Rapid structure determination of the hydrogen-containing compound Cs₂C₂O₄·H₂O by joint single-crystal X-ray and powder neutron diffraction

The structure determination of caesium oxalate monohydrate using single-crystal X-ray diffraction, powder neutron diffraction data and a combination of both has been undertaken. Results show that even for hydrogen-containing materials data collected rapidly on a high-flux neutron diffractometer improve the refinement such that accurate positional and thermal displacement parameters can be extracted for all atom types. This contrasts with structural models extracted from either data set alone that demonstrate the inherent limitations of the individual diffraction methods. The rapidity with which useful neutron diffraction data has been collected from hydrogen-containing compounds, 10 min in this study, indicates that the technique should be widely applicable allowing the facile and accurate extraction of hydrogen positions for many compounds.

Computing details

Data collection: COLLECT (Hooft, R.W.W., 1998) for 06mtw0002. Cell refinement: DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) for 06mtw0002. Data reduction: DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) for 06mtw0002. Program(s) used to solve structure: SHELXS97 (Sheldrick, 1997) for 06mtw0002. Program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) for 06mtw0002; GSAS for CSOXNEUT10MINS_publ, CSSXDRT_publ. Molecular graphics: CAMERON (Watkin, et al., 1993) for 06mtw0002. Software used to prepare material for publication: WinGX (Farrugia, 1998) for 06mtw0002.

Figures

(06mtw0002)

Crystal data

C2H2Cs2O5	F(000) = 656
Mr = 371.86	Dx = 3.416 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 10.0748 (5) Å	Cell parameters from 869 reflections
b = 6.6473 (3) Å	θ = 1.0–27.5°
c = 11.2997 (6) Å	µ = 10.04 mm^−1
β = 107.189 (3)°	T = 289 K
V = 722.94 (6) Å^3	Block, colourless
Z = 4	0.2 × 0.11 × 0.07 mm

Data collection

Bruker-Nonius CCD camera on κ-goniostat diffractometer	809 independent reflections
Radiation source: Bruker Nonius FR591 Rotating Anode	700 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.067
Detector resolution: 9.091 pixels mm^-1	θmax = 27.3°, θmin = 3.7°
ϕ & ω scans to fill the asymmetric unit	h = −12→12
Absorption correction: multi-scan SADABS V2.10 (Sheldrick, G.M., 2003)	k = −8→8
Tmin = 0.206, Tmax = 0.501	l = −14→14
4032 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.025	All H-atom parameters refined
wR(F^2) = 0.054	w = 1/[σ^2(Fo^2) + (0.0142P)^2 + 1.827P] where P = (Fo^2 + 2Fc^2)/3
S = 1.17	(Δ/σ)max = 0.001
809 reflections	Δρmax = 0.96 e Å^−3
47 parameters	Δρmin = −0.90 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0034 (2)

Special details

Experimental. SADABS was used to perform the Absorption correction Parameter refinement on 3332 reflections reduced R(int) from 0.1285 to 0.0275 Ratio of minimum to maximum apparent transmission: 0.544250 The given Tmin and Tmax were generated using the SHELX SIZE command

A thin coating of glue was applied to the crystal to reduce its deterioration during data collection

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
Cs1	0.87244 (3)	0.30550 (4)	0.37345 (2)	0.02732 (16)
O1	0.6398 (3)	0.2709 (6)	0.0934 (3)	0.0335 (8)
O2	0.8242 (3)	0.4550 (5)	0.0942 (3)	0.0303 (7)
O3	1.0000	−0.0535 (9)	0.2500	0.074 (2)
H1	0.968 (6)	−0.128 (9)	0.291 (5)	0.050 (18)*
C1	0.7393 (5)	0.3148 (6)	0.0543 (4)	0.0224 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cs1	0.02621 (19)	0.0275 (2)	0.0283 (2)	−0.00157 (11)	0.00824 (13)	−0.00304 (12)
O1	0.0317 (18)	0.0366 (18)	0.037 (2)	−0.0071 (15)	0.0183 (16)	−0.0071 (16)
O2	0.0331 (16)	0.0273 (16)	0.0308 (17)	−0.0049 (14)	0.0102 (14)	−0.0048 (13)
O3	0.124 (6)	0.029 (3)	0.110 (6)	0.000	0.095 (5)	0.000
C1	0.024 (2)	0.021 (2)	0.022 (2)	0.0055 (16)	0.0067 (18)	0.0041 (16)

Geometric parameters (Å, º)

Cs1—O2^i	3.116 (3)	O1—Cs1^iii	3.579 (4)
Cs1—O1^ii	3.120 (3)	O2—C1	1.256 (5)
Cs1—O1^iii	3.123 (4)	O2—Cs1^viii	3.116 (3)
Cs1—O2^iv	3.131 (3)	O2—Cs1^iv	3.131 (3)
Cs1—O2^v	3.149 (3)	O2—Cs1^iii	3.149 (3)
Cs1—O2	3.205 (3)	O3—Cs1^iv	3.217 (4)
Cs1—O3	3.217 (4)	O3—Cs1^ix	3.7162 (15)
Cs1—O1	3.343 (3)	O3—Cs1^v	3.7162 (15)
Cs1—C1	3.456 (4)	O3—H1	0.81 (6)
Cs1—O1^v	3.579 (4)	C1—C1^x	1.566 (9)
Cs1—C1^v	3.622 (4)	C1—Cs1^iii	3.622 (4)
Cs1—O3^vi	3.7162 (15)	C1—Cs1^v	3.733 (4)
Cs1—H1	3.26 (6)	C1—Cs1^viii	3.738 (4)
O1—C1	1.244 (6)	C1—Cs1^vii	3.743 (4)
O1—Cs1^vii	3.120 (3)	C1—Cs1^iv	3.753 (4)
O1—Cs1^v	3.123 (4)
O2^i—Cs1—O1^ii	75.37 (9)	O3—Cs1—H1	14.3 (10)
O2^i—Cs1—O1^iii	51.46 (9)	O1—Cs1—H1	81.6 (11)
O1^ii—Cs1—O1^iii	96.95 (8)	C1—Cs1—H1	77.0 (10)
O2^i—Cs1—O2^iv	97.01 (7)	O1^v—Cs1—H1	34.4 (10)
O1^ii—Cs1—O2^iv	51.36 (8)	C1^v—Cs1—H1	53.6 (10)
O1^iii—Cs1—O2^iv	75.12 (8)	O3^vi—Cs1—H1	117.9 (11)
O2^i—Cs1—O2^v	91.88 (8)	C1—O1—Cs1^vii	110.6 (3)
O1^ii—Cs1—O2^v	102.23 (9)	C1—O1—Cs1^v	109.8 (3)
O1^iii—Cs1—O2^v	132.11 (8)	Cs1^vii—O1—Cs1^v	83.05 (8)
O2^iv—Cs1—O2^v	147.93 (11)	C1—O1—Cs1	84.7 (3)
O2^i—Cs1—O2	127.99 (4)	Cs1^vii—O1—Cs1	164.58 (13)
O1^ii—Cs1—O2	132.74 (9)	Cs1^v—O1—Cs1	89.78 (9)
O1^iii—Cs1—O2	79.10 (8)	C1—O1—Cs1^iii	82.0 (2)
O2^iv—Cs1—O2	82.83 (9)	Cs1^vii—O1—Cs1^iii	101.34 (10)
O2^v—Cs1—O2	115.23 (6)	Cs1^v—O1—Cs1^iii	165.28 (13)
O2^i—Cs1—O3	154.52 (7)	Cs1—O1—Cs1^iii	82.46 (7)
O1^ii—Cs1—O3	82.14 (7)	C1—O2—Cs1^viii	110.1 (3)
O1^iii—Cs1—O3	145.25 (10)	C1—O2—Cs1^iv	110.1 (2)
O2^iv—Cs1—O3	77.58 (8)	Cs1^viii—O2—Cs1^iv	82.99 (7)
O2^v—Cs1—O3	81.21 (9)	C1—O2—Cs1^iii	101.9 (2)
O2—Cs1—O3	76.53 (7)	Cs1^viii—O2—Cs1^iii	88.12 (8)
O2^i—Cs1—O1	124.15 (8)	Cs1^iv—O2—Cs1^iii	147.93 (11)
O1^ii—Cs1—O1	160.33 (9)	C1—O2—Cs1	90.7 (2)
O1^iii—Cs1—O1	98.06 (8)	Cs1^viii—O2—Cs1	158.81 (11)
O2^iv—Cs1—O1	121.30 (8)	Cs1^iv—O2—Cs1	85.87 (7)
O2^v—Cs1—O1	76.69 (8)	Cs1^iii—O2—Cs1	91.88 (8)
O2—Cs1—O1	39.62 (8)	Cs1^iv—O3—Cs1	84.25 (14)
O3—Cs1—O1	78.27 (6)	Cs1^iv—O3—Cs1^ix	82.04 (3)
O2^i—Cs1—C1	136.21 (9)	Cs1—O3—Cs1^ix	120.85 (8)
O1^ii—Cs1—C1	144.25 (10)	Cs1^iv—O3—Cs1^v	120.85 (8)
O1^iii—Cs1—C1	95.19 (9)	Cs1—O3—Cs1^v	82.04 (3)
O2^iv—Cs1—C1	100.40 (9)	Cs1^ix—O3—Cs1^v	150.78 (18)
O2^v—Cs1—C1	94.06 (9)	Cs1^iv—O3—H1	169 (4)
O2—Cs1—C1	21.30 (8)	Cs1—O3—H1	86 (4)
O3—Cs1—C1	69.05 (7)	Cs1^ix—O3—H1	99 (4)
O1—Cs1—C1	20.99 (9)	Cs1^v—O3—H1	62 (4)
O2^i—Cs1—O1^v	113.90 (8)	O1—C1—O2	125.6 (4)
O1^ii—Cs1—O1^v	78.66 (10)	O1—C1—C1^x	117.5 (5)
O1^iii—Cs1—O1^v	165.28 (13)	O2—C1—C1^x	116.9 (5)
O2^iv—Cs1—O1^v	111.45 (8)	O1—C1—Cs1	74.4 (3)
O2^v—Cs1—O1^v	37.91 (8)	O2—C1—Cs1	68.0 (2)
O2—Cs1—O1^v	114.27 (8)	C1^x—C1—Cs1	135.0 (3)
O3—Cs1—O1^v	48.66 (9)	O1—C1—Cs1^iii	78.1 (2)
O1—Cs1—O1^v	89.69 (9)	O2—C1—Cs1^iii	58.3 (2)
C1—Cs1—O1^v	96.43 (9)	C1^x—C1—Cs1^iii	142.7 (3)
O2^i—Cs1—C1^v	98.47 (9)	Cs1—C1—Cs1^iii	80.30 (9)
O1^ii—Cs1—C1^v	85.79 (10)	O1—C1—Cs1^v	51.9 (2)
O1^iii—Cs1—C1^v	147.07 (10)	O2—C1—Cs1^v	144.3 (3)
O2^iv—Cs1—C1^v	128.12 (9)	C1^x—C1—Cs1^v	78.1 (3)
O2^v—Cs1—C1^v	19.83 (9)	Cs1—C1—Cs1^v	78.75 (8)
O2—Cs1—C1^v	122.30 (9)	Cs1^iii—C1—Cs1^v	129.32 (13)
O3—Cs1—C1^v	67.68 (10)	O1—C1—Cs1^viii	144.1 (3)
O1—Cs1—C1^v	88.49 (9)	O2—C1—Cs1^viii	51.6 (2)
C1—Cs1—C1^v	101.56 (10)	C1^x—C1—Cs1^viii	77.7 (3)
O1^v—Cs1—C1^v	19.88 (9)	Cs1—C1—Cs1^viii	119.42 (12)
O2^i—Cs1—O3^vi	78.03 (7)	Cs1^iii—C1—Cs1^viii	72.58 (7)
O1^ii—Cs1—O3^vi	151.44 (7)	Cs1^v—C1—Cs1^viii	155.80 (13)
O1^iii—Cs1—O3^vi	73.97 (10)	O1—C1—Cs1^vii	51.3 (2)
O2^iv—Cs1—O3^vi	143.73 (10)	O2—C1—Cs1^vii	144.4 (3)
O2^v—Cs1—O3^vi	68.28 (10)	C1^x—C1—Cs1^vii	78.3 (3)
O2—Cs1—O3^vi	73.13 (6)	Cs1—C1—Cs1^vii	125.59 (13)
O3—Cs1—O3^vi	120.85 (8)	Cs1^iii—C1—Cs1^vii	89.59 (9)
O1—Cs1—O3^vi	46.71 (7)	Cs1^v—C1—Cs1^vii	67.22 (7)
C1—Cs1—O3^vi	64.31 (7)	Cs1^viii—C1—Cs1^vii	107.56 (10)
O1^v—Cs1—O3^vi	103.15 (10)	O1—C1—Cs1^iv	144.8 (3)
C1^v—Cs1—O3^vi	88.01 (11)	O2—C1—Cs1^iv	51.6 (2)
O2^i—Cs1—H1	144.0 (10)	C1^x—C1—Cs1^iv	77.6 (3)
O1^ii—Cs1—H1	79.9 (11)	Cs1—C1—Cs1^iv	73.42 (8)
O1^iii—Cs1—H1	159.2 (10)	Cs1^iii—C1—Cs1^iv	109.83 (11)
O2^iv—Cs1—H1	87.3 (10)	Cs1^v—C1—Cs1^iv	107.45 (10)
O2^v—Cs1—H1	68.2 (10)	Cs1^viii—C1—Cs1^iv	67.08 (7)
O2—Cs1—H1	88.0 (10)	Cs1^vii—C1—Cs1^iv	155.89 (13)

Symmetry codes: (i) x, −y+1, z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) −x+2, y, −z+1/2; (v) −x+3/2, y−1/2, −z+1/2; (vi) x−1/2, y+1/2, z; (vii) x−1/2, −y+1/2, z−1/2; (viii) x, −y+1, z−1/2; (ix) x+1/2, y−1/2, z; (x) −x+3/2, −y+1/2, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H1···O1^v	0.81 (6)	2.05 (5)	2.819 (4)	161 (6)

Symmetry code: (v) −x+3/2, y−1/2, −z+1/2.

(CSOXJOINTRT_phase_1)

Crystal data

C2H2Cs2O5	β = 107.191 (4)°
Mr = 371.84	V = 727.98 (9) Å^3
Monoclinic, C2/c	Z = 4
a = 10.1125 (6) Å	? radiation, λ = 1.36 Å
b = 6.6535 (4) Å	?, ? × ? × ? mm
c = 11.3255 (7) Å

Data collection

2θmin = −0.400°, 2θmax = 154.400°, 2θstep = 0.1°

Refinement

Least-squares matrix: full	1549 data points
Rp = 0.010	Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 222.093 #2(GV) = -514.662 #3(GW) = 359.730 #4(LX) = 5.847 #5(LY) = 7.392 #6(trns) = 0.000 #7(asym) = 15.2584 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.013	73 parameters
Rexp = 0.009	0 restraints
R(F^2) = 0.06304	(Δ/σ)max = 0.02
χ^2 = 2.789	Background function: GSAS Background function number 2 with 10 terms. Cosine Fourier series 1: 10179.3 2: 5267.35 3: -576.316 4: 1077.15 5: -753.819 6: 677.534 7: -428.178 8: 169.871 9: -77.3448 10: 39.2779

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

	x	y	z	Uiso*/Ueq
O1	0.0	−0.4456 (5)	0.25	0.06563
O2	0.8606 (2)	−0.2708 (3)	0.40669 (19)	0.03119
O3	0.67580 (19)	−0.4548 (3)	0.40541 (17)	0.02845
CS4	0.872442 (19	0.194463 (26	0.373455 (17	0.0259
C5	0.7606 (3)	−0.3148 (3)	0.4454 (2)	0.01929
H6	0.9550 (9)	−0.3635 (11)	0.2968 (7)	0.04935

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.109 (3)	0.0288 (19)	0.095 (3)	0.0	0.086 (3)	0.0
O2	0.0322 (13)	0.0373 (12)	0.0311 (13)	−0.0061 (10)	0.0203 (11)	−0.0075 (10)
O3	0.0342 (11)	0.0270 (11)	0.0261 (12)	−0.0049 (9)	0.0121 (10)	−0.0063 (9)
CS4	0.02731 (16	0.02778 (17	0.02345 (17	0.00181 (8)	0.00882 (12	0.00307 (9)
C5	0.0224 (13)	0.0196 (14)	0.0161 (13)	0.0048 (11)	0.0061 (11)	0.0034 (10)
H6	0.052 (6)	0.044 (5)	0.065 (7)	0.004 (4)	0.036 (6)	−0.007 (5)

Geometric parameters (Å, º)

O1—O2^i	2.823 (2)	CS4—O1^xiii	3.7278 (8)
O1—O2^ii	2.823 (2)	CS4—O2	3.125 (2)
O1—O3^iii	3.985 (3)	CS4—O2^xx	3.583 (2)
O1—O3^iv	3.883 (3)	CS4—O2^xv	3.1260 (19)
O1—O3^v	3.985 (3)	CS4—O2^xxi	3.355 (2)
O1—O3^vi	3.883 (3)	CS4—O3^xx	3.1557 (18)
O1—CS4^vii	3.228 (2)	CS4—O3^xiii	3.1418 (18)
O1—CS4^viii	3.228 (2)	CS4—O3^xxi	3.2075 (19)
O1—CS4^iii	3.7278 (8)	CS4—O3^xii	3.1267 (18)
O1—CS4^v	3.7278 (8)	CS4—C5	3.738 (2)
O1—C5^i	3.832 (2)	CS4—C5^xx	3.626 (2)
O1—C5^ii	3.832 (2)	CS4—C5^xv	3.758 (3)
O1—C5^ix	3.920 (3)	CS4—C5^xiii	3.766 (3)
O1—C5^x	3.920 (3)	CS4—C5^xxi	3.462 (2)
O1—C5^iii	3.798 (3)	CS4—C5^xii	3.746 (2)
O1—C5^v	3.798 (3)	CS4—H6	3.957 (7)
O1—H6^i	0.964 (7)	CS4—H6^xx	3.245 (7)
O1—H6^ii	0.964 (7)	CS4—H6^xv	3.795 (8)
O2—O1^xi	2.823 (2)	CS4—H6^xxi	3.325 (9)
O2—O2^xii	3.514 (4)	C5—O1^xi	3.832 (2)
O2—O3	2.231 (3)	C5—O1^ix	3.920 (3)
O2—O3^xiii	3.822 (3)	C5—O1^xiii	3.798 (3)
O2—O3^xii	2.717 (3)	C5—O2	1.251 (3)
O2—CS4^xiv	3.583 (2)	C5—O2^xii	2.418 (3)
O2—CS4	3.125 (2)	C5—O3	1.256 (3)
O2—CS4^xv	3.1260 (19)	C5—O3^xii	2.417 (3)
O2—CS4^xvi	3.355 (2)	C5—CS4^xiv	3.626 (2)
O2—C5	1.251 (3)	C5—CS4	3.738 (2)
O2—C5^xii	2.418 (3)	C5—CS4^xv	3.758 (3)
O2—H6	1.881 (7)	C5—CS4^iii	3.766 (3)
O2—H6^xvii	3.422 (7)	C5—CS4^xvi	3.462 (2)
O3—O1^xviii	3.883 (3)	C5—CS4^xii	3.746 (2)
O3—O1^xiii	3.985 (3)	C5—C5^xii	1.573 (4)
O3—O2	2.231 (3)	C5—H6	2.959 (8)
O3—O2^iii	3.822 (3)	H6—O1^xi	0.964 (7)
O3—O2^xii	2.717 (3)	H6—O2	1.881 (7)
O3—O3^xii	3.516 (4)	H6—O2^xvii	3.422 (7)
O3—CS4^xiv	3.1557 (18)	H6—O3	3.450 (8)
O3—CS4^iii	3.1418 (18)	H6—O3^xiii	3.503 (8)
O3—CS4^xvi	3.2075 (19)	H6—O3^xxi	3.550 (8)
O3—CS4^xii	3.1267 (18)	H6—CS4^xiv	3.245 (7)
O3—C5	1.256 (3)	H6—CS4	3.957 (7)
O3—C5^xii	2.417 (3)	H6—CS4^xv	3.795 (8)
O3—H6	3.450 (8)	H6—CS4^xvi	3.325 (9)
O3—H6^iii	3.503 (8)	H6—C5	2.959 (8)
O3—H6^xvi	3.550 (8)	H6—H6^xvii	1.589 (14)
CS4—O1^xix	3.228 (2)
O2^i—O1—O2^ii	131.33 (14)	O1^xix—CS4—C5^xxi	69.09 (4)
O2^i—O1—O3^iii	108.24 (6)	O1^xix—CS4—C5^xxiv	172.62 (4)
O2^i—O1—O3^iv	67.37 (7)	O1^xix—CS4—H6	117.63 (11)
O2^i—O1—O3^v	112.80 (6)	O1^xix—CS4—H6^xx	17.14 (12)
O2^i—O1—O3^vi	72.04 (7)	O1^xix—CS4—H6^xv	94.59 (11)
O2^i—O1—CS4^vii	72.28 (5)	O1^xix—CS4—H6^xxi	106.96 (12)
O2^i—O1—CS4^viii	156.32 (10)	O1^xiii—CS4—O2	74.16 (6)
O2^i—O1—CS4^iii	107.34 (6)	O1^xiii—CS4—O2^xx	103.08 (6)
O2^i—O1—CS4^v	59.73 (4)	O1^xiii—CS4—O2^xv	151.44 (4)
O2^i—O1—C5^i	12.89 (5)	O1^xiii—CS4—O2^xxi	46.60 (4)
O2^i—O1—C5^ii	141.97 (11)	O1^xiii—CS4—O3^xx	68.09 (5)
O2^i—O1—C5^ix	84.70 (5)	O1^xiii—CS4—O3^xiii	143.91 (5)
O2^i—O1—C5^xxii	115.31 (6)	O1^xiii—CS4—O3^xxi	73.17 (4)
O2^i—O1—C5^iii	106.83 (6)	O1^xiii—CS4—O3^xxiii	78.07 (4)
O2^i—O1—C5^v	104.09 (5)	O1^xiii—CS4—C5	61.16 (5)
O2^i—O1—H6^i	10.3 (4)	O1^xiii—CS4—C5^xx	87.80 (6)
O2^i—O1—H6^ii	121.1 (5)	O1^xiii—CS4—C5^xv	169.52 (4)
O2^ii—O1—O3^iii	112.80 (6)	O1^xiii—CS4—C5^xiii	161.79 (5)
O2^ii—O1—O3^iv	72.04 (7)	O1^xiii—CS4—C5^xxi	64.30 (4)
O2^ii—O1—O3^v	108.24 (6)	O1^xiii—CS4—C5^xxiv	63.27 (5)
O2^ii—O1—O3^vi	67.37 (7)	O1^xiii—CS4—H6	86.46 (14)
O2^ii—O1—CS4^vii	156.32 (10)	O1^xiii—CS4—H6^xx	115.95 (17)
O2^ii—O1—CS4^viii	72.28 (5)	O1^xiii—CS4—H6^xv	124.26 (12)
O2^ii—O1—CS4^iii	59.73 (4)	O1^xiii—CS4—H6^xxi	14.30 (11)
O2^ii—O1—CS4^v	107.34 (6)	O2—CS4—O2^xx	165.30 (7)
O2^ii—O1—C5^i	141.97 (11)	O2—CS4—O2^xv	96.88 (5)
O2^ii—O1—C5^ii	12.89 (5)	O2—CS4—O2^xxi	98.10 (5)
O2^ii—O1—C5^ix	115.31 (6)	O2—CS4—O3^xx	132.15 (5)
O2^ii—O1—C5^xxii	84.70 (5)	O2—CS4—O3^xiii	75.16 (5)
O2^ii—O1—C5^iii	104.09 (5)	O2—CS4—O3^xxi	79.16 (5)
O2^ii—O1—C5^v	106.83 (6)	O2—CS4—O3^xxiii	51.51 (5)
O2^ii—O1—H6^i	121.1 (5)	O2—CS4—C5	18.36 (5)
O2^ii—O1—H6^ii	10.3 (4)	O2—CS4—C5^xx	147.06 (6)
O3^iii—O1—O3^iv	115.47 (5)	O2—CS4—C5^xv	102.25 (5)
O3^iii—O1—O3^v	63.59 (7)	O2—CS4—C5^xiii	91.84 (5)
O3^iii—O1—O3^vi	179.06 (5)	O2—CS4—C5^xxi	95.22 (5)
O3^iii—O1—CS4^vii	50.31 (5)	O2—CS4—C5^xxiv	39.94 (5)
O3^iii—O1—CS4^viii	51.51 (5)	O2—CS4—H6	27.77 (11)
O3^iii—O1—CS4^iii	77.15 (4)	O2—CS4—H6^xx	162.20 (13)
O3^iii—O1—CS4^v	130.36 (7)	O2—CS4—H6^xv	101.41 (11)
O3^iii—O1—C5^i	102.33 (5)	O2—CS4—H6^xxi	83.57 (13)
O3^iii—O1—C5^ii	99.94 (5)	O2^xx—CS4—O2^xv	78.62 (5)
O3^iii—O1—C5^ix	35.60 (5)	O2^xx—CS4—O2^xxi	89.72 (5)
O3^iii—O1—C5^xxii	97.01 (8)	O2^xx—CS4—O3^xx	37.99 (5)
O3^iii—O1—C5^iii	18.36 (4)	O2^xx—CS4—O3^xiii	111.31 (5)
O3^iii—O1—C5^v	81.36 (7)	O2^xx—CS4—O3^xxi	114.25 (5)
O3^iii—O1—H6^i	117.4 (5)	O2^xx—CS4—O3^xxiii	113.85 (5)
O3^iii—O1—H6^ii	120.2 (5)	O2^xx—CS4—C5	148.82 (5)
O3^iv—O1—O3^v	179.06 (5)	O2^xx—CS4—C5^xx	19.97 (5)
O3^iv—O1—O3^vi	65.47 (7)	O2^xx—CS4—C5^xv	77.84 (4)
O3^iv—O1—CS4^vii	128.00 (3)	O2^xx—CS4—C5^xiii	93.36 (5)
O3^iv—O1—CS4^viii	129.22 (3)	O2^xx—CS4—C5^xxi	96.46 (5)
O3^iv—O1—CS4^iii	48.94 (4)	O2^xx—CS4—C5^xxiv	125.70 (5)
O3^iv—O1—CS4^v	103.66 (7)	O2^xx—CS4—H6	165.98 (12)
O3^iv—O1—C5^i	80.21 (6)	O2^xx—CS4—H6^xx	31.50 (12)
O3^iv—O1—C5^ii	77.76 (6)	O2^xx—CS4—H6^xv	67.81 (12)
O3^iv—O1—C5^ix	82.07 (5)	O2^xx—CS4—H6^xxi	96.76 (13)
O3^iv—O1—C5^xxii	145.27 (8)	O2^xv—CS4—O2^xxi	160.40 (6)
O3^iv—O1—C5^iii	97.70 (5)	O2^xv—CS4—O3^xx	102.33 (5)
O3^iv—O1—C5^v	162.54 (7)	O2^xv—CS4—O3^xiii	51.37 (5)
O3^iv—O1—H6^i	60.1 (5)	O2^xv—CS4—O3^xxi	132.76 (5)
O3^iv—O1—H6^ii	62.9 (5)	O2^xv—CS4—O3^xxiii	75.36 (5)
O3^v—O1—O3^vi	115.47 (5)	O2^xv—CS4—C5	102.68 (6)
O3^v—O1—CS4^vii	51.51 (5)	O2^xv—CS4—C5^xx	85.87 (5)
O3^v—O1—CS4^viii	50.31 (5)	O2^xv—CS4—C5^xv	18.12 (5)
O3^v—O1—CS4^iii	130.36 (7)	O2^xv—CS4—C5^xiii	39.73 (5)
O3^v—O1—CS4^v	77.15 (4)	O2^xv—CS4—C5^xxi	144.26 (6)
O3^v—O1—C5^i	99.94 (5)	O2^xv—CS4—C5^xxiv	92.22 (5)
O3^v—O1—C5^ii	102.33 (5)	O2^xv—CS4—H6	97.98 (14)
O3^v—O1—C5^ix	97.01 (8)	O2^xv—CS4—H6^xx	80.55 (17)
O3^v—O1—C5^xxii	35.60 (5)	O2^xv—CS4—H6^xv	29.58 (13)
O3^v—O1—C5^iii	81.36 (7)	O2^xv—CS4—H6^xxi	163.39 (13)
O3^v—O1—C5^v	18.36 (4)	O2^xxi—CS4—O3^xx	76.54 (5)
O3^v—O1—H6^i	120.2 (5)	O2^xxi—CS4—O3^xiii	121.32 (5)
O3^v—O1—H6^ii	117.4 (5)	O2^xxi—CS4—O3^xxi	39.66 (5)
O3^vi—O1—CS4^vii	129.22 (3)	O2^xxi—CS4—O3^xxiii	124.08 (5)
O3^vi—O1—CS4^viii	128.00 (3)	O2^xxi—CS4—C5	95.46 (5)
O3^vi—O1—CS4^iii	103.66 (7)	O2^xxi—CS4—C5^xx	88.39 (5)
O3^vi—O1—CS4^v	48.94 (4)	O2^xxi—CS4—C5^xv	143.71 (5)
O3^vi—O1—C5^i	77.76 (6)	O2^xxi—CS4—C5^xiii	126.99 (5)
O3^vi—O1—C5^ii	80.21 (6)	O2^xxi—CS4—C5^xxi	21.07 (5)
O3^vi—O1—C5^ix	145.27 (8)	O2^xxi—CS4—C5^xxiv	107.38 (5)
O3^vi—O1—C5^xxii	82.07 (5)	O2^xxi—CS4—H6	89.54 (13)
O3^vi—O1—C5^iii	162.54 (7)	O2^xxi—CS4—H6^xx	81.32 (17)
O3^vi—O1—C5^v	97.70 (5)	O2^xxi—CS4—H6^xv	154.21 (12)
O3^vi—O1—H6^i	62.9 (5)	O2^xxi—CS4—H6^xxi	32.72 (12)
O3^vi—O1—H6^ii	60.1 (5)	O3^xx—CS4—O3^xiii	147.93 (7)
CS4^vii—O1—CS4^viii	84.22 (7)	O3^xx—CS4—O3^xxi	115.10 (4)
CS4^vii—O1—CS4^iii	120.79 (4)	O3^xx—CS4—O3^xxiii	91.87 (5)
CS4^vii—O1—CS4^v	81.904 (18)	O3^xx—CS4—C5	113.82 (5)
CS4^vii—O1—C5^i	61.10 (3)	O3^xx—CS4—C5^xx	19.82 (5)
CS4^vii—O1—C5^ii	145.11 (8)	O3^xx—CS4—C5^xv	109.51 (5)
CS4^vii—O1—C5^ix	62.56 (5)	O3^xx—CS4—C5^xiii	129.73 (5)
CS4^vii—O1—C5^xxii	81.81 (6)	O3^xx—CS4—C5^xxi	93.97 (5)
CS4^vii—O1—C5^iii	64.22 (6)	O3^xx—CS4—C5^xxiv	95.48 (5)
CS4^vii—O1—C5^v	58.36 (5)	O3^xx—CS4—H6	154.15 (14)
CS4^vii—O1—H6^i	82.4 (4)	O3^xx—CS4—H6^xx	65.22 (14)
CS4^vii—O1—H6^ii	166.6 (5)	O3^xx—CS4—H6^xv	77.88 (12)
CS4^viii—O1—CS4^iii	81.904 (18)	O3^xx—CS4—H6^xxi	66.36 (13)
CS4^viii—O1—CS4^v	120.79 (4)	O3^xiii—CS4—O3^xxi	82.81 (5)
CS4^viii—O1—C5^i	145.11 (8)	O3^xiii—CS4—O3^xxiii	97.16 (4)
CS4^viii—O1—C5^ii	61.10 (3)	O3^xiii—CS4—C5	92.10 (5)
CS4^viii—O1—C5^ix	81.81 (6)	O3^xiii—CS4—C5^xx	128.14 (6)
CS4^viii—O1—C5^xxii	62.56 (5)	O3^xiii—CS4—C5^xv	39.77 (5)
CS4^viii—O1—C5^iii	58.36 (5)	O3^xiii—CS4—C5^xiii	18.23 (5)
CS4^viii—O1—C5^v	64.22 (6)	O3^xiii—CS4—C5^xxi	100.35 (6)
CS4^viii—O1—H6^i	166.6 (5)	O3^xiii—CS4—C5^xxiv	102.72 (5)
CS4^viii—O1—H6^ii	82.4 (4)	O3^xiii—CS4—H6	57.78 (14)
CS4^iii—O1—CS4^v	151.04 (9)	O3^xiii—CS4—H6^xx	89.87 (16)
CS4^iii—O1—C5^i	117.87 (5)	O3^xiii—CS4—H6^xv	80.26 (13)
CS4^iii—O1—C5^ii	54.48 (4)	O3^xiii—CS4—H6^xxi	143.24 (13)
CS4^iii—O1—C5^ix	58.58 (4)	O3^xxi—CS4—O3^xxiii	128.06 (2)
CS4^iii—O1—C5^xxii	136.43 (4)	O3^xxi—CS4—C5	88.07 (5)
CS4^iii—O1—C5^iii	59.55 (4)	O3^xxi—CS4—C5^xx	122.22 (5)
CS4^iii—O1—C5^v	146.12 (7)	O3^xxi—CS4—C5^xv	116.21 (5)
CS4^iii—O1—H6^i	103.9 (6)	O3^xxi—CS4—C5^xiii	93.06 (5)
CS4^iii—O1—H6^ii	58.4 (6)	O3^xxi—CS4—C5^xxi	21.27 (5)
CS4^v—O1—C5^i	54.48 (4)	O3^xxi—CS4—C5^xxiv	110.85 (5)
CS4^v—O1—C5^ii	117.87 (5)	O3^xxi—CS4—H6	58.28 (12)
CS4^v—O1—C5^ix	136.43 (4)	O3^xxi—CS4—H6^xx	89.63 (13)
CS4^v—O1—C5^xxii	58.58 (4)	O3^xxi—CS4—H6^xv	162.27 (13)
CS4^v—O1—C5^iii	146.12 (7)	O3^xxi—CS4—H6^xxi	63.73 (13)
CS4^v—O1—C5^v	59.55 (4)	O3^xxiv—CS4—C5	40.00 (5)
CS4^v—O1—H6^i	58.4 (6)	O3^xxiv—CS4—C5^xx	98.42 (5)
CS4^v—O1—H6^ii	103.9 (6)	O3^xxiv—CS4—C5^xv	91.96 (5)
C5^i—O1—C5^ii	153.74 (11)	O3^xxiv—CS4—C5^xiii	102.57 (5)
C5^i—O1—C5^ix	85.16 (5)	O3^xxiv—CS4—C5^xxi	136.22 (5)
C5^i—O1—C5^xxii	105.61 (6)	O3^xxiv—CS4—C5^xxiv	18.37 (5)
C5^i—O1—C5^iii	104.97 (6)	O3^xxiv—CS4—H6	77.88 (11)
C5^i—O1—C5^v	92.03 (4)	O3^xxiv—CS4—H6^xx	142.18 (13)
C5^i—O1—H6^i	21.9 (5)	O3^xxiv—CS4—H6^xv	59.89 (12)
C5^i—O1—H6^ii	132.1 (5)	O3^xxiv—CS4—H6^xxi	92.35 (12)
C5^ii—O1—C5^ix	105.61 (6)	C5—CS4—C5^xx	129.24 (7)
C5^ii—O1—C5^xxii	85.16 (5)	C5—CS4—C5^xv	112.83 (4)
C5^ii—O1—C5^iii	92.03 (4)	C5—CS4—C5^xiii	107.53 (5)
C5^ii—O1—C5^v	104.97 (6)	C5—CS4—C5^xxi	99.32 (5)
C5^ii—O1—H6^i	132.1 (5)	C5—CS4—C5^xxiv	24.27 (7)
C5^ii—O1—H6^ii	21.9 (5)	C5—CS4—H6	45.12 (12)
C5^ix—O1—C5^xxii	132.02 (11)	C5—CS4—H6^xx	176.76 (16)
C5^ix—O1—C5^iii	23.45 (7)	C5—CS4—H6^xv	97.76 (12)
C5^ix—O1—C5^v	113.05 (7)	C5—CS4—H6^xxi	73.00 (13)
C5^ix—O1—H6^i	90.9 (5)	C5^xx—CS4—C5^xv	90.51 (5)
C5^ix—O1—H6^ii	116.4 (6)	C5^xx—CS4—C5^xiii	109.92 (6)
C5^xxii—O1—C5^iii	113.05 (7)	C5^xx—CS4—C5^xxi	101.52 (5)
C5^xxii—O1—C5^v	23.45 (7)	C5^xx—CS4—C5^xxiv	107.32 (4)
C5^xxii—O1—H6^i	116.4 (6)	C5^xx—CS4—H6	173.72 (12)
C5^xxii—O1—H6^ii	90.9 (5)	C5^xx—CS4—H6^xx	50.65 (13)
C5^iii—O1—C5^v	99.41 (10)	C5^xx—CS4—H6^xv	66.13 (12)
C5^iii—O1—H6^i	113.9 (5)	C5^xx—CS4—H6^xxi	84.92 (13)
C5^iii—O1—H6^ii	109.1 (5)	C5^xv—CS4—C5^xiii	24.14 (6)
C5^v—O1—H6^i	109.1 (5)	C5^xv—CS4—C5^xxi	126.14 (7)
C5^v—O1—H6^ii	113.9 (5)	C5^xv—CS4—C5^xxiv	107.53 (6)
H6^i—O1—H6^ii	110.9 (9)	C5^xv—CS4—H6	94.67 (14)
O1^xi—O2—O2^xii	159.36 (12)	C5^xv—CS4—H6^xx	70.26 (17)
O1^xi—O2—O3	110.07 (10)	C5^xv—CS4—H6^xv	46.13 (13)
O1^xi—O2—O3^xiii	69.66 (7)	C5^xv—CS4—H6^xxi	174.13 (12)
O1^xi—O2—O3^xxiii	158.23 (9)	C5^xiii—CS4—C5^xxi	106.51 (5)
O1^xi—O2—CS4^xiv	59.10 (7)	C5^xiii—CS4—C5^xxiv	112.98 (4)
O1^xi—O2—CS4	106.77 (9)	C5^xiii—CS4—H6	76.01 (13)
O1^xi—O2—CS4^xv	95.38 (6)	C5^xiii—CS4—H6^xx	74.86 (16)
O1^xi—O2—CS4^xvi	73.67 (5)	C5^xiii—CS4—H6^xv	69.22 (13)
O1^xi—O2—C5	136.90 (17)	C5^xiii—CS4—H6^xxi	156.79 (13)
O1^xi—O2—C5^xxiv	169.18 (12)	C5^xxi—CS4—C5^xxiv	117.88 (5)
O1^xi—O2—H6	5.3 (2)	C5^xxi—CS4—H6	78.26 (13)
O1^xi—O2—H6^xvii	13.96 (12)	C5^xxi—CS4—H6^xx	77.79 (15)
O2^xxiii—O2—O3	50.64 (7)	C5^xxi—CS4—H6^xv	162.88 (11)
O2^xxiii—O2—O3^xiii	129.70 (9)	C5^xxi—CS4—H6^xxi	51.66 (13)
O2^xxiii—O2—O3^xxiii	39.40 (6)	C5^xxiv—CS4—H6	67.70 (10)
O2^xxiv—O2—CS4^xiv	100.87 (8)	C5^xxiv—CS4—H6^xx	156.95 (12)
O2^xxiv—O2—CS4	92.75 (8)	C5^xxiv—CS4—H6^xv	78.23 (12)
O2^xxiv—O2—CS4^xv	93.53 (8)	C5^xxiv—CS4—H6^xxi	77.43 (12)
O2^xxiv—O2—CS4^xvi	100.37 (8)	H6—CS4—H6^xx	134.8 (2)
O2^xxiv—O2—C5	23.44 (12)	H6—CS4—H6^xv	115.36 (11)
O2^xxiv—O2—C5^xxiv	11.88 (6)	H6—CS4—H6^xxi	90.1 (2)
O2^xxiv—O2—H6	164.0 (3)	H6^xx—CS4—H6^xv	85.11 (19)
O2^xxiv—O2—H6^xvii	171.90 (17)	H6^xx—CS4—H6^xxi	103.93 (19)
O3—O2—O3^xiii	179.4294 (11)	H6^xv—CS4—H6^xxi	134.0 (2)
O3—O2—O3^xxiii	90.04 (10)	O1^xi—C5—O1^ix	94.84 (5)
O3—O2—CS4^xiv	60.56 (7)	O1^xi—C5—O1^xiii	104.97 (6)
O3—O2—CS4	127.19 (10)	O1^xi—C5—O2	30.22 (13)
O3—O2—CS4^xv	128.24 (10)	O1^xi—C5—O2^xii	171.79 (10)
O3—O2—CS4^xvi	66.61 (7)	O1^xi—C5—O3	95.95 (14)
O3—O2—C5	27.20 (12)	O1^xi—C5—O3^xxiii	119.27 (10)
O3—O2—C5^xxiv	62.52 (10)	O1^xi—C5—CS4^xiv	51.20 (5)
O3—O2—H6	113.8 (3)	O1^xi—C5—CS4	78.25 (7)
O3—O2—H6^xvii	121.28 (16)	O1^xi—C5—CS4^xv	70.91 (5)
O3^xiii—O2—O3^xxiii	90.30 (7)	O1^xi—C5—CS4^iii	132.44 (6)
O3^xiii—O2—CS4^xiv	119.49 (6)	O1^xi—C5—CS4^xvi	61.22 (4)
O3^xiii—O2—CS4	52.62 (4)	O1^xi—C5—CS4^xxiv	123.61 (7)
O3^xiii—O2—CS4^xv	52.33 (4)	O1^xi—C5—C5^xxiv	146.5 (2)
O3^xiii—O2—CS4^xvi	112.82 (6)	O1^xi—C5—H6	6.98 (14)
O3^xiii—O2—C5	153.14 (17)	O1^ix—C5—O1^xiii	156.55 (7)
O3^xiii—O2—C5^xxiv	117.83 (9)	O1^ix—C5—O2	92.88 (16)
O3^xiii—O2—H6	65.9 (3)	O1^ix—C5—O2^xii	78.10 (7)
O3^xiii—O2—H6^xvii	58.37 (14)	O1^ix—C5—O3	101.20 (15)
O3^xxiv—O2—CS4^xiv	130.34 (8)	O1^ix—C5—O3^xxiii	73.68 (8)
O3^xxiv—O2—CS4	64.27 (6)	O1^ix—C5—CS4^xiv	71.28 (6)
O3^xxiv—O2—CS4^xv	64.62 (6)	O1^ix—C5—CS4	114.35 (7)
O3^xxiv—O2—CS4^xvi	123.97 (8)	O1^ix—C5—CS4^xv	49.66 (4)
O3^xxiv—O2—C5	62.84 (15)	O1^ix—C5—CS4^iii	122.03 (6)
O3^xxiv—O2—C5^xxiv	27.53 (6)	O1^ix—C5—CS4^xvi	150.90 (8)
O3^xxiv—O2—H6	155.7 (3)	O1^ix—C5—CS4^xxiv	58.14 (4)
O3^xxiv—O2—H6^xvii	148.67 (16)	O1^ix—C5—C5^xxiv	73.93 (16)
CS4^xiv—O2—CS4	165.30 (7)	O1^ix—C5—H6	96.57 (18)
CS4^xiv—O2—CS4^xv	101.38 (5)	O1^xiii—C5—O2	97.95 (15)
CS4^xiv—O2—CS4^xvi	82.43 (4)	O1^xiii—C5—O2^xii	81.08 (7)
CS4^xiv—O2—C5	81.96 (14)	O1^xiii—C5—O3	89.28 (15)
CS4^xiv—O2—C5^xxiv	110.26 (9)	O1^xiii—C5—O3^xxiii	85.58 (7)
CS4^xiv—O2—H6	64.3 (2)	O1^xiii—C5—CS4^xiv	131.31 (7)
CS4^xiv—O2—H6^xvii	73.06 (12)	O1^xiii—C5—CS4	59.29 (4)
CS4—O2—CS4^xv	83.12 (5)	O1^xiii—C5—CS4^xv	125.68 (7)
CS4—O2—CS4^xvi	89.74 (5)	O1^xiii—C5—CS4^iii	50.52 (4)
CS4—O2—C5	109.74 (15)	O1^xiii—C5—CS4^xvi	52.55 (4)
CS4—O2—C5^xxiv	83.98 (8)	O1^xiii—C5—CS4^xxiv	117.11 (7)
CS4—O2—H6	101.5 (2)	O1^xiii—C5—C5^xxiv	82.62 (16)
CS4—O2—H6^xvii	92.84 (13)	O1^xiii—C5—H6	101.68 (17)
CS4^xv—O2—CS4^xvi	164.67 (8)	O2—C5—O2^xii	144.69 (17)
CS4^xv—O2—C5	110.88 (17)	O2—C5—O3	125.7 (2)
CS4^xv—O2—C5^xxiv	84.55 (7)	O2—C5—O3^xxiii	89.74 (17)
CS4^xv—O2—H6	95.3 (3)	O2—C5—CS4^xiv	78.07 (14)
CS4^xv—O2—H6^xvii	92.96 (17)	O2—C5—CS4	51.91 (13)
CS4^xvi—O2—C5	84.28 (15)	O2—C5—CS4^xv	51.00 (14)
CS4^xvi—O2—C5^xxiv	108.25 (9)	O2—C5—CS4^iii	145.07 (17)
CS4^xvi—O2—H6	72.8 (3)	O2—C5—CS4^xvi	74.65 (15)
CS4^xvi—O2—H6^xvii	73.80 (16)	O2—C5—CS4^xxiv	143.95 (16)
C5—O2—C5^xxiv	35.31 (17)	O2—C5—C5^xxiv	117.3 (3)
C5—O2—H6	140.9 (3)	O2—C5—H6	23.6 (2)
C5—O2—H6^xvii	148.5 (2)	O2^xxiii—C5—O3	89.60 (16)
C5^xxiv—O2—H6	174.4 (2)	O2^xxiii—C5—O3^xxiii	54.94 (8)
C5^xxiv—O2—H6^xvii	176.16 (16)	O2^xxiv—C5—CS4^xiv	128.58 (10)
H6—O2—H6^xvii	8.81 (15)	O2^xxiv—C5—CS4	100.68 (8)
O1^xviii—O3—O1^xiii	115.47 (5)	O2^xxiv—C5—CS4^xv	101.10 (8)
O1^xviii—O3—O2	137.30 (9)	O2^xxiv—C5—CS4^iii	55.73 (7)
O1^xviii—O3—O2^iii	42.97 (4)	O2^xxiv—C5—CS4^xvi	126.75 (9)
O1^xviii—O3—O2^xii	132.06 (7)	O2^xxiv—C5—CS4^xxiv	56.08 (7)
O1^xviii—O3—O3^xxiii	169.65 (9)	O2^xxiv—C5—C5^xxiv	27.36 (14)
O1^xviii—O3—CS4^xiv	62.97 (4)	O2^xxiv—C5—H6	167.9 (2)
O1^xviii—O3—CS4^iii	85.01 (5)	O3—C5—O3^xxiii	144.54 (17)
O1^xviii—O3—CS4^xvi	84.15 (4)	O3—C5—CS4^xiv	58.43 (12)
O1^xviii—O3—CS4^xxiv	77.00 (4)	O3—C5—CS4	144.27 (16)
O1^xviii—O3—C5	163.61 (15)	O3—C5—CS4^xv	144.44 (16)
O1^xviii—O3—C5^xxiv	158.85 (9)	O3—C5—CS4^iii	51.51 (12)
O1^xviii—O3—H6	107.44 (13)	O3—C5—CS4^xvi	67.89 (13)
O1^xviii—O3—H6^iii	13.81 (11)	O3—C5—CS4^xxiv	51.71 (13)
O1^xviii—O3—H6^xvi	14.00 (11)	O3—C5—C5^xxiv	117.0 (3)
O1^xiii—O3—O2	78.47 (8)	O3—C5—H6	102.2 (2)
O1^xiii—O3—O2^iii	101.87 (6)	O3^xxiv—C5—CS4^xiv	142.08 (10)
O1^xiii—O3—O2^xii	74.35 (6)	O3^xxiv—C5—CS4	56.25 (6)
O1^xiii—O3—O3^xxiii	70.42 (6)	O3^xxiv—C5—CS4^xv	56.24 (7)
O1^xiii—O3—CS4^xiv	142.37 (6)	O3^xxiv—C5—CS4^iii	100.62 (8)
O1^xiii—O3—CS4^iii	52.24 (3)	O3^xxiv—C5—CS4^xvi	131.07 (9)
O1^xiii—O3—CS4^xvi	51.97 (3)	O3^xxiv—C5—CS4^xxiv	100.49 (8)
O1^xiii—O3—CS4^xxiv	129.23 (5)	O3^xxiv—C5—C5^xxiv	27.58 (13)
O1^xiii—O3—C5	72.36 (14)	O3^xxiv—C5—H6	113.21 (19)
O1^xiii—O3—C5^xxiv	70.73 (7)	CS4^xiv—C5—CS4	129.24 (7)
O1^xiii—O3—H6	89.90 (14)	CS4^xiv—C5—CS4^xv	89.49 (5)
O1^xiii—O3—H6^iii	110.48 (15)	CS4^xiv—C5—CS4^iii	109.92 (6)
O1^xiii—O3—H6^xvi	109.49 (14)	CS4^xiv—C5—CS4^xvi	80.36 (5)
O2—O3—O2^iii	179.4287 (11)	CS4^xiv—C5—CS4^xxiv	72.68 (4)
O2—O3—O2^xii	89.96 (10)	CS4^xiv—C5—C5^xxiv	142.58 (19)
O2—O3—O3^xxiii	50.59 (7)	CS4^xiv—C5—H6	57.98 (14)
O2—O3—CS4^xiv	81.44 (8)	CS4—C5—CS4^xv	67.17 (4)
O2—O3—CS4^iii	127.97 (9)	CS4—C5—CS4^iii	107.53 (5)
O2—O3—CS4^xvi	73.73 (7)	CS4—C5—CS4^xvi	78.80 (5)
O2—O3—CS4^xxiv	127.12 (9)	CS4—C5—CS4^xxiv	155.73 (7)
O2—O3—C5	27.09 (13)	CS4—C5—C5^xxiv	78.13 (16)
O2—O3—C5^xxiv	62.54 (10)	CS4—C5—H6	71.36 (15)
O2—O3—H6	29.93 (14)	CS4^xv—C5—CS4^iii	155.86 (6)
O2—O3—H6^iii	150.95 (14)	CS4^xv—C5—CS4^xvi	125.60 (7)
O2—O3—H6^xvi	125.18 (15)	CS4^xv—C5—CS4^xxiv	107.53 (6)
O2^iii—O3—O2^xii	89.70 (7)	CS4^xv—C5—C5^xxiv	78.20 (18)
O2^iii—O3—O3^xxiii	129.07 (8)	CS4^xv—C5—H6	67.59 (19)
O2^iii—O3—CS4^xiv	98.51 (6)	CS4^iii—C5—CS4^xvi	73.46 (5)
O2^iii—O3—CS4^iii	52.22 (4)	CS4^iii—C5—CS4^xxiv	67.02 (4)
O2^iii—O3—CS4^xvi	106.84 (6)	CS4^iii—C5—C5^xxiv	77.66 (18)
O2^iii—O3—CS4^xxiv	52.31 (4)	CS4^iii—C5—H6	134.74 (19)
O2^iii—O3—C5	152.57 (16)	CS4^xvi—C5—CS4^xxiv	119.46 (7)
O2^iii—O3—C5^xxiv	117.11 (9)	CS4^xvi—C5—C5^xxiv	135.17 (19)
O2^iii—O3—H6	150.37 (14)	CS4^xvi—C5—H6	61.79 (18)
O2^iii—O3—H6^iii	29.35 (12)	CS4^xxiv—C5—C5^xxiv	77.60 (17)
O2^iii—O3—H6^xvi	55.17 (12)	CS4^xxiv—C5—H6	130.10 (15)
O2^xxiii—O3—O3^xxiii	39.37 (6)	C5^xxiv—C5—H6	140.7 (3)
O2^xxiv—O3—CS4^xiv	137.26 (8)	O1^xi—H6—O2	164.5 (6)
O2^xxiv—O3—CS4^iii	64.01 (5)	O1^xi—H6—O2^xvii	44.9 (4)
O2^xxiv—O3—CS4^xvi	125.73 (8)	O1^xi—H6—O3	131.7 (6)
O2^xxiv—O3—CS4^xxiv	64.22 (6)	O1^xi—H6—O3^xiii	106.1 (6)
O2^xxiv—O3—C5	62.87 (14)	O1^xi—H6—O3^xxi	103.0 (5)
O2^xxiv—O3—C5^xxiv	27.41 (7)	O1^xi—H6—CS4^xiv	80.4 (4)
O2^xxiv—O3—H6	119.78 (14)	O1^xi—H6—CS4	144.8 (5)
O2^xxiv—O3—H6^iii	118.94 (13)	O1^xi—H6—CS4^xv	123.7 (6)
O2^xxiv—O3—H6^xvi	144.87 (14)	O1^xi—H6—CS4^xvi	107.3 (6)
O3^xxiv—O3—CS4^xiv	118.23 (8)	O1^xi—H6—C5	151.1 (6)
O3^xxiv—O3—CS4^iii	92.96 (7)	O1^xi—H6—H6^xvii	34.5 (4)
O3^xxiv—O3—CS4^xvi	105.87 (8)	O2—H6—O2^xvii	150.5 (3)
O3^xxiv—O3—CS4^xxiv	92.68 (7)	O2—H6—O3	36.26 (17)
O3^xxiv—O3—C5	23.50 (11)	O2—H6—O3^xiii	84.8 (3)
O3^xxiv—O3—C5^xxiv	11.96 (6)	O2—H6—O3^xxi	90.6 (3)
O3^xxiv—O3—H6	80.44 (14)	O2—H6—CS4^xiv	84.2 (3)
O3^xxiv—O3—H6^iii	158.19 (14)	O2—H6—CS4	50.70 (18)
O3^xxiv—O3—H6^xvi	175.76 (14)	O2—H6—CS4^xv	55.1 (2)
CS4^xiv—O3—CS4^iii	147.93 (7)	O2—H6—CS4^xvi	74.5 (3)
CS4^xiv—O3—CS4^xvi	91.92 (5)	O2—H6—C5	15.46 (13)
CS4^xiv—O3—CS4^xxiv	88.13 (5)	O2—H6—H6^xvii	160.7 (3)
CS4^xiv—O3—C5	101.75 (14)	O2^xvii—H6—O3	159.7 (3)
CS4^xiv—O3—C5^xxiv	125.61 (9)	O2^xvii—H6—O3^xiii	71.27 (16)
CS4^xiv—O3—H6	58.63 (12)	O2^xvii—H6—O3^xxi	66.46 (14)
CS4^xiv—O3—H6^iii	75.14 (13)	O2^xvii—H6—CS4^xiv	125.3 (2)
CS4^xiv—O3—H6^xvi	59.11 (15)	O2^xvii—H6—CS4	99.84 (18)
CS4^iii—O3—CS4^xvi	85.96 (5)	O2^xvii—H6—CS4^xv	115.2 (3)
CS4^iii—O3—CS4^xxiv	82.84 (4)	O2^xvii—H6—CS4^xvi	103.6 (2)
CS4^iii—O3—C5	110.26 (15)	O2^xvii—H6—C5	161.7 (3)
CS4^iii—O3—C5^xxiv	83.99 (7)	O2^xvii—H6—H6^xvii	10.45 (14)
CS4^iii—O3—H6	141.01 (15)	O3—H6—O3^xiii	121.0 (2)
CS4^iii—O3—H6^iii	72.87 (13)	O3—H6—O3^xxi	100.2 (2)
CS4^iii—O3—H6^xvi	90.17 (15)	O3—H6—CS4^xiv	56.14 (13)
CS4^xvi—O3—CS4^xxiv	158.79 (7)	O3—H6—CS4	80.74 (14)
CS4^xvi—O3—C5	90.84 (14)	O3—H6—CS4^xv	83.58 (15)
CS4^xvi—O3—C5^xxiv	112.96 (8)	O3—H6—CS4^xvi	56.48 (15)
CS4^xvi—O3—H6	59.79 (15)	O3—H6—C5	20.84 (8)
CS4^xvi—O3—H6^iii	89.94 (13)	O3—H6—H6^xvii	158.2 (7)
CS4^xvi—O3—H6^xvi	71.49 (12)	O3^xiii—H6—O3^xxi	73.08 (15)
CS4^xxiv—O3—C5	109.92 (15)	O3^xiii—H6—CS4^xiv	142.9 (3)
CS4^xxiv—O3—C5^xxiv	83.74 (7)	O3^xiii—H6—CS4	49.35 (10)
CS4^xxiv—O3—H6	135.49 (16)	O3^xiii—H6—CS4^xv	50.54 (12)
CS4^xxiv—O3—H6^iii	69.57 (13)	O3^xiii—H6—CS4^xvi	122.4 (2)
CS4^xxiv—O3—H6^xvi	90.54 (11)	O3^xiii—H6—C5	100.2 (2)
C5—O3—C5^xxiv	35.46 (17)	O3^xiii—H6—H6^xvii	78.6 (4)
C5—O3—H6	56.97 (17)	O3^xxi—H6—CS4^xiv	142.3 (3)
C5—O3—H6^iii	176.8 (2)	O3^xxi—H6—CS4	50.23 (10)
C5—O3—H6^xvi	152.3 (2)	O3^xxi—H6—CS4^xv	112.53 (19)
C5^xxiv—O3—H6	92.39 (15)	O3^xxi—H6—CS4^xvi	54.53 (14)
C5^xxiv—O3—H6^iii	146.29 (15)	O3^xxi—H6—C5	95.7 (2)
C5^xxiv—O3—H6^xvi	172.28 (14)	O3^xxi—H6—H6^xvii	75.3 (4)
H6—O3—H6^iii	121.0 (2)	CS4^xiv—H6—CS4	134.8 (2)
H6—O3—H6^xvi	95.33 (18)	CS4^xiv—H6—CS4^xv	94.89 (19)
H6^iii—O3—H6^xvi	26.0 (2)	CS4^xiv—H6—CS4^xvi	88.3 (2)
O1^xix—CS4—O1^xiii	120.79 (4)	CS4^xiv—H6—C5	71.36 (16)
O1^xix—CS4—O2	145.23 (6)	CS4^xiv—H6—H6^xvii	114.96 (12)
O1^xix—CS4—O2^xx	48.62 (5)	CS4—H6—CS4^xv	64.64 (11)
O1^xix—CS4—O2^xv	82.12 (4)	CS4—H6—CS4^xvi	77.29 (15)
O1^xix—CS4—O2^xxi	78.36 (4)	CS4—H6—C5	63.51 (13)
O1^xix—CS4—O3^xx	81.20 (5)	CS4—H6—H6^xvii	110.24 (10)
O1^xix—CS4—O3^xiii	77.45 (4)	CS4^xv—H6—CS4^xvi	128.7 (2)
O1^xix—CS4—O3^xxi	76.53 (4)	CS4^xv—H6—C5	66.28 (14)
O1^xix—CS4—O3^xxiii	154.46 (4)	CS4^xv—H6—H6^xvii	118.0 (7)
O1^xix—CS4—C5	162.26 (5)	CS4^xvi—H6—C5	66.55 (19)
O1^xix—CS4—C5^xx	67.70 (5)	CS4^xvi—H6—H6^xvii	106.4 (7)
O1^xix—CS4—C5^xv	67.78 (4)	C5—H6—H6^xvii	171.0 (6)
O1^xix—CS4—C5^xiii	65.26 (4)

Symmetry codes: (i) x−1, y, z; (ii) −x+1, y, −z+1/2; (iii) x−1/2, y−1/2, z; (iv) x−1/2, y+1/2, z; (v) −x+1/2, y−1/2, −z+1/2; (vi) −x+1/2, y+1/2, −z+1/2; (vii) x−1, y−1, z; (viii) −x+1, y−1, −z+1/2; (ix) −x+1, −y−1, −z+1; (x) x−1, −y−1, z−1/2; (xi) x+1, y, z; (xii) −x+1/2, −y−3/2, −z+1; (xiii) x+1/2, y+1/2, z; (xiv) x, y−1, z; (xv) −x+2, −y, −z+1; (xvi) −x+3/2, y−1/2, −z+1/2; (xvii) −x+2, y, −z+1/2; (xviii) x+1/2, y−1/2, z; (xix) x+1, y+1, z; (xx) x, y+1, z; (xxi) −x+3/2, y+1/2, −z+1/2; (xxii) x−1, −y−1, z+1/2; (xxiii) −x+1/2, −y−3/2, −z; (xxiv) −x+3/2, −y−1/2, −z+1.