mo_B0257_0m

Table 1 Crystal data and structure refinement for mo_B0257_0m.
Identification code mo_B0257_0m
Empirical formula C63H71Br3Fe3N3O6Si4Zn1.25
Formula weight 1567.58
Temperature/K 123.01
Crystal system trigonal
Space group P321
a/Å 16.1933(6)
b/Å 16.1933(6)
c/Å 15.5940(7)
α/° 90
β/° 90
γ/° 120
Volume/Å3 3541.3(3)
Z 2
ρcalcg/cm3 1.470
μ/mm‑1 2.827
F(000) 1589.0
Crystal size/mm3 0.822 × 0.758 × 0.566
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 2.904 to 58.166
Index ranges -21 ≤ h ≤ 22, -22 ≤ k ≤ 21, -21 ≤ l ≤ 21
Reflections collected 45279
Independent reflections 6334 [Rint = 0.0586, Rsigma = 0.0352]
Data/restraints/parameters 6334/19/272
Goodness-of-fit on F2 1.064
Final R indexes [I>=2σ (I)] R1 = 0.0622, wR2 = 0.1677
Final R indexes [all data] R1 = 0.0699, wR2 = 0.1746
Largest diff. peak/hole / e Å-3 2.73/-1.77
Flack parameter0.017(5)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0257_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br13333666710442.1(7)29.1(3)
Zn1333366678914.1(7)19.2(3)
Fe12576.8(9)2831.1(8)6845.5(8)32.0(3)
Si13567.9(13)5253.8(13)7598.4(11)20.9(4)
Si2333366676464.0(18)20.8(5)
O13732(4)5992(4)6817(3)26.8(10)
O23192(4)5483(3)8471(3)24.3(10)
N11999(5)3899(4)9231(3)28.1(12)
C12608(5)4057(5)7252(4)23.1(12)
C22005(5)3252(5)7792(5)27.5(13)
C31267(7)2541(5)7276(5)37.2(16)
C41373(7)2869(6)6423(5)41.6(19)
C52216(6)3805(6)6408(5)31.5(15)
C63955(8)3080(9)6818(8)61(3)
C73410(15)2380(15)7390(8)86(5)
C82669(13)1644(11)6995(17)122(9)
C92760(12)1908(12)6095(12)89(5)
C103578(10)2819(12)6035(8)69(4)
C112136(5)3178(5)8728(5)27.5(14)
C122313(8)3944(7)10134(5)47(2)
C131006(6)3714(6)9167(6)42(2)
C144752(5)5344(6)7773(4)25.7(12)
C154895(5)4885(6)8466(5)33.0(16)
C165737(7)4889(7)8601(7)48(2)
C176480(7)5365(9)7994(6)50(2)
C186393(7)5869(9)7323(7)53(3)
C195500(6)5825(7)7207(5)37.9(19)
C203407(19)6758(16)5272(5)29(3)
C213760(20)6250(20)4839(10)43(5)
C223840(20)6304(18)3950(10)200(40)
C233562(15)6863(15)3495(5)39(6)
C243210(20)7369(19)3929(11)200(40)
C253130(20)7316(17)4817(11)43(5)
Br2540.5(17)1552.0(17)10787(3)84.4(11)
Br3008601(5)156(4)
Zn2001000045.6(11)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0257_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br135.2(4)35.2(4)16.7(5)0017.62(19)
Zn120.1(3)20.1(3)17.4(5)0010.07(17)
Fe137.8(6)29.9(5)33.3(6)-8.7(4)-1.1(5)20.7(5)
Si123.7(8)22.1(8)18.7(8)1.9(6)3.1(6)12.9(7)
Si222.5(8)22.5(8)17.4(12)0011.2(4)
O134(3)32(3)21(2)6.1(19)4.8(19)21(2)
O227(2)23(2)23(2)1.7(18)7.5(19)12.1(19)
N142(4)28(3)24(2)9(2)11(3)25(3)
C126(3)23(3)21(3)-3(2)0(2)12(3)
C232(3)24(3)27(3)1(3)-1(3)15(3)
C329(4)22(3)51(4)-7(3)6(4)6(3)
C444(5)48(5)40(4)-17(3)-15(4)29(4)
C536(4)42(4)25(3)-8(3)-4(3)25(3)
C654(6)66(7)87(9)-34(6)-15(6)49(6)
C7149(16)135(14)52(7)7(8)9(8)129(14)
C896(12)50(7)250(30)45(11)87(15)59(9)
C983(8)85(8)115(10)-60(7)-8(7)55(7)
C1078(8)103(10)57(7)2(7)24(6)68(8)
C1131(3)22(3)30(3)5(3)5(3)13(3)
C1276(7)55(5)20(3)10(3)14(4)40(5)
C1342(5)36(4)54(5)17(4)21(4)25(4)
C1422(3)28(3)25(3)-2(3)-2(3)11(3)
C1524(3)32(4)41(4)6(3)-2(3)13(3)
C1646(5)43(5)61(6)2(4)-18(4)27(4)
C1734(4)80(7)49(5)-16(5)-11(4)37(5)
C1834(5)87(8)41(5)-10(5)-4(4)33(5)
C1929(4)64(6)24(4)2(4)3(3)25(4)
C2029(4)29(4)29(4)-0.2(14)-0.1(14)14(2)
C2179(15)44(11)24(6)18(7)25(8)45(10)
C22530(120)180(40)30(8)66(18)90(30)280(60)
C2339(6)39(6)38(6)0.0(14)0.2(14)19(3)
C24530(120)180(40)30(8)66(18)90(30)280(60)
C2579(15)44(11)24(6)18(7)25(8)45(10)
Br244.8(11)45.5(11)175(3)31.1(15)37.4(15)31.8(10)
Br3197(6)197(6)75(4)0098(3)
Zn230.8(13)30.8(13)75(4)0015.4(7)

 

Table 4 Bond Lengths for mo_B0257_0m.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.3828(15) C4C51.446(13)
Zn1O21.941(5) C6C71.36(2)
Zn1O211.941(5) C6C101.337(17)
Zn1O221.941(5) C7C81.35(3)
Fe1C12.060(7) C8C91.45(3)
Fe1C22.033(7) C9C101.41(2)
Fe1C32.042(9) C14C151.396(10)
Fe1C42.087(10) C14C191.381(11)
Fe1C52.053(8) C15C161.377(11)
Fe1C62.061(11) C16C171.418(15)
Fe1C72.015(12) C17C181.378(16)
Fe1C82.015(12) C18C191.422(12)
Fe1C92.033(11) C20C211.3900
Fe1C102.064(10) C20C251.3900
Si1O11.633(5) C21C221.3900
Si1O21.608(5) C22C231.3900
Si1C11.858(7) C23C241.3900
Si1C141.869(7) C24C251.3900
Si2O121.618(5) Br2Br332.407(4)
Si2O111.618(5) Br2Zn22.528(3)
Si2O11.618(5) Br3Br242.407(4)
Si2C201.864(9) Br3Br232.407(4)
N1C111.512(9) Br3Br252.407(4)
N1C121.487(10) Br3Zn22.182(8)
N1C131.484(11) Zn2Br252.528(3)
C1C21.445(10) Zn2Br262.528(3)
C1C51.428(10) Zn2Br232.528(3)
C2C31.424(10) Zn2Br242.528(3)
C2C111.488(10) Zn2Br272.528(3)
C3C41.410(12) Zn2Br332.182(8)

11-Y,1+X-Y,+Z; 2+Y-X,1-X,+Z; 3+Y,+X,2-Z; 4-Y+X,-Y,2-Z; 5-X,-X+Y,2-Z; 6-Y,+X-Y,+Z; 7+Y-X,-X,+Z

 

Table 5 Bond Angles for mo_B0257_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O21Zn1Br1110.85(14) C3C2C11125.8(7)
O22Zn1Br1110.85(14) C11C2Fe1125.3(5)
O2Zn1Br1110.85(14) C2C3Fe169.2(5)
O21Zn1O22108.05(15) C4C3Fe171.7(5)
O22Zn1O2108.05(15) C4C3C2109.5(7)
O21Zn1O2108.05(15) C3C4Fe168.3(5)
C1Fe1C469.0(3) C3C4C5106.4(7)
C1Fe1C6108.4(4) C5C4Fe168.3(5)
C1Fe1C10123.8(5) C1C5Fe170.0(4)
C2Fe1C141.4(3) C1C5C4109.7(7)
C2Fe1C340.9(3) C4C5Fe170.8(5)
C2Fe1C468.3(3) C7C6Fe168.7(8)
C2Fe1C568.4(3) C10C6Fe171.2(7)
C2Fe1C6125.4(4) C10C6C7109.3(13)
C2Fe1C10160.0(5) C6C7Fe172.3(7)
C3Fe1C169.1(3) C8C7Fe170.5(9)
C3Fe1C439.9(4) C8C7C6110.9(14)
C3Fe1C567.9(3) C7C8Fe170.5(7)
C3Fe1C6161.8(5) C7C8C9105.5(13)
C3Fe1C10158.3(5) C9C8Fe169.7(8)
C5Fe1C140.6(3) C8C9Fe168.3(7)
C5Fe1C440.9(3) C10C9Fe171.1(7)
C5Fe1C6122.6(5) C10C9C8106.1(14)
C5Fe1C10109.3(5) C6C10Fe171.0(6)
C6Fe1C4157.5(5) C6C10C9108.2(14)
C6Fe1C1037.8(5) C9C10Fe168.7(7)
C7Fe1C1121.4(6) C2C11N1111.4(6)
C7Fe1C2108.4(4) C15C14Si1120.5(6)
C7Fe1C3125.8(6) C19C14Si1121.9(5)
C7Fe1C4161.4(7) C19C14C15117.5(7)
C7Fe1C5156.6(7) C16C15C14122.9(8)
C7Fe1C639.1(6) C15C16C17118.0(9)
C7Fe1C966.8(7) C18C17C16121.3(8)
C7Fe1C1065.4(5) C17C18C19118.0(9)
C8Fe1C1155.0(8) C14C19C18122.0(9)
C8Fe1C2120.0(7) C21C20Si2117.9(11)
C8Fe1C3107.8(5) C21C20C25120.0
C8Fe1C4125.5(7) C25C20Si2122.1(11)
C8Fe1C5163.1(8) C20C21C22120.0
C8Fe1C666.4(6) C21C22C23120.0
C8Fe1C739.0(8) C24C23C22120.0
C8Fe1C942.0(8) C25C24C23120.0
C8Fe1C1068.2(6) C24C25C20120.0
C9Fe1C1160.6(6) Br33Br2Zn252.41(18)
C9Fe1C2157.3(6) Br23Br3Br24105.3(2)
C9Fe1C3122.4(5) Br23Br3Br25105.3(2)
C9Fe1C4108.8(5) Br24Br3Br25105.3(2)
C9Fe1C5125.2(6) Zn2Br3Br2566.6(2)
C9Fe1C665.8(5) Zn2Br3Br2366.6(2)
C9Fe1C1040.2(6) Zn2Br3Br2466.6(2)
C10Fe1C4123.8(5) Br24Zn2Br2398.41(10)
O1Si1C1107.0(3) Br26Zn2Br2595.83(10)
O1Si1C14105.5(3) Br25Zn2Br269.61(15)
O2Si1O1113.8(3) Br23Zn2Br2598.41(10)
O2Si1C1105.7(3) Br24Zn2Br2795.83(10)
O2Si1C14110.5(3) Br27Zn2Br25162.64(10)
C1Si1C14114.5(3) Br24Zn2Br2669.61(15)
O12Si2O1109.02(19) Br23Zn2Br295.83(10)
O11Si2O1109.02(19) Br27Zn2Br2698.41(10)
O11Si2O12109.02(19) Br24Zn2Br2162.64(10)
O12Si2C20105.8(8) Br27Zn2Br298.41(10)
O1Si2C20111.2(7) Br24Zn2Br2598.41(10)
O11Si2C20112.6(8) Br26Zn2Br23162.64(10)
Si2O1Si1140.8(3) Br26Zn2Br298.41(10)
Si1O2Zn1131.1(3) Br27Zn2Br2369.61(15)
C12N1C11110.5(6) Br3Zn2Br2560.94(8)
C13N1C11111.8(7) Br3Zn2Br27119.06(8)
C13N1C12112.5(7) Br33Zn2Br25119.06(8)
Si1C1Fe1134.4(4) Br3Zn2Br2360.94(8)
C2C1Fe168.3(4) Br33Zn2Br260.94(8)
C2C1Si1127.3(5) Br3Zn2Br26119.06(8)
C5C1Fe169.4(4) Br33Zn2Br2760.94(8)
C5C1Si1125.9(6) Br3Zn2Br2460.94(8)
C5C1C2106.0(6) Br33Zn2Br24119.06(8)
C1C2Fe170.3(4) Br33Zn2Br23119.06(8)
C1C2C11125.8(6) Br3Zn2Br2119.06(8)
C3C2Fe169.9(5) Br33Zn2Br2660.94(8)
C3C2C1108.3(6) Br3Zn2Br33180.0

1+Y-X,1-X,+Z; 21-Y,1+X-Y,+Z; 3+Y,+X,2-Z; 4-Y+X,-Y,2-Z; 5-X,-X+Y,2-Z; 6-Y,+X-Y,+Z; 7+Y-X,-X,+Z

 

Table 6 Hydrogen Bonds for mo_B0257_0m.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1O21.001.612.600(8)170.6

 

Table 7 Torsion Angles for mo_B0257_0m.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.8(6) C1C2C3Fe160.0(5)
Fe1C1C2C11119.9(7) C1C2C3C4-0.6(10)
Fe1C1C5C459.9(6) C1C2C11N165.5(9)
Fe1C2C3C4-60.7(7) C2C1C5Fe1-58.8(5)
Fe1C2C11N1155.6(5) C2C1C5C41.1(9)
Fe1C3C4C5-57.8(6) C2C3C4Fe159.1(6)
Fe1C4C5C1-59.4(5) C2C3C4C51.3(10)
Fe1C6C7C860.2(9) C3C2C11N1-114.8(8)
Fe1C6C10C9-58.9(9) C3C4C5Fe157.9(6)
Fe1C7C8C961.3(9) C3C4C5C1-1.5(10)
Fe1C8C9C1061.4(9) C5C1C2Fe159.5(5)
Fe1C9C10C660.3(8) C5C1C2C3-0.3(8)
Si1C1C2Fe1-130.0(6) C5C1C2C11179.4(7)
Si1C1C2C3170.2(6) C6C7C8Fe1-61.3(9)
Si1C1C2C11-10.1(11) C6C7C8C90.0(14)
Si1C1C5Fe1130.6(6) C7C6C10Fe158.2(8)
Si1C1C5C4-169.5(6) C7C6C10C9-0.7(13)
Si1C14C15C16176.7(7) C7C8C9Fe1-61.8(9)
Si1C14C19C18-177.9(8) C7C8C9C10-0.4(14)
Si2C20C21C22-179.4(17) C8C9C10Fe1-59.6(8)
Si2C20C25C24179.4(18) C8C9C10C60.7(14)
O1Si1O2Zn1-26.0(5) C10C6C7Fe1-59.7(8)
O1Si1C1Fe1106.0(5) C10C6C7C80.4(14)
O1Si1C1C2-158.4(6) C11C2C3Fe1-119.7(7)
O1Si1C1C510.3(7) C11C2C3C4179.7(8)
O1Si1C14C15172.5(6) C12N1C11C2-169.0(7)
O1Si1C14C19-10.5(8) C13N1C11C264.8(8)
O11Si2O1Si1-23.6(6) C14Si1O1Si2-150.5(5)
O12Si2O1Si195.3(4) C14Si1O2Zn192.5(5)
O12Si2C20C21119.2(14) C14Si1C1Fe1-10.4(6)
O11Si2C20C21-121.8(14) C14Si1C1C285.1(7)
O1Si2C20C211.0(16) C14Si1C1C5-106.2(6)
O11Si2C20C2558.9(19) C14C15C16C17-1.3(14)
O12Si2C20C25-60.2(18) C15C14C19C18-0.8(14)
O1Si2C20C25-178.4(15) C15C16C17C184.6(16)
O2Si1O1Si2-29.1(7) C16C17C18C19-5.8(16)
O2Si1C1Fe1-132.3(5) C17C18C19C143.9(16)
O2Si1C1C2-36.8(7) C19C14C15C16-0.5(13)
O2Si1C1C5131.9(6) C20Si2O1Si1-148.4(10)
O2Si1C14C1549.0(7) C20C21C22C230.0
O2Si1C14C19-133.9(7) C21C20C25C240.0
C1Si1O1Si287.2(6) C21C22C23C240.0
C1Si1O2Zn1-143.1(4) C22C23C24C250.0
C1Si1C14C15-70.2(7) C23C24C25C200.0
C1Si1C14C19106.8(7) C25C20C21C220.0

1+Y-X,1-X,+Z; 21-Y,1+X-Y,+Z

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0257_0m.
AtomxyzU(eq)
H124234538896834
H37791938747545
H49702540595250
H524714193591338
H645163662695573
H7353624087988104
H8218710727250146
H9234115135613106
H1038193184552583
H11A27853285883433
H11B16712528892833
H12A192133231040971
H12B224344321044471
H12C298441081014371
H13A8653787857062
H13B9354169952962
H13C5643063936162
H1543894556886340
H1658184581908657
H1770505337805260
H1869136235694864
H1954166135672645
H2139535870515051
H22408359593654243
H2336156899288847
H24301677513618243
H2528867662511351

 

Table 9 Atomic Occupancy for mo_B0257_0m.
AtomOccupancy AtomOccupancy AtomOccupancy
C200.3333 C210.3333 H210.3333
C220.3333 H220.3333 C230.3333
H230.3333 C240.3333 H240.3333
C250.3333 H250.3333 Br20.5
Br30.5 Zn20.5   

 

Table 10 Solvent masks information for mo_B0257_0m.
NumberXYZVolumeElectron countContent
10.0000.0000.500364.0154.7Aceton und/oder Wasser?

Experimental

Single crystals of C63H71Br3Fe3N3O6Si4Zn1.25 [mo_B0257_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 123.01 K during data collection. Using Olex2 [1], the structure was solved with the XT [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. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [mo_B0257_0m]

Crystal Data for C63H71Br3Fe3N3O6Si4Zn1.25 (=1567.58 g/mol): trigonal, space group P321 (no. 150), a = 16.1933(6) Å, c = 15.5940(7) Å, = 3541.3(3) Å3, Z = 2, T = 123.01 K, μ(MoKα) = 2.827 mm-1, Dcalc = 1.470 g/cm3, 45279 reflections measured (2.904° ≤ 2Θ ≤ 58.166°), 6334 unique (Rint = 0.0586, Rsigma = 0.0352) which were used in all calculations. The final R1 was 0.0622 (I > 2σ(I)) and wR2 was 0.1746 (all data).

Refinement model description

Number of restraints - 19, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Rigid bond restraints
C21, C22
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C9) ≈ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C20) ≈ Ueq, Uanis(C20) ≈ Ueq, Uanis(C20) ≈ Ueq, Uanis(C23)
≈ Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C23) = Uanis(C23) = Uanis(C23)
Uanis(C20) = Uanis(C20) = Uanis(C20)
Uanis(C22) = Uanis(C22) = Uanis(C22) = Uanis(C24) = Uanis(C24) = Uanis(C24)
Uanis(C21) = Uanis(C21) = Uanis(C21) = Uanis(C25) = Uanis(C25) = Uanis(C25)
4. Others
Fixed Sof: C20(0.33333) C21(0.33333) H21(0.33333) C22(0.33333) H22(0.33333)
C23(0.33333) H23(0.33333) C24(0.33333) H24(0.33333) C25(0.33333) H25(0.33333)
Br2(0.5) Br3(0.16667) Zn2(0.08333)
5.a Ternary CH refined with riding coordinates:
N1(H1), C9(H9)
5.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C15(H15), C16(H16),
C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
5.d Fitted hexagon refined as free rotating group:
C20(C21,C22,C23,C24,C25)
5.e 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.