phw1106_twin1_hklf4

Crystal Submitted by:
LC
Crystal Submitted on:
20/4/2011
Data Collected on:
27/42011
Structure Solved by:
RJT

Table 1: Crystal data and structure refinement for phw1106_twin1_hklf4
Identification code phw1106_twin1_hklf4
Empirical formula C24H30N6Cl4Co2
Formula weight 662.20
Temperature / K 110.0
Crystal system monoclinic
Space group P21
a / Å, b / Å, c / Å 9.6223(3), 14.7571(3), 10.6813(3)
α/°, β/°, γ/° 90.00, 115.949(4), 90.00
Volume / Å3 1363.82(7)
Z 2
ρcalc / mg mm-3 1.613
μ / mm‑1 1.634
F(000) 676
Crystal size / mm3 0.06 × 0.04 × 0.04
2Θ range for data collection 6.96 to 58.22°
Index ranges -12 ≤ h ≤ 12, -20 ≤ k ≤ 19, -14 ≤ l ≤ 14
Reflections collected 13897
Independent reflections 5903[R(int) = 0.0319]
Data/restraints/parameters 5903/1/334
Goodness-of-fit on F2 1.040
Final R indexes [I>2σ (I)] R1 = 0.0349, wR2 = 0.0835
Final R indexes [all data] R1 = 0.0417, wR2 = 0.0854
Largest diff. peak/hole / e Å-3 0.472/-0.694

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1106_twin1_hklf4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C1-1078(4)1779(3)6742(4)22.8(9)
C2-1375(4)1494(3)5278(4)25.2(9)
C3-680(4)595(3)5176(4)23.4(8)
C4-1143(4)-144(3)5924(4)23.4(9)
C5-837(4)99(3)7402(4)19.7(8)
C6-1520(4)1018(3)7460(4)24.0(8)
C7965(4)2904(3)7174(4)21.5(8)
C82650(4)2976(2)7573(3)17.5(7)
C93357(5)3805(3)7707(4)25.8(9)
C104891(6)3846(3)7965(5)34.5(11)
C115683(5)3052(3)8094(4)32.9(10)
C124915(4)2240(3)7969(4)20.6(8)
C131751(5)-79(3)5350(4)23.1(8)
C143377(5)-257(2)6382(4)20.9(8)
C154343(5)-822(3)6085(5)27.1(10)
C165761(5)-1056(3)7135(6)33.6(11)
C176207(5)-699(3)8451(5)29(1)
C185227(5)-113(3)8668(4)23.6(8)
C191181(4)56(3)9813(4)18.6(8)
C202480(4)677(2)10694(4)15.2(7)
C212855(4)789(3)12089(4)18.1(8)
C224071(4)1335(3)12896(4)21.7(8)
C234897(4)1758(3)12297(4)21.0(8)
C244457(4)1622(3)10893(4)20.9(8)
Co12231.2(5)1010.7(3)7872.6(4)12.67(11)
N1552(4)2039(2)7607(3)18.5(7)
N21034(4)685(2)5722(3)18.6(7)
N3851(4)59(2)8326(3)16.0(6)
N43427(3)2201(2)7718(3)15.3(6)
N53825(3)107(2)7661(3)16.1(6)
N63267(3)1097(2)10089(3)15.1(6)
Cl37756.5(11)3111.0(6)2057.7(10)23.0(2)
Cl410305.7(10)2821.8(6)333.6(9)21.31(19)
Cl511742.1(10)2388.5(6)4099.5(9)20.04(19)
Cl68809.0(11)784.7(6)1527.1(10)22.4(2)
Co29657.2(5)2238.1(3)1983.6(5)15.65(12)

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1106_twin1_hklf4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
C110.8(18)27(2)30(2)9.4(17)8.4(16)6.8(15)
C211.5(19)35(2)25(2)12.4(18)3.8(16)-1.9(15)
C322(2)29(2)16.8(19)-0.6(16)6.8(16)-8.5(16)
C416.3(19)28(2)18.4(19)-2.5(16)1.0(15)-11.3(16)
C516.1(19)22(2)22.8(19)0.8(16)10.2(16)-5.6(15)
C615.7(18)29(2)29(2)4.9(19)11.2(15)-2.1(18)
C727(2)14.0(18)25.1(19)5.5(16)12.2(16)2.8(16)
C826(2)15.7(18)9.4(15)-0.7(14)6.9(14)-1.2(15)
C929(2)17(2)26(2)-0.8(16)7.2(18)-6.7(16)
C1034(3)19(2)46(3)-0.3(19)14(2)-12.0(19)
C1129(2)34(3)32(2)4.5(19)9.6(19)-14.5(19)
C1216.3(18)24.4(19)26.0(19)3.0(17)13.9(15)-3.6(17)
C1334(2)22.3(19)17.6(18)-7.7(16)15.8(17)-10.1(17)
C1427(2)18(2)28(2)-2.3(15)21.1(17)-4.4(15)
C1529(2)23(2)40(2)-10.6(18)26(2)-11.2(18)
C1635(3)19(2)68(3)-7(2)42(3)-4.4(18)
C1719(2)23(2)51(3)3.2(19)21(2)0.1(16)
C1821(2)21.0(19)31(2)1.2(17)13.9(17)-2.0(15)
C1921.4(19)17.9(19)18.6(18)-1.0(15)10.9(15)-4.2(15)
C2013.4(17)13.3(17)19.5(18)1.4(14)7.9(14)2.6(13)
C2114.8(18)20(2)21.6(18)3.6(15)9.8(15)5.5(14)
C2218.2(19)30(2)15.3(18)-0.5(15)5.3(15)6.8(16)
C2316.3(19)24(2)16.2(18)-0.5(15)1.0(15)0.0(15)
C2418(2)24(2)18.8(19)0.0(15)6.4(15)-3.4(15)
Co113.0(2)12.9(2)13.2(2)0.32(19)6.80(18)-0.78(19)
N120.2(16)19.2(17)17.6(15)4.6(13)9.9(13)2.0(13)
N220.1(17)19.0(16)17.7(16)3.5(13)9.2(13)-2.2(13)
N314.7(16)17.1(16)19.0(16)-0.9(13)10.0(13)0.1(12)
N418.1(14)14.8(15)13.0(13)-2.4(12)6.8(11)-3.2(13)
N517.4(16)14.6(16)21.5(16)1.4(13)13.5(13)-2.7(12)
N614.9(14)13.7(15)17.0(14)-0.1(12)7.3(11)1.0(12)
Cl320.6(5)19.0(5)35.6(5)-1.4(4)18.1(4)0.6(3)
Cl427.4(5)19.9(5)22.9(4)2.4(4)16.8(4)0.9(4)
Cl521.6(4)20.1(5)18.2(4)-0.9(3)8.5(3)-3.2(3)
Cl626.0(5)17.5(5)28.4(5)-5.8(3)16.3(4)-6.0(3)
Co217.0(3)14.7(2)17.3(2)-0.9(2)9.50(19)-0.7(2)

Table 4 Bond Lengths for phw1106_twin1_hklf4.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.521(6) C16C171.382(6)
C1C61.521(5) C17C181.373(6)
C1N11.481(5) C18N51.346(5)
C2C31.511(6) C19C201.503(5)
C3C41.529(5) C19N31.477(5)
C3N21.495(5) C20C211.381(5)
C4C51.517(5) C20N61.342(5)
C5C61.521(6) C21C221.372(5)
C5N31.487(5) C22C231.369(6)
C7C81.488(5) C23C241.383(5)
C7N11.471(5) C24N61.337(5)
C8C91.376(5) Co1N12.143(3)
C8N41.338(5) Co1N22.126(3)
C9C101.379(7) Co1N32.129(3)
C10C111.372(7) Co1N42.146(3)
C11C121.382(6) Co1N52.118(3)
C12N41.338(5) Co1N62.133(3)
C13C141.491(6) Cl3Co22.2665(10)
C13N21.464(5) Cl4Co22.2804(10)
C14C151.385(5) Cl5Co22.2834(10)
C14N51.351(5) Cl6Co22.2705(10)
C15C161.378(7)    

Table 5 Bond Angles for phw1106_twin1_hklf4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2C1C6110.2(3) N2Co1N389.98(12)
N1C1C2112.6(3) N2Co1N499.06(12)
N1C1C6109.3(3) N2Co1N6169.10(12)
C3C2C1115.3(3) N3Co1N189.31(12)
C2C3C4110.4(3) N3Co1N4165.09(12)
N2C3C2109.9(3) N3Co1N679.73(11)
N2C3C4112.5(3) N5Co1N1166.15(12)
C5C4C3114.0(3) N5Co1N279.48(12)
C4C5C6111.3(3) N5Co1N399.34(12)
N3C5C4109.9(3) N5Co1N493.98(12)
N3C5C6111.9(3) N5Co1N698.52(11)
C5C6C1114.7(3) N6Co1N193.62(12)
N1C7C8112.5(3) N6Co1N491.76(11)
C9C8C7121.3(3) C1N1Co1115.5(2)
N4C8C7117.1(3) C7N1C1112.8(3)
N4C8C9121.5(4) C7N1Co1111.4(2)
C8C9C10119.8(4) C3N2Co1115.2(2)
C11C10C9118.8(4) C13N2C3113.3(3)
C10C11C12118.7(4) C13N2Co1111.7(2)
N4C12C11122.5(4) C5N3Co1115.6(2)
N2C13C14113.7(3) C19N3C5111.9(3)
C15C14C13122.0(4) C19N3Co1112.6(2)
N5C14C13116.4(3) C8N4Co1114.7(2)
N5C14C15121.5(4) C12N4C8118.8(3)
C16C15C14119.3(4) C12N4Co1125.6(3)
C15C16C17119.3(4) C14N5Co1115.7(3)
C18C17C16118.8(4) C18N5C14118.5(3)
N5C18C17122.6(4) C18N5Co1125.8(3)
N3C19C20113.6(3) C20N6Co1114.7(2)
C21C20C19120.1(3) C24N6C20117.6(3)
N6C20C19118.0(3) C24N6Co1126.9(3)
N6C20C21121.9(3) Cl3Co2Cl4108.07(4)
C22C21C20119.7(3) Cl3Co2Cl5106.45(4)
C23C22C21119.0(3) Cl3Co2Cl6108.94(4)
C22C23C24118.4(4) Cl4Co2Cl5108.01(4)
N6C24C23123.4(4) Cl6Co2Cl4112.65(4)
N1Co1N478.95(12) Cl6Co2Cl5112.46(4)
N2Co1N189.80(13)     

Table 6 Torsion Angles for phw1106_twin1_hklf4.
ABCDAngle/˚
C1C2C3C451.9(4)
C1C2C3N2-72.8(4)
C2C1C6C550.5(4)
C2C1N1C771.0(4)
C2C1N1Co1-58.6(4)
C2C3C4C5-51.3(4)
C2C3N2C13-165.7(3)
C2C3N2Co163.9(4)
C3C4C5C651.2(4)
C3C4C5N3-73.3(4)
C4C3N2C1370.8(4)
C4C3N2Co1-59.6(4)
C4C5C6C1-51.2(4)
C4C5N3C19-165.3(3)
C4C5N3Co164.0(3)
C6C1C2C3-51.4(4)
C6C1N1C7-166.2(3)
C6C1N1Co164.2(4)
C6C5N3C1970.6(4)
C6C5N3Co1-60.1(3)
C7C8C9C10-174.7(4)
C7C8N4C12174.9(3)
C7C8N4Co1-15.4(4)
C8C7N1C1-155.1(3)
C8C7N1Co1-23.4(4)
C8C9C10C11-0.5(7)
C9C8N4C12-1.4(5)
C9C8N4Co1168.3(3)
C9C10C11C12-0.5(6)
C10C11C12N40.6(6)
C11C12N4C80.4(5)
C11C12N4Co1-168.1(3)
C13C14C15C16-171.5(4)
C13C14N5C18173.1(3)
C13C14N5Co1-8.1(4)
C14C13N2C3-151.0(3)
C14C13N2Co1-18.8(4)
C14C15C16C17-2.0(6)
C15C14N5C18-2.0(5)
C15C14N5Co1176.7(3)
C15C16C17C18-0.6(6)
C16C17C18N52.0(6)
C17C18N5C14-0.7(6)
C17C18N5Co1-179.3(3)
C19C20C21C22178.1(3)
C19C20N6C24-177.6(3)
C19C20N6Co111.7(4)
C20C19N3C5-135.9(3)
C20C19N3Co1-3.7(4)
C20C21C22C23-0.3(6)
C21C20N6C241.2(5)
C21C20N6Co1-169.5(3)
C21C22C23C240.7(6)
C22C23C24N6-0.2(6)
C23C24N6C20-0.8(6)
C23C24N6Co1168.6(3)
N1C1C2C370.9(4)
N1C1C6C5-73.8(4)
N1C7C8C9-157.5(4)
N1C7C8N426.2(4)
N1Co1N2C3-46.2(3)
N1Co1N2C13-177.4(2)
N1Co1N3C543.8(3)
N1Co1N3C19-86.5(3)
N1Co1N4C81.4(2)
N1Co1N4C12170.4(3)
N1Co1N5C14-41.8(6)
N1Co1N5C18136.9(5)
N1Co1N6C2078.1(3)
N1Co1N6C24-91.5(3)
N2C3C4C571.9(4)
N2C13C14C15-166.8(3)
N2C13C14N518.1(5)
N2Co1N1C143.3(3)
N2Co1N1C7-87.0(3)
N2Co1N3C5-46.0(3)
N2Co1N3C19-176.3(3)
N2Co1N4C889.5(2)
N2Co1N4C12-101.6(3)
N2Co1N5C14-1.9(3)
N2Co1N5C18176.7(3)
N2Co1N6C20-30.0(8)
N2Co1N6C24160.4(6)
N3C5C6C172.2(4)
N3C19C20C21175.9(3)
N3C19C20N6-5.3(5)
N3Co1N1C1-46.7(3)
N3Co1N1C7-177.0(2)
N3Co1N2C343.1(3)
N3Co1N2C13-88.1(2)
N3Co1N4C8-37.2(6)
N3Co1N4C12131.7(4)
N3Co1N5C1486.3(3)
N3Co1N5C18-95.0(3)
N3Co1N6C20-10.5(2)
N3Co1N6C24179.8(3)
N4C8C9C101.5(6)
N4Co1N1C1142.6(3)
N4Co1N1C712.3(2)
N4Co1N2C3-125.0(3)
N4Co1N2C13103.8(2)
N4Co1N3C581.6(5)
N4Co1N3C19-48.7(6)
N4Co1N5C14-100.4(3)
N4Co1N5C1878.3(3)
N4Co1N6C20157.2(3)
N4Co1N6C24-12.5(3)
N5C14C15C163.4(5)
N5Co1N1C182.4(6)
N5Co1N1C7-48.0(6)
N5Co1N2C3142.6(3)
N5Co1N2C1311.4(2)
N5Co1N3C5-125.3(3)
N5Co1N3C19104.3(2)
N5Co1N4C8169.4(2)
N5Co1N4C12-21.6(3)
N5Co1N6C20-108.5(2)
N5Co1N6C2481.8(3)
N6C20C21C22-0.6(5)
N6Co1N1C1-126.3(3)
N6Co1N1C7103.4(2)
N6Co1N2C362.2(7)
N6Co1N2C13-69.0(7)
N6Co1N3C5137.6(3)
N6Co1N3C197.3(2)
N6Co1N4C8-91.9(2)
N6Co1N4C1277.0(3)
N6Co1N5C14167.2(3)
N6Co1N5C18-14.1(3)

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1106_twin1_hklf4.
AtomxyzU(eq)
H1-17452315666827
H2A-25061465469830
H2B-9611969488030
H3-1110427416928
H4A-2259-274538228
H4B-569-706594528
H5-1355-367773424
H6A-11811185844829
H6B-2660964702429
H7A6533409760726
H7B3852966615126
H927904347762231
H1053904414805341
H1167383059826440
H1254651690806725
H13A173243443128
H13B1128-630525828
H154031-1047516833
H166424-1459695740
H177176-855919135
H185549148956628
H19A1443-5691017722
H19B236239989722
H2122734881248922
H22433714201385626
H23575321351283325
H24502919171047825
H1A 730.0(5) 2120.0(3) 8410.0(4)22
H2 1140.0(5) 1110.0(3) 5380.0(5)22
H3A 1140.0(5)-500.0(3) 8270.0(4)19

[RSC Journal Format]

Experimental

Single crystals of C24H30N6Cl4Co2 [phw1106_twin1_hklf4] were recrystallised from [solvents] mounted in inert oil and transferred to the cold gas stream of the diffractometer.

Crystal structure determination of [phw1106_twin1_hklf4]

Crystal Data. C24H30N6Cl4Co2, =662.20, monoclinic, a = 9.6223(3) Å, b = 14.7571(3) Å, c = 10.6813(3) Å, β = 115.949(4)°, = 1363.82(7) Å3, T = 110.0, space group P21 (no. 4), Z = 2, μ(Mo Kα) = 1.634, 13897 reflections measured, 5903 unique (Rint = 0.0319) which were used in all calculations. The final wR(F2) was 0.0854 (all data).

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