In the crystal structure of the title compound, [Ca(C
9H
5INO
4S)
2(H
2O)
2]·H
2O, the asymmetric unit consists of one calcium ion, two organic ligands, two coordinated water molecules and one uncoordinated water molecule. The calcium ion has a pentagonal-bipyramidal geometry, formed by O atoms of three different sulfonate groups, deprotonated O atoms of two different oxine rings and two water molecules. In the ligands of type I, two O atoms of the sulfonate group are involved in coordination, whereas in type II ligands, only one O atom is involved. Ligands of type I are stacked over one another, each pair of adjacent members of the stack being related by an inversion centre. Ligands of type II are also stacked in a similar manner. Both of these molecular stacks are cross-linked by Ca—O(sulfonate) and Ca—O(quinolinol) bonds, leading to a three-dimensional network. This network is further stabilized by a number of O—H
O and N—H
O hydrogen bonds.
Supporting information
CCDC reference: 209280
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.066
- wR factor = 0.103
- Data-to-parameter ratio = 14.7
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT761_ALERT_1_A CIF Contains no X-H Bonds ...................... ?
PLAT762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?
Alert level B
CELLV02_ALERT_1_B The supplied cell volume s.u. differs from that
calculated from the cell parameter s.u.'s by > 4
Calculated cell volume su = 10.12
Cell volume su given = 4.00
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
2 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: KM-4 CCD Software (Kuma, 1999); cell refinement: KM-4 CCD Software; data reduction: KM-4 CCD Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1997); software used to prepare material for publication: SHELXL97.
Diaquabis(µ-8-hydroxy-7-iodoquinoline-5-sulfonato)calcium(II) monohydrate
top
Crystal data top
[Ca(C9H5INO4S)2(H2O)2]H2O | F(000) = 1536 |
Mr = 794.35 | Dx = 2.182 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 10575 reflections |
a = 20.326 (4) Å | θ = 3.1–26.1° |
b = 6.958 (1) Å | µ = 3.05 mm−1 |
c = 19.219 (4) Å | T = 293 K |
β = 117.19 (3)° | Plate, red |
V = 2417.7 (4) Å3 | 0.40 × 0.15 × 0.05 mm |
Z = 4 | |
Data collection top
Kuma KM-4 CCD κ-geometry diffractometer | 4771 independent reflections |
Radiation source: fine-focus sealed tube | 4526 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
w scans | θmax = 26.1°, θmin = 3.1° |
Absorption correction: multi-scan (XEMP; Siemens, 1990) | h = −24→25 |
Tmin = 0.593, Tmax = 0.859 | k = −8→5 |
26674 measured reflections | l = −23→23 |
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)] = 0.066 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.103 | H-atom parameters constrained |
S = 1.36 | w = 1/[σ2(Fo2) + (0.0351P)2 + 1.7598P] where P = (Fo2 + 2Fc2)/3 |
4771 reflections | (Δ/σ)max = 0.002 |
325 parameters | Δρmax = 1.61 e Å−3 |
0 restraints | Δρmin = −0.88 e Å−3 |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All e.s.d.'s are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
I1 | 0.39873 (2) | 1.11688 (7) | 0.50962 (2) | 0.0316 (1) | |
I2 | 1.10907 (2) | 0.44831 (8) | 1.27273 (2) | 0.0401 (2) | |
Ca | 0.74517 (6) | 0.61074 (17) | 0.85379 (7) | 0.0181 (3) | |
S1 | 0.69333 (7) | 1.1018 (2) | 0.76432 (8) | 0.0171 (4) | |
S2 | 0.81681 (8) | 0.3093 (2) | 1.03438 (8) | 0.0190 (4) | |
O1 | 0.7776 (2) | 0.3650 (6) | 0.9525 (2) | 0.0256 (12) | |
O1W | 0.6868 (2) | 0.6495 (6) | 0.7108 (2) | 0.0242 (12) | |
O2 | 0.7970 (2) | 0.1148 (6) | 1.0466 (3) | 0.0281 (12) | |
O2W | 0.8021 (2) | 0.7644 (6) | 0.9872 (2) | 0.0288 (14) | |
O3 | 0.8098 (2) | 0.4473 (6) | 1.0871 (2) | 0.0271 (14) | |
O4 | 1.1364 (2) | 0.3525 (6) | 1.1235 (2) | 0.0271 (14) | |
O21 | 0.6992 (2) | 1.0448 (6) | 0.6945 (2) | 0.0231 (12) | |
O22 | 0.7213 (2) | 1.2938 (6) | 0.7902 (2) | 0.0259 (12) | |
O23 | 0.7263 (2) | 0.9616 (6) | 0.8268 (2) | 0.0223 (12) | |
O24 | 0.3705 (2) | 1.1169 (6) | 0.6609 (2) | 0.0280 (14) | |
N1 | 1.0437 (3) | 0.2360 (7) | 0.9783 (3) | 0.0223 (17) | |
N2 | 0.4628 (3) | 1.1176 (7) | 0.8140 (3) | 0.0227 (17) | |
C2 | 1.0026 (3) | 0.1770 (9) | 0.9055 (4) | 0.027 (2) | |
C3 | 0.9271 (3) | 0.1495 (8) | 0.8782 (4) | 0.0259 (17) | |
C4 | 0.8957 (3) | 0.1871 (8) | 0.9260 (3) | 0.0225 (17) | |
C5 | 0.9118 (3) | 0.3045 (8) | 1.0576 (3) | 0.0200 (17) | |
C6 | 0.9618 (3) | 0.3572 (8) | 1.1329 (3) | 0.0219 (19) | |
C7 | 1.0375 (3) | 0.3688 (9) | 1.1582 (3) | 0.0215 (17) | |
C8 | 1.0685 (3) | 0.3352 (8) | 1.1067 (3) | 0.0198 (17) | |
C9 | 0.9391 (3) | 0.2556 (8) | 1.0035 (3) | 0.0172 (17) | |
C10 | 1.0159 (3) | 0.2763 (8) | 1.0290 (3) | 0.0185 (17) | |
C22 | 0.5041 (4) | 1.1198 (9) | 0.8909 (4) | 0.029 (2) | |
C23 | 0.5804 (3) | 1.1206 (9) | 0.9226 (4) | 0.029 (2) | |
C24 | 0.6133 (3) | 1.1181 (8) | 0.8742 (3) | 0.0232 (17) | |
C25 | 0.5971 (3) | 1.1075 (8) | 0.7362 (3) | 0.0180 (17) | |
C26 | 0.5478 (3) | 1.1100 (8) | 0.6567 (3) | 0.0214 (17) | |
C27 | 0.4715 (3) | 1.1158 (8) | 0.6299 (3) | 0.0191 (17) | |
C28 | 0.4394 (3) | 1.1156 (8) | 0.6808 (3) | 0.0188 (17) | |
C29 | 0.5697 (3) | 1.1129 (8) | 0.7918 (3) | 0.0179 (17) | |
C30 | 0.4922 (3) | 1.1151 (8) | 0.7627 (3) | 0.0190 (17) | |
O3W | 0.6952 (2) | 1.3834 (6) | 0.6125 (2) | 0.0309 (16) | |
H1 | 0.41370 | 1.13220 | 0.79560 | 0.0270* | |
H1W | 0.69480 | 0.57210 | 0.68130 | 0.0290* | |
H2 | 0.48100 | 1.12230 | 0.92470 | 0.0350* | |
H2W | 0.68410 | 0.75600 | 0.68800 | 0.0290* | |
H3 | 0.61040 | 1.12150 | 0.97830 | 0.0350* | |
H3W | 0.80970 | 0.71580 | 1.03080 | 0.0350* | |
H4 | 0.66620 | 1.12070 | 0.89590 | 0.0280* | |
H4W | 0.79350 | 0.87580 | 0.99910 | 0.0350* | |
H5 | 0.56680 | 1.10760 | 0.61930 | 0.0260* | |
H6 | 1.09080 | 0.27430 | 0.99500 | 0.0260* | |
H7 | 1.02480 | 0.15360 | 0.87160 | 0.0320* | |
H8 | 0.89720 | 0.10380 | 0.82590 | 0.0310* | |
H9 | 0.84360 | 0.16720 | 0.90740 | 0.0270* | |
H10 | 0.94330 | 0.38710 | 1.16950 | 0.0260* | |
H5W | 0.70750 | 1.27890 | 0.63820 | 0.0370* | |
H6W | 0.73140 | 1.38200 | 0.60180 | 0.0370* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.0266 (2) | 0.0434 (3) | 0.0179 (2) | 0.0013 (2) | 0.0042 (2) | 0.0003 (2) |
I2 | 0.0259 (2) | 0.0680 (4) | 0.0207 (2) | −0.0093 (2) | 0.0057 (2) | −0.0078 (2) |
Ca | 0.0130 (5) | 0.0209 (6) | 0.0189 (6) | 0.0003 (5) | 0.0060 (5) | 0.0013 (5) |
S1 | 0.0144 (7) | 0.0153 (7) | 0.0202 (7) | −0.0004 (6) | 0.0066 (6) | −0.0002 (6) |
S2 | 0.0153 (7) | 0.0206 (8) | 0.0208 (7) | −0.0022 (6) | 0.0080 (6) | 0.0001 (6) |
O1 | 0.022 (2) | 0.029 (2) | 0.020 (2) | 0.0034 (19) | 0.0045 (18) | 0.0057 (18) |
O1W | 0.034 (2) | 0.019 (2) | 0.022 (2) | 0.0030 (18) | 0.015 (2) | 0.0004 (18) |
O2 | 0.029 (2) | 0.021 (2) | 0.033 (2) | −0.0018 (19) | 0.013 (2) | 0.0016 (19) |
O2W | 0.039 (3) | 0.021 (2) | 0.030 (2) | 0.003 (2) | 0.019 (2) | −0.0015 (19) |
O3 | 0.022 (2) | 0.032 (3) | 0.028 (2) | 0.0003 (19) | 0.0121 (19) | −0.0089 (19) |
O4 | 0.014 (2) | 0.039 (3) | 0.028 (2) | −0.0035 (19) | 0.0093 (18) | −0.002 (2) |
O21 | 0.027 (2) | 0.020 (2) | 0.025 (2) | −0.0003 (18) | 0.0143 (19) | −0.0025 (18) |
O22 | 0.024 (2) | 0.022 (2) | 0.028 (2) | −0.0054 (18) | 0.0088 (19) | −0.0016 (19) |
O23 | 0.023 (2) | 0.017 (2) | 0.025 (2) | 0.0041 (17) | 0.0094 (18) | 0.0061 (18) |
O24 | 0.014 (2) | 0.042 (3) | 0.027 (2) | 0.0011 (19) | 0.0084 (18) | 0.001 (2) |
N1 | 0.020 (3) | 0.023 (3) | 0.023 (3) | −0.001 (2) | 0.009 (2) | −0.002 (2) |
N2 | 0.019 (3) | 0.029 (3) | 0.021 (3) | 0.003 (2) | 0.010 (2) | 0.001 (2) |
C2 | 0.035 (4) | 0.022 (3) | 0.031 (4) | 0.003 (3) | 0.022 (3) | 0.002 (3) |
C3 | 0.030 (3) | 0.020 (3) | 0.023 (3) | 0.001 (3) | 0.008 (3) | −0.005 (3) |
C4 | 0.018 (3) | 0.021 (3) | 0.026 (3) | −0.002 (3) | 0.008 (3) | −0.001 (3) |
C5 | 0.016 (3) | 0.020 (3) | 0.023 (3) | −0.001 (2) | 0.008 (2) | 0.001 (2) |
C6 | 0.019 (3) | 0.028 (4) | 0.020 (3) | −0.001 (3) | 0.010 (2) | 0.003 (3) |
C7 | 0.018 (3) | 0.026 (3) | 0.017 (3) | −0.001 (3) | 0.005 (2) | −0.002 (3) |
C8 | 0.015 (3) | 0.022 (3) | 0.020 (3) | 0.002 (2) | 0.006 (2) | 0.005 (2) |
C9 | 0.015 (3) | 0.014 (3) | 0.023 (3) | −0.002 (2) | 0.009 (2) | 0.002 (2) |
C10 | 0.021 (3) | 0.015 (3) | 0.022 (3) | 0.002 (2) | 0.012 (3) | 0.005 (2) |
C22 | 0.033 (4) | 0.035 (4) | 0.021 (3) | 0.000 (3) | 0.014 (3) | −0.001 (3) |
C23 | 0.030 (4) | 0.035 (4) | 0.020 (3) | 0.002 (3) | 0.009 (3) | 0.001 (3) |
C24 | 0.016 (3) | 0.025 (3) | 0.023 (3) | −0.003 (3) | 0.004 (3) | 0.001 (3) |
C25 | 0.017 (3) | 0.015 (3) | 0.024 (3) | −0.001 (2) | 0.011 (2) | −0.003 (2) |
C26 | 0.022 (3) | 0.020 (3) | 0.024 (3) | 0.001 (3) | 0.012 (3) | 0.001 (3) |
C27 | 0.016 (3) | 0.018 (3) | 0.017 (3) | 0.000 (2) | 0.002 (2) | −0.003 (2) |
C28 | 0.016 (3) | 0.020 (3) | 0.021 (3) | 0.003 (2) | 0.009 (2) | 0.000 (2) |
C29 | 0.015 (3) | 0.015 (3) | 0.022 (3) | 0.000 (2) | 0.007 (2) | −0.001 (2) |
C30 | 0.020 (3) | 0.018 (3) | 0.020 (3) | 0.000 (2) | 0.010 (2) | 0.001 (2) |
O3W | 0.038 (3) | 0.030 (3) | 0.029 (2) | 0.001 (2) | 0.019 (2) | 0.000 (2) |
Geometric parameters (Å, º) top
Ca—O1 | 2.411 (4) | Ca—O22i | 2.460 (4) |
Ca—O1W | 2.460 (4) | Ca—O24ii | 2.237 (5) |
Ca—O2W | 2.519 (4) | Ca—O4iii | 2.256 (5) |
Ca—O23 | 2.489 (4) | | |
| | | |
I1···O24 | 3.210 (4) | C2···C9xiv | 3.410 (8) |
I1···C23ii | 3.646 (6) | C2···C10xiv | 3.479 (9) |
I1···C23iv | 3.695 (6) | C3···C10xiv | 3.378 (8) |
I1···O21v | 3.672 (4) | C3···I2iii | 3.852 (6) |
I2···O2vi | 3.314 (5) | C3···C7iii | 3.564 (9) |
I2···C3iii | 3.852 (6) | C3···C8xiv | 3.383 (8) |
I2···O4 | 3.230 (4) | C3···C8iii | 3.595 (8) |
I1···H5v | 3.2644 | C4···C10xiv | 3.599 (8) |
I1···H2vii | 3.3537 | C4···O4iii | 3.320 (7) |
I2···H6Wviii | 3.2523 | C4···O1 | 2.945 (8) |
I2···H7ix | 3.1657 | C4···O22i | 3.387 (7) |
S1···H2W | 2.7793 | C4···N1xiv | 3.391 (7) |
S1···H4 | 2.8268 | C4···C8iii | 3.520 (8) |
S1···H5W | 2.8486 | C6···C2iii | 3.473 (9) |
S1···H9x | 3.0696 | C7···C3iii | 3.564 (9) |
S2···H3W | 2.8313 | C7···C2iii | 3.352 (9) |
S2···H4Wi | 3.0804 | C8···C3xiv | 3.383 (8) |
S2···H9 | 2.9059 | C8···C9iii | 3.510 (8) |
S2···H6Wxi | 2.9190 | C8···C3iii | 3.595 (8) |
O1···O2W | 2.848 (6) | C8···C4iii | 3.520 (8) |
O1···O22i | 2.832 (5) | C9···N1xiv | 3.440 (7) |
O1···C4 | 2.945 (8) | C9···C10iii | 3.515 (8) |
O1W···O23 | 2.949 (5) | C9···C2xiv | 3.410 (8) |
O1W···O24ii | 3.180 (6) | C9···C8iii | 3.510 (8) |
O1W···N2ii | 2.863 (8) | C10···C3xiv | 3.378 (8) |
O1W···S1 | 3.295 (4) | C10···C9iii | 3.515 (8) |
O1W···O3Wi | 2.706 (6) | C10···C10iii | 3.270 (8) |
O1W···O21 | 2.793 (6) | C10···C4xiv | 3.599 (8) |
O1W···O22i | 2.823 (6) | C10···C2xiv | 3.479 (9) |
O2···I2xii | 3.314 (5) | C22···C27ii | 3.590 (9) |
O2···O3Wxi | 2.878 (7) | C22···C27iv | 3.535 (9) |
O2···O2Wi | 2.714 (6) | C22···C26iv | 3.564 (9) |
O2W···O4iii | 3.030 (6) | C23···I1iv | 3.646 (6) |
O2W···N1iii | 2.892 (8) | C23···O3Wxv | 3.314 (8) |
O2W···O1 | 2.848 (6) | C23···I1ii | 3.695 (6) |
O2W···O2x | 2.714 (6) | C24···O23 | 3.034 (8) |
O2W···O3 | 2.882 (6) | C26···C22ii | 3.564 (9) |
O2W···O23 | 3.069 (5) | C27···C22ii | 3.535 (9) |
O2W···S2 | 3.270 (4) | C27···C22iv | 3.590 (9) |
O3···O2W | 2.882 (6) | C28···C29iv | 3.518 (8) |
O3W···O1Wx | 2.706 (6) | C28···C29ii | 3.555 (8) |
O3W···C23vii | 3.314 (8) | C29···C28iv | 3.555 (8) |
O3W···O21 | 2.815 (6) | C29···C28ii | 3.518 (8) |
O3W···O2xiii | 2.878 (7) | C30···C30iv | 3.547 (8) |
O4···O2Wiii | 3.030 (6) | C30···C30ii | 3.547 (8) |
O4···I2 | 3.230 (4) | C5···H6iii | 3.0927 |
O4···C4iii | 3.320 (7) | H1···O24 | 2.3253 |
O4···N1 | 2.681 (6) | H1···H2Wiv | 2.3164 |
O21···O1W | 2.793 (6) | H1···O1Wiv | 1.9932 |
O21···I1v | 3.672 (4) | H1···H1Wiv | 2.4760 |
O21···O3W | 2.815 (6) | H1W···H1ii | 2.4760 |
O22···Cax | 2.460 (4) | H1W···O3Wi | 1.8661 |
O22···O1x | 2.832 (5) | H1W···H5Wi | 2.2606 |
O22···O1Wx | 2.823 (6) | H1W···H6Wi | 2.3825 |
O22···C4x | 3.387 (7) | H2···I1xv | 3.3537 |
O23···O1W | 2.949 (5) | H2W···S1 | 2.7793 |
O23···O2W | 3.069 (5) | H2W···O21 | 2.0280 |
O23···O24ii | 3.179 (6) | H2W···H1ii | 2.3164 |
O23···C24 | 3.034 (8) | H3···O3Wxv | 2.3583 |
O24···O23iv | 3.179 (6) | H3···H6Wxv | 2.5196 |
O24···I1 | 3.210 (4) | H3W···O3 | 2.1585 |
O24···N2 | 2.671 (6) | H3W···O2x | 2.8174 |
O24···O1Wiv | 3.180 (6) | H3W···S2 | 2.8313 |
O1···H3W | 2.7840 | H3W···H6iii | 2.2929 |
O1···H4i | 2.6361 | H4···O1x | 2.6361 |
O1···H9 | 2.3469 | H4···S1 | 2.8268 |
O1W···H1ii | 1.9932 | H4···O2x | 2.9020 |
O2···H4i | 2.9020 | H4···O23 | 2.4421 |
O2···H4Wi | 1.8827 | H4W···O2x | 1.8827 |
O2···H3Wi | 2.8174 | H4W···S2x | 3.0804 |
O2···H6Wxi | 2.0486 | H4W···H6iii | 2.5279 |
O2W···H6iii | 2.0610 | H5···O21 | 2.4429 |
O3···H3W | 2.1585 | H5···I1v | 3.2644 |
O3···H10 | 2.4737 | H5W···S1 | 2.8486 |
O3···H6Wxi | 2.8776 | H5W···O21 | 2.0048 |
O3W···H3vii | 2.3583 | H5W···O22 | 2.8062 |
O3W···H1Wx | 1.8661 | H5W···H1Wx | 2.2606 |
O4···H6 | 2.2721 | H6···O4 | 2.2721 |
O21···H5 | 2.4429 | H6···H3Wiii | 2.2929 |
O21···H2W | 2.0280 | H6···O2Wiii | 2.0610 |
O21···H5W | 2.0048 | H6···C5iii | 3.0927 |
O22···H5W | 2.8062 | H6···H4Wiii | 2.5279 |
O22···H9x | 2.6291 | H6W···H1Wx | 2.3825 |
O22···H1Wx | 2.7185 | H6W···I2viii | 3.2523 |
O23···H2W | 2.7941 | H6W···O2xiii | 2.0486 |
O23···H9x | 2.5991 | H6W···O3xiii | 2.8776 |
O23···H4 | 2.4421 | H6W···S2xiii | 2.9190 |
O24···H1 | 2.3253 | H6W···H3vii | 2.5196 |
N1···O4 | 2.681 (6) | H7···I2xvi | 3.1657 |
N1···O2Wiii | 2.892 (8) | H9···S2 | 2.9059 |
N1···C9xiv | 3.440 (7) | H9···O1 | 2.3469 |
N1···C4xiv | 3.391 (7) | H9···S1i | 3.0696 |
N2···O24 | 2.671 (6) | H9···O23i | 2.5991 |
N2···O1Wiv | 2.863 (8) | H9···O22i | 2.6291 |
C2···C7iii | 3.352 (9) | H10···O3 | 2.4737 |
C2···C6iii | 3.473 (9) | | |
| | | |
O1—Ca—O1W | 140.85 (15) | O2W—Ca—O24ii | 95.04 (15) |
O1—Ca—O2W | 70.54 (14) | O2W—Ca—O4iii | 78.56 (14) |
O1—Ca—O23 | 145.11 (14) | O22i—Ca—O23 | 143.06 (13) |
O1—Ca—O22i | 71.10 (13) | O23—Ca—O24ii | 84.37 (16) |
O1—Ca—O24ii | 90.38 (15) | O4iii—Ca—O23 | 88.76 (16) |
O1—Ca—O4iii | 92.54 (15) | O22i—Ca—O24ii | 89.84 (16) |
O1W—Ca—O2W | 148.57 (15) | O4iii—Ca—O22i | 98.54 (16) |
O1W—Ca—O23 | 73.14 (13) | O4iii—Ca—O24ii | 171.62 (16) |
O1W—Ca—O22i | 70.02 (14) | Ca—O1—S2 | 149.1 (3) |
O1W—Ca—O24ii | 85.09 (15) | Caiii—O4—C8 | 176.7 (3) |
O1W—Ca—O4iii | 97.53 (15) | Ca—O23—S1 | 143.2 (2) |
O2W—Ca—O23 | 75.59 (13) | Caiv—O24—C28 | 170.8 (3) |
O2W—Ca—O22i | 141.34 (14) | | |
| | | |
O1W—Ca—O1—S2 | 169.1 (4) | C2—N1—C10—C9 | −0.3 (8) |
O2W—Ca—O1—S2 | −13.0 (5) | C10—N1—C2—C3 | −1.4 (9) |
O23—Ca—O1—S2 | −27.5 (7) | C2—N1—C10—C8 | 178.8 (5) |
O22i—Ca—O1—S2 | 162.1 (6) | C30—N2—C22—C23 | 0.3 (9) |
O24ii—Ca—O1—S2 | −108.2 (5) | C22—N2—C30—C28 | −179.2 (5) |
O4iii—Ca—O1—S2 | 63.9 (5) | C22—N2—C30—C29 | 0.6 (8) |
O1—Ca—O23—S1 | −162.9 (4) | N1—C2—C3—C4 | 1.3 (9) |
O1W—Ca—O23—S1 | 6.2 (4) | C2—C3—C4—C9 | 0.4 (9) |
O2W—Ca—O23—S1 | −177.0 (5) | C3—C4—C9—C5 | 178.2 (6) |
O22i—Ca—O23—S1 | 1.9 (6) | C3—C4—C9—C10 | −2.0 (8) |
O24ii—Ca—O23—S1 | −80.3 (5) | S2—C5—C6—C7 | −176.9 (5) |
O4iii—Ca—O23—S1 | 104.5 (5) | S2—C5—C9—C4 | −6.1 (8) |
O4iii—Ca—O2W—H3W | −111.63 | C6—C5—C9—C4 | 175.8 (5) |
O4iii—Ca—O2W—H4W | 112.45 | C9—C5—C6—C7 | 1.4 (9) |
O24ii—Ca—O1W—H1W | −125.09 | C6—C5—C9—C10 | −4.0 (8) |
O24ii—Ca—O1W—H2W | 100.39 | S2—C5—C9—C10 | 174.1 (4) |
O4iii—Ca—O1W—H1W | 62.92 | C5—C6—C7—C8 | 2.9 (9) |
O4iii—Ca—O1W—H2W | −71.60 | C5—C6—C7—I2 | −179.8 (4) |
O1—Ca—O2W—H3W | −14.78 | I2—C7—C8—C10 | 178.6 (4) |
O1—Ca—O2W—H4W | −150.69 | C6—C7—C8—C10 | −4.0 (8) |
O1W—Ca—O2W—H3W | 162.66 | I2—C7—C8—O4 | −1.4 (8) |
O1—Ca—O1W—H1W | −40.55 | C6—C7—C8—O4 | 176.0 (6) |
O1—Ca—O1W—H2W | −175.07 | C7—C8—C10—C9 | 1.2 (8) |
O2W—Ca—O1W—H1W | 143.28 | C7—C8—C10—N1 | −177.8 (5) |
O2W—Ca—O1W—H2W | 8.77 | O4—C8—C10—C9 | −178.9 (5) |
O23—Ca—O1W—H1W | 149.31 | O4—C8—C10—N1 | 2.2 (8) |
O23—Ca—O1W—H2W | 14.80 | C4—C9—C10—C8 | −177.0 (5) |
O22i—Ca—O1W—H1W | −33.48 | C5—C9—C10—N1 | −178.2 (5) |
O22i—Ca—O1W—H2W | −167.99 | C4—C9—C10—N1 | 1.9 (8) |
O1W—Ca—O2W—H4W | 26.74 | C5—C9—C10—C8 | 2.8 (8) |
O23—Ca—O2W—H3W | 156.70 | N2—C22—C23—C24 | −0.3 (9) |
O23—Ca—O2W—H4W | 20.78 | C22—C23—C24—C29 | −0.6 (9) |
O22i—Ca—O2W—H3W | −22.22 | C23—C24—C29—C30 | 1.5 (8) |
O22i—Ca—O2W—H4W | −158.14 | C23—C24—C29—C25 | −179.2 (6) |
O24ii—Ca—O2W—H3W | 73.84 | C29—C25—C26—C27 | −0.7 (8) |
O24ii—Ca—O2W—H4W | −62.08 | C26—C25—C29—C24 | −177.6 (5) |
O22—S1—C25—C26 | 103.8 (5) | S1—C25—C29—C24 | 1.3 (8) |
O21—S1—O23—Ca | −36.2 (5) | S1—C25—C29—C30 | −179.4 (4) |
O22—S1—O23—Ca | −164.0 (4) | S1—C25—C26—C27 | −179.6 (4) |
C25—S1—O23—Ca | 79.2 (5) | C26—C25—C29—C30 | 1.8 (8) |
O23—S1—C25—C29 | 45.1 (5) | C25—C26—C27—C28 | −1.3 (9) |
O22—S1—C25—C29 | −75.1 (5) | C25—C26—C27—I1 | −179.4 (4) |
O23—S1—C25—C26 | −136.0 (4) | I1—C27—C28—C30 | −179.9 (4) |
O21—S1—C25—C26 | −16.2 (5) | I1—C27—C28—O24 | −0.3 (8) |
O21—S1—C25—C29 | 164.9 (5) | C26—C27—C28—O24 | −178.5 (5) |
O2—S2—C5—C9 | 87.1 (5) | C26—C27—C28—C30 | 1.9 (8) |
O3—S2—C5—C9 | −152.8 (5) | O24—C28—C30—N2 | −0.5 (8) |
C5—S2—O1—Ca | −72.6 (6) | C27—C28—C30—C29 | −0.7 (8) |
O3—S2—C5—C6 | 25.4 (5) | O24—C28—C30—C29 | 179.7 (5) |
O1—S2—C5—C9 | −31.8 (5) | C27—C28—C30—N2 | 179.1 (5) |
O2—S2—O1—Ca | 171.5 (5) | C24—C29—C30—N2 | −1.5 (8) |
O3—S2—O1—Ca | 43.6 (6) | C24—C29—C30—C28 | 178.3 (5) |
O1—S2—C5—C6 | 146.4 (4) | C25—C29—C30—N2 | 179.1 (5) |
O2—S2—C5—C6 | −94.7 (5) | C25—C29—C30—C28 | −1.1 (8) |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, y−1/2, −z+3/2; (iii) −x+2, −y+1, −z+2; (iv) −x+1, y+1/2, −z+3/2; (v) −x+1, −y+2, −z+1; (vi) −x+2, y+1/2, −z+5/2; (vii) x, −y+5/2, z−1/2; (viii) −x+2, −y+2, −z+2; (ix) x, −y+1/2, z+1/2; (x) x, y+1, z; (xi) x, −y+3/2, z+1/2; (xii) −x+2, y−1/2, −z+5/2; (xiii) x, −y+3/2, z−1/2; (xiv) −x+2, −y, −z+2; (xv) x, −y+5/2, z+1/2; (xvi) x, −y+1/2, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H1···O24 | 0.90 | 2.33 | 2.671 (6) | 103 |
N2—H1···O1Wiv | 0.90 | 1.99 | 2.863 (8) | 162 |
O1W—H1W···O3Wi | 0.85 | 1.87 | 2.706 (6) | 169 |
O1W—H2W···O21 | 0.85 | 2.03 | 2.793 (6) | 149 |
O2W—H3W···O3 | 0.85 | 2.16 | 2.882 (6) | 143 |
O2W—H4W···O2x | 0.85 | 1.88 | 2.714 (6) | 166 |
O3W—H5W···O21 | 0.85 | 2.00 | 2.815 (6) | 159 |
N1—H6···O4 | 0.90 | 2.27 | 2.681 (6) | 107 |
N1—H6···O2Wiii | 0.90 | 2.06 | 2.892 (8) | 153 |
O3W—H6W···O2xiii | 0.85 | 2.05 | 2.878 (7) | 165 |
C23—H3···O3Wxv | 0.96 | 2.36 | 3.314 (8) | 174 |
C24—H4···O23 | 0.96 | 2.44 | 3.034 (8) | 120 |
C26—H5···O21 | 0.96 | 2.44 | 2.857 (8) | 106 |
C4—H9···O1 | 0.96 | 2.35 | 2.945 (8) | 120 |
C4—H9···O23i | 0.96 | 2.60 | 3.457 (7) | 149 |
C6—H10···O3 | 0.96 | 2.47 | 2.868 (8) | 104 |
Symmetry codes: (i) x, y−1, z; (iii) −x+2, −y+1, −z+2; (iv) −x+1, y+1/2, −z+3/2; (x) x, y+1, z; (xiii) x, −y+3/2, z−1/2; (xv) x, −y+5/2, z+1/2. |