#------------------------------------------------------------------------------ #$Date: 2021-11-17 02:17:27 +0200 (Wed, 17 Nov 2021) $ #$Revision: 270708 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/88/7708869.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7708869 loop_ _publ_author_name 'Yao, Qing-Xia' 'Tian, Miaomiao' 'Zheng, Jun' 'Xue, Jintang' 'Pan, Xuze' 'Zhou, Dandan' 'Li, Yun-Wu' 'Duan, Wen-zeng' 'Su, Jie' 'Huang, Xianqiang' _publ_section_title ; A series of microporous and robust Ln-MOFs showing luminescent properties and catalytic performances towards Knoevenagel reactions ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03188K _journal_year 2021 _chemical_formula_moiety 'C25 H21 N2 O7 Pr, C4 H9 N O' _chemical_formula_sum 'C29 H30 N3 O8 Pr' _chemical_formula_weight 689.47 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2021-11-15 _audit_creation_method ; Olex2 1.5 (compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396) ; _audit_update_record ; 2021-11-15 deposited with the CCDC. 2021-11-16 downloaded from the CCDC. ; _cell_angle_alpha 112.080(3) _cell_angle_beta 92.371(3) _cell_angle_gamma 107.734(3) _cell_formula_units_Z 2 _cell_length_a 8.9119(3) _cell_length_b 13.3816(5) _cell_length_c 13.7490(5) _cell_measurement_reflns_used 9634 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.0130 _cell_measurement_theta_min 2.4150 _cell_volume 1424.45(10) _computing_cell_refinement 'CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.850 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0587 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.850 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 7574 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.850 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.782 _diffrn_reflns_theta_min 2.438 _exptl_absorpt_coefficient_mu 1.765 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.607 _exptl_crystal_description rod-like _exptl_crystal_F_000 696 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 2.501 _refine_diff_density_min -1.423 _refine_diff_density_rms 0.168 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 7574 _refine_ls_number_restraints 105 _refine_ls_restrained_S_all 1.150 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0550 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+6.9991P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1336 _refine_ls_wR_factor_ref 0.1363 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6889 _reflns_number_total 7574 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03188k2.cif _cod_data_source_block 1-Pr_tw _cod_database_code 7708869 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.789(2) 0.211(2) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances O7A-C22A = O7B-C22B 1.2 with sigma of 0.02 N1B-C1A = N1A-C1B = N1B-C8A = N1A-C8B = N1B-C15A = N1A-C15B 1.49 with sigma of 0.02 C22A-N2A = C22B-N2B 1.27 with sigma of 0.02 N2A-C24A = N2A-C25A = N2B-C24B = N2B-C25B 1.5 with sigma of 0.02 C22A-C23A = C22B-C23B 1.54 with sigma of 0.02 C4A-C7 = C4B-C7 = C18A-C21 = C18B-C21 1.52 with sigma of 0.02 Pr1-O7A \\sim Pr1-O7B with sigma of 0.02 4. Restrained planarity O7A, N2A, C22A, C23A, C24A, C25A with sigma of 0.1 O7B, N2B, C22B, C23B, C24B, C25B with sigma of 0.1 5. Uiso/Uaniso restraints and constraints Uanis(C24A) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C6B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(N1B) = Uanis(N1A) Uanis(O7A) = Uanis(O7B) Uanis(N2A) = Uanis(N2B) Uanis(C22A) = Uanis(C22B) Uanis(C23A) = Uanis(C23B) Uanis(C24A) = Uanis(C24B) Uanis(C25A) = Uanis(C25B) = Uanis(C28) Uanis(C8A) = Uanis(C8B) Uanis(C9A) = Uanis(C9B) Uanis(C10A) = Uanis(C10B) Uanis(C11A) = Uanis(C11B) Uanis(C12A) = Uanis(C12B) Uanis(C13A) = Uanis(C13B) Uanis(C1A) = Uanis(C1B) Uanis(C2A) = Uanis(C2B) Uanis(C3A) = Uanis(C3B) Uanis(C4A) = Uanis(C4B) Uanis(C5A) = Uanis(C5B) Uanis(C6A) = Uanis(C6B) Uanis(C15A) = Uanis(C15B) Uanis(C16A) = Uanis(C16B) Uanis(C17A) = Uanis(C17B) Uanis(C18A) = Uanis(C18B) = Uanis(C4A) Uanis(C19A) = Uanis(C19B) Uanis(C20A) = Uanis(C20B) 6. Others Sof(O7B)=Sof(N2B)=Sof(C22B)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24B)= Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1) Sof(O7A)=Sof(N2A)=Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24A)= Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1) Fixed Sof: N1B(0.5) N1A(0.5) C1A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5) C1B(0.5) C2B(0.5) H2B(0.5) C3B(0.5) H3B(0.5) C4B(0.5) C5B(0.5) H5B(0.5) C6B(0.5) H6B(0.5) C8A(0.5) C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5) H13A(0.5) C8B(0.5) C9B(0.5) H9B(0.5) C10B(0.5) H10B(0.5) C11B(0.5) C12B(0.5) H12B(0.5) C13B(0.5) H13B(0.5) C15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5) C18A(0.5) C19A(0.5) H19A(0.5) C20A(0.5) H20A(0.5) C15B(0.5) C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) C18B(0.5) C19B(0.5) H19B(0.5) C20B(0.5) H20B(0.5) 7.a Aromatic/amide H refined with riding coordinates: C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B), C9A(H9A), C10A(H10A), C12A(H12A), C13A(H13A), C9B(H9B), C10B(H10B), C12B(H12B), C13B(H13B), C16A(H16A), C17A(H17A), C19A(H19A), C20A(H20A), C16B(H16B), C17B(H17B), C19B(H19B), C20B(H20B) 7.b Fitted hexagon refined as free rotating group: C1A(C2A,C3A,C4A,C5A,C6A), C1B(C2B,C3B,C4B,C5B,C6B), C8A(C9A,C10A,C11A,C12A, C13A), C8B(C9B,C10B,C11B,C12B,C13B), C15A(C16A,C17A,C18A,C19A,C20A), C15B(C16B, C17B,C18B,C19B,C20B) 7.c Idealised Me refined with riding coordinates: C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F) 7.d Idealised Me refined as rotating group: C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F), C25A(H25A,H25B,H25C), C25B(H25D, H25E,H25F), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C) ; _shelx_res_file ; TITL 3_a.res in P-1 2_tw.res created by SHELXL-2018/3 at 20:28:42 on 15-Nov-2021 REM Old TITL 3 in P1 REM SHELXT solution in P-1 REM R1 0.116, Rweak 0.035, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C28 N4 O9 Pr REM 3_a.res in P-1 REM 370 parameters refined using 111 restraints REM Highest difference peak 2.482, deepest hole -1.438, 1-sigma level 0.169 REM wR2 = 0.1365, GooF = S = 1.155, Restrained GooF = 1.149 for all data REM Highest difference peak 2.498, deepest hole -1.422, 1-sigma level 0.168 REM wR2 = 0.1363, GooF = S = 1.155, Restrained GooF = 1.149 for all data REM Highest difference peak 2.499, deepest hole -1.422, 1-sigma level 0.168 CELL 0.71073 8.9119 13.3816 13.749 112.08 92.371 107.734 ZERR 2 0.0003 0.0005 0.0005 0.003 0.003 0.003 LATT 1 SFAC C H N O Pr UNIT 58 60 6 16 2 DFIX 1.2 O7A C22A O7B C22B EADP N1B N1A DFIX 1.49 N1B C1A N1A C1B N1B C8A N1A C8B N1B C15A N1A C15B DFIX 1.27 C22A N2A C22B N2B DFIX 1.5 N2A C24A N2A C25A N2B C24B N2B C25B DFIX 1.54 C22A C23A C22B C23B SADI Pr1 O7A Pr1 O7B FLAT O7A N2A C22A C23A C24A C25A FLAT O7B N2B C22B C23B C24B C25B ISOR 0.02 0.04 C24A C25A EADP O7A O7B EADP N2A N2B EADP C22A C22B EADP C23A C23B EADP C24A C24B EADP C25A C25B C28 EADP C8A C8B EADP C9A C9B EADP C10A C10B EADP C11A C11B EADP C12A C12B EADP C13A C13B EADP C1A C1B EADP C2A C2B EADP C3A C3B EADP C4A C4B EADP C5A C5B EADP C6A C6B EADP C15A C15B EADP C16A C16B EADP C17A C17B EADP C18A C18B C4A EADP C19A C19B EADP C20A C20B ISOR 0.02 0.04 C1A > C6B DFIX 1.52 C4A C7 C4B C7 C18A C21 C18B C21 L.S. 30 PLAN 1 TEMP -100 CONF GRID BOND $H MORE -1 fmap 2 ACTA MERG 0 OMIT -1 -5 12 OMIT -2 0 1 OMIT -1 0 1 OMIT 1 0 1 REM REM REM WGHT 0.038500 6.999100 BASF 0.21059 FVAR 11.06512 0.54669 PR1 5 0.250586 0.052374 -0.010948 11.00000 0.01913 0.01484 = 0.02151 0.00555 -0.00189 0.00679 O1 4 0.120707 0.164859 0.094334 11.00000 0.06135 0.05862 = 0.04042 0.00951 0.00710 0.04509 O2 4 -0.120367 0.141377 0.135184 11.00000 0.05654 0.02530 = 0.04189 0.00616 0.00563 -0.00355 O3 4 0.154895 0.953154 0.095171 11.00000 0.04070 0.04202 = 0.04851 0.02650 0.00529 0.01046 O4 4 -0.089923 0.924549 0.136619 11.00000 0.03895 0.04211 = 0.03838 0.01622 -0.00520 0.01896 O5 4 0.435128 1.004336 0.883371 11.00000 0.02703 0.04399 = 0.02964 0.00063 0.00352 0.00736 O6 4 0.545915 0.870297 0.862464 11.00000 0.03407 0.04609 = 0.02797 0.01247 -0.00769 0.00570 PART 1 O7A 4 0.401198 0.243666 0.008204 21.00000 0.03694 0.02763 = 0.04989 0.01741 0.00086 0.00440 PART 2 O7B 4 0.419380 0.222483 -0.026748 -21.00000 0.03694 0.02763 = 0.04989 0.01741 0.00086 0.00440 N1B 3 0.218158 0.684756 0.378150 10.50000 0.06167 0.02087 = 0.02025 0.00654 -0.00754 0.01444 PART 1 N1A 3 0.155536 0.681745 0.396101 10.50000 0.06167 0.02087 = 0.02025 0.00654 -0.00754 0.01444 N2A 3 0.653011 0.353737 0.034244 21.00000 0.03966 0.05094 = 0.12472 0.05567 0.00478 -0.00597 PART 2 N2B 3 0.581314 0.388970 -0.006632 -21.00000 0.03966 0.05094 = 0.12472 0.05567 0.00478 -0.00597 PART 1 AFIX 66 C1A 1 0.129126 0.560203 0.335309 10.50000 0.03235 0.02321 = 0.02339 0.01040 -0.00382 0.00354 C2A 1 0.002634 0.476799 0.347372 10.50000 0.03523 0.02048 = 0.03209 0.00260 0.00684 0.00731 AFIX 43 H2A 2 -0.062363 0.498825 0.398736 10.50000 -1.20000 AFIX 65 C3A 1 -0.028757 0.361168 0.284282 10.50000 0.02824 0.02226 = 0.03238 0.00518 0.00487 0.00547 AFIX 43 H3A 2 -0.115208 0.304165 0.292526 10.50000 -1.20000 AFIX 65 C4A 1 0.066344 0.328939 0.209128 10.50000 0.02706 0.02149 = 0.02621 0.00804 -0.00086 0.00873 C5A 1 0.192836 0.412343 0.197064 10.50000 0.04736 0.03035 = 0.04934 0.01546 0.02124 0.01291 AFIX 43 H5A 2 0.257832 0.390315 0.145699 10.50000 -1.20000 AFIX 65 C6A 1 0.224229 0.527974 0.260154 10.50000 0.05467 0.02945 = 0.04783 0.01578 0.01619 0.00352 AFIX 43 H6A 2 0.310680 0.584977 0.251909 10.50000 -1.20000 AFIX 66 PART 2 C1B 1 0.176566 0.563481 0.327303 10.50000 0.03235 0.02321 = 0.02339 0.01040 -0.00382 0.00354 C2B 1 0.047389 0.493031 0.351552 10.50000 0.03523 0.02048 = 0.03209 0.00260 0.00684 0.00731 AFIX 43 H2B 2 -0.006454 0.525941 0.406437 10.50000 -1.20000 AFIX 65 C3B 1 -0.003007 0.374429 0.295495 10.50000 0.02824 0.02226 = 0.03238 0.00518 0.00487 0.00547 AFIX 43 H3B 2 -0.091294 0.326280 0.312068 10.50000 -1.20000 AFIX 65 C4B 1 0.075774 0.326276 0.215189 10.50000 0.02706 0.02149 = 0.02621 0.00804 -0.00086 0.00873 C5B 1 0.204950 0.396725 0.190939 10.50000 0.04736 0.03035 = 0.04934 0.01546 0.02124 0.01291 AFIX 43 H5B 2 0.258793 0.363814 0.136053 10.50000 -1.20000 AFIX 65 C6B 1 0.255348 0.515327 0.246995 10.50000 0.05467 0.02945 = 0.04783 0.01578 0.01619 0.00352 AFIX 43 H6B 2 0.343635 0.563476 0.230422 10.50000 -1.20000 AFIX 0 PART 0 C7 1 0.019248 0.201232 0.141868 11.00000 0.04531 0.02364 = 0.02443 0.00677 0.00092 0.01769 PART 1 AFIX 66 C8A 1 0.126321 0.744850 0.337422 10.50000 0.04724 0.02227 = 0.02004 0.00715 -0.01130 0.00918 C9A 1 -0.025835 0.712092 0.280723 10.50000 0.03319 0.02767 = 0.03923 0.01872 -0.00404 -0.00694 AFIX 43 H9A 2 -0.111031 0.650640 0.283757 10.50000 -1.20000 AFIX 65 C10A 1 -0.053334 0.769248 0.219586 10.50000 0.02982 0.03532 = 0.04292 0.02012 -0.01233 0.00035 AFIX 43 H10A 2 -0.157326 0.746859 0.180836 10.50000 -1.20000 AFIX 65 C11A 1 0.071322 0.859162 0.215146 10.50000 0.03459 0.02736 = 0.02508 0.01378 -0.00276 0.00909 C12A 1 0.223477 0.891921 0.271844 10.50000 0.02826 0.03751 = 0.03880 0.02497 0.00393 0.01017 AFIX 43 H12A 2 0.308674 0.953373 0.268809 10.50000 -1.20000 AFIX 65 C13A 1 0.250979 0.834766 0.332982 10.50000 0.03687 0.03708 = 0.03200 0.01541 -0.00653 0.01219 AFIX 43 H13A 2 0.354971 0.857156 0.371733 10.50000 -1.20000 AFIX 66 PART 2 C8B 1 0.175049 0.741018 0.317886 10.50000 0.04724 0.02227 = 0.02004 0.00715 -0.01130 0.00918 C9B 1 0.016854 0.732738 0.296550 10.50000 0.03319 0.02767 = 0.03923 0.01872 -0.00404 -0.00694 AFIX 43 H9B 2 -0.063937 0.688175 0.321387 10.50000 -1.20000 AFIX 65 C10B 1 -0.023131 0.789659 0.238873 10.50000 0.02982 0.03532 = 0.04292 0.02012 -0.01233 0.00035 AFIX 43 H10B 2 -0.131250 0.783999 0.224291 10.50000 -1.20000 AFIX 65 C11B 1 0.095079 0.854861 0.202531 10.50000 0.03459 0.02736 = 0.02508 0.01378 -0.00276 0.00909 C12B 1 0.253274 0.863143 0.223867 10.50000 0.02826 0.03751 = 0.03880 0.02497 0.00393 0.01017 AFIX 43 H12B 2 0.334065 0.907706 0.199029 10.50000 -1.20000 AFIX 65 C13B 1 0.293261 0.806222 0.281544 10.50000 0.03687 0.03708 = 0.03200 0.01541 -0.00653 0.01219 AFIX 43 H13B 2 0.401380 0.811883 0.296126 10.50000 -1.20000 AFIX 0 PART 0 C14 1 0.046266 0.915810 0.141737 11.00000 0.03078 0.02429 = 0.02942 0.01246 -0.00298 0.00745 PART 1 AFIX 66 C15A 1 0.247226 0.743499 0.496466 10.50000 0.06367 0.02107 = 0.02994 0.00740 -0.01724 0.01227 C16A 1 0.224297 0.845381 0.557891 10.50000 0.05476 0.02704 = 0.04112 0.00604 -0.02401 0.01804 AFIX 43 H16A 2 0.159811 0.874343 0.526840 10.50000 -1.20000 AFIX 65 C17A 1 0.295719 0.904889 0.664750 10.50000 0.04225 0.02585 = 0.03286 0.00256 -0.00786 0.01835 AFIX 43 H17A 2 0.280048 0.974521 0.706731 10.50000 -1.20000 AFIX 65 C18A 1 0.390072 0.862514 0.710184 10.50000 0.02706 0.02149 = 0.02621 0.00804 -0.00086 0.00873 C19A 1 0.413002 0.760632 0.648759 10.50000 0.02824 0.01574 = 0.02530 0.01150 -0.00200 0.00475 AFIX 43 H19A 2 0.477488 0.731672 0.679812 10.50000 -1.20000 AFIX 65 C20A 1 0.341580 0.701124 0.541901 10.50000 0.04955 0.01474 = 0.02422 0.00529 -0.00439 0.01141 AFIX 43 H20A 2 0.357252 0.631492 0.499920 10.50000 -1.20000 AFIX 66 PART 2 C15B 1 0.260996 0.736410 0.494351 10.50000 0.06367 0.02107 = 0.02994 0.00740 -0.01724 0.01227 C16B 1 0.254478 0.844150 0.555437 10.50000 0.05476 0.02704 = 0.04112 0.00604 -0.02401 0.01804 AFIX 43 H16B 2 0.204733 0.880506 0.523465 10.50000 -1.20000 AFIX 65 C17B 1 0.320744 0.898696 0.663303 10.50000 0.04225 0.02585 = 0.03286 0.00256 -0.00786 0.01835 AFIX 43 H17B 2 0.316289 0.972332 0.705053 10.50000 -1.20000 AFIX 65 C18B 1 0.393529 0.845502 0.710084 10.50000 0.02706 0.02149 = 0.02621 0.00804 -0.00086 0.00873 C19B 1 0.400049 0.737762 0.648999 10.50000 0.02824 0.01574 = 0.02530 0.01150 -0.00200 0.00475 AFIX 43 H19B 2 0.449794 0.701407 0.680971 10.50000 -1.20000 AFIX 65 C20B 1 0.333783 0.683215 0.541132 10.50000 0.04955 0.01474 = 0.02422 0.00529 -0.00439 0.01141 AFIX 43 H20B 2 0.338238 0.609579 0.499383 10.50000 -1.20000 AFIX 0 PART 0 C21 1 0.462441 0.914729 0.827131 11.00000 0.01933 0.04108 = 0.02472 0.00957 -0.00051 0.00204 PART 1 C22A 1 0.519051 0.285604 -0.024554 21.00000 0.06161 0.04880 = 0.07630 0.02934 0.03460 0.01790 PART 2 C22B 1 0.553037 0.293820 -0.001069 -21.00000 0.06161 0.04880 = 0.07630 0.02934 0.03460 0.01790 PART 1 C23A 1 0.506089 0.251016 -0.144902 21.00000 0.07733 0.08648 = 0.06306 0.03268 0.01968 0.03214 AFIX 133 H23A 2 0.408850 0.184128 -0.182116 21.00000 -1.50000 H23B 2 0.599877 0.231590 -0.168155 21.00000 -1.50000 H23C 2 0.501237 0.315178 -0.161512 21.00000 -1.50000 AFIX 0 PART 2 C23B 1 0.701701 0.273899 0.039794 -21.00000 0.07733 0.08648 = 0.06306 0.03268 0.01968 0.03214 AFIX 133 H23D 2 0.720942 0.306324 0.117916 -21.00000 -1.50000 H23E 2 0.795476 0.311548 0.015274 -21.00000 -1.50000 H23F 2 0.682567 0.191244 0.011999 -21.00000 -1.50000 AFIX 0 PART 1 C24A 1 0.802863 0.403713 0.001162 21.00000 0.05057 0.13147 = 0.18109 0.09905 0.03999 0.02628 AFIX 137 H24A 2 0.864351 0.351752 -0.013360 21.00000 -1.50000 H24B 2 0.866145 0.478137 0.058334 21.00000 -1.50000 H24C 2 0.777730 0.414478 -0.063486 21.00000 -1.50000 AFIX 0 PART 2 C24B 1 0.439847 0.404722 -0.055279 -21.00000 0.05057 0.13147 = 0.18109 0.09905 0.03999 0.02628 AFIX 137 H24D 2 0.355717 0.329673 -0.093988 -21.00000 -1.50000 H24E 2 0.473443 0.440790 -0.104731 -21.00000 -1.50000 H24F 2 0.398553 0.453926 0.001305 -21.00000 -1.50000 AFIX 0 PART 1 C25A 1 0.656536 0.385360 0.152652 21.00000 0.10222 0.06474 = 0.13022 0.05739 0.00476 0.02170 AFIX 137 H25A 2 0.615768 0.448834 0.182587 21.00000 -1.50000 H25B 2 0.766801 0.409040 0.188347 21.00000 -1.50000 H25C 2 0.589315 0.318640 0.163534 21.00000 -1.50000 AFIX 0 PART 2 C25B 1 0.747847 0.476723 0.018512 -21.00000 0.10222 0.06474 = 0.13022 0.05739 0.00476 0.02170 AFIX 137 H25D 2 0.809238 0.479308 0.080757 -21.00000 -1.50000 H25E 2 0.740430 0.552594 0.033914 -21.00000 -1.50000 H25F 2 0.801679 0.455074 -0.042856 -21.00000 -1.50000 AFIX 0 PART 0 O8 4 0.621502 0.682733 0.352280 11.00000 0.06841 0.08387 = 0.07368 0.02005 -0.01484 0.01031 N3 3 0.746747 0.742990 0.518055 11.00000 0.06415 0.09904 = 0.08820 0.03594 0.00431 0.03030 C26 1 0.691846 0.755961 0.438499 11.00000 0.05078 0.10706 = 0.08498 0.03623 -0.00271 0.02084 C27 1 0.720441 0.886454 0.465088 11.00000 0.11254 0.06078 = 0.17700 0.06578 -0.02010 0.01399 AFIX 137 H27A 2 0.676781 0.893351 0.402248 11.00000 -1.50000 H27B 2 0.835521 0.930282 0.485116 11.00000 -1.50000 H27C 2 0.666784 0.916786 0.524417 11.00000 -1.50000 AFIX 0 C28 1 0.713026 0.618490 0.498920 11.00000 0.10222 0.06474 = 0.13022 0.05739 0.00476 0.02170 AFIX 137 H28A 2 0.651200 0.568563 0.427068 11.00000 -1.50000 H28B 2 0.651650 0.601191 0.551658 11.00000 -1.50000 H28C 2 0.814410 0.605161 0.505653 11.00000 -1.50000 AFIX 0 C29 1 0.823509 0.828889 0.627355 11.00000 0.07417 0.06517 = 0.07008 0.01952 -0.01261 0.02230 AFIX 137 H29A 2 0.857165 0.906144 0.628221 11.00000 -1.50000 H29B 2 0.917194 0.814218 0.650365 11.00000 -1.50000 H29C 2 0.747061 0.823256 0.675945 11.00000 -1.50000 AFIX 0 HKLF 5 REM 3_a.res in P-1 REM wR2 = 0.1363, GooF = S = 1.156, Restrained GooF = 1.150 for all data REM R1 = 0.0550 for 6889 Fo > 4sig(Fo) and 0.0605 for all 7574 data REM 370 parameters refined using 105 restraints END WGHT 0.0384 6.9992 REM Highest difference peak 2.501, deepest hole -1.423, 1-sigma level 0.168 Q1 1 0.1628 0.2695 -0.0017 11.00000 0.05 1.77 ; _shelx_res_checksum 275 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.25059(3) 0.05237(2) -0.01095(2) 0.01903(9) Uani 1 1 d D . . . . O1 O 0.1207(7) 0.1649(5) 0.0943(4) 0.0508(14) Uani 1 1 d . . . . . O2 O -0.1204(7) 0.1414(4) 0.1352(4) 0.0481(13) Uani 1 1 d . . . . . O3 O 0.1549(6) 0.9532(4) 0.0952(4) 0.0423(11) Uani 1 1 d . . . . . O4 O -0.0899(6) 0.9245(4) 0.1366(4) 0.0390(11) Uani 1 1 d . . . . . O5 O 0.4351(5) 1.0043(4) 0.8834(4) 0.0394(11) Uani 1 1 d . . . . . O6 O 0.5459(6) 0.8703(4) 0.8625(4) 0.0393(11) Uani 1 1 d . . . . . O7A O 0.401(2) 0.2437(8) 0.0082(13) 0.040(3) Uani 0.547(7) 1 d D . P A 1 O7B O 0.419(3) 0.2225(11) -0.0267(16) 0.040(3) Uani 0.453(7) 1 d D . P A 2 N1B N 0.218(2) 0.6848(19) 0.3782(17) 0.035(4) Uani 0.5 1 d . . P B 2 N1A N 0.156(2) 0.6817(19) 0.3961(17) 0.035(4) Uani 0.5 1 d . . P C 1 N2A N 0.6530(15) 0.3537(11) 0.0342(13) 0.071(4) Uani 0.547(7) 1 d D . P A 1 N2B N 0.5813(17) 0.3890(12) -0.0066(15) 0.071(4) Uani 0.453(7) 1 d D . P A 2 C1A C 0.1291(19) 0.5602(11) 0.335(2) 0.028(3) Uani 0.5 1 d G U P C 1 C2A C 0.003(2) 0.4768(17) 0.347(2) 0.032(3) Uani 0.5 1 d G U P C 1 H2A H -0.062363 0.498825 0.398736 0.039 Uiso 0.5 1 calc R U P C 1 C3A C -0.029(3) 0.3612(14) 0.284(2) 0.030(2) Uani 0.5 1 d G U P C 1 H3A H -0.115208 0.304165 0.292526 0.036 Uiso 0.5 1 calc R U P C 1 C4A C 0.066(3) 0.3289(12) 0.209(2) 0.0256(15) Uani 0.5 1 d DG U P C 1 C5A C 0.193(3) 0.4123(19) 0.197(2) 0.042(3) Uani 0.5 1 d G U P C 1 H5A H 0.257832 0.390315 0.145699 0.051 Uiso 0.5 1 calc R U P C 1 C6A C 0.224(3) 0.5280(16) 0.260(2) 0.046(4) Uani 0.5 1 d G U P C 1 H6A H 0.310680 0.584977 0.251909 0.056 Uiso 0.5 1 calc R U P C 1 C1B C 0.1766(19) 0.5635(11) 0.327(2) 0.028(3) Uani 0.5 1 d G U P B 2 C2B C 0.047(2) 0.4930(16) 0.3516(19) 0.032(3) Uani 0.5 1 d G U P B 2 H2B H -0.006454 0.525941 0.406437 0.039 Uiso 0.5 1 calc R U P B 2 C3B C -0.003(3) 0.3744(15) 0.295(2) 0.030(2) Uani 0.5 1 d G U P B 2 H3B H -0.091294 0.326280 0.312068 0.036 Uiso 0.5 1 calc R U P B 2 C4B C 0.076(3) 0.3263(11) 0.215(2) 0.0256(15) Uani 0.5 1 d DG U P B 2 C5B C 0.205(3) 0.3967(18) 0.191(2) 0.042(3) Uani 0.5 1 d G U P B 2 H5B H 0.258793 0.363814 0.136053 0.051 Uiso 0.5 1 calc R U P B 2 C6B C 0.255(3) 0.5153(17) 0.247(2) 0.046(4) Uani 0.5 1 d G U P B 2 H6B H 0.343635 0.563476 0.230422 0.056 Uiso 0.5 1 calc R U P B 2 C7 C 0.0192(8) 0.2012(5) 0.1419(5) 0.0308(13) Uani 1 1 d D . . . . C8A C 0.1263(17) 0.7449(10) 0.3374(11) 0.032(4) Uani 0.5 1 d G . P C 1 C9A C -0.0258(14) 0.7121(14) 0.2807(16) 0.036(3) Uani 0.5 1 d G . P C 1 H9A H -0.111031 0.650640 0.283757 0.044 Uiso 0.5 1 calc R U P C 1 C10A C -0.0533(11) 0.7692(19) 0.2196(16) 0.038(3) Uani 0.5 1 d G . P C 1 H10A H -0.157326 0.746859 0.180836 0.046 Uiso 0.5 1 calc R U P C 1 C11A C 0.0713(16) 0.8592(15) 0.2151(12) 0.029(2) Uani 0.5 1 d G . P C 1 C12A C 0.2235(12) 0.8919(9) 0.2718(8) 0.032(2) Uani 0.5 1 d G . P C 1 H12A H 0.308674 0.953373 0.268809 0.039 Uiso 0.5 1 calc R U P C 1 C13A C 0.2510(11) 0.8348(9) 0.3330(8) 0.035(2) Uani 0.5 1 d G . P C 1 H13A H 0.354971 0.857156 0.371733 0.043 Uiso 0.5 1 calc R U P C 1 C8B C 0.1750(16) 0.7410(10) 0.3179(11) 0.032(4) Uani 0.5 1 d G . P B 2 C9B C 0.0169(13) 0.7327(15) 0.2965(16) 0.036(3) Uani 0.5 1 d G . P B 2 H9B H -0.063937 0.688175 0.321387 0.044 Uiso 0.5 1 calc R U P B 2 C10B C -0.0231(10) 0.7897(19) 0.2389(16) 0.038(3) Uani 0.5 1 d G . P B 2 H10B H -0.131250 0.783999 0.224291 0.046 Uiso 0.5 1 calc R U P B 2 C11B C 0.0951(16) 0.8549(16) 0.2025(12) 0.029(2) Uani 0.5 1 d G . P B 2 C12B C 0.2533(13) 0.8631(9) 0.2239(8) 0.032(2) Uani 0.5 1 d G . P B 2 H12B H 0.334065 0.907706 0.199029 0.039 Uiso 0.5 1 calc R U P B 2 C13B C 0.2933(11) 0.8062(9) 0.2815(8) 0.035(2) Uani 0.5 1 d G . P B 2 H13B H 0.401380 0.811883 0.296126 0.043 Uiso 0.5 1 calc R U P B 2 C14 C 0.0463(7) 0.9158(5) 0.1417(5) 0.0285(12) Uani 1 1 d . . . . . C15A C 0.247(7) 0.743(4) 0.4965(17) 0.041(4) Uani 0.5 1 d G . P C 1 C16A C 0.224(6) 0.845(5) 0.558(3) 0.044(6) Uani 0.5 1 d G . P C 1 H16A H 0.159811 0.874343 0.526840 0.052 Uiso 0.5 1 calc R U P C 1 C17A C 0.296(4) 0.905(3) 0.665(3) 0.035(3) Uani 0.5 1 d G . P C 1 H17A H 0.280048 0.974521 0.706731 0.043 Uiso 0.5 1 calc R U P C 1 C18A C 0.390(3) 0.8625(13) 0.7102(11) 0.0256(15) Uani 0.5 1 d DG . P C 1 C19A C 0.413(4) 0.7606(17) 0.649(2) 0.023(3) Uani 0.5 1 d G . P C 1 H19A H 0.477488 0.731672 0.679812 0.028 Uiso 0.5 1 calc R U P C 1 C20A C 0.342(7) 0.701(3) 0.542(2) 0.031(4) Uani 0.5 1 d G . P C 1 H20A H 0.357252 0.631492 0.499920 0.037 Uiso 0.5 1 calc R U P C 1 C15B C 0.261(7) 0.736(4) 0.4944(17) 0.041(4) Uani 0.5 1 d G . P B 2 C16B C 0.254(6) 0.844(4) 0.555(3) 0.044(6) Uani 0.5 1 d G . P B 2 H16B H 0.204733 0.880506 0.523465 0.052 Uiso 0.5 1 calc R U P B 2 C17B C 0.321(4) 0.899(3) 0.663(3) 0.035(3) Uani 0.5 1 d G . P B 2 H17B H 0.316289 0.972332 0.705053 0.043 Uiso 0.5 1 calc R U P B 2 C18B C 0.394(3) 0.8455(13) 0.7101(11) 0.0256(15) Uani 0.5 1 d DG . P B 2 C19B C 0.400(4) 0.7378(16) 0.649(2) 0.023(3) Uani 0.5 1 d G . P B 2 H19B H 0.449794 0.701407 0.680971 0.028 Uiso 0.5 1 calc R U P B 2 C20B C 0.334(7) 0.683(3) 0.541(2) 0.031(4) Uani 0.5 1 d G . P B 2 H20B H 0.338238 0.609579 0.499383 0.037 Uiso 0.5 1 calc R U P B 2 C21 C 0.4624(7) 0.9147(6) 0.8271(4) 0.0318(13) Uani 1 1 d D . . . . C22A C 0.519(2) 0.2856(13) -0.0246(14) 0.061(4) Uani 0.547(7) 1 d D . P A 1 C22B C 0.553(2) 0.2938(15) -0.0011(15) 0.061(4) Uani 0.453(7) 1 d D . P A 2 C23A C 0.506(2) 0.2510(17) -0.1449(13) 0.074(4) Uani 0.547(7) 1 d D . P A 1 H23A H 0.408850 0.184128 -0.182116 0.111 Uiso 0.547(7) 1 calc R U P A 1 H23B H 0.599877 0.231590 -0.168155 0.111 Uiso 0.547(7) 1 calc R U P A 1 H23C H 0.501237 0.315178 -0.161512 0.111 Uiso 0.547(7) 1 calc R U P A 1 C23B C 0.702(3) 0.274(2) 0.0398(18) 0.074(4) Uani 0.453(7) 1 d D . P A 2 H23D H 0.720942 0.306324 0.117916 0.111 Uiso 0.453(7) 1 calc R U P A 2 H23E H 0.795476 0.311548 0.015274 0.111 Uiso 0.453(7) 1 calc R U P A 2 H23F H 0.682567 0.191244 0.011999 0.111 Uiso 0.453(7) 1 calc R U P A 2 C24A C 0.803(2) 0.404(2) 0.001(3) 0.111(7) Uani 0.547(7) 1 d D U P A 1 H24A H 0.864351 0.351752 -0.013360 0.166 Uiso 0.547(7) 1 calc R U P A 1 H24B H 0.866145 0.478137 0.058334 0.166 Uiso 0.547(7) 1 calc R U P A 1 H24C H 0.777730 0.414478 -0.063486 0.166 Uiso 0.547(7) 1 calc R U P A 1 C24B C 0.440(2) 0.405(3) -0.055(3) 0.111(7) Uani 0.453(7) 1 d D . P A 2 H24D H 0.355717 0.329673 -0.093988 0.166 Uiso 0.453(7) 1 calc R U P A 2 H24E H 0.473443 0.440790 -0.104731 0.166 Uiso 0.453(7) 1 calc R U P A 2 H24F H 0.398553 0.453926 0.001305 0.166 Uiso 0.453(7) 1 calc R U P A 2 C25A C 0.657(3) 0.3854(17) 0.1527(16) 0.096(3) Uani 0.547(7) 1 d D U P A 1 H25A H 0.615768 0.448834 0.182587 0.144 Uiso 0.547(7) 1 calc R U P A 1 H25B H 0.766801 0.409040 0.188347 0.144 Uiso 0.547(7) 1 calc R U P A 1 H25C H 0.589315 0.318640 0.163534 0.144 Uiso 0.547(7) 1 calc R U P A 1 C25B C 0.748(3) 0.477(2) 0.019(3) 0.096(3) Uani 0.453(7) 1 d D . P A 2 H25D H 0.809238 0.479308 0.080757 0.144 Uiso 0.453(7) 1 calc R U P A 2 H25E H 0.740430 0.552594 0.033914 0.144 Uiso 0.453(7) 1 calc R U P A 2 H25F H 0.801679 0.455074 -0.042856 0.144 Uiso 0.453(7) 1 calc R U P A 2 O8 O 0.6215(9) 0.6827(7) 0.3523(6) 0.084(2) Uani 1 1 d . . . . . N3 N 0.7467(11) 0.7430(9) 0.5181(8) 0.084(3) Uani 1 1 d . . . . . C26 C 0.6918(13) 0.7560(11) 0.4385(10) 0.084(3) Uani 1 1 d . . . . . C27 C 0.7204(17) 0.8865(10) 0.4651(13) 0.117(6) Uani 1 1 d . . . . . H27A H 0.676781 0.893351 0.402248 0.175 Uiso 1 1 calc R U . . . H27B H 0.835521 0.930282 0.485116 0.175 Uiso 1 1 calc R U . . . H27C H 0.666784 0.916786 0.524417 0.175 Uiso 1 1 calc R U . . . C28 C 0.7130(16) 0.6185(9) 0.4989(11) 0.096(3) Uani 1 1 d . . . . . H28A H 0.651200 0.568563 0.427068 0.144 Uiso 1 1 calc R U . . . H28B H 0.651650 0.601191 0.551658 0.144 Uiso 1 1 calc R U . . . H28C H 0.814410 0.605161 0.505653 0.144 Uiso 1 1 calc R U . . . C29 C 0.8235(13) 0.8289(9) 0.6274(8) 0.074(3) Uani 1 1 d . . . . . H29A H 0.857165 0.906144 0.628221 0.110 Uiso 1 1 calc R U . . . H29B H 0.917194 0.814218 0.650365 0.110 Uiso 1 1 calc R U . . . H29C H 0.747061 0.823256 0.675945 0.110 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.01913(14) 0.01484(13) 0.02151(15) 0.00555(10) -0.00189(10) 0.00679(9) O1 0.061(3) 0.059(3) 0.040(3) 0.010(2) 0.007(2) 0.045(3) O2 0.057(3) 0.025(2) 0.042(3) 0.006(2) 0.006(2) -0.004(2) O3 0.041(3) 0.042(3) 0.049(3) 0.026(2) 0.005(2) 0.010(2) O4 0.039(3) 0.042(3) 0.038(3) 0.016(2) -0.005(2) 0.019(2) O5 0.027(2) 0.044(3) 0.030(2) 0.0006(19) 0.0035(18) 0.0074(19) O6 0.034(2) 0.046(3) 0.028(2) 0.012(2) -0.0077(19) 0.006(2) O7A 0.037(5) 0.028(4) 0.050(10) 0.017(5) 0.001(5) 0.004(4) O7B 0.037(5) 0.028(4) 0.050(10) 0.017(5) 0.001(5) 0.004(4) N1B 0.062(12) 0.021(3) 0.020(6) 0.007(4) -0.008(6) 0.014(8) N1A 0.062(12) 0.021(3) 0.020(6) 0.007(4) -0.008(6) 0.014(8) N2A 0.040(6) 0.051(6) 0.125(11) 0.056(7) 0.005(6) -0.006(5) N2B 0.040(6) 0.051(6) 0.125(11) 0.056(7) 0.005(6) -0.006(5) C1A 0.032(9) 0.023(3) 0.023(4) 0.010(3) -0.004(6) 0.004(4) C2A 0.035(10) 0.020(5) 0.032(4) 0.003(4) 0.007(6) 0.007(6) C3A 0.028(7) 0.022(4) 0.032(5) 0.005(4) 0.005(5) 0.005(4) C4A 0.027(2) 0.021(2) 0.026(2) 0.0080(18) -0.0009(18) 0.009(2) C5A 0.047(5) 0.030(5) 0.049(5) 0.015(4) 0.021(4) 0.013(4) C6A 0.055(8) 0.029(5) 0.048(7) 0.016(5) 0.016(5) 0.004(5) C1B 0.032(9) 0.023(3) 0.023(4) 0.010(3) -0.004(6) 0.004(4) C2B 0.035(10) 0.020(5) 0.032(4) 0.003(4) 0.007(6) 0.007(6) C3B 0.028(7) 0.022(4) 0.032(5) 0.005(4) 0.005(5) 0.005(4) C4B 0.027(2) 0.021(2) 0.026(2) 0.0080(18) -0.0009(18) 0.009(2) C5B 0.047(5) 0.030(5) 0.049(5) 0.015(4) 0.021(4) 0.013(4) C6B 0.055(8) 0.029(5) 0.048(7) 0.016(5) 0.016(5) 0.004(5) C7 0.045(4) 0.024(3) 0.024(3) 0.007(2) 0.001(3) 0.018(3) C8A 0.047(9) 0.022(3) 0.020(5) 0.007(3) -0.011(5) 0.009(5) C9A 0.033(8) 0.028(7) 0.039(7) 0.019(6) -0.004(7) -0.007(6) C10A 0.030(5) 0.035(8) 0.043(8) 0.020(7) -0.012(5) 0.000(5) C11A 0.035(5) 0.027(3) 0.025(4) 0.014(3) -0.003(4) 0.009(3) C12A 0.028(5) 0.038(6) 0.039(7) 0.025(6) 0.004(4) 0.010(4) C13A 0.037(5) 0.037(5) 0.032(6) 0.015(5) -0.007(4) 0.012(4) C8B 0.047(9) 0.022(3) 0.020(5) 0.007(3) -0.011(5) 0.009(5) C9B 0.033(8) 0.028(7) 0.039(7) 0.019(6) -0.004(7) -0.007(6) C10B 0.030(5) 0.035(8) 0.043(8) 0.020(7) -0.012(5) 0.000(5) C11B 0.035(5) 0.027(3) 0.025(4) 0.014(3) -0.003(4) 0.009(3) C12B 0.028(5) 0.038(6) 0.039(7) 0.025(6) 0.004(4) 0.010(4) C13B 0.037(5) 0.037(5) 0.032(6) 0.015(5) -0.007(4) 0.012(4) C14 0.031(3) 0.024(3) 0.029(3) 0.012(2) -0.003(2) 0.007(2) C15A 0.064(9) 0.021(5) 0.030(3) 0.007(3) -0.017(4) 0.012(5) C16A 0.055(15) 0.027(3) 0.041(4) 0.006(3) -0.024(7) 0.018(8) C17A 0.042(10) 0.026(4) 0.033(4) 0.003(3) -0.008(5) 0.018(4) C18A 0.027(2) 0.021(2) 0.026(2) 0.0080(18) -0.0009(18) 0.009(2) C19A 0.028(6) 0.016(7) 0.025(3) 0.011(5) -0.002(3) 0.005(7) C20A 0.050(6) 0.015(8) 0.024(3) 0.005(4) -0.004(3) 0.011(8) C15B 0.064(9) 0.021(5) 0.030(3) 0.007(3) -0.017(4) 0.012(5) C16B 0.055(15) 0.027(3) 0.041(4) 0.006(3) -0.024(7) 0.018(8) C17B 0.042(10) 0.026(4) 0.033(4) 0.003(3) -0.008(5) 0.018(4) C18B 0.027(2) 0.021(2) 0.026(2) 0.0080(18) -0.0009(18) 0.009(2) C19B 0.028(6) 0.016(7) 0.025(3) 0.011(5) -0.002(3) 0.005(7) C20B 0.050(6) 0.015(8) 0.024(3) 0.005(4) -0.004(3) 0.011(8) C21 0.019(3) 0.041(3) 0.025(3) 0.010(3) -0.001(2) 0.002(2) C22A 0.062(9) 0.049(5) 0.076(10) 0.029(6) 0.035(8) 0.018(6) C22B 0.062(9) 0.049(5) 0.076(10) 0.029(6) 0.035(8) 0.018(6) C23A 0.077(10) 0.086(10) 0.063(9) 0.033(8) 0.020(7) 0.032(8) C23B 0.077(10) 0.086(10) 0.063(9) 0.033(8) 0.020(7) 0.032(8) C24A 0.051(9) 0.131(15) 0.181(19) 0.099(15) 0.040(11) 0.026(9) C24B 0.051(9) 0.131(15) 0.181(19) 0.099(15) 0.040(11) 0.026(9) C25A 0.102(8) 0.065(5) 0.130(9) 0.057(6) 0.005(7) 0.022(5) C25B 0.102(8) 0.065(5) 0.130(9) 0.057(6) 0.005(7) 0.022(5) O8 0.068(5) 0.084(5) 0.074(5) 0.020(4) -0.015(4) 0.010(4) N3 0.064(6) 0.099(7) 0.088(7) 0.036(6) 0.004(5) 0.030(5) C26 0.051(6) 0.107(9) 0.085(8) 0.036(7) -0.003(6) 0.021(6) C27 0.113(11) 0.061(7) 0.177(15) 0.066(9) -0.020(10) 0.014(7) C28 0.102(8) 0.065(5) 0.130(9) 0.057(6) 0.005(7) 0.022(5) C29 0.074(7) 0.065(6) 0.070(7) 0.020(5) -0.013(5) 0.022(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pr1 O2 124.0(2) . 2 ? O1 Pr1 O3 78.8(2) . 1_545 ? O1 Pr1 O4 77.24(18) . 2_565 ? O1 Pr1 O5 158.7(2) . 1_544 ? O1 Pr1 O6 87.68(18) . 2_666 ? O1 Pr1 O7A 75.8(4) . . ? O1 Pr1 O7B 87.2(5) . . ? O2 Pr1 O7A 144.7(4) 2 . ? O2 Pr1 O7B 133.4(4) 2 . ? O3 Pr1 O2 75.70(18) 1_545 2 ? O3 Pr1 O4 125.46(18) 1_545 2_565 ? O3 Pr1 O6 74.42(17) 1_545 2_666 ? O3 Pr1 O7A 139.6(4) 1_545 . ? O3 Pr1 O7B 149.8(5) 1_545 . ? O4 Pr1 O2 78.51(18) 2_565 2 ? O4 Pr1 O7A 78.4(5) 2_565 . ? O4 Pr1 O7B 76.1(7) 2_565 . ? O5 Pr1 O2 73.90(18) 1_544 2 ? O5 Pr1 O3 119.76(18) 1_544 1_545 ? O5 Pr1 O4 97.28(18) 1_544 2_565 ? O5 Pr1 O6 87.72(17) 1_544 2_666 ? O5 Pr1 O7A 83.0(3) 1_544 . ? O5 Pr1 O7B 71.4(5) 1_544 . ? O6 Pr1 O2 130.18(19) 2_666 2 ? O6 Pr1 O4 150.79(17) 2_666 2_565 ? O6 Pr1 O7A 73.7(5) 2_666 . ? O6 Pr1 O7B 78.4(6) 2_666 . ? C7 O1 Pr1 164.6(5) . . ? C7 O2 Pr1 125.7(4) . 2 ? C14 O3 Pr1 150.6(4) . 1_565 ? C14 O4 Pr1 133.7(4) . 2_565 ? C21 O5 Pr1 137.9(4) . 1_566 ? C21 O6 Pr1 132.1(4) . 2_666 ? C22A O7A Pr1 134.8(10) . . ? C22B O7B Pr1 144.8(19) . . ? C1B N1B C8B 118(2) . . ? C1B N1B C15B 116(3) . . ? C8B N1B C15B 124(3) . . ? C8A N1A C1A 117.0(19) . . ? C15A N1A C1A 123(3) . . ? C15A N1A C8A 118(3) . . ? C22A N2A C24A 128.0(19) . . ? C22A N2A C25A 114.8(15) . . ? C24A N2A C25A 117.2(19) . . ? C22B N2B C24B 115.1(17) . . ? C22B N2B C25B 123.5(17) . . ? C24B N2B C25B 120.9(17) . . ? C2A C1A N1A 120.1(14) . . ? C2A C1A C6A 120.0 . . ? C6A C1A N1A 119.8(14) . . ? C1A C2A H2A 120.0 . . ? C1A C2A C3A 120.0 . . ? C3A C2A H2A 120.0 . . ? C2A C3A H3A 120.0 . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3A 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A C7 116.0(18) . . ? C5A C4A C7 124.0(18) . . ? C4A C5A H5A 120.0 . . ? C6A C5A C4A 120.0 . . ? C6A C5A H5A 120.0 . . ? C1A C6A H6A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6A 120.0 . . ? C2B C1B N1B 119.6(14) . . ? C2B C1B C6B 120.0 . . ? C6B C1B N1B 120.2(14) . . ? C1B C2B H2B 120.0 . . ? C1B C2B C3B 120.0 . . ? C3B C2B H2B 120.0 . . ? C2B C3B H3B 120.0 . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C3B C4B C5B 120.0 . . ? C3B C4B C7 124.0(18) . . ? C5B C4B C7 115.6(18) . . ? C4B C5B H5B 120.0 . . ? C4B C5B C6B 120.0 . . ? C6B C5B H5B 120.0 . . ? C1B C6B H6B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B H6B 120.0 . . ? O1 C7 C4A 118.4(13) . . ? O1 C7 C4B 116.4(13) . . ? O2 C7 O1 124.9(6) . . ? O2 C7 C4A 116.6(13) . . ? O2 C7 C4B 118.6(13) . . ? C9A C8A N1A 119.6(12) . . ? C9A C8A C13A 120.0 . . ? C13A C8A N1A 120.3(12) . . ? C8A C9A H9A 120.0 . . ? C10A C9A C8A 120.0 . . ? C10A C9A H9A 120.0 . . ? C9A C10A H10A 120.0 . . ? C9A C10A C11A 120.0 . . ? C11A C10A H10A 120.0 . . ? C10A C11A C14 120.5(10) . . ? C12A C11A C10A 120.0 . . ? C12A C11A C14 119.3(10) . . ? C11A C12A H12A 120.0 . . ? C11A C12A C13A 120.0 . . ? C13A C12A H12A 120.0 . . ? C8A C13A H13A 120.0 . . ? C12A C13A C8A 120.0 . . ? C12A C13A H13A 120.0 . . ? C9B C8B N1B 120.7(11) . . ? C9B C8B C13B 120.0 . . ? C13B C8B N1B 119.3(11) . . ? C8B C9B H9B 120.0 . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9B 120.0 . . ? C9B C10B H10B 120.0 . . ? C9B C10B C11B 120.0 . . ? C11B C10B H10B 120.0 . . ? C10B C11B C14 118.0(10) . . ? C12B C11B C10B 120.0 . . ? C12B C11B C14 122.0(10) . . ? C11B C12B H12B 120.0 . . ? C11B C12B C13B 120.0 . . ? C13B C12B H12B 120.0 . . ? C8B C13B H13B 120.0 . . ? C12B C13B C8B 120.0 . . ? C12B C13B H13B 120.0 . . ? O3 C14 C11A 122.4(7) . . ? O3 C14 C11B 112.4(8) . . ? O4 C14 O3 125.0(6) . . ? O4 C14 C11A 112.6(8) . . ? O4 C14 C11B 122.6(8) . . ? N1A C15A C16A 116(4) . . ? N1A C15A C20A 123(4) . . ? C16A C15A C20A 120.0 . . ? C15A C16A H16A 120.0 . . ? C17A C16A C15A 120.0 . . ? C17A C16A H16A 120.0 . . ? C16A C17A H17A 120.0 . . ? C18A C17A C16A 120.0 . . ? C18A C17A H17A 120.0 . . ? C17A C18A C19A 120.0 . . ? C17A C18A C21 124.5(17) . . ? C19A C18A C21 115.4(17) . . ? C18A C19A H19A 120.0 . . ? C18A C19A C20A 120.0 . . ? C20A C19A H19A 120.0 . . ? C15A C20A H20A 120.0 . . ? C19A C20A C15A 120.0 . . ? C19A C20A H20A 120.0 . . ? C16B C15B N1B 122(4) . . ? C16B C15B C20B 120.0 . . ? C20B C15B N1B 117(4) . . ? C15B C16B H16B 120.0 . . ? C17B C16B C15B 120.0 . . ? C17B C16B H16B 120.0 . . ? C16B C17B H17B 120.0 . . ? C16B C17B C18B 120.0 . . ? C18B C17B H17B 120.0 . . ? C17B C18B C21 114.5(17) . . ? C19B C18B C17B 120.0 . . ? C19B C18B C21 125.4(17) . . ? C18B C19B H19B 120.0 . . ? C20B C19B C18B 120.0 . . ? C20B C19B H19B 120.0 . . ? C15B C20B H20B 120.0 . . ? C19B C20B C15B 120.0 . . ? C19B C20B H20B 120.0 . . ? O5 C21 O6 124.3(5) . . ? O5 C21 C18A 115.1(9) . . ? O5 C21 C18B 123.6(9) . . ? O6 C21 C18A 120.6(9) . . ? O6 C21 C18B 112.1(9) . . ? O7A C22A N2A 124.4(18) . . ? O7A C22A C23A 117.8(16) . . ? N2A C22A C23A 117.7(16) . . ? O7B C22B N2B 122.3(19) . . ? O7B C22B C23B 123(2) . . ? N2B C22B C23B 114.9(18) . . ? C22A C23A H23A 109.5 . . ? C22A C23A H23B 109.5 . . ? C22A C23A H23C 109.5 . . ? H23A C23A H23B 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? C22B C23B H23D 109.5 . . ? C22B C23B H23E 109.5 . . ? C22B C23B H23F 109.5 . . ? H23D C23B H23E 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? N2A C24A H24A 109.5 . . ? N2A C24A H24B 109.5 . . ? N2A C24A H24C 109.5 . . ? H24A C24A H24B 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? N2B C24B H24D 109.5 . . ? N2B C24B H24E 109.5 . . ? N2B C24B H24F 109.5 . . ? H24D C24B H24E 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? N2A C25A H25A 109.5 . . ? N2A C25A H25B 109.5 . . ? N2A C25A H25C 109.5 . . ? H25A C25A H25B 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? N2B C25B H25D 109.5 . . ? N2B C25B H25E 109.5 . . ? N2B C25B H25F 109.5 . . ? H25D C25B H25E 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C26 N3 C28 113.7(11) . . ? C26 N3 C29 130.0(11) . . ? C29 N3 C28 116.0(10) . . ? O8 C26 N3 128.0(13) . . ? O8 C26 C27 120.4(12) . . ? N3 C26 C27 111.6(11) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 H28A 109.5 . . ? N3 C28 H28B 109.5 . . ? N3 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 H29A 109.5 . . ? N3 C29 H29B 109.5 . . ? N3 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O1 2.294(5) . ? Pr1 O2 2.379(4) 2 ? Pr1 O3 2.343(5) 1_545 ? Pr1 O4 2.366(4) 2_565 ? Pr1 O5 2.317(5) 1_544 ? Pr1 O6 2.343(4) 2_666 ? Pr1 O7A 2.407(9) . ? Pr1 O7B 2.409(12) . ? O1 C7 1.249(8) . ? O2 C7 1.235(8) . ? O3 C14 1.263(8) . ? O4 C14 1.256(8) . ? O5 C21 1.261(8) . ? O6 C21 1.265(8) . ? O7A C22A 1.221(15) . ? O7B C22B 1.214(17) . ? N1B C1B 1.42(3) . ? N1B C8B 1.42(3) . ? N1B C15B 1.46(3) . ? N1A C1A 1.46(2) . ? N1A C8A 1.44(2) . ? N1A C15A 1.38(3) . ? N2A C22A 1.270(16) . ? N2A C24A 1.474(16) . ? N2A C25A 1.517(17) . ? N2B C22B 1.253(17) . ? N2B C24B 1.510(17) . ? N2B C25B 1.514(17) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A H2A 0.9500 . ? C2A C3A 1.3900 . ? C3A H3A 0.9500 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C4A C7 1.515(13) . ? C5A H5A 0.9500 . ? C5A C6A 1.3900 . ? C6A H6A 0.9500 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C2B H2B 0.9500 . ? C2B C3B 1.3900 . ? C3B H3B 0.9500 . ? C3B C4B 1.3900 . ? C4B C5B 1.3900 . ? C4B C7 1.499(13) . ? C5B H5B 0.9500 . ? C5B C6B 1.3900 . ? C6B H6B 0.9500 . ? C8A C9A 1.3900 . ? C8A C13A 1.3900 . ? C9A H9A 0.9500 . ? C9A C10A 1.3900 . ? C10A H10A 0.9500 . ? C10A C11A 1.3900 . ? C11A C12A 1.3900 . ? C11A C14 1.518(13) . ? C12A H12A 0.9500 . ? C12A C13A 1.3900 . ? C13A H13A 0.9500 . ? C8B C9B 1.3900 . ? C8B C13B 1.3900 . ? C9B H9B 0.9500 . ? C9B C10B 1.3900 . ? C10B H10B 0.9500 . ? C10B C11B 1.3900 . ? C11B C12B 1.3900 . ? C11B C14 1.501(12) . ? C12B H12B 0.9500 . ? C12B C13B 1.3900 . ? C13B H13B 0.9500 . ? C15A C16A 1.3900 . ? C15A C20A 1.3900 . ? C16A H16A 0.9500 . ? C16A C17A 1.3900 . ? C17A H17A 0.9500 . ? C17A C18A 1.3900 . ? C18A C19A 1.3900 . ? C18A C21 1.511(14) . ? C19A H19A 0.9500 . ? C19A C20A 1.3900 . ? C20A H20A 0.9500 . ? C15B C16B 1.3900 . ? C15B C20B 1.3900 . ? C16B H16B 0.9500 . ? C16B C17B 1.3900 . ? C17B H17B 0.9500 . ? C17B C18B 1.3900 . ? C18B C19B 1.3900 . ? C18B C21 1.509(14) . ? C19B H19B 0.9500 . ? C19B C20B 1.3900 . ? C20B H20B 0.9500 . ? C22A C23A 1.530(17) . ? C22B C23B 1.552(18) . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? O8 C26 1.204(13) . ? N3 C26 1.271(14) . ? N3 C28 1.515(14) . ? N3 C29 1.478(13) . ? C26 C27 1.578(16) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pr1 O1 C7 O2 1(2) . . . . ? Pr1 O1 C7 C4A -175.6(19) . . . . ? Pr1 O1 C7 C4B 179.0(19) . . . . ? Pr1 O2 C7 O1 -10.3(10) 2 . . . ? Pr1 O2 C7 C4A 166.8(13) 2 . . . ? Pr1 O2 C7 C4B 172.1(14) 2 . . . ? Pr1 O3 C14 O4 3.5(13) 1_565 . . . ? Pr1 O3 C14 C11A -173.6(10) 1_565 . . . ? Pr1 O3 C14 C11B -178.4(9) 1_565 . . . ? Pr1 O4 C14 O3 24.0(9) 2_565 . . . ? Pr1 O4 C14 C11A -158.6(8) 2_565 . . . ? Pr1 O4 C14 C11B -153.9(9) 2_565 . . . ? Pr1 O5 C21 O6 -87.3(8) 1_566 . . . ? Pr1 O5 C21 C18A 94.0(13) 1_566 . . . ? Pr1 O5 C21 C18B 90.3(14) 1_566 . . . ? Pr1 O6 C21 O5 -24.2(10) 2_666 . . . ? Pr1 O6 C21 C18A 154.5(12) 2_666 . . . ? Pr1 O6 C21 C18B 157.9(11) 2_666 . . . ? Pr1 O7A C22A N2A -113(2) . . . . ? Pr1 O7A C22A C23A 65(2) . . . . ? Pr1 O7B C22B N2B -161.5(18) . . . . ? Pr1 O7B C22B C23B 19(3) . . . . ? N1B C1B C2B C3B 174(2) . . . . ? N1B C1B C6B C5B -174(2) . . . . ? N1B C8B C9B C10B 179.0(14) . . . . ? N1B C8B C13B C12B -179.0(14) . . . . ? N1B C15B C16B C17B -169(5) . . . . ? N1B C15B C20B C19B 170(4) . . . . ? N1A C1A C2A C3A 176(2) . . . . ? N1A C1A C6A C5A -176(2) . . . . ? N1A C8A C9A C10A -176.9(14) . . . . ? N1A C8A C13A C12A 176.9(14) . . . . ? N1A C15A C16A C17A 171(4) . . . . ? N1A C15A C20A C19A -171(5) . . . . ? C1A N1A C8A C9A 60.8(16) . . . . ? C1A N1A C8A C13A -116.2(15) . . . . ? C1A N1A C15A C16A -161.0(19) . . . . ? C1A N1A C15A C20A 10(5) . . . . ? C1A C2A C3A C4A 0.0 . . . . ? C2A C1A C6A C5A 0.0 . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C2A C3A C4A C7 -178(2) . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C3A C4A C7 O1 -161.4(13) . . . . ? C3A C4A C7 O2 21(2) . . . . ? C4A C5A C6A C1A 0.0 . . . . ? C5A C4A C7 O1 21(2) . . . . ? C5A C4A C7 O2 -156.6(15) . . . . ? C6A C1A C2A C3A 0.0 . . . . ? C1B N1B C8B C9B 74.1(16) . . . . ? C1B N1B C8B C13B -106.8(15) . . . . ? C1B N1B C15B C16B -159(2) . . . . ? C1B N1B C15B C20B 31(4) . . . . ? C1B C2B C3B C4B 0.0 . . . . ? C2B C1B C6B C5B 0.0 . . . . ? C2B C3B C4B C5B 0.0 . . . . ? C2B C3B C4B C7 -173(2) . . . . ? C3B C4B C5B C6B 0.0 . . . . ? C3B C4B C7 O1 -161.2(15) . . . . ? C3B C4B C7 O2 17(2) . . . . ? C4B C5B C6B C1B 0.0 . . . . ? C5B C4B C7 O1 26.0(19) . . . . ? C5B C4B C7 O2 -156.2(13) . . . . ? C6B C1B C2B C3B 0.0 . . . . ? C7 C4A C5A C6A 178(2) . . . . ? C7 C4B C5B C6B 173(2) . . . . ? C8A N1A C1A C2A -111.1(19) . . . . ? C8A N1A C1A C6A 65(2) . . . . ? C8A N1A C15A C16A 38(4) . . . . ? C8A N1A C15A C20A -151(2) . . . . ? C8A C9A C10A C11A 0.0 . . . . ? C9A C8A C13A C12A 0.0 . . . . ? C9A C10A C11A C12A 0.0 . . . . ? C9A C10A C11A C14 175.0(13) . . . . ? C10A C11A C12A C13A 0.0 . . . . ? C10A C11A C14 O3 -145.1(8) . . . . ? C10A C11A C14 O4 37.4(9) . . . . ? C11A C12A C13A C8A 0.0 . . . . ? C12A C11A C14 O3 29.9(15) . . . . ? C12A C11A C14 O4 -147.6(9) . . . . ? C13A C8A C9A C10A 0.0 . . . . ? C8B N1B C1B C2B -104(2) . . . . ? C8B N1B C1B C6B 71(2) . . . . ? C8B N1B C15B C16B 3(5) . . . . ? C8B N1B C15B C20B -166.2(19) . . . . ? C8B C9B C10B C11B 0.0 . . . . ? C9B C8B C13B C12B 0.0 . . . . ? C9B C10B C11B C12B 0.0 . . . . ? C9B C10B C11B C14 -179.3(13) . . . . ? C10B C11B C12B C13B 0.0 . . . . ? C10B C11B C14 O3 -167.0(6) . . . . ? C10B C11B C14 O4 11.1(11) . . . . ? C11B C12B C13B C8B 0.0 . . . . ? C12B C11B C14 O3 13.7(14) . . . . ? C12B C11B C14 O4 -168.2(8) . . . . ? C13B C8B C9B C10B 0.0 . . . . ? C14 C11A C12A C13A -175.0(13) . . . . ? C14 C11B C12B C13B 179.3(13) . . . . ? C15A N1A C1A C2A 88(4) . . . . ? C15A N1A C1A C6A -96(4) . . . . ? C15A N1A C8A C9A -137(3) . . . . ? C15A N1A C8A C13A 46(4) . . . . ? C15A C16A C17A C18A 0.0 . . . . ? C16A C15A C20A C19A 0.0 . . . . ? C16A C17A C18A C19A 0.0 . . . . ? C16A C17A C18A C21 -175(2) . . . . ? C17A C18A C19A C20A 0.0 . . . . ? C17A C18A C21 O5 -2(2) . . . . ? C17A C18A C21 O6 179.4(16) . . . . ? C18A C19A C20A C15A 0.0 . . . . ? C19A C18A C21 O5 -176.9(16) . . . . ? C19A C18A C21 O6 4(2) . . . . ? C20A C15A C16A C17A 0.0 . . . . ? C15B N1B C1B C2B 60(4) . . . . ? C15B N1B C1B C6B -126(3) . . . . ? C15B N1B C8B C9B -88(4) . . . . ? C15B N1B C8B C13B 91(3) . . . . ? C15B C16B C17B C18B 0.0 . . . . ? C16B C15B C20B C19B 0.0 . . . . ? C16B C17B C18B C19B 0.0 . . . . ? C16B C17B C18B C21 179(2) . . . . ? C17B C18B C19B C20B 0.0 . . . . ? C17B C18B C21 O5 11(2) . . . . ? C17B C18B C21 O6 -170.9(15) . . . . ? C18B C19B C20B C15B 0.0 . . . . ? C19B C18B C21 O5 -169.7(18) . . . . ? C19B C18B C21 O6 8(2) . . . . ? C20B C15B C16B C17B 0.0 . . . . ? C21 C18A C19A C20A 175(2) . . . . ? C21 C18B C19B C20B -179(3) . . . . ? C24A N2A C22A O7A 176.8(17) . . . . ? C24A N2A C22A C23A -1(2) . . . . ? C24B N2B C22B O7B -4(2) . . . . ? C24B N2B C22B C23B 175(2) . . . . ? C25A N2A C22A O7A -2.6(19) . . . . ? C25A N2A C22A C23A 179.3(15) . . . . ? C25B N2B C22B O7B -176(2) . . . . ? C25B N2B C22B C23B 3(3) . . . . ? C28 N3 C26 O8 -1.6(19) . . . . ? C28 N3 C26 C27 176.3(11) . . . . ? C29 N3 C26 O8 -175.2(12) . . . . ? C29 N3 C26 C27 2.7(18) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.789(2) 2 0.211(2)