Bis(tetra­methyl­ammonium) tetra­chlorido­zincate(II), phase VI

Curtiss, A.B.S.; Musie, G.T.; Powell, D.R.

doi:10.1107/S1600536807065828

Bis(tetramethylammonium) tetrachloridozincate(II), phase VI

A. B. S. Curtiss, G. T. Musie and D. R. Powell

Phase VI of bis(tetramethylammonium) tetrachlorozincate(II), (C₄H₁₂N)₂[ZnCl₄], contains three formula units per asymmetric unit. Several short C—H

Cl contacts [2.70 (3) and 2.72 (4) Å] are observed, but they are believed to participate only in van der Waals interactions. The crystal studied exhibited inversion twinning.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807065828/mg2041sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807065828/mg2041Isup2.hkl Contains datablock I

CCDC reference: 674345

checkCIF report

Key indicators

Single-crystal X-ray study
T = 100 K
Mean (N-C) = 0.003 Å
R factor = 0.026
wR factor = 0.055
Data-to-parameter ratio = 23.6

checkCIF/PLATON results

No syntax errors found



Alert level C
STRVA01_ALERT_4_C           Flack test results are ambiguous.
           From the CIF: _refine_ls_abs_structure_Flack    0.611
           From the CIF: _refine_ls_abs_structure_Flack_su    0.006
PLAT033_ALERT_2_C Flack Parameter Value Deviates from zero .......       0.61
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........         72

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           26.00
           From the CIF: _reflns_number_total               9616
           Count of symmetry unique reflns         5398
           Completeness (_total/calc)            178.14%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      4218
           Fraction of Friedel pairs measured     0.781
           Are heavy atom types Z>Si present        yes

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 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
   0 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

Bis(tetramethylammonium) tetrachlorozincate(II) undergoes five solid-solid phase transitions with decreasing temperature according to a calorimetric study by Ruiz-Larrea et al. (1981). The room temperature phase I crystallized in the space group Pnma with a = 12.276 (2), b = 8.998 (2), and c = 15.541 (2) Å (Wiesner et al., 1967). Weak incommensurate lattice spots in phases II, III, and IV have shown that these two phases are small distortions of the room temperature phase (Madariaga et al., 1987). Similarly, phase V was found to be an incommensurately modulated structure related to phase I (Zuñiga et al., 1989).

No evidence of superlattice spots were observed in the frame data for phase VI. Short C—H···Cl contacts were observed, but because of the very large estimated pK_a of 42 for the protons of the cations (Zhang & Bordwell, 1994), it is unlikely that any of these contacts are weak hydrogen bonds. There were three formula units in the asymmetric unit of the cell (Fig. 1).

Related literature top

For related literature, see: Madariaga et al. (1987); Ruiz-Larrea et al. (1981); Wiesner et al. (1967); Zuñiga et al. (1989); Zhang & Bordwell (1994).

Experimental top

Single crystals of bis(tetramethylammonium) tetrachlorozincate(II) were grown by slow diffusion of diethyl ether into a methanol solution of ZnCl₂ and N(CH₃)₄OH in a 1:3 mole ratio over the course of three days.

Structure description top

For related literature, see: Madariaga et al. (1987); Ruiz-Larrea et al. (1981); Wiesner et al. (1967); Zuñiga et al. (1989); Zhang & Bordwell (1994).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL (Sheldrick, 2000); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL (Sheldrick, 2000).

Figures top

Fig. 1. View of the unique atoms showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms are omitted for clarity.

bis(tetramethylammonium) tetrachlorozincate(II) top

Crystal data top

(C₄H₁₂N)₂[ZnCl₄]	F(000) = 2208
M_r = 355.46	D_x = 1.442 Mg m⁻³
Orthorhombic, P2₁2₁2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 6850 reflections
a = 8.9114 (18) Å	θ = 2.5–28.2°
b = 15.105 (3) Å	µ = 2.13 mm⁻¹
c = 36.493 (7) Å	T = 100 K
V = 4912.2 (17) Å³	Plate, colourless
Z = 12	0.36 × 0.24 × 0.04 mm

Data collection top

Bruker APEX CCD diffractometer	9616 independent reflections
Radiation source: fine-focus sealed tube	9039 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.038
\ scans	θ_max = 26.0°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 2007)	h = −10→10
T_min = 0.512, T_max = 0.918	k = −18→18
32538 measured reflections	l = −44→45

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.026	H-atom parameters constrained
wR(F²) = 0.055	w = 1/[σ²(F_o²) + (0.022P)²] where P = (F_o² + 2F_c²)/3
S = 1.00	(Δ/σ)_max < 0.001
9616 reflections	Δρ_max = 0.43 e Å⁻³
407 parameters	Δρ_min = −0.29 e Å⁻³
0 restraints	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.611 (6)

Crystal data top

(C₄H₁₂N)₂[ZnCl₄]	V = 4912.2 (17) Å³
M_r = 355.46	Z = 12
Orthorhombic, P2₁2₁2₁	Mo Kα radiation
a = 8.9114 (18) Å	µ = 2.13 mm⁻¹
b = 15.105 (3) Å	T = 100 K
c = 36.493 (7) Å	0.36 × 0.24 × 0.04 mm

Data collection top

Bruker APEX CCD diffractometer	9616 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2007)	9039 reflections with I > 2σ(I)
T_min = 0.512, T_max = 0.918	R_int = 0.038
32538 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	H-atom parameters constrained
wR(F²) = 0.055	Δρ_max = 0.43 e Å⁻³
S = 1.00	Δρ_min = −0.29 e Å⁻³
9616 reflections	Absolute structure: Flack (1983)
407 parameters	Absolute structure parameter: 0.611 (6)
0 restraints

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Zn1A	0.22269 (3)	0.833130 (18)	0.249954 (7)	0.01451 (7)
Cl1A	0.27151 (7)	0.83942 (4)	0.311249 (16)	0.01927 (14)
Cl2A	0.42172 (7)	0.89470 (4)	0.220415 (17)	0.02094 (15)
Cl3A	0.01026 (7)	0.91090 (4)	0.236224 (17)	0.02043 (14)
Cl4A	0.18901 (8)	0.69109 (4)	0.231878 (17)	0.02295 (15)
Zn1B	0.80374 (3)	0.648812 (18)	0.085633 (7)	0.01432 (7)
Cl1B	0.78781 (7)	0.67180 (4)	0.024348 (16)	0.01814 (13)
Cl2B	0.99810 (7)	0.55514 (4)	0.098555 (17)	0.01982 (15)
Cl3B	0.58278 (8)	0.59089 (4)	0.106043 (18)	0.02098 (15)
Cl4B	0.84775 (8)	0.77752 (4)	0.115946 (17)	0.01842 (14)
Zn1C	0.27960 (3)	0.148178 (18)	0.084326 (7)	0.01390 (7)
Cl1C	0.30736 (7)	0.14537 (4)	0.145927 (16)	0.01915 (14)
Cl2C	0.32460 (8)	0.28462 (4)	0.060498 (18)	0.02114 (15)
Cl3C	0.44003 (8)	0.04975 (4)	0.057901 (18)	0.02362 (16)
Cl4C	0.04001 (7)	0.10798 (4)	0.069889 (17)	0.02188 (15)
N1D	0.7769 (2)	0.34272 (13)	0.04975 (5)	0.0161 (5)
C1D	0.7608 (3)	0.34836 (17)	0.09057 (6)	0.0214 (6)
H1D1	0.6561	0.3374	0.0974	0.032*
H1D2	0.7906	0.4075	0.0989	0.032*
H1D3	0.8253	0.3039	0.1021	0.032*
C2D	0.7222 (3)	0.25421 (16)	0.03673 (7)	0.0222 (6)
H2D1	0.7274	0.2518	0.0099	0.033*
H2D2	0.6181	0.2455	0.0446	0.033*
H2D3	0.7854	0.2074	0.0471	0.033*
C3D	0.6849 (3)	0.41380 (17)	0.03245 (7)	0.0268 (7)
H3D1	0.6954	0.4106	0.0058	0.040*
H3D2	0.7197	0.4717	0.0411	0.040*
H3D3	0.5793	0.4058	0.0391	0.040*
C4D	0.9376 (3)	0.35435 (19)	0.03958 (7)	0.0248 (6)
H4D1	0.9967	0.3053	0.0496	0.037*
H4D2	0.9747	0.4104	0.0496	0.037*
H4D3	0.9473	0.3550	0.0128	0.037*
N1E	0.2499 (2)	0.40749 (14)	0.17102 (5)	0.0148 (5)
C1E	0.1088 (3)	0.36434 (17)	0.15805 (8)	0.0252 (7)
H1E1	0.0675	0.3979	0.1374	0.038*
H1E2	0.0355	0.3631	0.1781	0.038*
H1E3	0.1306	0.3037	0.1502	0.038*
C2E	0.3602 (3)	0.41315 (18)	0.14052 (7)	0.0278 (7)
H2E1	0.3172	0.4477	0.1204	0.042*
H2E2	0.3842	0.3534	0.1318	0.042*
H2E3	0.4520	0.4420	0.1493	0.042*
C3E	0.2129 (3)	0.49855 (16)	0.18458 (7)	0.0218 (6)
H3E1	0.3047	0.5277	0.1931	0.033*
H3E2	0.1412	0.4943	0.2049	0.033*
H3E3	0.1685	0.5332	0.1646	0.033*
C4E	0.3153 (3)	0.35468 (17)	0.20164 (7)	0.0233 (6)
H4E1	0.3432	0.2958	0.1926	0.035*
H4E2	0.2410	0.3487	0.2213	0.035*
H4E3	0.4046	0.3848	0.2111	0.035*
N1F	0.2919 (3)	0.82358 (13)	0.11507 (5)	0.0179 (5)
C1F	0.2556 (3)	0.74168 (17)	0.13618 (8)	0.0279 (7)
H1F1	0.2800	0.7508	0.1621	0.042*
H1F2	0.3146	0.6921	0.1266	0.042*
H1F3	0.1485	0.7284	0.1337	0.042*
C2F	0.4559 (3)	0.84202 (19)	0.11789 (8)	0.0283 (7)
H2F1	0.4800	0.8957	0.1040	0.042*
H2F2	0.5124	0.7919	0.1079	0.042*
H2F3	0.4831	0.8506	0.1437	0.042*
C3F	0.2049 (3)	0.89951 (17)	0.13031 (8)	0.0284 (7)
H3F1	0.0973	0.8864	0.1288	0.043*
H3F2	0.2269	0.9530	0.1161	0.043*
H3F3	0.2332	0.9089	0.1560	0.043*
C4F	0.2506 (3)	0.8116 (2)	0.07569 (7)	0.0379 (8)
H4F1	0.2741	0.8658	0.0621	0.057*
H4F2	0.1429	0.7992	0.0738	0.057*
H4F3	0.3075	0.7620	0.0654	0.057*
N1G	0.7277 (2)	0.63485 (14)	0.21747 (5)	0.0161 (5)
C1G	0.5783 (3)	0.5939 (2)	0.21077 (8)	0.0304 (7)
H1G1	0.5017	0.6258	0.2248	0.046*
H1G2	0.5805	0.5318	0.2185	0.046*
H1G3	0.5544	0.5973	0.1846	0.046*
C2G	0.7243 (4)	0.73057 (17)	0.20696 (7)	0.0286 (7)
H2G1	0.8219	0.7576	0.2122	0.043*
H2G2	0.6461	0.7610	0.2210	0.043*
H2G3	0.7026	0.7359	0.1807	0.043*
C3G	0.8431 (3)	0.58795 (18)	0.19485 (7)	0.0244 (7)
H3G1	0.8174	0.5935	0.1688	0.037*
H3G2	0.8456	0.5252	0.2017	0.037*
H3G3	0.9419	0.6145	0.1992	0.037*
C4G	0.7650 (3)	0.62664 (18)	0.25733 (7)	0.0249 (7)
H4G1	0.6886	0.6574	0.2719	0.037*
H4G2	0.8634	0.6532	0.2620	0.037*
H4G3	0.7673	0.5639	0.2642	0.037*
N1H	0.2840 (2)	0.56575 (13)	−0.00491 (5)	0.0147 (5)
C1H	0.2778 (3)	0.46942 (16)	0.00445 (7)	0.0219 (6)
H1H1	0.2724	0.4624	0.0311	0.033*
H1H2	0.3682	0.4400	−0.0048	0.033*
H1H3	0.1889	0.4428	−0.0068	0.033*
C2H	0.1461 (3)	0.61057 (18)	0.00861 (8)	0.0264 (7)
H2H1	0.0579	0.5847	−0.0033	0.040*
H2H2	0.1515	0.6739	0.0029	0.040*
H2H3	0.1381	0.6027	0.0352	0.040*
C3H	0.2935 (3)	0.57694 (17)	−0.04539 (6)	0.0230 (6)
H3H1	0.3835	0.5470	−0.0546	0.035*
H3H2	0.2988	0.6401	−0.0513	0.035*
H3H3	0.2043	0.5510	−0.0569	0.035*
C4H	0.4208 (3)	0.60584 (18)	0.01198 (8)	0.0301 (7)
H4H1	0.5105	0.5767	0.0022	0.045*
H4H2	0.4172	0.5980	0.0386	0.045*
H4H3	0.4244	0.6692	0.0062	0.045*
N1I	0.7744 (2)	1.07188 (13)	0.16264 (5)	0.0150 (5)
C1I	0.9184 (3)	1.11122 (17)	0.17517 (7)	0.0216 (6)
H1I1	0.9615	1.0744	0.1946	0.032*
H1I2	0.9002	1.1710	0.1846	0.032*
H1I3	0.9886	1.1143	0.1545	0.032*
C2I	0.6673 (3)	1.06734 (18)	0.19391 (7)	0.0260 (7)
H2I1	0.7082	1.0285	0.2130	0.039*
H2I2	0.5711	1.0437	0.1854	0.039*
H2I3	0.6523	1.1268	0.2040	0.039*
C3I	0.8031 (4)	0.98137 (16)	0.14806 (7)	0.0286 (7)
H3I1	0.8714	0.9851	0.1271	0.043*
H3I2	0.7081	0.9547	0.1403	0.043*
H3I3	0.8487	0.9448	0.1672	0.043*
C4I	0.7082 (3)	1.12811 (17)	0.13312 (7)	0.0233 (6)
H4I1	0.7788	1.1323	0.1126	0.035*
H4I2	0.6880	1.1875	0.1428	0.035*
H4I3	0.6142	1.1014	0.1246	0.035*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1A	0.01419 (16)	0.01415 (15)	0.01521 (15)	0.00001 (13)	0.00065 (12)	0.00035 (12)
Cl1A	0.0185 (3)	0.0239 (3)	0.0154 (3)	−0.0007 (3)	−0.0014 (3)	0.0007 (3)
Cl2A	0.0165 (3)	0.0255 (4)	0.0209 (3)	−0.0037 (3)	0.0028 (3)	0.0024 (3)
Cl3A	0.0162 (3)	0.0223 (3)	0.0227 (3)	0.0038 (3)	−0.0018 (3)	0.0021 (3)
Cl4A	0.0318 (4)	0.0155 (3)	0.0215 (3)	−0.0028 (3)	−0.0004 (3)	−0.0019 (3)
Zn1B	0.01474 (15)	0.01379 (14)	0.01444 (14)	−0.00018 (13)	0.00038 (13)	0.00079 (12)
Cl1B	0.0189 (3)	0.0207 (3)	0.0149 (3)	0.0009 (3)	−0.0001 (3)	0.0016 (3)
Cl2B	0.0205 (4)	0.0189 (3)	0.0201 (3)	0.0046 (3)	−0.0015 (3)	0.0023 (3)
Cl3B	0.0177 (4)	0.0240 (3)	0.0212 (3)	−0.0048 (3)	0.0029 (3)	0.0013 (3)
Cl4B	0.0204 (4)	0.0157 (3)	0.0192 (3)	−0.0012 (3)	−0.0008 (3)	−0.0020 (3)
Zn1C	0.01250 (15)	0.01516 (14)	0.01404 (14)	0.00037 (13)	0.00063 (13)	−0.00004 (12)
Cl1C	0.0193 (3)	0.0243 (3)	0.0138 (3)	0.0011 (3)	−0.0003 (3)	−0.0010 (3)
Cl2C	0.0212 (4)	0.0187 (3)	0.0235 (3)	−0.0020 (3)	−0.0005 (3)	0.0038 (3)
Cl3C	0.0237 (4)	0.0247 (4)	0.0225 (3)	0.0072 (3)	0.0054 (3)	−0.0017 (3)
Cl4C	0.0145 (4)	0.0288 (4)	0.0224 (3)	−0.0039 (3)	−0.0024 (3)	−0.0007 (3)
N1D	0.0156 (11)	0.0178 (11)	0.0150 (11)	−0.0001 (10)	0.0002 (9)	−0.0003 (9)
C1D	0.0268 (16)	0.0229 (14)	0.0146 (13)	−0.0023 (12)	0.0036 (11)	−0.0007 (11)
C2D	0.0252 (16)	0.0192 (14)	0.0221 (15)	−0.0005 (13)	−0.0004 (13)	−0.0040 (11)
C3D	0.0293 (19)	0.0248 (15)	0.0262 (16)	0.0108 (14)	−0.0038 (14)	0.0033 (12)
C4D	0.0153 (15)	0.0317 (16)	0.0274 (15)	−0.0029 (13)	0.0060 (12)	0.0017 (13)
N1E	0.0126 (13)	0.0169 (11)	0.0150 (11)	0.0003 (9)	0.0010 (9)	−0.0013 (9)
C1E	0.0142 (15)	0.0238 (15)	0.0377 (17)	−0.0041 (12)	−0.0099 (13)	0.0033 (13)
C2E	0.0288 (18)	0.0265 (16)	0.0280 (16)	−0.0022 (14)	0.0104 (14)	−0.0014 (13)
C3E	0.0208 (16)	0.0181 (14)	0.0265 (15)	0.0017 (13)	−0.0006 (13)	−0.0041 (12)
C4E	0.0224 (16)	0.0277 (15)	0.0200 (14)	0.0081 (14)	−0.0014 (12)	0.0011 (12)
N1F	0.0177 (12)	0.0198 (11)	0.0163 (11)	−0.0004 (11)	−0.0012 (10)	−0.0019 (9)
C1F	0.0236 (17)	0.0210 (15)	0.0392 (18)	0.0014 (12)	0.0038 (14)	0.0097 (13)
C2F	0.0157 (15)	0.0356 (17)	0.0336 (16)	−0.0034 (14)	−0.0017 (12)	0.0066 (14)
C3F	0.0269 (17)	0.0231 (15)	0.0352 (17)	0.0040 (14)	−0.0053 (15)	−0.0052 (13)
C4F	0.035 (2)	0.060 (2)	0.0189 (16)	−0.0039 (16)	−0.0039 (13)	−0.0064 (15)
N1G	0.0156 (12)	0.0180 (11)	0.0146 (11)	0.0013 (10)	−0.0001 (9)	0.0000 (9)
C1G	0.0191 (16)	0.0458 (19)	0.0265 (16)	−0.0087 (15)	−0.0016 (13)	0.0008 (14)
C2G	0.044 (2)	0.0162 (14)	0.0253 (16)	0.0071 (14)	0.0024 (15)	0.0030 (12)
C3G	0.0211 (16)	0.0253 (15)	0.0269 (16)	0.0051 (13)	0.0043 (13)	−0.0059 (13)
C4G	0.0328 (18)	0.0256 (15)	0.0164 (14)	−0.0001 (13)	−0.0070 (12)	0.0015 (12)
N1H	0.0152 (12)	0.0142 (10)	0.0148 (11)	−0.0031 (10)	−0.0011 (10)	0.0020 (9)
C1H	0.0238 (16)	0.0156 (13)	0.0263 (15)	0.0000 (13)	0.0017 (13)	0.0049 (11)
C2H	0.0246 (17)	0.0232 (15)	0.0313 (16)	0.0063 (13)	0.0131 (13)	−0.0006 (13)
C3H	0.0274 (17)	0.0254 (15)	0.0163 (13)	−0.0005 (14)	0.0027 (13)	0.0053 (11)
C4H	0.0286 (18)	0.0240 (16)	0.0377 (18)	−0.0052 (14)	−0.0139 (14)	0.0024 (14)
N1I	0.0118 (11)	0.0180 (11)	0.0153 (11)	−0.0013 (9)	−0.0015 (9)	−0.0001 (9)
C1I	0.0171 (15)	0.0231 (15)	0.0246 (15)	−0.0039 (13)	−0.0024 (12)	−0.0027 (12)
C2I	0.0228 (17)	0.0345 (17)	0.0207 (15)	−0.0058 (14)	0.0032 (13)	0.0023 (13)
C3I	0.0325 (19)	0.0198 (14)	0.0336 (17)	0.0005 (14)	−0.0048 (15)	−0.0094 (13)
C4I	0.0198 (15)	0.0262 (15)	0.0238 (14)	0.0029 (13)	−0.0002 (13)	0.0043 (12)

Geometric parameters (Å, º) top

Zn1A—Cl4A	2.2645 (8)	C3F—H3F1	0.9800
Zn1A—Cl2A	2.2743 (8)	C3F—H3F2	0.9800
Zn1A—Cl1A	2.2807 (8)	C3F—H3F3	0.9800
Zn1A—Cl3A	2.2836 (8)	C4F—H4F1	0.9800
Zn1B—Cl1B	2.2677 (8)	C4F—H4F2	0.9800
Zn1B—Cl4B	2.2709 (7)	C4F—H4F3	0.9800
Zn1B—Cl3B	2.2797 (8)	N1G—C1G	1.488 (3)
Zn1B—Cl2B	2.2857 (8)	N1G—C2G	1.496 (3)
Zn1C—Cl1C	2.2620 (8)	N1G—C3G	1.497 (3)
Zn1C—Cl2C	2.2726 (8)	N1G—C4G	1.497 (3)
Zn1C—Cl3C	2.2770 (8)	C1G—H1G1	0.9800
Zn1C—Cl4C	2.2814 (8)	C1G—H1G2	0.9800
N1D—C4D	1.490 (3)	C1G—H1G3	0.9800
N1D—C3D	1.491 (3)	C2G—H2G1	0.9800
N1D—C1D	1.499 (3)	C2G—H2G2	0.9800
N1D—C2D	1.500 (3)	C2G—H2G3	0.9800
C1D—H1D1	0.9800	C3G—H3G1	0.9800
C1D—H1D2	0.9800	C3G—H3G2	0.9800
C1D—H1D3	0.9800	C3G—H3G3	0.9800
C2D—H2D1	0.9800	C4G—H4G1	0.9800
C2D—H2D2	0.9800	C4G—H4G2	0.9800
C2D—H2D3	0.9800	C4G—H4G3	0.9800
C3D—H3D1	0.9800	N1H—C2H	1.487 (3)
C3D—H3D2	0.9800	N1H—C3H	1.489 (3)
C3D—H3D3	0.9800	N1H—C4H	1.494 (3)
C4D—H4D1	0.9800	N1H—C1H	1.496 (3)
C4D—H4D2	0.9800	C1H—H1H1	0.9800
C4D—H4D3	0.9800	C1H—H1H2	0.9800
N1E—C2E	1.488 (3)	C1H—H1H3	0.9800
N1E—C4E	1.491 (3)	C2H—H2H1	0.9800
N1E—C1E	1.494 (3)	C2H—H2H2	0.9800
N1E—C3E	1.498 (3)	C2H—H2H3	0.9800
C1E—H1E1	0.9800	C3H—H3H1	0.9800
C1E—H1E2	0.9800	C3H—H3H2	0.9800
C1E—H1E3	0.9800	C3H—H3H3	0.9800
C2E—H2E1	0.9800	C4H—H4H1	0.9800
C2E—H2E2	0.9800	C4H—H4H2	0.9800
C2E—H2E3	0.9800	C4H—H4H3	0.9800
C3E—H3E1	0.9800	N1I—C1I	1.486 (3)
C3E—H3E2	0.9800	N1I—C3I	1.489 (3)
C3E—H3E3	0.9800	N1I—C2I	1.490 (3)
C4E—H4E1	0.9800	N1I—C4I	1.493 (3)
C4E—H4E2	0.9800	C1I—H1I1	0.9800
C4E—H4E3	0.9800	C1I—H1I2	0.9800
N1F—C2F	1.491 (3)	C1I—H1I3	0.9800
N1F—C3F	1.492 (3)	C2I—H2I1	0.9800
N1F—C1F	1.493 (3)	C2I—H2I2	0.9800
N1F—C4F	1.494 (3)	C2I—H2I3	0.9800
C1F—H1F1	0.9800	C3I—H3I1	0.9800
C1F—H1F2	0.9800	C3I—H3I2	0.9800
C1F—H1F3	0.9800	C3I—H3I3	0.9800
C2F—H2F1	0.9800	C4I—H4I1	0.9800
C2F—H2F2	0.9800	C4I—H4I2	0.9800
C2F—H2F3	0.9800	C4I—H4I3	0.9800

Cl4A—Zn1A—Cl2A	110.65 (3)	N1F—C3F—H3F3	109.5
Cl4A—Zn1A—Cl1A	110.51 (3)	H3F1—C3F—H3F3	109.5
Cl2A—Zn1A—Cl1A	107.40 (3)	H3F2—C3F—H3F3	109.5
Cl4A—Zn1A—Cl3A	108.27 (3)	N1F—C4F—H4F1	109.5
Cl2A—Zn1A—Cl3A	109.40 (3)	N1F—C4F—H4F2	109.5
Cl1A—Zn1A—Cl3A	110.60 (3)	H4F1—C4F—H4F2	109.5
Cl1B—Zn1B—Cl4B	111.11 (3)	N1F—C4F—H4F3	109.5
Cl1B—Zn1B—Cl3B	109.08 (3)	H4F1—C4F—H4F3	109.5
Cl4B—Zn1B—Cl3B	108.58 (3)	H4F2—C4F—H4F3	109.5
Cl1B—Zn1B—Cl2B	110.23 (3)	C1G—N1G—C2G	109.9 (2)
Cl4B—Zn1B—Cl2B	107.37 (3)	C1G—N1G—C3G	109.1 (2)
Cl3B—Zn1B—Cl2B	110.46 (3)	C2G—N1G—C3G	109.3 (2)
Cl1C—Zn1C—Cl2C	112.21 (3)	C1G—N1G—C4G	108.9 (2)
Cl1C—Zn1C—Cl3C	109.88 (3)	C2G—N1G—C4G	109.50 (19)
Cl2C—Zn1C—Cl3C	108.62 (3)	C3G—N1G—C4G	110.1 (2)
Cl1C—Zn1C—Cl4C	109.08 (3)	N1G—C1G—H1G1	109.5
Cl2C—Zn1C—Cl4C	108.55 (3)	N1G—C1G—H1G2	109.5
Cl3C—Zn1C—Cl4C	108.42 (3)	H1G1—C1G—H1G2	109.5
C4D—N1D—C3D	109.7 (2)	N1G—C1G—H1G3	109.5
C4D—N1D—C1D	109.4 (2)	H1G1—C1G—H1G3	109.5
C3D—N1D—C1D	109.11 (19)	H1G2—C1G—H1G3	109.5
C4D—N1D—C2D	109.8 (2)	N1G—C2G—H2G1	109.5
C3D—N1D—C2D	109.2 (2)	N1G—C2G—H2G2	109.5
C1D—N1D—C2D	109.54 (19)	H2G1—C2G—H2G2	109.5
N1D—C1D—H1D1	109.5	N1G—C2G—H2G3	109.5
N1D—C1D—H1D2	109.5	H2G1—C2G—H2G3	109.5
H1D1—C1D—H1D2	109.5	H2G2—C2G—H2G3	109.5
N1D—C1D—H1D3	109.5	N1G—C3G—H3G1	109.5
H1D1—C1D—H1D3	109.5	N1G—C3G—H3G2	109.5
H1D2—C1D—H1D3	109.5	H3G1—C3G—H3G2	109.5
N1D—C2D—H2D1	109.5	N1G—C3G—H3G3	109.5
N1D—C2D—H2D2	109.5	H3G1—C3G—H3G3	109.5
H2D1—C2D—H2D2	109.5	H3G2—C3G—H3G3	109.5
N1D—C2D—H2D3	109.5	N1G—C4G—H4G1	109.5
H2D1—C2D—H2D3	109.5	N1G—C4G—H4G2	109.5
H2D2—C2D—H2D3	109.5	H4G1—C4G—H4G2	109.5
N1D—C3D—H3D1	109.5	N1G—C4G—H4G3	109.5
N1D—C3D—H3D2	109.5	H4G1—C4G—H4G3	109.5
H3D1—C3D—H3D2	109.5	H4G2—C4G—H4G3	109.5
N1D—C3D—H3D3	109.5	C2H—N1H—C3H	108.9 (2)
H3D1—C3D—H3D3	109.5	C2H—N1H—C4H	110.7 (2)
H3D2—C3D—H3D3	109.5	C3H—N1H—C4H	108.5 (2)
N1D—C4D—H4D1	109.5	C2H—N1H—C1H	109.7 (2)
N1D—C4D—H4D2	109.5	C3H—N1H—C1H	109.81 (19)
H4D1—C4D—H4D2	109.5	C4H—N1H—C1H	109.3 (2)
N1D—C4D—H4D3	109.5	N1H—C1H—H1H1	109.5
H4D1—C4D—H4D3	109.5	N1H—C1H—H1H2	109.5
H4D2—C4D—H4D3	109.5	H1H1—C1H—H1H2	109.5
C2E—N1E—C4E	109.5 (2)	N1H—C1H—H1H3	109.5
C2E—N1E—C1E	110.2 (2)	H1H1—C1H—H1H3	109.5
C4E—N1E—C1E	109.4 (2)	H1H2—C1H—H1H3	109.5
C2E—N1E—C3E	109.9 (2)	N1H—C2H—H2H1	109.5
C4E—N1E—C3E	109.25 (19)	N1H—C2H—H2H2	109.5
C1E—N1E—C3E	108.6 (2)	H2H1—C2H—H2H2	109.5
N1E—C1E—H1E1	109.5	N1H—C2H—H2H3	109.5
N1E—C1E—H1E2	109.5	H2H1—C2H—H2H3	109.5
H1E1—C1E—H1E2	109.5	H2H2—C2H—H2H3	109.5
N1E—C1E—H1E3	109.5	N1H—C3H—H3H1	109.5
H1E1—C1E—H1E3	109.5	N1H—C3H—H3H2	109.5
H1E2—C1E—H1E3	109.5	H3H1—C3H—H3H2	109.5
N1E—C2E—H2E1	109.5	N1H—C3H—H3H3	109.5
N1E—C2E—H2E2	109.5	H3H1—C3H—H3H3	109.5
H2E1—C2E—H2E2	109.5	H3H2—C3H—H3H3	109.5
N1E—C2E—H2E3	109.5	N1H—C4H—H4H1	109.5
H2E1—C2E—H2E3	109.5	N1H—C4H—H4H2	109.5
H2E2—C2E—H2E3	109.5	H4H1—C4H—H4H2	109.5
N1E—C3E—H3E1	109.5	N1H—C4H—H4H3	109.5
N1E—C3E—H3E2	109.5	H4H1—C4H—H4H3	109.5
H3E1—C3E—H3E2	109.5	H4H2—C4H—H4H3	109.5
N1E—C3E—H3E3	109.5	C1I—N1I—C3I	109.2 (2)
H3E1—C3E—H3E3	109.5	C1I—N1I—C2I	109.63 (19)
H3E2—C3E—H3E3	109.5	C3I—N1I—C2I	110.0 (2)
N1E—C4E—H4E1	109.5	C1I—N1I—C4I	109.6 (2)
N1E—C4E—H4E2	109.5	C3I—N1I—C4I	109.4 (2)
H4E1—C4E—H4E2	109.5	C2I—N1I—C4I	109.0 (2)
N1E—C4E—H4E3	109.5	N1I—C1I—H1I1	109.5
H4E1—C4E—H4E3	109.5	N1I—C1I—H1I2	109.5
H4E2—C4E—H4E3	109.5	H1I1—C1I—H1I2	109.5
C2F—N1F—C3F	109.9 (2)	N1I—C1I—H1I3	109.5
C2F—N1F—C1F	109.4 (2)	H1I1—C1I—H1I3	109.5
C3F—N1F—C1F	109.4 (2)	H1I2—C1I—H1I3	109.5
C2F—N1F—C4F	109.3 (2)	N1I—C2I—H2I1	109.5
C3F—N1F—C4F	108.9 (2)	N1I—C2I—H2I2	109.5
C1F—N1F—C4F	110.0 (2)	H2I1—C2I—H2I2	109.5
N1F—C1F—H1F1	109.5	N1I—C2I—H2I3	109.5
N1F—C1F—H1F2	109.5	H2I1—C2I—H2I3	109.5
H1F1—C1F—H1F2	109.5	H2I2—C2I—H2I3	109.5
N1F—C1F—H1F3	109.5	N1I—C3I—H3I1	109.5
H1F1—C1F—H1F3	109.5	N1I—C3I—H3I2	109.5
H1F2—C1F—H1F3	109.5	H3I1—C3I—H3I2	109.5
N1F—C2F—H2F1	109.5	N1I—C3I—H3I3	109.5
N1F—C2F—H2F2	109.5	H3I1—C3I—H3I3	109.5
H2F1—C2F—H2F2	109.5	H3I2—C3I—H3I3	109.5
N1F—C2F—H2F3	109.5	N1I—C4I—H4I1	109.5
H2F1—C2F—H2F3	109.5	N1I—C4I—H4I2	109.5
H2F2—C2F—H2F3	109.5	H4I1—C4I—H4I2	109.5
N1F—C3F—H3F1	109.5	N1I—C4I—H4I3	109.5
N1F—C3F—H3F2	109.5	H4I1—C4I—H4I3	109.5
H3F1—C3F—H3F2	109.5	H4I2—C4I—H4I3	109.5

Experimental details

Crystal data
Chemical formula	(C₄H₁₂N)₂[ZnCl₄]
M_r	355.46
Crystal system, space group	Orthorhombic, P2₁2₁2₁
Temperature (K)	100
a, b, c (Å)	8.9114 (18), 15.105 (3), 36.493 (7)
V (Å³)	4912.2 (17)
Z	12
Radiation type	Mo Kα
µ (mm⁻¹)	2.13
Crystal size (mm)	0.36 × 0.24 × 0.04

Data collection
Diffractometer	Bruker APEX CCD
Absorption correction	Multi-scan (SADABS; Sheldrick, 2007)
T_min, T_max	0.512, 0.918
No. of measured, independent and observed [I > 2σ(I)] reflections	32538, 9616, 9039
R_int	0.038
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.055, 1.00
No. of reflections	9616
No. of parameters	407
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.43, −0.29
Absolute structure	Flack (1983)
Absolute structure parameter	0.611 (6)

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXTL (Sheldrick, 2000).

Selected geometric parameters (Å, º) top

Zn1A—Cl4A	2.2645 (8)	N1E—C1E	1.494 (3)
Zn1A—Cl2A	2.2743 (8)	N1E—C3E	1.498 (3)
Zn1A—Cl1A	2.2807 (8)	N1F—C2F	1.491 (3)
Zn1A—Cl3A	2.2836 (8)	N1F—C3F	1.492 (3)
Zn1B—Cl1B	2.2677 (8)	N1F—C1F	1.493 (3)
Zn1B—Cl4B	2.2709 (7)	N1F—C4F	1.494 (3)
Zn1B—Cl3B	2.2797 (8)	N1G—C1G	1.488 (3)
Zn1B—Cl2B	2.2857 (8)	N1G—C2G	1.496 (3)
Zn1C—Cl1C	2.2620 (8)	N1G—C3G	1.497 (3)
Zn1C—Cl2C	2.2726 (8)	N1G—C4G	1.497 (3)
Zn1C—Cl3C	2.2770 (8)	N1H—C2H	1.487 (3)
Zn1C—Cl4C	2.2814 (8)	N1H—C3H	1.489 (3)
N1D—C4D	1.490 (3)	N1H—C4H	1.494 (3)
N1D—C3D	1.491 (3)	N1H—C1H	1.496 (3)
N1D—C1D	1.499 (3)	N1I—C1I	1.486 (3)
N1D—C2D	1.500 (3)	N1I—C3I	1.489 (3)
N1E—C2E	1.488 (3)	N1I—C2I	1.490 (3)
N1E—C4E	1.491 (3)	N1I—C4I	1.493 (3)

Cl4A—Zn1A—Cl2A	110.65 (3)	C2E—N1E—C3E	109.9 (2)
Cl4A—Zn1A—Cl1A	110.51 (3)	C4E—N1E—C3E	109.25 (19)
Cl2A—Zn1A—Cl1A	107.40 (3)	C1E—N1E—C3E	108.6 (2)
Cl4A—Zn1A—Cl3A	108.27 (3)	C2F—N1F—C3F	109.9 (2)
Cl2A—Zn1A—Cl3A	109.40 (3)	C2F—N1F—C1F	109.4 (2)
Cl1A—Zn1A—Cl3A	110.60 (3)	C3F—N1F—C1F	109.4 (2)
Cl1B—Zn1B—Cl4B	111.11 (3)	C2F—N1F—C4F	109.3 (2)
Cl1B—Zn1B—Cl3B	109.08 (3)	C3F—N1F—C4F	108.9 (2)
Cl4B—Zn1B—Cl3B	108.58 (3)	C1F—N1F—C4F	110.0 (2)
Cl1B—Zn1B—Cl2B	110.23 (3)	C1G—N1G—C2G	109.9 (2)
Cl4B—Zn1B—Cl2B	107.37 (3)	C1G—N1G—C3G	109.1 (2)
Cl3B—Zn1B—Cl2B	110.46 (3)	C2G—N1G—C3G	109.3 (2)
Cl1C—Zn1C—Cl2C	112.21 (3)	C1G—N1G—C4G	108.9 (2)
Cl1C—Zn1C—Cl3C	109.88 (3)	C2G—N1G—C4G	109.50 (19)
Cl2C—Zn1C—Cl3C	108.62 (3)	C3G—N1G—C4G	110.1 (2)
Cl1C—Zn1C—Cl4C	109.08 (3)	C2H—N1H—C3H	108.9 (2)
Cl2C—Zn1C—Cl4C	108.55 (3)	C2H—N1H—C4H	110.7 (2)
Cl3C—Zn1C—Cl4C	108.42 (3)	C3H—N1H—C4H	108.5 (2)
C4D—N1D—C3D	109.7 (2)	C2H—N1H—C1H	109.7 (2)
C4D—N1D—C1D	109.4 (2)	C3H—N1H—C1H	109.81 (19)
C3D—N1D—C1D	109.11 (19)	C1I—N1I—C3I	109.2 (2)
C4D—N1D—C2D	109.8 (2)	C1I—N1I—C2I	109.63 (19)
C3D—N1D—C2D	109.2 (2)	C3I—N1I—C2I	110.0 (2)
C1D—N1D—C2D	109.54 (19)	C1I—N1I—C4I	109.6 (2)
C2E—N1E—C4E	109.5 (2)	C3I—N1I—C4I	109.4 (2)
C2E—N1E—C1E	110.2 (2)	C2I—N1I—C4I	109.0 (2)
C4E—N1E—C1E	109.4 (2)

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Bis(tetra­methyl­ammonium) tetra­chlorido­zincate(II), phase VI

Supporting information

Key indicators

checkCIF/PLATON results

Bis(tetramethylammonium) tetrachloridozincate(II), phase VI