Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618009798/fn3263sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229618009798/fn3263Isup2.hkl |
CCDC reference: 1854647
Data collection: CrysAlis PRO (Agilent, 2012); cell refinement: CrysAlis PRO (Agilent, 2012); data reduction: CrysAlis PRO (Agilent, 2012); program(s) used to solve structure: SHELXT (Sheldrick, 2015a) within WinGX (Farrugia, 2012); program(s) used to refine structure: SHELXL2016 (Sheldrick, 2015b) within WinGX (Farrugia, 2012); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXT (Sheldrick, 2015a) within WinGX (Farrugia, 2012).
CsMn(H2O)6(PO4) | Dx = 2.558 Mg m−3 |
Mr = 390.92 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63mc | Cell parameters from 3866 reflections |
a = 6.9809 (7) Å | θ = 3.4–32.5° |
c = 12.0270 (9) Å | µ = 5.02 mm−1 |
V = 507.59 (11) Å3 | T = 293 K |
Z = 2 | Hexagonal prism, colourless |
F(000) = 374 | 0.12 × 0.08 × 0.06 mm |
Agilent Xcalibur Sapphire3 diffractometer | 737 independent reflections |
Radiation source: Enhance X-ray Source | 687 reflections with I > 2σ(I) |
Detector resolution: 16.0630 pixels mm-1 | Rint = 0.045 |
ω scans | θmax = 32.5°, θmin = 3.4° |
Absorption correction: gaussian Numerical absorption correction based on gaussian integration over a multifaceted crystal model | h = −10→10 |
Tmin = 0.380, Tmax = 0.658 | k = −10→10 |
9705 measured reflections | l = −18→17 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.033 | All H-atom parameters refined |
wR(F2) = 0.066 | w = 1/[σ2(Fo2) + (0.020P)2 + 0.8P] where P = (Fo2 + 2Fc2)/3 |
S = 1.16 | (Δ/σ)max < 0.001 |
737 reflections | Δρmax = 0.76 e Å−3 |
41 parameters | Δρmin = −0.79 e Å−3 |
4 restraints | Absolute structure: Flack x determined using 283 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.015 (18) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Cs1 | 0.666667 | 0.333333 | 0.43938 (17) | 0.0518 (3) | |
Mn1 | 0.333333 | 0.666667 | 0.31642 (19) | 0.0238 (4) | |
P1 | 0.000000 | 0.000000 | 0.6603 (2) | 0.0185 (4) | |
O1 | 0.1198 (3) | 0.2396 (6) | 0.6191 (5) | 0.0269 (8) | |
O2 | 0.000000 | 0.000000 | 0.7891 (6) | 0.030 (2) | |
O3 | 0.1816 (4) | 0.3632 (9) | 0.4103 (3) | 0.0496 (16) | |
O4 | 0.4834 (6) | 0.5166 (6) | 0.2141 (5) | 0.0507 (17) | |
H1 | 0.126 (3) | 0.252 (6) | 0.374 (5) | 0.06 (3)* | |
H2 | 0.387 (9) | 0.413 (7) | 0.182 (4) | 0.05 (2)* | |
H3 | 0.168 (8) | 0.337 (15) | 0.4755 (16) | 0.07 (4)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.0498 (4) | 0.0498 (4) | 0.0558 (6) | 0.0249 (2) | 0.000 | 0.000 |
Mn1 | 0.0256 (6) | 0.0256 (6) | 0.0202 (8) | 0.0128 (3) | 0.000 | 0.000 |
P1 | 0.0214 (6) | 0.0214 (6) | 0.0127 (9) | 0.0107 (3) | 0.000 | 0.000 |
O1 | 0.0336 (14) | 0.0221 (17) | 0.0212 (17) | 0.0110 (9) | 0.0022 (10) | 0.004 (2) |
O2 | 0.040 (3) | 0.040 (3) | 0.011 (3) | 0.0199 (15) | 0.000 | 0.000 |
O3 | 0.083 (4) | 0.026 (2) | 0.021 (2) | 0.0128 (12) | 0.0016 (11) | 0.003 (2) |
O4 | 0.033 (2) | 0.033 (2) | 0.071 (4) | 0.006 (3) | 0.0201 (16) | −0.0201 (16) |
Cs1—O4i | 3.500 (8) | Mn1—O3iii | 2.154 (5) |
Cs1—O4ii | 3.500 (8) | Mn1—O3 | 2.154 (5) |
Cs1—O4 | 3.501 (8) | Mn1—O4ix | 2.192 (5) |
Cs1—O3iii | 3.5125 (6) | Mn1—O4iii | 2.192 (5) |
Cs1—O3iv | 3.5126 (6) | Mn1—O4 | 2.192 (5) |
Cs1—O3 | 3.5126 (6) | P1—O1x | 1.531 (4) |
Cs1—O3ii | 3.5126 (6) | P1—O1iv | 1.531 (4) |
Cs1—O3i | 3.5126 (6) | P1—O1 | 1.531 (4) |
Cs1—O3v | 3.5126 (6) | P1—O2 | 1.550 (8) |
Cs1—O4vi | 3.769 (8) | O3—H1 | 0.8000 (15) |
Cs1—O4vii | 3.769 (8) | O3—H3 | 0.8000 (15) |
Cs1—O4viii | 3.769 (8) | O4—H2 | 0.8000 (15) |
Mn1—O3ix | 2.154 (5) | O4—H2xi | 0.8000 (15) |
O4i—Cs1—O4ii | 66.50 (13) | O4vi—Cs1—O4viii | 49.27 (14) |
O4i—Cs1—O4 | 66.50 (13) | O4vii—Cs1—O4viii | 49.27 (14) |
O4ii—Cs1—O4 | 66.50 (13) | O3ix—Mn1—O3iii | 95.04 (19) |
O4i—Cs1—O3iii | 116.84 (10) | O3ix—Mn1—O3 | 95.04 (19) |
O4ii—Cs1—O3iii | 87.45 (9) | O3iii—Mn1—O3 | 95.04 (19) |
O4—Cs1—O3iii | 50.35 (10) | O3ix—Mn1—O4ix | 86.67 (16) |
O4i—Cs1—O3iv | 50.35 (10) | O3iii—Mn1—O4ix | 177.5 (3) |
O4ii—Cs1—O3iv | 116.84 (10) | O3—Mn1—O4ix | 86.67 (16) |
O4—Cs1—O3iv | 87.45 (9) | O3ix—Mn1—O4iii | 86.67 (16) |
O3iii—Cs1—O3iv | 119.02 (3) | O3iii—Mn1—O4iii | 86.67 (16) |
O4i—Cs1—O3 | 87.45 (9) | O3—Mn1—O4iii | 177.5 (3) |
O4ii—Cs1—O3 | 116.84 (10) | O4ix—Mn1—O4iii | 91.6 (3) |
O4—Cs1—O3 | 50.35 (10) | O3ix—Mn1—O4 | 177.5 (3) |
O3iii—Cs1—O3 | 53.79 (17) | O3iii—Mn1—O4 | 86.67 (16) |
O3iv—Cs1—O3 | 65.56 (17) | O3—Mn1—O4 | 86.67 (16) |
O4i—Cs1—O3ii | 116.84 (10) | O4ix—Mn1—O4 | 91.6 (3) |
O4ii—Cs1—O3ii | 50.35 (10) | O4iii—Mn1—O4 | 91.6 (3) |
O4—Cs1—O3ii | 87.45 (9) | O3ix—Mn1—Cs1 | 128.24 (15) |
O3iii—Cs1—O3ii | 65.56 (17) | O3iii—Mn1—Cs1 | 54.527 (13) |
O3iv—Cs1—O3ii | 167.14 (15) | O3—Mn1—Cs1 | 54.528 (13) |
O3—Cs1—O3ii | 119.02 (3) | O4ix—Mn1—Cs1 | 125.580 (11) |
O4i—Cs1—O3i | 50.35 (10) | O4iii—Mn1—Cs1 | 125.580 (11) |
O4ii—Cs1—O3i | 87.45 (9) | O4—Mn1—Cs1 | 54.3 (2) |
O4—Cs1—O3i | 116.84 (10) | O3ix—Mn1—Cs1xii | 54.528 (14) |
O3iii—Cs1—O3i | 167.14 (15) | O3iii—Mn1—Cs1xii | 54.529 (13) |
O3iv—Cs1—O3i | 53.78 (17) | O3—Mn1—Cs1xii | 128.24 (15) |
O3—Cs1—O3i | 119.02 (3) | O4ix—Mn1—Cs1xii | 125.578 (11) |
O3ii—Cs1—O3i | 119.02 (3) | O4iii—Mn1—Cs1xii | 54.3 (2) |
O4i—Cs1—O3v | 87.45 (9) | O4—Mn1—Cs1xii | 125.580 (11) |
O4ii—Cs1—O3v | 50.35 (10) | Cs1—Mn1—Cs1xii | 108.79 (2) |
O4—Cs1—O3v | 116.84 (10) | O3ix—Mn1—Cs1xiii | 54.528 (14) |
O3iii—Cs1—O3v | 119.02 (3) | O3iii—Mn1—Cs1xiii | 128.24 (15) |
O3iv—Cs1—O3v | 119.02 (3) | O3—Mn1—Cs1xiii | 54.528 (14) |
O3—Cs1—O3v | 167.14 (15) | O4ix—Mn1—Cs1xiii | 54.3 (2) |
O3ii—Cs1—O3v | 53.78 (17) | O4iii—Mn1—Cs1xiii | 125.578 (11) |
O3i—Cs1—O3v | 65.56 (17) | O4—Mn1—Cs1xiii | 125.580 (11) |
O4i—Cs1—O4vi | 146.19 (4) | Cs1—Mn1—Cs1xiii | 108.79 (2) |
O4ii—Cs1—O4vi | 146.19 (4) | Cs1xii—Mn1—Cs1xiii | 108.78 (2) |
O4—Cs1—O4vi | 111.95 (2) | O1x—P1—O1iv | 110.1 (2) |
O3iii—Cs1—O4vi | 70.16 (11) | O1x—P1—O1 | 110.1 (2) |
O3iv—Cs1—O4vi | 96.43 (8) | O1iv—P1—O1 | 110.1 (2) |
O3—Cs1—O4vi | 70.16 (11) | O1x—P1—O2 | 108.9 (2) |
O3ii—Cs1—O4vi | 96.43 (8) | O1iv—P1—O2 | 108.9 (2) |
O3i—Cs1—O4vi | 119.28 (10) | O1—P1—O2 | 108.9 (2) |
O3v—Cs1—O4vi | 119.28 (10) | Mn1—O3—Cs1 | 95.51 (8) |
O4i—Cs1—O4vii | 146.19 (4) | Mn1—O3—Cs1xiii | 95.51 (8) |
O4ii—Cs1—O4vii | 111.95 (2) | Cs1—O3—Cs1xiii | 167.14 (15) |
O4—Cs1—O4vii | 146.19 (4) | Mn1—O3—H1 | 115 (5) |
O3iii—Cs1—O4vii | 96.43 (8) | Cs1—O3—H1 | 90.7 (6) |
O3iv—Cs1—O4vii | 119.28 (10) | Cs1xiii—O3—H1 | 90.7 (6) |
O3—Cs1—O4vii | 119.28 (10) | Mn1—O3—H3 | 133 (7) |
O3ii—Cs1—O4vii | 70.16 (11) | Cs1—O3—H3 | 83.8 (2) |
O3i—Cs1—O4vii | 96.43 (8) | Cs1xiii—O3—H3 | 83.8 (2) |
O3v—Cs1—O4vii | 70.16 (11) | H1—O3—H3 | 112 (8) |
O4vi—Cs1—O4vii | 49.27 (14) | Mn1—O4—Cs1 | 95.1 (2) |
O4i—Cs1—O4viii | 111.95 (2) | Mn1—O4—Cs1xiv | 95.4 (2) |
O4ii—Cs1—O4viii | 146.19 (4) | Cs1—O4—Cs1xiv | 169.50 (16) |
O4—Cs1—O4viii | 146.19 (4) | Mn1—O4—H2 | 108 (6) |
O3iii—Cs1—O4viii | 119.28 (10) | Cs1—O4—H2 | 110 (5) |
O3iv—Cs1—O4viii | 70.16 (11) | Cs1xiv—O4—H2 | 66 (5) |
O3—Cs1—O4viii | 96.43 (8) | Mn1—O4—H2xi | 108 (6) |
O3ii—Cs1—O4viii | 119.28 (10) | Cs1—O4—H2xi | 110 (5) |
O3i—Cs1—O4viii | 70.16 (11) | Cs1xiv—O4—H2xi | 66 (5) |
O3v—Cs1—O4viii | 96.43 (8) | H2—O4—H2xi | 122 (9) |
Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z; (iii) −y+1, x−y+1, z; (iv) −x+y, −x, z; (v) x+1, y, z; (vi) −x+1, −y+1, z+1/2; (vii) x−y+1, x, z+1/2; (viii) y, −x+y, z+1/2; (ix) −x+y, −x+1, z; (x) −y, x−y, z; (xi) −y+1, −x+1, z; (xii) x, y+1, z; (xiii) x−1, y, z; (xiv) −x+1, −y+1, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H1···O2xv | 0.80 (1) | 1.84 (1) | 2.636 (7) | 179 (7) |
O4—H2···O1xvi | 0.80 (1) | 1.93 (3) | 2.676 (4) | 155 (8) |
O3—H3···O1 | 0.80 (1) | 1.83 (2) | 2.620 (7) | 173 (10) |
Symmetry codes: (xv) −x, −y, z−1/2; (xvi) y, −x+y, z−1/2. |
Cs | Mn | P | H1 | H2 | H3 | Σ | |
O1 | 1.28×3\downarrow | 0.24×2? | 0.28 | 2.04 | |||
O2 | 1.17 | 0.27×3→ | 1.98 | ||||
O3 | 0.087×6\downarrow×2→ | 0.348×3\downarrow | 0.73 | 0.72 | 1.97 | ||
O4 | 0.086×3\downarrow, 0.075×3\downarrow | 0.318×3\downarrow | 0.76×2→ | 2.00 | |||
Σ | 1 | 2 | 5 | 1 | 1 | 1 |
Algorithm and empirical parameters for calculations were used from (Pyatenko, 1972). The symbols \downarrow and → indicate a multiplication of the corresponding contribution in the columns or rows by symmetry. |
Compound | Unit-cell parameters a, b, c (Å) | rA (Å) | <dA—O> (Å) | Reference |
Orthorhombic (space group Pmn21, Z = 2) | The sequence of layers (Abc) | |||
Struvite-K, KMg(H2O)6(PO4) | 6.903 (3), 6.174 (2), 11.146 (3) | 1.59 | 3.27 | Mathew et al. (1979) |
Struvite, NH4Mg(H2O)6(PO4) | 6.955 (1), 6.142 (1), 11.218 (2) | 1.60 | 3.31 | Ferraris et al. (1986) |
NH4Ni(H2O)6(PO4) | 6.9240 (14) , 6.1040 (12), 11.166 (2) | 1.60 | 3.29 | Blachnik et al. (1997) |
NH4Co(H2O)6(PO4) | 6.946 (2), 6.157 (2), 11.172 (6) | 1.60 | 3.30 | El Bali et al. (2005) |
(H2O)Ni(H2O)6[HPO4] | 6.9160 (3), 6.1032 (3), 11.1679 (6) | 3.30 | Wang et al. (2005) | |
RbMg(H2O)6(PO4) | 6.8381 (9), 6.1407 (9), 11.2454 (19) | 1.65 | 3.31 | Weil (2008b) |
TlMg(H2O)6(PO4) | 6.8129 (8), 6.1148 (10), 11.2769 (16) | 1.66 | 3.30 | Weil (2008b) |
KMg(H2O)6[AsO4] | 6.99 (3), 6.22 (2), 11.26 (4) | 1.59 | 3.32 | Abdija et al. (2014) |
NH4Mg(H2O)6[AsO4] | 7.054 (4), 6.205 (3), 11.368 (6) | 1.60 | 3.35 | Ferraris et al. (1973) |
RbMg(H2O)6[AsO4] | 6.9310 (9), 6.2054 (7), 11.3991 (7) | 1.65 | 3.35 | Weil (2008b) |
TlMg(H2O)6[AsO4] | 6.9591 (7), 6.1937 (5), 11.4306 (6) | 1.66 | 3.34 | Weil (2008b) |
Hexagonal (space group P63mc, Z = 2) | The sequence of layers (AbγA'cβ) | |||
CsMg(H2O)6(PO4) | 6.8827 (8), 11.9188 (16) | 1.88 | 3.54 | Weil (2008a) |
CsMn(H2O)6(PO4) | 6.9809 (7), 12.0270 (9) | 1.88 | 3.57 | This work |
Cubic (space group F43m, Z = 4) | The sequence of layers (AbγBcαCaβ) | |||
CsMg(H2O)6(PO4) | 10.0308 (14) | 1.88 | 3.57 | Massa et al. (2003) |
CsFe(H2O)6(PO4) | 10.06024 (5) | 1.88 | 3.58 | Carver et al. (2006) |
CsFe(D2O)6(PO4) | 10.02420 (9) | 1.88 | 3.58 | Carver et al. (2006) |
CsMg(H2O)6[AsO4] | 10.1609 (5) | 1.88 | 3.62 | Weil (2009) |
Related structures: tetragonal (space group P42/mmc, Z = 2) and orthorhombic (space group Pmnb, Z = 4) | ||||
Na(H2O)Mg(H2O)6 (PO4) | 6.731 (2), 10.982 (4) | 1.02 | 2.50 | Mathew et al. (1982) |
Hazenite, KNa(H2O)2Mg2(H2O)12(PO4)2 | 6.9349 (4), 25.174 (2), 11.2195 (8) | 1.59, 1.02 | 3.29 2.49 | Yang et al. (2011) |