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The title complex, [Cr(C17H33NOSi2)(CO)3], has the typical three-legged piano-stool structure expected for η6-arenetri­carbonyl­chromium compounds. The conformation is staggered with respect to the methoxy group of the arene ring and one of the carbonyl ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805006008/hb6159sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805006008/hb6159Isup2.hkl
Contains datablock I

CCDC reference: 270327

Key indicators

  • Single-crystal X-ray study
  • T = 110 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.033
  • wR factor = 0.084
  • Data-to-parameter ratio = 22.8

checkCIF/PLATON results

No syntax errors found



Alert level C WEIGH01_ALERT_1_C Extra text has been found in the _refine_ls_weighting_scheme field. This should be in the _refine_ls_weighting_details field. Weighting scheme given as calc w = 1/[\s^2^(Fo^2^)+(0.0411P)^2^] where Weighting scheme identified as calc PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.75 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.50 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for O3 - C3 .. 5.97 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cr1 - C1 .. 7.22 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cr1 - C2 .. 5.50 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cr1 - C3 .. 8.52 su
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.34 From the CIF: _reflns_number_total 5984 Count of symmetry unique reflns 3406 Completeness (_total/calc) 175.69% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2578 Fraction of Friedel pairs measured 0.757 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1990); software used to prepare material for publication: SHELXL97.

Tricarbonyl[η6-(S,S)-1-[2-methoxy-3,6-bis(trimethylsilyl)phenyl]-N,N- dimethylethylamine]chromium(0) top
Crystal data top
[Cr(C17H33NOSi2)(CO)3]F(000) = 976
Mr = 459.65Dx = 1.269 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 8096 reflections
a = 7.1361 (12) Åθ = 1.6–28.3°
b = 17.251 (3) ŵ = 0.60 mm1
c = 19.541 (3) ÅT = 110 K
V = 2405.7 (7) Å3Rod, yellow
Z = 40.44 × 0.03 × 0.03 mm
Data collection top
Bruker SMART APEX CCD
diffractometer
5984 independent reflections
Radiation source: fine-focus sealed tube5037 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.071
ω scansθmax = 28.3°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 99
Tmin = 0.779, Tmax = 0.982k = 2222
33064 measured reflectionsl = 2626
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033H-atom parameters constrained
wR(F2) = 0.084Calculated w = 1/[σ2(Fo2) + (0.0411P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.92(Δ/σ)max = 0.001
5984 reflectionsΔρmax = 0.38 e Å3
263 parametersΔρmin = 0.28 e Å3
0 restraintsAbsolute structure: Flack (1983), 2578 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.006 (18)
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
Cr10.98443 (5)0.45762 (2)0.84988 (2)0.01594 (10)
Si11.17726 (11)0.27393 (4)0.78356 (4)0.02093 (17)
C30.8465 (4)0.54734 (16)0.85956 (13)0.0229 (6)
C10.9031 (4)0.45942 (18)0.75998 (14)0.0257 (6)
O10.8477 (3)0.46077 (14)0.70419 (10)0.0418 (6)
O30.7551 (3)0.60341 (11)0.86346 (10)0.0352 (5)
O41.0690 (2)0.30018 (10)0.93887 (8)0.0167 (4)
C1110.8744 (3)0.46147 (16)1.03395 (13)0.0199 (5)
H11A0.83880.45761.08230.026*
H11B0.79030.42931.00630.026*
H11C0.86490.51561.01910.026*
C1121.0769 (3)0.43323 (14)1.02488 (13)0.0151 (5)
H1121.08160.37881.03920.020*
O20.6397 (3)0.36598 (13)0.88574 (10)0.0345 (5)
C1081.1403 (3)0.43711 (13)0.94965 (12)0.0135 (5)
C1071.2075 (3)0.50808 (14)0.91974 (12)0.0154 (5)
C1041.2014 (3)0.36392 (14)0.84005 (12)0.0160 (5)
N1.2153 (3)0.47627 (12)1.06621 (10)0.0162 (4)
C20.7720 (4)0.40155 (16)0.87113 (13)0.0243 (6)
C1061.2772 (3)0.50371 (14)0.85110 (13)0.0172 (5)
H1061.32990.55040.82990.022*
C1141.1591 (4)0.48355 (16)1.13858 (12)0.0236 (6)
H11D1.04720.51631.14190.031*
H11E1.26140.50721.16480.031*
H11F1.13140.43201.15720.031*
C1091.1403 (3)0.36762 (14)0.90924 (12)0.0145 (5)
C1011.2286 (5)0.30497 (16)0.69358 (14)0.0318 (7)
H10A1.35940.32180.69030.041*
H10B1.14570.34800.68100.041*
H10C1.20750.26130.66240.041*
C1030.9352 (4)0.23323 (18)0.78814 (14)0.0316 (7)
H10D0.84870.26730.76330.041*
H10E0.89620.22950.83610.041*
H10F0.93350.18150.76740.041*
C1101.2124 (4)0.25447 (15)0.97172 (13)0.0219 (6)
H11G1.32550.25430.94320.028*
H11H1.16750.20120.97770.028*
H11I1.24170.27691.01650.028*
C1051.2723 (3)0.43419 (14)0.81309 (12)0.0172 (5)
H1051.32010.43460.76610.022*
C1131.3967 (3)0.43617 (15)1.06444 (13)0.0204 (6)
H11J1.43960.43191.01700.027*
H11K1.38290.38421.08410.027*
H11L1.48860.46561.09110.027*
C1021.3528 (5)0.19796 (17)0.80738 (16)0.0372 (8)
H10G1.36220.15970.77040.048*
H10H1.31290.17210.84960.048*
H10I1.47540.22230.81460.048*
Si21.23779 (10)0.60869 (4)0.96241 (4)0.01796 (15)
C1151.4685 (4)0.61550 (15)1.00738 (13)0.0248 (6)
H11M1.50840.66981.00920.032*
H11N1.56220.58500.98250.032*
H11O1.45580.59521.05400.032*
C1161.2506 (5)0.67954 (15)0.88914 (14)0.0281 (6)
H11P1.24510.73260.90700.036*
H11Q1.14480.67080.85810.036*
H11R1.36840.67210.86420.036*
C1171.0440 (4)0.64717 (15)1.01782 (14)0.0241 (6)
H11S1.03260.61501.05890.031*
H11T0.92580.64600.99230.031*
H11U1.07250.70071.03110.031*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0155 (2)0.01745 (19)0.01493 (18)0.00097 (18)0.00227 (17)0.00342 (17)
Si10.0294 (4)0.0177 (4)0.0158 (4)0.0003 (3)0.0012 (3)0.0003 (3)
C30.0228 (13)0.0263 (14)0.0197 (13)0.0021 (13)0.0030 (11)0.0027 (12)
C10.0209 (13)0.0318 (15)0.0244 (14)0.0034 (13)0.0005 (11)0.0030 (13)
O10.0365 (12)0.0668 (16)0.0220 (11)0.0052 (13)0.0087 (9)0.0041 (11)
O30.0327 (11)0.0291 (11)0.0437 (13)0.0150 (10)0.0011 (10)0.0034 (10)
O40.0183 (9)0.0148 (9)0.0169 (9)0.0015 (7)0.0028 (7)0.0038 (7)
C1110.0152 (12)0.0234 (13)0.0210 (13)0.0026 (11)0.0004 (10)0.0007 (12)
C1120.0165 (12)0.0131 (12)0.0156 (12)0.0003 (10)0.0008 (10)0.0003 (10)
O20.0199 (11)0.0421 (13)0.0416 (13)0.0063 (10)0.0052 (9)0.0160 (10)
C1080.0116 (11)0.0143 (12)0.0146 (12)0.0022 (9)0.0031 (9)0.0009 (9)
C1070.0124 (12)0.0157 (12)0.0180 (13)0.0006 (10)0.0017 (10)0.0015 (10)
C1040.0154 (12)0.0169 (12)0.0157 (12)0.0012 (10)0.0017 (10)0.0007 (10)
N0.0149 (10)0.0202 (11)0.0137 (10)0.0009 (9)0.0002 (8)0.0012 (8)
C20.0216 (14)0.0274 (15)0.0240 (14)0.0009 (13)0.0063 (11)0.0078 (12)
C1060.0150 (12)0.0167 (12)0.0199 (12)0.0013 (10)0.0011 (11)0.0042 (11)
C1140.0246 (14)0.0308 (15)0.0155 (13)0.0018 (12)0.0020 (11)0.0042 (11)
C1090.0099 (11)0.0155 (12)0.0181 (12)0.0006 (10)0.0031 (10)0.0032 (10)
C1010.053 (2)0.0226 (15)0.0202 (14)0.0036 (15)0.0048 (14)0.0045 (12)
C1030.0401 (18)0.0327 (17)0.0220 (15)0.0094 (14)0.0048 (13)0.0016 (13)
C1100.0241 (15)0.0181 (13)0.0234 (14)0.0025 (11)0.0004 (11)0.0052 (11)
C1050.0146 (12)0.0220 (13)0.0149 (12)0.0017 (10)0.0001 (10)0.0028 (10)
C1130.0161 (13)0.0246 (14)0.0207 (13)0.0026 (11)0.0048 (10)0.0002 (11)
C1020.050 (2)0.0285 (17)0.0328 (17)0.0128 (15)0.0065 (16)0.0111 (14)
Si20.0197 (4)0.0150 (3)0.0192 (4)0.0006 (3)0.0015 (3)0.0007 (3)
C1150.0235 (15)0.0214 (14)0.0296 (15)0.0055 (12)0.0030 (12)0.0008 (11)
C1160.0387 (17)0.0172 (13)0.0282 (15)0.0046 (13)0.0065 (14)0.0014 (11)
C1170.0240 (16)0.0185 (13)0.0299 (15)0.0030 (11)0.0006 (12)0.0022 (11)
Geometric parameters (Å, º) top
Cr1—C31.844 (3)C106—C1051.411 (3)
Cr1—C21.846 (3)C106—H1060.9800
Cr1—C11.850 (3)C114—H11D0.9801
Cr1—C1052.214 (3)C114—H11E0.9801
Cr1—C1092.235 (2)C114—H11F0.9801
Cr1—C1062.236 (2)C101—H10A0.9801
Cr1—C1042.246 (2)C101—H10B0.9801
Cr1—C1072.270 (2)C101—H10C0.9801
Cr1—C1082.272 (2)C103—H10D0.9801
Si1—C1031.867 (3)C103—H10E0.9801
Si1—C1021.872 (3)C103—H10F0.9801
Si1—C1011.874 (3)C110—H11G0.9801
Si1—C1041.913 (3)C110—H11H0.9801
C3—O31.169 (3)C110—H11I0.9801
C1—O11.160 (3)C105—H1050.9800
O4—C1091.396 (3)C113—H11J0.9801
O4—C1101.443 (3)C113—H11K0.9801
C111—C1121.535 (3)C113—H11L0.9801
C111—H11A0.9801C102—H10G0.9801
C111—H11B0.9801C102—H10H0.9801
C111—H11C0.9801C102—H10I0.9801
C112—N1.476 (3)Si2—C1151.870 (3)
C112—C1081.540 (3)Si2—C1171.877 (3)
C112—H1120.9800Si2—C1161.885 (3)
O2—C21.162 (3)C115—H11M0.9801
C108—C1091.435 (3)C115—H11N0.9801
C108—C1071.439 (3)C115—H11O0.9801
C107—C1061.433 (3)C116—H11P0.9801
C107—Si21.938 (3)C116—H11Q0.9801
C104—C1051.415 (3)C116—H11R0.9801
C104—C1091.422 (3)C117—H11S0.9801
N—C1131.468 (3)C117—H11T0.9801
N—C1141.475 (3)C117—H11U0.9801
C3—Cr1—C288.76 (12)C105—C106—C107121.9 (2)
C3—Cr1—C185.17 (12)C105—C106—Cr170.67 (14)
C2—Cr1—C187.98 (12)C107—C106—Cr172.78 (13)
C3—Cr1—C105133.00 (11)C105—C106—H106119.0
C2—Cr1—C105137.70 (11)C107—C106—H106119.0
C1—Cr1—C10589.19 (10)Cr1—C106—H106130.2
C3—Cr1—C109142.72 (10)N—C114—H11D109.5
C2—Cr1—C10985.86 (10)N—C114—H11E109.5
C1—Cr1—C109131.35 (11)H11D—C114—H11E109.5
C105—Cr1—C10965.16 (9)N—C114—H11F109.5
C3—Cr1—C106101.50 (10)H11D—C114—H11F109.5
C2—Cr1—C106162.11 (10)H11E—C114—H11F109.5
C1—Cr1—C106107.30 (11)O4—C109—C104118.0 (2)
C105—Cr1—C10636.97 (9)O4—C109—C108117.9 (2)
C109—Cr1—C10677.08 (9)C104—C109—C108124.1 (2)
C3—Cr1—C104168.71 (10)O4—C109—Cr1127.82 (16)
C2—Cr1—C104102.01 (11)C104—C109—Cr171.95 (13)
C1—Cr1—C10498.45 (11)C108—C109—Cr172.87 (13)
C105—Cr1—C10437.00 (9)Si1—C101—H10A109.5
C109—Cr1—C10437.01 (8)Si1—C101—H10B109.5
C106—Cr1—C10467.22 (9)H10A—C101—H10B109.5
C3—Cr1—C10789.48 (10)Si1—C101—H10C109.5
C2—Cr1—C107129.91 (10)H10A—C101—H10C109.5
C1—Cr1—C107141.65 (11)H10B—C101—H10C109.5
C105—Cr1—C10767.33 (9)Si1—C103—H10D109.5
C109—Cr1—C10766.76 (9)Si1—C103—H10E109.5
C106—Cr1—C10737.07 (9)H10D—C103—H10E109.5
C104—Cr1—C10781.04 (9)Si1—C103—H10F109.5
C3—Cr1—C108107.71 (10)H10D—C103—H10F109.5
C2—Cr1—C10897.33 (10)H10E—C103—H10F109.5
C1—Cr1—C108166.09 (10)O4—C110—H11G109.5
C105—Cr1—C10878.22 (9)O4—C110—H11H109.5
C109—Cr1—C10837.13 (8)H11G—C110—H11H109.5
C106—Cr1—C10865.71 (9)O4—C110—H11I109.5
C104—Cr1—C10867.91 (9)H11G—C110—H11I109.5
C107—Cr1—C10836.93 (8)H11H—C110—H11I109.5
C103—Si1—C102110.13 (15)C106—C105—C104122.7 (2)
C103—Si1—C101109.48 (14)C106—C105—Cr172.35 (14)
C102—Si1—C101107.61 (15)C104—C105—Cr172.75 (14)
C103—Si1—C104111.14 (12)C106—C105—H105118.6
C102—Si1—C104111.38 (12)C104—C105—H105118.6
C101—Si1—C104106.98 (12)Cr1—C105—H105128.7
O3—C3—Cr1177.4 (2)N—C113—H11J109.5
O1—C1—Cr1178.3 (2)N—C113—H11K109.5
C109—O4—C110112.43 (18)H11J—C113—H11K109.5
C112—C111—H11A109.5N—C113—H11L109.5
C112—C111—H11B109.5H11J—C113—H11L109.5
H11A—C111—H11B109.5H11K—C113—H11L109.5
C112—C111—H11C109.5Si1—C102—H10G109.5
H11A—C111—H11C109.5Si1—C102—H10H109.5
H11B—C111—H11C109.5H10G—C102—H10H109.5
N—C112—C111114.0 (2)Si1—C102—H10I109.5
N—C112—C108107.70 (19)H10G—C102—H10I109.5
C111—C112—C108111.9 (2)H10H—C102—H10I109.5
N—C112—H112107.7C115—Si2—C117110.81 (12)
C111—C112—H112107.7C115—Si2—C116105.88 (13)
C108—C112—H112107.7C117—Si2—C116104.16 (13)
C109—C108—C107119.2 (2)C115—Si2—C107110.90 (11)
C109—C108—C112119.3 (2)C117—Si2—C107118.86 (12)
C107—C108—C112121.5 (2)C116—Si2—C107105.03 (11)
C109—C108—Cr170.00 (13)Si2—C115—H11M109.5
C107—C108—Cr171.46 (13)Si2—C115—H11N109.5
C112—C108—Cr1133.00 (16)H11M—C115—H11N109.5
C106—C107—C108116.8 (2)Si2—C115—H11O109.5
C106—C107—Si2114.29 (17)H11M—C115—H11O109.5
C108—C107—Si2128.66 (18)H11N—C115—H11O109.5
C106—C107—Cr170.15 (13)Si2—C116—H11P109.5
C108—C107—Cr171.61 (13)Si2—C116—H11Q109.5
Si2—C107—Cr1132.88 (12)H11P—C116—H11Q109.5
C105—C104—C109115.2 (2)Si2—C116—H11R109.5
C105—C104—Si1120.83 (18)H11P—C116—H11R109.5
C109—C104—Si1123.89 (18)H11Q—C116—H11R109.5
C105—C104—Cr170.26 (14)Si2—C117—H11S109.5
C109—C104—Cr171.04 (13)Si2—C117—H11T109.5
Si1—C104—Cr1124.86 (12)H11S—C117—H11T109.5
C113—N—C114107.59 (19)Si2—C117—H11U109.5
C113—N—C112109.87 (19)H11S—C117—H11U109.5
C114—N—C112112.7 (2)H11T—C117—H11U109.5
O2—C2—Cr1178.7 (2)
 

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