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The title compound, [Cu(C3H9P4)4][CuCl2], previously reported by Chi et al. [J. Chem. Soc. Dalton Trans. (1992), pp. 3111-3117] has been rerefined with new intensity data. Geometric parameters agree quite well. However, our results are of significantly higher precision. Furthermore, our data indicate a different absolute structure than the one reported by Chi et al. The Cu, Cl atoms and one of the P atoms are located on a threefold rotation axis. As a result, there is just one third of both ions in the asymmetric unit.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804000790/lh6159sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804000790/lh6159Isup2.hkl
Contains datablock I

CCDC reference: 199145

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](Cu-Cl) = 0.001 Å
  • R factor = 0.031
  • wR factor = 0.080
  • Data-to-parameter ratio = 35.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.91
Author Response: The data are 96.2 % complete to 2theta = 50 deg.

Alert level C PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... P1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... P2 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cu2
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 31.32 From the CIF: _reflns_number_total 2172 Count of symmetry unique reflns 1486 Completeness (_total/calc) 146.16% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 686 Fraction of Friedel pairs measured 0.462 Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 1990).

(I) top
Crystal data top
[Cu(C3H9P4)4][CuCl2]Dx = 1.361 Mg m3
Mr = 502.27Mo Kα radiation, λ = 0.71073 Å
Cubic, P213Cell parameters from 5949 reflections
Hall symbol: P 2ac 2ab 3θ = 3.8–31.3°
a = 13.4832 (11) ŵ = 2.21 mm1
V = 2451.2 (3) Å3T = 173 K
Z = 4Block, colourless
F(000) = 10400.50 × 0.40 × 0.30 mm
Data collection top
Stoe IPDS-II two-circle
diffractometer
2172 independent reflections
Radiation source: fine-focus sealed tube2035 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ω scansθmax = 31.3°, θmin = 3.7°
Absorption correction: empirical
(MULABS; Spek, 1990; Blessing, 1995)
h = 1818
Tmin = 0.380, Tmax = 0.521k = 1119
4186 measured reflectionsl = 184
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)] = 0.031H-atom parameters constrained
wR(F2) = 0.080 w = 1/[σ2(Fo2) + (0.0565P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
2172 reflectionsΔρmax = 0.28 e Å3
61 parametersΔρmin = 0.37 e Å3
0 restraintsAbsolute structure: Flack (1983), 686 Friedels
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.012 (14)
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
Cu10.543243 (16)0.543243 (16)0.543243 (16)0.03172 (9)
P10.44661 (4)0.44661 (4)0.44661 (4)0.0444 (2)
P20.56283 (4)0.69364 (4)0.47078 (5)0.04043 (13)
C10.4214 (5)0.3225 (3)0.4927 (5)0.0959 (16)
H1A0.37890.28720.44540.144*
H1B0.38760.32690.55690.144*
H1C0.48390.28640.50070.144*
C20.6560 (2)0.7748 (2)0.5257 (3)0.0580 (7)
H2A0.71950.73960.52950.087*
H2B0.63490.79400.59250.087*
H2C0.66360.83420.48460.087*
C30.4546 (2)0.7750 (2)0.4689 (5)0.0833 (14)
H3A0.39780.73920.44090.125*
H3B0.46880.83340.42810.125*
H3C0.43890.79600.53670.125*
C40.6003 (5)0.6932 (4)0.3404 (3)0.0843 (13)
H4A0.55500.65100.30230.127*
H4B0.66800.66740.33470.127*
H4C0.59790.76100.31430.127*
Cu20.86620 (2)0.86620 (2)0.86620 (2)0.04708 (13)
Cl10.95586 (7)0.95586 (7)0.95586 (7)0.0914 (6)
Cl20.77738 (7)0.77738 (7)0.77738 (7)0.1003 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.03172 (9)0.03172 (9)0.03172 (9)0.00126 (8)0.00126 (8)0.00126 (8)
P10.0444 (2)0.0444 (2)0.0444 (2)0.0078 (2)0.0078 (2)0.0078 (2)
P20.0357 (3)0.0370 (2)0.0487 (3)0.00312 (18)0.0048 (2)0.0080 (2)
C10.121 (4)0.0518 (17)0.115 (4)0.037 (2)0.030 (3)0.005 (2)
C20.0480 (13)0.0481 (12)0.078 (2)0.0162 (10)0.0082 (13)0.0053 (13)
C30.0450 (14)0.0497 (13)0.155 (4)0.0053 (11)0.015 (2)0.024 (2)
C40.125 (4)0.077 (2)0.0507 (16)0.012 (2)0.006 (2)0.0215 (15)
Cu20.04708 (13)0.04708 (13)0.04708 (13)0.00266 (12)0.00266 (12)0.00266 (12)
Cl10.0914 (6)0.0914 (6)0.0914 (6)0.0242 (5)0.0242 (5)0.0242 (5)
Cl20.1003 (7)0.1003 (7)0.1003 (7)0.0301 (6)0.0301 (6)0.0301 (6)
Geometric parameters (Å, º) top
Cu1—P12.2567 (11)C1—H1C0.9800
Cu1—P2i2.2663 (6)C2—H2A0.9800
Cu1—P22.2664 (6)C2—H2B0.9800
Cu1—P2ii2.2664 (6)C2—H2C0.9800
P1—C1i1.818 (4)C3—H3A0.9800
P1—C11.818 (4)C3—H3B0.9800
P1—C1ii1.818 (4)C3—H3C0.9800
P2—C21.823 (3)C4—H4A0.9800
P2—C31.826 (3)C4—H4B0.9800
P2—C41.829 (4)C4—H4C0.9800
C1—H1A0.9800Cu2—Cl22.0743 (17)
C1—H1B0.9800Cu2—Cl12.0938 (16)
P1—Cu1—P2i109.570 (18)H1A—C1—H1C109.5
P1—Cu1—P2109.569 (17)H1B—C1—H1C109.5
P2i—Cu1—P2109.372 (17)P2—C2—H2A109.5
P1—Cu1—P2ii109.569 (17)P2—C2—H2B109.5
P2i—Cu1—P2ii109.373 (18)H2A—C2—H2B109.5
P2—Cu1—P2ii109.373 (18)P2—C2—H2C109.5
C1i—P1—C1101.9 (2)H2A—C2—H2C109.5
C1i—P1—C1ii101.9 (2)H2B—C2—H2C109.5
C1—P1—C1ii101.9 (2)P2—C3—H3A109.5
C1i—P1—Cu1116.26 (18)P2—C3—H3B109.5
C1—P1—Cu1116.26 (18)H3A—C3—H3B109.5
C1ii—P1—Cu1116.26 (18)P2—C3—H3C109.5
C2—P2—C3101.31 (18)H3A—C3—H3C109.5
C2—P2—C4101.7 (2)H3B—C3—H3C109.5
C3—P2—C4102.1 (3)P2—C4—H4A109.5
C2—P2—Cu1116.23 (11)P2—C4—H4B109.5
C3—P2—Cu1116.76 (13)H4A—C4—H4B109.5
C4—P2—Cu1116.35 (15)P2—C4—H4C109.5
P1—C1—H1A109.5H4A—C4—H4C109.5
P1—C1—H1B109.5H4B—C4—H4C109.5
H1A—C1—H1B109.5Cl2—Cu2—Cl1180.00 (3)
P1—C1—H1C109.5
P2i—Cu1—P1—C1i179.6 (3)P1—Cu1—P2—C2169.42 (13)
P2—Cu1—P1—C1i60.4 (3)P2i—Cu1—P2—C270.46 (13)
P2ii—Cu1—P1—C1i59.6 (3)P2ii—Cu1—P2—C249.30 (14)
P2i—Cu1—P1—C159.6 (3)P1—Cu1—P2—C371.0 (2)
P2—Cu1—P1—C1179.6 (3)P2i—Cu1—P2—C349.1 (2)
P2ii—Cu1—P1—C160.4 (3)P2ii—Cu1—P2—C3168.9 (2)
P2i—Cu1—P1—C1ii60.4 (3)P1—Cu1—P2—C449.7 (2)
P2—Cu1—P1—C1ii59.6 (3)P2i—Cu1—P2—C4169.8 (2)
P2ii—Cu1—P1—C1ii179.6 (3)P2ii—Cu1—P2—C470.4 (2)
Symmetry codes: (i) z, x, y; (ii) y, z, x.
 

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