Chem. J. Chinese Universities ›› 2015, Vol. 36 ›› Issue (11): 2311.doi: 10.7503/cjcu20150685
• Inorganic Chemistry • Previous Articles Next Articles
WANG Ning, SUN Qiming, YAN Yan, LIU Jiancong, YU Jihong*(), XU Ruren
Received:
2015-09-06
Online:
2015-11-10
Published:
2015-10-26
Contact:
YU Jihong
E-mail:jihong@jlu.edu.cn
Supported by:
CLC Number:
TrendMD:
WANG Ning, SUN Qiming, YAN Yan, LIU Jiancong, YU Jihong, XU Ruren. Organotemplate-free Synthesis and Proton Conduction Properties of a Layered Aluminophosphate Na4[Al4P4O18]·H2O†[J]. Chem. J. Chinese Universities, 2015, 36(11): 2311.
Fig.1 PXRD patterns of as-synthesized compound 1 and calcined samples as compared with the simulated XRD patterns a. Simulated; b. as-synthesized; calcination temperature/℃:c. 100; d. 200; e. 300; f. 400; g. 500; h. 600.
Empirical formula | Al4P4O19H2Na4 | Calculated density/(Mg·m-3) | 2.694 |
---|---|---|---|
Crystal system | Monoclinic | Absorption coefficient/mm-1 | 0.940 |
Space group | P21/c | F(000) | 616 |
a/nm | 1.00887(9) | Limiting indices | -13≤h≤7, -11≤k≤11, -11≤l≤13 |
b/nm | 0.86747(8) | Reflections collected/unique[R(int)=0.0270] | 5485/1935 |
c/nm | 0.97580(9) | Refinement method | Full-matrix least-squares on F2 |
α/(°) | 90 | Data/restraints/parameters | 1935/7/152 |
β/(°) | 115.0160(10) | Goodness-of-fit on F2 | 1.041 |
γ/(°) | 90 | Final R indices[I>2σ(I)] | R1=0.0307, wR2=0.0795 |
V/nm3 | 0.77387(12) | R indices(all data) | R1=0.0386, wR2=0.0835 |
Z | 2 |
Table 1 Crystal data and structure refinement parameters for compound 1
Empirical formula | Al4P4O19H2Na4 | Calculated density/(Mg·m-3) | 2.694 |
---|---|---|---|
Crystal system | Monoclinic | Absorption coefficient/mm-1 | 0.940 |
Space group | P21/c | F(000) | 616 |
a/nm | 1.00887(9) | Limiting indices | -13≤h≤7, -11≤k≤11, -11≤l≤13 |
b/nm | 0.86747(8) | Reflections collected/unique[R(int)=0.0270] | 5485/1935 |
c/nm | 0.97580(9) | Refinement method | Full-matrix least-squares on F2 |
α/(°) | 90 | Data/restraints/parameters | 1935/7/152 |
β/(°) | 115.0160(10) | Goodness-of-fit on F2 | 1.041 |
γ/(°) | 90 | Final R indices[I>2σ(I)] | R1=0.0307, wR2=0.0795 |
V/nm3 | 0.77387(12) | R indices(all data) | R1=0.0386, wR2=0.0835 |
Z | 2 |
Atom | x | y | z | Ueq | Atom | x | y | z | Ueq |
---|---|---|---|---|---|---|---|---|---|
Al1 | 6752(1) | 2981(1) | 7649(1) | 10(1) | O6 | 7890(2) | -346(2) | 10647(2) | 21(1) |
Al2 | 3834(1) | 3981(1) | 4444(1) | 10(1) | O7 | 3461(2) | -542(2) | 6108(2) | 15(1) |
P1 | 3981(1) | 1123(1) | 6456(1) | 10(1) | O8 | 5577(2) | 4088(2) | 6003(2) | 12(1) |
P2 | 8624(1) | 1262(1) | 10900(1) | 11(1) | O9 | 10259(2) | 1107(2) | 11597(2) | 24(1) |
O1 | 3307(2) | 2031(2) | 4977(2) | 14(1) | O1W | -75(17) | 220(20) | 5430(40) | 43(5) |
O2 | 5659(2) | 1229(2) | 7131(2) | 14(1) | O1W' | 0 | 0 | 5000 | 43(6) |
O3 | 8109(2) | 2037(2) | 9368(2) | 18(1) | Na1 | 9545(1) | 7345(2) | 5822(2) | 32(1) |
O4 | 8167(2) | 2807(2) | 6972(2) | 18(1) | Na2 | 2594(1) | 4450(1) | 7686(2) | 34(1) |
O5 | 3481(2) | 1845(2) | 7602(2) | 14(1) |
Table 2 Atomic coordinates(×104) and equivalent isotropic displacement parameters(10 nm2) for compound 1
Atom | x | y | z | Ueq | Atom | x | y | z | Ueq |
---|---|---|---|---|---|---|---|---|---|
Al1 | 6752(1) | 2981(1) | 7649(1) | 10(1) | O6 | 7890(2) | -346(2) | 10647(2) | 21(1) |
Al2 | 3834(1) | 3981(1) | 4444(1) | 10(1) | O7 | 3461(2) | -542(2) | 6108(2) | 15(1) |
P1 | 3981(1) | 1123(1) | 6456(1) | 10(1) | O8 | 5577(2) | 4088(2) | 6003(2) | 12(1) |
P2 | 8624(1) | 1262(1) | 10900(1) | 11(1) | O9 | 10259(2) | 1107(2) | 11597(2) | 24(1) |
O1 | 3307(2) | 2031(2) | 4977(2) | 14(1) | O1W | -75(17) | 220(20) | 5430(40) | 43(5) |
O2 | 5659(2) | 1229(2) | 7131(2) | 14(1) | O1W' | 0 | 0 | 5000 | 43(6) |
O3 | 8109(2) | 2037(2) | 9368(2) | 18(1) | Na1 | 9545(1) | 7345(2) | 5822(2) | 32(1) |
O4 | 8167(2) | 2807(2) | 6972(2) | 18(1) | Na2 | 2594(1) | 4450(1) | 7686(2) | 34(1) |
O5 | 3481(2) | 1845(2) | 7602(2) | 14(1) |
Al1—O4 | 0.18147(18) | Al2—O1 | 0.19098(18) | P2—O6 | 0.15493(19) |
---|---|---|---|---|---|
Al1—O8 | 0.18163(18) | Al2—Al2#3 | 0.27720(14) | O4—P2#2 | 0.15384(18) |
Al1—O2 | 0.18198(18) | P1—O7 | 0.15253(17) | O5—Al2#4 | 0.18248(18) |
Al1—O7#1 | 0.18381(18) | P1—O1 | 0.15275(17) | O6—Al2#5 | 0.18002(19) |
Al1—O3 | 0.18482(18) | P1—O2 | 0.15375(18) | O7—Al1#5 | 0.18381(18) |
Al2—O8 | 0.17752(18) | P1—O5 | 0.15413(17) | O8—Al2#3 | 0.18895(17) |
Al2—O6#1 | 0.18002(19) | P2—O9 | 0.15006(19) | O1W—O1W' | 0.050(4) |
Al2—O5#2 | 0.18248(18) | P2—O3 | 0.15164(17) | O1W—O1W#6 | 0.099(9) |
Al2—O8#3 | 0.18895(17) | P2—O4#4 | 0.15384(18) | O1W'—O1W#6 | 0.050(4) |
O4—Al1—O8 | 92.40(8) | O6#1—Al2—O1 | 85.80(8) | O9—P2—O6 | 110.56(11) |
O4—Al1—O2 | 107.89(9) | O5#2—Al2—O1 | 87.70(8) | O3—P2—O6 | 107.49(11) |
O8—Al1—O2 | 95.95(8) | O8#3—Al2—O1 | 177.59(8) | O4#4—P2—O6 | 108.68(10) |
O8—Al1—O7#1 | 90.01(8) | O6#1—Al2—Al2#3 | 117.05(7) | P1—O2—Al1 | 126.64(10) |
O2—Al1—O7#1 | 122.63(9) | O5#2—Al2—Al2#3 | 114.53(7) | P2—O3—Al1 | 154.78(12) |
O4—Al1—O3 | 84.21(8) | O8#3—Al2—Al2#3 | 39.33(5) | P2#2—O4—Al1 | 135.39(11) |
O8—Al1—O3 | 173.26(9) | O1—Al2—Al2#3 | 138.29(7) | P1—O5—Al2#4 | 124.65(11) |
O2—Al1—O3 | 90.64(8) | O7—P1—O1 | 107.72(9) | P2—O6—Al2#5 | 133.37(11) |
O7#1—Al1—O3 | 87.62(8) | O7—P1—O2 | 111.38(10) | P1—O7—Al1#5 | 129.71(10) |
O8—Al2—O6#1 | 127.69(9) | O1—P1—O2 | 110.14(10) | Al2—O8—Al1 | 140.33(10) |
O8—Al2—O5#2 | 125.03(9) | O7—P1—O5 | 111.00(10) | Al2—O8—Al2#3 | 98.24(8) |
O6#1—Al2—O5#2 | 107.27(9) | O1—P1—O5 | 108.93(10) | Al1—O8—Al2#3 | 121.43(9) |
O8—Al2—O8#3 | 81.76(8) | O2—P1—O5 | 107.65(10) | O1W'—O1W—O1W#6 | 0.002(15) |
O6#1—Al2—O8#3 | 95.32(8) | O9—P2—O3 | 109.84(11) | O1W—O1W'—O1W#6 | 180.00(2) |
O5#2—Al2—O8#3 | 94.00(8) | O9—P2—O4#4 | 109.07(11) | ||
O8—Al2—O1 | 95.87(8) | O3—P2—O4#4 | 111.19(10) |
Table 3 Selected bond lengths(nm) and bond angles(°) for compound 1*
Al1—O4 | 0.18147(18) | Al2—O1 | 0.19098(18) | P2—O6 | 0.15493(19) |
---|---|---|---|---|---|
Al1—O8 | 0.18163(18) | Al2—Al2#3 | 0.27720(14) | O4—P2#2 | 0.15384(18) |
Al1—O2 | 0.18198(18) | P1—O7 | 0.15253(17) | O5—Al2#4 | 0.18248(18) |
Al1—O7#1 | 0.18381(18) | P1—O1 | 0.15275(17) | O6—Al2#5 | 0.18002(19) |
Al1—O3 | 0.18482(18) | P1—O2 | 0.15375(18) | O7—Al1#5 | 0.18381(18) |
Al2—O8 | 0.17752(18) | P1—O5 | 0.15413(17) | O8—Al2#3 | 0.18895(17) |
Al2—O6#1 | 0.18002(19) | P2—O9 | 0.15006(19) | O1W—O1W' | 0.050(4) |
Al2—O5#2 | 0.18248(18) | P2—O3 | 0.15164(17) | O1W—O1W#6 | 0.099(9) |
Al2—O8#3 | 0.18895(17) | P2—O4#4 | 0.15384(18) | O1W'—O1W#6 | 0.050(4) |
O4—Al1—O8 | 92.40(8) | O6#1—Al2—O1 | 85.80(8) | O9—P2—O6 | 110.56(11) |
O4—Al1—O2 | 107.89(9) | O5#2—Al2—O1 | 87.70(8) | O3—P2—O6 | 107.49(11) |
O8—Al1—O2 | 95.95(8) | O8#3—Al2—O1 | 177.59(8) | O4#4—P2—O6 | 108.68(10) |
O8—Al1—O7#1 | 90.01(8) | O6#1—Al2—Al2#3 | 117.05(7) | P1—O2—Al1 | 126.64(10) |
O2—Al1—O7#1 | 122.63(9) | O5#2—Al2—Al2#3 | 114.53(7) | P2—O3—Al1 | 154.78(12) |
O4—Al1—O3 | 84.21(8) | O8#3—Al2—Al2#3 | 39.33(5) | P2#2—O4—Al1 | 135.39(11) |
O8—Al1—O3 | 173.26(9) | O1—Al2—Al2#3 | 138.29(7) | P1—O5—Al2#4 | 124.65(11) |
O2—Al1—O3 | 90.64(8) | O7—P1—O1 | 107.72(9) | P2—O6—Al2#5 | 133.37(11) |
O7#1—Al1—O3 | 87.62(8) | O7—P1—O2 | 111.38(10) | P1—O7—Al1#5 | 129.71(10) |
O8—Al2—O6#1 | 127.69(9) | O1—P1—O2 | 110.14(10) | Al2—O8—Al1 | 140.33(10) |
O8—Al2—O5#2 | 125.03(9) | O7—P1—O5 | 111.00(10) | Al2—O8—Al2#3 | 98.24(8) |
O6#1—Al2—O5#2 | 107.27(9) | O1—P1—O5 | 108.93(10) | Al1—O8—Al2#3 | 121.43(9) |
O8—Al2—O8#3 | 81.76(8) | O2—P1—O5 | 107.65(10) | O1W'—O1W—O1W#6 | 0.002(15) |
O6#1—Al2—O8#3 | 95.32(8) | O9—P2—O3 | 109.84(11) | O1W—O1W'—O1W#6 | 180.00(2) |
O5#2—Al2—O8#3 | 94.00(8) | O9—P2—O4#4 | 109.07(11) | ||
O8—Al2—O1 | 95.87(8) | O3—P2—O4#4 | 111.19(10) |
Fig.5 Polyhedral view of the structure of compound 1 showing interlayer stacking along [100] direction Na+ ions and H2O located between the layers are presented as balls. Na+ ions in blue; H2O in red.
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