Literature DB >> 22807741

3-Amino-pyridinium trans-diaqua-dioxalato-chromate(III).

Ichraf Chérif1, Mohamed Faouzi Zid, Malika El-Ghozzi, Daniel Avignant.   

Abstract

In the structure of the title compound, (C₅H₇N₂)[Cr(C₂O₄)₂(H₂O)₂], two crystallographically independent formula units are present. Both chromium atoms are six-coordinated in a distorted octa-hedral geometry by two chelating equatorial oxalato ligands and two axial water mol-ecules. The [Cr(C₂O₄)₂(H₂O)₂]⁻ anions and C₅H₇N₂ ⁺ cations are linked through a complex three-dimensional hydrogen-bonding network consisting of N-H⋯O and O-H⋯O inter-actions.

Entities:  

Year:  2012        PMID： 22807741      PMCID： PMC3393173          DOI： 10.1107/S1600536812025020

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For the versatility of the oxalato ligand, see: Hernández-Molina et al. (2001 ▶); Martak et al. (2009 ▶); Marinescu et al. (2011 ▶). For magnetic studies of oxalatochromium (III) complexes, see: Chen et al. (2005 ▶); Marinescu et al. (2011 ▶). For complexes containing the [Cr(C2O4)2(H2O)2]− motif com­pleted by various uncoordinated cations including quinolin­ium, 4-dimethyl­amino­pyridinium and 4-amino­pyridinium, see: Bélombé et al. (2009 ▶); Nenwa et al. (2010 ▶); Chérif et al. (2011 ▶).

Experimental

Crystal data

(C5H7N2)[Cr(C2O4)2(H2O)2] M = 359.20 Monoclinic, a = 7.3901 (15) Å b = 17.586 (4) Å c = 20.995 (5) Å β = 107.941 (11)° V = 2596.0 (10) Å3 Z = 8 Mo Kα radiation μ = 0.94 mm−1 T = 296 K 0.53 × 0.33 × 0.19 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.695, T max = 0.835 22038 measured reflections 5865 independent reflections 4091 reflections with I > 2σ(I) R int = 0.036

Refinement

R[F 2 > 2σ(F 2)] = 0.039 wR(F 2) = 0.112 S = 1.04 5865 reflections 421 parameters 12 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.68 e Å−3 Δρmin = −0.42 e Å−3 Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1998 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812025020/vn2039sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812025020/vn2039Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C5H7N2)[Cr(C2O4)2(H2O)2]F(000) = 1464
Mr = 359.20Dx = 1.838 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5082 reflections
a = 7.3901 (15) Åθ = 3.0–27.3°
b = 17.586 (4) ŵ = 0.94 mm−1
c = 20.995 (5) ÅT = 296 K
β = 107.941 (11)°Prism, violet
V = 2596.0 (10) Å30.53 × 0.33 × 0.19 mm
Z = 8
Bruker APEXII CCD diffractometer5865 independent reflections
Radiation source: fine-focus sealed tube4091 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
φ and ω scansθmax = 27.5°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Bruker, 2008)h = −9→9
Tmin = 0.695, Tmax = 0.835k = −22→22
22038 measured reflectionsl = −24→27
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.112H atoms treated by a mixture of independent and constrained refinement
S = 1.04w = 1/[σ2(Fo2) + (0.0522P)2 + 1.1562P] where P = (Fo2 + 2Fc2)/3
5865 reflections(Δ/σ)max = 0.001
421 parametersΔρmax = 0.68 e Å−3
12 restraintsΔρmin = −0.42 e Å−3
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles
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.
xyzUiso*/Ueq
Cr10.86991 (5)0.39632 (2)0.387432 (18)0.02059 (12)
O111.1473 (2)0.39735 (10)0.44297 (9)0.0262 (4)
H1111.205 (4)0.3619 (12)0.4303 (12)0.039*
H2111.160 (4)0.3939 (15)0.4838 (6)0.039*
O120.5955 (2)0.39686 (10)0.33227 (8)0.0265 (4)
H1120.531 (3)0.3644 (13)0.3449 (12)0.040*
H2120.575 (4)0.3931 (16)0.2906 (5)0.040*
O130.8080 (2)0.33173 (10)0.45283 (8)0.0252 (4)
O140.9080 (2)0.29864 (10)0.34754 (8)0.0276 (4)
O150.9201 (2)0.46853 (10)0.32268 (8)0.0255 (4)
O160.8323 (2)0.48926 (10)0.43257 (8)0.0252 (4)
O170.8865 (3)0.17386 (11)0.36410 (10)0.0379 (5)
O180.8431 (3)0.61488 (10)0.42415 (9)0.0320 (4)
O190.7775 (3)0.21093 (10)0.47675 (9)0.0359 (5)
O200.9095 (3)0.59268 (10)0.30172 (9)0.0304 (4)
C110.8736 (3)0.24077 (15)0.37920 (12)0.0252 (6)
C120.8138 (3)0.26020 (14)0.44180 (12)0.0228 (5)
C130.8984 (3)0.53796 (14)0.33634 (12)0.0223 (5)
C140.8543 (3)0.55075 (14)0.40331 (12)0.0228 (5)
Cr20.37874 (5)0.07363 (2)0.386675 (19)0.02155 (12)
O210.1084 (3)0.07383 (10)0.32683 (9)0.0272 (4)
H1210.103 (4)0.0772 (16)0.2865 (6)0.041*
H2210.036 (3)0.1047 (13)0.3372 (12)0.041*
O220.6505 (3)0.07089 (10)0.44535 (8)0.0259 (4)
H1220.663 (4)0.0556 (14)0.4848 (7)0.039*
H2220.704 (4)0.1132 (9)0.4470 (13)0.039*
O230.3433 (2)−0.02304 (9)0.42779 (8)0.0258 (4)
O240.4379 (2)0.00638 (10)0.31981 (8)0.0270 (4)
O250.3026 (2)0.13247 (10)0.45248 (8)0.0263 (4)
O260.4174 (2)0.17523 (10)0.35243 (9)0.0288 (4)
O270.3779 (3)0.29802 (11)0.37330 (10)0.0385 (5)
O280.4338 (3)−0.11727 (10)0.29469 (8)0.0315 (4)
O290.2676 (3)0.25175 (11)0.48140 (10)0.0375 (5)
O300.3577 (3)−0.14718 (10)0.41233 (9)0.0404 (5)
C210.3098 (3)0.20509 (15)0.44561 (13)0.0252 (6)
C220.3738 (3)0.22954 (15)0.38542 (13)0.0267 (6)
C230.4178 (3)−0.06459 (15)0.33022 (11)0.0227 (5)
C240.3688 (3)−0.08241 (14)0.39500 (12)0.0246 (6)
N110.1544 (4)0.41533 (17)0.06676 (15)0.0610 (8)
H11A0.17250.39510.03190.073*
H11B0.15200.46400.07040.073*
N120.1098 (3)0.24902 (15)0.15746 (14)0.0446 (6)
H120.11310.20060.15240.053*
C10.1011 (4)0.39996 (18)0.17377 (15)0.0418 (8)
H10.09670.45220.17990.050*
C20.0795 (5)0.3528 (2)0.22143 (17)0.0523 (9)
H20.06360.37320.26020.063*
C30.0805 (4)0.27507 (19)0.21400 (16)0.0485 (8)
H30.06190.24230.24620.058*
C40.1338 (4)0.29243 (18)0.10945 (16)0.0402 (8)
H40.15320.27020.07190.048*
C50.1303 (4)0.37163 (18)0.11460 (15)0.0396 (7)
N210.3221 (4)0.56454 (17)0.44750 (14)0.0603 (8)
H21A0.30770.58870.48120.072*
H21B0.31700.51570.44640.072*
N220.3907 (3)0.71990 (14)0.34738 (13)0.0405 (6)
H220.39520.76870.34990.049*
C60.3605 (4)0.68177 (17)0.39823 (15)0.0359 (7)
H60.34500.70800.43460.043*
C70.4141 (4)0.68807 (19)0.29359 (16)0.0454 (8)
H70.43400.71730.25950.055*
C80.4078 (4)0.6097 (2)0.28982 (15)0.0464 (8)
H80.42360.58530.25260.056*
C90.3789 (4)0.56839 (17)0.34007 (16)0.0412 (7)
H90.37670.51560.33700.049*
C100.3523 (4)0.60299 (17)0.39666 (15)0.0350 (7)
U11U22U33U12U13U23
Cr10.0306 (2)0.0155 (2)0.0179 (2)−0.00071 (16)0.01067 (16)0.00029 (15)
O110.0333 (10)0.0199 (10)0.0251 (9)0.0027 (8)0.0085 (8)−0.0015 (7)
O120.0326 (10)0.0269 (10)0.0212 (9)−0.0032 (8)0.0100 (8)0.0025 (8)
O130.0388 (10)0.0196 (9)0.0211 (9)−0.0010 (8)0.0149 (8)−0.0010 (7)
O140.0389 (10)0.0231 (10)0.0253 (9)−0.0014 (8)0.0163 (8)−0.0023 (8)
O150.0373 (10)0.0200 (10)0.0227 (9)0.0000 (8)0.0144 (8)0.0008 (7)
O160.0383 (10)0.0201 (9)0.0206 (9)0.0001 (8)0.0142 (8)−0.0006 (7)
O170.0400 (11)0.0233 (11)0.0496 (12)0.0021 (9)0.0129 (9)−0.0104 (9)
O180.0489 (11)0.0189 (10)0.0288 (10)0.0010 (8)0.0128 (9)−0.0030 (8)
O190.0536 (12)0.0226 (10)0.0324 (11)−0.0083 (9)0.0148 (9)0.0037 (8)
O200.0459 (11)0.0210 (10)0.0247 (10)−0.0048 (8)0.0116 (8)0.0041 (8)
C110.0212 (13)0.0257 (15)0.0268 (13)−0.0005 (11)0.0043 (10)−0.0032 (11)
C120.0237 (12)0.0203 (14)0.0224 (12)−0.0013 (10)0.0041 (10)0.0004 (10)
C130.0232 (12)0.0211 (13)0.0210 (12)−0.0027 (10)0.0046 (10)0.0002 (10)
C140.0247 (13)0.0206 (14)0.0204 (12)0.0005 (10)0.0030 (10)0.0001 (10)
Cr20.0317 (2)0.0164 (2)0.0186 (2)0.00061 (16)0.01077 (17)0.00100 (15)
O210.0335 (10)0.0263 (10)0.0230 (9)0.0036 (8)0.0102 (8)−0.0026 (8)
O220.0352 (10)0.0178 (9)0.0247 (9)−0.0015 (8)0.0092 (8)0.0025 (7)
O230.0392 (10)0.0200 (10)0.0212 (9)−0.0015 (8)0.0139 (8)−0.0004 (7)
O240.0387 (10)0.0258 (10)0.0208 (9)0.0008 (8)0.0157 (8)0.0000 (7)
O250.0385 (10)0.0197 (9)0.0233 (9)0.0011 (8)0.0133 (8)0.0005 (7)
O260.0370 (10)0.0247 (10)0.0273 (10)0.0011 (8)0.0138 (8)0.0069 (8)
O270.0391 (11)0.0206 (10)0.0539 (13)−0.0015 (9)0.0114 (10)0.0111 (9)
O280.0457 (11)0.0267 (11)0.0231 (9)0.0063 (8)0.0119 (8)−0.0056 (8)
O290.0495 (12)0.0260 (11)0.0393 (11)0.0064 (9)0.0168 (9)−0.0068 (9)
O300.0722 (14)0.0195 (11)0.0342 (11)−0.0016 (10)0.0234 (10)0.0006 (8)
C210.0230 (13)0.0220 (14)0.0275 (13)0.0017 (11)0.0032 (10)−0.0010 (11)
C220.0233 (13)0.0239 (14)0.0298 (14)0.0007 (11)0.0037 (11)0.0053 (11)
C230.0256 (13)0.0244 (14)0.0168 (12)0.0034 (10)0.0045 (10)0.0009 (10)
C240.0312 (14)0.0198 (14)0.0224 (13)−0.0002 (11)0.0077 (11)−0.0013 (10)
N110.091 (2)0.0408 (17)0.063 (2)−0.0057 (16)0.0408 (18)−0.0036 (15)
N120.0458 (15)0.0305 (14)0.0538 (17)0.0036 (12)0.0100 (13)−0.0005 (13)
C10.0465 (18)0.0302 (16)0.0490 (19)0.0060 (14)0.0154 (15)−0.0161 (14)
C20.057 (2)0.058 (2)0.047 (2)0.0019 (18)0.0239 (16)−0.0090 (17)
C30.0514 (19)0.045 (2)0.047 (2)0.0028 (16)0.0122 (16)−0.0084 (16)
C40.0322 (15)0.0386 (19)0.0459 (18)0.0040 (13)0.0063 (13)−0.0226 (15)
C50.0374 (16)0.0363 (18)0.0443 (18)0.0008 (13)0.0113 (14)0.0005 (14)
N210.087 (2)0.0436 (18)0.065 (2)−0.0002 (15)0.0444 (17)0.0071 (15)
N220.0423 (14)0.0288 (14)0.0484 (16)−0.0035 (11)0.0108 (12)−0.0017 (12)
C60.0349 (15)0.0326 (17)0.0402 (17)0.0000 (13)0.0114 (13)−0.0127 (13)
C70.0472 (18)0.051 (2)0.0379 (18)−0.0001 (16)0.0129 (15)0.0033 (15)
C80.0449 (18)0.060 (2)0.0375 (18)0.0007 (16)0.0169 (14)−0.0205 (16)
C90.0388 (17)0.0286 (16)0.056 (2)0.0046 (13)0.0140 (15)−0.0146 (15)
C100.0307 (15)0.0317 (16)0.0446 (18)0.0006 (12)0.0143 (13)−0.0036 (13)
Cr1—O112.0223 (18)O22—H1220.848 (16)
Cr1—O122.0017 (17)O22—H2220.84 (2)
Cr1—O131.9421 (17)N11—C51.320 (4)
Cr1—O141.9690 (18)N12—C31.351 (4)
Cr1—O151.9771 (18)N12—C41.319 (4)
Cr1—O161.9517 (18)N11—H11B0.8600
Cr2—O212.006 (2)N11—H11A0.8600
Cr2—O222.007 (2)N12—H120.8600
Cr2—O231.9604 (17)N21—C101.339 (4)
Cr2—O241.9846 (18)N22—C61.336 (4)
Cr2—O251.9429 (17)N22—C71.319 (4)
Cr2—O261.9793 (18)N21—H21A0.8600
O13—C121.282 (3)N21—H21B0.8600
O14—C111.283 (3)N22—H220.8600
O15—C131.276 (3)C11—C121.548 (3)
O16—C141.279 (3)C13—C141.554 (3)
O17—C111.230 (3)C21—C221.541 (4)
O18—C141.222 (3)C23—C241.544 (3)
O19—C121.218 (3)C1—C21.347 (5)
O20—C131.224 (3)C1—C51.415 (4)
O11—H2110.835 (13)C2—C31.376 (5)
O11—H1110.84 (3)C4—C51.398 (4)
O12—H2120.843 (11)C1—H10.9300
O12—H1120.84 (2)C2—H20.9300
O23—C241.296 (3)C3—H30.9300
O24—C231.284 (3)C4—H40.9300
O25—C211.288 (3)C6—C101.387 (4)
O26—C221.278 (3)C7—C81.380 (5)
O27—C221.233 (3)C8—C91.351 (4)
O28—C231.218 (3)C9—C101.402 (4)
O29—C211.216 (3)C6—H60.9300
O30—C241.206 (3)C7—H70.9300
O21—H1210.837 (15)C8—H80.9300
O21—H2210.84 (2)C9—H90.9300
Cr1···O28i3.7984 (19)O19···H1222.88 (3)
Cr2···O193.829 (2)O19···H6ii2.7100
Cr1···H21Aii3.4100O19···H2221.852 (18)
Cr1···H2iii3.4200O19···H4vi2.9000
O11···O142.824 (3)O20···H12i2.1600
O11···O152.855 (2)O20···H121i1.846 (15)
O11···O132.825 (2)O20···H3i2.8500
O11···O27iii3.103 (3)O21···H1xi2.6000
O11···O29iii2.749 (3)O22···H11Bv2.4600
O11···N21iii3.201 (4)O23···H1222.68 (3)
O11···C143.398 (3)O23···H122vii1.937 (17)
O11···O162.787 (2)O24···H8v2.5000
O11···O18iv2.777 (3)O24···H1212.66 (3)
O11···C14iv3.358 (3)O25···H11Aix2.2200
O12···O272.684 (3)O25···H1222.88 (3)
O12···O142.822 (2)O25···H2212.65 (2)
O12···O152.772 (2)O26···H1212.88 (3)
O12···O132.781 (2)O26···H2222.65 (3)
O12···O28i2.619 (2)O27···H1121.85 (2)
O12···C113.389 (3)O27···H111viii2.30 (3)
O12···C123.374 (3)O28···H212v1.781 (13)
O12···C133.325 (3)O28···H22x2.3800
O12···C143.384 (3)O29···H211viii2.63 (3)
O12···O162.805 (2)O29···H4ix2.3400
O13···C112.376 (3)O29···H111viii2.19 (2)
O13···O122.781 (2)O30···H22x2.0500
O13···O18iv3.178 (3)O30···H6x2.6000
O13···O142.603 (2)O30···H122vii2.74 (2)
O13···O162.817 (3)N11···O22i3.139 (4)
O13···O273.158 (3)N11···C23i3.254 (4)
O13···N21ii3.142 (3)N11···C24i3.364 (4)
O13···O112.825 (2)N11···O25xii3.047 (4)
O14···O132.603 (2)N12···O20v2.896 (3)
O14···C122.389 (3)N12···O18v2.998 (3)
O14···O122.822 (2)N21···O11viii3.201 (4)
O14···O153.039 (3)N21···C13viii3.312 (4)
O14···O112.824 (3)N21···C14viii3.301 (4)
O14···C2iii3.405 (4)N21···O13ii3.142 (3)
O15···C2iii3.405 (4)N21···O16ii3.211 (3)
O15···O122.772 (2)N22···O30xiii2.755 (3)
O15···O112.855 (2)N22···O28xiii3.121 (3)
O15···C142.388 (3)C1···O28i3.308 (4)
O15···O162.608 (2)C1···O30xiv3.417 (4)
O15···O143.039 (3)C1···C24xiv3.339 (4)
O16···C132.380 (3)C2···O273.410 (4)
O16···O112.787 (2)C2···O15viii3.405 (4)
O16···N21ii3.211 (3)C2···O14viii3.405 (4)
O16···O122.805 (2)C3···O273.413 (4)
O16···O16iv3.159 (2)C3···O20v3.228 (4)
O16···O152.608 (2)C4···O18v3.217 (4)
O16···O132.817 (3)C4···O19xv3.191 (4)
O17···O25iii3.149 (3)C4···O29xii3.232 (4)
O17···O21iii2.681 (3)C5···O28i3.204 (4)
O17···O192.800 (3)C5···C23i3.372 (4)
O17···C21iii3.117 (3)C6···O30xiii3.023 (4)
O17···C7v3.380 (4)C6···O29ii3.321 (4)
O18···O13iv3.178 (3)C7···O17i3.380 (4)
O18···O11iv2.777 (3)C8···O24i3.394 (4)
O18···O202.789 (3)C8···C143.577 (4)
O18···C4i3.217 (4)C9···C143.366 (4)
O18···N12i2.998 (3)C9···C13viii3.568 (4)
O19···O263.164 (3)C9···O20viii3.338 (4)
O19···O222.646 (3)C10···O20viii3.270 (4)
O19···C223.027 (3)C10···C13viii3.398 (4)
O19···C213.315 (3)C11···O29iii3.045 (3)
O19···C4vi3.191 (4)C11···C21iii3.156 (3)
O19···O172.800 (3)C12···C223.145 (3)
O19···O30vii3.019 (3)C12···O263.309 (3)
O19···Cr23.829 (2)C12···O29iii3.200 (3)
O20···N12i2.896 (3)C12···O273.168 (3)
O20···O21i2.682 (3)C13···N21iii3.312 (4)
O20···C3i3.228 (4)C13···C10iii3.398 (4)
O20···O182.789 (3)C13···C9iii3.568 (4)
O20···C10iii3.270 (4)C14···O11iv3.358 (3)
O20···C9iii3.338 (4)C14···C93.366 (4)
O21···C243.407 (3)C14···C83.577 (4)
O21···O20v2.682 (3)C14···N21iii3.301 (4)
O21···C233.325 (3)C21···C11viii3.156 (3)
O21···O17viii2.681 (3)C21···O30vii3.385 (3)
O21···O252.784 (3)C21···O193.315 (3)
O21···O242.753 (3)C21···O17viii3.117 (3)
O21···O232.853 (3)C22···C123.145 (3)
O21···C213.388 (3)C22···O193.027 (3)
O21···O262.816 (3)C23···C5v3.372 (4)
O21···C223.372 (3)C23···N11v3.254 (4)
O22···O232.739 (3)C24···C1xi3.339 (4)
O22···C243.371 (3)C24···N11v3.364 (4)
O22···O262.841 (3)C24···O22vii3.405 (3)
O22···C24vii3.405 (3)C11···H221iii2.93 (2)
O22···N11v3.139 (4)C12···H1123.04 (2)
O22···O192.646 (3)C12···H2222.722 (18)
O22···O252.836 (3)C13···H121i2.667 (16)
O22···O23vii2.780 (2)C13···H12i2.8700
O22···O242.855 (2)C14···H12i2.9200
O23···O242.622 (2)C14···H211iv2.594 (17)
O23···O22vii2.780 (2)C21···H2213.09 (2)
O23···O222.739 (3)C21···H11Aix2.9200
O23···C232.393 (3)C21···H111viii2.86 (2)
O23···O252.817 (2)C22···H1122.88 (2)
O23···O212.853 (3)C22···H111viii2.93 (2)
O24···O212.753 (3)C23···H22x2.9700
O24···O263.062 (3)C23···H212v2.660 (15)
O24···C242.385 (3)C24···H122vii2.648 (18)
O24···C8v3.394 (4)C24···H22x2.8100
O24···O232.622 (2)H1···H11B2.4600
O24···O222.855 (2)H1···O21xiv2.6000
O25···N11ix3.047 (4)H2···O15viii2.5500
O25···O212.784 (3)H2···O14viii2.7800
O25···O30vii3.168 (3)H2···Cr1viii3.4200
O25···O232.817 (2)H3···O20v2.8500
O25···O222.836 (3)H3···O14viii2.8800
O25···O262.607 (2)H4···O18v2.7300
O25···O17viii3.149 (3)H4···H11A2.3700
O25···C222.373 (3)H4···O29xii2.3400
O26···O222.841 (3)H4···O19xv2.9000
O26···O252.607 (2)H6···H21A2.3700
O26···O243.062 (3)H6···O30xiii2.6000
O26···C212.386 (3)H6···O19ii2.7100
O26···O193.164 (3)H8···O24i2.5000
O26···O212.816 (3)H9···H21B2.4700
O26···C123.309 (3)H9···O122.6600
O27···C33.413 (4)H11A···H42.3700
O27···C123.168 (3)H11A···O25xii2.2200
O27···O133.158 (3)H11A···C21xii2.9200
O27···O292.760 (3)H11B···O22i2.4600
O27···O122.684 (3)H11B···H12.4600
O27···C23.410 (4)H12···C13v2.8700
O27···O11viii3.103 (3)H12···C14v2.9200
O28···O302.748 (3)H12···O18v2.3000
O28···C5v3.204 (4)H12···O20v2.1600
O28···O12v2.619 (2)H21A···Cr1ii3.4100
O28···N22x3.121 (3)H21A···O16ii2.7200
O28···Cr1v3.7984 (19)H21A···O13ii2.3100
O28···C1v3.308 (4)H21A···H62.3700
O29···C6ii3.321 (4)H21B···H92.4700
O29···C12viii3.200 (3)H21B···O11viii2.4200
O29···C11viii3.045 (3)H22···O30xiii2.0500
O29···C4ix3.232 (4)H22···C23xiii2.9700
O29···O272.760 (3)H22···O28xiii2.3800
O29···O11viii2.749 (3)H22···C24xiii2.8100
O30···O19vii3.019 (3)H111···C21iii2.86 (2)
O30···O282.748 (3)H111···C22iii2.93 (2)
O30···C1xi3.417 (4)H111···O29iii2.19 (2)
O30···N22x2.755 (3)H111···O27iii2.30 (3)
O30···C21vii3.385 (3)H112···O271.85 (2)
O30···O25vii3.168 (3)H112···C123.04 (2)
O30···C6x3.023 (4)H112···C222.88 (2)
O11···H21Biii2.4200H121···O20v1.846 (14)
O12···H92.6600H121···C13v2.667 (16)
O13···H21Aii2.3100H122···O30vii2.74 (2)
O13···H2112.71 (3)H122···C24vii2.648 (18)
O13···H1122.61 (2)H122···O192.88 (3)
O14···H2122.90 (3)H122···O23vii1.937 (18)
O14···H1112.59 (3)H211···C14iv2.594 (17)
O14···H3iii2.8800H211···O29iii2.63 (3)
O14···H2iii2.7800H211···O18iv1.946 (15)
O15···H2122.77 (3)H211···O16iv2.69 (2)
O15···H2iii2.5500H212···O28i1.781 (13)
O16···H2112.87 (3)H212···C23i2.660 (15)
O16···H211iv2.69 (2)H221···C11viii2.93 (2)
O16···H21Aii2.7200H221···C213.09 (2)
O17···H221iii1.85 (2)H221···O17viii1.85 (2)
O17···H2222.73 (3)H222···C122.722 (18)
O18···H12i2.3000H222···O172.73 (3)
O18···H211iv1.946 (15)H222···O191.852 (18)
O18···H4i2.7300
O11—Cr1—O12179.21 (7)H21A—N21—H21B120.00
O11—Cr1—O1390.88 (7)C10—N21—H21A120.00
O11—Cr1—O1490.04 (7)C7—N22—H22118.00
O11—Cr1—O1591.10 (7)C6—N22—H22118.00
O11—Cr1—O1689.04 (7)O17—C11—C12119.7 (2)
O12—Cr1—O1389.69 (7)O14—C11—O17125.6 (2)
O12—Cr1—O1490.58 (7)O14—C11—C12114.8 (2)
O12—Cr1—O1588.30 (7)O13—C12—C11113.8 (2)
O12—Cr1—O1690.37 (7)O19—C12—C11121.9 (2)
O13—Cr1—O1483.46 (7)O13—C12—O19124.3 (2)
O13—Cr1—O15175.36 (7)O15—C13—C14114.7 (2)
O13—Cr1—O1692.68 (7)O15—C13—O20125.7 (2)
O14—Cr1—O15100.73 (7)O20—C13—C14119.6 (2)
O14—Cr1—O16176.02 (7)O16—C14—C13113.9 (2)
O15—Cr1—O1683.16 (7)O16—C14—O18125.2 (2)
O23—Cr2—O2483.29 (7)O18—C14—C13120.9 (2)
O23—Cr2—O2592.38 (7)O25—C21—C22113.7 (2)
O23—Cr2—O26175.27 (7)O25—C21—O29124.9 (2)
O24—Cr2—O25174.57 (7)O29—C21—C22121.4 (2)
O24—Cr2—O26101.13 (7)O27—C22—C21118.4 (2)
O25—Cr2—O2683.30 (7)O26—C22—O27126.3 (2)
O22—Cr2—O2491.32 (7)O26—C22—C21115.4 (2)
O21—Cr2—O22178.47 (8)O28—C23—C24118.6 (2)
O21—Cr2—O2392.00 (7)O24—C23—C24114.7 (2)
O21—Cr2—O2487.24 (7)O24—C23—O28126.7 (2)
O21—Cr2—O2589.64 (7)O23—C24—C23114.6 (2)
O21—Cr2—O2689.90 (7)O23—C24—O30124.5 (2)
O22—Cr2—O2387.31 (7)O30—C24—C23120.9 (2)
O22—Cr2—O2591.75 (7)C2—C1—C5121.4 (3)
O22—Cr2—O2690.89 (7)C1—C2—C3121.4 (3)
Cr1—O13—C12114.70 (15)N12—C3—C2116.4 (3)
Cr1—O14—C11113.24 (15)N12—C4—C5120.5 (3)
Cr1—O15—C13113.39 (15)C1—C5—C4115.5 (3)
Cr1—O16—C14114.63 (15)N11—C5—C1123.8 (3)
Cr1—O11—H211111 (2)N11—C5—C4120.8 (3)
H111—O11—H211111 (3)C2—C1—H1119.00
Cr1—O11—H111109.4 (18)C5—C1—H1119.00
H112—O12—H212110 (3)C1—C2—H2119.00
Cr1—O12—H212115 (2)C3—C2—H2119.00
Cr1—O12—H112112.8 (16)C2—C3—H3122.00
Cr2—O23—C24113.81 (15)N12—C3—H3122.00
Cr2—O24—C23113.37 (14)C5—C4—H4120.00
Cr2—O25—C21114.67 (15)N12—C4—H4120.00
Cr2—O26—C22112.90 (16)N22—C6—C10119.9 (3)
H121—O21—H221113 (3)N22—C7—C8117.5 (3)
Cr2—O21—H221115.6 (16)C7—C8—C9120.2 (3)
Cr2—O21—H121111 (2)C8—C9—C10121.7 (3)
H122—O22—H222109 (2)N21—C10—C9123.9 (3)
Cr2—O22—H122113 (2)C6—C10—C9115.9 (3)
Cr2—O22—H222112.0 (18)N21—C10—C6120.2 (3)
C3—N12—C4124.8 (3)N22—C6—H6120.00
H11A—N11—H11B120.00C10—C6—H6120.00
C5—N11—H11A120.00N22—C7—H7121.00
C5—N11—H11B120.00C8—C7—H7121.00
C4—N12—H12118.00C7—C8—H8120.00
C3—N12—H12118.00C9—C8—H8120.00
C6—N22—C7124.7 (3)C8—C9—H9119.00
C10—N21—H21B120.00C10—C9—H9119.00
O11—Cr1—O13—C12−91.40 (16)Cr2—O23—C24—C23−1.1 (2)
O12—Cr1—O13—C1289.16 (16)Cr2—O23—C24—O30178.4 (2)
O14—Cr1—O13—C12−1.46 (16)Cr2—O24—C23—O28175.3 (2)
O16—Cr1—O13—C12179.52 (16)Cr2—O24—C23—C24−4.8 (2)
O11—Cr1—O14—C1192.22 (16)Cr2—O25—C21—C221.2 (2)
O12—Cr1—O14—C11−88.28 (16)Cr2—O25—C21—O29179.8 (2)
O13—Cr1—O14—C111.34 (16)Cr2—O26—C22—C212.5 (3)
O15—Cr1—O14—C11−176.66 (15)Cr2—O26—C22—O27−177.3 (2)
O11—Cr1—O15—C13−91.84 (16)C3—N12—C4—C50.1 (5)
O12—Cr1—O15—C1387.64 (16)C4—N12—C3—C2−1.2 (5)
O14—Cr1—O15—C13177.91 (15)C7—N22—C6—C100.1 (5)
O16—Cr1—O15—C13−2.94 (16)C6—N22—C7—C8−0.3 (5)
O11—Cr1—O16—C1491.27 (16)O17—C11—C12—O19−0.5 (4)
O12—Cr1—O16—C14−88.20 (16)O14—C11—C12—O13−0.2 (3)
O13—Cr1—O16—C14−177.90 (16)O17—C11—C12—O13179.1 (2)
O15—Cr1—O16—C140.05 (16)O14—C11—C12—O19−179.7 (2)
O25—Cr2—O26—C22−1.51 (16)O15—C13—C14—O18175.1 (2)
O21—Cr2—O23—C2485.88 (16)O20—C13—C14—O18−4.9 (4)
O22—Cr2—O23—C24−92.75 (16)O15—C13—C14—O16−4.9 (3)
O24—Cr2—O23—C24−1.11 (15)O20—C13—C14—O16175.1 (2)
O25—Cr2—O23—C24175.60 (16)O25—C21—C22—O26−2.5 (3)
O21—Cr2—O24—C23−88.89 (16)O29—C21—C22—O26178.8 (2)
O22—Cr2—O24—C2390.59 (16)O29—C21—C22—O27−1.4 (4)
O23—Cr2—O24—C233.45 (15)O25—C21—C22—O27177.2 (2)
O26—Cr2—O24—C23−178.25 (15)O28—C23—C24—O304.4 (4)
O21—Cr2—O25—C21−89.89 (16)O28—C23—C24—O23−176.1 (2)
O22—Cr2—O25—C2190.74 (16)O24—C23—C24—O30−175.5 (2)
O23—Cr2—O25—C21178.12 (16)O24—C23—C24—O234.0 (3)
O26—Cr2—O25—C210.05 (17)C5—C1—C2—C3−1.5 (5)
O21—Cr2—O26—C2288.14 (17)C2—C1—C5—C40.3 (5)
O22—Cr2—O26—C22−93.17 (17)C2—C1—C5—N11−179.2 (3)
O24—Cr2—O26—C22175.31 (16)C1—C2—C3—N121.9 (5)
Cr1—O13—C12—C111.3 (2)N12—C4—C5—N11179.9 (3)
Cr1—O13—C12—O19−179.2 (2)N12—C4—C5—C10.4 (4)
Cr1—O14—C11—C12−1.0 (2)N22—C6—C10—N21180.0 (3)
Cr1—O14—C11—O17179.8 (2)N22—C6—C10—C90.5 (4)
Cr1—O15—C13—O20−175.2 (2)N22—C7—C8—C9−0.1 (5)
Cr1—O15—C13—C144.8 (2)C7—C8—C9—C100.8 (5)
Cr1—O16—C14—C132.4 (2)C8—C9—C10—N21179.6 (3)
Cr1—O16—C14—O18−177.6 (2)C8—C9—C10—C6−1.0 (5)
D—H···AD—HH···AD···AD—H···A
N11—H11A···O25xii0.862.223.047 (4)161
N11—H11B···O22i0.862.463.139 (4)136
N12—H12···O18v0.862.302.998 (3)139
N12—H12···O20v0.862.162.896 (3)144
N21—H21A···O13ii0.862.313.142 (3)163
N21—H21B···O11viii0.862.423.201 (4)151
N22—H22···O28xiii0.862.383.121 (3)145
N22—H22···O30xiii0.862.052.755 (3)138
O11—H111···O27iii0.84 (3)2.30 (3)3.103 (3)161 (2)
O11—H111···O29iii0.84 (3)2.19 (2)2.749 (3)123 (2)
O11—H211···O18iv0.84 (1)1.95 (2)2.777 (3)173 (3)
O12—H112···O270.84 (2)1.85 (2)2.684 (3)176 (2)
O12—H212···O28i0.84 (1)1.78 (1)2.619 (2)172 (3)
O21—H121···O20v0.84 (2)1.85 (1)2.682 (3)176 (3)
O21—H221···O17viii0.84 (2)1.85 (2)2.681 (3)177 (2)
O22—H122···O23vii0.85 (2)1.94 (2)2.780 (2)173 (3)
O22—H222···O190.84 (2)1.85 (2)2.646 (3)157 (3)
Table 1

Selected bond lengths (Å)

Cr1—O112.0223 (18)
Cr1—O122.0017 (17)
Cr1—O131.9421 (17)
Cr1—O141.9690 (18)
Cr1—O151.9771 (18)
Cr1—O161.9517 (18)
Cr2—O212.006 (2)
Cr2—O222.007 (2)
Cr2—O231.9604 (17)
Cr2—O241.9846 (18)
Cr2—O251.9429 (17)
Cr2—O261.9793 (18)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
N11—H11A⋯O25i 0.862.223.047 (4)161
N11—H11B⋯O22ii 0.862.463.139 (4)136
N12—H12⋯O18iii 0.862.302.998 (3)139
N12—H12⋯O20iii 0.862.162.896 (3)144
N21—H21A⋯O13iv 0.862.313.142 (3)163
N21—H21B⋯O11v 0.862.423.201 (4)151
N22—H22⋯O28vi 0.862.383.121 (3)145
N22—H22⋯O30vi 0.862.052.755 (3)138
O11—H111⋯O27vii 0.84 (3)2.30 (3)3.103 (3)161 (2)
O11—H111⋯O29vii 0.84 (3)2.19 (2)2.749 (3)123 (2)
O11—H211⋯O18viii 0.84 (1)1.95 (2)2.777 (3)173 (3)
O12—H112⋯O270.84 (2)1.85 (2)2.684 (3)176 (2)
O12—H212⋯O28ii 0.84 (1)1.78 (1)2.619 (2)172 (3)
O21—H121⋯O20iii 0.84 (2)1.85 (1)2.682 (3)176 (3)
O21—H221⋯O17v 0.84 (2)1.85 (2)2.681 (3)177 (2)
O22—H122⋯O23ix 0.85 (2)1.94 (2)2.780 (2)173 (3)
O22—H222⋯O190.84 (2)1.85 (2)2.646 (3)157 (3)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

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