catena-Poly[[diaqua­dinitratozinc(II)]bis­(μ-1,4-di-3-pyridyl-2,3-diaza-1,3-butadiene)]

The polymeric title complex, [Zn(NO₃)₂(C₂₄H₂₀N₈)(H₂O)₂]_n, features distorted ZnN₂O₄ octa­hedra with each Zn^II atom being located on an inversion center. Adjacent Zn ions are doubly bridged by two equivalent 1,4-di-3-pyridyl-2,3-diaza-1,3-butadiene ligands to form linear chains.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.029
• wR factor = 0.082
• Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000)         200 Deg.
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Zn1    -   O1      ..       7.90 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Zn1    -   N1      ..       5.78 su
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C11

   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
   3 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
   0 ALERT type 5 Informative message, check


checkCIF publication errors

Alert level A
PUBL024_ALERT_1_A The number of authors is greater than 5.
              Please specify the role of each of the co-authors
              for your paper.

Author Response: Shakoya Paulin was an undergraduate research assistant for NSF Grant 0315152, which help provide the funding for this collaborative research project that resulted in the submission of this manuscript. Shakoya assisted in the initial preparation of the manuscript, graphics, and cif.

 Pierre Kelly was an undergraduate research assistant for NSF Grant 0315152,
 which provided the funding for this collaborative research project that
 resulted in the submission of this manuscript.  Pierre synthesized,
 characterized, and prepared the crystals of the title compound.

 Ken Williams is the Co-PI for NSF Grant 0315152, which provided the funding
 for this collaborative research project that resulted in the submission of
 this manuscript.  Ken also helped supervise and direct the work of Pierre
 Kelly, the undergraduate student who prepared crystals of the title compound.
 Ken also assisted in the preparation and writing of this manuscript.

 Andrea Goforth was a graduate research assistant for the linked NSF Grant
 0314164, which help provide the funding for this collaborative research
 project that resulted in the submission of this manuscript.  Andrea
 provided assistance in the synthesis of the L2 ligand that was subsequently
 used to prepare the title compound.  Andrea also assisted in the preparation
 and writing of this manuscript.

 Mark Smith is the crystallographer who collected the diffraction data and
 solved the crystal structure of the title compound.  Mark also assisted
 in the preparation and writing of this manuscript.

 LeRoy Peterson, Jr. is the PI of NSF Grant 0315152, which provided the
 funding for this collaborative research project that resulted in the
 submission of this manuscript. LeRoy also helped supervise and direct
 the work of Pierre Kelly, the undergraduate student who prepared
 crystals of the title compound.  LeRoy also assisted in the preparation,
 writing, and was responsible for the submission of this manuscript.

 Hans-Conrad zur Loye is the PI for the linked NSF Grant 0314164, which helped
 provide the funding for this collaborative research project that resulted in
 the submission of this manuscript.  Hans-Conrad directed the work of graduate
 student Andrea Goforth, who in turn assisted undergraduate student Pierre
 Kelly in synthesizing the L2 ligand that was used in the preparation of
 the title compound.  Hans-Conrad also assisted in the preparation and writing
 of this manuscript.


   1 ALERT level A = Data missing that is essential or data in wrong format
   0 ALERT level G = General alerts. Data that may be required is missing

---

Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000) and DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXTL.

catena-Poly[[diaquadinitratozinc(II)]bis(µ-1,4-di-3-pyridyl-2,3-diaza-1,3- butadiene)]

Crystal data

[Zn(NO3)2(C24H20N8)(H2O)2]	Z = 1
Mr = 645.90	F(000) = 332
Triclinic, P1	Dx = 1.556 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.8267 (11) Å	Cell parameters from 4740 reflections
b = 8.5320 (11) Å	θ = 2.6–26.4°
c = 11.7409 (16) Å	µ = 0.96 mm^−1
α = 81.113 (2)°	T = 150 K
β = 73.696 (2)°	Irregular, yellow
γ = 66.468 (2)°	0.40 × 0.26 × 0.14 mm
V = 689.12 (16) Å^3

Data collection

Bruker SMART APEX CCD diffractometer	2831 independent reflections
Radiation source: fine-focus sealed tube	2720 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.027
ω scans	θmax = 26.4°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −9→9
Tmin = 0.670, Tmax = 0.870	k = −10→10
6421 measured reflections	l = −14→14

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.029	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0472P)^2 + 0.1395P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max < 0.001
2831 reflections	Δρmax = 0.28 e Å^−3
205 parameters	Δρmin = −0.27 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: 0.026 (4)

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	0.5000	0.5000	0.0000	0.03357 (12)
C1	0.3722 (2)	0.2031 (2)	0.11047 (14)	0.0358 (3)
H1	0.2514	0.2845	0.1007	0.043*
C2	0.3792 (2)	0.0474 (2)	0.16972 (14)	0.0352 (3)
C3	0.5572 (3)	−0.0753 (2)	0.17813 (16)	0.0408 (4)
H3	0.5679	−0.1843	0.2162	0.049*
C4	0.7184 (3)	−0.0358 (2)	0.13008 (17)	0.0451 (4)
H4	0.8420	−0.1177	0.1341	0.054*
C5	0.6975 (2)	0.1244 (2)	0.07606 (16)	0.0391 (4)
H5	0.8091	0.1510	0.0442	0.047*
C6	0.2005 (3)	0.0181 (2)	0.22407 (16)	0.0414 (4)
H6	0.0903	0.0773	0.1931	0.050*
C7	0.0083 (3)	−0.2000 (2)	0.44669 (15)	0.0426 (4)
H7	0.1146	−0.2418	0.4820	0.051*
C8	−0.1524 (3)	−0.3555 (2)	0.60328 (15)	0.0434 (4)
H8	−0.0445	−0.3890	0.6364	0.052*
C9	−0.1565 (2)	−0.2483 (2)	0.50224 (14)	0.0401 (4)
C10	−0.3145 (3)	−0.1988 (3)	0.45575 (19)	0.0633 (6)
H10	−0.3242	−0.1242	0.3868	0.076*
C11	−0.4586 (4)	−0.2590 (4)	0.5106 (2)	0.0813 (9)
H11	−0.5684	−0.2270	0.4797	0.098*
C12	−0.4411 (3)	−0.3657 (3)	0.61068 (19)	0.0627 (6)
H12	−0.5413	−0.4061	0.6482	0.075*
N1	0.52685 (18)	0.24419 (17)	0.06653 (12)	0.0339 (3)
N2	0.1943 (2)	−0.0869 (2)	0.31257 (14)	0.0454 (3)
N3	0.0145 (2)	−0.1040 (2)	0.35278 (14)	0.0465 (4)
N4	−0.2904 (2)	−0.4149 (2)	0.65726 (13)	0.0484 (4)
N5	0.8224 (2)	0.4606 (2)	0.12657 (14)	0.0438 (3)
O1	0.64636 (17)	0.52385 (17)	0.12592 (11)	0.0447 (3)
O2	0.94046 (18)	0.35775 (18)	0.05151 (14)	0.0567 (4)
O3	0.8737 (2)	0.5058 (2)	0.20222 (16)	0.0733 (5)
O4	0.74937 (18)	0.39905 (16)	−0.13198 (12)	0.0394 (3)
H4A	0.741 (3)	0.442 (3)	−0.196 (2)	0.052 (6)*
H4B	0.842 (4)	0.402 (3)	−0.121 (2)	0.064 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.03070 (16)	0.03123 (16)	0.03557 (16)	−0.01316 (11)	−0.00577 (10)	0.00758 (10)
C1	0.0325 (7)	0.0371 (8)	0.0390 (8)	−0.0156 (6)	−0.0112 (6)	0.0070 (6)
C2	0.0403 (8)	0.0389 (8)	0.0318 (7)	−0.0218 (7)	−0.0095 (6)	0.0037 (6)
C3	0.0469 (9)	0.0325 (8)	0.0425 (9)	−0.0176 (7)	−0.0112 (7)	0.0077 (6)
C4	0.0369 (8)	0.0385 (9)	0.0548 (10)	−0.0114 (7)	−0.0130 (8)	0.0078 (7)
C5	0.0335 (8)	0.0391 (8)	0.0446 (9)	−0.0166 (7)	−0.0088 (6)	0.0055 (7)
C6	0.0416 (9)	0.0444 (9)	0.0431 (9)	−0.0238 (7)	−0.0110 (7)	0.0068 (7)
C7	0.0452 (9)	0.0488 (9)	0.0395 (9)	−0.0259 (8)	−0.0107 (7)	0.0058 (7)
C8	0.0486 (9)	0.0498 (10)	0.0361 (8)	−0.0247 (8)	−0.0122 (7)	0.0069 (7)
C9	0.0449 (9)	0.0461 (9)	0.0334 (8)	−0.0250 (8)	−0.0074 (7)	0.0044 (7)
C10	0.0617 (12)	0.0912 (16)	0.0507 (11)	−0.0474 (12)	−0.0259 (10)	0.0324 (11)
C11	0.0663 (14)	0.129 (2)	0.0717 (15)	−0.0651 (16)	−0.0343 (12)	0.0426 (16)
C12	0.0596 (12)	0.0869 (16)	0.0544 (12)	−0.0500 (12)	−0.0103 (10)	0.0163 (11)
N1	0.0329 (6)	0.0356 (7)	0.0343 (6)	−0.0164 (5)	−0.0086 (5)	0.0060 (5)
N2	0.0442 (8)	0.0532 (9)	0.0453 (8)	−0.0301 (7)	−0.0101 (6)	0.0111 (7)
N3	0.0452 (8)	0.0559 (9)	0.0447 (8)	−0.0312 (7)	−0.0104 (6)	0.0129 (7)
N4	0.0573 (9)	0.0557 (9)	0.0363 (7)	−0.0326 (8)	−0.0063 (7)	0.0085 (6)
N5	0.0416 (8)	0.0451 (8)	0.0507 (8)	−0.0199 (7)	−0.0221 (7)	0.0114 (7)
O1	0.0350 (6)	0.0531 (7)	0.0492 (7)	−0.0172 (5)	−0.0170 (5)	0.0028 (5)
O2	0.0381 (7)	0.0538 (8)	0.0781 (10)	−0.0127 (6)	−0.0186 (7)	−0.0068 (7)
O3	0.0622 (9)	0.0967 (13)	0.0717 (10)	−0.0223 (9)	−0.0407 (8)	−0.0100 (9)
O4	0.0349 (6)	0.0442 (7)	0.0355 (6)	−0.0156 (5)	−0.0064 (5)	0.0063 (5)

Geometric parameters (Å, º)

Zn1—O1	2.1839 (12)	C7—N3	1.269 (2)
Zn1—O4	2.0795 (12)	C7—C9	1.458 (2)
Zn1—O4^i	2.0795 (12)	C7—H7	0.9500
Zn1—N1^i	2.1487 (13)	C8—N4	1.334 (2)
Zn1—N1	2.1487 (13)	C8—C9	1.381 (2)
Zn1—O1^i	2.1839 (12)	C8—H8	0.9500
C1—N1	1.3364 (19)	C9—C10	1.377 (3)
C1—C2	1.389 (2)	C10—C11	1.379 (3)
C1—H1	0.9500	C10—H10	0.9500
C2—C3	1.388 (2)	C11—C12	1.374 (3)
C2—C6	1.469 (2)	C11—H11	0.9500
C3—C4	1.380 (2)	C12—N4	1.328 (3)
C3—H3	0.9500	C12—H12	0.9500
C4—C5	1.382 (2)	N2—N3	1.412 (2)
C4—H4	0.9500	N5—O3	1.236 (2)
C5—N1	1.341 (2)	N5—O2	1.239 (2)
C5—H5	0.9500	N5—O1	1.2653 (18)
C6—N2	1.266 (2)	O4—H4A	0.79 (3)
C6—H6	0.9500	O4—H4B	0.78 (3)
O1—Zn1—O1^i	180.0	C2—C6—H6	120.3
O4—Zn1—O1	95.05 (5)	N3—C7—C9	122.27 (16)
O4^i—Zn1—O1	84.95 (5)	N3—C7—H7	118.9
O4—Zn1—O4^i	180.0	C9—C7—H7	118.9
O4—Zn1—N1^i	90.79 (5)	N4—C8—C9	124.09 (17)
O4^i—Zn1—N1^i	89.21 (5)	N4—C8—H8	118.0
O4—Zn1—N1	89.21 (5)	C9—C8—H8	118.0
O4^i—Zn1—N1	90.79 (5)	C10—C9—C8	117.51 (16)
N1—Zn1—O1^i	87.98 (5)	C10—C9—C7	123.18 (16)
N1^i—Zn1—N1	180.0	C8—C9—C7	119.24 (16)
N1^i—Zn1—O1	87.99 (5)	C9—C10—C11	119.09 (19)
N1—Zn1—O1	92.02 (5)	C9—C10—H10	120.5
O4—Zn1—O1^i	84.95 (5)	C11—C10—H10	120.5
O4^i—Zn1—O1^i	95.05 (5)	C12—C11—C10	119.1 (2)
N1^i—Zn1—O1^i	92.01 (5)	C12—C11—H11	120.4
N1—C1—C2	123.35 (14)	C10—C11—H11	120.4
N1—C1—H1	118.3	N4—C12—C11	122.91 (18)
C2—C1—H1	118.3	N4—C12—H12	118.5
C3—C2—C1	118.32 (14)	C11—C12—H12	118.5
C3—C2—C6	121.80 (14)	C1—N1—C5	117.43 (13)
C1—C2—C6	119.86 (15)	C1—N1—Zn1	121.21 (10)
C4—C3—C2	118.69 (15)	C5—N1—Zn1	121.06 (10)
C4—C3—H3	120.7	C6—N2—N3	112.69 (15)
C2—C3—H3	120.7	C7—N3—N2	111.10 (15)
C3—C4—C5	119.12 (16)	C12—N4—C8	117.30 (16)
C3—C4—H4	120.4	O3—N5—O2	121.08 (16)
C5—C4—H4	120.4	O3—N5—O1	118.59 (16)
N1—C5—C4	123.00 (15)	O2—N5—O1	120.32 (14)
N1—C5—H5	118.5	N5—O1—Zn1	130.56 (11)
C4—C5—H5	118.5	Zn1—O4—H4A	113.6 (16)
N2—C6—C2	119.47 (16)	Zn1—O4—H4B	115.2 (18)
N2—C6—H6	120.3	H4A—O4—H4B	107 (2)
N1—C1—C2—C3	−3.6 (2)	O4—Zn1—N1—C1	−143.55 (13)
N1—C1—C2—C6	174.83 (15)	O4^i—Zn1—N1—C1	36.45 (13)
C1—C2—C3—C4	1.6 (2)	O1—Zn1—N1—C1	121.43 (12)
C6—C2—C3—C4	−176.78 (16)	O1^i—Zn1—N1—C1	−58.57 (12)
C2—C3—C4—C5	0.5 (3)	O4—Zn1—N1—C5	42.97 (13)
C3—C4—C5—N1	−0.9 (3)	O4^i—Zn1—N1—C5	−137.02 (13)
C3—C2—C6—N2	25.5 (3)	O1—Zn1—N1—C5	−52.05 (13)
C1—C2—C6—N2	−152.91 (17)	O1^i—Zn1—N1—C5	127.95 (13)
N4—C8—C9—C10	0.8 (3)	C2—C6—N2—N3	−178.57 (15)
N4—C8—C9—C7	−176.20 (17)	C9—C7—N3—N2	−175.76 (16)
N3—C7—C9—C10	2.1 (3)	C6—N2—N3—C7	−175.11 (17)
N3—C7—C9—C8	178.92 (18)	C11—C12—N4—C8	0.4 (4)
C8—C9—C10—C11	−0.6 (4)	C9—C8—N4—C12	−0.6 (3)
C7—C9—C10—C11	176.2 (2)	O3—N5—O1—Zn1	173.23 (14)
C9—C10—C11—C12	0.5 (5)	O2—N5—O1—Zn1	−5.6 (2)
C10—C11—C12—N4	−0.3 (5)	O4—Zn1—O1—N5	−14.08 (15)
C2—C1—N1—C5	3.2 (2)	O4^i—Zn1—O1—N5	165.92 (15)
C2—C1—N1—Zn1	−170.48 (12)	N1^i—Zn1—O1—N5	−104.70 (14)
C4—C5—N1—C1	−0.9 (3)	N1—Zn1—O1—N5	75.30 (14)
C4—C5—N1—Zn1	172.79 (14)

Symmetry code: (i) −x+1, −y+1, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H4A···N4^ii	0.79 (3)	1.97 (3)	2.750 (2)	170 (2)
O4—H4B···O2	0.78 (3)	2.29 (3)	2.856 (2)	130 (2)

Symmetry code: (ii) x+1, y+1, z−1.