Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768107002340/ck5021sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768107002340/ck5021Ca5_Nb4_Ti_O17sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768107002340/ck5021Ca6_Nb,Ti6_O20sup3.hkl |
For both compounds, program(s) used to refine structure: (Jana2000; Petricek and Dusek, 2000); software used to prepare material for publication: (Jana2000; Petricek and Dusek, 2000).
Ca3.333Nb2.666O11.333Ti0.667 | V = 224.77 (2) Å3 |
Mr = 594.5 | Z = 1 |
Monoclinic, ?† | F(000) = 282 |
q = 0.08333b* | Dx = 4.391 Mg m−3 |
a = 7.6889 (3) Å | Mo Kα radiation, λ = 0.71069 Å |
b = 5.3381 (3) Å | µ = 5.87 mm−1 |
c = 5.4763 (1) Å | T = 295 K |
β = 90° | × × mm |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, −x3, 1/2−x4; (3) 1/4−x1, −x2, 1/2+x3, 1/4−x4; (4) x1, 1/2+x2, 1/2−x3, x4; (5) 1/2+x1, x2, x3, 1/2+x4; (6) 1/2−x1, −x2, −x3, −x4; (7) 3/4−x1, −x2, 1/2+x3, 3/4−x4; (8) 1/2+x1, 1/2+x2, 1/2−x3, 1/2+x4; (9) 3/4+x1, 1/2+x2, x3, 1/4+x4; (10) 3/4−x1, 1/2−x2, −x3, 3/4−x4; (11) −x1, 1/2−x2, 1/2+x3, 1/2−x4; (12) 3/4+x1, x2, 1/2−x3, 1/4+x4; (13) 1/4+x1, 1/2+x2, x3, 3/4+x4; (14) 1/4−x1, 1/2−x2, −x3, 1/4−x4; (15) 1/2−x1, 1/2−x2, 1/2+x3, −x4; (16) 1/4+x1, x2, 1/2−x3, 3/4+x4. |
3231 independent reflections | k = ?→? |
2731 reflections with I > 3σ(I) | l = ?→? |
h = ?→? |
Refinement on F | 146 parameters |
R[F2 > 2σ(F2)] = 0.051 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
wR(F2) = 0.061 | (Δ/σ)max = 0.005 |
S = 2.63 | Δρmax = 3.02 e Å−3 |
3231 reflections | Δρmin = −2.65 e Å−3 |
Ca3.333Nb2.666O11.333Ti0.667 | β = 90° |
Mr = 594.5 | V = 224.77 (2) Å3 |
Monoclinic, ?† | Z = 1 |
q = 0.08333b* | Mo Kα radiation |
a = 7.6889 (3) Å | µ = 5.87 mm−1 |
b = 5.3381 (3) Å | T = 295 K |
c = 5.4763 (1) Å | × × mm |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, −x3, 1/2−x4; (3) 1/4−x1, −x2, 1/2+x3, 1/4−x4; (4) x1, 1/2+x2, 1/2−x3, x4; (5) 1/2+x1, x2, x3, 1/2+x4; (6) 1/2−x1, −x2, −x3, −x4; (7) 3/4−x1, −x2, 1/2+x3, 3/4−x4; (8) 1/2+x1, 1/2+x2, 1/2−x3, 1/2+x4; (9) 3/4+x1, 1/2+x2, x3, 1/4+x4; (10) 3/4−x1, 1/2−x2, −x3, 3/4−x4; (11) −x1, 1/2−x2, 1/2+x3, 1/2−x4; (12) 3/4+x1, x2, 1/2−x3, 1/4+x4; (13) 1/4+x1, 1/2+x2, x3, 3/4+x4; (14) 1/4−x1, 1/2−x2, −x3, 1/4−x4; (15) 1/2−x1, 1/2−x2, 1/2+x3, −x4; (16) 1/4+x1, x2, 1/2−x3, 3/4+x4. |
R[F2 > 2σ(F2)] = 0.051 | 146 parameters |
wR(F2) = 0.061 | Δρmax = 3.02 e Å−3 |
S = 2.63 | Δρmin = −2.65 e Å−3 |
3231 reflections |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ca1 | −0.00010 (10) | −0.03459 (17) | 0.00495 (14) | 0.0107 (3) | 0.125 |
Ca2 | 0.00186 (16) | 0.3304 (2) | −0.0818 (2) | 0.0087 (3) | 0.0417 |
Ca3 | −0.00721 (17) | −0.2504 (3) | 0.0136 (3) | 0.0159 (4) | 0.0417 |
Nb11 | 0.25 | 0 | 0.5 | 0.00382 (16) | 0.167 (7) |
Ti11 | 0.25 | 0 | 0.5 | 0.00382 (16) | 0.041 (7) |
Nb12 | 0.25 | 0 | 0.5 | 0.00382 (16) | 0.144 (7) |
Ti12 | 0.25 | 0 | 0.5 | 0.00382 (16) | 0.022 (7) |
Nb13 | 0.25 | 0 | 0.5 | 0.00382 (16) | 0.078 (7) |
Ti13 | 0.25 | 0 | 0.5 | 0.00382 (16) | 0.005 (7) |
Nb21 | 0.75 | 0 | 0.5 | 0.00388 (16) | 0.172 (7) |
Ti21 | 0.75 | 0 | 0.5 | 0.00388 (16) | 0.036 (7) |
Nb22 | 0.75 | 0 | 0.5 | 0.00388 (16) | 0.148 (15) |
Ti22 | 0.75 | 0 | 0.5 | 0.00388 (16) | 0.019 (15) |
Nb23 | 0.75 | 0 | 0.5 | 0.00388 (16) | 0.079 (15) |
Ti23 | 0.75 | 0 | 0.5 | 0.00388 (16) | 0.004 (15) |
O1 | −0.0001 (2) | 0.0137 (3) | 0.5794 (4) | 0.0069 (6) | 0.2083 |
O2 | 0.2145 (2) | 0.2118 (3) | 0.2060 (3) | 0.0073 (5) | 0.25 |
O3 | 0.7864 (2) | 0.1989 (3) | 0.1976 (4) | 0.0077 (5) | 0.25 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ca1 | 0.0094 (5) | 0.0123 (4) | 0.0105 (5) | 0.0001 (3) | −0.0003 (3) | −0.0032 (3) |
Ca2 | 0.0057 (6) | 0.0117 (6) | 0.0088 (6) | −0.0006 (5) | −0.0002 (6) | −0.0013 (5) |
Ca3 | 0.0081 (6) | 0.0280 (8) | 0.0115 (7) | 0.0003 (6) | −0.0002 (6) | −0.0044 (6) |
Nb11 | 0.0032 (3) | 0.0041 (3) | 0.0042 (3) | 0.0001 (2) | −0.00012 (14) | 0.00052 (14) |
Ti11 | 0.0032 (3) | 0.0041 (3) | 0.0042 (3) | 0.0001 (2) | −0.00012 (14) | 0.00052 (14) |
Nb12 | 0.0032 (3) | 0.0041 (3) | 0.0042 (3) | 0.0001 (2) | −0.00012 (14) | 0.00052 (14) |
Ti12 | 0.0032 (3) | 0.0041 (3) | 0.0042 (3) | 0.0001 (2) | −0.00012 (14) | 0.00052 (14) |
Nb13 | 0.0032 (3) | 0.0041 (3) | 0.0042 (3) | 0.0001 (2) | −0.00012 (14) | 0.00052 (14) |
Ti13 | 0.0032 (3) | 0.0041 (3) | 0.0042 (3) | 0.0001 (2) | −0.00012 (14) | 0.00052 (14) |
Nb21 | 0.0032 (3) | 0.0043 (3) | 0.0042 (3) | −0.0005 (2) | 0.00000 (14) | 0.00025 (13) |
Ti21 | 0.0032 (3) | 0.0043 (3) | 0.0042 (3) | −0.0005 (2) | 0.00000 (14) | 0.00025 (13) |
Nb22 | 0.0032 (3) | 0.0043 (3) | 0.0042 (3) | −0.0005 (2) | 0.00000 (14) | 0.00025 (13) |
Ti22 | 0.0032 (3) | 0.0043 (3) | 0.0042 (3) | −0.0005 (2) | 0.00000 (14) | 0.00025 (13) |
Nb23 | 0.0032 (3) | 0.0043 (3) | 0.0042 (3) | −0.0005 (2) | 0.00000 (14) | 0.00025 (13) |
Ti23 | 0.0032 (3) | 0.0043 (3) | 0.0042 (3) | −0.0005 (2) | 0.00000 (14) | 0.00025 (13) |
O1 | 0.0046 (10) | 0.0096 (11) | 0.0065 (10) | 0.0000 (8) | 0.0003 (7) | 0.0010 (7) |
O2 | 0.0077 (9) | 0.0072 (9) | 0.0070 (8) | −0.0006 (7) | −0.0011 (7) | 0.0021 (7) |
O3 | 0.0088 (9) | 0.0062 (9) | 0.0081 (9) | 0.0002 (7) | 0.0008 (7) | 0.0020 (7) |
Average | Minimum | Maximum | |
Ca1—O1i | 2.36 (3) | 2.36 (3) | 2.36 (3) |
Ca1—O2 | 2.37 (3) | 2.37 (3) | 2.37 (3) |
Ca1—O2ii | 2.68 (3) | 2.68 (3) | 2.68 (3) |
Ca1—O3iii | 2.36 (3) | 2.36 (3) | 2.36 (3) |
Ca1—O3ii | 2.66 (3) | 2.66 (3) | 2.66 (3) |
Ca1—O11iv | 2.38 (2) | 2.38 (2) | 2.38 (2) |
Ca1—O11v | 2.97 (2) | 2.97 (2) | 2.97 (2) |
Ca1—O21iv | 2.64 (3) | 2.64 (3) | 2.64 (3) |
Ca1—O31vi | 2.65 (3) | 2.65 (3) | 2.65 (3) |
Ca2—O1i | 2.54 (2) | 2.54 (2) | 2.54 (2) |
Ca2—O2 | 2.36 (3) | 2.36 (3) | 2.36 (3) |
Ca2—O2vii | 2.46 (3) | 2.46 (3) | 2.46 (3) |
Ca2—O3iii | 2.31 (3) | 2.31 (3) | 2.31 (3) |
Ca2—O21viii | 2.45 (2) | 2.45 (2) | 2.45 (2) |
Ca2—O21ix | 2.444 (18) | 2.444 (18) | 2.444 (18) |
Ca2—O31ix | 2.470 (17) | 2.470 (17) | 2.470 (17) |
Ca3—O1i | 2.65 (2) | 2.65 (2) | 2.65 (2) |
Ca3—O2ii | 2.50 (3) | 2.50 (3) | 2.50 (3) |
Ca3—O3iii | 2.95 (3) | 2.95 (3) | 2.95 (3) |
Ca3—O3ii | 2.39 (3) | 2.39 (3) | 2.39 (3) |
Ca3—O21iv | 2.384 (19) | 2.384 (19) | 2.384 (19) |
Ca3—O31x | 2.428 (18) | 2.428 (18) | 2.428 (18) |
Ca3—O31vi | 2.446 (18) | 2.446 (18) | 2.446 (18) |
Nb11—O1 | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Nb11—O1xi | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Nb11—O2 | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Nb11—O2xi | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Nb11—O21xii | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb11—O21iv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti11—O1 | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Ti11—O1xi | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Ti11—O2 | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Ti11—O2xi | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Ti11—O21xii | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti11—O21iv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb12—O2xii | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Nb12—O2xiii | 2.16 (3) | 2.16 (3) | 2.16 (3) |
Nb12—O11 | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb12—O11xiv | 2.00 (3) | 2.00 (3) | 2.00 (3) |
Nb12—O21 | 1.90 (4) | 1.90 (4) | 1.90 (4) |
Nb12—O21xiv | 2.08 (3) | 2.08 (3) | 2.08 (3) |
Ti12—O2xii | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Ti12—O2xiii | 2.16 (3) | 2.16 (3) | 2.16 (3) |
Ti12—O11 | 1.98 (2) | 1.98 (2) | 1.98 (2) |
Ti12—O11xiv | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Ti12—O21 | 1.90 (4) | 1.90 (4) | 1.90 (4) |
Ti12—O21xiv | 2.08 (3) | 2.08 (3) | 2.08 (3) |
Nb13—O1 | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Nb13—O1xi | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Nb13—O2 | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Nb13—O2xi | 2.23 (3) | 2.23 (3) | 2.23 (3) |
Nb13—O21xii | 1.83 (2) | 1.83 (2) | 1.83 (2) |
Nb13—O21iv | 2.11 (4) | 2.11 (4) | 2.11 (4) |
Ti13—O1 | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Ti13—O1xi | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Ti13—O2 | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Ti13—O2xi | 2.23 (3) | 2.23 (3) | 2.23 (3) |
Ti13—O21xii | 1.83 (2) | 1.83 (2) | 1.83 (2) |
Ti13—O21iv | 2.11 (4) | 2.11 (4) | 2.11 (4) |
Nb21—O1xv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb21—O1xi | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb21—O3 | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Nb21—O3xvi | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Nb21—O31xvii | 1.99 (3) | 1.99 (3) | 1.99 (3) |
Nb21—O31iv | 1.99 (3) | 1.99 (3) | 1.99 (3) |
Ti21—O1xv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti21—O1xi | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti21—O3 | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Ti21—O3xvi | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Ti21—O31xvii | 1.99 (3) | 1.99 (3) | 1.99 (3) |
Ti21—O31iv | 1.99 (3) | 1.99 (3) | 1.99 (3) |
Nb22—O3xvii | 1.85 (3) | 1.85 (3) | 1.85 (3) |
Nb22—O3xiii | 2.17 (3) | 2.17 (3) | 2.17 (3) |
Nb22—O11xv | 1.97 (2) | 1.97 (2) | 1.97 (2) |
Nb22—O11xiv | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Nb22—O31 | 1.90 (4) | 1.90 (4) | 1.90 (4) |
Nb22—O31xviii | 2.09 (3) | 2.09 (3) | 2.09 (3) |
Ti22—O3xvii | 1.85 (3) | 1.85 (3) | 1.85 (3) |
Ti22—O3xiii | 2.17 (3) | 2.17 (3) | 2.17 (3) |
Ti22—O11xv | 1.97 (2) | 1.97 (2) | 1.97 (2) |
Ti22—O11xiv | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Ti22—O31 | 1.90 (4) | 1.90 (4) | 1.90 (4) |
Ti22—O31xviii | 2.09 (3) | 2.09 (3) | 2.09 (3) |
Nb23—O1xv | 1.98 (2) | 1.98 (2) | 1.98 (2) |
Nb23—O1xi | 2.02 (2) | 2.02 (2) | 2.02 (2) |
Nb23—O3 | 1.79 (3) | 1.79 (3) | 1.79 (3) |
Nb23—O3xvi | 2.26 (3) | 2.26 (3) | 2.26 (3) |
Nb23—O31xvii | 1.850 (18) | 1.850 (18) | 1.850 (18) |
Nb23—O31iv | 2.15 (4) | 2.15 (4) | 2.15 (4) |
Ti23—O1xv | 1.98 (2) | 1.98 (2) | 1.98 (2) |
Ti23—O1xi | 2.02 (2) | 2.02 (2) | 2.02 (2) |
Ti23—O3 | 1.79 (3) | 1.79 (3) | 1.79 (3) |
Ti23—O3xvi | 2.26 (3) | 2.26 (3) | 2.26 (3) |
Ti23—O31xvii | 1.850 (18) | 1.850 (18) | 1.850 (18) |
Ti23—O31iv | 2.15 (4) | 2.15 (4) | 2.15 (4) |
O1—O2 | 2.84 (4) | 2.77 (4) | 2.96 (4) |
O1—O2xi | 2.79 (4) | 2.75 (3) | 2.83 (3) |
O1—O3iii | 2.83 (4) | 2.78 (4) | 2.92 (4) |
O1—O3xi | 2.79 (4) | 2.74 (4) | 2.84 (3) |
O1—Ca11iv | 3.00 (2) | 2.83 (2) | 3.17 (3) |
O1—Ca11v | 2.48 (2) | 2.43 (2) | 2.52 (3) |
O1—O21xii | 2.75 (4) | 2.72 (4) | 2.77 (4) |
O1—O21iv | 2.81 (4) | 2.78 (4) | 2.84 (3) |
O1—O31xii | 2.76 (4) | 2.73 (4) | 2.78 (3) |
O1—O31vi | 2.84 (4) | 2.79 (4) | 2.90 (3) |
O2—Ca11v | 2.61 (3) | 2.53 (3) | 2.70 (3) |
O2—O11ix | 2.81 (4) | 2.73 (4) | 2.90 (3) |
O2—O11v | 2.80 (4) | 2.79 (4) | 2.81 (4) |
O2—O21viii | 2.97 (3) | 2.97 (3) | 2.97 (3) |
O2—O21ix | 2.87 (4) | 2.84 (4) | 2.91 (5) |
O2—O21xii | 2.78 (4) | 2.73 (4) | 2.83 (4) |
O2—O21iv | 2.83 (4) | 2.74 (4) | 2.98 (5) |
O2—O21v | 2.74 (4) | 2.74 (5) | 2.74 (4) |
O3—Ca11xix | 2.64 (3) | 2.56 (3) | 2.72 (3) |
O3—O11ix | 2.81 (4) | 2.72 (4) | 2.90 (3) |
O3—O11xix | 2.81 (4) | 2.79 (4) | 2.83 (4) |
O3—O21xx | 2.88 (3) | 2.88 (3) | 2.88 (3) |
O3—O31xxi | 2.89 (4) | 2.86 (4) | 2.93 (5) |
O3—O31xvii | 2.81 (4) | 2.80 (5) | 2.84 (4) |
O3—O31iv | 2.83 (4) | 2.75 (4) | 2.90 (3) |
O3—O31v | 2.74 (4) | 2.71 (5) | 2.77 (4) |
Ca11—O11i | 2.37 (2) | 2.37 (2) | 2.38 (2) |
Ca11—O21 | 2.38 (3) | 2.34 (4) | 2.42 (3) |
Ca11—O21xxii | 2.63 (3) | 2.53 (4) | 2.73 (3) |
Ca11—O31iii | 2.36 (3) | 2.31 (4) | 2.40 (3) |
Ca11—O31xxii | 2.61 (3) | 2.50 (4) | 2.73 (3) |
O11—O21 | 2.81 (4) | 2.74 (4) | 2.88 (5) |
O11—O21xiv | 2.79 (4) | 2.77 (4) | 2.81 (4) |
O11—O31iii | 2.81 (4) | 2.74 (4) | 2.88 (4) |
O11—O31xiv | 2.78 (4) | 2.77 (4) | 2.79 (4) |
Symmetry codes: (i) x1, x2, x3−1, x4; (ii) −x1+1/2, −x2, −x3, −x4; (iii) x1−1, x2, x3, x4; (iv) x1−1/2, x2−1/2, −x3+1/2, x1/2; (v) x1−1/2, x2+1/2, −x3+1/2, x1/2; (vi) x1−3/2, x2−1/2, −x3+1/2, x1/2; (vii) −x1+1/4, −x2+1, x3−1/2, −x1/4; (viii) x1−1/2, x2, x3, x1/2; (ix) −x1+3/4, −x2+1, x3−1/2, −x3/4; (x) −x1+1, −x2, −x3, −x1/2; (xi) −x1+1/2, −x2, −x3+1, −x4; (xii) −x1+3/4, −x2+1, x3+1/2, −x3/4; (xiii) x1, x2+1/2, −x3+1/2, x4; (xiv) −x1+1, −x2+1, −x3+1, −x1/2; (xv) x1+1, x2, x3, x4; (xvi) −x1+3/2, −x2, −x3+1, −x4; (xvii) −x1+7/4, −x2+1, x3+1/2, −x3/4; (xviii) −x1+2, −x2+1, −x3+1, −x1/2; (xix) x1+1/2, x2+1/2, −x3+1/2, x1/2; (xx) x1+1/2, x2, x3, x1/2; (xxi) −x1+7/4, −x2+1, x3−1/2, −x3/4; (xxii) −x1+1, −x2+1, −x3, −x1/2. |
Ca3.429Nb2.606O11.429Ti0.823 | V = 225.17 (2) Å3 |
Mr = 601.8 | Z = 1 |
Monoclinic, ?† | F(000) = 284 |
q = 0.07143b* | Dx = 4.437 Mg m−3 |
a = 7.6805 (3) Å | Mo Kα radiation, λ = 0.71069 Å |
b = 5.3641 (3) Å | µ = 5.77 mm−1 |
c = 5.4653 (1) Å | T = 295 K |
β = 90° | × × mm |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, −x3, 1/2−x4; (3) 1/4−x1, −x2, 1/2+x3, 1/4−x4; (4) x1, 1/2+x2, 1/2−x3, x4; (5) 3/4+x1, 1/2+x2, x3, 1/4+x4; (6) 3/4−x1, 1/2−x2, −x3, 3/4−x4; (7) −x1, 1/2−x2, 1/2+x3, 1/2−x4; (8) 3/4+x1, x2, 1/2−x3, 1/4+x4; (9) 1/2+x1, x2, x3, 1/2+x4; (10) 1/2−x1, −x2, −x3, −x4; (11) 3/4−x1, −x2, 1/2+x3, 3/4−x4; (12) 1/2+x1, 1/2+x2, 1/2−x3, 1/2+x4; (13) 1/4+x1, 1/2+x2, x3, 3/4+x4; (14) 1/4−x1, 1/2−x2, −x3, 1/4−x4; (15) 1/2−x1, 1/2−x2, 1/2+x3, −x4; (16) 1/4+x1, x2, 1/2−x3, 3/4+x4. |
5863 independent reflections | k = ?→? |
5186 reflections with I > 3σ(I) | l = ?→? |
h = ?→? |
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
R[F2 > 2σ(F2)] = 0.058 | (Δ/σ)max = 0.006 |
wR(F2) = 0.067 | Δρmax = 1.62 e Å−3 |
S = 2.59 | Δρmin = −1.31 e Å−3 |
5863 reflections | Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974) |
162 parameters | Extinction coefficient: 0.053181 |
Ca3.429Nb2.606O11.429Ti0.823 | β = 90° |
Mr = 601.8 | V = 225.17 (2) Å3 |
Monoclinic, ?† | Z = 1 |
q = 0.07143b* | Mo Kα radiation |
a = 7.6805 (3) Å | µ = 5.77 mm−1 |
b = 5.3641 (3) Å | T = 295 K |
c = 5.4653 (1) Å | × × mm |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, −x3, 1/2−x4; (3) 1/4−x1, −x2, 1/2+x3, 1/4−x4; (4) x1, 1/2+x2, 1/2−x3, x4; (5) 3/4+x1, 1/2+x2, x3, 1/4+x4; (6) 3/4−x1, 1/2−x2, −x3, 3/4−x4; (7) −x1, 1/2−x2, 1/2+x3, 1/2−x4; (8) 3/4+x1, x2, 1/2−x3, 1/4+x4; (9) 1/2+x1, x2, x3, 1/2+x4; (10) 1/2−x1, −x2, −x3, −x4; (11) 3/4−x1, −x2, 1/2+x3, 3/4−x4; (12) 1/2+x1, 1/2+x2, 1/2−x3, 1/2+x4; (13) 1/4+x1, 1/2+x2, x3, 3/4+x4; (14) 1/4−x1, 1/2−x2, −x3, 1/4−x4; (15) 1/2−x1, 1/2−x2, 1/2+x3, −x4; (16) 1/4+x1, x2, 1/2−x3, 3/4+x4. |
R[F2 > 2σ(F2)] = 0.058 | 162 parameters |
wR(F2) = 0.067 | Δρmax = 1.62 e Å−3 |
S = 2.59 | Δρmin = −1.31 e Å−3 |
5863 reflections |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ca1 | −0.00001 (9) | −0.03449 (14) | 0.00458 (12) | 0.0128 (2) | 0.1429 |
Ca2 | 0.0016 (2) | 0.3320 (2) | −0.0872 (3) | 0.0070 (3) | 0.0357 |
Ca3 | −0.0085 (2) | −0.2496 (3) | 0.0171 (4) | 0.0134 (4) | 0.0357 |
Nb11 | 0.25 | 0 | 0.5 | 0.00746 (13) | 0.032 (6) |
Ti11 | 0.25 | 0 | 0.5 | 0.00746 (13) | 0.040 (6) |
Nb12 | 0.25 | 0 | 0.5 | 0.00746 (13) | 0.127 (14) |
Ti12 | 0.25 | 0 | 0.5 | 0.00746 (13) | 0.016 (14) |
Nb13 | 0.25 | 0 | 0.5 | 0.00746 (13) | 0.071 (6) |
Ti13 | 0.25 | 0 | 0.5 | 0.00746 (13) | 0.001 (6) |
Nb21 | 0.75 | 0 | 0.5 | 0.00710 (13) | 0.034 (6) |
Ti21 | 0.75 | 0 | 0.5 | 0.00710 (13) | 0.038 (6) |
Nb22 | 0.75 | 0 | 0.5 | 0.00710 (13) | 0.129 (14) |
Ti22 | 0.75 | 0 | 0.5 | 0.00710 (13) | 0.013 (14) |
Nb23 | 0.75 | 0 | 0.5 | 0.00710 (13) | 0.071 (14) |
Ti23 | 0.75 | 0 | 0.5 | 0.00710 (13) | 0.000 (14) |
O1 | −0.0002 (2) | 0.0147 (3) | 0.5799 (4) | 0.0093 (5) | 0.2143 |
O2 | 0.2140 (2) | 0.2112 (3) | 0.2056 (3) | 0.0080 (5) | 0.25 |
O3 | 0.7869 (2) | 0.1981 (3) | 0.1964 (3) | 0.0100 (5) | 0.25 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ca1 | 0.0107 (4) | 0.0144 (3) | 0.0133 (4) | −0.0005 (3) | 0.0003 (4) | −0.0028 (3) |
Ca2 | 0.0067 (6) | 0.0084 (6) | 0.0060 (6) | −0.0021 (6) | 0.0003 (7) | 0.0017 (5) |
Ca3 | 0.0078 (6) | 0.0250 (7) | 0.0074 (6) | 0.0027 (7) | −0.0023 (8) | −0.0001 (7) |
Nb11 | 0.0058 (2) | 0.0081 (2) | 0.0086 (2) | −0.0037 (3) | −0.0001 (3) | 0.00002 (15) |
Ti11 | 0.0058 (2) | 0.0081 (2) | 0.0086 (2) | −0.0037 (3) | −0.0001 (3) | 0.00002 (15) |
Nb12 | 0.0058 (2) | 0.0081 (2) | 0.0086 (2) | −0.0037 (3) | −0.0001 (3) | 0.00002 (15) |
Ti12 | 0.0058 (2) | 0.0081 (2) | 0.0086 (2) | −0.0037 (3) | −0.0001 (3) | 0.00002 (15) |
Nb13 | 0.0058 (2) | 0.0081 (2) | 0.0086 (2) | −0.0037 (3) | −0.0001 (3) | 0.00003 (15) |
Ti13 | 0.0058 (2) | 0.0081 (2) | 0.0086 (2) | −0.0037 (3) | −0.0001 (3) | 0.00003 (15) |
Nb21 | 0.0053 (2) | 0.0080 (2) | 0.0080 (2) | −0.0041 (3) | −0.0006 (2) | 0.00040 (15) |
Ti21 | 0.0053 (2) | 0.0080 (2) | 0.0080 (2) | −0.0041 (3) | −0.0006 (2) | 0.00040 (15) |
Nb22 | 0.0053 (2) | 0.0080 (2) | 0.0080 (2) | −0.0041 (3) | −0.0006 (2) | 0.00040 (15) |
Ti22 | 0.0053 (2) | 0.0080 (2) | 0.0080 (2) | −0.0041 (3) | −0.0006 (2) | 0.00040 (15) |
Nb23 | 0.0053 (2) | 0.0080 (2) | 0.0080 (2) | −0.0041 (3) | −0.0006 (2) | 0.00040 (15) |
Ti23 | 0.0053 (2) | 0.0080 (2) | 0.0080 (2) | −0.0041 (3) | −0.0006 (2) | 0.00040 (15) |
O1 | 0.0040 (9) | 0.0117 (9) | 0.0121 (10) | −0.0020 (8) | −0.0001 (7) | 0.0002 (6) |
O2 | 0.0040 (10) | 0.0094 (8) | 0.0106 (8) | −0.0019 (7) | −0.0025 (7) | 0.0001 (6) |
O3 | 0.0099 (11) | 0.0099 (8) | 0.0101 (8) | −0.0010 (7) | −0.0002 (7) | 0.0027 (6) |
Average | Minimum | Maximum | |
Ca1—O1i | 2.36 (6) | 2.34 (4) | 2.38 (7) |
Ca1—O2 | 2.38 (3) | 2.35 (3) | 2.41 (3) |
Ca1—O3ii | 2.37 (3) | 2.35 (3) | 2.40 (3) |
Ca1—O11iii | 2.46 (4) | 2.44 (5) | 2.485 (18) |
Ca1—O11iv | 3.06 (4) | 2.95 (5) | 3.178 (18) |
Ca1—O21v | 2.620 (13) | 2.547 (16) | 2.693 (9) |
Ca1—O21iii | 2.594 (14) | 2.524 (17) | 2.664 (10) |
Ca1—O31v | 2.571 (13) | 2.465 (17) | 2.677 (9) |
Ca1—O31vi | 2.610 (14) | 2.533 (18) | 2.687 (10) |
Ca2—O1i | 2.52 (7) | 2.52 (7) | 2.52 (7) |
Ca2—O2 | 2.36 (3) | 2.36 (3) | 2.36 (3) |
Ca2—O2vii | 2.44 (3) | 2.44 (3) | 2.44 (3) |
Ca2—O2viii | 2.44 (2) | 2.44 (2) | 2.44 (2) |
Ca2—O2ix | 2.45 (3) | 2.45 (3) | 2.45 (3) |
Ca2—O3ii | 2.28 (3) | 2.28 (3) | 2.28 (3) |
Ca2—O3viii | 2.46 (2) | 2.46 (2) | 2.46 (2) |
Nb11—O1 | 1.98 (4) | 1.98 (4) | 1.98 (4) |
Nb11—O2 | 1.92 (3) | 1.92 (3) | 1.92 (3) |
Nb11—O2x | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb11—Nb111xi | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Nb11—Ti111xi | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Nb11—O11xi | 1.96 (2) | 1.96 (2) | 1.96 (2) |
Nb11—O21xi | 2.035 (11) | 2.035 (11) | 2.035 (11) |
Nb11—O21iii | 1.972 (11) | 1.972 (11) | 1.972 (11) |
Ti11—O1 | 1.98 (4) | 1.98 (4) | 1.98 (4) |
Ti11—O2 | 1.92 (3) | 1.92 (3) | 1.92 (3) |
Ti11—O2x | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti11—Nb111xi | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Ti11—Ti111xi | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Ti11—O11xi | 1.96 (2) | 1.96 (2) | 1.96 (2) |
Ti11—O21xi | 2.035 (11) | 2.035 (11) | 2.035 (11) |
Ti11—O21iii | 1.972 (11) | 1.972 (11) | 1.972 (11) |
Nb13—O1 | 2.01 (8) | 2.01 (8) | 2.01 (8) |
Nb13—O2 | 1.83 (3) | 1.83 (3) | 1.83 (3) |
Nb13—O2x | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Nb13—O11xi | 2.00 (8) | 2.00 (8) | 2.00 (8) |
Nb13—O21xi | 2.231 (18) | 2.231 (18) | 2.231 (18) |
Nb13—O21iii | 2.113 (17) | 2.113 (17) | 2.113 (17) |
Ti13—O1 | 2.01 (8) | 2.01 (8) | 2.01 (8) |
Ti13—O2 | 1.83 (3) | 1.83 (3) | 1.83 (3) |
Ti13—O2x | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Ti13—O11xi | 2.00 (8) | 2.00 (8) | 2.00 (8) |
Ti13—O21xi | 2.231 (18) | 2.231 (18) | 2.231 (18) |
Ti13—O21iii | 2.113 (17) | 2.113 (17) | 2.113 (17) |
Nb21—O1xii | 1.97 (4) | 1.97 (4) | 1.97 (4) |
Nb21—O3 | 1.91 (3) | 1.91 (3) | 1.91 (3) |
Nb21—O3xiii | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Nb21—Nb211xiv | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Nb21—Ti211xiv | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Nb21—O11xi | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Nb21—O31xiv | 2.041 (11) | 2.041 (11) | 2.041 (11) |
Nb21—O31iii | 1.982 (11) | 1.982 (11) | 1.982 (11) |
Ti21—O1xii | 1.97 (4) | 1.97 (4) | 1.97 (4) |
Ti21—O3 | 1.91 (3) | 1.91 (3) | 1.91 (3) |
Ti21—O3xiii | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Ti21—Nb211xiv | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Ti21—Ti211xiv | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Ti21—O11xi | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Ti21—O31xiv | 2.041 (11) | 2.041 (11) | 2.041 (11) |
Ti21—O31iii | 1.982 (11) | 1.982 (11) | 1.982 (11) |
Nb23—O1xii | 1.96 (8) | 1.96 (8) | 1.96 (8) |
Nb23—O3 | 1.81 (3) | 1.81 (3) | 1.81 (3) |
Nb23—O3xiii | 1.87 (3) | 1.87 (3) | 1.87 (3) |
Nb23—O11xi | 2.02 (8) | 2.02 (8) | 2.02 (8) |
Nb23—O31xiv | 2.263 (18) | 2.263 (18) | 2.263 (18) |
Nb23—O31iii | 2.162 (18) | 2.162 (18) | 2.162 (18) |
Ti23—O1xii | 1.96 (8) | 1.96 (8) | 1.96 (8) |
Ti23—O3 | 1.81 (3) | 1.81 (3) | 1.81 (3) |
Ti23—O3xiii | 1.87 (3) | 1.87 (3) | 1.87 (3) |
Ti23—O11xi | 2.02 (8) | 2.02 (8) | 2.02 (8) |
Ti23—O31xiv | 2.263 (18) | 2.263 (18) | 2.263 (18) |
Ti23—O31iii | 2.162 (18) | 2.162 (18) | 2.162 (18) |
O1—O2 | 2.83 (7) | 2.75 (8) | 2.96 (8) |
O1—O2x | 2.76 (6) | 2.73 (7) | 2.78 (5) |
O1—O3ii | 2.82 (7) | 2.74 (8) | 2.93 (8) |
O1—O3x | 2.76 (7) | 2.73 (8) | 2.77 (7) |
O1—Ca11iii | 2.97 (4) | 2.82 (6) | 3.11 (3) |
O1—Ca11iv | 2.46 (4) | 2.36 (6) | 2.56 (3) |
O1—Nb111xi | 1.98 (4) | 1.98 (4) | 1.98 (4) |
O1—Ti111xi | 1.98 (4) | 1.98 (4) | 1.98 (4) |
O1—Nb121xi | 2.00 (7) | 2.00 (7) | 2.00 (7) |
O1—Ti121xi | 2.00 (7) | 2.00 (7) | 2.00 (7) |
O1—Nb211xi | 1.97 (4) | 1.97 (4) | 1.97 (4) |
O1—Ti211xi | 1.97 (4) | 1.97 (4) | 1.97 (4) |
O1—Nb221xi | 1.99 (7) | 1.99 (7) | 1.99 (7) |
O1—Ti221xi | 1.99 (7) | 1.99 (7) | 1.99 (7) |
O1—O21xi | 2.80 (6) | 2.77 (7) | 2.83 (8) |
O1—O21iii | 2.82 (6) | 2.79 (7) | 2.83 (4) |
O1—O31xi | 2.78 (6) | 2.71 (7) | 2.83 (8) |
O1—O31vi | 2.82 (6) | 2.81 (7) | 2.83 (4) |
O2—O2vii | 2.96 (3) | 2.96 (3) | 2.96 (3) |
O2—O2xv | 2.96 (3) | 2.96 (3) | 2.96 (3) |
O2—O2viii | 2.81 (4) | 2.72 (4) | 2.85 (4) |
O2—O2x | 2.81 (4) | 2.72 (4) | 2.85 (4) |
O2—O3xvi | 2.87 (4) | 2.87 (4) | 2.87 (4) |
O2—Ca11v | 2.69 (3) | 2.66 (3) | 2.72 (3) |
O2—Ca11iv | 2.67 (3) | 2.62 (3) | 2.72 (3) |
O2—Ca31v | 2.52 (2) | 2.52 (2) | 2.52 (2) |
O2—Ca31iv | 2.39 (3) | 2.39 (3) | 2.39 (3) |
O2—Nb111xi | 1.92 (3) | 1.92 (3) | 1.92 (3) |
O2—Nb111iv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
O2—Ti111xi | 1.92 (3) | 1.92 (3) | 1.92 (3) |
O2—Ti111iv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
O2—Nb121xi | 2.08 (3) | 2.08 (3) | 2.08 (3) |
O2—Nb121iv | 2.17 (3) | 2.17 (3) | 2.17 (3) |
O2—Ti121xi | 2.08 (3) | 2.08 (3) | 2.08 (3) |
O2—Ti121iv | 2.17 (3) | 2.17 (3) | 2.17 (3) |
O2—O11xi | 2.77 (6) | 2.76 (7) | 2.78 (7) |
O2—O11iv | 2.81 (6) | 2.78 (7) | 2.85 (7) |
O2—O21iii | 2.82 (3) | 2.74 (3) | 3.00 (3) |
O2—O21iv | 2.77 (3) | 2.73 (3) | 2.80 (3) |
O3—O3xvii | 2.85 (4) | 2.82 (5) | 2.87 (5) |
O3—O3xiii | 2.85 (4) | 2.82 (5) | 2.87 (5) |
O3—Ca11v | 2.69 (3) | 2.65 (3) | 2.72 (3) |
O3—Ca11xviii | 2.68 (3) | 2.63 (3) | 2.74 (3) |
O3—Ca31xix | 2.41 (3) | 2.41 (3) | 2.41 (3) |
O3—Ca31v | 2.38 (3) | 2.38 (3) | 2.38 (3) |
O3—Ca31xviii | 2.46 (3) | 2.46 (3) | 2.46 (3) |
O3—Nb211xiv | 1.91 (3) | 1.91 (3) | 1.91 (3) |
O3—Nb211iv | 1.97 (3) | 1.97 (3) | 1.97 (3) |
O3—Ti211xiv | 1.91 (3) | 1.91 (3) | 1.91 (3) |
O3—Ti211iv | 1.97 (3) | 1.97 (3) | 1.97 (3) |
O3—Nb221xiv | 2.10 (3) | 2.10 (3) | 2.10 (3) |
O3—Nb221iv | 2.20 (3) | 2.20 (3) | 2.20 (3) |
O3—Ti221xiv | 2.10 (3) | 2.10 (3) | 2.10 (3) |
O3—Ti221iv | 2.20 (3) | 2.20 (3) | 2.20 (3) |
O3—O11xi | 2.78 (6) | 2.75 (7) | 2.80 (7) |
O3—O11xviii | 2.85 (6) | 2.81 (7) | 2.91 (7) |
O3—O31iii | 2.79 (3) | 2.74 (3) | 2.85 (3) |
O3—O31iv | 2.80 (3) | 2.70 (4) | 2.92 (3) |
Ca11—O11xx | 2.35 (5) | 2.33 (7) | 2.38 (2) |
Ca11—O21 | 2.362 (13) | 2.329 (17) | 2.395 (10) |
Ca11—O31xii | 2.359 (14) | 2.332 (17) | 2.387 (10) |
Ca31—O11xx | 2.64 (7) | 2.64 (7) | 2.64 (7) |
Ca31—O31xii | 2.924 (18) | 2.924 (18) | 2.924 (18) |
Nb111—O11 | 1.96 (2) | 1.96 (2) | 1.96 (2) |
Nb111—O21 | 2.035 (11) | 2.035 (11) | 2.035 (11) |
Nb111—O21xxi | 1.972 (11) | 1.972 (11) | 1.972 (11) |
Ti111—O11 | 1.96 (2) | 1.96 (2) | 1.96 (2) |
Ti111—O21 | 2.035 (11) | 2.035 (11) | 2.035 (11) |
Ti111—O21xxi | 1.972 (11) | 1.972 (11) | 1.972 (11) |
Nb121—O11 | 1.97 (7) | 1.97 (7) | 1.97 (7) |
Nb121—O21 | 1.891 (18) | 1.891 (18) | 1.891 (18) |
Nb121—O21xxi | 1.823 (18) | 1.823 (18) | 1.823 (18) |
Ti121—O11 | 1.97 (7) | 1.97 (7) | 1.97 (7) |
Ti121—O21 | 1.891 (18) | 1.891 (18) | 1.891 (18) |
Ti121—O21xxi | 1.823 (18) | 1.823 (18) | 1.823 (18) |
Nb211—O11ii | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Nb211—O31 | 2.041 (11) | 2.041 (11) | 2.041 (11) |
Nb211—O31xxii | 1.982 (11) | 1.982 (11) | 1.982 (11) |
Ti211—O11ii | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Ti211—O31 | 2.041 (11) | 2.041 (11) | 2.041 (11) |
Ti211—O31xxii | 1.982 (11) | 1.982 (11) | 1.982 (11) |
Nb221—O11ii | 2.00 (7) | 2.00 (7) | 2.00 (7) |
Nb221—O31 | 1.873 (18) | 1.873 (18) | 1.873 (18) |
Nb221—O31xxii | 1.848 (18) | 1.848 (18) | 1.848 (18) |
Ti221—O11ii | 2.00 (7) | 2.00 (7) | 2.00 (7) |
Ti221—O31 | 1.873 (18) | 1.873 (18) | 1.873 (18) |
Ti221—O31xxii | 1.848 (18) | 1.848 (18) | 1.848 (18) |
O11—O21 | 2.81 (5) | 2.78 (2) | 2.85 (7) |
O11—O21xxi | 2.78 (5) | 2.73 (2) | 2.86 (7) |
O11—O31xii | 2.83 (5) | 2.77 (7) | 2.90 (7) |
O11—O31xxi | 2.81 (5) | 2.72 (7) | 2.95 (7) |
O21—O21xxi | 2.84 (2) | 2.77 (3) | 2.91 (3) |
O21—O21xxiii | 2.84 (2) | 2.77 (3) | 2.91 (3) |
O31—O31xxii | 2.85 (2) | 2.79 (3) | 2.94 (3) |
O31—O31xxiv | 2.85 (2) | 2.79 (3) | 2.94 (3) |
Symmetry codes: (i) x1, x2, x3−1, x4; (ii) x1−1, x2, x3, x4; (iii) −x1, −x2−1, −x3, −x1/2; (iv) −x1, −x2, −x3, −x1/2; (v) x1+1/2, x2, x3, x1/2; (vi) −x1−1, −x2−1, −x3, −x1/2; (vii) x1−1/4, x2+1/2, x3, x1/4; (viii) −x1+1/2, −x2, −x3−1, −x4; (ix) −x1+1/4, −x2+3/2, −x3−1, −x1/4; (x) −x1+1/2, −x2, −x3, −x4; (xi) x1+1/2, x2, x3+1, x1/2; (xii) x1+1, x2, x3, x4; (xiii) −x1+3/2, −x2, −x3, −x4; (xiv) x1+3/2, x2, x3+1, x1/2; (xv) x1+1/4, x2−1/2, x3, x3/4; (xvi) x1−3/4, x2−1/2, x3, x3/4; (xvii) −x1+3/2, −x2, −x3−1, −x4; (xviii) −x1+1, −x2, −x3, −x1/2; (xix) x1+3/4, x2−1/2, x3, x1/4; (xx) x1, x2, x3+1, x4; (xxi) −x1−1/2, −x2−1, −x3−1, −x4; (xxii) −x1−3/2, −x2−1, −x3−1, −x4; (xxiii) −x1−1/2, −x2−1, −x3, −x4; (xxiv) −x1−3/2, −x2−1, −x3, −x4. |
Experimental details
(Ca5_Nb4_Ti_O17) | (Ca6_Nb,Ti6_O20) | |
Crystal data | ||
Chemical formula | Ca3.333Nb2.666O11.333Ti0.667 | Ca3.429Nb2.606O11.429Ti0.823 |
Mr | 594.5 | 601.8 |
Crystal system, space group | Monoclinic, ?† | Monoclinic, ?‡ |
Temperature (K) | 295 | 295 |
Wave vectors | q = 0.08333b* | q = 0.07143b* |
a, b, c (Å) | 7.6889 (3), 5.3381 (3), 5.4763 (1) | 7.6805 (3), 5.3641 (3), 5.4653 (1) |
γ (°) | 89.921 (4) | 90.036 (4) |
V (Å3) | 224.77 (2) | 225.17 (2) |
Z | 1 | 1 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 5.87 | 5.77 |
Crystal size (mm) | × × | × × |
Data collection | ||
Diffractometer | ? | ? |
Absorption correction | – | – |
No. of measured, independent and observed [I > 3σ(I)] reflections | ?, 3231, 2731 | ?, 5863, 5186 |
Rint | ? | ? |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.051, 0.061, 2.63 | 0.058, 0.067, 2.59 |
No. of reflections | 3231 | 5863 |
No. of parameters | 146 | 162 |
No. of restraints | ? | ? |
Δρmax, Δρmin (e Å−3) | 3.02, −2.65 | 1.62, −1.31 |
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, −x3, 1/2−x4; (3) 1/4−x1, −x2, 1/2+x3, 1/4−x4; (4) x1, 1/2+x2, 1/2−x3, x4; (5) 1/2+x1, x2, x3, 1/2+x4; (6) 1/2−x1, −x2, −x3, −x4; (7) 3/4−x1, −x2, 1/2+x3, 3/4−x4; (8) 1/2+x1, 1/2+x2, 1/2−x3, 1/2+x4; (9) 3/4+x1, 1/2+x2, x3, 1/4+x4; (10) 3/4−x1, 1/2−x2, −x3, 3/4−x4; (11) −x1, 1/2−x2, 1/2+x3, 1/2−x4; (12) 3/4+x1, x2, 1/2−x3, 1/4+x4; (13) 1/4+x1, 1/2+x2, x3, 3/4+x4; (14) 1/4−x1, 1/2−x2, −x3, 1/4−x4; (15) 1/2−x1, 1/2−x2, 1/2+x3, −x4; (16) 1/4+x1, x2, 1/2−x3, 3/4+x4.
‡ Symmetry operations: (1) x1, x2, x3, x4; (2) −x1, −x2, −x3, 1/2−x4; (3) 1/4−x1, −x2, 1/2+x3, 1/4−x4; (4) x1, 1/2+x2, 1/2−x3, x4; (5) 3/4+x1, 1/2+x2, x3, 1/4+x4; (6) 3/4−x1, 1/2−x2, −x3, 3/4−x4; (7) −x1, 1/2−x2, 1/2+x3, 1/2−x4; (8) 3/4+x1, x2, 1/2−x3, 1/4+x4; (9) 1/2+x1, x2, x3, 1/2+x4; (10) 1/2−x1, −x2, −x3, −x4; (11) 3/4−x1, −x2, 1/2+x3, 3/4−x4; (12) 1/2+x1, 1/2+x2, 1/2−x3, 1/2+x4; (13) 1/4+x1, 1/2+x2, x3, 3/4+x4; (14) 1/4−x1, 1/2−x2, −x3, 1/4−x4; (15) 1/2−x1, 1/2−x2, 1/2+x3, −x4; (16) 1/4+x1, x2, 1/2−x3, 3/4+x4.
Computer programs: (Jana2000; Petricek and Dusek, 2000).
Average | Minimum | Maximum | |
Ca1—O1i | 2.36 (3) | 2.36 (3) | 2.36 (3) |
Ca1—O2 | 2.37 (3) | 2.37 (3) | 2.37 (3) |
Ca1—O2ii | 2.68 (3) | 2.68 (3) | 2.68 (3) |
Ca1—O3iii | 2.36 (3) | 2.36 (3) | 2.36 (3) |
Ca1—O3ii | 2.66 (3) | 2.66 (3) | 2.66 (3) |
Ca1—O11iv | 2.38 (2) | 2.38 (2) | 2.38 (2) |
Ca1—O11v | 2.97 (2) | 2.97 (2) | 2.97 (2) |
Ca1—O21iv | 2.64 (3) | 2.64 (3) | 2.64 (3) |
Ca1—O31vi | 2.65 (3) | 2.65 (3) | 2.65 (3) |
Ca2—O1i | 2.54 (2) | 2.54 (2) | 2.54 (2) |
Ca2—O2 | 2.36 (3) | 2.36 (3) | 2.36 (3) |
Ca2—O2vii | 2.46 (3) | 2.46 (3) | 2.46 (3) |
Ca2—O3iii | 2.31 (3) | 2.31 (3) | 2.31 (3) |
Ca2—O21viii | 2.45 (2) | 2.45 (2) | 2.45 (2) |
Ca2—O21ix | 2.444 (18) | 2.444 (18) | 2.444 (18) |
Ca2—O31ix | 2.470 (17) | 2.470 (17) | 2.470 (17) |
Ca3—O1i | 2.65 (2) | 2.65 (2) | 2.65 (2) |
Ca3—O2ii | 2.50 (3) | 2.50 (3) | 2.50 (3) |
Ca3—O3iii | 2.95 (3) | 2.95 (3) | 2.95 (3) |
Ca3—O3ii | 2.39 (3) | 2.39 (3) | 2.39 (3) |
Ca3—O21iv | 2.384 (19) | 2.384 (19) | 2.384 (19) |
Ca3—O31x | 2.428 (18) | 2.428 (18) | 2.428 (18) |
Ca3—O31vi | 2.446 (18) | 2.446 (18) | 2.446 (18) |
Nb11—O1 | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Nb11—O1xi | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Nb11—O2 | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Nb11—O2xi | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Nb11—O21xii | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb11—O21iv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti11—O1 | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Ti11—O1xi | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Ti11—O2 | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Ti11—O2xi | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Ti11—O21xii | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti11—O21iv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb12—O2xii | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Nb12—O2xiii | 2.16 (3) | 2.16 (3) | 2.16 (3) |
Nb12—O11 | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb12—O11xiv | 2.00 (3) | 2.00 (3) | 2.00 (3) |
Nb12—O21 | 1.90 (4) | 1.90 (4) | 1.90 (4) |
Nb12—O21xiv | 2.08 (3) | 2.08 (3) | 2.08 (3) |
Ti12—O2xii | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Ti12—O2xiii | 2.16 (3) | 2.16 (3) | 2.16 (3) |
Ti12—O11 | 1.98 (2) | 1.98 (2) | 1.98 (2) |
Ti12—O11xiv | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Ti12—O21 | 1.90 (4) | 1.90 (4) | 1.90 (4) |
Ti12—O21xiv | 2.08 (3) | 2.08 (3) | 2.08 (3) |
Nb13—O1 | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Nb13—O1xi | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Nb13—O2 | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Nb13—O2xi | 2.23 (3) | 2.23 (3) | 2.23 (3) |
Nb13—O21xii | 1.83 (2) | 1.83 (2) | 1.83 (2) |
Nb13—O21iv | 2.11 (4) | 2.11 (4) | 2.11 (4) |
Ti13—O1 | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Ti13—O1xi | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Ti13—O2 | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Ti13—O2xi | 2.23 (3) | 2.23 (3) | 2.23 (3) |
Ti13—O21xii | 1.83 (2) | 1.83 (2) | 1.83 (2) |
Ti13—O21iv | 2.11 (4) | 2.11 (4) | 2.11 (4) |
Nb21—O1xv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb21—O1xi | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb21—O3 | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Nb21—O3xvi | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Nb21—O31xvii | 1.99 (3) | 1.99 (3) | 1.99 (3) |
Nb21—O31iv | 1.99 (3) | 1.99 (3) | 1.99 (3) |
Ti21—O1xv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti21—O1xi | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti21—O3 | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Ti21—O3xvi | 1.96 (3) | 1.96 (3) | 1.96 (3) |
Ti21—O31xvii | 1.99 (3) | 1.99 (3) | 1.99 (3) |
Ti21—O31iv | 1.99 (3) | 1.99 (3) | 1.99 (3) |
Nb22—O3xvii | 1.85 (3) | 1.85 (3) | 1.85 (3) |
Nb22—O3xiii | 2.17 (3) | 2.17 (3) | 2.17 (3) |
Nb22—O11xv | 1.97 (2) | 1.97 (2) | 1.97 (2) |
Nb22—O11xiv | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Nb22—O31 | 1.90 (4) | 1.90 (4) | 1.90 (4) |
Nb22—O31xviii | 2.09 (3) | 2.09 (3) | 2.09 (3) |
Ti22—O3xvii | 1.85 (3) | 1.85 (3) | 1.85 (3) |
Ti22—O3xiii | 2.17 (3) | 2.17 (3) | 2.17 (3) |
Ti22—O11xv | 1.97 (2) | 1.97 (2) | 1.97 (2) |
Ti22—O11xiv | 2.00 (2) | 2.00 (2) | 2.00 (2) |
Ti22—O31 | 1.90 (4) | 1.90 (4) | 1.90 (4) |
Ti22—O31xviii | 2.09 (3) | 2.09 (3) | 2.09 (3) |
Nb23—O1xv | 1.98 (2) | 1.98 (2) | 1.98 (2) |
Nb23—O1xi | 2.02 (2) | 2.02 (2) | 2.02 (2) |
Nb23—O3 | 1.79 (3) | 1.79 (3) | 1.79 (3) |
Nb23—O3xvi | 2.26 (3) | 2.26 (3) | 2.26 (3) |
Nb23—O31xvii | 1.850 (18) | 1.850 (18) | 1.850 (18) |
Nb23—O31iv | 2.15 (4) | 2.15 (4) | 2.15 (4) |
Ti23—O1xv | 1.98 (2) | 1.98 (2) | 1.98 (2) |
Ti23—O1xi | 2.02 (2) | 2.02 (2) | 2.02 (2) |
Ti23—O3 | 1.79 (3) | 1.79 (3) | 1.79 (3) |
Ti23—O3xvi | 2.26 (3) | 2.26 (3) | 2.26 (3) |
Ti23—O31xvii | 1.850 (18) | 1.850 (18) | 1.850 (18) |
Ti23—O31iv | 2.15 (4) | 2.15 (4) | 2.15 (4) |
O1—O2 | 2.84 (4) | 2.77 (4) | 2.96 (4) |
O1—O2xi | 2.79 (4) | 2.75 (3) | 2.83 (3) |
O1—O3iii | 2.83 (4) | 2.78 (4) | 2.92 (4) |
O1—O3xi | 2.79 (4) | 2.74 (4) | 2.84 (3) |
O1—Ca11iv | 3.00 (2) | 2.83 (2) | 3.17 (3) |
O1—Ca11v | 2.48 (2) | 2.43 (2) | 2.52 (3) |
O1—O21xii | 2.75 (4) | 2.72 (4) | 2.77 (4) |
O1—O21iv | 2.81 (4) | 2.78 (4) | 2.84 (3) |
O1—O31xii | 2.76 (4) | 2.73 (4) | 2.78 (3) |
O1—O31vi | 2.84 (4) | 2.79 (4) | 2.90 (3) |
O2—Ca11v | 2.61 (3) | 2.53 (3) | 2.70 (3) |
O2—O11ix | 2.81 (4) | 2.73 (4) | 2.90 (3) |
O2—O11v | 2.80 (4) | 2.79 (4) | 2.81 (4) |
O2—O21viii | 2.97 (3) | 2.97 (3) | 2.97 (3) |
O2—O21ix | 2.87 (4) | 2.84 (4) | 2.91 (5) |
O2—O21xii | 2.78 (4) | 2.73 (4) | 2.83 (4) |
O2—O21iv | 2.83 (4) | 2.74 (4) | 2.98 (5) |
O2—O21v | 2.74 (4) | 2.74 (5) | 2.74 (4) |
O3—Ca11xix | 2.64 (3) | 2.56 (3) | 2.72 (3) |
O3—O11ix | 2.81 (4) | 2.72 (4) | 2.90 (3) |
O3—O11xix | 2.81 (4) | 2.79 (4) | 2.83 (4) |
O3—O21xx | 2.88 (3) | 2.88 (3) | 2.88 (3) |
O3—O31xxi | 2.89 (4) | 2.86 (4) | 2.93 (5) |
O3—O31xvii | 2.81 (4) | 2.80 (5) | 2.84 (4) |
O3—O31iv | 2.83 (4) | 2.75 (4) | 2.90 (3) |
O3—O31v | 2.74 (4) | 2.71 (5) | 2.77 (4) |
Ca11—O11i | 2.37 (2) | 2.37 (2) | 2.38 (2) |
Ca11—O21 | 2.38 (3) | 2.34 (4) | 2.42 (3) |
Ca11—O21xxii | 2.63 (3) | 2.53 (4) | 2.73 (3) |
Ca11—O31iii | 2.36 (3) | 2.31 (4) | 2.40 (3) |
Ca11—O31xxii | 2.61 (3) | 2.50 (4) | 2.73 (3) |
O11—O21 | 2.81 (4) | 2.74 (4) | 2.88 (5) |
O11—O21xiv | 2.79 (4) | 2.77 (4) | 2.81 (4) |
O11—O31iii | 2.81 (4) | 2.74 (4) | 2.88 (4) |
O11—O31xiv | 2.78 (4) | 2.77 (4) | 2.79 (4) |
Symmetry codes: (i) x1, x2, x3−1, x4; (ii) −x1+1/2, −x2, −x3, −x4; (iii) x1−1, x2, x3, x4; (iv) x1−1/2, x2−1/2, −x3+1/2, x1/2; (v) x1−1/2, x2+1/2, −x3+1/2, x1/2; (vi) x1−3/2, x2−1/2, −x3+1/2, x1/2; (vii) −x1+1/4, −x2+1, x3−1/2, −x1/4; (viii) x1−1/2, x2, x3, x1/2; (ix) −x1+3/4, −x2+1, x3−1/2, −x3/4; (x) −x1+1, −x2, −x3, −x1/2; (xi) −x1+1/2, −x2, −x3+1, −x4; (xii) −x1+3/4, −x2+1, x3+1/2, −x3/4; (xiii) x1, x2+1/2, −x3+1/2, x4; (xiv) −x1+1, −x2+1, −x3+1, −x1/2; (xv) x1+1, x2, x3, x4; (xvi) −x1+3/2, −x2, −x3+1, −x4; (xvii) −x1+7/4, −x2+1, x3+1/2, −x3/4; (xviii) −x1+2, −x2+1, −x3+1, −x1/2; (xix) x1+1/2, x2+1/2, −x3+1/2, x1/2; (xx) x1+1/2, x2, x3, x1/2; (xxi) −x1+7/4, −x2+1, x3−1/2, −x3/4; (xxii) −x1+1, −x2+1, −x3, −x1/2. |
Average | Minimum | Maximum | |
Ca1—O1i | 2.36 (6) | 2.34 (4) | 2.38 (7) |
Ca1—O2 | 2.38 (3) | 2.35 (3) | 2.41 (3) |
Ca1—O3ii | 2.37 (3) | 2.35 (3) | 2.40 (3) |
Ca1—O11iii | 2.46 (4) | 2.44 (5) | 2.485 (18) |
Ca1—O11iv | 3.06 (4) | 2.95 (5) | 3.178 (18) |
Ca1—O21v | 2.620 (13) | 2.547 (16) | 2.693 (9) |
Ca1—O21iii | 2.594 (14) | 2.524 (17) | 2.664 (10) |
Ca1—O31v | 2.571 (13) | 2.465 (17) | 2.677 (9) |
Ca1—O31vi | 2.610 (14) | 2.533 (18) | 2.687 (10) |
Ca2—O1i | 2.52 (7) | 2.52 (7) | 2.52 (7) |
Ca2—O2 | 2.36 (3) | 2.36 (3) | 2.36 (3) |
Ca2—O2vii | 2.44 (3) | 2.44 (3) | 2.44 (3) |
Ca2—O2viii | 2.44 (2) | 2.44 (2) | 2.44 (2) |
Ca2—O2ix | 2.45 (3) | 2.45 (3) | 2.45 (3) |
Ca2—O3ii | 2.28 (3) | 2.28 (3) | 2.28 (3) |
Ca2—O3viii | 2.46 (2) | 2.46 (2) | 2.46 (2) |
Nb11—O1 | 1.98 (4) | 1.98 (4) | 1.98 (4) |
Nb11—O2 | 1.92 (3) | 1.92 (3) | 1.92 (3) |
Nb11—O2x | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Nb11—Nb111xi | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Nb11—Ti111xi | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Nb11—O11xi | 1.96 (2) | 1.96 (2) | 1.96 (2) |
Nb11—O21xi | 2.035 (11) | 2.035 (11) | 2.035 (11) |
Nb11—O21iii | 1.972 (11) | 1.972 (11) | 1.972 (11) |
Ti11—O1 | 1.98 (4) | 1.98 (4) | 1.98 (4) |
Ti11—O2 | 1.92 (3) | 1.92 (3) | 1.92 (3) |
Ti11—O2x | 1.98 (3) | 1.98 (3) | 1.98 (3) |
Ti11—Nb111xi | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Ti11—Ti111xi | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Ti11—O11xi | 1.96 (2) | 1.96 (2) | 1.96 (2) |
Ti11—O21xi | 2.035 (11) | 2.035 (11) | 2.035 (11) |
Ti11—O21iii | 1.972 (11) | 1.972 (11) | 1.972 (11) |
Nb13—O1 | 2.01 (8) | 2.01 (8) | 2.01 (8) |
Nb13—O2 | 1.83 (3) | 1.83 (3) | 1.83 (3) |
Nb13—O2x | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Nb13—O11xi | 2.00 (8) | 2.00 (8) | 2.00 (8) |
Nb13—O21xi | 2.231 (18) | 2.231 (18) | 2.231 (18) |
Nb13—O21iii | 2.113 (17) | 2.113 (17) | 2.113 (17) |
Ti13—O1 | 2.01 (8) | 2.01 (8) | 2.01 (8) |
Ti13—O2 | 1.83 (3) | 1.83 (3) | 1.83 (3) |
Ti13—O2x | 1.84 (3) | 1.84 (3) | 1.84 (3) |
Ti13—O11xi | 2.00 (8) | 2.00 (8) | 2.00 (8) |
Ti13—O21xi | 2.231 (18) | 2.231 (18) | 2.231 (18) |
Ti13—O21iii | 2.113 (17) | 2.113 (17) | 2.113 (17) |
Nb21—O1xii | 1.97 (4) | 1.97 (4) | 1.97 (4) |
Nb21—O3 | 1.91 (3) | 1.91 (3) | 1.91 (3) |
Nb21—O3xiii | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Nb21—Nb211xiv | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Nb21—Ti211xiv | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Nb21—O11xi | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Nb21—O31xiv | 2.041 (11) | 2.041 (11) | 2.041 (11) |
Nb21—O31iii | 1.982 (11) | 1.982 (11) | 1.982 (11) |
Ti21—O1xii | 1.97 (4) | 1.97 (4) | 1.97 (4) |
Ti21—O3 | 1.91 (3) | 1.91 (3) | 1.91 (3) |
Ti21—O3xiii | 1.97 (3) | 1.97 (3) | 1.97 (3) |
Ti21—Nb211xiv | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Ti21—Ti211xiv | 0.0000 (12) | 0.0000 (12) | 0.0000 (12) |
Ti21—O11xi | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Ti21—O31xiv | 2.041 (11) | 2.041 (11) | 2.041 (11) |
Ti21—O31iii | 1.982 (11) | 1.982 (11) | 1.982 (11) |
Nb23—O1xii | 1.96 (8) | 1.96 (8) | 1.96 (8) |
Nb23—O3 | 1.81 (3) | 1.81 (3) | 1.81 (3) |
Nb23—O3xiii | 1.87 (3) | 1.87 (3) | 1.87 (3) |
Nb23—O11xi | 2.02 (8) | 2.02 (8) | 2.02 (8) |
Nb23—O31xiv | 2.263 (18) | 2.263 (18) | 2.263 (18) |
Nb23—O31iii | 2.162 (18) | 2.162 (18) | 2.162 (18) |
Ti23—O1xii | 1.96 (8) | 1.96 (8) | 1.96 (8) |
Ti23—O3 | 1.81 (3) | 1.81 (3) | 1.81 (3) |
Ti23—O3xiii | 1.87 (3) | 1.87 (3) | 1.87 (3) |
Ti23—O11xi | 2.02 (8) | 2.02 (8) | 2.02 (8) |
Ti23—O31xiv | 2.263 (18) | 2.263 (18) | 2.263 (18) |
Ti23—O31iii | 2.162 (18) | 2.162 (18) | 2.162 (18) |
O1—O2 | 2.83 (7) | 2.75 (8) | 2.96 (8) |
O1—O2x | 2.76 (6) | 2.73 (7) | 2.78 (5) |
O1—O3ii | 2.82 (7) | 2.74 (8) | 2.93 (8) |
O1—O3x | 2.76 (7) | 2.73 (8) | 2.77 (7) |
O1—Ca11iii | 2.97 (4) | 2.82 (6) | 3.11 (3) |
O1—Ca11iv | 2.46 (4) | 2.36 (6) | 2.56 (3) |
O1—Nb111xi | 1.98 (4) | 1.98 (4) | 1.98 (4) |
O1—Ti111xi | 1.98 (4) | 1.98 (4) | 1.98 (4) |
O1—Nb121xi | 2.00 (7) | 2.00 (7) | 2.00 (7) |
O1—Ti121xi | 2.00 (7) | 2.00 (7) | 2.00 (7) |
O1—Nb211xi | 1.97 (4) | 1.97 (4) | 1.97 (4) |
O1—Ti211xi | 1.97 (4) | 1.97 (4) | 1.97 (4) |
O1—Nb221xi | 1.99 (7) | 1.99 (7) | 1.99 (7) |
O1—Ti221xi | 1.99 (7) | 1.99 (7) | 1.99 (7) |
O1—O21xi | 2.80 (6) | 2.77 (7) | 2.83 (8) |
O1—O21iii | 2.82 (6) | 2.79 (7) | 2.83 (4) |
O1—O31xi | 2.78 (6) | 2.71 (7) | 2.83 (8) |
O1—O31vi | 2.82 (6) | 2.81 (7) | 2.83 (4) |
O2—O2vii | 2.96 (3) | 2.96 (3) | 2.96 (3) |
O2—O2xv | 2.96 (3) | 2.96 (3) | 2.96 (3) |
O2—O2viii | 2.81 (4) | 2.72 (4) | 2.85 (4) |
O2—O2x | 2.81 (4) | 2.72 (4) | 2.85 (4) |
O2—O3xvi | 2.87 (4) | 2.87 (4) | 2.87 (4) |
O2—Ca11v | 2.69 (3) | 2.66 (3) | 2.72 (3) |
O2—Ca11iv | 2.67 (3) | 2.62 (3) | 2.72 (3) |
O2—Ca31v | 2.52 (2) | 2.52 (2) | 2.52 (2) |
O2—Ca31iv | 2.39 (3) | 2.39 (3) | 2.39 (3) |
O2—Nb111xi | 1.92 (3) | 1.92 (3) | 1.92 (3) |
O2—Nb111iv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
O2—Ti111xi | 1.92 (3) | 1.92 (3) | 1.92 (3) |
O2—Ti111iv | 1.98 (3) | 1.98 (3) | 1.98 (3) |
O2—Nb121xi | 2.08 (3) | 2.08 (3) | 2.08 (3) |
O2—Nb121iv | 2.17 (3) | 2.17 (3) | 2.17 (3) |
O2—Ti121xi | 2.08 (3) | 2.08 (3) | 2.08 (3) |
O2—Ti121iv | 2.17 (3) | 2.17 (3) | 2.17 (3) |
O2—O11xi | 2.77 (6) | 2.76 (7) | 2.78 (7) |
O2—O11iv | 2.81 (6) | 2.78 (7) | 2.85 (7) |
O2—O21iii | 2.82 (3) | 2.74 (3) | 3.00 (3) |
O2—O21iv | 2.77 (3) | 2.73 (3) | 2.80 (3) |
O3—O3xvii | 2.85 (4) | 2.82 (5) | 2.87 (5) |
O3—O3xiii | 2.85 (4) | 2.82 (5) | 2.87 (5) |
O3—Ca11v | 2.69 (3) | 2.65 (3) | 2.72 (3) |
O3—Ca11xviii | 2.68 (3) | 2.63 (3) | 2.74 (3) |
O3—Ca31xix | 2.41 (3) | 2.41 (3) | 2.41 (3) |
O3—Ca31v | 2.38 (3) | 2.38 (3) | 2.38 (3) |
O3—Ca31xviii | 2.46 (3) | 2.46 (3) | 2.46 (3) |
O3—Nb211xiv | 1.91 (3) | 1.91 (3) | 1.91 (3) |
O3—Nb211iv | 1.97 (3) | 1.97 (3) | 1.97 (3) |
O3—Ti211xiv | 1.91 (3) | 1.91 (3) | 1.91 (3) |
O3—Ti211iv | 1.97 (3) | 1.97 (3) | 1.97 (3) |
O3—Nb221xiv | 2.10 (3) | 2.10 (3) | 2.10 (3) |
O3—Nb221iv | 2.20 (3) | 2.20 (3) | 2.20 (3) |
O3—Ti221xiv | 2.10 (3) | 2.10 (3) | 2.10 (3) |
O3—Ti221iv | 2.20 (3) | 2.20 (3) | 2.20 (3) |
O3—O11xi | 2.78 (6) | 2.75 (7) | 2.80 (7) |
O3—O11xviii | 2.85 (6) | 2.81 (7) | 2.91 (7) |
O3—O31iii | 2.79 (3) | 2.74 (3) | 2.85 (3) |
O3—O31iv | 2.80 (3) | 2.70 (4) | 2.92 (3) |
Ca11—O11xx | 2.35 (5) | 2.33 (7) | 2.38 (2) |
Ca11—O21 | 2.362 (13) | 2.329 (17) | 2.395 (10) |
Ca11—O31xii | 2.359 (14) | 2.332 (17) | 2.387 (10) |
Ca31—O11xx | 2.64 (7) | 2.64 (7) | 2.64 (7) |
Ca31—O31xii | 2.924 (18) | 2.924 (18) | 2.924 (18) |
Nb111—O11 | 1.96 (2) | 1.96 (2) | 1.96 (2) |
Nb111—O21 | 2.035 (11) | 2.035 (11) | 2.035 (11) |
Nb111—O21xxi | 1.972 (11) | 1.972 (11) | 1.972 (11) |
Ti111—O11 | 1.96 (2) | 1.96 (2) | 1.96 (2) |
Ti111—O21 | 2.035 (11) | 2.035 (11) | 2.035 (11) |
Ti111—O21xxi | 1.972 (11) | 1.972 (11) | 1.972 (11) |
Nb121—O11 | 1.97 (7) | 1.97 (7) | 1.97 (7) |
Nb121—O21 | 1.891 (18) | 1.891 (18) | 1.891 (18) |
Nb121—O21xxi | 1.823 (18) | 1.823 (18) | 1.823 (18) |
Ti121—O11 | 1.97 (7) | 1.97 (7) | 1.97 (7) |
Ti121—O21 | 1.891 (18) | 1.891 (18) | 1.891 (18) |
Ti121—O21xxi | 1.823 (18) | 1.823 (18) | 1.823 (18) |
Nb211—O11ii | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Nb211—O31 | 2.041 (11) | 2.041 (11) | 2.041 (11) |
Nb211—O31xxii | 1.982 (11) | 1.982 (11) | 1.982 (11) |
Ti211—O11ii | 1.99 (2) | 1.99 (2) | 1.99 (2) |
Ti211—O31 | 2.041 (11) | 2.041 (11) | 2.041 (11) |
Ti211—O31xxii | 1.982 (11) | 1.982 (11) | 1.982 (11) |
Nb221—O11ii | 2.00 (7) | 2.00 (7) | 2.00 (7) |
Nb221—O31 | 1.873 (18) | 1.873 (18) | 1.873 (18) |
Nb221—O31xxii | 1.848 (18) | 1.848 (18) | 1.848 (18) |
Ti221—O11ii | 2.00 (7) | 2.00 (7) | 2.00 (7) |
Ti221—O31 | 1.873 (18) | 1.873 (18) | 1.873 (18) |
Ti221—O31xxii | 1.848 (18) | 1.848 (18) | 1.848 (18) |
O11—O21 | 2.81 (5) | 2.78 (2) | 2.85 (7) |
O11—O21xxi | 2.78 (5) | 2.73 (2) | 2.86 (7) |
O11—O31xii | 2.83 (5) | 2.77 (7) | 2.90 (7) |
O11—O31xxi | 2.81 (5) | 2.72 (7) | 2.95 (7) |
O21—O21xxi | 2.84 (2) | 2.77 (3) | 2.91 (3) |
O21—O21xxiii | 2.84 (2) | 2.77 (3) | 2.91 (3) |
O31—O31xxii | 2.85 (2) | 2.79 (3) | 2.94 (3) |
O31—O31xxiv | 2.85 (2) | 2.79 (3) | 2.94 (3) |
Symmetry codes: (i) x1, x2, x3−1, x4; (ii) x1−1, x2, x3, x4; (iii) −x1, −x2−1, −x3, −x1/2; (iv) −x1, −x2, −x3, −x1/2; (v) x1+1/2, x2, x3, x1/2; (vi) −x1−1, −x2−1, −x3, −x1/2; (vii) x1−1/4, x2+1/2, x3, x1/4; (viii) −x1+1/2, −x2, −x3−1, −x4; (ix) −x1+1/4, −x2+3/2, −x3−1, −x1/4; (x) −x1+1/2, −x2, −x3, −x4; (xi) x1+1/2, x2, x3+1, x1/2; (xii) x1+1, x2, x3, x4; (xiii) −x1+3/2, −x2, −x3, −x4; (xiv) x1+3/2, x2, x3+1, x1/2; (xv) x1+1/4, x2−1/2, x3, x3/4; (xvi) x1−3/4, x2−1/2, x3, x3/4; (xvii) −x1+3/2, −x2, −x3−1, −x4; (xviii) −x1+1, −x2, −x3, −x1/2; (xix) x1+3/4, x2−1/2, x3, x1/4; (xx) x1, x2, x3+1, x4; (xxi) −x1−1/2, −x2−1, −x3−1, −x4; (xxii) −x1−3/2, −x2−1, −x3−1, −x4; (xxiii) −x1−1/2, −x2−1, −x3, −x4; (xxiv) −x1−3/2, −x2−1, −x3, −x4. |
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