Hexakis[μ-9-methyl-3-(1H-tetra­zol-5-io)-4H-pyrido[1,2-a]pyrimidin-4-onato(2–)]tricadmium(II)

The centrosymmetric mol­ecule of the title Cd^II complex, [Cd₃(C₁₀H₇N₆O)₆], is located on a threefold axis. The pyridopyrimidine ligands bridge neighbouring Cd atoms, forming a trinuclear complex. π–π Stacking is observed between neighbouring complex mol­ecules.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.032
• wR factor = 0.079
• Data-to-parameter ratio = 15.4

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT411_ALERT_2_B Short Inter H...H Contact  H4A    ..  H4A     ..       1.92 Ang.

Alert level C
ABSTM02_ALERT_3_C  The ratio of Tmax/Tmin expected RT(exp) is > 1.10
            Absorption corrections should be applied.
            Tmin and Tmax expected:      0.614     0.710
            RT(exp) =      1.157
PLAT057_ALERT_3_C Correction for Absorption Required   RT(exp) ...       1.16
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT413_ALERT_2_C Short Inter XH3 .. XHn     H10B   ..  H10B    ..       2.12 Ang.

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   0 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
   2 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Hexakis[µ-9-methyl-3-(1H-tetrazol-5-io)-4H-pyrido[1,2-a]pyrimidin-4- onato(2-)]tricadmium(II)

Crystal data

[Cd3(C10H7N6O)6]	Dx = 1.878 Mg m^−3
Mr = 1700.53	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c	Cell parameters from 15120 reflections
Hall symbol: -R 3 2"c	θ = 1.8–28.3°
a = 18.302 (3) Å	µ = 1.14 mm^−1
c = 31.099 (6) Å	T = 293 K
V = 9021 (3) Å^3	Block, colourless
Z = 6	0.44 × 0.39 × 0.30 mm
F(000) = 5076.0

Data collection

Siemens SMART CCD diffractometer	1874 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.043
Graphite monochromator	θmax = 28.3°, θmin = 1.8°
φ and ω scans	h = −24→18
15306 measured reflections	k = −10→24
2466 independent reflections	l = −40→40

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.079	H-atom parameters constrained
S = 0.99	w = 1/[σ^2(Fo^2) + (0.0385P)^2] where P = (Fo^2 + 2Fc^2)/3
2466 reflections	(Δ/σ)max = 0.002
160 parameters	Δρmax = 0.88 e Å^−3
0 restraints	Δρmin = −0.66 e Å^−3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cd1	1.0000	1.0000	0.0000	0.01551 (12)
Cd2	1.0000	1.0000	0.129037 (10)	0.01639 (10)
C1	0.99809 (15)	0.82450 (15)	0.09670 (8)	0.0174 (5)
C2	0.97294 (15)	0.78122 (16)	0.13808 (8)	0.0192 (5)
C3	0.95033 (16)	0.81482 (16)	0.17287 (8)	0.0208 (6)
N6	0.92026 (13)	0.76042 (13)	0.21010 (7)	0.0214 (5)
C4	0.89595 (18)	0.7886 (2)	0.24498 (9)	0.0315 (7)
H4A	0.9015	0.8419	0.2442	0.038*
C5	0.86375 (17)	0.7402 (2)	0.28087 (9)	0.0321 (7)
H5A	0.8454	0.7593	0.3039	0.039*
C6	0.85866 (17)	0.66116 (18)	0.28260 (9)	0.0277 (6)
H6A	0.8376	0.6281	0.3072	0.033*
C7	0.88430 (16)	0.63223 (17)	0.24858 (9)	0.0251 (6)
C8	0.91581 (15)	0.68253 (16)	0.21046 (8)	0.0204 (6)
C9	0.96709 (16)	0.70237 (16)	0.14246 (8)	0.0227 (6)
H9A	0.9844	0.6827	0.1192	0.027*
C10	0.87995 (19)	0.54835 (17)	0.24912 (10)	0.0337 (7)
H10A	0.8626	0.5234	0.2771	0.051*
H10B	0.9346	0.5558	0.2426	0.051*
H10C	0.8400	0.5120	0.2280	0.051*
N1	1.00198 (12)	0.89788 (13)	0.08710 (6)	0.0172 (4)
N2	1.01909 (13)	0.90834 (13)	0.04467 (6)	0.0174 (4)
N3	1.02625 (13)	0.84484 (13)	0.02990 (7)	0.0213 (5)
N4	1.01348 (13)	0.79089 (14)	0.06188 (7)	0.0226 (5)
N5	0.93889 (14)	0.65317 (13)	0.17698 (7)	0.0239 (5)
O1	0.95216 (12)	0.88382 (12)	0.17567 (6)	0.0261 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.01798 (16)	0.01798 (16)	0.0106 (2)	0.00899 (8)	0.000	0.000
Cd2	0.01806 (13)	0.01806 (13)	0.01305 (17)	0.00903 (6)	0.000	0.000
C1	0.0165 (13)	0.0208 (13)	0.0161 (13)	0.0101 (11)	−0.0005 (10)	0.0003 (10)
C2	0.0188 (13)	0.0207 (13)	0.0174 (13)	0.0092 (11)	0.0004 (10)	0.0017 (10)
C3	0.0186 (14)	0.0218 (14)	0.0190 (13)	0.0079 (11)	−0.0005 (11)	0.0045 (11)
N6	0.0222 (12)	0.0256 (12)	0.0177 (11)	0.0128 (10)	0.0011 (9)	0.0025 (9)
C4	0.0427 (18)	0.0362 (17)	0.0233 (15)	0.0255 (15)	0.0087 (13)	0.0047 (13)
C5	0.0344 (17)	0.0415 (18)	0.0226 (15)	0.0205 (15)	0.0066 (13)	0.0056 (13)
C6	0.0211 (14)	0.0337 (17)	0.0209 (14)	0.0081 (13)	0.0006 (12)	0.0107 (12)
C7	0.0158 (13)	0.0260 (15)	0.0254 (15)	0.0044 (12)	−0.0046 (11)	0.0057 (12)
C8	0.0169 (13)	0.0208 (14)	0.0216 (14)	0.0080 (11)	−0.0032 (11)	0.0023 (11)
C9	0.0212 (14)	0.0245 (14)	0.0222 (14)	0.0113 (12)	0.0011 (11)	0.0013 (11)
C10	0.0324 (17)	0.0278 (16)	0.0325 (17)	0.0087 (14)	−0.0022 (14)	0.0102 (13)
N1	0.0187 (11)	0.0200 (11)	0.0137 (10)	0.0103 (9)	0.0021 (8)	0.0019 (9)
N2	0.0201 (12)	0.0225 (12)	0.0112 (10)	0.0119 (10)	0.0011 (9)	0.0003 (9)
N3	0.0241 (12)	0.0245 (12)	0.0179 (11)	0.0141 (10)	0.0033 (9)	0.0009 (9)
N4	0.0294 (13)	0.0253 (12)	0.0180 (12)	0.0173 (11)	0.0048 (10)	0.0038 (9)
N5	0.0252 (12)	0.0243 (13)	0.0228 (12)	0.0129 (10)	0.0012 (10)	0.0058 (10)
O1	0.0385 (12)	0.0253 (11)	0.0194 (10)	0.0197 (9)	0.0049 (8)	0.0031 (8)

Geometric parameters (Å, º)

Cd1—N2^i	2.335 (2)	N6—C4	1.367 (3)
Cd1—N2^ii	2.335 (2)	N6—C8	1.387 (3)
Cd1—N2^iii	2.335 (2)	C4—C5	1.362 (4)
Cd1—N2^iv	2.335 (2)	C4—H4A	0.9300
Cd1—N2^v	2.335 (2)	C5—C6	1.404 (4)
Cd1—N2	2.335 (2)	C5—H5A	0.9300
Cd2—N1^v	2.294 (2)	C6—C7	1.367 (4)
Cd2—N1^i	2.294 (2)	C6—H6A	0.9300
Cd2—N1	2.294 (2)	C7—C8	1.434 (4)
Cd2—O1^i	2.3514 (19)	C7—C10	1.497 (4)
Cd2—O1^v	2.3514 (19)	C8—N5	1.333 (3)
Cd2—O1	2.3514 (19)	C9—N5	1.328 (3)
C1—N1	1.342 (3)	C9—H9A	0.9300
C1—N4	1.343 (3)	C10—H10A	0.9600
C1—C2	1.460 (3)	C10—H10B	0.9600
C2—C9	1.399 (3)	C10—H10C	0.9600
C2—C3	1.405 (3)	N1—N2	1.348 (3)
C3—O1	1.250 (3)	N2—N3	1.316 (3)
C3—N6	1.445 (3)	N3—N4	1.337 (3)
N2^i—Cd1—N2^ii	180.0	C2—C3—N6	114.2 (2)
N2^i—Cd1—N2^iii	91.77 (7)	C4—N6—C8	121.2 (2)
N2^ii—Cd1—N2^iii	88.23 (7)	C4—N6—C3	117.4 (2)
N2^i—Cd1—N2^iv	91.77 (7)	C8—N6—C3	121.4 (2)
N2^ii—Cd1—N2^iv	88.23 (7)	C5—C4—N6	121.4 (3)
N2^iii—Cd1—N2^iv	88.23 (7)	C5—C4—H4A	119.3
N2^i—Cd1—N2^v	88.23 (7)	N6—C4—H4A	119.3
N2^ii—Cd1—N2^v	91.77 (7)	C4—C5—C6	119.1 (3)
N2^iii—Cd1—N2^v	91.77 (7)	C4—C5—H5A	120.5
N2^iv—Cd1—N2^v	180.0	C6—C5—H5A	120.5
N2^i—Cd1—N2	88.23 (7)	C7—C6—C5	120.7 (3)
N2^ii—Cd1—N2	91.77 (7)	C7—C6—H6A	119.6
N2^iii—Cd1—N2	180.00 (10)	C5—C6—H6A	119.6
N2^iv—Cd1—N2	91.77 (7)	C6—C7—C8	119.8 (2)
N2^v—Cd1—N2	88.23 (7)	C6—C7—C10	122.4 (3)
N1^v—Cd2—N1^i	90.88 (7)	C8—C7—C10	117.8 (3)
N1^v—Cd2—N1	90.87 (7)	N5—C8—N6	122.7 (2)
N1^i—Cd2—N1	90.87 (7)	N5—C8—C7	119.6 (2)
N1^v—Cd2—O1^i	151.88 (7)	N6—C8—C7	117.7 (2)
N1^i—Cd2—O1^i	76.37 (7)	N5—C9—C2	125.5 (3)
N1—Cd2—O1^i	113.92 (7)	N5—C9—H9A	117.2
N1^v—Cd2—O1^v	76.37 (7)	C2—C9—H9A	117.2
N1^i—Cd2—O1^v	113.92 (7)	C7—C10—H10A	109.5
N1—Cd2—O1^v	151.88 (7)	C7—C10—H10B	109.5
O1^i—Cd2—O1^v	85.95 (7)	H10A—C10—H10B	109.5
N1^v—Cd2—O1	113.92 (7)	C7—C10—H10C	109.5
N1^i—Cd2—O1	151.88 (7)	H10A—C10—H10C	109.5
N1—Cd2—O1	76.37 (7)	H10B—C10—H10C	109.5
O1^i—Cd2—O1	85.95 (7)	C1—N1—N2	104.61 (19)
O1^v—Cd2—O1	85.95 (7)	C1—N1—Cd2	132.38 (16)
N1—C1—N4	111.1 (2)	N2—N1—Cd2	122.55 (15)
N1—C1—C2	125.7 (2)	N3—N2—N1	109.57 (19)
N4—C1—C2	122.9 (2)	N3—N2—Cd1	122.93 (15)
C9—C2—C3	119.3 (2)	N1—N2—Cd1	125.24 (15)
C9—C2—C1	119.1 (2)	N2—N3—N4	109.6 (2)
C3—C2—C1	121.6 (2)	N3—N4—C1	105.1 (2)
O1—C3—C2	129.1 (2)	C9—N5—C8	116.9 (2)
O1—C3—N6	116.7 (2)	C3—O1—Cd2	132.89 (17)

Symmetry codes: (i) −y+2, x−y+1, z; (ii) y, −x+y+1, −z; (iii) −x+2, −y+2, −z; (iv) x−y+1, x, −z; (v) −x+y+1, −x+2, z.