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Crystal structure determination of: mfr200004 (C20H14CuF12N6O8S6)

Table 1 : Crystal data and structure refinement for mfr200004.

Identification code mfr200004
Empirical formula C20H14CuF12N6O8S6
Formula weight 950.27
Temperature/K 100.0(2)
Crystal system triclinic
Space group P-1
a/Å 8.3285(8)
b/Å 14.6788(15)
c/Å 15.9531(16)
α/° 113.555(2)
β/° 100.232(2)
γ/° 99.398(2)
Volume/Å3 1699.0(3)
Z 2
ρcalcg/cm3 1.858
μ/mm‑1 1.042
F(000) 946.0
Crystal size/mm3 0.19 × 0.063 × 0.021
Radiation Synchrotron (λ = 0.6889)
2Θ range for data collection/° 2.802 to 53.142
Index ranges -10 ≤ h ≤ 10, -19 ≤ k ≤ 19, -20 ≤ l ≤ 20
Reflections collected 21335
Independent reflections 7697 [Rint = 0.0634, Rsigma = 0.0731]
Data/restraints/parameters 7697/443/478
Goodness-of-fit on F2 1.097
Final R indexes [I>=2σ (I)] R1 = 0.0595, wR2 = 0.1684
Final R indexes [all data] R1 = 0.0674, wR2 = 0.1721
Largest diff. peak/hole / e Å-3 1.45/-0.96

Experimental

Crystal structure data for mfr200004 was collected on a DLS_I19_upgrade diffractometer equipped with an Synchrotron (λ Synchrotron = 0.6889 Å) and an Oxford Cryosystems CryostreamPlus open-flow N2 cooling device. Cell refinement, data collection and data reduction were undertaken via software SAINT V8.40A (Bruker, 2019). Intensities were corrected for absorption using SADABS-2016/2 (Bruker,2016) was used for absorption correction. wR2(int) was 0.1442 before and 0.0890 after correction. The Ratio of minimum to maximum transmission is 0.5711. The \l/2 correction factor is Not present..

Using Olex2 (Dolomanov, 2009), the structure was solved using SHELXT 2014/5 (Sheldrick, 2014) and refined by XL (Sheldrick, 2008).

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Crystal structure determination of [mfr200004]

Crystal Data for C20H14CuF12N6O8S6 (=950.27 g/mol): triclinic, space group P-1 (no. 2), a = 8.3285(8) Å, b = 14.6788(15) Å, c = 15.9531(16) Å, α = 113.555(2)°, β = 100.232(2)°, γ = 99.398(2)°, = 1699.0(3) Å3, Z = 2, T = 100.0(2) K, μ(Synchrotron) = 1.042 mm-1, Dcalc = 1.858 g/cm3, 21335 reflections measured (2.802° ≤ 2Θ ≤ 53.142°), 7697 unique (Rint = 0.0634, Rsigma = 0.0731) which were used in all calculations. The final R1 was 0.0595 (I > 2σ(I)) and wR2 was 0.1721 (all data).

Special details of refinement:

?

Comments:

N/A

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mfr200004. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Cu12179.6(5)2603.8(3)7267.8(2)15.96(14)
S11704.4(13)1082.5(9)4174.7(6)33.4(3)
S22574.1(12)5219.3(7)10008.8(5)21.7(2)
S3-2258.9(10)2188.1(7)7189.5(6)19.8(2)
S4-3238.7(10)3979.2(7)7391.8(5)20.5(2)
S52506.1(12)6709.5(8)6940.2(6)26.8(2)
S62409.7(13)8121.0(8)8736.7(7)30.0(2)
F1-2577(3)1095.9(18)8122.9(17)38.7(6)
F2-867(3)2606.0(18)8955.9(14)31.6(5)
F3-3551(3)2437.8(17)8619.0(14)27.9(5)
F4-4564(3)4363(2)6007.5(16)44.8(7)
F5-1980(3)4304(2)6117.2(18)50.6(7)
F6-3958(4)2901(2)5549.5(15)45.2(7)
F75071(4)6578(2)6222.0(18)53.0(8)
F85580(3)7912(2)7565(2)51.5(7)
F95446(3)6434(2)7534.6(18)45.9(7)
F109(5)8968(3)9223(2)84.8(12)
F11-535(5)7971(5)7737(2)139(2)
F12-632(4)7321(3)8737(2)75.4(10)
O1-795(3)1838(2)6967.0(17)24.6(5)
O2-3881(3)1573.2(19)6540.8(16)25.3(6)
O3-4897(3)3507(2)7377.6(18)29.8(6)
O4-2526(3)5052(2)8003.5(17)26.1(6)
O51865(4)5614(2)6405.7(19)37.9(7)
O62040(4)7373(2)6531(2)38.0(7)
O72928(4)8197(2)9671.4(19)37.8(7)
O83140(6)8951(3)8563(3)66.0(12)
N11766(3)2317(2)5896.5(19)20.6(6)
N22452(3)1203(2)6741.9(19)19.0(6)
N32725(3)2381(2)8401.4(17)14.8(5)
N42165(3)3973(2)8236.5(18)16.4(6)
N5-1857(3)3380(2)7503(2)20.1(6)
N62375(4)7022(2)7991(2)26.4(7)
C11229(5)2878(3)5358(2)27.6(8)
C21610(5)2395(4)4390(3)37.1(10)
C31960(4)1428(3)5366(2)22.3(7)
C42365(4)746(3)5818(2)20.3(7)
C52675(5)-215(3)5419(3)27.6(8)
C63032(5)-684(3)6004(3)29.5(8)
C73129(5)-198(3)6961(2)24.2(7)
C82845(4)772(3)7318(2)19.1(7)
C92947(4)1473(3)8326(2)17.4(6)
C103267(4)1299(3)9123(2)22.7(7)
C113348(5)2103(3)9991(2)24.5(8)
C123123(4)3040(3)10058(2)20.1(7)
C132816(4)3159(2)9235(2)16.3(6)
C142500(4)4062(3)9090(2)16.5(6)
C151716(5)5657(3)9147(2)22.3(7)
C162052(4)4955(3)8213(2)20.0(7)
C17-2309(4)2077(3)8288(2)23.6(7)
C18-3428(5)3882(3)6196(3)33.4(9)
C194787(5)6924(3)7084(3)33.0(9)
C20137(7)8068(5)8583(3)58.0(14)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mfr200004. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Cu116.4(2)21.4(2)8.7(2)2.97(16)4.74(15)9.33(18)
S132.6(5)52.9(7)10.1(4)7.7(4)6.6(4)14.2(5)
S230.9(5)21.3(5)11.0(4)2.7(3)6.4(3)12.8(4)
S312.9(4)25.5(5)14.5(4)1.0(3)5.7(3)6.7(3)
S416.3(4)29.0(5)12.4(4)3.3(3)4.8(3)10.1(4)
S526.9(5)34.3(5)24.0(4)14.9(4)8.4(4)13.3(4)
S637.1(6)29.9(5)31.2(5)14.7(4)17.3(4)18.1(5)
F152.7(16)30.7(13)36.1(13)13.7(10)18.2(12)15.3(12)
F218.9(11)48.6(15)21.2(10)10.5(10)3.8(8)8.1(10)
F319.7(11)38.0(13)23.8(10)7.9(9)12.4(9)10.2(9)
F456.7(17)54.9(16)23.9(12)14.0(11)2.5(11)35.2(14)
F548.7(16)80(2)38.2(14)34.4(14)24.3(13)20.3(15)
F665.0(18)44.5(15)14.7(10)0.0(10)4.6(11)26.5(13)
F751.5(17)87(2)38.4(14)31.7(15)29.8(13)33.5(16)
F833.6(14)48.0(17)66.7(19)19.4(14)17.4(13)6.1(12)
F944.5(15)68.4(18)39.8(14)28.3(13)15.9(12)36.2(14)
F10114(3)121(3)75(2)54(2)65(2)101(3)
F11106(3)326(7)51(2)97(3)47(2)162(4)
F1239.2(18)106(3)65(2)17(2)28.3(16)13.6(18)
O114.9(12)29.6(14)21.5(12)0.8(10)8.8(10)9.4(11)
O217.4(12)27.3(14)17.9(12)-2.1(10)3.7(10)4.3(10)
O317.7(13)37.8(16)30.5(14)7.8(12)10.8(11)12.9(12)
O428.0(14)27.0(14)17.6(12)3.7(10)4.3(10)11.1(11)
O546.7(18)37.9(17)22.9(14)8.7(12)8.6(13)8.0(14)
O640.6(17)51.3(19)36.8(16)28.1(15)13.3(13)24.5(15)
O738.9(17)40.7(18)27.9(14)10.3(12)4.9(12)12.9(14)
O8121(4)29.4(19)66(2)23.6(17)59(3)25(2)
N114.5(14)33.0(17)12.7(12)7.7(11)3.0(11)8.7(13)
N213.6(13)23.6(15)13.7(12)1.0(11)4.5(10)7.6(12)
N313.4(13)20.3(14)9.5(11)4.4(10)1.8(10)8.8(11)
N414.9(13)21.4(15)13.6(12)5.3(10)6.6(10)9.2(11)
N512.8(13)24.0(16)18.7(13)4.8(11)3.7(11)5.2(12)
N629.9(17)28.8(17)27.0(16)14.3(13)12.6(13)13.7(14)
C130(2)41(2)16.6(16)15.0(16)7.2(15)13.7(18)
C235(2)65(3)18.3(17)22.7(19)8.9(16)17(2)
C312.3(16)34(2)12.5(15)3.5(13)3.4(12)3.4(14)
C414.4(16)24.0(18)13.1(14)-1.1(12)5.8(12)2.6(14)
C523.9(19)30(2)19.4(17)0.1(14)7.8(14)9.6(16)
C630(2)24(2)27.9(19)1.4(15)10.4(16)13.6(17)
C722.9(18)21.0(18)24.2(17)4.9(14)6.1(14)7.9(15)
C814.1(16)24.1(18)15.7(15)3.9(13)5.5(12)7.8(14)
C914.6(16)20.3(17)14.5(14)2.7(12)6.1(12)8.0(13)
C1024.2(18)24.8(19)22.4(16)10.8(14)7.3(14)12.3(15)
C1128.1(19)34(2)14.4(15)10.5(14)6.8(14)13.7(17)
C1220.7(17)24.8(18)10.8(14)2.2(13)6.5(13)8.2(14)
C1311.3(15)18.3(17)15.0(14)2.1(12)5.1(12)4.5(13)
C1413.4(15)22.5(17)13.2(14)4.8(12)6.6(12)8.4(13)
C1530.0(19)23.8(18)18.8(16)10.3(14)8.3(14)17.3(16)
C1623.7(18)22.7(18)15.0(15)7.2(13)7.3(13)10.4(15)
C1720.2(17)26.8(19)19.8(16)3.9(14)9.1(13)8.1(15)
C1839(2)47(2)16.0(16)10.3(16)8.7(16)22.6(19)
C1929(2)45(2)30.0(19)15.7(17)14.1(16)18.9(18)
C2058(3)112(4)31(2)38(3)25(2)63(3)

 

Table 4 Bond Lengths for mfr200004.
AtomAtomLength/Å AtomAtomLength/Å
Cu1O12.422(2) F5C181.314(5)
Cu1N12.008(3) F6C181.332(5)
Cu1N21.955(3) F7C191.343(4)
Cu1N31.952(3) F8C191.322(5)
Cu1N41.990(3) F9C191.318(4)
S1C21.834(5) F10C201.344(6)
S1C31.723(3) F11C201.307(5)
S2C141.727(3) F12C201.310(7)
S2C151.822(3) N1C11.472(4)
S3O11.446(2) N1C31.297(5)
S3O21.439(3) N2C41.336(4)
S3N51.573(3) N2C81.333(4)
S3C171.831(4) N3C91.337(4)
S4O31.432(3) N3C131.342(4)
S4O41.430(3) N4C141.288(4)
S4N51.584(3) N4C161.475(4)
S4C181.831(4) C1C21.536(5)
S5O51.436(3) C3C41.493(5)
S5O61.437(3) C4C51.387(5)
S5N61.581(3) C5C61.384(5)
S5C191.831(4) C6C71.383(5)
S6O71.430(3) C7C81.385(5)
S6O81.421(4) C8C91.500(4)
S6N61.568(3) C9C101.384(5)
S6C201.849(5) C10C111.396(5)
F1C171.328(4) C11C121.383(5)
F2C171.327(4) C12C131.378(4)
F3C171.334(4) C13C141.488(4)
F4C181.331(4) C15C161.541(4)

 

Table 5 Bond Angles for mfr200004.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
N1Cu1O188.98(10) C1C2S1106.2(3)
N2Cu1O187.07(10) N1C3S1118.4(3)
N2Cu1N180.90(12) N1C3C4118.3(3)
N2Cu1N4158.91(11) C4C3S1123.3(3)
N3Cu1O191.10(10) N2C4C3110.2(3)
N3Cu1N1158.87(12) N2C4C5120.3(3)
N3Cu1N278.00(11) C5C4C3129.5(3)
N3Cu1N480.95(11) C6C5C4117.8(3)
N4Cu1O194.78(10) C7C6C5121.2(3)
N4Cu1N1120.10(12) C6C7C8118.0(3)
C3S1C289.43(17) N2C8C7120.2(3)
C14S2C1589.68(15) N2C8C9111.4(3)
O1S3N5108.61(16) C7C8C9128.4(3)
O1S3C17103.22(15) N3C9C8110.6(3)
O2S3O1117.23(15) N3C9C10120.2(3)
O2S3N5117.01(15) C10C9C8129.1(3)
O2S3C17104.83(17) C9C10C11117.4(3)
N5S3C17104.01(16) C12C11C10121.6(3)
O3S4N5115.10(17) C13C12C11117.8(3)
O3S4C18105.21(18) N3C13C12120.4(3)
O4S4O3118.74(15) N3C13C14110.0(3)
O4S4N5108.68(16) C12C13C14129.6(3)
O4S4C18104.18(18) N4C14S2118.6(3)
N5S4C18103.03(16) N4C14C13118.2(3)
O5S5O6119.88(18) C13C14S2123.2(2)
O5S5N6108.52(17) C16C15S2105.1(2)
O5S5C19103.76(19) N4C16C15108.4(3)
O6S5N6115.78(17) F1C17S3109.9(2)
O6S5C19103.96(19) F1C17F3108.5(3)
N6S5C19102.55(18) F2C17S3111.4(2)
O7S6N6109.24(17) F2C17F1108.6(3)
O7S6C20102.53(19) F2C17F3108.0(3)
O8S6O7118.3(2) F3C17S3110.3(2)
O8S6N6115.56(18) F4C18S4109.4(3)
O8S6C20106.6(3) F4C18F6107.7(3)
N6S6C20102.4(2) F5C18S4111.4(3)
S3O1Cu1137.13(15) F5C18F4108.5(4)
C1N1Cu1134.0(2) F5C18F6109.1(3)
C3N1Cu1112.8(2) F6C18S4110.7(3)
C3N1C1113.2(3) F7C19S5108.8(3)
C4N2Cu1117.6(2) F8C19S5111.5(3)
C8N2Cu1119.7(2) F8C19F7108.2(4)
C8N2C4122.4(3) F9C19S5111.6(3)
C9N3Cu1120.1(2) F9C19F7108.7(3)
C9N3C13122.6(3) F9C19F8108.0(4)
C13N3Cu1117.3(2) F10C20S6107.7(4)
C14N4Cu1113.5(2) F11C20S6109.8(3)
C14N4C16112.0(3) F11C20F10108.0(4)
C16N4Cu1134.0(2) F11C20F12111.9(6)
S3N5S4124.37(19) F12C20S6110.4(3)
S6N6S5126.5(2) F12C20F10109.0(4)
N1C1C2107.9(3)     

 

Table 6 Torsion Angles for mfr200004.
ABCDAngle/˚ ABCDAngle/˚
Cu1N1C1C2164.9(3) N3C9C10C11-0.1(5)
Cu1N1C3S1-178.30(17) N3C13C14S2-178.1(2)
Cu1N1C3C42.8(4) N3C13C14N41.5(4)
Cu1N2C4C3-3.4(4) N5S3O1Cu117.0(3)
Cu1N2C4C5175.1(3) N5S3C17F1-177.6(2)
Cu1N2C8C7-176.5(3) N5S3C17F2-57.2(3)
Cu1N2C8C92.3(4) N5S3C17F362.8(3)
Cu1N3C9C84.2(4) N5S4C18F4-179.8(3)
Cu1N3C9C10-177.4(3) N5S4C18F5-59.9(3)
Cu1N3C13C12177.2(2) N5S4C18F661.6(3)
Cu1N3C13C14-1.4(3) N6S5C19F7173.3(3)
Cu1N4C14S2178.71(15) N6S5C19F8-67.5(3)
Cu1N4C14C13-0.9(4) N6S5C19F953.4(3)
Cu1N4C16C15167.8(2) N6S6C20F10177.5(3)
S1C3C4N2-178.6(2) N6S6C20F11-65.2(5)
S1C3C4C53.1(5) N6S6C20F1258.6(4)
S2C15C16N425.7(3) C1N1C3S13.9(4)
O1S3N5S4153.1(2) C1N1C3C4-175.0(3)
O1S3C17F1-64.3(3) C2S1C3N19.1(3)
O1S3C17F256.2(3) C2S1C3C4-172.0(3)
O1S3C17F3176.1(2) C3S1C2C1-17.9(3)
O2S3O1Cu1152.4(2) C3N1C1C2-17.9(4)
O2S3N5S417.5(3) C3C4C5C6179.7(3)
O2S3C17F159.0(3) C4N2C8C7-2.1(5)
O2S3C17F2179.4(2) C4N2C8C9176.8(3)
O2S3C17F3-60.6(3) C4C5C6C7-2.0(6)
O3S4N5S325.9(3) C5C6C7C80.5(6)
O3S4C18F459.2(3) C6C7C8N21.5(5)
O3S4C18F5179.2(3) C6C7C8C9-177.2(3)
O3S4C18F6-59.3(3) C7C8C9N3174.7(3)
O4S4N5S3161.9(2) C7C8C9C10-3.4(6)
O4S4C18F4-66.4(3) C8N2C4C3-178.0(3)
O4S4C18F553.5(3) C8N2C4C50.5(5)
O4S4C18F6175.1(3) C8C9C10C11177.9(3)
O5S5N6S6-160.7(2) C9N3C13C12-1.0(5)
O5S5C19F760.4(3) C9N3C13C14-179.5(3)
O5S5C19F8179.6(3) C9C10C11C12-0.2(6)
O5S5C19F9-59.5(3) C10C11C12C13-0.1(5)
O6S5N6S6-22.6(3) C11C12C13N30.6(5)
O6S5C19F7-65.7(3) C11C12C13C14178.8(3)
O6S5C19F853.5(3) C12C13C14S23.5(5)
O6S5C19F9174.4(3) C12C13C14N4-176.9(3)
O7S6N6S5-157.2(2) C13N3C9C8-177.7(3)
O7S6C20F1064.2(4) C13N3C9C100.7(5)
O7S6C20F11-178.4(5) C14S2C15C16-19.5(3)
O7S6C20F12-54.6(4) C14N4C16C15-20.7(4)
O8S6N6S5-20.8(4) C15S2C14N49.4(3)
O8S6C20F10-60.8(4) C15S2C14C13-171.0(3)
O8S6C20F1156.6(5) C16N4C14S25.4(4)
O8S6C20F12-179.6(3) C16N4C14C13-174.3(3)
N1C1C2S122.8(4) C17S3O1Cu1-93.0(2)
N1C3C4N20.3(4) C17S3N5S4-97.5(2)
N1C3C4C5-178.0(3) C18S4N5S3-88.0(3)
N2C4C5C61.5(5) C19S5N6S689.9(3)
N2C8C9N3-4.0(4) C20S6N6S594.6(3)
N2C8C9C10177.8(3)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mfr200004.
AtomxyzU(eq)
H1A1850.793614.765706.5433
H1B5.192826.995268.5933
H2A2700.972793.94401.845
H2B708.272380.333884.7145
H52643.76-541.44766.1633
H63212.82-1352.515743.6535
H73383.68-519.67362.0329
H103425.63657.059081.3127
H113562.682003.6710549.529
H123179.033582.7510651.2624
H15A489.445587.019069.8527
H15B2289.556386.369350.1427
H16A1122.174829.197665.3224
H16B3120.475289.118143.9824

Refinement model description

Number of restraints - 443, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
All non-hydrogen atoms
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C2(H2A,H2B), C15(H15A,H15B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12)

This report has been created with Olex2, compiled on 2020.12.01 svn.r5f60950 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.