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The reaction of cadmium(II) chloride monohydrate with a self-assembling pyridine-containing ligand, LH2 {LH2 is [H2pyda]2+[pydc]2−, where pyda = 2,6-di­amino­pyridine and H2pydc = pyridine-2,6-di­carboxyl­ic acid}, in water leads to the formation of a centrosymmetric dinuclear CdII complex, di-μ-pyridine-2,6-di­carboxyl­ato-bis­[tri­aqua­cadmium(II)], [Cd(pydc)(H2O)3]2·2H2pydc or [Cd2(C7H3NO4)2(H2O)6]·2C7H5NO4. Each Cd atom is seven-coordinate and has a distorted pentagonal-bipyramidal geometry. The two metal fragments are linked via the central four-membered Cd2O2 ring and there is no [Hpyda]+ moiety in the structure of the complex. The structure self-assembles into layers via hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802009066/wn6091sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802009066/wn6091Isup2.hkl
Contains datablock I

CCDC reference: 168385

Key indicators

  • Single-crystal X-ray study
  • T = 110 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.039
  • wR factor = 0.091
  • Data-to-parameter ratio = 17.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
ABSTM_02 Alert B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.285 0.862 Tmin' and Tmax expected: 0.516 0.866 RR' = 0.555 Please check that your absorption correction is appropriate.
Author response: ... The values quoted are those present in the outputfile of the SADABS absorption correction program. It is common that they differ appreciably from the SHELXL-97 theoretical values.

0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
0 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1998); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Cd2(C7H3O4)2(H2O)6]·2C7H5O4F(000) = 992
Mr = 997.34Dx = 2.070 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 9.0531 (16) ÅCell parameters from 967 reflections
b = 14.667 (3) Åθ = 3–30°
c = 12.186 (2) ŵ = 1.44 mm1
β = 98.485 (4)°T = 110 K
V = 1600.4 (5) Å3Plate, colorless
Z = 20.45 × 0.35 × 0.10 mm
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer
4676 independent reflections
Radiation source: fine-focus sealed tube3769 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
φ and ω scansθmax = 30.1°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1998)
h = 1212
Tmin = 0.285, Tmax = 0.862k = 2020
18834 measured reflectionsl = 1717
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)] = 0.039Hydrogen site location: geom and difmap
wR(F2) = 0.091H-atom parameters constrained
S = 1.21 w = 1/[σ2(Fo2) + (0.045P)2]
where P = (Fo2 + 2Fc2)/3
4676 reflections(Δ/σ)max = 0.002
261 parametersΔρmax = 2.85 e Å3
0 restraintsΔρmin = 0.96 e Å3
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*/Ueq
Cd10.08391 (2)0.915353 (13)0.902269 (16)0.01153 (7)
O10.0780 (2)0.93091 (13)1.03935 (16)0.0130 (4)
O20.2026 (2)0.85577 (13)1.15671 (17)0.0150 (4)
O30.1482 (2)0.79271 (13)0.78084 (17)0.0152 (4)
O40.1391 (2)0.64399 (13)0.74347 (17)0.0155 (4)
O1W0.0994 (2)0.96293 (13)0.76298 (17)0.0154 (4)
H1WA0.11381.01880.76080.015 (8)*
H1WB0.18750.94540.77510.050 (14)*
O2W0.2613 (2)0.97219 (13)0.80776 (17)0.0165 (4)
H2WA0.25590.95810.73970.017 (9)*
H2WB0.25411.02840.80840.058 (15)*
O3W0.2884 (2)0.90593 (13)1.05349 (17)0.0145 (4)
H3WA0.26490.88721.11470.039 (12)*
H3WB0.33790.86471.04590.056 (16)*
N10.0158 (2)0.77532 (15)0.94144 (19)0.0114 (4)
C20.0986 (3)0.77090 (17)1.0233 (2)0.0101 (5)
C30.1561 (3)0.68894 (18)1.0563 (2)0.0144 (5)
H3A0.21280.68701.11590.017*
C40.1282 (3)0.61024 (19)0.9995 (2)0.0160 (5)
H4A0.16680.55321.01910.019*
C50.0433 (3)0.61583 (19)0.9139 (2)0.0149 (5)
H5A0.02370.56280.87360.018*
C60.0123 (3)0.69967 (18)0.8879 (2)0.0115 (5)
C70.1291 (3)0.85964 (18)1.0789 (2)0.0118 (5)
C80.1070 (3)0.71155 (18)0.7960 (2)0.0121 (5)
O50.3025 (2)0.77816 (13)0.62702 (18)0.0191 (4)
H5O0.25550.78980.68400.034 (11)*
O60.2991 (3)0.92695 (14)0.59154 (18)0.0203 (5)
O70.5754 (2)0.57418 (14)0.44913 (18)0.0169 (4)
H7O0.61190.52590.44290.047 (14)*
O80.6201 (2)0.60253 (15)0.27671 (18)0.0212 (5)
N20.4551 (2)0.74047 (16)0.46387 (19)0.0128 (4)
C90.4165 (3)0.82764 (18)0.4773 (2)0.0130 (5)
C100.4463 (3)0.89774 (19)0.4070 (2)0.0153 (5)
H10A0.41740.95860.42010.018*
C110.5184 (3)0.8776 (2)0.3181 (2)0.0170 (6)
H11A0.53900.92410.26820.020*
C120.5602 (3)0.7880 (2)0.3030 (2)0.0164 (5)
H12A0.61020.77180.24260.020*
C130.5272 (3)0.72249 (18)0.3783 (2)0.0130 (5)
C140.3335 (3)0.84903 (19)0.5718 (2)0.0144 (5)
C150.5774 (3)0.6264 (2)0.3624 (2)0.0154 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01394 (11)0.00909 (10)0.01269 (11)0.00075 (7)0.00569 (7)0.00055 (7)
O10.0162 (9)0.0109 (9)0.0133 (9)0.0008 (7)0.0066 (7)0.0010 (7)
O20.0188 (10)0.0120 (9)0.0162 (10)0.0017 (7)0.0091 (8)0.0004 (7)
O30.0201 (10)0.0114 (9)0.0161 (10)0.0019 (7)0.0092 (8)0.0013 (7)
O40.0180 (10)0.0120 (9)0.0177 (10)0.0005 (7)0.0072 (8)0.0041 (7)
O1W0.0169 (10)0.0110 (9)0.0191 (10)0.0002 (7)0.0047 (8)0.0010 (7)
O2W0.0224 (10)0.0120 (9)0.0176 (10)0.0018 (8)0.0110 (8)0.0024 (7)
O3W0.0150 (9)0.0149 (10)0.0143 (10)0.0016 (8)0.0050 (8)0.0014 (7)
N10.0117 (10)0.0107 (10)0.0119 (10)0.0009 (8)0.0027 (8)0.0009 (8)
C20.0118 (11)0.0102 (11)0.0085 (11)0.0005 (9)0.0019 (9)0.0008 (9)
C30.0167 (13)0.0121 (12)0.0153 (13)0.0035 (10)0.0049 (10)0.0012 (10)
C40.0205 (14)0.0102 (12)0.0182 (14)0.0033 (10)0.0062 (11)0.0005 (10)
C50.0192 (13)0.0097 (12)0.0162 (13)0.0008 (10)0.0043 (10)0.0004 (10)
C60.0105 (11)0.0115 (12)0.0125 (12)0.0012 (9)0.0015 (9)0.0016 (9)
C70.0122 (12)0.0127 (12)0.0108 (12)0.0007 (9)0.0024 (9)0.0006 (9)
C80.0108 (11)0.0115 (12)0.0141 (12)0.0005 (9)0.0018 (9)0.0001 (9)
O50.0281 (11)0.0129 (9)0.0202 (10)0.0004 (8)0.0160 (9)0.0004 (8)
O60.0293 (12)0.0148 (10)0.0189 (11)0.0041 (8)0.0103 (9)0.0007 (8)
O70.0187 (10)0.0149 (10)0.0183 (10)0.0037 (8)0.0067 (8)0.0004 (8)
O80.0219 (11)0.0246 (11)0.0188 (11)0.0045 (9)0.0086 (9)0.0035 (9)
N20.0129 (10)0.0131 (11)0.0134 (11)0.0003 (9)0.0048 (8)0.0009 (8)
C90.0126 (12)0.0129 (12)0.0136 (12)0.0003 (9)0.0024 (10)0.0008 (9)
C100.0160 (13)0.0143 (13)0.0163 (13)0.0014 (10)0.0042 (10)0.0010 (10)
C110.0191 (14)0.0156 (13)0.0176 (14)0.0050 (11)0.0064 (11)0.0019 (11)
C120.0150 (13)0.0206 (14)0.0151 (13)0.0034 (11)0.0069 (10)0.0006 (11)
C130.0098 (11)0.0147 (12)0.0149 (12)0.0004 (9)0.0036 (10)0.0026 (10)
C140.0145 (12)0.0139 (13)0.0146 (13)0.0002 (10)0.0013 (10)0.0005 (10)
C150.0106 (12)0.0180 (14)0.0182 (13)0.0009 (10)0.0041 (10)0.0029 (11)
Geometric parameters (Å, º) top
Cd1—O2W2.269 (2)C3—H3A0.9500
Cd1—O1W2.300 (2)C4—C51.387 (4)
Cd1—N12.321 (2)C4—H4A0.9500
Cd1—O1i2.3674 (19)C5—C61.383 (4)
Cd1—O12.3902 (19)C5—H5A0.9500
Cd1—O3W2.416 (2)C6—C81.518 (4)
Cd1—O32.4532 (19)O5—C141.291 (3)
O1—C71.267 (3)O5—H5O0.8834
O1—Cd1i2.3674 (19)O6—C141.218 (3)
O2—C71.237 (3)O7—C151.308 (4)
O3—C81.269 (3)O7—H7O0.7898
O4—C81.237 (3)O8—C151.217 (4)
O1W—H1WA0.8299N2—C131.336 (3)
O1W—H1WB0.8715N2—C91.342 (3)
O2W—H2WA0.8490C9—C101.390 (4)
O2W—H2WB0.8270C9—C141.498 (4)
O3W—H3WA0.8506C10—C111.377 (4)
O3W—H3WB0.7669C10—H10A0.9500
N1—C61.330 (3)C11—C121.387 (4)
N1—C21.335 (3)C11—H11A0.9500
C2—C31.393 (4)C12—C131.391 (4)
C2—C71.512 (4)C12—H12A0.9500
C3—C41.388 (4)C13—C151.502 (4)
O2W—Cd1—O1W90.09 (7)C4—C3—H3A121.0
O2W—Cd1—N1139.06 (7)C2—C3—H3A121.0
O1W—Cd1—N199.22 (8)C5—C4—C3119.2 (3)
O2W—Cd1—O1i81.47 (7)C5—C4—H4A120.4
O1W—Cd1—O1i83.51 (7)C3—C4—H4A120.4
N1—Cd1—O1i138.96 (7)C6—C5—C4119.0 (3)
O2W—Cd1—O1150.78 (7)C6—C5—H5A120.5
O1W—Cd1—O192.11 (7)C4—C5—H5A120.5
N1—Cd1—O169.12 (7)N1—C6—C5121.8 (2)
O1i—Cd1—O169.85 (7)N1—C6—C8115.8 (2)
O2W—Cd1—O3W83.58 (7)C5—C6—C8122.4 (2)
O1W—Cd1—O3W165.59 (7)O2—C7—O1126.7 (3)
N1—Cd1—O3W94.01 (7)O2—C7—C2117.3 (2)
O1i—Cd1—O3W82.77 (7)O1—C7—C2116.0 (2)
O1—Cd1—O3W87.26 (7)O4—C8—O3125.4 (3)
O2W—Cd1—O373.41 (7)O4—C8—C6119.4 (2)
O1W—Cd1—O389.24 (7)O3—C8—C6115.2 (2)
N1—Cd1—O367.00 (7)C14—O5—H5O114.9
O1i—Cd1—O3153.84 (7)C15—O7—H7O113.1
O1—Cd1—O3135.73 (6)C13—N2—C9116.7 (2)
O3W—Cd1—O3101.24 (7)N2—C9—C10123.5 (3)
C7—O1—Cd1i130.21 (17)N2—C9—C14117.6 (2)
C7—O1—Cd1118.91 (17)C10—C9—C14118.9 (2)
Cd1i—O1—Cd1110.15 (7)C11—C10—C9119.0 (3)
C8—O3—Cd1119.93 (16)C11—C10—H10A120.5
Cd1—O1W—H1WA114.6C9—C10—H10A120.5
Cd1—O1W—H1WB111.4C10—C11—C12118.6 (3)
H1WA—O1W—H1WB98.8C10—C11—H11A120.7
Cd1—O2W—H2WA117.6C12—C11—H11A120.7
Cd1—O2W—H2WB107.4C11—C12—C13118.5 (3)
H2WA—O2W—H2WB105.0C11—C12—H12A120.7
Cd1—O3W—H3WA115.2C13—C12—H12A120.7
Cd1—O3W—H3WB110.4N2—C13—C12123.8 (3)
H3WA—O3W—H3WB94.4N2—C13—C15118.6 (2)
C6—N1—C2119.6 (2)C12—C13—C15117.7 (2)
C6—N1—Cd1121.94 (18)O6—C14—O5124.8 (3)
C2—N1—Cd1118.35 (17)O6—C14—C9121.4 (3)
N1—C2—C3122.2 (2)O5—C14—C9113.8 (2)
N1—C2—C7117.0 (2)O8—C15—O7124.7 (3)
C3—C2—C7120.8 (2)O8—C15—C13121.4 (3)
C4—C3—C2118.1 (2)O7—C15—C13113.9 (2)
O2W—Cd1—O1—C7159.51 (19)C2—N1—C6—C50.6 (4)
O1W—Cd1—O1—C7106.5 (2)Cd1—N1—C6—C5177.9 (2)
N1—Cd1—O1—C77.47 (19)C2—N1—C6—C8179.8 (2)
O1i—Cd1—O1—C7171.2 (2)Cd1—N1—C6—C82.9 (3)
O3W—Cd1—O1—C787.9 (2)C4—C5—C6—N11.3 (4)
O3—Cd1—O1—C715.4 (2)C4—C5—C6—C8179.6 (3)
O2W—Cd1—O1—Cd1i11.67 (19)Cd1i—O1—C7—O23.9 (4)
O1W—Cd1—O1—Cd1i82.29 (9)Cd1—O1—C7—O2173.1 (2)
N1—Cd1—O1—Cd1i178.65 (11)Cd1i—O1—C7—C2177.18 (16)
O1i—Cd1—O1—Cd1i0.0Cd1—O1—C7—C28.1 (3)
O3W—Cd1—O1—Cd1i83.30 (8)N1—C2—C7—O2178.2 (2)
O3—Cd1—O1—Cd1i173.38 (7)C3—C2—C7—O22.3 (4)
O2W—Cd1—O3—C8166.1 (2)N1—C2—C7—O12.8 (4)
O1W—Cd1—O3—C8103.6 (2)C3—C2—C7—O1176.7 (3)
N1—Cd1—O3—C83.22 (19)Cd1—O3—C8—O4176.4 (2)
O1i—Cd1—O3—C8177.10 (18)Cd1—O3—C8—C62.9 (3)
O1—Cd1—O3—C811.3 (2)N1—C6—C8—O4179.2 (2)
O3W—Cd1—O3—C886.4 (2)C5—C6—C8—O41.6 (4)
O2W—Cd1—N1—C612.6 (3)N1—C6—C8—O30.2 (4)
O1W—Cd1—N1—C688.3 (2)C5—C6—C8—O3179.0 (3)
O1i—Cd1—N1—C6179.01 (18)C13—N2—C9—C100.7 (4)
O1—Cd1—N1—C6177.1 (2)C13—N2—C9—C14179.1 (2)
O3W—Cd1—N1—C697.4 (2)N2—C9—C10—C110.4 (4)
O3—Cd1—N1—C63.1 (2)C14—C9—C10—C11177.9 (3)
O2W—Cd1—N1—C2164.70 (17)C9—C10—C11—C120.8 (4)
O1W—Cd1—N1—C294.4 (2)C10—C11—C12—C130.1 (4)
O1i—Cd1—N1—C23.7 (3)C9—N2—C13—C121.5 (4)
O1—Cd1—N1—C25.64 (19)C9—N2—C13—C15177.8 (2)
O3W—Cd1—N1—C279.9 (2)C11—C12—C13—N21.1 (4)
O3—Cd1—N1—C2179.6 (2)C11—C12—C13—C15178.2 (3)
C6—N1—C2—C30.8 (4)N2—C9—C14—O6177.5 (3)
Cd1—N1—C2—C3176.5 (2)C10—C9—C14—O64.1 (4)
C6—N1—C2—C7178.7 (2)N2—C9—C14—O53.1 (4)
Cd1—N1—C2—C74.0 (3)C10—C9—C14—O5175.3 (3)
N1—C2—C3—C41.5 (4)N2—C13—C15—O8167.2 (3)
C7—C2—C3—C4177.9 (3)C12—C13—C15—O813.4 (4)
C2—C3—C4—C50.8 (4)N2—C13—C15—O715.0 (4)
C3—C4—C5—C60.5 (4)C12—C13—C15—O7164.3 (3)
Symmetry code: (i) x, y+2, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O4ii0.831.852.679 (3)178
O1W—H1WB···O8iii0.871.882.743 (3)170
O2W—H2WA···O60.851.962.787 (3)165
O2W—H2WB···O2i0.831.832.628 (3)162
O3W—H3WA···O4iv0.852.122.940 (3)162
O3W—H3WB···N2iv0.772.192.927 (3)160
O5—H5O···O30.881.642.507 (3)168
O7—H7O···O3Wv0.791.972.761 (3)173
Symmetry codes: (i) x, y+2, z+2; (ii) x, y+1/2, z+3/2; (iii) x1, y+3/2, z+1/2; (iv) x, y+3/2, z+1/2; (v) x+1, y1/2, z+3/2.
 

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