Prescott, Hillary A.: The Crystal Structures and Thermal Behavior of Hydrogen Monofluorophosphates and Basic Monofluorophosphates with Alkali Metal and N-containing Cations

110

Anhang A. Appendix

A.1 Selected Experimental Data of the Single Crystal Analysis

Tab. A1 The Structures with Infinite Chains

Formula

NaHPO3F·2.5H2O*<2>

[NH2Et2]HPO3F

[PipzH2][HPO3F]2

Formula weight

167.01

173.12

286.11

Crystal system

Monoclinic

Orthorhombic

Monoclinic

Space group

C2/c

Pbca

P21/c

Crystal Size

0.8 x 0.4 x 0.4

0.4 x 0.2 x 0.1

0.6 x 0.4 x 0.1

a

19.112(4)

12.892(4)

6.020(2)

b

5.341(1)

9.530(3)

13.012(3)

c

12.727(3)

13.555(4)

7.285(2)

â

110.18(3)

90

95.09(3)

V3, Z

1219.4(4), 8

1665.4(9), 8

568.4(3), 2

rhocalc./g·cm -3

1.819

1.381

1.672

Abs. corr. method/ µ/mm-1

Numerical/0.499

None, 0.304

None, 0.426

Transmission, min./max.

0.8454, 0.9741

 

 

Diffractometer

STADI-4

IPDS

IPDS

Temperature/K

160(2)

180(2)

180(2)

2theta range for data collection/°

3.0-60.0

3.3-52.1

3.3-52.1

Reflections collected

1567

11898

4462

Data/restraints/parameters

1388/0/103

1581/1/143

1027/1/101

wR2

0.0649

0.0591

0.0686

R1 [I>2sigma(I)]

0.0277

0.0288

0.0251

GOOF (obs.)

1.097

0.871

1.036

Deltazetamax.(eÅ-3), Deltazetamin.(eÅ-3)

0.463, -0.340

0.208, -0.219

0.372, -0.276

CSD-Nummer

411 318

 

 

Tab. A2 The Structures with Branched Chains or Isolated Dimers

Formula

KHPO3F

K3[H(PO3F)2]

Formula weight

138.08

314.25

Crystal system

Monoclinic

Monoclinic

Space group

P21

C2/c

Crystal Size

0.1 x 0.1 x 0.1

0.9 x 0.8 x 0.2

a

7.273(1)

7.973(3)

b

14.086(3)

11.635(4)

c

7.655(2)

9.668(4)

â

90.13(3)

113.52(4)

V3, Z

784.2(3), 8

822.3(5), 4

rhocalc./g·cm -3

2.339

2.538

Abs. corr. method/ µ/mm-1

None, 1.642

None, 2.076

Diffractometer

IPDS

IPDS

Temperature/K

180(2)

180(2)

2theta range for data collection/°

3.5-54.2

3.8-56.3

Reflections collected

5600

3397

Data/restraints/parameters

2745/2/233

742/1/63

wR2

0.0395

0.1615

R1 [I>2sigma(I)]

0.0214

0.0581

GOOF (obs.)

0.961

1.108

Deltazetamax.(eÅ-3), Deltazetamin.(eÅ-3)

0.283, -0.270

0.804, -1.160


111

Tab. A3 The Structures with Cyclic Dimers

Formula

CsHPO3F

[NHEt3]HPO3F

Formula weight

231.89

201.18

Crystal system

Monoclinic

Monoclinic

Space group

C2/m

P21/n

Crystal Size

0.4 x 0.2 x 0.1

0.5 x 0.4 x 0.2

a

14.478(8)

10.735(3)

b

5.929(3)

8.214(2)

c

5.413(2)

11.755(3)

â

103.30(4)

91.15(3)

V3, Z

452.2(3), 4

1036.3(5), 4

rhocalc./g·cm -3

3.406

1.289

Abs. corr. method/ µ/mm-1

Numerical, 8.439

None, 0.254

Transmission, min./max.

0.1927, 0.4768

 

Diffractometer

STADI-4

IPDS

Temperature/K

180(2)

180(2)

2theta range for data collection/°

5.8-62.0

3.3-52.1

Reflections collected

1025

7678

Data/restraints/parameters

530/1/39

1889/1/181

WR2

0.0373

0.1051

R1 [I>2sigma(I)]

0.0155

0.0387

GOOF (obs.)

1.127

1.044

Deltazetamax.(eÅ-3), Deltazetamin.(eÅ-3)

0.654, -0.830

0.349, -0.217

CSD-Nummer

410 932

 

Tab. A4 The Structures with Cyclic Dimers

Formula

[C(NH2)3]HPO3F

{HOC[NH(CH3)]2}HPO3F

Formula weight

159.07

188.10

Crystal system

Monoclinic

Monoclinic

Space group

P21/c

P21/c

Crystal Size

0.2 x 0.08 x 0.04

0.5 x 0.2 x 0.1

a

6.780(1)

5.435(1)

b

10.089(2)

17.634(4)

c

9.389(2)

8.507(2)

â

105.77(3)

100.47(3)

V/Å3, Z

618.1(2), 4

801.7(3), 4

rhocalc./g·cm -3

1.709

1.558

Abs. corr. method/ µ/mm-1

None, 0.410

None, 0.335

Diffractometer

IPDS

IPDS

Temperature/K

180(2)

180(2)

2theta range for data collection/°

3.3-52.1

3.3-52.1

Reflections collected

5235

6260

Data/restraints/parameters

1166/0/110

1445/0/140

wR2

0.1094

0.0679

R1 [I>2sigma(I)]

0.0449

0.0383

GOOF (obs.)

0.977

0.870

Deltazetamax.(eÅ-3), Deltazetamin.(eÅ-3)

0.532, -0.435

0.359, -0.274


112

Tab. A5 The Structures with Cyclic Tetramers

Formula

á-NH4HPO3F

â-NH4HPO3F

â-NH4HPO3F

alpha-RbHPO3F

Formula weight

117.02

117.02

117.02

184.45

Crystal system

P21/n

Pî

Pî

P21/n

Space group

Monoclinic

Triclinic

Triclinic

Monoclinic

Crystal Size

0.4 x 0.1 x 0.1

0.7 x 0.6 x 0.4

0.6 x 0.6 x 0.4

0.8 x 0.2 x 0.1

a

7.4650(7)

7.444(5)

7.481(1)

7.465(2)

b

15.586(2)

7.507(6)

7.511(1)

15.551(8)

c

7.5785(9)

7.778(6)

7.782(1)

7.563(4)

á

90

84.41(6)

84.31(1)

90

â

108.769(9)

84.51(5)

84.20(3)

105.38(5)

gamma

90

68.33(6)

68.67(2)

90

V3, Z

834.9(2), 8

401.2(5), 4

404.31(9), 4

846.5(7), 8

rhocalc./g·cm -3

1.862

1.937

1.922

2.894

Abs. corr. Method/ µ/mm-1

Psi scan, 0.557

None, 0.580

None, 0.576

Psi scan, 11.964

Transmission, min./max.

0.8512, 0.9991

 

 

0.3131, 0.9957

Diffractometer

STADI-4

STADI-4

STADI-4

STADI-4

Temperature/K

180(2)

180(2)

310(2)

180(2)

2theta range for data collection/°

3.0-55.0

3.0-60.0

3.0-52.0*

3.0-52.0

Reflections collected

3240

1802

3158

2938

Data/restraints/parameters

1629/1/149

1609/0/149

1579/149/0

1469/1/118

wR2

0.0818

0.1379

0.0735

0.0694

R1 [I>2sigma(I)]

0.0376

0.0535

0.0254

0.0365

GOOF (obs.)

1.016

1.105

1.018

1.025

Deltazetamax.(eÅ-3), Deltazetamin.(eÅ-3)

0.407, -0.421

0.799, -0.659

0.274, -0.358

0.874, -0.647

CSD-Nummer

411 903

411 901

411 902

 

Tab. A6 The Complex Structures and Hydrates

Formula

Cs3(NH4)2(HPO3F)3(PO3F)

[N(CH3)4]HPO3F·H2O

Na2PO3F·10H2O*

Formula weight

829.72

191.14

324.11

Crystal system

Monoclinic

Cubic

Monoclinic

Space group

P21/c

P213

P21/c

Crystal Size

0.6 x 0.6 x 0.6

0.8 x 0.8 x 0.24

0.5 x 0.5 x 0.4

a

20.619(4)

9.691(2)

11.380(3)

b

12.076(2)

9.691(2)

10.234(2)

c

15.856(3)

9.691(2)

13.051(4)

â

102.58(2)

90

106.49(3)

V3, Z

3853(1), 8

910.1(3), 4

1457.4(7), 4

rhocalc./g·cm -3

2.860

1.395

1.477

Abs. corr. Method/ µ/mm-1

Numerical, 6.067

None, 0.293

None/0.310

Transmission, min./max.

0.0497, 0.1504

 

 

Diffractometer

IPDS

IPDS

IPDS

Temperature/K

180(2)

180(2)

160

2theta range for data collection/°

3.8-56.3

5.94-51.24

3.8-56.3

Reflections collected

25658

5989

13174

Data/restraints/parameters

6339/27/546

582/0/65

3039/0/242

wR2

0.0976

0.0445

0.0581

R1 [I>2sigma(I)]

0.0455

0.0194

0.0266

GOOF (obs.)

1.187

1.006

1.030

Deltazetamax.(eÅ-3), Deltazetamin.(eÅ-3)

1.428, -1.407

0.111, -0.088

0.318, -0.366

CSD-Nummer

410 933

 

411 317


113

Tab. A7 The Complex Structures and Hydrates

Formula

Na5[N(CH3)4](PO3F)3·18H2O

[C(NH2)3]2PO3F

Formula weight

807.3

218.15

Crystal system

Triclinic

Monoclinic

Space group

Pî

Cm

Crystal Size

0.4 x 0.2 x 0.1

0.6 x 0.5 x 0.4

a

6.438(2)

13.201(3)

b

13.438(4)

7.291(1)

c

19.520(5)

11.680(2)

á

89.38(3)

90

â

88.84(3)

119.72(3)

gamma

88.18(3)

90

V3, Z

1687.5(8), 2

976.3(3), 4

rhocalc./g·cm -3

1.589

1.484

Abs. corr. Method/ µ/mm-1

None, 0.348

None, 0.290

Diffractometer

IPDS

STADI-4

Temperature/K

180(2)

180(2)

2theta range for data collection/°

3.5-54.2

6.2-50.0

Reflections collected

15107

1847

Data/restraints/parameters

5634/3/536

1844/12/181

wR2

0.0535

0.1097

R1 [I>2sigma(I)]

0.0306

0.0424

GOOF (obs.)

0.857

1.055

Deltazetamax.(eÅ-3), Deltazetamin.(eÅ-3)

0.245, -0.347

0.521, -0.280

Tab. A8 The Structure of beta-RbHPO3F

Formula

beta-RbHPO3F

Formula weight

184.45

Crystal system

Monoclinic

Space group

P21/n

Crystal Size

0.2 x 0.2 x 0.2

a

7.5157(8)

b

7.7244(7)

c

7.5582(8)

â

104.29(1)

V3, Z

425.21(7), 4

rhocalc./g·cm -3

2.877

Abs. corr. Method/ µ/mm-1

Numerical, 11.907

Transmission, min./max.

0.0861, 0.1569

Diffractometer

IPDS

Temperature/K

180(2)

2theta range for data collection/°

3.5-54.2

Reflections collected

2291

Data/restraints/parameters

757/1/60

wR2

0.0827

R1 [I>2sigma(I)]

0.0352

GOOF (obs.)

1.002

Deltazetamax.(eÅ-3), Deltazetamin.(eÅ-3)

1.038, -0.792


114

A.2 Atomic Coordinates and Equivalent Isotropic Displacement Parameters (Å2)

Tab. A9 NaHPO3F·2.5H2O

 

x

y

z

Ueq

Na

0.02129(4)

0.91511(2)

0.37976(6)

0.0148(2)

P

0.16319(2)

0.15824(9)

0.28108(4)

0.0117(2)

O1

0.08393(7)

0.1121(3)

0.2672(1)

0.0166(3)

O2

0.18950(7)

0.0805(3)

0.1870(1)

0.0157(3)

O3

0.18251(8)

0.4378(3)

0.3152(1)

0.0201(3)

F

0.21320(6)

0.0128(3)

0.3872(1)

0.0246(3)

Ow4

0.12324(8)

0.6499(3)

0.48432(1)

0.0172(3)

Ow5

0.06758(8)

0.8010(3)

0.0343(1)

0.0172(3)

Ow6

0

0.5747(4)

0.25

0.0185(4)

H1

0.223(2)

0.484(7)

0.309(3)

0.06(1)

H4A

0.148(1)

0.609(5)

0.444(2)

0.032(7)

H4B

0.148(2)

0.711(5)

0.538(2)

0.030(7)

H5A

0.080(2)

0.657(6)

0.015(2)

0.043(8)

H5B

0.107(2)

0.871(6)

0.079(3)

0.043(8)

H6

0.036(2)

0.478(6)

0.255(3)

0.052(9)

Tab. A10 [NH2Et2]HPO3F

 

x

y

z

Ueq

P

0.22352(3)

0.05963(4)

0.12262(3)

0.0182(1)

O1

0.1212(1)

0.0290(1)

0.0787(1)

0.0302(4)

O2

0.2702(1)

0.2002(1)

0.1062(1)

0.0324(4)

O3

0.3047(1)

-0.0547(1)

0.0988(1)

0.0327(4)

F

0.2098(1)

0.0427(1)

0.23676(8)

0.0448(3)

N

0.4876(1)

0.2129(2)

0.5140(1)

0.0207(4)

C1

0.5412(2)

0.2819(2)

0.5989(2)

0.0299(5)

C2

0.5830(2)

0.1735(3)

0.6689(2)

0.0421(6)

C3

0.4461(2)

0.3121(2)

0.4381(2)

0.0267(5)

C4

0.3829(2)

0.2343(3)

0.3626(2)

0.0419(6)

H1

0.280(2)

-0.122(2)

0.104(2)

0.033(7)

H2

0.534(2)

0.155(2)

0.485(2)

0.034(6)

H3

0.435(2)

0.157(2)

0.536(2)

0.047(7)

H4

0.492(2)

0.338(2)

0.629(2)

0.030(5)

H5

0.596(2)

0.340(2)

0.571(2)

0.030(5)

H6

0.616(2)

0.215(2)

0.721(2)

0.048(7)

H7

0.632(2)

0.114(2)

0.634(2)

0.049(7)

H8

0.527(2)

0.115(2)

0.696(2)

0.047(6)

H9

0.505(2)

0.359(2)

0.410(2)

0.029(5)

H10

0.406(2)

0.377(2)

0.476(2)

0.040(6)

H11

0.359(2)

0.301(3)

0.312(2)

0.055(7)

H12

0.324(2)

0.186(3)

0.395(2)

0.061(7)

H13

0.427(2)

0.166(2)

0.327(2)

0.054(7)

Tab. A11 [PipzH2][HPO3F]2

 

x

y

z

Ueq

P

0.15681(6)

0.66043(3)

0.53021(5)

0.0153(2)

O1

0.3739(2)

0.6412(1)

0.4547(2)

0.0311(3)

O2

0.1346(2)

0.62421(7)

0.7239(1)

0.0203(3)

O3

0.0786(2)

0.77375(8)

0.5135(2)

0.0227(3)

F

-0.0267(2)

0.60235(7)

0.4048(1)

0.0360(3)

N

0.5382(2)

0.5280(1)

0.1913(2)

0.0172(3)

C1

0.6113(2)

0.5967(1)

0.0440(2)

0.0187(3)

C2

0.3403(2)

0.4650(1)

0.1238(2)

0.0206(3)

H1

0.091(4)

0.796(2)

0.422(3)

0.043(7)

H2

0.643(3)

0.486(2)

0.228(2)

0.025(4)

H3

0.500(3)

0.563(2)

0.279(3)

0.030(5)

H4

0.740(3)

0.632(2)

0.090(3)

0.027(5)

H5

0.499(4)

0.642(2)

0.010(3)

0.033(5)

H6

0.222(3)

0.510(2)

0.101(3)

0.023(4)

H7

0.311(3)

0.426(2)

0.208(3)

0.030(5)


115

Tab. A12 KHPO3F

 

x

y

z

Ueq

K1

0.5100(1)

0.40632(8)

0.1939(1)

0.0162(2)

K2

0.1961(2)

0.40318(8)

0.7212(1)

0.0152(2)

K3

0.8080(2)

0.14393(8)

0.5916(1)

0.0167(3)

K4

0.1210(1)

0.17410(7)

0.0744(2)

0.0157(2)

P1

0.7004(2)

0.39931(9)

0.7144(1)

0.0119(2)

P2

0.0522(2)

0.41638(8)

0.2179(2)

0.0116(3)

P3

0.3543(2)

0.64428(9)

-0.1155(2)

0.0109(3)

P4

0.7018(2)

0.66338(8)

0.4077(2)

0.0137(3)

O1

0.6127(5)

0.3513(3)

0.8652(4)

0.0195(8)

O2

0.8296(5)

0.3413(2)

0.6083(4)

0.0201(9)

O3

0.5457(5)

0.4443(3)

0.6009(5)

0.0251(8)

F1

0.8113(5)

0.4863(2)

0.7860(4)

0.0375(8)

O4

0.1452(5)

0.3715(2)

0.0688(4)

0.0165(8)

O5

0.1657(4)

0.4533(2)

0.3647(4)

0.0189(8)

O6

-0.1111(5)

0.3526(3)

0.2815(5)

0.0282(9)

F2

-0.0571(5)

0.5047(2)

0.1426(4)

0.0367(8)

O7

0.2168(5)

0.6033(2)

-0.2366(4)

0.0181(8)

O8

0.5029(5)

0.7069(3)

-0.1885(5)

0.0183(8)

O9

0.2622(4)

0.6917(2)

0.0458(4)

0.0143(7)

F3

0.4580(4)

0.5588(2)

-0.0267(4)

0.0311(8)

O10

0.8001(5)

0.7052(3)

0.2599(4)

0.0221(9)

O11

0.5869(5)

0.5764(2)

0.3690(5)

0.0290(9)

O12

0.5777(6)

0.7374(3)

0.4983(5)

0.035(1)

F4

0.8442(4)

0.6326(3)

0.5509(4)

0.0332(8)

H1

0.59(1)

0.473(5)

0.536(8)

0.09(3)

H2

-0.12(1)

0.348(7)

0.39(1)

0.109

H3

0.302(8)

0.753(4)

0.066(8)

0.05(2)

H4

0.550(7)

0.719(4)

0.609(7)

0.029

Tab. A13 K3[H(PO3F)2]

 

x

y

z

Ueq

Occ

K1

0.50

0.63681(1)

0.25

0.0094(5)

 

K2

0.4051(3)

0.8672(2)

0.5626(2)

0.0419(6)

 

P

0.2898(2)

0.3822(1)

0.3230(2)

0.0056(5)

 

O1

0.2775(5)

0.2711(3)

0.2435(5)

0.0135(9)

 

O2

0.2184(5)

0.4869(3)

0.2286(5)

0.0126(9)

 

O3

0.4794(5)

0.4014(3)

0.4514(5)

0.0137(9)

 

F

0.1614(5)

0.3655(3)

0.4124(4)

0.0157(8)

 

H

0.50(2)

0.464(4)

0.47(2)

0.016

0.50

Tab. A14 CsHPO3F

 

x

y

z

Ueq

Occ.

Cs

0.36639(1)

0.5000

0.59125(3)

0.0196(1)

 

P

0.11792(7)

0.5000

0.839(2)

0.0179(2)

 

O1

0.1593(2)

0.5000

0.6146(5)

0.0246(6)

 

O2

0.0630(1)

0.7137(4)

0.8726(3)

0.0245(4)

 

F

0.2034(2)

0.5000

1.0808(4)

0.0355(6)

 

H

0.034(4)

0.68(1)

0.96(1)

0.03(2)

0.5


116

Tab. A15 [NHEt3]HPO3F

 

x

y

z

Ueq

Occ.

P

0.18183(4)

0.08544(6)

0.01316(5)

0.0362(2)

 

O1

0.3090(1)

0.0467(2)

0.0479(1)

0.0568(5)

 

O2

0.1412(2)

-0.0172(2)

-0.0876(2)

0.0555(5)

 

O3

0.0846(1)

0.0965(2)

0.1067(2)

0.0579(5)

 

F

0.1894(2)

0.2602(2)

-0.0395(2)

0.0873(6)

 

N

1.0329(1)

0.6032(2)

0.2838(2)

0.0340(4)

 

C1

0.9881(2)

0.4313(2)

0.2716(3)

0.0566(7)

 

C2

0.8854(3)

0.4106(3)

0.1895(3)

0.0723(9)

 

C3

0.9285(2)

0.7099(2)

0.3300(2)

0.0385(5)

 

C4

0.9748(2)

0.8652(3)

0.3818(2)

0.0521(6)

 

C5

1.0953(2)

0.6775(3)

0.1809(2)

0.0451(5)

 

C6

1.2163(2)

0.5962(5)

0.1469(3)

0.0610(7)

 

H1A

0.074(4)

-0.027(4)

-0.090(3)

0.02(1)

0.5

H1B

0.017(2)

0.090(7)

0.095(6)

0.08(2)

0.5

H2

1.089(2)

0.595(2)

0.335(2)

0.042(6)

 

H3

0.956(2)

0.332(2)

0.321(2)

0.026(4)

 

H4

1.058(3)

0.369(3)

0.243(2)

0.067(8)

 

H5

0.809(3)

0.481(4)

0.209(3)

0.10(1)

 

H6

0.864(3)

0.285(4)

0.192(2)

0.077(8)

 

H7

0.928(3)

0.443(4)

0.106(3)

0.093

 

H8

0.873(2)

0.735(3)

0.266(2)

0.049(6)

 

H9

0.883(2)

0.644(3)

0.388(2)

0.050(6)

 

H10

0.906(3)

0.928(3)

0.413(3)

0.069(8)

 

H11

1.017(3)

0.938(3)

0.324(3)

0.070(8)

 

H12

1.036(3)

0.839(4)

0.444(3)

0.076(9)

 

H13

1.032(2)

0.675(3)

0.119(2)

0.058(7)

 

H14

1.114(2)

0.797(3)

0.198(2)

0.056(7)

 

H15

1.266(3)

0.588(3)

0.208(3)

0.066(8)

 

H16

1.258(3)

0.652(4)

0.094(3)

0.09(1)

 

H17

1.201(3)

0.490(5)

0.126(3)

0.10(1)

 

Tab. A16 [C(NH2)3]HPO3F

 

x

y

z

Ueq

P

0.8442(1)

0.60983(8)

0.12227(9)

0.0228(3)

O1

0.6929(3)

0.6236(2)

0.2091(2)

0.0291(6)

O2

1.0434(4)

0.5456(3)

0.1909(3)

0.0416(7)

O3

0.7411(4)

0.5497(4)

-0.0294(3)

0.065(1)

F

0.8974(5)

0.7512(2)

0.0819(5)

0.089(1)

C

0.3386(4)

0.6249(3)

0.5526(3)

0.0200(7)

N1

0.3315(5)

0.7253(4)

0.4580(4)

0.0340(7)

N2

0.2422(5)

0.5139(3)

0.5065(4)

0.0269(6)

N3

0.4456(5)

0.6396(3)

0.6926(3)

0.0285(7)

H1

0.825(8)

0.520(5)

-0.068(6)

0.07(2)

H2

0.253(7)

0.718(4)

0.372(5)

0.05(1)

H3

0.388(7)

0.799(5)

0.489(5)

0.05(1)

H4

0.163(5)

0.505(3)

0.425(4)

0.019(9)

H5

0.245(6)

0.463(4)

0.570(5)

0.04(1)

H6

0.518(5)

0.701(4)

0.715(4)

0.016(9)

H7

0.457(5)

0.565(4)

0.740(4)

0.023(9)


117

Tab. A17 {HOC[NH(CH3)2]2}HPO3F

 

X

y

z

Ueq

P

0.4653(1)

0.56673(3)

0.19277(7)

0.0239(2)

O1

0.4761(3)

0.64289(9)

0.2717(2)

0.0303(4)

O2

0.2754(3)

0.55796(9)

0.0435(2)

0.0319(4)

O3

0.7314(3)

0.5424(1)

0.1749(2)

0.0345(5)

F

0.4018(3)

0.50873(8)

0.3169(2)

0.0496(5)

O4

1.2574(3)

0.7426(1)

0.6445(2)

0.0375(5)

N1

0.9490(4)

0.8121(1)

0.4879(2)

0.0284(5)

N2

0.9383(4)

0.6813(1)

0.4955(3)

0.0270(5)

C1

1.0484(5)

0.7466(1)

0.5418(3)

0.0243(5)

C2

0.7145(5)

0.8192(2)

0.3774(3)

0.0297(6)

C3

1.0453(7)

0.6083(2)

0.5563(4)

0.0396(7)

H1

0.746(7)

0.512(2)

0.096(5)

0.09(1)

H2

1.340(6)

0.789(2)

0.686(4)

0.06(1)

H3

1.030(5)

0.849(2)

0.511(3)

0.027(7)

H4

0.808(5)

0.683(1)

0.429(3)

0.025(7)

H5

0.685(6)

0.874(2)

0.355(3)

0.054(9)

H6

0.600(5)

0.799(2)

0.428(3)

0.034(7)

H7

0.732(4)

0.794(1)

0.283(3)

0.021(6)

H8

1.066(7)

0.611(2)

0.672(5)

0.08(1)

H9

0.930(8)

0.571(2)

0.517(5)

0.09(1)

H10

1.200(8)

0.608(2)

0.528(4)

0.08(1)

Tab. A18 alpha-NH4HPO3F

 

x

y

z

Ueq

P1

0.2399(1)

0.03512(5)

0.77387(9)

0.0142(2)

P2

0.6215(1)

0.29611(4)

0.7249(1)

0.0155(2)

O1

0.3598(3)

-0.0184(1)

0.6930(3)

0.0202(5)

O2

0.1142(3)

-0.0087(1)

0.8629(3)

0.0223(5)

O3

0.1253(3)

0.1039(2)

0.6368(3)

0.0300(6)

F1

0.3787(3)

0.0897(1)

0.9314(3)

0.0342(5)

O4

0.7232(3)

0.2384(1)

0.6322(3)

0.0197(5)

O5

0.7364(3)

0.3592(1)

0.8632(3)

0.0225(5)

O6

0.4450(3)

0.3369(2)

0.5810(3)

0.0277(5)

F2

0.5264(3)

0.2356(1)

0.8339(3)

0.0315(5)

N1

0.7727(4)

0.5528(2)

0.8033(4)

0.0193(5)

N2

0.6024(4)

0.2009(2)

0.2506(4)

0.0186(5)

H1

0.175(6)

0.114(3)

0.570(5)

0.06(2)

H2

0.419(5)

0.389(3)

0.603(5)

0.03(1)

H3

0.778(4)

0.612(2)

0.802(4)

0.013(7)

H4

0.851(5)

0.531(2)

0.766(5)

0.03(1)

H5

0.773(5)

0.538(2)

0.914(6)

0.029(9)

H6

0.669(6)

0.532(2)

0.737(5)

0.022(9)

H7

0.594(5)

0.143(3)

0.250(5)

0.03(1)

H8

0.637(4)

0.220(2)

0.355(5)

0.016(8)

H9

0.492(7)

0.220(3)

0.208(6)

0.05(1)

H10

0.657(6)

0.221(2)

0.180(6)

0.04(1)


118

Tab. A19 beta-NH4HPO3F bei 180 K

 

x

y

z

Ueq

P1

0.2828(2)

0.7668(2)

0.0577(1)

0.0118(3)

P2

0.2561(2)

0.2616(2)

0.4014(1)

0.0122(3)

O1

0.1828(4)

0.6663(4)

-0.0341(4)

0.0171(7)

O2

0.3862(4)

0.8794(4)

-0.0504(4)

0.0183(7)

O3

0.4203(5)

0.6375(5)

0.1959(4)

0.0236(8)

F1

0.1180(4)

0.9142(4)

0.1698(4)

0.0229(6)

O4

0.1440(4)

0.2003(4)

0.5502(4)

0.0165(7)

O5

0.3509(5)

0.4012(4)

0.4286(4)

0.0177(7)

O6

0.3975(5)

0.0798(5)

0.3129(5)

0.0240(8)

F2

0.1075(4)

0.3647(4)

0.2595(4)

0.0256(7)

N1

0.1990(6)

0.2899(6)

0.8873(5)

0.0162(8)

N2

0.7791(6)

0.2082(6)

0.4029(6)

0.0180(8)

H1

0.38(1)

0.56(1)

0.26(1)

0.07(3)

H2

0.47(1)

0.11(1)

0.24(1)

0.09(3)

H3

0.193(6)

0.274(6)

0.782(7)

0.00(1)

H4

0.286(9)

0.175(9)

0.928(8)

0.03(2)

H5

0.089(7)

0.296(7)

0.947(6)

0.01(1)

H6

0.228(8)

0.392(8)

0.901(7)

0.02(1)

H7

0.66(1)

0.285(9)

0.434(8)

0.03(2)

H8

0.80(1)

0.08(1)

0.411(9)

0.04(2)

H9

0.86(1)

0.224(9)

0.472(9)

0.04(2)

H10

0.793(9)

0.238(9)

0.298(9)

0.03(2)

Tab. A20 beta-NH4HPO3F bei 310 K

 

x

y

z

Ueq

P1

0.21852(5)

0.73469(5)

0.44267(5)

0.0198(1)

P2

0.24396(5)

0.23839(5)

0.10035(4)

0.0204(1)

O1

0.3166(2)

0.8352(2)

0.5324(2)

0.0292(3)

O2

0.1160(2)

0.6229(2)

0.5508(2)

0.0313(3)

O3

0.0828(2)

0.8611(2)

0.3052(2)

0.0381(3)

F1

0.3805(2)

0.5886(2)

0.3305(1)

0.0381(3)

O4

0.3536(2)

0.3018(2)

-0.0471(1)

0.0286(3)

O5

0.1518(2)

0.0993(2)

0.0723(2)

0.0304(3)

O6

0.1035(2)

0.4168(2)

0.1891(2)

0.0393(3)

F2

0.3912(2)

0.1372(2)

0.2410(1)

0.0426(3)

N1

0.2991(2)

0.2121(2)

0.6151(2)

0.0259(3)

N2

0.2785(2)

0.7102(2)

0.9033(2)

0.0293(3)

H1

0.111(4)

0.930(4)

0.248(4)

0.064(9)

H2

0.041(5)

0.397(5)

0.265(4)

0.08(1)

H3

0.411(3)

0.198(3)

0.557(3)

0.035(5)

H4

0.305(3)

0.224(3)

0.720(3)

0.041(6)

H5

0.275(4)

0.115(4)

0.603(3)

0.050(7)

H6

0.207(4)

0.315(4)

0.575(4)

0.056(7)

H7

0.296(3)

0.593(4)

0.915(3)

0.047(7)

H8

0.356(4)

0.729(4)

0.959(3)

0.052(7)

H9

0.156(4)

0.779(3)

0.935(3)

0.042(6)

H10

0.295(3)

0.752(3)

0.794(3)

0.039(6)

Tab. A21 alpha-RbHPO3F

 

x

y

z

Ueq

Rb1

0.24359(9)

0.45173(4)

1.22459(7)

0.0159(2)

Rb2

0.06693(9)

0.29538(4)

0.74534(7)

0.0169(2)

P1

0.2415(2)

0.5334(1)

0.7329(2)

0.0113(4)

P2

0.5926(2)

0.2973(1)

0.7197(2)

0.0132(4)

O1

0.1455(6)

0.4763(3)

0.8344(6)

0.019(1)

O2

0.3619(6)

0.4943(3)

0.6239(6)

0.020(1)

O3

0.3532(7)

0.6072(3)

0.8516(6)

0.024(1)

F1

0.0875(6)

0.5838(3)

0.5883(5)

0.0270(9)

O4

0.6814(7)

0.2308(3)

0.6317(5)

0.021(1)

O5

0.7163(6)

0.3612(3)

0.8410(5)

0.016(1)

O6

0.4259(8)

0.3401(4)

0.5789(6)

0.026(1)

F2

0.4890(6)

0.2490(3)

0.8487(5)

0.0261(9)

H1

0.35(1)

0.615(6)

0.949(5)

0.050

H2

0.40(1)

0.389(6)

0.60(1)

0.05(3)


119

Tab. A22 Non-hydrogen atoms in Cs3(NH4)2(HPO3F)3(PO3F)

 

x

y

z

Ueq

Occ.

Cs1

0.13882(2)

0.10401(4)

0.01109(3)

0.0244(1)

 

Cs2

0.20242(2)

0.93719(3)

0.31106(3)

0.0242(1)

 

Cs3

0.97521(2)

0.42686(3)

0.81963(3)

0.0238(1)

 

Cs4

0.36551(2)

0.88035(4)

0.99348(3)

0.0294(2)

 

Cs5

0.52003(3)

0.57770(4)

0.16689(3)

0.0327(2)

 

Cs6

0.28876(3)

0.42022(4)

0.18731(3)

0.0328(2)

 

P1

0.18478(9)

0.8735(1)

0.8592(1)

0.0186(4)

 

P2

0.31651(9)

0.1094(1)

0.1507(1)

0.0201(4)

 

P3

0.12436(9)

0.0277(1)

0.5109(1)

0.0175(4)

 

P4

0.04636(9)

0.8883(1)

0.1288(1)

0.0158(3)

 

P5

0.36480(9)

0.9827(1)

0.4923(1)

0.0218(4)

 

P6

0.55004(9)

0.8957(1)

0.1278(1)

0.0191(4)

 

P7

0.12612(8)

0.2397(1)

0.7710(1)

0.0137(3)

 

P8

0.37535(9)

0.7689(1)

0.2506(1)

0.0194(4)

 

O1

0.2213(3)

0.7880(4)

0.9181(3)

0.028(1)

 

O2

0.1163(3)

0.9042(4)

0.8644(4)

0.031(1)

 

O3

0.2289(3)

0.9768(4)

0.8596(5)

0.040(2)

 

F1

0.1788(3)

0.8269(4)

0.7647(3)

0.041(1)

 

O4

0.2815(3)

0.1946(4)

0.0895(3)

0.029(1)

 

O5

0.3867(3)

0.0827(4)

0.1516(4)

0.036(1)

 

O6

0.2731(3)

0.0044(5)

0.1459(4)

0.040(2)

 

F2

0.3159(3)

0.1561(4)

0.2430(3)

0.051(1)

 

O7

0.0998(3)

-0.0502(4)

0.4389(3)

0.026(1)

 

O8

0.1581(3)

-0.0170(4)

0.5956(3)

0.030(1)

 

O9

0.1648(3)

0.1246(4)

0.4825(4)

0.031(1)

 

F3

0.0608(3)

0.0895(4)

0.5267(3)

0.038(1)

 

O10

0.0005(3)

0.8100(4)

0.0728(3)

0.026(1)

 

O11

0.1164(3)

0.8973(4)

0.1207(3)

0.023(1)

 

O12

0.0442(3)

0.8730(5)

0.2253(3)

0.030(1)

 

F4

0.0160(2)

1.0077(4)

0.1090(3)

0.039(1)

 

O13

0.3357(3)

1.0426(5)

0.4125(4)

0.042(2)

 

O14

0.3953(3)

1.0463(4)

0.5704(3)

0.034(1)

 

O15

0.4128(4)

0.8928(6)

0.4742(4)

0.054(2)

 

F5

0.3072(3)

0.9140(5)

0.5158(4)

0.065(2)

 

O16

0.6208(3)

0.9136(4)

0.1286(4)

0.035(1)

 

O17

0.5129(3)

0.8114(4)

0.0687(3)

0.033(1)

 

O18

0.5398(3)

0.8800(6)

0.2208(4)

0.037(1)

 

F6

0.5153(3)

1.0098(4)

0.1012(3)

0.039(1)

 

O19

0.0603(2)

0.1873(4)

0.7321(3)

0.026(1)

 

O20

0.1788(3)

0.1621(4)

0.8148(4)

0.038(1)

 

O21

0.1222(3)

0.3417(4)

0.8224(4)

0.038(1)

 

F7

0.1510(3)

0.2818(4)

0.6896(3)

0.044(1)

 

O22

0.3263(7)

0.8191(9)

0.178(1)

0.038(3)

0.65(2)

O23

0.4451(5)

0.788(1)

0.2597(8)

0.060(4)

0.65(2)

O24

0.3568(8)

0.786(1)

0.3370(7)

0.067(5)

0.65(2)

F8

0.3607(4)

0.6434(4)

0.2453(5)

0.073(2)

 

O22A

0.310(1)

0.824(2)

0.213(1)

0.022(4)

0.35(2)

O23A

0.4246(8)

0.771(1)

0.191(1)

0.031(5)

0.35(2)

O24A

0.4079(8)

0.803(2)

0.340(1)

0.037(6)

0.35(2)

N1

0.2959(3)

0.2594(6)

0.4225(5)

0.022(1)

 

N2

0.4581(3)

0.2470(5)

0.0872(4)

0.019(1)

 

N3

0.7965(3)

0.2634(5)

0.9162(4)

0.019(1)

 

N4

0.9655(3)

0.2513(5)

0.0813(4)

0.017(1)

 


120

Tab. A23 Hydrogen atoms in Cs3(NH4)2(HPO3F)3(PO3F)

 

x

y

z

Ueq

H1

0.209(2)

1.020(3)

0.843(7)

0.049

H2

0.290(3)

-0.034(3)

0.173(6)

0.048

H3

0.155(4)

0.135(6)

0.440(2)

0.037

H4

0.012(5)

0.855(8)

0.228(6)

0.036

H5

0.403(4)

0.877(8)

0.431(3)

0.065

H6

0.509(3)

0.858(8)

0.218(7)

0.045

H7

0.321(3)

0.293(6)

0.413(6)

0.027

H8

0.262(2)

0.271(7)

0.406(6)

0.027

H9

0.305(4)

0.204(3)

0.416(6)

0.027

H10

0.293(5)

0.258(7)

0.467(3)

0.027

H11

0.488(3)

0.266(7)

0.115(5)

0.023

H12

0.470(4)

0.223(7)

0.053(4)

0.023

H13

0.442(4)

0.204(5)

0.104(5)

0.023

H14

0.441(4)

0.297(4)

0.089(6)

0.023

H15

0.791(4)

0.252(7)

0.959(3)

0.022

H16

0.810(4)

0.318(4)

0.918(5)

0.022

H17

0.818(4)

0.225(6)

0.901(5)

0.022

H18

0.767(3)

0.243(7)

0.893(5)

0.022

H19

0.993(3)

0.266(7)

0.116(4)

0.021

H20

0.978(4)

0.223(6)

0.048(4)

0.021

H21

0.948(4)

0.303(4)

0.072(5)

0.021

H22

0.948(4)

0.204(5)

0.092(5)

0.021

Tab. A24 [N(CH3)4]HPO3F·H2O

 

x

y

z

Ueq

Occ.

P

0.05561(3)

0.05561(3)

0.05561(3)

0.0240(2)

 

O1

0.0071(2)

-0.0585(2)

0.1483(2)

0.0451(5)

0.888(4)

F

0.14874(8)

0.14874(8)

0.14874(8)

0.0569(5)

 

O1A

0.083(1)

-0.0887(9)

0.099(1)

0.037(3)

0.112(4)

Ow2

0.1796(2)

0.8204(2)

0.3204(2)

0.0413(7)

0.888(4)

Ow2A

0.132(1)

0.868(1)

0.368(1)

0.036(4)

0.112(4)

N

1.0840(1)

0.58340(1)

0.9160(1)

0.0228(4)

 

C1

1.1731(1)

0.6731(1)

0.8269(1)

0.0300(5)

 

C2

0.9448(1)

0.6488(2)

0.9292(2)

0.0439(4)

 

H1

1.133(2)

0.674(2)

0.738(2)

0.039(4)

 

H2

0.956(2)

0.735(2)

0.976(2)

0.052(5)

 

H3

0.893(2)

0.588(2)

0.981(2)

0.064(6)

 

H4

0.911(2)

0.659(2)

0.838(2)

0.049(5)

 

H5

0.044(9)

-0.076(9)

0.201(9)

0.07(3)

0.296(2)

H6

0.224(3)

0.870(3)

0.348(3)

0.040(8)

0.592(3)


121

Tab. A25 Na2PO3F·10H2O

 

x

y

z

Ueq

Occ.

Na1

0.76241(5)

0.11186(4)

0.23800(4)

0.0157(1)

 

Na2

0.75240(5)

0.24128(4)

0.49222(4)

0.0165(1)

 

P

0.25291(3)

0.13985(3)

0.25237(2)

0.01163(9)

 

O1

0.24389(9)

0.18154(9)

0.36111(7)

0.0199(2)

 

O2

0.28236(9)

-0.00249(8)

0.24331(7)

0.0215(2)

 

O3

0.15381(9)

0.19442(9)

0.16000(7)

0.0221(2)

 

F

0.37463(8)

0.21322(8)

0.24354(7)

0.0276(2)

 

Ow4

0.35762(9)

0.4508(1)

0.38698(8)

0.0198(2)

 

Ow5

0.8857(1)

-0.04265(9)

0.35764(8)

0.0197(2)

 

Ow6

0.6478(1)

0.28448(9)

0.12452(7)

0.0176(2)

 

Ow7

0.8947(1)

0.1170(1)

0.11909(8)

0.0193(2)

 

Ow8

0.8532(1)

0.28569(9)

0.35744(7)

0.0176(2)

 

Ow9

0.6232(1)

0.1030(1)

0.35289(8)

0.0219(2)

 

Ow10

0.3867(1)

0.57609(9)

0.58247(8)

0.0216(2)

 

Ow11

0.8622(1)

0.45990(9)

0.05456(8)

0.0213(2)

 

Ow12

0.09908(9)

0.35056(9)

0.44299(8)

0.0187(2)

 

Ow13

0.3965(1)

0.1486(1)

0.56141(8)

0.0242(2)

 

H4A

0.330(2)

0.383(2)

0.378(2)

0.031(5)

 

H4B

0.354(2)

0.476(2)

0.442(2)

0.054(6)

 

H5A

0.872(2)

-0.122(2)

0.3482(2)

0.033(5)

 

H5B

0.870(2)

-0.021(2)

0.415(2)

0.018(6)

0.67

H5C

0.959(7)

-0.042(5)

0.376(4)

0.02(1)

0.33

H6A

0.671(2)

0.352(2)

0.160(2)

0.040(5)

 

H6B

0.574(2)

0.293(2)

0.098(2)

0.043(6)

 

H7A

0.967(2)

0.140(2)

0.140(2)

0.048(6)

 

H7B

0.899(2)

0.041(2)

0.102(2)

0.042(5)

 

H8A

0.825(2)

0.353(2)

0.330(2)

0.033(5)

 

H8B

0.929(2)

0.302(2)

0.382(1)

0.033(5)

 

H9A

0.558(2)

0.134(2)

0.327(2)

0.045(6)

 

H9B

0.615(2)

0.031(2)

0.375(1)

0.029(5)

 

H10A

0.367(2)

0.5445(2)

0.633(2)

0.030(5)

 

H10B

0.460(2)

0.571(2)

0.6052(2)

0.052(7)

 

H11A

0.834(2)

0.511(2)

0.085(2)

0.041(5)

 

H11B

0.934(3)

0.458(3)

0.093(2)

0.031(7)

0.67

H11C

0.839(5)

0.484(5)

-0.027(5)

0.03(1)

0.33

H12A

0.139(2)

0.295(2)

0.416(1)

0.030(4)

 

H12B

0.118(2)

0.340(2)

0.506(2)

0.035(5)

 

H13A

0.354(2)

0.153(2)

0.499(2)

0.036(5)

 

H13B

0.365(2)

0.196(2)

0.598(2)

0.036(5)

 


122

Tab. A26 Non-hydrogen atoms in Na5[N(CH3)4](PO3F)3·18H2O

 

x

y

z

Ueq

Na1

0.0006(2)

0.55757(7)

0.57768(5)

0.0180(2)

Na2

0.75154(15)

0.74930(7)

0.63313(5)

0.0157(2)

Na3

0.0146(2)

0.06404(7)

0.42505(5)

0.0180(2)

Na4

0.0846(2)

0.19265(7)

0.04182(5)

0.0184(2)

Na5

0.3565(2)

0.68056(7)

0.94487(5)

0.0206(2)

P1

0.3794(1)

0.24486(4)

0.59976(3)

0.0098(1)

P2

0.3528(1)

0.53017(4)

0.80604(3)

0.0112(2)

P3

0.6190(1)

0.03386(4)

0.19290(3)

0.0106(1)

O1

0.1495(3)

0.2480(1)

0.58915(9)

0.0176(4)

O2

0.4898(3)

0.3347(1)

0.57294(8)

0.0157(4)

O3

0.4869(3)

0.1465(1)

0.58096(8)

0.0164(4)

F1

0.4000(2)

0.2511(1)

0.68110(7)

0.0235(4)

O4

0.4537(3)

0.5415(1)

0.87459(8)

0.0200(4)

O5

0.4792(3)

0.5640(1)

0.74478(8)

0.0198(4)

O6

0.1288(3)

0.5675(1)

0.80512(8)

0.0157(4)

F2

0.3407(3)

0.4139(1)

0.79693(8)

0.0288(4)

O7

0.3960(3)

0.0699(1)

0.18821(8)

0.0187(4)

O8

0.7483(3)

0.0983(1)

0.23695(8)

0.0165(4)

O9

0.7219(3)

0.0061(1)

0.12479(8)

0.0168(4)

F3

0.6088(2)

-0.0674(1)

0.23449(7)

0.0249(4)

Ow11

0.3342(3)

0.5137(1)

0.61589(1)

0.0182(4)

Ow12

0.8732(4)

0.5984(1)

0.6927(1)

0.0198(5)

Ow13

0.7441(3)

0.1275(2)

0.0077(1)

0.0203(4)

Ow14

0.3497(3)

0.1191(1)

0.4444(1)

0.0179(4)

Ow15

0.8649(4)

0.5016(2)

0.9041(1)

0.0239(5)

Ow16

0.1015(4)

0.6031(1)

0.4592(1)

0.0199(4)

Ow17

0.1294(4)

0.1105(2)

0.3031(1)

0.0206(4)

Ow18

0.3410(3)

0.3786(1)

0.4430(1)

0.0175(4)

Ow19

0.1013(3)

0.7484(1)

0.5873(1)

0.0195(4)

Ow20

0.4144(3)

0.7461(2)

0.6844(1)

0.0176(4)

Ow21

0.1337(4)

0.0170(1)

0.0882(1)

0.0213(5)

Ow22

0.3321(3)

0.1603(2)

0.9541(1)

0.0214(4)

Ow23

0.0281(3)

0.6402(1)

0.9963(1)

0.0207(4)

Ow24

0.8790(3)

0.2449(2)

0.1393(1)

0.0189(4)

Ow25

0.5402(4)

0.6294(2)

0.0384(1)

0.0275(5)

Ow26

0.6389(3)

0.7538(2)

0.8857(1)

0.0231(5)

Ow27

0.6956(3)

0.0219(1)

0.3804(1)

0.0181(4)

Ow28

0.8990(3)

0.1033(1)

0.5421(1)

0.0189(4)

N

0.8676(3)

0.2414(1)

0.7782(1)

0.0146(5)

C1

0.6814(4)

0.2377(2)

0.8247(1)

0.0254(7)

C2

0.8614(5)

0.3362(2)

0.7371(2)

0.0260(7)

C3

1.0579(4)

0.2365(2)

0.8210(1)

0.0259(7)

C4

0.8725(4)

0.1543(2)

0.7303(1)

0.0232(6)


123

Tab. A27 Hydrogen atoms in Na5[N(CH3)4](PO3F)3·18H2O

 

x

y

z

Ueq

H1A

0.685(1)

0.1748(6)

0.8506(6)

0.038

H1B

0.5550(4)

0.242(1)

0.7975(2)

0.038

H1C

0.682(1)

0.2935(7)

0.8566(6)

0.038

H2A

0.984(1)

0.3379(6)

0.7065(6)

0.039

H2B

0.861(3)

0.3930(2)

0.7681(3)

0.039

H2C

0.735(1)

0.3396(6)

0.7099(7)

0.039

H3A

1.1819(4)

0.239(1)

0.7912(2)

0.039

H3B

1.062(2)

0.1741(7)

0.8475(7)

0.039

H3C

1.055(2)

0.2930(8)

0.8524(7)

0.039

H4A

0.996(1)

0.1572(7)

0.7001(6)

0.035

H4B

0.747(1)

0.1568(7)

0.7026(6)

0.035

H4C

0.878(3)

0.0921(2)

0.7570(1)

0.035

H11A

0.380(6)

0.522(3)

0.649(2)

0.05(1)

H11B

0.385(5)

0.457(3)

0.607(2)

0.037(9)

H12A

0.957(5)

0.590(2)

0.723(2)

0.036(9)

H12B

0.771(6)

0.579(3)

0.707(2)

0.04(1)

H13A

0.722(5)

0.094(2)

0.039(2)

0.04(1)

H13B

0.778(5)

0.088(2)

-0.020(2)

0.04(1)

H14A

0.392(5)

0.125(2)

0.479(2)

0.03(1)

H14B

0.453(5)

0.090(2)

0.426(2)

0.033(9)

H15A

0.743(5)

0.515(2)

0.893(2)

0.030(9)

H15B

0.942(6)

0.511(2)

0.876(2)

0.03(1)

H16A

0.033(5)

0.646(2)

0.445(2)

0.027(9)

H16B

0.214(5)

0.619(2)

0.448(2)

0.03(1)

H17A

0.030(5)

0.108(2)

0.283(2)

0.024(9)

H17B

0.216(6)

0.093(2)

0.276(2)

0.04(1)

H18A

0.432(6)

0.412(3)

0.426(2)

0.06(1)

H18B

0.373(5)

0.362(2)

0.481(2)

0.030(9)

H19A

0.201(5)

0.745(2)

0.611(2)

0.030(9)

H19B

0.152(6)

0.749(2)

0.549(2)

0.04(1)

H20A

0.432(5)

0.694(3)

0.706(2)

0.04(1)

H20B

0.378(5)

0.787(2)

0.706(2)

0.03(1)

H21A

0.212(5)

0.026(2)

0.117(2)

0.04(1)

H21B

0.011(6)

0.016(2)

0.103(2)

0.04(1)

H22A

0.449(5)

0.152(2)

0.969(1)

0.013(7)

H22B

0.313(5)

0.119(2)

0.932(2)

0.03(1)

H23A

0.063(5)

0.607(2)

1.031(2)

0.031(9)

H23B

-0.035(6)

0.605(3)

0.974(2)

0.05(1)

H24A

0.853(6)

0.201(3)

0.170(2)

0.05(1)

H24B

0.889(5)

0.292(3)

0.157(2)

0.04(1)

H25A

0.550(5)

0.581(3)

0.063(2)

0.04(1)

H25B

0.628(6)

0.662(3)

0.049(2)

0.06(1)

H26A

0.686(7)

0.714(3)

0.864(2)

0.07(2)

H26B

0.623(5)

0.802(3)

0.861(2)

0.03(1)

H27A

0.638(6)

-0.035(3)

0.393(2)

0.05(1)

H27B

0.692(5)

0.036(2)

0.345(1)

0.03(1)

H28A

0.967(7)

0.141(3)

0.557(2)

0.07(1)

H28B

0.769(7)

0.123(3)

0.551(2)

0.06(12)


124

Tab. A28 [C(NH2)3]2PO3F

 

x

y

z

Ueq

P1

0.19730(8)

1.000

0.1253(1)

0.0193(3)

P2

0.72469(9)

1.000

0.6976(1)

0.0211(3)

O1

0.3273(3)

1.000

0.1803(3)

0.0257(8)

O2

0.1534(2)

0.8257(3)

0.1554(2)

0.0254(5)

F1

0.1423(3)

1.000

-0.0291(3)

0.0321(7)

O3

0.8559(3)

1.000

0.7739(3)

0.0274(8)

O4

0.6746(2)

0.8262(3)

0.6205(2)

0.0294(6)

F2

0.6853(3)

1.000

0.8040(3)

0.0400(8)

N1

0.4585(3)

0.8415(4)

0.9121(4)

0.0300(6)

N2

0.3000(4)

1.000

0.7566(4)

0.029(1)

N3

0.7783(4)

1.000

0.1489(5)

0.0281(9)

N4

0.9311(3)

0.8423(4)

0.1523(3)

0.0277(6)

N5

0.7691(3)

0.7556(5)

0.4428(3)

0.0334(7)

N6

0.9367(3)

0.7165(5)

0.4318(3)

0.0322(7)

N7

0.9487(3)

0.7771(5)

0.6295(3)

0.0336(7)

C1

0.4051(4)

1.000

0.8595(5)

0.0219(9)

C2

0.8796(4)

1.000

0.1506(5)

0.024(1)

C3

0.8846(3)

0.7501(5)

0.5008(4)

0.0270(7)

H1A

0.425(3)

0.742(4)

0.873(4)

0.03(1)

H1B

0.525(2)

0.835(6)

0.979(3)

0.04(1)

H2

0.264(3)

1.101(4)

0.720(4)

0.04(1)

H3

0.753(4)

0.895(4)

0.156(4)

0.04(1)

H4A

0.993(3)

0.858(6)

0.141(4)

0.023(9)

H4B

0.897(4)

0.743(4)

0.151(5)

0.05(1)

H5A

0.723(4)

0.761(7)

0.360(2)

0.05(2)

H5B

0.734(3)

0.787(6)

0.486(3)

0.03(1)

H6A

0.902(5)

0.683(9)

0.350(7)

0.07(2)

H6B

1.012(2)

0.702(6)

0.481(3)

0.03(1)

H7A

0.928(4)

0.822(6)

0.682(4)

0.04(1)

H7B

1.023(2)

0.767(5)

0.660(4)

0.03(1)

Tab. A29 beta-RbHPO3F

 

x

y

z

Ueq

Occ.

Rb

0.09942(7)

0.67077(6)

0.23383(7)

0.0203(3)

 

P

0.4166(2)

0.3151(2)

0.7413(2)

0.0228(4)

 

O1

0.5212(5)

0.1905(5)

0.6565(6)

0.0227(9)

 

O2

0.5306(6)

0.4608(5)

0.8456(6)

0.0258(9)

 

O3

0.3067(6)

0.2306(5)

0.8652(6)

0.031(1)

0.70

FA

0.3067(6)

0.2306(5)

0.8652(6)

0.031(1)

0.30

F

0.2676(5)

0.3997(6)

0.5888(5)

0.040(1)

0.70

O3A

0.2676(5)

0.3997(6)

0.5888(5)

0.040(1)

0.30

H

0.53(2)

0.50(2)

0.94(1)

0.048

0.50


125

A.3 Selected Bond Lengths

Tab. A30 K-X bond lengths in KHPO3F (Å)

 

d

 

d

 

d

 

d

K1-O1

2.738(3)

K2-O4

2.724(3)

K3-O5

2.712(4)

K4-O10

2.660(4)

K1-F3

2.757(3)

K2-O3

2.768(4)

K3-F4

2.762(3)

K4-O4

2.787(4)

K1-O11

2.801(4)

K2-O10

2.793(4)

K3-O7

2.783(4)

K4-F1

2.895(3)

K1-O8

2.810(4)

K2-O5

2.827(3)

K3-O2

2.787(4)

K4-O8

2.906(4)

K1-O4

2.861(4)

K2-O7

2.841(4)

K3-O9

2.902(3)

K4-O7

2.930(4)

K1-O5

2.904(4)

K2-O2

2.933(4)

K3-O11

3.041(4)

K4-F4

2.938(3)

K1-O6

2.934(4)

K2-F1

3.075(4)

K3-O12

3.172(5)

K4-F2

2.943(3)

K1-O3

3.171(4)

 

 

K3-O10

3.185(4)

K4-O9

2.944(4)

Tab. A31 C-H bond lengths in [NHEt3]HPO3F (Å)

 

d

 

d

 

d

C1-H3

1.06(2)

C3-H8

0.97(3)

C5-H13

0.99(3)

C1-H4

0.97(3)

C3-H9

1.00(3)

C5-H14

1.02(3)

C2-H5

1.03(4)

C4-H10

0.98(3)

C6-H15

0.89(3)

C2-H6

1.06(3)

C4-H11

1.02(3)

C6-H16

0.90(4)

C2-H7

1.12(4)

C4-H12

1.00(3)

C6-H17

0.92(4)

Tab. A32 Rb-X bond lengths in alpha-RbHPO3F (Å)

 

d

 

d

Rb1-O2

2.871(5)

Rb2-O4

2.848(4)

Rb1-O4

2.931(5)

Rb2-O2

2.916(5)

Rb1-O5

2.980(5)

Rb2-O4´

2.953(5)

Rb1-O1

2.984(5)

Rb2-F2

2.982(4)

Rb1-O1´

2.988(5)

Rb2-O5

3.070(4)

Rb1-O2´

3.034(5)

Rb2-F1

3.112(4)

Rb1-O6

3.180(5)

Rb2-O3

3.113(5)

Rb1-F1

3.205(4)

Rb2-F2´

3.123(4)

Rb1-O3

3.339(5)

Rb2-O6

3.322(5)


126

Tab. A33 Cs-X bond lengths in Cs3(NH4)2(HPO3F)3PO3F (Å)

 

d

 

d

 

d

Cs1-O10

3.072(5)

Cs2-O13

3.136(7)

Cs3-O2

3.122(6)

Cs1-F7

3.109(4)

Cs2-O21

3.167(6)

Cs3-O21

3.191(6)

Cs1-O4

3.130(6)

Cs2-O1

3.184(5)

Cs3-O7

3.205(5)

Cs1-O11

3.133(5)

Cs2-O11

3.187(5)

Cs3-O19

3.292(5)

Cs1-O2

3.313(5)

Cs2-O7

3.237(5)

Cs3-O10

3.312(5)

Cs1-O6

3.333(6)

Cs2-O22A

3.28(2)

Cs3-O12

3.321(6)

Cs1-O9

3.368(6)

Cs2-F1

3.285(5)

Cs3-F3

3.336(5)

Cs1-F4

3.448(5)

Cs2-O12

3.341(6)

Cs3-F3´

3.378(5)

Cs1-O20

3.460(7)

Cs2-O6

3.362(7)

Cs3-O8

3.381(6)

Cs1-F4´

3.604(5)

Cs2-F5

3.497(7)

Cs3-F1

3.388(5)

Cs1-O3

3.678(7)

Cs2-O24

3.61(2)

Cs3-O12´

3.696(6)

 

 

Cs2-O9

3.746(6)

Cs3-F4

3.703(5)

 

 

 

 

 

 

Cs4-O17

3.125(6)

Cs5-O14

3.079(6)

Cs6-O8

3.005(6)

Cs4-O1

3.157(6)

Cs5-O5

3.094(6)

Cs6-O16

3.103(6)

Cs4-O24

3.169(12)

Cs5-O23A

3.13(2)

Cs6-F8

3.117(5)

Cs4-O16

3.202(6)

Cs5-O17

3.211(5)

Cs6-O4

3.123(5)

Cs4-O22

3.28(2)

Cs5-O18

3.368(6)

Cs6-O14

3.193(6)

Cs4-O3

3.346(6)

Cs5-O15

3.377(6)

Cs6-F2

3.325(5)

Cs4-O23A

3.38(2)

Cs5-O23

3.459(14)

Cs6-O3

3.464(7)

Cs4-F6

3.414(5)

Cs5-O13

3.499(7)

Cs6-F5

3.465(6)

Cs4-O5

3.460(6)

Cs5-F2

3.503(6)

Cs6-O20

3.495(7)

Cs4-O15

3.472(8)

Cs5-O15´

3.641(9)

Cs6-O18

3.551(6)

Cs4-O24A

3.53(2)

Cs5-O24A

3.65(2)

Cs6-O9

3.710(6)

Cs4-F6´

3.550(5)

Cs5-O23´

3.713(14)

Cs6-F7

3.750(6)


127

Tab. A34 N-H···O hydrogen bonding in Cs3(NH4)2(HPO3F)3PO3F (Å, °)

 

d(D-H)

d(H···A)

d(D···A)

angD-H···A

N1-H7···O16

0.70(8)

2.11(8)

2.771(9)

168(10)

N1-H8···O20

0.69(4)

2.15(7)

2.802(9)

156(10)

N1-H9···O13

0.69(5)

2.09(5)

2.758(9)

172(10)

N1-H10···O4

0.72(5)

2.09(6)

2.785(9)

163(10)

N2-H11···O23

0.70(6)

2.22(7)

2.83(1)

153(9)

N2-H11···O24A

0.75(2)

2.21(6)

2.84(2)

160(9)

N2-H12···O17

0.69(8)

2.08(7)

2.758(8)

162(10)

N2-H13···O5

0.69(7)

2.11(8)

2.792(8)

176(10)

N2-H14···O14

0.72(6)

2.18(6)

2.798(8)

169(10)

N3-H15···O1

0.72(6)

2.07(6)

2.800(8)

177(9)

N3-H16···O8

0.73(5)

2.15(5)

2.832(8)

171(9)

N3-H17···O11

0.74(8)

2.06(7)

2.791(8)

170(9)

N3-H18···O22

0.65(6)

2.08(6)

2.83(1)

178(9)

N3-H18···O22A

0.65(6)

2.11(7)

2.86(2)

163(9)

N4-H19···O19

0.72(6)

2.11(6)

2.837(8)

170(9)

N4-H20···O10

0.71(8)

2.10(7)

2.786(8)

160(9)

N4-H21···O7

0.75(6)

1.99(6)

2.734(8)

172(9)

N4-H22····O2

0.73(7)

2.03(8)

2.783(8)

166(9)

Tab. A35 Na-O, N-C, and C-H bond lengths in Na5[N(CH3)4](PO3F)3·18H2O (Å)

 

d

 

d

 

d

 

d

Na1-Ow11

2.343(2)

Na2-Ow20

2.373(2)

Na3-Ow27

2.336(2)

Na4-Ow22

2.351(2)

Na1-Ow18

2.376(2)

Na2-Ow18

2.382(2)

Na3-Ow14

2.342(2)

Na4-Ow24

2.394(2)

Na1-Ow16

2.399(2)

Na2-Ow14

2.399(2)

Na3-Ow28

2.383(2)

Na4-Ow26

2.428(2)

Na1-Ow12

2.438(2)

Na2-Ow19

2.406(2)

Na3-Ow28´

2.446(2)

Na4-Ow23

2.451(2)

Na1-Ow16

2.466(2)

Na2-Ow17

2.422(2)

Na3-Ow17

2.555(3)

Na4-Ow13

2.492(2)

Na1-Ow19

2.674(2)

Na2-Ow12

2.442(2)

Na3-Ow19

2.616(2)

Na4-Ow21

2.531(2)

 

 

 

 

 

 

 

 

Na5-Ow25

2.283(2)

N-C1

1.491(4)

C1-H1C

0.98

C3-H3C

0.98

Na5-Ow26

2.369(3)

N-C2

1.497(3)

C2-H2A

0.98

C4-H4A

0.98

Na5-O4

2.390(2)

N-C3

1.497(3)

C2-H2B

0.98

C4-H4B

0.98

Na5-Ow23

2.398(2)

N-C4

1.504(3)

C2-H2C

0.98

C4-H4C

0.98

Na5-Ow24

2.443(2)

C1-H1A

0.98

C3-H3A

0.98

 

 

Na5-Ow13

2.801(2)

C1-H1B

0.98

C3-H3B

0.98

 

 


128

Tab. A36 Hydrogen bonding in Na5[N(CH3)4](PO3F)3 (Å, °)

D-H···A

D-H

H···D

D···A

angDHA

Ow11-H11A···O5

0.72(2)

2.09(3)

2.798(3)

171(3)

Ow11-H11B···O2

0.84(3)

1.87(3)

2.710(3)

171(3)

Ow12-H12A···O6

0.81(3)

1.98(3)

2.788(3)

172(3)

Ow12-H12B···O5

0.76(4)

2.02(4)

2.764(3)

165(3)

Ow13-H13A···O9

0.78(4)

2.03(4)

2.797(3)

169(3)

Ow13-H13B···Ow21

0.78(3)

2.02(4)

2.796(3)

178(3)

Ow14-H14A···O3

0.73(3)

2.13(3)

2.856(3)

174(3)

Ow14-H14B···Ow27

0.83(4)

1.99(4)

2.823(3)

178(3)

Ow15-H15A···O4

0.83(3)

1.93(3)

2.755(3)

176(3)

Ow15-H15B···O6

0.74(4)

1.98(4)

2.706(3)

166(3)

Ow16-H16A···O1

0.77(3)

1.94(3)

2.706(3)

177(3)

Ow16-H16B···O2

0.79(4)

2.05(4)

2.842(3)

174(3)

Ow17-H17A···O8

0.76(3)

2.05(3)

2.806(3)

175(3)

Ow17-H17B···O7

0.79(4)

2.07(4)

2.843(3)

165(3)

Ow18-H18A···Ow11

0.81(4)

2.00(5)

2.802(3)

176(4)

Ow18-H18B···O2

0.79(3)

1.99(3)

2.780(3)

171(3)

Ow19-H19A···Ow20

0.80(3)

2.01(3)

2.794(3)

168(3)

Ow19-H19B

0.81(4)

 

 

 

Ow20-H20A···O5

0.82(3)

1.92(3)

2.729(3)

173(3)

Ow20-H20B···O8

0.73(3)

2.05(3)

2.774(3)

174(3)

Ow21-H21A···O7

0.77(3)

1.96(3)

2.723(3)

170(3)

Ow21-H21B···O9

0.84(4)

1.91(4)

2.740(3)

171(3)

Ow22-H22A···Ow13

0.81(3)

2.08(3)

2.890(3)

178(3)

Ow22-H22B···O9

0.72(2)

2.05(2)

2.763(3)

174(3)

Ow23-H23A···Ow15

0.84(3)

1.97(3)

2.790(3)

165(3)

Ow23-H23B···Ow15

0.77(4)

2.09(4)

2.843(3)

166(4)

Ow24-H24A···O8

0.85(4)

2.02(4)

2.861(3)

171(3)

Ow24-H24B···O6

0.73(3)

2.04(4)

2.754(3)

169(3)

Ow25-H25A···O4

0.80(4)

2.04(4)

2.841(3)

174(3)

Ow25-H25B···Ow22

0.76(4)

2.41(4)

2.973(3)

132(3)

Ow26-H26A

0.74(4)

 

 

 

Ow26-H26B···O7

0.80(3)

1.97(4)

2.765(3)

171(3)

Ow27-H27A···O3

0.90(4)

1.78(4)

2.677(3)

177(3)

Ow27-H27B···O8

0.71(2)

2.29(2)

2.988(3)

167(3)

Ow28-H28A···O1

0.74(4)

2.01(4)

2.743(3)

175(4)

Ow28-H28B···O3

0.89(4)

1.91(5)

2.790(3)

170(3)


129

A.4 19F, 31P, and 1H MAS NMR Data and Spectra

Tab. A37 19F MAS NMR data

Comp.

deltaiso

deltaaniso

eta

Linewidth

area

 

(ppm) ± 0.5 ppm

(ppm) ± 5 ppm

± 0.1

(ppm) ± 0.5ppm

% ± 0.5%

d

-68.5

-67

0.0

2.0

26.4

e

-70.8

-128

0.4

2.0

27.5

c

-72.7

-54

1.0

1.3

23.8

f

-75.0

-121

0.4

1.0

22.3

Fig. A1 19F MAS NMR spectra


130

Tab. A38 31P MAS NMR data

Comp.

deltaiso

deltaaniso

eta

Linewidth

area

 

(ppm) ± 0.5 ppm

(ppm) ± 5 ppm

± 0.1

(ppm) ± 0.5ppm

% ± 0.5%

d

-7.5

-75

0.8

1.3

15.1

e

-5.9

-75

0.8

2.3

33.9

c

-2.3

-133

1.0

1.8

19.3

f

-0.3

-119

1.0

2.4

31.7

Fig. A2 31P MAS NMR spectra


131

Tab. A39 1H MAS NMR data

Comp.

deltaiso

deltaaniso

eta

Linewidth

area

 

(ppm) ± 0.5 ppm

(ppm) ± 5 ppm

± 0.1

(ppm) ± 0.5ppm

% ± 0.5%

c

13.0

-27

0.8

1.8

69.8

d

5.9

-6

0.8

0.2

30.2

Fig. A3 1H MAS NMR spectra


Fußnoten:

<2>

*Data re-refined postpublication.


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