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Download Author Version (PDF) Dalton Transactions Accepted Manuscript This is an Accepted Manuscript, which has been through the Royal Society of Chemistry peer review process and has been accepted for publication. Accepted Manuscripts are published online shortly after acceptance, before technical editing, formatting and proof reading. Using this free service, authors can make their results available to the community, in citable form, before we publish the edited article. We will replace this Accepted Manuscript with the edited and formatted Advance Article as soon as it is available. You can find more information about Accepted Manuscripts in the Information for Authors. Please note that technical editing may introduce minor changes to the text and/or graphics, which may alter content. The journal’s standard Terms & Conditions and the Ethical guidelines still apply. In no event shall the Royal Society of Chemistry be held responsible for any errors or omissions in this Accepted Manuscript or any consequences arising from the use of any information it contains. www.rsc.org/dalton Page 1 of 9 Dalton Transactions Table of contents Manuscript title: Structural Insights for the Design of New Borate-phosphates: Synthesis, Crystal Structure and Optical Properties of Pb 4O(BO 3)(PO 4) and Bi 4O3(BO 3)(PO 4) Manuscript Accepted A principle to design new borate-phosphates has been proposed. Transactions Dalton Dalton Transactions Page 2 of 9 Dalton Transactions RSC Publishing PAPER Structural Insights for the Design of New Borate- phosphates: Synthesis, Crystal Structure and Optical Cite this: DOI: 10.1039/x0xx00000x Properties of Pb 4O(BO 3)(PO 4) and Bi 4O3(BO 3)(PO 4) † Ying Wang, a,b Shilie Pan, *a Shengshi Huang, a,b Lingyun Dong,a,b Min Zhang a Received 00th January 2012, Shujuan Han a and Xian Wang a Accepted 00th January 2012 DOI: 10.1039/x0xx00000x Two new metal borate-phosphates, Pb 4O(BO 3)(PO 4) ( 1) and Bi 4O3(BO 3)(PO 4) ( 2) have been successfully designed and synthesized. The structures of the title compounds were determined www.rsc.org/ by single-crystal X-ray diffraction.The title compounds have similar crystal structures consisting of oxygen-centered (OPb 4) or (OBi 4) tetrahedra as well as isolated BO 3 and PO 4 Manuscript groups. Structural comparison and the Madelung energy calculation indicate that the title compounds also exhibit strong correlation to known metal borates and phosphates. In addition, a strategy of BO 3-PO 4 substitution is proposed for designing new borate-phosphates. Thermal analyses, IR spectra and UV-vis-NIR diffuse reflectance spectra have also been performed. Introduction phosphates with novel properties. After carefully analyzing the known borate-phosphates, first of all, we noticed that the ratio Borate and phosphate compounds have been widely studied of borate to phosphate units equals one (B/P ratio = 1) in most over the past decades due to their rich structural chemistry and borate-phosphates, which suggests that borate-phosphates can Accepted magnetic, optical, and electrical applications. 1 In recent years, be synthesized by the reaction of stoichiometric metal borates many attempts have been made to explore new compounds and phosphates. For example, stoichiometric Mg (BO ) and containing both B-O and P-O groups, and a large number of 3 3 2 Mg (PO ) were used as precursors for preparing useful functional materials have be obtained. For example, 3 4 2 Mg (BO )(PO ). 10 d Moreover, according to J. G. Fletcher et al, M BP O (M= Fe, Cr) show interesting magnetic properties; 2 3 3 4 2 3 12 the BO groups can occupy PO sites of the apatite Ca (PO ) F, β-Zn (BO )(PO ), 3 MBPO (M = Sr and Ba), 4 Na Cd B(PO ) 5 3 4 5 4 3 3 3 4 5 3 3 4 4 leading to the new compound Ca (BO ) F. 17 Inspired by that and AMBP O (A= K, M = Sr, Ba and A = K, Rb, M = Pb) 6 are 5 3 3 2 8 finding, we analyzed the structures of all known borate- potential nonlinear optical materials; The Eu 2+ -doped phosphates. Interestingly, in some case, the structure of borate- Ba BP O have been found an application as a new 3 3 12 phosphates could be viewed as a borate in which half of BO scintillation material. 7 3 triangles are replaced by PO tetrahedra, or a phosphate in According to the classification proposed by R. Kniep et al, 8 4 which fifty percent of PO tetrahedra are substituted by BO there are two types of compounds containing both B-O and P-O 4 3 triangles. Fig. S1 in the ESI† illustrates an example of the groups but with obvious differences: a) borophosphates: the substitution relationship of BO -PO groups and the structural Transactions ones at least one BO (or BO ) group and one PO tetrahedron 3 4 3 4 4 similarities among Co (BO ) ,18 Co (PO ) ,19 and share a common O atom; b) borate-phosphates: isolated 3 3 2 3 4 2 Co (BO )(PO ). 10 b Therefore, we suppose that new borate- character of BO /BO and PO anionic units. So far, a large 3 3 4 3 4 4 phosphates may be obtained by mutual replacement between number of borophosphates with quite different structures have BO triangles and PO tetrahedra in known borates or been synthesized. 8-9 On the contrary, borate-phosphates are less 3 4 phosphates. common. To the best of our knowledge, M 3(BO 3)(PO 4) (M = 10 11 Leaving those insights, we pay much more attention on Ba, Co, Mg, Zn and Cd), SrCo (BO )(PO ), Dalton 2 3 4 metal borates or phosphates for discovering new borate- Ln O (BO )(PO ) (Ln= La, Pr, Nd, Sm, Gd, and Dy), 12 7 6 3 4 2 phosphates. Recently, a series of oxosalts, Pb B O ,20 K Ln[OB(OH) ] [HOPO ] (Ln = Yb and Lu), 13 M (BO )(PO ) 4 2 7 3 2 2 3 2 2 4 4 Pb O(PO ) ,21 Bi O (BO ) 22 and Bi (PO ) O (0.175 ≤ x (M = Th and U),14 Ba ((UO )(PO ) (B O )) (H O) 15 and the 4 4 2 4 3 3 2 4+x 4 2 3+3x/2 5 2 4 3 5 9 2 0.125 ≤ 1) 23 have been reported. We have, therefore, investigated the mineral Seamanite, Mn (OH) [B(OH) ][PO ]16 are the only 3 2 4 4 Pb-B-P-O and Bi-B-P-O system. Two new borate-phosphates: known borate-phosphates. Pb O(BO )(PO ) ( 1) and Bi O (BO )(PO ) ( 2) have been In order to enrich the borate-phosphate family, we are trying 4 3 4 4 3 3 4 obtained. As we expected, the two compounds show some to figure out an efficient way to design and synthesize borate- This journal is © The Royal Society of Chemistry 2013 Dalton Trans | 1 Page 3 of 9 Dalton Transactions PAPER Dalton Transactions structural similarities with corresponding metal borate and summarized in Table 1. The atomic coordinates and isotropic phosphate. Herein, we report the synthesis and characterization displacement coefficients are listed in Table S1 in the ESI†. of the two compounds with a focus on the structural Important bond lengths are listed in Table S2 in the ESI†. relationship among borate, phosphate and borate-phosphate. Table 1. Crystal Data and Structural Refinements for the two Experimental compounds. Synthesis compound 1 2 All commercially available chemicals are of reagent grade and used as received. Single crystals of compounds 1 and 2 were formula weight (g·mol -1) 998.54 1037.70 grown from a high temperature solution. A mixture of 1.115 g (5.00 mmol) of PbO, 0.062 g (1.00 mmol) of H 3BO 3, and 0.115 crystal system Monoclinic Orthorhombic g (1.00 mmol) of NH 4H2PO 4 for compound 1 and a mixture of 1.631 g (3.50 mmol) of Bi 2O3, 0.062 g (1.00 mmol) of H 3BO 3, space group P21/c Pbca and 0.230 g (2.00 mmol) of NH 4H2PO 4 for compound 2 were thoroughly ground. The respective mixtures were prepared in a a (Å) 10.202(2) 5.536(6) platinum crucible and held at 850 °C (950 °C for compound 2) for 12 h in a programmable temperature electric furnace. The b (Å) 7.0047(1) 14.102(1) homogenized solutions then slowly cooled down to 700 °C at a Manuscript rate of 3 °C/h, and finally cooled down to room temperature at c (Å) 12.921(4) 22.62(2) a rate of 50 °C/h. Colorless block crystals were separated from β (deg) 113.057(1) the crucible for structural characterization (estimated yield: 10- 15% for compound 1 and 5–10% for compound 2, based on the volume (Å 3) 849.6(4) 1766(3) P contents). It should be mentioned that side products were also observed. For compound 1, Pb 4O(PO 4)2 has been found, and for Z 4 8 compound 2, the side product is Bi 3PO 7. The ratio of main -3 products/side products for both compounds is about 1:1 as Dcalcd (g·cm ) 7.807 7.807 observed by naked eye and single crystal diffraction measurement. absorption coeffient (mm -1) 79.227 79.715 Accepted After structural analysis, polycrystalline samples of the two 2 compounds were prepared by conventional solid-state methods. GOF on F 1.059 1.011 Separate stoichiometric mixture of PbO/Bi O , H BO and 2 3 3 3 2 2 a R1, wR2 [Fo >2 σ( Fo )] 0.0508, 0.1258 0.0365, 0.0806 NH 4H2PO 4 was initially ground well.
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