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The title complex, [Cu2I2(C31H28N2P2)2]·CH2Cl2, has a dimeric structure where two CuI atoms are doubly bridged by two I atoms. An inversion center is located midway between the two Cu atoms. The coordination geometry around the Cu atom is distorted tetra­hedral, formed by two P atoms from a bidentate N,N-bis­(diphenyl­phosphinometh­yl)-2-pyridinamine ligand and two iodine atoms. The complex has a metal–metal inter­action with a Cu...Cu distance of 3.068 (3) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806049701/jh2042sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806049701/jh2042Isup2.hkl
Contains datablock I

CCDC reference: 630033

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.008 Å
  • Disorder in solvent or counterion
  • R factor = 0.037
  • wR factor = 0.095
  • Data-to-parameter ratio = 14.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C16 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT410_ALERT_2_C Short Intra H...H Contact H2A .. H4 .. 1.99 Ang. PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 39.90 Deg. C32 -CL1 -C32 2.556 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 44.10 Deg. CL1 -CL2 -C32 2.556 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 38.00 Deg. C32 -CL2 -C32 2.556 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 31.60 Deg. CL2 -C32 -CL1 2.556 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 29.90 Deg. CL1 -C32 -CL2 2.556 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 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 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).

Di-µ-iodo-bis{[N,N-bis(diphenylphosphinomethyl)-2-pyridinamine- κ2P,P']copper(I)} dichloromethane solvate top
Crystal data top
[Cu2I2(C31H28N2P2)2]·CH2Cl2Z = 1
Mr = 1446.79F(000) = 722
Triclinic, P1Dx = 1.583 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.510 (4) ÅCell parameters from 3425 reflections
b = 11.879 (4) Åθ = 2.4–27.4°
c = 12.935 (4) ŵ = 1.95 mm1
α = 72.992 (4)°T = 298 K
β = 81.788 (5)°Block, colorless
γ = 81.119 (5)°0.55 × 0.47 × 0.42 mm
V = 1517.6 (9) Å3
Data collection top
Bruker SMART APEX CCD
diffractometer
5288 independent reflections
Radiation source: fine-focus sealed tube4019 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
ω scansθmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 126
Tmin = 0.343, Tmax = 0.444k = 1314
7973 measured reflectionsl = 1514
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)] = 0.037H-atom parameters constrained
wR(F2) = 0.095 w = 1/[σ2(Fo2) + (0.0366P)2 + 0.656P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max < 0.001
5288 reflectionsΔρmax = 0.64 e Å3
362 parametersΔρmin = 0.59 e Å3
27 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0052 (6)
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*/UeqOcc. (<1)
Cu20.56363 (5)0.47231 (4)0.10564 (4)0.03834 (16)
I10.31082 (3)0.49507 (3)0.08996 (2)0.04650 (14)
Cl10.0492 (10)0.0809 (9)0.5577 (8)0.196 (3)0.50
Cl20.0337 (7)0.0784 (9)0.4328 (8)0.168 (3)0.50
N10.6210 (3)0.4696 (3)0.3744 (3)0.0382 (8)
N20.7623 (4)0.3854 (3)0.5077 (3)0.0500 (10)
P10.63471 (10)0.31553 (9)0.24065 (9)0.0360 (3)
P20.57302 (10)0.62458 (9)0.17552 (8)0.0337 (3)
C10.6010 (4)0.3512 (4)0.3741 (3)0.0400 (10)
H1A0.51180.33970.40170.048*
H1B0.65540.29420.42470.048*
C20.5264 (4)0.5658 (4)0.3238 (3)0.0388 (10)
H2A0.51900.62930.35820.047*
H2B0.44240.53730.33500.047*
C30.7006 (4)0.4852 (4)0.4457 (3)0.0386 (10)
C40.7169 (5)0.5961 (4)0.4525 (4)0.0527 (12)
H40.67630.66430.40740.063*
C50.7936 (6)0.6039 (5)0.5265 (4)0.0680 (15)
H50.80370.67780.53320.082*
C60.8559 (6)0.5031 (6)0.5910 (4)0.0714 (16)
H60.90790.50700.64210.086*
C70.8385 (5)0.3980 (5)0.5774 (4)0.0650 (15)
H70.88260.32970.61930.078*
C80.5683 (4)0.1722 (4)0.2883 (3)0.0426 (10)
C90.4402 (5)0.1714 (5)0.2778 (4)0.0629 (14)
H90.39130.24090.24320.076*
C100.3837 (7)0.0669 (6)0.3188 (5)0.086 (2)
H100.29680.06680.31200.103*
C110.4556 (8)0.0363 (5)0.3694 (5)0.0814 (19)
H110.41780.10630.39680.098*
C120.5816 (7)0.0354 (5)0.3791 (5)0.0726 (17)
H120.63030.10530.41310.087*
C130.6392 (5)0.0680 (4)0.3393 (4)0.0568 (13)
H130.72610.06720.34690.068*
C140.8084 (4)0.2729 (4)0.2220 (3)0.0414 (10)
C150.8972 (5)0.2993 (5)0.2751 (5)0.0618 (14)
H150.86900.33500.33070.074*
C161.0292 (5)0.2744 (6)0.2483 (6)0.086 (2)
H161.08800.29510.28480.103*
C171.0727 (5)0.2199 (5)0.1692 (5)0.0739 (17)
H171.16110.20240.15170.089*
C180.9853 (6)0.1913 (6)0.1158 (5)0.0790 (18)
H181.01460.15210.06280.095*
C190.8544 (5)0.2195 (5)0.1390 (4)0.0661 (15)
H190.79640.20290.09910.079*
C200.7247 (4)0.6830 (4)0.1727 (3)0.0389 (10)
C210.8378 (4)0.6140 (5)0.1525 (4)0.0562 (13)
H210.83540.54310.13630.067*
C220.9563 (5)0.6512 (6)0.1564 (5)0.0806 (19)
H221.03320.60460.14360.097*
C230.9593 (6)0.7562 (7)0.1790 (5)0.0805 (19)
H231.03840.78040.18220.097*
C240.8469 (6)0.8257 (5)0.1968 (4)0.0694 (16)
H240.84950.89760.21100.083*
C250.7301 (5)0.7896 (4)0.1938 (4)0.0504 (12)
H250.65380.83720.20610.060*
C260.4590 (4)0.7567 (3)0.1322 (3)0.0371 (10)
C270.3608 (4)0.7974 (4)0.1997 (4)0.0498 (12)
H270.35140.75800.27340.060*
C280.2748 (5)0.8978 (4)0.1576 (5)0.0602 (14)
H280.20930.92550.20370.072*
C290.2872 (5)0.9550 (4)0.0493 (5)0.0638 (15)
H290.22991.02150.02150.077*
C300.3836 (5)0.9146 (5)0.0183 (4)0.0672 (15)
H300.39220.95410.09200.081*
C310.4685 (5)0.8153 (4)0.0221 (4)0.0559 (13)
H310.53260.78750.02500.067*
C320.0503 (19)0.017 (2)0.504 (2)0.196 (7)0.50
H320.11780.02070.45680.235*0.50
H330.07860.08180.56250.235*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu20.0385 (3)0.0402 (3)0.0363 (3)0.0004 (2)0.0053 (2)0.0126 (2)
I10.03115 (17)0.0662 (2)0.03980 (19)0.00239 (13)0.00070 (12)0.01476 (15)
Cl10.237 (9)0.187 (6)0.165 (6)0.036 (8)0.041 (6)0.074 (5)
Cl20.150 (6)0.170 (5)0.195 (6)0.042 (5)0.089 (5)0.065 (4)
N10.049 (2)0.0334 (19)0.0302 (19)0.0002 (16)0.0053 (16)0.0074 (15)
N20.051 (2)0.057 (3)0.039 (2)0.0019 (19)0.0079 (18)0.0109 (19)
P10.0366 (6)0.0343 (6)0.0358 (6)0.0011 (5)0.0035 (5)0.0092 (5)
P20.0328 (6)0.0340 (6)0.0326 (6)0.0011 (5)0.0032 (4)0.0091 (5)
C10.046 (2)0.035 (2)0.036 (2)0.0010 (19)0.0030 (19)0.0083 (19)
C20.040 (2)0.040 (2)0.035 (2)0.0017 (19)0.0008 (18)0.0107 (19)
C30.041 (2)0.047 (3)0.027 (2)0.005 (2)0.0030 (18)0.0112 (19)
C40.073 (3)0.050 (3)0.037 (3)0.013 (2)0.010 (2)0.010 (2)
C50.084 (4)0.081 (4)0.052 (3)0.027 (3)0.013 (3)0.026 (3)
C60.072 (4)0.101 (5)0.052 (3)0.023 (3)0.017 (3)0.026 (3)
C70.060 (3)0.083 (4)0.047 (3)0.008 (3)0.016 (3)0.015 (3)
C80.050 (3)0.040 (3)0.040 (3)0.006 (2)0.004 (2)0.014 (2)
C90.069 (4)0.050 (3)0.066 (4)0.016 (3)0.017 (3)0.002 (3)
C100.097 (5)0.075 (4)0.092 (5)0.051 (4)0.021 (4)0.008 (4)
C110.125 (6)0.056 (4)0.070 (4)0.046 (4)0.006 (4)0.013 (3)
C120.116 (5)0.035 (3)0.063 (4)0.002 (3)0.016 (3)0.007 (3)
C130.071 (3)0.037 (3)0.061 (3)0.003 (2)0.014 (3)0.011 (2)
C140.044 (2)0.037 (2)0.037 (2)0.000 (2)0.003 (2)0.0042 (19)
C150.048 (3)0.067 (4)0.077 (4)0.001 (3)0.003 (3)0.036 (3)
C160.042 (3)0.105 (5)0.128 (6)0.004 (3)0.011 (3)0.061 (5)
C170.039 (3)0.088 (4)0.083 (4)0.008 (3)0.006 (3)0.019 (3)
C180.061 (4)0.109 (5)0.061 (4)0.027 (3)0.002 (3)0.037 (3)
C190.052 (3)0.097 (4)0.054 (3)0.011 (3)0.010 (2)0.036 (3)
C200.036 (2)0.044 (3)0.033 (2)0.0044 (19)0.0051 (18)0.0038 (19)
C210.043 (3)0.060 (3)0.060 (3)0.002 (2)0.003 (2)0.011 (3)
C220.036 (3)0.110 (5)0.082 (4)0.001 (3)0.003 (3)0.011 (4)
C230.061 (4)0.112 (6)0.064 (4)0.041 (4)0.018 (3)0.004 (4)
C240.077 (4)0.071 (4)0.065 (4)0.031 (3)0.025 (3)0.007 (3)
C250.051 (3)0.052 (3)0.048 (3)0.009 (2)0.010 (2)0.009 (2)
C260.037 (2)0.033 (2)0.045 (3)0.0026 (18)0.0089 (19)0.014 (2)
C270.045 (3)0.046 (3)0.055 (3)0.005 (2)0.004 (2)0.014 (2)
C280.045 (3)0.057 (3)0.079 (4)0.014 (2)0.007 (3)0.030 (3)
C290.062 (3)0.048 (3)0.080 (4)0.017 (3)0.030 (3)0.018 (3)
C300.082 (4)0.058 (3)0.052 (3)0.018 (3)0.024 (3)0.007 (3)
C310.065 (3)0.049 (3)0.049 (3)0.010 (2)0.007 (2)0.013 (2)
C320.195 (10)0.198 (9)0.199 (9)0.004 (8)0.026 (8)0.066 (7)
Geometric parameters (Å, º) top
Cu2—P12.2620 (13)C12—C131.382 (7)
Cu2—P22.2662 (13)C12—H120.9300
Cu2—I1i2.6313 (9)C13—H130.9300
Cu2—I12.6597 (10)C14—C151.356 (7)
Cl1—Cl2ii0.892 (11)C14—C191.394 (6)
Cl1—C32ii1.25 (2)C15—C161.388 (7)
Cl1—C321.684 (16)C15—H150.9300
Cl2—C32ii1.56 (2)C16—C171.355 (8)
Cl2—C321.721 (17)C16—H160.9300
N1—C31.397 (5)C17—C181.360 (8)
N1—C11.455 (5)C17—H170.9300
N1—C21.457 (5)C18—C191.376 (7)
N2—C71.341 (6)C18—H180.9300
N2—C31.351 (5)C19—H190.9300
P1—C141.819 (4)C20—C211.374 (6)
P1—C81.843 (4)C20—C251.382 (6)
P1—C11.869 (4)C21—C221.396 (7)
P2—C261.819 (4)C21—H210.9300
P2—C201.826 (4)C22—C231.367 (9)
P2—C21.860 (4)C22—H220.9300
C1—H1A0.9700C23—C241.365 (8)
C1—H1B0.9700C23—H230.9300
C2—H2A0.9700C24—C251.370 (7)
C2—H2B0.9700C24—H240.9300
C3—C41.384 (6)C25—H250.9300
C4—C51.367 (7)C26—C271.378 (6)
C4—H40.9300C26—C311.387 (6)
C5—C61.374 (8)C27—C281.401 (6)
C5—H50.9300C27—H270.9300
C6—C71.354 (7)C28—C291.364 (7)
C6—H60.9300C28—H280.9300
C7—H70.9300C29—C301.366 (7)
C8—C91.374 (7)C29—H290.9300
C8—C131.379 (6)C30—C311.381 (7)
C9—C101.388 (7)C30—H300.9300
C9—H90.9300C31—H310.9300
C10—C111.375 (9)C32—C32ii1.08 (4)
C10—H100.9300C32—H320.9444
C11—C121.349 (9)C32—H330.9520
C11—H110.9300
P1—Cu2—P2101.06 (5)C15—C14—P1125.1 (4)
P1—Cu2—I1i118.65 (4)C19—C14—P1117.0 (4)
P2—Cu2—I1i111.47 (4)C14—C15—C16121.6 (5)
P1—Cu2—I1114.38 (4)C14—C15—H15119.2
P2—Cu2—I1100.28 (3)C16—C15—H15119.2
I1i—Cu2—I1109.13 (2)C17—C16—C15120.3 (6)
Cu2i—I1—Cu270.87 (2)C17—C16—H16119.8
Cl2ii—Cl1—C32ii106.0 (16)C15—C16—H16119.8
Cl2ii—Cl1—C3266.8 (13)C16—C17—C18119.1 (5)
C32ii—Cl1—C3239.9 (14)C16—C17—H17120.5
Cl1ii—Cl2—C32ii81.6 (13)C18—C17—H17120.5
Cl1ii—Cl2—C3244.1 (12)C17—C18—C19121.1 (5)
C32ii—Cl2—C3238.0 (12)C17—C18—H18119.5
C3—N1—C1120.6 (3)C19—C18—H18119.5
C3—N1—C2120.8 (3)C18—C19—C14120.3 (5)
C1—N1—C2116.0 (3)C18—C19—H19119.8
C7—N2—C3117.3 (4)C14—C19—H19119.8
C14—P1—C8103.3 (2)C21—C20—C25119.5 (4)
C14—P1—C1106.3 (2)C21—C20—P2117.3 (4)
C8—P1—C195.80 (19)C25—C20—P2123.2 (3)
C14—P1—Cu2112.98 (14)C20—C21—C22119.5 (5)
C8—P1—Cu2125.43 (15)C20—C21—H21120.3
C1—P1—Cu2110.56 (14)C22—C21—H21120.3
C26—P2—C20103.83 (19)C23—C22—C21120.0 (5)
C26—P2—C2104.85 (19)C23—C22—H22120.0
C20—P2—C2102.32 (19)C21—C22—H22120.0
C26—P2—Cu2116.81 (14)C24—C23—C22120.3 (5)
C20—P2—Cu2122.20 (15)C24—C23—H23119.8
C2—P2—Cu2104.68 (14)C22—C23—H23119.8
N1—C1—P1116.8 (3)C23—C24—C25120.1 (6)
N1—C1—H1A108.1C23—C24—H24120.0
P1—C1—H1A108.1C25—C24—H24120.0
N1—C1—H1B108.1C24—C25—C20120.6 (5)
P1—C1—H1B108.1C24—C25—H25119.7
H1A—C1—H1B107.3C20—C25—H25119.7
N1—C2—P2111.6 (3)C27—C26—C31118.6 (4)
N1—C2—H2A109.3C27—C26—P2124.5 (3)
P2—C2—H2A109.3C31—C26—P2116.7 (3)
N1—C2—H2B109.3C26—C27—C28120.2 (5)
P2—C2—H2B109.3C26—C27—H27119.9
H2A—C2—H2B108.0C28—C27—H27119.9
N2—C3—C4121.4 (4)C29—C28—C27120.1 (5)
N2—C3—N1116.2 (4)C29—C28—H28119.9
C4—C3—N1122.4 (4)C27—C28—H28119.9
C5—C4—C3118.9 (5)C28—C29—C30120.0 (5)
C5—C4—H4120.6C28—C29—H29120.0
C3—C4—H4120.6C30—C29—H29120.0
C4—C5—C6120.4 (5)C29—C30—C31120.4 (5)
C4—C5—H5119.8C29—C30—H30119.8
C6—C5—H5119.8C31—C30—H30119.8
C7—C6—C5117.3 (5)C30—C31—C26120.6 (5)
C7—C6—H6121.3C30—C31—H31119.7
C5—C6—H6121.3C26—C31—H31119.7
N2—C7—C6124.6 (5)C32ii—C32—Cl1ii92 (2)
N2—C7—H7117.7C32ii—C32—Cl2ii78.9 (19)
C6—C7—H7117.7Cl1ii—C32—Cl2ii170 (2)
C9—C8—C13119.1 (4)C32ii—C32—Cl147.7 (15)
C9—C8—P1118.0 (3)Cl1ii—C32—Cl1140.1 (14)
C13—C8—P1122.9 (4)Cl2ii—C32—Cl131.6 (5)
C8—C9—C10120.1 (5)C32ii—C32—Cl263.1 (18)
C8—C9—H9120.0Cl1ii—C32—Cl229.9 (7)
C10—C9—H9120.0Cl2ii—C32—Cl2142.0 (12)
C11—C10—C9120.2 (6)Cl1—C32—Cl2110.6 (10)
C11—C10—H10119.9C32ii—C32—H32121.8
C9—C10—H10119.9Cl1ii—C32—H3290.1
C12—C11—C10119.6 (5)Cl2ii—C32—H3289.6
C12—C11—H11120.2Cl1—C32—H32109.7
C10—C11—H11120.2Cl2—C32—H32109.7
C11—C12—C13121.0 (5)C32ii—C32—H33123.3
C11—C12—H12119.5Cl1ii—C32—H3394.3
C13—C12—H12119.5Cl2ii—C32—H3395.3
C8—C13—C12120.1 (5)Cl1—C32—H33107.2
C8—C13—H13119.9Cl2—C32—H33105.1
C12—C13—H13119.9H32—C32—H33114.4
C15—C14—C19117.5 (4)
Symmetry codes: (i) x+1, y+1, z; (ii) x, y, z+1.
 

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