Literature DB >> 22590171

catena-Poly[[penta-μ-benzoato-μ-chlorido-dioxanedineodymium(III)] dioxane 2.5-solvate].

Jeffrey A Bertke1, Allen G Oliver, Kenneth W Henderson.   

Abstract

The asymmetric unit of the title compound, [Nd(2)(C(6)H(5)COO)(5)Cl(C(4)H(8)O(2))]·2.5C(4)H(8)O(2), consists of two Nd(III) ions bridged by one Cl(-) ion, five benzoate ions and one coordinating 1,4-dioxane mol-ecule. One Nd(III) ion is nine-coordinate, with a very distorted monocapped square-anti-prismatic geometry. It is coordinated by two chelating carboxyl-ate groups, three monodentate carboxyl-ate groups, one chloride ion and one dioxane mol-ecule. A second independent Nd(III) ion is eight-coordinated in a distorted square-anti-prismatic geometry by one chelating carboxyl-ate group, five monodentate carboxyl-ate groups and one chloride ion. The chains of the extended structure are parallel to the crystallographic b axis. There is a small amount of void space which is filled with five disordered dioxane solvent mol-ecules per unit cell. The intensity contribution of the disordered solvent molecules was removed by applying the SQUEEZE procedure in PLATON [Spek (2009). Acta Cryst. D65, 148-155].

Entities:  

Year:  2012        PMID： 22590171      PMCID： PMC3344409          DOI： 10.1107/S1600536812017746

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


Related literature

For recent research on ditopic-linked secondary building units, see: Morris et al. (2008 ▶). For 2-D neodymium adducts, see: Nayak et al. (2010 ▶). For the synthesis of the neodymium precursor, see: Andersen et al. (1978 ▶). For SQUEEZE analysis of the data, see: Spek (2009 ▶).

Experimental

Crystal data

[Nd2(C7H5O2)5Cl(C4H8O2)]·2.5C4H8O2 M = 1237.84 Triclinic, a = 12.7631 (5) Å b = 13.6077 (6) Å c = 14.2614 (7) Å α = 102.785 (3)° β = 96.943 (3)° γ = 104.316 (3)° V = 2299.68 (18) Å3 Z = 2 Mo Kα radiation μ = 2.37 mm−1 T = 100 K 0.32 × 0.18 × 0.16 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2008 ▶) T min = 0.606, T max = 0.685 27066 measured reflections 8104 independent reflections 4870 reflections with I > 2σ(I) R int = 0.087

Refinement

R[F 2 > 2σ(F 2)] = 0.052 wR(F 2) = 0.119 S = 0.90 8104 reflections 427 parameters H-atom parameters constrained Δρmax = 1.45 e Å−3 Δρmin = −0.94 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: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL and publCIF (Westrip, 2010 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812017746/fj2541sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812017746/fj2541Isup3.hkl Supplementary material file. DOI: 10.1107/S1600536812017746/fj2541Isup4.cdx Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Nd2(C7H5O2)5Cl(C4H8O2)]·2.5C4H8O2Z = 2
Mr = 1237.84F(000) = 1240
Triclinic, P1Dx = 1.788 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.7631 (5) ÅCell parameters from 2312 reflections
b = 13.6077 (6) Åθ = 2.4–19.0°
c = 14.2614 (7) ŵ = 2.37 mm−1
α = 102.785 (3)°T = 100 K
β = 96.943 (3)°Needle, blue
γ = 104.316 (3)°0.32 × 0.18 × 0.16 mm
V = 2299.68 (18) Å3
Bruker APEXII CCD diffractometer8104 independent reflections
Radiation source: fine-focus sealed tube4870 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.087
Detector resolution: 8.33 pixels mm-1θmax = 25.1°, θmin = 1.5°
φ and ω scansh = −15→15
Absorption correction: multi-scan (SADABS; Sheldrick, 2008)k = −16→16
Tmin = 0.606, Tmax = 0.685l = −13→17
27066 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.052Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.119H-atom parameters constrained
S = 0.90w = 1/[σ2(Fo2) + (0.0572P)2] where P = (Fo2 + 2Fc2)/3
8104 reflections(Δ/σ)max = 0.001
427 parametersΔρmax = 1.45 e Å−3
0 restraintsΔρmin = −0.94 e Å−3
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.
xyzUiso*/UeqOcc. (<1)
Nd10.42843 (3)0.05580 (3)0.39858 (3)0.02441 (14)
Nd20.46041 (4)0.35430 (3)0.41815 (4)0.03265 (16)
Cl10.27807 (15)0.17311 (16)0.36816 (16)0.0329 (5)
O10.5172 (4)0.2130 (4)0.3257 (4)0.0310 (14)
O20.4585 (4)0.0526 (4)0.2303 (4)0.0341 (14)
O30.6189 (4)0.0707 (5)0.3970 (5)0.0456 (17)
O40.7013 (4)0.0001 (4)0.5011 (4)0.0316 (14)
O50.4679 (4)−0.1024 (4)0.4236 (4)0.0300 (13)
O60.5077 (4)−0.2327 (4)0.4716 (4)0.0291 (13)
O70.5231 (7)0.4308 (5)0.2902 (5)0.063 (2)
O80.5524 (4)0.5571 (4)0.4251 (4)0.0368 (15)
O90.3103 (4)0.4307 (4)0.3939 (4)0.0358 (15)
O100.3508 (4)0.5843 (4)0.5070 (4)0.0377 (15)
O110.2669 (4)−0.0860 (4)0.2839 (4)0.0374 (15)
O120.0494 (6)−0.1857 (6)0.1846 (5)0.074 (2)
C10.5171 (7)0.1464 (7)0.2475 (6)0.032 (2)
C20.5931 (7)0.1778 (7)0.1806 (6)0.034 (2)
C30.6589 (7)0.2799 (7)0.1979 (7)0.041 (2)
H30.65340.33320.25120.049*
C40.7321 (7)0.3036 (8)0.1375 (7)0.044 (2)
H40.77580.37390.14800.052*
C50.7424 (9)0.2266 (9)0.0625 (8)0.061 (3)
H50.79490.24310.02240.074*
C60.6765 (11)0.1250 (10)0.0450 (9)0.087 (4)
H60.68280.0715−0.00770.104*
C70.6023 (9)0.1019 (8)0.1038 (7)0.062 (3)
H70.55630.03210.09130.074*
C80.7002 (7)0.0470 (7)0.4349 (7)0.036 (2)
C150.4761 (6)−0.1963 (6)0.4033 (6)0.0265 (19)
C160.4459 (6)−0.2587 (7)0.2995 (6)0.029 (2)
C170.4655 (7)−0.2070 (7)0.2282 (6)0.036 (2)
H170.4979−0.13310.24580.043*
C180.4375 (8)−0.2634 (8)0.1285 (7)0.049 (3)
H180.4518−0.22860.07860.059*
C190.3889 (10)−0.3704 (8)0.1055 (8)0.066 (3)
H190.3696−0.40970.03890.079*
C200.3682 (9)−0.4208 (8)0.1774 (7)0.063 (3)
H200.3328−0.49410.15980.075*
C210.3980 (6)−0.3665 (6)0.2748 (6)0.033 (2)
H210.3859−0.40230.32430.039*
C220.5731 (9)0.5236 (9)0.3398 (8)0.052 (3)
C230.6533 (9)0.5968 (8)0.3005 (8)0.050 (3)
C240.7152 (8)0.6935 (8)0.3578 (8)0.053 (3)
H240.70770.71610.42400.063*
C250.7892 (9)0.7580 (11)0.3175 (11)0.080 (4)
H250.83550.82410.35640.096*
C260.7940 (11)0.7236 (13)0.2186 (12)0.091 (5)
H260.84490.76650.19050.110*
C270.7268 (14)0.6292 (14)0.1617 (11)0.099 (5)
H270.72960.60840.09410.119*
C280.6564 (11)0.5655 (10)0.2008 (9)0.076 (4)
H280.60960.50000.16120.092*
C290.2858 (7)0.5090 (7)0.4387 (7)0.034 (2)
C360.2039 (7)−0.1803 (7)0.3002 (8)0.056 (3)
H36A0.2273−0.18240.36830.067*
H36B0.2163−0.24150.25550.067*
C370.0851 (8)−0.1856 (8)0.2826 (8)0.060 (3)
H37A0.0415−0.25030.29610.072*
H37B0.0729−0.12450.32770.072*
C380.2271 (8)−0.0800 (8)0.1877 (7)0.060 (3)
H38A0.2405−0.13720.13860.072*
H38B0.2679−0.01220.17780.072*
C390.1106 (9)−0.0887 (10)0.1734 (9)0.078 (4)
H39A0.0973−0.03060.22160.093*
H39B0.0858−0.08250.10710.093*
C90.8010 (9)0.0640 (11)0.3862 (10)0.021 (4)*0.50
C100.9017 (11)0.0620 (12)0.4340 (9)0.032 (9)*0.50
H100.90620.04140.49350.038*0.50
C110.9959 (8)0.0900 (11)0.3948 (10)0.031 (6)*0.50
H111.06470.08860.42750.037*0.50
C120.9893 (9)0.1201 (10)0.3077 (10)0.041 (5)*0.50
H121.05370.13920.28100.049*0.50
C130.8886 (11)0.1221 (12)0.2599 (8)0.084 (8)*0.50
H130.88420.14260.20040.101*0.50
C140.7945 (9)0.0941 (12)0.2991 (10)0.076 (7)*0.50
H140.72570.09550.26640.092*0.50
C9A0.8092 (8)0.0957 (9)0.4084 (8)0.019 (4)*0.50
C10A0.9047 (11)0.0748 (11)0.4459 (9)0.040 (10)*0.50
H10A0.90300.03440.49250.048*0.50
C11A1.0026 (8)0.1131 (11)0.4154 (10)0.032 (6)*0.50
H11A1.06780.09880.44110.039*0.50
C12A1.0050 (7)0.1723 (9)0.3474 (9)0.037 (4)*0.50
H12A1.07200.19840.32650.044*0.50
C13A0.9096 (8)0.1931 (8)0.3098 (8)0.042 (5)*0.50
H13A0.91130.23360.26330.051*0.50
C14A0.8117 (7)0.1548 (8)0.3403 (8)0.022 (3)*0.50
H14A0.74650.16910.31470.026*0.50
C300.1778 (10)0.5269 (13)0.4109 (13)0.029 (7)*0.50
C310.1526 (13)0.6120 (13)0.4677 (12)0.066 (10)*0.50
H310.20600.65990.52100.079*0.50
C320.0493 (14)0.6268 (12)0.4467 (12)0.062 (8)*0.50
H320.03210.68500.48560.074*0.50
C33−0.0288 (10)0.5566 (13)0.3688 (11)0.043 (5)*0.50
H33−0.09940.56680.35440.052*0.50
C34−0.0036 (11)0.4716 (11)0.3119 (10)0.089 (8)*0.50
H34−0.05700.42360.25870.106*0.50
C350.0997 (12)0.4567 (10)0.3329 (10)0.048 (5)*0.50
H350.11690.39860.29410.058*0.50
C30A0.1673 (10)0.5126 (12)0.4180 (12)0.031 (7)*0.50
C31A0.1370 (11)0.6039 (10)0.4499 (13)0.032 (6)*0.50
H31A0.19030.66580.48940.039*0.50
C32A0.0287 (12)0.6048 (11)0.4242 (13)0.035 (5)*0.50
H32A0.00800.66730.44600.043*0.50
C33A−0.0493 (9)0.5143 (14)0.3665 (12)0.079 (9)*0.50
H33A−0.12330.51490.34890.095*0.50
C34A−0.0190 (12)0.4229 (11)0.3346 (11)0.098 (9)*0.50
H34A−0.07230.36110.29510.117*0.50
C35A0.0892 (13)0.4221 (10)0.3603 (11)0.055 (6)*0.50
H35A0.10990.35960.33850.066*0.50
U11U22U33U12U13U23
Nd10.0195 (2)0.0248 (3)0.0326 (3)0.00797 (19)0.0064 (2)0.0122 (2)
Nd20.0263 (3)0.0245 (3)0.0492 (4)0.0104 (2)0.0034 (2)0.0121 (2)
Cl10.0200 (10)0.0315 (11)0.0472 (14)0.0080 (8)0.0016 (9)0.0118 (10)
O10.032 (3)0.030 (3)0.033 (4)0.010 (3)0.011 (3)0.008 (3)
O20.034 (3)0.027 (3)0.039 (4)0.003 (3)0.004 (3)0.011 (3)
O30.020 (3)0.069 (4)0.064 (4)0.019 (3)0.015 (3)0.040 (4)
O40.025 (3)0.042 (3)0.044 (4)0.015 (3)0.017 (3)0.031 (3)
O50.031 (3)0.027 (3)0.036 (4)0.012 (2)0.008 (3)0.011 (3)
O60.030 (3)0.028 (3)0.037 (4)0.012 (2)0.007 (3)0.018 (3)
O70.118 (7)0.041 (4)0.048 (5)0.040 (4)0.026 (4)0.021 (4)
O80.033 (3)0.040 (4)0.044 (4)0.016 (3)0.009 (3)0.015 (3)
O90.028 (3)0.027 (3)0.051 (4)0.013 (3)0.004 (3)0.005 (3)
O100.027 (3)0.029 (3)0.055 (4)0.009 (3)0.002 (3)0.009 (3)
O110.038 (3)0.028 (3)0.044 (4)0.003 (3)0.004 (3)0.014 (3)
O120.048 (4)0.090 (6)0.059 (5)−0.025 (4)−0.019 (4)0.034 (4)
C10.027 (5)0.038 (5)0.036 (6)0.017 (4)0.003 (4)0.017 (5)
C20.032 (5)0.048 (6)0.028 (5)0.013 (4)0.008 (4)0.022 (5)
C30.034 (5)0.052 (6)0.039 (6)0.009 (4)0.008 (4)0.017 (5)
C40.031 (5)0.048 (6)0.049 (7)−0.002 (4)0.004 (5)0.024 (5)
C50.067 (8)0.079 (8)0.043 (7)0.016 (6)0.021 (6)0.027 (6)
C60.112 (11)0.074 (9)0.062 (8)−0.009 (8)0.059 (8)0.010 (7)
C70.072 (8)0.057 (7)0.042 (7)−0.017 (6)0.027 (6)0.012 (6)
C80.023 (5)0.044 (5)0.044 (6)0.012 (4)0.014 (4)0.010 (5)
C150.012 (4)0.032 (5)0.034 (5)0.002 (3)0.002 (4)0.011 (4)
C160.023 (4)0.043 (5)0.027 (5)0.009 (4)0.001 (4)0.022 (4)
C170.034 (5)0.035 (5)0.039 (6)0.015 (4)0.005 (4)0.007 (5)
C180.064 (7)0.055 (7)0.029 (6)0.016 (5)0.003 (5)0.016 (5)
C190.101 (9)0.046 (7)0.045 (7)0.016 (6)0.000 (6)0.012 (6)
C200.090 (9)0.042 (6)0.043 (7)0.014 (6)−0.013 (6)0.003 (6)
C210.034 (5)0.038 (5)0.036 (6)0.016 (4)0.001 (4)0.024 (4)
C220.076 (8)0.059 (7)0.044 (7)0.050 (6)0.010 (6)0.029 (6)
C230.068 (7)0.047 (6)0.062 (8)0.041 (6)0.036 (6)0.031 (6)
C240.046 (6)0.065 (7)0.063 (7)0.027 (6)0.023 (6)0.029 (6)
C250.039 (7)0.100 (10)0.115 (12)0.012 (6)0.025 (7)0.058 (9)
C260.071 (9)0.129 (14)0.108 (13)0.031 (9)0.054 (9)0.076 (11)
C270.119 (14)0.124 (14)0.081 (11)0.062 (12)0.031 (10)0.042 (11)
C280.127 (12)0.064 (8)0.063 (9)0.040 (8)0.053 (8)0.036 (7)
C290.027 (5)0.036 (5)0.049 (6)0.013 (4)0.010 (4)0.023 (5)
C360.043 (6)0.041 (6)0.081 (8)0.002 (5)0.002 (5)0.026 (6)
C370.050 (7)0.054 (7)0.073 (8)0.004 (5)0.005 (6)0.024 (6)
C380.058 (7)0.069 (7)0.045 (7)−0.002 (6)−0.010 (5)0.031 (6)
C390.056 (7)0.083 (9)0.085 (9)−0.003 (6)−0.008 (6)0.040 (7)
Nd1—O32.392 (5)C22—C231.495 (14)
Nd1—O4i2.409 (5)C23—C241.370 (13)
Nd1—O52.418 (5)C23—C281.399 (14)
Nd1—O22.469 (5)C24—C251.392 (14)
Nd1—O112.543 (5)C24—H240.9500
Nd1—O6i2.565 (5)C25—C261.398 (17)
Nd1—O5i2.578 (5)C25—H250.9500
Nd1—O12.647 (5)C26—C271.368 (18)
Nd1—Cl12.835 (2)C26—H260.9500
Nd1—C12.918 (9)C27—C281.349 (17)
Nd1—C15i2.958 (8)C27—H270.9500
Nd1—Nd23.9235 (6)C28—H280.9500
Nd2—O8ii2.339 (6)C29—C301.482 (13)
Nd2—O10ii2.373 (5)C29—C30A1.521 (13)
Nd2—O12.400 (5)C36—C371.488 (13)
Nd2—O72.415 (7)C36—H36A0.9900
Nd2—O92.420 (5)C36—H36B0.9900
Nd2—O6i2.589 (5)C37—H37A0.9900
Nd2—O82.693 (6)C37—H37B0.9900
Nd2—Cl12.826 (2)C38—C391.447 (14)
Nd2—C222.918 (11)C38—H38A0.9900
Nd2—Nd2ii3.9428 (9)C38—H38B0.9900
O1—C11.272 (9)C39—H39A0.9900
O2—C11.262 (9)C39—H39B0.9900
O3—C81.258 (10)C9—C101.3900
O4—C81.251 (10)C9—C141.3900
O4—Nd1i2.409 (5)C10—C111.3900
O5—C151.280 (9)C10—H100.9500
O5—Nd1i2.578 (5)C11—C121.3900
O6—C151.254 (9)C11—H110.9500
O6—Nd1i2.565 (5)C12—C131.3900
O6—Nd2i2.589 (5)C12—H120.9500
O7—C221.265 (12)C13—C141.3900
O8—C221.284 (11)C13—H130.9500
O8—Nd2ii2.339 (6)C14—H140.9500
O9—C291.246 (9)C9A—C10A1.3900
O10—C291.276 (10)C9A—C14A1.3900
O10—Nd2ii2.373 (5)C10A—C11A1.3900
O11—C361.419 (10)C10A—H10A0.9500
O11—C381.431 (10)C11A—C12A1.3900
O12—C391.411 (12)C11A—H11A0.9500
O12—C371.417 (11)C12A—C13A1.3900
C1—C21.495 (11)C12A—H12A0.9500
C2—C71.368 (12)C13A—C14A1.3900
C2—C31.384 (12)C13A—H13A0.9500
C3—C41.374 (12)C14A—H14A0.9500
C3—H30.9500C30—C311.3900
C4—C51.365 (13)C30—C351.3900
C4—H40.9500C31—C321.3900
C5—C61.379 (15)C31—H310.9500
C5—H50.9500C32—C331.3900
C6—C71.366 (13)C32—H320.9500
C6—H60.9500C33—C341.3900
C7—H70.9500C33—H330.9500
C8—C9A1.517 (12)C34—C351.3900
C8—C91.528 (12)C34—H340.9500
C15—C161.486 (11)C35—H350.9500
C15—Nd1i2.958 (8)C30A—C31A1.3900
C16—C171.373 (11)C30A—C35A1.3900
C16—C211.387 (11)C31A—C32A1.3900
C17—C181.413 (12)C31A—H31A0.9500
C17—H170.9500C32A—C33A1.3900
C18—C191.380 (13)C32A—H32A0.9500
C18—H180.9500C33A—C34A1.3900
C19—C201.370 (14)C33A—H33A0.9500
C19—H190.9500C34A—C35A1.3900
C20—C211.378 (12)C34A—H34A0.9500
C20—H200.9500C35A—H35A0.9500
C21—H210.9500
O3—Nd1—O4i136.30 (19)C7—C6—C5119.5 (11)
O3—Nd1—O570.64 (19)C7—C6—H6120.2
O4i—Nd1—O577.57 (18)C5—C6—H6120.2
O3—Nd1—O272.27 (19)C6—C7—C2120.9 (10)
O4i—Nd1—O2145.82 (18)C6—C7—H7119.5
O5—Nd1—O2103.26 (18)C2—C7—H7119.5
O3—Nd1—O11125.9 (2)O4—C8—O3125.8 (8)
O4i—Nd1—O1173.60 (18)O4—C8—C9A118.0 (8)
O5—Nd1—O1178.40 (17)O3—C8—C9A115.4 (9)
O2—Nd1—O1173.18 (18)O4—C8—C9117.3 (8)
O3—Nd1—O6i86.92 (19)O3—C8—C9116.4 (9)
O4i—Nd1—O6i86.44 (18)C9A—C8—C917.2 (7)
O5—Nd1—O6i123.61 (17)O6—C15—O5119.0 (7)
O2—Nd1—O6i118.35 (17)O6—C15—C16122.6 (7)
O11—Nd1—O6i146.72 (17)O5—C15—C16118.4 (7)
O3—Nd1—O5i71.19 (19)O6—C15—Nd1i59.7 (4)
O4i—Nd1—O5i71.51 (17)O5—C15—Nd1i60.4 (4)
O5—Nd1—O5i73.42 (19)C16—C15—Nd1i170.4 (5)
O2—Nd1—O5i142.16 (17)C17—C16—C21120.7 (8)
O11—Nd1—O5i138.86 (17)C17—C16—C15118.4 (8)
O6i—Nd1—O5i50.26 (16)C21—C16—C15121.0 (7)
O3—Nd1—O169.33 (18)C16—C17—C18120.1 (8)
O4i—Nd1—O1144.00 (17)C16—C17—H17120.0
O5—Nd1—O1137.46 (17)C18—C17—H17120.0
O2—Nd1—O150.61 (17)C19—C18—C17118.3 (9)
O11—Nd1—O1114.92 (18)C19—C18—H18120.8
O6i—Nd1—O167.75 (17)C17—C18—H18120.8
O5i—Nd1—O1106.11 (17)C20—C19—C18120.9 (10)
O3—Nd1—Cl1138.05 (15)C20—C19—H19119.5
O4i—Nd1—Cl179.01 (13)C18—C19—H19119.5
O5—Nd1—Cl1151.08 (13)C19—C20—C21120.9 (10)
O2—Nd1—Cl186.96 (13)C19—C20—H20119.5
O11—Nd1—Cl178.90 (13)C21—C20—H20119.5
O6i—Nd1—Cl171.20 (12)C20—C21—C16119.0 (8)
O5i—Nd1—Cl1114.46 (12)C20—C21—H21120.5
O1—Nd1—Cl169.34 (12)C16—C21—H21120.5
O3—Nd1—C164.6 (2)O7—C22—O8119.3 (10)
O4i—Nd1—C1158.9 (2)O7—C22—C23121.7 (10)
O5—Nd1—C1119.2 (2)O8—C22—C23118.9 (10)
O2—Nd1—C125.4 (2)O7—C22—Nd254.6 (5)
O11—Nd1—C196.2 (2)O8—C22—Nd267.1 (5)
O6i—Nd1—C193.2 (2)C23—C22—Nd2165.5 (6)
O5i—Nd1—C1123.6 (2)C24—C23—C28121.4 (10)
O1—Nd1—C125.83 (19)C24—C23—C22121.4 (10)
Cl1—Nd1—C180.90 (16)C28—C23—C22117.0 (11)
O3—Nd1—C15i80.8 (2)C23—C24—C25118.9 (11)
O4i—Nd1—C15i75.3 (2)C23—C24—H24120.5
O5—Nd1—C15i99.0 (2)C25—C24—H24120.5
O2—Nd1—C15i136.5 (2)C24—C25—C26118.6 (13)
O11—Nd1—C15i148.63 (19)C24—C25—H25120.7
O6i—Nd1—C15i24.98 (18)C26—C25—H25120.7
O5i—Nd1—C15i25.58 (19)C27—C26—C25121.2 (13)
O1—Nd1—C15i88.4 (2)C27—C26—H26119.4
Cl1—Nd1—C15i91.23 (16)C25—C26—H26119.4
C1—Nd1—C15i111.7 (2)C28—C27—C26120.4 (14)
O3—Nd1—Nd294.43 (15)C28—C27—H27119.8
O4i—Nd1—Nd2107.76 (13)C26—C27—H27119.8
O5—Nd1—Nd2160.61 (12)C27—C28—C23119.3 (13)
O2—Nd1—Nd282.92 (12)C27—C28—H28120.4
O11—Nd1—Nd2120.94 (13)C23—C28—H28120.4
O6i—Nd1—Nd240.66 (12)O9—C29—O10125.1 (7)
O5i—Nd1—Nd290.33 (12)O9—C29—C30121.7 (10)
O1—Nd1—Nd236.76 (12)O10—C29—C30113.1 (9)
Cl1—Nd1—Nd246.03 (4)O9—C29—C30A118.6 (9)
C1—Nd1—Nd261.10 (17)O10—C29—C30A116.1 (9)
C15i—Nd1—Nd265.57 (16)C30—C29—C30A9.7 (12)
O8ii—Nd2—O10ii79.77 (19)O11—C36—C37109.7 (8)
O8ii—Nd2—O1144.98 (19)O11—C36—H36A109.7
O10ii—Nd2—O182.75 (18)C37—C36—H36A109.7
O8ii—Nd2—O7127.4 (2)O11—C36—H36B109.7
O10ii—Nd2—O784.2 (2)C37—C36—H36B109.7
O1—Nd2—O780.1 (2)H36A—C36—H36B108.2
O8ii—Nd2—O974.66 (19)O12—C37—C36110.5 (9)
O10ii—Nd2—O9136.64 (18)O12—C37—H37A109.6
O1—Nd2—O9135.61 (19)C36—C37—H37A109.6
O7—Nd2—O984.3 (2)O12—C37—H37B109.6
O8ii—Nd2—O6i74.84 (18)C36—C37—H37B109.6
O10ii—Nd2—O6i73.25 (17)H37A—C37—H37B108.1
O1—Nd2—O6i71.14 (17)O11—C38—C39111.2 (9)
O7—Nd2—O6i145.2 (2)O11—C38—H38A109.4
O9—Nd2—O6i130.15 (18)C39—C38—H38A109.4
O8ii—Nd2—O877.1 (2)O11—C38—H38B109.4
O10ii—Nd2—O866.96 (17)C39—C38—H38B109.4
O1—Nd2—O8122.75 (18)H38A—C38—H38B108.0
O7—Nd2—O850.7 (2)O12—C39—C38111.0 (10)
O9—Nd2—O873.49 (17)O12—C39—H39A109.4
O6i—Nd2—O8134.43 (17)C38—C39—H39A109.4
O8ii—Nd2—Cl1103.71 (14)O12—C39—H39B109.4
O10ii—Nd2—Cl1141.60 (14)C38—C39—H39B109.4
O1—Nd2—Cl172.87 (13)H39A—C39—H39B108.0
O7—Nd2—Cl1119.06 (19)C10—C9—C14120.0
O9—Nd2—Cl179.17 (13)C10—C9—C8120.3 (9)
O6i—Nd2—Cl171.02 (12)C14—C9—C8119.3 (9)
O8—Nd2—Cl1151.44 (12)C11—C10—C9120.0
O8ii—Nd2—C22103.1 (3)C11—C10—H10120.0
O10ii—Nd2—C2270.4 (2)C9—C10—H10120.0
O1—Nd2—C2299.2 (2)C10—C11—C12120.0
O7—Nd2—C2225.3 (2)C10—C11—H11120.0
O9—Nd2—C2282.0 (2)C12—C11—H11120.0
O6i—Nd2—C22143.3 (2)C13—C12—C11120.0
O8—Nd2—C2226.1 (2)C13—C12—H12120.0
Cl1—Nd2—C22141.6 (2)C11—C12—H12120.0
O8ii—Nd2—Nd1111.13 (14)C14—C13—C12120.0
O10ii—Nd2—Nd196.31 (13)C14—C13—H13120.0
O1—Nd2—Nd141.32 (13)C12—C13—H13120.0
O7—Nd2—Nd1120.26 (16)C13—C14—C9120.0
O9—Nd2—Nd1125.35 (13)C13—C14—H14120.0
O6i—Nd2—Nd140.19 (12)C9—C14—H14120.0
O8—Nd2—Nd1160.40 (12)C10A—C9A—C14A120.0
Cl1—Nd2—Nd146.23 (4)C10A—C9A—C8120.4 (8)
C22—Nd2—Nd1140.4 (2)C14A—C9A—C8119.4 (8)
O8ii—Nd2—Nd2ii41.74 (14)C11A—C10A—C9A120.0
O10ii—Nd2—Nd2ii68.11 (13)C11A—C10A—H10A120.0
O1—Nd2—Nd2ii148.79 (13)C9A—C10A—H10A120.0
O7—Nd2—Nd2ii85.83 (16)C10A—C11A—C12A120.0
O9—Nd2—Nd2ii69.45 (13)C10A—C11A—H11A120.0
O6i—Nd2—Nd2ii108.84 (12)C12A—C11A—H11A120.0
O8—Nd2—Nd2ii35.32 (13)C13A—C12A—C11A120.0
Cl1—Nd2—Nd2ii137.78 (5)C13A—C12A—H12A120.0
C22—Nd2—Nd2ii61.4 (2)C11A—C12A—H12A120.0
Nd1—Nd2—Nd2ii149.02 (2)C12A—C13A—C14A120.0
Nd2—Cl1—Nd187.74 (5)C12A—C13A—H13A120.0
C1—O1—Nd2153.5 (5)C14A—C13A—H13A120.0
C1—O1—Nd189.1 (5)C13A—C14A—C9A120.0
Nd2—O1—Nd1101.92 (19)C13A—C14A—H14A120.0
C1—O2—Nd197.6 (5)C9A—C14A—H14A120.0
C8—O3—Nd1143.1 (6)C31—C30—C35120.0
C8—O4—Nd1i134.2 (5)C31—C30—C29118.9 (11)
C15—O5—Nd1159.1 (5)C35—C30—C29121.0 (11)
C15—O5—Nd1i94.0 (5)C32—C31—C30120.0
Nd1—O5—Nd1i106.58 (19)C32—C31—H31120.0
C15—O6—Nd1i95.3 (5)C30—C31—H31120.0
C15—O6—Nd2i164.7 (5)C31—C32—C33120.0
Nd1i—O6—Nd2i99.15 (18)C31—C32—H32120.0
C22—O7—Nd2100.2 (6)C33—C32—H32120.0
C22—O8—Nd2ii169.6 (7)C32—C33—C34120.0
C22—O8—Nd286.8 (6)C32—C33—H33120.0
Nd2ii—O8—Nd2102.9 (2)C34—C33—H33120.0
C29—O9—Nd2135.2 (5)C33—C34—C35120.0
C29—O10—Nd2ii139.3 (5)C33—C34—H34120.0
C36—O11—C38109.3 (7)C35—C34—H34120.0
C36—O11—Nd1128.6 (5)C34—C35—C30120.0
C38—O11—Nd1122.1 (5)C34—C35—H35120.0
C39—O12—C37105.8 (8)C30—C35—H35120.0
O2—C1—O1119.9 (8)C31A—C30A—C35A120.0
O2—C1—C2120.4 (8)C31A—C30A—C29122.2 (10)
O1—C1—C2119.5 (8)C35A—C30A—C29117.7 (10)
O2—C1—Nd157.0 (4)C32A—C31A—C30A120.0
O1—C1—Nd165.1 (4)C32A—C31A—H31A120.0
C2—C1—Nd1160.5 (5)C30A—C31A—H31A120.0
C7—C2—C3119.5 (8)C31A—C32A—C33A120.0
C7—C2—C1118.6 (8)C31A—C32A—H32A120.0
C3—C2—C1121.8 (8)C33A—C32A—H32A120.0
C4—C3—C2119.6 (9)C34A—C33A—C32A120.0
C4—C3—H3120.2C34A—C33A—H33A120.0
C2—C3—H3120.2C32A—C33A—H33A120.0
C5—C4—C3120.4 (9)C33A—C34A—C35A120.0
C5—C4—H4119.8C33A—C34A—H34A120.0
C3—C4—H4119.8C35A—C34A—H34A120.0
C4—C5—C6120.0 (10)C34A—C35A—C30A120.0
C4—C5—H5120.0C34A—C35A—H35A120.0
C6—C5—H5120.0C30A—C35A—H35A120.0
  3 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Manipulation of molecular aggregation and supramolecular structure using self-assembled lithium mixed-anion complexes.

Authors:  J Jacob Morris; Dugald J Macdougall; Bruce C Noll; Kenneth W Henderson
Journal:  Dalton Trans       Date:  2008-04-11       Impact factor: 4.390

3.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
  3 in total

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