Diammine[pyridine-2,6-dicarboxyl­ato-κ³O²,N,O⁶]zinc(II)

The title complex, [Zn(C₇H₃NO₄)(NH₃)₂], was prepared by a hydro­thermal reaction at 413 K. The complex has mirror symmetry. The Zn^II ion is coordinated by a tridentate pyridine­dicarboxyl­ate dianion and two ammonia mol­ecules, in a distorted trigonal–bipyramidal coordination geometry. An inter­molecular N—H...O hydrogen-bonding network stabilizes the crystal structure.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.028
• wR factor = 0.074
• Data-to-parameter ratio = 13.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Zn1    -   O3      ..       7.50 su

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; 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.

Diammine[pyridine-2,6-dicarboxylato-κ³N,O,O']zinc(II)

Crystal data

[Zn(C7H3NO4)(NH3)2]	F(000) = 536.0
Mr = 264.56	Dx = 1.828 Mg m^−3
Orthorhombic, Pbcm	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2c 2b	Cell parameters from 121 reflections
a = 10.4696 (9) Å	θ = 2.2–26.0°
b = 12.6989 (11) Å	µ = 2.55 mm^−1
c = 7.2309 (6) Å	T = 295 K
V = 961.37 (14) Å^3	Block, white
Z = 4	0.36 × 0.32 × 0.25 mm

Data collection

Bruker APEX area-dectector diffractometer	1244 independent reflections
Radiation source: fine-focus sealed tube	1099 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
φ and ω scans	θmax = 27.9°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −13→5
Tmin = 0.390, Tmax = 0.530	k = −16→16
5637 measured reflections	l = −9→9

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)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.074	H-atom parameters constrained
S = 1.16	w = 1/[σ^2(Fo^2) + (0.0402P)^2 + 0.2581P] where P = (Fo^2 + 2Fc^2)/3
1244 reflections	(Δ/σ)max = 0.004
89 parameters	Δρmax = 0.39 e Å^−3
0 restraints	Δρmin = −0.79 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
Zn1	0.72628 (3)	0.496398 (18)	0.2500	0.02703 (13)
O3	0.52852 (15)	0.41952 (13)	0.2500	0.0316 (4)
N1	0.75974 (18)	0.34010 (15)	0.2500	0.0224 (4)
N2	0.69883 (15)	0.58910 (12)	0.4707 (2)	0.0336 (3)
H2A	0.6723	0.6522	0.4335	0.050*
H2B	0.7719	0.5958	0.5326	0.050*
H2C	0.6401	0.5604	0.5441	0.050*
C1	0.6643 (2)	0.27089 (17)	0.2500	0.0228 (5)
C2	0.5313 (2)	0.31943 (18)	0.2500	0.0251 (5)
C3	0.8811 (2)	0.30815 (17)	0.2500	0.0244 (5)
O4	0.43869 (17)	0.25949 (14)	0.2500	0.0357 (4)
C4	0.9780 (2)	0.39754 (18)	0.2500	0.0286 (5)
O2	1.09258 (16)	0.37400 (15)	0.2500	0.0384 (4)
C5	0.6877 (2)	0.16356 (19)	0.2500	0.0323 (5)
H5	0.6206	0.1155	0.2500	0.039*
O1	0.9304 (2)	0.48892 (13)	0.2500	0.0385 (5)
C6	0.8137 (3)	0.1294 (2)	0.2500	0.0368 (6)
H6	0.8319	0.0577	0.2500	0.044*
C7	0.9118 (2)	0.2022 (2)	0.2500	0.0323 (5)
H7	0.9967	0.1804	0.2500	0.039*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0277 (2)	0.01835 (18)	0.0351 (2)	0.00236 (9)	0.000	0.000
O3	0.0209 (8)	0.0231 (8)	0.0509 (10)	−0.0003 (7)	0.000	0.000
N1	0.0200 (9)	0.0190 (9)	0.0283 (10)	0.0000 (7)	0.000	0.000
N2	0.0319 (7)	0.0318 (8)	0.0371 (8)	0.0048 (6)	−0.0023 (6)	−0.0049 (6)
C1	0.0223 (11)	0.0218 (11)	0.0243 (10)	−0.0009 (8)	0.000	0.000
C2	0.0231 (11)	0.0244 (11)	0.0279 (11)	−0.0025 (9)	0.000	0.000
C3	0.0219 (10)	0.0232 (10)	0.0280 (11)	0.0016 (9)	0.000	0.000
O4	0.0231 (8)	0.0308 (9)	0.0532 (11)	−0.0078 (7)	0.000	0.000
C4	0.0210 (11)	0.0288 (12)	0.0360 (12)	−0.0015 (9)	0.000	0.000
O2	0.0190 (8)	0.0394 (10)	0.0569 (12)	0.0011 (8)	0.000	0.000
C5	0.0302 (12)	0.0213 (11)	0.0452 (15)	−0.0028 (10)	0.000	0.000
O1	0.0225 (9)	0.0237 (9)	0.0693 (14)	−0.0017 (7)	0.000	0.000
C6	0.0388 (14)	0.0201 (11)	0.0515 (16)	0.0055 (11)	0.000	0.000
C7	0.0264 (12)	0.0275 (12)	0.0430 (14)	0.0064 (10)	0.000	0.000

Geometric parameters (Å, º)

Zn1—N1	2.0154 (19)	C1—C2	1.522 (3)
Zn1—N2	2.0039 (15)	C2—O4	1.233 (3)
Zn1—N2^i	2.0039 (15)	C3—C7	1.384 (3)
Zn1—O1	2.139 (2)	C3—C4	1.522 (3)
Zn1—O3	2.2891 (16)	C4—O2	1.237 (3)
O3—C2	1.271 (3)	C4—O1	1.263 (3)
N1—C1	1.331 (3)	C5—C6	1.389 (4)
N1—C3	1.334 (3)	C5—H5	0.9300
N2—H2A	0.8900	C6—C7	1.383 (4)
N2—H2B	0.8900	C6—H6	0.9300
N2—H2C	0.8900	C7—H7	0.9300
C1—C5	1.385 (3)
N1—Zn1—O1	77.45 (7)	N1—C1—C2	114.79 (19)
N1—Zn1—O3	74.76 (7)	C5—C1—C2	124.1 (2)
N1—Zn1—N2	127.12 (5)	O4—C2—O3	126.8 (2)
N2^i—Zn1—N1	127.12 (5)	O4—C2—C1	118.0 (2)
N2—Zn1—N2^i	105.58 (9)	O3—C2—C1	115.19 (19)
N2^i—Zn1—O1	99.75 (5)	N1—C3—C7	121.2 (2)
N2—Zn1—O3	96.94 (5)	N1—C3—C4	114.07 (19)
N2^i—Zn1—O3	96.94 (5)	C7—C3—C4	124.8 (2)
O1—Zn1—O3	152.21 (6)	O2—C4—O1	127.2 (2)
O1—Zn1—N2	99.75 (5)	O2—C4—C3	117.8 (2)
C2—O3—Zn1	113.94 (14)	O1—C4—C3	115.0 (2)
C1—N1—C3	121.0 (2)	C1—C5—C6	118.4 (2)
C1—N1—Zn1	121.32 (15)	C1—C5—H5	120.8
C3—N1—Zn1	117.71 (15)	C6—C5—H5	120.8
Zn1—N2—H2A	109.5	C4—O1—Zn1	115.76 (16)
Zn1—N2—H2B	109.5	C7—C6—C5	119.8 (2)
H2A—N2—H2B	109.5	C7—C6—H6	120.1
Zn1—N2—H2C	109.5	C5—C6—H6	120.1
H2A—N2—H2C	109.5	C6—C7—C3	118.5 (2)
H2B—N2—H2C	109.5	C6—C7—H7	120.7
N1—C1—C5	121.1 (2)	C3—C7—H7	120.7

Symmetry code: (i) x, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O4^ii	0.89	2.23	3.050 (2)	153
N2—H2B···O2^iii	0.89	2.15	3.011 (2)	162
N2—H2C···O3^iv	0.89	2.32	3.123 (2)	150

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