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The CdII ion in the title compound, [Cd(C6H6N2O)2(H2O)4](C8H5O3)2, lies on a crystallographic inversion centre in a slightly distorted octa­hedral environment. In the crystal structure, cations and anions inter­act through inter­molecular hydrogen bonds to form a three-dimensional network. The amide group of the cation and the formyl group of the anion are each disordered over two sites, the approximate ratio of occupancies being 0.59:0.41 for both groups.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680703927X/lh2474sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680703927X/lh2474Isup2.hkl
Contains datablock I

CCDC reference: 660092

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.007 Å
  • Disorder in main residue
  • R factor = 0.048
  • wR factor = 0.151
  • Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT414_ALERT_2_B Short Intra D-H..H-X H5 .. H1N2 .. 1.88 Ang. PLAT731_ALERT_1_B Bond Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Ra O1W -H1W2 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 0.86(5), Rep 0.850(10) ...... 5.00 su-Ra O2W -H2W2 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Ra O1W -H2# 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.86(5), Rep 0.850(10) ...... 5.00 su-Ra O2W -H4# 1.555 1.555 PLAT736_ALERT_1_B H...A Calc 1.98(5), Rep 1.980(10) ...... 5.00 su-Ra H2# -O3 1.555 2.655 PLAT736_ALERT_1_B H...A Calc 1.93(5), Rep 1.930(10) ...... 5.00 su-Ra H4# -O3 1.555 4.576
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.37 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 13.00 Perc. PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... O1<I>W< CD1 O1<I>W< PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... O2<I>W< CD1 O2<I>W< PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O1W -H1W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O2W -H2W1 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O1W -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O2W -H3# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.02(4), Rep 2.020(10) ...... 4.00 su-Ra H3# -O3 1.555 3.666
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6
0 ALERT level A = In general: serious problem 7 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 15 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

Cadmium bis(4-formylbenzoate) forms a hydrated 1:2 adduct with imidazole; in the crystal structure, two molecules are linked by two Cd—Ocarboxyl interactions into a dinuclear species. The formylbenzoate anion functions in a chelating mode (Deng et al., 2006a). With the larger benzimidazole ligand, a 1:1 aqua adduct is formed, and one carboxylate anion is bidentate whereas the other is monodentate in the seven-coordinate structure (Deng et al., 2006b). Replacing the N-heterocycle by nicotinamide furnishes the title compound as a salt whose cation has two nicotinamide ligands binding to the tetraaquacadmium group; the carboxylate group is displaced from the coordination sphere and it exists as a free anion (Fig. 1). Hydrogen bonds link the cation and anion into a three-dimensional network.

Related literature top

For literature on metal 4-formylbenzoates, see, for example: Deng et al. (2006a,b).

Experimental top

Cadmium diacetate dihydrate (0.133 g, 0.5 mmol) was added to an aqueous solution of 4-formylbenzoic acid (0.15 g, 1 mmol) and nicotinamide (0.122 g, 1 mmol). The pH value of the mixture was about 5. The solution was set aside for the growth of colorless prismatic crystals. CH&N elemental analysis. Calc. for C28H30N4O12Cd: C 46.26, H 4.16, N 7.71%. Found: C 46.24, H 4.11, N 7.76%.

Refinement top

The amido and formyl parts are disordered over two positions; the occupancies refined to a 0.59 (1):0.41 ratio for both groups. The C6—O1 and C6—O1' bond distances were restrained to within 0.01 Å of each other, as were the C6—N1 and C6—N1' distances. The carbon- and nitrogen bound H atoms were generated geometrically (C—H 0.93, N—H 0.86 Å) and were included in the refinement in the riding-model approximation, with U(H) set to 1.2Ueq(C,N). The water H atoms were located in a difference Fourier map, and were refined with a distance restraint of O—H 0.85 (1) Å; their Uiso(H) values were freely refined. The final difference Fourier map had a large peak at about 1 Å from O3, but was otherwise diffuse.

Structure description top

Cadmium bis(4-formylbenzoate) forms a hydrated 1:2 adduct with imidazole; in the crystal structure, two molecules are linked by two Cd—Ocarboxyl interactions into a dinuclear species. The formylbenzoate anion functions in a chelating mode (Deng et al., 2006a). With the larger benzimidazole ligand, a 1:1 aqua adduct is formed, and one carboxylate anion is bidentate whereas the other is monodentate in the seven-coordinate structure (Deng et al., 2006b). Replacing the N-heterocycle by nicotinamide furnishes the title compound as a salt whose cation has two nicotinamide ligands binding to the tetraaquacadmium group; the carboxylate group is displaced from the coordination sphere and it exists as a free anion (Fig. 1). Hydrogen bonds link the cation and anion into a three-dimensional network.

For literature on metal 4-formylbenzoates, see, for example: Deng et al. (2006a,b).

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: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot of the formula unit of the salt, [(C6H6N2O)2(H2O)4Cd]2+ 2[C8H5O3]-; only the major disorder components is shown. Displacement ellipsoids are drawn at the 50% probability level, and H atoms are drawn as spheres of arbitrary radius. Symmetry code: i = 1 – x, 1 – y, 1 – z.
Tetraaquabis(nicotinamide-κN)cadmium(II) bis(4-formylbenzoate) top
Crystal data top
[Cd(C6H6N2O)2(H2O)4](C8H5O3)2F(000) = 740
Mr = 726.96Dx = 1.657 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 10447 reflections
a = 14.922 (1) Åθ = 3.1–27.5°
b = 7.0382 (4) ŵ = 0.82 mm1
c = 14.030 (1) ÅT = 295 K
β = 98.634 (2)°Prism, colourless
V = 1456.8 (2) Å30.35 × 0.24 × 0.18 mm
Z = 2
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
3332 independent reflections
Radiation source: fine-focus sealed tube2816 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1919
Tmin = 0.680, Tmax = 0.866k = 98
13559 measured reflectionsl = 1718
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.151H atoms treated by a mixture of independent and constrained refinement
S = 1.14 w = 1/[σ2(Fo2) + (0.0584P)2 + 5.994P]
where P = (Fo2 + 2Fc2)/3
3332 reflections(Δ/σ)max = 0.001
249 parametersΔρmax = 1.08 e Å3
6 restraintsΔρmin = 0.46 e Å3
Crystal data top
[Cd(C6H6N2O)2(H2O)4](C8H5O3)2V = 1456.8 (2) Å3
Mr = 726.96Z = 2
Monoclinic, P21/cMo Kα radiation
a = 14.922 (1) ŵ = 0.82 mm1
b = 7.0382 (4) ÅT = 295 K
c = 14.030 (1) Å0.35 × 0.24 × 0.18 mm
β = 98.634 (2)°
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
3332 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
2816 reflections with I > 2σ(I)
Tmin = 0.680, Tmax = 0.866Rint = 0.035
13559 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0486 restraints
wR(F2) = 0.151H atoms treated by a mixture of independent and constrained refinement
S = 1.14Δρmax = 1.08 e Å3
3332 reflectionsΔρmin = 0.46 e Å3
249 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cd10.50000.50000.50000.03018 (17)
O1W0.4608 (3)0.7588 (6)0.4012 (3)0.0380 (8)
H1W10.415 (2)0.739 (9)0.359 (3)0.042 (16)*
H1W20.498 (3)0.835 (7)0.381 (4)0.046 (18)*
O2W0.5403 (3)0.6836 (6)0.6390 (3)0.0429 (9)
H2W10.550 (4)0.626 (8)0.693 (2)0.047 (17)*
H2W20.503 (3)0.771 (7)0.649 (5)0.053 (19)*
O10.9598 (11)0.607 (3)0.579 (2)0.059 (5)0.589 (12)
N10.8621 (11)0.553 (2)0.6850 (11)0.047 (3)0.589 (12)
H1N10.90560.54240.73250.056*0.589 (12)
H1N20.80680.54080.69450.056*0.589 (12)
O1'0.8628 (13)0.638 (2)0.6856 (12)0.045 (4)0.411 (12)
N1'0.9589 (15)0.547 (5)0.587 (3)0.048 (7)0.411 (12)
H1N31.00320.55480.63380.057*0.411 (12)
H1N40.96870.51330.53070.057*0.411 (12)
O20.3258 (3)0.6507 (8)0.2597 (3)0.0641 (14)
O30.4294 (3)0.5203 (6)0.1818 (3)0.0447 (9)
O40.0030 (5)0.6015 (14)0.1545 (5)0.061 (3)0.589 (12)
O4'0.1012 (6)0.5493 (16)0.2424 (6)0.044 (3)0.411 (12)
N20.6443 (3)0.5390 (6)0.4632 (3)0.0329 (9)
C10.6592 (3)0.5775 (7)0.3732 (4)0.0348 (10)
H10.61040.57210.32350.042*
C20.7431 (4)0.6246 (8)0.3510 (3)0.0376 (11)
H20.75040.65530.28810.045*
C30.8166 (3)0.6255 (8)0.4242 (4)0.0352 (10)
H30.87430.65390.41080.042*
C40.8033 (3)0.5835 (7)0.5178 (3)0.0303 (9)
C50.7159 (3)0.5422 (7)0.5338 (3)0.0320 (10)
H50.70650.51540.59640.038*
C60.8796 (3)0.5866 (8)0.6012 (4)0.0388 (11)
C70.3503 (4)0.5841 (8)0.1864 (3)0.0361 (11)
C80.2813 (3)0.5820 (7)0.0956 (3)0.0314 (9)
C90.3067 (4)0.5421 (7)0.0065 (4)0.0361 (11)
H90.36670.51240.00250.043*
C100.2440 (4)0.5460 (8)0.0759 (4)0.0400 (12)
H100.26250.52570.13550.048*
C110.1527 (3)0.5804 (8)0.0705 (4)0.0360 (10)
C120.1262 (4)0.6195 (8)0.0193 (4)0.0414 (12)
H120.06560.64290.02400.050*
C130.1909 (3)0.6228 (8)0.1008 (4)0.0375 (11)
H130.17370.65270.16010.045*
C140.0842 (4)0.5798 (9)0.1583 (4)0.0465 (13)
H140.10300.56250.21790.056*0.589 (12)
H14'0.02430.60360.15100.056*0.411 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0234 (2)0.0379 (3)0.0283 (2)0.0023 (2)0.00111 (16)0.0026 (2)
O1W0.039 (2)0.040 (2)0.0349 (18)0.0032 (17)0.0037 (15)0.0051 (16)
O2W0.046 (2)0.041 (2)0.039 (2)0.0073 (18)0.0027 (17)0.0019 (17)
O10.029 (5)0.090 (15)0.061 (7)0.017 (6)0.009 (5)0.013 (10)
N10.030 (4)0.066 (9)0.039 (5)0.013 (7)0.009 (4)0.006 (6)
O1'0.041 (6)0.058 (10)0.034 (6)0.011 (8)0.003 (4)0.006 (7)
N1'0.026 (8)0.058 (16)0.053 (12)0.000 (8)0.013 (7)0.008 (11)
O20.058 (3)0.100 (4)0.0311 (19)0.025 (3)0.0045 (18)0.005 (2)
O30.045 (2)0.044 (2)0.044 (2)0.0017 (17)0.0005 (16)0.0002 (17)
O40.034 (4)0.107 (7)0.039 (4)0.010 (4)0.010 (3)0.007 (4)
O4'0.028 (4)0.075 (7)0.027 (4)0.010 (4)0.000 (3)0.000 (4)
N20.0265 (19)0.037 (2)0.035 (2)0.0021 (16)0.0027 (16)0.0034 (17)
C10.035 (2)0.035 (2)0.033 (2)0.003 (2)0.0001 (19)0.002 (2)
C20.043 (3)0.043 (3)0.029 (2)0.007 (2)0.011 (2)0.001 (2)
C30.030 (2)0.039 (3)0.039 (3)0.000 (2)0.0111 (19)0.001 (2)
C40.025 (2)0.032 (2)0.033 (2)0.0003 (19)0.0017 (17)0.0002 (19)
C50.029 (2)0.037 (3)0.030 (2)0.0011 (19)0.0039 (18)0.0063 (19)
C60.028 (2)0.043 (3)0.043 (3)0.003 (2)0.001 (2)0.000 (2)
C70.040 (3)0.040 (3)0.028 (2)0.002 (2)0.005 (2)0.005 (2)
C80.036 (2)0.027 (2)0.031 (2)0.004 (2)0.0028 (19)0.0007 (19)
C90.035 (2)0.040 (3)0.034 (2)0.002 (2)0.009 (2)0.003 (2)
C100.044 (3)0.043 (3)0.033 (2)0.000 (2)0.009 (2)0.002 (2)
C110.035 (2)0.032 (2)0.040 (3)0.005 (2)0.003 (2)0.001 (2)
C120.033 (2)0.046 (3)0.045 (3)0.001 (2)0.003 (2)0.007 (2)
C130.040 (3)0.038 (3)0.035 (2)0.001 (2)0.010 (2)0.002 (2)
C140.043 (3)0.050 (3)0.045 (3)0.005 (3)0.001 (2)0.003 (3)
Geometric parameters (Å, º) top
Cd1—N22.305 (4)C1—C21.376 (7)
Cd1—N2i2.305 (4)C1—H10.9300
Cd1—O1wi2.311 (4)C2—C31.385 (7)
Cd1—O1w2.311 (4)C2—H20.9300
Cd1—O2w2.342 (4)C3—C41.389 (7)
Cd1—O2wi2.342 (4)C3—H30.9300
O1W—H1W10.85 (1)C4—C51.387 (6)
O1W—H1W20.85 (1)C4—C61.505 (7)
O2W—H2W10.85 (1)C5—H50.9300
O2W—H2W20.85 (1)C7—C81.512 (7)
O1—C61.289 (15)C8—C91.388 (7)
N1—C61.264 (16)C8—C131.392 (7)
N1—H1N10.8600C9—C101.373 (8)
N1—H1N20.8600C9—H90.9300
O1'—C61.299 (15)C10—C111.397 (7)
N1'—C61.259 (19)C10—H100.9300
N1'—H1N30.8600C11—C121.404 (7)
N1'—H1N40.8600C11—C141.477 (7)
O2—C71.235 (6)C12—C131.381 (7)
O3—C71.274 (7)C12—H120.9300
O4—C141.231 (9)C13—H130.9300
O4'—C141.263 (10)C14—H140.9300
N2—C11.342 (6)C14—H14'0.9300
N2—C51.344 (6)
N2—Cd1—N2i180.00 (5)C5—C4—C6119.8 (4)
N2—Cd1—O1Wi93.85 (14)C3—C4—C6122.2 (4)
N2i—Cd1—O1Wi86.15 (14)N2—C5—C4123.2 (4)
N2—Cd1—O1W86.15 (14)N2—C5—H5118.4
N2i—Cd1—O1W93.85 (14)C4—C5—H5118.4
O1Wi—Cd1—O1W180.00 (15)N1'—C6—N1116 (2)
N2—Cd1—O2W89.39 (15)N1—C6—O1125.1 (15)
N2i—Cd1—O2W90.61 (15)N1'—C6—O1'121 (2)
O1Wi—Cd1—O2W85.69 (14)O1—C6—O1'120.1 (15)
O1W—Cd1—O2W94.31 (14)N1'—C6—C4120 (2)
N2—Cd1—O2Wi90.61 (15)N1—C6—C4118.9 (8)
N2i—Cd1—O2Wi89.39 (15)O1—C6—C4115.7 (13)
O1Wi—Cd1—O2Wi94.31 (14)O1'—C6—C4119.0 (9)
O1W—Cd1—O2Wi85.69 (14)O2—C7—O3124.6 (5)
O2W—Cd1—O2Wi180.0O2—C7—C8117.1 (5)
Cd1—O1W—H1W1113 (4)O3—C7—C8118.3 (4)
Cd1—O1W—H1W2126 (4)C9—C8—C13119.0 (5)
H1W1—O1W—H1W2111 (6)C9—C8—C7121.1 (4)
Cd1—O2W—H2W1118 (5)C13—C8—C7119.8 (4)
Cd1—O2W—H2W2116 (5)C10—C9—C8120.7 (5)
H2W1—O2W—H2W2103 (6)C10—C9—H9119.6
C6—N1—H1N1120.0C8—C9—H9119.6
C6—N1—H1N2120.0C9—C10—C11120.3 (5)
H1N1—N1—H1N2120.0C9—C10—H10119.8
C6—N1'—H1N3120.0C11—C10—H10119.8
C6—N1'—H1N4120.0C10—C11—C12119.4 (5)
H1N3—N1'—H1N4120.0C10—C11—C14120.9 (5)
C1—N2—C5117.7 (4)C12—C11—C14119.7 (5)
C1—N2—Cd1121.8 (3)C13—C12—C11119.3 (5)
C5—N2—Cd1120.2 (3)C13—C12—H12120.3
N2—C1—C2123.1 (5)C11—C12—H12120.3
N2—C1—H1118.4C12—C13—C8121.1 (5)
C2—C1—H1118.4C12—C13—H13119.5
C1—C2—C3118.7 (5)C8—C13—H13119.5
C1—C2—H2120.7O4—C14—C11121.8 (6)
C3—C2—H2120.7O4'—C14—C11124.6 (6)
C2—C3—C4119.3 (4)O4—C14—H14119.1
C2—C3—H3120.3C11—C14—H14119.1
C4—C3—H3120.3O4'—C14—H14'117.7
C5—C4—C3118.0 (4)C11—C14—H14'117.7
O1Wi—Cd1—N2—C1137.5 (4)C5—C4—C6—O1173.3 (11)
O1W—Cd1—N2—C142.5 (4)C3—C4—C6—O18.3 (13)
O2W—Cd1—N2—C1136.8 (4)C5—C4—C6—O1'31.8 (11)
O2Wi—Cd1—N2—C143.2 (4)C3—C4—C6—O1'146.6 (9)
O1Wi—Cd1—N2—C549.1 (4)O2—C7—C8—C9168.4 (5)
O1W—Cd1—N2—C5130.9 (4)O3—C7—C8—C910.6 (7)
O2W—Cd1—N2—C536.6 (4)O2—C7—C8—C1310.9 (8)
O2Wi—Cd1—N2—C5143.4 (4)O3—C7—C8—C13170.1 (5)
C5—N2—C1—C21.8 (8)C13—C8—C9—C101.2 (8)
Cd1—N2—C1—C2171.7 (4)C7—C8—C9—C10178.1 (5)
N2—C1—C2—C32.5 (8)C8—C9—C10—C113.4 (8)
C1—C2—C3—C41.5 (8)C9—C10—C11—C122.9 (8)
C2—C3—C4—C50.0 (8)C9—C10—C11—C14178.3 (5)
C2—C3—C4—C6178.5 (5)C10—C11—C12—C130.1 (8)
C1—N2—C5—C40.1 (7)C14—C11—C12—C13179.0 (5)
Cd1—N2—C5—C4173.5 (4)C11—C12—C13—C82.1 (8)
C3—C4—C5—N20.7 (8)C9—C8—C13—C121.6 (8)
C6—C4—C5—N2179.2 (5)C7—C8—C13—C12179.1 (5)
C5—C4—C6—N1'151.4 (18)C10—C11—C14—O4176.8 (8)
C3—C4—C6—N1'30.1 (19)C12—C11—C14—O44.4 (11)
C5—C4—C6—N10.7 (11)C10—C11—C14—O4'0.1 (11)
C3—C4—C6—N1177.7 (9)C12—C11—C14—O4'178.9 (8)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O20.85 (1)1.88 (2)2.715 (6)168 (6)
O1W—H1W2···O3ii0.85 (1)1.98 (1)2.828 (6)172 (6)
O2W—H2W1···O3i0.85 (1)2.02 (1)2.871 (6)178 (7)
O2W—H2W2···O3iii0.85 (1)1.93 (1)2.782 (6)174 (7)
N1—H1N1···O4iv0.862.032.86 (2)163
N1—H1N3···O4iv0.862.102.95 (4)173
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y+1/2, z+1/2; (iii) x, y+3/2, z+1/2; (iv) x+1, y, z+1.

Experimental details

Crystal data
Chemical formula[Cd(C6H6N2O)2(H2O)4](C8H5O3)2
Mr726.96
Crystal system, space groupMonoclinic, P21/c
Temperature (K)295
a, b, c (Å)14.922 (1), 7.0382 (4), 14.030 (1)
β (°) 98.634 (2)
V3)1456.8 (2)
Z2
Radiation typeMo Kα
µ (mm1)0.82
Crystal size (mm)0.35 × 0.24 × 0.18
Data collection
DiffractometerRigaku R-AXIS RAPID IP
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.680, 0.866
No. of measured, independent and
observed [I > 2σ(I)] reflections
13559, 3332, 2816
Rint0.035
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.048, 0.151, 1.14
No. of reflections3332
No. of parameters249
No. of restraints6
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.08, 0.46

Computer programs: RAPID-AUTO (Rigaku, 1998), RAPID-AUTO, CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O20.85 (1)1.88 (2)2.715 (6)168 (6)
O1W—H1W2···O3i0.85 (1)1.98 (1)2.828 (6)172 (6)
O2W—H2W1···O3ii0.85 (1)2.02 (1)2.871 (6)178 (7)
O2W—H2W2···O3iii0.85 (1)1.93 (1)2.782 (6)174 (7)
N1—H1N1···O4iv0.862.032.86 (2)163
N1'—H1N3···O4'iv0.862.102.95 (4)173
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x+1, y+1, z+1; (iii) x, y+3/2, z+1/2; (iv) x+1, y, z+1.
 

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