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Article

Synthesis, Structures, and Magnetism of Four One-Dimensional Complexes Using [Ni(CN)4]2− and Macrocyclic Metal Complexes

College of Chemistry and Bioengineering, Hunan University of Science and Engineering, Yongzhou 425199, China
*
Author to whom correspondence should be addressed.
Molecules 2023, 28(11), 4529; https://doi.org/10.3390/molecules28114529
Submission received: 6 April 2023 / Revised: 9 May 2023 / Accepted: 29 May 2023 / Published: 2 June 2023
(This article belongs to the Special Issue Macrocyclic Compounds: Derivatives and Applications)

Abstract

:
Four one-dimensional complexes, denoted as [NiL1][Ni(CN)4] (1), [CuL1][Ni(CN)4] (2), [NiL2][Ni(CN)4]·2H2O (3), and [CuL2][Ni(CN)4]·2H2O (4) (L1 = 1,8-dimethyl-1,3,6,8,10,13-hexaaza-cyclotetradecane; L2 = 1,8-dipropyl-1,3,6,8,10,13-hexaazacyclotetradecane) were synthesized by reacting nickel/copper macrocyclic complexes with K2[Ni(CN)4]. Subsequently, the synthesized complexes were characterized using elemental analysis, infrared spectroscopy analysis, thermogravimetric analysis, and X-ray powder diffraction. Single-crystal structure analysis revealed that the Ni(II)/Cu(II) atoms were coordinated by two nitrogen atoms from [Ni(CN)4]2− with four nitrogen atoms from a macrocyclic ligand, forming a six-coordinated octahedral coordination geometry. Nickel/copper macrocyclic complexes were bridged by [Ni(CN)4]2− to construct one-dimensional chain structures in 14. The characterization results showed that the four complexes obeyed the Curie–Weiss law with a weak antiferromagnetic exchange coupling.

1. Introduction

The rational construction of one to three-dimensional porous coordination complexes has attracted considerable attention because of their potential applications in gas adsorption and separation, catalysis, and magnetism [1,2,3,4]. The design and assembly of different dimensional cyano-bridged complexes have been extensively researched in recent decades. Cyano-bridged complexes with superior magnetic properties can be constructed using cyano complexes, such as [Ag(CN)2], [Cu(CN)3]2−, [M(CN)4]2− (M = Cd, Ni, Pd, and Pt), and [M(CN)6]3− (M = W, Mo, and Fe) [5,6,7,8,9,10,11,12,13,14,15]. Studies on tetracyanometallate anions [Ni(CN)4]2− exhibiting bridging characteristics with either one or two of the cyano groups have been reported [16,17,18,19,20,21,22,23,24,25,26,27,28].
In previous reports, a few cyano-bridged complexes with one-dimensional helical chains were prepared and structurally characterized using transition metal macrocyclic complexes [NiL0]2+ (L0 = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclo-tetradecane) and [Ni(CN)4]2− [24]. As a continuation of the above research, we used different macrocyclic ligands (L1 = 1,8-dimethyl-1,3,6,8,10,13-hexaazacyclotetradecane, L2 = 1,8-dipropyl-1,3,6,8,10,13-hexaazacyclotetradecane, represented in Scheme 1) for the construction of cyano-bridged complexes. In this study, we synthesized four cyano-bridged complexes: [NiL1][Ni(CN)4] (1), [CuL1][Ni(CN)4] (2), [NiL2][Ni(CN)4]·2H2O (3), and [CuL2][Ni(CN)4]·2H2O (4), which were isolated from the reactions of [ML](ClO4)2 with [Ni(CN)4]2−. In addition, the structures and magnetism of four cyano-bridged complexes were analyzed.

2. Results and Discussion

2.1. Description of Structures

Figure 1 shows the similarity between the structures of complexes 1 and 2. One asymmetric unit of the structure of complex 1 contained one [NiL1]2+ cation and one [Ni(CN)4]2− anion. Each Ni(1) was on an inversion center and coordinated with four nitrogen atoms, namely N(1), N(2), N(1A), and N(2A) (symmetry code: A, 1–x, 1–y, and 1–z), of the macrocyclic ligand in the equatorial plane and two nitrogen atoms, namely, N(4) and N(4B) (symmetry code: B, –x, –y, 1–z), of [Ni(CN)4]2− in axial positions, forming a six-coordinated octahedral geometry in 1. The distances [2.0498(16) and 2.0712(16) Å] of Ni(1)-N(macrocycle) were shorter than that of the Ni(1)-N(cyano) [2.1489(17) Å], and they were longer than that of the Ni(2)-C(cyano) [1.858(2)-1.866(2) Å] (Table 1). The [Ni(CN)4]2− anion bridged the macrocyclic complex [NiL1]2+ cation in trans-positions to form a one-dimensional chain along the b-axis (Figure 1). One-dimensional linear chains were formed when trans-M(II) tetradentate macrocyclic complexes were used because of steric hindrance. Four possible helical isomers can be formed when cis-M(II) tetradentate macrocyclic complexes and [Ni(CN)4]2− building blocks are used [18,19,24].
The six-coordinated Cu(II) ions of complex 2 displayed a distorted octahedral geometry by coordinating with four nitrogen atoms, namely, N(1), N(2), N(1A), and N(2A) (symmetry code: A, 1–x, 1–y, 1–z), of macrocyclic ligand in the equatorial plane and two nitrogen atoms, namely, N(5) and N(5B) (symmetry code: B, –x, –y, 1–z) of [Ni(CN)4]2− in axial positions (Figure 1). The Cu(1)-N(macrocycle) distances [2.0009(15) and 2.0240(16) Å] were shorter than the Cu(1)-N(cyano) distances [2.563(2) Å] due to the Jahn-Teller effect, but longer than the distances [1.861(2)-1.865(2) Å] of Ni(1)-C(cyano) (Table 1). The [Ni(CN)4]2− anion bridged the macrocyclic complex [CuL1]2+ cation in trans-positions to form a one-dimensional chain along the b-axis in 2 (Figure 1). Complexes 3 and 4 exhibited similar one-dimensional structures. The asymmetric unit of complex 3/4 contained one [Ni/CuL2]2+ cation, one [Ni(CN)4]2− anion, and two water molecules (Figure 2). The Ni(II)/Cu(II) ions were coordinated by four nitrogen atoms of ligands along the equatorial plane and two nitrogen atoms of [Ni(CN)4]2− in axial positions. The [Ni(CN)4]2− anion bridged the macrocyclic complex [Ni/CuL2]2+ cation in trans-positions to form a one-dimensional chain along the b-axis in 3/4 (Figure 2).
Due to the Jahn-Teller effect, the axial Cu–N(cyano) bonds were considerably longer [2.563(2) in 2 and 2.410(2) Å in 4 (Table 1)] than those of the equatorial with mean values of Cu–N(macrocycle) bonds of 2.0125(15) and 2.0159(19) Å in 2 and 4, respectively. The five-membered intra-chelate N-M-N angles had similar values [85.85(7), 86.28(7), 85.66(10), and 85.93(8) Å for 14, respectively]. The Ni–C–N angles slightly deviated from linearity, and the maximum deviation was observed for the Ni–C–N angle [171.6(7)°] in complex 1, and the Ni–C–N angles of coordinated cyano groups [171.6(7)°, 175.7(9)°, 177.1(2)°, and 178.0(2)° for 14, respectively] were smaller than those of uncoordinated cyano groups [176.0(2)°, 177.3(2)°, 178.9(3)°, and 178.8(3)° for 14, respectively]. However, the M–C–N angles significantly deviated from linearity. The M–C–N angles of the L1 ligand [149.7(5)° and 127.8(8)° for 1 and 2, respectively] were smaller than the M–C–N angles of L2 ligand [168.4(2)° and 160.8(2)° for 3 and 4, respectively], shortening the distances of neighboring macrocyclic metal center [9.834(2), 9.906(2), 10.187(2), and 10.647(2) Å for 14].

2.2. IR Spectra

The infrared spectra (Figures S1–S4) of complexes 3 and 4 had broad absorption bands near 3400 cm–1, and the absorption was attributed to the stretching vibration of O–H. The N–H absorption bands appeared near 3200 cm–1, and the absorption bands at 2136 (s) and 2125 (s), 2123 (s) and 2119 (s), 2152 (s) and 2131 (s), and 2136 (s) and 2129 (s) cm–1 were assigned to υ(M–CN–M) and υ(M–CN) (M = Ni or Cu) in complexes 14.

2.3. XRD and TG

X-ray powder diffraction measurements for 14 (Figure 3) showed that the peaks in the measured patterns for both complexes closely matched those in the simulated patterns generated from single-crystal diffraction data, indicating that single phases were formed.
Figure 4 shows the thermogravimetric analysis (TGA) curves of both complexes. The TGA of complex 1 revealed that a weight loss of approximately 24.2% occurred from room temperature to 613 K, corresponding to the release of adsorbed water from the air (2.3%) and four CN (calcd 22.5%).
The decomposition of the macrocyclic structure was observed after the further heating of the macrocyclic ligand. The TGA curve for 2 showed the first weight loss from room temperature to 523 K, and the observed weight loss of 22.8% was related to the release of four CN (calcd 22.7%). Then, the macrocyclic structure began to decompose after the macrocyclic ligand was further heated.
The TGA curve for complex 3 revealed that a weight loss of approximately 27.2% occurred from room temperature to 630K, which was attributed to the release of adsorbed water from the air (2.3%), two lattice water molecules (calcd 6.5%), and four CN (calcd 18.6%). The weight loss was attributed to the release of structural water molecules and four CN. The TGA curve of complex 4 was similar to that of complex 3, which revealed that an initial weight loss of 25.3% (calcd 25.5%) occurred from room temperature to 496 K, corresponding to the release of structural water molecules and four CN.

2.4. Magnetism

Magnetic susceptibility measurements were performed to investigate the magnetic behaviors of complexes 14 at 1000 G within the temperature range of 2–300 K. Plots of χM vs. T and µeff/µB vs. T of the complexes within the temperature range of 2–300 K are shown in Figure 5. Complexes 1 and 3 exhibited similar magnetic properties, and their µeff/µB values within the temperature range of 7–300 K were close to the theoretical value expected for two unpaired d electrons in Ni(II) ions. In addition, complexes 2 and 4 exhibited similar magnetic properties, and their µeff/µB values within the temperature range of 7–300 K were close to the theoretical value expected for an unpaired d electron in Cu(II) ions.
The magnetic susceptibility measurements between 2 and 300 K yielded C = 1.35 cm3·K·mol−1 and θ = −1.85 K for 1, while the corresponding values were C = 0.56 cm3·K·mol−1 and θ = −2.21 K for 2, C = 1.15 cm3·K·mol−1 and θ = −1.79 K for 3, and C = 0.43 cm3·K·mol−1 and θ = −2.20 K for 4. The antiferromagnetic interactions were confirmed because of the negative Weiss constants θ in complexes 14. Weak antiferromagnetic interactions were also observed in analogous complexes Cu(cyclam)M(CN)4 [cyclam = 1,4,8,11−tetraazacyclotetradecane, M = Ni, Pd], and the reported values of the Weiss constants θ were −0.79 K for M = Ni [21]. The characterization results showed that the four complexes 14 obeyed the Curie–Weiss law with a weak antiferromagnetic exchange coupling.

3. Materials and Methods

The Ni(II) and Cu(II) macrocycle complexes were prepared following the previous report procedure [29]. All of the chemicals used in this work were commercially available and were used without further purification. Elemental analyses were carried out using an Elementar Micro Cube elemental analyzer. Infrared spectra were recorded in the 4000−400 cm−1 region using KBr pellets and a Bruker EQUINOX 55 spectrometer (Bruker, Germany). Thermogravimetric analyses were performed using a Netzsch STA 449F3 instrument (Netzsch, Germany) in flowing air at a heating rate of 10 °C·min−1. X-ray powder diffraction data were recorded using a Bruker D8 ADVANCE X-ray powder diffractometer (Cu Kα radiation, λ = 1.5418 Å, Bruker, Germany). Magnetic susceptibility measurements were conducted to determine the magnetic behaviors of both complexes at 1000 G in a temperature range of 2–300 K.

Preparation of the Compounds

[NiL1][Ni(CN)4] (1): An aqueous solution (20 mL) of K2[Ni(CN)4] (0.024 g, 0.1 mmol) was layered on an acetonitrile solution (20 mL) of NiL1(ClO4)2 (0.048 g, 0.1 mmol). After a few days, green prism crystals of 1 with ~37% yield were obtained. Elemental Anal. Found: C, 37.62; H, 5.65; N, 31.25%. Calcd for C7H13NiN5: C, 37.22; H, 5.80; N, 31.00%. IR (KBr): 3226 (s), 2946 (m), 2870 (m), 2136 (s), 2125 (s), 1435 (m), 1283 (s), 1059 (m), 1015 (m), 834 (m), and 603 (m) cm–1.
[CuL1][Ni(CN)4] (2): An aqueous solution (20 mL) of K2[Ni(CN)4] (0.024 g, 0.1 mmol) was layered on an acetonitrile solution (20 mL) of CuL1(ClO4)2 (0.049 g, 0.1 mmol). After some weeks, red prism crystals of 2 with ~42% yield were obtained. Elemental Anal. Found: C, 36.45; H, 5.98; N, 30.92%. Calcd for C14H26CuN10Ni: C, 36.82; H, 5.74; N, 30.67%. IR (KBr): 3247 (m), 3180 (m), 2960 (w), 2123 (s), 2119 (s), 1430 (m), 1286 (m), 1090 (m), 1007 (s), 840 (m), 612 (m) cm–1.
[NiL2][Ni(CN)4]·2H2O (3): Crystals of complex 3 with ~28% yield were prepared following the similar synthetic method of complex 1; however, [NiL2](ClO4)2 (0.054 g, 0.1 mmol) was used in place of [NiL1](ClO4)2. Elemental Anal. Found: C, 39.92; H, 7.28; N, 25.52%. Calcd. for C18H38Ni2N10O2: C, 39.75; H, 7.04; N, 25.75%. IR (KBr): 3590 (m), 3405 (m), 3222 (m), 2870 (w), 2152 (s), 2131 (s), 1430 (w), 1284 (w), 1080 (m), 1019 (s), 908 (m), and 620 (m) cm–1.
[CuL2][Ni(CN)4]·2H2O (4): Crystals of complex 4 with ~35% yield were synthesized using a similar synthetic method of complex 1; however, [CuL2](ClO4)2 (0.055 g, 0.1 mmol) was used in place of [NiL1](ClO4)2. Elemental Anal. Found: C, 39.65; H, 6.65; N, 25.35%. Calcd. for C18H38CuNiN10O2: C, 39.39; H, 6.98; N, 25.52%. IR (KBr): 3599 (m), 3372 (m), 3181 (m), 2925 (w), 2136 (s), 2129 (s), 1426 (w), 1285 (w), 1087 (m), 1012 (s), 842 (m), and 627 (m) cm–1.
Crystal Structure Determination. Single-crystal data for 14 were collected using a Bruker Smart Apex II diffractometer (Bruker, Germany) with Mo-Kα radiation (λ = 0.71073 Å). All empirical absorption corrections were applied using the SADABS program [30]. All structures were solved using direct methods, which yielded the positions of all non-hydrogen atoms. The positions were first refined isotropically, then anisotropically. All the hydrogen atoms of the ligands were placed in calculated positions with fixed isotropic thermal parameters and included in the structure factor calculations in the final stage of full-matrix least-squares refinement. All calculations were performed using the SHELXTL 5.1 software package [31]. For complexes 3 and 4, the hydrogen atoms bonded to oxygen were introduced at idealized positions and refined as riders with isotropic displacement parameters assigned 1.2 times the Ueq value of the corresponding bonding partner. Selected bond lengths and angles are listed in Table 1. The crystallographic data of 14 are summarized in Table 2.

4. Conclusions

In this work, four one-dimensional linear chains were successfully obtained between the reactions of macrocyclic nickel/copper complexes and [Ni(CN)4]2−. All complexes exhibited one-dimensional linear chain structures, which were formed by bridging [NiL]2+/[CuL]2+ with [Ni(CN)4]2− moieties. The magnetic susceptibilities revealed Curie-Weiss behavior for complexes 14 and the existence of weak antiferromagnetic exchange coupling.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/molecules28114529/s1, Figure S1: The infrared spectra of complex 1; Figure S2: The infrared spectra of complex 2; Figure S3: The infrared spectra of complex 3; Figure S4: The infrared spectra of complex 4.

Author Contributions

Conceptualization, G.O.; methodology, G.O.; software, G.O.; validation, G.O.; formal analysis, Q.Z.; investigation, Q.Z.; resources, Q.W.; data curation, Q.Z.; writing—original draft preparation, Q.W. and Y.T.; writing—review and editing, G.O.; visualization, Y.T.; supervision, G.O.; project administration, G.O.; funding acquisition, G.O. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the Scientific Research Fund of Hunan Provincial Education Department, grant number 20A210, and the National Natural Science Foundation of China, grant number 51772091.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Crystallographic data for 14 have been deposited with the Cambridge Crystallographic Data Center as supplemental publication numbers CCDC 2178844, 2178845, 2178848, and 2178849, respectively. Copies of the data can be obtained free of charge via http://www.ccdc.cam.ac.uk (accessed on 30 August 2022).

Acknowledgments

We acknowledge the National Natural Science Foundation of China and the Scientific Research Fund of Hunan Provincial Education Department.

Conflicts of Interest

The authors declare no conflict of interest.

Sample Availability

Samples of the compounds are available from the authors.

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Scheme 1. Structural formula of macrocyclic complexes (R1 = CH3, R2 = C3H7, and M = Ni or Cu).
Scheme 1. Structural formula of macrocyclic complexes (R1 = CH3, R2 = C3H7, and M = Ni or Cu).
Molecules 28 04529 sch001
Figure 1. (I) The structure of complexes 1 and 2 (M = Ni or Cu) and the symmetry codes for the generated atoms: A(1−x, 1−y, 1−z), B(−x, −y, 1−z); (II) The [Ni(CN)4]2− bridges macrocyclic complex [ML1]2+ to form a one-dimensional chain along the b-axis.
Figure 1. (I) The structure of complexes 1 and 2 (M = Ni or Cu) and the symmetry codes for the generated atoms: A(1−x, 1−y, 1−z), B(−x, −y, 1−z); (II) The [Ni(CN)4]2− bridges macrocyclic complex [ML1]2+ to form a one-dimensional chain along the b-axis.
Molecules 28 04529 g001
Figure 2. (I) The structure of complexes 3 and 4 (M = Ni or Cu) and the symmetry codes for the generated atoms: A(1−x, 1−y, 1−z), B(−x, −y, 1−z); (II) The [Ni(CN)4]2− bridges macrocyclic complex [ML2]2+ to form a one-dimensional chain along the b-axis.
Figure 2. (I) The structure of complexes 3 and 4 (M = Ni or Cu) and the symmetry codes for the generated atoms: A(1−x, 1−y, 1−z), B(−x, −y, 1−z); (II) The [Ni(CN)4]2− bridges macrocyclic complex [ML2]2+ to form a one-dimensional chain along the b-axis.
Molecules 28 04529 g002
Figure 3. XRD patterns of complexes 14.
Figure 3. XRD patterns of complexes 14.
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Figure 4. TGA curves of complexes 14.
Figure 4. TGA curves of complexes 14.
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Figure 5. Plots of χM vs. T and μeff/μB vs. T (inset) of complexes 14 in the temperature range of 2–300 K.
Figure 5. Plots of χM vs. T and μeff/μB vs. T (inset) of complexes 14 in the temperature range of 2–300 K.
Molecules 28 04529 g005
Table 1. Selected bond distances (Å) and angles (°).
Table 1. Selected bond distances (Å) and angles (°).
1
Bond LengthBondLengthBondLength
Ni(1)-N(1)2.0498(16)Ni(1)-N(2)2.0712(16)Ni(1)-N(4)2.1489(17)
Ni(2)-C(6)1.866(2)Ni(2)-C(7)1.858(2)
BondAngleBondAngleBondAngle
N(1)-Ni(1)-N(2)94.15(7)N(1)-Ni(1)-N(2) #185.85(7)N(1)-Ni(1)-N(4) #190.27(6)
N(2)-Ni(1)-N(4) #188.33(6)N(1)-Ni(1)-N(4)89.73(6)N(2)-Ni(1)-N(4)91.67(6)
N(5)-C(7)-Ni(2)176.0(2)N(4)-C(6)-Ni(2)171.6(7)C(6)-N(6)-Ni(1)149.7(5)
2
Bond LengthBondLengthBondLength
Cu(1)-N(1)2.0009(15)Cu(1)-N(2)2.0240(16)Cu(1)-N(5)2.563(2)
Ni(1)-C(7)1.865(2)Ni(1)-C(6)1.861(2)
BondAngleBondAngleBondAngle
N(1)-Cu(1)-N(2)93.72(7)N(1)-Cu(1)-N(2) #186.28(7)C(6)-Ni(1)-C(7)88.08(9)
C(6)-Ni(1)-C(7) #291.92(9)N(5)-C(7)-Ni(1)175.7(9)N(4)-C(6)-Ni(1)177.3(2)
C(7)-N(5)-Cu(1)127.8(8)
3
Bond LengthBondLengthBondLength
Ni(1)-N(1)2.061(2)Ni(1)-N(2)2.068(2)Ni(1)-N(4)2.118(2)
Ni(2)-C(8)1.864(3)Ni(2)-C(9)1.862(3)
BondAngleBondAngleBondAngle
N(1)-Ni(1)-N(2) #185.66(10)N(1)-Ni(1)-N(2)94.34(10)N(1)-Ni(1)-N(4)92.09(10)
N(2)-Ni(1)-N(4)91.21(9)N(1)-Ni(1)-N(4) #187.91(10)N(2)-Ni(1)-N(4) #188.79(9)
C(9)-Ni(2)-C(8)91.14(11)C(9)-Ni(2)-C(8) #388.86(11)N(4)-C(8)-Ni(2)177.1(2)
N(5)-C(9)-Ni(2)178.9(3)C(8)-N(4)-Ni(1)148.4(2)
4
Bond LengthBondLengthBondLength
Cu(1)-N(1)2.016(2)Cu(1)-N(2)2.0159(19)Cu(1)-N(4)2.410(2)
Ni(1)-C(8)1.864(3)Ni(1)-C(9)1.865(3)
BondAngleBondAngleBondAngle
N(1)-Cu(1)-N(2) #485.93(8)N(1)-Cu(1)-N(2)94.07(8)N(1)-Cu(1)-N(4) #491.93(8)
N(2)-Cu(1)-N(4) #491.37(9)N(1)-Cu(1)-N(4)88.07(8)N(2)-Cu(1)-N(4)88.63(9)
C(8)-Ni(1)-C(9)90.18(11)C(8)-Ni(1)-C(9) #589.82(11)N(4)-C(8)-Ni(1)178.0(2)
N(5)-C(9)-Ni(1)178.8(3)C(8)-N(4)-Cu(1)160.8(2)
Symmetry transformation: #1x + 1, −y + 1, −z + 1; #2x, −y + 1, −z + 1; #3x + 2, −y + 1, −z; #4x + 1, −y + 1, −z + 2; #5x + 2, −y + 1, −z + 1.
Table 2. Crystallographic data.
Table 2. Crystallographic data.
Compound[NiL1][Ni(CN)4][CuL1][Ni(CN)4][NiL2][Ni(CN)4]·2H2O[CuL2][Ni(CN)4]·2H2O
Empirical formulaC14H26Ni2N10C14H26CuNiN10C18H38Ni2O2N10C18H38CuNiN10O2
Formula weight451.86456.70544.00548.83
Temperature (K)296(2)296(2)296(2)296(2)
Crystal systemMonoclinicMonoclinicTriclinicTriclinic
Space groupP2(1)/nP2(1)/nP-1P-1
a9.834(3)9.906(4) 8.588(8)8.400(4)
b9.167(3)9.110(4)8.873(8)8.771(4)
c10.910(4)10.785(5)10.001(9)10.098(4)
α909080.930(11)81.180(4)
β95.177(4)92.268(4)65.954(10)69.590(4)
γ909067.544(10)67.991(4)
V3979.5(6)972.6(7) 643.1(10)646.2(5)
Z4221
Dc/Mg cm−31.5321.5591.4051.410
μ/mm−11.9432.0821.4981.585
F (000)472474288289
Crystal size (mm)0.36 × 0.28 × 0.230.46 × 0.36 × 0.280.28 × 0.23 × 0.150.38 × 0.26 × 0.20
θ range 2.67–27.462.74–27.472.23–27.442.15–27.53
Collected/unique10687/2221(0.022)10594/2206(0.021)7227/2838(0.0295)6873/2872(0.0306)
Completeness to θ 99.3%99.1%97.0%96.3%
Goodness-of-fit on F21.0411.0120.9790.991
Final R indices [I > 2σ (I)]0.0279, 0.07210.0268, 0.07160.0340, 0.08280.0356, 0.0893
R indices (all data)0.0411, 0.07990.0417, 0.07920.0554, 0.09100.0551, 0.0981
Max. peak/hole (e. Å−3)0.290/−0.1730.196/−0.1780.460/−0.4640.605/−0.379
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Ou, G.; Wang, Q.; Tan, Y.; Zhou, Q. Synthesis, Structures, and Magnetism of Four One-Dimensional Complexes Using [Ni(CN)4]2− and Macrocyclic Metal Complexes. Molecules 2023, 28, 4529. https://doi.org/10.3390/molecules28114529

AMA Style

Ou G, Wang Q, Tan Y, Zhou Q. Synthesis, Structures, and Magnetism of Four One-Dimensional Complexes Using [Ni(CN)4]2− and Macrocyclic Metal Complexes. Molecules. 2023; 28(11):4529. https://doi.org/10.3390/molecules28114529

Chicago/Turabian Style

Ou, Guangchuan, Qiong Wang, Yingzhi Tan, and Qiang Zhou. 2023. "Synthesis, Structures, and Magnetism of Four One-Dimensional Complexes Using [Ni(CN)4]2− and Macrocyclic Metal Complexes" Molecules 28, no. 11: 4529. https://doi.org/10.3390/molecules28114529

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