#------------------------------------------------------------------------------ #$Date: 2019-11-08 01:09:51 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224431 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700033.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_7700033 loop_ _publ_author_name 'Fecker, Ann Christin' 'Freytag, Matthias' 'Jones, Peter G.' 'Walter, Marc D.' _publ_section_title ; Synthesis and molecular structure of enantiomerically pure pentadienyl complexes of the rare-earth metals. ; _journal_issue 23 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8297 _journal_page_last 8302 _journal_paper_doi 10.1039/c9dt01721f _journal_volume 48 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_sum 'C39 H57 Pr' _chemical_formula_weight 666.75 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2019-04-24 deposited with the CCDC. 2019-05-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.142(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.4762(3) _cell_length_b 18.0442(7) _cell_length_c 19.7324(7) _cell_measurement_reflns_used 17227 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.3750 _cell_measurement_theta_min 2.4300 _cell_volume 3347.9(2) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'Bruker XP' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.1419 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.961 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_unetI/netI 0.0741 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.961 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 154014 _diffrn_reflns_point_group_measured_fraction_full 0.967 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_theta_full 30.500 _diffrn_reflns_theta_max 30.891 _diffrn_reflns_theta_min 2.166 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 1.480 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1400 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.999 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.129 _refine_ls_abs_structure_details ; Flack x determined using 7004 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.035(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 813 _refine_ls_number_reflns 19885 _refine_ls_number_restraints 97 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0392 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.0689 _reflns_Friedel_coverage 0.901 _reflns_Friedel_fraction_full 0.949 _reflns_Friedel_fraction_max 0.917 _reflns_number_gt 16814 _reflns_number_total 19885 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt01721f2.cif _cod_data_source_block ann67 _cod_depositor_comments 'Adding full bibliography for 7700030--7700033.cif.' _cod_database_code 7700033 _shelx_shelxl_version_number 2017/1 _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. ; _shelx_estimated_absorpt_t_min 0.665 _shelx_estimated_absorpt_t_max 0.971 _shelx_res_file ; TITL ann67 in P2(1) shelx.res created by SHELXL-2017/1 at 11:51:46 on 17-Apr-2019 CELL 0.71073 9.476204 18.044158 19.732366 90.0000 97.1422 90.0000 ZERR 4.00 0.000300 0.000700 0.000700 0.0000 0.0030 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H Pr UNIT 156 228 4 OMIT -7 -11 21 OMIT 4 0 0 OMIT -10 -13 15 OMIT -2 0 1 FMAP 2 PLAN 10 ACTA 61 CONF C101 > C313 C401 > C413 RTAB CONT PR1 C105 RTAB CONT PR1 C205 RTAB CONT PR1 C305 RTAB CONT PR2 C405 RTAB CONT PR2 C505 RTAB CONT Pr2 C605 SADI C101 H10X C101 H10Y C201 H20X C201 H20Y C301 H30X C301 H30Y = C401 H40X C401 H40Y C501 H50X C501 H50Y C601 H60X C601 H60Y SADI C103 H103 C203 H203 C303 H303 C403 H403 C503 H503 C603 H603 SADI C105 H105 C205 H205 C305 H305 C405 H405 C505 H505 C605 H605 SIZE 0.3 0.15 0.02 TEMP -173 PLAN 10 L.S. 8 WGHT 0.023800 FVAR 1.08235 PR1 3 0.764687 0.205687 0.678053 11.00000 0.01200 0.01253 = 0.01297 -0.00050 0.00031 -0.00044 C101 1 0.492821 0.171785 0.709436 11.00000 0.01538 0.01504 = 0.03004 0.00740 0.00185 -0.00089 H10X 2 0.482576 0.221472 0.715123 11.00000 -1.20000 H10Y 2 0.469533 0.139242 0.742466 11.00000 -1.20000 C102 1 0.489214 0.147461 0.642731 11.00000 0.01044 0.01693 = 0.02589 0.00146 -0.00859 -0.00097 C103 1 0.527376 0.188956 0.586661 11.00000 0.01178 0.01781 = 0.01599 -0.00230 -0.00360 0.00157 H103 2 0.531379 0.162221 0.549510 11.00000 -1.20000 C104 1 0.544599 0.267739 0.579308 11.00000 0.00923 0.02074 = 0.01716 -0.00102 -0.00313 -0.00041 C105 1 0.539812 0.323253 0.625814 11.00000 0.01920 0.01607 = 0.01662 -0.00187 0.00258 0.00308 H105 2 0.519420 0.314767 0.670143 11.00000 -1.20000 C106 1 0.546175 0.403258 0.604832 11.00000 0.01577 0.01478 = 0.02075 -0.00297 -0.00017 0.00062 AFIX 23 H10A 2 0.625915 0.428109 0.633194 11.00000 -1.20000 H10B 2 0.456899 0.428462 0.612778 11.00000 -1.20000 AFIX 0 C107 1 0.566613 0.409928 0.530269 11.00000 0.01722 0.01598 = 0.01684 0.00161 0.00152 0.00261 AFIX 13 H107 2 0.574955 0.461648 0.513001 11.00000 -1.20000 AFIX 0 C108 1 0.686623 0.356631 0.516383 11.00000 0.01445 0.02143 = 0.02184 -0.00212 0.00074 -0.00076 AFIX 23 H10C 2 0.761369 0.349756 0.555617 11.00000 -1.20000 H10D 2 0.728277 0.367227 0.473822 11.00000 -1.20000 AFIX 0 C109 1 0.570501 0.295172 0.509131 11.00000 0.01665 0.01739 = 0.01619 -0.00108 -0.00282 0.00325 AFIX 13 H109 2 0.582040 0.255777 0.474603 11.00000 -1.20000 AFIX 0 C110 1 0.461456 0.358626 0.484944 11.00000 0.01578 0.01939 = 0.01923 0.00074 0.00229 0.00194 C111 1 0.309605 0.353474 0.501054 11.00000 0.01533 0.02336 = 0.02855 -0.00226 -0.00502 -0.00174 AFIX 137 H11A 2 0.264662 0.402387 0.495661 11.00000 -1.50000 H11B 2 0.309312 0.336422 0.548189 11.00000 -1.50000 H11C 2 0.256590 0.318280 0.469734 11.00000 -1.50000 AFIX 0 C112 1 0.458989 0.374348 0.408611 11.00000 0.02714 0.02394 = 0.02062 0.00222 -0.00324 0.00512 AFIX 137 H11D 2 0.402536 0.418993 0.396511 11.00000 -1.50000 H11E 2 0.416465 0.332155 0.382254 11.00000 -1.50000 H11F 2 0.556386 0.381967 0.398176 11.00000 -1.50000 AFIX 0 C113 1 0.455069 0.066885 0.628896 11.00000 0.02278 0.02012 = 0.03699 0.00594 -0.00494 -0.00494 AFIX 137 H11G 2 0.487064 0.037618 0.669767 11.00000 -1.50000 H11H 2 0.503794 0.049689 0.590815 11.00000 -1.50000 H11I 2 0.352146 0.060950 0.617111 11.00000 -1.50000 AFIX 0 C201 1 0.789537 0.210723 0.820054 11.00000 0.02239 0.02796 = 0.01437 -0.00134 0.00397 -0.00804 H20X 2 0.744632 0.181776 0.849526 11.00000 -1.20000 H20Y 2 0.879981 0.194264 0.818899 11.00000 -1.20000 C202 1 0.738689 0.279169 0.801653 11.00000 0.01345 0.03539 = 0.01453 -0.00682 0.00373 -0.01059 C203 1 0.790818 0.328582 0.755390 11.00000 0.01602 0.01598 = 0.01649 -0.00554 0.00081 0.00096 H203 2 0.739986 0.368906 0.746419 11.00000 -1.20000 C204 1 0.927455 0.330675 0.730960 11.00000 0.01382 0.01338 = 0.01536 -0.00402 -0.00045 -0.00082 C205 1 1.037406 0.281937 0.743537 11.00000 0.02017 0.01507 = 0.01687 0.00087 0.00396 0.00051 H205 2 1.034628 0.241873 0.773542 11.00000 -1.20000 C206 1 1.181664 0.300360 0.722787 11.00000 0.01582 0.02046 = 0.02407 -0.00005 0.00246 0.00171 AFIX 23 H20A 2 1.212438 0.260014 0.693950 11.00000 -1.20000 H20B 2 1.252230 0.304483 0.764045 11.00000 -1.20000 AFIX 0 C207 1 1.175478 0.373178 0.683258 11.00000 0.01474 0.02137 = 0.01758 0.00158 0.00393 -0.00408 AFIX 13 H207 2 1.266185 0.388546 0.666256 11.00000 -1.20000 AFIX 0 C208 1 1.043820 0.370057 0.628762 11.00000 0.02319 0.02250 = 0.01664 -0.00063 0.00232 -0.00005 AFIX 23 H20C 2 1.019370 0.319706 0.611131 11.00000 -1.20000 H20D 2 1.045450 0.406209 0.591128 11.00000 -1.20000 AFIX 0 C209 1 0.957925 0.395831 0.686513 11.00000 0.01263 0.01239 = 0.01848 -0.00161 0.00068 -0.00125 AFIX 13 H209 2 0.875496 0.429276 0.672095 11.00000 -1.20000 AFIX 0 C210 1 1.097943 0.435217 0.720320 11.00000 0.01780 0.01560 = 0.02018 0.00069 0.00214 -0.00676 C211 1 1.121773 0.440667 0.797509 11.00000 0.02327 0.02049 = 0.02083 -0.00481 0.00151 -0.00916 AFIX 137 H21A 2 1.217246 0.460223 0.811991 11.00000 -1.50000 H21B 2 1.112781 0.391363 0.817356 11.00000 -1.50000 H21C 2 1.050707 0.473942 0.813115 11.00000 -1.50000 AFIX 0 C212 1 1.112537 0.511840 0.689587 11.00000 0.02641 0.02342 = 0.03182 0.00692 0.00073 -0.00838 AFIX 137 H21D 2 1.034478 0.543520 0.700540 11.00000 -1.50000 H21E 2 1.108939 0.507561 0.639891 11.00000 -1.50000 H21F 2 1.203584 0.533746 0.708552 11.00000 -1.50000 AFIX 0 C213 1 0.599430 0.303535 0.827130 11.00000 0.02219 0.04592 = 0.02871 -0.01583 0.01442 -0.00714 AFIX 137 H21G 2 0.549820 0.259977 0.842090 11.00000 -1.50000 H21H 2 0.538937 0.328342 0.790035 11.00000 -1.50000 H21I 2 0.620554 0.337856 0.865543 11.00000 -1.50000 AFIX 0 C301 1 0.809542 0.058576 0.713512 11.00000 0.02175 0.02029 = 0.01787 0.00262 0.00507 0.00025 H30X 2 0.749918 0.053131 0.673823 11.00000 -1.20000 H30Y 2 0.771985 0.034323 0.748559 11.00000 -1.20000 C302 1 0.946017 0.085572 0.715144 11.00000 0.01824 0.01328 = 0.01631 -0.00282 0.00043 0.00670 C303 1 1.001366 0.124302 0.662635 11.00000 0.01058 0.01689 = 0.01552 -0.00283 0.00090 0.00193 H303 2 1.091216 0.138336 0.670362 11.00000 -1.20000 C304 1 0.950184 0.129808 0.590950 11.00000 0.01815 0.01052 = 0.01811 -0.00334 0.00301 0.00449 C305 1 0.825445 0.104798 0.557032 11.00000 0.01821 0.01766 = 0.01455 -0.00207 0.00098 0.00026 H305 2 0.762914 0.072808 0.574456 11.00000 -1.20000 C306 1 0.798918 0.109275 0.480065 11.00000 0.01448 0.02011 = 0.01658 -0.00370 -0.00233 0.00408 AFIX 23 H30A 2 0.710187 0.137284 0.466197 11.00000 -1.20000 H30B 2 0.786865 0.058708 0.460746 11.00000 -1.20000 AFIX 0 C307 1 0.922653 0.147465 0.452056 11.00000 0.02276 0.02014 = 0.01207 0.00073 0.00200 0.00530 AFIX 13 H307 2 0.911646 0.154126 0.401362 11.00000 -1.20000 AFIX 0 C308 1 0.959218 0.218162 0.494094 11.00000 0.02144 0.01599 = 0.01970 0.00475 0.00684 0.00367 AFIX 23 H30C 2 0.876817 0.241720 0.511786 11.00000 -1.20000 H30D 2 1.015867 0.254819 0.471691 11.00000 -1.20000 AFIX 0 C309 1 1.048630 0.166893 0.546159 11.00000 0.01843 0.01669 = 0.01677 -0.00376 0.00154 -0.00116 AFIX 13 H309 2 1.137159 0.189264 0.570686 11.00000 -1.20000 AFIX 0 C310 1 1.069950 0.114875 0.484510 11.00000 0.01763 0.01696 = 0.01675 -0.00457 0.00241 0.00322 C311 1 1.083230 0.031926 0.497746 11.00000 0.01774 0.02407 = 0.02338 -0.00147 0.00160 0.00395 AFIX 137 H31A 2 1.095775 0.006284 0.455125 11.00000 -1.50000 H31B 2 0.996837 0.013757 0.514854 11.00000 -1.50000 H31C 2 1.165630 0.022324 0.531783 11.00000 -1.50000 AFIX 0 C312 1 1.192835 0.139358 0.446512 11.00000 0.02479 0.02955 = 0.02404 -0.00304 0.00715 0.00289 AFIX 137 H31D 2 1.283314 0.125876 0.473263 11.00000 -1.50000 H31E 2 1.188941 0.193186 0.439940 11.00000 -1.50000 H31F 2 1.185137 0.114727 0.401941 11.00000 -1.50000 AFIX 0 C313 1 1.045359 0.079237 0.782047 11.00000 0.02163 0.02234 = 0.01951 0.00317 -0.00402 0.00409 AFIX 137 H31G 2 0.988947 0.077377 0.820405 11.00000 -1.50000 H31H 2 1.108674 0.122353 0.787167 11.00000 -1.50000 H31I 2 1.102194 0.033916 0.781494 11.00000 -1.50000 AFIX 0 PR2 3 0.110276 0.258434 0.074032 11.00000 0.01187 0.01559 = 0.01194 -0.00014 0.00181 -0.00152 C401 1 0.108159 0.301012 -0.059910 11.00000 0.02627 0.02345 = 0.01479 -0.00332 0.00201 -0.00526 H40X 2 0.056945 0.272791 -0.093087 11.00000 -1.20000 H40Y 2 0.078409 0.346238 -0.044449 11.00000 -1.20000 C402 1 0.247982 0.280678 -0.041896 11.00000 0.02307 0.02225 = 0.01395 0.00183 0.00825 -0.00577 C403 1 0.340069 0.306967 0.014953 11.00000 0.01390 0.01743 = 0.02076 0.00001 0.00674 -0.00210 H403 2 0.424093 0.285875 0.018210 11.00000 -1.20000 C404 1 0.326208 0.371307 0.056441 11.00000 0.01874 0.01260 = 0.01426 0.00194 0.00397 -0.00606 C405 1 0.212302 0.416778 0.058103 11.00000 0.01810 0.02232 = 0.01868 0.00010 0.00204 -0.00372 H405 2 0.128959 0.412614 0.026917 11.00000 -1.20000 C406 1 0.222773 0.485540 0.101002 11.00000 0.01637 0.01548 = 0.02538 0.00044 0.00489 -0.00060 AFIX 23 H40A 2 0.149870 0.483976 0.132820 11.00000 -1.20000 H40B 2 0.203657 0.529436 0.071174 11.00000 -1.20000 AFIX 0 C407 1 0.370215 0.492804 0.141827 11.00000 0.01923 0.01672 = 0.01832 0.00110 0.00201 -0.00014 AFIX 13 H407 2 0.384996 0.536911 0.172574 11.00000 -1.20000 AFIX 0 C408 1 0.407683 0.416431 0.175702 11.00000 0.01874 0.01976 = 0.01730 0.00132 -0.00092 -0.00237 AFIX 23 H40C 2 0.324657 0.388435 0.187965 11.00000 -1.20000 H40D 2 0.485387 0.418070 0.214163 11.00000 -1.20000 AFIX 0 C409 1 0.456178 0.393677 0.105952 11.00000 0.01228 0.01821 = 0.01959 0.00034 -0.00079 -0.00095 AFIX 13 H409 2 0.539785 0.359540 0.108377 11.00000 -1.20000 AFIX 0 C410 1 0.488046 0.478349 0.094697 11.00000 0.01737 0.01510 = 0.02182 0.00034 0.00249 -0.00022 C411 1 0.633437 0.501382 0.130599 11.00000 0.01335 0.02104 = 0.03701 -0.00045 0.00039 -0.00328 AFIX 137 H41A 2 0.640364 0.555572 0.131315 11.00000 -1.50000 H41B 2 0.708185 0.480838 0.105993 11.00000 -1.50000 H41C 2 0.645104 0.482524 0.177537 11.00000 -1.50000 AFIX 0 C412 1 0.468607 0.511055 0.023293 11.00000 0.02019 0.02120 = 0.02710 0.00608 0.00587 0.00136 AFIX 137 H41D 2 0.459540 0.565028 0.026210 11.00000 -1.50000 H41E 2 0.382489 0.490497 -0.002567 11.00000 -1.50000 H41F 2 0.551238 0.498761 0.000123 11.00000 -1.50000 AFIX 0 C413 1 0.305138 0.218441 -0.082474 11.00000 0.02845 0.03325 = 0.02443 -0.00438 0.01327 -0.00908 AFIX 137 H41G 2 0.227912 0.184004 -0.098072 11.00000 -1.50000 H41H 2 0.380162 0.191949 -0.053465 11.00000 -1.50000 H41I 2 0.344247 0.239183 -0.122085 11.00000 -1.50000 AFIX 0 C501 1 -0.179805 0.261583 0.026576 11.00000 0.01657 0.03247 = 0.01653 -0.00084 -0.00287 0.00464 H50X 2 -0.214029 0.253171 -0.019101 11.00000 -1.20000 H50Y 2 -0.190072 0.223656 0.057268 11.00000 -1.20000 C502 1 -0.150811 0.332593 0.044812 11.00000 0.00842 0.02689 = 0.01933 -0.00174 0.00206 0.00454 C503 1 -0.085173 0.358944 0.107908 11.00000 0.01472 0.01866 = 0.01541 0.00243 0.00402 0.00228 H503 2 -0.074729 0.408175 0.110157 11.00000 -1.20000 C504 1 -0.057606 0.321719 0.172761 11.00000 0.01487 0.02060 = 0.01216 0.00035 0.00449 -0.00030 C505 1 -0.079647 0.249274 0.188103 11.00000 0.01212 0.02361 = 0.01787 -0.00245 0.00444 -0.00248 H505 2 -0.135324 0.215800 0.159527 11.00000 -1.20000 C506 1 -0.049565 0.222506 0.261000 11.00000 0.01784 0.01979 = 0.01894 -0.00009 0.00511 0.00007 AFIX 23 H50A 2 0.017127 0.180096 0.263188 11.00000 -1.20000 H50B 2 -0.139102 0.205172 0.276762 11.00000 -1.20000 AFIX 0 C507 1 0.014121 0.283573 0.307537 11.00000 0.02234 0.01679 = 0.01030 0.00286 0.00082 -0.00231 AFIX 13 H507 2 0.041990 0.269013 0.356261 11.00000 -1.20000 AFIX 0 C508 1 0.131009 0.323467 0.272671 11.00000 0.01358 0.02356 = 0.01971 0.00301 -0.00029 -0.00384 AFIX 23 H50C 2 0.197528 0.353610 0.304078 11.00000 -1.20000 H50D 2 0.182622 0.290893 0.243736 11.00000 -1.20000 AFIX 0 C509 1 0.008382 0.368103 0.232954 11.00000 0.02106 0.01142 = 0.01210 -0.00024 0.00494 -0.00063 AFIX 13 H509 2 0.030295 0.420792 0.222522 11.00000 -1.20000 AFIX 0 C510 1 -0.075377 0.355486 0.296406 11.00000 0.02056 0.02088 = 0.01496 -0.00065 0.00454 0.00103 C511 1 -0.035801 0.411889 0.353516 11.00000 0.03907 0.02183 = 0.01863 -0.00196 0.00901 -0.00450 AFIX 137 H51A 2 -0.082605 0.459250 0.341051 11.00000 -1.50000 H51B 2 0.067535 0.418956 0.360085 11.00000 -1.50000 H51C 2 -0.066987 0.393586 0.395989 11.00000 -1.50000 AFIX 0 C512 1 -0.236477 0.348851 0.285189 11.00000 0.02508 0.02531 = 0.02409 0.00041 0.01046 0.00518 AFIX 137 H51D 2 -0.268810 0.320794 0.322893 11.00000 -1.50000 H51E 2 -0.265608 0.323027 0.242022 11.00000 -1.50000 H51F 2 -0.278892 0.398455 0.283419 11.00000 -1.50000 AFIX 0 C513 1 -0.182122 0.391492 -0.011442 11.00000 0.02711 0.03828 = 0.01811 -0.00103 -0.00120 0.01143 AFIX 137 H51G 2 -0.171159 0.369484 -0.055890 11.00000 -1.50000 H51H 2 -0.115450 0.432875 -0.002438 11.00000 -1.50000 H51I 2 -0.279697 0.409630 -0.011825 11.00000 -1.50000 AFIX 0 C601 1 0.073273 0.123782 0.004690 11.00000 0.02155 0.02385 = 0.01656 -0.00483 0.00340 -0.00821 H60X 2 0.006736 0.119244 -0.033455 11.00000 -1.20000 H60Y 2 0.166576 0.129508 -0.000984 11.00000 0.02571 C602 1 0.035474 0.107685 0.068341 11.00000 0.01564 0.01258 = 0.02189 -0.00198 0.00283 -0.00494 C603 1 0.117604 0.121991 0.131570 11.00000 0.01525 0.01540 = 0.01580 0.00079 0.00418 -0.00026 H603 2 0.074776 0.110750 0.167255 11.00000 -1.20000 C604 1 0.267965 0.139154 0.145953 11.00000 0.01759 0.01137 = 0.01728 0.00081 0.00159 0.00214 C605 1 0.366022 0.144414 0.102012 11.00000 0.01926 0.02101 = 0.02221 0.00005 0.00129 -0.00123 H605 2 0.345528 0.127532 0.057134 11.00000 0.01128 C606 1 0.522791 0.153201 0.129761 11.00000 0.01514 0.03029 = 0.03065 0.00247 0.00682 -0.00050 AFIX 23 H60A 2 0.576275 0.109038 0.117570 11.00000 -1.20000 H60B 2 0.562271 0.197114 0.108650 11.00000 -1.20000 AFIX 0 C607 1 0.540625 0.162322 0.206909 11.00000 0.01014 0.02292 = 0.03658 -0.00156 -0.00104 -0.00024 AFIX 13 H607 2 0.640203 0.171332 0.228632 11.00000 -1.20000 AFIX 0 C608 1 0.430238 0.219316 0.224208 11.00000 0.01897 0.02127 = 0.03252 -0.00111 -0.00024 -0.00466 AFIX 23 H60C 2 0.406282 0.257585 0.188686 11.00000 -1.20000 H60D 2 0.451164 0.241689 0.270170 11.00000 -1.20000 AFIX 0 C609 1 0.324587 0.153029 0.220380 11.00000 0.01161 0.01854 = 0.02157 -0.00075 0.00280 0.00042 AFIX 13 H609 2 0.251534 0.154968 0.252806 11.00000 -1.20000 AFIX 0 C610 1 0.456315 0.102459 0.242430 11.00000 0.01285 0.02095 = 0.02749 0.00269 -0.00324 0.00450 C611 1 0.493681 0.101394 0.320280 11.00000 0.02678 0.03894 = 0.02706 0.00081 -0.00436 0.00786 AFIX 137 H61A 2 0.418842 0.075404 0.340911 11.00000 -1.50000 H61B 2 0.501574 0.152368 0.337475 11.00000 -1.50000 H61C 2 0.584512 0.075730 0.332219 11.00000 -1.50000 AFIX 0 C612 1 0.451617 0.023150 0.216287 11.00000 0.02292 0.02562 = 0.03631 0.00983 0.00075 0.00432 AFIX 137 H61D 2 0.544155 -0.000473 0.229264 11.00000 -1.50000 H61E 2 0.429765 0.023210 0.166422 11.00000 -1.50000 H61F 2 0.377901 -0.004421 0.236320 11.00000 -1.50000 AFIX 0 C613 1 -0.113004 0.078770 0.071488 11.00000 0.01922 0.02668 = 0.02142 0.00022 0.00035 -0.00784 AFIX 137 H61G 2 -0.112773 0.024562 0.068440 11.00000 -1.50000 H61H 2 -0.177403 0.099152 0.033329 11.00000 -1.50000 H61I 2 -0.145254 0.093819 0.114741 11.00000 -1.50000 AFIX 0 HKLF 4 REM ann67 in P2(1) REM R1 = 0.0392 for 16814 Fo > 4sig(Fo) and 0.0578 for all 19885 data REM 813 parameters refined using 97 restraints END WGHT 0.0239 0.0000 REM Highest difference peak 0.999, deepest hole -0.767, 1-sigma level 0.129 Q1 1 0.1084 0.1536 0.0709 11.00000 0.05 1.00 Q2 1 0.4554 0.2053 0.4702 11.00000 0.05 0.97 Q3 1 0.0164 0.2061 0.1723 11.00000 0.05 0.96 Q4 1 0.7623 0.3102 0.6801 11.00000 0.05 0.92 Q5 1 0.4279 0.2565 0.2820 11.00000 0.05 0.83 Q6 1 0.0758 0.3209 0.0692 11.00000 0.05 0.82 Q7 1 0.7417 0.2602 0.6950 11.00000 0.05 0.74 Q8 1 0.0781 0.2031 0.0921 11.00000 0.05 0.74 Q9 1 0.0751 0.2001 0.0613 11.00000 0.05 0.74 Q10 1 0.1590 0.1980 0.0793 11.00000 0.05 0.66 ; _shelx_res_checksum 89578 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Pr1 Pr 0.76469(3) 0.20569(2) 0.67805(2) 0.01260(6) Uani 1 1 d . . C101 C 0.4928(6) 0.1718(3) 0.7094(3) 0.0202(12) Uani 1 1 d D . H10X H 0.483(6) 0.2215(14) 0.715(3) 0.024 Uiso 1 1 d D U H10Y H 0.470(5) 0.139(2) 0.742(2) 0.024 Uiso 1 1 d D U C102 C 0.4892(5) 0.1475(3) 0.6427(3) 0.0187(12) Uani 1 1 d . . C103 C 0.5274(5) 0.1890(3) 0.5867(3) 0.0156(11) Uani 1 1 d D . H103 H 0.531(5) 0.162(3) 0.5495(19) 0.019 Uiso 1 1 d D U C104 C 0.5446(5) 0.2677(3) 0.5793(2) 0.0161(10) Uani 1 1 d . . C105 C 0.5398(5) 0.3233(3) 0.6258(3) 0.0173(11) Uani 1 1 d D . H105 H 0.519(5) 0.315(3) 0.6701(17) 0.021 Uiso 1 1 d D U C106 C 0.5462(5) 0.4033(3) 0.6048(2) 0.0173(10) Uani 1 1 d . . H10A H 0.625915 0.428109 0.633194 0.021 Uiso 1 1 calc R U H10B H 0.456899 0.428462 0.612778 0.021 Uiso 1 1 calc R U C107 C 0.5666(5) 0.4099(3) 0.5303(2) 0.0167(10) Uani 1 1 d . . H107 H 0.574955 0.461648 0.513001 0.020 Uiso 1 1 calc R U C108 C 0.6866(5) 0.3566(3) 0.5164(3) 0.0194(11) Uani 1 1 d . . H10C H 0.761369 0.349756 0.555617 0.023 Uiso 1 1 calc R U H10D H 0.728277 0.367227 0.473822 0.023 Uiso 1 1 calc R U C109 C 0.5705(5) 0.2952(3) 0.5091(3) 0.0172(11) Uani 1 1 d . . H109 H 0.582040 0.255777 0.474603 0.021 Uiso 1 1 calc R U C110 C 0.4615(5) 0.3586(3) 0.4849(3) 0.0181(11) Uani 1 1 d . . C111 C 0.3096(5) 0.3535(3) 0.5011(3) 0.0231(12) Uani 1 1 d . . H11A H 0.264662 0.402387 0.495661 0.035 Uiso 1 1 calc R U H11B H 0.309312 0.336422 0.548189 0.035 Uiso 1 1 calc R U H11C H 0.256590 0.318280 0.469734 0.035 Uiso 1 1 calc R U C112 C 0.4590(6) 0.3743(3) 0.4086(3) 0.0244(12) Uani 1 1 d . . H11D H 0.402536 0.418993 0.396511 0.037 Uiso 1 1 calc R U H11E H 0.416465 0.332155 0.382254 0.037 Uiso 1 1 calc R U H11F H 0.556386 0.381967 0.398176 0.037 Uiso 1 1 calc R U C113 C 0.4551(6) 0.0669(3) 0.6289(3) 0.0274(14) Uani 1 1 d . . H11G H 0.487064 0.037618 0.669767 0.041 Uiso 1 1 calc R U H11H H 0.503794 0.049689 0.590815 0.041 Uiso 1 1 calc R U H11I H 0.352146 0.060950 0.617111 0.041 Uiso 1 1 calc R U C201 C 0.7895(5) 0.2107(4) 0.8201(2) 0.0214(11) Uani 1 1 d D . H20X H 0.745(5) 0.182(3) 0.850(2) 0.026 Uiso 1 1 d D U H20Y H 0.880(3) 0.194(3) 0.819(3) 0.026 Uiso 1 1 d D U C202 C 0.7387(5) 0.2792(3) 0.8017(3) 0.0210(12) Uani 1 1 d . . C203 C 0.7908(5) 0.3286(3) 0.7554(3) 0.0163(11) Uani 1 1 d D . H203 H 0.740(5) 0.369(2) 0.746(3) 0.020 Uiso 1 1 d D U C204 C 0.9275(5) 0.3307(3) 0.7310(3) 0.0144(11) Uani 1 1 d . . C205 C 1.0374(5) 0.2819(3) 0.7435(3) 0.0172(11) Uani 1 1 d D . H205 H 1.035(5) 0.242(2) 0.774(2) 0.021 Uiso 1 1 d D U C206 C 1.1817(5) 0.3004(3) 0.7228(3) 0.0201(12) Uani 1 1 d . . H20A H 1.212438 0.260014 0.693950 0.024 Uiso 1 1 calc R U H20B H 1.252230 0.304483 0.764045 0.024 Uiso 1 1 calc R U C207 C 1.1755(5) 0.3732(3) 0.6833(3) 0.0177(11) Uani 1 1 d . . H207 H 1.266185 0.388546 0.666256 0.021 Uiso 1 1 calc R U C208 C 1.0438(5) 0.3701(3) 0.6288(3) 0.0208(11) Uani 1 1 d . . H20C H 1.019370 0.319706 0.611131 0.025 Uiso 1 1 calc R U H20D H 1.045450 0.406209 0.591128 0.025 Uiso 1 1 calc R U C209 C 0.9579(5) 0.3958(3) 0.6865(3) 0.0146(10) Uani 1 1 d . . H209 H 0.875496 0.429276 0.672095 0.018 Uiso 1 1 calc R U C210 C 1.0979(5) 0.4352(3) 0.7203(3) 0.0179(11) Uani 1 1 d . . C211 C 1.1218(6) 0.4407(3) 0.7975(3) 0.0216(12) Uani 1 1 d . . H21A H 1.217246 0.460223 0.811991 0.032 Uiso 1 1 calc R U H21B H 1.112781 0.391363 0.817356 0.032 Uiso 1 1 calc R U H21C H 1.050707 0.473942 0.813115 0.032 Uiso 1 1 calc R U C212 C 1.1125(6) 0.5118(3) 0.6896(3) 0.0275(13) Uani 1 1 d . . H21D H 1.034478 0.543520 0.700540 0.041 Uiso 1 1 calc R U H21E H 1.108939 0.507561 0.639891 0.041 Uiso 1 1 calc R U H21F H 1.203584 0.533746 0.708552 0.041 Uiso 1 1 calc R U C213 C 0.5994(6) 0.3035(4) 0.8271(3) 0.0313(14) Uani 1 1 d . . H21G H 0.549820 0.259977 0.842090 0.047 Uiso 1 1 calc R U H21H H 0.538937 0.328342 0.790035 0.047 Uiso 1 1 calc R U H21I H 0.620554 0.337856 0.865543 0.047 Uiso 1 1 calc R U C301 C 0.8095(6) 0.0586(3) 0.7135(3) 0.0198(11) Uani 1 1 d D . H30X H 0.750(5) 0.053(3) 0.6738(17) 0.024 Uiso 1 1 d D U H30Y H 0.772(5) 0.034(3) 0.749(2) 0.024 Uiso 1 1 d D U C302 C 0.9460(5) 0.0856(3) 0.7151(3) 0.0161(11) Uani 1 1 d . . C303 C 1.0014(5) 0.1243(3) 0.6626(3) 0.0144(10) Uani 1 1 d D . H303 H 1.091(3) 0.138(3) 0.670(3) 0.017 Uiso 1 1 d D U C304 C 0.9502(5) 0.1298(3) 0.5909(3) 0.0155(10) Uani 1 1 d . . C305 C 0.8254(5) 0.1048(3) 0.5570(3) 0.0169(10) Uani 1 1 d D . H305 H 0.763(5) 0.073(2) 0.574(3) 0.020 Uiso 1 1 d D U C306 C 0.7989(5) 0.1093(3) 0.4801(2) 0.0174(11) Uani 1 1 d . . H30A H 0.710187 0.137284 0.466197 0.021 Uiso 1 1 calc R U H30B H 0.786865 0.058708 0.460746 0.021 Uiso 1 1 calc R U C307 C 0.9227(5) 0.1475(3) 0.4521(2) 0.0183(11) Uani 1 1 d . . H307 H 0.911646 0.154126 0.401362 0.022 Uiso 1 1 calc R U C308 C 0.9592(5) 0.2182(3) 0.4941(2) 0.0187(11) Uani 1 1 d . . H30C H 0.876817 0.241720 0.511786 0.022 Uiso 1 1 calc R U H30D H 1.015867 0.254819 0.471691 0.022 Uiso 1 1 calc R U C309 C 1.0486(5) 0.1669(3) 0.5462(2) 0.0174(11) Uani 1 1 d . . H309 H 1.137159 0.189264 0.570686 0.021 Uiso 1 1 calc R U C310 C 1.0699(5) 0.1149(3) 0.4845(3) 0.0171(11) Uani 1 1 d . . C311 C 1.0832(5) 0.0319(3) 0.4977(3) 0.0218(12) Uani 1 1 d . . H31A H 1.095775 0.006284 0.455125 0.033 Uiso 1 1 calc R U H31B H 0.996837 0.013757 0.514854 0.033 Uiso 1 1 calc R U H31C H 1.165630 0.022324 0.531783 0.033 Uiso 1 1 calc R U C312 C 1.1928(6) 0.1394(3) 0.4465(3) 0.0258(13) Uani 1 1 d . . H31D H 1.283314 0.125876 0.473263 0.039 Uiso 1 1 calc R U H31E H 1.188941 0.193186 0.439940 0.039 Uiso 1 1 calc R U H31F H 1.185137 0.114727 0.401941 0.039 Uiso 1 1 calc R U C313 C 1.0454(6) 0.0792(3) 0.7820(3) 0.0217(12) Uani 1 1 d . . H31G H 0.988947 0.077377 0.820405 0.033 Uiso 1 1 calc R U H31H H 1.108674 0.122353 0.787167 0.033 Uiso 1 1 calc R U H31I H 1.102194 0.033916 0.781494 0.033 Uiso 1 1 calc R U Pr2 Pr 0.11028(3) 0.25843(2) 0.07403(2) 0.01311(6) Uani 1 1 d . . C401 C 0.1082(6) 0.3010(3) -0.0599(3) 0.0215(12) Uani 1 1 d D . H40X H 0.057(5) 0.273(3) -0.093(2) 0.026 Uiso 1 1 d D U H40Y H 0.078(6) 0.3462(19) -0.044(3) 0.026 Uiso 1 1 d D U C402 C 0.2480(5) 0.2807(3) -0.0419(2) 0.0193(11) Uani 1 1 d . . C403 C 0.3401(5) 0.3070(3) 0.0150(3) 0.0170(10) Uani 1 1 d D . H403 H 0.424(4) 0.286(3) 0.018(3) 0.020 Uiso 1 1 d D U C404 C 0.3262(5) 0.3713(3) 0.0564(2) 0.0150(10) Uani 1 1 d . . C405 C 0.2123(5) 0.4168(3) 0.0581(3) 0.0197(11) Uani 1 1 d D . H405 H 0.129(4) 0.413(3) 0.027(2) 0.024 Uiso 1 1 d D U C406 C 0.2228(5) 0.4855(3) 0.1010(3) 0.0189(11) Uani 1 1 d . . H40A H 0.149870 0.483976 0.132820 0.023 Uiso 1 1 calc R U H40B H 0.203657 0.529436 0.071174 0.023 Uiso 1 1 calc R U C407 C 0.3702(5) 0.4928(3) 0.1418(3) 0.0181(11) Uani 1 1 d . . H407 H 0.384996 0.536911 0.172574 0.022 Uiso 1 1 calc R U C408 C 0.4077(5) 0.4164(3) 0.1757(3) 0.0189(11) Uani 1 1 d . . H40C H 0.324657 0.388435 0.187965 0.023 Uiso 1 1 calc R U H40D H 0.485387 0.418070 0.214163 0.023 Uiso 1 1 calc R U C409 C 0.4562(5) 0.3937(3) 0.1060(3) 0.0169(11) Uani 1 1 d . . H409 H 0.539785 0.359540 0.108377 0.020 Uiso 1 1 calc R U C410 C 0.4880(5) 0.4783(3) 0.0947(3) 0.0181(11) Uani 1 1 d . . C411 C 0.6334(5) 0.5014(3) 0.1306(3) 0.0240(12) Uani 1 1 d . . H41A H 0.640364 0.555572 0.131315 0.036 Uiso 1 1 calc R U H41B H 0.708185 0.480838 0.105993 0.036 Uiso 1 1 calc R U H41C H 0.645104 0.482524 0.177537 0.036 Uiso 1 1 calc R U C412 C 0.4686(6) 0.5111(3) 0.0233(3) 0.0226(12) Uani 1 1 d . . H41D H 0.459540 0.565028 0.026210 0.034 Uiso 1 1 calc R U H41E H 0.382489 0.490497 -0.002567 0.034 Uiso 1 1 calc R U H41F H 0.551238 0.498761 0.000123 0.034 Uiso 1 1 calc R U C413 C 0.3051(6) 0.2184(3) -0.0825(3) 0.0279(14) Uani 1 1 d . . H41G H 0.227912 0.184004 -0.098072 0.042 Uiso 1 1 calc R U H41H H 0.380162 0.191949 -0.053465 0.042 Uiso 1 1 calc R U H41I H 0.344247 0.239183 -0.122085 0.042 Uiso 1 1 calc R U C501 C -0.1798(5) 0.2616(4) 0.0266(3) 0.0223(11) Uani 1 1 d D . H50X H -0.214(5) 0.253(3) -0.0191(14) 0.027 Uiso 1 1 d D U H50Y H -0.190(5) 0.224(2) 0.057(2) 0.027 Uiso 1 1 d D U C502 C -0.1508(5) 0.3326(3) 0.0448(3) 0.0182(12) Uani 1 1 d . . C503 C -0.0852(5) 0.3589(3) 0.1079(3) 0.0161(10) Uani 1 1 d D . H503 H -0.075(5) 0.4082(16) 0.110(3) 0.019 Uiso 1 1 d D U C504 C -0.0576(5) 0.3217(3) 0.1728(2) 0.0156(10) Uani 1 1 d . . C505 C -0.0796(5) 0.2493(3) 0.1881(2) 0.0176(11) Uani 1 1 d D . H505 H -0.135(5) 0.216(2) 0.160(2) 0.021 Uiso 1 1 d D U C506 C -0.0496(5) 0.2225(3) 0.2610(2) 0.0186(11) Uani 1 1 d . . H50A H 0.017127 0.180096 0.263188 0.022 Uiso 1 1 calc R U H50B H -0.139102 0.205172 0.276762 0.022 Uiso 1 1 calc R U C507 C 0.0141(5) 0.2836(3) 0.3075(2) 0.0166(10) Uani 1 1 d . . H507 H 0.041990 0.269013 0.356261 0.020 Uiso 1 1 calc R U C508 C 0.1310(5) 0.3235(3) 0.2727(3) 0.0191(11) Uani 1 1 d . . H50C H 0.197528 0.353610 0.304078 0.023 Uiso 1 1 calc R U H50D H 0.182622 0.290893 0.243736 0.023 Uiso 1 1 calc R U C509 C 0.0084(5) 0.3681(3) 0.2330(2) 0.0146(10) Uani 1 1 d . . H509 H 0.030295 0.420792 0.222522 0.018 Uiso 1 1 calc R U C510 C -0.0754(5) 0.3555(3) 0.2964(3) 0.0186(11) Uani 1 1 d . . C511 C -0.0358(6) 0.4119(3) 0.3535(3) 0.0261(13) Uani 1 1 d . . H51A H -0.082605 0.459250 0.341051 0.039 Uiso 1 1 calc R U H51B H 0.067535 0.418956 0.360085 0.039 Uiso 1 1 calc R U H51C H -0.066987 0.393586 0.395989 0.039 Uiso 1 1 calc R U C512 C -0.2365(6) 0.3489(3) 0.2852(3) 0.0242(12) Uani 1 1 d . . H51D H -0.268810 0.320794 0.322893 0.036 Uiso 1 1 calc R U H51E H -0.265608 0.323027 0.242022 0.036 Uiso 1 1 calc R U H51F H -0.278892 0.398455 0.283419 0.036 Uiso 1 1 calc R U C513 C -0.1821(6) 0.3915(3) -0.0114(3) 0.0282(14) Uani 1 1 d . . H51G H -0.171159 0.369484 -0.055890 0.042 Uiso 1 1 calc R U H51H H -0.115450 0.432875 -0.002438 0.042 Uiso 1 1 calc R U H51I H -0.279697 0.409630 -0.011825 0.042 Uiso 1 1 calc R U C601 C 0.0733(6) 0.1238(3) 0.0047(3) 0.0206(12) Uani 1 1 d D . H60X H 0.007(4) 0.119(3) -0.0335(19) 0.025 Uiso 1 1 d D U H60Y H 0.167(3) 0.130(3) -0.001(3) 0.026(16) Uiso 1 1 d D . C602 C 0.0355(5) 0.1077(3) 0.0683(3) 0.0167(11) Uani 1 1 d . . C603 C 0.1176(5) 0.1220(3) 0.1316(3) 0.0153(10) Uani 1 1 d D . H603 H 0.075(5) 0.111(3) 0.167(2) 0.018 Uiso 1 1 d D U C604 C 0.2680(5) 0.1392(3) 0.1460(3) 0.0155(10) Uani 1 1 d . . C605 C 0.3660(6) 0.1444(3) 0.1020(3) 0.0209(12) Uani 1 1 d D . H605 H 0.346(5) 0.128(3) 0.0571(16) 0.011(13) Uiso 1 1 d D . C606 C 0.5228(5) 0.1532(3) 0.1298(3) 0.0250(13) Uani 1 1 d . . H60A H 0.576275 0.109038 0.117570 0.030 Uiso 1 1 calc R U H60B H 0.562271 0.197114 0.108650 0.030 Uiso 1 1 calc R U C607 C 0.5406(5) 0.1623(3) 0.2069(3) 0.0235(12) Uani 1 1 d . . H607 H 0.640203 0.171332 0.228632 0.028 Uiso 1 1 calc R U C608 C 0.4302(5) 0.2193(3) 0.2242(3) 0.0245(13) Uani 1 1 d . . H60C H 0.406282 0.257585 0.188686 0.029 Uiso 1 1 calc R U H60D H 0.451164 0.241689 0.270170 0.029 Uiso 1 1 calc R U C609 C 0.3246(5) 0.1530(3) 0.2204(3) 0.0172(11) Uani 1 1 d . . H609 H 0.251534 0.154968 0.252806 0.021 Uiso 1 1 calc R U C610 C 0.4563(5) 0.1025(3) 0.2424(3) 0.0209(11) Uani 1 1 d . . C611 C 0.4937(6) 0.1014(4) 0.3203(3) 0.0316(14) Uani 1 1 d . . H61A H 0.418842 0.075404 0.340911 0.047 Uiso 1 1 calc R U H61B H 0.501574 0.152368 0.337475 0.047 Uiso 1 1 calc R U H61C H 0.584512 0.075730 0.332219 0.047 Uiso 1 1 calc R U C612 C 0.4516(6) 0.0232(3) 0.2163(3) 0.0285(13) Uani 1 1 d . . H61D H 0.544155 -0.000473 0.229264 0.043 Uiso 1 1 calc R U H61E H 0.429765 0.023210 0.166422 0.043 Uiso 1 1 calc R U H61F H 0.377901 -0.004421 0.236320 0.043 Uiso 1 1 calc R U C613 C -0.1130(5) 0.0788(3) 0.0715(3) 0.0226(12) Uani 1 1 d . . H61G H -0.112773 0.024562 0.068440 0.034 Uiso 1 1 calc R U H61H H -0.177403 0.099152 0.033329 0.034 Uiso 1 1 calc R U H61I H -0.145254 0.093819 0.114741 0.034 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 0.01200(12) 0.01253(13) 0.01297(12) -0.00050(12) 0.00031(9) -0.00044(11) C101 0.015(3) 0.015(3) 0.030(3) 0.007(2) 0.002(2) -0.001(2) C102 0.010(2) 0.017(3) 0.026(3) 0.001(2) -0.009(2) -0.001(2) C103 0.012(2) 0.018(3) 0.016(2) -0.002(2) -0.0036(19) 0.0016(19) C104 0.009(2) 0.021(3) 0.017(2) -0.001(2) -0.0031(17) 0.000(2) C105 0.019(3) 0.016(3) 0.017(3) -0.002(2) 0.003(2) 0.003(2) C106 0.016(2) 0.015(3) 0.021(3) -0.003(2) 0.000(2) 0.001(2) C107 0.017(3) 0.016(3) 0.017(3) 0.002(2) 0.002(2) 0.003(2) C108 0.014(3) 0.021(3) 0.022(3) -0.002(2) 0.001(2) -0.001(2) C109 0.017(3) 0.017(3) 0.016(3) -0.001(2) -0.003(2) 0.003(2) C110 0.016(3) 0.019(3) 0.019(3) 0.001(2) 0.002(2) 0.002(2) C111 0.015(3) 0.023(3) 0.029(3) -0.002(2) -0.005(2) -0.002(2) C112 0.027(3) 0.024(3) 0.021(3) 0.002(2) -0.003(2) 0.005(2) C113 0.023(3) 0.020(3) 0.037(4) 0.006(3) -0.005(3) -0.005(2) C201 0.022(3) 0.028(3) 0.014(2) -0.001(3) 0.004(2) -0.008(3) C202 0.013(2) 0.035(4) 0.015(2) -0.007(2) 0.0037(19) -0.011(2) C203 0.016(3) 0.016(3) 0.016(3) -0.006(2) 0.001(2) 0.001(2) C204 0.014(2) 0.013(3) 0.015(2) -0.004(2) -0.0004(19) -0.0008(19) C205 0.020(3) 0.015(3) 0.017(3) 0.001(2) 0.004(2) 0.001(2) C206 0.016(3) 0.020(3) 0.024(3) 0.000(2) 0.002(2) 0.002(2) C207 0.015(2) 0.021(3) 0.018(3) 0.002(2) 0.004(2) -0.004(2) C208 0.023(3) 0.023(3) 0.017(3) -0.001(2) 0.002(2) 0.000(2) C209 0.013(2) 0.012(2) 0.018(3) -0.002(2) 0.001(2) -0.0013(19) C210 0.018(3) 0.016(3) 0.020(3) 0.001(2) 0.002(2) -0.007(2) C211 0.023(3) 0.020(3) 0.021(3) -0.005(2) 0.002(2) -0.009(2) C212 0.026(3) 0.023(3) 0.032(3) 0.007(3) 0.001(2) -0.008(2) C213 0.022(3) 0.046(4) 0.029(3) -0.016(3) 0.014(2) -0.007(3) C301 0.022(3) 0.020(3) 0.018(3) 0.003(2) 0.005(2) 0.000(2) C302 0.018(3) 0.013(3) 0.016(3) -0.003(2) 0.000(2) 0.007(2) C303 0.011(2) 0.017(3) 0.016(3) -0.003(2) 0.001(2) 0.002(2) C304 0.018(3) 0.011(2) 0.018(3) -0.003(2) 0.003(2) 0.004(2) C305 0.018(3) 0.018(3) 0.015(3) -0.002(2) 0.001(2) 0.000(2) C306 0.014(2) 0.020(3) 0.017(3) -0.004(2) -0.002(2) 0.004(2) C307 0.023(3) 0.020(3) 0.012(2) 0.001(2) 0.002(2) 0.005(2) C308 0.021(3) 0.016(3) 0.020(2) 0.005(2) 0.007(2) 0.004(2) C309 0.018(3) 0.017(3) 0.017(3) -0.004(2) 0.002(2) -0.001(2) C310 0.018(3) 0.017(3) 0.017(3) -0.005(2) 0.002(2) 0.003(2) C311 0.018(3) 0.024(3) 0.023(3) -0.001(2) 0.002(2) 0.004(2) C312 0.025(3) 0.030(3) 0.024(3) -0.003(3) 0.007(2) 0.003(3) C313 0.022(3) 0.022(3) 0.020(3) 0.003(2) -0.004(2) 0.004(2) Pr2 0.01187(12) 0.01559(13) 0.01194(12) -0.00014(12) 0.00181(9) -0.00152(12) C401 0.026(3) 0.023(3) 0.015(3) -0.003(2) 0.002(2) -0.005(2) C402 0.023(3) 0.022(3) 0.014(2) 0.002(2) 0.008(2) -0.006(2) C403 0.014(2) 0.017(3) 0.021(3) 0.000(2) 0.007(2) -0.002(2) C404 0.019(3) 0.013(3) 0.014(2) 0.002(2) 0.0040(19) -0.006(2) C405 0.018(3) 0.022(3) 0.019(3) 0.000(2) 0.002(2) -0.004(2) C406 0.016(3) 0.015(3) 0.025(3) 0.000(2) 0.005(2) -0.001(2) C407 0.019(3) 0.017(3) 0.018(3) 0.001(2) 0.002(2) 0.000(2) C408 0.019(3) 0.020(3) 0.017(3) 0.001(2) -0.001(2) -0.002(2) C409 0.012(2) 0.018(3) 0.020(3) 0.000(2) -0.001(2) -0.001(2) C410 0.017(3) 0.015(3) 0.022(3) 0.000(2) 0.002(2) 0.000(2) C411 0.013(3) 0.021(3) 0.037(3) 0.000(2) 0.000(2) -0.003(2) C412 0.020(3) 0.021(3) 0.027(3) 0.006(2) 0.006(2) 0.001(2) C413 0.028(3) 0.033(4) 0.024(3) -0.004(3) 0.013(2) -0.009(3) C501 0.017(2) 0.032(3) 0.017(2) -0.001(3) -0.0029(19) 0.005(3) C502 0.008(3) 0.027(3) 0.019(3) -0.002(2) 0.002(2) 0.005(2) C503 0.015(2) 0.019(3) 0.015(3) 0.002(2) 0.004(2) 0.002(2) C504 0.015(2) 0.021(3) 0.012(2) 0.000(2) 0.0045(19) 0.000(2) C505 0.012(2) 0.024(3) 0.018(2) -0.002(2) 0.0044(18) -0.002(2) C506 0.018(2) 0.020(3) 0.019(2) 0.000(2) 0.005(2) 0.000(2) C507 0.022(3) 0.017(3) 0.010(2) 0.0029(19) 0.0008(19) -0.002(2) C508 0.014(2) 0.024(3) 0.020(3) 0.003(2) 0.000(2) -0.004(2) C509 0.021(3) 0.011(2) 0.012(2) 0.000(2) 0.005(2) -0.001(2) C510 0.021(3) 0.021(3) 0.015(2) -0.001(2) 0.005(2) 0.001(2) C511 0.039(3) 0.022(3) 0.019(3) -0.002(2) 0.009(2) -0.005(3) C512 0.025(3) 0.025(3) 0.024(3) 0.000(2) 0.010(2) 0.005(2) C513 0.027(3) 0.038(4) 0.018(3) -0.001(3) -0.001(2) 0.011(3) C601 0.022(3) 0.024(3) 0.017(3) -0.005(2) 0.003(2) -0.008(2) C602 0.016(2) 0.013(3) 0.022(3) -0.002(2) 0.003(2) -0.005(2) C603 0.015(3) 0.015(3) 0.016(3) 0.001(2) 0.004(2) 0.000(2) C604 0.018(3) 0.011(3) 0.017(3) 0.001(2) 0.002(2) 0.002(2) C605 0.019(3) 0.021(3) 0.022(3) 0.000(2) 0.001(2) -0.001(2) C606 0.015(3) 0.030(3) 0.031(3) 0.002(3) 0.007(2) -0.001(2) C607 0.010(2) 0.023(3) 0.037(3) -0.002(2) -0.001(2) 0.000(2) C608 0.019(3) 0.021(3) 0.033(3) -0.001(2) 0.000(2) -0.005(2) C609 0.012(2) 0.019(3) 0.022(3) -0.001(2) 0.003(2) 0.000(2) C610 0.013(3) 0.021(3) 0.027(3) 0.003(2) -0.003(2) 0.004(2) C611 0.027(3) 0.039(4) 0.027(3) 0.001(3) -0.004(2) 0.008(3) C612 0.023(3) 0.026(3) 0.036(3) 0.010(3) 0.001(3) 0.004(2) C613 0.019(3) 0.027(3) 0.021(3) 0.000(2) 0.000(2) -0.008(2) 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' 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 C203 Pr1 C103 118.61(15) C203 Pr1 C303 119.25(15) C103 Pr1 C303 119.32(15) C203 Pr1 C301 130.43(17) C103 Pr1 C301 98.61(16) C303 Pr1 C301 53.77(16) C203 Pr1 C201 53.91(18) C103 Pr1 C201 129.10(15) C303 Pr1 C201 99.32(16) C301 Pr1 C201 77.61(18) C203 Pr1 C101 94.43(16) C103 Pr1 C101 54.04(16) C303 Pr1 C101 134.48(16) C301 Pr1 C101 81.40(16) C201 Pr1 C101 75.45(16) C203 Pr1 C302 118.64(15) C103 Pr1 C302 121.09(15) C303 Pr1 C302 29.35(15) C301 Pr1 C302 28.64(15) C201 Pr1 C302 77.89(17) C101 Pr1 C302 108.97(16) C203 Pr1 C202 29.57(16) C103 Pr1 C202 118.23(15) C303 Pr1 C202 120.79(15) C301 Pr1 C202 105.09(16) C201 Pr1 C202 28.09(17) C101 Pr1 C202 74.23(16) C302 Pr1 C202 104.76(15) C203 Pr1 C102 117.72(16) C103 Pr1 C102 29.63(15) C303 Pr1 C102 121.35(16) C301 Pr1 C102 79.24(16) C201 Pr1 C102 102.76(16) C101 Pr1 C102 28.55(16) C302 Pr1 C102 107.14(15) C202 Pr1 C102 102.22(15) C203 Pr1 C204 29.86(15) C103 Pr1 C204 134.01(15) C303 Pr1 C204 92.96(15) C301 Pr1 C204 127.35(15) C201 Pr1 C204 68.41(16) C101 Pr1 C204 124.29(16) C302 Pr1 C204 103.25(13) C202 Pr1 C204 54.02(14) C102 Pr1 C204 145.68(15) C203 Pr1 C104 94.06(15) C103 Pr1 C104 29.51(15) C303 Pr1 C104 131.76(14) C301 Pr1 C104 128.07(16) C201 Pr1 C104 128.91(15) C101 Pr1 C104 68.08(15) C302 Pr1 C104 147.19(14) C202 Pr1 C104 105.52(15) C102 Pr1 C104 53.89(15) C204 Pr1 C104 104.58(15) C203 Pr1 C304 134.11(15) C103 Pr1 C304 93.77(14) C303 Pr1 C304 29.10(14) C301 Pr1 C304 67.49(15) C201 Pr1 C304 128.37(16) C101 Pr1 C304 131.46(16) C302 Pr1 C304 53.30(14) C202 Pr1 C304 148.00(14) C102 Pr1 C304 106.50(15) C204 Pr1 C304 104.25(14) C104 Pr1 C304 102.67(14) C102 C101 Pr1 76.9(3) C101 C102 C103 126.5(5) C101 C102 C113 117.2(5) C103 C102 C113 115.9(5) C101 C102 Pr1 74.6(3) C103 C102 Pr1 71.2(3) C113 C102 Pr1 125.1(3) C102 C103 C104 130.0(5) C102 C103 Pr1 79.1(3) C104 C103 Pr1 82.1(3) C105 C104 C103 130.1(5) C105 C104 C109 113.4(5) C103 C104 C109 116.5(4) C105 C104 Pr1 85.0(3) C103 C104 Pr1 68.4(3) C109 C104 Pr1 123.7(3) C104 C105 C106 120.9(5) C105 C106 C107 111.0(4) C106 C107 C108 108.1(4) C106 C107 C110 111.2(4) C108 C107 C110 87.7(4) C107 C108 C109 86.1(4) C104 C109 C108 109.9(4) C104 C109 C110 109.8(4) C108 C109 C110 86.5(4) C111 C110 C112 108.6(4) C111 C110 C107 118.2(4) C112 C110 C107 112.7(4) C111 C110 C109 119.7(4) C112 C110 C109 111.2(4) C107 C110 C109 84.8(4) C202 C201 Pr1 77.2(3) C201 C202 C203 127.4(5) C201 C202 C213 117.6(5) C203 C202 C213 114.6(5) C201 C202 Pr1 74.7(3) C203 C202 Pr1 70.2(3) C213 C202 Pr1 126.2(3) C202 C203 C204 129.6(5) C202 C203 Pr1 80.2(3) C204 C203 Pr1 81.6(3) C205 C204 C203 128.5(5) C205 C204 C209 114.2(4) C203 C204 C209 117.3(4) C205 C204 Pr1 85.6(3) C203 C204 Pr1 68.5(3) C209 C204 Pr1 122.3(3) C204 C205 C206 120.4(5) C204 C205 Pr1 68.1(3) C206 C205 Pr1 136.7(3) C205 C206 C207 110.4(4) C206 C207 C208 107.5(4) C206 C207 C210 111.5(4) C208 C207 C210 88.0(4) C207 C208 C209 86.0(4) C204 C209 C208 110.3(4) C204 C209 C210 108.4(4) C208 C209 C210 87.4(4) C211 C210 C212 109.4(4) C211 C210 C207 119.7(4) C212 C210 C207 113.0(4) C211 C210 C209 117.8(4) C212 C210 C209 110.7(4) C207 C210 C209 84.2(4) C302 C301 Pr1 77.3(3) C301 C302 C303 126.4(5) C301 C302 C313 118.0(5) C303 C302 C313 115.4(5) C301 C302 Pr1 74.0(3) C303 C302 Pr1 72.3(3) C313 C302 Pr1 125.1(3) C302 C303 C304 130.4(5) C302 C303 Pr1 78.3(3) C304 C303 Pr1 83.8(3) C305 C304 C303 128.7(5) C305 C304 C309 114.8(4) C303 C304 C309 116.5(4) C305 C304 Pr1 84.0(3) C303 C304 Pr1 67.1(3) C309 C304 Pr1 126.1(3) C304 C305 C306 120.2(5) C305 C306 C307 110.5(4) C306 C307 C308 108.2(4) C306 C307 C310 111.5(4) C308 C307 C310 87.8(4) C307 C308 C309 86.0(4) C304 C309 C308 108.9(4) C304 C309 C310 109.6(4) C308 C309 C310 87.5(4) C311 C310 C312 108.5(4) C311 C310 C309 118.1(4) C312 C310 C309 112.8(4) C311 C310 C307 119.1(4) C312 C310 C307 112.6(4) C309 C310 C307 84.2(4) C603 Pr2 C503 118.91(15) C603 Pr2 C403 119.26(15) C503 Pr2 C403 119.39(16) C603 Pr2 C401 130.81(16) C503 Pr2 C401 97.21(16) C403 Pr2 C401 54.03(16) C603 Pr2 C601 53.76(16) C503 Pr2 C601 130.55(17) C403 Pr2 C601 97.35(16) C401 Pr2 C601 77.67(17) C603 Pr2 C501 97.58(18) C503 Pr2 C501 53.12(17) C403 Pr2 C501 130.73(16) C401 Pr2 C501 77.45(16) C601 Pr2 C501 78.15(18) C603 Pr2 C402 118.85(15) C503 Pr2 C402 120.23(15) C403 Pr2 C402 29.57(14) C401 Pr2 C402 28.74(15) C601 Pr2 C402 76.53(15) C501 Pr2 C402 105.22(15) C603 Pr2 C502 119.68(16) C503 Pr2 C502 29.30(15) C403 Pr2 C502 119.14(16) C401 Pr2 C502 76.62(17) C601 Pr2 C502 105.10(17) C501 Pr2 C502 27.89(17) C402 Pr2 C502 104.60(16) C603 Pr2 C602 29.53(14) C503 Pr2 C602 118.48(15) C403 Pr2 C602 120.17(15) C401 Pr2 C602 105.09(16) C601 Pr2 C602 28.52(15) C501 Pr2 C602 76.90(18) C402 Pr2 C602 104.30(14) C502 Pr2 C602 103.98(16) C603 Pr2 C604 29.82(14) C503 Pr2 C604 134.32(15) C403 Pr2 C604 93.28(15) C401 Pr2 C604 128.43(16) C601 Pr2 C604 67.54(16) C501 Pr2 C604 127.39(17) C402 Pr2 C604 104.06(15) C502 Pr2 C604 147.57(16) C602 Pr2 C604 53.92(14) C603 Pr2 C504 93.67(15) C503 Pr2 C504 29.44(14) C403 Pr2 C504 133.80(15) C401 Pr2 C504 126.65(16) C601 Pr2 C504 128.82(15) C501 Pr2 C504 67.52(15) C402 Pr2 C504 147.48(15) C502 Pr2 C504 53.64(15) C602 Pr2 C504 104.56(14) C604 Pr2 C504 104.88(14) C603 Pr2 C404 134.24(15) C503 Pr2 C404 94.13(15) C403 Pr2 C404 29.03(14) C401 Pr2 C404 67.34(15) C601 Pr2 C404 126.36(15) C501 Pr2 C404 128.12(17) C402 Pr2 C404 53.27(14) C502 Pr2 C404 104.72(16) C602 Pr2 C404 147.39(14) C604 Pr2 C404 104.42(14) C504 Pr2 C404 104.76(14) C402 C401 Pr2 77.6(3) C401 C402 C403 126.4(5) C401 C402 C413 117.1(5) C403 C402 C413 116.2(5) C401 C402 Pr2 73.6(3) C403 C402 Pr2 72.8(3) C413 C402 Pr2 123.9(3) C402 C403 C404 129.2(5) C402 C403 Pr2 77.6(3) C404 C403 Pr2 83.2(3) C405 C404 C403 129.1(5) C405 C404 C409 113.9(4) C403 C404 C409 117.0(4) C405 C404 Pr2 81.3(3) C403 C404 Pr2 67.7(3) C409 C404 Pr2 128.7(3) C404 C405 C406 121.1(5) C404 C405 Pr2 72.5(3) C406 C405 Pr2 135.9(3) C405 C406 C407 111.1(4) C406 C407 C408 107.2(4) C406 C407 C410 110.3(4) C408 C407 C410 88.0(4) C407 C408 C409 86.0(4) C404 C409 C408 109.3(4) C404 C409 C410 108.6(4) C408 C409 C410 87.2(4) C412 C410 C411 108.9(4) C412 C410 C407 118.3(4) C411 C410 C407 110.4(4) C412 C410 C409 120.3(4) C411 C410 C409 112.1(4) C407 C410 C409 85.1(4) C502 C501 Pr2 76.7(3) C501 C502 C503 127.7(5) C501 C502 C513 116.7(5) C503 C502 C513 115.5(5) C501 C502 Pr2 75.4(3) C503 C502 Pr2 72.4(3) C513 C502 Pr2 124.3(3) C502 C503 C504 129.9(5) C502 C503 Pr2 78.3(3) C504 C503 Pr2 81.6(3) C505 C504 C503 128.9(5) C505 C504 C509 114.4(4) C503 C504 C509 116.6(5) C505 C504 Pr2 83.3(3) C503 C504 Pr2 68.9(3) C509 C504 Pr2 122.3(3) C504 C505 C506 120.1(5) C504 C505 Pr2 70.4(3) C506 C505 Pr2 131.3(3) C505 C506 C507 111.1(4) C506 C507 C510 110.7(4) C506 C507 C508 108.8(4) C510 C507 C508 87.5(4) C509 C508 C507 86.2(4) C504 C509 C508 108.6(4) C504 C509 C510 109.9(4) C508 C509 C510 86.7(4) C512 C510 C511 108.0(4) C512 C510 C507 118.5(4) C511 C510 C507 111.9(4) C512 C510 C509 119.4(4) C511 C510 C509 112.7(4) C507 C510 C509 85.0(4) C602 C601 Pr2 76.6(3) C601 C602 C603 126.2(5) C601 C602 C613 117.3(5) C603 C602 C613 116.2(4) C601 C602 Pr2 74.9(3) C603 C602 Pr2 71.3(3) C613 C602 Pr2 124.4(3) C602 C603 C604 129.3(5) C602 C603 Pr2 79.2(3) C604 C603 Pr2 82.0(3) C605 C604 C603 128.8(5) C605 C604 C609 114.8(5) C603 C604 C609 116.4(4) C605 C604 Pr2 89.3(3) C603 C604 Pr2 68.1(3) C609 C604 Pr2 116.8(3) C604 C605 C606 119.6(5) C607 C606 C605 110.7(4) C606 C607 C608 107.5(4) C606 C607 C610 112.1(4) C608 C607 C610 87.9(4) C607 C608 C609 85.8(4) C604 C609 C608 108.7(4) C604 C609 C610 110.3(4) C608 C609 C610 87.0(4) C612 C610 C611 108.8(5) C612 C610 C607 119.6(5) C611 C610 C607 113.0(5) C612 C610 C609 117.8(4) C611 C610 C609 111.3(4) C607 C610 C609 84.6(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pr1 C203 2.686(5) Pr1 C103 2.719(5) Pr1 C303 2.729(5) Pr1 C301 2.765(5) Pr1 C201 2.784(5) Pr1 C101 2.791(5) Pr1 C302 2.806(5) Pr1 C202 2.814(5) Pr1 C102 2.820(5) Pr1 C204 2.856(5) Pr1 C104 2.896(4) Pr1 C304 2.944(5) C101 C102 1.384(8) C102 C103 1.419(7) C102 C113 1.507(8) C103 C104 1.440(7) C104 C105 1.363(7) C104 C109 1.519(7) C105 C106 1.505(7) C106 C107 1.512(7) C107 C108 1.540(7) C107 C110 1.558(7) C108 C109 1.556(7) C109 C110 1.576(7) C110 C111 1.515(7) C110 C112 1.530(7) C201 C202 1.359(8) C202 C203 1.409(7) C202 C213 1.534(7) C203 C204 1.437(7) C204 C205 1.362(7) C204 C209 1.516(7) C205 C206 1.512(7) C206 C207 1.525(7) C207 C208 1.544(7) C207 C210 1.569(7) C208 C209 1.552(7) C209 C210 1.578(7) C210 C211 1.515(7) C210 C212 1.523(7) C301 C302 1.379(7) C302 C303 1.404(7) C302 C313 1.527(7) C303 C304 1.441(7) C304 C305 1.361(7) C304 C309 1.518(7) C305 C306 1.510(7) C306 C307 1.522(7) C307 C308 1.538(7) C307 C310 1.575(7) C308 C309 1.553(7) C309 C310 1.569(7) C310 C311 1.522(7) C310 C312 1.527(7) Pr2 C603 2.708(5) Pr2 C503 2.734(5) Pr2 C403 2.738(5) Pr2 C401 2.750(5) Pr2 C601 2.789(6) Pr2 C501 2.792(5) Pr2 C402 2.800(5) Pr2 C502 2.809(5) Pr2 C602 2.810(5) Pr2 C604 2.890(5) Pr2 C504 2.898(5) Pr2 C404 2.938(5) C401 C402 1.378(7) C402 C403 1.415(7) C402 C413 1.518(7) C403 C404 1.436(7) C404 C405 1.359(7) C404 C409 1.528(7) C405 C406 1.498(7) C406 C407 1.529(7) C407 C408 1.553(7) C407 C410 1.561(7) C408 C409 1.559(7) C409 C410 1.578(7) C410 C412 1.518(7) C410 C411 1.526(7) C501 C502 1.350(8) C502 C503 1.404(7) C502 C513 1.539(8) C503 C504 1.440(7) C504 C505 1.364(7) C504 C509 1.522(7) C505 C506 1.511(7) C506 C507 1.511(7) C507 C510 1.551(7) C507 C508 1.552(7) C508 C509 1.545(7) C509 C510 1.580(7) C510 C512 1.520(7) C510 C511 1.530(7) C601 C602 1.379(7) C602 C603 1.410(7) C602 C613 1.509(7) C603 C604 1.451(7) C604 C605 1.351(7) C604 C609 1.520(7) C605 C606 1.526(7) C606 C607 1.520(7) C607 C608 1.535(7) C607 C610 1.561(7) C608 C609 1.556(7) C609 C610 1.564(7) C610 C612 1.520(8) C610 C611 1.533(7) 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 C101 C102 C103 C104 -16.9(9) C102 C103 C104 C105 5.7(9) C103 C104 C105 C106 -173.7(5) C104 C105 C106 C107 -3.4(7) C105 C106 C107 C108 -47.0(5) C106 C107 C108 C109 82.7(4) C107 C108 C109 C110 28.5(3) C108 C109 C110 C111 -147.8(5) C109 C110 C111 C112 -129.2(7) C113 C201 C202 C203 -91.3(5) C201 C202 C203 C204 -19.4(9) C202 C203 C204 C205 4.7(9) C203 C204 C205 C206 -169.8(5) C204 C205 C206 C207 -4.9(7) C205 C206 C207 C208 -47.4(5) C206 C207 C208 C209 83.6(4) C207 C208 C209 C210 28.2(4) C208 C209 C210 C211 -148.4(5) C209 C210 C211 C212 -127.6(7) C213 C301 C302 C303 -92.4(5) C301 C302 C303 C304 -17.8(9) C302 C303 C304 C305 7.8(9) C303 C304 C305 C306 -173.6(5) C304 C305 C306 C307 -3.1(7) C305 C306 C307 C308 -47.1(5) C306 C307 C308 C309 83.5(4) C307 C308 C309 C310 28.5(4) C308 C309 C310 C311 -147.9(4) C309 C310 C311 C312 -129.9(6) C313 C401 C402 C403 -43.3(4) C401 C402 C403 C404 -16.9(9) C402 C403 C404 C405 10.8(9) C403 C404 C405 C406 -174.6(5) C404 C405 C406 C407 -2.5(7) C405 C406 C407 C408 -47.4(5) C406 C407 C408 C409 83.0(4) C407 C408 C409 C410 27.3(4) C408 C409 C410 C411 82.9(5) C409 C410 C411 C412 135.5(6)