Glycine zinc sulfate penta­hydrate: redetermination at 10 K from time-of-flight neutron Laue diffraction

We report a redetermination based on single-crystal neutron diffraction data and Raman spectra for glycine zinc sulfate penta­hydrate.

Key indicators

• Single-crystal neutron study
• T = 10 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.089
• wR factor = 0.246
• Data-to-parameter ratio = 28.5

checkCIF/PLATON results

No syntax errors found



Alert level A
TYPE031_ALERT_1_A  _diffrn_radiation_wavelength is not of type numb.

Author Response: Data was collected with polychromatic neutrons wavelength is given as a range rather than a number.

CELL004_ALERT_1_A  _cell_measurement_theta_min is missing
            Minimum theta of reflections used to measure unit cell.
            The following tests will not be performed.
            CELLT_01

Author Response: Test not relevant for polychromatic radiation, see _exptl_special_details.

CELL005_ALERT_1_A  _cell_measurement_theta_max is missing
            Maximum theta of reflections used to measure unit cell.
            The following tests will not be performed.
            CELLT_01

Author Response: Test not relevant for polychromatic radiation, see _exptl_special_details.

TYPE036_ALERT_1_A  _exptl_absorpt_coefficient_mu is not of type numb.

Author Response: Data was collected with polychromatic neutrons and so the absorption, being wavelength dependent, is given as a an expression rather than a number.

PLAT184_ALERT_1_A Missing _cell_measurement_theta_min value ......     Please Do !

Author Response: Test not relevant for polychromatic neutrons, see _exptl_special_details for further information.

PLAT185_ALERT_1_A Missing _cell_measurement_theta_max value ......     Please Do !

Author Response: Test not relevant for polychromatic neutrons, see _exptl_special_details for further information.

Alert level B
DIFMN02_ALERT_2_B  The minimum difference density is < -0.1*ZMAX*1.00
            _refine_diff_density_min given =     -3.470
            Test value =     -3.000

Author Response: Value is in Fermi per cubic angstrom; test not relevant for polychromatic neutrons.

DIFMX01_ALERT_2_B  The maximum difference density is > 0.1*ZMAX*1.00
            _refine_diff_density_max given =      3.197
            Test value =      3.000

Author Response: Value is in Fermi per cubic angstrom; test not relevant for polychromatic neutrons.

Alert level C
CELLK01_ALERT_1_C  Check that the cell measurement temperature is in Kelvin.
            Value of measurement temperature given =    10.000

Author Response: The measurement was made at 10 Kelvin.

DIFMN03_ALERT_1_C  The minimum difference density is < -0.1*ZMAX*0.75
            The relevant atom site should be identified.

Author Response: Value is in Fermi per cubic angstrom; test not relevant for polychromatic neutrons.

DIFMX02_ALERT_1_C  The maximum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.

Author Response: Value is in Fermi per cubic angstrom; test not relevant for polychromatic neutrons.

PLAT480_ALERT_4_C Long H...A H-Bond Reported H2A    ..  O2      ..       2.68 Ang.

Author Response: This is expected for a weak C-H...O bond, as discussed in the main text.

PLAT480_ALERT_4_C Long H...A H-Bond Reported H2A    ..  O5      ..       2.72 Ang.

Author Response: This is expected for a weak C-H...O bond, as discussed in the main text.

PLAT918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) .          4 Check

Author Response: Examination of the SHELX .LST file reveals that F(obs)^2^ and F(calc)^2^ for these reflections, (3 5 1), (1 -2 -2), (2 0 6) and ( 0 2 3) differ by between 5 and 8 times the measurement ESD, which is within the limit of acceptability for SXD data.

PLAT977_ALERT_2_C Check the Negative Difference Density on     H2B      -0.66 eA-3

Author Response: Test not relevant for polychromatic neutrons.

PLAT977_ALERT_2_C Check the Negative Difference Density on     H2N      -1.06 eA-3

Author Response: Test not relevant for polychromatic neutrons.

PLAT977_ALERT_2_C Check the Negative Difference Density on     H3N      -0.49 eA-3

Author Response: Test not relevant for polychromatic neutrons.

PLAT977_ALERT_2_C Check the Negative Difference Density on     H9A      -0.74 eA-3

Author Response: Test not relevant for polychromatic neutrons.

PLAT977_ALERT_2_C Check the Negative Difference Density on    H10B      -0.54 eA-3

Author Response: Test not relevant for polychromatic neutrons.

PLAT977_ALERT_2_C Check the Negative Difference Density on    H11B      -0.90 eA-3

Author Response: Test not relevant for polychromatic neutrons.

PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density           0 Note

Author Response: Test not relevant for polychromatic neutrons.

Alert level G
ABSMU01_ALERT_1_G  Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          2 Report

Author Response: Light restraint applied to Uij of the zinc atoms using the SHELX ISOR command as described in the main text.

PLAT072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.14 Report

Author Response: Test not relevant for polychromatic neutrons.

PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      36.25 Why ?

Author Response: Test not relevant for polychromatic neutrons.

PLAT164_ALERT_4_G Nr. of Refined C-H H-Atoms in Heavy-Atom Struct.          2 Note

Author Response: This is entirely appropriate for a single crystal neutron refinement.

PLAT186_ALERT_4_G The CIF-Embedded .res File Contains ISOR Records          1 Report

Author Response: Light restraints applied to Uij of both zinc atoms using the SHELX ISOR command as described in the main text.

PLAT794_ALERT_5_G Tentative Bond Valency for Zn2     (II)    .....       2.12 Note

Author Response: Noted. The Zn-O bond lengths in both coordination polyhedra are normal.

PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         12 Note

Author Response: These correspond to the twelve lightly-restrained Uij of the zinc atoms.

PLAT871_ALERT_4_G Laue technique Related ALERTS are Suppressed ...          ! Info
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600      17744 Note
PLAT933_ALERT_2_G Number of OMIT records in Embedded RES .........         11 Note

Author Response: Outlying reflections were omitted; these typically occur near the edges of detectors and are thus poorly measured/integrated.

PLAT958_ALERT_1_G Calculated (ThMax) and Actual (FCF) Lmax Differ           7 Units
PLAT961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check

   6 ALERT level A = Most likely a serious problem - resolve or explain
   2 ALERT level B = A potentially serious problem, consider carefully
  13 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  13 ALERT level G = General information/check it is not something unexpected

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

---

Computing details

Data collection: SXD2001 (Gutmann, 2005); cell refinement: SXD2001 (Gutmann, 2005); data reduction: SXD2001 (Gutmann, 2005); program(s) used to solve structure: SHELXT2014 (Sheldrick, 2015a; Gruene et al., 2014); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b; Gruene et al., 2014); molecular graphics: DIAMOND (Putz & Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Hexaaquazinc(II) tetraaquadiglycinezinc(II) bis(sulfate)

Crystal data

[Zn(H2O)6][Zn(C2H5NO2)2(H2O)4](SO4)2	Z = 1
Mr = 653.20	F(000) = 336
Triclinic, P1	Dx = 2.086 Mg m^−3
a = 5.9601 (15) Å	Neutron radiation, λ = 0.48-7.0 Å
b = 6.7670 (17) Å	Cell parameters from 550 reflections
c = 13.112 (4) Å	µ = 5.02 + 0.0182 * λ mm^−1
α = 84.955 (18)°	T = 10 K
β = 83.25 (2)°	Tabular, colourless
γ = 83.042 (19)°	4 × 2.5 × 1 mm
V = 519.8 (2) Å^3

Data collection

SXD diffractometer	8296 reflections with I > 2σ(I)
Radiation source: ISIS neutron spallation source	Rint = 0.089
time–of–flight LAUE diffraction scans	θmax = 87.4°, θmin = 8.2°
Absorption correction: numerical The linear absorption coefficient is wavelength dependent and is calculated as: µ = 5.0165 + 0.0182 * λ [cm^-1] as determined by Gaussian integration in SXD2001 (Gutmann, 2005)	h = −15→15
	k = −18→16
8296 measured reflections	l = −28→29
8296 independent reflections

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.089	w = 1/[σ^2(Fo^2) + (0.1376P)^2 + 36.2519P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.246	(Δ/σ)max < 0.001
S = 1.09	Δρmax = 3.20 e Å^−3
8296 reflections	Δρmin = −3.47 e Å^−3
291 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
12 restraints	Extinction coefficient: 0.0386 (18)

Special details

Experimental. For peak integration a local UB matrix refined for each frame, using approximately 50 reflections from each of the 11 detectors. Hence _cell_measurement_reflns_used 550 For final cell dimensions a weighted average of all local cells was calculated Because of the nature of the experiment, it is not possible to give values of theta_min and theta_max for the cell determination. The same applies for the wavelength used for the experiment. The range of wavelengths used was 0.48–7.0 Angstroms, BUT the bulk of the diffraction information is obtained from wavelengths in the range 0.7–2.5 Angstroms. The data collection procedures on the SXD instrument used for the single-crystal neutron data collection are most recently summarized in the Appendix to the following paper Wilson, C.C. (1997). J. Mol. Struct. 405, 207–217

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

Refinement. The variable wavelength nature of the data collection procedure means that sensible values of _diffrn_reflns_theta_min & _diffrn_reflns_theta_max cannot be given instead the following limits are given _diffrn_reflns_sin(theta)/lambda_min 0.06 _diffrn_reflns_sin(theta)/lambda_max 1.38 _refine_diff_density_max/min is given in Fermi per angstrom cubed not electons per angstrom cubed. Another way to consider the _refine_diff_density_ is as a percentage of the scattering density of a given atom: _refine_diff_density_max = 5.7 % of hydrogen _refine_diff_density_min = -6.1 % of hydrogen 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	0.0141 (6)	0.9128 (6)	0.1847 (4)	0.0008 (6)
O1	0.1809 (4)	1.0196 (3)	0.1159 (2)	0.0036 (4)
O2	−0.0249 (4)	0.7303 (3)	0.1375 (2)	0.0037 (4)
O3	−0.2027 (4)	1.0416 (3)	0.2010 (2)	0.0040 (4)
O4	0.1050 (4)	0.8522 (4)	0.2845 (2)	0.0038 (3)
Zn1	0.5000	0.0000	0.5000	0.0017 (4)
O5	0.1954 (4)	0.1618 (4)	0.5392 (2)	0.0049 (4)
H5A	0.0913 (11)	0.1389 (11)	0.6009 (6)	0.0198 (11)
H5B	0.0998 (10)	0.2109 (9)	0.4826 (6)	0.0170 (10)
O6	0.4360 (4)	0.0464 (4)	0.3456 (2)	0.0043 (4)
H6A	0.5654 (10)	0.0305 (9)	0.2922 (5)	0.0162 (10)
H6B	0.3082 (10)	−0.0116 (10)	0.3229 (6)	0.0179 (11)
O7	0.6512 (4)	0.2793 (4)	0.4768 (2)	0.0037 (3)
O8	0.9812 (4)	0.3195 (4)	0.3809 (2)	0.0060 (4)
N1	0.3991 (2)	0.5025 (2)	0.34432 (14)	0.0044 (2)
H1N	0.3634 (11)	0.5559 (12)	0.4165 (6)	0.0218 (13)
H2N	0.3159 (12)	0.6073 (10)	0.2963 (7)	0.0212 (12)
H3N	0.3294 (11)	0.3719 (9)	0.3435 (6)	0.0199 (12)
C1	0.7711 (3)	0.3465 (3)	0.39746 (19)	0.0029 (3)
C2	0.6484 (3)	0.4781 (3)	0.3163 (2)	0.0041 (3)
H2A	0.7111 (11)	0.6233 (9)	0.3086 (7)	0.0220 (13)
H2B	0.6871 (11)	0.4134 (12)	0.2420 (6)	0.0222 (13)
Zn2	0.5000	0.5000	0.0000	0.0008 (3)
O9	0.2958 (4)	0.3897 (3)	0.1320 (2)	0.0045 (4)
H9A	0.2434 (11)	0.2593 (8)	0.1279 (6)	0.0175 (11)
H9B	0.1606 (10)	0.4824 (9)	0.1443 (6)	0.0190 (11)
O10	0.7911 (4)	0.3443 (4)	0.0509 (2)	0.0048 (4)
H10A	0.7828 (12)	0.2322 (9)	0.1030 (6)	0.0180 (10)
H10B	0.8989 (11)	0.2959 (10)	−0.0061 (6)	0.0197 (11)
O11	0.5434 (4)	0.7298 (4)	0.0881 (2)	0.0054 (4)
H11A	0.6938 (9)	0.7484 (9)	0.1036 (6)	0.0182 (11)
H11B	0.4422 (10)	0.8523 (8)	0.0915 (7)	0.0200 (12)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.0006 (10)	0.0009 (11)	0.0010 (18)	0.0001 (8)	−0.0003 (9)	0.0000 (11)
O1	0.0027 (6)	0.0037 (7)	0.0038 (10)	−0.0006 (5)	0.0016 (5)	0.0001 (7)
O2	0.0029 (6)	0.0028 (6)	0.0058 (11)	−0.0007 (5)	−0.0007 (6)	−0.0012 (7)
O3	0.0017 (6)	0.0040 (7)	0.0053 (11)	0.0018 (5)	0.0010 (6)	0.0000 (7)
O4	0.0039 (6)	0.0054 (7)	0.0018 (10)	0.0001 (5)	−0.0015 (6)	0.0011 (7)
Zn1	0.0015 (4)	0.0017 (4)	0.0017 (5)	−0.0001 (3)	−0.0001 (3)	0.0000 (3)
O5	0.0036 (7)	0.0071 (8)	0.0032 (11)	0.0014 (5)	−0.0002 (6)	0.0011 (7)
H5A	0.015 (2)	0.028 (3)	0.014 (3)	−0.0027 (18)	0.0046 (18)	0.002 (2)
H5B	0.015 (2)	0.019 (2)	0.016 (3)	0.0017 (15)	−0.0065 (17)	0.004 (2)
O6	0.0041 (7)	0.0064 (7)	0.0021 (11)	−0.0005 (5)	−0.0004 (6)	0.0002 (7)
H6A	0.0142 (18)	0.021 (2)	0.013 (3)	−0.0020 (15)	0.0034 (16)	−0.005 (2)
H6B	0.017 (2)	0.023 (2)	0.017 (3)	−0.0076 (17)	−0.0052 (18)	−0.005 (2)
O7	0.0042 (6)	0.0041 (7)	0.0026 (10)	−0.0011 (5)	−0.0004 (6)	0.0014 (7)
O8	0.0028 (7)	0.0091 (9)	0.0050 (12)	0.0008 (5)	0.0001 (6)	0.0022 (8)
N1	0.0030 (4)	0.0057 (5)	0.0041 (7)	0.0012 (3)	−0.0013 (4)	0.0004 (5)
H1N	0.017 (2)	0.033 (3)	0.015 (3)	0.002 (2)	0.0004 (19)	−0.009 (3)
H2N	0.019 (2)	0.020 (2)	0.025 (4)	0.0015 (18)	−0.011 (2)	0.006 (2)
H3N	0.018 (2)	0.015 (2)	0.027 (4)	−0.0066 (16)	−0.001 (2)	0.001 (2)
C1	0.0020 (5)	0.0034 (6)	0.0032 (9)	0.0000 (4)	−0.0011 (5)	0.0007 (6)
C2	0.0042 (6)	0.0047 (6)	0.0030 (9)	−0.0002 (4)	−0.0004 (5)	0.0017 (6)
H2A	0.020 (2)	0.013 (2)	0.033 (4)	−0.0078 (17)	−0.005 (2)	0.007 (2)
H2B	0.018 (2)	0.035 (3)	0.013 (3)	0.007 (2)	−0.0031 (19)	−0.006 (3)
Zn2	0.0008 (4)	0.0008 (4)	0.0009 (5)	−0.0001 (3)	−0.0001 (3)	0.0001 (3)
O9	0.0045 (7)	0.0035 (7)	0.0050 (11)	−0.0005 (5)	0.0005 (6)	0.0004 (7)
H9A	0.021 (2)	0.0115 (17)	0.021 (3)	−0.0064 (15)	−0.001 (2)	−0.001 (2)
H9B	0.0135 (19)	0.016 (2)	0.024 (4)	0.0064 (14)	0.0009 (18)	−0.001 (2)
O10	0.0039 (7)	0.0047 (7)	0.0050 (11)	0.0019 (5)	−0.0012 (6)	0.0010 (7)
H10A	0.024 (3)	0.015 (2)	0.013 (3)	0.0011 (17)	0.0002 (19)	0.0054 (19)
H10B	0.020 (2)	0.020 (2)	0.016 (3)	0.0065 (17)	0.0040 (19)	−0.002 (2)
O11	0.0033 (6)	0.0048 (7)	0.0086 (12)	0.0002 (5)	−0.0015 (6)	−0.0033 (8)
H11A	0.0091 (16)	0.022 (2)	0.025 (3)	−0.0030 (15)	−0.0057 (17)	−0.004 (2)
H11B	0.017 (2)	0.0118 (18)	0.031 (4)	0.0059 (14)	−0.003 (2)	−0.006 (2)

Geometric parameters (Å, º)

S1—O3	1.473 (4)	N1—H1N	1.033 (7)
S1—O1	1.474 (5)	N1—C2	1.481 (2)
S1—O4	1.480 (6)	C1—C2	1.523 (4)
S1—O2	1.484 (4)	C2—H2A	1.085 (6)
Zn1—O5	2.039 (2)	C2—H2B	1.091 (7)
Zn1—O5^i	2.039 (2)	Zn2—O10	2.067 (3)
Zn1—O6	2.093 (3)	Zn2—O10^ii	2.067 (3)
Zn1—O6^i	2.094 (3)	Zn2—O11^ii	2.075 (2)
Zn1—O7^i	2.173 (2)	Zn2—O11	2.075 (2)
Zn1—O7	2.173 (2)	Zn2—O9	2.129 (3)
O5—H5A	0.973 (7)	Zn2—O9^ii	2.129 (3)
O5—H5B	0.997 (7)	O9—H9B	0.966 (6)
O6—H6A	0.981 (6)	O9—H9A	0.979 (5)
O6—H6B	0.985 (6)	O10—H10A	0.977 (8)
O7—C1	1.272 (4)	O10—H10B	0.979 (6)
O8—C1	1.240 (3)	O11—H11B	0.966 (6)
N1—H3N	1.022 (6)	O11—H11A	0.966 (6)
N1—H2N	1.027 (8)
O3—S1—O1	110.2 (3)	O8—C1—O7	126.0 (3)
O3—S1—O4	110.1 (3)	O8—C1—C2	116.2 (2)
O1—S1—O4	109.5 (3)	O7—C1—C2	117.7 (2)
O3—S1—O2	109.3 (3)	H2A—C2—H2B	107.9 (7)
O1—S1—O2	109.3 (3)	H2A—C2—N1	109.5 (4)
O4—S1—O2	108.4 (3)	H2B—C2—N1	109.5 (4)
O5—Zn1—O5^i	180.0	H2A—C2—C1	108.5 (5)
O5—Zn1—O6	88.59 (11)	H2B—C2—C1	109.7 (4)
O5^i—Zn1—O6	91.41 (11)	O10—Zn2—O10^ii	180.0
O5—Zn1—O6^i	91.41 (11)	O10—Zn2—O11^ii	91.57 (10)
O5^i—Zn1—O6^i	88.59 (11)	O10^ii—Zn2—O11^ii	88.43 (10)
O6—Zn1—O6^i	180.0	O10—Zn2—O11	88.43 (10)
O5—Zn1—O7^i	92.01 (9)	O10^ii—Zn2—O11	91.57 (10)
O5^i—Zn1—O7^i	87.99 (9)	O11^ii—Zn2—O11	180.0
O6—Zn1—O7^i	93.38 (10)	O10—Zn2—O9	91.52 (11)
O6^i—Zn1—O7^i	86.62 (10)	O10^ii—Zn2—O9	88.48 (11)
O5—Zn1—O7	87.99 (9)	O11^ii—Zn2—O9	94.16 (10)
O5^i—Zn1—O7	92.01 (9)	O11—Zn2—O9	85.84 (10)
O6—Zn1—O7	86.62 (10)	O10—Zn2—O9^ii	88.48 (11)
O6^i—Zn1—O7	93.38 (10)	O10^ii—Zn2—O9^ii	91.52 (11)
O7^i—Zn1—O7	180.0	O11^ii—Zn2—O9^ii	85.84 (10)
H5A—O5—H5B	106.7 (6)	O11—Zn2—O9^ii	94.16 (10)
H6A—O6—H6B	108.1 (6)	O9—Zn2—O9^ii	180.00 (12)
C1—O7—Zn1	128.26 (18)	H9B—O9—H9A	106.2 (6)
H3N—N1—H2N	107.6 (6)	H10A—O10—H10B	106.1 (6)
H3N—N1—H1N	109.8 (7)	H11B—O11—H11A	111.4 (6)
H2N—N1—H1N	105.0 (6)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O4^iii	0.973 (7)	1.793 (7)	2.755 (4)	169.0 (7)
O5—H5B···O8^iv	0.997 (7)	1.656 (8)	2.642 (4)	168.9 (6)
O6—H6A···O3^v	0.981 (6)	1.722 (6)	2.696 (3)	170.8 (5)
O6—H6B···O4^vi	0.985 (6)	1.751 (5)	2.729 (3)	171.8 (7)
O9—H9A···O1^vi	0.979 (5)	1.732 (5)	2.707 (3)	173.8 (6)
O9—H9B···O2	0.966 (6)	1.895 (6)	2.811 (3)	157.2 (6)
O10—H10A···O3^v	0.977 (8)	1.740 (8)	2.713 (4)	173.0 (7)
O10—H10B···O2^ii	0.979 (6)	1.811 (7)	2.745 (4)	158.5 (7)
O11—H11A···O2^vii	0.966 (6)	1.772 (6)	2.726 (3)	168.6 (6)
O11—H11B···O1	0.966 (6)	1.824 (6)	2.750 (3)	159.5 (7)
C2—H2A···O2^vii	1.085 (6)	2.682 (9)	3.351 (4)	119.4 (6)
C2—H2A···O5^viii	1.085 (6)	2.716 (8)	3.489 (3)	127.9 (6)
C2—H2B···O10	1.091 (7)	2.579 (8)	3.649 (4)	166.7 (7)
N1—H1N···O7^viii	1.033 (7)	1.853 (7)	2.848 (3)	160.8 (7)
N1—H2N···O4	1.027 (8)	1.961 (7)	2.877 (3)	147.0 (7)
N1—H3N···O6	1.022 (6)	2.216 (7)	3.066 (3)	139.5 (5)

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