[H₃N(CH₂)₃NH₃]_0.5[ZnPO₄], an organically templated zincophosphate analogue of the aluminosilicate zeolite edingtonite

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 [d_av(Zn—O) = 1.945 (9) Å, d_av(P—O) = 1.513 (10) Å and θ_av(Zn—O—P) = 134 (5)°] encapsulate the highly disordered propane-1,3-di­ammonium cations in a three-dimensional 8-ring channel system.

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


 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.

 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

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)

Crystal data

0.5C3H12N2·ZnPO4	Dx = 2.024 Mg m^−3
Mr = 198.42	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P421c	Cell parameters from 3235 reflections
a = 9.9015 (12) Å	θ = 1.6–27.6°
c = 13.4199 (16) Å	µ = 4.86 mm^−1
V = 1315.7 (3) Å^3	T = 298 K
Z = 10	Rod, colourless
F(000) = 770	0.45 × 0.04 × 0.04 mm

Data collection

Bruker SMART1000 CCD diffractometer	1923 independent reflections
Radiation source: fine-focus sealed tube	1620 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.098
ω scans	θmax = 30.0°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −13→13
Tmin = 0.840, Tmax = 0.928	k = −6→13
10634 measured reflections	l = −18→18

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.085	H-atom parameters not defined?
wR(F^2) = 0.222	w = 1/[σ^2(Fo^2) + (0.1153P)^2 + 13.2499P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max = 0.001
1923 reflections	Δρmax = 2.66 e Å^−3
68 parameters	Δρmin = −2.55 e Å^−3
0 restraints	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.00 (9)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.0000	0.0000	0.0000	0.0388 (7)
Zn2	0.14685 (11)	−0.10025 (12)	0.30322 (10)	0.0237 (3)
P1	0.0000	0.0000	0.5000	0.0225 (10)
P2	0.1161 (2)	0.1729 (3)	0.1840 (2)	0.0220 (5)
O1	0.1232 (10)	0.1110 (11)	0.0782 (7)	0.048 (3)
O2	0.1867 (9)	0.0844 (8)	0.2593 (6)	0.0325 (19)
O3	−0.0323 (9)	0.1932 (11)	0.2101 (8)	0.047 (2)
O4	0.1815 (8)	0.3100 (9)	0.1840 (9)	0.043 (2)
O5	0.0723 (13)	−0.1044 (10)	0.4383 (7)	0.054 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0377 (10)	0.0377 (10)	0.0410 (17)	0.000	0.000	0.000
Zn2	0.0184 (5)	0.0231 (6)	0.0296 (6)	0.0046 (4)	0.0003 (5)	−0.0038 (5)
P1	0.0242 (15)	0.0242 (15)	0.019 (2)	0.000	0.000	0.000
P2	0.0179 (11)	0.0250 (12)	0.0230 (13)	−0.0080 (9)	0.0007 (10)	0.0045 (10)
O1	0.044 (5)	0.072 (7)	0.028 (4)	−0.032 (5)	−0.004 (4)	−0.013 (4)
O2	0.044 (5)	0.015 (3)	0.038 (4)	−0.011 (3)	−0.014 (4)	0.013 (3)
O3	0.023 (4)	0.057 (6)	0.061 (7)	0.002 (4)	0.000 (4)	0.019 (5)
O4	0.025 (4)	0.028 (4)	0.076 (7)	−0.015 (3)	−0.006 (5)	0.009 (5)
O5	0.096 (9)	0.041 (6)	0.024 (4)	0.030 (6)	0.006 (5)	0.003 (4)

Geometric parameters (Å, º)

Zn1—O1	1.948 (8)	P1—O5^v	1.505 (10)
Zn1—O1^i	1.948 (8)	P1—O5^vi	1.505 (10)
Zn1—O1^ii	1.948 (8)	P1—O5^i	1.505 (10)
Zn1—O1^iii	1.948 (8)	P1—O5	1.505 (10)
Zn2—O3^i	1.923 (10)	P2—O4	1.504 (8)
Zn2—O4^iv	1.926 (7)	P2—O2	1.509 (8)
Zn2—O5	1.957 (10)	P2—O3	1.523 (9)
Zn2—O2	1.961 (7)	P2—O1	1.549 (9)
O1—Zn1—O1^i	114.8 (6)	O5^v—P1—O5	107.6 (4)
O1—Zn1—O1^ii	106.9 (3)	O5^vi—P1—O5	107.6 (4)
O1^i—Zn1—O1^ii	106.9 (3)	O5^i—P1—O5	113.2 (7)
O1—Zn1—O1^iii	106.9 (3)	O4—P2—O2	109.0 (5)
O1^i—Zn1—O1^iii	106.9 (3)	O4—P2—O3	107.2 (6)
O1^ii—Zn1—O1^iii	114.8 (6)	O2—P2—O3	111.7 (5)
O3^i—Zn2—O4^iv	111.0 (4)	O4—P2—O1	109.7 (6)
O3^i—Zn2—O5	111.7 (5)	O2—P2—O1	111.3 (6)
O4^iv—Zn2—O5	104.0 (5)	O3—P2—O1	107.8 (6)
O3^i—Zn2—O2	111.7 (4)	P2—O1—Zn1	133.5 (6)
O4^iv—Zn2—O2	106.2 (4)	P2—O2—Zn2	130.5 (5)
O5—Zn2—O2	111.9 (4)	P2—O3—Zn2^i	130.9 (6)
O5^v—P1—O5^vi	113.2 (7)	P2—O4—Zn2^vii	142.8 (6)
O5^v—P1—O5^i	107.6 (4)	P1—O5—Zn2	132.4 (6)
O5^vi—P1—O5^i	107.6 (4)

Symmetry codes: (i) −x, −y, z; (ii) −y, x, −z; (iii) y, −x, −z; (iv) −x+1/2, y−1/2, −z+1/2; (v) y, −x, −z+1; (vi) −y, x, −z+1; (vii) −x+1/2, y+1/2, −z+1/2.