Di-μ_1,1-azido-bis­[azido­(N,N-dimethyl­propane-1,3-diamine-κ²N,N′)zinc(II)]

The title compound, [Zn₂(N₃)₄(C₅H₁₄N₂)₂], is a dinuclear zinc(II) compound. The mol­ecule is centrosymmetric, so pairs of equivalent ligands lie trans to each other in a slightly distorted square-pyramidal coordination geometry.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.028
• wR factor = 0.082
• Data-to-parameter ratio = 16.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.96
PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 =          3
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Zn1    -   N3      ..       5.72 su
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         N6
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N7
PLAT420_ALERT_2_C D-H Without Acceptor       N2     -   H2B    ...          ?

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 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
   4 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: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Di-µ_1,1-azido-bis[azido(N,N-dimethylpropane-1,3-diamine-κ²N,N')zinc(II)]

Crystal data

[Zn2(N3)4(C5H14N2)2]	F(000) = 520
Mr = 503.22	Dx = 1.606 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3740 reflections
a = 9.441 (1) Å	θ = 2.5–27.5°
b = 11.152 (2) Å	µ = 2.34 mm^−1
c = 10.211 (1) Å	T = 298 K
β = 104.534 (1)°	Block, colourless
V = 1040.7 (2) Å^3	0.22 × 0.21 × 0.21 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer	2145 independent reflections
Radiation source: fine-focus sealed tube	1909 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.022
ω scans	θmax = 26.5°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→11
Tmin = 0.627, Tmax = 0.640	k = −14→13
6979 measured reflections	l = −12→12

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) = 0.082	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0484P)^2 + 0.3686P] where P = (Fo^2 + 2Fc^2)/3
2145 reflections	(Δ/σ)max = 0.001
129 parameters	Δρmax = 0.40 e Å^−3
0 restraints	Δρmin = −0.36 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	0.47689 (3)	0.59393 (2)	0.62518 (3)	0.03133 (12)
N1	0.2939 (2)	0.68410 (17)	0.65052 (19)	0.0306 (4)
N2	0.5550 (2)	0.7404 (2)	0.5522 (3)	0.0472 (6)
H2A	0.5978	0.7868	0.6233	0.057*
H2B	0.6261	0.7161	0.5138	0.057*
N3	0.3580 (2)	0.50010 (19)	0.4211 (2)	0.0378 (5)
N4	0.2411 (2)	0.51676 (17)	0.34733 (19)	0.0317 (4)
N5	0.1266 (2)	0.5363 (2)	0.2782 (2)	0.0526 (6)
N6	0.4716 (3)	0.4889 (3)	0.7800 (3)	0.0646 (8)
N7	0.5515 (2)	0.41390 (19)	0.8242 (2)	0.0390 (5)
N8	0.6267 (3)	0.3355 (3)	0.8740 (3)	0.0624 (7)
C1	0.2316 (3)	0.7692 (2)	0.5388 (2)	0.0370 (5)
H1A	0.1485	0.8092	0.5594	0.044*
H1B	0.1950	0.7233	0.4566	0.044*
C2	0.3346 (3)	0.8639 (2)	0.5112 (3)	0.0406 (6)
H2C	0.2783	0.9219	0.4484	0.049*
H2D	0.3778	0.9056	0.5950	0.049*
C3	0.4551 (3)	0.8170 (2)	0.4540 (3)	0.0445 (6)
H3A	0.4134	0.7713	0.3726	0.053*
H3B	0.5092	0.8837	0.4295	0.053*
C4	0.3342 (3)	0.7483 (3)	0.7817 (3)	0.0449 (6)
H4A	0.2513	0.7926	0.7939	0.067*
H4B	0.4134	0.8025	0.7823	0.067*
H4C	0.3641	0.6913	0.8538	0.067*
C5	0.1763 (3)	0.5972 (2)	0.6556 (3)	0.0477 (7)
H5A	0.0911	0.6398	0.6650	0.072*
H5B	0.2094	0.5445	0.7314	0.072*
H5C	0.1524	0.5511	0.5736	0.072*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.02723 (17)	0.02911 (17)	0.03819 (19)	0.00370 (9)	0.00922 (12)	0.00429 (10)
N1	0.0276 (9)	0.0302 (9)	0.0364 (10)	0.0021 (8)	0.0125 (8)	0.0017 (8)
N2	0.0334 (11)	0.0377 (11)	0.0741 (16)	−0.0001 (9)	0.0200 (11)	0.0145 (11)
N3	0.0290 (10)	0.0426 (11)	0.0390 (11)	0.0105 (9)	0.0030 (8)	−0.0079 (9)
N4	0.0275 (9)	0.0313 (10)	0.0370 (10)	0.0004 (8)	0.0095 (8)	−0.0082 (8)
N5	0.0313 (11)	0.0659 (16)	0.0532 (14)	0.0076 (11)	−0.0031 (10)	−0.0131 (12)
N6	0.0606 (16)	0.0699 (17)	0.0748 (18)	0.0272 (14)	0.0386 (14)	0.0407 (15)
N7	0.0357 (11)	0.0449 (13)	0.0390 (12)	−0.0051 (10)	0.0142 (9)	0.0096 (9)
N8	0.0536 (15)	0.0669 (17)	0.0682 (17)	0.0182 (14)	0.0180 (13)	0.0327 (14)
C1	0.0305 (11)	0.0390 (13)	0.0397 (13)	0.0085 (10)	0.0053 (10)	0.0023 (10)
C2	0.0474 (14)	0.0297 (11)	0.0424 (13)	0.0072 (11)	0.0072 (11)	0.0080 (11)
C3	0.0514 (15)	0.0364 (13)	0.0488 (15)	−0.0013 (11)	0.0183 (12)	0.0100 (11)
C4	0.0526 (16)	0.0481 (15)	0.0364 (13)	0.0084 (12)	0.0158 (12)	−0.0028 (11)
C5	0.0370 (14)	0.0447 (15)	0.0684 (19)	−0.0019 (11)	0.0262 (13)	0.0052 (13)

Geometric parameters (Å, º)

Zn1—N6	1.977 (2)	N7—N8	1.160 (3)
Zn1—N2	2.011 (2)	C1—C2	1.509 (4)
Zn1—N3^i	2.031 (2)	C1—H1A	0.97
Zn1—N1	2.0704 (19)	C1—H1B	0.97
Zn1—N3	2.350 (2)	C2—C3	1.497 (4)
N1—C4	1.481 (3)	C2—H2C	0.97
N1—C5	1.484 (3)	C2—H2D	0.97
N1—C1	1.487 (3)	C3—H3A	0.97
N2—C3	1.466 (3)	C3—H3B	0.97
N2—H2A	0.90	C4—H4A	0.96
N2—H2B	0.90	C4—H4B	0.96
N3—N4	1.184 (3)	C4—H4C	0.96
N3—Zn1^i	2.031 (2)	C5—H5A	0.96
N4—N5	1.154 (3)	C5—H5B	0.96
N6—N7	1.142 (3)	C5—H5C	0.96
N6—Zn1—N2	149.58 (12)	N1—C1—H1A	108.3
N6—Zn1—N3^i	93.17 (10)	C2—C1—H1A	108.3
N2—Zn1—N3^i	87.66 (9)	N1—C1—H1B	108.3
N6—Zn1—N1	89.90 (9)	C2—C1—H1B	108.3
N2—Zn1—N1	92.67 (9)	H1A—C1—H1B	107.4
N3^i—Zn1—N1	173.36 (8)	C3—C2—C1	114.7 (2)
N6—Zn1—N3	110.04 (12)	C3—C2—H2C	108.6
N2—Zn1—N3	99.86 (10)	C1—C2—H2C	108.6
N3^i—Zn1—N3	77.73 (8)	C3—C2—H2D	108.6
N1—Zn1—N3	95.69 (7)	C1—C2—H2D	108.6
C4—N1—C5	108.0 (2)	H2C—C2—H2D	107.6
C4—N1—C1	110.34 (18)	N2—C3—C2	111.0 (2)
C5—N1—C1	106.7 (2)	N2—C3—H3A	109.4
C4—N1—Zn1	108.33 (15)	C2—C3—H3A	109.4
C5—N1—Zn1	110.00 (14)	N2—C3—H3B	109.4
C1—N1—Zn1	113.35 (14)	C2—C3—H3B	109.4
C3—N2—Zn1	119.59 (16)	H3A—C3—H3B	108.0
C3—N2—H2A	107.4	N1—C4—H4A	109.5
Zn1—N2—H2A	107.4	N1—C4—H4B	109.5
C3—N2—H2B	107.4	H4A—C4—H4B	109.5
Zn1—N2—H2B	107.4	N1—C4—H4C	109.5
H2A—N2—H2B	107.0	H4A—C4—H4C	109.5
N4—N3—Zn1^i	125.45 (16)	H4B—C4—H4C	109.5
N4—N3—Zn1	130.98 (16)	N1—C5—H5A	109.5
Zn1^i—N3—Zn1	102.27 (8)	N1—C5—H5B	109.5
N5—N4—N3	177.6 (2)	H5A—C5—H5B	109.5
N7—N6—Zn1	127.1 (2)	N1—C5—H5C	109.5
N6—N7—N8	175.6 (3)	H5A—C5—H5C	109.5
N1—C1—C2	116.1 (2)	H5B—C5—H5C	109.5

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···N5^ii	0.90	2.50	3.346 (4)	157

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