26A	0.5735	0.2979	0.0992	0.041*
H26B	0.5899	0.1923	0.0824	0.041*
H27A	0.7177	0.3177	−0.1286	0.039*
H27B	0.6032	0.3230	−0.0726	0.039*
H28A	0.5926	0.4471	−0.0046	0.036*
H28B	0.6127	0.4903	−0.1156	0.036*
H31A	0.4044	0.0424	0.5087	0.041*
H31B	0.3846	0.0036	0.6198	0.041*
H32A	0.2400	−0.0269	0.6263	0.044*
H32B	0.3400	−0.0950	0.5670	0.044*
H33A	0.3776	0.0083	0.3969	0.039*
H33B	0.3250	−0.0677	0.4023	0.039*
H34A	0.1997	0.0743	0.3305	0.038*
H34B	0.3110	0.0674	0.2641	0.038*
H35A	0.3925	0.1615	0.3036	0.044*
H35B	0.3530	0.2283	0.2098	0.044*
H36A	0.2561	0.3708	0.2732	0.044*
H36B	0.3740	0.3363	0.2735	0.044*
H37A	0.4216	0.1969	0.4182	0.047*
H37B	0.4031	0.3050	0.4313	0.047*
H38A	0.2858	0.2733	0.5737	0.049*
H38B	0.3931	0.1799	0.5773	0.049*
H41A	−0.0260	0.2964	0.6996	0.037*
H41B	−0.1398	0.3770	0.6959	0.037*
H42A	−0.1680	0.2648	0.6422	0.037*
H42B	−0.1408	0.2069	0.7422	0.037*
H43A	0.0105	0.0270	0.6085	0.033*
H43B	−0.1038	0.0662	0.6689	0.033*
H44A	−0.1530	0.1960	0.5329	0.035*
H44B	−0.1089	0.0836	0.5169	0.035*
H45A	0.0092	0.2334	0.3125	0.042*
H45B	−0.0973	0.2131	0.3565	0.042*
H46A	−0.1604	0.3497	0.4282	0.041*
H46B	−0.1296	0.3924	0.3174	0.041*
H47A	−0.0263	0.5026	0.4032	0.035*
H47B	−0.1327	0.5230	0.3834	0.035*
H48A	−0.1778	0.4193	0.5367	0.036*
H48B	−0.1566	0.5133	0.5413	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.0456 (3)	0.0172 (2)	0.0340 (3)	−0.0076 (2)	−0.0243 (2)	0.00278 (18)
Cu2	0.0448 (3)	0.0151 (2)	0.0482 (3)	−0.0098 (2)	−0.0300 (2)	0.00449 (19)
Cu3	0.0492 (3)	0.0165 (2)	0.0450 (3)	−0.0119 (2)	−0.0309 (2)	0.00662 (19)
Cu4	0.0437 (3)	0.0178 (2)	0.0307 (2)	−0.0069 (2)	−0.0237 (2)	0.00209 (18)
I1	0.02373 (11)	0.01329 (10)	0.01498 (10)	−0.00122 (8)	−0.00473 (8)	−0.00223 (8)
I2	0.02554 (12)	0.01789 (10)	0.02427 (11)	−0.00918 (9)	−0.01158 (9)	−0.00369 (8)
I3	0.02786 (12)	0.01916 (11)	0.02670 (11)	−0.01086 (9)	−0.01158 (9)	−0.00481 (9)
I4	0.02445 (12)	0.01306 (10)	0.01611 (10)	−0.00165 (8)	−0.00364 (8)	−0.00220 (8)
I5	0.01651 (11)	0.01301 (10)	0.02121 (10)	−0.00554 (8)	−0.00680 (8)	−0.00043 (8)
I6	0.01653 (11)	0.01358 (10)	0.02161 (11)	−0.00553 (8)	−0.00717 (8)	0.00030 (8)
K1	0.0148 (4)	0.0278 (4)	0.0278 (4)	−0.0046 (3)	−0.0031 (3)	−0.0089 (3)
C11	0.0250 (19)	0.0301 (19)	0.0255 (18)	−0.0131 (16)	0.0020 (14)	−0.0070 (15)
C12	0.028 (2)	0.0250 (18)	0.0261 (18)	−0.0112 (16)	−0.0062 (15)	0.0007 (15)
C13	0.036 (2)	0.029 (2)	0.037 (2)	−0.0169 (17)	−0.0169 (17)	0.0005 (16)
C14	0.049 (3)	0.033 (2)	0.038 (2)	−0.0220 (19)	−0.0181 (19)	−0.0064 (17)
C15	0.031 (2)	0.0277 (19)	0.033 (2)	−0.0091 (16)	−0.0181 (16)	0.0021 (15)
C16	0.033 (2)	0.0225 (18)	0.0293 (19)	−0.0087 (16)	−0.0126 (16)	0.0035 (15)
C17	0.033 (2)	0.0218 (18)	0.033 (2)	−0.0042 (16)	0.0020 (16)	−0.0078 (16)
C18	0.047 (2)	0.029 (2)	0.029 (2)	−0.0176 (18)	0.0025 (17)	−0.0133 (16)
O11	0.0230 (13)	0.0262 (13)	0.0250 (12)	−0.0078 (10)	−0.0072 (10)	−0.0038 (10)
O12	0.0304 (14)	0.0260 (13)	0.0290 (13)	−0.0116 (11)	−0.0117 (11)	−0.0038 (10)
O13	0.0252 (13)	0.0246 (13)	0.0265 (13)	−0.0093 (10)	−0.0048 (10)	−0.0058 (10)
O14	0.0267 (13)	0.0262 (13)	0.0255 (13)	−0.0117 (11)	−0.0038 (10)	−0.0047 (10)
C21	0.046 (2)	0.0207 (18)	0.032 (2)	−0.0154 (17)	−0.0103 (17)	−0.0034 (15)
C22	0.043 (2)	0.0207 (18)	0.030 (2)	−0.0056 (16)	−0.0139 (17)	−0.0084 (15)
C23	0.051 (2)	0.0254 (18)	0.0207 (17)	−0.0122 (17)	−0.0129 (17)	−0.0081 (14)
C24	0.044 (2)	0.0241 (18)	0.0224 (18)	−0.0106 (17)	0.0018 (16)	−0.0098 (15)
C25	0.040 (2)	0.0207 (17)	0.0299 (19)	−0.0166 (16)	−0.0068 (16)	−0.0046 (15)
C26	0.036 (2)	0.033 (2)	0.038 (2)	−0.0180 (18)	−0.0106 (17)	−0.0060 (17)
C27	0.046 (2)	0.033 (2)	0.0255 (19)	−0.0161 (18)	−0.0185 (17)	−0.0033 (15)
C28	0.035 (2)	0.0263 (19)	0.0268 (19)	−0.0047 (16)	−0.0174 (16)	−0.0024 (15)
O21	0.0375 (15)	0.0236 (12)	0.0239 (12)	−0.0123 (11)	−0.0092 (11)	−0.0046 (10)
O22	0.0369 (15)	0.0169 (12)	0.0252 (12)	−0.0078 (11)	−0.0091 (11)	−0.0067 (10)
O23	0.0363 (15)	0.0261 (13)	0.0262 (13)	−0.0094 (11)	−0.0128 (11)	−0.0055 (10)
O24	0.0394 (15)	0.0273 (13)	0.0232 (12)	−0.0156 (12)	−0.0072 (11)	−0.0066 (10)
K2	0.0163 (4)	0.0311 (4)	0.0295 (4)	−0.0049 (3)	−0.0027 (3)	−0.0118 (3)
C31	0.044 (2)	0.0268 (19)	0.033 (2)	−0.0074 (18)	−0.0218 (18)	−0.0026 (16)
C32	0.058 (3)	0.0257 (19)	0.029 (2)	−0.0176 (19)	−0.0211 (19)	0.0035 (16)
C33	0.043 (2)	0.0196 (18)	0.035 (2)	−0.0071 (17)	−0.0116 (18)	−0.0092 (15)
C34	0.044 (2)	0.0242 (18)	0.0286 (19)	−0.0101 (17)	−0.0074 (17)	−0.0127 (15)
C35	0.049 (3)	0.036 (2)	0.0259 (19)	−0.024 (2)	0.0036 (17)	−0.0102 (17)
C36	0.058 (3)	0.031 (2)	0.0241 (19)	−0.024 (2)	−0.0056 (18)	−0.0031 (16)
C37	0.043 (2)	0.035 (2)	0.045 (2)	−0.023 (2)	−0.022 (2)	0.0053 (18)
C38	0.059 (3)	0.037 (2)	0.042 (2)	−0.025 (2)	−0.027 (2)	−0.0027 (18)
O31	0.0344 (15)	0.0264 (13)	0.0229 (12)	−0.0132 (11)	−0.0088 (11)	−0.0039 (10)
O32	0.0352 (14)	0.0200 (12)	0.0253 (13)	−0.0080 (11)	−0.0080 (11)	−0.0082 (10)
O33	0.0371 (15)	0.0231 (12)	0.0246 (13)	−0.0095 (11)	−0.0111 (11)	−0.0051 (10)
O34	0.0361 (15)	0.0248 (13)	0.0260 (13)	−0.0119 (11)	−0.0091 (11)	−0.0046 (10)
C41	0.040 (2)	0.030 (2)	0.0225 (18)	−0.0145 (17)	−0.0033 (16)	−0.0083 (15)
C42	0.032 (2)	0.0264 (19)	0.0271 (19)	−0.0110 (16)	0.0024 (15)	−0.0083 (15)
C43	0.030 (2)	0.0203 (17)	0.0289 (19)	−0.0086 (15)	−0.0068 (15)	−0.0024 (14)
C44	0.027 (2)	0.0274 (19)	0.035 (2)	−0.0103 (16)	−0.0106 (16)	−0.0074 (16)
C45	0.055 (3)	0.030 (2)	0.029 (2)	−0.0133 (19)	−0.0232 (18)	−0.0048 (16)
C46	0.041 (2)	0.0268 (19)	0.042 (2)	−0.0125 (18)	−0.0279 (19)	0.0010 (17)
C47	0.036 (2)	0.0200 (17)	0.033 (2)	−0.0110 (16)	−0.0120 (16)	−0.0035 (15)
C48	0.027 (2)	0.0216 (18)	0.034 (2)	−0.0012 (15)	−0.0080 (16)	−0.0084 (15)
O41	0.0250 (13)	0.0249 (13)	0.0267 (13)	−0.0092 (11)	−0.0053 (10)	−0.0069 (10)
O42	0.0284 (13)	0.0246 (13)	0.0234 (12)	−0.0065 (11)	−0.0103 (10)	−0.0044 (10)
O43	0.0285 (14)	0.0267 (13)	0.0267 (13)	−0.0124 (11)	−0.0089 (10)	−0.0058 (10)
O44	0.0287 (13)	0.0263 (13)	0.0226 (12)	−0.0125 (11)	−0.0060 (10)	−0.0047 (10)

Geometric parameters (Å, º)

Cu1—Cu2	2.5053 (6)	C35—C36	1.503 (5)
Cu1—I4^i	2.5449 (5)	C36—O33	1.432 (4)
Cu1—Cu1^i	2.6156 (9)	C37—O33	1.421 (5)
Cu1—I3	2.6207 (5)	C37—C38	1.500 (6)
Cu1—I6	2.7514 (5)	C38—O34	1.432 (4)
Cu1—I4	2.8516 (5)	C41—O44	1.434 (4)
Cu2—I5	2.5451 (5)	C41—C42	1.503 (5)
Cu2—I3	2.6330 (5)	C42—O41	1.434 (4)
Cu2—Cu3	2.6439 (7)	C43—O41	1.427 (4)
Cu2—I4	2.7665 (6)	C43—C44	1.509 (5)
Cu2—I6	2.7871 (5)	C44—O42	1.430 (4)
Cu3—Cu4^ii	2.5024 (6)	C45—O42	1.428 (4)
Cu3—I6	2.5431 (5)	C45—C46	1.508 (5)
Cu3—I2	2.6320 (5)	C46—O43	1.421 (4)
Cu3—I1	2.7624 (6)	C47—O43	1.429 (4)
Cu3—I5	2.8264 (6)	C47—C48	1.510 (5)
Cu4—Cu3^ii	2.5024 (6)	C48—O44	1.428 (4)
Cu4—I1	2.5511 (5)	C11—H11A	0.9600
Cu4—Cu4^ii	2.6059 (9)	C11—H11B	0.9600
Cu4—I2^ii	2.6293 (5)	C12—H12A	0.9600
Cu4—I5^ii	2.7483 (5)	C12—H12B	0.9600
Cu4—I1^ii	2.8296 (5)	C13—H13A	0.9601
I1—Cu4^ii	2.8296 (5)	C13—H13B	0.9599
I2—Cu4^ii	2.6293 (5)	C14—H14A	0.9599
I4—Cu1^i	2.5450 (5)	C14—H14B	0.9600
I5—Cu4^ii	2.7483 (5)	C15—H15A	0.9600
K1—O21	2.705 (2)	C15—H15B	0.9600
K1—O13	2.721 (2)	C16—H16A	0.9600
K1—O23	2.754 (3)	C16—H16B	0.9600
K1—O24	2.754 (3)	C17—H17A	0.9600
K1—O14	2.764 (2)	C17—H17B	0.9599
K1—O11	2.770 (2)	C18—H18A	0.9599
K1—O12	2.776 (3)	C18—H18B	0.9599
K1—O22	2.795 (3)	C21—H21A	0.9600
K1—C23	3.451 (4)	C21—H21B	0.9600
K1—C16	3.458 (4)	C22—H22A	0.9599
K1—C27	3.487 (4)	C22—H22B	0.9599
K1—C21	3.490 (4)	C23—H23A	0.9599
C11—O14	1.426 (4)	C23—H23B	0.9599
C11—C12	1.508 (5)	C24—H24A	0.9600
C12—O11	1.434 (4)	C24—H24B	0.9600
C13—O11	1.424 (4)	C25—H25A	0.9599
C13—C14	1.505 (5)	C25—H25B	0.9600
C14—O12	1.428 (4)	C26—H26A	0.9600
C15—O12	1.430 (4)	C26—H26B	0.9600
C15—C16	1.510 (5)	C27—H27A	0.9599
C16—O13	1.428 (4)	C27—H27B	0.9601
C17—O13	1.426 (4)	C28—H28A	0.9600
C17—C18	1.498 (6)	C28—H28B	0.9601
C18—O14	1.440 (4)	C31—H31A	0.9600
C21—O24	1.429 (4)	C31—H31B	0.9600
C21—C22	1.524 (5)	C32—H32A	0.9600
C22—O21	1.421 (4)	C32—H32B	0.9599
C23—O21	1.424 (4)	C33—H33A	0.9600
C23—C24	1.511 (5)	C33—H33B	0.9601
C24—O22	1.419 (4)	C34—H34A	0.9601
C25—O22	1.421 (4)	C34—H34B	0.9600
C25—C26	1.512 (5)	C35—H35A	0.9600
C26—O23	1.420 (4)	C35—H35B	0.9601
C27—O23	1.426 (4)	C36—H36A	0.9600
C27—C28	1.530 (5)	C36—H36B	0.9600
C28—O24	1.414 (4)	C37—H37A	0.9599
K2—O32	2.708 (2)	C37—H37B	0.9601
K2—O44	2.737 (2)	C38—H38A	0.9600
K2—O41	2.752 (2)	C38—H38B	0.9600
K2—O34	2.757 (3)	C41—H41A	0.9599
K2—O31	2.769 (3)	C41—H41B	0.9600
K2—O42	2.771 (3)	C42—H42A	0.9599
K2—O33	2.775 (3)	C42—H42B	0.9601
K2—O43	2.776 (3)	C43—H43A	0.9599
K2—C34	3.459 (4)	C43—H43B	0.9600
K2—C41	3.487 (4)	C44—H44A	0.9599
K2—C43	3.499 (4)	C44—H44B	0.9600
K2—C45	3.517 (4)	C45—H45A	0.9600
C31—O34	1.414 (4)	C45—H45B	0.9601
C31—C32	1.494 (5)	C46—H46A	0.9599
C32—O31	1.431 (4)	C46—H46B	0.9600
C33—O31	1.425 (4)	C47—H47A	0.9600
C33—C34	1.493 (5)	C47—H47B	0.9601
C34—O32	1.426 (4)	C48—H48A	0.9600
C35—O32	1.429 (5)	C48—H48B	0.9600
Cu2—Cu1—I4^i	175.85 (3)	O31—K2—C45	93.65 (8)
Cu2—Cu1—Cu1^i	117.07 (3)	O42—K2—C45	22.49 (8)
I4^i—Cu1—Cu1^i	67.070 (18)	O33—K2—C45	126.34 (9)
Cu2—Cu1—I3	61.768 (15)	O43—K2—C45	42.43 (8)
I4^i—Cu1—I3	116.131 (18)	C34—K2—C45	70.92 (10)
Cu1^i—Cu1—I3	130.17 (3)	C41—K2—C45	95.38 (10)
Cu2—Cu1—I6	63.837 (16)	C43—K2—C45	63.13 (9)
I4^i—Cu1—I6	114.459 (19)	O34—C31—C32	109.8 (3)
Cu1^i—Cu1—I6	118.00 (3)	O31—C32—C31	112.6 (3)
I3—Cu1—I6	105.582 (17)	O31—C32—K2	47.65 (16)
Cu2—Cu1—I4	61.787 (16)	C31—C32—K2	81.9 (2)
I4^i—Cu1—I4	122.351 (18)	O31—C33—C34	108.9 (3)
Cu1^i—Cu1—I4	55.281 (17)	O32—C34—C33	113.6 (3)
I3—Cu1—I4	101.458 (17)	O32—C34—K2	47.50 (15)
I6—Cu1—I4	93.507 (14)	C33—C34—K2	84.5 (2)
Cu1—Cu2—I5	172.85 (2)	O32—C35—C36	108.3 (3)
Cu1—Cu2—I3	61.272 (15)	O33—C36—C35	112.4 (3)
I5—Cu2—I3	111.575 (18)	O33—C36—K2	47.78 (17)
Cu1—Cu2—Cu3	117.64 (2)	C35—C36—K2	81.9 (2)
I5—Cu2—Cu3	65.974 (16)	O33—C37—C38	108.8 (3)
I3—Cu2—Cu3	127.11 (2)	O34—C38—C37	112.7 (3)
Cu1—Cu2—I4	65.273 (16)	O34—C38—K2	47.20 (17)
I5—Cu2—I4	118.52 (2)	C37—C38—K2	83.7 (2)
I3—Cu2—I4	103.425 (17)	C33—O31—C32	113.8 (3)
Cu3—Cu2—I4	124.65 (2)	C33—O31—K2	116.36 (19)
Cu1—Cu2—I6	62.380 (16)	C32—O31—K2	109.9 (2)
I5—Cu2—I6	121.723 (19)	C34—O32—C35	113.0 (3)
I3—Cu2—I6	104.243 (17)	C34—O32—K2	109.6 (2)
Cu3—Cu2—I6	55.766 (15)	C35—O32—K2	119.6 (2)
I4—Cu2—I6	94.612 (16)	C37—O33—C36	114.0 (3)
Cu4^ii—Cu3—I6	175.33 (2)	C37—O33—K2	118.5 (2)
Cu4^ii—Cu3—I2	61.544 (15)	C36—O33—K2	109.8 (2)
I6—Cu3—I2	113.848 (19)	C31—O34—C38	114.3 (3)
Cu4^ii—Cu3—Cu2	117.00 (3)	C31—O34—K2	117.2 (2)
I6—Cu3—Cu2	64.971 (15)	C38—O34—K2	110.4 (2)
I2—Cu3—Cu2	130.55 (3)	O44—C41—C42	112.6 (3)
Cu4^ii—Cu3—I1	64.802 (16)	O44—C41—K2	47.76 (15)
I6—Cu3—I1	118.31 (2)	C42—C41—K2	83.41 (19)
I2—Cu3—I1	103.286 (17)	O41—C42—C41	108.4 (3)
Cu2—Cu3—I1	120.91 (2)	O41—C43—C44	113.1 (3)
Cu4^ii—Cu3—I5	61.742 (16)	O41—C43—K2	47.82 (15)
I6—Cu3—I5	120.286 (19)	C44—C43—K2	83.7 (2)
I2—Cu3—I5	103.675 (17)	O42—C44—C43	108.3 (3)
Cu2—Cu3—I5	55.332 (15)	O42—C45—C46	113.0 (3)
I1—Cu3—I5	94.392 (15)	O42—C45—K2	47.94 (16)
Cu3^ii—Cu4—I1	174.98 (2)	C46—C45—K2	82.9 (2)
Cu3^ii—Cu4—Cu4^ii	117.79 (3)	O43—C46—C45	108.6 (3)
I1—Cu4—Cu4^ii	66.546 (17)	O43—C47—C48	112.6 (3)
Cu3^ii—Cu4—I2^ii	61.654 (15)	O43—C47—K2	48.09 (16)
I1—Cu4—I2^ii	113.920 (18)	C48—C47—K2	82.7 (2)
Cu4^ii—Cu4—I2^ii	127.91 (3)	O44—C48—C47	108.1 (3)
Cu3^ii—Cu4—I5^ii	64.938 (16)	C43—O41—C42	114.1 (3)
I1—Cu4—I5^ii	115.647 (19)	C43—O41—K2	109.57 (19)
Cu4^ii—Cu4—I5^ii	120.75 (3)	C42—O41—K2	117.05 (19)
I2^ii—Cu4—I5^ii	105.932 (16)	C45—O42—C44	114.0 (3)
Cu3^ii—Cu4—I1^ii	62.047 (16)	C45—O42—K2	109.6 (2)
I1—Cu4—I1^ii	122.346 (17)	C44—O42—K2	117.25 (19)
Cu4^ii—Cu4—I1^ii	55.800 (17)	C46—O43—C47	113.7 (3)
I2^ii—Cu4—I1^ii	101.552 (17)	C46—O43—K2	117.3 (2)
I5^ii—Cu4—I1^ii	94.628 (14)	C47—O43—K2	109.4 (2)
Cu4—I1—Cu3	110.755 (16)	C48—O44—C41	113.6 (3)
Cu4—I1—Cu4^ii	57.654 (17)	C48—O44—K2	118.91 (19)
Cu3—I1—Cu4^ii	53.151 (13)	C41—O44—K2	109.4 (2)
Cu4^ii—I2—Cu3	56.801 (14)	O14—C11—H11A	109.4
Cu1—I3—Cu2	56.961 (14)	C12—C11—H11A	109.7
Cu1^i—I4—Cu2	110.588 (16)	O14—C11—H11B	109.6
Cu1^i—I4—Cu1	57.649 (18)	C12—C11—H11B	110.3
Cu2—I4—Cu1	52.940 (13)	H11A—C11—H11B	109.5
Cu2—I5—Cu4^ii	111.948 (16)	O11—C12—H12A	109.2
Cu2—I5—Cu3	58.693 (16)	C11—C12—H12A	107.4
Cu4^ii—I5—Cu3	53.323 (13)	K1—C12—H12A	83.2
Cu3—I6—Cu1	112.588 (17)	O11—C12—H12B	109.7
Cu3—I6—Cu2	59.263 (16)	C11—C12—H12B	107.9
Cu1—I6—Cu2	53.783 (14)	K1—C12—H12B	158.4
O21—K1—O13	137.84 (8)	H12A—C12—H12B	109.5
O21—K1—O23	93.37 (8)	O11—C13—H13A	109.4
O13—K1—O23	111.79 (8)	C14—C13—H13A	109.8
O21—K1—O24	62.48 (7)	O11—C13—H13B	109.1
O13—K1—O24	159.29 (8)	C14—C13—H13B	111.0
O23—K1—O24	62.83 (7)	H13A—C13—H13B	109.5
O21—K1—O14	141.76 (8)	O12—C14—H14A	109.2
O13—K1—O14	62.02 (7)	C13—C14—H14A	107.6
O23—K1—O14	108.47 (8)	K1—C14—H14A	86.2
O24—K1—O14	99.62 (7)	O12—C14—H14B	109.5
O21—K1—O11	81.67 (7)	C13—C14—H14B	108.0
O13—K1—O11	93.79 (7)	K1—C14—H14B	156.4
O23—K1—O11	145.15 (8)	H14A—C14—H14B	109.5
O24—K1—O11	84.78 (7)	O12—C15—H15A	109.1
O14—K1—O11	62.35 (7)	C16—C15—H15A	109.8
O21—K1—O12	78.69 (8)	O12—C15—H15B	109.3
O13—K1—O12	62.80 (7)	C16—C15—H15B	110.8
O23—K1—O12	151.13 (8)	H15A—C15—H15B	109.5
O24—K1—O12	132.14 (7)	O13—C16—H16A	108.9
O14—K1—O12	94.01 (8)	C15—C16—H16A	107.6
O11—K1—O12	61.75 (7)	K1—C16—H16A	82.1
O21—K1—O22	63.06 (7)	O13—C16—H16B	109.7
O13—K1—O22	99.62 (7)	C15—C16—H16B	108.5
O23—K1—O22	60.75 (7)	K1—C16—H16B	157.9
O24—K1—O22	94.61 (7)	H16A—C16—H16B	109.5
O14—K1—O22	155.18 (7)	O13—C17—H17A	109.6
O11—K1—O22	139.78 (7)	C18—C17—H17A	109.6
O12—K1—O22	91.33 (7)	O13—C17—H17B	109.5
O21—K1—C23	22.90 (8)	C18—C17—H17B	110.4
O13—K1—C23	120.46 (8)	H17A—C17—H17B	109.5
O23—K1—C23	89.45 (9)	O14—C18—H18A	109.6
O24—K1—C23	80.13 (8)	C17—C18—H18A	108.3
O14—K1—C23	159.89 (9)	K1—C18—H18A	86.9
O11—K1—C23	97.74 (8)	O14—C18—H18B	108.9
O12—K1—C23	72.41 (9)	C17—C18—H18B	107.9
O22—K1—C23	43.17 (8)	K1—C18—H18B	155.8
O21—K1—C16	114.83 (9)	H18A—C18—H18B	109.5
O13—K1—C16	23.01 (8)	O24—C21—H21A	109.0
O23—K1—C16	121.87 (8)	C22—C21—H21A	107.1
O24—K1—C16	175.17 (8)	K1—C21—H21A	83.8
O14—K1—C16	80.16 (8)	O24—C21—H21B	109.6
O11—K1—C16	90.88 (8)	C22—C21—H21B	108.8
O12—K1—C16	43.27 (8)	K1—C21—H21B	157.8
O22—K1—C16	87.32 (8)	H21A—C21—H21B	109.5
C23—K1—C16	98.40 (9)	O21—C22—H22A	109.4
O21—K1—C27	90.15 (9)	C21—C22—H22A	109.9
O13—K1—C27	125.72 (8)	O21—C22—H22B	109.2
O23—K1—C27	22.75 (8)	C21—C22—H22B	111.2
O24—K1—C27	43.03 (8)	H22A—C22—H22B	109.5
O14—K1—C27	98.14 (9)	O21—C23—H23A	109.2
O11—K1—C27	122.41 (8)	C24—C23—H23A	107.6
O12—K1—C27	167.59 (9)	K1—C23—H23A	83.5
O22—K1—C27	78.65 (8)	O21—C23—H23B	109.3
C23—K1—C27	95.20 (10)	C24—C23—H23B	108.6
C16—K1—C27	141.80 (9)	K1—C23—H23B	156.9
O21—K1—C21	42.85 (8)	H23A—C23—H23B	109.5
O13—K1—C21	166.57 (9)	O22—C24—H24A	109.1
O23—K1—C21	80.18 (8)	C23—C24—H24A	109.2
O24—K1—C21	22.79 (8)	O22—C24—H24B	109.7
O14—K1—C21	109.29 (8)	C23—C24—H24B	110.9
O11—K1—C21	72.81 (8)	H24A—C24—H24B	109.5
O12—K1—C21	109.80 (8)	O22—C25—H25A	109.0
O22—K1—C21	91.52 (8)	C26—C25—H25A	107.6
C23—K1—C21	63.82 (9)	O22—C25—H25B	109.7
C16—K1—C21	152.95 (9)	C26—C25—H25B	108.2
C27—K1—C21	63.70 (9)	H25A—C25—H25B	109.5
O14—C11—C12	108.4 (3)	O23—C26—H26A	109.8
O11—C12—C11	113.0 (3)	C25—C26—H26A	109.8
O11—C12—K1	48.68 (15)	O23—C26—H26B	109.1
C11—C12—K1	83.62 (19)	C25—C26—H26B	110.4
O11—C13—C14	108.0 (3)	H26A—C26—H26B	109.5
O12—C14—C13	113.0 (3)	O23—C27—H27A	109.7
O12—C14—K1	47.33 (16)	C28—C27—H27A	108.6
C13—C14—K1	82.6 (2)	K1—C27—H27A	85.0
O12—C15—C16	108.4 (3)	O23—C27—H27B	108.8
O13—C16—C15	112.5 (3)	C28—C27—H27B	108.5
O13—C16—K1	48.13 (15)	K1—C27—H27B	157.0
C15—C16—K1	84.6 (2)	H27A—C27—H27B	109.5
O13—C17—C18	108.1 (3)	O24—C28—H28A	109.8
O14—C18—C17	112.6 (3)	C27—C28—H28A	109.7
O14—C18—K1	47.48 (15)	O24—C28—H28B	109.2
C17—C18—K1	82.2 (2)	C27—C28—H28B	110.2
C13—O11—C12	113.6 (3)	H28A—C28—H28B	109.5
C13—O11—K1	118.0 (2)	O34—C31—H31A	109.3
C12—O11—K1	108.44 (19)	C32—C31—H31A	109.1
C14—O12—C15	114.0 (3)	O34—C31—H31B	109.1
C14—O12—K1	110.5 (2)	C32—C31—H31B	110.0
C15—O12—K1	116.1 (2)	H31A—C31—H31B	109.5
C17—O13—C16	114.1 (3)	O31—C32—H32A	108.9
C17—O13—K1	119.4 (2)	C31—C32—H32A	107.2
C16—O13—K1	108.86 (19)	K2—C32—H32A	85.3
C11—O14—C18	113.7 (3)	O31—C32—H32B	109.8
C11—O14—K1	117.73 (19)	C31—C32—H32B	108.9
C18—O14—K1	109.95 (19)	K2—C32—H32B	157.1
O24—C21—C22	112.8 (3)	H32A—C32—H32B	109.5
O24—C21—K1	48.27 (16)	O31—C33—H33A	109.1
C22—C21—K1	82.8 (2)	C34—C33—H33A	109.4
O21—C22—C21	107.6 (3)	O31—C33—H33B	109.4
O21—C23—C24	112.7 (3)	C34—C33—H33B	110.5
O21—C23—K1	47.64 (15)	H33A—C33—H33B	109.5
C24—C23—K1	84.27 (19)	O32—C34—H34A	109.1
O22—C24—C23	108.4 (3)	C33—C34—H34A	107.2
O22—C25—C26	112.8 (3)	K2—C34—H34A	84.2
O23—C26—C25	108.3 (3)	O32—C34—H34B	109.2
O23—C27—C28	111.7 (3)	C33—C34—H34B	108.2
O23—C27—K1	48.33 (16)	K2—C34—H34B	156.7
C28—C27—K1	82.3 (2)	H34A—C34—H34B	109.5
O24—C28—C27	108.4 (3)	O32—C35—H35A	109.1
C22—O21—C23	113.7 (3)	C36—C35—H35A	109.9
C22—O21—K1	119.87 (19)	O32—C35—H35B	109.3
C23—O21—K1	109.45 (19)	C36—C35—H35B	110.7
C24—O22—C25	112.9 (3)	H35A—C35—H35B	109.5
C24—O22—K1	114.79 (19)	O33—C36—H36A	109.4
C25—O22—K1	111.63 (19)	C35—C36—H36A	107.9
C26—O23—C27	113.4 (3)	K2—C36—H36A	85.9
C26—O23—K1	120.8 (2)	O33—C36—H36B	109.1
C27—O23—K1	108.9 (2)	C35—C36—H36B	108.6
C28—O24—C21	113.5 (3)	K2—C36—H36B	156.5
C28—O24—K1	116.62 (19)	H36A—C36—H36B	109.5
C21—O24—K1	108.9 (2)	O33—C37—H37A	109.3
O32—K2—O44	145.93 (8)	C38—C37—H37A	109.9
O32—K2—O41	140.19 (8)	O33—C37—H37B	109.1
O44—K2—O41	62.69 (7)	C38—C37—H37B	110.3
O32—K2—O34	93.22 (8)	H37A—C37—H37B	109.5
O44—K2—O34	110.22 (7)	O34—C38—H38A	109.6
O41—K2—O34	97.55 (8)	C37—C38—H38A	108.0
O32—K2—O31	62.79 (7)	K2—C38—H38A	85.6
O44—K2—O31	150.23 (8)	O34—C38—H38B	109.1
O41—K2—O31	88.92 (7)	C37—C38—H38B	107.9
O34—K2—O31	62.24 (7)	K2—C38—H38B	156.1
O32—K2—O42	84.08 (7)	H38A—C38—H38B	109.5
O44—K2—O42	93.87 (7)	O44—C41—H41A	109.0
O41—K2—O42	62.38 (7)	C42—C41—H41A	107.6
O34—K2—O42	137.40 (8)	K2—C41—H41A	84.0
O31—K2—O42	79.26 (7)	O44—C41—H41B	109.5
O32—K2—O33	62.02 (7)	C42—C41—H41B	108.6
O44—K2—O33	107.26 (7)	K2—C41—H41B	157.2
O41—K2—O33	153.53 (8)	H41A—C41—H41B	109.5
O34—K2—O33	61.53 (7)	O41—C42—H42A	109.1
O31—K2—O33	94.28 (7)	C41—C42—H42A	109.7
O42—K2—O33	144.00 (7)	O41—C42—H42B	109.5
O32—K2—O43	87.63 (7)	C41—C42—H42B	110.8
O44—K2—O43	62.02 (7)	H42A—C42—H42B	109.5
O41—K2—O43	94.23 (7)	O41—C43—H43A	109.2
O34—K2—O43	160.41 (8)	C44—C43—H43A	107.6
O31—K2—O43	133.83 (7)	K2—C43—H43A	84.5
O42—K2—O43	62.16 (7)	O41—C43—H43B	109.3
O33—K2—O43	102.23 (7)	C44—C43—H43B	108.1
O32—K2—C34	22.85 (8)	K2—C43—H43B	157.0
O44—K2—C34	159.43 (9)	H43A—C43—H43B	109.5
O41—K2—C34	118.62 (8)	O42—C44—H44A	109.3
O34—K2—C34	90.20 (9)	C43—C44—H44A	110.0
O31—K2—C34	43.06 (8)	O42—C44—H44B	109.2
O42—K2—C34	71.37 (9)	C43—C44—H44B	110.6
O33—K2—C34	79.80 (8)	H44A—C44—H44B	109.5
O43—K2—C34	97.84 (8)	O42—C45—H45A	109.1
O32—K2—C41	167.26 (9)	C46—C45—H45A	107.4
O44—K2—C41	22.82 (8)	K2—C45—H45A	84.6
O41—K2—C41	42.89 (8)	O42—C45—H45B	109.4
O34—K2—C41	98.55 (9)	C46—C45—H45B	108.5
O31—K2—C41	127.52 (8)	K2—C45—H45B	157.2
O42—K2—C41	90.50 (8)	H45A—C45—H45B	109.5
O33—K2—C41	119.92 (8)	O43—C46—H46A	108.8
O43—K2—C41	79.65 (8)	C45—C46—H46A	109.5
C34—K2—C41	160.27 (9)	O43—C46—H46B	109.5
O32—K2—C43	117.83 (8)	C45—C46—H46B	110.9
O44—K2—C43	79.90 (8)	H46A—C46—H46B	109.5
O41—K2—C43	22.61 (7)	O43—C47—H47A	109.3
O34—K2—C43	106.20 (8)	C48—C47—H47A	107.7
O31—K2—C43	75.49 (8)	K2—C47—H47A	84.7
O42—K2—C43	42.72 (8)	O43—C47—H47B	109.5
O33—K2—C43	167.14 (8)	C48—C47—H47B	108.3
O43—K2—C43	90.55 (8)	K2—C47—H47B	157.4
C34—K2—C43	97.19 (9)	H47A—C47—H47B	109.5
C41—K2—C43	63.42 (8)	O44—C48—H48A	109.5
O32—K2—C45	75.34 (9)	C47—C48—H48A	109.9
O44—K2—C45	89.91 (9)	O44—C48—H48B	109.3
O41—K2—C45	79.52 (9)	C47—C48—H48B	110.5
O34—K2—C45	155.85 (8)	H48A—C48—H48B	109.5

Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x+1, −y+1, −z+1.