30 Space-group corrections: two examples of false polymorphism and one of incorrect interpretation of the fine details of an IR spectrum

Revised structures are reported for 30 crystalline compounds, based on space groups of higher symmetry than originally reported. In 18 cases the Laue class is revised, in seven cases the center of symmetry is added, in two cases the Laue class change is coupled with the addition of the center of symmetry, in two cases the addition of the center of symmetry also requires the addition of systematic absences and, finally, one case of the addition of systematic absences without changing the Laue group is reported. Two examples (CSD refcodes: DAMLIM and ABPZCU01) of false polymorphism and one (PAVJUR) of the erroneous interpretation of the fine details of IR spectra, owing to incorrect space-group determination, have been detected.

Computing details

Program(s) used to solve structure: SHELXS97 (Sheldrick, 1990) for (2), (12), (15), (18), (23), (29). Program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) for (2), (12), (15), (18), (23), (29). Software used to prepare material for publication: PLATON (Spek, 1990) for (1), (3), (4), (5), (6), (7), (8), (9), (10), (11), (13), (14), (16), (17), (19), (20), (21), (22), (25), (26), (27), (28), (30).

Figures

Fig. 1.

(1) cis-Diaqua-(2,2-bipyridyl-N,N')-copper sulfate

Crystal data

C10H12CuN2O6S	γ = 90°
Mr = 351.84	V = 1265.9 (3) Å^3
Monclinic, I2/a	Z = 4
Hall symbol: -I 2ya	F(000) = 668
a = 6.963 (1) Å	Dx = 1.783 Mg m^−3
b = 12.4686 (16) Å	Mo K\a radiation, λ = 0.71070 Å
c = 14.8540 (15) Å	µ = 1.92 mm^−1
α = 90°	T = 0 K
β = 101.01 (1)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cu1	0.75	0.27434	0.5	0.02*
S1	0.25	0.3461	0.5	0.02*
O1	0.42125	0.28015	0.5348	0.02*
O2	0.20633	0.41637	0.57487	0.02*
O5	0.653	0.38345	0.40585	0.02*
N1	0.68405	0.1524	0.4118	0.02*
C1	0.61755	0.16135	0.32125	0.02*
C2	0.57847	0.07333	0.26497	0.02*
C3	0.6068	−0.02790	0.30380	0.02*
C4	0.67475	−0.03815	0.3973	0.02*
C5	0.71223	0.05418	0.44967	0.02*

Geometric parameters (Å, º)

Cu1—O1	2.4422	N1—C5	1.3463
Cu1—O5	1.9754	C1—C2	1.375
Cu1—N1	2.0023	C2—C3	1.3861
S1—O1	1.4594	C3—C4	1.385
S1—O2	1.492	C4—C5	1.386
N1—C1	1.3409	C5—C5^i	1.4872
Cu1···S1^ii	3.5946 (5)	O5···O2^iii	2.6047
Cu1···O2^ii	3.6221	O5···O2^vi	2.6766
Cu1···O2^iii	3.6221	C2···C3^vii	3.4876
S1···Cu1^iv	3.5946 (5)	C3···C2^viii	3.4876
O1···C4^v	3.2903	C3···C3^vii	3.5503
O2···Cu1^iv	3.6221	C3···C3^viii	3.5503
O2···Cu1^iii	3.6221	C4···O1^v	3.2903
O2···O5^iii	2.6047	C4···C5^vii	3.4603
O2···O5^vi	2.6766	C5···C4^viii	3.4603
O1—Cu1—O5	85.52	O1—S1—O1^iii	111.41
O1—Cu1—N1	93.09	O1—S1—O2^iii	109.02
O1—Cu1—O1^i	176.6	O1^iii—S1—O2	109.02
O1—Cu1—O5^i	92.14	O2—S1—O2^iii	108.08
O1—Cu1—N1^i	89.49	O1^iii—S1—O2^iii	109.63
O5—Cu1—N1	93.16	Cu1—O1—S1	132.63
O1^i—Cu1—O5	92.14	Cu1—N1—C1	125.82
O5—Cu1—O5^i	92.94	Cu1—N1—C5	114.86
O5—Cu1—N1^i	172.26	C1—N1—C5	119.32
O1^i—Cu1—N1	89.49	N1—C1—C2	122.26
O5^i—Cu1—N1	172.26	C1—C2—C3	118.55
N1—Cu1—N1^i	81.19	C2—C3—C4	119.7
O1^i—Cu1—O5^i	85.52	C3—C4—C5	118.54
O1^i—Cu1—N1^i	93.09	N1—C5—C4	121.62
O5^i—Cu1—N1^i	93.16	N1—C5—C5^i	114.54
O1—S1—O2	109.63	C4—C5—C5^i	123.83
O5—Cu1—O1—S1	−4.09	Cu1—N1—C1—C2	178.95
N1—Cu1—O1—S1	−97.02	C5—N1—C1—C2	−0.64
O5^i—Cu1—O1—S1	88.69	Cu1—N1—C5—C5^i	−0.12
N1^i—Cu1—O1—S1	−178.17	C1—N1—C5—C5^i	179.52
O1—Cu1—N1—C1	91.43	Cu1—N1—C5—C4	−179.43
O1—Cu1—N1—C5	−88.96	C1—N1—C5—C4	0.2
O5—Cu1—N1—C1	5.76	N1—C1—C2—C3	0.82
O5—Cu1—N1—C5	−174.64	C1—C2—C3—C4	−0.56
O1^i—Cu1—N1—C1	−86.36	C2—C3—C4—C5	0.15
O1^i—Cu1—N1—C5	93.25	C3—C4—C5—N1	0.03
N1^i—Cu1—N1—C1	−179.56	C3—C4—C5—C5^i	−179.22
N1^i—Cu1—N1—C5	0.04	N1—C5—C5^i—N1^i	0.15
O2—S1—O1—Cu1	−113.87	N1—C5—C5^i—C4^i	179.45
O1^iii—S1—O1—Cu1	125.38	C4—C5—C5^i—N1^i	179.45
O2^iii—S1—O1—Cu1	4.26	C4—C5—C5^i—C4^i	−1.25

Symmetry codes: (i) −x+3/2, y, −z+1; (ii) x+1, y, z; (iii) −x+1/2, y, −z+1; (iv) x−1, y, z; (v) −x+1, −y, −z+1; (vi) −x+1, −y+1, −z+1; (vii) x−1/2, −y, z; (viii) x+1/2, −y, z.

(2) Dinitro-(1,4,7,10-tetra-azacyclododecane) cobalt(iii) chloride monhydrate

Crystal data

C8H20CoN6O4·H2O·Cl	Z = 4
Mr = 376.70	F(000) = 784
Orthorhombic, Cmc21	Dx = 1.698 Mg m^−3
Hall symbol: C 2c -2	Mo Kα radiation, λ = 0.71073 Å
a = 9.515 (7) Å	µ = 1.38 mm^−1
b = 11.909 (9) Å	T = 293 K
c = 13.003 (10) Å	× × mm
V = 1473.4 (19) Å^3

Data collection

Radiation source: fine-focus sealed tube	θmax = 25.1°, θmin = 2.7°
1146 measured reflections	h = −8→11
654 independent reflections	k = −8→14
652 reflections with I > 2σ(I)	l = −15→0
Rint = 0.037

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.028	w = 1/[σ^2(Fo^2) + (0.P)^2 + 3.9018P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.088	(Δ/σ)max = 0.008
S = 1.46	Δρmax = 0.28 e Å^−3
654 reflections	Δρmin = −0.32 e Å^−3
118 parameters	Extinction correction: nne
2 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.01 (7)
Secondary atom site location: difference Fourier map

Special details

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 nt 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 (Ų)

	x	y	z	Uiso*/Ueq
Co1	0.5000	0.42147 (10)	0.50007 (13)	0.0194 (4)
O14	0.3888 (9)	0.5481 (7)	0.6579 (7)	0.058 (2)
O17	0.3895 (8)	0.6053 (6)	0.4014 (8)	0.060 (2)
N1	0.2946 (6)	0.3988 (4)	0.4964 (9)	0.0262 (13)
H1	0.2514	0.4652	0.5105	0.03 (2)*
N4	0.5000	0.3424 (8)	0.3680 (7)	0.022 (2)
H6	0.5000	0.3965	0.3187	0.04 (4)*
N10	0.5000	0.2873 (8)	0.5844 (8)	0.025 (2)
H16	0.5000	0.2265	0.5419	0.04 (4)*
N13	0.5000	0.5147 (9)	0.6200 (9)	0.033 (3)
N16	0.5000	0.5621 (8)	0.4251 (8)	0.028 (2)
C2	0.2552 (10)	0.3628 (8)	0.3918 (7)	0.029 (2)
H2	0.2513	0.4270	0.3460	0.03 (2)*
H3	0.1636	0.3270	0.3926	0.04 (3)*
C3	0.3662 (13)	0.2805 (9)	0.3558 (8)	0.027 (3)
H4	0.3656	0.2131	0.3977	0.015 (19)*
H5	0.3511	0.2597	0.2845	0.03 (3)*
C8	0.2499 (11)	0.3130 (8)	0.5755 (7)	0.035 (2)
H12	0.1720	0.3425	0.6152	0.04 (3)*
H13	0.2182	0.2455	0.5409	0.07 (4)*
C9	0.3691 (15)	0.2845 (9)	0.6465 (8)	0.031 (3)
H14	0.3744	0.3386	0.7021	0.03 (2)*
H15	0.3555	0.2104	0.6759	0.03 (2)*
O19	0.5000	0.0551 (14)	0.2499 (13)	0.107 (6)
H21	0.4370	−0.0102	0.1971	0.36 (19)*
Cl1	0.0000	0.4637 (2)	0.0112 (4)	0.0369 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0240 (6)	0.0177 (6)	0.0164 (6)	0.000	0.000	−0.0002 (8)
O14	0.064 (5)	0.054 (4)	0.056 (5)	0.007 (4)	0.013 (4)	−0.028 (4)
O17	0.052 (5)	0.039 (4)	0.088 (7)	0.018 (4)	−0.002 (5)	0.024 (5)
N1	0.026 (3)	0.026 (3)	0.027 (3)	0.004 (2)	0.004 (5)	0.001 (5)
N4	0.028 (5)	0.024 (5)	0.013 (5)	0.000	0.000	0.001 (4)
N10	0.026 (5)	0.026 (5)	0.021 (5)	0.000	0.000	−0.001 (5)
N13	0.046 (7)	0.024 (6)	0.028 (6)	0.000	0.000	−0.005 (5)
N16	0.041 (6)	0.014 (5)	0.030 (6)	0.000	0.000	−0.001 (4)
C2	0.025 (5)	0.031 (4)	0.032 (5)	−0.004 (4)	−0.002 (4)	0.002 (4)
C3	0.026 (6)	0.031 (6)	0.026 (5)	0.000 (5)	−0.007 (5)	−0.004 (4)
C8	0.031 (5)	0.042 (5)	0.032 (5)	−0.004 (5)	0.009 (4)	0.004 (4)
C9	0.038 (7)	0.025 (5)	0.030 (6)	−0.002 (5)	0.010 (6)	0.002 (4)
O19	0.165 (16)	0.083 (10)	0.072 (10)	0.000	0.000	−0.008 (9)
Cl1	0.0317 (13)	0.0274 (12)	0.052 (2)	0.000	0.000	−0.0009 (18)

Geometric parameters (Å, º)

Co1—N13	1.915 (11)	N1—C8	1.510 (12)
Co1—N10	1.938 (10)	N4—C3	1.479 (13)
Co1—N16	1.938 (10)	N4—C3^i	1.479 (13)
Co1—N4	1.958 (9)	N10—C9^i	1.485 (13)
Co1—N1	1.974 (6)	N10—C9	1.485 (13)
Co1—N1^i	1.974 (6)	N13—O14^i	1.233 (9)
O14—N13	1.233 (9)	N16—O17^i	1.211 (8)
O17—N16	1.211 (8)	C2—C3	1.515 (15)
N1—C2	1.474 (14)	C8—C9	1.501 (17)
N13—Co1—N10	91.0 (5)	C8—N1—Co1	110.8 (6)
N13—Co1—N16	84.8 (5)	C3—N4—C3^i	118.7 (10)
N10—Co1—N16	175.7 (5)	C3—N4—Co1	109.5 (6)
N13—Co1—N4	173.3 (5)	C3^i—N4—Co1	109.5 (6)
N10—Co1—N4	95.7 (5)	C9^i—N10—C9	114.0 (12)
N16—Co1—N4	88.6 (4)	C9^i—N10—Co1	109.0 (6)
N13—Co1—N1	95.7 (3)	C9—N10—Co1	109.0 (6)
N10—Co1—N1	84.3 (2)	O14^i—N13—O14	118.2 (11)
N16—Co1—N1	96.1 (2)	O14^i—N13—Co1	120.8 (6)
N4—Co1—N1	85.0 (3)	O14—N13—Co1	120.8 (6)
N13—Co1—N1^i	95.7 (3)	O17^i—N16—O17	120.6 (11)
N10—Co1—N1^i	84.3 (2)	O17^i—N16—Co1	119.7 (5)
N16—Co1—N1^i	96.1 (2)	O17—N16—Co1	119.7 (5)
N4—Co1—N1^i	85.0 (3)	N1—C2—C3	107.2 (8)
N1—Co1—N1^i	164.0 (3)	N4—C3—C2	104.2 (8)
C2—N1—C8	111.1 (7)	C9—C8—N1	111.1 (8)
C2—N1—Co1	108.3 (6)	N10—C9—C8	107.1 (8)
N13—Co1—N1—C2	160.2 (6)	N10—Co1—N13—O14^i	92.1 (9)
N10—Co1—N1—C2	−109.3 (6)	N16—Co1—N13—O14^i	−87.9 (9)
N16—Co1—N1—C2	74.9 (6)	N1—Co1—N13—O14^i	176.5 (9)
N4—Co1—N1—C2	−13.1 (5)	N1^i—Co1—N13—O14^i	7.7 (10)
N1^i—Co1—N1—C2	−65 (3)	N10—Co1—N13—O14	−92.1 (9)
N13—Co1—N1—C8	−77.7 (7)	N16—Co1—N13—O14	87.9 (9)
N10—Co1—N1—C8	12.7 (7)	N1—Co1—N13—O14	−7.7 (10)
N16—Co1—N1—C8	−163.0 (7)	N1^i—Co1—N13—O14	−176.5 (9)
N4—Co1—N1—C8	108.9 (7)	N13—Co1—N16—O17^i	90.4 (10)
N1^i—Co1—N1—C8	57 (3)	N4—Co1—N16—O17^i	−89.6 (10)
N10—Co1—N4—C3	65.9 (6)	N1—Co1—N16—O17^i	−174.4 (10)
N16—Co1—N4—C3	−114.1 (6)	N1^i—Co1—N16—O17^i	−4.8 (10)
N1—Co1—N4—C3	−17.9 (6)	N13—Co1—N16—O17	−90.4 (10)
N1^i—Co1—N4—C3	149.6 (7)	N4—Co1—N16—O17	89.6 (10)
N10—Co1—N4—C3^i	−65.9 (6)	N1—Co1—N16—O17	4.8 (10)
N16—Co1—N4—C3^i	114.1 (6)	N1^i—Co1—N16—O17	174.4 (10)
N1—Co1—N4—C3^i	−149.6 (7)	C8—N1—C2—C3	−81.1 (8)
N1^i—Co1—N4—C3^i	17.9 (6)	Co1—N1—C2—C3	40.7 (8)
N13—Co1—N10—C9^i	−62.5 (7)	C3^i—N4—C3—C2	170.1 (7)
N4—Co1—N10—C9^i	117.5 (7)	Co1—N4—C3—C2	43.4 (9)
N1—Co1—N10—C9^i	−158.1 (8)	N1—C2—C3—N4	−54.7 (10)
N1^i—Co1—N10—C9^i	33.1 (7)	C2—N1—C8—C9	130.3 (8)
N13—Co1—N10—C9	62.5 (7)	Co1—N1—C8—C9	10.0 (10)
N4—Co1—N10—C9	−117.5 (7)	C9^i—N10—C9—C8	167.9 (6)
N1—Co1—N10—C9	−33.1 (7)	Co1—N10—C9—C8	45.7 (10)
N1^i—Co1—N10—C9	158.1 (8)	N1—C8—C9—N10	−35.4 (11)

Symmetry code: (i) −x+1, y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O14	0.91	2.52	2.8941	105
N1—H1···O17	0.91	2.55	2.8964	103
N1—H1···Cl1^ii	0.91	2.54	3.2518	136
N1—H1···Cl1^iii	0.91	2.54	3.2518	136
N4—H6···O14^iv	0.91	2.43	3.2068	143
N4—H6···O14^v	0.91	2.43	3.2068	143
N10—H16···Cl1^vi	0.91	2.3	3.137 (2)	153
N10—H16···Cl1^vii	0.91	2.3	3.137 (2)	153
O19—H21···Cl1^viii	1.2	2.51	3.290 (3)	121
O19—H21···Cl1^ix	1.2	2.51	3.290 (3)	121
C2—H2···O17	0.97	2.6	3.1609	117
C9—H14···O14	0.97	2.56	3.1488	119

Symmetry codes: (ii) −x, −y+1, z+1/2; (iii) x, −y+1, z+1/2; (iv) −x+1, −y+1, z−1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, −y+1/2, z+1/2; (vii) x+1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) −x+1/2, y−1/2, z.

(3) 3',6'-O-(1,1,3,3-Tetraisopropyl-disiloxane-1,3-diyl)-neplancin A

Crystal data

C23H39N5O4Si2	Z = 8
Mr = 505.77	F(000) = 1864
Orthorhombic, C2221	Dx = 1.119 Mg m^−3
Hall symbol: C 2c 2	Mo K\a radiation, λ = 0.71073 Å
a = 13.1422 (15) Å	µ = 0.16 mm^−1
b = 12.1676 (15) Å	T = 0 K
c = 34.638 (4) Å	× × mm
V = 5538.9 (11) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text	Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Si1	0.63508	0.44078	0.13178	0.02*
Si2	0.70738	0.66313	0.17120	0.02*
O1	0.87493	0.27752	0.08375	0.02*
O2	0.72665	0.43305	0.09945	0.02*
O3	0.80542	0.68708	0.14310	0.02*
O4	0.65175	0.5497	0.1582	0.02*
N1	1.24808	0.24653	−0.01385	0.02*
N2	1.0726	0.2819	0.00225	0.02*
N3	1.38228	0.34722	0.01235	0.02*
N4	1.22315	0.47465	0.05575	0.02*
N5	1.05572	0.43607	0.0471	0.02*
C1	1.14848	0.22882	−0.01560	0.02*
C2	1.10867	0.36258	0.025	0.02*
C3	1.21035	0.3877	0.0304	0.02*
C4	1.28172	0.32783	0.00975	0.02*
C5	1.12843	0.50022	0.0646	0.02*
C6	0.94517	0.44578	0.05285	0.02*
C7	0.90843	0.38718	0.0895	0.02*
C8	0.82915	0.4653	0.10785	0.02*
C9	0.85185	0.57315	0.08925	0.02*
C10	0.914	0.56355	0.0595	0.02*
C11	0.80115	0.67760	0.10205	0.02*
C12	0.65413	0.88858	0.17395	0.02*
C13	0.61203	0.77697	0.16485	0.02*
C14	0.5119	0.759	0.1856	0.02*
C15	0.68975	0.62575	0.2515	0.02*
C16	0.76565	0.6495	0.2199	0.02*
C17	0.8508	0.5657	0.2201	0.02*
C18	0.42198	0.46662	0.1286	0.02*
C19	0.51508	0.45342	0.10325	0.02*
C20	0.52295	0.5462	0.0736	0.02*
C21	0.63133	0.21132	0.14165	0.02*
C22	0.64267	0.31877	0.16435	0.02*
C23	0.57	0.323	0.19905	0.02*

Geometric parameters (Å, º)

Si1—O2	1.6466	N5—C5	1.3747
Si1—O4	1.6254	N5—C6	1.4712
Si1—C19	1.8674	C2—C3	1.3835
Si1—C22	1.8673	C3—C4	1.3864
Si2—O3	1.6409	C6—C7	1.534
Si2—O4	1.6255	C6—C10	1.5081
Si2—C13	1.8808	C7—C8	1.547
Si2—C16	1.86	C8—C9	1.492
O1—C7	1.4191	C9—C10	1.3201
O2—C8	1.4329	C9—C11	1.5019
O3—C11	1.4277	C12—C13	1.4999
N1—C1	1.328	C13—C14	1.5153
N1—C4	1.3573	C15—C16	1.5088
N2—C1	1.3394	C16—C17	1.5139
N2—C2	1.3451	C18—C19	1.5145
N3—C4	1.3455	C19—C20	1.5297
N4—C3	1.3851	C21—C22	1.5329
N4—C5	1.3192	C22—C23	1.536
N5—C2	1.3674
Si1···C11	3.7586	N4···C4^iii	3.3935
Si2···C8	3.6291	C2···C5^iii	3.5336
O1···O2	2.7703	C3···N4^iii	3.4261
O1···N1^i	2.9542	C3···C3^iii	3.4502
O2···O1	2.7703	C4···N4^iii	3.3935
N1···O1^ii	2.9542	C5···C2^iii	3.5336
N2···N3^i	2.9967	C8···Si2	3.6291
N3···N4	3.0063	C11···Si1	3.7586
N3···N2^ii	2.9967	C18···C23	3.5767
N4···N3	3.0063	C23···C18	3.5767
N4···C3^iii	3.4261
O2—Si1—O4	109.33	N1—C4—C3	118.25
O2—Si1—C19	105.19	N3—C4—C3	122.54
O2—Si1—C22	109.05	N4—C5—N5	114.81
O4—Si1—C19	110.16	N5—C6—C7	112.68
O4—Si1—C22	107.51	N5—C6—C10	111.42
C19—Si1—C22	115.49	C7—C6—C10	103.28
O3—Si2—O4	109.86	O1—C7—C6	114.74
O3—Si2—C13	108.85	O1—C7—C8	115.24
O3—Si2—C16	103.33	C6—C7—C8	105.45
O4—Si2—C13	107.05	O2—C8—C7	112.43
O4—Si2—C16	111.14	O2—C8—C9	109.95
C13—Si2—C16	116.49	C7—C8—C9	103.2
Si1—O2—C8	122.23	C8—C9—C10	112.52
Si2—O3—C11	123.06	C8—C9—C11	121.88
Si1—O4—Si2	155.36	C10—C9—C11	125.44
C1—N1—C4	117.83	C6—C10—C9	111.8
C1—N2—C2	111.1	O3—C11—C9	110.18
C3—N4—C5	102.29	Si2—C13—C12	113.36
C2—N5—C5	105.33	Si2—C13—C14	114.64
C2—N5—C6	129.11	C12—C13—C14	110.57
C5—N5—C6	125.53	Si2—C16—C15	113.75
N1—C1—N2	129.39	Si2—C16—C17	111.63
N2—C2—N5	128.74	C15—C16—C17	110.88
N2—C2—C3	125.51	Si1—C19—C18	112.59
N5—C2—C3	105.75	Si1—C19—C20	111.04
N4—C3—C2	111.82	C18—C19—C20	111.45
N4—C3—C4	130.26	Si1—C22—C21	111.28
C2—C3—C4	117.88	Si1—C22—C23	114.39
N1—C4—N3	119.21	C21—C22—C23	111.68
O4—Si1—O2—C8	36.6	C2—N2—C1—N1	−0.87
C19—Si1—O2—C8	154.87	C1—N2—C2—C3	−1.26
C22—Si1—O2—C8	−80.69	C1—N2—C2—N5	178.43
O2—Si1—C22—C23	172.61	C3—N4—C5—N5	0.37
O4—Si1—C22—C23	54.18	C5—N4—C3—C2	−0.63
C19—Si1—C22—C23	−69.24	C5—N4—C3—C4	177.04
O2—Si1—O4—Si2	3.65	C5—N5—C6—C7	−81.86
C19—Si1—O4—Si2	−111.47	C5—N5—C2—N2	179.86
C22—Si1—O4—Si2	121.91	C6—N5—C2—C3	−178.70
O2—Si1—C19—C18	−177.48	C2—N5—C6—C10	−148.32
O4—Si1—C19—C18	−59.77	C5—N5—C2—C3	−0.40
C22—Si1—C19—C18	62.24	C6—N5—C2—N2	1.57
O2—Si1—C19—C20	−51.73	C2—N5—C6—C7	96.12
O4—Si1—C19—C20	65.99	C6—N5—C5—N4	178.39
C22—Si1—C19—C20	−172.00	C2—N5—C5—N4	0.03
O2—Si1—C22—C21	−59.65	C5—N5—C6—C10	33.69
O4—Si1—C22—C21	−178.08	N5—C2—C3—C4	−177.32
C19—Si1—C22—C21	58.5	N2—C2—C3—N4	−179.59
O4—Si2—O3—C11	46.01	N2—C2—C3—C4	2.42
C13—Si2—O3—C11	−70.91	N5—C2—C3—N4	0.67
C16—Si2—O3—C11	164.67	N4—C3—C4—N3	1.12
O4—Si2—C16—C15	−61.73	C2—C3—C4—N3	178.67
C13—Si2—C16—C15	61.23	N4—C3—C4—N1	−179.04
O3—Si2—C16—C17	−53.11	C2—C3—C4—N1	−1.49
O4—Si2—C16—C17	64.66	N5—C6—C7—O1	−93.45
C13—Si2—C16—C17	−172.38	N5—C6—C7—C8	138.63
O3—Si2—O4—Si1	−1.47	C10—C6—C7—C8	18.27
C13—Si2—O4—Si1	116.57	N5—C6—C10—C9	−132.88
C16—Si2—O4—Si1	−115.20	C10—C6—C7—O1	146.19
O3—Si2—C13—C12	−58.51	C7—C6—C10—C9	−11.67
O4—Si2—C13—C12	−177.20	O1—C7—C8—O2	−27.70
C16—Si2—C13—C12	57.74	O1—C7—C8—C9	−146.11
O3—Si2—C13—C14	173.24	C6—C7—C8—O2	99.92
O4—Si2—C13—C14	54.55	C6—C7—C8—C9	−18.49
C16—Si2—C13—C14	−70.51	C7—C8—C9—C11	−172.38
O3—Si2—C16—C15	−179.50	O2—C8—C9—C11	67.5
Si1—O2—C8—C9	−105.14	C7—C8—C9—C10	12.13
Si1—O2—C8—C7	140.5	O2—C8—C9—C10	−108.00
Si2—O3—C11—C9	−103.60	C8—C9—C10—C6	−0.37
C4—N1—C1—N2	1.67	C11—C9—C10—C6	−175.67
C1—N1—C4—N3	179.53	C8—C9—C11—O3	48.01
C1—N1—C4—C3	−0.32	C10—C9—C11—O3	−137.11

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

(4) (R*,R*)-4,4'-Bi(1 − t-butylcyclohexen-3-one)

Crystal data

C20H30O2	γ = 90°
Mr = 302.44	V = 1890.5 (13) Å^3
Monclinic, I2/a	Z = 4
Hall symbol: -I 2ya	F(000) = 544
a = 27.869 (1) Å	Dx = 0.956 Mg m^−3
b = 5.771 (3) Å	Mo K\a radiation, λ = 0.71070 Å
c = 11.758 (5) Å	µ = 0.06 mm^−1
α = 90°	T = 0 K
β = 91.43 (1)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
O1	0.18350	0.3012	0.6195	0.02*
C1	0.2271	0.4399	0.46215	0.02*
C2	0.22095	0.6572	0.3911	0.02*
C3	0.17722	0.63838	0.31233	0.02*
C4	0.13318	0.58117	0.37758	0.02*
C5	0.13745	0.47505	0.476	0.02*
C6	0.18245	0.39965	0.52725	0.02*
C13	0.0849	0.65935	0.32365	0.02*
C14	0.0423	0.5737	0.38965	0.02*
C15	0.07998	0.57582	0.20208	0.02*
C16	0.08325	0.9236	0.32655	0.02*

Geometric parameters (Å, º)

O1—C6	1.2242	C4—C5	1.3121
C1—C2	1.5142	C4—C13	1.5406
C1—C6	1.4953	C5—C6	1.4448
C1—C1^i	1.5378	C13—C14	1.5172
C2—C3	1.5161	C13—C15	1.5115
C3—C4	1.5003	C13—C16	1.5261
O1···C2^i	3.3681	C2···O1^i	3.3681
O1···C3^ii	3.4098	C3···O1^iii	3.4098
C2—C1—C6	109.08	O1—C6—C1	121.59
C1^i—C1—C2	113.59	O1—C6—C5	120.71
C1^i—C1—C6	113.14	C1—C6—C5	117.68
C1—C2—C3	110.85	C4—C13—C14	112.37
C2—C3—C4	111.02	C4—C13—C15	110.7
C3—C4—C5	119.76	C4—C13—C16	108.06
C3—C4—C13	116.25	C14—C13—C15	109.03
C5—C4—C13	123.97	C14—C13—C16	106.84
C4—C5—C6	124.55	C15—C13—C16	109.74
C6—C1—C2—C3	−56.98	C2—C3—C4—C13	153.97
C1^i—C1—C2—C3	175.8	C3—C4—C5—C6	−2.00
C2—C1—C6—O1	−150.68	C13—C4—C5—C6	179.63
C2—C1—C6—C5	31.12	C3—C4—C13—C14	174.42
C1^i—C1—C6—O1	−23.20	C3—C4—C13—C15	52.24
C1^i—C1—C6—C5	158.59	C3—C4—C13—C16	−67.95
C2—C1—C1^i—C2^i	50.69	C5—C4—C13—C14	−7.16
C2—C1—C1^i—C6^i	−74.38	C5—C4—C13—C15	−129.34
C6—C1—C1^i—C2^i	−74.38	C5—C4—C13—C16	110.46
C6—C1—C1^i—C6^i	160.55	C4—C5—C6—O1	−179.90
C1—C2—C3—C4	54.28	C4—C5—C6—C1	−1.67
C2—C3—C4—C5	−24.51

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

(5) N-(3-Aminpropyl)-N'-3-(anthracen-9-ylmethyl)aminpropylethane-1,2-diamin)- chloro-copper chloride monhydrate

Crystal data

C23H32ClCuN4^+·Cl^−·H2O	γ = 90°
Mr = 514.98	V = 4994.3 (12) Å^3
Monclinic, I2/a	Z = 8
Hall symbol: -I 2ya	F(000) = 2152
a = 18.6300 (18) Å	Dx = 1.370 Mg m^−3
b = 16.610 (2) Å	Mo K\a radiation, λ = 0.71070 Å
c = 16.972 (3) Å	µ = 1.11 mm^−1
α = 90°	T = 0 K
β = 108.020 (9)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cu1	0.38685	0.00029	0.3132	0.02*
Cl1	0.4667	−0.09995	0.42675	0.02*
N1	0.47375	0.006	0.2644	0.02*
N2	0.4234	0.1008	0.38235	0.02*
N3	0.2944	0.00885	0.3551	0.02*
N4	0.33455	−0.09005	0.23245	0.02*
C1	0.5107	0.0842	0.2543	0.02*
C2	0.53215	0.1337	0.33425	0.02*
C3	0.46522	0.16422	0.35618	0.02*
C4	0.35667	0.13412	0.40293	0.02*
C5	0.31337	0.06482	0.42408	0.02*
C6	0.26297	−0.06693	0.37653	0.02*
C7	0.23575	−0.12215	0.30035	0.02*
C8	0.29708	−0.15277	0.26978	0.02*
C9	0.281	−0.06250	0.1523	0.02*
C10	0.3216	−0.02465	0.0967	0.02*
C11	0.35395	−0.07415	0.04835	0.02*
C12	0.34935	−0.16110	0.04835	0.02*
C13	0.379	−0.20570	−0.00205	0.02*
C14	0.4122	−0.16955	−0.05620	0.02*
C15	0.41832	−0.08777	−0.05823	0.02*
C16	0.38878	−0.03863	−0.00738	0.02*
C17	0.39452	0.04557	−0.00993	0.02*
C18	0.36705	0.0939	0.04040	0.02*
C19	0.3774	0.1786	0.0405	0.02*
C20	0.35137	0.22688	0.08968	0.02*
C21	0.31125	0.194	0.1406	0.02*
C22	0.3001	0.11275	0.1434	0.02*
C23	0.32825	0.05915	0.0942	0.02*
Cl3	0.13337	0.09933	0.24243	0.02*
O1	0.52355	0.31205	0.2397	0.02*
H1	0.45685	−0.01670	0.21385	0.02*
H2	0.51118	−0.02602	0.29547	0.02*
H3	0.45572	0.08272	0.43132	0.02*
H4	0.25625	0.0321	0.3137	0.02*
H5	0.37305	−0.11590	0.2195	0.02*
H6	0.5564	0.07345	0.2389	0.02*
H7	0.47565	0.115	0.21	0.02*
H8	0.56333	0.17902	0.32828	0.02*
H9	0.56297	0.10057	0.37938	0.02*
H10	0.4309	0.19155	0.3085	0.02*
H11	0.48255	0.2033	0.4005	0.02*
H12	0.37378	0.17063	0.44963	0.02*
H13	0.32387	0.16367	0.35598	0.02*
H14	0.26695	0.0842	0.43365	0.02*
H15	0.34458	0.03833	0.47402	0.02*
H16	0.30207	−0.09427	0.42018	0.02*
H17	0.2203	−0.05500	0.39695	0.02*
H18	0.19940	−0.09275	0.25595	0.02*
H19	0.20888	−0.16768	0.31413	0.02*
H20	0.33582	−0.17797	0.31543	0.02*
H21	0.27595	−0.19400	0.2285	0.02*
H22	0.25128	−0.10812	0.12393	0.02*
H23	0.24567	−0.02367	0.16287	0.02*
H24	0.32605	−0.18680	0.08295	0.02*
H25	0.37690	−0.26160	0	0.02*
H26	0.43035	−0.20120	−0.09130	0.02*
H27	0.4422	−0.06410	−0.09340	0.02*
H28	0.41727	0.06912	−0.04618	0.02*
H29	0.40258	0.20122	0.00602	0.02*
H30	0.35995	0.28205	0.09	0.02*
H31	0.29205	0.2281	0.17290	0.02*
H32	0.27375	0.09235	0.17785	0.02*

Geometric parameters (Å, º)

Cu1—Cl1	2.6316	C18—C19	1.4199
Cu1—N1	2.0361	C18—C23	1.4484
Cu1—N2	2.0332	C19—C20	1.3511
Cu1—N3	2.0616	C20—C21	1.4154
Cu1—N4	2.0623	C21—C22	1.3685
N1—C1	1.5045	C22—C23	1.4268
N2—C3	1.4588	C1—H6	0.9812
N2—C4	1.4975	C1—H7	0.9745
N3—C5	1.4504	C2—H8	0.9751
N3—C6	1.4803	C2—H9	0.9732
N4—C8	1.4992	C3—H10	0.9745
N4—C9	1.4884	C3—H11	0.9701
N1—H1	0.9001	C4—H12	0.9702
N1—H2	0.9054	C4—H13	0.9737
N2—H3	0.9132	C5—H14	0.9822
N3—H4	0.916	C5—H15	0.9722
N4—H5	0.919	C6—H16	0.9756
C1—C2	1.5302	C6—H17	0.9807
C2—C3	1.4958	C7—H18	0.9743
C4—C5	1.5112	C7—H19	0.9745
C6—C7	1.5377	C8—H20	0.9749
C7—C8	1.4833	C8—H21	0.9717
C9—C10	1.5164	C9—H22	0.9735
C10—C11	1.4208	C9—H23	0.977
C10—C23	1.3992	C12—H24	0.9345
C11—C12	1.4468	C13—H25	0.9304
C11—C16	1.4295	C14—H26	0.9328
C12—C13	1.3704	C15—H27	0.9344
C13—C14	1.3926	C17—H28	0.9341
C14—C15	1.3645	C19—H29	0.9346
C15—C16	1.4169	C20—H30	0.9299
C16—C17	1.4043	C21—H31	0.9331
C17—C18	1.3807	C22—H32	0.9355
Cu1···C22	3.3948	H2···H9	2.5554
Cu1···C23	3.6677	H2···Cl3^x	2.9568
Cu1···O1^i	3.781	H3···Cl1^ii	2.4123
Cu1···H18	3.6645	H3···H15	2.5069
Cu1···H32	3.01	H3···H9	2.4386
Cu1···H9	3.5386	H4···H18	2.396
Cl1···O1^i	3.2354	H4···Cl3	2.4975
Cl1···N2^ii	3.2535	H4···H13	2.5137
Cl3···O1^iii	3.3695	H5···H24	2.5038
Cl3···N3	3.3713	H5···C11	2.8992
Cl1···H16	3.0359	H5···C12	2.8987
Cl1···H20	2.8886	H5···H1	2.2922
Cl1···H3^ii	2.4123	H5···O1^i	2.1903
Cl3···H32	3.135	H6···H27^vii	2.4825
Cl3···H2^iv	2.9568	H7···C18	2.9831
Cl3···H4	2.4975	H7···H10	2.4431
O1···C2	3.3492	H7···C19	3.0796
O1···Cl3^iii	3.3695	H7···C23	2.9875
O1···Cu1^v	3.781	H8···O1	2.6462
O1···Cl1^v	3.2354	H9···Cu1	3.5386
O1···N1^v	3.223	H9···H2	2.5554
O1···N4^v	3.0138	H9···H3	2.4386
O1···H2^v	2.7875	H10···C21	3.0267
O1···H5^v	2.1903	H10···H13	2.4153
O1···H8	2.6462	H10···H7	2.4431
N1···O1^i	3.223	H11···H12	2.4782
N1···C10	3.3769	H11···C13^v	3.0262
N1···C23	3.4098	H12···H30^xi	2.5961
N2···Cl1^ii	3.2535	H12···C19^xi	2.9309
N3···Cl3	3.3713	H12···C20^xi	3.0555
N4···O1^i	3.0138	H12···H11	2.4782
N4···C12	3.4299	H12···H29^xi	2.3274
C2···O1	3.3492	H13···H4	2.5137
C9···C11^vi	3.5578	H13···H10	2.4153
C9···C15^vi	3.5841	H14···H17	2.4808
C9···C16^vi	3.3761	H14···H14^xii	2.5202
C10···N1	3.3769	H15···H3	2.5069
C10···C11^vi	3.5286	H15···H16	2.4219
C10···C10^vi	3.5318	H16···H15	2.4219
C11···C10^vi	3.5286	H16···Cl1	3.0359
C11···C9^vi	3.5578	H16···H20	2.486
C12···C12^vi	3.555	H17···H14	2.4808
C12···N4	3.4299	H18···C9	2.7042
C15···C9^vi	3.5841	H18···Cu1	3.6645
C15···C17^vii	3.3899	H18···H4	2.396
C16···C9^vi	3.3761	H18···H23	2.3233
C17···C15^vii	3.3899	H19···H21^viii	2.4512
C22···Cu1	3.3948	H20···Cl1	2.8886
C23···C23^vi	3.5996	H20···H16	2.486
C23···Cu1	3.6677	H21···C8^viii	2.8904
C23···N1	3.4098	H21···H22	2.2116
C7···H21^viii	3.0898	H21···C7^viii	3.0898
C7···H23	2.9019	H21···H21^viii	2.3162
C8···H21^viii	2.8904	H21···H19^viii	2.4512
C9···H24	2.6389	H22···C12^vi	3.0736
C9···H32	2.6188	H22···C11^vi	3.0273
C9···H18	2.7042	H22···C12	2.6848
C10···H1	2.687	H22···H21	2.2116
C11···H5	2.8992	H22···H24	2.1752
C11···H1	3.0239	H22···C15^vi	3.0267
C11···H22^vi	3.0273	H22···C16^vi	2.9766
C12···H5	2.8987	H22···C14^vi	3.0777
C12···H22	2.6848	H23···C16^vi	3.0348
C12···H22^vi	3.0736	H23···H32	1.9924
C13···H11^i	3.0262	H23···C7	2.9019
C14···H22^vi	3.0777	H23···C22	2.5454
C15···H28^vii	3.043	H23···H18	2.3233
C15···H22^vi	3.0267	H24···C9	2.6389
C16···H22^vi	2.9766	H24···H5	2.5038
C16···H23^vi	3.0348	H24···H22	2.1752
C17···H27^vii	3.0204	H27···H28	2.4464
C18···H7	2.9831	H27···C17^vii	3.0204
C19···H12^ix	2.9309	H27···H6^vii	2.4825
C19···H7	3.0796	H28···H29	2.4133
C20···H12^ix	3.0555	H28···H27	2.4464
C21···H10	3.0267	H28···C15^vii	3.043
C22···H23	2.5454	H29···H12^ix	2.3274
C23···H1	2.9053	H29···H28	2.4133
C23···H7	2.9875	H30···H12^ix	2.5961
H1···C10	2.687	H32···H23	1.9924
H1···C23	2.9053	H32···Cu1	3.01
H1···H5	2.2922	H32···Cl3	3.135
H1···C11	3.0239	H32···C9	2.6188
H2···O1^i	2.7875
Cl1—Cu1—N1	89.25	C10—C23—C18	118.8
Cl1—Cu1—N2	94.83	C10—C23—C22	123.43
Cl1—Cu1—N3	97.72	N1—C1—H6	109.79
Cl1—Cu1—N4	94.02	N1—C1—H7	108.67
N1—Cu1—N2	91.72	C2—C1—H6	108.9
N1—Cu1—N3	172.47	C2—C1—H7	109.33
N1—Cu1—N4	92.02	H6—C1—H7	108.64
N2—Cu1—N3	84.87	C1—C2—H8	108.86
N2—Cu1—N4	170.43	C1—C2—H9	108.83
N3—Cu1—N4	90.35	C3—C2—H8	109.48
Cu1—N1—C1	122.41	C3—C2—H9	109.27
Cu1—N2—C3	122.16	H8—C2—H9	107.03
Cu1—N2—C4	106.51	N2—C3—H10	108.31
C3—N2—C4	111.36	N2—C3—H11	109.15
Cu1—N3—C5	107.56	C2—C3—H10	109.55
Cu1—N3—C6	117.53	C2—C3—H11	108.46
C5—N3—C6	111.27	H10—C3—H11	107.92
Cu1—N4—C8	114.26	N2—C4—H12	109.57
Cu1—N4—C9	115.4	N2—C4—H13	110.58
C8—N4—C9	109.38	C5—C4—H12	110.28
Cu1—N1—H2	107.57	C5—C4—H13	109.41
C1—N1—H1	106.89	H12—C4—H13	108.54
Cu1—N1—H1	106.29	N3—C5—H14	109.66
H1—N1—H2	106.76	N3—C5—H15	110.14
C1—N1—H2	106.05	C4—C5—H14	110.59
C3—N2—H3	104.52	C4—C5—H15	109.43
Cu1—N2—H3	105.32	H14—C5—H15	108.9
C4—N2—H3	105.69	N3—C6—H16	108.86
Cu1—N3—H4	107.29	N3—C6—H17	109.91
C5—N3—H4	106.64	C7—C6—H16	109.6
C6—N3—H4	105.96	C7—C6—H17	108.97
C9—N4—H5	106.09	H16—C6—H17	108.79
C8—N4—H5	106.04	C6—C7—H18	108.72
Cu1—N4—H5	104.81	C6—C7—H19	108.75
N1—C1—C2	111.47	C8—C7—H18	109.13
C1—C2—C3	113.18	C8—C7—H19	109.05
N2—C3—C2	113.32	H18—C7—H19	106.79
N2—C4—C5	108.46	N4—C8—H20	107.89
N3—C5—C4	108.13	N4—C8—H21	108.83
N3—C6—C7	110.69	C7—C8—H20	109.28
C6—C7—C8	114.16	C7—C8—H21	108.05
N4—C8—C7	114.79	H20—C8—H21	107.79
N4—C9—C10	111.95	N4—C9—H22	109.3
C9—C10—C23	119.81	N4—C9—H23	109.53
C11—C10—C23	120.05	C10—C9—H22	109.38
C9—C10—C11	120.12	C10—C9—H23	109.55
C12—C11—C16	116.81	H22—C9—H23	107
C10—C11—C12	122.82	C11—C12—H24	119.67
C10—C11—C16	120.25	C13—C12—H24	120.04
C11—C12—C13	120.29	C12—C13—H25	119.1
C12—C13—C14	121.73	C14—C13—H25	119.17
C13—C14—C15	120.23	C13—C14—H26	120.08
C14—C15—C16	120.45	C15—C14—H26	119.69
C11—C16—C17	119.07	C14—C15—H27	119.67
C11—C16—C15	120.44	C16—C15—H27	119.87
C15—C16—C17	120.48	C16—C17—H28	119.46
C16—C17—C18	120.9	C18—C17—H28	119.64
C17—C18—C23	120.74	C18—C19—H29	119.46
C17—C18—C19	120.04	C20—C19—H29	119.59
C19—C18—C23	119.22	C19—C20—H30	119.64
C18—C19—C20	120.95	C21—C20—H30	119.93
C19—C20—C21	120.43	C20—C21—H31	119.69
C20—C21—C22	121.08	C22—C21—H31	119.23
C21—C22—C23	120.52	C21—C22—H32	119.57
C18—C23—C22	117.76	C23—C22—H32	119.91
Cl1—Cu1—N1—C1	−123.16	C6—C7—C8—N4	−68.30
N2—Cu1—N1—C1	−28.35	N4—C9—C10—C23	−97.65
N4—Cu1—N1—C1	142.84	N4—C9—C10—C11	81.26
Cl1—Cu1—N2—C3	118.37	C23—C10—C11—C12	179.76
Cl1—Cu1—N2—C4	−112.21	C9—C10—C11—C12	0.86
N1—Cu1—N2—C3	28.98	C9—C10—C11—C16	176.71
N1—Cu1—N2—C4	158.4	C9—C10—C23—C22	1.58
N3—Cu1—N2—C3	−144.29	C11—C10—C23—C18	1.3
N3—Cu1—N2—C4	−14.87	C11—C10—C23—C22	−177.33
Cl1—Cu1—N3—C5	79.79	C23—C10—C11—C16	−4.39
Cl1—Cu1—N3—C6	−46.66	C9—C10—C23—C18	−179.79
N2—Cu1—N3—C5	−14.41	C10—C11—C12—C13	177.39
N2—Cu1—N3—C6	−140.86	C10—C11—C16—C17	3.77
N4—Cu1—N3—C5	173.89	C16—C11—C12—C13	1.4
N4—Cu1—N3—C6	47.45	C10—C11—C16—C15	−177.37
Cl1—Cu1—N4—C8	53.08	C12—C11—C16—C17	179.86
Cl1—Cu1—N4—C9	−178.84	C12—C11—C16—C15	−1.28
N1—Cu1—N4—C8	142.47	C11—C12—C13—C14	−1.92
N1—Cu1—N4—C9	−89.45	C12—C13—C14—C15	2.28
N3—Cu1—N4—C8	−44.68	C13—C14—C15—C16	−2.11
N3—Cu1—N4—C9	83.4	C14—C15—C16—C17	−179.48
Cu1—N1—C1—C2	49.57	C14—C15—C16—C11	1.67
C3—N2—C4—C5	176.4	C15—C16—C17—C18	−178.89
Cu1—N2—C4—C5	41	C11—C16—C17—C18	−0.03
Cu1—N2—C3—C2	−52.20	C16—C17—C18—C23	−3.07
C4—N2—C3—C2	−179.52	C16—C17—C18—C19	176.24
Cu1—N3—C6—C7	−61.09	C17—C18—C19—C20	−179.58
C6—N3—C5—C4	170.69	C17—C18—C23—C22	−178.86
Cu1—N3—C5—C4	40.64	C23—C18—C19—C20	−0.25
C5—N3—C6—C7	174.3	C17—C18—C23—C10	2.44
Cu1—N4—C8—C7	61.3	C19—C18—C23—C22	1.82
C9—N4—C8—C7	−69.79	C19—C18—C23—C10	−176.88
Cu1—N4—C9—C10	71.02	C18—C19—C20—C21	−1.77
C8—N4—C9—C10	−158.51	C19—C20—C21—C22	2.22
N1—C1—C2—C3	−67.61	C20—C21—C22—C23	−0.57
C1—C2—C3—N2	69.81	C21—C22—C23—C18	−1.41
N2—C4—C5—N3	−55.46	C21—C22—C23—C10	177.23
N3—C6—C7—C8	66.16

Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1, −y, −z+1; (iii) −x+1/2, −y+1/2, −z+1/2; (iv) x−1/2, −y, z; (v) −x+1, y+1/2, −z+1/2; (vi) −x+1/2, y, −z; (vii) −x+1, −y, −z; (viii) −x+1/2, −y−1/2, −z+1/2; (ix) x, −y+1/2, z−1/2; (x) x+1/2, −y, z; (xi) x, −y+1/2, z+1/2; (xii) −x+1/2, y, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H3···Cl1^ii	0.91	2.410	3.2535	153
N3—H4···Cl3	0.92	2.5	3.3713	160
N4—H5···O1^i	0.92	2.19	3.0138	149

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

(6) Calcium bis(phenxypenicillin) dihydrate

Crystal data

C32H38CaN4O12S2	Z = 4
Mr = 774.88	F(000) = 1472
Orthorhombic, C2221	Dx = 1.353 Mg m^−3
Hall symbol: C 2c 2	Mo K\a radiation, λ = 0.71070 Å
a = 19.036 (10) Å	µ = 0.35 mm^−1
b = 6.508 (2) Å	T = 0 K
c = 29.178 (18) Å	× × mm
V = 3615 (3) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text	Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.572	0.5	0	0.02*
S1	0.40325	0.65975	0.12550	0.02*
O1	0.58275	0.18975	−0.04250	0.02*
O3	0.23325	0.37175	0.053	0.02*
O4	0.494	0.361	0.05	0.02*
O5	0.476	0.0435	0.0735	0.02*
O6	0.166	0.889	0.0465	0.02*
O7	0.1845	0.901	0.1675	0.02*
N1	0.35425	0.43975	0.0575	0.02*
N2	0.258	0.817	0.091	0.02*
C1	0.38625	0.38175	0.1375	0.02*
C2	0.38575	0.28425	0.086	0.02*
C3	0.37425	0.65325	0.0655	0.02*
C4	0.297	0.714	0.055	0.02*
C5	0.28375	0.47725	0.054	0.02*
C6	0.4465	0.301	0.1675	0.02*
C7	0.315	0.356	0.16	0.02*
C8	0.45825	0.21975	0.0685	0.02*
C9	0.19425	0.89275	0.086	0.02*
C10	0.1605	0.9795	0.1285	0.02*
C11	0.15725	0.71975	0.1815	0.02*
C12	0.177	0.653	0.2225	0.02*
C13	0.152	0.471	0.24	0.02*
C14	0.107	0.353	0.2145	0.02*
C15	0.08725	0.41675	0.1755	0.02*
C16	0.11325	0.59525	0.154	0.02*

Geometric parameters (Å, º)

Ca1—O1	2.3783	N2—C9	1.318
Ca1—O4	2.2697	C1—C2	1.6312
S1—C1	1.871	C1—C6	1.5355
S1—C3	1.8361	C1—C7	1.5161
O3—C5	1.1817	C2—C8	1.5302
O4—C8	1.2647	C3—C4	1.5533
O5—C8	1.2046	C4—C5	1.5616
O6—C9	1.2721	C9—C10	1.5064
O7—C10	1.3284	C11—C12	1.3271
O7—C11	1.3518	C11—C16	1.4149
N1—C2	1.4406	C12—C13	1.3748
N1—C3	1.4595	C13—C14	1.3701
N1—C5	1.3679	C14—C15	1.2682
N2—C4	1.4505	C15—C16	1.41
S1···O4	3.4084	N2···S1	3.1154
S1···O5^i	3.2338	N2···O3	3.1381
S1···N2	3.1154	N2···O7	2.6905
O1···O5^ii	2.6929	N2···N1	3.2156
O1···O3^iii	2.9089	N2···C11	3.3244
O1···O6^iv	3.1687	C3···O4	3.0031
O3···N2	3.1381	C3···O5^i	3.2026
O3···C9^v	3.346	C4···C5^vi	3.4246
O3···C5^vi	3.4113	C5···C7	3.2469
O3···O1^vii	2.9089	C5···O3^vi	3.4113
O4···S1	3.4084	C5···C4^vi	3.4246
O4···N1	2.718	C5···C5^vi	3.1651
O4···C3	3.0031	C6···O5	3.2629
O5···S1^v	3.2338	C6···C16^x	3.4676
O5···C3^v	3.2026	C7···C5	3.2469
O5···C6	3.2629	C9···O3^i	3.3461
O5···O1^ii	2.6929	C9···C16	3.1722
O6···O6^viii	3.0742	C10···C15^i	3.4529
O6···O1^ix	3.1687	C11···N2	3.3244
O7···N2	2.6905	C15···C10^v	3.4529
N1···O4	2.718	C16···C9	3.1722
N1···N2	3.2156	C16···C6^xi	3.4676
O1—Ca1—O4	93.04	C6—C1—C7	112.55
O1—Ca1—O1^vi	170.13	N1—C2—C1	105.13
O1—Ca1—O4^vi	93.41	N1—C2—C8	112.06
O1—Ca1—O6^x	88.55	C1—C2—C8	114.13
O1—Ca1—O6^iv	83.96	S1—C3—N1	104.65
O1^vi—Ca1—O4	93.41	S1—C3—C4	117.83
O4—Ca1—O4^vi	98.28	N1—C3—C4	87.93
O4—Ca1—O6^x	90.26	N2—C4—C3	117.35
O4—Ca1—O6^iv	171.12	N2—C4—C5	112.76
O1^vi—Ca1—O4^vi	93.04	C3—C4—C5	84.57
O1^vi—Ca1—O6^x	83.96	O3—C5—N1	134.13
O1^vi—Ca1—O6^iv	88.55	O3—C5—C4	134.84
O4^vi—Ca1—O6^x	171.12	N1—C5—C4	90.93
O4^vi—Ca1—O6^iv	90.26	O4—C8—O5	126.36
O6^x—Ca1—O6^iv	81.33	O4—C8—C2	115.36
C1—S1—C3	95.98	O5—C8—C2	118.28
Ca1—O4—C8	156.36	O6—C9—N2	118.84
Ca1^xi—O6—C9	146.71	O6—C9—C10	124.94
C10—O7—C11	117.55	N2—C9—C10	116.22
C2—N1—C3	117.9	O7—C10—C9	114.48
C2—N1—C5	125.23	O7—C11—C12	116.7
C3—N1—C5	95.63	O7—C11—C16	123.74
C4—N2—C9	124.33	C12—C11—C16	119.44
S1—C1—C2	101.82	C11—C12—C13	121.25
S1—C1—C6	107.96	C12—C13—C14	119.84
S1—C1—C7	110.04	C13—C14—C15	119.29
C2—C1—C6	113.35	C14—C15—C16	124.38
C2—C1—C7	110.53	C11—C16—C15	115.3
O1—Ca1—O4—C8	7.74	C4—N2—C9—O6	−4.92
O1^vi—Ca1—O4—C8	−164.78	C4—N2—C9—C10	175.44
O4^vi—Ca1—O4—C8	101.64	C7—C1—C2—N1	81.33
O6^x—Ca1—O4—C8	−80.82	C6—C1—C2—N1	−151.24
C3—S1—C1—C2	20.74	C7—C1—C2—C8	−155.49
C3—S1—C1—C6	140.32	S1—C1—C2—N1	−35.55
C3—S1—C1—C7	−96.49	S1—C1—C2—C8	87.63
C1—S1—C3—C4	94.61	C6—C1—C2—C8	−28.06
C1—S1—C3—N1	−0.88	C1—C2—C8—O4	−85.28
Ca1—O4—C8—O5	33.53	C1—C2—C8—O5	94.53
Ca1—O4—C8—C2	−146.67	N1—C2—C8—O4	34.06
Ca1^xi—O6—C9—N2	−169.99	N1—C2—C8—O5	−146.13
Ca1^xi—O6—C9—C10	9.61	S1—C3—C4—N2	14.15
C11—O7—C10—C9	−82.43	S1—C3—C4—C5	−98.71
C10—O7—C11—C16	9.99	N1—C3—C4—N2	119.63
C10—O7—C11—C12	−173.98	N1—C3—C4—C5	6.78
C3—N1—C5—C4	7.7	N2—C4—C5—O3	51.97
C2—N1—C5—C4	137.88	C3—C4—C5—O3	169.4
C3—N1—C2—C8	−83.24	C3—C4—C5—N1	−7.23
C5—N1—C2—C8	156.12	N2—C4—C5—N1	−124.66
C5—N1—C3—S1	110.5	O6—C9—C10—O7	155.12
C5—N1—C2—C1	−79.37	N2—C9—C10—O7	−25.26
C3—N1—C5—O3	−168.97	O7—C11—C12—C13	179.64
C2—N1—C3—S1	−24.57	C16—C11—C12—C13	−4.15
C2—N1—C5—O3	−38.79	O7—C11—C16—C15	−176.96
C2—N1—C3—C4	−142.82	C12—C11—C16—C15	7.11
C5—N1—C3—C4	−7.75	C11—C12—C13—C14	1.42
C3—N1—C2—C1	41.27	C12—C13—C14—C15	−2.17
C9—N2—C4—C5	−90.01	C13—C14—C15—C16	5.92
C9—N2—C4—C3	174.17	C14—C15—C16—C11	−8.33

Symmetry codes: (i) x, y+1, z; (ii) x, −y, −z; (iii) x+1/2, −y+1/2, −z; (iv) x+1/2, −y+3/2, −z; (v) x, y−1, z; (vi) x, −y+1, −z; (vii) x−1/2, −y+1/2, −z; (viii) x, −y+2, −z; (ix) x−1/2, −y+3/2, −z; (x) x+1/2, y−1/2, z; (xi) x−1/2, y+1/2, z.

(7) tris(Methyltriethylammonium) bis(dicarbonyl-(4,4',5,5'-tetracyan-2,2'-bi -imidazole-N,N')-iridium) dicyan-(4,4',5,5'-tetracyan-2,2'-bi-imidazole-N,N') -platinum acetonitrile solvate.

Crystal data

2(C12IrN8O2^−)·(C12N10Pt^−)·3(C7H18N^+)·3(C2H3N)	Z = 4
Mr = see text	F(000) = 1160
Orthorhombic, Cmc21	Dx = 1.785 Mg m^−3
Hall symbol: C 2c -2	Mo K\a radiation, λ = 0.71073 Å
a = 15.151 (19) Å	µ = 6.13 mm^−1
b = 22.13 (2) Å	T = 0 K
c = 6.874 (5) Å	× × mm
V = 2305 (4) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text	Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pt	0.5	−0.00199	0.75	0.02*
O1	0.37096	−0.10019	0.75005	0.02*
N1	0.41492	0.06858	0.74534	0.02*
N2	0.3933	0.17459	0.75046	0.02*
N3	0.16788	0.21028	0.75020	0.02*
N4	0.20427	0.00112	0.75	0.02*
C1	0.45421	0.12635	0.74982	0.02*
C2	0.31665	0.1467	0.74765	0.02*
C3	0.32796	0.0855	0.74394	0.02*
C4	0.23525	0.18282	0.74445	0.02*
C5	0.25801	0.03965	0.75111	0.02*
C6	0.41741	−0.06162	0.74993	0.02*
N9	0	0.13781	0.24991	0.02*
C13	0	0.20265	0.24073	0.02*
C15	0.15324	0.13049	0.24966	0.02*
C17	0	0.10446	0.44837	0.02*
C18	0.07478	0.11149	0.11764	0.02*
C19	0	0.03652	0.3763	0.02*
N10	0	0.23123	0.75207	0.02*
C20	0	0.18005	0.74776	0.02*
C21	0	0.11271	0.74867	0.02*

Geometric parameters (Å, º)

Pt—N1	2.0252	N9—C13	1.4363 (18)
Pt—C6	1.8186	N9—C17	1.5511 (19)
O1—C6	1.1063	N10—C20	1.1330 (14)
N1—C1	1.4106	C1—C1^i	1.3875
N1—C3	1.3697	C2—C3	1.3654
N2—C1	1.4111	C2—C4	1.4698
N2—C2	1.3153	C3—C5	1.468
N3—C4	1.1886	C15—C18	1.5535
N4—C5	1.179	C17—C19	1.583 (2)
N9—C18	1.5651	C20—C21	1.4902 (19)
Pt···Pt^ii	3.438 (4)	C13···C20^xii	3.425 (4)
Pt···Pt^iii	3.438 (4)	C13···C20^xiii	3.425 (4)
Pt···N1^ii	3.9834	C13···N10^xiii	3.418 (4)
Pt···N1^iii	3.9277	C13···N2^xiv	3.162
Pt···C6^ii	3.9197	C13···N2^xv	3.162
Pt···C6^iii	3.9188	C15···C19	3.2362
Pt···Pt^iv	3.438 (4)	C15···N4^iv	3.0134
Pt···Pt^v	3.438 (4)	C15···O1^iv	3.3661
Pt···N1^iv	3.9834	C17···C20	2.652 (3)
Pt···N1^v	3.9277	C17···C21	2.072 (3)
Pt···C6^iv	3.9197	C17···C20^viii	2.652 (3)
Pt···C6^v	3.9188	C17···C21^viii	2.072 (3)
O1···C15^v	3.3661	C18···C20^xii	3.1702
N1···Pt^ii	3.9277	C18···C20^xiii	3.1702
N1···Pt^iii	3.9834	C18···C21^xii	2.778
N1···Pt^iv	3.9277	C18···N4^iv	3.2996
N1···Pt^v	3.9834	C18···C21^xiii	2.778
N1···C6^iv	3.4091	C19···C15	3.2362
N2···N2^i	3.2332	C19···C21^viii	3.065 (4)
N2···C13^vi	3.162	C19···N4^iv	3.3205
N2···C13^vii	3.162	C19···C21^iv	3.417 (4)
N3···N10	2.5855	C19···C21	3.065 (4)
N3···C20	2.6301	C19···N4^xvi	3.3205
N3···C21	3.3365	C19···C21^xvi	3.417 (4)
N3···N10^viii	2.5855	C19···C15^viii	3.2362
N3···C20^viii	2.6301	C20···N3	2.6301
N3···C21^viii	3.3365	C20···C4	3.5649
N4···C19^ix	3.3205	C20···C13	3.521 (4)
N4···C15^v	3.0134	C20···C13^x	3.425 (4)
N4···C18^v	3.2996	C20···C17	2.652 (3)
N4···C19^v	3.3205	C20···C18^x	3.1702
N10···C13^x	3.418 (4)	C20···N3^viii	2.6301
N10···N3^viii	2.5855	C20···C4^viii	3.5649
N10···C13^xi	3.418 (4)	C20···C13	3.521 (4)
N10···N3	2.5855	C20···C13^xi	3.425 (4)
C4···C20	3.5649	C20···C17	2.652 (3)
C4···C20^viii	3.5649	C20···C18^xi	3.1702
C5···C6	3.2947	C21···N3	3.3365
C6···Pt^ii	3.9188	C21···C17	2.072 (3)
C6···Pt^iii	3.9197	C21···C18^x	2.778
C6···C5	3.2947	C21···C19	3.065 (4)
C6···N1^v	3.4091	C21···C19^ix	3.417 (4)
C6···Pt^iv	3.9188	C21···N3^viii	3.3365
C6···Pt^v	3.9197	C21···C17	2.072 (3)
C13···C20	3.521 (4)	C21···C18^xi	2.778
C13···C20^viii	3.521 (4)	C21···C19	3.065 (4)
C13···N10^xii	3.418 (4)	C21···C19^v	3.417 (4)
N1—Pt—C6	96.98	N2—C1—C1^i	130.84
N1—Pt—N1^i	79.06	N1—C1—N2	114.19
N1—Pt—C6^i	175.95	N1—C1—C1^i	114.96
N1^i—Pt—C6	175.95	N2—C2—C4	119.07
C6—Pt—C6^i	86.96	N2—C2—C3	110.79
N1^i—Pt—C6^i	96.98	C3—C2—C4	130.12
Pt—N1—C1	115.46	N1—C3—C5	120.35
Pt—N1—C3	145.4	N1—C3—C2	113.06
C1—N1—C3	99.11	C2—C3—C5	126.47
C1—N2—C2	102.85	N3—C4—C2	176.48
C17—N9—C18	109.5	N4—C5—C3	176.56
C17—N9—C18^viii	109.5	Pt—C6—O1	176.03
C18—N9—C18^viii	92.75	N9—C17—C19	100.18
C13—N9—C18	110.26	N9—C18—C15	96.54
C13—N9—C18^viii	110.26	N10—C20—C21	178.26
C13—N9—C17	120.93
C6—Pt—N1—C1	178.31	C1—N2—C2—C4	−179.11
C6—Pt—N1—C3	0.73	C13—N9—C18—C15	72.25
N1^i—Pt—N1—C1	−2.57	C13—N9—C17—C19	180
N1^i—Pt—N1—C3	179.86	C18—N9—C17—C19	−50.17
Pt—N1—C1—N2	−178.77	C17—N9—C18—C15	−63.15
Pt—N1—C1—C1^i	2.18	C18^viii—N9—C18—C15	−174.96
C3—N1—C1—N2	−0.16	N1—C1—C1^i—N1^i	0.02
C3—N1—C1—C1^i	−179.21	N2—C1—C1^i—N1^i	−178.86
Pt—N1—C3—C2	177.65	N2—C1—C1^i—N2^i	0
Pt—N1—C3—C5	1.45	N1—C1—C1^i—N2^i	178.86
C1—N1—C3—C2	−0.13	C4—C2—C3—N1	178.87
C1—N1—C3—C5	−176.33	C4—C2—C3—C5	−5.21
C2—N2—C1—N1	0.39	N2—C2—C3—N1	0.4
C2—N2—C1—C1^i	179.25	N2—C2—C3—C5	176.32
C1—N2—C2—C3	−0.45

Symmetry codes: (i) −x+1, y, z; (ii) −x+1, −y, z−1/2; (iii) −x+1, −y, z+1/2; (iv) x, −y, z−1/2; (v) x, −y, z+1/2; (vi) −x+1/2, −y+1/2, z+1/2; (vii) x+1/2, −y+1/2, z+1/2; (viii) −x, y, z; (ix) −x, −y, z+1/2; (x) x, y, z+1; (xi) −x, y, z+1; (xii) −x, y, z−1; (xiii) x, y, z−1; (xiv) −x+1/2, −y+1/2, z−1/2; (xv) x−1/2, −y+1/2, z−1/2; (xvi) −x, −y, z−1/2.

(8) 4-(2-Chloro-4,5-dimethoxybenzylidene)-2-methyl-5-oxazolone

Crystal data

C13H12ClNO4	Z = 8
Mr = 281.69	F(000) = 1072
Orthorhombic, Cmca	Dx = 1.367 Mg m^−3
Hall symbol: -C 2bc 2	Mo K\a radiation, λ = 0.71073 Å
a = 6.707 (1) Å	µ = 0.30 mm^−1
b = 17.023 (4) Å	T = 0 K
c = 22.938 (2) Å	× × mm
V = 2618.9 (8) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cl1	0	0.3023	0.3021	0.02*
O1	0	−0.02870	0.3698	0.02*
O2	0	0.07805	0.4488	0.02*
O3	0	0.09395	0.0695	0.02*
O4	0	0.22365	0.0885	0.02*
N1	0	0.04165	0.16	0.02*
C1	0	0.2024	0.3186	0.02*
C2	0	0.1464	0.2742	0.02*
C3	0	0.06710	0.29210	0.02*
C4	0	0.04615	0.3495	0.02*
C5	0	0.10465	0.39340	0.02*
C6	0	0.1824	0.3774	0.02*
C7	0	−0.08920	0.327	0.02*
C8	0	0.13575	0.4946	0.02*
C9	0	0.169	0.2135	0.02*
C10	0	0.1241	0.1658	0.02*
C11	0	0.1581	0.1065	0.02*
C12	0	0.02845	0.1055	0.02*
C13	0	−0.04880	0.07460	0.02*

Geometric parameters (Å, º)

Cl1—C1	1.7422 (4)	C1—C2	1.3950 (3)
O1—C4	1.3566 (3)	C1—C6	1.3911 (3)
O1—C7	1.4229 (3)	C2—C3	1.4110 (3)
O2—C5	1.3490 (3)	C2—C9	1.4445 (3)
O2—C8	1.4382 (3)	C3—C4	1.3641 (3)
O3—C11	1.3830 (3)	C4—C5	1.4162 (3)
O3—C12	1.3875 (3)	C5—C6	1.3735 (3)
O4—C11	1.1898 (3)	C9—C10	1.3347 (3)
N1—C10	1.4098 (3)	C10—C11	1.4782 (3)
N1—C12	1.2702 (3)	C12—C13	1.4939 (4)
Cl1···C7^i	3.4901 (8)	C5···C11^ix	3.4747 (8)
Cl1···C7^ii	3.4901 (8)	C5···C11^x	3.4747 (8)
O1···O2	2.5663 (6)	C5···C12^ix	3.5957 (8)
O2···O1	2.5663 (6)	C5···C12^x	3.5957 (8)
O3···C13^iii	3.3935 (8)	C6···C11^vii	3.3990 (8)
O3···C13^iv	3.3935 (8)	C6···C11^viii	3.3990 (8)
O4···C8^v	3.2199 (8)	C6···C11^ix	3.3990 (8)
O4···C8^vi	3.2199 (8)	C6···C11^x	3.3990 (8)
N1···C3	3.0609 (7)	C7···Cl1^xi	3.4901 (8)
N1···C4^vii	3.3614 (8)	C7···Cl1^xii	3.4901 (8)
N1···C4^viii	3.3614 (8)	C8···O4^xiii	3.2199 (8)
N1···C4^ix	3.3614 (8)	C8···O4^xiv	3.2199 (8)
N1···C4^x	3.3614 (8)	C9···C1^vii	3.4801 (8)
C1···C9^vii	3.4801 (8)	C9···C1^viii	3.4801 (8)
C1···C9^viii	3.4801 (8)	C9···C2^vii	3.3873 (8)
C1···C9^ix	3.4801 (8)	C9···C2^viii	3.3873 (8)
C1···C9^x	3.4801 (8)	C9···C1^ix	3.4801 (8)
C2···C2^vii	3.5325 (8)	C9···C1^x	3.4801 (8)
C2···C2^viii	3.5325 (8)	C9···C2^ix	3.3873 (8)
C2···C9^vii	3.3873 (8)	C9···C2^x	3.3873 (8)
C2···C9^viii	3.3873 (8)	C11···C5^vii	3.4747 (8)
C2···C2^ix	3.5325 (8)	C11···C5^viii	3.4747 (8)
C2···C2^x	3.5325 (8)	C11···C6^vii	3.3990 (8)
C2···C9^ix	3.3873 (8)	C11···C6^viii	3.3990 (8)
C2···C9^x	3.3873 (8)	C11···C5^ix	3.4747 (8)
C3···N1	3.0609 (7)	C11···C5^x	3.4747 (8)
C4···N1^vii	3.3614 (8)	C11···C6^ix	3.3990 (8)
C4···N1^viii	3.3614 (8)	C11···C6^x	3.3990 (8)
C4···C12^vii	3.5217 (8)	C12···C4^vii	3.5217 (8)
C4···C12^viii	3.5217 (8)	C12···C4^viii	3.5217 (8)
C4···N1^ix	3.3614 (8)	C12···C5^vii	3.5957 (8)
C4···N1^x	3.3614 (8)	C12···C5^viii	3.5957 (8)
C4···C12^ix	3.5217 (8)	C12···C4^ix	3.5217 (8)
C4···C12^x	3.5217 (8)	C12···C4^x	3.5217 (8)
C5···C11^vii	3.4747 (8)	C12···C5^ix	3.5957 (8)
C5···C11^viii	3.4747 (8)	C12···C5^x	3.5957 (8)
C5···C12^vii	3.5957 (8)	C13···O3^iii	3.3935 (8)
C5···C12^viii	3.5957 (8)	C13···O3^iv	3.3935 (8)
C4—O1—C7	116.3	O2—C5—C4	115.71
C5—O2—C8	117.31	O2—C5—C6	125.11
C11—O3—C12	105.62	C4—C5—C6	119.18
C10—N1—C12	105.6	C1—C6—C5	119.67
Cl1—C1—C2	120.56	C2—C9—C10	129.62
Cl1—C1—C6	116.71	N1—C10—C9	130.35
C2—C1—C6	122.73	N1—C10—C11	107.64
C1—C2—C3	116.19	C9—C10—C11	122.01
C1—C2—C9	121.45	O3—C11—O4	121.84
C3—C2—C9	122.36	O3—C11—C10	104.8
C2—C3—C4	122.07	O4—C11—C10	133.36
O1—C4—C3	125.23	O3—C12—N1	116.33
O1—C4—C5	114.61	O3—C12—C13	115.15
C3—C4—C5	120.16	N1—C12—C13	128.51
C7—O1—C4—C5	180	C1—C2—C9—C10	−180.00
C7—O1—C4—C3	0	C3—C2—C9—C10	0
C8—O2—C5—C6	0	C9—C2—C3—C4	180
C8—O2—C5—C4	−180.00	C1—C2—C3—C4	0
C11—O3—C12—N1	0	C2—C3—C4—O1	180
C11—O3—C12—C13	180	C2—C3—C4—C5	0
C12—O3—C11—C10	0	O1—C4—C5—O2	0
C12—O3—C11—O4	180	C3—C4—C5—O2	180
C12—N1—C10—C11	0	O1—C4—C5—C6	−180.00
C12—N1—C10—C9	−180.00	C3—C4—C5—C6	0
C10—N1—C12—O3	0	C4—C5—C6—C1	0
C10—N1—C12—C13	−180.00	O2—C5—C6—C1	180
Cl1—C1—C6—C5	180	C2—C9—C10—C11	180
Cl1—C1—C2—C3	−180.00	C2—C9—C10—N1	0
Cl1—C1—C2—C9	0	C9—C10—C11—O4	0
C2—C1—C6—C5	0	N1—C10—C11—O3	0
C6—C1—C2—C9	−180.00	N1—C10—C11—O4	−180.00
C6—C1—C2—C3	0	C9—C10—C11—O3	180

Symmetry codes: (i) −x, y+1/2, −z+1/2; (ii) x, y+1/2, −z+1/2; (iii) x, −y, −z; (iv) −x, −y, −z; (v) −x, −y+1/2, z−1/2; (vi) x, −y+1/2, z−1/2; (vii) −x−1/2, y, −z+1/2; (viii) −x+1/2, y, −z+1/2; (ix) x−1/2, y, −z+1/2; (x) x+1/2, y, −z+1/2; (xi) −x, y−1/2, −z+1/2; (xii) x, y−1/2, −z+1/2; (xiii) −x, −y+1/2, z+1/2; (xiv) x, −y+1/2, z+1/2.

(9) Insine 5'-monphosphate nnahydrate

Crystal data

C10H12N4O8P·2.5(H2O)·8(H2O)	Z = 8
Mr = 536.38	F(000) = 2272
Orthorhombic, C2221	Dx = 1.621 Mg m^−3
Hall symbol: C 2c 2	Mo K\a radiation, λ = 0.71073 Å
a = 23.1914 (10) Å	µ = 0.22 mm^−1
b = 8.650 (1) Å	T = 0 K
c = 21.900 (1) Å	× × mm
V = 4393.3 (6) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text	Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
P1	0.12285	0.11165	0.2228	0.02*
O1	0.09027	0.00897	0.1788	0.02*
O2	0.19038	0.10198	0.2032	0.02*
O3	0.10808	0.28018	0.21455	0.02*
O4	0.1186	0.05475	0.28705	0.02*
O5	0.27233	−0.02242	0.1171	0.02*
O6	0.36817	0.27928	0.1555	0.02*
O7	0.3752	−0.00210	0.2031	0.02*
O8	0.24465	0.43745	−0.12720	0.02*
N1	0.2794	0.1908	0.0529	0.02*
N2	0.21102	0.30508	−0.00200	0.02*
N3	0.36167	0.22767	−0.01370	0.02*
N4	0.33413	0.35833	−0.10370	0.02*
C1	0.21635	−0.04615	0.21065	0.02*
C2	0.27540	−0.05215	0.1825	0.02*
C3	0.30827	0.10012	0.10215	0.02*
C4	0.31697	0.19173	0.16070	0.02*
C5	0.31955	0.0621	0.2074	0.02*
C6	0.22312	0.22523	0.04925	0.02*
C7	0.26235	0.31375	−0.03120	0.02*
C8	0.30602	0.24072	0.00120	0.02*
C9	0.37225	0.28225	−0.06795	0.02*
C10	0.27643	0.37638	−0.09065	0.02*
O25	0.03565	0.01155	0.3171	0.02*	0.5
O27	0.02365	−0.05735	0.33945	0.02*
O28	0.02108	0.08377	0.3542	0.02*
O17	0.041	0.64355	0.3152	0.02*
O19	0.0573	0.7091	0.20015	0.02*
O21	0.12765	0.5	0	0.02*	0.5
O22	0.12888	0.50378	0.12845	0.02*
O23	0	0.4153	0.25	0.02*	0.5
O26	0.115	0.91725	0.0637	0.02*
O31	0.46338	0.12762	0.066	0.02*
O32	0.47328	0.35322	0.054	0.02*
O35	0.0413	0.344	0.421	0.02*	0.5
O36	0.05065	0.62575	0.0712	0.02*	0.5

Geometric parameters (Å, º)

P1—O1	1.5127	N1—C3	1.4923
P1—O2	1.626	N2—C6	1.3474
P1—O3	1.5083	N2—C7	1.3534
P1—O4	1.4939	N3—C9	1.3018
O2—C1	1.4252	N3—C8	1.336
O5—C2	1.4569	N4—C9	1.3519
O5—C3	1.3876	N4—C10	1.3772
O6—C4	1.4129	C1—C2	1.5027
O7—C5	1.4082	C2—C5	1.5239
O8—C10	1.2095	C3—C4	1.5208
O25—O28	1.0792	C4—C5	1.5188
N1—C6	1.3411	C7—C8	1.3886
N1—C8	1.36	C7—C10	1.4475
P1···O25	3.0173	O22···O21	2.8134
O1···O19^i	2.7443	O23···O17	2.6155
O1···O26^i	2.7041	O23···O19	3.0686
O1···O25^ii	2.9217	O23···O3^ii	2.8725
O1···O28^ii	2.7585	O23···O19^ii	3.0686
O2···O5	2.8854	O23···O3	2.8725
O2···C4	3.1761	O23···O7^iii	3.1531
O3···O22	2.7439	O25···O32^v	3.1444
O3···O23	2.8725	O25···O4	2.0672
O3···O23^ii	2.8725	O25···P1	3.0173
O3···O7^iii	2.6362	O25···O6^v	3.0614
O3···C5^iii	3.4184	O25···O1^ii	2.9217
O4···O25	2.0672	O25···O17^i	3.1859
O4···O28	2.7094	O26···N2^viii	3.2378
O4···N4^iv	2.7371	O26···O36	2.9346
O4···O6^v	2.712	O28···O1^ii	2.7585
O5···O2	2.8854	O28···O35	2.7252
O5···O7	3.0446	O28···O4	2.7094
O5···N4^vi	3.2531	O28···C9^iv	3.2202
O5···C7^vi	3.1532	O28···O32^v	2.8348
O5···C8^vi	3.2997	O31···O32	1.9824
O5···C9^vi	3.4029	O31···O6	3.2308
O5···C10^vi	3.1175	O31···O35^x	3.1868
O6···O7	2.6528	O31···O17^v	2.6073
O6···O31	3.2308	O31···N3	3.0593
O6···N1	3.1421	O32···O28^iii	2.8348
O6···O4^iii	2.712	O32···O25^iii	3.1444
O6···O17^v	2.4955	O32···O31	1.9824
O6···O25^iii	3.0614	O32···N3	3.1745
O7···O5	3.0446	O35···O28	2.7252
O7···O6	2.6528	O35···O31^iii	2.4722
O7···O23^vii	3.1531	O35···N3^iv	2.7374
O7···O3^v	2.6362	O35···C9^iv	2.2958
O7···O17^v	2.3505	O36···O26	2.9346
O7···O19^v	3.2058	O36···O19	2.9187
O7···O23^v	3.1531	O36···O21	2.6083
O8···N2	3.072	O36···O22	2.4447
O8···O22^viii	2.7327	O36···O21^viii	2.6083
O8···C6^viii	3.4172	N1···O6	3.1421
O17···C5^iii	3.3467	N2···O21	2.5657
O17···O25^ix	3.1859	N2···O21^viii	2.5657
O17···O19^ii	2.3731	N2···O8	3.072
O17···O23^ii	2.6155	N2···O26^viii	3.2378
O17···O6^iii	2.4955	N3···O32	3.1745
O17···O7^iii	2.3505	N3···O35^x	2.7374
O17···O19	2.6101	N3···O31	3.0593
O17···O23	2.6155	N4···C2^vi	3.442
O17···C4^iii	3.3618	N4···O4^x	2.7371
O17···O31^iii	2.6073	N4···O5^vi	3.2531
O19···O22	2.8941	C2···C10^vi	3.4514
O19···O17	2.6101	C2···N4^vi	3.442
O19···O23^ii	3.0686	C4···O17^v	3.3618
O19···O23	3.0686	C4···O2	3.1761
O19···O36	2.9187	C5···O3^v	3.4184
O19···O7^iii	3.2058	C5···O17^v	3.3467
O21···O36	2.6083	C6···O8^viii	3.4172
O21···N2	2.5657	C7···O5^vi	3.1532
O21···O22	2.8134	C7···C7^viii	3.4999
O21···N2^viii	2.5657	C8···O5^vi	3.2997
O21···O22^viii	2.8134	C9···O5^vi	3.4029
O22···O3	2.7439	C9···O28^x	3.2202
O22···O21^viii	2.8134	C9···O35^x	2.2958
O22···O8^viii	2.7327	C10···O5^vi	3.1175
O22···O36	2.4447	C10···C2^vi	3.4514
O22···O19	2.8941
O1—P1—O2	106.42	O5—C3—C4	106.19
O1—P1—O3	112.19	N1—C3—C4	113.27
O1—P1—O4	111.94	O6—C4—C3	108.83
O2—P1—O3	103.7	O6—C4—C5	114.64
O2—P1—O4	107.17	C3—C4—C5	100.85
O3—P1—O4	114.6	O7—C5—C2	109.64
P1—O2—C1	115.03	O7—C5—C4	106.39
C2—O5—C3	109.72	C2—C5—C4	102.2
C3—N1—C6	126.62	N1—C6—N2	111.48
C3—N1—C8	124.4	N2—C7—C8	112.02
C6—N1—C8	108.76	N2—C7—C10	130.1
C6—N2—C7	103.82	C8—C7—C10	117.73
C8—N3—C9	111.98	N1—C8—N3	127.95
C9—N4—C10	124.78	N1—C8—C7	103.81
O2—C1—C2	111.67	N3—C8—C7	128.18
O5—C2—C1	110.65	N3—C9—N4	125.58
O5—C2—C5	105.67	O8—C10—N4	120.28
C1—C2—C5	116.3	O8—C10—C7	128.41
O5—C3—N1	107.61	N4—C10—C7	111.31
O1—P1—O2—C1	−65.28	C9—N4—C10—C7	4.48
O3—P1—O2—C1	176.22	C9—N4—C10—O8	−175.11
O4—P1—O2—C1	54.64	O2—C1—C2—C5	59.59
P1—O2—C1—C2	170.96	O2—C1—C2—O5	−60.96
C3—O5—C2—C5	−2.20	O5—C2—C5—C4	25.23
C2—O5—C3—N1	−143.71	C1—C2—C5—O7	149.48
C3—O5—C2—C1	124.49	C1—C2—C5—C4	−97.95
C2—O5—C3—C4	−22.12	O5—C2—C5—O7	−87.34
C3—N1—C8—N3	−4.29	O5—C3—C4—O6	158.08
C6—N1—C8—N3	−179.19	N1—C3—C4—O6	−84.03
C6—N1—C8—C7	3.15	O5—C3—C4—C5	37.16
C6—N1—C3—O5	40.54	N1—C3—C4—C5	155.05
C3—N1—C6—N2	−178.22	O6—C4—C5—O7	−38.56
C3—N1—C8—C7	178.05	O6—C4—C5—C2	−153.52
C8—N1—C3—C4	109.51	C3—C4—C5—O7	78.15
C8—N1—C3—O5	−133.44	C3—C4—C5—C2	−36.81
C6—N1—C3—C4	−76.51	C10—C7—C8—N3	4.42
C8—N1—C6—N2	−3.47	N2—C7—C10—O8	1.15
C7—N2—C6—N1	2.14	N2—C7—C10—N4	−178.40
C6—N2—C7—C8	−0.08	C8—C7—C10—O8	176.32
C6—N2—C7—C10	175.32	C8—C7—C10—N4	−3.22
C8—N3—C9—N4	6.57	N2—C7—C8—N1	−1.91
C9—N3—C8—N1	177.21	N2—C7—C8—N3	−179.56
C9—N3—C8—C7	−5.68	C10—C7—C8—N1	−177.92
C10—N4—C9—N3	−6.82

Symmetry codes: (i) x, y−1, z; (ii) −x, y, −z+1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x+1/2, −y+1/2, z+1/2; (v) −x+1/2, y−1/2, −z+1/2; (vi) x, −y, −z; (vii) x+1/2, y−1/2, z; (viii) x, −y+1, −z; (ix) x, y+1, z; (x) −x+1/2, −y+1/2, z−1/2.

(10) catena-((mu!2$-Acetato-O,O')-(acetato-O,O')-(pyridine)-zinc(ii))

Crystal data

C18H22N2O8Zn2	γ = 90°
Mr = 525.16	V = 2181.2 (11) Å^3
Monclinic, P21/n	Z = 4
Hall symbol: -P 2yn	F(000) = 984
a = 8.626 (2) Å	Dx = 1.532 Mg m^−3
b = 28.871 (8) Å	Mo K\a radiation, λ = 0.71073 Å
c = 8.868 (3) Å	µ = 2.24 mm^−1
α = 90°	T = 0 K
β = 99.02 (2)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Zn3	0.3766	0.10455	0.4451	0.02*
Zn4	0.36455	0.1493	−0.06510	0.02*
O1	0.40265	0.04545	0.32695	0.02*
O2	0.1564	0.05875	0.3237	0.02*
O3	0.3963	0.21215	−0.17870	0.02*
O4	0.16295	0.1895	−0.19330	0.02*
O5	0.27855	0.16465	0.3807	0.02*
O6	0.3374	0.1504	0.15385	0.02*
O7	0.3472	0.10235	0.66220	0.02*
O8	0.2784	0.08605	0.8828	0.02*
N1	0.6127	0.11995	0.48105	0.02*
N2	0.60040	0.13330	−0.02655	0.02*
C1	0.26205	0.03625	0.2767	0.02*
C2	0.2311	−0.00030	0.1591	0.02*
C3	0.25935	0.2165	−0.23535	0.02*
C4	0.2082	0.25235	−0.35235	0.02*
C5	0.27595	0.1753	0.24315	0.02*
C6	0.19755	0.2199	0.18915	0.02*
C7	0.2951	0.07475	0.7503	0.02*
C8	0.2552	0.02615	0.69985	0.02*
C9	0.67145	0.1628	0.4682	0.02*
C10	0.8296	0.17120	0.4867	0.02*
C11	0.93365	0.13510	0.51655	0.02*
C12	0.87435	0.09155	0.52915	0.02*
C13	0.716	0.0849	0.51155	0.02*
C14	0.69880	0.15255	−0.11150	0.02*
C15	0.85755	0.14375	−0.08780	0.02*
C16	0.91815	0.1142	0.02365	0.02*
C17	0.81495	0.09350	0.11525	0.02*
C18	0.6615	0.1041	0.084	0.02*

Geometric parameters (Å, º)

Zn3—O1	2.0331	O8—C7	1.2494
Zn3—O2	2.4237	N1—C9	1.3485
Zn3—O5	1.975	N1—C13	1.3474
Zn3—O7	1.9819	N2—C14	1.3407
Zn3—N1	2.06	N2—C18	1.337
Zn4—O3	2.114	C1—C2	1.4782
Zn4—O4	2.2458	C3—C4	1.4829
Zn4—O6	1.9921	C5—C6	1.4977
Zn4—N2	2.0618	C7—C8	1.4964
Zn4—O8^i	1.9982	C9—C10	1.3699
O1—C1	1.2532	C10—C11	1.3738
O2—C1	1.2431	C11—C12	1.3686
O3—C3	1.2156	C12—C13	1.3639
O4—C3	1.2391	C14—C15	1.3761
O5—C5	1.2547	C15—C16	1.3476
O6—C5	1.2476	C16—C17	1.427
O7—C7	1.248	C17—C18	1.3444
Zn3···Zn4	4.6908	O4···C15^iii	3.2145
Zn3···Zn4^ii	4.5484	C4···C14^v	3.5732
Zn3···C11^iii	4.0667	C11···Zn3^vi	4.0667
Zn4···Zn3^i	4.5484	C11···O4^vii	3.3769
Zn4···Zn3	4.6908	C12···O2^vi	3.3949
O2···C12^iii	3.3949	C14···C4^viii	3.5732
O2···C17^iii	3.3751	C15···O4^vi	3.2145
O4···C11^iv	3.3769	C17···O2^vi	3.3751
O1—Zn3—O2	57.01	Zn3—N1—C9	124.09
O1—Zn3—O5	131.7	Zn3—N1—C13	118.4
O1—Zn3—O7	121	C9—N1—C13	117.42
O1—Zn3—N1	94.27	Zn4—N2—C14	120.61
O2—Zn3—O5	94.62	Zn4—N2—C18	121.88
O2—Zn3—O7	101.73	C14—N2—C18	117.51
O2—Zn3—N1	150.86	O1—C1—O2	119.31
O5—Zn3—O7	101.23	O1—C1—C2	117.38
O5—Zn3—N1	102.9	O2—C1—C2	123.28
O7—Zn3—N1	97.5	O3—C3—O4	117.72
O3—Zn4—O4	57.52	O3—C3—C4	121.64
O3—Zn4—O6	119.64	O4—C3—C4	120.63
O3—Zn4—N2	94.19	O5—C5—O6	122.09
O3—Zn4—O8^i	138.2	O5—C5—C6	117.38
O4—Zn4—O6	106.57	O6—C5—C6	120.53
O4—Zn4—N2	149.92	O7—C7—O8	121.87
O4—Zn4—O8^i	97.17	O7—C7—C8	120.01
O6—Zn4—N2	96.07	O8—C7—C8	118.1
O6—Zn4—O8^i	98.26	N1—C9—C10	122.19
O8^i—Zn4—N2	98.92	C9—C10—C11	119.8
Zn3—O1—C1	100.49	C10—C11—C12	118.13
Zn3—O2—C1	82.49	C11—C12—C13	120.03
Zn4—O3—C3	95.48	N1—C13—C12	122.42
Zn4—O4—C3	88.54	N2—C14—C15	122.7
Zn3—O5—C5	115.97	C14—C15—C16	119.42
Zn4—O6—C5	138.98	C15—C16—C17	118.54
Zn3—O7—C7	137.91	C16—C17—C18	117.98
Zn4^ii—O8—C7	111.26	N2—C18—C17	123.84
O2—Zn3—O1—C1	4.85	O3—Zn4—N2—C14	−20.96
O5—Zn3—O1—C1	−58.42	O4—Zn4—N2—C14	−2.32
O7—Zn3—O1—C1	88.69	O6—Zn4—N2—C14	−141.39
N1—Zn3—O1—C1	−169.92	O8^i—Zn4—N2—C14	119.23
O1—Zn3—O2—C1	−4.85	O3—Zn4—N2—C18	158.21
O5—Zn3—O2—C1	133.15	O4—Zn4—N2—C18	176.86
O7—Zn3—O2—C1	−124.35	O6—Zn4—N2—C18	37.78
N1—Zn3—O2—C1	5.91	O8^i—Zn4—N2—C18	−61.60
O7—Zn3—N1—C13	83.43	Zn3—O1—C1—O2	−9.13
O1—Zn3—O7—C7	−26.17	Zn3—O1—C1—C2	168.83
O2—Zn3—O7—C7	32.23	Zn3—O2—C1—O1	7.58
O5—Zn3—O7—C7	129.42	Zn3—O2—C1—C2	−170.25
N1—Zn3—O7—C7	−125.76	Zn4—O3—C3—O4	8.71
O7—Zn3—N1—C9	−100.20	Zn4—O3—C3—C4	−170.51
O1—Zn3—N1—C13	−38.63	Zn4—O4—C3—O3	−8.16
O2—Zn3—N1—C13	−47.67	Zn4—O4—C3—C4	171.07
O1—Zn3—O5—C5	−26.62	Zn3—O5—C5—O6	−2.91
O2—Zn3—O5—C5	−75.34	Zn3—O5—C5—C6	177.96
O7—Zn3—O5—C5	−178.29	Zn4—O6—C5—O5	178.57
N1—Zn3—O5—C5	81.22	Zn4—O6—C5—C6	−2.34
O5—Zn3—N1—C9	3.21	Zn3—O7—C7—O8	−172.66
O1—Zn3—N1—C9	137.75	Zn3—O7—C7—C8	9.19
O5—Zn3—N1—C13	−173.17	Zn4^ii—O8—C7—O7	−5.68
O2—Zn3—N1—C9	128.71	Zn4^ii—O8—C7—C8	172.5
N2—Zn4—O4—C3	−17.29	Zn3—N1—C9—C10	−177.13
O6—Zn4—O3—C3	−96.56	C13—N1—C9—C10	−0.72
O8^i—Zn4—O4—C3	−139.24	Zn3—N1—C13—C12	176.57
O6—Zn4—O4—C3	119.89	C9—N1—C13—C12	−0.05
O3^ii—Zn4^ii—O8—C7	30.17	C18—N2—C14—C15	−0.71
O4^ii—Zn4^ii—O8—C7	78.01	Zn4—N2—C14—C15	178.49
O6^ii—Zn4^ii—O8—C7	−174.01	C14—N2—C18—C17	0.72
N2^ii—Zn4^ii—O8—C7	−76.49	Zn4—N2—C18—C17	−178.47
N2—Zn4—O3—C3	164.02	N1—C9—C10—C11	1.26
O8^i—Zn4—O3—C3	55.64	C9—C10—C11—C12	−0.99
O3—Zn4—O4—C3	4.91	C10—C11—C12—C13	0.26
O3—Zn4—O6—C5	35.3	C11—C12—C13—N1	0.27
O4—Zn4—O6—C5	−26.32	N2—C14—C15—C16	0.87
N2—Zn4—O6—C5	133.65	C14—C15—C16—C17	−0.95
O8^i—Zn4—O6—C5	−126.39	C15—C16—C17—C18	0.94
O4—Zn4—O3—C3	−5.03	C16—C17—C18—N2	−0.84

Symmetry codes: (i) x, y, z−1; (ii) x, y, z+1; (iii) x−1, y, z; (iv) x−1, y, z−1; (v) x−1/2, −y+1/2, z−1/2; (vi) x+1, y, z; (vii) x+1, y, z+1; (viii) x+1/2, −y+1/2, z+1/2.

(11) bis(Pyridine)-tetra-aqua-iron(ii) diacetate

Crystal data

C10H18FeN2O4·2(C2H3O2)	γ = 90°
Mr = 404.20	V = 934.5 (3) Å^3
Monclinic, I2/m	Z = 2
Hall symbol: -I 2y	F(000) = 376
a = 11.780 (2) Å	Dx = 1.350 Mg m^−3
b = 9.734 (2) Å	Mo K\a radiation, λ = 0.71070 Å
c = 8.401 (2) Å	µ = 0.85 mm^−1
α = 90°	T = 0 K
β = 104.05 (2)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0	0	1	0.02*
O1	−0.12083	0.15453	0.89028	0.02*
N1	0.0866	0	0.7939	0.02*
C1	0.1102	0.11555	0.72515	0.02*
C2	0.15573	0.12008	0.58847	0.02*
C3	0.1778	0	0.5195	0.02*
O3	0.35263	0.11323	0.19853	0.02*
C6	0.401	0	0.22	0.02*
C7	0.53195	0	0.27875	0.02*

Geometric parameters (Å, º)

Fe1—O1	2.1216	N1—C1	1.3244
Fe1—N1	2.2127 (5)	C1—C2	1.381
Fe1—N1^i	2.2127 (5)	C2—C3	1.3575
O3—C6	1.2337	C6—C7	1.5012 (4)
O1···O3^ii	2.6805	C2···C1^ii	3.5707
O1···O3^iii	2.7493	C3···C7^v	3.4278 (8)
O3···O1^ii	2.6805	C3···C7^vi	3.4278 (8)
O3···O1^iv	2.7493	C7···C3^vi	3.4278 (8)
C1···C2^ii	3.5707	C7···C3^v	3.4278 (8)
O1—Fe1—N1	92.76	O1^vii—Fe1—N1^i	92.76
O1—Fe1—O1^i	89.69	O1^viii—Fe1—N1^i	87.24
O1—Fe1—N1^i	87.24	O1^vii—Fe1—O1^viii	89.69
O1—Fe1—O1^vii	180	Fe1—N1—C1	121.78
O1—Fe1—O1^viii	90.31	Fe1—N1—C1^viii	121.78
O1^i—Fe1—N1	87.24	C1—N1—C1^viii	116.27
N1—Fe1—N1^i	180	N1—C1—C2	123.69
O1^vii—Fe1—N1	87.24	C1—C2—C3	118.73
O1^viii—Fe1—N1	92.76	C2—C3—C2^viii	118.87
O1^i—Fe1—N1^i	92.76	O3—C6—C7	116.7
O1^i—Fe1—O1^vii	90.31	O3—C6—O3^viii	126.6
O1^i—Fe1—O1^viii	180	O3^viii—C6—C7	116.7
O1—Fe1—N1—C1	42.37	Fe1—N1—C1—C2	−174.78
O1—Fe1—N1—C1^viii	−132.81	C1^viii—N1—C1—C2	0.65
O1^i—Fe1—N1—C1	−47.19	N1—C1—C2—C3	0.07
O1^vii—Fe1—N1—C1	−137.63	C1—C2—C3—C2^viii	−0.81
O1^viii—Fe1—N1—C1	132.81

Symmetry codes: (i) −x, y, −z+2; (ii) −x, y, −z+1; (iii) x−1/2, −y+1/2, z+1/2; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+1, −y, −z+1; (vi) −x+1, y, −z+1; (vii) −x, −y, −z+2; (viii) x, −y, z.

(12) trans-(1,4,8,11-Tetra-azacyclotetradecane)-dioxo-rhenium hexafluorophosphate

Crystal data

F6P·C10H24N4O2Re	γ = 90°
Mr = 563.49	V = 1706.4 (6) Å^3
Monclinic, I2/a	Z = 4
Hall symbol: -I 2ya	F(000) = 992
a = 17.257 (4) Å	Dx = 2.099 Mg m^−3
b = 5.533 (1) Å	Mo Kα radiation, λ = 0.71070 Å
c = 18.053 (4) Å	µ = 7.29 mm^−1
α = 90°	T = 293 K
β = 98.14 (2)°	× × mm

Data collection

Radiation source: fine-focus sealed tube	θmax = 30.1°, θmin = 2.3°
4752 measured reflections	h = −15→24
2500 independent reflections	k = −7→7
2150 reflections with I > 2σ(I)	l = −25→16
Rint = 0.121

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.077	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.192	w = 1/[σ^2(Fo^2) + (0.069P)^2 + 29.4858P] where P = (Fo^2 + 2Fc^2)/3
S = 1.32	(Δ/σ)max = 0.001
2500 reflections	Δρmax = 5.90 e Å^−3
129 parameters	Δρmin = −4.02 e Å^−3
1 restraint	Extinction correction: nne
Primary atom site location: structure-invariant direct methods

Special details

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 nt 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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Re1	0.0000	0.0000	0.0000	0.0191 (2)
O1	0.0620 (4)	0.2448 (13)	−0.0085 (4)	0.0287 (13)
N1	0.0946 (4)	−0.2413 (17)	−0.0057 (4)	0.0274 (15)
N2	−0.0417 (6)	0.0197 (14)	−0.1171 (5)	0.0274 (18)
C1	0.1374 (6)	−0.1928 (19)	−0.0719 (5)	0.0318 (19)
C2	0.0795 (7)	−0.203 (2)	−0.1450 (6)	0.041 (2)
C3	0.0263 (9)	0.022 (2)	−0.1628 (7)	0.038 (3)
C4	−0.0954 (6)	0.2315 (19)	−0.1296 (5)	0.034 (2)
C5	0.1472 (5)	−0.231 (2)	0.0680 (6)	0.036 (2)
P1	0.2500	0.2500	0.2500	0.0358 (8)
F1	0.268 (6)	0.20 (3)	0.165 (5)	0.080*	0.16 (4)
F2	0.314 (7)	0.39 (2)	0.203 (5)	0.080*	0.14 (4)
F3	0.222 (3)	0.044 (10)	0.302 (3)	0.080*	0.37 (5)
F4	0.162 (2)	0.290 (6)	0.210 (4)	0.080*	0.56 (8)
F5	0.238 (2)	0.525 (7)	0.279 (3)	0.080*	0.37 (4)
F6	0.183 (5)	0.270 (13)	0.179 (5)	0.080*	0.19 (4)
F7	0.152 (3)	0.248 (12)	0.233 (5)	0.080*	0.30 (10)
F8	0.224 (6)	0.16 (3)	0.330 (6)	0.080*	0.16 (4)
F9	0.229 (10)	0.27 (2)	0.161 (6)	0.080*	0.11 (3)
F10	0.2610 (17)	0.058 (9)	0.185 (2)	0.080*	0.44 (4)
F11	0.240 (4)	−0.051 (14)	0.263 (4)	0.080*	0.22 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re1	0.0219 (3)	0.0163 (3)	0.0181 (3)	−0.00234 (13)	−0.00104 (15)	−0.00013 (13)
O1	0.035 (3)	0.019 (3)	0.032 (3)	−0.007 (3)	0.003 (2)	0.005 (3)
N1	0.025 (3)	0.025 (4)	0.031 (3)	0.006 (3)	0.004 (3)	0.002 (3)
N2	0.036 (4)	0.028 (5)	0.016 (3)	−0.003 (3)	−0.002 (3)	0.000 (3)
C1	0.038 (5)	0.030 (5)	0.031 (4)	−0.001 (4)	0.016 (4)	−0.006 (4)
C2	0.049 (6)	0.040 (6)	0.036 (5)	0.001 (5)	0.010 (4)	−0.010 (5)
C3	0.059 (7)	0.032 (6)	0.024 (4)	−0.007 (4)	0.011 (4)	−0.007 (4)
C4	0.037 (4)	0.027 (5)	0.034 (4)	0.006 (4)	−0.009 (4)	0.010 (4)
C5	0.030 (4)	0.034 (5)	0.039 (5)	0.005 (4)	−0.015 (4)	−0.003 (4)
P1	0.0372 (17)	0.0275 (18)	0.0380 (17)	0.0000 (15)	−0.0104 (14)	−0.0010 (15)

Geometric parameters (Å, º)

Re1—O1^i	1.746 (7)	F2—F7^ii	1.43 (13)
Re1—O1	1.746 (7)	F2—F11^ii	1.50 (14)
Re1—N1^i	2.123 (8)	F2—F9	1.68 (18)
Re1—N1	2.123 (8)	F3—F2^ii	0.73 (10)
Re1—N2	2.136 (8)	F3—F8	0.80 (12)
Re1—N2^i	2.136 (8)	F3—F11	0.96 (8)
N1—C5	1.501 (11)	F3—F9^ii	1.42 (14)
N1—C1	1.515 (12)	F3—F1^ii	1.52 (13)
N2—C4	1.492 (13)	F3—F5^ii	1.73 (8)
N2—C3	1.528 (17)	F4—F7	0.52 (6)
C1—C2	1.540 (15)	F4—F6	0.73 (9)
C2—C3	1.552 (18)	F4—F9	1.56 (16)
C4—C5^i	1.522 (16)	F5—F10^ii	0.79 (5)
C5—C4^i	1.522 (16)	F5—F11^ii	0.89 (7)
P1—F3^ii	1.59 (4)	F5—F1^ii	1.63 (14)
P1—F3	1.59 (4)	F5—F3^ii	1.73 (8)
P1—F4	1.60 (2)	F6—F9	0.89 (14)
P1—F4^ii	1.60 (3)	F6—F7	1.19 (12)
P1—F6^ii	1.60 (6)	F6—F8^ii	1.68 (13)
P1—F6	1.60 (6)	F6—F10	1.77 (10)
P1—F9^ii	1.60 (10)	F7—F2^ii	1.43 (13)
P1—F9	1.60 (10)	F8—F1^ii	0.80 (13)
P1—F10^ii	1.61 (4)	F8—F2^ii	0.85 (13)
P1—F10	1.61 (4)	F8—F9^ii	0.90 (16)
P1—F1^ii	1.62 (8)	F8—F10^ii	1.64 (14)
P1—F1	1.62 (8)	F8—F6^ii	1.68 (13)
F1—F9	0.77 (14)	F8—F11	1.71 (15)
F1—F8^ii	0.80 (13)	F9—F8^ii	0.90 (16)
F1—F10	0.89 (13)	F9—F10	1.37 (14)
F1—F2	1.41 (17)	F9—F3^ii	1.42 (14)
F1—F3^ii	1.52 (13)	F10—F5^ii	0.79 (5)
F1—F6	1.55 (14)	F10—F11	1.61 (8)
F1—F5^ii	1.63 (14)	F10—F8^ii	1.64 (14)
F2—F3^ii	0.73 (10)	F11—F5^ii	0.89 (7)
F2—F8^ii	0.85 (13)	F11—F2^ii	1.50 (14)
O1^i—Re1—O1	180.0 (6)	F11—F3—F1^ii	139 (7)
O1^i—Re1—N1^i	89.9 (4)	F9^ii—F3—F1^ii	30 (5)
O1—Re1—N1^i	90.1 (4)	F2^ii—F3—P1	83 (8)
O1^i—Re1—N1	90.1 (4)	F8—F3—P1	80 (7)
O1—Re1—N1	89.9 (4)	F11—F3—P1	79 (6)
N1^i—Re1—N1	180.0 (5)	F9^ii—F3—P1	64 (5)
O1^i—Re1—N2	90.1 (3)	F1^ii—F3—P1	63 (4)
O1—Re1—N2	89.9 (3)	F2^ii—F3—F5^ii	117 (10)
N1^i—Re1—N2	82.1 (3)	F8—F3—F5^ii	136 (8)
N1—Re1—N2	97.9 (3)	F11—F3—F5^ii	20 (5)
O1^i—Re1—N2^i	89.9 (3)	F9^ii—F3—F5^ii	106 (7)
O1—Re1—N2^i	90.1 (3)	F1^ii—F3—F5^ii	119 (5)
N1^i—Re1—N2^i	97.9 (3)	P1—F3—F5^ii	59 (2)
N1—Re1—N2^i	82.1 (3)	F7—F4—F6	144 (10)
N2—Re1—N2^i	180.0 (6)	F7—F4—F9	141 (9)
C5—N1—C1	113.0 (7)	F6—F4—F9	18 (7)
C5—N1—Re1	107.8 (6)	F7—F4—P1	89 (7)
C1—N1—Re1	113.0 (6)	F6—F4—P1	77 (6)
C4—N2—C3	114.8 (8)	F9—F4—P1	61 (5)
C4—N2—Re1	107.8 (6)	F10^ii—F5—F11^ii	145 (8)
C3—N2—Re1	111.0 (7)	F10^ii—F5—P1	75 (4)
N1—C1—C2	109.9 (8)	F11^ii—F5—P1	78 (6)
C1—C2—C3	116.2 (9)	F10^ii—F5—F1^ii	16 (5)
N2—C3—C2	110.9 (9)	F11^ii—F5—F1^ii	136 (7)
N2—C4—C5^i	107.8 (8)	P1—F5—F1^ii	60 (4)
N1—C5—C4^i	107.7 (7)	F10^ii—F5—F3^ii	127 (5)
F3^ii—P1—F3	180 (4)	F11^ii—F5—F3^ii	22 (6)
F3^ii—P1—F4	89 (3)	P1—F5—F3^ii	57 (2)
F3—P1—F4	91 (3)	F1^ii—F5—F3^ii	115 (4)
F3^ii—P1—F4^ii	91 (3)	F4—F6—F9	148 (10)
F3—P1—F4^ii	89 (3)	F4—F6—F7	15 (5)
F4—P1—F4^ii	180 (4)	F9—F6—F7	146 (10)
F3^ii—P1—F6^ii	106 (4)	F4—F6—F1	138 (8)
F3—P1—F6^ii	74 (4)	F9—F6—F1	19 (10)
F4—P1—F6^ii	154 (3)	F7—F6—F1	130 (6)
F4^ii—P1—F6^ii	26 (3)	F4—F6—P1	77 (6)
F3^ii—P1—F6	74 (4)	F9—F6—P1	74 (8)
F3—P1—F6	106 (4)	F7—F6—P1	72 (4)
F4—P1—F6	26 (3)	F1—F6—P1	62 (4)
F4^ii—P1—F6	154 (3)	F4—F6—F8^ii	129 (9)
F6^ii—P1—F6	180.000 (11)	F9—F6—F8^ii	20 (9)
F3^ii—P1—F9^ii	127 (5)	F7—F6—F8^ii	131 (6)
F3—P1—F9^ii	53 (5)	F1—F6—F8^ii	28 (5)
F4—P1—F9^ii	122 (6)	P1—F6—F8^ii	61 (4)
F4^ii—P1—F9^ii	58 (6)	F4—F6—F10	120 (8)
F6^ii—P1—F9^ii	32 (5)	F9—F6—F10	49 (10)
F6—P1—F9^ii	148 (5)	F7—F6—F10	108 (5)
F3^ii—P1—F9	53 (5)	F1—F6—F10	30 (5)
F3—P1—F9	127 (5)	P1—F6—F10	57 (3)
F4—P1—F9	58 (6)	F8^ii—F6—F10	57 (5)
F4^ii—P1—F9	122 (6)	F4—F7—F6	21 (7)
F6^ii—P1—F9	148 (5)	F4—F7—F2^ii	137 (9)
F6—P1—F9	32 (5)	F6—F7—F2^ii	123 (6)
F9^ii—P1—F9	180.000 (12)	F4—F7—P1	73 (7)
F3^ii—P1—F10^ii	92 (3)	F6—F7—P1	65 (4)
F3—P1—F10^ii	88 (3)	F2^ii—F7—P1	64 (5)
F4—P1—F10^ii	92 (2)	F3—F8—F1^ii	145 (10)
F4^ii—P1—F10^ii	88 (2)	F3—F8—F2^ii	52 (10)
F6^ii—P1—F10^ii	67 (4)	F1^ii—F8—F2^ii	117 (10)
F6—P1—F10^ii	113 (4)	F3—F8—F9^ii	114 (10)
F9^ii—P1—F10^ii	50 (5)	F1^ii—F8—F9^ii	54 (10)
F9—P1—F10^ii	130 (5)	F2^ii—F8—F9^ii	147 (10)
F3^ii—P1—F10	88 (3)	F3—F8—F10^ii	129 (9)
F3—P1—F10	92 (3)	F1^ii—F8—F10^ii	16 (8)
F4—P1—F10	88 (2)	F2^ii—F8—F10^ii	106 (10)
F4^ii—P1—F10	92 (2)	F9^ii—F8—F10^ii	56 (10)
F6^ii—P1—F10	113 (4)	F3—F8—P1	71 (7)
F6—P1—F10	67 (4)	F1^ii—F8—P1	73 (9)
F9^ii—P1—F10	130 (5)	F2^ii—F8—P1	76 (9)
F9—P1—F10	50 (5)	F9^ii—F8—P1	71 (9)
F10^ii—P1—F10	180 (2)	F10^ii—F8—P1	59 (3)
F3^ii—P1—F1^ii	123 (5)	F3—F8—F6^ii	95 (9)
F3—P1—F1^ii	57 (5)	F1^ii—F8—F6^ii	67 (10)
F4—P1—F1^ii	96 (4)	F2^ii—F8—F6^ii	131 (10)
F4^ii—P1—F1^ii	84 (4)	F9^ii—F8—F6^ii	20 (9)
F6^ii—P1—F1^ii	58 (5)	F10^ii—F8—F6^ii	65 (5)
F6—P1—F1^ii	122 (5)	P1—F8—F6^ii	57 (4)
F9^ii—P1—F1^ii	28 (5)	F3—F8—F11	14 (6)
F9—P1—F1^ii	152 (5)	F1^ii—F8—F11	133 (10)
F10^ii—P1—F1^ii	32 (5)	F2^ii—F8—F11	61 (10)
F10—P1—F1^ii	148 (5)	F9^ii—F8—F11	101 (10)
F3^ii—P1—F1	57 (5)	F10^ii—F8—F11	119 (5)
F3—P1—F1	123 (5)	P1—F8—F11	60 (4)
F4—P1—F1	84 (4)	F6^ii—F8—F11	81 (6)
F4^ii—P1—F1	96 (4)	F1—F9—F6	138 (10)
F6^ii—P1—F1	122 (5)	F1—F9—F8^ii	57 (10)
F6—P1—F1	58 (5)	F6—F9—F8^ii	140 (10)
F9^ii—P1—F1	152 (5)	F1—F9—F10	38 (10)
F9—P1—F1	28 (5)	F6—F9—F10	101 (10)
F10^ii—P1—F1	148 (5)	F8^ii—F9—F10	91 (10)
F10—P1—F1	32 (5)	F1—F9—F3^ii	82 (10)
F1^ii—P1—F1	180.0 (15)	F6—F9—F3^ii	110 (10)
F9—F1—F8^ii	70 (10)	F8^ii—F9—F3^ii	31 (9)
F9—F1—F10	110 (10)	F10—F9—F3^ii	106 (10)
F8^ii—F1—F10	151 (10)	F1—F9—F4	132 (10)
F9—F1—F2	96 (10)	F6—F9—F4	14 (6)
F8^ii—F1—F2	33 (9)	F8^ii—F9—F4	127 (10)
F10—F1—F2	124 (10)	F10—F9—F4	99 (8)
F9—F1—F3^ii	68 (10)	F3^ii—F9—F4	97 (7)
F8^ii—F1—F3^ii	18 (8)	F1—F9—P1	77 (10)
F10—F1—F3^ii	133 (8)	F6—F9—P1	74 (8)
F2—F1—F3^ii	28 (5)	F8^ii—F9—P1	77 (9)
F9—F1—F6	23 (10)	F10—F9—P1	65 (5)
F8^ii—F1—F6	85 (10)	F3^ii—F9—P1	63 (5)
F10—F1—F6	89 (8)	F4—F9—P1	61 (4)
F2—F1—F6	104 (9)	F1—F9—F2	57 (10)
F3^ii—F1—F6	77 (6)	F6—F9—F2	127 (10)
F9—F1—P1	75 (10)	F8^ii—F9—F2	16 (7)
F8^ii—F1—P1	78 (10)	F10—F9—F2	84 (9)
F10—F1—P1	73 (6)	F3^ii—F9—F2	26 (4)
F2—F1—P1	66 (5)	F4—F9—F2	113 (7)
F3^ii—F1—P1	61 (4)	P1—F9—F2	61 (5)
F6—F1—P1	61 (4)	F5^ii—F10—F1	149 (9)
F9—F1—F5^ii	109 (10)	F5^ii—F10—F9	137 (8)
F8^ii—F1—F5^ii	136 (10)	F1—F10—F9	32 (8)
F10—F1—F5^ii	15 (4)	F5^ii—F10—F11	18 (4)
F2—F1—F5^ii	110 (7)	F1—F10—F11	138 (7)
F3^ii—F1—F5^ii	119 (5)	F9—F10—F11	119 (7)
F6—F1—F5^ii	87 (6)	F5^ii—F10—P1	77 (4)
P1—F1—F5^ii	60 (4)	F1—F10—P1	74 (7)
F3^ii—F2—F8^ii	60 (10)	F9—F10—P1	65 (5)
F3^ii—F2—F1	85 (10)	F11—F10—P1	63 (3)
F8^ii—F2—F1	30 (10)	F5^ii—F10—F8^ii	135 (7)
F3^ii—F2—F7^ii	128 (10)	F1—F10—F8^ii	14 (7)
F8^ii—F2—F7^ii	127 (10)	F9—F10—F8^ii	33 (6)
F1—F2—F7^ii	99 (8)	F11—F10—F8^ii	125 (5)
F3^ii—F2—F11^ii	32 (8)	P1—F10—F8^ii	61 (4)
F8^ii—F2—F11^ii	89 (10)	F5^ii—F10—F6	111 (6)
F1—F2—F11^ii	107 (9)	F1—F10—F6	61 (7)
F7^ii—F2—F11^ii	101 (6)	F9—F10—F6	30 (6)
F3^ii—F2—P1	71 (8)	F11—F10—F6	93 (4)
F8^ii—F2—P1	74 (9)	P1—F10—F6	56 (3)
F1—F2—P1	63 (5)	F8^ii—F10—F6	59 (4)
F7^ii—F2—P1	65 (5)	F5^ii—F11—F3	138 (10)
F11^ii—F2—P1	64 (5)	F5^ii—F11—F2^ii	127 (8)
F3^ii—F2—F9	57 (10)	F3—F11—F2^ii	24 (5)
F8^ii—F2—F9	17 (8)	F5^ii—F11—F10	16 (4)
F1—F2—F9	27 (5)	F3—F11—F10	125 (7)
F7^ii—F2—F9	114 (7)	F2^ii—F11—F10	111 (6)
F11^ii—F2—F9	81 (8)	F5^ii—F11—P1	71 (6)
P1—F2—F9	57 (5)	F3—F11—P1	67 (5)
F2^ii—F3—F8	68 (9)	F2^ii—F11—P1	63 (4)
F2^ii—F3—F11	125 (10)	F10—F11—P1	58 (3)
F8—F3—F11	154 (10)	F5^ii—F11—F8	128 (8)
F2^ii—F3—F9^ii	97 (10)	F3—F11—F8	12 (5)
F8—F3—F9^ii	35 (9)	F2^ii—F11—F8	30 (4)
F11—F3—F9^ii	120 (9)	F10—F11—F8	117 (5)
F2^ii—F3—F1^ii	67 (10)	P1—F11—F8	58 (4)
F8—F3—F1^ii	18 (8)

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

(13) bis(mu!4$-N,N-Diethylcarbamato-O,O',O'',O''')-tetrakis(mu!3$-N,N-diethylcarba- mato-O,O',O'')-hexakis(mu!2$-N,N-diethylcarbamato-O,O')-hexa-iron

Crystal data

C60H120Fe6N12O24	Z = 4
Mr = 1728.78	F(000) = 3168
Orthorhombic, Ccca	Dx = 1.259 Mg m^−3
Hall symbol: -C 2b 2bc	Mo K\a radiation, λ = 0.71073 Å
a = 20.939 (2) Å	µ = 1.07 mm^−1
b = 25.243 (4) Å	T = 0 K
c = 16.048 (1) Å	× × mm
V = 8482.4 (17) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.13156	0.20392	0.32463	0.02*
Fe3	0	0.16095	0.25	0.02*
O1	0.223	0.21055	0.28235	0.02*
O3	0.12755	0.1322	0.3766	0.02*
O4	0.1412	0.27105	0.39045	0.02*
O7	0.0987	0.17740	0.20855	0.02*
O9	0.02975	0.2134	0.34335	0.02*
O10	0.03490	0.10065	0.3225	0.02*
N1	0.09530	0.04935	0.4043	0.02*
N2	0.1485	0.35895	0.4016	0.02*
N3	0	0.25	0.4663	0.02*
N6	0.3149	0.25	0.25	0.02*
C1	0.0855	0.09645	0.36540	0.02*
C2	0.04775	0.00445	0.3956	0.02*
C3	0.0694	−0.02960	0.3245	0.02*
C4	0.15315	0.04035	0.4533	0.02*
C5	0.1394	0.05275	0.542	0.02*
C6	0.12945	0.316	0.36135	0.02*
C7	0.1854	0.3527	0.4801	0.02*
C8	0.1381	0.4124	0.37035	0.02*
C9	0.19365	0.4314	0.3148	0.02*
C10	0.25335	0.3314	0.466	0.02*
C11	0	0.25	0.3825	0.02*
C12	0.03335	0.20945	0.51325	0.02*
C13	−0.00605	0.16165	0.53225	0.02*
C26	0.2503	0.25	0.25	0.02*
C27	0.35015	0.2089	0.29265	0.02*
C28	0.36645	0.1639	0.2335	0.02*

Geometric parameters (Å, º)

Fe1—O1	2.0382	N1—C2	1.5151
Fe1—O3	1.9951	N1—C4	1.4619
Fe1—O4	2.007	N2—C6	1.3236
Fe1—O7	2.0957	N2—C7	1.4862
Fe1—O9	2.1661	N2—C8	1.4558
Fe3—O7	2.2104	N3—C11	1.3448 (2)
Fe3—O9	2.0941	N3—C12	1.4502
Fe3—O10	2.0505	N6—C26	1.3527 (2)
O1—C26	1.2601	N6—C27	1.4456
O3—C1	1.2736	C2—C3	1.4987
O4—C6	1.2514	C4—C5	1.4856
O7—C6^i	1.3041	C7—C10	1.5377
O9—C11	1.2792	C8—C9	1.542
O10—C1	1.268	C12—C13	1.4932
N1—C1	1.3585	C27—C28	1.5192
Fe1···C12	3.6621	C3···O10	3.3665
Fe1···Fe1^i	3.3391	C5···O3	3.3361
Fe3···C8^ii	3.9396	C6···C11	3.1997
Fe3···C8^i	3.9396	C6···C26	3.5174
O1···C28	3.3202	C8···Fe3^ii	3.9396
O3···C5	3.3361	C8···Fe3^ii	3.9396
O4···N3	3.2412	C9···O7^i	3.4112
O4···C10	3.0505	C10···O4	3.0505
O4···C12	3.3766	C11···C6	3.1997
O7···O9^i	3.2213	C11···C6^ii	3.1997
O7···C9^i	3.4112	C12···Fe1	3.6621
O9···C13	3.385	C12···O4	3.3766
O9···O7^i	3.2213	C13···O9	3.385
O10···C3	3.3665	C26···C6	3.5174
N3···O4	3.2412	C26···C6^i	3.5174
N3···O4^ii	3.2412	C28···O1	3.3202
O1—Fe1—O3	104.67	Fe3—O9—C11	131.54
O1—Fe1—O4	90.65	Fe3—O10—C1	131.91
O1—Fe1—O7	92.22	C1—N1—C2	120.87
O1—Fe1—O9	164.07	C1—N1—C4	120.55
O3—Fe1—O4	123.4	C2—N1—C4	118.54
O3—Fe1—O7	93.89	C6—N2—C7	118.91
O3—Fe1—O9	90.05	C6—N2—C8	123.09
O4—Fe1—O7	140.41	C7—N2—C8	117.91
O4—Fe1—O9	86.14	C11—N3—C12	121.3
O7—Fe1—O9	80.53	C11—N3—C12^ii	121.3
O7—Fe3—O9	79.54	C12—N3—C12^ii	117.4
O7—Fe3—O10	88.68	C26—N6—C27	120.7
O7—Fe3—O7^iii	158.34	C26—N6—C27^i	120.7
O7—Fe3—O9^iii	86.79	C27—N6—C27^i	118.59
O7—Fe3—O10^iii	107.57	O3—C1—O10	126.52
O9—Fe3—O10	87.56	O3—C1—N1	116.8
O7^iii—Fe3—O9	86.79	O10—C1—N1	116.67
O9—Fe3—O9^iii	101.57	N1—C2—C3	107.48
O9—Fe3—O10^iii	168.89	N1—C4—C5	108.79
O7^iii—Fe3—O10	107.57	O4—C6—N2	120.09
O9^iii—Fe3—O10	168.89	O4—C6—O7^i	122.27
O10—Fe3—O10^iii	84.14	O7^i—C6—N2	117.64
O7^iii—Fe3—O9^iii	79.54	N2—C7—C10	113.17
O7^iii—Fe3—O10^iii	88.68	N2—C8—C9	112
O9^iii—Fe3—O10^iii	87.56	O9—C11—N3	119.42
Fe1—O1—C26	128.91	O9—C11—O9^ii	121.17
Fe1—O3—C1	127.82	O9^ii—C11—N3	119.42
Fe1—O4—C6	123.32	N3—C12—C13	114.23
Fe1—O7—Fe3	95.71	O1—C26—N6	116.98
Fe1—O7—C6^i	124.17	O1—C26—O1^i	126.05
Fe3—O7—C6^i	138.11	O1^i—C26—N6	116.98
Fe1—O9—Fe3	97.11	N6—C27—C28	110.83
Fe1—O9—C11	128.84
O3—Fe1—O1—C26	−174.59	O7^iii—Fe3—O10—C1	−127.50
O4—Fe1—O1—C26	−49.70	O10^iii—Fe3—O10—C1	145.75
O7—Fe1—O1—C26	90.8	Fe1—O1—C26—O1^i	−19.30
O1—Fe1—O3—C1	−131.40	Fe1—O1—C26—N6	160.7
O4—Fe1—O3—C1	127.84	Fe1—O3—C1—N1	176.13
O7—Fe1—O3—C1	−38.08	Fe1—O3—C1—O10	−4.95
O9—Fe1—O3—C1	42.43	Fe1—O4—C6—N2	−166.62
O1—Fe1—O4—C6	88.61	Fe1—O4—C6—O7^i	13.22
O3—Fe1—O4—C6	−163.28	Fe1^i—O7^i—C6—N2	117.28
O7—Fe1—O4—C6	−5.67	Fe1^i—O7^i—C6—O4	−62.56
O9—Fe1—O4—C6	−75.77	Fe3—O9—C11—N3	126.7
O1—Fe1—O7—Fe3	174.7	Fe1—O9—C11—N3	−75.55
O1—Fe1—O7—C6^i	−18.84	Fe3—O9—C11—O9^ii	−53.30
O3—Fe1—O7—Fe3	69.83	Fe1—O9—C11—O9^ii	104.45
O3—Fe1—O7—C6^i	−123.71	Fe3—O10—C1—O3	3.48
O4—Fe1—O7—Fe3	−91.59	Fe3—O10—C1—N1	−177.59
O4—Fe1—O7—C6^i	74.87	C1—N1—C2—C3	93.05
O9—Fe1—O7—Fe3	−19.57	C4—N1—C2—C3	−84.95
O9—Fe1—O7—C6^i	146.89	C4—N1—C1—O10	178.34
O3—Fe1—O9—Fe3	−73.17	C2—N1—C1—O10	0.38
O3—Fe1—O9—C11	123.43	C2—N1—C1—O3	179.42
O4—Fe1—O9—Fe3	163.35	C1—N1—C4—C5	94.43
O4—Fe1—O9—C11	−0.06	C4—N1—C1—O3	−2.62
O7—Fe1—O9—Fe3	20.77	C2—N1—C4—C5	−87.57
O7—Fe1—O9—C11	−142.64	C7—N2—C6—O7^i	−178.14
O9—Fe3—O7—Fe1	20.34	C7—N2—C6—O4	1.71
O9—Fe3—O7—C6^i	−142.79	C8—N2—C6—O4	178.23
O10—Fe3—O7—Fe1	−67.42	C6—N2—C8—C9	−89.66
O10—Fe3—O7—C6^i	129.45	C7—N2—C8—C9	86.89
O7^iii—Fe3—O7—Fe1	72.08	C8—N2—C7—C10	−106.27
O9^iii—Fe3—O7—Fe1	122.73	C6—N2—C7—C10	70.43
O10^iii—Fe3—O7—Fe1	−150.85	C8—N2—C6—O7^i	−1.62
O7—Fe3—O9—Fe1	−19.71	C12^ii—N3—C11—O9	−179.69
O7—Fe3—O9—C11	143	C12—N3—C11—O9	0.31
O10—Fe3—O9—Fe1	69.4	C12^ii—N3—C12—C13	90.66
O10—Fe3—O9—C11	−127.89	C12—N3—C11—O9^ii	−179.69
O7^iii—Fe3—O9—Fe1	177.16	C11—N3—C12—C13	−89.34
O7^iii—Fe3—O9—C11	−20.13	C27—N6—C26—O1	−5.88
O9^iii—Fe3—O9—Fe1	−104.21	C27^i—N6—C26—O1	174.12
O9^iii—Fe3—O9—C11	58.5	C27—N6—C26—O1^i	174.12
O7—Fe3—O10—C1	37.94	C26—N6—C27—C28	93.08
O9—Fe3—O10—C1	−41.64	C27^i—N6—C27—C28	−86.92

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

(14) bis(2,2'-bis(p-tolylphosphin)-1,1-binaphthyl)-palladium(0) benzene solvate

Crystal data

C96H80P4Pd·4(C6H6)	Z = 4
Mr = 1776.33	F(000) = 3304
Orthorhombic, C2221	Dx = 1.162 Mg m^−3
Hall symbol: C 2c 2	Mo K\a radiation, λ = 0.71073 Å
a = 29.327 (12) Å	µ = 0.31 mm^−1
b = 16.743 (7) Å	T = 0 K
c = 19.458 (6) Å	× × mm
V = 9554 (6) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text	Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0	0.26357	0.25	0.02*
P1	0.06025	0.1953	0.30795	0.02*
P2	0.05415	0.335	0.18055	0.02*
C1	0.08672	0.25043	0.37955	0.02*
C2	0.06225	0.31235	0.4078	0.02*
C3	0.07878	0.35642	0.4636	0.02*
C4	0.12003	0.33983	0.49265	0.02*
C5	0.14548	0.27772	0.46425	0.02*
C6	0.1294	0.2334	0.4082	0.02*
C7	0.1374	0.3865	0.55415	0.02*
C8	0.05257	0.09622	0.34795	0.02*
C9	0.01047	0.05807	0.34415	0.02*
C10	0.00405	−0.01695	0.37475	0.02*
C11	0.03985	−0.05500	0.4095	0.02*
C12	0.08078	−0.01708	0.41295	0.02*
C13	0.08748	0.05748	0.38315	0.02*
C14	0.03385	−0.13470	0.44435	0.02*
C15	0.10742	0.17003	0.248	0.02*
C16	0.10817	0.09153	0.22185	0.02*
C17	0.13795	0.06980	0.1715	0.02*
C18	0.17088	0.12427	0.14515	0.02*
C19	0.20207	0.10302	0.09175	0.02*
C20	0.23345	0.15585	0.06725	0.02*
C21	0.23485	0.2336	0.0963	0.02*
C22	0.20470	0.25530	0.1464	0.02*
C23	0.17133	0.20207	0.173	0.02*
C24	0.13925	0.2253	0.2248	0.02*
C25	0.13968	0.31042	0.24985	0.02*
C26	0.17623	0.33528	0.2917	0.02*
C27	0.21285	0.28395	0.31195	0.02*
C28	0.24745	0.3103	0.3533	0.02*
C29	0.2478	0.38935	0.37835	0.02*
C30	0.21295	0.44015	0.3611	0.02*
C31	0.17677	0.41532	0.31855	0.02*
C32	0.1406	0.46695	0.3007	0.02*
C33	0.10728	0.44228	0.2579	0.02*
C34	0.10547	0.36283	0.23135	0.02*
C35	0.07718	0.28223	0.1048	0.02*
C36	0.05673	0.21072	0.08665	0.02*
C37	0.07147	0.16602	0.03145	0.02*
C38	0.10647	0.19218	−0.00765	0.02*
C39	0.12797	0.26237	0.0093	0.02*
C40	0.1139	0.3064	0.0663	0.02*
C41	0.12292	0.14247	−0.06965	0.02*
C42	0.04040	0.43325	0.14215	0.02*
C43	−0.00062	0.46797	0.15890	0.02*
C44	−0.01143	0.54488	0.13675	0.02*
C45	0.01795	0.5886	0.09905	0.02*
C46	0.05743	0.55413	0.08175	0.02*
C47	0.06915	0.48005	0.1047	0.02*
C48	0.0076	0.6748	0.0784	0.02*
C97	0.38575	0.18825	0.2585	0.02*
C98	0.34575	0.21875	0.245	0.02*
C99	0.34425	0.28875	0.226	0.02*
C100	0.37925	0.33925	0.223	0.02*
C101	0.42025	0.31525	0.2357	0.02*
C102	0.4225	0.23	0.2545	0.02*
C103	0.26525	0.08575	0.4415	0.02*
C104	0.29750	0.0585	0.4105	0.02*
C105	0.293	0.019	0.35750	0.02*
C106	0.25225	0.00975	0.32750	0.02*
C107	0.22	0.036	0.3655	0.02*
C108	0.22775	0.07825	0.425	0.02*

Geometric parameters (Å, º)

Pd1—P1	2.3875	C26—C27	1.4308
Pd1—P2	2.4038	C26—C31	1.4384
P1—C1	1.8427	C27—C28	1.3681
P1—C8	1.8462	C28—C29	1.4105
P1—C15	1.8583	C29—C30	1.3714
P2—C34	1.8599	C30—C31	1.4086
P2—C35	1.8464	C31—C32	1.4118
P2—C42	1.8512	C32—C33	1.3487
C1—C2	1.3755	C33—C34	1.428
C1—C6	1.3996	C35—C36	1.3849
C2—C3	1.3994	C35—C40	1.3728
C3—C4	1.3639	C36—C37	1.3786
C4—C5	1.3942	C37—C38	1.3507
C4—C7	1.5173	C38—C39	1.3738
C5—C6	1.4009	C38—C41	1.543
C8—C9	1.3921	C39—C40	1.3942
C8—C13	1.3921	C42—C43	1.3753
C9—C10	1.4027	C42—C47	1.3623
C10—C11	1.4019	C43—C44	1.3944
C11—C12	1.3596	C44—C45	1.3477
C11—C14	1.5071	C45—C46	1.3368
C12—C13	1.3904	C45—C48	1.5286
C15—C16	1.4096	C46—C47	1.3623
C15—C24	1.3898	C97—C98	1.3061
C16—C17	1.362	C97—C102	1.287
C17—C18	1.4238	C98—C99	1.2297
C18—C19	1.4293	C99—C100	1.3311
C18—C23	1.4109	C100—C101	1.2916
C19—C20	1.3626	C101—C102	1.4749
C20—C21	1.4198	C103—C104	1.211
C21—C22	1.3653	C103—C108	1.1525
C22—C23	1.4212	C104—C105	1.2322
C23—C24	1.4326	C105—C106	1.339
C24—C25	1.5063	C106—C107	1.2784
C25—C26	1.409	C107—C108	1.3757
C25—C34	1.3806
C1···C25	3.1289	C25···C1	3.1289
C1···C26	3.4396	C25···C6	3.3537
C1···C34	3.4871	C26···C1	3.4396
C2···C43^i	3.4264	C26···C6	3.1519
C3···C48^ii	3.4177	C26···C22	3.2378
C5···C27	3.5632	C27···C5	3.5632
C6···C13	3.2287	C27···C6	3.1958
C6···C24	3.5828	C27···C22	3.2656
C6···C25	3.3537	C27···C23	3.2668
C6···C26	3.1519	C33···C47	3.246
C6···C27	3.1958	C33···C43^i	3.5483
C9···C36^i	3.497	C34···C1	3.4871
C12···C12^iii	3.4356	C35···C15	3.4756
C13···C6	3.2287	C35···C23	3.3446
C13···C16	3.2471	C35···C24	3.1103
C14···C37^iv	3.562	C36···C15	3.5399
C14···C48^v	3.4419	C36···C9^i	3.497
C15···C35	3.4756	C37···C14^vi	3.5619
C15···C36	3.5399	C39···C21	3.5948
C16···C13	3.2471	C39···C22	3.492
C21···C39	3.5948	C39···C23	3.5752
C22···C26	3.2378	C40···C22	3.2019
C22···C27	3.2656	C40···C23	3.1935
C22···C39	3.492	C40···C24	3.4508
C22···C40	3.2019	C40···C47	3.2762
C23···C27	3.2668	C43···C2^i	3.4264
C23···C35	3.3446	C43···C33^i	3.5483
C23···C39	3.5752	C43···C43^i	3.5454
C23···C40	3.1935	C47···C33	3.246
C24···C6	3.5828	C47···C40	3.2762
C24···C35	3.1103	C48···C3^vii	3.4177
C24···C40	3.4508	C48···C14^viii	3.4419
P1—Pd1—P2	90.85	C15—C24—C23	119.27
P1—Pd1—P1^i	122.79	C15—C24—C25	122.04
P1—Pd1—P2^i	117.49	C23—C24—C25	118.62
P1^i—Pd1—P2	117.49	C24—C25—C26	118.22
P2—Pd1—P2^i	120.33	C24—C25—C34	120.72
P1^i—Pd1—P2^i	90.85	C26—C25—C34	121.05
Pd1—P1—C1	115.41	C25—C26—C27	123.55
Pd1—P1—C8	122.62	C25—C26—C31	119.57
Pd1—P1—C15	111.31	C27—C26—C31	116.83
C1—P1—C8	100.53	C26—C27—C28	121.67
C1—P1—C15	105.96	C27—C28—C29	120.75
C8—P1—C15	98.68	C28—C29—C30	119.47
Pd1—P2—C34	111.13	C29—C30—C31	121.48
Pd1—P2—C35	116.89	C26—C31—C30	119.78
Pd1—P2—C42	121.68	C26—C31—C32	118.22
C34—P2—C35	104.37	C30—C31—C32	122
C34—P2—C42	99.68	C31—C32—C33	120.58
C35—P2—C42	100.53	C32—C33—C34	122.38
P1—C1—C2	117.38	P2—C34—C25	124.57
P1—C1—C6	125.16	P2—C34—C33	117.11
C2—C1—C6	117.45	C25—C34—C33	118.08
C1—C2—C3	121.79	P2—C35—C36	117.31
C2—C3—C4	121.43	P2—C35—C40	125.56
C3—C4—C5	117.55	C36—C35—C40	117.09
C3—C4—C7	121.32	C35—C36—C37	122.16
C5—C4—C7	121.13	C36—C37—C38	120.07
C4—C5—C6	121.56	C37—C38—C39	119.4
C1—C6—C5	120.21	C37—C38—C41	120.21
P1—C8—C9	119.87	C39—C38—C41	120.37
P1—C8—C13	122.44	C38—C39—C40	120.49
C9—C8—C13	117.69	C35—C40—C39	120.69
C8—C9—C10	120.49	P2—C42—C43	118.07
C9—C10—C11	120.74	P2—C42—C47	126.31
C10—C11—C12	118.22	C43—C42—C47	115.15
C10—C11—C14	122.14	C42—C43—C44	121.06
C12—C11—C14	119.63	C43—C44—C45	121.63
C11—C12—C13	121.56	C44—C45—C46	117.15
C8—C13—C12	121.3	C44—C45—C48	121.93
P1—C15—C16	116.78	C46—C45—C48	120.89
P1—C15—C24	123.52	C45—C46—C47	121.94
C16—C15—C24	119.55	C42—C47—C46	122.88
C15—C16—C17	121.25	C98—C97—C102	121.85
C16—C17—C18	121.52	C97—C98—C99	117.72
C17—C18—C19	122.44	C98—C99—C100	126.23
C17—C18—C23	117.35	C99—C100—C101	120.79
C19—C18—C23	120.2	C100—C101—C102	112.96
C18—C19—C20	121.67	C97—C102—C101	120.21
C19—C20—C21	118.39	C104—C103—C108	124.43
C20—C21—C22	120.63	C103—C104—C105	122.37
C21—C22—C23	122.62	C104—C105—C106	121.5
C18—C23—C22	116.46	C105—C106—C107	111.62
C18—C23—C24	120.98	C106—C107—C108	122.77
C22—C23—C24	122.56	C103—C108—C107	116.62
P2—Pd1—P1—C1	83.08	P1—C15—C16—C17	172.1
P1^i—Pd1—P1—C1	−152.96	C24—C15—C16—C17	−3.56
P2^i—Pd1—P1—C1	−42.16	C16—C15—C24—C25	178.91
P2—Pd1—P1—C8	−153.95	P1—C15—C24—C23	−173.33
P1^i—Pd1—P1—C8	−29.99	C15—C16—C17—C18	2.72
P2^i—Pd1—P1—C8	80.81	C16—C17—C18—C23	−0.36
P2—Pd1—P1—C15	−37.73	C16—C17—C18—C19	−179.21
P1^i—Pd1—P1—C15	86.24	C23—C18—C19—C20	1.34
P2^i—Pd1—P1—C15	−162.97	C19—C18—C23—C24	177.74
P1—Pd1—P2—C34	−37.97	C19—C18—C23—C22	−1.62
P1^i—Pd1—P2—C34	−166.16	C17—C18—C23—C22	179.5
P2^i—Pd1—P2—C34	84.95	C17—C18—C19—C20	−179.84
P1—Pd1—P2—C35	81.65	C17—C18—C23—C24	−1.14
P1^i—Pd1—P2—C35	−46.54	C18—C19—C20—C21	0.28
P2^i—Pd1—P2—C35	−155.43	C19—C20—C21—C22	−1.56
P1—Pd1—P2—C42	−154.73	C20—C21—C22—C23	1.25
P1^i—Pd1—P2—C42	77.08	C21—C22—C23—C24	−178.99
P2^i—Pd1—P2—C42	−31.81	C21—C22—C23—C18	0.36
Pd1—P1—C1—C2	19.61	C18—C23—C24—C25	−176.70
C8—P1—C1—C2	−114.43	C18—C23—C24—C15	0.29
C15—P1—C1—C2	143.28	C22—C23—C24—C25	2.62
Pd1—P1—C1—C6	−161.54	C22—C23—C24—C15	179.62
C8—P1—C1—C6	64.41	C23—C24—C25—C26	−71.98
C15—P1—C1—C6	−37.87	C15—C24—C25—C34	−69.83
C8—P1—C15—C24	−152.93	C15—C24—C25—C26	111.12
C15—P1—C8—C13	59.33	C23—C24—C25—C34	107.08
C1—P1—C15—C24	−49.29	C24—C25—C34—P2	4.55
Pd1—P1—C8—C9	0.84	C26—C25—C34—P2	−176.42
C1—P1—C8—C9	130.41	C26—C25—C34—C33	−2.25
C15—P1—C8—C9	−121.45	C24—C25—C26—C27	−0.30
Pd1—P1—C8—C13	−178.38	C24—C25—C26—C31	−177.70
C1—P1—C8—C13	−48.81	C24—C25—C34—C33	178.73
Pd1—P1—C15—C24	76.91	C34—C25—C26—C31	3.25
Pd1—P1—C15—C16	−98.56	C34—C25—C26—C27	−179.35
C1—P1—C15—C16	135.24	C27—C26—C31—C32	−178.69
C8—P1—C15—C16	31.6	C25—C26—C27—C28	−179.27
C35—P2—C42—C47	−52.13	C31—C26—C27—C28	−1.80
C34—P2—C35—C40	−44.42	C25—C26—C31—C30	179.22
C35—P2—C34—C33	134.82	C25—C26—C31—C32	−1.11
C42—P2—C35—C40	58.53	C27—C26—C31—C30	1.65
Pd1—P2—C34—C33	−98.34	C26—C27—C28—C29	0.93
Pd1—P2—C35—C40	−167.59	C27—C28—C29—C30	0.16
Pd1—P2—C42—C47	176.93	C28—C29—C30—C31	−0.29
C42—P2—C35—C36	−123.89	C29—C30—C31—C32	179.7
Pd1—P2—C34—C25	75.89	C29—C30—C31—C26	−0.65
C35—P2—C34—C25	−50.95	C30—C31—C32—C33	177.66
C42—P2—C34—C25	−154.54	C26—C31—C32—C33	−2.00
C34—P2—C42—C47	54.59	C31—C32—C33—C34	3.1
C35—P2—C42—C43	136.13	C32—C33—C34—P2	173.65
C34—P2—C35—C36	133.15	C32—C33—C34—C25	−0.96
Pd1—P2—C42—C43	5.19	P2—C35—C40—C39	−179.03
C34—P2—C42—C43	−117.15	C40—C35—C36—C37	−1.56
Pd1—P2—C35—C36	9.98	P2—C35—C36—C37	−179.34
C42—P2—C34—C33	31.23	C36—C35—C40—C39	3.4
P1—C1—C2—C3	178.15	C35—C36—C37—C38	−1.08
P1—C1—C6—C5	−177.79	C36—C37—C38—C39	1.85
C6—C1—C2—C3	−0.78	C36—C37—C38—C41	−179.74
C2—C1—C6—C5	1.06	C41—C38—C39—C40	−178.41
C1—C2—C3—C4	−0.08	C37—C38—C39—C40	0
C2—C3—C4—C5	0.66	C38—C39—C40—C35	−2.71
C2—C3—C4—C7	−178.62	P2—C42—C43—C44	174.29
C3—C4—C5—C6	−0.36	C47—C42—C43—C44	1.64
C7—C4—C5—C6	178.91	P2—C42—C47—C46	−175.69
C4—C5—C6—C1	−0.51	C43—C42—C47—C46	−3.75
P1—C8—C9—C10	−179.52	C42—C43—C44—C45	−0.96
P1—C8—C13—C12	179.86	C43—C44—C45—C46	2.16
C13—C8—C9—C10	−0.26	C43—C44—C45—C48	−176.09
C9—C8—C13—C12	0.62	C44—C45—C46—C47	−4.24
C8—C9—C10—C11	−0.19	C48—C45—C46—C47	174.03
C9—C10—C11—C12	0.29	C45—C46—C47—C42	5.3
C9—C10—C11—C14	178.56	C102—C97—C98—C99	2.27
C14—C11—C12—C13	−178.24	C98—C97—C102—C101	1.34
C10—C11—C12—C13	0.07	C97—C98—C99—C100	−5.86
C11—C12—C13—C8	−0.54	C98—C99—C100—C101	5.51
C16—C15—C24—C23	2.02	C99—C100—C101—C102	−1.38
P1—C15—C24—C25	3.56

Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, −y+1, z+1/2; (iii) x, −y, −z+1; (iv) −x, −y, z+1/2; (v) −x, y−1, −z+1/2; (vi) −x, −y, z−1/2; (vii) −x, −y+1, z−1/2; (viii) −x, y+1, −z+1/2.

(15) bis(4-Amin-N-2-thiazolylbenzenesulfonamide-N)-dichloro-methanl-copper(ii) bis(Sulfathiazole-N)-dichloro-methanl-copper(ii)

Crystal data

C19H22Cl2CuN6O5S4	γ = 90°
Mr = 677.16	V = 2516 (3) Å^3
Monclinic, I2/a	Z = 4
Hall symbol: -I 2ya	F(000) = 1292
a = 30.123 (13) Å	Dx = 1.729 Mg m^−3
b = 7.564 (6) Å	Mo Kα radiation, λ = 0.71073 Å
c = 11.044 (6) Å	µ = 1.46 mm^−1
α = 90°	T = 293 K
β = 91.27 (1)°	× × mm

Data collection

Radiation source: fine-focus sealed tube	θmax = 27.6°, θmin = 3.4°
3814 measured reflections	h = −12→35
2078 independent reflections	k = −8→9
2062 reflections with I > 2σ(I)	l = −12→13
Rint = 0.069

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.053	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.156	w = 1/[σ^2(Fo^2) + (0.0576P)^2 + 14.5807P] where P = (Fo^2 + 2Fc^2)/3
S = 1.16	(Δ/σ)max < 0.001
2078 reflections	Δρmax = 0.70 e Å^−3
173 parameters	Δρmin = −0.90 e Å^−3
0 restraints	Extinction correction: nne
Primary atom site location: structure-invariant direct methods

Special details

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 nt 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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Cu1	0.2500	0.34015 (10)	0.5000	0.0295 (3)
Cl1	0.28148 (4)	0.4227 (2)	0.32840 (11)	0.0518 (4)
S1	0.09795 (4)	0.99494 (16)	0.38474 (11)	0.0351 (3)
S2	0.02339 (5)	0.9338 (2)	0.17310 (12)	0.0518 (4)
O1	0.10452 (12)	1.0688 (5)	0.2698 (4)	0.0517 (10)
O2	0.11481 (12)	1.0872 (5)	0.4873 (4)	0.0492 (10)
O5	0.2468 (3)	0.0425 (10)	0.5545 (7)	0.0507 (19)	0.50
N1	0.19059 (12)	0.3159 (5)	0.4140 (4)	0.0332 (9)
N2	0.04656 (12)	0.9685 (6)	0.4120 (3)	0.0338 (9)
N3	−0.02552 (13)	0.9384 (6)	0.3512 (4)	0.0369 (9)
C1	0.16547 (14)	0.4738 (6)	0.4012 (4)	0.0294 (9)
C2	0.13727 (14)	0.5210 (7)	0.4913 (4)	0.0314 (10)
C3	0.11592 (14)	0.6786 (7)	0.4835 (4)	0.0322 (10)
C4	0.12186 (13)	0.7872 (6)	0.3866 (4)	0.0294 (9)
C5	0.14925 (15)	0.7384 (7)	0.2949 (4)	0.0359 (11)
C6	0.17105 (16)	0.5807 (7)	0.3031 (4)	0.0372 (11)
C7	0.01734 (15)	0.9490 (6)	0.3255 (4)	0.0317 (10)
C8	−0.05359 (18)	0.9180 (8)	0.2530 (5)	0.0457 (13)
C9	−0.0326 (2)	0.9106 (9)	0.1505 (5)	0.0529 (14)
C19	0.2500	−0.1134 (13)	0.5000	0.079 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.0270 (4)	0.0269 (4)	0.0350 (5)	0.000	0.0088 (3)	0.000
Cl1	0.0417 (7)	0.0806 (11)	0.0333 (6)	−0.0263 (7)	0.0097 (5)	−0.0086 (7)
S1	0.0252 (6)	0.0342 (7)	0.0463 (7)	−0.0003 (4)	0.0104 (5)	0.0050 (5)
S2	0.0508 (8)	0.0694 (10)	0.0354 (7)	0.0055 (7)	0.0079 (6)	−0.0017 (7)
O1	0.042 (2)	0.052 (2)	0.062 (2)	0.0108 (17)	0.0236 (18)	0.024 (2)
O2	0.039 (2)	0.040 (2)	0.069 (3)	−0.0082 (16)	0.0035 (17)	−0.012 (2)
O5	0.073 (5)	0.035 (4)	0.043 (4)	−0.010 (4)	−0.009 (4)	0.004 (3)
N1	0.0285 (19)	0.0277 (19)	0.044 (2)	0.0000 (15)	0.0053 (16)	−0.0025 (17)
N2	0.0208 (18)	0.044 (2)	0.036 (2)	0.0033 (16)	0.0063 (15)	0.0026 (19)
N3	0.0254 (19)	0.041 (2)	0.045 (2)	0.0028 (17)	0.0013 (16)	−0.003 (2)
C1	0.026 (2)	0.031 (2)	0.032 (2)	−0.0031 (17)	0.0026 (17)	−0.005 (2)
C2	0.025 (2)	0.039 (3)	0.031 (2)	−0.0004 (18)	0.0044 (17)	0.003 (2)
C3	0.025 (2)	0.042 (3)	0.030 (2)	−0.0014 (19)	0.0063 (17)	0.001 (2)
C4	0.021 (2)	0.033 (2)	0.034 (2)	−0.0026 (17)	0.0044 (17)	0.000 (2)
C5	0.031 (2)	0.043 (3)	0.034 (2)	−0.001 (2)	0.0088 (18)	0.004 (2)
C6	0.037 (3)	0.043 (3)	0.033 (2)	0.001 (2)	0.0120 (19)	0.000 (2)
C7	0.030 (2)	0.029 (2)	0.036 (2)	0.0046 (18)	0.0063 (19)	0.003 (2)
C8	0.039 (3)	0.044 (3)	0.053 (3)	0.004 (2)	−0.010 (2)	−0.006 (3)
C9	0.053 (3)	0.056 (4)	0.049 (3)	0.004 (3)	−0.007 (3)	−0.005 (3)
C19	0.116 (9)	0.036 (5)	0.084 (8)	0.000	−0.006 (6)	0.000

Geometric parameters (Å, º)

Cu1—N1^i	2.016 (4)	O5—C19	1.329 (12)
Cu1—N1	2.016 (4)	N1—C1	1.419 (6)
Cu1—Cl1^i	2.2270 (15)	N2—C7	1.293 (6)
Cu1—Cl1	2.2270 (15)	N3—C7	1.330 (6)
Cu1—O5^i	2.333 (8)	N3—C8	1.368 (7)
Cu1—O5	2.333 (8)	C1—C6	1.365 (7)
S1—O1	1.404 (4)	C1—C2	1.370 (6)
S1—O2	1.415 (4)	C2—C3	1.356 (7)
S1—N2	1.596 (4)	C3—C4	1.365 (6)
S1—C4	1.729 (5)	C4—C5	1.371 (6)
S2—C7	1.701 (5)	C5—C6	1.364 (7)
S2—C9	1.710 (6)	C8—C9	1.310 (9)
O5—O5^i	1.223 (15)	C19—O5^i	1.329 (12)
N1^i—Cu1—N1	169.6 (2)	O5^i—O5—C19	62.6 (4)
N1^i—Cu1—Cl1^i	90.85 (12)	O5^i—O5—Cu1	74.81 (19)
N1—Cu1—Cl1^i	92.07 (12)	C19—O5—Cu1	137.4 (5)
N1^i—Cu1—Cl1	92.07 (12)	C1—N1—Cu1	115.9 (3)
N1—Cu1—Cl1	90.85 (12)	C7—N2—S1	121.5 (3)
Cl1^i—Cu1—Cl1	147.45 (10)	C7—N3—C8	115.1 (4)
N1^i—Cu1—O5^i	89.5 (2)	C6—C1—C2	120.7 (4)
N1—Cu1—O5^i	80.4 (2)	C6—C1—N1	120.2 (4)
Cl1^i—Cu1—O5^i	120.7 (2)	C2—C1—N1	119.0 (4)
Cl1—Cu1—O5^i	91.7 (2)	C3—C2—C1	118.9 (4)
N1^i—Cu1—O5	80.4 (2)	C2—C3—C4	120.6 (4)
N1—Cu1—O5	89.5 (2)	C3—C4—C5	120.6 (4)
Cl1^i—Cu1—O5	91.7 (2)	C3—C4—S1	119.6 (3)
Cl1—Cu1—O5	120.7 (2)	C5—C4—S1	119.6 (4)
O5^i—Cu1—O5	30.4 (4)	C6—C5—C4	118.9 (5)
O1—S1—O2	118.2 (3)	C5—C6—C1	120.2 (4)
O1—S1—N2	112.1 (2)	N2—C7—N3	119.9 (4)
O2—S1—N2	104.1 (2)	N2—C7—S2	130.7 (4)
O1—S1—C4	107.8 (2)	N3—C7—S2	109.4 (4)
O2—S1—C4	107.3 (2)	C9—C8—N3	112.9 (5)
N2—S1—C4	106.8 (2)	C8—C9—S2	111.2 (4)
C7—S2—C9	91.4 (3)	O5^i—C19—O5	54.8 (8)
N1^i—Cu1—O5—O5^i	−105.9 (8)	C2—C3—C4—S1	−174.6 (4)
N1—Cu1—O5—O5^i	71.5 (8)	O1—S1—C4—C3	−172.8 (4)
Cl1^i—Cu1—O5—O5^i	163.6 (8)	O2—S1—C4—C3	59.0 (4)
Cl1—Cu1—O5—O5^i	−19.2 (9)	N2—S1—C4—C3	−52.1 (4)
N1^i—Cu1—O5—C19	−105.9 (8)	O1—S1—C4—C5	12.0 (5)
N1—Cu1—O5—C19	71.5 (8)	O2—S1—C4—C5	−116.2 (4)
Cl1^i—Cu1—O5—C19	163.6 (8)	N2—S1—C4—C5	132.7 (4)
Cl1—Cu1—O5—C19	−19.2 (9)	C3—C4—C5—C6	−1.1 (7)
O5^i—Cu1—O5—C19	0.000 (2)	S1—C4—C5—C6	174.1 (4)
N1^i—Cu1—N1—C1	169.6 (3)	C4—C5—C6—C1	0.1 (8)
Cl1^i—Cu1—N1—C1	63.4 (3)	C2—C1—C6—C5	1.4 (7)
Cl1—Cu1—N1—C1	−84.2 (3)	N1—C1—C6—C5	−175.4 (4)
O5^i—Cu1—N1—C1	−175.8 (4)	S1—N2—C7—N3	−175.8 (4)
O5—Cu1—N1—C1	155.1 (4)	S1—N2—C7—S2	3.9 (7)
O1—S1—N2—C7	25.7 (5)	C8—N3—C7—N2	180.0 (5)
O2—S1—N2—C7	154.6 (4)	C8—N3—C7—S2	0.2 (6)
C4—S1—N2—C7	−92.1 (4)	C9—S2—C7—N2	179.5 (5)
Cu1—N1—C1—C6	88.3 (5)	C9—S2—C7—N3	−0.8 (4)
Cu1—N1—C1—C2	−88.6 (4)	C7—N3—C8—C9	0.7 (7)
C6—C1—C2—C3	−1.9 (7)	N3—C8—C9—S2	−1.3 (7)
N1—C1—C2—C3	174.9 (4)	C7—S2—C9—C8	1.2 (5)
C1—C2—C3—C4	1.0 (7)	Cu1—O5—C19—O5^i	0.000 (2)
C2—C3—C4—C5	0.5 (7)

Symmetry code: (i) −x+1/2, y, −z+1.

(16) catena-(tetrakis(mu!2$-4-Aminbenzoato)-diaqua-di-cadmium tetrahydrate)

Crystal data

C14H14CdN2O5·2(H2O)	γ = 90°
Mr = 438.71	V = 1623.2 (3) Å^3
Monclinic, C2/c	Z = 4
Hall symbol: -C 2yc	F(000) = 808
a = 15.2963 (19) Å	Dx = 1.721 Mg m^−3
b = 6.2028 (7) Å	Mo K\a radiation, λ = 0.71073 Å
c = 17.8150 (18) Å	µ = 1.38 mm^−1
α = 90°	T = 0 K
β = 106.196 (4)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cd1	0	−0.17340	0.25	0.02*
O1	0.08205	−0.22035	0.158	0.02*
O2	0.0499	0.1135	0.17995	0.02*
O5	0	−0.54260	0.25	0.02*
N1	0.1433	0.20835	−0.14825	0.02*
C1	0.07967	−0.02288	0.1405	0.02*
C2	0.1073	0.04715	0.07045	0.02*
C3	0.13842	−0.10448	0.0268	0.02*
C4	0.15397	−0.05058	−0.04390	0.02*
C5	0.13778	0.15778	−0.07225	0.02*
C6	0.10932	0.31343	−0.02725	0.02*
C7	0.09412	0.25853	0.04295	0.02*
O6	0.2574	0.06635	0.28135	0.02*

Geometric parameters (Å, º)

Cd1—O1	2.3439	C1—C2	1.4896
Cd1—O2	2.4162	C2—C3	1.3865
Cd1—O5	2.2901 (3)	C2—C7	1.3945
Cd1—C1	2.7365	C3—C4	1.3863
O1—C1	1.2619	C4—C5	1.3845
O2—C1	1.2631	C5—C6	1.3996
N1—C5	1.4151	C6—C7	1.377
Cd1···O5^i	3.9127 (5)	O6···O2	3.1976
Cd1···O6	4.0986	O6···C1	3.1919
Cd1···O5^ii	3.9127 (5)	O6···Cd1	4.0986
Cd1···O6^iii	4.0986	O6···Cd1	4.0986
O1···C6^iv	3.2441	N1···O6^x	2.9569
O1···O6^v	2.7329	C1···C6^iv	3.5245
O2···O5^i	2.6873	C1···C4^iv	3.537
O2···O6	3.1976	C1···O6	3.1919
O2···O5^ii	2.6873	C2···C2^iv	3.5807
O2···C4^iv	3.3963	C3···C7^iv	3.5558
O5···Cd1^vi	3.9127 (5)	C4···O2^iv	3.3963
O5···O2^vi	2.6873	C4···C1^iv	3.537
O5···Cd1^vii	3.9127 (5)	C6···C1^iv	3.5245
O5···O2^vii	2.6873	C6···O1^iv	3.2441
O6···N1^viii	2.9569	C7···C3^iv	3.5558
O6···O1^ix	2.7329
O1—Cd1—O2	54.72	O1^iii—Cd1—N1^iv	87.88
O1—Cd1—O5	82.86	O1^iii—Cd1—N1^viii	90.85
O1—Cd1—C1	27.39	O2^iii—Cd1—C1^iii	27.49
O1—Cd1—O1^iii	165.73	O2^iii—Cd1—N1^iv	95.84
O1—Cd1—O2^iii	139.51	O2^iii—Cd1—N1^viii	91.69
O1—Cd1—C1^iii	166.57	N1^iv—Cd1—C1^iii	94.23
O1—Cd1—N1^iv	90.85	N1^viii—Cd1—C1^iii	89.26
O1—Cd1—N1^viii	87.88	N1^iv—Cd1—N1^viii	169.78
O2—Cd1—O5	137.43	Cd1—O1—C1	93.9
O2—Cd1—C1	27.49	Cd1—O2—C1	90.51
O1^iii—Cd1—O2	139.51	Cd1^iv—N1—C5	114.28
O2—Cd1—O2^iii	85.13	Cd1—C1—O1	58.71
O2—Cd1—C1^iii	112.62	Cd1—C1—O2	62
O2—Cd1—N1^iv	91.69	Cd1—C1—C2	169.59
O2—Cd1—N1^viii	95.84	O1—C1—O2	120.17
O5—Cd1—C1	109.95	O1—C1—C2	119.65
O1^iii—Cd1—O5	82.86	O2—C1—C2	120.09
O2^iii—Cd1—O5	137.43	C1—C2—C3	119.61
O5—Cd1—C1^iii	109.95	C1—C2—C7	121.43
O5—Cd1—N1^iv	84.89	C3—C2—C7	118.64
O5—Cd1—N1^viii	84.89	C2—C3—C4	121.25
O1^iii—Cd1—C1	166.57	C3—C4—C5	119.87
O2^iii—Cd1—C1	112.62	N1—C5—C4	120.24
C1—Cd1—C1^iii	140.1	N1—C5—C6	120.41
N1^iv—Cd1—C1	89.26	C4—C5—C6	119.18
N1^viii—Cd1—C1	94.23	C5—C6—C7	120.52
O1^iii—Cd1—O2^iii	54.72	C2—C7—C6	120.47
O1^iii—Cd1—C1^iii	27.39
O2—Cd1—O1—C1	−4.72	N1^iv—Cd1—C1—O2	95.1
O5—Cd1—O1—C1	171.5	N1^viii—Cd1—C1—O2	−94.52
O2^iii—Cd1—O1—C1	−13.26	Cd1—O1—C1—O2	8.55
N1^iv—Cd1—O1—C1	86.75	Cd1—O1—C1—C2	−168.07
N1^viii—Cd1—O1—C1	−103.39	Cd1—O2—C1—O1	−8.27
O1—Cd1—O2—C1	4.71	Cd1—O2—C1—C2	168.33
O5—Cd1—O2—C1	−0.85	Cd1^iv—N1—C5—C4	91
O1^iii—Cd1—O2—C1	−173.86	Cd1^iv—N1—C5—C6	−84.19
O2^iii—Cd1—O2—C1	179.15	O1—C1—C2—C3	−2.28
C1^iii—Cd1—O2—C1	179.58	O2—C1—C2—C7	−5.43
N1^iv—Cd1—O2—C1	−85.13	O1—C1—C2—C7	171.19
N1^viii—Cd1—O2—C1	87.94	O2—C1—C2—C3	−178.90
O2—Cd1—C1—O1	171.63	C1—C2—C7—C6	−171.72
O5—Cd1—C1—O1	−8.98	C3—C2—C7—C6	1.82
O2^iii—Cd1—C1—O1	170.71	C1—C2—C3—C4	171.88
C1^iii—Cd1—C1—O1	171.02	C7—C2—C3—C4	−1.77
N1^iv—Cd1—C1—O1	−93.27	C2—C3—C4—C5	−0.43
N1^viii—Cd1—C1—O1	77.11	C3—C4—C5—C6	2.57
O1—Cd1—C1—O2	−171.63	C3—C4—C5—N1	−172.69
O5—Cd1—C1—O2	179.39	N1—C5—C6—C7	172.72
O2^iii—Cd1—C1—O2	−0.92	C4—C5—C6—C7	−2.53
C1^iii—Cd1—C1—O2	−0.61	C5—C6—C7—C2	0.32

Symmetry codes: (i) x, y+1, z; (ii) −x, y+1, −z+1/2; (iii) −x, y, −z+1/2; (iv) −x, −y, −z; (v) −x+1/2, y−1/2, −z+1/2; (vi) x, y−1, z; (vii) −x, y−1, −z+1/2; (viii) x, −y, z+1/2; (ix) −x+1/2, y+1/2, −z+1/2; (x) x, −y, z−1/2.

(17) 4-Ferrocenylmethylene-2-phenyl-4H-oxazol-5-one

Crystal data

C20H15FeNO2	γ = 90°
Mr = 357.18	V = 1543.8 (7) Å^3
Monclinic, P21/n	Z = 4
Hall symbol: -P 2yn	F(000) = 676
a = 10.391 (2) Å	Dx = 1.472 Mg m^−3
b = 7.252 (3) Å	Mo K\a radiation, λ = 0.71070 Å
c = 20.662 (2) Å	µ = 0.99 mm^−1
α = 90°	T = 0 K
β = 97.47 (2)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.49402	0.28301	0.22699	0.02*
O1	0.34705	0.28975	−0.05861	0.02*
O2	0.1385	0.24945	−0.04154	0.02*
N1	0.1493	0.31655	0.06581	0.02*
C1	0.3939	0.43825	0.15402	0.02*
C2	0.31085	0.3841	0.20045	0.02*
C3	0.36435	0.4541	0.2621	0.02*
C4	0.47905	0.54870	0.25466	0.02*
C5	0.4999	0.539	0.18883	0.02*
C6	0.48825	0.0034	0.23119	0.02*
C7	0.52585	0.07665	0.29383	0.02*
C8	0.64060	0.17875	0.29176	0.02*
C9	0.6727	0.16850	0.22756	0.02*
C10	0.579	0.05885	0.19063	0.02*
C11	0.3817	0.39485	0.08556	0.02*
C12	0.2734	0.3376	0.04803	0.02*
C13	0.2681	0.29385	−0.02152	0.02*
C14	0.07625	0.2689	0.01369	0.02*
C15	−0.06255	0.23475	0.00547	0.02*
C16	−0.13250	0.2691	0.05718	0.02*
C17	−0.26390	0.2399	0.05005	0.02*
C18	−0.32790	0.1749	−0.00840	0.02*
C19	−0.25940	0.14025	−0.05944	0.02*
C20	−0.12735	0.1705	−0.05305	0.02*

Geometric parameters (Å, º)

Fe1—C1	2.0531	C2—C3	1.4161
Fe1—C2	2.0468	C3—C4	1.4009
Fe1—C3	2.0336	C4—C5	1.4066
Fe1—C4	2.0216	C6—C7	1.4066
Fe1—C5	2.0210	C6—C10	1.3995
Fe1—C6	2.0308	C7—C8	1.4089
Fe1—C7	2.0341	C8—C9	1.4112
Fe1—C8	2.0378	C9—C10	1.4033
Fe1—C9	2.0326	C11—C12	1.3465
Fe1—C10	2.0394	C12—C13	1.4657
O1—C13	1.1936	C14—C15	1.4514
O2—C13	1.3941	C15—C16	1.3906
O2—C14	1.3901	C15—C20	1.3859
N1—C12	1.3944	C16—C17	1.3706
N1—C14	1.2817	C17—C18	1.3835
C1—C2	1.4264	C18—C19	1.3701
C1—C5	1.4347	C19—C20	1.3788
C1—C11	1.4385
N1···C2	3.0956	C13···C19^iv	3.5716
C2···N1	3.0956	C14···C19^iv	3.5849
C4···C6^i	3.3361	C14···C20^iv	3.3144
C5···C6^i	3.4858	C16···C13^iii	3.5077
C6···C4^ii	3.3361	C17···C13^iii	3.4315
C6···C5^ii	3.4858	C18···C11^iii	3.5154
C11···C18^iii	3.5154	C18···C13^iv	3.4963
C12···C19^iv	3.4777	C19···C12^iv	3.4777
C13···C16^iii	3.5077	C19···C13^iv	3.5716
C13···C17^iii	3.4315	C19···C14^iv	3.5849
C13···C18^iv	3.4963	C20···C14^iv	3.3144
C1—Fe1—C2	40.72	Fe1—C1—C11	125
C1—Fe1—C3	68.37	C2—C1—C5	107.17
C1—Fe1—C4	68.58	C2—C1—C11	128.13
C1—Fe1—C5	41.23	C5—C1—C11	124.62
C1—Fe1—C6	124.33	Fe1—C2—C1	69.88
C1—Fe1—C7	157.54	Fe1—C2—C3	69.19
C1—Fe1—C8	161.78	C1—C2—C3	107.77
C1—Fe1—C9	127.13	Fe1—C3—C2	70.2
C1—Fe1—C10	111.65	Fe1—C3—C4	69.33
C2—Fe1—C3	40.61	C2—C3—C4	108.48
C2—Fe1—C4	68.37	Fe1—C4—C3	70.25
C2—Fe1—C5	68.94	Fe1—C4—C5	69.62
C2—Fe1—C6	109.72	C3—C4—C5	108.77
C2—Fe1—C7	120.59	Fe1—C5—C1	70.59
C2—Fe1—C8	153.96	Fe1—C5—C4	69.66
C2—Fe1—C9	164.75	C1—C5—C4	107.79
C2—Fe1—C10	128.23	Fe1—C6—C7	69.88
C3—Fe1—C4	40.42	Fe1—C6—C10	70.22
C3—Fe1—C5	68.52	C7—C6—C10	108.32
C3—Fe1—C6	124.71	Fe1—C7—C6	69.63
C3—Fe1—C7	105.28	Fe1—C7—C8	69.9
C3—Fe1—C8	117.74	C6—C7—C8	107.79
C3—Fe1—C9	153.42	Fe1—C8—C7	69.62
C3—Fe1—C10	163.03	Fe1—C8—C9	69.52
C4—Fe1—C5	40.72	C7—C8—C9	107.77
C4—Fe1—C6	159.36	Fe1—C9—C8	69.91
C4—Fe1—C7	121.39	Fe1—C9—C10	70.1
C4—Fe1—C8	104.26	C8—C9—C10	107.99
C4—Fe1—C9	119.45	Fe1—C10—C6	69.56
C4—Fe1—C10	156.47	Fe1—C10—C9	69.58
C5—Fe1—C6	159.46	C6—C10—C9	108.12
C5—Fe1—C7	158.47	C1—C11—C12	126.44
C5—Fe1—C8	122.62	N1—C12—C11	127.9
C5—Fe1—C9	107.68	N1—C12—C13	108.45
C5—Fe1—C10	123.5	C11—C12—C13	123.6
C6—Fe1—C7	40.49	O1—C13—O2	121.45
C6—Fe1—C8	67.99	O1—C13—C12	133.91
C6—Fe1—C9	67.9	O2—C13—C12	104.63
C6—Fe1—C10	40.22	O2—C14—N1	115.41
C7—Fe1—C8	40.49	O2—C14—C15	116.61
C7—Fe1—C9	68.14	N1—C14—C15	127.97
C7—Fe1—C10	67.9	C14—C15—C16	119.35
C8—Fe1—C9	40.57	C14—C15—C20	121.48
C8—Fe1—C10	67.9	C16—C15—C20	119.17
C9—Fe1—C10	40.32	C15—C16—C17	120.17
C13—O2—C14	105.52	C16—C17—C18	120.37
C12—N1—C14	105.97	C17—C18—C19	119.7
Fe1—C1—C2	69.4	C18—C19—C20	120.48
Fe1—C1—C5	68.19	C15—C20—C19	120.1
C3—Fe1—C1—C2	−37.70	C9—Fe1—C6—C7	81.76
C4—Fe1—C1—C2	−81.30	C10—Fe1—C6—C7	119.17
C5—Fe1—C1—C2	−119.35	C8—Fe1—C9—C10	118.82
C6—Fe1—C1—C2	80.39	C6—Fe1—C10—C9	−119.54
C7—Fe1—C1—C2	39.74	C2—Fe1—C8—C7	52.27
C9—Fe1—C1—C2	167.27	C4—Fe1—C6—C10	−152.71
C10—Fe1—C1—C2	124.03	C5—Fe1—C6—C10	43.99
C2—Fe1—C1—C5	119.35	C1—Fe1—C10—C6	−118.05
C3—Fe1—C1—C5	81.64	C2—Fe1—C10—C6	−74.56
C4—Fe1—C1—C5	38.05	C9—Fe1—C6—C10	−37.41
C6—Fe1—C1—C5	−160.26	C7—Fe1—C10—C6	37.73
C7—Fe1—C1—C5	159.09	C8—Fe1—C10—C6	81.59
C9—Fe1—C1—C5	−73.38	C9—Fe1—C10—C6	119.54
C10—Fe1—C1—C5	−116.63	C1—Fe1—C10—C9	122.41
C2—Fe1—C1—C11	−122.83	C2—Fe1—C10—C9	165.9
C3—Fe1—C1—C11	−160.53	C4—Fe1—C10—C9	36.58
C4—Fe1—C1—C11	155.87	C10—Fe1—C7—C8	81.39
C5—Fe1—C1—C11	117.83	C5—Fe1—C10—C9	77.45
C6—Fe1—C1—C11	−42.44	C7—Fe1—C9—C10	81.15
C7—Fe1—C1—C11	−83.08	C8—Fe1—C10—C9	−37.95
C9—Fe1—C1—C11	44.45	C7—Fe1—C10—C9	−81.81
C10—Fe1—C1—C11	1.2	C1—Fe1—C9—C8	161.37
C6—Fe1—C8—C7	−37.83	C9—Fe1—C7—C6	−81.12
C9—Fe1—C8—C7	−119.11	C10—Fe1—C7—C6	−37.49
C10—Fe1—C8—C7	−81.38	C1—Fe1—C7—C8	174.81
C2—Fe1—C8—C9	171.38	C2—Fe1—C7—C8	−156.21
C3—Fe1—C8—C9	−159.96	C3—Fe1—C7—C8	−115.04
C4—Fe1—C8—C9	−118.88	C4—Fe1—C7—C8	−74.31
C5—Fe1—C8—C9	−78.85	C5—Fe1—C7—C8	−45.05
C6—Fe1—C8—C9	81.28	C6—Fe1—C7—C8	118.87
C7—Fe1—C8—C9	119.11	C9—Fe1—C7—C8	37.75
C10—Fe1—C8—C9	37.72	C4—Fe1—C9—C10	−164.14
C10—Fe1—C5—C1	85.17	C6—Fe1—C9—C10	37.33
C1—Fe1—C5—C4	118.43	C4—Fe1—C10—C6	156.12
C2—Fe1—C5—C4	80.89	C5—Fe1—C10—C6	−163.01
C3—Fe1—C2—C1	119.14	C7—Fe1—C9—C8	−37.68
C4—Fe1—C2—C1	81.87	C3—Fe1—C8—C7	80.94
C5—Fe1—C2—C1	38	C4—Fe1—C8—C7	122.01
C6—Fe1—C2—C1	−120.12	C3—Fe1—C9—C8	42.69
C7—Fe1—C2—C1	−163.52	C4—Fe1—C9—C8	77.03
C8—Fe1—C2—C1	159.86	C5—Fe1—C9—C10	−121.32
C10—Fe1—C2—C1	−78.73	C5—Fe1—C9—C8	119.85
C1—Fe1—C2—C3	−119.14	C6—Fe1—C9—C8	−81.50
C4—Fe1—C2—C3	−37.28	C10—Fe1—C9—C8	−118.82
C5—Fe1—C2—C3	−81.15	C1—Fe1—C9—C10	−79.81
C6—Fe1—C2—C3	120.74	C3—Fe1—C9—C10	161.51
C7—Fe1—C2—C3	77.34	C14—O2—C13—O1	179.94
C8—Fe1—C2—C3	40.72	C13—O2—C14—C15	178.44
C10—Fe1—C2—C3	162.13	C13—O2—C14—N1	−1.05
C1—Fe1—C6—C10	83.36	C14—O2—C13—C12	0.36
C2—Fe1—C6—C10	126.46	C14—N1—C12—C13	−0.93
C3—Fe1—C6—C10	169.34	C12—N1—C14—O2	1.25
C1—Fe1—C3—C2	37.8	C12—N1—C14—C15	−178.17
C4—Fe1—C3—C2	119.73	C14—N1—C12—C11	176.61
C5—Fe1—C3—C2	82.29	C11—C1—C2—C3	177.97
C6—Fe1—C3—C2	−79.80	C5—C1—C2—Fe1	−57.89
C7—Fe1—C3—C2	−119.46	Fe1—C1—C2—C3	59.02
C8—Fe1—C3—C2	−161.12	C11—C1—C2—Fe1	118.95
C9—Fe1—C3—C2	169	C5—C1—C2—C3	1.13
C1—Fe1—C3—C4	−81.93	C2—C1—C11—C12	19.19
C2—Fe1—C3—C4	−119.73	C2—C1—C5—Fe1	58.65
C5—Fe1—C3—C4	−37.44	Fe1—C1—C11—C12	109.4
C6—Fe1—C3—C4	160.47	Fe1—C1—C5—C4	−59.99
C7—Fe1—C3—C4	120.81	C11—C1—C5—Fe1	−118.32
C8—Fe1—C3—C4	79.15	C5—C1—C11—C12	−164.49
C9—Fe1—C3—C4	49.27	C11—C1—C5—C4	−178.31
C4—Fe1—C7—C6	166.81	C2—C1—C5—C4	−1.34
C5—Fe1—C7—C6	−163.92	C1—C2—C3—C4	−0.51
C8—Fe1—C7—C6	−118.87	C1—C2—C3—Fe1	−59.45
C1—Fe1—C4—C3	81.37	Fe1—C2—C3—C4	58.94
C2—Fe1—C4—C3	37.45	C2—C3—C4—C5	−0.34
C5—Fe1—C4—C3	119.88	Fe1—C3—C4—C5	59.14
C6—Fe1—C4—C3	−51.23	C2—C3—C4—Fe1	−59.48
C7—Fe1—C4—C3	−76.08	Fe1—C4—C5—C1	60.58
C8—Fe1—C4—C3	−116.25	C3—C4—C5—C1	1.04
C9—Fe1—C4—C3	−157.09	C3—C4—C5—Fe1	−59.53
C10—Fe1—C4—C3	176.63	C10—C6—C7—C8	0.21
C1—Fe1—C4—C5	−38.50	C7—C6—C10—C9	−0.65
C2—Fe1—C4—C5	−82.43	Fe1—C6—C10—C9	59.08
C3—Fe1—C4—C5	−119.88	C10—C6—C7—Fe1	59.94
C6—Fe1—C4—C5	−171.11	C7—C6—C10—Fe1	−59.73
C7—Fe1—C4—C5	164.04	Fe1—C6—C7—C8	−59.73
C8—Fe1—C4—C5	123.87	Fe1—C7—C8—C9	−59.26
C9—Fe1—C4—C5	83.03	C6—C7—C8—Fe1	59.56
C10—Fe1—C4—C5	56.75	C6—C7—C8—C9	0.3
C5—Fe1—C8—C7	162.04	Fe1—C8—C9—C10	−60.02
C7—Fe1—C6—C10	−119.17	C7—C8—C9—C10	−0.69
C8—Fe1—C6—C10	−81.35	C7—C8—C9—Fe1	59.32
C2—Fe1—C5—C1	−37.54	C8—C9—C10—Fe1	59.9
C3—Fe1—C5—C1	−81.26	Fe1—C9—C10—C6	−59.07
C4—Fe1—C5—C1	−118.43	C8—C9—C10—C6	0.83
C6—Fe1—C5—C1	52.64	C1—C11—C12—C13	−179.36
C7—Fe1—C5—C1	−158.20	C1—C11—C12—N1	3.44
C8—Fe1—C5—C1	168.74	C11—C12—C13—O2	−177.35
C9—Fe1—C5—C1	126.69	N1—C12—C13—O1	−179.18
C1—Fe1—C7—C6	55.94	N1—C12—C13—O2	0.33
C2—Fe1—C7—C6	84.92	C11—C12—C13—O1	3.15
C3—Fe1—C7—C6	126.09	O2—C14—C15—C16	−173.83
C3—Fe1—C5—C4	37.17	O2—C14—C15—C20	5.45
C6—Fe1—C5—C4	171.07	N1—C14—C15—C16	5.58
C7—Fe1—C5—C4	−39.76	N1—C14—C15—C20	−175.14
C8—Fe1—C5—C4	−72.83	C14—C15—C16—C17	179.17
C9—Fe1—C5—C4	−114.87	C20—C15—C16—C17	−0.13
C10—Fe1—C5—C4	−156.39	C14—C15—C20—C19	−179.68
C1—Fe1—C6—C7	−157.47	C16—C15—C20—C19	−0.40
C2—Fe1—C6—C7	−114.37	C15—C16—C17—C18	0.45
C3—Fe1—C6—C7	−71.48	C16—C17—C18—C19	−0.23
C4—Fe1—C6—C7	−33.54	C17—C18—C19—C20	−0.30
C5—Fe1—C6—C7	163.16	C18—C19—C20—C15	0.61
C8—Fe1—C6—C7	37.83

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

(18) bis((mu!2$-Chloro)-diaqua-(2,4-pentanedione-O,O')-magnesium) diaqua-bis(2,4-pe ntanedione-O,O')-magnesium dichloride

Crystal data

C10H24Cl2Mg2O8·C10H20MgO6·4(Cl)	Z = 2
Mr = 794.18	F(000) = 740
Orthorhombic, Pmna	Dx = 1.315 Mg m^−3
Hall symbol: -P 2ac 2	Mo Kα radiation, λ = 0.71070 Å
a = 13.303 (3) Å	µ = 0.55 mm^−1
b = 7.835 (2) Å	T = 0 K
c = 18.169 (4) Å	× × mm
V = 1893.7 (8) Å^3

Data collection

Radiation source: fine-focus sealed tube	θmax = 37.8°, θmin = 1.9°
16258 measured reflections	h = −13→13
2204 independent reflections	k = −8→8
1626 reflections with I > 2σ(I)	l = −18→18
Rint = 0.274

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.129	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.473	H atoms treated by a mixture of independent and constrained refinement
S = 2.65	w = 1/[σ^2(Fo^2) + (0.1P)^2] where P = (Fo^2 + 2Fc^2)/3
2204 reflections	(Δ/σ)max = 0.593
54 parameters	Extinction correction: nne
0 restraints

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is nt 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 (Ų)

	x	y	z	Uiso*/Ueq
Mg2	0.5	0.5	0	0.02*
O5	0.5	0.7546	0.0239	0.02*
O6	0.3832	0.4603	0.0739	0.02*
C6	0.29165	0.45435	0.0674	0.02*
C7	0.2381	0.5	0	0.02*
C9	0.22835	0.406	0.13295	0.02*
Cl1	0	1.20660	0.0285	0.02*
Mg1	0	0.9315	0.09570	0.02*
O1	0.15235	0.91845	0.1063	0.02*
O3	0	0.6986	0.15360	0.02*
O4	0	1.0335	0.2026	0.02*
C1	0	0.66110	0.2177	0.02*
C2	0	0.7871	0.279	0.02*
C3	0	0.9693	0.2639	0.02*
C4	0	0.4783	0.2428	0.02*
C5	0	1.0782	0.3334	0.02*
Cl2	0.25	0.79650	0.25	0.02*
Cl3	0.32480	0	0	0.02*

Geometric parameters (Å, º)

Cl1—Mg1	2.4772 (6)	O3—C1	1.2011 (3)
Mg2—O6	2.077	O4—C3	1.2221 (3)
Mg2—O5^i	2.0415 (5)	C6—C9	1.507
Mg2—O5	2.0415 (5)	C6—C7	1.4612
Mg1—O1	2.0384	C1—C2	1.4883 (4)
Mg1—O3	2.1063 (5)	C1—C4	1.5031 (4)
Mg1—O4	2.1003 (5)	C2—C3	1.4537 (4)
O6—C6	1.2245	C3—C5	1.5240 (4)
Cl1···Cl1^ii	3.3990 (9)	O1···Cl1^ii	3.3266
Cl1···Mg1^ii	2.5026 (6)	O1···Cl3^i	3.0662
Cl1···O1^ii	3.3266	O1···O3	2.7952
Cl1···O3^ii	3.3909 (9)	O3···O1	2.7952
Cl1···Cl1^iii	3.3990 (9)	O3···Cl1^iii	3.3909 (9)
Cl1···Mg1^iii	2.5026 (6)	O3···Cl1^ii	3.3909 (9)
Cl1···O1^iii	3.3266	O3···O4	2.7709 (7)
Cl1···O3^iii	3.3909 (9)	O3···O1^iv	2.7952
Cl1···O1^iv	3.347	O4···O3	2.7709 (7)
Cl1···O1	3.347	O4···O1	2.8252
Cl1···O4	3.4417 (9)	O4···O1^iv	2.8252
Cl2···C3^v	3.5996 (9)	O4···Cl1	3.4417 (9)
Cl2···C3	3.5996 (9)	O5···O6^x	2.8994
Cl2···C1	3.5398 (9)	O5···O6^i	2.8994
Cl2···C2	3.3680 (9)	O5···Cl3^x	3.0525 (8)
Cl2···C1	3.5398 (9)	O5···Cl3^ix	3.0525 (8)
Cl2···C2	3.3680 (9)	O5···O6	2.9251
Cl2···C3	3.5996 (9)	O5···Cl3^i	3.0525 (8)
Cl2···O1^vi	3.0687	O5···O6^xi	2.9251
Cl2···C1^vi	3.5398 (9)	O5···Cl3^xii	3.0525 (8)
Cl2···C2^vi	3.3680 (9)	O6···O6^xi	3.1076
Cl2···C3^vi	3.5996 (9)	O6···O5^i	2.8994
Cl2···C1^v	3.5398 (9)	O6···O5	2.9251
Cl2···C2^v	3.3680 (9)	O6···O5^i	2.8994
Cl2···O1	3.0687	O6···O6^i	2.7565
Cl3···O1^i	3.0662	C1···Cl2^iv	3.5398 (9)
Cl3···O5^i	3.0525 (8)	C1···Cl2	3.5398 (9)
Cl3···O5^i	3.0525 (8)	C1···Cl2^vi	3.5398 (9)
Cl3···O5^vii	3.0525 (8)	C1···Cl2^xiii	3.5398 (9)
Cl3···O5^viii	3.0525 (8)	C2···Cl2^xiii	3.3680 (9)
Cl3···O1^viii	3.0662	C2···Cl2^iv	3.3680 (9)
Mg1···Cl1^ii	2.5026 (6)	C2···Cl2^vi	3.3680 (9)
Mg1···Cl1^iii	2.5026 (6)	C2···Cl2	3.3680 (9)
Mg1···Mg1^iii	3.6394 (9)	C3···Cl2	3.5996 (9)
Mg1···Mg1^ii	3.6394 (9)	C3···Cl2^xiii	3.5996 (9)
O1···Cl2	3.0687	C3···Cl2^iv	3.5996 (9)
O1···Cl1	3.347	C3···Cl2^vi	3.5996 (9)
O1···O4	2.8252	C4···C5^xiv	3.5407 (9)
O1···Cl3^ix	3.0662	C4···C5^viii	3.5407 (9)
O1···Cl1^iii	3.3266	C5···C4^xv	3.5407 (9)
O1···Cl2^vi	3.0687	C5···C4^ix	3.5407 (9)
O5—Mg2—O6	90.51	Cl1—Mg1—O1	95.18
O5—Mg2—O5^i	180	Cl1—Mg1—O3	179.57
O5—Mg2—O6^i	89.49	O1^iv—Mg1—O4	86.08
O5—Mg2—O6^x	89.49	O3—Mg1—O4	82.4
O5—Mg2—O6^xi	90.51	O1^iv—Mg1—O3	84.8
O5^i—Mg2—O6	89.49	Mg2—O6—C6	133.43
O6—Mg2—O6^i	83.15	Mg1—O3—C1	134.12
O6—Mg2—O6^x	180	Mg1—O4—C3	133.33
O6—Mg2—O6^xi	96.85	C7—C6—C9	116.84
O5^i—Mg2—O6^i	90.51	O6—C6—C9	119.28
O5^i—Mg2—O6^x	90.51	O6—C6—C7	123.81
O5^i—Mg2—O6^xi	89.49	C6—C7—C6^i	121.64
O6^i—Mg2—O6^x	96.85	O3—C1—C2	124.29
O6^i—Mg2—O6^xi	180	O3—C1—C4	121.82
O6^x—Mg2—O6^xi	83.15	C2—C1—C4	113.89
Cl1—Mg1—O4	97.16	C1—C2—C3	120.67
Cl1—Mg1—O1^iv	95.18	O4—C3—C2	125.18
O1—Mg1—O3	84.8	O4—C3—C5	121.65
O1—Mg1—O4	86.08	C2—C3—C5	113.17
O1—Mg1—O1^iv	167.72
O5—Mg2—O6—C6	94.08	Mg1—O3—C1—C4	180
O5^i—Mg2—O6—C6	−85.92	Mg1—O3—C1—C2	0
O6^i—Mg2—O6—C6	4.65	Mg1—O4—C3—C5	−180.00
O6^xi—Mg2—O6—C6	−175.35	Mg1—O4—C3—C2	0
O1—Mg1—O4—C3	−85.27	C9—C6—C7—C6^i	−178.73
O3—Mg1—O4—C3	0	O6—C6—C7—C6^i	4.39
O4—Mg1—O3—C1	0	O3—C1—C2—C3	0
Cl1—Mg1—O4—C3	180	C4—C1—C2—C3	−180.00
O1—Mg1—O3—C1	86.73	C1—C2—C3—C5	180
Mg2—O6—C6—C9	174.32	C1—C2—C3—O4	0
Mg2—O6—C6—C7	−8.88

Symmetry codes: (i) x, −y+1, −z; (ii) x, −y+2, −z; (iii) −x, −y+2, −z; (iv) −x, y, z; (v) x+1/2, y, −z+1/2; (vi) −x+1/2, y, −z+1/2; (vii) −x+1, y−1, z; (viii) x, y−1, z; (ix) x, y+1, z; (x) −x+1, −y+1, −z; (xi) −x+1, y, z; (xii) −x+1, y+1, z; (xiii) x−1/2, y, −z+1/2; (xiv) −x, y−1, z; (xv) −x, y+1, z.

(19) tris((mu!2$-Cyan)-tetracarbonyl-rhenium)

Crystal data

C12N6O12Re3	Z = 4
Mr = 978.81	F(000) = 1740
Orthorhombic, Pnma	Dx = 2.820 Mg m^−3
Hall symbol: -P 2ac 2n	Mo K\a radiation, λ = 0.71073 Å
a = 20.639 (3) Å	µ = 15.78 mm^−1
b = 16.657 (3) Å	T = 0 K
c = 6.705 (3) Å	× × mm
V = 2305.1 (12) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Re1	0.12255	0.09275	0.51490	0.02*
Re2	−0.07920	0.25	0.2172	0.02*
O1	0.1973	0.13705	0.1247	0.02*
O2	0.04935	0.0573	0.9156	0.02*
O3	0.24705	0.0414	0.72845	0.02*
O4	0.09845	−0.07660	0.34295	0.02*
O5	−0.00740	0.25	−0.20150	0.02*
O6	−0.17165	0.1146	0.0793	0.02*
O7	−0.15240	0.25	0.62410	0.02*
N1	0.0301	0.1348	0.3735	0.02*
N3	0.1347	0.215	0.5818	0.02*
N13	−0.00600	0.1711	0.3139	0.02*
C1	0.1707	0.12375	0.26575	0.02*
C2	0.07370	0.0697	0.75875	0.02*
C3	0.20365	0.06195	0.6473	0.02*
C4	0.1073	−0.01415	0.4164	0.02*
C5	−0.03500	0.25	−0.04670	0.02*
C6	−0.13530	0.16535	0.1311	0.02*
C7	−0.12430	0.25	0.4866	0.02*

Geometric parameters (Å, º)

Re1—N1	2.2428	O1—C1	1.1158
Re1—N3	2.1002	O2—C2	1.1837
Re1—C1	2.0112	O3—C3	1.1025
Re1—C2	1.9589	O4—C4	1.1653
Re1—C3	1.9629	O5—C5	1.1840 (5)
Re1—C4	1.9251	O6—C6	1.1824
Re2—N13	2.1048	O7—C7	1.0892 (5)
Re2—C5	1.9908 (9)	N1—N13	1.0394
Re2—C6	1.9136	N3—N3^i	1.166
Re2—C7	2.0321 (9)
O2···O2^ii	3.0124	O7···C5^x	3.2777 (15)
O3···C1^iii	3.2422	O7···O4^xi	3.1034
O3···C4^iii	3.291	O7···O4^vi	3.1034
O3···O6^iv	2.9258	O7···O5^xii	3.2130 (14)
O4···O7^v	3.1034	O7···C5^xii	3.2777 (15)
O4···C7^v	3.1517	C1···O3^xiii	3.2422
O4···O7^vi	3.1034	C1···O6^iv	3.419
O4···C7^vi	3.1517	C3···O6^iv	3.1147
O5···O7^vii	3.2130 (14)	C4···O3^xiii	3.291
O5···C7^vii	3.1929 (14)	C5···O7^vii	3.2777 (15)
O5···O7^viii	3.2130 (14)	C5···O7^viii	3.2777 (15)
O5···C7^viii	3.1929 (14)	C7···O5^x	3.1929 (14)
O6···O3^ix	2.9258	C7···O4^xi	3.1517
O6···C1^ix	3.419	C7···O4^vi	3.1517
O6···C3^ix	3.1147	C7···O5^xii	3.1929 (14)
O7···O5^x	3.2130 (14)
N1—Re1—N3	83.63	C5—Re2—C6	90.52
N1—Re1—C1	89.37	C5—Re2—C7	179.97
N1—Re1—C2	88.63	N13^i—Re2—C5	86.84
N1—Re1—C3	176.62	C5—Re2—C6^i	90.52
N1—Re1—C4	90.27	C6—Re2—C7	89.49
N3—Re1—C1	82.5	N13^i—Re2—C6	170.86
N3—Re1—C2	94.2	C6—Re2—C6^i	94.92
N3—Re1—C3	93.15	N13^i—Re2—C7	93.15
N3—Re1—C4	171.75	C6^i—Re2—C7	89.49
C1—Re1—C2	176.32	N13^i—Re2—C6^i	93.85
C1—Re1—C3	91.23	Re1—N1—N13	162.55
C1—Re1—C4	91.91	Re1—N3—N3^i	165.84
C2—Re1—C3	90.58	Re2—N13—N1	174.98
C2—Re1—C4	91.2	Re1—C1—O1	176.52
C3—Re1—C4	93.03	Re1—C2—O2	173.86
N13—Re2—C5	86.84	Re1—C3—O3	175.66
N13—Re2—C6	93.85	Re1—C4—O4	175.06
N13—Re2—C7	93.15	Re2—C5—O5	178.51
N13—Re2—N13^i	77.28	Re2—C6—O6	177.85
N13—Re2—C6^i	170.86	Re2—C7—O7	175.09

Symmetry codes: (i) x, −y+1/2, z; (ii) −x, −y, −z+2; (iii) −x+1/2, −y, z+1/2; (iv) x+1/2, y, −z+1/2; (v) −x, y−1/2, −z+1; (vi) −x, −y, −z+1; (vii) x, y, z−1; (viii) x, −y+1/2, z−1; (ix) x−1/2, y, −z+1/2; (x) x, y, z+1; (xi) −x, y+1/2, −z+1; (xii) x, −y+1/2, z+1; (xiii) −x+1/2, −y, z−1/2.

(20) 2-(4'-Cyanphenylthio)-5-methylthiadiazole

Crystal data

C10H7N3S2	γ = 90°
Mr = 233.33	V = 524.1 (2) Å^3
Monclinic, P21/m	Z = 2
Hall symbol: -P 2yb	F(000) = 240
a = 5.628 (1) Å	Dx = 1.479 Mg m^−3
b = 7.207 (2) Å	Mo K\a radiation, λ = 0.71073 Å
c = 13.126 (2) Å	µ = 0.47 mm^−1
α = 90°	T = 0 K
β = 100.12 (6)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
S1	0.41806	0.25	0.18596	0.05*
S2	0.79678	0.25	0.04157	0.05*
N1	0.3413	0.25	−0.01690	0.05*
N2	0.4406	0.25	−0.10660	0.05*
N3	1.5272	0.25	0.54220	0.05*
C1	0.5051	0.25	0.0643	0.05*
C2	0.6743	0.25	−0.08820	0.05*
C3	0.8246	0.25	−0.17030	0.05*
C4	0.70310	0.25	0.2703	0.05*
C5	0.8097	0.0831	0.30425	0.05*
C6	1.0244	0.0828	0.37345	0.05*
C7	1.1292	0.25	0.4088	0.05*
C10	1.3526	0.25	0.4826	0.05*
H1	0.9921	0.25	−0.13910	0.05*
H2	0.78945	0.14135	−0.21250	0.05*
H4	0.73695	−0.02825	0.2806	0.05*
H5	1.098	−0.02875	0.39625	0.05*

Geometric parameters (Å, º)

S1—C1	1.7507 (5)	C4—C5	1.3825
S1—C4	1.7818 (5)	C5—C6	1.3782
S2—C1	1.7193 (5)	C6—C7	1.3853
S2—C2	1.7216 (5)	C7—C10	1.4461 (4)
N1—N2	1.3892 (4)	C3—H1	0.9595
N1—C1	1.2808 (4)	C3—H2	0.9595
N2—C2	1.2948 (4)	C5—H4	0.9292
N3—C10	1.1434 (3)	C6—H5	0.9295
C2—C3	1.4823 (4)
S1···S2^i	3.6728 (10)	N2···H1^ii	2.4849
S1···C7^i	3.5874 (10)	N3···H5^viii	2.6544
S1···C7^ii	3.5874 (10)	N3···H5^ix	2.6544
S1···S2^ii	3.6728 (10)	C3···N1^iv	3.2331 (9)
S2···N1^iii	3.2874 (9)	C3···N2^iv	3.4204 (9)
S2···S1^iii	3.6728 (10)	C3···N1^iii	3.2331 (9)
S2···S1^iv	3.6728 (10)	C3···N2^iii	3.4204 (9)
S2···N1^iv	3.2874 (9)	C5···S2	3.6404
S2···C5	3.6404	C6···C6^x	3.5857
S2···C5^v	3.6404	C7···S1^iv	3.5874 (10)
S1···H2^vi	3.0957	C7···S1^iii	3.5874 (10)
S1···H2^vii	3.0957	C6···H2^xi	2.9914
N1···S2^i	3.2874 (9)	H1···N1^iv	2.3081
N1···C3^i	3.2331 (9)	H1···N2^iv	2.4849
N1···S2^ii	3.2874 (9)	H1···N1^iii	2.3081
N1···C3^ii	3.2331 (9)	H1···N2^iii	2.4849
N2···C3^i	3.4204 (9)	H2···S1^xii	3.0957
N2···C3^ii	3.4204 (9)	H2···S1^vii	3.0957
N1···H1^i	2.3081	H2···C6^xi	2.9914
N1···H1^ii	2.3081	H4···N2^xii	2.8226
N2···H4^vi	2.8226	H4···N2^vii	2.8226
N2···H4^vii	2.8226	H5···N3^xiii	2.6544
N2···H1^i	2.4849	H5···N3^ix	2.6544
C1—S1—C4	101.60 (6)	C6—C7—C10	119.56
C1—S2—C2	86.74 (6)	C6—C7—C6^v	120.88
N2—N1—C1	111.55 (6)	C6^v—C7—C10	119.56
N1—N2—C2	112.87 (6)	N3—C10—C7	178.92 (6)
S1—C1—S2	125.95 (6)	C2—C3—H1	109.45
S1—C1—N1	118.89 (6)	C2—C3—H2	109.49
S2—C1—N1	115.16 (6)	C2—C3—H2^v	109.49
S2—C2—N2	113.67 (6)	H1—C3—H2	109.5
S2—C2—C3	122.61 (6)	H1—C3—H2^v	109.5
N2—C2—C3	123.72 (6)	H2—C3—H2^v	109.39
S1—C4—C5	119.51	C4—C5—H4	120.2
S1—C4—C5^v	119.51	C6—C5—H4	120.18
C5—C4—C5^v	120.92	C5—C6—H5	120.2
C4—C5—C6	119.63	C7—C6—H5	120.34
C5—C6—C7	119.46
C4—S1—C1—S2	0.00 (6)	N2—N1—C1—S1	180.00 (6)
C4—S1—C1—N1	180.00 (6)	N1—N2—C2—S2	0.00 (6)
C1—S1—C4—C5	−91.33	N1—N2—C2—C3	180.00 (6)
C1—S2—C2—N2	0.00 (6)	S1—C4—C5—C6	−176.85
C2—S2—C1—S1	180.00 (6)	C5^v—C4—C5—C6	0.45
C1—S2—C2—C3	180.00 (6)	C4—C5—C6—C7	0.63
C2—S2—C1—N1	0.00 (6)	C5—C6—C7—C10	179.08
N2—N1—C1—S2	0.00 (6)	C5—C6—C7—C6^v	−1.71
C1—N1—N2—C2	0.00 (6)

Symmetry codes: (i) x−1, y, z; (ii) x−1, −y+1/2, z; (iii) x+1, −y+1/2, z; (iv) x+1, y, z; (v) x, −y+1/2, z; (vi) −x+1, y+1/2, −z; (vii) −x+1, −y, −z; (viii) −x+3, y+1/2, −z+1; (ix) −x+3, −y, −z+1; (x) −x+2, −y, −z+1; (xi) −x+2, −y, −z; (xii) −x+1, y−1/2, −z; (xiii) −x+3, y−1/2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C3—H1···N1^iv	0.96	2.31	3.2331 (9)	162
C3—H1···N2^iv	0.96	2.48	3.4204 (9)	165
C3—H1···N1^iii	0.96	2.31	3.2331 (9)	162
C3—H1···N2^iii	0.96	2.48	3.4204 (9)	165

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

(21) trans-bis(mu!2$-Chloro)-dichloro-dicarbonyl-di-platinum(ii)

Crystal data

C2Cl4O2Pt2	Z = 2
Mr = 587.98	F(000) = 504
Tetragonal, P42/m	Dx = 4.430 Mg m^−3
Hall symbol: -P 4c	Mo K\a radiation, λ = 0.71073 Å
a = 11.183 (3) Å	µ = 32.85 mm^−1
c = 3.525 (2) Å	T = 0 K
V = 440.8 (3) Å^3	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pt1	0.3915	0.10905	0	0.02*
Cl1	0.59570	0.1045	0	0.02*
Cl2	0.3826	0.2987	0	0.02*
O1	0.13	0.1	0	0.02*
C1	0.226	0.103	0	0.02*

Geometric parameters (Å, º)

Pt1—Cl1	2.2841 (13)	Pt1—Cl1^i	2.3924 (14)
Pt1—Cl2	2.1232 (12)	O1—C1	1.0741 (6)
Pt1—C1	1.8520 (11)
Pt1···Pt1^ii	3.525 (2)	Cl2···Pt1^ii	4.115 (2)
Pt1···Pt1^iii	3.525 (2)	Cl2···Pt1^iii	4.115 (2)
Pt1···Cl1^ii	4.200 (2)	Cl2···Cl2^ii	3.525 (2)
Pt1···Cl1^iii	4.200 (2)	Cl2···Cl2^iii	3.525 (2)
Pt1···Cl2^ii	4.115 (2)	Cl2···Pt1^iv	4.115 (2)
Pt1···Cl2^iii	4.115 (2)	Cl2···Pt1^v	4.115 (2)
Pt1···C1^ii	3.982 (2)	Cl2···Cl2^iv	3.525 (2)
Pt1···C1^iii	3.982 (2)	Cl2···Cl2^v	3.525 (2)
Pt1···Pt1^iv	3.525 (2)	O1···O1^vi	3.1360 (18)
Pt1···Pt1^v	3.525 (2)	O1···O1^vii	3.1360 (18)
Pt1···Cl1^iv	4.200 (2)	O1···O1^viii	3.1360 (18)
Pt1···Cl1^v	4.200 (2)	O1···O1^ix	3.1360 (18)
Pt1···Cl2^iv	4.115 (2)	O1···O1^x	3.1360 (18)
Pt1···Cl2^v	4.115 (2)	O1···O1^xi	3.1360 (18)
Pt1···C1^iv	3.982 (2)	O1···O1^xii	3.1360 (18)
Pt1···C1^v	3.982 (2)	O1···O1^xiii	3.1360 (18)
Cl1···Pt1^ii	4.200 (2)	C1···Pt1^ii	3.982 (2)
Cl1···Pt1^iii	4.200 (2)	C1···Pt1^iii	3.982 (2)
Cl1···Cl1^ii	3.525 (2)	C1···C1^ii	3.525 (2)
Cl1···Cl1^iii	3.525 (2)	C1···C1^iii	3.525 (2)
Cl1···Pt1^iv	4.200 (2)	C1···Pt1^iv	3.982 (2)
Cl1···Pt1^v	4.200 (2)	C1···Pt1^v	3.982 (2)
Cl1···Cl1^iv	3.525 (2)	C1···C1^iv	3.525 (2)
Cl1···Cl1^v	3.525 (2)	C1···C1^v	3.525 (2)
Cl1—Pt1—Cl2	93.96	Cl1^i—Pt1—Cl2	179.26
Cl1—Pt1—C1	176.63	Cl1^i—Pt1—C1	91.34
Cl1—Pt1—Cl1^i	85.29	Pt1—Cl1—Pt1^i	94.71
Cl2—Pt1—C1	89.41	Pt1—C1—O1	179.7

Symmetry codes: (i) −x+1, −y, z; (ii) x, y, z−1; (iii) x, y, z+1; (iv) x, y, −z−1; (v) x, y, −z+1; (vi) −y, x, z−1/2; (vii) −y, x, z+1/2; (viii) y, −x, z−1/2; (ix) y, −x, z+1/2; (x) y, −x, −z−1/2; (xi) y, −x, −z+1/2; (xii) −y, x, −z−1/2; (xiii) −y, x, −z+1/2.

(22) Dihydro-1H-pyrrolizine-3,5(2H,6H)-dione

Crystal data

C7H9NO2	γ = 90°
Mr = 139.15	V = 340.0 (3) Å^3
Monclinic, P21/m	Z = 2
Hall symbol: -P 2yb	F(000) = 148
a = 7.110 (4) Å	Dx = 1.271 Mg m^−3
b = 6.993 (4) Å	Mo K\a radiation, λ = 0.71073 Å
c = 7.678 (4) Å	µ = 0.10 mm^−1
α = 90°	T = 0 K
β = 117.04 (4)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
O1	1.2838	0.25	0.7036	0.05*
O2	1.0045	0.25	0.2625	0.05*
N1	0.9252	0.25	0.51920	0.05*
C2	1.0457	0.25	0.8528	0.05*
C3	1.1091	0.25	0.6901	0.05*
C4	0.8777	0.25	0.3245	0.05*
C5	0.6408	0.25	0.2127	0.05*
C1	0.8092	0.2327	0.74910	0.05*	0.25
C1'	0.8092	0.2673	0.74910	0.05*	0.25
C6	0.5716	0.2283	0.3694	0.05*	0.25
C6'	0.5716	0.2717	0.3694	0.05*	0.25
C7	0.73510	0.29140	0.54940	0.05*	0.25
C7'	0.73510	0.2086	0.54940	0.05*	0.25

Geometric parameters (Å, º)

O1—C3	1.1986 (7)	C1'—C7'	1.4362
O2—C4	1.1957 (7)	C2—C3	1.5085 (9)
N1—C3	1.3680 (8)	C4—C5	1.5031 (9)
N1—C4	1.3747 (8)	C5—C6	1.5003
N1—C7	1.4998	C5—C6'	1.5003
N1—C7'	1.4998	C6—C6'	0.3035
C1—C7'	1.3865	C6—C7	1.4126
C1—C2	1.5029	C6—C7'	1.3489
C1—C1'	0.242	C6'—C7	1.3489
C1—C7	1.4362	C6'—C7'	1.4126
C1'—C2	1.5029	C7—C7'	0.579
C1'—C7	1.3865
O1···O2	3.0494 (17)	C3···C7'^iii	2.3896
O2···O1	3.0494 (17)	C4···C7'^iii	2.3844
O2···C2^i	3.2892 (19)	C4···C3^ix	3.501 (2)
O2···C2^ii	3.2892 (19)	C4···C1^iii	3.5105
N1···C1^iii	2.2659	C4···C1'^iii	3.5105
N1···C1'^iii	2.2659	C4···C3^vi	3.501 (2)
N1···C6^iii	2.2444	C4···C3^vii	3.501 (2)
N1···C6'^iii	2.2444	C4···C3^viii	3.501 (2)
N1···C7^iii	1.4998	C4···C7^iii	2.3844
N1···C7'^iii	1.4998	C4···C6^iii	2.3581
C1···C6^iii	2.6362	C4···C6'^iii	2.3581
C1···C6'^iii	2.6222	C5···C6^iii	1.5003
C1···C7^iii	1.3865	C5···C6'^iii	1.5003
C1···C7'^iii	1.4362	C5···C7^iii	2.375
C1···C1^iii	0.242	C5···C7'^iii	2.375
C1'···C1'^iii	0.242	C6···C1^iii	2.6362
C1'···C6'^iii	2.6362	C6···C1'^iii	2.6222
C1'···C7^iii	1.4362	C6···C6^iii	0.3035
C1'···C6^iii	2.6222	C6···C7^iii	1.3489
C1'···C7'^iii	1.3865	C6···C7'^iii	1.4126
C2···O2^iv	3.2892 (19)	C6'···C1^iii	2.6222
C2···C1^iii	1.5029	C6'···C1'^iii	2.6362
C2···O2^v	3.2892 (19)	C6'···C6'^iii	0.3035
C2···C7^iii	2.3895	C6'···C7^iii	1.4126
C2···C7'^iii	2.3895	C6'···C7'^iii	1.3489
C2···C1'^iii	1.5029	C7···C1^iii	1.3865
C3···C4^vi	3.501 (2)	C7···C1'^iii	1.4362
C3···C1^iii	2.3759	C7···C6^iii	1.3489
C3···C1'^iii	2.3759	C7···C6'^iii	1.4126
C3···C6^iii	3.4835	C7···C7^iii	0.579
C3···C6'^iii	3.4835	C7'···C1^iii	1.4362
C3···C7^iii	2.3896	C7'···C1'^iii	1.3865
C3···C4^vii	3.501 (2)	C7'···C6^iii	1.4126
C3···C4^viii	3.501 (2)	C7'···C6'^iii	1.3489
C3···C4^ix	3.501 (2)	C7'···C7'^iii	0.579
C3—N1—C4	134.29 (4)	C5—C6'—C6	84.19
C3—N1—C7	112.78	C5—C6'—C7	112.82
C3—N1—C7'	112.78	C5—C6'—C7'	109.21
C4—N1—C7	112.02	C6—C6'—C7	95.86
C4—N1—C7'	112.02	C6—C6'—C7'	71.8
C7—N1—C7'	22.26	C7—C6'—C7'	24.06
C1'—C1—C7	73.39	N1—C7—C1	101.01
C1'—C1—C7'	96.98	N1—C7—C1'	103.38
C7—C1—C7'	23.59	N1—C7—C6	100.78
C2—C1—C7	108.76	N1—C7—C6'	103.85
C2—C1—C7'	111.52	N1—C7—C7'	78.87
C1'—C1—C2	85.38	C1—C7—C1'	9.63
C1—C1'—C2	85.38	C1—C7—C6	133.99
C2—C1'—C7	111.52	C1—C7—C6'	142.34
C7—C1'—C7'	23.59	C1—C7—C7'	73.39
C2—C1'—C7'	108.76	C1'—C7—C6	140.71
C1—C1'—C7	96.98	C1'—C7—C6'	146.91
C1—C1'—C7'	73.39	C1'—C7—C7'	83.02
C1'—C2—C3	104.17	C6—C7—C6'	12.34
C1—C2—C1'	9.23	C6—C7—C7'	71.8
C1—C2—C3	104.17	C6'—C7—C7'	84.14
O1—C3—N1	125.73 (4)	N1—C7'—C1	103.38
O1—C3—C2	128.06 (4)	N1—C7'—C1'	101.01
N1—C3—C2	106.21 (4)	N1—C7'—C6	103.85
O2—C4—N1	125.17 (4)	N1—C7'—C6'	100.78
N1—C4—C5	106.17 (4)	N1—C7'—C7	78.87
O2—C4—C5	128.66 (4)	C1—C7'—C1'	9.63
C4—C5—C6'	103.47	C1—C7'—C6	146.91
C6—C5—C6'	11.61	C1—C7'—C6'	140.71
C4—C5—C6	103.47	C1—C7'—C7	83.02
C5—C6—C6'	84.19	C1'—C7'—C6	142.34
C5—C6—C7	109.21	C1'—C7'—C6'	133.99
C5—C6—C7'	112.82	C1'—C7'—C7	73.39
C6'—C6—C7	71.8	C6—C7'—C6'	12.34
C6'—C6—C7'	95.86	C6—C7'—C7	84.14
C7—C6—C7'	24.06	C6'—C7'—C7	71.8
C4—N1—C3—O1	0.00 (4)	C3—N1—C4—O2	0.00 (4)
C4—N1—C3—C2	180.00 (4)	C3—N1—C4—C5	180.00 (4)

Symmetry codes: (i) x, y, z−1; (ii) x, −y+1/2, z−1; (iii) x, −y+1/2, z; (iv) x, −y+1/2, z+1; (v) x, y, z+1; (vi) −x+2, −y+1, −z+1; (vii) −x+2, y−1/2, −z+1; (viii) −x+2, y+1/2, −z+1; (ix) −x+2, −y, −z+1.

(23) Dichloro-(S-methyl beta-N-((2-hydroxyphenyl)ethylidene)dithiocarbazato)-bis (triphenylphosphine)-rhenium(v)

Crystal data

C38H33Cl2N2P2ReS2	γ = 90°
Mr = 900.86	V = 3660.5 (14) Å^3
Monclinic, C2/c	Z = 4
Hall symbol: -C 2yc	F(000) = 1652
a = 17.514 (4) Å	Dx = 1.574 Mg m^−3
b = 10.639 (2) Å	Mo Kα radiation, λ = 0.71070 Å
c = 20.106 (4) Å	µ = 3.70 mm^−1
α = 90°	T = 0 K
β = 102.29 (3)°	× × mm

Data collection

Radiation source: fine-focus sealed tube	θmax = 41.8°, θmin = 2.1°
17044 measured reflections	h = −18→18
4363 independent reflections	k = −11→11
4277 reflections with I > 2σ(I)	l = −20→20
Rint = 0.022

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.049	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.259	w = 1/[σ^2(Fo^2) + (0.2P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.18	(Δ/σ)max = 0.946
4363 reflections	Δρmax = 2.01 e Å^−3
105 parameters	Δρmin = −2.68 e Å^−3
0 restraints	Extinction correction: nne
Primary atom site location: structure-invariant direct methods

Special details

Experimental. Since this work regards a space-group change and the experimental Reflection intensities are nt retained by the original Journal, the calculated Reflection intensities used in this work are obtained following the method reported in:

22 Space-group changes Dore Augusto CLEMENTE and Armando Marzotto Acta Crystallographica Section B (2003) B59, 43–50.

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is nt 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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Re1	0.5	0.22045	0.25	0.02*
Cl1	0.55910	0.4008	0.20727	0.02*
S1	0.45175	0.029	0.28915	0.02*	0.5
S2	0.4803	−0.23605	0.24985	0.02*	0.5
P1	0.4005	0.23975	0.14235	0.02*
N1	0.54705	0.09350	0.2145	0.02*	0.5
N3	0.54470	−0.02250	0.2096	0.02*	0.5
C1	0.5	−0.07550	0.25	0.02*
C2	0.39345	−0.25350	0.2865	0.02*	0.5
C4	0.43975	0.25665	0.0651	0.02*
C5	0.4151	0.34955	0.01795	0.02*
C6	0.4473	0.35930	−0.03940	0.02*
C7	0.50405	0.2761	−0.04945	0.02*
C8	0.52865	0.1832	−0.00225	0.02*
C9	0.4965	0.17345	0.05505	0.02*
C10	0.33485	0.1048	0.12515	0.02*
C11	0.3175	0.0453	0.0623	0.02*
C12	0.26285	−0.05100	0.05055	0.02*
C13	0.22545	−0.08785	0.1017	0.02*
C14	0.2428	−0.02835	0.16455	0.02*
C15	0.29745	0.068	0.17625	0.02*
C16	0.33225	0.37235	0.13845	0.02*
C17	0.36255	0.49205	0.15345	0.02*
C18	0.3125	0.59355	0.15335	0.02*
C19	0.23225	0.57525	0.1382	0.02*
C20	0.20195	0.4555	0.1232	0.02*
C21	0.25195	0.35405	0.1233	0.02*

Geometric parameters (Å, º)

Re1—Cl1	2.4227	C6—C7	1.3776
Re1—S1	2.4012	C7—C8	1.3744
Re1—P1	2.4815	C8—C9	1.3897
Re1—N1	1.8064	C10—C11	1.388
S1—C1	1.6891	C10—C15	1.3872
S2—C1	1.7425	C11—C12	1.3876
S2—C2	1.8353	C12—C13	1.3882
P1—C4	1.8363	C13—C14	1.388
P1—C10	1.8258	C14—C15	1.3879
P1—C16	1.8399	C16—C17	1.3879
N1—N3	1.238	C16—C21	1.3879
N3—C1	1.3643	C17—C18	1.3906
C4—C5	1.3739	C18—C19	1.387
C4—C9	1.3776	C19—C20	1.3884
C5—C6	1.3911	C20—C21	1.3896
Cl1···C17	3.5182	C9···C11	3.4501
Cl1···C17^i	3.0053	C9···S1^i	3.4332
Cl1···C14^ii	3.5824	C11···C9	3.4501
S1···C15	3.1649	C14···Cl1^vii	3.5824
S1···C9^i	3.4332	C15···S1	3.1649
S1···C20^iii	3.6032	C15···C21	3.2663
S2···C18^iv	3.6415	C15···N1^i	3.1255
N1···C9	3.2522	C15···N3^i	3.3371
N1···C15^i	3.1255	C17···Cl1	3.5182
N3···C15^i	3.3371	C17···C5	3.411
C2···C18^iv	3.1952	C17···Cl1^i	3.0053
C2···C7^v	3.4597	C18···S2^viii	3.6415
C2···C20^iii	3.5105	C18···C2^viii	3.1952
C5···C17	3.411	C20···S1^ix	3.6032
C7···C2^vi	3.4597	C20···C2^ix	3.5105
C9···N1	3.2522	C21···C15	3.2663
Cl1—Re1—S1	174.15	S1—C1—N3	114.38
Cl1—Re1—P1	84.2	S1—C1—S1^i	97.67
Cl1—Re1—N1	100.76	S1—C1—S2^i	139.73
Cl1—Re1—Cl1^i	75.26	S1—C1—N3^i	16.88
Cl1—Re1—S1^i	110.42	S2—C1—N3	122.86
Cl1—Re1—P1^i	88.28	S1^i—C1—S2	139.73
Cl1—Re1—N1^i	175.97	S2—C1—S2^i	22.8
S1—Re1—P1	97.2	S2—C1—N3^i	105.53
S1—Re1—N1	73.58	S1^i—C1—N3	16.88
Cl1^i—Re1—S1	110.42	S2^i—C1—N3	105.53
S1—Re1—S1^i	63.95	N3—C1—N3^i	131.18
S1—Re1—P1^i	90.86	S1^i—C1—S2^i	121.84
S1—Re1—N1^i	9.68	S1^i—C1—N3^i	114.38
P1—Re1—N1	90.68	S2^i—C1—N3^i	122.86
Cl1^i—Re1—P1	88.28	P1—C4—C5	122.33
S1^i—Re1—P1	90.86	P1—C4—C9	118.22
P1—Re1—P1^i	170.51	C5—C4—C9	119.44
P1—Re1—N1^i	96.42	C4—C5—C6	120.15
Cl1^i—Re1—N1	175.97	C5—C6—C7	120.41
S1^i—Re1—N1	9.68	C6—C7—C8	119.39
P1^i—Re1—N1	96.42	C7—C8—C9	120.22
N1—Re1—N1^i	83.22	C4—C9—C8	120.39
Cl1^i—Re1—S1^i	174.15	P1—C10—C11	122.55
Cl1^i—Re1—P1^i	84.2	P1—C10—C15	117.34
Cl1^i—Re1—N1^i	100.76	C11—C10—C15	119.95
S1^i—Re1—P1^i	97.2	C10—C11—C12	120.08
S1^i—Re1—N1^i	73.58	C11—C12—C13	119.97
P1^i—Re1—N1^i	90.68	C12—C13—C14	119.95
Re1—S1—C1	99.19	C13—C14—C15	120.04
C1—S2—C2	106.21	C10—C15—C14	120.01
Re1—P1—C4	115.22	P1—C16—C17	118.65
Re1—P1—C10	113.4	P1—C16—C21	121.37
Re1—P1—C16	115.46	C17—C16—C21	119.94
C4—P1—C10	104.53	C16—C17—C18	120.03
C4—P1—C16	104.22	C17—C18—C19	120.02
C10—P1—C16	102.57	C18—C19—C20	119.94
Re1—N1—N3	140.04	C19—C20—C21	120.05
N1—N3—C1	112.22	C16—C21—C20	120.01
S1—C1—S2	121.84
P1—Re1—S1—C1	87.43	C16—P1—C4—C5	−2.57
N1—Re1—S1—C1	−1.16	Re1—P1—C4—C9	49.16
Cl1^i—Re1—S1—C1	178.28	C10—P1—C4—C5	104.74
S1^i—Re1—S1—C1	0	C16—P1—C10—C11	102.6
P1^i—Re1—S1—C1	−97.59	Re1—P1—C16—C17	52.29
N1^i—Re1—S1—C1	173.4	Re1—P1—C10—C11	−132.21
Cl1—Re1—S1^i—C1	178.28	C4—P1—C10—C11	−5.93
S1—Re1—S1^i—C1	0	C10—P1—C16—C17	176.12
P1—Re1—S1^i—C1	−97.59	Re1—P1—C10—C15	52.43
N1—Re1—S1^i—C1	173.4	C10—P1—C4—C9	−75.97
Cl1—Re1—P1—C4	48.23	C16—P1—C4—C9	176.71
S1—Re1—P1—C4	−126.05	C16—P1—C10—C15	−72.77
N1—Re1—P1—C4	−52.52	Re1—P1—C16—C21	−125.41
Cl1^i—Re1—P1—C4	123.59	C4—P1—C16—C17	−75.12
S1^i—Re1—P1—C4	−62.20	C4—P1—C16—C21	107.18
N1^i—Re1—P1—C4	−135.77	C10—P1—C16—C21	−1.58
Cl1—Re1—P1—C10	168.62	C4—P1—C10—C15	178.71
S1—Re1—P1—C10	−5.66	Re1—N1—N3—C1	−10.81
N1—Re1—P1—C10	67.87	N1—N3—C1—S2	175.62
Cl1^i—Re1—P1—C10	−116.02	N1—N3—C1—N3^i	4.35
S1^i—Re1—P1—C10	58.19	N1—N3—C1—S1	6.41
N1^i—Re1—P1—C10	−15.38	N1—N3—C1—S2^i	−168.04
Cl1—Re1—P1—C16	−73.43	N1—N3—C1—S1^i	−2.11
S1—Re1—P1—C16	112.29	C9—C4—C5—C6	−0.02
N1—Re1—P1—C16	−174.18	P1—C4—C5—C6	179.26
Cl1^i—Re1—P1—C16	1.92	C5—C4—C9—C8	0.02
S1^i—Re1—P1—C16	176.14	P1—C4—C9—C8	−179.30
N1^i—Re1—P1—C16	102.57	C4—C5—C6—C7	0.03
Cl1—Re1—N1—N3	−174.10	C5—C6—C7—C8	−0.02
S1—Re1—N1—N3	7.43	C6—C7—C8—C9	0
P1—Re1—N1—N3	−89.88	C7—C8—C9—C4	0
S1^i—Re1—N1—N3	1.24	P1—C10—C11—C12	−175.30
P1^i—Re1—N1—N3	96.43	C11—C10—C15—C14	0.08
N1^i—Re1—N1—N3	6.5	C15—C10—C11—C12	−0.06
Re1—S1—C1—S1^i	0	P1—C10—C15—C14	175.57
Re1—S1—C1—S2	−171.82	C10—C11—C12—C13	0.03
Re1—S1—C1—N3	−2.49	C11—C12—C13—C14	−0.03
Re1—S1^i—C1—S1	0	C12—C13—C14—C15	0.05
Re1—S1—C1—S2^i	169.22	C13—C14—C15—C10	−0.08
Re1—S1—C1—N3^i	172.18	P1—C16—C17—C18	−177.68
Re1—S1^i—C1—S2	169.22	C21—C16—C17—C18	0.05
Re1—S1^i—C1—N3	172.18	P1—C16—C21—C20	177.63
C2—S2—C1—N3	−160.23	C17—C16—C21—C20	−0.04
C2—S2—C1—S1	8.2	C16—C17—C18—C19	−0.06
C2—S2—C1—S2^i	155.37	C17—C18—C19—C20	0.06
C2—S2—C1—S1^i	−159.20	C18—C19—C20—C21	−0.06
C2—S2—C1—N3^i	12.96	C19—C20—C21—C16	0.05
Re1—P1—C4—C5	−130.13

Symmetry codes: (i) −x+1, y, −z+1/2; (ii) x+1/2, y+1/2, z; (iii) −x+1/2, y−1/2, −z+1/2; (iv) x, y−1, z; (v) x, −y, z+1/2; (vi) x, −y, z−1/2; (vii) x−1/2, y−1/2, z; (viii) x, y+1, z; (ix) −x+1/2, y+1/2, −z+1/2.

(25) bis(eta$6!-Benzene)-chromium hydroxide trihydrate

Crystal data

(C12H12Cr^+)·(OH^−)·3(H2O)	Z = 4
Mr = 279.28	F(000) = 560
Orthorhombic, Cmca	Dx = 1.340 Mg m^−3
Hall symbol: -C 2bc 2	Mo K\a radiation, λ = 0.71070 Å
a = 16.409 (3) Å	µ = 0.85 mm^−1
b = 10.506 (4) Å	T = 0 K
c = 7.825 (3) Å	× × mm
V = 1349.0 (8) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cr1	0	0	0	0.02*
C1	0.0429	0.0134	0.25795	0.02*
C3	0.0849	0.10055	0.15615	0.02*
C4	0.043	0.18765	0.05095	0.02*
O1	0.22135	0.3721	0.07305	0.02*
H1	0.07141	−0.04432	0.32537	0.026*
H3	0.14157	0.10118	0.15774	0.026*
H4	0.07169	0.24441	−0.01760	0.026*

Geometric parameters (Å, º)

Cr1—C1	2.1423	C3—C4	1.4099
Cr1—C3	2.133	C4—C4^i	1.4112
Cr1—C4	2.1315	C1—H1	0.93
C1—C3	1.3956	C3—H3	0.93
C1—C1^i	1.4079	C4—H4	0.93
Cr1···H3^i	2.8372	C3···H4^vi	3.036
O1···O1^ii	2.9245	C4···H1^v	3.0139
O1···O1^iii	2.9205	H1···O1^vii	2.7306
O1···O1^iv	2.962	H1···C4^vii	3.0139
O1···H1^v	2.7306	H3···O1^iv	2.8982
O1···H4	2.8869	H4···C3^viii	3.036
O1···H3^iv	2.8982	H4···O1	2.8869
C1—Cr1—C3	38.11	C1^i—Cr1—C3^ix	141.89
C1—Cr1—C4	69.77	C3^ix—Cr1—C3^i	180
C1—Cr1—C1^ix	141.63	C3^ix—Cr1—C4^i	141.39
C1—Cr1—C3^ix	110.96	C1^x—Cr1—C4^ix	82.63
C1—Cr1—C4^ix	97.37	C3^x—Cr1—C4^ix	69.57
C1—Cr1—C1^x	180	C4^ix—Cr1—C4^x	38.66
C1—Cr1—C3^x	141.89	C1^i—Cr1—C4^ix	110.23
C1—Cr1—C4^x	110.23	C3^i—Cr1—C4^ix	141.39
C1—Cr1—C1^i	38.37	C4^ix—Cr1—C4^i	180
C1—Cr1—C3^i	69.04	C1^x—Cr1—C3^x	38.11
C1—Cr1—C4^i	82.63	C1^x—Cr1—C4^x	69.77
C3—Cr1—C4	38.61	C1^x—Cr1—C1^i	141.63
C1^ix—Cr1—C3	110.96	C1^x—Cr1—C3^i	110.96
C3—Cr1—C3^ix	98.44	C1^x—Cr1—C4^i	97.37
C3—Cr1—C4^ix	110.43	C3^x—Cr1—C4^x	38.61
C1^x—Cr1—C3	141.89	C1^i—Cr1—C3^x	110.96
C3—Cr1—C3^x	180	C3^x—Cr1—C3^i	98.44
C3—Cr1—C4^x	141.39	C3^x—Cr1—C4^i	110.43
C1^i—Cr1—C3	69.04	C1^i—Cr1—C4^x	97.37
C3—Cr1—C3^i	81.56	C3^i—Cr1—C4^x	110.43
C3—Cr1—C4^i	69.57	C4^x—Cr1—C4^i	141.34
C1^ix—Cr1—C4	97.37	C1^i—Cr1—C3^i	38.11
C3^ix—Cr1—C4	110.43	C1^i—Cr1—C4^i	69.77
C4—Cr1—C4^ix	141.34	C3^i—Cr1—C4^i	38.61
C1^x—Cr1—C4	110.23	Cr1—C1—C3	70.59
C3^x—Cr1—C4	141.39	Cr1—C1—C1^i	70.82
C4—Cr1—C4^x	180	C1^i—C1—C3	119.59
C1^i—Cr1—C4	82.63	Cr1—C3—C1	71.31
C3^i—Cr1—C4	69.57	Cr1—C3—C4	70.64
C4—Cr1—C4^i	38.66	C1—C3—C4	121.21
C1^ix—Cr1—C3^ix	38.11	Cr1—C4—C3	70.75
C1^ix—Cr1—C4^ix	69.77	Cr1—C4—C4^i	70.67
C1^ix—Cr1—C1^x	38.37	C3—C4—C4^i	119.19
C1^ix—Cr1—C3^x	69.04	Cr1—C1—H1	131.07
C1^ix—Cr1—C4^x	82.63	C3—C1—H1	120.2
C1^ix—Cr1—C1^i	180	C1^i—C1—H1	120.2
C1^ix—Cr1—C3^i	141.89	Cr1—C3—H3	131.62
C1^ix—Cr1—C4^i	110.23	C1—C3—H3	119.39
C3^ix—Cr1—C4^ix	38.61	C4—C3—H3	119.39
C1^x—Cr1—C3^ix	69.04	Cr1—C4—H4	130.74
C3^ix—Cr1—C3^x	81.56	C3—C4—H4	120.41
C3^ix—Cr1—C4^x	69.57	C4^i—C4—H4	120.41
C4—Cr1—C1—C3	−28.41	C1—Cr1—C3—C4	−134.33
C1^ix—Cr1—C1—C3	47.39	C1^ix—Cr1—C3—C4	74.96
C3^ix—Cr1—C1—C3	76.49	C3^ix—Cr1—C3—C4	112.3
C4^ix—Cr1—C1—C3	113.92	C4^ix—Cr1—C3—C4	150.33
C3^x—Cr1—C1—C3	179.98	C1^x—Cr1—C3—C4	45.67
C4^x—Cr1—C1—C3	151.59	C4^x—Cr1—C3—C4	180
C1^i—Cr1—C1—C3	−132.61	C1^i—Cr1—C3—C4	−105.04
C3^i—Cr1—C1—C3	−103.51	C3^i—Cr1—C3—C4	−67.70
C4^i—Cr1—C1—C3	−66.08	C4^i—Cr1—C3—C4	−29.67
C3—Cr1—C1—C1^i	132.61	C1^x—Cr1—C4—C3	−151.94
C4—Cr1—C1—C1^i	104.2	C1^ix—Cr1—C4—C3	−114.58
C3^x—Cr1—C4—C3	180	C3^ix—Cr1—C4—C3	−77.57
C1^i—Cr1—C4—C3	65.42	C1—Cr1—C4—C3	28.06
C3^i—Cr1—C4—C3	102.43	C3—Cr1—C4—C4^i	−132.06
C4^i—Cr1—C4—C3	132.06	C4^ix—Cr1—C4—C3	−47.94
C1—Cr1—C4—C4^i	−104.00	C1^i—C1—C3—C4	−0.97
C4—Cr1—C3—C1	134.33	C3—C1—C1^i—C3^i	0
C1^ix—Cr1—C3—C1	−150.71	Cr1—C1—C3—C4	52.1
C3^ix—Cr1—C3—C1	−113.37	C3—C1—C1^i—Cr1	52.97
C4^ix—Cr1—C3—C1	−75.34	C1^i—C1—C3—Cr1	−53.07
C1^x—Cr1—C3—C1	179.98	C1—C3—C4—Cr1	−52.40
C4^x—Cr1—C3—C1	−45.67	C1—C3—C4—C4^i	0.97
C1^i—Cr1—C3—C1	29.29	Cr1—C3—C4—C4^i	53.37
C3^i—Cr1—C3—C1	66.63	C3—C4—C4^i—Cr1	−53.41
C4^i—Cr1—C3—C1	104.66	C3—C4—C4^i—C3^i	0

Symmetry codes: (i) −x, y, z; (ii) −x+1/2, y, −z+1/2; (iii) x, −y+1, −z; (iv) −x+1/2, −y+1/2, −z; (v) x, y+1/2, −z+1/2; (vi) x, −y+1/2, z+1/2; (vii) x, y−1/2, −z+1/2; (viii) x, −y+1/2, z−1/2; (ix) x, −y, −z; (x) −x, −y, −z.

(26) mer,trans-Trichloro-phenylimido-bis(trimethylphosphine)-rhenium

Crystal data

C12H23Cl3NP2Re	Z = 4
Mr = 535.80	F(000) = 940
Orthorhombic, Cmcm	Dx = 1.692 Mg m^−3
Hall symbol: -C 2c 2	Mo K\a radiation, λ = 0.71073 Å
a = 11.0341 (10) Å	µ = 6.58 mm^−1
b = 16.814 (2) Å	T = 0 K
c = 10.844 (1) Å	× × mm
V = 2011.9 (4) Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Re1	0.5	0.3032	0.25	0.02*
Cl1	0.28155	0.31015	0.25	0.02*
Cl3	0.5	0.4478	0.25	0.02*
P1	0.5	0.3209	0.02735	0.02*
N1	0.5	0.2024	0.25	0.02*
C1	0.5	0.11915	0.25	0.02*
C2	0.39255	0.0779	0.25	0.02*
C3	0.3911	0.00005	0.25	0.02*
C4	0.5	−0.04080	0.25	0.02*
C7	0.5	0.2267	−0.05155	0.02*
C8	0.62874	0.37418	−0.03657	0.02*

Geometric parameters (Å, º)

Re1—Cl1	2.4132 (3)	P1—C8	1.8168
Re1—Cl3	2.4313 (3)	N1—C1	1.3998 (2)
Re1—P1	2.4327 (3)	C1—C2	1.3736 (2)
Re1—N1	1.6949 (2)	C1—C2^i	1.3736 (2)
Re1—Cl1^i	2.4132 (3)	C2—C3	1.3091 (2)
Re1—P1^i	2.4327 (3)	C3—C4	1.3841 (2)
P1—C7	1.8002 (2)
Cl1—Re1—Cl3	87.22	Cl1^i—Re1—P1^i	89.66
Cl1—Re1—P1	89.66	Re1—P1—C7	111.35
Cl1—Re1—N1	92.78	Re1—P1—C8	116.04
Cl1—Re1—Cl1^i	174.45	Re1—P1—C8^ii	116.04
Cl1—Re1—P1^i	89.66	C7—P1—C8	104.63
Cl3—Re1—P1	82.97	C7—P1—C8^ii	104.63
Cl3—Re1—N1	180	C8—P1—C8^ii	102.86
Cl1^i—Re1—Cl3	87.22	Re1—N1—C1	180
Cl3—Re1—P1^i	82.97	N1—C1—C2	120.33
P1—Re1—N1	97.03	N1—C1—C2^i	120.33
Cl1^i—Re1—P1	89.66	C2—C1—C2^i	119.35
P1—Re1—P1^i	165.95	C1—C2—C3	121.03
Cl1^i—Re1—N1	92.78	C2—C3—C4	119.05
P1^i—Re1—N1	97.03	C3—C4—C3^i	120.49
Cl1—Re1—P1—C7	−92.75	Cl3—Re1—P1—C8	60.48
Cl3—Re1—P1—C7	180	N1—Re1—P1—C8	−119.52
N1—Re1—P1—C7	0	N1—C1—C2—C3	180
Cl1—Re1—P1—C8	147.73	C1—C2—C3—C4	0

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

(27) mu!3$-eta$4!,eta$4!-Buta-1,3-dien-1,4-diyl)-(mu!2$-hydrido)-tris (eta$4!-cyclo-octa-1,5-diene)-tri-iridium

Crystal data

C12H13Ir3	Z = 4
Mr = 733.88	F(000) = 1212
Orthorhombic, Cmcm	Dx = 1.684 Mg m^−3
Hall symbol: -C 2c 2	Mo K\a radiation, λ = 0.71073 Å
a = 11.2624 Å	µ = 13.99 mm^−1
b = 9.711 Å	T = 0 K
c = 25.998 Å	× × mm
V = 2843.38 Å^3

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ir1	0	0.2933	0.25	0.02*
Ir2	0	0.0937	0.3243	0.02*
C1	−0.06657	−0.00873	0.25	0.02*
C2	−0.11713	0.12718	0.25	0.02*
C5	0.12583	0.44973	0.22328	0.02*
C6	0.0718	0.55247	0.18465	0.02*

Geometric parameters (Å, º)

Ir1—C2	2.0839	Ir2—C2^i	2.3616
Ir1—C5	2.1905	C1—C2	1.4374
Ir1—C2^i	2.0839	C1—C1^i	1.4995
Ir2—C1	2.2984	C5—C6	1.5409
Ir2—C2	2.3616	C5—C5^ii	1.3893
Ir2—C1^i	2.2984	C6—C6^iii	1.6173
C1···C5^iv	3.5562	C5···C1^vi	3.5562
C1···C5^v	3.5562	C5···C2^vi	3.4398
C2···C5^iv	3.4398	C5···C1^vii	3.5562
C2···C5^v	3.4398	C5···C2^vii	3.4398
C2—Ir1—C5	161.15	C2—Ir2—C2^i	67.92
C2—Ir1—C2^i	78.55	C1^i—Ir2—C2^i	35.9
C2—Ir1—C5^i	97.31	Ir2—C1—C2	74.45
C2—Ir1—C5^ii	161.15	Ir2—C1—Ir2^i	114.37
C2—Ir1—C5^iii	97.31	Ir2—C1—C1^i	70.96
C2^i—Ir1—C5	97.31	Ir2^i—C1—C2	74.45
C5—Ir1—C5^i	92.19	C1^i—C1—C2	113.34
C5—Ir1—C5^ii	36.98	Ir2^i—C1—C1^i	70.96
C5—Ir1—C5^iii	80.62	Ir1—C2—Ir2	75.7
C2^i—Ir1—C5^i	161.15	Ir1—C2—C1	117.39
C2^i—Ir1—C5^ii	97.31	Ir1—C2—Ir2^i	75.7
C2^i—Ir1—C5^iii	161.15	Ir2—C2—C1	69.65
C5^i—Ir1—C5^ii	80.62	Ir2—C2—Ir2^i	109.76
C5^i—Ir1—C5^iii	36.98	Ir2^i—C2—C1	69.65
C5^ii—Ir1—C5^iii	92.19	Ir1—C5—C6	113.59
C1—Ir2—C2	35.9	Ir1—C5—C5^ii	71.51
C1—Ir2—C1^i	38.08	C5^ii—C5—C6	130.68
C1—Ir2—C2^i	63.54	C5—C6—C6^iii	113.26
C1^i—Ir2—C2	63.54
C5^i—Ir1—C5—C6	−55.92	Ir1—C5—C6—C6^iii	17.04
C5^ii—Ir1—C5—C6	−127.15	C5^ii—C5—C6—C6^iii	−68.32
C2^i—Ir1—C5—C6	140.39	C6—C5—C5^ii—Ir1	105.61
C5^iii—Ir1—C5—C6	−20.67	C6—C5—C5^ii—C6^ii	0
C1—Ir2—C2—Ir1	−126.93	C5—C6—C6^iii—C5^iii	0
Ir2—C1—C2—Ir1	60.73

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

(28) bis(1,4-Dimethyl-9-triptycyl)ethyne chloroform solvate

Crystal data

C46H34·2(CHCl3)	γ = 90°
Mr = 825.47	V = 2040.4 (6) Å^3
Monclinic, P21/n	Z = 2
Hall symbol: -P 2yn	F(000) = 780
a = 15.592 (2) Å	Dx = 1.285 Mg m^−3
b = 8.642 (2) Å	Mo K\a radiation, λ = 0.71070 Å
c = 16.677 (2) Å	µ = 0.45 mm^−1
α = 90°	T = 0 K
β = 114.773 (9)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.0058	1.142	0.20020	0.02*
C3	0.00925	1.19650	0.2804	0.02*
C5	0.0084	1.1005	0.3457	0.02*
C7	0.0039	0.9415	0.33505	0.02*
C8	0.0018	0.8845	0.2561	0.02*
C11	0.15890	0.583	0.25655	0.02*
C13	0.23125	0.5735	0.2293	0.02*
C15	0.2303	0.6635	0.161	0.02*
C17	0.157	0.767	0.11865	0.02*
C18	0.085	0.77750	0.14615	0.02*
C21	−0.00055	0.889	0.1086	0.02*
C22	0.00165	0.9825	0.18915	0.02*
C25	−0.00005	0.7125	0.2345	0.02*
C26	0.08555	0.68550	0.21425	0.02*
C29	−0.08670	0.6875	0.1487	0.02*
C31	−0.08775	0.782	0.08055	0.02*
C33	−0.16145	0.773	−0.00230	0.02*
C35	−0.23420	0.6675	−0.01735	0.02*
C37	−0.23295	0.575	0.05025	0.02*
C39	−0.15900	0.5845	0.1341	0.02*
C41	0.00480	1.2595	0.1336	0.02*
C43	0.0013	0.8375	0.4064	0.02*
C45	−0.00060	0.975	0.03295	0.02*
Cl1	0.2107	0.3817	0.5223	0.02*	0.5
Cl2	0.16785	0.40005	0.49865	0.02*	0.5
Cl4	0.11555	0.5714	0.59945	0.02*	0.5
Cl5	0.1215	0.59745	0.61725	0.02*	0.5
Cl7	0.25745	0.3362	0.68585	0.02*	0.5
Cl8	0.2665	0.38545	0.68825	0.02*	0.5
C47	0.2133	0.48575	0.59875	0.02*	0.5
C48	0.221	0.49565	0.60495	0.02*	0.5

Geometric parameters (Å, º)

Cl1—C48	1.6462	C8—C22	1.4006
Cl1—C47	1.5467	C8—C25	1.5269
Cl1—Cl2	0.6374	C11—C26	1.3835
Cl2—C47	1.687	C11—C13	1.384
Cl2—C48	1.8113	C13—C15	1.3742
Cl4—Cl5	0.3526	C15—C17	1.3887
Cl4—C47	1.6988	C17—C18	1.3821
Cl4—C48	1.7361	C18—C21	1.5492
Cl5—C47	1.8563	C18—C26	1.3834
Cl5—C48	1.868	C21—C22	1.5556
Cl7—C48	1.8438	C21—C31	1.5458
Cl7—Cl8	0.4449	C21—C45	1.464
Cl7—C47	1.8483	C25—C26	1.5256
Cl8—C47	1.6216	C25—C29	1.5164
Cl8—C48	1.5856	C29—C31	1.394
C1—C41	1.5002	C29—C39	1.3756
C1—C3	1.3976	C31—C33	1.3802
C1—C22	1.3886	C33—C35	1.3937
C3—C5	1.3735	C35—C37	1.3755
C5—C7	1.3835	C37—C39	1.393
C7—C43	1.5052	C45—C45^i	1.1883
C7—C8	1.3933	C47—C48	0.1484
Cl5···C3^ii	3.6272	C13···C17^v	3.5748
Cl5···C5^ii	3.5138	C17···C45^i	3.4847
Cl7···C3^iii	3.5766	C17···C13^vi	3.5748
Cl8···C3^iii	3.5092	C33···C45^i	3.5314
Cl8···C5^iii	3.5827	C41···C45	2.9582
C3···Cl5^ii	3.6272	C41···C45^i	3.4167
C3···Cl7^iv	3.5766	C45···C33^i	3.5314
C3···Cl8^iv	3.5092	C45···C41^i	3.4167
C5···Cl8^iv	3.5827	C45···C41	2.9582
C5···Cl5^ii	3.5138	C45···C17^i	3.4847
C47—Cl1—C48	3.96	C25—C29—C39	126.82
Cl2—Cl1—C48	94.5	C31—C29—C39	120.4
Cl2—Cl1—C47	91.38	C21—C31—C29	113.29
Cl1—Cl2—C48	64.96	C21—C31—C33	126.47
Cl1—Cl2—C47	66.43	C29—C31—C33	120.24
C47—Cl2—C48	2.66	C31—C33—C35	119.38
Cl5—Cl4—C48	106.68	C33—C35—C37	120.11
Cl5—Cl4—C47	111.33	C35—C37—C39	120.67
C47—Cl4—C48	4.79	C29—C39—C37	119.21
Cl4—Cl5—C48	62.9	C21—C45—C45^i	170.78
C47—Cl5—C48	4.55	Cl1—C47—Cl2	22.19
Cl4—Cl5—C47	58.48	Cl1—C47—Cl4	123.04
C47—Cl7—C48	4.6	Cl1—C47—Cl5	133.13
Cl8—Cl7—C47	53.23	Cl1—C47—Cl7	96.53
Cl8—Cl7—C48	48.68	Cl1—C47—Cl8	105.94
C47—Cl8—C48	5.15	Cl1—C47—C48	130.06
Cl7—Cl8—C48	119.15	Cl2—C47—Cl4	101.07
Cl7—Cl8—C47	114.07	Cl2—C47—Cl5	111.06
C22—C1—C41	126.03	Cl2—C47—Cl7	109.54
C3—C1—C41	117.69	Cl2—C47—Cl8	121.12
C3—C1—C22	116.26	Cl2—C47—C48	145.52
C1—C3—C5	123.09	Cl4—C47—Cl5	10.19
C3—C5—C7	120.99	Cl4—C47—Cl7	109.82
C5—C7—C8	116.89	Cl4—C47—Cl8	109.93
C5—C7—C43	120.55	Cl4—C47—C48	102.14
C8—C7—C43	122.56	Cl5—C47—Cl7	106.99
C7—C8—C25	123.9	Cl5—C47—Cl8	104.93
C7—C8—C22	122.08	Cl5—C47—C48	92.26
C22—C8—C25	114.02	Cl7—C47—Cl8	12.7
C13—C11—C26	118.94	Cl7—C47—C48	85.95
C11—C13—C15	120.76	Cl8—C47—C48	73.4
C13—C15—C17	120.45	Cl1—C48—Cl2	20.54
C15—C17—C18	118.9	Cl1—C48—Cl4	115.05
C17—C18—C26	120.54	Cl1—C48—Cl5	125.42
C21—C18—C26	113.42	Cl1—C48—Cl7	93.3
C17—C18—C21	126.03	Cl1—C48—Cl8	103.01
C18—C21—C45	110.71	Cl1—C48—C47	45.98
C18—C21—C22	105.68	Cl2—C48—Cl4	94.91
C18—C21—C31	104.44	Cl2—C48—Cl5	105.18
C31—C21—C45	111.11	Cl2—C48—Cl7	104.45
C22—C21—C31	105.69	Cl2—C48—Cl8	115.9
C22—C21—C45	118.19	Cl2—C48—C47	31.82
C1—C22—C8	120.67	Cl4—C48—Cl5	10.42
C1—C22—C21	127.82	Cl4—C48—Cl7	108.37
C8—C22—C21	111.49	Cl4—C48—Cl8	109.81
C8—C25—C26	105.62	Cl4—C48—C47	73.07
C26—C25—C29	106.59	Cl5—C48—Cl7	106.69
C8—C25—C29	106.42	Cl5—C48—Cl8	105.9
C18—C26—C25	112.88	Cl5—C48—C47	83.19
C11—C26—C18	120.4	Cl7—C48—Cl8	12.16
C11—C26—C25	126.73	Cl7—C48—C47	89.44
C25—C29—C31	112.79	Cl8—C48—C47	101.45
Cl2—Cl1—C47—Cl5	6.93	Cl7—Cl8—C48—C47	9.39
C48—Cl1—C47—Cl5	149.12	C47—Cl8—C48—Cl1	−47.09
Cl2—Cl1—C47—Cl7	127.61	Cl7—Cl8—C48—Cl2	−20.68
C48—Cl1—C47—Cl7	−90.20	C47—Cl8—C48—Cl4	75.95
Cl2—Cl1—C47—Cl8	136.32	Cl7—Cl8—C48—Cl5	95.48
C48—Cl1—C47—Cl8	−81.49	C47—Cl8—C48—Cl5	86.09
C47—Cl1—Cl2—C48	2.43	C47—Cl8—C48—Cl7	−9.39
C48—Cl1—Cl2—C47	−2.43	Cl7—Cl8—C48—Cl1	−37.69
Cl2—Cl1—C48—Cl4	11.91	Cl7—Cl8—C48—Cl4	85.34
C47—Cl1—C48—Cl4	−26.03	Cl7—Cl8—C47—Cl1	−43.19
Cl2—Cl1—C48—Cl5	10.76	C47—Cl8—C48—Cl2	−30.07
C47—Cl1—C48—Cl5	−27.18	Cl7—Cl8—C47—C48	−171.02
C48—Cl1—C47—Cl2	142.19	C48—Cl8—C47—Cl1	127.83
Cl2—Cl1—C47—Cl4	8.82	C41—C1—C22—C8	−179.11
C48—Cl1—C47—Cl4	151.01	C3—C1—C22—C21	−178.53
Cl2—Cl1—C48—Cl8	131.38	C41—C1—C3—C5	178.53
C47—Cl1—C48—Cl8	93.44	C3—C1—C22—C8	−0.50
Cl2—Cl1—C48—C47	37.94	C22—C1—C3—C5	−0.19
Cl2—Cl1—C47—C48	−142.19	C41—C1—C22—C21	2.86
C47—Cl1—C48—Cl7	86.03	C1—C3—C5—C7	−0.06
C47—Cl1—C48—Cl2	−37.94	C3—C5—C7—C43	−178.93
Cl2—Cl1—C48—Cl7	123.96	C3—C5—C7—C8	0.97
C47—Cl2—C48—Cl1	123.02	C43—C7—C8—C25	−2.08
C47—Cl2—C48—Cl4	−46.16	C43—C7—C8—C22	178.22
C48—Cl2—C47—Cl4	131.55	C5—C7—C8—C22	−1.68
Cl1—Cl2—C48—Cl4	−169.18	C5—C7—C8—C25	178.02
C48—Cl2—C47—Cl5	129.44	C22—C8—C25—C29	−56.44
Cl1—Cl2—C47—Cl7	−56.62	C7—C8—C22—C1	1.48
Cl1—Cl2—C47—Cl5	−174.58	C25—C8—C22—C1	−178.24
C48—Cl2—C47—Cl1	−55.98	C25—C8—C22—C21	0.08
Cl1—Cl2—C47—C48	55.98	C7—C8—C22—C21	179.81
Cl1—Cl2—C47—Cl4	−172.47	C22—C8—C25—C26	56.6
C47—Cl2—C48—Cl7	64.25	C7—C8—C25—C29	123.84
Cl1—Cl2—C48—Cl8	−54.36	C7—C8—C25—C26	−123.12
C47—Cl2—C48—Cl8	68.66	C13—C11—C26—C25	179.95
Cl1—Cl2—C48—C47	−123.02	C13—C11—C26—C18	−0.36
Cl1—Cl2—C48—Cl5	−170.93	C26—C11—C13—C15	−0.39
C47—Cl2—C48—Cl5	−47.91	C11—C13—C15—C17	0.68
C48—Cl2—C47—Cl8	−106.85	C13—C15—C17—C18	−0.22
Cl1—Cl2—C48—Cl7	−58.77	C15—C17—C18—C26	−0.53
C48—Cl2—C47—Cl7	−112.60	C15—C17—C18—C21	178.21
Cl1—Cl2—C47—Cl8	−50.87	C21—C18—C26—C25	1.67
C48—Cl4—C47—Cl5	14.48	C17—C18—C21—C22	−123.93
C47—Cl4—C48—Cl8	−96.37	C17—C18—C21—C45	5.17
Cl5—Cl4—C48—C47	165.93	C26—C18—C21—C22	54.89
C47—Cl4—C48—Cl7	−83.58	C17—C18—C21—C31	124.83
Cl5—Cl4—C48—Cl8	69.56	C21—C18—C26—C11	−178.06
Cl5—Cl4—C47—Cl1	−172.18	C17—C18—C26—C11	0.82
C48—Cl4—C47—Cl1	−157.70	C17—C18—C26—C25	−179.45
Cl5—Cl4—C47—Cl2	−168.80	C26—C18—C21—C31	−56.35
C48—Cl4—C47—Cl2	−154.32	C26—C18—C21—C45	−176.02
Cl5—Cl4—C48—Cl1	−174.81	C18—C21—C31—C29	55.29
Cl5—Cl4—C47—Cl7	75.57	C45—C21—C22—C1	−1.60
Cl5—Cl4—C48—Cl7	82.35	C45—C21—C22—C8	−179.77
C47—Cl4—Cl5—C48	1.25	C31—C21—C22—C1	−126.69
C48—Cl4—Cl5—C47	−1.25	C31—C21—C22—C8	55.14
C48—Cl4—C47—Cl8	76.54	C45—C21—C31—C33	−4.66
Cl5—Cl4—C47—C48	−14.48	C22—C21—C31—C29	−55.95
C47—Cl4—C48—Cl2	23.43	C22—C21—C31—C33	124.71
C47—Cl4—C48—Cl1	19.26	C18—C21—C31—C33	−124.05
Cl5—Cl4—C48—Cl2	−170.64	C18—C21—C22—C8	−55.23
Cl5—Cl4—C47—Cl8	62.06	C45—C21—C31—C29	174.68
C47—Cl4—C48—Cl5	−165.93	C18—C21—C22—C1	122.95
C48—Cl4—C47—Cl7	90.04	C29—C25—C26—C11	−124.81
Cl4—Cl5—C48—Cl1	5.77	C8—C25—C26—C18	−57.44
C48—Cl5—C47—Cl7	86.46	C26—C25—C29—C39	123.08
Cl4—Cl5—C47—Cl8	−120.73	C8—C25—C26—C11	122.27
C48—Cl5—C47—Cl8	73.42	C29—C25—C26—C18	55.48
Cl4—Cl5—C47—C48	165.84	C8—C25—C29—C39	−124.54
Cl4—Cl5—C48—Cl8	−113.56	C26—C25—C29—C31	−56.40
Cl4—Cl5—C48—C47	−13.55	C8—C25—C29—C31	55.98
Cl4—Cl5—C47—Cl7	−107.70	C25—C29—C31—C33	179.51
Cl4—Cl5—C48—Cl7	−100.91	C25—C29—C31—C21	0.12
C47—Cl5—C48—Cl7	−87.36	C39—C29—C31—C33	0
Cl4—Cl5—C47—Cl1	8.99	C39—C29—C31—C21	−179.40
C48—Cl5—C47—Cl1	−156.85	C31—C29—C39—C37	0.44
C48—Cl5—C47—Cl4	−165.84	C25—C29—C39—C37	−179.01
C47—Cl5—C48—Cl8	−100.01	C21—C31—C33—C35	178.63
C48—Cl5—C47—Cl2	−154.05	C29—C31—C33—C35	−0.66
C47—Cl5—C48—Cl4	13.55	C31—C33—C35—C37	0.92
Cl4—Cl5—C48—Cl2	9.66	C33—C35—C37—C39	−0.50
C47—Cl5—C48—Cl2	23.21	C35—C37—C39—C29	−0.18
Cl4—Cl5—C47—Cl2	11.79	Cl8—C47—C48—Cl7	1.97
C47—Cl5—C48—Cl1	19.32	Cl8—C47—C48—Cl4	−107.45
Cl8—Cl7—C48—Cl4	−98.86	Cl8—C47—C48—Cl5	−104.91
C47—Cl7—C48—Cl4	71.94	Cl1—C47—C48—Cl2	24.14
C47—Cl7—C48—Cl2	−28.36	Cl1—C47—C48—Cl4	155.45
Cl8—Cl7—C48—Cl1	143.36	Cl1—C47—C48—Cl5	157.98
C47—Cl7—C48—Cl1	−45.84	Cl1—C47—C48—Cl7	−95.14
Cl8—Cl7—C48—Cl2	160.85	Cl1—C47—C48—Cl8	−97.11
Cl8—Cl7—C47—Cl5	−82.50	Cl2—C47—C48—Cl1	−24.14
C48—Cl7—C47—Cl5	−91.13	Cl2—C47—C48—Cl4	131.3
Cl8—Cl7—C48—Cl5	−88.08	Cl2—C47—C48—Cl5	133.84
Cl8—Cl7—C47—C48	8.63	Cl2—C47—C48—Cl7	−119.28
C47—Cl7—C48—Cl5	82.72	Cl2—C47—C48—Cl8	−121.25
C47—Cl7—C48—Cl8	170.8	Cl4—C47—C48—Cl1	−155.45
Cl8—Cl7—C48—C47	−170.80	Cl4—C47—C48—Cl2	−131.30
C48—Cl7—C47—Cl4	−101.45	Cl4—C47—C48—Cl5	2.54
C47—Cl7—Cl8—C48	−0.92	Cl4—C47—C48—Cl7	109.42
C48—Cl7—Cl8—C47	0.92	Cl4—C47—C48—Cl8	107.45
Cl8—Cl7—C47—Cl1	138.52	Cl5—C47—C48—Cl1	−157.98
C48—Cl7—C47—Cl2	148.4	Cl5—C47—C48—Cl2	−133.84
C48—Cl7—C47—Cl1	129.89	Cl5—C47—C48—Cl4	−2.54
Cl8—Cl7—C47—Cl2	157.03	Cl5—C47—C48—Cl7	106.88
C48—Cl7—C47—Cl8	−8.63	Cl5—C47—C48—Cl8	104.91
Cl8—Cl7—C47—Cl4	−92.83	Cl7—C47—C48—Cl1	95.14
C48—Cl8—C47—Cl7	171.02	Cl7—C47—C48—Cl2	119.28
C48—Cl8—C47—Cl2	145.57	Cl7—C47—C48—Cl4	−109.42
Cl7—Cl8—C47—Cl2	−25.45	Cl7—C47—C48—Cl5	−106.88
Cl7—Cl8—C47—Cl4	91.78	Cl7—C47—C48—Cl8	−1.97
C48—Cl8—C47—Cl4	−97.20	Cl8—C47—C48—Cl1	97.11
Cl7—Cl8—C47—Cl5	101.09	Cl8—C47—C48—Cl2	121.25
C48—Cl8—C47—Cl5	−87.89

Symmetry codes: (i) −x, −y+2, −z; (ii) −x, −y+2, −z+1; (iii) x+1/2, −y+3/2, z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) −x+1/2, y−1/2, −z+1/2; (vi) −x+1/2, y+1/2, −z+1/2.

(29) tris(1,2-Di-imidobenzene)-technetium(vii) pertechnetate

Crystal data

C18H18N6Tc^+·O4Tc^−	Z = 4
Mr = 580.20	F(000) = 944
Orthorhombic, Pnna	Dx = 1.718 Mg m^−3
Hall symbol: -P 2a 2bc	Mo Kα radiation, λ = 0.71070 Å
a = 13.869 (4) Å	µ = 1.45 mm^−1
b = 10.851 (3) Å	T = 293 K
c = 12.799 (5) Å	× × mm
V = 1926.2 (11) Å^3

Data collection

Radiation source: fine-focus sealed tube	θmax = 40.0°, θmin = 2.2°
18522 measured reflections	h = −14→14
2456 independent reflections	k = −12→12
2454 reflections with I > 2σ(I)	l = −13→13
Rint = 0.003

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.122	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.606	w = 1/[σ^2(Fo^2) + (0.2P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 3.25	(Δ/σ)max = 0.551
2456 reflections	Δρmax = 1.20 e Å^−3
52 parameters	Δρmin = −3.52 e Å^−3
0 restraints	Extinction correction: nne
Primary atom site location: structure-invariant direct methods

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is nt 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 (Ų)

	x	y	z	Uiso*/Ueq
Tc1	0.5069	0.75	0.25	0.02*
N1	0.45455	0.717	0.10655	0.02*
N2	0.4453	0.583	0.26345	0.02*
N5	0.62105	0.82545	0.17815	0.02*
C1	0.4178	0.6039	0.08625	0.02*
C2	0.3876	0.5574	−0.01130	0.02*
C3	0.35385	0.4435	−0.02180	0.02*
C4	0.344	0.3623	0.0721	0.02*
C5	0.3737	0.4057	0.16965	0.02*
C6	0.4116	0.53015	0.1766	0.02*
C13	0.7108	0.79425	0.207	0.02*
C14	0.7985	0.83635	0.16865	0.02*
C15	0.8846	0.7941	0.20855	0.02*
Tc2	0	0	0	0.02*

Geometric parameters (Å, º)

Tc1—N1	2.0066	C2—C3	1.3284
Tc1—N2	2.0108	C3—C4	1.4965
Tc1—N5	2.0056	C4—C5	1.3965
N1—C1	1.354	C5—C6	1.4518
N2—C6	1.3353	C13—C14	1.3889
N5—C13	1.3418	C13—C13^i	1.4607
C1—C2	1.4103	C14—C15	1.3773
C1—C6	1.4089	C15—C15^i	1.4289
Tc1···Tc2^ii	4.1960 (16)	N1···C3^x	3.3572
Tc1···Tc2^iii	4.1960 (16)	N2···Tc2^iii	3.2485
Tc1···Tc2^iv	4.1960 (16)	N2···Tc2^v	3.2485
Tc1···Tc2^v	4.1960 (16)	N5···Tc2^iv	3.4066
Tc2···Tc1^vi	4.1960 (16)	N5···Tc2^ii	3.4066
Tc2···N1^vi	3.4186	C1···C2^x	3.3567
Tc2···N5^vi	3.4066	C1···C3^x	3.3128
Tc2···Tc1^vii	4.1960 (16)	C2···C3^ii	3.3514
Tc2···N2^vii	3.2485	C2···C2^x	3.3698
Tc2···Tc1^viii	4.1960 (16)	C2···C4^ii	3.4951
Tc2···N2^viii	3.2485	C2···C1^x	3.3567
Tc2···C14^ix	3.9525	C3···C2^ii	3.3514
Tc2···C15^ix	3.8312	C3···C1^x	3.3128
Tc2···Tc1^ii	4.1960 (16)	C3···C3^ii	3.1307
Tc2···N1^ii	3.4186	C3···N1^x	3.3572
Tc2···N5^ii	3.4066	C4···C2^ii	3.4951
Tc2···C15^x	3.8312	C14···Tc2^x	3.9525
Tc2···C14^x	3.9525	C14···Tc2^xi	3.9525
N1···Tc2^ii	3.4186	C15···Tc2^x	3.8312
N1···Tc2^iv	3.4186	C15···Tc2^xi	3.8312
N1—Tc1—N2	76.34	Tc1—N5—C13	120.21
N1—Tc1—N5	86.5	N1—C1—C2	127.3
N1—Tc1—N1^i	137.57	N1—C1—C6	112.35
N1—Tc1—N2^i	85.91	C2—C1—C6	120.35
N1—Tc1—N5^i	129.22	C1—C2—C3	121.81
N2—Tc1—N5	137.95	C2—C3—C4	119.92
N1^i—Tc1—N2	85.91	C3—C4—C5	119.51
N2—Tc1—N2^i	129.71	C4—C5—C6	118.37
N2—Tc1—N5^i	85.89	N2—C6—C1	114.71
N1^i—Tc1—N5	129.22	N2—C6—C5	125.25
N2^i—Tc1—N5	85.89	C1—C6—C5	120.01
N5—Tc1—N5^i	75.75	N5—C13—C14	129.21
N1^i—Tc1—N2^i	76.34	N5—C13—C13^i	111.92
N1^i—Tc1—N5^i	86.5	C13^i—C13—C14	118.85
N2^i—Tc1—N5^i	137.95	C13—C14—C15	121.25
Tc1—N1—C1	118.26	C14—C15—C15^i	119.89
Tc1—N2—C6	117.68
N2—Tc1—N1—C1	−7.54	Tc1—N5—C13—C14	−179.14
N5—Tc1—N1—C1	133.76	C6—C1—C2—C3	−0.88
N1^i—Tc1—N1—C1	−75.54	N1—C1—C6—N2	−1.97
N2^i—Tc1—N1—C1	−140.12	N1—C1—C6—C5	179.94
N5^i—Tc1—N1—C1	65.38	N1—C1—C2—C3	178.98
N1—Tc1—N2—C6	6.31	C2—C1—C6—N2	177.91
N5—Tc1—N2—C6	−62.38	C2—C1—C6—C5	−0.18
N1^i—Tc1—N2—C6	147.48	C1—C2—C3—C4	2.07
N2^i—Tc1—N2—C6	79.02	C2—C3—C4—C5	−2.27
N5^i—Tc1—N2—C6	−125.75	C3—C4—C5—C6	1.22
N1—Tc1—N5—C13	−131.64	C4—C5—C6—N2	−177.94
N2—Tc1—N5—C13	−66.55	C4—C5—C6—C1	−0.07
N1^i—Tc1—N5—C13	73.58	N5—C13—C14—C15	179.61
N2^i—Tc1—N5—C13	142.21	C13^i—C13—C14—C15	1.5
N5^i—Tc1—N5—C13	0.36	N5—C13—C13^i—N5^i	1.14
Tc1—N1—C1—C2	−172.36	N5—C13—C13^i—C14^i	179.55
Tc1—N1—C1—C6	7.5	C14—C13—C13^i—N5^i	179.55
Tc1—N2—C6—C1	−4.33	C14—C13—C13^i—C14^i	−2.03
Tc1—N2—C6—C5	173.64	C13—C14—C15—C15^i	−0.43
Tc1—N5—C13—C13^i	−0.93	C14—C15—C15^i—C14^i	−0.15

Symmetry codes: (i) x, −y+3/2, −z+1/2; (ii) −x+1/2, −y+1, z; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x+1/2, y+1, −z; (v) x+1/2, −y+1/2, z+1/2; (vi) x−1/2, y−1, −z; (vii) x−1/2, −y+1/2, z−1/2; (viii) −x+1/2, y−1/2, −z+1/2; (ix) x−1, y−1, z; (x) −x+1, −y+1, −z; (xi) x+1, y+1, z.

(30) bis(n-propylamine)dichloropalladium(II)

Crystal data

C6H18Cl2N2Pd	γ = 90°
Mr = 295.54	V = 567.6 (2) Å^3
Monclinic, C2/m	Z = 2
Hall symbol: -C 2y	F(000) = 296
a = 8.929 (2) Å	Dx = 1.729 Mg m^−3
b = 8.437 (2) Å	Mo K\a radiation, λ = 0.71070 Å
c = 7.542 (2) Å	µ = 2.06 mm^−1
α = 90°	T = 0 K
β = 92.65 (3)°	× × mm

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0	0	1	0.02*
Cl1	0	0.272	1	0.02*
N1	0.1963	0	0.8671	0.02*
C1	0.1661	0	0.67330	0.02*
C2	0.3076	0	0.569	0.02*
C3	0.2705	0	0.3725	0.02*
H1	0.25054	0.08630	0.89844	0.02*
H2	0.10700	0.09286	0.64064	0.02*
H3	0.36696	0.09303	0.60024	0.02*
H4	0.36158	0	0.30969	0.02*
H5	0.21400	0.09346	0.34099	0.02*

Geometric parameters (Å, º)

Pd1—Cl1	2.2949 (6)	C1—C2	1.5189 (4)
Pd1—N1	2.0590 (5)	C2—C3	1.5036 (4)
Pd1—N1^i	2.0590 (5)	C1—H2	0.97
Pd1—Cl1^ii	2.2949 (6)	C2—H3	0.97
N1—C1	1.4740 (4)	C3—H4	0.96
N1—H1	0.9	C3—H5	0.96
Pd1···C3^iii	3.6192 (10)	C3···Pd1^v	3.6192 (10)
Pd1···C3^iv	3.6192 (10)	C3···Pd1^iv	3.6192 (10)
Pd1···C3^v	3.6192 (10)	C3···Pd1^xiv	3.6192 (10)
Pd1···C3^vi	3.6192 (10)	C3···Pd1^xv	3.6192 (10)
Pd1···H5^iii	3.2299	C2···H4^xvi	3.0516
Pd1···H5^iv	3.2299	C2···H4^xvii	3.0516
Pd1···H5^v	3.2299	H1···H3	2.5215
Pd1···H5^vi	3.2299	H1···Cl1^ix	2.6115
Cl1···N1^vii	3.4362 (9)	H1···Cl1^xiii	2.6115
Cl1···N1^viii	3.4362 (9)	H2···H5	2.494
Cl1···N1^ix	3.4362 (9)	H3···H1	2.5215
Cl1···N1^x	3.4362 (9)	H4···C2^xvi	3.0516
Cl1···H1^ix	2.6115	H4···C2^xvii	3.0516
Cl1···H1^x	2.6115	H5···Pd1^xiv	3.2299
N1···Cl1^xi	3.4362 (9)	H5···H2	2.494
N1···Cl1^xii	3.4362 (9)	H5···Pd1^v	3.2299
N1···Cl1^ix	3.4362 (9)	H5···Pd1^iv	3.2299
N1···Cl1^xiii	3.4362 (9)	H5···Pd1^xv	3.2299
Cl1—Pd1—N1	90.00 (3)	N1—C1—H2^xviii	108.92
Cl1—Pd1—N1^i	90.00 (3)	C2—C1—H2	108.92
Cl1—Pd1—Cl1^ii	180	C2—C1—H2^xviii	108.92
N1—Pd1—N1^i	180	H2—C1—H2^xviii	107.74
Cl1^ii—Pd1—N1	90.00 (3)	C1—C2—H3	109.42
Cl1^ii—Pd1—N1^i	90.00 (3)	C1—C2—H3^xviii	109.42
Pd1—N1—C1	111.22 (3)	C3—C2—H3	109.42
Pd1—N1—H1^xviii	109.39	C3—C2—H3^xviii	109.42
C1—N1—H1	109.39	H3—C2—H3^xviii	108.02
Pd1—N1—H1	109.39	C2—C3—H4	109.47
H1—N1—H1^xviii	108.01	C2—C3—H5	109.47
C1—N1—H1^xviii	109.39	C2—C3—H5^xviii	109.47
N1—C1—C2	113.27 (3)	H4—C3—H5	108.99
C1—C2—C3	111.09 (3)	H4—C3—H5^xviii	108.99
N1—C1—H2	108.92	H5—C3—H5^xviii	110.44
Cl1—Pd1—N1—C1	−90.00 (3)	N1—C1—C2—C3	−180.00 (3)
Pd1—N1—C1—C2	180.00 (3)

Symmetry codes: (i) −x, y, −z+2; (ii) −x, −y, −z+2; (iii) x, y, z+1; (iv) −x, −y, −z+1; (v) −x, y, −z+1; (vi) x, −y, z+1; (vii) x−1/2, y+1/2, z; (viii) −x+1/2, y+1/2, −z+2; (ix) −x+1/2, −y+1/2, −z+2; (x) x−1/2, −y+1/2, z; (xi) x+1/2, y−1/2, z; (xii) −x+1/2, y−1/2, −z+2; (xiii) x+1/2, −y+1/2, z; (xiv) x, y, z−1; (xv) x, −y, z−1; (xvi) −x+1, y, −z+1; (xvii) −x+1, −y, −z+1; (xviii) x, −y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···Cl1^ix	0.9	2.61	3.4362 (9)	153
N1—H1···Cl1^xiii	0.9	2.61	3.4362 (9)	153

Symmetry codes: (ix) −x+1/2, −y+1/2, −z+2; (xiii) x+1/2, −y+1/2, z.