catena-Poly[[(2,2′-bipyridine-κ²N,N′)-praseodym­ium(III)]-μ-dichloro­acetate-1κ²O:O′:2κO-di-μ-dichloro­acetato-κ⁴O:O′]

The title compound, [Pr(C₂HCl₂O₂)₃(C₁₀H₈N₂)]_n, was synthesized by reaction of praseodymium(III) dichloro­acetate with 2,2′-bipyridine in a water–ethanol (1:1) solution. There is a centre of symmetry at the mid-point of the Pr...Pr vector. The structure consists of chains running along the a axis. The Pr³⁺ ion is coordinated by seven O and two N atoms, giving a distorted monocapped square anti­prism.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.033
• wR factor = 0.079
• Data-to-parameter ratio = 18.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.94
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for        C12

Alert level C
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C22
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C32
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.11 Ratio

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   3 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
   1 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

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Computing details

Data collection: IPDS Software (Stoe & Cie, 1998); cell refinement: IPDS Software; data reduction: IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.

catena-Poly[[(2,2'-bipyridine-κ²N,N')-praseodymium(III)]- µ-dichloroacetate-1κ²O:O':2κO-di-µ-dichloroacetato-κ⁴O:O']

Crystal data

[Pr(C2HCl2O2)3(C10H8N2)]	Z = 2
Mr = 680.88	F(000) = 660
Triclinic, P1	Dx = 1.947 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.8787 (9) Å	Cell parameters from 7998 reflections
b = 12.2644 (12) Å	θ = 2.6–28.1°
c = 12.3537 (13) Å	µ = 2.82 mm^−1
α = 109.280 (12)°	T = 293 K
β = 104.493 (12)°	Needle, green
γ = 102.541 (12)°	0.23 × 0.14 × 0.13 mm
V = 1161.4 (3) Å^3

Data collection

STOE IPDS area-detector diffractometer	5261 independent reflections
Radiation source: fine-focus sealed tube	4404 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.048
φ scans	θmax = 28.3°, θmin = 2.5°
Absorption correction: multi-scan (Blessing, 1995)	h = −11→11
Tmin = 0.653, Tmax = 0.693	k = −16→16
20573 measured reflections	l = −16→16

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)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.079	H-atom parameters constrained
S = 0.97	w = 1/[σ^2(Fo^2) + (0.0514P)^2] where P = (Fo^2 + 2Fc^2)/3
5261 reflections	(Δ/σ)max = 0.001
280 parameters	Δρmax = 0.87 e Å^−3
0 restraints	Δρmin = −1.93 e Å^−3

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
Pr1	0.65325 (2)	0.88470 (2)	−0.008637 (18)	0.01878 (7)
Cl11	1.2261 (3)	1.1875 (2)	0.41765 (13)	0.1008 (8)
Cl12	1.0601 (5)	1.3109 (2)	0.2932 (3)	0.1313 (11)
Cl21	0.2443 (2)	0.8431 (2)	0.22203 (15)	0.0737 (5)
Cl22	0.05231 (17)	0.63990 (15)	−0.01078 (19)	0.0689 (5)
Cl31	0.7033 (3)	1.0247 (2)	0.44764 (13)	0.0806 (6)
Cl32	0.7404 (3)	1.2728 (2)	0.47545 (14)	0.0996 (8)
O11	0.9466 (3)	0.9928 (3)	0.1121 (3)	0.0336 (7)
O12	1.1941 (4)	1.1189 (3)	0.1497 (3)	0.0419 (8)
O21	0.3483 (4)	0.9178 (3)	0.0033 (3)	0.0341 (7)
O22	0.4017 (4)	0.7540 (3)	0.0126 (3)	0.0361 (7)
O31	0.6606 (4)	1.0051 (3)	0.2011 (2)	0.0305 (6)
O32	0.5390 (4)	1.1476 (3)	0.2052 (3)	0.0357 (7)
N1	0.6008 (5)	0.6517 (3)	−0.1383 (3)	0.0316 (8)
N2	0.7522 (4)	0.7520 (3)	0.1058 (3)	0.0295 (7)
C1	0.5354 (7)	0.6057 (5)	−0.2601 (4)	0.0458 (12)
H1	0.5076	0.6572	−0.2968	0.055*
C2	0.5071 (8)	0.4857 (5)	−0.3344 (5)	0.0539 (14)
H2	0.4608	0.4569	−0.4190	0.065*
C3	0.5488 (8)	0.4100 (5)	−0.2804 (5)	0.0548 (14)
H3	0.5329	0.3290	−0.3282	0.066*
C4	0.6142 (6)	0.4546 (5)	−0.1550 (5)	0.0434 (11)
H4	0.6418	0.4040	−0.1171	0.052*
C5	0.6386 (5)	0.5759 (4)	−0.0855 (4)	0.0288 (8)
C6	0.7123 (5)	0.6309 (4)	0.0494 (4)	0.0284 (8)
C7	0.7468 (6)	0.5604 (5)	0.1149 (5)	0.0410 (11)
H7	0.7151	0.4758	0.0746	0.049*
C8	0.8278 (7)	0.6168 (5)	0.2390 (5)	0.0496 (13)
H8	0.8533	0.5711	0.2835	0.059*
C9	0.8706 (6)	0.7413 (6)	0.2968 (5)	0.0475 (12)
H9	0.9268	0.7813	0.3808	0.057*
C10	0.8288 (6)	0.8063 (5)	0.2279 (4)	0.0391 (10)
H10	0.8546	0.8905	0.2674	0.047*
C11	1.0681 (5)	1.0868 (4)	0.1733 (3)	0.0275 (8)
C12	1.0598 (6)	1.1703 (5)	0.2937 (4)	0.0453 (12)
H12	0.9572	1.1319	0.3025	0.054*
C21	0.3170 (5)	0.8217 (4)	0.0212 (4)	0.0269 (8)
C22	0.1696 (6)	0.7954 (4)	0.0619 (5)	0.0379 (10)
H22	0.1001	0.8430	0.0414	0.045*
C31	0.6077 (5)	1.0864 (4)	0.2511 (3)	0.0289 (8)
C32	0.6225 (7)	1.1186 (5)	0.3854 (4)	0.0471 (13)
H32	0.5114	1.1078	0.3888	0.056*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pr1	0.01734 (10)	0.01784 (11)	0.02183 (10)	0.00468 (8)	0.00785 (7)	0.00883 (7)
Cl11	0.1037 (14)	0.152 (2)	0.0257 (6)	0.0538 (15)	0.0100 (7)	0.0134 (9)
Cl12	0.201 (3)	0.0873 (18)	0.153 (2)	0.096 (2)	0.101 (2)	0.0458 (17)
Cl21	0.0764 (10)	0.1117 (15)	0.0618 (9)	0.0391 (11)	0.0469 (8)	0.0473 (10)
Cl22	0.0358 (7)	0.0454 (9)	0.1322 (15)	0.0066 (7)	0.0428 (8)	0.0384 (9)
Cl31	0.1190 (15)	0.1132 (15)	0.0420 (7)	0.0706 (13)	0.0314 (8)	0.0472 (9)
Cl32	0.1379 (19)	0.0765 (14)	0.0359 (7)	0.0382 (14)	−0.0071 (9)	−0.0095 (8)
O11	0.0236 (14)	0.038 (2)	0.0297 (14)	0.0005 (14)	0.0067 (11)	0.0102 (13)
O12	0.0272 (15)	0.052 (2)	0.0288 (15)	−0.0051 (15)	0.0132 (12)	0.0047 (15)
O21	0.0456 (17)	0.0240 (17)	0.0363 (15)	0.0074 (15)	0.0180 (14)	0.0166 (13)
O22	0.0296 (15)	0.0285 (18)	0.064 (2)	0.0138 (15)	0.0268 (15)	0.0241 (16)
O31	0.0323 (15)	0.0383 (18)	0.0276 (13)	0.0186 (15)	0.0134 (12)	0.0147 (13)
O32	0.0385 (16)	0.0365 (19)	0.0285 (14)	0.0187 (16)	0.0062 (12)	0.0090 (13)
N1	0.0384 (19)	0.023 (2)	0.0329 (17)	0.0089 (17)	0.0148 (15)	0.0100 (15)
N2	0.0262 (16)	0.032 (2)	0.0341 (17)	0.0119 (16)	0.0106 (14)	0.0162 (16)
C1	0.065 (3)	0.033 (3)	0.036 (2)	0.015 (3)	0.017 (2)	0.011 (2)
C2	0.071 (4)	0.039 (3)	0.038 (3)	0.011 (3)	0.017 (2)	0.005 (2)
C3	0.061 (3)	0.026 (3)	0.063 (3)	0.012 (3)	0.021 (3)	0.003 (2)
C4	0.038 (2)	0.028 (3)	0.061 (3)	0.013 (2)	0.014 (2)	0.015 (2)
C5	0.0215 (18)	0.026 (2)	0.043 (2)	0.0103 (18)	0.0146 (16)	0.0138 (18)
C6	0.0254 (19)	0.027 (2)	0.046 (2)	0.0145 (19)	0.0200 (18)	0.0212 (19)
C7	0.043 (3)	0.042 (3)	0.060 (3)	0.022 (2)	0.030 (2)	0.033 (3)
C8	0.055 (3)	0.060 (4)	0.065 (3)	0.031 (3)	0.029 (3)	0.048 (3)
C9	0.045 (3)	0.065 (4)	0.044 (3)	0.022 (3)	0.016 (2)	0.034 (3)
C10	0.039 (2)	0.044 (3)	0.036 (2)	0.017 (2)	0.0096 (19)	0.019 (2)
C11	0.0201 (18)	0.036 (3)	0.0219 (17)	0.0035 (19)	0.0074 (14)	0.0099 (17)
C12	0.034 (2)	0.048 (3)	0.036 (2)	0.000 (2)	0.0161 (19)	0.000 (2)
C21	0.0246 (19)	0.021 (2)	0.035 (2)	0.0035 (18)	0.0117 (16)	0.0142 (17)
C22	0.032 (2)	0.036 (3)	0.064 (3)	0.016 (2)	0.028 (2)	0.030 (2)
C31	0.0246 (19)	0.035 (3)	0.0246 (18)	0.0113 (19)	0.0079 (15)	0.0089 (17)
C32	0.049 (3)	0.067 (4)	0.030 (2)	0.032 (3)	0.015 (2)	0.016 (2)

Geometric parameters (Å, º)

Pr1—O21^i	2.404 (3)	N1—C5	1.352 (5)
Pr1—O32^i	2.442 (3)	N2—C6	1.335 (5)
Pr1—O11	2.453 (3)	N2—C10	1.344 (6)
Pr1—O12^ii	2.456 (3)	C1—C2	1.379 (7)
Pr1—O31	2.499 (3)	C1—H1	0.9300
Pr1—O22	2.578 (3)	C2—C3	1.372 (8)
Pr1—N2	2.634 (3)	C2—H2	0.9300
Pr1—N1	2.641 (4)	C3—C4	1.374 (8)
Pr1—O21	2.855 (3)	C3—H3	0.9300
Pr1—C21	3.064 (4)	C4—C5	1.385 (6)
Cl11—C12	1.757 (5)	C4—H4	0.9300
Cl12—C12	1.727 (6)	C5—C6	1.477 (6)
Cl21—C22	1.762 (5)	C6—C7	1.395 (6)
Cl22—C22	1.751 (5)	C7—C8	1.370 (8)
Cl31—C32	1.761 (5)	C7—H7	0.9300
Cl32—C32	1.754 (6)	C8—C9	1.370 (8)
O11—C11	1.241 (5)	C8—H8	0.9300
O12—C11	1.240 (5)	C9—C10	1.385 (6)
O12—Pr1^ii	2.456 (3)	C9—H9	0.9300
O21—C21	1.255 (5)	C10—H10	0.9300
O21—Pr1^i	2.404 (3)	C11—C12	1.533 (6)
O22—C21	1.234 (5)	C12—H12	0.9800
O31—C31	1.241 (5)	C21—C22	1.524 (5)
O32—C31	1.250 (5)	C22—H22	0.9800
O32—Pr1^i	2.442 (3)	C31—C32	1.536 (6)
N1—C1	1.334 (6)	C32—H32	0.9800
O21^i—Pr1—O32^i	72.45 (11)	N1—C1—H1	118.4
O21^i—Pr1—O11	83.69 (11)	C2—C1—H1	118.4
O32^i—Pr1—O11	137.27 (11)	C3—C2—C1	118.4 (5)
O21^i—Pr1—O12^ii	86.00 (11)	C3—C2—H2	120.8
O32^i—Pr1—O12^ii	72.03 (10)	C1—C2—H2	120.8
O11—Pr1—O12^ii	71.40 (10)	C2—C3—C4	119.5 (5)
O21^i—Pr1—O31	74.36 (9)	C2—C3—H3	120.3
O32^i—Pr1—O31	128.11 (9)	C4—C3—H3	120.3
O11—Pr1—O31	75.21 (10)	C3—C4—C5	119.3 (5)
O12^ii—Pr1—O31	142.79 (10)	C3—C4—H4	120.4
O21^i—Pr1—O22	116.88 (10)	C5—C4—H4	120.4
O32^i—Pr1—O22	85.20 (11)	N1—C5—C4	121.5 (4)
O11—Pr1—O22	137.52 (10)	N1—C5—C6	116.2 (4)
O12^ii—Pr1—O22	141.37 (11)	C4—C5—C6	122.2 (4)
O31—Pr1—O22	75.67 (11)	N2—C6—C7	121.3 (4)
O21^i—Pr1—N2	149.07 (11)	N2—C6—C5	117.0 (3)
O32^i—Pr1—N2	138.24 (11)	C7—C6—C5	121.6 (4)
O11—Pr1—N2	73.45 (11)	C8—C7—C6	119.5 (5)
O12^ii—Pr1—N2	105.47 (11)	C8—C7—H7	120.3
O31—Pr1—N2	79.76 (10)	C6—C7—H7	120.3
O22—Pr1—N2	71.47 (10)	C9—C8—C7	119.3 (4)
O21^i—Pr1—N1	148.93 (10)	C9—C8—H8	120.4
O32^i—Pr1—N1	78.82 (11)	C7—C8—H8	120.4
O11—Pr1—N1	110.94 (11)	C8—C9—C10	118.8 (5)
O12^ii—Pr1—N1	73.93 (12)	C8—C9—H9	120.6
O31—Pr1—N1	134.88 (10)	C10—C9—H9	120.6
O22—Pr1—N1	71.25 (10)	N2—C10—C9	122.3 (5)
N2—Pr1—N1	61.24 (11)	N2—C10—H10	118.9
O21^i—Pr1—O21	69.76 (11)	C9—C10—H10	118.9
O32^i—Pr1—O21	66.48 (9)	O12—C11—O11	128.0 (4)
O11—Pr1—O21	136.64 (9)	O12—C11—C12	117.3 (4)
O12^ii—Pr1—O21	136.47 (10)	O11—C11—C12	114.6 (3)
O31—Pr1—O21	65.13 (9)	C11—C12—Cl12	110.7 (4)
O22—Pr1—O21	47.30 (8)	C11—C12—Cl11	109.9 (3)
N2—Pr1—O21	113.92 (9)	Cl12—C12—Cl11	110.5 (3)
N1—Pr1—O21	109.27 (10)	C11—C12—H12	108.5
O21^i—Pr1—C21	93.60 (11)	Cl12—C12—H12	108.5
O32^i—Pr1—C21	76.58 (11)	Cl11—C12—H12	108.5
O11—Pr1—C21	141.25 (10)	O22—C21—O21	123.7 (4)
O12^ii—Pr1—C21	147.18 (10)	O22—C21—C22	120.5 (4)
O31—Pr1—C21	66.93 (11)	O21—C21—C22	115.7 (3)
O22—Pr1—C21	23.28 (10)	O22—C21—Pr1	55.7 (2)
N2—Pr1—C21	91.55 (10)	O21—C21—Pr1	68.6 (2)
N1—Pr1—C21	90.98 (11)	C22—C21—Pr1	168.6 (3)
O21—Pr1—C21	24.16 (9)	C21—C22—Cl22	111.3 (3)
C11—O11—Pr1	152.9 (3)	C21—C22—Cl21	108.0 (3)
C11—O12—Pr1^ii	152.8 (3)	Cl22—C22—Cl21	110.7 (3)
C21—O21—Pr1^i	160.1 (3)	C21—C22—H22	108.9
C21—O21—Pr1	87.3 (2)	Cl22—C22—H22	108.9
Pr1^i—O21—Pr1	110.24 (11)	Cl21—C22—H22	108.9
C21—O22—Pr1	101.0 (2)	O31—C31—O32	128.0 (4)
C31—O31—Pr1	138.4 (2)	O31—C31—C32	118.7 (4)
C31—O32—Pr1^i	137.8 (3)	O32—C31—C32	113.3 (3)
C1—N1—C5	118.0 (4)	C31—C32—Cl32	110.3 (4)
C1—N1—Pr1	119.8 (3)	C31—C32—Cl31	113.9 (3)
C5—N1—Pr1	122.2 (3)	Cl32—C32—Cl31	110.1 (3)
C6—N2—C10	118.8 (4)	C31—C32—H32	107.4
C6—N2—Pr1	122.3 (3)	Cl32—C32—H32	107.4
C10—N2—Pr1	118.4 (3)	Cl31—C32—H32	107.4
N1—C1—C2	123.3 (5)

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