In the title compound, Na
3[Ni(C
3H
2O
4)
2]Cl·6H
2O, two crystallographically independent Ni atoms lie on centres of symmetry, each coordinated by four O atoms from two malonate ligands and by two water molecules in a distorted octahedral geometry. The Ni—O bond lengths are in the range 1.994 (18)–2.137 (2) Å. The three Na
+ ions are coordinated by seven O atoms, six O atoms, and five O and one Cl atom. The crystal packing is stabilized by the three-dimensional hydrogen-bonding network formed by O—H
O and O—H
Cl hydrogen bonds.
Supporting information
CCDC reference: 627477
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.003 Å
- R factor = 0.027
- wR factor = 0.075
- Data-to-parameter ratio = 16.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O6 - H8 ... ?
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.33 Ratio
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.
Trisodium diaquabis(malonato-
κ2O,
O')nickel(II) chloride
hexahydrate
top
Crystal data top
Na3[Ni(C3H2O4)2]Cl·6H2O | Z = 2 |
Mr = 511.35 | F(000) = 524 |
Triclinic, P1 | Dx = 1.833 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.053 (3) Å | Cell parameters from 8146 reflections |
b = 9.615 (5) Å | θ = 6.2–55.0° |
c = 14.624 (10) Å | µ = 1.34 mm−1 |
α = 93.51 (3)° | T = 295 K |
β = 92.75 (3)° | Block, green |
γ = 110.19 (2)° | 0.37 × 0.32 × 0.29 mm |
V = 926.5 (9) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 4156 independent reflections |
Radiation source: fine-focus sealed tube | 3809 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −9→9 |
Tmin = 0.641, Tmax = 0.699 | k = −12→12 |
8824 measured reflections | l = −18→18 |
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-atom parameters constrained |
wR(F2) = 0.075 | w = 1/[σ2(Fo2) + (0.0119P)2 + 0.8306P] where P = (Fo2 + 2Fc2)/3 |
S = 1.33 | (Δ/σ)max = 0.001 |
4156 reflections | Δρmax = 0.43 e Å−3 |
254 parameters | Δρmin = −0.30 e Å−3 |
24 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.066 (2) |
Special details top
Experimental. (See detailed section in the paper) |
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 | |
C1 | −0.1299 (3) | −0.0182 (2) | 0.09312 (14) | 0.0178 (4) | |
C2 | −0.0809 (3) | 0.1416 (2) | 0.13133 (16) | 0.0239 (5) | |
H2 | 0.0636 | 0.1829 | 0.1480 | 0.029* | |
H1 | −0.1486 | 0.1396 | 0.1877 | 0.029* | |
C3 | −0.1343 (3) | 0.2488 (2) | 0.07206 (14) | 0.0171 (4) | |
C4 | 0.1446 (3) | 0.8353 (2) | 0.37295 (14) | 0.0191 (4) | |
C5 | 0.1417 (4) | 0.9871 (3) | 0.34957 (16) | 0.0254 (5) | |
H4 | 0.2386 | 1.0228 | 0.3039 | 0.030* | |
H3 | 0.0087 | 0.9726 | 0.3208 | 0.030* | |
C6 | 0.1875 (3) | 1.1095 (2) | 0.42688 (15) | 0.0190 (4) | |
Cl1 | −0.40135 (10) | 0.31714 (7) | 0.26328 (4) | 0.03348 (15) | |
Na1 | 0.25998 (13) | 0.52820 (10) | 0.01397 (6) | 0.0247 (2) | |
Na2 | 0.01124 (15) | 0.53553 (11) | 0.22191 (6) | 0.0292 (2) | |
Na3 | 0.43181 (15) | 0.63680 (10) | 0.43278 (7) | 0.0293 (2) | |
Ni1 | −0.5000 | 0.0000 | 0.0000 | 0.01633 (11) | |
Ni2 | 0.5000 | 1.0000 | 0.5000 | 0.01679 (11) | |
O1 | −0.0028 (2) | −0.07761 (18) | 0.11152 (13) | 0.0310 (4) | |
O2 | −0.2974 (2) | −0.08777 (17) | 0.04910 (11) | 0.0219 (3) | |
O3 | −0.2895 (2) | 0.20289 (16) | 0.01606 (11) | 0.0220 (3) | |
O4 | −0.0247 (2) | 0.38199 (16) | 0.08347 (11) | 0.0234 (3) | |
O5 | −0.6013 (2) | 0.01393 (19) | 0.13266 (11) | 0.0255 (3) | |
H5 | −0.7289 | −0.0070 | 0.1273 | 0.038* | |
H6 | −0.5507 | 0.0961 | 0.1651 | 0.038* | |
O6 | 0.1934 (3) | 0.37001 (19) | −0.12860 (12) | 0.0316 (4) | |
H8 | 0.3051 | 0.3738 | −0.1489 | 0.047* | |
H7 | 0.1292 | 0.2802 | −0.1191 | 0.047* | |
O7 | 0.4204 (2) | 0.36209 (18) | 0.05954 (12) | 0.0278 (4) | |
H10 | 0.4631 | 0.3474 | 0.1118 | 0.042* | |
H9 | 0.3671 | 0.2787 | 0.0285 | 0.042* | |
O8 | 0.3292 (3) | 0.6798 (2) | 0.16333 (12) | 0.0374 (4) | |
H11 | 0.4252 | 0.7036 | 0.2049 | 0.056* | |
H12 | 0.3435 | 0.7557 | 0.1341 | 0.056* | |
O9 | 0.2227 (3) | 0.4355 (2) | 0.31759 (13) | 0.0357 (4) | |
H14 | 0.3167 | 0.4147 | 0.2927 | 0.054* | |
H13 | 0.1667 | 0.3662 | 0.3514 | 0.054* | |
O10 | 0.7062 (3) | 0.5291 (2) | 0.45710 (14) | 0.0454 (5) | |
H16 | 0.8094 | 0.6070 | 0.4683 | 0.068* | |
H15 | 0.7165 | 0.4874 | 0.4059 | 0.068* | |
O11 | 0.6262 (3) | 0.7585 (2) | 0.30692 (12) | 0.0331 (4) | |
H18 | 0.6460 | 0.8478 | 0.3263 | 0.050* | |
H17 | 0.7392 | 0.7458 | 0.3127 | 0.050* | |
O12 | 0.2919 (2) | 0.82908 (17) | 0.42269 (11) | 0.0230 (3) | |
O13 | 0.0040 (2) | 0.72321 (18) | 0.33774 (12) | 0.0277 (4) | |
O14 | 0.0748 (2) | 1.18546 (19) | 0.43087 (13) | 0.0312 (4) | |
O15 | 0.3426 (2) | 1.13638 (17) | 0.48094 (11) | 0.0234 (3) | |
O16 | 0.6704 (2) | 1.06760 (19) | 0.38339 (11) | 0.0252 (3) | |
H19 | 0.6400 | 1.1330 | 0.3555 | 0.038* | |
H20 | 0.7960 | 1.1051 | 0.4003 | 0.038* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0154 (9) | 0.0162 (10) | 0.0214 (10) | 0.0046 (8) | 0.0013 (7) | 0.0044 (8) |
C2 | 0.0246 (11) | 0.0165 (11) | 0.0280 (11) | 0.0060 (9) | −0.0097 (9) | −0.0015 (8) |
C3 | 0.0150 (9) | 0.0146 (10) | 0.0222 (10) | 0.0057 (8) | 0.0033 (7) | 0.0002 (8) |
C4 | 0.0169 (9) | 0.0215 (11) | 0.0187 (10) | 0.0072 (8) | 0.0006 (7) | −0.0027 (8) |
C5 | 0.0271 (11) | 0.0221 (12) | 0.0248 (11) | 0.0075 (10) | −0.0084 (9) | −0.0002 (9) |
C6 | 0.0154 (9) | 0.0166 (10) | 0.0241 (10) | 0.0039 (8) | 0.0000 (8) | 0.0052 (8) |
Cl1 | 0.0413 (3) | 0.0313 (3) | 0.0273 (3) | 0.0122 (3) | 0.0018 (2) | 0.0020 (2) |
Na1 | 0.0216 (4) | 0.0247 (5) | 0.0282 (5) | 0.0082 (4) | 0.0014 (3) | 0.0047 (4) |
Na2 | 0.0369 (5) | 0.0248 (5) | 0.0247 (5) | 0.0107 (4) | −0.0027 (4) | −0.0023 (4) |
Na3 | 0.0331 (5) | 0.0210 (5) | 0.0328 (5) | 0.0088 (4) | −0.0016 (4) | 0.0015 (4) |
Ni1 | 0.01339 (18) | 0.01281 (19) | 0.0217 (2) | 0.00382 (14) | −0.00293 (13) | 0.00105 (14) |
Ni2 | 0.01376 (18) | 0.0153 (2) | 0.0209 (2) | 0.00555 (15) | −0.00365 (13) | −0.00086 (14) |
O1 | 0.0184 (8) | 0.0201 (9) | 0.0551 (11) | 0.0086 (7) | −0.0065 (7) | 0.0044 (7) |
O2 | 0.0183 (7) | 0.0148 (7) | 0.0314 (8) | 0.0056 (6) | −0.0055 (6) | −0.0002 (6) |
O3 | 0.0192 (7) | 0.0145 (7) | 0.0300 (8) | 0.0037 (6) | −0.0057 (6) | 0.0032 (6) |
O4 | 0.0215 (7) | 0.0123 (7) | 0.0319 (9) | 0.0007 (6) | 0.0012 (6) | −0.0014 (6) |
O5 | 0.0190 (7) | 0.0297 (9) | 0.0259 (8) | 0.0069 (7) | 0.0006 (6) | −0.0014 (7) |
O6 | 0.0380 (10) | 0.0236 (9) | 0.0335 (9) | 0.0120 (8) | −0.0014 (7) | 0.0012 (7) |
O7 | 0.0297 (9) | 0.0221 (8) | 0.0331 (9) | 0.0113 (7) | −0.0015 (7) | 0.0028 (7) |
O8 | 0.0461 (11) | 0.0260 (10) | 0.0315 (10) | 0.0025 (8) | −0.0076 (8) | 0.0060 (7) |
O9 | 0.0396 (10) | 0.0317 (10) | 0.0364 (10) | 0.0129 (8) | 0.0017 (8) | 0.0047 (8) |
O10 | 0.0496 (12) | 0.0456 (12) | 0.0413 (11) | 0.0139 (10) | 0.0135 (9) | 0.0134 (9) |
O11 | 0.0265 (9) | 0.0360 (10) | 0.0345 (9) | 0.0100 (8) | −0.0045 (7) | −0.0045 (8) |
O12 | 0.0193 (7) | 0.0182 (8) | 0.0300 (8) | 0.0067 (6) | −0.0067 (6) | −0.0025 (6) |
O13 | 0.0229 (8) | 0.0240 (9) | 0.0322 (9) | 0.0063 (7) | −0.0077 (7) | −0.0088 (7) |
O14 | 0.0219 (8) | 0.0253 (9) | 0.0485 (11) | 0.0128 (7) | −0.0060 (7) | −0.0007 (8) |
O15 | 0.0218 (8) | 0.0201 (8) | 0.0288 (8) | 0.0102 (7) | −0.0080 (6) | −0.0035 (6) |
O16 | 0.0189 (7) | 0.0282 (9) | 0.0283 (8) | 0.0076 (7) | −0.0001 (6) | 0.0064 (7) |
Geometric parameters (Å, º) top
C1—O1 | 1.245 (3) | Na3—O11 | 2.457 (2) |
C1—O2 | 1.259 (3) | Na3—O9 | 2.480 (2) |
C1—C2 | 1.517 (3) | Na3—O10 | 2.512 (2) |
C2—C3 | 1.518 (3) | Na3—Na3iii | 3.730 (2) |
C2—H2 | 0.9700 | Ni1—O3 | 1.9942 (17) |
C2—H1 | 0.9700 | Ni1—O3v | 1.9942 (17) |
C3—O4 | 1.242 (3) | Ni1—O2v | 2.0195 (16) |
C3—O3 | 1.265 (3) | Ni1—O2 | 2.0195 (16) |
C3—Na1i | 2.916 (3) | Ni1—O5v | 2.112 (2) |
C4—O13 | 1.247 (3) | Ni1—O5 | 2.112 (2) |
C4—O12 | 1.260 (3) | Ni2—O15 | 2.0122 (16) |
C4—C5 | 1.526 (3) | Ni2—O15iv | 2.0122 (16) |
C5—C6 | 1.519 (3) | Ni2—O12 | 2.0202 (18) |
C5—H4 | 0.9700 | Ni2—O12iv | 2.0202 (18) |
C5—H3 | 0.9700 | Ni2—O16 | 2.137 (2) |
C6—O14 | 1.252 (3) | Ni2—O16iv | 2.137 (2) |
C6—O15 | 1.259 (3) | Ni2—Na3iv | 3.430 (2) |
Na1—O4 | 2.338 (2) | O3—Na1i | 2.588 (2) |
Na1—O7 | 2.362 (2) | O4—Na1i | 2.538 (2) |
Na1—O6 | 2.430 (2) | O5—H5 | 0.8502 |
Na1—O7ii | 2.466 (2) | O5—H6 | 0.8487 |
Na1—O8 | 2.480 (2) | O6—Na2i | 2.374 (2) |
Na1—O4i | 2.538 (2) | O6—H8 | 0.8453 |
Na1—O3i | 2.588 (2) | O6—H7 | 0.8493 |
Na1—C3i | 2.916 (3) | O7—Na1ii | 2.466 (2) |
Na1—Na1i | 3.517 (2) | O7—H10 | 0.8456 |
Na1—Na1ii | 3.647 (2) | O7—H9 | 0.8462 |
Na1—Na2i | 3.773 (3) | O8—H11 | 0.8472 |
Na1—H12 | 2.5992 | O8—H12 | 0.8470 |
Na2—O6i | 2.374 (2) | O9—H14 | 0.8473 |
Na2—O4 | 2.381 (2) | O9—H13 | 0.8495 |
Na2—O13 | 2.414 (2) | O10—Na3iii | 2.341 (2) |
Na2—O8 | 2.423 (2) | O10—H16 | 0.8457 |
Na2—O9 | 2.462 (2) | O10—H15 | 0.8453 |
Na2—Cl1 | 3.0579 (17) | O11—H18 | 0.8494 |
Na2—Na1i | 3.773 (3) | O11—H17 | 0.8480 |
Na3—O10iii | 2.341 (2) | O15—Na3iv | 2.440 (2) |
Na3—O12 | 2.386 (2) | O16—H19 | 0.85 |
Na3—O15iv | 2.440 (2) | O16—H20 | 0.85 |
| | | |
O1—C1—O2 | 122.6 (2) | O10iii—Na3—O12 | 114.05 (8) |
O1—C1—C2 | 117.01 (19) | O10iii—Na3—O15iv | 105.68 (9) |
O2—C1—C2 | 120.28 (18) | O12—Na3—O15iv | 70.42 (7) |
C1—C2—C3 | 119.03 (18) | O10iii—Na3—O11 | 163.19 (8) |
C1—C2—H2 | 107.6 | O12—Na3—O11 | 82.67 (7) |
C3—C2—H2 | 107.6 | O15iv—Na3—O11 | 80.88 (8) |
C1—C2—H1 | 107.6 | O10iii—Na3—O9 | 85.95 (9) |
C3—C2—H1 | 107.6 | O12—Na3—O9 | 104.78 (7) |
H2—C2—H1 | 107.0 | O15iv—Na3—O9 | 168.36 (7) |
O4—C3—O3 | 122.3 (2) | O11—Na3—O9 | 88.04 (8) |
O4—C3—C2 | 117.43 (19) | O10iii—Na3—O10 | 79.59 (8) |
O3—C3—C2 | 120.26 (18) | O12—Na3—O10 | 156.23 (8) |
O4—C3—Na1i | 60.18 (12) | O15iv—Na3—O10 | 87.48 (8) |
O3—C3—Na1i | 62.53 (11) | O11—Na3—O10 | 85.34 (7) |
C2—C3—Na1i | 170.47 (14) | O9—Na3—O10 | 95.22 (8) |
O13—C4—O12 | 123.5 (2) | O10iii—Na3—Na3iii | 41.48 (6) |
O13—C4—C5 | 117.47 (19) | O12—Na3—Na3iii | 150.69 (7) |
O12—C4—C5 | 118.92 (19) | O15iv—Na3—Na3iii | 98.05 (7) |
C6—C5—C4 | 118.35 (19) | O11—Na3—Na3iii | 123.10 (7) |
C6—C5—H4 | 107.7 | O9—Na3—Na3iii | 90.97 (7) |
C4—C5—H4 | 107.7 | O10—Na3—Na3iii | 38.11 (5) |
C6—C5—H3 | 107.7 | O3—Ni1—O3v | 180.00 (8) |
C4—C5—H3 | 107.7 | O3—Ni1—O2v | 89.63 (7) |
H4—C5—H3 | 107.1 | O3v—Ni1—O2v | 90.37 (7) |
O14—C6—O15 | 122.6 (2) | O3—Ni1—O2 | 90.37 (7) |
O14—C6—C5 | 118.15 (19) | O3v—Ni1—O2 | 89.63 (7) |
O15—C6—C5 | 119.13 (19) | O2v—Ni1—O2 | 180.00 (7) |
O4—Na1—O7 | 87.32 (7) | O3—Ni1—O5v | 85.98 (7) |
O4—Na1—O6 | 95.88 (8) | O3v—Ni1—O5v | 94.02 (7) |
O7—Na1—O6 | 81.69 (7) | O2v—Ni1—O5v | 90.39 (7) |
O4—Na1—O7ii | 168.56 (7) | O2—Ni1—O5v | 89.61 (7) |
O7—Na1—O7ii | 81.93 (7) | O3—Ni1—O5 | 94.02 (7) |
O6—Na1—O7ii | 78.76 (7) | O3v—Ni1—O5 | 85.98 (7) |
O4—Na1—O8 | 82.85 (7) | O2v—Ni1—O5 | 89.61 (7) |
O7—Na1—O8 | 95.89 (8) | O2—Ni1—O5 | 90.39 (7) |
O6—Na1—O8 | 177.33 (7) | O5v—Ni1—O5 | 180.00 (8) |
O7ii—Na1—O8 | 102.07 (8) | O15—Ni2—O15iv | 180.00 (9) |
O4—Na1—O4i | 87.78 (7) | O15—Ni2—O12 | 92.73 (7) |
O7—Na1—O4i | 156.58 (7) | O15iv—Ni2—O12 | 87.27 (7) |
O6—Na1—O4i | 76.06 (7) | O15—Ni2—O12iv | 87.27 (7) |
O7ii—Na1—O4i | 100.56 (7) | O15iv—Ni2—O12iv | 92.73 (7) |
O8—Na1—O4i | 106.19 (7) | O12—Ni2—O12iv | 180.0 |
O4—Na1—O3i | 118.19 (7) | O15—Ni2—O16 | 93.04 (7) |
O7—Na1—O3i | 148.50 (7) | O15iv—Ni2—O16 | 86.96 (7) |
O6—Na1—O3i | 111.32 (7) | O12—Ni2—O16 | 91.00 (8) |
O7ii—Na1—O3i | 73.25 (6) | O12iv—Ni2—O16 | 89.00 (8) |
O8—Na1—O3i | 71.35 (7) | O15—Ni2—O16iv | 86.96 (7) |
O4i—Na1—O3i | 50.70 (5) | O15iv—Ni2—O16iv | 93.04 (7) |
O4—Na1—C3i | 105.12 (7) | O12—Ni2—O16iv | 89.00 (8) |
O7—Na1—C3i | 166.79 (7) | O12iv—Ni2—O16iv | 91.00 (8) |
O6—Na1—C3i | 92.43 (8) | O16—Ni2—O16iv | 180.000 (1) |
O7ii—Na1—C3i | 85.34 (7) | O15—Ni2—Na3iv | 44.41 (5) |
O8—Na1—C3i | 90.18 (8) | O15iv—Ni2—Na3iv | 135.59 (5) |
O4i—Na1—C3i | 25.13 (5) | O12—Ni2—Na3iv | 137.13 (5) |
O3i—Na1—C3i | 25.69 (5) | O12iv—Ni2—Na3iv | 42.87 (5) |
O4—Na1—Na1i | 46.15 (5) | O16—Ni2—Na3iv | 90.59 (6) |
O7—Na1—Na1i | 129.14 (7) | O16iv—Ni2—Na3iv | 89.41 (6) |
O6—Na1—Na1i | 83.93 (6) | C1—O2—Ni1 | 126.69 (14) |
O7ii—Na1—Na1i | 141.61 (7) | C3—O3—Ni1 | 127.65 (14) |
O8—Na1—Na1i | 96.81 (6) | C3—O3—Na1i | 91.78 (12) |
O4i—Na1—Na1i | 41.62 (4) | Ni1—O3—Na1i | 137.89 (8) |
O3i—Na1—Na1i | 81.77 (5) | C3—O4—Na1 | 133.73 (14) |
C3i—Na1—Na1i | 61.31 (5) | C3—O4—Na2 | 124.32 (14) |
O4—Na1—Na1ii | 129.23 (7) | Na1—O4—Na2 | 99.14 (7) |
O7—Na1—Na1ii | 42.03 (5) | C3—O4—Na1i | 94.69 (13) |
O6—Na1—Na1ii | 76.97 (6) | Na1—O4—Na1i | 92.22 (7) |
O7ii—Na1—Na1ii | 39.90 (5) | Na2—O4—Na1i | 100.12 (7) |
O8—Na1—Na1ii | 101.99 (7) | Ni1—O5—H5 | 108.2 |
O4i—Na1—Na1ii | 135.93 (6) | Ni1—O5—H6 | 117.8 |
O3i—Na1—Na1ii | 110.95 (6) | H5—O5—H6 | 107.3 |
C3i—Na1—Na1ii | 125.15 (6) | Na2i—O6—Na1 | 103.48 (8) |
Na1i—Na1—Na1ii | 159.88 (6) | Na2i—O6—H8 | 115.9 |
O4—Na1—Na2i | 94.25 (6) | Na1—O6—H8 | 108.8 |
O7—Na1—Na2i | 119.32 (6) | Na2i—O6—H7 | 110.6 |
O6—Na1—Na2i | 37.74 (5) | Na1—O6—H7 | 110.4 |
O7ii—Na1—Na2i | 87.66 (6) | H8—O6—H7 | 107.6 |
O8—Na1—Na2i | 144.58 (6) | Na1—O7—Na1ii | 98.07 (7) |
O4i—Na1—Na2i | 38.41 (4) | Na1—O7—H10 | 131.6 |
O3i—Na1—Na2i | 79.33 (5) | Na1ii—O7—H10 | 101.5 |
C3i—Na1—Na2i | 56.36 (5) | Na1—O7—H9 | 110.1 |
Na1i—Na1—Na2i | 58.92 (4) | Na1ii—O7—H9 | 102.1 |
Na1ii—Na1—Na2i | 106.83 (5) | H10—O7—H9 | 108.3 |
O4—Na1—H12 | 94.9 | Na2—O8—Na1 | 94.20 (8) |
O7—Na1—H12 | 111.2 | Na2—O8—H11 | 111.0 |
O6—Na1—H12 | 163.6 | Na1—O8—H11 | 133.4 |
O7ii—Na1—H12 | 92.7 | Na2—O8—H12 | 123.0 |
O8—Na1—H12 | 19.0 | Na1—O8—H12 | 88.5 |
O4i—Na1—H12 | 92.0 | H11—O8—H12 | 107.4 |
O3i—Na1—H12 | 52.4 | Na2—O9—Na3 | 108.16 (8) |
C3i—Na1—H12 | 72.8 | Na2—O9—H14 | 117.8 |
Na1i—Na1—H12 | 94.7 | Na3—O9—H14 | 99.0 |
Na1ii—Na1—H12 | 105.4 | Na2—O9—H13 | 119.6 |
Na2i—Na1—H12 | 129.0 | Na3—O9—H13 | 101.8 |
O6i—Na2—O4 | 80.17 (7) | H14—O9—H13 | 107.3 |
O6i—Na2—O13 | 85.13 (8) | Na3iii—O10—Na3 | 100.41 (8) |
O4—Na2—O13 | 165.19 (7) | Na3iii—O10—H16 | 123.6 |
O6i—Na2—O8 | 95.66 (8) | Na3—O10—H16 | 101.3 |
O4—Na2—O8 | 83.20 (7) | Na3iii—O10—H15 | 114.0 |
O13—Na2—O8 | 96.56 (8) | Na3—O10—H15 | 106.8 |
O6i—Na2—O9 | 179.46 (7) | H16—O10—H15 | 108.3 |
O4—Na2—O9 | 99.30 (8) | Na3—O11—H18 | 97.7 |
O13—Na2—O9 | 95.41 (8) | Na3—O11—H17 | 106.1 |
O8—Na2—O9 | 84.39 (8) | H18—O11—H17 | 107.3 |
O6i—Na2—Cl1 | 82.28 (7) | C4—O12—Ni2 | 126.47 (14) |
O4—Na2—Cl1 | 86.33 (6) | C4—O12—Na3 | 130.88 (14) |
O13—Na2—Cl1 | 93.51 (6) | Ni2—O12—Na3 | 101.94 (7) |
O8—Na2—Cl1 | 169.52 (6) | C4—O13—Na2 | 129.62 (14) |
O9—Na2—Cl1 | 97.58 (7) | C6—O15—Ni2 | 126.16 (14) |
O6i—Na2—Na1i | 38.78 (5) | C6—O15—Na3iv | 132.69 (14) |
O4—Na2—Na1i | 41.47 (5) | Ni2—O15—Na3iv | 100.35 (7) |
O13—Na2—Na1i | 123.90 (6) | Ni2—O16—H19 | 113 |
O8—Na2—Na1i | 91.51 (7) | Ni2—O16—H20 | 109.7 |
O9—Na2—Na1i | 140.68 (6) | H19—O16—H20 | 107.3 |
Cl1—Na2—Na1i | 80.43 (5) | | |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+2, −z+1; (v) −x−1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H7···O1vi | 0.85 | 1.85 | 2.699 (3) | 173 |
O7—H10···Cl1vii | 0.85 | 2.44 | 3.289 (3) | 177 |
O7—H9···O2vi | 0.85 | 2.00 | 2.830 (3) | 169 |
O8—H11···O11 | 0.85 | 1.92 | 2.768 (3) | 175 |
O8—H12···O3i | 0.85 | 2.29 | 2.957 (3) | 136 |
O8—H12···O5viii | 0.85 | 2.38 | 3.142 (3) | 150 |
O9—H14···Cl1vii | 0.85 | 2.52 | 3.336 (2) | 163 |
O9—H13···O14ix | 0.85 | 2.08 | 2.922 (3) | 170 |
O10—H16···O14iv | 0.85 | 2.29 | 2.980 (3) | 140 |
O10—H16···O13vii | 0.85 | 2.50 | 2.998 (3) | 119 |
O10—H15···Cl1vii | 0.85 | 2.49 | 3.283 (3) | 157 |
O11—H18···O16 | 0.85 | 2.17 | 3.017 (3) | 174 |
O11—H17···O13vii | 0.85 | 1.97 | 2.819 (3) | 175 |
O16—H19···Cl1viii | 0.85 | 2.38 | 3.220 (2) | 171 |
O16—H20···O14vii | 0.85 | 1.87 | 2.717 (3) | 177 |
Symmetry codes: (i) −x, −y+1, −z; (iv) −x+1, −y+2, −z+1; (vi) −x, −y, −z; (vii) x+1, y, z; (viii) x+1, y+1, z; (ix) x, y−1, z. |