Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805024608/wm6073sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805024608/wm6073Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (O-B) = 0.011 Å
- Disorder in main residue
- R factor = 0.032
- wR factor = 0.079
- Data-to-parameter ratio = 13.0
checkCIF/PLATON results
No syntax errors found
Alert level C ABSMU01_ALERT_1_C The ratio of given/expected absorption coefficient lies outside the range 0.99 <> 1.01 Calculated value of mu = 11.211 Value of mu given = 11.328 DENSD01_ALERT_1_C The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.99 <> 1.01 Crystal density given = 4.686 Calculated crystal density = 4.821 PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio PLAT046_ALERT_1_C Reported Z, MW and D(calc) are Inconsistent .... 4.82 PLAT051_ALERT_1_C Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 1.04 Perc. PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT213_ALERT_2_C Atom O1 has ADP max/min Ratio ............. 3.30 prolat PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.41 PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc. PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. ZN2 -O2 -CD2 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. ZN2 -O2 -CD2 1.655 1.555 1.655 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. ZN1 -O2 -CD1 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. ZN1 -O3 -CD1 4.566 1.555 4.566 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. CD2 -O5 -ZN2 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 0.00 Deg. ZN2 -O5 -CD2 3.545 1.555 3.545
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 30.00 From the CIF: _reflns_number_total 1101 Count of symmetry unique reflns 721 Completeness (_total/calc) 152.70% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 380 Fraction of Friedel pairs measured 0.527 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 19 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.
Cd1.17Zn0.83B2O5 | F(000) = 512 |
Mr = 287.46 | Dx = 4.686 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 3098 reflections |
a = 3.4147 (4) Å | θ = 2.3–30.0° |
b = 6.5060 (7) Å | µ = 11.33 mm−1 |
c = 17.8263 (19) Å | T = 296 K |
V = 396.03 (8) Å3 | Needle, colorless |
Z = 4 | 0.22 × 0.10 × 0.10 mm |
Bruker SMART-APEX CCD diffractometer | 1101 independent reflections |
Radiation source: fine-focus sealed tube | 1100 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
ω scans | θmax = 30.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Bruker, 1997) | h = −4→4 |
Tmin = 0.090, Tmax = 0.322 | k = −5→9 |
2308 measured reflections | l = −23→24 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0118P)2 + 10.0237P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.032 | (Δ/σ)max = 0.001 |
wR(F2) = 0.079 | Δρmax = 2.83 e Å−3 |
S = 1.04 | Δρmin = −2.07 e Å−3 |
1101 reflections | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
85 parameters | Extinction coefficient: 0.040 (2) |
6 restraints | Absolute structure: Flack (1983), 380 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.13 (5) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cd1 | 0.61907 (16) | 0.47932 (8) | 0.47388 (3) | 0.0082 (2) | 0.924 (12) |
Zn1 | 0.61907 (16) | 0.47932 (8) | 0.47388 (3) | 0.0082 (2) | 0.076 (12) |
Cd2 | 0.0242 (2) | 0.60028 (12) | 0.29166 (4) | 0.0103 (3) | 0.247 (10) |
Zn2 | 0.0242 (2) | 0.60028 (12) | 0.29166 (4) | 0.0103 (3) | 0.753 (10) |
O1 | 0.2962 (18) | 0.0000 (9) | 0.3426 (3) | 0.0137 (13) | |
O2 | 0.521 (2) | 0.6623 (9) | 0.3564 (3) | 0.0151 (13) | |
O3 | 0.6091 (19) | 0.8913 (9) | 0.4581 (3) | 0.0135 (12) | |
O4 | 0.135 (2) | 0.2791 (9) | 0.4279 (3) | 0.0106 (12) | |
O5 | 0.018 (2) | 0.2935 (10) | 0.2950 (3) | 0.0180 (14) | |
B1 | 0.151 (3) | 0.1963 (13) | 0.3576 (5) | 0.0095 (16) | |
B2 | 0.486 (3) | 0.8572 (13) | 0.3875 (5) | 0.0082 (15) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0108 (3) | 0.0108 (3) | 0.0030 (2) | 0.00026 (18) | −0.00016 (17) | −0.00007 (18) |
Zn1 | 0.0108 (3) | 0.0108 (3) | 0.0030 (2) | 0.00026 (18) | −0.00016 (17) | −0.00007 (18) |
Cd2 | 0.0186 (5) | 0.0074 (4) | 0.0050 (4) | 0.0010 (3) | −0.0005 (3) | 0.0021 (3) |
Zn2 | 0.0186 (5) | 0.0074 (4) | 0.0050 (4) | 0.0010 (3) | −0.0005 (3) | 0.0021 (3) |
O1 | 0.025 (3) | 0.011 (2) | 0.005 (2) | 0.005 (2) | −0.0045 (19) | −0.0044 (19) |
O2 | 0.028 (3) | 0.006 (2) | 0.011 (3) | 0.000 (2) | 0.003 (2) | −0.002 (2) |
O3 | 0.018 (3) | 0.015 (3) | 0.007 (2) | 0.000 (2) | −0.003 (2) | 0.000 (2) |
O4 | 0.017 (3) | 0.009 (2) | 0.005 (2) | 0.000 (2) | 0.001 (2) | −0.0004 (18) |
O5 | 0.026 (3) | 0.019 (3) | 0.009 (3) | 0.006 (2) | −0.003 (3) | 0.007 (2) |
B1 | 0.015 (4) | 0.008 (3) | 0.005 (3) | −0.001 (3) | 0.000 (3) | 0.000 (3) |
B2 | 0.012 (3) | 0.009 (3) | 0.003 (3) | 0.001 (3) | 0.000 (3) | 0.003 (3) |
Cd1—O3i | 2.231 (6) | Zn2—O2 | 2.092 (7) |
Cd1—O4 | 2.260 (6) | Zn2—O2v | 2.108 (7) |
Cd1—O3ii | 2.283 (6) | Zn2—O1vi | 2.712 (5) |
Cd1—O4iii | 2.339 (6) | Zn2—O1vii | 2.907 (6) |
Cd1—O4iv | 2.428 (6) | O1—B2viii | 1.387 (10) |
Cd1—O2 | 2.432 (6) | O1—B1 | 1.396 (10) |
Cd1—O3 | 2.695 (6) | O2—B2 | 1.389 (10) |
Cd1—Cd1v | 3.4147 (4) | O2—Zn2iii | 2.108 (7) |
Cd1—Cd1iii | 3.4147 (4) | O2—Cd2iii | 2.108 (7) |
Zn1—O3i | 2.231 (6) | O3—B2 | 1.346 (10) |
Zn1—O4 | 2.260 (6) | O3—Zn1ii | 2.231 (6) |
Zn1—O3ii | 2.283 (6) | O3—Cd1ii | 2.231 (6) |
Zn1—O4iii | 2.339 (6) | O3—Zn1i | 2.283 (6) |
Zn1—O4iv | 2.428 (6) | O3—Cd1i | 2.283 (6) |
Zn1—O2 | 2.432 (6) | O4—B1 | 1.365 (10) |
Cd2—O5 | 1.997 (7) | O4—Zn1v | 2.339 (6) |
Cd2—O5vi | 1.997 (7) | O4—Cd1v | 2.339 (6) |
Cd2—O2 | 2.092 (7) | O4—Zn1ix | 2.428 (6) |
Cd2—O2v | 2.108 (7) | O4—Cd1ix | 2.428 (6) |
Cd2—B1vi | 2.797 (8) | O5—B1 | 1.360 (10) |
Cd2—Cd2iii | 3.4147 (4) | O5—Zn2x | 1.997 (7) |
Cd2—Cd2v | 3.4147 (4) | O5—Cd2x | 1.997 (7) |
Zn2—O5 | 1.997 (7) | B1—Cd2x | 2.797 (8) |
Zn2—O5vi | 1.997 (7) | B2—O1vii | 1.387 (10) |
O3i—Cd1—O4 | 164.5 (2) | B2—O2—Cd2iii | 117.6 (6) |
O3i—Cd1—O3ii | 98.3 (2) | Zn2—O2—Cd2iii | 108.8 (3) |
O4—Cd1—O3ii | 81.2 (2) | Cd2—O2—Cd2iii | 108.8 (3) |
O3i—Cd1—O4iii | 80.6 (2) | Zn2iii—O2—Cd2iii | 0.00 (6) |
O4—Cd1—O4iii | 95.9 (2) | B2—O2—Zn1 | 96.6 (4) |
O3ii—Cd1—O4iii | 165.0 (2) | Zn2—O2—Zn1 | 119.5 (3) |
O3i—Cd1—O4iv | 81.5 (2) | Cd2—O2—Zn1 | 119.5 (3) |
O4—Cd1—O4iv | 83.0 (2) | Zn2iii—O2—Zn1 | 105.4 (3) |
O3ii—Cd1—O4iv | 83.6 (2) | Cd2iii—O2—Zn1 | 105.4 (3) |
O4iii—Cd1—O4iv | 81.4 (2) | B2—O2—Cd1 | 96.6 (4) |
O3i—Cd1—O2 | 112.7 (2) | Zn2—O2—Cd1 | 119.5 (3) |
O4—Cd1—O2 | 82.5 (2) | Cd2—O2—Cd1 | 119.5 (3) |
O3ii—Cd1—O2 | 99.9 (2) | Zn2iii—O2—Cd1 | 105.4 (3) |
O4iii—Cd1—O2 | 94.2 (2) | Cd2iii—O2—Cd1 | 105.4 (3) |
O4iv—Cd1—O2 | 164.4 (2) | Zn1—O2—Cd1 | 0.00 (2) |
O3i—Cd1—O3 | 72.00 (18) | B2—O3—Zn1ii | 109.7 (5) |
O4—Cd1—O3 | 121.8 (2) | B2—O3—Cd1ii | 109.7 (5) |
O3ii—Cd1—O3 | 71.28 (19) | B2—O3—Zn1i | 142.7 (6) |
O4iii—Cd1—O3 | 121.8 (2) | Zn1ii—O3—Zn1i | 98.3 (2) |
O4iv—Cd1—O3 | 139.81 (17) | Cd1ii—O3—Zn1i | 98.3 (2) |
O2—Cd1—O3 | 54.67 (18) | B2—O3—Cd1i | 142.7 (6) |
O3i—Zn1—O4 | 164.5 (2) | Zn1ii—O3—Cd1i | 98.3 (2) |
O3i—Zn1—O3ii | 98.3 (2) | Cd1ii—O3—Cd1i | 98.3 (2) |
O4—Zn1—O3ii | 81.2 (2) | Zn1i—O3—Cd1i | 0.00 (2) |
O3i—Zn1—O4iii | 80.6 (2) | B2—O3—Cd1 | 86.4 (4) |
O4—Zn1—O4iii | 95.9 (2) | Zn1ii—O3—Cd1 | 109.2 (2) |
O3ii—Zn1—O4iii | 165.0 (2) | Cd1ii—O3—Cd1 | 109.2 (2) |
O3i—Zn1—O4iv | 81.5 (2) | Zn1i—O3—Cd1 | 107.6 (2) |
O4—Zn1—O4iv | 83.0 (2) | Cd1i—O3—Cd1 | 107.6 (2) |
O3ii—Zn1—O4iv | 83.6 (2) | B1—O4—Cd1 | 122.0 (6) |
O4iii—Zn1—O4iv | 81.4 (2) | B1—O4—Zn1 | 122.0 (6) |
O3i—Zn1—O2 | 112.7 (2) | B1—O4—Zn1v | 125.0 (6) |
O4—Zn1—O2 | 82.5 (2) | Cd1—O4—Zn1v | 95.9 (2) |
O3ii—Zn1—O2 | 99.9 (2) | Zn1—O4—Zn1v | 95.9 (2) |
O4iii—Zn1—O2 | 94.2 (2) | B1—O4—Cd1v | 125.0 (6) |
O4iv—Zn1—O2 | 164.4 (2) | Cd1—O4—Cd1v | 95.9 (2) |
O5—Cd2—O5vi | 130.67 (18) | Zn1—O4—Cd1v | 95.9 (2) |
O5—Cd2—O2 | 100.7 (3) | B1—O4—Zn1ix | 113.0 (5) |
O5vi—Cd2—O2 | 111.3 (3) | Cd1—O4—Zn1ix | 98.8 (2) |
O5—Cd2—O2v | 99.6 (3) | Zn1—O4—Zn1ix | 98.8 (2) |
O5vi—Cd2—O2v | 104.1 (3) | Zn1v—O4—Zn1ix | 96.7 (2) |
O2—Cd2—O2v | 108.8 (3) | Cd1v—O4—Zn1ix | 96.7 (2) |
O5—Zn2—O5vi | 130.67 (18) | B1—O4—Cd1ix | 113.0 (5) |
O5—Zn2—O2 | 100.7 (3) | Cd1—O4—Cd1ix | 98.8 (2) |
O5vi—Zn2—O2 | 111.3 (3) | Zn1—O4—Cd1ix | 98.8 (2) |
O5—Zn2—O2v | 99.6 (3) | Zn1v—O4—Cd1ix | 96.7 (2) |
O5vi—Zn2—O2v | 104.1 (3) | Cd1v—O4—Cd1ix | 96.7 (2) |
O2—Zn2—O2v | 108.8 (3) | B1—O5—Cd2 | 119.1 (5) |
O5—Zn2—O1vi | 77.4 (2) | B1—O5—Zn2 | 119.1 (5) |
O5vi—Zn2—O1vi | 55.9 (2) | Cd2—O5—Zn2 | 0.00 (4) |
O2—Zn2—O1vi | 149.4 (2) | B1—O5—Zn2x | 111.4 (5) |
O2v—Zn2—O1vi | 101.6 (2) | Cd2—O5—Zn2x | 127.4 (3) |
O5—Zn2—O1vii | 152.6 (2) | Zn2—O5—Zn2x | 127.4 (3) |
O5vi—Zn2—O1vii | 72.6 (2) | B1—O5—Cd2x | 111.4 (5) |
O2—Zn2—O1vii | 52.82 (19) | Cd2—O5—Cd2x | 127.4 (3) |
O2v—Zn2—O1vii | 85.3 (2) | Zn2—O5—Cd2x | 127.4 (3) |
O1vi—Zn2—O1vii | 128.32 (19) | Zn2x—O5—Cd2x | 0.00 (7) |
B2viii—O1—B1 | 132.0 (6) | O5—B1—O4 | 123.7 (8) |
B2—O2—Zn2 | 109.0 (6) | O5—B1—O1 | 112.8 (7) |
B2—O2—Cd2 | 109.0 (6) | O4—B1—O1 | 123.4 (7) |
Zn2—O2—Cd2 | 0.00 (5) | O3—B2—O1vii | 125.1 (7) |
B2—O2—Zn2iii | 117.6 (6) | O3—B2—O2 | 119.8 (7) |
Zn2—O2—Zn2iii | 108.8 (3) | O1vii—B2—O2 | 115.0 (7) |
Cd2—O2—Zn2iii | 108.8 (3) |
Symmetry codes: (i) x+1/2, −y+3/2, −z+1; (ii) x−1/2, −y+3/2, −z+1; (iii) x+1, y, z; (iv) x+1/2, −y+1/2, −z+1; (v) x−1, y, z; (vi) −x, y+1/2, −z+1/2; (vii) x, y+1, z; (viii) x, y−1, z; (ix) x−1/2, −y+1/2, −z+1; (x) −x, y−1/2, −z+1/2. |
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