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This paper reports 22 examples of space-group changes from low to higher symmetry. The revisions involve 15 crystal structures that were originally described in space group P21, six in P\bar 1 and one in P1. The relevance of higher-symmetry elements is discussed in connection with the crystallography, the molecular dimensions and, when possible, the spectroscopic properties.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768102022668/an0613sup1.cif
Contains datablocks global, barjaf, claecu, qanxos, sazpak, yakvip, bogpiw, novhub, nohned, nohned01, qelpus, aplsol, doqzak, bamubr, farner, farniv, himfue, horbiz, pejvab, sixfio, bihjux, bihlin, zexbuz01, pyrhsb

CCDC references: 205138; 205139; 205140; 205141; 205142; 205143; 205144; 205145; 205146; 205147; 205148; 205149; 205150; 205151; 205152; 205153; 205154; 205155; 205156; 205157; 205158; 205159; 206124

Computing details top

For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

(barjaf) bis(Nitrato)-((4S,5S)-2,2-dimethyl-4,5-bis(2-pyridyl)-1,3-dioxolane)-cobalt(ii) top
Crystal data top
C15H16CoN4O8γ = 90°
Mr = 439.25V = 1810.3 (6) Å3
C2221Z = 4
a = 7.625 (2) ÅF(000) = 900
b = 19.808 (2) ÅDx = 1.612 Mg m3
c = 11.986 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 1.00 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.046
Graphite monochromatorθmax = 46.0°, θmin = 2.1°
8912 measured reflectionsh = 88
2688 independent reflectionsk = 2828
2560 reflections with I > 2σ(I)l = 1212
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.018H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.109 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.58(Δ/σ)max = 4.200
2688 reflectionsΔρmax = 0.52 e Å3
105 parametersΔρmin = 0.22 e Å3
0 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.140 (8)
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)
Co10.00000.022600 (15)0.25000.02000 (9)*
O20.01940 (18)0.25290 (6)0.15650 (11)0.0200 (2)*
O30.17430 (17)0.02200 (7)0.14290 (11)0.0200 (2)*
O40.14130 (17)0.10820 (6)0.03250 (12)0.0200 (2)*
O50.08120 (19)0.06770 (7)0.12090 (12)0.0200 (2)*
N10.18870 (19)0.08220 (7)0.17230 (14)0.0200 (2)*
N40.0758 (2)0.06610 (8)0.09780 (14)0.0200 (3)*
C10.3360 (2)0.04790 (9)0.14270 (15)0.0200 (3)*
H10.343 (4)0.0021 (15)0.159 (3)0.020 (6)*
C20.4745 (2)0.07900 (8)0.08950 (16)0.0200 (2)*
H20.574 (4)0.0544 (13)0.071 (2)0.020 (6)*
C30.4643 (2)0.14570 (9)0.06430 (16)0.0200 (3)*
H30.555 (4)0.1672 (12)0.027 (3)0.020 (6)*
C40.3159 (2)0.18090 (8)0.09570 (16)0.0200 (3)*
H40.307 (4)0.2269 (13)0.081 (3)0.020 (6)*
C50.1802 (2)0.14760 (9)0.14880 (15)0.0200 (3)*
C60.0106 (2)0.18400 (8)0.18520 (13)0.0200 (3)*
H180.083 (4)0.1564 (14)0.144 (2)0.020 (6)*
C14?0.0622 (5)0.29070 (16)0.2570 (4)0.0200 (5)*0.50
C150.00000.35750 (11)0.25000.0200 (4)*
H90.033 (9)0.377 (3)0.321 (6)0.020 (12)*0.50
H100.052 (9)0.384 (3)0.192 (6)0.020 (13)*0.50
H110.124 (8)0.357 (2)0.243 (6)0.020 (11)*0.50
C17?0.2612 (5)0.29550 (17)0.2818 (3)0.0200 (6)*0.50
H15?0.321 (8)0.312 (3)0.217 (5)0.020 (13)*0.50
H16?0.305 (8)0.252 (3)0.301 (5)0.020 (12)*0.50
H17?0.280 (8)0.326 (3)0.343 (5)0.020 (12)*0.50
Geometric parameters (Å, º) top
Co1—O32.0481 (14)C1—C21.379 (2)
Co1—O3i2.0481 (14)C2—C31.358 (2)
Co1—N1i2.0812 (15)C3—C41.381 (2)
Co1—N12.0812 (15)C4—C51.382 (3)
O2—C61.409 (2)C5—C61.544 (2)
O2—C14?i1.422 (4)C6—C6i1.562 (3)
O2—C14?1.455 (5)C14?—C14?i0.963 (8)
O3—N41.273 (2)C14?—C151.408 (4)
O4—N41.248 (2)C14?—O2i1.422 (4)
O5—N41.229 (2)C14?—C17?1.549 (5)
N1—C51.327 (2)C15—C14?i1.408 (4)
N1—C11.360 (2)
O3—Co1—O3i128.89 (8)C3—C4—C5119.85 (15)
O3—Co1—N1i94.39 (6)N1—C5—C4121.80 (16)
O3i—Co1—N1i114.38 (6)N1—C5—C6115.90 (14)
O3—Co1—N1114.38 (6)C4—C5—C6122.30 (15)
O3i—Co1—N194.39 (6)O2—C6—C5110.09 (14)
N1i—Co1—N1110.88 (8)O2—C6—C6i104.34 (8)
C6—O2—C14?i108.13 (18)C5—C6—C6i111.58 (17)
C6—O2—C14?107.87 (18)C14?i—C14?—C1570.00 (16)
C14?i—O2—C14?39.1 (3)C14?i—C14?—O2i72.3 (4)
N4—O3—Co1100.33 (11)C15—C14?—O2i113.0 (3)
C5—N1—C1118.20 (15)C14?i—C14?—O268.6 (4)
C5—N1—Co1127.94 (12)C15—C14?—O2111.0 (3)
C1—N1—Co1113.85 (11)O2i—C14?—O2103.6 (2)
O5—N4—O4120.92 (17)C14?i—C14?—C17?176.3 (3)
O5—N4—O3119.79 (17)C15—C14?—C17?106.5 (2)
O4—N4—O3119.27 (15)O2i—C14?—C17?108.7 (3)
N1—C1—C2122.01 (16)O2—C14?—C17?114.2 (3)
C3—C2—C1119.59 (16)C14?i—C15—C14?40.0 (3)
C2—C3—C4118.53 (16)
Symmetry code: (i) x, y, z+1/2.
(claecu) bis(Chloroacetato)-(N,N,N',N'-tetramethylethylenediamine) copper(ii) top
Crystal data top
C10H20Cl2CuN2O4γ = 90°
Mr = 366.72V = 1523.5 (11) Å3
C2221Z = 4
a = 9.002 (3) ÅF(000) = 756
b = 11.400 (5) ÅDx = 1.599 Mg m3
c = 14.846 (7) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 1.79 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.006
Graphite monochromatorθmax = 45.6°, θmin = 2.7°
8366 measured reflectionsh = 1616
2103 independent reflectionsk = 1616
2095 reflections with I > 2σ(I)l = 1414
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.006H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.042 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.25(Δ/σ)max = 1.279
2103 reflectionsΔρmax = 0.10 e Å3
79 parametersΔρmin = 0.16 e Å3
0 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.003 (5)
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
Cu10.000000.103000 (12)0.250000.02000 (4)*
N10.14260 (7)0.02670 (6)0.21200 (5)0.02000 (11)*
C10.08360 (8)0.13590 (7)0.25390 (7)0.02000 (12)*
H10.1257 (15)0.2107 (12)0.2215 (9)0.020 (3)*
H20.1210 (14)0.1400 (12)0.3165 (10)0.020 (3)*
C30.15370 (7)0.04170 (8)0.11320 (6)0.02000 (13)*
H50.1915 (15)0.0310 (11)0.0870 (8)0.020 (3)*
H60.2118 (13)0.1108 (11)0.1010 (9)0.020 (3)*
H70.0608 (14)0.0527 (11)0.0830 (9)0.020 (3)*
C40.29120 (8)0.00080 (7)0.24880 (6)0.02000 (13)*
H80.3248 (14)0.0767 (12)0.2150 (8)0.020 (3)*
H90.3630 (14)0.0630 (12)0.2350 (9)0.020 (3)*
H100.2898 (13)0.0178 (11)0.3085 (9)0.020 (3)*
O10.10440 (6)0.22160 (5)0.17640 (4)0.02000 (10)*
C70.02140 (7)0.23430 (7)0.10700 (6)0.02000 (12)*
C80.08500 (8)0.32340 (8)0.04060 (6)0.02000 (12)*
H170.1833 (13)0.3037 (12)0.0180 (8)0.020 (3)*
H180.0920 (12)0.3990 (13)0.0710 (8)0.020 (3)*
Cl10.025500 (18)0.341600 (17)0.057800 (12)0.02000 (4)*
O20.09550 (6)0.18120 (6)0.09410 (4)0.02000 (11)*
Geometric parameters (Å, º) top
Cu1—O1i1.9761 (8)N1—C11.4895 (12)
Cu1—O11.9762 (8)C1—C1i1.5096 (15)
Cu1—N12.0377 (9)O1—C71.2809 (10)
Cu1—N1i2.0377 (9)C7—O21.2290 (9)
N1—C41.4786 (11)C7—C81.5268 (12)
N1—C31.4801 (14)C8—Cl11.7795 (11)
O1i—Cu1—O193.66 (5)C4—N1—Cu1108.29 (6)
O1i—Cu1—N1161.64 (3)C3—N1—Cu1113.62 (5)
O1—Cu1—N192.51 (4)C1—N1—Cu1105.44 (6)
O1i—Cu1—N1i92.51 (4)N1—C1—C1i108.87 (6)
O1—Cu1—N1i161.64 (3)C7—O1—Cu1104.16 (5)
N1—Cu1—N1i86.96 (5)O2—C7—O1124.69 (8)
C4—N1—C3109.24 (6)O2—C7—C8123.24 (8)
C4—N1—C1110.21 (7)O1—C7—C8112.07 (6)
C3—N1—C1109.96 (7)C7—C8—Cl1113.45 (6)
Symmetry code: (i) x, y, z+1/2.
(qanxos) (syn-rac)-trans-Dichloro-(5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclo- tetradeca-4,11-diene)-cobalt(iii) perchlorate top
Crystal data top
C16Cl3CoN4O4γ = 90°
Mr = 477.48V = 2188.1 (6) Å3
C2221Z = 4
a = 10.621 (2) ÅF(000) = 936
b = 11.624 (2) ÅDx = 1.449 Mg m3
c = 17.723 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 1.18 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.015
Graphite monochromatorθmax = 38.6°, θmin = 2.3°
9520 measured reflectionsh = 1616
2392 independent reflectionsk = 1616
2382 reflections with I > 2σ(I)l = 1616
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)] = 0.002 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.015(Δ/σ)max = 2.138
S = 0.09Δρmax = 0.06 e Å3
2392 reflectionsΔρmin = 0.08 e Å3
65 parametersAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 restraintsAbsolute structure parameter: 0.001 (2)
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)
Co10.321200 (4)0.00000.00000.02000 (2)*
Cl10.533000 (7)0.00000.00000.02000 (2)*
Cl20.109300 (7)0.00000.00000.02000 (2)*
N10.31570 (2)0.068800 (18)0.102200 (14)0.02000 (4)*
N20.32330 (2)0.144600 (19)0.053100 (15)0.02000 (4)*
C10.38630 (2)0.01010 (2)0.152600 (17)0.02000 (5)*
C20.34350 (2)0.13130 (2)0.135500 (16)0.02000 (5)*
C30.30130 (2)0.244700 (19)0.025700 (17)0.02000 (5)*
C40.26390 (2)0.25960 (2)0.054800 (17)0.02000 (5)*
C50.33980 (2)0.19680 (2)0.113500 (17)0.02000 (5)*
C110.30920 (2)0.35280 (2)0.072500 (17)0.02000 (4)*
C120.29180 (2)0.23070 (2)0.192300 (16)0.02000 (4)*
C130.47870 (2)0.22710 (2)0.107700 (17)0.02000 (4)*
Cl30.00000.038400 (6)0.25000.02000 (2)*
O10.00450 (4)0.15920 (3)0.268200 (18)0.02000 (8)*0.50
O20.10430 (3)0.01440 (3)0.27610 (3)0.02000 (7)*0.50
O30.04160 (3)0.01610 (3)0.17900 (2)0.02000 (6)*0.50
O40.11040 (3)0.00660 (3)0.30160 (2)0.02000 (7)*0.50
Geometric parameters (Å, º) top
Co1—N21.9265 (3)C5—C121.5381 (4)
Co1—N2i1.9265 (3)Cl3—O21.3483 (4)
Co1—N11.9808 (3)Cl3—O2ii1.3483 (4)
Co1—N1i1.9808 (3)Cl3—O3ii1.3586 (4)
Co1—Cl12.2495 (4)Cl3—O31.3586 (4)
Co1—Cl22.2506 (4)Cl3—O11.4415 (4)
N1—C11.4837 (4)Cl3—O1ii1.4415 (4)
N1—C5i1.5230 (4)Cl3—O41.5763 (4)
N2—C31.2823 (4)Cl3—O4ii1.5763 (4)
N2—C21.4841 (4)O1—O1ii0.6522 (6)
C1—C21.5111 (4)O2—O3ii1.0965 (6)
C3—C41.4911 (4)O2—O4ii1.3816 (7)
C3—C111.5080 (4)O3—O2ii1.0965 (6)
C4—C51.5050 (4)O3—O4ii1.6716 (6)
C5—C131.5202 (4)O4—O2ii1.3816 (7)
C5—N1i1.5230 (4)O4—O3ii1.6716 (6)
N2—Co1—N2i178.673 (13)O2—Cl3—O3119.88 (2)
N2—Co1—N184.601 (14)O2ii—Cl3—O347.79 (2)
N2i—Co1—N195.439 (13)O3ii—Cl3—O3158.00 (3)
N2—Co1—N1i95.439 (13)O2—Cl3—O1113.20 (2)
N2i—Co1—N1i84.601 (14)O2ii—Cl3—O1119.53 (2)
N1—Co1—N1i176.620 (13)O3ii—Cl3—O189.39 (2)
N2—Co1—Cl189.337 (7)O3—Cl3—O1112.48 (2)
N2i—Co1—Cl189.337 (7)O2—Cl3—O1ii119.53 (2)
N1—Co1—Cl191.690 (6)O2ii—Cl3—O1ii113.20 (2)
N1i—Co1—Cl191.690 (6)O3ii—Cl3—O1ii112.48 (2)
N2—Co1—Cl290.663 (7)O3—Cl3—O1ii89.39 (2)
N2i—Co1—Cl290.663 (7)O1—Cl3—O1ii26.15 (3)
N1—Co1—Cl288.310 (6)O2—Cl3—O4105.13 (2)
N1i—Co1—Cl288.310 (6)O2ii—Cl3—O455.72 (3)
Cl1—Co1—Cl2180.0O3ii—Cl3—O468.98 (2)
C1—N1—C5i116.09 (2)O3—Cl3—O4103.42 (2)
C1—N1—Co1106.621 (18)O1—Cl3—O499.72 (2)
C5i—N1—Co1120.645 (19)O1ii—Cl3—O4118.536 (19)
C3—N2—C2119.57 (2)O2—Cl3—O4ii55.72 (3)
C3—N2—Co1127.20 (2)O2ii—Cl3—O4ii105.13 (2)
C2—N2—Co1113.046 (17)O3ii—Cl3—O4ii103.42 (2)
N1—C1—C2107.67 (2)O3—Cl3—O4ii68.98 (2)
N2—C2—C1109.75 (2)O1—Cl3—O4ii118.536 (19)
N2—C3—C4121.08 (2)O1ii—Cl3—O4ii99.72 (2)
N2—C3—C11122.53 (3)O4—Cl3—O4ii141.24 (3)
C4—C3—C11116.38 (2)O1ii—O1—Cl376.926 (13)
C3—C4—C5117.54 (2)O3ii—O2—Cl366.60 (3)
C4—C5—C13111.14 (2)O3ii—O2—O4ii136.94 (5)
C4—C5—N1i107.03 (2)Cl3—O2—O4ii70.53 (3)
C13—C5—N1i112.37 (2)O2ii—O3—Cl365.61 (3)
C4—C5—C12109.02 (2)O2ii—O3—O4ii112.72 (4)
C13—C5—C12108.89 (2)Cl3—O3—O4ii61.67 (2)
N1i—C5—C12108.30 (2)O2ii—O4—Cl353.75 (2)
O2—Cl3—O2ii125.84 (3)O2ii—O4—O3ii99.79 (3)
O2—Cl3—O3ii47.79 (2)Cl3—O4—O3ii49.348 (19)
O2ii—Cl3—O3ii119.88 (2)
Symmetry codes: (i) x, y, z; (ii) x, y, z+1/2.
(sazpak) Diaqua-(ethylenediamine-N,N')-bis(guanosine 5'-monophosphate-N$7!)-nickel ethylenediamine hydrate top
Crystal data top
C24N14NiO24.50P2γ = 90°
Mr = 997.01V = 8603.1 (15) Å3
C2221Z = 8
a = 17.462 (2) ÅF(000) = 3968
b = 17.337 (2) ÅDx = 1.540 Mg m3
c = 28.417 (2) ÅMo Kα radiation, λ = 0.71073 Å
α = 90°µ = 0.63 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.042
Graphite monochromatorθmax = 27.1°, θmin = 1.4°
14536 measured reflectionsh = 2020
3648 independent reflectionsk = 2020
3605 reflections with I > 2σ(I)l = 1616
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)] = 0.006 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.039(Δ/σ)max = 0.880
S = 0.30Δρmax = 0.16 e Å3
3648 reflectionsΔρmin = 0.21 e Å3
267 parametersAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 restraintsAbsolute structure parameter: 0.010 (5)
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)
Ni10.298650 (15)0.00000.00000.02000 (8)*
P10.23220 (2)0.29400 (2)0.00420 (2)0.02000 (10)*
O10.30327 (5)0.10173 (5)0.04095 (5)0.0200 (2)*
O30.45785 (6)0.12660 (6)0.03725 (5)0.0200 (2)*
O40.42922 (6)0.25003 (6)0.10735 (5)0.0200 (3)*
O50.50230 (6)0.36440 (5)0.01020 (4)0.0200 (2)*
O60.59385 (6)0.29415 (6)0.07580 (5)0.0200 (2)*
O70.30607 (5)0.27387 (6)0.03695 (5)0.0200 (2)*
O80.16992 (5)0.31813 (6)0.03810 (5)0.0200 (2)*
O90.21407 (6)0.21787 (5)0.01960 (4)0.0200 (2)*
O100.25460 (6)0.35565 (5)0.02945 (5)0.0200 (2)*
N10.20748 (7)0.04338 (7)0.04070 (6)0.0200 (3)*
N30.38678 (7)0.03948 (7)0.04695 (6)0.0200 (3)*
N40.56972 (7)0.06397 (7)0.05040 (6)0.0200 (3)*
N50.68965 (7)0.01035 (7)0.06060 (6)0.0200 (3)*
N60.58475 (7)0.06510 (7)0.07595 (6)0.0200 (3)*
N70.46355 (7)0.13165 (7)0.07635 (6)0.0200 (3)*
C10.13870 (8)0.00740 (8)0.02415 (6)0.0200 (4)*
C30.45938 (9)0.00928 (9)0.05435 (7)0.0200 (4)*
C40.48853 (9)0.06447 (8)0.04705 (7)0.0200 (4)*
C50.61263 (8)0.00117 (9)0.06260 (7)0.0200 (3)*
C60.50773 (9)0.06693 (8)0.07015 (7)0.0200 (4)*
C70.39065 (9)0.11185 (8)0.06105 (7)0.0200 (4)*
C80.49200 (9)0.20405 (8)0.09200 (7)0.0200 (3)*
C90.42228 (8)0.31842 (8)0.07590 (7)0.0200 (3)*
C100.46997 (8)0.29792 (8)0.03315 (7)0.0200 (4)*
C110.53510 (8)0.24885 (8)0.05325 (7)0.0200 (3)*
C120.33885 (9)0.33100 (8)0.06725 (7)0.0200 (4)*
Ni20.50000.225350 (14)0.25000.02000 (8)*
P30.22225 (2)0.30960 (2)0.22155 (2)0.02000 (10)*
O190.60582 (5)0.22517 (5)0.21415 (5)0.0200 (2)*
O210.63575 (6)0.07470 (6)0.20845 (5)0.0200 (2)*
O220.25920 (6)0.08675 (5)0.14255 (4)0.0200 (2)*
O230.14867 (5)0.03987 (5)0.24615 (5)0.0200 (2)*
O240.21070 (6)0.07095 (5)0.18450 (5)0.0200 (2)*
O250.23750 (6)0.22365 (6)0.20230 (5)0.0200 (2)*
O260.29385 (5)0.32420 (5)0.24900 (5)0.0200 (2)*
O270.15137 (5)0.30417 (5)0.25170 (5)0.0200 (2)*
O280.21267 (6)0.36298 (5)0.18020 (5)0.0200 (2)*
N170.53875 (7)0.31540 (7)0.29335 (6)0.0200 (3)*
N190.46782 (7)0.13418 (7)0.20245 (6)0.0200 (3)*
N200.58525 (7)0.03820 (7)0.18255 (6)0.0200 (3)*
N210.54817 (7)0.15517 (7)0.14905 (6)0.0200 (3)*
N220.45540 (7)0.06000 (7)0.16135 (6)0.0200 (3)*
N230.37800 (7)0.05455 (7)0.17325 (6)0.0200 (3)*
C270.51533 (8)0.38872 (8)0.27005 (6)0.0200 (4)*
C290.49773 (9)0.06528 (9)0.19280 (6)0.0200 (4)*
C300.57735 (9)0.03755 (9)0.19640 (7)0.0200 (4)*
C310.52692 (8)0.08353 (8)0.16340 (7)0.0200 (4)*
C320.44627 (9)0.01367 (8)0.17370 (7)0.0200 (4)*
C330.39300 (8)0.12660 (9)0.19060 (7)0.0200 (4)*
C340.30295 (9)0.02320 (8)0.15980 (7)0.0200 (3)*
C350.19307 (9)0.09912 (8)0.17240 (7)0.0200 (4)*
C360.21265 (8)0.06035 (8)0.21845 (7)0.0200 (3)*
C370.26145 (8)0.01035 (8)0.20205 (7)0.0200 (4)*
C380.17805 (8)0.18565 (9)0.17510 (7)0.0200 (3)*
N130.14797 (7)0.29833 (7)0.34425 (6)0.0200 (3)*
N140.28272 (7)0.15217 (7)0.37800 (6)0.0200 (3)*
C230.21842 (9)0.26832 (8)0.36460 (7)0.0200 (4)*
C240.22548 (8)0.18463 (8)0.34900 (7)0.0200 (3)*
O480.02962 (11)0.18173 (11)0.36345 (9)0.0200 (5)*0.50
O490.05827 (11)0.23722 (11)0.40845 (10)0.0200 (5)*0.50
O370.38802 (6)0.55832 (6)0.03400 (5)0.0200 (2)*
O390.30772 (5)0.48513 (5)0.16625 (4)0.0200 (2)*
O410.08448 (6)0.19537 (5)0.06830 (5)0.0200 (2)*
O420.05268 (5)0.01863 (5)0.37895 (4)0.0200 (2)*
O450.00000.25415 (8)0.25000.0200 (3)*
O460.57687 (5)0.42682 (5)0.12830 (5)0.0200 (2)*
Geometric parameters (Å, º) top
Ni1—N1i2.1066 (14)Ni2—O19ii2.1100 (11)
Ni1—N12.1066 (14)Ni2—O192.1100 (11)
Ni1—O1i2.1146 (11)Ni2—N192.1541 (14)
Ni1—O12.1146 (11)Ni2—N19ii2.1541 (14)
Ni1—N32.1487 (14)P3—O261.4952 (11)
Ni1—N3i2.1487 (14)P3—O281.5051 (12)
P1—O101.4865 (12)P3—O271.5083 (12)
P1—O81.5119 (13)P3—O251.6096 (11)
P1—O91.5165 (10)O21—C301.2538 (19)
P1—O71.6284 (12)O22—C341.4275 (19)
O3—C41.2349 (19)O22—C351.449 (2)
O4—C81.424 (2)O23—C361.412 (2)
O4—C91.4897 (19)O24—C371.462 (2)
O5—C101.4396 (19)O25—C381.452 (2)
O6—C111.442 (2)N17—C271.4905 (19)
O7—C121.432 (2)N19—C291.332 (2)
N1—C11.433 (2)N19—C331.356 (2)
N3—C71.3189 (19)N20—C301.3779 (19)
N3—C31.388 (2)N20—C311.397 (2)
N4—C51.366 (2)N21—C311.359 (2)
N4—C41.4210 (19)N22—C311.315 (2)
N5—C51.3555 (19)N22—C321.334 (2)
N6—C51.304 (2)N23—C331.368 (2)
N6—C61.355 (2)N23—C321.387 (2)
N7—C61.373 (2)N23—C341.469 (2)
N7—C71.388 (2)C27—C27ii1.259 (3)
N7—C81.4213 (19)C29—C321.379 (3)
C1—C1i1.396 (3)C29—C301.475 (2)
C3—C61.383 (2)C34—C371.518 (3)
C3—C41.392 (2)C35—C361.510 (3)
C8—C111.543 (3)C35—C381.5249 (19)
C9—C121.493 (2)C36—C371.564 (2)
C9—C101.515 (3)N13—C231.456 (2)
C10—C111.531 (2)N14—C241.412 (2)
Ni2—N172.1007 (14)C23—C241.522 (2)
Ni2—N17ii2.1007 (14)O48—O491.677 (3)
N1i—Ni1—N181.82 (8)N17—Ni2—O19ii90.00 (5)
N1i—Ni1—O1i91.90 (5)N17ii—Ni2—O19ii90.12 (5)
N1—Ni1—O1i91.40 (5)N17—Ni2—O1990.12 (5)
N1i—Ni1—O191.40 (5)N17ii—Ni2—O1990.00 (5)
N1—Ni1—O191.90 (5)O19ii—Ni2—O19179.83 (6)
O1i—Ni1—O1175.63 (5)N17—Ni2—N19175.75 (5)
N1i—Ni1—N3174.81 (6)N17ii—Ni2—N1995.36 (5)
N1—Ni1—N394.97 (5)O19ii—Ni2—N1994.21 (5)
O1i—Ni1—N384.07 (5)O19—Ni2—N1985.67 (5)
O1—Ni1—N392.79 (5)N17—Ni2—N19ii95.36 (5)
N1i—Ni1—N3i94.97 (5)N17ii—Ni2—N19ii175.75 (5)
N1—Ni1—N3i174.81 (6)O19ii—Ni2—N19ii85.67 (5)
O1i—Ni1—N3i92.79 (5)O19—Ni2—N19ii94.21 (5)
O1—Ni1—N3i84.07 (5)N19—Ni2—N19ii85.59 (8)
N3—Ni1—N3i88.51 (8)O26—P3—O28113.34 (6)
O10—P1—O8113.59 (6)O26—P3—O27113.60 (8)
O10—P1—O9113.19 (7)O28—P3—O27113.00 (6)
O8—P1—O9112.01 (6)O26—P3—O25101.29 (6)
O10—P1—O7108.26 (6)O28—P3—O25108.80 (7)
O8—P1—O7105.36 (7)O27—P3—O25105.73 (6)
O9—P1—O7103.52 (6)C34—O22—C35109.86 (12)
C8—O4—C9108.93 (13)C38—O25—P3118.86 (9)
C12—O7—P1120.80 (9)C27—N17—Ni2106.56 (10)
C1—N1—Ni1107.33 (10)C29—N19—C33103.87 (13)
C7—N3—C3105.43 (13)C29—N19—Ni2133.22 (12)
C7—N3—Ni1121.90 (11)C33—N19—Ni2118.58 (11)
C3—N3—Ni1128.92 (11)C30—N20—C31125.07 (13)
C5—N4—C4124.68 (14)C31—N22—C32113.50 (13)
C5—N6—C6110.83 (14)C33—N23—C32107.38 (13)
C6—N7—C7105.84 (12)C33—N23—C34127.03 (12)
C6—N7—C8124.44 (12)C32—N23—C34125.45 (12)
C7—N7—C8129.56 (12)C27ii—C27—N17121.25 (9)
C1i—C1—N1113.75 (11)N19—C29—C32114.03 (14)
C6—C3—N3109.52 (13)N19—C29—C30130.36 (14)
C6—C3—C4119.27 (14)C32—C29—C30115.47 (14)
N3—C3—C4131.16 (14)O21—C30—N20119.09 (14)
O3—C4—C3132.56 (13)O21—C30—C29128.19 (13)
O3—C4—N4116.95 (14)N20—C30—C29112.66 (14)
C3—C4—N4110.45 (13)N22—C31—N21121.97 (14)
N6—C5—N5119.08 (15)N22—C31—N20122.36 (14)
N6—C5—N4124.82 (13)N21—C31—N20115.60 (13)
N5—C5—N4116.10 (15)N22—C32—C29130.29 (15)
N6—C6—N7124.13 (14)N22—C32—N23126.12 (15)
N6—C6—C3128.92 (16)C29—C32—N23103.42 (13)
N7—C6—C3106.81 (13)N19—C33—N23111.26 (13)
N3—C7—N7112.17 (13)O22—C34—N23106.33 (11)
N7—C8—O4108.73 (11)O22—C34—C37108.17 (12)
N7—C8—C11113.06 (16)N23—C34—C37111.21 (15)
O4—C8—C11108.19 (12)O22—C35—C36105.13 (12)
O4—C9—C12107.12 (12)O22—C35—C38108.19 (13)
O4—C9—C10104.45 (12)C36—C35—C38115.67 (16)
C12—C9—C10116.00 (16)O23—C36—C35114.57 (13)
O5—C10—C9113.01 (12)O23—C36—C37113.59 (12)
O5—C10—C11108.82 (11)C35—C36—C37102.36 (15)
C9—C10—C11103.86 (15)O24—C37—C34107.15 (15)
O6—C11—C10113.06 (12)O24—C37—C36109.55 (11)
O6—C11—C8107.69 (15)C34—C37—C36101.27 (13)
C10—C11—C8100.58 (13)O25—C38—C35110.50 (13)
O7—C12—C9112.83 (13)N13—C23—C24107.07 (14)
N17—Ni2—N17ii83.99 (8)N14—C24—C23105.50 (15)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z+1/2.
(yakvip) catena-(mu!2$-Aqua)bis(diaqua-(mu!3$-beta-N-oxalyl-L-alpha,beta-diaminopropionic acid)-sodium) trihydrate top
Crystal data top
C5H15N2NaO9γ = 90°
Mr = 270.18V = 2268.9 (6) Å3
C2221Z = 8
a = 9.453 (2) ÅF(000) = 1136
b = 17.812 (2) ÅDx = 1.582 Mg m3
c = 13.475 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 0.18 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.013
Graphite monochromatorθmax = 67.7°, θmin = 2.3°
18110 measured reflectionsh = 1212
5671 independent reflectionsk = 3636
4802 reflections with I > 2σ(I)l = 1414
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.009H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.057 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.25(Δ/σ)max = 3.198
5671 reflectionsΔρmax = 0.08 e Å3
113 parametersΔρmin = 0.21 e Å3
0 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.06 (8)
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)
Na10.46230 (2)0.130200 (8)0.088100 (15)0.02000 (3)*
N10.53650 (4)0.379200 (17)0.11550 (3)0.02000 (5)*
H130.6197 (9)0.3554 (5)0.1107 (7)0.0200 (16)*
N20.45060 (4)0.338300 (16)0.07680 (3)0.02000 (5)*
H10.5118 (9)0.2966 (5)0.0634 (6)0.0200 (16)*
H20.4028 (9)0.3303 (4)0.1389 (6)0.0200 (17)*
H30.5056 (9)0.3835 (4)0.0806 (6)0.0200 (16)*
O10.78280 (3)0.449700 (15)0.14750 (3)0.02000 (4)*
O20.68190 (3)0.559500 (15)0.11080 (3)0.02000 (4)*
O30.42420 (3)0.491600 (15)0.12270 (3)0.02000 (5)*
O40.12600 (3)0.279900 (15)0.03880 (3)0.02000 (4)*
O50.27360 (3)0.220900 (14)0.06470 (3)0.02000 (4)*
C10.67960 (4)0.490300 (18)0.12760 (4)0.02000 (5)*
C20.53260 (4)0.453400 (19)0.12160 (3)0.02000 (5)*
C30.41030 (5)0.333100 (19)0.10470 (4)0.02000 (5)*
H70.4419 (8)0.2783 (5)0.1174 (7)0.0200 (17)*
H80.3425 (9)0.3473 (5)0.1533 (6)0.0200 (17)*
C40.34080 (4)0.339700 (19)0.00240 (4)0.02000 (6)*
H90.2876 (8)0.3890 (4)0.0064 (6)0.0200 (17)*
C50.23740 (4)0.27410 (2)0.01060 (4)0.02000 (5)*
O110.80390 (3)0.181500 (15)0.25850 (3)0.02000 (5)*
O120.46930 (3)0.088300 (15)0.08200 (3)0.02000 (5)*
H160.3743 (9)0.0718 (4)0.0807 (6)0.0200 (17)*
H170.5124 (9)0.0450 (4)0.0945 (6)0.0200 (16)*
O140.00000.31080 (2)0.25000.02000 (6)*
O150.63510 (3)0.033400 (16)0.14920 (3)0.02000 (4)*
H200.7289 (16)0.0273 (9)0.1345 (12)0.020 (3)*0.50
H210.6519 (17)0.0227 (9)0.2164 (13)0.020 (3)*0.50
O180.50000.17990 (2)0.25000.02000 (6)*
Geometric parameters (Å, º) top
Na1—O4i2.3238 (4)O2—C11.2534 (4)
Na1—O1ii2.3548 (4)O3—C21.2301 (5)
Na1—O122.4114 (5)O4—C51.2501 (5)
Na1—O52.4272 (4)O4—Na1ii2.3238 (4)
Na1—O14i2.4476 (4)O5—C51.2436 (5)
Na1—O152.5138 (4)C1—C21.5393 (6)
N1—C21.3247 (5)C3—C41.5316 (7)
N1—C31.4555 (6)C4—C51.5334 (5)
N2—C41.4889 (7)O14—Na1ii2.4476 (4)
O1—C11.2436 (5)O14—Na1iii2.4476 (4)
O1—Na1i2.3548 (4)
O4i—Na1—O1ii173.443 (13)C5—O4—Na1ii140.37 (3)
O4i—Na1—O1285.599 (14)C5—O5—Na1141.77 (3)
O1ii—Na1—O1298.964 (14)O1—C1—O2126.67 (4)
O4i—Na1—O589.633 (17)O1—C1—C2118.11 (3)
O1ii—Na1—O585.231 (17)O2—C1—C2115.22 (3)
O12—Na1—O595.894 (13)O3—C2—N1125.15 (4)
O4i—Na1—O14i82.067 (13)O3—C2—C1121.01 (3)
O1ii—Na1—O14i93.523 (14)N1—C2—C1113.84 (3)
O12—Na1—O14i167.446 (12)N1—C3—C4113.47 (3)
O5—Na1—O14i86.389 (13)N2—C4—C3110.17 (4)
O4i—Na1—O1597.675 (18)N2—C4—C5110.47 (4)
O1ii—Na1—O1586.696 (17)C3—C4—C5108.53 (3)
O12—Na1—O1594.658 (14)O5—C5—O4127.37 (4)
O5—Na1—O15167.593 (15)O5—C5—C4118.18 (4)
O14i—Na1—O1584.719 (13)O4—C5—C4114.40 (4)
C2—N1—C3123.11 (3)Na1ii—O14—Na1iii129.146 (19)
C1—O1—Na1i147.50 (3)
Symmetry codes: (i) x+1/2, y1/2, z; (ii) x1/2, y1/2, z; (iii) x+1/2, y1/2, z+1/2.
(bogpiw) Dicarbonyl-(eta$5!-cyclopentadienyl)-(sulfur dioxide)-iron(iii) hexafluoroarsenate top
Crystal data top
C7H5AsF6FeO4Sγ = 90°
Mr = 429.94V = 1265.9 (5) Å3
Cmc21Z = 4
a = 8.068 (2) ÅF(000) = 832
b = 13.904 (4) ÅDx = 2.256 Mg m3
c = 11.285 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 4.03 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.023
Graphite monochromatorθmax = 53.1°, θmin = 2.9°
7020 measured reflectionsh = 1616
1916 independent reflectionsk = 1616
1903 reflections with I > 2σ(I)l = 1212
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.005H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.024 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.15(Δ/σ)max = 2.807
1916 reflectionsΔρmax = 0.19 e Å3
60 parametersΔρmin = 0.27 e Å3
1 restraintAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.0108 (18)
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
Fe10.00000.184900 (11)0.257400 (13)0.02000 (3)*
As10.50000.072700 (7)0.063800 (9)0.02000 (2)*
F10.50000.05280 (5)0.08470 (5)0.02000 (10)*
F20.35070 (4)0.16060 (3)0.04350 (4)0.02000 (7)*
F30.34890 (4)0.01220 (3)0.08470 (4)0.02000 (7)*
F50.50000.09780 (5)0.21090 (5)0.02000 (9)*
S10.00000.172300 (17)0.07120 (2)0.02000 (4)*
O10.00000.08190 (5)0.01370 (7)0.02000 (10)*
O20.00000.25750 (5)0.00080 (7)0.02000 (10)*
C10.13670 (7)0.10800 (6)0.38110 (6)0.02000 (9)*
C20.00000.14200 (7)0.43320 (9)0.02000 (14)*
C50.08820 (6)0.04820 (6)0.29260 (6)0.02000 (9)*
C60.16640 (6)0.27390 (5)0.25760 (7)0.02000 (9)*
O30.27090 (5)0.32580 (3)0.26000 (5)0.02000 (8)*
H10.2489 (12)0.1230 (5)0.4023 (9)0.020 (3)*
H20.00000.1852 (9)0.4994 (14)0.020 (4)*
H50.1592 (12)0.0127 (7)0.2401 (8)0.020 (2)*
Geometric parameters (Å, º) top
Fe1—C61.8258 (7)As1—F3ii1.7133 (5)
Fe1—C6i1.8258 (7)As1—F2ii1.7312 (5)
Fe1—C52.0680 (10)As1—F21.7312 (5)
Fe1—C5i2.0680 (10)S1—O11.4145 (9)
Fe1—C22.0716 (11)S1—O21.4264 (9)
Fe1—C12.0756 (8)C1—C21.3362 (9)
Fe1—C1i2.0756 (8)C1—C51.3572 (10)
Fe1—S12.1086 (5)C2—C1i1.3362 (9)
As1—F51.6963 (7)C5—C5i1.4232 (11)
As1—F11.6985 (7)C6—O31.1101 (8)
As1—F31.7133 (5)
C6—Fe1—C6i94.66 (4)F5—As1—F1177.50 (3)
C6—Fe1—C5111.69 (3)F5—As1—F390.40 (2)
C6i—Fe1—C5151.13 (3)F1—As1—F391.35 (2)
C6—Fe1—C5i151.13 (3)F5—As1—F3ii90.40 (2)
C6i—Fe1—C5i111.69 (3)F1—As1—F3ii91.35 (2)
C5—Fe1—C5i40.25 (3)F3—As1—F3ii90.72 (3)
C6—Fe1—C2101.18 (3)F5—As1—F2ii89.10 (2)
C6i—Fe1—C2101.18 (3)F1—As1—F2ii89.11 (2)
C5—Fe1—C263.35 (3)F3—As1—F2ii178.639 (18)
C5i—Fe1—C263.35 (3)F3ii—As1—F2ii90.55 (3)
C6—Fe1—C187.57 (3)F5—As1—F289.10 (2)
C6i—Fe1—C1137.65 (3)F1—As1—F289.11 (2)
C5—Fe1—C138.24 (3)F3—As1—F290.55 (3)
C5i—Fe1—C165.18 (3)F3ii—As1—F2178.639 (18)
C2—Fe1—C137.59 (2)F2ii—As1—F288.18 (3)
C6—Fe1—C1i137.65 (3)O1—S1—O2118.85 (5)
C6i—Fe1—C1i87.57 (3)O1—S1—Fe1122.07 (4)
C5—Fe1—C1i65.18 (3)O2—S1—Fe1119.08 (4)
C5i—Fe1—C1i38.24 (3)C2—C1—C5107.61 (6)
C2—Fe1—C1i37.59 (2)C2—C1—Fe171.04 (5)
C1—Fe1—C1i64.19 (4)C5—C1—Fe170.58 (5)
C6—Fe1—S193.30 (2)C1i—C2—C1111.25 (9)
C6i—Fe1—S193.30 (2)C1i—C2—Fe171.37 (5)
C5—Fe1—S196.61 (2)C1—C2—Fe171.37 (5)
C5i—Fe1—S196.61 (2)C1—C5—C5i106.76 (3)
C2—Fe1—S1158.50 (3)C1—C5—Fe171.19 (5)
C1—Fe1—S1128.86 (2)C5i—C5—Fe169.874 (17)
C1i—Fe1—S1128.86 (2)O3—C6—Fe1177.51 (6)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z.
(novhub) bis(mu!2$-bis(Diphenylphosphino)methane)-(mu!2$-nitrato)-dipyridyl-di-copper(i) nitrate methanol solvate top
Crystal data top
C61H58Cu2N4O7P4γ = 90°
Mr = 1210.07V = 5738.7 (11) Å3
Cmc21Z = 4
a = 21.719 (2) ÅF(000) = 2504
b = 16.545 (2) ÅDx = 1.401 Mg m3
c = 15.970 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 0.91 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.030
Graphite monochromatorθmax = 30.4°, θmin = 1.6°
10772 measured reflectionsh = 2020
2892 independent reflectionsk = 2020
2853 reflections with I > 2σ(I)l = 1212
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.011H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.046 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.34(Δ/σ)max = 1.469
2892 reflectionsΔρmax = 0.52 e Å3
275 parametersΔρmin = 0.21 e Å3
1 restraintAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.007 (5)
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
Cu10.084100 (12)0.681600 (11)0.070900 (15)0.02000 (8)*
X10.53100 (8)0.60450 (6)0.10790 (9)0.0200 (3)*
P10.07030 (3)0.81640 (2)0.06450 (4)0.02000 (13)*
P20.07070 (2)0.60340 (2)0.18580 (3)0.02000 (12)*
O30.00000.80850 (9)0.33590 (12)0.0200 (4)*
O40.04960 (7)0.62480 (7)0.04300 (8)0.0200 (3)*
O50.04850 (7)0.82290 (6)0.45130 (8)0.0200 (3)*
O60.00000.52200 (8)0.08560 (10)0.0200 (4)*
N10.00000.59110 (11)0.05750 (13)0.0200 (5)*
N20.00000.81740 (10)0.41360 (15)0.0200 (5)*
N40.17600 (8)0.65570 (8)0.03470 (9)0.0200 (3)*
C20.00000.61560 (14)0.24780 (17)0.0200 (5)*
C30.00000.86000 (13)0.11030 (18)0.0200 (6)*
C40.22180 (10)0.68860 (9)0.07670 (13)0.0200 (4)*
C50.07830 (9)0.86620 (11)0.03580 (13)0.0200 (4)*
C60.28260 (10)0.66730 (10)0.06600 (13)0.0200 (4)*
C70.07600 (9)0.95010 (11)0.04500 (13)0.0200 (4)*
C80.29610 (12)0.60910 (10)0.00880 (11)0.0200 (4)*
C90.08310 (9)0.98530 (11)0.12300 (13)0.0200 (4)*
C100.25020 (9)0.57390 (9)0.03560 (12)0.0200 (4)*
C110.09290 (10)0.93850 (10)0.19140 (13)0.0200 (4)*
C120.19020 (10)0.59870 (9)0.02220 (13)0.0200 (4)*
C130.09540 (10)0.85610 (10)0.18420 (13)0.0200 (4)*
C140.08790 (10)0.81970 (9)0.10600 (16)0.0200 (5)*
C150.13220 (10)0.86050 (9)0.12740 (12)0.0200 (4)*
C160.18450 (9)0.89290 (9)0.09120 (13)0.0200 (4)*
C170.23560 (11)0.91110 (11)0.13990 (12)0.0200 (4)*
C180.23490 (11)0.89860 (9)0.22370 (12)0.0200 (4)*
C190.18310 (10)0.86830 (9)0.26150 (13)0.0200 (4)*
C200.13180 (11)0.84930 (10)0.21410 (12)0.0200 (4)*
C210.07850 (9)0.49490 (10)0.17160 (12)0.0200 (4)*
C220.07980 (10)0.46300 (10)0.09130 (13)0.0200 (4)*
C230.08290 (9)0.37960 (10)0.08130 (15)0.0200 (4)*
C240.08610 (10)0.33050 (11)0.14740 (14)0.0200 (5)*
C250.08680 (10)0.36090 (11)0.22710 (13)0.0200 (4)*
C260.08260 (9)0.44350 (11)0.23900 (15)0.0200 (4)*
C270.13110 (10)0.62360 (10)0.26460 (11)0.0200 (4)*
C280.18930 (9)0.59360 (9)0.24910 (12)0.0200 (4)*
C290.23720 (10)0.61230 (9)0.30290 (11)0.0200 (4)*
C300.22740 (11)0.66010 (10)0.37120 (12)0.0200 (4)*
C310.16970 (11)0.68970 (9)0.38750 (12)0.0200 (4)*
C320.12170 (12)0.67090 (9)0.33390 (12)0.0200 (4)*
H10.0693 (10)0.9834 (11)0.0047 (14)0.020 (5)*
H20.0812 (9)1.0451 (12)0.1264 (15)0.020 (5)*
H30.0960 (10)0.9649 (10)0.2458 (14)0.020 (6)*
H40.1042 (11)0.8227 (10)0.2330 (14)0.020 (6)*
H50.0905 (9)0.7605 (10)0.1002 (13)0.020 (5)*
H60.1848 (9)0.9048 (10)0.0313 (14)0.020 (5)*
H70.2717 (10)0.9339 (10)0.1132 (12)0.020 (5)*
H80.2719 (10)0.9074 (10)0.2567 (13)0.020 (5)*
H90.1816 (9)0.8616 (10)0.3229 (13)0.020 (5)*
H100.0953 (11)0.8273 (10)0.2412 (16)0.020 (6)*
H110.0781 (8)0.4988 (12)0.0431 (13)0.020 (5)*
H120.0844 (9)0.3558 (11)0.0272 (15)0.020 (5)*
H130.0857 (9)0.2731 (13)0.1378 (12)0.020 (5)*
H140.0912 (10)0.3229 (10)0.2753 (15)0.020 (6)*
H150.0823 (9)0.4666 (11)0.2962 (14)0.020 (6)*
H160.1957 (9)0.5610 (10)0.1994 (12)0.020 (5)*
H170.2781 (10)0.5877 (10)0.2905 (11)0.020 (5)*
H180.2628 (10)0.6710 (11)0.4067 (13)0.020 (5)*
H190.1630 (9)0.7245 (10)0.4371 (11)0.020 (4)*
H200.0795 (10)0.6917 (12)0.3464 (15)0.020 (6)*
H460.2118 (10)0.7316 (10)0.1169 (12)0.020 (5)*
H470.3149 (9)0.6926 (10)0.1019 (12)0.020 (5)*
H480.3387 (11)0.5934 (10)0.0027 (11)0.020 (5)*
H490.2597 (9)0.5316 (10)0.0777 (12)0.020 (5)*
H500.1567 (10)0.5731 (9)0.0546 (11)0.020 (5)*
H510.00000.5760 (14)0.2929 (17)0.020 (6)*
H520.00000.6680 (14)0.2738 (16)0.020 (7)*
H530.00000.8514 (14)0.1698 (19)0.020 (7)*
H540.00000.9180 (14)0.1013 (16)0.020 (7)*
Geometric parameters (Å, º) top
Cu1—N42.1217 (17)C7—C91.384 (3)
Cu1—O42.1802 (13)C8—C101.355 (3)
Cu1—P12.2526 (5)C9—C111.356 (3)
Cu1—P22.2640 (6)C10—C121.383 (3)
X1—X1i1.347 (3)C11—C131.369 (2)
P1—C51.810 (2)C13—C141.396 (3)
P1—C151.830 (2)C15—C161.383 (3)
P1—C31.8403 (15)C15—C201.397 (3)
P2—C211.8173 (18)C16—C171.388 (3)
P2—C21.8382 (15)C17—C181.354 (3)
P2—C271.848 (2)C18—C191.372 (3)
O3—N21.250 (3)C19—C201.383 (3)
O4—N11.2349 (16)C21—C261.375 (3)
O5—N21.2167 (18)C21—C221.387 (3)
O6—N11.228 (2)C22—C231.391 (2)
N1—O4ii1.2349 (16)C23—C241.334 (3)
N2—O5ii1.2167 (18)C24—C251.369 (3)
N4—C41.317 (3)C25—C261.383 (2)
N4—C121.345 (2)C27—C321.371 (3)
C2—P2ii1.8382 (15)C27—C281.380 (3)
C3—P1ii1.8403 (15)C28—C291.384 (3)
C4—C61.377 (3)C29—C301.364 (3)
C5—C141.376 (3)C30—C311.370 (3)
C5—C71.397 (2)C31—C321.384 (3)
C6—C81.359 (3)
N4—Cu1—O490.51 (6)C8—C6—C4118.1 (2)
N4—Cu1—P1108.23 (4)C9—C7—C5120.60 (18)
O4—Cu1—P1110.07 (3)C10—C8—C6119.8 (2)
N4—Cu1—P2103.08 (4)C11—C9—C7120.16 (16)
O4—Cu1—P2112.69 (3)C8—C10—C12119.00 (17)
P1—Cu1—P2125.84 (2)C9—C11—C13120.5 (2)
C5—P1—C15103.52 (9)N4—C12—C10121.90 (19)
C5—P1—C3104.65 (11)C11—C13—C14120.00 (18)
C15—P1—C3103.60 (10)C5—C14—C13120.36 (15)
C5—P1—Cu1118.57 (6)C16—C15—C20118.1 (2)
C15—P1—Cu1105.79 (6)C16—C15—P1121.91 (15)
C3—P1—Cu1118.72 (7)C20—C15—P1119.12 (17)
C21—P2—C2104.69 (10)C15—C16—C17120.4 (2)
C21—P2—C27101.39 (8)C18—C17—C16120.8 (2)
C2—P2—C27101.90 (9)C17—C18—C19120.0 (2)
C21—P2—Cu1116.83 (7)C18—C19—C20120.19 (19)
C2—P2—Cu1118.76 (8)C19—C20—C15120.5 (2)
C27—P2—Cu1110.93 (6)C26—C21—C22119.16 (16)
N1—O4—Cu1130.61 (12)C26—C21—P2121.29 (14)
O6—N1—O4119.26 (9)C22—C21—P2119.55 (13)
O6—N1—O4ii119.26 (9)C21—C22—C23118.99 (18)
O4—N1—O4ii121.46 (18)C24—C23—C22121.1 (2)
O5—N2—O5ii119.9 (2)C23—C24—C25120.85 (18)
O5—N2—O3120.01 (12)C24—C25—C26119.36 (18)
O5ii—N2—O3120.01 (12)C21—C26—C25120.53 (19)
C4—N4—C12117.41 (18)C32—C27—C28119.11 (18)
C4—N4—Cu1119.22 (13)C32—C27—P2123.18 (17)
C12—N4—Cu1122.77 (13)C28—C27—P2117.57 (13)
P2ii—C2—P2113.30 (14)C27—C28—C29119.77 (17)
P1—C3—P1ii112.13 (13)C30—C29—C28120.6 (2)
N4—C4—C6123.71 (17)C29—C30—C31120.12 (19)
C14—C5—C7118.39 (19)C30—C31—C32119.40 (18)
C14—C5—P1118.77 (14)C27—C32—C31121.0 (2)
C7—C5—P1122.83 (15)
Symmetry codes: (i) x+1, y, z; (ii) x, y, z.
(nohned) 1,1'-Dihydroxy-2,2'-(1,4,7,10-tetraoxadeca-1,10-diyl)-6,6'-(2,5-diazahexa-1,5- -diene-1,6-diyl)dibenzene top
Crystal data top
C22N2O6γ = 90°
Mr = 388.24V = 2174.1 (7) Å3
P212121Z = 4
a = 12.148 (2) ÅF(000) = 776
b = 8.251 (2) ÅDx = 1.186 Mg m3
c = 21.690 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 0.09 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.021
Graphite monochromatorθmax = 32.9°, θmin = 1.9°
12290 measured reflectionsh = 1212
3081 independent reflectionsk = 88
3050 reflections with I > 2σ(I)l = 1414
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)] = 0.019 w = 1/[σ2(Fo2) + (0.P)2 + 0.0178P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.077(Δ/σ)max = 0.745
S = 0.63Δρmax = 0.59 e Å3
3081 reflectionsΔρmin = 0.58 e Å3
121 parametersAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 restraintsAbsolute structure parameter: 0.1 (6)
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
O10.48470 (7)0.01990 (11)0.07400 (5)0.0200 (2)*
O20.49230 (7)0.11310 (11)0.09220 (5)0.0200 (2)*
O30.64660 (7)0.02390 (11)0.16910 (5)0.0200 (2)*
O40.81390 (7)0.02970 (11)0.07060 (5)0.0200 (2)*
O50.85960 (7)0.04990 (11)0.06020 (5)0.0200 (2)*
O60.67100 (7)0.04800 (11)0.13490 (5)0.0200 (2)*
C10.60760 (11)0.14270 (15)0.21420 (8)0.0200 (3)*
C20.52320 (10)0.24260 (15)0.23560 (8)0.0200 (3)*
C30.42490 (11)0.25420 (16)0.20260 (7)0.0200 (3)*
C40.41100 (10)0.16610 (16)0.14840 (8)0.0200 (3)*
C50.49550 (11)0.06610 (15)0.12700 (8)0.0200 (3)*
C60.59380 (10)0.05450 (15)0.15990 (8)0.0200 (3)*
C70.31010 (10)0.18380 (16)0.11490 (8)0.0200 (3)*
N10.29180 (9)0.10300 (13)0.06330 (6)0.0200 (2)*
C80.18870 (10)0.12040 (15)0.02970 (8)0.0200 (3)*
C90.19740 (10)0.22580 (15)0.02480 (8)0.0200 (3)*
N20.28900 (9)0.16300 (13)0.06720 (7)0.0200 (2)*
C100.26260 (11)0.10710 (15)0.11970 (8)0.0200 (3)*
C110.31460 (10)0.01900 (15)0.21840 (8)0.0200 (3)*
C120.39290 (11)0.08680 (15)0.25770 (8)0.0200 (3)*
C130.50370 (11)0.08770 (15)0.24090 (8)0.0200 (3)*
C140.53630 (10)0.02060 (15)0.18470 (8)0.0200 (3)*
C150.45790 (10)0.04730 (16)0.14540 (8)0.0200 (3)*
C160.34710 (10)0.04800 (16)0.16230 (8)0.0200 (3)*
C170.66970 (11)0.15400 (15)0.12900 (8)0.0200 (3)*
C180.79130 (11)0.16050 (15)0.11140 (8)0.0200 (3)*
C190.92230 (10)0.03700 (16)0.04360 (8)0.0200 (3)*
C200.92130 (11)0.14000 (15)0.01580 (8)0.0200 (3)*
C210.85090 (10)0.13690 (15)0.11630 (8)0.0200 (3)*
C220.78000 (10)0.04060 (16)0.15820 (8)0.0200 (3)*
Geometric parameters (Å, º) top
O1—C51.3573 (18)C5—C61.3944 (19)
O2—C151.3420 (17)C7—N11.322 (2)
O3—C141.3823 (16)N1—C81.4562 (18)
O3—C171.4098 (18)C8—C91.471 (2)
O4—C181.4224 (18)C9—N21.5338 (18)
O4—C191.4425 (16)N2—C101.270 (2)
O5—C211.4167 (19)C10—C161.465 (2)
O5—C201.4290 (17)C11—C161.394 (2)
O6—C61.3743 (16)C11—C121.394 (2)
O6—C221.4186 (16)C12—C131.3945 (19)
C1—C61.395 (2)C13—C141.396 (2)
C1—C21.3950 (18)C14—C151.396 (2)
C2—C31.396 (2)C15—C161.3950 (19)
C3—C41.392 (2)C17—C181.5267 (19)
C4—C51.3964 (18)C19—C201.543 (2)
C4—C71.4324 (18)C21—C221.483 (2)
C14—O3—C17111.04 (11)C10—N2—C9118.50 (11)
C18—O4—C19113.40 (10)N2—C10—C16120.64 (12)
C21—O5—C20110.75 (10)C16—C11—C12119.98 (12)
C6—O6—C22118.03 (11)C11—C12—C13120.06 (15)
C6—C1—C2120.07 (13)C12—C13—C14119.99 (14)
C1—C2—C3119.92 (15)O3—C14—C15121.33 (13)
C4—C3—C2120.07 (12)O3—C14—C13118.74 (13)
C3—C4—C5120.00 (13)C15—C14—C13119.93 (12)
C3—C4—C7118.61 (12)O2—C15—C16121.65 (13)
C5—C4—C7121.38 (15)O2—C15—C14118.37 (12)
O1—C5—C6118.71 (12)C16—C15—C14119.98 (14)
O1—C5—C4121.29 (12)C11—C16—C15120.07 (14)
C6—C5—C4120.00 (15)C11—C16—C10118.97 (12)
O6—C6—C5115.13 (14)C15—C16—C10120.79 (15)
O6—C6—C1124.91 (12)O3—C17—C18111.94 (11)
C5—C6—C1119.96 (12)O4—C18—C17108.40 (11)
N1—C7—C4121.47 (12)O4—C19—C20110.78 (10)
C7—N1—C8121.25 (11)O5—C20—C19106.27 (10)
N1—C8—C9113.49 (11)O5—C21—C22107.35 (11)
C8—C9—N2109.52 (10)O6—C22—C21107.50 (12)
(nohned01) (1$2!,8$2!-Dihydroxy-1,8(1,3)-dibenzena-1,6-diaza-9,12,15,18-tetraoxacyclooctade caphane-2,6-diene) top
Crystal data top
C22H26N2O6γ = 90°
Mr = 414.45V = 2174.1 (7) Å3
P212121Z = 4
a = 12.148 (2) ÅF(000) = 880
b = 8.251 (2) ÅDx = 1.266 Mg m3
c = 21.690 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 0.09 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.022
Graphite monochromatorθmax = 30.5°, θmin = 1.9°
10320 measured reflectionsh = 1010
2588 independent reflectionsk = 88
2565 reflections with I > 2σ(I)l = 1414
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.019H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.081 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.51(Δ/σ)max = 9.439
2588 reflectionsΔρmax = 0.07 e Å3
217 parametersΔρmin = 0.29 e Å3
0 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.0 (7)
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
O10.48390 (8)0.01970 (12)0.07450 (6)0.0200 (2)*
O20.49260 (9)0.11210 (11)0.09210 (6)0.0200 (2)*
O30.64640 (9)0.02470 (11)0.16880 (6)0.0200 (2)*
O40.81450 (9)0.02870 (12)0.07080 (6)0.0200 (2)*
O50.86010 (9)0.05030 (12)0.06020 (6)0.0200 (2)*
O60.67050 (9)0.04680 (12)0.13530 (6)0.0200 (3)*
C10.60720 (15)0.14240 (16)0.21400 (9)0.0200 (3)*
H10.6733 (16)0.135 (2)0.2359 (9)0.020 (5)*
C20.52340 (13)0.24270 (17)0.23510 (10)0.0200 (3)*
H20.5334 (15)0.302 (2)0.2712 (9)0.020 (4)*
C30.42550 (14)0.25450 (17)0.20230 (9)0.0200 (3)*
H30.3697 (14)0.322 (2)0.2164 (8)0.020 (4)*
C40.41140 (12)0.16610 (17)0.14830 (9)0.0200 (3)*
C50.49520 (13)0.06580 (17)0.12720 (9)0.0200 (3)*
C60.59320 (13)0.05400 (17)0.16000 (9)0.0200 (3)*
C70.30960 (13)0.18270 (18)0.11430 (9)0.0200 (3)*
H40.2553 (15)0.2519 (19)0.1292 (9)0.020 (4)*
N10.29210 (11)0.10370 (14)0.06340 (7)0.0200 (3)*
C80.18920 (14)0.12110 (17)0.02990 (9)0.0200 (3)*
H50.1639 (13)0.014 (2)0.0176 (9)0.020 (4)*
H60.1343 (14)0.167 (2)0.0573 (9)0.020 (4)*
C90.19760 (14)0.22340 (17)0.02510 (9)0.0200 (3)*
H70.1279 (14)0.223 (2)0.0469 (9)0.020 (4)*
H80.2134 (14)0.334 (2)0.0129 (9)0.020 (4)*
N20.28830 (11)0.16210 (14)0.06770 (7)0.0200 (3)*
C100.26340 (15)0.10710 (16)0.11960 (9)0.0200 (3)*
H90.1897 (15)0.103 (2)0.1313 (8)0.020 (4)*
C110.31490 (14)0.01820 (16)0.21840 (8)0.0200 (3)*
H100.2411 (15)0.017 (2)0.2296 (8)0.020 (4)*
C120.39270 (14)0.08580 (17)0.25770 (10)0.0200 (3)*
H110.3709 (14)0.130 (2)0.2951 (9)0.020 (5)*
C130.50330 (14)0.08720 (16)0.24110 (10)0.0200 (3)*
H120.5553 (15)0.1324 (19)0.2673 (9)0.020 (4)*
C140.53590 (13)0.02070 (17)0.18500 (9)0.0200 (3)*
C150.45810 (12)0.04700 (17)0.14580 (9)0.0200 (3)*
C160.34760 (13)0.04830 (16)0.16250 (9)0.0200 (3)*
C170.67020 (14)0.15330 (16)0.12810 (10)0.0200 (3)*
H130.6266 (15)0.141 (2)0.0909 (9)0.020 (5)*
H140.6502 (14)0.255 (2)0.1473 (9)0.020 (5)*
C180.79020 (14)0.15600 (17)0.11150 (10)0.0200 (4)*
H150.8343 (15)0.1452 (19)0.1486 (9)0.020 (4)*
H160.8083 (14)0.259 (2)0.0923 (9)0.020 (4)*
C190.92040 (13)0.03910 (18)0.04390 (9)0.0200 (3)*
H170.9703 (14)0.090 (2)0.0731 (9)0.020 (4)*
H180.9473 (13)0.070 (2)0.0358 (9)0.020 (4)*
C200.92250 (14)0.13510 (17)0.01590 (9)0.0200 (3)*
H190.9976 (16)0.1479 (19)0.0301 (9)0.020 (4)*
H200.8913 (14)0.242 (2)0.0093 (9)0.020 (4)*
C210.85170 (14)0.13710 (17)0.11730 (9)0.0200 (3)*
H210.8200 (14)0.244 (2)0.1105 (9)0.020 (4)*
H220.9240 (15)0.1507 (19)0.1357 (8)0.020 (5)*
C220.78060 (13)0.04180 (17)0.15860 (10)0.0200 (3)*
H230.8062 (14)0.070 (2)0.1602 (9)0.020 (4)*
H240.7828 (14)0.086 (2)0.1999 (9)0.020 (4)*
Geometric parameters (Å, º) top
O1—C51.350 (2)C5—C61.390 (2)
O2—C151.349 (2)C7—N11.300 (2)
O3—C141.388 (2)N1—C81.453 (2)
O3—C171.4102 (19)C8—C91.465 (2)
O4—C181.403 (2)C9—N21.524 (2)
O4—C191.415 (2)N2—C101.251 (2)
O5—C201.410 (2)C10—C161.465 (2)
O5—C211.434 (2)C11—C161.389 (3)
O6—C61.3640 (18)C11—C121.390 (2)
O6—C221.430 (2)C12—C131.391 (3)
C1—C21.389 (2)C13—C141.392 (3)
C1—C61.390 (2)C14—C151.389 (2)
C2—C31.389 (3)C15—C161.390 (2)
C3—C41.390 (2)C17—C181.502 (3)
C4—C51.389 (2)C19—C201.520 (3)
C4—C71.446 (2)C21—C221.472 (2)
C14—O3—C17112.00 (12)C10—N2—C9119.41 (14)
C18—O4—C19113.90 (12)N2—C10—C16121.52 (16)
C20—O5—C21112.27 (12)C16—C11—C12119.97 (17)
C6—O6—C22119.17 (13)C11—C12—C13120.1 (2)
C2—C1—C6120.02 (17)C12—C13—C14119.85 (18)
C3—C2—C1120.02 (18)O3—C14—C15120.85 (16)
C2—C3—C4120.01 (15)O3—C14—C13119.14 (15)
C5—C4—C3119.98 (16)C15—C14—C13120.00 (16)
C5—C4—C7120.99 (16)O2—C15—C14118.51 (15)
C3—C4—C7119.02 (14)O2—C15—C16121.44 (15)
O1—C5—C4121.03 (15)C14—C15—C16120.05 (17)
O1—C5—C6118.93 (14)C11—C16—C15120.03 (15)
C4—C5—C6120.04 (17)C11—C16—C10119.04 (15)
O6—C6—C1124.51 (16)C15—C16—C10120.73 (17)
O6—C6—C5115.55 (16)O3—C17—C18111.12 (14)
C1—C6—C5119.94 (15)O4—C18—C17110.11 (14)
N1—C7—C4121.70 (14)O4—C19—C20113.49 (13)
C7—N1—C8121.06 (13)O5—C20—C19108.30 (13)
N1—C8—C9113.84 (13)O5—C21—C22107.49 (13)
C8—C9—N2110.66 (13)O6—C22—C21108.56 (14)
(qelpus) (S!C$)-trans-bis(mu!2$-Chloro)-bis(N,N-dimethyl-1-(2-naphthyl)ethylamine-C,N)- -dipalladium(ii) monohydrate top
Crystal data top
C28H32Cl2N2Pd2·H2Oγ = 90°
Mr = 698.27V = 3040.2 (7) Å3
P212121Z = 4
a = 6.6179 (7) ÅF(000) = 1400
b = 12.924 (2) ÅDx = 1.526 Mg m3
c = 35.545 (5) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 1.38 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.028
Graphite monochromatorθmax = 26.9°, θmin = 1.2°
8976 measured reflectionsh = 66
2252 independent reflectionsk = 1010
2240 reflections with I > 2σ(I)l = 1616
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.007H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.042 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.36(Δ/σ)max = 3.897
2252 reflectionsΔρmax = 0.16 e Å3
269 parametersΔρmin = 0.22 e Å3
0 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.015 (19)
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
Pd10.29800 (3)0.327500 (18)0.203400 (10)0.02000 (8)*
Pd20.62320 (3)0.435800 (18)0.137300 (11)0.02000 (8)*
Cl10.53520 (9)0.46130 (6)0.20440 (4)0.02000 (18)*
Cl20.44690 (9)0.27970 (6)0.14200 (4)0.02000 (17)*
O10.6635 (3)0.25870 (16)0.46260 (9)0.0200 (5)*
N10.0719 (3)0.2168 (2)0.20540 (12)0.0200 (6)*
N20.7921 (4)0.56950 (19)0.13160 (10)0.0200 (6)*
C10.1918 (4)0.3544 (2)0.25390 (13)0.0200 (7)*
C20.3020 (4)0.3999 (2)0.28330 (13)0.0200 (6)*
C30.2210 (4)0.4127 (2)0.31880 (13)0.0200 (7)*
C40.3265 (4)0.4588 (2)0.35060 (14)0.0200 (7)*
C50.2514 (4)0.4669 (2)0.38340 (15)0.0200 (8)*
C60.0561 (4)0.4322 (2)0.38980 (17)0.0200 (7)*
C70.0630 (4)0.3890 (2)0.36320 (15)0.0200 (7)*
C80.0157 (4)0.3745 (2)0.32560 (16)0.0200 (7)*
C90.0837 (4)0.3272 (2)0.29590 (14)0.0200 (7)*
C100.0042 (4)0.3142 (2)0.26140 (14)0.0200 (7)*
C110.0981 (4)0.2609 (2)0.22890 (14)0.0200 (7)*
C120.2628 (4)0.1856 (3)0.23910 (17)0.0200 (7)*
C130.1561 (4)0.1202 (3)0.22180 (16)0.0200 (7)*
C140.0049 (4)0.1912 (3)0.16700 (15)0.0200 (8)*
C150.6715 (4)0.4245 (2)0.08220 (14)0.0200 (7)*
C160.5654 (4)0.3708 (2)0.05660 (16)0.0200 (7)*
C170.6130 (4)0.3772 (2)0.01770 (15)0.0200 (7)*
C180.5025 (4)0.3228 (2)0.00960 (16)0.0200 (7)*
C190.5571 (4)0.3209 (2)0.04580 (17)0.0200 (7)*
C200.7217 (4)0.3776 (2)0.05780 (16)0.0200 (7)*
C210.8260 (4)0.4355 (2)0.03310 (15)0.0200 (7)*
C220.7743 (4)0.4390 (2)0.00630 (15)0.0200 (7)*
C230.8734 (4)0.4975 (2)0.03260 (16)0.0200 (7)*
C240.8293 (4)0.4925 (2)0.07010 (16)0.0200 (7)*
C250.9425 (4)0.5525 (3)0.10030 (15)0.0200 (7)*
C261.1223 (5)0.4905 (3)0.11230 (16)0.0200 (7)*
C270.6534 (4)0.6546 (3)0.11920 (16)0.0200 (8)*
C280.8932 (5)0.6028 (2)0.16710 (14)0.0200 (7)*
H10.433 (4)0.422 (2)0.2787 (11)0.020 (9)*
H20.457 (5)0.484 (2)0.3467 (11)0.020 (9)*
H30.327 (5)0.496 (2)0.4029 (12)0.020 (9)*
H40.004 (5)0.440 (2)0.4139 (12)0.020 (9)*
H50.194 (5)0.369 (2)0.3690 (11)0.020 (8)*
H60.215 (4)0.303 (2)0.2995 (11)0.020 (8)*
H70.161 (4)0.315 (2)0.2138 (11)0.020 (9)*
H80.318 (5)0.156 (2)0.2166 (12)0.020 (9)*
H90.368 (5)0.221 (2)0.2525 (11)0.020 (8)*
H100.208 (4)0.132 (2)0.2547 (11)0.020 (8)*
H110.262 (5)0.095 (2)0.2061 (12)0.020 (9)*
H120.051 (4)0.069 (2)0.2236 (11)0.020 (9)*
H130.209 (5)0.134 (2)0.2465 (13)0.020 (9)*
H140.060 (4)0.252 (3)0.1556 (12)0.020 (9)*
H150.108 (5)0.139 (2)0.1688 (11)0.020 (8)*
H160.104 (4)0.166 (2)0.1518 (12)0.020 (8)*
H170.459 (4)0.329 (2)0.0644 (11)0.020 (9)*
H180.387 (4)0.287 (2)0.0022 (12)0.020 (8)*
H190.484 (4)0.281 (2)0.0629 (11)0.020 (9)*
H200.760 (5)0.376 (2)0.0829 (12)0.020 (10)*
H210.935 (4)0.475 (2)0.0417 (12)0.020 (9)*
H220.975 (4)0.542 (2)0.0247 (11)0.020 (9)*
H230.987 (4)0.619 (3)0.0902 (12)0.020 (9)*
H241.195 (5)0.528 (2)0.1313 (11)0.020 (8)*
H251.209 (5)0.479 (2)0.0911 (12)0.020 (9)*
H261.078 (4)0.425 (2)0.1222 (11)0.020 (8)*
H270.556 (5)0.668 (2)0.1385 (13)0.020 (8)*
H280.585 (5)0.634 (2)0.0965 (14)0.020 (9)*
H290.730 (4)0.716 (2)0.1146 (11)0.020 (9)*
H300.793 (5)0.616 (2)0.1860 (12)0.020 (9)*
H310.968 (4)0.665 (2)0.1626 (11)0.020 (9)*
H320.983 (4)0.549 (2)0.1755 (12)0.020 (9)*
Geometric parameters (Å, º) top
Pd1—C11.959 (4)C12—H100.96 (3)
Pd1—N12.071 (2)C13—H110.96 (3)
Pd1—Cl12.3357 (7)C13—H120.96 (3)
Pd1—Cl22.4730 (12)C13—H130.96 (4)
Pd2—C151.990 (5)C14—H140.96 (3)
Pd2—N22.068 (2)C14—H150.96 (3)
Pd2—Cl22.3365 (8)C14—H160.96 (3)
Pd2—Cl12.4772 (13)C15—C161.343 (6)
N1—C131.486 (5)C15—C241.431 (4)
N1—C141.494 (6)C16—C171.421 (6)
N1—C111.513 (4)C16—H170.93 (3)
N2—C281.492 (5)C17—C221.393 (4)
N2—C271.499 (4)C17—C181.404 (6)
N2—C251.509 (5)C18—C191.337 (6)
C1—C101.372 (4)C18—H180.93 (3)
C1—C21.403 (6)C19—C201.380 (5)
C2—C31.381 (6)C19—H190.93 (3)
C2—H10.93 (3)C20—C211.344 (6)
C3—C41.456 (6)C20—H200.93 (4)
C3—C81.466 (4)C21—C221.442 (5)
C4—C51.272 (6)C21—H210.93 (3)
C4—H20.93 (3)C22—C231.370 (6)
C5—C61.387 (4)C23—C241.366 (6)
C5—H30.93 (4)C23—H220.93 (3)
C6—C71.352 (6)C24—C251.521 (6)
C6—H40.93 (4)C25—C261.497 (4)
C7—C81.447 (7)C25—H230.98 (3)
C7—H50.93 (3)C26—H240.96 (4)
C8—C91.386 (6)C26—H250.96 (4)
C9—C101.368 (6)C26—H260.96 (3)
C9—H60.93 (3)C27—H270.96 (4)
C10—C111.506 (6)C27—H280.96 (4)
C11—C121.506 (4)C27—H290.96 (3)
C11—H70.98 (3)C28—H300.96 (4)
C12—H80.96 (4)C28—H310.96 (3)
C12—H90.96 (3)C28—H320.96 (3)
C1—Pd1—N180.33 (14)H9—C12—H10110 (3)
C1—Pd1—Cl195.50 (9)N1—C13—H11110 (2)
N1—Pd1—Cl1175.05 (9)N1—C13—H12109.4 (19)
C1—Pd1—Cl2174.89 (10)H11—C13—H12110 (3)
N1—Pd1—Cl298.37 (11)N1—C13—H13109.4 (19)
Cl1—Pd1—Cl286.02 (3)H11—C13—H13109 (3)
C15—Pd2—N283.00 (13)H12—C13—H13109 (3)
C15—Pd2—Cl295.00 (9)N1—C14—H14109 (2)
N2—Pd2—Cl2176.77 (8)N1—C14—H15110 (2)
C15—Pd2—Cl1174.40 (9)H14—C14—H15109 (3)
N2—Pd2—Cl196.33 (10)N1—C14—H16109 (2)
Cl2—Pd2—Cl185.91 (3)H14—C14—H16109 (3)
Pd1—Cl1—Pd292.57 (4)H15—C14—H16109 (3)
Pd2—Cl2—Pd192.66 (4)C16—C15—C24119.7 (5)
C13—N1—C14107.5 (3)C16—C15—Pd2128.4 (3)
C13—N1—C11112.3 (3)C24—C15—Pd2111.6 (3)
C14—N1—C11109.6 (2)C15—C16—C17120.9 (4)
C13—N1—Pd1108.83 (17)C15—C16—H17120 (3)
C14—N1—Pd1111.6 (2)C17—C16—H17119 (3)
C11—N1—Pd1107.21 (18)C22—C17—C18119.0 (5)
C28—N2—C27108.2 (3)C22—C17—C16119.1 (4)
C28—N2—C25111.7 (2)C18—C17—C16121.9 (3)
C27—N2—C25107.1 (3)C19—C18—C17122.3 (4)
C28—N2—Pd2113.6 (2)C19—C18—H18119 (3)
C27—N2—Pd2108.12 (18)C17—C18—H18119 (3)
C25—N2—Pd2107.89 (19)C18—C19—C20120.1 (4)
C10—C1—C2119.0 (4)C18—C19—H19120 (2)
C10—C1—Pd1115.8 (3)C20—C19—H19120 (2)
C2—C1—Pd1124.8 (2)C21—C20—C19119.9 (5)
C3—C2—C1121.9 (3)C21—C20—H20119.9 (18)
C3—C2—H1119 (2)C19—C20—H20120.1 (19)
C1—C2—H1119 (2)C20—C21—C22122.0 (4)
C2—C3—C4124.9 (3)C20—C21—H21119 (3)
C2—C3—C8118.0 (4)C22—C21—H21119 (2)
C4—C3—C8117.0 (4)C23—C22—C17119.0 (5)
C5—C4—C3123.9 (3)C23—C22—C21124.5 (3)
C5—C4—H2118 (3)C17—C22—C21116.5 (4)
C3—C4—H2118 (3)C24—C23—C22122.5 (3)
C4—C5—C6119.2 (5)C24—C23—H22119 (2)
C4—C5—H3120 (2)C22—C23—H22119 (2)
C6—C5—H3120 (2)C23—C24—C15118.6 (4)
C7—C6—C5124.2 (5)C23—C24—C25124.0 (3)
C7—C6—H4118.0 (19)C15—C24—C25117.4 (5)
C5—C6—H4118 (2)C26—C25—N2113.1 (4)
C6—C7—C8119.3 (3)C26—C25—C24108.6 (3)
C6—C7—H5120 (3)N2—C25—C24105.6 (2)
C8—C7—H5120 (2)C26—C25—H23109.8 (17)
C9—C8—C7126.2 (3)N2—C25—H23110 (2)
C9—C8—C3117.6 (5)C24—C25—H23110 (2)
C7—C8—C3116.3 (4)C25—C26—H24109.4 (18)
C10—C9—C8122.4 (3)C25—C26—H25110 (2)
C10—C9—H6119 (2)H24—C26—H25109 (3)
C8—C9—H6119 (2)C25—C26—H26109.6 (17)
C9—C10—C1120.8 (4)H24—C26—H26110 (3)
C9—C10—C11123.6 (3)H25—C26—H26109 (2)
C1—C10—C11115.5 (4)N2—C27—H27109 (2)
C12—C11—C10115.9 (4)N2—C27—H28109.6 (18)
C12—C11—N1115.3 (3)H27—C27—H28109 (3)
C10—C11—N1105.2 (2)N2—C27—H29109.4 (17)
C12—C11—H7106.6 (17)H27—C27—H29109 (3)
C10—C11—H7107 (2)H28—C27—H29109 (3)
N1—C11—H7107 (2)N2—C28—H30109 (2)
C11—C12—H8110 (2)N2—C28—H31109 (2)
C11—C12—H9109.5 (18)H30—C28—H31109 (3)
H8—C12—H9109 (3)N2—C28—H32110 (2)
C11—C12—H10109.5 (18)H30—C28—H32110 (3)
H8—C12—H10109 (3)H31—C28—H32109 (2)
(aplsol) top
Crystal data top
C15BrO2γ = 90°
Mr = 292.06V = 1383.7 (10) Å3
P43Z = 4
a = 13.750 (5) ÅF(000) = 564
b = 13.750 (5) ÅDx = 1.402 Mg m3
c = 7.319 (4) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 2.96 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.053
Graphite monochromatorθmax = 47.1°, θmin = 1.5°
20164 measured reflectionsh = 1515
5044 independent reflectionsk = 1515
4914 reflections with I > 2σ(I)l = 1010
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)] = 0.009 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.050(Δ/σ)max = 0.261
S = 0.31Δρmax = 0.41 e Å3
5044 reflectionsΔρmin = 0.41 e Å3
73 parametersAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
1 restraintAbsolute structure parameter: 0.015 (2)
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
Br10.889000 (6)0.835000 (6)0.499500 (15)0.02000 (2)*
O40.78510 (5)0.53550 (5)0.05260 (9)0.02000 (10)*
O110.59220 (5)0.45900 (5)0.01880 (9)0.02000 (10)*
C10.87600 (6)0.41500 (7)0.32000 (11)0.02000 (12)*
C20.93450 (7)0.39800 (7)0.14500 (11)0.02000 (12)*
C30.85700 (6)0.37750 (6)0.00900 (12)0.02000 (12)*
C130.77000 (7)0.44650 (7)0.04250 (10)0.02000 (13)*
C40.81100 (7)0.60800 (7)0.05750 (11)0.02000 (12)*
C50.83300 (6)0.70200 (6)0.00850 (12)0.02000 (12)*
C60.85750 (7)0.77150 (7)0.13450 (11)0.02000 (12)*
C70.85500 (7)0.74450 (6)0.31800 (11)0.02000 (12)*
C80.83200 (7)0.64800 (7)0.37700 (11)0.02000 (12)*
C180.80750 (6)0.58100 (6)0.25200 (12)0.02000 (11)*
C280.78500 (6)0.47400 (6)0.26400 (11)0.02000 (12)*
C90.89200 (7)0.38000 (7)0.19600 (11)0.02000 (12)*
C100.67600 (6)0.40250 (7)0.00650 (12)0.02000 (12)*
C120.87550 (7)0.87700 (7)0.08550 (11)0.02000 (12)*
C310.70000 (7)0.45700 (7)0.38600 (11)0.02000 (13)*
Geometric parameters (Å, º) top
Br1—C71.8793 (11)C13—C281.6774 (14)
O4—C41.3304 (12)C4—C51.3750 (13)
O4—C131.4231 (12)C4—C181.4719 (14)
O11—C101.4020 (11)C5—C61.3701 (13)
C1—C21.5304 (13)C6—C71.3938 (14)
C1—C281.5465 (13)C6—C121.5147 (13)
C2—C31.4852 (13)C7—C81.4308 (13)
C3—C131.5464 (14)C8—C181.3413 (13)
C3—C91.5761 (14)C18—C281.5060 (13)
C13—C101.4715 (14)C28—C311.4893 (13)
C4—O4—C13112.78 (8)C5—C6—C12123.29 (8)
C2—C1—C28106.47 (7)C7—C6—C12119.16 (8)
C3—C2—C1102.29 (8)C6—C7—C8122.91 (8)
C2—C3—C13109.41 (7)C6—C7—Br1119.91 (7)
C2—C3—C9114.51 (8)C8—C7—Br1117.11 (7)
C13—C3—C9111.95 (7)C18—C8—C7119.12 (8)
O4—C13—C10111.25 (7)C8—C18—C4118.57 (8)
O4—C13—C3109.71 (7)C8—C18—C28133.06 (8)
C10—C13—C3112.87 (7)C4—C18—C28108.03 (7)
O4—C13—C28105.12 (7)C31—C28—C18110.46 (7)
C10—C13—C28115.86 (7)C31—C28—C1113.19 (7)
C3—C13—C28101.33 (7)C18—C28—C1111.21 (7)
O4—C4—C5127.25 (8)C31—C28—C13116.59 (8)
O4—C4—C18112.83 (8)C18—C28—C13100.90 (7)
C5—C4—C18119.77 (8)C1—C28—C13103.73 (7)
C6—C5—C4122.29 (8)O11—C10—C13117.51 (8)
C5—C6—C7117.18 (9)
(doqzak) (2-Hydroxyethanolato)-oxo-(N-(1-oxy-2-methylprop-2-yl)-2-oxy-1-naphthaldimato)- -vanadium(v) top
Crystal data top
C17H20NO5Vγ = 90°
Mr = 369.28V = 1720 (2) Å3
P43Z = 4
a = 9.717 (8) ÅF(000) = 768
b = 9.717 (8) ÅDx = 1.426 Mg m3
c = 18.217 (9) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 0.60 mm1
β = 90°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.014
Graphite monochromatorθmax = 45.5°, θmin = 2.1°
23096 measured reflectionsh = 1212
5780 independent reflectionsk = 1212
5762 reflections with I > 2σ(I)l = 1818
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.008H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.031 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.18(Δ/σ)max = 1.238
5780 reflectionsΔρmax = 0.07 e Å3
177 parametersΔρmin = 0.17 e Å3
1 restraintAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.009 (2)
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
V10.069400 (6)0.780500 (6)0.904700 (4)0.02000 (2)*
O10.01470 (3)0.66230 (3)0.944000 (18)0.02000 (4)*
O20.24500 (3)0.72300 (3)0.919600 (17)0.02000 (4)*
O30.07580 (3)0.85510 (3)0.848100 (18)0.02000 (4)*
O40.18240 (3)0.97420 (3)0.855800 (19)0.02000 (4)*
H360.1440 (7)0.9987 (7)0.8064 (4)0.0200 (14)*
O50.06890 (3)0.90760 (3)0.979400 (18)0.02000 (5)*
N10.11340 (3)0.67980 (3)0.80530 (2)0.02000 (5)*
C10.33160 (4)0.69930 (4)0.85840 (2)0.02000 (5)*
H10.4213 (7)0.6660 (7)0.8702 (4)0.0200 (14)*
H20.3473 (7)0.7872 (7)0.8361 (4)0.0200 (14)*
C20.25340 (4)0.61560 (3)0.80370 (2)0.02000 (5)*
C30.03330 (3)0.65850 (3)0.75130 (2)0.02000 (5)*
H370.0625 (7)0.5958 (7)0.7088 (4)0.0200 (15)*
C40.10290 (4)0.71460 (3)0.74200 (2)0.02000 (5)*
C50.14500 (3)0.81670 (3)0.79040 (2)0.02000 (5)*
C60.27200 (4)0.88860 (3)0.77550 (2)0.02000 (5)*
H30.3037 (7)0.9552 (7)0.8081 (4)0.0200 (14)*
C70.34410 (3)0.85950 (3)0.71490 (2)0.02000 (5)*
H40.4225 (7)0.9111 (7)0.7050 (4)0.0200 (15)*
C80.38570 (3)0.72790 (3)0.60060 (2)0.02000 (5)*
H50.4632 (7)0.7805 (7)0.5901 (4)0.0200 (14)*
C90.34860 (4)0.63010 (3)0.55650 (2)0.02000 (5)*
H60.4015 (7)0.6141 (7)0.5148 (4)0.0200 (14)*
C100.23600 (3)0.54940 (4)0.56820 (3)0.02000 (5)*
H70.2131 (7)0.4802 (7)0.5351 (4)0.0200 (14)*
C110.15530 (3)0.57210 (3)0.63060 (2)0.02000 (5)*
H80.0800 (6)0.5156 (7)0.6399 (4)0.0200 (15)*
C120.18600 (3)0.67770 (4)0.67910 (2)0.02000 (6)*
C130.30710 (3)0.75510 (4)0.66590 (2)0.02000 (5)*
C140.23600 (3)0.46700 (4)0.82990 (2)0.02000 (5)*
H90.1855 (7)0.4156 (7)0.7939 (4)0.0200 (14)*
H100.1866 (7)0.4662 (7)0.8756 (4)0.0200 (14)*
H110.3249 (7)0.4259 (7)0.8369 (4)0.0200 (14)*
C150.32350 (3)0.62830 (3)0.72900 (2)0.02000 (5)*
H120.2740 (7)0.5748 (7)0.6935 (4)0.0200 (14)*
H130.4163 (7)0.5950 (7)0.7325 (4)0.0200 (14)*
H140.3244 (7)0.7230 (7)0.7141 (4)0.0200 (14)*
C160.15860 (3)1.08410 (3)0.90740 (2)0.02000 (5)*
H150.2260 (7)1.1574 (7)0.9042 (4)0.0200 (14)*
H160.0696 (7)1.1241 (7)0.8981 (4)0.0200 (14)*
C170.15710 (3)1.02080 (4)0.97930 (2)0.02000 (6)*
H170.2494 (7)0.9914 (7)0.9923 (4)0.0200 (14)*
H180.1267 (7)1.0872 (7)1.0156 (4)0.0200 (14)*
Geometric parameters (Å, º) top
V1—O11.5810 (11)C6—H30.931 (7)
V1—O21.8159 (15)C7—C131.3983 (9)
V1—O51.8377 (9)C7—H40.930 (7)
V1—O31.8919 (12)C8—C91.2956 (9)
V1—N12.1022 (10)C8—C131.4381 (8)
V1—O42.3541 (17)C8—H50.930 (7)
O2—C11.4157 (8)C9—C101.3629 (12)
O3—C51.3024 (7)C9—H60.930 (7)
O4—C161.4413 (9)C10—C111.3985 (8)
O4—H361.003 (8)C10—H70.930 (7)
O5—C171.3944 (12)C11—C121.3866 (9)
N1—C31.2714 (8)C11—H80.930 (6)
N1—C21.4969 (13)C12—C131.4171 (12)
C1—C21.4939 (9)C14—H90.959 (7)
C1—H10.954 (7)C14—H100.961 (7)
C1—H20.958 (7)C14—H110.960 (7)
C2—C151.5268 (9)C15—H120.959 (7)
C2—C141.5302 (12)C15—H130.960 (7)
C3—C41.4413 (13)C15—H140.959 (7)
C3—H371.025 (7)C16—C171.4471 (9)
C4—C51.3889 (9)C16—H150.969 (6)
C4—C121.4469 (9)C16—H160.963 (7)
C5—C61.4438 (12)C17—H170.971 (7)
C6—C71.3377 (8)C17—H180.970 (7)
O1—V1—O2101.215 (17)C5—C6—H3120.0 (4)
O1—V1—O598.72 (5)C6—C7—C13123.06 (4)
O2—V1—O595.66 (2)C6—C7—H4118.4 (5)
O1—V1—O398.03 (3)C13—C7—H4118.6 (5)
O2—V1—O3154.18 (2)C9—C8—C13120.00 (5)
O5—V1—O398.29 (4)C9—C8—H5120.1 (5)
O1—V1—N199.03 (4)C13—C8—H5119.9 (5)
O2—V1—N178.14 (3)C8—C9—C10123.26 (5)
O5—V1—N1162.028 (15)C8—C9—H6118.4 (4)
O3—V1—N181.99 (5)C10—C9—H6118.4 (4)
O1—V1—O4173.358 (14)C9—C10—C11119.11 (4)
O2—V1—O482.200 (14)C9—C10—H7120.4 (4)
O5—V1—O475.17 (4)C11—C10—H7120.5 (4)
O3—V1—O480.52 (2)C12—C11—C10120.93 (4)
N1—V1—O487.21 (4)C12—C11—H8119.3 (4)
C1—O2—V1119.40 (4)C10—C11—H8119.7 (4)
C5—O3—V1135.65 (3)C11—C12—C13117.60 (4)
C16—O4—V1105.71 (4)C11—C12—C4124.61 (4)
C16—O4—H36110.5 (4)C13—C12—C4117.79 (3)
V1—O4—H36110.8 (4)C7—C13—C12119.36 (4)
C17—O5—V1121.84 (3)C7—C13—C8121.66 (4)
C3—N1—C2118.26 (4)C12—C13—C8118.93 (3)
C3—N1—V1128.15 (4)C2—C14—H9109.5 (4)
C2—N1—V1113.30 (3)C2—C14—H10109.5 (4)
O2—C1—C2108.15 (5)H9—C14—H10109.4 (6)
O2—C1—H1114.9 (5)C2—C14—H11109.5 (4)
C2—C1—H1115.5 (4)H9—C14—H11109.5 (6)
O2—C1—H2106.5 (4)H10—C14—H11109.3 (6)
C2—C1—H2106.5 (4)C2—C15—H12109.5 (4)
H1—C1—H2104.6 (6)C2—C15—H13109.4 (5)
C1—C2—N1102.85 (3)H12—C15—H13109.5 (6)
C1—C2—C15108.88 (5)C2—C15—H14109.5 (4)
N1—C2—C15112.90 (4)H12—C15—H14109.5 (6)
C1—C2—C14111.22 (5)H13—C15—H14109.5 (6)
N1—C2—C14106.67 (3)O4—C16—C17106.08 (6)
C15—C2—C14113.80 (3)O4—C16—H15113.4 (4)
N1—C3—C4126.27 (4)C17—C16—H15111.9 (5)
N1—C3—H37120.8 (4)O4—C16—H16109.2 (4)
C4—C3—H37113.0 (4)C17—C16—H16108.8 (5)
C5—C4—C3117.77 (4)H15—C16—H16107.4 (5)
C5—C4—C12121.02 (4)O5—C17—C16110.04 (4)
C3—C4—C12120.78 (4)O5—C17—H17109.6 (4)
O3—C5—C4124.40 (4)C16—C17—H17109.7 (5)
O3—C5—C6117.02 (3)O5—C17—H18109.7 (4)
C4—C5—C6118.56 (5)C16—C17—H18109.7 (4)
C7—C6—C5120.03 (4)H17—C17—H18108.1 (6)
C7—C6—H3120.0 (4)
(bamubr) bis(Tetra-n-butylammonium) tetrabromo-uranyl top
Crystal data top
C16Br2NOU0.50γ = 90°
Mr = 501.01V = 4298 (8) Å3
C2/cZ = 8
a = 17.731 (15) ÅF(000) = 1816
b = 14.681 (15) ÅDx = 1.549 Mg m3
c = 17.08 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 7.52 mm1
β = 104.80 (8)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.020
Graphite monochromatorθmax = 60.3°, θmin = 1.8°
22662 measured reflectionsh = 2424
7087 independent reflectionsk = 2424
6880 reflections with I > 2σ(I)l = 3030
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.010Secondary atom site location: difference Fourier map
wR(F2) = 0.086 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.57(Δ/σ)max = 3.860
7087 reflectionsΔρmax = 1.42 e Å3
83 parametersΔρmin = 0.75 e Å3
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
U10.00000.131200 (4)0.75000.02000 (3)*
Br10.162100 (11)0.127300 (9)0.820300 (9)0.02000 (4)*
Br30.00000.060300 (14)0.75000.02000 (5)*
Br40.00000.322300 (14)0.75000.02000 (5)*
O10.01450 (9)0.13100 (5)0.65450 (8)0.0200 (2)*
N10.21180 (8)0.08170 (8)0.13450 (7)0.02000 (18)*
C10.20170 (9)0.16820 (8)0.08500 (7)0.02000 (19)*
C20.12650 (9)0.21600 (8)0.07950 (7)0.02000 (19)*
C30.12330 (9)0.29930 (9)0.01800 (8)0.0200 (2)*
C40.05070 (10)0.35670 (9)0.01250 (8)0.0200 (2)*
C50.20750 (10)0.09500 (8)0.21900 (8)0.02000 (19)*
C60.26380 (9)0.16780 (8)0.26700 (7)0.02000 (19)*
C70.26900 (9)0.15900 (9)0.35800 (8)0.0200 (2)*
C80.31980 (9)0.08130 (9)0.39450 (7)0.02000 (19)*
C90.29300 (8)0.04500 (9)0.12750 (7)0.02000 (18)*
C100.31080 (8)0.04530 (9)0.17250 (7)0.02000 (19)*
C110.39100 (9)0.07500 (9)0.15550 (7)0.02000 (18)*
C120.41000 (9)0.17550 (8)0.19150 (7)0.0200 (2)*
C130.14750 (9)0.01150 (9)0.09800 (7)0.02000 (19)*
C140.14120 (9)0.00780 (8)0.01000 (7)0.0200 (2)*
C150.08050 (10)0.09300 (9)0.01600 (8)0.02000 (19)*
C160.11620 (9)0.17480 (8)0.00800 (8)0.02000 (19)*
Geometric parameters (Å, º) top
U1—O11.715 (2)C2—C31.604 (2)
U1—O1i1.715 (2)C3—C41.521 (2)
U1—Br42.806 (3)C5—C61.547 (2)
U1—Br32.811 (3)C6—C71.538 (3)
U1—Br12.818 (3)C7—C81.488 (2)
U1—Br1i2.818 (3)C9—C101.524 (2)
N1—C51.477 (2)C10—C111.583 (2)
N1—C11.511 (2)C11—C121.601 (2)
N1—C131.545 (2)C13—C141.505 (2)
N1—C91.570 (2)C14—C151.636 (2)
C1—C21.488 (2)C15—C161.371 (2)
O1—U1—O1i179.80 (5)C1—N1—C13111.42 (13)
O1—U1—Br490.10 (3)C5—N1—C9113.38 (13)
O1i—U1—Br490.10 (3)C1—N1—C9103.05 (11)
O1—U1—Br389.90 (3)C13—N1—C9109.69 (12)
O1i—U1—Br389.90 (3)C2—C1—N1114.07 (12)
Br4—U1—Br3180.0C1—C2—C3106.39 (12)
O1—U1—Br191.19 (10)C4—C3—C2110.53 (13)
O1i—U1—Br188.81 (10)N1—C5—C6114.94 (12)
Br4—U1—Br191.164 (3)C7—C6—C5109.96 (12)
Br3—U1—Br188.836 (3)C8—C7—C6111.17 (12)
O1—U1—Br1i88.81 (10)C10—C9—N1109.62 (11)
O1i—U1—Br1i91.19 (10)C9—C10—C11103.12 (11)
Br4—U1—Br1i91.164 (3)C10—C11—C12107.11 (11)
Br3—U1—Br1i88.836 (3)C14—C13—N1112.78 (12)
Br1—U1—Br1i177.672 (6)C13—C14—C15106.91 (12)
C5—N1—C1114.03 (11)C16—C15—C14111.55 (15)
C5—N1—C13105.39 (12)
Symmetry code: (i) x, y, z+3/2.
(farner) Tetrachloro-bis(N,N,N,N'-tetramethylurea)-uranium(iv) top
Crystal data top
C10Cl4N4O2Uγ = 90°
Mr = 587.97V = 2019.2 (4) Å3
C2/cZ = 4
a = 16.429 (2) ÅF(000) = 1056
b = 8.514 (1) ÅDx = 1.934 Mg m3
c = 16.418 (2) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 8.57 mm1
β = 118.45 (2)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.004
Graphite monochromatorθmax = 52.7°, θmin = 2.8°
9718 measured reflectionsh = 2626
3303 independent reflectionsk = 88
3049 reflections with I > 2σ(I)l = 2424
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.004Secondary atom site location: difference Fourier map
wR(F2) = 0.046 w = 1/[σ2(Fo2) + (0.P)2 + 0.0533P]
where P = (Fo2 + 2Fc2)/3
S = 0.49(Δ/σ)max = 2.086
3303 reflectionsΔρmax = 0.41 e Å3
42 parametersΔρmin = 0.25 e Å3
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
U10.2500000.2500000.000000.02000 (3)*
Cl10.393300 (13)0.061300 (17)0.071700 (14)0.02000 (5)*
Cl20.359100 (13)0.496100 (18)0.056600 (14)0.02000 (5)*
N10.34620 (12)0.24600 (6)0.20230 (13)0.0200 (3)*
N20.18350 (6)0.23820 (10)0.28790 (7)0.0200 (2)*
O10.25710 (11)0.24990 (4)0.13170 (12)0.0200 (3)*
C10.26210 (12)0.24460 (8)0.20710 (13)0.0200 (3)*
C20.42870 (4)0.28520 (16)0.11240 (5)0.02000 (9)*
C30.36330 (5)0.16840 (10)0.27530 (5)0.02000 (12)*
C40.09560 (5)0.19710 (9)0.28570 (5)0.02000 (14)*
C50.17310 (6)0.31540 (7)0.37460 (7)0.02000 (14)*
Geometric parameters (Å, º) top
U1—O1i2.2202 (17)N1—C21.490 (2)
U1—O12.2202 (17)N1—C31.5075 (18)
U1—Cl1i2.6209 (4)N2—C11.341 (2)
U1—Cl12.6209 (4)N2—C51.5019 (13)
U1—Cl2i2.6229 (3)N2—C41.5030 (12)
U1—Cl22.6229 (3)O1—C11.280 (2)
N1—C11.346 (2)
O1i—U1—O1180.000 (19)Cl1—U1—Cl290.833 (15)
O1i—U1—Cl1i89.11 (4)Cl2i—U1—Cl2180.000 (10)
O1—U1—Cl1i90.89 (4)C1—N1—C2118.94 (14)
O1i—U1—Cl190.89 (4)C1—N1—C3121.63 (13)
O1—U1—Cl189.11 (4)C2—N1—C3117.36 (11)
Cl1i—U1—Cl1180.0C1—N2—C5122.75 (10)
O1i—U1—Cl2i90.07 (3)C1—N2—C4117.98 (11)
O1—U1—Cl2i89.93 (3)C5—N2—C4116.61 (8)
Cl1i—U1—Cl2i90.833 (15)C1—O1—U1177.92 (6)
Cl1—U1—Cl2i89.167 (15)O1—C1—N2118.88 (16)
O1i—U1—Cl289.93 (3)O1—C1—N1118.69 (17)
O1—U1—Cl290.07 (3)N2—C1—N1122.42 (17)
Cl1i—U1—Cl289.167 (15)
Symmetry code: (i) x+1/2, y+1/2, z.
(farniv) Tetrabromo-bis(N,N,N',N'-tetramethylurea)-uranium(iv) top
Crystal data top
C10Br4N4O2Uγ = 90°
Mr = 765.81V = 2156.7 (12) Å3
C2/cZ = 4
a = 16.764 (5) ÅF(000) = 1344
b = 8.710 (4) ÅDx = 2.359 Mg m3
c = 16.655 (3) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 14.94 mm1
β = 117.52 (2)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.008
Graphite monochromatorθmax = 50.6°, θmin = 2.7°
9718 measured reflectionsh = 2626
3303 independent reflectionsk = 88
3198 reflections with I > 2σ(I)l = 2424
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.004Secondary atom site location: difference Fourier map
wR(F2) = 0.033 w = 1/[σ2(Fo2) + (0.P)2 + 0.0089P]
where P = (Fo2 + 2Fc2)/3
S = 0.39(Δ/σ)max = 1.266
3303 reflectionsΔρmax = 0.37 e Å3
42 parametersΔρmin = 0.36 e Å3
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
U10.2500000.2500000.0000000.02000 (3)*
Br10.397900 (6)0.054000 (13)0.071300 (7)0.02000 (3)*
Br20.361200 (7)0.506600 (12)0.055100 (7)0.02000 (3)*
N10.34020 (9)0.24560 (9)0.20330 (9)0.0200 (2)*
N20.18210 (7)0.23880 (11)0.28320 (8)0.0200 (2)*
O10.25540 (8)0.24970 (6)0.13030 (8)0.0200 (2)*
C10.25870 (10)0.24560 (10)0.20600 (11)0.0200 (3)*
C20.42070 (5)0.28650 (17)0.11930 (6)0.02000 (12)*
C30.35600 (6)0.16900 (12)0.27430 (7)0.02000 (16)*
C40.09800 (6)0.19720 (13)0.28080 (7)0.02000 (18)*
C50.17170 (7)0.31710 (10)0.36600 (8)0.02000 (18)*
Geometric parameters (Å, º) top
U1—O12.2134 (13)N1—C21.4699 (17)
U1—O1i2.2134 (13)N1—C31.4843 (17)
U1—Br22.7806 (9)N2—C11.334 (2)
U1—Br2i2.7806 (9)N2—C41.4740 (15)
U1—Br1i2.7841 (8)N2—C51.4748 (17)
U1—Br12.7841 (8)O1—C11.288 (2)
N1—C11.346 (2)
O1—U1—O1i180.00 (6)Br2i—U1—Br188.68 (3)
O1—U1—Br289.98 (3)Br1i—U1—Br1180.000 (5)
O1i—U1—Br290.02 (3)C1—N1—C2120.21 (12)
O1—U1—Br2i90.02 (3)C1—N1—C3121.69 (12)
O1i—U1—Br2i89.98 (3)C2—N1—C3116.35 (10)
Br2—U1—Br2i180.0C1—N2—C4119.44 (11)
O1—U1—Br1i90.82 (3)C1—N2—C5121.73 (10)
O1i—U1—Br1i89.18 (3)C4—N2—C5115.96 (10)
Br2—U1—Br1i88.68 (3)C1—O1—U1178.47 (6)
Br2i—U1—Br1i91.32 (3)O1—C1—N2119.15 (13)
O1—U1—Br189.18 (3)O1—C1—N1117.99 (14)
O1i—U1—Br190.82 (3)N2—C1—N1122.84 (14)
Br2—U1—Br191.32 (3)
Symmetry code: (i) x+1/2, y+1/2, z.
(himfue) (2,6-bis((Di-t-butylphosphino)methyl)phenoxy)-trifluoroacetato-palladium(ii) top
Crystal data top
C26H43F3O3P2Pdγ = 90°
Mr = 628.94V = 5761.9 (19) Å3
I2/aZ = 8
a = 20.244 (4) ÅF(000) = 2608
b = 10.714 (2) ÅDx = 1.450 Mg m3
c = 27.238 (5) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 0.80 mm1
β = 102.76 (3)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.016
Graphite monochromatorθmax = 47.4°, θmin = 1.5°
26382 measured reflectionsh = 3535
8546 independent reflectionsk = 1010
8103 reflections with I > 2σ(I)l = 4545
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)] = 0.014Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.065H atoms treated by a mixture of independent and constrained refinement
S = 0.64 w = 1/[σ2(Fo2) + (0.P)2 + 0.0757P]
where P = (Fo2 + 2Fc2)/3
8546 reflections(Δ/σ)max = 4.722
313 parametersΔρmax = 0.62 e Å3
0 restraintsΔρmin = 0.31 e Å3
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
Pd10.166400 (3)0.310100 (6)0.358900 (2)0.02000 (3)*
P10.262600 (10)0.42870 (2)0.353400 (8)0.02000 (4)*
P20.103200 (10)0.12920 (2)0.365800 (8)0.02000 (5)*
O10.20160 (3)0.19960 (5)0.31210 (3)0.02000 (12)*
O20.12750 (3)0.43130 (6)0.40390 (2)0.02000 (10)*
C10.08110 (4)0.49590 (8)0.38160 (3)0.02000 (13)*
O30.04970 (3)0.49200 (6)0.33760 (2)0.02000 (10)*
C20.05660 (4)0.59310 (8)0.41490 (3)0.02000 (12)*
F10.00680 (2)0.66760 (5)0.391300 (18)0.02000 (8)*
F20.10670 (2)0.66660 (5)0.437300 (18)0.02000 (8)*
F30.03350 (2)0.53820 (5)0.452100 (19)0.02000 (8)*
C30.25040 (4)0.13560 (8)0.34420 (3)0.02000 (13)*
C40.31530 (4)0.18580 (7)0.35650 (4)0.02000 (15)*
C50.36600 (4)0.11650 (8)0.38750 (3)0.02000 (12)*
C60.35020 (4)0.00390 (8)0.40620 (3)0.02000 (13)*
C70.28490 (4)0.04050 (8)0.39720 (3)0.02000 (12)*
C80.23240 (4)0.02780 (8)0.36640 (3)0.02000 (12)*
C90.32280 (4)0.31410 (7)0.33650 (3)0.02000 (15)*
C100.15790 (4)0.00260 (8)0.35510 (3)0.02000 (12)*
C110.31060 (3)0.50120 (8)0.41260 (3)0.02000 (13)*
C120.24400 (3)0.54040 (8)0.29880 (3)0.02000 (12)*
C130.33460 (4)0.39900 (9)0.44900 (3)0.02000 (12)*
C140.37210 (4)0.58130 (8)0.40370 (3)0.02000 (13)*
C150.26600 (4)0.58920 (8)0.43510 (3)0.02000 (13)*
C160.19420 (4)0.46850 (8)0.25690 (3)0.02000 (13)*
C170.30470 (4)0.57050 (8)0.27770 (3)0.02000 (13)*
C180.20690 (4)0.65410 (9)0.31240 (3)0.02000 (12)*
C190.02510 (4)0.10780 (8)0.31550 (3)0.02000 (12)*
C200.09060 (4)0.10040 (9)0.43090 (3)0.02000 (12)*
C210.05650 (4)0.02340 (8)0.43750 (3)0.02000 (12)*
C220.03300 (4)0.18590 (7)0.32590 (3)0.02000 (15)*
C230.00200 (4)0.02740 (8)0.30630 (3)0.02000 (13)*
C240.05000 (4)0.20590 (8)0.44820 (3)0.02000 (14)*
C250.16170 (4)0.10310 (9)0.46460 (3)0.02000 (12)*
C260.04280 (4)0.15510 (9)0.26740 (3)0.02000 (12)*
H10.4103 (6)0.1461 (12)0.3955 (5)0.020 (3)*
H20.3848 (6)0.0437 (12)0.4255 (5)0.020 (3)*
H30.2754 (6)0.1155 (12)0.4116 (5)0.020 (3)*
H40.3157 (7)0.3100 (10)0.3001 (5)0.020 (3)*
H50.3688 (6)0.3430 (13)0.3496 (5)0.020 (3)*
H60.1507 (6)0.0722 (11)0.3761 (5)0.020 (3)*
H70.1441 (6)0.0290 (12)0.3203 (5)0.020 (3)*
H80.3662 (6)0.3476 (12)0.4366 (5)0.020 (3)*
H90.2968 (6)0.3493 (12)0.4531 (5)0.020 (3)*
H100.3566 (6)0.4341 (12)0.4809 (5)0.020 (3)*
H110.3556 (6)0.6492 (12)0.3816 (5)0.020 (3)*
H120.4011 (6)0.5301 (12)0.3888 (5)0.020 (3)*
H130.3970 (6)0.6133 (12)0.4351 (5)0.020 (3)*
H140.2511 (6)0.6567 (13)0.4122 (5)0.020 (3)*
H150.2914 (6)0.6219 (11)0.4665 (5)0.020 (3)*
H160.2273 (6)0.5444 (12)0.4409 (5)0.020 (3)*
H170.1523 (6)0.4553 (12)0.2670 (5)0.020 (3)*
H180.2135 (6)0.3894 (11)0.2514 (5)0.020 (3)*
H190.1860 (6)0.5162 (12)0.2264 (5)0.020 (3)*
H200.3268 (6)0.4945 (12)0.2718 (5)0.020 (3)*
H210.3356 (6)0.6212 (11)0.3012 (5)0.020 (3)*
H220.2905 (6)0.6150 (12)0.2466 (5)0.020 (3)*
H230.1747 (6)0.6284 (11)0.3315 (5)0.020 (3)*
H240.1836 (7)0.6952 (10)0.2822 (5)0.020 (3)*
H250.2389 (6)0.7107 (12)0.3321 (5)0.020 (3)*
H260.0108 (6)0.0224 (12)0.4182 (5)0.020 (3)*
H270.0564 (6)0.0353 (12)0.4724 (5)0.020 (3)*
H280.0809 (6)0.0904 (12)0.4262 (5)0.020 (3)*
H290.0482 (6)0.1515 (13)0.3540 (5)0.020 (3)*
H300.0697 (7)0.1855 (10)0.2968 (5)0.020 (3)*
H310.0180 (6)0.2700 (13)0.3334 (5)0.020 (3)*
H320.0112 (6)0.0594 (11)0.3356 (5)0.020 (3)*
H330.0384 (6)0.0768 (11)0.2994 (5)0.020 (3)*
H340.0359 (6)0.0312 (12)0.2780 (5)0.020 (3)*
H350.0052 (7)0.2076 (12)0.4273 (5)0.020 (3)*
H360.0720 (6)0.2841 (13)0.4456 (5)0.020 (3)*
H370.0475 (7)0.1919 (10)0.4825 (5)0.020 (3)*
H380.1883 (6)0.0372 (12)0.4550 (5)0.020 (3)*
H390.1589 (6)0.0918 (12)0.4990 (5)0.020 (3)*
H400.1826 (7)0.1818 (11)0.4610 (5)0.020 (3)*
H410.0794 (6)0.1069 (11)0.2603 (5)0.020 (3)*
H420.0559 (6)0.2410 (12)0.2714 (5)0.020 (3)*
H430.0040 (6)0.1471 (12)0.2400 (5)0.020 (3)*
Geometric parameters (Å, º) top
Pd1—O11.9838 (7)C13—H100.961 (13)
Pd1—O22.0579 (7)C14—H110.956 (13)
Pd1—P22.3526 (4)C14—H120.957 (13)
Pd1—P12.3577 (4)C14—H130.955 (12)
Pd1—C32.6169 (9)C15—H140.959 (13)
P1—C91.8581 (9)C15—H150.961 (13)
P1—C111.8589 (9)C15—H160.961 (12)
P1—C121.8811 (9)C16—H170.958 (12)
P2—C101.8568 (9)C16—H180.959 (12)
P2—C191.8635 (10)C16—H190.958 (13)
P2—C201.8720 (9)C17—H200.960 (12)
O1—C31.3524 (11)C17—H210.959 (12)
O2—C11.2158 (10)C17—H220.959 (13)
C1—O31.2270 (10)C18—H230.960 (13)
C1—C21.5336 (12)C18—H240.960 (14)
C2—F21.3220 (10)C18—H250.960 (13)
C2—F11.3343 (9)C19—C261.5196 (12)
C2—F31.3419 (11)C19—C221.5202 (12)
C3—C81.3891 (12)C19—C231.5258 (12)
C3—C41.3904 (12)C20—C211.5241 (12)
C4—C51.3910 (12)C20—C251.5269 (11)
C4—C91.4986 (12)C20—C241.5318 (13)
C5—C61.3744 (12)C21—H260.958 (12)
C5—H10.931 (12)C21—H270.960 (12)
C6—C71.3750 (11)C21—H280.960 (12)
C6—H20.930 (13)C22—H290.959 (13)
C7—C81.4053 (12)C22—H300.959 (14)
C7—H30.933 (12)C22—H310.958 (13)
C8—C101.5068 (11)C23—H320.959 (12)
C9—H40.971 (14)C23—H330.959 (12)
C9—H50.971 (12)C23—H340.961 (12)
C10—H60.970 (12)C24—H350.959 (13)
C10—H70.969 (12)C24—H360.959 (13)
C11—C131.4850 (12)C24—H370.959 (14)
C11—C151.5245 (12)C25—H380.959 (12)
C11—C141.5744 (11)C25—H390.959 (13)
C12—C171.5021 (12)C25—H400.958 (12)
C12—C181.5193 (12)C26—H410.957 (12)
C12—C161.5505 (12)C26—H420.957 (13)
C13—H80.960 (13)C26—H430.960 (12)
C13—H90.959 (13)
O1—Pd1—O2176.64 (3)C11—C13—H10109.5 (8)
O1—Pd1—P280.71 (3)H8—C13—H10109.3 (10)
O2—Pd1—P2100.71 (2)H9—C13—H10109.5 (10)
O1—Pd1—P182.06 (3)C11—C14—H11109.5 (7)
O2—Pd1—P197.35 (2)C11—C14—H12109.4 (8)
P2—Pd1—P1156.998 (8)H11—C14—H12109.3 (10)
O1—Pd1—C330.41 (3)C11—C14—H13109.7 (8)
O2—Pd1—C3152.75 (3)H11—C14—H13109.4 (11)
P2—Pd1—C378.87 (2)H12—C14—H13109.5 (10)
P1—Pd1—C378.55 (2)C11—C15—H14109.5 (8)
C9—P1—C11104.20 (4)C11—C15—H15109.6 (7)
C9—P1—C12104.61 (4)H14—C15—H15109.5 (11)
C11—P1—C12113.26 (4)C11—C15—H16109.5 (8)
C9—P1—Pd1104.82 (3)H14—C15—H16109.4 (10)
C11—P1—Pd1116.81 (3)H15—C15—H16109.3 (11)
C12—P1—Pd1111.67 (3)C12—C16—H17109.6 (7)
C10—P2—C19103.27 (4)C12—C16—H18109.5 (7)
C10—P2—C20103.54 (4)H17—C16—H18109.4 (10)
C19—P2—C20113.90 (4)C12—C16—H19109.5 (7)
C10—P2—Pd1105.09 (3)H17—C16—H19109.4 (10)
C19—P2—Pd1115.51 (3)H18—C16—H19109.5 (11)
C20—P2—Pd1113.69 (3)C12—C17—H20109.4 (7)
C3—O1—Pd1101.65 (6)C12—C17—H21109.5 (8)
C1—O2—Pd1114.63 (6)H20—C17—H21109.5 (10)
O2—C1—O3130.16 (8)C12—C17—H22109.5 (7)
O2—C1—C2113.96 (7)H20—C17—H22109.5 (10)
O3—C1—C2115.81 (7)H21—C17—H22109.4 (11)
F2—C2—F1106.68 (7)C12—C18—H23109.5 (7)
F2—C2—F3105.81 (7)C12—C18—H24109.6 (8)
F1—C2—F3105.89 (6)H23—C18—H24109.4 (11)
F2—C2—C1111.23 (6)C12—C18—H25109.5 (8)
F1—C2—C1115.46 (7)H23—C18—H25109.5 (11)
F3—C2—C1111.17 (7)H24—C18—H25109.4 (10)
O1—C3—C8118.59 (7)C26—C19—C22108.46 (7)
O1—C3—C4118.43 (8)C26—C19—C23107.28 (7)
C8—C3—C4122.78 (7)C22—C19—C23109.36 (6)
O1—C3—Pd147.94 (4)C26—C19—P2105.64 (5)
C8—C3—Pd1106.59 (6)C22—C19—P2111.16 (6)
C4—C3—Pd1107.35 (6)C23—C19—P2114.65 (6)
C3—C4—C5118.10 (8)C21—C20—C25109.69 (7)
C3—C4—C9115.69 (7)C21—C20—C24108.55 (7)
C5—C4—C9126.15 (8)C25—C20—C24107.44 (7)
C6—C5—C4119.51 (7)C21—C20—P2114.53 (6)
C6—C5—H1120.2 (8)C25—C20—P2105.00 (6)
C4—C5—H1120.3 (8)C24—C20—P2111.37 (6)
C5—C6—C7122.06 (7)C20—C21—H26109.5 (8)
C5—C6—H2118.9 (8)C20—C21—H27109.4 (8)
C7—C6—H2119.1 (8)H26—C21—H27109.4 (10)
C6—C7—C8119.79 (8)C20—C21—H28109.5 (8)
C6—C7—H3120.2 (7)H26—C21—H28109.6 (10)
C8—C7—H3120.0 (8)H27—C21—H28109.4 (11)
C3—C8—C7117.15 (7)C19—C22—H29109.6 (8)
C3—C8—C10115.96 (7)C19—C22—H30109.5 (8)
C7—C8—C10126.89 (8)H29—C22—H30109.3 (11)
C4—C9—P1113.04 (7)C19—C22—H31109.6 (7)
C4—C9—H4109.0 (7)H29—C22—H31109.5 (11)
P1—C9—H4109.0 (7)H30—C22—H31109.4 (10)
C4—C9—H5108.9 (8)C19—C23—H32109.5 (7)
P1—C9—H5109.0 (8)C19—C23—H33109.6 (7)
H4—C9—H5107.7 (11)H32—C23—H33109.5 (10)
C8—C10—P2114.10 (6)C19—C23—H34109.5 (8)
C8—C10—H6108.6 (7)H32—C23—H34109.4 (10)
P2—C10—H6108.6 (7)H33—C23—H34109.4 (11)
C8—C10—H7108.8 (7)C20—C24—H35109.4 (8)
P2—C10—H7108.8 (7)C20—C24—H36109.4 (8)
H6—C10—H7107.7 (10)H35—C24—H36109.5 (11)
C13—C11—C15108.85 (7)C20—C24—H37109.4 (7)
C13—C11—C14110.58 (6)H35—C24—H37109.6 (11)
C15—C11—C14106.47 (7)H36—C24—H37109.5 (10)
C13—C11—P1107.60 (6)C20—C25—H38109.5 (7)
C15—C11—P1111.38 (5)C20—C25—H39109.5 (7)
C14—C11—P1111.95 (6)H38—C25—H39109.4 (10)
C17—C12—C18114.29 (7)C20—C25—H40109.5 (8)
C17—C12—C16106.20 (7)H38—C25—H40109.4 (11)
C18—C12—C16107.56 (6)H39—C25—H40109.5 (11)
C17—C12—P1113.66 (6)C19—C26—H41109.6 (8)
C18—C12—P1109.92 (6)C19—C26—H42109.6 (7)
C16—C12—P1104.47 (6)H41—C26—H42109.5 (10)
C11—C13—H8109.5 (8)C19—C26—H43109.4 (8)
C11—C13—H9109.6 (7)H41—C26—H43109.4 (11)
H8—C13—H9109.5 (11)H42—C26—H43109.4 (11)
(horbiz) trans-2-(alpha-Cumyl)cyclohexyl 2-(1,2-bis(benzyloxy)ethyl)-5-(tri-isopropylsily l)-2,3-dihydro-4H-4-pyridone-1-carboxylate top
Crystal data top
C47H63NO6Siγ = 90°
Mr = 766.07V = 8664 (2) Å3
I2/aZ = 8
a = 33.990 (4) ÅF(000) = 3312
b = 9.5179 (13) ÅDx = 1.175 Mg m3
c = 29.467 (4) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 0.10 mm1
β = 114.65 (3)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.020
Graphite monochromatorθmax = 45.1°, θmin = 1.3°
41716 measured reflectionsh = 5555
13023 independent reflectionsk = 1010
11934 reflections with I > 2σ(I)l = 4545
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.208H atoms treated by a mixture of independent and constrained refinement
S = 1.13 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
13023 reflections(Δ/σ)max = 13.453
473 parametersΔρmax = 1.14 e Å3
0 restraintsΔρmin = 0.24 e Å3
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
Si10.347800 (7)0.47870 (2)0.189600 (8)0.02000 (8)*
N10.36520 (2)0.36990 (7)0.04530 (2)0.02000 (13)*
O10.440800 (18)0.54280 (6)0.106700 (19)0.02000 (11)*
O20.394500 (19)0.10660 (6)0.03280 (2)0.02000 (11)*
O30.501900 (19)0.21040 (6)0.00240 (2)0.02000 (11)*
O40.517900 (19)0.05550 (6)0.07780 (2)0.02000 (11)*
O50.297600 (19)0.31790 (6)0.05030 (2)0.02000 (12)*
O60.357300 (19)0.29070 (6)0.02210 (2)0.02000 (11)*
C10.36400 (2)0.65510 (8)0.20590 (3)0.02000 (13)*
H10.3962 (5)0.6508 (13)0.1936 (5)0.020 (3)*
C20.35530 (2)0.77820 (8)0.17790 (2)0.02000 (13)*
H20.3648 (4)0.8659 (14)0.1877 (5)0.020 (3)*
H30.3714 (4)0.7640 (14)0.1419 (5)0.020 (3)*
H40.3243 (4)0.7835 (14)0.1863 (5)0.020 (3)*
C30.34710 (3)0.68620 (8)0.26120 (3)0.02000 (14)*
H50.3573 (4)0.7789 (14)0.2660 (5)0.020 (3)*
H60.3154 (4)0.6854 (14)0.2762 (5)0.020 (3)*
H70.3576 (4)0.6145 (14)0.2774 (5)0.020 (3)*
C40.28780 (2)0.45310 (8)0.21340 (3)0.02000 (13)*
H80.2835 (4)0.3619 (14)0.1991 (5)0.020 (3)*
C50.26370 (3)0.56530 (8)0.19690 (3)0.02000 (13)*
H90.2328 (4)0.5425 (15)0.2107 (5)0.020 (3)*
H100.2677 (4)0.6576 (14)0.2090 (5)0.020 (3)*
H110.2753 (4)0.5669 (14)0.1603 (5)0.020 (3)*
C60.26460 (2)0.43770 (8)0.27050 (3)0.02000 (12)*
H120.2336 (4)0.4236 (14)0.2804 (5)0.020 (3)*
H130.2765 (4)0.3567 (14)0.2811 (5)0.020 (3)*
H140.2691 (4)0.5231 (14)0.2864 (5)0.020 (3)*
C70.36920 (3)0.33680 (8)0.21800 (3)0.02000 (13)*
H150.3547 (4)0.3502 (14)0.2550 (5)0.020 (3)*
C80.41710 (2)0.34390 (8)0.20350 (3)0.02000 (13)*
H160.4256 (4)0.2677 (14)0.2200 (5)0.020 (3)*
H170.4327 (5)0.3340 (14)0.1672 (5)0.020 (3)*
H180.4243 (4)0.4345 (14)0.2139 (5)0.020 (3)*
C90.35740 (3)0.18820 (8)0.20750 (3)0.02000 (13)*
H190.3690 (4)0.1189 (14)0.2233 (5)0.020 (3)*
H200.3258 (5)0.1791 (14)0.2210 (5)0.020 (3)*
H210.3698 (4)0.1720 (14)0.1713 (5)0.020 (3)*
C100.37220 (2)0.45430 (8)0.11990 (3)0.02000 (13)*
C110.41720 (3)0.49120 (8)0.08880 (3)0.02000 (13)*
C120.43450 (3)0.47060 (8)0.03320 (3)0.02000 (14)*
H220.4308 (4)0.5591 (14)0.0177 (5)0.020 (3)*
H230.4658 (4)0.4500 (15)0.0198 (5)0.020 (3)*
C130.41190 (2)0.35250 (8)0.01880 (2)0.02000 (13)*
H240.4204 (4)0.3558 (14)0.0180 (5)0.020 (3)*
C140.34870 (2)0.40330 (8)0.09560 (3)0.02000 (14)*
H250.3186 (4)0.3896 (14)0.1148 (5)0.020 (3)*
C150.42540 (2)0.20720 (8)0.03280 (3)0.02000 (13)*
H260.4243 (4)0.2132 (14)0.0671 (5)0.020 (3)*
C160.47090 (3)0.17010 (8)0.00370 (3)0.02000 (13)*
C170.47420 (2)0.07980 (8)0.04740 (3)0.02000 (13)*
H270.4603 (4)0.1281 (14)0.0667 (5)0.020 (3)*
H280.4591 (4)0.0107 (14)0.0351 (5)0.020 (3)*
C180.52350 (3)0.03270 (8)0.11590 (3)0.02000 (13)*
H290.5535 (4)0.0687 (14)0.1297 (5)0.020 (3)*
H300.5038 (4)0.1139 (15)0.1027 (5)0.020 (3)*
C190.51480 (3)0.03570 (8)0.15870 (3)0.02000 (14)*
C200.53490 (3)0.13810 (7)0.18620 (3)0.02000 (13)*
H310.5552 (4)0.1880 (14)0.1778 (5)0.020 (3)*
C210.52900 (3)0.18000 (8)0.22620 (3)0.02000 (13)*
H320.5469 (4)0.2530 (15)0.2462 (5)0.020 (3)*
C220.50200 (3)0.12920 (8)0.23850 (3)0.02000 (13)*
H330.4972 (5)0.1678 (14)0.2654 (5)0.020 (3)*
C230.47900 (3)0.01670 (8)0.21290 (3)0.02000 (14)*
H340.4590 (5)0.0304 (14)0.2224 (5)0.020 (3)*
C240.48660 (3)0.02760 (7)0.17050 (3)0.02000 (13)*
H350.4707 (5)0.1047 (14)0.1509 (5)0.020 (3)*
C250.38910 (3)0.01040 (8)0.06610 (3)0.02000 (13)*
H360.4147 (4)0.0724 (14)0.0525 (5)0.020 (3)*
H370.3855 (4)0.0240 (13)0.0993 (5)0.020 (3)*
C260.35010 (3)0.08800 (8)0.07050 (3)0.02000 (13)*
C270.35380 (2)0.21340 (8)0.04670 (3)0.02000 (13)*
H380.3812 (4)0.2541 (14)0.0268 (5)0.020 (3)*
C280.31080 (2)0.28480 (8)0.05380 (3)0.02000 (13)*
H390.3086 (4)0.3714 (14)0.0392 (5)0.020 (3)*
C290.27370 (2)0.19830 (8)0.08690 (3)0.02000 (13)*
H400.2457 (4)0.2359 (14)0.0948 (5)0.020 (3)*
C300.27500 (3)0.08010 (8)0.10590 (3)0.02000 (13)*
H410.2492 (4)0.0303 (13)0.1253 (5)0.020 (3)*
C310.31090 (3)0.03180 (8)0.09860 (3)0.02000 (14)*
H420.3110 (4)0.0550 (15)0.1145 (5)0.020 (3)*
C320.33590 (3)0.32310 (8)0.02630 (3)0.02000 (14)*
C330.33260 (3)0.21700 (8)0.04540 (3)0.02000 (13)*
H430.3025 (4)0.2553 (14)0.0323 (5)0.020 (3)*
C340.33130 (2)0.06420 (8)0.03210 (3)0.02000 (13)*
H440.3613 (5)0.0297 (14)0.0421 (5)0.020 (3)*
H450.3157 (4)0.0532 (15)0.0046 (5)0.020 (3)*
C350.30900 (3)0.02490 (8)0.05770 (3)0.02000 (14)*
H460.2787 (4)0.0064 (14)0.0470 (5)0.020 (3)*
H470.3088 (4)0.1248 (14)0.0481 (5)0.020 (3)*
C360.33260 (2)0.00970 (8)0.11200 (3)0.02000 (13)*
H480.3628 (4)0.0428 (14)0.1226 (5)0.020 (3)*
H490.3187 (4)0.0679 (15)0.1290 (5)0.020 (3)*
C370.33260 (3)0.14280 (8)0.12650 (3)0.02000 (13)*
H500.3478 (5)0.1514 (14)0.1633 (5)0.020 (3)*
H510.3024 (5)0.1744 (14)0.1163 (5)0.020 (3)*
C380.35550 (3)0.24180 (8)0.10160 (3)0.02000 (13)*
H520.3855 (4)0.2041 (14)0.1122 (5)0.020 (3)*
C390.36080 (2)0.39670 (8)0.11800 (3)0.02000 (13)*
C400.31780 (3)0.47410 (7)0.09080 (3)0.02000 (14)*
H530.3095 (4)0.4706 (14)0.0547 (5)0.020 (3)*
H540.3212 (4)0.5724 (14)0.1018 (5)0.020 (3)*
H550.2954 (4)0.4292 (14)0.0985 (5)0.020 (3)*
C410.37470 (2)0.40660 (8)0.17560 (3)0.02000 (13)*
H560.3774 (5)0.5056 (14)0.1857 (5)0.020 (3)*
H570.4025 (4)0.3591 (14)0.1931 (5)0.020 (3)*
H580.3528 (5)0.3612 (14)0.1841 (5)0.020 (3)*
C420.39730 (3)0.46480 (8)0.10870 (3)0.02000 (14)*
C430.39200 (2)0.59350 (8)0.08540 (3)0.02000 (13)*
H590.3648 (4)0.6403 (14)0.0737 (5)0.020 (3)*
C440.42890 (2)0.65870 (8)0.07870 (3)0.02000 (13)*
H600.4257 (4)0.7465 (15)0.0622 (5)0.020 (3)*
C450.46690 (2)0.59010 (8)0.09670 (3)0.02000 (13)*
H610.4909 (4)0.6305 (14)0.0930 (5)0.020 (3)*
C460.47160 (3)0.46680 (8)0.11950 (3)0.02000 (14)*
H620.4985 (4)0.4190 (14)0.1313 (5)0.020 (3)*
C470.43780 (3)0.41010 (8)0.12580 (3)0.02000 (13)*
H630.4429 (5)0.3244 (14)0.1439 (5)0.020 (3)*
Geometric parameters (Å, º) top
Si1—C41.8754 (9)C19—C241.2964 (11)
Si1—C101.8813 (9)C20—C211.3363 (11)
Si1—C71.8871 (8)C20—H310.952 (13)
Si1—C11.8903 (8)C21—C221.2185 (12)
N1—C141.3853 (10)C21—H320.949 (14)
N1—C321.4031 (10)C22—C231.3546 (11)
N1—C131.4570 (10)C22—H330.948 (13)
O1—C111.2312 (10)C23—C241.4404 (11)
O2—C151.4212 (10)C23—H340.949 (14)
O2—C251.4444 (10)C24—H350.951 (14)
O3—C161.2032 (10)C25—C261.4752 (11)
O4—C181.3502 (9)C25—H360.987 (14)
O4—C171.3973 (10)C25—H370.990 (13)
O5—C321.1956 (11)C26—C311.3516 (11)
O6—C321.3390 (10)C26—C271.3633 (11)
O6—C331.4660 (10)C27—C281.5449 (11)
C1—C31.5140 (11)C27—H380.952 (13)
C1—C21.5312 (11)C28—C291.4810 (11)
C1—H11.000 (14)C28—H390.947 (13)
C2—H20.981 (14)C29—C301.2656 (10)
C2—H30.979 (13)C29—H400.950 (14)
C2—H40.978 (13)C30—C311.2360 (11)
C3—H50.980 (13)C30—H410.950 (14)
C3—H60.979 (13)C31—H420.950 (13)
C3—H70.981 (14)C33—C341.5021 (11)
C4—C61.5387 (11)C33—C381.5260 (11)
C4—C51.5427 (11)C33—H431.000 (13)
C4—H81.002 (13)C34—C351.5296 (11)
C5—H90.979 (13)C34—H440.992 (14)
C5—H100.979 (13)C34—H450.992 (13)
C5—H110.982 (13)C35—C361.4676 (11)
C6—H120.978 (13)C35—H460.989 (13)
C6—H130.980 (13)C35—H470.991 (14)
C6—H140.982 (13)C36—C371.5131 (10)
C7—C81.5025 (11)C36—H480.991 (13)
C7—C91.5364 (11)C36—H490.989 (13)
C7—H151.000 (14)C37—C381.5838 (11)
C8—H160.981 (13)C37—H500.991 (13)
C8—H170.980 (14)C37—H510.988 (14)
C8—H180.980 (13)C38—C391.5385 (11)
C9—H190.980 (13)C38—H521.000 (13)
C9—H200.981 (14)C39—C421.5225 (11)
C9—H210.982 (13)C39—C401.5310 (12)
C10—C141.3651 (11)C39—C411.5633 (11)
C10—C111.4606 (11)C40—H530.981 (13)
C11—C121.5049 (10)C40—H540.981 (13)
C12—C131.5184 (11)C40—H550.979 (13)
C12—H220.991 (13)C41—H560.981 (13)
C12—H230.988 (13)C41—H570.978 (14)
C13—C151.5656 (11)C41—H580.979 (13)
C13—H241.000 (13)C42—C471.3570 (11)
C14—H250.949 (14)C42—C431.3788 (11)
C15—C161.5119 (12)C43—C441.4845 (11)
C15—H260.997 (13)C43—H590.952 (14)
C16—C171.5129 (10)C44—C451.3433 (11)
C17—H270.991 (13)C44—H600.950 (14)
C17—H280.991 (13)C45—C461.3284 (10)
C18—C191.5534 (11)C45—H610.948 (13)
C18—H290.988 (13)C46—C471.3504 (12)
C18—H300.990 (14)C46—H620.948 (13)
C19—C201.2695 (10)C47—H630.950 (13)
C4—Si1—C10107.92 (4)C21—C20—H31118.2 (8)
C4—Si1—C7107.54 (4)C22—C21—C20123.55 (7)
C10—Si1—C7108.65 (4)C22—C21—H32118.2 (8)
C4—Si1—C1114.01 (4)C20—C21—H32118.2 (8)
C10—Si1—C1110.15 (4)C21—C22—C23118.64 (7)
C7—Si1—C1108.42 (4)C21—C22—H33120.6 (8)
C14—N1—C32117.50 (7)C23—C22—H33120.8 (8)
C14—N1—C13117.64 (6)C22—C23—C24116.35 (7)
C32—N1—C13123.09 (6)C22—C23—H34121.8 (8)
C15—O2—C25113.82 (6)C24—C23—H34121.8 (8)
C18—O4—C17112.30 (6)C19—C24—C23121.11 (7)
C32—O6—C33116.50 (6)C19—C24—H35119.5 (8)
C3—C1—C2111.01 (6)C23—C24—H35119.4 (8)
C3—C1—Si1115.29 (5)O2—C25—C26107.50 (6)
C2—C1—Si1113.61 (5)O2—C25—H36110.1 (8)
C3—C1—H1105.3 (7)C26—C25—H36110.1 (8)
C2—C1—H1105.3 (7)O2—C25—H37110.2 (8)
Si1—C1—H1105.2 (7)C26—C25—H37110.0 (8)
C1—C2—H2109.3 (8)H36—C25—H37108.9 (11)
C1—C2—H3109.4 (8)C31—C26—C27121.16 (7)
H2—C2—H3109.4 (11)C31—C26—C25118.41 (7)
C1—C2—H4109.4 (8)C27—C26—C25120.42 (7)
H2—C2—H4109.5 (11)C26—C27—C28115.87 (7)
H3—C2—H4109.7 (10)C26—C27—H38122.0 (8)
C1—C3—H5109.5 (8)C28—C27—H38122.1 (8)
C1—C3—H6109.7 (8)C29—C28—C27110.01 (7)
H5—C3—H6109.3 (11)C29—C28—H39125.2 (8)
C1—C3—H7109.6 (8)C27—C28—H39124.8 (8)
H5—C3—H7109.5 (11)C30—C29—C28127.46 (7)
H6—C3—H7109.3 (11)C30—C29—H40116.3 (8)
C6—C4—C5108.25 (6)C28—C29—H40116.3 (8)
C6—C4—Si1113.75 (6)C31—C30—C29117.89 (8)
C5—C4—Si1115.45 (5)C31—C30—H41121.0 (8)
C6—C4—H8106.2 (8)C29—C30—H41121.1 (8)
C5—C4—H8106.1 (7)C30—C31—C26127.51 (8)
Si1—C4—H8106.4 (8)C30—C31—H42116.3 (8)
C4—C5—H9109.5 (8)C26—C31—H42116.1 (8)
C4—C5—H10109.5 (8)O5—C32—O6126.46 (8)
H9—C5—H10109.6 (11)O5—C32—N1123.78 (7)
C4—C5—H11109.5 (8)O6—C32—N1109.72 (7)
H9—C5—H11109.2 (10)O6—C33—C34107.54 (6)
H10—C5—H11109.5 (11)O6—C33—C38107.56 (6)
C4—C6—H12109.6 (8)C34—C33—C38112.28 (6)
C4—C6—H13109.4 (8)O6—C33—H43109.8 (7)
H12—C6—H13109.5 (12)C34—C33—H43109.8 (8)
C4—C6—H14109.4 (8)C38—C33—H43109.8 (8)
H12—C6—H14109.5 (11)C33—C34—C35112.01 (6)
H13—C6—H14109.4 (11)C33—C34—H44109.2 (8)
C8—C7—C9109.09 (6)C35—C34—H44109.2 (8)
C8—C7—Si1114.46 (5)C33—C34—H45109.3 (8)
C9—C7—Si1112.85 (6)C35—C34—H45109.3 (8)
C8—C7—H15106.7 (8)H44—C34—H45107.8 (10)
C9—C7—H15106.6 (8)C36—C35—C34108.97 (7)
Si1—C7—H15106.6 (8)C36—C35—H46109.9 (7)
C7—C8—H16109.5 (8)C34—C35—H46109.9 (8)
C7—C8—H17109.6 (8)C36—C35—H47110.0 (8)
H16—C8—H17109.4 (11)C34—C35—H47109.7 (8)
C7—C8—H18109.5 (8)H46—C35—H47108.4 (11)
H16—C8—H18109.4 (11)C35—C36—C37109.76 (6)
H17—C8—H18109.5 (11)C35—C36—H48109.6 (8)
C7—C9—H19109.5 (8)C37—C36—H48109.7 (8)
C7—C9—H20109.5 (7)C35—C36—H49109.7 (8)
H19—C9—H20109.7 (11)C37—C36—H49109.8 (8)
C7—C9—H21109.5 (8)H48—C36—H49108.2 (11)
H19—C9—H21109.6 (11)C36—C37—C38112.46 (6)
H20—C9—H21109.1 (10)C36—C37—H50109.1 (8)
C14—C10—C11116.43 (6)C38—C37—H50109.0 (8)
C14—C10—Si1121.91 (6)C36—C37—H51109.2 (8)
C11—C10—Si1121.65 (6)C38—C37—H51109.1 (8)
O1—C11—C10121.74 (7)H50—C37—H51108.0 (11)
O1—C11—C12119.33 (7)C33—C38—C39115.40 (6)
C10—C11—C12118.89 (7)C33—C38—C37106.49 (6)
C11—C12—C13112.78 (6)C39—C38—C37116.13 (6)
C11—C12—H22108.9 (8)C33—C38—H52106.0 (8)
C13—C12—H22108.9 (8)C39—C38—H52106.0 (8)
C11—C12—H23109.1 (8)C37—C38—H52106.0 (8)
C13—C12—H23109.1 (8)C42—C39—C40111.87 (6)
H22—C12—H23107.9 (11)C42—C39—C38110.42 (6)
N1—C13—C12109.34 (6)C40—C39—C38109.60 (6)
N1—C13—C15109.43 (6)C42—C39—C41105.65 (6)
C12—C13—C15110.01 (6)C40—C39—C41109.24 (6)
N1—C13—H24109.6 (8)C38—C39—C41109.97 (6)
C12—C13—H24109.2 (7)C39—C40—H53109.4 (8)
C15—C13—H24109.3 (8)C39—C40—H54109.3 (8)
C10—C14—N1125.34 (7)H53—C40—H54109.4 (11)
C10—C14—H25117.2 (8)C39—C40—H55109.5 (8)
N1—C14—H25117.4 (8)H53—C40—H55109.7 (11)
O2—C15—C16112.29 (6)H54—C40—H55109.6 (11)
O2—C15—C13107.30 (6)C39—C41—H56109.6 (8)
C16—C15—C13110.13 (6)C39—C41—H57109.4 (8)
O2—C15—H26108.9 (8)H56—C41—H57109.7 (11)
C16—C15—H26109.2 (8)C39—C41—H58109.5 (8)
C13—C15—H26109.0 (8)H56—C41—H58109.3 (11)
O3—C16—C15121.26 (7)H57—C41—H58109.4 (12)
O3—C16—C17123.34 (7)C47—C42—C43115.30 (8)
C15—C16—C17115.40 (6)C47—C42—C39123.12 (7)
O4—C17—C16108.74 (6)C43—C42—C39121.39 (7)
O4—C17—H27110.0 (8)C42—C43—C44119.70 (7)
C16—C17—H27109.9 (8)C42—C43—H59120.1 (8)
O4—C17—H28109.9 (8)C44—C43—H59120.2 (8)
C16—C17—H28109.8 (8)C45—C44—C43118.09 (7)
H27—C17—H28108.4 (11)C45—C44—H60121.0 (8)
O4—C18—C19113.95 (6)C43—C44—H60120.9 (7)
O4—C18—H29108.7 (8)C46—C45—C44121.47 (8)
C19—C18—H29108.9 (8)C46—C45—H61119.2 (8)
O4—C18—H30108.7 (7)C44—C45—H61119.3 (8)
C19—C18—H30108.6 (8)C45—C46—C47119.53 (8)
H29—C18—H30107.7 (11)C45—C46—H62120.2 (8)
C20—C19—C24116.54 (7)C47—C46—H62120.2 (8)
C20—C19—C18127.30 (7)C46—C47—C42125.81 (7)
C24—C19—C18115.81 (7)C46—C47—H63117.0 (8)
C19—C20—C21123.60 (8)C42—C47—H63117.2 (8)
C19—C20—H31118.2 (8)
(pejvab) bis(mu!2$-Ethane-1,2-dithiolato-S,S,S',S')-bis(ethene-1,2-dithiolato)- -technetium(iv) top
Crystal data top
C8H12S8Tc2γ = 90°
Mr = 560.66V = 844.2 (8) Å3
I2/mZ = 2
a = 11.361 (6) ÅF(000) = 548
b = 8.303 (5) ÅDx = 2.206 Mg m3
c = 8.987 (5) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 2.61 mm1
β = 95.25 (5)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.016
Graphite monochromatorθmax = 68.7°, θmin = 2.8°
6858 measured reflectionsh = 2727
2519 independent reflectionsk = 99
2178 reflections with I > 2σ(I)l = 1818
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)] = 0.010Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.065H atoms treated by a mixture of independent and constrained refinement
S = 0.42 w = 1/[σ2(Fo2) + (0.P)2 + 0.0178P]
where P = (Fo2 + 2Fc2)/3
2519 reflections(Δ/σ)max = 2.510
38 parametersΔρmax = 0.87 e Å3
0 restraintsΔρmin = 1.25 e Å3
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
Tc10.401300 (6)0.00000.063600 (7)0.02000 (4)*
S10.436700 (15)0.17480 (3)0.138900 (19)0.02000 (4)*
S30.20160 (2)0.00000.00570 (3)0.02000 (5)*
S40.34530 (2)0.00000.30230 (3)0.02000 (5)*
C10.36160 (7)0.08990 (10)0.31090 (8)0.02000 (10)*
C30.12240 (9)0.00000.16090 (10)0.02000 (12)*
C40.18580 (9)0.00000.30030 (11)0.02000 (12)*
H10.4060 (14)0.131 (2)0.4050 (19)0.020 (3)*
H20.2713 (13)0.132 (2)0.3223 (17)0.020 (3)*
H50.0275 (19)0.00000.152 (3)0.020 (5)*
H60.142 (2)0.00000.400 (3)0.020 (5)*
Geometric parameters (Å, º) top
Tc1—S42.2927 (13)S3—C31.8160 (14)
Tc1—S32.2971 (13)S4—C41.8105 (14)
Tc1—S1i2.3904 (10)C1—C1i1.4929 (19)
Tc1—S12.3904 (10)C1—H11.080 (16)
Tc1—S1ii2.3925 (10)C1—H21.079 (15)
Tc1—S1iii2.3925 (10)C3—C41.3868 (17)
Tc1—Tc1iii2.6087 (14)C3—H51.07 (2)
S1—C11.8366 (12)C4—H61.06 (2)
S1—Tc1iii2.3925 (10)
S4—Tc1—S384.37 (5)S1ii—Tc1—Tc1iii56.91 (3)
S4—Tc1—S1i142.44 (2)S1iii—Tc1—Tc1iii56.91 (3)
S3—Tc1—S1i91.40 (4)C1—S1—Tc1108.07 (5)
S4—Tc1—S1142.44 (2)C1—S1—Tc1iii106.94 (5)
S3—Tc1—S191.40 (4)Tc1—S1—Tc1iii66.11 (4)
S1i—Tc1—S174.77 (5)C3—S3—Tc1109.15 (6)
S4—Tc1—S1ii90.43 (4)C4—S4—Tc1110.73 (6)
S3—Tc1—S1ii142.36 (2)C1i—C1—S1112.57 (3)
S1i—Tc1—S1ii113.89 (4)C1i—C1—H1108.6 (9)
S1—Tc1—S1ii70.63 (4)S1—C1—H1108.8 (9)
S4—Tc1—S1iii90.43 (4)C1i—C1—H2108.8 (9)
S3—Tc1—S1iii142.36 (2)S1—C1—H2108.7 (8)
S1i—Tc1—S1iii70.63 (4)H1—C1—H2109.3 (12)
S1—Tc1—S1iii113.89 (4)C4—C3—S3119.29 (9)
S1ii—Tc1—S1iii74.69 (5)C4—C3—H5120.4 (12)
S4—Tc1—Tc1iii137.16 (3)S3—C3—H5120.3 (12)
S3—Tc1—Tc1iii138.46 (3)C3—C4—S4116.46 (9)
S1i—Tc1—Tc1iii56.98 (3)C3—C4—H6121.5 (12)
S1—Tc1—Tc1iii56.98 (3)S4—C4—H6122.1 (12)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z; (iii) x+1, y, z.
(sixfio) (eta$3!-Allyl)-(N,N'-dimethyl-2-(diphenylphosphanyl)aniline-N,P)-palladium(ii) hexafluorophosphate top
Crystal data top
C23H25F6NP2Pdγ = 90°
Mr = 597.78V = 2425.1 (17) Å3
IaZ = 4
a = 15.197 (6) ÅF(000) = 1200
b = 9.042 (3) ÅDx = 1.637 Mg m3
c = 18.559 (9) ÅMo Kα radiation, λ = 0.71070 Å
α = 90°µ = 0.96 mm1
β = 108.02 (4)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.013
Graphite monochromatorθmax = 44.9°, θmin = 2.3°
9712 measured reflectionsh = 2222
6772 independent reflectionsk = 99
6443 reflections with I > 2σ(I)l = 3131
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.009H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.032 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.16(Δ/σ)max = 0.783
6772 reflectionsΔρmax = 0.18 e Å3
233 parametersΔρmin = 0.19 e Å3
2 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.004 (6)
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
Pd10.136600 (4)0.277800 (6)0.071000 (4)0.02000 (2)*
P10.286000 (16)0.33420 (2)0.131900 (14)0.02000 (4)*
N10.13570 (5)0.18680 (10)0.17890 (4)0.02000 (11)*
C10.30530 (7)0.22880 (9)0.22060 (6)0.02000 (17)*
C20.39300 (7)0.20910 (9)0.27130 (6)0.02000 (16)*
H10.4442 (11)0.2513 (16)0.2619 (9)0.020 (3)*
C30.40390 (6)0.12530 (10)0.33660 (5)0.02000 (13)*
H20.4625 (9)0.1100 (15)0.3708 (7)0.020 (3)*
C40.32860 (6)0.06680 (10)0.34950 (5)0.02000 (13)*
H30.3360 (9)0.0136 (15)0.3939 (7)0.020 (3)*
C50.24160 (6)0.08290 (10)0.29960 (5)0.02000 (13)*
H40.1908 (9)0.0399 (15)0.3094 (8)0.020 (3)*
C60.23010 (6)0.16590 (9)0.23270 (5)0.02000 (15)*
C70.08630 (6)0.04110 (9)0.16260 (5)0.02000 (14)*
H50.0254 (9)0.0556 (15)0.1278 (8)0.020 (3)*
H60.0816 (9)0.0003 (16)0.2090 (8)0.020 (3)*
H70.1202 (9)0.0253 (15)0.1407 (7)0.020 (3)*
C80.08270 (7)0.29020 (9)0.21360 (6)0.02000 (16)*
H80.0216 (10)0.3045 (16)0.1791 (8)0.020 (3)*
H90.1142 (9)0.3835 (16)0.2239 (8)0.020 (3)*
H100.0786 (11)0.2485 (16)0.2600 (9)0.020 (3)*
C90.01070 (7)0.27000 (9)0.00150 (6)0.02000 (17)*
H110.0438 (10)0.1782 (16)0.0015 (8)0.020 (3)*
H120.0477 (10)0.3578 (16)0.0023 (8)0.020 (3)*
C100.04710 (7)0.27330 (8)0.04370 (6)0.02000 (17)*
H130.0358 (11)0.2043 (16)0.0827 (9)0.020 (3)*
C110.11920 (6)0.36460 (11)0.03620 (5)0.02000 (13)*
H140.1047 (9)0.4692 (15)0.0424 (7)0.020 (3)*
H150.1639 (10)0.3335 (15)0.0607 (8)0.020 (3)*
C120.37580 (7)0.28290 (8)0.09130 (6)0.02000 (17)*
C130.35470 (6)0.18820 (12)0.02930 (5)0.02000 (12)*
H310.2942 (10)0.1451 (15)0.0104 (8)0.020 (3)*
C140.42180 (6)0.15360 (9)0.00470 (5)0.02000 (15)*
H320.4076 (9)0.0873 (16)0.0472 (8)0.020 (3)*
C150.51000 (7)0.21400 (9)0.02340 (6)0.02000 (17)*
H330.5563 (10)0.1906 (17)0.0003 (8)0.020 (3)*
C160.53110 (6)0.30870 (11)0.08530 (5)0.02000 (12)*
H340.5917 (9)0.3517 (15)0.1041 (8)0.020 (3)*
C170.46400 (6)0.34320 (9)0.11930 (5)0.02000 (15)*
H350.4783 (9)0.4095 (15)0.1617 (8)0.020 (3)*
C180.30760 (6)0.52580 (10)0.15740 (5)0.02000 (13)*
C190.29680 (6)0.62700 (10)0.09890 (5)0.02000 (13)*
H360.2787 (9)0.5931 (16)0.0474 (8)0.020 (3)*
C200.31250 (7)0.77660 (9)0.11520 (6)0.02000 (17)*
H370.3056 (9)0.8460 (15)0.0747 (8)0.020 (3)*
C210.33920 (6)0.82500 (10)0.18990 (5)0.02000 (14)*
H380.3505 (9)0.9282 (16)0.2010 (8)0.020 (3)*
C220.35010 (7)0.72370 (8)0.24840 (6)0.02000 (18)*
H390.3685 (11)0.7576 (16)0.3000 (9)0.020 (3)*
C230.33440 (6)0.57430 (10)0.23220 (5)0.02000 (13)*
H400.3416 (9)0.5048 (15)0.2728 (7)0.020 (3)*
P20.170000 (15)0.63070 (3)0.375400 (13)0.02000 (4)*
F10.15630 (3)0.68450 (7)0.29300 (3)0.02000 (8)*
F20.18200 (3)0.57270 (6)0.45920 (3)0.02000 (9)*
F30.27140 (4)0.69320 (7)0.40210 (3)0.02000 (9)*
F40.13170 (4)0.78090 (5)0.39450 (4)0.02000 (12)*
F50.20920 (3)0.47680 (6)0.35770 (3)0.02000 (9)*
F60.06910 (4)0.56400 (6)0.34930 (3)0.02000 (9)*
Geometric parameters (Å, º) top
Pd1—C112.0781 (13)C10—H130.930 (15)
Pd1—C102.1428 (16)C11—H140.970 (14)
Pd1—N12.1689 (12)C11—H150.969 (14)
Pd1—C92.2278 (15)C12—C131.3899 (15)
Pd1—P12.2594 (11)C12—C171.3903 (14)
P1—C181.7992 (11)C13—C141.3907 (15)
P1—C121.8115 (13)C13—H310.960 (14)
P1—C11.8454 (12)C14—C151.3908 (14)
N1—C61.4848 (13)C14—H320.961 (14)
N1—C71.5001 (13)C15—C161.3885 (14)
N1—C81.5028 (13)C15—H330.962 (15)
C1—C61.3560 (14)C16—C171.3905 (15)
C1—C21.3847 (15)C16—H340.960 (14)
C2—C31.3950 (14)C17—H350.959 (13)
C2—H10.930 (16)C18—C191.3902 (13)
C3—C41.3476 (13)C18—C231.3912 (14)
C3—H20.930 (12)C19—C201.3905 (13)
C4—C51.3672 (13)C19—H360.959 (14)
C4—H30.930 (13)C20—C211.3893 (15)
C5—C61.4146 (14)C20—H370.960 (14)
C5—H40.931 (13)C21—C221.3906 (14)
C7—H50.960 (13)C21—H380.960 (14)
C7—H60.962 (14)C22—C231.3885 (13)
C7—H70.959 (13)C22—H390.961 (16)
C8—H80.960 (14)C23—H400.961 (13)
C8—H90.960 (14)P2—F11.5562 (9)
C8—H100.960 (16)P2—F41.5609 (7)
C9—C101.3459 (17)P2—F31.5707 (8)
C9—H110.971 (15)P2—F61.5780 (8)
C9—H120.970 (14)P2—F51.5876 (7)
C10—C111.3443 (14)P2—F21.5974 (9)
C11—Pd1—C1037.10 (4)C11—C10—H13116.1 (10)
C11—Pd1—N1172.71 (3)C9—C10—H13116.2 (10)
C10—Pd1—N1136.61 (4)Pd1—C10—H13133.9 (9)
C11—Pd1—C968.11 (5)C10—C11—Pd174.06 (7)
C10—Pd1—C935.80 (5)C10—C11—H14116.0 (8)
N1—Pd1—C9104.68 (5)Pd1—C11—H14116.0 (8)
C11—Pd1—P1101.79 (4)C10—C11—H15116.1 (8)
C10—Pd1—P1137.06 (4)Pd1—C11—H15116.1 (8)
N1—Pd1—P185.19 (4)H14—C11—H15113.2 (11)
C9—Pd1—P1167.37 (3)C13—C12—C17119.99 (10)
C18—P1—C12104.85 (4)C13—C12—P1119.44 (8)
C18—P1—C1107.27 (5)C17—C12—P1120.49 (8)
C12—P1—C1107.85 (5)C12—C13—C14120.03 (9)
C18—P1—Pd1114.98 (3)C12—C13—H31120.2 (9)
C12—P1—Pd1120.26 (4)C14—C13—H31119.8 (9)
C1—P1—Pd1100.81 (5)C13—C14—C15119.89 (9)
C6—N1—C7110.06 (7)C13—C14—H32120.2 (8)
C6—N1—C8108.99 (8)C15—C14—H32119.9 (8)
C7—N1—C8109.37 (7)C16—C15—C14120.10 (10)
C6—N1—Pd1112.86 (7)C16—C15—H33120.0 (9)
C7—N1—Pd1107.02 (6)C14—C15—H33119.9 (9)
C8—N1—Pd1108.48 (6)C15—C16—C17119.98 (9)
C6—C1—C2121.12 (10)C15—C16—H34120.0 (8)
C6—C1—P1117.05 (8)C17—C16—H34120.0 (8)
C2—C1—P1121.77 (8)C12—C17—C16120.00 (9)
C1—C2—C3119.40 (10)C12—C17—H35120.0 (8)
C1—C2—H1120.3 (10)C16—C17—H35120.0 (8)
C3—C2—H1120.3 (10)C19—C18—C23119.95 (9)
C4—C3—C2119.23 (9)C19—C18—P1117.42 (7)
C4—C3—H2120.4 (8)C23—C18—P1122.63 (7)
C2—C3—H2120.3 (8)C18—C19—C20119.97 (9)
C3—C4—C5122.29 (9)C18—C19—H36119.7 (8)
C3—C4—H3118.9 (8)C20—C19—H36120.3 (8)
C5—C4—H3118.8 (8)C21—C20—C19120.07 (9)
C4—C5—C6118.82 (9)C21—C20—H37120.2 (8)
C4—C5—H4120.6 (8)C19—C20—H37119.7 (8)
C6—C5—H4120.5 (8)C20—C21—C22119.94 (9)
C1—C6—C5119.09 (9)C20—C21—H38119.9 (8)
C1—C6—N1121.58 (9)C22—C21—H38120.2 (8)
C5—C6—N1119.28 (8)C23—C22—C21120.05 (10)
N1—C7—H5109.5 (8)C23—C22—H39120.2 (9)
N1—C7—H6109.4 (8)C21—C22—H39119.7 (9)
H5—C7—H6109.4 (11)C22—C23—C18120.03 (9)
N1—C7—H7109.5 (8)C22—C23—H40119.7 (8)
H5—C7—H7109.4 (11)C18—C23—H40120.2 (8)
H6—C7—H7109.5 (12)F1—P2—F490.30 (4)
N1—C8—H8109.5 (9)F1—P2—F391.00 (5)
N1—C8—H9109.4 (8)F4—P2—F390.78 (4)
H8—C8—H9109.5 (12)F1—P2—F689.77 (5)
N1—C8—H10109.4 (9)F4—P2—F690.40 (4)
H8—C8—H10109.5 (13)F3—P2—F6178.58 (3)
H9—C8—H10109.5 (12)F1—P2—F590.88 (4)
C10—C9—Pd168.66 (7)F4—P2—F5178.82 (4)
C10—C9—H11116.8 (9)F3—P2—F589.22 (4)
Pd1—C9—H11116.8 (9)F6—P2—F589.58 (4)
C10—C9—H12116.9 (8)F1—P2—F2178.59 (3)
Pd1—C9—H12116.9 (8)F4—P2—F290.16 (4)
H11—C9—H12113.7 (13)F3—P2—F290.32 (5)
C11—C10—C9127.67 (9)F6—P2—F288.90 (5)
C11—C10—Pd168.83 (6)F5—P2—F288.66 (4)
C9—C10—Pd175.54 (7)
(bihjux) Tetra-aqua-(14-methyl-2,5,8-trioxa-11,14,17-triaza-1$2!,9$2!-dihydroxy- -1,9(1,3)-dibenzenacyclo-octadecaphane-10,17-diene)-cerium(iii) trichloride monohydrate top
Crystal data top
C46H78Ce2Cl6N6O20γ = 90°
Mr = 1528.08V = 1670.7 (12) Å3
P21/mZ = 1
a = 10.983 (5) ÅF(000) = 774
b = 16.960 (6) ÅDx = 1.519 Mg m3
c = 9.058 (4) ÅMo Kα radiation, λ = 0.71073 Å
α = 90°µ = 1.65 mm1
β = 98.03 (7)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.014
Graphite monochromatorθmax = 43.2°, θmin = 1.9°
17852 measured reflectionsh = 1111
4588 independent reflectionsk = 1818
4555 reflections with I > 2σ(I)l = 1010
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)] = 0.065Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.163H atoms treated by a mixture of independent and constrained refinement
S = 1.17 w = 1/[σ2(Fo2) + (0.P)2 + 11.9541P]
where P = (Fo2 + 2Fc2)/3
4588 reflections(Δ/σ)max = 165.835
93 parametersΔρmax = 1.97 e Å3
0 restraintsΔρmin = 3.41 e Å3
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)
Ce10.15730 (3)0.25000.66210 (4)0.02000 (12)*
Cl10.16990 (15)0.25000.15380 (16)0.0200 (3)*
Cl20.42720 (14)0.89250 (9)0.31880 (15)0.0200 (3)*0.75
Cl30.3277 (4)0.4726 (3)0.5107 (5)0.0200 (7)*0.25
O10.2309 (3)0.3593 (2)0.8124 (4)0.0200 (6)*
O30.0247 (3)0.1139 (2)0.6306 (4)0.0200 (6)*
O40.0668 (5)0.25000.5286 (5)0.0200 (9)*
O60.3912 (5)0.25000.7006 (5)0.0200 (9)*
O70.0117 (5)0.25000.8672 (5)0.0200 (9)*
O80.2016 (3)0.1629 (2)0.4463 (4)0.0200 (6)*
O100.2437 (5)0.25000.7946 (5)0.0200 (9)*
N10.3911 (4)0.4032 (2)1.0422 (4)0.0200 (7)*
N20.5127 (5)0.25001.1447 (6)0.0200 (10)*
C10.0030 (4)0.5107 (3)0.7561 (5)0.0200 (8)*
C20.0441 (4)0.5651 (3)0.8644 (5)0.0200 (8)*
C30.1544 (4)0.5495 (3)0.9557 (5)0.0200 (8)*
C40.2174 (4)0.4797 (3)0.9388 (5)0.0200 (8)*
C50.1703 (5)0.4254 (3)0.8304 (5)0.0200 (8)*
C60.0601 (4)0.4409 (3)0.7391 (5)0.0200 (8)*
C70.3252 (4)0.4660 (3)1.0417 (5)0.0200 (8)*
C80.4964 (4)0.3916 (3)1.1504 (5)0.0200 (8)*
C90.5090 (4)0.3187 (3)1.2346 (5)0.0200 (8)*
C100.6113 (6)0.25001.0641 (7)0.0200 (11)*
C200.0967 (4)0.1128 (3)0.5570 (5)0.0200 (8)*
C210.1093 (4)0.1780 (3)0.4492 (5)0.0200 (8)*
Geometric parameters (Å, º) top
Ce1—O12.374 (4)N1—C81.421 (6)
Ce1—O1i2.374 (4)N2—C101.388 (9)
Ce1—O62.544 (5)N2—C91.425 (6)
Ce1—O8i2.551 (4)N2—C9i1.425 (6)
Ce1—O82.551 (4)C1—C61.391 (7)
Ce1—O42.586 (5)C1—C21.393 (6)
Ce1—O72.615 (5)C2—C31.393 (7)
Ce1—O32.723 (4)C3—C41.390 (7)
Ce1—O3i2.723 (4)C4—C51.392 (7)
O1—C51.325 (6)C4—C71.420 (7)
O3—C6i1.369 (6)C5—C61.392 (7)
O3—C201.405 (6)C6—O3i1.369 (6)
O4—C211.460 (5)C8—C91.449 (7)
O4—C21i1.460 (5)C20—C211.469 (7)
N1—C71.287 (6)
O1—Ce1—O1i102.68 (17)O8—Ce1—O3i124.55 (11)
O1—Ce1—O670.42 (11)O4—Ce1—O3i59.39 (8)
O1i—Ce1—O670.42 (11)O7—Ce1—O3i72.74 (9)
O1—Ce1—O8i84.33 (12)O3—Ce1—O3i115.93 (15)
O1i—Ce1—O8i143.67 (12)C5—O1—Ce1126.5 (3)
O6—Ce1—O8i78.93 (13)C6i—O3—C20119.2 (4)
O1—Ce1—O8143.67 (12)C6i—O3—Ce1114.0 (3)
O1i—Ce1—O884.33 (12)C20—O3—Ce1121.3 (3)
O6—Ce1—O878.93 (13)C21—O4—C21i113.5 (5)
O8i—Ce1—O870.78 (16)C21—O4—Ce1116.6 (3)
O1—Ce1—O4119.58 (10)C21i—O4—Ce1116.6 (3)
O1i—Ce1—O4119.58 (10)C7—N1—C8121.3 (4)
O6—Ce1—O4160.22 (16)C10—N2—C9112.8 (4)
O8i—Ce1—O484.99 (13)C10—N2—C9i112.8 (4)
O8—Ce1—O484.99 (13)C9—N2—C9i109.7 (5)
O1—Ce1—O777.62 (11)C6—C1—C2120.0 (4)
O1i—Ce1—O777.62 (11)C1—C2—C3119.9 (4)
O6—Ce1—O7127.49 (16)C4—C3—C2120.1 (4)
O8i—Ce1—O7138.20 (10)C3—C4—C5120.0 (4)
O8—Ce1—O7138.20 (10)C3—C4—C7116.7 (4)
O4—Ce1—O772.28 (16)C5—C4—C7123.3 (5)
O1—Ce1—O3148.91 (11)O1—C5—C4120.2 (4)
O1i—Ce1—O362.12 (12)O1—C5—C6119.8 (4)
O6—Ce1—O3121.97 (8)C4—C5—C6120.0 (4)
O8i—Ce1—O3124.55 (11)O3i—C6—C1124.1 (4)
O8—Ce1—O365.49 (11)O3i—C6—C5115.7 (4)
O4—Ce1—O359.39 (8)C1—C6—C5120.0 (4)
O7—Ce1—O372.74 (9)N1—C7—C4123.7 (4)
O1—Ce1—O3i62.12 (12)N1—C8—C9119.3 (4)
O1i—Ce1—O3i148.91 (11)N2—C9—C8113.9 (4)
O6—Ce1—O3i121.97 (8)O3—C20—C21107.5 (4)
O8i—Ce1—O3i65.49 (11)O4—C21—C20107.9 (4)
Symmetry code: (i) x, y+1/2, z.
(bihlin) Tetra-aqua-(14-methyl-2,5,8-trioxa-11,14,17-triaza-1$2!,9$2!-dihydroxy- -1,9(1,3)-dibenzenacyclo-octadecaphane-10,17-diene)-dysprosium(iii) trichloride monohydrate top
Crystal data top
C46H78Cl6Dy2N6O20γ = 90°
Mr = 1572.84V = 1634.8 (12) Å3
P21/mZ = 1
a = 10.870 (5) ÅF(000) = 790
b = 16.785 (6) ÅDx = 1.598 Mg m3
c = 9.046 (4) ÅMo Kα radiation, λ = 0.71073 Å
α = 90°µ = 2.58 mm1
β = 97.91 (8)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.018
Graphite monochromatorθmax = 43.5°, θmin = 1.9°
17852 measured reflectionsh = 1111
4588 independent reflectionsk = 1818
4539 reflections with I > 2σ(I)l = 1010
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)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129H atoms treated by a mixture of independent and constrained refinement
S = 1.20 w = 1/[σ2(Fo2) + (0.P)2 + 5.4182P]
where P = (Fo2 + 2Fc2)/3
4588 reflections(Δ/σ)max = 61.082
93 parametersΔρmax = 2.33 e Å3
0 restraintsΔρmin = 2.63 e Å3
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)
Dy10.15690 (2)0.25000.66630 (3)0.02000 (9)*
Cl10.16210 (12)0.25000.16360 (14)0.0200 (3)*
Cl20.42750 (12)0.89130 (8)0.31740 (14)0.0200 (2)*0.75
Cl30.3243 (4)0.4745 (2)0.5197 (4)0.0200 (6)*0.25
O10.2307 (3)0.35530 (18)0.8130 (3)0.0200 (5)*
O30.0256 (3)0.11750 (18)0.6345 (3)0.0200 (5)*
O40.0559 (4)0.25000.5190 (5)0.0200 (8)*
O60.3815 (4)0.25000.6989 (5)0.0200 (8)*
O70.0173 (4)0.25000.8499 (5)0.0200 (8)*
O80.2001 (3)0.16530 (19)0.4627 (3)0.0200 (5)*
O100.2365 (4)0.25000.7849 (5)0.0200 (8)*
N10.3949 (3)0.4000 (2)1.0434 (4)0.0200 (6)*
N20.5169 (5)0.25001.1572 (6)0.0200 (9)*
C10.0028 (4)0.5095 (2)0.7595 (4)0.0200 (7)*
C20.0446 (4)0.5635 (2)0.8698 (4)0.0200 (7)*
C30.1553 (4)0.5470 (3)0.9617 (4)0.0200 (7)*
C40.2189 (4)0.4765 (3)0.9433 (4)0.0200 (7)*
C50.1716 (4)0.4225 (3)0.8329 (4)0.0200 (7)*
C60.0608 (4)0.4390 (3)0.7414 (4)0.0200 (7)*
C70.3266 (4)0.4629 (2)1.0433 (5)0.0200 (7)*
C80.5143 (4)0.3905 (3)1.1475 (4)0.0200 (7)*
C90.5143 (4)0.3217 (2)1.2395 (5)0.0200 (7)*
C100.6269 (6)0.25001.0768 (6)0.0200 (10)*
C200.0944 (4)0.1143 (3)0.5526 (4)0.0200 (7)*
C210.1028 (4)0.1787 (2)0.4404 (5)0.0200 (7)*
Geometric parameters (Å, º) top
Dy1—O12.288 (3)N1—C81.503 (5)
Dy1—O1i2.288 (3)N2—C91.417 (5)
Dy1—O72.399 (5)N2—C9i1.417 (5)
Dy1—O62.419 (5)N2—C101.483 (8)
Dy1—O82.423 (3)C1—C61.391 (6)
Dy1—O8i2.423 (3)C1—C21.393 (6)
Dy1—O42.506 (5)C2—C31.393 (6)
Dy1—O32.637 (3)C3—C41.392 (6)
Dy1—O3i2.637 (3)C4—C51.394 (6)
O1—C51.323 (5)C4—C71.396 (6)
O3—C6i1.371 (5)C5—C61.392 (6)
O3—C201.410 (5)C6—O3i1.371 (5)
O4—C211.448 (5)C8—C91.423 (6)
O4—C21i1.448 (5)C20—C211.477 (6)
N1—C71.291 (5)
O1—Dy1—O1i101.15 (16)O8—Dy1—O3i124.79 (10)
O1—Dy1—O778.65 (10)O8i—Dy1—O3i65.22 (11)
O1i—Dy1—O778.65 (10)O4—Dy1—O3i59.72 (7)
O1—Dy1—O670.23 (11)O3—Dy1—O3i115.01 (14)
O1i—Dy1—O670.23 (11)C5—O1—Dy1126.8 (3)
O7—Dy1—O6129.77 (15)C6i—O3—C20119.5 (3)
O1—Dy1—O8143.60 (11)C6i—O3—Dy1114.3 (2)
O1i—Dy1—O884.17 (11)C20—O3—Dy1122.5 (2)
O7—Dy1—O8137.17 (9)C21—O4—C21i111.4 (4)
O6—Dy1—O878.15 (12)C21—O4—Dy1119.9 (2)
O1—Dy1—O8i84.17 (11)C21i—O4—Dy1119.9 (2)
O1i—Dy1—O8i143.60 (11)C7—N1—C8122.3 (4)
O7—Dy1—O8i137.17 (9)C9—N2—C9i116.2 (5)
O6—Dy1—O8i78.15 (12)C9—N2—C10109.5 (3)
O8—Dy1—O8i71.85 (15)C9i—N2—C10109.5 (3)
O1—Dy1—O4122.19 (9)C6—C1—C2119.8 (4)
O1i—Dy1—O4122.19 (9)C3—C2—C1120.1 (4)
O7—Dy1—O475.08 (15)C4—C3—C2120.0 (4)
O6—Dy1—O4155.15 (14)C3—C4—C5119.9 (4)
O8—Dy1—O481.78 (12)C3—C4—C7116.6 (4)
O8i—Dy1—O481.78 (12)C5—C4—C7123.5 (4)
O1—Dy1—O3148.88 (10)O1—C5—C6119.0 (4)
O1i—Dy1—O363.45 (11)O1—C5—C4120.9 (4)
O7—Dy1—O372.01 (9)C6—C5—C4120.0 (4)
O6—Dy1—O3122.37 (7)O3i—C6—C1125.2 (4)
O8—Dy1—O365.22 (11)O3i—C6—C5114.6 (4)
O8i—Dy1—O3124.79 (10)C1—C6—C5120.2 (4)
O4—Dy1—O359.72 (7)N1—C7—C4124.4 (4)
O1—Dy1—O3i63.45 (11)C9—C8—N1112.5 (4)
O1i—Dy1—O3i148.88 (10)N2—C9—C8112.3 (4)
O7—Dy1—O3i72.01 (8)O3—C20—C21107.4 (3)
O6—Dy1—O3i122.37 (7)O4—C21—C20106.4 (3)
Symmetry code: (i) x, y+1/2, z.
(zexbuz01) Chloro-tris(2,2,6,6-tetramethyl-3,5-heptanedionato)-zirconium(iv) top
Crystal data top
C33H57ClO6Zrγ = 90°
Mr = 676.46V = 1895.2 (14) Å3
P21/mZ = 2
a = 10.679 (5) ÅF(000) = 720
b = 18.263 (7) ÅDx = 1.185 Mg m3
c = 10.973 (5) ÅMo Kα radiation, λ = 0.71073 Å
α = 90°µ = 0.40 mm1
β = 117.68 (5)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.006
Graphite monochromatorθmax = 52.2°, θmin = 2.1°
20610 measured reflectionsh = 1111
5289 independent reflectionsk = 1919
5255 reflections with I > 2σ(I)l = 1111
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)] = 0.221Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.395H atoms treated by a mixture of independent and constrained refinement
S = 0.74 w = 1/[σ2(Fo2) + (0.P)2 + 181.8093P]
where P = (Fo2 + 2Fc2)/3
5289 reflections(Δ/σ)max = 90.043
96 parametersΔρmax = 4.04 e Å3
0 restraintsΔρmin = 7.23 e Å3
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
Zr10.84820 (13)0.25000.37470 (13)0.0200 (3)*
Cl10.7498 (3)0.25000.1192 (3)0.0200 (6)*
O11.0691 (10)0.25000.5131 (9)0.0200 (17)*
O20.8539 (10)0.25000.5706 (9)0.0200 (17)*
O30.6790 (7)0.3235 (4)0.3429 (6)0.0200 (13)*
O40.9232 (7)0.3537 (4)0.3519 (6)0.0200 (12)*
C11.3069 (13)0.25000.6871 (13)0.020 (2)*
C21.3724 (9)0.1878 (5)0.7679 (9)0.0200 (16)*
C31.3349 (13)0.25000.5742 (13)0.020 (2)*
C51.1497 (13)0.25000.6406 (13)0.020 (2)*
C61.0969 (13)0.25000.7373 (13)0.020 (2)*
H11.17110.25000.84510.02 (4)*
C70.9524 (13)0.25000.6988 (13)0.020 (2)*
C80.8934 (13)0.25000.8012 (13)0.020 (2)*
C90.7997 (9)0.1813 (5)0.7744 (9)0.0200 (17)*
C101.0141 (13)0.25000.9509 (13)0.020 (2)*
C120.4996 (9)0.4111 (5)0.2713 (9)0.0200 (16)*
C130.4647 (9)0.4923 (5)0.2310 (9)0.0200 (16)*
C140.4822 (9)0.3934 (5)0.3975 (9)0.0200 (16)*
C150.3901 (9)0.3649 (5)0.1510 (9)0.0200 (16)*
C160.6440 (9)0.3873 (5)0.2952 (9)0.0200 (16)*
C170.7292 (9)0.4318 (5)0.2643 (9)0.0200 (16)*
H20.68610.48300.21400.02 (3)*
C180.8678 (9)0.4150 (5)0.2938 (9)0.0200 (16)*
C190.9565 (9)0.4637 (5)0.2537 (9)0.0200 (16)*
C200.9740 (9)0.4238 (5)0.1428 (9)0.0200 (16)*
C210.9017 (9)0.5386 (5)0.2176 (9)0.0200 (16)*
C221.1040 (9)0.4692 (5)0.3801 (9)0.0200 (16)*
Geometric parameters (Å, º) top
Zr1—O42.116 (7)C6—H11.0753
Zr1—O4i2.116 (7)C7—C81.52 (2)
Zr1—O22.122 (10)C8—C9i1.545 (12)
Zr1—O12.131 (9)C8—C91.545 (12)
Zr1—O32.145 (7)C8—C101.547 (17)
Zr1—O3i2.145 (7)C12—C161.503 (13)
Zr1—Cl12.495 (4)C12—C141.515 (13)
O1—C51.257 (15)C12—C131.543 (13)
O2—C71.308 (15)C12—C151.545 (12)
O3—C161.261 (12)C16—C171.375 (14)
O4—C181.288 (11)C17—C181.394 (13)
C1—C31.40 (2)C17—H21.0746
C1—C2i1.411 (12)C18—C191.506 (14)
C1—C21.411 (12)C19—C211.468 (13)
C1—C51.511 (18)C19—C201.503 (13)
C5—C61.41 (2)C19—C221.544 (12)
C6—C71.398 (18)
O4—Zr1—O4i127.0 (4)C7—C6—C5122.8 (12)
O4—Zr1—O2106.6 (2)C7—C6—H1118.6
O4i—Zr1—O2106.6 (2)C5—C6—H1118.6
O4—Zr1—O174.3 (2)O2—C7—C6123.3 (13)
O4i—Zr1—O174.3 (2)O2—C7—C8113.1 (11)
O2—Zr1—O177.1 (4)C6—C7—C8123.7 (11)
O4—Zr1—O375.9 (3)C7—C8—C9i108.2 (7)
O4i—Zr1—O3151.3 (3)C7—C8—C9108.2 (7)
O2—Zr1—O377.9 (3)C9i—C8—C9108.5 (10)
O1—Zr1—O3133.3 (2)C7—C8—C10110.9 (11)
O4—Zr1—O3i151.3 (3)C9i—C8—C10110.4 (7)
O4i—Zr1—O3i75.9 (3)C9—C8—C10110.4 (7)
O2—Zr1—O3i77.9 (3)C16—C12—C14109.3 (7)
O1—Zr1—O3i133.3 (2)C16—C12—C13114.8 (8)
O3—Zr1—O3i77.5 (4)C14—C12—C13110.6 (8)
O4—Zr1—Cl181.50 (18)C16—C12—C15107.4 (8)
O4i—Zr1—Cl181.50 (18)C14—C12—C15107.4 (8)
O2—Zr1—Cl1159.6 (3)C13—C12—C15107.1 (7)
O1—Zr1—Cl1123.3 (3)O3—C16—C17123.1 (9)
O3—Zr1—Cl186.21 (19)O3—C16—C12115.0 (9)
O3i—Zr1—Cl186.21 (19)C17—C16—C12121.9 (9)
C5—O1—Zr1138.8 (9)C16—C17—C18124.4 (9)
C7—O2—Zr1136.0 (9)C16—C17—H2117.8
C16—O3—Zr1135.3 (7)C18—C17—H2117.8
C18—O4—Zr1136.4 (6)O4—C18—C17120.0 (9)
C3—C1—C2i107.9 (8)O4—C18—C19116.8 (8)
C3—C1—C2107.9 (8)C17—C18—C19123.1 (8)
C2i—C1—C2107.3 (11)C21—C19—C20114.7 (8)
C3—C1—C5111.2 (11)C21—C19—C18113.8 (8)
C2i—C1—C5111.2 (8)C20—C19—C18106.4 (8)
C2—C1—C5111.2 (8)C21—C19—C22107.1 (8)
O1—C5—C6122.0 (12)C20—C19—C22107.5 (8)
O1—C5—C1117.1 (12)C18—C19—C22107.1 (7)
C6—C5—C1121.0 (11)
Symmetry code: (i) x, y+1/2, z.
(pyrhsb) Pyridinium hexachloro-antimony(v) top
Crystal data top
C5H6N+·Cl6Sbγ = 90°
Mr = 414.56V = 1286 (4) Å3
P21/aZ = 4
a = 15.42 (3) ÅF(000) = 784
b = 11.66 (2) ÅDx = 2.142 Mg m3
c = 7.21 (1) ÅMo Kα radiation, λ = 0.71073 Å
α = 90°µ = 3.35 mm1
β = 97.31 (4)°T = 293 K
Data collection top
Radiation source: fine-focus sealed tubeRint = 0.007
Graphite monochromatorθmax = 42.0°, θmin = 2.2°
12890 measured reflectionsh = 1515
3289 independent reflectionsk = 1212
3277 reflections with I > 2σ(I)l = 88
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)] = 0.061Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.167H atoms treated by a mixture of independent and constrained refinement
S = 1.35 w = 1/[σ2(Fo2) + (0.P)2 + 16.8959P]
where P = (Fo2 + 2Fc2)/3
3289 reflections(Δ/σ)max = 2.226
77 parametersΔρmax = 2.17 e Å3
0 restraintsΔρmin = 3.22 e Å3
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)
Sb10.33750 (4)0.32820 (4)0.25310 (7)0.02000 (15)*
Cl10.36500 (13)0.45900 (16)0.0180 (2)0.0200 (3)*
Cl50.31000 (13)0.19500 (16)0.4840 (2)0.0200 (3)*
Cl60.30550 (13)0.18600 (16)0.0295 (2)0.0200 (3)*
Cl70.36850 (13)0.46850 (16)0.4825 (2)0.0200 (3)*
Cl80.18950 (13)0.38400 (16)0.2155 (2)0.0200 (3)*
Cl90.48400 (13)0.27150 (16)0.2860 (2)0.0200 (3)*
N10.4420 (12)0.7237 (12)0.2380 (18)0.020 (3)*0.50
C30.5080 (12)0.7877 (16)0.194 (2)0.020 (3)*0.50
C40.5070 (11)0.9037 (14)0.240 (2)0.020 (3)*0.50
C50.4200 (13)0.9527 (14)0.277 (2)0.020 (3)*0.50
C60.3600 (11)0.8747 (18)0.318 (2)0.020 (3)*0.50
C70.3680 (13)0.7717 (17)0.290 (2)0.020 (3)*0.50
N2'0.3950 (12)0.7233 (12)0.2510 (18)0.020 (3)*0.50
C10'0.4760 (14)0.7573 (16)0.201 (2)0.020 (3)*0.50
C9'0.4980 (11)0.8623 (15)0.168 (2)0.020 (3)*0.50
C8'0.4510 (13)0.9483 (14)0.239 (2)0.020 (3)*0.50
C2'0.3640 (11)0.9243 (17)0.296 (2)0.020 (3)*0.50
C1'0.3420 (13)0.8053 (17)0.292 (2)0.020 (3)*0.50
Geometric parameters (Å, º) top
Sb1—Cl62.321 (3)C5—C8'0.58 (2)
Sb1—Cl72.332 (3)C5—C2'0.95 (2)
Sb1—Cl92.337 (5)C5—C61.36 (3)
Sb1—Cl52.354 (3)C5—C9'1.85 (3)
Sb1—Cl82.355 (5)C6—C2'0.605 (19)
Sb1—Cl12.358 (3)C6—C1'0.87 (2)
N1—C10'0.73 (2)C6—C71.23 (3)
N1—N2'0.743 (17)C6—C8'1.80 (3)
N1—C31.33 (2)C6—N2'1.93 (2)
N1—C71.37 (3)C7—C1'0.56 (2)
N1—C1'1.89 (2)C7—N2'0.78 (2)
N1—C9'1.93 (2)C7—C2'1.78 (3)
C3—C10'0.61 (2)C7—C10'1.87 (3)
C3—C9'0.90 (2)N2'—C1'1.32 (2)
C3—C41.39 (2)N2'—C10'1.40 (3)
C4—C9'0.710 (19)C10'—C9'1.30 (3)
C4—C8'1.01 (2)C9'—C8'1.37 (2)
C4—C51.51 (3)C8'—C2'1.48 (3)
C4—C10'1.79 (3)C2'—C1'1.43 (3)
Cl6—Sb1—Cl7178.76 (7)N2'—C7—C2'139 (2)
Cl6—Sb1—Cl989.18 (9)C6—C7—C2'9.4 (10)
Cl7—Sb1—Cl991.04 (9)N1—C7—C2'116.7 (15)
Cl6—Sb1—Cl588.76 (14)C1'—C7—C10'138 (4)
Cl7—Sb1—Cl590.02 (14)N2'—C7—C10'42.8 (18)
Cl9—Sb1—Cl590.02 (9)C6—C7—C10'104.9 (16)
Cl6—Sb1—Cl890.01 (9)N1—C7—C10'19.2 (8)
Cl7—Sb1—Cl889.77 (9)C2'—C7—C10'97.7 (12)
Cl9—Sb1—Cl8179.14 (7)N1—N2'—C7128 (3)
Cl5—Sb1—Cl890.26 (9)N1—N2'—C1'132 (2)
Cl6—Sb1—Cl190.26 (14)C7—N2'—C1'8.7 (15)
Cl7—Sb1—Cl190.96 (14)N1—N2'—C10'18.0 (15)
Cl9—Sb1—Cl189.77 (9)C7—N2'—C10'115 (2)
Cl5—Sb1—Cl1179.00 (7)C1'—N2'—C10'116.9 (15)
Cl8—Sb1—Cl189.93 (9)N1—N2'—C6109.6 (18)
C10'—N1—N2'144 (3)C7—N2'—C620.1 (18)
C10'—N1—C37.5 (16)C1'—N2'—C622.4 (10)
N2'—N1—C3145 (2)C10'—N2'—C695.3 (11)
C10'—N1—C7123 (2)C3—C10'—N1163 (3)
N2'—N1—C726.5 (15)C3—C10'—C9'38 (2)
C3—N1—C7121.7 (15)N1—C10'—C9'142 (3)
C10'—N1—C1'116 (2)C3—C10'—N2'159 (3)
N2'—N1—C1'31.1 (14)N1—C10'—N2'18.3 (16)
C3—N1—C1'115.7 (13)C9'—C10'—N2'125.1 (17)
C7—N1—C1'6.8 (11)C3—C10'—C442 (2)
C10'—N1—C9'24.6 (18)N1—C10'—C4130 (2)
N2'—N1—C9'121.0 (18)C9'—C10'—C419.6 (9)
C3—N1—C9'24.2 (9)N2'—C10'—C4117.4 (14)
C7—N1—C9'98.4 (12)C3—C10'—C7137 (3)
C1'—N1—C9'92.1 (10)N1—C10'—C737.9 (18)
C10'—C3—C9'117 (4)C9'—C10'—C7104.1 (15)
C10'—C3—N19.0 (18)N2'—C10'—C722.1 (8)
C9'—C3—N1118 (2)C4—C10'—C795.3 (12)
C10'—C3—C4120 (3)C4—C9'—C3120 (3)
C9'—C3—C426.3 (12)C4—C9'—C10'123 (2)
N1—C3—C4117.1 (15)C3—C9'—C10'24.9 (14)
C9'—C4—C8'105 (2)C4—C9'—C8'45.1 (18)
C9'—C4—C334.1 (17)C3—C9'—C8'135 (2)
C8'—C4—C3122.3 (19)C10'—C9'—C8'117.2 (16)
C9'—C4—C5107 (2)C4—C9'—C551.6 (19)
C8'—C4—C513.5 (12)C3—C9'—C5124.5 (18)
C3—C4—C5116.5 (15)C10'—C9'—C5105.1 (14)
C9'—C4—C10'37.9 (18)C8'—C9'—C512.2 (9)
C8'—C4—C10'106.3 (17)C4—C9'—N1116 (2)
C3—C4—C10'17.3 (9)C3—C9'—N137.4 (14)
C5—C4—C10'99.4 (13)C10'—C9'—N113.5 (10)
C8'—C5—C2'148 (3)C8'—C9'—N1103.8 (13)
C8'—C5—C6132 (3)C5—C9'—N191.7 (10)
C2'—C5—C622.8 (13)C5—C8'—C4143 (3)
C8'—C5—C424 (2)C5—C8'—C9'138 (3)
C2'—C5—C4137 (2)C4—C8'—C9'29.9 (12)
C6—C5—C4115.5 (15)C5—C8'—C2'20 (2)
C8'—C5—C9'30 (2)C4—C8'—C2'135.0 (19)
C2'—C5—C9'121.0 (18)C9'—C8'—C2'120.4 (16)
C6—C5—C9'102.1 (13)C5—C8'—C634 (2)
C4—C5—C9'21.6 (7)C4—C8'—C6117.0 (17)
C2'—C6—C1'151 (3)C9'—C8'—C6103.9 (13)
C2'—C6—C7151 (3)C2'—C8'—C618.1 (8)
C1'—C6—C724.2 (16)C6—C2'—C5120 (3)
C2'—C6—C538 (2)C6—C2'—C1'17.1 (19)
C1'—C6—C5142 (2)C5—C2'—C1'124 (2)
C7—C6—C5122.3 (18)C6—C2'—C8'112 (3)
C2'—C6—C8'50 (2)C5—C2'—C8'11.9 (13)
C1'—C6—C8'128 (2)C1'—C2'—C8'113.6 (16)
C7—C6—C8'108.4 (15)C6—C2'—C719 (2)
C5—C6—C8'14.0 (9)C5—C2'—C7108.0 (18)
C2'—C6—N2'140 (3)C1'—C2'—C715.8 (10)
C1'—C6—N2'35.3 (16)C8'—C2'—C798.4 (13)
C7—C6—N2'12.5 (11)C7—C1'—C6116 (4)
C5—C6—N2'109.8 (14)C7—C1'—N2'12 (2)
C8'—C6—N2'95.9 (11)C6—C1'—N2'122 (2)
C1'—C7—N2'159 (4)C7—C1'—C2'121 (4)
C1'—C7—C639 (3)C6—C1'—C2'11.8 (13)
N2'—C7—C6147 (3)N2'—C1'—C2'123.9 (17)
C1'—C7—N1156 (4)C7—C1'—N117 (3)
N2'—C7—N125.3 (15)C6—C1'—N1105 (2)
C6—C7—N1123.5 (19)N2'—C1'—N117.0 (8)
C1'—C7—C2'44 (3)C2'—C1'—N1107.1 (14)
 

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