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The title compound, catena-poly[[N-methyl­propane-1,3-diaminium [μ-phosphato-(μ-hydrogen phosphato)(μ-dihydrogen phosphato)dizincate(II)]], {(C4H14N2)[Zn2(PO4)(HPO4)(H2PO4)]}n, consists of macroanionic [Zn2(PO4)(HPO4)(H2PO4)]2− layers and inter­calated (C4H12N2)2+ cations. The layers are built up from ZnO4 and PO4/HPO4/H2PO4 tetra­hedra that result in small channels of approximate diameter 3.7 Å within the layers. Framework-to-framework O—H...O and template-to-framework N—H...O hydrogen bonds are important in stabilizing the structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805018908/hb6212sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805018908/hb6212Isup2.hkl
Contains datablock I

CCDC reference: 254432

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.028
  • wR factor = 0.086
  • Data-to-parameter ratio = 14.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 86 PerFit
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.440 From the CIF: _refine_ls_abs_structure_Flack_su 0.010 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.44 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.34 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10
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 27.48 From the CIF: _reflns_number_total 3108 Count of symmetry unique reflns 1709 Completeness (_total/calc) 181.86% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1399 Fraction of Friedel pairs measured 0.819 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 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 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Hooft, 2000); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and ATOMS (Dowty, 2004); software used to prepare material for publication: WinGX (Farrugia, 1999).

(I) top
Crystal data top
C4H14N22+·H3O12P3Zn22F(000) = 512
Mr = 508.85Dx = 2.273 Mg m3
Monoclinic, PnMelting point: structure decomposes befor melting K
Hall symbol: P -2yacMo Kα radiation, λ = 0.71073 Å
a = 11.8920 (2) ÅCell parameters from 1860 reflections
b = 5.1318 (1) Åθ = 2.6–27.5°
c = 12.3063 (2) ŵ = 3.61 mm1
β = 98.125 (1)°T = 295 K
V = 743.48 (2) Å3Prism, colourless
Z = 20.2 × 0.2 × 0.05 mm
Data collection top
Nonius KappaCCD area-detector
diffractometer
3108 independent reflections
Radiation source: fine-focus sealed tube3029 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.014
φ and ω scansθmax = 27.5°, θmin = 2.6°
Absorption correction: multi-scan
(DENZO-SMN; Otwinowski & Minor, 1997)
h = 1515
Tmin = 0.490, Tmax = 0.835k = 66
3295 measured reflectionsl = 1515
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028H-atom parameters constrained
wR(F2) = 0.087 w = 1/[σ2(Fo2) + (0.0502P)2 + 0.3227P]
where P = (Fo2 + 2Fc2)/3
S = 1.19(Δ/σ)max = 0.001
3108 reflectionsΔρmax = 0.64 e Å3
214 parametersΔρmin = 0.93 e Å3
2 restraintsAbsolute structure: Flack (1983), racemic twin, 1399 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.44 (1)
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
Zn10.24869 (3)0.18524 (7)0.24710 (3)0.01519 (13)
Zn20.09146 (3)0.20501 (7)0.44526 (3)0.01475 (13)
P10.08139 (13)0.43124 (15)0.59410 (12)0.01723 (16)
P20.23758 (10)0.28419 (19)0.49751 (10)0.0139 (2)
P30.09990 (10)0.30706 (15)0.19427 (10)0.0130 (2)
O10.0437 (3)0.2051 (5)0.2891 (3)0.0232 (8)
O20.1224 (3)0.1484 (6)0.5032 (3)0.0199 (7)
O30.3871 (3)0.2732 (7)0.1877 (3)0.0257 (7)
O40.0549 (3)0.2757 (7)0.4959 (3)0.0243 (7)
O50.2944 (3)0.1748 (5)0.4036 (3)0.0218 (7)
O60.2140 (3)0.1673 (5)0.1910 (3)0.0197 (7)
O70.0189 (3)0.2508 (9)0.0873 (3)0.0226 (7)
O80.3149 (3)0.2200 (7)0.6077 (3)0.0215 (7)
H80.38180.22510.59830.083 (6)*
O90.1197 (3)0.6007 (5)0.1994 (3)0.0239 (7)
O100.2225 (3)0.5783 (5)0.4894 (3)0.0243 (7)
O110.1778 (3)0.6248 (7)0.5468 (3)0.0279 (7)
H110.20450.69400.59750.083 (6)*
O120.0243 (3)0.5942 (7)0.6435 (3)0.0291 (8)
H120.04550.68440.59520.083 (6)*
N10.0314 (3)0.2361 (8)0.0148 (3)0.0294 (8)
H1A0.00790.10010.02720.083 (6)*
H1B0.10690.24230.02440.083 (6)*
H1C0.00360.38210.01750.083 (6)*
C10.0085 (6)0.2094 (17)0.1217 (5)0.058 (2)
H1D0.01990.35480.16800.083 (6)*
H1E0.02260.05070.15670.083 (6)*
C20.1371 (5)0.2013 (15)0.1127 (6)0.067 (2)
H2A0.16330.35970.14400.083 (6)*
H2B0.16920.19620.03570.083 (6)*
C30.1778 (6)0.0220 (12)0.1682 (6)0.0499 (15)
H3A0.13340.03860.24030.083 (6)*
H3B0.16600.17850.12700.083 (6)*
C40.3505 (5)0.2516 (11)0.2158 (5)0.0369 (12)
H4A0.40700.31390.15820.083 (6)*
H4B0.38480.22210.28080.083 (6)*
H4C0.29130.37900.23080.083 (6)*
N20.3017 (4)0.0026 (8)0.1809 (3)0.0364 (9)
H2C0.31020.12140.23080.083 (6)*
H2D0.34110.04770.11650.083 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0158 (3)0.0139 (2)0.0165 (3)0.00030 (14)0.00468 (19)0.00010 (15)
Zn20.0130 (3)0.0155 (2)0.0162 (3)0.00038 (16)0.00349 (18)0.00041 (17)
P10.0167 (3)0.0178 (4)0.0188 (3)0.0015 (4)0.0081 (2)0.0013 (4)
P20.0131 (6)0.0122 (5)0.0164 (6)0.0012 (3)0.0025 (5)0.0006 (3)
P30.0113 (6)0.0144 (5)0.0133 (6)0.0016 (3)0.0018 (4)0.0000 (3)
O10.019 (2)0.0321 (18)0.0190 (18)0.0050 (11)0.0051 (14)0.0030 (11)
O20.0166 (16)0.0160 (11)0.0284 (19)0.0033 (12)0.0074 (14)0.0034 (11)
O30.0180 (18)0.0325 (17)0.0288 (19)0.0015 (12)0.0115 (14)0.0074 (14)
O40.0215 (19)0.0259 (16)0.0277 (19)0.0001 (12)0.0115 (14)0.0096 (13)
O50.0204 (19)0.0310 (17)0.0144 (16)0.0088 (11)0.0043 (13)0.0019 (10)
O60.0167 (17)0.0129 (12)0.030 (2)0.0009 (10)0.0065 (14)0.0101 (10)
O70.0217 (19)0.0297 (13)0.0159 (17)0.0030 (14)0.0009 (13)0.0030 (13)
O80.0158 (17)0.0290 (17)0.0183 (17)0.0015 (12)0.0021 (12)0.0041 (12)
O90.0203 (16)0.0096 (13)0.041 (2)0.0002 (10)0.0020 (14)0.0002 (11)
O100.0196 (17)0.0131 (14)0.0397 (19)0.0008 (10)0.0017 (14)0.0025 (11)
O110.0287 (19)0.0292 (15)0.027 (2)0.0110 (14)0.0096 (15)0.0004 (13)
O120.0288 (19)0.0405 (19)0.0196 (17)0.0149 (14)0.0091 (14)0.0041 (13)
N10.024 (2)0.0335 (18)0.030 (2)0.0041 (14)0.0034 (15)0.0059 (15)
C10.028 (3)0.124 (7)0.024 (3)0.013 (3)0.008 (2)0.013 (3)
C20.029 (3)0.107 (6)0.067 (4)0.021 (3)0.014 (3)0.057 (4)
C30.036 (3)0.039 (3)0.068 (4)0.006 (2)0.014 (2)0.001 (3)
C40.047 (3)0.029 (2)0.035 (3)0.001 (2)0.007 (2)0.001 (2)
N20.036 (2)0.038 (2)0.036 (2)0.0057 (16)0.0084 (15)0.0062 (17)
Geometric parameters (Å, º) top
Zn1—O9i1.911 (3)O11—H110.8200
Zn1—O51.927 (4)O12—H120.8200
Zn1—O31.946 (3)N1—C11.465 (7)
Zn1—O61.960 (3)N1—H1A0.8900
Zn2—O11.926 (4)N1—H1B0.8900
Zn2—O10ii1.928 (3)N1—H1C0.8900
Zn2—O41.963 (3)C1—C21.518 (9)
Zn2—O21.965 (3)C1—H1D0.9700
P1—O3iii1.499 (4)C1—H1E0.9700
P1—O41.518 (3)C2—C31.452 (9)
P1—O121.560 (4)C2—H2A0.9700
P1—O111.566 (4)C2—H2B0.9700
P2—O101.522 (3)C3—N21.506 (8)
P2—O51.525 (3)C3—H3A0.9700
P2—O21.547 (3)C3—H3B0.9700
P2—O81.563 (4)C4—N21.492 (7)
P3—O11.517 (4)C4—H4A0.9600
P3—O91.525 (3)C4—H4B0.9600
P3—O61.540 (4)C4—H4C0.9600
P3—O71.545 (4)N2—H2C0.9000
O8—H80.8200N2—H2D0.9000
O9i—Zn1—O5115.08 (14)P1—O11—H11109.5
O9i—Zn1—O3115.87 (15)P1—O12—H12109.5
O5—Zn1—O3104.36 (16)C1—N1—H1A109.5
O9i—Zn1—O6107.62 (14)C1—N1—H1B109.5
O5—Zn1—O6109.99 (13)H1A—N1—H1B109.5
O3—Zn1—O6103.25 (15)C1—N1—H1C109.5
O1—Zn2—O10ii113.17 (15)H1A—N1—H1C109.5
O1—Zn2—O499.63 (16)H1B—N1—H1C109.5
O10ii—Zn2—O4121.41 (14)N1—C1—C2112.8 (5)
O1—Zn2—O2112.11 (13)N1—C1—H1D109.0
O10ii—Zn2—O2109.12 (14)C2—C1—H1D109.0
O4—Zn2—O2100.62 (14)N1—C1—H1E109.0
O3iii—P1—O4115.45 (15)C2—C1—H1E109.0
O3iii—P1—O12105.4 (2)H1D—C1—H1E107.8
O4—P1—O12110.2 (2)C3—C2—C1112.8 (5)
O3iii—P1—O11112.3 (2)C3—C2—H2A109.0
O4—P1—O11105.1 (2)C1—C2—H2A109.0
O12—P1—O11108.18 (16)C3—C2—H2B109.0
O10—P2—O5112.11 (19)C1—C2—H2B109.0
O10—P2—O2110.6 (2)H2A—C2—H2B107.8
O5—P2—O2111.0 (2)C2—C3—N2113.1 (5)
O10—P2—O8108.4 (2)C2—C3—H3A109.0
O5—P2—O8108.1 (2)N2—C3—H3A109.0
O2—P2—O8106.4 (2)C2—C3—H3B109.0
O1—P3—O9113.01 (19)N2—C3—H3B109.0
O1—P3—O6110.16 (19)H3A—C3—H3B107.8
O9—P3—O6109.27 (18)N2—C4—H4A109.5
O1—P3—O7107.6 (2)N2—C4—H4B109.5
O9—P3—O7107.1 (2)H4A—C4—H4B109.5
O6—P3—O7109.6 (2)N2—C4—H4C109.5
P3—O1—Zn2131.9 (2)H4A—C4—H4C109.5
P2—O2—Zn2121.39 (19)H4B—C4—H4C109.5
P1iv—O3—Zn1136.9 (3)C4—N2—C3113.5 (4)
P1—O4—Zn2130.0 (2)C4—N2—H2C108.9
P2—O5—Zn1130.9 (2)C3—N2—H2C108.9
P3—O6—Zn1124.30 (18)C4—N2—H2D108.9
P2—O8—H8109.5C3—N2—H2D108.9
P3—O9—Zn1ii133.9 (2)H2C—N2—H2D107.7
P2—O10—Zn2i132.3 (2)
O9—P3—O1—Zn261.8 (3)O10—P2—O5—Zn159.7 (3)
O6—P3—O1—Zn260.8 (3)O2—P2—O5—Zn164.6 (3)
O7—P3—O1—Zn2179.8 (3)O8—P2—O5—Zn1179.1 (2)
O10ii—Zn2—O1—P311.3 (3)O9i—Zn1—O5—P27.7 (3)
O4—Zn2—O1—P3141.6 (3)O3—Zn1—O5—P2135.8 (3)
O2—Zn2—O1—P3112.7 (2)O6—Zn1—O5—P2114.0 (3)
O10—P2—O2—Zn2150.3 (2)O1—P3—O6—Zn127.2 (3)
O5—P2—O2—Zn225.2 (3)O9—P3—O6—Zn1152.0 (2)
O8—P2—O2—Zn292.2 (3)O7—P3—O6—Zn191.0 (3)
O1—Zn2—O2—P282.5 (3)O9i—Zn1—O6—P343.9 (3)
O10ii—Zn2—O2—P243.7 (3)O5—Zn1—O6—P382.1 (3)
O4—Zn2—O2—P2172.4 (2)O3—Zn1—O6—P3167.0 (2)
O9i—Zn1—O3—P1iv16.6 (4)O1—P3—O9—Zn1ii99.8 (3)
O5—Zn1—O3—P1iv144.2 (3)O6—P3—O9—Zn1ii23.2 (4)
O6—Zn1—O3—P1iv100.8 (4)O7—P3—O9—Zn1ii141.9 (3)
O3iii—P1—O4—Zn2106.5 (3)O5—P2—O10—Zn2i104.5 (3)
O12—P1—O4—Zn212.8 (4)O2—P2—O10—Zn2i19.9 (4)
O11—P1—O4—Zn2129.1 (3)O8—P2—O10—Zn2i136.2 (3)
O1—Zn2—O4—P1145.4 (3)N1—C1—C2—C3127.5 (7)
O10ii—Zn2—O4—P120.6 (4)C1—C2—C3—N2167.6 (6)
O2—Zn2—O4—P199.7 (3)C2—C3—N2—C4167.8 (6)
Symmetry codes: (i) x, y+1, z; (ii) x, y1, z; (iii) x1/2, y, z+1/2; (iv) x+1/2, y, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8···O7v0.821.662.480 (5)176
O11—H11···O6vi0.821.762.567 (5)169
O12—H12···O2ii0.821.772.580 (5)167
N1—H1A···O70.891.962.823 (6)164
N1—H1B···O10vii0.892.253.085 (5)155
N2—H2D···O4iv0.902.082.938 (5)159
Symmetry codes: (ii) x, y1, z; (iv) x+1/2, y, z1/2; (v) x+1/2, y, z+1/2; (vi) x1/2, y1, z+1/2; (vii) x1/2, y+1, z1/2.
 

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