B-IncStrDB

Theoretical basis (to understand - for the) structural features and trends in the reactivity of thiosemicarbazonecopper(II) complexes. The case of the perchlorate - copper(II) system.

Authors:

Gil-Garcia, Ruben; Madariaga, Gotzon; Jimenez-Perez, Alondra; Herran-Torres,Ignacio; Gago-Gonzalez, Adrian; Ugalde, Maria; Januskaitis, Vaidas; Barrera-Garcia, Joaquin; Insausti, Maite; Galletero, Maria S.; Borras, Joaquin; Cuevas, Jose Vicente; Pedrido, Rosa; Gomez-Saiz, Patricia; Lezama, Luis; Garcia-Tojal, Javier

Journal:

CrystEngComm 25 2213-2226 (2023)

DOI:

https://doi.org/10.1039/d3ce00119a

B-IncStrDB ID: R50CsLsDyhg Entry date: 2022-11-10 Last revision: 2023-05-01

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I

Chemical data

Structural Formula Sum: C8 H8 Cl Cu N5 O4 S2 [ Help ]

Formula moiety: C8 H8 Cu N5 S2, Cl O4 [ Help ]

Formula weight: 401.3 Da [ Help ]

Crystallographic data and experimental details

Crystal system: monoclinic [ Help ]

Superspace group name: C2/m(α0γ)0s [ Help ]

Symmetry operations of the superspace group: (Show/hide table) [ Help ]

Operation code	Operation in algebraic form
1	x1,x2,x3,x4
2	-x1,x2,-x3,-x4+1/2
3	-x1,-x2,-x3,-x4
4	x1,-x2,x3,x4+1/2
5	x1+1/2,x2+1/2,x3,x4
6	-x1+1/2,x2+1/2,-x3,-x4+1/2
7	-x1+1/2,-x2+1/2,-x3,-x4
8	x1+1/2,-x2+1/2,x3,x4+1/2

a: 14.950(5) Å [ Help ]

b: 6.5697(17) Å [ Help ]

c: 15.010(5) Å [ Help ]

α: 90 ° [ Help ]

β: 106.96(2) ° [ Help ]

γ: 90 ° [ Help ]

Volume: 1410.1(7) Å³ [ Help ]

Modulation dimension: 1 [ Help ]

Measured independent wave vectors: (Show/hide table) [ Help ]

Wave vector id	q_x	q_y	q_z
1	-0.614888	0.000000	0.345313

Z: 4 [ Help ]

Cell determination reflection Nb.: 1520 [ Help ]

θ(min) for cell determination: 2.73 ° [ Help ]

θ(max) for cell determination: 24.12 ° [ Help ]

Cell measurement temperature: 293(2) K [ Help ]

μ: 2.056 mm^-1 [ Help ]

Absorption correction type: integration [ Help ]

Minimum transmission factor: 0.8111 [ Help ]

Maximum transmission factor: 0.9355 [ Help ]

Refinement details

Total nb. of reflections: 4656 [ Help ]

Nb. of observed reflections: 1389 [ Help ]

Intense reflections threshold: I>2.5σ(I) [ Help ]

Refinement based on: Fsqd [ Help ]

R(obs): 0.1122 [ Help ]

wR(obs): 0.1883 [ Help ]

R(all): 0.2814 [ Help ]

wR(all): 0.2220 [ Help ]

S(all): 1.7008 [ Help ]

S(obs): 2.7083 [ Help ]

Nb. of reflections: 4656 [ Help ]

Nb. of parameters: 113 [ Help ]

Number of restraints: 4 [ Help ]

Number of constraints: 17 [ Help ]

Weighting scheme: sigma [ Help ]

Weighting scheme remarks: w=1/(σ²(I)+0.0004I²) [ Help ]

Refinement of hydrogen atoms: constr [ Help ]

Δ/σ(max): 0.0005 [ Help ]

Δ/σ(mean): 0.0000 [ Help ]

Δρ(max): 1.64 e_Å^-3 [ Help ]

Δρ(min): -1.91 e_Å^-3 [ Help ]

Extinction method: none [ Help ]

Structural Information

Average Structure: (Show/hide table) [ Help ]

Atom site label	Atom symbol	x	y	z	ADP type	Uiso/equiv	Symmetry multiplicity	Occupancy	Coords from (d)iffraction or (c)alculated	Coords restraints or constraints	Disordered cluster	Disordered group
Cu1	Cu	0.22560(7)	0.5	0.14679(7)	Uani	0.0499(4)	4	1	d	.	.	.
S1	S	0.06735(19)	0.5	0.12702(18)	Uani	0.0499(8)	4	1	d	.	.	.
S2	S	0.2352(2)	0.5	-0.16011(19)	Uani	0.0546(19)	4	1	d	.	.	.
N1	N	0.3661(5)	0.5	0.2017(5)	Uani	0.0555(8)	4	1	d	.	.	.
N2	N	0.2354(5)	0.5	0.2784(5)	Uani	0.0476(7)	4	1	d	.	.	.
N3	N	0.1570(5)	0.5	0.3054(5)	Uani	0.0446(10)	4	1	d	.	.	.
H3n	H	0.160399	0.5	0.363643	Uani	0.0430(13)	4	1	d	.	.	.
N4	N	0.0005(5)	0.5	0.2719(5)	Uani	0.0460(18)	4	1	d	.	.	.
H4n2	H	0.0069(8)	0.5	0.3307(5)	Uani	0.043(2)	4	1	d	.	.	.
H4n1	H	-0.0545(5)	0.5	0.2327(8)	Uani	0.049(2)	4	1	d	.	.	.
N5	N	0.2202(5)	0.5	0.0183(5)	Uani	0.0521(7)	4	1	d	.	.	.
C1	C	0.4310(6)	0.5	0.1608(7)	Uani	0.0604(11)	4	1	d	.	.	.
H1	H	0.412334	0.5	0.096025	Uani	0.0591(11)	4	1	d	.	.	.
C2	C	0.5251(7)	0.5	0.2050(7)	Uani	0.069(2)	4	1	d	.	.	.
H2	H	0.569311	0.5	0.172456	Uani	0.074(2)	4	1	d	.	.	.
C3	C	0.5487(7)	0.5	0.2963(8)	Uani	0.073(3)	4	1	d	.	.	.
H3	H	0.612041	0.5	0.328717	Uani	0.081(4)	4	1	d	.	.	.
C4	C	0.4855(6)	0.5	0.3470(7)	Uani	0.065(2)	4	1	d	.	.	.
H4	H	0.504003	0.5	0.411724	Uani	0.068(3)	4	1	d	.	.	.
C5	C	0.3947(7)	0.5	0.2959(6)	Uani	0.0569(14)	4	1	d	.	.	.
C6	C	0.3164(6)	0.5	0.3353(6)	Uani	0.0507(12)	4	1	d	.	.	.
H6	H	0.325645	0.5	0.399279	Uani	0.0504(17)	4	1	d	.	.	.
C7	C	0.0751(7)	0.5	0.2417(6)	Uani	0.0460(11)	4	1	d	.	.	.
C8	C	0.2260(6)	0.5	-0.0549(6)	Uani	0.0532(11)	4	1	d	.	.	.
Cl1	Cl	0.339(2)	-0.002(7)	0.4496(17)	Uani	0.0535(13)	8	0.5	d	.	.	.
O1	O	0.298(3)	-0.132(10)	0.490(4)	Uani	0.207(9)	8	0.5	d	.	.	.
O2	O	0.279(3)	0.092(10)	0.379(3)	Uani	0.194(9)	8	0.5	d	.	.	.
O3	O	0.394(3)	-0.103(10)	0.408(3)	Uani	0.173(9)	8	0.5	d	.	.	.
O4	O	0.384(4)	0.138(10)	0.516(3)	Uani	0.098(9)	8	0.5	d	.	.	.

ADP components: (Show/hide table) [ Help ]

Atom site label	Atom site symbol	U11	U22	U33	U12	U13	U23
Cu1	Cu	0.0478(6)	0.0692(9)	0.0359(5)	0	0.0173(4)	0
S1	S	0.0481(6)	0.074(2)	0.0317(9)	0	0.0180(5)	0
S2	S	0.064(2)	0.066(5)	0.0436(6)	0	0.0319(10)	0
N1	N	0.0479(6)	0.074(2)	0.0461(7)	0	0.0160(5)	0
N2	N	0.0521(9)	0.0573(17)	0.0344(5)	0	0.0144(5)	0
N3	N	0.0556(12)	0.049(2)	0.0319(7)	0	0.0167(7)	0
H3n	H	0.0608(17)	0.039(3)	0.0318(8)	0	0.0170(9)	0
N4	N	0.0566(13)	0.053(5)	0.0344(17)	0	0.0227(13)	0
H4n2	H	0.0620(18)	0.040(6)	0.0349(18)	0	0.0246(16)	0
H4n1	H	0.0547(12)	0.064(5)	0.037(2)	0	0.0238(13)	0
N5	N	0.0499(9)	0.0739(17)	0.0380(5)	0	0.0216(5)	0
C1	C	0.0478(7)	0.081(3)	0.0555(12)	0	0.0196(7)	0
H1	H	0.0491(8)	0.078(3)	0.0555(12)	0	0.0237(8)	0
C2	C	0.0477(6)	0.093(6)	0.0679(19)	0	0.0186(8)	0
H2	H	0.0483(7)	0.099(7)	0.077(3)	0	0.0230(10)	0
C3	C	0.0489(7)	0.098(8)	0.0673(19)	0	0.0115(9)	0
H3	H	0.0493(7)	0.112(11)	0.077(2)	0	0.0093(10)	0
C4	C	0.0519(9)	0.084(7)	0.0555(12)	0	0.0079(8)	0
H4	H	0.0560(13)	0.083(10)	0.0554(12)	0	0.0039(10)	0
C5	C	0.0506(8)	0.072(4)	0.0462(7)	0	0.0114(6)	0
C6	C	0.0543(11)	0.058(3)	0.0382(5)	0	0.0113(5)	0
H6	H	0.0595(16)	0.051(5)	0.0376(5)	0	0.0096(6)	0
C7	C	0.0527(10)	0.058(3)	0.0319(10)	0	0.0189(8)	0
C8	C	0.0542(14)	0.073(3)	0.0400(5)	0	0.0252(6)	0
Cl1	Cl	0.051(3)	0.081(2)	0.0330(12)	-0.018(2)	0.0193(13)	-0.006(2)
O1	O	0.416(16)	0.111(10)	0.188(13)	-0.104(11)	0.238(12)	-0.036(9)
O2	O	0.225(13)	0.209(19)	0.071(8)	0.026(13)	-0.076(8)	0.003(10)
O3	O	0.078(14)	0.281(13)	0.179(15)	-0.058(11)	0.069(13)	-0.171(10)
O4	O	0.078(17)	0.135(15)	0.064(11)	-0.002(14)	-0.004(11)	-0.051(11)

Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): (Show/hide table) [ Help ]

Wave vector code	q_1
1	1

Occupation crenel coefficients: (Show/hide table) [ Help ]

Atom site label	Center (x0)	Width
Cl1	0.2229	0.5
O1	0.2622	0.5
O2	0.2352	0.5
O3	0.1742	0.5
O4	0.2179	0.5

Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]

Modulation code	Atom site label	Displacement axis	Wave vector code
Cu1y1	Cu1	y	1
S1y1	S1	y	1
S2y1	S2	y	1
N1y1	N1	y	1
N2y1	N2	y	1
N3y1	N3	y	1
H3ny1	H3n	y	1
N4y1	N4	y	1
H4n2y1	H4n2	y	1
H4n1y1	H4n1	y	1
N5y1	N5	y	1
C1y1	C1	y	1
H1y1	H1	y	1
C2y1	C2	y	1
H2y1	H2	y	1
C3y1	C3	y	1
H3y1	H3	y	1
C4y1	C4	y	1
H4y1	H4	y	1
C5y1	C5	y	1
C6y1	C6	y	1
H6y1	H6	y	1
C7y1	C7	y	1
C8y1	C8	y	1
Cl1x1	Cl1	x	1
Cl1y1	Cl1	y	1
Cl1z1	Cl1	z	1
O1x1	O1	x	1
O1y1	O1	y	1
O1z1	O1	z	1
O2x1	O2	x	1
O2y1	O2	y	1
O2z1	O2	z	1
O3x1	O3	x	1
O3y1	O3	y	1
O3z1	O3	z	1
O4x1	O4	x	1
O4y1	O4	y	1
O4z1	O4	z	1

Displacive (translational) Fourier coefficients: (Show/hide table) [ Help ]

Modulation code	Cosine coefficient	Sine coefficient
Cu1y1	-0.0099(3)	0.0368(3)
S1y1	-0.0271(5)	0.0464(5)
S2y1	0.0298(7)	0.0116(7)
N1y1	-0.0122(5)	0.0304(5)
N2y1	-0.0304(4)	0.0325(4)
N3y1	-0.0429(5)	0.0289(5)
H3ny1	-0.0504(5)	0.0213(5)
N4y1	-0.0611(7)	0.0218(7)
H4n2y1	-0.0654(8)	0.0106(8)
H4n1y1	-0.0661(8)	0.0219(9)
N5y1	0.0099(4)	0.0327(4)
C1y1	-0.0076(6)	0.0274(6)
H1y1	-0.0009(6)	0.0233(6)
C2y1	-0.0131(9)	0.0322(9)
H2y1	-0.0105(10)	0.0329(10)
C3y1	-0.0223(10)	0.0377(10)
H3y1	-0.0240(12)	0.0443(12)
C4y1	-0.0296(9)	0.0346(9)
H4y1	-0.0380(10)	0.0353(10)
C5y1	-0.0245(6)	0.0315(6)
C6y1	-0.0334(5)	0.0296(5)
H6y1	-0.0422(6)	0.0256(6)
C7y1	-0.0450(5)	0.0336(5)
C8y1	0.0198(5)	0.0257(5)
Cl1x1	-0.0034(11)	0.015(4)
Cl1y1	-0.0388(14)	-0.011(9)
Cl1z1	0.0019(9)	0.002(3)
O1x1	-0.005(2)	0.025(5)
O1y1	-0.040(4)	-0.028(12)
O1z1	0.0011(18)	0.009(5)
O2x1	-0.0076(14)	0.008(5)
O2y1	-0.046(4)	-0.043(16)
O2z1	0.0011(13)	-0.003(4)
O3x1	0.007(2)	0.022(5)
O3y1	-0.027(5)	0.009(13)
O3z1	0.0050(17)	0.006(4)
O4x1	-0.0085(17)	0.005(6)
O4y1	-0.030(4)	0.014(14)
O4z1	0.0003(15)	-0.005(5)