Crystal structure of catena-poly[N,N,N′,N′-tetra­methyl­guanidinium [(chlorido­cadmate)-di-μ-chlorido]]

The structure of the title salt, {(C₅H₁₄N₃)[CdCl₃]}_n, consists of infinite zigzag polyanionic ¹_∞[CdCl_4/2Cl_1/1]⁻ chains held together by tetra­methyl­guanidinium cations through N—H...Cl hydrogen bonds, leading to a layered structure parallel to (010).

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](N-C) = 0.002 Å
• R factor = 0.016
• wR factor = 0.040
• Data-to-parameter ratio = 21.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT051_ALERT_1_C Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       1.87 %
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2C    ..  CL4     ..       2.87 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3B    ..  CL1     ..       2.92 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H4B    ..  CL4     ..       2.87 Ang.
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          2 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1 Note

Alert level G
ABSMU01_ALERT_1_G  Calculation of _exptl_absorpt_correction_mu
                not performed for this radiation type.
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          1 Info
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT128_ALERT_4_G Alternate Setting for Input Space Group     C2/c       I2/a Note
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cd1    --  Cl2     ..        7.0 su
PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.25 Ratio
PLAT794_ALERT_5_G Tentative Bond Valency for Cd1     (II)    .....       1.95 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   6 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

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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
   5 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

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Computing details

Data collection: APEX2 (Bruker, 2014); cell refinement: SAINT (Bruker, 2014); data reduction: SAINT (Bruker, 2014); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009) and Mercury (Macrae et al., 2008); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009) and publCIF (Westrip, 2010).

catena-Poly[N,N,N',N'-tetramethylguanidinium [(chloridocadmate)-di-µ-chlorido]]

Crystal data

(C5H14N3)[CdCl3]	F(000) = 1312
Mr = 334.94	Dx = 1.981 Mg m^−3
Monoclinic, C2/c	Ga Kα radiation, λ = 1.34139 Å
a = 15.1305 (7) Å	Cell parameters from 9941 reflections
b = 14.2921 (6) Å	θ = 3.9–60.7°
c = 11.6939 (5) Å	µ = 14.50 mm^−1
β = 117.370 (2)°	T = 100 K
V = 2245.69 (17) Å^3	Block, clear light colourless
Z = 8	0.19 × 0.10 × 0.10 mm

Data collection

Bruker Venture Metaljet diffractometer	2593 independent reflections
Radiation source: Metal Jet, Gallium Liquid Metal Jet Source	2575 reflections with I > 2σ(I)
Helios MX Mirror Optics monochromator	Rint = 0.043
Detector resolution: 10.24 pixels mm^-1	θmax = 60.7°, θmin = 3.9°
ω and φ scans	h = −19→19
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	k = −18→18
Tmin = 0.400, Tmax = 0.752	l = −15→15
24837 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.016	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.040	w = 1/[σ^2(Fo^2) + (0.0144P)^2 + 2.6083P] where P = (Fo^2 + 2Fc^2)/3
S = 1.13	(Δ/σ)max = 0.001
2593 reflections	Δρmax = 0.63 e Å^−3
122 parameters	Δρmin = −0.40 e Å^−3
0 restraints

Special details

Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Venture diffractometer equipped with a Photon 100 CMOS Detector, a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode.

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.

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

	x	y	z	Uiso*/Ueq
N1	0.18403 (9)	0.36639 (9)	0.56127 (12)	0.0134 (2)
N2	0.35116 (10)	0.36153 (11)	0.61584 (14)	0.0191 (3)
N3	0.24068 (10)	0.42244 (9)	0.41914 (13)	0.0150 (3)
C1	0.25851 (11)	0.38434 (10)	0.53204 (15)	0.0132 (3)
C2	0.09488 (11)	0.42502 (11)	0.51613 (15)	0.0153 (3)
H2C	0.1042	0.4816	0.4756	0.023*
H2D	0.0835	0.4425	0.5894	0.023*
H2E	0.0373	0.3901	0.4532	0.023*
C3	0.19647 (12)	0.29906 (11)	0.66197 (15)	0.0152 (3)
H3A	0.2479	0.2535	0.6719	0.023*
H3B	0.1334	0.2664	0.6379	0.023*
H3C	0.2164	0.3322	0.7435	0.023*
C4	0.14557 (12)	0.41074 (12)	0.30272 (15)	0.0200 (3)
H4A	0.1074	0.3604	0.3163	0.030*
H4B	0.1581	0.3948	0.2300	0.030*
H4C	0.1076	0.4692	0.2842	0.030*
C5	0.32011 (13)	0.46786 (12)	0.40087 (17)	0.0212 (3)
H5A	0.3718	0.4902	0.4841	0.032*
H5B	0.2926	0.5210	0.3420	0.032*
H5C	0.3491	0.4228	0.3643	0.032*
Cd1	0.60861 (2)	0.27596 (2)	0.41882 (2)	0.01199 (5)
Cl1	0.54707 (3)	0.30385 (3)	0.57950 (3)	0.01619 (8)
Cl2	0.5000	0.15363 (3)	0.2500	0.01344 (10)
Cl3	0.5000	0.39855 (4)	0.2500	0.01852 (11)
Cl4	0.76617 (3)	0.35865 (2)	0.45006 (4)	0.01607 (8)
H2A	0.3944 (15)	0.3603 (16)	0.591 (2)	0.021 (5)*
H2B	0.3677 (16)	0.3540 (16)	0.694 (2)	0.026 (6)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
N1	0.0108 (6)	0.0151 (6)	0.0146 (6)	0.0020 (5)	0.0061 (5)	0.0016 (5)
N2	0.0120 (6)	0.0333 (8)	0.0139 (7)	0.0037 (5)	0.0076 (5)	0.0038 (6)
N3	0.0148 (6)	0.0161 (6)	0.0152 (6)	0.0008 (5)	0.0079 (5)	0.0010 (5)
C1	0.0143 (7)	0.0120 (7)	0.0141 (7)	0.0012 (5)	0.0072 (6)	−0.0027 (5)
C2	0.0118 (7)	0.0156 (7)	0.0196 (7)	0.0026 (5)	0.0083 (6)	−0.0001 (6)
C3	0.0140 (7)	0.0174 (7)	0.0151 (7)	0.0016 (6)	0.0073 (6)	0.0020 (6)
C4	0.0200 (8)	0.0249 (8)	0.0124 (7)	0.0067 (6)	0.0052 (6)	0.0027 (6)
C5	0.0232 (8)	0.0210 (8)	0.0254 (8)	0.0017 (6)	0.0163 (7)	0.0050 (7)
Cd1	0.00895 (7)	0.01692 (7)	0.01027 (7)	−0.00065 (3)	0.00457 (5)	−0.00147 (3)
Cl1	0.01164 (16)	0.02608 (19)	0.01180 (16)	0.00064 (14)	0.00620 (13)	−0.00316 (14)
Cl2	0.0121 (2)	0.0156 (2)	0.0115 (2)	0.000	0.00446 (18)	0.000
Cl3	0.0168 (2)	0.0176 (2)	0.0151 (2)	0.000	0.00209 (19)	0.000
Cl4	0.01132 (16)	0.01586 (16)	0.02072 (18)	−0.00045 (12)	0.00710 (14)	0.00232 (13)

Geometric parameters (Å, º)

N1—C1	1.3441 (19)	C4—H4A	0.9800
N1—C2	1.4649 (19)	C4—H4B	0.9800
N1—C3	1.4643 (19)	C4—H4C	0.9800
N2—C1	1.330 (2)	C5—H5A	0.9800
N2—H2A	0.83 (2)	C5—H5B	0.9800
N2—H2B	0.83 (2)	C5—H5C	0.9800
N3—C1	1.3360 (19)	Cd1—Cl1	2.4829 (4)
N3—C4	1.467 (2)	Cd1—Cl2	2.5829 (4)
N3—C5	1.465 (2)	Cd1—Cl3	2.5854 (4)
C2—H2C	0.9800	Cd1—Cl4	2.5323 (4)
C2—H2D	0.9800	Cd1—Cl4^i	2.6403 (4)
C2—H2E	0.9800	Cl2—Cd1^ii	2.5830 (4)
C3—H3A	0.9800	Cl3—Cd1^ii	2.5854 (4)
C3—H3B	0.9800	Cl4—Cd1^i	2.6402 (4)
C3—H3C	0.9800
C1—N1—C2	122.68 (13)	N3—C4—H4B	109.5
C1—N1—C3	121.14 (12)	N3—C4—H4C	109.5
C3—N1—C2	114.98 (12)	H4A—C4—H4B	109.5
C1—N2—H2A	118.6 (14)	H4A—C4—H4C	109.5
C1—N2—H2B	121.6 (15)	H4B—C4—H4C	109.5
H2A—N2—H2B	120 (2)	N3—C5—H5A	109.5
C1—N3—C4	122.47 (13)	N3—C5—H5B	109.5
C1—N3—C5	121.21 (14)	N3—C5—H5C	109.5
C5—N3—C4	115.83 (13)	H5A—C5—H5B	109.5
N2—C1—N1	119.26 (14)	H5A—C5—H5C	109.5
N2—C1—N3	119.57 (14)	H5B—C5—H5C	109.5
N3—C1—N1	121.14 (14)	Cl1—Cd1—Cl2	111.033 (10)
N1—C2—H2C	109.5	Cl1—Cd1—Cl3	98.115 (10)
N1—C2—H2D	109.5	Cl1—Cd1—Cl4^i	95.516 (13)
N1—C2—H2E	109.5	Cl1—Cd1—Cl4	118.137 (13)
H2C—C2—H2D	109.5	Cl2—Cd1—Cl3	85.262 (13)
H2C—C2—H2E	109.5	Cl2—Cd1—Cl4^i	89.152 (12)
H2D—C2—H2E	109.5	Cl3—Cd1—Cl4^i	166.347 (10)
N1—C3—H3A	109.5	Cl4—Cd1—Cl2	130.701 (9)
N1—C3—H3B	109.5	Cl4—Cd1—Cl3	91.126 (11)
N1—C3—H3C	109.5	Cl4—Cd1—Cl4^i	83.088 (12)
H3A—C3—H3B	109.5	Cd1—Cl2—Cd1^ii	94.798 (17)
H3A—C3—H3C	109.5	Cd1^ii—Cl3—Cd1	94.679 (18)
H3B—C3—H3C	109.5	Cd1—Cl4—Cd1^i	96.910 (13)
N3—C4—H4A	109.5
C2—N1—C1—N2	148.47 (15)	C4—N3—C1—N1	−27.1 (2)
C2—N1—C1—N3	−33.2 (2)	C4—N3—C1—N2	151.23 (15)
C3—N1—C1—N2	−18.4 (2)	C5—N3—C1—N1	161.27 (14)
C3—N1—C1—N3	159.92 (14)	C5—N3—C1—N2	−20.4 (2)

Symmetry codes: (i) −x+3/2, −y+1/2, −z+1; (ii) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2C···Cl4^iii	0.98	2.87	3.6567 (16)	138
C3—H3B···Cl1^iv	0.98	2.92	3.7614 (16)	144
C4—H4B···Cl4^ii	0.98	2.87	3.8347 (17)	169
N2—H2A···Cl1	0.83 (2)	2.51 (2)	3.2871 (15)	157 (2)
N2—H2B···Cl1^v	0.83 (2)	2.46 (2)	3.2710 (15)	164 (2)

Symmetry codes: (ii) −x+1, y, −z+1/2; (iii) −x+1, −y+1, −z+1; (iv) −x+1/2, −y+1/2, −z+1; (v) −x+1, y, −z+3/2.