Literature DB >> 22589862

trans-Bis[(2-bromo-phen-yl)diphenyl-phosphane-κP]carbonyl-chlorido-rhodium(I).

Frederick P Malan1, Rehana Malgas-Enus, Reinout Meijboom.   

Abstract

The title compound, trans-[RhCl(C(18)H(14)BrP)(2)(CO)], has a slightly disordered square-planar geometry with the Rh ion(I) situated on an inversion the centre and carbon-yl-chloride disorder observed as a result of the crystallographic inversion symmetry. Selected geometric parameters include: Rh-P = 2.3430 (8) Å, Rh-Cl = 2.434 (3) Å, Rh-C = 1.722 (8) Å, P-Rh-P = 180.00 (3)°, P-Rh-Cl = 95.40 (7)°, 84.60 (7)° and Rh-C-O = 177.9 (8)°.

Entities:  

Year:  2012        PMID： 22589862      PMCID： PMC3343894          DOI： 10.1107/S1600536812012421

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


Related literature

For background to Vaska-type complexes, see: Roodt et al. (2003 ▶); Lamb et al. (2009 ▶); Vaska & Di Luzio (1961 ▶). For related complexes, see: Burgoyne et al. (2010 ▶); Makhoba et al. (2011 ▶); Meijboom (2011 ▶); Meijboom et al. (2004 ▶); Otto et al. (2000 ▶); Otto & Roodt (2004 ▶); Chen et al. (1991 ▶); Kemp et al. (1995 ▶).

Experimental

Crystal data

[RhCl(C18H14BrP)2(CO)] M = 848.71 Monoclinic, a = 9.3250 (5) Å b = 17.041 (1) Å c = 10.8880 (6) Å β = 111.229 (1)° V = 1612.77 (16) Å3 Z = 2 Mo Kα radiation μ = 3.22 mm−1 T = 100 K 0.23 × 0.13 × 0.11 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T min = 0.618, T max = 0.697 15235 measured reflections 4032 independent reflections 3531 reflections with I > 2σ(I) R int = 0.026

Refinement

R[F 2 > 2σ(F 2)] = 0.027 wR(F 2) = 0.063 S = 1.11 4032 reflections 214 parameters H-atom parameters constrained Δρmax = 0.67 e Å−3 Δρmin = −0.81 e Å−3 Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg & Putz (2005 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812012421/hp2033sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812012421/hp2033Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[RhCl(C18H14BrP)2(CO)]F(000) = 840
Mr = 848.71Dx = 1.748 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ynCell parameters from 6197 reflections
a = 9.3250 (5) Åθ = 2.4–28.3°
b = 17.041 (1) ŵ = 3.22 mm−1
c = 10.8880 (6) ÅT = 100 K
β = 111.229 (1)°Rectangular, yellow
V = 1612.77 (16) Å30.23 × 0.13 × 0.11 mm
Z = 2
Bruker APEXII CCD diffractometer3531 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
φ and ω scansθmax = 28.4°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −12→12
Tmin = 0.618, Tmax = 0.697k = −22→22
15235 measured reflectionsl = −14→14
4032 independent 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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.063H-atom parameters constrained
S = 1.11w = 1/[σ2(Fo2) + (0.0246P)2 + 1.6443P] where P = (Fo2 + 2Fc2)/3
4032 reflections(Δ/σ)max = 0.001
214 parametersΔρmax = 0.67 e Å−3
0 restraintsΔρmin = −0.81 e Å−3
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.
xyzUiso*/UeqOcc. (<1)
Rh10.5010.01378 (7)
C10.5773 (7)−0.0478 (4)0.8993 (6)0.0178 (11)0.5
O10.6340 (10)−0.0800 (5)0.8343 (9)0.0236 (17)0.5
Cl10.6037 (3)−0.06666 (16)0.8527 (3)0.0174 (4)0.5
P10.50550 (6)0.11189 (4)0.87674 (5)0.01442 (12)
Br10.13942 (3)0.061590 (16)0.75242 (2)0.02135 (7)
C70.4960 (3)0.09681 (15)0.6146 (2)0.0189 (5)
H70.60060.10830.64840.023*
C20.4152 (3)0.09234 (14)0.7000 (2)0.0156 (4)
C80.4165 (3)0.20586 (14)0.8906 (2)0.0164 (5)
C120.3697 (3)0.30670 (16)1.0277 (3)0.0269 (6)
H120.3790.32481.11080.032*
C140.7017 (3)0.14283 (14)0.9010 (2)0.0174 (5)
C190.8252 (3)0.09824 (16)0.9810 (2)0.0237 (5)
H190.80690.05271.020.028*
C150.7317 (3)0.21089 (16)0.8434 (3)0.0255 (5)
H150.65040.24180.79080.031*
C180.9756 (3)0.12109 (19)1.0032 (3)0.0314 (6)
H181.05740.09141.05820.038*
C110.2947 (3)0.35167 (16)0.9183 (3)0.0263 (6)
H110.25290.39990.92750.032*
C40.1846 (3)0.06291 (15)0.5096 (2)0.0215 (5)
H40.07970.05230.4750.026*
C60.4238 (3)0.08449 (16)0.4807 (2)0.0231 (5)
H60.48030.08690.42590.028*
C171.0033 (3)0.18774 (18)0.9436 (3)0.0326 (7)
H171.10390.20250.9570.039*
C90.3404 (3)0.25267 (16)0.7805 (2)0.0233 (5)
H90.32920.23480.69680.028*
C30.2589 (3)0.07322 (14)0.6440 (2)0.0169 (5)
C50.2675 (3)0.06855 (15)0.4277 (2)0.0234 (5)
H50.21870.06170.33740.028*
C130.4314 (3)0.23448 (15)1.0149 (2)0.0220 (5)
H130.48310.20491.08970.026*
C100.2816 (3)0.32529 (16)0.7949 (3)0.0274 (6)
H100.23320.35630.72130.033*
C160.8815 (3)0.23287 (17)0.8639 (3)0.0306 (6)
H160.90050.2780.82410.037*
U11U22U33U12U13U23
Rh10.01221 (11)0.01690 (13)0.01105 (11)−0.00151 (9)0.00278 (9)0.00207 (10)
C10.021 (3)0.017 (3)0.015 (3)0.000 (2)0.007 (2)0.004 (2)
O10.024 (4)0.027 (4)0.026 (3)0.008 (2)0.017 (2)0.001 (2)
Cl10.0204 (12)0.0177 (11)0.0171 (11)0.0033 (8)0.0105 (7)0.0011 (8)
P10.0130 (3)0.0175 (3)0.0124 (3)−0.0011 (2)0.0041 (2)0.0022 (2)
Br10.01558 (11)0.03052 (15)0.01759 (12)−0.00259 (9)0.00558 (9)0.00252 (10)
C70.0188 (11)0.0208 (12)0.0185 (11)0.0022 (9)0.0085 (9)0.0024 (9)
C20.0193 (11)0.0150 (11)0.0129 (10)0.0016 (9)0.0063 (9)0.0014 (9)
C80.0139 (10)0.0191 (12)0.0164 (11)−0.0030 (9)0.0059 (9)−0.0013 (9)
C120.0326 (14)0.0271 (14)0.0274 (13)−0.0124 (11)0.0187 (12)−0.0121 (11)
C140.0161 (10)0.0194 (12)0.0178 (11)−0.0036 (9)0.0074 (9)−0.0034 (9)
C190.0190 (11)0.0281 (14)0.0228 (12)−0.0024 (10)0.0062 (10)0.0010 (11)
C150.0279 (13)0.0192 (13)0.0335 (14)−0.0036 (10)0.0160 (11)−0.0032 (11)
C180.0156 (12)0.0410 (17)0.0350 (15)−0.0016 (11)0.0059 (11)−0.0044 (13)
C110.0250 (13)0.0190 (13)0.0393 (15)−0.0041 (10)0.0171 (12)−0.0081 (11)
C40.0219 (12)0.0214 (13)0.0171 (11)−0.0012 (10)0.0022 (9)0.0012 (10)
C60.0304 (13)0.0250 (14)0.0176 (12)0.0037 (11)0.0132 (10)0.0024 (10)
C170.0219 (13)0.0383 (17)0.0443 (17)−0.0140 (12)0.0201 (12)−0.0196 (14)
C90.0255 (12)0.0235 (13)0.0178 (11)0.0023 (10)0.0041 (10)−0.0032 (10)
C30.0195 (11)0.0169 (12)0.0151 (11)0.0016 (9)0.0070 (9)0.0023 (9)
C50.0320 (14)0.0247 (14)0.0122 (11)0.0004 (11)0.0064 (10)−0.0012 (10)
C130.0243 (12)0.0239 (13)0.0171 (11)−0.0075 (10)0.0067 (10)−0.0039 (10)
C100.0265 (13)0.0207 (13)0.0294 (14)0.0011 (11)0.0033 (11)−0.0015 (11)
C160.0345 (14)0.0236 (14)0.0440 (17)−0.0130 (12)0.0266 (13)−0.0107 (12)
Rh1—C1i1.720 (7)C19—C181.390 (3)
Rh1—C11.720 (7)C19—H190.93
Rh1—P12.3429 (6)C15—C161.384 (4)
Rh1—P1i2.3429 (6)C15—H150.93
Rh1—Cl1i2.433 (3)C18—C171.378 (4)
Rh1—Cl12.433 (3)C18—H180.93
C1—O11.163 (7)C11—C101.379 (4)
P1—C141.829 (2)C11—H110.93
P1—C21.831 (2)C4—C51.379 (4)
P1—C81.835 (2)C4—C31.385 (3)
Br1—C31.904 (2)C4—H40.93
C7—C61.383 (3)C6—C51.386 (4)
C7—C21.394 (3)C6—H60.93
C7—H70.93C17—C161.386 (4)
C2—C31.399 (3)C17—H170.93
C8—C131.397 (3)C9—C101.385 (4)
C8—C91.400 (3)C9—H90.93
C12—C111.375 (4)C5—H50.93
C12—C131.387 (4)C13—H130.93
C12—H120.93C10—H100.93
C14—C191.391 (3)C16—H160.93
C14—C151.394 (4)
C1i—Rh1—C1180.0000 (10)C18—C19—H19119.7
C1i—Rh1—P194.63 (19)C14—C19—H19119.7
C1—Rh1—P185.37 (19)C16—C15—C14120.5 (3)
C1i—Rh1—P1i85.37 (19)C16—C15—H15119.7
C1—Rh1—P1i94.63 (19)C14—C15—H15119.7
P1—Rh1—P1i180C17—C18—C19119.9 (3)
C1i—Rh1—Cl1i1.46 (18)C17—C18—H18120.1
C1—Rh1—Cl1i178.54 (19)C19—C18—H18120.1
P1—Rh1—Cl1i95.39 (7)C12—C11—C10120.0 (2)
P1i—Rh1—Cl1i84.61 (7)C12—C11—H11120
C1i—Rh1—Cl1178.54 (18)C10—C11—H11120
C1—Rh1—Cl11.46 (19)C5—C4—C3119.4 (2)
P1—Rh1—Cl184.61 (7)C5—C4—H4120.3
P1i—Rh1—Cl195.39 (7)C3—C4—H4120.3
Cl1i—Rh1—Cl1180.0000 (10)C7—C6—C5120.4 (2)
O1—C1—Rh1177.9 (8)C7—C6—H6119.8
C14—P1—C2105.04 (11)C5—C6—H6119.8
C14—P1—C8101.26 (11)C18—C17—C16120.1 (2)
C2—P1—C8101.29 (10)C18—C17—H17120
C14—P1—Rh1112.34 (8)C16—C17—H17120
C2—P1—Rh1110.92 (8)C10—C9—C8120.7 (2)
C8—P1—Rh1123.96 (8)C10—C9—H9119.7
C6—C7—C2121.3 (2)C8—C9—H9119.7
C6—C7—H7119.3C4—C3—C2122.2 (2)
C2—C7—H7119.3C4—C3—Br1117.41 (18)
C7—C2—C3116.8 (2)C2—C3—Br1120.34 (17)
C7—C2—P1122.46 (18)C4—C5—C6119.7 (2)
C3—C2—P1120.68 (17)C4—C5—H5120.1
C13—C8—C9118.2 (2)C6—C5—H5120.1
C13—C8—P1119.67 (19)C12—C13—C8120.5 (2)
C9—C8—P1122.05 (18)C12—C13—H13119.8
C11—C12—C13120.5 (2)C8—C13—H13119.8
C11—C12—H12119.8C11—C10—C9120.2 (3)
C13—C12—H12119.8C11—C10—H10119.9
C19—C14—C15118.7 (2)C9—C10—H10119.9
C19—C14—P1119.39 (19)C15—C16—C17120.1 (3)
C15—C14—P1121.86 (19)C15—C16—H16120
C18—C19—C14120.7 (3)C17—C16—H16120
C1i—Rh1—C1—O19E1 (10)Rh1—P1—C8—C9−141.23 (18)
P1—Rh1—C1—O110E1 (2)C2—P1—C14—C19−117.8 (2)
P1i—Rh1—C1—O1−8E1 (2)C8—P1—C14—C19137.1 (2)
Cl1i—Rh1—C1—O1−2E1 (3)Rh1—P1—C14—C192.8 (2)
Cl1—Rh1—C1—O116E1 (3)C2—P1—C14—C1563.4 (2)
C1i—Rh1—P1—C14113.6 (2)C8—P1—C14—C15−41.7 (2)
C1—Rh1—P1—C14−66.4 (2)Rh1—P1—C14—C15−175.97 (18)
P1i—Rh1—P1—C14−93.80 (10)C15—C14—C19—C180.1 (4)
Cl1i—Rh1—P1—C14112.34 (10)P1—C14—C19—C18−178.8 (2)
Cl1—Rh1—P1—C14−67.66 (10)C19—C14—C15—C161.0 (4)
C1i—Rh1—P1—C2−129.2 (2)P1—C14—C15—C16179.8 (2)
C1—Rh1—P1—C250.8 (2)C14—C19—C18—C17−1.3 (4)
P1i—Rh1—P1—C223.42 (13)C13—C12—C11—C10−0.5 (4)
Cl1i—Rh1—P1—C2−130.44 (10)C2—C7—C6—C51.1 (4)
Cl1—Rh1—P1—C249.56 (10)C19—C18—C17—C161.4 (4)
C1i—Rh1—P1—C8−8.5 (2)C13—C8—C9—C100.0 (4)
C1—Rh1—P1—C8171.5 (2)P1—C8—C9—C10−176.5 (2)
P1i—Rh1—P1—C8144.10 (13)C5—C4—C3—C22.6 (4)
Cl1i—Rh1—P1—C8−9.76 (11)C5—C4—C3—Br1−178.16 (19)
Cl1—Rh1—P1—C8170.24 (11)C7—C2—C3—C4−3.1 (4)
C6—C7—C2—C31.3 (4)P1—C2—C3—C4175.85 (19)
C6—C7—C2—P1−177.7 (2)C7—C2—C3—Br1177.59 (18)
C14—P1—C2—C74.1 (2)P1—C2—C3—Br1−3.4 (3)
C8—P1—C2—C7109.2 (2)C3—C4—C5—C6−0.1 (4)
Rh1—P1—C2—C7−117.49 (19)C7—C6—C5—C4−1.7 (4)
C14—P1—C2—C3−174.83 (19)C11—C12—C13—C8−0.9 (4)
C8—P1—C2—C3−69.8 (2)C9—C8—C13—C121.2 (4)
Rh1—P1—C2—C363.6 (2)P1—C8—C13—C12177.67 (19)
C14—P1—C8—C13−84.6 (2)C12—C11—C10—C91.6 (4)
C2—P1—C8—C13167.38 (19)C8—C9—C10—C11−1.3 (4)
Rh1—P1—C8—C1342.4 (2)C14—C15—C16—C17−0.9 (4)
C14—P1—C8—C991.8 (2)C18—C17—C16—C15−0.3 (4)
C2—P1—C8—C9−16.2 (2)
  4 in total

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Authors:  George M Sheldrick
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Authors:  Sizwe Makhoba; Alfred Muller; Reinout Meijboom; Bernard Omondi
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-08-27

3.  trans-Carbonyl-chloridobis[tris(naph-thalen-1-yl)-phosphane-κP]rhodium(I) acetone trisolvate.

Authors:  Reinout Meijboom
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-09-30

4.  trans-Carbonyl-chloridobis[tris-(4-chloro-phen-yl)phosphane]rhodium(I) acetone monosolvate.

Authors:  Andrew R Burgoyne; Reinout Meijboom; Alfred Muller; Bernard O Omondi
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-10-09
  4 in total

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