Quick and robust PDF data acquisition using a laboratory single-crystal X-ray diffractometer for study of polynuclear lanthanide complexes in solid form and in solution

Tsymbarenko, D.; Grebenyuk, D.; Burlakova, M.; Zobel, M.

doi:10.1107/S1600576722005878

Quick and robust PDF data acquisition using a laboratory single-crystal X-ray diffractometer for study of polynuclear lanthanide complexes in solid form and in solution

D. Tsymbarenko, D. Grebenyuk, M. Burlakova and M. Zobel

Self-assembled polynuclear lanthanide hydroxo complexes are important objects in the reticular chemistry approach to the design of various functional materials. Revealing their structure in the solid state and understanding the molecular mechanism of self-assembly in solution require a universal and reliable structural method. Pair distribution function (PDF) analysis is a powerful technique which enables structural insight for a wide range of crystalline and amorphous materials on the nanoscale, but commonly measurements are performed at synchrotron X-ray sources or on specially designed laboratory diffractometers. In the present paper, a standard Bruker D8 QUEST single-crystal X-ray diffractometer equipped with a micro-focus Mo tube and CMOS Photon III detector was adapted to measure PDF data of high quality with Q_max = 16.97 Å^–1 for solid and liquid samples. An improved data collection strategy and the original data reduction software FormagiX enable calibration and azimuthal full-frame integration of 2D frames, delivering reliable PDFs up to 80 Å with instrumental parameters Q_damp = 0.018 Å⁻¹ and Q_broad = 0.010 Å⁻¹. The effectiveness of the developed approach was demonstrated with reference samples and real-case studies of tetranuclear lanthanide hydroxocarboxylates in solid form and in solution.

Keywords: total X-ray scattering; pair distribution function; polynuclear lanthanide complexes.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600576722005878/xx5001sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600576722005878/xx5001Isup2.hkl Contains datablock I
	Portable Document Format (PDF) file https://doi.org/10.1107/S1600576722005878/xx5001sup3.pdf Supporting information reports on details of pair distribution function generation, data collection strategy, data reduction, data analysis by Rietveld method and PDF for reference samples, results of PDF analysis of \[Sm4(OH)2(piv)10(H2O)2\]∞ powder, details of total scattering study of Ln(tfa)3+deta+iPrOH solutions, experimental details and description of FormagiX v.0.5 software solution for serial frame integration.

CCDC reference: 2165227

Computing details top

Program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2018).

(I) top

Crystal data top

C₃₄H₈₀F₉N₁₈O₁₈Pr₄·3(C₂F₃O₂)·C₂HF₃O₂·6(H₂O)	F(000) = 4608
M_r = 2324.98	D_x = 1.877 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 27.6254 (9) Å	Cell parameters from 9066 reflections
b = 12.7853 (4) Å	θ = 2.6–32.8°
c = 23.5496 (8) Å	µ = 2.46 mm⁻¹
β = 98.4791 (11)°	T = 100 K
V = 8226.8 (5) Å³	Block, pale green
Z = 4	0.23 × 0.21 × 0.14 mm

Data collection top

Bruker D8 Quest with Photon III detector diffractometer	7970 reflections with I > 2σ(I)
Radiation source: Micro-focus sealed X-ray tube	R_int = 0.043
ω scans	θ_max = 27.0°, θ_min = 1.9°
Absorption correction: numerical SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	h = −35→35
T_min = 0.674, T_max = 0.958	k = −16→16
45481 measured reflections	l = −30→30
8987 independent reflections

Refinement top

Refinement on F²	103 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.050	H-atom parameters constrained
wR(F²) = 0.138	w = 1/[σ²(F_o²) + (0.0695P)² + 112.3975P] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.002
8987 reflections	Δρ_max = 2.12 e Å⁻³
520 parameters	Δρ_min = −1.32 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pr1	0.52518 (2)	0.59868 (2)	0.67320 (2)	0.02235 (10)
Pr2	0.56940 (2)	0.38722 (2)	0.79082 (2)	0.02506 (10)
N1	0.5462 (2)	0.5068 (4)	0.5773 (2)	0.0366 (12)
H1A	0.563965	0.447993	0.587370	0.044*
H1B	0.517677	0.486691	0.555675	0.044*
N2	0.5540 (3)	0.7267 (4)	0.5944 (2)	0.0501 (17)
H2A	0.589665	0.738154	0.607868	0.060*
N3	0.4745 (3)	0.7754 (4)	0.6554 (2)	0.0447 (14)
H3A	0.442332	0.761402	0.656039	0.054*
H3B	0.484671	0.820507	0.684624	0.054*
N4	0.5598 (2)	0.2850 (4)	0.8880 (2)	0.0400 (13)
H4A	0.564685	0.330890	0.917843	0.048*
H4B	0.528705	0.260346	0.885439	0.048*
N5	0.6469 (2)	0.2725 (6)	0.8361 (2)	0.0537 (17)
H5C	0.676065	0.319815	0.839306	0.064*
N6	0.6129 (2)	0.2814 (5)	0.7139 (2)	0.0453 (14)
H6C	0.591472	0.232978	0.696566	0.054*
H6D	0.619709	0.326728	0.686384	0.054*
N7	0.3785 (2)	0.6152 (5)	0.5595 (2)	0.0457 (14)
H7C	0.391421	0.668954	0.543877	0.069*
N8	0.2995 (3)	0.5835 (9)	0.6424 (3)	0.084 (3)
H8C	0.330175	0.589732	0.662234	0.101*
H8D	0.294318	0.514695	0.633487	0.101*
N9	0.3082 (2)	0.5772 (7)	0.7781 (3)	0.0611 (19)
H9C	0.304427	0.618989	0.806840	0.092*
O1	0.51756 (14)	0.4110 (3)	0.69525 (15)	0.0228 (7)
H1C	0.527403	0.364255	0.664899	0.027*
O1S	0.5464 (2)	1.2720 (5)	0.6007 (3)	0.0626 (15)*
O1W	0.6729 (9)	0.3965 (17)	0.6107 (10)	0.288 (11)*
H1W	0.650621	0.356078	0.594571	0.432*
H2W	0.657001	0.440638	0.627721	0.432*
O2	0.45394 (13)	0.5718 (3)	0.72321 (15)	0.0226 (7)
H2B	0.426315	0.618538	0.706946	0.027*
O2S	0.6007 (3)	1.2616 (6)	0.5411 (3)	0.087 (2)*
O2W	0.7586 (10)	0.467 (2)	0.5866 (11)	0.340 (13)*
H3W	0.736561	0.431620	0.599675	0.509*
H4W	0.751171	0.529480	0.593305	0.509*
O3	0.5757 (2)	0.7607 (4)	0.71682 (19)	0.0460 (12)
O3W	0.6819 (15)	1.129 (3)	0.4921 (18)	0.51 (3)*
H5W	0.654780	1.161021	0.489688	0.768*
H6W	0.683400	1.112031	0.457428	0.768*
O4	0.6244 (2)	0.7272 (5)	0.7997 (2)	0.0578 (15)
O5	0.5383 (2)	0.2015 (3)	0.7731 (2)	0.0441 (11)
O6	0.38787 (15)	0.4847 (4)	0.62335 (18)	0.0369 (10)
O7	0.45377 (15)	0.5633 (3)	0.59779 (16)	0.0298 (8)
O8	0.35716 (16)	0.4785 (4)	0.7331 (2)	0.0445 (11)
O9	0.38668 (16)	0.5545 (4)	0.81737 (19)	0.0437 (11)
O12	0.7633 (9)	0.8719 (19)	0.6268 (11)	0.140 (4)*	0.5
O12A	0.7310 (11)	0.7107 (16)	0.6275 (11)	0.140 (4)*	0.5
O13	0.7128 (8)	0.9580 (16)	0.5553 (9)	0.140 (4)*	0.5
H13	0.699195	1.016574	0.542604	0.209*	0.5
O13A	0.7552 (11)	0.8979 (17)	0.6124 (14)	0.140 (4)*	0.5
C1	0.6121 (3)	0.7728 (6)	0.7539 (3)	0.0492 (18)
C1S	0.5707 (3)	1.2280 (6)	0.5697 (3)	0.0460 (16)*
C2	0.6467 (7)	0.8546 (11)	0.7327 (6)	0.077 (4)	0.5
C2A	0.6487 (8)	0.8610 (10)	0.7472 (5)	0.077 (4)	0.5
C2S	0.5632 (4)	1.1087 (8)	0.5677 (5)	0.073 (3)*
C3	0.500000	0.1608 (7)	0.750000	0.045 (2)
C4	0.500000	0.0413 (11)	0.750000	0.093 (5)
C5	0.5734 (3)	0.5723 (6)	0.5421 (3)	0.0475 (17)
H5A	0.571794	0.541267	0.503366	0.057*
H5B	0.608162	0.575811	0.559694	0.057*
C6	0.5523 (4)	0.6793 (6)	0.5373 (3)	0.057 (2)
H6A	0.570993	0.723172	0.513523	0.069*
H6B	0.517960	0.675981	0.518115	0.069*
C7	0.5327 (4)	0.8310 (6)	0.5933 (4)	0.070 (3)
H7A	0.535821	0.865128	0.556226	0.084*
H7B	0.550909	0.873722	0.624407	0.084*
C8	0.4797 (4)	0.8264 (6)	0.6007 (4)	0.063 (2)
H8A	0.466112	0.898139	0.600170	0.076*
H8B	0.461066	0.786762	0.568538	0.076*
C9	0.5940 (4)	0.1976 (6)	0.9002 (3)	0.060 (2)
H9A	0.584253	0.139312	0.873260	0.072*
H9B	0.593580	0.171906	0.939832	0.072*
C10	0.6438 (3)	0.2349 (8)	0.8937 (3)	0.061 (2)
H10A	0.653249	0.292130	0.921473	0.074*
H10B	0.667422	0.176983	0.903013	0.074*
C11	0.6561 (4)	0.1864 (8)	0.7965 (3)	0.077 (3)
H11A	0.687378	0.151262	0.811331	0.092*
H11B	0.629550	0.133942	0.794676	0.092*
C12	0.6584 (3)	0.2279 (8)	0.7386 (3)	0.067 (3)
H12A	0.686011	0.277739	0.740485	0.081*
H12B	0.664743	0.169677	0.712995	0.081*
C13	0.4079 (2)	0.5520 (5)	0.5947 (2)	0.0328 (13)
C14	0.3261 (3)	0.5981 (10)	0.5464 (3)	0.075 (3)
H14A	0.320029	0.521746	0.544434	0.090*
H14B	0.314493	0.627415	0.507916	0.090*
C15	0.2963 (4)	0.6448 (12)	0.5884 (4)	0.097 (4)
H15A	0.307854	0.716925	0.597701	0.117*
H15B	0.261675	0.648773	0.570312	0.117*
C16	0.2630 (3)	0.6182 (12)	0.6801 (4)	0.099 (5)
H16A	0.268456	0.693070	0.689746	0.119*
H16B	0.229508	0.611075	0.658635	0.119*
C17	0.2666 (3)	0.5558 (11)	0.7348 (4)	0.080 (3)
H17A	0.236467	0.567967	0.751964	0.096*
H17B	0.267314	0.480646	0.724771	0.096*
C18	0.3529 (2)	0.5349 (6)	0.7757 (3)	0.0423 (15)
C21	0.7293 (7)	0.8810 (16)	0.5851 (8)	0.140 (13)*	0.5
C21A	0.7342 (8)	0.8063 (15)	0.6127 (10)	0.081 (6)*	0.5
C22	0.7005 (7)	0.7815 (15)	0.5679 (8)	0.183 (11)*	0.5
C22A	0.6945 (8)	0.8266 (16)	0.5614 (10)	0.183 (11)*	0.5
F1	0.6543 (6)	0.8407 (12)	0.6793 (6)	0.125 (6)	0.5
F1A	0.6342 (6)	0.9158 (14)	0.7007 (6)	0.115 (5)	0.5
F1S	0.5176 (3)	1.0828 (6)	0.5656 (5)	0.160 (5)
F2	0.6290 (6)	0.9494 (10)	0.7346 (9)	0.126 (6)	0.5
F2A	0.6528 (5)	0.9279 (8)	0.7899 (5)	0.082 (4)	0.5
F2S	0.5871 (4)	1.0670 (6)	0.6140 (3)	0.181 (5)
F3	0.6903 (9)	0.855 (2)	0.7641 (9)	0.124 (6)	0.5
F3A	0.6936 (9)	0.829 (2)	0.7435 (9)	0.124 (6)	0.5
F3S	0.5783 (3)	1.0620 (6)	0.5257 (3)	0.134 (3)
F4	0.5182 (11)	0.0110 (12)	0.7024 (8)	0.131 (7)	0.5
F5	0.4623 (8)	−0.0002 (15)	0.7574 (16)	0.152 (8)	0.5
F6	0.5360 (6)	0.0008 (8)	0.7921 (7)	0.085 (4)	0.5
F10	0.6535 (6)	0.813 (2)	0.5514 (11)	0.196 (10)*	0.5
F10A	0.6554 (9)	0.883 (3)	0.5717 (16)	0.32 (2)*	0.5
F11	0.7203 (9)	0.7380 (16)	0.5242 (9)	0.190 (9)*	0.5
F11A	0.6730 (10)	0.740 (2)	0.5364 (11)	0.221 (12)*	0.5
F12	0.7050 (10)	0.7197 (18)	0.6152 (11)	0.253 (18)*	0.5
F12A	0.7083 (12)	0.878 (2)	0.5165 (10)	0.258 (16)*	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pr1	0.03414 (18)	0.01746 (15)	0.01712 (15)	−0.00544 (10)	0.00929 (11)	−0.00077 (10)
Pr2	0.02908 (17)	0.02668 (17)	0.02091 (16)	0.00771 (11)	0.00859 (12)	0.00098 (11)
N1	0.053 (3)	0.029 (3)	0.032 (3)	−0.003 (2)	0.018 (2)	−0.004 (2)
N2	0.099 (5)	0.028 (3)	0.029 (3)	−0.019 (3)	0.030 (3)	0.000 (2)
N3	0.074 (4)	0.023 (2)	0.038 (3)	0.001 (3)	0.010 (3)	0.002 (2)
N4	0.060 (4)	0.035 (3)	0.027 (3)	0.017 (3)	0.014 (2)	0.006 (2)
N5	0.052 (4)	0.075 (5)	0.035 (3)	0.037 (3)	0.008 (3)	0.006 (3)
N6	0.048 (3)	0.059 (4)	0.032 (3)	0.024 (3)	0.015 (2)	0.001 (3)
N7	0.046 (3)	0.060 (4)	0.031 (3)	0.015 (3)	0.006 (2)	0.009 (3)
N8	0.047 (4)	0.163 (9)	0.043 (4)	0.042 (5)	0.009 (3)	0.005 (5)
N9	0.041 (3)	0.100 (6)	0.044 (3)	0.021 (4)	0.010 (3)	−0.006 (4)
O1	0.0306 (19)	0.0197 (17)	0.0198 (17)	0.0008 (14)	0.0090 (15)	−0.0030 (14)
O2	0.0302 (19)	0.0208 (17)	0.0177 (16)	0.0035 (15)	0.0065 (14)	0.0015 (14)
O3	0.071 (3)	0.036 (2)	0.030 (2)	−0.027 (2)	0.006 (2)	−0.0022 (19)
O4	0.071 (4)	0.073 (4)	0.029 (2)	−0.037 (3)	0.008 (2)	−0.003 (2)
O5	0.071 (3)	0.026 (2)	0.038 (2)	0.008 (2)	0.014 (2)	0.0012 (19)
O6	0.034 (2)	0.048 (3)	0.029 (2)	−0.0038 (19)	0.0038 (17)	0.0022 (19)
O7	0.037 (2)	0.031 (2)	0.0215 (18)	−0.0005 (17)	0.0052 (16)	−0.0011 (16)
O8	0.033 (2)	0.064 (3)	0.038 (2)	0.000 (2)	0.0124 (19)	−0.005 (2)
O9	0.035 (2)	0.067 (3)	0.031 (2)	0.004 (2)	0.0125 (19)	0.000 (2)
C1	0.070 (5)	0.043 (4)	0.038 (4)	−0.029 (4)	0.019 (3)	−0.012 (3)
C2	0.087 (8)	0.071 (7)	0.065 (9)	−0.056 (6)	−0.014 (8)	0.014 (7)
C2A	0.087 (8)	0.071 (7)	0.065 (9)	−0.056 (6)	−0.014 (8)	0.014 (7)
C3	0.082 (8)	0.026 (4)	0.035 (5)	0.000	0.028 (5)	0.000
C4	0.109 (14)	0.031 (6)	0.143 (17)	0.000	0.029 (12)	0.000
C5	0.066 (5)	0.049 (4)	0.035 (3)	−0.013 (4)	0.029 (3)	−0.013 (3)
C6	0.108 (7)	0.042 (4)	0.027 (3)	−0.025 (4)	0.028 (4)	−0.002 (3)
C7	0.145 (10)	0.029 (4)	0.042 (4)	−0.012 (5)	0.032 (5)	0.008 (3)
C8	0.107 (7)	0.035 (4)	0.046 (4)	0.001 (4)	0.007 (4)	0.015 (3)
C9	0.099 (7)	0.053 (5)	0.032 (3)	0.039 (5)	0.019 (4)	0.012 (3)
C10	0.064 (5)	0.080 (6)	0.040 (4)	0.043 (5)	0.008 (3)	0.013 (4)
C11	0.094 (7)	0.098 (7)	0.041 (4)	0.074 (6)	0.021 (4)	0.012 (4)
C12	0.069 (5)	0.092 (7)	0.045 (4)	0.052 (5)	0.020 (4)	−0.002 (4)
C13	0.043 (3)	0.037 (3)	0.019 (2)	0.000 (3)	0.006 (2)	−0.002 (2)
C14	0.048 (5)	0.142 (10)	0.035 (4)	0.035 (5)	0.005 (3)	0.017 (5)
C15	0.059 (6)	0.180 (13)	0.055 (5)	0.058 (7)	0.015 (4)	0.022 (7)
C16	0.045 (5)	0.201 (15)	0.052 (5)	0.048 (7)	0.013 (4)	−0.001 (7)
C17	0.027 (4)	0.159 (11)	0.055 (5)	0.025 (5)	0.009 (3)	−0.010 (6)
C18	0.031 (3)	0.060 (4)	0.039 (3)	0.008 (3)	0.014 (3)	0.005 (3)
F1	0.146 (12)	0.129 (11)	0.121 (10)	−0.069 (9)	0.088 (9)	0.004 (9)
F1A	0.127 (9)	0.112 (9)	0.103 (8)	−0.051 (7)	0.010 (7)	0.054 (7)
F1S	0.157 (9)	0.054 (4)	0.269 (14)	−0.018 (5)	0.027 (9)	0.003 (6)
F2	0.182 (14)	0.054 (7)	0.166 (14)	−0.061 (8)	0.108 (12)	−0.028 (8)
F2A	0.115 (10)	0.039 (5)	0.086 (8)	−0.042 (6)	−0.005 (7)	−0.018 (5)
F2S	0.352 (15)	0.055 (4)	0.103 (6)	0.017 (6)	−0.069 (8)	0.033 (4)
F3	0.093 (6)	0.101 (13)	0.185 (14)	−0.054 (6)	0.045 (9)	0.006 (11)
F3A	0.093 (6)	0.101 (13)	0.185 (14)	−0.054 (6)	0.045 (9)	0.006 (11)
F3S	0.220 (10)	0.071 (4)	0.113 (6)	0.035 (5)	0.032 (6)	−0.037 (4)
F4	0.230 (17)	0.058 (8)	0.103 (10)	0.048 (10)	0.013 (11)	−0.047 (8)
F5	0.160 (14)	0.072 (10)	0.212 (17)	−0.038 (10)	−0.011 (14)	0.032 (13)
F6	0.122 (8)	0.032 (4)	0.097 (7)	0.012 (5)	0.004 (6)	0.026 (5)

Geometric parameters (Å, º) top

Pr1—O2ⁱ	2.447 (3)	O9—C18	1.275 (8)
Pr1—O2	2.462 (4)	O12—C21	1.261 (9)
Pr1—O1	2.470 (4)	O12A—C21A	1.278 (10)
Pr1—O9ⁱ	2.477 (5)	O13—C21	1.255 (9)
Pr1—O7	2.493 (4)	O13A—C21A	1.306 (10)
Pr1—O3	2.622 (4)	C1—C2A	1.539 (19)
Pr1—N3	2.658 (6)	C1—C2	1.549 (19)
Pr1—N2	2.683 (5)	C1S—C2S	1.539 (13)
Pr1—N1	2.683 (5)	C2—F1A	1.10 (2)
Pr1—Pr2	3.9340 (4)	C2—F2	1.310 (9)
Pr1—Pr2ⁱ	3.9379 (4)	C2—F3A	1.32 (4)
Pr1—Pr1ⁱ	4.0626 (5)	C2—F1	1.316 (9)
Pr2—O2ⁱ	2.456 (4)	C2—F3	1.319 (9)
Pr2—O8ⁱ	2.476 (5)	C2—F2A	1.631 (16)
Pr2—O1ⁱ	2.491 (4)	C2A—F1A	1.312 (9)
Pr2—O1	2.502 (4)	C2A—F2A	1.314 (9)
Pr2—O6ⁱ	2.515 (4)	C2A—F3A	1.321 (9)
Pr2—O5	2.539 (5)	C2S—F3S	1.276 (12)
Pr2—N4	2.682 (5)	C2S—F1S	1.296 (13)
Pr2—N6	2.682 (5)	C2S—F2S	1.303 (13)
Pr2—N5	2.684 (6)	C3—C4	1.529 (16)
Pr2—Pr2ⁱ	4.0277 (6)	C4—F5ⁱ	1.20 (2)
N1—C5	1.462 (8)	C4—F5	1.20 (2)
N2—C7	1.456 (10)	C4—F4	1.352 (17)
N2—C6	1.469 (8)	C4—F4ⁱ	1.352 (17)
N3—C8	1.469 (9)	C4—F6ⁱ	1.396 (13)
N4—C9	1.463 (9)	C4—F6	1.396 (13)
N5—C10	1.455 (9)	C5—C6	1.483 (11)
N5—C11	1.488 (10)	C7—C8	1.502 (14)
N6—C12	1.473 (9)	C9—C10	1.487 (13)
N7—C13	1.342 (8)	C11—C12	1.475 (11)
N7—C14	1.450 (11)	C14—C15	1.501 (13)
N8—C15	1.485 (13)	C16—C17	1.507 (15)
N8—C16	1.506 (11)	C21—C22	1.524 (10)
N9—C18	1.357 (9)	C21A—C22A	1.530 (10)
N9—C17	1.446 (11)	C22—F11	1.354 (10)
O1S—C1S	1.203 (9)	C22—F12	1.356 (10)
O2S—C1S	1.218 (10)	C22—F10	1.363 (10)
O3—C1	1.239 (9)	C22A—F12A	1.348 (10)
O4—C1	1.229 (9)	C22A—F10A	1.350 (10)
O5—C3	1.230 (6)	C22A—F11A	1.354 (10)
O6—C13	1.270 (7)	F4—F5ⁱ	1.03 (3)
O7—C13	1.267 (7)	F4—F6ⁱ	1.53 (3)
O8—C18	1.255 (8)	F5—F6ⁱ	1.17 (3)

O2ⁱ—Pr1—O2	65.86 (15)	Pr1ⁱ—Pr2—Pr2ⁱ	59.177 (7)
O2ⁱ—Pr1—O1	70.66 (12)	C5—N1—Pr1	114.8 (4)
O2—Pr1—O1	70.42 (12)	C7—N2—C6	113.8 (6)
O2ⁱ—Pr1—O9ⁱ	78.15 (13)	C7—N2—Pr1	114.3 (4)
O2—Pr1—O9ⁱ	140.32 (14)	C6—N2—Pr1	114.1 (4)
O1—Pr1—O9ⁱ	82.70 (15)	C8—N3—Pr1	113.5 (5)
O2ⁱ—Pr1—O7	136.89 (12)	C9—N4—Pr2	113.5 (4)
O2—Pr1—O7	73.20 (12)	C10—N5—C11	112.2 (7)
O1—Pr1—O7	83.72 (13)	C10—N5—Pr2	113.4 (4)
O9ⁱ—Pr1—O7	133.35 (14)	C11—N5—Pr2	110.8 (5)
O2ⁱ—Pr1—O3	71.75 (13)	C12—N6—Pr2	114.1 (4)
O2—Pr1—O3	109.86 (14)	C13—N7—C14	122.3 (7)
O1—Pr1—O3	137.92 (14)	C15—N8—C16	112.9 (8)
O9ⁱ—Pr1—O3	71.68 (18)	C18—N9—C17	121.9 (7)
O7—Pr1—O3	137.90 (15)	Pr1—O1—Pr2ⁱ	105.09 (13)
O2ⁱ—Pr1—N3	108.54 (15)	Pr1—O1—Pr2	104.61 (13)
O2—Pr1—N3	75.81 (16)	Pr2ⁱ—O1—Pr2	107.57 (13)
O1—Pr1—N3	143.09 (17)	Pr1ⁱ—O2—Pr2ⁱ	106.72 (13)
O9ⁱ—Pr1—N3	134.06 (19)	Pr1ⁱ—O2—Pr1	111.70 (14)
O7—Pr1—N3	72.48 (16)	Pr2ⁱ—O2—Pr1	106.40 (13)
O3—Pr1—N3	68.12 (19)	C1—O3—Pr1	134.7 (5)
O2ⁱ—Pr1—N2	136.49 (17)	C3—O5—Pr2	135.7 (5)
O2—Pr1—N2	139.12 (18)	C13—O6—Pr2ⁱ	125.0 (4)
O1—Pr1—N2	141.39 (15)	C13—O7—Pr1	137.8 (3)
O9ⁱ—Pr1—N2	79.2 (2)	C18—O8—Pr2ⁱ	129.0 (4)
O7—Pr1—N2	84.39 (18)	C18—O9—Pr1ⁱ	135.4 (4)
O3—Pr1—N2	66.02 (16)	O4—C1—O3	130.5 (6)
N3—Pr1—N2	64.9 (2)	O4—C1—C2A	109.7 (8)
O2ⁱ—Pr1—N1	136.80 (15)	O3—C1—C2A	119.7 (8)
O2—Pr1—N1	128.95 (15)	O4—C1—C2	120.0 (9)
O1—Pr1—N1	77.73 (14)	O3—C1—C2	109.3 (8)
O9ⁱ—Pr1—N1	69.14 (17)	C2A—C1—C2	12.9 (7)
O7—Pr1—N1	64.40 (16)	O1S—C1S—O2S	131.0 (8)
O3—Pr1—N1	120.46 (16)	O1S—C1S—C2S	113.4 (8)
N3—Pr1—N1	114.42 (17)	O2S—C1S—C2S	115.6 (8)
N2—Pr1—N1	64.01 (16)	F1A—C2—F3A	120 (3)
O2ⁱ—Pr1—Pr2	36.72 (8)	F2—C2—F1	105.8 (8)
O2—Pr1—Pr2	75.78 (8)	F2—C2—F3	107.3 (8)
O1—Pr1—Pr2	37.98 (9)	F1—C2—F3	105.8 (8)
O9ⁱ—Pr1—Pr2	65.24 (11)	F1A—C2—C1	123.6 (19)
O7—Pr1—Pr2	120.52 (9)	F2—C2—C1	111.2 (13)
O3—Pr1—Pr2	100.09 (11)	F3A—C2—C1	114 (2)
N3—Pr1—Pr2	142.83 (12)	F1—C2—C1	114.2 (12)
N2—Pr1—Pr2	144.45 (17)	F3—C2—C1	112.0 (18)
N1—Pr1—Pr2	102.02 (12)	F1A—C2—F2A	98.1 (14)
O2ⁱ—Pr1—Pr2ⁱ	75.84 (8)	F3A—C2—F2A	90.3 (16)
O2—Pr1—Pr2ⁱ	36.75 (8)	C1—C2—F2A	96.6 (9)
O1—Pr1—Pr2ⁱ	37.64 (9)	F1A—C2A—F2A	105.8 (8)
O9ⁱ—Pr1—Pr2ⁱ	119.91 (12)	F1A—C2A—F3A	106.5 (8)
O7—Pr1—Pr2ⁱ	63.15 (9)	F2A—C2A—F3A	106.2 (8)
O3—Pr1—Pr2ⁱ	142.19 (10)	F1A—C2A—C1	110.7 (13)
N3—Pr1—Pr2ⁱ	105.49 (14)	F2A—C2A—C1	112.5 (12)
N2—Pr1—Pr2ⁱ	147.35 (15)	F3A—C2A—C1	114.6 (18)
N1—Pr1—Pr2ⁱ	96.50 (11)	F3S—C2S—F1S	106.1 (9)
Pr2—Pr1—Pr2ⁱ	61.548 (10)	F3S—C2S—F2S	106.0 (9)
O2ⁱ—Pr1—Pr1ⁱ	34.27 (9)	F1S—C2S—F2S	107.2 (10)
O2—Pr1—Pr1ⁱ	34.03 (8)	F3S—C2S—C1S	115.4 (9)
O1—Pr1—Pr1ⁱ	76.22 (8)	F1S—C2S—C1S	112.3 (9)
O9ⁱ—Pr1—Pr1ⁱ	112.41 (10)	F2S—C2S—C1S	109.3 (9)
O7—Pr1—Pr1ⁱ	107.17 (9)	O5ⁱ—C3—O5	130.0 (9)
O3—Pr1—Pr1ⁱ	83.31 (10)	O5ⁱ—C3—C4	115.0 (4)
N3—Pr1—Pr1ⁱ	84.21 (12)	O5—C3—C4	115.0 (4)
N2—Pr1—Pr1ⁱ	142.35 (12)	F5ⁱ—C4—F5	128 (3)
N1—Pr1—Pr1ⁱ	153.39 (11)	F5ⁱ—C4—F4	47.0 (13)
Pr2—Pr1—Pr1ⁱ	58.977 (7)	F5—C4—F4	115.5 (16)
Pr2ⁱ—Pr1—Pr1ⁱ	58.882 (7)	F5ⁱ—C4—F4ⁱ	115.5 (16)
O2ⁱ—Pr2—O8ⁱ	74.00 (15)	F5—C4—F4ⁱ	47.0 (13)
O2ⁱ—Pr2—O1ⁱ	70.18 (12)	F4—C4—F4ⁱ	146.7 (19)
O8ⁱ—Pr2—O1ⁱ	144.18 (14)	F5ⁱ—C4—F6ⁱ	105.9 (14)
O2ⁱ—Pr2—O1	69.99 (11)	F5—C4—F6ⁱ	53.1 (15)
O8ⁱ—Pr2—O1	96.74 (14)	F4—C4—F6ⁱ	67.5 (11)
O1ⁱ—Pr2—O1	70.63 (13)	F4ⁱ—C4—F6ⁱ	99.8 (11)
O2ⁱ—Pr2—O6ⁱ	73.44 (13)	F5ⁱ—C4—F6	53.1 (15)
O8ⁱ—Pr2—O6ⁱ	69.29 (15)	F5—C4—F6	105.9 (14)
O1ⁱ—Pr2—O6ⁱ	100.43 (13)	F4—C4—F6	99.8 (11)
O1—Pr2—O6ⁱ	143.24 (13)	F4ⁱ—C4—F6	67.5 (11)
O2ⁱ—Pr2—O5	143.20 (15)	F6ⁱ—C4—F6	136.5 (15)
O8ⁱ—Pr2—O5	132.23 (16)	F5ⁱ—C4—C3	116.1 (13)
O1ⁱ—Pr2—O5	80.00 (14)	F5—C4—C3	116.1 (13)
O1—Pr2—O5	80.26 (14)	F4—C4—C3	106.6 (9)
O6ⁱ—Pr2—O5	134.65 (15)	F4ⁱ—C4—C3	106.6 (9)
O2ⁱ—Pr2—N4	121.74 (14)	F6ⁱ—C4—C3	111.8 (7)
O8ⁱ—Pr2—N4	127.64 (18)	F6—C4—C3	111.8 (7)
O1ⁱ—Pr2—N4	74.28 (15)	N1—C5—C6	110.1 (6)
O1—Pr2—N4	135.38 (16)	N2—C6—C5	110.6 (6)
O6ⁱ—Pr2—N4	69.46 (17)	N2—C7—C8	111.1 (7)
O5—Pr2—N4	67.12 (16)	N3—C8—C7	110.0 (7)
O2ⁱ—Pr2—N6	121.92 (16)	N4—C9—C10	108.3 (7)
O8ⁱ—Pr2—N6	67.71 (19)	N5—C10—C9	112.7 (7)
O1ⁱ—Pr2—N6	133.40 (17)	C12—C11—N5	110.3 (8)
O1—Pr2—N6	73.01 (15)	N6—C12—C11	112.5 (6)
O6ⁱ—Pr2—N6	126.06 (17)	O7—C13—O6	123.9 (6)
O5—Pr2—N6	65.89 (18)	O7—C13—N7	118.4 (6)
N4—Pr2—N6	116.14 (17)	O6—C13—N7	117.7 (6)
O2ⁱ—Pr2—N5	139.2 (2)	N7—C14—C15	115.2 (9)
O8ⁱ—Pr2—N5	73.4 (2)	N8—C15—C14	112.7 (9)
O1ⁱ—Pr2—N5	138.04 (17)	C17—C16—N8	112.4 (9)
O1—Pr2—N5	137.84 (15)	N9—C17—C16	116.6 (10)
O6ⁱ—Pr2—N5	72.48 (18)	O8—C18—O9	125.7 (6)
O5—Pr2—N5	77.6 (2)	O8—C18—N9	117.1 (7)
N4—Pr2—N5	64.42 (18)	O9—C18—N9	117.2 (6)
N6—Pr2—N5	65.28 (17)	O13—C21—O12	132.6 (16)
O2ⁱ—Pr2—Pr1	36.56 (8)	O13—C21—C22	111.9 (12)
O8ⁱ—Pr2—Pr1	72.29 (11)	O12—C21—C22	115.4 (13)
O1ⁱ—Pr2—Pr1	78.66 (8)	O12A—C21A—O13A	155 (3)
O1—Pr2—Pr1	37.42 (8)	O12A—C21A—C22A	108 (2)
O6ⁱ—Pr2—Pr1	106.60 (11)	O13A—C21A—C22A	96.3 (18)
O5—Pr2—Pr1	117.67 (11)	F11—C22—F12	112.8 (12)
N4—Pr2—Pr1	151.20 (11)	F11—C22—F10	112.4 (12)
N6—Pr2—Pr1	89.69 (12)	F12—C22—F10	112.1 (12)
N5—Pr2—Pr1	143.30 (15)	F11—C22—C21	107.0 (13)
O2ⁱ—Pr2—Pr1ⁱ	36.85 (8)	F12—C22—C21	106.6 (13)
O8ⁱ—Pr2—Pr1ⁱ	108.50 (12)	F10—C22—C21	105.4 (13)
O1ⁱ—Pr2—Pr1ⁱ	37.28 (8)	F12A—C22A—F10A	101.9 (19)
O1—Pr2—Pr1ⁱ	78.47 (8)	F12A—C22A—F11A	102.7 (18)
O6ⁱ—Pr2—Pr1ⁱ	74.62 (10)	F10A—C22A—F11A	101.7 (19)
O5—Pr2—Pr1ⁱ	117.27 (12)	F12A—C22A—C21A	116.7 (17)
N4—Pr2—Pr1ⁱ	89.95 (11)	F10A—C22A—C21A	116.6 (17)
N6—Pr2—Pr1ⁱ	150.33 (12)	F11A—C22A—C21A	115.0 (16)
N5—Pr2—Pr1ⁱ	143.69 (13)	C2—F1A—C2A	13.3 (10)
Pr1—Pr2—Pr1ⁱ	62.140 (9)	C2A—F2A—C2	5.6 (9)
O2ⁱ—Pr2—Pr2ⁱ	73.93 (9)	C2—F3A—C2A	15.1 (8)
O8ⁱ—Pr2—Pr2ⁱ	130.21 (11)	F5ⁱ—F4—C4	58.9 (17)
O1ⁱ—Pr2—Pr2ⁱ	36.31 (8)	F5ⁱ—F4—F6ⁱ	107 (3)
O1—Pr2—Pr2ⁱ	36.12 (8)	C4—F4—F6ⁱ	57.6 (10)
O6ⁱ—Pr2—Pr2ⁱ	133.20 (10)	F4ⁱ—F5—F6ⁱ	145 (3)
O5—Pr2—Pr2ⁱ	69.27 (12)	F4ⁱ—F5—C4	74.1 (17)
N4—Pr2—Pr2ⁱ	101.59 (14)	F6ⁱ—F5—C4	71.9 (19)
N6—Pr2—Pr2ⁱ	99.62 (13)	F5ⁱ—F6—C4	55.0 (11)
N5—Pr2—Pr2ⁱ	146.88 (18)	F5ⁱ—F6—F4ⁱ	105.6 (16)
Pr1—Pr2—Pr2ⁱ	59.273 (7)	C4—F6—F4ⁱ	54.9 (7)

Symmetry code: (i) −x+1, y, −z+3/2.

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