Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100012087/qa0369sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100012087/qa0369Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100012087/qa0369IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100012087/qa0369IIIsup4.hkl |
CCDC references: 152650; 152651; 152652
The three title complexes were synthesized in an identical manner. The oxide M2O3 (0.5 mmol) (M = Nd, Sm or Gd) was stirred in an aqueous solution of diglycollic acid (3.0 mmol in 30 ml water) and sodium bicarbonate (3.0 mmol). After an hour, NaBF4 (2.0 mmol) was added, and the solution allowed to evaporate in air, yielding large well formed crystals of the complexes. Small samples for the crystallographic analyses were cleaved from larger crystals.
The methylene H atoms were placed in calculated positions (C—H = 0.96 Å) and refined with a riding model. The initial positions of the H atoms of the water molecules were determined from a difference Fourier map and the H atoms were then refined with a riding model and a common isotropic displacement parameter. All calculations were carried out using the WinGX package (Farrugia, 1999).
For all compounds, data collection: CAD-4 EXPRESS (Enraf Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
Na5[Nd(C4H4O5)3](BF4)2·6H2O | Dx = 2.012 Mg m−3 |
Mr = 937.12 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R32 | Cell parameters from 25 reflections |
Hall symbol: R 3 2" | θ = 18.5–21.2° |
a = 9.7508 (7) Å | µ = 1.88 mm−1 |
c = 28.177 (2) Å | T = 291 K |
V = 2320.1 (3) Å3 | Cleaved from large crystal, pale violet |
Z = 3 | 0.55 × 0.45 × 0.1 mm |
F(000) = 1383 |
Enraf Nonius CAD-4 diffractometer | 1001 reflections with I > 2σ(I) |
Radiation source: Enraf Nonius FR590 | Rint = 0.030 |
Graphite monochromator | θmax = 30.0°, θmin = 2.5° |
non–profiled ω scans | h = −1→13 |
Absorption correction: ψ scan (North et al., 1968) | k = −11→1 |
Tmin = 0.425, Tmax = 0.834 | l = −3→39 |
1134 measured reflections | 3 standard reflections every 120 min |
1001 independent reflections | intensity decay: none |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.055 | w = 1/[σ2(Fo2) + (0.0427P)2 + 0.7263P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | (Δ/σ)max = 0.001 |
1001 reflections | Δρmax = 0.47 e Å−3 |
77 parameters | Δρmin = −0.51 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 121 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.010 (18) |
Na5[Nd(C4H4O5)3](BF4)2·6H2O | Z = 3 |
Mr = 937.12 | Mo Kα radiation |
Trigonal, R32 | µ = 1.88 mm−1 |
a = 9.7508 (7) Å | T = 291 K |
c = 28.177 (2) Å | 0.55 × 0.45 × 0.1 mm |
V = 2320.1 (3) Å3 |
Enraf Nonius CAD-4 diffractometer | 1001 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.030 |
Tmin = 0.425, Tmax = 0.834 | 3 standard reflections every 120 min |
1134 measured reflections | intensity decay: none |
1001 independent reflections |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.055 | Δρmax = 0.47 e Å−3 |
S = 1.13 | Δρmin = −0.51 e Å−3 |
1001 reflections | Absolute structure: Flack (1983), 121 Friedel pairs |
77 parameters | Absolute structure parameter: −0.010 (18) |
0 restraints |
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 | ||
Nd1 | 0 | 0 | 0 | 0.02133 (9) | |
O1 | 0.2598 (3) | 0.2598 (3) | 0 | 0.0327 (7) | |
O2 | 0.1957 (3) | 0.0335 (3) | 0.05928 (8) | 0.0350 (5) | |
O3 | 0.4177 (3) | 0.1676 (4) | 0.10017 (9) | 0.0496 (7) | |
C1 | 0.3851 (4) | 0.2912 (4) | 0.03223 (12) | 0.0380 (6) | |
H1A | 0.4142 | 0.3874 | 0.0499 | 0.046* | |
H1B | 0.4773 | 0.3062 | 0.0148 | 0.046* | |
C2 | 0.3305 (3) | 0.1520 (9) | 0.06642 (9) | 0.0309 (10) | |
B1 | 0.3333 | −0.3333 | 0.2366 (2) | 0.0459 (11) | |
F1 | 0.3333 | −0.3333 | 0.28508 (15) | 0.0914 (17) | |
F2 | 0.2506 (9) | −0.2633 (9) | 0.21964 (11) | 0.0779 (9) | |
Na1 | 0.6667 | 0.3333 | 0.13419 (7) | 0.0344 (3) | |
Na2 | 0.3333 | −0.0479 (3) | 0.1667 | 0.0596 (6) | |
O4 | 0.5888 (3) | 0.1118 (4) | 0.19083 (9) | 0.0489 (8) | |
H41 | 0.5663 | 0.1328 | 0.2203 | 0.21 (4)* | |
H42 | 0.7031 | 0.1464 | 0.1913 | 0.21 (4)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nd1 | 0.02158 (10) | 0.02158 (10) | 0.02081 (12) | 0.01079 (5) | 0 | 0 |
O1 | 0.0262 (10) | 0.0262 (10) | 0.0382 (14) | 0.0073 (11) | −0.0034 (6) | 0.0034 (6) |
O2 | 0.0301 (10) | 0.0357 (12) | 0.0360 (10) | 0.0140 (9) | −0.0084 (8) | 0.0017 (8) |
O3 | 0.0419 (13) | 0.0515 (16) | 0.0494 (12) | 0.0189 (11) | −0.0205 (11) | −0.0010 (11) |
C1 | 0.0264 (13) | 0.0367 (16) | 0.0423 (15) | 0.0094 (12) | −0.0074 (12) | −0.0002 (13) |
C2 | 0.0285 (11) | 0.031 (3) | 0.0353 (10) | 0.0169 (14) | −0.0073 (9) | −0.0050 (13) |
B1 | 0.0472 (18) | 0.0472 (18) | 0.043 (2) | 0.0236 (9) | 0 | 0 |
F1 | 0.115 (3) | 0.115 (3) | 0.0435 (18) | 0.0577 (14) | 0 | 0 |
F2 | 0.065 (2) | 0.100 (4) | 0.0878 (17) | 0.0559 (18) | −0.012 (3) | 0.000 (3) |
Na1 | 0.0327 (5) | 0.0327 (5) | 0.0377 (8) | 0.0164 (3) | 0 | 0 |
Na2 | 0.0418 (13) | 0.0579 (12) | 0.0737 (16) | 0.0209 (7) | −0.0014 (12) | −0.0007 (6) |
O4 | 0.0508 (19) | 0.0616 (17) | 0.0414 (10) | 0.0335 (13) | −0.0063 (10) | −0.0081 (12) |
Nd1—O2i | 2.432 (2) | B1—F2 | 1.377 (3) |
Nd1—O2 | 2.432 (2) | B1—F2vi | 1.377 (3) |
Nd1—O2ii | 2.432 (2) | B1—F2vii | 1.377 (3) |
Nd1—O2iii | 2.432 (2) | F2—Na2 | 2.365 (6) |
Nd1—O2iv | 2.432 (2) | Na1—O3viii | 2.345 (3) |
Nd1—O2v | 2.432 (2) | Na1—O3ix | 2.345 (3) |
Nd1—O1 | 2.533 (3) | Na1—O4viii | 2.480 (3) |
Nd1—O1ii | 2.533 (3) | Na1—O4 | 2.480 (3) |
Nd1—O1iv | 2.533 (3) | Na1—O4ix | 2.480 (3) |
O1—C1 | 1.427 (3) | Na1—Na2viii | 3.6247 (18) |
O1—C1v | 1.427 (3) | Na1—Na2 | 3.6247 (18) |
O2—C2 | 1.259 (4) | Na1—Na2ix | 3.6247 (18) |
O3—C2 | 1.233 (4) | Na2—O4 | 2.284 (3) |
O3—Na1 | 2.345 (3) | Na2—O4x | 2.284 (3) |
O3—Na2 | 2.622 (3) | Na2—F2x | 2.365 (6) |
C1—C2 | 1.527 (7) | Na2—O3x | 2.622 (3) |
B1—F1 | 1.367 (7) | Na2—Na1xi | 3.6247 (18) |
O2i—Nd1—O2 | 150.09 (12) | O3viii—Na1—O4 | 85.72 (10) |
O2i—Nd1—O2ii | 125.30 (11) | O3—Na1—O4 | 84.40 (10) |
O2—Nd1—O2ii | 78.02 (9) | O3ix—Na1—O4 | 164.04 (12) |
O2i—Nd1—O2iii | 78.02 (9) | O4viii—Na1—O4 | 83.03 (11) |
O2—Nd1—O2iii | 88.31 (12) | O3viii—Na1—O4ix | 164.04 (12) |
O2ii—Nd1—O2iii | 150.09 (12) | O3—Na1—O4ix | 85.72 (10) |
O2i—Nd1—O2iv | 88.31 (12) | O3ix—Na1—O4ix | 84.40 (10) |
O2—Nd1—O2iv | 78.02 (9) | O4viii—Na1—O4ix | 83.03 (11) |
O2ii—Nd1—O2iv | 78.02 (9) | O4—Na1—O4ix | 83.03 (11) |
O2iii—Nd1—O2iv | 125.30 (11) | O3viii—Na1—Na2viii | 46.22 (7) |
O2i—Nd1—O2v | 78.02 (9) | O3—Na1—Na2viii | 146.46 (8) |
O2—Nd1—O2v | 125.30 (11) | O3ix—Na1—Na2viii | 99.67 (9) |
O2ii—Nd1—O2v | 88.31 (12) | O4viii—Na1—Na2viii | 38.49 (7) |
O2iii—Nd1—O2v | 78.02 (9) | O4—Na1—Na2viii | 78.30 (8) |
O2iv—Nd1—O2v | 150.09 (12) | O4ix—Na1—Na2viii | 119.87 (8) |
O2i—Nd1—O1 | 135.85 (6) | O3viii—Na1—Na2 | 99.67 (9) |
O2—Nd1—O1 | 62.65 (6) | O3—Na1—Na2 | 46.22 (7) |
O2ii—Nd1—O1 | 75.05 (6) | O3ix—Na1—Na2 | 146.46 (8) |
O2iii—Nd1—O1 | 75.05 (6) | O4viii—Na1—Na2 | 119.87 (8) |
O2iv—Nd1—O1 | 135.85 (6) | O4—Na1—Na2 | 38.49 (7) |
O2v—Nd1—O1 | 62.65 (6) | O4ix—Na1—Na2 | 78.30 (8) |
O2i—Nd1—O1ii | 62.65 (6) | Na2viii—Na1—Na2 | 113.85 (2) |
O2—Nd1—O1ii | 135.85 (6) | O3viii—Na1—Na2ix | 146.46 (9) |
O2ii—Nd1—O1ii | 62.65 (6) | O3—Na1—Na2ix | 99.67 (9) |
O2iii—Nd1—O1ii | 135.85 (6) | O3ix—Na1—Na2ix | 46.22 (7) |
O2iv—Nd1—O1ii | 75.05 (6) | O4viii—Na1—Na2ix | 78.30 (8) |
O2v—Nd1—O1ii | 75.05 (6) | O4—Na1—Na2ix | 119.87 (8) |
O1—Nd1—O1ii | 120 | O4ix—Na1—Na2ix | 38.49 (7) |
O2i—Nd1—O1iv | 75.05 (6) | Na2viii—Na1—Na2ix | 113.85 (2) |
O2—Nd1—O1iv | 75.05 (6) | Na2—Na1—Na2ix | 113.85 (2) |
O2ii—Nd1—O1iv | 135.85 (6) | O4—Na2—O4x | 164.3 (2) |
O2iii—Nd1—O1iv | 62.65 (6) | O4—Na2—F2x | 90.39 (18) |
O2iv—Nd1—O1iv | 62.65 (6) | O4x—Na2—F2x | 100.90 (19) |
O2v—Nd1—O1iv | 135.85 (6) | O4—Na2—F2 | 100.89 (19) |
O1—Nd1—O1iv | 120 | O4x—Na2—F2 | 90.39 (18) |
O1ii—Nd1—O1iv | 120 | F2x—Na2—F2 | 88.35 (18) |
C1—O1—C1v | 115.3 (4) | O4—Na2—O3 | 82.43 (11) |
C1—O1—Nd1 | 122.36 (18) | O4x—Na2—O3 | 87.46 (10) |
C1v—O1—Nd1 | 122.36 (18) | F2x—Na2—O3 | 86.05 (10) |
C2—O2—Nd1 | 128.5 (3) | F2—Na2—O3 | 173.51 (16) |
C2—O3—Na1 | 144.3 (3) | O4—Na2—O3x | 87.46 (10) |
C2—O3—Na2 | 122.1 (3) | O4x—Na2—O3x | 82.43 (11) |
Na1—O3—Na2 | 93.56 (9) | F2x—Na2—O3x | 173.51 (16) |
O1—C1—C2 | 109.3 (2) | F2—Na2—O3x | 86.05 (10) |
O3—C2—O2 | 125.1 (5) | O3—Na2—O3x | 99.73 (17) |
O3—C2—C1 | 117.7 (4) | O4—Na2—Na1 | 42.51 (8) |
O2—C2—C1 | 117.1 (3) | O4x—Na2—Na1 | 125.42 (11) |
F1—B1—F2 | 110.3 (3) | F2x—Na2—Na1 | 91.44 (10) |
F1—B1—F2vi | 110.3 (3) | F2—Na2—Na1 | 143.40 (16) |
F2—B1—F2vi | 108.7 (3) | O3—Na2—Na1 | 40.22 (6) |
F1—B1—F2vii | 110.3 (3) | O3x—Na2—Na1 | 91.11 (10) |
F2—B1—F2vii | 108.7 (3) | O4—Na2—Na1xi | 125.42 (11) |
F2vi—B1—F2vii | 108.7 (3) | O4x—Na2—Na1xi | 42.51 (8) |
B1—F2—Na2 | 129.4 (4) | F2x—Na2—Na1xi | 143.40 (16) |
O3viii—Na1—O3 | 104.44 (10) | F2—Na2—Na1xi | 91.44 (10) |
O3viii—Na1—O3ix | 104.44 (10) | O3—Na2—Na1xi | 91.11 (10) |
O3—Na1—O3ix | 104.44 (10) | O3x—Na2—Na1xi | 40.22 (6) |
O3viii—Na1—O4viii | 84.40 (10) | Na1—Na2—Na1xi | 109.49 (8) |
O3—Na1—O4viii | 164.04 (12) | Na2—O4—Na1 | 99.00 (11) |
O3ix—Na1—O4viii | 85.72 (10) |
Symmetry codes: (i) −x, −x+y, −z; (ii) −y, x−y, z; (iii) x−y, −y, −z; (iv) −x+y, −x, z; (v) y, x, −z; (vi) −y, x−y−1, z; (vii) −x+y+1, −x, z; (viii) −y+1, x−y, z; (ix) −x+y+1, −x+1, z; (x) −x+2/3, −x+y+1/3, −z+1/3; (xi) y−1/3, x−2/3, −z+1/3. |
Na5[Sm(C4H4O5)3](BF4)2·6H2O | Dx = 2.045 Mg m−3 |
Mr = 943.23 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R32 | Cell parameters from 25 reflections |
Hall symbol: R 3 2" | θ = 20.9–22.3° |
a = 9.7223 (11) Å | µ = 2.12 mm−1 |
c = 28.0728 (14) Å | T = 291 K |
V = 2298.0 (4) Å3 | Irregular block cleaved from larger crystal, colourless |
Z = 3 | 0.6 × 0.4 × 0.4 mm |
F(000) = 1389 |
Enraf Nonius CAD4 diffractometer | 1085 reflections with I > 2σ(I) |
Radiation source: Enraf Nonius FR590 | Rint = 0.025 |
Graphite monochromator | θmax = 30.0°, θmin = 2.5° |
non–profiled ω scans | h = −12→1 |
Absorption correction: ψ scan (North et al., 1968) | k = −12→1 |
Tmin = 0.352, Tmax = 0.427 | l = −39→39 |
2301 measured reflections | 3 standard reflections every 120 min |
1085 independent reflections | intensity decay: 2% |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.014 | w = 1/[σ2(Fo2) + (0.0227P)2 + 0.043P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.037 | (Δ/σ)max = 0.001 |
S = 1.13 | Δρmax = 0.47 e Å−3 |
1085 reflections | Δρmin = −0.37 e Å−3 |
78 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0034 (2) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 209 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: −0.014 (11) |
Na5[Sm(C4H4O5)3](BF4)2·6H2O | Z = 3 |
Mr = 943.23 | Mo Kα radiation |
Trigonal, R32 | µ = 2.12 mm−1 |
a = 9.7223 (11) Å | T = 291 K |
c = 28.0728 (14) Å | 0.6 × 0.4 × 0.4 mm |
V = 2298.0 (4) Å3 |
Enraf Nonius CAD4 diffractometer | 1085 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.025 |
Tmin = 0.352, Tmax = 0.427 | 3 standard reflections every 120 min |
2301 measured reflections | intensity decay: 2% |
1085 independent reflections |
R[F2 > 2σ(F2)] = 0.014 | H-atom parameters constrained |
wR(F2) = 0.037 | Δρmax = 0.47 e Å−3 |
S = 1.13 | Δρmin = −0.37 e Å−3 |
1085 reflections | Absolute structure: Flack (1983), 209 Friedel pairs |
78 parameters | Absolute structure parameter: −0.014 (11) |
0 restraints |
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 | ||
Sm1 | 0 | 0 | 0 | 0.01790 (7) | |
O1 | 0.2581 (2) | 0.2581 (2) | 0 | 0.0284 (4) | |
O2 | 0.19341 (17) | 0.03111 (19) | 0.05890 (5) | 0.0290 (3) | |
O3 | 0.4165 (2) | 0.1649 (2) | 0.09996 (6) | 0.0415 (4) | |
C1 | 0.3830 (3) | 0.2891 (3) | 0.03217 (8) | 0.0334 (5) | |
H1A | 0.4119 | 0.3852 | 0.05 | 0.04* | |
H1B | 0.4756 | 0.3047 | 0.0146 | 0.04* | |
C2 | 0.3291 (2) | 0.1499 (5) | 0.06618 (6) | 0.0254 (7) | |
B1 | 0.3333 | −0.3333 | 0.23666 (14) | 0.0402 (8) | |
F1 | 0.3333 | −0.3333 | 0.28527 (9) | 0.0805 (10) | |
F2 | 0.2504 (6) | −0.2633 (6) | 0.21968 (7) | 0.0688 (5) | |
Na1 | 0.6667 | 0.3333 | 0.13396 (5) | 0.0308 (2) | |
Na2 | 0.3333 | −0.0479 (2) | 0.1667 | 0.0526 (4) | |
O4 | 0.5909 (2) | 0.1130 (3) | 0.19069 (6) | 0.0429 (5) | |
H41 | 0.5665 | 0.1335 | 0.2199 | 0.107 (11)* | |
H42 | 0.6006 | 0.0377 | 0.2015 | 0.107 (11)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sm1 | 0.02018 (8) | 0.02018 (8) | 0.01336 (10) | 0.01009 (4) | 0 | 0 |
O1 | 0.0249 (6) | 0.0249 (6) | 0.0274 (10) | 0.0064 (8) | −0.0040 (4) | 0.0040 (4) |
O2 | 0.0276 (6) | 0.0325 (8) | 0.0242 (7) | 0.0130 (6) | −0.0080 (5) | 0.0009 (6) |
O3 | 0.0369 (8) | 0.0449 (9) | 0.0372 (8) | 0.0162 (7) | −0.0170 (7) | 0.0004 (7) |
C1 | 0.0258 (9) | 0.0349 (11) | 0.0320 (11) | 0.0095 (9) | −0.0064 (8) | 0.0013 (9) |
C2 | 0.0254 (7) | 0.0275 (18) | 0.0242 (8) | 0.0139 (8) | −0.0041 (6) | −0.0024 (8) |
B1 | 0.0429 (11) | 0.0429 (11) | 0.0347 (17) | 0.0214 (6) | 0 | 0 |
F1 | 0.1029 (16) | 0.1029 (16) | 0.0357 (12) | 0.0514 (8) | 0 | 0 |
F2 | 0.0615 (15) | 0.087 (2) | 0.0753 (10) | 0.0506 (11) | −0.008 (2) | 0.003 (2) |
Na1 | 0.0318 (3) | 0.0318 (3) | 0.0288 (5) | 0.01588 (17) | 0 | 0 |
Na2 | 0.0389 (8) | 0.0534 (7) | 0.0606 (10) | 0.0194 (4) | −0.0018 (8) | −0.0009 (4) |
O4 | 0.0489 (12) | 0.0558 (10) | 0.0315 (7) | 0.0316 (8) | −0.0073 (7) | −0.0084 (8) |
Sm1—O2i | 2.4068 (13) | B1—F2 | 1.375 (2) |
Sm1—O2 | 2.4068 (13) | B1—F2vi | 1.375 (2) |
Sm1—O2ii | 2.4068 (13) | B1—F2vii | 1.375 (2) |
Sm1—O2iii | 2.4068 (13) | F2—Na2 | 2.358 (4) |
Sm1—O2iv | 2.4068 (13) | Na1—O3viii | 2.3504 (17) |
Sm1—O2v | 2.4068 (13) | Na1—O3ix | 2.3504 (17) |
Sm1—O1 | 2.509 (2) | Na1—O4viii | 2.468 (2) |
Sm1—O1ii | 2.509 (2) | Na1—O4 | 2.468 (2) |
Sm1—O1iv | 2.509 (2) | Na1—O4ix | 2.468 (2) |
O1—C1v | 1.419 (2) | Na1—Na2viii | 3.6156 (12) |
O1—C1 | 1.419 (2) | Na1—Na2 | 3.6156 (12) |
O2—C2 | 1.262 (3) | Na1—Na2ix | 3.6156 (12) |
O3—C2 | 1.233 (2) | Na2—O4 | 2.292 (2) |
O3—Na1 | 2.3504 (17) | Na2—O4x | 2.292 (2) |
O3—Na2 | 2.602 (2) | Na2—F2x | 2.358 (4) |
C1—C2 | 1.519 (4) | Na2—O3x | 2.602 (2) |
B1—F1 | 1.365 (5) | Na2—Na1xi | 3.6157 (12) |
O2i—Sm1—O2 | 149.27 (8) | O3viii—Na1—O4 | 85.70 (6) |
O2i—Sm1—O2ii | 126.07 (7) | O3—Na1—O4 | 84.34 (6) |
O2—Sm1—O2ii | 78.00 (6) | O3ix—Na1—O4 | 163.74 (8) |
O2i—Sm1—O2iii | 78.00 (6) | O4viii—Na1—O4 | 82.83 (7) |
O2—Sm1—O2iii | 88.15 (7) | O3viii—Na1—O4ix | 163.74 (8) |
O2ii—Sm1—O2iii | 149.27 (8) | O3—Na1—O4ix | 85.70 (6) |
O2i—Sm1—O2iv | 88.15 (7) | O3ix—Na1—O4ix | 84.34 (6) |
O2—Sm1—O2iv | 78.00 (6) | O4viii—Na1—O4ix | 82.83 (7) |
O2ii—Sm1—O2iv | 78.00 (6) | O4—Na1—O4ix | 82.83 (7) |
O2iii—Sm1—O2iv | 126.07 (7) | O3viii—Na1—Na2viii | 45.89 (5) |
O2i—Sm1—O2v | 78.00 (6) | O3—Na1—Na2viii | 146.07 (5) |
O2—Sm1—O2v | 126.07 (7) | O3ix—Na1—Na2viii | 100.12 (5) |
O2ii—Sm1—O2v | 88.15 (7) | O4viii—Na1—Na2viii | 38.79 (5) |
O2iii—Sm1—O2v | 78.00 (6) | O4—Na1—Na2viii | 77.88 (5) |
O2iv—Sm1—O2v | 149.27 (8) | O4ix—Na1—Na2viii | 119.85 (5) |
O2i—Sm1—O1 | 135.93 (4) | O3viii—Na1—Na2 | 100.12 (5) |
O2—Sm1—O1 | 63.03 (4) | O3—Na1—Na2 | 45.89 (5) |
O2ii—Sm1—O1 | 74.63 (4) | O3ix—Na1—Na2 | 146.07 (5) |
O2iii—Sm1—O1 | 74.63 (4) | O4viii—Na1—Na2 | 119.85 (5) |
O2iv—Sm1—O1 | 135.93 (4) | O4—Na1—Na2 | 38.79 (5) |
O2v—Sm1—O1 | 63.03 (4) | O4ix—Na1—Na2 | 77.88 (5) |
O2i—Sm1—O1ii | 63.03 (4) | Na2viii—Na1—Na2 | 113.784 (17) |
O2—Sm1—O1ii | 135.93 (4) | O3viii—Na1—Na2ix | 146.07 (5) |
O2ii—Sm1—O1ii | 63.03 (4) | O3—Na1—Na2ix | 100.12 (5) |
O2iii—Sm1—O1ii | 135.93 (4) | O3ix—Na1—Na2ix | 45.89 (5) |
O2iv—Sm1—O1ii | 74.63 (4) | O4viii—Na1—Na2ix | 77.88 (5) |
O2v—Sm1—O1ii | 74.63 (4) | O4—Na1—Na2ix | 119.85 (5) |
O1—Sm1—O1ii | 120 | O4ix—Na1—Na2ix | 38.79 (5) |
O2i—Sm1—O1iv | 74.63 (4) | Na2viii—Na1—Na2ix | 113.784 (17) |
O2—Sm1—O1iv | 74.63 (4) | Na2—Na1—Na2ix | 113.784 (17) |
O2ii—Sm1—O1iv | 135.93 (4) | O4—Na2—O4x | 164.31 (14) |
O2iii—Sm1—O1iv | 63.03 (4) | O4—Na2—F2x | 90.19 (12) |
O2iv—Sm1—O1iv | 63.03 (4) | O4x—Na2—F2x | 101.09 (12) |
O2v—Sm1—O1iv | 135.93 (4) | O4—Na2—F2 | 101.09 (12) |
O1—Sm1—O1iv | 120 | O4x—Na2—F2 | 90.19 (12) |
O1ii—Sm1—O1iv | 120 | F2x—Na2—F2 | 88.42 (11) |
C1v—O1—C1 | 115.5 (2) | O4—Na2—O3 | 82.52 (7) |
C1v—O1—Sm1 | 122.27 (12) | O4x—Na2—O3 | 87.46 (7) |
C1—O1—Sm1 | 122.27 (12) | F2x—Na2—O3 | 85.67 (6) |
C2—O2—Sm1 | 128.29 (18) | F2—Na2—O3 | 173.09 (10) |
C2—O3—Na1 | 143.8 (2) | O4—Na2—O3x | 87.46 (7) |
C2—O3—Na2 | 122.54 (19) | O4x—Na2—O3x | 82.51 (7) |
Na1—O3—Na2 | 93.66 (6) | F2x—Na2—O3x | 173.09 (10) |
O1—C1—C2 | 109.47 (17) | F2—Na2—O3x | 85.67 (6) |
O3—C2—O2 | 125.2 (3) | O3—Na2—O3x | 100.45 (11) |
O3—C2—C1 | 117.9 (2) | O4—Na2—Na1 | 42.41 (6) |
O2—C2—C1 | 116.79 (19) | O4x—Na2—Na1 | 125.51 (7) |
F1—B1—F2 | 110.28 (17) | F2x—Na2—Na1 | 91.34 (7) |
F1—B1—F2vi | 110.28 (17) | F2—Na2—Na1 | 143.50 (11) |
F2—B1—F2vi | 108.65 (18) | O3—Na2—Na1 | 40.45 (4) |
F1—B1—F2vii | 110.28 (17) | O3x—Na2—Na1 | 91.30 (6) |
F2—B1—F2vii | 108.65 (18) | O4—Na2—Na1xi | 125.51 (7) |
F2vi—B1—F2vii | 108.65 (18) | O4x—Na2—Na1xi | 42.41 (6) |
B1—F2—Na2 | 129.3 (3) | F2x—Na2—Na1xi | 143.51 (11) |
O3viii—Na1—O3 | 104.63 (6) | F2—Na2—Na1xi | 91.34 (6) |
O3viii—Na1—O3ix | 104.63 (6) | O3—Na2—Na1xi | 91.30 (6) |
O3—Na1—O3ix | 104.63 (6) | O3x—Na2—Na1xi | 40.45 (4) |
O3viii—Na1—O4viii | 84.34 (6) | Na1—Na2—Na1xi | 109.51 (5) |
O3—Na1—O4viii | 163.74 (8) | Na2—O4—Na1 | 98.79 (7) |
O3ix—Na1—O4viii | 85.70 (6) |
Symmetry codes: (i) −x, −x+y, −z; (ii) −y, x−y, z; (iii) x−y, −y, −z; (iv) −x+y, −x, z; (v) y, x, −z; (vi) −y, x−y−1, z; (vii) −x+y+1, −x, z; (viii) −y+1, x−y, z; (ix) −x+y+1, −x+1, z; (x) −x+2/3, −x+y+1/3, −z+1/3; (xi) y−1/3, x−2/3, −z+1/3. |
Na5[Gd(C4H4O5)3](BF4)2·6H2O | Dx = 2.071 Mg m−3 |
Mr = 950.13 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R32 | Cell parameters from 25 reflections |
Hall symbol: R 3 2" | θ = 12.1–15.2° |
a = 9.7041 (10) Å | µ = 2.38 mm−1 |
c = 28.025 (6) Å | T = 291 K |
V = 2285.5 (6) Å3 | Prism, colourless |
Z = 3 | 0.5 × 0.45 × 0.35 mm |
F(000) = 1395 |
Enraf Nonius CAD-4 diffractometer | 1078 reflections with I > 2σ(I) |
Radiation source: Enraf Nonius FR590 | Rint = 0.013 |
Graphite monochromator | θmax = 30.0°, θmin = 2.5° |
non–profiled ω scans | h = −13→1 |
Absorption correction: ψ scan (North et al., 1968) | k = −1→11 |
Tmin = 0.336, Tmax = 0.433 | l = −39→39 |
2033 measured reflections | 3 standard reflections every 120 min |
1078 independent reflections | intensity decay: 3% |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.012 | w = 1/[σ2(Fo2) + (0.0226P)2 + 0.5279P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.032 | (Δ/σ)max = 0.001 |
S = 1.07 | Δρmax = 0.38 e Å−3 |
1078 reflections | Δρmin = −0.26 e Å−3 |
78 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00258 (15) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 206 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: −0.005 (10) |
Na5[Gd(C4H4O5)3](BF4)2·6H2O | Z = 3 |
Mr = 950.13 | Mo Kα radiation |
Trigonal, R32 | µ = 2.38 mm−1 |
a = 9.7041 (10) Å | T = 291 K |
c = 28.025 (6) Å | 0.5 × 0.45 × 0.35 mm |
V = 2285.5 (6) Å3 |
Enraf Nonius CAD-4 diffractometer | 1078 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.013 |
Tmin = 0.336, Tmax = 0.433 | 3 standard reflections every 120 min |
2033 measured reflections | intensity decay: 3% |
1078 independent reflections |
R[F2 > 2σ(F2)] = 0.012 | H-atom parameters constrained |
wR(F2) = 0.032 | Δρmax = 0.38 e Å−3 |
S = 1.07 | Δρmin = −0.26 e Å−3 |
1078 reflections | Absolute structure: Flack (1983), 206 Friedel pairs |
78 parameters | Absolute structure parameter: −0.005 (10) |
0 restraints |
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 | ||
Gd1 | 0 | 0 | 0 | 0.01797 (6) | |
O1 | −0.2566 (2) | −0.2566 (2) | 0 | 0.0279 (4) | |
O2 | −0.19123 (16) | −0.02868 (17) | −0.05864 (5) | 0.0283 (3) | |
O3 | −0.4154 (2) | −0.1616 (2) | −0.09977 (5) | 0.0404 (4) | |
C1 | −0.3823 (2) | −0.2874 (3) | −0.03196 (7) | 0.0319 (4) | |
H1A | −0.4746 | −0.3022 | −0.0142 | 0.038* | |
H1B | −0.4122 | −0.384 | −0.0498 | 0.038* | |
C2 | −0.32749 (19) | −0.1480 (4) | −0.06592 (5) | 0.0251 (6) | |
B1 | −0.3333 | 0.3333 | −0.23679 (12) | 0.0393 (7) | |
F1 | −0.3333 | 0.3333 | −0.28550 (8) | 0.0783 (9) | |
F2 | −0.2482 (5) | 0.2641 (5) | −0.21977 (7) | 0.0668 (5) | |
Na1 | −0.6667 | −0.3333 | −0.13370 (4) | 0.0309 (2) | |
Na2 | −0.3333 | 0.04815 (18) | −0.1667 | 0.0499 (4) | |
O4 | −0.5922 (2) | −0.1134 (2) | −0.19064 (6) | 0.0418 (4) | |
H41 | −0.5676 | −0.1335 | −0.2193 | 0.079 (8)* | |
H42 | −0.5854 | −0.0383 | −0.2018 | 0.079 (8)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Gd1 | 0.02037 (7) | 0.02037 (7) | 0.01318 (7) | 0.01019 (3) | 0 | 0 |
O1 | 0.0249 (6) | 0.0249 (6) | 0.0271 (8) | 0.0074 (7) | −0.0050 (4) | 0.0050 (4) |
O2 | 0.0272 (6) | 0.0311 (7) | 0.0242 (5) | 0.0129 (6) | −0.0066 (5) | 0.0015 (5) |
O3 | 0.0356 (7) | 0.0447 (8) | 0.0358 (6) | 0.0163 (7) | −0.0160 (6) | 0.0012 (6) |
C1 | 0.0255 (8) | 0.0324 (9) | 0.0302 (8) | 0.0087 (8) | −0.0073 (7) | 0.0028 (8) |
C2 | 0.0262 (6) | 0.0287 (17) | 0.0230 (6) | 0.0155 (7) | −0.0041 (5) | −0.0021 (7) |
B1 | 0.0421 (10) | 0.0421 (10) | 0.0337 (14) | 0.0211 (5) | 0 | 0 |
F1 | 0.1010 (15) | 0.1010 (15) | 0.0328 (10) | 0.0505 (7) | 0 | 0 |
F2 | 0.0650 (15) | 0.077 (2) | 0.0740 (9) | 0.0476 (10) | −0.0099 (18) | 0.0011 (19) |
Na1 | 0.0321 (3) | 0.0321 (3) | 0.0284 (4) | 0.01606 (16) | 0 | 0 |
Na2 | 0.0390 (8) | 0.0519 (7) | 0.0545 (8) | 0.0195 (4) | −0.0020 (7) | −0.0010 (3) |
O4 | 0.0476 (11) | 0.0552 (10) | 0.0290 (6) | 0.0304 (8) | −0.0060 (6) | −0.0082 (7) |
Gd1—O2i | 2.3887 (13) | B1—F2 | 1.384 (2) |
Gd1—O2 | 2.3887 (13) | B1—F2vi | 1.384 (2) |
Gd1—O2ii | 2.3887 (13) | B1—F2vii | 1.384 (2) |
Gd1—O2iii | 2.3887 (13) | F2—Na2 | 2.358 (4) |
Gd1—O2iv | 2.3887 (13) | Na1—O3viii | 2.3585 (16) |
Gd1—O2v | 2.3887 (13) | Na1—O3ix | 2.3585 (16) |
Gd1—O1 | 2.490 (2) | Na1—O4 | 2.466 (2) |
Gd1—O1ii | 2.490 (2) | Na1—O4viii | 2.466 (2) |
Gd1—O1iv | 2.490 (2) | Na1—O4ix | 2.466 (2) |
O1—C1 | 1.420 (2) | Na1—Na2viii | 3.6120 (11) |
O1—C1v | 1.420 (2) | Na1—Na2 | 3.6120 (11) |
O2—C2 | 1.265 (2) | Na1—Na2ix | 3.6120 (11) |
O3—C2 | 1.238 (2) | Na2—O4 | 2.2985 (18) |
O3—Na1 | 2.3585 (16) | Na2—O4x | 2.2985 (18) |
O3—Na2 | 2.583 (2) | Na2—F2x | 2.357 (4) |
C1—C2 | 1.516 (4) | Na2—O3x | 2.583 (2) |
B1—F1 | 1.365 (4) | Na2—Na1xi | 3.6121 (11) |
O2i—Gd1—O2 | 148.44 (7) | O3viii—Na1—O4viii | 84.12 (6) |
O2i—Gd1—O2ii | 126.94 (7) | O3—Na1—O4viii | 163.41 (7) |
O2—Gd1—O2ii | 77.87 (5) | O3ix—Na1—O4viii | 85.80 (6) |
O2i—Gd1—O2iii | 77.87 (5) | O4—Na1—O4viii | 82.64 (6) |
O2—Gd1—O2iii | 88.12 (7) | O3viii—Na1—O4ix | 163.41 (7) |
O2ii—Gd1—O2iii | 148.44 (7) | O3—Na1—O4ix | 85.80 (6) |
O2i—Gd1—O2iv | 88.12 (7) | O3ix—Na1—O4ix | 84.12 (6) |
O2—Gd1—O2iv | 77.87 (5) | O4—Na1—O4ix | 82.64 (6) |
O2ii—Gd1—O2iv | 77.87 (5) | O4viii—Na1—O4ix | 82.64 (6) |
O2iii—Gd1—O2iv | 126.94 (7) | O3viii—Na1—Na2viii | 45.52 (4) |
O2i—Gd1—O2v | 77.87 (5) | O3—Na1—Na2viii | 145.60 (5) |
O2—Gd1—O2v | 126.94 (7) | O3ix—Na1—Na2viii | 100.65 (5) |
O2ii—Gd1—O2v | 88.12 (7) | O4—Na1—Na2viii | 77.53 (5) |
O2iii—Gd1—O2v | 77.87 (5) | O4viii—Na1—Na2viii | 39.00 (4) |
O2iv—Gd1—O2v | 148.44 (7) | O4ix—Na1—Na2viii | 119.76 (5) |
O2i—Gd1—O1 | 135.94 (3) | O3viii—Na1—Na2 | 100.65 (5) |
O2—Gd1—O1 | 63.47 (3) | O3—Na1—Na2 | 45.52 (4) |
O2ii—Gd1—O1 | 74.22 (4) | O3ix—Na1—Na2 | 145.60 (5) |
O2iii—Gd1—O1 | 74.22 (4) | O4—Na1—Na2 | 39.00 (4) |
O2iv—Gd1—O1 | 135.94 (3) | O4viii—Na1—Na2 | 119.76 (5) |
O2v—Gd1—O1 | 63.47 (3) | O4ix—Na1—Na2 | 77.53 (5) |
O2i—Gd1—O1ii | 63.47 (3) | Na2viii—Na1—Na2 | 113.693 (15) |
O2—Gd1—O1ii | 135.94 (3) | O3viii—Na1—Na2ix | 145.60 (5) |
O2ii—Gd1—O1ii | 63.47 (3) | O3—Na1—Na2ix | 100.65 (5) |
O2iii—Gd1—O1ii | 135.94 (3) | O3ix—Na1—Na2ix | 45.52 (4) |
O2iv—Gd1—O1ii | 74.22 (4) | O4—Na1—Na2ix | 119.76 (5) |
O2v—Gd1—O1ii | 74.22 (4) | O4viii—Na1—Na2ix | 77.53 (5) |
O1—Gd1—O1ii | 120 | O4ix—Na1—Na2ix | 39.00 (4) |
O2i—Gd1—O1iv | 74.22 (4) | Na2viii—Na1—Na2ix | 113.693 (15) |
O2—Gd1—O1iv | 74.22 (4) | Na2—Na1—Na2ix | 113.693 (15) |
O2ii—Gd1—O1iv | 135.94 (3) | O4—Na2—O4x | 164.42 (13) |
O2iii—Gd1—O1iv | 63.47 (3) | O4—Na2—F2x | 89.66 (11) |
O2iv—Gd1—O1iv | 63.47 (3) | O4x—Na2—F2x | 101.50 (12) |
O2v—Gd1—O1iv | 135.94 (3) | O4—Na2—F2 | 101.50 (12) |
O1—Gd1—O1iv | 120 | O4x—Na2—F2 | 89.66 (11) |
O1ii—Gd1—O1iv | 120 | F2x—Na2—F2 | 88.91 (11) |
C1—O1—C1v | 115.3 (2) | O4—Na2—O3 | 82.73 (7) |
C1—O1—Gd1 | 122.36 (11) | O4x—Na2—O3 | 87.41 (6) |
C1v—O1—Gd1 | 122.36 (11) | F2x—Na2—O3 | 85.03 (6) |
C2—O2—Gd1 | 127.83 (15) | F2—Na2—O3 | 172.60 (10) |
C2—O3—Na1 | 142.97 (18) | O4—Na2—O3x | 87.41 (6) |
C2—O3—Na2 | 123.19 (17) | O4x—Na2—O3x | 82.73 (7) |
Na1—O3—Na2 | 93.82 (5) | F2x—Na2—O3x | 172.60 (10) |
O1—C1—C2 | 109.07 (15) | F2—Na2—O3x | 85.03 (6) |
O3—C2—O2 | 124.8 (3) | O3—Na2—O3x | 101.32 (10) |
O3—C2—C1 | 118.0 (2) | O4—Na2—Na1 | 42.47 (5) |
O2—C2—C1 | 117.09 (17) | O4x—Na2—Na1 | 125.54 (7) |
F1—B1—F2 | 110.16 (15) | F2x—Na2—Na1 | 90.87 (7) |
F1—B1—F2vi | 110.16 (15) | F2—Na2—Na1 | 143.97 (10) |
F2—B1—F2vi | 108.78 (16) | O3—Na2—Na1 | 40.66 (4) |
F1—B1—F2vii | 110.16 (15) | O3x—Na2—Na1 | 91.55 (6) |
F2—B1—F2vii | 108.78 (16) | O4—Na2—Na1xi | 125.54 (7) |
F2vi—B1—F2vii | 108.78 (16) | O4x—Na2—Na1xi | 42.47 (5) |
B1—F2—Na2 | 128.3 (3) | F2x—Na2—Na1xi | 143.97 (10) |
O3viii—Na1—O3 | 104.84 (5) | F2—Na2—Na1xi | 90.87 (7) |
O3viii—Na1—O3ix | 104.84 (5) | O3—Na2—Na1xi | 91.55 (6) |
O3—Na1—O3ix | 104.84 (5) | O3x—Na2—Na1xi | 40.65 (4) |
O3viii—Na1—O4 | 85.80 (6) | Na1—Na2—Na1xi | 109.50 (5) |
O3—Na1—O4 | 84.12 (6) | Na2—O4—Na1 | 98.53 (7) |
O3ix—Na1—O4 | 163.41 (7) |
Symmetry codes: (i) −x, −x+y, −z; (ii) −y, x−y, z; (iii) x−y, −y, −z; (iv) −x+y, −x, z; (v) y, x, −z; (vi) −y, x−y+1, z; (vii) −x+y−1, −x, z; (viii) −y−1, x−y, z; (ix) −x+y−1, −x−1, z; (x) −x−2/3, −x+y−1/3, −z−1/3; (xi) y+1/3, x+2/3, −z−1/3. |
Experimental details
(I) | (II) | (III) | |
Crystal data | |||
Chemical formula | Na5[Nd(C4H4O5)3](BF4)2·6H2O | Na5[Sm(C4H4O5)3](BF4)2·6H2O | Na5[Gd(C4H4O5)3](BF4)2·6H2O |
Mr | 937.12 | 943.23 | 950.13 |
Crystal system, space group | Trigonal, R32 | Trigonal, R32 | Trigonal, R32 |
Temperature (K) | 291 | 291 | 291 |
a, c (Å) | 9.7508 (7), 28.177 (2) | 9.7223 (11), 28.0728 (14) | 9.7041 (10), 28.025 (6) |
V (Å3) | 2320.1 (3) | 2298.0 (4) | 2285.5 (6) |
Z | 3 | 3 | 3 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 1.88 | 2.12 | 2.38 |
Crystal size (mm) | 0.55 × 0.45 × 0.1 | 0.6 × 0.4 × 0.4 | 0.5 × 0.45 × 0.35 |
Data collection | |||
Diffractometer | Enraf Nonius CAD-4 diffractometer | Enraf Nonius CAD4 diffractometer | Enraf Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) | ψ scan (North et al., 1968) | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.425, 0.834 | 0.352, 0.427 | 0.336, 0.433 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1134, 1001, 1001 | 2301, 1085, 1085 | 2033, 1078, 1078 |
Rint | 0.030 | 0.025 | 0.013 |
(sin θ/λ)max (Å−1) | 0.703 | 0.703 | 0.703 |
Refinement | |||
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.055, 1.13 | 0.014, 0.037, 1.13 | 0.012, 0.032, 1.07 |
No. of reflections | 1001 | 1085 | 1078 |
No. of parameters | 77 | 78 | 78 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.47, −0.51 | 0.47, −0.37 | 0.38, −0.26 |
Absolute structure | Flack (1983), 121 Friedel pairs | Flack (1983), 209 Friedel pairs | Flack (1983), 206 Friedel pairs |
Absolute structure parameter | −0.010 (18) | −0.014 (11) | −0.005 (10) |
Computer programs: CAD-4 EXPRESS (Enraf Nonius, 1994), CAD-4 EXPRESS, XCAD4 (Harms & Wocadlo, 1995), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), WinGX (Farrugia, 1999).
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