exp_311

Table 1 Crystal data and structure refinement for exp_311.
Identification code exp_311
Empirical formula C6H30Cl3.5CoN6Na0.5O3
Formula weight 428.86
Temperature/K 293(2)
Crystal system trigonal
Space group P-3c1
a/Å 11.4290(2)
b/Å 11.4290(2)
c/Å 15.5815(2)
α/° 90
β/° 90
γ/° 120
Volume/Å3 1762.61(7)
Z 4
ρcalcg/cm3 1.616
μ/mm‑1 1.530
F(000) 896.0
Crystal size/mm3 0.385 × 0.289 × 0.217
Radiation Mo Kα (λ = 0.71073)
2Θ range for data collection/° 5.228 to 61.77
Index ranges -16 ≤ h ≤ 16, -16 ≤ k ≤ 16, -22 ≤ l ≤ 22
Reflections collected 65362
Independent reflections 1860 [Rint = 0.0274, Rsigma = 0.0086]
Data/restraints/parameters 1860/0/99
Goodness-of-fit on F2 1.057
Final R indexes [I>=2σ (I)] R1 = 0.0267, wR2 = 0.0716
Final R indexes [all data] R1 = 0.0312, wR2 = 0.0736
Largest diff. peak/hole / e Å-3 0.48/-0.78

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for exp_311. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Co13333.336666.678815.0(2)17.57(9)
Cl1-1024.3(4)5102.3(4)8748.3(2)34.23(11)
Cl2001000054.6(3)
Na100750054.2(5)
N12998.1(13)5111.7(12)9531.8(8)24.4(2)
N21859.4(13)5338.1(13)8095.5(8)27.3(2)
O11992.9(18)1108.1(17)8437.6(12)59.4(4)
C11722.2(16)3907.9(15)9257.3(10)30.2(3)
C21642.0(17)3974.4(16)8296.6(10)31.6(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for exp_311. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Co119.28(11)19.28(11)14.13(14)009.64(5)
Cl132.16(19)38.3(2)27.58(18)-2.44(13)2.03(13)14.08(15)
Cl256.8(5)56.8(5)50.2(7)0028.4(2)
Na151.5(7)51.5(7)59.6(13)0025.8(4)
N128.8(6)24.8(5)20.6(5)1.1(4)-1.4(4)14.1(5)
N227.7(6)29.6(6)22.2(5)-2.6(4)-5.3(4)12.6(5)
O152.9(9)48.3(9)68.0(10)-7.3(8)6.9(8)18.6(8)
C131.7(7)22.5(6)30.0(7)1.8(5)2.5(5)8.9(5)
C234.2(7)24.6(6)28.8(7)-6.7(5)-4.5(6)9.3(6)

 

Table 4 Bond Lengths for exp_311.
AtomAtomLength/Å AtomAtomLength/Å
Co1N111.9677(12) Na1O142.4579(19)
Co1N121.9677(12) Na1O152.4579(19)
Co1N11.9677(12) Na1O162.4579(19)
Co1N211.9601(12) Na1O172.4579(19)
Co1N221.9601(12) N1C11.4819(19)
Co1N21.9602(12) N2C21.484(2)
Na1O132.4579(19) C1C21.504(2)
Na1O12.4579(19)    

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

 

Table 5 Bond Angles for exp_311.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
N11Co1N1290.95(5) O14Na1O1588.29(6)
N11Co1N190.95(5) O15Na1O1688.29(6)
N12Co1N190.95(5) O15Na1O13174.04(8)
N21Co1N1174.50(5) O16Na1O187.73(9)
N22Co1N11174.50(6) O13Na1O1788.29(6)
N22Co1N1285.48(5) O16Na1O17174.04(8)
N2Co1N185.48(5) O15Na1O196.02(8)
N21Co1N1185.48(5) O13Na1O1696.02(8)
N22Co1N193.29(6) O17Na1O188.29(6)
N2Co1N1193.29(6) O14Na1O1796.02(8)
N2Co1N12174.50(5) O15Na1O1787.73(9)
N21Co1N1293.29(6) O14Na1O1387.73(9)
N21Co1N2290.53(6) O14Na1O1688.29(6)
N21Co1N290.54(6) C1N1Co1109.36(9)
N2Co1N2290.54(6) C2N2Co1108.70(9)
O13Na1O188.29(6) N1C1C2107.27(12)
O14Na1O1174.05(8) N2C2C1106.31(12)

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

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for exp_311.
AtomxyzU(eq)
H1E1740.28992.28961.9889
H2C2350(20)3860(20)8001(13)36(5)
H1A3630(20)4940(20)9450(13)37(5)
H1C1720(20)3120(20)9466(15)43(6)
H1D1040(20)3950(20)9506(13)33(5)
H2D800(20)3320(20)8100(13)40(5)
H2A1140(20)5330(20)8201(13)37(5)
H1B2910(20)5190(20)10036(15)40(6)
H2B1980(20)5470(20)7572(14)41(6)
H1F2820(40)1800(40)8520(20)92(11)

Experimental

Single crystals of C6H30Cl3.5CoN6Na0.5O3 [exp_311] were []. A suitable crystal was selected and [] on a XtaLAB Mini II diffractometer. The crystal was kept at 293(2) K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program using Intrinsic Phasing and refined with the ShelXL [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. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [exp_311]

Crystal Data for C6H30Cl3.5CoN6Na0.5O3 (=428.86 g/mol): trigonal, space group P-3c1 (no. 165), a = 11.4290(2) Å, c = 15.5815(2) Å, = 1762.61(7) Å3, Z = 4, T = 293(2) K, μ(Mo Kα) = 1.530 mm-1, Dcalc = 1.616 g/cm3, 65362 reflections measured (5.228° ≤ 2Θ ≤ 61.77°), 1860 unique (Rint = 0.0274, Rsigma = 0.0086) which were used in all calculations. The final R1 was 0.0267 (I > 2σ(I)) and wR2 was 0.0736 (all data).

Refinement model description

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

Details:

1. Fixed Uiso
At 1.5 times of:
All O(H) groups
2.a Rotating group:
O1(H1E)

This report has been created with Olex2, compiled on 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction. Please let us know if there are any errors or if you would like to have additional features.