3091

Table 1 Crystal data and structure refinement for 3091.
Identification code 3091
Empirical formula C46H52Br2Fe4N2O4Si2Zn2
Formula weight 1267.03
Temperature/K 173
Crystal system orthorhombic
Space group Pbcn
a/Å 15.5968(12)
b/Å 11.1687(9)
c/Å 27.587(2)
α/° 90
β/° 90
γ/° 90
Volume/Å3 4805.5(7)
Z 4
ρcalcg/cm3 1.751
μ/mm‑1 3.915
F(000) 2544.0
Crystal size/mm3 0.3 × 0.2 × 0.1
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.486 to 51.992
Index ranges -12 ≤ h ≤ 19, -13 ≤ k ≤ 12, -27 ≤ l ≤ 34
Reflections collected 17657
Independent reflections 4721 [Rint = 0.0611, Rsigma = 0.0644]
Data/restraints/parameters 4721/1/287
Goodness-of-fit on F2 1.043
Final R indexes [I>=2σ (I)] R1 = 0.0532, wR2 = 0.1000
Final R indexes [all data] R1 = 0.0942, wR2 = 0.1182
Largest diff. peak/hole / e Å-3 1.22/-1.18

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3091. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br11207.5(4)-157.4(7)2711.2(3)52.0(2)
Zn103617.7(8)250021.8(2)
Zn20988.5(8)250025.5(2)
Fe1-1084.7(6)4898.9(7)876.0(3)30.7(2)
Fe21026.5(6)252.7(8)850.9(4)38.5(3)
Si1-126.8(9)2474.0(13)1455.7(6)23.8(4)
O1100(2)2306(3)2023.4(13)24.7(9)
O2-1030(2)1786(4)1323.7(15)32.6(10)
N1-1146(3)4505(5)2485.8(18)34.4(12)
C1-267(3)4105(5)1359(2)23.9(13)
C2-876(3)4876(5)1602(2)26.6(13)
C3-766(4)6058(5)1418(2)38.1(16)
C4-106(4)6034(5)1069(2)36.5(16)
C5198(4)4848(5)1029(2)30.5(14)
C6-1652(4)3565(6)486(2)39.9(16)
C7-2265(4)4166(7)759(3)50.5(19)
C8-2268(5)5374(7)615(3)61(2)
C9-1638(6)5487(7)250(3)61(2)
C10-1258(4)4383(7)170(2)46.1(18)
C11-1504(3)4488(6)1976(2)31.4(15)
C12-1097(5)5777(6)2648(2)53(2)
C13-1746(4)3841(7)2814(2)49(2)
C14778(4)1956(5)1082(2)30.4(14)
C15834(5)1906(5)566(2)42.5(17)
C161652(5)1474(6)432(3)60(2)
C172124(5)1246(6)859(4)66(3)
C181596(4)1542(5)1261(3)40.6(17)
C1971(6)-863(6)629(3)58(2)
C20138(6)-878(6)1125(3)61(2)
C21959(9)-1264(8)1258(4)98(4)
C221393(6)-1464(7)803(6)97(5)
C23835(8)-1215(7)440(4)87(4)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3091. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br141.1(4)65.9(5)49.0(5)-5.9(4)-2.6(3)28.8(4)
Zn120.2(4)24.6(5)20.6(5)00.2(4)0
Zn224.4(5)25.8(5)26.3(6)0-1.5(4)0
Fe145.3(5)24.9(5)21.7(5)4.9(4)-2.9(4)1.7(4)
Fe246.1(6)22.4(5)47.0(6)-12.5(4)14.6(5)-5.8(4)
Si127.0(8)21.8(8)22.5(9)-1.3(6)0.0(7)-5.4(7)
O128(2)23(2)23(2)-2.4(17)-2.6(17)0.0(17)
O229(2)33(2)35(3)7(2)-5.8(19)-11.6(19)
N131(3)46(3)26(3)2(2)6(2)17(2)
C126(3)26(3)20(3)-1(2)-1(2)-5(2)
C234(3)25(3)21(3)0(3)-1(2)1(3)
C356(4)28(3)30(4)-4(3)-2(3)10(3)
C456(4)21(3)32(4)2(3)3(3)-9(3)
C534(3)28(3)30(3)-4(3)3(3)-12(3)
C650(4)40(4)29(4)-4(3)-19(3)2(3)
C742(4)73(5)37(4)8(4)-17(3)-2(4)
C869(5)63(5)51(5)-6(4)-25(4)33(4)
C999(6)47(5)37(5)21(4)-28(5)-9(4)
C1056(4)55(5)27(4)9(3)-3(3)2(4)
C1123(3)48(4)23(4)8(3)1(3)9(3)
C1269(5)54(5)34(4)-14(3)-12(4)32(4)
C1322(3)89(6)35(4)31(4)10(3)11(3)
C1442(4)20(3)29(4)-7(3)7(3)-10(3)
C1566(5)24(3)38(4)-7(3)19(4)-7(3)
C1680(6)31(4)70(6)-19(4)49(5)-17(4)
C1750(5)38(4)110(8)-35(5)35(5)-17(4)
C1835(4)27(3)60(5)-16(3)7(3)-7(3)
C1976(6)25(4)72(6)4(4)-24(5)-21(4)
C2091(6)29(4)63(6)-16(4)39(5)-20(4)
C21168(12)38(5)90(8)20(5)-79(8)-46(6)
C2253(6)18(4)220(16)-20(7)-2(8)6(4)
C23134(9)36(5)91(8)-38(5)67(7)-35(6)

 

Table 4 Bond Lengths for 3091.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn22.3504(8) Si1O11.617(4)
Zn1Zn22.9365(13) Si1O21.646(4)
Zn1O111.975(4) Si1C11.854(6)
Zn1O11.975(4) Si1C141.841(6)
Zn1N12.044(4) N1C111.514(7)
Zn1N112.044(4) N1C121.492(8)
Zn2Br112.3504(8) N1C131.499(7)
Zn2O111.979(4) C1C21.446(7)
Zn2O11.979(4) C1C51.428(8)
Fe1C12.045(5) C2C31.424(8)
Fe1C22.028(6) C2C111.488(8)
Fe1C32.039(6) C3C41.409(8)
Fe1C42.054(6) C4C51.412(8)
Fe1C52.045(6) C6C71.392(9)
Fe1C62.040(6) C6C101.403(9)
Fe1C72.041(7) C7C81.407(10)
Fe1C82.051(7) C8C91.412(10)
Fe1C92.040(7) C9C101.386(10)
Fe1C102.048(7) C14C151.426(8)
Fe2C142.044(5) C14C181.443(8)
Fe2C152.029(6) C15C161.414(9)
Fe2C162.038(7) C16C171.414(11)
Fe2C172.040(7) C17C181.421(9)
Fe2C182.035(6) C19C201.374(11)
Fe2C192.037(7) C19C231.358(11)
Fe2C202.021(7) C20C211.399(13)
Fe2C212.035(8) C21C221.443(14)
Fe2C222.006(8) C22C231.355(14)
Fe2C232.015(8)    

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

 

Table 5 Bond Angles for 3091.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O11Zn1Zn242.10(10) C22Fe2C1966.6(3)
O1Zn1Zn242.10(10) C22Fe2C2067.8(4)
O1Zn1O1184.2(2) C22Fe2C2141.8(4)
O1Zn1N1114.58(18) C22Fe2C2339.4(4)
O1Zn1N11107.67(17) C23Fe2C14154.8(5)
O11Zn1N1107.67(17) C23Fe2C15120.1(4)
O11Zn1N11114.58(18) C23Fe2C16107.2(3)
N11Zn1Zn2119.00(15) C23Fe2C17125.0(4)
N1Zn1Zn2119.00(15) C23Fe2C18162.3(4)
N1Zn1N11122.0(3) C23Fe2C1939.2(3)
Br11Zn2Br1114.02(5) C23Fe2C2066.5(3)
Br1Zn2Zn1122.99(3) C23Fe2C2168.0(4)
Br11Zn2Zn1122.99(3) O1Si1O2110.3(2)
O1Zn2Br11107.65(10) O1Si1C1106.3(2)
O11Zn2Br1107.65(10) O1Si1C14109.8(2)
O11Zn2Br11120.42(10) O2Si1C1109.0(2)
O1Zn2Br1120.42(10) O2Si1C14112.7(2)
O11Zn2Zn141.99(10) C14Si1C1108.6(3)
O1Zn2Zn141.99(10) Zn1O1Zn295.92(16)
O1Zn2O1184.0(2) Si1O1Zn1122.8(2)
C1Fe1C468.7(2) Si1O1Zn2135.5(2)
C1Fe1C8154.4(3) C11N1Zn1109.5(3)
C1Fe1C10125.4(3) C12N1Zn1114.3(4)
C2Fe1C141.6(2) C12N1C11108.1(5)
C2Fe1C341.0(2) C12N1C13108.7(5)
C2Fe1C468.5(2) C13N1Zn1107.2(4)
C2Fe1C568.8(2) C13N1C11108.9(5)
C2Fe1C6125.6(2) Si1C1Fe1126.4(3)
C2Fe1C7107.2(3) C2C1Fe168.6(3)
C2Fe1C8119.7(3) C2C1Si1126.6(4)
C2Fe1C9155.2(3) C5C1Fe169.5(3)
C2Fe1C10162.9(3) C5C1Si1127.0(4)
C3Fe1C169.3(2) C5C1C2106.4(5)
C3Fe1C440.3(2) C1C2Fe169.8(3)
C3Fe1C568.2(2) C1C2C11125.5(5)
C3Fe1C6163.0(3) C3C2Fe169.9(3)
C3Fe1C7126.2(3) C3C2C1107.9(5)
C3Fe1C8108.2(3) C3C2C11126.6(5)
C3Fe1C9121.3(3) C11C2Fe1125.6(4)
C3Fe1C10155.2(3) C2C3Fe169.1(3)
C5Fe1C140.9(2) C4C3Fe170.5(4)
C5Fe1C440.3(2) C4C3C2108.3(5)
C5Fe1C8163.7(3) C3C4Fe169.3(4)
C5Fe1C10108.5(3) C3C4C5108.4(5)
C6Fe1C1107.3(2) C5C4Fe169.5(3)
C6Fe1C4155.4(3) C1C5Fe169.6(3)
C6Fe1C5120.8(3) C4C5Fe170.2(4)
C6Fe1C739.9(3) C4C5C1109.0(5)
C6Fe1C867.3(3) C7C6Fe170.1(4)
C6Fe1C1040.1(3) C7C6C10108.9(6)
C7Fe1C1119.4(3) C10C6Fe170.3(4)
C7Fe1C4163.5(3) C6C7Fe170.0(4)
C7Fe1C5154.7(3) C6C7C8108.1(7)
C7Fe1C840.2(3) C8C7Fe170.3(4)
C7Fe1C1067.6(3) C7C8Fe169.5(4)
C8Fe1C4126.8(3) C7C8C9106.6(7)
C9Fe1C1162.7(3) C9C8Fe169.4(4)
C9Fe1C4109.6(3) C8C9Fe170.2(4)
C9Fe1C5126.7(3) C10C9Fe170.5(4)
C9Fe1C666.7(3) C10C9C8109.4(6)
C9Fe1C767.3(3) C6C10Fe169.6(4)
C9Fe1C840.4(3) C9C10Fe169.8(4)
C9Fe1C1039.6(3) C9C10C6107.0(6)
C10Fe1C4121.2(3) C2C11N1113.4(5)
C10Fe1C867.7(3) Si1C14Fe2127.7(3)
C15Fe2C1441.0(2) C15C14Fe268.9(3)
C15Fe2C1640.7(3) C15C14Si1128.1(5)
C15Fe2C1768.5(3) C15C14C18106.0(6)
C15Fe2C1868.6(3) C18C14Fe269.0(3)
C15Fe2C19109.4(3) C18C14Si1125.9(5)
C15Fe2C21164.4(5) C14C15Fe270.1(4)
C16Fe2C1469.2(2) C16C15Fe270.0(4)
C16Fe2C1740.6(3) C16C15C14109.3(7)
C17Fe2C1469.5(3) C15C16Fe269.3(4)
C18Fe2C1441.4(2) C17C16Fe269.8(4)
C18Fe2C1668.5(3) C17C16C15108.2(7)
C18Fe2C1740.8(3) C16C17Fe269.6(4)
C18Fe2C19156.8(3) C16C17C18107.9(7)
C19Fe2C14121.7(3) C18C17Fe269.4(4)
C19Fe2C16126.1(4) C14C18Fe269.6(3)
C19Fe2C17161.8(4) C17C18Fe269.8(4)
C20Fe2C14109.6(3) C17C18C14108.7(7)
C20Fe2C15127.7(3) C20C19Fe269.6(4)
C20Fe2C16163.5(4) C23C19Fe269.5(5)
C20Fe2C17155.6(4) C23C19C20108.1(8)
C20Fe2C18122.2(3) C19C20Fe270.8(4)
C20Fe2C1939.6(3) C19C20C21109.5(8)
C20Fe2C2140.4(4) C21C20Fe270.4(5)
C21Fe2C14126.4(4) C20C21Fe269.3(5)
C21Fe2C16153.6(5) C20C21C22104.4(8)
C21Fe2C17119.4(4) C22C21Fe268.0(5)
C21Fe2C18107.8(3) C21C22Fe270.2(5)
C21Fe2C1967.6(3) C23C22Fe270.7(5)
C22Fe2C14164.7(5) C23C22C21108.0(9)
C22Fe2C15152.5(5) C19C23Fe271.3(4)
C22Fe2C16117.8(4) C22C23Fe269.9(5)
C22Fe2C17106.4(3) C22C23C19109.9(9)
C22Fe2C18126.1(4)     

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

 

Table 6 Torsion Angles for 3091.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C11C2-50.1(6) C1C2C3C4-0.1(7)
Fe1C1C2C3-59.8(4) C1C2C11N187.4(7)
Fe1C1C2C11120.0(6) C2C1C5Fe1-58.9(4)
Fe1C1C5C459.3(4) C2C1C5C40.4(6)
Fe1C2C3C4-59.8(4) C2C3C4Fe158.9(4)
Fe1C2C11N1176.8(4) C2C3C4C50.3(7)
Fe1C3C4C5-58.6(4) C3C2C11N1-92.9(7)
Fe1C4C5C1-59.0(4) C3C4C5Fe158.5(4)
Fe1C6C7C860.2(5) C3C4C5C1-0.5(7)
Fe1C6C10C9-60.1(5) C5C1C2Fe159.5(4)
Fe1C7C8C959.7(5) C5C1C2C3-0.2(6)
Fe1C8C9C1059.9(5) C5C1C2C11179.5(5)
Fe1C9C10C659.9(5) C6C7C8Fe1-60.1(4)
Fe2C14C15C16-59.2(4) C6C7C8C9-0.3(8)
Fe2C14C18C1759.0(4) C7C6C10Fe159.7(4)
Fe2C15C16C17-59.2(5) C7C6C10C9-0.4(8)
Fe2C16C17C18-59.1(5) C7C8C9Fe1-59.8(5)
Fe2C17C18C14-58.9(4) C7C8C9C100.1(8)
Fe2C19C20C21-60.0(5) C8C9C10Fe1-59.7(5)
Fe2C19C23C2259.5(6) C8C9C10C60.2(8)
Fe2C20C21C22-59.2(5) C10C6C7Fe1-59.8(4)
Fe2C21C22C23-60.9(6) C10C6C7C80.5(7)
Fe2C22C23C19-60.3(6) C11C2C3Fe1-120.0(6)
Si1C1C2Fe1-120.2(4) C11C2C3C4-179.8(6)
Si1C1C2C3-179.9(4) C12N1C11C275.0(6)
Si1C1C2C11-0.2(8) C13N1C11C2-167.0(5)
Si1C1C5Fe1120.8(4) C14Si1O1Zn1127.6(3)
Si1C1C5C4-179.9(4) C14Si1O1Zn2-86.3(3)
Si1C14C15Fe2-122.1(5) C14Si1C1Fe194.6(4)
Si1C14C15C16178.7(4) C14Si1C1C2-176.5(5)
Si1C14C18Fe2122.1(4) C14Si1C1C53.9(6)
Si1C14C18C17-178.9(4) C14C15C16Fe259.2(4)
O1Si1C1Fe1-147.4(3) C14C15C16C170.0(7)
O1Si1C1C2-58.5(5) C15C14C18Fe2-59.3(4)
O1Si1C1C5121.9(5) C15C14C18C17-0.3(7)
O1Si1C14Fe285.8(4) C15C16C17Fe258.9(5)
O1Si1C14C15177.5(5) C15C16C17C18-0.2(8)
O1Si1C14C18-4.2(5) C16C17C18Fe259.2(5)
O2Si1O1Zn1-107.6(3) C16C17C18C140.3(7)
O2Si1O1Zn238.5(4) C18C14C15Fe259.3(4)
O2Si1C1Fe1-28.6(4) C18C14C15C160.2(7)
O2Si1C1C260.4(5) C19C20C21Fe260.2(5)
O2Si1C1C5-119.3(5) C19C20C21C221.0(9)
O2Si1C14Fe2-37.6(5) C20C19C23Fe2-59.1(5)
O2Si1C14C1554.1(6) C20C19C23C220.4(9)
O2Si1C14C18-127.6(5) C20C21C22Fe260.1(5)
C1Si1O1Zn110.4(3) C20C21C22C23-0.8(9)
C1Si1O1Zn2156.5(3) C21C22C23Fe260.6(6)
C1Si1C14Fe2-158.4(4) C21C22C23C190.2(10)
C1Si1C14C15-66.7(6) C23C19C20Fe259.0(5)
C1Si1C14C18111.5(5) C23C19C20C21-0.9(9)
C1C2C3Fe159.7(4)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3091.
AtomxyzU(eq)
H2-1370(40)1310(60)1550(20)100(30)
H3-10836744151446
H499670489144
H5640458581737
H6-1521273750948
H7-26213821100261
H8-2624599373873
H9-149762078573
H10-8144212-5555
H11A-16993665189938
H11B-20115020196238
H12A-8515811297579
H12B-16746124265379
H12C-7346232242479
H13A-17913007270773
H13B-23144217280373
H13C-15273867314773
H15391212834851
H161850135810973
H17269494787579
H1817541479159249
H19-424-64544869
H20-304-659134573
H211180-13711576118
H221969-1725765116
H23960-1277104104

Experimental

Single crystals of C46H52Br2Fe4N2O4Si2Zn2 [3091] 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 [3091]

Crystal Data for C46H52Br2Fe4N2O4Si2Zn2 (=1267.03 g/mol): orthorhombic, space group Pbcn (no. 60), a = 15.5968(12) Å, b = 11.1687(9) Å, c = 27.587(2) Å, = 4805.5(7) Å3, Z = 4, T = 173 K, μ(MoKα) = 3.915 mm-1, Dcalc = 1.751 g/cm3, 17657 reflections measured (4.486° ≤ 2Θ ≤ 51.992°), 4721 unique (Rint = 0.0611, Rsigma = 0.0644) which were used in all calculations. The final R1 was 0.0532 (I > 2σ(I)) and wR2 was 0.1182 (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.