mo_B0383_0m

Table 1 Crystal data and structure refinement for mo_B0383_0m.
Identification code mo_B0383_0m
Empirical formula C21H44Br2N2O5Zn3
Formula weight 760.51
Temperature/K 99.99
Crystal system monoclinic
Space group P21/n
a/Å 12.1460(7)
b/Å 21.0763(13)
c/Å 12.5832(7)
α/° 90
β/° 115.275(2)
γ/° 90
Volume/Å3 2912.8(3)
Z 4
ρcalcg/cm3 1.734
μ/mm‑1 5.225
F(000) 1536.0
Crystal size/mm3 0.22 × 0.17 × 0.13
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.182 to 53.998
Index ranges -15 ≤ h ≤ 15, -26 ≤ k ≤ 26, -16 ≤ l ≤ 16
Reflections collected 60917
Independent reflections 6355 [Rint = 0.0406, Rsigma = 0.0191]
Data/restraints/parameters 6355/0/323
Goodness-of-fit on F2 1.274
Final R indexes [I>=2σ (I)] R1 = 0.0176, wR2 = 0.0522
Final R indexes [all data] R1 = 0.0219, wR2 = 0.0702
Largest diff. peak/hole / e Å-3 0.92/-0.98

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0383_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br17956.6(2)6100.2(2)5900.6(2)21.64(7)
Br28056.6(2)3402.4(2)5399.7(2)21.98(7)
Zn24521.0(2)4965.8(2)3274.4(2)11.88(7)
Zn36134.5(2)3807.0(2)5136.1(2)11.85(6)
Zn16215.9(2)6311.1(2)4111.6(2)13.33(7)
O33716.0(14)5356.0(7)4123.0(13)16.2(3)
O14866.7(13)6713.7(7)4321.5(13)15.8(3)
O45035.5(13)4086.4(7)3558.7(12)13.1(3)
O25687.7(14)5557.8(7)3175.6(14)17.7(3)
N16357.3(16)7134.6(8)3232.4(16)16.0(3)
O57621.0(17)5227.4(10)2500.6(19)37.2(4)
N23270.1(15)4673.5(9)1554.4(14)15.1(3)
C57642(2)7367.5(11)3705(2)21.8(5)
C45644(2)7580.3(10)3613(2)19.4(4)
C104656.8(18)3727(1)2503.1(18)14.5(4)
C14507.5(19)7298.9(10)3689(2)18.2(4)
C68421(2)6946.1(12)3323(2)25.9(5)
C23426(2)7176.2(11)2502(2)24.1(5)
C133386.3(19)3972.3(10)1664.2(18)16.6(4)
C34149(2)7787.6(11)4385(2)26.2(5)
C115624(2)3783.5(11)2035(2)21.2(5)
C141994.2(19)4850.7(11)1300(2)21.0(4)
C124502(2)3031.8(10)2750(2)20.4(4)
C95852(2)7118.8(12)1922(2)22.8(5)
C183549(2)4909.9(12)580(2)24.5(5)
C151795(2)5562.4(12)1175(2)26.0(5)
C77908(2)6910.7(13)1988(2)30.2(5)
C219621(2)5269.3(13)2614(2)30.1(5)
C173393(2)5624.1(13)429(2)29.5(5)
C162109(2)5825.6(13)207(2)32.0(6)
C86588(2)6697.0(12)1490(2)26.9(5)
C198625(2)5035.8(15)2911(3)38.2(7)
C20B8770(5)4278(4)3187(8)48(3)
C20A9040(8)4762(6)4147(8)91(4)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0383_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br118.24(11)22.63(12)21.73(12)4.36(8)6.29(9)2.41(8)
Br214.31(11)23.20(12)30.65(13)4.03(9)11.71(9)5.93(8)
Zn212.43(12)9.61(12)14.46(12)-1.48(8)6.57(9)-0.81(8)
Zn311.70(12)10.76(12)14.39(12)0.31(8)6.82(9)1.34(8)
Zn113.25(12)9.42(12)19.37(13)0.94(8)8.92(10)-0.03(8)
O318.8(7)13.3(7)21.0(8)-4.3(6)12.8(6)-4.1(6)
O116.2(7)9.7(7)24.8(8)4.7(6)12.0(6)3.0(5)
O415.4(7)10.8(7)12.4(6)-3.1(5)5.2(6)-0.1(5)
O216.9(7)13.1(7)28.1(8)-3.1(6)14.3(7)-2.2(6)
N117.4(8)12.4(8)21.0(9)1.0(7)10.8(7)-1.8(7)
O531.9(10)37.0(11)52.8(12)2.7(9)27.9(9)4.8(8)
N214.7(8)17.8(9)12.4(8)0.7(7)5.5(7)-0.3(7)
C519.6(10)17.7(11)30.3(12)0.2(9)12.8(9)-6.2(9)
C424.8(11)9.5(9)28.4(11)2.1(8)15.6(9)0.4(8)
C1016.1(9)12.8(10)15.3(10)-6.3(7)7.3(8)-2.6(7)
C120.2(10)11.9(10)26.5(11)6.1(8)13.8(9)4.0(8)
C619.5(10)26.5(12)36.0(13)4.9(10)15.8(10)-1.0(9)
C219.3(10)24.1(12)29.6(12)9.9(9)11.1(9)5.1(9)
C1317(1)16.7(10)15.0(9)-4.6(8)5.7(8)-3.3(8)
C333.2(13)12.6(10)42.0(14)4.7(10)24.9(12)6.3(9)
C1121.6(11)25.3(12)21.4(11)-4.2(9)13.6(9)-0.3(9)
C1413.8(10)25.3(11)20.1(10)1.3(9)3.7(8)0.5(8)
C1222.5(10)12.3(10)26.7(11)-6.2(8)10.8(9)-2.9(8)
C922.6(11)24.7(12)21.8(11)6.7(9)10.3(9)1.0(9)
C1829.5(12)31.2(13)16.3(10)4.0(9)13.1(10)1.7(10)
C1521.3(11)27.1(13)26.7(12)6.1(10)7.6(10)7.2(10)
C731.9(13)32.0(14)38.0(14)5.2(11)25.7(12)1.1(11)
C2124.4(12)31.5(14)35.5(13)5.1(11)13.8(11)-1.5(10)
C1735.6(13)32.8(14)23.2(12)11.7(10)15.4(11)2.0(11)
C1636.1(14)29.8(13)23.7(12)12(1)6.5(11)5.5(11)
C832.6(13)29.2(13)24.0(12)0.8(10)16.9(10)-0.5(10)
C1926.6(13)47.6(18)40.2(15)21.1(13)14.0(12)3.6(12)
C20B19(3)48(4)74(6)37(4)17(3)4(3)
C20A81(6)143(10)71(6)69(6)52(5)55(6)

 

Table 4 Bond Lengths for mo_B0383_0m.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.3814(3) N2C131.485(3)
Br2Zn32.3719(3) N2C141.490(3)
Zn2O31.9143(15) N2C181.491(3)
Zn2O41.9397(14) C5C61.518(3)
Zn2O21.9314(15) C4C11.542(3)
Zn2N22.1364(17) C10C131.540(3)
Zn3O311.9672(15) C10C111.527(3)
Zn3O111.9641(14) C10C121.526(3)
Zn3O41.9508(14) C1C21.532(3)
Zn1O11.9609(14) C1C31.531(3)
Zn1O21.9168(15) C6C71.523(4)
Zn1N12.1045(17) C14C151.517(3)
O3Zn311.9672(15) C9C81.517(3)
O1Zn311.9641(14) C18C171.519(4)
O1C11.431(2) C15C161.528(3)
O4C101.424(2) C7C81.519(3)
N1C51.496(3) C21C191.493(3)
N1C41.489(3) C17C161.522(4)
N1C91.494(3) C19C20B1.628(8)
O5C191.175(3) C19C20A1.529(7)

11-X,1-Y,1-Z

 

Table 5 Bond Angles for mo_B0383_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O3Zn2O4120.57(6) C13N2C18111.29(17)
O3Zn2O2108.77(7) C14N2Zn2111.73(13)
O3Zn2N2112.17(7) C14N2C18108.68(17)
O4Zn2N286.85(6) C18N2Zn2115.08(14)
O2Zn2O4116.22(6) N1C5C6111.58(18)
O2Zn2N2110.19(7) N1C4C1115.87(17)
O31Zn3Br2111.71(5) O4C10C13106.90(16)
O11Zn3Br2117.97(4) O4C10C11108.86(16)
O11Zn3O31106.38(6) O4C10C12109.83(17)
O4Zn3Br2117.12(4) C11C10C13114.83(18)
O4Zn3O3195.51(6) C12C10C13106.70(17)
O4Zn3O11105.43(6) C12C10C11109.63(17)
O1Zn1Br1114.15(5) O1C1C4107.30(16)
O1Zn1N188.53(6) O1C1C2109.12(17)
O2Zn1Br1110.82(5) O1C1C3110.80(18)
O2Zn1O1111.19(7) C2C1C4114.97(18)
O2Zn1N1116.18(7) C3C1C4104.92(18)
N1Zn1Br1114.34(5) C3C1C2109.65(18)
Zn2O3Zn31133.15(9) C5C6C7111.2(2)
Zn1O1Zn31118.82(7) N2C13C10115.18(17)
C1O1Zn31126.01(12) N2C14C15112.06(18)
C1O1Zn1111.82(12) N1C9C8112.42(19)
Zn2O4Zn3120.18(7) N2C18C17111.95(19)
C10O4Zn2112.70(12) C14C15C16111.0(2)
C10O4Zn3126.63(12) C8C7C6109.41(19)
Zn1O2Zn2123.91(8) C18C17C16111.3(2)
C5N1Zn1111.54(13) C17C16C15109.74(19)
C4N1Zn199.31(12) C9C8C7111.0(2)
C4N1C5108.46(17) O5C19C21125.2(3)
C4N1C9110.37(17) O5C19C20B115.4(3)
C9N1Zn1118.33(14) O5C19C20A113.9(4)
C9N1C5108.25(17) C21C19C20B110.6(3)
C13N2Zn2101.21(12) C21C19C20A115.4(4)
C13N2C14108.55(16)     

11-X,1-Y,1-Z

 

Table 6 Torsion Angles for mo_B0383_0m.
ABCDAngle/˚ ABCDAngle/˚
Zn2O4C10C13-36.56(18) N1C4C1C3165.85(18)
Zn2O4C10C1188.02(17) N1C9C8C7-57.6(3)
Zn2O4C10C12-151.95(13) N2C14C15C1657.6(3)
Zn2N2C13C10-32.19(18) N2C18C17C16-57.3(3)
Zn2N2C14C1569.2(2) C5N1C4C1-154.89(19)
Zn2N2C18C17-67.6(2) C5N1C9C858.5(2)
Zn31O1C1C4171.95(13) C5C6C7C8-54.8(3)
Zn31O1C1C2-62.9(2) C4N1C5C6-178.37(18)
Zn31O1C1C357.9(2) C4N1C9C8177.02(18)
Zn3O4C10C13151.58(13) C6C7C8C954.1(3)
Zn3O4C10C11-83.84(19) C13N2C14C15179.93(18)
Zn3O4C10C1236.2(2) C13N2C18C17178.06(19)
Zn1O1C1C4-29.2(2) C11C10C13N2-73.4(2)
Zn1O1C1C296.01(16) C14N2C13C10-149.88(17)
Zn1O1C1C3-143.16(15) C14N2C18C1758.6(2)
Zn1N1C5C673.3(2) C14C15C16C17-53.6(3)
Zn1N1C4C1-38.3(2) C12C10C13N2164.87(17)
Zn1N1C9C8-69.6(2) C9N1C5C6-58.6(2)
O4C10C13N247.4(2) C9N1C4C186.7(2)
N1C5C6C758.5(2) C18N2C13C1090.6(2)
N1C4C1O147.9(2) C18N2C14C15-58.9(2)
N1C4C1C2-73.6(2) C18C17C16C1553.5(3)

11-X,1-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0383_0m.
AtomxyzU(eq)
H5A79937378457426
H5B76497805342426
H4A53837942305923
H4B61907750439623
H6A84566514364531
H6B92617116364331
H2A36226825210236
H2B32577559201736
H2C27087066263036
H13A3170379187420
H13B27873812194020
H3A34367635448339
H3B39528192395939
H3C48287850515939
H11A57784233194832
H11B53353573126932
H11C63783581258732
H14A18014695194325
H14B1431464156425
H12A52962853326831
H12B41602795200931
H12C39503001313331
H9A58397555162627
H9B50036963159827
H18A30034699-16229
H18B4398479674429
H15A23105771193031
H15B933565898631
H7A79617333166736
H7B83906607175936
H21A92675462183145
H21B101424913262245
H21C101085586319545
H17A35625760-24135
H17B39875837114535
H16A15215664-56738
H16B2055629419438
H8A6233671162132
H8B65506253173032
H20A83474165367271
H20B96364171360971
H20C84154041244771
H20D966250394715137
H20E938143384177137
H20F834247354343137
H33290(30)5135(13)4180(20)16(7)
H26190(30)5419(16)3060(30)39(9)

 

Table 8 Atomic Occupancy for mo_B0383_0m.
AtomOccupancy AtomOccupancy AtomOccupancy
C20B0.446(9) H20A0.446(9) H20B0.446(9)
H20C0.446(9) C20A0.554(9) H20D0.554(9)
H20E0.554(9) H20F0.554(9)   

Experimental

Single crystals of C21H44Br2N2O5Zn3 [mo_B0383_0m] were []. A suitable crystal was selected and [] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 99.99 K during data collection. Using Olex2 [1], the structure was solved with the SIR2004 [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. Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R. (2007). J. Appl. Cryst. 40, 609-613.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [mo_B0383_0m]

Crystal Data for C21H44Br2N2O5Zn3 (=760.51 g/mol): monoclinic, space group P21/n (no. 14), a = 12.1460(7) Å, b = 21.0763(13) Å, c = 12.5832(7) Å, β = 115.275(2)°, = 2912.8(3) Å3, Z = 4, T = 99.99 K, μ(MoKα) = 5.225 mm-1, Dcalc = 1.734 g/cm3, 60917 reflections measured (4.182° ≤ 2Θ ≤ 53.998°), 6355 unique (Rint = 0.0406, Rsigma = 0.0191) which were used in all calculations. The final R1 was 0.0176 (I > 2σ(I)) and wR2 was 0.0702 (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,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(1)
Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C5(H5A,H5B), C4(H4A,H4B), C6(H6A,H6B), C13(H13A,H13B), C14(H14A,H14B), C9(H9A,
H9B), C18(H18A,H18B), C15(H15A,H15B), C7(H7A,H7B), C17(H17A,H17B), C16(H16A,
H16B), C8(H8A,H8B)
3.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
C21(H21A,H21B,H21C), C20B(H20A,H20B,H20C), C20A(H20D,H20E,H20F)

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