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The crystal structure of Ga[B2P2O7(OH)5], obtained by mild hydrothermal synthesis, has been refined from X-ray powder diffraction data using the Rietveld method. It is isotypic with the iron borophosphate Fe[B2P2O7(OH)5] and has a two-dimensional layered structure.
Supporting information
Key indicators
- Powder X-ray study
- T = 295 K
- Mean (O-B) = 0.009 Å
- R factor = 0.000
- wR factor = 0.000
- Data-to-parameter ratio = 11.0
checkCIF/PLATON results
No syntax errors found
Alert level A
THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.4936
PLAT086_ALERT_2_A Unsatisfactory S Value (Too Low or Not Given) .. 0.00
Alert level C
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
calculated from the _atom_type* data lies outside
the range 0.99 <> 1.01
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_weight 350.32
TEST: Calculate formula weight from _atom _type_*
atom mass num sum
Ga 69.72 4 278.89
P 30.97 8 247.79
B 10.81 8 86.49
O 16.00 48 767.95
Calculated formula weight 345.28
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.99 <> 1.01
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_weight 350.32
TEST: Calculate formula weight from _atom_site_*
Note that site occupancies missing: assumed 1.0
atom mass num sum
Ga 69.72 1.00 69.72
P 30.97 2.00 61.95
B 10.81 2.00 21.62
O 16.00 12.00 191.99
Calculated formula weight 345.28
RADNW01_ALERT_1_C The radiation wavelength lies outside the expected range
for the supplied radiation type. Expected range 1.54175-1.54180
Wavelength given = 1.54060
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 350.32
PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_type* data.
Atom count from _chemical_formula_sum:H5 B2 Ga1 O12 P2
Atom count from the _atom_type data: B2 Ga1 O12 P2
FORMU01_ALERT_2_G 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:H5 B2 Ga1 O12 P2
Atom count from the _atom_site data: B2 Ga1 O12 P2
Note that site occupancies missing: assumed 1.0
RADNT01_ALERT_1_G Extra text has been found in the _diffrn_radiation_type field.
Radiation given as CuK\a~1~
Radiation identified as Cu K\a
2 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
4 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: WinXPOW (Stoe & Cie, 1999); cell refinement: CSD (Akselrud et al., 1989); data reduction: CSD; program(s) used to refine structure: CSD; molecular graphics: DIAMOND (Brandenburg, 1996–2001); software used to prepare material for publication: CSD.
gallium
catena-[monohydrogenborate-dihydrogenborate-bis(monohydrogenphosphate)]
top
Crystal data top
Ga[B2P2O7(OH)5] | Z = 4 |
Mr = 350.32 | F(000) = 688 |
Monoclinic, C2/c | Dx = 2.976 Mg m−3 |
Hall symbol: -C 2yc | CuKα1 radiation, λ = 1.540598 Å |
a = 17.6404 (3) Å | µ = 9.56 mm−1 |
b = 6.70735 (8) Å | T = 295 K |
c = 6.99525 (8) Å | Particle morphology: thin sheet |
β = 109.157 (1)° | white |
V = 781.85 (2) Å3 | Plate, 25 × 25 mm |
Data collection top
Stoe STADIP diffractometer | Data collection mode: transmission |
Ge(111) monochromator | Scan method: Stoe Guinier Image Plate |
Specimen mounting: packed powder pellet | 2θmin = 3°, 2θmax = 100°, 2θstep = 0.005° |
Refinement top
Refinement on Inet | 36 parameters |
Least-squares matrix: full with fixed elements per cycle | Primary atom site location: isomorphous structure methods |
Rp = 0.146 | H-atom parameters not refined |
Rwp = 0.069 | |
Rexp = 0.025 | (Δ/σ)max = 0.001 |
R(F) = 0.033 | Preferred orientation correction: Preferred orientation was refined using CSD
formula (Pecharsky et al., 1987): Icorr=Iobs/[1+(τ2-1).sin2φ]1/2 Axis 1 0 0, τ=1.869(1) |
Profile function: pseudo-Voigt | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ga1 | 0.25 | 0.25 | 0.5 | 0.0119 (3)* | |
P1 | 0.84767 (1) | 0.3729 (3) | 0.7048 (3) | 0.0157 (5)* | |
B1 | 0.0876 (5) | 0.2766 (12) | 0.1004 (9) | 0.011 (2)* | |
O1 | 0.3227 (2) | 0.2771 (6) | 0.3382 (5) | 0.0059 (12)* | |
O2 | 0.7788 (2) | 0.5137 (5) | 0.0476 (6) | 0.0057 (12)* | |
O3 | 0.0914 (3) | 0.4745 (6) | 0.1597 (6) | 0.0085 (12)* | |
O4 | 0.6059 (2) | 0.2585 (7) | 0.4110 (5) | 0.0189 (12)* | |
O5 | 0.5212 (3) | 0.3384 (5) | 0.5810 (6) | 0.0181 (14)* | |
O6 | 0.6573 (3) | 0.3410 (5) | 0.7551 (5) | 0.0181 (14)* | |
Geometric parameters (Å, º) top
Ga1—O2i | 1.840 (3) | O1—O2ii | 2.701 (5) |
Ga1—O2ii | 1.840 (3) | O1—O2i | 2.702 (5) |
Ga1—O1 | 1.978 (4) | O1—O6iv | 2.783 (5) |
Ga1—O1iii | 1.978 (4) | O1—O6v | 2.892 (6) |
Ga1—O6iv | 2.035 (4) | O2—O3i | 2.535 (6) |
Ga1—O6v | 2.035 (4) | O2—O4xii | 2.555 (6) |
P1—O1vi | 1.532 (4) | O2—O6xiii | 2.691 (6) |
P1—O2vii | 1.545 (4) | O2—O6ix | 2.795 (5) |
P1—O3viii | 1.560 (5) | O3—O6v | 2.401 (6) |
P1—O4ix | 1.593 (4) | O3—O5v | 2.407 (6) |
B1—O5v | 1.372 (10) | O3—O4v | 2.414 (6) |
B1—O3 | 1.386 (9) | O3—O4xiv | 2.547 (6) |
B1—O4v | 1.482 (8) | O4—O5 | 2.258 (6) |
B1—O6v | 1.559 (9) | O4—O6 | 2.343 (5) |
O1—O4i | 2.466 (5) | O5—O6 | 2.308 (7) |
O1—O3x | 2.530 (6) | O5—O5viii | 2.447 (5) |
O1—O2xi | 2.612 (5) | O5—O5iv | 2.704 (6) |
O1—O6viii | 2.695 (5) | | |
| | | |
O2i—Ga1—O2ii | 180.0 (2) | O6iv—Ga1—O6v | 180.0 (2) |
O2i—Ga1—O1 | 90.0 (2) | O1vi—P1—O2vii | 116.2 (2) |
O2i—Ga1—O1iii | 90.0 (2) | O1vi—P1—O3viii | 109.8 (2) |
O2i—Ga1—O6iv | 87.8 (2) | O1vi—P1—O4ix | 104.2 (2) |
O2i—Ga1—O6v | 92.2 (2) | O2vii—P1—O3viii | 109.5 (2) |
O2ii—Ga1—O1 | 90.0 (2) | O2vii—P1—O4ix | 109.0 (2) |
O2ii—Ga1—O1iii | 90.0 (2) | O3viii—P1—O4ix | 107.8 (2) |
O2ii—Ga1—O6iv | 92.2 (2) | O5v—B1—O3 | 121.6 (6) |
O2ii—Ga1—O6v | 87.8 (2) | O5v—B1—O4v | 104.6 (6) |
O1—Ga1—O1iii | 179.98 (15) | O5v—B1—O6v | 103.7 (5) |
O1—Ga1—O6iv | 87.8 (2) | O3—B1—O4v | 114.6 (6) |
O1—Ga1—O6v | 92.2 (2) | O3—B1—O6v | 109.1 (6) |
O1iii—Ga1—O6iv | 92.2 (2) | O4v—B1—O6v | 100.8 (5) |
O1iii—Ga1—O6v | 87.8 (2) | | |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) −x+1/2, −y+1/2, −z+1; (iv) −x+1, y, −z+3/2; (v) x−1/2, −y+1/2, z−1/2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x, −y+1, z+1/2; (viii) −x+1, −y+1, −z+1; (ix) −x+3/2, −y+1/2, −z+1; (x) −x+1/2, y−1/2, −z+1/2; (xi) x−1/2, y−1/2, z; (xii) −x+3/2, y+1/2, −z+1/2; (xiii) x, y, z−1; (xiv) x−1/2, y+1/2, z. |
Hydrogen-bond geometry (Å) top
D—H···A | D···A |
O1···O6iv | 2.783 (5) |
O1···O6v | 2.892 (6) |
O5···O5viii | 2.447 (5) |
O5···O5iv | 2.704 (6) |
Symmetry codes: (iv) −x+1, y, −z+3/2; (v) x−1/2, −y+1/2, z−1/2; (viii) −x+1, −y+1, −z+1. |
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