Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106023573/gp5011sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106023573/gp5011100_K_whole-datasetsup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106023573/gp5011100_K_averagesup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106023573/gp5011150_K_whole-datasetsup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106023573/gp5011200_K_whole-datasetsup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768106023573/gp5011250_K_whole-datasetsup6.hkl |
CCDC references: 624357; 624358; 624359; 624360; 624361
C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | Z = 4 |
Mr = 475.30 | F(000) = 1008 |
Monoclinic, P21 | Dx = 1.615 Mg m−3 |
Hall symbol: P 2yb | Mo Kα radiation, λ = 0.71073 Å |
a = 7.851 (3) Å | Cell parameters from 17710 reflections |
b = 21.976 (5) Å | µ = 0.31 mm−1 |
c = 11.332 (4) Å | T = 100 K |
β = 90.00 (3)° | Plates, colourless |
V = 1955.2 (11) Å3 | 0.40 × 0.18 × 0.10 mm |
Xcalibur PX diffractometer | 16051 independent reflections |
Radiation source: fine-focus sealed tube | 9264 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
ω scans | θmax = 38.6°, θmin = 4.5° |
Absorption correction: numerical CrysAlis RED, ver. 1.171, Oxford Diffraction Poland (1995-2003) | h = −13→13 |
Tmin = 0.888, Tmax = 0.970 | k = −38→28 |
49395 measured reflections | l = −19→19 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.046 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.087 | w = 1/[σ2(Fo2) + (0.0209P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.15 | (Δ/σ)max = 0.004 |
16051 reflections | Δρmax = 0.41 e Å−3 |
619 parameters | Δρmin = −0.45 e Å−3 |
37 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.03 (5) |
C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | V = 1955.2 (11) Å3 |
Mr = 475.30 | Z = 4 |
Monoclinic, P21 | Mo Kα radiation |
a = 7.851 (3) Å | µ = 0.31 mm−1 |
b = 21.976 (5) Å | T = 100 K |
c = 11.332 (4) Å | 0.40 × 0.18 × 0.10 mm |
β = 90.00 (3)° |
Xcalibur PX diffractometer | 16051 independent reflections |
Absorption correction: numerical CrysAlis RED, ver. 1.171, Oxford Diffraction Poland (1995-2003) | 9264 reflections with I > 2σ(I) |
Tmin = 0.888, Tmax = 0.970 | Rint = 0.043 |
49395 measured reflections |
R[F2 > 2σ(F2)] = 0.046 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.087 | Δρmax = 0.41 e Å−3 |
S = 1.15 | Δρmin = −0.45 e Å−3 |
16051 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
619 parameters | Absolute structure parameter: 0.03 (5) |
37 restraints |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
P1 | −0.24153 (6) | 0.85279 (3) | 1.11825 (5) | 0.01163 (11) | |
O11 | −0.26133 (18) | 0.91620 (7) | 1.07421 (13) | 0.0175 (3) | |
O21 | −0.22154 (19) | 0.85170 (7) | 1.25490 (12) | 0.0173 (3) | |
H210 | −0.2531 | 0.8177 | 1.2809 | 0.021* | |
O31 | −0.06029 (17) | 0.83039 (6) | 1.06550 (12) | 0.0131 (3) | |
O41 | −0.37528 (17) | 0.80719 (6) | 1.08190 (13) | 0.0154 (3) | |
C11 | 0.2271 (2) | 0.77946 (9) | 0.93718 (18) | 0.0124 (4) | |
C21 | 0.1885 (2) | 0.76684 (9) | 1.06883 (17) | 0.0115 (4) | |
H21 | 0.2293 | 0.7249 | 1.0882 | 0.014* | |
C31 | −0.0007 (2) | 0.77015 (9) | 1.09543 (19) | 0.0136 (4) | |
H311 | −0.0628 | 0.7393 | 1.0486 | 0.016* | |
H312 | −0.0211 | 0.7619 | 1.1802 | 0.016* | |
N1 | 0.2827 (2) | 0.81092 (8) | 1.14417 (15) | 0.0141 (4) | |
H1N1 | 0.3950 | 0.8105 | 1.1244 | 0.017* | |
H2N1 | 0.2709 | 0.8003 | 1.2213 | 0.017* | |
H3N1 | 0.2398 | 0.8490 | 1.1329 | 0.017* | |
O61 | 0.2044 (2) | 0.73575 (7) | 0.86714 (14) | 0.0233 (4) | |
O62 | 0.27933 (18) | 0.83089 (7) | 0.90887 (13) | 0.0173 (3) | |
P2 | 0.74494 (7) | 0.49784 (2) | 0.86704 (5) | 0.01152 (13) | |
O12 | 0.76497 (18) | 0.43449 (7) | 0.82252 (13) | 0.0175 (3) | |
O22 | 0.72781 (19) | 0.49917 (6) | 1.00356 (12) | 0.0158 (3) | |
H220 | 0.7647 | 0.5325 | 1.0294 | 0.019* | |
O32 | 0.56288 (16) | 0.52007 (6) | 0.81572 (12) | 0.0119 (3) | |
O42 | 0.87841 (17) | 0.54375 (7) | 0.82853 (13) | 0.0152 (3) | |
C12 | 0.2767 (2) | 0.57327 (9) | 0.68658 (18) | 0.0122 (4) | |
C22 | 0.3149 (2) | 0.58417 (9) | 0.81808 (17) | 0.0111 (4) | |
H22 | 0.2742 | 0.6259 | 0.8392 | 0.013* | |
C32 | 0.5044 (2) | 0.58032 (9) | 0.84641 (19) | 0.0126 (4) | |
H321 | 0.5680 | 0.6113 | 0.8006 | 0.015* | |
H322 | 0.5235 | 0.5880 | 0.9315 | 0.015* | |
N2 | 0.2199 (2) | 0.53930 (8) | 0.89193 (15) | 0.0124 (3) | |
H1N2 | 0.1065 | 0.5421 | 0.8761 | 0.015* | |
H2N2 | 0.2384 | 0.5474 | 0.9696 | 0.015* | |
H3N2 | 0.2569 | 0.5010 | 0.8750 | 0.015* | |
O51 | 0.3008 (2) | 0.61713 (7) | 0.61739 (15) | 0.0249 (4) | |
O52 | 0.22210 (19) | 0.52189 (7) | 0.65672 (13) | 0.0176 (3) | |
P3 | 0.74982 (7) | 0.50220 (2) | 0.36481 (5) | 0.01077 (12) | |
O13 | 0.76939 (18) | 0.43916 (7) | 0.31540 (13) | 0.0153 (3) | |
O43 | 0.88334 (17) | 0.54753 (6) | 0.32224 (13) | 0.0151 (3) | |
O33 | 0.56766 (17) | 0.52464 (6) | 0.31172 (12) | 0.0131 (3) | |
O23 | 0.73621 (18) | 0.50468 (7) | 0.49935 (12) | 0.0162 (3) | |
C13 | 0.2832 (3) | 0.57358 (10) | 0.18358 (18) | 0.0139 (4) | |
C23 | 0.3149 (2) | 0.58536 (9) | 0.31634 (17) | 0.0102 (4) | |
H23 | 0.2705 | 0.6267 | 0.3365 | 0.012* | |
C33 | 0.5040 (2) | 0.58332 (9) | 0.34499 (19) | 0.0131 (4) | |
H331 | 0.5649 | 0.6156 | 0.3010 | 0.016* | |
H332 | 0.5219 | 0.5901 | 0.4305 | 0.016* | |
O53 | 0.22571 (19) | 0.52293 (7) | 0.15397 (14) | 0.0169 (3) | |
O63 | 0.3220 (2) | 0.61604 (7) | 0.11476 (14) | 0.0240 (4) | |
N3 | 0.2222 (2) | 0.53964 (8) | 0.38849 (15) | 0.0130 (3) | |
H1N3 | 0.1113 | 0.5382 | 0.3653 | 0.016* | |
H2N3 | 0.2277 | 0.5503 | 0.4660 | 0.016* | |
H3N3 | 0.2707 | 0.5024 | 0.3784 | 0.016* | |
P4 | −0.25186 (6) | 0.85281 (2) | 0.61625 (5) | 0.01030 (10) | |
O14 | −0.27195 (17) | 0.91587 (6) | 0.56698 (12) | 0.0148 (3) | |
O44 | −0.38433 (17) | 0.80712 (6) | 0.57241 (13) | 0.0140 (3) | |
O34 | −0.06889 (16) | 0.83089 (6) | 0.56436 (12) | 0.0118 (3) | |
O24 | −0.23933 (17) | 0.85032 (6) | 0.75064 (12) | 0.0145 (3) | |
C14 | 0.2148 (3) | 0.78010 (9) | 0.43539 (18) | 0.0137 (4) | |
C24 | 0.1825 (2) | 0.76947 (8) | 0.56870 (17) | 0.0100 (4) | |
H24 | 0.2264 | 0.7282 | 0.5902 | 0.012* | |
C34 | −0.0058 (2) | 0.77218 (8) | 0.59827 (19) | 0.0118 (4) | |
H341 | −0.0678 | 0.7399 | 0.5552 | 0.014* | |
H342 | −0.0228 | 0.7658 | 0.6839 | 0.014* | |
O54 | 0.27299 (18) | 0.83057 (7) | 0.40537 (13) | 0.0169 (3) | |
O64 | 0.1749 (2) | 0.73767 (7) | 0.36763 (14) | 0.0235 (4) | |
N4 | 0.2764 (2) | 0.81584 (8) | 0.63956 (15) | 0.0115 (3) | |
H1N4 | 0.3891 | 0.8146 | 0.6208 | 0.014* | |
H2N4 | 0.2631 | 0.8077 | 0.7178 | 0.014* | |
H3N4 | 0.2344 | 0.8535 | 0.6233 | 0.014* | |
N11 | 1.0205 (3) | 0.92891 (9) | 0.37794 (19) | 0.0180 (4) | |
H11N | 0.940 (2) | 0.9562 (8) | 0.356 (2) | 0.022* | |
H21N | 1.085 (3) | 0.9545 (9) | 0.4223 (18) | 0.022* | |
H31N | 1.070 (3) | 0.9211 (11) | 0.3071 (10) | 0.022* | |
H41N | 0.992 (3) | 0.8930 (6) | 0.4128 (19) | 0.022* | |
N21 | 1.5197 (3) | 0.92494 (10) | 0.8754 (2) | 0.0189 (4) | |
H12N | 1.567 (3) | 0.9316 (11) | 0.9474 (9) | 0.023* | |
H22N | 1.587 (3) | 0.9054 (10) | 0.8223 (16) | 0.023* | |
H32N | 1.435 (2) | 0.8986 (9) | 0.894 (2) | 0.023* | |
H42N | 1.482 (3) | 0.9603 (6) | 0.843 (2) | 0.023* | |
N31 | 1.0013 (2) | 0.92349 (10) | 0.86407 (18) | 0.0155 (4) | |
H13N | 1.084 (2) | 0.9285 (10) | 0.8085 (15) | 0.019* | |
H23N | 0.937 (3) | 0.9574 (6) | 0.875 (2) | 0.019* | |
H33N | 1.041 (3) | 0.9057 (9) | 0.9310 (11) | 0.019* | |
H43N | 0.925 (2) | 0.8956 (8) | 0.836 (2) | 0.019* | |
N41 | 1.5002 (2) | 0.92942 (9) | 0.38612 (18) | 0.0154 (4) | |
H14N | 1.431 (2) | 0.8963 (7) | 0.380 (2) | 0.019* | |
H24N | 1.5907 (18) | 0.9254 (10) | 0.4357 (16) | 0.019* | |
H34N | 1.532 (3) | 0.9433 (10) | 0.3139 (9) | 0.019* | |
H44N | 1.427 (2) | 0.9574 (8) | 0.4174 (19) | 0.019* | |
N51 | 0.8629 (3) | 0.60202 (9) | 0.61423 (18) | 0.0183 (4) | |
H15N | 0.861 (3) | 0.5899 (11) | 0.6909 (7) | 0.022* | |
H25N | 0.787 (2) | 0.6332 (8) | 0.618 (2) | 0.022* | |
H35N | 0.9696 (13) | 0.6178 (10) | 0.607 (2) | 0.022* | |
H45N | 0.820 (3) | 0.5688 (7) | 0.5768 (19) | 0.022* | |
N61 | 0.6347 (3) | 0.75172 (9) | 0.86315 (18) | 0.0183 (4) | |
H16N | 0.622 (3) | 0.7695 (10) | 0.9351 (10) | 0.022* | |
H26N | 0.708 (2) | 0.7197 (7) | 0.861 (2) | 0.022* | |
H36N | 0.5311 (14) | 0.7355 (10) | 0.846 (2) | 0.022* | |
H46N | 0.646 (3) | 0.7863 (6) | 0.8195 (18) | 0.022* | |
O1W | 0.8612 (2) | 0.59363 (9) | 0.09925 (16) | 0.0283 (4) | |
H101 | 0.881 (3) | 0.5780 (12) | 0.1635 (12) | 0.034* | |
H102 | 0.791 (3) | 0.6211 (9) | 0.103 (3) | 0.034* | |
O2W | 0.9099 (2) | 0.67048 (8) | 0.8564 (2) | 0.0339 (5) | |
H201 | 0.995 (2) | 0.6906 (12) | 0.871 (2) | 0.041* | |
H202 | 0.871 (4) | 0.6387 (8) | 0.883 (3) | 0.041* | |
O3W | 0.6462 (2) | 0.75799 (9) | 0.35318 (16) | 0.0274 (4) | |
H301 | 0.619 (3) | 0.7739 (11) | 0.4159 (12) | 0.033* | |
H302 | 0.725 (2) | 0.7337 (10) | 0.359 (3) | 0.033* | |
O4W | 0.6126 (3) | 0.68018 (8) | 0.10271 (19) | 0.0343 (5) | |
H401 | 0.528 (2) | 0.6607 (12) | 0.121 (2) | 0.041* | |
H402 | 0.614 (4) | 0.7141 (6) | 0.132 (2) | 0.041* | |
O5W | 0.5936 (2) | 0.68573 (8) | 0.63467 (17) | 0.0291 (4) | |
H501 | 0.4974 (15) | 0.6718 (12) | 0.626 (2) | 0.035* | |
H502 | 0.577 (4) | 0.7221 (3) | 0.623 (3) | 0.035* | |
O6W | −0.1110 (2) | 0.66948 (8) | 0.38383 (18) | 0.0309 (4) | |
H601 | −0.0157 (16) | 0.6841 (12) | 0.375 (2) | 0.037* | |
H602 | −0.090 (4) | 0.6333 (3) | 0.375 (3) | 0.037* |
U11 | U22 | U33 | U12 | U13 | U23 | |
P1 | 0.0095 (2) | 0.0132 (2) | 0.0122 (3) | 0.0009 (2) | −0.00017 (19) | −0.0011 (2) |
O11 | 0.0186 (7) | 0.0152 (7) | 0.0186 (8) | 0.0035 (6) | −0.0001 (6) | 0.0014 (6) |
O21 | 0.0233 (7) | 0.0172 (7) | 0.0113 (7) | −0.0032 (7) | 0.0010 (6) | −0.0012 (6) |
O31 | 0.0107 (6) | 0.0137 (7) | 0.0150 (7) | 0.0024 (5) | 0.0030 (5) | 0.0030 (6) |
O41 | 0.0106 (7) | 0.0172 (7) | 0.0183 (8) | −0.0009 (6) | 0.0020 (6) | −0.0027 (6) |
C11 | 0.0091 (9) | 0.0158 (9) | 0.0125 (10) | 0.0008 (7) | −0.0005 (7) | 0.0012 (8) |
C21 | 0.0091 (9) | 0.0134 (9) | 0.0120 (10) | −0.0005 (7) | 0.0019 (7) | 0.0012 (8) |
C31 | 0.0101 (9) | 0.0141 (9) | 0.0166 (10) | 0.0030 (8) | 0.0023 (8) | 0.0027 (8) |
N1 | 0.0122 (8) | 0.0174 (9) | 0.0127 (9) | −0.0001 (7) | 0.0009 (6) | −0.0012 (7) |
O61 | 0.0352 (9) | 0.0202 (8) | 0.0146 (8) | −0.0021 (8) | 0.0028 (7) | −0.0067 (7) |
O62 | 0.0188 (7) | 0.0170 (7) | 0.0160 (8) | −0.0056 (6) | 0.0018 (6) | 0.0044 (6) |
P2 | 0.0085 (2) | 0.0137 (3) | 0.0124 (3) | 0.0013 (2) | 0.00090 (19) | 0.0027 (2) |
O12 | 0.0178 (7) | 0.0163 (8) | 0.0185 (8) | 0.0041 (6) | 0.0007 (6) | −0.0022 (6) |
O22 | 0.0217 (7) | 0.0153 (8) | 0.0105 (7) | −0.0020 (6) | −0.0004 (6) | 0.0015 (6) |
O32 | 0.0093 (6) | 0.0115 (7) | 0.0148 (7) | 0.0028 (5) | −0.0017 (5) | −0.0023 (5) |
O42 | 0.0106 (7) | 0.0191 (7) | 0.0159 (8) | −0.0002 (6) | −0.0012 (5) | 0.0038 (6) |
C12 | 0.0100 (9) | 0.0143 (10) | 0.0124 (10) | 0.0009 (8) | −0.0005 (7) | −0.0009 (8) |
C22 | 0.0132 (9) | 0.0093 (8) | 0.0107 (9) | −0.0004 (7) | −0.0014 (7) | −0.0008 (7) |
C32 | 0.0101 (9) | 0.0098 (9) | 0.0179 (11) | 0.0000 (7) | −0.0001 (7) | −0.0007 (8) |
N2 | 0.0103 (8) | 0.0154 (8) | 0.0114 (9) | 0.0005 (7) | −0.0001 (6) | 0.0011 (7) |
O51 | 0.0373 (10) | 0.0203 (8) | 0.0172 (8) | −0.0034 (8) | −0.0041 (7) | 0.0076 (7) |
O52 | 0.0215 (8) | 0.0208 (8) | 0.0104 (7) | −0.0025 (6) | −0.0011 (6) | −0.0040 (6) |
P3 | 0.0088 (2) | 0.0098 (3) | 0.0137 (3) | 0.00011 (19) | −0.00087 (19) | −0.0008 (2) |
O13 | 0.0144 (7) | 0.0107 (7) | 0.0207 (8) | 0.0027 (5) | 0.0003 (6) | 0.0005 (6) |
O43 | 0.0093 (6) | 0.0124 (7) | 0.0237 (8) | −0.0013 (5) | −0.0010 (6) | 0.0009 (6) |
O33 | 0.0095 (7) | 0.0124 (7) | 0.0175 (8) | 0.0013 (5) | −0.0020 (5) | −0.0030 (6) |
O23 | 0.0182 (7) | 0.0177 (8) | 0.0127 (7) | −0.0011 (6) | −0.0035 (6) | 0.0001 (6) |
C13 | 0.0110 (9) | 0.0189 (10) | 0.0118 (10) | 0.0042 (8) | −0.0031 (7) | −0.0005 (8) |
C23 | 0.0084 (8) | 0.0093 (8) | 0.0129 (10) | 0.0025 (7) | −0.0011 (7) | −0.0008 (8) |
C33 | 0.0104 (9) | 0.0128 (9) | 0.0160 (10) | 0.0008 (7) | −0.0019 (7) | −0.0031 (8) |
O53 | 0.0161 (7) | 0.0150 (7) | 0.0195 (8) | −0.0025 (6) | −0.0021 (6) | −0.0037 (6) |
O63 | 0.0348 (10) | 0.0234 (9) | 0.0138 (8) | −0.0024 (8) | −0.0015 (7) | 0.0055 (7) |
N3 | 0.0111 (8) | 0.0162 (9) | 0.0116 (9) | 0.0012 (7) | 0.0005 (6) | 0.0019 (7) |
P4 | 0.0081 (2) | 0.0099 (2) | 0.0128 (3) | 0.0004 (2) | 0.00070 (18) | −0.0003 (2) |
O14 | 0.0129 (7) | 0.0127 (6) | 0.0187 (8) | 0.0018 (6) | −0.0023 (6) | 0.0012 (6) |
O44 | 0.0094 (7) | 0.0137 (7) | 0.0188 (8) | −0.0006 (5) | −0.0005 (5) | −0.0031 (6) |
O34 | 0.0082 (6) | 0.0110 (6) | 0.0163 (7) | 0.0022 (5) | 0.0013 (5) | 0.0019 (6) |
O24 | 0.0166 (7) | 0.0159 (7) | 0.0111 (7) | −0.0001 (6) | 0.0018 (5) | −0.0005 (6) |
C14 | 0.0124 (9) | 0.0146 (9) | 0.0140 (10) | 0.0027 (8) | 0.0018 (7) | −0.0001 (8) |
C24 | 0.0112 (9) | 0.0083 (8) | 0.0106 (9) | 0.0016 (7) | 0.0001 (7) | 0.0008 (7) |
C34 | 0.0092 (9) | 0.0101 (9) | 0.0162 (10) | −0.0013 (7) | 0.0007 (7) | 0.0026 (8) |
O54 | 0.0168 (7) | 0.0183 (8) | 0.0158 (8) | 0.0009 (6) | 0.0028 (6) | 0.0044 (6) |
O64 | 0.0310 (9) | 0.0246 (9) | 0.0149 (8) | −0.0049 (8) | 0.0019 (7) | −0.0053 (7) |
N4 | 0.0103 (8) | 0.0129 (8) | 0.0114 (8) | 0.0009 (6) | −0.0009 (6) | 0.0002 (7) |
N11 | 0.0193 (9) | 0.0144 (9) | 0.0203 (9) | 0.0053 (8) | 0.0033 (7) | 0.0021 (8) |
N21 | 0.0169 (9) | 0.0183 (10) | 0.0214 (9) | −0.0018 (8) | −0.0012 (7) | 0.0004 (8) |
N31 | 0.0144 (9) | 0.0163 (9) | 0.0158 (9) | 0.0020 (7) | 0.0005 (7) | 0.0010 (7) |
N41 | 0.0142 (9) | 0.0151 (9) | 0.0171 (9) | −0.0057 (7) | −0.0044 (7) | 0.0033 (8) |
N51 | 0.0233 (10) | 0.0164 (10) | 0.0153 (9) | −0.0008 (8) | 0.0049 (8) | 0.0017 (7) |
N61 | 0.0201 (10) | 0.0166 (10) | 0.0184 (10) | 0.0012 (8) | −0.0020 (8) | −0.0035 (8) |
O1W | 0.0293 (10) | 0.0300 (10) | 0.0255 (10) | 0.0083 (8) | −0.0008 (8) | 0.0085 (8) |
O2W | 0.0272 (10) | 0.0149 (8) | 0.0596 (13) | −0.0037 (8) | −0.0026 (9) | −0.0086 (9) |
O3W | 0.0339 (10) | 0.0277 (10) | 0.0207 (9) | 0.0039 (8) | −0.0004 (8) | −0.0063 (8) |
O4W | 0.0303 (11) | 0.0188 (9) | 0.0537 (13) | −0.0054 (8) | 0.0024 (9) | 0.0067 (9) |
O5W | 0.0279 (10) | 0.0151 (8) | 0.0442 (11) | −0.0004 (7) | −0.0001 (8) | 0.0085 (8) |
O6W | 0.0256 (10) | 0.0178 (8) | 0.0493 (12) | −0.0035 (8) | 0.0046 (9) | −0.0080 (9) |
P1—O11 | 1.4883 (16) | P4—O24 | 1.5271 (16) |
P1—O41 | 1.5088 (16) | P4—O44 | 1.5286 (15) |
P1—O21 | 1.5566 (16) | P4—O34 | 1.6252 (15) |
P1—O31 | 1.6199 (15) | O34—C34 | 1.435 (2) |
O21—H210 | 0.8400 | C14—O54 | 1.247 (2) |
O31—C31 | 1.445 (2) | C14—O64 | 1.248 (2) |
C11—O62 | 1.244 (2) | C14—C24 | 1.549 (3) |
C11—O61 | 1.259 (2) | C24—N4 | 1.492 (2) |
C11—C21 | 1.548 (3) | C24—C34 | 1.517 (3) |
C21—N1 | 1.488 (3) | C24—H24 | 1.0000 |
C21—C31 | 1.517 (3) | C34—H341 | 0.9900 |
C21—H21 | 1.0000 | C34—H342 | 0.9900 |
C31—H311 | 0.9900 | N4—H1N4 | 0.9100 |
C31—H312 | 0.9900 | N4—H2N4 | 0.9100 |
N1—H1N1 | 0.9100 | N4—H3N4 | 0.9100 |
N1—H2N1 | 0.9100 | N11—H11N | 0.909 (3) |
N1—H3N1 | 0.9100 | N11—H21N | 0.910 (3) |
P2—O12 | 1.4891 (16) | N11—H31N | 0.909 (3) |
P2—O42 | 1.5187 (16) | N11—H41N | 0.910 (3) |
P2—O22 | 1.5532 (16) | N21—H12N | 0.909 (3) |
P2—O32 | 1.6186 (15) | N21—H22N | 0.910 (3) |
O22—H220 | 0.8400 | N21—H32N | 0.909 (3) |
O32—C32 | 1.444 (2) | N21—H42N | 0.909 (3) |
C12—O52 | 1.254 (2) | N31—H13N | 0.910 (3) |
C12—O51 | 1.257 (2) | N31—H23N | 0.909 (3) |
C12—C22 | 1.539 (3) | N31—H33N | 0.909 (3) |
C22—N2 | 1.493 (3) | N31—H43N | 0.910 (3) |
C22—C32 | 1.525 (3) | N41—H14N | 0.909 (3) |
C22—H22 | 1.0000 | N41—H24N | 0.910 (3) |
C32—H321 | 0.9900 | N41—H34N | 0.909 (3) |
C32—H322 | 0.9900 | N41—H44N | 0.911 (3) |
N2—H1N2 | 0.9100 | N51—H15N | 0.909 (3) |
N2—H2N2 | 0.9100 | N51—H25N | 0.909 (3) |
N2—H3N2 | 0.9100 | N51—H35N | 0.911 (3) |
P3—O13 | 1.5021 (15) | N51—H45N | 0.910 (3) |
P3—O43 | 1.5244 (15) | N61—H16N | 0.910 (3) |
P3—O23 | 1.5294 (16) | N61—H26N | 0.911 (3) |
P3—O33 | 1.6280 (15) | N61—H36N | 0.910 (3) |
O33—C33 | 1.434 (2) | N61—H46N | 0.910 (3) |
C13—O53 | 1.247 (2) | O1W—H101 | 0.820 (2) |
C13—O63 | 1.254 (3) | O1W—H102 | 0.820 (2) |
C13—C23 | 1.547 (3) | O2W—H201 | 0.820 (2) |
C23—N3 | 1.486 (3) | O2W—H202 | 0.819 (2) |
C23—C33 | 1.521 (3) | O3W—H301 | 0.820 (2) |
C23—H23 | 1.0000 | O3W—H302 | 0.820 (2) |
C33—H331 | 0.9900 | O4W—H401 | 0.820 (2) |
C33—H332 | 0.9900 | O4W—H402 | 0.819 (2) |
N3—H1N3 | 0.9100 | O5W—H501 | 0.820 (2) |
N3—H2N3 | 0.9100 | O5W—H502 | 0.820 (2) |
N3—H3N3 | 0.9100 | O6W—H601 | 0.820 (2) |
P4—O14 | 1.5024 (16) | O6W—H602 | 0.820 (2) |
O11—P1—O41 | 117.23 (9) | C23—C33—H332 | 110.1 |
O11—P1—O21 | 111.00 (9) | H331—C33—H332 | 108.4 |
O41—P1—O21 | 109.36 (9) | C23—N3—H1N3 | 109.5 |
O11—P1—O31 | 104.63 (8) | C23—N3—H2N3 | 109.5 |
O41—P1—O31 | 107.99 (8) | H1N3—N3—H2N3 | 109.5 |
O21—P1—O31 | 105.89 (9) | C23—N3—H3N3 | 109.5 |
P1—O21—H210 | 109.5 | H1N3—N3—H3N3 | 109.5 |
C31—O31—P1 | 118.46 (12) | H2N3—N3—H3N3 | 109.5 |
O62—C11—O61 | 125.3 (2) | O14—P4—O24 | 114.24 (9) |
O62—C11—C21 | 118.43 (18) | O14—P4—O44 | 114.44 (8) |
O61—C11—C21 | 116.31 (18) | O24—P4—O44 | 110.15 (8) |
N1—C21—C31 | 109.97 (16) | O14—P4—O34 | 103.40 (8) |
N1—C21—C11 | 109.80 (16) | O24—P4—O34 | 107.05 (8) |
C31—C21—C11 | 112.03 (16) | O44—P4—O34 | 106.80 (8) |
N1—C21—H21 | 108.3 | C34—O34—P4 | 118.36 (12) |
C31—C21—H21 | 108.3 | O54—C14—O64 | 126.1 (2) |
C11—C21—H21 | 108.3 | O54—C14—C24 | 117.38 (18) |
O31—C31—C21 | 108.33 (16) | O64—C14—C24 | 116.51 (18) |
O31—C31—H311 | 110.0 | N4—C24—C34 | 109.62 (15) |
C21—C31—H311 | 110.0 | N4—C24—C14 | 109.93 (15) |
O31—C31—H312 | 110.0 | C34—C24—C14 | 111.64 (16) |
C21—C31—H312 | 110.0 | N4—C24—H24 | 108.5 |
H311—C31—H312 | 108.4 | C34—C24—H24 | 108.5 |
C21—N1—H1N1 | 109.5 | C14—C24—H24 | 108.5 |
C21—N1—H2N1 | 109.5 | O34—C34—C24 | 108.23 (15) |
H1N1—N1—H2N1 | 109.5 | O34—C34—H341 | 110.1 |
C21—N1—H3N1 | 109.5 | C24—C34—H341 | 110.1 |
H1N1—N1—H3N1 | 109.5 | O34—C34—H342 | 110.1 |
H2N1—N1—H3N1 | 109.5 | C24—C34—H342 | 110.1 |
O12—P2—O42 | 116.80 (9) | H341—C34—H342 | 108.4 |
O12—P2—O22 | 111.36 (9) | C24—N4—H1N4 | 109.5 |
O42—P2—O22 | 109.48 (9) | C24—N4—H2N4 | 109.5 |
O12—P2—O32 | 104.70 (8) | H1N4—N4—H2N4 | 109.5 |
O42—P2—O32 | 107.79 (8) | C24—N4—H3N4 | 109.5 |
O22—P2—O32 | 106.01 (9) | H1N4—N4—H3N4 | 109.5 |
P2—O22—H220 | 109.5 | H2N4—N4—H3N4 | 109.5 |
C32—O32—P2 | 118.09 (12) | H11N—N11—H21N | 98 (2) |
O52—C12—O51 | 125.00 (19) | H11N—N11—H31N | 100 (2) |
O52—C12—C22 | 117.90 (18) | H21N—N11—H31N | 111 (2) |
O51—C12—C22 | 117.09 (18) | H11N—N11—H41N | 121 (2) |
N2—C22—C32 | 109.43 (16) | H21N—N11—H41N | 116 (2) |
N2—C22—C12 | 110.04 (16) | H31N—N11—H41N | 109 (2) |
C32—C22—C12 | 112.66 (16) | H12N—N21—H22N | 115 (2) |
N2—C22—H22 | 108.2 | H12N—N21—H32N | 101 (2) |
C32—C22—H22 | 108.2 | H22N—N21—H32N | 106 (2) |
C12—C22—H22 | 108.2 | H12N—N21—H42N | 111 (2) |
O32—C32—C22 | 108.09 (15) | H22N—N21—H42N | 109 (2) |
O32—C32—H321 | 110.1 | H32N—N21—H42N | 113 (2) |
C22—C32—H321 | 110.1 | H13N—N31—H23N | 113 (2) |
O32—C32—H322 | 110.1 | H13N—N31—H33N | 113 (2) |
C22—C32—H322 | 110.1 | H23N—N31—H33N | 116 (2) |
H321—C32—H322 | 108.4 | H13N—N31—H43N | 108 (2) |
C22—N2—H1N2 | 109.5 | H23N—N31—H43N | 103 (2) |
C22—N2—H2N2 | 109.5 | H33N—N31—H43N | 103 (2) |
H1N2—N2—H2N2 | 109.5 | H14N—N41—H24N | 116 (2) |
C22—N2—H3N2 | 109.5 | H14N—N41—H34N | 111 (2) |
H1N2—N2—H3N2 | 109.5 | H24N—N41—H34N | 112 (2) |
H2N2—N2—H3N2 | 109.5 | H14N—N41—H44N | 101 (2) |
O13—P3—O43 | 114.48 (8) | H24N—N41—H44N | 108 (2) |
O13—P3—O23 | 114.30 (9) | H34N—N41—H44N | 107 (2) |
O43—P3—O23 | 109.89 (9) | H15N—N51—H25N | 100 (2) |
O13—P3—O33 | 103.38 (8) | H15N—N51—H35N | 102 (2) |
O43—P3—O33 | 106.81 (8) | H25N—N51—H35N | 109 (2) |
O23—P3—O33 | 107.23 (9) | H15N—N51—H45N | 102 (2) |
C33—O33—P3 | 118.79 (12) | H25N—N51—H45N | 112 (2) |
O53—C13—O63 | 125.8 (2) | H35N—N51—H45N | 127 (2) |
O53—C13—C23 | 117.98 (18) | H16N—N61—H26N | 115 (2) |
O63—C13—C23 | 116.21 (18) | H16N—N61—H36N | 106 (2) |
N3—C23—C33 | 109.93 (16) | H26N—N61—H36N | 105 (2) |
N3—C23—C13 | 110.09 (16) | H16N—N61—H46N | 98 (2) |
C33—C23—C13 | 111.07 (16) | H26N—N61—H46N | 125 (2) |
N3—C23—H23 | 108.6 | H36N—N61—H46N | 107 (2) |
C33—C23—H23 | 108.6 | H101—O1W—H102 | 113 (3) |
C13—C23—H23 | 108.6 | H201—O2W—H202 | 134 (3) |
O33—C33—C23 | 108.10 (15) | H301—O3W—H302 | 114 (3) |
O33—C33—H331 | 110.1 | H401—O4W—H402 | 113 (3) |
C23—C33—H331 | 110.1 | H501—O5W—H502 | 101 (3) |
O33—C33—H332 | 110.1 | H601—O6W—H602 | 100 (3) |
O11—P1—O31—C31 | 178.29 (14) | O13—P3—O33—C33 | 177.67 (14) |
O41—P1—O31—C31 | −56.12 (16) | O43—P3—O33—C33 | −61.21 (16) |
O21—P1—O31—C31 | 60.94 (16) | O23—P3—O33—C33 | 56.56 (16) |
O62—C11—C21—N1 | −21.8 (2) | O53—C13—C23—N3 | −16.8 (2) |
O61—C11—C21—N1 | 157.42 (18) | O63—C13—C23—N3 | 164.74 (17) |
O62—C11—C21—C31 | 100.7 (2) | O53—C13—C23—C33 | 105.2 (2) |
O61—C11—C21—C31 | −80.1 (2) | O63—C13—C23—C33 | −73.3 (2) |
P1—O31—C31—C21 | −162.94 (13) | P3—O33—C33—C23 | −162.85 (13) |
N1—C21—C31—O31 | 62.8 (2) | N3—C23—C33—O33 | 63.5 (2) |
C11—C21—C31—O31 | −59.6 (2) | C13—C23—C33—O33 | −58.6 (2) |
O12—P2—O32—C32 | 178.57 (13) | O14—P4—O34—C34 | 177.74 (14) |
O42—P2—O32—C32 | −56.42 (15) | O24—P4—O34—C34 | 56.78 (15) |
O22—P2—O32—C32 | 60.73 (15) | O44—P4—O34—C34 | −61.19 (15) |
O52—C12—C22—N2 | −21.1 (2) | O54—C14—C24—N4 | −16.9 (2) |
O51—C12—C22—N2 | 157.99 (18) | O64—C14—C24—N4 | 165.17 (18) |
O52—C12—C22—C32 | 101.3 (2) | O54—C14—C24—C34 | 104.9 (2) |
O51—C12—C22—C32 | −79.6 (2) | O64—C14—C24—C34 | −73.0 (2) |
P2—O32—C32—C22 | −164.50 (12) | P4—O34—C34—C24 | −164.22 (12) |
N2—C22—C32—O32 | 62.4 (2) | N4—C24—C34—O34 | 63.12 (19) |
C12—C22—C32—O32 | −60.4 (2) | C14—C24—C34—O34 | −58.9 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O21—H210···O3Wi | 0.84 | 1.74 | 2.561 (2) | 166 |
N1—H1N1···O41ii | 0.91 | 1.87 | 2.778 (2) | 178 |
N1—H2N1···O54iii | 0.91 | 2.19 | 2.992 (2) | 147 |
N1—H2N1···O64iii | 0.91 | 2.28 | 3.118 (3) | 152 |
N1—H3N1···O12iv | 0.91 | 1.95 | 2.767 (2) | 149 |
O22—H220···O1Wiii | 0.84 | 1.73 | 2.565 (3) | 170 |
N2—H1N2···O42v | 0.91 | 1.87 | 2.778 (2) | 174 |
N2—H2N2···O53iii | 0.91 | 2.16 | 2.991 (2) | 152 |
N2—H2N2···O63iii | 0.91 | 2.33 | 3.141 (3) | 149 |
N2—H3N2···O11vi | 0.91 | 1.95 | 2.752 (2) | 146 |
N3—H1N3···O43v | 0.91 | 1.87 | 2.769 (2) | 172 |
N3—H2N3···O52 | 0.91 | 2.25 | 3.065 (2) | 149 |
N3—H2N3···O51 | 0.91 | 2.33 | 3.164 (3) | 152 |
N3—H3N3···O14vii | 0.91 | 2.00 | 2.794 (2) | 145 |
N4—H1N4···O44ii | 0.91 | 1.87 | 2.777 (2) | 175 |
N4—H2N4···O62 | 0.91 | 2.23 | 3.070 (2) | 154 |
N4—H2N4···O61 | 0.91 | 2.36 | 3.173 (2) | 148 |
N4—H3N4···O13viii | 0.91 | 2.01 | 2.781 (2) | 142 |
N11—H11N···O52viii | 0.91 (1) | 1.93 (1) | 2.821 (3) | 167 (2) |
N11—H31N···O12ix | 0.91 (1) | 1.98 (1) | 2.831 (3) | 155 (2) |
N11—H41N···O34ii | 0.91 (1) | 2.25 (1) | 3.098 (3) | 156 (2) |
N21—H12N···O11x | 0.91 (1) | 2.00 (1) | 2.840 (3) | 154 (2) |
N21—H22N···O24x | 0.91 (1) | 2.00 (1) | 2.875 (3) | 162 (2) |
N21—H32N···O62ii | 0.91 (1) | 1.93 (1) | 2.824 (3) | 167 (2) |
N21—H42N···O33ix | 0.91 (1) | 2.29 (1) | 3.125 (3) | 153 (2) |
N31—H13N···O13ix | 0.91 (1) | 1.83 (1) | 2.738 (3) | 174 (2) |
N31—H23N···O53viii | 0.91 (1) | 1.95 (1) | 2.827 (3) | 161 (2) |
N31—H33N···O31ii | 0.91 (1) | 2.39 (2) | 3.103 (3) | 136 (2) |
N31—H33N···O62ii | 0.91 (1) | 2.50 (2) | 3.027 (3) | 117 (2) |
N31—H43N···O24ii | 0.91 (1) | 1.90 (1) | 2.794 (3) | 167 (2) |
N41—H14N···O54ii | 0.91 (1) | 1.93 (1) | 2.820 (3) | 166 (2) |
N41—H24N···O14x | 0.91 (1) | 1.85 (1) | 2.736 (3) | 164 (2) |
N41—H34N···O32ix | 0.91 (1) | 2.36 (2) | 3.073 (2) | 135 (2) |
N41—H44N···O23ix | 0.91 (1) | 1.90 (1) | 2.805 (3) | 170 (2) |
N51—H15N···O42 | 0.91 (1) | 1.87 (1) | 2.748 (3) | 163 (2) |
N51—H15N···O2W | 0.91 (1) | 2.61 (2) | 3.151 (3) | 119 (2) |
N51—H25N···O5W | 0.91 (1) | 1.92 (1) | 2.812 (3) | 168 (2) |
N51—H35N···O51ii | 0.91 (1) | 2.60 (1) | 3.454 (3) | 156 (2) |
N51—H45N···O23 | 0.91 (1) | 1.79 (1) | 2.695 (3) | 178 (2) |
N61—H16N···O41ii | 0.91 (1) | 1.86 (1) | 2.764 (3) | 173 (2) |
N61—H26N···O2W | 0.91 (1) | 1.92 (1) | 2.804 (3) | 164 (2) |
N61—H36N···O61 | 0.91 (1) | 2.58 (1) | 3.397 (3) | 150 (2) |
N61—H46N···O24ii | 0.91 (1) | 1.85 (1) | 2.701 (3) | 156 (2) |
O1W—H101···O43 | 0.82 (1) | 1.92 (1) | 2.728 (2) | 168 (3) |
O1W—H102···O4W | 0.82 (1) | 1.91 (1) | 2.725 (3) | 174 (3) |
O2W—H201···O61ii | 0.82 (1) | 1.92 (1) | 2.724 (3) | 167 (3) |
O2W—H202···O42 | 0.82 (1) | 2.17 (2) | 2.814 (2) | 135 (3) |
O2W—H202···O1Wiii | 0.82 (1) | 2.65 (2) | 3.251 (3) | 132 (3) |
O3W—H301···O44ii | 0.82 (1) | 1.92 (1) | 2.719 (2) | 165 (3) |
O3W—H302···O6Wii | 0.82 (1) | 1.93 (1) | 2.745 (3) | 172 (3) |
O4W—H401···O63 | 0.82 (1) | 1.89 (1) | 2.685 (3) | 163 (3) |
O4W—H402···O41xi | 0.82 (1) | 2.13 (2) | 2.803 (2) | 140 (3) |
O5W—H501···O51 | 0.82 (1) | 1.96 (1) | 2.756 (3) | 164 (3) |
O5W—H502···O44ii | 0.82 (1) | 1.98 (1) | 2.765 (2) | 161 (3) |
O6W—H601···O64 | 0.82 (1) | 1.91 (1) | 2.705 (3) | 164 (3) |
Symmetry codes: (i) x−1, y, z+1; (ii) x+1, y, z; (iii) x, y, z+1; (iv) −x+1, y+1/2, −z+2; (v) x−1, y, z; (vi) −x, y−1/2, −z+2; (vii) −x, y−1/2, −z+1; (viii) −x+1, y+1/2, −z+1; (ix) −x+2, y+1/2, −z+1; (x) x+2, y, z; (xi) x+1, y, z−1. |
C6H13N2O12P2·H6NO·2(H4N)·2(H2O) | F(000) = 504 |
Mr = 475.30 | Dx = 1.615 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 17710 reflections |
a = 7.851 (3) Å | µ = 0.31 mm−1 |
b = 21.976 (5) Å | T = 100 K |
c = 5.666 (2) Å | Plates, colourless |
V = 977.6 (6) Å3 | 0.40 × 0.18 × 0.10 mm |
Z = 2 |
Xcalibur PX diffractometer | 5369 independent reflections |
Radiation source: fine-focus sealed tube | 4404 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
/w scans | θmax = 38.5°, θmin = 4.5° |
Absorption correction: numerical CrysAlis RED, ver. 1.171, Oxford Diffraction Poland (1995-2003) | h = −13→13 |
Tmin = 0.888, Tmax = 0.970 | k = −38→28 |
24631 measured reflections | l = −9→9 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.039 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.103 | w = 1/[σ2(Fo2) + (0.0599P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max < 0.001 |
5369 reflections | Δρmax = 0.36 e Å−3 |
184 parameters | Δρmin = −0.42 e Å−3 |
26 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.16 (8) |
C6H13N2O12P2·H6NO·2(H4N)·2(H2O) | V = 977.6 (6) Å3 |
Mr = 475.30 | Z = 2 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 7.851 (3) Å | µ = 0.31 mm−1 |
b = 21.976 (5) Å | T = 100 K |
c = 5.666 (2) Å | 0.40 × 0.18 × 0.10 mm |
Xcalibur PX diffractometer | 5369 independent reflections |
Absorption correction: numerical CrysAlis RED, ver. 1.171, Oxford Diffraction Poland (1995-2003) | 4404 reflections with I > 2σ(I) |
Tmin = 0.888, Tmax = 0.970 | Rint = 0.046 |
24631 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.103 | Δρmax = 0.36 e Å−3 |
S = 1.02 | Δρmin = −0.42 e Å−3 |
5369 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
184 parameters | Absolute structure parameter: −0.16 (8) |
26 restraints |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
P1 | 0.25297 (4) | 0.176373 (12) | 0.48324 (5) | 0.01177 (6) | |
O1 | 0.23300 (12) | 0.23961 (4) | 0.38964 (16) | 0.01733 (16) | |
O4 | 0.11981 (11) | 0.13075 (4) | 0.40253 (18) | 0.01627 (16) | |
O3 | 0.43511 (11) | 0.15424 (4) | 0.37913 (17) | 0.01333 (15) | |
O2 | 0.26847 (13) | 0.17443 (4) | 0.75465 (15) | 0.01790 (17) | |
H210 | 0.2358 | 0.1403 | 0.8041 | 0.021* | 0.50 |
C3 | 0.49629 (14) | 0.09467 (5) | 0.4429 (2) | 0.01345 (19) | |
H32 | 0.4341 | 0.0631 | 0.3528 | 0.016* | |
H31 | 0.4776 | 0.0873 | 0.6133 | 0.016* | |
C2 | 0.68536 (14) | 0.09175 (5) | 0.3864 (2) | 0.01103 (17) | |
H2 | 0.7278 | 0.0502 | 0.4277 | 0.013* | |
C1 | 0.72061 (15) | 0.10307 (5) | 0.1213 (2) | 0.01375 (19) | |
O5 | 0.77599 (12) | 0.15424 (4) | 0.06262 (16) | 0.01742 (17) | |
O6 | 0.68900 (16) | 0.05995 (4) | −0.01633 (19) | 0.0278 (2) | |
N1 | 0.77944 (12) | 0.13696 (4) | 0.53223 (18) | 0.01365 (17) | |
H11 | 0.7366 | 0.1748 | 0.5052 | 0.016* | |
H12 | 0.8918 | 0.1362 | 0.4930 | 0.016* | |
H13 | 0.7674 | 0.1275 | 0.6877 | 0.016* | |
N2 | 0.51025 (16) | 0.24943 (5) | −0.0098 (3) | 0.0222 (2) | |
H21 | 0.548 (2) | 0.2351 (7) | 0.1305 (15) | 0.027* | |
H22 | 0.4386 (15) | 0.2203 (5) | −0.070 (3) | 0.027* | |
H23 | 0.5947 (15) | 0.2543 (6) | −0.118 (2) | 0.027* | |
H24 | 0.4453 (16) | 0.2835 (4) | 0.004 (3) | 0.027* | |
O7 | 0.1456 (11) | 0.0819 (4) | −0.0527 (12) | 0.0220 (11) | 0.50 |
H71 | 0.103 (5) | 0.1026 (16) | 0.052 (5) | 0.026* | 0.50 |
H72 | 0.225 (4) | 0.0583 (14) | −0.034 (8) | 0.026* | 0.50 |
N7 | 0.1303 (11) | 0.0747 (4) | −0.0145 (13) | 0.0164 (8) | 0.50 |
H17 | 0.122 (4) | 0.0901 (12) | 0.135 (2) | 0.020* | 0.50 |
H27 | 0.202 (3) | 0.0420 (8) | −0.015 (5) | 0.020* | 0.50 |
H37 | 0.173 (3) | 0.1047 (9) | −0.109 (4) | 0.020* | 0.50 |
H47 | 0.0248 (18) | 0.0636 (11) | −0.066 (5) | 0.020* | 0.50 |
O81 | 0.3962 (6) | −0.0050 (2) | −0.039 (4) | 0.0316 (17) | 0.60 (5) |
O82 | 0.4008 (11) | −0.0087 (4) | 0.035 (3) | 0.0225 (15) | 0.40 (5) |
H82 | 0.4910 (10) | 0.0075 (8) | −0.003 (3) | 0.027* | |
H81 | 0.406 (3) | −0.0421 (2) | −0.029 (3) | 0.027* |
U11 | U22 | U33 | U12 | U13 | U23 | |
P1 | 0.00983 (10) | 0.01262 (10) | 0.01287 (11) | 0.00100 (9) | 0.00037 (11) | −0.00042 (9) |
O1 | 0.0167 (4) | 0.0140 (3) | 0.0212 (4) | 0.0031 (3) | 0.0000 (4) | 0.0028 (3) |
O4 | 0.0106 (3) | 0.0167 (4) | 0.0214 (4) | −0.0004 (3) | 0.0026 (3) | −0.0024 (3) |
O3 | 0.0097 (3) | 0.0139 (3) | 0.0164 (4) | 0.0027 (3) | 0.0023 (3) | 0.0025 (3) |
O2 | 0.0228 (4) | 0.0186 (4) | 0.0123 (3) | 0.0000 (4) | 0.0031 (3) | −0.0001 (3) |
C3 | 0.0100 (4) | 0.0137 (4) | 0.0166 (5) | 0.0000 (3) | 0.0011 (3) | 0.0023 (4) |
C2 | 0.0111 (4) | 0.0113 (4) | 0.0107 (4) | 0.0002 (3) | 0.0006 (4) | 0.0011 (4) |
C1 | 0.0134 (5) | 0.0153 (4) | 0.0125 (4) | 0.0015 (3) | 0.0015 (4) | 0.0008 (4) |
O5 | 0.0181 (4) | 0.0178 (4) | 0.0164 (4) | −0.0023 (3) | 0.0019 (3) | 0.0053 (3) |
O6 | 0.0461 (6) | 0.0222 (4) | 0.0151 (4) | −0.0057 (4) | 0.0033 (4) | −0.0059 (4) |
N1 | 0.0115 (4) | 0.0166 (4) | 0.0129 (4) | −0.0005 (3) | 0.0001 (3) | −0.0013 (3) |
N2 | 0.0224 (5) | 0.0194 (4) | 0.0248 (5) | 0.0085 (4) | 0.0084 (4) | 0.0063 (4) |
O7 | 0.0252 (17) | 0.028 (2) | 0.013 (2) | −0.0020 (14) | 0.0056 (14) | −0.0024 (14) |
N7 | 0.0202 (17) | 0.0172 (14) | 0.012 (2) | 0.0000 (12) | 0.0034 (15) | 0.0006 (14) |
O81 | 0.0376 (15) | 0.0156 (11) | 0.042 (5) | −0.0038 (9) | −0.0052 (16) | −0.0098 (13) |
O82 | 0.029 (2) | 0.0188 (14) | 0.020 (3) | −0.0022 (12) | −0.0007 (17) | −0.0050 (17) |
P1—O1 | 1.4956 (9) | N2—H23 | 0.908 (3) |
P1—O4 | 1.5190 (10) | N2—H24 | 0.909 (3) |
P1—O2 | 1.5432 (10) | O7—H71 | 0.820 (2) |
P1—O3 | 1.6216 (10) | O7—H72 | 0.820 (2) |
O3—C3 | 1.4404 (14) | O7—H17 | 1.094 (15) |
O2—H210 | 0.8400 | O7—H27 | 1.004 (17) |
C3—C2 | 1.5199 (17) | O7—H37 | 0.631 (12) |
C3—H32 | 0.9900 | O7—H47 | 1.033 (17) |
C3—H31 | 0.9900 | N7—H71 | 0.75 (2) |
C2—N1 | 1.4885 (15) | N7—H72 | 0.84 (2) |
C2—C1 | 1.5473 (17) | N7—H17 | 0.913 (3) |
C2—H2 | 1.0000 | N7—H27 | 0.911 (3) |
C1—O5 | 1.2507 (14) | N7—H37 | 0.913 (3) |
C1—O6 | 1.2521 (15) | N7—H47 | 0.911 (3) |
N1—H11 | 0.9100 | O81—H82 | 0.819 (2) |
N1—H12 | 0.9100 | O81—H81 | 0.821 (2) |
N1—H13 | 0.9100 | O82—H82 | 0.820 (2) |
N2—H21 | 0.906 (3) | O82—H81 | 0.819 (2) |
N2—H22 | 0.918 (3) | ||
O1—P1—O4 | 115.74 (6) | H23—N2—H24 | 111.8 (9) |
O1—P1—O2 | 112.79 (5) | H71—O7—H72 | 125 (5) |
O4—P1—O2 | 109.63 (6) | H71—O7—H17 | 30 (3) |
O1—P1—O3 | 104.01 (5) | H72—O7—H17 | 96 (4) |
O4—P1—O3 | 107.42 (5) | H71—O7—H27 | 121 (3) |
O2—P1—O3 | 106.54 (6) | H72—O7—H27 | 24 (3) |
C3—O3—P1 | 118.39 (7) | H17—O7—H27 | 90.6 (13) |
P1—O2—H210 | 109.5 | H71—O7—H37 | 94 (4) |
O3—C3—C2 | 108.13 (9) | H72—O7—H37 | 108 (4) |
O3—C3—H32 | 110.1 | H17—O7—H37 | 115 (2) |
C2—C3—H32 | 110.1 | H27—O7—H37 | 131 (2) |
O3—C3—H31 | 110.1 | H71—O7—H47 | 84 (4) |
C2—C3—H31 | 110.1 | H72—O7—H47 | 118 (3) |
H32—C3—H31 | 108.4 | H17—O7—H47 | 88.7 (12) |
N1—C2—C3 | 109.85 (9) | H27—O7—H47 | 94.5 (15) |
N1—C2—C1 | 110.05 (9) | H37—O7—H47 | 125 (3) |
C3—C2—C1 | 111.86 (9) | H71—N7—H72 | 133 (5) |
N1—C2—H2 | 108.3 | H71—N7—H17 | 38 (3) |
C3—C2—H2 | 108.3 | H72—N7—H17 | 110 (4) |
C1—C2—H2 | 108.3 | H71—N7—H27 | 145 (4) |
O5—C1—O6 | 125.72 (12) | H72—N7—H27 | 27 (3) |
O5—C1—C2 | 117.70 (10) | H17—N7—H27 | 109.8 (10) |
O6—C1—C2 | 116.58 (10) | H71—N7—H37 | 79 (3) |
C2—N1—H11 | 109.5 | H72—N7—H37 | 85 (3) |
C2—N1—H12 | 109.5 | H17—N7—H37 | 107.8 (10) |
H11—N1—H12 | 109.5 | H27—N7—H37 | 110.0 (10) |
C2—N1—H13 | 109.5 | H71—N7—H47 | 97 (4) |
H11—N1—H13 | 109.5 | H72—N7—H47 | 131 (3) |
H12—N1—H13 | 109.5 | H17—N7—H47 | 109.2 (10) |
H21—N2—H22 | 106.5 (9) | H27—N7—H47 | 110.3 (10) |
H21—N2—H23 | 113.1 (9) | H37—N7—H47 | 109.6 (10) |
H22—N2—H23 | 106.2 (9) | H82—O81—H81 | 103.3 (18) |
H21—N2—H24 | 113.2 (9) | H82—O82—H81 | 103.4 (18) |
H22—N2—H24 | 105.2 (9) | ||
O1—P1—O3—C3 | 178.20 (8) | O3—C3—C2—C1 | −59.65 (12) |
O4—P1—O3—C3 | −58.60 (10) | N1—C2—C1—O5 | −19.43 (14) |
O2—P1—O3—C3 | 58.82 (9) | C3—C2—C1—O5 | 102.97 (12) |
P1—O3—C3—C2 | −163.73 (8) | N1—C2—C1—O6 | 161.34 (11) |
O3—C3—C2—N1 | 62.87 (12) | C3—C2—C1—O6 | −76.26 (13) |
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H210···O7i | 0.84 | 1.68 | 2.501 (6) | 167 |
O2—H210···N7i | 0.84 | 1.95 | 2.773 (7) | 164 |
N1—H11···O1ii | 0.91 | 1.97 | 2.7725 (14) | 146 |
N1—H12···O4iii | 0.91 | 1.87 | 2.7749 (16) | 177 |
N1—H13···O5i | 0.91 | 2.21 | 3.0292 (17) | 150 |
N1—H13···O6i | 0.91 | 2.32 | 3.1482 (17) | 151 |
N2—H21···O3 | 0.91 (1) | 2.43 (1) | 3.0953 (17) | 130 (1) |
N2—H21···O5 | 0.91 (1) | 2.55 (2) | 2.9828 (16) | 110 (1) |
N2—H22···O2iv | 0.92 (1) | 1.95 (1) | 2.8462 (19) | 166 (2) |
N2—H23···O1v | 0.91 (1) | 1.89 (1) | 2.7835 (18) | 168 (2) |
N2—H24···O5vi | 0.91 (1) | 1.95 (1) | 2.8202 (15) | 161 (2) |
O7—H71···O4 | 0.82 (1) | 2.08 (2) | 2.801 (8) | 146 (4) |
O7—H71···O4 | 0.82 (1) | 2.08 (2) | 2.801 (8) | 146 (4) |
O7—H72···O81 | 0.82 (1) | 1.93 (1) | 2.744 (10) | 170 (4) |
O7—H72···O82 | 0.82 (1) | 2.05 (2) | 2.868 (15) | 172 (4) |
N7—H17···O4 | 0.91 (1) | 1.76 (1) | 2.666 (9) | 170 (3) |
N7—H17···O81vii | 0.91 (1) | 2.63 (3) | 3.106 (18) | 113 (2) |
N7—H27···O81 | 0.91 (1) | 1.85 (1) | 2.729 (10) | 162 (2) |
N7—H27···O82 | 0.91 (1) | 1.94 (2) | 2.819 (15) | 161 (2) |
N7—H37···O2iv | 0.91 (1) | 1.87 (1) | 2.773 (7) | 168 (3) |
N7—H47···O6viii | 0.91 (1) | 2.65 (2) | 3.480 (9) | 151 (2) |
O81—H82···O6 | 0.82 (1) | 1.94 (1) | 2.709 (5) | 157 (2) |
O82—H81···O4ix | 0.82 (1) | 2.00 (1) | 2.790 (6) | 163 (2) |
O81—H81···O4ix | 0.82 (1) | 2.00 (1) | 2.786 (4) | 161 (2) |
O82—H82···O6 | 0.82 (1) | 1.94 (1) | 2.734 (6) | 164 (2) |
Symmetry codes: (i) x, y, z+1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1, y, z; (iv) x, y, z−1; (v) x+1/2, −y+1/2, −z; (vi) x−1/2, −y+1/2, −z; (vii) −x+1/2, −y, z+1/2; (viii) x−1, y, z; (ix) −x+1/2, −y, z−1/2. |
C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | Z = 4 |
Mr = 475.30 | F(000) = 1008 |
Monoclinic, P21 | Dx = 1.610 Mg m−3 |
Hall symbol: P 2yb | Mo Kα radiation, λ = 0.71073 Å |
a = 7.851 (2) Å | Cell parameters from 17710 reflections |
b = 22.048 (4) Å | µ = 0.31 mm−1 |
c = 11.325 (3) Å | T = 50 K |
β = 90.04 (2)° | Plates, colourless |
V = 1960.3 (8) Å3 | 0.40 × 0.18 × 0.10 mm |
KM4CCD diffractometer | 16153 independent reflections |
Radiation source: fine-focus sealed tube | 9474 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
/w scans | θmax = 38.6°, θmin = 4.5° |
Absorption correction: numerical ? | h = −13→13 |
Tmin = 0.889, Tmax = 0.966 | k = −38→28 |
49468 measured reflections | l = −19→19 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.045 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.107 | w = 1/[σ2(Fo2) + (0.043P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
16153 reflections | Δρmax = 0.41 e Å−3 |
595 parameters | Δρmin = −0.46 e Å−3 |
37 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.06 (5) |
C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | V = 1960.3 (8) Å3 |
Mr = 475.30 | Z = 4 |
Monoclinic, P21 | Mo Kα radiation |
a = 7.851 (2) Å | µ = 0.31 mm−1 |
b = 22.048 (4) Å | T = 50 K |
c = 11.325 (3) Å | 0.40 × 0.18 × 0.10 mm |
β = 90.04 (2)° |
KM4CCD diffractometer | 16153 independent reflections |
Absorption correction: numerical ? | 9474 reflections with I > 2σ(I) |
Tmin = 0.889, Tmax = 0.966 | Rint = 0.034 |
49468 measured reflections |
R[F2 > 2σ(F2)] = 0.045 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.107 | Δρmax = 0.41 e Å−3 |
S = 1.00 | Δρmin = −0.46 e Å−3 |
16153 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
595 parameters | Absolute structure parameter: 0.06 (5) |
37 restraints |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
P1 | 0.25609 (6) | 0.06010 (2) | 0.13293 (4) | 0.01366 (13) | |
O11 | 0.6982 (2) | 0.17955 (7) | 0.38192 (14) | 0.0302 (4) | |
O21 | 0.27285 (19) | 0.06164 (6) | −0.00391 (12) | 0.0207 (3) | |
H210 | 0.2385 | 0.0953 | −0.0293 | 0.025* | |
O31 | 0.77807 (19) | 0.08502 (7) | 0.34397 (12) | 0.0218 (3) | |
O41 | 0.43774 (15) | 0.08227 (6) | 0.18382 (11) | 0.0147 (3) | |
O51 | 0.12235 (16) | 0.10552 (6) | 0.17156 (12) | 0.0190 (3) | |
O61 | 0.23734 (18) | −0.00322 (7) | 0.17718 (13) | 0.0220 (3) | |
N1 | 0.78058 (14) | 0.10152 (5) | 0.10860 (9) | 0.0147 (3) | |
H1N1 | 0.8934 | 0.1033 | 0.1267 | 0.018* | |
H2N1 | 0.7657 | 0.1103 | 0.0308 | 0.018* | |
H3N1 | 0.7405 | 0.0636 | 0.1237 | 0.018* | |
C11 | 0.72357 (19) | 0.13587 (6) | 0.31376 (9) | 0.0138 (4) | |
C21 | 0.68601 (14) | 0.14629 (5) | 0.18155 (9) | 0.0140 (3) | |
H21 | 0.7265 | 0.1878 | 0.1599 | 0.017* | |
C31 | 0.4968 (2) | 0.14215 (8) | 0.15308 (17) | 0.0135 (3) | |
H311 | 0.4331 | 0.1731 | 0.1986 | 0.016* | |
H312 | 0.4779 | 0.1497 | 0.0679 | 0.016* | |
P2 | 1.24039 (6) | 0.41536 (2) | −0.11844 (4) | 0.01388 (10) | |
O12 | 0.71960 (18) | 0.39284 (7) | 0.09156 (13) | 0.0223 (3) | |
O22 | 1.22080 (18) | 0.41408 (7) | −0.25539 (11) | 0.0215 (3) | |
H220 | 1.2661 | 0.3824 | −0.2822 | 0.026* | |
O32 | 0.7964 (2) | 0.29850 (7) | 0.13238 (13) | 0.0288 (4) | |
O42 | 1.05951 (16) | 0.39289 (6) | −0.06618 (11) | 0.0158 (3) | |
O52 | 1.25948 (18) | 0.47864 (7) | −0.07454 (13) | 0.0215 (3) | |
O62 | 1.37431 (16) | 0.36991 (6) | −0.08194 (12) | 0.0185 (3) | |
N2 | 0.71658 (14) | 0.37373 (5) | −0.14386 (9) | 0.0173 (3) | |
H1N2 | 0.6038 | 0.3724 | −0.1257 | 0.021* | |
H2N2 | 0.7311 | 0.3641 | −0.2213 | 0.021* | |
H3N2 | 0.7573 | 0.4117 | −0.1304 | 0.021* | |
C12 | 0.77253 (19) | 0.34155 (6) | 0.06248 (9) | 0.0146 (4) | |
C22 | 0.81069 (14) | 0.32955 (5) | −0.06905 (9) | 0.0134 (3) | |
H22 | 0.7697 | 0.2878 | −0.0890 | 0.016* | |
C32 | 0.9997 (2) | 0.33290 (8) | −0.09620 (17) | 0.0157 (4) | |
H321 | 1.0621 | 0.3021 | −0.0496 | 0.019* | |
H322 | 1.0195 | 0.3248 | −0.1811 | 0.019* | |
P3 | 1.25126 (6) | 0.41504 (2) | 0.38337 (4) | 0.01188 (9) | |
O13 | 0.8248 (2) | 0.30011 (7) | 0.63169 (13) | 0.0283 (4) | |
O23 | 0.72675 (18) | 0.39283 (7) | 0.59489 (13) | 0.0207 (3) | |
O33 | 1.06849 (15) | 0.39329 (6) | 0.43461 (11) | 0.0141 (3) | |
O43 | 1.27159 (17) | 0.47775 (6) | 0.43286 (12) | 0.0187 (3) | |
O53 | 1.23921 (17) | 0.41260 (6) | 0.24901 (11) | 0.0181 (3) | |
O63 | 1.38336 (16) | 0.36959 (6) | 0.42710 (12) | 0.0165 (3) | |
N3 | 0.72237 (14) | 0.37863 (5) | 0.36012 (9) | 0.0132 (3) | |
H1N3 | 0.6100 | 0.3776 | 0.3797 | 0.016* | |
H2N3 | 0.7343 | 0.3705 | 0.2818 | 0.016* | |
H3N3 | 0.7654 | 0.4161 | 0.3760 | 0.016* | |
C13 | 0.7852 (2) | 0.34277 (6) | 0.56449 (9) | 0.0153 (4) | |
C23 | 0.81649 (14) | 0.33219 (5) | 0.43038 (9) | 0.0119 (3) | |
H23 | 0.7723 | 0.2911 | 0.4088 | 0.014* | |
C33 | 1.0045 (2) | 0.33495 (8) | 0.40037 (16) | 0.0130 (3) | |
H331 | 1.0667 | 0.3026 | 0.4429 | 0.016* | |
H332 | 1.0209 | 0.3288 | 0.3145 | 0.016* | |
P4 | 0.25079 (6) | 0.06478 (2) | 0.63489 (4) | 0.01245 (12) | |
O14 | 0.77411 (18) | 0.08547 (6) | 0.84654 (13) | 0.0203 (3) | |
O24 | 0.6782 (2) | 0.17819 (7) | 0.88453 (14) | 0.0291 (4) | |
O34 | 0.43284 (16) | 0.08710 (6) | 0.68730 (12) | 0.0153 (3) | |
O44 | 0.23112 (17) | 0.00194 (6) | 0.68424 (12) | 0.0185 (3) | |
O54 | 0.11787 (16) | 0.10995 (6) | 0.67745 (13) | 0.0177 (3) | |
O64 | 0.26401 (17) | 0.06688 (6) | 0.50049 (12) | 0.0185 (3) | |
N4 | 0.77886 (14) | 0.10160 (5) | 0.61220 (9) | 0.0158 (3) | |
H1N4 | 0.8913 | 0.1028 | 0.6315 | 0.019* | |
H2N4 | 0.7662 | 0.1100 | 0.5340 | 0.019* | |
H3N4 | 0.7366 | 0.0640 | 0.6278 | 0.019* | |
C14 | 0.7169 (2) | 0.13577 (6) | 0.81589 (9) | 0.0168 (4) | |
C24 | 0.68536 (14) | 0.14714 (5) | 0.68255 (9) | 0.0119 (3) | |
H24 | 0.7302 | 0.1883 | 0.6621 | 0.014* | |
C34 | 0.4979 (2) | 0.14543 (9) | 0.65378 (17) | 0.0152 (4) | |
H341 | 0.4374 | 0.1778 | 0.6974 | 0.018* | |
H342 | 0.4804 | 0.1521 | 0.5682 | 0.018* | |
N11 | −0.0015 (2) | 0.48591 (9) | 0.13581 (18) | 0.0195 (4) | |
H11N | −0.080 (2) | 0.4905 (10) | 0.1944 (14) | 0.023* | |
H21N | 0.062 (3) | 0.5203 (6) | 0.129 (2) | 0.023* | |
H31N | −0.048 (3) | 0.4697 (9) | 0.0695 (12) | 0.023* | |
H41N | 0.077 (2) | 0.4576 (8) | 0.158 (2) | 0.023* | |
N21 | 0.4801 (2) | 0.48698 (9) | 0.12487 (19) | 0.0220 (4) | |
H12N | 0.565 (2) | 0.4614 (9) | 0.102 (2) | 0.026* | |
H22N | 0.430 (3) | 0.4916 (11) | 0.0531 (10) | 0.026* | |
H32N | 0.518 (3) | 0.5239 (5) | 0.149 (2) | 0.026* | |
H42N | 0.415 (2) | 0.4676 (9) | 0.1798 (15) | 0.026* | |
N31 | −0.0200 (2) | 0.49163 (9) | 0.62233 (18) | 0.0211 (4) | |
H13N | −0.082 (2) | 0.5161 (9) | 0.5740 (17) | 0.025* | |
H23N | 0.061 (2) | 0.5182 (8) | 0.647 (2) | 0.025* | |
H33N | −0.079 (3) | 0.4811 (10) | 0.6883 (12) | 0.025* | |
H43N | 0.005 (3) | 0.4578 (6) | 0.5797 (18) | 0.025* | |
N41 | 0.4994 (2) | 0.49171 (9) | 0.61314 (17) | 0.0192 (4) | |
H14N | 0.577 (2) | 0.4613 (7) | 0.622 (2) | 0.023* | |
H24N | 0.4089 (18) | 0.4878 (10) | 0.5635 (16) | 0.023* | |
H34N | 0.574 (2) | 0.5192 (8) | 0.5827 (19) | 0.023* | |
H44N | 0.472 (3) | 0.5064 (10) | 0.6856 (9) | 0.023* | |
N51 | 0.1380 (3) | 0.16459 (9) | 0.38522 (17) | 0.0224 (4) | |
H15N | 0.139 (3) | 0.1543 (11) | 0.3074 (6) | 0.027* | |
H25N | 0.0326 (13) | 0.1813 (10) | 0.393 (2) | 0.027* | |
H35N | 0.215 (2) | 0.1953 (8) | 0.379 (2) | 0.027* | |
H45N | 0.194 (3) | 0.1342 (7) | 0.4233 (18) | 0.027* | |
N61 | 0.3626 (3) | 0.31381 (9) | 0.13602 (17) | 0.0233 (4) | |
H16N | 0.375 (3) | 0.3350 (9) | 0.0676 (11) | 0.028* | |
H26N | 0.4674 (13) | 0.2986 (10) | 0.154 (2) | 0.028* | |
H36N | 0.289 (2) | 0.2820 (7) | 0.132 (2) | 0.028* | |
H46N | 0.361 (3) | 0.3493 (6) | 0.1771 (18) | 0.028* | |
O1W | 0.1410 (2) | 0.15627 (8) | 0.90080 (16) | 0.0325 (4) | |
H101 | 0.123 (4) | 0.1411 (11) | 0.8359 (11) | 0.039* | |
H102 | 0.210 (3) | 0.1841 (9) | 0.894 (3) | 0.039* | |
O2W | 0.3523 (2) | 0.32023 (8) | 0.64681 (15) | 0.0328 (4) | |
H201 | 0.374 (4) | 0.3400 (11) | 0.5873 (14) | 0.039* | |
H202 | 0.279 (3) | 0.2939 (9) | 0.641 (3) | 0.039* | |
O3W | 0.3889 (3) | 0.24283 (8) | 0.89539 (19) | 0.0414 (5) | |
H301 | 0.471 (2) | 0.2218 (11) | 0.878 (3) | 0.050* | |
H302 | 0.379 (4) | 0.2787 (4) | 0.878 (3) | 0.050* | |
O4W | 0.4074 (2) | 0.24856 (8) | 0.36458 (17) | 0.0350 (4) | |
H401 | 0.5020 (16) | 0.2336 (12) | 0.374 (2) | 0.042* | |
H402 | 0.403 (4) | 0.2855 (2) | 0.373 (3) | 0.042* | |
O5W | 0.1097 (2) | 0.23170 (8) | 0.61561 (18) | 0.0364 (4) | |
H501 | 0.0152 (17) | 0.2474 (12) | 0.619 (3) | 0.044* | |
H502 | 0.095 (4) | 0.1953 (3) | 0.626 (3) | 0.044* | |
O6W | 0.0892 (2) | 0.23225 (8) | 0.14290 (19) | 0.0393 (4) | |
H601 | 0.004 (2) | 0.2528 (12) | 0.130 (3) | 0.047* | |
H602 | 0.095 (4) | 0.2095 (11) | 0.0859 (17) | 0.047* |
U11 | U22 | U33 | U12 | U13 | U23 | |
P1 | 0.0104 (2) | 0.0162 (3) | 0.0144 (2) | −0.00129 (18) | 0.00069 (18) | −0.0028 (2) |
O11 | 0.0452 (10) | 0.0267 (8) | 0.0188 (8) | 0.0056 (8) | −0.0035 (7) | −0.0086 (6) |
O21 | 0.0262 (7) | 0.0217 (8) | 0.0142 (7) | 0.0028 (6) | −0.0006 (5) | −0.0030 (6) |
O31 | 0.0253 (8) | 0.0266 (8) | 0.0134 (7) | 0.0059 (6) | −0.0013 (6) | 0.0084 (6) |
O41 | 0.0102 (6) | 0.0148 (7) | 0.0192 (7) | −0.0031 (5) | −0.0021 (5) | 0.0032 (5) |
O51 | 0.0126 (6) | 0.0255 (8) | 0.0190 (7) | 0.0018 (6) | −0.0016 (5) | −0.0060 (6) |
O61 | 0.0218 (7) | 0.0202 (8) | 0.0242 (8) | −0.0046 (6) | 0.0018 (6) | 0.0017 (6) |
N1 | 0.0117 (7) | 0.0196 (8) | 0.0126 (8) | −0.0012 (6) | −0.0003 (6) | −0.0012 (6) |
C11 | 0.0120 (8) | 0.0165 (9) | 0.0128 (9) | 0.0001 (7) | −0.0010 (7) | 0.0005 (7) |
C21 | 0.0135 (8) | 0.0136 (8) | 0.0149 (9) | 0.0003 (7) | 0.0005 (7) | 0.0003 (7) |
C31 | 0.0115 (8) | 0.0125 (8) | 0.0164 (9) | −0.0005 (7) | −0.0009 (7) | 0.0002 (7) |
P2 | 0.0114 (2) | 0.0160 (2) | 0.0143 (2) | −0.0012 (2) | 0.00011 (17) | 0.0018 (2) |
O12 | 0.0244 (7) | 0.0247 (8) | 0.0178 (7) | 0.0059 (6) | 0.0028 (6) | −0.0065 (6) |
O22 | 0.0279 (7) | 0.0234 (7) | 0.0133 (7) | 0.0052 (7) | 0.0020 (5) | 0.0029 (6) |
O32 | 0.0443 (10) | 0.0250 (8) | 0.0171 (7) | 0.0021 (8) | 0.0032 (7) | 0.0076 (6) |
O42 | 0.0124 (6) | 0.0163 (6) | 0.0185 (7) | −0.0036 (5) | 0.0026 (5) | −0.0045 (5) |
O52 | 0.0226 (7) | 0.0166 (7) | 0.0255 (8) | −0.0052 (6) | −0.0002 (6) | −0.0009 (6) |
O62 | 0.0126 (6) | 0.0218 (7) | 0.0210 (7) | 0.0014 (5) | 0.0015 (5) | 0.0041 (6) |
N2 | 0.0132 (7) | 0.0234 (9) | 0.0154 (8) | 0.0002 (7) | 0.0018 (6) | 0.0030 (7) |
C12 | 0.0113 (8) | 0.0182 (9) | 0.0144 (9) | 0.0009 (7) | 0.0005 (7) | −0.0009 (7) |
C22 | 0.0123 (8) | 0.0138 (8) | 0.0141 (8) | 0.0007 (7) | 0.0012 (7) | −0.0007 (7) |
C32 | 0.0129 (8) | 0.0159 (9) | 0.0185 (9) | −0.0016 (7) | 0.0037 (7) | −0.0030 (7) |
P3 | 0.00928 (19) | 0.0117 (2) | 0.0147 (2) | −0.0004 (2) | 0.00048 (17) | 0.00040 (19) |
O13 | 0.0370 (9) | 0.0289 (9) | 0.0189 (8) | 0.0055 (8) | 0.0019 (7) | 0.0075 (6) |
O23 | 0.0209 (7) | 0.0228 (7) | 0.0184 (7) | 0.0013 (6) | 0.0008 (6) | −0.0062 (6) |
O33 | 0.0085 (5) | 0.0136 (6) | 0.0201 (7) | −0.0017 (5) | 0.0023 (5) | −0.0021 (5) |
O43 | 0.0170 (6) | 0.0150 (6) | 0.0240 (8) | −0.0025 (5) | −0.0041 (5) | −0.0024 (6) |
O53 | 0.0210 (6) | 0.0196 (7) | 0.0136 (6) | −0.0009 (6) | 0.0025 (5) | −0.0001 (6) |
O63 | 0.0112 (6) | 0.0152 (6) | 0.0230 (7) | 0.0001 (5) | 0.0000 (5) | 0.0026 (6) |
N3 | 0.0125 (7) | 0.0158 (8) | 0.0115 (7) | −0.0011 (6) | −0.0018 (6) | 0.0008 (6) |
C13 | 0.0134 (8) | 0.0193 (9) | 0.0131 (9) | −0.0032 (7) | 0.0016 (7) | −0.0017 (7) |
C23 | 0.0118 (7) | 0.0126 (8) | 0.0112 (8) | −0.0015 (6) | 0.0012 (6) | −0.0018 (7) |
C33 | 0.0102 (8) | 0.0116 (8) | 0.0172 (9) | 0.0009 (6) | 0.0012 (7) | −0.0026 (7) |
P4 | 0.0102 (2) | 0.0118 (3) | 0.0154 (2) | 0.00040 (18) | −0.00067 (18) | 0.00050 (19) |
O14 | 0.0199 (7) | 0.0183 (7) | 0.0227 (7) | 0.0025 (6) | −0.0019 (6) | 0.0048 (6) |
O24 | 0.0402 (10) | 0.0294 (9) | 0.0177 (8) | 0.0066 (8) | −0.0024 (7) | −0.0080 (6) |
O34 | 0.0123 (6) | 0.0151 (6) | 0.0186 (7) | −0.0016 (5) | −0.0026 (5) | 0.0028 (5) |
O44 | 0.0178 (6) | 0.0131 (6) | 0.0245 (8) | −0.0035 (5) | 0.0025 (6) | 0.0004 (6) |
O54 | 0.0104 (6) | 0.0164 (6) | 0.0264 (8) | 0.0017 (5) | −0.0005 (5) | −0.0015 (6) |
O64 | 0.0212 (7) | 0.0196 (7) | 0.0145 (7) | 0.0010 (6) | −0.0037 (5) | −0.0011 (6) |
N4 | 0.0130 (7) | 0.0193 (8) | 0.0150 (8) | −0.0021 (6) | 0.0004 (6) | −0.0011 (6) |
C14 | 0.0136 (8) | 0.0240 (10) | 0.0129 (9) | −0.0055 (8) | −0.0019 (7) | 0.0003 (8) |
C24 | 0.0118 (7) | 0.0115 (8) | 0.0125 (8) | −0.0031 (6) | −0.0019 (6) | 0.0025 (7) |
C34 | 0.0116 (8) | 0.0151 (9) | 0.0188 (9) | −0.0007 (7) | −0.0023 (7) | 0.0056 (7) |
N11 | 0.0170 (8) | 0.0207 (9) | 0.0208 (9) | −0.0016 (7) | 0.0014 (6) | −0.0025 (7) |
N21 | 0.0202 (9) | 0.0184 (9) | 0.0275 (9) | 0.0008 (8) | −0.0009 (7) | −0.0007 (8) |
N31 | 0.0204 (9) | 0.0182 (9) | 0.0246 (9) | −0.0055 (7) | 0.0025 (7) | −0.0010 (7) |
N41 | 0.0178 (8) | 0.0189 (9) | 0.0209 (9) | 0.0057 (7) | −0.0031 (7) | −0.0026 (7) |
N51 | 0.0281 (10) | 0.0196 (9) | 0.0197 (9) | 0.0002 (8) | 0.0035 (8) | −0.0019 (7) |
N61 | 0.0281 (10) | 0.0203 (10) | 0.0214 (9) | 0.0006 (8) | −0.0023 (8) | 0.0025 (7) |
O1W | 0.0363 (10) | 0.0327 (10) | 0.0286 (9) | −0.0077 (8) | −0.0007 (8) | −0.0078 (8) |
O2W | 0.0403 (10) | 0.0333 (10) | 0.0248 (9) | −0.0036 (8) | 0.0005 (8) | 0.0063 (8) |
O3W | 0.0393 (11) | 0.0224 (9) | 0.0626 (13) | 0.0084 (8) | 0.0019 (10) | −0.0081 (9) |
O4W | 0.0361 (10) | 0.0180 (8) | 0.0510 (11) | 0.0033 (8) | −0.0021 (9) | −0.0085 (8) |
O5W | 0.0327 (10) | 0.0226 (8) | 0.0539 (12) | 0.0054 (8) | 0.0056 (9) | 0.0116 (9) |
O6W | 0.0352 (10) | 0.0209 (9) | 0.0617 (13) | 0.0027 (8) | −0.0015 (10) | 0.0076 (9) |
P1—O61 | 1.4907 (16) | P4—O54 | 1.5212 (14) |
P1—O51 | 1.5156 (15) | P4—O64 | 1.5263 (15) |
P1—O21 | 1.5557 (15) | P4—O34 | 1.6237 (14) |
P1—O41 | 1.6137 (14) | O14—C14 | 1.2456 (17) |
O11—C11 | 1.2502 (18) | O24—C14 | 1.2536 (18) |
O21—H210 | 0.8400 | O34—C34 | 1.435 (2) |
O31—C11 | 1.2478 (17) | N4—C24 | 1.4773 |
O41—C31 | 1.442 (2) | N4—H1N4 | 0.9100 |
N1—C21 | 1.4863 | N4—H2N4 | 0.9100 |
N1—H1N1 | 0.9100 | N4—H3N4 | 0.9100 |
N1—H2N1 | 0.9100 | C14—C24 | 1.5506 |
N1—H3N1 | 0.9100 | C24—C34 | 1.507 (2) |
C11—C21 | 1.5430 | C24—H24 | 1.0000 |
C21—C31 | 1.523 (2) | C34—H341 | 0.9900 |
C21—H21 | 1.0000 | C34—H342 | 0.9900 |
C31—H311 | 0.9900 | N11—H11N | 0.911 (3) |
C31—H312 | 0.9900 | N11—H21N | 0.909 (3) |
P2—O52 | 1.4885 (16) | N11—H31N | 0.908 (3) |
P2—O62 | 1.5100 (15) | N11—H41N | 0.909 (3) |
P2—O22 | 1.5587 (15) | N21—H12N | 0.910 (3) |
P2—O42 | 1.6167 (14) | N21—H22N | 0.910 (3) |
O12—C12 | 1.2492 (18) | N21—H32N | 0.909 (3) |
O22—H220 | 0.8400 | N21—H42N | 0.911 (3) |
O32—C12 | 1.2498 (18) | N31—H13N | 0.910 (3) |
O42—C32 | 1.444 (2) | N31—H23N | 0.909 (3) |
N2—C22 | 1.4872 | N31—H33N | 0.909 (3) |
N2—H1N2 | 0.9100 | N31—H43N | 0.909 (3) |
N2—H2N2 | 0.9100 | N41—H14N | 0.909 (3) |
N2—H3N2 | 0.9100 | N41—H24N | 0.910 (3) |
C12—C22 | 1.5425 | N41—H34N | 0.911 (3) |
C22—C32 | 1.517 (2) | N41—H44N | 0.908 (3) |
C22—H22 | 1.0000 | N51—H15N | 0.910 (3) |
C32—H321 | 0.9900 | N51—H25N | 0.910 (3) |
C32—H322 | 0.9900 | N51—H35N | 0.910 (3) |
P3—O43 | 1.5003 (15) | N51—H45N | 0.910 (3) |
P3—O63 | 1.5246 (14) | N61—H16N | 0.909 (3) |
P3—O53 | 1.5255 (15) | N61—H26N | 0.910 (3) |
P3—O33 | 1.6208 (13) | N61—H36N | 0.911 (3) |
O13—C13 | 1.2489 (18) | N61—H46N | 0.910 (3) |
O23—C13 | 1.2440 (17) | O1W—H101 | 0.820 (2) |
O33—C33 | 1.434 (2) | O1W—H102 | 0.821 (2) |
N3—C23 | 1.4922 | O2W—H201 | 0.820 (2) |
N3—H1N3 | 0.9100 | O2W—H202 | 0.820 (2) |
N3—H2N3 | 0.9100 | O3W—H301 | 0.820 (2) |
N3—H3N3 | 0.9100 | O3W—H302 | 0.819 (2) |
C13—C23 | 1.5563 | O4W—H401 | 0.820 (2) |
C23—C33 | 1.516 (2) | O4W—H402 | 0.820 (2) |
C23—H23 | 1.0000 | O5W—H501 | 0.820 (2) |
C33—H331 | 0.9900 | O5W—H502 | 0.820 (2) |
C33—H332 | 0.9900 | O6W—H601 | 0.820 (2) |
P4—O44 | 1.5019 (15) | O6W—H602 | 0.819 (2) |
O61—P1—O51 | 116.94 (8) | C33—C23—H23 | 108.6 |
O61—P1—O21 | 111.34 (8) | C13—C23—H23 | 108.6 |
O51—P1—O21 | 109.40 (8) | O33—C33—C23 | 108.43 (13) |
O61—P1—O41 | 104.54 (8) | O33—C33—H331 | 110.0 |
O51—P1—O41 | 108.00 (8) | C23—C33—H331 | 110.0 |
O21—P1—O41 | 105.89 (8) | O33—C33—H332 | 110.0 |
P1—O21—H210 | 109.5 | C23—C33—H332 | 110.0 |
C31—O41—P1 | 118.38 (11) | H331—C33—H332 | 108.4 |
C21—N1—H1N1 | 109.5 | O44—P4—O54 | 114.54 (8) |
C21—N1—H2N1 | 109.5 | O44—P4—O64 | 113.97 (8) |
H1N1—N1—H2N1 | 109.5 | O54—P4—O64 | 110.08 (8) |
C21—N1—H3N1 | 109.5 | O44—P4—O34 | 103.55 (7) |
H1N1—N1—H3N1 | 109.5 | O54—P4—O34 | 106.83 (8) |
H2N1—N1—H3N1 | 109.5 | O64—P4—O34 | 107.15 (8) |
O31—C11—O11 | 125.28 (13) | C34—O34—P4 | 119.24 (11) |
O31—C11—C21 | 117.71 (9) | C24—N4—H1N4 | 109.5 |
O11—C11—C21 | 117.00 (10) | C24—N4—H2N4 | 109.5 |
N1—C21—C31 | 109.28 (8) | H1N4—N4—H2N4 | 109.5 |
N1—C21—C11 | 110.2 | C24—N4—H3N4 | 109.5 |
C31—C21—C11 | 112.48 (11) | H1N4—N4—H3N4 | 109.5 |
N1—C21—H21 | 108.3 | H2N4—N4—H3N4 | 109.5 |
C31—C21—H21 | 108.3 | O14—C14—O24 | 125.37 (13) |
C11—C21—H21 | 108.3 | O14—C14—C24 | 118.20 (9) |
O41—C31—C21 | 108.51 (13) | O24—C14—C24 | 116.40 (9) |
O41—C31—H311 | 110.0 | N4—C24—C34 | 110.60 (9) |
C21—C31—H311 | 110.0 | N4—C24—C14 | 109.6 |
O41—C31—H312 | 110.0 | C34—C24—C14 | 111.21 (11) |
C21—C31—H312 | 110.0 | N4—C24—H24 | 108.4 |
H311—C31—H312 | 108.4 | C34—C24—H24 | 108.4 |
O52—P2—O62 | 117.43 (8) | C14—C24—H24 | 108.4 |
O52—P2—O22 | 111.05 (9) | O34—C34—C24 | 108.25 (13) |
O62—P2—O22 | 109.18 (8) | O34—C34—H341 | 110.0 |
O52—P2—O42 | 104.67 (8) | C24—C34—H341 | 110.0 |
O62—P2—O42 | 107.93 (8) | O34—C34—H342 | 110.0 |
O22—P2—O42 | 105.82 (8) | C24—C34—H342 | 110.0 |
P2—O22—H220 | 109.5 | H341—C34—H342 | 108.4 |
C32—O42—P2 | 118.70 (11) | H11N—N11—H21N | 110 (2) |
C22—N2—H1N2 | 109.5 | H11N—N11—H31N | 112 (2) |
C22—N2—H2N2 | 109.5 | H21N—N11—H31N | 119 (2) |
H1N2—N2—H2N2 | 109.5 | H11N—N11—H41N | 109 (2) |
C22—N2—H3N2 | 109.5 | H21N—N11—H41N | 103 (2) |
H1N2—N2—H3N2 | 109.5 | H31N—N11—H41N | 103 (2) |
H2N2—N2—H3N2 | 109.5 | H12N—N21—H22N | 97 (2) |
O12—C12—O32 | 124.77 (13) | H12N—N21—H32N | 114 (2) |
O12—C12—C22 | 118.34 (9) | H22N—N21—H32N | 108 (2) |
O32—C12—C22 | 116.89 (10) | H12N—N21—H42N | 108 (2) |
N2—C22—C32 | 109.77 (8) | H22N—N21—H42N | 115 (2) |
N2—C22—C12 | 109.9 | H32N—N21—H42N | 113 (2) |
C32—C22—C12 | 112.20 (12) | H13N—N31—H23N | 100 (2) |
N2—C22—H22 | 108.3 | H13N—N31—H33N | 112 (2) |
C32—C22—H22 | 108.3 | H23N—N31—H33N | 105 (2) |
C12—C22—H22 | 108.3 | H13N—N31—H43N | 106 (2) |
O42—C32—C22 | 108.35 (13) | H23N—N31—H43N | 123 (2) |
O42—C32—H321 | 110.0 | H33N—N31—H43N | 110 (2) |
C22—C32—H321 | 110.0 | H14N—N41—H24N | 121 (2) |
O42—C32—H322 | 110.0 | H14N—N41—H34N | 96 (2) |
C22—C32—H322 | 110.0 | H24N—N41—H34N | 109 (2) |
H321—C32—H322 | 108.4 | H14N—N41—H44N | 109 (2) |
O43—P3—O63 | 114.34 (8) | H24N—N41—H44N | 114 (2) |
O43—P3—O53 | 114.31 (8) | H34N—N41—H44N | 105 (2) |
O63—P3—O53 | 110.03 (8) | H15N—N51—H25N | 102 (2) |
O43—P3—O33 | 103.47 (7) | H15N—N51—H35N | 96 (2) |
O63—P3—O33 | 106.94 (7) | H25N—N51—H35N | 108 (2) |
O53—P3—O33 | 107.00 (8) | H15N—N51—H45N | 106 (2) |
C33—O33—P3 | 118.59 (11) | H25N—N51—H45N | 134 (2) |
C23—N3—H1N3 | 109.5 | H35N—N51—H45N | 105 (2) |
C23—N3—H2N3 | 109.5 | H16N—N61—H26N | 106 (2) |
H1N3—N3—H2N3 | 109.5 | H16N—N61—H36N | 115 (2) |
C23—N3—H3N3 | 109.5 | H26N—N61—H36N | 107 (2) |
H1N3—N3—H3N3 | 109.5 | H16N—N61—H46N | 90 (2) |
H2N3—N3—H3N3 | 109.5 | H26N—N61—H46N | 103 (2) |
O23—C13—O13 | 126.24 (13) | H36N—N61—H46N | 132 (2) |
O23—C13—C23 | 117.49 (9) | H101—O1W—H102 | 110 (3) |
O13—C13—C23 | 116.26 (9) | H201—O2W—H202 | 117 (3) |
N3—C23—C33 | 109.56 (8) | H301—O3W—H302 | 124 (3) |
N3—C23—C13 | 109.8 | H401—O4W—H402 | 115 (3) |
C33—C23—C13 | 111.53 (11) | H501—O5W—H502 | 106 (3) |
N3—C23—H23 | 108.6 | H601—O6W—H602 | 104 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O21—H210···O1Wi | 0.84 | 1.74 | 2.567 (2) | 169 |
N1—H1N1···O51ii | 0.91 | 1.87 | 2.7773 (18) | 177 |
N1—H2N1···O14i | 0.91 | 2.16 | 2.989 (2) | 152 |
N1—H2N1···O24i | 0.91 | 2.34 | 3.153 (2) | 149 |
N1—H3N1···O52iii | 0.91 | 1.95 | 2.7546 (19) | 146 |
O22—H220···O2Wiv | 0.84 | 1.73 | 2.564 (2) | 173 |
N2—H1N2···O62v | 0.91 | 1.87 | 2.7789 (19) | 178 |
N2—H2N2···O23i | 0.91 | 2.18 | 2.9895 (19) | 148 |
N2—H2N2···O13i | 0.91 | 2.30 | 3.134 (2) | 152 |
N2—H3N2···O61vi | 0.91 | 1.95 | 2.7629 (19) | 148 |
N3—H1N3···O63v | 0.91 | 1.87 | 2.7753 (18) | 175 |
N3—H2N3···O12 | 0.91 | 2.21 | 3.0575 (19) | 154 |
N3—H2N3···O32 | 0.91 | 2.37 | 3.180 (2) | 148 |
N3—H3N3···O44vii | 0.91 | 2.01 | 2.7888 (18) | 142 |
N4—H1N4···O54ii | 0.91 | 1.86 | 2.7679 (18) | 176 |
N4—H2N4···O31 | 0.91 | 2.22 | 3.0596 (19) | 153 |
N4—H2N4···O11 | 0.91 | 2.37 | 3.186 (2) | 150 |
N4—H3N4···O43viii | 0.91 | 2.02 | 2.8059 (19) | 143 |
N11—H11N···O44ix | 0.91 (1) | 1.84 (1) | 2.745 (2) | 177 (2) |
N11—H21N···O14vii | 0.91 (1) | 1.95 (1) | 2.836 (2) | 165 (2) |
N11—H31N···O42v | 0.91 (1) | 2.44 (2) | 3.110 (2) | 131 (2) |
N11—H31N···O12v | 0.91 (1) | 2.50 (2) | 3.042 (3) | 119 (2) |
N11—H41N···O53v | 0.91 (1) | 1.92 (1) | 2.797 (2) | 162 (2) |
N21—H12N···O12 | 0.91 (1) | 1.94 (1) | 2.826 (2) | 163 (2) |
N21—H22N···O52v | 0.91 (1) | 1.99 (1) | 2.851 (3) | 158 (2) |
N21—H32N···O34vii | 0.91 (1) | 2.35 (1) | 3.140 (3) | 145 (2) |
N21—H42N···O53v | 0.91 (1) | 2.00 (1) | 2.872 (3) | 160 (2) |
N31—H13N···O64ix | 0.91 (1) | 2.00 (1) | 2.890 (3) | 165 (2) |
N31—H23N···O31vii | 0.91 (1) | 1.94 (1) | 2.827 (2) | 163 (2) |
N31—H33N···O61ix | 0.91 (1) | 2.00 (1) | 2.843 (3) | 154 (2) |
N31—H43N···O33v | 0.91 (1) | 2.23 (1) | 3.115 (2) | 164 (2) |
N41—H14N···O23 | 0.91 (1) | 1.94 (1) | 2.825 (2) | 164 (2) |
N41—H24N···O43v | 0.91 (1) | 1.84 (1) | 2.731 (2) | 164 (2) |
N41—H34N···O64vii | 0.91 (1) | 1.90 (1) | 2.803 (3) | 171 (2) |
N41—H44N···O41vii | 0.91 (1) | 2.34 (2) | 3.085 (2) | 139 (2) |
N51—H15N···O51 | 0.91 (1) | 1.88 (1) | 2.751 (2) | 159 (2) |
N51—H15N···O6W | 0.91 (1) | 2.57 (2) | 3.147 (3) | 122 (2) |
N51—H25N···O11v | 0.91 (1) | 2.63 (1) | 3.469 (3) | 154 (2) |
N51—H35N···O4W | 0.91 (1) | 1.92 (1) | 2.821 (3) | 169 (2) |
N51—H45N···O64 | 0.91 (1) | 1.81 (1) | 2.706 (2) | 169 (2) |
N61—H16N···O62v | 0.91 (1) | 1.86 (1) | 2.763 (2) | 171 (2) |
N61—H26N···O32 | 0.91 (1) | 2.59 (1) | 3.422 (3) | 152 (2) |
N61—H36N···O6W | 0.91 (1) | 1.92 (1) | 2.802 (3) | 163 (2) |
N61—H46N···O53v | 0.91 (1) | 1.88 (1) | 2.706 (2) | 150 (2) |
O1W—H101···O54 | 0.82 (1) | 1.92 (1) | 2.734 (2) | 170 (3) |
O1W—H102···O3W | 0.82 (1) | 1.91 (1) | 2.727 (3) | 172 (3) |
O2W—H201···O63v | 0.82 (1) | 1.93 (1) | 2.727 (2) | 164 (3) |
O2W—H202···O5W | 0.82 (1) | 1.93 (1) | 2.750 (3) | 176 (3) |
O3W—H301···O24 | 0.82 (1) | 1.89 (1) | 2.684 (3) | 163 (3) |
O3W—H302···O62x | 0.82 (1) | 2.06 (2) | 2.816 (2) | 153 (3) |
O4W—H401···O11 | 0.82 (1) | 1.95 (1) | 2.750 (3) | 165 (3) |
O4W—H402···O63v | 0.82 (1) | 1.96 (1) | 2.767 (2) | 168 (3) |
O5W—H501···O13v | 0.82 (1) | 1.90 (1) | 2.704 (2) | 167 (3) |
O5W—H502···O54 | 0.82 (1) | 1.98 (1) | 2.775 (2) | 164 (3) |
O6W—H601···O32v | 0.82 (1) | 1.92 (1) | 2.726 (3) | 168 (3) |
O6W—H602···O1Wi | 0.82 (1) | 2.43 (1) | 3.239 (3) | 170 (3) |
Symmetry codes: (i) x, y, z−1; (ii) x+1, y, z; (iii) −x+2, y−1/2, −z; (iv) x+1, y, z−1; (v) x−1, y, z; (vi) −x+1, y+1/2, −z; (vii) −x+1, y+1/2, −z+1; (viii) −x+2, y−1/2, −z+1; (ix) −x, y+1/2, −z+1; (x) x−1, y, z+1. |
C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | Z = 4 |
Mr = 475.30 | F(000) = 1008 |
Monoclinic, P21 | Dx = 1.607 Mg m−3 |
Hall symbol: P 2yb | Mo Kα radiation, λ = 0.71073 Å |
a = 7.855 (2) Å | Cell parameters from 17710 reflections |
b = 22.105 (4) Å | µ = 0.30 mm−1 |
c = 11.317 (3) Å | T = 200 K |
β = 90.05 (2)° | Plates, colourless |
V = 1965.0 (8) Å3 | 0.40 × 0.18 × 0.10 mm |
KM4CCD diffractometer | 16120 independent reflections |
Radiation source: fine-focus sealed tube | 8153 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
/w scans | θmax = 38.5°, θmin = 4.5° |
Absorption correction: numerical ? | h = −13→13 |
Tmin = 0.889, Tmax = 0.966 | k = −38→28 |
45319 measured reflections | l = −19→19 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.044 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.092 | w = 1/[σ2(Fo2) + (0.029P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.007 |
16120 reflections | Δρmax = 0.34 e Å−3 |
619 parameters | Δρmin = −0.41 e Å−3 |
37 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.02 (5) |
C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | V = 1965.0 (8) Å3 |
Mr = 475.30 | Z = 4 |
Monoclinic, P21 | Mo Kα radiation |
a = 7.855 (2) Å | µ = 0.30 mm−1 |
b = 22.105 (4) Å | T = 200 K |
c = 11.317 (3) Å | 0.40 × 0.18 × 0.10 mm |
β = 90.05 (2)° |
KM4CCD diffractometer | 16120 independent reflections |
Absorption correction: numerical ? | 8153 reflections with I > 2σ(I) |
Tmin = 0.889, Tmax = 0.966 | Rint = 0.034 |
45319 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.092 | Δρmax = 0.34 e Å−3 |
S = 1.01 | Δρmin = −0.41 e Å−3 |
16120 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
619 parameters | Absolute structure parameter: 0.02 (5) |
37 restraints |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
P1 | 0.25661 (7) | 0.05999 (3) | 0.13298 (5) | 0.01742 (16) | |
O11 | 0.6976 (3) | 0.17943 (8) | 0.38216 (15) | 0.0378 (4) | |
O21 | 0.27351 (19) | 0.06152 (7) | −0.00362 (13) | 0.0255 (4) | |
H210 | 0.2299 | 0.0935 | −0.0297 | 0.031* | |
O31 | 0.77880 (19) | 0.08531 (7) | 0.34435 (13) | 0.0279 (4) | |
O41 | 0.43772 (16) | 0.08229 (6) | 0.18371 (12) | 0.0183 (3) | |
O51 | 0.12286 (17) | 0.10497 (7) | 0.17190 (13) | 0.0238 (4) | |
O61 | 0.23869 (18) | −0.00313 (7) | 0.17721 (14) | 0.0279 (4) | |
N1 | 0.7813 (2) | 0.10115 (8) | 0.10870 (16) | 0.0189 (4) | |
H1N1 | 0.8939 | 0.1026 | 0.1275 | 0.023* | |
H2N1 | 0.7675 | 0.1100 | 0.0307 | 0.023* | |
H3N1 | 0.7404 | 0.0634 | 0.1235 | 0.023* | |
C11 | 0.7232 (2) | 0.13588 (10) | 0.31376 (19) | 0.0179 (5) | |
C21 | 0.6863 (2) | 0.14612 (9) | 0.18152 (18) | 0.0169 (4) | |
H21 | 0.7268 | 0.1875 | 0.1597 | 0.020* | |
C31 | 0.4970 (2) | 0.14184 (9) | 0.15293 (19) | 0.0170 (4) | |
H311 | 0.4332 | 0.1727 | 0.1983 | 0.020* | |
H312 | 0.4782 | 0.1493 | 0.0677 | 0.020* | |
P2 | 1.23985 (6) | 0.41553 (3) | −0.11821 (5) | 0.01758 (12) | |
O12 | 0.71949 (19) | 0.39243 (7) | 0.09228 (14) | 0.0277 (4) | |
O22 | 1.22070 (19) | 0.41436 (7) | −0.25516 (13) | 0.0265 (3) | |
H220 | 1.2562 | 0.3811 | −0.2813 | 0.032* | |
O32 | 0.7981 (2) | 0.29872 (8) | 0.13187 (14) | 0.0362 (4) | |
O42 | 1.05911 (16) | 0.39291 (6) | −0.06667 (12) | 0.0197 (3) | |
O52 | 1.25825 (18) | 0.47856 (7) | −0.07487 (14) | 0.0275 (4) | |
O62 | 1.37357 (17) | 0.37017 (7) | −0.08170 (13) | 0.0226 (3) | |
N2 | 0.7157 (2) | 0.37398 (9) | −0.14382 (15) | 0.0199 (4) | |
H1N2 | 0.6033 | 0.3730 | −0.1244 | 0.024* | |
H2N2 | 0.7284 | 0.3639 | −0.2213 | 0.024* | |
H3N2 | 0.7574 | 0.4119 | −0.1314 | 0.024* | |
C12 | 0.7721 (2) | 0.34165 (10) | 0.06240 (18) | 0.0176 (4) | |
C22 | 0.8105 (2) | 0.33013 (9) | −0.06924 (18) | 0.0170 (4) | |
H22 | 0.7697 | 0.2885 | −0.0894 | 0.020* | |
C32 | 0.9985 (2) | 0.33341 (9) | −0.09687 (19) | 0.0191 (5) | |
H321 | 1.0610 | 0.3025 | −0.0508 | 0.023* | |
H322 | 1.0176 | 0.3255 | −0.1819 | 0.023* | |
P3 | 1.25095 (6) | 0.41489 (2) | 0.38283 (5) | 0.01501 (11) | |
O13 | 0.8243 (2) | 0.30033 (8) | 0.63081 (14) | 0.0355 (4) | |
O23 | 0.72729 (18) | 0.39256 (7) | 0.59490 (14) | 0.0258 (4) | |
O33 | 1.06817 (16) | 0.39311 (6) | 0.43408 (12) | 0.0179 (3) | |
O43 | 1.27080 (18) | 0.47727 (7) | 0.43295 (13) | 0.0237 (3) | |
O53 | 1.23903 (17) | 0.41260 (7) | 0.24850 (13) | 0.0222 (3) | |
O63 | 1.38277 (16) | 0.36968 (7) | 0.42706 (13) | 0.0215 (3) | |
N3 | 0.7221 (2) | 0.37890 (8) | 0.36035 (15) | 0.0165 (4) | |
H1N3 | 0.6095 | 0.3775 | 0.3791 | 0.020* | |
H2N3 | 0.7355 | 0.3713 | 0.2819 | 0.020* | |
H3N3 | 0.7640 | 0.4163 | 0.3774 | 0.020* | |
C13 | 0.7857 (3) | 0.34281 (10) | 0.56377 (19) | 0.0188 (4) | |
C23 | 0.8159 (2) | 0.33254 (9) | 0.43017 (17) | 0.0146 (4) | |
H23 | 0.7713 | 0.2917 | 0.4085 | 0.017* | |
C33 | 1.0036 (2) | 0.33511 (9) | 0.39962 (19) | 0.0165 (4) | |
H331 | 1.0657 | 0.3027 | 0.4418 | 0.020* | |
H332 | 1.0194 | 0.3291 | 0.3136 | 0.020* | |
P4 | 0.25115 (7) | 0.06484 (2) | 0.63448 (5) | 0.01529 (14) | |
O14 | 0.77410 (19) | 0.08565 (7) | 0.84650 (14) | 0.0258 (4) | |
O24 | 0.6786 (2) | 0.17801 (8) | 0.88321 (15) | 0.0354 (4) | |
O34 | 0.43320 (16) | 0.08703 (6) | 0.68666 (13) | 0.0186 (3) | |
O44 | 0.23164 (18) | 0.00252 (7) | 0.68426 (13) | 0.0232 (4) | |
O54 | 0.11871 (17) | 0.10990 (6) | 0.67735 (14) | 0.0223 (3) | |
O64 | 0.26356 (18) | 0.06692 (7) | 0.50006 (13) | 0.0234 (4) | |
N4 | 0.7792 (2) | 0.10108 (8) | 0.61167 (15) | 0.0188 (4) | |
H1N4 | 0.8909 | 0.1011 | 0.6331 | 0.023* | |
H2N4 | 0.7702 | 0.1102 | 0.5335 | 0.023* | |
H3N4 | 0.7338 | 0.0638 | 0.6251 | 0.023* | |
C14 | 0.7170 (2) | 0.13568 (10) | 0.81524 (19) | 0.0197 (5) | |
C24 | 0.6857 (2) | 0.14695 (9) | 0.68233 (17) | 0.0142 (4) | |
H24 | 0.7305 | 0.1879 | 0.6617 | 0.017* | |
C34 | 0.4986 (2) | 0.14493 (9) | 0.6527 (2) | 0.0189 (4) | |
H341 | 0.4375 | 0.1774 | 0.6955 | 0.023* | |
H342 | 0.4819 | 0.1512 | 0.5668 | 0.023* | |
N11 | −0.0011 (2) | 0.48587 (11) | 0.1356 (2) | 0.0247 (4) | |
H11N | −0.077 (2) | 0.4910 (10) | 0.1955 (14) | 0.030* | |
H21N | 0.060 (3) | 0.5207 (6) | 0.130 (2) | 0.030* | |
H31N | −0.053 (3) | 0.4698 (10) | 0.0712 (13) | 0.030* | |
H41N | 0.069 (2) | 0.4559 (7) | 0.162 (2) | 0.030* | |
N21 | 0.4811 (3) | 0.48701 (10) | 0.1261 (2) | 0.0270 (4) | |
H12N | 0.564 (2) | 0.4624 (9) | 0.098 (2) | 0.032* | |
H22N | 0.437 (3) | 0.4899 (11) | 0.0520 (9) | 0.032* | |
H32N | 0.519 (3) | 0.5252 (4) | 0.140 (2) | 0.032* | |
H42N | 0.417 (2) | 0.4666 (9) | 0.1799 (16) | 0.032* | |
N31 | −0.0189 (3) | 0.49150 (10) | 0.6216 (2) | 0.0262 (4) | |
H13N | −0.084 (2) | 0.5176 (8) | 0.5786 (18) | 0.031* | |
H23N | 0.053 (2) | 0.5205 (8) | 0.649 (2) | 0.031* | |
H33N | −0.075 (3) | 0.4779 (10) | 0.6869 (12) | 0.031* | |
H43N | 0.002 (3) | 0.4543 (5) | 0.591 (2) | 0.031* | |
N41 | 0.4995 (3) | 0.49141 (10) | 0.61295 (19) | 0.0236 (4) | |
H14N | 0.570 (2) | 0.4591 (7) | 0.620 (2) | 0.028* | |
H24N | 0.4111 (19) | 0.4872 (10) | 0.5617 (16) | 0.028* | |
H34N | 0.576 (2) | 0.5182 (8) | 0.583 (2) | 0.028* | |
H44N | 0.478 (3) | 0.5069 (10) | 0.6857 (9) | 0.028* | |
N51 | 0.1398 (3) | 0.16472 (9) | 0.38481 (19) | 0.0278 (5) | |
H15N | 0.128 (3) | 0.1547 (11) | 0.3073 (7) | 0.033* | |
H25N | 0.0352 (14) | 0.1816 (10) | 0.395 (2) | 0.033* | |
H35N | 0.207 (3) | 0.1979 (7) | 0.376 (2) | 0.033* | |
H45N | 0.191 (3) | 0.1322 (7) | 0.4188 (19) | 0.033* | |
N61 | 0.3614 (3) | 0.31393 (10) | 0.13604 (19) | 0.0292 (5) | |
H16N | 0.372 (3) | 0.3312 (10) | 0.0635 (10) | 0.035* | |
H26N | 0.4639 (15) | 0.2984 (10) | 0.158 (2) | 0.035* | |
H36N | 0.285 (2) | 0.2828 (7) | 0.134 (2) | 0.035* | |
H46N | 0.349 (3) | 0.3490 (6) | 0.1770 (19) | 0.035* | |
O1W | 0.1431 (3) | 0.15660 (9) | 0.90069 (17) | 0.0397 (5) | |
H101 | 0.127 (4) | 0.1392 (12) | 0.8377 (13) | 0.048* | |
H102 | 0.214 (3) | 0.1837 (9) | 0.896 (3) | 0.048* | |
O2W | 0.3510 (3) | 0.32018 (9) | 0.64620 (17) | 0.0405 (5) | |
H201 | 0.371 (4) | 0.3385 (11) | 0.5847 (14) | 0.049* | |
H202 | 0.273 (2) | 0.2956 (10) | 0.644 (3) | 0.049* | |
O3W | 0.3904 (3) | 0.24330 (9) | 0.8939 (2) | 0.0504 (5) | |
H301 | 0.477 (2) | 0.2243 (13) | 0.878 (3) | 0.060* | |
H302 | 0.388 (4) | 0.2795 (3) | 0.879 (3) | 0.060* | |
O4W | 0.4084 (3) | 0.24879 (8) | 0.36482 (19) | 0.0436 (5) | |
H401 | 0.5011 (18) | 0.2322 (12) | 0.373 (3) | 0.052* | |
H402 | 0.410 (4) | 0.2855 (2) | 0.375 (3) | 0.052* | |
O5W | 0.1089 (2) | 0.23170 (9) | 0.6159 (2) | 0.0460 (5) | |
H501 | 0.0139 (17) | 0.2469 (13) | 0.620 (3) | 0.055* | |
H502 | 0.104 (4) | 0.1955 (3) | 0.631 (3) | 0.055* | |
O6W | 0.0882 (3) | 0.23178 (8) | 0.1409 (2) | 0.0479 (5) | |
H601 | 0.006 (2) | 0.2535 (12) | 0.127 (3) | 0.057* | |
H602 | 0.102 (4) | 0.1986 (7) | 0.110 (3) | 0.057* |
U11 | U22 | U33 | U12 | U13 | U23 | |
P1 | 0.0127 (2) | 0.0212 (4) | 0.0184 (3) | −0.0018 (2) | 0.0006 (2) | −0.0036 (2) |
O11 | 0.0573 (12) | 0.0325 (10) | 0.0235 (10) | 0.0061 (9) | −0.0060 (8) | −0.0120 (8) |
O21 | 0.0311 (8) | 0.0282 (10) | 0.0174 (8) | 0.0052 (7) | −0.0010 (6) | −0.0033 (7) |
O31 | 0.0320 (9) | 0.0360 (10) | 0.0158 (8) | 0.0077 (7) | −0.0016 (7) | 0.0086 (8) |
O41 | 0.0130 (6) | 0.0195 (8) | 0.0224 (8) | −0.0028 (6) | −0.0020 (6) | 0.0043 (6) |
O51 | 0.0140 (7) | 0.0336 (9) | 0.0239 (9) | 0.0022 (6) | −0.0011 (6) | −0.0072 (7) |
O61 | 0.0281 (8) | 0.0251 (10) | 0.0306 (10) | −0.0060 (7) | 0.0010 (7) | 0.0026 (7) |
N1 | 0.0140 (8) | 0.0253 (10) | 0.0174 (10) | −0.0006 (7) | 0.0000 (7) | −0.0023 (8) |
C11 | 0.0141 (9) | 0.0221 (11) | 0.0173 (12) | −0.0006 (8) | −0.0005 (8) | 0.0004 (9) |
C21 | 0.0165 (9) | 0.0165 (10) | 0.0176 (11) | 0.0001 (8) | 0.0006 (8) | 0.0018 (9) |
C31 | 0.0140 (9) | 0.0161 (10) | 0.0208 (11) | −0.0013 (8) | −0.0020 (8) | 0.0023 (9) |
P2 | 0.0139 (2) | 0.0204 (3) | 0.0184 (3) | −0.0011 (3) | −0.0008 (2) | 0.0025 (2) |
O12 | 0.0308 (8) | 0.0312 (9) | 0.0211 (9) | 0.0078 (7) | 0.0039 (7) | −0.0082 (7) |
O22 | 0.0348 (8) | 0.0268 (9) | 0.0179 (8) | 0.0064 (8) | 0.0011 (6) | 0.0036 (7) |
O32 | 0.0569 (11) | 0.0314 (10) | 0.0202 (9) | 0.0029 (9) | 0.0051 (8) | 0.0099 (8) |
O42 | 0.0150 (7) | 0.0205 (7) | 0.0235 (8) | −0.0027 (6) | 0.0040 (6) | −0.0064 (6) |
O52 | 0.0280 (8) | 0.0228 (8) | 0.0317 (10) | −0.0059 (7) | 0.0016 (7) | −0.0009 (8) |
O62 | 0.0151 (7) | 0.0276 (8) | 0.0251 (8) | 0.0028 (6) | 0.0018 (6) | 0.0042 (7) |
N2 | 0.0176 (9) | 0.0273 (10) | 0.0149 (9) | −0.0017 (8) | 0.0010 (7) | 0.0016 (8) |
C12 | 0.0129 (9) | 0.0262 (12) | 0.0137 (11) | −0.0002 (8) | 0.0015 (8) | −0.0037 (9) |
C22 | 0.0135 (9) | 0.0184 (10) | 0.0190 (11) | −0.0006 (8) | −0.0004 (8) | −0.0013 (9) |
C32 | 0.0162 (10) | 0.0197 (11) | 0.0214 (11) | −0.0022 (8) | 0.0040 (8) | −0.0049 (9) |
P3 | 0.0119 (2) | 0.0149 (3) | 0.0183 (3) | −0.0010 (2) | 0.0014 (2) | 0.0006 (2) |
O13 | 0.0452 (11) | 0.0379 (11) | 0.0233 (9) | 0.0079 (9) | 0.0020 (8) | 0.0095 (8) |
O23 | 0.0263 (8) | 0.0268 (9) | 0.0241 (9) | 0.0031 (7) | 0.0022 (6) | −0.0067 (7) |
O33 | 0.0118 (6) | 0.0179 (7) | 0.0238 (8) | −0.0022 (5) | 0.0023 (5) | −0.0021 (6) |
O43 | 0.0227 (7) | 0.0172 (7) | 0.0312 (9) | −0.0030 (6) | −0.0054 (6) | −0.0027 (7) |
O53 | 0.0246 (7) | 0.0248 (8) | 0.0173 (8) | −0.0007 (7) | 0.0039 (6) | 0.0002 (7) |
O63 | 0.0129 (7) | 0.0216 (8) | 0.0299 (9) | 0.0001 (6) | 0.0003 (6) | 0.0035 (7) |
N3 | 0.0151 (8) | 0.0187 (9) | 0.0156 (9) | −0.0029 (7) | 0.0000 (7) | 0.0000 (7) |
C13 | 0.0149 (9) | 0.0224 (11) | 0.0191 (12) | −0.0050 (8) | 0.0019 (8) | 0.0004 (9) |
C23 | 0.0167 (9) | 0.0136 (10) | 0.0134 (10) | −0.0021 (8) | 0.0030 (7) | −0.0019 (8) |
C33 | 0.0132 (9) | 0.0145 (10) | 0.0216 (11) | 0.0018 (8) | 0.0017 (8) | −0.0015 (9) |
P4 | 0.0127 (2) | 0.0144 (3) | 0.0188 (3) | 0.0003 (2) | −0.0009 (2) | 0.0003 (2) |
O14 | 0.0266 (8) | 0.0236 (9) | 0.0272 (9) | 0.0031 (7) | −0.0028 (7) | 0.0044 (7) |
O24 | 0.0483 (11) | 0.0357 (10) | 0.0220 (10) | 0.0075 (9) | −0.0039 (8) | −0.0091 (8) |
O34 | 0.0132 (6) | 0.0177 (8) | 0.0249 (8) | −0.0021 (6) | −0.0034 (6) | 0.0042 (6) |
O44 | 0.0226 (7) | 0.0169 (8) | 0.0301 (9) | −0.0035 (6) | 0.0025 (6) | 0.0008 (7) |
O54 | 0.0153 (7) | 0.0191 (8) | 0.0324 (10) | 0.0006 (6) | −0.0006 (6) | −0.0030 (7) |
O64 | 0.0252 (8) | 0.0256 (9) | 0.0193 (9) | 0.0007 (6) | −0.0042 (6) | −0.0015 (7) |
N4 | 0.0163 (8) | 0.0261 (10) | 0.0139 (9) | −0.0023 (7) | −0.0002 (7) | −0.0003 (8) |
C14 | 0.0163 (10) | 0.0262 (12) | 0.0165 (12) | −0.0061 (9) | −0.0023 (8) | 0.0001 (9) |
C24 | 0.0134 (9) | 0.0125 (9) | 0.0168 (11) | −0.0031 (7) | −0.0034 (8) | 0.0019 (8) |
C34 | 0.0149 (9) | 0.0177 (10) | 0.0240 (12) | −0.0009 (8) | −0.0014 (8) | 0.0044 (9) |
N11 | 0.0215 (10) | 0.0271 (11) | 0.0254 (11) | −0.0009 (8) | −0.0003 (8) | −0.0026 (9) |
N21 | 0.0230 (10) | 0.0219 (11) | 0.0361 (12) | 0.0012 (9) | 0.0019 (8) | 0.0018 (10) |
N31 | 0.0239 (10) | 0.0189 (10) | 0.0358 (12) | −0.0043 (8) | 0.0007 (8) | 0.0016 (9) |
N41 | 0.0227 (10) | 0.0249 (11) | 0.0232 (11) | 0.0044 (8) | −0.0048 (8) | −0.0043 (9) |
N51 | 0.0379 (12) | 0.0218 (11) | 0.0237 (11) | 0.0016 (9) | 0.0019 (9) | −0.0028 (9) |
N61 | 0.0337 (11) | 0.0273 (12) | 0.0267 (11) | −0.0021 (9) | −0.0009 (9) | 0.0027 (9) |
O1W | 0.0461 (11) | 0.0419 (12) | 0.0310 (11) | −0.0077 (9) | −0.0020 (9) | −0.0060 (9) |
O2W | 0.0497 (12) | 0.0406 (12) | 0.0313 (11) | −0.0040 (9) | 0.0014 (9) | 0.0087 (9) |
O3W | 0.0461 (12) | 0.0293 (12) | 0.0756 (15) | 0.0097 (10) | 0.0014 (11) | −0.0097 (11) |
O4W | 0.0439 (12) | 0.0235 (10) | 0.0635 (13) | 0.0013 (9) | −0.0026 (10) | −0.0123 (10) |
O5W | 0.0411 (12) | 0.0292 (11) | 0.0677 (14) | 0.0053 (10) | 0.0070 (10) | 0.0119 (11) |
O6W | 0.0463 (12) | 0.0222 (10) | 0.0751 (16) | 0.0056 (9) | 0.0006 (11) | 0.0115 (11) |
P1—O61 | 1.4890 (17) | P4—O54 | 1.5202 (15) |
P1—O51 | 1.5124 (16) | P4—O64 | 1.5251 (17) |
P1—O21 | 1.5521 (17) | P4—O34 | 1.6226 (14) |
P1—O41 | 1.6108 (14) | O14—C14 | 1.245 (3) |
O11—C11 | 1.252 (3) | O24—C14 | 1.248 (3) |
O21—H210 | 0.8400 | O34—C34 | 1.432 (2) |
O31—C11 | 1.249 (2) | N4—C24 | 1.486 (3) |
O41—C31 | 1.439 (2) | N4—H1N4 | 0.9100 |
N1—C21 | 1.492 (3) | N4—H2N4 | 0.9100 |
N1—H1N1 | 0.9100 | N4—H3N4 | 0.9100 |
N1—H2N1 | 0.9100 | C14—C24 | 1.544 (3) |
N1—H3N1 | 0.9100 | C24—C34 | 1.508 (3) |
C11—C21 | 1.541 (3) | C24—H24 | 1.0000 |
C21—C31 | 1.525 (3) | C34—H341 | 0.9900 |
C21—H21 | 1.0000 | C34—H342 | 0.9900 |
C31—H311 | 0.9900 | N11—H11N | 0.911 (3) |
C31—H312 | 0.9900 | N11—H21N | 0.909 (3) |
P2—O52 | 1.4841 (17) | N11—H31N | 0.908 (3) |
P2—O62 | 1.5094 (15) | N11—H41N | 0.910 (3) |
P2—O22 | 1.5573 (17) | N21—H12N | 0.909 (3) |
P2—O42 | 1.6146 (14) | N21—H22N | 0.911 (3) |
O12—C12 | 1.243 (2) | N21—H32N | 0.909 (3) |
O22—H220 | 0.8400 | N21—H42N | 0.911 (3) |
O32—C12 | 1.249 (3) | N31—H13N | 0.910 (3) |
O42—C32 | 1.440 (2) | N31—H23N | 0.909 (3) |
N2—C22 | 1.485 (3) | N31—H33N | 0.910 (3) |
N2—H1N2 | 0.9100 | N31—H43N | 0.909 (3) |
N2—H2N2 | 0.9100 | N41—H14N | 0.909 (3) |
N2—H3N2 | 0.9100 | N41—H24N | 0.910 (3) |
C12—C22 | 1.541 (3) | N41—H34N | 0.910 (3) |
C22—C32 | 1.511 (3) | N41—H44N | 0.908 (3) |
C22—H22 | 1.0000 | N51—H15N | 0.910 (3) |
C32—H321 | 0.9900 | N51—H25N | 0.910 (3) |
C32—H322 | 0.9900 | N51—H35N | 0.910 (3) |
P3—O43 | 1.4990 (16) | N51—H45N | 0.910 (3) |
P3—O63 | 1.5234 (15) | N61—H16N | 0.910 (3) |
P3—O53 | 1.5239 (16) | N61—H26N | 0.910 (3) |
P3—O33 | 1.6220 (14) | N61—H36N | 0.911 (3) |
O13—C13 | 1.244 (3) | N61—H46N | 0.909 (3) |
O23—C13 | 1.243 (2) | O1W—H101 | 0.820 (2) |
O33—C33 | 1.433 (2) | O1W—H102 | 0.820 (2) |
N3—C23 | 1.489 (2) | O2W—H201 | 0.820 (2) |
N3—H1N3 | 0.9100 | O2W—H202 | 0.820 (2) |
N3—H2N3 | 0.9100 | O3W—H301 | 0.820 (2) |
N3—H3N3 | 0.9100 | O3W—H302 | 0.819 (2) |
C13—C23 | 1.547 (3) | O4W—H401 | 0.820 (2) |
C23—C33 | 1.515 (3) | O4W—H402 | 0.819 (2) |
C23—H23 | 1.0000 | O5W—H501 | 0.820 (2) |
C33—H331 | 0.9900 | O5W—H502 | 0.819 (2) |
C33—H332 | 0.9900 | O6W—H601 | 0.820 (2) |
P4—O44 | 1.4962 (16) | O6W—H602 | 0.819 (2) |
O61—P1—O51 | 116.89 (9) | C33—C23—H23 | 108.6 |
O61—P1—O21 | 111.31 (9) | C13—C23—H23 | 108.6 |
O51—P1—O21 | 109.62 (9) | O33—C33—C23 | 108.40 (15) |
O61—P1—O41 | 104.52 (8) | O33—C33—H331 | 110.0 |
O51—P1—O41 | 107.97 (8) | C23—C33—H331 | 110.0 |
O21—P1—O41 | 105.79 (9) | O33—C33—H332 | 110.0 |
P1—O21—H210 | 109.5 | C23—C33—H332 | 110.0 |
C31—O41—P1 | 118.65 (12) | H331—C33—H332 | 108.4 |
C21—N1—H1N1 | 109.5 | O44—P4—O54 | 114.38 (8) |
C21—N1—H2N1 | 109.5 | O44—P4—O64 | 114.21 (9) |
H1N1—N1—H2N1 | 109.5 | O54—P4—O64 | 110.05 (9) |
C21—N1—H3N1 | 109.5 | O44—P4—O34 | 103.40 (8) |
H1N1—N1—H3N1 | 109.5 | O54—P4—O34 | 106.79 (8) |
H2N1—N1—H3N1 | 109.5 | O64—P4—O34 | 107.27 (8) |
O31—C11—O11 | 125.0 (2) | C34—O34—P4 | 119.25 (12) |
O31—C11—C21 | 117.78 (19) | C24—N4—H1N4 | 109.5 |
O11—C11—C21 | 117.23 (19) | C24—N4—H2N4 | 109.5 |
N1—C21—C31 | 109.24 (16) | H1N4—N4—H2N4 | 109.5 |
N1—C21—C11 | 110.20 (16) | C24—N4—H3N4 | 109.5 |
C31—C21—C11 | 112.29 (16) | H1N4—N4—H3N4 | 109.5 |
N1—C21—H21 | 108.3 | H2N4—N4—H3N4 | 109.5 |
C31—C21—H21 | 108.3 | O14—C14—O24 | 125.3 (2) |
C11—C21—H21 | 108.3 | O14—C14—C24 | 118.50 (19) |
O41—C31—C21 | 108.73 (15) | O24—C14—C24 | 116.2 (2) |
O41—C31—H311 | 109.9 | N4—C24—C34 | 110.01 (15) |
C21—C31—H311 | 109.9 | N4—C24—C14 | 109.62 (16) |
O41—C31—H312 | 109.9 | C34—C24—C14 | 111.49 (16) |
C21—C31—H312 | 109.9 | N4—C24—H24 | 108.5 |
H311—C31—H312 | 108.3 | C34—C24—H24 | 108.5 |
O52—P2—O62 | 117.75 (9) | C14—C24—H24 | 108.5 |
O52—P2—O22 | 110.71 (9) | O34—C34—C24 | 108.44 (15) |
O62—P2—O22 | 109.15 (9) | O34—C34—H341 | 110.0 |
O52—P2—O42 | 104.87 (8) | C24—C34—H341 | 110.0 |
O62—P2—O42 | 107.90 (8) | O34—C34—H342 | 110.0 |
O22—P2—O42 | 105.68 (9) | C24—C34—H342 | 110.0 |
P2—O22—H220 | 109.5 | H341—C34—H342 | 108.4 |
C32—O42—P2 | 119.20 (12) | H11N—N11—H21N | 107 (2) |
C22—N2—H1N2 | 109.5 | H11N—N11—H31N | 111 (2) |
C22—N2—H2N2 | 109.5 | H21N—N11—H31N | 121 (2) |
H1N2—N2—H2N2 | 109.5 | H11N—N11—H41N | 104 (2) |
C22—N2—H3N2 | 109.5 | H21N—N11—H41N | 109 (2) |
H1N2—N2—H3N2 | 109.5 | H31N—N11—H41N | 104 (2) |
H2N2—N2—H3N2 | 109.5 | H12N—N21—H22N | 89 (2) |
O12—C12—O32 | 124.7 (2) | H12N—N21—H32N | 112 (2) |
O12—C12—C22 | 118.52 (19) | H22N—N21—H32N | 103 (2) |
O32—C12—C22 | 116.80 (19) | H12N—N21—H42N | 110 (2) |
N2—C22—C32 | 109.91 (16) | H22N—N21—H42N | 116 (2) |
N2—C22—C12 | 110.06 (16) | H32N—N21—H42N | 122 (2) |
C32—C22—C12 | 112.59 (16) | H13N—N31—H23N | 95 (2) |
N2—C22—H22 | 108.0 | H13N—N31—H33N | 112 (2) |
C32—C22—H22 | 108.0 | H23N—N31—H33N | 105 (2) |
C12—C22—H22 | 108.0 | H13N—N31—H43N | 118 (2) |
O42—C32—C22 | 108.53 (16) | H23N—N31—H43N | 131 (2) |
O42—C32—H321 | 110.0 | H33N—N31—H43N | 96 (2) |
C22—C32—H321 | 110.0 | H14N—N41—H24N | 116 (2) |
O42—C32—H322 | 110.0 | H14N—N41—H34N | 98 (2) |
C22—C32—H322 | 110.0 | H24N—N41—H34N | 109 (2) |
H321—C32—H322 | 108.4 | H14N—N41—H44N | 110 (2) |
O43—P3—O63 | 114.12 (8) | H24N—N41—H44N | 118 (2) |
O43—P3—O53 | 114.48 (9) | H34N—N41—H44N | 103 (2) |
O63—P3—O53 | 110.31 (8) | H15N—N51—H25N | 98 (2) |
O43—P3—O33 | 103.27 (8) | H15N—N51—H35N | 98 (2) |
O63—P3—O33 | 106.82 (8) | H25N—N51—H35N | 102 (2) |
O53—P3—O33 | 107.05 (8) | H15N—N51—H45N | 105 (2) |
C33—O33—P3 | 118.79 (12) | H25N—N51—H45N | 132 (2) |
C23—N3—H1N3 | 109.5 | H35N—N51—H45N | 115 (2) |
C23—N3—H2N3 | 109.5 | H16N—N61—H26N | 109 (2) |
H1N3—N3—H2N3 | 109.5 | H16N—N61—H36N | 111 (2) |
C23—N3—H3N3 | 109.5 | H26N—N61—H36N | 108 (2) |
H1N3—N3—H3N3 | 109.5 | H16N—N61—H46N | 96 (2) |
H2N3—N3—H3N3 | 109.5 | H26N—N61—H46N | 106 (2) |
O23—C13—O13 | 125.8 (2) | H36N—N61—H46N | 126 (2) |
O23—C13—C23 | 117.62 (19) | H101—O1W—H102 | 113 (3) |
O13—C13—C23 | 116.59 (19) | H201—O2W—H202 | 117 (3) |
N3—C23—C33 | 109.53 (15) | H301—O3W—H302 | 118 (3) |
N3—C23—C13 | 109.97 (15) | H401—O4W—H402 | 115 (3) |
C33—C23—C13 | 111.56 (16) | H501—O5W—H502 | 110 (3) |
N3—C23—H23 | 108.6 | H601—O6W—H602 | 123 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O21—H210···O1Wi | 0.84 | 1.74 | 2.576 (3) | 174 |
N1—H1N1···O51ii | 0.91 | 1.87 | 2.777 (2) | 178 |
N1—H2N1···O14i | 0.91 | 2.15 | 2.987 (2) | 152 |
N1—H2N1···O24i | 0.91 | 2.35 | 3.169 (3) | 149 |
N1—H3N1···O52iii | 0.91 | 1.95 | 2.754 (2) | 146 |
O22—H220···O2Wiv | 0.84 | 1.74 | 2.575 (3) | 170 |
N2—H1N2···O62v | 0.91 | 1.87 | 2.780 (2) | 179 |
N2—H2N2···O23i | 0.91 | 2.17 | 2.987 (2) | 148 |
N2—H2N2···O13i | 0.91 | 2.31 | 3.144 (3) | 152 |
N2—H3N2···O61vi | 0.91 | 1.95 | 2.766 (2) | 148 |
N3—H1N3···O63v | 0.91 | 1.87 | 2.779 (2) | 175 |
N3—H2N3···O12 | 0.91 | 2.20 | 3.048 (2) | 155 |
N3—H2N3···O32 | 0.91 | 2.39 | 3.191 (2) | 147 |
N3—H3N3···O44vii | 0.91 | 2.03 | 2.803 (2) | 142 |
N4—H1N4···O54ii | 0.91 | 1.87 | 2.775 (2) | 174 |
N4—H2N4···O31 | 0.91 | 2.21 | 3.045 (2) | 152 |
N4—H2N4···O11 | 0.91 | 2.37 | 3.187 (3) | 150 |
N4—H3N4···O43viii | 0.91 | 2.02 | 2.811 (2) | 144 |
N11—H11N···O44ix | 0.91 (1) | 1.84 (1) | 2.753 (3) | 179 (2) |
N11—H21N···O14vii | 0.91 (1) | 1.96 (1) | 2.843 (3) | 165 (2) |
N11—H31N···O42v | 0.91 (1) | 2.47 (2) | 3.113 (3) | 128 (2) |
N11—H31N···O12v | 0.91 (1) | 2.48 (2) | 3.053 (3) | 121 (2) |
N11—H41N···O53v | 0.91 (1) | 1.91 (1) | 2.794 (3) | 162 (2) |
N21—H12N···O12 | 0.91 (1) | 1.97 (1) | 2.833 (3) | 158 (2) |
N21—H22N···O52v | 0.91 (1) | 2.02 (1) | 2.875 (3) | 156 (2) |
N21—H32N···O34vii | 0.91 (1) | 2.42 (2) | 3.135 (3) | 136 (2) |
N21—H42N···O53v | 0.91 (1) | 2.00 (1) | 2.871 (3) | 161 (2) |
N31—H13N···O64ix | 0.91 (1) | 2.00 (1) | 2.892 (3) | 169 (2) |
N31—H23N···O31vii | 0.91 (1) | 1.95 (1) | 2.829 (3) | 162 (2) |
N31—H33N···O61ix | 0.91 (1) | 2.05 (1) | 2.861 (3) | 148 (2) |
N31—H43N···O33v | 0.91 (1) | 2.29 (1) | 3.115 (3) | 151 (2) |
N41—H14N···O23 | 0.91 (1) | 1.94 (1) | 2.832 (3) | 167 (2) |
N41—H24N···O43v | 0.91 (1) | 1.84 (1) | 2.733 (3) | 167 (2) |
N41—H34N···O64vii | 0.91 (1) | 1.91 (1) | 2.809 (3) | 172 (2) |
N41—H44N···O41vii | 0.91 (1) | 2.33 (2) | 3.094 (3) | 142 (2) |
N51—H15N···O51 | 0.91 (1) | 1.89 (1) | 2.751 (3) | 158 (2) |
N51—H15N···O6W | 0.91 (1) | 2.56 (2) | 3.159 (3) | 124 (2) |
N51—H25N···O11v | 0.91 (1) | 2.66 (1) | 3.489 (3) | 152 (2) |
N51—H35N···O4W | 0.91 (1) | 1.95 (1) | 2.821 (3) | 161 (2) |
N51—H45N···O64 | 0.91 (1) | 1.80 (1) | 2.705 (3) | 171 (2) |
N61—H16N···O62v | 0.91 (1) | 1.86 (1) | 2.762 (3) | 174 (2) |
N61—H26N···O32 | 0.91 (1) | 2.64 (1) | 3.447 (3) | 148 (2) |
N61—H36N···O6W | 0.91 (1) | 1.92 (1) | 2.812 (3) | 167 (2) |
N61—H46N···O53v | 0.91 (1) | 1.84 (1) | 2.703 (3) | 158 (2) |
O1W—H101···O54 | 0.82 (1) | 1.93 (1) | 2.737 (3) | 169 (3) |
O1W—H102···O3W | 0.82 (1) | 1.91 (1) | 2.730 (3) | 175 (3) |
O2W—H201···O63v | 0.82 (1) | 1.92 (1) | 2.722 (2) | 168 (3) |
O2W—H202···O5W | 0.82 (1) | 1.94 (1) | 2.749 (3) | 170 (3) |
O3W—H301···O24 | 0.82 (1) | 1.89 (1) | 2.688 (3) | 166 (3) |
O3W—H302···O62x | 0.82 (1) | 2.05 (1) | 2.821 (3) | 156 (3) |
O4W—H401···O11 | 0.82 (1) | 1.94 (1) | 2.748 (3) | 169 (3) |
O4W—H402···O63v | 0.82 (1) | 1.96 (1) | 2.771 (2) | 168 (3) |
O5W—H501···O13v | 0.82 (1) | 1.91 (1) | 2.707 (3) | 166 (3) |
O5W—H502···O54 | 0.82 (1) | 1.97 (1) | 2.782 (2) | 173 (3) |
O6W—H601···O32v | 0.82 (1) | 1.92 (1) | 2.719 (3) | 166 (3) |
O6W—H602···O1Wi | 0.82 (1) | 2.56 (2) | 3.216 (3) | 138 (3) |
N21—H32N···O21vi | 0.91 (1) | 2.38 (2) | 2.890 (3) | 115 (2) |
O6W—H602···O51 | 0.82 (1) | 2.19 (2) | 2.838 (3) | 136 (3) |
Symmetry codes: (i) x, y, z−1; (ii) x+1, y, z; (iii) −x+2, y−1/2, −z; (iv) x+1, y, z−1; (v) x−1, y, z; (vi) −x+1, y+1/2, −z; (vii) −x+1, y+1/2, −z+1; (viii) −x+2, y−1/2, −z+1; (ix) −x, y+1/2, −z+1; (x) x−1, y, z+1. |
C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | Z = 4 |
Mr = 475.30 | F(000) = 1008 |
Monoclinic, P21 | Dx = 1.601 Mg m−3 |
Hall symbol: P 2yb | Mo Kα radiation, λ = 0.71073 Å |
a = 7.861 (2) Å | Cell parameters from 17710 reflections |
b = 22.163 (4) Å | µ = 0.30 mm−1 |
c = 11.315 (3) Å | T = 250 K |
β = 90.06 (2)° | Plates, colourless |
V = 1971.3 (8) Å3 | 0.40 × 0.18 × 0.10 mm |
KM4CCD diffractometer | 16208 independent reflections |
Radiation source: fine-focus sealed tube | 9135 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
/w scans | θmax = 38.5°, θmin = 4.5° |
Absorption correction: numerical ? | h = −13→13 |
Tmin = 0.889, Tmax = 0.966 | k = −38→27 |
47886 measured reflections | l = −19→19 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.047 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.122 | w = 1/[σ2(Fo2) + (0.051P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.008 |
16208 reflections | Δρmax = 0.36 e Å−3 |
619 parameters | Δρmin = −0.42 e Å−3 |
37 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.12 (6) |
C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | V = 1971.3 (8) Å3 |
Mr = 475.30 | Z = 4 |
Monoclinic, P21 | Mo Kα radiation |
a = 7.861 (2) Å | µ = 0.30 mm−1 |
b = 22.163 (4) Å | T = 250 K |
c = 11.315 (3) Å | 0.40 × 0.18 × 0.10 mm |
β = 90.06 (2)° |
KM4CCD diffractometer | 16208 independent reflections |
Absorption correction: numerical ? | 9135 reflections with I > 2σ(I) |
Tmin = 0.889, Tmax = 0.966 | Rint = 0.031 |
47886 measured reflections |
R[F2 > 2σ(F2)] = 0.047 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.122 | Δρmax = 0.36 e Å−3 |
S = 1.01 | Δρmin = −0.42 e Å−3 |
16208 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
619 parameters | Absolute structure parameter: 0.12 (6) |
37 restraints |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
P1 | 0.25753 (6) | 0.05967 (2) | 0.13338 (5) | 0.01978 (16) | |
O11 | 0.6987 (3) | 0.17942 (8) | 0.38121 (16) | 0.0439 (5) | |
O21 | 0.2735 (2) | 0.06121 (7) | −0.00346 (13) | 0.0294 (4) | |
H210 | 0.2538 | 0.0959 | −0.0276 | 0.035* | |
O31 | 0.7792 (2) | 0.08563 (8) | 0.34436 (14) | 0.0333 (4) | |
O41 | 0.43869 (16) | 0.08202 (6) | 0.18345 (13) | 0.0218 (3) | |
O51 | 0.12389 (17) | 0.10438 (7) | 0.17230 (13) | 0.0277 (4) | |
O61 | 0.2412 (2) | −0.00330 (7) | 0.17726 (15) | 0.0329 (4) | |
N1 | 0.7820 (2) | 0.10110 (8) | 0.10885 (15) | 0.0206 (3) | |
H1N1 | 0.8932 | 0.1030 | 0.1273 | 0.025* | |
H2N1 | 0.7679 | 0.1096 | 0.0317 | 0.025* | |
H3N1 | 0.7426 | 0.0638 | 0.1239 | 0.025* | |
C11 | 0.7238 (2) | 0.13596 (10) | 0.31375 (17) | 0.0205 (4) | |
C21 | 0.6864 (2) | 0.14569 (9) | 0.18100 (17) | 0.0188 (4) | |
H21 | 0.7264 | 0.1865 | 0.1592 | 0.023* | |
C31 | 0.4975 (2) | 0.14164 (9) | 0.15224 (19) | 0.0206 (4) | |
H311 | 0.4344 | 0.1721 | 0.1970 | 0.025* | |
H312 | 0.4790 | 0.1490 | 0.0678 | 0.025* | |
P2 | 1.23868 (6) | 0.41573 (3) | −0.11815 (5) | 0.01977 (11) | |
O12 | 0.7186 (2) | 0.39208 (8) | 0.09214 (14) | 0.0332 (4) | |
O22 | 1.2199 (2) | 0.41455 (8) | −0.25532 (13) | 0.0312 (3) | |
H220 | 1.2658 | 0.3837 | −0.2819 | 0.037* | |
O32 | 0.7974 (3) | 0.29873 (8) | 0.13111 (15) | 0.0418 (4) | |
O42 | 1.05800 (17) | 0.39311 (6) | −0.06684 (13) | 0.0228 (3) | |
O52 | 1.2560 (2) | 0.47844 (7) | −0.07472 (15) | 0.0321 (4) | |
O62 | 1.37220 (17) | 0.37081 (7) | −0.08148 (13) | 0.0272 (3) | |
N2 | 0.7149 (2) | 0.37409 (9) | −0.14392 (15) | 0.0226 (4) | |
H1N2 | 0.6036 | 0.3726 | −0.1257 | 0.027* | |
H2N2 | 0.7290 | 0.3648 | −0.2207 | 0.027* | |
H3N2 | 0.7548 | 0.4115 | −0.1303 | 0.027* | |
C12 | 0.7715 (2) | 0.34170 (10) | 0.06221 (17) | 0.0212 (4) | |
C22 | 0.8092 (2) | 0.33039 (9) | −0.07010 (17) | 0.0186 (4) | |
H22 | 0.7689 | 0.2893 | −0.0904 | 0.022* | |
C32 | 0.9982 (2) | 0.33384 (9) | −0.09759 (18) | 0.0218 (4) | |
H321 | 1.0601 | 0.3033 | −0.0520 | 0.026* | |
H322 | 1.0175 | 0.3262 | −0.1818 | 0.026* | |
P3 | 1.25085 (6) | 0.41477 (2) | 0.38253 (4) | 0.01722 (11) | |
O13 | 0.8251 (2) | 0.30062 (8) | 0.62976 (15) | 0.0402 (4) | |
O23 | 0.7284 (2) | 0.39247 (8) | 0.59503 (14) | 0.0300 (4) | |
O33 | 1.06780 (16) | 0.39327 (6) | 0.43280 (12) | 0.0204 (3) | |
O43 | 1.27019 (19) | 0.47686 (7) | 0.43278 (14) | 0.0281 (3) | |
O53 | 1.23973 (18) | 0.41253 (7) | 0.24824 (13) | 0.0258 (3) | |
O63 | 1.38268 (17) | 0.36962 (7) | 0.42688 (13) | 0.0245 (3) | |
N3 | 0.7212 (2) | 0.37932 (8) | 0.36002 (14) | 0.0197 (3) | |
H1N3 | 0.6110 | 0.3790 | 0.3816 | 0.024* | |
H2N3 | 0.7294 | 0.3709 | 0.2824 | 0.024* | |
H3N3 | 0.7659 | 0.4160 | 0.3743 | 0.024* | |
C13 | 0.7861 (3) | 0.34286 (10) | 0.56345 (18) | 0.0216 (4) | |
C23 | 0.8161 (2) | 0.33294 (8) | 0.42928 (16) | 0.0166 (4) | |
H23 | 0.7717 | 0.2926 | 0.4076 | 0.020* | |
C33 | 1.0028 (2) | 0.33533 (9) | 0.39845 (18) | 0.0191 (4) | |
H331 | 1.0643 | 0.3033 | 0.4402 | 0.023* | |
H332 | 1.0181 | 0.3294 | 0.3133 | 0.023* | |
P4 | 0.25138 (6) | 0.06508 (2) | 0.63438 (5) | 0.01718 (13) | |
O14 | 0.7726 (2) | 0.08568 (7) | 0.84682 (15) | 0.0298 (4) | |
O24 | 0.6779 (3) | 0.17789 (8) | 0.88270 (15) | 0.0410 (4) | |
O34 | 0.43350 (17) | 0.08730 (6) | 0.68574 (12) | 0.0216 (3) | |
O44 | 0.23221 (19) | 0.00276 (7) | 0.68460 (14) | 0.0268 (3) | |
O54 | 0.11892 (17) | 0.10976 (7) | 0.67757 (14) | 0.0259 (3) | |
O64 | 0.26289 (19) | 0.06707 (7) | 0.50017 (13) | 0.0262 (3) | |
N4 | 0.7800 (2) | 0.10069 (8) | 0.61161 (15) | 0.0214 (4) | |
H1N4 | 0.8904 | 0.1009 | 0.6325 | 0.026* | |
H2N4 | 0.7705 | 0.1095 | 0.5342 | 0.026* | |
H3N4 | 0.7355 | 0.0639 | 0.6255 | 0.026* | |
C14 | 0.7164 (2) | 0.13568 (10) | 0.81519 (18) | 0.0222 (4) | |
C24 | 0.6866 (2) | 0.14652 (8) | 0.68190 (16) | 0.0170 (4) | |
H24 | 0.7312 | 0.1869 | 0.6613 | 0.020* | |
C34 | 0.4994 (2) | 0.14464 (9) | 0.65217 (18) | 0.0206 (4) | |
H341 | 0.4392 | 0.1767 | 0.6946 | 0.025* | |
H342 | 0.4830 | 0.1509 | 0.5672 | 0.025* | |
O1W | 0.1442 (3) | 0.15636 (10) | 0.90106 (18) | 0.0459 (5) | |
H101 | 0.120 (4) | 0.1429 (13) | 0.8358 (12) | 0.055* | |
H102 | 0.214 (3) | 0.1837 (10) | 0.893 (3) | 0.055* | |
O2W | 0.3502 (3) | 0.32032 (10) | 0.64632 (18) | 0.0458 (5) | |
H201 | 0.375 (4) | 0.3438 (11) | 0.5931 (19) | 0.055* | |
H202 | 0.275 (3) | 0.2946 (10) | 0.647 (3) | 0.055* | |
O3W | 0.3903 (3) | 0.24343 (9) | 0.8940 (2) | 0.0556 (6) | |
H301 | 0.471 (3) | 0.2209 (12) | 0.881 (3) | 0.067* | |
H302 | 0.387 (5) | 0.2801 (2) | 0.903 (3) | 0.067* | |
O4W | 0.4100 (3) | 0.24912 (9) | 0.3641 (2) | 0.0484 (5) | |
H401 | 0.5050 (17) | 0.2340 (13) | 0.369 (3) | 0.058* | |
H402 | 0.400 (4) | 0.2853 (4) | 0.378 (3) | 0.058* | |
O5W | 0.1080 (3) | 0.23188 (9) | 0.6149 (2) | 0.0516 (5) | |
H501 | 0.015 (2) | 0.2476 (15) | 0.625 (3) | 0.062* | |
H502 | 0.101 (4) | 0.1956 (3) | 0.628 (3) | 0.062* | |
O6W | 0.0869 (3) | 0.23137 (9) | 0.1416 (2) | 0.0541 (6) | |
H601 | 0.005 (3) | 0.2519 (14) | 0.121 (3) | 0.065* | |
H602 | 0.070 (5) | 0.2062 (12) | 0.090 (2) | 0.065* | |
N11 | −0.0010 (3) | 0.48584 (11) | 0.1360 (2) | 0.0287 (4) | |
H11N | −0.079 (2) | 0.4875 (11) | 0.1954 (15) | 0.034* | |
H21N | 0.061 (3) | 0.5205 (7) | 0.135 (2) | 0.034* | |
H31N | −0.047 (3) | 0.4685 (10) | 0.0707 (13) | 0.034* | |
H41N | 0.082 (2) | 0.4585 (8) | 0.151 (2) | 0.034* | |
N21 | 0.4818 (3) | 0.48693 (10) | 0.1269 (2) | 0.0308 (4) | |
H12N | 0.561 (2) | 0.4625 (10) | 0.094 (2) | 0.037* | |
H22N | 0.430 (3) | 0.4906 (12) | 0.0554 (11) | 0.037* | |
H32N | 0.533 (3) | 0.5157 (8) | 0.1717 (19) | 0.037* | |
H42N | 0.404 (2) | 0.4662 (10) | 0.1710 (19) | 0.037* | |
N31 | −0.0191 (3) | 0.49157 (10) | 0.6208 (2) | 0.0290 (4) | |
H13N | −0.082 (3) | 0.5140 (10) | 0.5697 (17) | 0.035* | |
H23N | 0.049 (3) | 0.5217 (8) | 0.648 (2) | 0.035* | |
H33N | −0.076 (3) | 0.4807 (11) | 0.6875 (13) | 0.035* | |
H43N | 0.009 (3) | 0.4602 (8) | 0.5727 (18) | 0.035* | |
N41 | 0.4999 (3) | 0.49163 (10) | 0.61198 (19) | 0.0271 (4) | |
H14N | 0.578 (2) | 0.4613 (8) | 0.616 (2) | 0.033* | |
H24N | 0.4064 (19) | 0.4864 (11) | 0.5656 (18) | 0.033* | |
H34N | 0.575 (2) | 0.5184 (8) | 0.581 (2) | 0.033* | |
H44N | 0.481 (3) | 0.4991 (11) | 0.6897 (6) | 0.033* | |
N51 | 0.1396 (3) | 0.16470 (10) | 0.38432 (19) | 0.0330 (5) | |
H15N | 0.144 (3) | 0.1557 (12) | 0.3059 (6) | 0.040* | |
H25N | 0.0454 (19) | 0.1877 (9) | 0.396 (2) | 0.040* | |
H35N | 0.205 (3) | 0.1970 (8) | 0.365 (2) | 0.040* | |
H45N | 0.192 (3) | 0.1316 (7) | 0.415 (2) | 0.040* | |
N61 | 0.3604 (3) | 0.31310 (10) | 0.13534 (19) | 0.0349 (5) | |
H16N | 0.373 (3) | 0.3327 (10) | 0.0653 (12) | 0.042* | |
H26N | 0.4595 (17) | 0.3005 (11) | 0.169 (2) | 0.042* | |
H36N | 0.284 (3) | 0.2822 (8) | 0.132 (2) | 0.042* | |
H46N | 0.368 (3) | 0.3477 (7) | 0.178 (2) | 0.042* |
U11 | U22 | U33 | U12 | U13 | U23 | |
P1 | 0.0146 (2) | 0.0234 (4) | 0.0213 (3) | −0.0017 (2) | 0.00079 (19) | −0.0040 (2) |
O11 | 0.0637 (13) | 0.0399 (11) | 0.0280 (9) | 0.0078 (10) | −0.0053 (8) | −0.0127 (8) |
O21 | 0.0368 (8) | 0.0322 (10) | 0.0192 (8) | 0.0036 (7) | 0.0014 (6) | −0.0046 (6) |
O31 | 0.0391 (9) | 0.0402 (10) | 0.0206 (8) | 0.0099 (8) | 0.0001 (7) | 0.0120 (7) |
O41 | 0.0149 (6) | 0.0216 (7) | 0.0289 (8) | −0.0036 (5) | −0.0035 (5) | 0.0063 (6) |
O51 | 0.0169 (6) | 0.0391 (9) | 0.0271 (8) | 0.0037 (6) | −0.0001 (6) | −0.0080 (7) |
O61 | 0.0355 (9) | 0.0262 (9) | 0.0370 (10) | −0.0078 (7) | 0.0008 (7) | 0.0037 (7) |
N1 | 0.0178 (7) | 0.0281 (9) | 0.0158 (8) | −0.0005 (7) | 0.0008 (6) | −0.0011 (7) |
C11 | 0.0179 (8) | 0.0254 (10) | 0.0182 (10) | −0.0004 (8) | −0.0003 (7) | 0.0010 (8) |
C21 | 0.0174 (8) | 0.0192 (9) | 0.0199 (9) | 0.0000 (7) | −0.0006 (7) | 0.0002 (7) |
C31 | 0.0158 (8) | 0.0189 (9) | 0.0270 (11) | 0.0007 (7) | −0.0025 (7) | 0.0032 (8) |
P2 | 0.0158 (2) | 0.0229 (3) | 0.0206 (3) | −0.0010 (2) | 0.00058 (18) | 0.0028 (2) |
O12 | 0.0377 (9) | 0.0379 (9) | 0.0239 (8) | 0.0098 (8) | 0.0040 (7) | −0.0099 (7) |
O22 | 0.0372 (8) | 0.0348 (9) | 0.0216 (8) | 0.0074 (8) | 0.0014 (6) | 0.0042 (7) |
O32 | 0.0613 (12) | 0.0396 (11) | 0.0245 (9) | 0.0051 (9) | 0.0064 (8) | 0.0108 (7) |
O42 | 0.0170 (6) | 0.0239 (7) | 0.0276 (8) | −0.0036 (6) | 0.0045 (5) | −0.0065 (6) |
O52 | 0.0329 (9) | 0.0267 (8) | 0.0369 (10) | −0.0070 (7) | 0.0007 (7) | 0.0008 (7) |
O62 | 0.0172 (7) | 0.0352 (9) | 0.0290 (8) | 0.0034 (6) | 0.0008 (6) | 0.0063 (7) |
N2 | 0.0188 (8) | 0.0318 (10) | 0.0171 (8) | −0.0008 (7) | 0.0014 (6) | 0.0021 (7) |
C12 | 0.0164 (9) | 0.0300 (11) | 0.0172 (10) | −0.0007 (8) | 0.0025 (7) | 0.0003 (8) |
C22 | 0.0171 (8) | 0.0194 (9) | 0.0192 (9) | −0.0004 (7) | 0.0012 (7) | −0.0021 (7) |
C32 | 0.0167 (9) | 0.0238 (10) | 0.0249 (10) | −0.0025 (8) | 0.0068 (8) | −0.0054 (8) |
P3 | 0.0130 (2) | 0.0175 (2) | 0.0212 (3) | −0.0010 (2) | 0.00053 (18) | 0.0008 (2) |
O13 | 0.0496 (11) | 0.0433 (11) | 0.0277 (9) | 0.0081 (9) | 0.0036 (8) | 0.0116 (8) |
O23 | 0.0310 (8) | 0.0336 (9) | 0.0253 (8) | 0.0038 (7) | 0.0012 (6) | −0.0094 (7) |
O33 | 0.0127 (6) | 0.0205 (7) | 0.0280 (8) | −0.0019 (5) | 0.0035 (5) | −0.0042 (6) |
O43 | 0.0246 (7) | 0.0212 (7) | 0.0386 (10) | −0.0023 (6) | −0.0060 (7) | −0.0049 (7) |
O53 | 0.0287 (7) | 0.0294 (8) | 0.0193 (7) | 0.0008 (7) | 0.0025 (6) | 0.0020 (7) |
O63 | 0.0150 (6) | 0.0239 (7) | 0.0345 (8) | 0.0012 (6) | 0.0005 (6) | 0.0047 (6) |
N3 | 0.0170 (7) | 0.0237 (9) | 0.0184 (8) | −0.0016 (7) | −0.0011 (6) | 0.0005 (7) |
C13 | 0.0180 (9) | 0.0262 (10) | 0.0206 (10) | −0.0041 (8) | 0.0019 (7) | −0.0006 (8) |
C23 | 0.0158 (8) | 0.0176 (9) | 0.0165 (9) | −0.0019 (7) | 0.0015 (7) | −0.0014 (7) |
C33 | 0.0140 (8) | 0.0183 (9) | 0.0251 (10) | 0.0017 (7) | 0.0023 (7) | −0.0017 (8) |
P4 | 0.0142 (2) | 0.0161 (3) | 0.0212 (3) | −0.00002 (19) | −0.00114 (19) | −0.0001 (2) |
O14 | 0.0302 (8) | 0.0300 (9) | 0.0291 (8) | 0.0040 (7) | −0.0031 (6) | 0.0073 (7) |
O24 | 0.0530 (12) | 0.0443 (11) | 0.0256 (9) | 0.0103 (9) | −0.0032 (8) | −0.0134 (8) |
O34 | 0.0167 (6) | 0.0231 (8) | 0.0249 (8) | −0.0030 (5) | −0.0045 (5) | 0.0045 (6) |
O44 | 0.0262 (7) | 0.0178 (7) | 0.0365 (9) | −0.0034 (6) | 0.0047 (6) | 0.0014 (6) |
O54 | 0.0171 (6) | 0.0233 (7) | 0.0373 (9) | 0.0019 (6) | −0.0023 (6) | −0.0049 (7) |
O64 | 0.0298 (7) | 0.0281 (8) | 0.0206 (8) | 0.0010 (7) | −0.0050 (6) | −0.0011 (6) |
N4 | 0.0160 (7) | 0.0268 (9) | 0.0214 (9) | −0.0027 (7) | 0.0000 (6) | −0.0016 (7) |
C14 | 0.0168 (8) | 0.0295 (11) | 0.0204 (10) | −0.0045 (8) | −0.0027 (7) | 0.0008 (8) |
C24 | 0.0143 (8) | 0.0171 (8) | 0.0196 (9) | −0.0036 (7) | −0.0036 (7) | 0.0030 (7) |
C34 | 0.0166 (8) | 0.0210 (10) | 0.0243 (10) | −0.0013 (7) | −0.0032 (7) | 0.0046 (8) |
O1W | 0.0534 (12) | 0.0457 (12) | 0.0386 (11) | −0.0068 (9) | −0.0034 (9) | −0.0065 (9) |
O2W | 0.0564 (13) | 0.0452 (13) | 0.0357 (10) | −0.0048 (10) | 0.0055 (9) | 0.0051 (9) |
O3W | 0.0529 (13) | 0.0343 (12) | 0.0796 (16) | 0.0122 (10) | 0.0019 (11) | −0.0111 (11) |
O4W | 0.0518 (13) | 0.0272 (10) | 0.0662 (13) | 0.0018 (9) | −0.0040 (11) | −0.0103 (10) |
O5W | 0.0482 (12) | 0.0319 (10) | 0.0748 (15) | 0.0073 (10) | 0.0102 (11) | 0.0144 (11) |
O6W | 0.0524 (13) | 0.0286 (10) | 0.0813 (17) | 0.0034 (10) | −0.0013 (12) | 0.0093 (11) |
N11 | 0.0226 (9) | 0.0321 (11) | 0.0314 (11) | 0.0005 (8) | 0.0026 (7) | −0.0046 (9) |
N21 | 0.0235 (9) | 0.0284 (11) | 0.0406 (11) | 0.0017 (8) | 0.0005 (8) | −0.0009 (9) |
N31 | 0.0268 (10) | 0.0232 (10) | 0.0369 (11) | −0.0042 (8) | 0.0016 (8) | 0.0015 (8) |
N41 | 0.0261 (9) | 0.0280 (10) | 0.0272 (10) | 0.0023 (8) | −0.0031 (8) | −0.0008 (9) |
N51 | 0.0449 (12) | 0.0259 (11) | 0.0282 (10) | −0.0002 (9) | 0.0035 (9) | −0.0020 (9) |
N61 | 0.0436 (12) | 0.0321 (12) | 0.0290 (11) | 0.0024 (10) | −0.0008 (9) | 0.0045 (9) |
P1—O61 | 1.4871 (17) | P4—O54 | 1.5181 (15) |
P1—O51 | 1.5100 (16) | P4—O64 | 1.5220 (17) |
P1—O21 | 1.5540 (17) | P4—O34 | 1.6211 (14) |
P1—O41 | 1.6102 (14) | O14—C14 | 1.246 (3) |
O11—C11 | 1.245 (3) | O24—C14 | 1.245 (3) |
O21—H210 | 0.8300 | O34—C34 | 1.424 (2) |
O31—C11 | 1.247 (3) | N4—C24 | 1.485 (3) |
O41—C31 | 1.444 (2) | N4—H1N4 | 0.9000 |
N1—C21 | 1.486 (3) | N4—H2N4 | 0.9000 |
N1—H1N1 | 0.9000 | N4—H3N4 | 0.9000 |
N1—H2N1 | 0.9000 | C14—C24 | 1.545 (3) |
N1—H3N1 | 0.9000 | C24—C34 | 1.510 (3) |
C11—C21 | 1.545 (3) | C24—H24 | 0.9900 |
C21—C31 | 1.523 (3) | C34—H341 | 0.9800 |
C21—H21 | 0.9900 | C34—H342 | 0.9800 |
C31—H311 | 0.9800 | O1W—H101 | 0.820 (2) |
C31—H312 | 0.9800 | O1W—H102 | 0.820 (2) |
P2—O52 | 1.4804 (18) | O2W—H201 | 0.820 (2) |
P2—O62 | 1.5046 (16) | O2W—H202 | 0.820 (2) |
P2—O22 | 1.5591 (16) | O3W—H301 | 0.820 (2) |
P2—O42 | 1.6147 (14) | O3W—H302 | 0.819 (2) |
O12—C12 | 1.239 (3) | O4W—H401 | 0.820 (2) |
O22—H220 | 0.8300 | O4W—H402 | 0.820 (2) |
O32—C12 | 1.247 (3) | O5W—H501 | 0.820 (2) |
O42—C32 | 1.438 (2) | O5W—H502 | 0.819 (2) |
N2—C22 | 1.478 (3) | O6W—H601 | 0.820 (2) |
N2—H1N2 | 0.9000 | O6W—H602 | 0.819 (2) |
N2—H2N2 | 0.9000 | N11—H11N | 0.911 (3) |
N2—H3N2 | 0.9000 | N11—H21N | 0.910 (3) |
C12—C22 | 1.547 (3) | N11—H31N | 0.909 (3) |
C22—C32 | 1.520 (3) | N11—H41N | 0.909 (3) |
C22—H22 | 0.9900 | N21—H12N | 0.909 (3) |
C32—H321 | 0.9800 | N21—H22N | 0.910 (3) |
C32—H322 | 0.9800 | N21—H32N | 0.910 (3) |
P3—O43 | 1.4964 (16) | N21—H42N | 0.911 (3) |
P3—O53 | 1.5227 (16) | N31—H13N | 0.909 (3) |
P3—O63 | 1.5252 (15) | N31—H23N | 0.909 (3) |
P3—O33 | 1.6195 (14) | N31—H33N | 0.909 (3) |
O13—C13 | 1.238 (3) | N31—H43N | 0.909 (3) |
O23—C13 | 1.242 (3) | N41—H14N | 0.910 (3) |
O33—C33 | 1.436 (2) | N41—H24N | 0.910 (3) |
N3—C23 | 1.492 (2) | N41—H34N | 0.910 (3) |
N3—H1N3 | 0.9000 | N41—H44N | 0.908 (3) |
N3—H2N3 | 0.9000 | N51—H15N | 0.910 (3) |
N3—H3N3 | 0.9000 | N51—H25N | 0.910 (3) |
C13—C23 | 1.552 (3) | N51—H35N | 0.910 (3) |
C23—C33 | 1.510 (3) | N51—H45N | 0.910 (3) |
C23—H23 | 0.9900 | N61—H16N | 0.910 (3) |
C33—H331 | 0.9800 | N61—H26N | 0.910 (3) |
C33—H332 | 0.9800 | N61—H36N | 0.911 (3) |
P4—O44 | 1.5012 (16) | N61—H46N | 0.909 (3) |
O61—P1—O51 | 117.26 (9) | C33—C23—H23 | 108.4 |
O61—P1—O21 | 111.12 (9) | C13—C23—H23 | 108.4 |
O51—P1—O21 | 109.46 (9) | O33—C33—C23 | 108.33 (15) |
O61—P1—O41 | 104.36 (9) | O33—C33—H331 | 110.0 |
O51—P1—O41 | 108.11 (9) | C23—C33—H331 | 110.0 |
O21—P1—O41 | 105.75 (9) | O33—C33—H332 | 110.0 |
P1—O21—H210 | 109.5 | C23—C33—H332 | 110.0 |
C31—O41—P1 | 118.60 (11) | H331—C33—H332 | 108.4 |
C21—N1—H1N1 | 109.5 | O44—P4—O54 | 114.15 (9) |
C21—N1—H2N1 | 109.5 | O44—P4—O64 | 114.23 (9) |
H1N1—N1—H2N1 | 109.5 | O54—P4—O64 | 110.11 (9) |
C21—N1—H3N1 | 109.5 | O44—P4—O34 | 103.46 (8) |
H1N1—N1—H3N1 | 109.5 | O54—P4—O34 | 106.99 (8) |
H2N1—N1—H3N1 | 109.5 | O64—P4—O34 | 107.19 (8) |
O11—C11—O31 | 125.3 (2) | C34—O34—P4 | 119.78 (12) |
O11—C11—C21 | 117.25 (19) | C24—N4—H1N4 | 109.5 |
O31—C11—C21 | 117.45 (18) | C24—N4—H2N4 | 109.5 |
N1—C21—C31 | 109.68 (15) | H1N4—N4—H2N4 | 109.5 |
N1—C21—C11 | 110.21 (16) | C24—N4—H3N4 | 109.5 |
C31—C21—C11 | 112.58 (16) | H1N4—N4—H3N4 | 109.5 |
N1—C21—H21 | 108.1 | H2N4—N4—H3N4 | 109.5 |
C31—C21—H21 | 108.1 | O24—C14—O14 | 125.3 (2) |
C11—C21—H21 | 108.1 | O24—C14—C24 | 116.46 (19) |
O41—C31—C21 | 108.30 (15) | O14—C14—C24 | 118.18 (19) |
O41—C31—H311 | 110.0 | N4—C24—C34 | 110.12 (15) |
C21—C31—H311 | 110.0 | N4—C24—C14 | 110.02 (16) |
O41—C31—H312 | 110.0 | C34—C24—C14 | 111.08 (16) |
C21—C31—H312 | 110.0 | N4—C24—H24 | 108.5 |
H311—C31—H312 | 108.4 | C34—C24—H24 | 108.5 |
O52—P2—O62 | 117.76 (9) | C14—C24—H24 | 108.5 |
O52—P2—O22 | 110.78 (10) | O34—C34—C24 | 108.65 (15) |
O62—P2—O22 | 109.19 (9) | O34—C34—H341 | 110.0 |
O52—P2—O42 | 104.63 (9) | C24—C34—H341 | 110.0 |
O62—P2—O42 | 108.00 (8) | O34—C34—H342 | 110.0 |
O22—P2—O42 | 105.68 (9) | C24—C34—H342 | 110.0 |
P2—O22—H220 | 109.5 | H341—C34—H342 | 108.3 |
C32—O42—P2 | 118.95 (12) | H101—O1W—H102 | 109 (3) |
C22—N2—H1N2 | 109.5 | H201—O2W—H202 | 128 (3) |
C22—N2—H2N2 | 109.5 | H301—O3W—H302 | 131 (4) |
H1N2—N2—H2N2 | 109.5 | H401—O4W—H402 | 118 (4) |
C22—N2—H3N2 | 109.5 | H501—O5W—H502 | 109 (4) |
H1N2—N2—H3N2 | 109.5 | H601—O6W—H602 | 93 (3) |
H2N2—N2—H3N2 | 109.5 | H11N—N11—H21N | 110 (2) |
O12—C12—O32 | 124.9 (2) | H11N—N11—H31N | 110 (2) |
O12—C12—C22 | 118.38 (19) | H21N—N11—H31N | 124 (2) |
O32—C12—C22 | 116.75 (19) | H11N—N11—H41N | 112 (2) |
N2—C22—C32 | 109.94 (16) | H21N—N11—H41N | 100 (2) |
N2—C22—C12 | 110.15 (16) | H31N—N11—H41N | 99 (2) |
C32—C22—C12 | 112.21 (16) | H12N—N21—H22N | 90 (2) |
N2—C22—H22 | 108.1 | H12N—N21—H32N | 110 (2) |
C32—C22—H22 | 108.1 | H22N—N21—H32N | 129 (2) |
C12—C22—H22 | 108.1 | H12N—N21—H42N | 113 (2) |
O42—C32—C22 | 108.40 (15) | H22N—N21—H42N | 103 (2) |
O42—C32—H321 | 110.0 | H32N—N21—H42N | 110 (2) |
C22—C32—H321 | 110.0 | H13N—N31—H23N | 98 (2) |
O42—C32—H322 | 110.0 | H13N—N31—H33N | 114 (2) |
C22—C32—H322 | 110.0 | H23N—N31—H33N | 102 (2) |
H321—C32—H322 | 108.4 | H13N—N31—H43N | 100 (2) |
O43—P3—O53 | 114.51 (9) | H23N—N31—H43N | 128 (2) |
O43—P3—O63 | 114.18 (9) | H33N—N31—H43N | 114 (2) |
O53—P3—O63 | 110.19 (9) | H14N—N41—H24N | 118 (2) |
O43—P3—O33 | 103.13 (8) | H14N—N41—H34N | 93 (2) |
O53—P3—O33 | 106.90 (8) | H24N—N41—H34N | 113 (2) |
O63—P3—O33 | 107.16 (8) | H14N—N41—H44N | 102 (2) |
C33—O33—P3 | 118.96 (11) | H24N—N41—H44N | 117 (2) |
C23—N3—H1N3 | 109.5 | H34N—N41—H44N | 111 (2) |
C23—N3—H2N3 | 109.5 | H15N—N51—H25N | 108 (2) |
H1N3—N3—H2N3 | 109.5 | H15N—N51—H35N | 85 (2) |
C23—N3—H3N3 | 109.5 | H25N—N51—H35N | 93 (2) |
H1N3—N3—H3N3 | 109.5 | H15N—N51—H45N | 100 (2) |
H2N3—N3—H3N3 | 109.5 | H25N—N51—H45N | 139 (2) |
O13—C13—O23 | 125.8 (2) | H35N—N51—H45N | 118 (2) |
O13—C13—C23 | 116.62 (19) | H16N—N61—H26N | 114 (2) |
O23—C13—C23 | 117.55 (18) | H16N—N61—H36N | 114 (2) |
N3—C23—C33 | 109.88 (15) | H26N—N61—H36N | 110 (2) |
N3—C23—C13 | 109.87 (15) | H16N—N61—H46N | 93 (2) |
C33—C23—C13 | 111.68 (15) | H26N—N61—H46N | 89 (2) |
N3—C23—H23 | 108.4 | H36N—N61—H46N | 134 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O21—H210···O1Wi | 0.83 | 1.79 | 2.578 (3) | 159 |
N1—H1N1···O51ii | 0.90 | 1.88 | 2.782 (2) | 177 |
N1—H2N1···O14i | 0.90 | 2.16 | 2.985 (2) | 153 |
N1—H2N1···O24i | 0.90 | 2.37 | 3.179 (3) | 149 |
N1—H3N1···O52iii | 0.90 | 1.97 | 2.762 (2) | 146 |
O22—H220···O2Wiv | 0.83 | 1.75 | 2.579 (3) | 173 |
N2—H1N2···O62v | 0.90 | 1.89 | 2.787 (2) | 178 |
N2—H2N2···O23i | 0.90 | 2.17 | 2.984 (2) | 150 |
N2—H2N2···O13i | 0.90 | 2.34 | 3.157 (3) | 152 |
N2—H3N2···O61vi | 0.90 | 1.96 | 2.765 (3) | 148 |
N3—H1N3···O63v | 0.90 | 1.88 | 2.775 (2) | 174 |
N3—H2N3···O12 | 0.90 | 2.21 | 3.044 (2) | 155 |
N3—H2N3···O32 | 0.90 | 2.40 | 3.203 (3) | 148 |
N3—H3N3···O44vii | 0.90 | 2.04 | 2.806 (2) | 143 |
N4—H1N4···O54ii | 0.90 | 1.88 | 2.774 (2) | 174 |
N4—H2N4···O31 | 0.90 | 2.21 | 3.042 (3) | 153 |
N4—H2N4···O11 | 0.90 | 2.39 | 3.201 (3) | 150 |
N4—H3N4···O43viii | 0.90 | 2.04 | 2.818 (2) | 144 |
N11—H11N···O44ix | 0.91 (1) | 1.85 (1) | 2.752 (3) | 172 (2) |
N11—H21N···O14vii | 0.91 (1) | 1.96 (1) | 2.856 (3) | 168 (2) |
N11—H31N···O42v | 0.91 (1) | 2.43 (2) | 3.116 (3) | 132 (2) |
N11—H31N···O12v | 0.91 (1) | 2.51 (2) | 3.069 (3) | 120 (2) |
N11—H41N···O53v | 0.91 (1) | 1.94 (1) | 2.798 (3) | 156 (2) |
N21—H12N···O12 | 0.91 (1) | 1.99 (1) | 2.836 (3) | 154 (2) |
N21—H22N···O52v | 0.91 (1) | 2.03 (1) | 2.895 (3) | 159 (2) |
N21—H32N···O34vii | 0.91 (1) | 2.28 (1) | 3.144 (3) | 159 (2) |
N21—H42N···O53v | 0.91 (1) | 1.96 (1) | 2.869 (3) | 172 (2) |
N31—H13N···O64ix | 0.91 (1) | 2.01 (1) | 2.888 (3) | 163 (2) |
N31—H23N···O31vii | 0.91 (1) | 1.96 (1) | 2.838 (3) | 162 (2) |
N31—H33N···O61ix | 0.91 (1) | 2.04 (1) | 2.879 (3) | 153 (2) |
N31—H43N···O33v | 0.91 (1) | 2.22 (1) | 3.121 (3) | 171 (2) |
N41—H14N···O23 | 0.91 (1) | 1.95 (1) | 2.845 (3) | 170 (2) |
N41—H24N···O43v | 0.91 (1) | 1.86 (1) | 2.733 (3) | 161 (2) |
N41—H34N···O64vii | 0.91 (1) | 1.90 (1) | 2.809 (3) | 173 (2) |
N41—H44N···O41vii | 0.91 (1) | 2.42 (2) | 3.099 (3) | 132 (2) |
N51—H15N···O51 | 0.91 (1) | 1.90 (1) | 2.749 (3) | 155 (2) |
N51—H15N···O6W | 0.91 (1) | 2.54 (2) | 3.146 (3) | 124 (2) |
N51—H25N···O11v | 0.91 (1) | 2.74 (2) | 3.481 (3) | 140 (2) |
N51—H35N···O4W | 0.91 (1) | 1.98 (1) | 2.841 (3) | 157 (3) |
N51—H45N···O64 | 0.91 (1) | 1.81 (1) | 2.709 (3) | 168 (3) |
N61—H16N···O62v | 0.91 (1) | 1.86 (1) | 2.768 (3) | 173 (3) |
N61—H26N···O32 | 0.91 (1) | 2.69 (2) | 3.450 (3) | 142 (2) |
N61—H36N···O6W | 0.91 (1) | 1.92 (1) | 2.812 (3) | 166 (3) |
N61—H46N···O53v | 0.91 (1) | 1.92 (2) | 2.718 (3) | 145 (2) |
O1W—H101···O54 | 0.82 (1) | 1.94 (1) | 2.739 (3) | 166 (3) |
O1W—H102···O3W | 0.82 (1) | 1.92 (1) | 2.734 (3) | 172 (3) |
O2W—H201···O63v | 0.82 (1) | 1.97 (1) | 2.725 (3) | 153 (3) |
O2W—H202···O5W | 0.82 (1) | 1.95 (1) | 2.755 (3) | 169 (3) |
O3W—H301···O24 | 0.82 (1) | 1.89 (1) | 2.690 (3) | 166 (4) |
O3W—H302···O62x | 0.82 (1) | 2.02 (1) | 2.840 (3) | 178 (4) |
O4W—H401···O11 | 0.82 (1) | 1.95 (1) | 2.752 (3) | 166 (3) |
O4W—H402···O63v | 0.82 (1) | 1.96 (1) | 2.772 (2) | 174 (3) |
O5W—H501···O13v | 0.82 (1) | 1.90 (1) | 2.701 (3) | 166 (4) |
O5W—H502···O54 | 0.82 (1) | 1.99 (1) | 2.799 (3) | 170 (3) |
O6W—H601···O32v | 0.82 (1) | 1.94 (1) | 2.725 (3) | 160 (3) |
O6W—H602···O1Wi | 0.82 (1) | 2.48 (2) | 3.221 (3) | 152 (3) |
O3W—H302···N61xi | 0.82 (1) | 2.74 (3) | 3.146 (3) | 112 (3) |
N21—H32N···O44vii | 0.91 (1) | 2.47 (2) | 3.117 (3) | 128 (2) |
N31—H43N···O43v | 0.91 (1) | 2.62 (2) | 3.133 (3) | 116 (2) |
N61—H26N···O4W | 0.91 (1) | 2.52 (2) | 2.977 (3) | 112 (2) |
Symmetry codes: (i) x, y, z−1; (ii) x+1, y, z; (iii) −x+2, y−1/2, −z; (iv) x+1, y, z−1; (v) x−1, y, z; (vi) −x+1, y+1/2, −z; (vii) −x+1, y+1/2, −z+1; (viii) −x+2, y−1/2, −z+1; (ix) −x, y+1/2, −z+1; (x) x−1, y, z+1; (xi) x, y, z+1. |
Experimental details
(100_K_whole-dataset) | (100_K_average) | (150_K_whole-dataset) | (200_K_whole-dataset) | |
Crystal data | ||||
Chemical formula | C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | C6H13N2O12P2·H6NO·2(H4N)·2(H2O) | C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) | C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) |
Mr | 475.30 | 475.30 | 475.30 | 475.30 |
Crystal system, space group | Monoclinic, P21 | Orthorhombic, P212121 | Monoclinic, P21 | Monoclinic, P21 |
Temperature (K) | 100 | 100 | 50 | 200 |
a, b, c (Å) | 7.851 (3), 21.976 (5), 11.332 (4) | 7.851 (3), 21.976 (5), 5.666 (2) | 7.851 (2), 22.048 (4), 11.325 (3) | 7.855 (2), 22.105 (4), 11.317 (3) |
α, β, γ (°) | 90, 90.00 (3), 90 | 90, 90, 90 | 90, 90.04 (2), 90 | 90, 90.05 (2), 90 |
V (Å3) | 1955.2 (11) | 977.6 (6) | 1960.3 (8) | 1965.0 (8) |
Z | 4 | 2 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.31 | 0.31 | 0.31 | 0.30 |
Crystal size (mm) | 0.40 × 0.18 × 0.10 | 0.40 × 0.18 × 0.10 | 0.40 × 0.18 × 0.10 | 0.40 × 0.18 × 0.10 |
Data collection | ||||
Diffractometer | Xcalibur PX diffractometer | Xcalibur PX diffractometer | KM4CCD diffractometer | KM4CCD diffractometer |
Absorption correction | Numerical CrysAlis RED, ver. 1.171, Oxford Diffraction Poland (1995-2003) | Numerical CrysAlis RED, ver. 1.171, Oxford Diffraction Poland (1995-2003) | Numerical | Numerical |
Tmin, Tmax | 0.888, 0.970 | 0.888, 0.970 | 0.889, 0.966 | 0.889, 0.966 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 49395, 16051, 9264 | 24631, 5369, 4404 | 49468, 16153, 9474 | 45319, 16120, 8153 |
Rint | 0.043 | 0.046 | 0.034 | 0.034 |
(sin θ/λ)max (Å−1) | 0.877 | 0.875 | 0.877 | 0.876 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.087, 1.15 | 0.039, 0.103, 1.02 | 0.045, 0.107, 1.00 | 0.044, 0.092, 1.01 |
No. of reflections | 16051 | 5369 | 16153 | 16120 |
No. of parameters | 619 | 184 | 595 | 619 |
No. of restraints | 37 | 26 | 37 | 37 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.41, −0.45 | 0.36, −0.42 | 0.41, −0.46 | 0.34, −0.41 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0.03 (5) | −0.16 (8) | 0.06 (5) | 0.02 (5) |
(250_K_whole-dataset) | |
Crystal data | |
Chemical formula | C3H7NO6P·C3H6NO6P·3(H4N)·3(H2O) |
Mr | 475.30 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 250 |
a, b, c (Å) | 7.861 (2), 22.163 (4), 11.315 (3) |
α, β, γ (°) | 90, 90.06 (2), 90 |
V (Å3) | 1971.3 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.30 |
Crystal size (mm) | 0.40 × 0.18 × 0.10 |
Data collection | |
Diffractometer | KM4CCD diffractometer |
Absorption correction | Numerical |
Tmin, Tmax | 0.889, 0.966 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 47886, 16208, 9135 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.876 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.122, 1.01 |
No. of reflections | 16208 |
No. of parameters | 619 |
No. of restraints | 37 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.36, −0.42 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0.12 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
O21—H210···O3Wi | 0.84 | 1.74 | 2.561 (2) | 166.2 |
N1—H1N1···O41ii | 0.91 | 1.87 | 2.778 (2) | 178.3 |
N1—H2N1···O54iii | 0.91 | 2.19 | 2.992 (2) | 146.8 |
N1—H2N1···O64iii | 0.91 | 2.28 | 3.118 (3) | 152.4 |
N1—H3N1···O12iv | 0.91 | 1.95 | 2.767 (2) | 149.0 |
O22—H220···O1Wiii | 0.84 | 1.73 | 2.565 (3) | 170.1 |
N2—H1N2···O42v | 0.91 | 1.87 | 2.778 (2) | 173.9 |
N2—H2N2···O53iii | 0.91 | 2.16 | 2.991 (2) | 151.6 |
N2—H2N2···O63iii | 0.91 | 2.33 | 3.141 (3) | 148.9 |
N2—H3N2···O11vi | 0.91 | 1.95 | 2.752 (2) | 145.8 |
N3—H1N3···O43v | 0.91 | 1.87 | 2.769 (2) | 171.6 |
N3—H2N3···O52 | 0.91 | 2.25 | 3.065 (2) | 148.7 |
N3—H2N3···O51 | 0.91 | 2.33 | 3.164 (3) | 152.2 |
N3—H3N3···O14vii | 0.91 | 2.00 | 2.794 (2) | 144.9 |
N4—H1N4···O44ii | 0.91 | 1.87 | 2.777 (2) | 175.1 |
N4—H2N4···O62 | 0.91 | 2.23 | 3.070 (2) | 153.5 |
N4—H2N4···O61 | 0.91 | 2.36 | 3.173 (2) | 148.4 |
N4—H3N4···O13viii | 0.91 | 2.01 | 2.781 (2) | 142.1 |
N11—H11N···O52viii | 0.909 (3) | 1.927 (7) | 2.821 (3) | 167 (2) |
N11—H31N···O12ix | 0.909 (3) | 1.980 (11) | 2.831 (3) | 155 (2) |
N11—H41N···O34ii | 0.910 (3) | 2.246 (10) | 3.098 (3) | 156 (2) |
N21—H12N···O11x | 0.909 (3) | 1.998 (11) | 2.840 (3) | 154 (2) |
N21—H22N···O24x | 0.910 (3) | 1.995 (8) | 2.875 (3) | 162 (2) |
N21—H32N···O62ii | 0.909 (3) | 1.930 (7) | 2.824 (3) | 167 (2) |
N21—H42N···O33ix | 0.909 (3) | 2.286 (12) | 3.125 (3) | 153 (2) |
N31—H13N···O13ix | 0.910 (3) | 1.831 (5) | 2.738 (3) | 174 (2) |
N31—H23N···O53viii | 0.909 (3) | 1.951 (8) | 2.827 (3) | 161 (2) |
N31—H33N···O31ii | 0.909 (3) | 2.387 (16) | 3.103 (3) | 135.7 (19) |
N31—H33N···O62ii | 0.909 (3) | 2.50 (2) | 3.027 (3) | 117.2 (17) |
N31—H43N···O24ii | 0.910 (3) | 1.899 (7) | 2.794 (3) | 167 (2) |
N41—H14N···O54ii | 0.909 (3) | 1.927 (7) | 2.820 (3) | 166 (2) |
N41—H24N···O14x | 0.910 (3) | 1.849 (7) | 2.736 (3) | 164 (2) |
N41—H34N···O32ix | 0.909 (3) | 2.359 (17) | 3.073 (2) | 135.4 (19) |
N41—H44N···O23ix | 0.911 (3) | 1.903 (6) | 2.805 (3) | 170 (2) |
N51—H15N···O42 | 0.909 (3) | 1.865 (8) | 2.748 (3) | 163 (2) |
N51—H15N···O2W | 0.909 (3) | 2.61 (2) | 3.151 (3) | 119.0 (19) |
N51—H25N···O5W | 0.909 (3) | 1.917 (7) | 2.812 (3) | 168 (2) |
N51—H35N···O51ii | 0.911 (3) | 2.603 (11) | 3.454 (3) | 156 (2) |
N51—H45N···O23 | 0.910 (3) | 1.785 (4) | 2.695 (3) | 178 (2) |
N61—H16N···O41ii | 0.910 (3) | 1.858 (5) | 2.764 (3) | 173 (2) |
N61—H26N···O2W | 0.911 (3) | 1.918 (8) | 2.804 (3) | 164 (2) |
N61—H36N···O61 | 0.910 (3) | 2.576 (12) | 3.397 (3) | 150 (2) |
N61—H46N···O24ii | 0.910 (3) | 1.846 (11) | 2.701 (3) | 156 (2) |
O1W—H101···O43 | 0.820 (2) | 1.919 (6) | 2.728 (2) | 168 (3) |
O1W—H102···O4W | 0.820 (2) | 1.908 (4) | 2.725 (3) | 174 (3) |
O2W—H201···O61ii | 0.820 (2) | 1.920 (7) | 2.724 (3) | 167 (3) |
O2W—H202···O42 | 0.819 (2) | 2.17 (2) | 2.814 (2) | 135 (3) |
O2W—H202···O1Wiii | 0.819 (2) | 2.65 (2) | 3.251 (3) | 132 (3) |
O3W—H301···O44ii | 0.820 (2) | 1.918 (8) | 2.719 (2) | 165 (3) |
O3W—H302···O6Wii | 0.820 (2) | 1.931 (5) | 2.745 (3) | 172 (3) |
O4W—H401···O63 | 0.820 (2) | 1.891 (9) | 2.685 (3) | 163 (3) |
O4W—H402···O41xi | 0.819 (2) | 2.13 (2) | 2.803 (2) | 140 (3) |
O5W—H501···O51 | 0.820 (2) | 1.959 (9) | 2.756 (3) | 164 (3) |
O5W—H502···O44ii | 0.820 (2) | 1.978 (10) | 2.765 (2) | 161 (3) |
O6W—H601···O64 | 0.820 (2) | 1.906 (8) | 2.705 (3) | 164 (3) |
Symmetry codes: (i) x−1, y, z+1; (ii) x+1, y, z; (iii) x, y, z+1; (iv) −x+1, y+1/2, −z+2; (v) x−1, y, z; (vi) −x, y−1/2, −z+2; (vii) −x, y−1/2, −z+1; (viii) −x+1, y+1/2, −z+1; (ix) −x+2, y+1/2, −z+1; (x) x+2, y, z; (xi) x+1, y, z−1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H210···O7i | 0.84 | 1.68 | 2.501 (6) | 166.9 |
O2—H210···N7i | 0.84 | 1.95 | 2.773 (7) | 164.3 |
N1—H11···O1ii | 0.91 | 1.97 | 2.7725 (14) | 145.7 |
N1—H12···O4iii | 0.91 | 1.87 | 2.7749 (16) | 176.8 |
N1—H13···O5i | 0.91 | 2.21 | 3.0292 (17) | 150.3 |
N1—H13···O6i | 0.91 | 2.32 | 3.1482 (17) | 150.7 |
N2—H21···O3 | 0.906 (3) | 2.434 (12) | 3.0953 (17) | 130.0 (13) |
N2—H21···O5 | 0.906 (3) | 2.550 (15) | 2.9828 (16) | 109.9 (12) |
N2—H22···O2iv | 0.918 (3) | 1.946 (5) | 2.8462 (19) | 166.3 (15) |
N2—H23···O1v | 0.908 (3) | 1.890 (5) | 2.7835 (18) | 167.6 (15) |
N2—H24···O5vi | 0.909 (3) | 1.945 (6) | 2.8202 (15) | 161.0 (15) |
O7—H71···O4 | 0.820 (2) | 2.08 (2) | 2.801 (8) | 146 (4) |
O7—H71···O4 | 0.820 (2) | 2.08 (2) | 2.801 (8) | 146 (4) |
O7—H72···O81 | 0.820 (2) | 1.933 (13) | 2.744 (10) | 170 (4) |
O7—H72···O82 | 0.820 (2) | 2.054 (16) | 2.868 (15) | 172 (4) |
N7—H17···O4 | 0.913 (3) | 1.761 (11) | 2.666 (9) | 170 (3) |
N7—H17···O81vii | 0.913 (3) | 2.63 (3) | 3.106 (18) | 113 (2) |
N7—H27···O81 | 0.911 (3) | 1.849 (14) | 2.729 (10) | 162 (2) |
N7—H27···O82 | 0.911 (3) | 1.940 (17) | 2.819 (15) | 161 (2) |
N7—H37···O2iv | 0.913 (3) | 1.873 (9) | 2.773 (7) | 168 (3) |
N7—H47···O6viii | 0.911 (3) | 2.653 (15) | 3.480 (9) | 151 (2) |
O81—H82···O6 | 0.819 (2) | 1.937 (5) | 2.709 (5) | 156.8 (18) |
O82—H81···O4ix | 0.819 (2) | 1.997 (4) | 2.790 (6) | 162.8 (19) |
O81—H81···O4ix | 0.821 (2) | 1.997 (4) | 2.786 (4) | 161.0 (18) |
O82—H82···O6 | 0.820 (2) | 1.937 (5) | 2.734 (6) | 164 (2) |
Symmetry codes: (i) x, y, z+1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1, y, z; (iv) x, y, z−1; (v) x+1/2, −y+1/2, −z; (vi) x−1/2, −y+1/2, −z; (vii) −x+1/2, −y, z+1/2; (viii) x−1, y, z; (ix) −x+1/2, −y, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O21—H210···O1Wi | 0.84 | 1.74 | 2.567 (2) | 168.7 |
N1—H1N1···O51ii | 0.91 | 1.87 | 2.7773 (18) | 177.1 |
N1—H2N1···O14i | 0.91 | 2.16 | 2.989 (2) | 151.5 |
N1—H2N1···O24i | 0.91 | 2.34 | 3.153 (2) | 149.4 |
N1—H3N1···O52iii | 0.91 | 1.95 | 2.7546 (19) | 145.9 |
O22—H220···O2Wiv | 0.84 | 1.73 | 2.564 (2) | 173.4 |
N2—H1N2···O62v | 0.91 | 1.87 | 2.7789 (19) | 177.7 |
N2—H2N2···O23i | 0.91 | 2.18 | 2.9895 (19) | 148.4 |
N2—H2N2···O13i | 0.91 | 2.30 | 3.134 (2) | 151.7 |
N2—H3N2···O61vi | 0.91 | 1.95 | 2.7629 (19) | 148.0 |
N3—H1N3···O63v | 0.91 | 1.87 | 2.7753 (18) | 175.1 |
N3—H2N3···O12 | 0.91 | 2.21 | 3.0575 (19) | 154.1 |
N3—H2N3···O32 | 0.91 | 2.37 | 3.180 (2) | 148.1 |
N3—H3N3···O44vii | 0.91 | 2.01 | 2.7888 (18) | 142.3 |
N4—H1N4···O54ii | 0.91 | 1.86 | 2.7679 (18) | 176.0 |
N4—H2N4···O31 | 0.91 | 2.22 | 3.0596 (19) | 152.6 |
N4—H2N4···O11 | 0.91 | 2.37 | 3.186 (2) | 149.7 |
N4—H3N4···O43viii | 0.91 | 2.02 | 2.8059 (19) | 143.3 |
N11—H11N···O44ix | 0.911 (3) | 1.835 (4) | 2.745 (2) | 177 (2) |
N11—H21N···O14vii | 0.909 (3) | 1.949 (7) | 2.836 (2) | 165 (2) |
N11—H31N···O42v | 0.908 (3) | 2.439 (17) | 3.110 (2) | 130.8 (18) |
N11—H31N···O12v | 0.908 (3) | 2.50 (2) | 3.042 (3) | 118.5 (17) |
N11—H41N···O53v | 0.909 (3) | 1.919 (8) | 2.797 (2) | 162 (2) |
N21—H12N···O12 | 0.910 (3) | 1.943 (8) | 2.826 (2) | 163 (2) |
N21—H22N···O52v | 0.910 (3) | 1.989 (10) | 2.851 (3) | 158 (2) |
N21—H32N···O34vii | 0.909 (3) | 2.350 (14) | 3.140 (3) | 145 (2) |
N21—H42N···O53v | 0.911 (3) | 1.999 (9) | 2.872 (3) | 160 (2) |
N31—H13N···O64ix | 0.910 (3) | 2.001 (7) | 2.890 (3) | 165 (2) |
N31—H23N···O31vii | 0.909 (3) | 1.944 (8) | 2.827 (2) | 163 (2) |
N31—H33N···O61ix | 0.909 (3) | 1.999 (11) | 2.843 (3) | 154 (2) |
N31—H43N···O33v | 0.909 (3) | 2.231 (7) | 3.115 (2) | 164 (2) |
N41—H14N···O23 | 0.909 (3) | 1.940 (7) | 2.825 (2) | 164 (2) |
N41—H24N···O43v | 0.910 (3) | 1.843 (7) | 2.731 (2) | 164 (2) |
N41—H34N···O64vii | 0.911 (3) | 1.901 (5) | 2.803 (3) | 171 (2) |
N41—H44N···O41vii | 0.908 (3) | 2.343 (16) | 3.085 (2) | 138.8 (19) |
N51—H15N···O51 | 0.910 (3) | 1.881 (9) | 2.751 (2) | 159 (2) |
N51—H15N···O6W | 0.910 (3) | 2.57 (2) | 3.147 (3) | 122.3 (19) |
N51—H25N···O11v | 0.910 (3) | 2.629 (11) | 3.469 (3) | 153.8 (19) |
N51—H35N···O4W | 0.910 (3) | 1.921 (6) | 2.821 (3) | 169 (2) |
N51—H45N···O64 | 0.910 (3) | 1.808 (6) | 2.706 (2) | 169 (2) |
N61—H16N···O62v | 0.909 (3) | 1.861 (5) | 2.763 (2) | 171 (2) |
N61—H26N···O32 | 0.910 (3) | 2.594 (11) | 3.422 (3) | 151.6 (19) |
N61—H36N···O6W | 0.911 (3) | 1.917 (8) | 2.802 (3) | 163 (2) |
N61—H46N···O53v | 0.910 (3) | 1.878 (13) | 2.706 (2) | 150 (2) |
O1W—H101···O54 | 0.820 (2) | 1.922 (6) | 2.734 (2) | 170 (3) |
O1W—H102···O3W | 0.821 (2) | 1.912 (5) | 2.727 (3) | 172 (3) |
O2W—H201···O63v | 0.820 (2) | 1.929 (8) | 2.727 (2) | 164 (3) |
O2W—H202···O5W | 0.820 (2) | 1.931 (4) | 2.750 (3) | 176 (3) |
O3W—H301···O24 | 0.820 (2) | 1.889 (10) | 2.684 (3) | 163 (3) |
O3W—H302···O62x | 0.819 (2) | 2.062 (15) | 2.816 (2) | 153 (3) |
O4W—H401···O11 | 0.820 (2) | 1.949 (8) | 2.750 (3) | 165 (3) |
O4W—H402···O63v | 0.820 (2) | 1.961 (7) | 2.767 (2) | 168 (3) |
O5W—H501···O13v | 0.820 (2) | 1.899 (7) | 2.704 (2) | 167 (3) |
O5W—H502···O54 | 0.820 (2) | 1.977 (9) | 2.775 (2) | 164 (3) |
O6W—H601···O32v | 0.820 (2) | 1.919 (7) | 2.726 (3) | 168 (3) |
O6W—H602···O1Wi | 0.819 (2) | 2.430 (6) | 3.239 (3) | 170 (3) |
Symmetry codes: (i) x, y, z−1; (ii) x+1, y, z; (iii) −x+2, y−1/2, −z; (iv) x+1, y, z−1; (v) x−1, y, z; (vi) −x+1, y+1/2, −z; (vii) −x+1, y+1/2, −z+1; (viii) −x+2, y−1/2, −z+1; (ix) −x, y+1/2, −z+1; (x) x−1, y, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O21—H210···O1Wi | 0.84 | 1.74 | 2.576 (3) | 173.7 |
N1—H1N1···O51ii | 0.91 | 1.87 | 2.777 (2) | 177.8 |
N1—H2N1···O14i | 0.91 | 2.15 | 2.987 (2) | 151.9 |
N1—H2N1···O24i | 0.91 | 2.35 | 3.169 (3) | 149.4 |
N1—H3N1···O52iii | 0.91 | 1.95 | 2.754 (2) | 145.8 |
O22—H220···O2Wiv | 0.84 | 1.74 | 2.575 (3) | 169.5 |
N2—H1N2···O62v | 0.91 | 1.87 | 2.780 (2) | 178.8 |
N2—H2N2···O23i | 0.91 | 2.17 | 2.987 (2) | 148.3 |
N2—H2N2···O13i | 0.91 | 2.31 | 3.144 (3) | 151.8 |
N2—H3N2···O61vi | 0.91 | 1.95 | 2.766 (2) | 148.4 |
N3—H1N3···O63v | 0.91 | 1.87 | 2.779 (2) | 175.2 |
N3—H2N3···O12 | 0.91 | 2.20 | 3.048 (2) | 155.0 |
N3—H2N3···O32 | 0.91 | 2.39 | 3.191 (2) | 147.4 |
N3—H3N3···O44vii | 0.91 | 2.03 | 2.803 (2) | 141.8 |
N4—H1N4···O54ii | 0.91 | 1.87 | 2.775 (2) | 174.0 |
N4—H2N4···O31 | 0.91 | 2.21 | 3.045 (2) | 152.0 |
N4—H2N4···O11 | 0.91 | 2.37 | 3.187 (3) | 150.0 |
N4—H3N4···O43viii | 0.91 | 2.02 | 2.811 (2) | 143.9 |
N11—H11N···O44ix | 0.911 (3) | 1.842 (4) | 2.753 (3) | 179 (2) |
N11—H21N···O14vii | 0.909 (3) | 1.955 (7) | 2.843 (3) | 165 (2) |
N11—H31N···O42v | 0.908 (3) | 2.470 (18) | 3.113 (3) | 128.0 (18) |
N11—H31N···O12v | 0.908 (3) | 2.48 (2) | 3.053 (3) | 121.2 (18) |
N11—H41N···O53v | 0.910 (3) | 1.914 (8) | 2.794 (3) | 162 (2) |
N21—H12N···O12 | 0.909 (3) | 1.970 (10) | 2.833 (3) | 158 (2) |
N21—H22N···O52v | 0.911 (3) | 2.021 (10) | 2.875 (3) | 156 (2) |
N21—H32N···O34vii | 0.909 (3) | 2.420 (17) | 3.135 (3) | 136 (2) |
N21—H42N···O53v | 0.911 (3) | 1.995 (9) | 2.871 (3) | 161 (2) |
N31—H13N···O64ix | 0.910 (3) | 1.995 (6) | 2.892 (3) | 169 (2) |
N31—H23N···O31vii | 0.909 (3) | 1.951 (9) | 2.829 (3) | 162 (2) |
N31—H33N···O61ix | 0.910 (3) | 2.051 (13) | 2.861 (3) | 148 (2) |
N31—H43N···O33v | 0.909 (3) | 2.290 (12) | 3.115 (3) | 151 (2) |
N41—H14N···O23 | 0.909 (3) | 1.940 (7) | 2.832 (3) | 167 (2) |
N41—H24N···O43v | 0.910 (3) | 1.839 (6) | 2.733 (3) | 167 (2) |
N41—H34N···O64vii | 0.910 (3) | 1.905 (5) | 2.809 (3) | 172 (2) |
N41—H44N···O41vii | 0.908 (3) | 2.325 (15) | 3.094 (3) | 142 (2) |
N51—H15N···O51 | 0.910 (3) | 1.885 (10) | 2.751 (3) | 158 (2) |
N51—H15N···O6W | 0.910 (3) | 2.56 (2) | 3.159 (3) | 124 (2) |
N51—H25N···O11v | 0.910 (3) | 2.656 (12) | 3.489 (3) | 152 (2) |
N51—H35N···O4W | 0.910 (3) | 1.945 (9) | 2.821 (3) | 161 (2) |
N51—H45N···O64 | 0.910 (3) | 1.802 (5) | 2.705 (3) | 171 (2) |
N61—H16N···O62v | 0.910 (3) | 1.855 (5) | 2.762 (3) | 174 (2) |
N61—H26N···O32 | 0.910 (3) | 2.642 (13) | 3.447 (3) | 148 (2) |
N61—H36N···O6W | 0.911 (3) | 1.918 (7) | 2.812 (3) | 167 (2) |
N61—H46N···O53v | 0.909 (3) | 1.838 (10) | 2.703 (3) | 158 (2) |
O1W—H101···O54 | 0.820 (2) | 1.927 (6) | 2.737 (3) | 169 (3) |
O1W—H102···O3W | 0.820 (2) | 1.911 (4) | 2.730 (3) | 175 (3) |
O2W—H201···O63v | 0.820 (2) | 1.915 (7) | 2.722 (2) | 168 (3) |
O2W—H202···O5W | 0.820 (2) | 1.938 (6) | 2.749 (3) | 170 (3) |
O3W—H301···O24 | 0.820 (2) | 1.886 (8) | 2.688 (3) | 166 (3) |
O3W—H302···O62x | 0.819 (2) | 2.052 (14) | 2.821 (3) | 156 (3) |
O4W—H401···O11 | 0.820 (2) | 1.938 (7) | 2.748 (3) | 169 (3) |
O4W—H402···O63v | 0.819 (2) | 1.964 (7) | 2.771 (2) | 168 (3) |
O5W—H501···O13v | 0.820 (2) | 1.905 (8) | 2.707 (3) | 166 (3) |
O5W—H502···O54 | 0.819 (2) | 1.967 (5) | 2.782 (2) | 173 (3) |
O6W—H601···O32v | 0.820 (2) | 1.916 (8) | 2.719 (3) | 166 (3) |
O6W—H602···O1Wi | 0.819 (2) | 2.56 (2) | 3.216 (3) | 138 (3) |
N21—H32N···O21vi | 0.909 (3) | 2.38 (2) | 2.890 (3) | 115.3 (18) |
O6W—H602···O51 | 0.819 (2) | 2.19 (2) | 2.838 (3) | 136 (3) |
Symmetry codes: (i) x, y, z−1; (ii) x+1, y, z; (iii) −x+2, y−1/2, −z; (iv) x+1, y, z−1; (v) x−1, y, z; (vi) −x+1, y+1/2, −z; (vii) −x+1, y+1/2, −z+1; (viii) −x+2, y−1/2, −z+1; (ix) −x, y+1/2, −z+1; (x) x−1, y, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O21—H210···O1Wi | 0.83 | 1.79 | 2.578 (3) | 159.0 |
N1—H1N1···O51ii | 0.90 | 1.88 | 2.782 (2) | 177.2 |
N1—H2N1···O14i | 0.90 | 2.16 | 2.985 (2) | 152.5 |
N1—H2N1···O24i | 0.90 | 2.37 | 3.179 (3) | 149.1 |
N1—H3N1···O52iii | 0.90 | 1.97 | 2.762 (2) | 145.7 |
O22—H220···O2Wiv | 0.83 | 1.75 | 2.579 (3) | 173.2 |
N2—H1N2···O62v | 0.90 | 1.89 | 2.787 (2) | 177.7 |
N2—H2N2···O23i | 0.90 | 2.17 | 2.984 (2) | 149.5 |
N2—H2N2···O13i | 0.90 | 2.34 | 3.157 (3) | 151.5 |
N2—H3N2···O61vi | 0.90 | 1.96 | 2.765 (3) | 147.8 |
N3—H1N3···O63v | 0.90 | 1.88 | 2.775 (2) | 174.0 |
N3—H2N3···O12 | 0.90 | 2.21 | 3.044 (2) | 154.9 |
N3—H2N3···O32 | 0.90 | 2.40 | 3.203 (3) | 148.1 |
N3—H3N3···O44vii | 0.90 | 2.04 | 2.806 (2) | 142.9 |
N4—H1N4···O54ii | 0.90 | 1.88 | 2.774 (2) | 174.2 |
N4—H2N4···O31 | 0.90 | 2.21 | 3.042 (3) | 152.9 |
N4—H2N4···O11 | 0.90 | 2.39 | 3.201 (3) | 149.7 |
N4—H3N4···O43viii | 0.90 | 2.04 | 2.818 (2) | 143.9 |
N11—H11N···O44ix | 0.911 (3) | 1.848 (5) | 2.752 (3) | 172 (2) |
N11—H21N···O14vii | 0.910 (3) | 1.960 (7) | 2.856 (3) | 168 (2) |
N11—H31N···O42v | 0.909 (3) | 2.430 (18) | 3.116 (3) | 132 (2) |
N11—H31N···O12v | 0.909 (3) | 2.51 (2) | 3.069 (3) | 120.0 (19) |
N11—H41N···O53v | 0.909 (3) | 1.944 (11) | 2.798 (3) | 156 (2) |
N21—H12N···O12 | 0.909 (3) | 1.991 (12) | 2.836 (3) | 154 (2) |
N21—H22N···O52v | 0.910 (3) | 2.026 (10) | 2.895 (3) | 159 (2) |
N21—H32N···O34vii | 0.910 (3) | 2.277 (10) | 3.144 (3) | 159 (2) |
N21—H42N···O53v | 0.911 (3) | 1.964 (6) | 2.869 (3) | 172 (2) |
N31—H13N···O64ix | 0.909 (3) | 2.007 (8) | 2.888 (3) | 163 (2) |
N31—H23N···O31vii | 0.909 (3) | 1.959 (9) | 2.838 (3) | 162 (2) |
N31—H33N···O61ix | 0.909 (3) | 2.041 (12) | 2.879 (3) | 153 (2) |
N31—H43N···O33v | 0.909 (3) | 2.219 (6) | 3.121 (3) | 171 (2) |
N41—H14N···O23 | 0.910 (3) | 1.946 (6) | 2.845 (3) | 170 (2) |
N41—H24N···O43v | 0.910 (3) | 1.856 (9) | 2.733 (3) | 161 (2) |
N41—H34N···O64vii | 0.910 (3) | 1.903 (5) | 2.809 (3) | 173 (2) |
N41—H44N···O41vii | 0.908 (3) | 2.415 (19) | 3.099 (3) | 132 (2) |
N51—H15N···O51 | 0.910 (3) | 1.898 (12) | 2.749 (3) | 155 (2) |
N51—H15N···O6W | 0.910 (3) | 2.54 (2) | 3.146 (3) | 124 (2) |
N51—H25N···O11v | 0.910 (3) | 2.736 (17) | 3.481 (3) | 140 (2) |
N51—H35N···O4W | 0.910 (3) | 1.982 (12) | 2.841 (3) | 157 (3) |
N51—H45N···O64 | 0.910 (3) | 1.811 (7) | 2.709 (3) | 168 (3) |
N61—H16N···O62v | 0.910 (3) | 1.863 (5) | 2.768 (3) | 173 (3) |
N61—H26N···O32 | 0.910 (3) | 2.691 (16) | 3.450 (3) | 142 (2) |
N61—H36N···O6W | 0.911 (3) | 1.919 (8) | 2.812 (3) | 166 (3) |
N61—H46N···O53v | 0.909 (3) | 1.924 (16) | 2.718 (3) | 145 (2) |
O1W—H101···O54 | 0.820 (2) | 1.935 (8) | 2.739 (3) | 166 (3) |
O1W—H102···O3W | 0.820 (2) | 1.919 (6) | 2.734 (3) | 172 (3) |
O2W—H201···O63v | 0.820 (2) | 1.967 (14) | 2.725 (3) | 153 (3) |
O2W—H202···O5W | 0.820 (2) | 1.946 (7) | 2.755 (3) | 169 (3) |
O3W—H301···O24 | 0.820 (2) | 1.887 (9) | 2.690 (3) | 166 (4) |
O3W—H302···O62x | 0.819 (2) | 2.022 (4) | 2.840 (3) | 178 (4) |
O4W—H401···O11 | 0.820 (2) | 1.950 (9) | 2.752 (3) | 166 (3) |
O4W—H402···O63v | 0.820 (2) | 1.955 (5) | 2.772 (2) | 174 (3) |
O5W—H501···O13v | 0.820 (2) | 1.899 (9) | 2.701 (3) | 166 (4) |
O5W—H502···O54 | 0.819 (2) | 1.989 (7) | 2.799 (3) | 170 (3) |
O6W—H601···O32v | 0.820 (2) | 1.940 (12) | 2.725 (3) | 160 (3) |
O6W—H602···O1Wi | 0.819 (2) | 2.475 (17) | 3.221 (3) | 152 (3) |
O3W—H302···N61xi | 0.819 (2) | 2.74 (3) | 3.146 (3) | 112 (3) |
N21—H32N···O44vii | 0.910 (3) | 2.47 (2) | 3.117 (3) | 128 (2) |
N31—H43N···O43v | 0.909 (3) | 2.62 (2) | 3.133 (3) | 116.3 (19) |
N61—H26N···O4W | 0.910 (3) | 2.52 (2) | 2.977 (3) | 111.8 (18) |
Symmetry codes: (i) x, y, z−1; (ii) x+1, y, z; (iii) −x+2, y−1/2, −z; (iv) x+1, y, z−1; (v) x−1, y, z; (vi) −x+1, y+1/2, −z; (vii) −x+1, y+1/2, −z+1; (viii) −x+2, y−1/2, −z+1; (ix) −x, y+1/2, −z+1; (x) x−1, y, z+1; (xi) x, y, z+1. |