As_101322_auto_mI

Submitted by:	Faik N Musayev
		Virginia Commonwealth University
Solved by:	Faik N Musayev
Sample ID:	Copper complex

R1=2.95%

Crystal Data and Experimental

Experimental. Single dull light green plate-shaped crystals of As_101322_auto_mI were Solvent: DMF:Acetonitrile:Ethanol (1:2:4). A suitable crystal 0.32×0.13×0.09  mm3 was selected and MiTeGen Microloop on an XtaLAB AFC11 (RINC): quarter-chi single diffractometer. The crystal was kept at a steady T = 100.00(10) K during data collection. The structure was solved with the ShelXT 2014/4 (Sheldrick, 2014) structure solution program using the Intrinsic Phasing solution method and by using Olex2 (Dolomanov et al., 2009) as the graphical interface. The model was refined with version 2016/6 of ShelXL 2016/6 (Sheldrick, 2015) using Least Squares minimisation.
Crystal Data. C20H26.4Cu0.8N2.4O3.2, Mr = 402.47, monoclinic, I2/a (No. 15), a = 20.15032(10) Å, b = 8.51076(4) Å, c = 28.67360(13) Å, b = 97.1815(4)°, a = g = 90°, V = 4878.79(4) Å3, T = 100.00(10) K, Z = 10, Z' = 1.25, m(Cu Ka) = 1.554, 41399 reflections measured, 4951 unique (Rint = 0.0243) which were used in all calculations. The final wR2 was 0.0832 (all data) and R1 was 0.0295 (I > 2(I)).

Compound 	As_101322_auto_mI 	
 	 	
Formula 	C20H26.4Cu0.8N2.4O3.2 	
Dcalc./ g cm-3 	1.370 	
m/mm-1 	1.554 	
Formula Weight 	402.47 	
Colour 	dull light green 	
Shape 	plate 	
Size/mm3 	0.32×0.13×0.09 	
T/K 	100.00(10) 	
Crystal System 	monoclinic 	
Space Group 	I2/a 	
a/Å 	20.15032(10) 	
b/Å 	8.51076(4) 	
c/Å 	28.67360(13) 	
a/° 	90 	
b/° 	97.1815(4) 	
g/° 	90 	
V/Å3 	4878.79(4) 	
Z 	10 	
Z' 	1.25 	
Wavelength/Å 	1.54184 	
Radiation type 	Cu Ka 	
Qmin/° 	3.107 	
Qmax/° 	74.644 	
Measured Refl. 	41399 	
Independent Refl. 	4951 	
Reflections with I > 2(I) 	4817 	
Rint 	0.0243 	
Parameters 	307 	
Restraints 	0 	
Largest Peak 	0.463 	
Deepest Hole 	-0.463 	
GooF 	1.045 	
wR2 (all data) 	0.0832 	
wR2 	0.0828 	
R1 (all data) 	0.0300 	
R1 	0.0295 	

Structure Quality Indicators
Reflections:		
Refinement:		
Experimental Extended. A dull light green plate-shaped crystal with dimensions 0.32×0.13×0.09 mm3 was MiTeGen Microloop. Data were collected using an XtaLAB AFC11 (RINC): quarter-chi single diffractometer operating at T = 100.00(10) K.
Data were measured using w scans of 0.5° per frame for 0.6/2.4 s using Cu Ka radiation. The total number of runs and images was based on the strategy calculation from the program CrysAlisPro (Rigaku, V1.171.41.122a, 2021) The maximum resolution that was achieved was Q = 74.644° (0.80 Å).
The diffraction pattern was indexed The total number of runs and images was based on the strategy calculation from the program CrysAlisPro (Rigaku, V1.171.41.122a, 2021) and the unit cell was refined using CrysAlisPro (Rigaku, V1.171.41.122a, 2021) on 29677 reflections, 72% of the observed reflections.
Data reduction, scaling and absorption corrections were performed using CrysAlisPro (Rigaku, V1.171.41.122a, 2021). The final completeness is 100.00 % out to 74.644° in Q. A multi-scan absorption correction was performed using CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021) using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.. The absorption coefficient m of this material is 1.554 mm-1 at this wavelength (l = 1.542Å) and the minimum and maximum transmissions are 0.806 and 1.000.
The structure was solved and the space group I2/a (# 15) determined by the ShelXT 2014/4 (Sheldrick, 2014) structure solution program using Intrinsic Phasing and refined by Least Squares using version 2016/6 of ShelXL 2016/6 (Sheldrick, 2015). All non-hydrogen atoms were refined anisotropically. Hydrogen atom positions were calculated geometrically and refined using the riding model. Hydrogen atom positions were calculated geometrically and refined using the riding model.

_exptl_absorpt_process_details: CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021) using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.

Table 0: Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for As_101322_auto_mI. Ueq is defined as 1/3 of the trace of the orthogonalised Uij.

Atom	x	y	z	Ueq	
Cu1	5764.4(2)	2870.0(2)	5467.1(2)	17.65(8)	
O1	6243.7(5)	4172.5(12)	5911.3(4)	21.1(2)	
O3	5387.9(5)	1684.1(12)	4924.3(4)	20.5(2)	
O2	4998.5(5)	4202.1(12)	5513.6(4)	21.8(2)	
O4	6770.1(5)	-1383.6(13)	4421.0(4)	26.2(2)	
N1	6499.5(6)	1480.0(14)	5442.8(4)	18.3(2)	
N2	6411.7(6)	422.3(14)	5066.9(4)	20.2(2)	
N3	3925.9(7)	4950.0(18)	5382.1(5)	28.6(3)	
C7	7814.7(7)	2281.8(16)	6413.6(5)	17.7(3)	
C6	8044.1(7)	3334.1(17)	6759.7(5)	18.4(3)	
C1	7045.2(7)	1419.8(16)	5736.2(5)	18.6(3)	
C3	6822.0(7)	3905.0(17)	6162.5(5)	17.4(3)	
C2	7214.7(7)	2539.8(17)	6107.1(5)	17.3(3)	
C5	7662.2(7)	4720.2(18)	6790.5(5)	20.9(3)	
C16	5819.7(7)	668.0(17)	4816.8(5)	19.4(3)	
C4	7071.4(7)	5048.1(17)	6505.3(5)	19.8(3)	
C17	5663.4(7)	-242.4(17)	4377.3(5)	20.3(3)	
C23	4432.4(7)	4089.8(18)	5283.5(5)	21.6(3)	
C8	8669.2(7)	3052.4(18)	7116.7(5)	21.2(3)	
C18	6141.4(8)	-1194.3(17)	4196.3(5)	22.0(3)	
C22	5023.9(8)	-120.5(18)	4124.4(5)	23.0(3)	
C19	5971.8(9)	-1995.4(18)	3771.8(6)	26.3(3)	
C21	4853.6(9)	-936.2(19)	3708.4(6)	27.2(3)	
C9	8446.2(8)	2781(2)	7603.6(5)	27.6(3)	
C12	6674.0(8)	6576.3(19)	6549.7(6)	26.6(3)	
C20	5333.4(9)	-1876.1(19)	3534.4(6)	28.1(3)	
C11	9062.3(8)	1605(2)	6990.0(6)	28.9(3)	
C10	9140.7(8)	4478(2)	7143.0(6)	30.4(4)	
C13	6598.0(9)	7476.1(19)	6079.6(6)	29.7(3)	
C15	5976.8(9)	6215(2)	6693.5(6)	36.4(4)	
C25	3988.4(11)	5992(2)	5786.9(7)	40.1(5)	
C24	3258.0(8)	4747(3)	5131.5(7)	43.4(5)	
C14	7028.8(12)	7663(2)	6923.5(8)	51.2(6)	
Table 0: Anisotropic Displacement Parameters (×104) As_101322_auto_mI. The anisotropic displacement factor exponent takes the form: -2p2[h2a*2 × U11+ ... +2hka* × b* × U12]

Atom	U11	U22	U33	U23	U13	U12	
Cu1	16.50(12)	16.07(12)	19.63(13)	-2.67(8)	-0.73(8)	2.23(7)	
O1	18.8(5)	17.6(5)	25.2(5)	-3.2(4)	-3.8(4)	3.6(4)	
O3	19.3(5)	19.5(5)	22.1(5)	-4.0(4)	-0.2(4)	2.1(4)	
O2	19.9(5)	22.4(5)	22.2(5)	-2.3(4)	-0.5(4)	4.4(4)	
O4	21.6(5)	24.5(6)	33.1(6)	-8.9(5)	5.6(4)	-0.9(4)	
N1	19.5(6)	14.9(5)	20.0(6)	-2.9(5)	0.7(5)	-0.4(5)	
N2	20.9(6)	16.6(6)	22.7(6)	-4.6(5)	0.9(5)	0.2(5)	
N3	23.4(6)	35.0(8)	28.2(7)	10.0(6)	6.7(5)	10.5(6)	
C7	17.8(7)	16.3(7)	19.1(7)	2.9(5)	2.9(5)	1.6(5)	
C6	18.0(6)	20.3(7)	16.5(6)	3.5(5)	0.5(5)	0.5(5)	
C1	17.5(6)	15.2(6)	23.0(7)	0.8(5)	2.4(5)	1.6(5)	
C3	18.1(6)	16.9(6)	17.0(6)	2.4(5)	1.0(5)	0.6(5)	
C2	17.6(6)	15.9(6)	18.2(6)	1.7(5)	1.6(5)	-0.5(5)	
C5	25.1(7)	19.7(7)	16.7(6)	-1.1(5)	-1.7(5)	1.0(6)	
C16	20.3(7)	15.9(6)	21.9(7)	-0.2(5)	2.4(5)	-1.0(5)	
C4	24.2(7)	17.2(7)	17.5(6)	0.5(5)	0.1(5)	2.9(6)	
C17	24.1(7)	15.8(6)	20.9(7)	-1.3(5)	2.6(6)	-2.8(6)	
C23	21.2(7)	24.1(7)	19.6(7)	3.1(6)	3.1(5)	2.1(6)	
C8	20.7(7)	22.8(7)	19.0(7)	0.7(6)	-2.2(6)	2.1(6)	
C18	24.0(7)	16.9(7)	25.7(7)	-0.9(6)	5.4(6)	-4.0(6)	
C22	25.8(7)	20.0(7)	22.7(7)	-1.3(6)	0.6(6)	0.4(6)	
C19	34.8(9)	19.6(7)	26.0(8)	-4.7(6)	9.6(7)	-2.4(6)	
C21	32.0(8)	24.5(8)	23.7(7)	-2.1(6)	-2.5(6)	-1.4(6)	
C9	27.7(8)	34.8(9)	19.0(7)	3.5(6)	-2.5(6)	4.4(7)	
C12	31.9(8)	20.9(7)	24.1(7)	-6.4(6)	-8.3(6)	8.6(6)	
C20	41.4(9)	21.7(7)	20.7(7)	-4.5(6)	2.2(7)	-4.6(7)	
C11	24.0(7)	32.3(9)	27.9(8)	-3.5(7)	-6.1(6)	9.1(7)	
C10	24.6(8)	31.6(9)	32.5(8)	2.8(7)	-6.6(6)	-3.8(7)	
C13	31.7(8)	17.7(7)	37.4(9)	2.8(7)	-4.8(7)	3.2(6)	
C15	41.2(10)	37.6(10)	31.3(9)	-1.3(7)	8.2(7)	18.6(8)	
C25	54.7(12)	34.3(9)	35.5(9)	6.0(8)	22.2(9)	20.0(9)	
C24	19.4(8)	60.2(13)	50.9(11)	30.3(10)	5.3(7)	8.4(8)	
C14	55.3(13)	35.1(10)	54.3(12)	-25.6(9)	-28.5(10)	22.9(9)	
Table 0: Bond Lengths in Å for As_101322_auto_mI.

Atom	Atom	Length/Å	
Cu1	O1	1.8646(10)	
Cu1	O3	1.9291(10)	
Cu1	O2	1.9329(10)	
Cu1	N1	1.9038(12)	
O1	C3	1.3109(17)	
O3	C16	1.2910(18)	
O2	C23	1.2480(18)	
O4	C18	1.3572(19)	
N1	N2	1.3985(16)	
N1	C1	1.2992(19)	
N2	C16	1.3293(19)	
N3	C23	1.315(2)	
N3	C25	1.453(2)	
N3	C24	1.455(2)	
C7	C6	1.373(2)	
C7	C2	1.420(2)	
C6	C5	1.417(2)	
C6	C8	1.5394(19)	
C1	C2	1.437(2)	
C3	C2	1.426(2)	
C3	C4	1.429(2)	
C5	C4	1.386(2)	
C16	C17	1.479(2)	
C4	C12	1.541(2)	
C17	C18	1.407(2)	
C17	C22	1.401(2)	
C8	C9	1.537(2)	
C8	C11	1.533(2)	
C8	C10	1.537(2)	
C18	C19	1.400(2)	
C22	C21	1.386(2)	
C19	C20	1.382(2)	
C21	C20	1.394(2)	
C12	C13	1.541(2)	
C12	C15	1.544(3)	
C12	C14	1.525(2)	

Table 0: Bond Angles in ° for As_101322_auto_mI.

Atom	Atom	Atom	Angle/°	
O1	Cu1	O3	168.55(5)	
O1	Cu1	O2	87.36(4)	
O1	Cu1	N1	93.18(5)	
O3	Cu1	O2	97.22(4)	
N1	Cu1	O3	82.80(5)	
N1	Cu1	O2	176.95(5)	
C3	O1	Cu1	128.38(9)	
C16	O3	Cu1	109.53(9)	
C23	O2	Cu1	127.12(10)	
N2	N1	Cu1	113.84(9)	
C1	N1	Cu1	126.88(10)	
C1	N1	N2	119.27(12)	
C16	N2	N1	109.46(11)	
C23	N3	C25	121.28(15)	
C23	N3	C24	121.51(16)	
C25	N3	C24	116.70(15)	
C6	C7	C2	122.01(13)	
C7	C6	C5	116.84(13)	
C7	C6	C8	123.55(13)	
C5	C6	C8	119.57(13)	
N1	C1	C2	123.82(13)	
O1	C3	C2	123.23(13)	
O1	C3	C4	118.14(12)	
C2	C3	C4	118.63(13)	
C7	C2	C1	117.43(13)	
C7	C2	C3	119.90(13)	
C3	C2	C1	122.61(13)	
C4	C5	C6	124.32(13)	
O3	C16	N2	124.24(13)	
O3	C16	C17	118.43(13)	
N2	C16	C17	117.28(13)	
C3	C4	C12	119.33(13)	
C5	C4	C3	118.11(13)	
C5	C4	C12	122.55(13)	
C18	C17	C16	122.23(13)	
C22	C17	C16	119.09(13)	
C22	C17	C18	118.66(13)	
O2	C23	N3	121.75(15)	
C9	C8	C6	108.65(12)	
C9	C8	C10	108.88(13)	
C11	C8	C6	111.81(12)	
C11	C8	C9	108.24(13)	
C11	C8	C10	108.14(13)	
C10	C8	C6	111.04(12)	
O4	C18	C17	122.33(13)	
O4	C18	C19	117.84(14)	
C19	C18	C17	119.83(14)	
C21	C22	C17	121.40(15)	
C20	C19	C18	120.24(15)	
C22	C21	C20	119.17(15)	
C4	C12	C13	110.06(13)	
C4	C12	C15	110.71(14)	
C13	C12	C15	109.77(13)	
C14	C12	C4	111.56(13)	
C14	C12	C13	107.45(16)	
C14	C12	C15	107.19(16)	
C19	C20	C21	120.68(15)	

Table 0: Hydrogen Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for As_101322_auto_mI. Ueq is defined as 1/3 of the trace of the orthogonalised Uij.

Atom	x	y	z	Ueq	
H4	6804.94	-912.13	4680.3	39	
H7	8064.91	1352.81	6378.2	21	
H1	7349.86	586.91	5703.61	22	
H5	7821.66	5474.2	7022.07	25	
H23	4365.58	3363.71	5030.34	26	
H22	4700.16	535.37	4240.65	28	
H19	6296.75	-2623.45	3646.41	32	
H21	4415.53	-856.11	3543.83	33	
H9A	8198.08	3700.79	7692.77	41	
H9B	8840.4	2616.95	7835.46	41	
H9C	8157.74	1850.93	7593.14	41	
H20	5220.27	-2440.28	3249.65	34	
H11A	8780.75	667.85	6994.97	43	
H11B	9462.77	1482.63	7218.86	43	
H11C	9194.78	1739.36	6674.95	43	
H10A	9304.77	4626.13	6838.36	46	
H10B	9520.28	4296.61	7385.83	46	
H10C	8897.8	5419.68	7221.54	46	
H13A	7038.67	7610.6	5974.04	45	
H13B	6399.78	8509.39	6122.6	45	
H13C	6307.21	6880.49	5843.21	45	
H15A	5733.14	5516.71	6459.98	55	
H15B	5726.83	7197.19	6709.79	55	
H15C	6027.83	5702.21	7001.86	55	
H25A	3772.81	5510.04	6039.58	60	
H25B	3771.56	6997.01	5697.85	60	
H25C	4462.86	6169.93	5896.1	60	
H24A	3271.92	3971.04	4880.41	65	
H24B	3097.11	5753.24	4994.75	65	
H24C	2955.07	4380.2	5350.52	65	
H14A	7079.79	7128.73	7228.56	77	
H14B	6763.74	8621.39	6942.63	77	
H14C	7470.97	7938.9	6839.5	77	

Citations
O.V. Dolomanov and L.J. Bourhis and R.J. Gildea and J.A.K. Howard and H. Puschmann, Olex2: A complete structure solution, refinement and analysis program, J. Appl. Cryst., (2009), 42, 339-341.