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The binicotinate dianion in cadmium binicotinate, [Cd(C12H6N2O4)], lies on a special position of 2 symmetry; the Cd atom lies on another special position of 2 symmetry. The carboxy CO2 unit chelates to the Cd atom [Cd-O 2.304 (2) and 2.396 (2) Å]; the Cd atom is linked to one N atom of another binicotinate group [Cd-N1 2.315 (2) Å] and to the N atom of a third binicotinate group in a six-coordinate, distorted octahedral environment.
Supporting information
CCDC reference: 236048
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.004 Å
- R factor = 0.019
- wR factor = 0.045
- Data-to-parameter ratio = 15.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
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 28.20
From the CIF: _reflns_number_total 1314
Count of symmetry unique reflns 772
Completeness (_total/calc) 170.21%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 542
Fraction of Friedel pairs measured 0.702
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 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
0 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
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
2,2'-Bipyridyl-3,3'-dicarboxylatocadmium(II)
top
Crystal data top
[Cd(C12H6N2O4)] | Dx = 2.144 Mg m−3 |
Mr = 354.59 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P4n2 | Cell parameters from 2772 reflections |
Hall symbol: P -4 -2n | θ = 3.5–28.2° |
a = 8.1791 (6) Å | µ = 2.00 mm−1 |
c = 16.420 (1) Å | T = 294 K |
V = 1098.4 (1) Å3 | Needle, yellow |
Z = 4 | 0.30 × 0.10 × 0.10 mm |
F(000) = 688 | |
Data collection top
Bruker SMART APEX area-detector diffractometer | 1314 independent reflections |
Radiation source: fine-focus sealed tube | 1276 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
φ and ω scan | θmax = 28.2°, θmin = 3.5° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −10→10 |
Tmin = 0.678, Tmax = 0.825 | k = −9→8 |
4888 measured reflections | l = −21→15 |
Refinement top
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)] = 0.019 | H-atom parameters constrained |
wR(F2) = 0.045 | w = 1/[σ2(Fo2) + (0.0236P)2 + 0.1528P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
1314 reflections | Δρmax = 0.37 e Å−3 |
87 parameters | Δρmin = −0.35 e Å−3 |
0 restraints | Absolute structure: Flack parameter from 548 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.01 (3) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0.71465 (2) | 0.78535 (2) | 0.7500 | 0.01865 (8) | |
N1 | 1.4751 (3) | 0.8065 (2) | 0.8244 (1) | 0.0196 (4) | |
O1 | 0.8972 (2) | 0.8095 (2) | 0.8635 (1) | 0.0318 (4) | |
O2 | 0.9953 (3) | 0.7960 (2) | 0.7387 (1) | 0.0338 (5) | |
C1 | 1.3220 (5) | 0.8087 (4) | 0.7954 (1) | 0.0161 (5) | |
C2 | 1.1858 (3) | 0.8106 (3) | 0.8475 (2) | 0.0196 (5) | |
C3 | 1.2131 (3) | 0.8108 (4) | 0.9308 (2) | 0.0259 (6) | |
C4 | 1.3711 (3) | 0.8066 (3) | 0.9603 (2) | 0.0293 (6) | |
C5 | 1.4982 (3) | 0.8037 (3) | 0.9054 (2) | 0.0251 (5) | |
C6 | 1.0142 (3) | 0.8048 (3) | 0.8144 (2) | 0.0225 (5) | |
H3 | 1.1252 | 0.8138 | 0.9667 | 0.031* | |
H4 | 1.3912 | 0.8058 | 1.0161 | 0.035* | |
H5 | 1.6046 | 0.7996 | 0.9252 | 0.030* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0169 (1) | 0.0169 (1) | 0.0222 (1) | 0.0003 (1) | 0.0001 (1) | 0.0001 (1) |
N1 | 0.017 (1) | 0.020 (1) | 0.022 (1) | −0.001 (1) | −0.001 (1) | 0.002 (1) |
O1 | 0.018 (1) | 0.045 (1) | 0.033 (1) | 0.000 (1) | 0.004 (1) | −0.003 (1) |
O2 | 0.019 (1) | 0.058 (1) | 0.025 (1) | −0.001 (1) | −0.003 (1) | 0.007 (1) |
C1 | 0.019 (2) | 0.009 (1) | 0.020 (1) | 0.000 (1) | 0.001 (1) | 0.000 (1) |
C2 | 0.017 (1) | 0.020 (1) | 0.021 (1) | 0.000 (1) | 0.001 (1) | 0.000 (1) |
C3 | 0.022 (1) | 0.033 (2) | 0.023 (1) | −0.003 (1) | 0.005 (1) | 0.001 (1) |
C4 | 0.029 (2) | 0.040 (2) | 0.019 (1) | −0.004 (1) | −0.003 (1) | 0.003 (1) |
C5 | 0.022 (1) | 0.032 (2) | 0.022 (1) | 0.000 (1) | −0.005 (1) | 0.005 (1) |
C6 | 0.018 (1) | 0.015 (1) | 0.034 (2) | 0.000 (1) | −0.001 (1) | 0.004 (1) |
Geometric parameters (Å, º) top
Cd1—O1 | 2.396 (2) | C1—C2 | 1.405 (4) |
Cd1—O1i | 2.396 (2) | C1—C1iv | 1.498 (4) |
Cd1—O2 | 2.304 (2) | C2—C3 | 1.386 (4) |
Cd1—O2i | 2.304 (2) | C2—C6 | 1.506 (4) |
Cd1—N1ii | 2.315 (2) | C3—C4 | 1.381 (4) |
Cd1—N1iii | 2.315 (2) | C4—C5 | 1.376 (4) |
N1—C1 | 1.339 (5) | C3—H3 | 0.93 |
N1—C5 | 1.344 (3) | C4—H4 | 0.93 |
O1—C6 | 1.251 (3) | C5—H5 | 0.93 |
O2—C6 | 1.256 (3) | | |
| | | |
O1—Cd1—O1i | 135.0 (1) | C6—O2—Cd1 | 92.6 (2) |
O1—Cd1—O2 | 55.9 (1) | N1—C1—C2 | 121.6 (2) |
O1—Cd1—O2i | 92.5 (1) | N1—C1—C1iv | 115.0 (3) |
O1—Cd1—N1ii | 96.4 (1) | C2—C1—C1iv | 123.2 (4) |
O1—Cd1—N1iii | 112.8 (1) | C3—C2—C1 | 118.3 (2) |
O1i—Cd1—O2 | 92.5 (1) | C3—C2—C6 | 120.4 (2) |
O1i—Cd1—O2i | 55.9 (1) | C1—C2—C6 | 121.3 (2) |
O1i—Cd1—N1ii | 112.8 (1) | C4—C3—C2 | 119.8 (2) |
O1i—Cd1—N1iii | 96.4 (1) | C5—C4—C3 | 118.5 (2) |
O2—Cd1—O2i | 94.7 (1) | N1—C5—C4 | 122.8 (2) |
O2—Cd1—N1ii | 152.0 (1) | O1—C6—O2 | 123.0 (3) |
O2—Cd1—N1iii | 90.0 (1) | O1—C6—C2 | 118.7 (2) |
O2i—Cd1—N1ii | 90.0 (1) | O2—C6—C2 | 118.3 (2) |
O2i—Cd1—N1iii | 152.0 (1) | C4—C3—H3 | 120.1 |
N1ii—Cd1—N1iii | 98.7 (1) | C2—C3—H3 | 120.1 |
C1—N1—C5 | 118.9 (2) | C5—C4—H4 | 120.7 |
C1—N1—Cd1v | 127.2 (2) | C3—C4—H4 | 120.7 |
C5—N1—Cd1v | 113.7 (2) | N1—C5—H5 | 118.6 |
C6—O1—Cd1 | 88.5 (2) | C4—C5—H5 | 118.6 |
| | | |
O2i—Cd1—O1—C6 | 93.0 (2) | N1—C1—C2—C6 | −177.0 (3) |
O2—Cd1—O1—C6 | −1.1 (1) | C1iv—C1—C2—C6 | 7.9 (6) |
N1ii—Cd1—O1—C6 | −176.8 (2) | C1—C2—C3—C4 | −1.0 (4) |
N1iii—Cd1—O1—C6 | −74.5 (2) | C6—C2—C3—C4 | 176.3 (2) |
O1i—Cd1—O1—C6 | 51.7 (1) | C2—C3—C4—C5 | 0.5 (4) |
O2i—Cd1—O2—C6 | −88.7 (1) | C1—N1—C5—C4 | −1.5 (4) |
N1ii—Cd1—O2—C6 | 10.1 (2) | Cd1v—N1—C5—C4 | −176.7 (2) |
N1iii—Cd1—O2—C6 | 118.9 (2) | C3—C4—C5—N1 | 0.7 (4) |
O1i—Cd1—O2—C6 | −144.7 (1) | Cd1—O1—C6—O2 | 1.9 (3) |
O1—Cd1—O2—C6 | 1.0 (1) | Cd1—O1—C6—C2 | −178.3 (2) |
C5—N1—C1—C2 | 1.0 (4) | Cd1—O2—C6—O1 | −2.0 (3) |
Cd1v—N1—C1—C2 | 175.5 (2) | Cd1—O2—C6—C2 | 178.3 (2) |
C5—N1—C1—C1iv | 176.4 (3) | C3—C2—C6—O1 | 4.0 (4) |
Cd1v—N1—C1—C1iv | −9.0 (5) | C1—C2—C6—O1 | −178.9 (3) |
N1—C1—C2—C3 | 0.2 (5) | C3—C2—C6—O2 | −176.3 (2) |
C1iv—C1—C2—C3 | −174.8 (4) | C1—C2—C6—O2 | 0.9 (4) |
Symmetry codes: (i) −y+3/2, −x+3/2, −z+3/2; (ii) x−1, y, z; (iii) −y+3/2, −x+5/2, −z+3/2; (iv) y+1/2, x−1/2, −z+3/2; (v) x+1, y, z. |
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