Structure refinement of a twinned pseudo-symmetric crystal of [Mn(C10H24N4)(NCO)2]+·ClO_4^-

Rae, A.D.; Mossin, S.; Sørensen, H.O.

doi:10.1107/S0108768105015211

Structure refinement of a twinned pseudo-symmetric crystal of [Mn(C₁₀H₂₄N₄)(NCO)₂]⁺·ClO

The crystal studied is a 0.545 (1):0.455 twin, space group C $\bar 1$ , Z = 16, and is a commensurate occupational and displacive modulation of a Z = 4 idealized parent structure with the space group A2/a and a_p = a/2, b_p = b/2, c_p = c. A hierarchical approach to solution and refinement led sequentially to structures in the space groups A2/a, P2₁/n, $P\bar 1$ and finally $C\bar 1$ . The major and minor components of the reflection intensities could be identified using irreducible representations of A2/a and P2₁/n, which in turn suggested suitable constraints and restraints for optimizing the refinement pathway. Comparative refinement was used to show the correctness of the final structure solution and how appropriately chosen constrained refinement allowed an escape from a false minima.

Keywords: commensurately modulated structure; twinned crystal; constrained refinement; pseudo symmetry; comparative refinement.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105015211/ck5009sup1.cif Contains datablocks large, global
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768105015211/ck5009sup2.hkl Contains datablock soren

CCDC reference: 280356

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: DIRAX (Duisenberg, 1992); data reduction: EVALCCD (Duisenberg, 1998) and DREAD (Blessing, 1987); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: RAELS2000 (Rae, 2000); molecular graphics: PLATON (Spek, 1990); software used to prepare material for publication: RAELS2000 and manual editing.

Figures top

trans-dicyanato-(1,4,8,11-tetraazacyclotetradecane)mangan(III)perchlorate top

Crystal data top

C₁₂H₂₄MnN₆O₂·ClO₄	Z = 16
M_r = 438.76	F(000) = 3648
Triclinic, C1	D_x = 1.690 Mg m⁻³
a = 30.5936 (10) Å	Mo Kα radiation, λ = 0.71073 Å
b = 18.8967 (3) Å	Cell parameters from 976 reflections
c = 12.8288 (5) Å	θ = 4.0–33.3°
α = 90.180 (2)°	µ = 0.97 mm⁻¹
β = 111.561 (2)°	T = 122 K
γ = 90.083 (2)°	Block, yellow-green
V = 6897.9 (4) Å³	0.39 × 0.27 × 0.18 mm

Data collection top

Nonius KappaCCD diffractometer	17584 reflections with > 3σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.065
Graphite monochromator	θ_max = 34.7°, θ_min = 2.5°
ω scans with κ offsets	h = −48→48
152267 measured reflections	k = −30→30
27998 independent reflections	l = −20→20

Refinement top

Refinement on F	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.061	H-atom parameters constrained
S = 1.31	w = 1/[σ²(F_o) + (0.02F_o)²]
27998 reflections	(Δ/σ)_max = 0.1
497 parameters	Δρ_max = 1.00 e Å⁻³
56 restraints	Δρ_min = −1.01 e Å⁻³

Crystal data top

C₁₂H₂₄MnN₆O₂·ClO₄	γ = 90.083 (2)°
M_r = 438.76	V = 6897.9 (4) Å³
Triclinic, C1	Z = 16
a = 30.5936 (10) Å	Mo Kα radiation
b = 18.8967 (3) Å	µ = 0.97 mm⁻¹
c = 12.8288 (5) Å	T = 122 K
α = 90.180 (2)°	0.39 × 0.27 × 0.18 mm
β = 111.561 (2)°

Data collection top

Nonius KappaCCD diffractometer	17584 reflections with > 3σ(I)
152267 measured reflections	R_int = 0.065
27998 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.041	56 restraints
wR(F²) = 0.061	H-atom parameters constrained
S = 1.31	(Δ/σ)_max = 0.1
27998 reflections	Δρ_max = 1.00 e Å⁻³
497 parameters	Δρ_min = −1.01 e Å⁻³

Special details top

Refinement. Refinement of F against 17584 reflections with F² > σ(F²). The weighted R-factor wR and goodness of fit S and conventional R-factors R are based on F, with F set to zero for negative F². The 10414 reflections excluded from refinement were monitored and shown to have satisfactory agreement.

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

	x	y	z	U_iso*/U_eq
Mn1	0.50000	0.00000	0.00000	0.0068 (2)
Mn2	0.50000	0.50000	0.00000	0.0068 (2)
Mn3	0.50239 (1)	0.25084 (2)	0.50614 (3)	0.0060 (2)
Mn4	0.75000	0.25000	0.50000	0.0079 (2)
Mn5	0.75000	0.75000	0.50000	0.0072 (2)
Mn6	0.75110 (2)	0.50012 (2)	0.00344 (4)	0.0082 (2)
N11	0.4696 (1)	0.0977 (1)	−0.0230 (2)	0.0103 (2)
N12	0.5647 (1)	0.0357 (1)	0.1003 (2)	0.0111 (2)
C11	0.4181 (1)	0.0856 (1)	−0.0670 (2)	0.014 (1)
C12	0.4843 (1)	0.1450 (1)	0.0759 (2)	0.014 (1)
C13	0.5372 (1)	0.1555 (1)	0.1256 (2)	0.016 (1)
C14	0.5657 (1)	0.0916 (1)	0.1822 (2)	0.016 (1)
C15	0.5925 (1)	−0.0280 (1)	0.1537 (2)	0.015 (1)
N13	0.5194 (1)	0.0165 (1)	−0.1426 (2)	0.014 (1)
C16	0.5329 (1)	0.0447 (2)	−0.2064 (3)	0.014 (1)
O11	0.5464 (1)	0.0696 (1)	−0.2747 (2)	0.026 (1)
N21	0.4495 (1)	0.5737 (1)	−0.0695 (2)	0.012 (1)
N22	0.5501 (1)	0.5724 (1)	0.0841 (2)	0.012 (1)
C21	0.4042 (1)	0.5356 (1)	−0.1168 (2)	0.017 (1)
C22	0.4478 (1)	0.6344 (1)	0.0020 (2)	0.017 (1)
C23	0.4941 (1)	0.6736 (1)	0.0444 (3)	0.018 (1)
C24	0.5349 (1)	0.6352 (1)	0.1312 (2)	0.017 (1)
C25	0.5880 (1)	0.5322 (1)	0.1697 (2)	0.017 (1)
N23	0.5218 (1)	0.5106 (1)	−0.1410 (2)	0.014 (1)
C26	0.5332 (1)	0.5406 (2)	−0.2076 (3)	0.014 (1)
O21	0.5444 (1)	0.5680 (2)	−0.2780 (2)	0.025 (1)
N31	0.4482 (1)	0.3188 (1)	0.4278 (2)	0.009 (1)
N32	0.5458 (1)	0.3287 (1)	0.5987 (2)	0.009 (1)
C31	0.4061 (1)	0.2739 (1)	0.3733 (3)	0.011 (1)
C32	0.4396 (1)	0.3746 (1)	0.4990 (2)	0.012 (1)
C33	0.4832 (1)	0.4198 (2)	0.5532 (3)	0.013 (1)
C34	0.5236 (1)	0.3837 (2)	0.6444 (2)	0.012 (1)
C35	0.5845 (1)	0.2915 (1)	0.6881 (2)	0.012 (1)
N33	0.5284 (1)	0.2697 (1)	0.3746 (2)	0.013 (1)
C36	0.5382 (1)	0.3022 (2)	0.3084 (2)	0.012 (1)
O31	0.5493 (1)	0.3326 (1)	0.2401 (2)	0.022 (1)
N31'	0.5564 (1)	0.1830 (1)	0.5844 (2)	0.009 (1)
N32'	0.4594 (1)	0.1736 (1)	0.4114 (2)	0.009 (1)
C31'	0.5987 (1)	0.2275 (1)	0.6376 (3)	0.011 (1)
C32'	0.5652 (1)	0.1262 (1)	0.5144 (2)	0.012 (1)
C33'	0.5215 (1)	0.0817 (2)	0.4577 (3)	0.013 (1)
C34'	0.4823 (1)	0.1194 (2)	0.3658 (2)	0.012 (1)
C35'	0.4210 (1)	0.2111 (1)	0.3215 (2)	0.012 (1)
N33'	0.4765 (1)	0.2325 (1)	0.6378 (2)	0.013 (1)
C36'	0.4651 (1)	0.2054 (2)	0.7059 (2)	0.012 (1)
O31'	0.4526 (1)	0.1802 (1)	0.7762 (2)	0.022 (1)
N41	0.8035 (1)	0.3186 (1)	0.5770 (2)	0.013 (1)
N42	0.7034 (1)	0.3276 (1)	0.4213 (2)	0.012 (1)
C41	0.8467 (1)	0.2753 (1)	0.6201 (2)	0.017 (1)
C42	0.8074 (1)	0.3793 (1)	0.5086 (2)	0.018 (1)
C43	0.7632 (1)	0.4238 (1)	0.4682 (2)	0.018 (1)
C44	0.7211 (1)	0.3897 (1)	0.3788 (2)	0.016 (1)
C45	0.6640 (1)	0.2924 (1)	0.3313 (2)	0.016 (1)
N43	0.7281 (1)	0.2602 (2)	0.6408 (2)	0.015 (1)
C46	0.7168 (1)	0.2892 (2)	0.7085 (2)	0.012 (1)
O41	0.7043 (1)	0.3166 (1)	0.7769 (2)	0.022 (1)
N51	0.7826 (1)	0.8461 (1)	0.5297 (2)	0.014 (1)
N52	0.6872 (1)	0.7906 (1)	0.3979 (2)	0.013 (1)
C51	0.8335 (1)	0.8302 (2)	0.5778 (2)	0.020 (1)
C52	0.7705 (1)	0.8953 (1)	0.4334 (2)	0.021 (1)
C53	0.7182 (1)	0.9087 (2)	0.3822 (3)	0.023 (1)
C54	0.6882 (1)	0.8474 (1)	0.3200 (2)	0.021 (1)
C55	0.6582 (1)	0.7286 (2)	0.3389 (2)	0.020 (1)
N53	0.7284 (1)	0.7664 (1)	0.6397 (2)	0.014 (1)
C56	0.7150 (1)	0.7921 (2)	0.7058 (2)	0.012 (1)
O51	0.7002 (1)	0.8166 (1)	0.7721 (2)	0.022 (1)
N61	0.8059 (1)	0.5673 (1)	0.0816 (2)	0.011 (1)
N62	0.7080 (1)	0.5773 (1)	−0.0907 (2)	0.011 (1)
C61	0.8477 (1)	0.5224 (2)	0.1348 (3)	0.014 (1)
C62	0.8139 (1)	0.6241 (2)	0.0112 (3)	0.015 (1)
C63	0.7708 (1)	0.6695 (2)	−0.0450 (3)	0.016 (1)
C64	0.7304 (1)	0.6324 (2)	−0.1362 (2)	0.015 (1)
C65	0.6688 (1)	0.5416 (2)	−0.1811 (2)	0.014 (1)
N63	0.7251 (1)	0.5196 (2)	0.1349 (2)	0.015 (1)
C66	0.7150 (1)	0.5433 (2)	0.2076 (2)	0.012 (1)
O61	0.7042 (1)	0.5659 (1)	0.2822 (2)	0.022 (1)
N61'	0.6962 (1)	0.4326 (1)	−0.0745 (2)	0.011 (1)
N62'	0.7942 (1)	0.4231 (1)	0.0977 (2)	0.011 (1)
C61'	0.6546 (1)	0.4782 (2)	−0.1293 (3)	0.014 (1)
C62'	0.6880 (1)	0.3763 (2)	−0.0037 (3)	0.015 (1)
C63'	0.7311 (1)	0.3312 (2)	0.0531 (3)	0.016 (1)
C64'	0.7716 (1)	0.3684 (2)	0.1432 (2)	0.015 (1)
C65'	0.8339 (1)	0.4587 (2)	0.1872 (2)	0.014 (1)
N63'	0.7773 (1)	0.4795 (2)	−0.1277 (2)	0.015 (1)
C66'	0.7907 (1)	0.4478 (2)	−0.1888 (2)	0.013 (1)
O61'	0.8050 (1)	0.4180 (1)	−0.2522 (2)	0.022 (1)
CL1	0.6209 (1)	0.1878 (1)	−0.0222 (1)	0.013 (1)
O12	0.6244 (1)	0.1122 (1)	−0.0031 (2)	0.017 (1)
O13	0.6337 (1)	0.2256 (1)	0.0815 (2)	0.026 (1)
O14	0.6520 (1)	0.2060 (1)	−0.0792 (2)	0.025 (1)
O15	0.5736 (1)	0.2051 (2)	−0.0929 (2)	0.025 (1)
CL2	0.6195 (1)	0.6920 (1)	−0.0242 (1)	0.014 (1)
O22	0.6309 (1)	0.6209 (1)	0.0172 (3)	0.039 (1)
O23	0.6306 (1)	0.7417 (1)	0.0660 (2)	0.030 (1)
O24	0.6453 (1)	0.7078 (1)	−0.0947 (2)	0.022 (1)
O25	0.5701 (1)	0.6948 (2)	−0.0899 (3)	0.035 (1)
CL3	0.6281 (1)	0.9362 (1)	0.5243 (1)	0.012 (1)
O32	0.6215 (1)	0.8624 (1)	0.4908 (2)	0.022 (1)
O33	0.6161 (1)	0.9795 (1)	0.4265 (2)	0.028 (1)
O34	0.5975 (1)	0.9529 (1)	0.5833 (2)	0.021 (1)
O35	0.6762 (1)	0.9482 (2)	0.5955 (2)	0.024 (1)
CL4	0.6320 (1)	0.4411 (1)	0.5276 (1)	0.012 (1)
O42	0.6213 (1)	0.3682 (1)	0.4947 (2)	0.028 (1)
O43	0.6208 (1)	0.4843 (2)	0.4302 (2)	0.039 (1)
O44	0.6046 (1)	0.4628 (1)	0.5917 (2)	0.025 (1)
O45	0.6813 (1)	0.4473 (2)	0.5935 (2)	0.028 (1)
H1N11	0.4775	0.1219	−0.0830	0.013
H1N12	0.5797	0.0561	0.0499	0.013
H1C11	0.4014	0.1300	−0.1017	0.020
H2C11	0.4078	0.0708	−0.0048	0.014
H1C12	0.4738	0.1240	0.1343	0.014
H2C12	0.4690	0.1921	0.0529	0.019
H1C13	0.5441	0.1944	0.1824	0.021
H2C13	0.5477	0.1700	0.0636	0.018
H1C14	0.5990	0.1067	0.2230	0.022
H2C14	0.5526	0.0720	0.2369	0.016
H1C15	0.5836	−0.0439	0.2175	0.017
H2C15	0.6268	−0.0164	0.1821	0.021
H1N21	0.4557	0.5940	−0.1346	0.015
H1N22	0.5638	0.5905	0.0294	0.014
H1C21	0.3807	0.5655	−0.1747	0.025
H2C21	0.3923	0.5245	−0.0558	0.018
H1C22	0.4407	0.6165	0.0675	0.016
H2C22	0.4224	0.6675	−0.0427	0.024
H1C23	0.4893	0.7191	0.0786	0.025
H2C23	0.5032	0.6839	−0.0215	0.021
H1C24	0.5620	0.6687	0.1612	0.024
H2C24	0.5250	0.6195	0.1935	0.016
H1C25	0.5784	0.5211	0.2345	0.019
H2C25	0.6176	0.5609	0.1965	0.025
H1N31	0.4556	0.3430	0.3669	0.011
H1N32	0.5600	0.3528	0.5493	0.011
H1C31	0.3815	0.3014	0.3139	0.015
H2C31	0.3932	0.2574	0.4303	0.012
H1C32	0.4308	0.3519	0.5589	0.011
H2C32	0.4132	0.4054	0.4517	0.016
H1C33	0.4740	0.4623	0.5870	0.017
H2C33	0.4946	0.4351	0.4931	0.015
H1C34	0.5478	0.4202	0.6840	0.017
H2C34	0.5114	0.3613	0.6988	0.012
H1C35	0.5733	0.2762	0.7487	0.013
H2C35	0.6120	0.3241	0.7203	0.016
H1N31'	0.5493	0.1594	0.6460	0.011
H1N32'	0.4449	0.1488	0.4596	0.011
H1C31'	0.6117	0.2428	0.5800	0.012
H2C31'	0.6232	0.2001	0.6975	0.015
H1C32'	0.5909	0.0951	0.5630	0.016
H2C32'	0.5749	0.1483	0.4556	0.011
H1C33'	0.5091	0.0664	0.5162	0.015
H2C33'	0.5307	0.0392	0.4241	0.017
H1C34'	0.4957	0.1428	0.3145	0.012
H2C34'	0.4582	0.0837	0.3228	0.017
H1C35'	0.3937	0.1784	0.2872	0.016
H2C35'	0.4327	0.2277	0.2624	0.013
H1N41	0.7980	0.3384	0.6436	0.015
H1N42	0.6903	0.3459	0.4770	0.013
H1C41	0.8719	0.3023	0.6797	0.024
H2C41	0.8576	0.2638	0.5575	0.018
H1C42	0.8135	0.3610	0.4420	0.018
H2C42	0.8344	0.4098	0.5549	0.026
H1C43	0.7705	0.4688	0.4370	0.025
H2C43	0.7544	0.4348	0.5342	0.019
H1C44	0.6954	0.4255	0.3513	0.021
H2C44	0.7304	0.3742	0.3153	0.017
H1C45	0.6734	0.2814	0.2661	0.017
H2C45	0.6358	0.3238	0.3063	0.021
H1N51	0.7742	0.8701	0.5894	0.016
H1N52	0.6717	0.8107	0.4478	0.015
H1C51	0.8512	0.8733	0.6161	0.029
H2C51	0.8444	0.8153	0.5166	0.021
H1C52	0.7811	0.8743	0.3750	0.021
H2C52	0.7871	0.9413	0.4598	0.030
H1C53	0.7129	0.9488	0.3283	0.033
H2C53	0.7074	0.9226	0.4440	0.023
H1C54	0.6554	0.8644	0.2790	0.030
H2C54	0.7014	0.8281	0.2650	0.020
H1C55	0.6678	0.7132	0.2757	0.021
H2C55	0.6242	0.7417	0.3089	0.029
H1N61	0.7990	0.5910	0.1436	0.013
H1N62	0.6940	0.6019	−0.0413	0.013
H1C61	0.8724	0.5501	0.1941	0.019
H2C61	0.8602	0.5062	0.0770	0.015
H1C62	0.8233	0.6018	−0.0483	0.014
H2C62	0.8400	0.6552	0.0596	0.020
H1C63	0.7805	0.7112	−0.0794	0.021
H2C63	0.7591	0.6863	0.0140	0.018
H1C64	0.7062	0.6685	−0.1761	0.020
H2C64	0.7427	0.6098	−0.1904	0.015
H1C65	0.6794	0.5259	−0.2425	0.015
H2C65	0.6416	0.5746	−0.2121	0.019
H1N61'	0.7033	0.4084	−0.1359	0.013
H1N62'	0.8079	0.3981	0.0480	0.013
H1C61'	0.6417	0.4946	−0.0722	0.015
H2C61'	0.6300	0.4505	−0.1891	0.019
H1C62'	0.6620	0.3450	−0.0519	0.020
H2C62'	0.6785	0.3989	0.0554	0.014
H1C63'	0.7427	0.3138	−0.0058	0.018
H2C63'	0.7215	0.2899	0.0884	0.021
H1C64'	0.7594	0.3915	0.1972	0.015
H2C64'	0.7957	0.3324	0.1833	0.020
H1C65'	0.8610	0.4255	0.2171	0.019
H2C65'	0.8237	0.4741	0.2495	0.015

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.0085 (3)	0.0061 (3)	0.0067 (3)	0.0007 (2)	0.0037 (3)	0.0009 (2)
Mn2	0.0076 (3)	0.0069 (3)	0.0075 (3)	0.0010 (2)	0.0044 (3)	0.0020 (2)
Mn3	0.0072 (3)	0.0050 (2)	0.0064 (3)	−0.0010 (2)	0.0033 (2)	0.0009 (2)
Mn4	0.0073 (3)	0.0086 (3)	0.0081 (3)	−0.0013 (2)	0.0030 (2)	−0.0010 (2)
Mn5	0.0073 (3)	0.0077 (3)	0.0063 (3)	0.0006 (2)	0.0020 (2)	0.0004 (2)
Mn6	0.0085 (3)	0.0081 (3)	0.0081 (3)	0.0003 (2)	0.0034 (2)	0.0002 (2)
N11	0.0126 (4)	0.0090 (3)	0.0112 (4)	0.0014 (3)	0.0066 (3)	0.0020 (3)
N12	0.0114 (4)	0.0113 (4)	0.0109 (4)	0.0007 (3)	0.0045 (3)	−0.0006 (3)
C11	0.011 (1)	0.012 (1)	0.018 (1)	0.004 (1)	0.005 (1)	0.001 (1)
C12	0.018 (1)	0.010 (1)	0.017 (1)	0.001 (1)	0.009 (1)	−0.003 (1)
C13	0.016 (1)	0.011 (1)	0.021 (1)	−0.002 (1)	0.008 (1)	−0.005 (1)
C14	0.016 (1)	0.016 (1)	0.013 (1)	−0.001 (1)	0.004 (1)	−0.006 (1)
C15	0.013 (1)	0.016 (1)	0.014 (1)	0.004 (1)	0.001 (1)	0.001 (1)
N13	0.019 (1)	0.014 (1)	0.013 (1)	0.000 (1)	0.010 (1)	0.002 (1)
C16	0.021 (1)	0.010 (1)	0.014 (1)	0.003 (1)	0.010 (1)	0.002 (1)
O11	0.042 (1)	0.021 (1)	0.025 (1)	0.003 (1)	0.025 (1)	0.009 (1)
N21	0.013 (1)	0.013 (1)	0.013 (1)	0.004 (1)	0.007 (1)	0.005 (1)
N22	0.012 (1)	0.014 (1)	0.012 (1)	−0.001 (1)	0.007 (1)	−0.001 (1)
C21	0.010 (1)	0.022 (1)	0.020 (1)	0.004 (1)	0.004 (1)	0.003 (1)
C22	0.021 (1)	0.012 (1)	0.023 (1)	0.006 (1)	0.014 (1)	0.002 (1)
C23	0.025 (1)	0.009 (1)	0.026 (1)	0.001 (1)	0.017 (1)	0.000 (1)
C24	0.021 (1)	0.014 (1)	0.019 (1)	−0.004 (1)	0.013 (1)	−0.006 (1)
C25	0.012 (1)	0.024 (1)	0.014 (1)	0.000 (1)	0.002 (1)	−0.001 (1)
N23	0.019 (1)	0.015 (1)	0.013 (1)	−0.000 (1)	0.011 (1)	0.002 (1)
C26	0.019 (1)	0.011 (1)	0.014 (1)	0.002 (1)	0.010 (1)	0.002 (1)
O21	0.041 (1)	0.023 (1)	0.022 (1)	0.001 (1)	0.024 (1)	0.009 (1)
N31	0.010 (1)	0.008 (1)	0.009 (1)	−0.001 (1)	0.005 (1)	0.002 (1)
N32	0.010 (1)	0.009 (1)	0.010 (1)	−0.001 (1)	0.004 (1)	0.000 (1)
C31	0.009 (1)	0.010 (1)	0.014 (1)	−0.001 (1)	0.003 (1)	0.000 (1)
C32	0.012 (1)	0.010 (1)	0.015 (1)	0.001 (1)	0.006 (1)	−0.002 (1)
C33	0.012 (1)	0.008 (1)	0.018 (1)	0.000 (1)	0.005 (1)	−0.002 (1)
C34	0.013 (1)	0.011 (1)	0.014 (1)	0.000 (1)	0.005 (1)	−0.004 (1)
C35	0.011 (1)	0.012 (1)	0.011 (1)	0.000 (1)	0.001 (1)	−0.001 (1)
N33	0.016 (1)	0.014 (1)	0.012 (1)	−0.001 (1)	0.008 (1)	0.002 (1)
C36	0.013 (1)	0.012 (1)	0.011 (1)	0.002 (1)	0.005 (1)	0.003 (1)
O31	0.028 (1)	0.025 (1)	0.019 (1)	0.002 (1)	0.016 (1)	0.012 (1)
N31'	0.010 (1)	0.008 (1)	0.009 (1)	−0.001 (1)	0.005 (1)	0.002 (1)
N32'	0.009 (1)	0.009 (1)	0.010 (1)	−0.001 (1)	0.004 (1)	0.000 (1)
C31'	0.009 (1)	0.010 (1)	0.014 (1)	−0.001 (1)	0.003 (1)	0.000 (1)
C32'	0.012 (1)	0.010 (1)	0.015 (1)	0.001 (1)	0.006 (1)	−0.002 (1)
C33'	0.012 (1)	0.008 (1)	0.018 (1)	0.000 (1)	0.005 (1)	−0.002 (1)
C34'	0.013 (1)	0.011 (1)	0.013 (1)	0.000 (1)	0.005 (1)	−0.004 (1)
C35'	0.011 (1)	0.012 (1)	0.010 (1)	0.000 (1)	0.001 (1)	−0.001 (1)
N33'	0.016 (1)	0.014 (1)	0.011 (1)	−0.001 (1)	0.008 (1)	0.002 (1)
C36'	0.012 (1)	0.012 (1)	0.011 (1)	0.002 (1)	0.005 (1)	0.003 (1)
O31'	0.027 (1)	0.026 (1)	0.019 (1)	0.002 (1)	0.015 (1)	0.011 (1)
N41	0.011 (1)	0.014 (1)	0.014 (1)	−0.003 (1)	0.006 (1)	−0.004 (1)
N42	0.012 (1)	0.014 (1)	0.009 (1)	0.001 (1)	0.005 (1)	0.000 (1)
C41	0.009 (1)	0.021 (1)	0.020 (1)	−0.002 (1)	0.003 (1)	−0.005 (1)
C42	0.019 (1)	0.014 (1)	0.025 (1)	−0.007 (1)	0.013 (1)	−0.002 (1)
C43	0.025 (1)	0.011 (1)	0.024 (1)	−0.002 (1)	0.014 (1)	0.000 (1)
C44	0.024 (1)	0.014 (1)	0.015 (1)	0.003 (1)	0.011 (1)	0.004 (1)
C45	0.012 (1)	0.021 (1)	0.011 (1)	0.003 (1)	0.001 (1)	−0.002 (1)
N43	0.017 (1)	0.016 (1)	0.013 (1)	0.001 (1)	0.008 (1)	0.000 (1)
C46	0.013 (1)	0.012 (1)	0.011 (1)	0.002 (1)	0.004 (1)	0.002 (1)
O41	0.030 (1)	0.024 (1)	0.016 (1)	0.006 (1)	0.013 (1)	−0.002 (1)
N51	0.017 (1)	0.012 (1)	0.015 (1)	−0.003 (1)	0.009 (1)	−0.003 (1)
N52	0.012 (1)	0.019 (1)	0.009 (1)	0.004 (1)	0.003 (1)	0.000 (1)
C51	0.013 (1)	0.023 (1)	0.024 (1)	−0.008 (1)	0.009 (1)	−0.008 (1)
C52	0.034 (1)	0.012 (1)	0.025 (1)	−0.001 (1)	0.020 (1)	0.003 (1)
C53	0.037 (1)	0.015 (1)	0.022 (1)	0.011 (1)	0.017 (1)	0.008 (1)
C54	0.027 (1)	0.024 (1)	0.011 (1)	0.013 (1)	0.007 (1)	0.008 (1)
C55	0.011 (1)	0.030 (1)	0.014 (1)	−0.001 (1)	0.000 (1)	−0.007 (1)
N53	0.017 (1)	0.016 (1)	0.011 (1)	0.002 (1)	0.007 (1)	0.000 (1)
C56	0.014 (1)	0.012 (1)	0.010 (1)	0.000 (1)	0.004 (1)	0.001 (1)
O51	0.030 (1)	0.022 (1)	0.018 (1)	0.003 (1)	0.015 (1)	−0.005 (1)
N61	0.012 (1)	0.012 (1)	0.012 (1)	0.000 (1)	0.005 (1)	−0.001 (1)
N62	0.012 (1)	0.012 (1)	0.011 (1)	0.001 (1)	0.005 (1)	0.001 (1)
C61	0.010 (1)	0.016 (1)	0.016 (1)	0.000 (1)	0.003 (1)	0.000 (1)
C62	0.015 (1)	0.013 (1)	0.019 (1)	−0.003 (1)	0.008 (1)	0.001 (1)
C63	0.017 (1)	0.011 (1)	0.021 (1)	0.000 (1)	0.008 (1)	0.002 (1)
C64	0.017 (1)	0.014 (1)	0.015 (1)	0.001 (1)	0.007 (1)	0.005 (1)
C65	0.012 (1)	0.017 (1)	0.011 (1)	0.001 (1)	0.002 (1)	0.001 (1)
N63	0.017 (1)	0.016 (1)	0.013 (1)	0.001 (1)	0.008 (1)	−0.001 (1)
C66	0.012 (1)	0.014 (1)	0.011 (1)	−0.001 (1)	0.004 (1)	−0.000 (1)
O61	0.025 (1)	0.027 (1)	0.017 (1)	−0.001 (1)	0.012 (1)	−0.008 (1)
N61'	0.012 (1)	0.012 (1)	0.012 (1)	0.000 (1)	0.005 (1)	−0.001 (1)
N62'	0.012 (1)	0.012 (1)	0.011 (1)	0.001 (1)	0.005 (1)	0.001 (1)
C61'	0.010 (1)	0.016 (1)	0.016 (1)	0.000 (1)	0.003 (1)	0.000 (1)
C62'	0.015 (1)	0.013 (1)	0.019 (1)	−0.003 (1)	0.008 (1)	0.001 (1)
C63'	0.017 (1)	0.011 (1)	0.021 (1)	0.000 (1)	0.008 (1)	0.002 (1)
C64'	0.017 (1)	0.014 (1)	0.015 (1)	0.000 (1)	0.007 (1)	0.005 (1)
C65'	0.012 (1)	0.017 (1)	0.012 (1)	0.001 (1)	0.002 (1)	0.001 (1)
N63'	0.017 (1)	0.016 (1)	0.013 (1)	0.001 (1)	0.008 (1)	−0.001 (1)
C66'	0.012 (1)	0.014 (1)	0.012 (1)	−0.001 (1)	0.004 (1)	0.000 (1)
O61'	0.026 (1)	0.026 (1)	0.019 (1)	0.000 (1)	0.013 (1)	−0.008 (1)
CL1	0.013 (1)	0.012 (1)	0.016 (1)	0.002 (1)	0.007 (1)	0.001 (1)
O12	0.022 (1)	0.013 (1)	0.022 (1)	0.004 (1)	0.013 (1)	0.004 (1)
O13	0.029 (1)	0.025 (1)	0.024 (1)	−0.002 (1)	0.011 (1)	−0.010 (1)
O14	0.032 (1)	0.016 (1)	0.041 (1)	−0.001 (1)	0.028 (1)	0.001 (1)
O15	0.019 (1)	0.029 (1)	0.025 (1)	0.012 (1)	0.005 (1)	0.004 (1)
CL2	0.015 (1)	0.012 (1)	0.018 (1)	0.001 (1)	0.009 (1)	0.003 (1)
O22	0.047 (1)	0.018 (1)	0.065 (1)	0.011 (1)	0.037 (1)	0.021 (1)
O23	0.037 (1)	0.035 (1)	0.025 (1)	−0.006 (1)	0.018 (1)	−0.011 (1)
O24	0.029 (1)	0.019 (1)	0.028 (1)	−0.001 (1)	0.022 (1)	0.001 (1)
O25	0.013 (1)	0.036 (1)	0.050 (1)	−0.002 (1)	0.007 (1)	−0.007 (1)
CL3	0.012 (1)	0.011 (1)	0.013 (1)	−0.002 (1)	0.007 (1)	0.000 (1)
O32	0.029 (1)	0.014 (1)	0.026 (1)	−0.005 (1)	0.014 (1)	−0.007 (1)
O33	0.036 (1)	0.028 (1)	0.021 (1)	−0.002 (1)	0.011 (1)	0.012 (1)
O34	0.020 (1)	0.023 (1)	0.025 (1)	0.001 (1)	0.015 (1)	−0.003 (1)
O35	0.013 (1)	0.032 (1)	0.025 (1)	−0.008 (1)	0.006 (1)	−0.002 (1)
CL4	0.014 (1)	0.012 (1)	0.013 (1)	0.000 (1)	0.008 (1)	0.002 (1)
O42	0.037 (1)	0.018 (1)	0.032 (1)	−0.006 (1)	0.017 (1)	−0.011 (1)
O43	0.046 (1)	0.044 (1)	0.028 (1)	0.003 (1)	0.015 (1)	0.023 (1)
O44	0.027 (1)	0.024 (1)	0.033 (1)	0.006 (1)	0.021 (1)	−0.002 (1)
O45	0.014 (1)	0.035 (1)	0.034 (1)	−0.005 (1)	0.008 (1)	0.003 (1)
H1N11	0.019	0.010	0.014	0.002	0.009	0.004
H1N12	0.013	0.013	0.016	−0.002	0.008	−0.002
H1C11	0.018	0.017	0.023	0.010	0.007	0.003
H2C11	0.010	0.014	0.021	0.001	0.007	−0.001
H1C12	0.016	0.013	0.015	0.001	0.009	−0.004
H2C12	0.026	0.011	0.024	0.004	0.014	−0.002
H1C13	0.023	0.015	0.027	−0.005	0.012	−0.010
H2C13	0.020	0.011	0.026	−0.004	0.013	−0.004
H1C14	0.018	0.026	0.019	−0.004	0.004	−0.011
H2C14	0.018	0.018	0.009	0.002	0.003	−0.004
H1C15	0.018	0.017	0.012	0.007	0.001	0.004
H2C15	0.012	0.027	0.020	0.004	0.000	−0.002
H1N21	0.020	0.015	0.014	0.007	0.009	0.008
H1N22	0.016	0.014	0.017	−0.004	0.012	−0.002
H1C21	0.014	0.036	0.023	0.012	0.003	0.006
H2C21	0.009	0.022	0.024	0.001	0.007	0.000
H1C22	0.017	0.013	0.022	0.003	0.013	−0.001
H2C22	0.029	0.019	0.031	0.014	0.018	0.007
H1C23	0.038	0.010	0.037	0.000	0.027	−0.002
H2C23	0.032	0.009	0.029	0.001	0.021	0.003
H1C24	0.029	0.021	0.028	−0.011	0.019	−0.013
H2C24	0.020	0.017	0.015	−0.003	0.010	−0.006
H1C25	0.015	0.027	0.011	0.002	0.000	0.001
H2C25	0.013	0.037	0.021	−0.006	0.003	−0.008
H1N31	0.014	0.010	0.011	0.001	0.006	0.004
H1N32	0.012	0.009	0.014	−0.003	0.007	0.000
H1C31	0.011	0.018	0.015	0.003	0.002	0.000
H2C31	0.008	0.011	0.017	−0.003	0.004	−0.002
H1C32	0.010	0.012	0.014	0.000	0.005	−0.004
H2C32	0.016	0.013	0.018	0.005	0.007	0.000
H1C33	0.017	0.009	0.024	0.001	0.007	−0.004
H2C33	0.017	0.007	0.021	−0.001	0.008	0.001
H1C34	0.016	0.014	0.020	−0.003	0.007	−0.009
H2C34	0.012	0.014	0.010	0.002	0.003	−0.004
H1C35	0.012	0.015	0.008	0.003	0.001	0.000
H2C35	0.012	0.018	0.016	−0.002	0.002	−0.006
H1N31'	0.014	0.010	0.010	0.001	0.006	0.004
H1N32'	0.012	0.009	0.014	−0.003	0.007	0.000
H1C31'	0.008	0.011	0.017	−0.003	0.004	−0.002
H2C31'	0.011	0.018	0.015	0.003	0.002	0.000
H1C32'	0.016	0.013	0.018	0.005	0.007	0.000
H2C32'	0.010	0.012	0.014	0.000	0.006	−0.004
H1C33'	0.017	0.007	0.021	−0.001	0.008	0.001
H2C33'	0.017	0.009	0.024	0.001	0.007	−0.004
H1C34'	0.012	0.014	0.010	0.002	0.003	−0.004
H2C34'	0.016	0.014	0.020	−0.002	0.007	−0.009
H1C35'	0.012	0.018	0.015	−0.002	0.002	−0.006
H2C35'	0.013	0.015	0.008	0.003	0.001	0.001
H1N41	0.015	0.015	0.014	−0.004	0.005	−0.006
H1N42	0.015	0.015	0.011	0.003	0.007	0.000
H1C41	0.011	0.033	0.026	−0.006	0.002	−0.009
H2C41	0.008	0.022	0.023	−0.001	0.006	−0.003
H1C42	0.018	0.015	0.026	−0.004	0.014	0.001
H2C42	0.026	0.021	0.035	−0.014	0.016	−0.006
H1C43	0.039	0.012	0.034	−0.003	0.023	0.001
H2C43	0.027	0.011	0.023	−0.002	0.013	−0.002
H1C44	0.032	0.019	0.019	0.009	0.016	0.008
H2C44	0.024	0.016	0.015	0.003	0.011	0.005
H1C45	0.015	0.023	0.010	0.003	0.000	−0.003
H2C45	0.015	0.032	0.014	0.009	0.002	0.001
H1N51	0.021	0.012	0.017	−0.003	0.011	−0.005
H1N52	0.013	0.022	0.011	0.007	0.005	0.001
H1C51	0.023	0.033	0.034	−0.018	0.015	−0.016
H2C51	0.013	0.025	0.027	−0.007	0.011	−0.007
H1C52	0.032	0.014	0.024	−0.001	0.020	0.004
H2C52	0.052	0.014	0.038	−0.008	0.032	−0.001
H1C53	0.059	0.019	0.031	0.018	0.028	0.014
H2C53	0.038	0.014	0.024	0.012	0.018	0.007
H1C54	0.033	0.041	0.014	0.023	0.007	0.012
H2C54	0.027	0.024	0.009	0.011	0.006	0.007
H1C55	0.014	0.031	0.013	−0.001	−0.001	−0.009
H2C55	0.011	0.051	0.019	0.002	−0.001	−0.009
H1N61	0.015	0.014	0.013	−0.002	0.007	−0.004
H1N62	0.014	0.012	0.014	0.003	0.008	0.001
H1C61	0.012	0.025	0.018	−0.004	0.003	−0.002
H2C61	0.009	0.016	0.018	0.002	0.004	0.002
H1C62	0.013	0.015	0.017	−0.001	0.008	0.004
H2C62	0.020	0.018	0.024	−0.008	0.010	−0.001
H1C63	0.024	0.012	0.029	−0.001	0.013	0.004
H2C63	0.021	0.010	0.024	0.000	0.011	0.000
H1C64	0.022	0.018	0.022	0.005	0.011	0.010
H2C64	0.015	0.017	0.013	0.000	0.006	0.005
H1C65	0.014	0.020	0.010	−0.001	0.001	0.000
H2C65	0.014	0.025	0.016	0.005	0.003	0.006
H1N61'	0.015	0.013	0.013	−0.002	0.007	−0.004
H1N62'	0.014	0.012	0.014	0.003	0.008	0.001
H1C61'	0.009	0.016	0.018	0.002	0.004	0.002
H2C61'	0.012	0.025	0.018	−0.004	0.003	−0.002
H1C62'	0.020	0.018	0.024	−0.008	0.010	−0.001
H2C62'	0.013	0.015	0.017	−0.001	0.008	0.004
H1C63'	0.021	0.010	0.024	0.000	0.011	0.000
H2C63'	0.024	0.012	0.028	−0.001	0.013	0.004
H1C64'	0.015	0.017	0.012	−0.001	0.006	0.005
H2C64'	0.022	0.018	0.021	0.005	0.011	0.010
H1C65'	0.014	0.025	0.016	0.005	0.003	0.006
H2C65'	0.014	0.020	0.010	−0.001	0.001	0.000

Geometric parameters (Å, º) top

Mn1—N11	2.041 (2)	CL4—O42	1.442 (1)
Mn2—N21	2.032 (2)	CL4—O43	1.427 (1)
Mn4—N41	2.033 (2)	CL4—O44	1.434 (1)
Mn5—N51	2.037 (2)	CL4—O45	1.437 (1)
Mn3—N31	2.049 (2)	N11—O31'^v	2.895 (3)
Mn3—N31'	2.044 (2)	N21—O31ⁱⁱ	2.830 (3)
Mn6—N61	2.044 (2)	N31—O21ⁱⁱ	2.942 (3)
Mn6—N61'	2.050 (2)	N31'—O11^vi	2.896 (3)
Mn1—N12	2.036 (2)	N41—O61'^vi	2.868 (3)
Mn2—N22	2.039 (2)	N51—O61^iv	2.830 (3)
Mn4—N42	2.039 (2)	N61—O51^iv	2.933 (3)
Mn5—N52	2.040 (2)	N61'—O41^v	2.970 (3)
Mn3—N32	2.041 (2)	N11—H1N11	1.000
Mn3—N32'	2.037 (2)	N12—H1N12	1.000
Mn6—N62	2.042 (2)	C11—H1C11	1.000
Mn6—N62'	2.041 (2)	C11—H2C11	1.000
Mn1—N13	2.144 (2)	C12—H1C12	1.000
Mn2—N23	2.155 (2)	C12—H2C12	1.000
Mn4—N43	2.153 (2)	C13—H1C13	1.000
Mn5—N53	2.147 (2)	C13—H2C13	1.000
Mn3—N33	2.144 (2)	C14—H1C14	1.000
Mn3—N33'	2.142 (2)	C14—H2C14	1.000
Mn6—N63	2.144 (2)	C15—H1C15	1.000
Mn6—N63'	2.148 (2)	C15—H2C15	1.000
N11—C11	1.482 (3)	N21—H1N21	1.000
N21—C21	1.477 (3)	N22—H1N22	1.000
N41—C41	1.481 (3)	C21—H1C21	1.000
N51—C51	1.481 (3)	C21—H2C21	1.000
N31—C31	1.484 (3)	C22—H1C22	1.000
N31'—C31'	1.481 (3)	C22—H2C22	1.000
N61—C61	1.478 (3)	C23—H1C23	1.000
N61'—C61'	1.485 (3)	C23—H2C23	1.000
N11—C12	1.479 (3)	C24—H1C24	1.000
N21—C22	1.478 (3)	C24—H2C24	1.000
N41—C42	1.478 (3)	C25—H1C25	1.000
N51—C52	1.483 (3)	C25—H2C25	1.000
N31—C32	1.479 (3)	N31—H1N31	1.000
N31'—C32'	1.483 (3)	N32—H1N32	1.000
N61—C62	1.483 (3)	C31—H1C31	1.000
N61'—C62'	1.482 (3)	C31—H2C31	1.000
N12—C14	1.480 (3)	C32—H1C32	1.000
N22—C24	1.481 (3)	C32—H2C32	1.000
N42—C44	1.480 (3)	C33—H1C33	1.000
N52—C54	1.477 (3)	C33—H2C33	1.000
N32—C34	1.475 (3)	C34—H1C34	1.000
N32'—C34'	1.477 (3)	C34—H2C34	1.000
N62—C64	1.480 (3)	C35—H1C35	1.000
N62'—C64'	1.477 (3)	C35—H2C35	1.000
N12—C15	1.491 (3)	N31'—H1N31'	1.000
N22—C25	1.482 (3)	N32'—H1N32'	1.000
N42—C45	1.482 (3)	C31'—H1C31'	1.000
N52—C55	1.492 (3)	C31'—H2C31'	1.000
N32—C35	1.489 (3)	C32'—H1C32'	1.000
N32'—C35'	1.492 (3)	C32'—H2C32'	1.000
N62—C65	1.487 (3)	C33'—H1C33'	1.000
N62'—C65'	1.487 (3)	C33'—H2C33'	1.000
C11—C15ⁱ	1.502 (3)	C34'—H1C34'	1.000
C21—C25ⁱⁱ	1.508 (3)	C34'—H2C34'	1.000
C41—C45ⁱⁱⁱ	1.513 (3)	C35'—H1C35'	1.000
C51—C55^iv	1.499 (3)	C35'—H2C35'	1.000
C31—C35'	1.508 (3)	N41—H1N41	1.000
C31'—C35	1.510 (3)	N42—H1N42	1.000
C61—C65'	1.513 (3)	C41—H1C41	1.000
C61'—C65	1.509 (3)	C41—H2C41	1.000
C12—C13	1.517 (3)	C42—H1C42	1.000
C22—C23	1.512 (3)	C42—H2C42	1.000
C42—C43	1.515 (3)	C43—H1C43	1.000
C52—C53	1.513 (3)	C43—H2C43	1.000
C32—C33	1.516 (3)	C44—H1C44	1.000
C32'—C33'	1.516 (3)	C44—H2C44	1.000
C62—C63	1.519 (3)	C45—H1C45	1.000
C62'—C63'	1.516 (3)	C45—H2C45	1.000
C13—C14	1.513 (3)	N51—H1N51	1.000
C23—C24	1.520 (3)	N52—H1N52	1.000
C43—C44	1.516 (3)	C51—H1C51	1.000
C53—C54	1.508 (3)	C51—H2C51	1.000
C33—C34	1.520 (3)	C52—H1C52	1.000
C33'—C34'	1.518 (3)	C52—H2C52	1.000
C63—C64	1.522 (3)	C53—H1C53	1.000
C63'—C64'	1.519 (3)	C53—H2C53	1.000
N13—C16	1.173 (3)	C54—H1C54	1.000
N23—C26	1.181 (3)	C54—H2C54	1.000
N43—C46	1.180 (3)	C55—H1C55	1.000
N53—C56	1.174 (3)	C55—H2C55	1.000
N33—C36	1.174 (3)	N61—H1N61	1.000
N33'—C36'	1.171 (3)	N62—H1N62	1.000
N63—C66	1.172 (3)	C61—H1C61	1.000
N63'—C66'	1.172 (3)	C61—H2C61	1.000
C16—O11	1.193 (3)	C62—H1C62	1.000
C26—O21	1.197 (3)	C62—H2C62	1.000
C46—O41	1.195 (3)	C63—H1C63	1.000
C56—O51	1.194 (3)	C63—H2C63	1.000
C36—O31	1.197 (2)	C64—H1C64	1.000
C36'—O31'	1.202 (2)	C64—H2C64	1.000
C66—O61	1.199 (3)	C65—H1C65	1.000
C66'—O61'	1.196 (3)	C65—H2C65	1.000
CL1—O12	1.448 (1)	N61'—H1N61'	1.000
CL1—O13	1.429 (1)	N62'—H1N62'	1.000
CL1—O14	1.439 (1)	C61'—H1C61'	1.000
CL1—O15	1.435 (1)	C61'—H2C61'	1.000
CL2—O22	1.441 (1)	C62'—H1C62'	1.000
CL2—O23	1.427 (1)	C62'—H2C62'	1.000
CL2—O24	1.433 (1)	C63'—H1C63'	1.000
CL2—O25	1.436 (1)	C63'—H2C63'	1.000
CL3—O32	1.449 (1)	C64'—H1C64'	1.000
CL3—O33	1.431 (1)	C64'—H2C64'	1.000
CL3—O34	1.439 (1)	C65'—H1C65'	1.000
CL3—O35	1.435 (1)	C65'—H2C65'	1.000

N11—Mn1—N12	94.6 (1)	N12—C15—H2C15	109.8 (2)
N11—Mn1—N12ⁱ	85.4 (1)	C11ⁱ—C15—H1C15	109.8 (2)
N11—Mn1—N13	89.8 (1)	C11ⁱ—C15—H2C15	109.8 (2)
N11—Mn1—N13ⁱ	90.2 (1)	H1C15—C15—H2C15	109.5 (2)
N12—Mn1—N13	88.9 (1)	Mn2—N21—H1N21	106.4 (1)
N12—Mn1—N13ⁱ	91.1 (1)	C21—N21—H1N21	106.4 (2)
N11—Mn1—N11ⁱ	180.0 (2)	C22—N21—H1N21	106.4 (2)
N12—Mn1—N12ⁱ	180.0 (1)	Mn2—N22—H1N22	106.6 (1)
N13—Mn1—N13ⁱ	180.0 (2)	C24—N22—H1N22	106.6 (2)
N21—Mn2—N22	94.3 (1)	C25—N22—H1N22	106.6 (2)
N21—Mn2—N22ⁱⁱ	85.7 (1)	N21—C21—H1C21	109.7 (2)
N21—Mn2—N23	89.2 (1)	N21—C21—H2C21	109.7 (2)
N21—Mn2—N23ⁱⁱ	90.8 (1)	C25ⁱⁱ—C21—H1C21	109.7 (2)
N22—Mn2—N23	88.6 (1)	C25ⁱⁱ—C21—H2C21	109.7 (2)
N22—Mn2—N23ⁱⁱ	91.4 (1)	H1C21—C21—H2C21	109.5 (2)
N23—Mn2—N23ⁱⁱ	180.0 (2)	N21—C22—H1C22	109.1 (2)
N21—Mn2—N21ⁱⁱ	180.0 (2)	N21—C22—H2C22	109.1 (2)
N22—Mn2—N22ⁱⁱ	180.0 (1)	C23—C22—H1C22	109.1 (2)
N31—Mn3—N32	94.0 (1)	C23—C22—H2C22	109.1 (2)
N31—Mn3—N33	88.6 (1)	H1C22—C22—H2C22	109.5 (3)
N31—Mn3—N32'	85.9 (1)	C22—C23—H1C23	107.8 (2)
N31—Mn3—N33'	91.4 (1)	C22—C23—H2C23	107.8 (2)
N32—Mn3—N33	89.2 (1)	C24—C23—H1C23	107.8 (2)
N32—Mn3—N31'	86.0 (1)	C24—C23—H2C23	107.8 (2)
N32—Mn3—N33'	90.5 (1)	H1C23—C23—H2C23	109.5 (2)
N33—Mn3—N31'	91.4 (1)	N22—C24—H1C24	108.7 (2)
N33—Mn3—N32'	89.8 (1)	N22—C24—H2C24	108.7 (2)
N31'—Mn3—N32'	94.1 (1)	C23—C24—H1C24	108.7 (2)
N31'—Mn3—N33'	88.6 (1)	C23—C24—H2C24	108.7 (2)
N32'—Mn3—N33'	90.5 (1)	H1C24—C24—H2C24	109.5 (2)
N31—Mn3—N31'	180.0 (1)	N22—C25—H1C25	109.8 (2)
N32—Mn3—N32'	179.0 (1)	N22—C25—H2C25	109.8 (2)
N33—Mn3—N33'	179.7 (1)	C21ⁱⁱ—C25—H1C25	109.8 (2)
N41—Mn4—N42	94.2 (1)	C21ⁱⁱ—C25—H2C25	109.8 (2)
N41—Mn4—N42ⁱⁱⁱ	85.8 (1)	H1C25—C25—H2C25	109.5 (2)
N41—Mn4—N43	88.9 (1)	Mn3—N31—H1N31	107.4 (1)
N41—Mn4—N43ⁱⁱⁱ	91.1 (1)	C31—N31—H1N31	107.4 (2)
N42—Mn4—N43	88.6 (1)	C32—N31—H1N31	107.4 (2)
N42—Mn4—N43ⁱⁱⁱ	91.4 (1)	Mn3—N32—H1N32	107.5 (1)
N41—Mn4—N41ⁱⁱⁱ	180.0 (1)	C34—N32—H1N32	107.5 (2)
N42—Mn4—N42ⁱⁱⁱ	180.0 (2)	C35—N32—H1N32	107.5 (2)
N43—Mn4—N43ⁱⁱⁱ	180.0 (2)	N31—C31—H1C31	109.9 (2)
N51—Mn5—N52	93.6 (1)	N31—C31—H2C31	109.9 (2)
N51—Mn5—N52^iv	86.4 (1)	C35'—C31—H1C31	109.9 (2)
N51—Mn5—N53	89.8 (1)	C35'—C31—H2C31	109.9 (3)
N51—Mn5—N53^iv	90.2 (1)	H1C31—C31—H2C31	109.5 (3)
N52—Mn5—N53	88.6 (1)	N31—C32—H1C32	109.1 (2)
N52—Mn5—N53^iv	91.4 (1)	N31—C32—H2C32	109.1 (2)
N51—Mn5—N51^iv	180.0 (2)	C33—C32—H1C32	109.1 (2)
N52—Mn5—N52^iv	180.0 (2)	C33—C32—H2C32	109.1 (2)
N53—Mn5—N53^iv	180.0 (2)	H1C32—C32—H2C32	109.5 (3)
N61—Mn6—N62	94.7 (1)	C32—C33—H1C33	107.9 (3)
N61—Mn6—N63	89.1 (1)	C32—C33—H2C33	107.9 (3)
N61—Mn6—N62'	85.2 (1)	C34—C33—H1C33	107.9 (2)
N61—Mn6—N63'	91.2 (1)	C34—C33—H2C33	107.9 (3)
N62—Mn6—N63	89.9 (1)	H1C33—C33—H2C33	109.5 (3)
N62—Mn6—N61'	85.4 (1)	N32—C34—H1C34	108.8 (2)
N62—Mn6—N63'	90.6 (1)	N32—C34—H2C34	108.8 (2)
N63—Mn6—N61'	90.8 (1)	C33—C34—H1C34	108.8 (2)
N63—Mn6—N62'	90.1 (1)	C33—C34—H2C34	108.8 (3)
N61'—Mn6—N62'	94.6 (1)	H1C34—C34—H2C34	109.5 (3)
N61'—Mn6—N63'	88.9 (1)	N32—C35—H1C35	109.6 (3)
N62'—Mn6—N63'	89.4 (1)	N32—C35—H2C35	109.6 (2)
N61—Mn6—N61'	179.8 (1)	C31'—C35—H1C35	109.6 (3)
N62—Mn6—N62'	179.9 (1)	C31'—C35—H2C35	109.6 (3)
N63—Mn6—N63'	179.4 (1)	H1C35—C35—H2C35	109.5 (2)
Mn1—N11—C11	106.4 (1)	Mn3—N31'—H1N31'	107.3 (1)
Mn1—N11—C12	116.3 (1)	C31'—N31'—H1N31'	107.3 (2)
C11—N11—C12	111.3 (2)	C32'—N31'—H1N31'	107.3 (2)
Mn1—N12—C14	116.4 (2)	Mn3—N32'—H1N32'	107.6 (1)
Mn1—N12—C15	106.5 (1)	C34'—N32'—H1N32'	107.6 (2)
C14—N12—C15	113.0 (2)	C35'—N32'—H1N32'	107.6 (2)
N11—C11—C15ⁱ	107.5 (2)	C35—C31'—H1C31'	109.8 (3)
N11—C12—C13	112.2 (2)	C35—C31'—H2C31'	109.8 (2)
C12—C13—C14	116.0 (2)	N31'—C31'—H1C31'	109.8 (2)
N12—C14—C13	111.8 (2)	N31'—C31'—H2C31'	109.8 (2)
N12—C15—C11ⁱ	108.2 (2)	H1C31'—C31'—H2C31'	109.5 (3)
Mn1—N13—C16	160.4 (3)	N31'—C32'—H1C32'	109.0 (2)
N13—C16—O11	176.0 (4)	N31'—C32'—H2C32'	109.0 (2)
Mn2—N21—C21	107.0 (1)	C33'—C32'—H1C32'	109.0 (2)
Mn2—N21—C22	117.0 (2)	C33'—C32'—H2C32'	109.0 (2)
C21—N21—C22	112.9 (2)	H1C32'—C32'—H2C32'	109.5 (3)
Mn2—N22—C24	117.5 (2)	C32'—C33'—H1C33'	108.2 (3)
Mn2—N22—C25	106.1 (1)	C32'—C33'—H2C33'	108.2 (3)
C24—N22—C25	112.8 (2)	C34'—C33'—H1C33'	108.2 (3)
N21—C21—C25ⁱⁱ	108.5 (2)	C34'—C33'—H2C33'	108.2 (2)
N21—C22—C23	111.0 (2)	H1C33'—C33'—H2C33'	109.5 (3)
C22—C23—C24	115.9 (2)	N32'—C34'—H1C34'	108.8 (2)
N22—C24—C23	112.5 (2)	N32'—C34'—H2C34'	108.8 (2)
N22—C25—C21ⁱⁱ	108.3 (2)	C33'—C34'—H1C34'	108.8 (3)
Mn2—N23—C26	156.7 (3)	C33'—C34'—H2C34'	108.8 (2)
N23—C26—O21	176.9 (4)	H1C34'—C34'—H2C34'	109.5 (3)
Mn3—N31—C31	106.2 (2)	C31—C35'—H1C35'	109.7 (3)
Mn3—N31—C32	116.1 (2)	C31—C35'—H2C35'	109.7 (3)
C31—N31—C32	112.0 (2)	N32'—C35'—H1C35'	109.7 (2)
Mn3—N32—C34	116.1 (2)	N32'—C35'—H2C35'	109.7 (3)
Mn3—N32—C35	105.6 (2)	H1C35'—C35'—H2C35'	109.5 (2)
C34—N32—C35	112.4 (2)	Mn4—N41—H1N41	107.1 (1)
N31—C31—C35'	107.7 (2)	C41—N41—H1N41	107.1 (2)
N31—C32—C33	110.8 (2)	C42—N41—H1N41	107.1 (2)
C32—C33—C34	115.5 (2)	Mn4—N42—H1N42	106.6 (1)
N32—C34—C33	112.1 (2)	C44—N42—H1N42	106.6 (2)
N32—C35—C31'	108.9 (2)	C45—N42—H1N42	106.6 (2)
Mn3—N33—C36	157.7 (3)	N41—C41—H1C41	109.6 (2)
N33—C36—O31	177.0 (3)	N41—C41—H2C41	109.6 (2)
Mn3—N31'—C31'	106.4 (2)	C45ⁱⁱⁱ—C41—H1C41	109.6 (2)
Mn3—N31'—C32'	116.8 (2)	C45ⁱⁱⁱ—C41—H2C41	109.6 (2)
C31'—N31'—C32'	111.4 (2)	H1C41—C41—H2C41	109.5 (3)
Mn3—N32'—C34'	115.7 (2)	N41—C42—H1C42	108.8 (2)
Mn3—N32'—C35'	105.8 (2)	N41—C42—H2C42	108.8 (2)
C34'—N32'—C35'	112.3 (2)	C43—C42—H1C42	108.8 (2)
C35—C31'—N31'	108.0 (2)	C43—C42—H2C42	108.8 (2)
N31'—C32'—C33'	111.4 (2)	H1C42—C42—H2C42	109.5 (3)
C32'—C33'—C34'	114.6 (2)	C42—C43—H1C43	108.0 (2)
N32'—C34'—C33'	112.0 (2)	C42—C43—H2C43	108.0 (2)
C31—C35'—N32'	108.4 (2)	C44—C43—H1C43	108.0 (2)
Mn3—N33'—C36'	163.3 (3)	C44—C43—H2C43	108.0 (3)
N33'—C36'—O31'	177.3 (3)	H1C43—C43—H2C43	109.5 (2)
Mn4—N41—C41	106.1 (1)	N42—C44—H1C44	108.7 (2)
Mn4—N41—C42	115.6 (2)	N42—C44—H2C44	108.7 (2)
C41—N41—C42	113.4 (2)	C43—C44—H1C44	108.7 (2)
Mn4—N42—C44	118.1 (2)	C43—C44—H2C44	108.7 (3)
Mn4—N42—C45	106.5 (1)	H1C44—C44—H2C44	109.5 (2)
C44—N42—C45	111.6 (2)	N42—C45—H1C45	110.1 (2)
N41—C41—C45ⁱⁱⁱ	108.9 (2)	N42—C45—H2C45	110.1 (2)
N41—C42—C43	112.3 (2)	C41ⁱⁱⁱ—C45—H1C45	110.1 (2)
C42—C43—C44	115.3 (2)	C41ⁱⁱⁱ—C45—H2C45	110.1 (2)
N42—C44—C43	112.4 (2)	H1C45—C45—H2C45	109.5 (2)
N42—C45—C41ⁱⁱⁱ	107.0 (2)	Mn5—N51—H1N51	107.4 (1)
Mn4—N43—C46	157.4 (3)	C51—N51—H1N51	107.4 (2)
N43—C46—O41	177.6 (4)	C52—N51—H1N51	107.4 (2)
Mn5—N51—C51	105.2 (1)	Mn5—N52—H1N52	106.8 (1)
Mn5—N51—C52	116.8 (2)	C54—N52—H1N52	106.8 (2)
C51—N51—C52	112.2 (2)	C55—N52—H1N52	106.8 (2)
Mn5—N52—C54	117.5 (2)	N51—C51—H1C51	109.6 (2)
Mn5—N52—C55	105.8 (1)	N51—C51—H2C51	109.6 (2)
C54—N52—C55	112.5 (2)	C55^iv—C51—H1C51	109.6 (2)
N51—C51—C55^iv	109.1 (2)	C55^iv—C51—H2C51	109.6 (3)
N51—C52—C53	111.6 (2)	H1C51—C51—H2C51	109.5 (3)
C52—C53—C54	116.1 (2)	N51—C52—H1C52	108.9 (2)
N52—C54—C53	111.1 (2)	N51—C52—H2C52	108.9 (2)
N52—C55—C51^iv	107.8 (2)	C53—C52—H1C52	108.9 (3)
Mn5—N53—C56	163.4 (3)	C53—C52—H2C52	108.9 (2)
N53—C56—O51	178.0 (4)	H1C52—C52—H2C52	109.5 (3)
Mn6—N61—C61	106.5 (2)	C52—C53—H1C53	107.8 (3)
Mn6—N61—C62	116.1 (2)	C52—C53—H2C53	107.8 (3)
C61—N61—C62	113.0 (2)	C54—C53—H1C53	107.8 (2)
Mn6—N62—C64	116.6 (2)	C54—C53—H2C53	107.8 (3)
Mn6—N62—C65	107.4 (2)	H1C53—C53—H2C53	109.5 (3)
C64—N62—C65	111.6 (2)	N52—C54—H1C54	109.1 (2)
N61—C61—C65'	109.2 (2)	N52—C54—H2C54	109.1 (2)
N61—C62—C63	113.0 (3)	C53—C54—H1C54	109.1 (2)
C62—C63—C64	115.1 (3)	C53—C54—H2C54	109.1 (3)
N62—C64—C63	112.4 (2)	H1C54—C54—H2C54	109.5 (2)
N62—C65—C61'	107.2 (2)	N52—C55—H1C55	109.9 (2)
Mn6—N63—C66	166.5 (3)	N52—C55—H2C55	109.9 (2)
N63—C66—O61	178.3 (4)	C51^iv—C55—H1C55	109.9 (3)
Mn6—N61'—C61'	106.0 (2)	C51^iv—C55—H2C55	109.9 (3)
Mn6—N61'—C62'	116.1 (2)	H1C55—C55—H2C55	109.5 (2)
C61'—N61'—C62'	113.7 (2)	Mn6—N61—H1N61	106.9 (2)
Mn6—N62'—C64'	116.2 (2)	C61—N61—H1N61	106.9 (2)
Mn6—N62'—C65'	107.6 (2)	C62—N61—H1N61	106.9 (2)
C64'—N62'—C65'	112.1 (2)	Mn6—N62—H1N62	106.9 (1)
C65—C61'—N61'	109.7 (2)	C64—N62—H1N62	106.9 (2)
N61'—C62'—C63'	112.8 (3)	C65—N62—H1N62	106.9 (2)
C62'—C63'—C64'	115.4 (3)	N61—C61—H1C61	109.5 (2)
N62'—C64'—C63'	113.0 (2)	N61—C61—H2C61	109.5 (3)
C61—C65'—N62'	107.3 (2)	C65'—C61—H1C61	109.5 (3)
Mn6—N63'—C66'	159.7 (3)	C65'—C61—H2C61	109.5 (3)
N63'—C66'—O61'	177.4 (3)	H1C61—C61—H2C61	109.5 (3)
O12—CL1—O13	110.8 (1)	N61—C62—H1C62	108.6 (3)
O12—CL1—O14	107.6 (1)	N61—C62—H2C62	108.6 (2)
O12—CL1—O15	109.2 (1)	C63—C62—H1C62	108.6 (3)
O13—CL1—O14	110.4 (1)	C63—C62—H2C62	108.6 (3)
O13—CL1—O15	110.0 (1)	H1C62—C62—H2C62	109.5 (3)
O14—CL1—O15	108.9 (2)	C62—C63—H1C63	108.0 (3)
O22—CL2—O23	111.0 (2)	C62—C63—H2C63	108.0 (3)
O22—CL2—O24	108.3 (1)	C64—C63—H1C63	108.0 (3)
O22—CL2—O25	108.2 (1)	C64—C63—H2C63	108.0 (3)
O23—CL2—O24	110.7 (1)	H1C63—C63—H2C63	109.5 (3)
O23—CL2—O25	109.5 (1)	N62—C64—H1C64	108.7 (2)
O24—CL2—O25	109.0 (2)	N62—C64—H2C64	108.7 (3)
O32—CL3—O33	109.2 (1)	C63—C64—H1C64	108.7 (3)
O32—CL3—O34	108.7 (1)	C63—C64—H2C64	108.7 (3)
O32—CL3—O35	109.6 (1)	H1C64—C64—H2C64	109.5 (3)
O33—CL3—O34	109.1 (1)	N62—C65—H1C65	110.0 (3)
O33—CL3—O35	110.0 (1)	N62—C65—H2C65	110.0 (2)
O34—CL3—O35	110.1 (1)	C61'—C65—H1C65	110.0 (3)
O42—CL4—O43	109.7 (2)	C61'—C65—H2C65	110.0 (3)
O42—CL4—O44	108.8 (1)	H1C65—C65—H2C65	109.5 (3)
O42—CL4—O45	108.9 (1)	Mn6—N61'—H1N61'	106.8 (2)
O43—CL4—O44	109.6 (1)	C61'—N61'—H1N61'	106.8 (2)
O43—CL4—O45	109.5 (1)	C62'—N61'—H1N61'	106.8 (2)
O44—CL4—O45	110.4 (2)	Mn6—N62'—H1N62'	106.8 (1)
Mn1—N11—H1N11	107.5 (1)	C64'—N62'—H1N62'	106.8 (2)
C11—N11—H1N11	107.5 (2)	C65'—N62'—H1N62'	106.8 (2)
C12—N11—H1N11	107.5 (2)	C65—C61'—H1C61'	109.4 (3)
Mn1—N12—H1N12	106.8 (1)	C65—C61'—H2C61'	109.4 (3)
C14—N12—H1N12	106.8 (2)	N61'—C61'—H1C61'	109.4 (3)
C15—N12—H1N12	106.8 (2)	N61'—C61'—H2C61'	109.4 (2)
N11—C11—H1C11	110.0 (2)	H1C61'—C61'—H2C61'	109.5 (3)
N11—C11—H2C11	110.0 (2)	N61'—C62'—H1C62'	108.6 (2)
C15ⁱ—C11—H1C11	110.0 (2)	N61'—C62'—H2C62'	108.6 (3)
C15ⁱ—C11—H2C11	110.0 (2)	C63'—C62'—H1C62'	108.6 (3)
H1C11—C11—H2C11	109.5 (2)	C63'—C62'—H2C62'	108.6 (3)
N11—C12—H1C12	108.8 (2)	H1C62'—C62'—H2C62'	109.5 (3)
N11—C12—H2C12	108.8 (2)	C62'—C63'—H1C63'	108.0 (3)
C13—C12—H1C12	108.8 (2)	C62'—C63'—H2C63'	108.0 (3)
C13—C12—H2C12	108.8 (2)	C64'—C63'—H1C63'	108.0 (3)
H1C12—C12—H2C12	109.5 (2)	C64'—C63'—H2C63'	108.0 (3)
C12—C13—H1C13	107.8 (2)	H1C63'—C63'—H2C63'	109.5 (3)
C12—C13—H2C13	107.8 (2)	N62'—C64'—H1C64'	108.6 (3)
C14—C13—H1C13	107.8 (2)	N62'—C64'—H2C64'	108.6 (2)
C14—C13—H2C13	107.8 (2)	C63'—C64'—H1C64'	108.6 (3)
H1C13—C13—H2C13	109.5 (2)	C63'—C64'—H2C64'	108.6 (3)
N12—C14—H1C14	108.9 (2)	H1C64'—C64'—H2C64'	109.5 (3)
N12—C14—H2C14	108.9 (2)	C61—C65'—H1C65'	110.0 (3)
C13—C14—H1C14	108.9 (2)	C61—C65'—H2C65'	110.0 (3)
C13—C14—H2C14	108.9 (2)	N62'—C65'—H1C65'	110.0 (2)
H1C14—C14—H2C14	109.5 (2)	N62'—C65'—H2C65'	110.0 (3)
N12—C15—H1C15	109.8 (2)	H1C65'—C65'—H2C65'	109.5 (3)

C15ⁱ—C11—N11—Mn1	−43.0 (2)	C45ⁱⁱⁱ—C41—N41—Mn4	−41.0 (2)
C15ⁱ—C11—N11—C12	−170.6 (2)	C45ⁱⁱⁱ—C41—N41—C42	−169.0 (2)
C13—C12—N11—Mn1	55.3 (3)	C43—C42—N41—Mn4	58.6 (3)
C13—C12—N11—C11	177.4 (2)	C43—C42—N41—C41	−178.5 (2)
C13—C14—N12—Mn1	−56.3 (3)	C43—C44—N42—Mn4	−52.6 (3)
C13—C14—N12—C15	−180.0 (2)	C43—C44—N42—C45	−176.6 (2)
C11ⁱ—C15—N12—Mn1	40.8 (2)	C41ⁱⁱⁱ—C45—N42—Mn4	42.1 (2)
C11ⁱ—C15—N12—C14	169.8 (2)	C41ⁱⁱⁱ—C45—N42—C44	172.4 (2)
C14—C13—C12—N11	−69.2 (3)	C44—C43—C42—N41	−70.9 (3)
N12—C14—C13—C12	69.5 (3)	N42—C44—C43—C42	66.8 (3)
C25ⁱⁱ—C21—N21—Mn2	−39.5 (2)	C55^iv—C51—N51—Mn5	−42.6 (2)
C25ⁱⁱ—C21—N21—C22	−169.6 (2)	C55^iv—C51—N51—C52	−170.6 (2)
C23—C22—N21—Mn2	57.5 (3)	C53—C52—N51—Mn5	56.1 (3)
C23—C22—N21—C21	−177.6 (2)	C53—C52—N51—C51	177.6 (2)
C23—C24—N22—Mn2	−52.5 (3)	C53—C54—N52—Mn5	−56.0 (3)
C23—C24—N22—C25	−176.5 (2)	C53—C54—N52—C55	−179.3 (2)
C21ⁱⁱ—C25—N22—Mn2	41.9 (2)	C51^iv—C55—N52—Mn5	40.5 (2)
C21ⁱⁱ—C25—N22—C24	171.9 (2)	C51^iv—C55—N52—C54	170.1 (2)
C24—C23—C22—N21	−70.5 (3)	C54—C53—C52—N51	−69.9 (3)
N22—C24—C23—C22	68.1 (3)	N52—C54—C53—C52	69.4 (3)
C35'—C31—N31—Mn3	−41.6 (3)	C65'—C61—N61—Mn6	−41.3 (3)
C35'—C31—N31—C32	−169.4 (2)	C65'—C61—N61—C62	−169.9 (3)
C33—C32—N31—Mn3	58.0 (3)	C63—C62—N61—Mn6	55.6 (3)
C33—C32—N31—C31	−179.8 (2)	C63—C62—N61—C61	179.1 (3)
C33—C34—N32—Mn3	−56.3 (3)	C63—C64—N62—Mn6	−55.9 (3)
C33—C34—N32—C35	−178.0 (2)	C63—C64—N62—C65	−179.8 (3)
C31'—C35—N32—Mn3	41.5 (3)	C61'—C65—N62—Mn6	40.7 (3)
C31'—C35—N32—C34	169.0 (2)	C61'—C65—N62—C64	169.7 (3)
N32'—C35'—C31—N31	57.4 (3)	N62'—C65'—C61—N61	55.0 (3)
C34—C33—C32—N31	−70.7 (3)	C64—C63—C62—N61	−69.0 (4)
N32—C34—C33—C32	70.3 (4)	N62—C64—C63—C62	68.8 (4)
N31'—C31'—C35—N32	−56.4 (3)	N61'—C61'—C65—N62	−55.3 (3)
C35—C31'—N31'—Mn3	40.9 (3)	C65—C61'—N61'—Mn6	40.6 (3)
C35—C31'—N31'—C32'	169.2 (2)	C65—C61'—N61'—C62'	169.4 (3)
C33'—C32'—N31'—Mn3	−56.2 (3)	C63'—C62'—N61'—Mn6	−55.6 (3)
C33'—C32'—N31'—C31'	−178.7 (2)	C63'—C62'—N61'—C61'	−179.0 (2)
C33'—C34'—N32'—Mn3	58.1 (3)	C63'—C64'—N62'—Mn6	55.9 (3)
C33'—C34'—N32'—C35'	179.6 (2)	C63'—C64'—N62'—C65'	−179.7 (3)
C31—C35'—N32'—Mn3	−42.3 (3)	C61—C65'—N62'—Mn6	−39.9 (3)
C31—C35'—N32'—C34'	−169.4 (2)	C61—C65'—N62'—C64'	−168.9 (3)
C34'—C33'—C32'—N31'	70.0 (3)	C64'—C63'—C62'—N61'	68.5 (4)
N32'—C34'—C33'—C32'	−71.7 (4)	N62'—C64'—C63'—C62'	−68.7 (4)

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

Experimental details

Crystal data
Chemical formula	C₁₂H₂₄MnN₆O₂·ClO₄
M_r	438.76
Crystal system, space group	Triclinic, C1
Temperature (K)	122
a, b, c (Å)	30.5936 (10), 18.8967 (3), 12.8288 (5)
α, β, γ (°)	90.180 (2), 111.561 (2), 90.083 (2)
V (Å³)	6897.9 (4)
Z	16
Radiation type	Mo Kα
µ (mm⁻¹)	0.97
Crystal size (mm)	0.39 × 0.27 × 0.18

Data collection
Diffractometer	Nonius KappaCCD diffractometer
Absorption correction	–
No. of measured, independent and observed [ > 3σ(I)] reflections	152267, 27998, 17584
R_int	0.065
(sin θ/λ)_max (Å⁻¹)	0.800

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.061, 1.31
No. of reflections	27998
No. of parameters	497
No. of restraints	56
H-atom treatment	H-atom parameters constrained
(Δ/σ)_max	0.1
Δρ_max, Δρ_min (e Å⁻³)	1.00, −1.01

Computer programs: COLLECT (Nonius, 1999), DIRAX (Duisenberg, 1992), EVALCCD (Duisenberg, 1998) and DREAD (Blessing, 1987), SHELXS97 (Sheldrick, 1990), RAELS2000 (Rae, 2000), PLATON (Spek, 1990), RAELS2000 and manual editing.

Selected geometric parameters (Å, º) top

Mn1—N11	2.041 (2)	C31—C35'	1.508 (3)
Mn2—N21	2.032 (2)	C31'—C35	1.510 (3)
Mn4—N41	2.033 (2)	C61—C65'	1.513 (3)
Mn5—N51	2.037 (2)	C61'—C65	1.509 (3)
Mn3—N31	2.049 (2)	C12—C13	1.517 (3)
Mn3—N31'	2.044 (2)	C22—C23	1.512 (3)
Mn6—N61	2.044 (2)	C42—C43	1.515 (3)
Mn6—N61'	2.050 (2)	C52—C53	1.513 (3)
Mn1—N12	2.036 (2)	C32—C33	1.516 (3)
Mn2—N22	2.039 (2)	C32'—C33'	1.516 (3)
Mn4—N42	2.039 (2)	C62—C63	1.519 (3)
Mn5—N52	2.040 (2)	C62'—C63'	1.516 (3)
Mn3—N32	2.041 (2)	C13—C14	1.513 (3)
Mn3—N32'	2.037 (2)	C23—C24	1.520 (3)
Mn6—N62	2.042 (2)	C43—C44	1.516 (3)
Mn6—N62'	2.041 (2)	C53—C54	1.508 (3)
Mn1—N13	2.144 (2)	C33—C34	1.520 (3)
Mn2—N23	2.155 (2)	C33'—C34'	1.518 (3)
Mn4—N43	2.153 (2)	C63—C64	1.522 (3)
Mn5—N53	2.147 (2)	C63'—C64'	1.519 (3)
Mn3—N33	2.144 (2)	N13—C16	1.173 (3)
Mn3—N33'	2.142 (2)	N23—C26	1.181 (3)
Mn6—N63	2.144 (2)	N43—C46	1.180 (3)
Mn6—N63'	2.148 (2)	N53—C56	1.174 (3)
N11—C11	1.482 (3)	N33—C36	1.174 (3)
N21—C21	1.477 (3)	N33'—C36'	1.171 (3)
N41—C41	1.481 (3)	N63—C66	1.172 (3)
N51—C51	1.481 (3)	N63'—C66'	1.172 (3)
N31—C31	1.484 (3)	C16—O11	1.193 (3)
N31'—C31'	1.481 (3)	C26—O21	1.197 (3)
N61—C61	1.478 (3)	C46—O41	1.195 (3)
N61'—C61'	1.485 (3)	C56—O51	1.194 (3)
N11—C12	1.479 (3)	C36—O31	1.197 (2)
N21—C22	1.478 (3)	C36'—O31'	1.202 (2)
N41—C42	1.478 (3)	C66—O61	1.199 (3)
N51—C52	1.483 (3)	C66'—O61'	1.196 (3)
N31—C32	1.479 (3)	CL1—O12	1.448 (1)
N31'—C32'	1.483 (3)	CL1—O13	1.429 (1)
N61—C62	1.483 (3)	CL1—O14	1.439 (1)
N61'—C62'	1.482 (3)	CL1—O15	1.435 (1)
N12—C14	1.480 (3)	CL2—O22	1.441 (1)
N22—C24	1.481 (3)	CL2—O23	1.427 (1)
N42—C44	1.480 (3)	CL2—O24	1.433 (1)
N52—C54	1.477 (3)	CL2—O25	1.436 (1)
N32—C34	1.475 (3)	CL3—O32	1.449 (1)
N32'—C34'	1.477 (3)	CL3—O33	1.431 (1)
N62—C64	1.480 (3)	CL3—O34	1.439 (1)
N62'—C64'	1.477 (3)	CL3—O35	1.435 (1)
N12—C15	1.491 (3)	CL4—O42	1.442 (1)
N22—C25	1.482 (3)	CL4—O43	1.427 (1)
N42—C45	1.482 (3)	CL4—O44	1.434 (1)
N52—C55	1.492 (3)	CL4—O45	1.437 (1)
N32—C35	1.489 (3)	N11—O31'^v	2.895 (3)
N32'—C35'	1.492 (3)	N21—O31ⁱⁱ	2.830 (3)
N62—C65	1.487 (3)	N31—O21ⁱⁱ	2.942 (3)
N62'—C65'	1.487 (3)	N31'—O11^vi	2.896 (3)
C11—C15ⁱ	1.502 (3)	N41—O61'^vi	2.868 (3)
C21—C25ⁱⁱ	1.508 (3)	N51—O61^iv	2.830 (3)
C41—C45ⁱⁱⁱ	1.513 (3)	N61—O51^iv	2.933 (3)
C51—C55^iv	1.499 (3)	N61'—O41^v	2.970 (3)

N11—Mn1—N12	94.6 (1)	C34—N32—C35	112.4 (2)
N11—Mn1—N12ⁱ	85.4 (1)	N31—C31—C35'	107.7 (2)
N11—Mn1—N13	89.8 (1)	N31—C32—C33	110.8 (2)
N11—Mn1—N13ⁱ	90.2 (1)	C32—C33—C34	115.5 (2)
N12—Mn1—N13	88.9 (1)	N32—C34—C33	112.1 (2)
N12—Mn1—N13ⁱ	91.1 (1)	N32—C35—C31'	108.9 (2)
N11—Mn1—N11ⁱ	180.0 (2)	Mn3—N33—C36	157.7 (3)
N12—Mn1—N12ⁱ	180.0 (1)	N33—C36—O31	177.0 (3)
N13—Mn1—N13ⁱ	180.0 (2)	Mn3—N31'—C31'	106.4 (2)
N21—Mn2—N22	94.3 (1)	Mn3—N31'—C32'	116.8 (2)
N21—Mn2—N22ⁱⁱ	85.7 (1)	C31'—N31'—C32'	111.4 (2)
N21—Mn2—N23	89.2 (1)	Mn3—N32'—C34'	115.7 (2)
N21—Mn2—N23ⁱⁱ	90.8 (1)	Mn3—N32'—C35'	105.8 (2)
N22—Mn2—N23	88.6 (1)	C34'—N32'—C35'	112.3 (2)
N22—Mn2—N23ⁱⁱ	91.4 (1)	C35—C31'—N31'	108.0 (2)
N23—Mn2—N23ⁱⁱ	180.0 (2)	N31'—C32'—C33'	111.4 (2)
N21—Mn2—N21ⁱⁱ	180.0 (2)	C32'—C33'—C34'	114.6 (2)
N22—Mn2—N22ⁱⁱ	180.0 (1)	N32'—C34'—C33'	112.0 (2)
N31—Mn3—N32	94.0 (1)	C31—C35'—N32'	108.4 (2)
N31—Mn3—N33	88.6 (1)	Mn3—N33'—C36'	163.3 (3)
N31—Mn3—N32'	85.9 (1)	N33'—C36'—O31'	177.3 (3)
N31—Mn3—N33'	91.4 (1)	Mn4—N41—C41	106.1 (1)
N32—Mn3—N33	89.2 (1)	Mn4—N41—C42	115.6 (2)
N32—Mn3—N31'	86.0 (1)	C41—N41—C42	113.4 (2)
N32—Mn3—N33'	90.5 (1)	Mn4—N42—C44	118.1 (2)
N33—Mn3—N31'	91.4 (1)	Mn4—N42—C45	106.5 (1)
N33—Mn3—N32'	89.8 (1)	C44—N42—C45	111.6 (2)
N31'—Mn3—N32'	94.1 (1)	N41—C41—C45ⁱⁱⁱ	108.9 (2)
N31'—Mn3—N33'	88.6 (1)	N41—C42—C43	112.3 (2)
N32'—Mn3—N33'	90.5 (1)	C42—C43—C44	115.3 (2)
N31—Mn3—N31'	180.0 (1)	N42—C44—C43	112.4 (2)
N32—Mn3—N32'	179.0 (1)	N42—C45—C41ⁱⁱⁱ	107.0 (2)
N33—Mn3—N33'	179.7 (1)	Mn4—N43—C46	157.4 (3)
N41—Mn4—N42	94.2 (1)	N43—C46—O41	177.6 (4)
N41—Mn4—N42ⁱⁱⁱ	85.8 (1)	Mn5—N51—C51	105.2 (1)
N41—Mn4—N43	88.9 (1)	Mn5—N51—C52	116.8 (2)
N41—Mn4—N43ⁱⁱⁱ	91.1 (1)	C51—N51—C52	112.2 (2)
N42—Mn4—N43	88.6 (1)	Mn5—N52—C54	117.5 (2)
N42—Mn4—N43ⁱⁱⁱ	91.4 (1)	Mn5—N52—C55	105.8 (1)
N41—Mn4—N41ⁱⁱⁱ	180.0 (1)	C54—N52—C55	112.5 (2)
N42—Mn4—N42ⁱⁱⁱ	180.0 (2)	N51—C51—C55^iv	109.1 (2)
N43—Mn4—N43ⁱⁱⁱ	180.0 (2)	N51—C52—C53	111.6 (2)
N51—Mn5—N52	93.6 (1)	C52—C53—C54	116.1 (2)
N51—Mn5—N52^iv	86.4 (1)	N52—C54—C53	111.1 (2)
N51—Mn5—N53	89.8 (1)	N52—C55—C51^iv	107.8 (2)
N51—Mn5—N53^iv	90.2 (1)	Mn5—N53—C56	163.4 (3)
N52—Mn5—N53	88.6 (1)	N53—C56—O51	178.0 (4)
N52—Mn5—N53^iv	91.4 (1)	Mn6—N61—C61	106.5 (2)
N51—Mn5—N51^iv	180.0 (2)	Mn6—N61—C62	116.1 (2)
N52—Mn5—N52^iv	180.0 (2)	C61—N61—C62	113.0 (2)
N53—Mn5—N53^iv	180.0 (2)	Mn6—N62—C64	116.6 (2)
N61—Mn6—N62	94.7 (1)	Mn6—N62—C65	107.4 (2)
N61—Mn6—N63	89.1 (1)	C64—N62—C65	111.6 (2)
N61—Mn6—N62'	85.2 (1)	N61—C61—C65'	109.2 (2)
N61—Mn6—N63'	91.2 (1)	N61—C62—C63	113.0 (3)
N62—Mn6—N63	89.9 (1)	C62—C63—C64	115.1 (3)
N62—Mn6—N61'	85.4 (1)	N62—C64—C63	112.4 (2)
N62—Mn6—N63'	90.6 (1)	N62—C65—C61'	107.2 (2)
N63—Mn6—N61'	90.8 (1)	Mn6—N63—C66	166.5 (3)
N63—Mn6—N62'	90.1 (1)	N63—C66—O61	178.3 (4)
N61'—Mn6—N62'	94.6 (1)	Mn6—N61'—C61'	106.0 (2)
N61'—Mn6—N63'	88.9 (1)	Mn6—N61'—C62'	116.1 (2)
N62'—Mn6—N63'	89.4 (1)	C61'—N61'—C62'	113.7 (2)
N61—Mn6—N61'	179.8 (1)	Mn6—N62'—C64'	116.2 (2)
N62—Mn6—N62'	179.9 (1)	Mn6—N62'—C65'	107.6 (2)
N63—Mn6—N63'	179.4 (1)	C64'—N62'—C65'	112.1 (2)
Mn1—N11—C11	106.4 (1)	C65—C61'—N61'	109.7 (2)
Mn1—N11—C12	116.3 (1)	N61'—C62'—C63'	112.8 (3)
C11—N11—C12	111.3 (2)	C62'—C63'—C64'	115.4 (3)
Mn1—N12—C14	116.4 (2)	N62'—C64'—C63'	113.0 (2)
Mn1—N12—C15	106.5 (1)	C61—C65'—N62'	107.3 (2)
C14—N12—C15	113.0 (2)	Mn6—N63'—C66'	159.7 (3)
N11—C11—C15ⁱ	107.5 (2)	N63'—C66'—O61'	177.4 (3)
N11—C12—C13	112.2 (2)	O12—CL1—O13	110.8 (1)
C12—C13—C14	116.0 (2)	O12—CL1—O14	107.6 (1)
N12—C14—C13	111.8 (2)	O12—CL1—O15	109.2 (1)
N12—C15—C11ⁱ	108.2 (2)	O13—CL1—O14	110.4 (1)
Mn1—N13—C16	160.4 (3)	O13—CL1—O15	110.0 (1)
N13—C16—O11	176.0 (4)	O14—CL1—O15	108.9 (2)
Mn2—N21—C21	107.0 (1)	O22—CL2—O23	111.0 (2)
Mn2—N21—C22	117.0 (2)	O22—CL2—O24	108.3 (1)
C21—N21—C22	112.9 (2)	O22—CL2—O25	108.2 (1)
Mn2—N22—C24	117.5 (2)	O23—CL2—O24	110.7 (1)
Mn2—N22—C25	106.1 (1)	O23—CL2—O25	109.5 (1)
C24—N22—C25	112.8 (2)	O24—CL2—O25	109.0 (2)
N21—C21—C25ⁱⁱ	108.5 (2)	O32—CL3—O33	109.2 (1)
N21—C22—C23	111.0 (2)	O32—CL3—O34	108.7 (1)
C22—C23—C24	115.9 (2)	O32—CL3—O35	109.6 (1)
N22—C24—C23	112.5 (2)	O33—CL3—O34	109.1 (1)
N22—C25—C21ⁱⁱ	108.3 (2)	O33—CL3—O35	110.0 (1)
Mn2—N23—C26	156.7 (3)	O34—CL3—O35	110.1 (1)
N23—C26—O21	176.9 (4)	O42—CL4—O43	109.7 (2)
Mn3—N31—C31	106.2 (2)	O42—CL4—O44	108.8 (1)
Mn3—N31—C32	116.1 (2)	O42—CL4—O45	108.9 (1)
C31—N31—C32	112.0 (2)	O43—CL4—O44	109.6 (1)
Mn3—N32—C34	116.1 (2)	O43—CL4—O45	109.5 (1)
Mn3—N32—C35	105.6 (2)	O44—CL4—O45	110.4 (2)

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

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