NbSb3O8 crystallizes in the triclinic P1 space group. There are four inequivalent Nb sites. In the first Nb site, Nb(1) is bonded to one O(14), one O(15), one O(30), one O(32), one O(6), and one O(8) atom to form NbO6 octahedra that share corners with four equivalent Sb(10)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-44°. In the second Nb site, Nb(2) is bonded to one O(10), one O(12), one O(18), one O(19), one O(2), and one O(4) atom to form corner-sharing NbO6 octahedra. The corner-sharing octahedral tilt angles range from 35-48°. In the third Nb site, Nb(3) is bonded to one O(1), one O(17), one O(20), one O(25), one O(27), and one O(3) atom to form NbO6 octahedra that share corners with four equivalent Sb(4)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-44°. In the fourth Nb site, Nb(4) is bonded to one O(18), one O(19), one O(2), one O(26), one O(28), and one O(4) atom to form corner-sharing NbO6 octahedra. The corner-sharing octahedral tilt angles range from 35-48°. There are twelve inequivalent Sb sites. In the first Sb site, Sb(1) is bonded in a 5-coordinate geometry to one O(1), one O(11), one O(23), one O(27), and one O(7) atom. In the second Sb site, Sb(2) is bonded in a 5-coordinate geometry to one O(12), one O(2), one O(24), one O(28), and one O(8) atom. In the third Sb site, Sb(3) is bonded to one O(13), one O(16), one O(29), one O(31), one O(5), and one O(7) atom to form corner-sharing SbO6 octahedra. The corner-sharing octahedral tilt angles range from 42-46°. In the fourth Sb site, Sb(4) is bonded to one O(1), one O(11), one O(17), one O(20), one O(3), and one O(9) atom to form SbO6 octahedra that share corners with four equivalent Nb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-44°. In the fifth Sb site, Sb(5) is bonded in a 5-coordinate geometry to one O(15), one O(21), one O(25), one O(6), and one O(9) atom. In the sixth Sb site, Sb(6) is bonded in a 5-coordinate geometry to one O(10), one O(16), one O(22), one O(26), and one O(5) atom. In the seventh Sb site, Sb(7) is bonded in a 5-coordinate geometry to one O(11), one O(17), one O(23), one O(27), and one O(7) atom. In the eighth Sb site, Sb(8) is bonded in a 5-coordinate geometry to one O(12), one O(18), one O(24), one O(28), and one O(8) atom. In the ninth Sb site, Sb(9) is bonded to one O(13), one O(16), one O(22), one O(23), one O(29), and one O(31) atom to form corner-sharing SbO6 octahedra. The corner-sharing octahedral tilt angles range from 42-46°. In the tenth Sb site, Sb(10) is bonded to one O(14), one O(15), one O(21), one O(24), one O(30), and one O(32) atom to form SbO6 octahedra that share corners with four equivalent Nb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-44°. In the eleventh Sb site, Sb(11) is bonded in a 5-coordinate geometry to one O(21), one O(25), one O(32), one O(6), and one O(9) atom. In the twelfth Sb site, Sb(12) is bonded in a 5-coordinate geometry to one O(10), one O(22), one O(26), one O(31), and one O(5) atom. There are thirty-two inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one Nb(3), one Sb(1), and one Sb(4) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to one Nb(2), one Nb(4), and one Sb(2) atom. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one Nb(3) and one Sb(4) atom. In the fourth O site, O(4) is bonded in a bent 150 degrees geometry to one Nb(2) and one Nb(4) atom. In the fifth O site, O(5) is bonded in a trigonal planar geometry to one Sb(12), one Sb(3), and one Sb(6) atom. In the sixth O site, O(6) is bonded in a trigonal planar geometry to one Nb(1), one Sb(11), and one Sb(5) atom. In the seventh O site, O(7) is bonded in a distorted trigonal planar geometry to one Sb(1), one Sb(3), and one Sb(7) atom. In the eighth O site, O(8) is bonded in a distorted trigonal planar geometry to one Nb(1), one Sb(2), and one Sb(8) atom. In the ninth O site, O(9) is bonded in a distorted trigonal planar geometry to one Sb(11), one Sb(4), and one Sb(5) atom. In the tenth O site, O(10) is bonded in a distorted trigonal planar geometry to one Nb(2), one Sb(12), and one Sb(6) atom. In the eleventh O site, O(11) is bonded in a trigonal planar geometry to one Sb(1), one Sb(4), and one Sb(7) atom. In the twelfth O site, O(12) is bonded in a trigonal planar geometry to one Nb(2), one Sb(2), and one Sb(8) atom. In the thirteenth O site, O(13) is bonded in a bent 150 degrees geometry to one Sb(3) and one Sb(9) atom. In the fourteenth O site, O(14) is bonded in a bent 150 degrees geometry to one Nb(1) and one Sb(10) atom. In the fifteenth O site, O(15) is bonded in a 3-coordinate geometry to one Nb(1), one Sb(10), and one Sb(5) atom. In the sixteenth O site, O(16) is bonded in a 3-coordinate geometry to one Sb(3), one Sb(6), and one Sb(9) atom. In the seventeenth O site, O(17) is bonded in a 3-coordinate geometry to one Nb(3), one Sb(4), and one Sb(7) atom. In the eighteenth O site, O(18) is bonded in a 3-coordinate geometry to one Nb(2), one Nb(4), and one Sb(8) atom. In the nineteenth O site, O(19) is bonded in a bent 150 degrees geometry to one Nb(2) and one Nb(4) atom. In the twentieth O site, O(20) is bonded in a bent 150 degrees geometry to one Nb(3) and one Sb(4) atom. In the twenty-first O site, O(21) is bonded in a trigonal planar geometry to one Sb(10), one Sb(11), and one Sb(5) atom. In the twenty-second O site, O(22) is bonded in a trigonal planar geometry to one Sb(12), one Sb(6), and one Sb(9) atom. In the twenty-third O site, O(23) is bonded in a distorted trigonal planar geometry to one Sb(1), one Sb(7), and one Sb(9) atom. In the twenty-fourth O site, O(24) is bonded in a distorted trigonal planar geometry to one Sb(10), one Sb(2), and one Sb(8) atom. In the twenty-fifth O site, O(25) is bonded in a distorted trigonal planar geometry to one Nb(3), one Sb(11), and one Sb(5) atom. In the twenty-sixth O site, O(26) is bonded in a distorted trigonal planar geometry to one Nb(4), one Sb(12), and one Sb(6) atom. In the twenty-seventh O site, O(27) is bonded in a trigonal planar geometry to one Nb(3), one Sb(1), and one Sb(7) atom. In the twenty-eighth O site, O(28) is bonded in a trigonal planar geometry to one Nb(4), one Sb(2), and one Sb(8) atom. In the twenty-ninth O site, O(29) is bonded in a bent 150 degrees geometry to one Sb(3) and one Sb(9) atom. In the thirtieth O site, O(30) is bonded in a bent 150 degrees geometry to one Nb(1) and one Sb(10) atom. In the thirty-first O site, O(31) is bonded in a 3-coordinate geometry to one Sb(12), one Sb(3), and one Sb(9) atom. In the thirty-second O site, O(32) is bonded in a 3-coordinate geometry to one Nb(1), one Sb(10), and one Sb(11) atom.
NbSb3O8 crystallizes in the triclinic P1 space group. There are four inequivalent Nb sites. In the first Nb site, Nb(1) is bonded to one O(14), one O(15), one O(30), one O(32), one O(6), and one O(8) atom to form NbO6 octahedra that share corners with four equivalent Sb(10)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-44°. The Nb(1)-O(14) bond length is 2.00 Å. The Nb(1)-O(15) bond length is 2.06 Å. The Nb(1)-O(30) bond length is 1.94 Å. The Nb(1)-O(32) bond length is 2.02 Å. The Nb(1)-O(6) bond length is 2.10 Å. The Nb(1)-O(8) bond length is 2.01 Å. In the second Nb site, Nb(2) is bonded to one O(10), one O(12), one O(18), one O(19), one O(2), and one O(4) atom to form corner-sharing NbO6 octahedra. The corner-sharing octahedral tilt angles range from 35-48°. The Nb(2)-O(10) bond length is 2.03 Å. The Nb(2)-O(12) bond length is 2.10 Å. The Nb(2)-O(18) bond length is 1.90 Å. The Nb(2)-O(19) bond length is 1.87 Å. The Nb(2)-O(2) bond length is 2.14 Å. The Nb(2)-O(4) bond length is 2.11 Å. In the third Nb site, Nb(3) is bonded to one O(1), one O(17), one O(20), one O(25), one O(27), and one O(3) atom to form NbO6 octahedra that share corners with four equivalent Sb(4)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-44°. The Nb(3)-O(1) bond length is 2.02 Å. The Nb(3)-O(17) bond length is 2.06 Å. The Nb(3)-O(20) bond length is 2.00 Å. The Nb(3)-O(25) bond length is 2.01 Å. The Nb(3)-O(27) bond length is 2.10 Å. The Nb(3)-O(3) bond length is 1.94 Å. In the fourth Nb site, Nb(4) is bonded to one O(18), one O(19), one O(2), one O(26), one O(28), and one O(4) atom to form corner-sharing NbO6 octahedra. The corner-sharing octahedral tilt angles range from 35-48°. The Nb(4)-O(18) bond length is 2.14 Å. The Nb(4)-O(19) bond length is 2.10 Å. The Nb(4)-O(2) bond length is 1.90 Å. The Nb(4)-O(26) bond length is 2.03 Å. The Nb(4)-O(28) bond length is 2.11 Å. The Nb(4)-O(4) bond length is 1.87 Å. There are twelve inequivalent Sb sites. In the first Sb site, Sb(1) is bonded in a 5-coordinate geometry to one O(1), one O(11), one O(23), one O(27), and one O(7) atom. The Sb(1)-O(1) bond length is 2.64 Å. The Sb(1)-O(11) bond length is 2.19 Å. The Sb(1)-O(23) bond length is 2.30 Å. The Sb(1)-O(27) bond length is 2.06 Å. The Sb(1)-O(7) bond length is 2.07 Å. In the second Sb site, Sb(2) is bonded in a 5-coordinate geometry to one O(12), one O(2), one O(24), one O(28), and one O(8) atom. The Sb(2)-O(12) bond length is 2.17 Å. The Sb(2)-O(2) bond length is 2.61 Å. The Sb(2)-O(24) bond length is 2.32 Å. The Sb(2)-O(28) bond length is 2.05 Å. The Sb(2)-O(8) bond length is 2.06 Å. In the third Sb site, Sb(3) is bonded to one O(13), one O(16), one O(29), one O(31), one O(5), and one O(7) atom to form corner-sharing SbO6 octahedra. The corner-sharing octahedral tilt angles range from 42-46°. The Sb(3)-O(13) bond length is 2.02 Å. The Sb(3)-O(16) bond length is 2.04 Å. The Sb(3)-O(29) bond length is 1.99 Å. The Sb(3)-O(31) bond length is 2.03 Å. The Sb(3)-O(5) bond length is 2.07 Å. The Sb(3)-O(7) bond length is 2.01 Å. In the fourth Sb site, Sb(4) is bonded to one O(1), one O(11), one O(17), one O(20), one O(3), and one O(9) atom to form SbO6 octahedra that share corners with four equivalent Nb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-44°. The Sb(4)-O(1) bond length is 2.01 Å. The Sb(4)-O(11) bond length is 2.07 Å. The Sb(4)-O(17) bond length is 1.98 Å. The Sb(4)-O(20) bond length is 1.97 Å. The Sb(4)-O(3) bond length is 2.02 Å. The Sb(4)-O(9) bond length is 2.03 Å. In the fifth Sb site, Sb(5) is bonded in a 5-coordinate geometry to one O(15), one O(21), one O(25), one O(6), and one O(9) atom. The Sb(5)-O(15) bond length is 2.64 Å. The Sb(5)-O(21) bond length is 2.07 Å. The Sb(5)-O(25) bond length is 2.30 Å. The Sb(5)-O(6) bond length is 2.18 Å. The Sb(5)-O(9) bond length is 2.06 Å. In the sixth Sb site, Sb(6) is bonded in a 5-coordinate geometry to one O(10), one O(16), one O(22), one O(26), and one O(5) atom. The Sb(6)-O(10) bond length is 2.06 Å. The Sb(6)-O(16) bond length is 2.60 Å. The Sb(6)-O(22) bond length is 2.07 Å. The Sb(6)-O(26) bond length is 2.30 Å. The Sb(6)-O(5) bond length is 2.19 Å. In the seventh Sb site, Sb(7) is bonded in a 5-coordinate geometry to one O(11), one O(17), one O(23), one O(27), and one O(7) atom. The Sb(7)-O(11) bond length is 2.07 Å. The Sb(7)-O(17) bond length is 2.62 Å. The Sb(7)-O(23) bond length is 2.07 Å. The Sb(7)-O(27) bond length is 2.17 Å. The Sb(7)-O(7) bond length is 2.32 Å. In the eighth Sb site, Sb(8) is bonded in a 5-coordinate geometry to one O(12), one O(18), one O(24), one O(28), and one O(8) atom. The Sb(8)-O(12) bond length is 2.06 Å. The Sb(8)-O(18) bond length is 2.64 Å. The Sb(8)-O(24) bond length is 2.05 Å. The Sb(8)-O(28) bond length is 2.19 Å. The Sb(8)-O(8) bond length is 2.29 Å. In the ninth Sb site, Sb(9) is bonded to one O(13), one O(16), one O(22), one O(23), one O(29), and one O(31) atom to form corner-sharing SbO6 octahedra. The corner-sharing octahedral tilt angles range from 42-46°. The Sb(9)-O(13) bond length is 1.99 Å. The Sb(9)-O(16) bond length is 2.03 Å. The Sb(9)-O(22) bond length is 2.06 Å. The Sb(9)-O(23) bond length is 2.01 Å. The Sb(9)-O(29) bond length is 2.02 Å. The Sb(9)-O(31) bond length is 2.03 Å. In the tenth Sb site, Sb(10) is bonded to one O(14), one O(15), one O(21), one O(24), one O(30), and one O(32) atom to form SbO6 octahedra that share corners with four equivalent Nb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-44°. The Sb(10)-O(14) bond length is 1.97 Å. The Sb(10)-O(15) bond length is 1.98 Å. The Sb(10)-O(21) bond length is 2.06 Å. The Sb(10)-O(24) bond length is 2.03 Å. The Sb(10)-O(30) bond length is 2.02 Å. The Sb(10)-O(32) bond length is 2.01 Å. In the eleventh Sb site, Sb(11) is bonded in a 5-coordinate geometry to one O(21), one O(25), one O(32), one O(6), and one O(9) atom. The Sb(11)-O(21) bond length is 2.19 Å. The Sb(11)-O(25) bond length is 2.06 Å. The Sb(11)-O(32) bond length is 2.63 Å. The Sb(11)-O(6) bond length is 2.05 Å. The Sb(11)-O(9) bond length is 2.31 Å. In the twelfth Sb site, Sb(12) is bonded in a 5-coordinate geometry to one O(10), one O(22), one O(26), one O(31), and one O(5) atom. The Sb(12)-O(10) bond length is 2.29 Å. The Sb(12)-O(22) bond length is 2.19 Å. The Sb(12)-O(26) bond length is 2.06 Å. The Sb(12)-O(31) bond length is 2.60 Å. The Sb(12)-O(5) bond length is 2.07 Å. There are thirty-two inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one Nb(3), one Sb(1), and one Sb(4) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to one Nb(2), one Nb(4), and one Sb(2) atom. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one Nb(3) and one Sb(4) atom. In the fourth O site, O(4) is bonded in a bent 150 degrees geometry to one Nb(2) and one Nb(4) atom. In the fifth O site, O(5) is bonded in a trigonal planar geometry to one Sb(12), one Sb(3), and one Sb(6) atom. In the sixth O site, O(6) is bonded in a trigonal planar geometry to one Nb(1), one Sb(11), and one Sb(5) atom. In the seventh O site, O(7) is bonded in a distorted trigonal planar geometry to one Sb(1), one Sb(3), and one Sb(7) atom. In the eighth O site, O(8) is bonded in a distorted trigonal planar geometry to one Nb(1), one Sb(2), and one Sb(8) atom. In the ninth O site, O(9) is bonded in a distorted trigonal planar geometry to one Sb(11), one Sb(4), and one Sb(5) atom. In the tenth O site, O(10) is bonded in a distorted trigonal planar geometry to one Nb(2), one Sb(12), and one Sb(6) atom. In the eleventh O site, O(11) is bonded in a trigonal planar geometry to one Sb(1), one Sb(4), and one Sb(7) atom. In the twelfth O site, O(12) is bonded in a trigonal planar geometry to one Nb(2), one Sb(2), and one Sb(8) atom. In the thirteenth O site, O(13) is bonded in a bent 150 degrees geometry to one Sb(3) and one Sb(9) atom. In the fourteenth O site, O(14) is bonded in a bent 150 degrees geometry to one Nb(1) and one Sb(10) atom. In the fifteenth O site, O(15) is bonded in a 3-coordinate geometry to one Nb(1), one Sb(10), and one Sb(5) atom. In the sixteenth O site, O(16) is bonded in a 3-coordinate geometry to one Sb(3), one Sb(6), and one Sb(9) atom. In the seventeenth O site, O(17) is bonded in a 3-coordinate geometry to one Nb(3), one Sb(4), and one Sb(7) atom. In the eighteenth O site, O(18) is bonded in a 3-coordinate geometry to one Nb(2), one Nb(4), and one Sb(8) atom. In the nineteenth O site, O(19) is bonded in a bent 150 degrees geometry to one Nb(2) and one Nb(4) atom. In the twentieth O site, O(20) is bonded in a bent 150 degrees geometry to one Nb(3) and one Sb(4) atom. In the twenty-first O site, O(21) is bonded in a trigonal planar geometry to one Sb(10), one Sb(11), and one Sb(5) atom. In the twenty-second O site, O(22) is bonded in a trigonal planar geometry to one Sb(12), one Sb(6), and one Sb(9) atom. In the twenty-third O site, O(23) is bonded in a distorted trigonal planar geometry to one Sb(1), one Sb(7), and one Sb(9) atom. In the twenty-fourth O site, O(24) is bonded in a distorted trigonal planar geometry to one Sb(10), one Sb(2), and one Sb(8) atom. In the twenty-fifth O site, O(25) is bonded in a distorted trigonal planar geometry to one Nb(3), one Sb(11), and one Sb(5) atom. In the twenty-sixth O site, O(26) is bonded in a distorted trigonal planar geometry to one Nb(4), one Sb(12), and one Sb(6) atom. In the twenty-seventh O site, O(27) is bonded in a trigonal planar geometry to one Nb(3), one Sb(1), and one Sb(7) atom. In the twenty-eighth O site, O(28) is bonded in a trigonal planar geometry to one Nb(4), one Sb(2), and one Sb(8) atom. In the twenty-ninth O site, O(29) is bonded in a bent 150 degrees geometry to one Sb(3) and one Sb(9) atom. In the thirtieth O site, O(30) is bonded in a bent 150 degrees geometry to one Nb(1) and one Sb(10) atom. In the thirty-first O site, O(31) is bonded in a 3-coordinate geometry to one Sb(12), one Sb(3), and one Sb(9) atom. In the thirty-second O site, O(32) is bonded in a 3-coordinate geometry to one Nb(1), one Sb(10), and one Sb(11) atom.