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Acta Cryst. (2007). E63, m2049-m2050
https://doi.org/10.1107/S1600536807031789
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Hexakis{μ2-4-[2-(diisopropyl­amino)ethyl­amino]pent-3-en-2-onato-κ3N,O:O}tricalcium(II) hexane solvate

P. Richard, M. Eleter, L. G. Hubert-Pfalzgraf and S. Daniele
The title compound, [Ca3(C13H25N2O)6]·C6H14, is a trinuclear complex with all Ca atoms presenting octa­hedral coordination. The central Ca atom (as well as the hexane solvent mol­ecule) is located on a crystallographic twofold rotation axis and is coordinated by six bridging O atoms, with Ca—O distances ranging from 2.344 (1) to 2.351 (1) Å. The terminal Ca atoms are coordinated by three bridging O atoms, with Ca—O distances ranging from 2.311 (1) to 2.335 (1) Å, and three N atoms of the β-ketoiminate ligands, with Ca—N distances ranging from 2.432 (1) to 2.452 (1) Å. One of the diisopropylamino groups is disordered over two positions, with site occipancy factors of ca 0.54 and 0.46.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807031789/dn2209sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807031789/dn2209Isup2.hkl
Contains datablock I

CCDC reference: 657524

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 110 K
  • Mean [sigma](C-C) = 0.002 Å
  • Disorder in main residue
  • R factor = 0.041
  • wR factor = 0.105
  • Data-to-parameter ratio = 19.5

checkCIF/PLATON results

No syntax errors found




Alert level C
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.60 Ratio
PLAT301_ALERT_3_C Main Residue  Disorder .........................      12.00 Perc.
PLAT410_ALERT_2_C Short Intra H...H Contact  H7A    ..  H11X    ..       1.94 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          3
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      12.20 Deg.
              N2X  -C7   -N2      1.555   1.555   1.555


Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......         14


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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 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
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check
Comment top

The title compound was obtained by reaction between the Ca silylamide Ca[N(SiMe3)2]2(THF)2 (Westerhausen, 1991) and the ketoimine. Its solid state structure is similar to that of the strontium derivative. However, 1H NMR data in solution (CDCl3 or C6D6) show the presence of two different molecular species. In concentrated solution (1.4 M in CDCl3), one specie accounts for about 90% of the resonances while the amount of the second specie increases by dilution. These data suggest an equilibrium between a trinuclear form (I) having the solid state structure and a dimeric structure which could be similar to that reported for a tetrakis(β-ketoiminate)di-magnesium (Corazza et al., 1988).

In the title compound (I), the Ca atoms are hexacoordinated. The ketoiminate ligands are linked to the two terminal Ca atoms in a "three blades propeller" mode while the central Ca atom is bonded to the six bridging oxygen atoms of the six ligands and exhibits a distorded trigonal antiprismatic geometry. This coordination scheme is similar to that reported for the Sr analog (Pasko et al., 2005). An other very similar coordination scheme was also reported for a trimagnesium compound linked to a slightly different β-ketoiminate ligand (Matthews et al., 2005). For the terminal Ca atoms, the Ca—N distances [Ca1—N1 2.4323 (12), Ca1—N3 2.4522 (12) and Ca1—N5 2.4510 (12) Å] are in good agreement with those observed for the few β-ketoiminate known (Sanchez et al., 2002; Sarazin et al., 2006 & Westerhausen et al., 2003) while, due to the bridging nature of the O atoms, the Ca—O distances [Ca1—O1 2.335 (1), Ca1—O2 2.311 (1) and Ca1—O3 2.314 (1) Å] are longer than those reported. The Ca—O distances for the central Ca atom [Ca2—O1 2.344 (1), Ca2—O2 2.349 (1) & Ca2—O3 2.351 (1) Å] are in good agreement with those observed for bridging O atoms (see for example Deacon et al., 2004).

Related literature top

For related literature, see: Corazza et al. (1988); Deacon et al. (2004); Matthews et al. (2005); Pasko et al. (2005); Sanchez et al. (2002); Sarazin et al. (2006); Westerhausen (1991); Westerhausen et al. (2003).

Experimental top

Synthesis of calcium 4-(2-diisopropylamino-ethylamino)-pent-3-en-2-onate [CaLiPr2]3. A solution of 885 mg (3.91 mmol) of 4-(2-diisopropylamino-ethylamino)-pent-3-en-2-one in 2 ml of hexane was added to 989 mg (1.96 mmol) of Ca[N(SiMe3)2]2(THF)2 in 10 ml of hexane. After stirring for 24 h at rt, concentration gave a white crystalline solid (648 mg, 68%). FT—IR (cm-1): 1618m (νC=O); 1589m, 1578 s, 1517m (νC=C); 498 s (νCa=N). 1H NMR (250 MHz, CDCl3); 1.01 [d, 72H, Me(iPr), 3 J = 6.65 Hz); 1.92, 1.99 [s, 36H, Me(acac)]; 2.59 (t, 12H, CH2—NiPr2, 3 J = 7.43 Hz); 3.00 [sep, 12H, CH(iPr)), 3 J = 6.71 Hz]; 3.2 [t, 12H, CH2—N(acac)]; 4.94 [s, 6H, CH(acac)] for B; 0.90 [d, 72H, Me(iPr), 3 J = 6.47 Hz); 1.73, 1.85 [s, 36H, Me(acac)]; 2.33 (t, 12H, CH2—NiPr2, 3 J = 5.84 Hz); 2.88 [sep, 12H, CH(iPr), 3 J = 6.64 Hz]; 3.22 [t, 12H, CH2—N(acac)]; 4.54 [s, 6H, CH(acac)] for (I).

Refinement top

The complex as well as the solvate molecule are located on a twofold axis and only the half of these molecules are present in the asymetric unit. One of the di(isopropyl)-amino groups was found to be disordered over two positions [occupancies: 0.537:0.463]. The lenghts of equivalent bonds in both components of the disordered groups were restrained to be similar during refinement. All H atoms were placed in idealized positions (C—H=0.93 to 0.98 Å) and refined using a riding model [Uiso(H)=1.2Ueq(CH, CH2) and 1.5Ueq(CH3)]. Torsion angles of the methyl groups attached to sp2 C were refined.

Structure description top

The title compound was obtained by reaction between the Ca silylamide Ca[N(SiMe3)2]2(THF)2 (Westerhausen, 1991) and the ketoimine. Its solid state structure is similar to that of the strontium derivative. However, 1H NMR data in solution (CDCl3 or C6D6) show the presence of two different molecular species. In concentrated solution (1.4 M in CDCl3), one specie accounts for about 90% of the resonances while the amount of the second specie increases by dilution. These data suggest an equilibrium between a trinuclear form (I) having the solid state structure and a dimeric structure which could be similar to that reported for a tetrakis(β-ketoiminate)di-magnesium (Corazza et al., 1988).

In the title compound (I), the Ca atoms are hexacoordinated. The ketoiminate ligands are linked to the two terminal Ca atoms in a "three blades propeller" mode while the central Ca atom is bonded to the six bridging oxygen atoms of the six ligands and exhibits a distorded trigonal antiprismatic geometry. This coordination scheme is similar to that reported for the Sr analog (Pasko et al., 2005). An other very similar coordination scheme was also reported for a trimagnesium compound linked to a slightly different β-ketoiminate ligand (Matthews et al., 2005). For the terminal Ca atoms, the Ca—N distances [Ca1—N1 2.4323 (12), Ca1—N3 2.4522 (12) and Ca1—N5 2.4510 (12) Å] are in good agreement with those observed for the few β-ketoiminate known (Sanchez et al., 2002; Sarazin et al., 2006 & Westerhausen et al., 2003) while, due to the bridging nature of the O atoms, the Ca—O distances [Ca1—O1 2.335 (1), Ca1—O2 2.311 (1) and Ca1—O3 2.314 (1) Å] are longer than those reported. The Ca—O distances for the central Ca atom [Ca2—O1 2.344 (1), Ca2—O2 2.349 (1) & Ca2—O3 2.351 (1) Å] are in good agreement with those observed for bridging O atoms (see for example Deacon et al., 2004).

For related literature, see: Corazza et al. (1988); Deacon et al. (2004); Matthews et al. (2005); Pasko et al. (2005); Sanchez et al. (2002); Sarazin et al. (2006); Westerhausen (1991); Westerhausen et al. (2003).

Computing details top

Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO–SMN (Otwinowski & Minor, 1997); data reduction: DENZO–SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. Molecular view of (I) with the atom labelling scheme. Ellipsoids are drawn at the 30% probability level. Forclarity, the hexane solvate molecule is not shown and only one component of the disordered diethyl amino group is shown.[Symmetry code: (i) -x, y, -z + 1/2]
Hexakis{µ2-4-[2-(diisopropylamino)ethylamino]pent-3-en-2-onato- κ3N,O:O}tricalcium(II) hexane solvate top
Crystal data top
[Ca3(C13H25N2O)6]·C6H14F(000) = 3440
Mr = 1558.51Dx = 1.099 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 9659 reflections
a = 24.1444 (3) Åθ = 1–27.5°
b = 15.3089 (2) ŵ = 0.23 mm−1
c = 26.6679 (5) ÅT = 110 K
β = 107.132 (1)°Prism, colourless
V = 9419.7 (3) Å30.3 × 0.3 × 0.25 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer		8196 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.035
Graphite monochromatorθmax = 27.5°, θmin = 2.1°
φ scans (κ = 0) + additional ω scansh = −30→30
19153 measured reflectionsk = −19→18
10664 independent reflectionsl = −34→34
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0458P)2 + 5.2682P]
where P = (Fo2 + 2Fc2)/3
10664 reflections(Δ/σ)max = 0.001
547 parametersΔρmax = 0.21 e Å−3
14 restraintsΔρmin = −0.23 e Å−3
Crystal data top
[Ca3(C13H25N2O)6]·C6H14V = 9419.7 (3) Å3
Mr = 1558.51Z = 4
Monoclinic, C2/cMo Kα radiation
a = 24.1444 (3) ŵ = 0.23 mm−1
b = 15.3089 (2) ÅT = 110 K
c = 26.6679 (5) Å0.3 × 0.3 × 0.25 mm
β = 107.132 (1)°
Data collection top
Nonius KappaCCD
diffractometer		8196 reflections with I > 2σ(I)
19153 measured reflectionsRint = 0.035
10664 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04114 restraints
wR(F2) = 0.105H-atom parameters constrained
S = 1.03Δρmax = 0.21 e Å−3
10664 reflectionsΔρmin = −0.23 e Å−3
547 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*/UeqOcc. (<1)
C10.03612 (7)0.01492 (10)0.19167 (6)0.0264 (3)
H1A0.06760.04950.21270.040*
H1B0.0508−0.02790.17260.040*
H1C0.0171−0.01400.21400.040*
C2−0.00666 (6)0.07331 (9)0.15352 (6)0.0201 (3)
C3−0.02456 (6)0.05069 (10)0.10133 (6)0.0224 (3)
H3−0.0098−0.00180.09330.027*
C4−0.06277 (6)0.09587 (10)0.05709 (6)0.0212 (3)
C5−0.07075 (7)0.05060 (11)0.00496 (6)0.0306 (4)
H5A−0.11120.0392−0.01120.046*
H5B−0.0498−0.00360.01060.046*
H5C−0.05640.0874−0.01750.046*
C6−0.12108 (6)0.21628 (11)0.01393 (6)0.0261 (3)
H6A−0.15710.23830.01830.031*
H6B−0.13060.1766−0.01570.031*
C7−0.08580 (7)0.29214 (11)0.00281 (7)0.0302 (4)
H7A−0.10950.3259−0.02650.036*
H7B−0.07440.33010.03320.036*
N2−0.0335 (4)0.2609 (9)−0.0097 (4)0.0202 (16)0.54
C80.01620 (13)0.2779 (2)0.03670 (14)0.0250 (6)0.54
H80.00340.26330.06730.030*0.54
C90.0646 (3)0.2142 (4)0.0370 (3)0.0333 (11)0.54
H9A0.04920.15600.03150.050*0.54
H9B0.09410.21720.07020.050*0.54
H9C0.08100.22920.00940.050*0.54
C100.0389 (2)0.3719 (3)0.04501 (17)0.0337 (9)0.54
H10A0.00770.41070.04520.051*0.54
H10B0.05460.38790.01710.051*0.54
H10C0.06870.37600.07800.051*0.54
C11−0.02796 (17)0.2864 (2)−0.06088 (13)0.0274 (7)0.54
H110.01290.2784−0.05870.033*0.54
C12−0.0434 (3)0.3802 (4)−0.0801 (2)0.0430 (13)0.54
H12A−0.02120.4205−0.05440.064*0.54
H12B−0.08390.3901−0.08540.064*0.54
H12C−0.03470.3887−0.11270.064*0.54
C13−0.0619 (2)0.2222 (3)−0.10225 (16)0.0387 (9)0.54
H13A−0.05180.1636−0.09030.058*0.54
H13B−0.05260.2316−0.13440.058*0.54
H13C−0.10270.2310−0.10800.058*0.54
N2X−0.0405 (5)0.2711 (11)−0.0197 (4)0.0208 (18)0.46
C8X0.02092 (15)0.2937 (2)0.00340 (18)0.0322 (8)0.46
H8X0.04020.2847−0.02380.039*0.46
C9X0.0489 (3)0.2328 (5)0.0481 (3)0.051 (2)0.46
H9X10.04150.17350.03650.077*0.46
H9X20.03310.24330.07660.077*0.46
H9X30.09000.24300.05960.077*0.46
C10X0.0314 (3)0.3897 (4)0.0215 (2)0.0450 (14)0.46
H10D0.01310.4278−0.00720.068*0.46
H10E0.07220.40130.03320.068*0.46
H10F0.01520.39980.04990.068*0.46
C11X−0.06212 (19)0.2748 (3)−0.07734 (16)0.0252 (7)0.46
H11X−0.10330.2593−0.08650.030*0.46
C12X−0.0600 (3)0.3671 (4)−0.0997 (2)0.0349 (13)0.46
H12D−0.07730.4079−0.08140.052*0.46
H12E−0.08100.3675−0.13640.052*0.46
H12F−0.02040.3832−0.09520.052*0.46
C13X−0.0344 (2)0.2077 (4)−0.1049 (2)0.0426 (13)0.46
H13D−0.03550.1511−0.08970.064*0.46
H13E0.00510.2238−0.10070.064*0.46
H13F−0.05540.2060−0.14150.064*0.46
C140.03140 (7)0.43725 (11)0.18893 (8)0.0356 (4)
H14A0.03890.43940.22630.053*
H14B0.03410.49500.17590.053*
H14C0.05940.40000.18050.053*
C15−0.02842 (6)0.40173 (9)0.16407 (6)0.0221 (3)
C16−0.06666 (6)0.44917 (10)0.12539 (6)0.0240 (3)
H16−0.05120.49920.11490.029*
C17−0.12707 (6)0.43358 (10)0.09841 (6)0.0223 (3)
C18−0.15555 (7)0.50790 (11)0.06224 (7)0.0341 (4)
H18A−0.16370.48940.02640.051*
H18B−0.12990.55730.06840.051*
H18C−0.19110.52390.06910.051*
C19−0.21716 (6)0.35616 (10)0.08018 (6)0.0228 (3)
H19A−0.22680.29990.06310.027*
H19B−0.23010.40130.05380.027*
C20−0.24847 (6)0.36647 (10)0.12203 (6)0.0224 (3)
H20A−0.28880.35040.10710.027*
H20B−0.23150.32660.15070.027*
C21−0.29068 (6)0.51364 (10)0.11119 (6)0.0244 (3)
H21−0.29690.49760.07440.029*
C22−0.27038 (8)0.60871 (11)0.11683 (7)0.0349 (4)
H22A−0.23350.61290.11010.052*
H22B−0.26670.62860.15180.052*
H22C−0.29820.64430.09210.052*
C23−0.34947 (7)0.50708 (11)0.12156 (7)0.0296 (4)
H23A−0.36250.44750.11750.044*
H23B−0.37700.54320.09700.044*
H23C−0.34580.52630.15660.044*
C24−0.23473 (7)0.46046 (11)0.20018 (6)0.0267 (3)
H24−0.24430.52010.20810.032*
C25−0.17030 (7)0.44731 (12)0.22745 (7)0.0344 (4)
H25A−0.14820.48650.21270.052*
H25B−0.15980.38810.22260.052*
H25C−0.16230.45900.26430.052*
C26−0.27080 (8)0.39859 (13)0.22335 (7)0.0381 (4)
H26A−0.31120.40760.20590.057*
H26B−0.26300.41030.26010.057*
H26C−0.26070.33920.21850.057*
C27−0.12638 (7)0.22155 (11)0.30709 (6)0.0272 (3)
H27A−0.09170.19140.32610.041*
H27B−0.15750.20540.32090.041*
H27C−0.12010.28340.31080.041*
C28−0.14193 (6)0.19710 (9)0.24988 (6)0.0200 (3)
C29−0.19634 (6)0.16570 (10)0.22532 (6)0.0229 (3)
H29−0.22090.16290.24640.027*
C30−0.22169 (6)0.13627 (9)0.17216 (6)0.0215 (3)
C31−0.28271 (7)0.10094 (12)0.16156 (7)0.0319 (4)
H31A−0.30980.14160.14010.048*
H31B−0.29130.09290.19420.048*
H31C−0.28570.04590.14370.048*
C32−0.22305 (6)0.10384 (10)0.08364 (6)0.0232 (3)
H32A−0.21880.14420.05700.028*
H32B−0.26410.09600.07890.028*
C33−0.19624 (7)0.01598 (10)0.07648 (6)0.0252 (3)
H33A−0.20930.00010.03960.030*
H33B−0.15440.02230.08650.030*
C34−0.26656 (7)−0.09638 (10)0.08128 (6)0.0269 (3)
H34−0.2935−0.04930.06540.032*
C35−0.29155 (8)−0.14053 (12)0.12123 (7)0.0351 (4)
H35A−0.2909−0.10020.14900.053*
H35B−0.2687−0.19090.13560.053*
H35C−0.3308−0.15820.10430.053*
C36−0.26749 (8)−0.16028 (11)0.03701 (7)0.0367 (4)
H36A−0.2518−0.13240.01200.055*
H36B−0.3067−0.17790.02000.055*
H36C−0.2446−0.21070.05120.055*
C37−0.16169 (7)−0.11353 (11)0.13201 (7)0.0299 (4)
H37−0.1782−0.16550.14360.036*
C38−0.12600 (8)−0.14521 (12)0.09636 (8)0.0420 (5)
H38A−0.1512−0.17280.06580.063*
H38B−0.0974−0.18640.11510.063*
H38C−0.1071−0.09630.08590.063*
C39−0.12278 (7)−0.06952 (12)0.18109 (7)0.0376 (4)
H39A−0.1458−0.05050.20290.056*
H39B−0.1040−0.02010.17110.056*
H39C−0.0941−0.11030.20020.056*
C400.47431 (10)0.18978 (15)0.26053 (9)0.0564 (6)
H40A0.47840.14150.28490.068*
H40B0.47480.24340.28010.068*
C410.41649 (11)0.18220 (16)0.21952 (10)0.0638 (6)
H41A0.41380.12530.20300.077*
H41B0.41420.22600.19270.077*
C420.36531 (11)0.19359 (19)0.24107 (11)0.0717 (7)
H42A0.32990.18810.21300.108*
H42B0.36700.25030.25680.108*
H42C0.36670.14960.26700.108*
Ca1−0.107689 (11)0.224696 (18)0.140247 (11)0.01547 (7)
Ca20.00000.22675 (3)0.25000.01720 (9)
O1−0.02404 (4)0.14111 (7)0.17375 (4)0.0220 (2)
O2−0.03891 (4)0.32665 (6)0.18186 (4)0.0243 (2)
O3−0.10101 (4)0.20875 (7)0.22811 (4)0.0230 (2)
N1−0.08916 (5)0.16878 (8)0.06134 (5)0.0203 (3)
N3−0.15417 (5)0.36245 (8)0.10367 (5)0.0199 (3)
N4−0.24532 (5)0.45532 (8)0.14261 (5)0.0211 (3)
N5−0.19571 (5)0.14134 (8)0.13566 (5)0.0205 (3)
N6−0.21080 (5)−0.05430 (8)0.10712 (5)0.0231 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0279 (8)0.0246 (8)0.0268 (8)0.0088 (7)0.0079 (7)0.0032 (7)
C20.0179 (7)0.0195 (7)0.0243 (8)0.0009 (6)0.0084 (6)0.0006 (6)
C30.0250 (8)0.0184 (7)0.0254 (8)0.0009 (6)0.0097 (6)−0.0040 (6)
C40.0199 (7)0.0239 (7)0.0210 (8)−0.0044 (6)0.0078 (6)−0.0037 (6)
C50.0334 (9)0.0341 (9)0.0243 (8)0.0004 (7)0.0088 (7)−0.0089 (7)
C60.0210 (7)0.0388 (9)0.0191 (8)0.0052 (7)0.0067 (6)0.0022 (7)
C70.0357 (9)0.0300 (9)0.0291 (9)0.0100 (7)0.0162 (7)0.0094 (7)
N20.018 (3)0.026 (4)0.017 (3)0.006 (2)0.005 (2)0.008 (2)
C80.0229 (16)0.0235 (15)0.0258 (17)0.0013 (13)0.0029 (13)0.0006 (14)
C90.024 (3)0.033 (2)0.039 (3)0.0037 (18)0.0027 (17)0.0006 (18)
C100.029 (2)0.030 (2)0.040 (3)−0.0002 (16)0.006 (2)−0.0024 (19)
C110.0266 (17)0.0329 (18)0.0244 (17)−0.0036 (15)0.0101 (15)0.0048 (14)
C120.053 (4)0.041 (3)0.035 (3)−0.010 (2)0.012 (2)0.011 (2)
C130.057 (3)0.040 (2)0.0202 (18)−0.007 (2)0.012 (2)−0.0016 (17)
N2X0.016 (2)0.016 (3)0.025 (4)0.005 (2)−0.002 (2)0.008 (3)
C8X0.0245 (18)0.032 (2)0.036 (2)−0.0019 (15)0.0021 (16)0.0067 (17)
C9X0.033 (4)0.040 (4)0.064 (5)−0.016 (3)−0.013 (3)0.016 (3)
C10X0.045 (3)0.033 (3)0.046 (4)−0.017 (2)−0.003 (3)0.003 (3)
C11X0.024 (2)0.032 (2)0.0212 (19)−0.0042 (17)0.0091 (16)0.0009 (17)
C12X0.034 (3)0.037 (3)0.037 (4)−0.002 (2)0.014 (3)0.010 (3)
C13X0.052 (3)0.045 (3)0.039 (3)0.006 (3)0.026 (3)−0.001 (2)
C140.0286 (9)0.0257 (8)0.0438 (11)−0.0079 (7)−0.0030 (8)0.0064 (8)
C150.0229 (7)0.0188 (7)0.0240 (8)−0.0014 (6)0.0058 (6)−0.0005 (6)
C160.0250 (8)0.0203 (7)0.0275 (8)−0.0006 (6)0.0088 (6)0.0047 (6)
C170.0253 (8)0.0233 (7)0.0193 (7)0.0055 (6)0.0080 (6)0.0033 (6)
C180.0297 (9)0.0322 (9)0.0388 (10)0.0048 (7)0.0074 (8)0.0149 (8)
C190.0212 (7)0.0228 (7)0.0217 (8)0.0046 (6)0.0022 (6)−0.0019 (6)
C200.0186 (7)0.0218 (7)0.0253 (8)0.0025 (6)0.0042 (6)0.0005 (6)
C210.0254 (8)0.0248 (8)0.0216 (8)0.0084 (6)0.0051 (6)0.0003 (6)
C220.0398 (10)0.0262 (8)0.0407 (10)0.0090 (7)0.0153 (8)0.0039 (8)
C230.0226 (8)0.0339 (9)0.0298 (9)0.0076 (7)0.0035 (7)−0.0038 (7)
C240.0269 (8)0.0306 (8)0.0205 (8)0.0075 (7)0.0038 (6)−0.0038 (7)
C250.0292 (9)0.0407 (10)0.0278 (9)0.0077 (8)−0.0005 (7)−0.0041 (8)
C260.0384 (10)0.0504 (11)0.0282 (9)0.0082 (9)0.0142 (8)0.0058 (8)
C270.0299 (8)0.0321 (8)0.0224 (8)−0.0029 (7)0.0118 (7)−0.0007 (7)
C280.0221 (7)0.0192 (7)0.0204 (7)0.0032 (6)0.0087 (6)0.0029 (6)
C290.0233 (7)0.0233 (7)0.0255 (8)0.0000 (6)0.0125 (6)−0.0003 (6)
C300.0187 (7)0.0179 (7)0.0279 (8)0.0008 (6)0.0069 (6)0.0016 (6)
C310.0242 (8)0.0374 (9)0.0366 (10)−0.0066 (7)0.0128 (7)−0.0051 (8)
C320.0230 (7)0.0239 (7)0.0210 (8)−0.0053 (6)0.0036 (6)0.0002 (6)
C330.0299 (8)0.0230 (8)0.0231 (8)−0.0057 (6)0.0085 (6)−0.0032 (6)
C340.0280 (8)0.0236 (8)0.0249 (8)−0.0069 (6)0.0013 (7)−0.0014 (6)
C350.0347 (9)0.0349 (9)0.0336 (10)−0.0143 (8)0.0069 (8)0.0010 (8)
C360.0478 (11)0.0270 (8)0.0298 (9)−0.0089 (8)0.0031 (8)−0.0035 (7)
C370.0304 (8)0.0251 (8)0.0313 (9)−0.0035 (7)0.0046 (7)0.0025 (7)
C380.0419 (10)0.0336 (10)0.0508 (12)0.0071 (8)0.0140 (9)0.0006 (9)
C390.0293 (9)0.0445 (10)0.0333 (10)−0.0067 (8)0.0006 (7)0.0039 (8)
C400.0796 (17)0.0473 (12)0.0545 (14)−0.0031 (12)0.0389 (13)0.0011 (11)
C410.0844 (18)0.0534 (14)0.0609 (16)−0.0170 (13)0.0331 (14)−0.0008 (12)
C420.0645 (16)0.0838 (19)0.0715 (18)−0.0185 (14)0.0270 (14)−0.0046 (15)
Ca10.01479 (13)0.01616 (14)0.01496 (14)0.00052 (11)0.00360 (10)0.00004 (11)
Ca20.01669 (19)0.01833 (19)0.0150 (2)0.0000.00218 (15)0.000
O10.0220 (5)0.0237 (5)0.0185 (5)0.0056 (4)0.0030 (4)−0.0033 (4)
O20.0258 (5)0.0174 (5)0.0238 (6)−0.0037 (4)−0.0020 (4)0.0033 (4)
O30.0185 (5)0.0346 (6)0.0168 (5)−0.0012 (4)0.0066 (4)0.0012 (4)
N10.0177 (6)0.0253 (6)0.0180 (6)0.0001 (5)0.0053 (5)0.0008 (5)
N30.0184 (6)0.0217 (6)0.0195 (6)0.0032 (5)0.0055 (5)0.0001 (5)
N40.0202 (6)0.0211 (6)0.0207 (7)0.0047 (5)0.0041 (5)−0.0005 (5)
N50.0211 (6)0.0186 (6)0.0215 (6)−0.0020 (5)0.0058 (5)−0.0003 (5)
N60.0239 (6)0.0206 (6)0.0228 (7)−0.0057 (5)0.0039 (5)0.0005 (5)
Geometric parameters (Å, º) top
C1—C21.510 (2)C21—N41.4691 (19)
C1—H1A0.9600C21—C231.527 (2)
C1—H1B0.9600C21—C221.529 (2)
C1—H1C0.9600C21—H210.9800
C2—O11.2953 (17)C22—H22A0.9600
C2—C31.375 (2)C22—H22B0.9600
C3—C41.442 (2)C22—H22C0.9600
C3—H30.9300C23—H23A0.9600
C4—N11.3066 (19)C23—H23B0.9600
C4—C51.514 (2)C23—H23C0.9600
C5—H5A0.9600C24—N41.4824 (19)
C5—H5B0.9600C24—C251.524 (2)
C5—H5C0.9600C24—C261.534 (2)
C6—N11.4652 (19)C24—H240.9800
C6—C71.520 (2)C25—H25A0.9600
C6—H6A0.9700C25—H25B0.9600
C6—H6B0.9700C25—H25C0.9600
C7—N2X1.431 (12)C26—H26A0.9600
C7—N21.478 (9)C26—H26B0.9600
C7—H7A0.9700C26—H26C0.9600
C7—H7B0.9700C27—C281.507 (2)
N2—C111.464 (9)C27—H27A0.9600
N2—C81.470 (10)C27—H27B0.9600
C8—C91.520 (5)C27—H27C0.9600
C8—C101.533 (5)C28—O31.2974 (17)
C8—H80.9800C28—C291.371 (2)
C9—H9A0.9600C29—C301.441 (2)
C9—H9B0.9600C29—H290.9300
C9—H9C0.9600C30—N51.3063 (19)
C10—H10A0.9600C30—C311.516 (2)
C10—H10B0.9600C31—H31A0.9600
C10—H10C0.9600C31—H31B0.9600
C11—C131.524 (5)C31—H31C0.9600
C11—C121.533 (7)C32—N51.4663 (19)
C11—H110.9800C32—C331.529 (2)
C12—H12A0.9600C32—H32A0.9700
C12—H12B0.9600C32—H32B0.9700
C12—H12C0.9600C33—N61.4552 (19)
C13—H13A0.9600C33—H33A0.9700
C13—H13B0.9600C33—H33B0.9700
C13—H13C0.9600C34—N61.4683 (19)
N2X—C8X1.469 (12)C34—C351.528 (2)
N2X—C11X1.472 (11)C34—C361.528 (2)
C8X—C9X1.507 (8)C34—H340.9800
C8X—C10X1.545 (7)C35—H35A0.9600
C8X—H8X0.9800C35—H35B0.9600
C9X—H9X10.9600C35—H35C0.9600
C9X—H9X20.9600C36—H36A0.9600
C9X—H9X30.9600C36—H36B0.9600
C10X—H10D0.9600C36—H36C0.9600
C10X—H10E0.9600C37—N61.485 (2)
C10X—H10F0.9600C37—C391.525 (2)
C11X—C13X1.527 (6)C37—C381.538 (2)
C11X—C12X1.539 (7)C37—H370.9800
C11X—H11X0.9800C38—H38A0.9600
C12X—H12D0.9600C38—H38B0.9600
C12X—H12E0.9600C38—H38C0.9600
C12X—H12F0.9600C39—H39A0.9600
C13X—H13D0.9600C39—H39B0.9600
C13X—H13E0.9600C39—H39C0.9600
C13X—H13F0.9600C40—C411.503 (3)
C14—C151.502 (2)C40—C40i1.505 (4)
C14—H14A0.9600C40—H40A0.9700
C14—H14B0.9600C40—H40B0.9700
C14—H14C0.9600C41—C421.519 (3)
C15—O21.2965 (17)C41—H41A0.9700
C15—C161.372 (2)C41—H41B0.9700
C16—C171.444 (2)C42—H42A0.9600
C16—H160.9300C42—H42B0.9600
C17—N31.2990 (19)C42—H42C0.9600
C17—C181.519 (2)Ca1—O12.3348 (10)
C18—H18A0.9600Ca1—O22.3107 (10)
C18—H18B0.9600Ca1—O32.3136 (10)
C18—H18C0.9600Ca1—N12.4323 (12)
C19—N31.4675 (18)Ca1—N32.4522 (12)
C19—C201.529 (2)Ca1—N52.4510 (12)
C19—H19A0.9700Ca1—Ca23.2931 (3)
C19—H19B0.9700Ca2—O12.3442 (10)
C20—N41.4602 (19)Ca2—O22.3490 (10)
C20—H20A0.9700Ca2—O32.3506 (10)
C20—H20B0.9700
C2—C1—H1A109.5C24—C25—H25A109.5
C2—C1—H1B109.5C24—C25—H25B109.5
H1A—C1—H1B109.5H25A—C25—H25B109.5
C2—C1—H1C109.5C24—C25—H25C109.5
H1A—C1—H1C109.5H25A—C25—H25C109.5
H1B—C1—H1C109.5H25B—C25—H25C109.5
O1—C2—C3125.43 (13)C24—C26—H26A109.5
O1—C2—C1115.79 (13)C24—C26—H26B109.5
C3—C2—C1118.78 (13)H26A—C26—H26B109.5
C2—C3—C4129.94 (14)C24—C26—H26C109.5
C2—C3—H3115.0H26A—C26—H26C109.5
C4—C3—H3115.0H26B—C26—H26C109.5
N1—C4—C3123.34 (13)C28—C27—H27A109.5
N1—C4—C5122.49 (14)C28—C27—H27B109.5
C3—C4—C5114.16 (13)H27A—C27—H27B109.5
C4—C5—H5A109.5C28—C27—H27C109.5
C4—C5—H5B109.5H27A—C27—H27C109.5
H5A—C5—H5B109.5H27B—C27—H27C109.5
C4—C5—H5C109.5O3—C28—C29125.69 (14)
H5A—C5—H5C109.5O3—C28—C27115.04 (13)
H5B—C5—H5C109.5C29—C28—C27119.26 (13)
N1—C6—C7111.40 (13)C28—C29—C30130.49 (13)
N1—C6—H6A109.3C28—C29—H29114.8
C7—C6—H6A109.3C30—C29—H29114.8
N1—C6—H6B109.3N5—C30—C29123.81 (13)
C7—C6—H6B109.3N5—C30—C31122.41 (14)
H6A—C6—H6B108.0C29—C30—C31113.75 (13)
N2X—C7—N212.2 (8)C30—C31—H31A109.5
N2X—C7—C6116.8 (7)C30—C31—H31B109.5
N2—C7—C6111.2 (6)H31A—C31—H31B109.5
N2X—C7—H7A97.2C30—C31—H31C109.5
N2—C7—H7A109.4H31A—C31—H31C109.5
C6—C7—H7A109.4H31B—C31—H31C109.5
N2X—C7—H7B115.0N5—C32—C33111.92 (12)
N2—C7—H7B109.4N5—C32—H32A109.2
C6—C7—H7B109.4C33—C32—H32A109.2
H7A—C7—H7B108.0N5—C32—H32B109.2
C11—N2—C8117.5 (8)C33—C32—H32B109.2
C11—N2—C7116.2 (6)H32A—C32—H32B107.9
C8—N2—C7107.0 (7)N6—C33—C32113.53 (12)
N2—C8—C9109.0 (6)N6—C33—H33A108.9
N2—C8—C10117.2 (6)C32—C33—H33A108.9
C9—C8—C10111.1 (4)N6—C33—H33B108.9
N2—C8—H8106.3C32—C33—H33B108.9
C9—C8—H8106.3H33A—C33—H33B107.7
C10—C8—H8106.3N6—C34—C35111.27 (13)
C8—C9—H9A109.5N6—C34—C36116.49 (14)
C8—C9—H9B109.5C35—C34—C36109.67 (13)
H9A—C9—H9B109.5N6—C34—H34106.2
C8—C9—H9C109.5C35—C34—H34106.2
H9A—C9—H9C109.5C36—C34—H34106.2
H9B—C9—H9C109.5C34—C35—H35A109.5
C8—C10—H10A109.5C34—C35—H35B109.5
C8—C10—H10B109.5H35A—C35—H35B109.5
H10A—C10—H10B109.5C34—C35—H35C109.5
C8—C10—H10C109.5H35A—C35—H35C109.5
H10A—C10—H10C109.5H35B—C35—H35C109.5
H10B—C10—H10C109.5C34—C36—H36A109.5
N2—C11—C13109.0 (6)C34—C36—H36B109.5
N2—C11—C12118.9 (6)H36A—C36—H36B109.5
C13—C11—C12109.6 (3)C34—C36—H36C109.5
N2—C11—H11106.2H36A—C36—H36C109.5
C13—C11—H11106.2H36B—C36—H36C109.5
C12—C11—H11106.2N6—C37—C39108.83 (13)
C11—C12—H12A109.5N6—C37—C38115.81 (14)
C11—C12—H12B109.5C39—C37—C38110.75 (14)
H12A—C12—H12B109.5N6—C37—H37107.0
C11—C12—H12C109.5C39—C37—H37107.0
H12A—C12—H12C109.5C38—C37—H37107.0
H12B—C12—H12C109.5C37—C38—H38A109.5
C11—C13—H13A109.5C37—C38—H38B109.5
C11—C13—H13B109.5H38A—C38—H38B109.5
H13A—C13—H13B109.5C37—C38—H38C109.5
C11—C13—H13C109.5H38A—C38—H38C109.5
H13A—C13—H13C109.5H38B—C38—H38C109.5
H13B—C13—H13C109.5C37—C39—H39A109.5
C7—N2X—C8X124.9 (9)C37—C39—H39B109.5
C7—N2X—C11X110.4 (7)H39A—C39—H39B109.5
C8X—N2X—C11X115.6 (8)C37—C39—H39C109.5
N2X—C8X—C9X110.4 (6)H39A—C39—H39C109.5
N2X—C8X—C10X114.0 (7)H39B—C39—H39C109.5
C9X—C8X—C10X110.3 (5)C41—C40—C40i114.8 (3)
N2X—C8X—H8X107.3C41—C40—H40A108.6
C9X—C8X—H8X107.3C40i—C40—H40A108.6
C10X—C8X—H8X107.3C41—C40—H40B108.6
C8X—C9X—H9X1109.5C40i—C40—H40B108.6
C8X—C9X—H9X2109.5H40A—C40—H40B107.5
H9X1—C9X—H9X2109.5C40—C41—C42113.6 (2)
C8X—C9X—H9X3109.5C40—C41—H41A108.8
H9X1—C9X—H9X3109.5C42—C41—H41A108.8
H9X2—C9X—H9X3109.5C40—C41—H41B108.8
C8X—C10X—H10D109.5C42—C41—H41B108.8
C8X—C10X—H10E109.5H41A—C41—H41B107.7
H10D—C10X—H10E109.5C41—C42—H42A109.5
C8X—C10X—H10F109.5C41—C42—H42B109.5
H10D—C10X—H10F109.5H42A—C42—H42B109.5
H10E—C10X—H10F109.5C41—C42—H42C109.5
N2X—C11X—C13X113.9 (6)H42A—C42—H42C109.5
N2X—C11X—C12X113.4 (7)H42B—C42—H42C109.5
C13X—C11X—C12X111.2 (4)O2—Ca1—O376.06 (4)
N2X—C11X—H11X105.8O2—Ca1—O176.59 (4)
C13X—C11X—H11X105.8O3—Ca1—O176.13 (4)
C12X—C11X—H11X105.8O2—Ca1—N1111.34 (4)
C11X—C12X—H12D109.5O3—Ca1—N1149.69 (4)
C11X—C12X—H12E109.5O1—Ca1—N177.25 (4)
H12D—C12X—H12E109.5O2—Ca1—N5149.95 (4)
C11X—C12X—H12F109.5O3—Ca1—N578.25 (4)
H12D—C12X—H12F109.5O1—Ca1—N5111.92 (4)
H12E—C12X—H12F109.5N1—Ca1—N598.70 (4)
C11X—C13X—H13D109.5O2—Ca1—N377.88 (4)
C11X—C13X—H13E109.5O3—Ca1—N3112.38 (4)
H13D—C13X—H13E109.5O1—Ca1—N3150.05 (4)
C11X—C13X—H13F109.5N1—Ca1—N397.92 (4)
H13D—C13X—H13F109.5N5—Ca1—N398.02 (4)
H13E—C13X—H13F109.5O2—Ca1—Ca245.51 (3)
C15—C14—H14A109.5O3—Ca1—Ca245.54 (2)
C15—C14—H14B109.5O1—Ca1—Ca245.38 (3)
H14A—C14—H14B109.5N1—Ca1—Ca2118.30 (3)
C15—C14—H14C109.5N5—Ca1—Ca2119.69 (3)
H14A—C14—H14C109.5N3—Ca1—Ca2119.62 (3)
H14B—C14—H14C109.5O1—Ca2—O1ii111.99 (5)
O2—C15—C16125.71 (14)O1—Ca2—O2ii167.31 (4)
O2—C15—C14115.18 (13)O1ii—Ca2—O2ii75.68 (4)
C16—C15—C14119.11 (14)O1—Ca2—O275.68 (4)
C15—C16—C17130.12 (14)O1ii—Ca2—O2167.31 (4)
C15—C16—H16114.9O2ii—Ca2—O298.76 (5)
C17—C16—H16114.9O1—Ca2—O375.24 (3)
N3—C17—C16123.50 (13)O1ii—Ca2—O397.10 (4)
N3—C17—C18123.25 (14)O2ii—Ca2—O3114.69 (4)
C16—C17—C18113.24 (13)O2—Ca2—O374.63 (4)
C17—C18—H18A109.5O1—Ca2—O3ii97.10 (3)
C17—C18—H18B109.5O1ii—Ca2—O3ii75.24 (3)
H18A—C18—H18B109.5O2ii—Ca2—O3ii74.63 (4)
C17—C18—H18C109.5O2—Ca2—O3ii114.69 (4)
H18A—C18—H18C109.5O3—Ca2—O3ii166.53 (6)
H18B—C18—H18C109.5O1—Ca2—Ca145.15 (2)
N3—C19—C20110.76 (12)O1ii—Ca2—Ca1133.99 (3)
N3—C19—H19A109.5O2ii—Ca2—Ca1136.46 (3)
C20—C19—H19A109.5O2—Ca2—Ca144.56 (2)
N3—C19—H19B109.5O3—Ca2—Ca144.63 (2)
C20—C19—H19B109.5O3ii—Ca2—Ca1135.18 (2)
H19A—C19—H19B108.1O1—Ca2—Ca1ii133.99 (3)
N4—C20—C19112.84 (12)O1ii—Ca2—Ca1ii45.15 (2)
N4—C20—H20A109.0O2ii—Ca2—Ca1ii44.56 (2)
C19—C20—H20A109.0O2—Ca2—Ca1ii136.46 (3)
N4—C20—H20B109.0O3—Ca2—Ca1ii135.18 (2)
C19—C20—H20B109.0O3ii—Ca2—Ca1ii44.63 (2)
H20A—C20—H20B107.8Ca1—Ca2—Ca1178.905 (17)
N4—C21—C23115.67 (13)C2—O1—Ca1129.03 (9)
N4—C21—C22111.04 (13)C2—O1—Ca2141.40 (9)
C23—C21—C22109.44 (13)Ca1—O1—Ca289.47 (3)
N4—C21—H21106.7C15—O2—Ca1127.83 (9)
C23—C21—H21106.7C15—O2—Ca2141.58 (9)
C22—C21—H21106.7Ca1—O2—Ca289.93 (4)
C21—C22—H22A109.5C28—O3—Ca1129.24 (9)
C21—C22—H22B109.5C28—O3—Ca2140.91 (9)
H22A—C22—H22B109.5Ca1—O3—Ca289.82 (3)
C21—C22—H22C109.5C4—N1—C6119.69 (13)
H22A—C22—H22C109.5C4—N1—Ca1126.46 (10)
H22B—C22—H22C109.5C6—N1—Ca1112.81 (9)
C21—C23—H23A109.5C17—N3—C19120.03 (12)
C21—C23—H23B109.5C17—N3—Ca1125.30 (9)
H23A—C23—H23B109.5C19—N3—Ca1114.12 (9)
C21—C23—H23C109.5C20—N4—C21113.84 (12)
H23A—C23—H23C109.5C20—N4—C24114.37 (12)
H23B—C23—H23C109.5C21—N4—C24115.50 (12)
N4—C24—C25109.12 (13)C30—N5—C32120.04 (12)
N4—C24—C26116.05 (13)C30—N5—Ca1126.39 (10)
C25—C24—C26110.30 (14)C32—N5—Ca1113.15 (9)
N4—C24—H24107.0C33—N6—C34113.61 (12)
C25—C24—H24107.0C33—N6—C37114.16 (12)
C26—C24—H24107.0C34—N6—C37116.29 (12)
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x, y, −z+1/2.

Experimental details

Crystal data
Chemical formula[Ca3(C13H25N2O)6]·C6H14
Mr1558.51
Crystal system, space groupMonoclinic, C2/c
Temperature (K)110
a, b, c (Å)24.1444 (3), 15.3089 (2), 26.6679 (5)
β (°) 107.132 (1)
V (Å3)9419.7 (3)
Z4
Radiation typeMo Kα
µ (mm−1)0.23
Crystal size (mm)0.3 × 0.3 × 0.25
Data collection
DiffractometerNonius KappaCCD
Absorption correction–
No. of measured, independent and
observed [I > 2σ(I)] reflections		19153, 10664, 8196
Rint0.035
(sin θ/λ)max (Å−1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.105, 1.03
No. of reflections10664
No. of parameters547
No. of restraints14
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.21, −0.23

Computer programs: KappaCCD Server Software (Nonius, 1997), DENZO–SMN (Otwinowski & Minor, 1997), DENZO–SMN, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997), SHELXL97 and WinGX (Farrugia, 1999).

Selected bond lengths (Å) top
Ca1—O12.3348 (10)Ca1—N52.4510 (12)
Ca1—O22.3107 (10)Ca2—O12.3442 (10)
Ca1—O32.3136 (10)Ca2—O22.3490 (10)
Ca1—N12.4323 (12)Ca2—O32.3506 (10)
Ca1—N32.4522 (12)
 

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