Literature DB >> 21581179

catena-Poly[[(1,10-phenanthroline-κN,N')copper(I)]-μ-thiocyanato-κN:S-[(1,10-phenanthroline-κN,N')copper(I)]-μ-cyanido-κN:C].

Jun Zhao1, Wen-Wen Dong, Dong-Sheng Li, Xi-Jun Ke.   

Abstract

In the title complex, [Cu(2)(CN)(NCS)(C(12)H(8)N(2))(2)], which was synthesized under hydro-thermal conditions, both Cu(I) atoms have a slightly distorted tetra-hedral geometry. They are coordinated by two N atoms of one 1,10-phenanthroline ligand, one bridging thio-cyanate anion and one bridging cyanide anion. In the crystal structure, infinite helical {Cu-CN-Cu-SCN}(n) chains are formed along [01].

Entities:  

Year:  2008        PMID: 21581179      PMCID: PMC2959958          DOI: 10.1107/S1600536808037744

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


Related literature

For related literature, see: Cheng et al. (2006 ▶); Greig & Philp (2001 ▶); Luan et al. (2006 ▶); Piguet et al. (1997 ▶).

Experimental

Crystal data

[Cu2(CN)(NCS)(C12H8N2)2] M = 571.59 Monoclinic, a = 13.046 (7) Å b = 13.470 (7) Å c = 13.538 (7) Å β = 90.044 (9)° V = 2379 (2) Å3 Z = 4 Mo Kα radiation μ = 1.90 mm−1 T = 293 (2) K 0.30 × 0.15 × 0.12 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan SADABS (Sheldrick, 1996 ▶) T min = 0.599, T max = 0.804 15496 measured reflections 4959 independent reflections 3662 reflections with I > 2σ(I) R int = 0.081

Refinement

R[F 2 > 2σ(F 2)] = 0.061 wR(F 2) = 0.164 S = 1.00 4959 reflections 316 parameters H-atom parameters constrained Δρmax = 0.47 e Å−3 Δρmin = −0.57 e Å−3 Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); 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 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S1600536808037744/bt2813sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808037744/bt2813Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu2(CN)(NCS)(C12H8N2)2]F000 = 1152
Mr = 571.59Dx = 1.596 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2103 reflections
a = 13.046 (7) Åθ = 2.2–27.5º
b = 13.470 (7) ŵ = 1.90 mm1
c = 13.538 (7) ÅT = 293 (2) K
β = 90.044 (9)ºPrism, red
V = 2379 (2) Å30.30 × 0.15 × 0.12 mm
Z = 4
Bruker SMART CCD diffractometer4959 independent reflections
Radiation source: fine-focus sealed tube3662 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.081
Detector resolution: 13.6612 pixels mm-1θmax = 27.5º
T = 293(2) Kθmin = 2.2º
CCD Profile fitting scansh = −15→16
Absorption correction: multi-scanSADABS (Sheldrick, 1996)k = −17→15
Tmin = 0.599, Tmax = 0.804l = −17→17
15496 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.061H-atom parameters constrained
wR(F2) = 0.164  w = 1/[σ2(Fo2) + (0.0669P)2 + 0.4979P] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
4959 reflectionsΔρmax = 0.47 e Å3
316 parametersΔρmin = −0.57 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
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*/Ueq
Cu10.08441 (4)0.73813 (3)0.04132 (4)0.06012 (19)
Cu20.45032 (3)0.76203 (3)−0.04863 (3)0.05589 (18)
C10.3089 (3)0.7520 (2)−0.0233 (3)0.0502 (8)
N20.5019 (2)0.8164 (2)−0.1747 (2)0.0623 (7)
N3−0.0405 (2)0.73312 (19)−0.0551 (2)0.0557 (7)
N40.0024 (2)0.86301 (19)0.0898 (2)0.0524 (6)
N50.54334 (18)0.8232 (2)0.06500 (19)0.0501 (6)
N60.5591 (2)0.64667 (19)−0.02813 (19)0.0515 (6)
N10.2232 (2)0.74724 (19)−0.0059 (2)0.0619 (8)
C20.5338 (2)0.8478 (2)−0.2473 (2)0.0505 (7)
C3−0.0636 (3)0.6686 (3)−0.1262 (3)0.0712 (10)
H3A−0.02260.6125−0.13250.085*
C4−0.1433 (4)0.6793 (3)−0.1905 (4)0.0901 (14)
H4A−0.15490.6324−0.23970.108*
C5−0.2064 (4)0.7608 (3)−0.1815 (4)0.0854 (15)
H5A−0.26100.7697−0.22480.103*
C6−0.1878 (2)0.8295 (2)−0.1071 (3)0.0609 (9)
C7−0.2500 (3)0.9176 (3)−0.0924 (3)0.0709 (10)
H7A−0.30600.9296−0.13330.085*
C8−0.2269 (3)0.9819 (3)−0.0200 (3)0.0662 (10)
H8A−0.26751.0380−0.01190.079*
C9−0.1417 (2)0.9670 (2)0.0451 (3)0.0523 (7)
C10−0.1156 (3)1.0327 (2)0.1207 (3)0.0597 (9)
H10A−0.15451.08960.13110.072*
C11−0.0333 (3)1.0133 (3)0.1790 (3)0.0682 (10)
H11A−0.01551.05630.22990.082*
C120.0254 (3)0.9263 (3)0.1610 (2)0.0625 (9)
H12A0.08200.91350.20080.075*
C13−0.0798 (2)0.8824 (2)0.0330 (2)0.0473 (7)
C14−0.1038 (2)0.8128 (2)−0.0458 (2)0.0502 (7)
C150.5371 (3)0.9102 (3)0.1122 (3)0.0639 (9)
H15A0.48490.95360.09430.077*
C160.6044 (3)0.9392 (3)0.1865 (3)0.0747 (10)
H16A0.59681.00080.21670.090*
C170.6812 (3)0.8776 (3)0.2149 (3)0.0733 (10)
H17A0.72530.89540.26590.088*
C180.6929 (3)0.7856 (3)0.1653 (3)0.0559 (8)
C190.7759 (3)0.7185 (3)0.1877 (3)0.0692 (10)
H19A0.82190.73320.23820.083*
C200.7865 (3)0.6345 (3)0.1351 (3)0.0696 (10)
H20A0.84240.59370.14780.084*
C210.7157 (2)0.6058 (2)0.0611 (3)0.0581 (8)
C220.7226 (3)0.5174 (3)0.0063 (3)0.0743 (12)
H22A0.77700.47400.01680.089*
C230.6491 (3)0.4955 (3)−0.0622 (3)0.0783 (12)
H23A0.65300.4370−0.09850.094*
C240.5680 (3)0.5616 (3)−0.0775 (3)0.0641 (9)
H24A0.51820.5455−0.12400.077*
C250.6313 (2)0.6691 (2)0.0399 (2)0.0471 (7)
C260.6224 (3)0.7617 (2)0.0929 (2)0.0468 (7)
S10.58145 (8)0.89734 (6)−0.34839 (7)0.0644 (3)
U11U22U33U12U13U23
Cu10.0442 (3)0.0592 (3)0.0770 (4)0.01178 (17)0.0058 (2)0.00483 (19)
Cu20.0407 (3)0.0623 (3)0.0646 (3)0.00543 (17)−0.0032 (2)0.00538 (18)
C10.0387 (17)0.0418 (15)0.070 (2)0.0058 (12)0.0049 (15)0.0057 (13)
N20.0498 (15)0.0711 (19)0.0659 (18)−0.0020 (14)−0.0025 (13)0.0112 (15)
N30.0468 (16)0.0429 (14)0.077 (2)0.0043 (11)0.0045 (15)−0.0008 (12)
N40.0538 (14)0.0452 (13)0.0582 (15)0.0046 (12)0.0092 (12)0.0053 (12)
N50.0421 (13)0.0504 (14)0.0577 (15)0.0087 (11)0.0024 (11)−0.0010 (12)
N60.0503 (14)0.0457 (14)0.0584 (15)0.0028 (11)0.0049 (12)0.0001 (12)
N10.0516 (19)0.0502 (16)0.084 (2)0.0083 (12)0.0027 (16)0.0065 (14)
C20.0389 (14)0.0447 (16)0.068 (2)0.0002 (13)−0.0035 (14)−0.0008 (14)
C30.061 (2)0.056 (2)0.097 (3)0.0088 (17)−0.003 (2)−0.023 (2)
C40.084 (3)0.067 (3)0.119 (4)0.008 (2)−0.017 (3)−0.036 (3)
C50.060 (3)0.069 (3)0.127 (4)0.0007 (19)−0.027 (3)−0.022 (2)
C60.0396 (15)0.0487 (17)0.094 (3)−0.0007 (14)−0.0049 (16)−0.0069 (17)
C70.0495 (18)0.0507 (19)0.113 (3)0.0065 (16)−0.0176 (19)−0.005 (2)
C80.0518 (19)0.0413 (17)0.106 (3)0.0098 (15)−0.0004 (19)0.0024 (18)
C90.0471 (16)0.0394 (15)0.071 (2)0.0027 (13)0.0081 (15)0.0049 (14)
C100.067 (2)0.0431 (17)0.069 (2)0.0091 (15)0.0118 (18)0.0027 (15)
C110.089 (3)0.056 (2)0.060 (2)0.006 (2)0.004 (2)0.0001 (16)
C120.071 (2)0.060 (2)0.0563 (19)0.0092 (18)−0.0005 (16)0.0008 (16)
C130.0384 (14)0.0383 (15)0.0653 (18)0.0014 (12)0.0091 (13)0.0044 (13)
C140.0395 (14)0.0389 (15)0.072 (2)0.0000 (12)0.0074 (14)0.0024 (14)
C150.0590 (19)0.060 (2)0.072 (2)0.0170 (17)0.0047 (17)−0.0110 (17)
C160.078 (2)0.074 (2)0.072 (2)0.011 (2)−0.001 (2)−0.023 (2)
C170.071 (2)0.085 (3)0.065 (2)−0.006 (2)−0.0035 (18)−0.016 (2)
C180.0430 (17)0.066 (2)0.0590 (19)−0.0033 (16)−0.0031 (14)0.0115 (17)
C190.049 (2)0.086 (3)0.072 (2)0.003 (2)−0.0150 (17)0.017 (2)
C200.0497 (18)0.073 (2)0.086 (3)0.0160 (18)−0.0044 (18)0.030 (2)
C210.0468 (17)0.0500 (18)0.077 (2)0.0118 (14)0.0091 (16)0.0149 (16)
C220.072 (3)0.052 (2)0.099 (3)0.0215 (19)0.020 (2)0.013 (2)
C230.092 (3)0.047 (2)0.097 (3)0.012 (2)0.021 (3)−0.005 (2)
C240.075 (2)0.0519 (18)0.065 (2)0.0020 (17)0.0054 (17)−0.0055 (16)
C250.0397 (14)0.0446 (15)0.0570 (17)0.0076 (12)0.0079 (13)0.0080 (13)
C260.0429 (17)0.0476 (16)0.0500 (17)0.0051 (12)0.0054 (14)0.0045 (12)
S10.0725 (6)0.0491 (5)0.0717 (6)−0.0137 (4)0.0150 (5)−0.0022 (4)
Cu1—N11.924 (3)C8—H8A0.9300
Cu1—N32.089 (3)C9—C101.395 (5)
Cu1—N42.099 (3)C9—C131.406 (4)
Cu1—S1i2.3581 (13)C10—C111.358 (5)
Cu2—C11.882 (3)C10—H10A0.9300
Cu2—N21.976 (3)C11—C121.420 (5)
Cu2—N62.123 (3)C11—H11A0.9300
Cu2—N52.125 (3)C12—H12A0.9300
C1—N11.145 (5)C13—C141.454 (5)
N2—C21.148 (4)C15—C161.391 (5)
N3—C31.331 (5)C15—H15A0.9300
N3—C141.360 (4)C16—C171.356 (6)
N4—C121.322 (4)C16—H16A0.9300
N4—C131.345 (4)C17—C181.417 (5)
N5—C151.336 (4)C17—H17A0.9300
N5—C261.376 (4)C18—C261.382 (5)
N6—C241.331 (4)C18—C191.443 (5)
N6—C251.351 (4)C19—C201.343 (6)
C2—S11.645 (3)C19—H19A0.9300
C3—C41.363 (6)C20—C211.416 (5)
C3—H3A0.9300C20—H20A0.9300
C4—C51.377 (6)C21—C221.406 (5)
C4—H4A0.9300C21—C251.421 (4)
C5—C61.390 (6)C22—C231.366 (6)
C5—H5A0.9300C22—H22A0.9300
C6—C141.392 (5)C23—C241.399 (5)
C6—C71.452 (5)C23—H23A0.9300
C7—C81.341 (5)C24—H24A0.9300
C7—H7A0.9300C25—C261.444 (4)
C8—C91.433 (5)S1—Cu1ii2.3581 (13)
N1—Cu1—N3121.90 (14)C9—C10—H10A120.1
N1—Cu1—N4122.18 (11)C10—C11—C12119.1 (3)
N3—Cu1—N479.83 (11)C10—C11—H11A120.5
N1—Cu1—S1i105.99 (9)C12—C11—H11A120.5
N3—Cu1—S1i110.96 (8)N4—C12—C11122.4 (3)
N4—Cu1—S1i114.43 (8)N4—C12—H12A118.8
C1—Cu2—N2121.25 (14)C11—C12—H12A118.8
C1—Cu2—N6125.39 (12)N4—C13—C9123.2 (3)
N2—Cu2—N698.99 (11)N4—C13—C14117.7 (3)
C1—Cu2—N5117.10 (13)C9—C13—C14119.0 (3)
N2—Cu2—N5106.65 (12)N3—C14—C6123.4 (3)
N6—Cu2—N578.93 (11)N3—C14—C13116.6 (3)
N1—C1—Cu2178.3 (4)C6—C14—C13120.1 (3)
C2—N2—Cu2178.7 (3)N5—C15—C16123.6 (3)
C3—N3—C14116.5 (3)N5—C15—H15A118.2
C3—N3—Cu1130.5 (2)C16—C15—H15A118.2
C14—N3—Cu1112.9 (2)C17—C16—C15119.9 (4)
C12—N4—C13118.2 (3)C17—C16—H16A120.1
C12—N4—Cu1129.0 (2)C15—C16—H16A120.1
C13—N4—Cu1112.6 (2)C16—C17—C18118.8 (4)
C15—N5—C26116.2 (3)C16—C17—H17A120.6
C15—N5—Cu2130.6 (2)C18—C17—H17A120.6
C26—N5—Cu2113.1 (2)C26—C18—C17117.9 (3)
C24—N6—C25118.3 (3)C26—C18—C19120.1 (4)
C24—N6—Cu2128.5 (3)C17—C18—C19122.0 (4)
C25—N6—Cu2113.0 (2)C20—C19—C18119.6 (4)
C1—N1—Cu1172.5 (4)C20—C19—H19A120.2
N2—C2—S1177.3 (3)C18—C19—H19A120.2
N3—C3—C4124.4 (4)C19—C20—C21122.5 (3)
N3—C3—H3A117.8C19—C20—H20A118.7
C4—C3—H3A117.8C21—C20—H20A118.7
C3—C4—C5118.9 (4)C22—C21—C20124.2 (3)
C3—C4—H4A120.5C22—C21—C25116.8 (4)
C5—C4—H4A120.5C20—C21—C25118.9 (3)
C4—C5—C6119.4 (4)C23—C22—C21119.7 (3)
C4—C5—H5A120.3C23—C22—H22A120.1
C6—C5—H5A120.3C21—C22—H22A120.1
C14—C6—C5117.5 (3)C22—C23—C24119.5 (4)
C14—C6—C7119.4 (3)C22—C23—H23A120.2
C5—C6—C7123.1 (4)C24—C23—H23A120.2
C8—C7—C6120.1 (3)N6—C24—C23122.7 (4)
C8—C7—H7A119.9N6—C24—H24A118.7
C6—C7—H7A119.9C23—C24—H24A118.7
C7—C8—C9122.2 (3)N6—C25—C21122.9 (3)
C7—C8—H8A118.9N6—C25—C26118.4 (3)
C9—C8—H8A118.9C21—C25—C26118.7 (3)
C10—C9—C13117.4 (3)N5—C26—C18123.6 (3)
C10—C9—C8123.4 (3)N5—C26—C25116.4 (3)
C13—C9—C8119.1 (3)C18—C26—C25120.0 (3)
C11—C10—C9119.7 (3)C2—S1—Cu1ii102.69 (12)
C11—C10—H10A120.1
N2—Cu2—C1—N1−122 (11)Cu1—N4—C13—C144.5 (3)
N6—Cu2—C1—N1107 (11)C10—C9—C13—N4−0.5 (4)
N5—Cu2—C1—N111 (11)C8—C9—C13—N4179.1 (3)
C1—Cu2—N2—C2178 (100)C10—C9—C13—C14−179.2 (3)
N6—Cu2—N2—C2−41 (13)C8—C9—C13—C140.3 (4)
N5—Cu2—N2—C240 (13)C3—N3—C14—C6−1.2 (5)
N1—Cu1—N3—C359.4 (4)Cu1—N3—C14—C6175.1 (3)
N4—Cu1—N3—C3−178.9 (3)C3—N3—C14—C13178.9 (3)
S1i—Cu1—N3—C3−66.5 (3)Cu1—N3—C14—C13−4.8 (4)
N1—Cu1—N3—C14−116.3 (2)C5—C6—C14—N3−0.3 (5)
N4—Cu1—N3—C145.5 (2)C7—C6—C14—N3−179.0 (3)
S1i—Cu1—N3—C14117.9 (2)C5—C6—C14—C13179.6 (4)
N1—Cu1—N4—C12−58.1 (3)C7—C6—C14—C130.9 (5)
N3—Cu1—N4—C12−179.6 (3)N4—C13—C14—N30.2 (4)
S1i—Cu1—N4—C1271.9 (3)C9—C13—C14—N3179.0 (3)
N1—Cu1—N4—C13116.1 (2)N4—C13—C14—C6−179.7 (3)
N3—Cu1—N4—C13−5.3 (2)C9—C13—C14—C6−0.9 (4)
S1i—Cu1—N4—C13−113.87 (19)C26—N5—C15—C16−0.8 (5)
C1—Cu2—N5—C15−55.7 (3)Cu2—N5—C15—C16179.4 (3)
N2—Cu2—N5—C1583.8 (3)N5—C15—C16—C17−0.3 (6)
N6—Cu2—N5—C15−180.0 (3)C15—C16—C17—C182.0 (6)
C1—Cu2—N5—C26124.4 (2)C16—C17—C18—C26−2.6 (5)
N2—Cu2—N5—C26−96.0 (2)C16—C17—C18—C19176.6 (4)
N6—Cu2—N5—C260.2 (2)C26—C18—C19—C202.5 (5)
C1—Cu2—N6—C2467.3 (3)C17—C18—C19—C20−176.7 (4)
N2—Cu2—N6—C24−71.8 (3)C18—C19—C20—C21−3.5 (6)
N5—Cu2—N6—C24−177.2 (3)C19—C20—C21—C22−178.3 (4)
C1—Cu2—N6—C25−117.6 (2)C19—C20—C21—C251.4 (5)
N2—Cu2—N6—C25103.2 (2)C20—C21—C22—C23178.7 (3)
N5—Cu2—N6—C25−2.1 (2)C25—C21—C22—C23−0.9 (5)
Cu2—C1—N1—Cu1−39 (13)C21—C22—C23—C240.3 (6)
N3—Cu1—N1—C1−177 (2)C25—N6—C24—C23−0.6 (5)
N4—Cu1—N1—C185 (2)Cu2—N6—C24—C23174.2 (3)
S1i—Cu1—N1—C1−49 (2)C22—C23—C24—N60.5 (6)
Cu2—N2—C2—S1−66 (17)C24—N6—C25—C21−0.2 (4)
C14—N3—C3—C42.1 (6)Cu2—N6—C25—C21−175.7 (2)
Cu1—N3—C3—C4−173.4 (3)C24—N6—C25—C26179.4 (3)
N3—C3—C4—C5−1.3 (8)Cu2—N6—C25—C263.9 (3)
C3—C4—C5—C6−0.3 (8)C22—C21—C25—N60.9 (5)
C4—C5—C6—C141.1 (7)C20—C21—C25—N6−178.7 (3)
C4—C5—C6—C7179.7 (4)C22—C21—C25—C26−178.7 (3)
C14—C6—C7—C8−0.4 (6)C20—C21—C25—C261.7 (4)
C5—C6—C7—C8−179.0 (4)C15—N5—C26—C180.1 (5)
C6—C7—C8—C9−0.2 (6)Cu2—N5—C26—C18180.0 (2)
C7—C8—C9—C10179.7 (4)C15—N5—C26—C25−178.1 (3)
C7—C8—C9—C130.2 (5)Cu2—N5—C26—C251.8 (3)
C13—C9—C10—C11−0.1 (5)C17—C18—C26—N51.6 (5)
C8—C9—C10—C11−179.7 (3)C19—C18—C26—N5−177.7 (3)
C9—C10—C11—C120.6 (5)C17—C18—C26—C25179.7 (3)
C13—N4—C12—C11−0.2 (5)C19—C18—C26—C250.5 (5)
Cu1—N4—C12—C11173.8 (2)N6—C25—C26—N5−3.8 (4)
C10—C11—C12—N4−0.4 (5)C21—C25—C26—N5175.8 (3)
C12—N4—C13—C90.6 (4)N6—C25—C26—C18177.9 (3)
Cu1—N4—C13—C9−174.3 (2)C21—C25—C26—C18−2.5 (4)
C12—N4—C13—C14179.4 (3)N2—C2—S1—Cu1ii163 (6)
  3 in total

1.  Helicates as Versatile Supramolecular Complexes.

Authors:  Claude Piguet; Gérald Bernardinelli; Gérard Hopfgartner
Journal:  Chem Rev       Date:  1997-10-01       Impact factor: 60.622

2.  An investigation of the self-assembly of neutral, interlaced, triple-stranded molecular braids.

Authors:  Xin-Jun Luan; Xue-Hua Cai; Yao-Yu Wang; Dong-Sheng Li; Cui-Juan Wang; Ping Liu; Huai-Ming Hu; Qi-Zhen Shi; Shie-Ming Peng
Journal:  Chemistry       Date:  2006-08-16       Impact factor: 5.236

3.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

  3 in total

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