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The transition-metal orthophosphate, β-Cd3(PO4)2, was synthesized by a solid-state reaction and characterized by single-crystal X-ray diffraction and EDS spectroscopy. It crystallizes in the monoclinic system, space group P21/n.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989023009775/oo2001sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989023009775/oo2001Isup2.hkl
Contains datablock I

CCDC reference: 2306650

Computing details top

Tricadmium bis(orthophosphate) top
Crystal data top
Cd3(PO4)2F(000) = 2856
Mr = 527.14Dx = 5.165 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 9.1895 (7) ÅCell parameters from 9851 reflections
b = 10.3507 (8) Åθ = 2.2–36.3°
c = 21.6887 (16) ŵ = 9.81 mm1
β = 99.644 (3)°T = 296 K
V = 2033.8 (3) Å3Parallelepiped, colourless
Z = 120.31 × 0.27 × 0.22 mm
Data collection top
Bruker X8 APEX Diffractometer9851 independent reflections
Radiation source: fine-focus sealed tube8280 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
φ and ω scansθmax = 36.3°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
h = 1515
Tmin = 0.544, Tmax = 0.747k = 1717
129694 measured reflectionsl = 3636
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: dual
R[F2 > 2σ(F2)] = 0.023Secondary atom site location: difference Fourier map
wR(F2) = 0.054 w = 1/[σ2(Fo2) + (0.0205P)2 + 4.3579P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.004
9851 reflectionsΔρmax = 1.60 e Å3
352 parametersΔρmin = 1.74 e Å3
Special details top

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.

Refinement. The crystal structure of β-Cd3(PO4)2 was investigated using single-crystal X-ray diffraction data collected at room temperature with a Bruker D8 Venture Super DUO Diffractometer equipped with a PHOTON100 CMOS area-detector and monochromatic MoKα radiation (λ=0.71073 Å). APEX3 (Bruker, APEX3 (Version 5.054), SAINT (Version 6.36A), SADABS. (Bruker, 2016) software was used for data reduction and the absorption correction was performed by multi-scan semi-empirical method using SADABS program (Krause, et al. 2015). The crystal structure was solved using dual space algorithm as implemented in SHELXT program (Sheldrick, 2015a), completed by a Difference Fourier map and refined by least-squares using SHELXL program (Sheldrick 2015b) integrated into the WinGX interface (Farrugia, 2012).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cd10.74691 (2)0.71080 (2)0.36476 (2)0.01178 (3)
Cd20.27909 (2)0.39633 (2)0.92293 (2)0.01251 (3)
Cd30.60228 (2)0.39417 (2)0.58439 (2)0.01124 (3)
Cd40.94569 (2)0.28838 (2)0.95686 (2)0.01149 (3)
Cd50.71202 (2)0.41020 (2)0.77990 (2)0.01002 (3)
Cd60.05148 (2)0.60385 (2)0.74786 (2)0.01157 (3)
Cd70.60491 (2)0.60229 (2)0.89221 (2)0.00988 (3)
Cd80.40399 (2)0.70425 (2)0.70409 (2)0.01088 (3)
Cd90.93970 (2)0.59251 (2)0.56014 (2)0.01049 (3)
P10.69824 (6)0.43486 (5)0.43995 (2)0.00739 (9)
P20.95135 (6)0.36168 (6)0.67096 (3)0.00825 (9)
P30.69971 (7)0.64250 (6)0.66858 (3)0.00801 (9)
P40.35072 (6)0.42713 (5)0.77938 (2)0.00705 (9)
P50.03383 (6)0.57903 (5)0.89456 (2)0.00714 (9)
P60.62768 (7)0.35381 (6)1.00079 (3)0.00835 (9)
O10.7195 (2)0.32411 (17)0.39518 (8)0.0153 (3)
O20.62835 (19)0.55464 (17)0.40326 (8)0.0120 (3)
O30.84808 (19)0.46875 (17)0.47901 (8)0.0132 (3)
O40.5870 (2)0.39020 (19)0.48128 (8)0.0158 (3)
O50.8179 (2)0.30534 (18)0.62739 (9)0.0161 (3)
O61.0338 (2)0.4652 (2)0.63983 (10)0.0255 (5)
O71.0579 (2)0.24766 (18)0.68907 (8)0.0166 (3)
O80.9105 (2)0.41803 (19)0.73139 (8)0.0175 (4)
O90.7346 (2)0.57633 (18)0.60939 (8)0.0153 (3)
O100.5947 (2)0.75733 (17)0.64955 (8)0.0149 (3)
O110.8400 (2)0.70048 (17)0.70769 (9)0.0154 (3)
O120.6177 (2)0.5506 (2)0.70596 (9)0.0204 (4)
O130.28310 (19)0.54515 (17)0.74156 (8)0.0117 (3)
O140.3730 (2)0.31593 (17)0.73519 (8)0.0138 (3)
O150.50013 (19)0.45790 (17)0.82041 (8)0.0125 (3)
O160.2369 (2)0.38617 (18)0.82065 (8)0.0138 (3)
O170.0602 (2)0.63773 (19)0.84925 (8)0.0163 (3)
O180.18533 (19)0.53473 (17)0.85947 (8)0.0128 (3)
O190.0598 (2)0.68256 (17)0.94219 (8)0.0136 (3)
O200.05089 (19)0.46386 (16)0.92864 (8)0.0117 (3)
O210.4881 (2)0.30043 (18)0.95967 (9)0.0168 (3)
O220.6649 (2)0.49060 (17)0.98153 (8)0.0156 (3)
O230.7475 (2)0.25479 (18)0.99447 (9)0.0186 (4)
O240.6119 (2)0.36004 (19)1.07107 (8)0.0167 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01169 (7)0.01256 (7)0.01087 (6)0.00280 (6)0.00125 (5)0.00014 (5)
Cd20.01060 (7)0.01629 (8)0.00983 (6)0.00050 (6)0.00060 (5)0.00269 (5)
Cd30.00935 (7)0.01100 (7)0.01280 (7)0.00021 (5)0.00021 (5)0.00116 (5)
Cd40.01258 (7)0.01305 (7)0.00873 (6)0.00046 (6)0.00142 (5)0.00123 (5)
Cd50.01194 (7)0.00914 (7)0.00902 (6)0.00021 (5)0.00187 (5)0.00066 (5)
Cd60.00914 (7)0.01060 (7)0.01430 (7)0.00063 (5)0.00009 (5)0.00122 (5)
Cd70.01032 (7)0.01008 (7)0.00935 (6)0.00014 (5)0.00200 (5)0.00078 (5)
Cd80.01204 (7)0.01262 (7)0.00817 (6)0.00067 (5)0.00220 (5)0.00167 (5)
Cd90.01215 (7)0.01086 (7)0.00841 (6)0.00036 (5)0.00158 (5)0.00089 (5)
P10.0078 (2)0.0074 (2)0.0064 (2)0.00011 (18)0.00040 (17)0.00001 (17)
P20.0080 (2)0.0090 (2)0.0074 (2)0.00023 (18)0.00032 (17)0.00032 (18)
P30.0085 (2)0.0079 (2)0.0072 (2)0.00045 (18)0.00022 (17)0.00030 (17)
P40.0076 (2)0.0069 (2)0.00626 (19)0.00028 (18)0.00013 (17)0.00019 (17)
P50.0077 (2)0.0068 (2)0.0065 (2)0.00028 (18)0.00001 (17)0.00010 (17)
P60.0090 (2)0.0093 (2)0.0066 (2)0.00031 (18)0.00063 (18)0.00027 (18)
O10.0210 (9)0.0105 (7)0.0122 (7)0.0037 (6)0.0040 (6)0.0047 (6)
O20.0108 (7)0.0113 (7)0.0139 (7)0.0031 (6)0.0018 (6)0.0041 (6)
O30.0094 (7)0.0163 (8)0.0127 (7)0.0006 (6)0.0016 (6)0.0052 (6)
O40.0163 (8)0.0198 (9)0.0118 (7)0.0071 (7)0.0042 (6)0.0019 (6)
O50.0124 (8)0.0132 (8)0.0194 (8)0.0010 (6)0.0070 (6)0.0054 (6)
O60.0160 (9)0.0360 (12)0.0225 (9)0.0078 (8)0.0023 (7)0.0188 (9)
O70.0176 (9)0.0154 (8)0.0157 (8)0.0064 (7)0.0010 (6)0.0020 (6)
O80.0161 (9)0.0231 (9)0.0145 (7)0.0024 (7)0.0060 (6)0.0087 (7)
O90.0155 (8)0.0166 (8)0.0145 (7)0.0019 (7)0.0048 (6)0.0060 (6)
O100.0162 (8)0.0117 (8)0.0157 (7)0.0051 (6)0.0004 (6)0.0013 (6)
O110.0124 (8)0.0102 (8)0.0203 (8)0.0006 (6)0.0066 (6)0.0037 (6)
O120.0143 (9)0.0254 (10)0.0212 (9)0.0013 (7)0.0022 (7)0.0144 (8)
O130.0094 (7)0.0108 (7)0.0144 (7)0.0015 (6)0.0002 (6)0.0046 (6)
O140.0175 (8)0.0109 (7)0.0116 (7)0.0043 (6)0.0020 (6)0.0042 (6)
O150.0095 (7)0.0145 (8)0.0122 (7)0.0004 (6)0.0019 (6)0.0030 (6)
O160.0138 (8)0.0177 (8)0.0103 (7)0.0043 (6)0.0034 (6)0.0015 (6)
O170.0179 (9)0.0194 (9)0.0122 (7)0.0069 (7)0.0045 (6)0.0041 (6)
O180.0080 (7)0.0155 (8)0.0141 (7)0.0006 (6)0.0004 (6)0.0058 (6)
O190.0199 (9)0.0095 (7)0.0098 (6)0.0042 (6)0.0025 (6)0.0026 (6)
O200.0115 (7)0.0093 (7)0.0141 (7)0.0022 (6)0.0015 (6)0.0029 (6)
O210.0134 (8)0.0153 (8)0.0185 (8)0.0015 (6)0.0065 (6)0.0026 (7)
O220.0207 (9)0.0112 (8)0.0133 (7)0.0040 (6)0.0017 (6)0.0036 (6)
O230.0153 (9)0.0152 (8)0.0272 (9)0.0027 (7)0.0092 (7)0.0004 (7)
O240.0165 (9)0.0258 (10)0.0080 (6)0.0053 (7)0.0030 (6)0.0029 (6)
Geometric parameters (Å, º) top
Cd1—O22.1913 (17)Cd8—O132.2156 (17)
Cd1—O14i2.2782 (17)Cd8—O1i2.2783 (17)
Cd1—O17ii2.3068 (18)Cd8—O16xii2.2973 (18)
Cd1—O24iii2.3243 (18)Cd8—O7iii2.3285 (18)
Cd1—O7iv2.338 (2)Cd8—O102.3381 (19)
Cd2—O162.1896 (17)Cd8—O122.522 (2)
Cd2—O212.1900 (19)Cd9—O32.2248 (17)
Cd2—O202.2336 (18)Cd9—O62.2297 (19)
Cd2—O22v2.3602 (18)Cd9—O21iii2.3135 (19)
Cd2—O1vi2.3996 (18)Cd9—O92.3230 (18)
Cd3—O42.2176 (17)Cd9—O3iv2.3411 (18)
Cd3—O52.2409 (18)Cd9—O23iii2.550 (2)
Cd3—O2i2.2437 (17)P1—O31.5316 (18)
Cd3—O92.2598 (18)P1—O11.5358 (18)
Cd3—O19vii2.2818 (18)P1—O41.5388 (18)
Cd4—O232.1454 (19)P1—O21.5529 (17)
Cd4—O20viii2.1924 (17)P2—O61.533 (2)
Cd4—O4ix2.2702 (18)P2—O51.5327 (18)
Cd4—O19v2.2836 (17)P2—O81.5376 (18)
Cd4—O10x2.2978 (18)P2—O71.5417 (19)
Cd5—O122.2292 (18)P3—O121.5283 (19)
Cd5—O18viii2.2326 (17)P3—O91.5354 (18)
Cd5—O11x2.2486 (18)P3—O111.5409 (18)
Cd5—O82.2543 (18)P3—O101.5430 (18)
Cd5—O152.3196 (18)P4—O141.5334 (18)
Cd6—O172.2150 (18)P4—O151.5391 (18)
Cd6—O11xi2.2293 (18)P4—O131.5430 (17)
Cd6—O132.2396 (17)P4—O161.5451 (18)
Cd6—O14xii2.3131 (18)P5—O191.5348 (18)
Cd6—O8xi2.313 (2)P5—O171.5383 (18)
Cd7—O222.2441 (17)P5—O181.5404 (18)
Cd7—O152.2547 (17)P5—O201.5429 (17)
Cd7—O18viii2.2732 (17)P6—O231.527 (2)
Cd7—O5iii2.2808 (18)P6—O221.5311 (19)
Cd7—O24v2.2990 (19)P6—O211.5372 (19)
Cd7—O7iii2.5935 (19)P6—O241.5566 (18)
O2—Cd1—O14i94.64 (7)O15—Cd7—O7iii77.53 (6)
O2—Cd1—O17ii98.73 (7)O18viii—Cd7—O7iii112.89 (6)
O14i—Cd1—O17ii73.41 (6)O5iii—Cd7—O7iii60.05 (6)
O2—Cd1—O24iii121.70 (6)O24v—Cd7—O7iii72.69 (6)
O14i—Cd1—O24iii141.54 (7)O13—Cd8—O1i92.86 (7)
O17ii—Cd1—O24iii87.86 (7)O13—Cd8—O16xii113.40 (7)
O2—Cd1—O7iv142.93 (6)O1i—Cd8—O16xii73.32 (6)
O14i—Cd1—O7iv80.58 (7)O13—Cd8—O7iii77.26 (6)
O17ii—Cd1—O7iv114.60 (7)O1i—Cd8—O7iii158.96 (7)
O24iii—Cd1—O7iv77.21 (6)O16xii—Cd8—O7iii93.39 (6)
O16—Cd2—O21110.02 (7)O13—Cd8—O10145.55 (6)
O16—Cd2—O2093.60 (7)O1i—Cd8—O1081.31 (7)
O21—Cd2—O20153.63 (7)O16xii—Cd8—O1097.48 (6)
O16—Cd2—O22v152.72 (7)O7iii—Cd8—O10117.23 (7)
O21—Cd2—O22v81.75 (7)O13—Cd8—O1287.84 (6)
O20—Cd2—O22v82.22 (7)O1i—Cd8—O12101.36 (7)
O16—Cd2—O1vi72.91 (6)O16xii—Cd8—O12158.06 (6)
O21—Cd2—O1vi79.03 (7)O7iii—Cd8—O1296.82 (7)
O20—Cd2—O1vi97.73 (7)O10—Cd8—O1260.58 (6)
O22v—Cd2—O1vi134.32 (6)O3—Cd9—O6108.60 (8)
O4—Cd3—O5108.31 (7)O3—Cd9—O21iii118.11 (7)
O4—Cd3—O2i102.91 (7)O6—Cd9—O21iii127.43 (7)
O5—Cd3—O2i146.53 (7)O3—Cd9—O995.37 (6)
O4—Cd3—O9101.42 (7)O6—Cd9—O980.79 (7)
O5—Cd3—O980.78 (7)O21iii—Cd9—O9115.63 (7)
O2i—Cd3—O9104.80 (7)O3—Cd9—O3iv77.59 (7)
O4—Cd3—O19vii75.41 (6)O6—Cd9—O3iv83.26 (7)
O5—Cd3—O19vii79.23 (6)O21iii—Cd9—O3iv84.39 (7)
O2i—Cd3—O19vii97.58 (7)O9—Cd9—O3iv159.49 (7)
O9—Cd3—O19vii157.50 (7)O3—Cd9—O23iii82.85 (6)
O23—Cd4—O20viii133.04 (7)O6—Cd9—O23iii153.31 (7)
O23—Cd4—O4ix105.57 (7)O21iii—Cd9—O23iii59.54 (6)
O20viii—Cd4—O4ix118.55 (7)O9—Cd9—O23iii74.04 (6)
O23—Cd4—O19v86.54 (7)O3iv—Cd9—O23iii123.24 (6)
O20viii—Cd4—O19v90.31 (7)O3—P1—O1108.84 (10)
O4ix—Cd4—O19v74.37 (6)O3—P1—O4111.71 (10)
O23—Cd4—O10x110.78 (8)O1—P1—O4108.13 (11)
O20viii—Cd4—O10x80.80 (6)O3—P1—O2110.91 (10)
O4ix—Cd4—O10x96.33 (6)O1—P1—O2110.94 (10)
O19v—Cd4—O10x162.23 (7)O4—P1—O2106.28 (10)
O12—Cd5—O18viii104.06 (7)O6—P2—O5113.44 (11)
O12—Cd5—O11x130.59 (7)O6—P2—O8108.65 (12)
O18viii—Cd5—O11x122.38 (7)O5—P2—O8112.67 (11)
O12—Cd5—O883.60 (7)O6—P2—O7107.92 (12)
O18viii—Cd5—O894.01 (7)O5—P2—O7105.92 (10)
O11x—Cd5—O8107.18 (7)O8—P2—O7107.98 (11)
O12—Cd5—O1583.32 (7)O12—P3—O9110.88 (12)
O18viii—Cd5—O1581.78 (6)O12—P3—O11113.07 (11)
O11x—Cd5—O1587.22 (7)O9—P3—O11111.18 (11)
O8—Cd5—O15164.84 (7)O12—P3—O10106.22 (11)
O17—Cd6—O11xi101.60 (7)O9—P3—O10109.20 (10)
O17—Cd6—O13103.11 (7)O11—P3—O10105.98 (10)
O11xi—Cd6—O13150.83 (7)O14—P4—O15108.48 (10)
O17—Cd6—O14xii74.45 (6)O14—P4—O13110.24 (10)
O11xi—Cd6—O14xii81.67 (6)O15—P4—O13112.60 (10)
O13—Cd6—O14xii90.24 (7)O14—P4—O16109.29 (11)
O17—Cd6—O8xi102.19 (6)O15—P4—O16110.29 (10)
O11xi—Cd6—O8xi83.31 (7)O13—P4—O16105.89 (10)
O13—Cd6—O8xi106.17 (7)O19—P5—O17108.76 (11)
O14xii—Cd6—O8xi163.55 (7)O19—P5—O18108.10 (10)
O22—Cd7—O15105.64 (7)O17—P5—O18111.09 (10)
O22—Cd7—O18viii90.72 (7)O19—P5—O20109.87 (9)
O15—Cd7—O18viii82.34 (6)O17—P5—O20108.60 (11)
O22—Cd7—O5iii126.62 (7)O18—P5—O20110.39 (10)
O15—Cd7—O5iii126.31 (7)O23—P6—O22113.50 (11)
O18viii—Cd7—O5iii85.34 (7)O23—P6—O21104.52 (11)
O22—Cd7—O24v83.70 (7)O22—P6—O21112.15 (10)
O15—Cd7—O24v93.27 (7)O23—P6—O24107.62 (11)
O18viii—Cd7—O24v171.73 (7)O22—P6—O24106.90 (11)
O5iii—Cd7—O24v102.88 (7)O21—P6—O24112.17 (11)
O22—Cd7—O7iii156.36 (7)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1/2, y+3/2, z1/2; (iii) x+3/2, y+1/2, z+3/2; (iv) x+2, y+1, z+1; (v) x+1, y+1, z+2; (vi) x1/2, y+1/2, z+1/2; (vii) x+1/2, y1/2, z+3/2; (viii) x+1, y, z; (ix) x+1/2, y+1/2, z+1/2; (x) x+3/2, y1/2, z+3/2; (xi) x1, y, z; (xii) x+1/2, y+1/2, z+3/2.
Infrared bands of β-Cd3(PO4)2 and their assignments top
BandAssignment
431PO4 v2 out of plane bending modes
531PO4 v4 out of plane bending modes
544PO4 v4 out of plane bending modes
558PO4 v4 out of plane bending modes
570PO4 v4 out of plane bending modes
597PO4 v4 out of plane bending modes
624PO4 v4 out of plane bending modes
936The symmetric P—O stretching corresponds to the fundamental vibrational mode v1
971The symmetric P—O stretching corresponds to the fundamental vibrational mode v1
1026The triple-degenerate asymmetric P—O stretching mode corresponds to the v3 fundamental vibrational mode
1051The triple-degenerate asymmetric P—O stretching mode corresponds to the v3 fundamental vibrational mode
Divalent cation-based orthophosphates [M3(PO4)2] summary crystallographic data (Å, °, Å3) top
CompoundSpace groupabcβZVReference
Ca3(PO4)2P21/a12.89 (6)27.28 (5)15.22 (3)126.2 (9)244317.5Mathew et al. (1977)
Cd3(PO4)2P21/c9.22 (4)10.34 (9)24.90 (2)120.7 (1)122030.0Stephens (1967)
P21/n9.19 (7)10.35 (1)21.69 (9)99.6 (2)122033.8Present work
Co3(PO4)2P21/n5.06 (8)8.36 (2)8.79 (4)121.0 (1)2319.4Anderson et al. (1975)
Cr3(PO4)2P21/n4.97 (9)9.50 (3)6.48 (2)91.4 (3)2305.6Glaum et al. (2011)
Fe3(PO4)2P21/a10.44 (3)4.79 (2)6.03 (2)91.0 (5)2301.3Ericsson & Khangi (1988)
P21/n8.88 (2)11.17 (3)6.15 (8)99.4 (8)4601.0Kostiner & Rea (1974)
Mg3(PO4)2P21/n7.60 (7)8.23 (1)5.08 (1)94.1 (5)2316.6Nord & Kierkegaard (1968)
P21/m7.605 (2)8.233 (3)5.080 (1)94.19 (3)2317.2Baykal et al. (1997)
P21/n10.25 (9)4.72 (2)5.92 (4)90.9 (1)2287.0Nord & Stefanidis (1983)
Mn3(PO4)2P21/c8.94 (3)10.04 (1)24.12 (8)120.8 (3)121861.1Stephens & Calvo (1969)
P21/c8.80 (4)11.45 (1)6.25 (5)99.0 (2)4621.9Volkova et al. (2016)
P21/c8.92 (1)9.15 (9)8.66 (9)111.7 (1)4657.2Neher & Salguero (2017)
Ni3(PO4)2P21/n5.82 (6)4.69 (2)10.10 (5)91.1 (3)2276.1Escobal et al. (2005)
P21/c8.70 (2)11.12 (1)6.11 (2)100.0 (8)4581.7Nord & Stefanidis (1983)
Pb3(PO4)2C2/c13.81 (8)5.69 (8)9.43 (3)102.4 (3)4723.5Brixner et al. (1973)
Sr3(PO4)2R3m5.3901 (8)5.3901 (8)19.785 (5)4497.8Sugiyama & Tokonami (1990)
Ba3(PO4)2R3m5.6038 (7)5.6038 (7)21.000 (5)4571.1Sugiyama & Tokonami (1990)
Zn3(PO4)2P21/c5.07 (2)8.47 (3)8.77 (2)120.5 (5)2323.1Calvo (1963); Stephens & Calvo (1967)
C2/c8.14 (7)5.63 (3)15.04 (9)105.1 (8)4665.4Calvo (1965)
P21/n9.39 (8)9.17 (1)8.69 (3)125.7 (3)4607.3Stephens & Calvo (1969)
 

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