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The title compound, [Cu4(C9H11)4(C3H9P)2] or [Cu4(Mes)4(PMe3)2] (Mes = 2,4,6-tri­methyl­phenyl), was synthesized from copper(I) mesityl and tri­methyl­phosphane in THF as solvent. The mol­ecular structure of the complex has C2 symmetry and consists of four copper(I) atoms bridged by four μ-mesityl groups, giving an eight-membered puckered {Cu4C4} ring. Additionally, two copper(I) atoms at opposite corners of the Cu4 rhomb are each linked to a terminal PMe3 ligand. The PMe3-bearing copper(I) atoms exhibit a distorted trigonal–planar coordination mode whereas the remaining Cu atoms linked to two mesityl groups are nearly linearly coordinated.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314621005940/wm4146sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2414314621005940/wm4146Isup2.hkl
Contains datablock I

CCDC reference: 2088681

Key indicators

  • Single-crystal X-ray study
  • T = 213 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.033
  • wR factor = 0.100
  • Data-to-parameter ratio = 17.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of P Check PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L= 0.597 46 Report PLAT977_ALERT_2_C Check Negative Difference Density on H7A -0.35 eA-3 PLAT977_ALERT_2_C Check Negative Difference Density on H16C -0.35 eA-3
Alert level G PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large 5.63 Why ? PLAT343_ALERT_2_G Unusual sp? Angle Range in Main Residue for C1 Check PLAT343_ALERT_2_G Unusual sp? Angle Range in Main Residue for C10 Check PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety ..... C7 Check PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety ..... C8 Check PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety ..... C9 Check PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety ..... C16 Check PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety ..... C17 Check PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety ..... C18 Check PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio PLAT794_ALERT_5_G Tentative Bond Valency for Cu1 (I) . 0.44 Info PLAT794_ALERT_5_G Tentative Bond Valency for Cu2 (I) . 0.59 Info PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still 57% Note PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF .... 1 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 2 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 4 ALERT level C = Check. Ensure it is not caused by an omission or oversight 15 ALERT level G = General information/check it is not something unexpected 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check

Computing details top

Data collection: (X-AREA; Stoe & Cie, 2016); cell refinement: (X-AREA; Stoe & Cie, 2016); data reduction: (X-AREA; Stoe & Cie, 2016); program(s) used to solve structure: ShelXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

cyclo-Tetrakis(µ-2,4,6-trimethylphenyl-κC1:κC1)bis(trimethylphosphane)-1κP,3κP-tetracopper(I) top
Crystal data top
[Cu4(C9H11)4(C3H9P)2]F(000) = 1840
Mr = 883.01Dx = 1.346 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 12.0750 (8) ÅCell parameters from 10871 reflections
b = 27.5202 (18) Åθ = 1.5–25.6°
c = 14.3164 (9) ŵ = 2.03 mm1
β = 113.668 (5)°T = 213 K
V = 4357.3 (5) Å3Block, pale yellow
Z = 40.51 × 0.32 × 0.19 mm
Data collection top
Stoe IPDS 2
diffractometer
3043 reflections with I > 2σ(I)
rotation method scansRint = 0.050
Absorption correction: integration
(X-AREA; Stoe & Cie, 2016)
θmax = 25.1°, θmin = 1.5°
Tmin = 0.508, Tmax = 0.758h = 1413
10982 measured reflectionsk = 3231
3839 independent reflectionsl = 1717
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033H-atom parameters constrained
wR(F2) = 0.100 w = 1/[σ2(Fo2) + (0.0519P)2 + 5.6305P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max < 0.001
3839 reflectionsΔρmax = 0.48 e Å3
217 parametersΔρmin = 0.44 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.5285 (3)0.14472 (10)0.0734 (2)0.0352 (6)
C20.5698 (3)0.11189 (11)0.0184 (2)0.0406 (7)
C30.6133 (3)0.12859 (13)0.0520 (3)0.0535 (9)
H30.6379720.1061310.0882300.064*
C40.6210 (3)0.17740 (14)0.0697 (3)0.0567 (9)
C50.5825 (3)0.21013 (13)0.0155 (3)0.0542 (9)
H50.5872810.2432440.0263990.065*
C60.5369 (3)0.19478 (11)0.0549 (2)0.0422 (7)
C70.5670 (3)0.05827 (11)0.0365 (3)0.0530 (8)
H7A0.5347170.0526140.0868690.064*
H7B0.5168430.0424750.0260480.064*
H7C0.6475340.0454160.0602290.064*
C80.6704 (5)0.1944 (2)0.1462 (4)0.0953 (16)
H8A0.6692550.2292660.1488530.114*
H8B0.7519500.1830730.1258600.114*
H8C0.6212370.1816470.2123910.114*
C90.4929 (4)0.23236 (11)0.1078 (3)0.0564 (9)
H9A0.4642290.2166500.1537140.068*
H9B0.5580680.2539240.1454630.068*
H9C0.4282040.2505770.0580720.068*
C100.2575 (3)0.10497 (11)0.1661 (2)0.0362 (6)
C110.1633 (3)0.13739 (12)0.1595 (2)0.0428 (7)
C120.0481 (3)0.12024 (13)0.1414 (3)0.0525 (8)
H120.0114750.1423600.1382760.063*
C130.0193 (3)0.07129 (14)0.1277 (2)0.0531 (9)
C140.1118 (3)0.03930 (12)0.1352 (2)0.0490 (8)
H140.0949310.0062270.1265720.059*
C150.2281 (3)0.05497 (11)0.1551 (2)0.0390 (6)
C160.1869 (3)0.19137 (12)0.1699 (3)0.0605 (9)
H16A0.2698290.1975120.1821500.073*
H16B0.1351410.2073480.1081260.073*
H16C0.1706400.2036030.2259130.073*
C170.1068 (3)0.05407 (19)0.1057 (3)0.0798 (13)
H17A0.1102770.0193510.0985860.096*
H17B0.1285220.0631890.1608980.096*
H17C0.1622400.0686600.0436440.096*
C180.3221 (3)0.01757 (11)0.1617 (3)0.0517 (8)
H18A0.3979280.0334490.1757200.062*
H18B0.3312560.0050100.2153740.062*
H18C0.2970230.0004600.0980440.062*
C190.0817 (4)0.1129 (2)0.0945 (3)0.0864 (15)
H19A0.0736050.0836450.0611810.104*
H19B0.0529080.1399980.0685660.104*
H19C0.0351690.1099880.1666320.104*
C200.2658 (4)0.07802 (15)0.1540 (3)0.0816 (13)
H20A0.2703850.0460470.1258550.098*
H20B0.2003050.0793210.2200720.098*
H20C0.3403150.0853740.1601200.098*
C210.2352 (4)0.17798 (14)0.1387 (3)0.0667 (10)
H21A0.2217830.2048700.1017930.080*
H21B0.3106110.1823630.1452710.080*
H21C0.1706010.1763100.2052230.080*
P0.24013 (8)0.12219 (3)0.07038 (6)0.0456 (2)
Cu10.58712 (3)0.12496 (2)0.22033 (2)0.03340 (13)
Cu20.37473 (3)0.12434 (2)0.09729 (2)0.03274 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0323 (15)0.0399 (15)0.0349 (14)0.0001 (12)0.0150 (12)0.0030 (12)
C20.0351 (17)0.0472 (16)0.0426 (16)0.0017 (13)0.0190 (14)0.0047 (13)
C30.050 (2)0.073 (2)0.0488 (19)0.0064 (17)0.0318 (17)0.0115 (17)
C40.054 (2)0.077 (2)0.0462 (19)0.0117 (18)0.0282 (17)0.0040 (17)
C50.057 (2)0.0540 (19)0.053 (2)0.0120 (16)0.0234 (17)0.0129 (16)
C60.0404 (17)0.0453 (16)0.0400 (16)0.0012 (13)0.0152 (14)0.0047 (13)
C70.049 (2)0.0495 (18)0.072 (2)0.0015 (15)0.0367 (18)0.0122 (16)
C80.106 (4)0.126 (4)0.078 (3)0.030 (3)0.063 (3)0.006 (3)
C90.073 (2)0.0370 (16)0.067 (2)0.0041 (16)0.0358 (19)0.0051 (16)
C100.0283 (15)0.0459 (16)0.0339 (14)0.0003 (12)0.0119 (12)0.0013 (12)
C110.0336 (16)0.0562 (17)0.0378 (16)0.0050 (14)0.0137 (13)0.0015 (14)
C120.0307 (17)0.081 (2)0.0451 (18)0.0086 (16)0.0150 (14)0.0009 (16)
C130.0315 (17)0.086 (3)0.0418 (18)0.0104 (16)0.0144 (14)0.0045 (17)
C140.0411 (18)0.063 (2)0.0443 (17)0.0192 (16)0.0184 (14)0.0052 (15)
C150.0355 (16)0.0478 (16)0.0348 (15)0.0065 (13)0.0151 (13)0.0042 (13)
C160.046 (2)0.057 (2)0.078 (3)0.0148 (17)0.0246 (18)0.0009 (18)
C170.041 (2)0.129 (4)0.070 (3)0.025 (2)0.023 (2)0.012 (2)
C180.052 (2)0.0406 (16)0.065 (2)0.0060 (14)0.0261 (17)0.0058 (15)
C190.044 (2)0.164 (5)0.041 (2)0.016 (3)0.0063 (17)0.015 (2)
C200.076 (3)0.081 (3)0.066 (3)0.007 (2)0.005 (2)0.025 (2)
C210.072 (3)0.073 (2)0.054 (2)0.013 (2)0.024 (2)0.0139 (18)
P0.0392 (5)0.0616 (5)0.0320 (4)0.0034 (4)0.0103 (3)0.0025 (3)
Cu10.0285 (2)0.0388 (2)0.0322 (2)0.00097 (13)0.01154 (16)0.00234 (13)
Cu20.0284 (2)0.0384 (2)0.0314 (2)0.00060 (13)0.01196 (15)0.00072 (13)
Geometric parameters (Å, º) top
C1—C21.415 (4)C13—C141.392 (5)
C1—C61.414 (4)C13—C171.502 (5)
C1—Cu12.006 (3)C14—H140.9300
C1—Cu22.095 (3)C14—C151.385 (4)
C2—C31.388 (4)C15—C181.507 (4)
C2—C71.501 (4)C16—H16A0.9600
C3—H30.9300C16—H16B0.9600
C3—C41.377 (5)C16—H16C0.9600
C4—C51.385 (5)C17—H17A0.9600
C4—C81.516 (5)C17—H17B0.9600
C5—H50.9300C17—H17C0.9600
C5—C61.395 (4)C18—H18A0.9600
C6—C91.500 (4)C18—H18B0.9600
C7—H7A0.9600C18—H18C0.9600
C7—H7B0.9600C19—H19A0.9600
C7—H7C0.9600C19—H19B0.9600
C8—H8A0.9600C19—H19C0.9600
C8—H8B0.9600C19—P1.820 (4)
C8—H8C0.9600C20—H20A0.9600
C9—H9A0.9600C20—H20B0.9600
C9—H9B0.9600C20—H20C0.9600
C9—H9C0.9600C20—P1.818 (4)
C10—C111.419 (4)C21—H21A0.9600
C10—C151.414 (4)C21—H21B0.9600
C10—Cu1i2.005 (3)C21—H21C0.9600
C10—Cu22.093 (3)C21—P1.808 (4)
C11—C121.390 (5)P—Cu22.2967 (9)
C11—C161.509 (5)Cu1—Cu1i2.5657 (7)
C12—H120.9300Cu1—Cu22.4603 (5)
C12—C131.386 (5)Cu1—Cu2i2.4625 (5)
C2—C1—Cu1110.9 (2)C11—C16—H16B109.5
C2—C1—Cu2117.0 (2)C11—C16—H16C109.5
C6—C1—C2116.7 (3)H16A—C16—H16B109.5
C6—C1—Cu1116.0 (2)H16A—C16—H16C109.5
C6—C1—Cu2115.2 (2)H16B—C16—H16C109.5
Cu1—C1—Cu273.70 (9)C13—C17—H17A109.5
C1—C2—C7119.6 (3)C13—C17—H17B109.5
C3—C2—C1120.9 (3)C13—C17—H17C109.5
C3—C2—C7119.5 (3)H17A—C17—H17B109.5
C2—C3—H3119.0H17A—C17—H17C109.5
C4—C3—C2122.0 (3)H17B—C17—H17C109.5
C4—C3—H3119.0C15—C18—H18A109.5
C3—C4—C5117.9 (3)C15—C18—H18B109.5
C3—C4—C8120.7 (4)C15—C18—H18C109.5
C5—C4—C8121.4 (4)H18A—C18—H18B109.5
C4—C5—H5119.1H18A—C18—H18C109.5
C4—C5—C6121.8 (3)H18B—C18—H18C109.5
C6—C5—H5119.1H19A—C19—H19B109.5
C1—C6—C9120.7 (3)H19A—C19—H19C109.5
C5—C6—C1120.7 (3)H19B—C19—H19C109.5
C5—C6—C9118.6 (3)P—C19—H19A109.5
C2—C7—H7A109.5P—C19—H19B109.5
C2—C7—H7B109.5P—C19—H19C109.5
C2—C7—H7C109.5H20A—C20—H20B109.5
H7A—C7—H7B109.5H20A—C20—H20C109.5
H7A—C7—H7C109.5H20B—C20—H20C109.5
H7B—C7—H7C109.5P—C20—H20A109.5
C4—C8—H8A109.5P—C20—H20B109.5
C4—C8—H8B109.5P—C20—H20C109.5
C4—C8—H8C109.5H21A—C21—H21B109.5
H8A—C8—H8B109.5H21A—C21—H21C109.5
H8A—C8—H8C109.5H21B—C21—H21C109.5
H8B—C8—H8C109.5P—C21—H21A109.5
C6—C9—H9A109.5P—C21—H21B109.5
C6—C9—H9B109.5P—C21—H21C109.5
C6—C9—H9C109.5C19—P—Cu2116.81 (13)
H9A—C9—H9B109.5C20—P—C19103.0 (2)
H9A—C9—H9C109.5C20—P—Cu2117.98 (14)
H9B—C9—H9C109.5C21—P—C19102.3 (2)
C11—C10—Cu1i110.2 (2)C21—P—C20100.9 (2)
C11—C10—Cu2119.0 (2)C21—P—Cu2113.53 (14)
C15—C10—C11116.5 (3)C1—Cu1—Cu1i110.85 (8)
C15—C10—Cu1i117.9 (2)C1—Cu1—Cu254.80 (8)
C15—C10—Cu2112.5 (2)C1—Cu1—Cu2i161.89 (8)
Cu1i—C10—Cu273.85 (9)C10i—Cu1—C1138.26 (11)
C10—C11—C16119.9 (3)C10i—Cu1—Cu1i110.89 (8)
C12—C11—C10120.9 (3)C10i—Cu1—Cu2i54.72 (8)
C12—C11—C16119.2 (3)C10i—Cu1—Cu2161.12 (8)
C11—C12—H12118.9Cu2i—Cu1—Cu1i58.546 (15)
C13—C12—C11122.2 (3)Cu2—Cu1—Cu1i58.630 (15)
C13—C12—H12118.9Cu2—Cu1—Cu2i117.169 (16)
C12—C13—C14117.1 (3)C1—Cu2—P97.94 (8)
C12—C13—C17120.8 (4)C1—Cu2—Cu151.50 (8)
C14—C13—C17122.1 (4)C1—Cu2—Cu1i111.73 (8)
C13—C14—H14118.8C10—Cu2—C1163.04 (11)
C15—C14—C13122.3 (3)C10—Cu2—P99.02 (8)
C15—C14—H14118.8C10—Cu2—Cu1111.87 (8)
C10—C15—C18120.6 (3)C10—Cu2—Cu1i51.43 (8)
C14—C15—C10121.0 (3)P—Cu2—Cu1i149.44 (3)
C14—C15—C18118.4 (3)P—Cu2—Cu1147.71 (3)
C11—C16—H16A109.5Cu1—Cu2—Cu1i62.824 (16)
C1—C2—C3—C41.5 (5)C15—C10—C11—C121.1 (4)
C2—C1—C6—C50.8 (4)C15—C10—C11—C16179.7 (3)
C2—C1—C6—C9178.6 (3)C16—C11—C12—C13177.8 (3)
C2—C3—C4—C50.7 (6)C17—C13—C14—C15179.8 (3)
C2—C3—C4—C8179.3 (4)Cu1—C1—C2—C3137.4 (3)
C3—C4—C5—C60.2 (5)Cu1—C1—C2—C742.3 (3)
C4—C5—C6—C10.1 (5)Cu1—C1—C6—C5134.4 (3)
C4—C5—C6—C9177.8 (3)Cu1—C1—C6—C947.8 (4)
C6—C1—C2—C31.6 (4)Cu1i—C10—C11—C12139.0 (3)
C6—C1—C2—C7178.2 (3)Cu1i—C10—C11—C1642.5 (3)
C7—C2—C3—C4178.2 (3)Cu1i—C10—C15—C14136.9 (3)
C8—C4—C5—C6179.9 (4)Cu1i—C10—C15—C1845.0 (4)
C10—C11—C12—C130.7 (5)Cu2—C1—C2—C3140.8 (3)
C11—C10—C15—C142.3 (4)Cu2—C1—C2—C739.4 (4)
C11—C10—C15—C18179.6 (3)Cu2—C1—C6—C5142.2 (3)
C11—C12—C13—C141.4 (5)Cu2—C1—C6—C935.6 (4)
C11—C12—C13—C17178.5 (3)Cu2—C10—C11—C12138.7 (3)
C12—C13—C14—C150.2 (5)Cu2—C10—C11—C1639.8 (4)
C13—C14—C15—C101.8 (5)Cu2—C10—C15—C14140.1 (2)
C13—C14—C15—C18179.9 (3)Cu2—C10—C15—C1838.0 (3)
Symmetry code: (i) x+1, y, z+1/2.
 

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