22 Space-group changes

Clemente, D.A.; Marzotto, A.

doi:10.1107/S0108768102022668

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22 Space-group changes

D. A. Clemente and A. Marzotto

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.

Keywords: space-group changes.

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Supporting information

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

C₁₅H₁₆CoN₄O₈	γ = 90°
M_r = 439.25	V = 1810.3 (6) Å³
C222₁	Z = 4
a = 7.625 (2) Å	F(000) = 900
b = 19.808 (2) Å	D_x = 1.612 Mg m⁻³
c = 11.986 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 1.00 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.046
Graphite monochromator	θ_max = 46.0°, θ_min = 2.1°
8912 measured reflections	h = −8→8
2688 independent reflections	k = −28→28
2560 reflections with I > 2σ(I)	l = −12→12

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.018	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.109	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.58	(Δ/σ)_max = 4.200
2688 reflections	Δρ_max = 0.52 e Å⁻³
105 parameters	Δρ_min = −0.22 e Å⁻³
0 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute 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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Co1	0.0000	0.022600 (15)	0.2500	0.02000 (9)*
O2	0.01940 (18)	0.25290 (6)	0.15650 (11)	0.0200 (2)*
O3	−0.17430 (17)	−0.02200 (7)	0.14290 (11)	0.0200 (2)*
O4	−0.14130 (17)	−0.10820 (6)	0.03250 (12)	0.0200 (2)*
O5	0.08120 (19)	−0.06770 (7)	0.12090 (12)	0.0200 (2)*
N1	0.18870 (19)	0.08220 (7)	0.17230 (14)	0.0200 (2)*
N4	−0.0758 (2)	−0.06610 (8)	0.09780 (14)	0.0200 (3)*
C1	0.3360 (2)	0.04790 (9)	0.14270 (15)	0.0200 (3)*
H1	0.343 (4)	0.0021 (15)	0.159 (3)	0.020 (6)*
C2	0.4745 (2)	0.07900 (8)	0.08950 (16)	0.0200 (2)*
H2	0.574 (4)	0.0544 (13)	0.071 (2)	0.020 (6)*
C3	0.4643 (2)	0.14570 (9)	0.06430 (16)	0.0200 (3)*
H3	0.555 (4)	0.1672 (12)	0.027 (3)	0.020 (6)*
C4	0.3159 (2)	0.18090 (8)	0.09570 (16)	0.0200 (3)*
H4	0.307 (4)	0.2269 (13)	0.081 (3)	0.020 (6)*
C5	0.1802 (2)	0.14760 (9)	0.14880 (15)	0.0200 (3)*
C6	0.0106 (2)	0.18400 (8)	0.18520 (13)	0.0200 (3)*
H18	−0.083 (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
C15	0.0000	0.35750 (11)	0.2500	0.0200 (4)*
H9	−0.033 (9)	0.377 (3)	0.321 (6)	0.020 (12)*	0.50
H10	−0.052 (9)	0.384 (3)	0.192 (6)	0.020 (13)*	0.50
H11	0.124 (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—O3	2.0481 (14)	C1—C2	1.379 (2)
Co1—O3ⁱ	2.0481 (14)	C2—C3	1.358 (2)
Co1—N1ⁱ	2.0812 (15)	C3—C4	1.381 (2)
Co1—N1	2.0812 (15)	C4—C5	1.382 (3)
O2—C6	1.409 (2)	C5—C6	1.544 (2)
O2—C14?ⁱ	1.422 (4)	C6—C6ⁱ	1.562 (3)
O2—C14?	1.455 (5)	C14?—C14?ⁱ	0.963 (8)
O3—N4	1.273 (2)	C14?—C15	1.408 (4)
O4—N4	1.248 (2)	C14?—O2ⁱ	1.422 (4)
O5—N4	1.229 (2)	C14?—C17?	1.549 (5)
N1—C5	1.327 (2)	C15—C14?ⁱ	1.408 (4)
N1—C1	1.360 (2)

O3—Co1—O3ⁱ	128.89 (8)	C3—C4—C5	119.85 (15)
O3—Co1—N1ⁱ	94.39 (6)	N1—C5—C4	121.80 (16)
O3ⁱ—Co1—N1ⁱ	114.38 (6)	N1—C5—C6	115.90 (14)
O3—Co1—N1	114.38 (6)	C4—C5—C6	122.30 (15)
O3ⁱ—Co1—N1	94.39 (6)	O2—C6—C5	110.09 (14)
N1ⁱ—Co1—N1	110.88 (8)	O2—C6—C6ⁱ	104.34 (8)
C6—O2—C14?ⁱ	108.13 (18)	C5—C6—C6ⁱ	111.58 (17)
C6—O2—C14?	107.87 (18)	C14?ⁱ—C14?—C15	70.00 (16)
C14?ⁱ—O2—C14?	39.1 (3)	C14?ⁱ—C14?—O2ⁱ	72.3 (4)
N4—O3—Co1	100.33 (11)	C15—C14?—O2ⁱ	113.0 (3)
C5—N1—C1	118.20 (15)	C14?ⁱ—C14?—O2	68.6 (4)
C5—N1—Co1	127.94 (12)	C15—C14?—O2	111.0 (3)
C1—N1—Co1	113.85 (11)	O2ⁱ—C14?—O2	103.6 (2)
O5—N4—O4	120.92 (17)	C14?ⁱ—C14?—C17?	176.3 (3)
O5—N4—O3	119.79 (17)	C15—C14?—C17?	106.5 (2)
O4—N4—O3	119.27 (15)	O2ⁱ—C14?—C17?	108.7 (3)
N1—C1—C2	122.01 (16)	O2—C14?—C17?	114.2 (3)
C3—C2—C1	119.59 (16)	C14?ⁱ—C15—C14?	40.0 (3)
C2—C3—C4	118.53 (16)

Symmetry code: (i) −x, y, −z+1/2.

(claecu) bis(Chloroacetato)-(N,N,N',N'-tetramethylethylenediamine) copper(ii) top

Crystal data top

C₁₀H₂₀Cl₂CuN₂O₄	γ = 90°
M_r = 366.72	V = 1523.5 (11) Å³
C222₁	Z = 4
a = 9.002 (3) Å	F(000) = 756
b = 11.400 (5) Å	D_x = 1.599 Mg m⁻³
c = 14.846 (7) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 1.79 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.006
Graphite monochromator	θ_max = 45.6°, θ_min = 2.7°
8366 measured reflections	h = −16→16
2103 independent reflections	k = −16→16
2095 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.006	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.042	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.25	(Δ/σ)_max = 1.279
2103 reflections	Δρ_max = 0.10 e Å⁻³
79 parameters	Δρ_min = −0.16 e Å⁻³
0 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.003 (5)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cu1	0.00000	0.103000 (12)	0.25000	0.02000 (4)*
N1	−0.14260 (7)	−0.02670 (6)	0.21200 (5)	0.02000 (11)*
C1	−0.08360 (8)	−0.13590 (7)	0.25390 (7)	0.02000 (12)*
H1	−0.1257 (15)	−0.2107 (12)	0.2215 (9)	0.020 (3)*
H2	−0.1210 (14)	−0.1400 (12)	0.3165 (10)	0.020 (3)*
C3	−0.15370 (7)	−0.04170 (8)	0.11320 (6)	0.02000 (13)*
H5	−0.1915 (15)	0.0310 (11)	0.0870 (8)	0.020 (3)*
H6	−0.2118 (13)	−0.1108 (11)	0.1010 (9)	0.020 (3)*
H7	−0.0608 (14)	−0.0527 (11)	0.0830 (9)	0.020 (3)*
C4	−0.29120 (8)	0.00080 (7)	0.24880 (6)	0.02000 (13)*
H8	−0.3248 (14)	0.0767 (12)	0.2150 (8)	0.020 (3)*
H9	−0.3630 (14)	−0.0630 (12)	0.2350 (9)	0.020 (3)*
H10	−0.2898 (13)	0.0178 (11)	0.3085 (9)	0.020 (3)*
O1	−0.10440 (6)	0.22160 (5)	0.17640 (4)	0.02000 (10)*
C7	−0.02140 (7)	0.23430 (7)	0.10700 (6)	0.02000 (12)*
C8	−0.08500 (8)	0.32340 (8)	0.04060 (6)	0.02000 (12)*
H17	−0.1833 (13)	0.3037 (12)	0.0180 (8)	0.020 (3)*
H18	−0.0920 (12)	0.3990 (13)	0.0710 (8)	0.020 (3)*
Cl1	0.025500 (18)	0.341600 (17)	−0.057800 (12)	0.02000 (4)*
O2	0.09550 (6)	0.18120 (6)	0.09410 (4)	0.02000 (11)*

Geometric parameters (Å, º) top

Cu1—O1ⁱ	1.9761 (8)	N1—C1	1.4895 (12)
Cu1—O1	1.9762 (8)	C1—C1ⁱ	1.5096 (15)
Cu1—N1	2.0377 (9)	O1—C7	1.2809 (10)
Cu1—N1ⁱ	2.0377 (9)	C7—O2	1.2290 (9)
N1—C4	1.4786 (11)	C7—C8	1.5268 (12)
N1—C3	1.4801 (14)	C8—Cl1	1.7795 (11)

O1ⁱ—Cu1—O1	93.66 (5)	C4—N1—Cu1	108.29 (6)
O1ⁱ—Cu1—N1	161.64 (3)	C3—N1—Cu1	113.62 (5)
O1—Cu1—N1	92.51 (4)	C1—N1—Cu1	105.44 (6)
O1ⁱ—Cu1—N1ⁱ	92.51 (4)	N1—C1—C1ⁱ	108.87 (6)
O1—Cu1—N1ⁱ	161.64 (3)	C7—O1—Cu1	104.16 (5)
N1—Cu1—N1ⁱ	86.96 (5)	O2—C7—O1	124.69 (8)
C4—N1—C3	109.24 (6)	O2—C7—C8	123.24 (8)
C4—N1—C1	110.21 (7)	O1—C7—C8	112.07 (6)
C3—N1—C1	109.96 (7)	C7—C8—Cl1	113.45 (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

C₁₆Cl₃CoN₄O₄	γ = 90°
M_r = 477.48	V = 2188.1 (6) Å³
C222₁	Z = 4
a = 10.621 (2) Å	F(000) = 936
b = 11.624 (2) Å	D_x = 1.449 Mg m⁻³
c = 17.723 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 1.18 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.015
Graphite monochromator	θ_max = 38.6°, θ_min = 2.3°
9520 measured reflections	h = −16→16
2392 independent reflections	k = −16→16
2382 reflections with I > 2σ(I)	l = −16→16

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.002	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.015	(Δ/σ)_max = 2.138
S = 0.09	Δρ_max = 0.06 e Å⁻³
2392 reflections	Δρ_min = −0.08 e Å⁻³
65 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 restraints	Absolute structure parameter: −0.001 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Co1	0.321200 (4)	0.0000	0.0000	0.02000 (2)*
Cl1	0.533000 (7)	0.0000	0.0000	0.02000 (2)*
Cl2	0.109300 (7)	0.0000	0.0000	0.02000 (2)*
N1	0.31570 (2)	0.068800 (18)	0.102200 (14)	0.02000 (4)*
N2	0.32330 (2)	−0.144600 (19)	0.053100 (15)	0.02000 (4)*
C1	0.38630 (2)	−0.01010 (2)	0.152600 (17)	0.02000 (5)*
C2	0.34350 (2)	−0.13130 (2)	0.135500 (16)	0.02000 (5)*
C3	0.30130 (2)	−0.244700 (19)	0.025700 (17)	0.02000 (5)*
C4	0.26390 (2)	−0.25960 (2)	−0.054800 (17)	0.02000 (5)*
C5	0.33980 (2)	−0.19680 (2)	−0.113500 (17)	0.02000 (5)*
C11	0.30920 (2)	−0.35280 (2)	0.072500 (17)	0.02000 (4)*
C12	0.29180 (2)	−0.23070 (2)	−0.192300 (16)	0.02000 (4)*
C13	0.47870 (2)	−0.22710 (2)	−0.107700 (17)	0.02000 (4)*
Cl3	0.0000	0.038400 (6)	0.2500	0.02000 (2)*
O1	0.00450 (4)	0.15920 (3)	0.268200 (18)	0.02000 (8)*	0.50
O2	−0.10430 (3)	−0.01440 (3)	0.27610 (3)	0.02000 (7)*	0.50
O3	0.04160 (3)	0.01610 (3)	0.17900 (2)	0.02000 (6)*	0.50
O4	0.11040 (3)	−0.00660 (3)	0.30160 (2)	0.02000 (7)*	0.50

Geometric parameters (Å, º) top

Co1—N2	1.9265 (3)	C5—C12	1.5381 (4)
Co1—N2ⁱ	1.9265 (3)	Cl3—O2	1.3483 (4)
Co1—N1	1.9808 (3)	Cl3—O2ⁱⁱ	1.3483 (4)
Co1—N1ⁱ	1.9808 (3)	Cl3—O3ⁱⁱ	1.3586 (4)
Co1—Cl1	2.2495 (4)	Cl3—O3	1.3586 (4)
Co1—Cl2	2.2506 (4)	Cl3—O1	1.4415 (4)
N1—C1	1.4837 (4)	Cl3—O1ⁱⁱ	1.4415 (4)
N1—C5ⁱ	1.5230 (4)	Cl3—O4	1.5763 (4)
N2—C3	1.2823 (4)	Cl3—O4ⁱⁱ	1.5763 (4)
N2—C2	1.4841 (4)	O1—O1ⁱⁱ	0.6522 (6)
C1—C2	1.5111 (4)	O2—O3ⁱⁱ	1.0965 (6)
C3—C4	1.4911 (4)	O2—O4ⁱⁱ	1.3816 (7)
C3—C11	1.5080 (4)	O3—O2ⁱⁱ	1.0965 (6)
C4—C5	1.5050 (4)	O3—O4ⁱⁱ	1.6716 (6)
C5—C13	1.5202 (4)	O4—O2ⁱⁱ	1.3816 (7)
C5—N1ⁱ	1.5230 (4)	O4—O3ⁱⁱ	1.6716 (6)

N2—Co1—N2ⁱ	178.673 (13)	O2—Cl3—O3	119.88 (2)
N2—Co1—N1	84.601 (14)	O2ⁱⁱ—Cl3—O3	47.79 (2)
N2ⁱ—Co1—N1	95.439 (13)	O3ⁱⁱ—Cl3—O3	158.00 (3)
N2—Co1—N1ⁱ	95.439 (13)	O2—Cl3—O1	113.20 (2)
N2ⁱ—Co1—N1ⁱ	84.601 (14)	O2ⁱⁱ—Cl3—O1	119.53 (2)
N1—Co1—N1ⁱ	176.620 (13)	O3ⁱⁱ—Cl3—O1	89.39 (2)
N2—Co1—Cl1	89.337 (7)	O3—Cl3—O1	112.48 (2)
N2ⁱ—Co1—Cl1	89.337 (7)	O2—Cl3—O1ⁱⁱ	119.53 (2)
N1—Co1—Cl1	91.690 (6)	O2ⁱⁱ—Cl3—O1ⁱⁱ	113.20 (2)
N1ⁱ—Co1—Cl1	91.690 (6)	O3ⁱⁱ—Cl3—O1ⁱⁱ	112.48 (2)
N2—Co1—Cl2	90.663 (7)	O3—Cl3—O1ⁱⁱ	89.39 (2)
N2ⁱ—Co1—Cl2	90.663 (7)	O1—Cl3—O1ⁱⁱ	26.15 (3)
N1—Co1—Cl2	88.310 (6)	O2—Cl3—O4	105.13 (2)
N1ⁱ—Co1—Cl2	88.310 (6)	O2ⁱⁱ—Cl3—O4	55.72 (3)
Cl1—Co1—Cl2	180.0	O3ⁱⁱ—Cl3—O4	68.98 (2)
C1—N1—C5ⁱ	116.09 (2)	O3—Cl3—O4	103.42 (2)
C1—N1—Co1	106.621 (18)	O1—Cl3—O4	99.72 (2)
C5ⁱ—N1—Co1	120.645 (19)	O1ⁱⁱ—Cl3—O4	118.536 (19)
C3—N2—C2	119.57 (2)	O2—Cl3—O4ⁱⁱ	55.72 (3)
C3—N2—Co1	127.20 (2)	O2ⁱⁱ—Cl3—O4ⁱⁱ	105.13 (2)
C2—N2—Co1	113.046 (17)	O3ⁱⁱ—Cl3—O4ⁱⁱ	103.42 (2)
N1—C1—C2	107.67 (2)	O3—Cl3—O4ⁱⁱ	68.98 (2)
N2—C2—C1	109.75 (2)	O1—Cl3—O4ⁱⁱ	118.536 (19)
N2—C3—C4	121.08 (2)	O1ⁱⁱ—Cl3—O4ⁱⁱ	99.72 (2)
N2—C3—C11	122.53 (3)	O4—Cl3—O4ⁱⁱ	141.24 (3)
C4—C3—C11	116.38 (2)	O1ⁱⁱ—O1—Cl3	76.926 (13)
C3—C4—C5	117.54 (2)	O3ⁱⁱ—O2—Cl3	66.60 (3)
C4—C5—C13	111.14 (2)	O3ⁱⁱ—O2—O4ⁱⁱ	136.94 (5)
C4—C5—N1ⁱ	107.03 (2)	Cl3—O2—O4ⁱⁱ	70.53 (3)
C13—C5—N1ⁱ	112.37 (2)	O2ⁱⁱ—O3—Cl3	65.61 (3)
C4—C5—C12	109.02 (2)	O2ⁱⁱ—O3—O4ⁱⁱ	112.72 (4)
C13—C5—C12	108.89 (2)	Cl3—O3—O4ⁱⁱ	61.67 (2)
N1ⁱ—C5—C12	108.30 (2)	O2ⁱⁱ—O4—Cl3	53.75 (2)
O2—Cl3—O2ⁱⁱ	125.84 (3)	O2ⁱⁱ—O4—O3ⁱⁱ	99.79 (3)
O2—Cl3—O3ⁱⁱ	47.79 (2)	Cl3—O4—O3ⁱⁱ	49.348 (19)
O2ⁱⁱ—Cl3—O3ⁱⁱ	119.88 (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

C₂₄N₁₄NiO_24.50P₂	γ = 90°
M_r = 997.01	V = 8603.1 (15) Å³
C222₁	Z = 8
a = 17.462 (2) Å	F(000) = 3968
b = 17.337 (2) Å	D_x = 1.540 Mg m⁻³
c = 28.417 (2) Å	Mo Kα radiation, λ = 0.71073 Å
α = 90°	µ = 0.63 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.042
Graphite monochromator	θ_max = 27.1°, θ_min = 1.4°
14536 measured reflections	h = −20→20
3648 independent reflections	k = −20→20
3605 reflections with I > 2σ(I)	l = −16→16

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.006	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.039	(Δ/σ)_max = 0.880
S = 0.30	Δρ_max = 0.16 e Å⁻³
3648 reflections	Δρ_min = −0.21 e Å⁻³
267 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 restraints	Absolute structure parameter: 0.010 (5)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ni1	0.298650 (15)	0.0000	0.0000	0.02000 (8)*
P1	0.23220 (2)	0.29400 (2)	0.00420 (2)	0.02000 (10)*
O1	0.30327 (5)	0.10173 (5)	−0.04095 (5)	0.0200 (2)*
O3	0.45785 (6)	−0.12660 (6)	0.03725 (5)	0.0200 (2)*
O4	0.42922 (6)	0.25003 (6)	0.10735 (5)	0.0200 (3)*
O5	0.50230 (6)	0.36440 (5)	0.01020 (4)	0.0200 (2)*
O6	0.59385 (6)	0.29415 (6)	0.07580 (5)	0.0200 (2)*
O7	0.30607 (5)	0.27387 (6)	0.03695 (5)	0.0200 (2)*
O8	0.16992 (5)	0.31813 (6)	0.03810 (5)	0.0200 (2)*
O9	0.21407 (6)	0.21787 (5)	−0.01960 (4)	0.0200 (2)*
O10	0.25460 (6)	0.35565 (5)	−0.02945 (5)	0.0200 (2)*
N1	0.20748 (7)	0.04338 (7)	0.04070 (6)	0.0200 (3)*
N3	0.38678 (7)	0.03948 (7)	0.04695 (6)	0.0200 (3)*
N4	0.56972 (7)	−0.06397 (7)	0.05040 (6)	0.0200 (3)*
N5	0.68965 (7)	−0.01035 (7)	0.06060 (6)	0.0200 (3)*
N6	0.58475 (7)	0.06510 (7)	0.07595 (6)	0.0200 (3)*
N7	0.46355 (7)	0.13165 (7)	0.07635 (6)	0.0200 (3)*
C1	0.13870 (8)	0.00740 (8)	0.02415 (6)	0.0200 (4)*
C3	0.45938 (9)	0.00928 (9)	0.05435 (7)	0.0200 (4)*
C4	0.48853 (9)	−0.06447 (8)	0.04705 (7)	0.0200 (4)*
C5	0.61263 (8)	−0.00117 (9)	0.06260 (7)	0.0200 (3)*
C6	0.50773 (9)	0.06693 (8)	0.07015 (7)	0.0200 (4)*
C7	0.39065 (9)	0.11185 (8)	0.06105 (7)	0.0200 (4)*
C8	0.49200 (9)	0.20405 (8)	0.09200 (7)	0.0200 (3)*
C9	0.42228 (8)	0.31842 (8)	0.07590 (7)	0.0200 (3)*
C10	0.46997 (8)	0.29792 (8)	0.03315 (7)	0.0200 (4)*
C11	0.53510 (8)	0.24885 (8)	0.05325 (7)	0.0200 (3)*
C12	0.33885 (9)	0.33100 (8)	0.06725 (7)	0.0200 (4)*
Ni2	0.5000	0.225350 (14)	0.2500	0.02000 (8)*
P3	0.22225 (2)	0.30960 (2)	0.22155 (2)	0.02000 (10)*
O19	0.60582 (5)	0.22517 (5)	0.21415 (5)	0.0200 (2)*
O21	0.63575 (6)	0.07470 (6)	0.20845 (5)	0.0200 (2)*
O22	0.25920 (6)	0.08675 (5)	0.14255 (4)	0.0200 (2)*
O23	0.14867 (5)	0.03987 (5)	0.24615 (5)	0.0200 (2)*
O24	0.21070 (6)	−0.07095 (5)	0.18450 (5)	0.0200 (2)*
O25	0.23750 (6)	0.22365 (6)	0.20230 (5)	0.0200 (2)*
O26	0.29385 (5)	0.32420 (5)	0.24900 (5)	0.0200 (2)*
O27	0.15137 (5)	0.30417 (5)	0.25170 (5)	0.0200 (2)*
O28	0.21267 (6)	0.36298 (5)	0.18020 (5)	0.0200 (2)*
N17	0.53875 (7)	0.31540 (7)	0.29335 (6)	0.0200 (3)*
N19	0.46782 (7)	0.13418 (7)	0.20245 (6)	0.0200 (3)*
N20	0.58525 (7)	−0.03820 (7)	0.18255 (6)	0.0200 (3)*
N21	0.54817 (7)	−0.15517 (7)	0.14905 (6)	0.0200 (3)*
N22	0.45540 (7)	−0.06000 (7)	0.16135 (6)	0.0200 (3)*
N23	0.37800 (7)	0.05455 (7)	0.17325 (6)	0.0200 (3)*
C27	0.51533 (8)	0.38872 (8)	0.27005 (6)	0.0200 (4)*
C29	0.49773 (9)	0.06528 (9)	0.19280 (6)	0.0200 (4)*
C30	0.57735 (9)	0.03755 (9)	0.19640 (7)	0.0200 (4)*
C31	0.52692 (8)	−0.08353 (8)	0.16340 (7)	0.0200 (4)*
C32	0.44627 (9)	0.01367 (8)	0.17370 (7)	0.0200 (4)*
C33	0.39300 (8)	0.12660 (9)	0.19060 (7)	0.0200 (4)*
C34	0.30295 (9)	0.02320 (8)	0.15980 (7)	0.0200 (3)*
C35	0.19307 (9)	0.09912 (8)	0.17240 (7)	0.0200 (4)*
C36	0.21265 (8)	0.06035 (8)	0.21845 (7)	0.0200 (3)*
C37	0.26145 (8)	−0.01035 (8)	0.20205 (7)	0.0200 (4)*
C38	0.17805 (8)	0.18565 (9)	0.17510 (7)	0.0200 (3)*
N13	0.14797 (7)	0.29833 (7)	0.34425 (6)	0.0200 (3)*
N14	0.28272 (7)	0.15217 (7)	0.37800 (6)	0.0200 (3)*
C23	0.21842 (9)	0.26832 (8)	0.36460 (7)	0.0200 (4)*
C24	0.22548 (8)	0.18463 (8)	0.34900 (7)	0.0200 (3)*
O48	0.02962 (11)	0.18173 (11)	0.36345 (9)	0.0200 (5)*	0.50
O49	0.05827 (11)	0.23722 (11)	0.40845 (10)	0.0200 (5)*	0.50
O37	0.38802 (6)	0.55832 (6)	0.03400 (5)	0.0200 (2)*
O39	0.30772 (5)	0.48513 (5)	0.16625 (4)	0.0200 (2)*
O41	0.08448 (6)	0.19537 (5)	0.06830 (5)	0.0200 (2)*
O42	0.05268 (5)	0.01863 (5)	0.37895 (4)	0.0200 (2)*
O45	0.0000	0.25415 (8)	0.2500	0.0200 (3)*
O46	0.57687 (5)	0.42682 (5)	0.12830 (5)	0.0200 (2)*

Geometric parameters (Å, º) top

Ni1—N1ⁱ	2.1066 (14)	Ni2—O19ⁱⁱ	2.1100 (11)
Ni1—N1	2.1066 (14)	Ni2—O19	2.1100 (11)
Ni1—O1ⁱ	2.1146 (11)	Ni2—N19	2.1541 (14)
Ni1—O1	2.1146 (11)	Ni2—N19ⁱⁱ	2.1541 (14)
Ni1—N3	2.1487 (14)	P3—O26	1.4952 (11)
Ni1—N3ⁱ	2.1487 (14)	P3—O28	1.5051 (12)
P1—O10	1.4865 (12)	P3—O27	1.5083 (12)
P1—O8	1.5119 (13)	P3—O25	1.6096 (11)
P1—O9	1.5165 (10)	O21—C30	1.2538 (19)
P1—O7	1.6284 (12)	O22—C34	1.4275 (19)
O3—C4	1.2349 (19)	O22—C35	1.449 (2)
O4—C8	1.424 (2)	O23—C36	1.412 (2)
O4—C9	1.4897 (19)	O24—C37	1.462 (2)
O5—C10	1.4396 (19)	O25—C38	1.452 (2)
O6—C11	1.442 (2)	N17—C27	1.4905 (19)
O7—C12	1.432 (2)	N19—C29	1.332 (2)
N1—C1	1.433 (2)	N19—C33	1.356 (2)
N3—C7	1.3189 (19)	N20—C30	1.3779 (19)
N3—C3	1.388 (2)	N20—C31	1.397 (2)
N4—C5	1.366 (2)	N21—C31	1.359 (2)
N4—C4	1.4210 (19)	N22—C31	1.315 (2)
N5—C5	1.3555 (19)	N22—C32	1.334 (2)
N6—C5	1.304 (2)	N23—C33	1.368 (2)
N6—C6	1.355 (2)	N23—C32	1.387 (2)
N7—C6	1.373 (2)	N23—C34	1.469 (2)
N7—C7	1.388 (2)	C27—C27ⁱⁱ	1.259 (3)
N7—C8	1.4213 (19)	C29—C32	1.379 (3)
C1—C1ⁱ	1.396 (3)	C29—C30	1.475 (2)
C3—C6	1.383 (2)	C34—C37	1.518 (3)
C3—C4	1.392 (2)	C35—C36	1.510 (3)
C8—C11	1.543 (3)	C35—C38	1.5249 (19)
C9—C12	1.493 (2)	C36—C37	1.564 (2)
C9—C10	1.515 (3)	N13—C23	1.456 (2)
C10—C11	1.531 (2)	N14—C24	1.412 (2)
Ni2—N17	2.1007 (14)	C23—C24	1.522 (2)
Ni2—N17ⁱⁱ	2.1007 (14)	O48—O49	1.677 (3)

N1ⁱ—Ni1—N1	81.82 (8)	N17—Ni2—O19ⁱⁱ	90.00 (5)
N1ⁱ—Ni1—O1ⁱ	91.90 (5)	N17ⁱⁱ—Ni2—O19ⁱⁱ	90.12 (5)
N1—Ni1—O1ⁱ	91.40 (5)	N17—Ni2—O19	90.12 (5)
N1ⁱ—Ni1—O1	91.40 (5)	N17ⁱⁱ—Ni2—O19	90.00 (5)
N1—Ni1—O1	91.90 (5)	O19ⁱⁱ—Ni2—O19	179.83 (6)
O1ⁱ—Ni1—O1	175.63 (5)	N17—Ni2—N19	175.75 (5)
N1ⁱ—Ni1—N3	174.81 (6)	N17ⁱⁱ—Ni2—N19	95.36 (5)
N1—Ni1—N3	94.97 (5)	O19ⁱⁱ—Ni2—N19	94.21 (5)
O1ⁱ—Ni1—N3	84.07 (5)	O19—Ni2—N19	85.67 (5)
O1—Ni1—N3	92.79 (5)	N17—Ni2—N19ⁱⁱ	95.36 (5)
N1ⁱ—Ni1—N3ⁱ	94.97 (5)	N17ⁱⁱ—Ni2—N19ⁱⁱ	175.75 (5)
N1—Ni1—N3ⁱ	174.81 (6)	O19ⁱⁱ—Ni2—N19ⁱⁱ	85.67 (5)
O1ⁱ—Ni1—N3ⁱ	92.79 (5)	O19—Ni2—N19ⁱⁱ	94.21 (5)
O1—Ni1—N3ⁱ	84.07 (5)	N19—Ni2—N19ⁱⁱ	85.59 (8)
N3—Ni1—N3ⁱ	88.51 (8)	O26—P3—O28	113.34 (6)
O10—P1—O8	113.59 (6)	O26—P3—O27	113.60 (8)
O10—P1—O9	113.19 (7)	O28—P3—O27	113.00 (6)
O8—P1—O9	112.01 (6)	O26—P3—O25	101.29 (6)
O10—P1—O7	108.26 (6)	O28—P3—O25	108.80 (7)
O8—P1—O7	105.36 (7)	O27—P3—O25	105.73 (6)
O9—P1—O7	103.52 (6)	C34—O22—C35	109.86 (12)
C8—O4—C9	108.93 (13)	C38—O25—P3	118.86 (9)
C12—O7—P1	120.80 (9)	C27—N17—Ni2	106.56 (10)
C1—N1—Ni1	107.33 (10)	C29—N19—C33	103.87 (13)
C7—N3—C3	105.43 (13)	C29—N19—Ni2	133.22 (12)
C7—N3—Ni1	121.90 (11)	C33—N19—Ni2	118.58 (11)
C3—N3—Ni1	128.92 (11)	C30—N20—C31	125.07 (13)
C5—N4—C4	124.68 (14)	C31—N22—C32	113.50 (13)
C5—N6—C6	110.83 (14)	C33—N23—C32	107.38 (13)
C6—N7—C7	105.84 (12)	C33—N23—C34	127.03 (12)
C6—N7—C8	124.44 (12)	C32—N23—C34	125.45 (12)
C7—N7—C8	129.56 (12)	C27ⁱⁱ—C27—N17	121.25 (9)
C1ⁱ—C1—N1	113.75 (11)	N19—C29—C32	114.03 (14)
C6—C3—N3	109.52 (13)	N19—C29—C30	130.36 (14)
C6—C3—C4	119.27 (14)	C32—C29—C30	115.47 (14)
N3—C3—C4	131.16 (14)	O21—C30—N20	119.09 (14)
O3—C4—C3	132.56 (13)	O21—C30—C29	128.19 (13)
O3—C4—N4	116.95 (14)	N20—C30—C29	112.66 (14)
C3—C4—N4	110.45 (13)	N22—C31—N21	121.97 (14)
N6—C5—N5	119.08 (15)	N22—C31—N20	122.36 (14)
N6—C5—N4	124.82 (13)	N21—C31—N20	115.60 (13)
N5—C5—N4	116.10 (15)	N22—C32—C29	130.29 (15)
N6—C6—N7	124.13 (14)	N22—C32—N23	126.12 (15)
N6—C6—C3	128.92 (16)	C29—C32—N23	103.42 (13)
N7—C6—C3	106.81 (13)	N19—C33—N23	111.26 (13)
N3—C7—N7	112.17 (13)	O22—C34—N23	106.33 (11)
N7—C8—O4	108.73 (11)	O22—C34—C37	108.17 (12)
N7—C8—C11	113.06 (16)	N23—C34—C37	111.21 (15)
O4—C8—C11	108.19 (12)	O22—C35—C36	105.13 (12)
O4—C9—C12	107.12 (12)	O22—C35—C38	108.19 (13)
O4—C9—C10	104.45 (12)	C36—C35—C38	115.67 (16)
C12—C9—C10	116.00 (16)	O23—C36—C35	114.57 (13)
O5—C10—C9	113.01 (12)	O23—C36—C37	113.59 (12)
O5—C10—C11	108.82 (11)	C35—C36—C37	102.36 (15)
C9—C10—C11	103.86 (15)	O24—C37—C34	107.15 (15)
O6—C11—C10	113.06 (12)	O24—C37—C36	109.55 (11)
O6—C11—C8	107.69 (15)	C34—C37—C36	101.27 (13)
C10—C11—C8	100.58 (13)	O25—C38—C35	110.50 (13)
O7—C12—C9	112.83 (13)	N13—C23—C24	107.07 (14)
N17—Ni2—N17ⁱⁱ	83.99 (8)	N14—C24—C23	105.50 (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

C₅H₁₅N₂NaO₉	γ = 90°
M_r = 270.18	V = 2268.9 (6) Å³
C222₁	Z = 8
a = 9.453 (2) Å	F(000) = 1136
b = 17.812 (2) Å	D_x = 1.582 Mg m⁻³
c = 13.475 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 0.18 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.013
Graphite monochromator	θ_max = 67.7°, θ_min = 2.3°
18110 measured reflections	h = −12→12
5671 independent reflections	k = −36→36
4802 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.009	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.057	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.25	(Δ/σ)_max = 3.198
5671 reflections	Δρ_max = 0.08 e Å⁻³
113 parameters	Δρ_min = −0.21 e Å⁻³
0 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.06 (8)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0.46230 (2)	−0.130200 (8)	−0.088100 (15)	0.02000 (3)*
N1	0.53650 (4)	−0.379200 (17)	0.11550 (3)	0.02000 (5)*
H13	0.6197 (9)	−0.3554 (5)	0.1107 (7)	0.0200 (16)*
N2	0.45060 (4)	−0.338300 (16)	−0.07680 (3)	0.02000 (5)*
H1	0.5118 (9)	−0.2966 (5)	−0.0634 (6)	0.0200 (16)*
H2	0.4028 (9)	−0.3303 (4)	−0.1389 (6)	0.0200 (17)*
H3	0.5056 (9)	−0.3835 (4)	−0.0806 (6)	0.0200 (16)*
O1	0.78280 (3)	−0.449700 (15)	0.14750 (3)	0.02000 (4)*
O2	0.68190 (3)	−0.559500 (15)	0.11080 (3)	0.02000 (4)*
O3	0.42420 (3)	−0.491600 (15)	0.12270 (3)	0.02000 (5)*
O4	0.12600 (3)	−0.279900 (15)	0.03880 (3)	0.02000 (4)*
O5	0.27360 (3)	−0.220900 (14)	−0.06470 (3)	0.02000 (4)*
C1	0.67960 (4)	−0.490300 (18)	0.12760 (4)	0.02000 (5)*
C2	0.53260 (4)	−0.453400 (19)	0.12160 (3)	0.02000 (5)*
C3	0.41030 (5)	−0.333100 (19)	0.10470 (4)	0.02000 (5)*
H7	0.4419 (8)	−0.2783 (5)	0.1174 (7)	0.0200 (17)*
H8	0.3425 (9)	−0.3473 (5)	0.1533 (6)	0.0200 (17)*
C4	0.34080 (4)	−0.339700 (19)	0.00240 (4)	0.02000 (6)*
H9	0.2876 (8)	−0.3890 (4)	−0.0064 (6)	0.0200 (17)*
C5	0.23740 (4)	−0.27410 (2)	−0.01060 (4)	0.02000 (5)*
O11	0.80390 (3)	−0.181500 (15)	0.25850 (3)	0.02000 (5)*
O12	0.46930 (3)	−0.088300 (15)	0.08200 (3)	0.02000 (5)*
H16	0.3743 (9)	−0.0718 (4)	0.0807 (6)	0.0200 (17)*
H17	0.5124 (9)	−0.0450 (4)	0.0945 (6)	0.0200 (16)*
O14	0.0000	−0.31080 (2)	0.2500	0.02000 (6)*
O15	0.63510 (3)	−0.033400 (16)	−0.14920 (3)	0.02000 (4)*
H20	0.7289 (16)	−0.0273 (9)	−0.1345 (12)	0.020 (3)*	0.50
H21	0.6519 (17)	−0.0227 (9)	−0.2164 (13)	0.020 (3)*	0.50
O18	−0.5000	−0.17990 (2)	0.2500	0.02000 (6)*

Geometric parameters (Å, º) top

Na1—O4ⁱ	2.3238 (4)	O2—C1	1.2534 (4)
Na1—O1ⁱⁱ	2.3548 (4)	O3—C2	1.2301 (5)
Na1—O12	2.4114 (5)	O4—C5	1.2501 (5)
Na1—O5	2.4272 (4)	O4—Na1ⁱⁱ	2.3238 (4)
Na1—O14ⁱ	2.4476 (4)	O5—C5	1.2436 (5)
Na1—O15	2.5138 (4)	C1—C2	1.5393 (6)
N1—C2	1.3247 (5)	C3—C4	1.5316 (7)
N1—C3	1.4555 (6)	C4—C5	1.5334 (5)
N2—C4	1.4889 (7)	O14—Na1ⁱⁱ	2.4476 (4)
O1—C1	1.2436 (5)	O14—Na1ⁱⁱⁱ	2.4476 (4)
O1—Na1ⁱ	2.3548 (4)

O4ⁱ—Na1—O1ⁱⁱ	173.443 (13)	C5—O4—Na1ⁱⁱ	140.37 (3)
O4ⁱ—Na1—O12	85.599 (14)	C5—O5—Na1	141.77 (3)
O1ⁱⁱ—Na1—O12	98.964 (14)	O1—C1—O2	126.67 (4)
O4ⁱ—Na1—O5	89.633 (17)	O1—C1—C2	118.11 (3)
O1ⁱⁱ—Na1—O5	85.231 (17)	O2—C1—C2	115.22 (3)
O12—Na1—O5	95.894 (13)	O3—C2—N1	125.15 (4)
O4ⁱ—Na1—O14ⁱ	82.067 (13)	O3—C2—C1	121.01 (3)
O1ⁱⁱ—Na1—O14ⁱ	93.523 (14)	N1—C2—C1	113.84 (3)
O12—Na1—O14ⁱ	167.446 (12)	N1—C3—C4	113.47 (3)
O5—Na1—O14ⁱ	86.389 (13)	N2—C4—C3	110.17 (4)
O4ⁱ—Na1—O15	97.675 (18)	N2—C4—C5	110.47 (4)
O1ⁱⁱ—Na1—O15	86.696 (17)	C3—C4—C5	108.53 (3)
O12—Na1—O15	94.658 (14)	O5—C5—O4	127.37 (4)
O5—Na1—O15	167.593 (15)	O5—C5—C4	118.18 (4)
O14ⁱ—Na1—O15	84.719 (13)	O4—C5—C4	114.40 (4)
C2—N1—C3	123.11 (3)	Na1ⁱⁱ—O14—Na1ⁱⁱⁱ	129.146 (19)
C1—O1—Na1ⁱ	147.50 (3)

Symmetry codes: (i) x+1/2, −y−1/2, −z; (ii) x−1/2, −y−1/2, −z; (iii) −x+1/2, −y−1/2, z+1/2.

(bogpiw) Dicarbonyl-(eta$5!-cyclopentadienyl)-(sulfur dioxide)-iron(iii) hexafluoroarsenate top

Crystal data top

C₇H₅AsF₆FeO₄S	γ = 90°
M_r = 429.94	V = 1265.9 (5) Å³
Cmc2₁	Z = 4
a = 8.068 (2) Å	F(000) = 832
b = 13.904 (4) Å	D_x = 2.256 Mg m⁻³
c = 11.285 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 4.03 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.023
Graphite monochromator	θ_max = 53.1°, θ_min = 2.9°
7020 measured reflections	h = −16→16
1916 independent reflections	k = −16→16
1903 reflections with I > 2σ(I)	l = −12→12

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.005	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.024	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.15	(Δ/σ)_max = 2.807
1916 reflections	Δρ_max = 0.19 e Å⁻³
60 parameters	Δρ_min = −0.27 e Å⁻³
1 restraint	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.0108 (18)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe1	0.0000	0.184900 (11)	0.257400 (13)	0.02000 (3)*
As1	0.5000	0.072700 (7)	0.063800 (9)	0.02000 (2)*
F1	0.5000	0.05280 (5)	−0.08470 (5)	0.02000 (10)*
F2	0.35070 (4)	0.16060 (3)	0.04350 (4)	0.02000 (7)*
F3	0.34890 (4)	−0.01220 (3)	0.08470 (4)	0.02000 (7)*
F5	0.5000	0.09780 (5)	0.21090 (5)	0.02000 (9)*
S1	0.0000	0.172300 (17)	0.07120 (2)	0.02000 (4)*
O1	0.0000	0.08190 (5)	0.01370 (7)	0.02000 (10)*
O2	0.0000	0.25750 (5)	0.00080 (7)	0.02000 (10)*
C1	0.13670 (7)	0.10800 (6)	0.38110 (6)	0.02000 (9)*
C2	0.0000	0.14200 (7)	0.43320 (9)	0.02000 (14)*
C5	0.08820 (6)	0.04820 (6)	0.29260 (6)	0.02000 (9)*
C6	0.16640 (6)	0.27390 (5)	0.25760 (7)	0.02000 (9)*
O3	0.27090 (5)	0.32580 (3)	0.26000 (5)	0.02000 (8)*
H1	0.2489 (12)	0.1230 (5)	0.4023 (9)	0.020 (3)*
H2	0.0000	0.1852 (9)	0.4994 (14)	0.020 (4)*
H5	0.1592 (12)	0.0127 (7)	0.2401 (8)	0.020 (2)*

Geometric parameters (Å, º) top

Fe1—C6	1.8258 (7)	As1—F3ⁱⁱ	1.7133 (5)
Fe1—C6ⁱ	1.8258 (7)	As1—F2ⁱⁱ	1.7312 (5)
Fe1—C5	2.0680 (10)	As1—F2	1.7312 (5)
Fe1—C5ⁱ	2.0680 (10)	S1—O1	1.4145 (9)
Fe1—C2	2.0716 (11)	S1—O2	1.4264 (9)
Fe1—C1	2.0756 (8)	C1—C2	1.3362 (9)
Fe1—C1ⁱ	2.0756 (8)	C1—C5	1.3572 (10)
Fe1—S1	2.1086 (5)	C2—C1ⁱ	1.3362 (9)
As1—F5	1.6963 (7)	C5—C5ⁱ	1.4232 (11)
As1—F1	1.6985 (7)	C6—O3	1.1101 (8)
As1—F3	1.7133 (5)

C6—Fe1—C6ⁱ	94.66 (4)	F5—As1—F1	177.50 (3)
C6—Fe1—C5	111.69 (3)	F5—As1—F3	90.40 (2)
C6ⁱ—Fe1—C5	151.13 (3)	F1—As1—F3	91.35 (2)
C6—Fe1—C5ⁱ	151.13 (3)	F5—As1—F3ⁱⁱ	90.40 (2)
C6ⁱ—Fe1—C5ⁱ	111.69 (3)	F1—As1—F3ⁱⁱ	91.35 (2)
C5—Fe1—C5ⁱ	40.25 (3)	F3—As1—F3ⁱⁱ	90.72 (3)
C6—Fe1—C2	101.18 (3)	F5—As1—F2ⁱⁱ	89.10 (2)
C6ⁱ—Fe1—C2	101.18 (3)	F1—As1—F2ⁱⁱ	89.11 (2)
C5—Fe1—C2	63.35 (3)	F3—As1—F2ⁱⁱ	178.639 (18)
C5ⁱ—Fe1—C2	63.35 (3)	F3ⁱⁱ—As1—F2ⁱⁱ	90.55 (3)
C6—Fe1—C1	87.57 (3)	F5—As1—F2	89.10 (2)
C6ⁱ—Fe1—C1	137.65 (3)	F1—As1—F2	89.11 (2)
C5—Fe1—C1	38.24 (3)	F3—As1—F2	90.55 (3)
C5ⁱ—Fe1—C1	65.18 (3)	F3ⁱⁱ—As1—F2	178.639 (18)
C2—Fe1—C1	37.59 (2)	F2ⁱⁱ—As1—F2	88.18 (3)
C6—Fe1—C1ⁱ	137.65 (3)	O1—S1—O2	118.85 (5)
C6ⁱ—Fe1—C1ⁱ	87.57 (3)	O1—S1—Fe1	122.07 (4)
C5—Fe1—C1ⁱ	65.18 (3)	O2—S1—Fe1	119.08 (4)
C5ⁱ—Fe1—C1ⁱ	38.24 (3)	C2—C1—C5	107.61 (6)
C2—Fe1—C1ⁱ	37.59 (2)	C2—C1—Fe1	71.04 (5)
C1—Fe1—C1ⁱ	64.19 (4)	C5—C1—Fe1	70.58 (5)
C6—Fe1—S1	93.30 (2)	C1ⁱ—C2—C1	111.25 (9)
C6ⁱ—Fe1—S1	93.30 (2)	C1ⁱ—C2—Fe1	71.37 (5)
C5—Fe1—S1	96.61 (2)	C1—C2—Fe1	71.37 (5)
C5ⁱ—Fe1—S1	96.61 (2)	C1—C5—C5ⁱ	106.76 (3)
C2—Fe1—S1	158.50 (3)	C1—C5—Fe1	71.19 (5)
C1—Fe1—S1	128.86 (2)	C5ⁱ—C5—Fe1	69.874 (17)
C1ⁱ—Fe1—S1	128.86 (2)	O3—C6—Fe1	177.51 (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

C₆₁H₅₈Cu₂N₄O₇P₄	γ = 90°
M_r = 1210.07	V = 5738.7 (11) Å³
Cmc2₁	Z = 4
a = 21.719 (2) Å	F(000) = 2504
b = 16.545 (2) Å	D_x = 1.401 Mg m⁻³
c = 15.970 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 0.91 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.030
Graphite monochromator	θ_max = 30.4°, θ_min = 1.6°
10772 measured reflections	h = −20→20
2892 independent reflections	k = −20→20
2853 reflections with I > 2σ(I)	l = −12→12

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.011	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.046	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.34	(Δ/σ)_max = 1.469
2892 reflections	Δρ_max = 0.52 e Å⁻³
275 parameters	Δρ_min = −0.21 e Å⁻³
1 restraint	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.007 (5)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cu1	0.084100 (12)	0.681600 (11)	0.070900 (15)	0.02000 (8)*
X1	0.53100 (8)	0.60450 (6)	0.10790 (9)	0.0200 (3)*
P1	0.07030 (3)	0.81640 (2)	0.06450 (4)	0.02000 (13)*
P2	0.07070 (2)	0.60340 (2)	0.18580 (3)	0.02000 (12)*
O3	0.0000	0.80850 (9)	0.33590 (12)	0.0200 (4)*
O4	0.04960 (7)	0.62480 (7)	−0.04300 (8)	0.0200 (3)*
O5	0.04850 (7)	0.82290 (6)	0.45130 (8)	0.0200 (3)*
O6	0.0000	0.52200 (8)	−0.08560 (10)	0.0200 (4)*
N1	0.0000	0.59110 (11)	−0.05750 (13)	0.0200 (5)*
N2	0.0000	0.81740 (10)	0.41360 (15)	0.0200 (5)*
N4	0.17600 (8)	0.65570 (8)	0.03470 (9)	0.0200 (3)*
C2	0.0000	0.61560 (14)	0.24780 (17)	0.0200 (5)*
C3	0.0000	0.86000 (13)	0.11030 (18)	0.0200 (6)*
C4	0.22180 (10)	0.68860 (9)	0.07670 (13)	0.0200 (4)*
C5	0.07830 (9)	0.86620 (11)	−0.03580 (13)	0.0200 (4)*
C6	0.28260 (10)	0.66730 (10)	0.06600 (13)	0.0200 (4)*
C7	0.07600 (9)	0.95010 (11)	−0.04500 (13)	0.0200 (4)*
C8	0.29610 (12)	0.60910 (10)	0.00880 (11)	0.0200 (4)*
C9	0.08310 (9)	0.98530 (11)	−0.12300 (13)	0.0200 (4)*
C10	0.25020 (9)	0.57390 (9)	−0.03560 (12)	0.0200 (4)*
C11	0.09290 (10)	0.93850 (10)	−0.19140 (13)	0.0200 (4)*
C12	0.19020 (10)	0.59870 (9)	−0.02220 (13)	0.0200 (4)*
C13	0.09540 (10)	0.85610 (10)	−0.18420 (13)	0.0200 (4)*
C14	0.08790 (10)	0.81970 (9)	−0.10600 (16)	0.0200 (5)*
C15	0.13220 (10)	0.86050 (9)	0.12740 (12)	0.0200 (4)*
C16	0.18450 (9)	0.89290 (9)	0.09120 (13)	0.0200 (4)*
C17	0.23560 (11)	0.91110 (11)	0.13990 (12)	0.0200 (4)*
C18	0.23490 (11)	0.89860 (9)	0.22370 (12)	0.0200 (4)*
C19	0.18310 (10)	0.86830 (9)	0.26150 (13)	0.0200 (4)*
C20	0.13180 (11)	0.84930 (10)	0.21410 (12)	0.0200 (4)*
C21	0.07850 (9)	0.49490 (10)	0.17160 (12)	0.0200 (4)*
C22	0.07980 (10)	0.46300 (10)	0.09130 (13)	0.0200 (4)*
C23	0.08290 (9)	0.37960 (10)	0.08130 (15)	0.0200 (4)*
C24	0.08610 (10)	0.33050 (11)	0.14740 (14)	0.0200 (5)*
C25	0.08680 (10)	0.36090 (11)	0.22710 (13)	0.0200 (4)*
C26	0.08260 (9)	0.44350 (11)	0.23900 (15)	0.0200 (4)*
C27	0.13110 (10)	0.62360 (10)	0.26460 (11)	0.0200 (4)*
C28	0.18930 (9)	0.59360 (9)	0.24910 (12)	0.0200 (4)*
C29	0.23720 (10)	0.61230 (9)	0.30290 (11)	0.0200 (4)*
C30	0.22740 (11)	0.66010 (10)	0.37120 (12)	0.0200 (4)*
C31	0.16970 (11)	0.68970 (9)	0.38750 (12)	0.0200 (4)*
C32	0.12170 (12)	0.67090 (9)	0.33390 (12)	0.0200 (4)*
H1	0.0693 (10)	0.9834 (11)	0.0047 (14)	0.020 (5)*
H2	0.0812 (9)	1.0451 (12)	−0.1264 (15)	0.020 (5)*
H3	0.0960 (10)	0.9649 (10)	−0.2458 (14)	0.020 (6)*
H4	0.1042 (11)	0.8227 (10)	−0.2330 (14)	0.020 (6)*
H5	0.0905 (9)	0.7605 (10)	−0.1002 (13)	0.020 (5)*
H6	0.1848 (9)	0.9048 (10)	0.0313 (14)	0.020 (5)*
H7	0.2717 (10)	0.9339 (10)	0.1132 (12)	0.020 (5)*
H8	0.2719 (10)	0.9074 (10)	0.2567 (13)	0.020 (5)*
H9	0.1816 (9)	0.8616 (10)	0.3229 (13)	0.020 (5)*
H10	0.0953 (11)	0.8273 (10)	0.2412 (16)	0.020 (6)*
H11	0.0781 (8)	0.4988 (12)	0.0431 (13)	0.020 (5)*
H12	0.0844 (9)	0.3558 (11)	0.0272 (15)	0.020 (5)*
H13	0.0857 (9)	0.2731 (13)	0.1378 (12)	0.020 (5)*
H14	0.0912 (10)	0.3229 (10)	0.2753 (15)	0.020 (6)*
H15	0.0823 (9)	0.4666 (11)	0.2962 (14)	0.020 (6)*
H16	0.1957 (9)	0.5610 (10)	0.1994 (12)	0.020 (5)*
H17	0.2781 (10)	0.5877 (10)	0.2905 (11)	0.020 (5)*
H18	0.2628 (10)	0.6710 (11)	0.4067 (13)	0.020 (5)*
H19	0.1630 (9)	0.7245 (10)	0.4371 (11)	0.020 (4)*
H20	0.0795 (10)	0.6917 (12)	0.3464 (15)	0.020 (6)*
H46	0.2118 (10)	0.7316 (10)	0.1169 (12)	0.020 (5)*
H47	0.3149 (9)	0.6926 (10)	0.1019 (12)	0.020 (5)*
H48	0.3387 (11)	0.5934 (10)	0.0027 (11)	0.020 (5)*
H49	0.2597 (9)	0.5316 (10)	−0.0777 (12)	0.020 (5)*
H50	0.1567 (10)	0.5731 (9)	−0.0546 (11)	0.020 (5)*
H51	0.0000	0.5760 (14)	0.2929 (17)	0.020 (6)*
H52	0.0000	0.6680 (14)	0.2738 (16)	0.020 (7)*
H53	0.0000	0.8514 (14)	0.1698 (19)	0.020 (7)*
H54	0.0000	0.9180 (14)	0.1013 (16)	0.020 (7)*

Geometric parameters (Å, º) top

Cu1—N4	2.1217 (17)	C7—C9	1.384 (3)
Cu1—O4	2.1802 (13)	C8—C10	1.355 (3)
Cu1—P1	2.2526 (5)	C9—C11	1.356 (3)
Cu1—P2	2.2640 (6)	C10—C12	1.383 (3)
X1—X1ⁱ	1.347 (3)	C11—C13	1.369 (2)
P1—C5	1.810 (2)	C13—C14	1.396 (3)
P1—C15	1.830 (2)	C15—C16	1.383 (3)
P1—C3	1.8403 (15)	C15—C20	1.397 (3)
P2—C21	1.8173 (18)	C16—C17	1.388 (3)
P2—C2	1.8382 (15)	C17—C18	1.354 (3)
P2—C27	1.848 (2)	C18—C19	1.372 (3)
O3—N2	1.250 (3)	C19—C20	1.383 (3)
O4—N1	1.2349 (16)	C21—C26	1.375 (3)
O5—N2	1.2167 (18)	C21—C22	1.387 (3)
O6—N1	1.228 (2)	C22—C23	1.391 (2)
N1—O4ⁱⁱ	1.2349 (16)	C23—C24	1.334 (3)
N2—O5ⁱⁱ	1.2167 (18)	C24—C25	1.369 (3)
N4—C4	1.317 (3)	C25—C26	1.383 (2)
N4—C12	1.345 (2)	C27—C32	1.371 (3)
C2—P2ⁱⁱ	1.8382 (15)	C27—C28	1.380 (3)
C3—P1ⁱⁱ	1.8403 (15)	C28—C29	1.384 (3)
C4—C6	1.377 (3)	C29—C30	1.364 (3)
C5—C14	1.376 (3)	C30—C31	1.370 (3)
C5—C7	1.397 (2)	C31—C32	1.384 (3)
C6—C8	1.359 (3)

N4—Cu1—O4	90.51 (6)	C8—C6—C4	118.1 (2)
N4—Cu1—P1	108.23 (4)	C9—C7—C5	120.60 (18)
O4—Cu1—P1	110.07 (3)	C10—C8—C6	119.8 (2)
N4—Cu1—P2	103.08 (4)	C11—C9—C7	120.16 (16)
O4—Cu1—P2	112.69 (3)	C8—C10—C12	119.00 (17)
P1—Cu1—P2	125.84 (2)	C9—C11—C13	120.5 (2)
C5—P1—C15	103.52 (9)	N4—C12—C10	121.90 (19)
C5—P1—C3	104.65 (11)	C11—C13—C14	120.00 (18)
C15—P1—C3	103.60 (10)	C5—C14—C13	120.36 (15)
C5—P1—Cu1	118.57 (6)	C16—C15—C20	118.1 (2)
C15—P1—Cu1	105.79 (6)	C16—C15—P1	121.91 (15)
C3—P1—Cu1	118.72 (7)	C20—C15—P1	119.12 (17)
C21—P2—C2	104.69 (10)	C15—C16—C17	120.4 (2)
C21—P2—C27	101.39 (8)	C18—C17—C16	120.8 (2)
C2—P2—C27	101.90 (9)	C17—C18—C19	120.0 (2)
C21—P2—Cu1	116.83 (7)	C18—C19—C20	120.19 (19)
C2—P2—Cu1	118.76 (8)	C19—C20—C15	120.5 (2)
C27—P2—Cu1	110.93 (6)	C26—C21—C22	119.16 (16)
N1—O4—Cu1	130.61 (12)	C26—C21—P2	121.29 (14)
O6—N1—O4	119.26 (9)	C22—C21—P2	119.55 (13)
O6—N1—O4ⁱⁱ	119.26 (9)	C21—C22—C23	118.99 (18)
O4—N1—O4ⁱⁱ	121.46 (18)	C24—C23—C22	121.1 (2)
O5—N2—O5ⁱⁱ	119.9 (2)	C23—C24—C25	120.85 (18)
O5—N2—O3	120.01 (12)	C24—C25—C26	119.36 (18)
O5ⁱⁱ—N2—O3	120.01 (12)	C21—C26—C25	120.53 (19)
C4—N4—C12	117.41 (18)	C32—C27—C28	119.11 (18)
C4—N4—Cu1	119.22 (13)	C32—C27—P2	123.18 (17)
C12—N4—Cu1	122.77 (13)	C28—C27—P2	117.57 (13)
P2ⁱⁱ—C2—P2	113.30 (14)	C27—C28—C29	119.77 (17)
P1—C3—P1ⁱⁱ	112.13 (13)	C30—C29—C28	120.6 (2)
N4—C4—C6	123.71 (17)	C29—C30—C31	120.12 (19)
C14—C5—C7	118.39 (19)	C30—C31—C32	119.40 (18)
C14—C5—P1	118.77 (14)	C27—C32—C31	121.0 (2)
C7—C5—P1	122.83 (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

C₂₂N₂O₆	γ = 90°
M_r = 388.24	V = 2174.1 (7) Å³
P2₁2₁2₁	Z = 4
a = 12.148 (2) Å	F(000) = 776
b = 8.251 (2) Å	D_x = 1.186 Mg m⁻³
c = 21.690 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 0.09 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.021
Graphite monochromator	θ_max = 32.9°, θ_min = 1.9°
12290 measured reflections	h = −12→12
3081 independent reflections	k = −8→8
3050 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.019	w = 1/[σ²(F_o²) + (0.P)² + 0.0178P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.077	(Δ/σ)_max = 0.745
S = 0.63	Δρ_max = 0.59 e Å⁻³
3081 reflections	Δρ_min = −0.58 e Å⁻³
121 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 restraints	Absolute structure parameter: 0.1 (6)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
O1	0.48470 (7)	0.01990 (11)	0.07400 (5)	0.0200 (2)*
O2	0.49230 (7)	−0.11310 (11)	−0.09220 (5)	0.0200 (2)*
O3	0.64660 (7)	0.02390 (11)	−0.16910 (5)	0.0200 (2)*
O4	0.81390 (7)	0.02970 (11)	−0.07060 (5)	0.0200 (2)*
O5	0.85960 (7)	0.04990 (11)	0.06020 (5)	0.0200 (2)*
O6	0.67100 (7)	0.04800 (11)	0.13490 (5)	0.0200 (2)*
C1	0.60760 (11)	−0.14270 (15)	0.21420 (8)	0.0200 (3)*
C2	0.52320 (10)	−0.24260 (15)	0.23560 (8)	0.0200 (3)*
C3	0.42490 (11)	−0.25420 (16)	0.20260 (7)	0.0200 (3)*
C4	0.41100 (10)	−0.16610 (16)	0.14840 (8)	0.0200 (3)*
C5	0.49550 (11)	−0.06610 (15)	0.12700 (8)	0.0200 (3)*
C6	0.59380 (10)	−0.05450 (15)	0.15990 (8)	0.0200 (3)*
C7	0.31010 (10)	−0.18380 (16)	0.11490 (8)	0.0200 (3)*
N1	0.29180 (9)	−0.10300 (13)	0.06330 (6)	0.0200 (2)*
C8	0.18870 (10)	−0.12040 (15)	0.02970 (8)	0.0200 (3)*
C9	0.19740 (10)	−0.22580 (15)	−0.02480 (8)	0.0200 (3)*
N2	0.28900 (9)	−0.16300 (13)	−0.06720 (7)	0.0200 (2)*
C10	0.26260 (11)	−0.10710 (15)	−0.11970 (8)	0.0200 (3)*
C11	0.31460 (10)	0.01900 (15)	−0.21840 (8)	0.0200 (3)*
C12	0.39290 (11)	0.08680 (15)	−0.25770 (8)	0.0200 (3)*
C13	0.50370 (11)	0.08770 (15)	−0.24090 (8)	0.0200 (3)*
C14	0.53630 (10)	0.02060 (15)	−0.18470 (8)	0.0200 (3)*
C15	0.45790 (10)	−0.04730 (16)	−0.14540 (8)	0.0200 (3)*
C16	0.34710 (10)	−0.04800 (16)	−0.16230 (8)	0.0200 (3)*
C17	0.66970 (11)	0.15400 (15)	−0.12900 (8)	0.0200 (3)*
C18	0.79130 (11)	0.16050 (15)	−0.11140 (8)	0.0200 (3)*
C19	0.92230 (10)	0.03700 (16)	−0.04360 (8)	0.0200 (3)*
C20	0.92130 (11)	0.14000 (15)	0.01580 (8)	0.0200 (3)*
C21	0.85090 (10)	0.13690 (15)	0.11630 (8)	0.0200 (3)*
C22	0.78000 (10)	0.04060 (16)	0.15820 (8)	0.0200 (3)*

Geometric parameters (Å, º) top

O1—C5	1.3573 (18)	C5—C6	1.3944 (19)
O2—C15	1.3420 (17)	C7—N1	1.322 (2)
O3—C14	1.3823 (16)	N1—C8	1.4562 (18)
O3—C17	1.4098 (18)	C8—C9	1.471 (2)
O4—C18	1.4224 (18)	C9—N2	1.5338 (18)
O4—C19	1.4425 (16)	N2—C10	1.270 (2)
O5—C21	1.4167 (19)	C10—C16	1.465 (2)
O5—C20	1.4290 (17)	C11—C16	1.394 (2)
O6—C6	1.3743 (16)	C11—C12	1.394 (2)
O6—C22	1.4186 (16)	C12—C13	1.3945 (19)
C1—C6	1.395 (2)	C13—C14	1.396 (2)
C1—C2	1.3950 (18)	C14—C15	1.396 (2)
C2—C3	1.396 (2)	C15—C16	1.3950 (19)
C3—C4	1.392 (2)	C17—C18	1.5267 (19)
C4—C5	1.3964 (18)	C19—C20	1.543 (2)
C4—C7	1.4324 (18)	C21—C22	1.483 (2)

C14—O3—C17	111.04 (11)	C10—N2—C9	118.50 (11)
C18—O4—C19	113.40 (10)	N2—C10—C16	120.64 (12)
C21—O5—C20	110.75 (10)	C16—C11—C12	119.98 (12)
C6—O6—C22	118.03 (11)	C11—C12—C13	120.06 (15)
C6—C1—C2	120.07 (13)	C12—C13—C14	119.99 (14)
C1—C2—C3	119.92 (15)	O3—C14—C15	121.33 (13)
C4—C3—C2	120.07 (12)	O3—C14—C13	118.74 (13)
C3—C4—C5	120.00 (13)	C15—C14—C13	119.93 (12)
C3—C4—C7	118.61 (12)	O2—C15—C16	121.65 (13)
C5—C4—C7	121.38 (15)	O2—C15—C14	118.37 (12)
O1—C5—C6	118.71 (12)	C16—C15—C14	119.98 (14)
O1—C5—C4	121.29 (12)	C11—C16—C15	120.07 (14)
C6—C5—C4	120.00 (15)	C11—C16—C10	118.97 (12)
O6—C6—C5	115.13 (14)	C15—C16—C10	120.79 (15)
O6—C6—C1	124.91 (12)	O3—C17—C18	111.94 (11)
C5—C6—C1	119.96 (12)	O4—C18—C17	108.40 (11)
N1—C7—C4	121.47 (12)	O4—C19—C20	110.78 (10)
C7—N1—C8	121.25 (11)	O5—C20—C19	106.27 (10)
N1—C8—C9	113.49 (11)	O5—C21—C22	107.35 (11)
C8—C9—N2	109.52 (10)	O6—C22—C21	107.50 (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

C₂₂H₂₆N₂O₆	γ = 90°
M_r = 414.45	V = 2174.1 (7) Å³
P2₁2₁2₁	Z = 4
a = 12.148 (2) Å	F(000) = 880
b = 8.251 (2) Å	D_x = 1.266 Mg m⁻³
c = 21.690 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 0.09 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.022
Graphite monochromator	θ_max = 30.5°, θ_min = 1.9°
10320 measured reflections	h = −10→10
2588 independent reflections	k = −8→8
2565 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.019	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.081	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.51	(Δ/σ)_max = 9.439
2588 reflections	Δρ_max = 0.07 e Å⁻³
217 parameters	Δρ_min = −0.29 e Å⁻³
0 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.0 (7)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
O1	0.48390 (8)	0.01970 (12)	0.07450 (6)	0.0200 (2)*
O2	0.49260 (9)	−0.11210 (11)	−0.09210 (6)	0.0200 (2)*
O3	0.64640 (9)	0.02470 (11)	−0.16880 (6)	0.0200 (2)*
O4	0.81450 (9)	0.02870 (12)	−0.07080 (6)	0.0200 (2)*
O5	0.86010 (9)	0.05030 (12)	0.06020 (6)	0.0200 (2)*
O6	0.67050 (9)	0.04680 (12)	0.13530 (6)	0.0200 (3)*
C1	0.60720 (15)	−0.14240 (16)	0.21400 (9)	0.0200 (3)*
H1	0.6733 (16)	−0.135 (2)	0.2359 (9)	0.020 (5)*
C2	0.52340 (13)	−0.24270 (17)	0.23510 (10)	0.0200 (3)*
H2	0.5334 (15)	−0.302 (2)	0.2712 (9)	0.020 (4)*
C3	0.42550 (14)	−0.25450 (17)	0.20230 (9)	0.0200 (3)*
H3	0.3697 (14)	−0.322 (2)	0.2164 (8)	0.020 (4)*
C4	0.41140 (12)	−0.16610 (17)	0.14830 (9)	0.0200 (3)*
C5	0.49520 (13)	−0.06580 (17)	0.12720 (9)	0.0200 (3)*
C6	0.59320 (13)	−0.05400 (17)	0.16000 (9)	0.0200 (3)*
C7	0.30960 (13)	−0.18270 (18)	0.11430 (9)	0.0200 (3)*
H4	0.2553 (15)	−0.2519 (19)	0.1292 (9)	0.020 (4)*
N1	0.29210 (11)	−0.10370 (14)	0.06340 (7)	0.0200 (3)*
C8	0.18920 (14)	−0.12110 (17)	0.02990 (9)	0.0200 (3)*
H5	0.1639 (13)	−0.014 (2)	0.0176 (9)	0.020 (4)*
H6	0.1343 (14)	−0.167 (2)	0.0573 (9)	0.020 (4)*
C9	0.19760 (14)	−0.22340 (17)	−0.02510 (9)	0.0200 (3)*
H7	0.1279 (14)	−0.223 (2)	−0.0469 (9)	0.020 (4)*
H8	0.2134 (14)	−0.334 (2)	−0.0129 (9)	0.020 (4)*
N2	0.28830 (11)	−0.16210 (14)	−0.06770 (7)	0.0200 (3)*
C10	0.26340 (15)	−0.10710 (16)	−0.11960 (9)	0.0200 (3)*
H9	0.1897 (15)	−0.103 (2)	−0.1313 (8)	0.020 (4)*
C11	0.31490 (14)	0.01820 (16)	−0.21840 (8)	0.0200 (3)*
H10	0.2411 (15)	0.017 (2)	−0.2296 (8)	0.020 (4)*
C12	0.39270 (14)	0.08580 (17)	−0.25770 (10)	0.0200 (3)*
H11	0.3709 (14)	0.130 (2)	−0.2951 (9)	0.020 (5)*
C13	0.50330 (14)	0.08720 (16)	−0.24110 (10)	0.0200 (3)*
H12	0.5553 (15)	0.1324 (19)	−0.2673 (9)	0.020 (4)*
C14	0.53590 (13)	0.02070 (17)	−0.18500 (9)	0.0200 (3)*
C15	0.45810 (12)	−0.04700 (17)	−0.14580 (9)	0.0200 (3)*
C16	0.34760 (13)	−0.04830 (16)	−0.16250 (9)	0.0200 (3)*
C17	0.67020 (14)	0.15330 (16)	−0.12810 (10)	0.0200 (3)*
H13	0.6266 (15)	0.141 (2)	−0.0909 (9)	0.020 (5)*
H14	0.6502 (14)	0.255 (2)	−0.1473 (9)	0.020 (5)*
C18	0.79020 (14)	0.15600 (17)	−0.11150 (10)	0.0200 (4)*
H15	0.8343 (15)	0.1452 (19)	−0.1486 (9)	0.020 (4)*
H16	0.8083 (14)	0.259 (2)	−0.0923 (9)	0.020 (4)*
C19	0.92040 (13)	0.03910 (18)	−0.04390 (9)	0.0200 (3)*
H17	0.9703 (14)	0.090 (2)	−0.0731 (9)	0.020 (4)*
H18	0.9473 (13)	−0.070 (2)	−0.0358 (9)	0.020 (4)*
C20	0.92250 (14)	0.13510 (17)	0.01590 (9)	0.0200 (3)*
H19	0.9976 (16)	0.1479 (19)	0.0301 (9)	0.020 (4)*
H20	0.8913 (14)	0.242 (2)	0.0093 (9)	0.020 (4)*
C21	0.85170 (14)	0.13710 (17)	0.11730 (9)	0.0200 (3)*
H21	0.8200 (14)	0.244 (2)	0.1105 (9)	0.020 (4)*
H22	0.9240 (15)	0.1507 (19)	0.1357 (8)	0.020 (5)*
C22	0.78060 (13)	0.04180 (17)	0.15860 (10)	0.0200 (3)*
H23	0.8062 (14)	−0.070 (2)	0.1602 (9)	0.020 (4)*
H24	0.7828 (14)	0.086 (2)	0.1999 (9)	0.020 (4)*

Geometric parameters (Å, º) top

O1—C5	1.350 (2)	C5—C6	1.390 (2)
O2—C15	1.349 (2)	C7—N1	1.300 (2)
O3—C14	1.388 (2)	N1—C8	1.453 (2)
O3—C17	1.4102 (19)	C8—C9	1.465 (2)
O4—C18	1.403 (2)	C9—N2	1.524 (2)
O4—C19	1.415 (2)	N2—C10	1.251 (2)
O5—C20	1.410 (2)	C10—C16	1.465 (2)
O5—C21	1.434 (2)	C11—C16	1.389 (3)
O6—C6	1.3640 (18)	C11—C12	1.390 (2)
O6—C22	1.430 (2)	C12—C13	1.391 (3)
C1—C2	1.389 (2)	C13—C14	1.392 (3)
C1—C6	1.390 (2)	C14—C15	1.389 (2)
C2—C3	1.389 (3)	C15—C16	1.390 (2)
C3—C4	1.390 (2)	C17—C18	1.502 (3)
C4—C5	1.389 (2)	C19—C20	1.520 (3)
C4—C7	1.446 (2)	C21—C22	1.472 (2)

C14—O3—C17	112.00 (12)	C10—N2—C9	119.41 (14)
C18—O4—C19	113.90 (12)	N2—C10—C16	121.52 (16)
C20—O5—C21	112.27 (12)	C16—C11—C12	119.97 (17)
C6—O6—C22	119.17 (13)	C11—C12—C13	120.1 (2)
C2—C1—C6	120.02 (17)	C12—C13—C14	119.85 (18)
C3—C2—C1	120.02 (18)	O3—C14—C15	120.85 (16)
C2—C3—C4	120.01 (15)	O3—C14—C13	119.14 (15)
C5—C4—C3	119.98 (16)	C15—C14—C13	120.00 (16)
C5—C4—C7	120.99 (16)	O2—C15—C14	118.51 (15)
C3—C4—C7	119.02 (14)	O2—C15—C16	121.44 (15)
O1—C5—C4	121.03 (15)	C14—C15—C16	120.05 (17)
O1—C5—C6	118.93 (14)	C11—C16—C15	120.03 (15)
C4—C5—C6	120.04 (17)	C11—C16—C10	119.04 (15)
O6—C6—C1	124.51 (16)	C15—C16—C10	120.73 (17)
O6—C6—C5	115.55 (16)	O3—C17—C18	111.12 (14)
C1—C6—C5	119.94 (15)	O4—C18—C17	110.11 (14)
N1—C7—C4	121.70 (14)	O4—C19—C20	113.49 (13)
C7—N1—C8	121.06 (13)	O5—C20—C19	108.30 (13)
N1—C8—C9	113.84 (13)	O5—C21—C22	107.49 (13)
C8—C9—N2	110.66 (13)	O6—C22—C21	108.56 (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·H₂O	γ = 90°
M_r = 698.27	V = 3040.2 (7) Å³
P2₁2₁2₁	Z = 4
a = 6.6179 (7) Å	F(000) = 1400
b = 12.924 (2) Å	D_x = 1.526 Mg m⁻³
c = 35.545 (5) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 1.38 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.028
Graphite monochromator	θ_max = 26.9°, θ_min = 1.2°
8976 measured reflections	h = −6→6
2252 independent reflections	k = −10→10
2240 reflections with I > 2σ(I)	l = −16→16

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.007	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.042	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.36	(Δ/σ)_max = 3.897
2252 reflections	Δρ_max = 0.16 e Å⁻³
269 parameters	Δρ_min = −0.22 e Å⁻³
0 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.015 (19)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pd1	0.29800 (3)	0.327500 (18)	0.203400 (10)	0.02000 (8)*
Pd2	0.62320 (3)	0.435800 (18)	0.137300 (11)	0.02000 (8)*
Cl1	0.53520 (9)	0.46130 (6)	0.20440 (4)	0.02000 (18)*
Cl2	0.44690 (9)	0.27970 (6)	0.14200 (4)	0.02000 (17)*
O1	0.6635 (3)	0.25870 (16)	0.46260 (9)	0.0200 (5)*
N1	0.0719 (3)	0.2168 (2)	0.20540 (12)	0.0200 (6)*
N2	0.7921 (4)	0.56950 (19)	0.13160 (10)	0.0200 (6)*
C1	0.1918 (4)	0.3544 (2)	0.25390 (13)	0.0200 (7)*
C2	0.3020 (4)	0.3999 (2)	0.28330 (13)	0.0200 (6)*
C3	0.2210 (4)	0.4127 (2)	0.31880 (13)	0.0200 (7)*
C4	0.3265 (4)	0.4588 (2)	0.35060 (14)	0.0200 (7)*
C5	0.2514 (4)	0.4669 (2)	0.38340 (15)	0.0200 (8)*
C6	0.0561 (4)	0.4322 (2)	0.38980 (17)	0.0200 (7)*
C7	−0.0630 (4)	0.3890 (2)	0.36320 (15)	0.0200 (7)*
C8	0.0157 (4)	0.3745 (2)	0.32560 (16)	0.0200 (7)*
C9	−0.0837 (4)	0.3272 (2)	0.29590 (14)	0.0200 (7)*
C10	0.0042 (4)	0.3142 (2)	0.26140 (14)	0.0200 (7)*
C11	−0.0981 (4)	0.2609 (2)	0.22890 (14)	0.0200 (7)*
C12	−0.2628 (4)	0.1856 (3)	0.23910 (17)	0.0200 (7)*
C13	0.1561 (4)	0.1202 (3)	0.22180 (16)	0.0200 (7)*
C14	−0.0049 (4)	0.1912 (3)	0.16700 (15)	0.0200 (8)*
C15	0.6715 (4)	0.4245 (2)	0.08220 (14)	0.0200 (7)*
C16	0.5654 (4)	0.3708 (2)	0.05660 (16)	0.0200 (7)*
C17	0.6130 (4)	0.3772 (2)	0.01770 (15)	0.0200 (7)*
C18	0.5025 (4)	0.3228 (2)	−0.00960 (16)	0.0200 (7)*
C19	0.5571 (4)	0.3209 (2)	−0.04580 (17)	0.0200 (7)*
C20	0.7217 (4)	0.3776 (2)	−0.05780 (16)	0.0200 (7)*
C21	0.8260 (4)	0.4355 (2)	−0.03310 (15)	0.0200 (7)*
C22	0.7743 (4)	0.4390 (2)	0.00630 (15)	0.0200 (7)*
C23	0.8734 (4)	0.4975 (2)	0.03260 (16)	0.0200 (7)*
C24	0.8293 (4)	0.4925 (2)	0.07010 (16)	0.0200 (7)*
C25	0.9425 (4)	0.5525 (3)	0.10030 (15)	0.0200 (7)*
C26	1.1223 (5)	0.4905 (3)	0.11230 (16)	0.0200 (7)*
C27	0.6534 (4)	0.6546 (3)	0.11920 (16)	0.0200 (8)*
C28	0.8932 (5)	0.6028 (2)	0.16710 (14)	0.0200 (7)*
H1	0.433 (4)	0.422 (2)	0.2787 (11)	0.020 (9)*
H2	0.457 (5)	0.484 (2)	0.3467 (11)	0.020 (9)*
H3	0.327 (5)	0.496 (2)	0.4029 (12)	0.020 (9)*
H4	0.004 (5)	0.440 (2)	0.4139 (12)	0.020 (9)*
H5	−0.194 (5)	0.369 (2)	0.3690 (11)	0.020 (8)*
H6	−0.215 (4)	0.303 (2)	0.2995 (11)	0.020 (8)*
H7	−0.161 (4)	0.315 (2)	0.2138 (11)	0.020 (9)*
H8	−0.318 (5)	0.156 (2)	0.2166 (12)	0.020 (9)*
H9	−0.368 (5)	0.221 (2)	0.2525 (11)	0.020 (8)*
H10	−0.208 (4)	0.132 (2)	0.2547 (11)	0.020 (8)*
H11	0.262 (5)	0.095 (2)	0.2061 (12)	0.020 (9)*
H12	0.051 (4)	0.069 (2)	0.2236 (11)	0.020 (9)*
H13	0.209 (5)	0.134 (2)	0.2465 (13)	0.020 (9)*
H14	−0.060 (4)	0.252 (3)	0.1556 (12)	0.020 (9)*
H15	−0.108 (5)	0.139 (2)	0.1688 (11)	0.020 (8)*
H16	0.104 (4)	0.166 (2)	0.1518 (12)	0.020 (8)*
H17	0.459 (4)	0.329 (2)	0.0644 (11)	0.020 (9)*
H18	0.387 (4)	0.287 (2)	−0.0022 (12)	0.020 (8)*
H19	0.484 (4)	0.281 (2)	−0.0629 (11)	0.020 (9)*
H20	0.760 (5)	0.376 (2)	−0.0829 (12)	0.020 (10)*
H21	0.935 (4)	0.475 (2)	−0.0417 (12)	0.020 (9)*
H22	0.975 (4)	0.542 (2)	0.0247 (11)	0.020 (9)*
H23	0.987 (4)	0.619 (3)	0.0902 (12)	0.020 (9)*
H24	1.195 (5)	0.528 (2)	0.1313 (11)	0.020 (8)*
H25	1.209 (5)	0.479 (2)	0.0911 (12)	0.020 (9)*
H26	1.078 (4)	0.425 (2)	0.1222 (11)	0.020 (8)*
H27	0.556 (5)	0.668 (2)	0.1385 (13)	0.020 (8)*
H28	0.585 (5)	0.634 (2)	0.0965 (14)	0.020 (9)*
H29	0.730 (4)	0.716 (2)	0.1146 (11)	0.020 (9)*
H30	0.793 (5)	0.616 (2)	0.1860 (12)	0.020 (9)*
H31	0.968 (4)	0.665 (2)	0.1626 (11)	0.020 (9)*
H32	0.983 (4)	0.549 (2)	0.1755 (12)	0.020 (9)*

Geometric parameters (Å, º) top

Pd1—C1	1.959 (4)	C12—H10	0.96 (3)
Pd1—N1	2.071 (2)	C13—H11	0.96 (3)
Pd1—Cl1	2.3357 (7)	C13—H12	0.96 (3)
Pd1—Cl2	2.4730 (12)	C13—H13	0.96 (4)
Pd2—C15	1.990 (5)	C14—H14	0.96 (3)
Pd2—N2	2.068 (2)	C14—H15	0.96 (3)
Pd2—Cl2	2.3365 (8)	C14—H16	0.96 (3)
Pd2—Cl1	2.4772 (13)	C15—C16	1.343 (6)
N1—C13	1.486 (5)	C15—C24	1.431 (4)
N1—C14	1.494 (6)	C16—C17	1.421 (6)
N1—C11	1.513 (4)	C16—H17	0.93 (3)
N2—C28	1.492 (5)	C17—C22	1.393 (4)
N2—C27	1.499 (4)	C17—C18	1.404 (6)
N2—C25	1.509 (5)	C18—C19	1.337 (6)
C1—C10	1.372 (4)	C18—H18	0.93 (3)
C1—C2	1.403 (6)	C19—C20	1.380 (5)
C2—C3	1.381 (6)	C19—H19	0.93 (3)
C2—H1	0.93 (3)	C20—C21	1.344 (6)
C3—C4	1.456 (6)	C20—H20	0.93 (4)
C3—C8	1.466 (4)	C21—C22	1.442 (5)
C4—C5	1.272 (6)	C21—H21	0.93 (3)
C4—H2	0.93 (3)	C22—C23	1.370 (6)
C5—C6	1.387 (4)	C23—C24	1.366 (6)
C5—H3	0.93 (4)	C23—H22	0.93 (3)
C6—C7	1.352 (6)	C24—C25	1.521 (6)
C6—H4	0.93 (4)	C25—C26	1.497 (4)
C7—C8	1.447 (7)	C25—H23	0.98 (3)
C7—H5	0.93 (3)	C26—H24	0.96 (4)
C8—C9	1.386 (6)	C26—H25	0.96 (4)
C9—C10	1.368 (6)	C26—H26	0.96 (3)
C9—H6	0.93 (3)	C27—H27	0.96 (4)
C10—C11	1.506 (6)	C27—H28	0.96 (4)
C11—C12	1.506 (4)	C27—H29	0.96 (3)
C11—H7	0.98 (3)	C28—H30	0.96 (4)
C12—H8	0.96 (4)	C28—H31	0.96 (3)
C12—H9	0.96 (3)	C28—H32	0.96 (3)

C1—Pd1—N1	80.33 (14)	H9—C12—H10	110 (3)
C1—Pd1—Cl1	95.50 (9)	N1—C13—H11	110 (2)
N1—Pd1—Cl1	175.05 (9)	N1—C13—H12	109.4 (19)
C1—Pd1—Cl2	174.89 (10)	H11—C13—H12	110 (3)
N1—Pd1—Cl2	98.37 (11)	N1—C13—H13	109.4 (19)
Cl1—Pd1—Cl2	86.02 (3)	H11—C13—H13	109 (3)
C15—Pd2—N2	83.00 (13)	H12—C13—H13	109 (3)
C15—Pd2—Cl2	95.00 (9)	N1—C14—H14	109 (2)
N2—Pd2—Cl2	176.77 (8)	N1—C14—H15	110 (2)
C15—Pd2—Cl1	174.40 (9)	H14—C14—H15	109 (3)
N2—Pd2—Cl1	96.33 (10)	N1—C14—H16	109 (2)
Cl2—Pd2—Cl1	85.91 (3)	H14—C14—H16	109 (3)
Pd1—Cl1—Pd2	92.57 (4)	H15—C14—H16	109 (3)
Pd2—Cl2—Pd1	92.66 (4)	C16—C15—C24	119.7 (5)
C13—N1—C14	107.5 (3)	C16—C15—Pd2	128.4 (3)
C13—N1—C11	112.3 (3)	C24—C15—Pd2	111.6 (3)
C14—N1—C11	109.6 (2)	C15—C16—C17	120.9 (4)
C13—N1—Pd1	108.83 (17)	C15—C16—H17	120 (3)
C14—N1—Pd1	111.6 (2)	C17—C16—H17	119 (3)
C11—N1—Pd1	107.21 (18)	C22—C17—C18	119.0 (5)
C28—N2—C27	108.2 (3)	C22—C17—C16	119.1 (4)
C28—N2—C25	111.7 (2)	C18—C17—C16	121.9 (3)
C27—N2—C25	107.1 (3)	C19—C18—C17	122.3 (4)
C28—N2—Pd2	113.6 (2)	C19—C18—H18	119 (3)
C27—N2—Pd2	108.12 (18)	C17—C18—H18	119 (3)
C25—N2—Pd2	107.89 (19)	C18—C19—C20	120.1 (4)
C10—C1—C2	119.0 (4)	C18—C19—H19	120 (2)
C10—C1—Pd1	115.8 (3)	C20—C19—H19	120 (2)
C2—C1—Pd1	124.8 (2)	C21—C20—C19	119.9 (5)
C3—C2—C1	121.9 (3)	C21—C20—H20	119.9 (18)
C3—C2—H1	119 (2)	C19—C20—H20	120.1 (19)
C1—C2—H1	119 (2)	C20—C21—C22	122.0 (4)
C2—C3—C4	124.9 (3)	C20—C21—H21	119 (3)
C2—C3—C8	118.0 (4)	C22—C21—H21	119 (2)
C4—C3—C8	117.0 (4)	C23—C22—C17	119.0 (5)
C5—C4—C3	123.9 (3)	C23—C22—C21	124.5 (3)
C5—C4—H2	118 (3)	C17—C22—C21	116.5 (4)
C3—C4—H2	118 (3)	C24—C23—C22	122.5 (3)
C4—C5—C6	119.2 (5)	C24—C23—H22	119 (2)
C4—C5—H3	120 (2)	C22—C23—H22	119 (2)
C6—C5—H3	120 (2)	C23—C24—C15	118.6 (4)
C7—C6—C5	124.2 (5)	C23—C24—C25	124.0 (3)
C7—C6—H4	118.0 (19)	C15—C24—C25	117.4 (5)
C5—C6—H4	118 (2)	C26—C25—N2	113.1 (4)
C6—C7—C8	119.3 (3)	C26—C25—C24	108.6 (3)
C6—C7—H5	120 (3)	N2—C25—C24	105.6 (2)
C8—C7—H5	120 (2)	C26—C25—H23	109.8 (17)
C9—C8—C7	126.2 (3)	N2—C25—H23	110 (2)
C9—C8—C3	117.6 (5)	C24—C25—H23	110 (2)
C7—C8—C3	116.3 (4)	C25—C26—H24	109.4 (18)
C10—C9—C8	122.4 (3)	C25—C26—H25	110 (2)
C10—C9—H6	119 (2)	H24—C26—H25	109 (3)
C8—C9—H6	119 (2)	C25—C26—H26	109.6 (17)
C9—C10—C1	120.8 (4)	H24—C26—H26	110 (3)
C9—C10—C11	123.6 (3)	H25—C26—H26	109 (2)
C1—C10—C11	115.5 (4)	N2—C27—H27	109 (2)
C12—C11—C10	115.9 (4)	N2—C27—H28	109.6 (18)
C12—C11—N1	115.3 (3)	H27—C27—H28	109 (3)
C10—C11—N1	105.2 (2)	N2—C27—H29	109.4 (17)
C12—C11—H7	106.6 (17)	H27—C27—H29	109 (3)
C10—C11—H7	107 (2)	H28—C27—H29	109 (3)
N1—C11—H7	107 (2)	N2—C28—H30	109 (2)
C11—C12—H8	110 (2)	N2—C28—H31	109 (2)
C11—C12—H9	109.5 (18)	H30—C28—H31	109 (3)
H8—C12—H9	109 (3)	N2—C28—H32	110 (2)
C11—C12—H10	109.5 (18)	H30—C28—H32	110 (3)
H8—C12—H10	109 (3)	H31—C28—H32	109 (2)

(aplsol) top

Crystal data top

C₁₅BrO₂	γ = 90°
M_r = 292.06	V = 1383.7 (10) Å³
P4₃	Z = 4
a = 13.750 (5) Å	F(000) = 564
b = 13.750 (5) Å	D_x = 1.402 Mg m⁻³
c = 7.319 (4) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 2.96 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.053
Graphite monochromator	θ_max = 47.1°, θ_min = 1.5°
20164 measured reflections	h = −15→15
5044 independent reflections	k = −15→15
4914 reflections with I > 2σ(I)	l = −10→10

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.009	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.050	(Δ/σ)_max = 0.261
S = 0.31	Δρ_max = 0.41 e Å⁻³
5044 reflections	Δρ_min = −0.41 e Å⁻³
73 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
1 restraint	Absolute structure parameter: 0.015 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Br1	0.889000 (6)	0.835000 (6)	0.499500 (15)	0.02000 (2)*
O4	0.78510 (5)	0.53550 (5)	−0.05260 (9)	0.02000 (10)*
O11	0.59220 (5)	0.45900 (5)	0.01880 (9)	0.02000 (10)*
C1	0.87600 (6)	0.41500 (7)	0.32000 (11)	0.02000 (12)*
C2	0.93450 (7)	0.39800 (7)	0.14500 (11)	0.02000 (12)*
C3	0.85700 (6)	0.37750 (6)	0.00900 (12)	0.02000 (12)*
C13	0.77000 (7)	0.44650 (7)	0.04250 (10)	0.02000 (13)*
C4	0.81100 (7)	0.60800 (7)	0.05750 (11)	0.02000 (12)*
C5	0.83300 (6)	0.70200 (6)	0.00850 (12)	0.02000 (12)*
C6	0.85750 (7)	0.77150 (7)	0.13450 (11)	0.02000 (12)*
C7	0.85500 (7)	0.74450 (6)	0.31800 (11)	0.02000 (12)*
C8	0.83200 (7)	0.64800 (7)	0.37700 (11)	0.02000 (12)*
C18	0.80750 (6)	0.58100 (6)	0.25200 (12)	0.02000 (11)*
C28	0.78500 (6)	0.47400 (6)	0.26400 (11)	0.02000 (12)*
C9	0.89200 (7)	0.38000 (7)	−0.19600 (11)	0.02000 (12)*
C10	0.67600 (6)	0.40250 (7)	−0.00650 (12)	0.02000 (12)*
C12	0.87550 (7)	0.87700 (7)	0.08550 (11)	0.02000 (12)*
C31	0.70000 (7)	0.45700 (7)	0.38600 (11)	0.02000 (13)*

Geometric parameters (Å, º) top

Br1—C7	1.8793 (11)	C13—C28	1.6774 (14)
O4—C4	1.3304 (12)	C4—C5	1.3750 (13)
O4—C13	1.4231 (12)	C4—C18	1.4719 (14)
O11—C10	1.4020 (11)	C5—C6	1.3701 (13)
C1—C2	1.5304 (13)	C6—C7	1.3938 (14)
C1—C28	1.5465 (13)	C6—C12	1.5147 (13)
C2—C3	1.4852 (13)	C7—C8	1.4308 (13)
C3—C13	1.5464 (14)	C8—C18	1.3413 (13)
C3—C9	1.5761 (14)	C18—C28	1.5060 (13)
C13—C10	1.4715 (14)	C28—C31	1.4893 (13)

C4—O4—C13	112.78 (8)	C5—C6—C12	123.29 (8)
C2—C1—C28	106.47 (7)	C7—C6—C12	119.16 (8)
C3—C2—C1	102.29 (8)	C6—C7—C8	122.91 (8)
C2—C3—C13	109.41 (7)	C6—C7—Br1	119.91 (7)
C2—C3—C9	114.51 (8)	C8—C7—Br1	117.11 (7)
C13—C3—C9	111.95 (7)	C18—C8—C7	119.12 (8)
O4—C13—C10	111.25 (7)	C8—C18—C4	118.57 (8)
O4—C13—C3	109.71 (7)	C8—C18—C28	133.06 (8)
C10—C13—C3	112.87 (7)	C4—C18—C28	108.03 (7)
O4—C13—C28	105.12 (7)	C31—C28—C18	110.46 (7)
C10—C13—C28	115.86 (7)	C31—C28—C1	113.19 (7)
C3—C13—C28	101.33 (7)	C18—C28—C1	111.21 (7)
O4—C4—C5	127.25 (8)	C31—C28—C13	116.59 (8)
O4—C4—C18	112.83 (8)	C18—C28—C13	100.90 (7)
C5—C4—C18	119.77 (8)	C1—C28—C13	103.73 (7)
C6—C5—C4	122.29 (8)	O11—C10—C13	117.51 (8)
C5—C6—C7	117.18 (9)

(doqzak) (2-Hydroxyethanolato)-oxo-(N-(1-oxy-2-methylprop-2-yl)-2-oxy-1-naphthaldimato)- -vanadium(v) top

Crystal data top

C₁₇H₂₀NO₅V	γ = 90°
M_r = 369.28	V = 1720 (2) Å³
P4₃	Z = 4
a = 9.717 (8) Å	F(000) = 768
b = 9.717 (8) Å	D_x = 1.426 Mg m⁻³
c = 18.217 (9) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 0.60 mm⁻¹
β = 90°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.014
Graphite monochromator	θ_max = 45.5°, θ_min = 2.1°
23096 measured reflections	h = −12→12
5780 independent reflections	k = −12→12
5762 reflections with I > 2σ(I)	l = −18→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.008	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.031	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.18	(Δ/σ)_max = 1.238
5780 reflections	Δρ_max = 0.07 e Å⁻³
177 parameters	Δρ_min = −0.17 e Å⁻³
1 restraint	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.009 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
V1	0.069400 (6)	0.780500 (6)	0.904700 (4)	0.02000 (2)*
O1	−0.01470 (3)	0.66230 (3)	0.944000 (18)	0.02000 (4)*
O2	0.24500 (3)	0.72300 (3)	0.919600 (17)	0.02000 (4)*
O3	−0.07580 (3)	0.85510 (3)	0.848100 (18)	0.02000 (4)*
O4	0.18240 (3)	0.97420 (3)	0.855800 (19)	0.02000 (4)*
H36	0.1440 (7)	0.9987 (7)	0.8064 (4)	0.0200 (14)*
O5	0.06890 (3)	0.90760 (3)	0.979400 (18)	0.02000 (5)*
N1	0.11340 (3)	0.67980 (3)	0.80530 (2)	0.02000 (5)*
C1	0.33160 (4)	0.69930 (4)	0.85840 (2)	0.02000 (5)*
H1	0.4213 (7)	0.6660 (7)	0.8702 (4)	0.0200 (14)*
H2	0.3473 (7)	0.7872 (7)	0.8361 (4)	0.0200 (14)*
C2	0.25340 (4)	0.61560 (3)	0.80370 (2)	0.02000 (5)*
C3	0.03330 (3)	0.65850 (3)	0.75130 (2)	0.02000 (5)*
H37	0.0625 (7)	0.5958 (7)	0.7088 (4)	0.0200 (15)*
C4	−0.10290 (4)	0.71460 (3)	0.74200 (2)	0.02000 (5)*
C5	−0.14500 (3)	0.81670 (3)	0.79040 (2)	0.02000 (5)*
C6	−0.27200 (4)	0.88860 (3)	0.77550 (2)	0.02000 (5)*
H3	−0.3037 (7)	0.9552 (7)	0.8081 (4)	0.0200 (14)*
C7	−0.34410 (3)	0.85950 (3)	0.71490 (2)	0.02000 (5)*
H4	−0.4225 (7)	0.9111 (7)	0.7050 (4)	0.0200 (15)*
C8	−0.38570 (3)	0.72790 (3)	0.60060 (2)	0.02000 (5)*
H5	−0.4632 (7)	0.7805 (7)	0.5901 (4)	0.0200 (14)*
C9	−0.34860 (4)	0.63010 (3)	0.55650 (2)	0.02000 (5)*
H6	−0.4015 (7)	0.6141 (7)	0.5148 (4)	0.0200 (14)*
C10	−0.23600 (3)	0.54940 (4)	0.56820 (3)	0.02000 (5)*
H7	−0.2131 (7)	0.4802 (7)	0.5351 (4)	0.0200 (14)*
C11	−0.15530 (3)	0.57210 (3)	0.63060 (2)	0.02000 (5)*
H8	−0.0800 (6)	0.5156 (7)	0.6399 (4)	0.0200 (15)*
C12	−0.18600 (3)	0.67770 (4)	0.67910 (2)	0.02000 (6)*
C13	−0.30710 (3)	0.75510 (4)	0.66590 (2)	0.02000 (5)*
C14	0.23600 (3)	0.46700 (4)	0.82990 (2)	0.02000 (5)*
H9	0.1855 (7)	0.4156 (7)	0.7939 (4)	0.0200 (14)*
H10	0.1866 (7)	0.4662 (7)	0.8756 (4)	0.0200 (14)*
H11	0.3249 (7)	0.4259 (7)	0.8369 (4)	0.0200 (14)*
C15	0.32350 (3)	0.62830 (3)	0.72900 (2)	0.02000 (5)*
H12	0.2740 (7)	0.5748 (7)	0.6935 (4)	0.0200 (14)*
H13	0.4163 (7)	0.5950 (7)	0.7325 (4)	0.0200 (14)*
H14	0.3244 (7)	0.7230 (7)	0.7141 (4)	0.0200 (14)*
C16	0.15860 (3)	1.08410 (3)	0.90740 (2)	0.02000 (5)*
H15	0.2260 (7)	1.1574 (7)	0.9042 (4)	0.0200 (14)*
H16	0.0696 (7)	1.1241 (7)	0.8981 (4)	0.0200 (14)*
C17	0.15710 (3)	1.02080 (4)	0.97930 (2)	0.02000 (6)*
H17	0.2494 (7)	0.9914 (7)	0.9923 (4)	0.0200 (14)*
H18	0.1267 (7)	1.0872 (7)	1.0156 (4)	0.0200 (14)*

Geometric parameters (Å, º) top

V1—O1	1.5810 (11)	C6—H3	0.931 (7)
V1—O2	1.8159 (15)	C7—C13	1.3983 (9)
V1—O5	1.8377 (9)	C7—H4	0.930 (7)
V1—O3	1.8919 (12)	C8—C9	1.2956 (9)
V1—N1	2.1022 (10)	C8—C13	1.4381 (8)
V1—O4	2.3541 (17)	C8—H5	0.930 (7)
O2—C1	1.4157 (8)	C9—C10	1.3629 (12)
O3—C5	1.3024 (7)	C9—H6	0.930 (7)
O4—C16	1.4413 (9)	C10—C11	1.3985 (8)
O4—H36	1.003 (8)	C10—H7	0.930 (7)
O5—C17	1.3944 (12)	C11—C12	1.3866 (9)
N1—C3	1.2714 (8)	C11—H8	0.930 (6)
N1—C2	1.4969 (13)	C12—C13	1.4171 (12)
C1—C2	1.4939 (9)	C14—H9	0.959 (7)
C1—H1	0.954 (7)	C14—H10	0.961 (7)
C1—H2	0.958 (7)	C14—H11	0.960 (7)
C2—C15	1.5268 (9)	C15—H12	0.959 (7)
C2—C14	1.5302 (12)	C15—H13	0.960 (7)
C3—C4	1.4413 (13)	C15—H14	0.959 (7)
C3—H37	1.025 (7)	C16—C17	1.4471 (9)
C4—C5	1.3889 (9)	C16—H15	0.969 (6)
C4—C12	1.4469 (9)	C16—H16	0.963 (7)
C5—C6	1.4438 (12)	C17—H17	0.971 (7)
C6—C7	1.3377 (8)	C17—H18	0.970 (7)

O1—V1—O2	101.215 (17)	C5—C6—H3	120.0 (4)
O1—V1—O5	98.72 (5)	C6—C7—C13	123.06 (4)
O2—V1—O5	95.66 (2)	C6—C7—H4	118.4 (5)
O1—V1—O3	98.03 (3)	C13—C7—H4	118.6 (5)
O2—V1—O3	154.18 (2)	C9—C8—C13	120.00 (5)
O5—V1—O3	98.29 (4)	C9—C8—H5	120.1 (5)
O1—V1—N1	99.03 (4)	C13—C8—H5	119.9 (5)
O2—V1—N1	78.14 (3)	C8—C9—C10	123.26 (5)
O5—V1—N1	162.028 (15)	C8—C9—H6	118.4 (4)
O3—V1—N1	81.99 (5)	C10—C9—H6	118.4 (4)
O1—V1—O4	173.358 (14)	C9—C10—C11	119.11 (4)
O2—V1—O4	82.200 (14)	C9—C10—H7	120.4 (4)
O5—V1—O4	75.17 (4)	C11—C10—H7	120.5 (4)
O3—V1—O4	80.52 (2)	C12—C11—C10	120.93 (4)
N1—V1—O4	87.21 (4)	C12—C11—H8	119.3 (4)
C1—O2—V1	119.40 (4)	C10—C11—H8	119.7 (4)
C5—O3—V1	135.65 (3)	C11—C12—C13	117.60 (4)
C16—O4—V1	105.71 (4)	C11—C12—C4	124.61 (4)
C16—O4—H36	110.5 (4)	C13—C12—C4	117.79 (3)
V1—O4—H36	110.8 (4)	C7—C13—C12	119.36 (4)
C17—O5—V1	121.84 (3)	C7—C13—C8	121.66 (4)
C3—N1—C2	118.26 (4)	C12—C13—C8	118.93 (3)
C3—N1—V1	128.15 (4)	C2—C14—H9	109.5 (4)
C2—N1—V1	113.30 (3)	C2—C14—H10	109.5 (4)
O2—C1—C2	108.15 (5)	H9—C14—H10	109.4 (6)
O2—C1—H1	114.9 (5)	C2—C14—H11	109.5 (4)
C2—C1—H1	115.5 (4)	H9—C14—H11	109.5 (6)
O2—C1—H2	106.5 (4)	H10—C14—H11	109.3 (6)
C2—C1—H2	106.5 (4)	C2—C15—H12	109.5 (4)
H1—C1—H2	104.6 (6)	C2—C15—H13	109.4 (5)
C1—C2—N1	102.85 (3)	H12—C15—H13	109.5 (6)
C1—C2—C15	108.88 (5)	C2—C15—H14	109.5 (4)
N1—C2—C15	112.90 (4)	H12—C15—H14	109.5 (6)
C1—C2—C14	111.22 (5)	H13—C15—H14	109.5 (6)
N1—C2—C14	106.67 (3)	O4—C16—C17	106.08 (6)
C15—C2—C14	113.80 (3)	O4—C16—H15	113.4 (4)
N1—C3—C4	126.27 (4)	C17—C16—H15	111.9 (5)
N1—C3—H37	120.8 (4)	O4—C16—H16	109.2 (4)
C4—C3—H37	113.0 (4)	C17—C16—H16	108.8 (5)
C5—C4—C3	117.77 (4)	H15—C16—H16	107.4 (5)
C5—C4—C12	121.02 (4)	O5—C17—C16	110.04 (4)
C3—C4—C12	120.78 (4)	O5—C17—H17	109.6 (4)
O3—C5—C4	124.40 (4)	C16—C17—H17	109.7 (5)
O3—C5—C6	117.02 (3)	O5—C17—H18	109.7 (4)
C4—C5—C6	118.56 (5)	C16—C17—H18	109.7 (4)
C7—C6—C5	120.03 (4)	H17—C17—H18	108.1 (6)
C7—C6—H3	120.0 (4)

(bamubr) bis(Tetra-n-butylammonium) tetrabromo-uranyl top

Crystal data top

C₁₆Br₂NOU_0.50	γ = 90°
M_r = 501.01	V = 4298 (8) Å³
C2/c	Z = 8
a = 17.731 (15) Å	F(000) = 1816
b = 14.681 (15) Å	D_x = 1.549 Mg m⁻³
c = 17.08 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 7.52 mm⁻¹
β = 104.80 (8)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.020
Graphite monochromator	θ_max = 60.3°, θ_min = 1.8°
22662 measured reflections	h = −24→24
7087 independent reflections	k = −24→24
6880 reflections with I > 2σ(I)	l = −30→30

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.010	Secondary atom site location: difference Fourier map
wR(F²) = 0.086	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.57	(Δ/σ)_max = 3.860
7087 reflections	Δρ_max = 1.42 e Å⁻³
83 parameters	Δρ_min = −0.75 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
U1	0.0000	0.131200 (4)	0.7500	0.02000 (3)*
Br1	0.162100 (11)	0.127300 (9)	0.820300 (9)	0.02000 (4)*
Br3	0.0000	−0.060300 (14)	0.7500	0.02000 (5)*
Br4	0.0000	0.322300 (14)	0.7500	0.02000 (5)*
O1	0.01450 (9)	0.13100 (5)	0.65450 (8)	0.0200 (2)*
N1	0.21180 (8)	0.08170 (8)	0.13450 (7)	0.02000 (18)*
C1	0.20170 (9)	0.16820 (8)	0.08500 (7)	0.02000 (19)*
C2	0.12650 (9)	0.21600 (8)	0.07950 (7)	0.02000 (19)*
C3	0.12330 (9)	0.29930 (9)	0.01800 (8)	0.0200 (2)*
C4	0.05070 (10)	0.35670 (9)	0.01250 (8)	0.0200 (2)*
C5	0.20750 (10)	0.09500 (8)	0.21900 (8)	0.02000 (19)*
C6	0.26380 (9)	0.16780 (8)	0.26700 (7)	0.02000 (19)*
C7	0.26900 (9)	0.15900 (9)	0.35800 (8)	0.0200 (2)*
C8	0.31980 (9)	0.08130 (9)	0.39450 (7)	0.02000 (19)*
C9	0.29300 (8)	0.04500 (9)	0.12750 (7)	0.02000 (18)*
C10	0.31080 (8)	−0.04530 (9)	0.17250 (7)	0.02000 (19)*
C11	0.39100 (9)	−0.07500 (9)	0.15550 (7)	0.02000 (18)*
C12	0.41000 (9)	−0.17550 (8)	0.19150 (7)	0.0200 (2)*
C13	0.14750 (9)	0.01150 (9)	0.09800 (7)	0.02000 (19)*
C14	0.14120 (9)	−0.00780 (8)	0.01000 (7)	0.0200 (2)*
C15	0.08050 (10)	−0.09300 (9)	−0.01600 (8)	0.02000 (19)*
C16	0.11620 (9)	−0.17480 (8)	0.00800 (8)	0.02000 (19)*

Geometric parameters (Å, º) top

U1—O1	1.715 (2)	C2—C3	1.604 (2)
U1—O1ⁱ	1.715 (2)	C3—C4	1.521 (2)
U1—Br4	2.806 (3)	C5—C6	1.547 (2)
U1—Br3	2.811 (3)	C6—C7	1.538 (3)
U1—Br1	2.818 (3)	C7—C8	1.488 (2)
U1—Br1ⁱ	2.818 (3)	C9—C10	1.524 (2)
N1—C5	1.477 (2)	C10—C11	1.583 (2)
N1—C1	1.511 (2)	C11—C12	1.601 (2)
N1—C13	1.545 (2)	C13—C14	1.505 (2)
N1—C9	1.570 (2)	C14—C15	1.636 (2)
C1—C2	1.488 (2)	C15—C16	1.371 (2)

O1—U1—O1ⁱ	179.80 (5)	C1—N1—C13	111.42 (13)
O1—U1—Br4	90.10 (3)	C5—N1—C9	113.38 (13)
O1ⁱ—U1—Br4	90.10 (3)	C1—N1—C9	103.05 (11)
O1—U1—Br3	89.90 (3)	C13—N1—C9	109.69 (12)
O1ⁱ—U1—Br3	89.90 (3)	C2—C1—N1	114.07 (12)
Br4—U1—Br3	180.0	C1—C2—C3	106.39 (12)
O1—U1—Br1	91.19 (10)	C4—C3—C2	110.53 (13)
O1ⁱ—U1—Br1	88.81 (10)	N1—C5—C6	114.94 (12)
Br4—U1—Br1	91.164 (3)	C7—C6—C5	109.96 (12)
Br3—U1—Br1	88.836 (3)	C8—C7—C6	111.17 (12)
O1—U1—Br1ⁱ	88.81 (10)	C10—C9—N1	109.62 (11)
O1ⁱ—U1—Br1ⁱ	91.19 (10)	C9—C10—C11	103.12 (11)
Br4—U1—Br1ⁱ	91.164 (3)	C10—C11—C12	107.11 (11)
Br3—U1—Br1ⁱ	88.836 (3)	C14—C13—N1	112.78 (12)
Br1—U1—Br1ⁱ	177.672 (6)	C13—C14—C15	106.91 (12)
C5—N1—C1	114.03 (11)	C16—C15—C14	111.55 (15)
C5—N1—C13	105.39 (12)

Symmetry code: (i) −x, y, −z+3/2.

(farner) Tetrachloro-bis(N,N,N,N'-tetramethylurea)-uranium(iv) top

Crystal data top

C₁₀Cl₄N₄O₂U	γ = 90°
M_r = 587.97	V = 2019.2 (4) Å³
C2/c	Z = 4
a = 16.429 (2) Å	F(000) = 1056
b = 8.514 (1) Å	D_x = 1.934 Mg m⁻³
c = 16.418 (2) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 8.57 mm⁻¹
β = 118.45 (2)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.004
Graphite monochromator	θ_max = 52.7°, θ_min = 2.8°
9718 measured reflections	h = −26→26
3303 independent reflections	k = −8→8
3049 reflections with I > 2σ(I)	l = −24→24

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.004	Secondary atom site location: difference Fourier map
wR(F²) = 0.046	w = 1/[σ²(F_o²) + (0.P)² + 0.0533P] where P = (F_o² + 2F_c²)/3
S = 0.49	(Δ/σ)_max = 2.086
3303 reflections	Δρ_max = 0.41 e Å⁻³
42 parameters	Δρ_min = −0.25 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
U1	0.250000	0.250000	0.00000	0.02000 (3)*
Cl1	0.393300 (13)	0.061300 (17)	0.071700 (14)	0.02000 (5)*
Cl2	0.359100 (13)	0.496100 (18)	0.056600 (14)	0.02000 (5)*
N1	0.34620 (12)	0.24600 (6)	−0.20230 (13)	0.0200 (3)*
N2	0.18350 (6)	0.23820 (10)	−0.28790 (7)	0.0200 (2)*
O1	0.25710 (11)	0.24990 (4)	−0.13170 (12)	0.0200 (3)*
C1	0.26210 (12)	0.24460 (8)	−0.20710 (13)	0.0200 (3)*
C2	0.42870 (4)	0.28520 (16)	−0.11240 (5)	0.02000 (9)*
C3	0.36330 (5)	0.16840 (10)	−0.27530 (5)	0.02000 (12)*
C4	0.09560 (5)	0.19710 (9)	−0.28570 (5)	0.02000 (14)*
C5	0.17310 (6)	0.31540 (7)	−0.37460 (7)	0.02000 (14)*

Geometric parameters (Å, º) top

U1—O1ⁱ	2.2202 (17)	N1—C2	1.490 (2)
U1—O1	2.2202 (17)	N1—C3	1.5075 (18)
U1—Cl1ⁱ	2.6209 (4)	N2—C1	1.341 (2)
U1—Cl1	2.6209 (4)	N2—C5	1.5019 (13)
U1—Cl2ⁱ	2.6229 (3)	N2—C4	1.5030 (12)
U1—Cl2	2.6229 (3)	O1—C1	1.280 (2)
N1—C1	1.346 (2)

O1ⁱ—U1—O1	180.000 (19)	Cl1—U1—Cl2	90.833 (15)
O1ⁱ—U1—Cl1ⁱ	89.11 (4)	Cl2ⁱ—U1—Cl2	180.000 (10)
O1—U1—Cl1ⁱ	90.89 (4)	C1—N1—C2	118.94 (14)
O1ⁱ—U1—Cl1	90.89 (4)	C1—N1—C3	121.63 (13)
O1—U1—Cl1	89.11 (4)	C2—N1—C3	117.36 (11)
Cl1ⁱ—U1—Cl1	180.0	C1—N2—C5	122.75 (10)
O1ⁱ—U1—Cl2ⁱ	90.07 (3)	C1—N2—C4	117.98 (11)
O1—U1—Cl2ⁱ	89.93 (3)	C5—N2—C4	116.61 (8)
Cl1ⁱ—U1—Cl2ⁱ	90.833 (15)	C1—O1—U1	177.92 (6)
Cl1—U1—Cl2ⁱ	89.167 (15)	O1—C1—N2	118.88 (16)
O1ⁱ—U1—Cl2	89.93 (3)	O1—C1—N1	118.69 (17)
O1—U1—Cl2	90.07 (3)	N2—C1—N1	122.42 (17)
Cl1ⁱ—U1—Cl2	89.167 (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

C₁₀Br₄N₄O₂U	γ = 90°
M_r = 765.81	V = 2156.7 (12) Å³
C2/c	Z = 4
a = 16.764 (5) Å	F(000) = 1344
b = 8.710 (4) Å	D_x = 2.359 Mg m⁻³
c = 16.655 (3) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 14.94 mm⁻¹
β = 117.52 (2)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.008
Graphite monochromator	θ_max = 50.6°, θ_min = 2.7°
9718 measured reflections	h = −26→26
3303 independent reflections	k = −8→8
3198 reflections with I > 2σ(I)	l = −24→24

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.004	Secondary atom site location: difference Fourier map
wR(F²) = 0.033	w = 1/[σ²(F_o²) + (0.P)² + 0.0089P] where P = (F_o² + 2F_c²)/3
S = 0.39	(Δ/σ)_max = 1.266
3303 reflections	Δρ_max = 0.37 e Å⁻³
42 parameters	Δρ_min = −0.36 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
U1	0.250000	0.250000	0.000000	0.02000 (3)*
Br1	0.397900 (6)	0.054000 (13)	0.071300 (7)	0.02000 (3)*
Br2	0.361200 (7)	0.506600 (12)	0.055100 (7)	0.02000 (3)*
N1	0.34020 (9)	0.24560 (9)	−0.20330 (9)	0.0200 (2)*
N2	0.18210 (7)	0.23880 (11)	−0.28320 (8)	0.0200 (2)*
O1	0.25540 (8)	0.24970 (6)	−0.13030 (8)	0.0200 (2)*
C1	0.25870 (10)	0.24560 (10)	−0.20600 (11)	0.0200 (3)*
C2	0.42070 (5)	0.28650 (17)	−0.11930 (6)	0.02000 (12)*
C3	0.35600 (6)	0.16900 (12)	−0.27430 (7)	0.02000 (16)*
C4	0.09800 (6)	0.19720 (13)	−0.28080 (7)	0.02000 (18)*
C5	0.17170 (7)	0.31710 (10)	−0.36600 (8)	0.02000 (18)*

Geometric parameters (Å, º) top

U1—O1	2.2134 (13)	N1—C2	1.4699 (17)
U1—O1ⁱ	2.2134 (13)	N1—C3	1.4843 (17)
U1—Br2	2.7806 (9)	N2—C1	1.334 (2)
U1—Br2ⁱ	2.7806 (9)	N2—C4	1.4740 (15)
U1—Br1ⁱ	2.7841 (8)	N2—C5	1.4748 (17)
U1—Br1	2.7841 (8)	O1—C1	1.288 (2)
N1—C1	1.346 (2)

O1—U1—O1ⁱ	180.00 (6)	Br2ⁱ—U1—Br1	88.68 (3)
O1—U1—Br2	89.98 (3)	Br1ⁱ—U1—Br1	180.000 (5)
O1ⁱ—U1—Br2	90.02 (3)	C1—N1—C2	120.21 (12)
O1—U1—Br2ⁱ	90.02 (3)	C1—N1—C3	121.69 (12)
O1ⁱ—U1—Br2ⁱ	89.98 (3)	C2—N1—C3	116.35 (10)
Br2—U1—Br2ⁱ	180.0	C1—N2—C4	119.44 (11)
O1—U1—Br1ⁱ	90.82 (3)	C1—N2—C5	121.73 (10)
O1ⁱ—U1—Br1ⁱ	89.18 (3)	C4—N2—C5	115.96 (10)
Br2—U1—Br1ⁱ	88.68 (3)	C1—O1—U1	178.47 (6)
Br2ⁱ—U1—Br1ⁱ	91.32 (3)	O1—C1—N2	119.15 (13)
O1—U1—Br1	89.18 (3)	O1—C1—N1	117.99 (14)
O1ⁱ—U1—Br1	90.82 (3)	N2—C1—N1	122.84 (14)
Br2—U1—Br1	91.32 (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

C₂₆H₄₃F₃O₃P₂Pd	γ = 90°
M_r = 628.94	V = 5761.9 (19) Å³
I2/a	Z = 8
a = 20.244 (4) Å	F(000) = 2608
b = 10.714 (2) Å	D_x = 1.450 Mg m⁻³
c = 27.238 (5) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 0.80 mm⁻¹
β = 102.76 (3)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.016
Graphite monochromator	θ_max = 47.4°, θ_min = 1.5°
26382 measured reflections	h = −35→35
8546 independent reflections	k = −10→10
8103 reflections with I > 2σ(I)	l = −45→45

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.014	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.065	H atoms treated by a mixture of independent and constrained refinement
S = 0.64	w = 1/[σ²(F_o²) + (0.P)² + 0.0757P] where P = (F_o² + 2F_c²)/3
8546 reflections	(Δ/σ)_max = 4.722
313 parameters	Δρ_max = 0.62 e Å⁻³
0 restraints	Δρ_min = −0.31 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pd1	0.166400 (3)	0.310100 (6)	0.358900 (2)	0.02000 (3)*
P1	0.262600 (10)	0.42870 (2)	0.353400 (8)	0.02000 (4)*
P2	0.103200 (10)	0.12920 (2)	0.365800 (8)	0.02000 (5)*
O1	0.20160 (3)	0.19960 (5)	0.31210 (3)	0.02000 (12)*
O2	0.12750 (3)	0.43130 (6)	0.40390 (2)	0.02000 (10)*
C1	0.08110 (4)	0.49590 (8)	0.38160 (3)	0.02000 (13)*
O3	0.04970 (3)	0.49200 (6)	0.33760 (2)	0.02000 (10)*
C2	0.05660 (4)	0.59310 (8)	0.41490 (3)	0.02000 (12)*
F1	0.00680 (2)	0.66760 (5)	0.391300 (18)	0.02000 (8)*
F2	0.10670 (2)	0.66660 (5)	0.437300 (18)	0.02000 (8)*
F3	0.03350 (2)	0.53820 (5)	0.452100 (19)	0.02000 (8)*
C3	0.25040 (4)	0.13560 (8)	0.34420 (3)	0.02000 (13)*
C4	0.31530 (4)	0.18580 (7)	0.35650 (4)	0.02000 (15)*
C5	0.36600 (4)	0.11650 (8)	0.38750 (3)	0.02000 (12)*
C6	0.35020 (4)	0.00390 (8)	0.40620 (3)	0.02000 (13)*
C7	0.28490 (4)	−0.04050 (8)	0.39720 (3)	0.02000 (12)*
C8	0.23240 (4)	0.02780 (8)	0.36640 (3)	0.02000 (12)*
C9	0.32280 (4)	0.31410 (7)	0.33650 (3)	0.02000 (15)*
C10	0.15790 (4)	−0.00260 (8)	0.35510 (3)	0.02000 (12)*
C11	0.31060 (3)	0.50120 (8)	0.41260 (3)	0.02000 (13)*
C12	0.24400 (3)	0.54040 (8)	0.29880 (3)	0.02000 (12)*
C13	0.33460 (4)	0.39900 (9)	0.44900 (3)	0.02000 (12)*
C14	0.37210 (4)	0.58130 (8)	0.40370 (3)	0.02000 (13)*
C15	0.26600 (4)	0.58920 (8)	0.43510 (3)	0.02000 (13)*
C16	0.19420 (4)	0.46850 (8)	0.25690 (3)	0.02000 (13)*
C17	0.30470 (4)	0.57050 (8)	0.27770 (3)	0.02000 (13)*
C18	0.20690 (4)	0.65410 (9)	0.31240 (3)	0.02000 (12)*
C19	0.02510 (4)	0.10780 (8)	0.31550 (3)	0.02000 (12)*
C20	0.09060 (4)	0.10040 (9)	0.43090 (3)	0.02000 (12)*
C21	0.05650 (4)	−0.02340 (8)	0.43750 (3)	0.02000 (12)*
C22	−0.03300 (4)	0.18590 (7)	0.32590 (3)	0.02000 (15)*
C23	0.00200 (4)	−0.02740 (8)	0.30630 (3)	0.02000 (13)*
C24	0.05000 (4)	0.20590 (8)	0.44820 (3)	0.02000 (14)*
C25	0.16170 (4)	0.10310 (9)	0.46460 (3)	0.02000 (12)*
C26	0.04280 (4)	0.15510 (9)	0.26740 (3)	0.02000 (12)*
H1	0.4103 (6)	0.1461 (12)	0.3955 (5)	0.020 (3)*
H2	0.3848 (6)	−0.0437 (12)	0.4255 (5)	0.020 (3)*
H3	0.2754 (6)	−0.1155 (12)	0.4116 (5)	0.020 (3)*
H4	0.3157 (7)	0.3100 (10)	0.3001 (5)	0.020 (3)*
H5	0.3688 (6)	0.3430 (13)	0.3496 (5)	0.020 (3)*
H6	0.1507 (6)	−0.0722 (11)	0.3761 (5)	0.020 (3)*
H7	0.1441 (6)	−0.0290 (12)	0.3203 (5)	0.020 (3)*
H8	0.3662 (6)	0.3476 (12)	0.4366 (5)	0.020 (3)*
H9	0.2968 (6)	0.3493 (12)	0.4531 (5)	0.020 (3)*
H10	0.3566 (6)	0.4341 (12)	0.4809 (5)	0.020 (3)*
H11	0.3556 (6)	0.6492 (12)	0.3816 (5)	0.020 (3)*
H12	0.4011 (6)	0.5301 (12)	0.3888 (5)	0.020 (3)*
H13	0.3970 (6)	0.6133 (12)	0.4351 (5)	0.020 (3)*
H14	0.2511 (6)	0.6567 (13)	0.4122 (5)	0.020 (3)*
H15	0.2914 (6)	0.6219 (11)	0.4665 (5)	0.020 (3)*
H16	0.2273 (6)	0.5444 (12)	0.4409 (5)	0.020 (3)*
H17	0.1523 (6)	0.4553 (12)	0.2670 (5)	0.020 (3)*
H18	0.2135 (6)	0.3894 (11)	0.2514 (5)	0.020 (3)*
H19	0.1860 (6)	0.5162 (12)	0.2264 (5)	0.020 (3)*
H20	0.3268 (6)	0.4945 (12)	0.2718 (5)	0.020 (3)*
H21	0.3356 (6)	0.6212 (11)	0.3012 (5)	0.020 (3)*
H22	0.2905 (6)	0.6150 (12)	0.2466 (5)	0.020 (3)*
H23	0.1747 (6)	0.6284 (11)	0.3315 (5)	0.020 (3)*
H24	0.1836 (7)	0.6952 (10)	0.2822 (5)	0.020 (3)*
H25	0.2389 (6)	0.7107 (12)	0.3321 (5)	0.020 (3)*
H26	0.0108 (6)	−0.0224 (12)	0.4182 (5)	0.020 (3)*
H27	0.0564 (6)	−0.0353 (12)	0.4724 (5)	0.020 (3)*
H28	0.0809 (6)	−0.0904 (12)	0.4262 (5)	0.020 (3)*
H29	−0.0482 (6)	0.1515 (13)	0.3540 (5)	0.020 (3)*
H30	−0.0697 (7)	0.1855 (10)	0.2968 (5)	0.020 (3)*
H31	−0.0180 (6)	0.2700 (13)	0.3334 (5)	0.020 (3)*
H32	−0.0112 (6)	−0.0594 (11)	0.3356 (5)	0.020 (3)*
H33	0.0384 (6)	−0.0768 (11)	0.2994 (5)	0.020 (3)*
H34	−0.0359 (6)	−0.0312 (12)	0.2780 (5)	0.020 (3)*
H35	0.0052 (7)	0.2076 (12)	0.4273 (5)	0.020 (3)*
H36	0.0720 (6)	0.2841 (13)	0.4456 (5)	0.020 (3)*
H37	0.0475 (7)	0.1919 (10)	0.4825 (5)	0.020 (3)*
H38	0.1883 (6)	0.0372 (12)	0.4550 (5)	0.020 (3)*
H39	0.1589 (6)	0.0918 (12)	0.4990 (5)	0.020 (3)*
H40	0.1826 (7)	0.1818 (11)	0.4610 (5)	0.020 (3)*
H41	0.0794 (6)	0.1069 (11)	0.2603 (5)	0.020 (3)*
H42	0.0559 (6)	0.2410 (12)	0.2714 (5)	0.020 (3)*
H43	0.0040 (6)	0.1471 (12)	0.2400 (5)	0.020 (3)*

Geometric parameters (Å, º) top

Pd1—O1	1.9838 (7)	C13—H10	0.961 (13)
Pd1—O2	2.0579 (7)	C14—H11	0.956 (13)
Pd1—P2	2.3526 (4)	C14—H12	0.957 (13)
Pd1—P1	2.3577 (4)	C14—H13	0.955 (12)
Pd1—C3	2.6169 (9)	C15—H14	0.959 (13)
P1—C9	1.8581 (9)	C15—H15	0.961 (13)
P1—C11	1.8589 (9)	C15—H16	0.961 (12)
P1—C12	1.8811 (9)	C16—H17	0.958 (12)
P2—C10	1.8568 (9)	C16—H18	0.959 (12)
P2—C19	1.8635 (10)	C16—H19	0.958 (13)
P2—C20	1.8720 (9)	C17—H20	0.960 (12)
O1—C3	1.3524 (11)	C17—H21	0.959 (12)
O2—C1	1.2158 (10)	C17—H22	0.959 (13)
C1—O3	1.2270 (10)	C18—H23	0.960 (13)
C1—C2	1.5336 (12)	C18—H24	0.960 (14)
C2—F2	1.3220 (10)	C18—H25	0.960 (13)
C2—F1	1.3343 (9)	C19—C26	1.5196 (12)
C2—F3	1.3419 (11)	C19—C22	1.5202 (12)
C3—C8	1.3891 (12)	C19—C23	1.5258 (12)
C3—C4	1.3904 (12)	C20—C21	1.5241 (12)
C4—C5	1.3910 (12)	C20—C25	1.5269 (11)
C4—C9	1.4986 (12)	C20—C24	1.5318 (13)
C5—C6	1.3744 (12)	C21—H26	0.958 (12)
C5—H1	0.931 (12)	C21—H27	0.960 (12)
C6—C7	1.3750 (11)	C21—H28	0.960 (12)
C6—H2	0.930 (13)	C22—H29	0.959 (13)
C7—C8	1.4053 (12)	C22—H30	0.959 (14)
C7—H3	0.933 (12)	C22—H31	0.958 (13)
C8—C10	1.5068 (11)	C23—H32	0.959 (12)
C9—H4	0.971 (14)	C23—H33	0.959 (12)
C9—H5	0.971 (12)	C23—H34	0.961 (12)
C10—H6	0.970 (12)	C24—H35	0.959 (13)
C10—H7	0.969 (12)	C24—H36	0.959 (13)
C11—C13	1.4850 (12)	C24—H37	0.959 (14)
C11—C15	1.5245 (12)	C25—H38	0.959 (12)
C11—C14	1.5744 (11)	C25—H39	0.959 (13)
C12—C17	1.5021 (12)	C25—H40	0.958 (12)
C12—C18	1.5193 (12)	C26—H41	0.957 (12)
C12—C16	1.5505 (12)	C26—H42	0.957 (13)
C13—H8	0.960 (13)	C26—H43	0.960 (12)
C13—H9	0.959 (13)

O1—Pd1—O2	176.64 (3)	C11—C13—H10	109.5 (8)
O1—Pd1—P2	80.71 (3)	H8—C13—H10	109.3 (10)
O2—Pd1—P2	100.71 (2)	H9—C13—H10	109.5 (10)
O1—Pd1—P1	82.06 (3)	C11—C14—H11	109.5 (7)
O2—Pd1—P1	97.35 (2)	C11—C14—H12	109.4 (8)
P2—Pd1—P1	156.998 (8)	H11—C14—H12	109.3 (10)
O1—Pd1—C3	30.41 (3)	C11—C14—H13	109.7 (8)
O2—Pd1—C3	152.75 (3)	H11—C14—H13	109.4 (11)
P2—Pd1—C3	78.87 (2)	H12—C14—H13	109.5 (10)
P1—Pd1—C3	78.55 (2)	C11—C15—H14	109.5 (8)
C9—P1—C11	104.20 (4)	C11—C15—H15	109.6 (7)
C9—P1—C12	104.61 (4)	H14—C15—H15	109.5 (11)
C11—P1—C12	113.26 (4)	C11—C15—H16	109.5 (8)
C9—P1—Pd1	104.82 (3)	H14—C15—H16	109.4 (10)
C11—P1—Pd1	116.81 (3)	H15—C15—H16	109.3 (11)
C12—P1—Pd1	111.67 (3)	C12—C16—H17	109.6 (7)
C10—P2—C19	103.27 (4)	C12—C16—H18	109.5 (7)
C10—P2—C20	103.54 (4)	H17—C16—H18	109.4 (10)
C19—P2—C20	113.90 (4)	C12—C16—H19	109.5 (7)
C10—P2—Pd1	105.09 (3)	H17—C16—H19	109.4 (10)
C19—P2—Pd1	115.51 (3)	H18—C16—H19	109.5 (11)
C20—P2—Pd1	113.69 (3)	C12—C17—H20	109.4 (7)
C3—O1—Pd1	101.65 (6)	C12—C17—H21	109.5 (8)
C1—O2—Pd1	114.63 (6)	H20—C17—H21	109.5 (10)
O2—C1—O3	130.16 (8)	C12—C17—H22	109.5 (7)
O2—C1—C2	113.96 (7)	H20—C17—H22	109.5 (10)
O3—C1—C2	115.81 (7)	H21—C17—H22	109.4 (11)
F2—C2—F1	106.68 (7)	C12—C18—H23	109.5 (7)
F2—C2—F3	105.81 (7)	C12—C18—H24	109.6 (8)
F1—C2—F3	105.89 (6)	H23—C18—H24	109.4 (11)
F2—C2—C1	111.23 (6)	C12—C18—H25	109.5 (8)
F1—C2—C1	115.46 (7)	H23—C18—H25	109.5 (11)
F3—C2—C1	111.17 (7)	H24—C18—H25	109.4 (10)
O1—C3—C8	118.59 (7)	C26—C19—C22	108.46 (7)
O1—C3—C4	118.43 (8)	C26—C19—C23	107.28 (7)
C8—C3—C4	122.78 (7)	C22—C19—C23	109.36 (6)
O1—C3—Pd1	47.94 (4)	C26—C19—P2	105.64 (5)
C8—C3—Pd1	106.59 (6)	C22—C19—P2	111.16 (6)
C4—C3—Pd1	107.35 (6)	C23—C19—P2	114.65 (6)
C3—C4—C5	118.10 (8)	C21—C20—C25	109.69 (7)
C3—C4—C9	115.69 (7)	C21—C20—C24	108.55 (7)
C5—C4—C9	126.15 (8)	C25—C20—C24	107.44 (7)
C6—C5—C4	119.51 (7)	C21—C20—P2	114.53 (6)
C6—C5—H1	120.2 (8)	C25—C20—P2	105.00 (6)
C4—C5—H1	120.3 (8)	C24—C20—P2	111.37 (6)
C5—C6—C7	122.06 (7)	C20—C21—H26	109.5 (8)
C5—C6—H2	118.9 (8)	C20—C21—H27	109.4 (8)
C7—C6—H2	119.1 (8)	H26—C21—H27	109.4 (10)
C6—C7—C8	119.79 (8)	C20—C21—H28	109.5 (8)
C6—C7—H3	120.2 (7)	H26—C21—H28	109.6 (10)
C8—C7—H3	120.0 (8)	H27—C21—H28	109.4 (11)
C3—C8—C7	117.15 (7)	C19—C22—H29	109.6 (8)
C3—C8—C10	115.96 (7)	C19—C22—H30	109.5 (8)
C7—C8—C10	126.89 (8)	H29—C22—H30	109.3 (11)
C4—C9—P1	113.04 (7)	C19—C22—H31	109.6 (7)
C4—C9—H4	109.0 (7)	H29—C22—H31	109.5 (11)
P1—C9—H4	109.0 (7)	H30—C22—H31	109.4 (10)
C4—C9—H5	108.9 (8)	C19—C23—H32	109.5 (7)
P1—C9—H5	109.0 (8)	C19—C23—H33	109.6 (7)
H4—C9—H5	107.7 (11)	H32—C23—H33	109.5 (10)
C8—C10—P2	114.10 (6)	C19—C23—H34	109.5 (8)
C8—C10—H6	108.6 (7)	H32—C23—H34	109.4 (10)
P2—C10—H6	108.6 (7)	H33—C23—H34	109.4 (11)
C8—C10—H7	108.8 (7)	C20—C24—H35	109.4 (8)
P2—C10—H7	108.8 (7)	C20—C24—H36	109.4 (8)
H6—C10—H7	107.7 (10)	H35—C24—H36	109.5 (11)
C13—C11—C15	108.85 (7)	C20—C24—H37	109.4 (7)
C13—C11—C14	110.58 (6)	H35—C24—H37	109.6 (11)
C15—C11—C14	106.47 (7)	H36—C24—H37	109.5 (10)
C13—C11—P1	107.60 (6)	C20—C25—H38	109.5 (7)
C15—C11—P1	111.38 (5)	C20—C25—H39	109.5 (7)
C14—C11—P1	111.95 (6)	H38—C25—H39	109.4 (10)
C17—C12—C18	114.29 (7)	C20—C25—H40	109.5 (8)
C17—C12—C16	106.20 (7)	H38—C25—H40	109.4 (11)
C18—C12—C16	107.56 (6)	H39—C25—H40	109.5 (11)
C17—C12—P1	113.66 (6)	C19—C26—H41	109.6 (8)
C18—C12—P1	109.92 (6)	C19—C26—H42	109.6 (7)
C16—C12—P1	104.47 (6)	H41—C26—H42	109.5 (10)
C11—C13—H8	109.5 (8)	C19—C26—H43	109.4 (8)
C11—C13—H9	109.6 (7)	H41—C26—H43	109.4 (11)
H8—C13—H9	109.5 (11)	H42—C26—H43	109.4 (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

C₄₇H₆₃NO₆Si	γ = 90°
M_r = 766.07	V = 8664 (2) Å³
I2/a	Z = 8
a = 33.990 (4) Å	F(000) = 3312
b = 9.5179 (13) Å	D_x = 1.175 Mg m⁻³
c = 29.467 (4) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 0.10 mm⁻¹
β = 114.65 (3)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.020
Graphite monochromator	θ_max = 45.1°, θ_min = 1.3°
41716 measured reflections	h = −55→55
13023 independent reflections	k = −10→10
11934 reflections with I > 2σ(I)	l = −45→45

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.208	H atoms treated by a mixture of independent and constrained refinement
S = 1.13	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
13023 reflections	(Δ/σ)_max = 13.453
473 parameters	Δρ_max = 1.14 e Å⁻³
0 restraints	Δρ_min = −0.24 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Si1	0.347800 (7)	0.47870 (2)	−0.189600 (8)	0.02000 (8)*
N1	0.36520 (2)	0.36990 (7)	−0.04530 (2)	0.02000 (13)*
O1	0.440800 (18)	0.54280 (6)	−0.106700 (19)	0.02000 (11)*
O2	0.394500 (19)	0.10660 (6)	−0.03280 (2)	0.02000 (11)*
O3	0.501900 (19)	0.21040 (6)	−0.00240 (2)	0.02000 (11)*
O4	0.517900 (19)	0.05550 (6)	0.07780 (2)	0.02000 (11)*
O5	0.297600 (19)	0.31790 (6)	−0.05030 (2)	0.02000 (12)*
O6	0.357300 (19)	0.29070 (6)	0.02210 (2)	0.02000 (11)*
C1	0.36400 (2)	0.65510 (8)	−0.20590 (3)	0.02000 (13)*
H1	0.3962 (5)	0.6508 (13)	−0.1936 (5)	0.020 (3)*
C2	0.35530 (2)	0.77820 (8)	−0.17790 (2)	0.02000 (13)*
H2	0.3648 (4)	0.8659 (14)	−0.1877 (5)	0.020 (3)*
H3	0.3714 (4)	0.7640 (14)	−0.1419 (5)	0.020 (3)*
H4	0.3243 (4)	0.7835 (14)	−0.1863 (5)	0.020 (3)*
C3	0.34710 (3)	0.68620 (8)	−0.26120 (3)	0.02000 (14)*
H5	0.3573 (4)	0.7789 (14)	−0.2660 (5)	0.020 (3)*
H6	0.3154 (4)	0.6854 (14)	−0.2762 (5)	0.020 (3)*
H7	0.3576 (4)	0.6145 (14)	−0.2774 (5)	0.020 (3)*
C4	0.28780 (2)	0.45310 (8)	−0.21340 (3)	0.02000 (13)*
H8	0.2835 (4)	0.3619 (14)	−0.1991 (5)	0.020 (3)*
C5	0.26370 (3)	0.56530 (8)	−0.19690 (3)	0.02000 (13)*
H9	0.2328 (4)	0.5425 (15)	−0.2107 (5)	0.020 (3)*
H10	0.2677 (4)	0.6576 (14)	−0.2090 (5)	0.020 (3)*
H11	0.2753 (4)	0.5669 (14)	−0.1603 (5)	0.020 (3)*
C6	0.26460 (2)	0.43770 (8)	−0.27050 (3)	0.02000 (12)*
H12	0.2336 (4)	0.4236 (14)	−0.2804 (5)	0.020 (3)*
H13	0.2765 (4)	0.3567 (14)	−0.2811 (5)	0.020 (3)*
H14	0.2691 (4)	0.5231 (14)	−0.2864 (5)	0.020 (3)*
C7	0.36920 (3)	0.33680 (8)	−0.21800 (3)	0.02000 (13)*
H15	0.3547 (4)	0.3502 (14)	−0.2550 (5)	0.020 (3)*
C8	0.41710 (2)	0.34390 (8)	−0.20350 (3)	0.02000 (13)*
H16	0.4256 (4)	0.2677 (14)	−0.2200 (5)	0.020 (3)*
H17	0.4327 (5)	0.3340 (14)	−0.1672 (5)	0.020 (3)*
H18	0.4243 (4)	0.4345 (14)	−0.2139 (5)	0.020 (3)*
C9	0.35740 (3)	0.18820 (8)	−0.20750 (3)	0.02000 (13)*
H19	0.3690 (4)	0.1189 (14)	−0.2233 (5)	0.020 (3)*
H20	0.3258 (5)	0.1791 (14)	−0.2210 (5)	0.020 (3)*
H21	0.3698 (4)	0.1720 (14)	−0.1713 (5)	0.020 (3)*
C10	0.37220 (2)	0.45430 (8)	−0.11990 (3)	0.02000 (13)*
C11	0.41720 (3)	0.49120 (8)	−0.08880 (3)	0.02000 (13)*
C12	0.43450 (3)	0.47060 (8)	−0.03320 (3)	0.02000 (14)*
H22	0.4308 (4)	0.5591 (14)	−0.0177 (5)	0.020 (3)*
H23	0.4658 (4)	0.4500 (15)	−0.0198 (5)	0.020 (3)*
C13	0.41190 (2)	0.35250 (8)	−0.01880 (2)	0.02000 (13)*
H24	0.4204 (4)	0.3558 (14)	0.0180 (5)	0.020 (3)*
C14	0.34870 (2)	0.40330 (8)	−0.09560 (3)	0.02000 (14)*
H25	0.3186 (4)	0.3896 (14)	−0.1148 (5)	0.020 (3)*
C15	0.42540 (2)	0.20720 (8)	−0.03280 (3)	0.02000 (13)*
H26	0.4243 (4)	0.2132 (14)	−0.0671 (5)	0.020 (3)*
C16	0.47090 (3)	0.17010 (8)	0.00370 (3)	0.02000 (13)*
C17	0.47420 (2)	0.07980 (8)	0.04740 (3)	0.02000 (13)*
H27	0.4603 (4)	0.1281 (14)	0.0667 (5)	0.020 (3)*
H28	0.4591 (4)	−0.0107 (14)	0.0351 (5)	0.020 (3)*
C18	0.52350 (3)	−0.03270 (8)	0.11590 (3)	0.02000 (13)*
H29	0.5535 (4)	−0.0687 (14)	0.1297 (5)	0.020 (3)*
H30	0.5038 (4)	−0.1139 (15)	0.1027 (5)	0.020 (3)*
C19	0.51480 (3)	0.03570 (8)	0.15870 (3)	0.02000 (14)*
C20	0.53490 (3)	0.13810 (7)	0.18620 (3)	0.02000 (13)*
H31	0.5552 (4)	0.1880 (14)	0.1778 (5)	0.020 (3)*
C21	0.52900 (3)	0.18000 (8)	0.22620 (3)	0.02000 (13)*
H32	0.5469 (4)	0.2530 (15)	0.2462 (5)	0.020 (3)*
C22	0.50200 (3)	0.12920 (8)	0.23850 (3)	0.02000 (13)*
H33	0.4972 (5)	0.1678 (14)	0.2654 (5)	0.020 (3)*
C23	0.47900 (3)	0.01670 (8)	0.21290 (3)	0.02000 (14)*
H34	0.4590 (5)	−0.0304 (14)	0.2224 (5)	0.020 (3)*
C24	0.48660 (3)	−0.02760 (7)	0.17050 (3)	0.02000 (13)*
H35	0.4707 (5)	−0.1047 (14)	0.1509 (5)	0.020 (3)*
C25	0.38910 (3)	−0.01040 (8)	−0.06610 (3)	0.02000 (13)*
H36	0.4147 (4)	−0.0724 (14)	−0.0525 (5)	0.020 (3)*
H37	0.3855 (4)	0.0240 (13)	−0.0993 (5)	0.020 (3)*
C26	0.35010 (3)	−0.08800 (8)	−0.07050 (3)	0.02000 (13)*
C27	0.35380 (2)	−0.21340 (8)	−0.04670 (3)	0.02000 (13)*
H38	0.3812 (4)	−0.2541 (14)	−0.0268 (5)	0.020 (3)*
C28	0.31080 (2)	−0.28480 (8)	−0.05380 (3)	0.02000 (13)*
H39	0.3086 (4)	−0.3714 (14)	−0.0392 (5)	0.020 (3)*
C29	0.27370 (2)	−0.19830 (8)	−0.08690 (3)	0.02000 (13)*
H40	0.2457 (4)	−0.2359 (14)	−0.0948 (5)	0.020 (3)*
C30	0.27500 (3)	−0.08010 (8)	−0.10590 (3)	0.02000 (13)*
H41	0.2492 (4)	−0.0303 (13)	−0.1253 (5)	0.020 (3)*
C31	0.31090 (3)	−0.03180 (8)	−0.09860 (3)	0.02000 (14)*
H42	0.3110 (4)	0.0550 (15)	−0.1145 (5)	0.020 (3)*
C32	0.33590 (3)	0.32310 (8)	−0.02630 (3)	0.02000 (14)*
C33	0.33260 (3)	0.21700 (8)	0.04540 (3)	0.02000 (13)*
H43	0.3025 (4)	0.2553 (14)	0.0323 (5)	0.020 (3)*
C34	0.33130 (2)	0.06420 (8)	0.03210 (3)	0.02000 (13)*
H44	0.3613 (5)	0.0297 (14)	0.0421 (5)	0.020 (3)*
H45	0.3157 (4)	0.0532 (15)	−0.0046 (5)	0.020 (3)*
C35	0.30900 (3)	−0.02490 (8)	0.05770 (3)	0.02000 (14)*
H46	0.2787 (4)	0.0064 (14)	0.0470 (5)	0.020 (3)*
H47	0.3088 (4)	−0.1248 (14)	0.0481 (5)	0.020 (3)*
C36	0.33260 (2)	−0.00970 (8)	0.11200 (3)	0.02000 (13)*
H48	0.3628 (4)	−0.0428 (14)	0.1226 (5)	0.020 (3)*
H49	0.3187 (4)	−0.0679 (15)	0.1290 (5)	0.020 (3)*
C37	0.33260 (3)	0.14280 (8)	0.12650 (3)	0.02000 (13)*
H50	0.3478 (5)	0.1514 (14)	0.1633 (5)	0.020 (3)*
H51	0.3024 (5)	0.1744 (14)	0.1163 (5)	0.020 (3)*
C38	0.35550 (3)	0.24180 (8)	0.10160 (3)	0.02000 (13)*
H52	0.3855 (4)	0.2041 (14)	0.1122 (5)	0.020 (3)*
C39	0.36080 (2)	0.39670 (8)	0.11800 (3)	0.02000 (13)*
C40	0.31780 (3)	0.47410 (7)	0.09080 (3)	0.02000 (14)*
H53	0.3095 (4)	0.4706 (14)	0.0547 (5)	0.020 (3)*
H54	0.3212 (4)	0.5724 (14)	0.1018 (5)	0.020 (3)*
H55	0.2954 (4)	0.4292 (14)	0.0985 (5)	0.020 (3)*
C41	0.37470 (2)	0.40660 (8)	0.17560 (3)	0.02000 (13)*
H56	0.3774 (5)	0.5056 (14)	0.1857 (5)	0.020 (3)*
H57	0.4025 (4)	0.3591 (14)	0.1931 (5)	0.020 (3)*
H58	0.3528 (5)	0.3612 (14)	0.1841 (5)	0.020 (3)*
C42	0.39730 (3)	0.46480 (8)	0.10870 (3)	0.02000 (14)*
C43	0.39200 (2)	0.59350 (8)	0.08540 (3)	0.02000 (13)*
H59	0.3648 (4)	0.6403 (14)	0.0737 (5)	0.020 (3)*
C44	0.42890 (2)	0.65870 (8)	0.07870 (3)	0.02000 (13)*
H60	0.4257 (4)	0.7465 (15)	0.0622 (5)	0.020 (3)*
C45	0.46690 (2)	0.59010 (8)	0.09670 (3)	0.02000 (13)*
H61	0.4909 (4)	0.6305 (14)	0.0930 (5)	0.020 (3)*
C46	0.47160 (3)	0.46680 (8)	0.11950 (3)	0.02000 (14)*
H62	0.4985 (4)	0.4190 (14)	0.1313 (5)	0.020 (3)*
C47	0.43780 (3)	0.41010 (8)	0.12580 (3)	0.02000 (13)*
H63	0.4429 (5)	0.3244 (14)	0.1439 (5)	0.020 (3)*

Geometric parameters (Å, º) top

Si1—C4	1.8754 (9)	C19—C24	1.2964 (11)
Si1—C10	1.8813 (9)	C20—C21	1.3363 (11)
Si1—C7	1.8871 (8)	C20—H31	0.952 (13)
Si1—C1	1.8903 (8)	C21—C22	1.2185 (12)
N1—C14	1.3853 (10)	C21—H32	0.949 (14)
N1—C32	1.4031 (10)	C22—C23	1.3546 (11)
N1—C13	1.4570 (10)	C22—H33	0.948 (13)
O1—C11	1.2312 (10)	C23—C24	1.4404 (11)
O2—C15	1.4212 (10)	C23—H34	0.949 (14)
O2—C25	1.4444 (10)	C24—H35	0.951 (14)
O3—C16	1.2032 (10)	C25—C26	1.4752 (11)
O4—C18	1.3502 (9)	C25—H36	0.987 (14)
O4—C17	1.3973 (10)	C25—H37	0.990 (13)
O5—C32	1.1956 (11)	C26—C31	1.3516 (11)
O6—C32	1.3390 (10)	C26—C27	1.3633 (11)
O6—C33	1.4660 (10)	C27—C28	1.5449 (11)
C1—C3	1.5140 (11)	C27—H38	0.952 (13)
C1—C2	1.5312 (11)	C28—C29	1.4810 (11)
C1—H1	1.000 (14)	C28—H39	0.947 (13)
C2—H2	0.981 (14)	C29—C30	1.2656 (10)
C2—H3	0.979 (13)	C29—H40	0.950 (14)
C2—H4	0.978 (13)	C30—C31	1.2360 (11)
C3—H5	0.980 (13)	C30—H41	0.950 (14)
C3—H6	0.979 (13)	C31—H42	0.950 (13)
C3—H7	0.981 (14)	C33—C34	1.5021 (11)
C4—C6	1.5387 (11)	C33—C38	1.5260 (11)
C4—C5	1.5427 (11)	C33—H43	1.000 (13)
C4—H8	1.002 (13)	C34—C35	1.5296 (11)
C5—H9	0.979 (13)	C34—H44	0.992 (14)
C5—H10	0.979 (13)	C34—H45	0.992 (13)
C5—H11	0.982 (13)	C35—C36	1.4676 (11)
C6—H12	0.978 (13)	C35—H46	0.989 (13)
C6—H13	0.980 (13)	C35—H47	0.991 (14)
C6—H14	0.982 (13)	C36—C37	1.5131 (10)
C7—C8	1.5025 (11)	C36—H48	0.991 (13)
C7—C9	1.5364 (11)	C36—H49	0.989 (13)
C7—H15	1.000 (14)	C37—C38	1.5838 (11)
C8—H16	0.981 (13)	C37—H50	0.991 (13)
C8—H17	0.980 (14)	C37—H51	0.988 (14)
C8—H18	0.980 (13)	C38—C39	1.5385 (11)
C9—H19	0.980 (13)	C38—H52	1.000 (13)
C9—H20	0.981 (14)	C39—C42	1.5225 (11)
C9—H21	0.982 (13)	C39—C40	1.5310 (12)
C10—C14	1.3651 (11)	C39—C41	1.5633 (11)
C10—C11	1.4606 (11)	C40—H53	0.981 (13)
C11—C12	1.5049 (10)	C40—H54	0.981 (13)
C12—C13	1.5184 (11)	C40—H55	0.979 (13)
C12—H22	0.991 (13)	C41—H56	0.981 (13)
C12—H23	0.988 (13)	C41—H57	0.978 (14)
C13—C15	1.5656 (11)	C41—H58	0.979 (13)
C13—H24	1.000 (13)	C42—C47	1.3570 (11)
C14—H25	0.949 (14)	C42—C43	1.3788 (11)
C15—C16	1.5119 (12)	C43—C44	1.4845 (11)
C15—H26	0.997 (13)	C43—H59	0.952 (14)
C16—C17	1.5129 (10)	C44—C45	1.3433 (11)
C17—H27	0.991 (13)	C44—H60	0.950 (14)
C17—H28	0.991 (13)	C45—C46	1.3284 (10)
C18—C19	1.5534 (11)	C45—H61	0.948 (13)
C18—H29	0.988 (13)	C46—C47	1.3504 (12)
C18—H30	0.990 (14)	C46—H62	0.948 (13)
C19—C20	1.2695 (10)	C47—H63	0.950 (13)

C4—Si1—C10	107.92 (4)	C21—C20—H31	118.2 (8)
C4—Si1—C7	107.54 (4)	C22—C21—C20	123.55 (7)
C10—Si1—C7	108.65 (4)	C22—C21—H32	118.2 (8)
C4—Si1—C1	114.01 (4)	C20—C21—H32	118.2 (8)
C10—Si1—C1	110.15 (4)	C21—C22—C23	118.64 (7)
C7—Si1—C1	108.42 (4)	C21—C22—H33	120.6 (8)
C14—N1—C32	117.50 (7)	C23—C22—H33	120.8 (8)
C14—N1—C13	117.64 (6)	C22—C23—C24	116.35 (7)
C32—N1—C13	123.09 (6)	C22—C23—H34	121.8 (8)
C15—O2—C25	113.82 (6)	C24—C23—H34	121.8 (8)
C18—O4—C17	112.30 (6)	C19—C24—C23	121.11 (7)
C32—O6—C33	116.50 (6)	C19—C24—H35	119.5 (8)
C3—C1—C2	111.01 (6)	C23—C24—H35	119.4 (8)
C3—C1—Si1	115.29 (5)	O2—C25—C26	107.50 (6)
C2—C1—Si1	113.61 (5)	O2—C25—H36	110.1 (8)
C3—C1—H1	105.3 (7)	C26—C25—H36	110.1 (8)
C2—C1—H1	105.3 (7)	O2—C25—H37	110.2 (8)
Si1—C1—H1	105.2 (7)	C26—C25—H37	110.0 (8)
C1—C2—H2	109.3 (8)	H36—C25—H37	108.9 (11)
C1—C2—H3	109.4 (8)	C31—C26—C27	121.16 (7)
H2—C2—H3	109.4 (11)	C31—C26—C25	118.41 (7)
C1—C2—H4	109.4 (8)	C27—C26—C25	120.42 (7)
H2—C2—H4	109.5 (11)	C26—C27—C28	115.87 (7)
H3—C2—H4	109.7 (10)	C26—C27—H38	122.0 (8)
C1—C3—H5	109.5 (8)	C28—C27—H38	122.1 (8)
C1—C3—H6	109.7 (8)	C29—C28—C27	110.01 (7)
H5—C3—H6	109.3 (11)	C29—C28—H39	125.2 (8)
C1—C3—H7	109.6 (8)	C27—C28—H39	124.8 (8)
H5—C3—H7	109.5 (11)	C30—C29—C28	127.46 (7)
H6—C3—H7	109.3 (11)	C30—C29—H40	116.3 (8)
C6—C4—C5	108.25 (6)	C28—C29—H40	116.3 (8)
C6—C4—Si1	113.75 (6)	C31—C30—C29	117.89 (8)
C5—C4—Si1	115.45 (5)	C31—C30—H41	121.0 (8)
C6—C4—H8	106.2 (8)	C29—C30—H41	121.1 (8)
C5—C4—H8	106.1 (7)	C30—C31—C26	127.51 (8)
Si1—C4—H8	106.4 (8)	C30—C31—H42	116.3 (8)
C4—C5—H9	109.5 (8)	C26—C31—H42	116.1 (8)
C4—C5—H10	109.5 (8)	O5—C32—O6	126.46 (8)
H9—C5—H10	109.6 (11)	O5—C32—N1	123.78 (7)
C4—C5—H11	109.5 (8)	O6—C32—N1	109.72 (7)
H9—C5—H11	109.2 (10)	O6—C33—C34	107.54 (6)
H10—C5—H11	109.5 (11)	O6—C33—C38	107.56 (6)
C4—C6—H12	109.6 (8)	C34—C33—C38	112.28 (6)
C4—C6—H13	109.4 (8)	O6—C33—H43	109.8 (7)
H12—C6—H13	109.5 (12)	C34—C33—H43	109.8 (8)
C4—C6—H14	109.4 (8)	C38—C33—H43	109.8 (8)
H12—C6—H14	109.5 (11)	C33—C34—C35	112.01 (6)
H13—C6—H14	109.4 (11)	C33—C34—H44	109.2 (8)
C8—C7—C9	109.09 (6)	C35—C34—H44	109.2 (8)
C8—C7—Si1	114.46 (5)	C33—C34—H45	109.3 (8)
C9—C7—Si1	112.85 (6)	C35—C34—H45	109.3 (8)
C8—C7—H15	106.7 (8)	H44—C34—H45	107.8 (10)
C9—C7—H15	106.6 (8)	C36—C35—C34	108.97 (7)
Si1—C7—H15	106.6 (8)	C36—C35—H46	109.9 (7)
C7—C8—H16	109.5 (8)	C34—C35—H46	109.9 (8)
C7—C8—H17	109.6 (8)	C36—C35—H47	110.0 (8)
H16—C8—H17	109.4 (11)	C34—C35—H47	109.7 (8)
C7—C8—H18	109.5 (8)	H46—C35—H47	108.4 (11)
H16—C8—H18	109.4 (11)	C35—C36—C37	109.76 (6)
H17—C8—H18	109.5 (11)	C35—C36—H48	109.6 (8)
C7—C9—H19	109.5 (8)	C37—C36—H48	109.7 (8)
C7—C9—H20	109.5 (7)	C35—C36—H49	109.7 (8)
H19—C9—H20	109.7 (11)	C37—C36—H49	109.8 (8)
C7—C9—H21	109.5 (8)	H48—C36—H49	108.2 (11)
H19—C9—H21	109.6 (11)	C36—C37—C38	112.46 (6)
H20—C9—H21	109.1 (10)	C36—C37—H50	109.1 (8)
C14—C10—C11	116.43 (6)	C38—C37—H50	109.0 (8)
C14—C10—Si1	121.91 (6)	C36—C37—H51	109.2 (8)
C11—C10—Si1	121.65 (6)	C38—C37—H51	109.1 (8)
O1—C11—C10	121.74 (7)	H50—C37—H51	108.0 (11)
O1—C11—C12	119.33 (7)	C33—C38—C39	115.40 (6)
C10—C11—C12	118.89 (7)	C33—C38—C37	106.49 (6)
C11—C12—C13	112.78 (6)	C39—C38—C37	116.13 (6)
C11—C12—H22	108.9 (8)	C33—C38—H52	106.0 (8)
C13—C12—H22	108.9 (8)	C39—C38—H52	106.0 (8)
C11—C12—H23	109.1 (8)	C37—C38—H52	106.0 (8)
C13—C12—H23	109.1 (8)	C42—C39—C40	111.87 (6)
H22—C12—H23	107.9 (11)	C42—C39—C38	110.42 (6)
N1—C13—C12	109.34 (6)	C40—C39—C38	109.60 (6)
N1—C13—C15	109.43 (6)	C42—C39—C41	105.65 (6)
C12—C13—C15	110.01 (6)	C40—C39—C41	109.24 (6)
N1—C13—H24	109.6 (8)	C38—C39—C41	109.97 (6)
C12—C13—H24	109.2 (7)	C39—C40—H53	109.4 (8)
C15—C13—H24	109.3 (8)	C39—C40—H54	109.3 (8)
C10—C14—N1	125.34 (7)	H53—C40—H54	109.4 (11)
C10—C14—H25	117.2 (8)	C39—C40—H55	109.5 (8)
N1—C14—H25	117.4 (8)	H53—C40—H55	109.7 (11)
O2—C15—C16	112.29 (6)	H54—C40—H55	109.6 (11)
O2—C15—C13	107.30 (6)	C39—C41—H56	109.6 (8)
C16—C15—C13	110.13 (6)	C39—C41—H57	109.4 (8)
O2—C15—H26	108.9 (8)	H56—C41—H57	109.7 (11)
C16—C15—H26	109.2 (8)	C39—C41—H58	109.5 (8)
C13—C15—H26	109.0 (8)	H56—C41—H58	109.3 (11)
O3—C16—C15	121.26 (7)	H57—C41—H58	109.4 (12)
O3—C16—C17	123.34 (7)	C47—C42—C43	115.30 (8)
C15—C16—C17	115.40 (6)	C47—C42—C39	123.12 (7)
O4—C17—C16	108.74 (6)	C43—C42—C39	121.39 (7)
O4—C17—H27	110.0 (8)	C42—C43—C44	119.70 (7)
C16—C17—H27	109.9 (8)	C42—C43—H59	120.1 (8)
O4—C17—H28	109.9 (8)	C44—C43—H59	120.2 (8)
C16—C17—H28	109.8 (8)	C45—C44—C43	118.09 (7)
H27—C17—H28	108.4 (11)	C45—C44—H60	121.0 (8)
O4—C18—C19	113.95 (6)	C43—C44—H60	120.9 (7)
O4—C18—H29	108.7 (8)	C46—C45—C44	121.47 (8)
C19—C18—H29	108.9 (8)	C46—C45—H61	119.2 (8)
O4—C18—H30	108.7 (7)	C44—C45—H61	119.3 (8)
C19—C18—H30	108.6 (8)	C45—C46—C47	119.53 (8)
H29—C18—H30	107.7 (11)	C45—C46—H62	120.2 (8)
C20—C19—C24	116.54 (7)	C47—C46—H62	120.2 (8)
C20—C19—C18	127.30 (7)	C46—C47—C42	125.81 (7)
C24—C19—C18	115.81 (7)	C46—C47—H63	117.0 (8)
C19—C20—C21	123.60 (8)	C42—C47—H63	117.2 (8)
C19—C20—H31	118.2 (8)

(pejvab) bis(mu!2$-Ethane-1,2-dithiolato-S,S,S',S')-bis(ethene-1,2-dithiolato)- -technetium(iv) top

Crystal data top

C₈H₁₂S₈Tc₂	γ = 90°
M_r = 560.66	V = 844.2 (8) Å³
I2/m	Z = 2
a = 11.361 (6) Å	F(000) = 548
b = 8.303 (5) Å	D_x = 2.206 Mg m⁻³
c = 8.987 (5) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 2.61 mm⁻¹
β = 95.25 (5)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.016
Graphite monochromator	θ_max = 68.7°, θ_min = 2.8°
6858 measured reflections	h = −27→27
2519 independent reflections	k = −9→9
2178 reflections with I > 2σ(I)	l = −18→18

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.010	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.065	H atoms treated by a mixture of independent and constrained refinement
S = 0.42	w = 1/[σ²(F_o²) + (0.P)² + 0.0178P] where P = (F_o² + 2F_c²)/3
2519 reflections	(Δ/σ)_max = 2.510
38 parameters	Δρ_max = 0.87 e Å⁻³
0 restraints	Δρ_min = −1.25 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Tc1	0.401300 (6)	0.0000	0.063600 (7)	0.02000 (4)*
S1	0.436700 (15)	0.17480 (3)	−0.138900 (19)	0.02000 (4)*
S3	0.20160 (2)	0.0000	−0.00570 (3)	0.02000 (5)*
S4	0.34530 (2)	0.0000	0.30230 (3)	0.02000 (5)*
C1	0.36160 (7)	0.08990 (10)	−0.31090 (8)	0.02000 (10)*
C3	0.12240 (9)	0.0000	0.16090 (10)	0.02000 (12)*
C4	0.18580 (9)	0.0000	0.30030 (11)	0.02000 (12)*
H1	0.4060 (14)	0.131 (2)	−0.4050 (19)	0.020 (3)*
H2	0.2713 (13)	0.132 (2)	−0.3223 (17)	0.020 (3)*
H5	0.0275 (19)	0.0000	0.152 (3)	0.020 (5)*
H6	0.142 (2)	0.0000	0.400 (3)	0.020 (5)*

Geometric parameters (Å, º) top

Tc1—S4	2.2927 (13)	S3—C3	1.8160 (14)
Tc1—S3	2.2971 (13)	S4—C4	1.8105 (14)
Tc1—S1ⁱ	2.3904 (10)	C1—C1ⁱ	1.4929 (19)
Tc1—S1	2.3904 (10)	C1—H1	1.080 (16)
Tc1—S1ⁱⁱ	2.3925 (10)	C1—H2	1.079 (15)
Tc1—S1ⁱⁱⁱ	2.3925 (10)	C3—C4	1.3868 (17)
Tc1—Tc1ⁱⁱⁱ	2.6087 (14)	C3—H5	1.07 (2)
S1—C1	1.8366 (12)	C4—H6	1.06 (2)
S1—Tc1ⁱⁱⁱ	2.3925 (10)

S4—Tc1—S3	84.37 (5)	S1ⁱⁱ—Tc1—Tc1ⁱⁱⁱ	56.91 (3)
S4—Tc1—S1ⁱ	142.44 (2)	S1ⁱⁱⁱ—Tc1—Tc1ⁱⁱⁱ	56.91 (3)
S3—Tc1—S1ⁱ	91.40 (4)	C1—S1—Tc1	108.07 (5)
S4—Tc1—S1	142.44 (2)	C1—S1—Tc1ⁱⁱⁱ	106.94 (5)
S3—Tc1—S1	91.40 (4)	Tc1—S1—Tc1ⁱⁱⁱ	66.11 (4)
S1ⁱ—Tc1—S1	74.77 (5)	C3—S3—Tc1	109.15 (6)
S4—Tc1—S1ⁱⁱ	90.43 (4)	C4—S4—Tc1	110.73 (6)
S3—Tc1—S1ⁱⁱ	142.36 (2)	C1ⁱ—C1—S1	112.57 (3)
S1ⁱ—Tc1—S1ⁱⁱ	113.89 (4)	C1ⁱ—C1—H1	108.6 (9)
S1—Tc1—S1ⁱⁱ	70.63 (4)	S1—C1—H1	108.8 (9)
S4—Tc1—S1ⁱⁱⁱ	90.43 (4)	C1ⁱ—C1—H2	108.8 (9)
S3—Tc1—S1ⁱⁱⁱ	142.36 (2)	S1—C1—H2	108.7 (8)
S1ⁱ—Tc1—S1ⁱⁱⁱ	70.63 (4)	H1—C1—H2	109.3 (12)
S1—Tc1—S1ⁱⁱⁱ	113.89 (4)	C4—C3—S3	119.29 (9)
S1ⁱⁱ—Tc1—S1ⁱⁱⁱ	74.69 (5)	C4—C3—H5	120.4 (12)
S4—Tc1—Tc1ⁱⁱⁱ	137.16 (3)	S3—C3—H5	120.3 (12)
S3—Tc1—Tc1ⁱⁱⁱ	138.46 (3)	C3—C4—S4	116.46 (9)
S1ⁱ—Tc1—Tc1ⁱⁱⁱ	56.98 (3)	C3—C4—H6	121.5 (12)
S1—Tc1—Tc1ⁱⁱⁱ	56.98 (3)	S4—C4—H6	122.1 (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

C₂₃H₂₅F₆NP₂Pd	γ = 90°
M_r = 597.78	V = 2425.1 (17) Å³
Ia	Z = 4
a = 15.197 (6) Å	F(000) = 1200
b = 9.042 (3) Å	D_x = 1.637 Mg m⁻³
c = 18.559 (9) Å	Mo Kα radiation, λ = 0.71070 Å
α = 90°	µ = 0.96 mm⁻¹
β = 108.02 (4)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.013
Graphite monochromator	θ_max = 44.9°, θ_min = 2.3°
9712 measured reflections	h = −22→22
6772 independent reflections	k = −9→9
6443 reflections with I > 2σ(I)	l = −31→31

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.009	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.032	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
S = 0.16	(Δ/σ)_max = 0.783
6772 reflections	Δρ_max = 0.18 e Å⁻³
233 parameters	Δρ_min = −0.19 e Å⁻³
2 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.004 (6)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pd1	0.136600 (4)	0.277800 (6)	0.071000 (4)	0.02000 (2)*
P1	0.286000 (16)	0.33420 (2)	0.131900 (14)	0.02000 (4)*
N1	0.13570 (5)	0.18680 (10)	0.17890 (4)	0.02000 (11)*
C1	0.30530 (7)	0.22880 (9)	0.22060 (6)	0.02000 (17)*
C2	0.39300 (7)	0.20910 (9)	0.27130 (6)	0.02000 (16)*
H1	0.4442 (11)	0.2513 (16)	0.2619 (9)	0.020 (3)*
C3	0.40390 (6)	0.12530 (10)	0.33660 (5)	0.02000 (13)*
H2	0.4625 (9)	0.1100 (15)	0.3708 (7)	0.020 (3)*
C4	0.32860 (6)	0.06680 (10)	0.34950 (5)	0.02000 (13)*
H3	0.3360 (9)	0.0136 (15)	0.3939 (7)	0.020 (3)*
C5	0.24160 (6)	0.08290 (10)	0.29960 (5)	0.02000 (13)*
H4	0.1908 (9)	0.0399 (15)	0.3094 (8)	0.020 (3)*
C6	0.23010 (6)	0.16590 (9)	0.23270 (5)	0.02000 (15)*
C7	0.08630 (6)	0.04110 (9)	0.16260 (5)	0.02000 (14)*
H5	0.0254 (9)	0.0556 (15)	0.1278 (8)	0.020 (3)*
H6	0.0816 (9)	−0.0003 (16)	0.2090 (8)	0.020 (3)*
H7	0.1202 (9)	−0.0253 (15)	0.1407 (7)	0.020 (3)*
C8	0.08270 (7)	0.29020 (9)	0.21360 (6)	0.02000 (16)*
H8	0.0216 (10)	0.3045 (16)	0.1791 (8)	0.020 (3)*
H9	0.1142 (9)	0.3835 (16)	0.2239 (8)	0.020 (3)*
H10	0.0786 (11)	0.2485 (16)	0.2600 (9)	0.020 (3)*
C9	−0.01070 (7)	0.27000 (9)	−0.00150 (6)	0.02000 (17)*
H11	−0.0438 (10)	0.1782 (16)	−0.0015 (8)	0.020 (3)*
H12	−0.0477 (10)	0.3578 (16)	−0.0023 (8)	0.020 (3)*
C10	0.04710 (7)	0.27330 (8)	−0.04370 (6)	0.02000 (17)*
H13	0.0358 (11)	0.2043 (16)	−0.0827 (9)	0.020 (3)*
C11	0.11920 (6)	0.36460 (11)	−0.03620 (5)	0.02000 (13)*
H14	0.1047 (9)	0.4692 (15)	−0.0424 (7)	0.020 (3)*
H15	0.1639 (10)	0.3335 (15)	−0.0607 (8)	0.020 (3)*
C12	0.37580 (7)	0.28290 (8)	0.09130 (6)	0.02000 (17)*
C13	0.35470 (6)	0.18820 (12)	0.02930 (5)	0.02000 (12)*
H31	0.2942 (10)	0.1451 (15)	0.0104 (8)	0.020 (3)*
C14	0.42180 (6)	0.15360 (9)	−0.00470 (5)	0.02000 (15)*
H32	0.4076 (9)	0.0873 (16)	−0.0472 (8)	0.020 (3)*
C15	0.51000 (7)	0.21400 (9)	0.02340 (6)	0.02000 (17)*
H33	0.5563 (10)	0.1906 (17)	−0.0003 (8)	0.020 (3)*
C16	0.53110 (6)	0.30870 (11)	0.08530 (5)	0.02000 (12)*
H34	0.5917 (9)	0.3517 (15)	0.1041 (8)	0.020 (3)*
C17	0.46400 (6)	0.34320 (9)	0.11930 (5)	0.02000 (15)*
H35	0.4783 (9)	0.4095 (15)	0.1617 (8)	0.020 (3)*
C18	0.30760 (6)	0.52580 (10)	0.15740 (5)	0.02000 (13)*
C19	0.29680 (6)	0.62700 (10)	0.09890 (5)	0.02000 (13)*
H36	0.2787 (9)	0.5931 (16)	0.0474 (8)	0.020 (3)*
C20	0.31250 (7)	0.77660 (9)	0.11520 (6)	0.02000 (17)*
H37	0.3056 (9)	0.8460 (15)	0.0747 (8)	0.020 (3)*
C21	0.33920 (6)	0.82500 (10)	0.18990 (5)	0.02000 (14)*
H38	0.3505 (9)	0.9282 (16)	0.2010 (8)	0.020 (3)*
C22	0.35010 (7)	0.72370 (8)	0.24840 (6)	0.02000 (18)*
H39	0.3685 (11)	0.7576 (16)	0.3000 (9)	0.020 (3)*
C23	0.33440 (6)	0.57430 (10)	0.23220 (5)	0.02000 (13)*
H40	0.3416 (9)	0.5048 (15)	0.2728 (7)	0.020 (3)*
P2	0.170000 (15)	0.63070 (3)	0.375400 (13)	0.02000 (4)*
F1	0.15630 (3)	0.68450 (7)	0.29300 (3)	0.02000 (8)*
F2	0.18200 (3)	0.57270 (6)	0.45920 (3)	0.02000 (9)*
F3	0.27140 (4)	0.69320 (7)	0.40210 (3)	0.02000 (9)*
F4	0.13170 (4)	0.78090 (5)	0.39450 (4)	0.02000 (12)*
F5	0.20920 (3)	0.47680 (6)	0.35770 (3)	0.02000 (9)*
F6	0.06910 (4)	0.56400 (6)	0.34930 (3)	0.02000 (9)*

Geometric parameters (Å, º) top

Pd1—C11	2.0781 (13)	C10—H13	0.930 (15)
Pd1—C10	2.1428 (16)	C11—H14	0.970 (14)
Pd1—N1	2.1689 (12)	C11—H15	0.969 (14)
Pd1—C9	2.2278 (15)	C12—C13	1.3899 (15)
Pd1—P1	2.2594 (11)	C12—C17	1.3903 (14)
P1—C18	1.7992 (11)	C13—C14	1.3907 (15)
P1—C12	1.8115 (13)	C13—H31	0.960 (14)
P1—C1	1.8454 (12)	C14—C15	1.3908 (14)
N1—C6	1.4848 (13)	C14—H32	0.961 (14)
N1—C7	1.5001 (13)	C15—C16	1.3885 (14)
N1—C8	1.5028 (13)	C15—H33	0.962 (15)
C1—C6	1.3560 (14)	C16—C17	1.3905 (15)
C1—C2	1.3847 (15)	C16—H34	0.960 (14)
C2—C3	1.3950 (14)	C17—H35	0.959 (13)
C2—H1	0.930 (16)	C18—C19	1.3902 (13)
C3—C4	1.3476 (13)	C18—C23	1.3912 (14)
C3—H2	0.930 (12)	C19—C20	1.3905 (13)
C4—C5	1.3672 (13)	C19—H36	0.959 (14)
C4—H3	0.930 (13)	C20—C21	1.3893 (15)
C5—C6	1.4146 (14)	C20—H37	0.960 (14)
C5—H4	0.931 (13)	C21—C22	1.3906 (14)
C7—H5	0.960 (13)	C21—H38	0.960 (14)
C7—H6	0.962 (14)	C22—C23	1.3885 (13)
C7—H7	0.959 (13)	C22—H39	0.961 (16)
C8—H8	0.960 (14)	C23—H40	0.961 (13)
C8—H9	0.960 (14)	P2—F1	1.5562 (9)
C8—H10	0.960 (16)	P2—F4	1.5609 (7)
C9—C10	1.3459 (17)	P2—F3	1.5707 (8)
C9—H11	0.971 (15)	P2—F6	1.5780 (8)
C9—H12	0.970 (14)	P2—F5	1.5876 (7)
C10—C11	1.3443 (14)	P2—F2	1.5974 (9)

C11—Pd1—C10	37.10 (4)	C11—C10—H13	116.1 (10)
C11—Pd1—N1	172.71 (3)	C9—C10—H13	116.2 (10)
C10—Pd1—N1	136.61 (4)	Pd1—C10—H13	133.9 (9)
C11—Pd1—C9	68.11 (5)	C10—C11—Pd1	74.06 (7)
C10—Pd1—C9	35.80 (5)	C10—C11—H14	116.0 (8)
N1—Pd1—C9	104.68 (5)	Pd1—C11—H14	116.0 (8)
C11—Pd1—P1	101.79 (4)	C10—C11—H15	116.1 (8)
C10—Pd1—P1	137.06 (4)	Pd1—C11—H15	116.1 (8)
N1—Pd1—P1	85.19 (4)	H14—C11—H15	113.2 (11)
C9—Pd1—P1	167.37 (3)	C13—C12—C17	119.99 (10)
C18—P1—C12	104.85 (4)	C13—C12—P1	119.44 (8)
C18—P1—C1	107.27 (5)	C17—C12—P1	120.49 (8)
C12—P1—C1	107.85 (5)	C12—C13—C14	120.03 (9)
C18—P1—Pd1	114.98 (3)	C12—C13—H31	120.2 (9)
C12—P1—Pd1	120.26 (4)	C14—C13—H31	119.8 (9)
C1—P1—Pd1	100.81 (5)	C13—C14—C15	119.89 (9)
C6—N1—C7	110.06 (7)	C13—C14—H32	120.2 (8)
C6—N1—C8	108.99 (8)	C15—C14—H32	119.9 (8)
C7—N1—C8	109.37 (7)	C16—C15—C14	120.10 (10)
C6—N1—Pd1	112.86 (7)	C16—C15—H33	120.0 (9)
C7—N1—Pd1	107.02 (6)	C14—C15—H33	119.9 (9)
C8—N1—Pd1	108.48 (6)	C15—C16—C17	119.98 (9)
C6—C1—C2	121.12 (10)	C15—C16—H34	120.0 (8)
C6—C1—P1	117.05 (8)	C17—C16—H34	120.0 (8)
C2—C1—P1	121.77 (8)	C12—C17—C16	120.00 (9)
C1—C2—C3	119.40 (10)	C12—C17—H35	120.0 (8)
C1—C2—H1	120.3 (10)	C16—C17—H35	120.0 (8)
C3—C2—H1	120.3 (10)	C19—C18—C23	119.95 (9)
C4—C3—C2	119.23 (9)	C19—C18—P1	117.42 (7)
C4—C3—H2	120.4 (8)	C23—C18—P1	122.63 (7)
C2—C3—H2	120.3 (8)	C18—C19—C20	119.97 (9)
C3—C4—C5	122.29 (9)	C18—C19—H36	119.7 (8)
C3—C4—H3	118.9 (8)	C20—C19—H36	120.3 (8)
C5—C4—H3	118.8 (8)	C21—C20—C19	120.07 (9)
C4—C5—C6	118.82 (9)	C21—C20—H37	120.2 (8)
C4—C5—H4	120.6 (8)	C19—C20—H37	119.7 (8)
C6—C5—H4	120.5 (8)	C20—C21—C22	119.94 (9)
C1—C6—C5	119.09 (9)	C20—C21—H38	119.9 (8)
C1—C6—N1	121.58 (9)	C22—C21—H38	120.2 (8)
C5—C6—N1	119.28 (8)	C23—C22—C21	120.05 (10)
N1—C7—H5	109.5 (8)	C23—C22—H39	120.2 (9)
N1—C7—H6	109.4 (8)	C21—C22—H39	119.7 (9)
H5—C7—H6	109.4 (11)	C22—C23—C18	120.03 (9)
N1—C7—H7	109.5 (8)	C22—C23—H40	119.7 (8)
H5—C7—H7	109.4 (11)	C18—C23—H40	120.2 (8)
H6—C7—H7	109.5 (12)	F1—P2—F4	90.30 (4)
N1—C8—H8	109.5 (9)	F1—P2—F3	91.00 (5)
N1—C8—H9	109.4 (8)	F4—P2—F3	90.78 (4)
H8—C8—H9	109.5 (12)	F1—P2—F6	89.77 (5)
N1—C8—H10	109.4 (9)	F4—P2—F6	90.40 (4)
H8—C8—H10	109.5 (13)	F3—P2—F6	178.58 (3)
H9—C8—H10	109.5 (12)	F1—P2—F5	90.88 (4)
C10—C9—Pd1	68.66 (7)	F4—P2—F5	178.82 (4)
C10—C9—H11	116.8 (9)	F3—P2—F5	89.22 (4)
Pd1—C9—H11	116.8 (9)	F6—P2—F5	89.58 (4)
C10—C9—H12	116.9 (8)	F1—P2—F2	178.59 (3)
Pd1—C9—H12	116.9 (8)	F4—P2—F2	90.16 (4)
H11—C9—H12	113.7 (13)	F3—P2—F2	90.32 (5)
C11—C10—C9	127.67 (9)	F6—P2—F2	88.90 (5)
C11—C10—Pd1	68.83 (6)	F5—P2—F2	88.66 (4)
C9—C10—Pd1	75.54 (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

C₄₆H₇₈Ce₂Cl₆N₆O₂₀	γ = 90°
M_r = 1528.08	V = 1670.7 (12) Å³
P2₁/m	Z = 1
a = 10.983 (5) Å	F(000) = 774
b = 16.960 (6) Å	D_x = 1.519 Mg m⁻³
c = 9.058 (4) Å	Mo Kα radiation, λ = 0.71073 Å
α = 90°	µ = 1.65 mm⁻¹
β = 98.03 (7)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.014
Graphite monochromator	θ_max = 43.2°, θ_min = 1.9°
17852 measured reflections	h = −11→11
4588 independent reflections	k = −18→18
4555 reflections with I > 2σ(I)	l = −10→10

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.065	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.163	H atoms treated by a mixture of independent and constrained refinement
S = 1.17	w = 1/[σ²(F_o²) + (0.P)² + 11.9541P] where P = (F_o² + 2F_c²)/3
4588 reflections	(Δ/σ)_max = 165.835
93 parameters	Δρ_max = 1.97 e Å⁻³
0 restraints	Δρ_min = −3.41 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ce1	0.15730 (3)	0.2500	0.66210 (4)	0.02000 (12)*
Cl1	0.16990 (15)	0.2500	0.15380 (16)	0.0200 (3)*
Cl2	0.42720 (14)	0.89250 (9)	0.31880 (15)	0.0200 (3)*	0.75
Cl3	0.3277 (4)	0.4726 (3)	0.5107 (5)	0.0200 (7)*	0.25
O1	0.2309 (3)	0.3593 (2)	0.8124 (4)	0.0200 (6)*
O3	0.0247 (3)	0.1139 (2)	0.6306 (4)	0.0200 (6)*
O4	−0.0668 (5)	0.2500	0.5286 (5)	0.0200 (9)*
O6	0.3912 (5)	0.2500	0.7006 (5)	0.0200 (9)*
O7	0.0117 (5)	0.2500	0.8672 (5)	0.0200 (9)*
O8	0.2016 (3)	0.1629 (2)	0.4463 (4)	0.0200 (6)*
O10	−0.2437 (5)	0.2500	0.7946 (5)	0.0200 (9)*
N1	0.3911 (4)	0.4032 (2)	1.0422 (4)	0.0200 (7)*
N2	0.5127 (5)	0.2500	1.1447 (6)	0.0200 (10)*
C1	−0.0030 (4)	0.5107 (3)	0.7561 (5)	0.0200 (8)*
C2	0.0441 (4)	0.5651 (3)	0.8644 (5)	0.0200 (8)*
C3	0.1544 (4)	0.5495 (3)	0.9557 (5)	0.0200 (8)*
C4	0.2174 (4)	0.4797 (3)	0.9388 (5)	0.0200 (8)*
C5	0.1703 (5)	0.4254 (3)	0.8304 (5)	0.0200 (8)*
C6	0.0601 (4)	0.4409 (3)	0.7391 (5)	0.0200 (8)*
C7	0.3252 (4)	0.4660 (3)	1.0417 (5)	0.0200 (8)*
C8	0.4964 (4)	0.3916 (3)	1.1504 (5)	0.0200 (8)*
C9	0.5090 (4)	0.3187 (3)	1.2346 (5)	0.0200 (8)*
C10	0.6113 (6)	0.2500	1.0641 (7)	0.0200 (11)*
C20	−0.0967 (4)	0.1128 (3)	0.5570 (5)	0.0200 (8)*
C21	−0.1093 (4)	0.1780 (3)	0.4492 (5)	0.0200 (8)*

Geometric parameters (Å, º) top

Ce1—O1	2.374 (4)	N1—C8	1.421 (6)
Ce1—O1ⁱ	2.374 (4)	N2—C10	1.388 (9)
Ce1—O6	2.544 (5)	N2—C9	1.425 (6)
Ce1—O8ⁱ	2.551 (4)	N2—C9ⁱ	1.425 (6)
Ce1—O8	2.551 (4)	C1—C6	1.391 (7)
Ce1—O4	2.586 (5)	C1—C2	1.393 (6)
Ce1—O7	2.615 (5)	C2—C3	1.393 (7)
Ce1—O3	2.723 (4)	C3—C4	1.390 (7)
Ce1—O3ⁱ	2.723 (4)	C4—C5	1.392 (7)
O1—C5	1.325 (6)	C4—C7	1.420 (7)
O3—C6ⁱ	1.369 (6)	C5—C6	1.392 (7)
O3—C20	1.405 (6)	C6—O3ⁱ	1.369 (6)
O4—C21	1.460 (5)	C8—C9	1.449 (7)
O4—C21ⁱ	1.460 (5)	C20—C21	1.469 (7)
N1—C7	1.287 (6)

O1—Ce1—O1ⁱ	102.68 (17)	O8—Ce1—O3ⁱ	124.55 (11)
O1—Ce1—O6	70.42 (11)	O4—Ce1—O3ⁱ	59.39 (8)
O1ⁱ—Ce1—O6	70.42 (11)	O7—Ce1—O3ⁱ	72.74 (9)
O1—Ce1—O8ⁱ	84.33 (12)	O3—Ce1—O3ⁱ	115.93 (15)
O1ⁱ—Ce1—O8ⁱ	143.67 (12)	C5—O1—Ce1	126.5 (3)
O6—Ce1—O8ⁱ	78.93 (13)	C6ⁱ—O3—C20	119.2 (4)
O1—Ce1—O8	143.67 (12)	C6ⁱ—O3—Ce1	114.0 (3)
O1ⁱ—Ce1—O8	84.33 (12)	C20—O3—Ce1	121.3 (3)
O6—Ce1—O8	78.93 (13)	C21—O4—C21ⁱ	113.5 (5)
O8ⁱ—Ce1—O8	70.78 (16)	C21—O4—Ce1	116.6 (3)
O1—Ce1—O4	119.58 (10)	C21ⁱ—O4—Ce1	116.6 (3)
O1ⁱ—Ce1—O4	119.58 (10)	C7—N1—C8	121.3 (4)
O6—Ce1—O4	160.22 (16)	C10—N2—C9	112.8 (4)
O8ⁱ—Ce1—O4	84.99 (13)	C10—N2—C9ⁱ	112.8 (4)
O8—Ce1—O4	84.99 (13)	C9—N2—C9ⁱ	109.7 (5)
O1—Ce1—O7	77.62 (11)	C6—C1—C2	120.0 (4)
O1ⁱ—Ce1—O7	77.62 (11)	C1—C2—C3	119.9 (4)
O6—Ce1—O7	127.49 (16)	C4—C3—C2	120.1 (4)
O8ⁱ—Ce1—O7	138.20 (10)	C3—C4—C5	120.0 (4)
O8—Ce1—O7	138.20 (10)	C3—C4—C7	116.7 (4)
O4—Ce1—O7	72.28 (16)	C5—C4—C7	123.3 (5)
O1—Ce1—O3	148.91 (11)	O1—C5—C4	120.2 (4)
O1ⁱ—Ce1—O3	62.12 (12)	O1—C5—C6	119.8 (4)
O6—Ce1—O3	121.97 (8)	C4—C5—C6	120.0 (4)
O8ⁱ—Ce1—O3	124.55 (11)	O3ⁱ—C6—C1	124.1 (4)
O8—Ce1—O3	65.49 (11)	O3ⁱ—C6—C5	115.7 (4)
O4—Ce1—O3	59.39 (8)	C1—C6—C5	120.0 (4)
O7—Ce1—O3	72.74 (9)	N1—C7—C4	123.7 (4)
O1—Ce1—O3ⁱ	62.12 (12)	N1—C8—C9	119.3 (4)
O1ⁱ—Ce1—O3ⁱ	148.91 (11)	N2—C9—C8	113.9 (4)
O6—Ce1—O3ⁱ	121.97 (8)	O3—C20—C21	107.5 (4)
O8ⁱ—Ce1—O3ⁱ	65.49 (11)	O4—C21—C20	107.9 (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

C₄₆H₇₈Cl₆Dy₂N₆O₂₀	γ = 90°
M_r = 1572.84	V = 1634.8 (12) Å³
P2₁/m	Z = 1
a = 10.870 (5) Å	F(000) = 790
b = 16.785 (6) Å	D_x = 1.598 Mg m⁻³
c = 9.046 (4) Å	Mo Kα radiation, λ = 0.71073 Å
α = 90°	µ = 2.58 mm⁻¹
β = 97.91 (8)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.018
Graphite monochromator	θ_max = 43.5°, θ_min = 1.9°
17852 measured reflections	h = −11→11
4588 independent reflections	k = −18→18
4539 reflections with I > 2σ(I)	l = −10→10

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.129	H atoms treated by a mixture of independent and constrained refinement
S = 1.20	w = 1/[σ²(F_o²) + (0.P)² + 5.4182P] where P = (F_o² + 2F_c²)/3
4588 reflections	(Δ/σ)_max = 61.082
93 parameters	Δρ_max = 2.33 e Å⁻³
0 restraints	Δρ_min = −2.63 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Dy1	0.15690 (2)	0.2500	0.66630 (3)	0.02000 (9)*
Cl1	0.16210 (12)	0.2500	0.16360 (14)	0.0200 (3)*
Cl2	0.42750 (12)	0.89130 (8)	0.31740 (14)	0.0200 (2)*	0.75
Cl3	0.3243 (4)	0.4745 (2)	0.5197 (4)	0.0200 (6)*	0.25
O1	0.2307 (3)	0.35530 (18)	0.8130 (3)	0.0200 (5)*
O3	0.0256 (3)	0.11750 (18)	0.6345 (3)	0.0200 (5)*
O4	−0.0559 (4)	0.2500	0.5190 (5)	0.0200 (8)*
O6	0.3815 (4)	0.2500	0.6989 (5)	0.0200 (8)*
O7	0.0173 (4)	0.2500	0.8499 (5)	0.0200 (8)*
O8	0.2001 (3)	0.16530 (19)	0.4627 (3)	0.0200 (5)*
O10	−0.2365 (4)	0.2500	0.7849 (5)	0.0200 (8)*
N1	0.3949 (3)	0.4000 (2)	1.0434 (4)	0.0200 (6)*
N2	0.5169 (5)	0.2500	1.1572 (6)	0.0200 (9)*
C1	−0.0028 (4)	0.5095 (2)	0.7595 (4)	0.0200 (7)*
C2	0.0446 (4)	0.5635 (2)	0.8698 (4)	0.0200 (7)*
C3	0.1553 (4)	0.5470 (3)	0.9617 (4)	0.0200 (7)*
C4	0.2189 (4)	0.4765 (3)	0.9433 (4)	0.0200 (7)*
C5	0.1716 (4)	0.4225 (3)	0.8329 (4)	0.0200 (7)*
C6	0.0608 (4)	0.4390 (3)	0.7414 (4)	0.0200 (7)*
C7	0.3266 (4)	0.4629 (2)	1.0433 (5)	0.0200 (7)*
C8	0.5143 (4)	0.3905 (3)	1.1475 (4)	0.0200 (7)*
C9	0.5143 (4)	0.3217 (2)	1.2395 (5)	0.0200 (7)*
C10	0.6269 (6)	0.2500	1.0768 (6)	0.0200 (10)*
C20	−0.0944 (4)	0.1143 (3)	0.5526 (4)	0.0200 (7)*
C21	−0.1028 (4)	0.1787 (2)	0.4404 (5)	0.0200 (7)*

Geometric parameters (Å, º) top

Dy1—O1	2.288 (3)	N1—C8	1.503 (5)
Dy1—O1ⁱ	2.288 (3)	N2—C9	1.417 (5)
Dy1—O7	2.399 (5)	N2—C9ⁱ	1.417 (5)
Dy1—O6	2.419 (5)	N2—C10	1.483 (8)
Dy1—O8	2.423 (3)	C1—C6	1.391 (6)
Dy1—O8ⁱ	2.423 (3)	C1—C2	1.393 (6)
Dy1—O4	2.506 (5)	C2—C3	1.393 (6)
Dy1—O3	2.637 (3)	C3—C4	1.392 (6)
Dy1—O3ⁱ	2.637 (3)	C4—C5	1.394 (6)
O1—C5	1.323 (5)	C4—C7	1.396 (6)
O3—C6ⁱ	1.371 (5)	C5—C6	1.392 (6)
O3—C20	1.410 (5)	C6—O3ⁱ	1.371 (5)
O4—C21	1.448 (5)	C8—C9	1.423 (6)
O4—C21ⁱ	1.448 (5)	C20—C21	1.477 (6)
N1—C7	1.291 (5)

O1—Dy1—O1ⁱ	101.15 (16)	O8—Dy1—O3ⁱ	124.79 (10)
O1—Dy1—O7	78.65 (10)	O8ⁱ—Dy1—O3ⁱ	65.22 (11)
O1ⁱ—Dy1—O7	78.65 (10)	O4—Dy1—O3ⁱ	59.72 (7)
O1—Dy1—O6	70.23 (11)	O3—Dy1—O3ⁱ	115.01 (14)
O1ⁱ—Dy1—O6	70.23 (11)	C5—O1—Dy1	126.8 (3)
O7—Dy1—O6	129.77 (15)	C6ⁱ—O3—C20	119.5 (3)
O1—Dy1—O8	143.60 (11)	C6ⁱ—O3—Dy1	114.3 (2)
O1ⁱ—Dy1—O8	84.17 (11)	C20—O3—Dy1	122.5 (2)
O7—Dy1—O8	137.17 (9)	C21—O4—C21ⁱ	111.4 (4)
O6—Dy1—O8	78.15 (12)	C21—O4—Dy1	119.9 (2)
O1—Dy1—O8ⁱ	84.17 (11)	C21ⁱ—O4—Dy1	119.9 (2)
O1ⁱ—Dy1—O8ⁱ	143.60 (11)	C7—N1—C8	122.3 (4)
O7—Dy1—O8ⁱ	137.17 (9)	C9—N2—C9ⁱ	116.2 (5)
O6—Dy1—O8ⁱ	78.15 (12)	C9—N2—C10	109.5 (3)
O8—Dy1—O8ⁱ	71.85 (15)	C9ⁱ—N2—C10	109.5 (3)
O1—Dy1—O4	122.19 (9)	C6—C1—C2	119.8 (4)
O1ⁱ—Dy1—O4	122.19 (9)	C3—C2—C1	120.1 (4)
O7—Dy1—O4	75.08 (15)	C4—C3—C2	120.0 (4)
O6—Dy1—O4	155.15 (14)	C3—C4—C5	119.9 (4)
O8—Dy1—O4	81.78 (12)	C3—C4—C7	116.6 (4)
O8ⁱ—Dy1—O4	81.78 (12)	C5—C4—C7	123.5 (4)
O1—Dy1—O3	148.88 (10)	O1—C5—C6	119.0 (4)
O1ⁱ—Dy1—O3	63.45 (11)	O1—C5—C4	120.9 (4)
O7—Dy1—O3	72.01 (9)	C6—C5—C4	120.0 (4)
O6—Dy1—O3	122.37 (7)	O3ⁱ—C6—C1	125.2 (4)
O8—Dy1—O3	65.22 (11)	O3ⁱ—C6—C5	114.6 (4)
O8ⁱ—Dy1—O3	124.79 (10)	C1—C6—C5	120.2 (4)
O4—Dy1—O3	59.72 (7)	N1—C7—C4	124.4 (4)
O1—Dy1—O3ⁱ	63.45 (11)	C9—C8—N1	112.5 (4)
O1ⁱ—Dy1—O3ⁱ	148.88 (10)	N2—C9—C8	112.3 (4)
O7—Dy1—O3ⁱ	72.01 (8)	O3—C20—C21	107.4 (3)
O6—Dy1—O3ⁱ	122.37 (7)	O4—C21—C20	106.4 (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

C₃₃H₅₇ClO₆Zr	γ = 90°
M_r = 676.46	V = 1895.2 (14) Å³
P2₁/m	Z = 2
a = 10.679 (5) Å	F(000) = 720
b = 18.263 (7) Å	D_x = 1.185 Mg m⁻³
c = 10.973 (5) Å	Mo Kα radiation, λ = 0.71073 Å
α = 90°	µ = 0.40 mm⁻¹
β = 117.68 (5)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.006
Graphite monochromator	θ_max = 52.2°, θ_min = 2.1°
20610 measured reflections	h = −11→11
5289 independent reflections	k = −19→19
5255 reflections with I > 2σ(I)	l = −11→11

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.221	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.395	H atoms treated by a mixture of independent and constrained refinement
S = 0.74	w = 1/[σ²(F_o²) + (0.P)² + 181.8093P] where P = (F_o² + 2F_c²)/3
5289 reflections	(Δ/σ)_max = 90.043
96 parameters	Δρ_max = 4.04 e Å⁻³
0 restraints	Δρ_min = −7.23 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Zr1	0.84820 (13)	0.2500	0.37470 (13)	0.0200 (3)*
Cl1	0.7498 (3)	0.2500	0.1192 (3)	0.0200 (6)*
O1	1.0691 (10)	0.2500	0.5131 (9)	0.0200 (17)*
O2	0.8539 (10)	0.2500	0.5706 (9)	0.0200 (17)*
O3	0.6790 (7)	0.3235 (4)	0.3429 (6)	0.0200 (13)*
O4	0.9232 (7)	0.3537 (4)	0.3519 (6)	0.0200 (12)*
C1	1.3069 (13)	0.2500	0.6871 (13)	0.020 (2)*
C2	1.3724 (9)	0.1878 (5)	0.7679 (9)	0.0200 (16)*
C3	1.3349 (13)	0.2500	0.5742 (13)	0.020 (2)*
C5	1.1497 (13)	0.2500	0.6406 (13)	0.020 (2)*
C6	1.0969 (13)	0.2500	0.7373 (13)	0.020 (2)*
H1	1.1711	0.2500	0.8451	0.02 (4)*
C7	0.9524 (13)	0.2500	0.6988 (13)	0.020 (2)*
C8	0.8934 (13)	0.2500	0.8012 (13)	0.020 (2)*
C9	0.7997 (9)	0.1813 (5)	0.7744 (9)	0.0200 (17)*
C10	1.0141 (13)	0.2500	0.9509 (13)	0.020 (2)*
C12	0.4996 (9)	0.4111 (5)	0.2713 (9)	0.0200 (16)*
C13	0.4647 (9)	0.4923 (5)	0.2310 (9)	0.0200 (16)*
C14	0.4822 (9)	0.3934 (5)	0.3975 (9)	0.0200 (16)*
C15	0.3901 (9)	0.3649 (5)	0.1510 (9)	0.0200 (16)*
C16	0.6440 (9)	0.3873 (5)	0.2952 (9)	0.0200 (16)*
C17	0.7292 (9)	0.4318 (5)	0.2643 (9)	0.0200 (16)*
H2	0.6861	0.4830	0.2140	0.02 (3)*
C18	0.8678 (9)	0.4150 (5)	0.2938 (9)	0.0200 (16)*
C19	0.9565 (9)	0.4637 (5)	0.2537 (9)	0.0200 (16)*
C20	0.9740 (9)	0.4238 (5)	0.1428 (9)	0.0200 (16)*
C21	0.9017 (9)	0.5386 (5)	0.2176 (9)	0.0200 (16)*
C22	1.1040 (9)	0.4692 (5)	0.3801 (9)	0.0200 (16)*

Geometric parameters (Å, º) top

Zr1—O4	2.116 (7)	C6—H1	1.0753
Zr1—O4ⁱ	2.116 (7)	C7—C8	1.52 (2)
Zr1—O2	2.122 (10)	C8—C9ⁱ	1.545 (12)
Zr1—O1	2.131 (9)	C8—C9	1.545 (12)
Zr1—O3	2.145 (7)	C8—C10	1.547 (17)
Zr1—O3ⁱ	2.145 (7)	C12—C16	1.503 (13)
Zr1—Cl1	2.495 (4)	C12—C14	1.515 (13)
O1—C5	1.257 (15)	C12—C13	1.543 (13)
O2—C7	1.308 (15)	C12—C15	1.545 (12)
O3—C16	1.261 (12)	C16—C17	1.375 (14)
O4—C18	1.288 (11)	C17—C18	1.394 (13)
C1—C3	1.40 (2)	C17—H2	1.0746
C1—C2ⁱ	1.411 (12)	C18—C19	1.506 (14)
C1—C2	1.411 (12)	C19—C21	1.468 (13)
C1—C5	1.511 (18)	C19—C20	1.503 (13)
C5—C6	1.41 (2)	C19—C22	1.544 (12)
C6—C7	1.398 (18)

O4—Zr1—O4ⁱ	127.0 (4)	C7—C6—C5	122.8 (12)
O4—Zr1—O2	106.6 (2)	C7—C6—H1	118.6
O4ⁱ—Zr1—O2	106.6 (2)	C5—C6—H1	118.6
O4—Zr1—O1	74.3 (2)	O2—C7—C6	123.3 (13)
O4ⁱ—Zr1—O1	74.3 (2)	O2—C7—C8	113.1 (11)
O2—Zr1—O1	77.1 (4)	C6—C7—C8	123.7 (11)
O4—Zr1—O3	75.9 (3)	C7—C8—C9ⁱ	108.2 (7)
O4ⁱ—Zr1—O3	151.3 (3)	C7—C8—C9	108.2 (7)
O2—Zr1—O3	77.9 (3)	C9ⁱ—C8—C9	108.5 (10)
O1—Zr1—O3	133.3 (2)	C7—C8—C10	110.9 (11)
O4—Zr1—O3ⁱ	151.3 (3)	C9ⁱ—C8—C10	110.4 (7)
O4ⁱ—Zr1—O3ⁱ	75.9 (3)	C9—C8—C10	110.4 (7)
O2—Zr1—O3ⁱ	77.9 (3)	C16—C12—C14	109.3 (7)
O1—Zr1—O3ⁱ	133.3 (2)	C16—C12—C13	114.8 (8)
O3—Zr1—O3ⁱ	77.5 (4)	C14—C12—C13	110.6 (8)
O4—Zr1—Cl1	81.50 (18)	C16—C12—C15	107.4 (8)
O4ⁱ—Zr1—Cl1	81.50 (18)	C14—C12—C15	107.4 (8)
O2—Zr1—Cl1	159.6 (3)	C13—C12—C15	107.1 (7)
O1—Zr1—Cl1	123.3 (3)	O3—C16—C17	123.1 (9)
O3—Zr1—Cl1	86.21 (19)	O3—C16—C12	115.0 (9)
O3ⁱ—Zr1—Cl1	86.21 (19)	C17—C16—C12	121.9 (9)
C5—O1—Zr1	138.8 (9)	C16—C17—C18	124.4 (9)
C7—O2—Zr1	136.0 (9)	C16—C17—H2	117.8
C16—O3—Zr1	135.3 (7)	C18—C17—H2	117.8
C18—O4—Zr1	136.4 (6)	O4—C18—C17	120.0 (9)
C3—C1—C2ⁱ	107.9 (8)	O4—C18—C19	116.8 (8)
C3—C1—C2	107.9 (8)	C17—C18—C19	123.1 (8)
C2ⁱ—C1—C2	107.3 (11)	C21—C19—C20	114.7 (8)
C3—C1—C5	111.2 (11)	C21—C19—C18	113.8 (8)
C2ⁱ—C1—C5	111.2 (8)	C20—C19—C18	106.4 (8)
C2—C1—C5	111.2 (8)	C21—C19—C22	107.1 (8)
O1—C5—C6	122.0 (12)	C20—C19—C22	107.5 (8)
O1—C5—C1	117.1 (12)	C18—C19—C22	107.1 (7)
C6—C5—C1	121.0 (11)

Symmetry code: (i) x, −y+1/2, z.

(pyrhsb) Pyridinium hexachloro-antimony(v) top

Crystal data top

C₅H₆N⁺·Cl₆Sb⁻	γ = 90°
M_r = 414.56	V = 1286 (4) Å³
P2₁/a	Z = 4
a = 15.42 (3) Å	F(000) = 784
b = 11.66 (2) Å	D_x = 2.142 Mg m⁻³
c = 7.21 (1) Å	Mo Kα radiation, λ = 0.71073 Å
α = 90°	µ = 3.35 mm⁻¹
β = 97.31 (4)°	T = 293 K

Data collection top

Radiation source: fine-focus sealed tube	R_int = 0.007
Graphite monochromator	θ_max = 42.0°, θ_min = 2.2°
12890 measured reflections	h = −15→15
3289 independent reflections	k = −12→12
3277 reflections with I > 2σ(I)	l = −8→8

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.061	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.167	H atoms treated by a mixture of independent and constrained refinement
S = 1.35	w = 1/[σ²(F_o²) + (0.P)² + 16.8959P] where P = (F_o² + 2F_c²)/3
3289 reflections	(Δ/σ)_max = 2.226
77 parameters	Δρ_max = 2.17 e Å⁻³
0 restraints	Δρ_min = −3.22 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Sb1	0.33750 (4)	0.32820 (4)	0.25310 (7)	0.02000 (15)*
Cl1	0.36500 (13)	0.45900 (16)	0.0180 (2)	0.0200 (3)*
Cl5	0.31000 (13)	0.19500 (16)	0.4840 (2)	0.0200 (3)*
Cl6	0.30550 (13)	0.18600 (16)	0.0295 (2)	0.0200 (3)*
Cl7	0.36850 (13)	0.46850 (16)	0.4825 (2)	0.0200 (3)*
Cl8	0.18950 (13)	0.38400 (16)	0.2155 (2)	0.0200 (3)*
Cl9	0.48400 (13)	0.27150 (16)	0.2860 (2)	0.0200 (3)*
N1	0.4420 (12)	0.7237 (12)	0.2380 (18)	0.020 (3)*	0.50
C3	0.5080 (12)	0.7877 (16)	0.194 (2)	0.020 (3)*	0.50
C4	0.5070 (11)	0.9037 (14)	0.240 (2)	0.020 (3)*	0.50
C5	0.4200 (13)	0.9527 (14)	0.277 (2)	0.020 (3)*	0.50
C6	0.3600 (11)	0.8747 (18)	0.318 (2)	0.020 (3)*	0.50
C7	0.3680 (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—Cl6	2.321 (3)	C5—C8'	0.58 (2)
Sb1—Cl7	2.332 (3)	C5—C2'	0.95 (2)
Sb1—Cl9	2.337 (5)	C5—C6	1.36 (3)
Sb1—Cl5	2.354 (3)	C5—C9'	1.85 (3)
Sb1—Cl8	2.355 (5)	C6—C2'	0.605 (19)
Sb1—Cl1	2.358 (3)	C6—C1'	0.87 (2)
N1—C10'	0.73 (2)	C6—C7	1.23 (3)
N1—N2'	0.743 (17)	C6—C8'	1.80 (3)
N1—C3	1.33 (2)	C6—N2'	1.93 (2)
N1—C7	1.37 (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—C4	1.39 (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—C5	1.51 (3)	C8'—C2'	1.48 (3)
C4—C10'	1.79 (3)	C2'—C1'	1.43 (3)

Cl6—Sb1—Cl7	178.76 (7)	N2'—C7—C2'	139 (2)
Cl6—Sb1—Cl9	89.18 (9)	C6—C7—C2'	9.4 (10)
Cl7—Sb1—Cl9	91.04 (9)	N1—C7—C2'	116.7 (15)
Cl6—Sb1—Cl5	88.76 (14)	C1'—C7—C10'	138 (4)
Cl7—Sb1—Cl5	90.02 (14)	N2'—C7—C10'	42.8 (18)
Cl9—Sb1—Cl5	90.02 (9)	C6—C7—C10'	104.9 (16)
Cl6—Sb1—Cl8	90.01 (9)	N1—C7—C10'	19.2 (8)
Cl7—Sb1—Cl8	89.77 (9)	C2'—C7—C10'	97.7 (12)
Cl9—Sb1—Cl8	179.14 (7)	N1—N2'—C7	128 (3)
Cl5—Sb1—Cl8	90.26 (9)	N1—N2'—C1'	132 (2)
Cl6—Sb1—Cl1	90.26 (14)	C7—N2'—C1'	8.7 (15)
Cl7—Sb1—Cl1	90.96 (14)	N1—N2'—C10'	18.0 (15)
Cl9—Sb1—Cl1	89.77 (9)	C7—N2'—C10'	115 (2)
Cl5—Sb1—Cl1	179.00 (7)	C1'—N2'—C10'	116.9 (15)
Cl8—Sb1—Cl1	89.93 (9)	N1—N2'—C6	109.6 (18)
C10'—N1—N2'	144 (3)	C7—N2'—C6	20.1 (18)
C10'—N1—C3	7.5 (16)	C1'—N2'—C6	22.4 (10)
N2'—N1—C3	145 (2)	C10'—N2'—C6	95.3 (11)
C10'—N1—C7	123 (2)	C3—C10'—N1	163 (3)
N2'—N1—C7	26.5 (15)	C3—C10'—C9'	38 (2)
C3—N1—C7	121.7 (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'—C4	42 (2)
C10'—N1—C9'	24.6 (18)	N1—C10'—C4	130 (2)
N2'—N1—C9'	121.0 (18)	C9'—C10'—C4	19.6 (9)
C3—N1—C9'	24.2 (9)	N2'—C10'—C4	117.4 (14)
C7—N1—C9'	98.4 (12)	C3—C10'—C7	137 (3)
C1'—N1—C9'	92.1 (10)	N1—C10'—C7	37.9 (18)
C10'—C3—C9'	117 (4)	C9'—C10'—C7	104.1 (15)
C10'—C3—N1	9.0 (18)	N2'—C10'—C7	22.1 (8)
C9'—C3—N1	118 (2)	C4—C10'—C7	95.3 (12)
C10'—C3—C4	120 (3)	C4—C9'—C3	120 (3)
C9'—C3—C4	26.3 (12)	C4—C9'—C10'	123 (2)
N1—C3—C4	117.1 (15)	C3—C9'—C10'	24.9 (14)
C9'—C4—C8'	105 (2)	C4—C9'—C8'	45.1 (18)
C9'—C4—C3	34.1 (17)	C3—C9'—C8'	135 (2)
C8'—C4—C3	122.3 (19)	C10'—C9'—C8'	117.2 (16)
C9'—C4—C5	107 (2)	C4—C9'—C5	51.6 (19)
C8'—C4—C5	13.5 (12)	C3—C9'—C5	124.5 (18)
C3—C4—C5	116.5 (15)	C10'—C9'—C5	105.1 (14)
C9'—C4—C10'	37.9 (18)	C8'—C9'—C5	12.2 (9)
C8'—C4—C10'	106.3 (17)	C4—C9'—N1	116 (2)
C3—C4—C10'	17.3 (9)	C3—C9'—N1	37.4 (14)
C5—C4—C10'	99.4 (13)	C10'—C9'—N1	13.5 (10)
C8'—C5—C2'	148 (3)	C8'—C9'—N1	103.8 (13)
C8'—C5—C6	132 (3)	C5—C9'—N1	91.7 (10)
C2'—C5—C6	22.8 (13)	C5—C8'—C4	143 (3)
C8'—C5—C4	24 (2)	C5—C8'—C9'	138 (3)
C2'—C5—C4	137 (2)	C4—C8'—C9'	29.9 (12)
C6—C5—C4	115.5 (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'—C6	34 (2)
C4—C5—C9'	21.6 (7)	C4—C8'—C6	117.0 (17)
C2'—C6—C1'	151 (3)	C9'—C8'—C6	103.9 (13)
C2'—C6—C7	151 (3)	C2'—C8'—C6	18.1 (8)
C1'—C6—C7	24.2 (16)	C6—C2'—C5	120 (3)
C2'—C6—C5	38 (2)	C6—C2'—C1'	17.1 (19)
C1'—C6—C5	142 (2)	C5—C2'—C1'	124 (2)
C7—C6—C5	122.3 (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'—C7	19 (2)
C5—C6—C8'	14.0 (9)	C5—C2'—C7	108.0 (18)
C2'—C6—N2'	140 (3)	C1'—C2'—C7	15.8 (10)
C1'—C6—N2'	35.3 (16)	C8'—C2'—C7	98.4 (13)
C7—C6—N2'	12.5 (11)	C7—C1'—C6	116 (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—C6	39 (3)	C6—C1'—C2'	11.8 (13)
N2'—C7—C6	147 (3)	N2'—C1'—C2'	123.9 (17)
C1'—C7—N1	156 (4)	C7—C1'—N1	17 (3)
N2'—C7—N1	25.3 (15)	C6—C1'—N1	105 (2)
C6—C7—N1	123.5 (19)	N2'—C1'—N1	17.0 (8)
C1'—C7—C2'	44 (3)	C2'—C1'—N1	107.1 (14)

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