The asymmetric unit of the compound (NH
4)
7(HPO
4)
2(PO
4) consists of two hydrogen phosphate anions, one phosphate anion and seven ammonium cations, all of them located in general positions. The two [PO
3(OH)]
2− anions are linked to the PO
43− anion
via an O—H
O hydrogen bond to form a three-anion unit, which is surrounded by the ammonium cations. The anions and cations are further connected
via N—H
O hydrogen bonding.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (P-O) = 0.002 Å
- R factor = 0.031
- wR factor = 0.084
- Data-to-parameter ratio = 12.5
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.92
Alert level C
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.95 Ratio
PLAT731_ALERT_1_C Bond Calc 0.89(4), Rep 0.891(19) ...... 2.11 su-Rat
N2 -H24 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.86(4), Rep 0.866(19) ...... 2.11 su-Rat
N6 -H64 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.89(4), Rep 0.891(19) ...... 2.11 su-Rat
N2 -H24 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(4), Rep 0.866(19) ...... 2.11 su-Rat
N6 -H64 1.555 1.555
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4
H4 N
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5
H4 N
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 6
H4 N
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7
H4 N
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 10
H4 N
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 28.13
From the CIF: _reflns_number_total 4004
Count of symmetry unique reflns 2401
Completeness (_total/calc) 166.76%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 1603
Fraction of Friedel pairs measured 0.668
Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
12 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
Data collection: IPDS (Stoe & Cie, 1996); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: CIF-Editor (Wieczorrek, 2004).
heptaammonium bis(hydrogenphosphate) phosphate
top
Crystal data top
(NH4)7(HPO4)2(PO4) | F(000) = 440 |
Mr = 413.22 | Dx = 1.523 Mg m−3 |
Monoclinic, P21 | Melting point: unknown K |
Hall symbol: P 2yb | Mo Kα radiation, λ = 0.71073 Å |
a = 10.4667 (17) Å | Cell parameters from 1206 reflections |
b = 6.2976 (7) Å | θ = 1.9–28.2° |
c = 14.072 (2) Å | µ = 0.39 mm−1 |
β = 103.738 (19)° | T = 293 K |
V = 901.0 (2) Å3 | Column, colourless |
Z = 2 | 0.5 × 0.25 × 0.25 mm |
Data collection top
Stoe IPDS I diffractometer | 4004 independent reflections |
Radiation source: fine-focus sealed tube | 3538 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
Detector resolution: not measured pixels mm-1 | θmax = 28.1°, θmin = 2.8° |
φ scans | h = −13→13 |
Absorption correction: numerical The absorption correction (X-RED; Stoe & Cie, 2001) was performed after
optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999). | k = −7→7 |
Tmin = 0.902, Tmax = 0.962 | l = −18→18 |
8608 measured reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.031 | w = 1/[σ2(Fo2) + (0.0526P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.084 | (Δ/σ)max = 0.001 |
S = 1.06 | Δρmax = 0.43 e Å−3 |
4004 reflections | Δρmin = −0.45 e Å−3 |
320 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
29 restraints | Extinction coefficient: 0.081 (5) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983) |
Secondary atom site location: difference Fourier map | Absolute structure parameter: −0.02 (8) |
Special details top
Experimental. A suitable single-crystal was carefully selected under a polarizing microscope
and mounted in a glass capillary. The scattering intensities were collected on
an imaging plate diffractometer (IPDS I, Stoe & Cie) equipped with a
fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 40 mA. Intensity data for the title compound were collected at room
temperature by φ-scans in 100 frames (0 < φ < 200°, Δφ = 2°, exposure
time of 5 min) in the 2 Θ range 3.8 to 56.3°. Structure solution and
refinement were carried out using the programs SIR92 (Altomare et
al., 1993) and SHELXL97 (Sheldrick, 1997). A numerical absorption
correction (X-RED (Stoe & Cie, 2001) was applied after optimization of
the crystal shape (X-SHAPE (Stoe & Cie, 1999)). The last cycles of
refinement included atomic positions for all atoms, anisotropic parameters for
all non-hydrogen atoms and isotropic thermal parameters for all hydrogen
atoms. The final difference maps were free of any chemically significant
features. The refinement was based on F2 for ALL reflections. |
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 (Å2) top | x | y | z | Uiso*/Ueq | |
P1 | 0.06286 (5) | 0.70682 (11) | 0.69882 (4) | 0.01697 (14) | |
P2 | 0.50392 (5) | 0.20332 (11) | 0.65964 (4) | 0.01664 (14) | |
P3 | 0.73850 (6) | 0.30542 (10) | 0.97653 (4) | 0.01667 (14) | |
O11 | 0.18639 (18) | 0.8277 (4) | 0.76074 (14) | 0.0335 (5) | |
H111 | 0.189 (4) | 0.847 (8) | 0.822 (3) | 0.066 (14)* | |
O12 | −0.06103 (17) | 0.7967 (4) | 0.72264 (14) | 0.0286 (4) | |
O13 | 0.06793 (16) | 0.7483 (3) | 0.59310 (12) | 0.0265 (5) | |
O14 | 0.07606 (18) | 0.4717 (3) | 0.72402 (14) | 0.0285 (4) | |
O21 | 0.49282 (19) | 0.3334 (4) | 0.75288 (15) | 0.0307 (5) | |
H211 | 0.548 (6) | 0.370 (11) | 0.790 (4) | 0.10 (2)* | |
O22 | 0.38360 (16) | 0.2665 (3) | 0.57963 (13) | 0.0274 (5) | |
O23 | 0.63168 (16) | 0.2661 (3) | 0.63262 (12) | 0.0240 (4) | |
O24 | 0.50188 (18) | −0.0326 (3) | 0.68323 (13) | 0.0268 (4) | |
O31 | 0.68406 (17) | 0.4504 (3) | 0.88660 (12) | 0.0240 (4) | |
O32 | 0.85225 (17) | 0.1739 (3) | 0.95559 (13) | 0.0269 (5) | |
O33 | 0.79062 (19) | 0.4514 (3) | 1.06460 (13) | 0.0277 (4) | |
O34 | 0.63092 (18) | 0.1584 (3) | 0.99590 (13) | 0.0272 (5) | |
N1 | 0.7063 (2) | 0.8299 (5) | 1.13488 (17) | 0.0273 (5) | |
H11 | 0.646 (3) | 0.805 (7) | 1.168 (2) | 0.049 (10)* | |
H12 | 0.716 (3) | 0.706 (4) | 1.106 (3) | 0.041 (9)* | |
H13 | 0.678 (3) | 0.929 (5) | 1.092 (2) | 0.037 (9)* | |
H14 | 0.777 (3) | 0.859 (7) | 1.181 (2) | 0.043 (10)* | |
N2 | 0.5190 (2) | −0.1752 (5) | 0.87680 (17) | 0.0292 (5) | |
H21 | 0.456 (3) | −0.215 (7) | 0.904 (2) | 0.048 (10)* | |
H22 | 0.485 (4) | −0.165 (7) | 0.8124 (15) | 0.051 (11)* | |
H23 | 0.572 (3) | −0.286 (4) | 0.882 (2) | 0.032 (8)* | |
H24 | 0.560 (4) | −0.070 (6) | 0.914 (3) | 0.059 (12)* | |
N3 | −0.1209 (2) | 0.2149 (5) | 0.76305 (15) | 0.0260 (4) | |
H31 | −0.201 (2) | 0.228 (7) | 0.724 (2) | 0.048 (10)* | |
H32 | −0.072 (3) | 0.325 (4) | 0.753 (2) | 0.025 (8)* | |
H33 | −0.125 (4) | 0.211 (8) | 0.8234 (15) | 0.052 (10)* | |
H34 | −0.094 (3) | 0.091 (4) | 0.749 (2) | 0.035 (9)* | |
N4 | 0.3232 (2) | −0.2974 (5) | 0.55885 (16) | 0.0260 (4) | |
H41 | 0.244 (2) | −0.278 (6) | 0.563 (2) | 0.034 (8)* | |
H42 | 0.346 (3) | −0.430 (3) | 0.576 (2) | 0.034 (9)* | |
H43 | 0.323 (3) | −0.278 (7) | 0.4968 (15) | 0.047 (10)* | |
H44 | 0.368 (3) | −0.203 (5) | 0.597 (2) | 0.038 (9)* | |
N5 | 0.1203 (2) | 0.1947 (5) | 0.57987 (15) | 0.0246 (4) | |
H51 | 0.2068 (18) | 0.196 (6) | 0.586 (2) | 0.029 (7)* | |
H52 | 0.106 (3) | 0.065 (3) | 0.596 (2) | 0.029 (9)* | |
H53 | 0.067 (2) | 0.219 (6) | 0.5208 (15) | 0.028 (7)* | |
H54 | 0.107 (3) | 0.282 (5) | 0.624 (2) | 0.034 (9)* | |
N6 | 0.32090 (19) | 0.2056 (5) | 0.37697 (16) | 0.0260 (4) | |
H61 | 0.2386 (19) | 0.230 (6) | 0.350 (2) | 0.028 (8)* | |
H62 | 0.337 (3) | 0.218 (7) | 0.4413 (14) | 0.036 (8)* | |
H63 | 0.339 (3) | 0.073 (3) | 0.367 (2) | 0.023 (8)* | |
H64 | 0.361 (4) | 0.289 (6) | 0.345 (3) | 0.055 (12)* | |
N7 | 0.9065 (2) | −0.2428 (4) | 0.91732 (19) | 0.0291 (6) | |
H71 | 0.975 (2) | −0.274 (7) | 0.9652 (19) | 0.039 (9)* | |
H72 | 0.879 (3) | −0.117 (4) | 0.934 (2) | 0.021 (8)* | |
H73 | 0.851 (3) | −0.337 (5) | 0.927 (3) | 0.050 (11)* | |
H74 | 0.926 (5) | −0.241 (9) | 0.859 (2) | 0.083 (16)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
P1 | 0.0166 (2) | 0.0172 (3) | 0.0174 (3) | −0.0006 (3) | 0.00444 (18) | −0.0006 (3) |
P2 | 0.0159 (2) | 0.0166 (3) | 0.0175 (2) | 0.0001 (3) | 0.00408 (18) | −0.0003 (3) |
P3 | 0.0209 (3) | 0.0131 (3) | 0.0170 (3) | −0.0002 (2) | 0.0065 (2) | −0.0007 (2) |
O11 | 0.0271 (9) | 0.0465 (14) | 0.0268 (9) | −0.0146 (9) | 0.0061 (7) | −0.0087 (9) |
O12 | 0.0221 (8) | 0.0324 (12) | 0.0320 (9) | 0.0040 (8) | 0.0076 (7) | −0.0063 (8) |
O13 | 0.0263 (8) | 0.0341 (14) | 0.0188 (8) | −0.0024 (7) | 0.0047 (6) | 0.0021 (7) |
O14 | 0.0336 (9) | 0.0195 (12) | 0.0340 (10) | 0.0037 (7) | 0.0113 (8) | 0.0057 (8) |
O21 | 0.0224 (9) | 0.0415 (14) | 0.0282 (9) | −0.0007 (8) | 0.0059 (7) | −0.0149 (9) |
O22 | 0.0231 (8) | 0.0316 (14) | 0.0251 (9) | 0.0018 (7) | 0.0008 (6) | 0.0017 (7) |
O23 | 0.0196 (7) | 0.0274 (14) | 0.0259 (8) | −0.0012 (6) | 0.0072 (6) | 0.0006 (7) |
O24 | 0.0332 (9) | 0.0181 (11) | 0.0299 (10) | 0.0001 (7) | 0.0090 (7) | 0.0040 (8) |
O31 | 0.0297 (9) | 0.0196 (11) | 0.0213 (8) | −0.0029 (7) | 0.0032 (7) | 0.0029 (7) |
O32 | 0.0286 (8) | 0.0244 (13) | 0.0295 (9) | 0.0070 (7) | 0.0107 (7) | −0.0028 (8) |
O33 | 0.0386 (10) | 0.0225 (12) | 0.0205 (8) | 0.0005 (8) | 0.0045 (7) | −0.0047 (7) |
O34 | 0.0318 (9) | 0.0239 (13) | 0.0295 (9) | −0.0064 (7) | 0.0144 (7) | 0.0012 (7) |
N1 | 0.0307 (11) | 0.0232 (16) | 0.0283 (12) | −0.0002 (10) | 0.0075 (9) | 0.0011 (10) |
N2 | 0.0346 (12) | 0.0249 (16) | 0.0307 (12) | −0.0036 (10) | 0.0127 (9) | −0.0016 (11) |
N3 | 0.0274 (10) | 0.0254 (14) | 0.0278 (10) | 0.0013 (11) | 0.0114 (8) | 0.0007 (12) |
N4 | 0.0254 (10) | 0.0253 (14) | 0.0276 (10) | −0.0001 (11) | 0.0073 (8) | 0.0006 (12) |
N5 | 0.0262 (9) | 0.0231 (14) | 0.0244 (10) | 0.0002 (11) | 0.0060 (7) | 0.0020 (11) |
N6 | 0.0240 (10) | 0.0239 (14) | 0.0298 (11) | 0.0008 (11) | 0.0062 (8) | −0.0001 (12) |
N7 | 0.0259 (11) | 0.0241 (18) | 0.0398 (13) | −0.0015 (8) | 0.0129 (10) | 0.0026 (10) |
Geometric parameters (Å, º) top
P1—O14 | 1.521 (2) | N2—H24 | 0.891 (19) |
P1—O12 | 1.5233 (18) | N3—H31 | 0.887 (18) |
P1—O13 | 1.5237 (17) | N3—H32 | 0.893 (18) |
P1—O11 | 1.573 (2) | N3—H33 | 0.859 (18) |
P2—O24 | 1.523 (2) | N3—H34 | 0.868 (19) |
P2—O23 | 1.5266 (17) | N4—H41 | 0.853 (18) |
P2—O22 | 1.5292 (18) | N4—H42 | 0.886 (19) |
P2—O21 | 1.574 (2) | N4—H43 | 0.882 (18) |
P3—O34 | 1.5312 (18) | N4—H44 | 0.861 (19) |
P3—O32 | 1.5352 (18) | N5—H51 | 0.888 (17) |
P3—O33 | 1.5356 (19) | N5—H52 | 0.876 (19) |
P3—O31 | 1.5548 (19) | N5—H53 | 0.896 (17) |
O11—H111 | 0.87 (4) | N5—H54 | 0.863 (18) |
O21—H211 | 0.72 (6) | N6—H61 | 0.868 (18) |
N1—H11 | 0.879 (19) | N6—H62 | 0.883 (18) |
N1—H12 | 0.899 (19) | N6—H63 | 0.873 (18) |
N1—H13 | 0.864 (19) | N6—H64 | 0.866 (19) |
N1—H14 | 0.882 (19) | N7—H71 | 0.884 (18) |
N2—H21 | 0.881 (18) | N7—H72 | 0.893 (18) |
N2—H22 | 0.894 (19) | N7—H73 | 0.864 (19) |
N2—H23 | 0.880 (18) | N7—H74 | 0.885 (19) |
| | | |
O14—P1—O12 | 110.20 (12) | H23—N2—H24 | 109 (4) |
O14—P1—O13 | 111.85 (11) | H31—N3—H32 | 109 (3) |
O12—P1—O13 | 112.33 (11) | H31—N3—H33 | 111 (3) |
O14—P1—O11 | 108.96 (12) | H32—N3—H33 | 110 (4) |
O12—P1—O11 | 109.20 (12) | H31—N3—H34 | 105 (4) |
O13—P1—O11 | 104.07 (11) | H32—N3—H34 | 115 (3) |
O24—P2—O23 | 111.42 (11) | H33—N3—H34 | 106 (4) |
O24—P2—O22 | 111.24 (11) | H41—N4—H42 | 109 (3) |
O23—P2—O22 | 111.48 (10) | H41—N4—H43 | 106 (3) |
O24—P2—O21 | 108.55 (12) | H42—N4—H43 | 110 (4) |
O23—P2—O21 | 108.38 (11) | H41—N4—H44 | 105 (3) |
O22—P2—O21 | 105.51 (11) | H42—N4—H44 | 114 (3) |
O34—P3—O32 | 110.16 (11) | H43—N4—H44 | 113 (4) |
O34—P3—O33 | 110.71 (11) | H51—N5—H52 | 103 (3) |
O32—P3—O33 | 109.56 (11) | H51—N5—H53 | 119 (3) |
O34—P3—O31 | 110.92 (11) | H52—N5—H53 | 108 (3) |
O32—P3—O31 | 108.16 (11) | H51—N5—H54 | 105 (3) |
O33—P3—O31 | 107.24 (11) | H52—N5—H54 | 110 (3) |
P1—O11—H111 | 117 (3) | H53—N5—H54 | 112 (3) |
P2—O21—H211 | 125 (5) | H61—N6—H62 | 111 (3) |
H11—N1—H12 | 105 (4) | H61—N6—H63 | 109 (3) |
H11—N1—H13 | 108 (3) | H62—N6—H63 | 104 (3) |
H12—N1—H13 | 112 (3) | H61—N6—H64 | 103 (3) |
H11—N1—H14 | 103 (3) | H62—N6—H64 | 119 (4) |
H12—N1—H14 | 111 (4) | H63—N6—H64 | 110 (4) |
H13—N1—H14 | 117 (4) | H71—N7—H72 | 105 (3) |
H21—N2—H22 | 108 (3) | H71—N7—H73 | 101 (4) |
H21—N2—H23 | 105 (4) | H72—N7—H73 | 107 (3) |
H22—N2—H23 | 104 (4) | H71—N7—H74 | 113 (4) |
H21—N2—H24 | 105 (3) | H72—N7—H74 | 113 (4) |
H22—N2—H24 | 125 (4) | H73—N7—H74 | 118 (4) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O11—H111···O33i | 0.87 (4) | 1.69 (5) | 2.535 (3) | 164 (5) |
O21—H211···O31 | 0.72 (6) | 1.79 (6) | 2.510 (3) | 177 (8) |
N1—H11···O21i | 0.88 (2) | 2.04 (2) | 2.899 (3) | 165 (4) |
N1—H12···O33 | 0.90 (2) | 1.93 (2) | 2.802 (3) | 163 (3) |
N1—H13···O34ii | 0.86 (2) | 1.97 (2) | 2.828 (3) | 174 (3) |
N1—H14···O14i | 0.88 (2) | 1.92 (2) | 2.789 (3) | 170 (4) |
N2—H21···O34iii | 0.88 (2) | 2.01 (2) | 2.847 (3) | 159 (3) |
N2—H22···O24 | 0.89 (2) | 2.05 (3) | 2.833 (3) | 146 (4) |
N2—H23···O31iv | 0.88 (2) | 2.03 (2) | 2.907 (3) | 176 (3) |
N2—H24···O34 | 0.89 (2) | 1.88 (2) | 2.768 (3) | 174 (4) |
N3—H31···O23v | 0.89 (2) | 1.93 (2) | 2.814 (3) | 176 (4) |
N3—H32···O14 | 0.89 (2) | 1.93 (2) | 2.776 (3) | 158 (3) |
N3—H33···O32v | 0.86 (2) | 1.95 (2) | 2.801 (3) | 173 (4) |
N3—H34···O12iv | 0.87 (2) | 1.94 (2) | 2.797 (4) | 170 (3) |
N4—H41···O13iv | 0.85 (2) | 1.99 (2) | 2.840 (3) | 172 (3) |
N4—H42···O22iv | 0.89 (2) | 1.95 (2) | 2.818 (4) | 166 (3) |
N4—H43···O23vi | 0.88 (2) | 2.01 (2) | 2.872 (3) | 167 (3) |
N4—H44···O24 | 0.86 (2) | 1.94 (2) | 2.791 (3) | 167 (4) |
N5—H51···O22 | 0.89 (2) | 1.93 (2) | 2.794 (3) | 165 (3) |
N5—H52···O13iv | 0.88 (2) | 2.03 (2) | 2.879 (4) | 163 (3) |
N5—H53···O13vii | 0.90 (2) | 1.88 (2) | 2.764 (3) | 169 (3) |
N5—H54···O14 | 0.86 (2) | 1.93 (2) | 2.796 (3) | 178 (4) |
N6—H61···O12vii | 0.87 (2) | 1.94 (2) | 2.807 (3) | 173 (3) |
N6—H62···O22 | 0.88 (2) | 1.92 (2) | 2.797 (3) | 174 (4) |
N6—H63···O23vi | 0.87 (2) | 1.96 (2) | 2.821 (4) | 169 (3) |
N6—H64···O24viii | 0.87 (2) | 1.93 (2) | 2.761 (3) | 160 (4) |
N7—H71···O32ix | 0.88 (2) | 1.91 (2) | 2.776 (3) | 166 (3) |
N7—H72···O32 | 0.89 (2) | 1.89 (2) | 2.765 (3) | 166 (3) |
N7—H73···O31iv | 0.86 (2) | 2.17 (2) | 2.977 (3) | 156 (3) |
N7—H73···O33iv | 0.86 (2) | 2.55 (3) | 3.266 (3) | 141 (3) |
N7—H74···O12x | 0.89 (2) | 1.97 (2) | 2.850 (3) | 169 (5) |
Symmetry codes: (i) −x+1, y+1/2, −z+2; (ii) x, y+1, z; (iii) −x+1, y−1/2, −z+2; (iv) x, y−1, z; (v) x−1, y, z; (vi) −x+1, y−1/2, −z+1; (vii) −x, y−1/2, −z+1; (viii) −x+1, y+1/2, −z+1; (ix) −x+2, y−1/2, −z+2; (x) x+1, y−1, z. |