Table 1 : Crystal data and structure refinement for mfr200002.
Identification code | mfr200002 |
Empirical formula | C22H18CuF12N6O8S4 |
Formula weight | 914.20 |
Temperature/K | 100.0(2) |
Crystal system | monoclinic |
Space group | Pn |
a/Å | 8.77390(11) |
b/Å | 10.90700(13) |
c/Å | 17.79310(19) |
α/° | 90 |
β/° | 102.1740(10) |
γ/° | 90 |
Volume/Å3 | 1664.45(3) |
Z | 2 |
ρcalcg/cm3 | 1.824 |
μ/mm‑1 | 0.949 |
F(000) | 914.0 |
Crystal size/mm3 | 0.51 × 0.105 × 0.102 |
Radiation | Synchrotron (λ = 0.6889) |
2Θ range for data collection/° | 3.62 to 53.144 |
Index ranges | -11 ≤ h ≤ 11, -14 ≤ k ≤ 14, -23 ≤ l ≤ 23 |
Reflections collected | 22609 |
Independent reflections | 7453 [Rint = 0.0486, Rsigma = 0.0554] |
Data/restraints/parameters | 7453/614/523 |
Goodness-of-fit on F2 | 1.039 |
Final R indexes [I>=2σ (I)] | R1 = 0.0276, wR2 = 0.0703 |
Final R indexes [all data] | R1 = 0.0281, wR2 = 0.0706 |
Largest diff. peak/hole / e Å-3 | 0.52/-0.28 |
Flack parameter | 0.015(5) |
Experimental
Crystal structure data for mfr200002 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 ?.
Intensities were corrected for absorption using ?.
Using Olex2 (Dolomanov, 2009), the structure was solved using ShelXT (Sheldrick, 2015) and refined by ShelXL (Sheldrick, 2015).
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 [mfr200002]
Crystal Data for C22H18CuF12N6O8S4 (M =914.20 g/mol): monoclinic, space group Pn (no. 7), a = 8.77390(11) Å, b = 10.90700(13) Å, c = 17.79310(19) Å, β = 102.1740(10)°, V = 1664.45(3) Å3, Z = 2, T = 100.0(2) K, μ(Synchrotron) = 0.949 mm-1, Dcalc = 1.824 g/cm3, 22609 reflections measured (3.62° ≤ 2Θ ≤ 53.144°), 7453 unique (Rint = 0.0486, Rsigma = 0.0554) which were used in all calculations. The final R1 was 0.0276 (I > 2σ(I)) and wR2 was 0.0706 (all data).
Special details of refinement:
Parts of this structure have been modelled as disordered over two sites. In all cases the occupancies of the disordered sites were refined independently of the atomic displacement parameters and fixed prior to anisotropic refinement of the non-hydrogen atoms. The geometry of the disordered moieties were restrained using the SADI card and the displacement parameters of all partially-occupied non-hydrogen atoms were restrained using the SIMU card.Comments:
N/A
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Cu1 | 225.6(4) | -4927.3(3) | -5515.0(2) | 17.67(9) |
S1 | -3995.1(8) | -3688.9(6) | -6020.7(4) | 17.65(14) |
S2 | -5468.2(8) | -5466.4(7) | -5287.6(4) | 18.80(15) |
S3 | 414.9(9) | -10638.1(7) | -3331.1(4) | 20.50(15) |
S4 | 2844.2(10) | -8934.0(8) | -3191.3(5) | 32.2(2) |
F1 | -2083(3) | -2015.3(19) | -5388.5(13) | 35.6(5) |
F2 | -4454(3) | -1658.9(19) | -5304.0(13) | 38.7(5) |
F3 | -3117(3) | -3024(2) | -4575.4(11) | 37.2(5) |
F4 | -5577(3) | -7801(2) | -5629.9(15) | 47.7(6) |
F5 | -6863(3) | -6646(2) | -6526.0(13) | 42.8(6) |
F6 | -4371(2) | -6728.2(18) | -6318.1(11) | 27.8(4) |
F7 | -1485(4) | -11352(3) | -2488(2) | 77.5(11) |
F8 | 195(5) | -10013(3) | -1942.6(17) | 72.8(11) |
F9 | -1751(4) | -9455(3) | -2828.9(18) | 61.3(8) |
O1 | -2662(3) | -4479(2) | -5948.2(14) | 24.0(5) |
O2 | -4465(3) | -2980(2) | -6705.0(12) | 27.0(5) |
O3 | -4070(3) | -5686(2) | -4722.0(13) | 25.9(5) |
O4 | -6942(3) | -5522(2) | -5051.9(14) | 25.7(5) |
O5 | -732(3) | -10922(2) | -3995.6(16) | 41.0(7) |
O6 | 1506(3) | -11567(2) | -3001.5(15) | 32.4(6) |
O7 | 2942(4) | -7634(3) | -3123(3) | 68.4(11) |
O8 | 3825(3) | -9661(3) | -2617.9(16) | 39.4(7) |
N1 | 889(3) | -3339(2) | -5900.9(16) | 21.6(5) |
N2 | 109(3) | -5362(2) | -6591.9(15) | 18.8(5) |
N3 | -507(3) | -6619(2) | -5531.6(14) | 16.2(5) |
N4 | 18(3) | -5086(2) | -4429.1(16) | 18.9(5) |
N5 | -5497(3) | -4285(2) | -5809.2(14) | 19.5(5) |
N6 | 1078(4) | -9319(3) | -3419.9(19) | 32.1(7) |
C1 | 1564(4) | -2181(3) | -5537(2) | 27.2(7) |
C2 | 1732(5) | -1357(3) | -6216(2) | 37.9(9) |
C3 | 1692(4) | -2249(3) | -6885(2) | 30.4(7) |
C4 | 973(3) | -3355(3) | -6609.3(19) | 22.1(6) |
C5 | 459(4) | -4502(3) | -7049.3(18) | 22.0(6) |
C6 | 352(4) | -4742(4) | -7827(2) | 28.5(7) |
C7 | -94(4) | -5920(4) | -8088.8(18) | 31.0(8) |
C8 | -470(4) | -6820(3) | -7602.1(18) | 26.1(6) |
C9 | -366(3) | -6497(3) | -6828.8(17) | 18.9(6) |
C10 | -745(3) | -7248(3) | -6192.9(16) | 17.7(5) |
C11 | -1327(4) | -8443(3) | -6214.1(18) | 22.9(6) |
C12 | -1666(4) | -8916(3) | -5544.4(19) | 26.1(7) |
C13 | -1448(4) | -8226(3) | -4872.0(18) | 23.5(6) |
C14 | -840(3) | -7054(3) | -4887.0(16) | 17.5(5) |
C15 | -496(4) | -6132(3) | -4259.3(16) | 18.4(6) |
C16 | -683(5) | -6268(3) | -3448.5(17) | 28.3(7) |
C18 | 332(4) | -4283(3) | -3738.6(18) | 27.0(7) |
C19 | -3374(4) | -2527(3) | -5267.8(18) | 25.1(6) |
C20 | -5577(4) | -6746(3) | -5983.3(19) | 24.4(6) |
C21 | -721(6) | -10339(4) | -2598(3) | 42.8(10) |
F10A | 4932(10) | -8685(8) | -3996(6) | 54.0(19) |
F11A | 3429(10) | -10270(8) | -4276(4) | 61.3(17) |
F12A | 2545(8) | -8474(7) | -4636(4) | 64.9(19) |
C17B | 228(17) | -5089(9) | -3068(6) | 38(2) |
C22A | 3477(12) | -9106(10) | -4083(5) | 45(2) |
F10B | 5124(18) | -9179(14) | -3983(12) | 79(4) |
F11B | 3738(15) | -10759(11) | -4037(6) | 65(3) |
F12B | 2833(13) | -9218(12) | -4710(5) | 76(3) |
C17A | -555(14) | -4939(8) | -3174(5) | 35(2) |
C22B | 3660(20) | -9520(17) | -4010(9) | 59(4) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Cu1 | 18.61(17) | 18.43(16) | 17.13(16) | -2.14(13) | 6.36(12) | -2.80(14) |
S1 | 15.3(3) | 21.8(3) | 15.6(3) | -1.2(3) | 2.5(2) | 0.4(3) |
S2 | 14.8(3) | 23.9(3) | 17.9(3) | 0.6(3) | 3.9(3) | 1.1(3) |
S3 | 21.6(4) | 18.3(3) | 20.1(3) | -2.4(3) | 0.8(3) | -1.0(3) |
S4 | 26.4(4) | 34.3(4) | 31.6(4) | 9.8(3) | -3.5(3) | -9.9(3) |
F1 | 30.9(12) | 34.2(11) | 43.1(12) | -11.3(9) | 10.8(9) | -14.2(9) |
F2 | 37.3(13) | 29.7(10) | 50.3(14) | -13.4(9) | 11.6(11) | 3.3(9) |
F3 | 47.6(14) | 42.5(11) | 18.5(9) | -4.2(8) | 0.2(9) | -12.0(10) |
F4 | 69.5(18) | 24.8(10) | 56.4(14) | 1.9(10) | 30.4(13) | -7.6(11) |
F5 | 22.7(11) | 52.7(13) | 46.5(13) | -27.6(11) | -7.5(9) | 8.1(10) |
F6 | 23.3(10) | 29.3(9) | 32.6(10) | -7.2(8) | 10.4(8) | 1.3(7) |
F7 | 70(2) | 73(2) | 106(3) | 45.6(19) | 55(2) | 6.3(17) |
F8 | 112(3) | 82(2) | 25.6(13) | -3.9(12) | 18.4(16) | 31.0(19) |
F9 | 59.1(19) | 57.3(16) | 76(2) | 9.7(14) | 34.4(16) | 31.2(14) |
O1 | 15.2(11) | 28.6(12) | 28.7(12) | -0.8(9) | 6.1(9) | 2.3(9) |
O2 | 25.5(12) | 36.0(12) | 18.7(11) | 5.5(9) | 3.2(9) | 0.2(10) |
O3 | 21.3(12) | 34.4(12) | 20.2(11) | 3.8(9) | 0.4(9) | 3.7(9) |
O4 | 19.2(12) | 32.0(12) | 27.7(12) | 1.7(9) | 9.0(9) | 1.5(9) |
O5 | 40.6(16) | 36.2(13) | 36.7(15) | -7.9(12) | -13.5(12) | -4.4(12) |
O6 | 29.5(14) | 22.0(11) | 41.6(14) | -3.6(10) | -1.8(11) | 4.4(10) |
O7 | 43(2) | 38.0(16) | 117(3) | 13.5(19) | 1(2) | -15.2(14) |
O8 | 31.0(15) | 48.2(15) | 32.3(14) | 14.8(12) | -8.9(11) | -13.4(12) |
N1 | 12.7(12) | 20.7(12) | 31.0(14) | 0.3(10) | 4.1(10) | 0.1(10) |
N2 | 13.9(13) | 26.5(12) | 16.5(12) | -0.1(10) | 4.4(10) | 2.6(10) |
N3 | 13.1(12) | 19.1(11) | 16.0(11) | -2.8(9) | 2.4(9) | 0.2(9) |
N4 | 17.2(14) | 22.9(12) | 15.9(12) | -4.2(9) | 1.8(10) | 0.5(9) |
N5 | 12.7(12) | 23.6(12) | 21.1(13) | -1.8(9) | 1.7(10) | 1.5(9) |
N6 | 24.1(16) | 25.1(14) | 42.3(18) | 10.4(12) | -4.2(13) | -6.2(12) |
C1 | 18.3(16) | 20.5(15) | 40.4(19) | -1.8(13) | 0.8(13) | -2.6(12) |
C2 | 26.9(19) | 26.9(17) | 54(2) | 11.0(16) | -4.4(17) | -6.7(14) |
C3 | 17.6(16) | 32.0(17) | 40.2(19) | 18.8(14) | 3.1(13) | 0.7(13) |
C4 | 10.9(14) | 25.1(14) | 29.5(15) | 7.8(12) | 2.6(11) | 3.7(11) |
C5 | 12.0(14) | 31.1(16) | 23.1(15) | 3.1(12) | 3.9(11) | 4.2(12) |
C6 | 19.3(17) | 45.9(18) | 21.1(16) | 11.3(14) | 6.0(13) | 1.2(14) |
C7 | 21.6(17) | 57(2) | 15.4(15) | -2.7(14) | 5.7(13) | -1.0(15) |
C8 | 19.6(16) | 39.7(17) | 18.7(14) | -6.7(12) | 3.5(11) | -1.4(13) |
C9 | 11.4(13) | 26.8(14) | 17.9(13) | -3.0(11) | 1.8(10) | 3.0(11) |
C10 | 12.7(13) | 23.3(14) | 15.7(12) | -3.8(10) | -0.3(10) | 4.4(10) |
C11 | 22.7(16) | 21.8(14) | 21.0(14) | -3.8(11) | -2.2(12) | 3.0(12) |
C12 | 28.5(17) | 18.3(14) | 28.2(17) | 1.3(11) | -1.6(13) | -1.7(12) |
C13 | 23.7(16) | 23.9(14) | 20.8(14) | 6.3(11) | -0.4(12) | 0.4(12) |
C14 | 17.0(14) | 18.3(13) | 16.2(13) | 1.4(10) | 1.0(10) | 3.9(11) |
C15 | 16.9(14) | 24.3(14) | 13.2(13) | -0.5(10) | 1.3(10) | 5.0(11) |
C16 | 43(2) | 29.7(16) | 12.8(14) | 2.7(11) | 6.6(13) | 6.1(14) |
C18 | 28.7(18) | 31.7(16) | 18.5(15) | -9.8(12) | -0.2(13) | 2.2(13) |
C19 | 24.8(16) | 25.4(15) | 25.3(15) | -5.9(12) | 6.1(13) | -3.3(12) |
C20 | 18.6(15) | 24.6(14) | 30.1(16) | -3.9(12) | 5.2(12) | 1.5(12) |
C21 | 53(3) | 41.5(19) | 40(2) | 8.4(17) | 24(2) | 13.0(19) |
F10A | 30(3) | 89(5) | 46(3) | 21(4) | 14(2) | -11(3) |
F11A | 58(4) | 89(5) | 42(4) | -19(3) | 21(3) | -4(4) |
F12A | 41(3) | 113(5) | 37(3) | 40(4) | 1(2) | -9(4) |
C17B | 66(8) | 33(5) | 13(4) | -7(3) | 7(5) | -2(5) |
C22A | 32(4) | 74(5) | 28(4) | 14(4) | 7(3) | -10(4) |
F10B | 48(6) | 123(11) | 70(6) | 29(8) | 20(5) | -23(7) |
F11B | 60(6) | 101(7) | 43(5) | -3(4) | 26(4) | -7(5) |
F12B | 67(6) | 127(8) | 30(4) | 34(5) | 0(4) | -37(6) |
C17A | 52(6) | 35(4) | 18(4) | -3(3) | 8(4) | 9(4) |
C22B | 50(7) | 98(8) | 27(6) | 17(7) | 2(5) | -31(7) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Cu1 | N1 | 1.995(3) | N2 | C5 | 1.320(4) | |
Cu1 | N2 | 1.956(3) | N2 | C9 | 1.345(4) | |
Cu1 | N3 | 1.952(2) | N3 | C10 | 1.340(3) | |
Cu1 | N4 | 1.986(3) | N3 | C14 | 1.329(4) | |
S1 | O1 | 1.436(2) | N4 | C15 | 1.286(4) | |
S1 | O2 | 1.428(2) | N4 | C18 | 1.487(4) | |
S1 | N5 | 1.585(3) | C1 | C2 | 1.538(5) | |
S1 | C19 | 1.841(3) | C2 | C3 | 1.532(6) | |
S2 | O3 | 1.433(2) | C3 | C4 | 1.490(4) | |
S2 | O4 | 1.442(2) | C4 | C5 | 1.495(5) | |
S2 | N5 | 1.585(3) | C5 | C6 | 1.392(5) | |
S2 | C20 | 1.855(3) | C6 | C7 | 1.395(6) | |
S3 | O5 | 1.416(3) | C7 | C8 | 1.394(5) | |
S3 | O6 | 1.432(2) | C8 | C9 | 1.404(4) | |
S3 | N6 | 1.572(3) | C9 | C10 | 1.490(4) | |
S3 | C21 | 1.831(4) | C10 | C11 | 1.398(4) | |
S4 | O7 | 1.424(3) | C11 | C12 | 1.387(5) | |
S4 | O8 | 1.428(3) | C12 | C13 | 1.392(5) | |
S4 | N6 | 1.574(3) | C13 | C14 | 1.388(4) | |
S4 | C22A | 1.799(10) | C14 | C15 | 1.486(4) | |
S4 | C22B | 1.867(16) | C15 | C16 | 1.494(4) | |
F1 | C19 | 1.320(4) | C16 | C17B | 1.588(11) | |
F2 | C19 | 1.332(4) | C16 | C17A | 1.526(9) | |
F3 | C19 | 1.321(4) | C18 | C17B | 1.500(12) | |
F4 | C20 | 1.311(4) | C18 | C17A | 1.568(11) | |
F5 | C20 | 1.326(4) | F10A | C22A | 1.335(10) | |
F6 | C20 | 1.319(4) | F11A | C22A | 1.313(12) | |
F7 | C21 | 1.328(5) | F12A | C22A | 1.331(10) | |
F8 | C21 | 1.317(6) | F10B | C22B | 1.327(16) | |
F9 | C21 | 1.325(5) | F11B | C22B | 1.354(19) | |
N1 | C1 | 1.484(4) | F12B | C22B | 1.344(16) | |
N1 | C4 | 1.278(4) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
N2 | Cu1 | N1 | 80.33(11) | C6 | C5 | C4 | 128.9(3) | |
N2 | Cu1 | N4 | 159.31(11) | C5 | C6 | C7 | 117.4(3) | |
N3 | Cu1 | N1 | 159.17(10) | C8 | C7 | C6 | 121.9(3) | |
N3 | Cu1 | N2 | 78.87(11) | C7 | C8 | C9 | 117.2(3) | |
N3 | Cu1 | N4 | 80.50(10) | N2 | C9 | C8 | 119.3(3) | |
N4 | Cu1 | N1 | 120.25(11) | N2 | C9 | C10 | 111.8(2) | |
O1 | S1 | N5 | 115.77(14) | C8 | C9 | C10 | 128.9(3) | |
O1 | S1 | C19 | 103.71(15) | N3 | C10 | C9 | 111.5(3) | |
O2 | S1 | O1 | 119.00(14) | N3 | C10 | C11 | 119.3(3) | |
O2 | S1 | N5 | 108.64(14) | C11 | C10 | C9 | 129.1(3) | |
O2 | S1 | C19 | 103.63(14) | C12 | C11 | C10 | 117.9(3) | |
N5 | S1 | C19 | 104.05(14) | C11 | C12 | C13 | 121.4(3) | |
O3 | S2 | O4 | 118.42(14) | C14 | C13 | C12 | 117.8(3) | |
O3 | S2 | N5 | 116.91(14) | N3 | C14 | C13 | 120.0(3) | |
O3 | S2 | C20 | 105.00(15) | N3 | C14 | C15 | 111.1(3) | |
O4 | S2 | N5 | 107.44(14) | C13 | C14 | C15 | 128.8(3) | |
O4 | S2 | C20 | 103.86(15) | N4 | C15 | C14 | 116.7(3) | |
N5 | S2 | C20 | 103.23(14) | N4 | C15 | C16 | 115.5(3) | |
O5 | S3 | O6 | 118.92(16) | C14 | C15 | C16 | 127.8(3) | |
O5 | S3 | N6 | 109.20(16) | C15 | C16 | C17B | 100.5(5) | |
O5 | S3 | C21 | 103.7(2) | C15 | C16 | C17A | 101.5(4) | |
O6 | S3 | N6 | 117.34(16) | N4 | C18 | C17B | 106.2(4) | |
O6 | S3 | C21 | 104.57(18) | N4 | C18 | C17A | 103.3(4) | |
N6 | S3 | C21 | 100.2(2) | F1 | C19 | S1 | 107.8(2) | |
O7 | S4 | O8 | 118.3(2) | F1 | C19 | F2 | 108.5(3) | |
O7 | S4 | N6 | 109.02(19) | F1 | C19 | F3 | 110.0(3) | |
O7 | S4 | C22A | 99.0(4) | F2 | C19 | S1 | 110.9(2) | |
O7 | S4 | C22B | 112.4(6) | F3 | C19 | S1 | 111.3(2) | |
O8 | S4 | N6 | 116.66(16) | F3 | C19 | F2 | 108.4(3) | |
O8 | S4 | C22A | 108.7(4) | F4 | C20 | S2 | 110.2(2) | |
O8 | S4 | C22B | 95.4(6) | F4 | C20 | F5 | 109.6(3) | |
N6 | S4 | C22A | 102.4(4) | F4 | C20 | F6 | 108.1(3) | |
N6 | S4 | C22B | 103.1(6) | F5 | C20 | S2 | 109.9(2) | |
C1 | N1 | Cu1 | 135.0(2) | F6 | C20 | S2 | 110.9(2) | |
C4 | N1 | Cu1 | 114.2(2) | F6 | C20 | F5 | 108.1(3) | |
C4 | N1 | C1 | 109.9(3) | F7 | C21 | S3 | 108.8(3) | |
C5 | N2 | Cu1 | 117.5(2) | F8 | C21 | S3 | 110.9(4) | |
C5 | N2 | C9 | 123.9(3) | F8 | C21 | F7 | 109.1(4) | |
C9 | N2 | Cu1 | 118.6(2) | F8 | C21 | F9 | 109.1(4) | |
C10 | N3 | Cu1 | 119.1(2) | F9 | C21 | S3 | 110.3(3) | |
C14 | N3 | Cu1 | 117.12(19) | F9 | C21 | F7 | 108.6(4) | |
C14 | N3 | C10 | 123.6(3) | C18 | C17B | C16 | 104.2(6) | |
C15 | N4 | Cu1 | 114.5(2) | F10A | C22A | S4 | 109.1(8) | |
C15 | N4 | C18 | 110.0(3) | F11A | C22A | S4 | 109.4(7) | |
C18 | N4 | Cu1 | 135.5(2) | F11A | C22A | F10A | 109.9(9) | |
S1 | N5 | S2 | 124.14(16) | F11A | C22A | F12A | 109.1(8) | |
S3 | N6 | S4 | 125.7(2) | F12A | C22A | S4 | 110.0(7) | |
N1 | C1 | C2 | 104.5(3) | F12A | C22A | F10A | 109.3(8) | |
C3 | C2 | C1 | 104.4(3) | C16 | C17A | C18 | 104.0(6) | |
C4 | C3 | C2 | 101.6(3) | F10B | C22B | S4 | 113.8(13) | |
N1 | C4 | C3 | 115.5(3) | F10B | C22B | F11B | 103.1(14) | |
N1 | C4 | C5 | 117.0(3) | F10B | C22B | F12B | 107.2(14) | |
C3 | C4 | C5 | 127.4(3) | F11B | C22B | S4 | 113.5(10) | |
N2 | C5 | C4 | 110.8(3) | F12B | C22B | S4 | 114.7(13) | |
N2 | C5 | C6 | 120.3(3) | F12B | C22B | F11B | 103.4(13) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
Cu1 | N1 | C1 | C2 | -178.9(2) | N4 | C15 | C16 | C17B | -12.3(6) | |
Cu1 | N1 | C4 | C3 | -171.2(2) | N4 | C15 | C16 | C17A | 13.8(6) | |
Cu1 | N1 | C4 | C5 | 4.4(3) | N4 | C18 | C17B | C16 | -17.7(9) | |
Cu1 | N2 | C5 | C4 | 3.2(3) | N4 | C18 | C17A | C16 | 23.2(7) | |
Cu1 | N2 | C5 | C6 | -178.0(2) | N5 | S1 | C19 | F1 | 177.7(2) | |
Cu1 | N2 | C9 | C8 | 179.4(2) | N5 | S1 | C19 | F2 | -63.7(3) | |
Cu1 | N2 | C9 | C10 | 0.4(3) | N5 | S1 | C19 | F3 | 57.1(3) | |
Cu1 | N3 | C10 | C9 | 0.7(3) | N5 | S2 | C20 | F4 | -179.4(2) | |
Cu1 | N3 | C10 | C11 | -177.5(2) | N5 | S2 | C20 | F5 | -58.6(3) | |
Cu1 | N3 | C14 | C13 | 176.4(2) | N5 | S2 | C20 | F6 | 60.9(2) | |
Cu1 | N3 | C14 | C15 | -2.7(3) | N6 | S3 | C21 | F7 | 175.1(3) | |
Cu1 | N4 | C15 | C14 | 0.5(4) | N6 | S3 | C21 | F8 | -64.9(3) | |
Cu1 | N4 | C15 | C16 | -179.2(2) | N6 | S3 | C21 | F9 | 56.1(4) | |
Cu1 | N4 | C18 | C17B | -168.1(6) | N6 | S4 | C22A | F10A | 173.6(6) | |
Cu1 | N4 | C18 | C17A | 165.1(4) | N6 | S4 | C22A | F11A | -66.2(7) | |
O1 | S1 | N5 | S2 | 20.9(2) | N6 | S4 | C22A | F12A | 53.7(8) | |
O1 | S1 | C19 | F1 | 56.2(3) | N6 | S4 | C22B | F10B | 173.0(12) | |
O1 | S1 | C19 | F2 | 174.8(2) | N6 | S4 | C22B | F11B | -69.5(12) | |
O1 | S1 | C19 | F3 | -64.4(3) | N6 | S4 | C22B | F12B | 49.1(13) | |
O2 | S1 | N5 | S2 | 157.83(18) | C1 | N1 | C4 | C3 | -0.3(4) | |
O2 | S1 | C19 | F1 | -68.7(3) | C1 | N1 | C4 | C5 | 175.3(3) | |
O2 | S1 | C19 | F2 | 49.9(3) | C1 | C2 | C3 | C4 | 18.8(3) | |
O2 | S1 | C19 | F3 | 170.7(2) | C2 | C3 | C4 | N1 | -12.3(4) | |
O3 | S2 | N5 | S1 | 28.2(2) | C2 | C3 | C4 | C5 | 172.6(3) | |
O3 | S2 | C20 | F4 | 57.6(3) | C3 | C4 | C5 | N2 | 169.9(3) | |
O3 | S2 | C20 | F5 | 178.5(2) | C3 | C4 | C5 | C6 | -8.7(5) | |
O3 | S2 | C20 | F6 | -62.1(3) | C4 | N1 | C1 | C2 | 12.9(4) | |
O4 | S2 | N5 | S1 | 164.18(18) | C4 | C5 | C6 | C7 | 176.9(3) | |
O4 | S2 | C20 | F4 | -67.4(3) | C5 | N2 | C9 | C8 | 1.6(5) | |
O4 | S2 | C20 | F5 | 53.5(3) | C5 | N2 | C9 | C10 | -177.4(3) | |
O4 | S2 | C20 | F6 | 172.9(2) | C5 | C6 | C7 | C8 | 2.0(5) | |
O5 | S3 | N6 | S4 | -138.0(3) | C6 | C7 | C8 | C9 | -0.7(5) | |
O5 | S3 | C21 | F7 | 62.3(3) | C7 | C8 | C9 | N2 | -1.1(5) | |
O5 | S3 | C21 | F8 | -177.7(3) | C7 | C8 | C9 | C10 | 177.7(3) | |
O5 | S3 | C21 | F9 | -56.7(4) | C8 | C9 | C10 | N3 | -179.5(3) | |
O6 | S3 | N6 | S4 | 1.2(4) | C8 | C9 | C10 | C11 | -1.5(5) | |
O6 | S3 | C21 | F7 | -63.0(4) | C9 | N2 | C5 | C4 | -178.9(3) | |
O6 | S3 | C21 | F8 | 57.1(3) | C9 | N2 | C5 | C6 | -0.2(5) | |
O6 | S3 | C21 | F9 | 178.0(3) | C9 | C10 | C11 | C12 | -176.5(3) | |
O7 | S4 | N6 | S3 | -161.7(3) | C10 | N3 | C14 | C13 | 1.0(5) | |
O7 | S4 | C22A | F10A | 61.7(7) | C10 | N3 | C14 | C15 | -178.1(3) | |
O7 | S4 | C22A | F11A | -178.1(6) | C10 | C11 | C12 | C13 | 0.5(5) | |
O7 | S4 | C22A | F12A | -58.2(8) | C11 | C12 | C13 | C14 | -1.6(5) | |
O7 | S4 | C22B | F10B | 55.7(14) | C12 | C13 | C14 | N3 | 0.9(5) | |
O7 | S4 | C22B | F11B | 173.2(9) | C12 | C13 | C14 | C15 | 179.9(3) | |
O7 | S4 | C22B | F12B | -68.2(13) | C13 | C14 | C15 | N4 | -177.6(3) | |
O8 | S4 | N6 | S3 | -24.4(4) | C13 | C14 | C15 | C16 | 2.0(5) | |
O8 | S4 | C22A | F10A | -62.4(7) | C14 | N3 | C10 | C9 | 176.0(3) | |
O8 | S4 | C22A | F11A | 57.8(7) | C14 | N3 | C10 | C11 | -2.2(4) | |
O8 | S4 | C22A | F12A | 177.7(6) | C14 | C15 | C16 | C17B | 168.1(6) | |
O8 | S4 | C22B | F10B | -68.0(13) | C14 | C15 | C16 | C17A | -165.8(5) | |
O8 | S4 | C22B | F11B | 49.5(11) | C15 | N4 | C18 | C17B | 11.0(7) | |
O8 | S4 | C22B | F12B | 168.1(12) | C15 | N4 | C18 | C17A | -15.7(5) | |
N1 | C1 | C2 | C3 | -19.6(3) | C15 | C16 | C17B | C18 | 17.6(8) | |
N1 | C4 | C5 | N2 | -5.1(4) | C15 | C16 | C17A | C18 | -21.7(7) | |
N1 | C4 | C5 | C6 | 176.3(3) | C18 | N4 | C15 | C14 | -178.9(3) | |
N2 | C5 | C6 | C7 | -1.6(5) | C18 | N4 | C15 | C16 | 1.5(4) | |
N2 | C9 | C10 | N3 | -0.7(4) | C19 | S1 | N5 | S2 | -92.2(2) | |
N2 | C9 | C10 | C11 | 177.3(3) | C20 | S2 | N5 | S1 | -86.4(2) | |
N3 | C10 | C11 | C12 | 1.4(5) | C21 | S3 | N6 | S4 | 113.5(3) | |
N3 | C14 | C15 | N4 | 1.4(4) | C22A | S4 | N6 | S3 | 94.2(4) | |
N3 | C14 | C15 | C16 | -179.0(3) | C22B | S4 | N6 | S3 | 78.7(6) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H1A | 2590.77 | -2331.24 | -5193.74 | 33 |
H1B | 861.13 | -1801.56 | -5235.12 | 33 |
H2A | 861.69 | -762.75 | -6337.17 | 45 |
H2B | 2729.77 | -901.05 | -6099.52 | 45 |
H3A | 1042.64 | -1928.99 | -7368.19 | 36 |
H3B | 2753.27 | -2425.4 | -6963.93 | 36 |
H6 | 575.25 | -4126.93 | -8166.56 | 34 |
H7 | -142.94 | -6115.33 | -8613.73 | 37 |
H8 | -784.04 | -7617.86 | -7785.68 | 31 |
H11 | -1485.65 | -8915.95 | -6672.41 | 27 |
H12 | -2055.43 | -9729.15 | -5544.57 | 31 |
H13 | -1705.98 | -8546.59 | -4418.3 | 28 |
H16A | -198.38 | -7033.93 | -3212.14 | 34 |
H16B | -1794.34 | -6247.82 | -3413.36 | 34 |
H16C | 153.36 | -6782.22 | -3143.32 | 34 |
H16D | -1710.12 | -6624.72 | -3425.23 | 34 |
H18A | -448.87 | -3615.84 | -3791.68 | 32 |
H18B | 1383.01 | -3912.59 | -3668.48 | 32 |
H18C | -79.95 | -3445.83 | -3865.12 | 32 |
H18D | 1463.67 | -4231.61 | -3515.51 | 32 |
H17A | -350.32 | -4676.06 | -2719.22 | 45 |
H17B | 1280.42 | -5311.16 | -2774.67 | 45 |
H17C | 40.42 | -4881.92 | -2636.58 | 42 |
H17D | -1600.3 | -4574.86 | -3206.59 | 42 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
H16A | 0.4706 | H16B | 0.4706 | H16C | 0.5294 | ||
H16D | 0.5294 | H18A | 0.4706 | H18B | 0.4706 | ||
H18C | 0.5294 | H18D | 0.5294 | F10A | 0.5914 | ||
F11A | 0.5914 | F12A | 0.5914 | C17B | 0.4706 | ||
H17A | 0.4706 | H17B | 0.4706 | C22A | 0.5914 | ||
F10B | 0.4086 | F11B | 0.4086 | F12B | 0.4086 | ||
C17A | 0.5294 | H17C | 0.5294 | H17D | 0.5294 | ||
C22B | 0.4086 |
Refinement model description
Number of restraints - 614, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
C17B-C16 ≈ C17A-C16
with sigma of 0.02
F10A-F11A ≈ F10B-F11B
with sigma of 0.04
S4-C22A ≈ S4-C22B
with sigma of 0.02
F10A-C22A ≈ F10B-C22B
with sigma of 0.02
S4-F12A ≈ S4-F12B
with sigma of 0.04
F11A-F12A ≈ F11B-F12B
with sigma of 0.04
F10A-F12A ≈ F10B-F12B
with sigma of 0.04
F12A-C22A ≈ F12B-C22B
with sigma of 0.02
F11A-C22A ≈ F11B-C22B
with sigma of 0.02
S4-F10A ≈ S4-F10B
with sigma of 0.04
S4-F11A ≈ S4-F11B
with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C17B ≈ C17A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
F10A ≈ F11A ≈ F12A ≈ C22A ≈ F10B ≈ F11B ≈ F12B ≈
C22B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.02
4. 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
5. Others
Fixed Sof: H16A(0.47062) H16B(0.47062) H16C(0.52938) H16D(0.52938)
H18A(0.47062) H18B(0.47062) H18C(0.52938) H18D(0.52938) F10A(0.59139)
F11A(0.59139) F12A(0.59139) C17B(0.47062) H17A(0.47062) H17B(0.47062)
C22A(0.59139) F10B(0.40861) F11B(0.40861) F12B(0.40861) C17A(0.52938)
H17C(0.52938) H17D(0.52938) C22B(0.40861)
6.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C16(H16A,H16B), C16(H16C,H16D),
C18(H18A,H18B), C18(H18C,H18D), C17B(H17A,H17B), C17A(H17C,H17D)
6.b Aromatic/amide H refined with riding coordinates:
C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13)
This report has been created with Olex2, compiled on 2018.05.29 svn.r3508 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.