Chlorido­tetra­kis­(imidazole)­copper(II) chloride. Corrigendum

Ting Bin Li; Ya Li Hu; Ji Kun Li; Guo Fang He

doi:10.1107/S2056989021002267

. 2021 Mar 31;77(Pt 4):450–451. doi: 10.1107/S2056989021002267

Chloridotetrakis(imidazole)copper(II) chloride. Corrigendum

Ting Bin Li ^a,^*, Ya Li Hu ^a, Ji Kun Li ^a, Guo Fang He ^a

PMCID: PMC8025866 PMID: 33939780

Corrigendum to Acta Cryst. (2007), E63, m2536.

Abstract

In the article by Li et al. [Acta Cryst. (2007), E63, m2536], four imidazole H atoms are missing in the refinement.<!?tpb=20pt>

The structure of chloridotetrakis(imidazole)copper(II) chloride, reported in the article by Li et al. (2007 ▸), has been rerefined to include four missing imidazole H atoms. The crystal was twinned by pseudomerohedry, which was dealt with using standard SHELXL methods (TWIN and BASF commands). The revised crystal data, data collection and structure refinement details are summarized in Table 1 ▸ and the revised chemical drawing is shown in Fig. 1 ▸.<!?tpb=-40pt>

Table 1. Experimental details.

Crystal data
Chemical formula	[CuCl(C₃H₄N₂)₄]Cl
M _r	406.77
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	8.8662 (3), 13.3199 (4), 13.9190 (4)
β (°)	90.042 (1)
V (Å³)	1643.79 (9)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	1.67
Crystal size (mm)	0.15 × 0.12 × 0.10

Data collection
Diffractometer	Bruker CCD
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 ▸)
T _min, T _max	0.788, 0.851
No. of measured, independent and observed [I > 2σ(I)] reflections	18819, 3317, 2798
R _int	0.039
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F ² > 2σ(F ²)], wR(F ²), S	0.026, 0.057, 0.94
No. of reflections	3317
No. of parameters	209
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.25, −0.37

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Computer programs: SMART (Siemens, 1996 ▸), SAINT (Siemens, 1996 ▸), SHELXT (Sheldrick, 2015a ▸) and SHELXL2018 (Sheldrick, 2015b ▸).

Chemical scheme for chloridotetrakis(imidazole)copper(II) chloride.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989021002267/me6126sup1.cif

e-77-00450-sup1.cif^{(572.3KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989021002267/me6126Isup2.hkl

e-77-00450-Isup2.hkl^{(264.9KB, hkl)}

CCDC reference: 2066475

Additional supporting information: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Crystal data

[CuCl(C₃H₄N₂)₄]Cl	F(000) = 828
M_r = 406.77	D_x = 1.644 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 8.8662 (3) Å	Cell parameters from 8636 reflections
b = 13.3199 (4) Å	θ = 2.7–27.4°
c = 13.9190 (4) Å	µ = 1.67 mm⁻¹
β = 90.042 (1)°	T = 293 K
V = 1643.79 (9) Å³	Block, blue
Z = 4	0.15 × 0.12 × 0.10 mm

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Data collection

Bruker CCD diffractometer	3317 independent reflections
Radiation source: fine-focus sealed-tube	2798 reflections with I > 2σ(I)
Detector resolution: 9.1 pixels mm^-1	R_int = 0.039
φ and ω scans at fixed χ = 55°	θ_max = 27.5°, θ_min = 1.5°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −11→11
T_min = 0.788, T_max = 0.851	k = −17→17
18819 measured reflections	l = −17→17

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Refinement

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.026	Hydrogen site location: difference Fourier map
wR(F²) = 0.057	H-atom parameters constrained
S = 0.94	w = 1/[σ²(F_o²) + (0.022P)²] where P = (F_o² + 2F_c²)/3
3317 reflections	(Δ/σ)_max = 0.001
209 parameters	Δρ_max = 0.25 e Å⁻³
0 restraints	Δρ_min = −0.37 e Å⁻³

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Special details

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

Refinement. Refined as a two-component twin.

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Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

	x	y	z	U_iso*/U_eq
Cu1	0.68666 (3)	0.28667 (2)	0.37745 (2)	0.02393 (7)
N1	0.6959 (2)	0.28765 (13)	0.23419 (13)	0.0259 (4)
N2	0.6679 (2)	0.32558 (15)	0.08280 (14)	0.0348 (5)
H2N	0.636864	0.355523	0.031725	0.042*
N3	0.58536 (18)	0.15168 (11)	0.37424 (14)	0.0261 (4)
N4	0.4040 (2)	0.04018 (13)	0.37092 (16)	0.0356 (4)
H4N	0.314625	0.015090	0.369077	0.043*
N5	0.6952 (2)	0.27930 (12)	0.52089 (13)	0.0279 (4)
N6	0.6741 (3)	0.31834 (16)	0.67249 (14)	0.0378 (5)
H6N	0.649042	0.350481	0.723635	0.045*
N7	0.85774 (18)	0.38627 (12)	0.37990 (14)	0.0272 (4)
N8	1.0848 (2)	0.44900 (14)	0.37450 (16)	0.0391 (5)
H8N	1.181520	0.452439	0.371463	0.047*
C1	0.6293 (3)	0.34862 (18)	0.17279 (17)	0.0307 (5)
H1	0.564507	0.400524	0.189836	0.037*
C2	0.7649 (3)	0.24628 (19)	0.08597 (19)	0.0388 (6)
H2	0.810447	0.214439	0.034083	0.047*
C3	0.7813 (3)	0.22351 (17)	0.17973 (17)	0.0332 (6)
H3	0.841423	0.172116	0.203825	0.040*
C4	0.4387 (2)	0.13815 (16)	0.37156 (17)	0.0306 (5)
H4	0.368157	0.189789	0.370286	0.037*
C5	0.5354 (2)	−0.01236 (16)	0.3737 (2)	0.0391 (5)
H5	0.546237	−0.081805	0.374264	0.047*
C6	0.6467 (2)	0.05655 (15)	0.3755 (2)	0.0359 (5)
H6	0.749319	0.042122	0.377214	0.043*
C7	0.6409 (3)	0.34477 (18)	0.58258 (18)	0.0334 (6)
H7	0.586607	0.401851	0.565718	0.040*
C8	0.7550 (3)	0.2312 (2)	0.6690 (2)	0.0421 (7)
H8	0.793436	0.195461	0.720941	0.050*
C9	0.7680 (3)	0.20719 (18)	0.57536 (18)	0.0354 (6)
H9	0.817889	0.151193	0.551229	0.042*
C10	1.0020 (2)	0.36497 (17)	0.3752 (2)	0.0347 (5)
H10	1.041431	0.300308	0.372764	0.042*
C11	0.9878 (3)	0.52801 (17)	0.3794 (2)	0.0415 (6)
H11	1.012833	0.595805	0.380273	0.050*
C12	0.8483 (2)	0.48821 (16)	0.3828 (2)	0.0367 (5)
H12	0.759181	0.524784	0.386633	0.044*
Cl1	0.44359 (6)	0.39845 (4)	0.37917 (5)	0.03331 (12)
Cl2	1.05460 (6)	0.09206 (4)	0.37508 (5)	0.03696 (13)

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Atomic displacement parameters (Å²)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.02695 (13)	0.02467 (12)	0.02018 (13)	−0.00402 (10)	−0.00038 (13)	−0.00037 (12)
N1	0.0273 (10)	0.0266 (9)	0.0237 (10)	−0.0037 (8)	−0.0006 (8)	0.0001 (7)
N2	0.0360 (11)	0.0460 (12)	0.0225 (10)	−0.0039 (10)	−0.0034 (9)	0.0096 (9)
N3	0.0288 (9)	0.0259 (8)	0.0236 (9)	−0.0016 (7)	0.0004 (9)	−0.0013 (9)
N4	0.0293 (9)	0.0336 (10)	0.0440 (12)	−0.0093 (8)	−0.0001 (10)	−0.0009 (10)
N5	0.031 (1)	0.0302 (9)	0.0225 (10)	−0.0027 (8)	0.0000 (9)	−0.0005 (8)
N6	0.0375 (12)	0.0557 (13)	0.0202 (10)	−0.0025 (11)	0.0028 (10)	−0.0095 (9)
N7	0.0291 (9)	0.0289 (9)	0.0236 (9)	−0.0028 (7)	−0.0004 (9)	0.0008 (8)
N8	0.0235 (9)	0.0516 (11)	0.0421 (11)	−0.0108 (8)	0.0014 (11)	−0.0032 (12)
C1	0.0297 (13)	0.0338 (13)	0.0286 (13)	−0.0002 (10)	−0.0006 (10)	0.0024 (10)
C2	0.0491 (17)	0.0373 (13)	0.0301 (14)	−0.0023 (11)	0.0079 (12)	−0.0052 (11)
C3	0.0391 (15)	0.0295 (12)	0.0310 (14)	0.0038 (10)	0.0036 (11)	0.0003 (10)
C4	0.0313 (11)	0.0302 (11)	0.0303 (12)	0.0012 (9)	−0.0010 (12)	0.0011 (10)
C5	0.0376 (12)	0.0234 (10)	0.0563 (15)	−0.0005 (9)	−0.0038 (14)	0.0010 (13)
C6	0.0296 (11)	0.0304 (10)	0.0477 (14)	0.0029 (8)	0.0006 (13)	−0.0008 (13)
C7	0.0325 (14)	0.0356 (13)	0.0321 (13)	−0.0019 (10)	−0.0009 (10)	−0.0044 (10)
C8	0.0417 (15)	0.0546 (17)	0.0299 (15)	0.0018 (13)	−0.0061 (12)	0.0089 (12)
C9	0.0389 (14)	0.0367 (13)	0.0306 (14)	0.0048 (11)	−0.0027 (11)	0.0012 (10)
C10	0.0337 (12)	0.0314 (11)	0.0390 (13)	−0.0017 (9)	−0.0002 (12)	−0.0019 (12)
C11	0.0449 (14)	0.0307 (12)	0.0489 (15)	−0.0092 (10)	0.0008 (14)	0.0005 (13)
C12	0.0337 (12)	0.0289 (11)	0.0476 (14)	0.0013 (9)	0.0003 (13)	0.0008 (12)
Cl1	0.0305 (3)	0.0333 (3)	0.0362 (3)	0.0070 (2)	−0.0006 (3)	−0.0032 (3)
Cl2	0.0329 (3)	0.0478 (3)	0.0302 (3)	−0.0087 (2)	0.0001 (3)	−0.0025 (3)

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Geometric parameters (Å, º)

Cu1—N1	1.9959 (18)	N7—C12	1.361 (3)
Cu1—N5	2.0002 (18)	N8—C10	1.338 (3)
Cu1—N3	2.0104 (16)	N8—C11	1.361 (3)
Cu1—N7	2.0154 (16)	N8—H8N	0.8600
Cu1—Cl1	2.6195 (5)	C1—H1	0.9300
N1—C1	1.318 (3)	C2—C3	1.348 (3)
N1—C3	1.371 (3)	C2—H2	0.9300
N2—C1	1.334 (3)	C3—H3	0.9300
N2—C2	1.363 (3)	C4—H4	0.9300
N2—H2N	0.8600	C5—C6	1.348 (3)
N3—C4	1.313 (3)	C5—H5	0.9300
N3—C6	1.379 (2)	C6—H6	0.9300
N4—C4	1.341 (3)	C7—H7	0.9300
N4—C5	1.360 (3)	C8—C9	1.347 (4)
N4—H4N	0.8600	C8—H8	0.9300
N5—C7	1.315 (3)	C9—H9	0.9300
N5—C9	1.383 (3)	C10—H10	0.9300
N6—C7	1.333 (3)	C11—C12	1.346 (3)
N6—C8	1.366 (3)	C11—H11	0.9300
N6—H6N	0.8600	C12—H12	0.9300
N7—C10	1.312 (3)

N1—Cu1—N5	174.86 (7)	N1—C1—H1	124.7
N1—Cu1—N3	90.12 (7)	N2—C1—H1	124.7
N5—Cu1—N3	89.71 (7)	C3—C2—N2	105.9 (2)
N1—Cu1—N7	88.92 (8)	C3—C2—H2	127.1
N5—Cu1—N7	89.28 (8)	N2—C2—H2	127.1
N3—Cu1—N7	157.71 (7)	C2—C3—N1	109.6 (2)
N1—Cu1—Cl1	92.27 (6)	C2—C3—H3	125.2
N5—Cu1—Cl1	92.84 (6)	N1—C3—H3	125.2
N3—Cu1—Cl1	98.11 (5)	N3—C4—N4	111.18 (19)
N7—Cu1—Cl1	104.18 (5)	N3—C4—H4	124.4
C1—N1—C3	105.83 (19)	N4—C4—H4	124.4
C1—N1—Cu1	129.29 (16)	C6—C5—N4	106.12 (18)
C3—N1—Cu1	124.85 (15)	C6—C5—H5	126.9
C1—N2—C2	108.0 (2)	N4—C5—H5	126.9
C1—N2—H2N	126.0	C5—C6—N3	109.66 (19)
C2—N2—H2N	126.0	C5—C6—H6	125.2
C4—N3—C6	105.36 (17)	N3—C6—H6	125.2
C4—N3—Cu1	124.45 (14)	N5—C7—N6	110.9 (2)
C6—N3—Cu1	130.19 (14)	N5—C7—H7	124.5
C4—N4—C5	107.68 (18)	N6—C7—H7	124.5
C4—N4—H4N	126.2	C9—C8—N6	106.4 (2)
C5—N4—H4N	126.2	C9—C8—H8	126.8
C7—N5—C9	105.9 (2)	N6—C8—H8	126.8
C7—N5—Cu1	127.25 (17)	C8—C9—N5	109.0 (2)
C9—N5—Cu1	126.77 (15)	C8—C9—H9	125.5
C7—N6—C8	107.9 (2)	N5—C9—H9	125.5
C7—N6—H6N	126.1	N7—C10—N8	110.73 (19)
C8—N6—H6N	126.1	N7—C10—H10	124.6
C10—N7—C12	106.09 (18)	N8—C10—H10	124.6
C10—N7—Cu1	126.20 (14)	C12—C11—N8	106.1 (2)
C12—N7—Cu1	127.67 (14)	C12—C11—H11	126.9
C10—N8—C11	107.46 (18)	N8—C11—H11	126.9
C10—N8—H8N	126.3	C11—C12—N7	109.6 (2)
C11—N8—H8N	126.3	C11—C12—H12	125.2
N1—C1—N2	110.6 (2)	N7—C12—H12	125.2

C3—N1—C1—N2	0.4 (3)	C9—N5—C7—N6	−0.3 (3)
Cu1—N1—C1—N2	178.33 (16)	Cu1—N5—C7—N6	−176.65 (17)
C2—N2—C1—N1	−0.4 (3)	C8—N6—C7—N5	0.3 (3)
C1—N2—C2—C3	0.3 (3)	C7—N6—C8—C9	−0.1 (3)
N2—C2—C3—N1	0.0 (3)	N6—C8—C9—N5	−0.1 (3)
C1—N1—C3—C2	−0.2 (3)	C7—N5—C9—C8	0.2 (3)
Cu1—N1—C3—C2	−178.27 (18)	Cu1—N5—C9—C8	176.59 (19)
C6—N3—C4—N4	−0.1 (3)	C12—N7—C10—N8	−0.4 (3)
Cu1—N3—C4—N4	−179.35 (16)	Cu1—N7—C10—N8	177.33 (16)
C5—N4—C4—N3	0.2 (3)	C11—N8—C10—N7	0.3 (3)
C4—N4—C5—C6	−0.3 (3)	C10—N8—C11—C12	−0.1 (3)
N4—C5—C6—N3	0.3 (3)	N8—C11—C12—N7	−0.1 (3)
C4—N3—C6—C5	−0.1 (3)	C10—N7—C12—C11	0.3 (3)
Cu1—N3—C6—C5	179.09 (19)	Cu1—N7—C12—C11	−177.3 (2)

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Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···Cl2ⁱ	0.86	2.40	3.251 (2)	169
N4—H4N···Cl2ⁱⁱ	0.86	2.52	3.1742 (19)	133
N6—H6N···Cl2ⁱⁱⁱ	0.86	2.39	3.241 (2)	168
N8—H8N···Cl1^iv	0.86	2.43	3.2523 (19)	159

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Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) x−1, y, z; (iii) x−1/2, −y+1/2, z+1/2; (iv) x+1, y, z.

References

Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3–10. [DOI] [PMC free article] [PubMed]
Li, T. B., Hu, Y. L., Li, J. K. & He, G. F. (2007). Acta Cryst. E63, m2536.
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3–8.
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3–8.
Siemens (1996). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989021002267/me6126sup1.cif

e-77-00450-sup1.cif^{(572.3KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989021002267/me6126Isup2.hkl

e-77-00450-Isup2.hkl^{(264.9KB, hkl)}

CCDC reference: 2066475

Additional supporting information: crystallographic information; 3D view; checkCIF report

[bb1] Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3–10. [DOI] [PMC free article] [PubMed]

[bb2] Li, T. B., Hu, Y. L., Li, J. K. & He, G. F. (2007). Acta Cryst. E63, m2536.

[bb3] Sheldrick, G. M. (2015a). Acta Cryst. A71, 3–8.

[bb4] Sheldrick, G. M. (2015b). Acta Cryst. C71, 3–8.

[bb5] Siemens (1996). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

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Chloridotetrakis(imidazole)copper(II) chloride. Corrigendum

Ting Bin Li

Ya Li Hu

Ji Kun Li

Guo Fang He

Abstract

Table 1. Experimental details.

Figure 1.

Supplementary Material

supplementary crystallographic information

Crystal data

Data collection

Refinement

Special details

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

Atomic displacement parameters (Å²)

Geometric parameters (Å, º)

Hydrogen-bond geometry (Å, º)

References

Associated Data

Supplementary Materials

ACTIONS

PERMALINK

RESOURCES

Cite

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PERMALINK

Chlorido­tetra­kis­(imidazole)­copper(II) chloride. Corrigendum

Ting Bin Li

Ya Li Hu

Ji Kun Li

Guo Fang He

Abstract

Table 1. Experimental details.

Figure 1.

Supplementary Material

supplementary crystallographic information

Crystal data

Data collection

Refinement

Special details

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

Atomic displacement parameters (Å2)

Geometric parameters (Å, º)

Hydrogen-bond geometry (Å, º)

References

Associated Data

Supplementary Materials

ACTIONS

PERMALINK

RESOURCES

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Chloridotetrakis(imidazole)copper(II) chloride. Corrigendum

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

Atomic displacement parameters (Å²)