fac-[Bis(2-pyridylmeth­yl)amine-κ³N]tribromo­indium(III)

In the title compound, fac-[InBr₃{NH(CH₂C₅H₄N)₂}], the In^III atom is coordinated by three bromide ligands and a tridentate bis­(2-pyridylmeth­yl)amine ligand. A mirror plane passes through the In atom, one Br atom and central NH group. The mol­ecule exhibits facial octa­hedral stereochemistry, with In—Br bond lengths of 2.5682 (13) and 2.6060 (9) Å, and In—N bond lengths of 2.311 (6) and 2.328 (9) Å.

Key indicators

• Single-crystal X-ray study
• T = 203 K
• Mean [sigma](C-C) = 0.012 Å
• R factor = 0.053
• wR factor = 0.125
• Data-to-parameter ratio = 20.2

checkCIF/PLATON results

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Alert level C
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         12

   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
   0 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
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: CrystalClear (Rigaku, 2001); cell refinement: CrystalClear; data reduction: TEXSAN (Molecular Structure Corporation, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

(I)

Crystal data

[InBr3(C12H13N3)]	F(000) = 1040
Mr = 553.80	Dx = 2.319 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ac 2n	Cell parameters from 5462 reflections
a = 13.995 (2) Å	θ = 4.1–27.5°
b = 14.227 (2) Å	µ = 9.04 mm^−1
c = 7.9682 (12) Å	T = 203 K
V = 1586.6 (4) Å^3	Plate, colorless
Z = 4	0.12 × 0.06 × 0.02 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer	1802 reflections with I > 2σ(I)
Detector resolution: 14.6199 pixels mm^-1	Rint = 0.056
ω scans	θmax = 27.5°, θmin = 4.1°
Absorption correction: multi-scan (Jacobson, 1998)	h = −15→18
Tmin = 0.410, Tmax = 0.840	k = −18→16
14768 measured reflections	l = −10→10
1877 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.053	w = 1/[σ^2(Fo^2) + (0.05P)^2 + 3P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.125	(Δ/σ)max < 0.001
S = 1.01	Δρmax = 0.84 e Å^−3
1877 reflections	Δρmin = −0.69 e Å^−3
93 parameters

Special details

Experimental. ¹H NMR (400 MHz, DMSO-d₆): δ 4.16 (d, J = 16.8 Hz, 2H, CH₂), 4.64 (d, J = 16.8 Hz, 1H, CH₂), 4.66 (d, J = 16.8 Hz, 1H, CH₂), 6.42 (s, 1H, NH), 7.50 (br, 2H, py), 7.55 (br, 2H, py), 7.97 (br, 2H, py), 8.88 (br, 2H, py); ¹³C NMR (100.4 MHz, DMSO-d₆): δ 51.32 (s, CH₂), 124.61 (s, 2 C, CH), 140.55 (s, CH), 144.72 (s, CH), 151.69 (s, ipso-C); elemental analysis found: C 25.65, H 2.22, N 7.16%; calculated for C₁₂H₁₃Br₃InN₃: C 26.03, H 2.37, N 7.59%.

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
In1	0.87159 (5)	0.2500	0.70375 (9)	0.01798 (19)
Br1	1.01642 (8)	0.2500	0.90168 (14)	0.0305 (3)
Br2	0.77399 (6)	0.38912 (6)	0.82974 (10)	0.0291 (2)
N1	0.7668 (6)	0.2500	0.4769 (11)	0.0201 (17)
H1N	0.707 (9)	0.2500	0.521 (16)	0.024*
N2	0.9383 (4)	0.1506 (4)	0.5066 (8)	0.0203 (12)
C1	0.7813 (5)	0.1617 (5)	0.3776 (10)	0.0261 (16)
H1A	0.7429	0.1112	0.4272	0.031*
H1B	0.7587	0.1718	0.2626	0.031*
C2	0.8837 (5)	0.1319 (5)	0.3730 (9)	0.0224 (15)
C3	0.9204 (7)	0.0843 (6)	0.2343 (11)	0.0319 (18)
H3A	0.8814	0.0713	0.1410	0.038*
C4	1.0142 (7)	0.0567 (6)	0.2364 (10)	0.0321 (18)
H4A	1.0399	0.0245	0.1438	0.038*
C5	1.0710 (6)	0.0760 (5)	0.3734 (10)	0.0268 (16)
H5A	1.1352	0.0567	0.3766	0.032*
C6	1.0304 (5)	0.1248 (5)	0.5068 (10)	0.0227 (15)
H6A	1.0687	0.1401	0.5998	0.027*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
In1	0.0137 (3)	0.0230 (3)	0.0172 (3)	0.000	0.0003 (3)	0.000
Br1	0.0205 (6)	0.0476 (7)	0.0234 (6)	0.000	−0.0061 (4)	0.000
Br2	0.0218 (4)	0.0328 (4)	0.0326 (4)	0.0034 (3)	0.0039 (3)	−0.0083 (3)
N1	0.013 (4)	0.023 (4)	0.024 (4)	0.000	0.001 (3)	0.000
N2	0.021 (3)	0.019 (3)	0.021 (3)	−0.003 (2)	0.002 (2)	0.003 (2)
C1	0.019 (4)	0.027 (4)	0.032 (4)	−0.005 (3)	−0.009 (3)	−0.005 (3)
C2	0.021 (4)	0.024 (3)	0.022 (3)	0.000 (3)	−0.004 (3)	0.005 (3)
C3	0.039 (5)	0.032 (4)	0.024 (4)	0.002 (4)	−0.003 (3)	−0.006 (3)
C4	0.043 (5)	0.034 (4)	0.019 (4)	−0.001 (4)	0.009 (3)	−0.004 (3)
C5	0.021 (4)	0.027 (4)	0.032 (4)	0.001 (3)	0.005 (3)	0.000 (3)
C6	0.017 (3)	0.024 (4)	0.027 (4)	−0.001 (3)	−0.002 (3)	0.003 (3)

Geometric parameters (Å, º)

In1—N1	2.328 (9)	C1—C2	1.496 (10)
In1—N2	2.311 (6)	C1—H1A	0.9800
In1—N2^i	2.311 (6)	C1—H1B	0.9800
In1—Br1	2.5682 (13)	C2—C3	1.394 (11)
In1—Br2	2.6060 (9)	C3—C4	1.370 (13)
In1—Br2^i	2.6060 (9)	C3—H3A	0.9400
N1—C1^i	1.498 (9)	C4—C5	1.378 (12)
N1—C1	1.498 (9)	C4—H4A	0.9400
N1—H1N	0.91 (13)	C5—C6	1.391 (11)
N2—C2	1.336 (9)	C5—H5A	0.9400
N2—C6	1.341 (9)	C6—H6A	0.9400
N1—In1—N2	74.1 (2)	C6—N2—In1	123.7 (5)
N2—In1—N2^i	75.5 (3)	C2—C1—N1	112.4 (6)
N2^i—In1—N1	74.1 (2)	C2—C1—H1A	109.1
N2—In1—Br1	95.67 (16)	N1—C1—H1A	109.1
N2^i—In1—Br1	95.67 (16)	C2—C1—H1B	109.1
N1—In1—Br1	166.9 (2)	N1—C1—H1B	109.1
N2—In1—Br2	159.80 (16)	H1A—C1—H1B	107.9
N2^i—In1—Br2	90.49 (14)	N2—C2—C3	121.2 (7)
N1—In1—Br2	88.21 (14)	N2—C2—C1	118.1 (7)
Br1—In1—Br2	100.20 (3)	C3—C2—C1	120.7 (7)
N2—In1—Br2^i	90.49 (14)	C4—C3—C2	118.8 (8)
N2^i—In1—Br2^i	159.80 (16)	C4—C3—H3A	120.6
N1—In1—Br2^i	88.21 (14)	C2—C3—H3A	120.6
Br1—In1—Br2^i	100.20 (3)	C3—C4—C5	120.4 (8)
Br2—In1—Br2^i	98.84 (4)	C3—C4—H4A	119.8
C1^i—N1—C1	113.9 (9)	C5—C4—H4A	119.8
C1^i—N1—In1	108.9 (5)	C4—C5—C6	118.0 (7)
C1—N1—In1	108.9 (5)	C4—C5—H5A	121.0
C1^i—N1—H1N	109 (4)	C6—C5—H5A	121.0
C1—N1—H1N	109 (4)	N2—C6—C5	121.9 (7)
In1—N1—H1N	106 (8)	N2—C6—H6A	119.1
C2—N2—C6	119.7 (7)	C5—C6—H6A	119.1
C2—N2—In1	115.6 (5)
N2—In1—N1—C1^i	−101.9 (6)	Br2—In1—N2—C6	131.6 (5)
N2^i—In1—N1—C1^i	−22.9 (5)	Br2^i—In1—N2—C6	−110.5 (5)
Br1—In1—N1—C1^i	−62.4 (5)	C1^i—N1—C1—C2	85.9 (9)
Br2—In1—N1—C1^i	68.1 (5)	In1—N1—C1—C2	−35.9 (8)
Br2^i—In1—N1—C1^i	167.0 (5)	C6—N2—C2—C3	1.3 (11)
N2—In1—N1—C1	22.9 (5)	In1—N2—C2—C3	170.7 (6)
N2^i—In1—N1—C1	101.9 (6)	C6—N2—C2—C1	179.9 (6)
Br1—In1—N1—C1	62.4 (5)	In1—N2—C2—C1	−10.7 (8)
Br2—In1—N1—C1	−167.0 (5)	N1—C1—C2—N2	32.4 (10)
Br2^i—In1—N1—C1	−68.1 (5)	N1—C1—C2—C3	−149.0 (7)
N2^i—In1—N2—C2	−84.6 (5)	N2—C2—C3—C4	−0.2 (12)
N1—In1—N2—C2	−7.4 (5)	C1—C2—C3—C4	−178.8 (8)
Br1—In1—N2—C2	−179.1 (5)	C2—C3—C4—C5	0.0 (13)
Br2—In1—N2—C2	−37.3 (8)	C3—C4—C5—C6	−0.7 (12)
Br2^i—In1—N2—C2	80.6 (5)	C2—N2—C6—C5	−2.1 (11)
N2^i—In1—N2—C6	84.3 (6)	In1—N2—C6—C5	−170.6 (5)
N1—In1—N2—C6	161.5 (6)	C4—C5—C6—N2	1.9 (11)
Br1—In1—N2—C6	−10.2 (6)

Symmetry code: (i) x, −y+1/2, z.