3118

Table 1 Crystal data and structure refinement for 3118.
Identification code 3118
Empirical formula C46H52Cl2Fe4N2O4Si2Zn2
Formula weight 1178.11
Temperature/K 173.15
Crystal system orthorhombic
Space group Pbcn
a/Å 15.0001(6)
b/Å 11.2793(5)
c/Å 27.6027(12)
α/° 90
β/° 90
γ/° 90
Volume/Å3 4670.1(3)
Z 4
ρcalcg/cm3 1.676
μ/mm‑1 2.431
F(000) 2400.0
Crystal size/mm3 0.2 × 0.1 × 0.05
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.518 to 53.998
Index ranges -19 ≤ h ≤ 19, -13 ≤ k ≤ 14, -35 ≤ l ≤ 34
Reflections collected 35271
Independent reflections 5097 [Rint = 0.0431, Rsigma = 0.0282]
Data/restraints/parameters 5097/1/287
Goodness-of-fit on F2 1.082
Final R indexes [I>=2σ (I)] R1 = 0.0449, wR2 = 0.1050
Final R indexes [all data] R1 = 0.0607, wR2 = 0.1138
Largest diff. peak/hole / e Å-3 0.73/-0.61

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3118. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn150003675.8(5)250021.20(14)
Zn250001082.3(5)250024.77(15)
Fe16088.8(4)4935.5(5)4123.2(2)26.12(14)
Fe23988.0(4)294.5(5)4131.9(2)32.05(16)
Cl13815.8(8)53.0(12)2280.8(4)51.7(3)
Si15137.5(6)2544.3(8)3535.4(4)21.1(2)
O14873.8(15)2388(2)2972.8(9)23.8(5)
O26095.5(17)1893(2)3646.1(10)30.7(6)
N16188(2)4558(3)2522.0(11)30.6(7)
C15261(2)4163(3)3634.2(12)21.7(7)
C25893(2)4930(3)3397.3(12)25.4(8)
C35772(3)6095(3)3583.7(14)33.1(9)
C45075(3)6066(3)3928.2(15)34.9(9)
C54761(2)4890(3)3957.5(13)26.4(8)
C66646(3)3609(4)4517.5(14)36.7(10)
C77298(3)4183(5)4245.7(16)45.7(11)
C87314(3)5372(5)4388.0(18)56.6(14)
C96658(4)5522(4)4747.5(16)53.1(13)
C106247(3)4426(4)4826.3(14)40.9(10)
C116554(2)4533(4)3030.0(13)29.8(8)
C126144(3)5802(4)2348.9(16)49.4(13)
C136821(3)3892(5)2201.3(16)50.4(13)
C144226(2)2004(3)3918.2(14)27.0(8)
C154196(3)1920(3)4430.6(15)36.4(10)
C163349(3)1472(4)4571.6(19)50.2(13)
C172848(3)1264(4)4149(2)54.6(15)
C183373(3)1583(4)3743.3(17)38.4(10)
C194965(3)-782(4)3874.2(19)46.0(12)
C204939(4)-838(4)4378.2(19)49.8(12)
C214100(5)-1226(5)4509(2)70.1(19)
C223602(4)-1405(4)4094(4)88(3)
C234145(5)-1138(4)3698(2)70.3(19)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3118. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Zn120.8(3)25.8(3)17.1(3)00.3(2)0
Zn227.1(3)24.8(3)22.4(3)0-1.8(2)0
Fe136.5(3)24.7(3)17.2(3)-2.4(2)-1.1(2)-2.4(2)
Fe234.0(3)21.6(3)40.5(4)9.7(2)7.6(2)2.5(2)
Cl145.8(6)66.5(8)42.8(6)10.1(6)-5.2(5)-29.9(6)
Si123.8(5)21.3(5)18.1(5)0.9(4)0.4(4)2.4(4)
O128.9(13)24.5(13)18.1(12)0.3(10)-0.9(10)0.2(10)
O227.3(13)34.1(15)30.7(15)-5.4(12)-5.1(11)7.8(11)
N131.0(16)42.6(19)18.2(15)-3.8(14)4.9(12)-14.1(15)
C124.7(17)24.9(18)15.7(16)1.8(14)-1.5(13)1.9(14)
C233.2(19)26.3(18)16.8(17)1.2(14)-0.9(14)-4.6(16)
C353(2)21.3(18)25(2)1.9(16)-1.6(18)-5.0(17)
C452(3)23.2(19)29(2)-1.2(17)0.4(18)11.5(18)
C531.7(19)25.8(19)21.7(18)1.5(15)4.0(15)10.0(15)
C644(2)39(2)27(2)2.0(18)-13.4(18)5.9(19)
C732(2)72(3)32(2)-6(2)-9.2(18)8(2)
C857(3)68(3)44(3)9(3)-19(2)-27(3)
C984(4)47(3)29(2)-16(2)-24(2)6(3)
C1047(2)57(3)18(2)1(2)-4.6(17)7(2)
C1126.1(18)42(2)21.3(19)-4.1(17)0.8(14)-10.9(16)
C1262(3)57(3)30(2)8(2)-1(2)-28(3)
C1328(2)92(4)31(2)-26(2)9.2(18)-16(2)
C1433.0(19)18.3(17)30(2)4.9(15)6.5(16)5.3(15)
C1554(3)25(2)31(2)2.4(17)14.0(19)5.7(18)
C1662(3)36(2)53(3)13(2)34(3)12(2)
C1737(2)35(2)92(4)26(3)25(3)8(2)
C1834(2)30(2)51(3)14(2)2.1(19)5.0(17)
C1959(3)23(2)56(3)7(2)20(2)13(2)
C2066(3)33(2)50(3)0(2)-10(2)19(2)
C2191(4)41(3)78(4)38(3)45(4)29(3)
C2246(3)21(2)197(9)12(4)-3(4)-8(2)
C23116(5)31(3)64(4)-9(3)-37(4)17(3)

 

Table 4 Bond Lengths for 3118.
AtomAtomLength/Å AtomAtomLength/Å
Zn1Zn22.9253(9) Si1O11.612(3)
Zn1O111.962(2) Si1O21.643(3)
Zn1O11.962(2) Si1C11.856(4)
Zn1N12.042(3) Si1C141.832(4)
Zn1N112.042(3) N1C111.506(5)
Zn2Cl112.2067(11) N1C121.483(6)
Zn2Cl12.2067(11) N1C131.499(5)
Zn2O111.977(2) C1C21.440(5)
Zn2O11.977(2) C1C51.425(5)
Fe1C12.030(3) C2C31.422(5)
Fe1C22.025(3) C2C111.487(5)
Fe1C32.038(4) C3C41.414(6)
Fe1C42.057(4) C4C51.410(5)
Fe1C52.044(4) C6C71.392(6)
Fe1C62.030(4) C6C101.390(6)
Fe1C72.031(4) C7C81.398(7)
Fe1C82.038(5) C8C91.407(7)
Fe1C92.034(4) C9C101.399(7)
Fe1C102.038(4) C14C151.418(6)
Fe2C142.048(4) C14C181.447(6)
Fe2C152.034(4) C15C161.421(6)
Fe2C162.039(4) C16C171.408(8)
Fe2C172.030(4) C17C181.416(6)
Fe2C182.028(4) C19C201.393(7)
Fe2C192.032(4) C19C231.383(8)
Fe2C202.032(4) C20C211.380(8)
Fe2C212.012(5) C21C221.381(10)
Fe2C222.005(5) C22C231.397(9)
Fe2C232.025(5)    

11-X,+Y,1/2-Z

 

Table 5 Bond Angles for 3118.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O11Zn1Zn242.24(7) C22Fe2C18121.8(3)
O1Zn1Zn242.24(7) C22Fe2C1967.6(2)
O1Zn1O1184.49(14) C22Fe2C2067.6(2)
O11Zn1N11115.17(12) C22Fe2C2140.2(3)
O1Zn1N11107.24(11) C22Fe2C2340.6(3)
O11Zn1N1107.24(11) C23Fe2C14124.1(2)
O1Zn1N1115.16(12) C23Fe2C15160.2(3)
N11Zn1Zn2119.17(10) C23Fe2C16157.9(3)
N1Zn1Zn2119.17(10) C23Fe2C17122.8(3)
N11Zn1N1121.7(2) C23Fe2C18108.2(2)
Cl1Zn2Zn1121.74(4) C23Fe2C1939.9(2)
Cl11Zn2Zn1121.74(4) C23Fe2C2067.3(2)
Cl1Zn2Cl11116.51(8) O1Si1O2110.18(14)
O11Zn2Zn141.83(7) O1Si1C1105.86(14)
O1Zn2Zn141.83(7) O1Si1C14109.64(16)
O1Zn2Cl11106.74(7) O2Si1C1109.00(15)
O11Zn2Cl11119.73(8) O2Si1C14113.38(16)
O1Zn2Cl1119.73(8) C14Si1C1108.48(16)
O11Zn2Cl1106.74(7) Zn1O1Zn295.92(11)
O11Zn2O183.67(14) Si1O1Zn1122.45(14)
C1Fe1C369.31(15) Si1O1Zn2133.92(14)
C1Fe1C468.88(15) C11N1Zn1109.6(2)
C1Fe1C540.94(14) C12N1Zn1114.3(3)
C1Fe1C7118.53(17) C12N1C11109.5(3)
C1Fe1C8153.32(19) C12N1C13108.2(3)
C1Fe1C9163.66(19) C13N1Zn1106.9(2)
C1Fe1C10125.70(17) C13N1C11108.1(3)
C2Fe1C141.60(14) Si1C1Fe1125.51(18)
C2Fe1C340.98(15) C2C1Fe169.0(2)
C2Fe1C468.62(16) C2C1Si1126.2(3)
C2Fe1C568.72(15) C5C1Fe170.1(2)
C2Fe1C6126.03(16) C5C1Si1127.3(3)
C2Fe1C7107.06(17) C5C1C2106.6(3)
C2Fe1C8119.11(18) C1C2Fe169.40(19)
C2Fe1C9154.18(19) C1C2C11124.6(3)
C2Fe1C10163.41(17) C3C2Fe170.0(2)
C3Fe1C440.39(16) C3C2C1107.8(3)
C3Fe1C567.99(16) C3C2C11127.6(3)
C5Fe1C440.22(15) C11C2Fe1125.3(3)
C6Fe1C1106.97(16) C2C3Fe169.0(2)
C6Fe1C3163.88(18) C4C3Fe170.5(2)
C6Fe1C4154.37(18) C4C3C2108.5(3)
C6Fe1C5120.15(17) C3C4Fe169.1(2)
C6Fe1C740.11(18) C5C4Fe169.4(2)
C6Fe1C867.3(2) C5C4C3107.9(3)
C6Fe1C967.22(18) C1C5Fe169.0(2)
C6Fe1C1039.97(17) C4C5Fe170.4(2)
C7Fe1C3126.76(19) C4C5C1109.2(3)
C7Fe1C4164.43(19) C7C6Fe170.0(3)
C7Fe1C5153.75(18) C10C6Fe170.3(2)
C7Fe1C840.2(2) C10C6C7108.9(4)
C7Fe1C967.7(2) C6C7Fe169.9(2)
C7Fe1C1067.63(18) C6C7C8107.9(4)
C8Fe1C3108.52(19) C8C7Fe170.2(3)
C8Fe1C4127.7(2) C7C8Fe169.6(3)
C8Fe1C5164.8(2) C7C8C9107.6(4)
C9Fe1C3120.55(18) C9C8Fe169.6(3)
C9Fe1C4109.30(19) C8C9Fe169.9(3)
C9Fe1C5127.36(19) C10C9Fe170.1(2)
C9Fe1C840.4(2) C10C9C8108.1(4)
C9Fe1C1040.17(19) C6C10Fe169.7(2)
C10Fe1C3154.68(18) C6C10C9107.5(4)
C10Fe1C4120.68(17) C9C10Fe169.8(2)
C10Fe1C5108.64(17) C2C11N1112.7(3)
C10Fe1C867.75(19) Si1C14Fe2127.54(19)
C15Fe2C1440.67(15) C15C14Fe269.1(2)
C15Fe2C1640.83(18) C15C14Si1128.4(3)
C16Fe2C1468.89(16) C15C14C18106.4(3)
C17Fe2C1469.29(16) C18C14Fe268.5(2)
C17Fe2C1568.5(2) C18C14Si1125.2(3)
C17Fe2C1640.5(2) C14C15Fe270.2(2)
C17Fe2C19159.6(2) C14C15C16109.0(4)
C17Fe2C20157.2(2) C16C15Fe269.8(3)
C18Fe2C1441.58(16) C15C16Fe269.4(2)
C18Fe2C1568.78(18) C17C16Fe269.4(3)
C18Fe2C1668.5(2) C17C16C15108.0(4)
C18Fe2C1740.84(18) C16C17Fe270.1(3)
C18Fe2C19124.81(19) C16C17C18108.4(4)
C18Fe2C20161.2(2) C18C17Fe269.5(2)
C19Fe2C14109.63(16) C14C18Fe269.9(2)
C19Fe2C15124.74(19) C17C18Fe269.7(2)
C19Fe2C16159.5(2) C17C18C14108.2(4)
C20Fe2C14124.49(19) C20C19Fe269.9(3)
C20Fe2C15108.9(2) C23C19Fe269.8(3)
C20Fe2C16122.7(2) C23C19C20108.2(5)
C20Fe2C1940.1(2) C19C20Fe270.0(3)
C21Fe2C14159.5(3) C21C20Fe269.3(3)
C21Fe2C15123.1(2) C21C20C19107.6(5)
C21Fe2C16106.7(2) C20C21Fe270.8(3)
C21Fe2C17121.1(2) C20C21C22108.8(5)
C21Fe2C18157.2(2) C22C21Fe269.6(3)
C21Fe2C1967.2(2) C21C22Fe270.2(3)
C21Fe2C2039.9(2) C21C22C23107.6(5)
C21Fe2C2367.4(3) C23C22Fe270.5(3)
C22Fe2C14159.3(3) C19C23Fe270.4(3)
C22Fe2C15157.9(3) C19C23C22107.9(5)
C22Fe2C16121.2(3) C22C23Fe269.0(3)
C22Fe2C17105.8(2)     

11-X,+Y,1/2-Z

 

Table 6 Torsion Angles for 3118.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C11C2-51.2(4) C1C2C3C4-0.4(4)
Fe1C1C2C3-59.7(3) C1C2C11N188.1(4)
Fe1C1C2C11119.4(4) C2C1C5Fe1-59.6(2)
Fe1C1C5C459.0(3) C2C1C5C4-0.6(4)
Fe1C2C3C4-59.7(3) C2C3C4Fe158.8(3)
Fe1C2C11N1176.1(2) C2C3C4C50.0(5)
Fe1C3C4C5-58.8(3) C3C2C11N1-92.9(5)
Fe1C4C5C1-58.2(3) C3C4C5Fe158.6(3)
Fe1C6C7C860.2(3) C3C4C5C10.4(4)
Fe1C6C10C9-59.8(3) C5C1C2Fe160.3(2)
Fe1C7C8C959.5(3) C5C1C2C30.6(4)
Fe1C8C9C1059.9(3) C5C1C2C11179.7(3)
Fe1C9C10C659.7(3) C6C7C8Fe1-60.0(3)
Fe2C14C15C16-59.2(3) C6C7C8C9-0.5(5)
Fe2C14C18C1759.4(3) C7C6C10Fe159.6(3)
Fe2C15C16C17-58.9(3) C7C6C10C9-0.2(5)
Fe2C16C17C18-59.1(3) C7C8C9Fe1-59.5(3)
Fe2C17C18C14-59.6(3) C7C8C9C100.4(5)
Fe2C19C20C2159.3(3) C8C9C10Fe1-59.8(3)
Fe2C19C23C22-59.0(4) C8C9C10C6-0.1(5)
Fe2C20C21C2259.4(4) C10C6C7Fe1-59.8(3)
Fe2C21C22C2360.9(4) C10C6C7C80.4(5)
Fe2C22C23C1959.9(3) C11C2C3Fe1-119.8(4)
Si1C1C2Fe1-119.3(3) C11C2C3C4-179.5(4)
Si1C1C2C3-179.0(3) C12N1C11C275.0(4)
Si1C1C2C110.1(5) C13N1C11C2-167.3(3)
Si1C1C5Fe1120.0(3) C14Si1O1Zn1131.01(17)
Si1C1C5C4179.0(3) C14Si1O1Zn2-87.6(2)
Si1C14C15Fe2-122.0(3) C14Si1C1Fe192.4(2)
Si1C14C15C16178.8(3) C14Si1C1C2-179.0(3)
Si1C14C18Fe2121.6(3) C14Si1C1C51.4(4)
Si1C14C18C17-179.1(3) C14C15C16Fe259.4(3)
O1Si1C1Fe1-150.04(19) C14C15C16C170.6(5)
O1Si1C1C2-61.4(3) C15C14C18Fe2-59.0(3)
O1Si1C1C5119.0(3) C15C14C18C170.4(4)
O1Si1C14Fe284.4(3) C15C16C17Fe258.8(3)
O1Si1C14C15176.5(3) C15C16C17C18-0.3(5)
O1Si1C14C18-4.2(4) C16C17C18Fe259.5(3)
O2Si1O1Zn1-103.54(17) C16C17C18C14-0.1(5)
O2Si1O1Zn237.9(2) C18C14C15Fe258.6(3)
O2Si1C1Fe1-31.5(3) C18C14C15C16-0.6(4)
O2Si1C1C257.1(3) C19C20C21Fe2-59.8(3)
O2Si1C1C5-122.5(3) C19C20C21C22-0.3(6)
O2Si1C14Fe2-39.2(3) C20C19C23Fe259.6(3)
O2Si1C14C1552.9(4) C20C19C23C220.6(5)
O2Si1C14C18-127.8(3) C20C21C22Fe2-60.2(4)
C1Si1O1Zn114.2(2) C20C21C22C230.7(6)
C1Si1O1Zn2155.61(19) C21C22C23Fe2-60.7(4)
C1Si1C14Fe2-160.4(2) C21C22C23C19-0.8(6)
C1Si1C14C15-68.4(4) C23C19C20Fe2-59.5(3)
C1Si1C14C18111.0(3) C23C19C20C21-0.2(5)
C1C2C3Fe159.3(2)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3118.
AtomxyzU(eq)
H26230(30)1470(40)3350(11)55(15)
H361036777349240
H448566723410842
H542904624416132
H664972792449644
H776673829400655
H876985970426468
H965196243490964
H1057814269505049
H11A67463715310836
H11B70855052304736
H12A57486260256174
H12B59125817201774
H12C67426151235574
H13A74234218223876
H13B66313970186376
H13C68223053229376
H1546662128464544
H1631551338489560
H172258960413865
H1831971531341346
H195462-540368455
H205412-645459360
H213897-1349483184
H222999-16634081106
H233980-1191336684

Experimental

Single crystals of C46H52Cl2Fe4N2O4Si2Zn2 [3118] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 K during data collection. Using Olex2 [1], the structure was solved with the ShelXS [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.

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

Crystal structure determination of [3118]

Crystal Data for C46H52Cl2Fe4N2O4Si2Zn2 (=1178.11 g/mol): orthorhombic, space group Pbcn (no. 60), a = 15.0001(6) Å, b = 11.2793(5) Å, c = 27.6027(12) Å, = 4670.1(3) Å3, Z = 4, T = 173.15 K, μ(MoKα) = 2.431 mm-1, Dcalc = 1.676 g/cm3, 35271 reflections measured (4.518° ≤ 2Θ ≤ 53.998°), 5097 unique (Rint = 0.0431, Rsigma = 0.0282) which were used in all calculations. The final R1 was 0.0449 (I > 2σ(I)) and wR2 was 0.1138 (all data).

Refinement model description

Number of restraints - 1, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
O2-H2
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)

This report has been created with Olex2, compiled on 2017.01.04 svn.r3372 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.