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The title compound, sodium pamidronate monohydrate, Na+·C3H10NO7P{}_{2}^{\,- }·H2O, crystallizes in sheets in the ab plane through Na-O coordination and hydrogen bonding to the pamidronate zwitterion. The neutral sheets are connected through hydrogen bonding, including the water molecule in the c direction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804032568/bv6006sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804032568/bv6006Isup2.hkl
Contains datablock I

CCDC reference: 262266

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.045
  • wR factor = 0.111
  • Data-to-parameter ratio = 17.6

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.17 PLAT417_ALERT_2_C Short Inter D-H..H-D H9 .. H12 .. 2.12 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXTL.

sodium 3-ammonium-1-hydroxypropylidene-1,1-bisphosphonate monohydrate top
Crystal data top
Na+·C3H10NO7P2·H2OZ = 2
Mr = 275.07F(000) = 284
Triclinic, P1Dx = 1.883 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 5.8699 (5) ÅCell parameters from 3147 reflections
b = 9.1235 (8) Åθ = 3.1–30.7°
c = 9.3113 (8) ŵ = 0.52 mm1
α = 86.746 (2)°T = 120 K
β = 77.125 (2)°Lath like, colorless
γ = 87.728 (2)°0.35 × 0.08 × 0.02 mm
V = 485.15 (7) Å3
Data collection top
Bruker SMART APEX
diffractometer
2811 independent reflections
Radiation source: fine-focus sealed tube2543 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω scans, frame data integrationθmax = 30.8°, θmin = 2.2°
Absorption correction: multi-scan
SADABS (Sheldrick, 2002)
h = 88
Tmin = 0.8, Tmax = 1.0k = 1313
6525 measured reflectionsl = 1313
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: difference Fourier map
wR(F2) = 0.111H atoms treated by a mixture of independent and constrained refinement
S = 1.10 w = 1/[σ2(Fo2) + (0.056P)2 + 0.4254P]
where P = (Fo2 + 2Fc2)/3
2811 reflections(Δ/σ)max < 0.001
160 parametersΔρmax = 0.96 e Å3
5 restraintsΔρmin = 0.44 e Å3
Special details top

Experimental. Oxford Cryosystem liquid nitrogen cryostream cooler

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 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Na0.29895 (14)0.39826 (9)0.11810 (9)0.00902 (18)
O80.1372 (3)0.30519 (18)0.52726 (18)0.0130 (3)
H110.255 (4)0.322 (3)0.457 (3)0.020*
H120.126 (5)0.376 (3)0.587 (3)0.020*
P10.14952 (9)0.25656 (5)0.04207 (5)0.00579 (13)
O10.0999 (2)0.33818 (16)0.07714 (16)0.0083 (3)
H100.095 (5)0.402 (3)0.135 (3)0.012*
O20.1462 (3)0.12529 (15)0.14890 (16)0.0090 (3)
O30.3404 (3)0.36108 (15)0.03975 (16)0.0085 (3)
P20.26402 (9)0.33484 (5)0.28981 (5)0.00640 (13)
O40.0906 (3)0.46301 (15)0.25636 (16)0.0084 (3)
O50.2384 (3)0.26740 (16)0.43723 (16)0.0093 (3)
H90.112 (4)0.288 (3)0.462 (3)0.014*
O60.5157 (3)0.36392 (16)0.30145 (16)0.0102 (3)
O70.0656 (3)0.15823 (15)0.15782 (17)0.0086 (3)
H80.084 (5)0.071 (2)0.161 (3)0.013*
C10.1666 (3)0.1903 (2)0.1451 (2)0.0063 (3)
C20.3327 (4)0.0552 (2)0.1592 (2)0.0085 (4)
H10.48130.08400.13940.010*
H20.26610.01860.08230.010*
C30.3840 (4)0.0168 (2)0.3071 (2)0.0091 (4)
H30.23950.02380.34210.011*
H40.49400.04200.38050.011*
N10.4874 (3)0.16689 (19)0.2859 (2)0.0097 (3)
H50.619 (5)0.167 (3)0.243 (3)0.015*
H60.382 (5)0.227 (3)0.227 (3)0.015*
H70.527 (5)0.206 (3)0.371 (3)0.015*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na0.0085 (4)0.0084 (4)0.0108 (4)0.0018 (3)0.0030 (3)0.0011 (3)
O80.0127 (7)0.0148 (7)0.0113 (7)0.0020 (6)0.0029 (6)0.0012 (6)
P10.0066 (2)0.0042 (2)0.0068 (2)0.00070 (16)0.00188 (18)0.00056 (16)
O10.0069 (6)0.0077 (6)0.0110 (7)0.0005 (5)0.0028 (5)0.0032 (5)
O20.0129 (7)0.0060 (6)0.0086 (7)0.0012 (5)0.0030 (5)0.0002 (5)
O30.0086 (7)0.0060 (6)0.0112 (7)0.0035 (5)0.0021 (5)0.0020 (5)
P20.0075 (2)0.0051 (2)0.0068 (2)0.00044 (17)0.00178 (18)0.00077 (16)
O40.0108 (7)0.0044 (6)0.0100 (7)0.0009 (5)0.0021 (5)0.0015 (5)
O50.0100 (7)0.0109 (7)0.0078 (7)0.0017 (5)0.0035 (5)0.0028 (5)
O60.0085 (7)0.0130 (7)0.0094 (7)0.0023 (5)0.0023 (5)0.0001 (5)
O70.0077 (7)0.0055 (6)0.0139 (7)0.0016 (5)0.0045 (5)0.0017 (5)
C10.0069 (8)0.0049 (8)0.0076 (8)0.0006 (6)0.0023 (7)0.0019 (6)
C20.0097 (9)0.0077 (8)0.0081 (8)0.0010 (7)0.0023 (7)0.0012 (6)
C30.0115 (9)0.0052 (8)0.0107 (9)0.0024 (7)0.0027 (7)0.0012 (6)
N10.0131 (9)0.0054 (7)0.0109 (8)0.0014 (6)0.0031 (7)0.0015 (6)
Geometric parameters (Å, º) top
Na—O6i2.2611 (17)P2—O51.5751 (15)
Na—O3i2.3174 (16)P2—C11.843 (2)
Na—O3ii2.3394 (16)O5—H90.837 (17)
Na—O12.3987 (17)O7—C11.436 (2)
Na—O42.4382 (17)O7—H80.807 (17)
Na—O72.5371 (17)C1—C21.534 (3)
O8—H110.852 (17)C2—C31.523 (3)
O8—H120.818 (17)C2—H10.9800
P1—O31.4956 (15)C2—H20.9800
P1—O21.5108 (14)C3—N11.496 (2)
P1—O11.5913 (15)C3—H30.9800
P1—C11.858 (2)C3—H40.9800
O1—H100.817 (17)N1—H50.94 (3)
P2—O61.4902 (15)N1—H60.91 (3)
P2—O41.5185 (15)N1—H70.87 (3)
O6i—Na—O3i85.65 (6)O5—P2—C1104.85 (8)
O6i—Na—O3ii113.04 (6)P2—O5—H9115 (2)
O3i—Na—O3ii85.70 (6)C1—O7—H8112 (2)
O6i—Na—O1158.87 (6)O7—C1—C2113.34 (15)
O3i—Na—O191.46 (6)O7—C1—P2104.80 (12)
O3ii—Na—O187.54 (6)C2—C1—P2112.75 (13)
O6i—Na—O4101.74 (6)O7—C1—P1108.29 (13)
O3i—Na—O4171.20 (6)C2—C1—P1106.06 (13)
O3ii—Na—O486.98 (6)P2—C1—P1111.64 (10)
O1—Na—O483.34 (6)C3—C2—C1116.35 (16)
O6i—Na—O793.08 (6)C3—C2—H1108
O3i—Na—O7110.80 (6)C1—C2—H1108
O3ii—Na—O7150.48 (6)C3—C2—H2108
O1—Na—O768.39 (5)C1—C2—H2108
O4—Na—O773.91 (5)H1—C2—H2107
H11—O8—H12108 (3)N1—C3—C2108.03 (16)
O3—P1—O2114.45 (8)N1—C3—H3110
O3—P1—O1111.03 (8)C2—C3—H3110
O2—P1—O1108.83 (8)N1—C3—H4110
O3—P1—C1110.64 (8)C2—C3—H4110
O2—P1—C1108.74 (8)H3—C3—H4108
O1—P1—C1102.45 (8)C3—N1—H5113.5 (18)
P1—O1—H10108 (2)C3—N1—H6111.6 (19)
O6—P2—O4117.49 (9)H5—N1—H6107 (2)
O6—P2—O5108.37 (9)C3—N1—H7108.3 (19)
O4—P2—O5108.96 (8)H5—N1—H7109 (3)
O6—P2—C1109.99 (9)H6—N1—H7107 (3)
O4—P2—C1106.46 (8)
Symmetry codes: (i) x1, y, z; (ii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H5···O2iii0.94 (3)1.85 (3)2.782 (2)167 (3)
N1—H6···O1iv0.91 (3)2.16 (3)3.060 (2)171 (3)
N1—H7···O5v0.87 (3)2.09 (3)2.895 (2)155 (3)
O7—H8···O2iv0.81 (2)1.84 (2)2.641 (2)174 (3)
O5—H9···O80.84 (2)1.70 (2)2.532 (2)171 (3)
O1—H10···O4ii0.82 (2)1.73 (2)2.544 (2)179 (3)
O8—H11···O6i0.85 (2)1.79 (2)2.644 (2)175 (3)
O8—H12···O4vi0.82 (2)2.00 (2)2.815 (2)176 (3)
Symmetry codes: (i) x1, y, z; (ii) x, y+1, z; (iii) x+1, y, z; (iv) x, y, z; (v) x+1, y, z1; (vi) x, y+1, z1.
 

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