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Acta Cryst. (2007). E63, m2531-m2532
https://doi.org/10.1107/S1600536807043693
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Bis(1,10-phenanthroline-κ2N,N′)-bis­(cyanido-κC)cobalt(III) bis­(azido-κ1N)[1,2-bis­(pyridine-2-carboxamido)benzene-κ4N]chromate(III) monohydrate

Z.-H. Ni
The structure of the title compound, [Co(C12H8N2)2(CN)2][Cr(C18H12N4O2)(N3)2]·H2O, comprises a [CoIII(phen)2(CN)2]+ (phen = 1,10-phenanthroline) cation, a [CrIII(bpb)(N3)2]− [bpb2− = 1,2-bis­(pyridine-2-carboxamido)benzene] anion and an uncoordinated water mol­ecule. The Co and Cr ions are six-coordinated by N4C2 and N6 sets, respectively, yielding distorted octa­hedral coordination geometries. The [CoIII(phen)2(CN)2]+ and [CrIII(bpb)(N3)2]− ions and water mol­ecules are connected by π–π inter­actions [shortest distance 3.376 (2) Å] and O—H...O, O—H...N, C—H...O and C—H...N hydrogen bonds into a three-dimensional supra­molecular network structure.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807043693/hg2289sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807043693/hg2289Isup2.hkl
Contains datablock I

CCDC reference: 663595

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.055
  • wR factor = 0.162
  • Data-to-parameter ratio = 13.2

checkCIF/PLATON results

No syntax errors found




Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    N     Ueq(max)/Ueq(min) ...       3.66 Ratio


Alert level C
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT230_ALERT_2_C Hirshfeld Test Diff for    N6     -   N7      ..       5.41 su
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N4
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N7
PLAT480_ALERT_4_C Long H...A H-Bond Reported H22    ..  N5      ..       2.68 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H23    ..  O1W     ..       2.62 Ang.


Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
PLAT794_ALERT_5_G Check Predicted Bond Valency for Co          (3)       3.18
PLAT794_ALERT_5_G Check Predicted Bond Valency for Cr          (3)       3.23


   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   4 ALERT level G = General alerts; check

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check
Comment top

The crystal structures of the monomeric complexes [Cr(bpb)(H2O)(OH)] and [Cr(bpb)(H2O)(N3)] (Ni et al., 2006), [CrV(bpb)(N)] (Che et al., 1988), [CoIII(bpb)(Et)(H2O)] (Mak et al., 1991), (Et3HN)[FeIII(bpb)(Cl)2].CH3CN (Yang et al., 1991) and Na[FeIII(bpb)(N3)2] and Na[FeIII(bpb)(CN)2] (Dutta et al., 2000) contain a large in-plane pyridine carboxamide ligand bpb2-.

The monomeric complexes [Co(phen)2(CN)2].EtOH.H2O (Jian et al., 2004) and [Fe(phen)2)(CN)2].3H2O (Zhan et al., 1996) show two phen ligands and two cyanide groups. Herein, we report a new ion-pair complex [CoIII(phen)2(CN)2][CrIII(bpb)(N3)2].H2O (I) containing a large in-plane pyridine carboxamide ligand bpb2- and two phen ligands and two cyanide groups as well as two azide groups.

The geometry and labeling scheme for the crystal structure of the title complex are depicted in Figure 1. The title compound a [CoIII(phen)2(CN)2]+ cation and a [CrIII(bpb)(N3)2]- anion as well as a free water molecule. The Co(III) ion in the cation is coordinated by four nitrogen atoms from two cis phen ligands and two carbon atoms from two cis cyanide groups, giving a distorted octahedral coordination environment. The averaged Co—Nphen bond length is 1.970 (3) Å. The Co—Ccyanide bond lengths are 1.913 (4)Å for Co—C1 and 1.891 (3) for Co—C2. The two phen molecules in [CoIII(phen)2(CN)2]+ cation are nearly planar, and the two planes are almost vertical with a dihedral angle of 89.7 (1)°.

The Cr(III) ion in the anion unit [CrIII(bpb)(N3)2]- is coordinated in the equatorial plane by a large in-plane bpb2- ligand through two pyridine and two deprotonated carboxamide nitrogen atoms. The two trans positions were occupied by two azide groups. The ligand bpb2-, two azide N atoms provide a six-coordination circumstance around Cr(III) center for [CrIII(bpb)(N3)2]- unit. The C—O, Cpyridine—N, and Ccarboxy—N bond distances from bpb2- ligand in the title complex agree with those reported for other mononuclear complexes such as [CoIII(bpb)(Et)(H2O)], [FeIII(bpb)(Cl)2]- and [FeIII(bpb)(CN)2]-, which indicate these bond lengths do not vary much with the nature of central metal ion and their spin states. The average bond distances of Cr—Namide and Cr—Npyridine are 1.989 (3) Å and 2.112 (3) Å, which is in agreement with the fact that the deprotonated amide group is a very strong σ-donor.

There exist hydrogen bonds involving free water molecule and carboxamide oxygen atoms and cyanide and azide nitrogen atoms (Table 1), and π-π interactions between phen and bpb2- ligands with the shorest distance of 3.376 (2) Å, which link the [CoIII(phen)2(CN)2][CrIII(bpb)(N3)2].H2O (I) molecules into a three-dimensional supramolecular structure.

The formation mechanism of (I) is due to that Na[Cr(bpb)(N3)2] and [Cr(phen)2(CN)2]+ is more stable than precursor Na[Cr(bpb)(CN)2] in the reaction system. In addition, oxidation Co(II) is observed in this reaction system.

Related literature top

For monomeric complexes with the ligand bpb2-, see Ni et al. (2006); Che et al. (1988); for [CoIII(bpb)(Et)(H2O)] see Mak et al. (1991); Yang et al. (1991); and Dutta et al. (2000). For monomeric compounds containing two phen ligands and two cyanide groups, see Jian et al. (2004) and Zhan et al. (1996). For the synthesis of the precursor of (I), see Ni et al. (2005) and Zhong et al. (2006).

Experimental top

K[Cr(bpb)(CN)2] was synthesized according to literature (Ni et al., 2005). [Co(phen)2(Cl)2] was synthesized according to literature (Zhong et al., 2006). The title complex was prepared as follows. A methanol solution (5 ml) of [Co(phen)2(Cl)2] (97 mg, 0.2 mmol) was added to a MeOH and H2O solution (20 ml, MeOH/H2O = 4:1 v/v) of K[Cr(bpb)(CN)2] (92 mg, 0.2 mmol). Then, an aqueous solution (5 ml) of NaN3 (33 mg, 0.6 mmol) was added. The mixture was carefully filtered and the resulting solution was kept at room temperature for about two days, producing block brown crystals of (I).

Refinement top

The coordinates of the H atoms of the water molecules were found from difference Fourier maps and normalized to O—H distances of 0.85 Å. H atoms bound to C atoms were placed using the HFIX commands in SHELXL-97, with C—H distances of 0.93 Å. All H atoms were allowed for as riding atoms with Uiso(H) = 1.2Ueq(C) and 1.5Ueq(O). A value for Rint could not be determined as data processing of the title complex was based on averaged intensities of diffraction spots.

Structure description top

The crystal structures of the monomeric complexes [Cr(bpb)(H2O)(OH)] and [Cr(bpb)(H2O)(N3)] (Ni et al., 2006), [CrV(bpb)(N)] (Che et al., 1988), [CoIII(bpb)(Et)(H2O)] (Mak et al., 1991), (Et3HN)[FeIII(bpb)(Cl)2].CH3CN (Yang et al., 1991) and Na[FeIII(bpb)(N3)2] and Na[FeIII(bpb)(CN)2] (Dutta et al., 2000) contain a large in-plane pyridine carboxamide ligand bpb2-.

The monomeric complexes [Co(phen)2(CN)2].EtOH.H2O (Jian et al., 2004) and [Fe(phen)2)(CN)2].3H2O (Zhan et al., 1996) show two phen ligands and two cyanide groups. Herein, we report a new ion-pair complex [CoIII(phen)2(CN)2][CrIII(bpb)(N3)2].H2O (I) containing a large in-plane pyridine carboxamide ligand bpb2- and two phen ligands and two cyanide groups as well as two azide groups.

The geometry and labeling scheme for the crystal structure of the title complex are depicted in Figure 1. The title compound a [CoIII(phen)2(CN)2]+ cation and a [CrIII(bpb)(N3)2]- anion as well as a free water molecule. The Co(III) ion in the cation is coordinated by four nitrogen atoms from two cis phen ligands and two carbon atoms from two cis cyanide groups, giving a distorted octahedral coordination environment. The averaged Co—Nphen bond length is 1.970 (3) Å. The Co—Ccyanide bond lengths are 1.913 (4)Å for Co—C1 and 1.891 (3) for Co—C2. The two phen molecules in [CoIII(phen)2(CN)2]+ cation are nearly planar, and the two planes are almost vertical with a dihedral angle of 89.7 (1)°.

The Cr(III) ion in the anion unit [CrIII(bpb)(N3)2]- is coordinated in the equatorial plane by a large in-plane bpb2- ligand through two pyridine and two deprotonated carboxamide nitrogen atoms. The two trans positions were occupied by two azide groups. The ligand bpb2-, two azide N atoms provide a six-coordination circumstance around Cr(III) center for [CrIII(bpb)(N3)2]- unit. The C—O, Cpyridine—N, and Ccarboxy—N bond distances from bpb2- ligand in the title complex agree with those reported for other mononuclear complexes such as [CoIII(bpb)(Et)(H2O)], [FeIII(bpb)(Cl)2]- and [FeIII(bpb)(CN)2]-, which indicate these bond lengths do not vary much with the nature of central metal ion and their spin states. The average bond distances of Cr—Namide and Cr—Npyridine are 1.989 (3) Å and 2.112 (3) Å, which is in agreement with the fact that the deprotonated amide group is a very strong σ-donor.

There exist hydrogen bonds involving free water molecule and carboxamide oxygen atoms and cyanide and azide nitrogen atoms (Table 1), and π-π interactions between phen and bpb2- ligands with the shorest distance of 3.376 (2) Å, which link the [CoIII(phen)2(CN)2][CrIII(bpb)(N3)2].H2O (I) molecules into a three-dimensional supramolecular structure.

The formation mechanism of (I) is due to that Na[Cr(bpb)(N3)2] and [Cr(phen)2(CN)2]+ is more stable than precursor Na[Cr(bpb)(CN)2] in the reaction system. In addition, oxidation Co(II) is observed in this reaction system.

For monomeric complexes with the ligand bpb2-, see Ni et al. (2006); Che et al. (1988); for [CoIII(bpb)(Et)(H2O)] see Mak et al. (1991); Yang et al. (1991); and Dutta et al. (2000). For monomeric compounds containing two phen ligands and two cyanide groups, see Jian et al. (2004) and Zhan et al. (1996). For the synthesis of the precursor of (I), see Ni et al. (2005) and Zhong et al. (2006).

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Sheldrick, 1998); software used to prepare material for publication: SHELXL97 and XP (Sheldrick, 1998).

Figures top
[Figure 1] Fig. 1. A view of (I) with the unique atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level, solvate water molecules and all H atoms bonded to C atoms are omitted.
[Figure 2] Fig. 2. A stereoview of part of the crystal structure of (I) along a axis, showing two-dimensional supramolecular structure through π-π interactions and hydrogen bonds.
Bis(1,10-phenanthroline-κ2N,N')- bis(cyanido-κC)cobalt(III) bis(azido-κ1N)[1,2-bis(pyridine-2-carboxamido)benzene- κ4N]chromate(III) monohydrate top
Crystal data top
[Co(C12H8N2)2(CN)2][Cr(C18H12N4O2)(N3)2]·H2OF(000) = 1924
Mr = 941.77Dx = 1.560 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7868 reflections
a = 12.488 (3) Åθ = 3.1–26.0°
b = 20.633 (4) ŵ = 0.75 mm−1
c = 16.152 (3) ÅT = 293 K
β = 105.51 (3)°Block, brown
V = 4010.2 (14) Å30.12 × 0.08 × 0.06 mm
Z = 4
Data collection top
Bruker APEXII CCD area-detector
diffractometer		7868 independent reflections
Radiation source: fine-focus sealed tube6341 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
φ and ω scansθmax = 26.0°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		h = −15→15
Tmin = 0.932, Tmax = 0.955k = −22→25
14094 measured reflectionsl = −19→19
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.162H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.1216P)2]
where P = (Fo2 + 2Fc2)/3
7868 reflections(Δ/σ)max < 0.001
594 parametersΔρmax = 0.72 e Å−3
0 restraintsΔρmin = −0.85 e Å−3
Crystal data top
[Co(C12H8N2)2(CN)2][Cr(C18H12N4O2)(N3)2]·H2OV = 4010.2 (14) Å3
Mr = 941.77Z = 4
Monoclinic, P21/cMo Kα radiation
a = 12.488 (3) ŵ = 0.75 mm−1
b = 20.633 (4) ÅT = 293 K
c = 16.152 (3) Å0.12 × 0.08 × 0.06 mm
β = 105.51 (3)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer		7868 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		6341 reflections with I > 2σ(I)
Tmin = 0.932, Tmax = 0.955Rint = 0.046
14094 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0550 restraints
wR(F2) = 0.162H-atom parameters constrained
S = 1.08Δρmax = 0.72 e Å−3
7868 reflectionsΔρmin = −0.85 e Å−3
594 parameters
Special details top

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 (Å2) top
xyzUiso*/Ueq
Co0.48482 (3)0.43739 (2)0.26435 (3)0.03403 (15)
Cr0.04038 (4)0.31652 (2)0.78682 (3)0.02753 (14)
N160.4510 (2)0.36270 (12)0.18250 (16)0.0355 (6)
N140.4596 (2)0.49881 (12)0.16649 (16)0.0340 (6)
N130.3268 (2)0.45023 (13)0.25147 (18)0.0387 (6)
N150.6384 (2)0.42009 (12)0.26441 (16)0.0345 (6)
C20.5214 (3)0.50586 (15)0.3448 (2)0.0363 (7)
C440.3497 (3)0.51591 (15)0.13662 (19)0.0375 (7)
C310.6473 (2)0.36849 (14)0.21268 (18)0.0320 (6)
C260.7494 (3)0.29169 (16)0.1469 (2)0.0422 (8)
H260.81630.27680.13910.051*
C250.6524 (3)0.26162 (16)0.1057 (2)0.0413 (7)
H250.65430.22620.07050.050*
C320.5461 (3)0.33708 (14)0.16906 (18)0.0326 (6)
C270.7491 (3)0.34638 (15)0.2023 (2)0.0375 (7)
C420.2629 (3)0.42475 (17)0.2973 (2)0.0485 (9)
H420.29540.39990.34550.058*
C430.2782 (3)0.48836 (16)0.1827 (2)0.0402 (7)
C330.5317 (3)0.52480 (15)0.1277 (2)0.0378 (7)
H330.60660.51420.14750.045*
C300.7311 (3)0.45073 (15)0.3062 (2)0.0381 (7)
H300.72610.48580.34120.046*
C390.1631 (3)0.50154 (19)0.1558 (2)0.0497 (9)
C10.5089 (3)0.38246 (17)0.3630 (2)0.0477 (8)
C360.3083 (3)0.55698 (17)0.0659 (2)0.0455 (8)
C240.5466 (3)0.28377 (15)0.11573 (19)0.0359 (7)
C340.4979 (3)0.56720 (16)0.0586 (2)0.0442 (8)
H340.55020.58480.03350.053*
N20.5447 (2)0.54653 (14)0.39523 (18)0.0439 (7)
C210.3543 (3)0.33494 (17)0.1426 (2)0.0431 (8)
H210.28910.35170.15140.052*
C220.3479 (3)0.28153 (17)0.0882 (2)0.0457 (8)
H220.27900.26370.06140.055*
C230.4426 (3)0.25524 (16)0.0740 (2)0.0428 (8)
H230.43870.21960.03800.051*
C280.8464 (3)0.37959 (16)0.2482 (2)0.0442 (8)
H280.91590.36640.24390.053*
C290.8367 (3)0.43134 (17)0.2990 (2)0.0471 (8)
H290.89990.45380.32870.057*
C400.0974 (3)0.4723 (2)0.2051 (3)0.0601 (11)
H400.02090.47870.19040.072*
C410.1474 (3)0.4346 (2)0.2741 (3)0.0568 (10)
H410.10440.41530.30630.068*
C350.3872 (3)0.58321 (17)0.0271 (2)0.0484 (8)
H350.36470.6112−0.01950.058*
N10.5321 (3)0.35124 (16)0.4228 (2)0.0646 (10)
C370.1908 (3)0.5694 (2)0.0390 (2)0.0575 (10)
H370.16160.5957−0.00840.069*
C380.1223 (3)0.5429 (2)0.0825 (3)0.0594 (11)
H380.04660.55180.06420.071*
O10.16269 (17)0.41625 (10)0.61221 (13)0.0341 (5)
N100.04882 (19)0.37818 (11)0.69427 (15)0.0287 (5)
N90.2114 (2)0.30820 (11)0.79160 (16)0.0318 (5)
C14−0.1470 (2)0.38842 (13)0.68146 (17)0.0285 (6)
C9−0.0538 (2)0.40809 (14)0.65158 (18)0.0284 (6)
C70.2385 (2)0.34648 (13)0.73176 (18)0.0293 (6)
O2−0.28973 (18)0.33717 (12)0.78485 (15)0.0425 (5)
N30.0139 (2)0.23662 (13)0.71132 (18)0.0389 (6)
C10−0.0714 (2)0.45191 (13)0.58276 (18)0.0303 (6)
H10−0.01180.46580.56300.036*
N12−0.0250 (2)0.26168 (12)0.87107 (15)0.0326 (5)
N11−0.11798 (19)0.34461 (12)0.75174 (15)0.0298 (5)
C80.1444 (2)0.38425 (13)0.67296 (18)0.0296 (6)
C13−0.2535 (2)0.41110 (15)0.64024 (19)0.0335 (6)
H13−0.31410.39740.65890.040*
N60.0900 (2)0.38274 (14)0.88251 (17)0.0421 (6)
N40.0581 (2)0.21842 (14)0.65907 (18)0.0432 (7)
C15−0.1905 (2)0.32277 (15)0.79499 (19)0.0333 (6)
C60.3468 (3)0.35121 (15)0.72515 (19)0.0350 (7)
H60.36310.37710.68300.042*
C30.2934 (3)0.27424 (16)0.8455 (2)0.0393 (7)
H30.27520.24710.88570.047*
C16−0.1345 (2)0.27401 (14)0.86214 (18)0.0336 (6)
N70.1550 (3)0.42476 (17)0.8833 (2)0.0571 (9)
C17−0.1936 (3)0.24049 (17)0.9103 (2)0.0422 (8)
H17−0.26830.24960.90410.051*
C50.4312 (3)0.31656 (15)0.7828 (2)0.0381 (7)
H50.50450.31960.77990.046*
C40.4039 (3)0.27792 (16)0.8437 (2)0.0422 (8)
H40.45850.25470.88300.051*
C200.0263 (3)0.21634 (16)0.9270 (2)0.0408 (7)
H200.10130.20840.93300.049*
C19−0.0279 (3)0.18087 (17)0.9763 (2)0.0450 (8)
H190.00970.14951.01440.054*
C18−0.1399 (3)0.19328 (17)0.9675 (2)0.0460 (8)
H18−0.17840.17010.99970.055*
N50.0992 (4)0.1979 (2)0.6088 (3)0.0848 (13)
N80.2144 (4)0.4691 (2)0.8828 (3)0.1045 (18)
O1W0.2765 (2)0.36408 (11)0.49069 (15)0.0454 (5)
C11−0.1783 (3)0.47473 (15)0.54393 (18)0.0346 (7)
H11−0.18900.50420.49890.042*
C12−0.2696 (3)0.45383 (15)0.57176 (19)0.0369 (7)
H12−0.34060.46850.54440.044*
H1A0.23840.37540.52450.055*
H1B0.34190.37970.50700.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0382 (3)0.0328 (2)0.0358 (2)−0.00662 (17)0.01811 (18)−0.00425 (17)
Cr0.0251 (2)0.0305 (3)0.0292 (2)−0.00140 (17)0.01109 (18)0.00460 (18)
N160.0385 (14)0.0345 (13)0.0386 (13)−0.0076 (11)0.0190 (11)−0.0037 (11)
N140.0363 (14)0.0340 (13)0.0362 (13)−0.0057 (11)0.0172 (11)−0.0071 (11)
N130.0411 (15)0.0392 (14)0.0408 (14)−0.0081 (12)0.0196 (12)−0.0100 (12)
N150.0372 (14)0.0311 (13)0.0360 (13)−0.0010 (11)0.0110 (11)−0.0017 (11)
C20.0354 (16)0.0374 (17)0.0406 (16)−0.0035 (13)0.0179 (13)−0.0024 (14)
C440.0414 (17)0.0373 (17)0.0373 (16)0.0017 (14)0.0163 (13)−0.0095 (13)
C310.0371 (16)0.0285 (14)0.0319 (14)0.0027 (12)0.0119 (12)0.0022 (12)
C260.0405 (18)0.0386 (17)0.0471 (18)0.0119 (14)0.0108 (14)−0.0020 (15)
C250.0492 (19)0.0315 (16)0.0421 (17)0.0089 (14)0.0103 (14)−0.0022 (13)
C320.0386 (16)0.0311 (15)0.0307 (14)−0.0013 (12)0.0135 (12)0.0003 (12)
C270.0359 (17)0.0321 (16)0.0421 (17)0.0058 (13)0.0062 (13)0.0023 (13)
C420.060 (2)0.0448 (19)0.052 (2)−0.0142 (16)0.0351 (18)−0.0120 (16)
C430.0412 (17)0.0460 (18)0.0397 (17)−0.0044 (14)0.0219 (14)−0.0168 (14)
C330.0409 (17)0.0364 (16)0.0409 (17)−0.0079 (13)0.0190 (14)−0.0041 (14)
C300.0363 (17)0.0360 (16)0.0406 (17)−0.0036 (13)0.0079 (13)−0.0056 (13)
C390.0413 (19)0.058 (2)0.054 (2)0.0003 (16)0.0204 (16)−0.0227 (18)
C10.063 (2)0.0397 (19)0.047 (2)−0.0150 (16)0.0257 (17)−0.0051 (16)
C360.053 (2)0.0433 (19)0.0416 (18)0.0054 (16)0.0148 (15)−0.0090 (15)
C240.0448 (18)0.0330 (16)0.0309 (14)−0.0031 (13)0.0117 (13)0.0001 (12)
C340.058 (2)0.0417 (18)0.0406 (18)−0.0042 (16)0.0269 (16)−0.0042 (15)
N20.0464 (17)0.0456 (16)0.0440 (16)−0.0035 (13)0.0197 (13)−0.0026 (14)
C210.0381 (18)0.0483 (19)0.0466 (19)−0.0076 (15)0.0176 (15)−0.0053 (16)
C220.0455 (19)0.048 (2)0.0469 (18)−0.0153 (16)0.0173 (15)−0.0131 (16)
C230.056 (2)0.0361 (17)0.0396 (17)−0.0096 (15)0.0184 (15)−0.0060 (14)
C280.0334 (17)0.0446 (19)0.0526 (19)0.0062 (14)0.0078 (14)−0.0045 (15)
C290.0375 (18)0.046 (2)0.055 (2)−0.0030 (15)0.0063 (16)−0.0113 (16)
C400.0376 (19)0.073 (3)0.076 (3)−0.0107 (19)0.0267 (19)−0.038 (2)
C410.054 (2)0.060 (2)0.067 (3)−0.0208 (19)0.035 (2)−0.024 (2)
C350.070 (2)0.0411 (18)0.0382 (17)0.0057 (17)0.0218 (17)−0.0002 (15)
N10.093 (3)0.0475 (19)0.0525 (19)−0.0193 (18)0.0174 (18)−0.0004 (16)
C370.056 (2)0.069 (3)0.046 (2)0.021 (2)0.0112 (18)−0.0079 (18)
C380.0367 (19)0.077 (3)0.063 (2)0.0106 (18)0.0106 (17)−0.027 (2)
O10.0360 (11)0.0369 (11)0.0349 (11)−0.0014 (9)0.0189 (9)0.0054 (9)
N100.0267 (12)0.0304 (12)0.0309 (12)−0.0008 (9)0.0110 (9)0.0023 (10)
N90.0294 (13)0.0319 (13)0.0352 (13)−0.0026 (10)0.0106 (10)0.0033 (10)
C140.0329 (15)0.0298 (14)0.0252 (13)0.0008 (12)0.0120 (11)−0.0017 (11)
C90.0310 (15)0.0281 (14)0.0294 (13)0.0021 (11)0.0134 (11)−0.0017 (11)
C70.0278 (14)0.0268 (14)0.0343 (14)−0.0040 (11)0.0101 (11)−0.0023 (12)
O20.0334 (12)0.0527 (13)0.0472 (13)0.0067 (10)0.0208 (10)0.0123 (11)
N30.0340 (14)0.0373 (14)0.0526 (16)−0.0067 (11)0.0243 (12)−0.0050 (12)
C100.0366 (16)0.0276 (14)0.0305 (14)0.0016 (12)0.0153 (12)−0.0005 (12)
N120.0307 (13)0.0356 (13)0.0328 (12)−0.0024 (10)0.0106 (10)0.0048 (11)
N110.0288 (12)0.0320 (13)0.0306 (12)−0.0002 (10)0.0113 (10)0.0053 (10)
C80.0337 (15)0.0272 (14)0.0303 (14)−0.0039 (12)0.0129 (11)−0.0007 (11)
C130.0293 (15)0.0373 (16)0.0352 (15)0.0010 (12)0.0109 (12)−0.0018 (13)
N60.0441 (16)0.0480 (16)0.0390 (14)−0.0097 (13)0.0194 (12)−0.0063 (12)
N40.0390 (15)0.0460 (16)0.0477 (16)0.0054 (12)0.0170 (13)0.0062 (13)
C150.0300 (15)0.0383 (16)0.0339 (15)−0.0003 (12)0.0128 (12)−0.0004 (12)
C60.0365 (16)0.0349 (16)0.0377 (15)−0.0053 (13)0.0173 (13)−0.0011 (13)
C30.0351 (17)0.0405 (18)0.0425 (17)0.0016 (13)0.0104 (13)0.0080 (14)
C160.0352 (16)0.0359 (16)0.0331 (15)−0.0024 (13)0.0148 (12)0.0030 (12)
N70.0446 (17)0.071 (2)0.065 (2)−0.0131 (17)0.0302 (15)−0.0287 (17)
C170.0376 (18)0.050 (2)0.0448 (18)0.0018 (14)0.0212 (14)0.0090 (15)
C50.0278 (15)0.0432 (18)0.0456 (17)−0.0015 (13)0.0135 (13)−0.0069 (14)
C40.0361 (17)0.0414 (18)0.0469 (18)0.0063 (14)0.0073 (14)0.0031 (15)
C200.0374 (17)0.0465 (19)0.0399 (16)−0.0008 (14)0.0128 (14)0.0102 (15)
C190.049 (2)0.0461 (19)0.0403 (17)−0.0002 (15)0.0119 (15)0.0161 (15)
C180.050 (2)0.049 (2)0.0466 (19)−0.0047 (15)0.0276 (16)0.0150 (16)
N50.089 (3)0.112 (3)0.069 (2)0.039 (3)0.048 (2)0.004 (2)
N80.093 (3)0.113 (4)0.136 (4)−0.061 (3)0.079 (3)−0.073 (3)
O1W0.0485 (14)0.0441 (13)0.0477 (13)0.0022 (11)0.0203 (11)−0.0017 (10)
C110.0463 (18)0.0303 (15)0.0280 (14)0.0059 (13)0.0113 (12)0.0036 (12)
C120.0377 (17)0.0380 (17)0.0356 (16)0.0071 (13)0.0107 (13)−0.0018 (13)
Geometric parameters (Å, º) top
Co—C21.891 (3)C28—H280.9300
Co—C11.913 (4)C29—H290.9300
Co—N131.946 (3)C40—C411.366 (6)
Co—N151.951 (3)C40—H400.9300
Co—N141.984 (3)C41—H410.9300
Co—N162.001 (3)C35—H350.9300
Cr—N101.987 (2)C37—C381.359 (6)
Cr—N111.992 (2)C37—H370.9300
Cr—N32.024 (3)C38—H380.9300
Cr—N62.032 (3)O1—C81.254 (3)
Cr—N122.096 (2)N10—C81.333 (4)
Cr—N92.123 (3)N10—C91.423 (4)
N16—C211.336 (4)N9—C31.350 (4)
N16—C321.370 (4)N9—C71.359 (4)
N14—C331.340 (4)C14—C131.399 (4)
N14—C441.373 (4)C14—N111.420 (4)
N13—C421.333 (4)C14—C91.433 (4)
N13—C431.364 (4)C9—C101.404 (4)
N15—C301.333 (4)C7—C61.388 (4)
N15—C311.376 (4)C7—C81.514 (4)
C2—N21.152 (4)O2—C151.242 (4)
C44—C361.405 (5)N3—N41.187 (4)
C44—C431.426 (4)C10—C111.396 (4)
C31—C271.402 (4)C10—H100.9300
C31—C321.427 (4)N12—C201.339 (4)
C26—C251.366 (5)N12—C161.360 (4)
C26—C271.441 (4)N11—C151.360 (4)
C26—H260.9300C13—C121.387 (4)
C25—C241.447 (5)C13—H130.9300
C25—H250.9300N6—N71.186 (4)
C32—C241.398 (4)N4—N51.152 (4)
C27—C281.420 (4)C15—C161.507 (4)
C42—C411.405 (6)C6—C51.402 (4)
C42—H420.9300C6—H60.9300
C43—C391.411 (5)C3—C41.389 (5)
C33—C341.392 (5)C3—H30.9300
C33—H330.9300C16—C171.392 (4)
C30—C291.413 (5)N7—N81.179 (5)
C30—H300.9300C17—C181.386 (5)
C39—C401.422 (6)C17—H170.9300
C39—C381.439 (6)C5—C41.379 (5)
C1—N11.132 (5)C5—H50.9300
C36—C351.409 (5)C4—H40.9300
C36—C371.438 (5)C20—C191.384 (4)
C24—C231.422 (4)C20—H200.9300
C34—C351.380 (5)C19—C181.392 (5)
C34—H340.9300C19—H190.9300
C21—C221.398 (5)C18—H180.9300
C21—H210.9300O1W—H1A0.8472
C22—C231.375 (5)O1W—H1B0.8517
C22—H220.9300C11—C121.401 (4)
C23—H230.9300C11—H110.9300
C28—C291.371 (5)C12—H120.9300
C2—Co—C185.12 (14)C24—C23—H23120.8
C2—Co—N1391.34 (12)C29—C28—C27119.2 (3)
C1—Co—N1395.68 (14)C29—C28—H28120.4
C2—Co—N1594.57 (12)C27—C28—H28120.4
C1—Co—N1587.44 (14)C28—C29—C30120.3 (3)
N13—Co—N15173.54 (11)C28—C29—H29119.9
C2—Co—N1491.60 (12)C30—C29—H29119.9
C1—Co—N14176.61 (12)C41—C40—C39119.5 (4)
N13—Co—N1483.53 (11)C41—C40—H40120.2
N15—Co—N1493.67 (11)C39—C40—H40120.2
C2—Co—N16177.62 (13)C40—C41—C42120.8 (4)
C1—Co—N1693.01 (13)C40—C41—H41119.6
N13—Co—N1690.31 (11)C42—C41—H41119.6
N15—Co—N1683.87 (11)C34—C35—C36119.6 (3)
N14—Co—N1690.29 (10)C34—C35—H35120.2
N10—Cr—N1181.26 (10)C36—C35—H35120.2
N10—Cr—N395.81 (10)C38—C37—C36120.3 (4)
N11—Cr—N394.33 (11)C38—C37—H37119.9
N10—Cr—N694.30 (11)C36—C37—H37119.9
N11—Cr—N695.64 (11)C37—C38—C39122.1 (3)
N3—Cr—N6166.76 (12)C37—C38—H38119.0
N10—Cr—N12160.45 (10)C39—C38—H38119.0
N11—Cr—N1279.19 (10)C8—N10—C9125.9 (2)
N3—Cr—N1285.53 (10)C8—N10—Cr119.05 (19)
N6—Cr—N1287.81 (10)C9—N10—Cr114.84 (18)
N10—Cr—N979.86 (10)C3—N9—C7118.0 (3)
N11—Cr—N9161.12 (10)C3—N9—Cr130.4 (2)
N3—Cr—N987.54 (10)C7—N9—Cr111.50 (19)
N6—Cr—N985.85 (11)C13—C14—N11126.9 (3)
N12—Cr—N9119.69 (10)C13—C14—C9120.0 (3)
C21—N16—C32117.9 (3)N11—C14—C9113.1 (2)
C21—N16—Co130.7 (2)C10—C9—N10126.4 (3)
C32—N16—Co111.3 (2)C10—C9—C14118.7 (3)
C33—N14—C44117.8 (3)N10—C9—C14114.9 (2)
C33—N14—Co130.2 (2)N9—C7—C6121.9 (3)
C44—N14—Co112.0 (2)N9—C7—C8116.5 (2)
C42—N13—C43118.4 (3)C6—C7—C8121.6 (3)
C42—N13—Co128.9 (3)N4—N3—Cr130.8 (2)
C43—N13—Co112.6 (2)C11—C10—C9120.1 (3)
C30—N15—C31118.4 (3)C11—C10—H10120.0
C30—N15—Co129.3 (2)C9—C10—H10120.0
C31—N15—Co112.3 (2)C20—N12—C16119.3 (3)
N2—C2—Co178.4 (3)C20—N12—Cr128.0 (2)
N14—C44—C36123.8 (3)C16—N12—Cr112.65 (18)
N14—C44—C43114.9 (3)C15—N11—C14124.0 (2)
C36—C44—C43121.3 (3)C15—N11—Cr120.28 (19)
N15—C31—C27123.2 (3)C14—N11—Cr115.74 (18)
N15—C31—C32116.6 (3)O1—C8—N10128.0 (3)
C27—C31—C32120.3 (3)O1—C8—C7119.2 (3)
C25—C26—C27120.5 (3)N10—C8—C7112.8 (2)
C25—C26—H26119.7C12—C13—C14120.6 (3)
C27—C26—H26119.7C12—C13—H13119.7
C26—C25—C24121.3 (3)C14—C13—H13119.7
C26—C25—H25119.3N7—N6—Cr124.6 (2)
C24—C25—H25119.3N5—N4—N3176.9 (4)
N16—C32—C24123.3 (3)O2—C15—N11129.1 (3)
N16—C32—C31115.9 (3)O2—C15—C16120.6 (3)
C24—C32—C31120.8 (3)N11—C15—C16110.3 (2)
C31—C27—C28117.3 (3)C7—C6—C5119.3 (3)
C31—C27—C26118.9 (3)C7—C6—H6120.4
C28—C27—C26123.9 (3)C5—C6—H6120.4
N13—C42—C41121.4 (4)N9—C3—C4123.0 (3)
N13—C42—H42119.3N9—C3—H3118.5
C41—C42—H42119.3C4—C3—H3118.5
N13—C43—C39123.9 (3)N12—C16—C17121.1 (3)
N13—C43—C44116.7 (3)N12—C16—C15117.5 (2)
C39—C43—C44119.4 (3)C17—C16—C15121.3 (3)
N14—C33—C34121.9 (3)N8—N7—N6176.0 (5)
N14—C33—H33119.0C18—C17—C16119.2 (3)
C34—C33—H33119.0C18—C17—H17120.4
N15—C30—C29121.8 (3)C16—C17—H17120.4
N15—C30—H30119.1C4—C5—C6118.9 (3)
C29—C30—H30119.1C4—C5—H5120.6
C43—C39—C40116.0 (4)C6—C5—H5120.6
C43—C39—C38118.4 (3)C5—C4—C3118.9 (3)
C40—C39—C38125.6 (3)C5—C4—H4120.6
N1—C1—Co174.4 (4)C3—C4—H4120.6
C44—C36—C35116.4 (3)N12—C20—C19122.6 (3)
C44—C36—C37118.5 (3)N12—C20—H20118.7
C35—C36—C37125.1 (3)C19—C20—H20118.7
C32—C24—C23117.6 (3)C20—C19—C18118.5 (3)
C32—C24—C25118.2 (3)C20—C19—H19120.8
C23—C24—C25124.2 (3)C18—C19—H19120.8
C35—C34—C33120.4 (3)C17—C18—C19119.4 (3)
C35—C34—H34119.8C17—C18—H18120.3
C33—C34—H34119.8C19—C18—H18120.3
N16—C21—C22122.2 (3)H1A—O1W—H1B110.7
N16—C21—H21118.9C10—C11—C12121.0 (3)
C22—C21—H21118.9C10—C11—H11119.5
C23—C22—C21120.5 (3)C12—C11—H11119.5
C23—C22—H22119.7C13—C12—C11119.7 (3)
C21—C22—H22119.7C13—C12—H12120.1
C22—C23—C24118.4 (3)C11—C12—H12120.1
C22—C23—H23120.8
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1A···O10.852.082.919 (2)171
O1W—H1B···N2i0.852.373.095 (2)143
C4—H4···N1ii0.932.393.194 (5)144
C21—H21···N5iii0.932.503.158 (6)128
C22—H22···N5iii0.932.683.239 (6)120
C23—H23···O1Wiii0.932.623.268 (2)128
C26—H26···N3iv0.932.453.240 (5)143
C30—H30···O1i0.932.453.177 (3)135
C33—H33···N8i0.932.443.223 (6)142
C38—H38···N6v0.932.503.241 (5)137
C42—H42···O1W0.932.533.327 (2)144
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, −y+1/2, z+1/2; (iii) x, −y+1/2, z−1/2; (iv) x+1, −y+1/2, z−1/2; (v) −x, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula[Co(C12H8N2)2(CN)2][Cr(C18H12N4O2)(N3)2]·H2O
Mr941.77
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)12.488 (3), 20.633 (4), 16.152 (3)
β (°) 105.51 (3)
V (Å3)4010.2 (14)
Z4
Radiation typeMo Kα
µ (mm−1)0.75
Crystal size (mm)0.12 × 0.08 × 0.06
Data collection
DiffractometerBruker APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.932, 0.955
No. of measured, independent and
observed [I > 2σ(I)] reflections		14094, 7868, 6341
Rint0.046
(sin θ/λ)max (Å−1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.055, 0.162, 1.08
No. of reflections7868
No. of parameters594
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.72, −0.85

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97 and XP (Sheldrick, 1998).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1A···O10.8472.0802.919 (2)170.84
O1W—H1B···N2i0.8522.3713.095 (2)143.26
C4—H4···N1ii0.9312.3923.194 (5)144.36
C21—H21···N5iii0.9302.5043.158 (6)127.56
C22—H22···N5iii0.9292.6793.239 (6)119.48
C23—H23···O1Wiii0.9312.6153.268 (2)127.68
C26—H26···N3iv0.9302.4473.240 (5)143.22
C30—H30···O1i0.9312.4543.177 (3)134.62
C33—H33···N8i0.9302.4373.223 (6)142.16
C38—H38···N6v0.9302.5023.241 (5)136.52
C42—H42···O1W0.9302.5293.327 (2)144.03
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, −y+1/2, z+1/2; (iii) x, −y+1/2, z−1/2; (iv) x+1, −y+1/2, z−1/2; (v) −x, −y+1, −z+1.
 

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