3105

Table 1 Crystal data and structure refinement for 3105.
Identification code 3105
Empirical formula C46H48Br2Fe2N2O4Si2Zn2
Formula weight 1151.30
Temperature/K 173
Crystal system monoclinic
Space group P21/c
a/Å 11.8205(7)
b/Å 10.6777(4)
c/Å 18.3320(6)
α/° 90
β/° 99.305(4)
γ/° 90
Volume/Å3 2283.34(17)
Z 2
ρcalcg/cm3 1.675
μ/mm‑1 3.508
F(000) 1160.0
Crystal size/mm3 0.2 × 0.1 × 0.05
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.43 to 52
Index ranges -14 ≤ h ≤ 14, -13 ≤ k ≤ 13, -22 ≤ l ≤ 22
Reflections collected 40953
Independent reflections 4482 [Rint = 0.0446, Rsigma = 0.0230]
Data/restraints/parameters 4482/0/277
Goodness-of-fit on F2 1.037
Final R indexes [I>=2σ (I)] R1 = 0.0516, wR2 = 0.1331
Final R indexes [all data] R1 = 0.0632, wR2 = 0.1424
Largest diff. peak/hole / e Å-3 2.89/-0.77

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3105. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br111263.1(6)1891.7(5)3859.8(3)57.1(2)
Zn110317.0(5)150.9(5)4264.6(3)35.88(17)
Fe16520.4(6)-547.6(6)2515.9(3)38.3(2)
Si17616.2(12)379.7(12)4319.8(7)35.8(3)
O18943(3)371(3)4729.2(16)36.4(7)
O26965(4)-878(4)4553(2)49.1(9)
N110147(3)-1295(4)3503(2)39.3(9)
C17621(4)384(4)3313(2)36.6(10)
C28230(4)-464(4)2899(2)37.3(10)
C38003(4)-110(5)2139(3)41.4(11)
C47278(4)946(5)2072(3)42.7(11)
C57030(4)1264(4)2789(3)38.8(10)
C65813(5)-2070(5)2940(3)49.8(13)
C76029(5)-2343(5)2235(3)55.0(14)
C85398(6)-1500(6)1743(3)61.5(16)
C94799(5)-700(6)2141(4)70.1(19)
C105064(5)-1069(7)2900(4)64.2(17)
C118907(4)-1579(4)3220(3)40.7(11)
C1210747(5)-993(6)2871(3)53.9(13)
C1310670(5)-2439(5)3873(3)53.0(13)
C146875(4)1791(4)4621(2)37.9(10)
C155936(5)1602(5)4970(3)48.1(12)
C165401(5)2578(6)5290(3)53.4(13)
C175842(5)3764(6)5287(3)52.6(14)
C186787(4)4028(5)4934(3)44.8(11)
C197259(6)5250(5)4938(3)57.8(15)
C208168(6)5488(5)4604(4)64.2(17)
C218687(5)4525(5)4242(3)54.3(13)
C228253(5)3327(5)4236(3)44.1(11)
C237294(4)3036(4)4583(2)39.2(10)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3105. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br172.9(4)49.2(3)49.6(3)8.2(2)11.2(3)-11.3(3)
Zn142.7(3)36.0(3)27.2(3)-0.6(2)0.3(2)-0.3(2)
Fe141.7(4)40.6(4)29.7(3)0.4(3)-3.0(3)-5.2(3)
Si140.1(7)36.2(6)29.4(6)-0.4(5)0.1(5)-2.8(5)
O140.9(18)39.5(17)27.2(14)0.4(12)0.7(13)1.7(14)
O258(2)47(2)39.4(19)4.9(16)-1.0(17)-11.1(18)
N144(2)41(2)30.5(18)-4.2(16)-0.6(16)5.2(17)
C142(3)35(2)32(2)-0.6(18)-0.8(18)-2.0(19)
C239(3)38(2)32(2)-1.9(18)-1.0(18)-4.0(19)
C348(3)45(3)30(2)-0.6(19)3(2)-8(2)
C446(3)44(3)35(2)9(2)-2(2)-6(2)
C539(2)36(2)39(2)2.0(19)-1.8(19)-3.4(19)
C652(3)53(3)43(3)6(2)1(2)-16(3)
C758(3)46(3)60(3)-8(3)7(3)-15(3)
C871(4)70(4)37(3)2(3)-9(3)-30(3)
C945(3)55(4)101(5)12(4)-17(3)-10(3)
C1052(3)77(4)67(4)-22(3)20(3)-26(3)
C1149(3)38(2)33(2)-4.2(19)0(2)1(2)
C1256(3)68(4)39(3)-12(2)8(2)-1(3)
C1359(3)44(3)52(3)-7(2)-4(3)12(3)
C1439(3)44(3)30(2)-0.9(18)1.1(18)3(2)
C1545(3)57(3)41(3)0(2)3(2)-5(2)
C1649(3)71(4)40(3)-3(3)8(2)2(3)
C1753(3)69(4)34(2)-9(2)2(2)16(3)
C1844(3)50(3)37(2)-5(2)-3(2)5(2)
C1967(4)45(3)59(3)-10(3)4(3)8(3)
C2083(5)38(3)71(4)-5(3)12(3)-10(3)
C2156(3)47(3)61(3)1(3)12(3)-9(3)
C2249(3)39(3)44(3)0(2)7(2)5(2)
C2341(3)42(3)31(2)0.3(18)-3.3(19)3(2)

 

Table 4 Bond Lengths for 3105.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.3506(8) C1C21.446(7)
Zn1Zn112.9305(10) C1C51.440(6)
Zn1O111.989(3) C2C31.427(6)
Zn1O11.966(3) C2C111.500(7)
Zn1N12.069(4) C3C41.410(7)
Fe1C12.050(4) C4C51.432(7)
Fe1C22.032(5) C6C71.388(8)
Fe1C32.039(5) C6C101.382(9)
Fe1C42.060(5) C7C81.400(9)
Fe1C52.063(5) C8C91.390(10)
Fe1C62.038(5) C9C101.430(9)
Fe1C72.045(5) C14C151.382(7)
Fe1C82.048(5) C14C231.424(7)
Fe1C92.046(6) C15C161.397(8)
Fe1C102.040(6) C16C171.370(9)
Si1O11.625(3) C17C181.407(8)
Si1O21.639(4) C18C191.419(8)
Si1C11.847(5) C18C231.421(7)
Si1C141.871(5) C19C201.344(9)
O1Zn111.989(3) C20C211.416(9)
N1C111.505(6) C21C221.377(7)
N1C121.489(7) C22C231.421(7)
N1C131.483(6)    

12-X,-Y,1-Z

 

Table 5 Bond Angles for 3105.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br1Zn1Zn11125.66(3) Si1O1Zn1127.13(17)
O11Zn1Br1110.72(10) Si1O1Zn11132.59(19)
O1Zn1Br1120.72(9) C11N1Zn1111.5(3)
O11Zn1Zn1141.89(10) C12N1Zn1110.9(3)
O1Zn1Zn1142.49(9) C12N1C11109.6(4)
O1Zn1O1184.39(14) C13N1Zn1108.5(3)
O11Zn1N1113.39(14) C13N1C11107.6(4)
O1Zn1N1112.61(15) C13N1C12108.6(4)
N1Zn1Br1112.09(12) Si1C1Fe1127.4(3)
N1Zn1Zn11121.83(12) C2C1Fe168.6(2)
C1Fe1C468.86(18) C2C1Si1127.2(3)
C1Fe1C540.98(17) C5C1Fe170.0(3)
C2Fe1C141.51(19) C5C1Si1126.1(4)
C2Fe1C341.04(18) C5C1C2106.7(4)
C2Fe1C468.34(19) C1C2Fe169.9(3)
C2Fe1C568.87(19) C1C2C11124.8(4)
C2Fe1C6110.5(2) C3C2Fe169.7(3)
C2Fe1C7110.8(2) C3C2C1108.4(4)
C2Fe1C8139.3(3) C3C2C11126.7(4)
C2Fe1C9177.9(2) C11C2Fe1122.6(3)
C2Fe1C10137.8(2) C2C3Fe169.2(3)
C3Fe1C169.48(19) C4C3Fe170.7(3)
C3Fe1C440.2(2) C4C3C2108.2(4)
C3Fe1C568.6(2) C3C4Fe169.1(3)
C3Fe1C7110.7(2) C3C4C5108.7(4)
C3Fe1C8112.1(2) C5C4Fe169.8(3)
C3Fe1C9140.1(3) C1C5Fe169.0(3)
C3Fe1C10177.3(3) C4C5Fe169.5(3)
C4Fe1C540.66(19) C4C5C1108.0(4)
C6Fe1C1111.56(19) C7C6Fe170.4(3)
C6Fe1C3137.7(2) C10C6Fe170.2(3)
C6Fe1C4177.8(2) C10C6C7109.0(5)
C6Fe1C5141.0(2) C6C7Fe169.8(3)
C6Fe1C739.8(2) C6C7C8107.7(6)
C6Fe1C866.9(2) C8C7Fe170.1(3)
C6Fe1C967.5(2) C7C8Fe169.9(3)
C6Fe1C1039.6(3) C9C8Fe170.1(3)
C7Fe1C1139.1(2) C9C8C7108.8(5)
C7Fe1C4138.6(2) C8C9Fe170.2(4)
C7Fe1C5179.2(2) C8C9C10106.9(6)
C7Fe1C840.0(2) C10C9Fe169.3(3)
C7Fe1C967.3(3) C6C10Fe170.1(3)
C8Fe1C1178.3(2) C6C10C9107.6(6)
C8Fe1C4112.7(2) C9C10Fe169.7(4)
C8Fe1C5139.9(2) C2C11N1113.8(4)
C9Fe1C1139.4(3) C15C14Si1117.9(4)
C9Fe1C4113.6(2) C15C14C23118.1(5)
C9Fe1C5113.0(2) C23C14Si1123.7(4)
C9Fe1C839.7(3) C14C15C16122.5(5)
C10Fe1C1111.1(2) C17C16C15119.4(5)
C10Fe1C4142.4(3) C16C17C18121.1(5)
C10Fe1C5113.7(2) C17C18C19121.5(5)
C10Fe1C767.0(3) C17C18C23118.9(5)
C10Fe1C867.3(3) C19C18C23119.5(5)
C10Fe1C941.0(3) C20C19C18121.0(5)
O1Si1O2109.48(19) C19C20C21120.9(5)
O1Si1C1107.6(2) C22C21C20119.3(6)
O1Si1C14109.35(19) C21C22C23121.5(5)
O2Si1C1109.9(2) C18C23C14119.9(5)
O2Si1C14108.7(2) C18C23C22117.7(5)
C1Si1C14111.7(2) C22C23C14122.4(4)
Zn1O1Zn1195.62(14)     

12-X,-Y,1-Z

 

Table 6 Torsion Angles for 3105.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C11C255.1(4) C3C2C11N194.9(5)
Fe1C1C2C359.3(3) C3C4C5Fe1-58.2(3)
Fe1C1C2C11-116.3(5) C3C4C5C10.2(5)
Fe1C1C5C4-58.8(3) C5C1C2Fe1-59.9(3)
Fe1C2C3C460.2(3) C5C1C2C3-0.6(5)
Fe1C2C11N1-177.2(3) C5C1C2C11-176.2(4)
Fe1C3C4C558.7(3) C6C7C8Fe160.0(4)
Fe1C4C5C158.5(3) C6C7C8C90.4(7)
Fe1C6C7C8-60.1(4) C7C6C10Fe1-59.9(4)
Fe1C6C10C959.9(4) C7C6C10C90.0(6)
Fe1C7C8C9-59.5(4) C7C8C9Fe159.4(4)
Fe1C8C9C10-59.8(4) C7C8C9C10-0.4(7)
Fe1C9C10C6-60.2(4) C8C9C10Fe160.5(4)
Si1C1C2Fe1121.4(4) C8C9C10C60.3(6)
Si1C1C2C3-179.2(4) C10C6C7Fe159.8(4)
Si1C1C2C115.1(7) C10C6C7C8-0.3(6)
Si1C1C5Fe1-122.3(4) C11C2C3Fe1116.1(5)
Si1C1C5C4178.9(4) C11C2C3C4176.3(5)
Si1C14C15C16172.6(4) C12N1C11C2-68.2(5)
Si1C14C23C18-169.6(3) C13N1C11C2173.9(4)
Si1C14C23C227.0(6) C14Si1O1Zn1180.4(3)
O1Si1C1Fe1141.9(3) C14Si1O1Zn1-130.0(2)
O1Si1C1C251.7(5) C14Si1C1Fe1-98.0(3)
O1Si1C1C5-126.7(4) C14Si1C1C2171.8(4)
O1Si1C14C15-120.0(4) C14Si1C1C5-6.7(5)
O1Si1C14C2353.0(4) C14C15C16C17-2.6(8)
O2Si1O1Zn1111.0(2) C15C14C23C183.4(7)
O2Si1O1Zn11-38.6(3) C15C14C23C22-180.0(4)
O2Si1C1Fe122.7(4) C15C16C17C183.4(8)
O2Si1C1C2-67.4(5) C16C17C18C19-179.1(5)
O2Si1C1C5114.1(4) C16C17C18C23-0.7(7)
O2Si1C14C15-0.5(4) C17C18C19C20179.5(6)
O2Si1C14C23172.4(4) C17C18C23C14-2.7(7)
C1Si1O1Zn11-158.0(2) C17C18C23C22-179.5(4)
C1Si1O1Zn1-8.4(3) C18C19C20C21-0.4(10)
C1Si1C14C15120.9(4) C19C18C23C14175.7(5)
C1Si1C14C23-66.1(4) C19C18C23C22-1.1(7)
C1C2C3Fe1-59.5(3) C19C20C21C22-0.3(10)
C1C2C3C40.7(5) C20C21C22C230.2(9)
C1C2C11N1-90.2(6) C21C22C23C14-176.2(5)
C2C1C5Fe159.0(3) C21C22C23C180.4(7)
C2C1C5C40.2(5) C23C14C15C16-0.8(7)
C2C3C4Fe1-59.3(3) C23C18C19C201.1(8)
C2C3C4C5-0.6(6)      

12-X,-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3105.
AtomxyzU(eq)
H27180(70)-1190(70)4900(40)90(30)
H38290-517174650
H469991377162651
H565601936290047
H66129-2501337960
H76517-2987210866
H85382-1479122474
H94308-34194784
H104778-694330377
H11A8865-2237283649
H11B8550-1917363149
H12A10411-236262181
H12B10663-1694252181
H12C11562-850305481
H13A11495-2308402480
H13B10542-3148353180
H13C10317-2616431180
H155644777499358
H1647382421550764
H1755034420552863
H1969285909518069
H2084676315461077
H2193274704400665
H2286042681399553

Experimental

Single crystals of C46H48Br2Fe2N2O4Si2Zn2 [3105] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 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 [3105]

Crystal Data for C46H48Br2Fe2N2O4Si2Zn2 (=1151.30 g/mol): monoclinic, space group P21/c (no. 14), a = 11.8205(7) Å, b = 10.6777(4) Å, c = 18.3320(6) Å, β = 99.305(4)°, = 2283.34(17) Å3, Z = 2, T = 173 K, μ(MoKα) = 3.508 mm-1, Dcalc = 1.675 g/cm3, 40953 reflections measured (4.43° ≤ 2Θ ≤ 52°), 4482 unique (Rint = 0.0446, Rsigma = 0.0230) which were used in all calculations. The final R1 was 0.0516 (I > 2σ(I)) and wR2 was 0.1424 (all data).

Refinement model description

Number of restraints - 0, 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.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
2.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), C19(H19), C20(H20), C21(H21), C22(H22)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)

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