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The title compound, [Mn2(N3)4(C14H17N3)2], comprises two [Mn(bpea)(N3)]+ fragments [where bpea is the tridentate ligand N,N-bis­(2-pyridylmeth­yl)ethyl­amine] bridged by two azide anions to form a centrosymmetric dinuclear complex. The coordination environment around the MnII atoms is distorted octa­hedral.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807005405/bi2156sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807005405/bi2156Isup2.hkl
Contains datablock I

CCDC reference: 614209

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.026
  • wR factor = 0.069
  • Data-to-parameter ratio = 13.1

checkCIF/PLATON results

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Alert level B PLAT230_ALERT_2_B Hirshfeld Test Diff for N4 - N5 .. 31.65 su PLAT230_ALERT_2_B Hirshfeld Test Diff for N5 - N6 .. 10.18 su
Alert level C PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.85 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 - N4 .. 5.23 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N8
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_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 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 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

Computing details top

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

Bis(µ-azido-κ2N:N)bis[(azido-κN)[N,N-bis(2-pyridylmethyl- κN)ethylamine]manganese(II) top
Crystal data top
[Mn2(N3)4(C14H17N3)2]Z = 1
Mr = 732.61F(000) = 378
Triclinic, P1Dx = 1.482 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.8943 (18) ÅCell parameters from 3298 reflections
b = 9.1784 (19) Åθ = 2.7–27.8°
c = 10.963 (2) ŵ = 0.82 mm1
α = 74.254 (2)°T = 293 K
β = 76.212 (2)°Block, colourless
γ = 75.797 (3)°0.36 × 0.22 × 0.14 mm
V = 820.8 (3) Å3
Data collection top
Bruker SMART CCD
diffractometer
2851 independent reflections
Radiation source: fine-focus sealed tube2627 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.010
φ and ω scansθmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 910
Tmin = 0.742, Tmax = 0.891k = 1010
4422 measured reflectionsl = 1313
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0298P)2 + 0.423P]
where P = (Fo2 + 2Fc2)/3
2851 reflections(Δ/σ)max < 0.001
218 parametersΔρmax = 0.36 e Å3
0 restraintsΔρmin = 0.24 e Å3
Special details top

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 (Å2) top
xyzUiso*/Ueq
Mn10.48019 (3)0.06585 (3)0.33525 (2)0.03146 (10)
N10.62510 (19)0.05477 (19)0.17180 (15)0.0399 (4)
N20.33657 (18)0.11375 (17)0.32158 (14)0.0339 (3)
N30.24754 (17)0.19962 (17)0.27929 (14)0.0335 (3)
N40.59403 (18)0.26502 (19)0.25100 (17)0.0408 (4)
N50.6488 (2)0.3005 (2)0.1416 (2)0.0602 (5)
N60.7094 (4)0.3445 (3)0.0305 (3)0.0953 (9)
N70.64453 (19)0.08553 (19)0.46262 (15)0.0421 (4)
N80.75848 (18)0.17766 (18)0.43475 (15)0.0372 (4)
N90.8692 (2)0.2657 (2)0.4075 (2)0.0667 (6)
C10.7811 (2)0.0665 (3)0.13284 (19)0.0485 (5)
H10.82980.00200.15100.058*
C20.8729 (3)0.1755 (3)0.0671 (2)0.0585 (6)
H20.98120.18070.04140.070*
C30.8009 (3)0.2758 (3)0.0405 (2)0.0635 (7)
H30.86060.35170.00230.076*
C40.6395 (3)0.2644 (3)0.0773 (2)0.0556 (6)
H40.58880.33100.05870.067*
C50.5548 (2)0.1511 (2)0.14271 (17)0.0405 (4)
C60.3794 (2)0.1270 (2)0.18594 (19)0.0429 (5)
H6A0.33010.03370.13190.051*
H6B0.34090.21310.17720.051*
C70.3822 (2)0.2636 (2)0.4120 (2)0.0431 (5)
H7A0.35840.24610.49850.052*
H7B0.49560.29740.39060.052*
C80.3039 (3)0.3935 (3)0.4132 (3)0.0678 (7)
H8A0.19140.36110.43200.102*
H8B0.33630.48230.47820.102*
H8C0.33450.41930.33040.102*
C90.1681 (2)0.0495 (2)0.3533 (2)0.0417 (4)
H9A0.13430.07490.44610.050*
H9B0.10960.09710.31590.050*
C100.1294 (2)0.1228 (2)0.30508 (17)0.0339 (4)
C110.0239 (2)0.1986 (2)0.29585 (19)0.0432 (5)
H110.10320.14300.30970.052*
C120.0577 (2)0.3576 (3)0.2658 (2)0.0499 (5)
H120.16060.41050.26180.060*
C130.0626 (3)0.4366 (2)0.2420 (2)0.0497 (5)
H130.04240.54390.22310.060*
C140.2132 (2)0.3542 (2)0.2468 (2)0.0422 (5)
H140.29510.40800.22650.051*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.02806 (16)0.03521 (16)0.03230 (16)0.00054 (11)0.00843 (11)0.01207 (11)
N10.0411 (9)0.0418 (9)0.0341 (8)0.0000 (7)0.0060 (7)0.0120 (7)
N20.0367 (8)0.0314 (8)0.0337 (8)0.0023 (6)0.0103 (6)0.0078 (6)
N30.0331 (8)0.0339 (8)0.0353 (8)0.0007 (6)0.0120 (6)0.0108 (6)
N40.0299 (8)0.0506 (10)0.0415 (9)0.0157 (7)0.0015 (7)0.0074 (8)
N50.0528 (12)0.0460 (11)0.0880 (17)0.0103 (9)0.0229 (12)0.0160 (11)
N60.117 (2)0.0869 (18)0.0745 (17)0.0413 (17)0.0034 (16)0.0039 (14)
N70.0392 (9)0.0495 (10)0.0357 (9)0.0103 (8)0.0134 (7)0.0176 (7)
N80.0343 (9)0.0413 (9)0.0350 (8)0.0034 (8)0.0072 (7)0.0096 (7)
N90.0529 (12)0.0653 (13)0.0658 (13)0.0207 (11)0.0055 (10)0.0218 (11)
C10.0417 (12)0.0578 (13)0.0386 (11)0.0025 (10)0.0031 (9)0.0090 (9)
C20.0488 (13)0.0725 (16)0.0356 (11)0.0113 (11)0.0004 (10)0.0084 (11)
C30.0737 (17)0.0604 (15)0.0398 (12)0.0247 (13)0.0076 (11)0.0204 (11)
C40.0759 (17)0.0481 (12)0.0418 (11)0.0069 (11)0.0152 (11)0.0219 (10)
C50.0509 (12)0.0394 (10)0.0289 (9)0.0027 (9)0.0117 (8)0.0103 (8)
C60.0513 (12)0.0439 (11)0.0389 (10)0.0043 (9)0.0168 (9)0.0154 (9)
C70.0483 (12)0.0328 (10)0.0471 (11)0.0039 (8)0.0156 (9)0.0048 (8)
C80.0824 (18)0.0372 (12)0.0875 (19)0.0145 (12)0.0279 (15)0.0069 (12)
C90.0348 (10)0.0414 (11)0.0471 (11)0.0086 (8)0.0081 (8)0.0055 (9)
C100.0336 (10)0.0394 (10)0.0293 (9)0.0034 (8)0.0088 (7)0.0093 (7)
C110.0309 (10)0.0556 (12)0.0419 (11)0.0034 (9)0.0095 (8)0.0108 (9)
C120.0383 (11)0.0559 (13)0.0500 (12)0.0118 (10)0.0149 (9)0.0157 (10)
C130.0552 (13)0.0375 (11)0.0564 (13)0.0089 (9)0.0223 (11)0.0160 (9)
C140.0455 (11)0.0352 (10)0.0502 (12)0.0026 (8)0.0188 (9)0.0128 (9)
Geometric parameters (Å, º) top
Mn1—N12.3180 (16)C3—H30.930
Mn1—N22.3728 (15)C4—C51.388 (3)
Mn1—N32.2617 (15)C4—H40.930
Mn1—N42.1832 (17)C5—C61.497 (3)
Mn1—N72.2226 (16)C6—H6A0.970
Mn1—N7i2.2628 (16)C6—H6B0.970
N1—C11.337 (3)C7—C81.517 (3)
N1—C51.339 (3)C7—H7A0.970
N2—C91.464 (2)C7—H7B0.970
N2—C61.475 (2)C8—H8A0.960
N2—C71.489 (2)C8—H8B0.960
N3—C101.340 (2)C8—H8C0.960
N3—C141.341 (2)C9—C101.505 (3)
N4—N51.170 (3)C9—H9A0.970
N5—N61.210 (3)C9—H9B0.970
N7—N81.186 (2)C10—C111.384 (3)
N7—Mn1i2.2628 (16)C11—C121.378 (3)
N8—N91.145 (2)C11—H110.930
C1—C21.377 (3)C12—C131.372 (3)
C1—H10.930C12—H120.930
C2—C31.366 (4)C13—C141.372 (3)
C2—H20.930C13—H130.930
C3—C41.381 (4)C14—H140.930
N1—Mn1—N272.88 (6)C5—C4—H4120.8
N1—Mn1—N3108.85 (6)N1—C5—C4122.0 (2)
N1—Mn1—N491.00 (6)N1—C5—C6115.01 (16)
N1—Mn1—N788.39 (6)C4—C5—C6123.0 (2)
N1—Mn1—N7i157.36 (6)N2—C6—C5110.34 (15)
N2—Mn1—N372.11 (5)N2—C6—H6A109.6
N2—Mn1—N4151.84 (6)C5—C6—H6A109.6
N2—Mn1—N7100.79 (6)N2—C6—H6B109.6
N2—Mn1—N7i94.86 (6)C5—C6—H6B109.6
N3—Mn1—N492.46 (6)H6A—C6—H6B108.1
N3—Mn1—N7157.59 (6)N2—C7—C8116.23 (17)
N3—Mn1—N7i84.29 (6)N2—C7—H7A108.2
N4—Mn1—N7101.69 (7)C8—C7—H7A108.2
N4—Mn1—N7i107.18 (6)N2—C7—H7B108.2
N7—Mn1—N7i75.02 (6)C8—C7—H7B108.2
C1—N1—C5118.35 (17)H7A—C7—H7B107.4
C1—N1—Mn1123.68 (14)C7—C8—H8A109.5
C5—N1—Mn1115.35 (13)C7—C8—H8B109.5
C9—N2—C6110.21 (15)H8A—C8—H8B109.5
C9—N2—C7111.61 (15)C7—C8—H8C109.5
C6—N2—C7112.05 (15)H8A—C8—H8C109.5
C9—N2—Mn1108.09 (11)H8B—C8—H8C109.5
C6—N2—Mn1105.39 (11)N2—C9—C10112.97 (15)
C7—N2—Mn1109.23 (11)N2—C9—H9A109.0
C10—N3—C14118.12 (16)C10—C9—H9A109.0
C10—N3—Mn1117.57 (12)N2—C9—H9B109.0
C14—N3—Mn1122.89 (12)C10—C9—H9B109.0
N5—N4—Mn1123.86 (15)H9A—C9—H9B107.8
N4—N5—N6175.6 (2)N3—C10—C11121.75 (17)
N8—N7—Mn1127.53 (13)N3—C10—C9117.10 (16)
N8—N7—Mn1i126.22 (13)C11—C10—C9121.02 (17)
Mn1—N7—Mn1i104.98 (6)C12—C11—C10119.25 (19)
N9—N8—N7179.5 (2)C12—C11—H11120.4
N1—C1—C2123.0 (2)C10—C11—H11120.4
N1—C1—H1118.5C13—C12—C11119.06 (19)
C2—C1—H1118.5C13—C12—H12120.5
C3—C2—C1118.3 (2)C11—C12—H12120.5
C3—C2—H2120.8C14—C13—C12118.69 (19)
C1—C2—H2120.8C14—C13—H13120.7
C2—C3—C4120.0 (2)C12—C13—H13120.7
C2—C3—H3120.0N3—C14—C13123.02 (19)
C4—C3—H3120.0N3—C14—H14118.5
C3—C4—C5118.3 (2)C13—C14—H14118.5
C3—C4—H4120.8
N4—Mn1—N1—C147.77 (16)N1—Mn1—N7—N83.26 (18)
N7—Mn1—N1—C153.90 (16)N2—Mn1—N7—N875.50 (18)
N3—Mn1—N1—C1140.71 (15)N4—Mn1—N7—Mn1i104.88 (8)
N7i—Mn1—N1—C196.2 (2)N3—Mn1—N7—Mn1i23.17 (19)
N2—Mn1—N1—C1155.70 (17)N7i—Mn1—N7—Mn1i0.0
N4—Mn1—N1—C5150.93 (13)N1—Mn1—N7—Mn1i164.43 (7)
N7—Mn1—N1—C5107.41 (14)N2—Mn1—N7—Mn1i92.19 (7)
N3—Mn1—N1—C557.99 (14)C5—N1—C1—C21.7 (3)
N7i—Mn1—N1—C565.1 (2)Mn1—N1—C1—C2159.13 (16)
N2—Mn1—N1—C55.60 (13)N1—C1—C2—C30.1 (3)
N4—Mn1—N2—C988.86 (16)C1—C2—C3—C41.2 (3)
N7—Mn1—N2—C9128.67 (12)C2—C3—C4—C50.9 (3)
N3—Mn1—N2—C929.36 (11)C1—N1—C5—C41.9 (3)
N7i—Mn1—N2—C953.03 (12)Mn1—N1—C5—C4160.42 (15)
N1—Mn1—N2—C9146.41 (12)C1—N1—C5—C6178.05 (17)
N4—Mn1—N2—C628.97 (18)Mn1—N1—C5—C619.6 (2)
N7—Mn1—N2—C6113.49 (11)C3—C4—C5—N10.7 (3)
N3—Mn1—N2—C688.47 (12)C3—C4—C5—C6179.31 (19)
N7i—Mn1—N2—C6170.86 (11)C9—N2—C6—C5164.70 (15)
N1—Mn1—N2—C628.57 (11)C7—N2—C6—C570.4 (2)
N4—Mn1—N2—C7149.52 (14)Mn1—N2—C6—C548.31 (17)
N7—Mn1—N2—C77.06 (13)N1—C5—C6—N247.7 (2)
N3—Mn1—N2—C7150.98 (13)C4—C5—C6—N2132.29 (19)
N7i—Mn1—N2—C768.59 (12)C9—N2—C7—C861.9 (2)
N1—Mn1—N2—C791.98 (12)C6—N2—C7—C862.2 (2)
N4—Mn1—N3—C10176.61 (13)Mn1—N2—C7—C8178.59 (17)
N7—Mn1—N3—C1053.9 (2)C6—N2—C9—C1078.8 (2)
N7i—Mn1—N3—C1076.36 (13)C7—N2—C9—C10156.05 (16)
N1—Mn1—N3—C1084.71 (13)Mn1—N2—C9—C1035.92 (18)
N2—Mn1—N3—C1020.63 (12)C14—N3—C10—C111.6 (3)
N4—Mn1—N3—C1417.25 (15)Mn1—N3—C10—C11168.38 (14)
N7—Mn1—N3—C14112.24 (19)C14—N3—C10—C9174.46 (17)
N7i—Mn1—N3—C1489.77 (15)Mn1—N3—C10—C97.6 (2)
N1—Mn1—N3—C14109.15 (15)N2—C9—C10—N320.8 (2)
N2—Mn1—N3—C14173.23 (16)N2—C9—C10—C11163.19 (17)
N7—Mn1—N4—N5113.73 (18)N3—C10—C11—C123.4 (3)
N3—Mn1—N4—N583.75 (18)C9—C10—C11—C12172.47 (18)
N7i—Mn1—N4—N5168.53 (17)C10—C11—C12—C131.9 (3)
N1—Mn1—N4—N525.17 (18)C11—C12—C13—C141.1 (3)
N2—Mn1—N4—N528.6 (2)C10—N3—C14—C131.7 (3)
N4—Mn1—N7—N887.43 (18)Mn1—N3—C14—C13164.33 (15)
N3—Mn1—N7—N8144.52 (16)C12—C13—C14—N33.1 (3)
N7i—Mn1—N7—N8167.7 (2)
Symmetry code: (i) x+1, y, z+1.
 

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