Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805025705/wm6085sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805025705/wm6085Isup2.hkl |
Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.
CsGd(PO3)4 | F(000) = 1100 |
Mr = 606.04 | Dx = 4.070 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 9641 reflections |
a = 10.3229 (2) Å | θ = 2–40° |
b = 8.9307 (2) Å | µ = 11.04 mm−1 |
c = 11.1826 (2) Å | T = 292 K |
β = 106.371 (1)° | Needle, colourless |
V = 989.13 (3) Å3 | 0.26 × 0.20 × 0.16 mm |
Z = 4 |
Nonius KappaCCD diffractometer | 6980 independent reflections |
Radiation source: fine-focus sealed tube | 5595 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.071 |
Detector resolution: 9 pixels mm-1 | θmax = 42.1°, θmin = 3.0° |
ω scans | h = −14→19 |
Absorption correction: analytical (de Meulenaer & Tompa, 1965) | k = −16→15 |
Tmin = 0.177, Tmax = 0.271 | l = −21→20 |
19421 measured reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: heavy-atom method |
R[F2 > 2σ(F2)] = 0.018 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.046 | w = 1/[σ2(Fo2) + (0.0187P)2 + 2.8091P] where P = (Fo2 + 2Fc2)/3 |
S = 1.24 | (Δ/σ)max = 0.001 |
6980 reflections | Δρmax = 0.89 e Å−3 |
164 parameters | Δρmin = −0.58 e Å−3 |
Experimental. Data were corrected for Lorentz-polarization effects and an analytical absorption correction (Meulenaer & Tompa, 1965) was applied. The structure was solved in the P 1 21/n 1 space group by the Patterson method (Cs and Gd) and subsequent difference Fourier syntheses (all other atoms). |
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 | ||
Gd | 0.497879 (11) | 0.273491 (14) | 0.180789 (11) | 0.00726 (4) | |
Cs | 0.67903 (2) | 0.56590 (3) | 0.459719 (19) | 0.01910 (6) | |
P1 | 0.64512 (6) | −0.09227 (9) | 0.25790 (7) | 0.00809 (11) | |
P2 | 0.45955 (7) | −0.32517 (9) | 0.13266 (7) | 0.00799 (11) | |
P3 | 0.24454 (6) | −0.47205 (9) | 0.21423 (6) | 0.00771 (11) | |
P4 | 0.17229 (6) | −0.60738 (9) | −0.02627 (7) | 0.00818 (11) | |
O1 | 0.13635 (19) | −0.5429 (3) | 0.09486 (19) | 0.0106 (3) | |
O2 | 0.3514 (2) | −0.5836 (3) | 0.2739 (2) | 0.0111 (3) | |
O3 | 0.5209 (2) | −0.2067 (3) | 0.2421 (2) | 0.0116 (3) | |
O4 | 0.6009 (2) | 0.0399 (3) | 0.1762 (2) | 0.0123 (3) | |
O5 | 0.4394 (2) | −0.2544 (3) | 0.0091 (2) | 0.0133 (3) | |
O6 | 0.1682 (2) | −0.4037 (3) | 0.2944 (2) | 0.0121 (3) | |
O7 | 0.7638 (2) | −0.1780 (3) | 0.2463 (2) | 0.0139 (4) | |
O8 | 0.0641 (2) | −0.7111 (3) | −0.0963 (2) | 0.0126 (4) | |
O9 | 0.3129 (2) | −0.6654 (3) | 0.0140 (2) | 0.0135 (4) | |
O10 | 0.5363 (2) | −0.4673 (3) | 0.1652 (2) | 0.0130 (4) | |
O11 | 0.31122 (19) | −0.3412 (3) | 0.1532 (2) | 0.0106 (3) | |
O12 | 0.6668 (2) | −0.0479 (3) | 0.4002 (2) | 0.0139 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Gd | 0.00551 (6) | 0.00778 (7) | 0.00655 (6) | 0.00047 (3) | −0.00147 (4) | 0.00069 (3) |
Cs | 0.02011 (9) | 0.02358 (11) | 0.01103 (9) | −0.00406 (6) | 0.00018 (6) | 0.00080 (6) |
P1 | 0.0065 (2) | 0.0081 (3) | 0.0074 (2) | −0.00007 (18) | −0.00168 (17) | −0.0006 (2) |
P2 | 0.0073 (2) | 0.0076 (3) | 0.0073 (2) | −0.00007 (18) | −0.00079 (17) | −0.0001 (2) |
P3 | 0.0062 (2) | 0.0087 (3) | 0.0065 (2) | 0.00102 (18) | −0.00098 (17) | −0.00025 (19) |
P4 | 0.0060 (2) | 0.0095 (3) | 0.0063 (2) | −0.00002 (18) | −0.00268 (17) | 0.0001 (2) |
O1 | 0.0076 (6) | 0.0161 (9) | 0.0064 (7) | −0.0018 (6) | −0.0009 (5) | −0.0022 (6) |
O2 | 0.0095 (7) | 0.0126 (8) | 0.0099 (8) | 0.0037 (6) | 0.0003 (5) | 0.0013 (6) |
O3 | 0.0120 (7) | 0.0113 (8) | 0.0096 (8) | −0.0041 (6) | −0.0003 (6) | −0.0031 (6) |
O4 | 0.0157 (8) | 0.0096 (8) | 0.0104 (8) | 0.0018 (6) | 0.0018 (6) | 0.0037 (6) |
O5 | 0.0115 (7) | 0.0174 (9) | 0.0104 (8) | 0.0024 (7) | 0.0022 (6) | 0.0024 (7) |
O6 | 0.0113 (7) | 0.0144 (9) | 0.0108 (8) | 0.0036 (6) | 0.0034 (6) | −0.0011 (7) |
O7 | 0.0083 (7) | 0.0158 (10) | 0.0150 (9) | 0.0027 (6) | −0.0009 (6) | −0.0015 (7) |
O8 | 0.0114 (8) | 0.0129 (9) | 0.0114 (8) | −0.0033 (6) | −0.0002 (6) | −0.0040 (7) |
O9 | 0.0071 (6) | 0.0220 (11) | 0.0093 (8) | 0.0051 (6) | −0.0013 (5) | 0.0016 (7) |
O10 | 0.0088 (7) | 0.0102 (9) | 0.0184 (10) | 0.0011 (6) | 0.0012 (6) | 0.0018 (7) |
O11 | 0.0062 (6) | 0.0117 (8) | 0.0122 (8) | −0.0008 (5) | 0.0000 (5) | 0.0026 (6) |
O12 | 0.0193 (9) | 0.0115 (9) | 0.0074 (8) | 0.0006 (7) | −0.0018 (6) | −0.0024 (6) |
Gd—O9i | 2.327 (2) | P2—Csvii | 3.7855 (7) |
Gd—O4 | 2.349 (2) | P2—Csx | 3.8451 (7) |
Gd—O10i | 2.363 (2) | P3—O6 | 1.481 (2) |
Gd—O5ii | 2.394 (3) | P3—O2 | 1.497 (2) |
Gd—O7iii | 2.403 (2) | P3—O11 | 1.603 (2) |
Gd—O6iv | 2.406 (2) | P3—O1 | 1.609 (2) |
Gd—O2i | 2.426 (2) | P3—Csviii | 3.6052 (7) |
Gd—O8v | 2.456 (2) | P4—O9 | 1.487 (2) |
Gd—Cs | 4.0936 (3) | P4—O8 | 1.492 (2) |
Gd—Csvi | 4.4703 (3) | P4—O12xi | 1.605 (3) |
Gd—Csvii | 4.6417 (3) | P4—O1 | 1.608 (2) |
Cs—O4iii | 3.077 (2) | P4—Csxi | 4.0992 (8) |
Cs—O2viii | 3.086 (2) | O2—Gdx | 2.426 (2) |
Cs—O5ix | 3.087 (2) | O2—Csviii | 3.086 (2) |
Cs—O6viii | 3.115 (2) | O2—Csx | 3.684 (2) |
Cs—O10i | 3.220 (2) | O3—Csx | 3.236 (2) |
Cs—O3i | 3.237 (2) | O4—Csvi | 3.077 (2) |
Cs—O11ix | 3.305 (2) | O5—Gdii | 2.394 (3) |
Cs—O7iii | 3.341 (3) | O5—Csvii | 3.087 (2) |
Cs—O8v | 3.379 (3) | O6—Gdxii | 2.406 (2) |
Cs—O12i | 3.509 (3) | O6—Csviii | 3.115 (2) |
Cs—O7i | 3.588 (3) | O7—Gdvi | 2.403 (2) |
Cs—P3viii | 3.6052 (7) | O7—Csvi | 3.341 (3) |
P1—O7 | 1.481 (2) | O7—Csx | 3.588 (3) |
P1—O4 | 1.484 (2) | O8—Gdxi | 2.456 (2) |
P1—O12 | 1.593 (2) | O8—Csxi | 3.379 (3) |
P1—O3 | 1.610 (2) | O9—Gdx | 2.327 (2) |
P1—Csvi | 3.7017 (8) | O10—Gdx | 2.363 (2) |
P1—Csx | 3.7537 (8) | O10—Csx | 3.220 (2) |
P2—O5 | 1.480 (3) | O11—Csvii | 3.305 (2) |
P2—O10 | 1.486 (2) | O12—P4v | 1.605 (3) |
P2—O3 | 1.607 (2) | O12—Csx | 3.509 (3) |
P2—O11 | 1.617 (2) | ||
O9i—Gd—O4 | 117.72 (9) | O3i—Cs—O7i | 42.74 (5) |
O9i—Gd—O10i | 80.10 (9) | O11ix—Cs—O7i | 80.11 (6) |
O4—Gd—O10i | 141.43 (8) | O7iii—Cs—O7i | 80.407 (7) |
O9i—Gd—O5ii | 70.82 (8) | O8v—Cs—O7i | 127.81 (6) |
O4—Gd—O5ii | 71.35 (9) | O12i—Cs—O7i | 41.36 (6) |
O10i—Gd—O5ii | 84.91 (9) | O4iii—Cs—P3viii | 120.02 (4) |
O9i—Gd—O7iii | 139.47 (9) | O2viii—Cs—P3viii | 24.29 (4) |
O4—Gd—O7iii | 74.98 (9) | O5ix—Cs—P3viii | 90.83 (5) |
O10i—Gd—O7iii | 70.81 (8) | O6viii—Cs—P3viii | 24.07 (4) |
O5ii—Gd—O7iii | 78.88 (8) | O10i—Cs—P3viii | 156.86 (5) |
O9i—Gd—O6iv | 78.25 (9) | O3i—Cs—P3viii | 145.75 (5) |
O4—Gd—O6iv | 76.14 (8) | O11ix—Cs—P3viii | 65.08 (4) |
O10i—Gd—O6iv | 142.42 (8) | O7iii—Cs—P3viii | 120.98 (4) |
O5ii—Gd—O6iv | 115.80 (9) | O8v—Cs—P3viii | 86.26 (4) |
O7iii—Gd—O6iv | 140.72 (8) | O12i—Cs—P3viii | 113.98 (4) |
O9i—Gd—O2i | 75.57 (8) | O7i—Cs—P3viii | 142.77 (4) |
O4—Gd—O2i | 144.84 (8) | O7—P1—O4 | 118.41 (15) |
O10i—Gd—O2i | 69.77 (8) | O7—P1—O12 | 109.23 (13) |
O5ii—Gd—O2i | 140.80 (8) | O4—P1—O12 | 110.44 (14) |
O7iii—Gd—O2i | 117.49 (8) | O7—P1—O3 | 108.38 (14) |
O6iv—Gd—O2i | 75.27 (9) | O4—P1—O3 | 109.87 (13) |
O9i—Gd—O8v | 142.91 (8) | O12—P1—O3 | 98.69 (14) |
O4—Gd—O8v | 79.78 (8) | O7—P1—Csvi | 64.44 (11) |
O10i—Gd—O8v | 107.00 (8) | O4—P1—Csvi | 54.15 (10) |
O5ii—Gd—O8v | 144.76 (8) | O12—P1—Csvi | 127.20 (10) |
O7iii—Gd—O8v | 74.38 (8) | O3—P1—Csvi | 133.87 (9) |
O6iv—Gd—O8v | 74.77 (8) | O7—P1—Csx | 72.13 (11) |
O2i—Gd—O8v | 73.30 (8) | O4—P1—Csx | 167.86 (10) |
O9i—Gd—Cs | 123.81 (7) | O12—P1—Csx | 68.84 (10) |
O4—Gd—Cs | 118.09 (5) | O3—P1—Csx | 59.10 (9) |
O10i—Gd—Cs | 51.77 (6) | Csvi—P1—Csx | 136.53 (2) |
O5ii—Gd—Cs | 122.79 (6) | O5—P2—O10 | 121.21 (15) |
O7iii—Gd—Cs | 54.71 (7) | O5—P2—O3 | 110.56 (15) |
O6iv—Gd—Cs | 121.25 (6) | O10—P2—O3 | 107.91 (13) |
O2i—Gd—Cs | 62.83 (5) | O5—P2—O11 | 106.33 (12) |
O8v—Gd—Cs | 55.56 (6) | O10—P2—O11 | 110.51 (13) |
O9i—Gd—Csvi | 109.91 (6) | O3—P2—O11 | 97.80 (13) |
O4—Gd—Csvi | 40.24 (6) | O5—P2—Csvii | 51.39 (10) |
O10i—Gd—Csvi | 102.88 (6) | O10—P2—Csvii | 157.79 (9) |
O5ii—Gd—Csvi | 40.87 (5) | O3—P2—Csvii | 93.82 (9) |
O7iii—Gd—Csvi | 53.14 (7) | O11—P2—Csvii | 60.54 (8) |
O6iv—Gd—Csvi | 113.24 (6) | O5—P2—Csx | 152.39 (10) |
O2i—Gd—Csvi | 170.37 (5) | O10—P2—Csx | 54.57 (10) |
O8v—Gd—Csvi | 103.94 (6) | O3—P2—Csx | 56.10 (9) |
Cs—Gd—Csvi | 107.850 (4) | O11—P2—Csx | 99.80 (8) |
O9i—Gd—Csvii | 55.10 (7) | Csvii—P2—Csx | 143.27 (2) |
O4—Gd—Csvii | 70.48 (5) | O6—P3—O2 | 117.10 (14) |
O10i—Gd—Csvii | 135.15 (5) | O6—P3—O11 | 108.81 (14) |
O5ii—Gd—Csvii | 79.02 (6) | O2—P3—O11 | 108.89 (13) |
O7iii—Gd—Csvii | 143.41 (7) | O6—P3—O1 | 107.52 (12) |
O6iv—Gd—Csvii | 37.88 (6) | O2—P3—O1 | 111.11 (13) |
O2i—Gd—Csvii | 97.94 (5) | O11—P3—O1 | 102.39 (12) |
O8v—Gd—Csvii | 110.20 (6) | O6—P3—Csviii | 59.08 (9) |
Cs—Gd—Csvii | 157.736 (7) | O2—P3—Csviii | 58.04 (9) |
Csvi—Gd—Csvii | 91.678 (5) | O11—P3—Csviii | 127.03 (8) |
O4iii—Cs—O2viii | 140.42 (6) | O1—P3—Csviii | 130.57 (9) |
O4iii—Cs—O5ix | 53.32 (6) | O9—P4—O8 | 117.73 (15) |
O2viii—Cs—O5ix | 96.88 (6) | O9—P4—O12xi | 110.27 (15) |
O4iii—Cs—O6viii | 98.08 (6) | O8—P4—O12xi | 110.76 (13) |
O2viii—Cs—O6viii | 48.36 (6) | O9—P4—O1 | 107.87 (12) |
O5ix—Cs—O6viii | 84.10 (7) | O8—P4—O1 | 110.37 (13) |
O4iii—Cs—O10i | 71.13 (6) | O12xi—P4—O1 | 98.02 (14) |
O2viii—Cs—O10i | 148.23 (6) | O9—P4—Csxi | 68.78 (11) |
O5ix—Cs—O10i | 110.95 (6) | O8—P4—Csxi | 51.52 (10) |
O6viii—Cs—O10i | 146.29 (6) | O12xi—P4—Csxi | 147.33 (10) |
O4iii—Cs—O3i | 87.83 (6) | O1—P4—Csxi | 113.58 (10) |
O2viii—Cs—O3i | 121.78 (6) | P4—O1—P3 | 124.64 (13) |
O5ix—Cs—O3i | 91.24 (6) | P3—O2—Gdx | 128.98 (13) |
O6viii—Cs—O3i | 168.04 (6) | P3—O2—Csviii | 97.67 (11) |
O10i—Cs—O3i | 45.60 (6) | Gdx—O2—Csviii | 133.35 (8) |
O4iii—Cs—O11ix | 98.82 (6) | P3—O2—Csx | 117.04 (12) |
O2viii—Cs—O11ix | 57.71 (6) | Gdx—O2—Csx | 81.30 (5) |
O5ix—Cs—O11ix | 45.50 (6) | Csviii—O2—Csx | 76.36 (5) |
O6viii—Cs—O11ix | 75.83 (6) | P2—O3—P1 | 129.22 (17) |
O10i—Cs—O11ix | 136.34 (6) | P2—O3—Csx | 99.57 (11) |
O3i—Cs—O11ix | 93.04 (6) | P1—O3—Csx | 95.63 (9) |
O4iii—Cs—O7iii | 46.53 (6) | P1—O4—Gd | 139.09 (15) |
O2viii—Cs—O7iii | 141.67 (6) | P1—O4—Csvi | 102.84 (11) |
O5ix—Cs—O7iii | 99.49 (6) | Gd—O4—Csvi | 110.23 (8) |
O6viii—Cs—O7iii | 99.30 (6) | P2—O5—Gdii | 142.75 (16) |
O10i—Cs—O7iii | 49.74 (6) | P2—O5—Csvii | 106.61 (12) |
O3i—Cs—O7iii | 92.32 (6) | Gdii—O5—Csvii | 108.63 (8) |
O11ix—Cs—O7iii | 144.65 (5) | P3—O6—Gdxii | 149.17 (14) |
O4iii—Cs—O8v | 96.15 (6) | P3—O6—Csviii | 96.85 (10) |
O2viii—Cs—O8v | 95.79 (6) | Gdxii—O6—Csviii | 113.81 (8) |
O5ix—Cs—O8v | 141.91 (6) | P1—O7—Gdvi | 148.91 (15) |
O6viii—Cs—O8v | 77.96 (6) | P1—O7—Csvi | 91.98 (12) |
O10i—Cs—O8v | 71.86 (6) | Gdvi—O7—Csvi | 89.35 (8) |
O3i—Cs—O8v | 111.88 (5) | P1—O7—Csx | 84.74 (12) |
O11ix—Cs—O8v | 151.33 (6) | Gdvi—O7—Csx | 94.45 (7) |
O7iii—Cs—O8v | 51.83 (6) | Csvi—O7—Csx | 176.20 (7) |
O4iii—Cs—O12i | 88.42 (6) | P4—O8—Gdxi | 128.81 (15) |
O2viii—Cs—O12i | 97.18 (6) | P4—O8—Csxi | 108.26 (11) |
O5ix—Cs—O12i | 58.71 (6) | Gdxi—O8—Csxi | 87.61 (7) |
O6viii—Cs—O12i | 127.37 (6) | P4—O9—Gdx | 146.63 (15) |
O10i—Cs—O12i | 85.11 (6) | P2—O10—Gdx | 139.94 (13) |
O3i—Cs—O12i | 41.99 (5) | P2—O10—Csx | 103.33 (12) |
O11ix—Cs—O12i | 51.61 (5) | Gdx—O10—Csx | 93.03 (7) |
O7iii—Cs—O12i | 120.93 (6) | P3—O11—P2 | 131.48 (15) |
O8v—Cs—O12i | 153.46 (5) | P3—O11—Csvii | 132.32 (10) |
O4iii—Cs—O7i | 50.73 (6) | P2—O11—Csvii | 94.24 (10) |
O2viii—Cs—O7i | 136.04 (6) | P1—O12—P4v | 134.56 (18) |
O5ix—Cs—O7i | 53.70 (6) | P1—O12—Csx | 86.12 (10) |
O6viii—Cs—O7i | 136.57 (5) | P4v—O12—Csx | 139.26 (12) |
O10i—Cs—O7i | 60.35 (6) |
Symmetry codes: (i) x, y+1, z; (ii) −x+1, −y, −z; (iii) −x+3/2, y+1/2, −z+1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x+1/2, −y−1/2, z+1/2; (vi) −x+3/2, y−1/2, −z+1/2; (vii) x−1/2, −y+1/2, z−1/2; (viii) −x+1, −y, −z+1; (ix) x+1/2, −y+1/2, z+1/2; (x) x, y−1, z; (xi) x−1/2, −y−1/2, z−1/2; (xii) −x+1/2, y−1/2, −z+1/2. |