Syntheses, crystal structures and thermal properties of catena-poly[cadmium(II)-di-μ-bromido-μ-pyridazine-κ²N¹:N²] and catena-poly[cadmium(II)-di-μ-iodido-μ-pyridazine-κ²N¹:N²]

In the crystal structures of the title compounds, the cadmium cations are octa­hedrally coordinated by four halide anions and two pyridazine ligands in a trans-CdX₄N₂ (X = Br, I) arrangement and are linked into chains by the halide anions and the pyridazine ligands.

Key indicators

Structure: 1

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.020
• wR factor = 0.057
• Data-to-parameter ratio = 26.5

Structure: 2

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.016
• wR factor = 0.046
• Data-to-parameter ratio = 29.6

checkCIF/PLATON results

No syntax errors found



Datablock: 1


Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.06 Report

Alert level G
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          1 Info
PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check
PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cd1      --Br1      .       10.5 s.u.
PLAT794_ALERT_5_G Tentative Bond Valency for Cd1       (II)      .       1.96 Info
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         41 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          1 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   1 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   7 ALERT level G = General information/check it is not something unexpected

   2 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
   2 ALERT type 5 Informative message, check




Datablock: 2


Alert level C
PLAT112_ALERT_2_C ADDSYM Detects New (Pseudo) Symm. Elem       b/2         80 %Fit

Alert level G
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          1 Info
PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check
PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  I1       --Cd1      .       21.9 s.u.
PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.25 Ratio
PLAT794_ALERT_5_G Tentative Bond Valency for Cd1       (II)      .       1.98 Info
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         49 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          1 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   1 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   8 ALERT level G = General information/check it is not something unexpected

   2 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

---

Computing details

For both structures, data collection: CrysAlis PRO 1.171.42.67a (Rigaku OD, 2022); cell refinement: CrysAlis PRO 1.171.42.67a (Rigaku OD, 2022); data reduction: CrysAlis PRO 1.171.42.67a (Rigaku OD, 2022); program(s) used to solve structure: SHELXT2014/4 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2016/6 (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

catena-Poly[cadmium(II)-di-µ-bromido-µ-pyridazine-κ²N¹:N²] (1)

Crystal data

[CdBr2(C4H4N2)]	Dx = 3.143 Mg m^−3
Mr = 352.31	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Imma	Cell parameters from 4638 reflections
a = 7.2540 (2) Å	θ = 3.0–33.2°
b = 7.7223 (2) Å	µ = 13.58 mm^−1
c = 13.2910 (4) Å	T = 293 K
V = 744.53 (4) Å^3	Block, colourless
Z = 4	0.08 × 0.06 × 0.04 mm
F(000) = 640

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	769 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Mo) X-ray Source	684 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.039
Detector resolution: 10.0000 pixels mm^-1	θmax = 33.3°, θmin = 3.1°
ω scans	h = −10→10
Absorption correction: multi-scan (CrysAlisPro; Rigaku OD, 2022)	k = −11→11
Tmin = 0.582, Tmax = 1.000	l = −19→20
6952 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.020	H-atom parameters constrained
wR(F^2) = 0.057	w = 1/[σ^2(Fo^2) + (0.0315P)^2 + 0.191P] where P = (Fo^2 + 2Fc^2)/3
S = 1.16	(Δ/σ)max < 0.001
769 reflections	Δρmax = 1.07 e Å^−3
29 parameters	Δρmin = −0.52 e Å^−3
0 restraints

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.

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

	x	y	z	Uiso*/Ueq
Cd1	0.250000	0.250000	0.250000	0.02829 (10)
Br1	0.500000	0.49073 (3)	0.18013 (2)	0.03175 (10)
N1	0.4072 (3)	0.250000	0.40756 (16)	0.0294 (4)
C1	0.3181 (4)	0.250000	0.4947 (2)	0.0365 (6)
H1	0.189944	0.250000	0.493718	0.044*
C2	0.4065 (4)	0.250000	0.5870 (2)	0.0369 (6)
H2	0.340042	0.250000	0.646880	0.044*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.01738 (14)	0.04001 (17)	0.02748 (15)	0.000	−0.00137 (9)	0.000
Br1	0.02359 (15)	0.03169 (16)	0.03996 (18)	0.000	0.000	0.00394 (10)
N1	0.0203 (10)	0.0403 (11)	0.0276 (11)	0.000	0.0005 (9)	0.000
C1	0.0216 (13)	0.0565 (18)	0.0313 (13)	0.000	0.0041 (12)	0.000
C2	0.0317 (14)	0.0527 (16)	0.0262 (12)	0.000	0.0042 (12)	0.000

Geometric parameters (Å, º)

Cd1—Br1	2.7581 (2)	N1—N1^ii	1.346 (4)
Cd1—Br1^i	2.7581 (2)	N1—C1	1.326 (4)
Cd1—Br1^ii	2.7581 (2)	C1—H1	0.9300
Cd1—Br1^iii	2.7581 (2)	C1—C2	1.385 (4)
Cd1—N1	2.385 (2)	C2—C2^ii	1.357 (6)
Cd1—N1^iii	2.385 (2)	C2—H2	0.9300
Br1—Cd1—Br1^iii	180.0	N1^iii—Cd1—Br1^i	88.92 (4)
Br1^iii—Cd1—Br1^ii	95.243 (9)	N1—Cd1—N1^iii	180.0
Br1^ii—Cd1—Br1^i	180.0	Cd1—Br1—Cd1^ii	82.223 (7)
Br1^iii—Cd1—Br1^i	84.757 (9)	N1^ii—N1—Cd1	118.58 (5)
Br1—Cd1—Br1^i	95.244 (9)	C1—N1—Cd1	122.26 (19)
Br1—Cd1—Br1^ii	84.756 (9)	C1—N1—N1^ii	119.16 (16)
N1^iii—Cd1—Br1^ii	91.08 (4)	N1—C1—H1	118.4
N1—Cd1—Br1	88.92 (4)	N1—C1—C2	123.3 (3)
N1—Cd1—Br1^iii	91.08 (4)	C2—C1—H1	118.4
N1^iii—Cd1—Br1^iii	88.92 (4)	C1—C2—H2	121.2
N1—Cd1—Br1^i	91.08 (4)	C2^ii—C2—C1	117.57 (17)
N1—Cd1—Br1^ii	88.92 (4)	C2^ii—C2—H2	121.2
N1^iii—Cd1—Br1	91.08 (4)

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

catena-Poly[cadmium(II)-di-µ-iodido-µ-pyridazine-κ²N¹:N²] (2)

Crystal data

[CdI2(C4H4N2)]	Dx = 3.484 Mg m^−3
Mr = 446.29	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Imma	Cell parameters from 6483 reflections
a = 7.5740 (2) Å	θ = 2.9–33.4°
b = 8.2979 (2) Å	µ = 9.75 mm^−1
c = 13.5363 (4) Å	T = 293 K
V = 850.73 (4) Å^3	Needle, colourless
Z = 4	0.12 × 0.03 × 0.02 mm
F(000) = 784

Data collection

XtaLAB Synergy, Dualflex, HyPix diffractometer	889 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Mo) X-ray Source	857 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.037
Detector resolution: 10.0000 pixels mm^-1	θmax = 33.4°, θmin = 2.9°
ω scans	h = −11→11
Absorption correction: multi-scan (CrysalisPro; Rigaku OD, 2022)	k = −12→12
Tmin = 0.382, Tmax = 1.000	l = −20→19
7478 measured reflections

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.016	w = 1/[σ^2(Fo^2) + (0.0233P)^2 + 0.8677P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.046	(Δ/σ)max = 0.001
S = 1.18	Δρmax = 0.78 e Å^−3
889 reflections	Δρmin = −0.56 e Å^−3
30 parameters	Extinction correction: SHELXL2016/6 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00206 (14)
Primary atom site location: dual

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.

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

	x	y	z	Uiso*/Ueq
Cd1	0.250000	0.250000	0.250000	0.02666 (8)
I1	0.500000	0.49464 (2)	0.17507 (2)	0.02931 (8)
N1	0.4115 (3)	0.250000	0.40441 (14)	0.0272 (4)
C1	0.3246 (4)	0.250000	0.48983 (19)	0.0354 (6)
H1	0.201820	0.250000	0.488661	0.042*
C2	0.4099 (4)	0.250000	0.5807 (2)	0.0377 (6)
H2	0.346328	0.250000	0.639534	0.045*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.01738 (12)	0.03918 (15)	0.02342 (12)	0.000	−0.00147 (7)	0.000
I1	0.02338 (10)	0.02851 (11)	0.03603 (12)	0.000	0.000	0.00422 (5)
N1	0.0194 (9)	0.0420 (11)	0.0203 (8)	0.000	−0.0006 (7)	0.000
C1	0.0224 (11)	0.0607 (19)	0.0230 (10)	0.000	0.0017 (9)	0.000
C2	0.0303 (13)	0.0615 (18)	0.0212 (10)	0.000	0.0031 (10)	0.000

Geometric parameters (Å, º)

Cd1—I1	2.9555 (1)	N1—N1^ii	1.341 (4)
Cd1—I1^i	2.9555 (1)	N1—C1	1.330 (3)
Cd1—I1^ii	2.9555 (1)	C1—H1	0.9300
Cd1—I1^iii	2.9555 (1)	C1—C2	1.390 (4)
Cd1—N1	2.4216 (19)	C2—C2^ii	1.366 (6)
Cd1—N1^iii	2.4216 (19)	C2—H2	0.9300
I1^iii—Cd1—I1	180.0	N1^iii—Cd1—I1	91.56 (4)
I1^iii—Cd1—I1^ii	93.237 (5)	N1—Cd1—N1^iii	180.0
I1^iii—Cd1—I1^i	86.763 (5)	Cd1—I1—Cd1^ii	79.683 (4)
I1^i—Cd1—I1^ii	180.0	N1^ii—N1—Cd1	120.33 (5)
I1^ii—Cd1—I1	86.763 (5)	C1—N1—Cd1	120.03 (18)
I1^i—Cd1—I1	93.237 (5)	C1—N1—N1^ii	119.64 (16)
N1^iii—Cd1—I1^ii	91.56 (4)	N1—C1—H1	118.7
N1—Cd1—I1^iii	91.56 (4)	N1—C1—C2	122.7 (3)
N1—Cd1—I1^i	91.56 (4)	C2—C1—H1	118.7
N1^iii—Cd1—I1^i	88.44 (4)	C1—C2—H2	121.2
N1—Cd1—I1	88.44 (4)	C2^ii—C2—C1	117.69 (17)
N1—Cd1—I1^ii	88.44 (4)	C2^ii—C2—H2	121.2
N1^iii—Cd1—I1^iii	88.44 (4)

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