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The crystal structure of piperazinediium hexa­aqua­zinc(II) bis­(sulfate), (C4H12N2)[Zn(H2O)6](SO4)2, is built from isolated [Zn(H2O)6]2+, SO42- and C4H12N22+ ions linked together by a hydrogen-bonding network. The title compound exhibits strong analogies with some double aluminium sulfates, also known as Tutton's salts.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805005982/dn6201sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805005982/dn6201Isup2.hkl
Contains datablock I

CCDC reference: 270315

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.044
  • wR factor = 0.126
  • Data-to-parameter ratio = 30.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn - O13 .. 6.08 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).

Piperazinediium hexaaquazinc(II) bis(sulfate) top
Crystal data top
(C4H12N2)[Zn(H2O)6](SO4)2F(000) = 944
Mr = 453.74Dx = 1.795 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P_2ynCell parameters from 15427 reflections
a = 12.9562 (2) Åθ = 2.0–35.0°
b = 10.6502 (2) ŵ = 1.78 mm1
c = 13.3251 (2) ÅT = 292 K
β = 114.032 (1)°Prism, colourless
V = 1679.30 (5) Å30.20 × 0.18 × 0.15 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
7387 independent reflections
Radiation source: fine-focus sealed tube5221 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.073
Detector resolution: 9 pixels mm-1θmax = 35.0°, θmin = 2.5°
CCD rotation images, thick slices scansh = 2017
Absorption correction: analytical
(de Meulenaer & Tompa, 1965)
k = 1717
Tmin = 0.708, Tmax = 0.794l = 1921
27290 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.126H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0621P)2 + 0.263P]
where P = (Fo2 + 2Fc2)/3
7387 reflections(Δ/σ)max = 0.001
244 parametersΔρmax = 0.84 e Å3
18 restraintsΔρmin = 0.82 e Å3
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
xyzUiso*/Ueq
Zn0.495570 (17)0.506100 (17)0.241814 (16)0.03122 (7)
S10.79318 (4)0.37112 (4)0.13085 (3)0.02819 (9)
S20.24946 (4)0.64659 (4)0.39741 (3)0.02938 (9)
O10.72107 (17)0.48116 (15)0.09485 (14)0.0533 (4)
O20.91309 (12)0.40992 (16)0.17905 (11)0.0509 (4)
O30.77691 (13)0.28903 (13)0.03696 (11)0.0429 (3)
O40.76991 (14)0.30429 (14)0.21558 (13)0.0475 (4)
O50.25276 (19)0.51183 (13)0.38332 (19)0.0623 (6)
O60.25092 (13)0.71410 (13)0.30188 (11)0.0413 (3)
O70.34830 (16)0.6868 (2)0.49369 (13)0.0734 (6)
O80.14674 (14)0.67782 (13)0.41288 (15)0.0497 (4)
O110.42748 (14)0.41605 (13)0.09260 (12)0.0459 (4)
H110.383 (2)0.458 (2)0.0404 (19)0.055*
H120.406 (2)0.3433 (16)0.093 (2)0.055*
O120.60563 (14)0.35058 (16)0.29210 (13)0.0500 (4)
H210.635 (2)0.335 (3)0.3628 (14)0.060*
H220.658 (2)0.340 (3)0.270 (2)0.060*
O130.56650 (13)0.58934 (13)0.40060 (11)0.0411 (3)
H310.594 (2)0.5319 (18)0.4524 (18)0.049*
H320.6200 (18)0.6457 (18)0.422 (2)0.049*
O140.59735 (14)0.60520 (14)0.18522 (14)0.0459 (4)
H410.634 (2)0.564 (2)0.155 (2)0.055*
H420.644 (2)0.662 (2)0.224 (2)0.055*
O150.37782 (13)0.65604 (14)0.18686 (13)0.0435 (3)
H510.340 (2)0.676 (2)0.2230 (18)0.052*
H520.340 (2)0.666 (2)0.1200 (13)0.052*
O160.39560 (12)0.40605 (12)0.30433 (12)0.0379 (3)
H610.3542 (18)0.445 (2)0.3319 (19)0.045*
H620.3541 (19)0.3420 (18)0.2695 (19)0.045*
C10.59458 (18)1.0545 (2)0.08923 (17)0.0466 (5)
H1A0.65490.99560.09870.056*
H1B0.62511.12100.14310.056*
C20.4492 (2)0.89096 (19)0.02419 (19)0.0473 (5)
H2A0.38740.85300.03670.057*
H2B0.50410.82590.03110.057*
C30.54717 (18)0.89400 (18)0.57069 (16)0.0407 (4)
H3A0.60090.82530.59430.049*
H3B0.50320.89230.61470.049*
C40.38988 (17)0.98316 (19)0.41127 (17)0.0405 (4)
H4A0.33980.98470.44910.049*
H4B0.34420.97160.33340.049*
N10.47084 (13)0.87697 (14)0.45325 (13)0.0354 (3)
H1C0.43210.80480.44520.042*
H1D0.51240.87110.41330.042*
N20.50253 (15)0.98935 (15)0.10714 (14)0.0399 (4)
H2C0.53060.95440.17450.048*
H2D0.44981.04580.10450.048*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn0.02868 (12)0.03594 (12)0.02783 (12)0.00031 (7)0.01027 (9)0.00016 (7)
S10.0285 (2)0.03256 (19)0.02380 (19)0.00383 (14)0.01090 (15)0.00245 (13)
S20.0287 (2)0.03223 (19)0.0280 (2)0.00045 (14)0.01241 (16)0.00281 (14)
O10.0707 (12)0.0523 (8)0.0413 (9)0.0306 (8)0.0275 (8)0.0145 (6)
O20.0384 (8)0.0850 (11)0.0310 (7)0.0178 (7)0.0158 (6)0.0164 (7)
O30.0436 (8)0.0446 (7)0.0362 (7)0.0002 (6)0.0118 (6)0.0108 (5)
O40.0533 (9)0.0507 (8)0.0535 (9)0.0164 (6)0.0370 (8)0.0216 (6)
O50.0887 (15)0.0330 (7)0.0952 (15)0.0124 (7)0.0681 (13)0.0099 (7)
O60.0492 (8)0.0446 (7)0.0340 (7)0.0102 (6)0.0210 (6)0.0123 (5)
O70.0515 (10)0.1249 (16)0.0311 (8)0.0403 (11)0.0039 (7)0.0121 (9)
O80.0459 (9)0.0370 (7)0.0807 (11)0.0022 (6)0.0407 (9)0.0014 (7)
O110.0581 (10)0.0376 (7)0.0290 (7)0.0065 (6)0.0044 (6)0.0020 (5)
O120.0483 (9)0.0692 (10)0.0367 (8)0.0244 (7)0.0218 (7)0.0149 (7)
O130.0440 (8)0.0444 (7)0.0296 (7)0.0038 (6)0.0097 (6)0.0018 (5)
O140.0490 (9)0.0479 (8)0.0522 (9)0.0144 (6)0.0321 (8)0.0175 (6)
O150.0438 (8)0.0509 (8)0.0363 (7)0.0137 (6)0.0167 (6)0.0075 (6)
O160.0377 (7)0.0367 (6)0.0432 (7)0.0046 (5)0.0204 (6)0.0051 (5)
C10.0374 (11)0.0544 (12)0.0375 (10)0.0051 (9)0.0047 (8)0.0042 (9)
C20.0458 (12)0.0428 (10)0.0546 (13)0.0057 (8)0.0217 (10)0.0108 (8)
C30.0407 (10)0.0445 (9)0.0355 (9)0.0020 (8)0.0141 (8)0.0086 (7)
C40.0278 (9)0.0527 (11)0.0346 (10)0.0012 (7)0.0063 (7)0.0013 (7)
N10.0319 (8)0.0390 (7)0.0375 (8)0.0064 (6)0.0165 (7)0.0049 (6)
N20.0382 (9)0.0559 (9)0.0274 (7)0.0152 (7)0.0152 (7)0.0108 (6)
Geometric parameters (Å, º) top
Zn—O112.0549 (14)O15—H520.830 (16)
Zn—O142.0571 (15)O16—H610.868 (15)
Zn—O162.0942 (14)O16—H620.876 (15)
Zn—O122.1089 (14)C1—N21.481 (3)
Zn—O152.1222 (14)C1—C2i1.498 (3)
Zn—O132.1268 (14)C1—H1A0.9700
S1—O11.4531 (15)C1—H1B0.9700
S1—O41.4661 (14)C2—N21.475 (3)
S1—O31.4694 (13)C2—C1i1.498 (3)
S1—O21.4779 (15)C2—H2A0.9700
S2—O51.4503 (15)C2—H2B0.9700
S2—O71.4598 (17)C3—N11.483 (3)
S2—O81.4655 (15)C3—C4ii1.508 (3)
S2—O61.4688 (13)C3—H3A0.9700
O11—H110.830 (15)C3—H3B0.9700
O11—H120.827 (15)C4—N11.488 (3)
O12—H210.877 (16)C4—C3ii1.508 (3)
O12—H220.849 (16)C4—H4A0.9700
O13—H310.882 (15)C4—H4B0.9700
O13—H320.872 (15)N1—H1C0.9000
O14—H410.855 (15)N1—H1D0.9000
O14—H420.863 (16)N2—H2C0.9000
O15—H510.849 (15)N2—H2D0.9000
O11—Zn—O1488.36 (6)H51—O15—H52111 (2)
O11—Zn—O1693.21 (6)Zn—O16—H61120.9 (16)
O14—Zn—O16178.25 (6)Zn—O16—H62122.1 (16)
O11—Zn—O1284.79 (6)H61—O16—H62104.1 (18)
O14—Zn—O1293.90 (7)N2—C1—C2i110.19 (17)
O16—Zn—O1285.51 (6)N2—C1—H1A109.6
O11—Zn—O1593.00 (6)C2i—C1—H1A109.6
O14—Zn—O1588.02 (6)N2—C1—H1B109.6
O16—Zn—O1592.64 (6)C2i—C1—H1B109.6
O12—Zn—O15177.02 (6)H1A—C1—H1B108.1
O11—Zn—O13176.77 (5)N2—C2—C1i110.48 (16)
O14—Zn—O1393.96 (6)N2—C2—H2A109.6
O16—Zn—O1384.44 (6)C1i—C2—H2A109.6
O12—Zn—O1392.81 (6)N2—C2—H2B109.6
O15—Zn—O1389.33 (6)C1i—C2—H2B109.6
O1—S1—O4109.85 (9)H2A—C2—H2B108.1
O1—S1—O3110.41 (9)N1—C3—C4ii111.05 (15)
O4—S1—O3111.32 (9)N1—C3—H3A109.4
O1—S1—O2109.80 (11)C4ii—C3—H3A109.4
O4—S1—O2108.10 (9)N1—C3—H3B109.4
O3—S1—O2107.30 (9)C4ii—C3—H3B109.4
O5—S2—O7110.02 (14)H3A—C3—H3B108.0
O5—S2—O8108.61 (10)N1—C4—C3ii110.28 (16)
O7—S2—O8109.37 (12)N1—C4—H4A109.6
O5—S2—O6111.15 (10)C3ii—C4—H4A109.6
O7—S2—O6107.57 (9)N1—C4—H4B109.6
O8—S2—O6110.11 (9)C3ii—C4—H4B109.6
Zn—O11—H11116.1 (19)H4A—C4—H4B108.1
Zn—O11—H12116.0 (18)C3—N1—C4111.64 (14)
H11—O11—H12113 (2)C3—N1—H1C109.3
Zn—O12—H21115.8 (17)C4—N1—H1C109.3
Zn—O12—H22121.8 (18)C3—N1—H1D109.3
H21—O12—H22106 (2)C4—N1—H1D109.3
Zn—O13—H31111.3 (17)H1C—N1—H1D108.0
Zn—O13—H32124.7 (17)C2—N2—C1111.98 (16)
H31—O13—H32102.1 (18)C2—N2—H2C109.2
Zn—O14—H41117.7 (18)C1—N2—H2C109.2
Zn—O14—H42122.4 (18)C2—N2—H2D109.2
H41—O14—H42105.4 (19)C1—N2—H2D109.2
Zn—O15—H51120.0 (17)H2C—N2—H2D107.9
Zn—O15—H52119.5 (17)
Symmetry codes: (i) x+1, y+2, z; (ii) x+1, y+2, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O11—H11···O1iii0.83 (2)1.87 (2)2.688 (2)167 (3)
O11—H12···O8iv0.83 (2)1.88 (2)2.7038 (19)177 (3)
O12—H21···O7v0.88 (2)1.85 (2)2.697 (2)162 (2)
O12—H22···O40.85 (2)1.91 (2)2.753 (2)176 (3)
O13—H31···O5v0.88 (2)2.32 (2)3.073 (3)143 (2)
O13—H31···O7v0.88 (2)2.46 (2)3.253 (3)150 (2)
O13—H32···O3vi0.87 (2)1.95 (2)2.821 (2)172 (2)
O14—H41···O10.86 (2)1.86 (2)2.709 (2)176 (2)
O14—H42···O4vi0.86 (2)1.86 (2)2.711 (2)169 (3)
O15—H51···O60.85 (2)1.89 (2)2.736 (2)177 (3)
O15—H52···O3iii0.83 (2)2.08 (2)2.896 (2)168 (2)
O16—H61···O50.87 (2)1.86 (2)2.718 (2)173 (2)
O16—H62···O6iv0.88 (2)1.89 (2)2.7564 (19)172 (2)
N1—H1C···O70.901.942.759 (2)151
N1—H1C···O60.902.543.243 (2)136
N1—H1D···O2vi0.901.892.766 (2)163
N2—H2C···O2vi0.901.852.737 (2)170
N2—H2D···O8vii0.901.832.724 (2)170
Symmetry codes: (iii) x+1, y+1, z; (iv) x+1/2, y1/2, z+1/2; (v) x+1, y+1, z+1; (vi) x+3/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1/2.
 

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