phw1103

Crystal Submitted by:
Luisa Ciano
Crystal Submitted on:
Data Collected on:
24/03/2011
Structure Solved by:
Adrian Whitwood

Table 1: Crystal data and structure refinement for phw1103
Identification code phw1103
Empirical formula C29H39Cl2CoN6O2.5
Formula weight 641.49
Temperature / K 110.0
Crystal system monoclinic
Space group P21/n
a / Å, b / Å, c / Å 11.3868(9), 14.0237(11), 19.2597(15)
α/°, β/°, γ/° 90.00, 99.711(9), 90.00
Volume / Å3 3031.4(4)
Z 4
ρcalc / mg mm-3 1.406
μ / mm‑1 0.782
F(000) 1344
Crystal size / mm3 0.3941 × 0.1767 × 0.0965
2Θ range for data collection 5.82 to 55.9°
Index ranges -14 ≤ h ≤ 14, -17 ≤ k ≤ 12, -24 ≤ l ≤ 21
Reflections collected 12340
Independent reflections 6108[R(int) = 0.0218]
Data/restraints/parameters 6108/6/382
Goodness-of-fit on F2 1.043
Final R indexes [I>2σ (I)] R1 = 0.0497, wR2 = 0.1215
Final R indexes [all data] R1 = 0.0589, wR2 = 0.1284
Largest diff. peak/hole / e Å-3 1.412/-0.735

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1103. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C14742(3)790(2)3150.1(15)22.5(6)
C24175(3)873(2)2375.9(15)23.5(6)
C34087(3)1902(2)2109.7(15)23.4(6)
C45312(3)2385(2)2259.0(16)23.9(6)
C55904(3)2326(2)3034.6(15)21.6(6)
C65950(3)1300(2)3300.9(15)22.6(6)
C73783(3)738(2)4146.2(15)22.1(6)
C83203(2)1220(2)4672.3(15)21.3(6)
C92916(3)729(2)5245.6(16)26.3(7)
C102477(3)1239(3)5765.0(16)30.2(7)
C112379(3)2218(3)5694.8(16)28.6(7)
C122666(3)2651(2)5100.3(15)23.3(6)
C132193(3)2609(2)2097.1(15)21.2(6)
C141249(3)2933(2)2475.0(15)20.1(6)
C15107(3)3151(2)2127.8(16)25.3(7)
C16-762(3)3385(2)2526.0(17)27.8(7)
C17-467(3)3388(2)3251.5(17)25.6(7)
C18694(3)3151(2)3557.3(16)22.6(6)
C195626(3)3759(2)3634.3(15)21.7(6)
C204841(3)4436(2)3909.5(15)20.5(6)
C215231(3)5344(2)4116.6(16)25.6(7)
C224438(3)5969(2)4345.6(17)29.6(7)
C233285(3)5670(2)4346.9(17)29.4(7)
C242952(3)4751(2)4119.9(16)25.0(6)
Co13444.9(3)2643.8(3)3564.89(19)16.18(12)
N13975(2)1208.4(16)3615.0(12)18.1(5)
N23201(2)2398.7(17)2454.1(12)19.8(5)
N35212(2)2943.6(17)3435.3(12)19.2(5)
N43051(2)2169.3(18)4582.7(12)19.6(5)
N51550(2)2935.9(17)3186.5(12)19.3(5)
N63711(2)4133.8(17)3905.5(13)20.6(5)
C258773(5)1852(4)4694(3)48.0(14)
C269238(6)1542(5)5433(3)65.6(17)
O17896(17)2590(15)4630(8)65(3)
C25A8971(15)2276(10)5116(9)48.0(14)
C26A9359(18)1343(11)4838(11)65.6(17)
O1A 8040.0(5) 2530.0(5) 4560.0(2)65(3)
C275406(6)5468(4)1841(3)81.0(17)
C284276(5)5345(4)2068(3)73.2(16)
O26274(3)4756(2)2078.9(19)55.4(8)
C299645(11)4652(8)5017(4)68(2)
C3010107(11)5612(8)4832(6)68(2)
O39563(6)4621(5)5741(3)64.0(18)
Cl13987.1(7)8355.0(5)4663.6(4)24.84(18)
Cl27867.1(8)5529.5(7)3394.1(6)46.0(3)

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1103. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
C127.8(15)16.8(14)23.9(15)-2.5(12)7.3(12)3.4(12)
C229.2(16)22.6(15)19.7(14)-7.8(12)7.0(12)1.5(12)
C327.5(15)27.4(16)15.4(13)-2.0(12)4.6(11)3.0(13)
C427.7(16)25.1(16)21.2(15)1.6(12)10.7(12)2.8(12)
C519.6(14)23.9(15)22.2(14)-2.6(12)6.5(11)-0.3(12)
C624.1(15)23.2(15)20.7(14)-2.9(12)4.5(11)6.8(12)
C724.4(15)17.3(14)24.2(15)1.1(12)2.8(12)-1.3(11)
C818.1(13)24.9(16)19.5(14)-0.2(12)-0.8(11)-1.1(11)
C923.0(15)32.1(17)23.6(15)4.9(13)3.2(12)-5.6(13)
C1022.2(15)48(2)20.6(15)2.3(14)3.2(12)-9.2(14)
C1119.6(15)47(2)19.8(15)-7.3(14)4.3(12)-3.2(14)
C1217.8(14)31.0(17)20.3(14)-6.2(13)0.9(11)-0.4(12)
C1328.0(15)18.7(14)16.0(13)0.4(11)1.0(11)-0.8(12)
C1423.3(14)15.5(14)20.5(14)-1.0(12)0.6(11)-1.3(11)
C1527.9(16)22.4(16)23.2(15)2.9(13)-2.2(12)1.7(12)
C1622.8(15)27.6(17)31.1(17)4.5(14)-1.2(13)3.0(12)
C1721.6(15)25.6(16)29.5(16)-0.5(13)4.4(12)1.7(12)
C1822.5(15)22.3(15)22.5(15)-3.2(12)1.9(12)-1.6(12)
C1923.7(15)21.6(15)19.2(14)1.5(12)2.1(11)-2.9(12)
C2026.9(15)17.4(14)16.2(13)3.4(11)0.2(11)-1.5(11)
C2135.9(17)18.5(15)21.2(15)1.9(12)0.9(13)-6.8(13)
C2244.4(19)15.8(15)25.6(16)0.3(13)-2.5(14)-2.3(13)
C2339.2(18)19.6(15)26.1(16)-2.5(13)-4.0(14)10.8(14)
C2424.9(15)22.3(15)25.7(15)-3.4(13)-1.5(12)3.9(12)
Co118.2(2)14.8(2)15.2(2)-1.93(14)1.98(14)0.69(14)
N122.5(12)14.1(11)17.5(11)-1.3(10)3.1(9)-1.4(9)
N224.0(13)19.0(12)16.8(11)0(1)4.6(10)1.9(10)
N320.8(12)18.0(12)18.6(12)0.4(10)2.8(9)1.7(10)
N417.3(11)23.8(13)17.3(12)-2(1)1.7(9)-0.2(10)
N518.8(12)18.8(12)19.3(12)-2.4(10)0.3(9)-1.3(9)
N625.1(12)15.0(12)19.8(12)-0.7(10)-1.7(10)1.9(10)
C2553(3)41(3)56(3)-9(3)31(3)-14(3)
O158(5)56(3)84(4)13(3)21(4)-7(2)
C25A53(3)41(3)56(3)-9(3)31(3)-14(3)
O1A58(5)56(3)84(4)13(3)21(4)-7(2)
C27103(5)44(3)91(4)23(3)1(4)-5(3)
C2892(4)61(3)67(3)16(3)17(3)33(3)
O270(2)41.0(17)61(2)-8.6(16)26.1(18)-1.8(15)
O362(4)79(5)54(4)-3(3)18(3)-1(4)
Cl129.0(4)19.3(4)24.8(4)-2.4(3)0.3(3)1.9(3)
Cl237.5(5)33.9(5)70.4(7)7.2(5)19.8(5)-4.7(4)

Table 4 Bond Lengths for phw1103.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.526(4) C18N51.336(4)
C1C61.534(4) C19C201.463(4)
C1N11.474(4) C19N31.271(4)
C2C31.529(4) C20C211.385(4)
C3C41.534(4) C20N61.354(4)
C3N21.473(4) C21C221.382(5)
C4C51.534(4) C22C231.379(5)
C5C61.525(4) C23C241.393(4)
C5N31.474(4) C24N61.336(4)
C7C81.465(4) Co1N12.099(2)
C7N11.267(4) Co1N22.138(2)
C8C91.387(4) Co1N32.111(2)
C8N41.350(4) Co1N42.187(2)
C9C101.390(5) Co1N52.197(2)
C10C111.382(5) Co1N62.196(2)
C11C121.383(5) C25C261.497(4)
C12N41.338(4) C25O11.429(5)
C13C141.468(4) C25AC26A1.508(5)
C13N21.269(4) C25AO1A1.425(5)
C14C151.392(4) C27C281.438(8)
C14N51.355(4) C27O21.425(6)
C15C161.390(5) C29C301.509(5)
C16C171.381(4) C29O31.414(5)
C17C181.393(4)    

Table 5 Bond Angles for phw1103.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2C1C6111.6(2) N1Co1N385.64(9)
N1C1C2111.5(2) N1Co1N476.58(9)
N1C1C6107.7(2) N1Co1N5116.92(9)
C1C2C3113.1(2) N1Co1N6151.02(9)
C2C3C4110.4(2) N2Co1N4146.73(9)
N2C3C2107.9(2) N2Co1N575.12(9)
N2C3C4112.2(2) N2Co1N6116.11(9)
C5C4C3113.3(2) N3Co1N283.08(9)
C6C5C4111.3(2) N3Co1N4120.68(9)
N3C5C4107.0(2) N3Co1N5145.71(9)
N3C5C6111.7(2) N3Co1N676.10(9)
C5C6C1113.4(2) N4Co1N590.89(9)
N1C7C8118.5(3) N4Co1N693.47(9)
C9C8C7121.1(3) N6Co1N589.99(9)
N4C8C7115.4(3) C1N1Co1123.28(18)
N4C8C9123.3(3) C7N1C1118.9(2)
C8C9C10118.6(3) C7N1Co1116.7(2)
C11C10C9118.3(3) C3N2Co1122.90(18)
C10C11C12119.4(3) C13N2C3119.4(2)
N4C12C11123.2(3) C13N2Co1117.3(2)
N2C13C14118.3(3) C5N3Co1123.30(18)
C15C14C13122.2(3) C19N3C5118.9(3)
N5C14C13114.9(2) C19N3Co1117.1(2)
N5C14C15122.8(3) C8N4Co1111.92(19)
C16C15C14118.8(3) C12N4C8117.0(3)
C17C16C15119.0(3) C12N4Co1131.0(2)
C16C17C18118.6(3) C14N5Co1113.69(19)
N5C18C17123.6(3) C18N5C14117.3(2)
N3C19C20118.4(3) C18N5Co1128.98(19)
C21C20C19121.1(3) C20N6Co1112.51(19)
N6C20C19115.6(3) C24N6C20117.3(3)
N6C20C21123.2(3) C24N6Co1130.2(2)
C22C21C20118.7(3) O1C25C26115.0(8)
C23C22C21118.8(3) O1AC25AC26A100(2)
C22C23C24119.3(3) O2C27C28115.2(4)
N6C24C23122.7(3) O3C29C30110.2(7)
N1Co1N283.09(9)     

Table 6 Torsion Angles for phw1103.
ABCDAngle/˚
C1C2C3C453.9(3)
C1C2C3N2-68.9(3)
C2C1C6C551.5(3)
C2C1N1C7132.4(3)
C2C1N1Co1-59.9(3)
C2C3C4C5-53.9(3)
C2C3N2C13-107.7(3)
C2C3N2Co164.8(3)
C3C4C5C652.8(3)
C3C4C5N3-69.5(3)
C4C3N2C13130.6(3)
C4C3N2Co1-56.9(3)
C4C5C6C1-51.2(3)
C4C5N3C19-102.7(3)
C4C5N3Co167.5(3)
C6C1C2C3-53.0(3)
C6C1N1C7-104.9(3)
C6C1N1Co162.8(3)
C6C5N3C19135.3(3)
C6C5N3Co1-54.5(3)
C7C8C9C10173.6(3)
C7C8N4C12-171.6(2)
C7C8N4Co110.1(3)
C8C7N1C1169.2(2)
C8C7N1Co10.7(3)
C8C9C10C11-1.8(4)
C9C8N4C123.9(4)
C9C8N4Co1-174.4(2)
C9C10C11C122.9(4)
C10C11C12N4-0.6(5)
C11C12N4C8-2.7(4)
C11C12N4Co1175.1(2)
C13C14C15C16175.3(3)
C13C14N5C18-174.7(3)
C13C14N5Co18.0(3)
C14C13N2C3168.4(3)
C14C13N2Co1-4.5(4)
C14C15C16C17-0.4(5)
C15C14N5C180.7(4)
C15C14N5Co1-176.5(2)
C15C16C17C18-0.2(5)
C16C17C18N51.2(5)
C17C18N5C14-1.4(4)
C17C18N5Co1175.3(2)
C19C20C21C22177.4(3)
C19C20N6C24-176.7(3)
C19C20N6Co15.0(3)
C20C19N3C5168.4(2)
C20C19N3Co1-2.4(3)
C20C21C22C23-1.2(4)
C21C20N6C24-0.6(4)
C21C20N6Co1-178.8(2)
C21C22C23C240.2(5)
C22C23C24N60.7(5)
C23C24N6C20-0.5(4)
C23C24N6Co1177.3(2)
N1C1C2C367.5(3)
N1C1C6C5-71.2(3)
N1C7C8C9176.7(3)
N1C7C8N4-7.7(4)
N1Co1N2C3-45.8(2)
N1Co1N2C13126.9(2)
N1Co1N3C536.1(2)
N1Co1N3C19-153.5(2)
N1Co1N4C8-7.46(18)
N1Co1N4C12174.6(3)
N1Co1N5C14-81.8(2)
N1Co1N5C18101.4(3)
N1Co1N6C2047.8(3)
N1Co1N6C24-130.1(3)
N2C3C4C566.4(3)
N2C13C14C15-178.1(3)
N2C13C14N5-2.6(4)
N2Co1N1C142.1(2)
N2Co1N1C7-149.9(2)
N2Co1N3C5-47.4(2)
N2Co1N3C19122.9(2)
N2Co1N4C846.4(3)
N2Co1N4C12-131.5(2)
N2Co1N5C14-7.72(19)
N2Co1N5C18175.4(3)
N2Co1N6C20-79.6(2)
N2Co1N6C24102.4(3)
N3C5C6C168.3(3)
N3C19C20C21-178.2(3)
N3C19C20N6-2.0(4)
N3Co1N1C1-41.4(2)
N3Co1N1C7126.6(2)
N3Co1N2C340.6(2)
N3Co1N2C13-146.7(2)
N3Co1N4C8-84.0(2)
N3Co1N4C1298.0(3)
N3Co1N5C1444.6(3)
N3Co1N5C18-132.2(2)
N3Co1N6C20-4.68(19)
N3Co1N6C24177.4(3)
N4C8C9C10-1.7(4)
N4Co1N1C1-164.4(2)
N4Co1N1C73.6(2)
N4Co1N2C3-98.1(3)
N4Co1N2C1374.5(3)
N4Co1N3C5107.7(2)
N4Co1N3C19-81.9(2)
N4Co1N5C14-157.2(2)
N4Co1N5C1826.0(3)
N4Co1N6C20116.09(19)
N4Co1N6C24-61.8(3)
N5C14C15C160.2(5)
N5Co1N1C1111.6(2)
N5Co1N1C7-80.5(2)
N5Co1N2C3-166.1(2)
N5Co1N2C136.6(2)
N5Co1N3C5-97.8(2)
N5Co1N3C1972.5(3)
N5Co1N4C8110.05(19)
N5Co1N4C12-67.9(3)
N5Co1N6C20-153.0(2)
N5Co1N6C2429.0(3)
N6C20C21C221.5(4)
N6Co1N1C1-92.0(3)
N6Co1N1C776.0(3)
N6Co1N2C3111.4(2)
N6Co1N2C13-75.9(2)
N6Co1N3C5-166.5(2)
N6Co1N3C193.8(2)
N6Co1N4C8-159.90(19)
N6Co1N4C1222.2(3)
N6Co1N5C14109.4(2)
N6Co1N5C18-67.5(3)

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1103.
AtomxyzU(eq)
H14867100327027
H2A3365593231128
H2B4651497208828
H338011897158928
H4A58412080196529
H4B52223064212029
H567352578308326
H6A62381300381627
H6B6533939307627
H7401187420227
H9301757528332
H102250923615836
H1121172590605234
H1225873324505728
H1320532558159825
H15-753141162830
H16-15473542230333
H17-10433547353631
H188873142405727
H1964253924360526
H2160275534410231
H2246846592449935
H2327246087450135
H2421534555411730
H25C94522076447758
H25D84241291442258
H26D97801001542598
H26E85711351566498
H26F96682071569498
H1B73452430484698
H25A86752191556758
H25B96212753517858
H26A87691138443598
H26B9426859520998
H26C101341427468998
H1A77572035434598
H27A52725478131997
H27B57346097200797
H28A370958171833110
H28B437554332579110
H28C397347021945110
H2 6720.0(3) 4970.0(3)2442(19)21(9)
H29A88494539473282
H29B101884144490782
H30A1024856024344102
H30B1085657515148102
H30C951961054884102
H3A98084090590896

[RSC Journal Format]

Experimental

Single crystals of C29H39Cl2CoN6O2.5 [phw1103] were recrystallised from [solvents] mounted in inert oil and transferred to the cold gas stream of the diffractometer.

Crystal structure determination of [phw1103]

Crystal Data. C29H39Cl2CoN6O2.5, =641.49, monoclinic, a = 11.3868(9) Å, b = 14.0237(11) Å, c = 19.2597(15) Å, β = 99.711(9)°, = 3031.4(4) Å3, T = 110.0, space group P21/n (no. 14), Z = 4, μ(Mo Kα) = 0.782, 12340 reflections measured, 6108 unique (Rint = 0.0218) which were used in all calculations. The final wR(F2) was 0.1284 (all data).

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