3103_twin1_hklf4

Table 1 Crystal data and structure refinement for 3103_twin1_hklf4.
Identification code 3103_twin1_hklf4
Empirical formula C23H28ClFe2NO2Si
Formula weight 525.70
Temperature/K 173
Crystal system monoclinic
Space group P21/c
a/Å 7.5429(5)
b/Å 10.7933(6)
c/Å 26.917(2)
α/° 90
β/° 93.719(6)
γ/° 90
Volume/Å3 2186.7(2)
Z 4
ρcalcg/cm3 1.597
μ/mm‑1 1.525
F(000) 1088.0
Crystal size/mm3 0.35 × 0.2 × 0.15
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.842 to 53.998
Index ranges -9 ≤ h ≤ 9, -13 ≤ k ≤ 13, -34 ≤ l ≤ 34
Reflections collected 5183
Independent reflections 5183 [Rint = ?, Rsigma = 0.0494]
Data/restraints/parameters 5183/6/280
Goodness-of-fit on F2 1.142
Final R indexes [I>=2σ (I)] R1 = 0.0869, wR2 = 0.2406
Final R indexes [all data] R1 = 0.0986, wR2 = 0.2450
Largest diff. peak/hole / e Å-3 0.87/-1.16

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3103_twin1_hklf4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe1652.0(18)6460.7(14)901.1(6)21.3(3)
Fe25108.0(18)1394.0(14)913.5(6)23.8(3)
Cl14681(4)1909(3)2776.3(11)34.4(7)
Si12741(4)3819(2)1414.6(11)22.8(6)
O12215(10)3141(8)1934(3)33.6(19)
O24562(10)4629(7)1495(3)30.4(17)
N1-1246(12)5302(8)2357(3)23.5(19)
C1726(12)4726(9)1215(4)18.6(19)
C2-284(13)5594(9)1497(4)22(2)
C3-1729(13)6054(9)1175(4)25(2)
C4-1645(14)5527(10)704(4)29(2)
C5-117(13)4704(9)721(4)22(2)
C63161(13)7034(11)792(5)34(3)
C72460(15)7791(11)1151(5)34(3)
C8927(17)8333(9)918(6)42(3)
C9707(17)7934(11)417(5)40(3)
C102110(20)7106(12)340(5)46(4)
C1181(13)5879(10)2028(4)25(2)
C12-652(19)5356(12)2878(4)41(3)
C13-1761(16)4027(11)2222(4)33(3)
C143087(13)2705(9)913(4)20(2)
C154232(15)2879(10)502(4)30(2)
C164150(15)1798(11)205(4)32(3)
C173035(14)924(11)415(4)29(2)
C182418(13)1473(11)854(4)30(2)
C196552(14)1482(12)1585(4)33(3)
C207614(14)1798(10)1192(4)30(2)
C217625(15)771(10)863(4)29.8(18)
C226603(16)-170(11)1046(5)39(3)
C235917(15)259(11)1504(5)33(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3103_twin1_hklf4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe118.1(7)17.1(7)28.7(7)1.3(6)3.0(6)0.6(6)
Fe217.8(7)19.8(7)33.9(8)-1.4(7)3.6(6)2.9(6)
Cl124.5(13)38.1(15)39.9(15)12.9(13)-2.8(11)-12.6(12)
Si119.7(13)14.3(13)34.5(15)0.7(11)3.7(12)4.5(11)
O119(4)43(5)39(5)6(4)1(3)11(3)
O228(4)22(4)41(5)-5(3)0(3)10(3)
N125(5)22(4)25(4)-2(4)10(4)-1(4)
C111(4)17(4)29(5)5(4)4(4)-1(4)
C220(5)19(5)29(5)6(4)8(4)3(4)
C314(5)18(5)44(6)12(5)12(4)5(4)
C415(5)31(6)41(6)9(5)-3(4)-4(4)
C520(5)20(5)26(5)0(4)-4(4)-8(4)
C67(5)35(6)62(8)5(6)3(5)-5(4)
C731(6)29(6)42(7)7(5)-8(5)-16(5)
C840(7)9(5)76(9)8(5)8(7)-2(5)
C934(7)34(7)50(7)21(6)-4(6)-6(6)
C1074(10)35(7)31(6)-1(5)16(7)-23(7)
C1115(5)21(5)40(6)3(4)4(4)-6(4)
C1251(8)36(7)34(6)2(5)-4(6)-2(6)
C1328(6)34(6)36(6)-4(5)5(5)-15(5)
C1416(5)27(5)17(4)-3(4)-1(4)4(4)
C1527(6)23(5)40(6)0(5)4(5)8(5)
C1631(6)33(6)31(6)-4(5)0(5)1(5)
C1721(5)28(6)39(6)-6(5)-2(4)0(4)
C1815(5)38(6)36(6)4(5)3(4)6(5)
C1923(5)40(6)36(6)0(5)1(5)8(5)
C2020(5)27(6)43(7)-1(5)6(5)-3(4)
C2129.8(18)29.8(18)29.8(18)0.00(11)1.94(16)0.01(11)
C2232(6)20(5)61(8)-3(5)-19(6)10(5)
C2325(6)33(6)42(7)11(5)-1(5)2(5)

 

Table 4 Bond Lengths for 3103_twin1_hklf4.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.053(9) N1C111.514(12)
Fe1C22.024(10) N1C121.445(14)
Fe1C32.033(10) N1C131.468(13)
Fe1C42.044(11) C1C21.453(14)
Fe1C52.032(10) C1C51.436(13)
Fe1C62.030(10) C2C31.436(14)
Fe1C72.062(11) C2C111.468(14)
Fe1C82.032(10) C3C41.394(16)
Fe1C92.058(12) C4C51.454(15)
Fe1C102.045(12) C6C71.394(18)
Fe2C142.080(10) C6C101.411(18)
Fe2C152.034(11) C7C81.406(17)
Fe2C162.042(11) C8C91.417(19)
Fe2C172.057(11) C9C101.408(19)
Fe2C182.027(10) C14C151.458(14)
Fe2C192.051(11) C14C181.427(15)
Fe2C202.035(11) C15C161.414(15)
Fe2C212.027(11) C16C171.406(16)
Fe2C222.049(11) C17C181.427(15)
Fe2C232.068(11) C19C201.410(15)
Si1O11.649(8) C19C231.417(17)
Si1O21.631(8) C20C211.420(15)
Si1C11.858(10) C21C221.386(16)
Si1C141.840(10) C22C231.444(17)

 

Table 5 Bond Angles for 3103_twin1_hklf4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C7120.1(4) C22Fe2C14162.9(5)
C1Fe1C9164.5(5) C22Fe2C17107.3(5)
C2Fe1C141.8(4) C22Fe2C1968.3(5)
C2Fe1C341.5(4) C22Fe2C2341.0(5)
C2Fe1C469.1(4) C23Fe2C14125.7(4)
C2Fe1C569.5(4) O1Si1C1104.0(4)
C2Fe1C6129.2(5) O1Si1C14112.7(5)
C2Fe1C7108.7(5) O2Si1O1111.9(4)
C2Fe1C8118.8(5) O2Si1C1115.0(4)
C2Fe1C9151.9(5) O2Si1C14106.9(4)
C2Fe1C10166.9(5) C14Si1C1106.5(4)
C3Fe1C169.8(4) C12N1C11112.1(9)
C3Fe1C440.0(5) C12N1C13109.8(9)
C3Fe1C7127.8(5) C13N1C11114.5(8)
C3Fe1C9116.8(5) Si1C1Fe1126.8(5)
C3Fe1C10150.5(5) C2C1Fe168.1(5)
C4Fe1C169.9(4) C2C1Si1129.4(8)
C4Fe1C7163.5(5) C5C1Fe168.6(5)
C4Fe1C9105.6(5) C5C1Si1124.3(8)
C4Fe1C10117.6(5) C5C1C2106.2(8)
C5Fe1C141.2(4) C1C2Fe170.2(5)
C5Fe1C368.9(4) C1C2C11124.9(9)
C5Fe1C441.8(4) C3C2Fe169.6(5)
C5Fe1C7154.1(5) C3C2C1108.1(9)
C5Fe1C9125.9(5) C3C2C11127.0(9)
C5Fe1C10107.5(5) C11C2Fe1128.4(7)
C6Fe1C1109.7(4) C2C3Fe168.9(5)
C6Fe1C3166.3(5) C4C3Fe170.4(6)
C6Fe1C4153.6(5) C4C3C2109.3(9)
C6Fe1C5120.3(5) C3C4Fe169.6(6)
C6Fe1C739.8(5) C3C4C5107.7(9)
C6Fe1C866.7(5) C5C4Fe168.7(6)
C6Fe1C967.4(5) C1C5Fe170.2(5)
C6Fe1C1040.5(5) C1C5C4108.7(9)
C8Fe1C1153.9(5) C4C5Fe169.5(6)
C8Fe1C3107.3(5) C7C6Fe171.3(6)
C8Fe1C4125.4(5) C7C6C10110.3(11)
C8Fe1C5163.9(5) C10C6Fe170.3(7)
C8Fe1C740.1(5) C6C7Fe168.9(6)
C8Fe1C940.5(5) C6C7C8105.9(11)
C8Fe1C1067.6(5) C8C7Fe168.8(6)
C9Fe1C768.2(5) C7C8Fe171.1(6)
C10Fe1C1127.8(5) C7C8C9109.8(11)
C10Fe1C768.1(5) C9C8Fe170.7(7)
C10Fe1C940.1(5) C8C9Fe168.8(6)
C15Fe2C1441.5(4) C10C9Fe169.4(7)
C15Fe2C1640.6(4) C10C9C8106.8(11)
C15Fe2C1768.4(5) C6C10Fe169.2(6)
C15Fe2C19125.3(5) C9C10Fe170.4(7)
C15Fe2C20107.0(5) C9C10C6107.1(11)
C15Fe2C22154.2(5) C2C11N1113.2(8)
C15Fe2C23162.7(5) Si1C14Fe2125.6(5)
C16Fe2C1468.9(4) C15C14Fe267.6(6)
C16Fe2C1740.1(5) C15C14Si1126.3(8)
C16Fe2C19161.5(5) C18C14Fe267.7(5)
C16Fe2C22119.7(5) C18C14Si1128.6(8)
C16Fe2C23156.0(5) C18C14C15105.0(9)
C17Fe2C1468.9(4) C14C15Fe270.9(6)
C17Fe2C23122.0(5) C16C15Fe270.0(6)
C18Fe2C1440.7(4) C16C15C14108.4(10)
C18Fe2C1568.6(5) C15C16Fe269.4(6)
C18Fe2C1668.0(5) C17C16Fe270.5(7)
C18Fe2C1740.9(4) C17C16C15109.3(10)
C18Fe2C19122.6(4) C16C17Fe269.4(6)
C18Fe2C20157.1(5) C16C17C18106.9(10)
C18Fe2C22125.8(5) C18C17Fe268.4(6)
C18Fe2C23109.2(5) C14C18Fe271.7(6)
C19Fe2C14108.5(4) C17C18Fe270.7(6)
C19Fe2C17157.5(5) C17C18C14110.2(10)
C19Fe2C2340.2(5) C20C19Fe269.2(6)
C20Fe2C14121.2(4) C20C19C23108.3(10)
C20Fe2C16124.2(5) C23C19Fe270.5(7)
C20Fe2C17160.4(5) C19C20Fe270.4(6)
C20Fe2C1940.4(4) C19C20C21107.8(10)
C20Fe2C2268.0(5) C21C20Fe269.2(6)
C20Fe2C2367.9(5) C20C21Fe269.9(6)
C21Fe2C14156.2(4) C22C21Fe271.0(7)
C21Fe2C15119.8(4) C22C21C20108.9(10)
C21Fe2C16106.5(5) C21C22Fe269.3(6)
C21Fe2C17123.4(5) C21C22C23107.9(10)
C21Fe2C18161.1(5) C23C22Fe270.2(6)
C21Fe2C1968.2(4) C19C23Fe269.2(6)
C21Fe2C2040.9(4) C19C23C22107.1(10)
C21Fe2C2239.7(5) C22C23Fe268.8(6)
C21Fe2C2367.9(5)     

 

Table 6 Hydrogen Bonds for 3103_twin1_hklf4.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1Cl10.842.383.134(8)150.3
O2H2Cl110.842.413.175(8)152.2
N1H1ACl121.03(9)2.10(10)3.120(9)173(8)

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

 

Table 7 Torsion Angles for 3103_twin1_hklf4.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C359.5(7) C1C2C11N1-105.8(11)
Fe1C1C2C11-123.6(10) C2C1C5Fe157.9(6)
Fe1C1C5C4-59.1(7) C2C1C5C4-1.2(11)
Fe1C2C3C459.0(7) C2C3C4Fe1-58.1(7)
Fe1C2C11N1162.7(7) C2C3C4C50.1(12)
Fe1C3C4C558.2(7) C3C2C11N170.5(13)
Fe1C4C5C159.5(7) C3C4C5Fe1-58.8(7)
Fe1C6C7C8-59.1(8) C3C4C5C10.7(11)
Fe1C6C10C960.5(8) C5C1C2Fe1-58.2(6)
Fe1C7C8C9-60.4(8) C5C1C2C31.3(11)
Fe1C8C9C10-59.3(8) C5C1C2C11178.2(9)
Fe1C9C10C6-59.7(8) C6C7C8Fe159.1(8)
Fe2C14C15C1660.2(8) C6C7C8C9-1.2(13)
Fe2C14C18C17-60.4(7) C7C6C10Fe1-60.4(8)
Fe2C15C16C1759.3(8) C7C6C10C90.1(13)
Fe2C16C17C1858.3(7) C7C8C9Fe160.6(8)
Fe2C17C18C1461.0(7) C7C8C9C101.3(13)
Fe2C19C20C21-59.4(8) C8C9C10Fe158.8(8)
Fe2C19C23C2258.6(8) C8C9C10C6-0.9(13)
Fe2C20C21C22-60.5(8) C10C6C7Fe159.7(8)
Fe2C21C22C23-59.8(8) C10C6C7C80.7(13)
Fe2C22C23C19-58.9(8) C11C2C3Fe1123.3(10)
Si1C1C2Fe1120.4(8) C11C2C3C4-177.7(10)
Si1C1C2C3179.9(7) C12N1C11C2167.1(9)
Si1C1C2C11-3.2(15) C13N1C11C241.2(13)
Si1C1C5Fe1-120.8(7) C14Si1C1Fe1-99.4(7)
Si1C1C5C4-179.9(7) C14Si1C1C2170.0(9)
Si1C14C15Fe2118.6(8) C14Si1C1C5-11.7(9)
Si1C14C15C16178.9(8) C14C15C16Fe2-60.8(7)
Si1C14C18Fe2-118.6(8) C14C15C16C17-1.5(13)
Si1C14C18C17-179.0(8) C15C14C18Fe257.5(7)
O1Si1C1Fe1141.4(6) C15C14C18C17-2.9(11)
O1Si1C1C250.7(10) C15C16C17Fe2-58.7(8)
O1Si1C1C5-130.9(8) C15C16C17C18-0.3(13)
O1Si1C14Fe2-65.5(7) C16C17C18Fe2-58.9(8)
O1Si1C14C15-152.3(8) C16C17C18C142.1(12)
O1Si1C14C1823.0(10) C18C14C15Fe2-57.6(7)
O2Si1C1Fe118.7(8) C18C14C15C162.7(12)
O2Si1C1C2-71.9(10) C19C20C21Fe260.1(8)
O2Si1C1C5106.5(8) C19C20C21C22-0.4(13)
O2Si1C14Fe257.7(7) C20C19C23Fe2-59.1(8)
O2Si1C14C15-29.0(10) C20C19C23C22-0.6(12)
O2Si1C14C18146.3(9) C20C21C22Fe259.8(8)
C1Si1C14Fe2-178.9(6) C20C21C22C230.0(13)
C1Si1C14C1594.3(9) C21C22C23Fe259.2(8)
C1Si1C14C18-90.4(10) C21C22C23C190.3(13)
C1C2C3Fe1-59.9(7) C23C19C20Fe260.0(8)
C1C2C3C4-0.9(11) C23C19C20C210.6(13)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3103_twin1_hklf4.
AtomxyzU(eq)
H131413011211750
H245005089174546
H1A-2340(130)5860(90)2280(30)10(20)
H3-26036628126830
H4-2444567942335
H5262423045027
H64199654184541
H729237915148341
H81558885107450
H9-209817717848
H10230666774155
H11A696789207330
H11B12865578213430
H12A4334863293561
H12B-15795024307961
H12C-4066219297361
H13A-23894023189249
H13B-25423699246849
H13C-6943510221749
H154917359744436
H1647541679-9038
H17274712228935
H1816691075107636
H1963042001185740
H2082152563115436
H21823373556536
H226392-95989747
H235179-194171240

Experimental

Single crystals of C23H28ClFe2NO2Si [3103_twin1_hklf4] 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 [3103_twin1_hklf4]

Crystal Data for C23H28ClFe2NO2Si (=525.70 g/mol): monoclinic, space group P21/c (no. 14), a = 7.5429(5) Å, b = 10.7933(6) Å, c = 26.917(2) Å, β = 93.719(6)°, = 2186.7(2) Å3, Z = 4, T = 173 K, μ(MoKα) = 1.525 mm-1, Dcalc = 1.597 g/cm3, 5183 reflections measured (4.842° ≤ 2Θ ≤ 53.998°), 5183 unique (Rint = ?, Rsigma = 0.0494) which were used in all calculations. The final R1 was 0.0869 (I > 2σ(I)) and wR2 was 0.2450 (all data).

Refinement model description

Number of restraints - 6, number of constraints - unknown.

Details:

1. Twinned data refinement
Scales: 0.733(2) 0.267(2)
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, All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C21) ≈ Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
4.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
4.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)
4.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
4.d Idealised tetrahedral OH refined as rotating group:
O1(H1), O2(H2)

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