mo_B0429_0m

Table 1 Crystal data and structure refinement for mo_B0429_0m.
Identification code mo_B0429_0m
Empirical formula C30H46Cl5Fe2N2O2Si2Zn1.5
Formula weight 909.87
Temperature/K 100.0
Crystal system monoclinic
Space group C2
a/Å 29.03(2)
b/Å 7.296(5)
c/Å 22.441(15)
α/° 90
β/° 126.677(13)
γ/° 90
Volume/Å3 3811(4)
Z 4
ρcalcg/cm3 1.586
μ/mm‑1 2.126
F(000) 1864.0
Crystal size/mm3 ? × ? × ?
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.852 to 49.956
Index ranges -27 ≤ h ≤ 33, -8 ≤ k ≤ 8, -24 ≤ l ≤ 19
Reflections collected 4868
Independent reflections 3876 [Rint = 0.1676, Rsigma = 0.3006]
Data/restraints/parameters 3876/1/234
Goodness-of-fit on F2 1.047
Final R indexes [I>=2σ (I)] R1 = 0.1037, wR2 = 0.1571
Final R indexes [all data] R1 = 0.2225, wR2 = 0.2087
Largest diff. peak/hole / e Å-3 0.89/-0.74
Flack parameter0.04(4)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0429_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn150003366(6)500025.7(18)
Cl14580(4)5217(12)5368(6)37(3)
Cl25732(4)1603(12)5856(6)56(4)
Zn22874.4(18)-2018(5)5946(2)31.5(12)
Cl33660(6)-3102(14)6076(8)68(4)
Cl43014(4)728(12)6452(5)32(3)
Cl52458(4)-4077(11)6207(6)35(3)
O22310(9)-1570(30)4842(14)43(7)
Fe18084(2)4178(6)8553(3)23.7(15)
Fe24789(2)2823(7)8391(3)21.7(14)
Si16865(4)2733(14)8353(6)24(3)
Si25773(4)4371(13)8122(6)22(3)
O16215(9)3470(30)7975(13)32(7)
N16463(11)5660(30)6378(16)20(7)
N24382(13)650(40)6335(18)43(9)
C17289(13)4540(40)8254(18)12(8)
C27321(14)5190(40)7730(20)19(9)
C37758(12)6520(40)8008(19)9(8)
C48004(16)6800(40)8730(20)33(10)
C57716(15)5690(40)8930(20)34(10)
C68367(14)1580(40)8940(20)21(9)
C78217(15)1780(40)8250(20)28(10)
C88568(16)3110(50)8270(20)58(13)
C98930(15)3730(40)9070(20)25(10)
C108788(15)2880(50)9440(20)41(10)
C116959(11)4470(30)6897(16)4(7)
C126105(16)6160(40)6590(20)33(10)
C136652(15)7380(40)6190(20)31(10)
C146774(16)610(40)7800(20)42(11)
C157225(15)2230(40)9340(20)32(11)
C165351(14)6050(40)7430(20)26(9)
C176196(14)5530(40)9040(19)25(9)
C185369(13)2490(40)8185(19)12(8)
C194807(14)1690(40)7590(20)19(8)
C204678(18)390(50)7910(20)47(12)
C215129(15)250(40)8680(20)29(10)
C225540(16)1550(40)8790(20)31(10)
C234620(14)5520(40)8400(20)25(9)
C244123(16)4630(40)7840(20)37(11)
C254083(18)3430(50)8300(30)51(13)
C264517(15)3440(40)9040(20)32(10)
C274883(15)4870(40)9110(20)25(10)
C284392(16)2160(40)6760(20)32(11)
C293915(17)1120(50)5510(30)58(13)
C304920(20)490(60)6400(30)98(18)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0429_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Zn125(4)22(4)31(5)017(4)0
Cl129(6)44(6)29(9)2(5)13(6)-1(5)
Cl239(7)31(6)45(10)0(5)-4(7)-3(5)
Zn241(3)29(2)24(4)2(2)19(3)2(2)
Cl389(9)49(7)108(13)23(7)81(10)23(6)
Cl440(6)42(6)13(8)-5(4)15(6)-17(5)
Cl529(6)28(5)45(9)-1(5)21(6)-6(5)
Fe117(3)15(3)38(5)3(3)16(3)-1(2)
Fe222(3)24(3)28(4)-11(3)20(3)-10(3)
Si114(6)41(6)16(8)10(5)8(5)2(6)

 

Table 4 Bond Lengths for mo_B0429_0m.
AtomAtomLength/Å AtomAtomLength/Å
Zn1Cl112.279(10) Si2O11.64(3)
Zn1Cl12.279(10) Si2C161.78(3)
Zn1Cl22.232(10) Si2C171.86(3)
Zn1Cl212.232(10) Si2C181.86(3)
Zn2Cl32.262(13) N1C111.48(3)
Zn2Cl42.217(10) N1C121.43(4)
Zn2Cl52.216(10) N1C131.52(3)
Zn2O22.02(3) N2C281.45(4)
Fe1C12.00(3) N2C291.54(5)
Fe1C21.99(3) N2C301.49(5)
Fe1C31.98(3) C1C21.32(4)
Fe1C41.99(3) C1C51.52(5)
Fe1C52.04(4) C2C31.42(4)
Fe1C62.04(3) C2C111.59(4)
Fe1C72.00(3) C3C41.34(4)
Fe1C82.01(4) C4C51.41(5)
Fe1C92.02(3) C6C71.34(5)
Fe1C102.04(4) C6C101.42(5)
Fe2C182.01(3) C7C81.38(5)
Fe2C192.02(4) C8C91.51(5)
Fe2C202.00(4) C9C101.28(5)
Fe2C212.04(3) C18C191.48(4)
Fe2C222.02(3) C18C221.32(4)
Fe2C232.03(3) C19C201.37(5)
Fe2C242.04(4) C19C281.52(5)
Fe2C251.98(4) C20C211.42(5)
Fe2C262.07(4) C21C221.43(4)
Fe2C272.10(4) C23C241.38(4)
Si1O11.63(2) C23C271.38(5)
Si1C11.90(3) C24C251.39(5)
Si1C141.91(4) C25C261.36(5)
Si1C151.84(4) C26C271.42(4)

11-X,+Y,1-Z

 

Table 5 Bond Angles for mo_B0429_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Cl11Zn1Cl1107.3(5) C25Fe2C2440.6(15)
Cl21Zn1Cl11118.0(4) C25Fe2C2639.2(14)
Cl2Zn1Cl1118.0(4) C25Fe2C2764.7(16)
Cl21Zn1Cl1102.3(4) C26Fe2C2739.9(12)
Cl2Zn1Cl11102.3(4) O1Si1C1109.8(12)
Cl21Zn1Cl2109.6(5) O1Si1C14105.3(15)
Cl4Zn2Cl3112.8(4) O1Si1C15109.9(15)
Cl5Zn2Cl3113.3(4) C1Si1C14109.3(17)
Cl5Zn2Cl4116.1(4) C15Si1C1109.7(15)
O2Zn2Cl3103.3(8) C15Si1C14112.8(16)
O2Zn2Cl4104.4(7) O1Si2C16108.1(16)
O2Zn2Cl5105.2(7) O1Si2C17109.1(14)
C1Fe1C544.1(13) O1Si2C18108.8(13)
C1Fe1C6110.8(13) C16Si2C17108.3(16)
C1Fe1C8145.9(15) C16Si2C18116.1(15)
C1Fe1C9167.9(16) C17Si2C18106.3(15)
C1Fe1C10132.2(15) Si1O1Si2146.0(17)
C2Fe1C138.7(12) C11N1C13111(2)
C2Fe1C567.4(14) C12N1C11117(3)
C2Fe1C6132.7(13) C12N1C13109(2)
C2Fe1C7109.9(15) C28N2C29106(3)
C2Fe1C8116.7(16) C28N2C30113(3)
C2Fe1C9152.8(15) C30N2C29105(3)
C2Fe1C10170.2(15) Si1C1Fe1124.6(15)
C3Fe1C169.6(12) C2C1Fe170(2)
C3Fe1C241.7(11) C2C1Si1138(3)
C3Fe1C439.4(13) C2C1C5104(3)
C3Fe1C567.2(14) C5C1Fe169.2(18)
C3Fe1C6169.9(15) C5C1Si1118(3)
C3Fe1C7131.4(16) C1C2Fe171(2)
C3Fe1C8107.8(16) C1C2C3112(3)
C3Fe1C9117.5(13) C1C2C11125(3)
C3Fe1C10146.3(14) C3C2Fe168.8(18)
C4Fe1C172.1(13) C3C2C11122(3)
C4Fe1C268.5(14) C11C2Fe1124(2)
C4Fe1C540.9(14) C2C3Fe169.5(17)
C4Fe1C6150.7(16) C4C3Fe171(2)
C4Fe1C7167.7(16) C4C3C2109(3)
C4Fe1C8128.5(17) C3C4Fe170(2)
C4Fe1C9106.7(15) C3C4C5108(3)
C4Fe1C10114.8(17) C5C4Fe171(2)
C5Fe1C6120.6(15) C1C5Fe166.7(19)
C5Fe1C10108.6(16) C4C5Fe168(2)
C6Fe1C1040.7(13) C4C5C1107(4)
C7Fe1C1114.8(13) C7C6Fe169(2)
C7Fe1C5150.8(15) C7C6C10112(3)
C7Fe1C638.7(14) C10C6Fe169.8(19)
C7Fe1C840.3(14) C6C7Fe172(2)
C7Fe1C968.8(14) C6C7C8108(3)
C7Fe1C1068.9(16) C8C7Fe170(2)
C8Fe1C5168.1(16) C7C8Fe169(2)
C8Fe1C665.8(16) C7C8C9103(4)
C8Fe1C944.0(14) C9C8Fe168(2)
C8Fe1C1069.1(17) C8C9Fe168(2)
C9Fe1C5127.5(16) C10C9Fe173(2)
C9Fe1C664.1(13) C10C9C8111(4)
C9Fe1C1036.8(13) C6C10Fe170(2)
C18Fe2C1943.2(12) C9C10Fe171(2)
C18Fe2C2169.5(13) C9C10C6106(4)
C18Fe2C2238.3(13) N1C11C2113(2)
C18Fe2C23111.3(13) Si2C18Fe2125.4(14)
C18Fe2C24124.4(14) C19C18Fe268.6(18)
C18Fe2C26155.4(14) C19C18Si2129(3)
C18Fe2C27121.6(12) C22C18Fe271(2)
C19Fe2C2168.9(14) C22C18Si2126(3)
C19Fe2C2267.0(15) C22C18C19105(3)
C19Fe2C23123.1(14) C18C19Fe268.2(19)
C19Fe2C24104.5(16) C18C19C28131(3)
C19Fe2C26160.1(13) C20C19Fe270(2)
C19Fe2C27157.6(13) C20C19C18107(4)
C20Fe2C1869.8(14) C20C19C28122(3)
C20Fe2C1939.9(14) C28C19Fe2125(2)
C20Fe2C2141.1(14) C19C20Fe271(2)
C20Fe2C2267.4(15) C19C20C21111(4)
C20Fe2C23154.6(16) C21C20Fe271(2)
C20Fe2C24117.4(17) C20C21Fe268(2)
C20Fe2C26124.4(15) C20C21C22103(3)
C20Fe2C27162.3(16) C22C21Fe268.6(18)
C21Fe2C26106.9(15) C18C22Fe270(2)
C21Fe2C27126.4(15) C18C22C21114(3)
C22Fe2C2141.2(12) C21C22Fe270(2)
C22Fe2C23130.1(14) C24C23Fe270.4(19)
C22Fe2C24161.6(15) C27C23Fe273(2)
C22Fe2C26123.5(16) C27C23C24116(4)
C22Fe2C27112.1(15) C23C24Fe270(2)
C23Fe2C21164.3(15) C23C24C2598(4)
C23Fe2C2439.7(12) C25C24Fe268(2)
C23Fe2C2665.4(14) C24C25Fe272(2)
C23Fe2C2739.0(12) C26C25Fe274(2)
C24Fe2C21153.2(14) C26C25C24118(4)
C24Fe2C2670.1(16) C25C26Fe267(2)
C24Fe2C2769.2(15) C25C26C27103(3)
C25Fe2C18163.3(16) C27C26Fe271(2)
C25Fe2C19125.0(16) C23C27Fe268(2)
C25Fe2C20108.5(17) C23C27C26105(3)
C25Fe2C21120.8(15) C26C27Fe269.0(19)
C25Fe2C22157.6(16) N2C28C19109(3)
C25Fe2C2362.7(14)     

11-X,+Y,1-Z

 

Table 6 Hydrogen Bonds for mo_B0429_0m.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1Cl111.002.373.23(3)143.4
N2H2Cl31.002.393.28(3)147.5

11-X,+Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0429_0m.
AtomxyzU(eq)
H162144953590324
H24292-532647252
H378617126772711
H483267661906740
H577785677939441
H68209678907125
H779221128782033
H885793522787870
H992284715928030
H1089343071994050
H11A7211440767395
H11B6819321768755
H12A59095075659249
H12B58207063623749
H12C63426703708949
H13A69048107664646
H13B63148105582446
H13C68607030599246
H14A6658-429795463
H14B7139331788063
H14C6478845726663
H15A72923380961247
H15B75941630955147
H15C69811424939647
H16A55697193756438
H16B49976267738138
H16C52525612695038
H17A63614606943538
H17B59446345907438
H17C65056246909638
H204334-313765156
H215151-529903835
H2259031728925438
H2347726520830129
H2438854785732144
H2537632635809261
H2645652673941139
H2752325279955830
H28A40022362662539
H28B45183292665839
H29A35831655545987
H29B3797-1521487
H29C40691999534387
H30A4890-5446097147
H30B498116256216147
H30C52472976918147

Experimental

Single crystals of C30H46Cl5Fe2N2O2Si2Zn1.5 [mo_B0429_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 100.0 K during data collection. Using Olex2 [1], the structure was solved with the XT [2] structure solution program using Intrinsic Phasing 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_B0429_0m]

Crystal Data for C30H46Cl5Fe2N2O2Si2Zn1.5 (=909.87 g/mol): monoclinic, space group C2 (no. 5), a = 29.03(2) Å, b = 7.296(5) Å, c = 22.441(15) Å, β = 126.677(13)°, = 3811(4) Å3, Z = 4, T = 100.0 K, μ(MoKα) = 2.126 mm-1, Dcalc = 1.586 g/cm3, 4868 reflections measured (5.852° ≤ 2Θ ≤ 49.956°), 3876 unique (Rint = 0.1676, Rsigma = 0.3006) which were used in all calculations. The final R1 was 0.1037 (I > 2σ(I)) and wR2 was 0.2087 (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, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
N1(H1), N2(H2), C4(H4), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C28(H28A,H28B)
2.c Me refined with riding coordinates:
C30(H30A,H30B,H30C)
2.d Aromatic/amide H refined with riding coordinates:
C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C20(H20), C21(H21),
C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.e Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C)

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