Structure determination of two metal-organic complexes from high-resolution synchrotron powder diffraction data

Dova, E.; Goubitz, K.; Langevelde, A. van; Driessen, R.; Mahabiersing, T.; Blaauw, R.; Peschar, R.; Schenk, H.

doi:10.1107/S0909049501013784

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Structure determination of two metal-organic complexes from high-resolution synchrotron powder diffraction data

E. Dova, K. Goubitz, A. van Langevelde, R. Driessen, T. Mahabiersing, R. Blaauw, R. Peschar and H. Schenk

The crystal structures of [1,2-bis(2,6-diisopropylphenylimino)acenaphthene-N,N′]carbonylchlororhodium(I) (1) and [N,N′-ethylene-bis(3-methylsalicylideneiminato)-O,N,N′,O′](tetrahydrofurfuryl)-cobalt(II) (2) have been determined from high-resolution synchrotron X-ray powder diffraction data. Compound 1 is the first neutral Rh complex, in contrast with findings in the literature, containing a bidentate nitrogen ligand, and compound 2 is the first three-dimensional structure of a (five-coordinated) tetrahydrofurfurylcobalt(III) complex. Grid-search and Rietveld refinement have been used to determine and refine the structures, respectively. Crystals of 1 are orthorhombic, space group Pbca, Z = 8, with cell parameters a = 21.729 (2), b = 27.376 (3), c = 11.580 (1) Å. Crystals of 2 are monoclinic, space group P2₁/n, Z = 4, a = 16.6701 (6), b = 9.4170 (4), c = 13.7088 (7) Å and β = 96.520 (3)°. Chemical diagrams for the two compounds are given. Soft restraints were applied during Rietveld refinement; for 1 converging to R_p = 8.4%, R_w = 11.0%, GoF = 2.3, and for 2 converging to R_p = 8.5%, R_w = 11.4%, GoF = 7.6.

Keywords: structure determination; powder diffraction; grid-search techniques.

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Supporting information

Crystallographic Information File (CIF) https://doi.org/10.1107/S0909049501013784/wl2002sup1.cif
Contains datablocks global, Compound_1, Compound_2

Computing details top

For both compounds, cell refinement: UnitCell; data reduction: MRIA; program(s) used to solve structure: MRIA; program(s) used to refine structure: MRIA; molecular graphics: CHEMDRAW and PLATON.

Figures top

(Compound_1) chloro-CO-(bis(2,6-di-isoprpopylpheylimino)acenaphtene-N,N')-rhodium top

Crystal data top

C₃₇H₄₀ClN₂ORh	V = 6888 (2) Å³
M_r = 667.07	Z = 8
Orthorhombic, Pbca	Synchrotron radiation, λ = 0.65296 Å
Hall symbol: -p 2ac 2ab	µ = 0.6 mm⁻¹
a = 21.729 (2) Å	T = 293 K
b = 27.376 (3) Å	cylinder, ? × 0.7 mm mm
c = 11.579 (1) Å

Data collection top

ESRF BM16 diffractometer	Data collection mode: transmission
Radiation source: synchrotron	Scan method: continuous
Specimen mounting: capillary	2θ_min = 2.500°, 2θ_max = 25.00°, 2θ_step = 0.005°

Refinement top

R_p = 8.4	175 parameters
R_wp = 11.1	38 restraints
R_exp = ?	Calculated and kept fixed
χ² = 6.250
4500 data points	Background function: polynomal
Profile function: split-type pseudo-Voigt	Preferred orientation correction: 'Ahtee and Jarvinen'

Crystal data top

C₃₇H₄₀ClN₂ORh	V = 6888 (2) Å³
M_r = 667.07	Z = 8
Orthorhombic, Pbca	Synchrotron radiation, λ = 0.65296 Å
a = 21.729 (2) Å	µ = 0.6 mm⁻¹
b = 27.376 (3) Å	T = 293 K
c = 11.579 (1) Å	cylinder, ? × 0.7 mm mm

Data collection top

ESRF BM16 diffractometer	Scan method: continuous
Specimen mounting: capillary	2θ_min = 2.500°, 2θ_max = 25.00°, 2θ_step = 0.005°
Data collection mode: transmission

Refinement top

R_p = 8.4	4500 data points
R_wp = 11.1	175 parameters
R_exp = ?	38 restraints
χ² = 6.250	Calculated and kept fixed

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

	x	y	z	B_iso*/B_eq
Rh1	0.5684 (6)	0.3673 (4)	0.5327 (10)	*
Cl1	0.4653 (12)	0.3676 (9)	0.5116 (18)	*
N1	0.6610 (10)	0.3707 (8)	0.5681 (19)	*
N2	0.5655 (10)	0.3838 (8)	0.705 (2)	*
C1	0.6703 (10)	0.3808 (9)	0.6734 (18)	*
C2	0.7244 (10)	0.3815 (11)	0.7402 (17)	*
C3	0.7880 (12)	0.3750 (10)	0.7166 (16)	*
C4	0.8308 (11)	0.373 (2)	0.817 (3)	*
C5	0.8095 (12)	0.380 (3)	0.928 (3)	*
C6	0.7467 (12)	0.398 (4)	0.946 (3)	*
C7	0.7179 (12)	0.400 (3)	1.056 (2)	*
C8	0.6529 (14)	0.400 (2)	1.067 (2)	*
C9	0.6151 (9)	0.3976 (9)	0.971 (2)	*
C10	0.6424 (9)	0.3921 (10)	0.862 (2)	*
C11	0.6204 (10)	0.3875 (9)	0.746 (2)	*
C12	0.7058 (9)	0.3892 (14)	0.854 (2)	*
C13	0.5804 (12)	0.3525 (11)	0.366 (3)	*
O13	0.5851 (13)	0.3448 (11)	0.278 (3)	*
C14	0.7077 (11)	0.3555 (6)	0.4867 (18)	*
C15	0.7234 (12)	0.3054 (8)	0.476 (2)	*
C16	0.7707 (13)	0.2902 (8)	0.400 (2)	*
C18	0.7842 (13)	0.3743 (8)	0.340 (2)	*
C19	0.7381 (12)	0.3904 (8)	0.417 (2)	*
C20	0.6896 (11)	0.2656 (8)	0.549 (2)	*
C21	0.7335 (12)	0.2405 (8)	0.630 (2)	*
C22	0.6568 (10)	0.2288 (8)	0.471 (2)	*
C23	0.7212 (12)	0.4459 (9)	0.425 (2)	*
C24	0.7764 (13)	0.4753 (8)	0.467 (2)	*
C25	0.6980 (11)	0.4648 (8)	0.311 (2)	*
C26	0.5108 (10)	0.3813 (6)	0.775 (2)	*
C27	0.4782 (12)	0.4246 (8)	0.802 (2)	*
C28	0.4273 (12)	0.4218 (8)	0.878 (3)	*
C29	0.4099 (14)	0.3770 (8)	0.929 (3)	*
C17	0.8011 (15)	0.3254 (8)	0.335 (3)	*
C30	0.4385 (12)	0.3338 (8)	0.894 (3)	*
C31	0.4897 (12)	0.3352 (7)	0.819 (2)	*
C32	0.4987 (12)	0.4744 (9)	0.752 (2)	*
C33	0.4493 (14)	0.4978 (9)	0.675 (2)	*
C34	0.5171 (11)	0.5094 (8)	0.852 (2)	*
C35	0.5223 (12)	0.2876 (8)	0.788 (2)	*
C36	0.4807 (12)	0.2510 (8)	0.726 (2)	*
C37	0.5498 (11)	0.2642 (8)	0.898 (2)	*
H1	0.80273	0.36977	0.63452	*
H2	0.87553	0.37255	0.79426	*
H3	0.83992	0.38567	0.98991	*
H4	0.74619	0.39694	1.12774	*
H5	0.63566	0.40459	1.14665	*
H6	0.56971	0.40008	0.97761	*
H7	0.77919	0.25485	0.38967	*
H8	0.83211	0.31403	0.27445	*
H9	0.80656	0.39862	0.28890	*
H10	0.65634	0.28327	0.59441	*
H11	0.76640	0.22461	0.58515	*
H12	0.75116	0.26574	0.68351	*
H13	0.71101	0.21551	0.67785	*
H14	0.62441	0.24620	0.42087	*
H15	0.68620	0.21209	0.41974	*
H16	0.63330	0.20350	0.51744	*
H17	0.68886	0.44885	0.48102	*
H18	0.79058	0.46276	0.54411	*
H19	0.81327	0.47030	0.41072	*
H20	0.76802	0.51043	0.47085	*
H21	0.73195	0.45969	0.24681	*
H22	0.66150	0.44596	0.28395	*
H23	0.68910	0.50012	0.31176	*
H24	0.40127	0.45159	0.89068	*
H25	0.36719	0.37442	0.96421	*
H26	0.42220	0.30131	0.91827	*
H27	0.53578	0.46870	0.70549	*
H28	0.43986	0.47522	0.61058	*
H29	0.41007	0.50198	0.72382	*
H30	0.46204	0.52997	0.64681	*
H31	0.47990	0.51334	0.90543	*
H32	0.55086	0.49359	0.89863	*
H33	0.52987	0.54112	0.82320	*
H34	0.55903	0.29602	0.73582	*
H35	0.44626	0.24312	0.77591	*
H36	0.46760	0.26601	0.65177	*
H37	0.50485	0.21997	0.70692	*
H38	0.58117	0.28854	0.93443	*
H39	0.51778	0.25752	0.95441	*
H40	0.57413	0.23387	0.88007	*

Geometric parameters (Å, º) top

Rh1—C13	1.99 (3)	C21—H13	1.01 (2)
Rh1—N2	2.04 (3)	C22—H15	0.99 (2)
Rh1—N1	2.06 (2)	C22—H16	1.01 (2)
Rh1—Cl1	2.26 (3)	C22—H14	1.03 (2)
N1—C1	1.27 (3)	C23—H17	0.96 (3)
N1—C14	1.45 (3)	C23—C25	1.50 (4)
N2—C11	1.29 (3)	C23—C24	1.52 (4)
N2—C26	1.44 (3)	C24—H20	0.98 (2)
C1—C11	1.38 (3)	C24—H18	1.00 (2)
C1—C2	1.41 (3)	C24—H19	1.04 (3)
C2—C12	1.40 (3)	C25—H23	0.99 (2)
C2—C3	1.42 (3)	C25—H22	1.00 (2)
C3—H1	1.01 (2)	C25—H21	1.06 (3)
C3—C4	1.49 (4)	C26—C27	1.41 (3)
C4—H2	1.01 (3)	C26—C31	1.43 (3)
C4—C5	1.38 (4)	C27—C28	1.41 (4)
C5—H3	0.98 (3)	C27—C32	1.55 (3)
C5—C6	1.46 (6)	C28—H24	1.00 (2)
C6—C12	1.40 (4)	C28—C29	1.42 (4)
C6—C7	1.43 (4)	C29—H25	1.01 (3)
C7—H4	1.03 (3)	C29—C30	1.40 (3)
C7—C8	1.42 (4)	C17—H8	1.02 (3)
C8—H5	1.00 (3)	C30—H26	1.00 (2)
C8—C9	1.39 (4)	C30—C31	1.41 (4)
C9—H6	0.99 (2)	C31—C35	1.53 (3)
C9—C10	1.40 (3)	C32—H27	0.98 (3)
C10—C12	1.38 (3)	C32—C33	1.53 (4)
C10—C11	1.44 (3)	C32—C34	1.55 (4)
C13—O13	1.04 (4)	C33—H30	0.98 (2)
C14—C19	1.41 (3)	C33—H28	0.99 (2)
C14—C15	1.42 (3)	C33—H29	1.03 (3)
C15—C16	1.42 (4)	C34—H33	0.97 (2)
C15—C20	1.56 (3)	C34—H32	1.01 (2)
C16—H7	0.99 (2)	C34—H31	1.02 (3)
C16—C17	1.39 (4)	C35—H34	1.02 (3)
C18—H9	1.02 (2)	C35—C36	1.52 (3)
C18—C17	1.39 (3)	C35—C37	1.55 (4)
C18—C19	1.41 (4)	C36—H35	0.97 (2)
C19—C23	1.57 (3)	C36—H36	1.00 (2)
C20—H10	1.01 (2)	C36—H37	1.02 (2)
C20—C21	1.50 (3)	C37—H39	0.98 (2)
C20—C22	1.53 (3)	C37—H40	1.00 (2)
C21—H11	0.98 (2)	C37—H38	1.04 (2)
C21—H12	1.01 (2)

C37···H14ⁱ	1.67 (2)	C14···C21	3.60 (3)
C22···H38	1.76 (2)	C2···C9	3.60 (3)
C25···H17	2.02 (3)	C6···C11	3.60 (4)
C4···H3	2.04 (3)	C20···C37	3.60 (3)
C24···H17	2.04 (3)	C26···C37	3.60 (3)
C20···H12	2.05 (3)	O13···C14	3.61 (4)
C20···H11	2.05 (2)	C14···C24	3.61 (3)
C35···H35	2.06 (2)	C3···C10	3.62 (3)
C35···H36	2.06 (3)	C26···C34	3.62 (3)
C19···H17	2.06 (2)	C14···C25	3.62 (3)
C22···H10	2.06 (2)	C13···C19	3.63 (4)
C27···H27	2.07 (3)	C9···C27	3.64 (3)
C34···H27	2.07 (3)	C22···C35	3.64 (3)
C33···H27	2.07 (3)	C14···C22	3.64 (3)
C7···H5	2.07 (3)	C26···C33	3.65 (3)
C30···H25	2.07 (3)	C3···C15	3.65 (3)
C32···H28	2.07 (3)	C3···C19	3.65 (3)
C37···H34	2.08 (3)	C11···C14	3.66 (3)
C17···H9	2.08 (2)	C7···C18	3.66 (4)
C10···H6	2.08 (2)	C12···C22ⁱ	3.66 (4)
C20···H13	2.08 (2)	C1···C26	3.66 (3)
C16···H8	2.08 (3)	C9···C31	3.67 (3)
C31···H34	2.08 (2)	C26···C36	3.67 (3)
C8···H6	2.08 (3)	C3···C11	3.67 (3)
C31···H26	2.08 (3)	C1···C9	3.68 (3)
C21···H10	2.09 (2)	C3···C30	3.69 (4)
C23···H22	2.09 (3)	C2···C15	3.70 (3)
C15···H10	2.09 (3)	C2···C7	3.70 (3)
C17···H7	2.09 (2)	C10···C31	3.70 (3)
C29···H26	2.09 (2)	Cl1···C31	3.70 (4)
C9···H5	2.09 (2)	C8···C22ⁱ	3.70 (6)
C32···H29	2.09 (3)	Cl1···C27	3.72 (4)
C23···H18	2.09 (3)	C5···C10	3.72 (3)
C18···H8	2.10 (2)	C10···C27	3.74 (3)
C28···H25	2.10 (3)	N2···C28	3.75 (4)
C15···H7	2.10 (2)	C4···C27	3.76 (4)
C27···H24	2.10 (3)	C2···C19	3.76 (3)
C20···H15	2.10 (2)	N1···C18	3.76 (4)
C23···H23	2.10 (2)	C4···C7	3.77 (4)
C29···H24	2.10 (2)	N2···C30	3.78 (4)
C35···H39	2.10 (3)	N1···C16	3.78 (3)
C32···H30	2.10 (3)	C5···C8	3.80 (4)
C36···H34	2.10 (2)	C8···C11	3.80 (3)
C23···H20	2.11 (2)	Rh1···C35	3.80 (3)
C3···H2	2.11 (2)	Cl1···O13	3.81 (4)
C35···H37	2.11 (2)	N1···O13	3.81 (4)
C6···H4	2.11 (3)	C18···C29	3.82 (4)
C23···H21	2.11 (3)	Rh1···C15	3.83 (3)
C32···H32	2.11 (3)	C29···C35	3.83 (4)
C23···H19	2.11 (3)	Rh1···C31	3.83 (3)
C32···H31	2.11 (3)	C20···C17	3.84 (4)
C19···H9	2.12 (3)	Rh1···C20	3.84 (3)
C32···H33	2.12 (2)	C28···C34	3.85 (4)
C6···H3	2.12 (3)	C1···C4	3.87 (3)
C20···H14	2.12 (3)	C23···C17	3.87 (3)
C2···H1	2.12 (2)	C27···C35	3.87 (3)
C5···H2	2.12 (3)	O13···C35	3.88 (4)
C20···H16	2.13 (2)	C29···C17	3.88 (5)
C35···H38	2.13 (3)	C29···C32	3.88 (4)
C35···H40	2.14 (2)	C19···C20	3.89 (3)
C8···H4	2.15 (3)	C15···C23	3.89 (3)
C4···H1	2.20 (3)	C31···C32	3.89 (3)
C11···C12	2.24 (3)	C9···O13	3.90 (4)
C1···C12	2.24 (3)	C7···C22ⁱ	3.90 (7)
C2···C11	2.27 (3)	O13···C19	3.90 (4)
N1···C11	2.29 (3)	C8···C24	3.91 (6)
C1···C10	2.29 (3)	C13···C36	3.91 (4)
C2···C10	2.29 (3)	O13···C15	3.93 (4)
N2···C1	2.31 (3)	C4···C31	3.93 (4)
C7···C12	2.37 (4)	C2···C20	3.94 (3)
C8···C10	2.39 (3)	Rh1···C37	3.95 (2)
C9···C12	2.40 (3)	C12···C24	3.95 (4)
C1···C14	2.41 (3)	C7···C21ⁱ	3.96 (7)
C11···C26	2.41 (3)	N1···C21	3.96 (3)
C15···C17	2.42 (4)	C13···C22	3.96 (4)
C5···C12	2.42 (3)	C10···C35	3.97 (3)
C16···C18	2.42 (3)	C13···C20	3.97 (4)
C3···C12	2.43 (3)	Rh1···C19	3.97 (3)
C28···C30	2.43 (3)	C9···C34	3.97 (3)
C14···C18	2.43 (4)	N2···C34	3.98 (3)
C26···C28	2.43 (3)	N2···C37	3.98 (3)
N1···C2	2.44 (3)	N1···C24	3.98 (3)
C19···C17	2.44 (4)	C3···C24	3.99 (3)
C29···C31	2.44 (4)	C3···C21	4.00 (3)
C7···C9	2.44 (3)	C6···C22ⁱ	4.00 (10)
C15···C19	2.45 (3)	Rh1···C27	4.00 (3)
C4···C6	2.45 (5)	C9···C37	4.01 (3)
C26···C30	2.46 (3)	N1···C25	4.01 (3)
C14···C16	2.46 (3)	C24···C28	4.02 (4)
C27···C29	2.47 (4)	C8···C13	4.02 (4)
C27···C31	2.47 (3)	N2···C33	4.03 (3)
C6···C10	2.47 (4)	N2···C13	4.03 (4)
C2···C6	2.47 (4)	N1···C22	4.04 (3)
N2···C27	2.47 (3)	C13···C23	4.05 (4)
C6···C8	2.48 (4)	C13···C25	4.05 (4)
N1···C19	2.48 (3)	Cl1···C33	4.05 (3)
N1···C15	2.48 (3)	C2···C23	4.05 (3)
C22···C37	2.48 (3)	C10···C32	4.06 (3)
N2···C10	2.49 (3)	C4···C26	4.06 (3)
C2···C4	2.49 (3)	C10···C37	4.06 (3)
N2···C31	2.49 (3)	Cl1···C36	4.06 (3)
C24···C25	2.50 (4)	N1···C26	4.06 (3)
C21···C22	2.50 (3)	N2···C14	4.07 (3)
C3···C5	2.50 (4)	Cl1···C35	4.07 (3)
C36···C37	2.51 (3)	C2···C21	4.07 (4)
C31···C37	2.51 (3)	N2···C36	4.08 (3)
C15···C21	2.52 (3)	Cl1···C32	4.10 (3)
C19···C25	2.53 (3)	C11···C37	4.10 (3)
C30···C35	2.54 (4)	C1···C21	4.11 (3)
C19···C24	2.54 (3)	C36···C37	4.12 (4)
C27···C34	2.54 (3)	O13···C25	4.12 (4)
C33···C34	2.54 (4)	C2···C8	4.13 (3)
C5···C7	2.54 (4)	C18···C21	4.13 (3)
C31···C36	2.55 (3)	C24···C29	4.13 (4)
C15···C22	2.55 (3)	C1···C13	4.14 (4)
C16···C20	2.55 (4)	C13···C35	4.14 (4)
C27···C33	2.56 (3)	C19···C29	4.15 (4)
C28···C32	2.57 (4)	C7···O13	4.15 (5)
C26···C32	2.58 (3)	Rh1···C23	4.15 (3)
C26···C35	2.58 (3)	C9···C32	4.15 (3)
C18···C23	2.58 (3)	C3···C23	4.16 (3)
C14···C20	2.59 (3)	C3···C20	4.16 (3)
C14···C23	2.59 (3)	C4···C10	4.16 (3)
C1···C3	2.61 (3)	Rh1···C32	4.16 (3)
C9···C11	2.62 (3)	Rh1···C2	4.17 (2)
N1···N2	2.64 (3)	C23···C33	4.18 (4)
C8···C12	2.74 (4)	C13···C33	4.18 (4)
Rh1···C11	2.77 (2)	O13···C22	4.19 (4)
Rh1···C1	2.77 (2)	C7···C11	4.19 (3)
C4···C12	2.78 (3)	C11···C22ⁱ	4.19 (3)
C7···C10	2.79 (3)	Rh1···C10	4.20 (3)
C15···C18	2.79 (3)	C9···C35	4.20 (3)
C14···C17	2.81 (4)	C9···C24	4.20 (3)
C28···C31	2.81 (3)	C11···C34	4.20 (3)
C26···C29	2.83 (4)	C1···C24	4.21 (3)
C27···C30	2.84 (3)	C10···C34	4.21 (3)
C16···C19	2.84 (3)	C7···C19	4.21 (4)
C2···C5	2.86 (4)	C10···C24	4.21 (4)
C3···C6	2.87 (4)	C15···C21	4.21 (3)
C6···C9	2.87 (3)	C7···C17	4.22 (5)
N2···C32	2.92 (3)	C1···C5	4.22 (4)
N1···C20	2.95 (3)	C2···C24	4.23 (3)
N1···C23	2.95 (3)	C6···C25	4.23 (10)
N2···C35	2.95 (3)	N1···C17	4.26 (4)
N1···C13	2.97 (4)	Cl1···C37	4.26 (3)
Rh1···O13	3.03 (3)	N2···C29	4.27 (4)
C2···C14	3.04 (3)	C4···C33	4.27 (5)
Cl1···C13	3.05 (4)	C9···C28	4.27 (3)
C10···C26	3.05 (3)	C3···C7	4.27 (3)
C30···C37	3.08 (3)	C5···C9	4.28 (3)
C16···C21	3.09 (4)	C2···C22ⁱ	4.29 (3)
Rh1···C14	3.09 (3)	C8···C21ⁱ	4.29 (6)
Rh1···C26	3.10 (3)	Cl1···N1	4.30 (3)
C13···C14	3.10 (4)	Rh1···C22	4.31 (3)
C16···C22	3.10 (3)	C9···C30	4.31 (3)
C28···C34	3.11 (3)	C11···C20	4.31 (3)
C30···C36	3.12 (4)	C1···C35	4.31 (3)
C18···C25	3.12 (3)	C29···C34	4.32 (4)
C18···C24	3.13 (3)	C8···C18	4.32 (4)
C3···C29	3.14 (4)	C16···C29	4.32 (4)
Cl1···N2	3.15 (3)	C15···C37	4.32 (3)
C28···C33	3.17 (4)	C6···C23	4.33 (11)
C3···C14	3.23 (3)	Rh1···C36	4.34 (3)
C8···O13	3.23 (5)	O13···C21	4.34 (4)
Cl1···C26	3.23 (3)	C28···C35	4.34 (3)
C9···C26	3.24 (3)	C12···C26	4.34 (3)
N1···C3	3.25 (3)	C17···C30	4.34 (4)
C13···C37	3.28 (4)	C24···C25	4.35 (4)
C1···C15	3.28 (3)	C29···C37	4.35 (3)
N2···C9	3.29 (3)	C18···C20	4.35 (3)
C11···C31	3.29 (3)	C3···C16	4.35 (3)
C11···C27	3.32 (3)	C9···C34	4.35 (3)
C1···C19	3.32 (3)	C3···C27	4.36 (4)
C21···C17ⁱ	3.32 (4)	C12···C14	4.36 (3)
C4···C29	3.33 (5)	C3···C18	4.36 (3)
C16···C21	3.34 (4)	Cl1···C11	4.36 (3)
C4···C28	3.35 (4)	C6···C21ⁱ	4.36 (10)
C25···C33	3.36 (4)	C5···C21ⁱ	4.37 (6)
O13···C37	3.38 (4)	O13···C22	4.37 (4)
C3···C28	3.46 (4)	C21···C22ⁱ	4.38 (3)
C7···C25	3.47 (5)	C21···C17	4.38 (4)
Cl1···C5	3.47 (4)	C30···C32	4.39 (3)
C8···C25	3.48 (5)	O13···C23	4.39 (4)
N2···C2	3.48 (3)	C22···C17	4.40 (4)
N1···C10	3.48 (3)	C5···C24	4.40 (7)
C1···C20	3.49 (3)	C27···C34	4.40 (4)
N1···C12	3.49 (3)	C29···C34	4.40 (3)
C11···C35	3.50 (3)	C22···C31	4.40 (3)
C6···C24	3.51 (11)	C16···C23	4.41 (3)
N2···C12	3.51 (3)	O13···C33	4.41 (4)
O13···C36	3.52 (4)	C24···C17	4.41 (3)
Cl1···C4	3.54 (4)	Rh1···C33	4.42 (3)
C34···C34	3.55 (4)	C25···C17	4.43 (3)
C4···C30	3.55 (4)	Cl1···C30	4.56 (4)
C10···C22ⁱ	3.56 (4)	Cl1···C28	4.56 (4)
C11···C32	3.56 (3)	Cl1···C36	4.64 (3)
C1···C23	3.56 (3)	Rh1···C25	4.65 (3)
C7···C24	3.57 (7)	Cl1···C33	4.66 (3)
C9···C22ⁱ	3.58 (3)	Rh1···C33	4.71 (3)
C1···C6	3.59 (4)	Rh1···C12	4.81 (2)
C13···C15	3.60 (4)

C13—Rh1—N2	174.2 (12)	H16—C22—H14	106 (2)
C13—Rh1—N1	94.3 (11)	H16—C22—C20	112 (2)
C13—Rh1—Cl1	91.4 (10)	H14—C22—C20	110 (2)
N2—Rh1—N1	80.0 (10)	H17—C23—C25	108 (2)
N2—Rh1—Cl1	94.2 (9)	H17—C23—C24	108 (2)
N1—Rh1—Cl1	174.0 (10)	H17—C23—C19	107 (2)
C1—N1—C14	125 (2)	C25—C23—C24	111 (2)
C1—N1—Rh1	111.0 (17)	C25—C23—C19	111 (2)
C14—N1—Rh1	122.9 (16)	C24—C23—C19	110 (2)
C11—N2—C26	124 (2)	H20—C24—H18	111 (2)
C11—N2—Rh1	110.3 (17)	H20—C24—H19	107 (2)
C26—N2—Rh1	124.6 (17)	H20—C24—C23	113 (2)
N1—C1—C11	119 (2)	H18—C24—H19	106 (2)
N1—C1—C2	132 (2)	H18—C24—C23	110 (2)
C11—C1—C2	108.6 (19)	H19—C24—C23	110 (2)
C12—C2—C1	106.3 (19)	H23—C25—H22	111 (2)
C12—C2—C3	118.8 (18)	H23—C25—H21	106 (2)
C1—C2—C3	134.8 (19)	H23—C25—C23	114 (2)
H1—C3—C2	120 (2)	H22—C25—H21	105 (2)
H1—C3—C4	122 (2)	H22—C25—C23	112 (2)
C2—C3—C4	117.5 (18)	H21—C25—C23	110 (2)
H2—C4—C5	125 (3)	C27—C26—C31	120 (2)
H2—C4—C3	114 (3)	C27—C26—N2	119.6 (18)
C5—C4—C3	121 (2)	C31—C26—N2	120.2 (18)
H3—C5—C4	118 (3)	C28—C27—C26	119 (2)
H3—C5—C6	118 (4)	C28—C27—C32	120 (2)
C4—C5—C6	119 (3)	C26—C27—C32	121 (2)
C12—C6—C7	114 (3)	H24—C28—C27	119 (2)
C12—C6—C5	115 (5)	H24—C28—C29	119 (3)
C7—C6—C5	123 (4)	C27—C28—C29	121 (2)
H4—C7—C8	121 (2)	H25—C29—C30	118 (2)
H4—C7—C6	117 (3)	H25—C29—C28	118 (2)
C8—C7—C6	121 (2)	C30—C29—C28	119 (3)
H5—C8—C9	122 (3)	H8—C17—C18	120 (3)
H5—C8—C7	117 (3)	H8—C17—C16	118 (2)
C9—C8—C7	121 (2)	C18—C17—C16	121 (3)
H6—C9—C8	121 (2)	H26—C30—C29	121 (3)
H6—C9—C10	120 (2)	H26—C30—C31	119 (2)
C8—C9—C10	119 (2)	C29—C30—C31	121 (2)
C12—C10—C9	119 (2)	C30—C31—C26	119 (2)
C12—C10—C11	105.2 (19)	C30—C31—C35	119 (2)
C9—C10—C11	135.5 (19)	C26—C31—C35	121 (2)
N2—C11—C1	119 (2)	H27—C32—C33	109 (2)
N2—C11—C10	131 (2)	H27—C32—C27	108 (2)
C1—C11—C10	108.7 (18)	H27—C32—C34	107 (2)
C10—C12—C2	111 (2)	C33—C32—C27	113 (2)
C10—C12—C6	125 (2)	C33—C32—C34	111 (2)
C2—C12—C6	124 (2)	C27—C32—C34	110 (2)
O13—C13—Rh1	178 (3)	H30—C33—H28	112 (2)
C19—C14—C15	120 (2)	H30—C33—H29	109 (2)
C19—C14—N1	120.2 (17)	H30—C33—C32	112 (2)
C15—C14—N1	120 (2)	H28—C33—H29	108 (3)
C14—C15—C16	121 (2)	H28—C33—C32	109 (2)
C14—C15—C20	121 (2)	H29—C33—C32	108 (2)
C16—C15—C20	118.2 (19)	H33—C34—H32	111 (2)
H7—C16—C17	121 (3)	H33—C34—H31	110 (2)
H7—C16—C15	120 (2)	H33—C34—C32	112 (2)
C17—C16—C15	119 (2)	H32—C34—H31	107 (2)
H9—C18—C17	118 (3)	H32—C34—C32	109 (2)
H9—C18—C19	120 (2)	H31—C34—C32	108 (2)
C17—C18—C19	121 (2)	H34—C35—C36	110 (2)
C18—C19—C14	119 (2)	H34—C35—C31	108 (2)
C18—C19—C23	120 (2)	H34—C35—C37	106 (2)
C14—C19—C23	121 (2)	C36—C35—C31	113 (2)
H10—C20—C21	110 (2)	C36—C35—C37	109.8 (18)
H10—C20—C22	107 (2)	C31—C35—C37	110 (2)
H10—C20—C15	106.4 (18)	H35—C36—H36	113 (2)
C21—C20—C22	111.1 (18)	H35—C36—H37	110 (2)
C21—C20—C15	111 (2)	H35—C36—C35	109 (2)
C22—C20—C15	111 (2)	H36—C36—H37	107 (2)
H11—C21—H12	111 (2)	H36—C36—C35	108 (2)
H11—C21—H13	110 (2)	H37—C36—C35	110 (2)
H11—C21—C20	110 (2)	H39—C37—H40	111 (2)
H12—C21—H13	108 (2)	H39—C37—H38	108 (2)
H12—C21—C20	108.2 (19)	H39—C37—C35	111 (2)
H13—C21—C20	110 (2)	H40—C37—H38	105 (2)
H15—C22—H16	109 (2)	H40—C37—C35	112 (2)
H15—C22—H14	108 (2)	H38—C37—C35	108.9 (19)
H15—C22—C20	111 (2)

Cl1—Rh1—N1—C1	16 (11)	H9—C18—C17—H8	−6 (5)
Cl1—Rh1—N1—C14	−174 (9)	C14—C19—C23—C24	117 (3)
N2—Rh1—N1—C1	−0.0 (18)	C14—C19—C23—C25	−119 (3)
N2—Rh1—N1—C14	170.6 (18)	C14—C19—C23—H17	0 (3)
C13—Rh1—N1—C1	179 (2)	C18—C19—C23—C24	−63 (3)
C13—Rh1—N1—C14	−10 (2)	C18—C19—C23—C25	61 (3)
Cl1—Rh1—N2—C11	−178.7 (18)	C18—C19—C23—H17	179 (2)
Cl1—Rh1—N2—C26	13.7 (19)	C15—C20—C21—H11	−60 (3)
N1—Rh1—N2—C11	−0.3 (18)	C15—C20—C21—H12	61 (3)
N1—Rh1—N2—C26	−168.0 (19)	C15—C20—C21—H13	178 (2)
C13—Rh1—N2—C11	−9 (13)	C22—C20—C21—H11	64 (3)
C13—Rh1—N2—C26	−177 (12)	C22—C20—C21—H12	−175 (2)
Cl1—Rh1—C13—O13	6 (91)	C22—C20—C21—H13	−57 (3)
N1—Rh1—C13—O13	−172 (91)	H10—C20—C21—H11	−178 (2)
N2—Rh1—C13—O13	−163 (84)	H10—C20—C21—H12	−57 (3)
Rh1—N1—C1—C2	172 (3)	H10—C20—C21—H13	61 (3)
Rh1—N1—C1—C11	0 (3)	C15—C20—C22—H14	−60 (3)
C14—N1—C1—C2	1 (4)	C15—C20—C22—H15	60 (3)
C14—N1—C1—C11	−170 (2)	C15—C20—C22—H16	−178 (2)
Rh1—N1—C14—C15	−82 (3)	C21—C20—C22—H14	176 (2)
Rh1—N1—C14—C19	98 (2)	C21—C20—C22—H15	−64 (3)
C1—N1—C14—C15	87 (3)	C21—C20—C22—H16	58 (3)
C1—N1—C14—C19	−93 (3)	H10—C20—C22—H14	55 (3)
Rh1—N2—C11—C1	0 (3)	H10—C20—C22—H15	175 (2)
Rh1—N2—C11—C10	−171 (2)	H10—C20—C22—H16	−62 (3)
C26—N2—C11—C1	168 (2)	C19—C23—C24—H18	−57 (3)
C26—N2—C11—C10	−3 (4)	C19—C23—C24—H19	59 (3)
Rh1—N2—C26—C27	−101 (2)	C19—C23—C24—H20	178 (2)
Rh1—N2—C26—C31	80 (3)	C25—C23—C24—H18	178 (2)
C11—N2—C26—C27	93 (3)	C25—C23—C24—H19	−65 (3)
C11—N2—C26—C31	−87 (3)	C25—C23—C24—H20	54 (3)
N1—C1—C2—C3	5 (6)	H17—C23—C24—H18	59 (3)
N1—C1—C2—C12	−172 (3)	H17—C23—C24—H19	175 (2)
C11—C1—C2—C3	177 (3)	H17—C23—C24—H20	−65 (3)
C11—C1—C2—C12	0 (3)	C19—C23—C25—H21	−59 (3)
N1—C1—C11—N2	0 (4)	C19—C23—C25—H22	57 (3)
N1—C1—C11—C10	173 (2)	C19—C23—C25—H23	−177 (2)
C2—C1—C11—N2	−174 (2)	C24—C23—C25—H21	65 (3)
C2—C1—C11—C10	0 (3)	C24—C23—C25—H22	−179 (2)
C1—C2—C3—C4	−173 (4)	C24—C23—C25—H23	−53 (3)
C1—C2—C3—H1	3 (5)	H17—C23—C25—H21	−176 (2)
C12—C2—C3—C4	4 (5)	H17—C23—C25—H22	−60 (3)
C12—C2—C3—H1	−179 (3)	H17—C23—C25—H23	66 (3)
C1—C2—C12—C6	−172 (6)	N2—C26—C27—C28	−176 (2)
C1—C2—C12—C10	1 (4)	N2—C26—C27—C32	3 (4)
C3—C2—C12—C6	10 (7)	C31—C26—C27—C28	4 (4)
C3—C2—C12—C10	−177 (3)	C31—C26—C27—C32	−177 (2)
C2—C3—C4—C5	−3 (7)	N2—C26—C31—C30	176 (2)
C2—C3—C4—H2	−173 (4)	N2—C26—C31—C35	−3 (4)
H1—C3—C4—C5	−179 (5)	C27—C26—C31—C30	−4 (4)
H1—C3—C4—H2	10 (6)	C27—C26—C31—C35	178 (2)
C3—C4—C5—C6	−12 (*)	C26—C27—C28—C29	2 (4)
C3—C4—C5—H3	−167 (5)	C26—C27—C28—H24	−174 (3)
H2—C4—C5—C6	158 (7)	C32—C27—C28—C29	−176 (3)
H2—C4—C5—H3	2 (11)	C32—C27—C28—H24	8 (4)
C4—C5—C6—C7	171 (7)	C26—C27—C32—C33	118 (3)
C4—C5—C6—C12	24 (11)	C26—C27—C32—C34	−118 (3)
H3—C5—C6—C7	−33 (13)	C26—C27—C32—H27	−2 (4)
H3—C5—C6—C12	−180 (6)	C28—C27—C32—C33	−63 (3)
C5—C6—C7—C8	−157 (7)	C28—C27—C32—C34	61 (3)
C5—C6—C7—H4	16 (13)	C28—C27—C32—H27	177 (3)
C12—C6—C7—C8	−9 (12)	C27—C28—C29—C30	−8 (5)
C12—C6—C7—H4	163 (7)	C27—C28—C29—H25	−163 (3)
C5—C6—C12—C2	−24 (10)	H24—C28—C29—C30	168 (3)
C5—C6—C12—C10	164 (5)	H24—C28—C29—H25	13 (5)
C7—C6—C12—C2	−174 (6)	C28—C29—C30—C31	8 (5)
C7—C6—C12—C10	14 (11)	C28—C29—C30—H26	−169 (3)
C6—C7—C8—C9	1 (10)	H25—C29—C30—C31	163 (3)
C6—C7—C8—H5	−175 (7)	H25—C29—C30—H26	−14 (5)
H4—C7—C8—C9	−171 (6)	C29—C30—C31—C26	−2 (4)
H4—C7—C8—H5	13 (*)	C29—C30—C31—C35	176 (3)
C7—C8—C9—C10	4 (7)	H26—C30—C31—C26	175 (3)
C7—C8—C9—H6	−176 (5)	H26—C30—C31—C35	−6 (4)
H5—C8—C9—C10	179 (4)	C26—C31—C35—C36	−121 (3)
H5—C8—C9—H6	0 (7)	C26—C31—C35—C37	116 (3)
C8—C9—C10—C11	179 (4)	C26—C31—C35—H34	1 (4)
C8—C9—C10—C12	0 (5)	C30—C31—C35—C36	61 (3)
H6—C9—C10—C11	−2 (5)	C30—C31—C35—C37	−62 (3)
H6—C9—C10—C12	180 (3)	C30—C31—C35—H34	−177 (2)
C9—C10—C11—N2	−5 (5)	C27—C32—C33—H28	−59 (3)
C9—C10—C11—C1	−177 (3)	C27—C32—C33—H29	58 (3)
C12—C10—C11—N2	174 (3)	C27—C32—C33—H30	177 (2)
C12—C10—C11—C1	1 (3)	C34—C32—C33—H28	178 (2)
C9—C10—C12—C2	177 (3)	C34—C32—C33—H29	−65 (3)
C9—C10—C12—C6	−10 (7)	C34—C32—C33—H30	54 (3)
C11—C10—C12—C2	−2 (4)	H27—C32—C33—H28	60 (3)
C11—C10—C12—C6	171 (6)	H27—C32—C33—H29	177 (2)
N1—C14—C15—C16	−178 (2)	H27—C32—C33—H30	−63 (3)
N1—C14—C15—C20	2 (3)	C27—C32—C34—H31	−59 (3)
C19—C14—C15—C16	2 (4)	C27—C32—C34—H32	57 (3)
C19—C14—C15—C20	−178 (2)	C27—C32—C34—H33	−180 (2)
N1—C14—C19—C18	179 (2)	C33—C32—C34—H31	66 (3)
N1—C14—C19—C23	−1 (4)	C33—C32—C34—H32	−178 (2)
C15—C14—C19—C18	0 (4)	C33—C32—C34—H33	−55 (3)
C15—C14—C19—C23	179 (2)	H27—C32—C34—H31	−175 (2)
C14—C15—C16—C17	0 (4)	H27—C32—C34—H32	−59 (3)
C14—C15—C16—H7	−176 (2)	H27—C32—C34—H33	64 (3)
C20—C15—C16—C17	180 (3)	C31—C35—C36—H35	−60 (3)
C20—C15—C16—H7	5 (4)	C31—C35—C36—H36	63 (3)
C14—C15—C20—C21	−117 (2)	C31—C35—C36—H37	179 (2)
C14—C15—C20—C22	119 (2)	C37—C35—C36—H35	64 (3)
C14—C15—C20—H10	3 (3)	C37—C35—C36—H36	−174 (2)
C16—C15—C20—C21	63 (3)	C37—C35—C36—H37	−57 (3)
C16—C15—C20—C22	−61 (3)	H34—C35—C36—H35	180 (2)
C16—C15—C20—H10	−177 (2)	H34—C35—C36—H36	−58 (3)
C15—C16—C17—C18	−2 (4)	H34—C35—C36—H37	59 (3)
C15—C16—C17—H8	−174 (3)	C31—C35—C37—H38	−60 (3)
H7—C16—C17—C18	173 (3)	C31—C35—C37—H39	59 (3)
H7—C16—C17—H8	0 (5)	C31—C35—C37—H40	−176 (2)
C17—C18—C19—C14	−2 (4)	C36—C35—C37—H38	175 (2)
C17—C18—C19—C23	178 (3)	C36—C35—C37—H39	−66 (3)
H9—C18—C19—C14	179 (2)	C36—C35—C37—H40	59 (3)
H9—C18—C19—C23	0 (4)	H34—C35—C37—H38	57 (3)
C19—C18—C17—C16	4 (5)	H34—C35—C37—H39	175 (2)
C19—C18—C17—H8	176 (3)	H34—C35—C37—H40	−60 (3)
H9—C18—C17—C16	−178 (3)

Symmetry code: (i) x, −y+1/2, z+1/2.

(Compound_2) tetrahydrofurfuryl-(N,N'-ethylene-bis(3-methyl-salicylideneiminato –N,N',O,O')-cobalt top

Crystal data top

C₂₃H₂₇CoN₂O₃	β = 96.520 (3)°
M_r = 438.41	V = 2138.1 (2) Å³
Monoclinic, P2₁/n	Z = 4
Hall symbol: -p 2yn	Synchrotron radiation, λ = 0.65051 Å
a = 16.6701 (6) Å	µ = 0.8 mm⁻¹
b = 9.4170 (4) Å	T = 293 K
c = 13.7088 (7) Å	cylinder, ? × 0.7 mm mm

Data collection top

ESRF BM16 diffractometer	Data collection mode: transmission
Radiation source: synchrotron	Scan method: continuous
Specimen mounting: capillary	2θ_min = 0.010°, 2θ_max = 30.00°, 2θ_step = 0.005°

Refinement top

R_p = 8.5	142 parameters
R_wp = 11.4	Calculated and kept fixed
R_exp = ?
χ² = 57.760	Background function: polynomal
5999 data points	Preferred orientation correction: 'Ahtee and Jarvinen'
Profile function: split-type pseudo-Voigt

Crystal data top

C₂₃H₂₇CoN₂O₃	V = 2138.1 (2) Å³
M_r = 438.41	Z = 4
Monoclinic, P2₁/n	Synchrotron radiation, λ = 0.65051 Å
a = 16.6701 (6) Å	µ = 0.8 mm⁻¹
b = 9.4170 (4) Å	T = 293 K
c = 13.7088 (7) Å	cylinder, ? × 0.7 mm mm
β = 96.520 (3)°

Data collection top

ESRF BM16 diffractometer	Scan method: continuous
Specimen mounting: capillary	2θ_min = 0.010°, 2θ_max = 30.00°, 2θ_step = 0.005°
Data collection mode: transmission

Refinement top

R_p = 8.5	5999 data points
R_wp = 11.4	142 parameters
R_exp = ?	Calculated and kept fixed
χ² = 57.760

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

	x	y	z	B_iso*/B_eq
Co	0.5091 (7)	0.6512 (9)	0.4239 (9)	*
O1	0.531 (3)	0.551 (5)	0.315 (3)	*
O2	0.395 (3)	0.637 (5)	0.377 (4)	*
O3	0.540 (4)	0.932 (5)	0.193 (3)	*
N1	0.616 (4)	0.677 (5)	0.475 (4)	*
N2	0.486 (4)	0.750 (5)	0.542 (5)	*
C1	0.599 (5)	0.502 (8)	0.294 (5)	*
C2	0.671 (4)	0.526 (9)	0.353 (5)	*
C3	0.676 (4)	0.600 (7)	0.448 (5)	*
C4	0.337 (4)	0.724 (8)	0.415 (5)	*
C5	0.349 (4)	0.796 (7)	0.504 (5)	*
C6	0.423 (4)	0.802 (7)	0.561 (5)	*
C7	0.562 (5)	0.754 (7)	0.615 (5)	*
C8	0.630 (5)	0.764 (6)	0.562 (5)	*
C9	0.603 (5)	0.433 (8)	0.203 (6)	*
C10	0.679 (5)	0.383 (7)	0.177 (5)	*
C11	0.748 (5)	0.438 (8)	0.238 (7)	*
C12	0.741 (5)	0.496 (8)	0.325 (5)	*
C13	0.534 (4)	0.387 (7)	0.138 (4)	*
C14	0.253 (5)	0.698 (8)	0.377 (5)	*
C15	0.190 (4)	0.745 (7)	0.424 (5)	*
C16	0.206 (4)	0.827 (7)	0.511 (5)	*
C17	0.285 (4)	0.863 (7)	0.543 (5)	*
C18	0.242 (5)	0.623 (7)	0.278 (6)	*
C19	0.504 (5)	0.834 (6)	0.343 (5)	*
C20	0.519 (5)	0.801 (7)	0.240 (4)	*
C21	0.508 (5)	0.917 (6)	0.097 (5)	*
C22	0.463 (4)	0.783 (5)	0.076 (5)	*
C23	0.449 (5)	0.740 (6)	0.179 (5)	*
H1	0.72884	0.61379	0.48906	*
H2	0.43276	0.90214	0.60771	*
H3	0.55768	0.84416	0.65820	*
H4	0.56422	0.67196	0.65380	*
H5	0.63725	0.87313	0.53487	*
H6	0.68218	0.74487	0.60020	*
H7	0.68471	0.34137	0.11580	*
H8	0.80489	0.39637	0.22219	*
H9	0.79623	0.51885	0.37329	*
H10	0.49656	0.33205	0.17186	*
H11	0.50302	0.48493	0.11774	*
H12	0.53528	0.34401	0.07094	*
H13	0.13313	0.73514	0.39212	*
H14	0.15992	0.85422	0.54692	*
H15	0.29630	0.90654	0.61220	*
H16	0.26695	0.69110	0.22854	*
H17	0.26302	0.53630	0.28082	*
H18	0.18150	0.62065	0.24375	*
H19	0.45160	0.86780	0.33850	*
H20	0.54797	0.88792	0.37344	*
H21	0.57209	0.73194	0.23607	*
H22	0.47607	0.99620	0.06920	*
H23	0.55818	0.91210	0.04944	*
H24	0.40989	0.79650	0.03228	*
H25	0.49384	0.70628	0.03658	*
H26	0.40026	0.76273	0.19330	*
H27	0.45486	0.62278	0.17759	*

Geometric parameters (Å, º) top

Co—O1	1.83 (5)	C10—C11	1.43 (11)
Co—N1	1.86 (6)	C11—H8	1.08 (9)
Co—N2	1.94 (6)	C11—C12	1.34 (12)
Co—O2	1.95 (5)	C12—H9	1.09 (8)
Co—C19	2.05 (6)	C13—H10	0.97 (7)
O1—C1	1.30 (9)	C13—H12	1.00 (6)
O2—C4	1.40 (9)	C13—H11	1.07 (6)
O3—C21	1.36 (8)	C14—C15	1.37 (11)
O3—C20	1.45 (8)	C14—C18	1.52 (10)
N1—C3	1.31 (9)	C15—H13	1.01 (6)
N1—C8	1.44 (9)	C15—C16	1.42 (9)
N2—C6	1.22 (10)	C16—H14	0.99 (8)
N2—C7	1.52 (9)	C16—C17	1.38 (10)
C1—C2	1.38 (10)	C17—H15	1.03 (7)
C1—C9	1.42 (11)	C18—H17	0.88 (7)
C2—C12	1.31 (11)	C18—H16	1.05 (8)
C2—C3	1.46 (10)	C18—H18	1.07 (8)
C3—H1	1.00 (6)	C19—H19	0.93 (8)
C4—C5	1.39 (10)	C19—H20	0.95 (7)
C4—C14	1.46 (11)	C19—C20	1.49 (9)
C5—C6	1.39 (9)	C20—H21	1.10 (8)
C5—C17	1.40 (10)	C20—C23	1.48 (10)
C6—H2	1.14 (7)	C21—H22	0.97 (7)
C7—H4	0.94 (7)	C21—H23	1.12 (9)
C7—H3	1.04 (7)	C21—C22	1.48 (9)
C7—C8	1.42 (11)	C22—H24	1.01 (7)
C8—H6	0.98 (7)	C22—H25	1.07 (6)
C8—H5	1.10 (6)	C22—C23	1.52 (10)
C9—C13	1.43 (10)	C23—H26	0.88 (8)
C9—C10	1.44 (11)	C23—H27	1.11 (6)
C10—H7	0.94 (7)

N1···H1	1.95 (6)	C1···C19	3.60 (10)
C20···H19	1.96 (7)	C5···C19	3.61 (11)
N2···H2	1.96 (6)	C6···C16	3.61 (10)
C8···H4	1.96 (8)	O2···N1	3.61 (7)
C9···H11	1.98 (7)	C10···C16	3.61 (10)
O3···H22	1.99 (5)	N1···C20	3.63 (8)
C9···H10	2.01 (7)	O1···C10	3.65 (9)
C20···H20	2.01 (6)	C2···C5	3.65 (10)
C22···H22	2.02 (5)	N2···C1	3.67 (10)
C22···H26	2.03 (7)	C13···C23	3.68 (9)
O3···H21	2.03 (4)	C19···C22	3.68 (9)
O3···H23	2.03 (5)	O2···C15	3.68 (8)
C8···H3	2.03 (8)	C11···C13	3.70 (11)
N2···H4	2.03 (6)	C6···C14	3.70 (10)
C14···H17	2.03 (7)	C2···C6	3.71 (10)
N1···H6	2.04 (6)	C5···C7	3.72 (10)
N1···H5	2.04 (5)	C7···C18	3.73 (10)
C7···H6	2.04 (8)	O3···C12	3.74 (10)
C20···H26	2.05 (8)	O2···C17	3.74 (9)
C16···H15	2.06 (7)	N1···C6	3.75 (10)
C22···H23	2.07 (7)	C2···C8	3.75 (10)
C14···H13	2.07 (8)	C21···C22	3.75 (9)
C22···H27	2.07 (6)	O2···C7	3.76 (8)
C14···H16	2.07 (7)	C2···C13	3.76 (9)
C11···H7	2.08 (8)	C5···C18	3.76 (10)
N2···H3	2.08 (6)	C3···C19	3.77 (9)
C2···H9	2.08 (7)	O1···C6	3.77 (8)
C15···H14	2.08 (7)	O1···N2	3.77 (8)
C5···H15	2.09 (7)	C3···C9	3.79 (10)
C12···H8	2.09 (8)	C9···C20	3.79 (10)
C7···H5	2.09 (7)	C3···C14	3.79 (9)
C11···H9	2.09 (9)	Co···N2	3.80 (5)
C17···H14	2.09 (7)	O2···N1	3.81 (7)
C9···H7	2.10 (8)	C11···C16	3.81 (11)
C21···H24	2.10 (8)	C3···C5	3.82 (9)
C16···H13	2.11 (7)	C2···C20	3.82 (10)
C23···H24	2.11 (7)	C7···C19	3.82 (9)
C23···H21	2.11 (7)	C12···C16	3.82 (10)
C10···H8	2.12 (7)	N2···C3	3.82 (10)
C20···H27	2.12 (7)	C6···C19	3.82 (9)
C5···H2	2.13 (7)	C16···C18	3.83 (10)
C21···H25	2.15 (6)	C9···C23	3.85 (10)
C2···H1	2.16 (7)	C12···C17	3.88 (10)
O1···H21	2.17 (5)	C10···C12	3.88 (11)
C19···H21	2.17 (7)	O2···C8	3.90 (8)
C9···H12	2.18 (7)	C4···C23	3.92 (11)
C14···H18	2.19 (7)	C1···C7	3.92 (11)
C23···H25	2.19 (7)	O2···C1	3.93 (9)
C20···C21	2.23 (9)	O1···O3	3.97 (6)
C21···C23	2.30 (10)	C2···C4	3.97 (10)
C2···C11	2.31 (12)	C13···C15	3.97 (9)
C3···C12	2.32 (11)	C13···C22	3.97 (8)
N2···C5	2.33 (9)	C2···C17	3.97 (10)
N1···C7	2.33 (10)	C1···C5	3.97 (10)
O1···C9	2.34 (9)	C6···C9	3.98 (10)
O1···C2	2.34 (9)	O1···C4	3.99 (9)
C20···C22	2.35 (9)	O1···C22	4.00 (8)
C1···C12	2.35 (11)	C18···C23	4.00 (12)
O3···C23	2.35 (8)	C2···C19	4.00 (10)
C6···C17	2.36 (10)	C9···C16	4.00 (11)
N2···C8	2.38 (10)	Co···C7	4.01 (7)
C3···C8	2.38 (10)	C5···C12	4.01 (10)
C6···C7	2.39 (10)	O1···C11	4.02 (11)
O3···C19	2.39 (8)	Co···O2	4.05 (5)
O3···C22	2.39 (8)	N2···C2	4.06 (10)
C5···C14	2.41 (10)	Co···N1	4.07 (6)
C2···C9	2.41 (10)	C11···C20	4.07 (12)
C9···C11	2.41 (11)	C7···C19	4.09 (9)
C15···C17	2.41 (9)	C3···C10	4.10 (10)
C14···C16	2.41 (10)	C3···C20	4.10 (9)
C5···C16	2.41 (10)	N1···C4	4.11 (9)
C10···C12	2.42 (10)	O1···C8	4.11 (8)
O2···C14	2.42 (10)	C8···C17	4.11 (10)
C10···C13	2.42 (10)	Co···C9	4.11 (8)
C4···C17	2.43 (10)	C3···C6	4.12 (9)
N1···C2	2.43 (10)	C7···C13	4.13 (10)
C4···C6	2.44 (10)	C4···C20	4.15 (11)
Co···H20	2.443 (9)	C6···C15	4.15 (9)
C1···C10	2.47 (11)	C13···C20	4.16 (9)
C4···C15	2.48 (10)	C12···C15	4.17 (9)
O2···C5	2.48 (9)	Co···O1	4.17 (5)
Co···H19	2.489 (10)	O2···C7	4.19 (8)
C19···C23	2.49 (9)	C12···C13	4.19 (10)
C4···C18	2.50 (10)	O3···C6	4.19 (8)
C1···C3	2.51 (9)	Co···O3	4.20 (5)
C1···C13	2.53 (9)	C11···C17	4.21 (11)
C15···C18	2.54 (10)	C3···C15	4.21 (9)
N1···N2	2.55 (9)	O3···C21	4.21 (8)
O1···C20	2.57 (8)	O2···C16	4.21 (9)
O1···O2	2.64 (8)	N2···C19	4.22 (8)
O2···C19	2.68 (9)	C2···C16	4.22 (10)
O1···C19	2.73 (7)	C12···C17	4.23 (10)
O2···C18	2.74 (9)	C2···C10	4.24 (11)
C1···C11	2.74 (12)	O2···N2	4.24 (7)
O1···N1	2.74 (7)	C11···C16	4.24 (11)
C9···C12	2.76 (10)	C3···C10	4.24 (10)
C14···C17	2.76 (9)	C11···C12	4.25 (11)
C2···C10	2.79 (10)	O2···C2	4.26 (9)
O2···N2	2.79 (8)	Co···C14	4.26 (8)
C5···C15	2.79 (9)	C5···C8	4.26 (9)
Co···C3	2.80 (7)	C10···C22	4.26 (9)
Co···C8	2.81 (7)	N2···C3	4.27 (9)
O1···C23	2.81 (8)	N2···C20	4.27 (9)
Co···C1	2.83 (8)	C12···C21	4.27 (12)
Co···C7	2.83 (7)	C17···C18	4.27 (10)
C4···C16	2.84 (11)	N2···C14	4.29 (10)
N1···C19	2.86 (8)	C7···C9	4.29 (11)
Co···C6	2.87 (7)	C9···C22	4.29 (9)
N2···C4	2.87 (9)	C16···C21	4.30 (11)
O1···C13	2.89 (8)	C13···C21	4.31 (9)
O1···C3	2.89 (8)	N2···C9	4.31 (10)
N2···C19	2.89 (9)	C13···C16	4.32 (10)
Co···C20	2.91 (6)	C2···C14	4.32 (10)
Co···C4	2.94 (7)	C6···C12	4.33 (11)
O2···C6	2.96 (8)	C2···C11	4.34 (11)
N1···C1	2.96 (9)	C15···C21	4.34 (11)
C21···C21	3.07 (9)	C9···C22	4.35 (10)
O2···C23	3.11 (9)	O3···C1	4.35 (9)
C1···C20	3.16 (10)	O3···C13	4.35 (8)
Co···C2	3.19 (8)	C3···C11	4.36 (11)
C4···C19	3.23 (11)	N1···N2	4.36 (7)
Co···C5	3.30 (7)	N1···C9	4.36 (9)
O2···C20	3.33 (9)	C13···C13	4.36 (8)
C13···C22	3.34 (9)	C16···C22	4.37 (11)
C11···C17	3.37 (11)	C3···C18	4.38 (10)
C6···C19	3.44 (10)	C9···C17	4.38 (11)
O1···C7	3.45 (8)	C4···C7	4.38 (10)
C3···C7	3.46 (10)	C1···C8	4.40 (10)
C6···C8	3.46 (11)	Co···C3	4.40 (7)
C19···C21	3.46 (10)	C3···C17	4.41 (10)
O1···N2	3.48 (7)	Co···C6	4.41 (6)
Co···C23	3.49 (7)	C1···C22	4.42 (9)
C8···C18	3.50 (10)	C1···C17	4.42 (10)
N1···C12	3.52 (10)	C2···C15	4.43 (9)
C8···C19	3.52 (10)	C13···C16	4.43 (10)
N2···C17	3.52 (10)	C4···C12	4.44 (11)
C1···C6	3.53 (10)	C11···C21	4.44 (12)
O1···C12	3.53 (10)	Co···C12	4.48 (9)
Co···Co	3.564 (14)	Co···C8	4.56 (7)
O3···C11	3.57 (10)	Co···C18	4.67 (8)
O2···C3	3.57 (9)	Co···C1	4.68 (8)
C3···C11	3.58 (11)	Co···C17	4.70 (8)
C1···C23	3.59 (10)	Co···C13	4.70 (6)
C10···C17	3.59 (10)	Co···C4	4.76 (7)
C3···C4	3.60 (10)	Co···C2	4.82 (8)

O1—Co—N1	96 (3)	H9—C12—C2	120 (7)
O1—Co—N2	178 (2)	H9—C12—C11	118 (8)
O1—Co—O2	88 (2)	C2—C12—C11	121 (7)
O1—Co—C19	89 (2)	H10—C13—H12	108 (6)
N1—Co—N2	84 (3)	H10—C13—H11	105 (6)
N1—Co—O2	175 (2)	H10—C13—C9	112 (6)
N1—Co—C19	94 (3)	H12—C13—H11	100 (5)
N2—Co—O2	92 (2)	H12—C13—C9	126 (7)
N2—Co—C19	93 (2)	H11—C13—C9	103 (5)
O2—Co—C19	84 (3)	C15—C14—C4	122 (6)
C1—O1—Co	129 (5)	C15—C14—C18	123 (7)
C4—O2—Co	121 (4)	C4—C14—C18	114 (7)
C21—O3—C20	105 (5)	H13—C15—C14	120 (6)
C3—N1—C8	120 (6)	H13—C15—C16	120 (6)
C3—N1—Co	123 (4)	C14—C15—C16	119 (6)
C8—N1—Co	116 (5)	H14—C16—C17	123 (7)
C6—N2—C7	121 (6)	H14—C16—C15	118 (6)
C6—N2—Co	129 (5)	C17—C16—C15	119 (7)
C7—N2—Co	109 (5)	H15—C17—C16	118 (7)
O1—C1—C2	122 (7)	H15—C17—C5	118 (6)
O1—C1—C9	119 (6)	C16—C17—C5	120 (6)
C2—C1—C9	119 (7)	H17—C18—H16	114 (9)
C12—C2—C1	122 (7)	H17—C18—H18	110 (7)
C12—C2—C3	114 (6)	H17—C18—C14	113 (7)
C1—C2—C3	124 (7)	H16—C18—H18	98 (6)
H1—C3—N1	114 (6)	H16—C18—C14	106 (6)
H1—C3—C2	121 (7)	H18—C18—C14	115 (7)
N1—C3—C2	123 (6)	H19—C19—H20	121 (7)
C5—C4—O2	125 (6)	H19—C19—C20	106 (6)
C5—C4—C14	116 (7)	H19—C19—Co	108 (5)
O2—C4—C14	116 (6)	H20—C19—C20	109 (7)
C4—C5—C6	123 (7)	H20—C19—Co	103 (5)
C4—C5—C17	121 (6)	C20—C19—Co	110 (4)
C6—C5—C17	116 (6)	H21—C20—O3	105 (6)
H2—C6—N2	113 (6)	H21—C20—C23	109 (5)
H2—C6—C5	114 (6)	H21—C20—C19	113 (5)
N2—C6—C5	127 (7)	O3—C20—C23	107 (5)
H4—C7—H3	110 (7)	O3—C20—C19	109 (5)
H4—C7—C8	111 (7)	C23—C20—C19	114 (7)
H4—C7—N2	110 (6)	H22—C21—H23	102 (6)
H3—C7—C8	110 (6)	H22—C21—O3	116 (6)
H3—C7—N2	107 (6)	H22—C21—C22	110 (7)
C8—C7—N2	109 (6)	H23—C21—O3	109 (7)
H6—C8—H5	103 (6)	H23—C21—C22	104 (5)
H6—C8—C7	115 (7)	O3—C21—C22	114 (5)
H6—C8—N1	113 (6)	H24—C22—H25	103 (5)
H5—C8—C7	111 (6)	H24—C22—C21	113 (5)
H5—C8—N1	105 (6)	H24—C22—C23	112 (7)
C7—C8—N1	109 (6)	H25—C22—C21	114 (7)
C1—C9—C13	125 (7)	H25—C22—C23	115 (5)
C1—C9—C10	119 (6)	C21—C22—C23	100 (5)
C13—C9—C10	115 (6)	H26—C23—H27	110 (6)
H7—C10—C11	122 (8)	H26—C23—C20	118 (6)
H7—C10—C9	122 (7)	H26—C23—C22	112 (6)
C11—C10—C9	114 (7)	H27—C23—C20	109 (6)
H8—C11—C12	119 (8)	H27—C23—C22	103 (5)
H8—C11—C10	115 (7)	C20—C23—C22	103 (6)
C12—C11—C10	122 (8)

O2—Co—O1—C1	−174 (6)	C4—C5—C6—N2	2 (12)
N1—Co—O1—C1	8 (6)	C4—C5—C6—H2	151 (7)
N2—Co—O1—C1	−82 (66)	C17—C5—C6—N2	179 (7)
C19—Co—O1—C1	102 (6)	C17—C5—C6—H2	−32 (9)
O1—Co—O2—C4	−164 (5)	C4—C5—C17—C16	19 (10)
N1—Co—O2—C4	−7 (32)	C4—C5—C17—H15	174 (6)
N2—Co—O2—C4	18 (5)	C6—C5—C17—C16	−159 (6)
C19—Co—O2—C4	−75 (5)	C6—C5—C17—H15	−3 (*)
O1—Co—N1—C3	−19 (6)	N2—C7—C8—N1	−38 (7)
O1—Co—N1—C8	176 (4)	N2—C7—C8—H5	77 (7)
O2—Co—N1—C3	−176 (27)	N2—C7—C8—H6	−166 (5)
O2—Co—N1—C8	18 (32)	H3—C7—C8—N1	−155 (5)
N2—Co—N1—C3	159 (6)	H3—C7—C8—H5	−40 (8)
N2—Co—N1—C8	−7 (4)	H3—C7—C8—H6	77 (7)
C19—Co—N1—C3	−108 (6)	H4—C7—C8—N1	82 (7)
C19—Co—N1—C8	86 (5)	H4—C7—C8—H5	−162 (6)
O1—Co—N2—C6	−103 (64)	H4—C7—C8—H6	−46 (9)
O1—Co—N2—C7	76 (65)	C1—C9—C10—C11	−13 (10)
O2—Co—N2—C6	−12 (6)	C1—C9—C10—H7	−176 (7)
O2—Co—N2—C7	167 (4)	C13—C9—C10—C11	175 (6)
N1—Co—N2—C6	166 (6)	C13—C9—C10—H7	12 (11)
N1—Co—N2—C7	−15 (4)	C1—C9—C13—H10	−51 (*)
C19—Co—N2—C6	72 (6)	C1—C9—C13—H11	62 (9)
C19—Co—N2—C7	−108 (4)	C1—C9—C13—H12	175 (7)
O1—Co—C19—C20	0 (5)	C10—C9—C13—H10	120 (7)
O1—Co—C19—H19	115 (5)	C10—C9—C13—H11	−127 (6)
O1—Co—C19—H20	−116 (5)	C10—C9—C13—H12	−14 (10)
O2—Co—C19—C20	−88 (5)	C9—C10—C11—C12	17 (11)
O2—Co—C19—H19	26 (5)	C9—C10—C11—H8	176 (7)
O2—Co—C19—H20	156 (5)	H7—C10—C11—C12	−179 (7)
N1—Co—C19—C20	96 (5)	H7—C10—C11—H8	−21 (11)
N1—Co—C19—H19	−149 (5)	C10—C11—C12—C2	−11 (12)
N1—Co—C19—H20	−20 (5)	C10—C11—C12—H9	170 (7)
N2—Co—C19—C20	−180 (5)	H8—C11—C12—C2	−169 (8)
N2—Co—C19—H19	−65 (5)	H8—C11—C12—H9	12 (12)
N2—Co—C19—H20	64 (5)	C4—C14—C15—C16	3 (10)
Co—O1—C1—C2	−3 (11)	C4—C14—C15—H13	173 (6)
Co—O1—C1—C9	−177 (5)	C18—C14—C15—C16	−174 (6)
Co—O2—C4—C5	−19 (9)	C18—C14—C15—H13	−4 (10)
Co—O2—C4—C14	−177 (5)	C4—C14—C18—H16	−62 (8)
C21—O3—C20—C19	−146 (6)	C4—C14—C18—H17	64 (*)
C21—O3—C20—C23	−22 (8)	C4—C14—C18—H18	−169 (6)
C21—O3—C20—H21	93 (6)	C15—C14—C18—H16	115 (8)
C20—O3—C21—C22	2 (9)	C15—C14—C18—H17	−120 (9)
C20—O3—C21—H22	131 (8)	C15—C14—C18—H18	8 (*)
C20—O3—C21—H23	−114 (6)	C14—C15—C16—C17	3 (*)
Co—N1—C3—C2	24 (9)	C14—C15—C16—H14	−176 (6)
Co—N1—C3—H1	−170 (5)	H13—C15—C16—C17	−167 (6)
C8—N1—C3—C2	−170 (6)	H13—C15—C16—H14	14 (*)
C8—N1—C3—H1	−5 (9)	C15—C16—C17—C5	−14 (*)
Co—N1—C8—C7	28 (6)	C15—C16—C17—H15	−169 (6)
Co—N1—C8—H5	−92 (6)	H14—C16—C17—C5	166 (6)
Co—N1—C8—H6	157 (5)	H14—C16—C17—H15	10 (11)
C3—N1—C8—C7	−138 (6)	Co—C19—C20—O3	−163 (5)
C3—N1—C8—H5	102 (7)	Co—C19—C20—C23	78 (6)
C3—N1—C8—H6	−9 (9)	Co—C19—C20—H21	−47 (7)
Co—N2—C6—C5	4 (11)	H19—C19—C20—O3	81 (7)
Co—N2—C6—H2	−145 (5)	H19—C19—C20—C23	−38 (7)
C7—N2—C6—C5	−175 (6)	H19—C19—C20—H21	−163 (6)
C7—N2—C6—H2	35 (9)	H20—C19—C20—O3	−51 (8)
Co—N2—C7—C8	33 (6)	H20—C19—C20—C23	−170 (5)
Co—N2—C7—H3	152 (5)	H20—C19—C20—H21	65 (7)
Co—N2—C7—H4	−88 (7)	O3—C20—C23—C22	33 (7)
C6—N2—C7—C8	−147 (6)	O3—C20—C23—H26	−91 (8)
C6—N2—C7—H3	−28 (9)	O3—C20—C23—H27	142 (6)
C6—N2—C7—H4	91 (8)	C19—C20—C23—C22	153 (5)
O1—C1—C2—C3	4 (12)	C19—C20—C23—H26	29 (9)
O1—C1—C2—C12	−170 (7)	C19—C20—C23—H27	−98 (7)
C9—C1—C2—C3	179 (7)	H21—C20—C23—C22	−79 (6)
C9—C1—C2—C12	5 (12)	H21—C20—C23—H26	156 (6)
O1—C1—C9—C10	178 (7)	H21—C20—C23—H27	30 (8)
O1—C1—C9—C13	−12 (11)	O3—C21—C22—C23	18 (8)
C2—C1—C9—C10	3 (11)	O3—C21—C22—H24	136 (7)
C2—C1—C9—C13	173 (7)	O3—C21—C22—H25	−106 (7)
C1—C2—C3—N1	−16 (12)	H22—C21—C22—C23	−115 (7)
C1—C2—C3—H1	179 (7)	H22—C21—C22—H24	4 (*)
C12—C2—C3—N1	158 (7)	H22—C21—C22—H25	122 (7)
C12—C2—C3—H1	−6 (11)	H23—C21—C22—C23	137 (6)
C1—C2—C12—C11	−1 (13)	H23—C21—C22—H24	−105 (7)
C1—C2—C12—H9	178 (7)	H23—C21—C22—H25	13 (8)
C3—C2—C12—C11	−176 (7)	C21—C22—C23—C20	−30 (7)
C3—C2—C12—H9	4 (11)	C21—C22—C23—H26	99 (7)
O2—C4—C5—C6	7 (11)	C21—C22—C23—H27	−143 (6)
O2—C4—C5—C17	−170 (7)	H24—C22—C23—C20	−149 (5)
C14—C4—C5—C6	165 (7)	H24—C22—C23—H26	−21 (7)
C14—C4—C5—C17	−12 (*)	H24—C22—C23—H27	97 (6)
O2—C4—C14—C15	162 (6)	H25—C22—C23—C20	93 (6)
O2—C4—C14—C18	−21 (9)	H25—C22—C23—H26	−138 (6)
C5—C4—C14—C15	2 (10)	H25—C22—C23—H27	−20 (8)
C5—C4—C14—C18	178 (6)

Experimental details

	(Compound_1)	(Compound_2)
Crystal data
Chemical formula	C₃₇H₄₀ClN₂ORh	C₂₃H₂₇CoN₂O₃
M_r	667.07	438.41
Crystal system, space group	Orthorhombic, Pbca	Monoclinic, P2₁/n
Temperature (K)	293	293
a, b, c (Å)	21.729 (2), 27.376 (3), 11.579 (1)	16.6701 (6), 9.4170 (4), 13.7088 (7)
α, β, γ (°)	90, 90, 90	90, 96.520 (3), 90
V (Å³)	6888 (2)	2138.1 (2)
Z	8	4
Radiation type	Synchrotron, λ = 0.65296 Å	Synchrotron, λ = 0.65051 Å
µ (mm⁻¹)	0.6	0.8
Specimen shape, size (mm)	Cylinder, ? × 0.7 mm	Cylinder, ? × 0.7 mm

Data collection
Data collection method	ESRF BM16	ESRF BM16
Specimen mounting	Capillary	Capillary
Data collection mode	Transmission	Transmission
Scan method	Continuous	Continuous
2θ values (°)	2θ_min = 2.500 2θ_max = 25.00 2θ_step = 0.005	2θ_min = 0.010 2θ_max = 30.00 2θ_step = 0.005

Refinement
R factors and goodness of fit	R_p = 8.4, R_wp = 11.1, R_exp = ?, χ² = 6.250	R_p = 8.5, R_wp = 11.4, R_exp = ?, χ² = 57.760
No. of data points	4500	5999
No. of parameters	175	142
No. of restraints	38	?
H-atom treatment	Calculated and kept fixed	Calculated and kept fixed

Computer programs: UnitCell, MRIA, CHEMDRAW and PLATON.

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