Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807007593/bh2071sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807007593/bh2071Isup2.hkl |
CCDC reference: 642909
Key indicators
- Single-crystal X-ray study
- T = 291 K
- Mean (C-C) = 0.008 Å
- Disorder in main residue
- R factor = 0.038
- wR factor = 0.107
- Data-to-parameter ratio = 12.0
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O1 PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O1' PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Cd1 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N4 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N4'
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C6 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C3 PLAT301_ALERT_3_C Main Residue Disorder ......................... 19.00 Perc.
0 ALERT level A = In general: serious problem 5 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[Cd(NO3)2(C9H9N3)2] | F(000) = 556 |
Mr = 554.80 | Dx = 1.638 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2258 reflections |
a = 8.3567 (17) Å | θ = 2.8–27.9° |
b = 16.327 (3) Å | µ = 1.02 mm−1 |
c = 9.0472 (18) Å | T = 291 K |
β = 114.330 (3)° | Block, colourless |
V = 1124.8 (4) Å3 | 0.30 × 0.24 × 0.16 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 1960 independent reflections |
Radiation source: fine-focus sealed tube | 1630 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.012 |
φ and ω scans | θmax = 25.1°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.749, Tmax = 0.853 | k = −19→16 |
3912 measured reflections | l = −10→10 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0606P)2 + 1.6575P] where P = (Fo2 + 2Fc2)/3 |
1960 reflections | (Δ/σ)max < 0.001 |
164 parameters | Δρmax = 1.03 e Å−3 |
162 restraints | Δρmin = −0.66 e Å−3 |
Refinement. Highest peak 1.03 at 0.9222 0.0436 0.7103 [1.20 A from O1'] Deepest hole -0.66 at 0.0532 0.0007 0.3640 [0.34 A from O2] |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
O1 | −0.2664 (7) | 0.4367 (5) | 0.8171 (8) | 0.0968 (19) | 0.675 (6) |
O2 | −0.4231 (16) | 0.5007 (6) | 0.9044 (14) | 0.169 (4) | 0.675 (6) |
O3 | −0.5469 (10) | 0.4200 (6) | 0.7129 (16) | 0.101 (2) | 0.675 (6) |
N4 | −0.4134 (10) | 0.4557 (5) | 0.7998 (13) | 0.0749 (16) | 0.675 (6) |
O1' | −0.3066 (17) | 0.4942 (9) | 0.842 (2) | 0.0968 (19) | 0.325 (6) |
O2' | −0.371 (3) | 0.3750 (9) | 0.888 (2) | 0.169 (4) | 0.325 (6) |
O3' | −0.559 (2) | 0.4459 (13) | 0.702 (3) | 0.101 (2) | 0.325 (6) |
N4' | −0.408 (2) | 0.4365 (10) | 0.802 (3) | 0.0749 (16) | 0.325 (6) |
Cd1 | 0.0000 | 0.5000 | 1.0000 | 0.04614 (19) | |
N1 | 0.0899 (5) | 0.3647 (2) | 0.9652 (5) | 0.0568 (9) | |
N2 | 0.3827 (7) | 0.0977 (2) | 0.9013 (6) | 0.0668 (12) | |
N3 | 0.4766 (5) | 0.0508 (2) | 0.7258 (4) | 0.0484 (8) | |
C1 | 0.0094 (7) | 0.3010 (4) | 0.9990 (7) | 0.0766 (18) | |
H1 | −0.0878 | 0.3113 | 1.0214 | 0.092* | |
C2 | 0.0628 (9) | 0.2222 (3) | 1.0021 (8) | 0.0770 (16) | |
H2 | 0.0041 | 0.1803 | 1.0292 | 0.092* | |
C3 | 0.2034 (7) | 0.2039 (3) | 0.9654 (6) | 0.0640 (13) | |
C4 | 0.2835 (7) | 0.2678 (3) | 0.9265 (7) | 0.0700 (14) | |
H4 | 0.3764 | 0.2585 | 0.8972 | 0.084* | |
C5 | 0.2247 (7) | 0.3473 (3) | 0.9309 (6) | 0.0628 (12) | |
H5 | 0.2839 | 0.3904 | 0.9083 | 0.075* | |
C6 | 0.2601 (10) | 0.1151 (3) | 0.9762 (9) | 0.092 (2) | |
H6A | 0.3151 | 0.0994 | 1.0896 | 0.110* | |
H6B | 0.1563 | 0.0813 | 0.9242 | 0.110* | |
C7 | 0.3364 (7) | 0.0639 (3) | 0.7535 (6) | 0.0566 (11) | |
H7 | 0.2220 | 0.0517 | 0.6817 | 0.068* | |
C8 | 0.6154 (7) | 0.0778 (3) | 0.8609 (6) | 0.0643 (12) | |
H8 | 0.7321 | 0.0758 | 0.8750 | 0.077* | |
C9 | 0.5611 (9) | 0.1073 (3) | 0.9694 (6) | 0.0729 (15) | |
H9 | 0.6299 | 0.1297 | 1.0702 | 0.087* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.054 (3) | 0.127 (4) | 0.113 (4) | −0.017 (3) | 0.038 (3) | −0.020 (4) |
O2 | 0.156 (6) | 0.162 (6) | 0.165 (6) | 0.024 (4) | 0.043 (5) | −0.049 (5) |
O3 | 0.063 (3) | 0.101 (6) | 0.117 (4) | −0.008 (3) | 0.016 (2) | −0.038 (5) |
N4 | 0.053 (2) | 0.094 (4) | 0.075 (3) | 0.001 (3) | 0.023 (2) | −0.020 (3) |
O1' | 0.054 (3) | 0.127 (4) | 0.113 (4) | −0.017 (3) | 0.038 (3) | −0.020 (4) |
O2' | 0.156 (6) | 0.162 (6) | 0.165 (6) | 0.024 (4) | 0.043 (5) | −0.049 (5) |
O3' | 0.063 (3) | 0.101 (6) | 0.117 (4) | −0.008 (3) | 0.016 (2) | −0.038 (5) |
N4' | 0.053 (2) | 0.094 (4) | 0.075 (3) | 0.001 (3) | 0.023 (2) | −0.020 (3) |
Cd1 | 0.0630 (3) | 0.0340 (3) | 0.0525 (3) | 0.00870 (17) | 0.0350 (2) | 0.00675 (16) |
N1 | 0.075 (2) | 0.0355 (18) | 0.075 (3) | 0.0065 (17) | 0.046 (2) | 0.0036 (17) |
N2 | 0.112 (4) | 0.038 (2) | 0.074 (3) | 0.011 (2) | 0.063 (3) | −0.0013 (18) |
N3 | 0.061 (2) | 0.0408 (19) | 0.0486 (19) | −0.0003 (15) | 0.0274 (16) | −0.0056 (15) |
C1 | 0.091 (4) | 0.044 (3) | 0.128 (5) | 0.002 (2) | 0.079 (4) | −0.002 (3) |
C2 | 0.108 (4) | 0.040 (3) | 0.118 (5) | −0.006 (3) | 0.081 (4) | −0.003 (3) |
C3 | 0.105 (4) | 0.038 (2) | 0.075 (3) | 0.007 (2) | 0.063 (3) | 0.003 (2) |
C4 | 0.099 (4) | 0.047 (3) | 0.095 (4) | 0.016 (2) | 0.072 (3) | 0.008 (2) |
C5 | 0.084 (3) | 0.041 (2) | 0.082 (3) | 0.005 (2) | 0.054 (3) | 0.006 (2) |
C6 | 0.167 (6) | 0.042 (3) | 0.124 (5) | 0.021 (3) | 0.117 (5) | 0.010 (3) |
C7 | 0.072 (3) | 0.040 (2) | 0.071 (3) | 0.000 (2) | 0.044 (2) | −0.002 (2) |
C8 | 0.067 (3) | 0.054 (3) | 0.063 (3) | 0.009 (2) | 0.017 (2) | −0.011 (2) |
C9 | 0.094 (4) | 0.064 (3) | 0.052 (3) | 0.016 (3) | 0.020 (3) | −0.010 (2) |
O1—N4 | 1.213 (8) | N3—C7 | 1.313 (5) |
O1—Cd1 | 2.393 (6) | N3—C8 | 1.365 (6) |
O2—N4 | 1.227 (9) | N3—Cd1iv | 2.287 (3) |
O3—N4 | 1.217 (7) | C1—C2 | 1.359 (7) |
O1'—N4' | 1.221 (9) | C1—H1 | 0.9300 |
O1'—Cd1 | 2.366 (13) | C2—C3 | 1.380 (7) |
O2'—N4' | 1.227 (10) | C2—H2 | 0.9300 |
O3'—N4' | 1.220 (9) | C3—C4 | 1.362 (6) |
Cd1—N3i | 2.287 (3) | C3—C6 | 1.516 (6) |
Cd1—N3ii | 2.287 (3) | C4—C5 | 1.394 (6) |
Cd1—O1'iii | 2.366 (13) | C4—H4 | 0.9300 |
Cd1—O1iii | 2.393 (6) | C5—H5 | 0.9300 |
Cd1—N1iii | 2.396 (3) | C6—H6A | 0.9700 |
Cd1—N1 | 2.396 (3) | C6—H6B | 0.9700 |
N1—C5 | 1.317 (6) | C7—H7 | 0.9300 |
N1—C1 | 1.340 (6) | C8—C9 | 1.330 (7) |
N2—C7 | 1.347 (6) | C8—H8 | 0.9300 |
N2—C9 | 1.368 (8) | C9—H9 | 0.9300 |
N2—C6 | 1.470 (6) | ||
N4—O1—Cd1 | 125.6 (6) | C1—N1—Cd1 | 118.1 (3) |
O1—N4—O3 | 124.8 (9) | C7—N2—C9 | 107.9 (4) |
O1—N4—O2 | 116.0 (8) | C7—N2—C6 | 124.5 (5) |
O3—N4—O2 | 116.8 (9) | C9—N2—C6 | 127.4 (5) |
N4'—O1'—Cd1 | 131.2 (11) | C7—N3—C8 | 105.8 (4) |
O3'—N4'—O1' | 120.2 (11) | C7—N3—Cd1iv | 129.9 (3) |
O3'—N4'—O2' | 119.3 (11) | C8—N3—Cd1iv | 124.2 (3) |
O1'—N4'—O2' | 118.7 (11) | N1—C1—C2 | 123.3 (4) |
N3i—Cd1—N3ii | 180.000 (1) | N1—C1—H1 | 118.4 |
N3i—Cd1—O1' | 93.2 (4) | C2—C1—H1 | 118.4 |
N3ii—Cd1—O1' | 86.8 (4) | C1—C2—C3 | 120.3 (5) |
N3i—Cd1—O1'iii | 86.8 (4) | C1—C2—H2 | 119.8 |
N3ii—Cd1—O1'iii | 93.2 (4) | C3—C2—H2 | 119.8 |
O1'—Cd1—O1'iii | 180.000 (2) | C4—C3—C2 | 117.0 (4) |
N3i—Cd1—O1 | 93.64 (19) | C4—C3—C6 | 125.2 (4) |
N3ii—Cd1—O1 | 86.36 (19) | C2—C3—C6 | 117.8 (4) |
O1'—Cd1—O1 | 25.5 (3) | C3—C4—C5 | 119.3 (4) |
O1'iii—Cd1—O1 | 154.5 (3) | C3—C4—H4 | 120.3 |
N3i—Cd1—O1iii | 86.36 (19) | C5—C4—H4 | 120.3 |
N3ii—Cd1—O1iii | 93.64 (19) | N1—C5—C4 | 123.5 (4) |
O1'—Cd1—O1iii | 154.5 (3) | N1—C5—H5 | 118.2 |
O1'iii—Cd1—O1iii | 25.5 (3) | C4—C5—H5 | 118.2 |
O1—Cd1—O1iii | 180.000 (1) | N2—C6—C3 | 114.4 (4) |
N3i—Cd1—N1iii | 94.05 (12) | N2—C6—H6A | 108.6 |
N3ii—Cd1—N1iii | 85.95 (12) | C3—C6—H6A | 108.6 |
O1'—Cd1—N1iii | 78.2 (4) | N2—C6—H6B | 108.6 |
O1'iii—Cd1—N1iii | 101.8 (4) | C3—C6—H6B | 108.6 |
O1—Cd1—N1iii | 103.7 (2) | H6A—C6—H6B | 107.6 |
O1iii—Cd1—N1iii | 76.3 (2) | N3—C7—N2 | 110.0 (4) |
N3i—Cd1—N1 | 85.95 (12) | N3—C7—H7 | 125.0 |
N3ii—Cd1—N1 | 94.05 (12) | N2—C7—H7 | 125.0 |
O1'—Cd1—N1 | 101.8 (4) | C9—C8—N3 | 110.8 (5) |
O1'iii—Cd1—N1 | 78.2 (4) | C9—C8—H8 | 124.6 |
O1—Cd1—N1 | 76.3 (2) | N3—C8—H8 | 124.6 |
O1iii—Cd1—N1 | 103.7 (2) | C8—C9—N2 | 105.5 (4) |
N1iii—Cd1—N1 | 180.000 (1) | C8—C9—H9 | 127.3 |
C5—N1—C1 | 116.5 (4) | N2—C9—H9 | 127.3 |
C5—N1—Cd1 | 125.1 (3) | ||
Cd1—O1—N4—O3 | −175.7 (10) | C5—N1—C1—C2 | 1.4 (8) |
Cd1—O1—N4—O2 | −13.6 (15) | Cd1—N1—C1—C2 | −172.1 (5) |
Cd1—O1'—N4'—O3' | −171 (2) | N1—C1—C2—C3 | −1.7 (9) |
Cd1—O1'—N4'—O2' | 25 (4) | C1—C2—C3—C4 | −0.1 (9) |
N4'—O1'—Cd1—N3i | −61 (2) | C1—C2—C3—C6 | 178.1 (6) |
N4'—O1'—Cd1—N3ii | 119 (2) | C2—C3—C4—C5 | 2.2 (8) |
N4'—O1'—Cd1—N1iii | −155 (2) | C6—C3—C4—C5 | −176.0 (6) |
N4'—O1'—Cd1—N1 | 25 (2) | C1—N1—C5—C4 | 0.8 (8) |
N4—O1—Cd1—N3i | 69.5 (9) | Cd1—N1—C5—C4 | 173.7 (4) |
N4—O1—Cd1—N3ii | −110.5 (9) | C3—C4—C5—N1 | −2.6 (9) |
N4—O1—Cd1—N1iii | −25.5 (9) | C7—N2—C6—C3 | −100.6 (6) |
N4—O1—Cd1—N1 | 154.5 (9) | C9—N2—C6—C3 | 83.7 (7) |
N3i—Cd1—N1—C5 | −134.2 (4) | C4—C3—C6—N2 | −14.9 (10) |
N3ii—Cd1—N1—C5 | 45.8 (4) | C2—C3—C6—N2 | 167.0 (6) |
O1'—Cd1—N1—C5 | 133.3 (6) | C8—N3—C7—N2 | −0.3 (5) |
O1'iii—Cd1—N1—C5 | −46.7 (6) | Cd1iv—N3—C7—N2 | −177.6 (3) |
O1—Cd1—N1—C5 | 131.0 (4) | C9—N2—C7—N3 | 0.8 (5) |
O1iii—Cd1—N1—C5 | −49.0 (4) | C6—N2—C7—N3 | −175.6 (4) |
N3i—Cd1—N1—C1 | 38.6 (4) | C7—N3—C8—C9 | −0.3 (6) |
N3ii—Cd1—N1—C1 | −141.4 (4) | Cd1iv—N3—C8—C9 | 177.2 (3) |
O1'—Cd1—N1—C1 | −53.9 (6) | N3—C8—C9—N2 | 0.7 (6) |
O1'iii—Cd1—N1—C1 | 126.1 (6) | C7—N2—C9—C8 | −0.9 (5) |
O1—Cd1—N1—C1 | −56.2 (4) | C6—N2—C9—C8 | 175.3 (4) |
O1iii—Cd1—N1—C1 | 123.8 (4) |
Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (ii) −x+1/2, y+1/2, −z+3/2; (iii) −x, −y+1, −z+2; (iv) −x+1/2, y−1/2, −z+3/2. |
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