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CaMo5O8 (calcium pentamolybdenum octaoxide) crystallizes in the space group P21/c and belongs to the LaMo5O8 structure type. Its crystal structure consists of Mo10O18 cluster units, interconnected through Mo-Mo bonds of 2.7669 Å to form infinite molybdenum oxide chains. These are interconnected through Mo-O-Mo bonds to create four-sided channels, in which the Ca2+ cations are located.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802010218/br6051sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802010218/br6051Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Mo-O) = 0.003 Å
  • R factor = 0.031
  • wR factor = 0.073
  • Data-to-parameter ratio = 31.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_732 Alert C Angle Calc 176.41(4), Rep 176.41(1) .... 2.67 s.u-Ratio MO4 -MO1 -MO2 1.555 1.555 1.555 General Notes
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 0.438 Tmax scaled 0.438 Tmin scaled 0.331
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: WinGX (Farrugia, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
CaMo5O8F(000) = 1176
Mr = 647.78Dx = 6.702 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ybcCell parameters from 25 reflections
a = 7.550 (5) Åθ = 8.3–16.1°
b = 9.068 (5) ŵ = 10.31 mm1
c = 9.983 (5) ÅT = 293 K
β = 110.07 (4)°Irregular, black
V = 642.0 (6) Å30.12 × 0.11 × 0.08 mm
Z = 4
Data collection top
Enraf-Nonius CAD-4
diffractometer
2812 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.025
Graphite monochromatorθmax = 39.9°, θmin = 2.9°
θ–2θ scansh = 013
Absorption correction: ψ scan
(North et al. 1968)
k = 016
Tmin = 0.755, Tmax = 1.00l = 1816
4174 measured reflections3 standard reflections every 60 min
3965 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031 w = 1/[σ2(Fo2) + (0.0301P)2 + 0.820P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.073(Δ/σ)max = 0.001
S = 1.05Δρmax = 1.99 e Å3
3965 reflectionsΔρmin = 2.44 e Å3
128 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00189 (13)
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
Ca0.26502 (12)0.50520 (10)0.52649 (9)0.01094 (13)
Mo10.61063 (4)0.11555 (3)0.48386 (3)0.00331 (5)
Mo20.38311 (4)0.11560 (3)0.68223 (3)0.00319 (5)
Mo30.17729 (4)0.12651 (3)0.38673 (3)0.00322 (5)
Mo40.81176 (4)0.13391 (3)0.30011 (3)0.00319 (5)
Mo50.00045 (4)0.12368 (3)0.58644 (3)0.00299 (5)
O10.3994 (4)0.0079 (3)0.8417 (3)0.0044 (4)
O20.0073 (4)0.2212 (3)0.9361 (3)0.0044 (4)
O30.0133 (4)0.0007 (3)0.2366 (3)0.0049 (4)
O40.4009 (4)0.2532 (3)0.0205 (3)0.0047 (4)
O50.8011 (4)0.2458 (3)0.1175 (3)0.0056 (4)
O60.2055 (4)0.2469 (3)0.2170 (3)0.0054 (4)
O70.6066 (4)0.2339 (3)0.8309 (3)0.0051 (4)
O80.3842 (4)0.0014 (3)0.3326 (3)0.0055 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca0.0099 (3)0.0114 (3)0.0104 (3)0.0003 (3)0.0021 (2)0.0009 (3)
Mo10.00338 (10)0.00300 (11)0.00351 (10)0.00028 (8)0.00116 (8)0.00004 (8)
Mo20.00314 (10)0.00313 (11)0.00320 (10)0.00024 (8)0.00094 (8)0.00026 (8)
Mo30.00326 (10)0.00292 (11)0.00367 (10)0.00013 (9)0.00145 (8)0.00013 (8)
Mo40.00375 (11)0.00313 (11)0.00276 (10)0.00015 (8)0.00123 (8)0.00013 (8)
Mo50.00334 (10)0.00263 (10)0.00282 (10)0.00018 (9)0.00085 (8)0.00018 (8)
O10.0044 (9)0.0048 (10)0.0022 (9)0.0017 (8)0.0010 (7)0.0002 (8)
O20.0045 (10)0.0060 (10)0.0020 (9)0.0011 (8)0.0002 (8)0.0014 (7)
O30.0065 (10)0.0038 (10)0.0060 (10)0.0007 (8)0.0041 (8)0.0016 (8)
O40.0033 (10)0.0047 (10)0.0061 (10)0.0005 (7)0.0015 (8)0.0014 (8)
O50.0053 (11)0.0058 (11)0.0059 (10)0.0006 (8)0.0023 (9)0.0020 (8)
O60.0057 (11)0.0063 (10)0.0041 (10)0.0002 (8)0.0018 (8)0.0015 (8)
O70.0047 (10)0.0057 (10)0.0039 (10)0.0023 (8)0.0002 (8)0.0005 (8)
O80.0067 (10)0.0046 (10)0.0069 (10)0.0010 (8)0.0044 (8)0.0008 (8)
Geometric parameters (Å, º) top
Ca—O1i2.394 (3)Mo4—O52.064 (3)
Ca—O1ii2.421 (3)Mo4—O1ix2.074 (3)
Ca—O4iii2.481 (3)Mo4—O2xv2.091 (3)
Ca—O7ii2.592 (3)Mo4—Mo3x2.5943 (19)
Ca—O5iv2.647 (3)Mo4—Mo5x2.7229 (16)
Ca—O3v2.662 (3)Mo4—Mo2ix2.7373 (12)
Ca—O2i2.689 (3)Mo4—Mo12.7587 (14)
Ca—O8iii2.874 (3)Mo4—Mo5ix2.7653 (13)
Ca—O2vi3.018 (3)Mo4—Caxvi3.3556 (18)
Ca—O6iii3.035 (3)Mo5—O5xvii2.021 (3)
Ca—Mo4iv3.3556 (18)Mo5—O6vii2.022 (3)
Ca—Mo2ii3.378 (2)Mo5—O3xiv2.063 (3)
Mo1—O5vii2.028 (3)Mo5—O2viii2.071 (3)
Mo1—O7viii2.041 (3)Mo5—Mo3xiv2.6957 (12)
Mo1—O8ix2.106 (3)Mo5—Mo22.715 (2)
Mo1—O4vii2.111 (3)Mo5—Mo4xiii2.7229 (16)
Mo1—O82.122 (3)Mo5—Mo32.7541 (13)
Mo1—Mo2ix2.6830 (11)Mo5—Mo4ix2.7653 (13)
Mo1—Mo42.7587 (14)Mo5—Mo1xiii2.765 (2)
Mo1—Mo3ix2.7625 (13)Mo5—Mo5xiv2.8288 (12)
Mo1—Mo5x2.765 (2)O1—Mo4ix2.074 (3)
Mo1—Mo1ix2.7669 (13)O1—Caiii2.394 (3)
Mo1—Mo23.0343 (15)O1—Caxi2.421 (3)
Mo1—Mo33.078 (2)O2—Mo3vii2.057 (3)
Mo2—O11.915 (3)O2—Mo5vii2.071 (3)
Mo2—O6vii1.948 (3)O2—Mo4xvii2.091 (3)
Mo2—O4vii2.047 (3)O2—Caiii2.689 (3)
Mo2—O8ix2.100 (3)O2—Caxviii3.018 (3)
Mo2—O72.117 (3)O3—Mo4xiii2.052 (3)
Mo2—Mo1ix2.6830 (11)O3—Mo5xiv2.063 (3)
Mo2—Mo52.715 (2)O3—Caxix2.662 (3)
Mo2—Mo4ix2.7373 (12)O4—Mo2viii2.047 (3)
Mo2—Mo32.8250 (17)O4—Mo3viii2.068 (3)
Mo2—Caxi3.378 (2)O4—Mo1viii2.111 (3)
Mo2—Caxii3.753 (2)O4—Cai2.481 (3)
Mo3—O32.042 (3)O5—Mo5xv2.021 (3)
Mo3—O2viii2.057 (3)O5—Mo1viii2.028 (3)
Mo3—O4vii2.068 (3)O5—Caxvi2.647 (3)
Mo3—O62.087 (3)O6—Mo2viii1.948 (3)
Mo3—O82.145 (3)O6—Mo5viii2.022 (3)
Mo3—Mo4xiii2.5943 (19)O6—Cai3.035 (3)
Mo3—Mo5xiv2.6957 (12)O7—Mo1vii2.041 (3)
Mo3—Mo52.7541 (13)O7—Mo4vii2.063 (3)
Mo3—Mo1ix2.7625 (13)O7—Caxi2.592 (3)
Mo3—Mo22.8250 (17)O8—Mo2ix2.100 (3)
Mo3—Caxii3.592 (2)O8—Mo1ix2.106 (3)
Mo4—O3x2.052 (3)O8—Cai2.874 (3)
Mo4—O7viii2.063 (3)
O5vii—Mo1—O7viii84.42 (12)Mo4xiii—Mo3—Mo561.12 (4)
O5vii—Mo1—O8ix86.71 (12)Mo5xiv—Mo3—Mo562.53 (2)
O7viii—Mo1—O8ix168.26 (11)Mo4xiii—Mo3—Mo1ix123.78 (3)
O5vii—Mo1—O4vii86.62 (12)Mo5xiv—Mo3—Mo1ix60.87 (4)
O7viii—Mo1—O4vii86.15 (11)Mo5—Mo3—Mo1ix90.07 (3)
O8ix—Mo1—O4vii85.66 (11)Mo4xiii—Mo3—Mo2119.34 (4)
O5vii—Mo1—O8170.73 (11)Mo5xiv—Mo3—Mo288.91 (3)
O7viii—Mo1—O889.56 (11)Mo5—Mo3—Mo258.22 (4)
O8ix—Mo1—O898.24 (11)Mo1ix—Mo3—Mo257.38 (2)
O4vii—Mo1—O885.95 (11)Mo4xiii—Mo3—Mo1178.903 (15)
Mo2ix—Mo1—Mo460.38 (3)Mo5xiv—Mo3—Mo1116.94 (3)
Mo2ix—Mo1—Mo3ix62.48 (4)Mo5—Mo3—Mo1119.90 (4)
Mo4—Mo1—Mo3ix89.77 (3)Mo1ix—Mo3—Mo156.24 (3)
Mo2ix—Mo1—Mo5x90.43 (3)Mo2—Mo3—Mo161.68 (4)
Mo4—Mo1—Mo5x59.06 (4)O3x—Mo4—O7viii170.84 (10)
Mo3ix—Mo1—Mo5x58.37 (3)O3x—Mo4—O581.59 (11)
Mo2ix—Mo1—Mo1ix67.64 (4)O7viii—Mo4—O592.42 (11)
Mo4—Mo1—Mo1ix127.97 (3)O3x—Mo4—O1ix83.50 (11)
Mo3ix—Mo1—Mo1ix67.66 (5)O7viii—Mo4—O1ix88.92 (12)
Mo5x—Mo1—Mo1ix125.83 (3)O5—Mo4—O1ix83.13 (11)
Mo2ix—Mo1—Mo2122.51 (2)O3x—Mo4—O2xv100.88 (11)
Mo4—Mo1—Mo2176.412 (15)O7viii—Mo4—O2xv86.39 (12)
Mo3ix—Mo1—Mo293.55 (3)O5—Mo4—O2xv93.97 (11)
Mo5x—Mo1—Mo2121.82 (4)O1ix—Mo4—O2xv174.38 (10)
Mo1ix—Mo1—Mo254.86 (3)Mo3x—Mo4—Mo5x62.34 (4)
Mo2ix—Mo1—Mo394.17 (3)Mo3x—Mo4—Mo2ix119.40 (3)
Mo4—Mo1—Mo3123.82 (4)Mo5x—Mo4—Mo2ix90.19 (3)
Mo3ix—Mo1—Mo3123.76 (3)Mo3x—Mo4—Mo1122.83 (4)
Mo5x—Mo1—Mo3175.386 (15)Mo5x—Mo4—Mo160.59 (4)
Mo1ix—Mo1—Mo356.10 (3)Mo2ix—Mo4—Mo158.44 (2)
Mo2—Mo1—Mo355.05 (4)Mo3x—Mo4—Mo5ix60.29 (2)
O1—Mo2—O6vii94.47 (12)Mo5x—Mo4—Mo5ix62.05 (2)
O1—Mo2—O4vii173.00 (11)Mo2ix—Mo4—Mo5ix59.12 (4)
O6vii—Mo2—O4vii90.23 (12)Mo1—Mo4—Mo5ix89.92 (3)
O1—Mo2—O8ix86.93 (12)O5xvii—Mo5—O6vii90.40 (12)
O6vii—Mo2—O8ix168.42 (11)O5xvii—Mo5—O3xiv90.21 (11)
O4vii—Mo2—O8ix87.43 (12)O6vii—Mo5—O3xiv87.77 (11)
O1—Mo2—O784.56 (11)O5xvii—Mo5—O2viii85.33 (11)
O6vii—Mo2—O789.00 (12)O6vii—Mo5—O2viii82.47 (11)
O4vii—Mo2—O790.35 (11)O3xiv—Mo5—O2viii169.22 (11)
O8ix—Mo2—O779.68 (12)Mo3xiv—Mo5—Mo2116.62 (3)
Mo1ix—Mo2—Mo592.62 (3)Mo3xiv—Mo5—Mo4xiii91.95 (3)
Mo1ix—Mo2—Mo4ix61.18 (4)Mo2—Mo5—Mo4xiii118.74 (4)
Mo5—Mo2—Mo4ix60.95 (3)Mo3xiv—Mo5—Mo3117.47 (2)
Mo1ix—Mo2—Mo360.14 (3)Mo2—Mo5—Mo362.20 (4)
Mo5—Mo2—Mo359.58 (4)Mo4xiii—Mo5—Mo356.54 (4)
Mo4ix—Mo2—Mo388.91 (3)Mo3xiv—Mo5—Mo4ix56.71 (4)
Mo1ix—Mo2—Mo157.49 (2)Mo2—Mo5—Mo4ix59.92 (2)
Mo5—Mo2—Mo1122.85 (4)Mo4xiii—Mo5—Mo4ix117.95 (2)
Mo4ix—Mo2—Mo1118.63 (3)Mo3—Mo5—Mo4ix89.81 (3)
Mo3—Mo2—Mo163.27 (5)Mo3xiv—Mo5—Mo1xiii60.76 (2)
O3—Mo3—O2viii102.40 (11)Mo2—Mo5—Mo1xiii176.756 (15)
O3—Mo3—O4vii170.32 (11)Mo4xiii—Mo5—Mo1xiii60.35 (4)
O2viii—Mo3—O4vii85.95 (12)Mo3—Mo5—Mo1xiii116.80 (4)
O3—Mo3—O686.68 (11)Mo4ix—Mo5—Mo1xiii117.39 (3)
O2viii—Mo3—O695.11 (11)Mo3xiv—Mo5—Mo5xiv59.75 (4)
O4vii—Mo3—O687.71 (11)Mo2—Mo5—Mo5xiv88.45 (3)
O3—Mo3—O884.66 (11)Mo4xiii—Mo5—Mo5xiv59.71 (3)
O2viii—Mo3—O8169.69 (11)Mo3—Mo5—Mo5xiv57.72 (2)
O4vii—Mo3—O886.43 (11)Mo4ix—Mo5—Mo5xiv58.24 (4)
O6—Mo3—O877.65 (11)Mo1xiii—Mo5—Mo5xiv88.48 (3)
Mo4xiii—Mo3—Mo5xiv63.00 (3)
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x+1, y+1/2, z+3/2; (iii) x, y+1/2, z+1/2; (iv) x+1, y+1/2, z+1/2; (v) x, y+1/2, z+1/2; (vi) x, y+1/2, z+3/2; (vii) x, y1/2, z+1/2; (viii) x, y1/2, z1/2; (ix) x+1, y, z+1; (x) x+1, y, z; (xi) x+1, y1/2, z+3/2; (xii) x, y1, z; (xiii) x1, y, z; (xiv) x, y, z+1; (xv) x+1, y1/2, z1/2; (xvi) x+1, y1/2, z+1/2; (xvii) x1, y1/2, z+1/2; (xviii) x, y1/2, z+3/2; (xix) x, y1/2, z+1/2.
 

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