Crystal structure of the deuterated hepta­hydrate of potassium phosphate, K₃PO₄·7D₂O

An intricate network of medium-strong O—D...O hydrogen bonds consolidates the crystal structure of water-rich K₃PO₄·7D₂O.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](P-O) = 0.001 Å
• R factor = 0.016
• wR factor = 0.020
• Data-to-parameter ratio = 22.1

checkCIF/PLATON results

No syntax errors found



Alert level G
PLAT005_ALERT_5_G No Embedded Refinement Details Found  in the CIF     Please Do !
PLAT066_ALERT_1_G Predicted and Reported Tmin&Tmax Range Identical          ? Check
PLAT395_ALERT_2_G Deviating  X-O-Y    Angle From 120 for O1W            107.2 Degree
PLAT395_ALERT_2_G Deviating  X-O-Y    Angle From 120 for O2W            112.6 Degree
PLAT395_ALERT_2_G Deviating  X-O-Y    Angle From 120 for O3W            113.5 Degree
PLAT395_ALERT_2_G Deviating  X-O-Y    Angle From 120 for O4W             95.1 Degree
PLAT395_ALERT_2_G Deviating  X-O-Y    Angle From 120 for O5W            102.9 Degree
PLAT395_ALERT_2_G Deviating  X-O-Y    Angle From 120 for O6W            104.0 Degree
PLAT395_ALERT_2_G Deviating  X-O-Y    Angle From 120 for O7W            104.7 Degree
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          4 Note
              D2 O
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          5 Note
              D2 O
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          7 Note
              D2 O
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #         10 Note
              K
PLAT808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found     Please Check
PLAT929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not Checked          ! Info
PLAT960_ALERT_3_G Number of Intensities with I  <   - 2*sig(I) ...          1 Check

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

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

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Computing details

Data collection: APEX2 (Bruker, 2016); cell refinement: SAINT-Plus (Bruker, 2016); data reduction: SAINT-Plus (Bruker, 2016); program(s) used to solve structure: SHELXT (Sheldrick, 2015); program(s) used to refine structure: Jana2006 (Petříček et al., 2014); molecular graphics: ATOMS (Dowty, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Potassium phosphate heptahydrate

Crystal data

K3PO4·7D2O	F(000) = 348
Mr = 352.5	Dx = 2.000 Mg m^−3
Monoclinic, P21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2yb	Cell parameters from 7382 reflections
a = 7.8325 (7) Å	θ = 2.6–32.6°
b = 9.3406 (8) Å	µ = 1.34 mm^−1
c = 8.4471 (7) Å	T = 100 K
β = 108.727 (2)°	Rod, colourless
V = 585.28 (9) Å^3	0.46 × 0.09 × 0.01 mm
Z = 2

Data collection

Bruker Kappa APEXII CCD diffractometer	4273 independent reflections
Radiation source: X-ray tube	4127 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.021
ω– and φ–scans	θmax = 32.6°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2016)	h = −10→11
Tmin = 0.54, Tmax = 0.99	k = −14→14
9464 measured reflections	l = −12→10

Refinement

Refinement on F	1 constraint
R[F^2 > 2σ(F^2)] = 0.016	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + 0.0001F^2)
wR(F^2) = 0.020	(Δ/σ)max = 0.019
S = 1.02	Δρmax = 0.16 e Å^−3
4273 reflections	Δρmin = −0.13 e Å^−3
193 parameters	Absolute structure: 2017 Friedel pairs used in the refinement (Flack, 1983)
0 restraints	Absolute structure parameter: 0.004 (16)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.42550 (3)	0.01804 (2)	0.73444 (3)	0.00950 (6)
K2	−0.14458 (3)	−0.00537 (2)	0.62341 (3)	0.00990 (6)
K3	0.52865 (3)	0.39152 (2)	0.81480 (3)	0.01224 (6)
P1	0.02505 (3)	0.04285 (3)	0.25261 (3)	0.00571 (7)
O1	0.08740 (10)	0.03291 (8)	0.44490 (9)	0.00823 (19)
O2	−0.06671 (10)	−0.09902 (8)	0.17723 (10)	0.0101 (2)
O3	−0.10938 (10)	0.16905 (8)	0.19358 (10)	0.0092 (2)
O4	0.18924 (10)	0.07033 (8)	0.19270 (10)	0.0086 (2)
O1w	0.50577 (11)	0.08478 (8)	0.45314 (11)	0.0119 (2)
O2w	0.22528 (11)	0.27301 (8)	0.61723 (11)	0.0106 (2)
O3w	0.23569 (11)	−0.22553 (8)	0.56243 (11)	0.0116 (2)
O4w	−0.18873 (12)	0.20109 (9)	0.83725 (11)	0.0129 (2)
O5w	0.53272 (11)	0.15028 (9)	1.03669 (11)	0.0126 (2)
O6w	0.71314 (11)	−0.16355 (8)	0.86601 (11)	0.0119 (2)
O7w	0.17243 (11)	−0.04581 (9)	0.88427 (10)	0.0103 (2)
D11	0.564 (2)	0.161 (2)	0.442 (2)	0.027 (5)*
D12	0.409 (3)	0.091 (2)	0.390 (3)	0.033 (5)*
D21	0.172 (3)	0.315 (2)	0.680 (2)	0.034 (5)*
D22	0.173 (3)	0.213 (2)	0.570 (3)	0.037 (6)*
D31	0.182 (2)	−0.162 (2)	0.506 (3)	0.031 (5)*
D32	0.179 (3)	−0.261 (3)	0.642 (3)	0.052 (7)*
D41	−0.153 (2)	0.1885 (19)	0.936 (3)	0.022 (4)*
D42	−0.113 (3)	0.258 (3)	0.837 (3)	0.049 (7)*
D51	0.477 (2)	0.2098 (19)	1.068 (2)	0.021 (4)*
D52	0.634 (2)	0.1654 (19)	1.093 (2)	0.023 (4)*
D61	0.776 (3)	−0.143 (2)	0.950 (3)	0.031 (5)*
D62	0.759 (2)	−0.240 (2)	0.842 (2)	0.023 (4)*
D71	0.132 (2)	−0.123 (2)	0.877 (2)	0.023 (4)*
D72	0.166 (2)	−0.0150 (19)	0.973 (2)	0.019 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.01055 (8)	0.00951 (9)	0.00895 (9)	0.00141 (6)	0.00384 (7)	0.00041 (7)
K2	0.00815 (8)	0.01323 (9)	0.00836 (9)	0.00028 (7)	0.00272 (7)	−0.00109 (7)
K3	0.01205 (9)	0.00943 (9)	0.01200 (11)	−0.00261 (7)	−0.00067 (8)	0.00104 (7)
P1	0.00639 (10)	0.00552 (10)	0.00530 (11)	−0.00037 (8)	0.00201 (8)	0.00003 (8)
O1	0.0102 (3)	0.0084 (3)	0.0056 (3)	0.0002 (2)	0.0020 (2)	−0.0001 (2)
O2	0.0131 (3)	0.0080 (3)	0.0086 (3)	−0.0040 (3)	0.0027 (3)	−0.0020 (3)
O3	0.0086 (3)	0.0090 (3)	0.0099 (4)	0.0029 (2)	0.0028 (3)	0.0022 (3)
O4	0.0089 (3)	0.0088 (3)	0.0092 (4)	−0.0002 (2)	0.0046 (3)	0.0004 (2)
O1w	0.0078 (3)	0.0150 (4)	0.0114 (4)	−0.0011 (3)	0.0010 (3)	0.0026 (3)
O2w	0.0091 (3)	0.0103 (3)	0.0120 (4)	−0.0011 (3)	0.0026 (3)	−0.0033 (3)
O3w	0.0127 (3)	0.0109 (3)	0.0123 (4)	0.0032 (3)	0.0056 (3)	0.0032 (3)
O4w	0.0182 (4)	0.0112 (3)	0.0102 (4)	−0.0007 (3)	0.0059 (3)	0.0003 (3)
O5w	0.0084 (3)	0.0168 (4)	0.0122 (4)	−0.0016 (3)	0.0030 (3)	−0.0033 (3)
O6w	0.0111 (3)	0.0099 (3)	0.0122 (4)	0.0020 (3)	0.0003 (3)	−0.0024 (3)
O7w	0.0126 (3)	0.0098 (3)	0.0091 (4)	−0.0010 (3)	0.0041 (3)	−0.0008 (3)

Geometric parameters (Å, º)

K1—O5w	2.7153 (10)	K3—O5w	2.9246 (10)
K1—O1w	2.7183 (11)	P1—O1	1.5414 (8)
K1—O7w	2.7381 (10)	P1—O2	1.5440 (8)
K1—O6w	2.7532 (9)	P1—O4	1.5472 (10)
K1—O3w	2.8479 (9)	P1—O3	1.5523 (8)
K1—O2w	2.8486 (9)	O1w—D11	0.86 (2)
K1—O1	2.9757 (9)	O1w—D12	0.778 (18)
K2—O1	2.7317 (10)	O2w—D21	0.87 (2)
K2—O4w	2.7391 (10)	O2w—D22	0.73 (2)
K2—O7w	2.7659 (9)	O3w—D31	0.796 (19)
K2—O1w^i	2.7836 (9)	O3w—D32	0.98 (3)
K2—O2w^ii	2.8269 (9)	O4w—D41	0.80 (2)
K2—O3w^iii	3.0144 (9)	O4w—D42	0.79 (2)
K2—O6w^i	3.0151 (10)	O5w—D51	0.80 (2)
K3—O2w	2.6665 (9)	O5w—D52	0.795 (17)
K3—O4^iv	2.7867 (9)	O6w—D61	0.748 (19)
K3—O4w^v	2.7983 (10)	O6w—D62	0.85 (2)
K3—O5w^vi	2.8344 (10)	O7w—D71	0.783 (19)
K3—O1w^iv	2.8394 (10)	O7w—D72	0.823 (19)
K3—O7w^vi	2.9094 (9)
O1—K1—O1w	70.45 (2)	O1w^iv—K3—O5w^vi	79.89 (3)
O1—K1—O2w	55.25 (2)	O1w^iv—K3—O7w^vi	114.35 (2)
O1—K1—O3w	55.73 (2)	O2w—K3—O4w^v	107.76 (3)
O1—K1—O5w	132.58 (3)	O2w—K3—O5w	84.57 (2)
O1—K1—O6w	139.24 (2)	O2w—K3—O5w^vi	112.79 (3)
O1—K1—O7w	78.74 (2)	O2w—K3—O7w^vi	159.36 (3)
O1w—K1—O2w	76.14 (3)	O4w^v—K3—O5w	67.74 (3)
O1w—K1—O3w	88.09 (3)	O4w^v—K3—O5w^vi	139.02 (2)
O1w—K1—O5w	128.98 (3)	O4w^v—K3—O7w^vi	70.82 (3)
O1w—K1—O6w	96.04 (3)	O5w—K3—O5w^vi	109.99 (3)
O1w—K1—O7w	149.19 (2)	O5w—K3—O7w^vi	75.81 (2)
O2w—K1—O3w	110.59 (2)	O5w^vi—K3—O7w^vi	69.21 (2)
O2w—K1—O5w	85.18 (3)	O1—P1—O2	109.32 (4)
O2w—K1—O6w	160.60 (2)	O1—P1—O3	109.69 (5)
O2w—K1—O7w	86.75 (3)	O1—P1—O4	109.83 (4)
O3w—K1—O5w	142.78 (3)	O2—P1—O3	109.96 (4)
O3w—K1—O6w	86.52 (2)	O2—P1—O4	109.46 (5)
O3w—K1—O7w	74.04 (3)	O3—P1—O4	108.56 (4)
O5w—K1—O6w	86.26 (3)	K2—O1—P1	123.21 (4)
O5w—K1—O7w	73.48 (3)	K3^vii—O4—P1	131.03 (4)
O6w—K1—O7w	107.41 (3)	K1—O1w—K2^v	86.80 (2)
O1—K2—O1w^i	113.18 (3)	K1—O1w—K3^vii	124.16 (3)
O1—K2—O2w^ii	74.56 (3)	K2^v—O1w—K3^vii	92.60 (3)
O1—K2—O3w^iii	71.77 (3)	K1—O2w—K2^iii	146.43 (4)
O1—K2—O4w	121.27 (3)	K1—O2w—K3	81.32 (2)
O1—K2—O6w^i	153.61 (2)	K2^iii—O2w—K3	95.43 (3)
O1—K2—O7w	82.62 (3)	D21—O2w—D22	113 (3)
O1w^i—K2—O2w^ii	83.93 (2)	K1—O3w—D31	78.3 (13)
O1w^i—K2—O3w^iii	55.91 (2)	K1—O3w—D32	101.6 (14)
O1w^i—K2—O4w	79.41 (3)	D31—O3w—D32	114 (2)
O1w^i—K2—O6w^i	88.99 (3)	K2—O4w—K3^i	131.87 (3)
O1w^i—K2—O7w	159.32 (3)	K2—O4w—D41	120.6 (14)
O2w^ii—K2—O3w^iii	107.43 (3)	K2—O4w—D42	102.2 (19)
O2w^ii—K2—O4w	160.62 (3)	K3^i—O4w—D41	99.7 (15)
O2w^ii—K2—O6w^i	94.81 (3)	K3^i—O4w—D42	98.8 (17)
O2w^ii—K2—O7w	114.15 (3)	D41—O4w—D42	95 (2)
O3w^iii—K2—O4w	70.97 (3)	K1—O5w—K3^viii	89.03 (2)
O3w^iii—K2—O6w^i	134.55 (3)	K1—O5w—D51	126.3 (11)
O3w^iii—K2—O7w	122.36 (2)	K1—O5w—D52	126.4 (16)
O4w—K2—O6w^i	75.19 (3)	K3^viii—O5w—D51	104.9 (14)
O4w—K2—O7w	80.90 (3)	K3^viii—O5w—D52	99.4 (13)
O6w^i—K2—O7w	79.91 (3)	D51—O5w—D52	102.5 (18)
O4^iv—K3—O1w^iv	58.26 (2)	K1—O6w—D61	115.4 (16)
O4^iv—K3—O2w	142.03 (3)	K1—O6w—D62	140.5 (11)
O4^iv—K3—O4w^v	76.51 (3)	D61—O6w—D62	104 (2)
O4^iv—K3—O5w	129.11 (2)	K1—O7w—K2	101.53 (3)
O4^iv—K3—O5w^vi	75.37 (3)	K1—O7w—D71	120.0 (16)
O4^iv—K3—O7w^vi	58.52 (2)	K1—O7w—D72	127.9 (12)
O1w^iv—K3—O2w	85.85 (3)	K2—O7w—D71	80.0 (11)
O1w^iv—K3—O4w^v	109.19 (3)	K2—O7w—D72	112.2 (11)
O1w^iv—K3—O5w	168.35 (2)	D71—O7w—D72	105 (2)

Symmetry codes: (i) x−1, y, z; (ii) −x, y−1/2, −z+1; (iii) −x, y+1/2, −z+1; (iv) −x+1, y+1/2, −z+1; (v) x+1, y, z; (vi) −x+1, y+1/2, −z+2; (vii) −x+1, y−1/2, −z+1; (viii) −x+1, y−1/2, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—D11···O3w^iv	0.86 (2)	1.91 (2)	2.7255 (13)	158 (2)
O1w—D12···O4	0.78 (2)	1.98 (2)	2.7391 (11)	164 (2)
O2w—D21···O2^iii	0.87 (2)	1.85 (2)	2.7149 (13)	177 (2)
O2w—D22···O1	0.73 (2)	1.99 (2)	2.7029 (11)	167 (3)
O3w—D31···O1	0.80 (2)	1.97 (2)	2.7242 (11)	159 (2)
O3w—D32···O3^ii	0.98 (3)	1.77 (3)	2.7395 (14)	171 (2)
O4w—D41···O3^ix	0.80 (2)	2.10 (2)	2.8870 (14)	169 (2)
O4w—D42···O2^iii	0.79 (2)	1.97 (2)	2.7679 (13)	177 (2)
O5w—D51···O6w^vi	0.80 (2)	2.11 (2)	2.9025 (13)	168 (2)
O5w—D52···O3^x	0.80 (2)	1.92 (2)	2.6944 (12)	166 (2)
O6w—D61···O2^x	0.75 (2)	1.96 (2)	2.7087 (12)	176 (2)
O6w—D62···O4^vii	0.85 (2)	1.86 (2)	2.6931 (12)	165 (2)
O7w—D71···O3^ii	0.78 (2)	2.02 (2)	2.7498 (12)	155 (2)
O7w—D72···O4^ix	0.82 (2)	1.97 (2)	2.7859 (13)	171 (2)

Symmetry codes: (ii) −x, y−1/2, −z+1; (iii) −x, y+1/2, −z+1; (iv) −x+1, y+1/2, −z+1; (vi) −x+1, y+1/2, −z+2; (vii) −x+1, y−1/2, −z+1; (ix) x, y, z+1; (x) x+1, y, z+1.