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The title compound, [ZnCl2(C16H20N4)]n, was prepared from the reaction of N,N′-bis(4-pyridylmethyl)piperazine (bpmp) and ZnCl2. The asymmetric unit contains one Cl atom, half a ZnII ion and half a bmpb moiety. The ZnII ion, which lies on a twofold axis, has a distorted tetrahedral coordination geometry, with the central piperazine group in bpmp bridging ZnCl2 units to form a one-dimensional polymeric chain. The piperazine connector in bpmp adopts a stable chair conformation.
Supporting information
CCDC reference: 251598
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.006 Å
- R factor = 0.043
- wR factor = 0.116
- Data-to-parameter ratio = 10.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97
PLAT048_ALERT_1_C MoietyFormula Not Given ........................ ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.85
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 10
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.02
PLAT350_ALERT_3_C Short C-H Bond (0.96A) C4 - H4A ... 0.81 Ang.
PLAT350_ALERT_3_C Short C-H Bond (0.96A) C6 - H6B ... 0.81 Ang.
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.845
Tmax scaled 0.845 Tmin scaled 0.612
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 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
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
checkCIF publication errors
Alert level A
PUBL003_ALERT_1_A The contact author's name is missing,
_publ_contact_author_name.
1 ALERT level A = Data missing that is essential or data in wrong format
0 ALERT level G = General alerts. Data that may be required is missing
Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SAINT (Siemens, 1994); program(s) used to solve structure: SHELXTL-PC (Sheldrick, 1997); program(s) used to refine structure: SHELXTL-PC; molecular graphics: reference?; software used to prepare material for publication: reference?.
catena-Poly[[dichlorozinc(II)]-µ-
N,
N'-bis(4-pyridylmethyl)piperazine]
top
Crystal data top
[ZnCl2(C16H20N4)] | F(000) = 832 |
Mr = 404.63 | Dx = 1.508 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 22.167 (2) Å | Cell parameters from 62 reflections |
b = 5.8534 (4) Å | θ = 3.0–25.1° |
c = 14.2600 (12) Å | µ = 1.68 mm−1 |
β = 105.629 (3)° | T = 173 K |
V = 1781.9 (3) Å3 | Needle, colorless |
Z = 4 | 0.38 × 0.16 × 0.10 mm |
Data collection top
Siemens SMART CCD diffractometer | 1525 independent reflections |
Radiation source: fine-focus sealed tube | 1306 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
ω scan | θmax = 25.1°, θmin = 3.0° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −26→8 |
Tmin = 0.724, Tmax = 1.000 | k = −6→6 |
2306 measured reflections | l = −16→16 |
Refinement top
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.116 | All H-atom parameters refined |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0624P)2 + 3.1799P] where P = (Fo2 + 2Fc2)/3 |
1525 reflections | (Δ/σ)max < 0.001 |
145 parameters | Δρmax = 0.33 e Å−3 |
0 restraints | Δρmin = −0.67 e Å−3 |
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. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Zn | 0.0000 | 0.90223 (10) | 0.2500 | 0.0351 (2) | |
Cl | 0.04961 (6) | 1.0826 (2) | 0.38525 (8) | 0.0604 (4) | |
N1 | 0.05951 (13) | 0.6809 (5) | 0.2063 (2) | 0.0350 (7) | |
C1 | 0.0975 (2) | 0.5442 (8) | 0.2701 (3) | 0.0515 (11) | |
H1 | 0.094 (2) | 0.560 (7) | 0.335 (3) | 0.052 (12)* | |
N2 | 0.19766 (14) | 0.2351 (5) | 0.0404 (2) | 0.0394 (7) | |
C2 | 0.1337 (2) | 0.3784 (7) | 0.2433 (3) | 0.0511 (10) | |
H2 | 0.162 (2) | 0.281 (8) | 0.290 (3) | 0.061 (13)* | |
C3 | 0.13162 (17) | 0.3495 (6) | 0.1468 (3) | 0.0398 (9) | |
C4 | 0.1676 (2) | 0.1623 (8) | 0.1144 (4) | 0.0521 (11) | |
H4B | 0.200 (2) | 0.099 (7) | 0.173 (3) | 0.051 (12)* | |
H4A | 0.144 (2) | 0.056 (7) | 0.098 (3) | 0.044 (13)* | |
C5 | 0.24960 (18) | 0.3898 (7) | 0.0801 (3) | 0.0407 (9) | |
H5B | 0.2816 (16) | 0.317 (6) | 0.130 (2) | 0.022 (8)* | |
H5A | 0.238 (2) | 0.521 (8) | 0.110 (3) | 0.055 (12)* | |
C6 | 0.2789 (2) | 0.4629 (7) | 0.0016 (4) | 0.0462 (10) | |
H6B | 0.308 (2) | 0.550 (8) | 0.018 (3) | 0.052 (13)* | |
H6A | 0.2444 (19) | 0.558 (7) | −0.047 (3) | 0.043 (11)* | |
C7 | 0.0932 (2) | 0.4945 (8) | 0.0812 (3) | 0.0506 (10) | |
H7 | 0.0929 (18) | 0.483 (7) | 0.013 (3) | 0.047 (11)* | |
C8 | 0.05781 (18) | 0.6549 (7) | 0.1130 (3) | 0.0442 (9) | |
H8 | 0.0322 (18) | 0.749 (8) | 0.065 (3) | 0.047 (12)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn | 0.0380 (3) | 0.0373 (4) | 0.0365 (4) | 0.000 | 0.0216 (3) | 0.000 |
Cl | 0.0687 (7) | 0.0678 (8) | 0.0508 (6) | −0.0247 (5) | 0.0267 (5) | −0.0198 (5) |
N1 | 0.0376 (15) | 0.0395 (16) | 0.0345 (16) | −0.0001 (13) | 0.0211 (13) | 0.0024 (13) |
C1 | 0.064 (3) | 0.063 (3) | 0.034 (2) | 0.017 (2) | 0.0256 (19) | 0.007 (2) |
N2 | 0.0415 (16) | 0.0332 (17) | 0.0516 (19) | 0.0003 (13) | 0.0266 (14) | −0.0068 (14) |
C2 | 0.059 (2) | 0.055 (3) | 0.046 (2) | 0.020 (2) | 0.025 (2) | 0.015 (2) |
C3 | 0.0424 (19) | 0.034 (2) | 0.053 (2) | −0.0012 (16) | 0.0306 (18) | −0.0019 (17) |
C4 | 0.061 (3) | 0.037 (2) | 0.071 (3) | 0.005 (2) | 0.041 (2) | 0.001 (2) |
C5 | 0.042 (2) | 0.036 (2) | 0.047 (2) | 0.0049 (17) | 0.0180 (18) | −0.0100 (17) |
C6 | 0.047 (2) | 0.033 (2) | 0.068 (3) | −0.0027 (19) | 0.033 (2) | −0.011 (2) |
C7 | 0.061 (2) | 0.064 (3) | 0.034 (2) | 0.015 (2) | 0.0262 (19) | 0.000 (2) |
C8 | 0.048 (2) | 0.055 (2) | 0.034 (2) | 0.0153 (19) | 0.0189 (17) | 0.0059 (18) |
Geometric parameters (Å, º) top
Zn—N1i | 2.061 (3) | C3—C7 | 1.375 (6) |
Zn—N1 | 2.061 (3) | C3—C4 | 1.500 (5) |
Zn—Cl | 2.2139 (11) | C4—H4B | 1.02 (4) |
Zn—Cli | 2.2139 (11) | C4—H4A | 0.81 (4) |
N1—C1 | 1.328 (5) | C5—C6 | 1.500 (6) |
N1—C8 | 1.330 (5) | C5—H5B | 0.96 (3) |
C1—C2 | 1.377 (6) | C5—H5A | 0.95 (5) |
C1—H1 | 0.96 (4) | C6—N2ii | 1.462 (5) |
N2—C5 | 1.454 (5) | C6—H6B | 0.81 (5) |
N2—C4 | 1.455 (5) | C6—H6A | 1.05 (4) |
N2—C6ii | 1.462 (5) | C7—C8 | 1.376 (6) |
C2—C3 | 1.375 (6) | C7—H7 | 0.97 (4) |
C2—H2 | 0.97 (5) | C8—H8 | 0.94 (4) |
| | | |
N1i—Zn—N1 | 102.13 (16) | C3—C4—H4B | 110 (2) |
N1i—Zn—Cl | 104.15 (8) | N2—C4—H4A | 115 (3) |
N1—Zn—Cl | 110.79 (9) | C3—C4—H4A | 106 (3) |
N1i—Zn—Cli | 110.79 (9) | H4B—C4—H4A | 103 (4) |
N1—Zn—Cli | 104.15 (8) | N2—C5—C6 | 110.1 (3) |
Cl—Zn—Cli | 123.02 (7) | N2—C5—H5B | 111 (2) |
C1—N1—C8 | 117.2 (3) | C6—C5—H5B | 107.1 (19) |
C1—N1—Zn | 120.7 (2) | N2—C5—H5A | 113 (3) |
C8—N1—Zn | 121.8 (3) | C6—C5—H5A | 110 (3) |
N1—C1—C2 | 123.0 (4) | H5B—C5—H5A | 106 (3) |
N1—C1—H1 | 114 (3) | N2ii—C6—C5 | 110.7 (3) |
C2—C1—H1 | 123 (3) | N2ii—C6—H6B | 106 (3) |
C5—N2—C4 | 111.6 (3) | C5—C6—H6B | 116 (3) |
C5—N2—C6ii | 108.8 (3) | N2ii—C6—H6A | 115 (2) |
C4—N2—C6ii | 110.4 (3) | C5—C6—H6A | 105 (2) |
C3—C2—C1 | 119.9 (4) | H6B—C6—H6A | 104 (4) |
C3—C2—H2 | 117 (3) | C3—C7—C8 | 120.1 (4) |
C1—C2—H2 | 123 (3) | C3—C7—H7 | 118 (2) |
C7—C3—C2 | 116.9 (4) | C8—C7—H7 | 122 (3) |
C7—C3—C4 | 121.7 (4) | N1—C8—C7 | 122.8 (4) |
C2—C3—C4 | 121.4 (4) | N1—C8—H8 | 121 (2) |
N2—C4—C3 | 113.3 (3) | C7—C8—H8 | 117 (2) |
N2—C4—H4B | 110 (2) | | |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x+1/2, −y+1/2, −z. |
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