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Crystals of germanium-doped rubidium titanyl phosphate, Rb2(Ti)(Ge0.121Ti0.879)O2(PO4)2 (GeRTP#1) and Rb2(Ge0.125­Ti0.875)(Ge0.225Ti0.775)O2(PO4)2 (GeRTP#2), have been structurally characterized from X-ray diffraction data at room temperature. In addition, a third structure, Rb2(TiO)2(PO4)2 (RTP), has been reinvestigated. The exchange of titanium for germanium results in a less distorted octahedral coordination around the two crystallographically independent titanium sites. Additionally, rubidium split-cation positions have been found in these doped RTP crystals. Dielectric measurements show that the phase-transition temperature, Tc, decreases with increasing germanium concentration, and a direct correlation between the room-temperature split of the rubidium cations and Tc has been discovered. General trends regarding the relationship between the room-temperature structures of KTP-like compounds and their Tc values are discussed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768103018688/os0109sup1.cif
Contains datablocks global, RTP, GeRTP1, GeRTP2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103018688/os0109RTP1sup2.hkl
Contains datablock RTP

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103018688/os0109GERTP1sup3.hkl
Contains datablock GERTP1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768103018688/os0109GERTP2sup4.hkl
Contains datablock GERTP2

Computing details top

For all compounds, data collection: SMART (Siemens, 1995); cell refinement: CAD-4 Software (Enraf-Nonius, 1989); data reduction: SAINT (Siemens, 1995) and SADABS (Sheldrick, 2001); program(s) used to solve structure: Atomic parameters from Norberg et al. (2000); program(s) used to refine structure: Xtal3.71 (Hall et al., 2000) program: CRYLSQ; molecular graphics: ORTEPIII for Windows (Farrugia, 1997); software used to prepare material for publication: Xtal3.71 (Hall et al., 2000) programs: BONDLA; ATABLE; CIFIO.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(RTP) top
Crystal data top
O10P2Rb2Ti2F(000) = 912
Mr = 488.64Dx = 3.645 Mg m3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: p 2c -2nCell parameters from 18 reflections
a = 12.9625 (15) Åθ = 17.9–23.9°
b = 6.5031 (3) ŵ = 13.06 mm1
c = 10.5615 (3) ÅT = 293 K
V = 890.30 (11) Å3Rectangular, colourless
Z = 40.14 × 0.12 × 0.08 mm
Data collection top
Siemens SMART CCD
diffractometer
2054 independent reflections
Radiation source: normal-focus sealed tube2054 reflections with F > 0σ(F)
Graphite monochromatorRint = 0.052
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
h = 1616
Tmin = 0.175, Tmax = 0.353k = 88
10947 measured reflectionsl = 1313
Refinement top
Refinement on F w = 1/[σ2(F) + 0.0020(F)2]
Least-squares matrix: full(Δ/σ)max = 0.001
R[F2 > 2σ(F2)] = 0.024Δρmax = 1.11 e Å3
wR(F2) = 0.037Δρmin = 0.71 e Å3
S = 1.13Extinction correction: Isotropic Gaussian, Zachariasen, 1967; Larson (1970), Eq22 p292 "Cryst. Comp." Munksgaard 1970
2054 reflectionsExtinction coefficient: 117E2 (5)
146 parametersAbsolute structure: Flack (1983) parameter refined
0 restraintsAbsolute structure parameter: 0.497 (9)
0 constraints
Crystal data top
O10P2Rb2Ti2V = 890.30 (11) Å3
Mr = 488.64Z = 4
Orthorhombic, Pna21Mo Kα radiation
a = 12.9625 (15) ŵ = 13.06 mm1
b = 6.5031 (3) ÅT = 293 K
c = 10.5615 (3) Å0.14 × 0.12 × 0.08 mm
Data collection top
Siemens SMART CCD
diffractometer
2054 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
2054 reflections with F > 0σ(F)
Tmin = 0.175, Tmax = 0.353Rint = 0.052
10947 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.037Δρmax = 1.11 e Å3
S = 1.13Δρmin = 0.71 e Å3
2054 reflectionsAbsolute structure: Flack (1983) parameter refined
146 parametersAbsolute structure parameter: 0.497 (9)
Special details top

Refinement. No constraints or restraints were used.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Rb10.61502 (4)0.78353 (9)0.70080 (11)0.0171 (3)
Rb20.89447 (4)0.69214 (9)0.95204 (11)0.0151 (3)
Ti10.62713 (6)0.49974 (12)1.02650 (12)0.0048 (4)
Ti20.75173 (6)0.26802 (12)0.77515 (13)0.0043 (4)
P10.50027 (9)0.3331 (2)0.76890 (16)0.0045 (6)
P20.82010 (9)0.50192 (16)0.51433 (14)0.0048 (5)
O10.5145 (3)0.4791 (6)0.8806 (3)0.0069 (18)
O20.4864 (3)0.4611 (6)0.6463 (3)0.0100 (18)
O30.5981 (3)0.2018 (6)0.7472 (4)0.0081 (18)
O40.4055 (3)0.1938 (6)0.7896 (4)0.0072 (17)
O110.7220 (3)0.4607 (6)0.8835 (3)0.0077 (17)
O120.7774 (3)0.0451 (6)0.6365 (3)0.0096 (18)
O50.8862 (3)0.3115 (7)0.4842 (4)0.008 (2)
O60.8871 (3)0.6904 (6)0.5421 (4)0.010 (2)
O70.7490 (3)0.5437 (6)0.3994 (3)0.0089 (17)
O80.7479 (3)0.4579 (6)0.6263 (11)0.0096 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb10.0176 (3)0.0092 (3)0.0244 (3)0.00395 (16)0.0058 (2)0.0021 (2)
Rb20.0099 (3)0.0150 (3)0.0203 (3)0.00427 (16)0.0008 (2)0.0014 (2)
Ti10.0043 (4)0.0054 (4)0.0047 (4)0.0003 (3)0.0005 (3)0.0008 (3)
Ti20.0036 (4)0.0060 (4)0.0033 (4)0.0002 (3)0.0001 (3)0.0001 (3)
P10.0031 (6)0.0065 (6)0.0040 (5)0.0000 (4)0.0009 (4)0.0009 (5)
P20.0058 (5)0.0058 (6)0.0029 (5)0.0001 (4)0.0002 (4)0.0002 (4)
O10.0065 (18)0.0107 (19)0.0037 (16)0.0021 (13)0.0021 (12)0.0045 (14)
O20.0080 (19)0.0101 (18)0.0118 (18)0.0004 (15)0.0009 (13)0.0029 (15)
O30.0082 (19)0.0068 (17)0.0092 (19)0.0002 (12)0.0006 (13)0.0023 (13)
O40.0049 (16)0.0085 (16)0.0083 (17)0.0014 (12)0.0022 (14)0.0001 (13)
O110.0088 (19)0.0101 (17)0.0041 (16)0.0009 (14)0.0028 (12)0.0020 (13)
O120.007 (2)0.0090 (16)0.0124 (17)0.0018 (14)0.0031 (13)0.0002 (15)
O50.011 (2)0.008 (2)0.006 (2)0.0007 (12)0.0008 (12)0.0010 (13)
O60.012 (2)0.0042 (16)0.014 (2)0.0006 (11)0.0053 (14)0.0001 (15)
O70.0101 (18)0.0122 (17)0.0043 (15)0.0019 (14)0.0006 (12)0.0040 (15)
O80.0078 (17)0.0118 (18)0.0092 (17)0.0023 (13)0.0062 (14)0.0009 (15)
Geometric parameters (Å, º) top
Rb1—O13.037 (4)Ti1—O21.957 (4)
Rb1—O22.740 (4)Ti1—O111.964 (4)
Rb1—O32.773 (4)Ti1—O121.723 (4)
Rb1—O113.171 (4)Ti1—O52.083 (4)
Rb1—O122.790 (4)Ti1—O62.027 (4)
Rb1—O52.998 (4)Ti2—O32.059 (4)
Rb1—O63.400 (4)Ti2—O4i2.015 (4)
Rb1—O73.220 (4)Ti2—O111.740 (4)
Rb1—O82.841 (5)Ti2—O122.087 (4)
Rb2—O12.749 (4)Ti2—O71.962 (4)
Rb2—O23.107 (4)Ti2—O82.000 (10)
Rb2—O33.120 (4)P1—O11.526 (4)
Rb2—O4i3.043 (4)P1—O21.550 (4)
Rb2—O112.791 (4)P1—O31.545 (4)
Rb2—O123.110 (4)P1—O41.542 (4)
Rb2—O52.863 (4)P2—O51.539 (4)
Rb2—O73.000 (4)P2—O61.531 (4)
Rb2—O83.127 (8)P2—O71.548 (4)
Ti1—O12.127 (4)P2—O81.535 (9)
O1—Rb1—O251.06 (10)O3—Rb2—O1253.30 (10)
O1—Rb1—O1151.35 (10)O3—Rb2—O7100.91 (10)
O1—Rb1—O887.00 (18)O3—Rb2—O854.5 (2)
O1—Rb1—O3119.66 (11)O3—Rb2—O4i125.35 (10)
O1—Rb1—O12150.85 (11)O3—Rb2—O1103.94 (10)
O1—Rb1—O554.06 (11)O12—Rb2—O784.63 (10)
O1—Rb1—O799.79 (10)O12—Rb2—O851.59 (12)
O1—Rb1—O688.16 (10)O12—Rb2—O4i97.67 (10)
O2—Rb1—O1183.53 (11)O12—Rb2—O1144.71 (11)
O2—Rb1—O874.95 (13)O7—Rb2—O847.30 (19)
O2—Rb1—O3137.70 (12)O7—Rb2—O4i123.59 (11)
O2—Rb1—O12150.98 (12)O7—Rb2—O172.99 (12)
O2—Rb1—O5104.65 (11)O8—Rb2—O4i144.62 (11)
O2—Rb1—O7150.70 (11)O8—Rb2—O193.76 (12)
O2—Rb1—O653.56 (11)O4i—Rb2—O1117.37 (11)
O11—Rb1—O853.8 (2)O1—Ti1—O1182.21 (15)
O11—Rb1—O3125.21 (11)O1—Ti1—O287.73 (16)
O11—Rb1—O12102.83 (11)O1—Ti1—O686.21 (17)
O11—Rb1—O555.59 (10)O1—Ti1—O12172.91 (18)
O11—Rb1—O773.28 (10)O1—Ti1—O581.31 (16)
O11—Rb1—O6135.46 (10)O11—Ti1—O2169.92 (17)
O8—Rb1—O3145.93 (12)O11—Ti1—O689.51 (17)
O8—Rb1—O1285.97 (13)O11—Ti1—O1295.20 (17)
O8—Rb1—O5109.0 (2)O11—Ti1—O590.72 (16)
O8—Rb1—O7103.91 (18)O2—Ti1—O690.45 (17)
O8—Rb1—O6115.30 (19)O2—Ti1—O1294.71 (18)
O3—Rb1—O1260.31 (11)O2—Ti1—O587.13 (16)
O3—Rb1—O576.33 (12)O6—Ti1—O12100.40 (18)
O3—Rb1—O754.03 (11)O6—Ti1—O5167.37 (17)
O3—Rb1—O688.25 (10)O12—Ti1—O592.15 (17)
O12—Rb1—O5102.13 (11)O3—Ti2—O1191.74 (17)
O12—Rb1—O754.92 (10)O3—Ti2—O1284.74 (15)
O12—Rb1—O6120.32 (11)O3—Ti2—O889.57 (17)
O5—Rb1—O747.23 (10)O3—Ti2—O786.29 (17)
O5—Rb1—O6118.97 (10)O3—Ti2—O4i173.61 (16)
O7—Rb1—O6140.38 (10)O11—Ti2—O12175.38 (17)
O11—Rb2—O5145.27 (12)O11—Ti2—O893.8 (3)
O11—Rb2—O2150.82 (11)O11—Ti2—O795.42 (17)
O11—Rb2—O3107.15 (10)O11—Ti2—O4i94.63 (17)
O11—Rb2—O1254.75 (10)O12—Ti2—O883.2 (3)
O11—Rb2—O782.30 (11)O12—Ti2—O787.34 (15)
O11—Rb2—O888.73 (12)O12—Ti2—O4i88.92 (16)
O11—Rb2—O4i56.42 (11)O8—Ti2—O7170.0 (3)
O11—Rb2—O1143.27 (11)O8—Ti2—O4i90.45 (17)
O5—Rb2—O255.45 (12)O7—Ti2—O4i92.65 (17)
O5—Rb2—O381.42 (11)O1—P1—O2109.0 (2)
O5—Rb2—O12129.38 (11)O1—P1—O3111.1 (2)
O5—Rb2—O7130.09 (12)O1—P1—O4110.6 (2)
O5—Rb2—O8121.38 (15)O2—P1—O3105.6 (2)
O5—Rb2—O4i90.76 (11)O2—P1—O4110.0 (2)
O5—Rb2—O158.47 (12)O3—P1—O4110.4 (2)
O2—Rb2—O346.64 (10)O5—P2—O6111.6 (2)
O2—Rb2—O1296.63 (11)O5—P2—O7108.1 (2)
O2—Rb2—O790.09 (11)O5—P2—O8110.4 (2)
O2—Rb2—O866.02 (15)O6—P2—O7110.3 (2)
O2—Rb2—O4i144.40 (11)O6—P2—O8110.3 (3)
O2—Rb2—O157.47 (10)O7—P2—O8105.9 (3)
Symmetry code: (i) x+1/2, y+1/2, z.
(GeRTP1) top
Crystal data top
Ge0.121O10P2Rb2Ti1.879F(000) = 916.8
Mr = 491.62Dx = 3.714 Mg m3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: p 2c -2nCell parameters from 23 reflections
a = 12.9386 (18) Åθ = 19.6–27.3°
b = 6.5085 (8) ŵ = 13.53 mm1
c = 10.4408 (10) ÅT = 293 K
V = 879.23 (18) Å3Rectangular, colourless
Z = 40.60 × 0.10 × 0.04 mm
Data collection top
Siemens SMART CCD
diffractometer
2513 independent reflections
Radiation source: normal-focus sealed tube2513 reflections with F > 0σ(F)
Graphite monochromatorRint = 0.031
ω scansθmax = 29.8°, θmin = 3.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
h = 1818
Tmin = 0.207, Tmax = 0.578k = 99
12286 measured reflectionsl = 1414
Refinement top
Refinement on F w = 1/[σ2(F) + 0.0015(F)2]
Least-squares matrix: full(Δ/σ)max = 0.00039
R[F2 > 2σ(F2)] = 0.021Δρmax = 0.61 e Å3
wR(F2) = 0.032Δρmin = 0.60 e Å3
S = 1.05Extinction correction: Isotropic Gaussian, Zachariasen, 1967; Larson (1970), Eq22 p292 "Cryst. Comp." Munksgaard 1970
2513 reflectionsExtinction coefficient: 4E2 (1)
158 parametersAbsolute structure: Flack (1983) parameter refined
0 restraintsAbsolute structure parameter: 0.429 (8)
21 constraints
Crystal data top
Ge0.121O10P2Rb2Ti1.879V = 879.23 (18) Å3
Mr = 491.62Z = 4
Orthorhombic, Pna21Mo Kα radiation
a = 12.9386 (18) ŵ = 13.53 mm1
b = 6.5085 (8) ÅT = 293 K
c = 10.4408 (10) Å0.60 × 0.10 × 0.04 mm
Data collection top
Siemens SMART CCD
diffractometer
2513 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
2513 reflections with F > 0σ(F)
Tmin = 0.207, Tmax = 0.578Rint = 0.031
12286 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0210 restraints
wR(F2) = 0.032Δρmax = 0.61 e Å3
S = 1.05Δρmin = 0.60 e Å3
2513 reflectionsAbsolute structure: Flack (1983) parameter refined
158 parametersAbsolute structure parameter: 0.429 (8)
Special details top

Refinement. The following constraints were used during the refinement:

H-atom parameters constrained pop(Rb1b)=1.0–1.0*pop(Rb1a) H-atom parameters constrained U11(Rb1b)=0.0 + 1.0*U11(Rb1a) H-atom parameters constrained U22(Rb1b)=0.0 + 1.0*U22(Rb1a) H-atom parameters constrained U33(Rb1b)=0.0 + 1.0*U33(Rb1a) H-atom parameters constrained U12(Rb1b)=0.0 + 1.0*U12(Rb1a) H-atom parameters constrained U13(Rb1b)=0.0 + 1.0*U13(Rb1a) H-atom parameters constrained U23(Rb1b)=0.0 + 1.0*U23(Rb1a) H-atom parameters constrained pop(Rb2b)=1.0–1.0*pop(Rb2a) H-atom parameters constrained U11(Rb2b)=0.0 + 1.0*U11(Rb2a) H-atom parameters constrained U22(Rb2b)=0.0 + 1.0*U22(Rb2a) H-atom parameters constrained U33(Rb2b)=0.0 + 1.0*U33(Rb2a) H-atom parameters constrained U12(Rb2b)=0.0 + 1.0*U12(Rb2a) H-atom parameters constrained U13(Rb2b)=0.0 + 1.0*U13(Rb2a) H-atom parameters constrained U23(Rb2b)=0.0 + 1.0*U23(Rb2a) H-atom parameters constrained pop(Ge2)=1.0–1.0*pop(Ti2) H-atom parameters constrained U11(Ge2)=0.0 + 1.0*U11(Ti2) H-atom parameters constrained U22(Ge2)=0.0 + 1.0*U22(Ti2) H-atom parameters constrained U33(Ge2)=0.0 + 1.0*U33(Ti2) H-atom parameters constrained U12(Ge2)=0.0 + 1.0*U12(Ti2) H-atom parameters constrained U13(Ge2)=0.0 + 1.0*U13(Ti2) H-atom parameters constrained U23(Ge2)=0.0 + 1.0*U23(Ti2)

No restraints used.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Rb1a0.61417 (4)0.78418 (8)0.6950 (2)0.0186 (4)0.927 (5)
Rb1b0.6075 (7)0.7936 (12)0.6430 (17)0.0186 (4)0.073 (5)
Rb2a0.89399 (4)0.69389 (9)0.94809 (19)0.0164 (5)0.945 (11)
Rb2b0.8911 (9)0.699 (2)0.905 (4)0.0164 (5)0.055 (11)
Ti10.62797 (5)0.49940 (9)1.0236 (3)0.0058 (3)
Ti20.7536 (4)0.2656 (7)0.7738 (6)0.0049 (9)0.879 (6)
Ge20.7464 (19)0.245 (3)0.766 (2)0.0049 (9)0.121 (6)
P10.50047 (7)0.33234 (15)0.7685 (3)0.0060 (4)
P20.82052 (7)0.50249 (13)0.5159 (3)0.0059 (4)
O10.5140 (3)0.4766 (5)0.8819 (4)0.0118 (14)
O20.4859 (3)0.4611 (5)0.6455 (4)0.0108 (14)
O30.5981 (2)0.2009 (5)0.7464 (4)0.0106 (14)
O40.4049 (2)0.1936 (5)0.7895 (4)0.0104 (14)
O110.7219 (2)0.4582 (5)0.8860 (4)0.0109 (13)
O120.7771 (2)0.0490 (5)0.6396 (4)0.0102 (13)
O50.8869 (2)0.3134 (5)0.4837 (4)0.0111 (14)
O60.8873 (2)0.6918 (5)0.5457 (4)0.0117 (14)
O70.7485 (3)0.5443 (5)0.4004 (4)0.0118 (13)
O80.7480 (3)0.4570 (5)0.630 (5)0.0117 (14)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb1a0.0199 (2)0.0093 (2)0.0266 (7)0.00422 (14)0.0062 (2)0.0018 (2)
Rb1b0.0199 (2)0.0093 (2)0.0266 (7)0.00422 (14)0.0062 (2)0.0018 (2)
Rb2a0.0119 (2)0.0152 (2)0.0219 (9)0.00397 (13)0.0011 (2)0.0019 (2)
Rb2b0.0119 (2)0.0152 (2)0.0219 (9)0.00397 (13)0.0011 (2)0.0019 (2)
Ti10.0060 (3)0.0048 (3)0.0065 (3)0.0007 (2)0.0012 (3)0.0007 (2)
Ti20.0052 (9)0.0045 (11)0.0050 (8)0.0022 (6)0.0006 (6)0.0006 (7)
Ge20.0052 (9)0.0045 (11)0.0050 (8)0.0022 (6)0.0006 (6)0.0006 (7)
P10.0051 (4)0.0057 (4)0.0073 (4)0.0007 (3)0.0011 (3)0.0007 (4)
P20.0067 (4)0.0049 (4)0.0062 (4)0.0001 (3)0.0001 (3)0.0007 (3)
O10.0098 (14)0.0115 (15)0.0142 (14)0.0023 (11)0.0038 (11)0.0053 (12)
O20.0092 (14)0.0101 (14)0.0132 (13)0.0037 (11)0.0030 (10)0.0055 (11)
O30.0078 (14)0.0090 (14)0.0152 (14)0.0017 (9)0.0008 (10)0.0047 (11)
O40.0068 (13)0.0091 (14)0.0153 (15)0.0022 (9)0.0002 (10)0.0015 (11)
O110.0092 (13)0.0113 (13)0.0122 (13)0.0017 (11)0.0012 (10)0.0035 (11)
O120.0103 (14)0.0093 (13)0.0109 (12)0.0014 (11)0.0035 (10)0.0008 (11)
O50.0128 (14)0.0070 (14)0.0134 (14)0.0011 (10)0.0030 (9)0.0028 (11)
O60.0157 (15)0.0073 (14)0.0122 (15)0.0003 (9)0.0034 (10)0.0009 (10)
O70.0151 (14)0.0100 (13)0.0103 (12)0.0029 (12)0.0030 (10)0.0032 (11)
O80.0110 (14)0.0113 (14)0.0127 (14)0.0041 (10)0.0049 (11)0.0026 (11)
Geometric parameters (Å, º) top
Rb1a—O13.082 (4)Rb2b—O72.882 (13)
Rb1a—O22.728 (4)Ti1—O12.094 (4)
Rb1a—O32.773 (3)Ti1—O21.964 (4)
Rb1a—O113.228 (4)Ti1—O111.902 (4)
Rb1a—O122.783 (3)Ti1—O121.755 (4)
Rb1a—O53.021 (5)Ti1—O52.095 (4)
Rb1a—O63.327 (4)Ti1—O62.025 (3)
Rb1a—O73.260 (4)Ti2—O32.077 (6)
Rb1a—O82.828 (13)Ti2—O4i1.982 (6)
Rb1a—Rb1b0.553 (17)Ti2—O111.764 (7)
Rb1b—O22.675 (9)Ti2—O122.011 (7)
Rb1b—O32.865 (10)Ti2—O71.956 (7)
Rb1b—O122.753 (9)Ti2—O81.95 (4)
Rb1b—O63.026 (10)Ti2—Ge20.18 (2)
Rb1b—O82.850 (9)Ge2—O31.95 (2)
Rb2a—O12.737 (4)Ge2—O4i2.10 (2)
Rb2a—O23.113 (4)Ge2—O111.89 (2)
Rb2a—O33.116 (5)Ge2—O121.88 (2)
Rb2a—O4i3.020 (4)Ge2—O71.92 (2)
Rb2a—O112.780 (3)Ge2—O81.98 (4)
Rb2a—O123.128 (4)P1—O11.521 (5)
Rb2a—O52.859 (3)P1—O21.545 (5)
Rb2a—O72.974 (4)P1—O31.542 (3)
Rb2a—O83.15 (3)P1—O41.546 (3)
Rb2a—Rb2b0.45 (4)P2—O51.538 (3)
Rb2b—O12.652 (13)P2—O61.536 (3)
Rb2b—O4i2.83 (2)P2—O71.548 (5)
Rb2b—O112.701 (13)P2—O81.54 (4)
Rb2b—O52.988 (16)
O1—Rb1a—O250.46 (11)O12—Rb2a—O1143.05 (11)
O1—Rb1a—O1150.47 (9)O7—Rb2a—O847.3 (7)
O1—Rb1a—O885.4 (7)O7—Rb2a—O4i125.28 (11)
O1—Rb1a—O3118.76 (13)O7—Rb2a—O173.05 (10)
O1—Rb1a—O12148.47 (13)O8—Rb2a—O4i144.30 (13)
O1—Rb1a—O553.62 (10)O8—Rb2a—O193.3 (2)
O1—Rb1a—O798.62 (12)O4i—Rb2a—O1119.31 (12)
O1—Rb1a—O687.48 (10)O11—Rb2b—O5141.6 (6)
O2—Rb1a—O1182.72 (10)O11—Rb2b—O786.8 (4)
O2—Rb1a—O875.32 (17)O11—Rb2b—O4i59.7 (4)
O2—Rb1a—O3138.15 (10)O11—Rb2b—O1160.2 (9)
O2—Rb1a—O12153.97 (14)O5—Rb2b—O7129.0 (6)
O2—Rb1a—O5103.57 (12)O5—Rb2b—O4i91.8 (4)
O2—Rb1a—O7148.93 (14)O5—Rb2b—O158.1 (3)
O2—Rb1a—O653.90 (10)O7—Rb2b—O4i137.3 (9)
O11—Rb1a—O852.4 (10)O7—Rb2b—O175.8 (3)
O11—Rb1a—O3123.76 (13)O4i—Rb2b—O1129.9 (10)
O11—Rb1a—O12102.02 (10)O1—Ti1—O1184.62 (19)
O11—Rb1a—O555.03 (10)O1—Ti1—O286.49 (15)
O11—Rb1a—O772.50 (10)O1—Ti1—O686.66 (15)
O11—Rb1a—O6134.53 (8)O1—Ti1—O12173.45 (15)
O8—Rb1a—O3146.03 (10)O1—Ti1—O582.17 (16)
O8—Rb1a—O1287.3 (2)O11—Ti1—O2171.1 (2)
O8—Rb1a—O5106.9 (10)O11—Ti1—O690.51 (16)
O8—Rb1a—O7102.5 (6)O11—Ti1—O1295.71 (16)
O8—Rb1a—O6117.6 (7)O11—Ti1—O592.62 (17)
O3—Rb1a—O1259.44 (10)O2—Ti1—O689.00 (16)
O3—Rb1a—O575.22 (12)O2—Ti1—O1293.1 (2)
O3—Rb1a—O753.53 (10)O2—Ti1—O586.12 (15)
O3—Rb1a—O688.76 (9)O6—Ti1—O1299.87 (17)
O12—Rb1a—O599.90 (11)O6—Ti1—O5168.06 (15)
O12—Rb1a—O753.30 (11)O12—Ti1—O591.28 (15)
O12—Rb1a—O6122.80 (11)O3—Ti2—O1190.6 (3)
O5—Rb1a—O746.61 (9)O3—Ti2—O1284.7 (2)
O5—Rb1a—O6117.41 (10)O3—Ti2—O889.2 (3)
O7—Rb1a—O6139.89 (9)O3—Ti2—O786.0 (2)
O2—Rb1b—O875.8 (2)O3—Ti2—O4i174.8 (3)
O2—Rb1b—O3136.0 (5)O11—Ti2—O12174.9 (4)
O2—Rb1b—O12163.2 (4)O11—Ti2—O892.8 (10)
O2—Rb1b—O658.3 (2)O11—Ti2—O794.1 (3)
O8—Rb1b—O3139.2 (7)O11—Ti2—O4i94.6 (3)
O8—Rb1b—O1287.4 (3)O12—Ti2—O885.2 (10)
O8—Rb1b—O6127.5 (6)O12—Ti2—O787.5 (2)
O3—Rb1b—O1258.7 (2)O12—Ti2—O4i90.2 (3)
O3—Rb1b—O693.3 (3)O8—Ti2—O7171.6 (9)
O12—Rb1b—O6136.6 (4)O8—Ti2—O4i90.9 (3)
O11—Rb2a—O5144.59 (10)O7—Ti2—O4i93.2 (3)
O11—Rb2a—O2149.60 (12)O3—Ge2—O1190.8 (10)
O11—Rb2a—O3105.53 (11)O3—Ge2—O1291.9 (10)
O11—Rb2a—O1254.28 (10)O3—Ge2—O892.1 (10)
O11—Rb2a—O783.55 (10)O3—Ge2—O790.7 (10)
O11—Rb2a—O888.5 (3)O3—Ge2—O4i177.5 (13)
O11—Rb2a—O4i56.56 (9)O11—Ge2—O12175.3 (14)
O11—Rb2a—O1145.88 (13)O11—Ge2—O888.1 (14)
O5—Rb2a—O255.13 (10)O11—Ge2—O791.3 (11)
O5—Rb2a—O380.65 (11)O11—Ge2—O4i87.0 (9)
O5—Rb2a—O12127.83 (12)O12—Ge2—O888.0 (14)
O5—Rb2a—O7130.46 (10)O12—Ge2—O792.5 (10)
O5—Rb2a—O8120.6 (5)O12—Ge2—O4i90.2 (10)
O5—Rb2a—O4i90.63 (10)O8—Ge2—O7177.2 (15)
O5—Rb2a—O158.89 (10)O8—Ge2—O4i86.6 (9)
O2—Rb2a—O346.65 (9)O7—Ge2—O4i90.6 (10)
O2—Rb2a—O1295.65 (11)O1—P1—O2109.0 (2)
O2—Rb2a—O789.53 (10)O1—P1—O3111.4 (2)
O2—Rb2a—O865.7 (4)O1—P1—O4110.0 (3)
O2—Rb2a—O4i143.73 (9)O2—P1—O3106.0 (3)
O2—Rb2a—O156.35 (11)O2—P1—O4109.7 (2)
O3—Rb2a—O1252.35 (9)O3—P1—O4110.61 (17)
O3—Rb2a—O7100.16 (10)O5—P2—O6111.83 (17)
O3—Rb2a—O853.8 (7)O5—P2—O7107.8 (3)
O3—Rb2a—O4i123.95 (10)O5—P2—O8110.8 (2)
O3—Rb2a—O1102.83 (11)O6—P2—O7110.8 (2)
O12—Rb2a—O784.24 (10)O6—P2—O8109.9 (10)
O12—Rb2a—O850.6 (3)O7—P2—O8105.5 (11)
O12—Rb2a—O4i97.56 (9)
Symmetry code: (i) x+1/2, y+1/2, z.
(GeRTP2) top
Crystal data top
Ge0.35O10P2Rb2Ti1.65F(000) = 925.6
Mr = 497.28Dx = 3.785 Mg m3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: p 2c -2nCell parameters from 19 reflections
a = 12.9179 (12) Åθ = 16.3–29.6°
b = 6.5189 (8) ŵ = 14.21 mm1
c = 10.3633 (14) ÅT = 293 K
V = 872.70 (18) Å3Rectangular, colourless
Z = 40.10 × 0.05 × 0.04 mm
Data collection top
Siemens SMART CCD
diffractometer
2497 independent reflections
Radiation source: normal-focus sealed tube2497 reflections with F > 0σ(F)
Graphite monochromatorRint = 0.039
ω scansθmax = 29.8°, θmin = 3.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
h = 1818
Tmin = 0.421, Tmax = 0.564k = 99
12604 measured reflectionsl = 1414
Refinement top
Refinement on F34 constraints
Least-squares matrix: full w = 1/[σ2(F) + 0.0020(F)2]
R[F2 > 2σ(F2)] = 0.025(Δ/σ)max = 0.001
wR(F2) = 0.039Δρmax = 0.73 e Å3
S = 1.04Δρmin = 0.91 e Å3
2497 reflectionsAbsolute structure: Flack (1983) parameter refined
156 parametersAbsolute structure parameter: 0.487 (11)
0 restraints
Crystal data top
Ge0.35O10P2Rb2Ti1.65V = 872.70 (18) Å3
Mr = 497.28Z = 4
Orthorhombic, Pna21Mo Kα radiation
a = 12.9179 (12) ŵ = 14.21 mm1
b = 6.5189 (8) ÅT = 293 K
c = 10.3633 (14) Å0.10 × 0.05 × 0.04 mm
Data collection top
Siemens SMART CCD
diffractometer
2497 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
2497 reflections with F > 0σ(F)
Tmin = 0.421, Tmax = 0.564Rint = 0.039
12604 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0250 restraints
wR(F2) = 0.039Δρmax = 0.73 e Å3
S = 1.04Δρmin = 0.91 e Å3
2497 reflectionsAbsolute structure: Flack (1983) parameter refined
156 parametersAbsolute structure parameter: 0.487 (11)
Special details top

Refinement. The following constraints were used during the refinement:

H-atom parameters constrained pop(Rb1b)=1.0–1.0*pop(Rb1a) H-atom parameters constrained U11(Rb1b)=0.0 + 1.0*U11(Rb1a) H-atom parameters constrained U22(Rb1b)=0.0 + 1.0*U22(Rb1a) H-atom parameters constrained U33(Rb1b)=0.0 + 1.0*U33(Rb1a) H-atom parameters constrained U12(Rb1b)=0.0 + 1.0*U12(Rb1a) H-atom parameters constrained U13(Rb1b)=0.0 + 1.0*U13(Rb1a) H-atom parameters constrained U23(Rb1b)=0.0 + 1.0*U23(Rb1a) H-atom parameters constrained pop(Rb2b)=1.0–1.0*pop(Rb2a) H-atom parameters constrained U11(Rb2b)=0.0 + 1.0*U11(Rb2a) H-atom parameters constrained U22(Rb2b)=0.0 + 1.0*U22(Rb2a) H-atom parameters constrained U33(Rb2b)=0.0 + 1.0*U33(Rb2a) H-atom parameters constrained U12(Rb2b)=0.0 + 1.0*U12(Rb2a) H-atom parameters constrained U13(Rb2b)=0.0 + 1.0*U13(Rb2a) H-atom parameters constrained U23(Rb2b)=0.0 + 1.0*U23(Rb2a) H-atom parameters constrained pop(Ge1)=1.0–1.0*pop(Ti1) H-atom parameters constrained x(Ge1)=0.0 + 1.0*x(Ti1) H-atom parameters constrained y(Ge1)=0.0 + 1.0*y(Ti1) H-atom parameters constrained z(Ge1)=0.0 + 1.0*z(Ti1) H-atom parameters constrained U11(Ge1)=0.0 + 1.0*U11(Ti1) H-atom parameters constrained U22(Ge1)=0.0 + 1.0*U22(Ti1) H-atom parameters constrained U33(Ge1)=0.0 + 1.0*U33(Ti1) H-atom parameters constrained U12(Ge1)=0.0 + 1.0*U12(Ti1) H-atom parameters constrained U13(Ge1)=0.0 + 1.0*U13(Ti1) H-atom parameters constrained U23(Ge1)=0.0 + 1.0*U23(Ti1) H-atom parameters constrained pop(Ge2)=1.0–1.0*pop(Ti2) H-atom parameters constrained x(Ge2)=0.0 + 1.0*x(Ti2) H-atom parameters constrained y(Ge2)=0.0 + 1.0*y(Ti2) H-atom parameters constrained z(Ge2)=0.0 + 1.0*z(Ti2) H-atom parameters constrained U11(Ge2)=0.0 + 1.0*U11(Ti2) H-atom parameters constrained U22(Ge2)=0.0 + 1.0*U22(Ti2) H-atom parameters constrained U33(Ge2)=0.0 + 1.0*U33(Ti2) H-atom parameters constrained U12(Ge2)=0.0 + 1.0*U12(Ti2) H-atom parameters constrained U13(Ge2)=0.0 + 1.0*U13(Ti2) H-atom parameters constrained U23(Ge2)=0.0 + 1.0*U23(Ti2)

No restraints used.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Rb1a0.61351 (7)0.78509 (13)0.6842 (3)0.0204 (6)0.883 (8)
Rb1b0.6079 (7)0.7937 (13)0.6302 (19)0.0204 (6)0.117 (8)
Rb2a0.89346 (7)0.69529 (14)0.9373 (3)0.0183 (6)0.939 (6)
Rb2b0.8892 (11)0.705 (2)0.880 (3)0.0183 (6)0.061 (6)
Ti10.62817 (7)0.49922 (13)1.0151 (2)0.0078 (5)0.875 (10)
Ge10.62817 (7)0.49922 (13)1.0151 (2)0.0078 (5)0.125 (10)
Ti20.75268 (6)0.25812 (12)0.7649 (3)0.0078 (4)0.775 (8)
Ge20.75268 (6)0.25812 (12)0.7649 (3)0.0078 (4)0.225 (8)
P10.50068 (10)0.3321 (2)0.7620 (4)0.0070 (6)
P20.82103 (11)0.5026 (2)0.5103 (3)0.0064 (6)
O10.5150 (5)0.4773 (10)0.8759 (7)0.015 (3)
O20.4860 (5)0.4610 (10)0.6390 (7)0.013 (3)
O30.5979 (3)0.1994 (7)0.7407 (7)0.011 (2)
O40.4050 (3)0.1940 (7)0.7845 (5)0.011 (2)
O110.7216 (4)0.4563 (10)0.8817 (6)0.011 (2)
O120.7765 (5)0.0514 (9)0.6353 (6)0.012 (2)
O50.8872 (3)0.3131 (8)0.4784 (6)0.013 (2)
O60.8875 (4)0.6919 (9)0.5404 (7)0.012 (3)
O70.7479 (5)0.5444 (11)0.3955 (6)0.014 (2)
O80.7487 (5)0.4587 (10)0.6258 (6)0.013 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb1a0.0195 (4)0.0107 (3)0.0310 (12)0.0042 (2)0.0076 (4)0.0028 (4)
Rb1b0.0195 (4)0.0107 (3)0.0310 (12)0.0042 (2)0.0076 (4)0.0028 (4)
Rb2a0.0120 (3)0.0157 (4)0.0271 (9)0.0043 (2)0.0016 (4)0.0023 (4)
Rb2b0.0120 (3)0.0157 (4)0.0271 (9)0.0043 (2)0.0016 (4)0.0023 (4)
Ti10.0073 (5)0.0073 (5)0.0089 (5)0.0002 (3)0.0007 (4)0.0002 (3)
Ge10.0073 (5)0.0073 (5)0.0089 (5)0.0002 (3)0.0007 (4)0.0002 (3)
Ti20.0059 (4)0.0099 (4)0.0075 (6)0.0001 (3)0.0004 (4)0.0026 (4)
Ge20.0059 (4)0.0099 (4)0.0075 (6)0.0001 (3)0.0004 (4)0.0026 (4)
P10.0057 (5)0.0063 (5)0.0089 (7)0.0006 (4)0.0005 (6)0.0003 (8)
P20.0060 (6)0.0064 (6)0.0069 (6)0.0001 (5)0.0004 (6)0.0005 (5)
O10.010 (3)0.008 (2)0.025 (3)0.0028 (19)0.002 (2)0.006 (2)
O20.009 (3)0.015 (3)0.015 (2)0.003 (2)0.004 (2)0.006 (2)
O30.0059 (17)0.0100 (19)0.016 (3)0.0027 (11)0.001 (2)0.005 (2)
O40.007 (2)0.013 (2)0.012 (3)0.0011 (13)0.0012 (15)0.0007 (16)
O110.008 (2)0.014 (2)0.012 (2)0.004 (2)0.0017 (18)0.004 (2)
O120.013 (3)0.009 (2)0.014 (2)0.000 (2)0.002 (2)0.0022 (18)
O50.011 (2)0.008 (2)0.021 (3)0.0009 (16)0.0020 (17)0.0015 (19)
O60.016 (3)0.010 (2)0.011 (3)0.0013 (18)0.0041 (19)0.0001 (19)
O70.014 (3)0.016 (2)0.012 (2)0.004 (2)0.0050 (19)0.004 (2)
O80.015 (3)0.010 (2)0.015 (2)0.007 (2)0.006 (2)0.004 (2)
Geometric parameters (Å, º) top
Rb1a—O13.098 (7)Ti1—O21.973 (7)
Rb1a—O22.720 (7)Ti1—O111.856 (6)
Rb1a—O32.771 (5)Ti1—O121.785 (6)
Rb1a—O113.277 (7)Ti1—O52.090 (5)
Rb1a—O122.776 (6)Ti1—O62.030 (6)
Rb1a—O53.055 (7)Ge1—O12.058 (7)
Rb1a—O63.281 (6)Ge1—O21.973 (7)
Rb1a—O73.295 (7)Ge1—O111.856 (6)
Rb1a—O82.818 (6)Ge1—O121.785 (6)
Rb1a—Rb1b0.57 (2)Ge1—O52.090 (5)
Rb1b—O22.682 (11)Ge1—O62.030 (6)
Rb1b—O32.886 (12)Ti2—O32.051 (4)
Rb1b—O122.751 (10)Ti2—O4i2.003 (4)
Rb1b—O62.996 (12)Ti2—O111.816 (7)
Rb1b—O82.842 (11)Ti2—O121.927 (7)
Rb2a—O12.725 (6)Ti2—O71.942 (7)
Rb2a—O23.130 (7)Ti2—O81.947 (7)
Rb2a—O33.147 (8)Ge2—O32.051 (4)
Rb2a—O4i2.995 (5)Ge2—O4i2.003 (4)
Rb2a—O112.773 (6)Ge2—O111.816 (7)
Rb2a—O123.149 (6)Ge2—O121.927 (7)
Rb2a—O52.866 (5)Ge2—O71.942 (7)
Rb2a—O72.950 (7)Ge2—O81.947 (7)
Rb2a—O83.184 (7)P1—O11.525 (8)
Rb2a—Rb2b0.60 (3)P1—O21.538 (8)
Rb2b—O12.632 (16)P1—O31.540 (4)
Rb2b—O4i2.792 (19)P1—O41.546 (5)
Rb2b—O112.706 (16)P2—O51.538 (5)
Rb2b—O53.067 (18)P2—O61.536 (6)
Rb2b—O72.837 (16)P2—O71.544 (7)
Ti1—O12.058 (7)P2—O81.545 (7)
O1—Rb1a—O250.1 (2)O11—Rb2b—O5136.7 (8)
O1—Rb1a—O1149.49 (16)O11—Rb2b—O788.1 (4)
O1—Rb1a—O884.44 (18)O11—Rb2b—O4i60.1 (4)
O1—Rb1a—O3117.8 (2)O11—Rb2b—O1165.0 (6)
O1—Rb1a—O12146.5 (2)O5—Rb2b—O7126.8 (7)
O1—Rb1a—O552.92 (17)O5—Rb2b—O4i90.7 (4)
O1—Rb1a—O797.4 (2)O5—Rb2b—O156.9 (3)
O1—Rb1a—O687.45 (16)O7—Rb2b—O4i142.4 (8)
O2—Rb1a—O1181.80 (18)O7—Rb2b—O176.9 (4)
O2—Rb1a—O875.63 (19)O4i—Rb2b—O1133.0 (8)
O2—Rb1a—O3138.54 (16)O1—Ti1—O1186.0 (3)
O2—Rb1a—O12156.1 (2)O1—Ti1—O286.2 (3)
O2—Rb1a—O5102.49 (19)O1—Ti1—O687.2 (3)
O2—Rb1a—O7147.3 (2)O1—Ti1—O12173.0 (3)
O2—Rb1a—O654.44 (17)O1—Ti1—O582.7 (2)
O11—Rb1a—O851.40 (17)O11—Ti1—O2172.2 (3)
O11—Rb1a—O3122.4 (2)O11—Ti1—O690.7 (3)
O11—Rb1a—O12101.52 (17)O11—Ti1—O1295.8 (3)
O11—Rb1a—O554.30 (15)O11—Ti1—O594.2 (3)
O11—Rb1a—O771.87 (17)O2—Ti1—O688.3 (3)
O11—Rb1a—O6133.85 (15)O2—Ti1—O1292.0 (3)
O8—Rb1a—O3145.73 (16)O2—Ti1—O585.3 (2)
O8—Rb1a—O1287.88 (18)O6—Ti1—O1299.6 (3)
O8—Rb1a—O5105.13 (17)O6—Ti1—O5168.4 (2)
O8—Rb1a—O7101.14 (18)O12—Ti1—O590.3 (3)
O8—Rb1a—O6119.23 (19)O1—Ge1—O1186.0 (3)
O3—Rb1a—O1258.95 (15)O1—Ge1—O286.2 (3)
O3—Rb1a—O574.4 (2)O1—Ge1—O687.2 (3)
O3—Rb1a—O753.05 (17)O1—Ge1—O12173.0 (3)
O3—Rb1a—O689.24 (15)O1—Ge1—O582.7 (2)
O12—Rb1a—O598.44 (17)O11—Ge1—O2172.2 (3)
O12—Rb1a—O752.27 (17)O11—Ge1—O690.7 (3)
O12—Rb1a—O6124.31 (19)O11—Ge1—O1295.8 (3)
O5—Rb1a—O746.18 (15)O11—Ge1—O594.2 (3)
O5—Rb1a—O6116.62 (16)O2—Ge1—O688.3 (3)
O7—Rb1a—O6139.62 (16)O2—Ge1—O1292.0 (3)
O2—Rb1b—O875.8 (3)O2—Ge1—O585.3 (2)
O2—Rb1b—O3134.5 (5)O6—Ge1—O1299.6 (3)
O2—Rb1b—O12163.4 (4)O6—Ge1—O5168.4 (2)
O2—Rb1b—O658.5 (3)O12—Ge1—O590.3 (3)
O8—Rb1b—O3137.7 (5)O3—Ti2—O1189.9 (3)
O8—Rb1b—O1287.9 (3)O3—Ti2—O1286.6 (3)
O8—Rb1b—O6128.8 (4)O3—Ti2—O890.5 (3)
O3—Rb1b—O1257.9 (2)O3—Ti2—O787.0 (3)
O3—Rb1b—O693.0 (3)O3—Ti2—O4i177.8 (2)
O12—Rb1b—O6137.6 (4)O11—Ti2—O12176.0 (3)
O11—Rb2a—O5144.28 (17)O11—Ti2—O890.6 (3)
O11—Rb2a—O2148.0 (2)O11—Ti2—O792.6 (3)
O11—Rb2a—O3103.93 (16)O11—Ti2—O4i92.2 (2)
O11—Rb2a—O1253.81 (17)O12—Ti2—O887.6 (3)
O11—Rb2a—O784.69 (18)O12—Ti2—O789.1 (3)
O11—Rb2a—O888.20 (18)O12—Ti2—O4i91.3 (2)
O11—Rb2a—O4i56.91 (16)O8—Ti2—O7176.0 (3)
O11—Rb2a—O1148.5 (2)O8—Ti2—O4i89.8 (2)
O5—Rb2a—O254.50 (17)O7—Ti2—O4i92.6 (2)
O5—Rb2a—O379.42 (16)O3—Ge2—O1189.9 (3)
O5—Rb2a—O12125.9 (2)O3—Ge2—O1286.6 (3)
O5—Rb2a—O7130.43 (16)O3—Ge2—O890.5 (3)
O5—Rb2a—O8119.29 (18)O3—Ge2—O787.0 (3)
O5—Rb2a—O4i90.76 (14)O3—Ge2—O4i177.8 (2)
O5—Rb2a—O158.66 (17)O11—Ge2—O12176.0 (3)
O2—Rb2a—O346.37 (15)O11—Ge2—O890.6 (3)
O2—Rb2a—O1294.38 (18)O11—Ge2—O792.6 (3)
O2—Rb2a—O788.81 (18)O11—Ge2—O4i92.2 (2)
O2—Rb2a—O865.08 (17)O12—Ge2—O887.6 (3)
O2—Rb2a—O4i142.86 (15)O12—Ge2—O789.1 (3)
O2—Rb2a—O155.7 (2)O12—Ge2—O4i91.3 (2)
O3—Rb2a—O1251.38 (14)O8—Ge2—O7176.0 (3)
O3—Rb2a—O799.33 (16)O8—Ge2—O4i89.8 (2)
O3—Rb2a—O853.32 (14)O7—Ge2—O4i92.6 (2)
O3—Rb2a—O4i122.26 (14)O1—P1—O2108.5 (4)
O3—Rb2a—O1101.89 (18)O1—P1—O3111.1 (4)
O12—Rb2a—O783.91 (17)O1—P1—O4110.0 (4)
O12—Rb2a—O850.09 (16)O2—P1—O3106.8 (4)
O12—Rb2a—O4i97.30 (14)O2—P1—O4110.1 (3)
O12—Rb2a—O1141.9 (2)O3—P1—O4110.3 (2)
O7—Rb2a—O846.92 (17)O5—P2—O6112.2 (3)
O7—Rb2a—O4i127.38 (18)O5—P2—O7108.4 (4)
O7—Rb2a—O173.62 (18)O5—P2—O8110.7 (3)
O8—Rb2a—O4i144.11 (15)O6—P2—O7110.9 (4)
O8—Rb2a—O193.05 (18)O6—P2—O8109.3 (4)
O4i—Rb2a—O1120.8 (2)O7—P2—O8105.1 (3)
Symmetry code: (i) x+1/2, y+1/2, z.

Experimental details

(RTP)(GeRTP1)(GeRTP2)
Crystal data
Chemical formulaO10P2Rb2Ti2Ge0.121O10P2Rb2Ti1.879Ge0.35O10P2Rb2Ti1.65
Mr488.64491.62497.28
Crystal system, space groupOrthorhombic, Pna21Orthorhombic, Pna21Orthorhombic, Pna21
Temperature (K)293293293
a, b, c (Å)12.9625 (15), 6.5031 (3), 10.5615 (3)12.9386 (18), 6.5085 (8), 10.4408 (10)12.9179 (12), 6.5189 (8), 10.3633 (14)
α, β, γ (°)90, 90, 9090, 90, 9090, 90, 90
V3)890.30 (11)879.23 (18)872.70 (18)
Z444
Radiation typeMo KαMo KαMo Kα
µ (mm1)13.0613.5314.21
Crystal size (mm)0.14 × 0.12 × 0.080.60 × 0.10 × 0.040.10 × 0.05 × 0.04
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Siemens SMART CCD
diffractometer
Siemens SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2001)
Multi-scan
(SADABS; Sheldrick, 2001)
Multi-scan
(SADABS; Sheldrick, 2001)
Tmin, Tmax0.175, 0.3530.207, 0.5780.421, 0.564
No. of measured, independent and
observed [F > 0σ(F)] reflections
10947, 2054, 2054 12286, 2513, 2513 12604, 2497, 2497
Rint0.0520.0310.039
(sin θ/λ)max1)0.6500.7000.700
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.037, 1.13 0.021, 0.032, 1.05 0.025, 0.039, 1.04
No. of reflections205425132497
No. of parameters146158156
Δρmax, Δρmin (e Å3)1.11, 0.710.61, 0.600.73, 0.91
Absolute structureFlack (1983) parameter refinedFlack (1983) parameter refinedFlack (1983) parameter refined
Absolute structure parameter0.497 (9)0.429 (8)0.487 (11)

Computer programs: SMART (Siemens, 1995), CAD-4 Software (Enraf-Nonius, 1989), SAINT (Siemens, 1995) and SADABS (Sheldrick, 2001), Atomic parameters from Norberg et al. (2000), Xtal3.71 (Hall et al., 2000) program: CRYLSQ, ORTEPIII for Windows (Farrugia, 1997), Xtal3.71 (Hall et al., 2000) programs: BONDLA; ATABLE; CIFIO.

 

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