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β-NH4[(MeO)2cDHAP] (where cDHAP is cyclic dihydroxyacetone phosphate) has been investigated by X-ray crystallography in the temperature range 350–100 K. Three reversible single-crystal-to-single-crystal phase transitions have been examined and four phases (high-, room-, medium- and low-temperature phase, HTP, RTP, MTP and LTP, respectively) have been structurally determined: HTP (at 350 K, P21/a, Z = 24), RTP (290 K, P \overline{1}, Z = 12), MTP (205 K, P21/a, Z = 4) and LTP (100 K, P \overline{1}, Z = 24). Various puckering modes of the 1,3,2-dioxaphosphorinane ring of the organic cyclic phosphate anion have been revealed in the crystal: chair and skew. The chairskew ring flipping, which has been shown to take place during the phase transitions, results in various populations of skew and chair conformers in different phases. The flexibility in the coordination geometry of ammonium cations is considered to assist in the conformational flexibility of the dioxaphosphorinane ring.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520615020259/wf5120sup1.cif
Contains datablocks HTP_sl8-350, RTP_new, MTP_sl8mt, LTP_sl8lt

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615020259/wf5120HTP_sl8-350sup2.hkl
Contains datablock sl8-350

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615020259/wf5120RTP_newsup3.hkl
Contains datablock new

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615020259/wf5120MTP_sl8mtsup4.hkl
Contains datablock sl8mt

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615020259/wf5120LTP_sl8ltsup5.hkl
Contains datablock sl8lt

gif

Graphic Interchange Format (GIF) image https://doi.org/10.1107/S2052520615020259/wf5120sup6.gif
Animation related to Figure 2.

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520615020259/wf5120sup7.pdf
Supporting figures and tables

CCDC references: 1041936; 1041937; 1041938; 1041939

Computing details top

Data collection: CrysAlis PRO, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) for HTP_sl8-350; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) for RTP_new, MTP_sl8mt, LTP_sl8lt. Cell refinement: CrysAlis PRO, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) for HTP_sl8-350; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) for RTP_new, MTP_sl8mt, LTP_sl8lt. Data reduction: CrysAlis PRO, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) for HTP_sl8-350; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) for RTP_new, MTP_sl8mt, LTP_sl8lt. For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2013).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
(HTP_sl8-350) ammonium 5,5-dimethoxy-2-oxo-1,3,2-dioxaphosphorinan-2-olate top
Crystal data top
C5H10O6P·H4NDx = 1.437 Mg m3
Mr = 215.14Melting point = 444–448 K
Monoclinic, P21/aMo Kα radiation, λ = 0.71073 Å
a = 11.910 (5) ÅCell parameters from 4955 reflections
b = 19.682 (8) Åθ = 2.8–28.8°
c = 25.516 (9) ŵ = 0.28 mm1
β = 93.74 (3)°T = 350 K
V = 5969 (4) Å3Plate, colourless
Z = 240.40 × 0.23 × 0.10 mm
F(000) = 2736
Data collection top
Xcalibur R kappa-geometry
diffractometer with a Ruby CCD camera
3275 reflections with I > 2σ(I)
Radiation source: Enhance (Mo) X-ray SourceRint = 0.190
ω scansθmax = 25.0°, θmin = 2.8°
Absorption correction: multi-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
h = 1414
Tmin = 0.458, Tmax = 1.000k = 2323
81666 measured reflectionsl = 3030
10503 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.077Hydrogen site location: mixed
wR(F2) = 0.177H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.035P)2]
where P = (Fo2 + 2Fc2)/3
10503 reflections(Δ/σ)max < 0.001
844 parametersΔρmax = 0.34 e Å3
1050 restraintsΔρmin = 0.20 e Å3
Crystal data top
C5H10O6P·H4NV = 5969 (4) Å3
Mr = 215.14Z = 24
Monoclinic, P21/aMo Kα radiation
a = 11.910 (5) ŵ = 0.28 mm1
b = 19.682 (8) ÅT = 350 K
c = 25.516 (9) Å0.40 × 0.23 × 0.10 mm
β = 93.74 (3)°
Data collection top
Xcalibur R kappa-geometry
diffractometer with a Ruby CCD camera
10503 independent reflections
Absorption correction: multi-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
3275 reflections with I > 2σ(I)
Tmin = 0.458, Tmax = 1.000Rint = 0.190
81666 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0771050 restraints
wR(F2) = 0.177H-atom parameters constrained
S = 1.00Δρmax = 0.34 e Å3
10503 reflectionsΔρmin = 0.20 e Å3
844 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
P1A0.4294 (3)0.37324 (18)0.17633 (13)0.0457 (10)0.749 (7)
O1A0.4393 (4)0.3858 (3)0.11577 (18)0.0581 (18)0.749 (7)
O21A0.5524 (5)0.2278 (3)0.0690 (3)0.0672 (19)0.749 (7)
O22A0.6599 (5)0.3204 (3)0.1023 (3)0.078 (2)0.749 (7)
O3A0.5340 (4)0.3259 (3)0.19108 (16)0.0544 (18)0.749 (7)
O4A0.3227 (4)0.3364 (4)0.1857 (3)0.063 (2)0.749 (7)
O5A0.4539 (7)0.4388 (3)0.2038 (3)0.075 (3)0.749 (7)
C1A0.4542 (6)0.3270 (3)0.0826 (2)0.058 (2)0.749 (7)
H1A10.46370.34210.04700.070*0.749 (7)
H1A20.38710.29900.08200.070*0.749 (7)
C2A0.5558 (6)0.2844 (3)0.1017 (3)0.055 (2)0.749 (7)
C3A0.5454 (6)0.2657 (4)0.1586 (3)0.062 (2)0.749 (7)
H3A10.48020.23670.16140.075*0.749 (7)
H3A20.61140.24040.17130.075*0.749 (7)
C4A0.6215 (8)0.1713 (4)0.0851 (3)0.074 (3)0.749 (7)
H4A10.61240.13580.05940.111*0.749 (7)
H4A20.59980.15490.11840.111*0.749 (7)
H4A30.69890.18530.08830.111*0.749 (7)
C5A0.6968 (8)0.3407 (5)0.0547 (3)0.094 (4)0.749 (7)
H5A10.76530.36610.06050.141*0.749 (7)
H5A20.64050.36880.03690.141*0.749 (7)
H5A30.71010.30150.03370.141*0.749 (7)
P10A0.4082 (10)0.3633 (7)0.1756 (4)0.055 (3)*0.251 (7)
O10A0.4093 (9)0.3590 (7)0.1138 (4)0.051 (4)*0.251 (7)
O23A0.5543 (14)0.2449 (8)0.0672 (7)0.059 (4)*0.251 (7)
O24A0.7010 (10)0.3008 (9)0.1161 (6)0.074 (5)*0.251 (7)
O30A0.5180 (11)0.3221 (10)0.1938 (4)0.056 (5)*0.251 (7)
O40A0.3066 (12)0.3286 (11)0.1942 (6)0.048 (6)*0.251 (7)
O50A0.4316 (19)0.4351 (8)0.1909 (7)0.050 (6)*0.251 (7)
C10A0.5183 (11)0.3555 (7)0.0917 (5)0.062 (5)*0.251 (7)
H10A0.56280.39460.10340.074*0.251 (7)
H10B0.50790.35760.05370.074*0.251 (7)
C20A0.5824 (10)0.2907 (7)0.1074 (5)0.063 (4)*0.251 (7)
C30A0.5473 (13)0.2662 (7)0.1599 (6)0.064 (5)*0.251 (7)
H30A0.48300.23620.15440.077*0.251 (7)
H30B0.60830.24030.17710.077*0.251 (7)
C40A0.625 (2)0.1867 (10)0.0633 (10)0.081 (7)*0.251 (7)
H40A0.59890.16020.03330.122*0.251 (7)
H40B0.62190.15980.09450.122*0.251 (7)
H40C0.70080.20110.05940.122*0.251 (7)
C50A0.7570 (15)0.3260 (16)0.0746 (9)0.093 (9)*0.251 (7)
H50A0.83500.33220.08540.140*0.251 (7)
H50B0.72470.36880.06370.140*0.251 (7)
H50C0.75030.29440.04590.140*0.251 (7)
P1B0.91321 (12)0.46573 (8)0.16897 (7)0.0502 (5)
O1B1.0299 (3)0.5026 (2)0.18231 (13)0.0551 (11)
O21B1.0579 (3)0.6191 (2)0.07557 (16)0.0771 (13)
O22B1.1201 (3)0.50588 (19)0.07739 (15)0.0655 (12)
O3B0.9080 (3)0.4633 (2)0.10615 (13)0.0558 (11)
O4B0.8180 (3)0.50830 (18)0.18661 (13)0.0568 (11)
O5B0.9265 (3)0.39603 (18)0.18949 (15)0.0646 (12)
C1B1.0530 (5)0.5654 (3)0.1549 (2)0.0593 (17)
H1B11.12770.58150.16610.071*
H1B20.99910.59990.16370.071*
C2B1.0454 (4)0.55369 (18)0.0965 (2)0.0534 (16)
C3B0.9311 (5)0.5248 (3)0.0794 (2)0.0618 (18)
H3B10.87360.55810.08620.074*
H3B20.92770.51630.04190.074*
C5B1.2327 (4)0.5151 (4)0.0922 (3)0.120 (3)
H5B11.27620.48040.07650.181*
H5B21.24380.51240.12970.181*
H5B31.25630.55900.08060.181*
C4B1.0700 (8)0.6263 (4)0.0225 (2)0.131 (5)0.912 (11)
H4B11.05720.67290.01250.197*0.912 (11)
H4B21.01650.59780.00330.197*0.912 (11)
H4B31.14490.61330.01480.197*0.912 (11)
C40B1.165 (2)0.639 (3)0.065 (3)0.07 (3)*0.088 (11)
H40D1.18180.68210.08060.112*0.088 (11)
H40E1.16980.64210.02740.112*0.088 (11)
H40F1.21830.60560.07860.112*0.088 (11)
P1C0.41138 (13)0.69487 (9)0.17327 (7)0.0570 (5)
O1C0.4012 (3)0.6930 (2)0.11101 (15)0.0734 (13)
O21C0.5465 (4)0.5897 (2)0.05551 (17)0.0826 (14)
O22C0.6928 (3)0.6499 (2)0.09944 (18)0.0907 (15)
O3C0.5237 (3)0.6526 (2)0.18580 (14)0.0654 (12)
O4C0.3119 (3)0.6578 (2)0.19069 (15)0.0706 (13)
O5C0.4332 (3)0.7638 (2)0.19335 (16)0.0799 (14)
C1C0.5024 (5)0.6976 (3)0.0861 (2)0.081 (2)
H1C10.54320.73770.09880.098*
H1C20.48590.70280.04860.098*
C2C0.5764 (5)0.6349 (4)0.0962 (3)0.0672 (19)
C3C0.5513 (5)0.6035 (4)0.1489 (2)0.091 (2)
H3C10.48930.57180.14360.109*
H3C20.61670.57830.16260.109*
C4C0.6025 (6)0.5233 (4)0.0604 (3)0.129 (3)
H4C10.57860.49540.03090.193*
H4C20.58300.50160.09220.193*
H4C30.68250.52950.06120.193*
C5C0.7335 (5)0.6820 (4)0.0559 (3)0.133 (3)
H5C10.81310.68920.06190.199*
H5C20.69640.72490.05050.199*
H5C30.71930.65390.02540.199*
P1D0.5912 (3)0.6363 (2)0.33217 (14)0.035 (2)*0.511 (5)
O1D0.4655 (5)0.6654 (4)0.3192 (2)0.048 (3)*0.511 (5)
O21D0.4419 (7)0.7896 (4)0.4229 (3)0.101 (3)*0.511 (5)
O22D0.3787 (6)0.6753 (4)0.4238 (3)0.080 (3)*0.511 (5)
O3D0.6078 (5)0.6441 (4)0.39435 (19)0.047 (3)*0.511 (5)
O4D0.6747 (6)0.6798 (4)0.3069 (3)0.068 (4)*0.511 (5)
O5D0.5833 (7)0.5626 (3)0.3182 (3)0.053 (3)*0.511 (5)
C1D0.4351 (7)0.7262 (4)0.3429 (3)0.080 (5)*0.511 (5)
H1D10.35620.73570.33400.096*0.511 (5)
H1D20.47910.76340.32990.096*0.511 (5)
C2D0.4563 (6)0.7207 (5)0.4041 (3)0.061 (3)*0.511 (5)
C3D0.5764 (7)0.6956 (4)0.4200 (3)0.071 (4)*0.511 (5)
H3D10.62880.73250.41530.086*0.511 (5)
H3D20.58060.68420.45710.086*0.511 (5)
C4D0.4252 (13)0.7963 (7)0.4761 (5)0.135 (6)*0.511 (5)
H4D10.41320.84330.48420.202*0.511 (5)
H4D20.49030.77990.49640.202*0.511 (5)
H4D30.36050.77030.48440.202*0.511 (5)
C5D0.2648 (9)0.6817 (8)0.4023 (5)0.116 (6)*0.511 (5)
H5D10.21940.64690.41670.174*0.511 (5)
H5D20.26280.67690.36480.174*0.511 (5)
H5D30.23600.72550.41110.174*0.511 (5)
P10D0.5921 (4)0.6364 (3)0.32853 (19)0.074 (3)*0.489 (5)
O10D0.4832 (5)0.6837 (4)0.31423 (19)0.042 (3)*0.489 (5)
O23D0.4483 (6)0.7431 (4)0.4450 (2)0.083 (3)*0.489 (5)
O24D0.3109 (7)0.6744 (5)0.3990 (3)0.092 (3)*0.489 (5)
O30D0.5887 (6)0.6285 (4)0.3907 (2)0.062 (3)*0.489 (5)
O40D0.6966 (6)0.6733 (4)0.3164 (3)0.054 (4)*0.489 (5)
O50D0.5651 (7)0.5698 (4)0.3027 (3)0.066 (4)*0.489 (5)
C10D0.4543 (7)0.7313 (4)0.3520 (3)0.034 (3)*0.489 (5)
H10C0.39010.75780.33840.041*0.489 (5)
H10D0.51670.76210.35970.041*0.489 (5)
C20D0.4245 (7)0.6937 (4)0.4035 (3)0.060 (3)*0.489 (5)
C30D0.4977 (7)0.6300 (4)0.4145 (3)0.070 (4)*0.489 (5)
H30C0.51660.62710.45200.084*0.489 (5)
H30D0.45350.59020.40440.084*0.489 (5)
C40D0.3916 (13)0.8048 (6)0.4392 (5)0.106 (5)*0.489 (5)
H40G0.41150.83340.46880.160*0.489 (5)
H40H0.31190.79680.43710.160*0.489 (5)
H40I0.41220.82680.40760.160*0.489 (5)
C50D0.2671 (9)0.6461 (7)0.4453 (4)0.104 (5)*0.489 (5)
H50D0.18960.63400.43800.157*0.489 (5)
H50E0.27280.67910.47300.157*0.489 (5)
H50F0.30950.60640.45580.157*0.489 (5)
P1E1.0856 (4)0.5292 (3)0.32618 (18)0.0560 (15)0.624 (7)
O1E1.0929 (5)0.5270 (3)0.3884 (2)0.059 (2)0.624 (7)
O21E0.9503 (6)0.4184 (4)0.4414 (3)0.087 (3)0.624 (7)
O22E0.8037 (6)0.4744 (4)0.3939 (3)0.072 (2)0.624 (7)
O3E0.9772 (6)0.4826 (4)0.3119 (2)0.050 (2)0.624 (7)
O4E1.1872 (6)0.4975 (5)0.3070 (4)0.075 (3)0.624 (7)
O5E1.0562 (8)0.5996 (4)0.3077 (4)0.071 (3)0.624 (7)
C1E0.9859 (6)0.5297 (4)0.4111 (3)0.074 (3)0.624 (7)
H1E10.94260.56780.39660.089*0.624 (7)
H1E20.99710.53620.44880.089*0.624 (7)
C2E0.9213 (6)0.4631 (4)0.3995 (3)0.060 (3)0.624 (7)
C3E0.9521 (7)0.4317 (4)0.3475 (3)0.055 (3)0.624 (7)
H3E11.01660.40200.35360.066*0.624 (7)
H3E20.88960.40460.33290.066*0.624 (7)
C4E0.9063 (12)0.3525 (6)0.4398 (6)0.121 (5)0.624 (7)
H4E10.93220.32840.47100.181*0.624 (7)
H4E20.93090.32920.40950.181*0.624 (7)
H4E30.82560.35460.43770.181*0.624 (7)
C5E0.7585 (9)0.5102 (7)0.4369 (4)0.103 (4)0.624 (7)
H5E10.67920.51700.42970.154*0.624 (7)
H5E20.79510.55350.44130.154*0.624 (7)
H5E30.77110.48420.46860.154*0.624 (7)
P10E1.0665 (7)0.5371 (5)0.3220 (3)0.050 (3)*0.376 (7)
O10E1.0568 (8)0.5524 (4)0.3825 (3)0.065 (4)*0.376 (7)
O23E0.9444 (11)0.3932 (6)0.4286 (5)0.091 (4)*0.376 (7)
O24E0.8446 (9)0.4910 (6)0.4026 (5)0.077 (3)*0.376 (7)
O30E0.9575 (9)0.4909 (6)0.3086 (3)0.054 (4)*0.376 (7)
O40E1.1701 (9)0.4981 (8)0.3150 (5)0.050 (4)*0.376 (7)
O50E1.0491 (13)0.6015 (6)0.2912 (5)0.069 (5)*0.376 (7)
C10E1.0499 (8)0.4931 (5)0.4149 (4)0.069 (4)*0.376 (7)
H10E1.04700.50660.45140.083*0.376 (7)
H10F1.11610.46510.41180.083*0.376 (7)
C20E0.9436 (9)0.4525 (5)0.3975 (4)0.059 (4)*0.376 (7)
C30E0.9425 (11)0.4333 (5)0.3393 (4)0.062 (4)*0.376 (7)
H30E1.00230.40090.33410.075*0.376 (7)
H30F0.87140.41180.32850.075*0.376 (7)
C40E0.8690 (16)0.3410 (7)0.4141 (7)0.082 (6)*0.376 (7)
H40J0.87510.30550.44000.123*0.376 (7)
H40K0.88660.32300.38060.123*0.376 (7)
H40L0.79370.35850.41170.123*0.376 (7)
C50E0.8160 (16)0.5023 (13)0.4558 (6)0.140 (9)*0.376 (7)
H50G0.74830.52880.45580.210*0.376 (7)
H50H0.87620.52630.47460.210*0.376 (7)
H50I0.80450.45940.47260.210*0.376 (7)
P1F0.5818 (4)0.2959 (3)0.32627 (17)0.043 (2)0.571 (6)
O1F0.4618 (5)0.3335 (4)0.3153 (2)0.046 (2)0.571 (6)
O21F0.4518 (8)0.4457 (4)0.4267 (4)0.086 (3)0.571 (6)
O22F0.3771 (5)0.3366 (4)0.4195 (3)0.074 (3)0.571 (6)
O3F0.5952 (5)0.2921 (3)0.3888 (2)0.0424 (19)0.571 (6)
O4F0.6731 (5)0.3373 (4)0.3057 (3)0.046 (2)0.571 (6)
O5F0.5654 (9)0.2246 (4)0.3074 (4)0.067 (4)0.571 (6)
C1F0.4428 (7)0.3933 (4)0.3439 (3)0.046 (3)0.571 (6)
H1F10.36730.40970.33480.056*0.571 (6)
H1F20.49550.42810.33450.056*0.571 (6)
C2F0.4568 (6)0.3802 (4)0.4023 (3)0.050 (3)0.571 (6)
C3F0.5770 (7)0.3522 (5)0.4151 (3)0.064 (3)0.571 (6)
H3F10.63160.38580.40530.077*0.571 (6)
H3F20.58830.34450.45260.077*0.571 (6)
C4F0.4391 (12)0.4549 (6)0.4754 (4)0.144 (7)0.571 (6)
H4F10.43700.50280.48260.216*0.571 (6)
H4F20.50090.43460.49580.216*0.571 (6)
H4F30.36990.43440.48450.216*0.571 (6)
C5F0.2581 (7)0.3488 (7)0.4034 (5)0.118 (5)0.571 (6)
H5F10.21250.31460.41850.177*0.571 (6)
H5F20.24760.34680.36580.177*0.571 (6)
H5F30.23630.39280.41530.177*0.571 (6)
P10F0.5774 (6)0.2953 (4)0.3248 (3)0.057 (3)*0.429 (6)
O10F0.4765 (7)0.3466 (6)0.3063 (3)0.044 (3)*0.429 (6)
O23F0.4371 (10)0.4419 (5)0.4245 (5)0.085 (4)*0.429 (6)
O24F0.3371 (7)0.3459 (6)0.3958 (3)0.091 (4)*0.429 (6)
O30F0.5551 (7)0.2810 (4)0.3848 (3)0.047 (3)*0.429 (6)
O40F0.6880 (6)0.3287 (6)0.3206 (4)0.038 (4)*0.429 (6)
O50F0.5535 (11)0.2303 (5)0.2961 (4)0.056 (4)*0.429 (6)
C10F0.4588 (9)0.4032 (5)0.3387 (4)0.045 (4)*0.429 (6)
H10G0.39510.42920.32400.055*0.429 (6)
H10H0.52460.43230.33990.055*0.429 (6)
C20F0.4366 (8)0.3809 (5)0.3938 (4)0.055 (4)*0.429 (6)
C30F0.5378 (9)0.3375 (6)0.4153 (4)0.077 (4)*0.429 (6)
H30G0.60510.36540.41700.092*0.429 (6)
H30H0.52480.32300.45070.092*0.429 (6)
C40F0.3715 (10)0.4921 (6)0.4146 (5)0.070 (5)*0.429 (6)
H40M0.38360.52580.44160.105*0.429 (6)
H40N0.29480.47690.41370.105*0.429 (6)
H40O0.38660.51140.38130.105*0.429 (6)
C50F0.3002 (12)0.3249 (9)0.4472 (5)0.112 (7)*0.429 (6)
H50J0.22980.30120.44240.168*0.429 (6)
H50K0.29090.36440.46860.168*0.429 (6)
H50L0.35570.29550.46410.168*0.429 (6)
N10.8452 (3)0.2877 (2)0.24735 (15)0.0610 (14)
H1N0.85690.32340.22630.092*
H2N0.82870.25070.22760.092*
H3N0.78740.29700.26730.092*
H4N0.90770.27980.26820.092*
N21.1450 (3)0.3796 (2)0.24714 (16)0.0651 (15)
H5N1.20290.36860.22780.098*
H6N1.12920.34420.26780.098*
H7N1.16360.41590.26730.098*
H8N1.08410.38950.22570.098*
N30.6609 (3)0.4587 (2)0.25482 (16)0.0700 (16)
H9N0.67420.42070.27390.105*
H10N0.72180.46850.23710.105*
H11N0.64660.49340.27630.105*
H12N0.60120.45200.23190.105*
N40.3614 (3)0.5448 (2)0.25624 (15)0.0612 (14)
H13N0.38110.50870.23720.092*
H14N0.34820.58070.23490.092*
H15N0.29860.53490.27250.092*
H16N0.41750.55480.28030.092*
N50.8468 (3)0.6265 (2)0.24680 (16)0.0711 (15)
H17N0.82890.59350.22330.107*
H18N0.78640.63630.26490.107*
H19N0.90360.61240.26910.107*
H20N0.86820.66400.22980.107*
N61.1404 (3)0.7086 (2)0.24867 (17)0.0751 (16)
H21N1.15910.74590.26770.113*
H22N1.19720.69770.22860.113*
H23N1.12750.67390.27040.113*
H24N1.07790.71710.22800.113*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P1A0.0403 (16)0.0356 (17)0.0639 (18)0.0017 (13)0.0228 (13)0.0022 (12)
O1A0.064 (4)0.054 (4)0.059 (3)0.011 (3)0.025 (3)0.014 (3)
O21A0.073 (4)0.061 (4)0.069 (3)0.013 (3)0.016 (3)0.032 (3)
O22A0.066 (4)0.080 (4)0.090 (4)0.022 (3)0.035 (3)0.009 (3)
O3A0.053 (3)0.069 (4)0.043 (3)0.002 (3)0.017 (2)0.019 (3)
O4A0.043 (3)0.069 (4)0.082 (5)0.002 (3)0.036 (3)0.010 (3)
O5A0.092 (6)0.048 (4)0.088 (5)0.007 (3)0.025 (4)0.030 (3)
C1A0.060 (4)0.070 (5)0.046 (4)0.002 (4)0.010 (3)0.005 (4)
C2A0.050 (4)0.058 (5)0.061 (4)0.001 (4)0.030 (4)0.006 (4)
C3A0.056 (4)0.063 (5)0.070 (5)0.022 (4)0.018 (4)0.004 (4)
C4A0.115 (7)0.047 (5)0.064 (6)0.026 (5)0.032 (5)0.015 (4)
C5A0.112 (8)0.098 (7)0.078 (6)0.040 (7)0.054 (6)0.007 (6)
P1B0.0428 (9)0.0387 (10)0.0711 (12)0.0064 (7)0.0186 (8)0.0059 (8)
O1B0.052 (2)0.055 (3)0.059 (2)0.005 (2)0.0057 (19)0.011 (2)
O21B0.099 (3)0.052 (3)0.085 (3)0.004 (2)0.044 (3)0.018 (2)
O22B0.056 (2)0.052 (3)0.091 (3)0.009 (2)0.024 (2)0.007 (2)
O3B0.055 (2)0.051 (3)0.061 (2)0.017 (2)0.005 (2)0.007 (2)
O4B0.047 (2)0.052 (3)0.074 (3)0.0019 (19)0.024 (2)0.003 (2)
O5B0.073 (3)0.030 (2)0.093 (3)0.009 (2)0.021 (2)0.014 (2)
C1B0.055 (4)0.058 (4)0.066 (4)0.022 (3)0.011 (3)0.005 (3)
C2B0.050 (4)0.039 (4)0.071 (4)0.011 (3)0.012 (3)0.005 (3)
C3B0.073 (4)0.066 (4)0.048 (3)0.001 (3)0.015 (3)0.017 (3)
C5B0.041 (4)0.149 (8)0.171 (8)0.026 (5)0.008 (5)0.001 (6)
C4B0.232 (12)0.092 (7)0.079 (7)0.007 (7)0.074 (7)0.039 (5)
P1C0.0523 (10)0.0475 (11)0.0737 (12)0.0092 (8)0.0236 (9)0.0005 (9)
O1C0.058 (3)0.083 (3)0.080 (3)0.026 (2)0.012 (2)0.008 (2)
O21C0.081 (3)0.085 (4)0.081 (3)0.014 (3)0.001 (3)0.018 (3)
O22C0.069 (3)0.087 (4)0.120 (4)0.007 (3)0.025 (3)0.005 (3)
O3C0.063 (3)0.075 (3)0.059 (3)0.013 (2)0.019 (2)0.004 (2)
O4C0.049 (2)0.066 (3)0.100 (3)0.000 (2)0.024 (2)0.006 (2)
O5C0.091 (3)0.044 (3)0.107 (3)0.003 (2)0.026 (3)0.010 (2)
C1C0.102 (5)0.084 (5)0.062 (4)0.035 (4)0.038 (4)0.026 (4)
C2C0.059 (4)0.084 (5)0.061 (4)0.021 (4)0.023 (4)0.006 (4)
C3C0.088 (5)0.107 (6)0.077 (5)0.055 (4)0.012 (4)0.014 (4)
C4C0.116 (6)0.080 (6)0.189 (8)0.018 (5)0.003 (6)0.057 (6)
C5C0.094 (6)0.145 (8)0.167 (8)0.010 (5)0.064 (6)0.044 (6)
P1E0.049 (2)0.057 (3)0.064 (3)0.000 (2)0.0161 (17)0.0015 (16)
O1E0.050 (4)0.071 (5)0.055 (4)0.017 (4)0.008 (3)0.005 (3)
O21E0.079 (5)0.084 (6)0.099 (5)0.000 (4)0.009 (4)0.022 (5)
O22E0.062 (4)0.064 (5)0.091 (5)0.009 (4)0.000 (4)0.000 (4)
O3E0.044 (4)0.053 (4)0.054 (4)0.014 (3)0.003 (3)0.002 (3)
O4E0.059 (5)0.078 (6)0.095 (6)0.001 (4)0.047 (4)0.005 (4)
O5E0.080 (6)0.054 (5)0.080 (6)0.003 (4)0.020 (5)0.022 (4)
C1E0.073 (6)0.074 (7)0.078 (6)0.005 (5)0.020 (5)0.009 (5)
C2E0.060 (5)0.055 (5)0.067 (5)0.002 (5)0.013 (5)0.008 (5)
C3E0.047 (5)0.050 (6)0.067 (6)0.003 (4)0.008 (5)0.011 (5)
C4E0.112 (9)0.110 (10)0.141 (10)0.000 (8)0.001 (9)0.012 (9)
C5E0.081 (8)0.112 (9)0.116 (9)0.042 (8)0.012 (8)0.001 (8)
P1F0.052 (3)0.041 (3)0.039 (2)0.0002 (14)0.0198 (15)0.0053 (14)
O1F0.052 (4)0.045 (5)0.044 (4)0.001 (4)0.016 (3)0.000 (4)
O21F0.085 (5)0.099 (6)0.073 (5)0.008 (5)0.006 (5)0.054 (5)
O22F0.060 (5)0.080 (5)0.083 (6)0.004 (4)0.025 (4)0.008 (4)
O3F0.027 (4)0.048 (4)0.054 (4)0.005 (3)0.012 (3)0.008 (3)
O4F0.045 (4)0.054 (5)0.038 (5)0.004 (3)0.003 (4)0.012 (4)
O5F0.084 (6)0.044 (5)0.073 (6)0.008 (4)0.015 (5)0.016 (5)
C1F0.051 (5)0.040 (6)0.050 (6)0.008 (5)0.024 (5)0.012 (5)
C2F0.061 (6)0.061 (6)0.032 (5)0.002 (5)0.019 (5)0.016 (5)
C3F0.034 (5)0.090 (7)0.067 (6)0.001 (5)0.000 (5)0.028 (6)
C4F0.193 (17)0.138 (15)0.100 (12)0.024 (12)0.000 (12)0.036 (10)
C5F0.058 (8)0.136 (11)0.155 (11)0.010 (8)0.027 (8)0.002 (9)
N10.071 (3)0.039 (3)0.077 (3)0.001 (3)0.039 (3)0.004 (3)
N20.061 (3)0.043 (3)0.093 (4)0.008 (3)0.024 (3)0.008 (3)
N30.055 (3)0.061 (4)0.097 (4)0.000 (3)0.035 (3)0.003 (3)
N40.064 (3)0.044 (3)0.078 (3)0.004 (3)0.022 (3)0.004 (3)
N50.075 (3)0.038 (3)0.104 (4)0.003 (3)0.039 (3)0.001 (3)
N60.063 (3)0.058 (4)0.109 (4)0.005 (3)0.037 (3)0.003 (3)
Geometric parameters (Å, º) top
P1A—O5A1.487 (5)C10D—C20D1.568 (7)
P1A—O4A1.496 (5)C10D—H10C0.9700
P1A—O1A1.577 (4)C10D—H10D0.9700
P1A—O3A1.581 (4)C20D—C30D1.542 (9)
O1A—C1A1.451 (7)C30D—H30C0.9700
O21A—C2A1.390 (6)C30D—H30D0.9700
O21A—C4A1.427 (7)C40D—H40G0.9600
O22A—C5A1.377 (6)C40D—H40H0.9600
O22A—C2A1.428 (7)C40D—H40I0.9600
O3A—C3A1.458 (6)C50D—H50D0.9600
C1A—C2A1.526 (8)C50D—H50E0.9600
C1A—H1A10.9700C50D—H50F0.9600
C1A—H1A20.9700P1E—O4E1.474 (5)
C2A—C3A1.510 (7)P1E—O5E1.498 (5)
C3A—H3A10.9700P1E—O1E1.584 (4)
C3A—H3A20.9700P1E—O3E1.606 (4)
C4A—H4A10.9600O1E—C1E1.435 (7)
C4A—H4A20.9600O21E—C4E1.398 (10)
C4A—H4A30.9600O21E—C2E1.411 (7)
C5A—H5A10.9600O22E—C2E1.416 (7)
C5A—H5A20.9600O22E—C5E1.440 (8)
C5A—H5A30.9600O3E—C3E1.398 (6)
P10A—O50A1.487 (5)C1E—C2E1.539 (9)
P10A—O40A1.495 (5)C1E—H1E10.9700
P10A—O10A1.579 (4)C1E—H1E20.9700
P10A—O30A1.582 (4)C2E—C3E1.530 (8)
O10A—C10A1.451 (7)C3E—H3E10.9700
O23A—C20A1.391 (7)C3E—H3E20.9700
O23A—C40A1.427 (7)C4E—H4E10.9600
O24A—C50A1.378 (7)C4E—H4E20.9600
O24A—C20A1.429 (7)C4E—H4E30.9600
O30A—C30A1.457 (6)C5E—H5E10.9600
C10A—C20A1.525 (8)C5E—H5E20.9600
C10A—H10A0.9700C5E—H5E30.9600
C10A—H10B0.9700P10E—O40E1.474 (5)
C20A—C30A1.508 (7)P10E—O50E1.499 (5)
C30A—H30A0.9700P10E—O10E1.583 (5)
C30A—H30B0.9700P10E—O30E1.605 (4)
C40A—H40A0.9600O10E—C10E1.435 (7)
C40A—H40B0.9600O23E—C40E1.399 (11)
C40A—H40C0.9600O23E—C20E1.411 (7)
C50A—H50A0.9600O24E—C20E1.416 (8)
C50A—H50B0.9600O24E—C50E1.440 (8)
C50A—H50C0.9600O30E—C30E1.397 (6)
P1B—O5B1.473 (4)C10E—C20E1.539 (9)
P1B—O4B1.502 (3)C10E—H10E0.9700
P1B—O1B1.586 (4)C10E—H10F0.9700
P1B—O3B1.601 (4)C20E—C30E1.530 (8)
O1B—C1B1.454 (6)C30E—H30E0.9700
O21B—C4B1.378 (4)C30E—H30F0.9700
O21B—C40B1.379 (5)C40E—H40J0.9600
O21B—C2B1.406 (4)C40E—H40K0.9600
O22B—C5B1.380 (4)C40E—H40L0.9600
O22B—C2B1.405 (4)C50E—H50G0.9600
O3B—C3B1.426 (6)C50E—H50H0.9600
C1B—C2B1.506 (7)C50E—H50I0.9600
C1B—H1B10.9700P1F—O4F1.482 (4)
C1B—H1B20.9700P1F—O5F1.492 (4)
C2B—C3B1.512 (7)P1F—O3F1.595 (4)
C3B—H3B10.9700P1F—O1F1.617 (4)
C3B—H3B20.9700O1F—C1F1.411 (6)
C5B—H5B10.9600O21F—C4F1.274 (11)
C5B—H5B20.9600O21F—C2F1.434 (7)
C5B—H5B30.9600O22F—C2F1.373 (7)
C4B—H4B10.9600O22F—C5F1.470 (8)
C4B—H4B20.9600O3F—C3F1.383 (7)
C4B—H4B30.9600C1F—C2F1.511 (7)
C40B—H40D0.9600C1F—H1F10.9700
C40B—H40E0.9600C1F—H1F20.9700
C40B—H40F0.9600C2F—C3F1.549 (8)
P1C—O5C1.467 (4)C3F—H3F10.9700
P1C—O4C1.484 (4)C3F—H3F20.9700
P1C—O1C1.586 (4)C4F—H4F10.9600
P1C—O3C1.591 (4)C4F—H4F20.9600
O1C—C1C1.402 (6)C4F—H4F30.9600
O21C—C2C1.396 (7)C5F—H5F10.9600
O21C—C4C1.469 (7)C5F—H5F20.9600
O22C—C5C1.392 (6)C5F—H5F30.9600
O22C—C2C1.415 (6)P10F—O40F1.482 (4)
O3C—C3C1.403 (6)P10F—O50F1.492 (4)
C1C—C2C1.528 (8)P10F—O30F1.595 (4)
C1C—H1C10.9700P10F—O10F1.617 (4)
C1C—H1C20.9700O10F—C10F1.412 (6)
C2C—C3C1.526 (7)O23F—C40F1.274 (11)
C3C—H3C10.9700O23F—C20F1.435 (7)
C3C—H3C20.9700O24F—C20F1.373 (7)
C4C—H4C10.9600O24F—C50F1.469 (8)
C4C—H4C20.9600O30F—C30F1.382 (7)
C4C—H4C30.9600C10F—C20F1.511 (7)
C5C—H5C10.9600C10F—H10G0.9700
C5C—H5C20.9600C10F—H10H0.9700
C5C—H5C30.9600C20F—C30F1.548 (8)
P1D—O4D1.491 (4)C30F—H30G0.9700
P1D—O5D1.495 (4)C30F—H30H0.9700
P1D—O3D1.593 (4)C40F—H40M0.9600
P1D—O1D1.617 (4)C40F—H40N0.9600
O1D—C1D1.399 (6)C40F—H40O0.9600
O21D—C4D1.392 (9)C50F—H50J0.9600
O21D—C2D1.452 (9)C50F—H50K0.9600
O22D—C2D1.403 (10)C50F—H50L0.9600
O22D—C5D1.435 (9)N1—H1N0.9001
O3D—C3D1.276 (7)N1—H2N0.9000
C1D—C2D1.568 (7)N1—H3N0.9001
C1D—H1D10.9700N1—H4N0.9003
C1D—H1D20.9700N2—H5N0.8999
C2D—C3D1.543 (9)N2—H6N0.9006
C3D—H3D10.9700N2—H7N0.9000
C3D—H3D20.9700N2—H8N0.9000
C4D—H4D10.9600N3—H9N0.9002
C4D—H4D20.9600N3—H10N0.9002
C4D—H4D30.9600N3—H11N0.9001
C5D—H5D10.9600N3—H12N0.9000
C5D—H5D20.9600N4—H13N0.9004
C5D—H5D30.9600N4—H14N0.9001
P10D—O40D1.490 (4)N4—H15N0.9002
P10D—O50D1.493 (4)N4—H16N0.8999
P10D—O30D1.596 (4)N5—H17N0.9000
P10D—O10D1.619 (4)N5—H18N0.9002
O10D—C10D1.402 (6)N5—H19N0.9001
O23D—C40D1.393 (9)N5—H20N0.9003
O23D—C20D1.452 (9)N6—H21N0.9003
O24D—C20D1.404 (10)N6—H22N0.9002
O24D—C50D1.435 (9)N6—H23N0.9001
O30D—C30D1.277 (7)N6—H24N0.9001
O5A—P1A—O4A119.2 (2)H10C—C10D—H10D108.2
O5A—P1A—O1A107.6 (3)O24D—C20D—O23D112.5 (6)
O4A—P1A—O1A110.5 (3)O24D—C20D—C30D108.9 (6)
O5A—P1A—O3A105.7 (3)O23D—C20D—C30D109.3 (6)
O4A—P1A—O3A109.9 (3)O24D—C20D—C10D109.2 (6)
O1A—P1A—O3A102.6 (2)O23D—C20D—C10D104.6 (6)
C1A—O1A—P1A117.8 (4)C30D—C20D—C10D112.3 (6)
C2A—O21A—C4A117.2 (5)O30D—C30D—C20D114.8 (6)
C5A—O22A—C2A117.4 (6)O30D—C30D—H30C108.6
C3A—O3A—P1A116.4 (3)C20D—C30D—H30C108.6
O1A—C1A—C2A112.1 (5)O30D—C30D—H30D108.6
O1A—C1A—H1A1109.2C20D—C30D—H30D108.6
C2A—C1A—H1A1109.2H30C—C30D—H30D107.5
O1A—C1A—H1A2109.2O23D—C40D—H40G109.5
C2A—C1A—H1A2109.2O23D—C40D—H40H109.5
H1A1—C1A—H1A2107.9H40G—C40D—H40H109.5
O21A—C2A—O22A113.4 (5)O23D—C40D—H40I109.5
O21A—C2A—C3A112.4 (5)H40G—C40D—H40I109.5
O22A—C2A—C3A103.6 (5)H40H—C40D—H40I109.5
O21A—C2A—C1A104.9 (5)O24D—C50D—H50D109.5
O22A—C2A—C1A113.6 (6)O24D—C50D—H50E109.5
C3A—C2A—C1A109.1 (5)H50D—C50D—H50E109.5
O3A—C3A—C2A111.5 (5)O24D—C50D—H50F109.5
O3A—C3A—H3A1109.3H50D—C50D—H50F109.5
C2A—C3A—H3A1109.3H50E—C50D—H50F109.5
O3A—C3A—H3A2109.3O4E—P1E—O5E117.9 (3)
C2A—C3A—H3A2109.3O4E—P1E—O1E109.2 (3)
H3A1—C3A—H3A2108.0O5E—P1E—O1E109.7 (3)
O21A—C4A—H4A1109.5O4E—P1E—O3E110.4 (3)
O21A—C4A—H4A2109.5O5E—P1E—O3E106.8 (3)
H4A1—C4A—H4A2109.5O1E—P1E—O3E101.7 (2)
O21A—C4A—H4A3109.5C1E—O1E—P1E114.4 (5)
H4A1—C4A—H4A3109.5C4E—O21E—C2E118.9 (8)
H4A2—C4A—H4A3109.5C2E—O22E—C5E114.5 (7)
O22A—C5A—H5A1109.5C3E—O3E—P1E117.7 (4)
O22A—C5A—H5A2109.5O1E—C1E—C2E109.6 (5)
H5A1—C5A—H5A2109.5O1E—C1E—H1E1109.7
O22A—C5A—H5A3109.5C2E—C1E—H1E1109.7
H5A1—C5A—H5A3109.5O1E—C1E—H1E2109.7
H5A2—C5A—H5A3109.5C2E—C1E—H1E2109.7
O50A—P10A—O40A119.5 (3)H1E1—C1E—H1E2108.2
O50A—P10A—O10A107.5 (4)O21E—C2E—O22E111.5 (6)
O40A—P10A—O10A110.6 (3)O21E—C2E—C3E110.2 (6)
O50A—P10A—O30A105.8 (4)O22E—C2E—C3E105.4 (6)
O40A—P10A—O30A110.0 (3)O21E—C2E—C1E106.9 (6)
O10A—P10A—O30A101.9 (3)O22E—C2E—C1E111.4 (6)
C10A—O10A—P10A117.2 (5)C3E—C2E—C1E111.5 (6)
C20A—O23A—C40A117.2 (6)O3E—C3E—C2E110.4 (5)
C50A—O24A—C20A117.0 (7)O3E—C3E—H3E1109.6
C30A—O30A—P10A116.0 (4)C2E—C3E—H3E1109.6
O10A—C10A—C20A112.5 (5)O3E—C3E—H3E2109.6
O10A—C10A—H10A109.1C2E—C3E—H3E2109.6
C20A—C10A—H10A109.1H3E1—C3E—H3E2108.1
O10A—C10A—H10B109.1O21E—C4E—H4E1109.5
C20A—C10A—H10B109.1O21E—C4E—H4E2109.5
H10A—C10A—H10B107.8H4E1—C4E—H4E2109.5
O23A—C20A—O24A113.0 (5)O21E—C4E—H4E3109.5
O23A—C20A—C30A112.3 (6)H4E1—C4E—H4E3109.5
O24A—C20A—C30A103.7 (6)H4E2—C4E—H4E3109.5
O23A—C20A—C10A104.8 (6)O22E—C5E—H5E1109.5
O24A—C20A—C10A113.4 (6)O22E—C5E—H5E2109.5
C30A—C20A—C10A109.8 (5)H5E1—C5E—H5E2109.5
O30A—C30A—C20A112.1 (5)O22E—C5E—H5E3109.5
O30A—C30A—H30A109.2H5E1—C5E—H5E3109.5
C20A—C30A—H30A109.2H5E2—C5E—H5E3109.5
O30A—C30A—H30B109.2O40E—P10E—O50E117.7 (3)
C20A—C30A—H30B109.2O40E—P10E—O10E109.4 (4)
H30A—C30A—H30B107.9O50E—P10E—O10E109.6 (4)
O23A—C40A—H40A109.5O40E—P10E—O30E110.5 (3)
O23A—C40A—H40B109.5O50E—P10E—O30E106.6 (3)
H40A—C40A—H40B109.5O10E—P10E—O30E101.9 (3)
O23A—C40A—H40C109.5C10E—O10E—P10E114.7 (5)
H40A—C40A—H40C109.5C40E—O23E—C20E118.5 (8)
H40B—C40A—H40C109.5C20E—O24E—C50E114.8 (7)
O24A—C50A—H50A109.5C30E—O30E—P10E118.1 (5)
O24A—C50A—H50B109.5O10E—C10E—C20E109.5 (6)
H50A—C50A—H50B109.5O10E—C10E—H10E109.8
O24A—C50A—H50C109.5C20E—C10E—H10E109.8
H50A—C50A—H50C109.5O10E—C10E—H10F109.8
H50B—C50A—H50C109.5C20E—C10E—H10F109.8
O5B—P1B—O4B118.6 (2)H10E—C10E—H10F108.2
O5B—P1B—O1B106.1 (2)O23E—C20E—O24E111.5 (6)
O4B—P1B—O1B110.4 (2)O23E—C20E—C30E110.0 (7)
O5B—P1B—O3B108.9 (2)O24E—C20E—C30E105.5 (6)
O4B—P1B—O3B109.7 (2)O23E—C20E—C10E107.0 (6)
O1B—P1B—O3B101.82 (19)O24E—C20E—C10E111.7 (7)
C1B—O1B—P1B118.5 (3)C30E—C20E—C10E111.3 (6)
C4B—O21B—C2B119.2 (5)O30E—C30E—C20E110.6 (5)
C40B—O21B—C2B117 (3)O30E—C30E—H30E109.5
C5B—O22B—C2B116.3 (4)C20E—C30E—H30E109.5
C3B—O3B—P1B117.2 (3)O30E—C30E—H30F109.5
O1B—C1B—C2B110.2 (4)C20E—C30E—H30F109.5
O1B—C1B—H1B1109.6H30E—C30E—H30F108.1
C2B—C1B—H1B1109.6O23E—C40E—H40J109.5
O1B—C1B—H1B2109.6O23E—C40E—H40K109.5
C2B—C1B—H1B2109.6H40J—C40E—H40K109.5
H1B1—C1B—H1B2108.1O23E—C40E—H40L109.5
O22B—C2B—O21B113.4 (4)H40J—C40E—H40L109.5
O22B—C2B—C1B116.6 (4)H40K—C40E—H40L109.5
O21B—C2B—C1B103.6 (4)O24E—C50E—H50G109.5
O22B—C2B—C3B103.1 (4)O24E—C50E—H50H109.5
O21B—C2B—C3B110.5 (4)H50G—C50E—H50H109.5
C1B—C2B—C3B109.7 (4)O24E—C50E—H50I109.5
O3B—C3B—C2B112.3 (4)H50G—C50E—H50I109.5
O3B—C3B—H3B1109.1H50H—C50E—H50I109.5
C2B—C3B—H3B1109.1O4F—P1F—O5F119.1 (3)
O3B—C3B—H3B2109.1O4F—P1F—O3F110.7 (3)
C2B—C3B—H3B2109.1O5F—P1F—O3F106.3 (3)
H3B1—C3B—H3B2107.9O4F—P1F—O1F110.4 (3)
O22B—C5B—H5B1109.5O5F—P1F—O1F106.2 (3)
O22B—C5B—H5B2109.5O3F—P1F—O1F103.0 (2)
H5B1—C5B—H5B2109.5C1F—O1F—P1F117.5 (4)
O22B—C5B—H5B3109.5C4F—O21F—C2F124.2 (8)
H5B1—C5B—H5B3109.5C2F—O22F—C5F118.9 (5)
H5B2—C5B—H5B3109.5C3F—O3F—P1F115.8 (4)
O21B—C4B—H4B1109.5O1F—C1F—C2F110.9 (5)
O21B—C4B—H4B2109.5O1F—C1F—H1F1109.5
H4B1—C4B—H4B2109.5C2F—C1F—H1F1109.5
O21B—C4B—H4B3109.5O1F—C1F—H1F2109.5
H4B1—C4B—H4B3109.5C2F—C1F—H1F2109.5
H4B2—C4B—H4B3109.5H1F1—C1F—H1F2108.0
O21B—C40B—H40D109.5O22F—C2F—O21F112.0 (5)
O21B—C40B—H40E109.5O22F—C2F—C1F112.8 (6)
H40D—C40B—H40E109.5O21F—C2F—C1F105.7 (5)
O21B—C40B—H40F109.5O22F—C2F—C3F111.1 (6)
H40D—C40B—H40F109.5O21F—C2F—C3F107.0 (6)
H40E—C40B—H40F109.5C1F—C2F—C3F108.0 (5)
O5C—P1C—O4C118.5 (2)O3F—C3F—C2F112.0 (6)
O5C—P1C—O1C111.8 (3)O3F—C3F—H3F1109.2
O4C—P1C—O1C106.1 (2)C2F—C3F—H3F1109.2
O5C—P1C—O3C106.6 (2)O3F—C3F—H3F2109.2
O4C—P1C—O3C111.1 (2)C2F—C3F—H3F2109.2
O1C—P1C—O3C101.4 (2)H3F1—C3F—H3F2107.9
C1C—O1C—P1C116.2 (4)O21F—C4F—H4F1109.5
C2C—O21C—C4C114.3 (5)O21F—C4F—H4F2109.5
C5C—O22C—C2C116.1 (5)H4F1—C4F—H4F2109.5
C3C—O3C—P1C117.1 (4)O21F—C4F—H4F3109.5
O1C—C1C—C2C112.0 (5)H4F1—C4F—H4F3109.5
O1C—C1C—H1C1109.2H4F2—C4F—H4F3109.5
C2C—C1C—H1C1109.2O22F—C5F—H5F1109.5
O1C—C1C—H1C2109.2O22F—C5F—H5F2109.5
C2C—C1C—H1C2109.2H5F1—C5F—H5F2109.5
H1C1—C1C—H1C2107.9O22F—C5F—H5F3109.5
O21C—C2C—O22C112.2 (5)H5F1—C5F—H5F3109.5
O21C—C2C—C3C110.0 (6)H5F2—C5F—H5F3109.5
O22C—C2C—C3C106.3 (5)O40F—P10F—O50F119.1 (3)
O21C—C2C—C1C105.8 (5)O40F—P10F—O30F110.7 (3)
O22C—C2C—C1C113.2 (6)O50F—P10F—O30F106.3 (3)
C3C—C2C—C1C109.4 (5)O40F—P10F—O10F110.4 (3)
O3C—C3C—C2C112.4 (6)O50F—P10F—O10F106.1 (3)
O3C—C3C—H3C1109.1O30F—P10F—O10F102.9 (3)
C2C—C3C—H3C1109.1C10F—O10F—P10F117.3 (4)
O3C—C3C—H3C2109.1C40F—O23F—C20F124.1 (8)
C2C—C3C—H3C2109.1C20F—O24F—C50F118.9 (6)
H3C1—C3C—H3C2107.9C30F—O30F—P10F116.1 (5)
O21C—C4C—H4C1109.5O10F—C10F—C20F110.9 (6)
O21C—C4C—H4C2109.5O10F—C10F—H10G109.5
H4C1—C4C—H4C2109.5C20F—C10F—H10G109.5
O21C—C4C—H4C3109.5O10F—C10F—H10H109.5
H4C1—C4C—H4C3109.5C20F—C10F—H10H109.5
H4C2—C4C—H4C3109.5H10G—C10F—H10H108.1
O22C—C5C—H5C1109.5O24F—C20F—O23F111.8 (5)
O22C—C5C—H5C2109.5O24F—C20F—C10F112.6 (6)
H5C1—C5C—H5C2109.5O23F—C20F—C10F105.6 (5)
O22C—C5C—H5C3109.5O24F—C20F—C30F111.4 (6)
H5C1—C5C—H5C3109.5O23F—C20F—C30F107.0 (6)
H5C2—C5C—H5C3109.5C10F—C20F—C30F108.1 (5)
O4D—P1D—O5D119.2 (3)O30F—C30F—C20F112.6 (6)
O4D—P1D—O3D109.5 (3)O30F—C30F—H30G109.1
O5D—P1D—O3D109.4 (3)C20F—C30F—H30G109.1
O4D—P1D—O1D110.0 (3)O30F—C30F—H30H109.1
O5D—P1D—O1D104.6 (3)C20F—C30F—H30H109.1
O3D—P1D—O1D102.8 (2)H30G—C30F—H30H107.8
C1D—O1D—P1D118.5 (4)O23F—C40F—H40M109.5
C4D—O21D—C2D116.0 (6)O23F—C40F—H40N109.5
C2D—O22D—C5D115.8 (6)H40M—C40F—H40N109.5
C3D—O3D—P1D124.5 (5)O23F—C40F—H40O109.5
O1D—C1D—C2D110.0 (6)H40M—C40F—H40O109.5
O1D—C1D—H1D1109.7H40N—C40F—H40O109.5
C2D—C1D—H1D1109.7O24F—C50F—H50J109.5
O1D—C1D—H1D2109.7O24F—C50F—H50K109.5
C2D—C1D—H1D2109.7H50J—C50F—H50K109.5
H1D1—C1D—H1D2108.2O24F—C50F—H50L109.5
O22D—C2D—O21D112.4 (6)H50J—C50F—H50L109.5
O22D—C2D—C3D108.8 (6)H50K—C50F—H50L109.5
O21D—C2D—C3D109.9 (5)H1N—N1—H2N109.5
O22D—C2D—C1D109.5 (6)H1N—N1—H3N109.5
O21D—C2D—C1D104.5 (6)H2N—N1—H3N109.5
C3D—C2D—C1D111.8 (6)H1N—N1—H4N109.5
O3D—C3D—C2D114.6 (6)H2N—N1—H4N109.5
O3D—C3D—H3D1108.6H3N—N1—H4N109.5
C2D—C3D—H3D1108.6H5N—N2—H6N109.4
O3D—C3D—H3D2108.6H5N—N2—H7N109.5
C2D—C3D—H3D2108.6H6N—N2—H7N109.4
H3D1—C3D—H3D2107.6H5N—N2—H8N109.5
O21D—C4D—H4D1109.5H6N—N2—H8N109.4
O21D—C4D—H4D2109.5H7N—N2—H8N109.5
H4D1—C4D—H4D2109.5H9N—N3—H10N109.4
O21D—C4D—H4D3109.5H9N—N3—H11N109.5
H4D1—C4D—H4D3109.5H10N—N3—H11N109.5
H4D2—C4D—H4D3109.5H9N—N3—H12N109.5
O22D—C5D—H5D1109.5H10N—N3—H12N109.5
O22D—C5D—H5D2109.5H11N—N3—H12N109.5
H5D1—C5D—H5D2109.5H13N—N4—H14N109.4
O22D—C5D—H5D3109.5H13N—N4—H15N109.4
H5D1—C5D—H5D3109.5H14N—N4—H15N109.5
H5D2—C5D—H5D3109.5H13N—N4—H16N109.5
O40D—P10D—O50D119.7 (3)H14N—N4—H16N109.5
O40D—P10D—O30D109.2 (3)H15N—N4—H16N109.5
O50D—P10D—O30D109.5 (3)H17N—N5—H18N109.5
O40D—P10D—O10D109.9 (4)H17N—N5—H19N109.5
O50D—P10D—O10D105.1 (3)H18N—N5—H19N109.5
O30D—P10D—O10D102.0 (2)H17N—N5—H20N109.5
C10D—O10D—P10D117.3 (4)H18N—N5—H20N109.4
C40D—O23D—C20D115.8 (6)H19N—N5—H20N109.5
C20D—O24D—C50D116.0 (6)H21N—N6—H22N109.5
C30D—O30D—P10D123.2 (5)H21N—N6—H23N109.5
O10D—C10D—C20D109.9 (6)H22N—N6—H23N109.5
O10D—C10D—H10C109.7H21N—N6—H24N109.5
C20D—C10D—H10C109.7H22N—N6—H24N109.5
O10D—C10D—H10D109.7H23N—N6—H24N109.5
C20D—C10D—H10D109.7
O5A—P1A—O1A—C1A161.0 (5)C1D—C2D—C3D—O3D46.9 (8)
O4A—P1A—O1A—C1A67.3 (5)O40D—P10D—O10D—C10D83.7 (6)
O3A—P1A—O1A—C1A49.8 (5)O50D—P10D—O10D—C10D146.3 (6)
O5A—P1A—O3A—C3A164.2 (5)O30D—P10D—O10D—C10D32.1 (6)
O4A—P1A—O3A—C3A66.0 (5)O40D—P10D—O30D—C30D145.7 (8)
O1A—P1A—O3A—C3A51.6 (5)O50D—P10D—O30D—C30D81.5 (8)
P1A—O1A—C1A—C2A55.3 (6)O10D—P10D—O30D—C30D29.4 (8)
C4A—O21A—C2A—O22A69.8 (9)P10D—O10D—C10D—C20D61.8 (8)
C4A—O21A—C2A—C3A47.3 (9)C50D—O24D—C20D—O23D57.6 (10)
C4A—O21A—C2A—C1A165.7 (7)C50D—O24D—C20D—C30D63.8 (11)
C5A—O22A—C2A—O21A53.9 (9)C50D—O24D—C20D—C10D173.2 (9)
C5A—O22A—C2A—C3A176.0 (7)C40D—O23D—C20D—O24D61.5 (11)
C5A—O22A—C2A—C1A65.8 (8)C40D—O23D—C20D—C30D177.4 (10)
O1A—C1A—C2A—O21A174.9 (5)C40D—O23D—C20D—C10D56.9 (11)
O1A—C1A—C2A—O22A60.8 (7)O10D—C10D—C20D—O24D85.5 (8)
O1A—C1A—C2A—C3A54.3 (6)O10D—C10D—C20D—O23D153.9 (6)
P1A—O3A—C3A—C2A59.6 (6)O10D—C10D—C20D—C30D35.5 (9)
O21A—C2A—C3A—O3A172.4 (5)P10D—O30D—C30D—C20D54.7 (9)
O22A—C2A—C3A—O3A64.9 (6)O24D—C20D—C30D—O30D140.5 (7)
C1A—C2A—C3A—O3A56.4 (6)O23D—C20D—C30D—O30D96.2 (9)
O50A—P10A—O10A—C10A80.1 (10)C10D—C20D—C30D—O30D19.4 (9)
O40A—P10A—O10A—C10A147.9 (10)O4E—P1E—O1E—C1E155.8 (6)
O30A—P10A—O10A—C10A30.9 (10)O5E—P1E—O1E—C1E73.7 (6)
O50A—P10A—O30A—C30A144.8 (9)O3E—P1E—O1E—C1E39.1 (6)
O40A—P10A—O30A—C30A84.8 (9)O4E—P1E—O3E—C3E87.7 (6)
O10A—P10A—O30A—C30A32.5 (9)O5E—P1E—O3E—C3E143.0 (6)
P10A—O10A—C10A—C20A64.4 (8)O1E—P1E—O3E—C3E28.1 (6)
C40A—O23A—C20A—O24A39 (2)P1E—O1E—C1E—C2E69.3 (6)
C40A—O23A—C20A—C30A77.9 (19)C4E—O21E—C2E—O22E60.4 (12)
C40A—O23A—C20A—C10A162.9 (19)C4E—O21E—C2E—C3E56.2 (11)
C50A—O24A—C20A—O23A60 (2)C4E—O21E—C2E—C1E177.6 (9)
C50A—O24A—C20A—C30A178 (2)C5E—O22E—C2E—O21E66.4 (10)
C50A—O24A—C20A—C10A59 (2)C5E—O22E—C2E—C3E174.1 (8)
O10A—C10A—C20A—O23A92.7 (10)C5E—O22E—C2E—C1E53.0 (10)
O10A—C10A—C20A—O24A143.5 (10)O1E—C1E—C2E—O21E90.4 (7)
O10A—C10A—C20A—C30A28.1 (10)O1E—C1E—C2E—O22E147.5 (6)
P10A—O30A—C30A—C20A67.5 (8)O1E—C1E—C2E—C3E30.1 (7)
O23A—C20A—C30A—O30A148.5 (9)P1E—O3E—C3E—C2E64.6 (6)
O24A—C20A—C30A—O30A89.2 (10)O21E—C2E—C3E—O3E150.7 (6)
C10A—C20A—C30A—O30A32.3 (10)O22E—C2E—C3E—O3E88.8 (7)
O5B—P1B—O1B—C1B163.6 (4)C1E—C2E—C3E—O3E32.2 (8)
O4B—P1B—O1B—C1B66.7 (4)O40E—P10E—O10E—C10E61.2 (7)
O3B—P1B—O1B—C1B49.7 (4)O50E—P10E—O10E—C10E168.3 (7)
O5B—P1B—O3B—C3B160.6 (4)O30E—P10E—O10E—C10E55.7 (7)
O4B—P1B—O3B—C3B68.2 (4)O40E—P10E—O30E—C30E62.5 (7)
O1B—P1B—O3B—C3B48.8 (4)O50E—P10E—O30E—C30E168.5 (7)
P1B—O1B—C1B—C2B57.6 (5)O10E—P10E—O30E—C30E53.6 (7)
C5B—O22B—C2B—O21B67.3 (7)P10E—O10E—C10E—C20E61.5 (7)
C5B—O22B—C2B—C1B52.9 (7)C40E—O23E—C20E—O24E69.9 (15)
C5B—O22B—C2B—C3B173.2 (5)C40E—O23E—C20E—C30E46.7 (15)
C4B—O21B—C2B—O22B44.1 (8)C40E—O23E—C20E—C10E167.8 (13)
C40B—O21B—C2B—O22B34 (3)C50E—O24E—C20E—O23E48.2 (17)
C4B—O21B—C2B—C1B171.4 (6)C50E—O24E—C20E—C30E167.5 (15)
C40B—O21B—C2B—C1B93 (3)C50E—O24E—C20E—C10E71.5 (16)
C4B—O21B—C2B—C3B71.1 (7)O10E—C10E—C20E—O23E176.8 (8)
C40B—O21B—C2B—C3B149 (3)O10E—C10E—C20E—O24E60.9 (9)
O1B—C1B—C2B—O22B60.5 (6)O10E—C10E—C20E—C30E56.7 (7)
O1B—C1B—C2B—O21B174.2 (4)P10E—O30E—C30E—C20E55.4 (8)
O1B—C1B—C2B—C3B56.2 (5)O23E—C20E—C30E—O30E171.8 (8)
P1B—O3B—C3B—C2B57.0 (5)O24E—C20E—C30E—O30E67.9 (8)
O22B—C2B—C3B—O3B67.6 (5)C10E—C20E—C30E—O30E53.4 (7)
O21B—C2B—C3B—O3B170.9 (4)O4F—P1F—O1F—C1F69.6 (6)
C1B—C2B—C3B—O3B57.3 (5)O5F—P1F—O1F—C1F160.0 (5)
O5C—P1C—O1C—C1C75.8 (5)O3F—P1F—O1F—C1F48.5 (6)
O4C—P1C—O1C—C1C153.6 (4)O4F—P1F—O3F—C3F68.4 (6)
O3C—P1C—O1C—C1C37.4 (5)O5F—P1F—O3F—C3F160.9 (6)
O5C—P1C—O3C—C3C144.7 (4)O1F—P1F—O3F—C3F49.5 (6)
O4C—P1C—O3C—C3C84.8 (5)P1F—O1F—C1F—C2F56.9 (7)
O1C—P1C—O3C—C3C27.6 (5)C5F—O22F—C2F—O21F70.4 (10)
P1C—O1C—C1C—C2C67.4 (6)C5F—O22F—C2F—C1F48.6 (10)
C4C—O21C—C2C—O22C60.7 (7)C5F—O22F—C2F—C3F170.0 (8)
C4C—O21C—C2C—C3C57.4 (7)C4F—O21F—C2F—O22F43.0 (13)
C4C—O21C—C2C—C1C175.4 (5)C4F—O21F—C2F—C1F166.2 (11)
C5C—O22C—C2C—O21C62.4 (8)C4F—O21F—C2F—C3F78.9 (12)
C5C—O22C—C2C—C3C177.3 (6)O1F—C1F—C2F—O22F65.5 (7)
C5C—O22C—C2C—C1C57.3 (8)O1F—C1F—C2F—O21F171.9 (5)
O1C—C1C—C2C—O21C90.6 (6)O1F—C1F—C2F—C3F57.6 (7)
O1C—C1C—C2C—O22C146.2 (5)P1F—O3F—C3F—C2F59.7 (8)
O1C—C1C—C2C—C3C27.9 (8)O22F—C2F—C3F—O3F63.9 (8)
P1C—O3C—C3C—C2C64.7 (6)O21F—C2F—C3F—O3F173.6 (6)
O21C—C2C—C3C—O3C149.5 (5)C1F—C2F—C3F—O3F60.2 (8)
O22C—C2C—C3C—O3C88.9 (6)O40F—P10F—O10F—C10F68.9 (7)
C1C—C2C—C3C—O3C33.6 (8)O50F—P10F—O10F—C10F160.7 (6)
O4D—P1D—O1D—C1D71.0 (6)O30F—P10F—O10F—C10F49.2 (6)
O5D—P1D—O1D—C1D159.9 (6)O40F—P10F—O30F—C30F68.7 (7)
O3D—P1D—O1D—C1D45.5 (6)O50F—P10F—O30F—C30F160.6 (6)
O4D—P1D—O3D—C3D75.3 (8)O10F—P10F—O30F—C30F49.2 (7)
O5D—P1D—O3D—C3D152.4 (7)P10F—O10F—C10F—C20F57.6 (8)
O1D—P1D—O3D—C3D41.6 (8)C50F—O24F—C20F—O23F57.2 (13)
P1D—O1D—C1D—C2D54.6 (8)C50F—O24F—C20F—C10F175.9 (11)
C5D—O22D—C2D—O21D72.5 (10)C50F—O24F—C20F—C30F62.5 (13)
C5D—O22D—C2D—C3D165.6 (10)C40F—O23F—C20F—O24F64.3 (14)
C5D—O22D—C2D—C1D43.2 (12)C40F—O23F—C20F—C10F58.5 (13)
C4D—O21D—C2D—O22D44.1 (11)C40F—O23F—C20F—C30F173.5 (12)
C4D—O21D—C2D—C3D77.2 (11)O10F—C10F—C20F—O24F66.2 (8)
C4D—O21D—C2D—C1D162.7 (10)O10F—C10F—C20F—O23F171.5 (6)
O1D—C1D—C2D—O22D69.6 (8)O10F—C10F—C20F—C30F57.2 (8)
O1D—C1D—C2D—O21D169.8 (7)P10F—O30F—C30F—C20F58.6 (9)
O1D—C1D—C2D—C3D51.0 (8)O24F—C20F—C30F—O30F65.2 (9)
P1D—O3D—C3D—C2D46.0 (9)O23F—C20F—C30F—O30F172.3 (7)
O22D—C2D—C3D—O3D74.2 (9)C10F—C20F—C30F—O30F59.1 (9)
O21D—C2D—C3D—O3D162.4 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O5B0.901.932.801 (5)163
N1—H2N···O4Ai0.902.022.908 (8)169
N1—H2N···O40Ai0.901.792.685 (18)173
N1—H3N···O4F0.901.902.786 (7)167
N1—H3N···O40F0.901.962.846 (9)167
N1—H4N···O1Fi0.902.593.211 (8)126
N1—H4N···O5Fi0.902.072.961 (11)169
N1—H4N···O50Fi0.901.842.725 (13)166
N2—H5N···O4Aii0.901.952.845 (7)175
N2—H5N···O40Aii0.901.742.622 (15)167
N2—H6N···O5Fi0.901.882.767 (7)168
N2—H6N···O50Fi0.901.892.756 (9)161
N2—H7N···O4E0.901.912.805 (10)173
N2—H7N···O40E0.902.022.909 (14)168
N2—H8N···O1B0.902.553.191 (6)129
N2—H8N···O5B0.902.042.923 (6)166
N3—H9N···O4F0.901.832.717 (9)168
N3—H9N···O40F0.902.173.065 (12)174
N3—H10N···O4B0.901.942.812 (5)162
N3—H11N···O5D0.901.922.801 (7)168
N3—H11N···O50D0.901.932.786 (7)157
N3—H12N···O5A0.901.872.741 (10)162
N3—H12N···O50A0.902.243.12 (2)167
N4—H13N···O5A0.901.862.748 (7)167
N4—H13N···O50A0.901.992.885 (14)175
N4—H14N···O4C0.901.922.822 (6)177
N4—H15N···O4Eiii0.901.802.682 (8)168
N4—H15N···O40Eiii0.902.062.954 (12)170
N4—H16N···O1D0.902.453.082 (7)128
N4—H16N···O5D0.902.153.011 (9)161
N4—H16N···O50D0.901.842.677 (10)154
N5—H17N···O4B0.901.922.797 (6)164
N5—H18N···O4D0.901.962.839 (8)165
N5—H18N···O40D0.901.892.760 (8)161
N5—H19N···O5E0.902.032.900 (10)164
N5—H19N···O50E0.901.802.640 (15)155
N5—H20N···O5Civ0.901.892.786 (6)172
N6—H21N···O4Div0.901.772.667 (9)172
N6—H21N···O40Div0.902.052.947 (10)175
N6—H22N···O4Cii0.901.902.784 (5)169
N6—H23N···O5E0.901.972.842 (8)164
N6—H23N···O50E0.901.802.638 (11)154
N6—H24N···O5Civ0.901.922.815 (6)171
C50D—H50D···O10Eiii0.962.613.424 (15)143
C5F—H5F1···O3Fv0.962.613.391 (13)139
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+1, y, z; (iii) x1, y, z; (iv) x+1/2, y+3/2, z; (v) x1/2, y+1/2, z.
(RTP_new) ammonium 5,5-dimethoxy-2-oxo-1,3,2-dioxaphosphorinan-2-olate top
Crystal data top
C5H10O6P·H4NF(000) = 1368
Mr = 215.14Dx = 1.459 Mg m3
Triclinic, P1Melting point = 444–448 K
a = 11.873 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.569 (6) ÅCell parameters from 11097 reflections
c = 14.218 (5) Åθ = 2.3–38.5°
α = 116.88 (3)°µ = 0.28 mm1
β = 93.62 (3)°T = 290 K
γ = 90.15 (3)°Plate, colourless
V = 2938.8 (18) Å30.45 × 0.16 × 0.06 mm
Z = 12
Data collection top
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
9154 reflections with I > 2σ(I)
Radiation source: Enhance (Mo) X-ray SourceRint = 0.026
ω and phi scansθmax = 30.0°, θmin = 2.3°
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
h = 1616
Tmin = 0.968, Tmax = 1.000k = 1727
35436 measured reflectionsl = 2019
16643 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: mixed
wR(F2) = 0.093H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.036P)2]
where P = (Fo2 + 2Fc2)/3
16643 reflections(Δ/σ)max = 0.001
833 parametersΔρmax = 0.32 e Å3
264 restraintsΔρmin = 0.28 e Å3
Crystal data top
C5H10O6P·H4Nγ = 90.15 (3)°
Mr = 215.14V = 2938.8 (18) Å3
Triclinic, P1Z = 12
a = 11.873 (4) ÅMo Kα radiation
b = 19.569 (6) ŵ = 0.28 mm1
c = 14.218 (5) ÅT = 290 K
α = 116.88 (3)°0.45 × 0.16 × 0.06 mm
β = 93.62 (3)°
Data collection top
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
16643 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
9154 reflections with I > 2σ(I)
Tmin = 0.968, Tmax = 1.000Rint = 0.026
35436 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.040264 restraints
wR(F2) = 0.093H atoms treated by a mixture of independent and constrained refinement
S = 1.00Δρmax = 0.32 e Å3
16643 reflectionsΔρmin = 0.28 e Å3
833 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
P1A0.40977 (3)0.14414 (2)0.33242 (3)0.03680 (10)
O1A0.40385 (9)0.10333 (6)0.20647 (8)0.0420 (3)
O21A0.56192 (10)0.07012 (6)0.15195 (9)0.0544 (3)
O22A0.61932 (9)0.04506 (6)0.15352 (9)0.0469 (3)
O3A0.52859 (8)0.11802 (6)0.36237 (8)0.0420 (3)
O4A0.31633 (9)0.11381 (6)0.36951 (9)0.0459 (3)
O5A0.42175 (9)0.22775 (6)0.37030 (10)0.0517 (3)
C1A0.42688 (13)0.02303 (9)0.15512 (13)0.0439 (4)
H1A10.42140.00460.07910.053*
H1A20.37110.00530.17190.053*
C2A0.54425 (13)0.00932 (8)0.19093 (13)0.0380 (4)
C3A0.55332 (13)0.03821 (8)0.30950 (12)0.0408 (4)
H3A10.50080.00900.32820.049*
H3A20.62910.03090.33230.049*
C4A0.5781 (2)0.11107 (11)0.04357 (16)0.0935 (8)
H4A10.52010.09900.00370.140*
H4A20.57440.16510.02280.140*
H4A30.65070.09710.03010.140*
C5A0.73489 (15)0.05007 (13)0.19038 (19)0.0801 (7)
H5A10.74580.09070.26120.120*
H5A20.78130.06050.14520.120*
H5A30.75550.00240.18960.120*
P1B0.92949 (13)0.24843 (7)0.35572 (9)0.0365 (3)0.800 (3)
O1B1.0327 (2)0.30903 (14)0.38763 (12)0.0425 (10)0.800 (3)
O21B1.05739 (17)0.32173 (14)0.14048 (16)0.0505 (6)0.800 (3)
O22B1.16551 (19)0.25716 (13)0.21563 (16)0.0579 (6)0.800 (3)
O3B0.94427 (16)0.19456 (9)0.23422 (12)0.0534 (5)0.800 (3)
O4B0.82124 (19)0.28829 (15)0.3698 (2)0.0483 (7)0.800 (3)
O5B0.9530 (2)0.20155 (14)0.4124 (2)0.0570 (6)0.800 (3)
C1B1.0445 (2)0.34657 (12)0.32228 (19)0.0404 (11)0.800 (3)
H1B11.10890.38230.34950.049*0.800 (3)
H1B20.97760.37530.32380.049*0.800 (3)
C2B1.0605 (2)0.28825 (12)0.20969 (15)0.0386 (6)0.800 (3)
C3B0.9607 (2)0.23083 (13)0.16780 (16)0.0558 (7)0.800 (3)
H3B10.89280.25700.16340.067*0.800 (3)
H3B20.97350.19200.09710.067*0.800 (3)
C4B1.1284 (3)0.38751 (16)0.1704 (3)0.0560 (7)0.800 (3)
H4B11.09000.43240.21580.084*0.800 (3)
H4B21.14690.39170.10840.084*0.800 (3)
H4B31.19640.38320.20730.084*0.800 (3)
C5B1.2064 (3)0.20287 (17)0.1198 (3)0.0824 (11)0.800 (3)
H5B11.15420.15960.08670.124*0.800 (3)
H5B21.27860.18620.13410.124*0.800 (3)
H5B31.21420.22590.07350.124*0.800 (3)
P10B0.9163 (5)0.2517 (3)0.3510 (4)0.052 (2)*0.200 (3)
O10B1.0254 (7)0.3080 (5)0.3864 (4)0.041 (4)*0.200 (3)
O23B1.0558 (7)0.2993 (5)0.1303 (6)0.052 (3)*0.200 (3)
O24B1.2026 (5)0.2786 (4)0.2307 (6)0.050 (2)*0.200 (3)
O30B0.9131 (4)0.2168 (3)0.2258 (4)0.0384 (18)*0.200 (3)
O40B0.8147 (7)0.2966 (5)0.3914 (7)0.037 (3)*0.200 (3)
O50B0.9432 (9)0.1884 (5)0.3783 (6)0.047 (3)*0.200 (3)
C10B1.0490 (7)0.3415 (3)0.3181 (6)0.041 (4)*0.200 (3)
H10A1.10840.38090.35180.049*0.200 (3)
H10B0.98190.36550.30600.049*0.200 (3)
C20B1.0852 (5)0.2812 (3)0.2135 (5)0.044 (3)*0.200 (3)
C30B1.0209 (5)0.2055 (3)0.1811 (5)0.052 (2)*0.200 (3)
H30A1.00960.17870.10470.062*0.200 (3)
H30B1.06560.17370.20420.062*0.200 (3)
C40B1.0958 (16)0.3711 (7)0.1421 (12)0.096 (6)*0.200 (3)
H40A1.07070.37720.08090.145*0.200 (3)
H40B1.17690.37350.14960.145*0.200 (3)
H40C1.06710.41140.20390.145*0.200 (3)
C50B1.2600 (7)0.2241 (6)0.1459 (8)0.069 (4)*0.200 (3)
H50A1.33910.22750.16670.104*0.200 (3)
H50B1.24930.23420.08600.104*0.200 (3)
H50C1.23060.17350.12750.104*0.200 (3)
P1C0.42809 (8)0.49192 (5)0.35245 (7)0.0348 (3)0.890 (3)
O1C0.43792 (13)0.46375 (9)0.22938 (10)0.0487 (4)0.890 (3)
O21C0.55104 (15)0.27544 (9)0.13794 (16)0.0534 (5)0.890 (3)
O22C0.65860 (14)0.39001 (8)0.20384 (13)0.0588 (5)0.890 (3)
O3C0.53399 (16)0.45392 (12)0.38260 (11)0.0416 (7)0.890 (3)
O4C0.32179 (15)0.46151 (16)0.3708 (2)0.0459 (6)0.890 (3)
O5C0.4511 (2)0.57625 (8)0.4062 (2)0.0528 (6)0.890 (3)
C1C0.45276 (17)0.38356 (11)0.16496 (14)0.0503 (6)0.890 (3)
H1C10.46140.37420.09280.060*0.890 (3)
H1C20.38590.35490.16490.060*0.890 (3)
C2C0.55556 (18)0.35512 (10)0.20453 (15)0.0386 (5)0.890 (3)
C3C0.54642 (19)0.37326 (13)0.31882 (17)0.0411 (7)0.890 (3)
H3C10.48180.34520.32450.049*0.890 (3)
H3C20.61360.35700.34450.049*0.890 (3)
C4C0.6257 (3)0.23066 (12)0.1680 (2)0.0665 (8)0.890 (3)
H4C10.61540.17760.11760.100*0.890 (3)
H4C20.60960.23680.23670.100*0.890 (3)
H4C30.70230.24740.17010.100*0.890 (3)
C5C0.6932 (3)0.37869 (15)0.1053 (2)0.0927 (10)0.890 (3)
H5C10.69800.32480.06000.139*0.890 (3)
H5C20.76580.40350.11490.139*0.890 (3)
H5C30.63930.40000.07360.139*0.890 (3)
P10C0.4202 (9)0.4872 (6)0.3513 (7)0.071 (4)*0.110 (3)
O10C0.4179 (7)0.4383 (5)0.2261 (7)0.041 (3)*0.110 (3)
O23C0.5560 (11)0.2916 (5)0.1374 (11)0.041 (3)*0.110 (3)
O24C0.7066 (7)0.3783 (6)0.2292 (8)0.052 (3)*0.110 (3)
O30C0.5305 (10)0.4568 (9)0.3884 (6)0.038 (5)*0.110 (3)
O40C0.3189 (11)0.4684 (12)0.3917 (12)0.033 (5)*0.110 (3)
O50C0.4451 (17)0.5685 (5)0.3769 (11)0.040 (5)*0.110 (3)
C10C0.5251 (8)0.4186 (6)0.1815 (7)0.050 (4)*0.110 (3)
H10C0.57050.46510.20230.060*0.110 (3)
H10D0.51340.39350.10500.060*0.110 (3)
C20C0.5890 (7)0.3658 (5)0.2166 (7)0.041 (3)*0.110 (3)
C30C0.5563 (11)0.3783 (8)0.3239 (10)0.035 (5)*0.110 (3)
H30C0.49090.34560.31530.042*0.110 (3)
H30D0.61790.36400.35890.042*0.110 (3)
C40C0.620 (2)0.2298 (6)0.136 (2)0.076 (8)*0.110 (3)
H40D0.59360.18290.07630.114*0.110 (3)
H40E0.61150.22560.20000.114*0.110 (3)
H40F0.69830.23910.13090.114*0.110 (3)
C50C0.7615 (10)0.3711 (12)0.1406 (12)0.075 (6)*0.110 (3)
H50D0.84100.38150.15920.112*0.110 (3)
H50E0.73170.40690.11730.112*0.110 (3)
H50F0.74920.31990.08470.112*0.110 (3)
P1D0.91600 (3)0.57801 (2)0.34239 (3)0.03660 (10)
O1D1.03339 (8)0.62561 (6)0.36902 (8)0.0419 (3)
O21D1.05401 (10)0.67122 (7)0.15320 (10)0.0561 (3)
O22D1.12185 (9)0.56043 (6)0.15796 (9)0.0501 (3)
O3D0.91077 (9)0.53209 (6)0.21674 (8)0.0428 (3)
O4D0.82035 (9)0.63049 (6)0.37550 (9)0.0439 (3)
O5D0.93200 (9)0.52260 (6)0.38592 (10)0.0518 (3)
C1D1.05299 (13)0.66912 (9)0.31309 (12)0.0404 (4)
H1D11.12780.69350.33450.049*
H1D20.99840.70910.33090.049*
C2D1.04336 (13)0.61847 (9)0.19510 (12)0.0380 (4)
C3D0.92808 (13)0.57735 (9)0.16191 (13)0.0449 (4)
H3D10.86970.61480.17750.054*
H3D20.92250.54430.08630.054*
C4D1.0685 (2)0.64142 (14)0.04657 (18)0.1029 (9)
H4D11.14090.61860.03230.154*
H4D21.06460.68170.02580.154*
H4D31.01010.60320.00740.154*
C5D1.23675 (16)0.58258 (13)0.19260 (19)0.0850 (7)
H5D11.25510.62800.18600.127*
H5D21.28390.54200.15000.127*
H5D31.24910.59280.26520.127*
P1E0.41657 (4)0.81139 (2)0.34746 (4)0.04214 (11)
O1E0.40840 (9)0.76842 (7)0.22186 (9)0.0525 (3)
O21E0.55273 (10)0.62840 (7)0.10940 (10)0.0611 (3)
O22E0.69942 (10)0.71615 (7)0.20537 (10)0.0568 (3)
O3E0.52916 (9)0.77669 (6)0.37414 (9)0.0477 (3)
O4E0.31579 (9)0.78616 (7)0.38136 (10)0.0532 (3)
O5E0.44041 (10)0.89460 (6)0.39035 (10)0.0606 (3)
C1E0.51453 (15)0.75901 (10)0.17554 (14)0.0546 (5)
H1E10.55660.80770.20630.066*
H1E20.50180.74200.10010.066*
C2E0.58227 (14)0.69996 (10)0.19535 (14)0.0446 (4)
C3E0.55372 (14)0.70137 (10)0.29957 (14)0.0512 (5)
H3E10.48900.66720.28710.061*
H3E20.61710.68330.32760.061*
C4E0.60150 (18)0.56389 (11)0.11729 (19)0.0863 (7)
H4E10.67730.57740.14880.129*
H4E20.60240.52150.04800.129*
H4E30.55730.54970.16040.129*
C5E0.74319 (17)0.72064 (13)0.11749 (18)0.0821 (7)
H5E10.72380.67410.05440.123*
H5E20.82390.72770.12850.123*
H5E30.71150.76320.11020.123*
P1F0.90603 (3)0.92163 (2)0.34103 (4)0.03922 (11)
O1F0.89452 (9)0.88590 (6)0.21557 (9)0.0493 (3)
O21F1.04941 (10)0.94776 (7)0.10488 (10)0.0612 (3)
O22F1.19096 (10)0.91508 (7)0.19679 (10)0.0605 (3)
O3F1.02340 (9)0.96954 (6)0.36764 (9)0.0455 (3)
O4F0.80974 (9)0.97289 (6)0.38012 (9)0.0501 (3)
O5F0.92409 (10)0.86278 (6)0.37802 (10)0.0537 (3)
C1F0.99909 (15)0.86069 (10)0.16731 (14)0.0540 (5)
H1F10.98430.82970.09170.065*
H1F21.03670.82940.19580.065*
C2F1.07553 (13)0.93000 (10)0.18864 (14)0.0452 (4)
C3F1.05232 (14)0.99704 (9)0.29491 (14)0.0484 (4)
H3F11.11891.03080.32330.058*
H3F20.99091.02620.28480.058*
C4F1.10462 (18)1.01607 (13)0.11398 (19)0.0876 (8)
H4F11.06871.06020.16420.131*
H4F21.09951.01620.04640.131*
H4F31.18261.01750.13740.131*
C5F1.23079 (18)0.85228 (12)0.10938 (19)0.0932 (8)
H5F11.20170.80550.10650.140*
H5F21.31180.85330.11630.140*
H5F31.20610.85510.04570.140*
N10.86314 (12)0.12792 (8)0.51519 (12)0.0481 (4)
H1N0.88360.14990.47490.057 (5)*
H2N0.84230.07860.47210.063 (6)*
H3N0.92480.12960.55650.072 (6)*
H4N0.80270.15220.54900.081 (7)*
N20.63893 (12)0.28272 (7)0.48559 (11)0.0448 (3)
H5N0.70130.28420.45370.059 (5)*
H6N0.57900.25850.44030.066 (6)*
H7N0.65770.26220.52950.070 (6)*
H8N0.61680.33070.52550.056 (5)*
N30.84780 (11)0.45257 (8)0.49975 (11)0.0444 (3)
H9N0.83360.40230.45740.066 (6)*
H10N0.86500.47540.45960.059 (5)*
H11N0.91180.46100.54150.079 (7)*
H12N0.78520.47230.53340.053 (5)*
N40.66436 (12)0.62767 (8)0.51377 (12)0.0489 (4)
H13N0.72220.62610.47490.053 (5)*
H14N0.60030.60900.47190.080 (7)*
H15N0.65190.67730.55640.083 (7)*
H16N0.68140.60310.55280.082 (7)*
N50.83748 (13)0.79113 (8)0.48941 (12)0.0529 (4)
H17N0.85310.81400.44900.071 (6)*
H18N0.82020.74100.44840.094 (8)*
H19N0.90190.79550.52910.081 (7)*
H20N0.77800.81280.52700.065 (6)*
N60.64709 (13)0.96078 (8)0.50411 (13)0.0526 (4)
H21N0.70620.96080.46740.074 (6)*
H22N0.58630.93390.46220.075 (7)*
H23N0.66470.94030.54830.068 (6)*
H24N0.62821.00950.54410.081 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P1A0.0347 (2)0.0318 (2)0.0446 (3)0.00786 (18)0.01067 (18)0.0169 (2)
O1A0.0430 (6)0.0422 (6)0.0440 (7)0.0122 (5)0.0063 (5)0.0221 (6)
O21A0.0749 (9)0.0322 (6)0.0551 (8)0.0138 (6)0.0257 (7)0.0161 (6)
O22A0.0422 (7)0.0482 (7)0.0586 (8)0.0050 (5)0.0170 (6)0.0299 (6)
O3A0.0382 (6)0.0380 (6)0.0425 (7)0.0098 (5)0.0038 (5)0.0116 (5)
O4A0.0411 (6)0.0440 (7)0.0556 (7)0.0070 (5)0.0169 (5)0.0235 (6)
O5A0.0517 (7)0.0329 (6)0.0694 (8)0.0105 (5)0.0161 (6)0.0206 (6)
C1A0.0441 (10)0.0410 (10)0.0417 (10)0.0013 (8)0.0035 (8)0.0145 (8)
C2A0.0414 (9)0.0294 (8)0.0432 (10)0.0058 (7)0.0129 (7)0.0153 (8)
C3A0.0423 (9)0.0389 (9)0.0451 (10)0.0134 (7)0.0107 (7)0.0213 (8)
C4A0.143 (2)0.0506 (13)0.0672 (16)0.0235 (14)0.0385 (15)0.0052 (12)
C5A0.0442 (12)0.1051 (18)0.1057 (19)0.0071 (12)0.0118 (12)0.0600 (16)
P1B0.0388 (4)0.0347 (5)0.0424 (5)0.0056 (3)0.0165 (3)0.0212 (4)
O1B0.0424 (13)0.0529 (14)0.0364 (12)0.0003 (7)0.0091 (6)0.0231 (9)
O21B0.0557 (11)0.0590 (14)0.0506 (11)0.0031 (10)0.0083 (8)0.0366 (10)
O22B0.0487 (12)0.0701 (14)0.0662 (12)0.0275 (12)0.0275 (10)0.0377 (11)
O3B0.0676 (12)0.0410 (10)0.0506 (10)0.0025 (9)0.0203 (8)0.0180 (8)
O4B0.0402 (11)0.0534 (13)0.0561 (15)0.0092 (8)0.0194 (9)0.0270 (11)
O5B0.0684 (14)0.0577 (13)0.0640 (16)0.0126 (10)0.0203 (13)0.0423 (14)
C1B0.0412 (15)0.0362 (14)0.0459 (16)0.0007 (9)0.0139 (10)0.0191 (11)
C2B0.0394 (12)0.0452 (13)0.0399 (13)0.0085 (10)0.0104 (9)0.0258 (11)
C3B0.0649 (16)0.0610 (15)0.0377 (13)0.0121 (13)0.0083 (11)0.0185 (12)
C4B0.0557 (18)0.0638 (17)0.069 (2)0.0029 (14)0.0125 (15)0.0470 (16)
C5B0.092 (3)0.076 (2)0.092 (2)0.044 (2)0.058 (2)0.0430 (19)
P1C0.0375 (3)0.0313 (3)0.0378 (4)0.0098 (2)0.0144 (2)0.0161 (2)
O1C0.0614 (10)0.0469 (10)0.0436 (8)0.0195 (8)0.0171 (7)0.0238 (7)
O21C0.0556 (10)0.0342 (8)0.0542 (10)0.0097 (8)0.0079 (7)0.0055 (8)
O22C0.0465 (10)0.0578 (9)0.0657 (10)0.0035 (8)0.0269 (8)0.0196 (8)
O3C0.0425 (9)0.0390 (9)0.0356 (9)0.0104 (6)0.0067 (6)0.0096 (6)
O4C0.0405 (10)0.0445 (11)0.0515 (13)0.0078 (6)0.0174 (8)0.0190 (10)
O5C0.0646 (12)0.0328 (8)0.0586 (14)0.0080 (7)0.0173 (11)0.0170 (8)
C1C0.0555 (13)0.0518 (13)0.0358 (11)0.0144 (10)0.0068 (9)0.0125 (10)
C2C0.0356 (11)0.0332 (10)0.0409 (11)0.0031 (8)0.0104 (9)0.0104 (9)
C3C0.0424 (12)0.0381 (12)0.0432 (13)0.0120 (9)0.0101 (9)0.0178 (9)
C4C0.0774 (18)0.0468 (14)0.068 (2)0.0271 (12)0.0174 (15)0.0175 (12)
C5C0.103 (2)0.0822 (18)0.099 (2)0.0102 (17)0.066 (2)0.0398 (17)
P1D0.0366 (2)0.0363 (2)0.0439 (3)0.00471 (18)0.01316 (19)0.0230 (2)
O1D0.0395 (6)0.0524 (7)0.0409 (6)0.0035 (5)0.0056 (5)0.0269 (6)
O21D0.0705 (9)0.0591 (8)0.0584 (8)0.0137 (6)0.0259 (7)0.0413 (7)
O22D0.0437 (7)0.0483 (7)0.0635 (8)0.0139 (6)0.0199 (6)0.0278 (6)
O3D0.0460 (7)0.0356 (6)0.0450 (7)0.0044 (5)0.0100 (5)0.0159 (6)
O4D0.0418 (6)0.0438 (6)0.0536 (7)0.0107 (5)0.0184 (5)0.0268 (6)
O5D0.0558 (7)0.0510 (7)0.0671 (8)0.0097 (6)0.0197 (6)0.0409 (7)
C1D0.0408 (9)0.0400 (9)0.0433 (10)0.0013 (7)0.0107 (7)0.0203 (8)
C2D0.0412 (9)0.0400 (9)0.0413 (10)0.0069 (7)0.0141 (7)0.0243 (8)
C3D0.0452 (10)0.0516 (10)0.0394 (10)0.0019 (8)0.0056 (8)0.0216 (9)
C4D0.149 (3)0.115 (2)0.0779 (18)0.0278 (18)0.0455 (17)0.0683 (17)
C5D0.0451 (13)0.0994 (18)0.1055 (19)0.0198 (12)0.0081 (12)0.0417 (16)
P1E0.0405 (2)0.0408 (3)0.0511 (3)0.0105 (2)0.0147 (2)0.0246 (2)
O1E0.0463 (7)0.0652 (8)0.0526 (8)0.0184 (6)0.0089 (6)0.0319 (7)
O21E0.0589 (8)0.0496 (8)0.0664 (9)0.0048 (6)0.0048 (7)0.0188 (7)
O22E0.0441 (7)0.0572 (8)0.0712 (9)0.0008 (6)0.0122 (6)0.0298 (7)
O3E0.0479 (7)0.0503 (7)0.0436 (7)0.0132 (6)0.0074 (5)0.0197 (6)
O4E0.0436 (7)0.0558 (7)0.0696 (9)0.0095 (6)0.0199 (6)0.0347 (7)
O5E0.0661 (9)0.0416 (7)0.0778 (9)0.0097 (6)0.0232 (7)0.0280 (7)
C1E0.0617 (12)0.0614 (12)0.0499 (11)0.0191 (10)0.0202 (9)0.0311 (10)
C2E0.0410 (10)0.0479 (10)0.0472 (10)0.0105 (8)0.0108 (8)0.0226 (9)
C3E0.0492 (11)0.0534 (11)0.0590 (12)0.0144 (9)0.0099 (9)0.0317 (10)
C4E0.0782 (16)0.0424 (12)0.124 (2)0.0060 (11)0.0062 (14)0.0254 (13)
C5E0.0669 (14)0.0924 (17)0.1056 (19)0.0056 (12)0.0361 (13)0.0573 (15)
P1F0.0357 (2)0.0400 (2)0.0450 (3)0.00117 (19)0.00905 (19)0.0211 (2)
O1F0.0424 (7)0.0543 (7)0.0465 (7)0.0106 (6)0.0046 (5)0.0186 (6)
O21F0.0584 (8)0.0740 (9)0.0631 (9)0.0050 (7)0.0042 (7)0.0416 (8)
O22F0.0460 (8)0.0611 (8)0.0767 (9)0.0108 (6)0.0171 (7)0.0316 (8)
O3F0.0429 (7)0.0501 (7)0.0415 (7)0.0074 (5)0.0046 (5)0.0189 (6)
O4F0.0408 (7)0.0526 (7)0.0630 (8)0.0104 (6)0.0160 (6)0.0299 (6)
O5F0.0542 (8)0.0512 (7)0.0677 (9)0.0055 (6)0.0130 (6)0.0361 (7)
C1F0.0598 (12)0.0489 (11)0.0466 (11)0.0013 (9)0.0182 (9)0.0139 (9)
C2F0.0401 (10)0.0489 (11)0.0480 (11)0.0011 (8)0.0102 (8)0.0223 (9)
C3F0.0459 (10)0.0428 (10)0.0555 (12)0.0062 (8)0.0078 (8)0.0209 (9)
C4F0.0790 (16)0.1013 (18)0.119 (2)0.0148 (14)0.0010 (14)0.0834 (18)
C5F0.0699 (16)0.0825 (17)0.114 (2)0.0232 (13)0.0388 (15)0.0292 (16)
N10.0423 (9)0.0460 (10)0.0660 (10)0.0088 (7)0.0170 (8)0.0325 (9)
N20.0420 (8)0.0384 (8)0.0574 (9)0.0049 (7)0.0138 (8)0.0235 (8)
N30.0433 (9)0.0409 (9)0.0587 (9)0.0108 (7)0.0209 (8)0.0288 (8)
N40.0489 (9)0.0407 (9)0.0663 (10)0.0138 (7)0.0294 (9)0.0290 (8)
N50.0518 (10)0.0418 (9)0.0758 (11)0.0144 (7)0.0335 (9)0.0323 (9)
N60.0491 (10)0.0483 (9)0.0750 (11)0.0142 (8)0.0274 (9)0.0377 (9)
Geometric parameters (Å, º) top
P1A—O5A1.4764 (12)C10C—H10D0.9700
P1A—O4A1.4882 (12)C20C—C30C1.508 (3)
P1A—O1A1.5938 (13)C30C—H30C0.9700
P1A—O3A1.5993 (11)C30C—H30D0.9700
O1A—C1A1.4378 (18)C40C—H40D0.9600
O21A—C4A1.405 (2)C40C—H40E0.9600
O21A—C2A1.4161 (18)C40C—H40F0.9600
O22A—C2A1.3998 (18)C50C—H50D0.9600
O22A—C5A1.424 (2)C50C—H50E0.9600
O3A—C3A1.4349 (18)C50C—H50F0.9600
C1A—C2A1.519 (2)P1D—O5D1.4793 (11)
C1A—H1A10.9700P1D—O4D1.4840 (12)
C1A—H1A20.9700P1D—O3D1.5928 (14)
C2A—C3A1.513 (2)P1D—O1D1.6003 (12)
C3A—H3A10.9700O1D—C1D1.4304 (17)
C3A—H3A20.9700O21D—C4D1.379 (2)
C4A—H4A10.9600O21D—C2D1.4147 (17)
C4A—H4A20.9600O22D—C2D1.4008 (17)
C4A—H4A30.9600O22D—C5D1.418 (2)
C5A—H5A10.9600O3D—C3D1.4416 (17)
C5A—H5A20.9600C1D—C2D1.511 (2)
C5A—H5A30.9600C1D—H1D10.9700
P1B—O4B1.4822 (16)C1D—H1D20.9700
P1B—O5B1.4871 (15)C2D—C3D1.521 (2)
P1B—O3B1.5870 (15)C3D—H3D10.9700
P1B—O1B1.5970 (15)C3D—H3D20.9700
O1B—C1B1.4337 (18)C4D—H4D10.9600
O21B—C2B1.406 (2)C4D—H4D20.9600
O21B—C4B1.415 (3)C4D—H4D30.9600
O22B—C2B1.403 (3)C5D—H5D10.9600
O22B—C5B1.414 (2)C5D—H5D20.9600
O3B—C3B1.436 (2)C5D—H5D30.9600
C1B—C2B1.513 (2)P1E—O5E1.4769 (13)
C1B—H1B10.9700P1E—O4E1.4809 (12)
C1B—H1B20.9700P1E—O1E1.5892 (14)
C2B—C3B1.523 (3)P1E—O3E1.6018 (12)
C3B—H3B10.9700O1E—C1E1.4324 (19)
C3B—H3B20.9700O21E—C2E1.405 (2)
C4B—H4B10.9600O21E—C4E1.437 (2)
C4B—H4B20.9600O22E—C2E1.410 (2)
C4B—H4B30.9600O22E—C5E1.421 (2)
C5B—H5B10.9600O3E—C3E1.418 (2)
C5B—H5B20.9600C1E—C2E1.527 (2)
C5B—H5B30.9600C1E—H1E10.9700
P10B—O40B1.481 (2)C1E—H1E20.9700
P10B—O50B1.485 (2)C2E—C3E1.529 (2)
P10B—O30B1.590 (2)C3E—H3E10.9700
P10B—O10B1.599 (2)C3E—H3E20.9700
O10B—C10B1.435 (2)C4E—H4E10.9600
O23B—C20B1.407 (3)C4E—H4E20.9600
O23B—C40B1.414 (3)C4E—H4E30.9600
O24B—C20B1.404 (3)C5E—H5E10.9600
O24B—C50B1.414 (3)C5E—H5E20.9600
O30B—C30B1.438 (3)C5E—H5E30.9600
C10B—C20B1.512 (3)P1F—O5F1.4776 (11)
C10B—H10A0.9700P1F—O4F1.4846 (12)
C10B—H10B0.9700P1F—O1F1.5908 (14)
C20B—C30B1.523 (3)P1F—O3F1.6031 (13)
C30B—H30A0.9700O1F—C1F1.4354 (19)
C30B—H30B0.9700O21F—C2F1.4013 (19)
C40B—H40A0.9600O21F—C4F1.436 (2)
C40B—H40B0.9600O22F—C5F1.405 (2)
C40B—H40C0.9600O22F—C2F1.4105 (19)
C50B—H50A0.9600O3F—C3F1.4227 (18)
C50B—H50B0.9600C1F—C2F1.530 (2)
C50B—H50C0.9600C1F—H1F10.9700
P1C—O4C1.4807 (14)C1F—H1F20.9700
P1C—O5C1.4876 (15)C2F—C3F1.530 (2)
P1C—O1C1.5916 (14)C3F—H3F10.9700
P1C—O3C1.5946 (12)C3F—H3F20.9700
O1C—C1C1.433 (2)C4F—H4F10.9600
O21C—C2C1.410 (2)C4F—H4F20.9600
O21C—C4C1.425 (2)C4F—H4F30.9600
O22C—C2C1.402 (2)C5F—H5F10.9600
O22C—C5C1.405 (2)C5F—H5F20.9600
O3C—C3C1.4350 (19)C5F—H5F30.9600
C1C—C2C1.522 (2)N1—H1N0.9000
C1C—H1C10.9700N1—H2N0.9013
C1C—H1C20.9700N1—H3N0.8997
C2C—C3C1.510 (2)N1—H4N0.9000
C3C—H3C10.9700N2—H5N0.8994
C3C—H3C20.9700N2—H6N0.9000
C4C—H4C10.9600N2—H7N0.9002
C4C—H4C20.9600N2—H8N0.8998
C4C—H4C30.9600N3—H9N0.8992
C5C—H5C10.9600N3—H10N0.9005
C5C—H5C20.9600N3—H11N0.9003
C5C—H5C30.9600N3—H12N0.8995
P10C—O40C1.480 (2)N4—H13N0.9001
P10C—O50C1.486 (2)N4—H14N0.9012
P10C—O10C1.593 (2)N4—H15N0.9005
P10C—O30C1.596 (2)N4—H16N0.8998
O10C—C10C1.433 (3)N5—H17N0.8993
O23C—C20C1.411 (3)N5—H18N0.9000
O23C—C40C1.425 (3)N5—H19N0.9012
O24C—C20C1.403 (3)N5—H20N0.8999
O24C—C50C1.405 (3)N6—H21N0.9013
O30C—C30C1.435 (3)N6—H22N0.9010
C10C—C20C1.521 (3)N6—H23N0.9009
C10C—H10C0.9700N6—H24N0.8991
O5A—P1A—O4A118.63 (7)O23C—C20C—C30C111.6 (3)
O5A—P1A—O1A108.40 (7)O24C—C20C—C10C114.2 (3)
O4A—P1A—O1A109.92 (7)O23C—C20C—C10C103.7 (3)
O5A—P1A—O3A106.10 (7)C30C—C20C—C10C110.6 (2)
O4A—P1A—O3A110.09 (6)O30C—C30C—C20C111.3 (3)
O1A—P1A—O3A102.45 (7)O30C—C30C—H30C109.4
C1A—O1A—P1A116.85 (9)C20C—C30C—H30C109.4
C4A—O21A—C2A116.38 (13)O30C—C30C—H30D109.4
C2A—O22A—C5A116.34 (13)C20C—C30C—H30D109.4
C3A—O3A—P1A118.21 (10)H30C—C30C—H30D108.0
O1A—C1A—C2A110.51 (13)O23C—C40C—H40D109.5
O1A—C1A—H1A1109.5O23C—C40C—H40E109.5
C2A—C1A—H1A1109.5H40D—C40C—H40E109.5
O1A—C1A—H1A2109.5O23C—C40C—H40F109.5
C2A—C1A—H1A2109.5H40D—C40C—H40F109.5
H1A1—C1A—H1A2108.1H40E—C40C—H40F109.5
O22A—C2A—O21A112.63 (12)O24C—C50C—H50D109.5
O22A—C2A—C3A115.01 (14)O24C—C50C—H50E109.5
O21A—C2A—C3A103.02 (12)H50D—C50C—H50E109.5
O22A—C2A—C1A105.67 (12)O24C—C50C—H50F109.5
O21A—C2A—C1A110.85 (14)H50D—C50C—H50F109.5
C3A—C2A—C1A109.77 (13)H50E—C50C—H50F109.5
O3A—C3A—C2A110.56 (11)O5D—P1D—O4D118.86 (7)
O3A—C3A—H3A1109.5O5D—P1D—O3D108.39 (7)
C2A—C3A—H3A1109.5O4D—P1D—O3D109.82 (7)
O3A—C3A—H3A2109.5O5D—P1D—O1D105.72 (7)
C2A—C3A—H3A2109.5O4D—P1D—O1D110.64 (7)
H3A1—C3A—H3A2108.1O3D—P1D—O1D102.04 (7)
O21A—C4A—H4A1109.5C1D—O1D—P1D117.76 (10)
O21A—C4A—H4A2109.5C4D—O21D—C2D117.20 (15)
H4A1—C4A—H4A2109.5C2D—O22D—C5D116.78 (14)
O21A—C4A—H4A3109.5C3D—O3D—P1D115.91 (10)
H4A1—C4A—H4A3109.5O1D—C1D—C2D110.96 (12)
H4A2—C4A—H4A3109.5O1D—C1D—H1D1109.4
O22A—C5A—H5A1109.5C2D—C1D—H1D1109.4
O22A—C5A—H5A2109.5O1D—C1D—H1D2109.4
H5A1—C5A—H5A2109.5C2D—C1D—H1D2109.4
O22A—C5A—H5A3109.5H1D1—C1D—H1D2108.0
H5A1—C5A—H5A3109.5O22D—C2D—O21D112.62 (12)
H5A2—C5A—H5A3109.5O22D—C2D—C1D115.29 (13)
O4B—P1B—O5B118.64 (9)O21D—C2D—C1D103.19 (13)
O4B—P1B—O3B110.78 (12)O22D—C2D—C3D105.43 (13)
O5B—P1B—O3B106.91 (12)O21D—C2D—C3D110.76 (13)
O4B—P1B—O1B109.85 (9)C1D—C2D—C3D109.62 (13)
O5B—P1B—O1B106.95 (10)O3D—C3D—C2D110.80 (12)
O3B—P1B—O1B102.42 (8)O3D—C3D—H3D1109.5
C1B—O1B—P1B116.82 (12)C2D—C3D—H3D1109.5
C2B—O21B—C4B116.65 (16)O3D—C3D—H3D2109.5
C2B—O22B—C5B117.4 (2)C2D—C3D—H3D2109.5
C3B—O3B—P1B117.54 (14)H3D1—C3D—H3D2108.1
O1B—C1B—C2B110.31 (14)O21D—C4D—H4D1109.5
O1B—C1B—H1B1109.6O21D—C4D—H4D2109.5
C2B—C1B—H1B1109.6H4D1—C4D—H4D2109.5
O1B—C1B—H1B2109.6O21D—C4D—H4D3109.5
C2B—C1B—H1B2109.6H4D1—C4D—H4D3109.5
H1B1—C1B—H1B2108.1H4D2—C4D—H4D3109.5
O22B—C2B—O21B112.27 (15)O22D—C5D—H5D1109.5
O22B—C2B—C1B104.43 (17)O22D—C5D—H5D2109.5
O21B—C2B—C1B111.93 (16)H5D1—C5D—H5D2109.5
O22B—C2B—C3B115.20 (19)O22D—C5D—H5D3109.5
O21B—C2B—C3B103.58 (18)H5D1—C5D—H5D3109.5
C1B—C2B—C3B109.63 (16)H5D2—C5D—H5D3109.5
O3B—C3B—C2B111.88 (17)O5E—P1E—O4E117.94 (8)
O3B—C3B—H3B1109.2O5E—P1E—O1E112.62 (7)
C2B—C3B—H3B1109.2O4E—P1E—O1E106.78 (8)
O3B—C3B—H3B2109.2O5E—P1E—O3E105.99 (8)
C2B—C3B—H3B2109.2O4E—P1E—O3E111.29 (7)
H3B1—C3B—H3B2107.9O1E—P1E—O3E100.97 (7)
O21B—C4B—H4B1109.5C1E—O1E—P1E114.68 (11)
O21B—C4B—H4B2109.5C2E—O21E—C4E114.88 (15)
H4B1—C4B—H4B2109.5C2E—O22E—C5E115.12 (15)
O21B—C4B—H4B3109.5C3E—O3E—P1E116.24 (11)
H4B1—C4B—H4B3109.5O1E—C1E—C2E109.64 (13)
H4B2—C4B—H4B3109.5O1E—C1E—H1E1109.7
O22B—C5B—H5B1109.5C2E—C1E—H1E1109.7
O22B—C5B—H5B2109.5O1E—C1E—H1E2109.7
H5B1—C5B—H5B2109.5C2E—C1E—H1E2109.7
O22B—C5B—H5B3109.5H1E1—C1E—H1E2108.2
H5B1—C5B—H5B3109.5O21E—C2E—O22E111.46 (14)
H5B2—C5B—H5B3109.5O21E—C2E—C1E106.29 (14)
O40B—P10B—O50B119.2 (2)O22E—C2E—C1E111.76 (14)
O40B—P10B—O30B110.6 (2)O21E—C2E—C3E111.06 (14)
O50B—P10B—O30B107.1 (2)O22E—C2E—C3E105.96 (14)
O40B—P10B—O10B109.7 (2)C1E—C2E—C3E110.38 (13)
O50B—P10B—O10B107.3 (2)O3E—C3E—C2E110.56 (13)
O30B—P10B—O10B101.43 (18)O3E—C3E—H3E1109.5
C10B—O10B—P10B115.8 (3)C2E—C3E—H3E1109.5
C20B—O23B—C40B116.8 (4)O3E—C3E—H3E2109.5
C20B—O24B—C50B116.9 (4)C2E—C3E—H3E2109.5
C30B—O30B—P10B116.1 (3)H3E1—C3E—H3E2108.1
O10B—C10B—C20B110.7 (3)O21E—C4E—H4E1109.5
O10B—C10B—H10A109.5O21E—C4E—H4E2109.5
C20B—C10B—H10A109.5H4E1—C4E—H4E2109.5
O10B—C10B—H10B109.5O21E—C4E—H4E3109.5
C20B—C10B—H10B109.5H4E1—C4E—H4E3109.5
H10A—C10B—H10B108.1H4E2—C4E—H4E3109.5
O24B—C20B—O23B112.4 (3)O22E—C5E—H5E1109.5
O24B—C20B—C10B104.2 (3)O22E—C5E—H5E2109.5
O23B—C20B—C10B112.0 (3)H5E1—C5E—H5E2109.5
O24B—C20B—C30B114.6 (3)O22E—C5E—H5E3109.5
O23B—C20B—C30B103.5 (3)H5E1—C5E—H5E3109.5
C10B—C20B—C30B110.4 (2)H5E2—C5E—H5E3109.5
O30B—C30B—C20B112.0 (3)O5F—P1F—O4F118.02 (7)
O30B—C30B—H30A109.2O5F—P1F—O1F112.41 (8)
C20B—C30B—H30A109.2O4F—P1F—O1F106.68 (7)
O30B—C30B—H30B109.2O5F—P1F—O3F106.06 (7)
C20B—C30B—H30B109.2O4F—P1F—O3F111.50 (7)
H30A—C30B—H30B107.9O1F—P1F—O3F100.90 (7)
O23B—C40B—H40A109.5C1F—O1F—P1F113.77 (11)
O23B—C40B—H40B109.5C2F—O21F—C4F115.27 (15)
H40A—C40B—H40B109.5C5F—O22F—C2F116.11 (16)
O23B—C40B—H40C109.5C3F—O3F—P1F116.51 (10)
H40A—C40B—H40C109.5O1F—C1F—C2F109.97 (13)
H40B—C40B—H40C109.5O1F—C1F—H1F1109.7
O24B—C50B—H50A109.5C2F—C1F—H1F1109.7
O24B—C50B—H50B109.5O1F—C1F—H1F2109.7
H50A—C50B—H50B109.5C2F—C1F—H1F2109.7
O24B—C50B—H50C109.5H1F1—C1F—H1F2108.2
H50A—C50B—H50C109.5O21F—C2F—O22F111.86 (13)
H50B—C50B—H50C109.5O21F—C2F—C1F105.86 (14)
O4C—P1C—O5C118.60 (9)O22F—C2F—C1F112.17 (14)
O4C—P1C—O1C110.46 (11)O21F—C2F—C3F111.30 (13)
O5C—P1C—O1C107.07 (10)O22F—C2F—C3F105.82 (15)
O4C—P1C—O3C110.24 (8)C1F—C2F—C3F109.91 (13)
O5C—P1C—O3C106.95 (9)O3F—C3F—C2F110.34 (13)
O1C—P1C—O3C102.22 (7)O3F—C3F—H3F1109.6
C1C—O1C—P1C117.28 (13)C2F—C3F—H3F1109.6
C2C—O21C—C4C116.54 (16)O3F—C3F—H3F2109.6
C2C—O22C—C5C117.35 (19)C2F—C3F—H3F2109.6
C3C—O3C—P1C117.18 (11)H3F1—C3F—H3F2108.1
O1C—C1C—C2C111.84 (16)O21F—C4F—H4F1109.5
O1C—C1C—H1C1109.2O21F—C4F—H4F2109.5
C2C—C1C—H1C1109.2H4F1—C4F—H4F2109.5
O1C—C1C—H1C2109.2O21F—C4F—H4F3109.5
C2C—C1C—H1C2109.2H4F1—C4F—H4F3109.5
H1C1—C1C—H1C2107.9H4F2—C4F—H4F3109.5
O22C—C2C—O21C112.52 (14)O22F—C5F—H5F1109.5
O22C—C2C—C3C104.58 (17)O22F—C5F—H5F2109.5
O21C—C2C—C3C111.78 (14)H5F1—C5F—H5F2109.5
O22C—C2C—C1C114.61 (16)O22F—C5F—H5F3109.5
O21C—C2C—C1C103.69 (17)H5F1—C5F—H5F3109.5
C3C—C2C—C1C109.85 (14)H5F2—C5F—H5F3109.5
O3C—C3C—C2C110.73 (13)H1N—N1—H2N108.1
O3C—C3C—H3C1109.5H1N—N1—H3N106.7
C2C—C3C—H3C1109.5H2N—N1—H3N109.4
O3C—C3C—H3C2109.5H1N—N1—H4N107.9
C2C—C3C—H3C2109.5H2N—N1—H4N108.3
H3C1—C3C—H3C2108.1H3N—N1—H4N116.1
O21C—C4C—H4C1109.5H5N—N2—H6N113.8
O21C—C4C—H4C2109.5H5N—N2—H7N107.4
H4C1—C4C—H4C2109.5H6N—N2—H7N113.0
O21C—C4C—H4C3109.5H5N—N2—H8N109.9
H4C1—C4C—H4C3109.5H6N—N2—H8N105.2
H4C2—C4C—H4C3109.5H7N—N2—H8N107.3
O22C—C5C—H5C1109.5H9N—N3—H10N108.7
O22C—C5C—H5C2109.5H9N—N3—H11N111.9
H5C1—C5C—H5C2109.5H10N—N3—H11N102.0
O22C—C5C—H5C3109.5H9N—N3—H12N108.0
H5C1—C5C—H5C3109.5H10N—N3—H12N110.3
H5C2—C5C—H5C3109.5H11N—N3—H12N115.7
O40C—P10C—O50C118.8 (3)H13N—N4—H14N110.4
O40C—P10C—O10C110.4 (3)H13N—N4—H15N107.8
O50C—P10C—O10C107.4 (3)H14N—N4—H15N105.5
O40C—P10C—O30C110.2 (3)H13N—N4—H16N110.4
O50C—P10C—O30C107.0 (3)H14N—N4—H16N112.7
O10C—P10C—O30C101.5 (2)H15N—N4—H16N109.9
C10C—O10C—P10C116.6 (3)H17N—N5—H18N110.1
C20C—O23C—C40C116.8 (4)H17N—N5—H19N105.4
C20C—O24C—C50C117.3 (4)H18N—N5—H19N108.7
C30C—O30C—P10C116.5 (3)H17N—N5—H20N110.1
O10C—C10C—C20C112.5 (3)H18N—N5—H20N108.3
O10C—C10C—H10C109.1H19N—N5—H20N114.2
C20C—C10C—H10C109.1H21N—N6—H22N112.9
O10C—C10C—H10D109.1H21N—N6—H23N111.4
C20C—C10C—H10D109.1H22N—N6—H23N106.9
H10C—C10C—H10D107.8H21N—N6—H24N109.0
O24C—C20C—O23C112.4 (3)H22N—N6—H24N109.3
O24C—C20C—C30C104.5 (3)H23N—N6—H24N107.1
O5A—P1A—O1A—C1A161.43 (10)O40C—P10C—O10C—C10C148.9 (8)
O4A—P1A—O1A—C1A67.46 (11)O50C—P10C—O10C—C10C80.1 (8)
O3A—P1A—O1A—C1A49.55 (11)O30C—P10C—O10C—C10C32.0 (7)
O5A—P1A—O3A—C3A162.24 (10)O40C—P10C—O30C—C30C84.9 (8)
O4A—P1A—O3A—C3A68.23 (12)O50C—P10C—O30C—C30C144.5 (7)
O1A—P1A—O3A—C3A48.66 (11)O10C—P10C—O30C—C30C32.1 (7)
P1A—O1A—C1A—C2A58.76 (15)P10C—O10C—C10C—C20C64.4 (7)
C5A—O22A—C2A—O21A67.9 (2)C50C—O24C—C20C—O23C59.3 (13)
C5A—O22A—C2A—C3A49.76 (19)C50C—O24C—C20C—C30C179.6 (12)
C5A—O22A—C2A—C1A170.98 (15)C50C—O24C—C20C—C10C58.5 (13)
C4A—O21A—C2A—O22A44.7 (2)C40C—O23C—C20C—O24C43 (2)
C4A—O21A—C2A—C3A169.23 (16)C40C—O23C—C20C—C30C74 (2)
C4A—O21A—C2A—C1A73.4 (2)C40C—O23C—C20C—C10C167.1 (19)
O1A—C1A—C2A—O22A65.56 (16)O10C—C10C—C20C—O24C145.5 (7)
O1A—C1A—C2A—O21A172.14 (11)O10C—C10C—C20C—O23C91.9 (8)
O1A—C1A—C2A—C3A59.00 (16)O10C—C10C—C20C—C30C28.0 (7)
P1A—O3A—C3A—C2A56.28 (15)P10C—O30C—C30C—C20C67.1 (6)
O22A—C2A—C3A—O3A61.57 (16)O24C—C20C—C30C—O30C90.4 (7)
O21A—C2A—C3A—O3A175.50 (12)O23C—C20C—C30C—O30C147.9 (7)
C1A—C2A—C3A—O3A57.39 (17)C10C—C20C—C30C—O30C32.9 (7)
O4B—P1B—O1B—C1B66.2 (2)O5D—P1D—O1D—C1D163.90 (10)
O5B—P1B—O1B—C1B163.82 (18)O4D—P1D—O1D—C1D66.17 (12)
O3B—P1B—O1B—C1B51.58 (18)O3D—P1D—O1D—C1D50.63 (11)
O4B—P1B—O3B—C3B68.2 (2)O5D—P1D—O3D—C3D162.78 (10)
O5B—P1B—O3B—C3B161.17 (18)O4D—P1D—O3D—C3D65.89 (11)
O1B—P1B—O3B—C3B48.9 (2)O1D—P1D—O3D—C3D51.50 (11)
P1B—O1B—C1B—C2B60.0 (2)P1D—O1D—C1D—C2D56.93 (15)
C5B—O22B—C2B—O21B55.3 (3)C5D—O22D—C2D—O21D68.56 (19)
C5B—O22B—C2B—C1B176.8 (2)C5D—O22D—C2D—C1D49.49 (19)
C5B—O22B—C2B—C3B63.0 (3)C5D—O22D—C2D—C3D170.55 (14)
C4B—O21B—C2B—O22B66.0 (3)C4D—O21D—C2D—O22D44.0 (2)
C4B—O21B—C2B—C1B51.1 (3)C4D—O21D—C2D—C1D168.92 (17)
C4B—O21B—C2B—C3B169.1 (2)C4D—O21D—C2D—C3D73.8 (2)
O1B—C1B—C2B—O22B66.1 (2)O1D—C1D—C2D—O22D62.23 (17)
O1B—C1B—C2B—O21B172.16 (18)O1D—C1D—C2D—O21D174.56 (11)
O1B—C1B—C2B—C3B57.8 (2)O1D—C1D—C2D—C3D56.52 (16)
P1B—O3B—C3B—C2B55.2 (2)P1D—O3D—C3D—C2D59.77 (15)
O22B—C2B—C3B—O3B61.6 (2)O22D—C2D—C3D—O3D66.31 (15)
O21B—C2B—C3B—O3B175.36 (19)O21D—C2D—C3D—O3D171.59 (12)
C1B—C2B—C3B—O3B55.8 (2)C1D—C2D—C3D—O3D58.37 (16)
O40B—P10B—O10B—C10B86.0 (6)O5E—P1E—O1E—C1E74.02 (12)
O50B—P10B—O10B—C10B143.2 (5)O4E—P1E—O1E—C1E155.00 (10)
O30B—P10B—O10B—C10B31.0 (5)O3E—P1E—O1E—C1E38.60 (12)
O40B—P10B—O30B—C30B150.7 (5)O5E—P1E—O3E—C3E147.02 (11)
O50B—P10B—O30B—C30B78.0 (5)O4E—P1E—O3E—C3E83.58 (12)
O10B—P10B—O30B—C30B34.3 (5)O1E—P1E—O3E—C3E29.44 (12)
P10B—O10B—C10B—C20B68.6 (5)P1E—O1E—C1E—C2E70.83 (17)
C50B—O24B—C20B—O23B60.8 (9)C4E—O21E—C2E—O22E62.59 (19)
C50B—O24B—C20B—C10B177.7 (8)C4E—O21E—C2E—C1E175.40 (15)
C50B—O24B—C20B—C30B56.9 (8)C4E—O21E—C2E—C3E55.32 (19)
C40B—O23B—C20B—O24B61.0 (12)C5E—O22E—C2E—O21E61.47 (18)
C40B—O23B—C20B—C10B56.0 (12)C5E—O22E—C2E—C1E57.3 (2)
C40B—O23B—C20B—C30B174.9 (12)C5E—O22E—C2E—C3E177.60 (14)
O10B—C10B—C20B—O24B87.7 (5)O1E—C1E—C2E—O21E89.98 (17)
O10B—C10B—C20B—O23B150.5 (5)O1E—C1E—C2E—O22E148.21 (14)
O10B—C10B—C20B—C30B35.8 (5)O1E—C1E—C2E—C3E30.5 (2)
P10B—O30B—C30B—C20B65.6 (5)P1E—O3E—C3E—C2E67.02 (16)
O24B—C20B—C30B—O30B143.7 (5)O21E—C2E—C3E—O3E150.81 (13)
O23B—C20B—C30B—O30B93.6 (6)O22E—C2E—C3E—O3E87.99 (16)
C10B—C20B—C30B—O30B26.3 (5)C1E—C2E—C3E—O3E33.2 (2)
O4C—P1C—O1C—C1C67.70 (18)O5F—P1F—O1F—C1F72.77 (12)
O5C—P1C—O1C—C1C161.84 (16)O4F—P1F—O1F—C1F156.39 (10)
O3C—P1C—O1C—C1C49.59 (17)O3F—P1F—O1F—C1F39.82 (12)
O4C—P1C—O3C—C3C66.23 (17)O5F—P1F—O3F—C3F145.70 (11)
O5C—P1C—O3C—C3C163.55 (15)O4F—P1F—O3F—C3F84.59 (12)
O1C—P1C—O3C—C3C51.22 (15)O1F—P1F—O3F—C3F28.36 (11)
P1C—O1C—C1C—C2C56.1 (2)P1F—O1F—C1F—C2F71.86 (16)
C5C—O22C—C2C—O21C54.8 (2)C4F—O21F—C2F—O22F63.0 (2)
C5C—O22C—C2C—C3C176.31 (17)C4F—O21F—C2F—C1F174.55 (15)
C5C—O22C—C2C—C1C63.4 (2)C4F—O21F—C2F—C3F55.16 (19)
C4C—O21C—C2C—O22C66.6 (3)C5F—O22F—C2F—O21F61.9 (2)
C4C—O21C—C2C—C3C50.8 (3)C5F—O22F—C2F—C1F56.9 (2)
C4C—O21C—C2C—C1C169.0 (2)C5F—O22F—C2F—C3F176.72 (14)
O1C—C1C—C2C—O22C61.6 (2)O1F—C1F—C2F—O21F89.79 (16)
O1C—C1C—C2C—O21C175.37 (16)O1F—C1F—C2F—O22F147.94 (14)
O1C—C1C—C2C—C3C55.8 (2)O1F—C1F—C2F—C3F30.50 (19)
P1C—O3C—C3C—C2C58.87 (19)P1F—O3F—C3F—C2F67.04 (15)
O22C—C2C—C3C—O3C66.73 (18)O21F—C2F—C3F—O3F150.68 (13)
O21C—C2C—C3C—O3C171.25 (16)O22F—C2F—C3F—O3F87.59 (15)
C1C—C2C—C3C—O3C56.7 (2)C1F—C2F—C3F—O3F33.73 (19)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O5B0.901.842.728 (2)168
N1—H1N···O50B0.902.002.899 (7)173
N1—H2N···O4Fi0.901.902.804 (2)176
N1—H3N···O5Fii0.901.942.826 (2)167
N1—H4N···O4Eiii0.901.882.771 (2)173
N2—H5N···O4B0.901.942.832 (3)172
N2—H5N···O40B0.901.732.627 (8)173
N2—H6N···O3A0.902.513.123 (2)126
N2—H6N···O5A0.902.012.890 (2)164
N2—H7N···O4Eiii0.901.912.8045 (18)175
N2—H8N···O5Ciii0.901.852.740 (2)170
N2—H8N···O50Ciii0.902.012.900 (11)173
N3—H9N···O4B0.902.002.898 (3)173
N3—H9N···O40B0.901.852.740 (10)169
N3—H10N···O5D0.901.892.7747 (17)168
N3—H11N···O1Dii0.902.603.1736 (19)122
N3—H11N···O5Dii0.902.022.908 (2)171
N3—H12N···O4Ciii0.901.942.821 (3)164
N3—H12N···O40Ciii0.901.752.633 (12)166
N4—H13N···O4D0.901.922.8027 (19)167
N4—H14N···O5C0.901.912.805 (3)170
N4—H14N···O50C0.902.133.035 (18)178
N4—H15N···O5Aiii0.901.922.789 (2)162
N4—H16N···O4Ciii0.902.012.885 (3)165
N4—H16N···O40Ciii0.901.892.763 (17)163
N5—H17N···O5F0.901.902.7818 (18)166
N5—H18N···O4D0.901.932.810 (2)165
N5—H19N···O5Bii0.901.852.745 (3)170
N5—H19N···O50Bii0.902.133.029 (10)177
N5—H20N···O4Aiii0.901.952.815 (2)162
N6—H21N···O4F0.901.892.7745 (19)168
N6—H22N···O5E0.901.922.811 (2)168
N6—H23N···O4Aiii0.901.902.7972 (18)171
N6—H24N···O5Eiv0.901.892.777 (2)168
C4B—H4B3···O4Cv0.962.513.303 (5)140
Symmetry codes: (i) x, y1, z; (ii) x+2, y+1, z+1; (iii) x+1, y+1, z+1; (iv) x+1, y+2, z+1; (v) x+1, y, z.
(MTP_sl8mt) ammonium 5,5-dimethoxy-2-oxo-1,3,2-dioxaphosphorinan-2-olate top
Crystal data top
C5H10O6P·H4NDx = 1.511 Mg m3
Mr = 215.14Melting point = 444–448 K
Monoclinic, P21/aMo Kα radiation, λ = 0.71073 Å
a = 11.390 (4) ÅCell parameters from 5808 reflections
b = 6.862 (2) Åθ = 2.3–38.4°
c = 12.216 (5) ŵ = 0.29 mm1
β = 97.86 (3)°T = 205 K
V = 945.8 (6) Å3Plate, colourless
Z = 40.45 × 0.16 × 0.06 mm
F(000) = 456
Data collection top
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
3051 reflections with I > 2σ(I)
Radiation source: Enhance (Mo) X-ray SourceRint = 0.026
ω and phi scansθmax = 38.5°, θmin = 3.4°
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
h = 1918
Tmin = 0.851, Tmax = 1.000k = 811
14164 measured reflectionsl = 2017
4906 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: mixed
wR(F2) = 0.114H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.0583P)2 + 0.0177P]
where P = (Fo2 + 2Fc2)/3
4906 reflections(Δ/σ)max < 0.001
192 parametersΔρmax = 0.40 e Å3
30 restraintsΔρmin = 0.26 e Å3
Crystal data top
C5H10O6P·H4NV = 945.8 (6) Å3
Mr = 215.14Z = 4
Monoclinic, P21/aMo Kα radiation
a = 11.390 (4) ŵ = 0.29 mm1
b = 6.862 (2) ÅT = 205 K
c = 12.216 (5) Å0.45 × 0.16 × 0.06 mm
β = 97.86 (3)°
Data collection top
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
4906 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
3051 reflections with I > 2σ(I)
Tmin = 0.851, Tmax = 1.000Rint = 0.026
14164 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04030 restraints
wR(F2) = 0.114H atoms treated by a mixture of independent and constrained refinement
S = 1.01Δρmax = 0.40 e Å3
4906 reflectionsΔρmin = 0.26 e Å3
192 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
P10.40746 (10)0.59840 (17)0.34360 (7)0.0237 (2)0.7821 (19)
O10.40067 (8)0.58475 (17)0.21205 (8)0.0301 (2)0.7821 (19)
O210.54607 (12)0.2655 (2)0.11137 (12)0.0317 (4)0.7821 (19)
O220.70227 (10)0.42140 (17)0.22038 (10)0.0371 (3)0.782 (2)
O30.52398 (16)0.4703 (3)0.38127 (10)0.0257 (4)0.7821 (19)
O40.30034 (14)0.5007 (2)0.37393 (15)0.0291 (4)0.7821 (19)
O50.43473 (13)0.80081 (18)0.38344 (14)0.0317 (3)0.7821 (19)
C10.51319 (13)0.58478 (19)0.17144 (12)0.0325 (3)0.7821 (19)
H1A0.56140.69370.20420.039*0.7821 (19)
H1B0.50100.60220.09110.039*0.7821 (19)
C20.57821 (17)0.39317 (17)0.20047 (12)0.0250 (3)0.7821 (19)
C30.54384 (14)0.3126 (2)0.30852 (12)0.0236 (13)0.7821 (19)
H3A0.47170.23400.29280.028*0.7821 (19)
H3B0.60740.22850.34430.028*0.7821 (19)
C40.5967 (2)0.0728 (2)0.12769 (17)0.0478 (5)0.7821 (19)
H4A0.67960.08350.15840.072*0.7821 (19)
H4B0.59010.00530.05740.072*0.7821 (19)
H4C0.55450.00040.17820.072*0.7821 (19)
C50.75371 (17)0.4952 (3)0.12792 (16)0.0514 (5)0.7821 (19)
H5A0.73780.40540.06640.077*0.7821 (19)
H5B0.83870.50880.14820.077*0.7821 (19)
H5C0.71940.62130.10660.077*0.7821 (19)
P100.4188 (3)0.6175 (6)0.3469 (2)0.0216 (7)0.2179 (19)
O100.4242 (3)0.6655 (4)0.2198 (2)0.0267 (8)*0.2179 (19)
O2100.5465 (4)0.2287 (6)0.1141 (4)0.0229 (13)*0.2179 (19)
O2200.6542 (3)0.4969 (5)0.1927 (2)0.0250 (7)*0.2179 (19)
O300.5352 (5)0.4859 (8)0.3761 (3)0.0242 (18)*0.2179 (19)
O400.3097 (5)0.5040 (9)0.3552 (5)0.0258 (15)*0.2179 (19)
O500.4392 (5)0.7996 (7)0.4136 (3)0.0257 (12)*0.2179 (19)
C100.4383 (3)0.5058 (5)0.1477 (3)0.0234 (9)*0.2179 (19)
H10A0.44360.55570.07340.028*0.2179 (19)
H10B0.36850.42130.14330.028*0.2179 (19)
C200.5491 (3)0.3867 (4)0.1875 (3)0.0238 (15)*0.2179 (19)
C300.5437 (5)0.3190 (6)0.3064 (3)0.035 (6)*0.2179 (19)
H30A0.47470.23440.30830.042*0.2179 (19)
H30B0.61510.24420.33340.042*0.2179 (19)
C400.6453 (5)0.0963 (8)0.1341 (6)0.0372 (16)*0.2179 (19)
H40A0.71880.16860.13650.056*0.2179 (19)
H40B0.64000.00080.07510.056*0.2179 (19)
H40C0.64350.03050.20410.056*0.2179 (19)
C500.6837 (5)0.5662 (8)0.0892 (3)0.0368 (12)*0.2179 (19)
H50A0.68660.45720.03910.055*0.2179 (19)
H50B0.76050.62970.10110.055*0.2179 (19)
H50C0.62420.65860.05750.055*0.2179 (19)
N10.15523 (9)0.63512 (14)0.51855 (9)0.0315 (2)
H1N0.2156 (14)0.608 (2)0.4751 (13)0.045 (4)*
H2N0.0866 (13)0.6616 (19)0.4760 (12)0.037 (4)*
H3N0.1446 (13)0.530 (2)0.5643 (12)0.044 (4)*
H4N0.1787 (14)0.740 (2)0.5589 (13)0.051 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P10.0264 (3)0.0201 (3)0.0259 (4)0.0021 (2)0.0082 (2)0.0022 (2)
O10.0327 (5)0.0339 (6)0.0247 (5)0.0080 (4)0.0068 (4)0.0020 (4)
O210.0414 (7)0.0270 (6)0.0284 (6)0.0018 (5)0.0109 (4)0.0056 (5)
O220.0314 (5)0.0420 (6)0.0403 (6)0.0074 (5)0.0140 (4)0.0010 (5)
O30.0284 (6)0.0287 (7)0.0213 (6)0.0054 (5)0.0076 (4)0.0024 (4)
O40.0288 (6)0.0291 (6)0.0320 (7)0.0018 (4)0.0132 (5)0.0020 (5)
O50.0384 (6)0.0223 (6)0.0355 (8)0.0006 (4)0.0092 (6)0.0056 (5)
C10.0455 (8)0.0264 (7)0.0288 (7)0.0046 (5)0.0163 (6)0.0059 (5)
C20.0290 (7)0.0239 (7)0.0242 (6)0.0005 (5)0.0109 (5)0.0024 (5)
C30.0294 (16)0.0210 (13)0.0224 (13)0.0067 (5)0.0106 (6)0.0020 (4)
C40.0694 (15)0.0289 (8)0.0460 (10)0.0114 (8)0.0109 (10)0.0094 (7)
C50.0484 (9)0.0559 (11)0.0560 (11)0.0163 (8)0.0289 (8)0.0017 (9)
P100.0188 (8)0.0258 (13)0.0214 (11)0.0016 (7)0.0069 (7)0.0001 (8)
N10.0308 (4)0.0244 (5)0.0419 (5)0.0010 (3)0.0142 (4)0.0012 (4)
Geometric parameters (Å, º) top
P1—O41.4828 (13)P10—O101.5962 (19)
P1—O51.4904 (12)P10—O301.6033 (17)
P1—O11.6011 (12)O10—C101.429 (2)
P1—O31.6058 (10)O210—C201.405 (2)
O1—C11.4362 (16)O210—C401.440 (3)
O21—C21.4062 (17)O220—C201.410 (3)
O21—C41.4454 (19)O220—C501.433 (3)
O22—C21.414 (2)O30—C301.438 (2)
O22—C51.4340 (19)C10—C201.526 (3)
O3—C31.4381 (13)C10—H10A0.9800
C1—C21.5268 (19)C10—H10B0.9800
C1—H1A0.9800C20—C301.534 (2)
C1—H1B0.9800C30—H30A0.9800
C2—C31.5307 (17)C30—H30B0.9800
C3—H3A0.9800C40—H40A0.9700
C3—H3B0.9800C40—H40B0.9700
C4—H4A0.9700C40—H40C0.9700
C4—H4B0.9700C50—H50A0.9700
C4—H4C0.9700C50—H50B0.9700
C5—H5A0.9700C50—H50C0.9700
C5—H5B0.9700N1—H1N0.943 (16)
C5—H5C0.9700N1—H2N0.897 (14)
P10—O401.4818 (19)N1—H3N0.929 (15)
P10—O501.4931 (18)N1—H4N0.895 (16)
O4—P1—O5118.79 (8)O40—P10—O30111.4 (2)
O4—P1—O1107.21 (9)O50—P10—O30106.7 (2)
O5—P1—O1111.20 (9)O10—P10—O30101.09 (17)
O4—P1—O3110.91 (9)C10—O10—P10117.6 (2)
O5—P1—O3106.82 (8)C20—O210—C40115.5 (3)
O1—P1—O3100.38 (6)C20—O220—C50116.0 (3)
C1—O1—P1115.07 (10)C30—O30—P10115.9 (2)
C2—O21—C4113.97 (13)O10—C10—C20111.9 (2)
C2—O22—C5114.78 (13)O10—C10—H10A109.2
C3—O3—P1115.38 (9)C20—C10—H10A109.2
O1—C1—C2110.31 (10)O10—C10—H10B109.2
O1—C1—H1A109.6C20—C10—H10B109.2
C2—C1—H1A109.6H10A—C10—H10B107.9
O1—C1—H1B109.6O210—C20—O220112.7 (2)
C2—C1—H1B109.6O210—C20—C10105.4 (2)
H1A—C1—H1B108.1O220—C20—C10112.8 (2)
O21—C2—O22111.52 (11)O210—C20—C30111.8 (2)
O21—C2—C1106.86 (15)O220—C20—C30105.3 (2)
O22—C2—C1111.32 (12)C10—C20—C30109.0 (2)
O21—C2—C3111.85 (12)O30—C30—C20109.5 (2)
O22—C2—C3105.58 (14)O30—C30—H30A109.8
C1—C2—C3109.78 (10)C20—C30—H30A109.8
O3—C3—C2109.95 (13)O30—C30—H30B109.8
O3—C3—H3A109.7C20—C30—H30B109.8
C2—C3—H3A109.7H30A—C30—H30B108.2
O3—C3—H3B109.7O210—C40—H40A109.5
C2—C3—H3B109.7O210—C40—H40B109.5
H3A—C3—H3B108.2H40A—C40—H40B109.5
O21—C4—H4A109.5O210—C40—H40C109.5
O21—C4—H4B109.5H40A—C40—H40C109.5
H4A—C4—H4B109.5H40B—C40—H40C109.5
O21—C4—H4C109.5O220—C50—H50A109.5
H4A—C4—H4C109.5O220—C50—H50B109.5
H4B—C4—H4C109.5H50A—C50—H50B109.5
O22—C5—H5A109.5O220—C50—H50C109.5
O22—C5—H5B109.5H50A—C50—H50C109.5
H5A—C5—H5B109.5H50B—C50—H50C109.5
O22—C5—H5C109.5H1N—N1—H2N111.0 (13)
H5A—C5—H5C109.5H1N—N1—H3N110.5 (12)
H5B—C5—H5C109.5H2N—N1—H3N109.3 (13)
O40—P10—O50118.1 (2)H1N—N1—H4N106.5 (13)
O40—P10—O10108.6 (2)H2N—N1—H4N109.1 (13)
O50—P10—O10109.5 (2)H3N—N1—H4N110.3 (14)
O4—P1—O1—C1152.09 (11)O40—P10—O10—C1065.9 (3)
O5—P1—O1—C176.54 (12)O50—P10—O10—C10163.7 (3)
O3—P1—O1—C136.20 (13)O30—P10—O10—C1051.3 (3)
O4—P1—O3—C380.82 (16)O40—P10—O30—C3060.5 (4)
O5—P1—O3—C3148.32 (15)O50—P10—O30—C30169.2 (4)
O1—P1—O3—C332.26 (16)O10—P10—O30—C3054.7 (4)
P1—O1—C1—C270.39 (14)P10—O10—C10—C2056.6 (4)
C4—O21—C2—O2260.53 (19)C40—O210—C20—O22055.3 (5)
C4—O21—C2—C1177.61 (17)C40—O210—C20—C10178.7 (5)
C4—O21—C2—C357.4 (2)C40—O210—C20—C3063.0 (5)
C5—O22—C2—O2157.62 (17)C50—O220—C20—O21053.8 (4)
C5—O22—C2—C161.63 (15)C50—O220—C20—C1065.4 (4)
C5—O22—C2—C3179.30 (12)C50—O220—C20—C30175.9 (4)
O1—C1—C2—O2191.05 (14)O10—C10—C20—O210175.8 (3)
O1—C1—C2—O22146.96 (11)O10—C10—C20—O22060.9 (3)
O1—C1—C2—C330.43 (18)O10—C10—C20—C3055.7 (3)
P1—O3—C3—C269.87 (17)P10—O30—C30—C2062.7 (4)
O21—C2—C3—O3152.53 (13)O210—C20—C30—O30174.6 (3)
O22—C2—C3—O386.00 (13)O220—C20—C30—O3062.8 (4)
C1—C2—C3—O334.09 (18)C10—C20—C30—O3058.4 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O40.94 (2)1.82 (2)2.739 (2)163 (2)
N1—H1N···O400.94 (2)2.06 (2)2.974 (5)164 (2)
N1—H2N···O5i0.90 (2)1.95 (2)2.845 (2)176 (2)
N1—H2N···O50i0.90 (2)1.77 (2)2.652 (5)169 (2)
N1—H3N···O5ii0.93 (2)1.96 (2)2.8428 (17)157 (2)
N1—H3N···O50ii0.93 (2)1.89 (2)2.718 (4)148 (2)
N1—H4N···O4iii0.90 (2)1.97 (2)2.845 (2)167 (2)
N1—H4N···O40iii0.90 (2)2.09 (2)2.963 (6)166 (2)
C40—H40C···O40iv0.972.473.146 (9)127
Symmetry codes: (i) x1/2, y+3/2, z; (ii) x+1/2, y1/2, z+1; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y+1/2, z.
(LTP_sl8lt) ammonium 5,5-dimethoxy-2-oxo-1,3,2-dioxaphosphorinan-2-olate top
Crystal data top
C5H10O6P·H4NF(000) = 2736
Mr = 215.14Dx = 1.525 Mg m3
Triclinic, P1Melting point = 444–448 K
a = 11.336 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 20.486 (5) ÅCell parameters from 15395 reflections
c = 25.369 (6) Åθ = 2.2–38.5°
α = 105.60 (3)°µ = 0.30 mm1
β = 97.50 (3)°T = 100 K
γ = 90.17 (3)°Plate, colourless
V = 5621 (3) Å30.45 × 0.16 × 0.06 mm
Z = 24
Data collection top
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
14062 reflections with I > 2σ(I)
Radiation source: Enhance (Mo) X-ray SourceRint = 0.038
ω and phi scansθmax = 30.0°, θmin = 2.2°
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
h = 1515
Tmin = 0.827, Tmax = 1.000k = 2028
77940 measured reflectionsl = 3534
32235 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: mixed
wR(F2) = 0.079H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.016P)2]
where P = (Fo2 + 2Fc2)/3
32235 reflections(Δ/σ)max = 0.001
1568 parametersΔρmax = 0.53 e Å3
438 restraintsΔρmin = 0.37 e Å3
Crystal data top
C5H10O6P·H4Nγ = 90.17 (3)°
Mr = 215.14V = 5621 (3) Å3
Triclinic, P1Z = 24
a = 11.336 (3) ÅMo Kα radiation
b = 20.486 (5) ŵ = 0.30 mm1
c = 25.369 (6) ÅT = 100 K
α = 105.60 (3)°0.45 × 0.16 × 0.06 mm
β = 97.50 (3)°
Data collection top
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
32235 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
14062 reflections with I > 2σ(I)
Tmin = 0.827, Tmax = 1.000Rint = 0.038
77940 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.041438 restraints
wR(F2) = 0.079H-atom parameters constrained
S = 1.00Δρmax = 0.53 e Å3
32235 reflectionsΔρmin = 0.37 e Å3
1568 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
P1A0.41187 (6)0.17288 (3)0.42291 (3)0.01328 (15)
O1A0.40727 (13)0.14763 (7)0.35699 (7)0.0162 (4)
O21A0.54824 (14)0.02242 (8)0.30665 (7)0.0155 (4)
O22A0.70853 (12)0.08967 (7)0.36314 (7)0.0166 (4)
O3A0.52775 (14)0.13546 (8)0.44193 (7)0.0138 (4)
O4A0.30152 (14)0.14445 (8)0.43576 (8)0.0161 (4)
O5A0.43945 (14)0.24697 (8)0.44515 (8)0.0181 (4)
C1A0.52282 (18)0.14089 (10)0.33860 (9)0.0137 (5)
H1A10.57300.18230.35730.016*
H1A20.51420.13540.29830.016*
C2A0.5823 (2)0.07921 (11)0.35187 (10)0.0133 (5)
C3A0.5436 (2)0.06969 (12)0.40528 (11)0.0134 (6)
H3A10.46800.04230.39660.016*
H3A20.60500.04550.42330.016*
C4A0.5865 (2)0.04159 (10)0.31498 (11)0.0217 (6)
H4A10.66450.03490.33790.033*
H4A20.59260.07380.27920.033*
H4A30.52850.05950.33350.033*
C5A0.76254 (19)0.10034 (12)0.31801 (10)0.0215 (5)
H5A10.74380.06110.28570.032*
H5A20.84910.10600.32840.032*
H5A30.73170.14120.30900.032*
P1B0.89576 (6)0.27297 (3)0.41852 (3)0.01343 (15)
O1B0.88874 (13)0.25723 (7)0.35264 (7)0.0169 (4)
O21B1.04361 (14)0.34572 (8)0.30417 (7)0.0157 (4)
O22B1.19570 (13)0.30791 (8)0.35909 (7)0.0213 (4)
O3B1.01447 (14)0.32099 (8)0.43837 (7)0.0137 (4)
O4B0.78780 (14)0.31097 (8)0.43382 (8)0.0161 (4)
O5B0.92088 (14)0.21161 (8)0.43813 (7)0.0183 (4)
C1B1.00174 (19)0.24859 (11)0.33308 (10)0.0194 (5)
H1B10.99000.22960.29240.023*
H1B21.04750.21610.34950.023*
C2B1.0719 (2)0.31669 (12)0.34853 (11)0.0146 (6)
C3B1.0374 (2)0.36194 (12)0.40208 (11)0.0138 (6)
H3B11.10270.39580.42050.017*
H3B20.96530.38650.39390.017*
C4B1.1005 (2)0.41123 (11)0.31256 (11)0.0262 (6)
H4B11.07040.44390.34330.039*
H4B21.08300.42620.27890.039*
H4B31.18670.40830.32130.039*
C5B1.2455 (2)0.26763 (12)0.31210 (11)0.0304 (7)
H5B11.20780.22200.30060.046*
H5B21.33140.26470.32210.046*
H5B31.23120.28880.28160.046*
P1C0.40500 (6)0.50647 (3)0.42136 (3)0.01307 (15)
O1C0.39563 (13)0.48027 (7)0.35531 (7)0.0169 (4)
O21C0.54245 (14)0.35805 (8)0.30353 (7)0.0166 (4)
O22C0.70043 (13)0.42870 (8)0.35901 (7)0.0197 (4)
O3C0.52246 (14)0.46931 (8)0.43952 (7)0.0137 (4)
O4C0.29640 (14)0.47876 (8)0.43625 (8)0.0168 (4)
O5C0.43369 (14)0.58066 (8)0.44253 (8)0.0191 (4)
C1C0.50971 (17)0.47565 (10)0.33524 (9)0.0149 (5)
H1C10.55790.51810.35290.018*
H1C20.49800.46940.29480.018*
C2C0.5753 (2)0.41539 (11)0.34865 (10)0.0123 (5)
C3C0.5401 (2)0.40456 (12)0.40214 (11)0.0139 (6)
H3C10.46580.37600.39370.017*
H3C20.60370.38090.41950.017*
C4C0.5941 (2)0.29633 (11)0.31033 (11)0.0235 (6)
H4C10.68070.30320.31920.035*
H4C20.57460.26010.27600.035*
H4C30.56210.28360.34040.035*
C5C0.7508 (2)0.43851 (13)0.31286 (11)0.0273 (6)
H5C10.72860.39950.28070.041*
H5C20.83780.44280.32170.041*
H5C30.72070.47990.30440.041*
P1D0.91489 (6)0.61022 (3)0.42410 (3)0.01335 (15)
O1D0.90780 (13)0.59197 (7)0.35802 (7)0.0152 (4)
O21D1.05085 (14)0.68126 (8)0.30621 (7)0.0155 (4)
O22D1.20960 (13)0.65087 (7)0.36214 (7)0.0189 (4)
O3D1.03093 (14)0.66081 (8)0.44251 (7)0.0148 (4)
O4D0.80551 (14)0.64708 (8)0.43870 (7)0.0157 (4)
O5D0.94358 (14)0.55030 (8)0.44527 (8)0.0180 (4)
C1D1.02247 (19)0.58522 (10)0.33869 (10)0.0184 (5)
H1D11.01220.56390.29830.022*
H1D21.07200.55570.35700.022*
C2D1.0845 (2)0.65517 (11)0.35167 (11)0.0134 (5)
C3D1.0471 (2)0.70091 (12)0.40467 (11)0.0134 (6)
H3D11.10900.73720.42210.016*
H3D20.97180.72250.39580.016*
C4D1.0907 (2)0.75091 (11)0.31389 (11)0.0207 (6)
H4D11.03130.78160.33050.031*
H4D21.10090.75800.27800.031*
H4D31.16680.76020.33830.031*
C5D1.2614 (2)0.60862 (12)0.31709 (11)0.0252 (6)
H5D11.22800.56220.30850.038*
H5D21.34790.60870.32730.038*
H5D31.24390.62600.28460.038*
P1E0.41359 (8)0.84738 (5)0.42118 (4)0.0112 (2)0.9185 (18)
O1E0.41666 (14)0.83990 (8)0.35675 (7)0.0143 (4)0.9185 (18)
O21E0.54737 (17)0.67780 (8)0.30740 (8)0.0133 (4)0.9185 (18)
O22E0.65339 (12)0.78290 (7)0.34396 (6)0.0134 (4)0.9185 (18)
O3E0.53232 (16)0.81040 (10)0.43739 (8)0.0130 (4)0.9185 (18)
O4E0.30701 (16)0.81119 (12)0.42990 (10)0.0142 (4)0.918 (2)
O5E0.43330 (19)0.92098 (9)0.45016 (9)0.0160 (5)0.9185 (18)
C1E0.43460 (17)0.77329 (10)0.32227 (9)0.0112 (5)0.9185 (18)
H1E10.43760.77580.28400.013*0.9185 (18)
H1E20.36640.74260.32160.013*0.9185 (18)
C2E0.5494 (2)0.74433 (11)0.34314 (10)0.0108 (5)0.9185 (18)
C3E0.5489 (2)0.74351 (13)0.40328 (12)0.0152 (6)0.9185 (18)
H3E10.48390.71230.40540.018*0.9185 (18)
H3E20.62520.72660.41710.018*0.9185 (18)
C4E0.6480 (2)0.63868 (11)0.31814 (11)0.0180 (6)0.9185 (18)
H4E10.63900.59360.29170.027*0.9185 (18)
H4E20.65280.63400.35580.027*0.9185 (18)
H4E30.72100.66170.31430.027*0.9185 (18)
C5E0.67930 (19)0.78779 (11)0.29168 (9)0.0198 (5)0.9185 (18)
H5E10.75280.81540.29680.030*0.9185 (18)
H5E20.61350.80900.27430.030*0.9185 (18)
H5E30.68940.74230.26800.030*0.9185 (18)
P10E0.3946 (9)0.8369 (6)0.4193 (5)0.0189 (18)*0.0815 (18)
O10E0.3984 (8)0.8145 (6)0.3538 (4)0.0107 (16)*0.0815 (18)
O23E0.5454 (14)0.6941 (6)0.3070 (6)0.0109 (16)*0.0815 (18)
O24E0.7072 (9)0.7622 (7)0.3626 (6)0.012 (2)*0.0815 (18)
O30E0.5139 (12)0.8044 (9)0.4413 (4)0.012 (2)*0.0815 (18)
O40E0.2884 (12)0.8065 (12)0.4337 (7)0.0142 (4)0.0815 (18)
O50E0.4149 (19)0.9120 (6)0.4380 (7)0.012 (3)*0.0815 (18)
C10E0.5151 (10)0.8090 (6)0.3365 (5)0.008 (2)*0.0815 (18)
H10A0.56140.85220.35390.010*0.0815 (18)
H10B0.50700.80120.29600.010*0.0815 (18)
C20E0.5822 (9)0.7513 (5)0.3523 (5)0.0110 (17)*0.0815 (18)
C30E0.5477 (13)0.7417 (7)0.4062 (6)0.015 (2)*0.0815 (18)
H30A0.48050.70790.39760.018*0.0815 (18)
H30B0.61600.72400.42600.018*0.0815 (18)
C40E0.589 (3)0.6306 (5)0.3134 (10)0.020 (3)*0.0815 (18)
H40A0.55830.59410.28070.030*0.0815 (18)
H40B0.56260.62190.34620.030*0.0815 (18)
H40C0.67640.63250.31770.030*0.0815 (18)
C50E0.7636 (13)0.7684 (15)0.3172 (8)0.026 (4)*0.0815 (18)
H50A0.84950.77660.32890.039*0.0815 (18)
H50B0.73090.80640.30420.039*0.0815 (18)
H50C0.74940.72640.28720.039*0.0815 (18)
P1F0.92001 (6)0.93428 (3)0.42269 (3)0.01302 (15)
O1F0.92396 (13)0.89729 (7)0.35873 (7)0.0180 (4)
O21F1.04389 (13)1.02554 (8)0.30623 (7)0.0152 (4)
O22F1.15772 (13)0.95027 (7)0.34444 (7)0.0201 (4)
O3F1.03665 (14)0.98353 (8)0.43826 (7)0.0149 (4)
O4F0.81192 (14)0.97512 (8)0.42986 (8)0.0158 (4)
O5F0.94141 (14)0.88165 (8)0.45287 (7)0.0178 (4)
C1F0.93900 (18)0.93875 (10)0.32329 (9)0.0175 (5)
H1F10.86860.96690.32120.021*
H1F20.94410.90960.28570.021*
C2F1.0517 (2)0.98524 (12)0.34350 (11)0.0149 (5)
C3F1.0484 (2)1.02706 (12)0.40253 (11)0.0154 (6)
H3F11.12241.05570.41600.019*
H3F20.98031.05740.40370.019*
C4F1.14120 (19)1.07457 (11)0.31582 (10)0.0215 (6)
H4F11.13791.10910.35080.032*
H4F21.13501.09620.28550.032*
H4F31.21691.05170.31770.032*
C5F1.1837 (2)0.90911 (11)0.29250 (10)0.0250 (6)
H5F11.12050.87390.27690.038*
H5F21.26000.88780.29780.038*
H5F31.18830.93740.26720.038*
P1G1.08682 (6)0.89424 (3)0.07751 (3)0.01157 (14)
O1G1.09082 (13)0.91017 (7)0.14324 (7)0.0158 (4)
O21G0.94505 (14)0.81528 (8)0.19025 (7)0.0145 (4)
O22G0.78705 (12)0.84927 (7)0.13521 (7)0.0164 (4)
O3G0.96991 (14)0.84459 (8)0.05714 (7)0.0133 (4)
O4G1.19631 (14)0.85787 (8)0.06351 (8)0.0158 (4)
O5G1.05976 (14)0.95531 (8)0.05757 (8)0.0174 (4)
C1G0.97510 (17)0.91478 (10)0.16153 (10)0.0146 (5)
H1G10.92600.94530.14420.018*
H1G20.98390.93410.20210.018*
C2G0.91312 (19)0.84439 (11)0.14585 (10)0.0136 (5)
C3G0.9508 (2)0.80138 (11)0.09202 (11)0.0123 (5)
H3G11.02510.77840.10000.015*
H3G20.88810.76620.07290.015*
C4G0.8942 (2)0.74811 (11)0.18128 (11)0.0220 (6)
H4G10.80870.74750.16840.033*
H4G20.90610.73500.21600.033*
H4G30.93300.71600.15340.033*
C5G0.73438 (19)0.88577 (11)0.18232 (10)0.0205 (5)
H5G10.75160.86360.21210.031*
H5G20.64800.88620.17220.031*
H5G30.76750.93250.19490.031*
P1H0.58681 (6)0.65715 (3)0.07741 (3)0.01183 (15)
O1H0.58986 (13)0.68490 (7)0.14322 (7)0.0164 (4)
O21H0.44492 (13)0.81131 (8)0.18948 (7)0.0147 (4)
O22H0.28725 (12)0.74048 (7)0.13455 (7)0.0196 (4)
O3H0.47039 (14)0.69297 (8)0.05688 (7)0.0136 (4)
O4H0.69640 (14)0.68432 (8)0.06349 (8)0.0158 (4)
O5H0.55963 (14)0.58269 (8)0.05756 (8)0.0174 (4)
C1H0.47376 (18)0.69327 (11)0.16101 (10)0.0203 (5)
H1H10.48190.70090.20160.024*
H1H20.42390.65130.14360.024*
C2H0.41320 (19)0.75278 (11)0.14557 (10)0.0150 (5)
C3H0.4512 (2)0.75970 (12)0.09169 (11)0.0133 (5)
H3H10.38850.78190.07240.016*
H3H20.52540.78820.09970.016*
C4H0.3943 (2)0.87243 (11)0.18055 (11)0.0234 (6)
H4H10.43430.88660.15320.035*
H4H20.40480.90840.21540.035*
H4H30.30910.86400.16690.035*
C5H0.23441 (19)0.73606 (13)0.18189 (10)0.0256 (6)
H5H10.27220.70060.19680.038*
H5H20.14900.72480.17110.038*
H5H30.24590.77970.21020.038*
P1I1.08358 (10)0.56380 (6)0.07785 (4)0.0106 (2)0.888 (2)
O1I1.07650 (14)0.60146 (8)0.14127 (7)0.0135 (4)0.888 (2)
O21I0.95898 (17)0.47216 (9)0.19513 (9)0.0139 (5)0.888 (2)
O22I0.84625 (14)0.54622 (8)0.15360 (7)0.0140 (4)0.888 (2)
O3I0.97037 (18)0.51202 (11)0.06240 (8)0.0132 (5)0.888 (2)
O4I1.19527 (18)0.52563 (12)0.07277 (11)0.0150 (5)0.888 (2)
O5I1.06004 (19)0.61526 (10)0.04660 (10)0.0153 (5)0.888 (2)
C1I1.06438 (18)0.55931 (10)0.17784 (9)0.0125 (5)0.888 (2)
H1I11.05850.58840.21540.015*0.888 (2)
H1I21.13580.53190.17990.015*0.888 (2)
C2I0.9535 (2)0.51230 (12)0.15716 (11)0.0112 (6)0.888 (2)
C3I0.9594 (2)0.46892 (12)0.09817 (12)0.0135 (6)0.888 (2)
H3I11.02860.43950.09790.016*0.888 (2)
H3I20.88640.43940.08460.016*0.888 (2)
C4I0.8608 (2)0.42438 (12)0.18611 (12)0.0176 (6)0.888 (2)
H4I10.87180.39900.21400.026*0.888 (2)
H4I20.85710.39280.14920.026*0.888 (2)
H4I30.78650.44860.18900.026*0.888 (2)
C5I0.8168 (2)0.58860 (11)0.20411 (11)0.0202 (6)0.888 (2)
H5I10.74080.60950.19710.030*0.888 (2)
H5I20.87940.62410.22000.030*0.888 (2)
H5I30.80980.56140.23000.030*0.888 (2)
P10I1.1019 (7)0.5571 (5)0.0792 (3)0.0163 (17)*0.112 (2)
O10I1.1043 (6)0.5776 (5)0.1448 (3)0.0108 (15)*0.112 (2)
O23I0.9580 (10)0.4889 (6)0.1948 (5)0.0115 (16)*0.112 (2)
O24I0.7971 (7)0.5207 (5)0.1397 (4)0.0091 (18)*0.112 (2)
O30I0.9834 (10)0.5092 (7)0.0592 (3)0.014 (2)*0.112 (2)
O40I1.2080 (10)0.5175 (8)0.0635 (6)0.010 (4)*0.112 (2)
O50I1.0791 (14)0.6198 (6)0.0613 (5)0.014 (4)*0.112 (2)
C10I0.9903 (8)0.5840 (4)0.1651 (4)0.013 (2)*0.112 (2)
H10C0.94290.61660.14950.016*0.112 (2)
H10D1.00290.60220.20580.016*0.112 (2)
C20I0.9216 (7)0.5160 (4)0.1493 (4)0.0112 (16)*0.112 (2)
C30I0.9543 (11)0.4699 (4)0.0954 (5)0.014 (2)*0.112 (2)
H30C1.02330.44310.10370.017*0.112 (2)
H30D0.88640.43790.07670.017*0.112 (2)
C40I0.9102 (18)0.4220 (7)0.1887 (8)0.022 (3)*0.112 (2)
H40D0.94110.40680.22110.033*0.112 (2)
H40E0.93380.39080.15540.033*0.112 (2)
H40F0.82310.42270.18540.033*0.112 (2)
C50I0.7445 (10)0.5626 (8)0.1842 (6)0.017 (3)*0.112 (2)
H50D0.65840.56320.17330.025*0.112 (2)
H50E0.77910.60890.19340.025*0.112 (2)
H50F0.75990.54470.21640.025*0.112 (2)
P1J0.59548 (6)0.32763 (3)0.07858 (3)0.01184 (15)
O1J0.60550 (13)0.35196 (7)0.14475 (7)0.0152 (4)
O21J0.46972 (14)0.47653 (8)0.19891 (7)0.0169 (4)
O22J0.30557 (13)0.41092 (7)0.14589 (7)0.0200 (4)
O3J0.47751 (14)0.36477 (8)0.06188 (7)0.0138 (4)
O4J0.70313 (14)0.35672 (8)0.06387 (8)0.0155 (4)
O5J0.56863 (14)0.25340 (8)0.05661 (8)0.0170 (4)
C1J0.49316 (19)0.35883 (11)0.16553 (10)0.0185 (5)
H1J10.50590.36430.20590.022*
H1J20.44220.31740.14780.022*
C2J0.4311 (2)0.42045 (12)0.15362 (11)0.0141 (5)
C3J0.4626 (2)0.43004 (12)0.09917 (11)0.0132 (6)
H3J10.39820.45370.08240.016*
H3J20.53710.45820.10630.016*
C4J0.4350 (2)0.54126 (11)0.19126 (11)0.0272 (6)
H4J10.48760.55550.16830.041*
H4J20.44110.57500.22730.041*
H4J30.35260.53740.17300.041*
C5J0.2574 (2)0.39915 (12)0.19235 (11)0.0261 (6)
H5J10.28830.35730.19950.039*
H5J20.17030.39490.18430.039*
H5J30.28070.43730.22500.039*
P1K1.09563 (6)0.22460 (3)0.07833 (3)0.01168 (14)
O1K1.10564 (13)0.24400 (7)0.14438 (7)0.0146 (4)
O21K0.96710 (14)0.15614 (8)0.19845 (7)0.0165 (4)
O22K0.80326 (13)0.18636 (7)0.14469 (7)0.0179 (4)
O3K0.97696 (14)0.17640 (8)0.06150 (7)0.0136 (4)
O4K1.20311 (14)0.18559 (8)0.06370 (8)0.0157 (4)
O5K1.06990 (14)0.28438 (8)0.05653 (8)0.0171 (4)
C1K0.99187 (18)0.25194 (10)0.16500 (9)0.0145 (5)
H1K10.94200.28150.14690.017*
H1K21.00400.27360.20530.017*
C2K0.9294 (2)0.18233 (12)0.15290 (11)0.0122 (5)
C3K0.9612 (2)0.13605 (12)0.09863 (11)0.0139 (6)
H3K11.03540.11280.10590.017*
H3K20.89660.10110.08180.017*
C4K0.9310 (2)0.08620 (11)0.19024 (11)0.0242 (6)
H4K10.84940.07790.17090.036*
H4K20.93430.07640.22620.036*
H4K30.98470.05670.16810.036*
C5K0.75462 (19)0.22857 (11)0.19065 (11)0.0233 (6)
H5K10.78160.21400.22390.035*
H5K20.66750.22480.18320.035*
H5K30.78140.27580.19640.035*
P1L0.58642 (9)0.01150 (6)0.07799 (5)0.01129 (18)0.940 (3)
O1L0.58017 (16)0.00526 (8)0.14180 (7)0.0173 (4)0.940 (3)
O21L0.45871 (15)0.15626 (9)0.19483 (8)0.0147 (4)0.940 (3)
O22L0.34534 (15)0.05561 (8)0.15312 (7)0.0181 (4)0.940 (3)
O3L0.47218 (17)0.02858 (9)0.06216 (8)0.0132 (4)0.940 (3)
O4L0.69663 (16)0.02322 (11)0.07105 (9)0.0146 (5)0.940 (3)
O5L0.56328 (19)0.08437 (9)0.04839 (9)0.0179 (5)0.940 (3)
C1L0.56475 (19)0.05920 (10)0.17744 (9)0.0173 (5)0.940 (3)
H1L10.63530.08910.18010.021*0.940 (3)
H1L20.55870.05460.21490.021*0.940 (3)
C2L0.4522 (2)0.09188 (12)0.15678 (11)0.0133 (5)0.940 (3)
C3L0.4590 (2)0.09538 (12)0.09765 (11)0.0123 (6)0.940 (3)
H3L10.38560.11490.08360.015*0.940 (3)
H3L20.52750.12530.09750.015*0.940 (3)
C4L0.3608 (2)0.19887 (11)0.18591 (11)0.0187 (6)0.940 (3)
H4L10.37200.24250.21420.028*0.940 (3)
H4L20.28580.17650.18830.028*0.940 (3)
H4L30.35810.20640.14920.028*0.940 (3)
C5L0.3154 (2)0.04691 (11)0.20393 (10)0.0223 (6)0.940 (3)
H5L10.23880.02170.19700.033*0.940 (3)
H5L20.30960.09150.23000.033*0.940 (3)
H5L30.37730.02160.21970.033*0.940 (3)
P10L0.5686 (14)0.0053 (8)0.0785 (6)0.01129 (18)0.060 (3)
O10L0.5348 (16)0.0055 (7)0.1378 (6)0.018 (2)*0.060 (3)
O23L0.4279 (18)0.1598 (7)0.1917 (7)0.014 (2)*0.060 (3)
O24L0.3045 (12)0.0684 (10)0.1370 (7)0.016 (2)*0.060 (3)
O30L0.4675 (16)0.0404 (9)0.0584 (5)0.011 (2)*0.060 (3)
O40L0.6881 (14)0.0280 (13)0.0838 (10)0.013 (4)*0.060 (3)
O50L0.546 (2)0.0759 (8)0.0430 (8)0.010 (4)*0.060 (3)
C10L0.5143 (15)0.0566 (8)0.1752 (5)0.0173 (17)*0.060 (3)
H10E0.58990.08400.18710.021*0.060 (3)
H10F0.48800.04750.20840.021*0.060 (3)
C20L0.4199 (13)0.0977 (6)0.1504 (6)0.0162 (17)*0.060 (3)
C30L0.4527 (17)0.1058 (7)0.0957 (6)0.012 (2)*0.060 (3)
H30E0.38920.12960.07860.015*0.060 (3)
H30F0.52760.13360.10290.015*0.060 (3)
C40L0.423 (4)0.2193 (7)0.1713 (11)0.033 (4)*0.060 (3)
H40G0.48990.25060.19020.049*0.060 (3)
H40H0.34780.24170.17830.049*0.060 (3)
H40I0.42660.20580.13150.049*0.060 (3)
C50L0.247 (2)0.0617 (19)0.1823 (10)0.019 (4)*0.060 (3)
H50G0.18200.02720.16870.029*0.060 (3)
H50H0.21470.10520.20000.029*0.060 (3)
H50I0.30470.04800.20920.029*0.060 (3)
N10.83346 (16)0.11681 (9)0.48824 (9)0.0157 (5)
H1N0.90460.11730.50880.024*
H2N0.77700.13120.51020.024*
H3N0.84310.14200.46490.024*
H4N0.82050.07430.46600.024*
N20.65569 (16)0.29106 (9)0.51313 (9)0.0155 (5)
H5N0.64120.33430.52990.023*
H6N0.58630.27430.49210.023*
H7N0.71280.29550.49260.023*
H8N0.67480.26250.53410.023*
N30.84162 (16)0.45157 (9)0.48693 (9)0.0156 (5)
H9N0.81970.41040.46380.023*
H10N0.86260.47810.46630.023*
H11N0.90980.44760.50830.023*
H12N0.78620.46870.50880.023*
N40.65215 (16)0.62529 (9)0.50954 (9)0.0162 (5)
H13N0.67360.59830.53160.024*
H14N0.63610.66730.52880.024*
H15N0.58230.60720.48980.024*
H16N0.71150.63250.49110.024*
N50.85680 (16)0.78529 (9)0.49817 (9)0.0167 (5)
H17N0.92460.78530.52100.025*
H18N0.86870.81230.47650.025*
H19N0.79720.80070.51800.025*
H20N0.84030.74320.47580.025*
N60.66109 (17)0.95550 (9)0.50437 (9)0.0173 (5)
H21N0.64760.99870.52180.026*
H22N0.71990.95890.48440.026*
H23N0.58900.94070.48520.026*
H24N0.67990.92620.52470.026*
N70.84057 (16)0.95508 (9)0.00648 (9)0.0160 (5)
H25N0.85520.98260.02730.024*
H26N0.91010.95310.01470.024*
H27N0.81520.91270.02590.024*
H28N0.78240.97270.01350.024*
N80.65182 (16)0.78903 (9)0.00867 (9)0.0149 (5)
H29N0.67000.75940.02880.022*
H30N0.70870.79330.01200.022*
H31N0.58150.77450.01240.022*
H32N0.64220.82960.03220.022*
N90.83946 (16)0.61624 (9)0.01318 (9)0.0166 (5)
H33N0.81340.57500.03500.025*
H34N0.91030.61350.00660.025*
H35N0.85460.64360.03410.025*
H36N0.78180.63150.00790.025*
N100.65996 (17)0.45948 (9)0.00662 (9)0.0160 (5)
H37N0.67540.42900.02610.024*
H38N0.58960.44460.01420.024*
H39N0.71710.46470.01370.024*
H40N0.65420.49940.03170.024*
N110.84896 (16)0.28312 (9)0.00844 (9)0.0153 (5)
H41N0.86260.31070.02950.023*
H42N0.82490.24110.02930.023*
H43N0.79050.30050.01150.023*
H44N0.91870.28120.01250.023*
N120.65982 (17)0.12548 (9)0.01303 (9)0.0161 (5)
H45N0.67790.09820.03520.024*
H46N0.58840.11020.00660.024*
H47N0.71780.12930.00730.024*
H48N0.65520.16610.03750.024*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P1A0.0132 (3)0.0123 (4)0.0146 (4)0.0029 (3)0.0033 (3)0.0035 (3)
O1A0.0148 (8)0.0213 (9)0.0128 (9)0.0067 (6)0.0028 (6)0.0047 (8)
O21A0.0179 (8)0.0136 (9)0.0139 (9)0.0016 (6)0.0019 (6)0.0022 (7)
O22A0.0127 (7)0.0203 (8)0.0180 (9)0.0000 (6)0.0042 (6)0.0064 (7)
O3A0.0141 (8)0.0137 (9)0.0128 (10)0.0050 (7)0.0013 (7)0.0024 (8)
O4A0.0140 (8)0.0169 (9)0.0176 (10)0.0010 (7)0.0030 (7)0.0043 (8)
O5A0.0185 (9)0.0116 (9)0.0238 (11)0.0028 (7)0.0032 (7)0.0039 (8)
C1A0.0159 (11)0.0110 (11)0.0152 (13)0.0029 (8)0.0057 (9)0.0036 (10)
C2A0.0161 (11)0.0096 (12)0.0140 (13)0.0019 (9)0.0041 (9)0.0017 (10)
C3A0.0158 (12)0.0132 (13)0.0127 (14)0.0049 (9)0.0045 (10)0.0050 (11)
C4A0.0307 (13)0.0106 (12)0.0232 (14)0.0045 (9)0.0066 (10)0.0021 (10)
C5A0.0195 (12)0.0258 (13)0.0220 (14)0.0003 (10)0.0092 (10)0.0083 (11)
P1B0.0148 (3)0.0121 (3)0.0145 (4)0.0003 (2)0.0032 (3)0.0050 (3)
O1B0.0167 (8)0.0204 (9)0.0131 (9)0.0032 (7)0.0034 (7)0.0031 (8)
O21B0.0189 (8)0.0154 (9)0.0149 (10)0.0001 (7)0.0028 (7)0.0074 (8)
O22B0.0166 (8)0.0274 (10)0.0227 (10)0.0080 (7)0.0073 (7)0.0093 (8)
O3B0.0168 (8)0.0147 (9)0.0106 (10)0.0007 (7)0.0033 (7)0.0046 (8)
O4B0.0159 (8)0.0150 (9)0.0187 (10)0.0034 (7)0.0062 (7)0.0049 (8)
O5B0.0203 (9)0.0147 (9)0.0220 (11)0.0006 (7)0.0050 (7)0.0077 (8)
C1B0.0259 (13)0.0173 (13)0.0141 (13)0.0006 (10)0.0055 (10)0.0013 (11)
C2B0.0164 (12)0.0156 (13)0.0137 (14)0.0013 (10)0.0050 (10)0.0057 (11)
C3B0.0164 (12)0.0125 (13)0.0137 (14)0.0000 (10)0.0048 (10)0.0043 (11)
C4B0.0420 (15)0.0133 (12)0.0260 (15)0.0048 (10)0.0079 (12)0.0083 (11)
C5B0.0242 (14)0.0351 (16)0.0356 (18)0.0132 (11)0.0160 (12)0.0104 (14)
P1C0.0149 (3)0.0106 (3)0.0141 (4)0.0030 (3)0.0038 (3)0.0032 (3)
O1C0.0172 (8)0.0209 (9)0.0134 (9)0.0069 (7)0.0031 (6)0.0053 (8)
O21C0.0189 (8)0.0148 (9)0.0151 (10)0.0033 (6)0.0025 (7)0.0022 (8)
O22C0.0158 (8)0.0243 (9)0.0192 (9)0.0019 (6)0.0065 (7)0.0044 (7)
O3C0.0156 (9)0.0127 (9)0.0122 (10)0.0037 (7)0.0025 (7)0.0021 (8)
O4C0.0161 (8)0.0156 (9)0.0191 (10)0.0007 (7)0.0046 (7)0.0044 (8)
O5C0.0190 (9)0.0143 (9)0.0234 (11)0.0028 (7)0.0047 (8)0.0033 (8)
C1C0.0214 (11)0.0129 (11)0.0127 (12)0.0034 (9)0.0073 (9)0.0049 (10)
C2C0.0178 (11)0.0084 (11)0.0108 (12)0.0032 (9)0.0053 (9)0.0009 (10)
C3C0.0175 (12)0.0134 (13)0.0130 (14)0.0038 (10)0.0046 (10)0.0060 (12)
C4C0.0347 (14)0.0125 (12)0.0245 (15)0.0074 (10)0.0077 (11)0.0052 (11)
C5C0.0224 (12)0.0330 (14)0.0296 (16)0.0024 (10)0.0142 (11)0.0085 (12)
P1D0.0126 (3)0.0138 (4)0.0149 (4)0.0009 (3)0.0026 (3)0.0055 (3)
O1D0.0125 (8)0.0183 (9)0.0151 (10)0.0000 (7)0.0019 (7)0.0048 (8)
O21D0.0189 (8)0.0138 (9)0.0154 (10)0.0002 (7)0.0018 (7)0.0068 (8)
O22D0.0159 (8)0.0229 (9)0.0183 (10)0.0062 (7)0.0054 (7)0.0049 (8)
O3D0.0152 (8)0.0175 (9)0.0125 (10)0.0025 (7)0.0023 (7)0.0056 (8)
O4D0.0150 (8)0.0158 (9)0.0171 (10)0.0030 (7)0.0052 (7)0.0045 (8)
O5D0.0191 (9)0.0168 (9)0.0205 (10)0.0005 (7)0.0031 (7)0.0088 (8)
C1D0.0247 (13)0.0151 (13)0.0159 (14)0.0016 (10)0.0071 (10)0.0030 (11)
C2D0.0140 (12)0.0120 (12)0.0151 (14)0.0012 (9)0.0033 (9)0.0047 (11)
C3D0.0170 (12)0.0119 (13)0.0110 (14)0.0013 (10)0.0041 (10)0.0014 (11)
C4D0.0265 (13)0.0158 (13)0.0230 (15)0.0013 (10)0.0059 (10)0.0094 (11)
C5D0.0235 (13)0.0264 (14)0.0282 (16)0.0083 (10)0.0132 (11)0.0073 (12)
P1E0.0109 (4)0.0102 (5)0.0126 (4)0.0009 (3)0.0023 (3)0.0031 (3)
O1E0.0183 (8)0.0127 (9)0.0124 (9)0.0042 (7)0.0036 (6)0.0037 (8)
O21E0.0155 (8)0.0087 (9)0.0140 (10)0.0040 (7)0.0032 (7)0.0002 (8)
O22E0.0097 (7)0.0177 (8)0.0126 (8)0.0026 (6)0.0013 (6)0.0037 (7)
O3E0.0128 (9)0.0128 (10)0.0122 (10)0.0039 (7)0.0029 (7)0.0009 (8)
O4E0.0120 (9)0.0152 (9)0.0163 (10)0.0010 (8)0.0035 (7)0.0051 (8)
O5E0.0166 (11)0.0100 (10)0.0181 (12)0.0001 (8)0.0012 (8)0.0011 (8)
C1E0.0113 (10)0.0125 (11)0.0085 (11)0.0013 (8)0.0015 (8)0.0005 (9)
C2E0.0113 (11)0.0112 (11)0.0084 (12)0.0011 (9)0.0025 (9)0.0004 (10)
C3E0.0152 (12)0.0146 (14)0.0166 (15)0.0063 (10)0.0037 (10)0.0049 (12)
C4E0.0191 (13)0.0163 (13)0.0177 (14)0.0103 (9)0.0025 (10)0.0032 (11)
C5E0.0186 (12)0.0244 (13)0.0193 (14)0.0025 (10)0.0058 (10)0.0096 (11)
O40E0.0120 (9)0.0152 (9)0.0163 (10)0.0010 (8)0.0035 (7)0.0051 (8)
P1F0.0128 (3)0.0139 (3)0.0131 (4)0.0006 (2)0.0022 (3)0.0047 (3)
O1F0.0196 (8)0.0207 (9)0.0134 (9)0.0045 (7)0.0039 (7)0.0032 (8)
O21F0.0133 (8)0.0195 (9)0.0152 (10)0.0014 (6)0.0032 (7)0.0086 (8)
O22F0.0172 (8)0.0278 (9)0.0168 (9)0.0099 (7)0.0043 (7)0.0073 (8)
O3F0.0151 (8)0.0186 (9)0.0125 (10)0.0030 (7)0.0009 (7)0.0075 (8)
O4F0.0150 (8)0.0145 (9)0.0178 (10)0.0010 (7)0.0022 (7)0.0044 (8)
O5F0.0180 (8)0.0164 (9)0.0216 (10)0.0007 (7)0.0017 (7)0.0101 (8)
C1F0.0197 (11)0.0191 (12)0.0122 (12)0.0019 (9)0.0011 (9)0.0021 (10)
C2F0.0149 (11)0.0168 (13)0.0161 (14)0.0033 (9)0.0051 (9)0.0082 (11)
C3F0.0155 (12)0.0169 (13)0.0151 (14)0.0016 (10)0.0027 (10)0.0060 (11)
C4F0.0258 (13)0.0185 (13)0.0216 (14)0.0055 (10)0.0034 (11)0.0076 (11)
C5F0.0281 (13)0.0251 (13)0.0225 (15)0.0109 (10)0.0106 (11)0.0039 (12)
P1G0.0128 (3)0.0125 (3)0.0105 (4)0.0000 (2)0.0036 (2)0.0039 (3)
O1G0.0138 (8)0.0209 (9)0.0119 (9)0.0046 (7)0.0033 (6)0.0023 (8)
O21G0.0165 (8)0.0159 (9)0.0129 (10)0.0004 (7)0.0023 (7)0.0066 (8)
O22G0.0122 (8)0.0200 (9)0.0173 (9)0.0023 (6)0.0015 (6)0.0055 (7)
O3G0.0151 (8)0.0144 (9)0.0116 (10)0.0024 (7)0.0022 (7)0.0053 (8)
O4G0.0142 (8)0.0157 (9)0.0181 (10)0.0004 (7)0.0041 (7)0.0050 (8)
O5G0.0162 (8)0.0149 (9)0.0242 (11)0.0017 (7)0.0048 (7)0.0099 (8)
C1G0.0155 (11)0.0151 (12)0.0142 (13)0.0017 (9)0.0058 (9)0.0037 (10)
C2G0.0113 (11)0.0168 (13)0.0151 (14)0.0008 (9)0.0030 (9)0.0081 (11)
C3G0.0155 (12)0.0095 (12)0.0128 (14)0.0024 (9)0.0042 (10)0.0034 (11)
C4G0.0235 (12)0.0200 (13)0.0262 (16)0.0021 (10)0.0035 (10)0.0127 (12)
C5G0.0156 (11)0.0268 (13)0.0210 (14)0.0081 (9)0.0062 (10)0.0077 (11)
P1H0.0121 (3)0.0118 (3)0.0110 (4)0.0023 (3)0.0032 (3)0.0014 (3)
O1H0.0113 (7)0.0240 (9)0.0146 (9)0.0048 (6)0.0025 (6)0.0064 (8)
O21H0.0149 (8)0.0113 (8)0.0165 (10)0.0007 (6)0.0012 (7)0.0017 (7)
O22H0.0141 (8)0.0232 (9)0.0210 (9)0.0012 (6)0.0050 (6)0.0038 (7)
O3H0.0152 (8)0.0124 (9)0.0112 (10)0.0044 (7)0.0023 (7)0.0005 (8)
O4H0.0152 (8)0.0144 (9)0.0186 (10)0.0020 (7)0.0045 (7)0.0050 (8)
O5H0.0176 (9)0.0117 (9)0.0223 (11)0.0018 (7)0.0040 (7)0.0032 (8)
C1H0.0220 (12)0.0240 (13)0.0159 (13)0.0051 (9)0.0066 (9)0.0049 (11)
C2H0.0142 (11)0.0148 (12)0.0162 (14)0.0033 (9)0.0038 (9)0.0035 (10)
C3H0.0173 (12)0.0113 (13)0.0123 (14)0.0040 (9)0.0050 (10)0.0033 (11)
C4H0.0242 (13)0.0149 (12)0.0274 (15)0.0098 (9)0.0029 (10)0.0006 (11)
C5H0.0210 (12)0.0290 (14)0.0268 (15)0.0035 (10)0.0106 (10)0.0040 (12)
P1I0.0117 (4)0.0102 (4)0.0114 (4)0.0015 (3)0.0044 (3)0.0040 (3)
O1I0.0170 (9)0.0112 (9)0.0136 (10)0.0009 (7)0.0048 (7)0.0043 (8)
O21I0.0180 (9)0.0135 (11)0.0128 (10)0.0026 (8)0.0030 (7)0.0077 (9)
O22I0.0098 (8)0.0172 (9)0.0155 (9)0.0030 (7)0.0023 (7)0.0051 (8)
O3I0.0147 (9)0.0142 (10)0.0119 (10)0.0029 (7)0.0031 (7)0.0053 (8)
O4I0.0138 (10)0.0156 (11)0.0170 (12)0.0025 (8)0.0073 (8)0.0044 (9)
O5I0.0152 (10)0.0146 (10)0.0184 (13)0.0005 (8)0.0003 (9)0.0093 (9)
C1I0.0130 (11)0.0147 (12)0.0099 (12)0.0018 (9)0.0022 (9)0.0032 (10)
C2I0.0108 (11)0.0132 (12)0.0101 (13)0.0016 (9)0.0004 (9)0.0043 (10)
C3I0.0163 (13)0.0133 (14)0.0131 (15)0.0020 (10)0.0055 (11)0.0056 (12)
C4I0.0163 (14)0.0152 (13)0.0212 (15)0.0064 (11)0.0034 (11)0.0044 (12)
C5I0.0197 (13)0.0189 (14)0.0229 (16)0.0086 (10)0.0074 (11)0.0050 (12)
P1J0.0131 (3)0.0115 (3)0.0109 (4)0.0022 (3)0.0030 (3)0.0023 (3)
O1J0.0147 (8)0.0182 (9)0.0141 (9)0.0041 (6)0.0032 (6)0.0059 (8)
O21J0.0250 (9)0.0110 (8)0.0145 (10)0.0011 (7)0.0045 (7)0.0020 (7)
O22J0.0152 (8)0.0234 (9)0.0225 (10)0.0016 (6)0.0045 (7)0.0075 (8)
O3J0.0154 (8)0.0125 (9)0.0116 (10)0.0020 (7)0.0017 (7)0.0000 (8)
O4J0.0157 (8)0.0137 (9)0.0180 (10)0.0015 (7)0.0054 (7)0.0044 (8)
O5J0.0163 (9)0.0120 (9)0.0212 (11)0.0022 (7)0.0022 (7)0.0021 (8)
C1J0.0208 (12)0.0202 (13)0.0168 (13)0.0027 (9)0.0061 (10)0.0071 (11)
C2J0.0132 (11)0.0148 (13)0.0147 (13)0.0010 (9)0.0059 (9)0.0031 (11)
C3J0.0151 (12)0.0107 (13)0.0147 (14)0.0028 (9)0.0037 (10)0.0041 (11)
C4J0.0355 (15)0.0175 (13)0.0276 (16)0.0066 (10)0.0060 (12)0.0039 (11)
C5J0.0228 (12)0.0285 (14)0.0326 (16)0.0022 (10)0.0153 (11)0.0123 (13)
P1K0.0135 (3)0.0116 (3)0.0108 (4)0.0003 (2)0.0038 (2)0.0036 (3)
O1K0.0137 (8)0.0166 (9)0.0131 (9)0.0015 (6)0.0030 (6)0.0027 (7)
O21K0.0230 (9)0.0144 (9)0.0138 (10)0.0029 (7)0.0044 (7)0.0059 (8)
O22K0.0142 (8)0.0196 (9)0.0205 (10)0.0034 (6)0.0062 (7)0.0045 (8)
O3K0.0157 (8)0.0143 (9)0.0122 (10)0.0027 (7)0.0029 (7)0.0056 (8)
O4K0.0155 (8)0.0159 (9)0.0166 (10)0.0014 (7)0.0043 (7)0.0051 (8)
O5K0.0172 (8)0.0143 (9)0.0227 (10)0.0008 (7)0.0043 (7)0.0091 (8)
C1K0.0166 (11)0.0138 (12)0.0136 (13)0.0037 (9)0.0069 (9)0.0022 (10)
C2K0.0126 (11)0.0127 (13)0.0124 (14)0.0024 (9)0.0048 (9)0.0038 (11)
C3K0.0177 (12)0.0099 (13)0.0151 (15)0.0022 (10)0.0063 (10)0.0034 (11)
C4K0.0314 (13)0.0191 (13)0.0252 (15)0.0014 (10)0.0060 (11)0.0106 (11)
C5K0.0192 (12)0.0216 (13)0.0309 (16)0.0068 (10)0.0141 (11)0.0053 (12)
P1L0.0116 (4)0.0113 (4)0.0114 (4)0.0046 (3)0.0041 (3)0.0023 (3)
O1L0.0174 (9)0.0237 (9)0.0114 (9)0.0103 (7)0.0032 (7)0.0050 (8)
O21L0.0108 (9)0.0179 (9)0.0125 (10)0.0069 (7)0.0021 (7)0.0012 (8)
O22L0.0171 (8)0.0215 (9)0.0154 (9)0.0036 (7)0.0041 (7)0.0037 (7)
O3L0.0168 (9)0.0106 (10)0.0114 (10)0.0052 (7)0.0018 (7)0.0016 (8)
O4L0.0151 (9)0.0132 (10)0.0160 (12)0.0021 (7)0.0052 (8)0.0035 (9)
O5L0.0170 (10)0.0098 (10)0.0257 (12)0.0041 (7)0.0025 (8)0.0032 (9)
C1L0.0134 (11)0.0231 (12)0.0151 (12)0.0051 (9)0.0006 (9)0.0052 (10)
C2L0.0123 (11)0.0163 (12)0.0131 (12)0.0030 (9)0.0036 (9)0.0059 (10)
C3L0.0155 (12)0.0107 (13)0.0112 (14)0.0054 (10)0.0038 (10)0.0027 (11)
C4L0.0239 (13)0.0134 (12)0.0208 (14)0.0090 (10)0.0078 (10)0.0056 (11)
C5L0.0260 (13)0.0222 (13)0.0224 (14)0.0021 (10)0.0111 (10)0.0086 (11)
P10L0.0116 (4)0.0113 (4)0.0114 (4)0.0046 (3)0.0041 (3)0.0023 (3)
N10.0168 (10)0.0150 (11)0.0165 (12)0.0022 (8)0.0040 (8)0.0052 (9)
N20.0152 (10)0.0138 (11)0.0195 (13)0.0022 (8)0.0055 (9)0.0062 (10)
N30.0158 (10)0.0133 (11)0.0183 (12)0.0008 (8)0.0063 (8)0.0035 (9)
N40.0141 (10)0.0149 (11)0.0229 (13)0.0048 (8)0.0081 (9)0.0080 (10)
N50.0155 (10)0.0143 (11)0.0231 (13)0.0024 (8)0.0083 (8)0.0070 (9)
N60.0179 (10)0.0121 (11)0.0243 (13)0.0041 (8)0.0065 (9)0.0072 (10)
N70.0158 (10)0.0133 (11)0.0213 (13)0.0010 (8)0.0048 (8)0.0077 (9)
N80.0161 (10)0.0125 (11)0.0169 (12)0.0022 (8)0.0044 (8)0.0040 (9)
N90.0178 (10)0.0139 (11)0.0202 (13)0.0013 (8)0.0085 (9)0.0054 (9)
N100.0173 (10)0.0117 (11)0.0194 (13)0.0003 (8)0.0047 (9)0.0038 (10)
N110.0156 (10)0.0128 (11)0.0186 (12)0.0018 (8)0.0051 (8)0.0047 (9)
N120.0172 (10)0.0145 (11)0.0180 (12)0.0008 (8)0.0065 (9)0.0051 (10)
Geometric parameters (Å, º) top
P1A—O5A1.4868 (17)C2H—C3H1.527 (4)
P1A—O4A1.4881 (17)C3H—H3H10.9900
P1A—O1A1.6059 (19)C3H—H3H20.9900
P1A—O3A1.6079 (17)C4H—H4H10.9800
O1A—C1A1.442 (2)C4H—H4H20.9800
O21A—C2A1.408 (3)C4H—H4H30.9800
O21A—C4A1.442 (2)C5H—H5H10.9800
O22A—C2A1.426 (2)C5H—H5H20.9800
O22A—C5A1.432 (3)C5H—H5H30.9800
O3A—C3A1.443 (3)P1I—O5I1.4855 (18)
C1A—C2A1.529 (3)P1I—O4I1.492 (2)
C1A—H1A10.9900P1I—O1I1.5990 (19)
C1A—H1A20.9900P1I—O3I1.6009 (17)
C2A—C3A1.538 (4)O1I—C1I1.445 (2)
C3A—H3A10.9900O21I—C2I1.421 (3)
C3A—H3A20.9900O21I—C4I1.433 (2)
C4A—H4A10.9800O22I—C2I1.407 (3)
C4A—H4A20.9800O22I—C5I1.422 (3)
C4A—H4A30.9800O3I—C3I1.442 (3)
C5A—H5A10.9800C1I—C2I1.527 (3)
C5A—H5A20.9800C1I—H1I10.9900
C5A—H5A30.9800C1I—H1I20.9900
P1B—O5B1.4868 (16)C2I—C3I1.531 (4)
P1B—O4B1.4904 (18)C3I—H3I10.9900
P1B—O1B1.6059 (18)C3I—H3I20.9900
P1B—O3B1.6065 (16)C4I—H4I10.9800
O1B—C1B1.428 (3)C4I—H4I20.9800
O21B—C2B1.411 (3)C4I—H4I30.9800
O21B—C4B1.438 (2)C5I—H5I10.9800
O22B—C2B1.415 (3)C5I—H5I20.9800
O22B—C5B1.439 (3)C5I—H5I30.9800
O3B—C3B1.448 (3)P10I—O50I1.485 (3)
C1B—C2B1.533 (3)P10I—O40I1.490 (3)
C1B—H1B10.9900P10I—O10I1.601 (3)
C1B—H1B20.9900P10I—O30I1.603 (2)
C2B—C3B1.524 (4)O10I—C10I1.445 (3)
C3B—H3B10.9900O23I—C20I1.423 (3)
C3B—H3B20.9900O23I—C40I1.434 (3)
C4B—H4B10.9800O24I—C20I1.409 (3)
C4B—H4B20.9800O24I—C50I1.423 (3)
C4B—H4B30.9800O30I—C30I1.441 (3)
C5B—H5B10.9800C10I—C20I1.524 (3)
C5B—H5B20.9800C10I—H10C0.9900
C5B—H5B30.9800C10I—H10D0.9900
P1C—O4C1.4876 (17)C20I—C30I1.529 (4)
P1C—O5C1.4888 (17)C30I—H30C0.9900
P1C—O1C1.6053 (19)C30I—H30D0.9900
P1C—O3C1.6122 (18)C40I—H40D0.9800
O1C—C1C1.445 (2)C40I—H40E0.9800
O21C—C2C1.411 (3)C40I—H40F0.9800
O21C—C4C1.438 (2)C50I—H50D0.9800
O22C—C2C1.421 (2)C50I—H50E0.9800
O22C—C5C1.428 (3)C50I—H50F0.9800
O3C—C3C1.440 (3)P1J—O5J1.4876 (17)
C1C—C2C1.535 (3)P1J—O4J1.4892 (17)
C1C—H1C10.9900P1J—O3J1.6057 (18)
C1C—H1C20.9900P1J—O1J1.6060 (19)
C2C—C3C1.534 (3)O1J—C1J1.434 (3)
C3C—H3C10.9900O21J—C2J1.410 (3)
C3C—H3C20.9900O21J—C4J1.440 (2)
C4C—H4C10.9800O22J—C2J1.417 (3)
C4C—H4C20.9800O22J—C5J1.437 (3)
C4C—H4C30.9800O3J—C3J1.440 (3)
C5C—H5C10.9800C1J—C2J1.528 (3)
C5C—H5C20.9800C1J—H1J10.9900
C5C—H5C30.9800C1J—H1J20.9900
P1D—O5D1.4873 (17)C2J—C3J1.532 (4)
P1D—O4D1.4899 (18)C3J—H3J10.9900
P1D—O1D1.6074 (19)C3J—H3J20.9900
P1D—O3D1.6105 (16)C4J—H4J10.9800
O1D—C1D1.442 (3)C4J—H4J20.9800
O21D—C2D1.407 (3)C4J—H4J30.9800
O21D—C4D1.450 (2)C5J—H5J10.9800
O22D—C2D1.415 (3)C5J—H5J20.9800
O22D—C5D1.431 (3)C5J—H5J30.9800
O3D—C3D1.449 (3)P1K—O5K1.4882 (17)
C1D—C2D1.529 (3)P1K—O4K1.4918 (19)
C1D—H1D10.9900P1K—O1K1.6033 (18)
C1D—H1D20.9900P1K—O3K1.6069 (16)
C2D—C3D1.530 (4)O1K—C1K1.447 (2)
C3D—H3D10.9900O21K—C2K1.418 (3)
C3D—H3D20.9900O21K—C4K1.441 (2)
C4D—H4D10.9800O22K—C2K1.423 (3)
C4D—H4D20.9800O22K—C5K1.428 (3)
C4D—H4D30.9800O3K—C3K1.437 (3)
C5D—H5D10.9800C1K—C2K1.527 (3)
C5D—H5D20.9800C1K—H1K10.9900
C5D—H5D30.9800C1K—H1K20.9900
P1E—O4E1.4870 (17)C2K—C3K1.534 (4)
P1E—O5E1.4910 (18)C3K—H3K10.9900
P1E—O1E1.6052 (19)C3K—H3K20.9900
P1E—O3E1.6074 (18)C4K—H4K10.9800
O1E—C1E1.440 (3)C4K—H4K20.9800
O21E—C2E1.418 (3)C4K—H4K30.9800
O21E—C4E1.436 (3)C5K—H5K10.9800
O22E—C2E1.412 (2)C5K—H5K20.9800
O22E—C5E1.424 (3)C5K—H5K30.9800
O3E—C3E1.438 (3)P1L—O5L1.4847 (18)
C1E—C2E1.523 (3)P1L—O4L1.4891 (17)
C1E—H1E10.9900P1L—O1L1.6000 (19)
C1E—H1E20.9900P1L—O3L1.6002 (18)
C2E—C3E1.531 (4)O1L—C1L1.412 (3)
C3E—H3E10.9900O21L—C2L1.405 (3)
C3E—H3E20.9900O21L—C4L1.446 (3)
C4E—H4E10.9800O22L—C2L1.398 (2)
C4E—H4E20.9800O22L—C5L1.430 (3)
C4E—H4E30.9800O3L—C3L1.442 (3)
C5E—H5E10.9800C1L—C2L1.540 (3)
C5E—H5E20.9800C1L—H1L10.9900
C5E—H5E30.9800C1L—H1L20.9900
P10E—O40E1.485 (2)C2L—C3L1.533 (4)
P10E—O50E1.490 (3)C3L—H3L10.9900
P10E—O10E1.608 (3)C3L—H3L20.9900
P10E—O30E1.610 (3)C4L—H4L10.9800
O10E—C10E1.442 (3)C4L—H4L20.9800
O23E—C20E1.419 (3)C4L—H4L30.9800
O23E—C40E1.436 (3)C5L—H5L10.9800
O24E—C20E1.413 (3)C5L—H5L20.9800
O24E—C50E1.424 (3)C5L—H5L30.9800
O30E—C30E1.437 (3)P10L—O50L1.484 (3)
C10E—C20E1.522 (3)P10L—O40L1.489 (2)
C10E—H10A0.9900P10L—O10L1.600 (3)
C10E—H10B0.9900P10L—O30L1.600 (3)
C20E—C30E1.530 (4)O10L—C10L1.409 (3)
C30E—H30A0.9900O23L—C20L1.407 (3)
C30E—H30B0.9900O23L—C40L1.446 (3)
C40E—H40A0.9800O24L—C20L1.398 (3)
C40E—H40B0.9800O24L—C50L1.430 (3)
C40E—H40C0.9800O30L—C30L1.442 (3)
C50E—H50A0.9800C10L—C20L1.537 (3)
C50E—H50B0.9800C10L—H10E0.9900
C50E—H50C0.9800C10L—H10F0.9900
P1F—O5F1.4847 (17)C20L—C30L1.532 (4)
P1F—O4F1.4890 (18)C30L—H30E0.9900
P1F—O3F1.6012 (16)C30L—H30F0.9900
P1F—O1F1.6023 (18)C40L—H40G0.9800
O1F—C1F1.417 (2)C40L—H40H0.9800
O21F—C2F1.408 (3)C40L—H40I0.9800
O21F—C4F1.441 (2)C50L—H50G0.9800
O22F—C2F1.401 (3)C50L—H50H0.9800
O22F—C5F1.428 (3)C50L—H50I0.9800
O3F—C3F1.449 (3)N1—H1N0.9004
C1F—C2F1.537 (3)N1—H2N0.9015
C1F—H1F10.9900N1—H3N0.8997
C1F—H1F20.9900N1—H4N0.9008
C2F—C3F1.518 (4)N2—H5N0.9005
C3F—H3F10.9900N2—H6N0.9010
C3F—H3F20.9900N2—H7N0.9015
C4F—H4F10.9800N2—H8N0.9005
C4F—H4F20.9800N3—H9N0.9009
C4F—H4F30.9800N3—H10N0.9002
C5F—H5F10.9800N3—H11N0.9011
C5F—H5F20.9800N3—H12N0.9017
C5F—H5F30.9800N4—H13N0.9001
P1G—O4G1.4831 (19)N4—H14N0.9003
P1G—O5G1.4890 (17)N4—H15N0.9005
P1G—O1G1.6054 (19)N4—H16N0.9013
P1G—O3G1.6090 (16)N5—H17N0.9007
O1G—C1G1.443 (2)N5—H18N0.8995
O21G—C2G1.418 (3)N5—H19N0.9014
O21G—C4G1.439 (2)N5—H20N0.8997
O22G—C2G1.428 (2)N6—H21N0.8998
O22G—C5G1.433 (3)N6—H22N0.9011
O3G—C3G1.443 (3)N6—H23N0.9008
C1G—C2G1.531 (3)N6—H24N0.8997
C1G—H1G10.9900N7—H25N0.8994
C1G—H1G20.9900N7—H26N0.9012
C2G—C3G1.527 (4)N7—H27N0.9000
C3G—H3G10.9900N7—H28N0.9015
C3G—H3G20.9900N8—H29N0.9000
C4G—H4G10.9800N8—H30N0.9011
C4G—H4G20.9800N8—H31N0.9004
C4G—H4G30.9800N8—H32N0.8999
C5G—H5G10.9800N9—H33N0.9007
C5G—H5G20.9800N9—H34N0.9006
C5G—H5G30.9800N9—H35N0.8999
P1H—O4H1.4811 (17)N9—H36N0.9014
P1H—O5H1.4895 (17)N10—H37N0.8999
P1H—O3H1.6072 (18)N10—H38N0.9006
P1H—O1H1.6083 (19)N10—H39N0.9012
O1H—C1H1.442 (3)N10—H40N0.8999
O21H—C2H1.408 (3)N11—H41N0.9002
O21H—C4H1.440 (2)N11—H42N0.9007
O22H—C2H1.427 (2)N11—H43N0.9016
O22H—C5H1.434 (3)N11—H44N0.9008
O3H—C3H1.449 (3)N12—H45N0.9002
C1H—C2H1.518 (3)N12—H46N0.9008
C1H—H1H10.9900N12—H47N0.9012
C1H—H1H20.9900N12—H48N0.9004
O5A—P1A—O4A118.36 (11)O21H—C2H—O22H111.47 (19)
O5A—P1A—O1A112.43 (10)O21H—C2H—C1H107.96 (18)
O4A—P1A—O1A106.24 (10)O22H—C2H—C1H110.38 (17)
O5A—P1A—O3A106.60 (10)O21H—C2H—C3H111.85 (18)
O4A—P1A—O3A111.44 (9)O22H—C2H—C3H105.67 (18)
O1A—P1A—O3A100.36 (10)C1H—C2H—C3H109.5 (2)
C1A—O1A—P1A113.98 (13)O3H—C3H—C2H109.23 (18)
C2A—O21A—C4A114.83 (17)O3H—C3H—H3H1109.8
C2A—O22A—C5A114.12 (17)C2H—C3H—H3H1109.8
C3A—O3A—P1A114.35 (15)O3H—C3H—H3H2109.8
O1A—C1A—C2A109.69 (16)C2H—C3H—H3H2109.8
O1A—C1A—H1A1109.7H3H1—C3H—H3H2108.3
C2A—C1A—H1A1109.7O21H—C4H—H4H1109.5
O1A—C1A—H1A2109.7O21H—C4H—H4H2109.5
C2A—C1A—H1A2109.7H4H1—C4H—H4H2109.5
H1A1—C1A—H1A2108.2O21H—C4H—H4H3109.5
O21A—C2A—O22A111.63 (19)H4H1—C4H—H4H3109.5
O21A—C2A—C1A107.79 (18)H4H2—C4H—H4H3109.5
O22A—C2A—C1A111.10 (17)O22H—C5H—H5H1109.5
O21A—C2A—C3A111.50 (18)O22H—C5H—H5H2109.5
O22A—C2A—C3A105.38 (19)H5H1—C5H—H5H2109.5
C1A—C2A—C3A109.5 (2)O22H—C5H—H5H3109.5
O3A—C3A—C2A108.93 (18)H5H1—C5H—H5H3109.5
O3A—C3A—H3A1109.9H5H2—C5H—H5H3109.5
C2A—C3A—H3A1109.9O5I—P1I—O4I118.82 (11)
O3A—C3A—H3A2109.9O5I—P1I—O1I106.73 (11)
C2A—C3A—H3A2109.9O4I—P1I—O1I110.04 (12)
H3A1—C3A—H3A2108.3O5I—P1I—O3I107.71 (11)
O21A—C4A—H4A1109.5O4I—P1I—O3I110.07 (10)
O21A—C4A—H4A2109.5O1I—P1I—O3I102.12 (10)
H4A1—C4A—H4A2109.5C1I—O1I—P1I117.23 (14)
O21A—C4A—H4A3109.5C2I—O21I—C4I114.91 (18)
H4A1—C4A—H4A3109.5C2I—O22I—C5I116.05 (19)
H4A2—C4A—H4A3109.5C3I—O3I—P1I117.02 (15)
O22A—C5A—H5A1109.5O1I—C1I—C2I110.56 (18)
O22A—C5A—H5A2109.5O1I—C1I—H1I1109.5
H5A1—C5A—H5A2109.5C2I—C1I—H1I1109.5
O22A—C5A—H5A3109.5O1I—C1I—H1I2109.5
H5A1—C5A—H5A3109.5C2I—C1I—H1I2109.5
H5A2—C5A—H5A3109.5H1I1—C1I—H1I2108.1
O5B—P1B—O4B118.20 (10)O22I—C2I—O21I113.1 (2)
O5B—P1B—O1B112.23 (10)O22I—C2I—C1I114.24 (19)
O4B—P1B—O1B106.58 (10)O21I—C2I—C1I103.36 (19)
O5B—P1B—O3B106.18 (9)O22I—C2I—C3I104.7 (2)
O4B—P1B—O3B111.59 (10)O21I—C2I—C3I111.66 (19)
O1B—P1B—O3B100.72 (9)C1I—C2I—C3I110.0 (2)
C1B—O1B—P1B114.13 (14)O3I—C3I—C2I109.92 (19)
C2B—O21B—C4B114.09 (18)O3I—C3I—H3I1109.7
C2B—O22B—C5B113.91 (19)C2I—C3I—H3I1109.7
C3B—O3B—P1B114.97 (15)O3I—C3I—H3I2109.7
O1B—C1B—C2B110.41 (19)C2I—C3I—H3I2109.7
O1B—C1B—H1B1109.6H3I1—C3I—H3I2108.2
C2B—C1B—H1B1109.6O21I—C4I—H4I1109.5
O1B—C1B—H1B2109.6O21I—C4I—H4I2109.5
C2B—C1B—H1B2109.6H4I1—C4I—H4I2109.5
H1B1—C1B—H1B2108.1O21I—C4I—H4I3109.5
O21B—C2B—O22B111.79 (19)H4I1—C4I—H4I3109.5
O21B—C2B—C3B111.5 (2)H4I2—C4I—H4I3109.5
O22B—C2B—C3B105.9 (2)O22I—C5I—H5I1109.5
O21B—C2B—C1B106.84 (19)O22I—C5I—H5I2109.5
O22B—C2B—C1B111.18 (19)H5I1—C5I—H5I2109.5
C3B—C2B—C1B109.7 (2)O22I—C5I—H5I3109.5
O3B—C3B—C2B109.73 (19)H5I1—C5I—H5I3109.5
O3B—C3B—H3B1109.7H5I2—C5I—H5I3109.5
C2B—C3B—H3B1109.7O50I—P10I—O40I119.2 (3)
O3B—C3B—H3B2109.7O50I—P10I—O10I106.9 (3)
C2B—C3B—H3B2109.7O40I—P10I—O10I110.2 (3)
H3B1—C3B—H3B2108.2O50I—P10I—O30I107.6 (3)
O21B—C4B—H4B1109.5O40I—P10I—O30I110.2 (3)
O21B—C4B—H4B2109.5O10I—P10I—O30I101.2 (2)
H4B1—C4B—H4B2109.5C10I—O10I—P10I116.7 (3)
O21B—C4B—H4B3109.5C20I—O23I—C40I114.7 (4)
H4B1—C4B—H4B3109.5C20I—O24I—C50I115.6 (4)
H4B2—C4B—H4B3109.5C30I—O30I—P10I116.7 (3)
O22B—C5B—H5B1109.5O10I—C10I—C20I111.4 (3)
O22B—C5B—H5B2109.5O10I—C10I—H10C109.3
H5B1—C5B—H5B2109.5C20I—C10I—H10C109.3
O22B—C5B—H5B3109.5O10I—C10I—H10D109.3
H5B1—C5B—H5B3109.5C20I—C10I—H10D109.3
H5B2—C5B—H5B3109.5H10C—C10I—H10D108.0
O4C—P1C—O5C118.48 (11)O24I—C20I—O23I112.3 (3)
O4C—P1C—O1C106.17 (10)O24I—C20I—C10I114.1 (3)
O5C—P1C—O1C112.33 (10)O23I—C20I—C10I103.4 (3)
O4C—P1C—O3C111.46 (9)O24I—C20I—C30I104.8 (3)
O5C—P1C—O3C106.29 (10)O23I—C20I—C30I111.4 (3)
O1C—P1C—O3C100.73 (10)C10I—C20I—C30I111.1 (3)
C1C—O1C—P1C113.59 (13)O30I—C30I—C20I110.9 (3)
C2C—O21C—C4C114.20 (17)O30I—C30I—H30C109.5
C2C—O22C—C5C114.02 (18)C20I—C30I—H30C109.5
C3C—O3C—P1C114.64 (15)O30I—C30I—H30D109.5
O1C—C1C—C2C109.53 (16)C20I—C30I—H30D109.5
O1C—C1C—H1C1109.8H30C—C30I—H30D108.0
C2C—C1C—H1C1109.8O23I—C40I—H40D109.5
O1C—C1C—H1C2109.8O23I—C40I—H40E109.5
C2C—C1C—H1C2109.8H40D—C40I—H40E109.5
H1C1—C1C—H1C2108.2O23I—C40I—H40F109.5
O21C—C2C—O22C112.03 (19)H40D—C40I—H40F109.5
O21C—C2C—C3C111.10 (18)H40E—C40I—H40F109.5
O22C—C2C—C3C105.71 (19)O24I—C50I—H50D109.5
O21C—C2C—C1C107.18 (18)O24I—C50I—H50E109.5
O22C—C2C—C1C111.11 (17)H50D—C50I—H50E109.5
C3C—C2C—C1C109.7 (2)O24I—C50I—H50F109.5
O3C—C3C—C2C109.34 (18)H50D—C50I—H50F109.5
O3C—C3C—H3C1109.8H50E—C50I—H50F109.5
C2C—C3C—H3C1109.8O5J—P1J—O4J118.38 (11)
O3C—C3C—H3C2109.8O5J—P1J—O3J106.85 (10)
C2C—C3C—H3C2109.8O4J—P1J—O3J111.45 (9)
H3C1—C3C—H3C2108.3O5J—P1J—O1J111.90 (10)
O21C—C4C—H4C1109.5O4J—P1J—O1J106.36 (10)
O21C—C4C—H4C2109.5O3J—P1J—O1J100.49 (10)
H4C1—C4C—H4C2109.5C1J—O1J—P1J114.34 (14)
O21C—C4C—H4C3109.5C2J—O21J—C4J114.69 (18)
H4C1—C4C—H4C3109.5C2J—O22J—C5J114.55 (18)
H4C2—C4C—H4C3109.5C3J—O3J—P1J114.61 (14)
O22C—C5C—H5C1109.5O1J—C1J—C2J110.02 (17)
O22C—C5C—H5C2109.5O1J—C1J—H1J1109.7
H5C1—C5C—H5C2109.5C2J—C1J—H1J1109.7
O22C—C5C—H5C3109.5O1J—C1J—H1J2109.7
H5C1—C5C—H5C3109.5C2J—C1J—H1J2109.7
H5C2—C5C—H5C3109.5H1J1—C1J—H1J2108.2
O5D—P1D—O4D118.34 (11)O21J—C2J—O22J111.2 (2)
O5D—P1D—O1D111.86 (10)O21J—C2J—C1J106.78 (19)
O4D—P1D—O1D106.86 (10)O22J—C2J—C1J111.56 (17)
O5D—P1D—O3D106.92 (9)O21J—C2J—C3J112.17 (18)
O4D—P1D—O3D111.02 (10)O22J—C2J—C3J105.60 (19)
O1D—P1D—O3D100.40 (10)C1J—C2J—C3J109.6 (2)
C1D—O1D—P1D113.87 (14)O3J—C3J—C2J109.41 (18)
C2D—O21D—C4D114.89 (18)O3J—C3J—H3J1109.8
C2D—O22D—C5D114.37 (18)C2J—C3J—H3J1109.8
C3D—O3D—P1D114.25 (15)O3J—C3J—H3J2109.8
O1D—C1D—C2D109.61 (18)C2J—C3J—H3J2109.8
O1D—C1D—H1D1109.7H3J1—C3J—H3J2108.2
C2D—C1D—H1D1109.7O21J—C4J—H4J1109.5
O1D—C1D—H1D2109.7O21J—C4J—H4J2109.5
C2D—C1D—H1D2109.7H4J1—C4J—H4J2109.5
H1D1—C1D—H1D2108.2O21J—C4J—H4J3109.5
O21D—C2D—O22D111.69 (19)H4J1—C4J—H4J3109.5
O21D—C2D—C1D107.24 (19)H4J2—C4J—H4J3109.5
O22D—C2D—C1D110.94 (18)O22J—C5J—H5J1109.5
O21D—C2D—C3D111.41 (19)O22J—C5J—H5J2109.5
O22D—C2D—C3D106.10 (19)H5J1—C5J—H5J2109.5
C1D—C2D—C3D109.50 (19)O22J—C5J—H5J3109.5
O3D—C3D—C2D109.47 (18)H5J1—C5J—H5J3109.5
O3D—C3D—H3D1109.8H5J2—C5J—H5J3109.5
C2D—C3D—H3D1109.8O5K—P1K—O4K118.43 (11)
O3D—C3D—H3D2109.8O5K—P1K—O1K112.00 (10)
C2D—C3D—H3D2109.8O4K—P1K—O1K106.11 (10)
H3D1—C3D—H3D2108.2O5K—P1K—O3K106.93 (9)
O21D—C4D—H4D1109.5O4K—P1K—O3K111.49 (9)
O21D—C4D—H4D2109.5O1K—P1K—O3K100.46 (10)
H4D1—C4D—H4D2109.5C1K—O1K—P1K113.93 (13)
O21D—C4D—H4D3109.5C2K—O21K—C4K114.34 (18)
H4D1—C4D—H4D3109.5C2K—O22K—C5K114.59 (18)
H4D2—C4D—H4D3109.5C3K—O3K—P1K114.61 (15)
O22D—C5D—H5D1109.5O1K—C1K—C2K109.20 (17)
O22D—C5D—H5D2109.5O1K—C1K—H1K1109.8
H5D1—C5D—H5D2109.5C2K—C1K—H1K1109.8
O22D—C5D—H5D3109.5O1K—C1K—H1K2109.8
H5D1—C5D—H5D3109.5C2K—C1K—H1K2109.8
H5D2—C5D—H5D3109.5H1K1—C1K—H1K2108.3
O4E—P1E—O5E118.35 (11)O21K—C2K—O22K111.13 (19)
O4E—P1E—O1E111.28 (11)O21K—C2K—C1K106.94 (19)
O5E—P1E—O1E106.70 (11)O22K—C2K—C1K111.69 (18)
O4E—P1E—O3E110.07 (10)O21K—C2K—C3K111.79 (19)
O5E—P1E—O3E107.06 (10)O22K—C2K—C3K105.42 (19)
O1E—P1E—O3E102.07 (10)C1K—C2K—C3K109.95 (19)
C1E—O1E—P1E117.21 (13)O3K—C3K—C2K109.07 (18)
C2E—O21E—C4E115.10 (18)O3K—C3K—H3K1109.9
C2E—O22E—C5E115.99 (17)C2K—C3K—H3K1109.9
C3E—O3E—P1E117.23 (15)O3K—C3K—H3K2109.9
O1E—C1E—C2E111.56 (17)C2K—C3K—H3K2109.9
O1E—C1E—H1E1109.3H3K1—C3K—H3K2108.3
C2E—C1E—H1E1109.3O21K—C4K—H4K1109.5
O1E—C1E—H1E2109.3O21K—C4K—H4K2109.5
C2E—C1E—H1E2109.3H4K1—C4K—H4K2109.5
H1E1—C1E—H1E2108.0O21K—C4K—H4K3109.5
O22E—C2E—O21E112.9 (2)H4K1—C4K—H4K3109.5
O22E—C2E—C1E114.19 (17)H4K2—C4K—H4K3109.5
O21E—C2E—C1E103.61 (18)O22K—C5K—H5K1109.5
O22E—C2E—C3E104.68 (19)O22K—C5K—H5K2109.5
O21E—C2E—C3E111.67 (18)H5K1—C5K—H5K2109.5
C1E—C2E—C3E110.0 (2)O22K—C5K—H5K3109.5
O3E—C3E—C2E110.71 (19)H5K1—C5K—H5K3109.5
O3E—C3E—H3E1109.5H5K2—C5K—H5K3109.5
C2E—C3E—H3E1109.5O5L—P1L—O4L118.70 (12)
O3E—C3E—H3E2109.5O5L—P1L—O1L106.23 (10)
C2E—C3E—H3E2109.5O4L—P1L—O1L110.96 (11)
H3E1—C3E—H3E2108.1O5L—P1L—O3L107.78 (10)
O21E—C4E—H4E1109.5O4L—P1L—O3L109.92 (10)
O21E—C4E—H4E2109.5O1L—P1L—O3L101.87 (10)
H4E1—C4E—H4E2109.5C1L—O1L—P1L118.70 (13)
O21E—C4E—H4E3109.5C2L—O21L—C4L114.74 (18)
H4E1—C4E—H4E3109.5C2L—O22L—C5L115.94 (18)
H4E2—C4E—H4E3109.5C3L—O3L—P1L117.21 (15)
O22E—C5E—H5E1109.5O1L—C1L—C2L111.61 (18)
O22E—C5E—H5E2109.5O1L—C1L—H1L1109.3
H5E1—C5E—H5E2109.5C2L—C1L—H1L1109.3
O22E—C5E—H5E3109.5O1L—C1L—H1L2109.3
H5E1—C5E—H5E3109.5C2L—C1L—H1L2109.3
H5E2—C5E—H5E3109.5H1L1—C1L—H1L2108.0
O40E—P10E—O50E118.8 (3)O22L—C2L—O21L113.2 (2)
O40E—P10E—O10E111.4 (3)O22L—C2L—C3L104.62 (19)
O50E—P10E—O10E106.7 (3)O21L—C2L—C3L112.67 (18)
O40E—P10E—O30E110.2 (3)O22L—C2L—C1L115.00 (18)
O50E—P10E—O30E107.0 (3)O21L—C2L—C1L102.42 (18)
O10E—P10E—O30E101.1 (2)C3L—C2L—C1L109.1 (2)
C10E—O10E—P10E116.2 (3)O3L—C3L—C2L110.33 (18)
C20E—O23E—C40E115.1 (4)O3L—C3L—H3L1109.6
C20E—O24E—C50E116.1 (4)C2L—C3L—H3L1109.6
C30E—O30E—P10E116.9 (3)O3L—C3L—H3L2109.6
O10E—C10E—C20E111.8 (3)C2L—C3L—H3L2109.6
O10E—C10E—H10A109.3H3L1—C3L—H3L2108.1
C20E—C10E—H10A109.3O21L—C4L—H4L1109.5
O10E—C10E—H10B109.3O21L—C4L—H4L2109.5
C20E—C10E—H10B109.3H4L1—C4L—H4L2109.5
H10A—C10E—H10B107.9O21L—C4L—H4L3109.5
O24E—C20E—O23E112.6 (3)H4L1—C4L—H4L3109.5
O24E—C20E—C10E114.2 (3)H4L2—C4L—H4L3109.5
O23E—C20E—C10E103.5 (3)O22L—C5L—H5L1109.5
O24E—C20E—C30E104.6 (3)O22L—C5L—H5L2109.5
O23E—C20E—C30E111.5 (3)H5L1—C5L—H5L2109.5
C10E—C20E—C30E110.6 (3)O22L—C5L—H5L3109.5
O30E—C30E—C20E111.5 (3)H5L1—C5L—H5L3109.5
O30E—C30E—H30A109.3H5L2—C5L—H5L3109.5
C20E—C30E—H30A109.3O50L—P10L—O40L118.7 (3)
O30E—C30E—H30B109.3O50L—P10L—O10L106.2 (3)
C20E—C30E—H30B109.3O40L—P10L—O10L111.0 (3)
H30A—C30E—H30B108.0O50L—P10L—O30L108.0 (3)
O23E—C40E—H40A109.5O40L—P10L—O30L109.9 (3)
O23E—C40E—H40B109.5O10L—P10L—O30L101.6 (2)
H40A—C40E—H40B109.5C10L—O10L—P10L119.0 (4)
O23E—C40E—H40C109.5C20L—O23L—C40L114.7 (4)
H40A—C40E—H40C109.5C20L—O24L—C50L116.2 (4)
H40B—C40E—H40C109.5C30L—O30L—P10L116.8 (3)
O24E—C50E—H50A109.5O10L—C10L—C20L112.9 (4)
O24E—C50E—H50B109.5O10L—C10L—H10E109.0
H50A—C50E—H50B109.5C20L—C10L—H10E109.0
O24E—C50E—H50C109.5O10L—C10L—H10F109.0
H50A—C50E—H50C109.5C20L—C10L—H10F109.0
H50B—C50E—H50C109.5H10E—C10L—H10F107.8
O5F—P1F—O4F118.88 (11)O24L—C20L—O23L112.9 (3)
O5F—P1F—O3F107.10 (9)O24L—C20L—C30L104.6 (3)
O4F—P1F—O3F109.86 (9)O23L—C20L—C30L112.3 (3)
O5F—P1F—O1F106.64 (10)O24L—C20L—C10L115.6 (3)
O4F—P1F—O1F110.75 (10)O23L—C20L—C10L102.1 (3)
O3F—P1F—O1F102.26 (10)C30L—C20L—C10L109.6 (3)
C1F—O1F—P1F117.59 (13)O30L—C30L—C20L110.6 (3)
C2F—O21F—C4F114.43 (17)O30L—C30L—H30E109.5
C2F—O22F—C5F116.31 (18)C20L—C30L—H30E109.5
C3F—O3F—P1F115.93 (15)O30L—C30L—H30F109.5
O1F—C1F—C2F111.94 (18)C20L—C30L—H30F109.5
O1F—C1F—H1F1109.2H30E—C30L—H30F108.1
C2F—C1F—H1F1109.2O23L—C40L—H40G109.5
O1F—C1F—H1F2109.2O23L—C40L—H40H109.5
C2F—C1F—H1F2109.2H40G—C40L—H40H109.5
H1F1—C1F—H1F2107.9O23L—C40L—H40I109.5
O22F—C2F—O21F112.75 (19)H40G—C40L—H40I109.5
O22F—C2F—C3F105.80 (19)H40H—C40L—H40I109.5
O21F—C2F—C3F112.2 (2)O24L—C50L—H50G109.5
O22F—C2F—C1F113.92 (18)O24L—C50L—H50H109.5
O21F—C2F—C1F102.73 (18)H50G—C50L—H50H109.5
C3F—C2F—C1F109.6 (2)O24L—C50L—H50I109.5
O3F—C3F—C2F110.75 (19)H50G—C50L—H50I109.5
O3F—C3F—H3F1109.5H50H—C50L—H50I109.5
C2F—C3F—H3F1109.5H1N—N1—H2N110.2
O3F—C3F—H3F2109.5H1N—N1—H3N106.7
C2F—C3F—H3F2109.5H2N—N1—H3N114.3
H3F1—C3F—H3F2108.1H1N—N1—H4N106.2
O21F—C4F—H4F1109.5H2N—N1—H4N114.7
O21F—C4F—H4F2109.5H3N—N1—H4N103.9
H4F1—C4F—H4F2109.5H5N—N2—H6N104.4
O21F—C4F—H4F3109.5H5N—N2—H7N103.0
H4F1—C4F—H4F3109.5H6N—N2—H7N112.0
H4F2—C4F—H4F3109.5H5N—N2—H8N118.7
O22F—C5F—H5F1109.5H6N—N2—H8N105.7
O22F—C5F—H5F2109.5H7N—N2—H8N112.8
H5F1—C5F—H5F2109.5H9N—N3—H10N107.3
O22F—C5F—H5F3109.5H9N—N3—H11N108.1
H5F1—C5F—H5F3109.5H10N—N3—H11N104.2
H5F2—C5F—H5F3109.5H9N—N3—H12N112.9
O4G—P1G—O5G118.47 (10)H10N—N3—H12N114.7
O4G—P1G—O1G106.67 (10)H11N—N3—H12N109.0
O5G—P1G—O1G112.01 (10)H13N—N4—H14N112.2
O4G—P1G—O3G111.67 (10)H13N—N4—H15N105.4
O5G—P1G—O3G106.32 (9)H14N—N4—H15N105.4
O1G—P1G—O3G100.24 (9)H13N—N4—H16N112.2
C1G—O1G—P1G114.11 (13)H14N—N4—H16N103.5
C2G—O21G—C4G114.05 (18)H15N—N4—H16N118.1
C2G—O22G—C5G114.01 (17)H17N—N5—H18N108.6
C3G—O3G—P1G115.05 (14)H17N—N5—H19N109.9
O1G—C1G—C2G110.13 (18)H18N—N5—H19N110.1
O1G—C1G—H1G1109.6H17N—N5—H20N109.1
C2G—C1G—H1G1109.6H18N—N5—H20N107.0
O1G—C1G—H1G2109.6H19N—N5—H20N112.1
C2G—C1G—H1G2109.6H21N—N6—H22N104.5
H1G1—C1G—H1G2108.1H21N—N6—H23N102.0
O21G—C2G—O22G111.26 (18)H22N—N6—H23N116.5
O21G—C2G—C3G111.88 (19)H21N—N6—H24N118.7
O22G—C2G—C3G106.00 (18)H22N—N6—H24N110.3
O21G—C2G—C1G107.50 (18)H23N—N6—H24N105.2
O22G—C2G—C1G110.58 (18)H25N—N7—H26N105.9
C3G—C2G—C1G109.66 (19)H25N—N7—H27N114.4
O3G—C3G—C2G109.17 (18)H26N—N7—H27N108.9
O3G—C3G—H3G1109.8H25N—N7—H28N108.4
C2G—C3G—H3G1109.8H26N—N7—H28N112.9
O3G—C3G—H3G2109.8H27N—N7—H28N106.6
C2G—C3G—H3G2109.8H29N—N8—H30N112.7
H3G1—C3G—H3G2108.3H29N—N8—H31N106.9
O21G—C4G—H4G1109.5H30N—N8—H31N111.5
O21G—C4G—H4G2109.5H29N—N8—H32N107.8
H4G1—C4G—H4G2109.5H30N—N8—H32N109.3
O21G—C4G—H4G3109.5H31N—N8—H32N108.4
H4G1—C4G—H4G3109.5H33N—N9—H34N110.4
H4G2—C4G—H4G3109.5H33N—N9—H35N109.8
O22G—C5G—H5G1109.5H34N—N9—H35N104.3
O22G—C5G—H5G2109.5H33N—N9—H36N106.3
H5G1—C5G—H5G2109.5H34N—N9—H36N113.5
O22G—C5G—H5G3109.5H35N—N9—H36N112.7
H5G1—C5G—H5G3109.5H37N—N10—H38N104.0
H5G2—C5G—H5G3109.5H37N—N10—H39N114.6
O4H—P1H—O5H118.42 (11)H38N—N10—H39N112.6
O4H—P1H—O3H111.61 (9)H37N—N10—H40N105.7
O5H—P1H—O3H106.45 (10)H38N—N10—H40N111.9
O4H—P1H—O1H107.02 (10)H39N—N10—H40N107.8
O5H—P1H—O1H111.72 (10)H41N—N11—H42N111.4
O3H—P1H—O1H100.15 (10)H41N—N11—H43N108.2
C1H—O1H—P1H114.09 (14)H42N—N11—H43N108.3
C2H—O21H—C4H114.33 (17)H41N—N11—H44N106.2
C2H—O22H—C5H113.58 (17)H42N—N11—H44N109.5
C3H—O3H—P1H115.20 (14)H43N—N11—H44N113.3
O1H—C1H—C2H111.00 (17)H45N—N12—H46N106.2
O1H—C1H—H1H1109.4H45N—N12—H47N113.3
C2H—C1H—H1H1109.4H46N—N12—H47N115.0
O1H—C1H—H1H2109.4H45N—N12—H48N102.3
C2H—C1H—H1H2109.4H46N—N12—H48N111.7
H1H1—C1H—H1H2108.0H47N—N12—H48N107.6
O5A—P1A—O1A—C1A77.31 (16)C5G—O22G—C2G—O21G55.5 (2)
O4A—P1A—O1A—C1A151.74 (13)C5G—O22G—C2G—C3G177.37 (16)
O3A—P1A—O1A—C1A35.62 (15)C5G—O22G—C2G—C1G63.8 (2)
O5A—P1A—O3A—C3A151.84 (16)O1G—C1G—C2G—O21G89.8 (2)
O4A—P1A—O3A—C3A77.65 (18)O1G—C1G—C2G—O22G148.55 (18)
O1A—P1A—O3A—C3A34.51 (16)O1G—C1G—C2G—C3G32.0 (2)
P1A—O1A—C1A—C2A72.02 (19)P1G—O3G—C3G—C2G71.4 (2)
C4A—O21A—C2A—O22A64.1 (2)O21G—C2G—C3G—O3G152.83 (17)
C4A—O21A—C2A—C1A173.60 (18)O22G—C2G—C3G—O3G85.7 (2)
C4A—O21A—C2A—C3A53.4 (2)C1G—C2G—C3G—O3G33.6 (2)
C5A—O22A—C2A—O21A59.4 (2)O4H—P1H—O1H—C1H150.76 (14)
C5A—O22A—C2A—C1A61.0 (2)O5H—P1H—O1H—C1H78.12 (16)
C5A—O22A—C2A—C3A179.46 (18)O3H—P1H—O1H—C1H34.27 (15)
O1A—C1A—C2A—O21A89.0 (2)O4H—P1H—O3H—C3H78.67 (18)
O1A—C1A—C2A—O22A148.37 (18)O5H—P1H—O3H—C3H150.74 (16)
O1A—C1A—C2A—C3A32.4 (2)O1H—P1H—O3H—C3H34.33 (17)
P1A—O3A—C3A—C2A72.0 (2)P1H—O1H—C1H—C2H71.0 (2)
O21A—C2A—C3A—O3A153.16 (17)C4H—O21H—C2H—O22H59.0 (2)
O22A—C2A—C3A—O3A85.6 (2)C4H—O21H—C2H—C1H179.65 (18)
C1A—C2A—C3A—O3A34.0 (2)C4H—O21H—C2H—C3H59.1 (2)
O5B—P1B—O1B—C1B74.97 (16)C5H—O22H—C2H—O21H55.2 (2)
O4B—P1B—O1B—C1B154.17 (14)C5H—O22H—C2H—C1H64.8 (2)
O3B—P1B—O1B—C1B37.61 (16)C5H—O22H—C2H—C3H176.92 (19)
O5B—P1B—O3B—C3B148.13 (17)O1H—C1H—C2H—O21H89.6 (2)
O4B—P1B—O3B—C3B81.78 (19)O1H—C1H—C2H—O22H148.30 (18)
O1B—P1B—O3B—C3B31.00 (18)O1H—C1H—C2H—C3H32.4 (2)
P1B—O1B—C1B—C2B71.2 (2)P1H—O3H—C3H—C2H71.2 (2)
C4B—O21B—C2B—O22B59.5 (3)O21H—C2H—C3H—O3H152.78 (17)
C4B—O21B—C2B—C3B58.9 (3)O22H—C2H—C3H—O3H85.8 (2)
C4B—O21B—C2B—C1B178.66 (19)C1H—C2H—C3H—O3H33.1 (2)
C5B—O22B—C2B—O21B56.7 (3)O5I—P1I—O1I—C1I163.79 (15)
C5B—O22B—C2B—C3B178.29 (18)O4I—P1I—O1I—C1I66.01 (17)
C5B—O22B—C2B—C1B62.7 (3)O3I—P1I—O1I—C1I50.87 (17)
O1B—C1B—C2B—O21B90.9 (2)O5I—P1I—O3I—C3I164.12 (19)
O1B—C1B—C2B—O22B146.8 (2)O4I—P1I—O3I—C3I64.9 (2)
O1B—C1B—C2B—C3B30.1 (3)O1I—P1I—O3I—C3I51.9 (2)
P1B—O3B—C3B—C2B69.9 (2)P1I—O1I—C1I—C2I57.5 (2)
O21B—C2B—C3B—O3B153.47 (17)C5I—O22I—C2I—O21I55.9 (2)
O22B—C2B—C3B—O3B84.7 (2)C5I—O22I—C2I—C1I62.0 (3)
C1B—C2B—C3B—O3B35.3 (3)C5I—O22I—C2I—C3I177.65 (17)
O4C—P1C—O1C—C1C154.18 (13)C4I—O21I—C2I—O22I53.8 (3)
O5C—P1C—O1C—C1C74.83 (15)C4I—O21I—C2I—C1I177.8 (2)
O3C—P1C—O1C—C1C37.91 (14)C4I—O21I—C2I—C3I63.9 (3)
O4C—P1C—O3C—C3C80.53 (18)O1I—C1I—C2I—O22I60.2 (3)
O5C—P1C—O3C—C3C149.03 (16)O1I—C1I—C2I—O21I176.48 (19)
O1C—P1C—O3C—C3C31.75 (16)O1I—C1I—C2I—C3I57.1 (2)
P1C—O1C—C1C—C2C72.06 (19)P1I—O3I—C3I—C2I59.2 (2)
C4C—O21C—C2C—O22C59.6 (2)O22I—C2I—C3I—O3I65.3 (2)
C4C—O21C—C2C—C3C58.4 (2)O21I—C2I—C3I—O3I172.03 (19)
C4C—O21C—C2C—C1C178.29 (18)C1I—C2I—C3I—O3I57.9 (3)
C5C—O22C—C2C—O21C57.3 (2)O50I—P10I—O10I—C10I79.4 (7)
C5C—O22C—C2C—C3C178.44 (19)O40I—P10I—O10I—C10I149.6 (7)
C5C—O22C—C2C—C1C62.6 (2)O30I—P10I—O10I—C10I33.0 (7)
O1C—C1C—C2C—O21C89.8 (2)O50I—P10I—O30I—C30I144.2 (7)
O1C—C1C—C2C—O22C147.47 (18)O40I—P10I—O30I—C30I84.4 (8)
O1C—C1C—C2C—C3C30.9 (2)O10I—P10I—O30I—C30I32.2 (7)
P1C—O3C—C3C—C2C70.8 (2)P10I—O10I—C10I—C20I65.9 (6)
O21C—C2C—C3C—O3C153.58 (17)C50I—O24I—C20I—O23I60.1 (12)
O22C—C2C—C3C—O3C84.7 (2)C50I—O24I—C20I—C10I57.2 (11)
C1C—C2C—C3C—O3C35.2 (2)C50I—O24I—C20I—C30I178.8 (11)
O5D—P1D—O1D—C1D75.85 (15)C40I—O23I—C20I—O24I59.9 (14)
O4D—P1D—O1D—C1D153.15 (13)C40I—O23I—C20I—C10I176.6 (14)
O3D—P1D—O1D—C1D37.26 (15)C40I—O23I—C20I—C30I57.3 (14)
O5D—P1D—O3D—C3D149.19 (17)O10I—C10I—C20I—O24I147.3 (7)
O4D—P1D—O3D—C3D80.38 (19)O10I—C10I—C20I—O23I90.3 (7)
O1D—P1D—O3D—C3D32.35 (18)O10I—C10I—C20I—C30I29.2 (7)
P1D—O1D—C1D—C2D72.4 (2)P10I—O30I—C30I—C20I66.8 (7)
C4D—O21D—C2D—O22D65.0 (3)O24I—C20I—C30I—O30I91.8 (7)
C4D—O21D—C2D—C1D173.27 (18)O23I—C20I—C30I—O30I146.6 (7)
C4D—O21D—C2D—C3D53.5 (2)C10I—C20I—C30I—O30I31.9 (7)
C5D—O22D—C2D—O21D59.5 (2)O5J—P1J—O1J—C1J78.25 (16)
C5D—O22D—C2D—C1D60.0 (2)O4J—P1J—O1J—C1J151.07 (14)
C5D—O22D—C2D—C3D178.87 (17)O3J—P1J—O1J—C1J34.84 (15)
O1D—C1D—C2D—O21D89.7 (2)O5J—P1J—O3J—C3J151.44 (16)
O1D—C1D—C2D—O22D148.10 (19)O4J—P1J—O3J—C3J77.82 (18)
O1D—C1D—C2D—C3D31.3 (2)O1J—P1J—O3J—C3J34.54 (16)
P1D—O3D—C3D—C2D71.3 (2)P1J—O1J—C1J—C2J71.3 (2)
O21D—C2D—C3D—O3D153.51 (17)C4J—O21J—C2J—O22J67.3 (2)
O22D—C2D—C3D—O3D84.7 (2)C4J—O21J—C2J—C1J170.78 (18)
C1D—C2D—C3D—O3D35.1 (2)C4J—O21J—C2J—C3J50.7 (3)
O4E—P1E—O1E—C1E67.24 (18)C5J—O22J—C2J—O21J59.6 (2)
O5E—P1E—O1E—C1E162.30 (15)C5J—O22J—C2J—C1J59.5 (3)
O3E—P1E—O1E—C1E50.14 (16)C5J—O22J—C2J—C3J178.51 (18)
O4E—P1E—O3E—C3E67.1 (2)O1J—C1J—C2J—O21J89.0 (2)
O5E—P1E—O3E—C3E163.08 (18)O1J—C1J—C2J—O22J149.31 (19)
O1E—P1E—O3E—C3E51.19 (18)O1J—C1J—C2J—C3J32.7 (2)
P1E—O1E—C1E—C2E56.9 (2)P1J—O3J—C3J—C2J71.1 (2)
C5E—O22E—C2E—O21E54.4 (2)O21J—C2J—C3J—O3J151.54 (18)
C5E—O22E—C2E—C1E63.7 (3)O22J—C2J—C3J—O3J87.2 (2)
C5E—O22E—C2E—C3E176.04 (18)C1J—C2J—C3J—O3J33.1 (2)
C4E—O21E—C2E—O22E55.7 (3)O5K—P1K—O1K—C1K77.44 (15)
C4E—O21E—C2E—C1E179.73 (19)O4K—P1K—O1K—C1K151.94 (13)
C4E—O21E—C2E—C3E62.0 (3)O3K—P1K—O1K—C1K35.76 (15)
O1E—C1E—C2E—O22E61.2 (3)O5K—P1K—O3K—C3K151.33 (17)
O1E—C1E—C2E—O21E175.60 (17)O4K—P1K—O3K—C3K77.78 (19)
O1E—C1E—C2E—C3E56.1 (2)O1K—P1K—O3K—C3K34.30 (18)
P1E—O3E—C3E—C2E58.3 (2)P1K—O1K—C1K—C2K72.04 (19)
O22E—C2E—C3E—O3E66.5 (2)C4K—O21K—C2K—O22K66.9 (3)
O21E—C2E—C3E—O3E171.05 (19)C4K—O21K—C2K—C1K170.95 (18)
C1E—C2E—C3E—O3E56.6 (2)C4K—O21K—C2K—C3K50.6 (2)
O40E—P10E—O10E—C10E148.8 (9)C5K—O22K—C2K—O21K59.7 (2)
O50E—P10E—O10E—C10E80.0 (9)C5K—O22K—C2K—C1K59.6 (3)
O30E—P10E—O10E—C10E31.6 (9)C5K—O22K—C2K—C3K179.00 (17)
O40E—P10E—O30E—C30E84.8 (9)O1K—C1K—C2K—O21K88.7 (2)
O50E—P10E—O30E—C30E144.7 (9)O1K—C1K—C2K—O22K149.57 (19)
O10E—P10E—O30E—C30E33.2 (9)O1K—C1K—C2K—C3K32.9 (2)
P10E—O10E—C10E—C20E66.7 (7)P1K—O3K—C3K—C2K71.4 (2)
C50E—O24E—C20E—O23E55.0 (18)O21K—C2K—C3K—O3K151.78 (17)
C50E—O24E—C20E—C10E62.7 (18)O22K—C2K—C3K—O3K87.4 (2)
C50E—O24E—C20E—C30E176.2 (17)C1K—C2K—C3K—O3K33.2 (2)
C40E—O23E—C20E—O24E60.9 (19)O5L—P1L—O1L—C1L162.08 (16)
C40E—O23E—C20E—C10E175.2 (18)O4L—P1L—O1L—C1L67.60 (18)
C40E—O23E—C20E—C30E56.3 (18)O3L—P1L—O1L—C1L49.36 (17)
O10E—C10E—C20E—O24E150.0 (9)O5L—P1L—O3L—C3L162.19 (16)
O10E—C10E—C20E—O23E87.3 (9)O4L—P1L—O3L—C3L67.1 (2)
O10E—C10E—C20E—C30E32.2 (8)O1L—P1L—O3L—C3L50.64 (18)
P10E—O30E—C30E—C20E66.0 (7)P1L—O1L—C1L—C2L56.2 (2)
O24E—C20E—C30E—O30E94.3 (8)C5L—O22L—C2L—O21L55.0 (2)
O23E—C20E—C30E—O30E143.8 (8)C5L—O22L—C2L—C3L178.07 (18)
C10E—C20E—C30E—O30E29.2 (8)C5L—O22L—C2L—C1L62.3 (3)
O5F—P1F—O1F—C1F162.89 (14)C4L—O21L—C2L—O22L54.5 (3)
O4F—P1F—O1F—C1F66.40 (16)C4L—O21L—C2L—C3L63.9 (3)
O3F—P1F—O1F—C1F50.62 (16)C4L—O21L—C2L—C1L178.99 (19)
O5F—P1F—O3F—C3F163.99 (17)O1L—C1L—C2L—O22L61.2 (3)
O4F—P1F—O3F—C3F65.6 (2)O1L—C1L—C2L—O21L175.55 (17)
O1F—P1F—O3F—C3F52.06 (18)O1L—C1L—C2L—C3L56.0 (2)
P1F—O1F—C1F—C2F56.0 (2)P1L—O3L—C3L—C2L59.4 (2)
C5F—O22F—C2F—O21F54.5 (2)O22L—C2L—C3L—O3L66.3 (2)
C5F—O22F—C2F—C3F177.42 (17)O21L—C2L—C3L—O3L170.31 (18)
C5F—O22F—C2F—C1F62.1 (2)C1L—C2L—C3L—O3L57.3 (2)
C4F—O21F—C2F—O22F56.7 (3)O50L—P10L—O10L—C10L162.1 (7)
C4F—O21F—C2F—C3F62.7 (3)O40L—P10L—O10L—C10L67.5 (8)
C4F—O21F—C2F—C1F179.70 (18)O30L—P10L—O10L—C10L49.3 (7)
O1F—C1F—C2F—O22F62.9 (3)O50L—P10L—O30L—C30L163.7 (7)
O1F—C1F—C2F—O21F174.81 (18)O40L—P10L—O30L—C30L65.4 (8)
O1F—C1F—C2F—C3F55.4 (2)O10L—P10L—O30L—C30L52.3 (7)
P1F—O3F—C3F—C2F59.9 (2)P10L—O10L—C10L—C20L54.0 (8)
O22F—C2F—C3F—O3F66.2 (2)C50L—O24L—C20L—O23L51 (2)
O21F—C2F—C3F—O3F170.50 (17)C50L—O24L—C20L—C30L174 (2)
C1F—C2F—C3F—O3F57.1 (2)C50L—O24L—C20L—C10L66 (2)
O4G—P1G—O1G—C1G151.85 (13)C40L—O23L—C20L—O24L97 (2)
O5G—P1G—O1G—C1G77.02 (15)C40L—O23L—C20L—C30L21 (2)
O3G—P1G—O1G—C1G35.38 (15)C40L—O23L—C20L—C10L138 (2)
O4G—P1G—O3G—C3G78.68 (19)O10L—C10L—C20L—O24L65.1 (8)
O5G—P1G—O3G—C3G150.72 (17)O10L—C10L—C20L—O23L171.9 (7)
O1G—P1G—O3G—C3G33.99 (18)O10L—C10L—C20L—C30L52.8 (7)
P1G—O1G—C1G—C2G71.35 (19)P10L—O30L—C30L—C20L60.3 (7)
C4G—O21G—C2G—O22G59.4 (3)O24L—C20L—C30L—O30L69.1 (7)
C4G—O21G—C2G—C3G58.9 (2)O23L—C20L—C30L—O30L168.1 (6)
C4G—O21G—C2G—C1G179.37 (18)C10L—C20L—C30L—O30L55.5 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O5Fi0.901.882.779 (3)176
N1—H2N···O4Eii0.902.012.873 (3)161
N1—H2N···O40Eii0.901.872.711 (18)154
N1—H3N···O5B0.901.992.831 (2)156
N1—H4N···O4Fiii0.901.992.875 (3)168
N2—H5N···O5Cii0.901.942.815 (3)165
N2—H6N···O5A0.901.902.801 (3)174
N2—H7N···O4B0.901.902.772 (3)161
N2—H8N···O4Eii0.901.962.851 (3)169
N2—H8N···O40Eii0.901.842.73 (2)171
N3—H9N···O4B0.901.992.859 (3)162
N3—H10N···O5D0.901.962.828 (2)160
N3—H11N···O5Di0.901.902.799 (3)174
N3—H12N···O4Cii0.901.882.756 (3)165
N4—H13N···O4Cii0.901.972.855 (3)166
N4—H14N···O5Aii0.901.952.821 (3)164
N4—H15N···O5C0.901.922.812 (3)171
N4—H16N···O4D0.901.892.774 (3)166
N5—H17N···O5Bi0.901.912.801 (3)172
N5—H18N···O5F0.901.912.763 (2)158
N5—H19N···O4Aii0.901.882.758 (3)164
N5—H20N···O4D0.901.952.845 (3)170
N6—H21N···O5Eiv0.901.902.765 (3)161
N6—H21N···O50Eiv0.902.022.908 (12)169
N6—H22N···O4F0.901.932.812 (3)165
N6—H23N···O5E0.901.862.757 (3)173
N6—H23N···O50E0.902.163.061 (19)176
N6—H24N···O4Aii0.901.972.861 (3)172
N7—H25N···O5Gv0.901.962.824 (3)160
N7—H26N···O5G0.901.892.785 (3)175
N7—H27N···O4Kvi0.901.982.865 (3)167
N7—H28N···O4Lvii0.901.932.803 (3)164
N7—H28N···O40Lvii0.902.243.110 (19)162
N8—H29N···O4H0.901.972.867 (3)171
N8—H30N···O4Kvi0.901.882.765 (3)165
N8—H31N···O5Jviii0.901.912.806 (3)178
N8—H32N···O5Lvii0.901.952.761 (3)150
N8—H32N···O50Lvii0.902.192.974 (15)145
N9—H33N···O4Ivi0.902.022.892 (3)162
N9—H33N···O40Ivi0.901.842.713 (16)162
N9—H34N···O5I0.901.852.753 (3)175
N9—H34N···O50I0.902.193.088 (14)173
N9—H35N···O5Kvi0.901.952.810 (2)159
N9—H36N···O4H0.901.912.781 (3)163
N10—H37N···O4J0.901.972.871 (3)176
N10—H38N···O5Hviii0.901.892.787 (3)178
N10—H39N···O4Ivi0.901.952.834 (3)165
N10—H39N···O40Ivi0.901.732.601 (13)163
N10—H40N···O5H0.902.022.825 (3)148
N11—H41N···O5Ivi0.901.932.769 (3)155
N11—H41N···O50Ivi0.901.972.852 (10)167
N11—H42N···O4Gvi0.901.982.862 (3)166
N11—H43N···O4J0.901.902.773 (3)163
N11—H44N···O5K0.901.912.809 (3)175
N12—H45N···O4L0.901.982.869 (3)168
N12—H45N···O40L0.902.123.01 (3)170
N12—H46N···O5Lix0.901.892.790 (3)176
N12—H46N···O50Lix0.901.722.62 (2)176
N12—H47N···O4Gvi0.901.902.780 (3)164
N12—H48N···O5J0.902.022.813 (3)147
C1B—H1B1···O21K0.992.433.402 (3)166
C1C—H1C2···O21J0.992.463.434 (3)170
C3C—H3C2···O4B0.992.583.532 (3)162
C3D—H3D1···O40Ex0.992.423.359 (16)159
C4D—H4D3···O4Ex0.982.603.513 (3)156
C4D—H4D3···O40Ex0.982.563.451 (19)151
C4E—H4E2···O4D0.982.503.295 (3)139
C5E—H5E1···O1F0.982.613.507 (3)152
C4F—H4F1···O4Axi0.982.593.288 (3)128
C5F—H5F2···O1Ex0.982.543.433 (3)151
C5H—H5H2···O1Ixii0.982.543.135 (3)119
C1I—H1I1···O21D0.992.573.553 (3)170
C3I—H3I2···O4J0.992.583.564 (3)171
C4I—H4I2···O4J0.982.533.311 (3)136
C10I—H10D···O21D0.992.613.574 (9)164
C30I—H30D···O4J0.992.593.534 (9)160
C1J—H1J1···O21C0.992.503.477 (3)171
C3J—H3J1···O40Ixii0.992.583.547 (13)164
C1K—H1K2···O21B0.992.533.508 (3)171
C1L—H1L2···O21A0.992.603.582 (3)171
C3L—H3L1···O4Kxii0.992.603.578 (3)169
C30L—H30E···O4Kxii0.992.443.389 (17)161
C4L—H4L3···O4Kxii0.982.553.313 (3)135
C50L—H50G···O1Gxiii0.982.493.41 (3)155
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x, y1, z; (iv) x+1, y+2, z+1; (v) x+2, y+2, z; (vi) x+2, y+1, z; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) x+1, y, z; (x) x+1, y, z; (xi) x+1, y+1, z; (xii) x1, y, z; (xiii) x1, y1, z.

Experimental details

(HTP_sl8-350)(RTP_new)(MTP_sl8mt)(LTP_sl8lt)
Crystal data
Chemical formulaC5H10O6P·H4NC5H10O6P·H4NC5H10O6P·H4NC5H10O6P·H4N
Mr215.14215.14215.14215.14
Crystal system, space groupMonoclinic, P21/aTriclinic, P1Monoclinic, P21/aTriclinic, P1
Temperature (K)350290205100
a, b, c (Å)11.910 (5), 19.682 (8), 25.516 (9)11.873 (4), 19.569 (6), 14.218 (5)11.390 (4), 6.862 (2), 12.216 (5)11.336 (3), 20.486 (5), 25.369 (6)
α, β, γ (°)90, 93.74 (3), 90116.88 (3), 93.62 (3), 90.15 (3)90, 97.86 (3), 90105.60 (3), 97.50 (3), 90.17 (3)
V3)5969 (4)2938.8 (18)945.8 (6)5621 (3)
Z2412424
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.280.280.290.30
Crystal size (mm)0.40 × 0.23 × 0.100.45 × 0.16 × 0.060.45 × 0.16 × 0.060.45 × 0.16 × 0.06
Data collection
DiffractometerXcalibur R kappa-geometry
diffractometer with a Ruby CCD camera
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
Xcalibur PX kappa-geometry
diffractometer with an Onyx CCD camera
Absorption correctionMulti-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
Multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
Multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
Multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
Tmin, Tmax0.458, 1.0000.968, 1.0000.851, 1.0000.827, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
81666, 10503, 3275 35436, 16643, 9154 14164, 4906, 3051 77940, 32235, 14062
Rint0.1900.0260.0260.038
(sin θ/λ)max1)0.5950.7030.8760.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.077, 0.177, 1.00 0.040, 0.093, 1.00 0.040, 0.114, 1.01 0.041, 0.079, 1.00
No. of reflections1050316643490632235
No. of parameters8448331921568
No. of restraints105026430438
H-atom treatmentH-atom parameters constrainedH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.34, 0.200.32, 0.280.40, 0.260.53, 0.37

Computer programs: CrysAlis PRO, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012, 15:38:31), CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009, 17:40:42), CrysAlis RED, SHELXS97 (Sheldrick, 2008), SHELXL2013 (Sheldrick, 2013).

Hydrogen-bond geometry (Å, º) for (HTP_sl8-350) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O5B0.901.932.801 (5)163.3
N1—H2N···O4Ai0.902.022.908 (8)169.3
N1—H2N···O40Ai0.901.792.685 (18)172.9
N1—H3N···O4F0.901.902.786 (7)167.0
N1—H3N···O40F0.901.962.846 (9)166.8
N1—H4N···O1Fi0.902.593.211 (8)126.4
N1—H4N···O5Fi0.902.072.961 (11)169.1
N1—H4N···O50Fi0.901.842.725 (13)165.6
N2—H5N···O4Aii0.901.952.845 (7)174.6
N2—H5N···O40Aii0.901.742.622 (15)166.8
N2—H6N···O5Fi0.901.882.767 (7)168.3
N2—H6N···O50Fi0.901.892.756 (9)161.2
N2—H7N···O4E0.901.912.805 (10)173.4
N2—H7N···O40E0.902.022.909 (14)167.8
N2—H8N···O1B0.902.553.191 (6)128.6
N2—H8N···O5B0.902.042.923 (6)165.6
N3—H9N···O4F0.901.832.717 (9)167.8
N3—H9N···O40F0.902.173.065 (12)174.3
N3—H10N···O4B0.901.942.812 (5)161.5
N3—H11N···O5D0.901.922.801 (7)167.8
N3—H11N···O50D0.901.932.786 (7)157.3
N3—H12N···O5A0.901.872.741 (10)162.0
N3—H12N···O50A0.902.243.12 (2)167.4
N4—H13N···O5A0.901.862.748 (7)167.3
N4—H13N···O50A0.901.992.885 (14)174.7
N4—H14N···O4C0.901.922.822 (6)176.8
N4—H15N···O4Eiii0.901.802.682 (8)167.6
N4—H15N···O40Eiii0.902.062.954 (12)170.2
N4—H16N···O1D0.902.453.082 (7)128.0
N4—H16N···O5D0.902.153.011 (9)160.7
N4—H16N···O50D0.901.842.677 (10)154.3
N5—H17N···O4B0.901.922.797 (6)163.8
N5—H18N···O4D0.901.962.839 (8)165.4
N5—H18N···O40D0.901.892.760 (8)160.8
N5—H19N···O5E0.902.032.900 (10)163.7
N5—H19N···O50E0.901.802.640 (15)154.6
N5—H20N···O5Civ0.901.892.786 (6)171.7
N6—H21N···O4Div0.901.772.667 (9)171.6
N6—H21N···O40Div0.902.052.947 (10)175.2
N6—H22N···O4Cii0.901.902.784 (5)169.2
N6—H23N···O5E0.901.972.842 (8)163.6
N6—H23N···O50E0.901.802.638 (11)153.5
N6—H24N···O5Civ0.901.922.815 (6)171.4
C50D—H50D···O10Eiii0.962.613.424 (15)143.2
C5F—H5F1···O3Fv0.962.613.391 (13)138.9
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+1, y, z; (iii) x1, y, z; (iv) x+1/2, y+3/2, z; (v) x1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) for (RTP_new) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O5B0.901.842.728 (2)168
N1—H1N···O50B0.902.002.899 (7)173
N1—H2N···O4Fi0.901.902.804 (2)176
N1—H3N···O5Fii0.901.942.826 (2)167
N1—H4N···O4Eiii0.901.882.771 (2)173
N2—H5N···O4B0.901.942.832 (3)172
N2—H5N···O40B0.901.732.627 (8)173
N2—H6N···O3A0.902.513.123 (2)126
N2—H6N···O5A0.902.012.890 (2)164
N2—H7N···O4Eiii0.901.912.8045 (18)175
N2—H8N···O5Ciii0.901.852.740 (2)170
N2—H8N···O50Ciii0.902.012.900 (11)173
N3—H9N···O4B0.902.002.898 (3)173
N3—H9N···O40B0.901.852.740 (10)169
N3—H10N···O5D0.901.892.7747 (17)168
N3—H11N···O1Dii0.902.603.1736 (19)122
N3—H11N···O5Dii0.902.022.908 (2)171
N3—H12N···O4Ciii0.901.942.821 (3)164
N3—H12N···O40Ciii0.901.752.633 (12)166
N4—H13N···O4D0.901.922.8027 (19)167
N4—H14N···O5C0.901.912.805 (3)170
N4—H14N···O50C0.902.133.035 (18)178
N4—H15N···O5Aiii0.901.922.789 (2)162
N4—H16N···O4Ciii0.902.012.885 (3)165
N4—H16N···O40Ciii0.901.892.763 (17)163
N5—H17N···O5F0.901.902.7818 (18)166
N5—H18N···O4D0.901.932.810 (2)165
N5—H19N···O5Bii0.901.852.745 (3)170
N5—H19N···O50Bii0.902.133.029 (10)177
N5—H20N···O4Aiii0.901.952.815 (2)162
N6—H21N···O4F0.901.892.7745 (19)168
N6—H22N···O5E0.901.922.811 (2)168
N6—H23N···O4Aiii0.901.902.7972 (18)171
N6—H24N···O5Eiv0.901.892.777 (2)168
C4B—H4B3···O4Cv0.962.513.303 (5)140
Symmetry codes: (i) x, y1, z; (ii) x+2, y+1, z+1; (iii) x+1, y+1, z+1; (iv) x+1, y+2, z+1; (v) x+1, y, z.
Hydrogen-bond geometry (Å, º) for (MTP_sl8mt) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O40.94 (2)1.82 (2)2.739 (2)163 (2)
N1—H1N···O400.94 (2)2.06 (2)2.974 (5)164 (2)
N1—H2N···O5i0.90 (2)1.95 (2)2.845 (2)176 (2)
N1—H2N···O50i0.90 (2)1.77 (2)2.652 (5)169 (2)
N1—H3N···O5ii0.93 (2)1.96 (2)2.8428 (17)157 (2)
N1—H3N···O50ii0.93 (2)1.89 (2)2.718 (4)148 (2)
N1—H4N···O4iii0.90 (2)1.97 (2)2.845 (2)167 (2)
N1—H4N···O40iii0.90 (2)2.09 (2)2.963 (6)166 (2)
C40—H40C···O40iv0.972.473.146 (9)127
Symmetry codes: (i) x1/2, y+3/2, z; (ii) x+1/2, y1/2, z+1; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) for (LTP_sl8lt) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O5Fi0.901.882.779 (3)175.6
N1—H2N···O4Eii0.902.012.873 (3)160.5
N1—H2N···O40Eii0.901.872.711 (18)153.7
N1—H3N···O5B0.901.992.831 (2)156.1
N1—H4N···O4Fiii0.901.992.875 (3)168.0
N2—H5N···O5Cii0.901.942.815 (3)164.5
N2—H6N···O5A0.901.902.801 (3)174.3
N2—H7N···O4B0.901.902.772 (3)160.7
N2—H8N···O4Eii0.901.962.851 (3)169.2
N2—H8N···O40Eii0.901.842.73 (2)170.8
N3—H9N···O4B0.901.992.859 (3)162.2
N3—H10N···O5D0.901.962.828 (2)160.3
N3—H11N···O5Di0.901.902.799 (3)173.6
N3—H12N···O4Cii0.901.882.756 (3)164.9
N4—H13N···O4Cii0.901.972.855 (3)165.7
N4—H14N···O5Aii0.901.952.821 (3)163.5
N4—H15N···O5C0.901.922.812 (3)170.9
N4—H16N···O4D0.901.892.774 (3)166.2
N5—H17N···O5Bi0.901.912.801 (3)172.1
N5—H18N···O5F0.901.912.763 (2)158.2
N5—H19N···O4Aii0.901.882.758 (3)163.9
N5—H20N···O4D0.901.952.845 (3)170.4
N6—H21N···O5Eiv0.901.902.765 (3)161.0
N6—H21N···O50Eiv0.902.022.908 (12)168.5
N6—H22N···O4F0.901.932.812 (3)164.5
N6—H23N···O5E0.901.862.757 (3)172.6
N6—H23N···O50E0.902.163.061 (19)176.0
N6—H24N···O4Aii0.901.972.861 (3)171.6
N7—H25N···O5Gv0.901.962.824 (3)160.4
N7—H26N···O5G0.901.892.785 (3)175.4
N7—H27N···O4Kvi0.901.982.865 (3)167.0
N7—H28N···O4Lvii0.901.932.803 (3)163.5
N7—H28N···O40Lvii0.902.243.110 (19)161.7
N8—H29N···O4H0.901.972.867 (3)171.4
N8—H30N···O4Kvi0.901.882.765 (3)165.1
N8—H31N···O5Jviii0.901.912.806 (3)178.2
N8—H32N···O5Lvii0.901.952.761 (3)149.5
N8—H32N···O50Lvii0.902.192.974 (15)144.7
N9—H33N···O4Ivi0.902.022.892 (3)161.7
N9—H33N···O40Ivi0.901.842.713 (16)162.2
N9—H34N···O5I0.901.852.753 (3)175.0
N9—H34N···O50I0.902.193.088 (14)172.7
N9—H35N···O5Kvi0.901.952.810 (2)159.4
N9—H36N···O4H0.901.912.781 (3)162.6
N10—H37N···O4J0.901.972.871 (3)175.6
N10—H38N···O5Hviii0.901.892.787 (3)177.5
N10—H39N···O4Ivi0.901.952.834 (3)164.8
N10—H39N···O40Ivi0.901.732.601 (13)163.3
N10—H40N···O5H0.902.022.825 (3)148.1
N11—H41N···O5Ivi0.901.932.769 (3)155.4
N11—H41N···O50Ivi0.901.972.852 (10)166.9
N11—H42N···O4Gvi0.901.982.862 (3)166.1
N11—H43N···O4J0.901.902.773 (3)163.1
N11—H44N···O5K0.901.912.809 (3)175.4
N12—H45N···O4L0.901.982.869 (3)167.7
N12—H45N···O40L0.902.123.01 (3)169.8
N12—H46N···O5Lix0.901.892.790 (3)175.9
N12—H46N···O50Lix0.901.722.62 (2)176.1
N12—H47N···O4Gvi0.901.902.780 (3)164.1
N12—H48N···O5J0.902.022.813 (3)146.7
C1B—H1B1···O21K0.992.433.402 (3)165.6
C1C—H1C2···O21J0.992.463.434 (3)169.6
C3C—H3C2···O4B0.992.583.532 (3)161.9
C3D—H3D1···O40Ex0.992.423.359 (16)159.1
C4D—H4D3···O4Ex0.982.603.513 (3)155.9
C4D—H4D3···O40Ex0.982.563.451 (19)151.3
C4E—H4E2···O4D0.982.503.295 (3)138.5
C5E—H5E1···O1F0.982.613.507 (3)152.1
C4F—H4F1···O4Axi0.982.593.288 (3)128.0
C5F—H5F2···O1Ex0.982.543.433 (3)151.2
C5H—H5H2···O1Ixii0.982.543.135 (3)119.3
C1I—H1I1···O21D0.992.573.553 (3)170.0
C3I—H3I2···O4J0.992.583.564 (3)170.8
C4I—H4I2···O4J0.982.533.311 (3)136.0
C10I—H10D···O21D0.992.613.574 (9)163.9
C30I—H30D···O4J0.992.593.534 (9)159.7
C1J—H1J1···O21C0.992.503.477 (3)170.9
C3J—H3J1···O40Ixii0.992.583.547 (13)164.4
C1K—H1K2···O21B0.992.533.508 (3)170.9
C1L—H1L2···O21A0.992.603.582 (3)171.0
C3L—H3L1···O4Kxii0.992.603.578 (3)168.9
C30L—H30E···O4Kxii0.992.443.389 (17)160.6
C4L—H4L3···O4Kxii0.982.553.313 (3)135.1
C50L—H50G···O1Gxiii0.982.493.41 (3)155.2
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x, y1, z; (iv) x+1, y+2, z+1; (v) x+2, y+2, z; (vi) x+2, y+1, z; (vii) x, y+1, z; (viii) x+1, y+1, z; (ix) x+1, y, z; (x) x+1, y, z; (xi) x+1, y+1, z; (xii) x1, y, z; (xiii) x1, y1, z.
 

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