Seven Group 1 and Group 2 1,5-naphthalenedisulfonates (1,5-nds) have been synthesized and structurally characterized by single-crystal X-ray diffraction, IR spectroscopy and thermal gravimetric analysis. For Group 1 metal complexes, with
M = Li
+ (1), Na
+ (2) and K
+ (3), all crystallize in the same space group (
P2
1/
c) with the same composition, [
M2(1,5-nds)(H
2O)
2]. They adopt similar three-dimensional packing arrangements with the metal-sulfonate inorganic layers pillared by naphthalene rings. However, the coordination behavior of three metal cations toward the SO
group and water molecule are different, resulting in different architectures for the inorganic portion. For Group 2 complexes with
M = Mg
2+ (4), Ca
2+ (5), Sr
2+ (6) and Ba
2+ (7), Mg
2+ shows no direct coordination by the SO
group while Ca
2+ is coordinated by four SO
groups and a two-dimensional network is formed. Complexes (6) and (7) are isostructural, adopting the same three-dimensional, inorganic-organic pillared framework as seen for (1)-(3). The coordination behavior of the metal cations in these structures neatly illustrates the increase in coordination strength with decreasing charge/radius ratio for Group 1 and Group 2 metal cations with large organic anions.
Supporting information
CCDC references: 152299; 152300; 152301; 152302; 152303; 152304; 152305
For all compounds, data collection: Bruker SMART; cell refinement: Bruker SMART; data reduction: Bruker SHELXTL; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Bruker SHELXTL; software used to prepare material for publication: Bruker SHELXTL.
(1) Dilithium 1,5-naphthalenedisulfonate dihydrate
top
Crystal data top
2(Li+)·C10H6O6S22−·2(H2O) | F(000) = 344 |
Mr = 336.18 | Dx = 1.664 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.8901 (17) Å | θ = 4.4–30.0° |
b = 7.8842 (13) Å | µ = 0.43 mm−1 |
c = 8.0619 (13) Å | T = 293 K |
β = 104.228 (3)° | Plate, colorless |
V = 670.96 (19) Å3 | 0.33 × 0.21 × 0.06 mm |
Z = 2 | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1727 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.018 |
Graphite monochromator | θmax = 30.0°, θmin = 4.4° |
phi and ω scans | h = −13→15 |
4629 measured reflections | k = −9→11 |
1940 independent reflections | l = −10→11 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0612P)2 + 0.1528P] where P = (Fo2 + 2Fc2)/3 |
1940 reflections | (Δ/σ)max = 0.001 |
108 parameters | Δρmax = 0.45 e Å−3 |
0 restraints | Δρmin = −0.59 e Å−3 |
Crystal data top
2(Li+)·C10H6O6S22−·2(H2O) | V = 670.96 (19) Å3 |
Mr = 336.18 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.8901 (17) Å | µ = 0.43 mm−1 |
b = 7.8842 (13) Å | T = 293 K |
c = 8.0619 (13) Å | 0.33 × 0.21 × 0.06 mm |
β = 104.228 (3)° | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1727 reflections with I > 2σ(I) |
4629 measured reflections | Rint = 0.018 |
1940 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.035 | 0 restraints |
wR(F2) = 0.101 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | Δρmax = 0.45 e Å−3 |
1940 reflections | Δρmin = −0.59 e Å−3 |
108 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
S1 | 0.82435 (3) | 1.01202 (4) | 0.58212 (4) | 0.01804 (12) | |
Li1 | 0.9093 (2) | 0.6449 (3) | 0.7512 (3) | 0.0245 (5) | |
O1 | 0.85128 (9) | 0.87409 (13) | 0.70623 (13) | 0.0271 (2) | |
O2 | 0.82737 (10) | 0.95808 (16) | 0.41179 (14) | 0.0305 (2) | |
O3 | 0.90527 (9) | 1.15798 (13) | 0.64168 (14) | 0.0279 (2) | |
OW | 0.86614 (13) | 0.51191 (16) | 0.54838 (17) | 0.0346 (3) | |
HW1 | 0.858 (2) | 0.543 (3) | 0.452 (4) | 0.052 (7)* | |
HW2 | 0.891 (2) | 0.409 (3) | 0.550 (3) | 0.050 (6)* | |
C1 | 0.66697 (11) | 1.07846 (15) | 0.57230 (16) | 0.0184 (2) | |
C2 | 0.64935 (12) | 1.23803 (17) | 0.63050 (18) | 0.0236 (3) | |
H2A | 0.7189 | 1.3065 | 0.6769 | 0.028* | |
C3 | 0.56217 (11) | 0.96836 (16) | 0.50425 (16) | 0.0178 (2) | |
C4 | 0.57708 (12) | 0.80127 (17) | 0.44675 (18) | 0.0239 (3) | |
H4A | 0.6580 | 0.7589 | 0.4546 | 0.029* | |
C5 | 0.47411 (13) | 0.70207 (18) | 0.3801 (2) | 0.0270 (3) | |
H5A | 0.4856 | 0.5936 | 0.3412 | 0.032* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
S1 | 0.01563 (18) | 0.01743 (18) | 0.02027 (19) | 0.00080 (9) | 0.00289 (12) | −0.00071 (10) |
Li1 | 0.0248 (11) | 0.0223 (11) | 0.0264 (12) | 0.0018 (9) | 0.0064 (9) | 0.0020 (9) |
O1 | 0.0299 (5) | 0.0201 (5) | 0.0284 (5) | 0.0053 (4) | 0.0016 (4) | 0.0042 (4) |
O2 | 0.0260 (5) | 0.0428 (6) | 0.0246 (5) | 0.0033 (4) | 0.0097 (4) | −0.0062 (4) |
O3 | 0.0178 (4) | 0.0200 (5) | 0.0436 (6) | −0.0025 (3) | 0.0029 (4) | −0.0029 (4) |
OW | 0.0512 (8) | 0.0267 (6) | 0.0270 (6) | 0.0001 (5) | 0.0116 (6) | 0.0006 (4) |
C1 | 0.0163 (5) | 0.0181 (6) | 0.0204 (6) | 0.0004 (4) | 0.0036 (4) | −0.0014 (4) |
C2 | 0.0203 (6) | 0.0201 (6) | 0.0298 (7) | −0.0025 (5) | 0.0048 (5) | −0.0061 (5) |
C3 | 0.0172 (6) | 0.0168 (5) | 0.0193 (6) | 0.0004 (4) | 0.0041 (4) | −0.0019 (4) |
C4 | 0.0198 (6) | 0.0193 (6) | 0.0324 (7) | 0.0031 (5) | 0.0063 (5) | −0.0054 (5) |
C5 | 0.0253 (6) | 0.0178 (6) | 0.0382 (8) | 0.0005 (5) | 0.0084 (5) | −0.0096 (5) |
Geometric parameters (Å, º) top
S1—O2 | 1.4456 (11) | O3—Li1iv | 1.994 (3) |
S1—O3 | 1.4572 (10) | C1—C2 | 1.3726 (17) |
S1—O1 | 1.4579 (10) | C1—C3 | 1.4315 (17) |
S1—C1 | 1.7753 (12) | C2—C5v | 1.4077 (18) |
Li1—OW | 1.902 (3) | C3—C4 | 1.4191 (17) |
Li1—O1 | 1.919 (3) | C3—C3v | 1.429 (2) |
Li1—O2i | 1.924 (3) | C4—C5 | 1.3644 (18) |
Li1—O3ii | 1.994 (3) | C5—C2v | 1.4077 (18) |
O2—Li1iii | 1.924 (3) | | |
| | | |
O2—S1—O3 | 113.09 (7) | S1—O1—Li1 | 146.43 (10) |
O2—S1—O1 | 112.63 (7) | S1—O2—Li1iii | 152.39 (10) |
O3—S1—O1 | 111.07 (6) | S1—O3—Li1iv | 124.60 (9) |
O2—S1—C1 | 106.95 (6) | C2—C1—C3 | 121.44 (11) |
O3—S1—C1 | 106.30 (6) | C2—C1—S1 | 118.02 (10) |
O1—S1—C1 | 106.25 (6) | C3—C1—S1 | 120.54 (9) |
OW—Li1—O1 | 110.87 (13) | C1—C2—C5v | 119.90 (12) |
OW—Li1—O2i | 106.76 (13) | C4—C3—C3v | 119.45 (14) |
O1—Li1—O2i | 109.80 (12) | C4—C3—C1 | 122.94 (11) |
OW—Li1—O3ii | 114.27 (13) | C3v—C3—C1 | 117.62 (14) |
O1—Li1—O3ii | 106.54 (12) | C5—C4—C3 | 120.79 (12) |
O2i—Li1—O3ii | 108.56 (12) | C4—C5—C2v | 120.78 (12) |
| | | |
O2—S1—O1—Li1 | 10.66 (19) | O1—S1—C1—C2 | 113.58 (11) |
O3—S1—O1—Li1 | −117.37 (17) | O2—S1—C1—C3 | 53.64 (12) |
C1—S1—O1—Li1 | 127.44 (17) | O3—S1—C1—C3 | 174.73 (10) |
OW—Li1—O1—S1 | −31.3 (2) | O1—S1—C1—C3 | −66.89 (12) |
O2i—Li1—O1—S1 | −149.06 (13) | C3—C1—C2—C5v | −1.6 (2) |
O3ii—Li1—O1—S1 | 93.57 (18) | S1—C1—C2—C5v | 177.93 (11) |
O3—S1—O2—Li1iii | 71.5 (2) | C2—C1—C3—C4 | −178.46 (13) |
O1—S1—O2—Li1iii | −55.5 (2) | S1—C1—C3—C4 | 2.02 (18) |
C1—S1—O2—Li1iii | −171.9 (2) | C2—C1—C3—C3v | 1.2 (2) |
O2—S1—O3—Li1iv | −83.66 (12) | S1—C1—C3—C3v | −178.30 (12) |
O1—S1—O3—Li1iv | 44.12 (13) | C3v—C3—C4—C5 | 1.5 (2) |
C1—S1—O3—Li1iv | 159.28 (11) | C1—C3—C4—C5 | −178.86 (13) |
O2—S1—C1—C2 | −125.90 (12) | C3—C4—C5—C2v | −1.1 (2) |
O3—S1—C1—C2 | −4.81 (13) | | |
Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) −x+2, y−1/2, −z+3/2; (iii) x, −y+3/2, z−1/2; (iv) −x+2, y+1/2, −z+3/2; (v) −x+1, −y+2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···O1iii | 0.80 (3) | 2.07 (3) | 2.8676 (17) | 175 (2) |
OW—HW2···O3vi | 0.85 (3) | 2.11 (3) | 2.8942 (17) | 153 (2) |
Symmetry codes: (iii) x, −y+3/2, z−1/2; (vi) x, y−1, z. |
(2) disodium 1,5-naphthalenedisulfonate hihydrate
top
Crystal data top
2(Na+)·C10H6O6S22−·2(H2O) | F(000) = 376 |
Mr = 368.28 | Dx = 1.777 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.6398 (17) Å | θ = 4.4–28.3° |
b = 5.5507 (8) Å | µ = 0.49 mm−1 |
c = 10.7148 (16) Å | T = 293 K |
β = 96.187 (3)° | Block, colorless |
V = 688.24 (17) Å3 | 0.33 × 0.16 × 0.11 mm |
Z = 2 | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1516 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.026 |
Graphite monochromator | θmax = 28.3°, θmin = 4.4° |
phi and ω scans | h = −15→15 |
4234 measured reflections | k = −5→7 |
1692 independent reflections | l = −12→14 |
Refinement top
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)] = 0.031 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.092 | w = 1/[σ2(Fo2) + (0.0547P)2 + 0.2432P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.012 |
1692 reflections | Δρmax = 0.36 e Å−3 |
109 parameters | Δρmin = −0.49 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.164 (9) |
Crystal data top
2(Na+)·C10H6O6S22−·2(H2O) | V = 688.24 (17) Å3 |
Mr = 368.28 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.6398 (17) Å | µ = 0.49 mm−1 |
b = 5.5507 (8) Å | T = 293 K |
c = 10.7148 (16) Å | 0.33 × 0.16 × 0.11 mm |
β = 96.187 (3)° | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1516 reflections with I > 2σ(I) |
4234 measured reflections | Rint = 0.026 |
1692 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | Δρmax = 0.36 e Å−3 |
1692 reflections | Δρmin = −0.49 e Å−3 |
109 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Na1 | 0.60064 (6) | −0.09071 (11) | 0.68026 (6) | 0.0302 (2) | |
S1 | 0.70611 (3) | 0.07573 (6) | 0.99844 (3) | 0.02210 (16) | |
O1 | 0.68449 (10) | 0.1058 (2) | 0.86273 (11) | 0.0297 (3) | |
O2 | 0.64795 (10) | 0.2544 (2) | 1.06735 (12) | 0.0358 (3) | |
O3 | 0.68285 (10) | −0.1713 (2) | 1.03583 (10) | 0.0298 (3) | |
OW | 0.41353 (12) | 0.0735 (2) | 0.68658 (13) | 0.0335 (3) | |
C1 | 0.85708 (12) | 0.1246 (2) | 1.03620 (13) | 0.0217 (3) | |
C2 | 0.94004 (12) | −0.0257 (3) | 0.98395 (13) | 0.0212 (3) | |
C3 | 0.90822 (13) | −0.2221 (3) | 0.90238 (14) | 0.0253 (3) | |
H3A | 0.8304 | −0.2567 | 0.8809 | 0.030* | |
C4 | 0.89168 (13) | 0.3125 (3) | 1.11398 (14) | 0.0264 (3) | |
H4A | 0.8367 | 0.4088 | 1.1466 | 0.032* | |
C5 | 1.01005 (14) | 0.3606 (3) | 1.14486 (15) | 0.0279 (3) | |
H5A | 1.0327 | 0.4884 | 1.1981 | 0.033* | |
HW1 | 0.388 (3) | 0.134 (7) | 0.612 (4) | 0.098 (12)* | |
HW2 | 0.377 (3) | −0.040 (6) | 0.687 (3) | 0.078 (10)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.0370 (4) | 0.0268 (3) | 0.0280 (4) | 0.0027 (2) | 0.0095 (3) | 0.0013 (2) |
S1 | 0.0244 (2) | 0.0196 (2) | 0.0227 (2) | −0.00025 (12) | 0.00433 (14) | −0.00181 (12) |
O1 | 0.0346 (6) | 0.0292 (6) | 0.0242 (6) | 0.0009 (4) | −0.0023 (4) | 0.0024 (4) |
O2 | 0.0310 (6) | 0.0336 (6) | 0.0438 (7) | 0.0029 (5) | 0.0091 (5) | −0.0147 (5) |
O3 | 0.0351 (6) | 0.0241 (5) | 0.0314 (6) | −0.0056 (4) | 0.0091 (5) | 0.0025 (4) |
OW | 0.0396 (7) | 0.0251 (6) | 0.0355 (7) | −0.0016 (5) | 0.0035 (5) | −0.0003 (5) |
C1 | 0.0246 (7) | 0.0201 (6) | 0.0207 (6) | −0.0001 (5) | 0.0036 (5) | 0.0000 (5) |
C2 | 0.0269 (7) | 0.0191 (6) | 0.0181 (6) | −0.0005 (5) | 0.0044 (5) | −0.0003 (5) |
C3 | 0.0261 (7) | 0.0243 (7) | 0.0254 (7) | −0.0033 (5) | 0.0022 (5) | −0.0042 (5) |
C4 | 0.0295 (7) | 0.0237 (7) | 0.0266 (7) | 0.0018 (6) | 0.0056 (6) | −0.0050 (5) |
C5 | 0.0335 (8) | 0.0227 (7) | 0.0271 (7) | −0.0030 (6) | 0.0022 (6) | −0.0086 (6) |
Geometric parameters (Å, º) top
Na1—O3i | 2.3185 (12) | O2—Na1v | 2.3230 (13) |
Na1—O2ii | 2.3230 (13) | O3—Na1vi | 2.3185 (13) |
Na1—O1 | 2.3567 (13) | OW—Na1iv | 2.3636 (14) |
Na1—OWiii | 2.3636 (14) | C1—C4 | 1.368 (2) |
Na1—OW | 2.3687 (15) | C1—C2 | 1.4347 (19) |
Na1—Na1iv | 4.0224 (10) | C2—C3 | 1.421 (2) |
Na1—Na1iii | 4.0224 (10) | C2—C2vii | 1.430 (3) |
S1—O2 | 1.4472 (11) | C3—C5vii | 1.362 (2) |
S1—O1 | 1.4584 (12) | C4—C5 | 1.407 (2) |
S1—O3 | 1.4619 (12) | C5—C3vii | 1.362 (2) |
S1—C1 | 1.7810 (15) | | |
| | | |
O3i—Na1—O2ii | 88.41 (5) | Na1iv—Na1—Na1iii | 87.26 (3) |
O3i—Na1—O1 | 130.82 (5) | O2—S1—O1 | 112.97 (7) |
O2ii—Na1—O1 | 87.69 (5) | O2—S1—O3 | 113.08 (7) |
O3i—Na1—OWiii | 90.82 (5) | O1—S1—O3 | 111.32 (7) |
O2ii—Na1—OWiii | 169.72 (6) | O2—S1—C1 | 106.51 (7) |
O1—Na1—OWiii | 85.06 (5) | O1—S1—C1 | 105.61 (7) |
O3i—Na1—OW | 133.26 (5) | O3—S1—C1 | 106.74 (7) |
O2ii—Na1—OW | 88.62 (5) | S1—O1—Na1 | 141.78 (7) |
O1—Na1—OW | 95.62 (5) | S1—O2—Na1v | 165.14 (8) |
OWiii—Na1—OW | 99.32 (4) | S1—O3—Na1vi | 145.02 (7) |
O3i—Na1—Na1iv | 160.05 (4) | Na1iv—OW—Na1 | 116.42 (6) |
O2ii—Na1—Na1iv | 79.58 (3) | C4—C1—C2 | 120.97 (13) |
O1—Na1—Na1iv | 65.04 (3) | C4—C1—S1 | 118.22 (11) |
OWiii—Na1—Na1iv | 103.79 (4) | C2—C1—S1 | 120.79 (11) |
OW—Na1—Na1iv | 31.75 (3) | C3—C2—C2vii | 118.94 (16) |
O3i—Na1—Na1iii | 98.84 (3) | C3—C2—C1 | 122.98 (13) |
O2ii—Na1—Na1iii | 158.17 (4) | C2vii—C2—C1 | 118.08 (16) |
O1—Na1—Na1iii | 102.53 (4) | C5vii—C3—C2 | 121.02 (13) |
OWiii—Na1—Na1iii | 31.83 (3) | C1—C4—C5 | 120.29 (14) |
OW—Na1—Na1iii | 71.39 (4) | C3vii—C5—C4 | 120.70 (14) |
| | | |
O2—S1—O1—Na1 | −117.06 (12) | OWiii—Na1—OW—Na1iv | 101.18 (9) |
O3—S1—O1—Na1 | 11.44 (14) | Na1iii—Na1—OW—Na1iv | 116.63 (7) |
C1—S1—O1—Na1 | 126.91 (11) | O2—S1—C1—C4 | −2.20 (14) |
O3i—Na1—O1—S1 | −95.81 (13) | O1—S1—C1—C4 | 118.17 (12) |
O2ii—Na1—O1—S1 | 178.29 (12) | O3—S1—C1—C4 | −123.27 (12) |
OWiii—Na1—O1—S1 | −9.00 (12) | O2—S1—C1—C2 | 179.27 (12) |
OW—Na1—O1—S1 | 89.91 (12) | O1—S1—C1—C2 | −60.37 (13) |
Na1iv—Na1—O1—S1 | 98.71 (12) | O3—S1—C1—C2 | 58.20 (13) |
Na1iii—Na1—O1—S1 | 17.77 (12) | C4—C1—C2—C3 | −179.74 (14) |
O1—S1—O2—Na1v | −96.0 (3) | S1—C1—C2—C3 | −1.2 (2) |
O3—S1—O2—Na1v | 136.4 (3) | C4—C1—C2—C2vii | 0.3 (2) |
C1—S1—O2—Na1v | 19.5 (4) | S1—C1—C2—C2vii | 178.82 (13) |
O2—S1—O3—Na1vi | −9.05 (15) | C2vii—C2—C3—C5vii | 0.1 (3) |
O1—S1—O3—Na1vi | −137.49 (12) | C1—C2—C3—C5vii | −179.84 (14) |
C1—S1—O3—Na1vi | 107.74 (12) | C2—C1—C4—C5 | −0.4 (2) |
O3i—Na1—OW—Na1iv | −158.78 (6) | S1—C1—C4—C5 | −178.96 (12) |
O2ii—Na1—OW—Na1iv | −72.26 (7) | C1—C4—C5—C3vii | 0.3 (2) |
O1—Na1—OW—Na1iv | 15.28 (7) | | |
Symmetry codes: (i) x, −y−1/2, z−1/2; (ii) x, −y+1/2, z−1/2; (iii) −x+1, y−1/2, −z+3/2; (iv) −x+1, y+1/2, −z+3/2; (v) x, −y+1/2, z+1/2; (vi) x, −y−1/2, z+1/2; (vii) −x+2, −y, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···O3iv | 0.89 (4) | 2.02 (4) | 2.8927 (18) | 168 (3) |
OW—HW2···O1iii | 0.76 (4) | 2.14 (4) | 2.8619 (18) | 159 (3) |
Symmetry codes: (iii) −x+1, y−1/2, −z+3/2; (iv) −x+1, y+1/2, −z+3/2. |
(3) dipotassium 1,5-naphthalenedisulfonate dihydrate
top
Crystal data top
2(K+)·C10H6O6S22−·2(H2O) | F(000) = 408 |
Mr = 400.50 | Dx = 1.805 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.0278 (18) Å | θ = 4.3–30.1° |
b = 8.5748 (14) Å | µ = 0.96 mm−1 |
c = 7.9845 (13) Å | T = 293 K |
β = 102.631 (3)° | Block, colorless |
V = 736.8 (2) Å3 | 0.36 × 0.20 × 0.17 mm |
Z = 2 | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1860 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 30.1°, θmin = 4.3° |
phi and ω scans | h = −15→15 |
5435 measured reflections | k = −12→5 |
2131 independent reflections | l = −11→11 |
Refinement top
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)] = 0.033 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.094 | w = 1/[σ2(Fo2) + (0.0422P)2 + 0.4224P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max < 0.001 |
2131 reflections | Δρmax = 0.37 e Å−3 |
109 parameters | Δρmin = −0.37 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.065 (4) |
Crystal data top
2(K+)·C10H6O6S22−·2(H2O) | V = 736.8 (2) Å3 |
Mr = 400.50 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.0278 (18) Å | µ = 0.96 mm−1 |
b = 8.5748 (14) Å | T = 293 K |
c = 7.9845 (13) Å | 0.36 × 0.20 × 0.17 mm |
β = 102.631 (3)° | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1860 reflections with I > 2σ(I) |
5435 measured reflections | Rint = 0.022 |
2131 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.033 | 0 restraints |
wR(F2) = 0.094 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.10 | Δρmax = 0.37 e Å−3 |
2131 reflections | Δρmin = −0.37 e Å−3 |
109 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.02531 (4) | 0.22911 (5) | 0.20591 (6) | 0.03973 (15) | |
S1 | 0.20366 (4) | 0.56240 (5) | 0.05415 (6) | 0.02907 (14) | |
O1 | 0.14169 (12) | 0.51168 (17) | −0.11652 (19) | 0.0398 (3) | |
O2 | 0.20563 (14) | 0.4415 (2) | 0.1818 (2) | 0.0476 (4) | |
O3 | 0.15252 (12) | 0.70802 (17) | 0.1008 (2) | 0.0406 (3) | |
OW | 0.1386 (2) | 0.0476 (2) | −0.0062 (3) | 0.0603 (5) | |
HW1 | 0.177 (3) | 0.036 (4) | −0.079 (4) | 0.059 (9)* | |
HW2 | 0.157 (3) | −0.017 (4) | 0.059 (5) | 0.070 (11)* | |
C1 | 0.39444 (15) | 0.3271 (2) | −0.0426 (3) | 0.0325 (4) | |
H1A | 0.3132 | 0.3007 | −0.0393 | 0.039* | |
C2 | 0.43727 (14) | 0.48094 (19) | 0.0009 (2) | 0.0247 (3) | |
C3 | 0.36089 (14) | 0.6001 (2) | 0.0486 (2) | 0.0264 (3) | |
C4 | 0.40665 (17) | 0.7457 (2) | 0.0928 (3) | 0.0340 (4) | |
H4A | 0.3558 | 0.8211 | 0.1257 | 0.041* | |
C5 | 0.53002 (17) | 0.7824 (2) | 0.0890 (3) | 0.0373 (4) | |
H5A | 0.5603 | 0.8822 | 0.1183 | 0.045* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0379 (2) | 0.0403 (2) | 0.0448 (3) | 0.00407 (17) | 0.01724 (18) | 0.01040 (18) |
S1 | 0.01926 (19) | 0.0325 (2) | 0.0380 (2) | 0.00043 (15) | 0.01178 (16) | 0.00035 (17) |
O1 | 0.0252 (6) | 0.0431 (8) | 0.0492 (8) | −0.0006 (6) | 0.0038 (6) | −0.0089 (7) |
O2 | 0.0369 (7) | 0.0544 (9) | 0.0579 (9) | 0.0018 (6) | 0.0243 (7) | 0.0193 (7) |
O3 | 0.0277 (6) | 0.0426 (8) | 0.0561 (9) | 0.0045 (5) | 0.0189 (6) | −0.0087 (7) |
OW | 0.0710 (12) | 0.0563 (11) | 0.0644 (12) | 0.0200 (9) | 0.0385 (11) | 0.0155 (10) |
C1 | 0.0213 (7) | 0.0302 (8) | 0.0473 (10) | −0.0057 (6) | 0.0100 (7) | −0.0038 (7) |
C2 | 0.0201 (7) | 0.0266 (7) | 0.0283 (7) | −0.0014 (6) | 0.0076 (6) | −0.0015 (6) |
C3 | 0.0193 (6) | 0.0309 (8) | 0.0307 (8) | −0.0005 (6) | 0.0091 (6) | −0.0014 (6) |
C4 | 0.0262 (8) | 0.0312 (9) | 0.0461 (10) | 0.0008 (7) | 0.0114 (7) | −0.0086 (8) |
C5 | 0.0289 (8) | 0.0281 (8) | 0.0554 (12) | −0.0059 (7) | 0.0099 (8) | −0.0092 (8) |
Geometric parameters (Å, º) top
K1—O1i | 2.6693 (15) | S1—K1iii | 3.4045 (7) |
K1—O2 | 2.7339 (16) | S1—K1vi | 3.7690 (7) |
K1—O3ii | 2.7536 (14) | O1—K1v | 2.6693 (15) |
K1—OW | 2.789 (2) | O1—K1iii | 2.8751 (15) |
K1—O3iii | 2.8346 (17) | O3—K1vi | 2.7536 (14) |
K1—O1iii | 2.8751 (15) | O3—K1iii | 2.8346 (17) |
K1—OWi | 3.042 (2) | OW—K1v | 3.042 (2) |
K1—OWiv | 3.191 (2) | OW—K1iv | 3.191 (2) |
K1—S1iii | 3.4045 (7) | C1—C5vii | 1.359 (3) |
K1—S1ii | 3.7690 (7) | C1—C2 | 1.418 (2) |
K1—K1i | 4.0083 (6) | C2—C2vii | 1.425 (3) |
K1—K1v | 4.0083 (7) | C2—C3 | 1.428 (2) |
S1—O2 | 1.4509 (16) | C3—C4 | 1.364 (2) |
S1—O1 | 1.4511 (15) | C4—C5 | 1.403 (3) |
S1—O3 | 1.4520 (14) | C5—C1vii | 1.359 (3) |
S1—C3 | 1.7738 (16) | | |
| | | |
O1i—K1—O2 | 106.26 (5) | O1iii—K1—K1i | 92.22 (3) |
O1i—K1—O3ii | 88.29 (5) | OWi—K1—K1i | 44.00 (4) |
O2—K1—O3ii | 134.53 (5) | OWiv—K1—K1i | 116.16 (4) |
O1i—K1—OW | 70.34 (6) | S1iii—K1—K1i | 113.516 (17) |
O2—K1—OW | 84.24 (6) | S1ii—K1—K1i | 51.809 (11) |
O3ii—K1—OW | 140.55 (6) | O1i—K1—K1v | 119.57 (4) |
O1i—K1—O3iii | 140.13 (5) | O2—K1—K1v | 73.26 (4) |
O2—K1—O3iii | 100.89 (5) | O3ii—K1—K1v | 135.98 (3) |
O3ii—K1—O3iii | 93.08 (4) | OW—K1—K1v | 49.27 (5) |
OW—K1—O3iii | 84.19 (6) | O3iii—K1—K1v | 43.37 (3) |
O1i—K1—O1iii | 159.610 (18) | O1iii—K1—K1v | 79.81 (3) |
O2—K1—O1iii | 84.49 (5) | OWi—K1—K1v | 127.36 (4) |
O3ii—K1—O1iii | 72.17 (5) | OWiv—K1—K1v | 72.06 (4) |
OW—K1—O1iii | 128.94 (6) | S1iii—K1—K1v | 60.471 (13) |
O3iii—K1—O1iii | 49.75 (4) | S1ii—K1—K1v | 133.321 (13) |
O1i—K1—OWi | 90.87 (6) | K1i—K1—K1v | 169.75 (3) |
O2—K1—OWi | 56.57 (5) | O2—S1—O1 | 112.16 (10) |
O3ii—K1—OWi | 80.98 (5) | O2—S1—O3 | 112.41 (10) |
OW—K1—OWi | 130.20 (9) | O1—S1—O3 | 111.67 (9) |
O3iii—K1—OWi | 128.72 (6) | O2—S1—C3 | 106.46 (9) |
O1iii—K1—OWi | 80.56 (5) | O1—S1—C3 | 107.05 (8) |
O1i—K1—OWiv | 81.05 (5) | O3—S1—C3 | 106.65 (8) |
O2—K1—OWiv | 143.27 (6) | O2—S1—K1iii | 134.34 (6) |
O3ii—K1—OWiv | 80.57 (5) | O1—S1—K1iii | 56.66 (6) |
OW—K1—OWiv | 64.00 (7) | O3—S1—K1iii | 55.05 (6) |
O3iii—K1—OWiv | 60.01 (5) | C3—S1—K1iii | 119.19 (6) |
O1iii—K1—OWiv | 100.87 (5) | O2—S1—K1vi | 79.79 (7) |
OWi—K1—OWiv | 160.03 (3) | O1—S1—K1vi | 111.14 (6) |
O1i—K1—S1iii | 159.47 (4) | O3—S1—K1vi | 37.09 (6) |
O2—K1—S1iii | 93.51 (4) | C3—S1—K1vi | 135.31 (6) |
O3ii—K1—S1iii | 81.50 (4) | K1iii—S1—K1vi | 67.720 (15) |
OW—K1—S1iii | 107.09 (5) | S1—O1—K1v | 143.48 (9) |
O3iii—K1—S1iii | 24.83 (3) | S1—O1—K1iii | 98.40 (7) |
O1iii—K1—S1iii | 24.94 (3) | K1v—O1—K1iii | 104.99 (5) |
OWi—K1—S1iii | 104.93 (5) | S1—O2—K1 | 128.76 (9) |
OWiv—K1—S1iii | 79.75 (4) | S1—O3—K1vi | 124.37 (8) |
O1i—K1—S1ii | 74.60 (3) | S1—O3—K1iii | 100.13 (8) |
O2—K1—S1ii | 150.09 (4) | K1vi—O3—K1iii | 91.65 (4) |
O3ii—K1—S1ii | 18.54 (3) | K1—OW—K1v | 86.73 (6) |
OW—K1—S1ii | 122.41 (5) | K1—OW—K1iv | 116.00 (7) |
O3iii—K1—S1ii | 95.60 (3) | K1v—OW—K1iv | 89.77 (6) |
O1iii—K1—S1ii | 87.45 (3) | C5vii—C1—C2 | 121.19 (15) |
OWi—K1—S1ii | 93.72 (4) | C1—C2—C2vii | 118.89 (18) |
OWiv—K1—S1ii | 66.59 (4) | C1—C2—C3 | 123.12 (14) |
S1iii—K1—S1ii | 91.101 (18) | C2vii—C2—C3 | 117.99 (18) |
O1i—K1—K1i | 69.19 (4) | C4—C3—C2 | 121.18 (14) |
O2—K1—K1i | 99.73 (4) | C4—C3—S1 | 117.93 (13) |
O3ii—K1—K1i | 44.98 (3) | C2—C3—S1 | 120.88 (12) |
OW—K1—K1i | 138.78 (5) | C3—C4—C5 | 120.32 (16) |
O3iii—K1—K1i | 133.86 (3) | C1vii—C5—C4 | 120.41 (17) |
| | | |
O2—S1—O1—K1v | −0.23 (16) | O3iii—K1—OW—K1v | 28.77 (5) |
O3—S1—O1—K1v | −127.44 (13) | O1iii—K1—OW—K1v | 5.29 (9) |
C3—S1—O1—K1v | 116.18 (13) | OWi—K1—OW—K1v | −108.72 (9) |
K1iii—S1—O1—K1v | −129.68 (15) | OWiv—K1—OW—K1v | 88.15 (8) |
K1vi—S1—O1—K1v | −87.50 (13) | S1iii—K1—OW—K1v | 19.07 (6) |
O2—S1—O1—K1iii | 129.45 (8) | S1ii—K1—OW—K1v | 121.72 (4) |
O3—S1—O1—K1iii | 2.25 (9) | K1i—K1—OW—K1v | −171.03 (3) |
C3—S1—O1—K1iii | −114.14 (7) | O1i—K1—OW—K1iv | 89.45 (8) |
K1vi—S1—O1—K1iii | 42.19 (6) | O2—K1—OW—K1iv | −160.99 (8) |
O1—S1—O2—K1 | −37.87 (14) | O3ii—K1—OW—K1iv | 28.40 (13) |
O3—S1—O2—K1 | 88.94 (13) | O3iii—K1—OW—K1iv | −59.38 (7) |
C3—S1—O2—K1 | −154.64 (10) | O1iii—K1—OW—K1iv | −82.86 (9) |
K1iii—S1—O2—K1 | 26.56 (18) | OWi—K1—OW—K1iv | 163.13 (6) |
K1vi—S1—O2—K1 | 70.94 (10) | S1iii—K1—OW—K1iv | −69.08 (7) |
O1i—K1—O2—S1 | 155.72 (12) | S1ii—K1—OW—K1iv | 33.57 (10) |
O3ii—K1—O2—S1 | −100.20 (13) | K1i—K1—OW—K1iv | 100.82 (9) |
OW—K1—O2—S1 | 88.16 (13) | K1v—K1—OW—K1iv | −88.15 (8) |
O3iii—K1—O2—S1 | 5.23 (13) | C5vii—C1—C2—C2vii | −1.4 (3) |
O1iii—K1—O2—S1 | −41.96 (12) | C5vii—C1—C2—C3 | 179.34 (18) |
OWi—K1—O2—S1 | −124.28 (14) | C1—C2—C3—C4 | 178.64 (18) |
OWiv—K1—O2—S1 | 58.84 (16) | C2vii—C2—C3—C4 | −0.6 (3) |
S1iii—K1—O2—S1 | −18.68 (12) | C1—C2—C3—S1 | −0.7 (2) |
S1ii—K1—O2—S1 | −117.03 (12) | C2vii—C2—C3—S1 | −179.97 (16) |
K1i—K1—O2—S1 | −133.27 (12) | O2—S1—C3—C4 | −117.53 (17) |
K1v—K1—O2—S1 | 39.03 (11) | O1—S1—C3—C4 | 122.34 (16) |
O2—S1—O3—K1vi | −30.29 (13) | O3—S1—C3—C4 | 2.68 (18) |
O1—S1—O3—K1vi | 96.78 (11) | K1iii—S1—C3—C4 | 61.49 (17) |
C3—S1—O3—K1vi | −146.60 (9) | K1vi—S1—C3—C4 | −25.5 (2) |
K1iii—S1—O3—K1vi | 99.07 (9) | O2—S1—C3—C2 | 61.84 (17) |
O2—S1—O3—K1iii | −129.36 (8) | O1—S1—C3—C2 | −58.29 (16) |
O1—S1—O3—K1iii | −2.29 (9) | O3—S1—C3—C2 | −177.95 (14) |
C3—S1—O3—K1iii | 114.34 (7) | K1iii—S1—C3—C2 | −119.14 (13) |
K1vi—S1—O3—K1iii | −99.07 (9) | K1vi—S1—C3—C2 | 153.89 (10) |
O1i—K1—OW—K1v | 177.60 (7) | C2—C3—C4—C5 | 1.3 (3) |
O2—K1—OW—K1v | −72.84 (6) | S1—C3—C4—C5 | −179.35 (16) |
O3ii—K1—OW—K1v | 116.55 (8) | C3—C4—C5—C1vii | −0.6 (3) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x, y−1/2, −z+1/2; (iii) −x, −y+1, −z; (iv) −x, −y, −z; (v) x, −y+1/2, z−1/2; (vi) −x, y+1/2, −z+1/2; (vii) −x+1, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···O2v | 0.79 (3) | 2.01 (3) | 2.751 (3) | 154 (3) |
OW—HW2···O3viii | 0.76 (4) | 2.39 (4) | 3.029 (3) | 144 (3) |
OW—HW2···O1i | 0.76 (4) | 2.63 (4) | 3.145 (3) | 127 (3) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (v) x, −y+1/2, z−1/2; (viii) x, y−1, z. |
(4) (hexaaqua)-magnesium(II) 1,5-naphthalenedisulfonate
top
Crystal data top
MgH12O62+·C10H6S2O62− | F(000) = 436 |
Mr = 418.67 | Dx = 1.630 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 13.1955 (8) Å | θ = 4.3–30.0° |
b = 6.6981 (4) Å | µ = 0.41 mm−1 |
c = 9.6616 (6) Å | T = 293 K |
β = 92.304 (1)° | Plate, colorless |
V = 853.25 (9) Å3 | 0.27 × 0.21 × 0.19 mm |
Z = 2 | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 2250 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.019 |
Graphite monochromator | θmax = 30.0°, θmin = 4.3° |
phi and ω scans | h = −14→18 |
5674 measured reflections | k = −9→9 |
2449 independent reflections | l = −11→13 |
Refinement top
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)] = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.086 | w = 1/[σ2(Fo2) + (0.0591P)2 + 0.1019P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max < 0.001 |
2449 reflections | Δρmax = 0.41 e Å−3 |
152 parameters | Δρmin = −0.36 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.083 (5) |
Crystal data top
MgH12O62+·C10H6S2O62− | V = 853.25 (9) Å3 |
Mr = 418.67 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.1955 (8) Å | µ = 0.41 mm−1 |
b = 6.6981 (4) Å | T = 293 K |
c = 9.6616 (6) Å | 0.27 × 0.21 × 0.19 mm |
β = 92.304 (1)° | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 2250 reflections with I > 2σ(I) |
5674 measured reflections | Rint = 0.019 |
2449 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.028 | 0 restraints |
wR(F2) = 0.086 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 0.41 e Å−3 |
2449 reflections | Δρmin = −0.36 e Å−3 |
152 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
S | 0.249906 (17) | 1.03340 (4) | 0.91547 (3) | 0.02187 (11) | |
Mg | 0.5000 | 0.5000 | 1.0000 | 0.01887 (13) | |
O1 | 0.37721 (7) | 0.53746 (12) | 0.86804 (9) | 0.02859 (19) | |
H1OB | 0.3498 (14) | 0.648 (3) | 0.8496 (18) | 0.046 (5)* | |
H1OA | 0.3305 (16) | 0.456 (3) | 0.863 (2) | 0.053 (5)* | |
O2 | 0.58743 (6) | 0.64910 (12) | 0.85493 (8) | 0.02499 (17) | |
H2OA | 0.6281 (15) | 0.575 (3) | 0.807 (2) | 0.052 (5)* | |
H2OB | 0.6200 (15) | 0.746 (3) | 0.885 (2) | 0.053 (5)* | |
O3 | 0.52744 (7) | 0.23274 (12) | 0.90278 (9) | 0.02935 (19) | |
H3OA | 0.5771 (16) | 0.159 (3) | 0.9151 (19) | 0.047 (5)* | |
H3OB | 0.5015 (15) | 0.197 (3) | 0.825 (2) | 0.051 (5)* | |
O4 | 0.29958 (6) | 1.01868 (13) | 1.05314 (9) | 0.03076 (19) | |
O5 | 0.30036 (6) | 0.90794 (13) | 0.81460 (9) | 0.03055 (19) | |
O6 | 0.23895 (6) | 1.23775 (12) | 0.86707 (10) | 0.0325 (2) | |
C1 | 0.12570 (7) | 0.93521 (15) | 0.92759 (10) | 0.02125 (19) | |
C2 | 0.10362 (8) | 0.75921 (16) | 0.86043 (11) | 0.0270 (2) | |
H2CA | 0.1546 (14) | 0.690 (3) | 0.8103 (17) | 0.043 (4)* | |
C3 | 0.00501 (8) | 0.67951 (17) | 0.86104 (12) | 0.0303 (2) | |
H3CA | −0.0061 (12) | 0.548 (2) | 0.8201 (16) | 0.032 (4)* | |
C4 | 0.07016 (8) | 1.22210 (17) | 1.07353 (12) | 0.0279 (2) | |
H4CA | 0.1364 (13) | 1.275 (3) | 1.0775 (18) | 0.043 (4)* | |
C5 | 0.05010 (7) | 1.04079 (14) | 1.00103 (10) | 0.0206 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
S | 0.01609 (14) | 0.02129 (16) | 0.02835 (16) | −0.00139 (7) | 0.00235 (9) | 0.00147 (8) |
Mg | 0.0185 (2) | 0.0197 (2) | 0.0185 (2) | 0.00009 (16) | 0.00119 (17) | 0.00024 (16) |
O1 | 0.0237 (4) | 0.0249 (4) | 0.0364 (4) | −0.0024 (3) | −0.0075 (3) | 0.0042 (3) |
O2 | 0.0245 (4) | 0.0257 (4) | 0.0251 (3) | −0.0039 (3) | 0.0059 (3) | −0.0008 (3) |
O3 | 0.0309 (4) | 0.0277 (4) | 0.0292 (4) | 0.0067 (3) | −0.0031 (3) | −0.0082 (3) |
O4 | 0.0219 (4) | 0.0365 (4) | 0.0334 (4) | −0.0016 (3) | −0.0043 (3) | −0.0002 (3) |
O5 | 0.0273 (4) | 0.0281 (4) | 0.0372 (4) | 0.0003 (3) | 0.0119 (3) | −0.0012 (3) |
O6 | 0.0263 (4) | 0.0222 (4) | 0.0492 (5) | −0.0027 (3) | 0.0037 (3) | 0.0072 (3) |
C1 | 0.0167 (4) | 0.0218 (4) | 0.0253 (4) | −0.0019 (3) | 0.0011 (3) | 0.0005 (3) |
C2 | 0.0230 (5) | 0.0250 (5) | 0.0333 (5) | −0.0012 (4) | 0.0033 (4) | −0.0050 (4) |
C3 | 0.0262 (5) | 0.0266 (5) | 0.0382 (6) | −0.0059 (4) | 0.0018 (4) | −0.0108 (4) |
C4 | 0.0216 (4) | 0.0275 (5) | 0.0347 (5) | −0.0071 (4) | 0.0019 (4) | −0.0078 (4) |
C5 | 0.0175 (4) | 0.0209 (4) | 0.0232 (4) | −0.0028 (3) | 0.0002 (3) | −0.0002 (3) |
Geometric parameters (Å, º) top
S—O6 | 1.4517 (8) | Mg—O2i | 2.1031 (7) |
S—O4 | 1.4624 (9) | C1—C2 | 1.3713 (14) |
S—O5 | 1.4667 (8) | C1—C5 | 1.4337 (13) |
S—C1 | 1.7743 (10) | C2—C3 | 1.4067 (15) |
Mg—O1i | 2.0366 (8) | C3—C4ii | 1.3668 (15) |
Mg—O1 | 2.0366 (8) | C4—C3ii | 1.3668 (15) |
Mg—O3i | 2.0604 (8) | C4—C5 | 1.4215 (14) |
Mg—O3 | 2.0604 (8) | C5—C5ii | 1.4301 (19) |
Mg—O2 | 2.1031 (7) | | |
| | | |
O6—S—O4 | 113.06 (5) | O3—Mg—O2 | 89.86 (3) |
O6—S—O5 | 111.60 (5) | O1i—Mg—O2i | 88.18 (3) |
O4—S—O5 | 111.52 (5) | O1—Mg—O2i | 91.82 (3) |
O6—S—C1 | 106.89 (5) | O3i—Mg—O2i | 89.86 (3) |
O4—S—C1 | 107.24 (5) | O3—Mg—O2i | 90.14 (3) |
O5—S—C1 | 106.06 (5) | O2—Mg—O2i | 180.000 (1) |
O1i—Mg—O1 | 180.0 | C2—C1—C5 | 121.29 (9) |
O1i—Mg—O3i | 88.37 (4) | C2—C1—S | 117.82 (7) |
O1—Mg—O3i | 91.63 (3) | C5—C1—S | 120.85 (7) |
O1i—Mg—O3 | 91.63 (3) | C1—C2—C3 | 120.21 (9) |
O1—Mg—O3 | 88.37 (4) | C4ii—C3—C2 | 120.50 (10) |
O3i—Mg—O3 | 180.000 (1) | C3ii—C4—C5 | 121.04 (9) |
O1i—Mg—O2 | 91.82 (3) | C4—C5—C1 | 123.08 (9) |
O1—Mg—O2 | 88.18 (3) | C4—C5—C5ii | 119.14 (11) |
O3i—Mg—O2 | 90.14 (3) | C1—C5—C5ii | 117.77 (11) |
| | | |
O6—S—C1—C2 | 126.72 (9) | C1—C2—C3—C4ii | 1.07 (18) |
O4—S—C1—C2 | −111.75 (9) | C3ii—C4—C5—C1 | 178.18 (11) |
O5—S—C1—C2 | 7.53 (10) | C3ii—C4—C5—C5ii | −1.07 (19) |
O6—S—C1—C5 | −51.02 (9) | C2—C1—C5—C4 | 179.12 (10) |
O4—S—C1—C5 | 70.51 (9) | S—C1—C5—C4 | −3.22 (14) |
O5—S—C1—C5 | −170.21 (8) | C2—C1—C5—C5ii | −1.62 (17) |
C5—C1—C2—C3 | 0.77 (16) | S—C1—C5—C5ii | 176.04 (9) |
S—C1—C2—C3 | −176.96 (9) | | |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) −x, −y+2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1OB···O5 | 0.84 (2) | 1.88 (2) | 2.7223 (12) | 174.4 (19) |
O1—H1OB···S | 0.84 (2) | 2.98 (2) | 3.7588 (9) | 155.4 (15) |
O1—H1OA···O6iii | 0.82 (2) | 1.90 (2) | 2.7124 (11) | 170 (2) |
O2—H2OA···O5iv | 0.88 (2) | 1.90 (2) | 2.7712 (11) | 171.9 (19) |
O2—H2OA···Siv | 0.88 (2) | 2.75 (2) | 3.5332 (8) | 149.5 (17) |
O2—H2OB···O4v | 0.83 (2) | 1.98 (2) | 2.8030 (12) | 177 (2) |
O2—H2OB···Sv | 0.83 (2) | 2.93 (2) | 3.6970 (9) | 155.8 (17) |
O3—H3OA···O4i | 0.82 (2) | 2.03 (2) | 2.8548 (12) | 179 (2) |
O3—H3OB···O2iv | 0.85 (2) | 2.08 (2) | 2.9168 (12) | 167.6 (18) |
Symmetry codes: (i) −x+1, −y+1, −z+2; (iii) x, y−1, z; (iv) −x+1, y−1/2, −z+3/2; (v) −x+1, −y+2, −z+2. |
(5) calcium 1,5-naphthalenedisulfonate dihydrate
top
Crystal data top
Ca2+·C10H6O6S22−·2(H2O) | V = 689.48 (12) Å3 |
Mr = 362.38 | Z = 2 |
Triclinic, P1 | F(000) = 372 |
a = 7.8971 (8) Å | Dx = 1.746 Mg m−3 |
b = 8.1750 (8) Å | Mo Kα radiation, λ = 0.71073 Å |
c = 11.2358 (11) Å | µ = 0.79 mm−1 |
α = 73.945 (2)° | T = 293 K |
β = 83.063 (2)° | Plate, colorless |
γ = 83.435 (2)° | 0.36 × 0.20 × 0.06 mm |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 2456 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.031 |
Graphite monochromator | θmax = 26.4°, θmin = 4.1° |
phi and ω scans | h = −9→9 |
3839 measured reflections | k = −9→10 |
2751 independent reflections | l = −14→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0707P)2] where P = (Fo2 + 2Fc2)/3 |
2751 reflections | (Δ/σ)max = 0.002 |
194 parameters | Δρmax = 0.74 e Å−3 |
0 restraints | Δρmin = −0.53 e Å−3 |
Crystal data top
Ca2+·C10H6O6S22−·2(H2O) | γ = 83.435 (2)° |
Mr = 362.38 | V = 689.48 (12) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.8971 (8) Å | Mo Kα radiation |
b = 8.1750 (8) Å | µ = 0.79 mm−1 |
c = 11.2358 (11) Å | T = 293 K |
α = 73.945 (2)° | 0.36 × 0.20 × 0.06 mm |
β = 83.063 (2)° | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 2456 reflections with I > 2σ(I) |
3839 measured reflections | Rint = 0.031 |
2751 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.101 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | Δρmax = 0.74 e Å−3 |
2751 reflections | Δρmin = −0.53 e Å−3 |
194 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca | 0.22621 (5) | 0.24251 (4) | 1.00325 (3) | 0.01912 (14) | |
S1 | 0.41485 (6) | −0.05652 (5) | 0.81516 (4) | 0.02116 (15) | |
S2 | −0.09776 (6) | 0.46076 (6) | 0.81216 (4) | 0.02205 (15) | |
O1 | 0.28473 (18) | −0.17457 (18) | 0.82942 (13) | 0.0331 (3) | |
O3 | 0.42120 (18) | 0.14632 (18) | 1.15037 (13) | 0.0330 (3) | |
O2 | 0.3603 (2) | 0.07556 (18) | 0.87865 (13) | 0.0333 (3) | |
O4 | −0.27107 (18) | 0.4214 (2) | 0.81379 (14) | 0.0387 (4) | |
O5 | 0.01609 (17) | 0.30696 (16) | 0.85880 (12) | 0.0272 (3) | |
O6 | 0.0815 (2) | 0.41062 (18) | 1.12376 (13) | 0.0346 (4) | |
OW1 | 0.05004 (19) | 0.03686 (18) | 1.12536 (14) | 0.0355 (4) | |
HW1 | 0.0462 | −0.0664 | 1.1199 | 0.050 (7)* | |
HW2 | −0.0537 | 0.0712 | 1.1397 | 0.056 (8)* | |
OW2 | 0.3809 (2) | 0.46687 (19) | 0.88644 (16) | 0.0425 (4) | |
HW4 | 0.3521 | 0.5745 | 0.8719 | 0.058 (8)* | |
HW3 | 0.4882 | 0.4637 | 0.8602 | 0.051 (8)* | |
C1 | 0.4421 (2) | 0.0493 (2) | 0.65425 (16) | 0.0214 (4) | |
C2 | 0.4019 (3) | 0.2226 (2) | 0.61857 (18) | 0.0273 (4) | |
H2A | 0.3689 | 0.2823 | 0.6783 | 0.033* | |
C3 | 0.4107 (3) | 0.3097 (2) | 0.49161 (18) | 0.0280 (4) | |
H3A | 0.3830 | 0.4272 | 0.4679 | 0.034* | |
C4 | 0.5406 (2) | −0.2248 (2) | 0.59756 (17) | 0.0249 (4) | |
H4A | 0.5367 | −0.2849 | 0.6811 | 0.030* | |
C5 | 0.4959 (2) | −0.0460 (2) | 0.56453 (16) | 0.0199 (4) | |
C6 | −0.0208 (2) | 0.5491 (2) | 0.65480 (16) | 0.0223 (4) | |
C7 | 0.0439 (3) | 0.7047 (3) | 0.62417 (18) | 0.0322 (5) | |
H7A | 0.0493 | 0.7599 | 0.6856 | 0.039* | |
C8 | 0.1021 (3) | 0.7817 (3) | 0.50065 (19) | 0.0341 (5) | |
H8A | 0.1456 | 0.8880 | 0.4806 | 0.041* | |
C9 | −0.0957 (3) | 0.2979 (2) | 0.59063 (17) | 0.0288 (4) | |
H9A | −0.1351 | 0.2452 | 0.6722 | 0.035* | |
C10 | −0.0301 (2) | 0.4597 (2) | 0.56273 (16) | 0.0206 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca | 0.0209 (2) | 0.0219 (2) | 0.0161 (2) | 0.00058 (14) | −0.00275 (14) | −0.00824 (15) |
S1 | 0.0223 (2) | 0.0256 (3) | 0.0165 (2) | 0.00341 (18) | −0.00316 (18) | −0.00874 (18) |
S2 | 0.0239 (2) | 0.0266 (3) | 0.0161 (2) | 0.00487 (18) | −0.00304 (18) | −0.00882 (18) |
O1 | 0.0304 (7) | 0.0361 (8) | 0.0322 (8) | −0.0070 (6) | 0.0010 (6) | −0.0082 (6) |
O3 | 0.0286 (7) | 0.0454 (8) | 0.0260 (7) | 0.0120 (6) | −0.0111 (6) | −0.0136 (6) |
O2 | 0.0463 (8) | 0.0329 (7) | 0.0227 (7) | 0.0061 (6) | −0.0006 (6) | −0.0157 (6) |
O4 | 0.0229 (7) | 0.0596 (10) | 0.0326 (8) | −0.0005 (7) | 0.0005 (6) | −0.0132 (7) |
O5 | 0.0315 (7) | 0.0258 (7) | 0.0249 (7) | 0.0045 (6) | −0.0086 (6) | −0.0078 (5) |
O6 | 0.0532 (9) | 0.0320 (7) | 0.0210 (7) | 0.0045 (7) | −0.0011 (6) | −0.0152 (6) |
OW1 | 0.0326 (8) | 0.0291 (8) | 0.0440 (9) | −0.0078 (6) | 0.0000 (7) | −0.0078 (6) |
OW2 | 0.0306 (8) | 0.0294 (8) | 0.0598 (11) | −0.0044 (6) | 0.0085 (7) | −0.0037 (7) |
C1 | 0.0221 (9) | 0.0263 (9) | 0.0169 (9) | 0.0005 (7) | −0.0033 (7) | −0.0081 (7) |
C2 | 0.0321 (10) | 0.0268 (9) | 0.0254 (10) | 0.0041 (8) | −0.0041 (8) | −0.0128 (7) |
C3 | 0.0365 (11) | 0.0205 (9) | 0.0263 (10) | 0.0050 (8) | −0.0053 (8) | −0.0072 (7) |
C4 | 0.0306 (10) | 0.0233 (9) | 0.0199 (9) | 0.0019 (7) | −0.0036 (7) | −0.0056 (7) |
C5 | 0.0203 (8) | 0.0230 (9) | 0.0178 (9) | 0.0012 (7) | −0.0044 (7) | −0.0079 (7) |
C6 | 0.0260 (9) | 0.0259 (9) | 0.0164 (9) | 0.0014 (7) | −0.0025 (7) | −0.0089 (7) |
C7 | 0.0454 (12) | 0.0325 (10) | 0.0239 (10) | −0.0066 (9) | −0.0047 (9) | −0.0139 (8) |
C8 | 0.0496 (13) | 0.0273 (10) | 0.0284 (10) | −0.0123 (9) | −0.0029 (9) | −0.0092 (8) |
C9 | 0.0373 (11) | 0.0280 (10) | 0.0209 (9) | −0.0060 (8) | −0.0015 (8) | −0.0056 (7) |
C10 | 0.0221 (9) | 0.0234 (9) | 0.0176 (9) | 0.0018 (7) | −0.0043 (7) | −0.0080 (7) |
Geometric parameters (Å, º) top
Ca—O2 | 2.3048 (13) | O6—S2ii | 1.4534 (13) |
Ca—O6 | 2.3075 (13) | C1—C2 | 1.373 (3) |
Ca—O3 | 2.3110 (13) | C1—C5 | 1.435 (2) |
Ca—OW2 | 2.3177 (15) | C2—C3 | 1.404 (3) |
Ca—OW1 | 2.3328 (14) | C3—C4iii | 1.366 (3) |
Ca—O5 | 2.3755 (13) | C4—C3iii | 1.366 (3) |
S1—O2 | 1.4511 (13) | C4—C5 | 1.418 (2) |
S1—O3i | 1.4532 (14) | C5—C5iii | 1.435 (4) |
S1—O1 | 1.4541 (14) | C6—C7 | 1.364 (3) |
S1—C1 | 1.7739 (18) | C6—C10 | 1.435 (2) |
S2—O4 | 1.4382 (15) | C7—C8 | 1.401 (3) |
S2—O6ii | 1.4534 (13) | C8—C9iv | 1.367 (3) |
S2—O5 | 1.4678 (13) | C9—C8iv | 1.367 (3) |
S2—C6 | 1.7753 (18) | C9—C10 | 1.416 (3) |
O3—S1i | 1.4532 (14) | C10—C10iv | 1.429 (4) |
| | | |
O2—Ca—O6 | 177.54 (6) | O6ii—S2—C6 | 105.67 (8) |
O2—Ca—O3 | 93.39 (5) | O5—S2—C6 | 106.38 (8) |
O6—Ca—O3 | 88.93 (5) | S1i—O3—Ca | 148.91 (8) |
O2—Ca—OW2 | 89.25 (6) | S1—O2—Ca | 166.63 (10) |
O6—Ca—OW2 | 91.41 (6) | S2—O5—Ca | 132.43 (7) |
O3—Ca—OW2 | 94.22 (6) | S2ii—O6—Ca | 144.93 (10) |
O2—Ca—OW1 | 95.78 (5) | C2—C1—C5 | 121.48 (16) |
O6—Ca—OW1 | 83.46 (5) | C2—C1—S1 | 117.92 (13) |
O3—Ca—OW1 | 88.01 (5) | C5—C1—S1 | 120.53 (14) |
OW2—Ca—OW1 | 174.37 (5) | C1—C2—C3 | 119.78 (16) |
O2—Ca—O5 | 83.70 (5) | C4iii—C3—C2 | 121.05 (17) |
O6—Ca—O5 | 93.91 (5) | C3iii—C4—C5 | 120.91 (17) |
O3—Ca—O5 | 173.07 (5) | C4—C5—C5iii | 119.14 (19) |
OW2—Ca—O5 | 92.03 (5) | C4—C5—C1 | 123.23 (16) |
OW1—Ca—O5 | 86.03 (5) | C5iii—C5—C1 | 117.63 (19) |
O2—S1—O3i | 112.77 (9) | C7—C6—C10 | 121.40 (17) |
O2—S1—O1 | 112.38 (9) | C7—C6—S2 | 118.15 (13) |
O3i—S1—O1 | 111.52 (9) | C10—C6—S2 | 120.44 (14) |
O2—S1—C1 | 106.28 (9) | C6—C7—C8 | 120.29 (17) |
O3i—S1—C1 | 107.14 (8) | C9iv—C8—C7 | 120.61 (18) |
O1—S1—C1 | 106.23 (8) | C8iv—C9—C10 | 120.88 (17) |
O4—S2—O6ii | 113.92 (9) | C9—C10—C10iv | 119.35 (19) |
O4—S2—O5 | 111.99 (9) | C9—C10—C6 | 123.18 (17) |
O6ii—S2—O5 | 110.62 (8) | C10iv—C10—C6 | 117.5 (2) |
O4—S2—C6 | 107.73 (9) | | |
| | | |
O2—Ca—O3—S1i | 13.61 (19) | O1—S1—C1—C2 | 116.78 (15) |
O6—Ca—O3—S1i | −167.23 (19) | O2—S1—C1—C5 | −179.90 (14) |
OW2—Ca—O3—S1i | −75.89 (19) | O3i—S1—C1—C5 | 59.30 (16) |
OW1—Ca—O3—S1i | 109.28 (19) | O1—S1—C1—C5 | −60.02 (16) |
O5—Ca—O3—S1i | 78.5 (4) | C5—C1—C2—C3 | 1.0 (3) |
O3i—S1—O2—Ca | −110.2 (4) | S1—C1—C2—C3 | −175.82 (15) |
O1—S1—O2—Ca | 16.9 (5) | C1—C2—C3—C4iii | −0.2 (3) |
C1—S1—O2—Ca | 132.7 (4) | C3iii—C4—C5—C5iii | −0.7 (3) |
O6—Ca—O2—S1 | −63.7 (13) | C3iii—C4—C5—C1 | 179.29 (18) |
O3—Ca—O2—S1 | 96.5 (4) | C2—C1—C5—C4 | 179.18 (17) |
OW2—Ca—O2—S1 | −169.3 (4) | S1—C1—C5—C4 | −4.1 (3) |
OW1—Ca—O2—S1 | 8.2 (4) | C2—C1—C5—C5iii | −0.8 (3) |
O5—Ca—O2—S1 | −77.2 (4) | S1—C1—C5—C5iii | 175.85 (16) |
O4—S2—O5—Ca | −133.15 (10) | O4—S2—C6—C7 | 125.41 (17) |
O6ii—S2—O5—Ca | −4.89 (13) | O6ii—S2—C6—C7 | 3.3 (2) |
C6—S2—O5—Ca | 109.40 (11) | O5—S2—C6—C7 | −114.34 (17) |
O2—Ca—O5—S2 | −147.63 (11) | O4—S2—C6—C10 | −53.36 (17) |
O6—Ca—O5—S2 | 32.94 (11) | O6ii—S2—C6—C10 | −175.49 (15) |
O3—Ca—O5—S2 | 146.9 (3) | O5—S2—C6—C10 | 66.89 (17) |
OW2—Ca—O5—S2 | −58.60 (11) | C10—C6—C7—C8 | 0.4 (3) |
OW1—Ca—O5—S2 | 116.10 (11) | S2—C6—C7—C8 | −178.35 (17) |
O2—Ca—O6—S2ii | −146.9 (11) | C6—C7—C8—C9iv | −0.3 (3) |
O3—Ca—O6—S2ii | 52.79 (16) | C8iv—C9—C10—C10iv | 0.1 (3) |
OW2—Ca—O6—S2ii | −41.41 (16) | C8iv—C9—C10—C6 | 179.85 (19) |
OW1—Ca—O6—S2ii | 140.91 (16) | C7—C6—C10—C9 | 179.8 (2) |
O5—Ca—O6—S2ii | −133.54 (15) | S2—C6—C10—C9 | −1.4 (3) |
O2—S1—C1—C2 | −3.10 (18) | C7—C6—C10—C10iv | −0.4 (3) |
O3i—S1—C1—C2 | −123.91 (15) | S2—C6—C10—C10iv | 178.36 (17) |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x, −y+1, −z+2; (iii) −x+1, −y, −z+1; (iv) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—HW1···O5v | 0.87 | 2.02 | 2.8708 (18) | 165 |
OW1—HW2···O1v | 0.85 | 1.95 | 2.798 (2) | 174 |
OW2—HW4···O1vi | 0.86 | 2.00 | 2.855 (2) | 177 |
OW2—HW3···O4vii | 0.86 | 1.93 | 2.784 (2) | 172 |
Symmetry codes: (v) −x, −y, −z+2; (vi) x, y+1, z; (vii) x+1, y, z. |
(6) strontium 1,5-naphthalenedisulfonate monohydrate
top
Crystal data top
Sr2+·C10H6O6S22−·H2O | F(000) = 776 |
Mr = 391.90 | Dx = 2.162 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
a = 9.5424 (11) Å | µ = 4.85 mm−1 |
b = 21.705 (2) Å | T = 293 K |
c = 5.8137 (7) Å | Needle, colorless |
V = 1204.1 (2) Å3 | 0.23 × 0.08 × 0.06 mm |
Z = 4 | |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1529 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.025 |
Graphite monochromator | θmax = 30.0°, θmin = 4.2° |
phi and ω scans | h = −13→12 |
8022 measured reflections | k = −26→30 |
1792 independent reflections | l = −8→7 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.059 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0361P)2] where P = (Fo2 + 2Fc2)/3 |
1792 reflections | (Δ/σ)max = 0.001 |
98 parameters | Δρmax = 0.52 e Å−3 |
0 restraints | Δρmin = −0.48 e Å−3 |
Crystal data top
Sr2+·C10H6O6S22−·H2O | V = 1204.1 (2) Å3 |
Mr = 391.90 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 9.5424 (11) Å | µ = 4.85 mm−1 |
b = 21.705 (2) Å | T = 293 K |
c = 5.8137 (7) Å | 0.23 × 0.08 × 0.06 mm |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1529 reflections with I > 2σ(I) |
8022 measured reflections | Rint = 0.025 |
1792 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.023 | 0 restraints |
wR(F2) = 0.059 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Δρmax = 0.52 e Å−3 |
1792 reflections | Δρmin = −0.48 e Å−3 |
98 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sr | 0.78320 (2) | 0.2500 | 1.08584 (4) | 0.01479 (8) | |
S | 0.94780 (5) | 0.343834 (19) | 0.57116 (7) | 0.01710 (10) | |
O1 | 0.8819 (2) | 0.31616 (6) | 0.7688 (3) | 0.0439 (5) | |
O2 | 1.09408 (16) | 0.32613 (7) | 0.5494 (3) | 0.0327 (4) | |
O3 | 0.87038 (18) | 0.33370 (7) | 0.3592 (3) | 0.0353 (4) | |
OW | 0.5987 (3) | 0.2500 | 1.4362 (4) | 0.0340 (5) | |
C1 | 0.85741 (18) | 0.50660 (8) | 0.8644 (3) | 0.0191 (4) | |
H1A | 0.8078 | 0.5191 | 0.9939 | 0.023* | |
C2 | 0.87023 (19) | 0.44371 (8) | 0.8167 (3) | 0.0175 (3) | |
H2A | 0.8299 | 0.4149 | 0.9148 | 0.021* | |
C3 | 0.94218 (17) | 0.42449 (8) | 0.6256 (3) | 0.0145 (3) | |
C4 | 1.00666 (18) | 0.46789 (8) | 0.4742 (3) | 0.0142 (3) | |
C5 | 1.08377 (18) | 0.45013 (8) | 0.2751 (3) | 0.0175 (3) | |
H5A | 1.0941 | 0.4086 | 0.2401 | 0.021* | |
HW1 | 0.603 (3) | 0.2800 (13) | 1.506 (5) | 0.047 (8)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sr | 0.01639 (12) | 0.01303 (11) | 0.01494 (12) | 0.000 | −0.00124 (9) | 0.000 |
S | 0.0205 (2) | 0.0102 (2) | 0.0206 (2) | 0.00017 (15) | 0.00277 (16) | 0.00016 (14) |
O1 | 0.0748 (12) | 0.0149 (7) | 0.0421 (9) | 0.0014 (7) | 0.0329 (9) | 0.0073 (6) |
O2 | 0.0236 (7) | 0.0204 (7) | 0.0542 (10) | 0.0078 (6) | 0.0017 (7) | −0.0053 (6) |
O3 | 0.0445 (9) | 0.0234 (7) | 0.0379 (8) | −0.0011 (7) | −0.0164 (7) | −0.0105 (6) |
OW | 0.0374 (13) | 0.0364 (14) | 0.0281 (12) | 0.000 | 0.0057 (10) | 0.000 |
C1 | 0.0212 (9) | 0.0199 (9) | 0.0161 (8) | 0.0014 (7) | 0.0047 (6) | −0.0032 (6) |
C2 | 0.0191 (8) | 0.0160 (8) | 0.0174 (8) | 0.0004 (7) | 0.0024 (7) | 0.0018 (6) |
C3 | 0.0155 (8) | 0.0102 (7) | 0.0179 (8) | 0.0005 (6) | −0.0018 (6) | −0.0003 (6) |
C4 | 0.0148 (7) | 0.0129 (7) | 0.0149 (8) | 0.0006 (6) | −0.0010 (6) | −0.0011 (6) |
C5 | 0.0205 (8) | 0.0137 (7) | 0.0184 (8) | 0.0020 (7) | 0.0012 (7) | −0.0031 (6) |
Geometric parameters (Å, º) top
Sr—O1i | 2.5190 (14) | S—C3 | 1.7798 (17) |
Sr—O1 | 2.5190 (14) | O2—Srvii | 2.5700 (14) |
Sr—O3ii | 2.5531 (14) | O3—Srviii | 2.5531 (14) |
Sr—O3iii | 2.5531 (14) | OW—Srix | 3.014 (3) |
Sr—O2iv | 2.5700 (14) | C1—C5x | 1.362 (2) |
Sr—O2v | 2.5700 (14) | C1—C2 | 1.398 (2) |
Sr—OW | 2.692 (2) | C2—C3 | 1.371 (2) |
Sr—OWvi | 3.014 (3) | C3—C4 | 1.429 (2) |
S—O1 | 1.4412 (15) | C4—C5 | 1.424 (2) |
S—O2 | 1.4533 (15) | C4—C4x | 1.432 (3) |
S—O3 | 1.4536 (15) | C5—C1x | 1.362 (2) |
| | | |
O1i—Sr—O1 | 69.51 (7) | O3iii—Sr—OWvi | 72.60 (5) |
O1i—Sr—O3ii | 137.67 (6) | O2iv—Sr—OWvi | 133.51 (4) |
O1—Sr—O3ii | 85.86 (6) | O2v—Sr—OWvi | 133.51 (4) |
O1i—Sr—O3iii | 85.86 (6) | OW—Sr—OWvi | 133.27 (4) |
O1—Sr—O3iii | 137.67 (6) | O1—S—O2 | 112.24 (11) |
O3ii—Sr—O3iii | 90.74 (7) | O1—S—O3 | 113.03 (11) |
O1i—Sr—O2iv | 70.86 (5) | O2—S—O3 | 111.98 (10) |
O1—Sr—O2iv | 113.91 (6) | O1—S—C3 | 104.77 (8) |
O3ii—Sr—O2iv | 151.25 (6) | O2—S—C3 | 107.73 (8) |
O3iii—Sr—O2iv | 87.80 (5) | O3—S—C3 | 106.51 (8) |
O1i—Sr—O2v | 113.91 (6) | S—O1—Sr | 169.77 (9) |
O1—Sr—O2v | 70.86 (5) | S—O2—Srvii | 150.59 (10) |
O3ii—Sr—O2v | 87.80 (5) | S—O3—Srviii | 143.22 (9) |
O3iii—Sr—O2v | 151.25 (6) | Sr—OW—Srix | 128.39 (9) |
O2iv—Sr—O2v | 80.02 (7) | C5x—C1—C2 | 121.27 (16) |
O1i—Sr—OW | 142.94 (4) | C3—C2—C1 | 120.10 (16) |
O1—Sr—OW | 142.94 (4) | C2—C3—C4 | 120.96 (15) |
O3ii—Sr—OW | 75.05 (6) | C2—C3—S | 117.29 (13) |
O3iii—Sr—OW | 75.05 (6) | C4—C3—S | 121.73 (12) |
O2iv—Sr—OW | 76.84 (6) | C5—C4—C3 | 123.00 (15) |
O2v—Sr—OW | 76.84 (6) | C5—C4—C4x | 118.68 (19) |
O1i—Sr—OWvi | 66.13 (6) | C3—C4—C4x | 118.32 (19) |
O1—Sr—OWvi | 66.13 (6) | C1x—C5—C4 | 120.66 (15) |
O3ii—Sr—OWvi | 72.60 (5) | | |
| | | |
O2—S—O1—Sr | −52.3 (8) | O3iii—Sr—OW—Srix | −132.56 (4) |
O3—S—O1—Sr | 75.5 (7) | O2iv—Sr—OW—Srix | −41.32 (4) |
C3—S—O1—Sr | −168.9 (7) | O2v—Sr—OW—Srix | 41.32 (4) |
O1i—Sr—O1—S | −8.4 (8) | OWvi—Sr—OW—Srix | 180.0 |
O3ii—Sr—O1—S | 136.5 (7) | C5x—C1—C2—C3 | −0.5 (3) |
O3iii—Sr—O1—S | 50.0 (8) | C1—C2—C3—C4 | 0.9 (3) |
O2iv—Sr—O1—S | −65.1 (7) | C1—C2—C3—S | −177.60 (14) |
O2v—Sr—O1—S | −134.4 (7) | O1—S—C3—C2 | −5.88 (17) |
OW—Sr—O1—S | −165.1 (7) | O2—S—C3—C2 | −125.57 (15) |
OWvi—Sr—O1—S | 63.7 (7) | O3—S—C3—C2 | 114.12 (15) |
O1—S—O2—Srvii | 84.0 (2) | O1—S—C3—C4 | 175.67 (15) |
O3—S—O2—Srvii | −44.3 (2) | O2—S—C3—C4 | 55.98 (16) |
C3—S—O2—Srvii | −161.14 (19) | O3—S—C3—C4 | −64.32 (16) |
O1—S—O3—Srviii | −62.34 (19) | C2—C3—C4—C5 | 179.28 (16) |
O2—S—O3—Srviii | 65.61 (19) | S—C3—C4—C5 | −2.3 (2) |
C3—S—O3—Srviii | −176.86 (15) | C2—C3—C4—C4x | −0.5 (3) |
O1i—Sr—OW—Srix | −71.07 (10) | S—C3—C4—C4x | 177.89 (17) |
O1—Sr—OW—Srix | 71.07 (10) | C3—C4—C5—C1x | 179.64 (16) |
O3ii—Sr—OW—Srix | 132.56 (4) | C4x—C4—C5—C1x | −0.6 (3) |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, y, z+1; (iii) x, −y+1/2, z+1; (iv) x−1/2, −y+1/2, −z+3/2; (v) x−1/2, y, −z+3/2; (vi) x+1/2, y, −z+5/2; (vii) x+1/2, y, −z+3/2; (viii) x, y, z−1; (ix) x−1/2, y, −z+5/2; (x) −x+2, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···O1ix | 0.77 (3) | 2.60 (3) | 3.047 (3) | 118 (3) |
Symmetry code: (ix) x−1/2, y, −z+5/2. |
(7) barium 1,5-naphthalenedisulfonate monohydrate
top
Crystal data top
Ba2+·C10H6O6S22−·H2O | F(000) = 848 |
Mr = 441.62 | Dx = 2.272 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
a = 9.7662 (14) Å | θ = 3.5–30.0° |
b = 22.080 (3) Å | µ = 3.43 mm−1 |
c = 5.9870 (8) Å | T = 293 K |
V = 1291.0 (3) Å3 | Needle, colorless |
Z = 4 | 0.40 × 0.07 × 0.04 mm |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1636 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.023 |
Graphite monochromator | θmax = 30.0°, θmin = 3.5° |
phi and ω scans | h = −10→13 |
6956 measured reflections | k = −25→30 |
1873 independent reflections | l = −8→7 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.056 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0338P)2 + 0.4684P] where P = (Fo2 + 2Fc2)/3 |
1873 reflections | (Δ/σ)max = 0.001 |
98 parameters | Δρmax = 1.26 e Å−3 |
0 restraints | Δρmin = −0.69 e Å−3 |
Crystal data top
Ba2+·C10H6O6S22−·H2O | V = 1291.0 (3) Å3 |
Mr = 441.62 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 9.7662 (14) Å | µ = 3.43 mm−1 |
b = 22.080 (3) Å | T = 293 K |
c = 5.9870 (8) Å | 0.40 × 0.07 × 0.04 mm |
Data collection top
Bruker Smart 1000 CCD area detector diffractometer | 1636 reflections with I > 2σ(I) |
6956 measured reflections | Rint = 0.023 |
1873 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.023 | 0 restraints |
wR(F2) = 0.056 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | Δρmax = 1.26 e Å−3 |
1873 reflections | Δρmin = −0.69 e Å−3 |
98 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ba1 | 0.781091 (18) | 0.7500 | 0.58819 (3) | 0.02005 (7) | |
S1 | 0.94448 (6) | 0.84699 (2) | 1.07146 (9) | 0.02414 (13) | |
O1 | 0.8744 (3) | 0.83755 (9) | 0.8615 (4) | 0.0540 (6) | |
O2 | 0.8752 (3) | 0.81970 (8) | 1.2577 (4) | 0.0612 (7) | |
O3 | 1.0865 (2) | 0.82884 (9) | 1.0585 (4) | 0.0514 (6) | |
OW | 0.5954 (3) | 0.7500 | 0.9618 (5) | 0.0408 (7) | |
C1 | 1.0813 (2) | 0.95018 (9) | 0.7831 (4) | 0.0237 (4) | |
H1A | 1.0903 | 0.9092 | 0.7506 | 0.028* | |
C2 | 1.0061 (2) | 0.96841 (9) | 0.9754 (4) | 0.0186 (4) | |
C3 | 0.9411 (2) | 0.92635 (9) | 1.1232 (4) | 0.0196 (4) | |
C4 | 0.8704 (2) | 0.94577 (10) | 1.3075 (4) | 0.0243 (4) | |
H4A | 0.8293 | 0.9178 | 1.4023 | 0.029* | |
C5 | 0.8599 (2) | 1.00824 (10) | 1.3532 (4) | 0.0262 (5) | |
H5A | 0.8120 | 1.0211 | 1.4787 | 0.031* | |
HW1 | 0.603 (4) | 0.7198 (16) | 1.031 (6) | 0.056 (11)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ba1 | 0.02012 (11) | 0.01746 (10) | 0.02258 (11) | 0.000 | −0.00234 (7) | 0.000 |
S1 | 0.0285 (3) | 0.0141 (2) | 0.0299 (3) | 0.0001 (2) | 0.0043 (2) | −0.00025 (19) |
O1 | 0.0771 (17) | 0.0305 (10) | 0.0546 (13) | −0.0075 (10) | −0.0270 (13) | −0.0118 (9) |
O2 | 0.1028 (19) | 0.0203 (8) | 0.0606 (14) | 0.0019 (10) | 0.0450 (14) | 0.0091 (9) |
O3 | 0.0342 (11) | 0.0272 (10) | 0.0927 (19) | 0.0111 (8) | 0.0074 (11) | −0.0065 (10) |
OW | 0.0398 (16) | 0.0455 (18) | 0.0370 (16) | 0.000 | 0.0052 (13) | 0.000 |
C1 | 0.0261 (11) | 0.0180 (9) | 0.0270 (11) | 0.0017 (8) | 0.0030 (9) | −0.0055 (8) |
C2 | 0.0169 (9) | 0.0173 (9) | 0.0216 (10) | 0.0005 (7) | −0.0013 (8) | −0.0025 (8) |
C3 | 0.0215 (10) | 0.0130 (9) | 0.0243 (10) | 0.0020 (7) | −0.0013 (8) | −0.0010 (7) |
C4 | 0.0261 (11) | 0.0219 (10) | 0.0249 (11) | −0.0004 (8) | 0.0047 (9) | 0.0019 (8) |
C5 | 0.0294 (11) | 0.0253 (10) | 0.0238 (10) | 0.0023 (9) | 0.0078 (10) | −0.0036 (9) |
Geometric parameters (Å, º) top
Ba1—O2i | 2.6698 (19) | S1—C3 | 1.780 (2) |
Ba1—O2ii | 2.6698 (19) | O2—Ba1vii | 2.6698 (19) |
Ba1—O1 | 2.6915 (19) | O3—Ba1vi | 2.7229 (19) |
Ba1—O1iii | 2.6915 (19) | OW—Ba1v | 3.084 (3) |
Ba1—O3iv | 2.7229 (19) | C1—C5viii | 1.356 (3) |
Ba1—O3v | 2.7229 (19) | C1—C2 | 1.424 (3) |
Ba1—OW | 2.880 (3) | C2—C2viii | 1.431 (4) |
Ba1—OWvi | 3.084 (3) | C2—C3 | 1.431 (3) |
S1—O2 | 1.437 (2) | C3—C4 | 1.370 (3) |
S1—O3 | 1.446 (2) | C4—C5 | 1.410 (3) |
S1—O1 | 1.447 (2) | C5—C1viii | 1.356 (3) |
| | | |
O2i—Ba1—O2ii | 70.40 (8) | O1iii—Ba1—OWvi | 73.87 (7) |
O2i—Ba1—O1 | 138.42 (9) | O3iv—Ba1—OWvi | 131.56 (6) |
O2ii—Ba1—O1 | 85.41 (8) | O3v—Ba1—OWvi | 131.56 (6) |
O2i—Ba1—O1iii | 85.41 (8) | OW—Ba1—OWvi | 134.60 (6) |
O2ii—Ba1—O1iii | 138.42 (9) | O2—S1—O3 | 112.14 (15) |
O1—Ba1—O1iii | 91.82 (9) | O2—S1—O1 | 113.03 (17) |
O2i—Ba1—O3iv | 68.46 (7) | O3—S1—O1 | 111.57 (14) |
O2ii—Ba1—O3iv | 111.70 (8) | O2—S1—C3 | 105.61 (11) |
O1—Ba1—O3iv | 153.07 (8) | O3—S1—C3 | 107.47 (11) |
O1iii—Ba1—O3iv | 88.46 (7) | O1—S1—C3 | 106.52 (11) |
O2i—Ba1—O3v | 111.70 (8) | S1—O1—Ba1 | 142.37 (12) |
O2ii—Ba1—O3v | 68.46 (7) | S1—O2—Ba1vii | 168.26 (13) |
O1—Ba1—O3v | 88.46 (7) | S1—O3—Ba1vi | 149.78 (13) |
O1iii—Ba1—O3v | 153.07 (8) | Ba1—OW—Ba1v | 123.46 (11) |
O3iv—Ba1—O3v | 79.48 (9) | C5viii—C1—C2 | 120.91 (19) |
O2i—Ba1—OW | 142.42 (5) | C1—C2—C2viii | 119.0 (2) |
O2ii—Ba1—OW | 142.42 (5) | C1—C2—C3 | 123.05 (18) |
O1—Ba1—OW | 74.98 (7) | C2viii—C2—C3 | 118.0 (2) |
O1iii—Ba1—OW | 74.98 (7) | C4—C3—C2 | 121.22 (18) |
O3iv—Ba1—OW | 79.11 (7) | C4—C3—S1 | 117.23 (16) |
O3v—Ba1—OW | 79.11 (7) | C2—C3—S1 | 121.53 (15) |
O2i—Ba1—OWvi | 65.50 (8) | C3—C4—C5 | 119.9 (2) |
O2ii—Ba1—OWvi | 65.50 (8) | C1viii—C5—C4 | 121.0 (2) |
O1—Ba1—OWvi | 73.87 (7) | | |
| | | |
O2—S1—O1—Ba1 | −57.9 (3) | O1iii—Ba1—OW—Ba1v | −131.96 (5) |
O3—S1—O1—Ba1 | 69.6 (3) | O3iv—Ba1—OW—Ba1v | −40.62 (5) |
C3—S1—O1—Ba1 | −173.4 (2) | O3v—Ba1—OW—Ba1v | 40.62 (5) |
O2i—Ba1—O1—S1 | −86.0 (3) | OWvi—Ba1—OW—Ba1v | 180.0 |
O2ii—Ba1—O1—S1 | −139.3 (3) | C5viii—C1—C2—C2viii | −0.5 (4) |
O1iii—Ba1—O1—S1 | −0.9 (3) | C5viii—C1—C2—C3 | 179.4 (2) |
O3iv—Ba1—O1—S1 | 89.3 (3) | C1—C2—C3—C4 | 179.6 (2) |
O3v—Ba1—O1—S1 | 152.2 (3) | C2viii—C2—C3—C4 | −0.6 (4) |
OW—Ba1—O1—S1 | 73.1 (3) | C1—C2—C3—S1 | −2.3 (3) |
OWvi—Ba1—O1—S1 | −73.5 (3) | C2viii—C2—C3—S1 | 177.6 (2) |
O3—S1—O2—Ba1vii | −32.6 (9) | O2—S1—C3—C4 | −4.3 (2) |
O1—S1—O2—Ba1vii | 94.6 (9) | O3—S1—C3—C4 | −124.15 (19) |
C3—S1—O2—Ba1vii | −149.3 (8) | O1—S1—C3—C4 | 116.2 (2) |
O2—S1—O3—Ba1vi | 88.2 (3) | O2—S1—C3—C2 | 177.5 (2) |
O1—S1—O3—Ba1vi | −39.8 (3) | O3—S1—C3—C2 | 57.6 (2) |
C3—S1—O3—Ba1vi | −156.2 (2) | O1—S1—C3—C2 | −62.1 (2) |
O2i—Ba1—OW—Ba1v | −70.94 (13) | C2—C3—C4—C5 | 0.4 (3) |
O2ii—Ba1—OW—Ba1v | 70.94 (13) | S1—C3—C4—C5 | −177.80 (19) |
O1—Ba1—OW—Ba1v | 131.96 (5) | C3—C4—C5—C1viii | 0.2 (4) |
Symmetry codes: (i) x, −y+3/2, z−1; (ii) x, y, z−1; (iii) x, −y+3/2, z; (iv) x−1/2, −y+3/2, −z+3/2; (v) x−1/2, y, −z+3/2; (vi) x+1/2, y, −z+3/2; (vii) x, y, z+1; (viii) −x+2, −y+2, −z+2. |
Experimental details
| (1) | (2) | (3) | (4) |
Crystal data |
Chemical formula | 2(Li+)·C10H6O6S22−·2(H2O) | 2(Na+)·C10H6O6S22−·2(H2O) | 2(K+)·C10H6O6S22−·2(H2O) | MgH12O62+·C10H6S2O62− |
Mr | 336.18 | 368.28 | 400.50 | 418.67 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 293 | 293 | 293 | 293 |
a, b, c (Å) | 10.8901 (17), 7.8842 (13), 8.0619 (13) | 11.6398 (17), 5.5507 (8), 10.7148 (16) | 11.0278 (18), 8.5748 (14), 7.9845 (13) | 13.1955 (8), 6.6981 (4), 9.6616 (6) |
α, β, γ (°) | 90, 104.228 (3), 90 | 90, 96.187 (3), 90 | 90, 102.631 (3), 90 | 90, 92.304 (1), 90 |
V (Å3) | 670.96 (19) | 688.24 (17) | 736.8 (2) | 853.25 (9) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.43 | 0.49 | 0.96 | 0.41 |
Crystal size (mm) | 0.33 × 0.21 × 0.06 | 0.33 × 0.16 × 0.11 | 0.36 × 0.20 × 0.17 | 0.27 × 0.21 × 0.19 |
|
Data collection |
Diffractometer | Bruker Smart 1000 CCD area detector diffractometer | Bruker Smart 1000 CCD area detector diffractometer | Bruker Smart 1000 CCD area detector diffractometer | Bruker Smart 1000 CCD area detector diffractometer |
Absorption correction | – | – | – | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4629, 1940, 1727 | 4234, 1692, 1516 | 5435, 2131, 1860 | 5674, 2449, 2250 |
Rint | 0.018 | 0.026 | 0.022 | 0.019 |
(sin θ/λ)max (Å−1) | 0.704 | 0.667 | 0.705 | 0.703 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.101, 1.11 | 0.031, 0.092, 1.06 | 0.033, 0.094, 1.10 | 0.028, 0.086, 1.05 |
No. of reflections | 1940 | 1692 | 2131 | 2449 |
No. of parameters | 108 | 109 | 109 | 152 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.45, −0.59 | 0.36, −0.49 | 0.37, −0.37 | 0.41, −0.36 |
| (5) | (6) | (7) |
Crystal data |
Chemical formula | Ca2+·C10H6O6S22−·2(H2O) | Sr2+·C10H6O6S22−·H2O | Ba2+·C10H6O6S22−·H2O |
Mr | 362.38 | 391.90 | 441.62 |
Crystal system, space group | Triclinic, P1 | Orthorhombic, Pnma | Orthorhombic, Pnma |
Temperature (K) | 293 | 293 | 293 |
a, b, c (Å) | 7.8971 (8), 8.1750 (8), 11.2358 (11) | 9.5424 (11), 21.705 (2), 5.8137 (7) | 9.7662 (14), 22.080 (3), 5.9870 (8) |
α, β, γ (°) | 73.945 (2), 83.063 (2), 83.435 (2) | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 689.48 (12) | 1204.1 (2) | 1291.0 (3) |
Z | 2 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.79 | 4.85 | 3.43 |
Crystal size (mm) | 0.36 × 0.20 × 0.06 | 0.23 × 0.08 × 0.06 | 0.40 × 0.07 × 0.04 |
|
Data collection |
Diffractometer | Bruker Smart 1000 CCD area detector diffractometer | Bruker Smart 1000 CCD area detector diffractometer | Bruker Smart 1000 CCD area detector diffractometer |
Absorption correction | – | – | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3839, 2751, 2456 | 8022, 1792, 1529 | 6956, 1873, 1636 |
Rint | 0.031 | 0.025 | 0.023 |
(sin θ/λ)max (Å−1) | 0.625 | 0.703 | 0.703 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.101, 1.09 | 0.023, 0.059, 1.03 | 0.023, 0.056, 1.01 |
No. of reflections | 2751 | 1792 | 1873 |
No. of parameters | 194 | 98 | 98 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.74, −0.53 | 0.52, −0.48 | 1.26, −0.69 |
Hydrogen-bond geometry (Å, º) for (1) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···O1i | 0.80 (3) | 2.07 (3) | 2.8676 (17) | 175 (2) |
OW—HW2···O3ii | 0.85 (3) | 2.11 (3) | 2.8942 (17) | 153 (2) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, y−1, z. |
Hydrogen-bond geometry (Å, º) for (2) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···O3i | 0.89 (4) | 2.02 (4) | 2.8927 (18) | 168 (3) |
OW—HW2···O1ii | 0.76 (4) | 2.14 (4) | 2.8619 (18) | 159 (3) |
Symmetry codes: (i) −x+1, y+1/2, −z+3/2; (ii) −x+1, y−1/2, −z+3/2. |
Hydrogen-bond geometry (Å, º) for (3) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···O2i | 0.79 (3) | 2.01 (3) | 2.751 (3) | 154 (3) |
OW—HW2···O3ii | 0.76 (4) | 2.39 (4) | 3.029 (3) | 144 (3) |
OW—HW2···O1iii | 0.76 (4) | 2.63 (4) | 3.145 (3) | 127 (3) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, y−1, z; (iii) x, −y+1/2, z+1/2. |
Hydrogen-bond geometry (Å, º) for (4) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1OB···O5 | 0.84 (2) | 1.88 (2) | 2.7223 (12) | 174.4 (19) |
O1—H1OB···S | 0.84 (2) | 2.98 (2) | 3.7588 (9) | 155.4 (15) |
O1—H1OA···O6i | 0.82 (2) | 1.90 (2) | 2.7124 (11) | 170 (2) |
O2—H2OA···O5ii | 0.88 (2) | 1.90 (2) | 2.7712 (11) | 171.9 (19) |
O2—H2OA···Sii | 0.88 (2) | 2.75 (2) | 3.5332 (8) | 149.5 (17) |
O2—H2OB···O4iii | 0.83 (2) | 1.98 (2) | 2.8030 (12) | 177 (2) |
O2—H2OB···Siii | 0.83 (2) | 2.93 (2) | 3.6970 (9) | 155.8 (17) |
O3—H3OA···O4iv | 0.82 (2) | 2.03 (2) | 2.8548 (12) | 179 (2) |
O3—H3OB···O2ii | 0.85 (2) | 2.08 (2) | 2.9168 (12) | 167.6 (18) |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, y−1/2, −z+3/2; (iii) −x+1, −y+2, −z+2; (iv) −x+1, −y+1, −z+2. |
Hydrogen-bond geometry (Å, º) for (5) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—HW1···O5i | 0.87 | 2.02 | 2.8708 (18) | 164.8 |
OW1—HW2···O1i | 0.85 | 1.95 | 2.798 (2) | 173.9 |
OW2—HW4···O1ii | 0.86 | 2.00 | 2.855 (2) | 177.2 |
OW2—HW3···O4iii | 0.86 | 1.93 | 2.784 (2) | 171.6 |
Symmetry codes: (i) −x, −y, −z+2; (ii) x, y+1, z; (iii) x+1, y, z. |
Hydrogen-bond geometry (Å, º) for (6) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW—HW1···O1i | 0.77 (3) | 2.60 (3) | 3.047 (3) | 118 (3) |
Symmetry code: (i) x−1/2, y, −z+5/2. |