research papers
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 Rwp = 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.
Keywords: molecular mechanics; molecular modelling; X-ray powder diffraction; thiazine; copper(II) complex.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889804024653/zm5020sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0021889804024653/zm5020sup2.rtv |
CCDC reference: 256387
Computing details top
Program(s) used to solve structure: FOX; program(s) used to refine structure: FULLPROF.
(Modelo_Polak) top
Crystal data top
C18H22CuN7O3S2·NO3 | β = 112.090 (2)° |
Mr = 574.10 | V = 2340.9 (12) Å3 |
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 |
Crystal data top
C18H22CuN7O3S2·NO3 | β = 112.090 (2)° |
Mr = 574.10 | V = 2340.9 (12) Å3 |
Monoclinic, P121/N1 | Z = 4 |
a = 20.695 (7) Å | Cu Kα radiation |
b = 8.054 (2) Å | T = 291 K |
c = 15.157 (4) Å | × × mm |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
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* |
Experimental details
Crystal data | |
Chemical formula | C18H22CuN7O3S2·NO3 |
Mr | 574.10 |
Crystal system, space group | Monoclinic, P121/N1 |
Temperature (K) | 291 |
a, b, c (Å) | 20.695 (7), 8.054 (2), 15.157 (4) |
β (°) | 112.090 (2) |
V (Å3) | 2340.9 (12) |
Z | 4 |
Radiation type | Cu Kα |
µ (mm−1) | ? |
Crystal size (mm) | × × |
Data collection | |
Diffractometer | ? |
Absorption correction | – |
No. of measured, independent and observed (?) reflections | ?, ?, ? |
Rint | ? |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? |
No. of reflections | 5233 |
No. of parameters | 54 |
No. of restraints | 13 |
Δρmax, Δρmin (e Å−3) | ?, ? |
Computer programs: FOX, FULLPROF.