Tri(L-isoleucinium) sulfate bi­sulfate

The title compound, 3C₆H₁₄NO₂⁺·HSO₄⁻·SO₄²⁻, comprises three cationic isoleucinium mol­ecules, and sulfate and bi­sulfate anions (1:1). The mol­ecules are held together by strong N—H...O and O—H...O hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.010 Å
• R factor = 0.047
• wR factor = 0.125
• Data-to-parameter ratio = 11.1

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes



REFLT_03
         From the CIF: _diffrn_reflns_theta_max           24.97
         From the CIF: _reflns_number_total               3764
         Count of symmetry unique reflns         2909
         Completeness (_total/calc)            129.39%
         TEST3: Check Friedels for noncentro structure
         Estimate of Friedel pairs measured       855
         Fraction of Friedel pairs measured     0.294
         Are heavy atom types Z>Si present          yes
          WARNING: Large fraction of Friedel related reflns may
                   be needed to determine absolute structure

---

Computing details

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: CAD-4 Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: PLATON (Spek, 1999); software used to prepare material for publication: SHELXL97.

'Tri (L-Isoleucinium) sulfate bisulfate'

Crystal data

3C6H14NO2^+·HSO4^−·SO4^2^−	Dx = 1.354 Mg m^−3 Dm = 1.35 Mg m^−3 Dm measured by flotation measured
Mr = 589.67	Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, P212121	Cell parameters from 25 reflections
a = 6.743 (5) Å	θ = 9.9–14.1°
b = 19.418 (5) Å	µ = 0.25 mm^−1
c = 22.095 (5) Å	T = 293 K
V = 2893 (2) Å^3	Needles, colorless
Z = 4	0.33 × 0.13 × 0.10 mm
F(000) = 1264

Data collection

Enraf-Nonius sealed tube diffractometer	1902 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.035
Graphite monochromator	θmax = 25.0°, θmin = 1.8°
ω–2θ scans	h = −1→8
Absorption correction: ψ scan (North et al., 1968)	k = −2→23
Tmin = 0.945, Tmax = 0.970	l = −2→26
4192 measured reflections	3 standard reflections every 60 reflections
3764 independent reflections	intensity decay: none

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)] = 0.047	H-atom parameters constrained
wR(F^2) = 0.125	w = 1/[σ^2(Fo^2) + (0.0508P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.99	(Δ/σ)max = 0.001
3764 reflections	Δρmax = 0.29 e Å^−3
339 parameters	Δρmin = −0.29 e Å^−3
0 restraints	Absolute structure: (Flack, 1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.15 (15)

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
S1	0.0559 (3)	0.89357 (9)	0.32327 (8)	0.0354 (5)
O1	0.2169 (7)	0.9427 (2)	0.3217 (2)	0.0497 (14)
O2	0.1063 (7)	0.8393 (2)	0.3715 (2)	0.0479 (14)
H2	0.2163	0.8231	0.3646	0.072*
O3	−0.1263 (7)	0.9233 (2)	0.3450 (2)	0.0421 (13)
O4	0.0321 (9)	0.8594 (2)	0.2659 (2)	0.0542 (15)
S2	0.5194 (3)	0.74344 (8)	0.33020 (7)	0.0333 (4)
O5	0.5541 (8)	0.7659 (2)	0.26814 (19)	0.0511 (14)
O6	0.4630 (7)	0.8041 (2)	0.36764 (19)	0.0402 (12)
O7	0.7028 (7)	0.7151 (3)	0.3554 (2)	0.0493 (14)
O8	0.3596 (7)	0.6933 (2)	0.3336 (2)	0.0457 (14)
O11	−0.1544 (9)	0.5779 (2)	0.1668 (2)	0.0597 (16)
H11	−0.1823	0.5380	0.1753	0.090*
O12	−0.0097 (9)	0.5792 (2)	0.2575 (2)	0.0583 (16)
C11	−0.0729 (11)	0.6080 (4)	0.2140 (3)	0.0385 (18)
C12	−0.0571 (12)	0.6839 (3)	0.2037 (3)	0.0394 (18)
H12	−0.1897	0.7011	0.1937	0.047*
N1	0.0038 (9)	0.7155 (2)	0.2625 (2)	0.0377 (15)
H1A	0.0134	0.7609	0.2581	0.057*
H1B	0.1206	0.6985	0.2737	0.057*
H1C	−0.0866	0.7059	0.2906	0.057*
C13	0.0833 (11)	0.7060 (3)	0.1532 (3)	0.0406 (19)
H13	0.1036	0.7558	0.1575	0.049*
C14	0.2880 (12)	0.6717 (4)	0.1593 (3)	0.062 (3)
H14A	0.3373	0.6784	0.1996	0.093*
H14B	0.3782	0.6920	0.1308	0.093*
H14C	0.2761	0.6233	0.1512	0.093*
C15	−0.0046 (12)	0.6940 (4)	0.0903 (3)	0.051 (2)
H15A	−0.0017	0.6451	0.0817	0.061*
H15B	−0.1423	0.7084	0.0906	0.061*
C16	0.1025 (15)	0.7320 (5)	0.0400 (4)	0.089 (3)
H16A	0.0380	0.7228	0.0021	0.133*
H16B	0.2376	0.7165	0.0380	0.133*
H16C	0.0998	0.7805	0.0479	0.133*
O21	0.6398 (9)	1.0582 (2)	0.1579 (2)	0.0508 (15)
H21	0.6233	1.0996	0.1634	0.076*
O22	0.5173 (10)	1.0487 (2)	0.2517 (2)	0.0575 (16)
C21	0.5887 (11)	1.0239 (3)	0.2076 (4)	0.0383 (19)
C22	0.6394 (11)	0.9489 (3)	0.2016 (3)	0.0329 (17)
H22	0.7844	0.9459	0.2015	0.039*
N2	0.5699 (8)	0.9128 (2)	0.2578 (2)	0.0346 (14)
H2A	0.6009	0.8683	0.2555	0.052*
H2B	0.4391	0.9173	0.2612	0.052*
H2C	0.6286	0.9313	0.2900	0.052*
C23	0.5679 (13)	0.9133 (3)	0.1433 (3)	0.044 (2)
H23	0.6040	0.9434	0.1094	0.053*
C24	0.6759 (16)	0.8457 (4)	0.1342 (4)	0.077 (3)
H24A	0.8164	0.8535	0.1355	0.116*
H24B	0.6404	0.8266	0.0956	0.116*
H24C	0.6392	0.8141	0.1657	0.116*
C25	0.3447 (13)	0.9025 (4)	0.1402 (4)	0.064 (3)
H25A	0.3153	0.8758	0.1042	0.077*
H25B	0.3053	0.8750	0.1749	0.077*
C26	0.2197 (13)	0.9661 (5)	0.1391 (4)	0.083 (3)
H26A	0.0821	0.9534	0.1381	0.125*
H26B	0.2513	0.9928	0.1038	0.125*
H26C	0.2454	0.9929	0.1748	0.125*
O31	0.4458 (9)	0.8625 (2)	0.5848 (2)	0.0584 (15)
H31	0.3516	0.8398	0.5971	0.088*
O32	0.4624 (9)	0.7802 (2)	0.5148 (2)	0.0642 (17)
C31	0.5196 (12)	0.8334 (3)	0.5367 (3)	0.0383 (18)
C32	0.7003 (11)	0.8715 (3)	0.5125 (3)	0.0359 (18)
H32	0.8103	0.8634	0.5406	0.043*
N3	0.7516 (8)	0.8378 (3)	0.4536 (2)	0.0371 (16)
H3A	0.8560	0.8589	0.4373	0.056*
H3B	0.6488	0.8408	0.4285	0.056*
H3C	0.7805	0.7937	0.4600	0.056*
C33	0.6718 (12)	0.9484 (4)	0.5070 (3)	0.045 (2)
H33	0.6315	0.9650	0.5471	0.054*
C34	0.8693 (13)	0.9842 (4)	0.4919 (3)	0.072 (3)
H34A	0.8481	1.0330	0.4886	0.109*
H34B	0.9195	0.9668	0.4543	0.109*
H34C	0.9635	0.9753	0.5235	0.109*
C35	0.5080 (14)	0.9683 (3)	0.4635 (3)	0.059 (2)
H35A	0.3921	0.9405	0.4725	0.071*
H35B	0.5502	0.9569	0.4228	0.071*
C36	0.4481 (18)	1.0436 (4)	0.4650 (4)	0.105 (4)
H36A	0.3374	1.0508	0.4384	0.158*
H36B	0.5576	1.0716	0.4521	0.158*
H36C	0.4113	1.0562	0.5055	0.158*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.0348 (11)	0.0339 (9)	0.0374 (10)	0.0011 (10)	0.0040 (10)	0.0014 (9)
O1	0.039 (3)	0.036 (3)	0.075 (4)	0.001 (3)	0.012 (3)	0.003 (3)
O2	0.036 (3)	0.054 (3)	0.053 (3)	0.012 (3)	0.013 (3)	0.021 (3)
O3	0.024 (3)	0.057 (3)	0.045 (3)	0.011 (3)	0.002 (3)	−0.006 (3)
O4	0.076 (4)	0.046 (3)	0.041 (3)	−0.001 (3)	0.007 (3)	−0.010 (2)
S2	0.0322 (11)	0.0321 (9)	0.0356 (9)	0.0047 (9)	−0.0061 (10)	0.0017 (8)
O5	0.068 (4)	0.048 (3)	0.037 (3)	0.004 (3)	−0.008 (3)	0.006 (2)
O6	0.034 (3)	0.041 (3)	0.046 (3)	0.005 (3)	−0.010 (3)	−0.013 (2)
O7	0.036 (3)	0.058 (3)	0.054 (3)	0.014 (3)	−0.012 (3)	0.008 (3)
O8	0.032 (3)	0.032 (3)	0.074 (4)	−0.002 (2)	−0.002 (3)	−0.001 (3)
O11	0.079 (4)	0.043 (3)	0.057 (3)	−0.019 (3)	−0.008 (4)	0.001 (3)
O12	0.067 (4)	0.044 (3)	0.064 (3)	−0.006 (3)	−0.012 (4)	0.017 (3)
C11	0.040 (5)	0.040 (4)	0.036 (4)	−0.009 (4)	−0.001 (4)	−0.008 (4)
C12	0.042 (5)	0.039 (4)	0.037 (4)	−0.008 (4)	−0.003 (4)	−0.004 (3)
N1	0.043 (4)	0.034 (3)	0.036 (3)	0.002 (3)	0.007 (3)	0.001 (2)
C13	0.049 (5)	0.036 (4)	0.036 (4)	0.001 (4)	0.002 (4)	−0.003 (3)
C14	0.043 (5)	0.090 (7)	0.054 (6)	−0.012 (5)	0.007 (5)	−0.002 (5)
C15	0.053 (5)	0.060 (5)	0.038 (4)	−0.005 (5)	−0.011 (5)	−0.004 (4)
C16	0.095 (8)	0.121 (8)	0.050 (5)	−0.009 (8)	−0.001 (6)	0.012 (6)
O21	0.068 (4)	0.033 (3)	0.051 (3)	−0.010 (3)	0.006 (3)	0.007 (3)
O22	0.078 (4)	0.039 (3)	0.056 (3)	−0.006 (3)	0.011 (4)	−0.012 (2)
C21	0.038 (5)	0.031 (4)	0.046 (5)	−0.006 (4)	−0.002 (4)	−0.003 (4)
C22	0.033 (4)	0.042 (4)	0.024 (4)	−0.002 (4)	0.004 (4)	0.009 (3)
N2	0.036 (4)	0.035 (3)	0.032 (3)	0.002 (3)	0.000 (3)	0.000 (2)
C23	0.057 (6)	0.036 (4)	0.040 (4)	0.004 (4)	0.005 (4)	0.006 (4)
C24	0.133 (9)	0.050 (5)	0.049 (5)	0.022 (6)	−0.003 (6)	−0.003 (4)
C25	0.083 (7)	0.066 (6)	0.044 (5)	−0.014 (6)	−0.010 (5)	0.002 (5)
C26	0.048 (6)	0.108 (8)	0.094 (7)	−0.007 (6)	0.010 (6)	−0.015 (7)
O31	0.068 (4)	0.054 (3)	0.053 (3)	−0.014 (3)	0.033 (3)	−0.002 (3)
O32	0.078 (4)	0.058 (3)	0.057 (3)	−0.033 (4)	0.021 (4)	−0.006 (3)
C31	0.046 (5)	0.040 (4)	0.030 (4)	−0.003 (5)	0.009 (4)	0.011 (3)
C32	0.035 (4)	0.046 (4)	0.026 (4)	−0.006 (4)	0.000 (4)	−0.002 (3)
N3	0.034 (4)	0.039 (4)	0.039 (4)	−0.002 (3)	0.003 (3)	−0.004 (3)
C33	0.063 (6)	0.036 (4)	0.036 (4)	−0.003 (4)	0.006 (5)	0.001 (4)
C34	0.082 (7)	0.073 (6)	0.063 (6)	−0.040 (6)	0.024 (6)	−0.023 (5)
C35	0.073 (6)	0.049 (5)	0.056 (5)	0.013 (5)	0.001 (6)	0.001 (4)
C36	0.153 (12)	0.067 (6)	0.096 (7)	0.029 (8)	−0.003 (9)	0.019 (5)

Geometric parameters (Å, º)

S1—O4	1.439 (4)	N2—H2A	0.8900
S1—O3	1.439 (5)	N2—H2B	0.8900
S1—O1	1.446 (5)	N2—H2C	0.8900
S1—O2	1.537 (5)	C23—C24	1.515 (10)
O2—H2	0.8200	C23—C25	1.521 (11)
S2—O8	1.454 (5)	C23—H23	0.9800
S2—O5	1.458 (5)	C24—H24A	0.9600
S2—O7	1.464 (5)	C24—H24B	0.9600
S2—O6	1.489 (4)	C24—H24C	0.9600
O11—C11	1.316 (7)	C25—C26	1.495 (11)
O11—H11	0.8200	C25—H25A	0.9700
O12—C11	1.191 (7)	C25—H25B	0.9700
C11—C12	1.495 (9)	C26—H26A	0.9600
C12—N1	1.494 (7)	C26—H26B	0.9600
C12—C13	1.526 (9)	C26—H26C	0.9600
C12—H12	0.9800	O31—C31	1.303 (7)
N1—H1A	0.8900	O31—H31	0.8200
N1—H1B	0.8900	O32—C31	1.203 (8)
N1—H1C	0.8900	C31—C32	1.523 (10)
C13—C15	1.528 (9)	C32—N3	1.496 (7)
C13—C14	1.539 (10)	C32—C33	1.511 (9)
C13—H13	0.9800	C32—H32	0.9800
C14—H14A	0.9600	N3—H3A	0.8900
C14—H14B	0.9600	N3—H3B	0.8900
C14—H14C	0.9600	N3—H3C	0.8900
C15—C16	1.517 (10)	C33—C35	1.514 (10)
C15—H15A	0.9700	C33—C34	1.538 (11)
C15—H15B	0.9700	C33—H33	0.9800
C16—H16A	0.9600	C34—H34A	0.9600
C16—H16B	0.9600	C34—H34B	0.9600
C16—H16C	0.9600	C34—H34C	0.9600
O21—C21	1.330 (8)	C35—C36	1.519 (10)
O21—H21	0.8200	C35—H35A	0.9700
O22—C21	1.190 (8)	C35—H35B	0.9700
C21—C22	1.502 (9)	C36—H36A	0.9600
C22—N2	1.501 (7)	C36—H36B	0.9600
C22—C23	1.539 (9)	C36—H36C	0.9600
C22—H22	0.9800
O4—S1—O3	112.5 (3)	H2A—N2—H2C	109.5
O4—S1—O1	111.5 (3)	H2B—N2—H2C	109.5
O3—S1—O1	112.6 (3)	C24—C23—C25	110.5 (7)
O4—S1—O2	108.6 (3)	C24—C23—C22	110.5 (7)
O3—S1—O2	103.5 (3)	C25—C23—C22	114.2 (7)
O1—S1—O2	107.7 (3)	C24—C23—H23	107.1
S1—O2—H2	109.5	C25—C23—H23	107.1
O8—S2—O5	111.5 (3)	C22—C23—H23	107.1
O8—S2—O7	110.8 (3)	C23—C24—H24A	109.5
O5—S2—O7	109.6 (3)	C23—C24—H24B	109.5
O8—S2—O6	108.1 (3)	H24A—C24—H24B	109.5
O5—S2—O6	109.1 (3)	C23—C24—H24C	109.5
O7—S2—O6	107.6 (3)	H24A—C24—H24C	109.5
C11—O11—H11	109.5	H24B—C24—H24C	109.5
O12—C11—O11	125.5 (7)	C26—C25—C23	116.4 (7)
O12—C11—C12	124.1 (6)	C26—C25—H25A	108.2
O11—C11—C12	110.3 (6)	C23—C25—H25A	108.2
N1—C12—C11	107.0 (5)	C26—C25—H25B	108.2
N1—C12—C13	110.5 (6)	C23—C25—H25B	108.2
C11—C12—C13	115.7 (6)	H25A—C25—H25B	107.3
N1—C12—H12	107.8	C25—C26—H26A	109.5
C11—C12—H12	107.8	C25—C26—H26B	109.5
C13—C12—H12	107.8	H26A—C26—H26B	109.5
C12—N1—H1A	109.5	C25—C26—H26C	109.5
C12—N1—H1B	109.5	H26A—C26—H26C	109.5
H1A—N1—H1B	109.5	H26B—C26—H26C	109.5
C12—N1—H1C	109.5	C31—O31—H31	109.5
H1A—N1—H1C	109.5	O32—C31—O31	125.3 (7)
H1B—N1—H1C	109.5	O32—C31—C32	122.2 (7)
C12—C13—C15	112.4 (6)	O31—C31—C32	112.4 (6)
C12—C13—C14	111.7 (6)	N3—C32—C33	113.1 (6)
C15—C13—C14	111.2 (6)	N3—C32—C31	106.1 (5)
C12—C13—H13	107.0	C33—C32—C31	114.0 (6)
C15—C13—H13	107.0	N3—C32—H32	107.8
C14—C13—H13	107.0	C33—C32—H32	107.8
C13—C14—H14A	109.5	C31—C32—H32	107.8
C13—C14—H14B	109.5	C32—N3—H3A	109.5
H14A—C14—H14B	109.5	C32—N3—H3B	109.5
C13—C14—H14C	109.5	H3A—N3—H3B	109.5
H14A—C14—H14C	109.5	C32—N3—H3C	109.5
H14B—C14—H14C	109.5	H3A—N3—H3C	109.5
C16—C15—C13	114.1 (6)	H3B—N3—H3C	109.5
C16—C15—H15A	108.7	C32—C33—C35	113.3 (6)
C13—C15—H15A	108.7	C32—C33—C34	110.7 (7)
C16—C15—H15B	108.7	C35—C33—C34	112.3 (6)
C13—C15—H15B	108.7	C32—C33—H33	106.7
H15A—C15—H15B	107.6	C35—C33—H33	106.7
C15—C16—H16A	109.5	C34—C33—H33	106.7
C15—C16—H16B	109.5	C33—C34—H34A	109.5
H16A—C16—H16B	109.5	C33—C34—H34B	109.5
C15—C16—H16C	109.5	H34A—C34—H34B	109.5
H16A—C16—H16C	109.5	C33—C34—H34C	109.5
H16B—C16—H16C	109.5	H34A—C34—H34C	109.5
C21—O21—H21	109.5	H34B—C34—H34C	109.5
O22—C21—O21	125.3 (6)	C33—C35—C36	115.2 (7)
O22—C21—C22	123.9 (7)	C33—C35—H35A	108.5
O21—C21—C22	110.7 (6)	C36—C35—H35A	108.5
N2—C22—C21	108.0 (6)	C33—C35—H35B	108.5
N2—C22—C23	112.7 (5)	C36—C35—H35B	108.5
C21—C22—C23	116.0 (6)	H35A—C35—H35B	107.5
N2—C22—H22	106.6	C35—C36—H36A	109.5
C21—C22—H22	106.6	C35—C36—H36B	109.5
C23—C22—H22	106.6	H36A—C36—H36B	109.5
C22—N2—H2A	109.5	C35—C36—H36C	109.5
C22—N2—H2B	109.5	H36A—C36—H36C	109.5
H2A—N2—H2B	109.5	H36B—C36—H36C	109.5
C22—N2—H2C	109.5
O12—C11—C12—N1	−13.4 (11)	C21—C22—C23—C24	163.7 (7)
O11—C11—C12—N1	170.6 (6)	N2—C22—C23—C25	54.1 (8)
O12—C11—C12—C13	110.2 (8)	C21—C22—C23—C25	−71.1 (9)
O11—C11—C12—C13	−65.8 (9)	C24—C23—C25—C26	−171.1 (7)
N1—C12—C13—C15	−162.5 (5)	C22—C23—C25—C26	63.7 (10)
C11—C12—C13—C15	75.8 (8)	O32—C31—C32—N3	11.1 (9)
N1—C12—C13—C14	71.7 (7)	O31—C31—C32—N3	−172.9 (6)
C11—C12—C13—C14	−50.1 (9)	O32—C31—C32—C33	136.2 (7)
C12—C13—C15—C16	164.5 (7)	O31—C31—C32—C33	−47.7 (8)
C14—C13—C15—C16	−69.4 (8)	N3—C32—C33—C35	59.7 (9)
O22—C21—C22—N2	4.3 (10)	C31—C32—C33—C35	−61.7 (8)
O21—C21—C22—N2	−177.5 (5)	N3—C32—C33—C34	−67.5 (8)
O22—C21—C22—C23	131.8 (8)	C31—C32—C33—C34	171.1 (6)
O21—C21—C22—C23	−50.0 (9)	C32—C33—C35—C36	169.3 (8)
N2—C22—C23—C24	−71.1 (8)	C34—C33—C35—C36	−64.4 (10)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O6	0.82	1.71	2.502 (7)	163
O11—H11···O1^i	0.82	1.87	2.671 (6)	167
N1—H1A···O4	0.89	1.92	2.802 (6)	169
N1—H1B···O8	0.89	2.09	2.900 (8)	152
N1—H1C···O7^ii	0.89	2.02	2.887 (7)	163
O21—H21···O8^iii	0.82	1.83	2.631 (6)	167
N2—H2A···O5	0.89	2.03	2.864 (6)	155
N2—H2B···O1	0.89	2.07	2.828 (7)	143
N2—H2C···O3^iv	0.89	2.06	2.819 (7)	143
O31—H31···O7^v	0.82	1.80	2.588 (7)	161
N3—H3A···O2^iv	0.89	2.26	3.002 (7)	141
N3—H3A···O3^iv	0.89	2.40	3.033 (7)	129
N3—H3B···O6	0.89	1.97	2.797 (7)	154
N3—H3C···O32^vi	0.89	1.97	2.786 (7)	152

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