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The structure of the title pentaborate, [Pb2(B5O9)Br] (dilead pentaborate bromide), known from powder data, has been refined based on single-crystal data (R = 0.034) and is discussed in terms of intercrossing anionic and cationic frameworks.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804023232/wm6030sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804023232/wm6030Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](O-B) = 0.019 Å
  • R factor = 0.034
  • wR factor = 0.080
  • Data-to-parameter ratio = 29.2

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT220_ALERT_2_A Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.67 Ratio
Author Response: low quality of U values due to the presence of Pb and Br, acentric space group, twinning, and pseudosymmetry...

Alert level G REFLT03_ALERT_4_G 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. From the CIF: _diffrn_reflns_theta_max 31.00 From the CIF: _reflns_number_total 2544 Count of symmetry unique reflns 1488 Completeness (_total/calc) 170.97% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1056 Fraction of Friedel pairs measured 0.710 Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Crystal Impact, 2000); software used to prepare material for publication: SHELXL97.

Dilead pentaborate bromide top
Crystal data top
[Pb2(B5O9)Br]F(000) = 1184
Mr = 692.34Dx = 5.341 Mg m3
Orthorhombic, Pnn2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2 -2nCell parameters from 4734 reflections
a = 11.4935 (19) Åθ = 3.5–36.0°
b = 11.4717 (19) ŵ = 43.73 mm1
c = 6.5297 (11) ÅT = 293 K
V = 860.9 (2) Å3Column, colourless
Z = 40.13 × 0.03 × 0.02 mm
Data collection top
Stoe IPDS-II
diffractometer
2544 independent reflections
Radiation source: fine-focus sealed tube2429 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.068
Detector resolution: 150 pixels mm-1θmax = 31.0°, θmin = 3.6°
ω scansh = 1216
Absorption correction: numerical
(XPREP in SHELXTL; Sheldrick, 1996).
k = 1616
Tmin = 0.093, Tmax = 0.387l = 89
7497 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0337P)2 + 13.5461P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.034(Δ/σ)max < 0.001
wR(F2) = 0.080Δρmax = 1.96 e Å3
S = 1.06Δρmin = 2.13 e Å3
2544 reflectionsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
87 parametersExtinction coefficient: 0.00036 (10)
1 restraintAbsolute structure: Flack (1983), 1059 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.03 (2)
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 as pseudomerohedral (110) twin, twin ratio 31.2 (2)%. 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
Pb10.25762 (6)0.04280 (6)0.00433 (9)0.01489 (12)
Pb20.02631 (6)0.23505 (5)0.66205 (14)0.01614 (13)
Br10.00000.00000.9081 (5)0.0289 (6)
Br20.00000.50000.6476 (6)0.0259 (5)
O10.2376 (8)0.3135 (8)0.5784 (14)0.0030 (16)*
O20.2084 (8)0.4248 (8)0.173 (2)0.0108 (16)*
O30.2717 (8)0.2256 (9)0.2448 (16)0.0079 (19)*
O40.0686 (11)0.2753 (11)0.2398 (19)0.017 (2)*
O50.2790 (9)0.4487 (11)0.835 (2)0.015 (2)*
O60.3827 (9)0.2616 (9)0.8357 (17)0.0092 (18)*
O70.1785 (8)0.2698 (9)0.9231 (15)0.0046 (16)*
O80.4168 (8)0.2110 (9)0.4921 (18)0.0090 (16)*
O90.2339 (9)0.1103 (10)0.5577 (16)0.0106 (19)*
B10.2706 (13)0.3217 (14)0.795 (2)0.008 (3)*
B20.1803 (13)0.3009 (14)0.146 (3)0.012 (3)*
B30.2864 (14)0.2180 (15)0.460 (2)0.010 (3)*
B40.4556 (13)0.2354 (16)0.683 (3)0.011 (3)*
B50.2513 (15)0.4950 (14)0.019 (3)0.009 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.0172 (2)0.0170 (2)0.0105 (2)0.0011 (2)0.0010 (2)0.0004 (3)
Pb20.0187 (2)0.0179 (2)0.0118 (3)0.0013 (2)0.0034 (3)0.0000 (3)
Br10.0202 (12)0.0154 (10)0.0511 (19)0.0011 (10)0.0000.000
Br20.0188 (11)0.0179 (10)0.0411 (16)0.0002 (8)0.0000.000
Geometric parameters (Å, º) top
Pb1—O5i2.497 (13)O1—Pb1viii2.686 (9)
Pb1—O2i2.534 (12)B2—O21.468 (19)
Pb1—O32.659 (11)B2—O31.504 (19)
Pb1—O1i2.686 (9)B2—O41.450 (19)
Pb1—O7ii2.798 (10)B2—O7ii1.50 (2)
Pb1—O9ii2.975 (11)O2—Pb1viii2.534 (12)
Pb1—Br2i2.9977 (16)B3—O11.453 (19)
Pb1—Br1ii3.0554 (10)B3—O31.417 (19)
Pb1—O6ii3.076 (11)B3—O81.516 (19)
Pb1—B5i3.160 (19)B3—O91.52 (2)
Pb2—O72.475 (10)B4—O4x1.358 (19)
Pb2—O8iii2.571 (11)B4—O61.34 (2)
Pb2—O12.647 (9)B4—O81.35 (2)
Pb2—O6iv2.695 (11)B5—O21.38 (2)
Pb2—O42.838 (13)B5—O5ii1.36 (2)
Pb2—O92.864 (11)B5—O9xi1.358 (19)
Pb2—O3iii3.010 (10)O3—Pb2xii3.010 (10)
Pb2—Br23.0559 (8)O4—B4iv1.358 (19)
Pb2—B13.104 (15)O5—B5vi1.36 (2)
Pb2—Br13.153 (2)O5—Pb1viii2.497 (13)
Br1—Pb1v3.0554 (10)O6—Pb2x2.695 (11)
Br1—Pb1vi3.0554 (10)O6—Pb1vi3.076 (11)
Br1—Pb2vii3.1532 (19)O7—B2vi1.50 (2)
Br2—Pb1viii2.9977 (16)O7—Pb1vi2.798 (10)
Br2—Pb1iii2.9977 (16)O8—Pb2xii2.571 (11)
Br2—Pb2ix3.0559 (8)O9—B5xiii1.358 (19)
B1—O11.470 (18)O9—Pb1vi2.975 (11)
B1—O51.48 (2)B1—Pb1viii3.220 (16)
B1—O61.485 (18)B4—Pb2x3.25 (2)
B1—O71.473 (18)B5—Pb1viii3.160 (19)
O5i—Pb1—O2i122.1 (4)B2—O3—Pb198.6 (9)
O5i—Pb1—O379.0 (4)B3—O3—Pb2xii94.1 (8)
O2i—Pb1—O3157.0 (3)B2—O3—Pb2xii121.1 (8)
O5i—Pb1—O1i53.3 (3)Pb1—O3—Pb2xii93.9 (3)
O2i—Pb1—O1i68.9 (3)B4iv—O4—B2138.5 (15)
O3—Pb1—O1i130.4 (3)B4iv—O4—Pb295.0 (11)
O5i—Pb1—O7ii119.8 (3)B2—O4—Pb2126.4 (10)
O2i—Pb1—O7ii114.0 (3)B5vi—O5—B1121.5 (13)
O3—Pb1—O7ii52.4 (3)B5vi—O5—Pb1viii125.4 (10)
O1i—Pb1—O7ii162.2 (3)B1—O5—Pb1viii105.2 (9)
O5i—Pb1—O9ii161.5 (3)B4—O6—B1121.0 (13)
O2i—Pb1—O9ii49.8 (3)B4—O6—Pb2x102.2 (9)
O3—Pb1—O9ii112.8 (3)B1—O6—Pb2x131.6 (9)
O1i—Pb1—O9ii116.8 (3)B4—O6—Pb1vi111.3 (10)
O7ii—Pb1—O9ii64.2 (3)B1—O6—Pb1vi91.9 (8)
O5i—Pb1—Br2i78.0 (3)Pb2x—O6—Pb1vi91.7 (3)
O2i—Pb1—Br2i92.5 (2)B1—O7—B2vi116.3 (11)
O3—Pb1—Br2i82.6 (2)B1—O7—Pb2100.6 (8)
O1i—Pb1—Br2i75.76 (19)B2vi—O7—Pb2135.8 (8)
O7ii—Pb1—Br2i120.7 (2)Pb1viii—Br2—Pb294.66 (3)
O9ii—Pb1—Br2i116.5 (2)Pb1iii—Br2—Pb286.52 (3)
O5i—Pb1—Br1ii86.2 (3)Pb1viii—Br2—Pb2ix86.52 (3)
O2i—Pb1—Br1ii84.7 (2)Pb1iii—Br2—Pb2ix94.66 (3)
O3—Pb1—Br1ii107.5 (2)Pb2—Br2—Pb2ix176.46 (16)
O1i—Pb1—Br1ii84.26 (19)B3—O1—B1117.5 (11)
O7ii—Pb1—Br1ii78.6 (2)B3—O1—Pb2102.0 (8)
O9ii—Pb1—Br1ii76.9 (2)B1—O1—Pb293.4 (7)
Br2i—Pb1—Br1ii159.43 (5)B3—O1—Pb1viii128.5 (8)
O5i—Pb1—O6ii137.1 (3)B1—O1—Pb1viii97.2 (8)
O2i—Pb1—O6ii94.7 (3)Pb2—O1—Pb1viii113.1 (3)
O3—Pb1—O6ii62.3 (3)B5—O2—B2123.9 (14)
O1i—Pb1—O6ii149.1 (3)B5—O2—Pb1viii103.8 (9)
O7ii—Pb1—O6ii48.3 (3)B2—O2—Pb1viii130.6 (11)
O9ii—Pb1—O6ii60.3 (3)B3—O3—B2122.8 (13)
Br2i—Pb1—O6ii79.1 (2)B3—O3—Pb1124.4 (10)
Br1ii—Pb1—O6ii121.4 (2)B2—O3—Pb198.6 (9)
O5i—Pb1—B5i142.3 (4)B3—O3—Pb2xii94.1 (8)
O2i—Pb1—B5i25.1 (4)B2—O3—Pb2xii121.1 (8)
O3—Pb1—B5i137.8 (4)Pb1—O3—Pb2xii93.9 (3)
O1i—Pb1—B5i91.6 (4)B4iv—O4—B2138.5 (15)
O7ii—Pb1—B5i89.1 (4)B4iv—O4—Pb295.0 (11)
O9ii—Pb1—B5i25.3 (4)B2—O4—Pb2126.4 (10)
Br2i—Pb1—B5i109.1 (3)B5vi—O5—B1121.5 (13)
Br1ii—Pb1—B5i75.9 (3)B5vi—O5—Pb1viii125.4 (10)
O6ii—Pb1—B5i79.8 (4)B1—O5—Pb1viii105.2 (9)
O7—Pb2—O8iii74.3 (3)B4—O6—B1121.0 (13)
O7—Pb2—O155.9 (3)B4—O6—Pb2x102.2 (9)
O8iii—Pb2—O1122.7 (3)B1—O6—Pb2x131.6 (9)
O7—Pb2—O6iv167.2 (3)B4—O6—Pb1vi111.3 (10)
O8iii—Pb2—O6iv111.1 (3)B1—O6—Pb1vi91.9 (8)
O1—Pb2—O6iv113.2 (3)Pb2x—O6—Pb1vi91.7 (3)
O7—Pb2—O4121.4 (3)B1—O7—B2vi116.3 (11)
O8iii—Pb2—O4149.2 (3)B1—O7—Pb2100.6 (8)
O1—Pb2—O465.6 (3)B2vi—O7—Pb2135.8 (8)
O6iv—Pb2—O448.3 (3)B1—O7—Pb1vi103.8 (8)
O7—Pb2—O969.8 (3)B2vi—O7—Pb1vi93.0 (7)
O8iii—Pb2—O9136.7 (3)Pb2—O7—Pb1vi101.3 (3)
O1—Pb2—O949.9 (3)B4—O8—B3116.3 (12)
O6iv—Pb2—O9109.2 (3)B4—O8—Pb2xii124.1 (9)
O4—Pb2—O973.0 (4)B3—O8—Pb2xii110.8 (8)
O7—Pb2—O3iii122.7 (3)B5xiii—O9—B3131.8 (13)
O8iii—Pb2—O3iii48.5 (3)B5xiii—O9—Pb2129.5 (10)
O1—Pb2—O3iii151.4 (3)B3—O9—Pb291.4 (8)
O6iv—Pb2—O3iii62.9 (3)B5xiii—O9—Pb1vi85.0 (9)
O4—Pb2—O3iii108.5 (3)B3—O9—Pb1vi125.5 (8)
O9—Pb2—O3iii158.0 (3)Pb2—O9—Pb1vi88.7 (3)
O7—Pb2—Br286.1 (2)O1—B1—O7109.5 (11)
O8iii—Pb2—Br274.8 (2)O1—B1—O5104.2 (12)
O1—Pb2—Br275.3 (2)O7—B1—O5110.3 (12)
O6iv—Pb2—Br284.3 (2)O1—B1—O6111.4 (12)
O4—Pb2—Br279.9 (3)O7—B1—O6109.6 (12)
O9—Pb2—Br2124.9 (2)O5—B1—O6111.7 (11)
O3iii—Pb2—Br276.1 (2)O1—B1—Pb258.3 (6)
O7—Pb2—B127.8 (4)O7—B1—Pb251.6 (6)
O8iii—Pb2—B197.5 (4)O5—B1—Pb2115.0 (9)
O1—Pb2—B128.2 (4)O6—B1—Pb2133.3 (9)
O6iv—Pb2—B1140.5 (4)O1—B1—Pb1viii55.9 (6)
O4—Pb2—B193.8 (4)O7—B1—Pb1viii126.2 (9)
O9—Pb2—B158.2 (4)O5—B1—Pb1viii48.5 (7)
O3iii—Pb2—B1141.4 (4)O6—B1—Pb1viii124.1 (9)
Br2—Pb2—B177.3 (3)Pb2—B1—Pb1viii89.4 (4)
O7—Pb2—Br181.6 (2)O4—B2—O2109.9 (13)
O8iii—Pb2—Br174.4 (2)O4—B2—O7ii110.4 (12)
O1—Pb2—Br1118.9 (2)O2—B2—O7ii110.4 (14)
O6iv—Pb2—Br1110.9 (2)O4—B2—O3108.8 (13)
O4—Pb2—Br1130.6 (3)O2—B2—O3110.5 (12)
O9—Pb2—Br176.9 (2)O7ii—B2—O3106.7 (12)
O3iii—Pb2—Br186.8 (2)O4—B2—Pb1100.7 (9)
Br2—Pb2—Br1148.95 (10)O2—B2—Pb1149.2 (10)
B1—Pb2—Br1102.6 (3)O7ii—B2—Pb159.5 (6)
Pb1v—Br1—Pb1vi158.42 (14)O3—B2—Pb154.2 (7)
Pb1v—Br1—Pb2109.01 (4)O3—B3—O1115.8 (13)
Pb1vi—Br1—Pb282.24 (3)O3—B3—O8105.0 (12)
Pb1v—Br1—Pb2vii82.24 (3)O1—B3—O8110.3 (12)
Pb1vi—Br1—Pb2vii109.01 (4)O3—B3—O9114.8 (13)
Pb2—Br1—Pb2vii118.74 (11)O1—B3—O9103.7 (11)
Pb1viii—Br2—Pb1iii141.35 (15)O8—B3—O9107.0 (11)
Pb1viii—Br2—Pb294.66 (3)O3—B3—Pb2106.7 (9)
Pb1iii—Br2—Pb286.52 (3)O1—B3—Pb252.3 (6)
Pb1viii—Br2—Pb2ix86.52 (3)O8—B3—Pb2148.2 (10)
Pb1iii—Br2—Pb2ix94.66 (3)O9—B3—Pb261.0 (7)
Pb2—Br2—Pb2ix176.46 (16)O6—B4—O8121.9 (13)
B3—O1—B1117.5 (11)O6—B4—O4x114.5 (17)
B3—O1—Pb2102.0 (8)O8—B4—O4x123.4 (16)
B1—O1—Pb293.4 (7)O6—B4—Pb2x54.1 (9)
B3—O1—Pb1viii128.5 (8)O8—B4—Pb2x172.2 (11)
B1—O1—Pb1viii97.2 (8)O4x—B4—Pb2x60.4 (10)
Pb2—O1—Pb1viii113.1 (3)O5ii—B5—O9xi121.1 (15)
B5—O2—B2123.9 (14)O5ii—B5—O2120.3 (14)
B5—O2—Pb1viii103.8 (9)O9xi—B5—O2118.7 (15)
B2—O2—Pb1viii130.6 (11)O5ii—B5—Pb1viii162.0 (11)
B3—O3—B2122.8 (13)O9xi—B5—Pb1viii69.7 (9)
B3—O3—Pb1124.4 (10)O2—B5—Pb1viii51.1 (8)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x, y, z+1; (iii) x1/2, y+1/2, z1/2; (iv) x1/2, y+1/2, z+1/2; (v) x, y, z1; (vi) x, y, z1; (vii) x, y, z; (viii) x+1/2, y+1/2, z1/2; (ix) x, y+1, z; (x) x+1/2, y+1/2, z1/2; (xi) x+1/2, y+1/2, z+1/2; (xii) x+1/2, y+1/2, z+1/2; (xiii) x+1/2, y1/2, z1/2.
 

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