3120_twin1_hklf4

Table 1 Crystal data and structure refinement for 3120_twin1_hklf4.
Identification code 3120_twin1_hklf4
Empirical formula C48H56Br2Fe4N2O4Si2Zn2
Formula weight 1295.08
Temperature/K 173.15
Crystal system monoclinic
Space group P21/c
a/Å 8.1910(6)
b/Å 30.593(2)
c/Å 9.8539(7)
α/° 90
β/° 103.762(7)
γ/° 90
Volume/Å3 2398.3(3)
Z 2
ρcalcg/cm3 1.793
μ/mm‑1 3.924
F(000) 1304.0
Crystal size/mm3 0.3 × 0.1 × 0.05
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.46 to 52
Index ranges -10 ≤ h ≤ 10, -37 ≤ k ≤ 37, -12 ≤ l ≤ 12
Reflections collected 9157
Independent reflections 9157 [Rint = ?, Rsigma = 0.0956]
Data/restraints/parameters 9157/0/293
Goodness-of-fit on F2 1.122
Final R indexes [I>=2σ (I)] R1 = 0.0818, wR2 = 0.2449
Final R indexes [all data] R1 = 0.1253, wR2 = 0.2662
Largest diff. peak/hole / e Å-3 1.65/-1.06

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3120_twin1_hklf4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br112249.0(16)5520.8(4)2927.2(16)65.0(4)
Zn110021.4(15)5218.7(4)3708.2(13)39.5(4)
Fe17261.2(19)6703.3(5)3765.5(17)43.1(4)
Fe211730.5(19)6609.1(5)8618.4(16)41.5(4)
Si19475(4)5878.4(9)6135(3)40.9(7)
O19688(11)5391(2)5571(8)50.6(18)
O27997(10)5895(2)6996(9)50.8(19)
N17677(10)5325(2)2399(9)35.8(17)
C19031(11)6228(3)4535(11)37(2)
C28039(12)6112(3)3179(9)35(2)
C38157(14)6428(3)2173(14)51(3)
C49278(14)6771(4)2896(13)50(3)
C59830(12)6636(3)4313(13)45(3)
C65833(14)6836(3)5194(13)49(3)
C74787(15)6646(3)3961(16)57(3)
C84898(14)6918(4)2855(14)69(4)
C95961(15)7272(4)3317(14)61(4)
C106532(15)7224(4)4770(13)58(3)
C1411305(12)6043(3)7453(10)33(2)
C1511596(16)5965(3)8949(12)48(3)
C1613274(14)6109(4)9674(12)49(3)
C1713973(16)6302(4)8659(14)61(3)
C1812843(12)6264(3)7357(13)44(2)
C239819(17)7027(5)7773(13)69(4)
C199716(16)6896(4)9066(13)54(3)
C2011115(17)7024(3)10064(13)55(3)
C2112186(14)7244(3)9287(15)55(3)
C2211390(20)7215(4)7888(14)69(4)
C246391(16)5711(4)6590(14)57(3)
C116850(13)5713(3)2897(12)43(2)
C127843(19)5401(5)958(13)70(4)
C136585(14)4949(4)2404(14)56(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3120_twin1_hklf4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br150.8(8)65.8(8)83.3(11)7.1(7)25.9(7)-5.3(6)
Zn141.6(7)38.3(6)39.5(7)0.9(5)11.2(5)0.7(5)
Fe144.7(8)39.7(8)42.6(9)-0.7(6)5.9(7)1.5(6)
Fe246.4(9)41.5(8)35.6(8)-1.7(6)7.7(6)4.5(6)
Si145.5(16)39.8(14)39.8(16)-5.5(12)14.7(12)-1.3(12)
O166(5)43(4)43(5)-3(3)13(4)-2(3)
O255(5)47(4)52(5)4(3)16(4)2(3)
N134(4)39(4)35(5)0(3)10(3)-8(3)
C131(5)32(4)50(6)7(4)11(4)12(4)
C240(5)49(5)19(4)-10(4)14(4)2(4)
C348(6)46(6)60(8)6(5)16(5)-18(5)
C448(6)44(6)63(8)9(5)19(5)-1(5)
C531(5)31(4)69(8)0(5)7(5)-14(4)
C653(7)34(5)63(8)28(5)22(6)-1(5)
C743(6)36(5)101(11)1(6)38(7)17(5)
C834(6)76(8)68(9)-12(7)-44(6)12(5)
C946(6)46(6)70(9)13(6)-26(6)20(5)
C1055(7)69(7)42(7)-16(6)-1(6)13(6)
C1441(5)27(4)33(5)3(4)16(4)17(4)
C1581(8)41(5)34(6)-10(4)34(6)-1(5)
C1644(6)58(6)37(6)-6(5)-5(5)-4(5)
C1749(7)74(8)51(7)-8(6)-8(6)-4(6)
C1832(5)35(5)59(7)9(5)1(5)-8(4)
C2356(8)99(10)39(7)0(7)-11(6)22(7)
C1957(7)52(6)55(8)-20(6)17(6)-6(5)
C2085(9)41(6)40(6)-8(5)19(6)14(6)
C2145(6)20(4)90(10)-19(5)-6(6)5(4)
C22113(13)48(7)42(7)-19(6)10(7)23(7)
C2467(8)59(7)49(7)-8(6)25(6)0(6)
C1136(5)45(6)49(7)-14(5)9(4)-4(4)
C1287(10)75(8)32(6)-10(6)-15(6)22(7)
C1332(5)50(6)72(9)2(6)-14(5)19(5)

 

Table 4 Bond Lengths for 3120_twin1_hklf4.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.3332(16) Si1C141.806(11)
Zn1Zn112.884(2) O1Zn111.988(7)
Zn1O111.988(7) O2C241.399(15)
Zn1O11.990(8) N1C111.507(12)
Zn1N12.069(8) N1C121.477(15)
Fe1C12.066(9) N1C131.458(14)
Fe1C22.046(9) C1C21.433(13)
Fe1C32.064(12) C1C51.451(13)
Fe1C42.044(11) C2C31.404(15)
Fe1C52.054(10) C2C111.545(14)
Fe1C62.073(11) C3C41.463(16)
Fe1C72.088(11) C4C51.423(17)
Fe1C82.039(10) C6C71.433(19)
Fe1C92.032(10) C6C101.422(16)
Fe1C102.037(11) C7C81.390(18)
Fe2C142.062(9) C8C91.397(17)
Fe2C152.006(10) C9C101.404(17)
Fe2C162.097(12) C14C151.456(14)
Fe2C172.054(13) C14C181.453(13)
Fe2C182.007(12) C15C161.458(16)
Fe2C232.039(13) C16C171.397(18)
Fe2C192.009(12) C17C181.397(16)
Fe2C202.058(10) C23C191.357(18)
Fe2C212.056(9) C23C221.39(2)
Fe2C221.983(13) C19C201.377(18)
Si1O11.616(8) C20C211.458(17)
Si1O21.637(8) C21C221.381(18)
Si1C11.868(11)    

12-X,1-Y,1-Z

 

Table 5 Bond Angles for 3120_twin1_hklf4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br1Zn1Zn11130.52(8) C22Fe2C16151.5(6)
O11Zn1Br1116.9(2) C22Fe2C17118.9(6)
O1Zn1Br1119.3(2) C22Fe2C18108.2(5)
O11Zn1Zn1143.6(2) C22Fe2C2340.3(6)
O1Zn1Zn1143.5(2) C22Fe2C1967.6(6)
O11Zn1O187.1(3) C22Fe2C2068.8(5)
O11Zn1N1112.6(3) C22Fe2C2139.9(5)
O1Zn1N1102.9(3) O1Si1O2111.1(4)
N1Zn1Br1114.5(2) O1Si1C1104.7(4)
N1Zn1Zn11114.8(2) O1Si1C14111.4(4)
C1Fe1C6110.4(4) O2Si1C1113.6(4)
C1Fe1C7121.3(4) O2Si1C14102.0(4)
C2Fe1C140.8(4) C14Si1C1114.2(4)
C2Fe1C339.9(4) Zn11O1Zn192.9(3)
C2Fe1C567.5(4) Si1O1Zn1127.6(4)
C2Fe1C6129.0(4) Si1O1Zn11139.1(5)
C2Fe1C7109.0(4) C24O2Si1126.9(8)
C3Fe1C169.3(5) C11N1Zn1110.1(6)
C3Fe1C6163.0(4) C12N1Zn1109.9(7)
C3Fe1C7124.4(5) C12N1C11109.8(9)
C4Fe1C170.1(4) C13N1Zn1110.7(6)
C4Fe1C268.6(4) C13N1C11107.3(8)
C4Fe1C341.7(4) C13N1C12109.0(10)
C4Fe1C540.6(5) Si1C1Fe1133.8(5)
C4Fe1C6155.1(5) C2C1Fe168.8(5)
C4Fe1C7161.0(6) C2C1Si1126.8(7)
C5Fe1C141.2(4) C2C1C5104.4(9)
C5Fe1C368.4(5) C5C1Fe169.0(5)
C5Fe1C6123.3(5) C5C1Si1128.0(8)
C5Fe1C7157.4(5) C1C2Fe170.4(5)
C6Fe1C740.3(5) C1C2C11123.8(9)
C8Fe1C1153.9(5) C3C2Fe170.7(6)
C8Fe1C2119.1(5) C3C2C1111.7(9)
C8Fe1C3105.6(6) C3C2C11124.3(9)
C8Fe1C4124.1(6) C11C2Fe1121.6(6)
C8Fe1C5162.5(5) C2C3Fe169.3(6)
C8Fe1C666.8(5) C2C3C4106.9(11)
C8Fe1C739.3(5) C4C3Fe168.4(7)
C9Fe1C1165.4(5) C3C4Fe169.9(6)
C9Fe1C2151.3(5) C5C4Fe170.1(6)
C9Fe1C3116.5(5) C5C4C3106.6(9)
C9Fe1C4104.8(5) C1C5Fe169.8(5)
C9Fe1C5126.4(4) C4C5Fe169.3(6)
C9Fe1C668.2(5) C4C5C1110.4(9)
C9Fe1C767.8(5) C7C6Fe170.4(6)
C9Fe1C840.1(5) C10C6Fe168.4(6)
C9Fe1C1040.4(5) C10C6C7106.9(10)
C10Fe1C1129.3(5) C6C7Fe169.3(6)
C10Fe1C2167.1(5) C8C7Fe168.4(6)
C10Fe1C3152.4(5) C8C7C6106.6(10)
C10Fe1C4118.9(5) C7C8Fe172.3(6)
C10Fe1C5110.5(5) C7C8C9111.1(11)
C10Fe1C640.5(5) C9C8Fe169.7(6)
C10Fe1C767.5(5) C8C9Fe170.2(6)
C10Fe1C866.8(5) C8C9C10106.4(11)
C14Fe2C1670.4(4) C10C9Fe170.0(6)
C15Fe2C1441.9(4) C6C10Fe171.1(7)
C15Fe2C1641.6(5) C9C10Fe169.6(7)
C15Fe2C1768.4(5) C9C10C6109.1(11)
C15Fe2C1868.5(4) Si1C14Fe2129.5(4)
C15Fe2C23128.0(6) C15C14Fe267.0(5)
C15Fe2C19108.3(5) C15C14Si1126.2(8)
C15Fe2C20117.5(4) C18C14Fe267.1(6)
C15Fe2C21152.8(5) C18C14Si1131.9(8)
C17Fe2C1470.1(4) C18C14C15101.9(9)
C17Fe2C1639.3(5) C14C15Fe271.1(5)
C17Fe2C20129.3(5) C14C15C16110.8(9)
C17Fe2C21109.4(5) C16C15Fe272.6(6)
C18Fe2C1441.8(4) C15C16Fe265.9(6)
C18Fe2C1667.3(4) C17C16Fe268.7(7)
C18Fe2C1740.2(5) C17C16C15106.1(10)
C18Fe2C23119.6(5) C16C17Fe272.0(7)
C18Fe2C19152.1(5) C16C17C18109.1(11)
C18Fe2C20167.2(5) C18C17Fe268.1(7)
C18Fe2C21128.4(5) C14C18Fe271.1(6)
C23Fe2C14106.7(5) C17C18Fe271.7(8)
C23Fe2C16166.9(6) C17C18C14112.0(11)
C23Fe2C17152.9(6) C19C23Fe269.2(7)
C23Fe2C2066.8(5) C19C23C22108.0(12)
C23Fe2C2166.5(5) C22C23Fe267.7(7)
C19Fe2C14116.8(4) C23C19Fe271.6(7)
C19Fe2C16129.8(5) C23C19C20111.1(12)
C19Fe2C17166.6(5) C20C19Fe272.1(7)
C19Fe2C2339.2(5) C19C20Fe268.3(7)
C19Fe2C2039.6(5) C19C20C21105.0(11)
C19Fe2C2167.2(5) C21C20Fe269.2(6)
C20Fe2C14150.1(4) C20C21Fe269.3(5)
C20Fe2C16109.0(5) C22C21Fe267.2(6)
C21Fe2C14165.0(5) C22C21C20107.0(12)
C21Fe2C16119.2(5) C23C22Fe272.0(8)
C21Fe2C2041.5(5) C21C22Fe272.9(7)
C22Fe2C14126.3(4) C21C22C23108.6(13)
C22Fe2C15165.6(6) N1C11C2111.6(8)

12-X,1-Y,1-Z

 

Table 6 Torsion Angles for 3120_twin1_hklf4.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C11C249.5(10) C1C2C3Fe1-58.5(6)
Fe1C1C2C358.7(7) C1C2C3C4-0.2(12)
Fe1C1C2C11-115.5(9) C1C2C11N1-97.0(11)
Fe1C1C5C4-57.4(8) C2C1C5Fe160.2(6)
Fe1C2C3C458.3(8) C2C1C5C42.7(11)
Fe1C2C11N1176.6(6) C2C3C4Fe1-58.9(7)
Fe1C3C4C560.8(7) C2C3C4C51.9(12)
Fe1C4C5C157.7(7) C3C2C11N189.5(12)
Fe1C6C7C8-58.5(7) C3C4C5Fe1-60.6(7)
Fe1C6C10C959.5(8) C3C4C5C1-2.9(12)
Fe1C7C8C9-59.1(9) C5C1C2Fe1-60.2(6)
Fe1C8C9C10-61.0(8) C5C1C2C3-1.5(10)
Fe1C9C10C6-60.4(8) C5C1C2C11-175.7(9)
Fe2C14C15C16-62.1(7) C6C7C8Fe159.0(7)
Fe2C14C18C1760.3(9) C6C7C8C9-0.1(13)
Fe2C15C16C17-57.1(8) C7C6C10Fe1-60.2(7)
Fe2C16C17C18-58.1(9) C7C6C10C9-0.7(13)
Fe2C17C18C14-59.9(7) C7C8C9Fe160.6(8)
Fe2C23C19C2061.7(9) C7C8C9C10-0.4(14)
Fe2C23C22C21-64.2(8) C8C9C10Fe161.1(8)
Fe2C19C20C2159.8(7) C8C9C10C60.7(14)
Fe2C20C21C2256.7(7) C10C6C7Fe158.9(7)
Fe2C21C22C2363.7(9) C10C6C7C80.5(12)
Si1C1C2Fe1129.5(7) C14Si1O1Zn1162.6(9)
Si1C1C2C3-171.7(8) C14Si1O1Zn1-109.1(6)
Si1C1C2C1114.1(13) C14Si1O2C24-165.1(9)
Si1C1C5Fe1-129.8(8) C14Si1C1Fe1-105.4(7)
Si1C1C5C4172.8(7) C14Si1C1C2159.4(7)
Si1C14C15Fe2-123.1(6) C14Si1C1C5-8.6(10)
Si1C14C15C16174.9(7) C14C15C16Fe261.2(7)
Si1C14C18Fe2123.3(7) C14C15C16C174.1(12)
Si1C14C18C17-176.5(8) C15C14C18Fe2-58.5(6)
O1Si1O2C24-46.2(10) C15C14C18C171.8(11)
O1Si1C1Fe1132.5(7) C15C16C17Fe255.3(8)
O1Si1C1C237.2(9) C15C16C17C18-2.8(14)
O1Si1C1C5-130.8(9) C16C17C18Fe260.5(9)
O1Si1C14Fe2-176.7(5) C16C17C18C140.6(14)
O1Si1C14C15-88.1(8) C18C14C15Fe258.5(6)
O1Si1C14C1889.8(9) C18C14C15C16-3.5(10)
O2Si1O1Zn1137.8(6) C23C19C20Fe2-61.4(9)
O2Si1O1Zn11-50.5(9) C23C19C20C21-1.6(13)
O2Si1C1Fe111.1(9) C19C23C22Fe257.5(9)
O2Si1C1C2-84.2(9) C19C23C22C21-6.7(15)
O2Si1C1C5107.8(9) C19C20C21Fe2-59.2(7)
O2Si1C14Fe2-58.0(7) C19C20C21C22-2.5(11)
O2Si1C14C1530.6(8) C20C21C22Fe2-58.0(7)
O2Si1C14C18-151.5(8) C20C21C22C235.6(12)
C1Si1O1Zn11-173.5(7) C22C23C19Fe2-56.6(9)
C1Si1O1Zn114.8(7) C22C23C19C205.1(15)
C1Si1O2C2471.5(10) C11C2C3Fe1115.7(9)
C1Si1C14Fe264.9(7) C11C2C3C4174.0(9)
C1Si1C14C15153.5(7) C12N1C11C2-71.6(11)
C1Si1C14C18-28.6(10) C13N1C11C2170.0(9)

12-X,1-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3120_twin1_hklf4.
AtomxyzU(eq)
H376146420120761
H495787033249761
H5106116792501454
H660236724611858
H741436386390968
H843266869190982
H962417500275973
H1072687419537369
H15108015837939258
H161378760781064059
H17150456438882774
H18130556370650952
H2389676996693682
H1988006737925865
H201133569791104466
H21132347381967166
H22118377307713283
H24A59235675741185
H24B64645425616185
H24C56605903591285
H11A65115635376652
H11B58225791218252
H12A85145665934104
H12B67245440336104
H12C83995150646104
H13A70784690207184
H13B54775007178984
H13C64644897335784

Experimental

Single crystals of C48H56Br2Fe4N2O4Si2Zn2 [3120_twin1_hklf4] 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 [3120_twin1_hklf4]

Crystal Data for C48H56Br2Fe4N2O4Si2Zn2 (=1295.08 g/mol): monoclinic, space group P21/c (no. 14), a = 8.1910(6) Å, b = 30.593(2) Å, c = 9.8539(7) Å, β = 103.762(7)°, = 2398.3(3) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 3.924 mm-1, Dcalc = 1.793 g/cm3, 9157 reflections measured (4.46° ≤ 2Θ ≤ 52°), 9157 unique (Rint = ?, Rsigma = 0.0956) which were used in all calculations. The final R1 was 0.0818 (I > 2σ(I)) and wR2 was 0.2662 (all data).

Refinement model description

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

Details:

1. Twinned data refinement
Scales: 0.8412(14) 0.1588(14)
2. 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
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), C23(H23), C19(H19), C20(H20), C21(H21), C22(H22)
3.c Idealised Me refined as rotating group:
C24(H24A,H24B,H24C), 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.