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In the title compound, Na2[Ni(C3H2O4)2(H2O)2]·2H2O, the Ni atom is coordinated by four O atoms from two malonate ligands and two water mol­ecules in a distorted octa­hedral geometry. The two independent Na+ ions are coordinated by five and six O atoms, respectively. The crystal structure is stabilized by the three-dimensional hydrogen-bonding network formed by O—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806055632/cv2171sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806055632/cv2171Isup2.hkl
Contains datablock I

CCDC reference: 636229

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.005 Å
  • Disorder in main residue
  • R factor = 0.035
  • wR factor = 0.082
  • Data-to-parameter ratio = 15.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 1
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.12 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.44 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O12A PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.23 Ratio
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.48 From the CIF: _reflns_number_total 2858 Count of symmetry unique reflns 1724 Completeness (_total/calc) 165.78% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1134 Fraction of Friedel pairs measured 0.658 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

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.

Disodium diaquabis(malonato-κ2O,O')nickel(II) dihydrate top
Crystal data top
Na2[Ni(C3H2O4)2(H2O)2]·2H2OF(000) = 776
Mr = 380.85Dx = 1.954 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 10182 reflections
a = 7.287 (3) Åθ = 6.1–55.1°
b = 10.070 (5) ŵ = 1.63 mm1
c = 17.646 (10) ÅT = 291 K
V = 1294.9 (11) Å3Block, green
Z = 40.30 × 0.29 × 0.22 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
2858 independent reflections
Radiation source: fine-focus sealed tube2678 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 99
Tmin = 0.639, Tmax = 0.712k = 1311
11928 measured reflectionsl = 2222
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H-atom parameters constrained
wR(F2) = 0.082 w = 1/[σ2(Fo2) + (0.0527P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
2858 reflectionsΔρmax = 0.94 e Å3
190 parametersΔρmin = 0.49 e Å3
6 restraintsAbsolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.009 (15)
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
xyzUiso*/UeqOcc. (<1)
C10.9032 (4)0.8623 (3)0.67488 (16)0.0249 (6)
C20.9735 (4)0.9916 (3)0.70892 (18)0.0268 (7)
H11.06020.96970.74870.032*
H21.04071.03890.66990.032*
C30.8325 (4)1.0845 (3)0.74146 (16)0.0189 (5)
C40.5507 (4)0.5950 (3)0.87993 (16)0.0212 (6)
C50.4454 (6)0.6693 (4)0.9404 (2)0.0350 (8)
H30.31620.65710.92900.042*
H40.46820.62320.98780.042*
C60.4716 (4)0.8154 (3)0.95634 (17)0.0239 (6)
Na10.39261 (18)1.09929 (14)0.81517 (8)0.0329 (3)
Na20.3528 (4)1.08315 (18)1.01614 (11)0.0664 (6)
Ni10.66821 (5)0.84807 (4)0.810627 (19)0.01772 (10)
O10.7798 (3)0.7983 (2)0.70965 (12)0.0240 (5)
O20.9703 (4)0.8261 (3)0.61386 (15)0.0439 (7)
O30.7190 (3)1.0434 (2)0.79097 (12)0.0246 (5)
O40.8334 (3)1.2013 (2)0.71909 (14)0.0301 (5)
O50.6104 (3)0.6541 (2)0.82266 (11)0.0237 (4)
O60.5712 (5)0.4727 (2)0.88942 (15)0.0432 (7)
O70.5444 (3)0.8935 (2)0.90976 (13)0.0296 (5)
O80.4078 (4)0.8538 (3)1.01879 (13)0.0387 (6)
O90.9173 (3)0.8222 (2)0.86757 (12)0.0249 (5)
H50.99170.78960.83580.037*
H60.91830.77240.90670.037*
O100.4169 (3)0.8827 (2)0.75736 (12)0.0257 (5)
H80.32300.83410.76230.039*
H70.41880.91250.71240.039*
O110.1439 (4)1.0618 (3)0.90675 (15)0.0406 (6)
H90.08991.13400.89480.061*
H100.06480.99980.90210.061*
O120.5554 (13)1.2054 (7)0.9193 (4)0.060 (2)*0.616 (19)
H120.65421.22480.89340.090*0.616 (19)
H110.56661.12340.93070.090*0.616 (19)
O12A0.468 (3)1.2210 (12)0.9338 (7)0.074 (4)*0.384 (19)
H12A0.38581.26840.92020.110*0.384 (19)
H11A0.53191.25790.96890.110*0.384 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0306 (14)0.0226 (16)0.0214 (14)0.0007 (12)0.0027 (10)0.0020 (12)
C20.0258 (14)0.0178 (15)0.0368 (18)0.0004 (12)0.0108 (12)0.0018 (12)
C30.0191 (12)0.0147 (13)0.0227 (13)0.0025 (11)0.0009 (11)0.0025 (9)
C40.0273 (15)0.0157 (14)0.0207 (14)0.0037 (11)0.0007 (11)0.0023 (10)
C50.053 (2)0.0237 (17)0.0284 (17)0.0047 (15)0.0140 (14)0.0008 (13)
C60.0278 (15)0.0266 (17)0.0171 (13)0.0023 (12)0.0041 (11)0.0020 (11)
Na10.0351 (7)0.0300 (7)0.0337 (7)0.0045 (5)0.0047 (5)0.0003 (6)
Na20.1113 (17)0.0398 (10)0.0482 (10)0.0077 (10)0.0415 (11)0.0045 (7)
Ni10.02099 (16)0.01576 (17)0.01640 (16)0.00020 (14)0.00253 (13)0.00098 (13)
O10.0294 (11)0.0218 (11)0.0210 (11)0.0058 (8)0.0061 (8)0.0020 (8)
O20.0649 (17)0.0340 (15)0.0327 (13)0.0167 (13)0.0257 (12)0.0103 (11)
O30.0268 (10)0.0187 (10)0.0284 (12)0.0005 (8)0.0060 (8)0.0016 (8)
O40.0269 (10)0.0199 (10)0.0433 (13)0.0015 (10)0.0095 (10)0.0046 (9)
O50.0357 (10)0.0171 (10)0.0183 (10)0.0017 (8)0.0030 (7)0.0002 (8)
O60.0778 (19)0.0191 (13)0.0328 (14)0.0038 (12)0.0088 (13)0.0029 (10)
O70.0429 (13)0.0212 (11)0.0248 (12)0.0026 (10)0.0104 (9)0.0002 (9)
O80.0611 (15)0.0330 (14)0.0219 (11)0.0072 (13)0.0158 (10)0.0004 (11)
O90.0291 (10)0.0249 (12)0.0208 (10)0.0054 (9)0.0004 (8)0.0020 (8)
O100.0232 (10)0.0259 (12)0.0280 (11)0.0054 (8)0.0003 (8)0.0073 (9)
O110.0468 (15)0.0350 (13)0.0399 (14)0.0063 (12)0.0021 (11)0.0052 (11)
Geometric parameters (Å, º) top
C1—O21.237 (4)Na2—O12A2.178 (13)
C1—O11.265 (4)Na2—O2ii2.339 (3)
C1—C21.523 (4)Na2—O82.345 (4)
C2—C31.504 (4)Na2—O112.468 (3)
C2—H10.9700Na2—O122.572 (8)
C2—H20.9700Na2—O6iii2.703 (4)
C3—O41.240 (4)Na2—H112.2055
C3—O31.272 (4)Na2—H12A2.5310
C4—O51.251 (4)Na2—H11A2.3444
C4—O61.252 (4)Ni1—O52.009 (2)
C4—C51.512 (5)Ni1—O72.021 (2)
C5—C61.511 (5)Ni1—O12.022 (2)
C5—H30.9700Ni1—O32.032 (2)
C5—H40.9700Ni1—O102.088 (2)
C6—O71.255 (4)Ni1—O92.091 (2)
C6—O81.257 (4)Ni1—Na1iv3.376 (2)
Na1—O1i2.406 (3)O1—Na1iv2.406 (3)
Na1—O102.415 (3)O2—Na2v2.339 (3)
Na1—O122.434 (6)O5—Na1iv2.494 (3)
Na1—O112.458 (3)O6—Na2vi2.703 (4)
Na1—O32.481 (3)O9—H50.8464
Na1—O12A2.486 (12)O9—H60.8537
Na1—O5i2.494 (3)O10—H80.8452
Na1—O72.881 (3)O10—H70.8485
Na1—Ni1i3.376 (2)O11—H90.8535
Na1—H72.6196O11—H100.8529
Na1—H92.6393O12—H120.8749
Na1—H122.6718O12—H110.8537
Na1—H112.4129O12A—H12A0.8032
Na1—H12A2.5173O12A—H11A0.8599
O2—C1—O1123.5 (3)H11—Na1—H12A47.2
O2—C1—C2117.5 (3)O12A—Na2—O2ii91.7 (3)
O1—C1—C2118.9 (3)O12A—Na2—O8125.1 (5)
C3—C2—C1116.9 (3)O2ii—Na2—O8106.00 (12)
C3—C2—H1108.1O12A—Na2—O1176.8 (4)
C1—C2—H1108.1O2ii—Na2—O11161.96 (13)
C3—C2—H2108.1O8—Na2—O1192.02 (11)
C1—C2—H2108.1O12A—Na2—O1214.2 (4)
H1—C2—H2107.3O2ii—Na2—O1289.22 (18)
O4—C3—O3122.0 (3)O8—Na2—O12112.7 (2)
O4—C3—C2117.7 (3)O11—Na2—O1282.89 (17)
O3—C3—C2120.3 (2)O12A—Na2—O6iii146.8 (5)
O5—C4—O6122.3 (3)O2ii—Na2—O6iii92.60 (12)
O5—C4—C5120.8 (3)O8—Na2—O6iii84.98 (11)
O6—C4—C5116.9 (3)O11—Na2—O6iii89.76 (13)
C6—C5—C4123.3 (3)O12—Na2—O6iii160.9 (2)
C6—C5—H3106.5O12A—Na2—H1132.3
C4—C5—H3106.5O2ii—Na2—H1192.4
C6—C5—H4106.5O8—Na2—H1194.2
C4—C5—H4106.5O11—Na2—H1185.2
H3—C5—H4106.5O12—Na2—H1118.6
O7—C6—O8122.5 (3)O6iii—Na2—H11174.9
O7—C6—C5122.8 (3)O12A—Na2—H12A17.7
O8—C6—C5114.6 (3)O2ii—Na2—H12A98.8
O1i—Na1—O10135.56 (10)O8—Na2—H12A136.3
O1i—Na1—O1291.5 (2)O11—Na2—H12A66.4
O10—Na1—O12132.8 (2)O12—Na2—H12A31.6
O1i—Na1—O1182.10 (9)O6iii—Na2—H12A129.7
O10—Na1—O11101.12 (10)H11—Na2—H12A48.7
O12—Na1—O1186.0 (2)O12A—Na2—H11A21.5
O1i—Na1—O3131.17 (10)O2ii—Na2—H11A70.2
O10—Na1—O369.65 (8)O8—Na2—H11A130.6
O12—Na1—O376.2 (3)O11—Na2—H11A97.5
O11—Na1—O3141.75 (11)O12—Na2—H11A23.8
O1i—Na1—O12A81.8 (4)O6iii—Na2—H11A143.0
O10—Na1—O12A141.7 (3)H11—Na2—H11A39.2
O12—Na1—O12A16.4 (3)H12A—Na2—H11A32.4
O11—Na1—O12A71.7 (4)O5—Ni1—O792.01 (9)
O3—Na1—O12A92.6 (5)O5—Ni1—O186.36 (8)
O1i—Na1—O5i68.50 (8)O7—Ni1—O1177.04 (10)
O10—Na1—O5i77.81 (9)O5—Ni1—O3175.94 (9)
O12—Na1—O5i130.02 (19)O7—Ni1—O390.57 (9)
O11—Na1—O5i131.97 (10)O1—Ni1—O390.93 (9)
O3—Na1—O5i83.73 (8)O5—Ni1—O1091.48 (9)
O12A—Na1—O5i135.5 (3)O7—Ni1—O1087.72 (10)
O1i—Na1—O7154.82 (9)O1—Ni1—O1089.85 (9)
O10—Na1—O764.33 (8)O3—Ni1—O1085.49 (9)
O12—Na1—O772.03 (17)O5—Ni1—O990.58 (9)
O11—Na1—O777.96 (9)O7—Ni1—O989.99 (10)
O3—Na1—O764.45 (8)O1—Ni1—O992.49 (9)
O12A—Na1—O777.4 (3)O3—Ni1—O992.55 (9)
O5i—Na1—O7136.68 (8)O10—Ni1—O9176.97 (9)
O1i—Na1—Ni1i36.26 (5)O5—Ni1—Na1iv47.21 (6)
O10—Na1—Ni1i113.72 (8)O7—Ni1—Na1iv132.72 (8)
O12—Na1—Ni1i103.56 (16)O1—Ni1—Na1iv44.72 (7)
O11—Na1—Ni1i116.72 (8)O3—Ni1—Na1iv129.06 (7)
O3—Na1—Ni1i100.42 (7)O10—Ni1—Na1iv73.30 (7)
O12A—Na1—Ni1i102.5 (3)O9—Ni1—Na1iv109.72 (7)
O5i—Na1—Ni1i36.24 (5)C1—O1—Ni1125.9 (2)
O7—Na1—Ni1i164.76 (7)C1—O1—Na1iv135.0 (2)
O1i—Na1—H7120.7Ni1—O1—Na1iv99.02 (9)
O10—Na1—H718.8C1—O2—Na2v138.1 (2)
O12—Na1—H7143.3C3—O3—Ni1123.41 (18)
O11—Na1—H7113.5C3—O3—Na1131.88 (19)
O3—Na1—H769.4Ni1—O3—Na190.89 (9)
O12A—Na1—H7157.0C4—O5—Ni1128.4 (2)
O5i—Na1—H759.0C4—O5—Na1iv132.8 (2)
O7—Na1—H781.8Ni1—O5—Na1iv96.55 (8)
Ni1i—Na1—H795.0C4—O6—Na2vi112.2 (2)
O1i—Na1—H963.3C6—O7—Ni1127.9 (2)
O10—Na1—H9113.9C6—O7—Na1131.9 (2)
O12—Na1—H987.0Ni1—O7—Na180.38 (8)
O11—Na1—H918.8C6—O8—Na2110.4 (2)
O3—Na1—H9157.4Ni1—O9—H5106.6
O12A—Na1—H970.8Ni1—O9—H6118.0
O5i—Na1—H9118.9H5—O9—H6107.7
O7—Na1—H996.2Ni1—O10—Na191.42 (9)
Ni1i—Na1—H998.2Ni1—O10—H8124.5
H7—Na1—H9121.7Na1—O10—H8114.8
O1i—Na1—H1294.2Ni1—O10—H7117.7
O10—Na1—H12126.4Na1—O10—H794.4
O12—Na1—H1219.0H8—O10—H7108.3
O11—Na1—H12105.0Na1—O11—Na292.64 (13)
O3—Na1—H1260.8Na1—O11—H992.7
O12A—Na1—H1234.3Na2—O11—H9113.7
O5i—Na1—H12113.9Na1—O11—H10123.2
O7—Na1—H1276.5Na2—O11—H10123.7
Ni1i—Na1—H1294.7H9—O11—H10106.8
H7—Na1—H12130.2Na1—O12—Na290.7 (2)
H9—Na1—H12105.0Na1—O12—H1296.1
O1i—Na1—H11110.1Na2—O12—H12157.9
O10—Na1—H11114.2Na1—O12—H1178.5
O12—Na1—H1120.3Na2—O12—H1155.6
O11—Na1—H1181.2H12—O12—H11105.1
O3—Na1—H1170.4Na1—O12—H12A77.0
O12A—Na1—H1128.7Na2—O12—H12A72.6
O5i—Na1—H11143.7H12—O12—H12A129.5
O7—Na1—H1151.8H11—O12—H12A121.6
Ni1i—Na1—H11123.3Na1—O12—H11A141.3
H7—Na1—H11128.2Na2—O12—H11A65.7
H9—Na1—H1188.6H12—O12—H11A117.5
H12—Na1—H1130.8H11—O12—H11A108.0
O1i—Na1—H12A63.9H12A—O12—H11A67.1
O10—Na1—H12A157.5Na2—O12A—Na199.3 (5)
O12—Na1—H12A32.5Na2—O12A—H1175.1
O11—Na1—H12A66.8Na1—O12A—H1172.3
O3—Na1—H12A107.4Na2—O12A—H12A106.9
O12A—Na1—H12A18.5Na1—O12A—H12A82.9
O5i—Na1—H12A124.6H11—O12A—H12A155.0
O7—Na1—H12A93.9Na2—O12A—H11A90.2
Ni1i—Na1—H12A88.8Na1—O12A—H11A160.0
H7—Na1—H12A175.4H11—O12A—H11A93.5
H9—Na1—H12A60.1H12A—O12A—H11A111.2
H12—Na1—H12A46.7
Symmetry codes: (i) x+1, y+1/2, z+3/2; (ii) x+3/2, y+2, z+1/2; (iii) x1/2, y+3/2, z+2; (iv) x+1, y1/2, z+3/2; (v) x+3/2, y+2, z1/2; (vi) x+1/2, y+3/2, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H5···O4vii0.851.832.669 (3)170
O9—H6···O8vi0.851.832.677 (4)171
O10—H8···O4iv0.851.792.614 (3)165
O10—H7···O6i0.851.902.746 (4)178
O11—H9···O2i0.851.992.813 (4)162
O11—H10···O9viii0.852.173.004 (4)164
Symmetry codes: (i) x+1, y+1/2, z+3/2; (iv) x+1, y1/2, z+3/2; (vi) x+1/2, y+3/2, z+2; (vii) x+2, y1/2, z+3/2; (viii) x1, y, z.
 

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