Literature DB >> 21587392

catena-Poly[[(tetra-hydro-furan-κO)lithium(I)]-bis-(μ-trimethyl-silanolato-κO:O)-gallium(III)-bis-(μ-trimethyl-silanolato-κO:O)-[(tetra-hydro-furan-κO)lithium(I)]-μ-bromido].

Rafał Grubba1, Katarzyna Baranowska, Jerzy Pikies.   

Abstract

The title chain polymer compound, [GaLi(2)Br(C(3)H(9)OSi)(4)(C(4)H(8)O)(2)](n), was obtained in the reaction of GaBr(3) with Me(3)SiOLi in toluene/tetra-hydro-furan. The Ga(III) atom, located on a twofold rotation axis, is coordinated by four trimethyl-silanolate ligands and has a distorted tetra-hedral geometry. The Li(I) atom is four coordinated by one bridging Br atom located on an inversion centre, two trimethyl-silanolate ligands and one tetra-hydro-furane mol-ecule in a distorted tetra-hedral geometry. The polymeric chains extend along [001]. The tetra-hydro-furane mol-ecule is disordered over two positions with site-occupancy factors of 0.57 (2) and 0.43 (2).

Entities:  

Year:  2010        PMID: 21587392      PMCID: PMC2983186          DOI: 10.1107/S1600536810035518

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For the structures of similar compounds, see: Wheatley (1963 ▶); Barry & Richeson (1994 ▶); Chisholm et al. (2001 ▶). For the properties of GaBr, see: Dohmeier et al. (1996 ▶).

Experimental

Crystal data

[GaLi2Br(C3H9OSi)4(C4H8O)2] M = 664.49 Monoclinic, a = 25.802 (8) Å b = 9.761 (2) Å c = 18.689 (6) Å β = 130.81 (2)° V = 3563 (2) Å3 Z = 4 Mo Kα radiation μ = 2.06 mm−1 T = 150 K 0.2 × 0.18 × 0.09 mm

Data collection

Stoe Stadi IPDS 2 diffractometer Absorption correction: numerical (X-RED32; Stoe & Cie, 2008 ▶) T min = 0.503, T max = 0.734 19442 measured reflections 3098 independent reflections 2926 reflections with I > 2σ(I) R int = 0.080

Refinement

R[F 2 > 2σ(F 2)] = 0.031 wR(F 2) = 0.084 S = 1.05 3098 reflections 199 parameters H-atom parameters constrained Δρmax = 0.44 e Å−3 Δρmin = −0.60 e Å−3 Data collection: IPDS (Stoe & Cie, 2008 ▶); cell refinement: IPDS; data reduction: X-RED32 (Stoe & Cie, 2008 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810035518/is2596sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810035518/is2596Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[GaLi2Br(C3H9OSi)4(C4H8O)2]F(000) = 1392
Mr = 664.49Dx = 1.239 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 29109 reflections
a = 25.802 (8) Åθ = 1.4–25.0°
b = 9.761 (2) ŵ = 2.06 mm1
c = 18.689 (6) ÅT = 150 K
β = 130.81 (2)°Prism, colourless
V = 3563 (2) Å30.2 × 0.18 × 0.09 mm
Z = 4
Stoe Stadi IPDS 2 diffractometer3098 independent reflections
Radiation source: fine-focus sealed tube2926 reflections with I > 2σ(I)
graphiteRint = 0.080
Detector resolution: 6.67 pixels mm-1θmax = 25.0°, θmin = 2.2°
ω scanh = −30→30
Absorption correction: numerical (X-RED32; Stoe & Cie, 2008)k = −11→11
Tmin = 0.503, Tmax = 0.734l = −22→22
19442 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.084H-atom parameters constrained
S = 1.05w = 1/[σ2(Fo2) + (0.0478P)2 + 2.5155P] where P = (Fo2 + 2Fc2)/3
3098 reflections(Δ/σ)max < 0.001
199 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = −0.59 e Å3
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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.
xyzUiso*/UeqOcc. (<1)
Br10000.1153 (3)
Ga100.08220 (2)0.250.02639 (11)
Si10.11720 (3)−0.13978 (6)0.32580 (5)0.04353 (16)
Si2−0.08944 (3)0.28619 (7)0.07510 (4)0.04904 (18)
O10.06525 (7)−0.01375 (13)0.26059 (9)0.0343 (3)
O2−0.02655 (7)0.18106 (14)0.14841 (9)0.0366 (3)
O30.12462 (10)0.19275 (18)0.19590 (15)0.0616 (5)
C10.11245 (16)−0.2675 (3)0.2482 (3)0.0730 (8)
H1A0.124−0.22330.21310.109*
H1B0.0659−0.30490.20360.109*
H1C0.1449−0.34190.28690.109*
C20.20664 (14)−0.0753 (4)0.4125 (2)0.0775 (9)
H2A0.2116−0.01860.45990.116*
H2B0.2171−0.02030.37950.116*
H2C0.2383−0.1530.44370.116*
C30.09372 (16)−0.2196 (3)0.3913 (2)0.0759 (9)
H3A0.0489−0.26390.34650.114*
H3B0.0917−0.1490.42670.114*
H3C0.1282−0.28830.43540.114*
C5−0.15978 (19)0.1939 (5)−0.0340 (2)0.1035 (14)
H5A−0.17460.1167−0.01770.155*
H5B−0.14360.1598−0.06570.155*
H5C−0.19840.2565−0.07630.155*
C4−0.0577 (2)0.4234 (4)0.0441 (3)0.0990 (13)
H4A−0.04660.38460.00720.149*
H4B−0.01650.46480.10210.149*
H4C−0.09320.49370.00660.149*
C6−0.12074 (18)0.3621 (3)0.1317 (2)0.0776 (9)
H6A−0.08330.41190.18870.116*
H6B−0.1370.2890.14870.116*
H6C−0.15840.42540.08740.116*
Li10.0429 (2)0.0908 (4)0.1507 (3)0.0437 (8)
C70.1816 (6)0.1116 (11)0.2192 (8)0.064 (2)0.57 (2)
H7A0.21950.1080.28850.077*0.57 (2)
H7B0.16650.01690.19510.077*0.57 (2)
C80.2033 (6)0.1793 (15)0.1742 (11)0.092 (4)0.57 (2)
H8A0.25290.16550.21060.11*0.57 (2)
H8B0.17760.14480.10910.11*0.57 (2)
C90.1886 (8)0.3183 (16)0.1736 (15)0.102 (5)0.57 (2)
H9A0.17990.36720.12030.123*0.57 (2)
H9B0.22710.36350.23350.123*0.57 (2)
C100.1277 (9)0.3169 (18)0.1630 (13)0.102 (5)0.57 (2)
H10A0.12950.39310.19950.123*0.57 (2)
H10B0.08640.32890.09560.123*0.57 (2)
C7A0.1685 (12)0.126 (2)0.187 (2)0.125 (8)0.43 (2)
H7C0.14210.07470.12680.15*0.43 (2)
H7D0.19920.06110.24030.15*0.43 (2)
C8A0.2101 (9)0.247 (4)0.1900 (10)0.146 (15)0.43 (2)
H8C0.25960.23740.24540.175*0.43 (2)
H8D0.2040.24730.13190.175*0.43 (2)
C9A0.1826 (8)0.375 (2)0.1970 (14)0.110 (8)0.43 (2)
H9C0.18130.44930.16020.132*0.43 (2)
H9D0.21060.40410.26370.132*0.43 (2)
C10A0.1110 (9)0.336 (2)0.1559 (9)0.076 (4)0.43 (2)
H10C0.09370.39710.17850.091*0.43 (2)
H10D0.07840.33550.0860.091*0.43 (2)
U11U22U33U12U13U23
Br10.1081 (4)0.1890 (7)0.0632 (3)−0.0066 (4)0.0623 (3)−0.0435 (4)
Ga10.02674 (16)0.02626 (16)0.02663 (16)00.01764 (13)0
Si10.0344 (3)0.0407 (3)0.0561 (4)0.0103 (2)0.0299 (3)0.0130 (3)
Si20.0548 (4)0.0490 (3)0.0400 (3)0.0205 (3)0.0295 (3)0.0161 (3)
O10.0327 (7)0.0349 (6)0.0390 (7)0.0039 (5)0.0251 (6)0.0045 (5)
O20.0420 (7)0.0371 (7)0.0338 (7)0.0091 (6)0.0261 (6)0.0076 (5)
O30.0746 (12)0.0558 (9)0.0834 (13)−0.0096 (9)0.0644 (11)0.0009 (9)
C10.0711 (18)0.0480 (13)0.115 (2)0.0111 (13)0.0675 (19)−0.0024 (15)
C20.0367 (13)0.092 (2)0.075 (2)0.0094 (13)0.0240 (14)0.0147 (16)
C30.0673 (17)0.0797 (19)0.091 (2)0.0280 (15)0.0563 (18)0.0480 (17)
C50.072 (2)0.118 (3)0.0516 (17)0.026 (2)0.0097 (16)−0.0016 (18)
C40.137 (4)0.076 (2)0.121 (3)0.044 (2)0.101 (3)0.057 (2)
C60.082 (2)0.082 (2)0.0751 (19)0.0426 (17)0.0540 (18)0.0226 (16)
Li10.051 (2)0.0485 (19)0.0458 (19)0.0031 (15)0.0378 (18)0.0035 (15)
C70.046 (3)0.068 (4)0.076 (4)−0.003 (3)0.038 (3)0.002 (3)
C80.056 (5)0.108 (8)0.126 (9)−0.001 (5)0.066 (6)0.017 (6)
C90.088 (8)0.102 (11)0.123 (12)−0.003 (7)0.072 (9)0.038 (8)
C100.112 (10)0.063 (5)0.182 (13)0.018 (6)0.118 (11)0.042 (6)
C7A0.084 (12)0.167 (14)0.17 (2)0.014 (10)0.103 (14)0.016 (13)
C8A0.077 (10)0.31 (4)0.058 (6)−0.118 (19)0.047 (6)−0.039 (14)
C9A0.063 (8)0.116 (13)0.079 (8)−0.044 (8)0.015 (6)0.038 (8)
C10A0.059 (7)0.079 (10)0.060 (6)−0.020 (6)0.027 (5)0.019 (5)
Br1—Li12.422 (4)C5—H5A0.98
Br1—Li1i2.422 (4)C5—H5B0.98
Ga1—O2ii1.8180 (14)C5—H5C0.98
Ga1—O21.8180 (14)C4—H4A0.98
Ga1—O1ii1.8207 (13)C4—H4B0.98
Ga1—O11.8207 (13)C4—H4C0.98
Ga1—Li1ii2.713 (3)C6—H6A0.98
Ga1—Li12.713 (3)C6—H6B0.98
Si1—O11.6310 (14)C6—H6C0.98
Si1—C11.855 (3)C7—C81.441 (18)
Si1—C31.855 (3)C7—H7A0.99
Si1—C21.860 (3)C7—H7B0.99
Si2—O21.6301 (14)C8—C91.41 (2)
Si2—C41.850 (3)C8—H8A0.99
Si2—C51.851 (4)C8—H8B0.99
Si2—C61.853 (3)C9—C101.45 (2)
O1—Li12.011 (4)C9—H9A0.99
O2—Li11.972 (4)C9—H9B0.99
O3—C101.385 (17)C10—H10A0.99
O3—C7A1.41 (2)C10—H10B0.99
O3—C71.463 (14)C7A—C8A1.58 (3)
O3—C10A1.513 (19)C7A—H7C0.99
O3—Li11.955 (4)C7A—H7D0.99
C1—H1A0.98C8A—C9A1.48 (3)
C1—H1B0.98C8A—H8C0.99
C1—H1C0.98C8A—H8D0.99
C2—H2A0.98C9A—C10A1.51 (2)
C2—H2B0.98C9A—H9C0.99
C2—H2C0.98C9A—H9D0.99
C3—H3A0.98C10A—H10C0.99
C3—H3B0.98C10A—H10D0.99
C3—H3C0.98
Li1—Br1—Li1i180.00 (12)H4A—C4—H4B109.5
O2ii—Ga1—O2115.88 (9)Si2—C4—H4C109.5
O2ii—Ga1—O1ii94.42 (6)H4A—C4—H4C109.5
O2—Ga1—O1ii117.97 (7)H4B—C4—H4C109.5
O2ii—Ga1—O1117.97 (7)Si2—C6—H6A109.5
O2—Ga1—O194.42 (6)Si2—C6—H6B109.5
O1ii—Ga1—O1118.09 (8)H6A—C6—H6B109.5
O2ii—Ga1—Li1ii46.60 (9)Si2—C6—H6C109.5
O2—Ga1—Li1ii130.87 (9)H6A—C6—H6C109.5
O1ii—Ga1—Li1ii47.83 (9)H6B—C6—H6C109.5
O1—Ga1—Li1ii134.67 (9)O3—Li1—O2119.32 (19)
O2ii—Ga1—Li1130.87 (9)O3—Li1—O1108.0 (2)
O2—Ga1—Li146.60 (9)O2—Li1—O184.19 (14)
O1ii—Ga1—Li1134.67 (9)O3—Li1—Br1103.47 (15)
O1—Ga1—Li147.83 (9)O2—Li1—Br1114.85 (18)
Li1ii—Ga1—Li1176.47 (15)O1—Li1—Br1127.60 (17)
O1—Si1—C1108.71 (12)O3—Li1—Ga1121.79 (17)
O1—Si1—C3110.29 (10)O2—Li1—Ga142.05 (7)
C1—Si1—C3110.49 (15)O1—Li1—Ga142.14 (7)
O1—Si1—C2109.97 (12)Br1—Li1—Ga1134.71 (16)
C1—Si1—C2108.59 (15)C8—C7—O3106.1 (8)
C3—Si1—C2108.77 (16)C8—C7—H7A110.5
O2—Si2—C4108.53 (14)O3—C7—H7A110.5
O2—Si2—C5109.90 (14)C8—C7—H7B110.5
C4—Si2—C5108.9 (2)O3—C7—H7B110.5
O2—Si2—C6109.74 (11)H7A—C7—H7B108.7
C4—Si2—C6109.66 (17)C9—C8—C7104.0 (12)
C5—Si2—C6110.09 (18)C9—C8—H8A111
Si1—O1—Ga1135.98 (8)C7—C8—H8A111
Si1—O1—Li1133.87 (13)C9—C8—H8B111
Ga1—O1—Li190.02 (11)C7—C8—H8B111
Si2—O2—Ga1134.48 (8)H8A—C8—H8B109
Si2—O2—Li1133.68 (12)C8—C9—C10104.8 (12)
Ga1—O2—Li191.34 (11)C8—C9—H9A110.8
C10—O3—C7A94.2 (11)C10—C9—H9A110.8
C10—O3—C7105.5 (8)C8—C9—H9B110.8
C7A—O3—C10A108.6 (12)C10—C9—H9B110.8
C7—O3—C10A120.7 (10)H9A—C9—H9B108.9
C10—O3—Li1127.8 (7)O3—C10—C9108.6 (12)
C7A—O3—Li1115.8 (9)O3—C10—H10A110
C7—O3—Li1116.3 (4)C9—C10—H10A110
C10A—O3—Li1114.8 (7)O3—C10—H10B110
Si1—C1—H1A109.5C9—C10—H10B110
Si1—C1—H1B109.5H10A—C10—H10B108.3
H1A—C1—H1B109.5O3—C7A—C8A103.3 (18)
Si1—C1—H1C109.5O3—C7A—H7C111.1
H1A—C1—H1C109.5C8A—C7A—H7C111.1
H1B—C1—H1C109.5O3—C7A—H7D111.1
Si1—C2—H2A109.5C8A—C7A—H7D111.1
Si1—C2—H2B109.5H7C—C7A—H7D109.1
H2A—C2—H2B109.5C9A—C8A—C7A106.1 (14)
Si1—C2—H2C109.5C9A—C8A—H8C110.5
H2A—C2—H2C109.5C7A—C8A—H8C110.5
H2B—C2—H2C109.5C9A—C8A—H8D110.5
Si1—C3—H3A109.5C7A—C8A—H8D110.5
Si1—C3—H3B109.5H8C—C8A—H8D108.7
H3A—C3—H3B109.5C8A—C9A—C10A104.0 (13)
Si1—C3—H3C109.5C8A—C9A—H9C111
H3A—C3—H3C109.5C10A—C9A—H9C111
H3B—C3—H3C109.5C8A—C9A—H9D111
Si2—C5—H5A109.5C10A—C9A—H9D111
Si2—C5—H5B109.5H9C—C9A—H9D109
H5A—C5—H5B109.5O3—C10A—C9A99.6 (12)
Si2—C5—H5C109.5O3—C10A—H10C111.9
H5A—C5—H5C109.5C9A—C10A—H10C111.9
H5B—C5—H5C109.5O3—C10A—H10D111.9
Si2—C4—H4A109.5C9A—C10A—H10D111.9
Si2—C4—H4B109.5H10C—C10A—H10D109.6
C1—Si1—O1—Ga1132.69 (14)Si2—O2—Li1—O1−171.36 (12)
C3—Si1—O1—Ga111.41 (19)Ga1—O2—Li1—O11.13 (11)
C2—Si1—O1—Ga1−108.54 (17)Si2—O2—Li1—Br1−42.4 (3)
C1—Si1—O1—Li1−41.9 (2)Ga1—O2—Li1—Br1130.09 (14)
C3—Si1—O1—Li1−163.2 (2)Si2—O2—Li1—Ga1−172.49 (19)
C2—Si1—O1—Li176.8 (2)Si1—O1—Li1—O3−65.9 (2)
O2ii—Ga1—O1—Si162.64 (14)Ga1—O1—Li1—O3117.85 (16)
O2—Ga1—O1—Si1−174.90 (12)Si1—O1—Li1—O2175.13 (12)
O1ii—Ga1—O1—Si1−49.84 (10)Ga1—O1—Li1—O2−1.13 (11)
Li1ii—Ga1—O1—Si17.31 (19)Si1—O1—Li1—Br158.1 (3)
Li1—Ga1—O1—Si1−176.12 (19)Ga1—O1—Li1—Br1−118.2 (2)
O2ii—Ga1—O1—Li1−121.24 (13)Si1—O1—Li1—Ga1176.26 (18)
O2—Ga1—O1—Li11.22 (12)O2ii—Ga1—Li1—O311.3 (3)
O1ii—Ga1—O1—Li1126.28 (12)O2—Ga1—Li1—O3100.0 (2)
Li1ii—Ga1—O1—Li1−176.57 (15)O1ii—Ga1—Li1—O3−171.58 (13)
C4—Si2—O2—Ga1143.96 (18)O1—Ga1—Li1—O3−81.7 (2)
C5—Si2—O2—Ga1−97.1 (2)O2ii—Ga1—Li1—O2−88.64 (16)
C6—Si2—O2—Ga124.14 (19)O1ii—Ga1—Li1—O288.45 (14)
C4—Si2—O2—Li1−46.6 (2)O1—Ga1—Li1—O2178.32 (17)
C5—Si2—O2—Li172.4 (2)O2ii—Ga1—Li1—O193.04 (13)
C6—Si2—O2—Li1−166.4 (2)O2—Ga1—Li1—O1−178.32 (17)
O2ii—Ga1—O2—Si2−64.78 (11)O1ii—Ga1—Li1—O1−89.87 (16)
O1ii—Ga1—O2—Si245.99 (14)O2ii—Ga1—Li1—Br1−166.26 (14)
O1—Ga1—O2—Si2171.14 (12)O2—Ga1—Li1—Br1−77.6 (2)
Li1ii—Ga1—O2—Si2−10.94 (19)O1ii—Ga1—Li1—Br110.8 (3)
Li1—Ga1—O2—Si2172.39 (19)O1—Ga1—Li1—Br1100.7 (2)
O2ii—Ga1—O2—Li1122.83 (13)C10—O3—C7—C8−15.5 (15)
O1ii—Ga1—O2—Li1−126.40 (13)C7A—O3—C7—C839 (3)
O1—Ga1—O2—Li1−1.25 (13)C10A—O3—C7—C8−14.6 (13)
Li1ii—Ga1—O2—Li1176.67 (14)Li1—O3—C7—C8132.3 (9)
C10—O3—Li1—O2−56.0 (10)O3—C7—C8—C930.4 (14)
C7A—O3—Li1—O2−174.4 (14)C7—C8—C9—C10−33.0 (18)
C7—O3—Li1—O2164.5 (6)C7A—O3—C10—C9−20 (2)
C10A—O3—Li1—O2−46.6 (9)C7—O3—C10—C9−5.1 (18)
C10—O3—Li1—O1−149.4 (10)C10A—O3—C10—C9178 (6)
C7A—O3—Li1—O192.1 (15)Li1—O3—C10—C9−147.9 (12)
C7—O3—Li1—O171.0 (6)C8—C9—C10—O324 (2)
C10A—O3—Li1—O1−140.1 (8)C10—O3—C7A—C8A22.8 (19)
C10—O3—Li1—Br173.1 (10)C7—O3—C7A—C8A−105 (4)
C7A—O3—Li1—Br1−45.4 (15)C10A—O3—C7A—C8A28 (2)
C7—O3—Li1—Br1−66.4 (6)Li1—O3—C7A—C8A158.7 (10)
C10A—O3—Li1—Br182.5 (8)O3—C7A—C8A—C9A−2(2)
C10—O3—Li1—Ga1−105.1 (10)C7A—C8A—C9A—C10A−24.0 (16)
C7A—O3—Li1—Ga1136.4 (14)C10—O3—C10A—C9A−23 (4)
C7—O3—Li1—Ga1115.3 (6)C7A—O3—C10A—C9A−42.8 (19)
C10A—O3—Li1—Ga1−95.8 (8)C7—O3—C10A—C9A−26.8 (14)
Si2—O2—Li1—O381.3 (3)Li1—O3—C10A—C9A−174.2 (11)
Ga1—O2—Li1—O3−106.2 (2)C8A—C9A—C10A—O339.0 (15)
  2 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Siloxide and triflate gallium(III) complexes supported by the BDI ligand.

Authors:  M H Chisholm; D Navarro-Llobet; J Gallucci
Journal:  Inorg Chem       Date:  2001-12-03       Impact factor: 5.165

  2 in total

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