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The CuI atom of the title complex, [Cu(C7H8N2S)4]Cl, is located on a \overline 4 inversion axis and has distorted tetrahedral coordination geometry, formed by four phenyl­thio­urea S atoms. Within the phenyl­thio­urea ligands, the C—N(imino) bonds [1.341 (2) Å] are significantly longer than the C—N(amino) bonds [1.316 (3) Å]. The Cl anion is located on another \overline 4 inversion axis and links with four complex cations via N—H...Cl hydrogen bonding.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401582X/cv6337sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680401582X/cv6337Isup2.hkl
Contains datablock I

CCDC reference: 248712

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.026
  • wR factor = 0.065
  • Data-to-parameter ratio = 18.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cu - S .. 20.62 su
Alert level C PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C5 PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2B ... ?
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 1957 Count of symmetry unique reflns 1028 Completeness (_total/calc) 190.37% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 929 Fraction of Friedel pairs measured 0.904 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I) top
Crystal data top
[Cu(C7H8N2S)4]ClDx = 1.386 Mg m3
Mr = 707.85Mo Kα radiation, λ = 0.71069 Å
Tetragonal, I4Cell parameters from 7866 reflections
Hall symbol: I -4θ = 2.5–26.0°
a = 11.4847 (3) ŵ = 1.00 mm1
c = 12.8612 (4) ÅT = 295 K
V = 1696.37 (8) Å3Prism, pale-yellow
Z = 20.38 × 0.26 × 0.24 mm
F(000) = 732
Data collection top
Rigaku R-AXIS RAPID
diffractometer
1957 independent reflections
Radiation source: fine-focus sealed tube1868 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
Detector resolution: 10.00 pixels mm-1θmax = 27.5°, θmin = 2.4°
ω scansh = 1414
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1414
Tmin = 0.68, Tmax = 0.78l = 1616
8326 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.039P)2 + 0.2897P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
1957 reflectionsΔρmax = 0.13 e Å3
104 parametersΔρmin = 0.21 e Å3
0 restraintsAbsolute structure: Flack (1983), 932 Friedel Pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.001 (12)
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu0.50000.00000.75000.05386 (14)
Cl0.50000.50000.50000.0527 (2)
S0.51034 (5)0.17313 (4)0.65581 (4)0.05544 (14)
N10.35821 (16)0.06011 (13)0.53791 (13)0.0517 (4)
N20.3862 (2)0.25346 (15)0.50004 (19)0.0717 (6)
C10.29141 (16)0.03378 (16)0.44721 (15)0.0473 (4)
C20.19393 (19)0.0962 (2)0.4208 (2)0.0651 (6)
H20.16790.15600.46370.078*
C30.1345 (2)0.0700 (3)0.3303 (2)0.0807 (8)
H30.07030.11450.31110.097*
C40.1688 (2)0.0199 (3)0.2694 (2)0.0857 (8)
H40.12830.03700.20860.103*
C50.2643 (3)0.0863 (3)0.2979 (2)0.0935 (10)
H50.28640.14980.25760.112*
C60.3268 (2)0.0582 (2)0.38591 (19)0.0666 (6)
H60.39250.10110.40390.080*
C70.41019 (18)0.16215 (15)0.55805 (15)0.0480 (4)
H1A0.383 (2)0.003 (3)0.575 (2)0.080*
H2A0.424 (3)0.314 (3)0.510 (3)0.080*
H2B0.345 (3)0.238 (3)0.446 (2)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu0.06454 (19)0.06454 (19)0.0325 (2)0.0000.0000.000
Cl0.0348 (2)0.0348 (2)0.0886 (7)0.0000.0000.000
S0.0771 (3)0.0434 (2)0.0458 (2)0.0088 (2)0.0116 (2)0.00645 (18)
N10.0673 (10)0.0396 (7)0.0481 (9)0.0108 (7)0.0098 (7)0.0034 (6)
N20.0946 (14)0.0458 (9)0.0746 (13)0.0247 (9)0.0329 (12)0.0174 (9)
C10.0503 (10)0.0460 (9)0.0455 (9)0.0128 (7)0.0023 (7)0.0006 (7)
C20.0533 (11)0.0559 (11)0.0860 (16)0.0036 (9)0.0096 (11)0.0098 (11)
C30.0541 (12)0.0882 (17)0.100 (2)0.0045 (12)0.0266 (13)0.0076 (16)
C40.0666 (14)0.127 (2)0.0630 (16)0.0126 (15)0.0177 (12)0.0115 (15)
C50.0809 (17)0.130 (3)0.0696 (16)0.0138 (18)0.0133 (14)0.0448 (17)
C60.0590 (11)0.0766 (14)0.0640 (13)0.0086 (10)0.0110 (10)0.0192 (11)
C70.0606 (10)0.0399 (8)0.0434 (9)0.0080 (7)0.0011 (8)0.0003 (7)
Geometric parameters (Å, º) top
Cu—S2.3313 (5)C2—C31.383 (4)
S—C71.709 (2)C2—H20.9300
N1—C71.341 (2)C3—C41.355 (4)
N1—C11.429 (2)C3—H30.9300
N1—H1A0.92 (3)C4—C51.386 (4)
N2—C71.316 (3)C4—H40.9300
N2—H2A0.83 (3)C5—C61.379 (3)
N2—H2B0.86 (3)C5—H50.9300
C1—C21.372 (3)C6—H60.9300
C1—C61.380 (3)
S—Cu—Si117.38 (2)C4—C3—C2120.6 (2)
S—Cu—Sii105.666 (10)C4—C3—H3119.7
C7—S—Cu106.57 (6)C2—C3—H3119.7
C7—N1—C1125.59 (16)C3—C4—C5119.8 (2)
C7—N1—H1A116.8 (17)C3—C4—H4120.1
C1—N1—H1A115.4 (17)C5—C4—H4120.1
C7—N2—H2A118 (2)C6—C5—C4120.0 (3)
C7—N2—H2B114 (2)C6—C5—H5120.0
H2A—N2—H2B125 (3)C4—C5—H5120.0
C2—C1—C6119.97 (19)C5—C6—C1119.7 (2)
C2—C1—N1121.97 (19)C5—C6—H6120.2
C6—C1—N1118.07 (18)C1—C6—H6120.2
C1—C2—C3119.8 (2)N2—C7—N1119.59 (18)
C1—C2—H2120.1N2—C7—S119.95 (14)
C3—C2—H2120.1N1—C7—S120.43 (14)
Symmetry codes: (i) x+1, y, z; (ii) y+1/2, x+1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···Si0.91 (3)2.53 (3)3.4284 (17)168 (2)
N2—H2A···Cl0.83 (4)2.31 (3)3.1185 (18)164 (4)
Symmetry code: (i) x+1, y, z.
 

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