New refinement of the crystal structure of Zn(NH₃)₂Cl₂ at 100 K

The crystal structure of Zn(NH₃)₂Cl₂ was redetermined at low temperature, revealing the positions of the hydrogen atoms.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](Zn-N) = 0.001 Å
• R factor = 0.015
• wR factor = 0.036
• Data-to-parameter ratio = 28.3

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level C
PLAT352_ALERT_3_C Short  N-H (X0.87,N1.01A)  N1       - H1B      .       0.74 Ang.
PLAT420_ALERT_2_C D-H Without Acceptor       N1       --H1B      .     Please Check
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1A      ..CL1      .       2.90 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1B      ..CL1      .       2.95 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1B      ..CL1      .       2.95 Ang.
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report

Alert level G
PLAT019_ALERT_1_G _diffrn_measured_fraction_theta_full/*_max < 1.0      0.993 Report
PLAT794_ALERT_5_G Tentative Bond Valency for Zn1       (II)      .       1.88 Info
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          3 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
   3 ALERT level G = General information/check it is not something unexpected

   1 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
   3 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

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Computing details

Data collection: CrysAlis PRO (Rigaku OD, 2019); cell refinement: CrysAlis PRO (Rigaku OD, 2019); data reduction: CrysAlis PRO (Rigaku OD, 2019); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Diamminedichloridozinc

Crystal data

[ZnCl2(NH3)2]	Dx = 2.165 Mg m^−3
Mr = 170.34	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Imma	Cell parameters from 1597 reflections
a = 7.7077 (2) Å	θ = 3.6–37.4°
b = 8.0226 (2) Å	µ = 5.56 mm^−1
c = 8.4526 (3) Å	T = 100 K
V = 522.67 (3) Å^3	Irregular, colourless
Z = 4	0.26 × 0.18 × 0.16 mm
F(000) = 336

Data collection

Rigaku SuperNOVA diffractometer	678 reflections with I > 2σ(I)
Radiation source: micro-focus sealed X-ray tube	Rint = 0.017
ω scans	θmax = 36.3°, θmin = 3.5°
Absorption correction: analytical (CrysAlis PRO; Rigaku OD, 2019)	h = −12→8
Tmin = 0.277, Tmax = 0.454	k = −13→12
2303 measured reflections	l = −12→14
708 independent reflections

Refinement

Refinement on F^2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.015	w = 1/[σ^2(Fo^2) + (0.0188P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.036	(Δ/σ)max = 0.001
S = 1.04	Δρmax = 0.50 e Å^−3
708 reflections	Δρmin = −0.55 e Å^−3
25 parameters	Extinction correction: SHELXL2018 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0043 (6)
Primary atom site location: structure-invariant direct methods

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
Zn1	0.500000	0.250000	0.61168 (2)	0.01163 (6)
Cl1	0.500000	0.47954 (3)	0.76915 (3)	0.01375 (6)
N1	0.28237 (15)	0.250000	0.47949 (13)	0.01603 (17)
H1A	0.274 (3)	0.3281 (19)	0.416 (2)	0.045 (4)*
H1B	0.206 (5)	0.250000	0.533 (4)	0.090 (11)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.01002 (9)	0.01352 (9)	0.01134 (9)	0.000	0.000	0.000
Cl1	0.01288 (11)	0.01346 (11)	0.01490 (11)	0.000	0.000	−0.00253 (7)
N1	0.0136 (4)	0.0211 (4)	0.0134 (4)	0.000	−0.0016 (3)	0.000

Geometric parameters (Å, º)

Zn1—Cl1^i	2.2722 (3)	N1—H1A^ii	0.825 (17)
Zn1—Cl1	2.2722 (3)	N1—H1A	0.825 (17)
Zn1—N1^i	2.0155 (11)	N1—H1B	0.74 (4)
Zn1—N1	2.0155 (11)
Cl1^i—Zn1—Cl1	108.282 (14)	Zn1—N1—H1A^ii	115.0 (13)
N1—Zn1—Cl1	108.951 (17)	Zn1—N1—H1A	115.0 (13)
N1^i—Zn1—Cl1^i	108.951 (17)	Zn1—N1—H1B	109 (3)
N1—Zn1—Cl1^i	108.951 (17)	H1A—N1—H1A^ii	99 (2)
N1^i—Zn1—Cl1	108.950 (17)	H1A—N1—H1B	109 (2)
N1^i—Zn1—N1	112.66 (7)	H1B—N1—H1A^ii	109 (2)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1^iii	0.825 (17)	2.806 (18)	3.4552 (9)	137.0 (17)
N1—H1A···Cl1^iv	0.825 (17)	2.897 (18)	3.5505 (9)	137.6 (16)
N1—H1B···Cl1^v	0.74 (4)	2.95 (3)	3.5556 (10)	141 (1)
N1—H1B···Cl1^vi	0.74 (4)	2.95 (3)	3.5556 (10)	141 (1)

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