Synthesis, crystal structure and properties of poly[di-μ₃-chlorido-di-μ₂-chlorido-bis­[4-methyl-N-(pyridin-2-yl­methyl­idene)aniline]dicadmium(II)]

The bidentate N,N′-chelating Schiff base ligand L and cadmium(II) chloride create a self-assembled polymeric chain structure [Cd₂Cl₄(L)]_n comprising a defect cubane-like motif.

Key indicators

Structure: I

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.007 Å
• R factor = 0.030
• wR factor = 0.066
• Data-to-parameter ratio = 17.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      2.810 Check

Alert level G
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          1 Info
PLAT013_ALERT_1_G N.O.K.   _shelx_hkl_checksum Found in CIF ......     Please Check
PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.001 Degree
PLAT794_ALERT_5_G Tentative Bond Valency for Cd1       (II)      .       1.93 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cd2       (II)      .       1.90 Info
PLAT802_ALERT_4_G CIF Input Record(s) with more than 80 Characters          1 Info
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          3 Note
                0  1  0,   0 -1  1,   0  0  1,
PLAT933_ALERT_2_G Number of HKL-OMIT Records in Embedded .res File          1 Note
                1  0  0,
PLAT969_ALERT_5_G The 'Henn et al.' R-Factor-gap value ...........       2.31 Note
              Predicted wR2: Based on SigI   2  2.83 or SHELX Weight  6.56       
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          0 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
  10 ALERT level G = General information/check it is not something unexpected

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   4 ALERT type 5 Informative message, check

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Computing details

Poly[di-µ₃-chlorido-di-µ₂-chlorido-[4-methyl-N-(pyridin-2-ylmethylidene)aniline]dicadmium(II)]

Crystal data

[Cd2Cl4(C13H12N2)]	Z = 2
Mr = 562.85	F(000) = 536
Triclinic, P1	Dx = 2.241 Mg m^−3
a = 6.8597 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.8855 (4) Å	Cell parameters from 1412 reflections
c = 12.8106 (5) Å	θ = 3.2–25.2°
α = 107.566 (1)°	µ = 3.18 mm^−1
β = 100.523 (1)°	T = 296 K
γ = 106.799 (1)°	Block, yellow
V = 834.02 (5) Å^3	0.18 × 0.14 × 0.14 mm

Data collection

Bruker D8 QUEST CMOS PHOTON II diffractometer	3418 independent reflections
Radiation source: sealed x-ray tube, Mo	2553 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.050
Detector resolution: 7.39 pixels mm^-1	θmax = 26.4°, θmin = 3.2°
ω and φ scans	h = −8→8
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	k = −13→13
Tmin = 0.696, Tmax = 0.745	l = −15→15
20153 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)] = 0.030	H-atom parameters constrained
wR(F^2) = 0.066	w = 1/[σ^2(Fo^2) + (0.0267P)^2 + 0.7296P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max < 0.001
3418 reflections	Δρmax = 0.73 e Å^−3
191 parameters	Δρmin = −0.41 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	0.43896 (5)	0.25775 (3)	0.19523 (2)	0.03039 (10)
Cd2	−0.17441 (5)	0.09278 (3)	0.07673 (2)	0.03114 (10)
Cl1	0.11124 (16)	0.18034 (11)	0.27038 (9)	0.0364 (3)
Cl3	0.46812 (15)	0.00951 (10)	0.13602 (8)	0.0274 (2)
Cl4	0.76831 (17)	0.31838 (11)	0.11374 (9)	0.0369 (3)
Cl2	0.15327 (15)	0.15624 (10)	−0.01197 (8)	0.0294 (2)
N1	0.4732 (6)	0.4839 (3)	0.2237 (3)	0.0345 (8)
N2	0.6415 (5)	0.3967 (3)	0.3893 (3)	0.0298 (8)
C1	0.4082 (8)	0.5310 (5)	0.1449 (4)	0.0456 (12)
H1	0.322184	0.467069	0.072599	0.055*
C2	0.4618 (8)	0.6699 (5)	0.1650 (4)	0.0522 (13)
H2	0.415590	0.698893	0.107078	0.063*
C3	0.5849 (8)	0.7646 (5)	0.2725 (5)	0.0525 (13)
H3	0.622400	0.859025	0.288606	0.063*
C4	0.6520 (7)	0.7183 (5)	0.3561 (4)	0.0424 (11)
H4	0.733459	0.780776	0.429718	0.051*
C5	0.5963 (6)	0.5771 (4)	0.3286 (3)	0.0322 (10)
C6	0.6732 (6)	0.5254 (4)	0.4146 (4)	0.0334 (10)
H6	0.746876	0.587535	0.489373	0.040*
C7	0.7158 (6)	0.3456 (4)	0.4728 (3)	0.0303 (9)
C8	0.8273 (7)	0.4274 (5)	0.5868 (4)	0.0365 (10)
H8	0.863455	0.522899	0.613147	0.044*
C9	0.8839 (7)	0.3655 (5)	0.6609 (4)	0.0416 (11)
H9	0.959473	0.421358	0.736998	0.050*
C10	0.8331 (7)	0.2238 (5)	0.6266 (4)	0.0427 (11)
C11	0.7295 (9)	0.1463 (5)	0.5128 (4)	0.0563 (14)
H11	0.700061	0.051484	0.485576	0.068*
C12	0.6677 (8)	0.2051 (5)	0.4378 (4)	0.0512 (14)
H12	0.591889	0.148618	0.361789	0.061*
C13	0.8854 (9)	0.1584 (6)	0.7100 (5)	0.0617 (15)
H13A	0.989813	0.228147	0.779111	0.093*
H13B	0.941330	0.089598	0.676953	0.093*
H13C	0.758629	0.115638	0.727315	0.093*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.03240 (18)	0.02790 (18)	0.02645 (17)	0.01212 (14)	0.00518 (13)	0.00540 (13)
Cd2	0.02639 (17)	0.03096 (18)	0.03128 (19)	0.01317 (14)	0.00606 (14)	0.00424 (14)
Cl1	0.0329 (6)	0.0427 (6)	0.0300 (5)	0.0128 (5)	0.0076 (4)	0.0107 (5)
Cl3	0.0302 (5)	0.0259 (5)	0.0252 (5)	0.0115 (4)	0.0081 (4)	0.0075 (4)
Cl4	0.0367 (6)	0.0292 (6)	0.0432 (6)	0.0126 (5)	0.0138 (5)	0.0096 (5)
Cl2	0.0305 (5)	0.0300 (5)	0.0262 (5)	0.0126 (4)	0.0056 (4)	0.0087 (4)
N1	0.039 (2)	0.031 (2)	0.036 (2)	0.0180 (17)	0.0102 (17)	0.0116 (17)
N2	0.0279 (18)	0.031 (2)	0.0265 (18)	0.0080 (16)	0.0069 (15)	0.0093 (15)
C1	0.060 (3)	0.046 (3)	0.039 (3)	0.030 (3)	0.013 (2)	0.018 (2)
C2	0.067 (4)	0.057 (3)	0.053 (3)	0.034 (3)	0.022 (3)	0.036 (3)
C3	0.060 (3)	0.038 (3)	0.069 (4)	0.021 (3)	0.023 (3)	0.027 (3)
C4	0.044 (3)	0.033 (3)	0.049 (3)	0.015 (2)	0.014 (2)	0.014 (2)
C5	0.032 (2)	0.032 (2)	0.032 (2)	0.0137 (19)	0.0112 (19)	0.0095 (19)
C6	0.031 (2)	0.033 (3)	0.030 (2)	0.009 (2)	0.0087 (18)	0.0076 (19)
C7	0.030 (2)	0.032 (2)	0.028 (2)	0.0112 (19)	0.0059 (18)	0.0099 (18)
C8	0.034 (2)	0.034 (2)	0.033 (2)	0.006 (2)	0.0050 (19)	0.011 (2)
C9	0.035 (2)	0.050 (3)	0.030 (2)	0.007 (2)	0.003 (2)	0.014 (2)
C10	0.037 (3)	0.052 (3)	0.040 (3)	0.017 (2)	0.011 (2)	0.018 (2)
C11	0.087 (4)	0.038 (3)	0.044 (3)	0.029 (3)	0.010 (3)	0.015 (2)
C12	0.079 (4)	0.034 (3)	0.029 (2)	0.021 (3)	0.002 (2)	0.004 (2)
C13	0.059 (3)	0.075 (4)	0.065 (4)	0.022 (3)	0.016 (3)	0.047 (3)

Geometric parameters (Å, º)

Cd1—Cl1	2.6221 (11)	C3—H3	0.9300
Cd1—Cl3	2.6548 (10)	C3—C4	1.375 (7)
Cd1—Cl4	2.6543 (11)	C4—H4	0.9300
Cd1—Cl2	2.6805 (10)	C4—C5	1.385 (6)
Cd1—N1	2.311 (3)	C5—C6	1.463 (6)
Cd1—N2	2.378 (3)	C6—H6	0.9300
Cd2—Cl1	2.5729 (10)	C7—C8	1.388 (6)
Cd2—Cl3^i	2.7555 (10)	C7—C12	1.375 (6)
Cd2—Cl3^ii	2.6874 (10)	C8—H8	0.9300
Cd2—Cl4^ii	2.5165 (11)	C8—C9	1.381 (6)
Cd2—Cl2	2.7074 (11)	C9—H9	0.9300
Cd2—Cl2^i	2.6404 (10)	C9—C10	1.385 (6)
N1—C1	1.327 (5)	C10—C11	1.369 (6)
N1—C5	1.348 (5)	C10—C13	1.497 (6)
N2—C6	1.281 (5)	C11—H11	0.9300
N2—C7	1.426 (5)	C11—C12	1.376 (6)
C1—H1	0.9300	C12—H12	0.9300
C1—C2	1.377 (6)	C13—H13A	0.9600
C2—H2	0.9300	C13—H13B	0.9600
C2—C3	1.374 (7)	C13—H13C	0.9600
Cl1—Cd1—Cl3	93.00 (3)	C7—N2—Cd1	125.1 (2)
Cl1—Cd1—Cl4	176.14 (3)	N1—C1—H1	118.4
Cl1—Cd1—Cl2	86.03 (3)	N1—C1—C2	123.2 (4)
Cl3—Cd1—Cl2	85.58 (3)	C2—C1—H1	118.4
Cl4—Cd1—Cl3	83.17 (3)	C1—C2—H2	120.7
Cl4—Cd1—Cl2	93.13 (3)	C3—C2—C1	118.6 (5)
N1—Cd1—Cl1	100.54 (9)	C3—C2—H2	120.7
N1—Cd1—Cl3	166.29 (9)	C2—C3—H3	120.4
N1—Cd1—Cl4	83.26 (9)	C2—C3—C4	119.3 (5)
N1—Cd1—Cl2	93.16 (9)	C4—C3—H3	120.4
N1—Cd1—N2	72.51 (12)	C3—C4—H4	120.6
N2—Cd1—Cl1	87.37 (8)	C3—C4—C5	118.8 (4)
N2—Cd1—Cl3	110.60 (9)	C5—C4—H4	120.6
N2—Cd1—Cl4	94.46 (8)	N1—C5—C4	122.0 (4)
N2—Cd1—Cl2	162.83 (8)	N1—C5—C6	118.1 (4)
Cl1—Cd2—Cl3^ii	100.81 (3)	C4—C5—C6	119.9 (4)
Cl1—Cd2—Cl3^i	176.84 (3)	N2—C6—C5	121.6 (4)
Cl1—Cd2—Cl2^i	93.06 (3)	N2—C6—H6	119.2
Cl1—Cd2—Cl2	86.45 (3)	C5—C6—H6	119.2
Cl3^ii—Cd2—Cl3^i	81.21 (3)	C8—C7—N2	124.5 (4)
Cl3^ii—Cd2—Cl2	172.42 (3)	C12—C7—N2	117.3 (4)
Cl4^ii—Cd2—Cl1	94.45 (4)	C12—C7—C8	118.2 (4)
Cl4^ii—Cd2—Cl3^ii	85.18 (3)	C7—C8—H8	120.3
Cl4^ii—Cd2—Cl3^i	88.13 (3)	C9—C8—C7	119.3 (4)
Cl4^ii—Cd2—Cl2^i	172.49 (3)	C9—C8—H8	120.3
Cl4^ii—Cd2—Cl2	96.53 (3)	C8—C9—H9	118.6
Cl2^i—Cd2—Cl3^i	84.37 (3)	C8—C9—C10	122.8 (4)
Cl2^i—Cd2—Cl3^ii	93.30 (3)	C10—C9—H9	118.6
Cl2—Cd2—Cl3^i	91.45 (3)	C9—C10—C13	121.8 (4)
Cl2^i—Cd2—Cl2	84.04 (3)	C11—C10—C9	116.5 (4)
Cd2—Cl1—Cd1	95.92 (4)	C11—C10—C13	121.7 (5)
Cd1—Cl3—Cd2^iii	93.50 (3)	C10—C11—H11	119.1
Cd1—Cl3—Cd2^i	93.98 (3)	C10—C11—C12	121.7 (5)
Cd2^iii—Cl3—Cd2^i	98.79 (3)	C12—C11—H11	119.1
Cd2^iii—Cl4—Cd1	97.59 (4)	C7—C12—C11	121.3 (4)
Cd1—Cl2—Cd2	91.47 (3)	C7—C12—H12	119.3
Cd2^i—Cl2—Cd1	96.07 (3)	C11—C12—H12	119.3
Cd2^i—Cl2—Cd2	95.96 (3)	C10—C13—H13A	109.5
C1—N1—Cd1	126.8 (3)	C10—C13—H13B	109.5
C1—N1—C5	118.1 (4)	C10—C13—H13C	109.5
C5—N1—Cd1	114.5 (3)	H13A—C13—H13B	109.5
C6—N2—Cd1	113.0 (3)	H13A—C13—H13C	109.5
C6—N2—C7	121.8 (3)	H13B—C13—H13C	109.5
Cd1—N1—C1—C2	−170.1 (4)	C3—C4—C5—C6	177.4 (4)
Cd1—N1—C5—C4	173.0 (3)	C4—C5—C6—N2	−173.4 (4)
Cd1—N1—C5—C6	−6.4 (5)	C5—N1—C1—C2	0.6 (7)
Cd1—N2—C6—C5	−2.2 (5)	C6—N2—C7—C8	−0.1 (6)
Cd1—N2—C7—C8	−177.5 (3)	C6—N2—C7—C12	178.0 (4)
Cd1—N2—C7—C12	0.5 (5)	C7—N2—C6—C5	−179.9 (4)
N1—C1—C2—C3	−1.4 (8)	C7—C8—C9—C10	−0.4 (7)
N1—C5—C6—N2	6.0 (6)	C8—C7—C12—C11	−0.6 (8)
N2—C7—C8—C9	177.5 (4)	C8—C9—C10—C11	2.6 (7)
N2—C7—C12—C11	−178.8 (5)	C8—C9—C10—C13	−176.4 (4)
C1—N1—C5—C4	1.2 (6)	C9—C10—C11—C12	−3.8 (8)
C1—N1—C5—C6	−178.3 (4)	C10—C11—C12—C7	2.9 (9)
C1—C2—C3—C4	0.5 (8)	C12—C7—C8—C9	−0.6 (7)
C2—C3—C4—C5	1.1 (7)	C13—C10—C11—C12	175.2 (5)
C3—C4—C5—N1	−2.0 (7)

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