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Hydro­thermally prepared propane-1,3-di­ammonium bis­(zinc phosphate), [H3N(CH2)3NH3]0.5[ZnPO4] is an analogue of the aluminosilicate zeolite edingtonite. A three-dimensional network of vertex-sharing ZnO4 and PO4 tetrahedra [dav(Zn—O) = 1.945 (9) Å, dav(P—O) = 1.513 (10) Å and θav(Zn—O—P) = 134 (5)°] encapsulate the highly disordered propane-1,3-di­ammonium cations in a three-dimensional 8-ring channel system.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801008327/bt6049sup1.cif
Contains datablocks I, zpedis

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801008327/bt6049Isup2.hkl
Contains datablock I

CCDC reference: 170281

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](P-O) = 0.010 Å
  • Some non-H atoms missing
  • R factor = 0.085
  • wR factor = 0.222
  • Data-to-parameter ratio = 28.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
REFI_014 _refine_ls_hydrogen_treatment is missing Code for H-atom treatment. The following tests will not be performed HYDTR_01 ABSMU_01 Alert A The ratio of given/expected absorption coefficient lies outside the range 0.90 <> 1.10 Calculated value of mu = 6.119 Value of mu given = 4.860
Author response: this may have arisen due to the SQUEEZED data (see below)?
CHEMW_01  Alert A The ratio of given/expected molecular weight as calculated
          from the _chemical_formula_sum lies outside
          the range 0.90 <> 1.10
          Calculated formula weight =   248.0275
          Formula weight given      =   198.4200

DENSD_01  Alert A The ratio of the submitted crystal density and that
          calculated from the formula is outside the range 0.90 <> 1.10
          Crystal density given    =      2.024
          Calculated crystal density =      2.504
Author response: this may have arisen due to the SQUEEZED data (see below)?
PLAT_601  Alert A Structure Contains Solvent Accessible VOIDS of     259.00 A   3
Author response: Disordered template in an zeolite-like open framework as discussed below.

Yellow Alert Alert Level C:
CHEMW_01 Alert C The difference between the given and expected weight for compound is greater 1 mass unit. Check that all hydrogen atoms have been taken into account. DIFMN_02 Alert C The minimum difference density is < -0.1*ZMAX*0.75 _refine_diff_density_min given = -2.549 Test value = -2.250 DIFMN_03 Alert C The minimum difference density is < -0.1*ZMAX*0.75 The relevant atom site should be identified. DIFMX_01 Alert C The maximum difference density is > 0.1*ZMAX*0.75 _refine_diff_density_max given = 2.660 Test value = 2.250 DIFMX_02 Alert C The minimum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C1.875 H7.5 N1.25 O5 P1.25 Z Atom count from _chemical_formula_moiety:C1.5 H6 N1 O4 P1 Zn1 FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C1.875 H7.5 N1.25 O5 P1.25 Zn1. Atom count from the _atom_site data: O4 P1 Zn1 ABSTM_02 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 0.887 Tmax scaled 0.823 Tmin scaled 0.745 CELLZ_01 From the CIF: _cell_formula_units_Z 10 From the CIF: _chemical_formula_sum C1.875 H7.5 N1.25 O5 P1.25 Zn1.25 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 18.75 0.00 18.75 H 75.00 0.00 75.00 N 12.50 0.00 12.50 O 50.00 40.00 10.00 P 12.50 10.00 2.50 Zn 12.50 10.00 2.50 Difference between formula and atom_site contents detected. ALERT: Large difference may be due to a symmetry error - see SYMMG tests CHEMW_03 From the CIF: _cell_formula_units_Z 10 From the CIF: _chemical_formula_weight 198.42 TEST: Calculate formula weight from _atom_site_* atom mass num sum Zn 65.39 1.00 65.39 P 30.97 1.00 30.97 O 16.00 4.00 64.00 Calculated formula weight 160.36 ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 REFLT_03 From the CIF: _diffrn_reflns_theta_max 30.04 From the CIF: _reflns_number_total 1923 Count of symmetry unique reflns 1104 Completeness (_total/calc) 174.18% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 819 Fraction of Friedel pairs measured 0.742 Are heavy atom types Z>Si present yes 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.
4 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
5 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SMART; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997), ATOMS (Shape Software, 1999); software used to prepare material for publication: SHELXL97.

propane-1,3-diammonium bis(zinc phosphate) top
Crystal data top
0.5C3H12N2·ZnPO4Dx = 2.024 Mg m3
Mr = 198.42Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P421cCell parameters from 3235 reflections
a = 9.9015 (12) Åθ = 1.6–27.6°
c = 13.4199 (16) ŵ = 4.86 mm1
V = 1315.7 (3) Å3T = 298 K
Z = 10Rod, colourless
F(000) = 7700.45 × 0.04 × 0.04 mm
Data collection top
Bruker SMART1000 CCD
diffractometer
1923 independent reflections
Radiation source: fine-focus sealed tube1620 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.098
ω scansθmax = 30.0°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Bruker, 1999)
h = 1313
Tmin = 0.840, Tmax = 0.928k = 613
10634 measured reflectionsl = 1818
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)] = 0.085H-atom parameters not defined?
wR(F2) = 0.222 w = 1/[σ2(Fo2) + (0.1153P)2 + 13.2499P]
where P = (Fo2 + 2Fc2)/3
S = 1.10(Δ/σ)max = 0.001
1923 reflectionsΔρmax = 2.66 e Å3
68 parametersΔρmin = 2.55 e Å3
0 restraintsAbsolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.00 (9)
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
Zn10.00000.00000.00000.0388 (7)
Zn20.14685 (11)0.10025 (12)0.30322 (10)0.0237 (3)
P10.00000.00000.50000.0225 (10)
P20.1161 (2)0.1729 (3)0.1840 (2)0.0220 (5)
O10.1232 (10)0.1110 (11)0.0782 (7)0.048 (3)
O20.1867 (9)0.0844 (8)0.2593 (6)0.0325 (19)
O30.0323 (9)0.1932 (11)0.2101 (8)0.047 (2)
O40.1815 (8)0.3100 (9)0.1840 (9)0.043 (2)
O50.0723 (13)0.1044 (10)0.4383 (7)0.054 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0377 (10)0.0377 (10)0.0410 (17)0.0000.0000.000
Zn20.0184 (5)0.0231 (6)0.0296 (6)0.0046 (4)0.0003 (5)0.0038 (5)
P10.0242 (15)0.0242 (15)0.019 (2)0.0000.0000.000
P20.0179 (11)0.0250 (12)0.0230 (13)0.0080 (9)0.0007 (10)0.0045 (10)
O10.044 (5)0.072 (7)0.028 (4)0.032 (5)0.004 (4)0.013 (4)
O20.044 (5)0.015 (3)0.038 (4)0.011 (3)0.014 (4)0.013 (3)
O30.023 (4)0.057 (6)0.061 (7)0.002 (4)0.000 (4)0.019 (5)
O40.025 (4)0.028 (4)0.076 (7)0.015 (3)0.006 (5)0.009 (5)
O50.096 (9)0.041 (6)0.024 (4)0.030 (6)0.006 (5)0.003 (4)
Geometric parameters (Å, º) top
Zn1—O11.948 (8)P1—O5v1.505 (10)
Zn1—O1i1.948 (8)P1—O5vi1.505 (10)
Zn1—O1ii1.948 (8)P1—O5i1.505 (10)
Zn1—O1iii1.948 (8)P1—O51.505 (10)
Zn2—O3i1.923 (10)P2—O41.504 (8)
Zn2—O4iv1.926 (7)P2—O21.509 (8)
Zn2—O51.957 (10)P2—O31.523 (9)
Zn2—O21.961 (7)P2—O11.549 (9)
O1—Zn1—O1i114.8 (6)O5v—P1—O5107.6 (4)
O1—Zn1—O1ii106.9 (3)O5vi—P1—O5107.6 (4)
O1i—Zn1—O1ii106.9 (3)O5i—P1—O5113.2 (7)
O1—Zn1—O1iii106.9 (3)O4—P2—O2109.0 (5)
O1i—Zn1—O1iii106.9 (3)O4—P2—O3107.2 (6)
O1ii—Zn1—O1iii114.8 (6)O2—P2—O3111.7 (5)
O3i—Zn2—O4iv111.0 (4)O4—P2—O1109.7 (6)
O3i—Zn2—O5111.7 (5)O2—P2—O1111.3 (6)
O4iv—Zn2—O5104.0 (5)O3—P2—O1107.8 (6)
O3i—Zn2—O2111.7 (4)P2—O1—Zn1133.5 (6)
O4iv—Zn2—O2106.2 (4)P2—O2—Zn2130.5 (5)
O5—Zn2—O2111.9 (4)P2—O3—Zn2i130.9 (6)
O5v—P1—O5vi113.2 (7)P2—O4—Zn2vii142.8 (6)
O5v—P1—O5i107.6 (4)P1—O5—Zn2132.4 (6)
O5vi—P1—O5i107.6 (4)
Symmetry codes: (i) x, y, z; (ii) y, x, z; (iii) y, x, z; (iv) x+1/2, y1/2, z+1/2; (v) y, x, z+1; (vi) y, x, z+1; (vii) x+1/2, y+1/2, z+1/2.
 

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