catena-Poly­[[di­aqua­[3-(2-pyridyl)-1H-pyrazole-κN²]­cadmium(II)]-μ-squarato-κ²O:O′]

The squarate dianion in the crystal structure of the title compound, [Cd(C₄O₄)(C₈H₇N₃)(H₂O)₂]_n, links the heterocycle-chelated water-coordinated Cd atoms into a zigzag chain. The O atoms of the squarate dianions are aligned trans to each other in the octahedron surrounding the Cd atom. There are two independent square dianions and both lie on inversion centers.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.022
• wR factor = 0.073
• Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT301_ALERT_3_C Main Residue  Disorder .........................       4.00 Perc.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          7

   0 ALERT level A = In general: serious problem
   0 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
   0 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

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Computing details

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: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

catena-Poly[[diaqua[3-(2-pyridyl)-1H-pyrazole-κN²]cadmium(II)]- µ-squarato-κ²O:O']

Crystal data

[Cd(C4O4)(C8H7N3)(H2O)2]	Z = 2
Mr = 405.64	F(000) = 400
Triclinic, P1	Dx = 2.028 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.066 (1) Å	Cell parameters from 6304 reflections
b = 8.643 (2) Å	θ = 3.2–27.5°
c = 13.272 (3) Å	µ = 1.68 mm^−1
α = 104.87 (3)°	T = 295 K
β = 97.27 (3)°	Prism, yellow
γ = 93.29 (3)°	0.38 × 0.25 × 0.18 mm
V = 664.2 (2) Å^3

Data collection

Rigaki R-AXIS RAPID IP diffractometer	2938 independent reflections
Radiation source: fine-focus sealed tube	2774 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.013
ω scans	θmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −7→6
Tmin = 0.504, Tmax = 0.737	k = −11→11
6388 measured reflections	l = −17→17

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.073	H-atom parameters constrained
S = 1.34	w = 1/[σ^2(Fo^2) + (0.0287P)^2 + 0.7719P] where P = (Fo^2 + 2Fc^2)/3
2938 reflections	(Δ/σ)max = 0.001
212 parameters	Δρmax = 0.45 e Å^−3
0 restraints	Δρmin = −0.41 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Cd1	0.62460 (3)	0.71725 (2)	0.80709 (2)	0.02507 (8)
O1w	0.420 (2)	0.8281 (9)	0.9450 (7)	0.033 (2)	0.59 (3)
O1w'	0.525 (4)	0.839 (1)	0.970 (1)	0.039 (3)	0.41 (3)
O2w	0.4143 (4)	0.4914 (3)	0.7966 (2)	0.0327 (5)
O1	0.9381 (4)	0.6824 (3)	0.9044 (2)	0.0411 (6)
O2	0.6527 (4)	0.3684 (3)	0.9353 (2)	0.0333 (5)
O3	0.7597 (3)	0.5917 (3)	0.6483 (2)	0.0287 (4)
O4	0.6985 (4)	0.6391 (3)	0.4110 (2)	0.0374 (6)
N1	0.7774 (4)	0.9589 (3)	0.7895 (2)	0.0249 (5)
N2	0.3586 (4)	0.8138 (3)	0.7008 (2)	0.0261 (5)
N3	0.1620 (4)	0.7612 (3)	0.6383 (2)	0.0305 (6)
C1	0.9790 (5)	1.0326 (4)	0.8361 (2)	0.0330 (7)
C2	1.0708 (5)	1.1665 (4)	0.8135 (3)	0.0359 (7)
C3	0.9493 (6)	1.2308 (4)	0.7418 (3)	0.0356 (7)
C4	0.7405 (5)	1.1580 (4)	0.6940 (2)	0.0289 (6)
C5	0.6599 (5)	1.0208 (3)	0.7188 (2)	0.0221 (5)
C6	0.4417 (5)	0.9355 (3)	0.6681 (2)	0.0224 (5)
C7	0.2960 (5)	0.9607 (4)	0.5848 (3)	0.0329 (7)
C8	0.1198 (5)	0.8465 (4)	0.5687 (3)	0.0355 (7)
C9	0.9687 (5)	0.5809 (4)	0.9562 (2)	0.0274 (6)
C10	0.8420 (5)	0.4410 (4)	0.9708 (2)	0.0264 (6)
C11	0.6177 (5)	0.5418 (3)	0.5664 (2)	0.0229 (5)
C12	0.5917 (5)	0.5632 (3)	0.4599 (2)	0.0245 (6)
H1w1	0.2812	0.8127	0.9216	0.040*	0.59 (3)
H1w2	0.4473	0.7830	0.9945	0.040*	0.59 (3)
H1w3	0.4228	0.7789	0.9830	0.047*	0.41 (3)
H1w4	0.6382	0.8530	1.0169	0.047*	0.41 (3)
H2w1	0.3836	0.4372	0.7326	0.039*
H2w2	0.4852	0.4363	0.8322	0.039*
H3n	0.0754	0.6831	0.6426	0.037*
H1	1.0601	0.9911	0.8858	0.040*
H2	1.2125	1.2130	0.8461	0.043*
H3	1.0073	1.3222	0.7259	0.043*
H4	0.6551	1.2000	0.6459	0.035*
H7	0.3145	1.0381	0.5484	0.040*
H8	−0.0064	0.8313	0.5183	0.043*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.0263 (1)	0.0251 (1)	0.0258 (1)	−0.0007 (1)	0.0001 (1)	0.0128 (1)
O1w	0.038 (5)	0.034 (3)	0.032 (3)	0.008 (3)	0.008 (3)	0.014 (2)
O1w'	0.042 (8)	0.042 (4)	0.033 (4)	−0.011 (4)	0.011 (4)	0.011 (3)
O2w	0.033 (1)	0.033 (1)	0.033 (1)	−0.006 (1)	−0.002 (1)	0.015 (1)
O1	0.0457 (1)	0.036 (1)	0.044 (1)	−0.005 (1)	−0.016 (1)	0.026 (1)
O2	0.0324 (1)	0.038 (1)	0.030 (1)	−0.004 (1)	−0.003 (1)	0.016 (1)
O3	0.0236 (1)	0.038 (1)	0.023 (1)	−0.005 (1)	−0.001 (1)	0.007 (1)
O4	0.0353 (1)	0.047 (1)	0.029 (1)	−0.019 (1)	−0.002 (1)	0.017 (1)
N1	0.0221 (1)	0.025 (1)	0.028 (1)	−0.001 (1)	−0.001 (1)	0.009 (1)
N2	0.0207 (1)	0.029 (1)	0.030 (1)	−0.002 (1)	−0.002 (1)	0.011 (1)
N3	0.0205 (1)	0.032 (1)	0.037 (1)	−0.006 (1)	0.000 (1)	0.007 (1)
C1	0.0269 (2)	0.039 (2)	0.031 (2)	0.000 (1)	−0.005 (1)	0.008 (1)
C2	0.0242 (2)	0.038 (2)	0.039 (2)	−0.010 (1)	0.001 (1)	0.002 (1)
C3	0.0341 (2)	0.032 (2)	0.039 (2)	−0.010 (1)	0.009 (1)	0.007 (1)
C4	0.0329 (2)	0.025 (1)	0.032 (2)	0.001 (1)	0.005 (1)	0.012 (1)
C5	0.0216 (1)	0.022 (1)	0.024 (1)	0.002 (1)	0.003 (1)	0.007 (1)
C6	0.0194 (1)	0.023 (1)	0.026 (1)	0.001 (1)	0.003 (1)	0.008 (1)
C7	0.0268 (2)	0.039 (2)	0.036 (2)	−0.002 (1)	−0.004 (1)	0.018 (1)
C8	0.0242 (2)	0.047 (2)	0.033 (2)	0.001 (1)	−0.006 (1)	0.011 (1)
C9	0.034 (2)	0.024 (1)	0.023 (1)	0.003 (1)	−0.003 (1)	0.009 (1)
C10	0.034 (2)	0.025 (1)	0.021 (1)	0.002 (1)	0.000 (1)	0.009 (1)
C11	0.0208 (1)	0.024 (1)	0.023 (1)	−0.002 (1)	0.002 (1)	0.006 (1)
C12	0.023 (1)	0.025 (1)	0.024 (1)	−0.003 (1)	0.001 (1)	0.006 (1)

Geometric parameters (Å, º)

Cd1—O1	2.240 (2)	C6—C7	1.396 (4)
Cd1—O3	2.378 (2)	C7—C8	1.369 (5)
Cd1—O1w	2.371 (6)	C9—C10^i	1.459 (4)
Cd1—O1w'	2.314 (8)	C9—C10	1.463 (4)
Cd1—O2w	2.233 (2)	C10—C9^i	1.459 (4)
Cd1—N1	2.315 (3)	C11—C12	1.462 (4)
Cd1—N2	2.339 (3)	C11—C12^ii	1.467 (4)
O1—C9	1.255 (4)	C12—C11^ii	1.467 (4)
O2—C10	1.250 (4)	O1w—H1w1	0.851
O3—C11	1.261 (3)	O1w—H1w2	0.85
O4—C12	1.244 (4)	O1w'—H1w3	0.85
N1—C5	1.343 (4)	O1w'—H1w4	0.85
N1—C1	1.342 (4)	O2w—H2w1	0.85
N2—C6	1.334 (4)	O2w—H2w2	0.85
N2—N3	1.346 (3)	N3—H3n	0.85
N3—C8	1.332 (4)	C1—H1	0.93
C1—C2	1.373 (5)	C2—H2	0.93
C2—C3	1.378 (5)	C3—H3	0.93
C3—C4	1.380 (5)	C4—H4	0.93
C4—C5	1.388 (4)	C7—H7	0.93
C5—C6	1.469 (4)	C8—H8	0.93
O1—Cd1—O3	91.4 (1)	C7—C6—C5	129.4 (3)
O1—Cd1—O1w	98.9 (3)	C8—C7—C6	104.8 (3)
O1—Cd1—O1w'	83.4 (6)	N3—C8—C7	107.6 (3)
O1—Cd1—O2w	100.9 (1)	O3—C11—C12	135.6 (3)
O1—Cd1—N1	92.1 (1)	O1—C9—C10^i	132.4 (3)
O1—Cd1—N2	164.2 (1)	O1—C9—C10	137.1 (3)
O3—Cd1—O1w	168.8 (4)	C10^i—C9—C10	90.5 (2)
O3—Cd1—O1w'	174.8 (6)	O2—C10—C9^i	134.8 (3)
O3—Cd1—O2w	90.5 (1)	O2—C10—C9	135.8 (3)
O3—Cd1—N1	87.1 (1)	C9^i—C10—C9	89.5 (2)
O3—Cd1—N2	86.1 (1)	O3—C11—C12^ii	134.0 (3)
O1w—Cd1—O2w	83.3 (3)	C12—C11—C12^ii	90.4 (2)
O1w—Cd1—N1	96.8 (2)	O4—C12—C11	136.0 (3)
O1w—Cd1—N2	85.1 (3)	O4—C12—C11^ii	134.5 (3)
O1w'—Cd1—O2w	91.3 (3)	C11—C12—C11^ii	89.6 (2)
O1w'—Cd1—N1	92.3 (2)	Cd1—O1w—H1w1	109.5
O1w'—Cd1—N2	98.6 (6)	Cd1—O1w—H1w2	109.5
O2w—Cd1—N1	166.8 (1)	Cd1—O1w'—H1w3	109.5
O2w—Cd1—N2	94.7 (1)	Cd1—O1w'—H1w4	109.5
N1—Cd1—N2	72.3 (1)	H1w3—O1w'—H1w4	109.5
C9—O1—Cd1	128.6 (2)	Cd1—O2w—H2w1	109.5
C11—O3—Cd1	117.1 (2)	Cd1—O2w—H2w2	109.5
C5—N1—C1	118.2 (3)	H2w1—O2w—H2w2	109.5
C5—N1—Cd1	115.9 (2)	C8—N3—H3n	124.1
C1—N1—Cd1	125.6 (2)	N2—N3—H3n	124.1
C6—N2—N3	105.3 (2)	N1—C1—H1	118.6
C6—N2—Cd1	113.1 (2)	C2—C1—H1	118.6
N3—N2—Cd1	138.6 (2)	C1—C2—H2	120.6
C8—N3—N2	111.7 (3)	C3—C2—H2	120.6
N1—C1—C2	122.8 (3)	C4—C3—H3	120.4
C1—C2—C3	118.9 (3)	C2—C3—H3	120.4
C4—C3—C2	119.1 (3)	C3—C4—H4	120.5
C3—C4—C5	118.9 (3)	C5—C4—H4	120.5
N1—C5—C4	122.0 (3)	C8—C7—H7	127.6
N1—C5—C6	116.7 (2)	C6—C7—H7	127.6
C4—C5—C6	121.3 (3)	N3—C8—H8	126.2
N2—C6—C7	110.6 (3)	C7—C8—H8	126.2
N2—C6—C5	120.0 (2)
O2w—Cd1—O1—C9	−12.9 (3)	Cd1—N2—N3—C8	−158.2 (3)
O1w'—Cd1—O1—C9	77.1 (4)	C5—N1—C1—C2	−0.9 (5)
N1—Cd1—O1—C9	169.2 (3)	Cd1—N1—C1—C2	172.6 (2)
N2—Cd1—O1—C9	175.7 (3)	N1—C1—C2—C3	1.6 (5)
O1w—Cd1—O1—C9	72.0 (4)	C1—C2—C3—C4	−0.7 (5)
O3—Cd1—O1—C9	−103.6 (3)	C2—C3—C4—C5	−0.6 (5)
O2w—Cd1—O3—C11	60.8 (2)	C1—N1—C5—C4	−0.5 (4)
O1—Cd1—O3—C11	161.7 (2)	Cd1—N1—C5—C4	−174.6 (2)
N1—Cd1—O3—C11	−106.3 (2)	C1—N1—C5—C6	179.0 (3)
N2—Cd1—O3—C11	−33.9 (2)	Cd1—N1—C5—C6	4.9 (3)
O1w—Cd1—O3—C11	4.5 (8)	C3—C4—C5—N1	1.3 (5)
O2w—Cd1—N1—C5	−1.6 (5)	C3—C4—C5—C6	−178.2 (3)
O1—Cd1—N1—C5	169.2 (2)	N3—N2—C6—C7	0.4 (3)
O1w'—Cd1—N1—C5	−107.3 (7)	Cd1—N2—C6—C7	164.6 (2)
N2—Cd1—N1—C5	−9.0 (2)	N3—N2—C6—C5	−179.1 (3)
O1w—Cd1—N1—C5	−91.6 (4)	Cd1—N2—C6—C5	−14.9 (3)
O3—Cd1—N1—C5	77.8 (2)	N1—C5—C6—N2	7.2 (4)
O2w—Cd1—N1—C1	−175.2 (3)	C4—C5—C6—N2	−173.3 (3)
O1—Cd1—N1—C1	−4.5 (3)	N1—C5—C6—C7	−172.3 (3)
O1w'—Cd1—N1—C1	79.0 (7)	C4—C5—C6—C7	7.2 (5)
N2—Cd1—N1—C1	177.4 (3)	N2—C6—C7—C8	−0.3 (4)
O1w—Cd1—N1—C1	94.8 (4)	C5—C6—C7—C8	179.2 (3)
O3—Cd1—N1—C1	−95.8 (3)	N2—N3—C8—C7	0.3 (4)
O2w—Cd1—N2—C6	−166.0 (2)	C6—C7—C8—N3	0.0 (4)
O1—Cd1—N2—C6	5.6 (5)	Cd1—O3—C11—C12	127.2 (3)
O1w'—Cd1—N2—C6	102.0 (4)	Cd1—O3—C11—C12^ii	−52.8 (4)
N1—Cd1—N2—C6	12.3 (2)	O1—C9—C10—O2	0.9 (7)
O1w—Cd1—N2—C6	111.1 (4)	C10^i—C9—C10—O2	−179.3 (5)
O3—Cd1—N2—C6	−75.8 (2)	O1—C9—C10—C9^i	−179.9 (5)
O2w—Cd1—N2—N3	−9.4 (3)	C10^i—C9—C10—C9^i	0.0
O1—Cd1—N2—N3	162.2 (3)	Cd1—O1—C9—C10^i	−173.1 (3)
O1w'—Cd1—N2—N3	−101.4 (4)	Cd1—O1—C9—C10	6.7 (6)
N1—Cd1—N2—N3	168.9 (3)	O3—C11—C12—O4	−0.7 (7)
O1w—Cd1—N2—N3	−92.3 (4)	C12^ii—C11—C12—O4	179.3 (5)
O3—Cd1—N2—N3	80.7 (3)	O3—C11—C12—C11^ii	180.0 (4)
C6—N2—N3—C8	−0.5 (4)	C12^ii—C11—C12—C11^ii	0.0

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1w1···O1^iii	0.85	2.26	3.04 (2)	152
O1w—H1w2···O2^iv	0.85	1.90	2.661 (6)	148
O1w′—H1w3···O2^iv	0.85	1.94	2.692 (9)	146
O2w—H2w2···O2	0.85	1.84	2.668 (3)	165
O2w—H2w1···O4^ii	0.85	1.84	2.679 (3)	168
N3—H3n···O3^iii	0.85	2.05	2.809 (3)	149

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