Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680702140X/lh2361sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680702140X/lh2361Isup2.hkl |
CCDC reference: 639562
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.013 Å
- Disorder in main residue
- R factor = 0.050
- wR factor = 0.161
- Data-to-parameter ratio = 23.6
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT026_ALERT_3_B Ratio Observed / Unique Reflections too Low .... 39 Perc. PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.64 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.58 Ratio PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C7
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.63 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.25 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C19 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C14 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Zn1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 8.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 13 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C7 - C8 ... 1.41 Ang.
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 106
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Some research related to zinc(II) compounds has already been published (Wang, Zhuang et al., 2007; Yu et al., 2007; Zhang et al., 2007; Liu et al., 2007; Tian et al., 2007; Wang, Moorefield et al., 2007).
A solution of ZnBr2 0.0207 g (0.1 mmol) in CH3CN (5 ml) was added to a solution of tacntp (0.1 mmol) (tacntp = 1,4,7-triazacyclononane-1,4,7-tripropionate) in CH3CN (15 ml). The reaction mixture was stirred at room temperature for 30 min. Then (C4H9)4N (0.1 mmol) was added to the solution. The reaction mixture was continuously stirred for 2 h at room temperature. Several months later, crystals suitable for X-ray diffraction were obtained by slow evaporation of the filtrate. Calculated for [(C4H9)4N]2[ZnBr4]: C 44.14, H 8.28, N 3.22, Br 32.65%; found: C 44.15, H 8.27, N3.24, Br 32.67%.
H atoms were placed in calculated positions with C—H = 0.96–0.97 Å and were included in the riding-motion approximation with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(C) for methyl H atoms. In one of the cation molecules three C atoms are disordered over two sites with refined occupancies of 0.500 (16). The C—C bonds distances of the disorder components were restained to 1.54 (1) Å.
In recent years, the crystal engineering of materials containing Zn(II) has become an intensively active field due to not only their structural diversity, but also their promising applications in the fields of catalysis, (Wang, Zhuang et al., 2007) medicine, magnetism, photochemistry, fluorescence (Yu et al., 2007; Zhang et al., 2007) and electrical chemistry (Liu et al., 2007; Tian et al., 2007; Wang, Moorefield et al., 2007). With this in mind, we have synthesized the title complex and its crystal structure is determined herein. The ZnII ion is coordinated by four Br atoms in a slightly distorted tetrhedral geometry. The asymmetric unit of (I) is shown in Fig. 1.
Some research related to zinc(II) compounds has already been published (Wang, Zhuang et al., 2007; Yu et al., 2007; Zhang et al., 2007; Liu et al., 2007; Tian et al., 2007; Wang, Moorefield et al., 2007).
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
Fig. 1. The asymmtric unit of (I) shown with 30% displacement ellipsoids. The disorder is not showm. |
[(C4H9)4N]2[ZnBr4] | F(000) = 1792 |
Mr = 869.93 | Dx = 1.347 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3229 reflections |
a = 16.530 (2) Å | θ = 1.4–26.4° |
b = 15.4906 (18) Å | µ = 4.32 mm−1 |
c = 18.657 (2) Å | T = 294 K |
β = 116.133 (2)° | Block, colourless |
V = 4289.0 (9) Å3 | 0.22 × 0.20 × 0.16 mm |
Z = 4 |
Bruker APEXII diffractometer | 8766 independent reflections |
Radiation source: fine-focus sealed tube | 3455 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.079 |
φ and ω scans | θmax = 26.4°, θmin = 1.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −20→20 |
Tmin = 0.399, Tmax = 0.500 | k = −14→19 |
24548 measured reflections | l = −19→23 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.161 | H-atom parameters constrained |
S = 0.96 | w = 1/[σ2(Fo2) + (0.0697P)2] where P = (Fo2 + 2Fc2)/3 |
8766 reflections | (Δ/σ)max = 0.001 |
371 parameters | Δρmax = 0.50 e Å−3 |
106 restraints | Δρmin = −0.65 e Å−3 |
[(C4H9)4N]2[ZnBr4] | V = 4289.0 (9) Å3 |
Mr = 869.93 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 16.530 (2) Å | µ = 4.32 mm−1 |
b = 15.4906 (18) Å | T = 294 K |
c = 18.657 (2) Å | 0.22 × 0.20 × 0.16 mm |
β = 116.133 (2)° |
Bruker APEXII diffractometer | 8766 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3455 reflections with I > 2σ(I) |
Tmin = 0.399, Tmax = 0.500 | Rint = 0.079 |
24548 measured reflections |
R[F2 > 2σ(F2)] = 0.050 | 106 restraints |
wR(F2) = 0.161 | H-atom parameters constrained |
S = 0.96 | Δρmax = 0.50 e Å−3 |
8766 reflections | Δρmin = −0.65 e Å−3 |
371 parameters |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Zn1 | 0.49076 (5) | 0.13616 (5) | 0.72626 (5) | 0.0547 (2) | |
Br1 | 0.57269 (6) | 0.25277 (5) | 0.70430 (5) | 0.0833 (3) | |
Br2 | 0.57414 (5) | 0.07205 (6) | 0.85543 (5) | 0.0858 (3) | |
Br3 | 0.35194 (6) | 0.19646 (5) | 0.71636 (6) | 0.0862 (3) | |
Br4 | 0.45436 (5) | 0.02280 (5) | 0.62795 (5) | 0.0744 (3) | |
N1 | 0.3318 (3) | 0.2229 (3) | 0.4325 (3) | 0.0540 (14) | |
N2 | 0.2736 (4) | 0.9413 (3) | 0.7667 (4) | 0.0663 (17) | |
C1 | 0.6498 (6) | 0.2236 (6) | 0.4602 (6) | 0.128 (4) | |
H1A | 0.7102 | 0.2102 | 0.4985 | 0.192* | |
H1B | 0.6460 | 0.2837 | 0.4463 | 0.192* | |
H1C | 0.6341 | 0.1891 | 0.4132 | 0.192* | |
C2 | 0.5864 (5) | 0.2049 (6) | 0.4955 (5) | 0.093 (3) | |
H2A | 0.5910 | 0.1442 | 0.5094 | 0.111* | |
H2B | 0.6049 | 0.2379 | 0.5444 | 0.111* | |
C3 | 0.4911 (5) | 0.2254 (5) | 0.4419 (5) | 0.080 (2) | |
H3A | 0.4704 | 0.1892 | 0.3946 | 0.096* | |
H3B | 0.4863 | 0.2851 | 0.4250 | 0.096* | |
C4 | 0.4325 (4) | 0.2106 (4) | 0.4837 (4) | 0.0573 (18) | |
H4A | 0.4518 | 0.2498 | 0.5288 | 0.069* | |
H4B | 0.4426 | 0.1523 | 0.5047 | 0.069* | |
C5 | 0.3112 (5) | 0.3131 (5) | 0.3960 (4) | 0.067 (2) | |
H5A | 0.3422 | 0.3201 | 0.3627 | 0.081* | |
H5B | 0.2471 | 0.3166 | 0.3614 | 0.081* | |
C6 | 0.3363 (5) | 0.3872 (5) | 0.4531 (5) | 0.094 (3) | |
H6A | 0.3981 | 0.3808 | 0.4933 | 0.113* | |
H6B | 0.2975 | 0.3885 | 0.4797 | 0.113* | |
C7 | 0.3262 (7) | 0.4708 (6) | 0.4068 (6) | 0.118 (3) | |
H7A | 0.3636 | 0.4671 | 0.3789 | 0.142* | |
H7B | 0.2641 | 0.4757 | 0.3669 | 0.142* | |
C8 | 0.3496 (10) | 0.5466 (8) | 0.4538 (8) | 0.210 (7) | |
H8A | 0.3421 | 0.5958 | 0.4202 | 0.316* | |
H8B | 0.4113 | 0.5430 | 0.4931 | 0.316* | |
H8C | 0.3113 | 0.5525 | 0.4800 | 0.316* | |
C9 | 0.0428 (6) | 0.2096 (6) | 0.4610 (6) | 0.126 (4) | |
H9A | 0.0193 | 0.2193 | 0.4991 | 0.189* | |
H9B | 0.0286 | 0.1518 | 0.4405 | 0.189* | |
H9C | 0.0163 | 0.2500 | 0.4179 | 0.189* | |
C10 | 0.1426 (5) | 0.2213 (5) | 0.5007 (5) | 0.085 (2) | |
H10A | 0.1565 | 0.2793 | 0.5221 | 0.103* | |
H10B | 0.1688 | 0.1812 | 0.5450 | 0.103* | |
C11 | 0.1841 (4) | 0.2070 (5) | 0.4452 (4) | 0.068 (2) | |
H11A | 0.1623 | 0.2509 | 0.4039 | 0.081* | |
H11B | 0.1648 | 0.1513 | 0.4195 | 0.081* | |
C12 | 0.2862 (4) | 0.2096 (4) | 0.4861 (4) | 0.0585 (19) | |
H12A | 0.3049 | 0.2556 | 0.5253 | 0.070* | |
H12B | 0.3078 | 0.1557 | 0.5148 | 0.070* | |
C13 | 0.2967 (5) | 0.1583 (5) | 0.3646 (4) | 0.071 (2) | |
H13A | 0.2328 | 0.1691 | 0.3332 | 0.085* | |
H13B | 0.3258 | 0.1703 | 0.3305 | 0.085* | |
C14 | 0.3083 (5) | 0.0645 (5) | 0.3845 (4) | 0.076 (2) | |
H14A | 0.3719 | 0.0504 | 0.4115 | 0.092* | |
H14B | 0.2813 | 0.0505 | 0.4199 | 0.092* | |
C15 | 0.2641 (7) | 0.0134 (6) | 0.3095 (5) | 0.120 (4) | |
H15A | 0.2028 | 0.0340 | 0.2794 | 0.144* | |
H15B | 0.2960 | 0.0232 | 0.2773 | 0.144* | |
C16 | 0.2618 (7) | −0.0797 (7) | 0.3230 (6) | 0.148 (5) | |
H16A | 0.2315 | −0.1087 | 0.2726 | 0.223* | |
H16B | 0.2301 | −0.0901 | 0.3546 | 0.223* | |
H16C | 0.3222 | −0.1012 | 0.3505 | 0.223* | |
C17 | 0.5576 (8) | 0.7840 (8) | 0.8043 (7) | 0.176 (6) | |
H17A | 0.5868 | 0.7288 | 0.8185 | 0.263* | |
H17B | 0.5938 | 0.8265 | 0.8424 | 0.263* | |
H17C | 0.5504 | 0.8000 | 0.7521 | 0.263* | |
C18 | 0.4636 (8) | 0.7787 (7) | 0.8040 (7) | 0.141 (4) | |
H18A | 0.4276 | 0.7353 | 0.7658 | 0.170* | |
H18B | 0.4712 | 0.7606 | 0.8564 | 0.170* | |
C19 | 0.4140 (6) | 0.8633 (5) | 0.7832 (5) | 0.089 (3) | |
H19A | 0.4505 | 0.9072 | 0.8206 | 0.107* | |
H19B | 0.4046 | 0.8807 | 0.7302 | 0.107* | |
C20 | 0.3271 (5) | 0.8575 (4) | 0.7856 (5) | 0.078 (2) | |
H20A | 0.3372 | 0.8384 | 0.8384 | 0.094* | |
H20B | 0.2911 | 0.8139 | 0.7477 | 0.094* | |
C21 | 0.2545 (5) | 0.9748 (4) | 0.6845 (5) | 0.071 (2) | |
H21A | 0.2243 | 1.0301 | 0.6770 | 0.085* | |
H21B | 0.3116 | 0.9850 | 0.6830 | 0.085* | |
C22 | 0.1991 (5) | 0.9184 (5) | 0.6164 (5) | 0.086 (2) | |
H22A | 0.1431 | 0.9040 | 0.6186 | 0.104* | |
H22B | 0.2312 | 0.8652 | 0.6190 | 0.104* | |
C23 | 0.1789 (7) | 0.9655 (6) | 0.5384 (6) | 0.115 (3) | |
H23A | 0.1562 | 1.0224 | 0.5416 | 0.138* | |
H23B | 0.2356 | 0.9737 | 0.5355 | 0.138* | |
C24 | 0.1164 (8) | 0.9265 (8) | 0.4647 (7) | 0.166 (5) | |
H24A | 0.1099 | 0.9628 | 0.4207 | 0.249* | |
H24B | 0.0589 | 0.9198 | 0.4652 | 0.249* | |
H24C | 0.1387 | 0.8710 | 0.4590 | 0.249* | |
C25 | 0.3386 (7) | 1.1502 (6) | 0.9471 (6) | 0.127 (4) | |
H25A | 0.3734 | 1.1972 | 0.9797 | 0.191* | |
H25B | 0.2897 | 1.1374 | 0.9599 | 0.191* | |
H25C | 0.3151 | 1.1660 | 0.8918 | 0.191* | |
C26 | 0.3968 (6) | 1.0731 (6) | 0.9623 (5) | 0.096 (3) | |
H26A | 0.4200 | 1.0575 | 1.0182 | 0.115* | |
H26B | 0.4478 | 1.0876 | 0.9520 | 0.115* | |
C27 | 0.3496 (6) | 0.9970 (5) | 0.9126 (5) | 0.088 (3) | |
H27A | 0.2946 | 0.9863 | 0.9177 | 0.106* | |
H27B | 0.3877 | 0.9464 | 0.9321 | 0.106* | |
C28 | 0.3269 (5) | 1.0111 (4) | 0.8248 (5) | 0.067 (2) | |
H28A | 0.2933 | 1.0646 | 0.8078 | 0.081* | |
H28B | 0.3829 | 1.0189 | 0.8208 | 0.081* | |
C29 | 0.1874 (5) | 0.9230 (5) | 0.7726 (5) | 0.083 (3) | |
H29A | 0.1562 | 0.8769 | 0.7356 | 0.099* | |
H29B | 0.2027 | 0.9019 | 0.8260 | 0.099* | |
C30 | 0.1237 (6) | 0.9969 (6) | 0.7561 (7) | 0.114 (3) | 0.500 (16) |
H30A | 0.1183 | 1.0251 | 0.7077 | 0.137* | 0.500 (16) |
H30B | 0.1511 | 1.0382 | 0.7992 | 0.137* | 0.500 (16) |
C31 | 0.0270 (9) | 0.9777 (17) | 0.7460 (11) | 0.127 (8) | 0.500 (16) |
H31A | −0.0148 | 1.0234 | 0.7172 | 0.152* | 0.500 (16) |
H31B | 0.0044 | 0.9231 | 0.7191 | 0.152* | 0.500 (16) |
C32 | 0.0444 (17) | 0.9742 (15) | 0.8335 (11) | 0.136 (9) | 0.500 (16) |
H32A | −0.0102 | 0.9585 | 0.8366 | 0.205* | 0.500 (16) |
H32B | 0.0641 | 1.0298 | 0.8575 | 0.205* | 0.500 (16) |
H32C | 0.0902 | 0.9321 | 0.8613 | 0.205* | 0.500 (16) |
C30' | 0.1237 (6) | 0.9969 (6) | 0.7561 (7) | 0.114 (3) | 0.500 (16) |
H30C | 0.0942 | 1.0101 | 0.6994 | 0.137* | 0.500 (16) |
H30D | 0.1550 | 1.0481 | 0.7850 | 0.137* | 0.500 (16) |
C32' | −0.0040 (13) | 1.0404 (12) | 0.7878 (14) | 0.128 (9) | 0.500 (16) |
H32D | −0.0465 | 1.0203 | 0.8063 | 0.192* | 0.500 (16) |
H32E | −0.0358 | 1.0641 | 0.7352 | 0.192* | 0.500 (16) |
H32F | 0.0336 | 1.0841 | 0.8234 | 0.192* | 0.500 (16) |
C31' | 0.0545 (15) | 0.9649 (13) | 0.7856 (18) | 0.118 (7) | 0.500 (16) |
H31C | 0.0167 | 0.9204 | 0.7501 | 0.141* | 0.500 (16) |
H31D | 0.0861 | 0.9402 | 0.8386 | 0.141* | 0.500 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.0535 (5) | 0.0543 (5) | 0.0499 (5) | −0.0035 (4) | 0.0170 (4) | −0.0008 (4) |
Br1 | 0.0844 (6) | 0.0921 (6) | 0.0646 (6) | −0.0296 (5) | 0.0249 (4) | −0.0038 (4) |
Br2 | 0.0744 (6) | 0.0979 (7) | 0.0682 (6) | −0.0048 (5) | 0.0159 (4) | 0.0198 (5) |
Br3 | 0.0811 (6) | 0.0670 (5) | 0.1121 (8) | 0.0109 (4) | 0.0442 (5) | 0.0056 (5) |
Br4 | 0.0878 (6) | 0.0639 (5) | 0.0726 (6) | −0.0061 (4) | 0.0362 (5) | −0.0105 (4) |
N1 | 0.047 (3) | 0.073 (4) | 0.038 (3) | 0.001 (3) | 0.015 (3) | 0.007 (3) |
N2 | 0.067 (4) | 0.045 (4) | 0.090 (5) | −0.010 (3) | 0.037 (4) | 0.005 (3) |
C1 | 0.084 (7) | 0.153 (10) | 0.156 (10) | −0.011 (6) | 0.061 (7) | −0.017 (8) |
C2 | 0.062 (5) | 0.119 (7) | 0.100 (7) | 0.003 (5) | 0.038 (5) | 0.004 (5) |
C3 | 0.058 (5) | 0.106 (6) | 0.077 (6) | −0.003 (4) | 0.028 (5) | 0.003 (5) |
C4 | 0.043 (4) | 0.067 (5) | 0.049 (4) | −0.003 (3) | 0.008 (3) | 0.007 (3) |
C5 | 0.058 (5) | 0.078 (6) | 0.048 (5) | 0.000 (4) | 0.008 (4) | 0.014 (4) |
C6 | 0.083 (6) | 0.076 (6) | 0.102 (7) | −0.008 (5) | 0.022 (5) | 0.004 (6) |
C7 | 0.133 (9) | 0.069 (7) | 0.139 (10) | −0.003 (6) | 0.047 (7) | 0.019 (7) |
C8 | 0.32 (2) | 0.099 (10) | 0.189 (15) | −0.028 (11) | 0.089 (14) | −0.005 (9) |
C9 | 0.075 (6) | 0.169 (10) | 0.161 (11) | 0.020 (6) | 0.077 (7) | 0.033 (8) |
C10 | 0.083 (6) | 0.089 (6) | 0.094 (7) | 0.009 (5) | 0.048 (5) | 0.008 (5) |
C11 | 0.057 (5) | 0.087 (6) | 0.063 (5) | 0.010 (4) | 0.029 (4) | 0.006 (4) |
C12 | 0.054 (4) | 0.066 (5) | 0.051 (5) | 0.000 (4) | 0.019 (4) | 0.003 (4) |
C13 | 0.057 (5) | 0.108 (7) | 0.041 (4) | −0.006 (4) | 0.015 (4) | −0.007 (4) |
C14 | 0.082 (6) | 0.077 (6) | 0.061 (5) | 0.006 (4) | 0.024 (4) | −0.003 (4) |
C15 | 0.149 (9) | 0.104 (8) | 0.073 (7) | 0.001 (7) | 0.018 (6) | −0.018 (6) |
C16 | 0.183 (11) | 0.107 (9) | 0.114 (9) | 0.023 (8) | 0.027 (8) | −0.026 (7) |
C17 | 0.177 (13) | 0.215 (14) | 0.141 (11) | 0.101 (11) | 0.075 (10) | 0.013 (9) |
C18 | 0.162 (11) | 0.134 (9) | 0.145 (11) | 0.064 (8) | 0.082 (9) | 0.038 (7) |
C19 | 0.093 (7) | 0.074 (6) | 0.100 (7) | 0.017 (5) | 0.043 (5) | 0.006 (5) |
C20 | 0.088 (6) | 0.053 (5) | 0.104 (7) | 0.008 (4) | 0.052 (5) | 0.015 (4) |
C21 | 0.066 (5) | 0.059 (5) | 0.081 (6) | −0.014 (4) | 0.027 (4) | 0.000 (4) |
C22 | 0.072 (6) | 0.090 (6) | 0.101 (7) | −0.016 (5) | 0.041 (5) | −0.008 (6) |
C23 | 0.113 (8) | 0.131 (9) | 0.078 (7) | −0.041 (6) | 0.021 (6) | −0.011 (6) |
C24 | 0.158 (11) | 0.196 (13) | 0.118 (10) | −0.036 (10) | 0.038 (9) | −0.005 (9) |
C25 | 0.132 (9) | 0.119 (9) | 0.140 (10) | 0.000 (7) | 0.069 (8) | −0.035 (7) |
C26 | 0.099 (7) | 0.111 (8) | 0.080 (7) | 0.005 (6) | 0.042 (5) | 0.001 (6) |
C27 | 0.106 (7) | 0.079 (6) | 0.093 (7) | 0.002 (5) | 0.056 (6) | 0.003 (5) |
C28 | 0.082 (5) | 0.052 (5) | 0.076 (6) | −0.001 (4) | 0.042 (5) | 0.008 (4) |
C29 | 0.078 (6) | 0.065 (5) | 0.131 (8) | −0.013 (4) | 0.070 (6) | 0.002 (5) |
C30 | 0.091 (5) | 0.122 (5) | 0.147 (6) | −0.005 (4) | 0.068 (4) | −0.003 (5) |
C31 | 0.123 (10) | 0.134 (10) | 0.125 (11) | 0.006 (8) | 0.055 (8) | 0.008 (8) |
C32 | 0.134 (12) | 0.143 (12) | 0.136 (12) | −0.002 (8) | 0.063 (9) | 0.000 (8) |
C30' | 0.091 (5) | 0.122 (5) | 0.147 (6) | −0.005 (4) | 0.068 (4) | −0.003 (5) |
C32' | 0.119 (11) | 0.150 (12) | 0.131 (12) | 0.001 (8) | 0.070 (8) | 0.007 (8) |
C31' | 0.109 (9) | 0.134 (10) | 0.126 (10) | 0.004 (8) | 0.067 (8) | 0.001 (8) |
Zn1—Br1 | 2.3986 (11) | C16—H16A | 0.9600 |
Zn1—Br2 | 2.4014 (11) | C16—H16B | 0.9600 |
Zn1—Br3 | 2.4082 (11) | C16—H16C | 0.9600 |
Zn1—Br4 | 2.4162 (11) | C17—C18 | 1.555 (13) |
N1—C12 | 1.507 (8) | C17—H17A | 0.9600 |
N1—C13 | 1.516 (8) | C17—H17B | 0.9600 |
N1—C4 | 1.524 (7) | C17—H17C | 0.9600 |
N1—C5 | 1.526 (8) | C18—C19 | 1.503 (11) |
N2—C29 | 1.502 (8) | C18—H18A | 0.9700 |
N2—C28 | 1.509 (8) | C18—H18B | 0.9700 |
N2—C21 | 1.515 (9) | C19—C20 | 1.459 (10) |
N2—C20 | 1.522 (8) | C19—H19A | 0.9700 |
C1—C2 | 1.490 (11) | C19—H19B | 0.9700 |
C1—H1A | 0.9600 | C20—H20A | 0.9700 |
C1—H1B | 0.9600 | C20—H20B | 0.9700 |
C1—H1C | 0.9600 | C21—C22 | 1.481 (9) |
C2—C3 | 1.483 (9) | C21—H21A | 0.9700 |
C2—H2A | 0.9700 | C21—H21B | 0.9700 |
C2—H2B | 0.9700 | C22—C23 | 1.526 (11) |
C3—C4 | 1.503 (9) | C22—H22A | 0.9700 |
C3—H3A | 0.9700 | C22—H22B | 0.9700 |
C3—H3B | 0.9700 | C23—C24 | 1.440 (12) |
C4—H4A | 0.9700 | C23—H23A | 0.9700 |
C4—H4B | 0.9700 | C23—H23B | 0.9700 |
C5—C6 | 1.495 (10) | C24—H24A | 0.9600 |
C5—H5A | 0.9700 | C24—H24B | 0.9600 |
C5—H5B | 0.9700 | C24—H24C | 0.9600 |
C6—C7 | 1.523 (11) | C25—C26 | 1.480 (11) |
C6—H6A | 0.9700 | C25—H25A | 0.9600 |
C6—H6B | 0.9700 | C25—H25B | 0.9600 |
C7—C8 | 1.414 (13) | C25—H25C | 0.9600 |
C7—H7A | 0.9700 | C26—C27 | 1.489 (10) |
C7—H7B | 0.9700 | C26—H26A | 0.9700 |
C8—H8A | 0.9600 | C26—H26B | 0.9700 |
C8—H8B | 0.9600 | C27—C28 | 1.527 (10) |
C8—H8C | 0.9600 | C27—H27A | 0.9700 |
C9—C10 | 1.492 (10) | C27—H27B | 0.9700 |
C9—H9A | 0.9600 | C28—H28A | 0.9700 |
C9—H9B | 0.9600 | C28—H28B | 0.9700 |
C9—H9C | 0.9600 | C29—C30 | 1.493 (10) |
C10—C11 | 1.489 (9) | C29—H29A | 0.9700 |
C10—H10A | 0.9700 | C29—H29B | 0.9700 |
C10—H10B | 0.9700 | C30—C31 | 1.555 (9) |
C11—C12 | 1.515 (8) | C30—H30A | 0.9700 |
C11—H11A | 0.9700 | C30—H30B | 0.9700 |
C11—H11B | 0.9700 | C31—C32 | 1.528 (10) |
C12—H12A | 0.9700 | C31—H31A | 0.9700 |
C12—H12B | 0.9700 | C31—H31B | 0.9700 |
C13—C14 | 1.492 (9) | C32—H32A | 0.9600 |
C13—H13A | 0.9700 | C32—H32B | 0.9600 |
C13—H13B | 0.9700 | C32—H32C | 0.9600 |
C14—C15 | 1.490 (10) | C32'—C31' | 1.529 (10) |
C14—H14A | 0.9700 | C32'—H32D | 0.9600 |
C14—H14B | 0.9700 | C32'—H32E | 0.9600 |
C15—C16 | 1.467 (11) | C32'—H32F | 0.9600 |
C15—H15A | 0.9700 | C31'—H31C | 0.9700 |
C15—H15B | 0.9700 | C31'—H31D | 0.9700 |
Br1—Zn1—Br2 | 111.42 (4) | H16A—C16—H16B | 109.5 |
Br1—Zn1—Br3 | 106.59 (4) | C15—C16—H16C | 109.5 |
Br2—Zn1—Br3 | 110.10 (4) | H16A—C16—H16C | 109.5 |
Br1—Zn1—Br4 | 112.84 (4) | H16B—C16—H16C | 109.5 |
Br2—Zn1—Br4 | 107.59 (4) | C18—C17—H17A | 109.5 |
Br3—Zn1—Br4 | 108.26 (4) | C18—C17—H17B | 109.5 |
C12—N1—C13 | 110.2 (5) | H17A—C17—H17B | 109.5 |
C12—N1—C4 | 107.2 (5) | C18—C17—H17C | 109.5 |
C13—N1—C4 | 110.6 (5) | H17A—C17—H17C | 109.5 |
C12—N1—C5 | 110.1 (5) | H17B—C17—H17C | 109.5 |
C13—N1—C5 | 107.7 (5) | C19—C18—C17 | 112.7 (9) |
C4—N1—C5 | 111.2 (5) | C19—C18—H18A | 109.1 |
C29—N2—C28 | 110.8 (6) | C17—C18—H18A | 109.1 |
C29—N2—C21 | 110.9 (6) | C19—C18—H18B | 109.1 |
C28—N2—C21 | 106.1 (5) | C17—C18—H18B | 109.1 |
C29—N2—C20 | 107.2 (5) | H18A—C18—H18B | 107.8 |
C28—N2—C20 | 110.4 (6) | C20—C19—C18 | 111.7 (8) |
C21—N2—C20 | 111.5 (6) | C20—C19—H19A | 109.3 |
C2—C1—H1A | 109.5 | C18—C19—H19A | 109.3 |
C2—C1—H1B | 109.5 | C20—C19—H19B | 109.3 |
H1A—C1—H1B | 109.5 | C18—C19—H19B | 109.3 |
C2—C1—H1C | 109.5 | H19A—C19—H19B | 107.9 |
H1A—C1—H1C | 109.5 | C19—C20—N2 | 114.9 (6) |
H1B—C1—H1C | 109.5 | C19—C20—H20A | 108.6 |
C3—C2—C1 | 114.0 (8) | N2—C20—H20A | 108.6 |
C3—C2—H2A | 108.8 | C19—C20—H20B | 108.6 |
C1—C2—H2A | 108.8 | N2—C20—H20B | 108.6 |
C3—C2—H2B | 108.8 | H20A—C20—H20B | 107.5 |
C1—C2—H2B | 108.8 | C22—C21—N2 | 116.2 (6) |
H2A—C2—H2B | 107.7 | C22—C21—H21A | 108.2 |
C2—C3—C4 | 110.7 (7) | N2—C21—H21A | 108.2 |
C2—C3—H3A | 109.5 | C22—C21—H21B | 108.2 |
C4—C3—H3A | 109.5 | N2—C21—H21B | 108.2 |
C2—C3—H3B | 109.5 | H21A—C21—H21B | 107.4 |
C4—C3—H3B | 109.5 | C21—C22—C23 | 109.2 (7) |
H3A—C3—H3B | 108.1 | C21—C22—H22A | 109.8 |
C3—C4—N1 | 115.6 (5) | C23—C22—H22A | 109.8 |
C3—C4—H4A | 108.4 | C21—C22—H22B | 109.8 |
N1—C4—H4A | 108.4 | C23—C22—H22B | 109.8 |
C3—C4—H4B | 108.4 | H22A—C22—H22B | 108.3 |
N1—C4—H4B | 108.4 | C24—C23—C22 | 118.2 (9) |
H4A—C4—H4B | 107.4 | C24—C23—H23A | 107.8 |
C6—C5—N1 | 116.6 (6) | C22—C23—H23A | 107.8 |
C6—C5—H5A | 108.1 | C24—C23—H23B | 107.8 |
N1—C5—H5A | 108.1 | C22—C23—H23B | 107.8 |
C6—C5—H5B | 108.1 | H23A—C23—H23B | 107.1 |
N1—C5—H5B | 108.1 | C23—C24—H24A | 109.5 |
H5A—C5—H5B | 107.3 | C23—C24—H24B | 109.5 |
C5—C6—C7 | 108.8 (8) | H24A—C24—H24B | 109.5 |
C5—C6—H6A | 109.9 | C23—C24—H24C | 109.5 |
C7—C6—H6A | 109.9 | H24A—C24—H24C | 109.5 |
C5—C6—H6B | 109.9 | H24B—C24—H24C | 109.5 |
C7—C6—H6B | 109.9 | C26—C25—H25A | 109.5 |
H6A—C6—H6B | 108.3 | C26—C25—H25B | 109.5 |
C8—C7—C6 | 115.0 (10) | H25A—C25—H25B | 109.5 |
C8—C7—H7A | 108.5 | C26—C25—H25C | 109.5 |
C6—C7—H7A | 108.5 | H25A—C25—H25C | 109.5 |
C8—C7—H7B | 108.5 | H25B—C25—H25C | 109.5 |
C6—C7—H7B | 108.5 | C25—C26—C27 | 113.7 (8) |
H7A—C7—H7B | 107.5 | C25—C26—H26A | 108.8 |
C7—C8—H8A | 109.5 | C27—C26—H26A | 108.8 |
C7—C8—H8B | 109.5 | C25—C26—H26B | 108.8 |
H8A—C8—H8B | 109.5 | C27—C26—H26B | 108.8 |
C7—C8—H8C | 109.5 | H26A—C26—H26B | 107.7 |
H8A—C8—H8C | 109.5 | C26—C27—C28 | 111.6 (7) |
H8B—C8—H8C | 109.5 | C26—C27—H27A | 109.3 |
C10—C9—H9A | 109.5 | C28—C27—H27A | 109.3 |
C10—C9—H9B | 109.5 | C26—C27—H27B | 109.3 |
H9A—C9—H9B | 109.5 | C28—C27—H27B | 109.3 |
C10—C9—H9C | 109.5 | H27A—C27—H27B | 108.0 |
H9A—C9—H9C | 109.5 | N2—C28—C27 | 117.3 (6) |
H9B—C9—H9C | 109.5 | N2—C28—H28A | 108.0 |
C11—C10—C9 | 112.6 (7) | C27—C28—H28A | 108.0 |
C11—C10—H10A | 109.1 | N2—C28—H28B | 108.0 |
C9—C10—H10A | 109.1 | C27—C28—H28B | 108.0 |
C11—C10—H10B | 109.1 | H28A—C28—H28B | 107.2 |
C9—C10—H10B | 109.1 | C30—C29—N2 | 116.4 (6) |
H10A—C10—H10B | 107.8 | C30—C29—H29A | 108.2 |
C10—C11—C12 | 113.5 (6) | N2—C29—H29A | 108.2 |
C10—C11—H11A | 108.9 | C30—C29—H29B | 108.2 |
C12—C11—H11A | 108.9 | N2—C29—H29B | 108.2 |
C10—C11—H11B | 108.9 | H29A—C29—H29B | 107.3 |
C12—C11—H11B | 108.9 | C29—C30—C31 | 118.2 (12) |
H11A—C11—H11B | 107.7 | C29—C30—H30A | 107.8 |
N1—C12—C11 | 116.2 (5) | C31—C30—H30A | 107.8 |
N1—C12—H12A | 108.2 | C29—C30—H30B | 107.8 |
C11—C12—H12A | 108.2 | C31—C30—H30B | 107.8 |
N1—C12—H12B | 108.2 | H30A—C30—H30B | 107.1 |
C11—C12—H12B | 108.2 | C32—C31—C30 | 100.3 (14) |
H12A—C12—H12B | 107.4 | C32—C31—H31A | 111.7 |
C14—C13—N1 | 118.4 (6) | C30—C31—H31A | 111.7 |
C14—C13—H13A | 107.7 | C32—C31—H31B | 111.7 |
N1—C13—H13A | 107.7 | C30—C31—H31B | 111.7 |
C14—C13—H13B | 107.7 | H31A—C31—H31B | 109.5 |
N1—C13—H13B | 107.7 | C31—C32—H32A | 109.5 |
H13A—C13—H13B | 107.1 | C31—C32—H32B | 109.5 |
C15—C14—C13 | 109.1 (7) | H32A—C32—H32B | 109.5 |
C15—C14—H14A | 109.9 | C31—C32—H32C | 109.5 |
C13—C14—H14A | 109.9 | H32A—C32—H32C | 109.5 |
C15—C14—H14B | 109.9 | H32B—C32—H32C | 109.5 |
C13—C14—H14B | 109.9 | C31'—C32'—H32D | 109.5 |
H14A—C14—H14B | 108.3 | C31'—C32'—H32E | 109.5 |
C16—C15—C14 | 113.6 (8) | H32D—C32'—H32E | 109.5 |
C16—C15—H15A | 108.9 | C31'—C32'—H32F | 109.5 |
C14—C15—H15A | 108.9 | H32D—C32'—H32F | 109.5 |
C16—C15—H15B | 108.9 | H32E—C32'—H32F | 109.5 |
C14—C15—H15B | 108.9 | C32'—C31'—H31C | 109.7 |
H15A—C15—H15B | 107.7 | C32'—C31'—H31D | 109.7 |
C15—C16—H16A | 109.5 | H31C—C31'—H31D | 108.2 |
C15—C16—H16B | 109.5 | ||
C1—C2—C3—C4 | −176.0 (7) | C17—C18—C19—C20 | −178.4 (8) |
C2—C3—C4—N1 | −175.5 (6) | C18—C19—C20—N2 | 178.9 (7) |
C12—N1—C4—C3 | −177.3 (6) | C29—N2—C20—C19 | −179.6 (7) |
C13—N1—C4—C3 | 62.6 (7) | C28—N2—C20—C19 | −58.8 (9) |
C5—N1—C4—C3 | −56.9 (8) | C21—N2—C20—C19 | 58.9 (9) |
C12—N1—C5—C6 | 57.0 (7) | C29—N2—C21—C22 | −57.2 (8) |
C13—N1—C5—C6 | 177.1 (6) | C28—N2—C21—C22 | −177.6 (6) |
C4—N1—C5—C6 | −61.6 (8) | C20—N2—C21—C22 | 62.2 (8) |
N1—C5—C6—C7 | 170.2 (7) | N2—C21—C22—C23 | 174.6 (7) |
C5—C6—C7—C8 | −178.8 (10) | C21—C22—C23—C24 | −172.3 (9) |
C9—C10—C11—C12 | −174.1 (7) | C25—C26—C27—C28 | 69.3 (10) |
C13—N1—C12—C11 | −51.8 (7) | C29—N2—C28—C27 | 55.2 (8) |
C4—N1—C12—C11 | −172.1 (6) | C21—N2—C28—C27 | 175.6 (7) |
C5—N1—C12—C11 | 66.8 (7) | C20—N2—C28—C27 | −63.4 (8) |
C10—C11—C12—N1 | −162.0 (6) | C26—C27—C28—N2 | −176.2 (6) |
C12—N1—C13—C14 | −59.8 (8) | C28—N2—C29—C30 | 59.6 (9) |
C4—N1—C13—C14 | 58.6 (8) | C21—N2—C29—C30 | −57.9 (9) |
C5—N1—C13—C14 | −179.8 (6) | C20—N2—C29—C30 | −179.9 (8) |
N1—C13—C14—C15 | 176.5 (7) | N2—C29—C30—C31 | 169.0 (10) |
C13—C14—C15—C16 | −172.9 (8) | C29—C30—C31—C32 | 82 (2) |
Experimental details
Crystal data | |
Chemical formula | [(C4H9)4N]2[ZnBr4] |
Mr | 869.93 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 294 |
a, b, c (Å) | 16.530 (2), 15.4906 (18), 18.657 (2) |
β (°) | 116.133 (2) |
V (Å3) | 4289.0 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 4.32 |
Crystal size (mm) | 0.22 × 0.20 × 0.16 |
Data collection | |
Diffractometer | Bruker APEXII |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.399, 0.500 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 24548, 8766, 3455 |
Rint | 0.079 |
(sin θ/λ)max (Å−1) | 0.626 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.050, 0.161, 0.96 |
No. of reflections | 8766 |
No. of parameters | 371 |
No. of restraints | 106 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.50, −0.65 |
Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998), SHELXTL.
Zn1—Br1 | 2.3986 (11) | Zn1—Br3 | 2.4082 (11) |
Zn1—Br2 | 2.4014 (11) | Zn1—Br4 | 2.4162 (11) |
Br1—Zn1—Br2 | 111.42 (4) | Br1—Zn1—Br4 | 112.84 (4) |
Br1—Zn1—Br3 | 106.59 (4) | Br2—Zn1—Br4 | 107.59 (4) |
Br2—Zn1—Br3 | 110.10 (4) | Br3—Zn1—Br4 | 108.26 (4) |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
In recent years, the crystal engineering of materials containing Zn(II) has become an intensively active field due to not only their structural diversity, but also their promising applications in the fields of catalysis, (Wang, Zhuang et al., 2007) medicine, magnetism, photochemistry, fluorescence (Yu et al., 2007; Zhang et al., 2007) and electrical chemistry (Liu et al., 2007; Tian et al., 2007; Wang, Moorefield et al., 2007). With this in mind, we have synthesized the title complex and its crystal structure is determined herein. The ZnII ion is coordinated by four Br atoms in a slightly distorted tetrhedral geometry. The asymmetric unit of (I) is shown in Fig. 1.