Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024024/br6122sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024024/br6122Isup2.hkl |
Data collection: COLLECT (Nonius, 1999); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2000); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) and local procedures.
NaRb3(VO3)4(H2O) | F(000) = 1280 |
Mr = 693.18 | Dx = 3.140 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 2407 reflections |
a = 11.1610 (5) Å | θ = 2.9–33.1° |
b = 8.3050 (11) Å | µ = 12.45 mm−1 |
c = 15.8180 (8) Å | T = 150 K |
V = 1466.2 (2) Å3 | Prism, light yellow |
Z = 4 | 0.14 × 0.13 × 0.10 mm |
Nonius KappaCCD diffractometer | 2271 independent reflections |
Radiation source: fine-focus sealed tube, KappaCCD | 2175 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.083 |
φ and ω scans | θmax = 30.0°, θmin = 3.2° |
Absorption correction: multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997) | h = −15→15 |
Tmin = 0.203, Tmax = 0.288 | k = −11→11 |
24175 measured reflections | l = −22→22 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.034 | w = 1/[σ2(Fo2) + (0.0136P)2 + 4.7048P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.077 | (Δ/σ)max = 0.001 |
S = 1.14 | Δρmax = 1.09 e Å−3 |
2271 reflections | Δρmin = −1.87 e Å−3 |
107 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0036 (5) |
Primary atom site location: structure-invariant direct methods |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Rb1 | 0.52769 (4) | 0.7500 | 0.89948 (3) | 0.02539 (14) | |
Rb2 | 0.48559 (4) | 0.7500 | 0.62101 (3) | 0.01808 (12) | |
Rb3 | 0.48232 (5) | 0.2500 | 0.69433 (4) | 0.02690 (14) | |
V1 | 0.71486 (4) | 0.45993 (6) | 0.52643 (3) | 0.01183 (13) | |
V2 | 0.74207 (5) | 0.54938 (7) | 0.73235 (3) | 0.01450 (14) | |
Na | 0.68488 (18) | 0.2500 | 0.91556 (11) | 0.0189 (4) | |
O1 | 0.8537 (2) | 0.5234 (3) | 0.51424 (14) | 0.0216 (5) | |
O2 | 0.7038 (3) | −0.7500 | 0.4986 (2) | 0.0218 (7) | |
O3 | 0.6281 (2) | 0.5647 (3) | 0.46424 (15) | 0.0218 (5) | |
O4 | 0.6691 (2) | 0.4897 (3) | 0.63472 (13) | 0.0203 (5) | |
O5 | 0.8889 (2) | 0.5460 (3) | 0.72709 (16) | 0.0260 (6) | |
O6 | 0.6904 (3) | 0.7500 | 0.7572 (2) | 0.0227 (7) | |
O7 | 0.6958 (3) | 0.4309 (4) | 0.80725 (17) | 0.0349 (7) | |
Ow | 0.4771 (3) | 0.2500 | 0.8920 (2) | 0.0251 (8) | |
H8 | 0.4333 | 0.3413 | 0.9146 | 0.030* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rb1 | 0.0199 (2) | 0.0300 (3) | 0.0263 (3) | 0.000 | 0.00265 (17) | 0.000 |
Rb2 | 0.0153 (2) | 0.0185 (2) | 0.0205 (2) | 0.000 | −0.00518 (15) | 0.000 |
Rb3 | 0.0239 (3) | 0.0157 (2) | 0.0411 (3) | 0.000 | 0.00626 (19) | 0.000 |
V1 | 0.0129 (2) | 0.0109 (3) | 0.0117 (2) | −0.00049 (17) | 0.00012 (17) | 0.00071 (18) |
V2 | 0.0165 (3) | 0.0146 (3) | 0.0124 (2) | −0.00063 (19) | −0.00209 (18) | 0.00365 (19) |
Na | 0.0260 (10) | 0.0164 (9) | 0.0143 (8) | 0.000 | 0.0009 (7) | 0.000 |
O1 | 0.0162 (11) | 0.0292 (13) | 0.0194 (11) | −0.0075 (10) | 0.0018 (8) | −0.0008 (10) |
O2 | 0.0298 (18) | 0.0129 (16) | 0.0226 (17) | 0.000 | −0.0080 (14) | 0.000 |
O3 | 0.0254 (12) | 0.0211 (12) | 0.0190 (11) | 0.0049 (10) | −0.0029 (9) | 0.0041 (9) |
O4 | 0.0165 (11) | 0.0310 (14) | 0.0134 (10) | −0.0005 (9) | 0.0005 (8) | −0.0022 (10) |
O5 | 0.0187 (12) | 0.0296 (14) | 0.0298 (13) | 0.0043 (10) | −0.0049 (10) | 0.0028 (11) |
O6 | 0.0213 (17) | 0.0166 (16) | 0.0302 (18) | 0.000 | 0.0033 (14) | 0.000 |
O7 | 0.0488 (18) | 0.0349 (16) | 0.0211 (13) | −0.0178 (14) | −0.0072 (12) | 0.0135 (12) |
Ow | 0.0216 (18) | 0.025 (2) | 0.0287 (19) | 0.000 | 0.0025 (14) | 0.000 |
Rb1—O6 | 2.892 (4) | V1—O3 | 1.632 (2) |
Rb1—O1i | 3.029 (2) | V1—O1 | 1.648 (2) |
Rb1—O1ii | 3.029 (2) | V1—O2xiv | 1.8025 (10) |
Rb1—O5i | 3.046 (3) | V1—O4 | 1.804 (2) |
Rb1—O5ii | 3.046 (3) | V2—O7 | 1.624 (3) |
Rb1—O1iii | 3.194 (3) | V2—O5 | 1.641 (2) |
Rb1—O1iv | 3.194 (3) | V2—O6 | 1.8064 (15) |
Rb1—Owv | 3.299 (4) | V2—O4 | 1.815 (2) |
Rb1—O2vi | 3.382 (4) | Na—O7 | 2.282 (3) |
Rb1—O7 | 3.560 (3) | Na—O7xii | 2.282 (3) |
Rb1—O7vii | 3.560 (4) | Na—Ow | 2.349 (4) |
Rb2—O2viii | 2.837 (3) | Na—O1iv | 2.483 (3) |
Rb2—O4 | 2.986 (3) | Na—O1xv | 2.483 (3) |
Rb2—O4vii | 2.986 (3) | Na—O3iv | 2.705 (3) |
Rb2—O5ii | 3.132 (3) | Na—O3xv | 2.705 (3) |
Rb2—O5i | 3.132 (3) | O6—V2vii | 1.8064 (15) |
Rb2—O6 | 3.140 (4) | O5—Rb3xvi | 2.946 (3) |
Rb2—O3ix | 3.203 (3) | O5—Rb1xvi | 3.046 (3) |
Rb2—O3x | 3.203 (3) | O5—Rb2xvi | 3.132 (3) |
Rb2—O3vii | 3.324 (2) | O2—V1xvii | 1.8025 (10) |
Rb2—O3 | 3.324 (2) | O2—V1xviii | 1.8025 (10) |
Rb3—O5i | 2.946 (3) | O2—Rb2viii | 2.837 (3) |
Rb3—O5xi | 2.946 (3) | O2—Rb1xix | 3.382 (4) |
Rb3—O4 | 3.033 (3) | O1—Naxx | 2.483 (3) |
Rb3—O4xii | 3.033 (2) | O1—Rb1xvi | 3.029 (2) |
Rb3—Ow | 3.127 (4) | O1—Rb1xx | 3.194 (3) |
Rb3—O3xiii | 3.190 (2) | O3—Naxx | 2.705 (3) |
Rb3—O3ix | 3.190 (2) | O3—Rb3ix | 3.190 (2) |
Rb3—O7 | 3.335 (3) | O3—Rb2ix | 3.203 (3) |
Rb3—O7xii | 3.335 (3) | Ow—Rb1v | 3.299 (4) |
Rb3—O7xi | 3.533 (3) | Ow—H8 | 0.9704 |
Rb3—O7i | 3.533 (3) | O7—Rb3xvi | 3.533 (3) |
O6—Rb1—O1i | 138.87 (5) | O3ix—Rb2—O3 | 59.85 (8) |
O6—Rb1—O1ii | 138.87 (5) | O3x—Rb2—O3 | 104.67 (4) |
O1i—Rb1—O1ii | 76.82 (10) | O3vii—Rb2—O3 | 55.16 (9) |
O6—Rb1—O5i | 78.90 (8) | O5i—Rb3—O5xi | 113.16 (10) |
O1i—Rb1—O5i | 67.96 (7) | O5i—Rb3—O4 | 80.02 (7) |
O1ii—Rb1—O5i | 108.40 (7) | O5xi—Rb3—O4 | 157.27 (7) |
O6—Rb1—O5ii | 78.90 (8) | O5i—Rb3—O4xii | 157.26 (7) |
O1i—Rb1—O5ii | 108.40 (7) | O5xi—Rb3—O4xii | 80.02 (7) |
O1ii—Rb1—O5ii | 67.96 (7) | O4—Rb3—O4xii | 82.04 (10) |
O5i—Rb1—O5ii | 67.58 (10) | O5i—Rb3—Ow | 64.63 (6) |
O6—Rb1—O1iii | 100.50 (7) | O5xi—Rb3—Ow | 64.63 (6) |
O1i—Rb1—O1iii | 116.82 (3) | O4—Rb3—Ow | 108.89 (6) |
O1ii—Rb1—O1iii | 64.40 (7) | O4xii—Rb3—Ow | 108.89 (6) |
O5i—Rb1—O1iii | 168.42 (7) | O5i—Rb3—O3xiii | 126.70 (7) |
O5ii—Rb1—O1iii | 100.89 (7) | O5xi—Rb3—O3xiii | 78.02 (7) |
O6—Rb1—O1iv | 100.50 (7) | O4—Rb3—O3xiii | 109.73 (6) |
O1i—Rb1—O1iv | 64.40 (7) | O4xii—Rb3—O3xiii | 72.82 (6) |
O1ii—Rb1—O1iv | 116.82 (3) | Ow—Rb3—O3xiii | 141.16 (6) |
O5i—Rb1—O1iv | 100.89 (7) | O5i—Rb3—O3ix | 78.02 (7) |
O5ii—Rb1—O1iv | 168.42 (7) | O5xi—Rb3—O3ix | 126.70 (7) |
O1iii—Rb1—O1iv | 90.61 (9) | O4—Rb3—O3ix | 72.82 (6) |
O6—Rb1—Owv | 142.04 (10) | O4xii—Rb3—O3ix | 109.73 (6) |
O1i—Rb1—Owv | 62.55 (6) | Ow—Rb3—O3ix | 141.16 (6) |
O1ii—Rb1—Owv | 62.55 (6) | O3xiii—Rb3—O3ix | 57.68 (9) |
O5i—Rb1—Owv | 130.47 (7) | O5i—Rb3—O7 | 69.57 (8) |
O5ii—Rb1—Owv | 130.47 (7) | O5xi—Rb3—O7 | 113.75 (7) |
O1iii—Rb1—Owv | 55.84 (5) | O4—Rb3—O7 | 51.67 (6) |
O1iv—Rb1—Owv | 55.84 (5) | O4xii—Rb3—O7 | 88.34 (8) |
O6—Rb1—O2vi | 78.73 (9) | Ow—Rb3—O7 | 58.53 (7) |
O1i—Rb1—O2vi | 111.05 (6) | O3xiii—Rb3—O7 | 156.10 (7) |
O1ii—Rb1—O2vi | 111.05 (6) | O3ix—Rb3—O7 | 118.67 (7) |
O5i—Rb1—O2vi | 139.05 (6) | O5i—Rb3—O7xii | 113.75 (7) |
O5ii—Rb1—O2vi | 139.05 (6) | O5xi—Rb3—O7xii | 69.57 (8) |
O1iii—Rb1—O2vi | 50.91 (5) | O4—Rb3—O7xii | 88.34 (8) |
O1iv—Rb1—O2vi | 50.91 (5) | O4xii—Rb3—O7xii | 51.67 (6) |
Owv—Rb1—O2vi | 63.31 (8) | Ow—Rb3—O7xii | 58.53 (7) |
O6—Rb1—O7 | 49.47 (5) | O3xiii—Rb3—O7xii | 118.67 (7) |
O1i—Rb1—O7 | 93.44 (7) | O3ix—Rb3—O7xii | 156.10 (7) |
O1ii—Rb1—O7 | 170.09 (7) | O7—Rb3—O7xii | 53.53 (11) |
O5i—Rb1—O7 | 65.46 (7) | O5i—Rb3—O7xi | 92.15 (7) |
O5ii—Rb1—O7 | 114.37 (7) | O5xi—Rb3—O7xi | 47.76 (7) |
O1iii—Rb1—O7 | 122.94 (6) | O4—Rb3—O7xi | 154.03 (6) |
O1iv—Rb1—O7 | 59.02 (6) | O4xii—Rb3—O7xi | 109.94 (7) |
Owv—Rb1—O7 | 114.72 (6) | Ow—Rb3—O7xi | 89.44 (7) |
O2vi—Rb1—O7 | 73.91 (6) | O3xiii—Rb3—O7xi | 55.93 (6) |
O6—Rb1—O7vii | 49.47 (5) | O3ix—Rb3—O7xi | 81.37 (6) |
O1i—Rb1—O7vii | 170.09 (7) | O7—Rb3—O7xi | 147.34 (4) |
O1ii—Rb1—O7vii | 93.44 (7) | O7xii—Rb3—O7xi | 117.32 (8) |
O5i—Rb1—O7vii | 114.37 (7) | O5i—Rb3—O7i | 47.76 (7) |
O5ii—Rb1—O7vii | 65.46 (7) | O5xi—Rb3—O7i | 92.15 (7) |
O1iii—Rb1—O7vii | 59.02 (6) | O4—Rb3—O7i | 109.94 (7) |
O1iv—Rb1—O7vii | 122.94 (7) | O4xii—Rb3—O7i | 154.03 (6) |
Owv—Rb1—O7vii | 114.72 (6) | Ow—Rb3—O7i | 89.44 (7) |
O2vi—Rb1—O7vii | 73.91 (6) | O3xiii—Rb3—O7i | 81.37 (6) |
O7—Rb1—O7vii | 96.23 (9) | O3ix—Rb3—O7i | 55.93 (6) |
O2viii—Rb2—O4 | 124.03 (6) | O7—Rb3—O7i | 117.32 (8) |
O2viii—Rb2—O4vii | 124.03 (6) | O7xii—Rb3—O7i | 147.34 (4) |
O4—Rb2—O4vii | 92.77 (10) | O7xi—Rb3—O7i | 50.32 (10) |
O2viii—Rb2—O5ii | 104.76 (8) | O3—V1—O1 | 108.47 (13) |
O4—Rb2—O5ii | 124.91 (6) | O3—V1—O2xiv | 109.15 (14) |
O4vii—Rb2—O5ii | 77.82 (6) | O1—V1—O2xiv | 110.18 (15) |
O2viii—Rb2—O5i | 104.76 (8) | O3—V1—O4 | 109.36 (12) |
O4—Rb2—O5i | 77.82 (6) | O1—V1—O4 | 109.47 (11) |
O4vii—Rb2—O5i | 124.91 (6) | O2xiv—V1—O4 | 110.19 (14) |
O5ii—Rb2—O5i | 65.49 (10) | O7—V2—O5 | 110.13 (15) |
O2viii—Rb2—O6 | 178.52 (10) | O7—V2—O6 | 107.39 (16) |
O4—Rb2—O6 | 56.70 (6) | O5—V2—O6 | 110.22 (15) |
O4vii—Rb2—O6 | 56.70 (6) | O7—V2—O4 | 108.21 (13) |
O5ii—Rb2—O6 | 74.01 (7) | O5—V2—O4 | 113.59 (12) |
O5i—Rb2—O6 | 74.01 (7) | O6—V2—O4 | 107.07 (15) |
O2viii—Rb2—O3ix | 54.83 (4) | O7—Na—O7xii | 82.34 (17) |
O4—Rb2—O3ix | 73.23 (6) | O7—Na—Ow | 86.20 (12) |
O4vii—Rb2—O3ix | 153.26 (6) | O7xii—Na—Ow | 86.20 (12) |
O5ii—Rb2—O3ix | 128.90 (7) | O7—Na—O1iv | 88.99 (10) |
O5i—Rb2—O3ix | 75.24 (6) | O7xii—Na—O1iv | 168.63 (12) |
O6—Rb2—O3ix | 125.24 (4) | Ow—Na—O1iv | 85.90 (10) |
O2viii—Rb2—O3x | 54.83 (4) | O7—Na—O1xv | 168.63 (12) |
O4—Rb2—O3x | 153.26 (6) | O7xii—Na—O1xv | 88.99 (10) |
O4vii—Rb2—O3x | 73.23 (6) | Ow—Na—O1xv | 85.90 (10) |
O5ii—Rb2—O3x | 75.24 (6) | O1iv—Na—O1xv | 98.58 (13) |
O5i—Rb2—O3x | 128.90 (7) | O7—Na—O3iv | 78.35 (10) |
O6—Rb2—O3x | 125.24 (4) | O7xii—Na—O3iv | 123.16 (12) |
O3ix—Rb2—O3x | 109.37 (8) | Ow—Na—O3iv | 143.80 (7) |
O2viii—Rb2—O3vii | 81.90 (8) | O1iv—Na—O3iv | 61.56 (8) |
O4—Rb2—O3vii | 93.50 (6) | O1xv—Na—O3iv | 112.71 (10) |
O4vii—Rb2—O3vii | 52.46 (6) | O7—Na—O3xv | 123.16 (12) |
O5ii—Rb2—O3vii | 119.14 (7) | O7xii—Na—O3xv | 78.35 (10) |
O5i—Rb2—O3vii | 171.03 (6) | Ow—Na—O3xv | 143.80 (7) |
O6—Rb2—O3vii | 99.40 (7) | O1iv—Na—O3xv | 112.71 (10) |
O3ix—Rb2—O3vii | 104.67 (4) | O1xv—Na—O3xv | 61.56 (8) |
O3x—Rb2—O3vii | 59.85 (8) | O3iv—Na—O3xv | 69.34 (12) |
O2viii—Rb2—O3 | 81.90 (8) | V2vii—O6—V2 | 134.5 (2) |
O4—Rb2—O3 | 52.46 (6) | V1xvii—O2—V1xviii | 150.6 (2) |
O4vii—Rb2—O3 | 93.50 (6) | V1—O4—V2 | 135.92 (14) |
O5ii—Rb2—O3 | 171.03 (6) | Na—Ow—H8 | 116.0 |
O5i—Rb2—O3 | 119.14 (7) | Rb3—Ow—H8 | 112.2 |
O6—Rb2—O3 | 99.40 (7) | Rb1v—Ow—H8 | 67.9 |
Symmetry codes: (i) x−1/2, y, −z+3/2; (ii) x−1/2, −y+3/2, −z+3/2; (iii) −x+3/2, y+1/2, z+1/2; (iv) −x+3/2, −y+1, z+1/2; (v) −x+1, −y+1, −z+2; (vi) −x+3/2, −y, z+1/2; (vii) x, −y+3/2, z; (viii) −x+1, −y, −z+1; (ix) −x+1, −y+1, −z+1; (x) −x+1, y+1/2, −z+1; (xi) x−1/2, −y+1/2, −z+3/2; (xii) x, −y+1/2, z; (xiii) −x+1, y−1/2, −z+1; (xiv) x, y+1, z; (xv) −x+3/2, y−1/2, z+1/2; (xvi) x+1/2, y, −z+3/2; (xvii) x, y−1, z; (xviii) x, −y−1/2, z; (xix) −x+3/2, −y, z−1/2; (xx) −x+3/2, −y+1, z−1/2. |