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Hydrothermal Synthesis and Crystal Structure of (enH_2)_5[(VO)_(12)O_6B_(18)O_(36)(OH)_6]·2(H_3O) ·6H_2O

Zun-Xing Huang

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Abstract

A hydrothermal reaction of NH_(4)VO_(3),H_(3)BO_(3),NH_(2)CH_(2)CH_(2)NH_(2),MoO_(3),H_(2)O in a molar ratio of 2∶20∶9∶3∶222 gives a black prism crystal(enH_(2))_(5)[(VO)_(12)O_(6)B_(18)O_(36)(OH)_(6)]·2(H_(3)O)·6H_(2)O.It crystallizes in triclinic system with space group Pī and unit cell parameters a=1.336 8(3) nm,b=(1.599 8(3) nm), c=1.663 4(3) nm,α=94.040(1)°,β=91.530(1)°,γ=95.830(1)°,V=(3.528 1(12) nm~(3)),Z=2,Dc=2.099 g/cm~(3),μ=1.648 mm~(-1),F(000)=2 228,the final R_(1)=(0.047 5),wR_(2)=0.150 4,S=1.039 for 15 641 observed reflections with I 2σ(I).The structure is mainly composed of a [(VO)_(12)O_(6)B_(18)O_(36)(OH)_(6)]~(12-)cluster.The cluster consists of a B_(18)O_(36)(OH)_(6) ring sandwiched between two vanadium-oxygen rings V_(6)O_(18) by eighteen B—(μ_(3)-O)—V bonds,the intercluster space is filled by (enH_(2))~(2+) and water molecules.

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A hydrothermal reaction of NH_(4)VO_(3),H_(3)BO_(3),NH_(2)CH_(2)CH_(2)NH_(2),MoO_(3),H_(2)O in a molar ratio of 2∶20∶9∶3∶222 gives a black prism crystal(enH_(2))_(5)[(VO)_(12)O_(6)B_(18)O_(36)(OH)_(6)]·2(H_(3)O)·6H_(2)O.It crystallizes in triclinic system with space group Pī and unit cell parameters a=1.336 8(3) nm,b=(1.599 8(3) nm), c=1.663 4(3) nm,α=94.040(1)°,β=91.530(1)°,γ=95.830(1)°,V=(3.528 1(12) nm~(3)),Z=2,Dc=2.099 g/cm~(3),μ=1.648 mm~(-1),F(000)=2 228,the final R_(1)=(0.047 5),wR_(2)=0.150 4,S=1.039 for 15 641 observed reflections with I 2σ(I).The structure is mainly composed of a [(VO)_(12)O_(6)B_(18)O_(36)(OH)_(6)]~(12-)cluster.The cluster consists of a B_(18)O_(36)(OH)_(6) ring sandwiched between two vanadium-oxygen rings V_(6)O_(18) by eighteen B—(μ_(3)-O)—V bonds,the intercluster space is filled by (enH_(2))~(2+) and water molecules.

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Available abstract

A hydrothermal reaction of NH_(4)VO_(3),H_(3)BO_(3),NH_(2)CH_(2)CH_(2)NH_(2),MoO_(3),H_(2)O in a molar ratio of 2∶20∶9∶3∶222 gives a black prism crystal(enH_(2))_(5)[(VO)_(12)O_(6)B_(18)O_(36)(OH)_(6)]·2(H_(3)O)·6H_(2)O.It crystallizes in triclinic system with space group Pī and unit cell parameters a=1.336 8(3) nm,b=(1.599 8(3) nm), c=1.663 4(3) nm,α=94.040(1)°,β=91.530(1)°,γ=95.830(1)°,V=(3.528 1(12) nm~(3)),Z=2,Dc=2.099 g/cm~(3),μ=1.648 mm~(-1),F(000)=2 228,the final R_(1)=(0.047 5),wR_(2)=0.150 4,S=1.039 for 15 641 observed reflections with I 2σ(I).The structure is mainly composed of a [(VO)_(12)O_(6)B_(18)O_(36)(OH)_(6)]~(12-)cluster.The cluster consists of a B_(18)O_(36)(OH)_(6) ring sandwiched between two vanadium-oxygen rings V_(6)O_(18) by eighteen B—(μ_(3)-O)—V bonds,the intercluster space is filled by (enH_(2))~(2+) and water molecules.

Key concepts: Triclinic crystal system, Crystallography, Crystal structure, Chemistry, Hydrothermal synthesis, Molecule, Hydrothermal circulation, Molar ratio

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Hydrothermal Synthesis and Crystal Structure of (enH_2)_5[(VO)_(12)O_6B_(18)O_(36)(OH)_6]·2(H_3O) ·6H_2O — Research Paper | ScholarLens