Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806030625/cv2080sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806030625/cv2080Isup2.hkl |
CCDC reference: 620771
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å
- R factor = 0.023
- wR factor = 0.060
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.40 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.03 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
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 25.71 From the CIF: _reflns_number_total 1074 Count of symmetry unique reflns 604 Completeness (_total/calc) 177.81% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 470 Fraction of Friedel pairs measured 0.778 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Cd(C10H10N4)3](NO3)2 | Dx = 1.572 Mg m−3 |
Mr = 795.08 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, R32 | Cell parameters from 3806 reflections |
a = 14.8206 (15) Å | θ = 2.2–27.9° |
c = 13.248 (3) Å | µ = 0.72 mm−1 |
V = 2520.1 (6) Å3 | T = 298 K |
Z = 3 | Cuboid, yellow |
F(000) = 1212 | 0.60 × 0.45 × 0.42 mm |
Bruker SMART APEX CCD diffractometer | 1074 independent reflections |
Radiation source: fine-focus sealed tube | 1070 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
φ and ω scans | θmax = 25.7°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −18→14 |
Tmin = 0.673, Tmax = 0.753 | k = −18→17 |
4406 measured reflections | l = −16→16 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.023 | H-atom parameters constrained |
wR(F2) = 0.060 | w = 1/[σ2(Fo2) + (0.041P)2 + 0.3368P] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max = 0.001 |
1074 reflections | Δρmax = 0.44 e Å−3 |
78 parameters | Δρmin = −0.18 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 470 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.06 (3) |
Experimental. The IR stretching vibrations of the pyridine ring and amino groups appeared at 1636, 1586, 1464, 1445 and 1384 cm-1. |
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 | ||
Cd1 | 0.0000 | 0.0000 | 0.0000 | 0.04228 (13) | |
C1 | 0.1773 (5) | 0.3639 (2) | 0.1277 (2) | 0.0713 (7) | |
H1 | 0.2038 | 0.4340 | 0.1427 | 0.086* | |
N1 | 0.09801 (14) | 0.15646 (16) | 0.08613 (15) | 0.0461 (6) | |
C4 | 0.18362 (19) | 0.22741 (19) | 0.03703 (19) | 0.0455 (5) | |
C3 | 0.0541 (2) | 0.1866 (2) | 0.1558 (2) | 0.0604 (7) | |
H3 | −0.0056 | 0.1368 | 0.1887 | 0.073* | |
C2 | 0.0955 (3) | 0.2905 (3) | 0.1802 (3) | 0.0730 (9) | |
H2 | 0.0669 | 0.3098 | 0.2327 | 0.088* | |
C5 | 0.2228 (2) | 0.3349 (2) | 0.0505 (3) | 0.0584 (7) | |
N2 | 0.2979 (3) | 0.4090 (2) | −0.0090 (3) | 0.0857 (10) | |
H2A | 0.3176 | 0.4737 | 0.0005 | 0.103* | |
H2B | 0.3257 | 0.3913 | −0.0563 | 0.103* | |
N3 | 0.3333 | 0.6667 | 0.0434 (2) | 0.0492 (6) | |
O1 | 0.3962 (2) | 0.6345 (2) | 0.04380 (18) | 0.0757 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.03442 (14) | 0.03442 (14) | 0.0580 (2) | 0.01721 (7) | 0.000 | 0.000 |
C1 | 0.074 (3) | 0.0478 (12) | 0.0980 (17) | 0.035 (2) | 0.000 (3) | −0.0176 (12) |
N1 | 0.0424 (14) | 0.0422 (9) | 0.0558 (10) | 0.0227 (8) | 0.0026 (8) | −0.0031 (8) |
C4 | 0.0388 (12) | 0.0390 (12) | 0.0615 (13) | 0.0215 (10) | −0.0039 (10) | −0.0048 (10) |
C3 | 0.0598 (16) | 0.0584 (16) | 0.0652 (16) | 0.0312 (14) | 0.0092 (13) | −0.0005 (13) |
C2 | 0.086 (2) | 0.070 (2) | 0.0777 (19) | 0.0494 (19) | 0.0073 (17) | −0.0170 (15) |
C5 | 0.0485 (15) | 0.0367 (13) | 0.0873 (19) | 0.0192 (12) | −0.0037 (13) | −0.0066 (12) |
N2 | 0.072 (2) | 0.0355 (12) | 0.140 (3) | 0.0197 (13) | 0.0288 (19) | 0.0042 (15) |
N3 | 0.0458 (9) | 0.0458 (9) | 0.0562 (14) | 0.0229 (5) | 0.000 | 0.000 |
O1 | 0.0571 (17) | 0.0606 (17) | 0.1183 (15) | 0.0360 (16) | −0.0014 (12) | −0.0053 (12) |
Cd1—N1 | 2.328 (2) | C4—C5 | 1.408 (4) |
Cd1—N1i | 2.328 (2) | C4—C4iii | 1.492 (5) |
Cd1—N1ii | 2.328 (2) | C3—C2 | 1.381 (5) |
Cd1—N1iii | 2.328 (2) | C3—H3 | 0.9300 |
Cd1—N1iv | 2.328 (2) | C2—H2 | 0.9300 |
Cd1—N1v | 2.328 (2) | C5—N2 | 1.358 (4) |
C1—C2 | 1.348 (6) | N2—H2A | 0.8600 |
C1—C5 | 1.405 (5) | N2—H2B | 0.8600 |
C1—H1 | 0.9300 | N3—O1vi | 1.241 (2) |
N1—C3 | 1.329 (3) | N3—O1vii | 1.241 (2) |
N1—C4 | 1.343 (3) | N3—O1 | 1.241 (2) |
N1—Cd1—N1i | 165.53 (9) | C4—N1—Cd1 | 114.65 (15) |
N1—Cd1—N1ii | 93.68 (9) | N1—C4—C5 | 121.2 (2) |
N1i—Cd1—N1ii | 98.03 (6) | N1—C4—C4iii | 115.09 (15) |
N1—Cd1—N1iii | 71.82 (9) | C5—C4—C4iii | 123.6 (2) |
N1i—Cd1—N1iii | 98.03 (6) | N1—C3—C2 | 121.2 (3) |
N1ii—Cd1—N1iii | 98.03 (6) | N1—C3—H3 | 119.4 |
N1—Cd1—N1iv | 98.03 (6) | C2—C3—H3 | 119.4 |
N1i—Cd1—N1iv | 71.82 (9) | C1—C2—C3 | 119.8 (3) |
N1ii—Cd1—N1iv | 165.53 (9) | C1—C2—H2 | 120.1 |
N1iii—Cd1—N1iv | 93.68 (9) | C3—C2—H2 | 120.1 |
N1—Cd1—N1v | 98.03 (6) | N2—C5—C1 | 120.0 (3) |
N1i—Cd1—N1v | 93.68 (9) | N2—C5—C4 | 123.3 (3) |
N1ii—Cd1—N1v | 71.82 (9) | C1—C5—C4 | 116.7 (3) |
N1iii—Cd1—N1v | 165.53 (9) | C5—N2—H2A | 120.0 |
N1iv—Cd1—N1v | 98.03 (6) | C5—N2—H2B | 120.0 |
C2—C1—C5 | 120.3 (3) | H2A—N2—H2B | 120.0 |
C2—C1—H1 | 119.9 | O1vi—N3—O1vii | 119.998 (3) |
C5—C1—H1 | 119.9 | O1vi—N3—O1 | 119.998 (4) |
C3—N1—C4 | 120.2 (2) | O1vii—N3—O1 | 119.998 (3) |
C3—N1—Cd1 | 120.59 (19) | ||
N1i—Cd1—N1—C3 | −147.7 (2) | C3—N1—C4—C4iii | 178.2 (3) |
N1ii—Cd1—N1—C3 | 68.20 (19) | Cd1—N1—C4—C4iii | −25.7 (3) |
N1iii—Cd1—N1—C3 | 165.5 (2) | C4—N1—C3—C2 | −0.7 (4) |
N1iv—Cd1—N1—C3 | −103.29 (17) | Cd1—N1—C3—C2 | −155.4 (3) |
N1v—Cd1—N1—C3 | −3.9 (2) | C5—C1—C2—C3 | −2.1 (7) |
N1i—Cd1—N1—C4 | 56.3 (4) | N1—C3—C2—C1 | 4.9 (6) |
N1ii—Cd1—N1—C4 | −87.8 (4) | C2—C1—C5—N2 | 173.1 (4) |
N1iii—Cd1—N1—C4 | 9.43 (19) | C2—C1—C5—C4 | −4.5 (7) |
N1iv—Cd1—N1—C4 | 100.7 (4) | N1—C4—C5—N2 | −168.7 (3) |
N1v—Cd1—N1—C4 | −159.9 (4) | C4iii—C4—C5—N2 | 6.4 (5) |
C3—N1—C4—C5 | −6.3 (4) | N1—C4—C5—C1 | 8.8 (5) |
Cd1—N1—C4—C5 | 149.8 (2) | C4iii—C4—C5—C1 | −176.1 (4) |
Symmetry codes: (i) x−y, −y, −z; (ii) −x, −x+y, −z; (iii) y, x, −z; (iv) −x+y, −x, z; (v) −y, x−y, z; (vi) −y+1, x−y+1, z; (vii) −x+y, −x+1, z. |
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