Structure determination of nitrato-κO-bis[2-(2-pyridyl-κN)amino-5,6-dihydro-4H-1,3-thiazine-κN]copper(II) nitrate via molecular modelling coupled with X-ray powder diffractometry

The title copper(II) coordination compound, C₁₈H₂₂CuN₈O₆S₂ {[Cu(NO₃)(PyTz)₂]NO₃}, was synthesized in the form of small crystals unsuitable for structure determination by single-crystal X-ray diffractometry. It was therefore characterized by molecular modelling coupled with X-ray powder diffractometry [monoclinic, space group P2₁/n, a = 20.695 (7) Å, b = 8.054 (2) Å, c = 15.157 (4) Å, β = 112.09 (2)° and R_wp = 0.129]. The procedure used to resolve the structure followed direct space methods with a `Monte Carlo/parallel tempering' search algorithm, where the starting configuration was obtained by means of molecular mechanics. A final refinement was performed with the Rietveld method. Bond distances, bond angles and torsion angles were compared with those of similar compounds deposited in the Cambridge Structural Database.

Computing details

Program(s) used to solve structure: FOX; program(s) used to refine structure: FULLPROF.

Figures

(Modelo_Polak)

Crystal data

C18H22CuN7O3S2·NO3	β = 112.090 (2)°
Mr = 574.10	V = 2340.9 (12) Å^3
Monoclinic, P121/N1	Z = 4
Hall symbol: -P 2yn	Cu Kα radiation, λ = 1.54183 Å
a = 20.695 (7) Å	T = 291 K
b = 8.054 (2) Å	× × mm
c = 15.157 (4) Å

Data collection

C 111 monochromator	k = ?→?
h = ?→?	l = ?→?

Refinement

5233 reflections	13 restraints
54 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cu	0.5498 (5)	0.5485 (10)	0.2567 (5)	0.00000*
O1	0.5317 (9)	0.3986 (17)	0.1564 (14)	0.00000*
N1	0.5678 (9)	0.2693 (17)	0.1712 (14)	0.00000*
O2	0.5524 (9)	0.1604 (17)	0.1093 (14)	0.00000*
O3	0.6185 (9)	0.2468 (17)	0.2471 (14)	0.00000*
NP1	0.4580 (6)	0.666 (2)	0.1875 (11)	0.00000*
CP11	0.4034 (6)	0.687 (2)	0.2086 (11)	0.00000*
H1	0.4070 (6)	0.637 (2)	0.2781 (11)	0.00000*
CP12	0.3410 (6)	0.769 (2)	0.1492 (11)	0.00000*
H2	0.2960 (6)	0.783 (2)	0.1708 (11)	0.00000*
CP13	0.3393 (6)	0.831 (2)	0.0603 (11)	0.00000*
H3	0.2929 (6)	0.896 (2)	0.0100 (11)	0.00000*
CP14	0.4593 (6)	0.725 (2)	0.1086 (11)	0.00000*
CP15	0.4010 (6)	0.806 (2)	0.0413 (11)	0.00000*
H4	0.4034 (6)	0.854 (2)	−0.0257 (11)	0.00000*
NE1	0.5074 (15)	0.739 (6)	0.070 (3)	0.00000*
H5	0.5000 (15)	0.783 (6)	0.004 (3)	0.00000*
NT1	0.5907 (8)	0.603 (2)	0.1622 (13)	0.00000*
CT11	0.5721 (8)	0.669 (2)	0.0788 (13)	0.00000*
ST1	0.6371 (8)	0.734 (2)	0.0307 (13)	0.00000*
CT12	0.7278 (8)	0.678 (2)	0.1066 (13)	0.00000*
H6	0.7578 (8)	0.632 (2)	0.0636 (13)	0.00000*
H7	0.7558 (8)	0.786 (2)	0.1499 (13)	0.00000*
CT13	0.6656 (8)	0.582 (2)	0.2216 (13)	0.00000*
H8	0.6671 (8)	0.483 (2)	0.2742 (13)	0.00000*
H9	0.6838 (8)	0.698 (2)	0.2637 (13)	0.00000*
CT14	0.7202 (8)	0.543 (2)	0.1714 (13)	0.00000*
H10	0.7010 (8)	0.425 (2)	0.1308 (13)	0.00000*
H11	0.7732 (8)	0.515 (2)	0.2264 (13)	0.00000*
NT2	0.5854 (6)	0.6903 (17)	0.3555 (8)	0.00000*
CT21	0.5749 (6)	0.8725 (17)	0.3331 (8)	0.00000*
H12	0.5669 (6)	0.8839 (17)	0.2564 (8)	0.00000*
H13	0.5244 (6)	0.9081 (17)	0.3387 (8)	0.00000*
CT22	0.6336 (6)	0.9982 (17)	0.3883 (8)	0.00000*
H14	0.6832 (6)	0.9609 (17)	0.3803 (8)	0.00000*
H15	0.6198 (6)	1.1236 (17)	0.3549 (8)	0.00000*
ST2	0.6580 (6)	0.7965 (17)	0.5376 (8)	0.00000*
CT23	0.6197 (6)	0.6455 (17)	0.4414 (8)	0.00000*
CT24	0.6450 (6)	1.0110 (17)	0.4943 (8)	0.00000*
H16	0.6919 (6)	1.0880 (17)	0.5342 (8)	0.00000*
H17	0.5984 (6)	1.0675 (17)	0.5030 (8)	0.00000*
NE2	0.606 (2)	0.493 (4)	0.468 (2)	0.00000*
H18	0.639 (2)	0.469 (4)	0.537 (2)	0.00000*
NP2	0.5165 (10)	0.3879 (19)	0.3286 (14)	0.00000*
CP21	0.5592 (10)	0.3813 (19)	0.4160 (14)	0.00000*
CP22	0.5490 (10)	0.2713 (19)	0.4838 (14)	0.00000*
H19	0.5864 (10)	0.2678 (19)	0.5586 (14)	0.00000*
CP23	0.4898 (10)	0.1677 (19)	0.4528 (14)	0.00000*
H20	0.4788 (10)	0.0808 (19)	0.5018 (14)	0.00000*
CP24	0.4614 (10)	0.2952 (19)	0.3010 (14)	0.00000*
H21	0.4257 (10)	0.3064 (19)	0.2256 (14)	0.00000*
CP25	0.4435 (10)	0.1832 (19)	0.3557 (14)	0.00000*
H22	0.3956 (10)	0.1074 (19)	0.3261 (14)	0.00000*
NA	0.7691 (15)	0.756 (3)	0.852 (2)	0.00000*
OB	0.8304 (15)	0.719 (3)	0.883 (2)	0.00000*
OC	0.7324 (15)	0.726 (3)	0.766 (2)	0.00000*
OD	0.7439 (15)	0.823 (3)	0.905 (2)	0.00000*