Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618000025/eg3232sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229618000025/eg3232Isup2.hkl |
CCDC reference: 1814183
Data collection: APEX2 (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXLT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2005); software used to prepare material for publication: publCIF (Westrip, 2010).
[Cd(C12H6N6O4)(H2O)2] | F(000) = 880 |
Mr = 446.66 | Dx = 2.000 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 20.0932 (9) Å | Cell parameters from 5786 reflections |
b = 7.1128 (3) Å | θ = 3.0–28.2° |
c = 10.4548 (4) Å | µ = 1.52 mm−1 |
β = 96.857 (1)° | T = 298 K |
V = 1483.50 (11) Å3 | Rhombic, white |
Z = 4 | 0.20 × 0.20 × 0.10 mm |
Bruker APEXII CCD diffractometer | 1734 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.022 |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | θmax = 28.3°, θmin = 3.0° |
Tmin = 0.683, Tmax = 0.746 | h = −26→26 |
6888 measured reflections | k = −9→9 |
1816 independent reflections | l = −12→13 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.016 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.039 | w = 1/[σ2(Fo2) + (0.0178P)2 + 1.1701P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max < 0.001 |
1816 reflections | Δρmax = 0.39 e Å−3 |
122 parameters | Δρmin = −0.35 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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 | 0.14436 (2) | 0.2500 | 0.01513 (5) | |
O1 | 0.08596 (5) | 0.15441 (16) | 0.11747 (11) | 0.0245 (2) | |
O2 | 0.16855 (6) | 0.0854 (3) | 0.27234 (14) | 0.0495 (4) | |
O3 | 0.06470 (6) | −0.09414 (18) | 0.35380 (13) | 0.0290 (3) | |
H3A | 0.0691 (14) | −0.114 (3) | 0.438 (3) | 0.053 (8)* | |
H3B | 0.1051 (15) | −0.048 (4) | 0.333 (3) | 0.071 (9)* | |
N1 | 0.13667 (6) | 0.48158 (18) | −0.01553 (12) | 0.0186 (2) | |
N2 | 0.11585 (8) | 0.5724 (2) | 0.08670 (13) | 0.0295 (3) | |
N3 | 0.05439 (7) | 0.65764 (18) | −0.09719 (13) | 0.0235 (3) | |
C1 | 0.19361 (7) | 0.3595 (2) | −0.00502 (14) | 0.0188 (3) | |
C2 | 0.19957 (7) | 0.2079 (2) | 0.07980 (14) | 0.0193 (3) | |
C3 | 0.25735 (7) | 0.0986 (2) | 0.08314 (15) | 0.0220 (3) | |
H3 | 0.2630 | −0.0039 | 0.1386 | 0.026* | |
C4 | 0.14741 (8) | 0.1455 (2) | 0.16448 (16) | 0.0228 (3) | |
C5 | 0.09981 (7) | 0.5340 (2) | −0.12351 (15) | 0.0224 (3) | |
H5 | 0.1052 | 0.4901 | −0.2054 | 0.027* | |
C6 | 0.06632 (9) | 0.6767 (2) | 0.03246 (17) | 0.0300 (4) | |
H6 | 0.0416 | 0.7566 | 0.0790 | 0.036* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.01299 (7) | 0.01765 (8) | 0.01486 (8) | 0.000 | 0.00206 (5) | 0.000 |
O1 | 0.0152 (5) | 0.0374 (6) | 0.0222 (6) | 0.0029 (4) | 0.0072 (4) | 0.0039 (5) |
O2 | 0.0217 (6) | 0.0955 (12) | 0.0323 (7) | 0.0056 (7) | 0.0079 (5) | 0.0338 (8) |
O3 | 0.0262 (6) | 0.0321 (6) | 0.0287 (7) | 0.0042 (5) | 0.0036 (5) | 0.0099 (5) |
N1 | 0.0164 (5) | 0.0239 (6) | 0.0165 (6) | 0.0071 (5) | 0.0059 (5) | 0.0034 (5) |
N2 | 0.0330 (7) | 0.0379 (8) | 0.0184 (7) | 0.0151 (6) | 0.0065 (6) | 0.0004 (6) |
N3 | 0.0211 (6) | 0.0271 (7) | 0.0231 (7) | 0.0087 (5) | 0.0050 (5) | 0.0047 (5) |
C1 | 0.0139 (6) | 0.0242 (7) | 0.0190 (7) | 0.0069 (5) | 0.0044 (5) | 0.0037 (5) |
C2 | 0.0139 (6) | 0.0259 (7) | 0.0190 (7) | 0.0040 (5) | 0.0059 (5) | 0.0050 (5) |
C3 | 0.0174 (7) | 0.0268 (7) | 0.0229 (7) | 0.0060 (6) | 0.0070 (6) | 0.0100 (6) |
C4 | 0.0166 (6) | 0.0312 (8) | 0.0221 (7) | 0.0047 (6) | 0.0086 (6) | 0.0075 (6) |
C5 | 0.0218 (7) | 0.0270 (8) | 0.0184 (7) | 0.0079 (6) | 0.0024 (6) | 0.0015 (6) |
C6 | 0.0329 (9) | 0.0348 (9) | 0.0234 (8) | 0.0168 (7) | 0.0081 (7) | 0.0014 (6) |
Cd1—N3i | 2.3051 (13) | N2—C6 | 1.314 (2) |
Cd1—N3ii | 2.3051 (13) | N3—C5 | 1.3200 (19) |
Cd1—O3iii | 2.3256 (12) | N3—C6 | 1.355 (2) |
Cd1—O3 | 2.3256 (12) | N3—Cd1ii | 2.3051 (13) |
Cd1—O1iii | 2.3408 (11) | C1—C3iv | 1.385 (2) |
Cd1—O1 | 2.3408 (11) | C1—C2 | 1.392 (2) |
O1—C4 | 1.2750 (19) | C2—C3 | 1.394 (2) |
O2—C4 | 1.233 (2) | C2—C4 | 1.517 (2) |
O3—H3A | 0.88 (3) | C3—C1iv | 1.385 (2) |
O3—H3B | 0.92 (3) | C3—H3 | 0.9300 |
N1—C5 | 1.3274 (19) | C5—H5 | 0.9300 |
N1—N2 | 1.3570 (18) | C6—H6 | 0.9300 |
N1—C1 | 1.4299 (17) | ||
N3i—Cd1—N3ii | 104.68 (7) | C6—N2—N1 | 102.56 (13) |
N3i—Cd1—O3iii | 164.04 (5) | C5—N3—C6 | 103.35 (13) |
N3ii—Cd1—O3iii | 85.98 (5) | C5—N3—Cd1ii | 123.03 (11) |
N3i—Cd1—O3 | 85.98 (5) | C6—N3—Cd1ii | 130.17 (11) |
N3ii—Cd1—O3 | 164.04 (5) | C3iv—C1—C2 | 121.92 (13) |
O3iii—Cd1—O3 | 86.32 (7) | C3iv—C1—N1 | 116.31 (13) |
N3i—Cd1—O1iii | 83.88 (4) | C2—C1—N1 | 121.77 (13) |
N3ii—Cd1—O1iii | 93.98 (4) | C1—C2—C3 | 117.13 (13) |
O3iii—Cd1—O1iii | 83.55 (4) | C1—C2—C4 | 125.82 (13) |
O3—Cd1—O1iii | 99.03 (4) | C3—C2—C4 | 116.98 (13) |
N3i—Cd1—O1 | 93.98 (4) | C1iv—C3—C2 | 120.95 (14) |
N3ii—Cd1—O1 | 83.88 (4) | C1iv—C3—H3 | 119.5 |
O3iii—Cd1—O1 | 99.03 (4) | C2—C3—H3 | 119.5 |
O3—Cd1—O1 | 83.55 (4) | O2—C4—O1 | 125.57 (14) |
O1iii—Cd1—O1 | 176.50 (6) | O2—C4—C2 | 116.66 (14) |
C4—O1—Cd1 | 121.29 (10) | O1—C4—C2 | 117.74 (13) |
Cd1—O3—H3A | 124.3 (17) | N3—C5—N1 | 109.83 (14) |
Cd1—O3—H3B | 95.2 (18) | N3—C5—H5 | 125.1 |
H3A—O3—H3B | 108 (2) | N1—C5—H5 | 125.1 |
C5—N1—N2 | 110.06 (12) | N2—C6—N3 | 114.19 (14) |
C5—N1—C1 | 126.57 (13) | N2—C6—H6 | 122.9 |
N2—N1—C1 | 123.20 (12) | N3—C6—H6 | 122.9 |
C5—N1—N2—C6 | 0.07 (19) | Cd1—O1—C4—C2 | −162.87 (10) |
C1—N1—N2—C6 | 175.63 (15) | C1—C2—C4—O2 | −143.50 (18) |
C5—N1—C1—C3iv | 50.1 (2) | C3—C2—C4—O2 | 39.5 (2) |
N2—N1—C1—C3iv | −124.72 (17) | C1—C2—C4—O1 | 38.4 (2) |
C5—N1—C1—C2 | −130.37 (17) | C3—C2—C4—O1 | −138.58 (16) |
N2—N1—C1—C2 | 54.8 (2) | C6—N3—C5—N1 | 0.21 (18) |
C3iv—C1—C2—C3 | 0.0 (3) | Cd1ii—N3—C5—N1 | 161.12 (10) |
N1—C1—C2—C3 | −179.53 (14) | N2—N1—C5—N3 | −0.19 (19) |
C3iv—C1—C2—C4 | −177.03 (16) | C1—N1—C5—N3 | −175.56 (14) |
N1—C1—C2—C4 | 3.4 (2) | N1—N2—C6—N3 | 0.1 (2) |
C1—C2—C3—C1iv | 0.0 (3) | C5—N3—C6—N2 | −0.2 (2) |
C4—C2—C3—C1iv | 177.30 (15) | Cd1ii—N3—C6—N2 | −159.15 (13) |
Cd1—O1—C4—O2 | 19.3 (2) |
Symmetry codes: (i) x, −y+1, z+1/2; (ii) −x, −y+1, −z; (iii) −x, y, −z+1/2; (iv) −x+1/2, −y+1/2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C6—H6···O3v | 0.93 | 2.56 | 3.428 (2) | 156 |
C5—H5···N2vi | 0.93 | 2.25 | 3.176 (2) | 172 |
O3—H3B···O2 | 0.92 (3) | 1.77 (3) | 2.6711 (19) | 165 (3) |
O3—H3A···O1vii | 0.88 (3) | 1.89 (3) | 2.7720 (18) | 175 (3) |
Symmetry codes: (v) −x, y+1, −z+1/2; (vi) x, −y+1, z−1/2; (vii) x, −y, z+1/2. |