Single crystals of the compounds CuM[B5O10] (M = Tm3+(I), Lu3+(II) have been obtained by a B2O3 flux technique. Their structures are isotypic with CuTb[B5O10]. X-ray investigations on single crystals led to the space group C212v-Iba2 (Nr. 45); I: a = 622,0(2) pm; b = 844,7(1) pm; c = 1266,3(4) pm; Z = 4 and II: a = 618.4(1) pm; b = 845,9(2) pm; c = 1260,9(4) pm; Z = 4. The structure contains 1∞[B5O10]5- chains that include twelve membered rings of boron and oxygen. Each ring consists of two tetrahedral BO4 and two planar B2O5 groups and is connected with neighboring rings via the BO4 units. M3+ (M = Tm3+, Lu3+) is eight-coordinated, while Cu2+ is hexa-coordinated by oxygen.
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