Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806002170/bt6805sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806002170/bt6805Isup2.hkl |
CCDC reference: 298378
Key indicators
- Single-crystal synchrotron study
- T = 150 K
- Mean (C-C) = 0.005 Å
- Disorder in main residue
- R factor = 0.049
- wR factor = 0.118
- Data-to-parameter ratio = 24.2
checkCIF/PLATON results
No syntax errors found
Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.647 1.000 Tmin(prime) and Tmax expected: 0.979 0.989 RR(prime) = 0.654 Please check that your absorption correction is appropriate.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT128_ALERT_4_C Non-standard setting of Space group C2/c .... I2/a PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc.
Alert level G ABSMU_01 Radiation type not identified. Calculation of _exptl_absorpt_correction_mu not performed. CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G ALERT: check formula stoichiometry or atom site occupancies. From the CIF: _cell_formula_units_Z 8 From the CIF: _chemical_formula_sum C6 H24 Cd N8 O6 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 48.00 48.00 0.00 H 192.00 192.00 0.00 Cd 8.00 8.00 0.00 N 64.00 64.02 -0.02 O 48.00 48.07 -0.07
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion
checkCIF publication errors
Alert level A PUBL022_ALERT_1_A There is a mismatched ~ on line 128 The title compound, [Cd(C~2~H~8~N~2)~3~](NO~3~)~2~, crystallises with distorted If you require a ~ then it should be escaped with a \, i.e. \~ Otherwise there must be a matching closing ~, e.g. C~2~H~4~
1 ALERT level A = Data missing that is essential or data in wrong format 0 ALERT level G = General alerts. Data that may be required is missing
Data collection: APEXII (Bruker, 2004); cell refinement: APEXII; data reduction: APEXII; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: WinGX (Version 1.64; Farrugia, 1999); software used to prepare material for publication: SHELXL97.
[Cd(C2H8N2)3](NO3)2 | F(000) = 1696 |
Mr = 416.73 | Dx = 1.715 Mg m−3 |
Monoclinic, I2/a | Synchrotron radiation, λ = 0.67110 Å |
Hall symbol: -I 2ya | Cell parameters from 2733 reflections |
a = 15.2574 (12) Å | θ = 2.9–23.0° |
b = 11.0441 (8) Å | µ = 1.39 mm−1 |
c = 19.155 (2) Å | T = 150 K |
β = 90.246 (1)° | Block, colourless |
V = 3227.6 (5) Å3 | 0.02 × 0.01 × 0.01 mm |
Z = 8 |
Bruker D8 diffractometer | 5813 independent reflections |
Radiation source: Daresbury SRS, Station 9.8 | 4525 reflections with I > 2σ(I) |
Silicon 111 monochromator | Rint = 0.076 |
ω rotation with narrow frame scans | θmax = 31.1°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | h = −22→23 |
Tmin = 0.647, Tmax = 1.00 | k = −16→16 |
20814 measured reflections | l = −29→28 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.118 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0288P)2 + 0.6151P] where P = (Fo2 + 2Fc2)/3 |
5813 reflections | (Δ/σ)max = 0.001 |
240 parameters | Δρmax = 1.03 e Å−3 |
27 restraints | Δρmin = −0.69 e Å−3 |
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 | 0.442462 (15) | 0.23521 (2) | 0.129797 (11) | 0.02619 (8) | |
N1 | 0.5590 (2) | 0.3111 (3) | 0.06172 (18) | 0.0370 (7) | |
N2 | 0.5730 (2) | 0.1975 (3) | 0.19676 (17) | 0.0349 (6) | |
N3 | 0.3995 (2) | 0.4060 (3) | 0.19550 (14) | 0.0304 (6) | |
N4 | 0.33449 (18) | 0.3296 (2) | 0.06123 (14) | 0.0267 (5) | |
N5 | 0.3585 (2) | 0.1068 (3) | 0.20132 (15) | 0.0311 (6) | |
N6 | 0.4291 (2) | 0.0502 (3) | 0.06669 (15) | 0.0337 (6) | |
C2 | 0.6452 (3) | 0.2678 (3) | 0.1657 (2) | 0.0437 (10) | |
H2A | 0.7009 | 0.2366 | 0.1825 | 0.052* | |
H2B | 0.6406 | 0.3518 | 0.1800 | 0.052* | |
C1 | 0.6422 (3) | 0.2600 (3) | 0.0876 (2) | 0.0420 (9) | |
H1A | 0.6910 | 0.3045 | 0.0680 | 0.050* | |
H1B | 0.6471 | 0.1761 | 0.0732 | 0.050* | |
C3 | 0.3177 (2) | 0.4542 (3) | 0.16578 (17) | 0.0342 (7) | |
H3A | 0.3087 | 0.5363 | 0.1823 | 0.041* | |
H3B | 0.2687 | 0.4053 | 0.1813 | 0.041* | |
C4 | 0.3208 (2) | 0.4540 (3) | 0.08681 (17) | 0.0317 (7) | |
H4A | 0.2662 | 0.4857 | 0.0682 | 0.038* | |
H4B | 0.3682 | 0.5056 | 0.0710 | 0.038* | |
C5 | 0.3646 (2) | −0.0180 (3) | 0.17641 (19) | 0.0384 (8) | |
H5A | 0.3175 | −0.0656 | 0.1963 | 0.046* | |
H5B | 0.4198 | −0.0529 | 0.1915 | 0.046* | |
C6 | 0.3586 (2) | −0.0220 (3) | 0.09748 (19) | 0.0384 (8) | |
H6A | 0.3631 | −0.1052 | 0.0816 | 0.046* | |
H6B | 0.3023 | 0.0095 | 0.0824 | 0.046* | |
N20 | 0.0311 (5) | 0.3791 (7) | 0.1174 (3) | 0.0309 (9)* | 0.477 (8) |
O20 | −0.0252 (4) | 0.2931 (6) | 0.1166 (5) | 0.0418 (7)* | 0.477 (8) |
O21 | 0.0435 (5) | 0.4291 (8) | 0.1724 (4) | 0.0418 (7)* | 0.477 (8) |
O22 | 0.0550 (5) | 0.4171 (8) | 0.0609 (4) | 0.0418 (7)* | 0.477 (8) |
N20B | 0.0159 (5) | 0.3553 (6) | 0.1143 (3) | 0.0309 (9)* | 0.331 (6) |
O20B | −0.0219 (6) | 0.2656 (7) | 0.0867 (6) | 0.0418 (7)* | 0.331 (6) |
O21B | 0.0136 (6) | 0.3783 (9) | 0.1762 (4) | 0.0418 (7)* | 0.331 (6) |
O22B | 0.0724 (6) | 0.4106 (10) | 0.0732 (5) | 0.0418 (7)* | 0.331 (6) |
N20C | 0.0159 (5) | 0.3553 (6) | 0.1143 (3) | 0.0309 (9)* | 0.195 (7) |
O20C | −0.0367 (10) | 0.3012 (14) | 0.1498 (10) | 0.0418 (7)* | 0.195 (7) |
O21C | 0.0640 (11) | 0.4458 (16) | 0.1619 (9) | 0.0418 (7)* | 0.195 (7) |
O22C | 0.0388 (11) | 0.3729 (16) | 0.0589 (8) | 0.0418 (7)* | 0.195 (7) |
O10 | 0.17031 (18) | 0.1547 (2) | 0.05793 (12) | 0.0404 (6) | |
O11 | 0.17461 (16) | 0.1930 (2) | 0.16849 (12) | 0.0330 (5) | |
O12 | 0.09792 (18) | 0.0432 (2) | 0.12984 (14) | 0.0456 (7) | |
N10 | 0.14703 (17) | 0.1306 (2) | 0.11827 (13) | 0.0247 (5) | |
H2C | 0.564 (3) | 0.218 (4) | 0.2379 (12) | 0.042 (12)* | |
H1D | 0.557 (2) | 0.3877 (17) | 0.0653 (18) | 0.026 (9)* | |
H4D | 0.2885 (17) | 0.286 (3) | 0.062 (2) | 0.028 (10)* | |
H5C | 0.3063 (14) | 0.130 (3) | 0.200 (2) | 0.040 (11)* | |
H4C | 0.353 (2) | 0.329 (3) | 0.0198 (11) | 0.031 (10)* | |
H2D | 0.584 (2) | 0.1221 (18) | 0.1935 (19) | 0.037 (11)* | |
H1C | 0.548 (3) | 0.291 (4) | 0.0189 (12) | 0.054 (14)* | |
H6D | 0.420 (3) | 0.067 (4) | 0.0234 (11) | 0.048 (12)* | |
H6C | 0.4763 (17) | 0.011 (3) | 0.0670 (19) | 0.039 (11)* | |
H5D | 0.382 (3) | 0.116 (4) | 0.2401 (13) | 0.044 (12)* | |
H3C | 0.4376 (18) | 0.462 (2) | 0.1950 (18) | 0.027 (9)* | |
H3D | 0.398 (3) | 0.395 (4) | 0.2386 (10) | 0.055 (13)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.02701 (13) | 0.03150 (13) | 0.02006 (12) | 0.00162 (8) | 0.00162 (9) | 0.00239 (7) |
N1 | 0.0351 (16) | 0.0348 (16) | 0.0413 (18) | 0.0020 (13) | 0.0124 (14) | 0.0086 (14) |
N2 | 0.0404 (17) | 0.0319 (15) | 0.0323 (16) | 0.0044 (13) | −0.0076 (13) | −0.0013 (12) |
N3 | 0.0405 (16) | 0.0345 (15) | 0.0162 (12) | −0.0058 (12) | 0.0033 (11) | −0.0048 (10) |
N4 | 0.0278 (13) | 0.0306 (14) | 0.0217 (12) | 0.0023 (11) | −0.0022 (10) | −0.0015 (10) |
N5 | 0.0295 (15) | 0.0383 (15) | 0.0254 (14) | −0.0033 (12) | 0.0017 (12) | 0.0039 (11) |
N6 | 0.0396 (17) | 0.0371 (15) | 0.0244 (14) | 0.0153 (13) | −0.0035 (12) | −0.0055 (11) |
C2 | 0.0306 (19) | 0.040 (2) | 0.061 (3) | 0.0014 (15) | −0.0097 (18) | −0.0065 (17) |
C1 | 0.0331 (19) | 0.0345 (19) | 0.058 (3) | −0.0006 (14) | 0.0100 (18) | −0.0022 (16) |
C3 | 0.0379 (18) | 0.0331 (17) | 0.0318 (17) | 0.0048 (14) | 0.0050 (14) | −0.0084 (13) |
C4 | 0.0351 (17) | 0.0306 (16) | 0.0293 (16) | 0.0048 (13) | −0.0035 (13) | −0.0012 (12) |
C5 | 0.041 (2) | 0.0319 (17) | 0.042 (2) | −0.0007 (15) | −0.0039 (16) | 0.0075 (15) |
C6 | 0.044 (2) | 0.0280 (16) | 0.043 (2) | 0.0029 (14) | −0.0110 (16) | −0.0068 (14) |
O10 | 0.0489 (16) | 0.0518 (16) | 0.0205 (11) | −0.0044 (12) | 0.0014 (10) | 0.0049 (10) |
O11 | 0.0342 (13) | 0.0391 (13) | 0.0256 (11) | −0.0047 (10) | −0.0014 (9) | −0.0069 (10) |
O12 | 0.0501 (16) | 0.0372 (14) | 0.0495 (16) | −0.0209 (12) | −0.0042 (13) | 0.0067 (12) |
N10 | 0.0266 (13) | 0.0250 (12) | 0.0224 (12) | −0.0002 (10) | −0.0020 (10) | 0.0034 (9) |
Cd1—N1 | 2.364 (3) | C2—C1 | 1.499 (6) |
Cd1—N2 | 2.400 (3) | C2—H2A | 0.9700 |
Cd1—N3 | 2.362 (3) | C2—H2B | 0.9700 |
Cd1—N4 | 2.347 (3) | C1—H1A | 0.9700 |
Cd1—N5 | 2.355 (3) | C1—H1B | 0.9700 |
Cd1—N6 | 2.382 (3) | C3—C4 | 1.514 (5) |
N1—C1 | 1.473 (5) | C3—H3A | 0.9700 |
N1—H1D | 0.849 (18) | C3—H3B | 0.9700 |
N1—H1C | 0.863 (19) | C4—H4A | 0.9700 |
N2—C2 | 1.476 (5) | C4—H4B | 0.9700 |
N2—H2C | 0.832 (19) | C5—C6 | 1.515 (5) |
N2—H2D | 0.851 (18) | C5—H5A | 0.9700 |
N3—C3 | 1.469 (5) | C5—H5B | 0.9700 |
N3—H3C | 0.849 (18) | C6—H6A | 0.9700 |
N3—H3D | 0.835 (19) | C6—H6B | 0.9700 |
N4—C4 | 1.474 (4) | N20—O21 | 1.205 (8) |
N4—H4D | 0.851 (18) | N20—O22 | 1.217 (8) |
N4—H4C | 0.842 (18) | N20—O20 | 1.280 (8) |
N5—C5 | 1.461 (5) | N20B—O21B | 1.213 (8) |
N5—H5C | 0.836 (18) | N20B—O20B | 1.261 (9) |
N5—H5D | 0.831 (18) | N20B—O22B | 1.319 (10) |
N6—C6 | 1.466 (5) | O10—N10 | 1.240 (3) |
N6—H6D | 0.861 (18) | O11—N10 | 1.255 (3) |
N6—H6C | 0.839 (18) | O12—N10 | 1.243 (3) |
N4—Cd1—N5 | 102.16 (10) | C6—N6—H6C | 110 (3) |
N1—Cd1—N2 | 74.45 (12) | Cd1—N6—H6C | 112 (3) |
N3—Cd1—N4 | 75.38 (10) | H6D—N6—H6C | 105 (3) |
N5—Cd1—N6 | 74.52 (11) | N2—C2—C1 | 110.6 (3) |
N5—Cd1—N3 | 91.03 (10) | N2—C2—H2A | 109.5 |
N4—Cd1—N1 | 93.54 (11) | C1—C2—H2A | 109.5 |
N5—Cd1—N1 | 161.31 (11) | N2—C2—H2B | 109.5 |
N3—Cd1—N1 | 102.82 (11) | C1—C2—H2B | 109.5 |
N4—Cd1—N6 | 92.23 (10) | H2A—C2—H2B | 108.1 |
N3—Cd1—N6 | 158.76 (11) | N1—C1—C2 | 109.7 (3) |
N1—Cd1—N6 | 94.99 (12) | N1—C1—H1A | 109.7 |
N4—Cd1—N2 | 162.73 (11) | C2—C1—H1A | 109.7 |
N5—Cd1—N2 | 92.11 (11) | N1—C1—H1B | 109.7 |
N3—Cd1—N2 | 94.91 (11) | C2—C1—H1B | 109.7 |
N6—Cd1—N2 | 101.01 (10) | H1A—C1—H1B | 108.2 |
C1—N1—Cd1 | 109.1 (2) | N3—C3—C4 | 110.9 (3) |
C1—N1—H1D | 113 (2) | N3—C3—H3A | 109.5 |
Cd1—N1—H1D | 107 (2) | C4—C3—H3A | 109.5 |
C1—N1—H1C | 112 (3) | N3—C3—H3B | 109.5 |
Cd1—N1—H1C | 107 (3) | C4—C3—H3B | 109.5 |
H1D—N1—H1C | 109 (4) | H3A—C3—H3B | 108.0 |
C2—N2—Cd1 | 108.2 (2) | N4—C4—C3 | 109.8 (3) |
C2—N2—H2C | 111 (3) | N4—C4—H4A | 109.7 |
Cd1—N2—H2C | 109 (3) | C3—C4—H4A | 109.7 |
C2—N2—H2D | 110 (3) | N4—C4—H4B | 109.7 |
Cd1—N2—H2D | 107 (3) | C3—C4—H4B | 109.7 |
H2C—N2—H2D | 112 (4) | H4A—C4—H4B | 108.2 |
C3—N3—Cd1 | 108.67 (19) | N5—C5—C6 | 110.5 (3) |
C3—N3—H3C | 108 (2) | N5—C5—H5A | 109.6 |
Cd1—N3—H3C | 113 (2) | C6—C5—H5A | 109.6 |
C3—N3—H3D | 114 (3) | N5—C5—H5B | 109.6 |
Cd1—N3—H3D | 115 (3) | C6—C5—H5B | 109.6 |
H3C—N3—H3D | 98 (4) | H5A—C5—H5B | 108.1 |
C4—N4—Cd1 | 109.17 (19) | N6—C6—C5 | 110.1 (3) |
C4—N4—H4D | 114 (2) | N6—C6—H6A | 109.6 |
Cd1—N4—H4D | 109 (2) | C5—C6—H6A | 109.6 |
C4—N4—H4C | 112 (3) | N6—C6—H6B | 109.6 |
Cd1—N4—H4C | 107 (2) | C5—C6—H6B | 109.6 |
H4D—N4—H4C | 107 (3) | H6A—C6—H6B | 108.1 |
C5—N5—Cd1 | 110.0 (2) | O21—N20—O22 | 125.0 (7) |
C5—N5—H5C | 110 (3) | O21—N20—O20 | 116.9 (7) |
Cd1—N5—H5C | 109 (3) | O22—N20—O20 | 116.6 (7) |
C5—N5—H5D | 112 (3) | O21B—N20B—O20B | 124.0 (8) |
Cd1—N5—H5D | 102 (3) | O21B—N20B—O22B | 120.5 (8) |
H5C—N5—H5D | 114 (4) | O20B—N20B—O22B | 114.4 (8) |
C6—N6—Cd1 | 108.9 (2) | O10—N10—O12 | 120.6 (3) |
C6—N6—H6D | 113 (3) | O10—N10—O11 | 120.0 (3) |
Cd1—N6—H6D | 109 (3) | O12—N10—O11 | 119.4 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4D···O10 | 0.85 (2) | 2.31 (2) | 3.163 (4) | 175 (3) |
N5—H5C···O11 | 0.84 (2) | 2.21 (2) | 3.026 (4) | 166 (4) |
N4—H4C···O10i | 0.84 (2) | 2.46 (3) | 2.991 (3) | 122 (3) |
N6—H6D···O10i | 0.86 (2) | 2.29 (3) | 3.050 (4) | 148 (4) |
N2—H2D···O12ii | 0.85 (2) | 2.21 (2) | 2.976 (4) | 150 (3) |
N6—H6C···O12ii | 0.84 (2) | 2.29 (3) | 3.022 (4) | 146 (4) |
N3—H3D···O11iii | 0.84 (2) | 2.31 (3) | 3.047 (4) | 147 (4) |
Symmetry codes: (i) −x+1/2, y, −z; (ii) x+1/2, −y, z; (iii) −x+1/2, −y+1/2, −z+1/2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register