catena-Poly[[[bis­(3-amino­pyridine-κN)copper(II)]-di-μ-chloro] hydrate]

The title compound, {[CuCl₂(C₅H₆N₂)₂]·H₂O}_n, comprises centrosymmetric mononuclear CuCl₂L₂ (L = 3-amino­pyridine) units, with a trans geometry of the ligands, connected into infinite linear chains through bridging chloride ligands. The chains are oriented along the c axis and form channels, which are occupied by disordered water mol­ecules.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.007 Å
• H-atom completeness 86%
• Disorder in solvent or counterion
• R factor = 0.069
• wR factor = 0.222
• Data-to-parameter ratio = 23.7

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of .     179.00 A   3  

Alert level C
CELLV02_ALERT_1_C  The supplied cell volume s.u. differs from that
            calculated from the cell parameter s.u.'s by > 2
            Calculated cell volume su =      12.83
            Cell volume su given      =      15.00
CHEMW01_ALERT_1_C  The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
DIFMX01_ALERT_2_C  The maximum difference density is > 0.1*ZMAX*0.75
            _refine_diff_density_max given =      2.210
            Test value =      2.175
DIFMX02_ALERT_1_C  The minimum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............       2.21 e/A   3
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.11
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      50.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          7
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          1

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C10 H14 Cl2 Cu1 N4 O1
            Atom count from the _atom_site data:  C10 H12 Cl2 Cu1 N4 O1
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    9
           From the CIF: _chemical_formula_sum  C10 H14 Cl2 Cu1 N4 O
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         90.00     90.00    0.00
           H        126.00    108.00   18.00
           Cl        18.00     18.00    0.00
           Cu         9.00      9.00    0.00
           N         36.00     36.00    0.00
           O          9.00      9.00    0.00
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
           From the CIF: _diffrn_reflns_theta_max           27.50
           From the CIF: _reflns_number_total               1991
           From the CIF: _diffrn_reflns_limit_ max hkl   43.   37.    5.
           From the CIF: _diffrn_reflns_limit_ min hkl  -44.  -36.   -5.
           TEST1: Expected hkl limits for theta max
           Calculated maximum hkl   44.   44.    5.
           Calculated minimum hkl  -44.  -44.   -5.

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  12 ALERT level C = Check and explain
   4 ALERT level G = General alerts; check

   9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 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

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Computing details

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

catena-Poly[[[bis(3-aminopyridine-κN)copper(II)]-di-µ-chloro] hydrate]

Crystal data

[CuCl2(C5H6N2)2]·H2O	Dx = 1.294 Mg m^−3
Mr = 338.68	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3	Cell parameters from 2142 reflections
Hall symbol: -R 3	θ = 1.0–28.3°
a = 33.9602 (7) Å	µ = 1.56 mm^−1
c = 3.9152 (1) Å	T = 150 K
V = 3910.43 (15) Å^3	Block, yellow–green
Z = 9	0.15 × 0.10 × 0.10 mm
F(000) = 1539

Data collection

Nonius KappaCCD diffractometer	1652 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.024
Graphite monochromator	θmax = 27.5°, θmin = 1.2°
ω scans at κ = 55 °	h = −44→43
3701 measured reflections	k = −36→37
1991 independent reflections	l = −5→5

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.069	H-atom parameters constrained
wR(F^2) = 0.222	w = 1/[σ^2(Fo^2) + (0.1406P)^2 + 3.9571P] where P = (Fo^2 + 2Fc^2)/3
S = 1.25	(Δ/σ)max = 0.002
1991 reflections	Δρmax = 2.21 e Å^−3
84 parameters	Δρmin = −1.25 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0092 (12)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Cu1	0.5000	0.0000	0.5000	0.0316 (4)
Cl1	0.56042 (3)	0.04681 (3)	0.8380 (3)	0.0313 (4)
N1	0.48025 (12)	0.04665 (12)	0.4888 (9)	0.0288 (8)
N2	0.38064 (13)	0.05380 (14)	0.7476 (11)	0.0370 (9)
H2A	0.3704	0.0724	0.7444	0.044*
H2B	0.3644	0.0271	0.8334	0.044*
C2	0.43931 (14)	0.03596 (15)	0.6133 (11)	0.0283 (9)
H2	0.4209	0.0070	0.7022	0.034*
C3	0.42328 (14)	0.06690 (14)	0.6142 (10)	0.0262 (9)
C4	0.45063 (17)	0.10937 (15)	0.4735 (11)	0.0331 (10)
H4	0.4408	0.1305	0.4639	0.040*
C5	0.49323 (16)	0.12013 (17)	0.3460 (13)	0.0359 (10)
H5	0.5122	0.1486	0.2516	0.043*
C6	0.50721 (16)	0.08815 (16)	0.3605 (12)	0.0343 (10)
H6	0.5359	0.0957	0.2793	0.041*
OW1	0.6144 (6)	0.1832 (6)	−0.192 (5)	0.128 (5)*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.0285 (5)	0.0296 (5)	0.0466 (6)	0.0221 (4)	−0.0167 (3)	−0.0161 (3)
Cl1	0.0267 (6)	0.0316 (6)	0.0394 (7)	0.0175 (5)	−0.0122 (4)	−0.0122 (4)
N1	0.0276 (18)	0.0279 (18)	0.0354 (18)	0.0173 (16)	−0.0106 (14)	−0.0095 (15)
N2	0.030 (2)	0.037 (2)	0.052 (2)	0.0225 (18)	−0.0018 (17)	0.0020 (17)
C2	0.028 (2)	0.027 (2)	0.035 (2)	0.0179 (17)	−0.0071 (16)	−0.0046 (16)
C3	0.027 (2)	0.028 (2)	0.029 (2)	0.0180 (17)	−0.0063 (16)	−0.0057 (15)
C4	0.042 (3)	0.032 (2)	0.039 (2)	0.029 (2)	0.0021 (19)	0.0000 (18)
C5	0.036 (2)	0.030 (2)	0.046 (3)	0.019 (2)	0.0095 (19)	0.0060 (19)
C6	0.033 (2)	0.033 (2)	0.043 (3)	0.021 (2)	0.0029 (19)	−0.0021 (19)

Geometric parameters (Å, º)

Cu1—N1^i	2.006 (3)	N2—H2B	0.8600
Cu1—N1	2.006 (3)	C3—C4	1.381 (6)
Cu1—Cl1^i	2.2862 (9)	C4—C5	1.396 (6)
Cu1—Cl1	2.2862 (9)	C4—H4	0.9300
Cu1—Cl1^ii	3.1926 (12)	C5—C6	1.387 (6)
Cu1—Cl1^iii	3.1926 (12)	C5—H5	0.9300
Cu1—Cu1^iii	3.9152 (1)	C6—H6	0.9300
N1—C2	1.341 (5)	N1—C6	1.337 (6)
N2—H2A	0.8600	N2—C3	1.387 (6)
N1^i—Cu1—N1	180.00 (13)	C6—N1—C2	119.6 (4)
N1^i—Cu1—Cl1^i	90.10 (10)	C6—N1—Cu1	121.2 (3)
N1—Cu1—Cl1^i	89.90 (10)	C2—N1—Cu1	119.3 (3)
N1^i—Cu1—Cl1	89.90 (10)	C3—N2—H2A	120.0
N1—Cu1—Cl1	90.10 (10)	C3—N2—H2B	120.0
Cl1^i—Cu1—Cl1	180.00 (9)	H2A—N2—H2B	120.0
N1^i—Cu1—Cl1^ii	88.53 (11)	N1—C2—C3	122.4 (4)
N1—Cu1—Cl1^ii	91.47 (11)	N1—C2—H2	118.8
Cl1^i—Cu1—Cl1^ii	89.64 (3)	C3—C2—H2	118.8
Cl1—Cu1—Cl1^ii	90.36 (3)	C4—C3—N2	122.3 (4)
N1^i—Cu1—Cl1^iii	91.47 (11)	C4—C3—C2	118.1 (4)
N1—Cu1—Cl1^iii	88.53 (11)	N2—C3—C2	119.6 (4)
Cl1^i—Cu1—Cl1^iii	90.36 (3)	C3—C4—C5	118.9 (4)
Cl1—Cu1—Cl1^iii	89.64 (3)	C3—C4—H4	120.5
Cl1^ii—Cu1—Cl1^iii	180.00 (7)	C5—C4—H4	120.5
N1^i—Cu1—Cu1^iii	91.25 (10)	C6—C5—C4	119.8 (4)
N1—Cu1—Cu1^iii	88.75 (10)	C6—C5—H5	120.1
Cl1^i—Cu1—Cu1^iii	54.63 (3)	C4—C5—H5	120.1
Cl1—Cu1—Cu1^iii	125.37 (3)	N1—C6—C5	121.2 (4)
Cl1^ii—Cu1—Cu1^iii	144.273 (17)	N1—C6—H6	119.4
Cl1^iii—Cu1—Cu1^iii	35.727 (17)	C5—C6—H6	119.4

Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y, −z+2; (iii) x, y, z−1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···Cl1^iv	0.86	2.61	3.394 (4)	152

Symmetry code: (iv) y+1/3, −x+y+2/3, −z+5/3.