Cm_mnt_beta

Table 1 Crystal data and structure refinement for Cm_mnt_beta.
Identification code Cm_mnt_beta
Empirical formula C28CmN14Na5S8
Formula weight 1147.85
Temperature/K 100.00
Crystal system monoclinic
Space group P21/n
a/Å 13.7182(5)
b/Å 18.3443(7)
c/Å 17.4906(6)
α/° 90
β/° 92.4140(10)
γ/° 90
Volume/Å3 4397.6(3)
Z 4
ρcalcg/cm3 1.734
μ/mm‑1 2.322
F(000) 2180.0
Crystal size/mm3 0.172 × 0.161 × 0.072
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 3.698 to 66.466
Index ranges -21 ≤ h ≤ 21, -28 ≤ k ≤ 28, -26 ≤ l ≤ 26
Reflections collected 95942
Independent reflections 16847 [Rint = 0.0572, Rsigma = 0.0416]
Data/restraints/parameters 16847/0/505
Goodness-of-fit on F2 1.069
Final R indexes [I>=2σ (I)] R1 = 0.0390, wR2 = 0.0817
Final R indexes [all data] R1 = 0.0552, wR2 = 0.0878
Largest diff. peak/hole / e Å-3 1.80/-1.40

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for Cm_mnt_beta. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Cm11486.8(2)1934.2(2)7455.6(2)15.80(3)
S33093.8(6)2185.0(5)6524.8(5)19.85(16)
S14235.1(6)5735.2(5)6645.9(5)19.50(16)
S810190.0(7)1419.8(5)6221.6(5)20.81(16)
S42161.5(7)544.9(5)6963.9(6)25.20(19)
S512715.0(7)8325.2(5)7102.6(6)23.50(18)
S710709.0(7)3147.5(5)6558.2(5)21.62(16)
S25127.6(7)7454.7(5)6713.2(6)26.61(19)
S612093.7(9)6740.3(7)6326.7(7)37.5(3)
Na36263.7(10)1881.5(8)4484.0(8)17.5(3)
Na27047.3(11)4099.5(8)4818.2(9)24.2(3)
Na18345.2(11)7629.2(9)4733.4(9)25.2(3)
Na58415.0(13)5325.7(11)3012.5(10)34.4(4)
Na49440.5(16)10257.5(10)7131.5(11)41.3(5)
N16180(3)5051.9(19)5444(2)29.3(7)
C63086(3)689.9(19)6338(2)20.2(6)
C83448(3)50(2)5978(2)23.9(7)
C15271(2)6034.6(19)6194(2)19.1(6)
C25614(3)6735(2)6221(2)20.4(6)
N27168(3)7020(2)5487(2)32.4(8)
C149362(3)2129.1(19)6054(2)20.3(6)
N43693(3)-487(2)5707(2)35.5(8)
C35784(3)5495(2)5773(2)21.0(6)
C911587(3)8148(2)6658(2)21.0(6)
N78311(3)3816.9(19)5786(2)32.9(8)
N34887(3)1483(2)5252(3)43.1(10)
C53464(3)1357(2)6162(2)19.8(6)
N510339(3)9207(2)6645(2)36.1(8)
C74250(3)1405(2)5646(2)27.9(8)
C46481(3)6893(2)5812(2)23.6(7)
C139589(2)2845.5(18)6186(2)17.9(6)
N95903(3)3145(2)5357(2)41.5(9)
N87700(3)1809(2)5393(3)38.1(9)
N69662(3)7347(2)5629(2)34.7(8)
C1110886(3)8733(2)6639(2)25.2(7)
C175325(4)3400(2)5737(3)37.7(10)
N128060(3)8767(3)5459(3)45.7(10)
C1011345(3)7500(2)6325(2)21.9(7)
C1210400(3)7422(2)5945(2)27.3(8)
C158880(3)3383(2)5965(2)24.4(7)
N118243(4)5224(3)4432(4)66.1(16)
C168437(3)1954(2)5694(2)27.0(7)
C238332(3)9330(3)5303(3)35.7(10)
C248654(4)10049(3)5078(3)42.8(11)
C184568(5)3731(3)6188(3)49.3(14)
C218533(5)5385(3)5021(5)65(2)
N1010037(7)4980(7)2478(5)147(4)
N138431(5)9320(4)7629(4)95(2)
N147881(6)10969(4)7228(4)89(2)
C1910519(7)5133(7)1903(5)105(3)
C2011098(6)5316(8)1245(6)133(5)
C277167(10)11348(6)7245(6)121(4)
C257950(6)8810(5)7539(4)78(2)
C228851(7)5577(4)5816(6)106(4)
C267378(13)8157(9)7383(8)212(10)
C286049(17)11708(10)7289(8)264(13)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for Cm_mnt_beta. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Cm116.56(5)14.18(5)16.85(5)0.29(4)3.04(3)-0.81(4)
S319.1(4)17.2(3)23.6(4)0.2(3)5.4(3)-2.5(3)
S118.7(4)17.6(4)22.6(4)-3.2(3)5.4(3)-0.4(3)
S820.4(4)15.4(3)26.4(4)-2.4(3)-1.7(3)0.2(3)
S426.7(4)15.8(4)34.1(5)-1.5(3)13.7(4)-1.4(3)
S518.2(4)18.8(4)33.0(5)4.8(3)-4.7(3)-0.6(3)
S722.7(4)15.4(4)26.4(4)1.4(3)-3.5(3)-4.0(3)
S226.9(4)19.0(4)35.0(5)-3.7(4)13.9(4)-2.8(3)
S643.1(6)37.3(6)30.6(5)-17.3(4)-14.8(5)16.9(5)
Na313.7(6)23.1(7)16.0(6)-1.4(5)2.0(5)2.3(5)
Na224.4(7)21.6(7)26.6(8)-2.0(6)-0.1(6)5.0(6)
Na119.6(7)34.3(8)21.9(7)4.1(6)1.1(5)-3.1(6)
Na531.1(9)47.6(11)24.8(8)-14.5(7)5.1(7)-15.2(8)
Na457.2(12)27.2(9)38.7(11)4.1(8)-7.2(9)-8.1(9)
N128.8(17)26.3(16)33.4(18)-2.5(14)9.2(14)3.5(14)
C618.5(15)21.1(16)21.2(16)-1.9(12)2.8(12)-0.4(12)
C823.2(17)24.6(17)24.3(18)-1.8(14)4.8(13)0.5(14)
C117.3(14)21.2(15)19.1(15)-2.1(12)3.2(12)2.7(12)
C216.6(14)22.0(15)23.0(17)0.8(12)5.3(12)1.0(12)
N227.6(17)35.3(19)35.0(19)0.4(15)9.0(14)-1.9(15)
C1420.3(15)14.6(13)26.0(17)1.1(12)-0.7(13)-1.3(12)
N434.6(19)29.3(18)44(2)-6.5(16)15.2(16)2.7(15)
C319.3(15)22.8(16)21.1(16)-1.5(13)3.1(12)-0.9(13)
C917.2(14)25.5(17)20.3(16)2.7(13)1.3(12)0.3(13)
N734.6(19)21.6(16)42(2)1.3(14)-7.8(16)4.0(14)
N346(2)31.0(19)55(3)-1.5(18)29(2)0.6(18)
C518.6(15)22.4(16)18.6(16)-1.1(12)3.4(12)1.2(13)
N523.6(16)31.1(18)53(2)-2.9(17)-7.8(16)1.7(15)
C728.6(19)23.1(17)33(2)0.0(15)11.4(16)1.7(15)
C423.5(16)23.8(16)23.6(17)-0.2(14)3.0(13)0.9(14)
C1319.3(15)15.5(13)18.9(15)-0.1(11)0.5(12)-0.5(12)
N946(2)43(2)35(2)9.2(18)-3.2(18)-10.1(19)
N829.9(18)26.7(18)57(3)-3.9(16)-10.4(17)-0.8(14)
N631.0(18)39(2)33(2)-1.0(16)-10.1(15)-1.8(16)
C1120.8(16)28.1(18)26.2(19)1.4(14)-4.2(13)-2.9(14)
C1755(3)26(2)31(2)4.8(17)-4(2)-16(2)
N1250(3)42(2)45(3)-2.3(19)-1(2)5(2)
C1021.0(16)26.3(17)18.0(16)-1.3(13)-3.0(12)1.3(14)
C1229.9(19)31.3(19)20.3(17)-1.4(14)-3.0(14)1.4(16)
C1529.5(18)18.0(16)25.2(18)0.6(13)-5.3(14)-1.3(14)
N1157(3)32(2)111(5)5(3)20(3)-10(2)
C1626.7(18)19.7(16)34(2)-0.1(15)-3.4(15)0.5(15)
C2330(2)38(2)39(2)-11.9(19)-2.7(17)5.8(18)
C2442(3)36(2)49(3)-8(2)-8(2)0(2)
C1871(4)33(2)45(3)-8(2)19(3)-19(3)
C2152(4)19(2)123(7)7(3)-3(4)-8(2)
N10109(7)264(14)64(5)-44(7)-39(5)-12(8)
N1394(5)96(5)97(6)-15(4)24(4)-41(4)
N1487(5)82(5)97(5)19(4)1(4)3(4)
C1989(6)165(10)59(5)23(6)-28(5)-16(7)
C2056(5)250(14)93(7)101(8)23(4)19(7)
C27159(11)115(9)90(7)24(6)9(7)63(8)
C2587(6)86(6)62(4)-1(4)7(4)-36(5)
C22132(8)29(3)151(9)-6(4)-84(7)5(4)
C26280(19)226(16)135(11)-83(11)72(12)-206(15)
C28450(30)216(17)117(11)-29(11)-79(15)250(20)

 

Table 4 Bond Lengths for Cm_mnt_beta.
AtomAtomLength/Å AtomAtomLength/Å
Cm1S32.8327(9) Na1N62.397(4)
Cm1S112.9017(8) Na1N122.483(5)
Cm1S822.8965(9) Na5N112.510(7)
Cm1S42.8564(9) Na5N102.531(10)
Cm1S532.8698(9) Na4N52.459(4)
Cm1S722.9007(9) Na4N132.395(7)
Cm1S212.8637(9) Na4N142.518(8)
Cm1S632.8470(11) N1C31.146(5)
Cm1Na143.9278(15) C6C81.430(5)
S3Na142.9138(18) C6C51.370(5)
S3C51.731(4) C8N41.150(5)
S1Na243.0601(18) C1C21.369(5)
S1Na432.884(2) C1C31.436(5)
S1C11.743(4) C2C41.442(5)
S8Na153.1866(18) N2C41.146(5)
S8Na462.877(2) C14C131.368(5)
S8C141.744(4) C14C161.429(5)
S4Na572.9336(19) C9C111.440(5)
S4C61.730(4) C9C101.360(5)
S5Na353.1835(17) N7C151.148(5)
S5Na583.074(2) N3C71.144(5)
S5C91.733(4) C5C71.437(5)
S7Na153.0107(19) N5C111.149(5)
S7Na553.127(2) C13C151.427(5)
S7C131.735(4) N9C171.154(7)
S2Na343.0290(18) N8C161.150(5)
S2C21.726(4) N6C121.142(5)
S6Na252.8232(19) C17C181.463(8)
S6C101.731(4) N12C231.135(7)
Na3N492.581(4) C10C121.438(5)
Na3N32.474(4) N11C211.127(9)
Na3N92.831(5) C23C241.450(7)
Na3N82.483(4) C21C221.482(12)
Na2N12.403(4) N10C191.257(12)
Na2N72.427(4) N13C251.152(9)
Na2N92.558(4) N14C271.201(12)
Na2N112.739(5) C19C201.466(12)
Na2C213.127(6) C27C281.67(2)
Na1N22.402(4) C25C261.451(12)

11/2-X,-1/2+Y,3/2-Z; 2-1+X,+Y,+Z; 33/2-X,-1/2+Y,3/2-Z; 41-X,1-Y,1-Z; 52-X,1-Y,1-Z; 6+X,-1+Y,+Z; 7-1/2+X,1/2-Y,1/2+Z; 81/2+X,3/2-Y,1/2+Z; 91-X,-Y,1-Z

 

Table 5 Bond Angles for Cm_mnt_beta.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
S3Cm1S11136.55(3) N9Na2C21151.8(2)
S3Cm1S8295.34(3) N11Na2S1492.76(16)
S3Cm1S472.66(3) N11Na2S6787.93(14)
S3Cm1S5373.32(3) N11Na2C2120.83(19)
S3Cm1S7280.90(3) S34Na1Cm1446.02(3)
S3Cm1S21151.02(3) S34Na1S8787.83(5)
S3Cm1S6385.75(3) S34Na1S7777.78(5)
S3Cm1Na1447.75(3) S87Na1Cm1446.62(3)
S11Cm1Na14135.88(3) S77Na1Cm1447.17(3)
S82Cm1S1186.77(3) S77Na1S8764.18(4)
S82Cm1S7269.29(2) N2Na1Cm14134.26(11)
S82Cm1Na1453.10(3) N2Na1S3491.09(11)
S4Cm1S1166.98(3) N2Na1S87174.50(12)
S4Cm1S8271.44(3) N2Na1S77120.83(11)
S4Cm1S53138.56(3) N2Na1N1289.22(15)
S4Cm1S72129.66(3) N6Na1Cm14127.42(11)
S4Cm1S21135.86(3) N6Na1S34170.66(12)
S4Cm1Na1481.69(3) N6Na1S8789.23(11)
S53Cm1S11131.54(3) N6Na1S7792.96(11)
S53Cm1S82134.89(3) N6Na1N292.66(15)
S53Cm1S7265.86(3) N6Na1N1288.73(15)
S53Cm1Na1492.51(3) N12Na1Cm14110.13(12)
S72Cm1S11138.46(3) N12Na1S3499.88(12)
S72Cm1Na1449.57(3) N12Na1S8785.65(12)
S21Cm1S1171.87(3) N12Na1S77149.75(13)
S21Cm1S8291.32(3) S413Na5S51487.28(6)
S21Cm1S5382.03(3) S413Na5S77147.89(8)
S21Cm1S7275.18(3) S514Na5S7760.77(4)
S21Cm1Na14120.35(3) N11Na5S413120.07(14)
S63Cm1S1174.83(3) N11Na5S514122.09(14)
S63Cm1S82153.63(3) N11Na5S7783.10(13)
S63Cm1S483.89(4) N11Na5N10117.9(2)
S63Cm1S5370.64(3) N10Na5S41397.7(2)
S63Cm1S72136.48(3) N10Na5S514105.7(3)
S63Cm1S21100.43(4) N10Na5S7788.7(3)
S63Cm1Na14133.50(3) S815Na4S11087.49(6)
Cm1S3Na1486.23(4) N5Na4S110100.69(11)
C5S3Cm1108.41(12) N5Na4S815101.16(12)
C5S3Na1491.46(13) N5Na4N14150.4(2)
Cm15S1Na24100.42(4) N13Na4S110107.7(2)
Na43S1Cm1592.72(5) N13Na4S815163.6(2)
Na43S1Na24166.59(6) N13Na4N582.5(2)
C1S1Cm15108.05(12) N13Na4N1480.9(3)
C1S1Na2492.30(13) N14Na4S110107.67(19)
C1S1Na4386.09(13) N14Na4S81588.68(17)
Cm16S8Na1780.28(4) C3N1Na2177.0(3)
Na48S8Cm1692.97(5) C8C6S4115.4(3)
Na48S8Na17160.71(6) C5C6S4125.1(3)
C14S8Cm16104.94(12) C5C6C8119.5(3)
C14S8Na1785.65(13) N4C8C6175.9(4)
C14S8Na48113.61(13) C2C1S1124.5(3)
Cm1S4Na59119.10(5) C2C1C3119.3(3)
C6S4Cm1107.99(12) C3C1S1116.2(3)
C6S4Na5993.03(13) C1C2S2126.5(3)
Cm110S5Na3787.25(4) C1C2C4117.5(3)
Cm110S5Na511117.97(4) C4C2S2116.0(3)
Na511S5Na37114.07(5) C4N2Na1162.5(3)
C9S5Cm110106.12(13) C13C14S8123.1(3)
C9S5Na3790.23(13) C13C14C16118.8(3)
C9S5Na511129.54(13) C16C14S8117.8(3)
Cm16S7Na1783.26(4) C8N4Na312155.7(3)
Cm16S7Na57115.37(5) N1C3C1178.4(4)
Na17S7Na57115.51(5) C11C9S5117.0(3)
C13S7Cm16104.96(12) C10C9S5123.6(3)
C13S7Na1788.28(12) C10C9C11119.4(3)
C13S7Na57134.57(12) C15N7Na2142.7(3)
Cm15S2Na3490.39(4) C7N3Na3169.7(4)
C2S2Cm15108.79(12) C6C5S3125.6(3)
C2S2Na34102.02(13) C6C5C7119.8(3)
Na27S6Cm110107.82(5) C7C5S3114.6(3)
C10S6Cm110106.76(13) C11N5Na4159.0(4)
C10S6Na27134.68(14) N3C7C5175.9(5)
S24Na3S5774.50(4) N2C4C2179.8(5)
N412Na3S5775.88(9) C14C13S7124.2(3)
N412Na3S24109.06(11) C14C13C15118.1(3)
N412Na3N9152.48(13) C15C13S7117.6(3)
N3Na3S57144.32(12) Na2N9Na3103.75(16)
N3Na3S2491.22(12) C17N9Na3141.4(4)
N3Na3N41278.43(13) C17N9Na2112.5(3)
N3Na3N978.13(13) C16N8Na3159.9(4)
N3Na3N8103.88(17) C12N6Na1156.8(4)
N9Na3S57131.38(10) N5C11C9177.8(4)
N9Na3S2485.65(10) N9C17C18177.5(6)
N8Na3S57100.66(12) C23N12Na1125.5(4)
N8Na3S24157.55(11) C9C10S6124.7(3)
N8Na3N41290.44(14) C9C10C12118.9(3)
N8Na3N981.42(13) C12C10S6116.4(3)
S14Na2C21111.65(16) N6C12C10178.0(5)
S67Na2S1472.72(5) N7C15C13179.8(5)
S67Na2C21101.67(16) Na5N11Na2112.5(2)
N1Na2S1491.79(10) C21N11Na299.4(5)
N1Na2S67161.67(11) C21N11Na5147.1(5)
N1Na2N7100.96(14) N8C16C14178.7(5)
N1Na2N990.36(15) N12C23C24177.8(6)
N1Na2N1182.98(16) N11C21Na259.8(4)
N1Na2C2174.51(17) N11C21C22176.1(8)
N7Na2S14166.70(11) C22C21Na2116.8(5)
N7Na2S6794.06(11) C19N10Na5137.7(9)
N7Na2N991.63(14) C25N13Na4150.4(7)
N7Na2N1185.14(18) C27N14Na4175.4(8)
N7Na2C2168.85(17) N10C19C20178.7(10)
N9Na2S1492.06(11) N14C27C28167.9(15)
N9Na2S6799.73(12) N13C25C26176.4(10)
N9Na2N11171.89(19)     

11/2-X,-1/2+Y,3/2-Z; 2-1+X,+Y,+Z; 33/2-X,-1/2+Y,3/2-Z; 41-X,1-Y,1-Z; 51/2-X,1/2+Y,3/2-Z; 61+X,+Y,+Z; 72-X,1-Y,1-Z; 8+X,-1+Y,+Z; 9-1/2+X,1/2-Y,1/2+Z; 103/2-X,1/2+Y,3/2-Z; 111/2+X,3/2-Y,1/2+Z; 121-X,-Y,1-Z; 131/2+X,1/2-Y,-1/2+Z; 14-1/2+X,3/2-Y,-1/2+Z; 15+X,1+Y,+Z

 

Table 6 Torsion Angles for Cm_mnt_beta.
ABCDAngle/˚ ABCDAngle/˚
Cm1S3C5C6-4.1(4) Na25S1C1C3-83.5(3)
Cm1S3C5C7177.1(3) Na24S6C10C9-118.6(3)
Cm11S1C1C2-4.9(4) Na24S6C10C1262.0(4)
Cm11S1C1C3174.8(2) Na15S3C5C6-90.7(3)
Cm12S8C14C1329.0(3) Na15S3C5C790.6(3)
Cm12S8C14C16-157.1(3) Na14S8C14C13-49.7(3)
Cm1S4C6C8-174.3(3) Na14S8C14C16124.2(3)
Cm1S4C6C54.3(4) Na14S7C13C1456.0(3)
Cm13S5C9C11157.3(3) Na14S7C13C15-120.4(3)
Cm13S5C9C10-23.7(3) Na56S4C6C863.7(3)
Cm12S7C13C14-26.5(3) Na56S4C6C5-117.7(3)
Cm12S7C13C15157.0(3) Na57S5C9C116.6(4)
Cm11S2C2C12.9(4) Na57S5C9C10-174.4(3)
Cm11S2C2C4-175.8(3) Na54S7C13C14-178.9(2)
Cm13S6C10C919.7(4) Na54S7C13C154.7(4)
Cm13S6C10C12-159.7(3) Na5N11C21Na2-165.8(10)
S1C1C2S21.5(5) Na48S1C1C2-96.5(3)
S1C1C2C4-179.8(3) Na48S1C1C383.2(3)
S8C14C13S7-1.7(5) Na49S8C14C13129.1(3)
S8C14C13C15174.7(3) Na49S8C14C16-57.0(3)
S4C6C5S3-0.1(5) C8C6C5S3178.4(3)
S4C6C5C7178.5(3) C8C6C5C7-2.9(6)
S5C9C10S63.1(5) C3C1C2S2-178.1(3)
S5C9C10C12-177.5(3) C3C1C2C40.5(5)
Na34S5C9C11-115.5(3) C11C9C10S6-178.0(3)
Na34S5C9C1063.5(3) C11C9C10C121.4(5)
Na35S2C2C1-91.7(3) C16C14C13S7-175.6(3)
Na35S2C2C489.6(3) C16C14C13C150.8(5)
Na25S1C1C296.8(3)      

11/2-X,1/2+Y,3/2-Z; 21+X,+Y,+Z; 33/2-X,1/2+Y,3/2-Z; 42-X,1-Y,1-Z; 51-X,1-Y,1-Z; 6-1/2+X,1/2-Y,1/2+Z; 71/2+X,3/2-Y,1/2+Z; 83/2-X,-1/2+Y,3/2-Z; 9+X,-1+Y,+Z

Experimental

Single crystals of C28CmN14Na5S8 [Cm_mnt_beta] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 100.00 K during data collection. Using Olex2 [1], the structure was solved with the Unknown [2] structure solution program using Unknown and refined with the Unknown [3] refinement package using Unknown minimisation.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.

Crystal structure determination of [Cm_mnt_beta]

Crystal Data for C28CmN14Na5S8 (=1147.85 g/mol): monoclinic, space group P21/n (no. 14), a = 13.7182(5) Å, b = 18.3443(7) Å, c = 17.4906(6) Å, β = 92.4140(10)°, = 4397.6(3) Å3, Z = 4, T = 100.00 K, μ(MoKα) = 2.322 mm-1, Dcalc = 1.734 g/cm3, 95942 reflections measured (3.698° ≤ 2Θ ≤ 66.466°), 16847 unique (Rint = 0.0572, Rsigma = 0.0416) which were used in all calculations. The final R1 was 0.0390 (I > 2σ(I)) and wR2 was 0.0878 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

N/A

This report has been created with Olex2, compiled on 2020.11.12 svn.r5f609507 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.