#------------------------------------------------------------------------------ #$Date: 2018-01-13 03:57:05 +0200 (Sat, 13 Jan 2018) $ #$Revision: 205140 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/11/7121136.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_7121136 loop_ _publ_author_name 'Koner, Abhishek' 'Kelemen, Zsolt' 'Schnakenburg, Gregor' 'Nyul\'aszi, L\'aszl\'o' 'Streubel, Rainer' _publ_section_title ; 1,4-Additions of tricyclic 1,4-diphosphinines -- a novel system to study \s-bond activation and \p--\p dispersion interactions ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C7CC09349G _journal_year 2018 _chemical_formula_moiety '2(C28 H42 N4 O4 P2 S2), C7 H8' _chemical_formula_sum 'C63 H92 N8 O8 P4 S4' _chemical_formula_weight 1341.56 _chemical_name_systematic ABK-435 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-09-14 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2017-12-05 deposited with the CCDC. 2018-01-12 downloaded from the CCDC. ; _cell_angle_alpha 67.920(3) _cell_angle_beta 78.389(3) _cell_angle_gamma 73.028(3) _cell_formula_units_Z 2 _cell_length_a 14.6456(8) _cell_length_b 15.5637(9) _cell_length_c 17.4714(10) _cell_measurement_reflns_used 9788 _cell_measurement_temperature 100 _cell_measurement_theta_max 30.58 _cell_measurement_theta_min 2.45 _cell_volume 3510.8(4) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker Photon100 detector' _diffrn_detector_area_resol_mean 8 _diffrn_detector_type 'CMOS area detector' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker X8-KappaApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0476 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 23083 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.999 _diffrn_reflns_theta_min 1.462 _diffrn_source 'sealed tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6036 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; TWINABS-2012/1 (Bruker,2012) was used for absorption correction. For component 1: wR2(int) was 0.1417 before and 0.0721 after correction. The Ratio of minimum to maximum transmission not present. The \l/2 correction factor is Not present For component 2: wR2(int) was 0.1337 before and 0.0701 after correction. The Ratio of minimum to maximum transmission is 0.81. The \l/2 correction factor is Not present Final HKLF 4 output contains 142568 reflections, Rint = 0.0744 (94879 with I > 3sig(I), Rint = 0.0629) ; _exptl_crystal_colour 'clear orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.269 _exptl_crystal_description plank _exptl_crystal_F_000 1428 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.303 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.133 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 844 _refine_ls_number_reflns 23083 _refine_ls_number_restraints 246 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0970 _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^)+(0.0643P)^2^+25.8602P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2324 _refine_ls_wR_factor_ref 0.2482 _reflns_Friedel_coverage 0.000 _reflns_number_gt 20538 _reflns_number_total 23083 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cc09349g2.cif _cod_data_source_block 2a _cod_database_code 7121136 _shelx_shelxl_version_number 2014/7 _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_max 0.994 _shelx_estimated_absorpt_t_min 0.905 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.4413(14) 0.5587(14) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C19'-C20' = C20'-C21' = C21'-C22' = C20S-C21S = C21S-C22S = C19'-C20S 1.54 with sigma of 0.001 C20'-C22' = C20S-C22S 2.54 with sigma of 0.001 C5S-C6S = C6S-C7S = C5-C6 = C6-C7 1.5 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints C20' \\sim C20S \\sim C21' \\sim C21S \\sim C22' \\sim C22S: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 C5 \\sim C5S \\sim C6 \\sim C6S \\sim C7 \\sim C7S: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(C20') \\sim Ueq, Uanis(C21') \\sim Ueq, Uanis(C22') \\sim Ueq, Uanis(C20S) \\sim Ueq, Uanis(C21S) \\sim Ueq, Uanis(C22S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(C11) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 5. Others Sof(H19E)=Sof(H19F)=Sof(C20S)=Sof(H20E)=Sof(H20F)=Sof(C21S)=Sof(H21E)= Sof(H21F)=Sof(C22S)=Sof(H22G)=Sof(H22H)=Sof(H22I)=1-FVAR(1) Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20C)=Sof(H20D)=Sof(C21')=Sof(H21C)= Sof(H21D)=Sof(C22')=Sof(H22D)=Sof(H22E)=Sof(H22F)=FVAR(1) Sof(H4BC)=Sof(H4BD)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)= Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=1-FVAR(2) Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)= Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(2) 6.a Secondary CH2 refined with riding coordinates: C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C5S(H5SA,H5SB), C6(H6A,H6B), C6S(H6SA,H6SB), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C4'(H4'A,H4'B), C5'(H5'A,H5'B), C6'(H6'A,H6'B), C8'(H8'A,H8'B), C9'(H9'A, H9'B), C10'(H10C,H10D), C15'(H15C,H15D), C16'(H16C,H16D), C17'(H17C,H17D), C19'(H19C,H19D), C19'(H19E,H19F), C20'(H20C,H20D), C20S(H20E,H20F), C21'(H21C, H21D), C21S(H21E,H21F) 6.b Aromatic/amide H refined with riding coordinates: C30(H30), C31(H31), C32(H32), C33(H33), C34(H34) 6.c Fitted hexagon refined as free rotating group: C29(C30,C31,C32,C33,C34) 6.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C7S(H7SA,H7SB,H7SC), C11(H11A,H11B,H11C), C18(H18A,H18B, H18C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C7'(H7'A, H7'B,H7'C), C11'(H11D,H11E,H11F), C18'(H18D,H18E,H18F), C22'(H22D,H22E,H22F), C22S(H22G,H22H,H22I), C26'(H26D,H26E,H26F), C28'(H28D,H28E,H28F), C35(H35A, H35B,H35C) ; _shelx_res_file ; 5306_0m_4.res created by SHELXL-2014/7 TITL 5306_0m_4_a.res in P-1 REM Old TITL 5306_0m_4 in P-1 REM SHELXT solution in P-1 REM R1 0.233, Rweak 0.037, Alpha 0.065, Orientation as input REM Formula found by SHELXT: C59 N11 O6 S8 CELL 0.71073 14.6456 15.5637 17.4714 67.92 78.389 73.028 ZERR 2 0.0008 0.0009 0.001 0.003 0.003 0.003 LATT 1 SFAC C H N O P S UNIT 126 184 16 16 8 8 DFIX 1.54 0.001 C19' C20' C20' C21' C21' C22' C20S C21S C21S C22S C19' C20S DFIX 2.54 0.001 C20' C22' C20S C22S DFIX 1.5 0.01 C5S C6S C6S C7S C5 C6 C6 C7 SIMU 0.001 0.002 2 C20' > C22S SIMU 0.005 0.01 2 C29 > C35 SIMU 0.005 0.01 2 C5 > C7S ISOR 0.01 0.01 C31 C32 C33 C30 C34 C35 ISOR 0.01 0.01 C20' C21' C22' C20S C21S C22S ISOR 0.002 0.004 C11 L.S. 14 PLAN 20 SIZE 0.02 0.06 0.36 TEMP -173.15 BOND $H list 4 fmap 2 ACTA MERG 0 OMIT -2 52 OMIT 0 1 1 OMIT 0 1 0 OMIT -3 0 2 OMIT -3 1 0 OMIT 3 0 1 OMIT 3 1 2 OMIT -2 1 0 OMIT -2 0 2 OMIT -1 0 2 OMIT -1 1 0 OMIT 0 0 2 OMIT 1 1 0 OMIT 1 0 2 OMIT 2 1 0 OMIT 3 1 0 OMIT 0 0 1 OMIT 2 0 2 OMIT 3 0 2 REM REM REM WGHT 0.064300 25.860199 BASF 0.55866 FVAR 0.43025 0.49881 0.71384 S1 6 1.000076 -0.183604 0.618466 11.00000 0.01820 0.02663 = 0.02665 -0.00570 -0.00771 0.00376 S2 6 0.409592 0.124488 0.353983 11.00000 0.01877 0.03124 = 0.03077 -0.00295 -0.01096 -0.00781 P1 5 0.781573 0.127173 0.388398 11.00000 0.01259 0.02024 = 0.01703 -0.00573 -0.00278 -0.00248 P2 5 0.655704 0.096984 0.574580 11.00000 0.01290 0.02426 = 0.01807 -0.00595 -0.00211 -0.00238 O1 4 0.793143 0.333484 0.313229 11.00000 0.02101 0.02115 = 0.02045 -0.00530 -0.00350 -0.00290 O2 4 0.808059 0.352544 0.431421 11.00000 0.03305 0.02394 = 0.03095 -0.01175 -0.00557 -0.00957 O3 4 0.719024 0.254023 0.626025 11.00000 0.05462 0.04619 = 0.02478 -0.01637 -0.01066 -0.01534 O4 4 0.623811 0.354963 0.526491 11.00000 0.03034 0.04027 = 0.06099 -0.03750 -0.01667 0.01262 N1 3 0.905299 -0.041472 0.491778 11.00000 0.01291 0.01791 = 0.01645 -0.00372 -0.00127 -0.00121 N2 3 0.823037 -0.060790 0.614590 11.00000 0.01332 0.02145 = 0.01642 -0.00556 -0.00250 -0.00273 N3 3 0.512194 0.109271 0.474875 11.00000 0.01273 0.02361 = 0.02129 -0.00186 -0.00253 -0.00350 N4 3 0.594926 0.127147 0.353463 11.00000 0.01608 0.02040 = 0.01936 -0.00646 -0.00334 -0.00505 C1 1 0.818924 0.026239 0.480610 11.00000 0.01201 0.02067 = 0.01497 -0.00308 -0.00395 0.00121 C2 1 0.768490 0.014852 0.556231 11.00000 0.01286 0.02679 = 0.02041 -0.00722 -0.00461 -0.00361 C3 1 0.908405 -0.095109 0.574527 11.00000 0.01650 0.02234 = 0.02137 -0.00576 -0.00839 -0.00238 C4 1 0.978551 -0.061990 0.425377 11.00000 0.01373 0.02732 = 0.02222 -0.00723 0.00001 -0.00197 PART 1 AFIX 23 H4AA 2 1.040889 -0.096436 0.448206 31.00000 -1.20000 H4AB 2 0.986738 -0.001431 0.381212 31.00000 -1.20000 AFIX 23 PART 0 PART 2 H4BC 2 0.974995 -0.002929 0.376313 -31.00000 -1.20000 H4BD 2 1.042794 -0.079843 0.444630 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C5 1 0.947156 -0.123220 0.388810 31.00000 0.02861 0.03527 = 0.02727 -0.01786 -0.00193 -0.00570 AFIX 23 H5A 2 0.938081 -0.183107 0.433545 31.00000 -1.20000 H5B 2 0.884773 -0.088300 0.366203 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C5S 1 0.969166 -0.137008 0.400267 -31.00000 0.02897 0.03594 = 0.02821 -0.01867 -0.00185 -0.00708 AFIX 23 H5SA 2 0.970345 -0.195278 0.449885 -31.00000 -1.20000 H5SB 2 1.025816 -0.151215 0.361269 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C6 1 1.019568 -0.147073 0.321121 31.00000 0.03060 0.03716 = 0.02947 -0.02012 -0.00107 -0.00479 AFIX 23 H6A 2 1.079762 -0.187960 0.345238 31.00000 -1.20000 H6B 2 1.034076 -0.087387 0.279667 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C6S 1 0.880466 -0.116102 0.359653 -31.00000 0.02967 0.03475 = 0.02757 -0.02098 -0.00322 -0.00519 AFIX 23 H6SA 2 0.876734 -0.055604 0.312090 -31.00000 -1.20000 H6SB 2 0.823623 -0.106645 0.399914 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C7 1 0.985337 -0.198115 0.277754 31.00000 0.05169 0.05428 = 0.04671 -0.03401 -0.00512 -0.00294 AFIX 137 H7A 2 1.034789 -0.211240 0.233935 31.00000 -1.50000 H7B 2 0.926114 -0.157734 0.253182 31.00000 -1.50000 H7C 2 0.972962 -0.258392 0.318088 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C7S 1 0.876369 -0.193318 0.329083 -31.00000 0.04670 0.04879 = 0.04083 -0.03113 -0.00538 -0.00145 AFIX 137 H7SA 2 0.932278 -0.203203 0.289039 -31.00000 -1.50000 H7SB 2 0.817518 -0.174154 0.302179 -31.00000 -1.50000 H7SC 2 0.876646 -0.252816 0.376151 -31.00000 -1.50000 AFIX 0 PART 0 C8 1 0.796590 -0.094780 0.703597 11.00000 0.01854 0.03038 = 0.01348 -0.00150 0.00004 -0.00749 AFIX 23 H8A 2 0.835987 -0.160146 0.728034 11.00000 -1.20000 H8B 2 0.728440 -0.097940 0.714393 11.00000 -1.20000 AFIX 0 C9 1 0.810586 -0.031430 0.744909 11.00000 0.04919 0.05092 = 0.02380 -0.01304 0.00458 -0.02658 AFIX 23 H9A 2 0.777986 0.035341 0.715432 11.00000 -1.20000 H9B 2 0.879975 -0.034684 0.739788 11.00000 -1.20000 AFIX 0 C10 1 0.772683 -0.057617 0.835125 11.00000 0.06159 0.06456 = 0.03016 -0.02412 -0.00216 -0.00497 AFIX 23 H10A 2 0.708120 -0.069002 0.841187 11.00000 -1.20000 H10B 2 0.814908 -0.118356 0.866315 11.00000 -1.20000 AFIX 0 C11 1 0.765604 0.015344 0.873829 11.00000 0.11102 0.11225 = 0.09924 -0.04495 -0.01318 -0.01783 AFIX 137 H11A 2 0.711136 0.069373 0.854567 11.00000 -1.50000 H11B 2 0.824919 0.037760 0.857871 11.00000 -1.50000 H11C 2 0.756120 -0.013302 0.934405 11.00000 -1.50000 AFIX 0 C12 1 0.605014 0.106032 0.484043 11.00000 0.01339 0.02154 = 0.01992 -0.00344 -0.00323 -0.00665 C13 1 0.656797 0.117469 0.408751 11.00000 0.01244 0.02240 = 0.02653 -0.00925 -0.00518 -0.00349 C14 1 0.506126 0.120173 0.394200 11.00000 0.01707 0.01777 = 0.02410 -0.00089 -0.00623 -0.00283 C15 1 0.430041 0.111054 0.537694 11.00000 0.01257 0.02847 = 0.02668 -0.00376 0.00178 -0.00356 AFIX 23 H15A 2 0.452260 0.074677 0.593426 11.00000 -1.20000 H15B 2 0.384951 0.079405 0.529506 11.00000 -1.20000 AFIX 0 C16 1 0.377219 0.213500 0.533651 11.00000 0.02545 0.03247 = 0.03809 -0.00986 0.00670 0.00571 AFIX 23 H16A 2 0.423332 0.244662 0.540958 11.00000 -1.20000 H16B 2 0.355927 0.249218 0.477518 11.00000 -1.20000 AFIX 0 C17 1 0.292297 0.221920 0.596074 11.00000 0.05719 0.05273 = 0.05655 -0.01400 0.00565 -0.01119 AFIX 23 H17A 2 0.312873 0.188007 0.652611 11.00000 -1.20000 H17B 2 0.245502 0.191022 0.589478 11.00000 -1.20000 AFIX 0 C18 1 0.243198 0.327661 0.586275 11.00000 0.07287 0.05738 = 0.06966 -0.02752 -0.00119 0.01227 AFIX 137 H18A 2 0.206570 0.356499 0.537895 11.00000 -1.50000 H18B 2 0.292221 0.362498 0.578475 11.00000 -1.50000 H18C 2 0.199752 0.330852 0.636257 11.00000 -1.50000 AFIX 0 C19 1 0.621150 0.143809 0.264606 11.00000 0.01934 0.02738 = 0.01270 0.00054 -0.00471 -0.00578 AFIX 23 H19A 2 0.669608 0.182526 0.243941 11.00000 -1.20000 H19B 2 0.563716 0.180773 0.234690 11.00000 -1.20000 AFIX 0 C20 1 0.661106 0.052113 0.245740 11.00000 0.04198 0.02822 = 0.02941 -0.01122 -0.00774 0.00202 AFIX 23 H20A 2 0.611238 0.015176 0.263429 11.00000 -1.20000 H20B 2 0.716134 0.013416 0.278339 11.00000 -1.20000 AFIX 0 C21 1 0.693826 0.068895 0.154365 11.00000 0.03086 0.05471 = 0.03300 -0.02286 -0.01051 0.01133 AFIX 23 H21A 2 0.638735 0.107844 0.121916 11.00000 -1.20000 H21B 2 0.743607 0.105919 0.136842 11.00000 -1.20000 AFIX 0 C22 1 0.733651 -0.021397 0.134323 11.00000 0.08279 0.06629 = 0.05988 -0.04218 -0.01416 0.01253 AFIX 137 H22A 2 0.755139 -0.005733 0.074865 11.00000 -1.50000 H22B 2 0.683741 -0.056897 0.148648 11.00000 -1.50000 H22C 2 0.788110 -0.060594 0.166353 11.00000 -1.50000 AFIX 0 C23 1 0.755915 0.217707 0.441597 11.00000 0.01319 0.02136 = 0.01853 -0.00477 -0.00573 0.00011 C24 1 0.705961 0.206073 0.515793 11.00000 0.01243 0.02571 = 0.01736 -0.00822 -0.00241 0.00074 C25 1 0.788339 0.306442 0.388179 11.00000 0.01088 0.01816 = 0.02447 -0.00513 -0.00741 0.00028 C26 1 0.835322 0.440814 0.381479 11.00000 0.05817 0.02640 = 0.04172 -0.00465 -0.00612 -0.02397 AFIX 137 H26A 2 0.891173 0.428191 0.342191 11.00000 -1.50000 H26B 2 0.851553 0.468309 0.417590 11.00000 -1.50000 H26C 2 0.781735 0.485824 0.350776 11.00000 -1.50000 AFIX 0 C27 1 0.685784 0.273217 0.562291 11.00000 0.02071 0.03551 = 0.02606 -0.01443 0.00367 -0.01036 C28 1 0.609894 0.430542 0.560743 11.00000 0.06467 0.06321 = 0.11986 -0.07489 -0.03163 0.02657 AFIX 137 H28A 2 0.578360 0.491539 0.521937 11.00000 -1.50000 H28B 2 0.672306 0.434700 0.569421 11.00000 -1.50000 H28C 2 0.569655 0.416214 0.613905 11.00000 -1.50000 AFIX 0 S1' 6 1.108242 0.348990 0.128572 11.00000 0.01438 0.02795 = 0.02617 -0.00376 -0.00413 0.00048 S2' 6 0.551444 0.591295 -0.162790 11.00000 0.03488 0.06011 = 0.02409 -0.00531 -0.01287 -0.01892 P1' 5 0.756353 0.617215 0.063718 11.00000 0.01577 0.01917 = 0.02251 -0.00281 -0.00448 -0.00291 P2' 5 0.711859 0.400439 0.139370 11.00000 0.01614 0.02114 = 0.02092 -0.00518 -0.00298 -0.00457 O1' 4 0.689995 0.669839 0.240345 11.00000 0.04505 0.05231 = 0.05706 -0.03603 0.00201 -0.01230 O2' 4 0.547044 0.691730 0.199431 11.00000 0.03607 0.03749 = 0.04468 -0.01635 -0.00052 0.00660 O3' 4 0.581758 0.504656 0.324850 11.00000 0.05132 0.03475 = 0.03140 -0.01533 0.00796 -0.01254 O4' 4 0.574142 0.381446 0.290802 11.00000 0.01715 0.03056 = 0.02449 -0.01160 0.00429 -0.01199 N1' 3 0.948452 0.495504 0.095277 11.00000 0.01317 0.02253 = 0.01585 -0.00440 -0.00213 -0.00253 N2' 3 0.918329 0.353231 0.141453 11.00000 0.01373 0.01509 = 0.01741 -0.00356 -0.00295 0.00239 N3' 3 0.653862 0.623439 -0.065415 11.00000 0.01784 0.02997 = 0.01851 0.00188 -0.00538 -0.00304 N4' 3 0.631536 0.478983 -0.018912 11.00000 0.02423 0.03862 = 0.02155 -0.00556 -0.00769 -0.01213 C1' 1 0.849973 0.507860 0.094275 11.00000 0.01554 0.01603 = 0.01816 -0.00260 -0.00155 -0.00440 C2' 1 0.832417 0.420001 0.123055 11.00000 0.01224 0.02193 = 0.01293 -0.00033 -0.00210 -0.00186 C3' 1 0.990369 0.399358 0.123115 11.00000 0.01698 0.02031 = 0.01317 -0.00434 -0.00308 -0.00184 C4' 1 0.931086 0.250453 0.173036 11.00000 0.01792 0.01977 = 0.02130 -0.00491 -0.00343 -0.00203 AFIX 23 H4'A 2 0.873936 0.234352 0.211199 11.00000 -1.20000 H4'B 2 0.987401 0.220918 0.205290 11.00000 -1.20000 AFIX 0 C5' 1 0.945662 0.208666 0.104406 11.00000 0.03074 0.02250 = 0.02244 -0.00497 -0.00119 -0.01058 AFIX 23 H5'A 2 0.891599 0.241040 0.069652 11.00000 -1.20000 H5'B 2 1.005539 0.220234 0.068553 11.00000 -1.20000 AFIX 0 C6' 1 0.951649 0.102261 0.139861 11.00000 0.03891 0.02820 = 0.04128 -0.01638 -0.00423 -0.00908 AFIX 23 H6'A 2 0.891482 0.091225 0.175448 11.00000 -1.20000 H6'B 2 1.005093 0.070490 0.175330 11.00000 -1.20000 AFIX 0 C7' 1 0.967336 0.057009 0.073214 11.00000 0.07556 0.04849 = 0.05354 -0.02931 -0.00054 -0.02127 AFIX 137 H7'A 2 1.026496 0.068138 0.037381 11.00000 -1.50000 H7'B 2 0.912879 0.085591 0.039773 11.00000 -1.50000 H7'C 2 0.972728 -0.011824 0.099599 11.00000 -1.50000 AFIX 0 C8' 1 1.001416 0.569501 0.073025 11.00000 0.01952 0.02635 = 0.02149 -0.00638 -0.00273 -0.00892 AFIX 23 H8'A 2 0.964422 0.630139 0.036443 11.00000 -1.20000 H8'B 2 1.063581 0.550930 0.041495 11.00000 -1.20000 AFIX 0 C9' 1 1.019834 0.585264 0.148425 11.00000 0.03000 0.03934 = 0.02784 -0.01452 -0.00990 -0.01202 AFIX 23 H9'A 2 1.066829 0.625405 0.130874 11.00000 -1.20000 H9'B 2 1.049172 0.522815 0.188152 11.00000 -1.20000 AFIX 0 C10' 1 0.930266 0.632751 0.193004 11.00000 0.04001 0.03545 = 0.03086 -0.01702 -0.00038 -0.01080 AFIX 23 H10C 2 0.945831 0.628874 0.246964 11.00000 -1.20000 H10D 2 0.879935 0.597434 0.204437 11.00000 -1.20000 AFIX 0 C11' 1 0.890922 0.737970 0.142186 11.00000 0.05470 0.03517 = 0.04881 -0.02223 -0.00492 -0.00783 AFIX 137 H11D 2 0.870545 0.741921 0.090620 11.00000 -1.50000 H11E 2 0.941210 0.772827 0.128906 11.00000 -1.50000 H11F 2 0.835935 0.766227 0.174643 11.00000 -1.50000 AFIX 0 C12' 1 0.696484 0.575065 0.007408 11.00000 0.01539 0.02108 = 0.02136 0.00141 -0.00523 -0.00860 C13' 1 0.681470 0.485993 0.037274 11.00000 0.01582 0.02847 = 0.02133 -0.00715 -0.00260 -0.00617 C14' 1 0.612464 0.564297 -0.082316 11.00000 0.02439 0.03663 = 0.02480 -0.00148 -0.00793 -0.01258 C15' 1 0.648744 0.722700 -0.118345 11.00000 0.01504 0.03018 = 0.02824 0.00385 -0.00530 -0.00247 AFIX 23 H15C 2 0.649565 0.728425 -0.176850 11.00000 -1.20000 H15D 2 0.706061 0.741397 -0.113991 11.00000 -1.20000 AFIX 0 C16' 1 0.558656 0.790776 -0.094698 11.00000 0.02677 0.03069 = 0.03702 -0.00557 -0.00834 0.00011 AFIX 23 H16C 2 0.553078 0.854484 -0.138306 11.00000 -1.20000 H16D 2 0.501971 0.767795 -0.093682 11.00000 -1.20000 AFIX 0 C17' 1 0.556445 0.801200 -0.012552 11.00000 0.05493 0.05115 = 0.04471 -0.01315 -0.01579 0.00498 AFIX 23 H17C 2 0.618671 0.812103 -0.009379 11.00000 -1.20000 H17D 2 0.549207 0.740643 0.032079 11.00000 -1.20000 AFIX 0 C18' 1 0.477093 0.881314 0.002868 11.00000 0.09430 0.09376 = 0.08205 -0.04930 -0.02895 0.04101 AFIX 137 H18D 2 0.478257 0.940094 -0.044741 11.00000 -1.50000 H18E 2 0.486118 0.890713 0.053004 11.00000 -1.50000 H18F 2 0.415158 0.865378 0.010395 11.00000 -1.50000 AFIX 0 C19' 1 0.610749 0.392040 -0.017173 11.00000 0.04983 0.04455 = 0.03858 -0.01524 -0.00900 -0.02611 PART 1 AFIX 23 H19C 2 0.565910 0.409669 -0.059087 21.00000 -1.20000 H19D 2 0.577482 0.363298 0.037975 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H19E 2 0.556014 0.407234 -0.049113 -21.00000 -1.20000 H19F 2 0.595841 0.351111 0.040549 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C20' 1 0.698910 0.315980 -0.033994 21.00000 0.10503 0.08833 = 0.09332 -0.04105 0.00483 -0.02999 AFIX 23 H20C 2 0.750416 0.312464 -0.003136 21.00000 -1.20000 H20D 2 0.681507 0.253556 -0.009543 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C20S 1 0.704152 0.342919 -0.058038 -21.00000 0.10504 0.08839 = 0.09326 -0.04103 0.00497 -0.02994 AFIX 23 H20E 2 0.730720 0.391091 -0.105860 -21.00000 -1.20000 H20F 2 0.752421 0.309767 -0.017559 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C21' 1 0.741731 0.327594 -0.124354 21.00000 0.10497 0.08851 = 0.09341 -0.04072 0.00486 -0.02982 AFIX 23 H21C 2 0.779953 0.376290 -0.144127 21.00000 -1.20000 H21D 2 0.689110 0.350132 -0.160181 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C21S 1 0.681385 0.270492 -0.087500 -21.00000 0.10501 0.08858 = 0.09346 -0.04066 0.00495 -0.02973 AFIX 23 H21E 2 0.625831 0.247292 -0.051732 -21.00000 -1.20000 H21F 2 0.737127 0.214976 -0.082212 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C22' 1 0.806144 0.232456 -0.131410 21.00000 0.10566 0.08991 = 0.09459 -0.03882 0.00615 -0.02773 AFIX 137 H22D 2 0.842861 0.244175 -0.186303 21.00000 -1.50000 H22E 2 0.766087 0.188732 -0.124016 21.00000 -1.50000 H22F 2 0.850464 0.203929 -0.088399 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C22S 1 0.658334 0.315992 -0.178475 -21.00000 0.10470 0.08886 = 0.09325 -0.04047 0.00415 -0.02951 AFIX 137 H22G 2 0.717184 0.304630 -0.215247 -21.00000 -1.50000 H22H 2 0.631962 0.384867 -0.191477 -21.00000 -1.50000 H22I 2 0.611190 0.287431 -0.186591 -21.00000 -1.50000 AFIX 0 PART 0 C23' 1 0.675391 0.576783 0.163875 11.00000 0.01800 0.02657 = 0.02427 -0.00910 -0.00250 -0.00039 C24' 1 0.658790 0.489800 0.194765 11.00000 0.01946 0.02650 = 0.01602 -0.00448 -0.00398 -0.00219 C25' 1 0.639191 0.649458 0.207193 11.00000 0.02188 0.02222 = 0.03725 -0.00779 0.00556 -0.00272 C26' 1 0.505764 0.758577 0.244537 11.00000 0.06009 0.03883 = 0.06831 -0.02605 0.01459 0.01349 AFIX 137 H26D 2 0.531712 0.815447 0.217667 11.00000 -1.50000 H26E 2 0.522001 0.728079 0.301957 11.00000 -1.50000 H26F 2 0.435836 0.777130 0.244302 11.00000 -1.50000 AFIX 0 C27' 1 0.600511 0.460464 0.276600 11.00000 0.02326 0.02668 = 0.02883 -0.00814 0.00169 -0.00483 C28' 1 0.505807 0.356357 0.363240 11.00000 0.02014 0.02901 = 0.02190 -0.00375 0.00149 -0.00737 AFIX 137 H28D 2 0.480193 0.305200 0.362387 11.00000 -1.50000 H28E 2 0.453120 0.412428 0.362650 11.00000 -1.50000 H28F 2 0.537924 0.334486 0.413639 11.00000 -1.50000 AFIX 66 C29 1 0.830577 0.586170 0.646742 11.00000 0.09623 0.11563 = 0.08773 -0.04888 -0.04232 -0.02518 C30 1 0.912386 0.549543 0.601952 11.00000 0.10740 0.13054 = 0.10082 -0.04348 -0.02101 -0.01041 AFIX 43 H30 2 0.960276 0.584684 0.577075 11.00000 -1.20000 AFIX 65 C31 1 0.924123 0.461501 0.593559 11.00000 0.12315 0.14256 = 0.11762 -0.03326 -0.02214 -0.00783 AFIX 43 H31 2 0.980036 0.436468 0.562947 11.00000 -1.20000 AFIX 65 C32 1 0.854053 0.410084 0.629957 11.00000 0.12523 0.13991 = 0.11616 -0.03761 -0.02860 -0.02194 AFIX 43 H32 2 0.862075 0.349911 0.624221 11.00000 -1.20000 AFIX 65 C33 1 0.772243 0.446710 0.674747 11.00000 0.12003 0.14256 = 0.11372 -0.02533 -0.04043 -0.03024 AFIX 43 H33 2 0.724353 0.411568 0.699623 11.00000 -1.20000 AFIX 65 C34 1 0.760505 0.534752 0.683140 11.00000 0.09692 0.12539 = 0.09472 -0.03305 -0.04643 -0.03439 AFIX 43 H34 2 0.704592 0.559785 0.713752 11.00000 -1.20000 AFIX 0 C35 1 0.815690 0.673856 0.656073 11.00000 0.12115 0.10687 = 0.12306 -0.05119 -0.06133 -0.01233 AFIX 137 H35A 2 0.866349 0.672077 0.686108 11.00000 -1.50000 H35B 2 0.753103 0.688039 0.687473 11.00000 -1.50000 H35C 2 0.817078 0.723535 0.601243 11.00000 -1.50000 AFIX 0 HKLF 5 REM 5306_0m_4_a.res in P-1 REM R1 = 0.0970 for 20538 Fo > 4sig(Fo) and 0.1155 for all 23083 data REM 844 parameters refined using 246 restraints END WGHT 0.0644 25.8496 REM Highest difference peak 1.303, deepest hole -0.859, 1-sigma level 0.133 Q1 1 0.7598 0.2954 -0.0449 11.00000 0.05 1.30 Q2 1 0.9198 0.6103 0.5983 11.00000 0.05 1.18 Q3 1 0.4029 0.2554 0.5733 11.00000 0.05 1.18 Q4 1 0.3425 0.3559 0.5637 11.00000 0.05 1.17 Q5 1 0.6568 0.3523 -0.0774 11.00000 0.05 1.17 Q6 1 0.6811 -0.0136 0.8509 11.00000 0.05 0.97 Q7 1 0.7844 0.5125 0.6697 11.00000 0.05 0.95 Q8 1 0.7475 0.6179 0.6676 11.00000 0.05 0.94 Q9 1 0.8194 0.2486 -0.0981 11.00000 0.05 0.93 Q10 1 0.9650 0.5171 0.5567 11.00000 0.05 0.91 Q11 1 0.8546 0.4816 0.6543 11.00000 0.05 0.80 Q12 1 0.7884 0.6542 0.6907 11.00000 0.05 0.77 Q13 1 0.5992 0.8632 0.0034 11.00000 0.05 0.74 Q14 1 1.0554 -0.1916 0.5893 11.00000 0.05 0.67 Q15 1 0.6405 0.8995 -0.0682 11.00000 0.05 0.63 Q16 1 0.9315 0.5192 0.6301 11.00000 0.05 0.62 Q17 1 0.5159 0.5165 0.2681 11.00000 0.05 0.59 Q18 1 0.8161 0.4216 0.6386 11.00000 0.05 0.59 Q19 1 1.0839 0.2656 0.1198 11.00000 0.05 0.56 Q20 1 1.0107 -0.1796 0.6409 11.00000 0.05 0.53 ; _shelx_res_checksum 76811 _shelx_hkl_file ; 1 0 0 0.00198 0.02186 1 2 0 0 95.6375 3.04982 2 2 0 0 0.12791 0.04639 1 3 0 0 462.006 14.7347 2 4 0 0 50.2492 1.63835 2 4 0 0 34.3425 2.04501 1 5 0 0 440.861 9.37855 1 5 0 0 541.387 9.79238 2 5 3 3 1032.12 45.0640 -2 5 0 0 1032.12 45.0640 1 6 0 0 0.23839 0.55871 1 6 0 0 1.96977 0.34635 2 7 4 4 116.873 2.82787 -2 7 0 0 116.873 2.82787 1 8 0 0 11.7662 0.91393 2 8 0 0 8.57386 0.83350 1 9 5 5 167.683 3.64093 -2 9 0 0 167.683 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4 2.14865 2.69445 -2 4 9 23 2.14865 2.69445 1 -5 17 3 6.66837 2.94472 -2 5 9 23 6.66837 2.94472 1 -6 17 3 3.21376 3.14495 -2 6 9 23 3.21376 3.14495 1 -7 16 2 5.10409 2.92089 -2 7 9 23 5.10409 2.92089 1 8 9 23 1.28306 0.69073 2 -9 15 1 24.4979 8.57814 -2 9 9 23 24.4979 8.57814 1 10 9 23 1.53114 0.90783 2 -2 10 23 0.59049 1.18913 2 -2 10 23 3.34595 1.61226 1 1 21 8 11.4240 3.33060 -2 -1 10 23 11.4240 3.33060 1 0 20 7 52.6410 8.29574 -2 0 10 23 52.6410 8.29574 1 -1 20 7 9.77029 3.14235 -2 1 10 23 9.77029 3.14235 1 -2 19 6 20.1811 4.21266 -2 2 10 23 20.1811 4.21266 1 3 10 23 19.8370 3.57600 2 3 10 23 4.38860 1.29818 1 -4 18 5 5.82477 2.22336 -2 4 10 23 5.82477 2.22336 1 5 10 23 22.4252 2.86968 2 5 10 23 3.46161 2.53084 1 -6 17 4 14.6800 3.61766 -2 6 10 23 14.6800 3.61766 1 -7 16 3 5.76601 3.27329 -2 7 10 23 5.76601 3.27329 1 -8 16 3 14.1228 12.1724 -2 8 10 23 14.1228 12.1724 1 10 10 23 12.5999 2.07471 2 -2 11 23 0.14005 0.84813 2 -2 11 23 1.42501 1.70593 1 1 21 9 18.6865 3.59834 -2 -1 11 23 18.6865 3.59834 1 0 11 23 12.6299 2.07263 2 0 11 23 1.09547 1.54536 1 -1 20 8 30.1165 6.75735 -2 1 11 23 30.1165 6.75735 1 2 11 23 4.30320 1.36095 1 -3 19 7 1.18822 2.90335 -2 3 11 23 1.18822 2.90335 1 -4 18 6 77.2529 13.1804 -2 4 11 23 77.2529 13.1804 1 5 11 23 0.17437 0.99987 2 -5 18 6 1.02161 3.03671 -2 5 11 23 1.02161 3.03671 1 -6 17 5 11.3501 2.60858 -2 6 11 23 11.3501 2.60858 1 7 11 23 1.05834 1.81680 2 7 11 23 0.93020 1.38508 1 -8 16 4 37.0524 14.4348 -2 8 11 23 37.0524 14.4348 1 9 11 23 35.2307 11.7082 1 9 11 23 63.0728 7.64249 2 -11 14 2 3.22460 6.49652 -2 11 11 23 3.22460 6.49652 1 1 21 10 29.8894 5.46714 -2 -1 12 23 29.8894 5.46714 1 0 21 10 2.84886 3.90412 -2 0 12 23 2.84886 3.90412 1 -1 20 9 26.6675 5.38889 -2 1 12 23 26.6675 5.38889 1 2 12 23 4.50444 1.44037 1 -3 19 8 4.27173 2.34892 -2 3 12 23 4.27173 2.34892 1 4 12 23 0.56759 0.71588 2 4 12 23 1.01887 1.37305 1 9 12 23 1.44980 1.15976 2 -10 15 4 36.0335 10.5159 -2 10 12 23 36.0335 10.5159 1 11 12 23 6.26144 3.19345 1 11 12 23 18.3212 1.45548 2 6 13 23 0.40142 0.71161 2 6 13 23 2.16021 1.39834 1 -7 17 7 28.6526 8.84062 -2 7 13 23 28.6526 8.84062 1 -8 16 6 47.2181 12.0247 -2 8 13 23 47.2181 12.0247 1 8 13 23 3.03694 1.49567 1 8 13 23 10.8771 2.11164 2 -9 16 6 26.0277 8.41524 -2 9 13 23 26.0277 8.41524 1 -10 15 5 35.2585 9.91734 -2 10 13 23 35.2585 9.91734 1 11 13 23 1.94735 0.73500 2 1 14 23 4.02334 1.75566 1 -2 20 11 2.69418 1.53112 -2 2 14 23 2.69418 1.53112 1 3 14 23 1.96741 1.52441 1 -7 17 8 16.3014 6.85815 -2 7 14 23 16.3014 6.85815 1 8 14 23 0.69819 1.57312 1 -8 17 8 133.939 20.4744 -2 8 14 23 133.939 20.4744 1 8 14 23 6.78172 14.8414 2 -9 16 7 18.2073 9.47652 -2 9 14 23 18.2073 9.47652 1 -10 15 6 41.5394 10.7265 -2 10 14 23 41.5394 10.7265 1 10 14 23 5.63214 0.73827 2 3 15 23 21.0497 3.08113 2 3 15 23 18.5917 7.80034 1 5 15 23 2.48061 0.87418 2 5 15 23 0.42911 1.55749 1 -6 18 10 31.1632 8.97950 -2 6 15 23 31.1632 8.97950 1 7 15 23 2.26992 1.58859 1 -7 17 9 48.2920 11.2860 -2 7 15 23 48.2920 11.2860 1 7 15 23 0.58559 1.19986 2 8 15 23 13.4785 7.83378 1 8 15 23 2.61401 0.61810 2 0 3 24 -1.4037 1.67220 1 1 -19 2 6.66292 4.75505 -2 1 3 24 6.66292 4.75505 1 2 3 24 -0.1592 1.61925 1 2 3 24 -0.9081 1.26489 2 3 -18 3 -4.0557 3.31115 -2 3 3 24 -4.0557 3.31115 1 -1 4 24 0.41014 1.58625 1 0 20 0 1.87024 3.50261 -2 0 4 24 1.87024 3.50261 1 0 4 24 4.78657 1.27543 2 1 -19 1 -2.9707 3.71382 -2 1 4 24 -2.9707 3.71382 1 2 4 24 23.3618 14.0081 2 2 -19 1 2.56567 3.93356 -2 2 4 24 2.56567 3.93356 1 3 -18 2 29.4804 6.47709 -2 3 4 24 29.4804 6.47709 1 4 4 24 51.3078 8.22971 1 4 4 24 169.132 27.2939 2 6 4 24 -1.0384 0.99829 2 7 4 24 0.57563 0.77194 2 -1 5 24 18.0266 2.22668 2 -1 5 24 0.85280 1.46262 1 0 20 1 11.6450 3.41644 -2 0 5 24 11.6450 3.41644 1 1 5 24 0.93559 1.45596 1 -2 19 0 -0.2561 2.92170 -2 2 5 24 -0.2561 2.92170 1 3 -18 1 -1.1723 3.69771 -2 3 5 24 -1.1723 3.69771 1 4 -18 1 1.52793 3.65985 -2 4 5 24 1.52793 3.65985 1 6 5 24 36.3652 12.3706 2 1 21 3 0.42535 3.48718 -2 -1 6 24 0.42535 3.48718 1 -1 6 24 6.57227 2.34820 2 0 20 2 5.02890 3.62895 -2 0 6 24 5.02890 3.62895 1 -1 20 2 44.2688 8.76702 -2 1 6 24 44.2688 8.76702 1 -2 19 1 1.94681 2.87639 -2 2 6 24 1.94681 2.87639 1 3 6 24 3.14719 1.04596 2 3 6 24 2.49999 1.40799 1 -4 18 0 7.75250 2.40970 -2 4 6 24 7.75250 2.40970 1 5 6 24 0.16384 1.45279 1 1 21 4 16.4311 5.18493 -2 -1 7 24 16.4311 5.18493 1 0 7 24 1.14333 1.46989 1 -1 20 3 8.15591 3.96291 -2 1 7 24 8.15591 3.96291 1 -2 19 2 35.4577 6.48164 -2 2 7 24 35.4577 6.48164 1 -3 19 2 -0.1181 3.42888 -2 3 7 24 -0.1181 3.42888 1 -4 18 1 3.79643 3.23816 -2 4 7 24 3.79643 3.23816 1 5 7 24 1.10176 1.41428 1 7 7 24 -0.2945 0.68220 2 8 -16 1 18.7621 7.90545 -2 8 7 24 18.7621 7.90545 1 9 7 24 -3.0276 7.57807 1 1 21 5 17.0259 5.34840 -2 -1 8 24 17.0259 5.34840 1 0 21 5 44.3647 8.26895 -2 0 8 24 44.3647 8.26895 1 0 8 24 129.179 31.9794 2 2 8 24 33.6788 7.38596 1 2 8 24 63.2415 7.29408 2 -3 19 3 6.03790 3.19550 -2 3 8 24 6.03790 3.19550 1 4 8 24 -0.7079 1.34041 1 -5 18 2 10.1525 3.37668 -2 5 8 24 10.1525 3.37668 1 -6 17 1 0.57327 3.39840 -2 6 8 24 0.57327 3.39840 1 9 8 24 0.63683 0.50193 2 -1 9 24 1.83857 1.64688 1 0 9 24 17.7726 14.5078 2 0 21 6 0.84551 3.30880 -2 0 9 24 0.84551 3.30880 1 -1 20 5 1.42252 3.51972 -2 1 9 24 1.42252 3.51972 1 -2 20 5 0.86176 3.23239 -2 2 9 24 0.86176 3.23239 1 -3 19 4 4.00429 2.88937 -2 3 9 24 4.00429 2.88937 1 4 9 24 -0.0967 1.35979 1 -5 18 3 1.40476 2.52711 -2 5 9 24 1.40476 2.52711 1 6 9 24 3.87365 0.68714 2 6 9 24 -0.1958 1.40791 1 0 21 7 6.12250 3.17623 -2 0 10 24 6.12250 3.17623 1 1 10 24 1.24453 1.46726 1 -2 20 6 20.4441 3.56967 -2 2 10 24 20.4441 3.56967 1 3 10 24 0.72981 1.42206 1 -4 19 5 2.16659 2.95259 -2 4 10 24 2.16659 2.95259 1 -5 18 4 4.28641 3.16990 -2 5 10 24 4.28641 3.16990 1 -6 18 4 3.15849 3.33799 -2 6 10 24 3.15849 3.33799 1 -7 17 3 2.37783 2.97616 -2 7 10 24 2.37783 2.97616 1 8 10 24 5.61248 1.01293 2 -9 16 2 19.3029 6.90447 -2 9 10 24 19.3029 6.90447 1 0 21 8 49.5861 9.96701 -2 0 11 24 49.5861 9.96701 1 1 11 24 0.63158 1.56001 1 1 11 24 24.9542 15.9782 2 -2 20 7 8.39113 3.29965 -2 2 11 24 8.39113 3.29965 1 3 11 24 13.9386 2.11920 2 3 11 24 3.47628 1.47508 1 -4 19 6 10.7562 3.62149 -2 4 11 24 10.7562 3.62149 1 5 11 24 0.53151 1.47990 1 5 11 24 1.92626 0.76343 2 -6 18 5 1.32085 2.81023 -2 6 11 24 1.32085 2.81023 1 -7 17 4 7.96217 4.00960 -2 7 11 24 7.96217 4.00960 1 8 11 24 -3.6215 11.0503 2 1 12 24 36.7249 5.45819 2 1 12 24 17.2322 3.93469 1 2 12 24 2.43335 1.58503 1 3 12 24 40.7215 21.3703 2 -3 20 8 7.28513 3.26776 -2 3 12 24 7.28513 3.26776 1 -4 19 7 10.6421 3.31857 -2 4 12 24 10.6421 3.31857 1 -5 19 7 2.25364 3.62467 -2 5 12 24 2.25364 3.62467 1 5 12 24 -9.2576 13.1591 2 -6 18 6 12.1241 2.99195 -2 6 12 24 12.1241 2.99195 1 7 12 24 4.49066 4.67343 1 7 12 24 10.2753 1.95005 2 -8 17 5 20.6572 9.87097 -2 8 12 24 20.6572 9.87097 1 9 12 24 3.33490 1.00753 2 -3 20 9 6.18692 2.76160 -2 3 13 24 6.18692 2.76160 1 4 13 24 4.51984 1.17175 2 4 13 24 1.44184 1.59221 1 5 13 24 -4.8398 12.9519 2 7 13 24 4.08524 0.67672 2 7 13 24 21.0110 9.14226 1 -4 19 2 -0.3871 3.54855 -2 4 8 25 -0.3871 3.54855 1 5 8 25 0.34962 1.15050 2 5 8 25 0.77669 1.61098 1 4 9 25 8.36254 1.58569 1 5 9 25 2.22264 1.30766 2 5 9 25 4.08141 1.58527 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 2923 _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 S1 S 1.00008(12) -0.18360(13) 0.61847(12) 0.0261(4) Uani 1 1 d . . . . . S2 S 0.40959(12) 0.12449(13) 0.35398(11) 0.0275(4) Uani 1 1 d . . . . . P1 P 0.78157(11) 0.12717(12) 0.38840(10) 0.0169(3) Uani 1 1 d . . . . . P2 P 0.65570(11) 0.09698(12) 0.57458(10) 0.0192(4) Uani 1 1 d . . . . . O1 O 0.7931(3) 0.3335(3) 0.3132(3) 0.0217(10) Uani 1 1 d . . . . . O2 O 0.8081(3) 0.3525(3) 0.4314(3) 0.0276(11) Uani 1 1 d . . . . . O3 O 0.7190(4) 0.2540(4) 0.6260(3) 0.0388(14) Uani 1 1 d . . . . . O4 O 0.6238(4) 0.3550(4) 0.5265(4) 0.0407(14) Uani 1 1 d . . . . . N1 N 0.9053(3) -0.0415(4) 0.4918(3) 0.0170(11) Uani 1 1 d . . . . . N2 N 0.8230(3) -0.0608(4) 0.6146(3) 0.0175(11) Uani 1 1 d . . . . . N3 N 0.5122(4) 0.1093(4) 0.4749(3) 0.0210(12) Uani 1 1 d . . . . . N4 N 0.5949(4) 0.1271(4) 0.3535(3) 0.0183(11) Uani 1 1 d . . . . . C1 C 0.8189(4) 0.0262(5) 0.4806(4) 0.0175(13) Uani 1 1 d . . . . . C2 C 0.7685(4) 0.0149(5) 0.5562(4) 0.0201(13) Uani 1 1 d . . . . . C3 C 0.9084(4) -0.0951(5) 0.5745(4) 0.0201(13) Uani 1 1 d . . . . . C4 C 0.9786(4) -0.0620(5) 0.4254(4) 0.0224(14) Uani 1 1 d . . . . . H4AA H 1.0409 -0.0964 0.4482 0.027 Uiso 0.714(11) 1 calc R . P A 1 H4AB H 0.9867 -0.0014 0.3812 0.027 Uiso 0.714(11) 1 calc R . P A 1 H4BC H 0.9750 -0.0029 0.3763 0.027 Uiso 0.286(11) 1 calc R . P A 2 H4BD H 1.0428 -0.0798 0.4446 0.027 Uiso 0.286(11) 1 calc R . P A 2 C5 C 0.9472(8) -0.1232(12) 0.3888(8) 0.029(2) Uani 0.714(11) 1 d D U P A 1 H5A H 0.9381 -0.1831 0.4335 0.035 Uiso 0.714(11) 1 calc R . P A 1 H5B H 0.8848 -0.0883 0.3662 0.035 Uiso 0.714(11) 1 calc R . P A 1 C5S C 0.969(2) -0.137(3) 0.400(2) 0.029(3) Uani 0.286(11) 1 d D U P A 2 H5SA H 0.9703 -0.1953 0.4499 0.035 Uiso 0.286(11) 1 calc R . P A 2 H5SB H 1.0258 -0.1512 0.3613 0.035 Uiso 0.286(11) 1 calc R . P A 2 C6 C 1.0196(7) -0.1471(8) 0.3211(6) 0.031(2) Uani 0.714(11) 1 d D U P A 1 H6A H 1.0798 -0.1880 0.3452 0.037 Uiso 0.714(11) 1 calc R . P A 1 H6B H 1.0341 -0.0874 0.2797 0.037 Uiso 0.714(11) 1 calc R . P A 1 C6S C 0.8805(17) -0.1161(17) 0.3597(15) 0.028(3) Uani 0.286(11) 1 d D U P A 2 H6SA H 0.8767 -0.0556 0.3121 0.034 Uiso 0.286(11) 1 calc R . P A 2 H6SB H 0.8236 -0.1066 0.3999 0.034 Uiso 0.286(11) 1 calc R . P A 2 C7 C 0.9853(9) -0.1981(9) 0.2778(8) 0.048(3) Uani 0.714(11) 1 d D U P A 1 H7A H 1.0348 -0.2112 0.2339 0.072 Uiso 0.714(11) 1 calc GR . P A 1 H7B H 0.9261 -0.1577 0.2532 0.072 Uiso 0.714(11) 1 calc GR . P A 1 H7C H 0.9730 -0.2584 0.3181 0.072 Uiso 0.714(11) 1 calc GR . P A 1 C7S C 0.876(2) -0.1933(19) 0.3291(19) 0.043(5) Uani 0.286(11) 1 d D U P A 2 H7SA H 0.9323 -0.2032 0.2890 0.064 Uiso 0.286(11) 1 calc GR . P A 2 H7SB H 0.8175 -0.1742 0.3022 0.064 Uiso 0.286(11) 1 calc GR . P A 2 H7SC H 0.8766 -0.2528 0.3762 0.064 Uiso 0.286(11) 1 calc GR . P A 2 C8 C 0.7966(5) -0.0948(5) 0.7036(4) 0.0225(14) Uani 1 1 d . . . . . H8A H 0.8360 -0.1601 0.7280 0.027 Uiso 1 1 calc R . . . . H8B H 0.7284 -0.0979 0.7144 0.027 Uiso 1 1 calc R . . . . C9 C 0.8106(6) -0.0314(6) 0.7449(5) 0.0391(19) Uani 1 1 d . . . . . H9A H 0.7780 0.0353 0.7154 0.047 Uiso 1 1 calc R . . . . H9B H 0.8800 -0.0347 0.7398 0.047 Uiso 1 1 calc R . . . . C10 C 0.7727(7) -0.0576(7) 0.8351(5) 0.052(2) Uani 1 1 d . . . . . H10A H 0.7081 -0.0690 0.8412 0.063 Uiso 1 1 calc R . . . . H10B H 0.8149 -0.1184 0.8663 0.063 Uiso 1 1 calc R . . . . C11 C 0.7656(12) 0.0153(11) 0.8738(10) 0.106(5) Uani 1 1 d . U . . . H11A H 0.7111 0.0694 0.8546 0.160 Uiso 1 1 calc GR . . . . H11B H 0.8249 0.0378 0.8579 0.160 Uiso 1 1 calc GR . . . . H11C H 0.7561 -0.0133 0.9344 0.160 Uiso 1 1 calc GR . . . . C12 C 0.6050(4) 0.1060(5) 0.4840(4) 0.0186(13) Uani 1 1 d . . . . . C13 C 0.6568(4) 0.1175(5) 0.4088(4) 0.0198(14) Uani 1 1 d . . . . . C14 C 0.5061(4) 0.1202(5) 0.3942(4) 0.0212(14) Uani 1 1 d . . . . . C15 C 0.4300(4) 0.1111(5) 0.5377(4) 0.0251(15) Uani 1 1 d . . . . . H15A H 0.4523 0.0747 0.5934 0.030 Uiso 1 1 calc R . . . . H15B H 0.3850 0.0794 0.5295 0.030 Uiso 1 1 calc R . . . . C16 C 0.3772(5) 0.2135(6) 0.5337(5) 0.0370(19) Uani 1 1 d . . . . . H16A H 0.4233 0.2447 0.5410 0.044 Uiso 1 1 calc R . . . . H16B H 0.3559 0.2492 0.4775 0.044 Uiso 1 1 calc R . . . . C17 C 0.2923(7) 0.2219(7) 0.5961(7) 0.059(3) Uani 1 1 d . . . . . H17A H 0.3129 0.1880 0.6526 0.071 Uiso 1 1 calc R . . . . H17B H 0.2455 0.1910 0.5895 0.071 Uiso 1 1 calc R . . . . C18 C 0.2432(9) 0.3277(8) 0.5863(7) 0.072(3) Uani 1 1 d . . . . . H18A H 0.2066 0.3565 0.5379 0.108 Uiso 1 1 calc GR . . . . H18B H 0.2922 0.3625 0.5785 0.108 Uiso 1 1 calc GR . . . . H18C H 0.1998 0.3309 0.6363 0.108 Uiso 1 1 calc GR . . . . C19 C 0.6211(5) 0.1438(5) 0.2646(4) 0.0215(14) Uani 1 1 d . . . . . H19A H 0.6696 0.1825 0.2439 0.026 Uiso 1 1 calc R . . . . H19B H 0.5637 0.1808 0.2347 0.026 Uiso 1 1 calc R . . . . C20 C 0.6611(6) 0.0521(5) 0.2457(5) 0.0345(18) Uani 1 1 d . . . . . H20A H 0.6112 0.0152 0.2634 0.041 Uiso 1 1 calc R . . . . H20B H 0.7161 0.0134 0.2783 0.041 Uiso 1 1 calc R . . . . C21 C 0.6938(6) 0.0689(6) 0.1544(5) 0.041(2) Uani 1 1 d . . . . . H21A H 0.6387 0.1078 0.1219 0.049 Uiso 1 1 calc R . . . . H21B H 0.7436 0.1059 0.1368 0.049 Uiso 1 1 calc R . . . . C22 C 0.7337(9) -0.0214(8) 0.1343(7) 0.069(3) Uani 1 1 d . . . . . H22A H 0.7551 -0.0057 0.0749 0.104 Uiso 1 1 calc GR . . . . H22B H 0.6837 -0.0569 0.1486 0.104 Uiso 1 1 calc GR . . . . H22C H 0.7881 -0.0606 0.1664 0.104 Uiso 1 1 calc GR . . . . C23 C 0.7559(4) 0.2177(5) 0.4416(4) 0.0186(13) Uani 1 1 d . . . . . C24 C 0.7060(4) 0.2061(5) 0.5158(4) 0.0193(13) Uani 1 1 d . . . . . C25 C 0.7883(4) 0.3064(4) 0.3882(4) 0.0185(13) Uani 1 1 d . . . . . C26 C 0.8353(7) 0.4408(6) 0.3815(5) 0.041(2) Uani 1 1 d . . . . . H26A H 0.8912 0.4282 0.3422 0.061 Uiso 1 1 calc GR . . . . H26B H 0.8516 0.4683 0.4176 0.061 Uiso 1 1 calc GR . . . . H26C H 0.7817 0.4858 0.3508 0.061 Uiso 1 1 calc GR . . . . C27 C 0.6858(5) 0.2732(5) 0.5623(4) 0.0263(15) Uani 1 1 d . . . . . C28 C 0.6099(8) 0.4305(8) 0.5607(8) 0.075(4) Uani 1 1 d . . . . . H28A H 0.5784 0.4915 0.5219 0.113 Uiso 1 1 calc GR . . . . H28B H 0.6723 0.4347 0.5694 0.113 Uiso 1 1 calc GR . . . . H28C H 0.5697 0.4162 0.6139 0.113 Uiso 1 1 calc GR . . . . S1' S 1.10824(11) 0.34899(13) 0.12857(11) 0.0254(4) Uani 1 1 d . . . . . S2' S 0.55144(15) 0.59129(17) -0.16279(12) 0.0392(5) Uani 1 1 d . . . . . P1' P 0.75635(12) 0.61722(12) 0.06372(11) 0.0203(4) Uani 1 1 d . . . . . P2' P 0.71186(12) 0.40044(12) 0.13937(11) 0.0198(4) Uani 1 1 d . . . . . O1' O 0.6900(4) 0.6698(4) 0.2403(4) 0.0471(15) Uani 1 1 d . . . . . O2' O 0.5470(4) 0.6917(4) 0.1994(4) 0.0427(14) Uani 1 1 d . . . . . O3' O 0.5818(4) 0.5047(4) 0.3248(3) 0.0393(13) Uani 1 1 d . . . . . O4' O 0.5741(3) 0.3814(3) 0.2908(3) 0.0229(10) Uani 1 1 d . . . . . N1' N 0.9485(4) 0.4955(4) 0.0953(3) 0.0181(11) Uani 1 1 d . . . . . N2' N 0.9183(4) 0.3532(4) 0.1415(3) 0.0171(11) Uani 1 1 d . . . . . N3' N 0.6539(4) 0.6234(4) -0.0654(3) 0.0252(13) Uani 1 1 d . . . . . N4' N 0.6315(4) 0.4790(5) -0.0189(4) 0.0277(13) Uani 1 1 d . . . . . C1' C 0.8500(4) 0.5079(4) 0.0943(4) 0.0174(13) Uani 1 1 d . . . . . C2' C 0.8324(4) 0.4200(5) 0.1231(4) 0.0178(13) Uani 1 1 d . . . . . C3' C 0.9904(4) 0.3994(5) 0.1231(4) 0.0176(13) Uani 1 1 d . . . . . C4' C 0.9311(5) 0.2505(5) 0.1730(4) 0.0206(13) Uani 1 1 d . . . . . H4'A H 0.8739 0.2344 0.2112 0.025 Uiso 1 1 calc R . . . . H4'B H 0.9874 0.2209 0.2053 0.025 Uiso 1 1 calc R . . . . C5' C 0.9457(5) 0.2087(5) 0.1044(4) 0.0253(15) Uani 1 1 d . . . . . H5'A H 0.8916 0.2410 0.0697 0.030 Uiso 1 1 calc R . . . . H5'B H 1.0055 0.2202 0.0686 0.030 Uiso 1 1 calc R . . . . C6' C 0.9516(6) 0.1023(5) 0.1399(5) 0.0345(17) Uani 1 1 d . . . . . H6'A H 0.8915 0.0912 0.1754 0.041 Uiso 1 1 calc R . . . . H6'B H 1.0051 0.0705 0.1753 0.041 Uiso 1 1 calc R . . . . C7' C 0.9673(8) 0.0570(7) 0.0732(6) 0.055(3) Uani 1 1 d . . . . . H7'A H 1.0265 0.0681 0.0374 0.083 Uiso 1 1 calc GR . . . . H7'B H 0.9129 0.0856 0.0398 0.083 Uiso 1 1 calc GR . . . . H7'C H 0.9727 -0.0118 0.0996 0.083 Uiso 1 1 calc GR . . . . C8' C 1.0014(5) 0.5695(5) 0.0730(4) 0.0221(14) Uani 1 1 d . . . . . H8'A H 0.9644 0.6301 0.0364 0.027 Uiso 1 1 calc R . . . . H8'B H 1.0636 0.5509 0.0415 0.027 Uiso 1 1 calc R . . . . C9' C 1.0198(5) 0.5853(6) 0.1484(4) 0.0295(16) Uani 1 1 d . . . . . H9'A H 1.0668 0.6254 0.1309 0.035 Uiso 1 1 calc R . . . . H9'B H 1.0492 0.5228 0.1882 0.035 Uiso 1 1 calc R . . . . C10' C 0.9303(6) 0.6328(6) 0.1930(5) 0.0338(17) Uani 1 1 d . . . . . H10C H 0.9458 0.6289 0.2470 0.041 Uiso 1 1 calc R . . . . H10D H 0.8799 0.5974 0.2044 0.041 Uiso 1 1 calc R . . . . C11' C 0.8909(7) 0.7380(6) 0.1422(6) 0.045(2) Uani 1 1 d . . . . . H11D H 0.8705 0.7419 0.0906 0.067 Uiso 1 1 calc GR . . . . H11E H 0.9412 0.7728 0.1289 0.067 Uiso 1 1 calc GR . . . . H11F H 0.8359 0.7662 0.1746 0.067 Uiso 1 1 calc GR . . . . C12' C 0.6965(4) 0.5751(5) 0.0074(4) 0.0204(13) Uani 1 1 d . . . . . C13' C 0.6815(4) 0.4860(5) 0.0373(4) 0.0220(14) Uani 1 1 d . . . . . C14' C 0.6125(5) 0.5643(6) -0.0823(4) 0.0293(16) Uani 1 1 d . . . . . C15' C 0.6487(5) 0.7227(5) -0.1183(5) 0.0288(16) Uani 1 1 d . . . . . H15C H 0.6496 0.7284 -0.1768 0.035 Uiso 1 1 calc R . . . . H15D H 0.7061 0.7414 -0.1140 0.035 Uiso 1 1 calc R . . . . C16' C 0.5587(5) 0.7908(6) -0.0947(5) 0.0341(17) Uani 1 1 d . . . . . H16C H 0.5531 0.8545 -0.1383 0.041 Uiso 1 1 calc R . . . . H16D H 0.5020 0.7678 -0.0937 0.041 Uiso 1 1 calc R . . . . C17' C 0.5564(7) 0.8012(7) -0.0126(6) 0.054(2) Uani 1 1 d . . . . . H17C H 0.6187 0.8121 -0.0094 0.064 Uiso 1 1 calc R . . . . H17D H 0.5492 0.7406 0.0321 0.064 Uiso 1 1 calc R . . . . C18' C 0.4771(10) 0.8813(10) 0.0029(8) 0.096(5) Uani 1 1 d . . . . . H18D H 0.4783 0.9401 -0.0447 0.143 Uiso 1 1 calc GR . . . . H18E H 0.4861 0.8907 0.0530 0.143 Uiso 1 1 calc GR . . . . H18F H 0.4152 0.8654 0.0104 0.143 Uiso 1 1 calc GR . . . . C19' C 0.6107(6) 0.3920(6) -0.0172(5) 0.0399(19) Uani 1 1 d D . . . . H19C H 0.5659 0.4097 -0.0591 0.048 Uiso 0.499(12) 1 calc R . P B 1 H19D H 0.5775 0.3633 0.0380 0.048 Uiso 0.499(12) 1 calc R . P B 1 H19E H 0.5560 0.4072 -0.0491 0.048 Uiso 0.501(12) 1 calc R . P B 2 H19F H 0.5958 0.3511 0.0405 0.048 Uiso 0.501(12) 1 calc R . P B 2 C20' C 0.6989(13) 0.3160(13) -0.0340(11) 0.093(3) Uani 0.499(12) 1 d D U P B 1 H20C H 0.7504 0.3125 -0.0031 0.112 Uiso 0.499(12) 1 calc R . P B 1 H20D H 0.6815 0.2536 -0.0095 0.112 Uiso 0.499(12) 1 calc R . P B 1 C20S C 0.7042(8) 0.3429(14) -0.0580(11) 0.093(3) Uani 0.501(12) 1 d D U P B 2 H20E H 0.7307 0.3911 -0.1059 0.112 Uiso 0.501(12) 1 calc R . P B 2 H20F H 0.7524 0.3098 -0.0176 0.112 Uiso 0.501(12) 1 calc R . P B 2 C21' C 0.7417(19) 0.3276(11) -0.1244(10) 0.093(3) Uani 0.499(12) 1 d D U P B 1 H21C H 0.7800 0.3763 -0.1441 0.112 Uiso 0.499(12) 1 calc R . P B 1 H21D H 0.6891 0.3501 -0.1602 0.112 Uiso 0.499(12) 1 calc R . P B 1 C21S C 0.681(2) 0.2705(11) -0.0875(10) 0.094(3) Uani 0.501(12) 1 d D U P B 2 H21E H 0.6258 0.2473 -0.0517 0.112 Uiso 0.501(12) 1 calc R . P B 2 H21F H 0.7371 0.2150 -0.0822 0.112 Uiso 0.501(12) 1 calc R . P B 2 C22' C 0.8061(18) 0.2325(14) -0.1314(12) 0.096(3) Uani 0.499(12) 1 d D U P B 1 H22D H 0.8429 0.2442 -0.1863 0.144 Uiso 0.499(12) 1 calc GR . P B 1 H22E H 0.7661 0.1887 -0.1240 0.144 Uiso 0.499(12) 1 calc GR . P B 1 H22F H 0.8505 0.2039 -0.0884 0.144 Uiso 0.499(12) 1 calc GR . P B 1 C22S C 0.6583(19) 0.3160(17) -0.1785(10) 0.093(3) Uani 0.501(12) 1 d D U P B 2 H22G H 0.7172 0.3046 -0.2152 0.140 Uiso 0.501(12) 1 calc GR . P B 2 H22H H 0.6320 0.3849 -0.1915 0.140 Uiso 0.501(12) 1 calc GR . P B 2 H22I H 0.6112 0.2874 -0.1866 0.140 Uiso 0.501(12) 1 calc GR . P B 2 C23' C 0.6754(5) 0.5768(5) 0.1639(4) 0.0239(14) Uani 1 1 d . . . . . C24' C 0.6588(5) 0.4898(5) 0.1948(4) 0.0219(14) Uani 1 1 d . . . . . C25' C 0.6392(5) 0.6495(5) 0.2072(5) 0.0297(16) Uani 1 1 d . . . . . C26' C 0.5058(7) 0.7586(7) 0.2445(7) 0.062(3) Uani 1 1 d . . . . . H26D H 0.5317 0.8154 0.2177 0.094 Uiso 1 1 calc GR . . . . H26E H 0.5220 0.7281 0.3020 0.094 Uiso 1 1 calc GR . . . . H26F H 0.4358 0.7771 0.2443 0.094 Uiso 1 1 calc GR . . . . C27' C 0.6005(5) 0.4605(5) 0.2766(4) 0.0276(15) Uani 1 1 d . . . . . C28' C 0.5058(5) 0.3564(5) 0.3632(4) 0.0254(15) Uani 1 1 d . . . . . H28D H 0.4802 0.3052 0.3624 0.038 Uiso 1 1 calc GR . . . . H28E H 0.4531 0.4124 0.3627 0.038 Uiso 1 1 calc GR . . . . H28F H 0.5379 0.3345 0.4136 0.038 Uiso 1 1 calc GR . . . . C29 C 0.8306(8) 0.5862(6) 0.6467(6) 0.090(3) Uani 1 1 d . U . . . C30 C 0.9124(7) 0.5495(8) 0.6020(6) 0.114(3) Uani 1 1 d G U . . . H30 H 0.9603 0.5847 0.5771 0.137 Uiso 1 1 calc R . . . . C31 C 0.9241(7) 0.4615(9) 0.5936(7) 0.135(4) Uani 1 1 d G U . . . H31 H 0.9800 0.4365 0.5629 0.162 Uiso 1 1 calc R . . . . C32 C 0.8541(10) 0.4101(6) 0.6300(7) 0.129(4) Uani 1 1 d G U . . . H32 H 0.8621 0.3499 0.6242 0.154 Uiso 1 1 calc R . . . . C33 C 0.7722(8) 0.4467(8) 0.6747(7) 0.127(4) Uani 1 1 d G U . . . H33 H 0.7244 0.4116 0.6996 0.152 Uiso 1 1 calc R . . . . C34 C 0.7605(6) 0.5348(8) 0.6831(6) 0.100(3) Uani 1 1 d G U . . . H34 H 0.7046 0.5598 0.7138 0.119 Uiso 1 1 calc R . . . . C35 C 0.8157(12) 0.6739(11) 0.6561(10) 0.109(4) Uani 1 1 d . U . . . H35A H 0.8663 0.6721 0.6861 0.164 Uiso 1 1 calc GR . . . . H35B H 0.7531 0.6880 0.6875 0.164 Uiso 1 1 calc GR . . . . H35C H 0.8171 0.7235 0.6012 0.164 Uiso 1 1 calc GR . . . . 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 S1 0.0182(8) 0.0266(9) 0.0266(9) -0.0057(7) -0.0077(7) 0.0038(7) S2 0.0188(8) 0.0312(10) 0.0308(9) -0.0029(8) -0.0110(7) -0.0078(7) P1 0.0126(7) 0.0202(9) 0.0170(8) -0.0057(7) -0.0028(6) -0.0025(6) P2 0.0129(7) 0.0243(9) 0.0181(8) -0.0059(7) -0.0021(6) -0.0024(6) O1 0.021(2) 0.021(2) 0.020(2) -0.0053(19) -0.0035(18) -0.0029(19) O2 0.033(3) 0.024(3) 0.031(3) -0.012(2) -0.006(2) -0.010(2) O3 0.055(4) 0.046(3) 0.025(3) -0.016(3) -0.011(3) -0.015(3) O4 0.030(3) 0.040(3) 0.061(4) -0.038(3) -0.017(3) 0.013(2) N1 0.013(2) 0.018(3) 0.016(3) -0.004(2) -0.001(2) -0.001(2) N2 0.013(2) 0.021(3) 0.016(3) -0.006(2) -0.003(2) -0.003(2) N3 0.013(2) 0.024(3) 0.021(3) -0.002(2) -0.003(2) -0.003(2) N4 0.016(3) 0.020(3) 0.019(3) -0.006(2) -0.003(2) -0.005(2) C1 0.012(3) 0.021(3) 0.015(3) -0.003(3) -0.004(2) 0.001(2) C2 0.013(3) 0.027(4) 0.020(3) -0.007(3) -0.005(2) -0.004(3) C3 0.016(3) 0.022(3) 0.021(3) -0.006(3) -0.008(3) -0.002(3) C4 0.014(3) 0.027(4) 0.022(3) -0.007(3) 0.000(3) -0.002(3) C5 0.029(5) 0.035(5) 0.027(4) -0.018(4) -0.002(4) -0.006(4) C5S 0.029(5) 0.036(5) 0.028(5) -0.019(5) -0.002(5) -0.007(5) C6 0.031(4) 0.037(4) 0.029(4) -0.020(4) -0.001(3) -0.005(4) C6S 0.030(5) 0.035(5) 0.028(5) -0.021(5) -0.003(4) -0.005(5) C7 0.052(6) 0.054(6) 0.047(6) -0.034(5) -0.005(5) -0.003(5) C7S 0.047(9) 0.049(9) 0.041(8) -0.031(7) -0.005(8) -0.001(8) C8 0.019(3) 0.030(4) 0.013(3) -0.002(3) 0.000(2) -0.007(3) C9 0.049(5) 0.051(5) 0.024(4) -0.013(4) 0.005(3) -0.027(4) C10 0.062(6) 0.065(6) 0.030(4) -0.024(4) -0.002(4) -0.005(5) C11 0.111(7) 0.112(7) 0.099(6) -0.045(5) -0.013(5) -0.018(5) C12 0.013(3) 0.022(3) 0.020(3) -0.003(3) -0.003(2) -0.007(2) C13 0.012(3) 0.022(3) 0.027(3) -0.009(3) -0.005(3) -0.003(3) C14 0.017(3) 0.018(3) 0.024(3) -0.001(3) -0.006(3) -0.003(3) C15 0.013(3) 0.028(4) 0.027(4) -0.004(3) 0.002(3) -0.004(3) C16 0.025(4) 0.032(4) 0.038(4) -0.010(3) 0.007(3) 0.006(3) C17 0.057(6) 0.053(6) 0.057(6) -0.014(5) 0.006(5) -0.011(5) C18 0.073(7) 0.057(7) 0.070(7) -0.028(6) -0.001(6) 0.012(6) C19 0.019(3) 0.027(4) 0.013(3) 0.001(3) -0.005(2) -0.006(3) C20 0.042(4) 0.028(4) 0.029(4) -0.011(3) -0.008(3) 0.002(3) C21 0.031(4) 0.055(5) 0.033(4) -0.023(4) -0.011(3) 0.011(4) C22 0.083(8) 0.066(7) 0.060(7) -0.042(6) -0.014(6) 0.013(6) C23 0.013(3) 0.021(3) 0.019(3) -0.005(3) -0.006(2) 0.000(2) C24 0.012(3) 0.026(3) 0.017(3) -0.008(3) -0.002(2) 0.001(3) C25 0.011(3) 0.018(3) 0.024(3) -0.005(3) -0.007(2) 0.000(2) C26 0.058(5) 0.026(4) 0.042(5) -0.005(4) -0.006(4) -0.024(4) C27 0.021(3) 0.036(4) 0.026(4) -0.014(3) 0.004(3) -0.010(3) C28 0.065(7) 0.063(7) 0.120(10) -0.075(7) -0.032(7) 0.027(5) S1' 0.0144(7) 0.0279(9) 0.0262(9) -0.0038(7) -0.0041(6) 0.0005(7) S2' 0.0349(10) 0.0601(14) 0.0241(10) -0.0053(9) -0.0129(8) -0.0189(10) P1' 0.0158(7) 0.0192(8) 0.0225(8) -0.0028(7) -0.0045(6) -0.0029(7) P2' 0.0161(8) 0.0211(9) 0.0209(8) -0.0052(7) -0.0030(6) -0.0046(7) O1' 0.045(3) 0.052(4) 0.057(4) -0.036(3) 0.002(3) -0.012(3) O2' 0.036(3) 0.037(3) 0.045(3) -0.016(3) -0.001(3) 0.007(3) O3' 0.051(3) 0.035(3) 0.031(3) -0.015(2) 0.008(3) -0.013(3) O4' 0.017(2) 0.031(3) 0.024(2) -0.012(2) 0.0043(18) -0.012(2) N1' 0.013(2) 0.023(3) 0.016(3) -0.004(2) -0.002(2) -0.003(2) N2' 0.014(2) 0.015(3) 0.017(3) -0.004(2) -0.003(2) 0.002(2) N3' 0.018(3) 0.030(3) 0.019(3) 0.002(2) -0.005(2) -0.003(2) N4' 0.024(3) 0.039(4) 0.022(3) -0.006(3) -0.008(2) -0.012(3) C1' 0.016(3) 0.016(3) 0.018(3) -0.003(3) -0.002(2) -0.004(2) C2' 0.012(3) 0.022(3) 0.013(3) 0.000(3) -0.002(2) -0.002(2) C3' 0.017(3) 0.020(3) 0.013(3) -0.004(2) -0.003(2) -0.002(3) C4' 0.018(3) 0.020(3) 0.021(3) -0.005(3) -0.003(3) -0.002(3) C5' 0.031(4) 0.022(4) 0.022(3) -0.005(3) -0.001(3) -0.011(3) C6' 0.039(4) 0.028(4) 0.041(4) -0.016(3) -0.004(4) -0.009(3) C7' 0.076(7) 0.048(6) 0.054(6) -0.029(5) -0.001(5) -0.021(5) C8' 0.020(3) 0.026(4) 0.021(3) -0.006(3) -0.003(3) -0.009(3) C9' 0.030(4) 0.039(4) 0.028(4) -0.015(3) -0.010(3) -0.012(3) C10' 0.040(4) 0.035(4) 0.031(4) -0.017(3) 0.000(3) -0.011(3) C11' 0.055(5) 0.035(5) 0.049(5) -0.022(4) -0.005(4) -0.008(4) C12' 0.015(3) 0.021(3) 0.021(3) 0.001(3) -0.005(3) -0.009(3) C13' 0.016(3) 0.028(4) 0.021(3) -0.007(3) -0.003(3) -0.006(3) C14' 0.024(3) 0.037(4) 0.025(4) -0.001(3) -0.008(3) -0.013(3) C15' 0.015(3) 0.030(4) 0.028(4) 0.004(3) -0.005(3) -0.002(3) C16' 0.027(4) 0.031(4) 0.037(4) -0.006(3) -0.008(3) 0.000(3) C17' 0.055(6) 0.051(6) 0.045(5) -0.013(4) -0.016(4) 0.005(5) C18' 0.094(10) 0.094(10) 0.082(9) -0.049(8) -0.029(8) 0.041(8) C19' 0.050(5) 0.045(5) 0.039(4) -0.015(4) -0.009(4) -0.026(4) C20' 0.105(5) 0.088(5) 0.093(5) -0.041(4) 0.005(4) -0.030(4) C20S 0.105(5) 0.088(5) 0.093(5) -0.041(4) 0.005(4) -0.030(4) C21' 0.105(5) 0.089(5) 0.093(5) -0.041(4) 0.005(4) -0.030(4) C21S 0.105(5) 0.089(5) 0.093(5) -0.041(4) 0.005(4) -0.030(4) C22' 0.106(5) 0.090(5) 0.095(5) -0.039(4) 0.006(4) -0.028(4) C22S 0.105(5) 0.089(5) 0.093(5) -0.040(4) 0.004(4) -0.030(4) C23' 0.018(3) 0.027(4) 0.024(3) -0.009(3) -0.002(3) 0.000(3) C24' 0.019(3) 0.027(4) 0.016(3) -0.004(3) -0.004(3) -0.002(3) C25' 0.022(3) 0.022(4) 0.037(4) -0.008(3) 0.006(3) -0.003(3) C26' 0.060(6) 0.039(5) 0.068(7) -0.026(5) 0.015(5) 0.013(5) C27' 0.023(3) 0.027(4) 0.029(4) -0.008(3) 0.002(3) -0.005(3) C28' 0.020(3) 0.029(4) 0.022(3) -0.004(3) 0.001(3) -0.007(3) C29 0.096(5) 0.116(6) 0.088(5) -0.049(4) -0.042(4) -0.025(5) C30 0.107(6) 0.131(6) 0.101(5) -0.043(5) -0.021(5) -0.010(5) C31 0.123(6) 0.143(6) 0.118(6) -0.033(5) -0.022(5) -0.008(5) C32 0.125(6) 0.140(6) 0.116(6) -0.038(5) -0.029(5) -0.022(5) C33 0.120(6) 0.143(6) 0.114(6) -0.025(5) -0.040(5) -0.030(5) C34 0.097(5) 0.125(6) 0.095(5) -0.033(5) -0.046(4) -0.034(5) C35 0.121(8) 0.107(8) 0.123(8) -0.051(6) -0.061(7) -0.012(7) 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C1 P1 C13 94.0(3) C1 P1 C23 94.0(3) C13 P1 C23 92.7(3) C2 P2 C24 93.0(3) C12 P2 C2 95.0(3) C12 P2 C24 92.7(3) C25 O2 C26 114.7(6) C27 O4 C28 115.7(6) C1 N1 C4 126.1(5) C3 N1 C1 109.5(5) C3 N1 C4 124.1(5) C2 N2 C8 126.0(5) C3 N2 C2 108.6(5) C3 N2 C8 125.3(5) C12 N3 C15 126.1(6) C14 N3 C12 109.6(5) C14 N3 C15 124.0(5) C13 N4 C19 124.9(5) C14 N4 C13 110.0(5) C14 N4 C19 125.1(5) N1 C1 P1 129.2(5) C2 C1 P1 122.7(5) C2 C1 N1 107.3(5) N2 C2 P2 128.2(5) C1 C2 P2 123.3(5) C1 C2 N2 108.1(5) N1 C3 S1 126.8(5) N2 C3 S1 126.7(5) N2 C3 N1 106.5(5) N1 C4 H4AA 109.8 N1 C4 H4AB 109.8 N1 C4 H4BC 108.6 N1 C4 H4BD 108.6 N1 C4 C5 109.6(6) H4AA C4 H4AB 108.2 H4BC C4 H4BD 107.6 C5 C4 H4AA 109.8 C5 C4 H4AB 109.8 C5S C4 N1 114.5(16) C5S C4 H4BC 108.6 C5S C4 H4BD 108.6 C4 C5 H5A 109.2 C4 C5 H5B 109.2 H5A C5 H5B 107.9 C6 C5 C4 111.9(10) C6 C5 H5A 109.2 C6 C5 H5B 109.2 C4 C5S H5SA 108.4 C4 C5S H5SB 108.4 C4 C5S C6S 116(3) H5SA C5S H5SB 107.5 C6S C5S H5SA 108.4 C6S C5S H5SB 108.4 C5 C6 H6A 109.0 C5 C6 H6B 109.0 C5 C6 C7 112.9(10) H6A C6 H6B 107.8 C7 C6 H6A 109.0 C7 C6 H6B 109.0 C5S C6S H6SA 108.7 C5S C6S H6SB 108.7 C5S C6S C7S 114(3) H6SA C6S H6SB 107.6 C7S C6S H6SA 108.7 C7S C6S H6SB 108.7 C6 C7 H7A 109.5 C6 C7 H7B 109.5 C6 C7 H7C 109.5 H7A C7 H7B 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C6S C7S H7SA 109.5 C6S C7S H7SB 109.5 C6S C7S H7SC 109.5 H7SA C7S H7SB 109.5 H7SA C7S H7SC 109.5 H7SB C7S H7SC 109.5 N2 C8 H8A 109.2 N2 C8 H8B 109.2 N2 C8 C9 112.1(6) H8A C8 H8B 107.9 C9 C8 H8A 109.2 C9 C8 H8B 109.2 C8 C9 H9A 108.9 C8 C9 H9B 108.9 C8 C9 C10 113.4(7) H9A C9 H9B 107.7 C10 C9 H9A 108.9 C10 C9 H9B 108.9 C9 C10 H10A 108.5 C9 C10 H10B 108.5 H10A C10 H10B 107.5 C11 C10 C9 115.0(10) C11 C10 H10A 108.5 C11 C10 H10B 108.5 C10 C11 H11A 109.5 C10 C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11B 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 N3 C12 P2 130.0(5) C13 C12 P2 122.2(5) C13 C12 N3 107.7(5) N4 C13 P1 129.3(5) C12 C13 P1 123.6(5) C12 C13 N4 106.9(5) N3 C14 S2 127.1(5) N4 C14 S2 127.1(5) N4 C14 N3 105.8(5) N3 C15 H15A 109.2 N3 C15 H15B 109.2 N3 C15 C16 111.9(6) H15A C15 H15B 107.9 C16 C15 H15A 109.2 C16 C15 H15B 109.2 C15 C16 H16A 108.4 C15 C16 H16B 108.4 H16A C16 H16B 107.5 C17 C16 C15 115.4(7) C17 C16 H16A 108.4 C17 C16 H16B 108.4 C16 C17 H17A 109.3 C16 C17 H17B 109.3 C16 C17 C18 111.6(8) H17A C17 H17B 108.0 C18 C17 H17A 109.3 C18 C17 H17B 109.3 C17 C18 H18A 109.5 C17 C18 H18B 109.5 C17 C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 N4 C19 H19A 109.1 N4 C19 H19B 109.1 N4 C19 C20 112.5(6) H19A C19 H19B 107.8 C20 C19 H19A 109.1 C20 C19 H19B 109.1 C19 C20 H20A 109.0 C19 C20 H20B 109.0 C19 C20 C21 112.7(6) H20A C20 H20B 107.8 C21 C20 H20A 109.0 C21 C20 H20B 109.0 C20 C21 H21A 108.9 C20 C21 H21B 108.9 H21A C21 H21B 107.7 C22 C21 C20 113.5(8) C22 C21 H21A 108.9 C22 C21 H21B 108.9 C21 C22 H22A 109.5 C21 C22 H22B 109.5 C21 C22 H22C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C24 C23 P1 122.2(5) C24 C23 C25 124.6(6) C25 C23 P1 112.9(4) C23 C24 P2 122.1(5) C23 C24 C27 124.9(6) C27 C24 P2 113.0(5) O1 C25 O2 124.5(6) O1 C25 C23 121.9(6) O2 C25 C23 113.5(5) O2 C26 H26A 109.5 O2 C26 H26B 109.5 O2 C26 H26C 109.5 H26A C26 H26B 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 O3 C27 O4 124.9(7) O3 C27 C24 123.4(7) O4 C27 C24 111.7(6) O4 C28 H28A 109.5 O4 C28 H28B 109.5 O4 C28 H28C 109.5 H28A C28 H28B 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C1' P1' C12' 95.3(3) C1' P1' C23' 92.9(3) C12' P1' C23' 92.5(3) C2' P2' C13' 93.1(3) C2' P2' C24' 93.8(3) C13' P2' C24' 94.4(3) C25' O2' C26' 114.8(7) C27' O4' C28' 115.3(5) C1' N1' C8' 127.8(5) C3' N1' C1' 108.6(5) C3' N1' C8' 123.5(5) C2' N2' C4' 125.8(5) C3' N2' C2' 109.2(5) C3' N2' C4' 125.0(5) C12' N3' C14' 109.8(6) C12' N3' C15' 127.4(6) C14' N3' C15' 122.8(6) C13' N4' C19' 126.1(6) C14' N4' C13' 109.9(6) C14' N4' C19' 123.7(6) N1' C1' P1' 129.8(5) C2' C1' P1' 123.0(5) C2' C1' N1' 107.2(5) N2' C2' P2' 128.7(5) C1' C2' P2' 123.0(5) C1' C2' N2' 108.2(5) N1' C3' S1' 126.3(5) N2' C3' S1' 126.9(5) N2' C3' N1' 106.7(5) N2' C4' H4'A 109.1 N2' C4' H4'B 109.1 N2' C4' C5' 112.6(5) H4'A C4' H4'B 107.8 C5' C4' H4'A 109.1 C5' C4' H4'B 109.1 C4' C5' H5'A 109.4 C4' C5' H5'B 109.4 H5'A C5' H5'B 108.0 C6' C5' C4' 111.2(6) C6' C5' H5'A 109.4 C6' C5' H5'B 109.4 C5' C6' H6'A 109.0 C5' C6' H6'B 109.0 C5' C6' C7' 113.1(7) H6'A C6' H6'B 107.8 C7' C6' H6'A 109.0 C7' C6' H6'B 109.0 C6' C7' H7'A 109.5 C6' C7' H7'B 109.5 C6' C7' H7'C 109.5 H7'A C7' H7'B 109.5 H7'A C7' H7'C 109.5 H7'B C7' H7'C 109.5 N1' C8' H8'A 109.1 N1' C8' H8'B 109.1 N1' C8' C9' 112.4(6) H8'A C8' H8'B 107.9 C9' C8' H8'A 109.1 C9' C8' H8'B 109.1 C8' C9' H9'A 108.7 C8' C9' H9'B 108.7 C8' C9' C10' 114.3(6) H9'A C9' H9'B 107.6 C10' C9' H9'A 108.7 C10' C9' H9'B 108.7 C9' C10' H10C 109.1 C9' C10' H10D 109.1 C9' C10' C11' 112.6(7) H10C C10' H10D 107.8 C11' C10' H10C 109.1 C11' C10' H10D 109.1 C10' C11' H11D 109.5 C10' C11' H11E 109.5 C10' C11' H11F 109.5 H11D C11' H11E 109.5 H11D C11' H11F 109.5 H11E C11' H11F 109.5 N3' C12' P1' 129.9(5) C13' C12' P1' 122.3(5) C13' C12' N3' 107.6(6) N4' C13' P2' 128.9(5) C12' C13' P2' 123.4(5) C12' C13' N4' 107.3(6) N3' C14' S2' 127.4(6) N4' C14' S2' 127.3(6) N4' C14' N3' 105.3(6) N3' C15' H15C 109.1 N3' C15' H15D 109.1 N3' C15' C16' 112.3(6) H15C C15' H15D 107.9 C16' C15' H15C 109.1 C16' C15' H15D 109.1 C15' C16' H16C 108.6 C15' C16' H16D 108.6 H16C C16' H16D 107.6 C17' C16' C15' 114.5(6) C17' C16' H16C 108.6 C17' C16' H16D 108.6 C16' C17' H17C 108.8 C16' C17' H17D 108.8 C16' C17' C18' 113.9(8) H17C C17' H17D 107.7 C18' C17' H17C 108.8 C18' C17' H17D 108.8 C17' C18' H18D 109.5 C17' C18' H18E 109.5 C17' C18' H18F 109.5 H18D C18' H18E 109.5 H18D C18' H18F 109.5 H18E C18' H18F 109.5 N4' C19' H19C 108.5 N4' C19' H19D 108.5 N4' C19' H19E 111.0 N4' C19' H19F 111.0 N4' C19' C20' 115.2(12) N4' C19' C20S 103.6(9) H19C C19' H19D 107.5 H19E C19' H19F 109.0 C20' C19' H19C 108.5 C20' C19' H19D 108.5 C20S C19' H19E 111.0 C20S C19' H19F 111.0 C19' C20' H20C 107.6 C19' C20' H20D 107.6 H20C C20' H20D 107.0 C21' C20' C19' 118.9(13) C21' C20' H20C 107.6 C21' C20' H20D 107.6 C19' C20S H20E 110.0 C19' C20S H20F 110.0 H20E C20S H20F 108.4 C21S C20S C19' 108.5(14) C21S C20S H20E 110.0 C21S C20S H20F 110.0 C20' C21' H21C 109.4 C20' C21' H21D 109.4 C20' C21' C22' 111.06(14) H21C C21' H21D 108.0 C22' C21' H21C 109.4 C22' C21' H21D 109.4 C20S C21S H21E 109.4 C20S C21S H21F 109.4 C20S C21S C22S 111.07(14) H21E C21S H21F 108.0 C22S C21S H21E 109.4 C22S C21S H21F 109.4 C21' C22' H22D 109.5 C21' C22' H22E 109.5 C21' C22' H22F 109.5 H22D C22' H22E 109.5 H22D C22' H22F 109.5 H22E C22' H22F 109.5 C21S C22S H22G 109.5 C21S C22S H22H 109.5 C21S C22S H22I 109.5 H22G C22S H22H 109.5 H22G C22S H22I 109.5 H22H C22S H22I 109.5 C24' C23' P1' 122.5(5) C24' C23' C25' 123.8(6) C25' C23' P1' 113.5(5) C23' C24' P2' 121.3(5) C23' C24' C27' 119.7(6) C27' C24' P2' 118.9(5) O1' C25' O2' 124.7(7) O1' C25' C23' 123.1(6) O2' C25' C23' 112.0(7) O2' C26' H26D 109.5 O2' C26' H26E 109.5 O2' C26' H26F 109.5 H26D C26' H26E 109.5 H26D C26' H26F 109.5 H26E C26' H26F 109.5 O3' C27' O4' 124.7(7) O3' C27' C24' 123.0(7) O4' C27' C24' 112.3(6) O4' C28' H28D 109.5 O4' C28' H28E 109.5 O4' C28' H28F 109.5 H28D C28' H28E 109.5 H28D C28' H28F 109.5 H28E C28' H28F 109.5 C30 C29 C34 120.0 C35 C29 C30 121.9(11) C35 C29 C34 118.1(11) C29 C30 H30 120.0 C31 C30 C29 120.0 C31 C30 H30 120.0 C30 C31 H31 120.0 C32 C31 C30 120.0 C32 C31 H31 120.0 C31 C32 H32 120.0 C31 C32 C33 120.0 C33 C32 H32 120.0 C32 C33 H33 120.0 C32 C33 C34 120.0 C34 C33 H33 120.0 C29 C34 H34 120.0 C33 C34 C29 120.0 C33 C34 H34 120.0 C29 C35 H35A 109.5 C29 C35 H35B 109.5 C29 C35 H35C 109.5 H35A C35 H35B 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C3 1.682(6) S2 C14 1.675(6) P1 C1 1.820(6) P1 C13 1.830(6) P1 C23 1.878(7) P2 C2 1.824(6) P2 C12 1.821(6) P2 C24 1.896(7) O1 C25 1.209(8) O2 C25 1.336(8) O2 C26 1.445(9) O3 C27 1.204(8) O4 C27 1.338(9) O4 C28 1.457(10) N1 C1 1.384(8) N1 C3 1.373(8) N1 C4 1.475(8) N2 C2 1.393(8) N2 C3 1.370(8) N2 C8 1.452(8) N3 C12 1.385(8) N3 C14 1.373(9) N3 C15 1.458(8) N4 C13 1.393(8) N4 C14 1.364(8) N4 C19 1.463(8) C1 C2 1.353(9) C4 H4AA 0.9900 C4 H4AB 0.9900 C4 H4BC 0.9900 C4 H4BD 0.9900 C4 C5 1.536(17) C4 C5S 1.44(4) C5 H5A 0.9900 C5 H5B 0.9900 C5 C6 1.502(11) C5S H5SA 0.9900 C5S H5SB 0.9900 C5S C6S 1.499(13) C6 H6A 0.9900 C6 H6B 0.9900 C6 C7 1.515(10) C6S H6SA 0.9900 C6S H6SB 0.9900 C6S C7S 1.507(12) C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C7S H7SA 0.9800 C7S H7SB 0.9800 C7S H7SC 0.9800 C8 H8A 0.9900 C8 H8B 0.9900 C8 C9 1.499(10) C9 H9A 0.9900 C9 H9B 0.9900 C9 C10 1.502(11) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.496(17) C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 C13 1.356(9) C15 H15A 0.9900 C15 H15B 0.9900 C15 C16 1.537(10) C16 H16A 0.9900 C16 H16B 0.9900 C16 C17 1.490(12) C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.550(14) C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 H19A 0.9900 C19 H19B 0.9900 C19 C20 1.509(10) C20 H20A 0.9900 C20 H20B 0.9900 C20 C21 1.516(11) C21 H21A 0.9900 C21 H21B 0.9900 C21 C22 1.499(12) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 C24 1.329(9) C23 C25 1.496(9) C24 C27 1.483(9) C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 S1' C3' 1.680(6) S2' C14' 1.672(7) P1' C1' 1.820(6) P1' C12' 1.826(7) P1' C23' 1.907(7) P2' C2' 1.827(6) P2' C13' 1.828(7) P2' C24' 1.885(7) O1' C25' 1.200(9) O2' C25' 1.327(9) O2' C26' 1.458(10) O3' C27' 1.221(9) O4' C27' 1.316(9) O4' C28' 1.450(8) N1' C1' 1.401(8) N1' C3' 1.375(8) N1' C8' 1.464(8) N2' C2' 1.384(7) N2' C3' 1.365(8) N2' C4' 1.450(8) N3' C12' 1.379(8) N3' C14' 1.380(9) N3' C15' 1.461(9) N4' C13' 1.388(8) N4' C14' 1.368(9) N4' C19' 1.460(9) C1' C2' 1.351(9) C4' H4'A 0.9900 C4' H4'B 0.9900 C4' C5' 1.519(9) C5' H5'A 0.9900 C5' H5'B 0.9900 C5' C6' 1.517(10) C6' H6'A 0.9900 C6' H6'B 0.9900 C6' C7' 1.523(11) C7' H7'A 0.9800 C7' H7'B 0.9800 C7' H7'C 0.9800 C8' H8'A 0.9900 C8' H8'B 0.9900 C8' C9' 1.514(9) C9' H9'A 0.9900 C9' H9'B 0.9900 C9' C10' 1.526(10) C10' H10C 0.9900 C10' H10D 0.9900 C10' C11' 1.538(11) C11' H11D 0.9800 C11' H11E 0.9800 C11' H11F 0.9800 C12' C13' 1.353(9) C15' H15C 0.9900 C15' H15D 0.9900 C15' C16' 1.526(10) C16' H16C 0.9900 C16' H16D 0.9900 C16' C17' 1.497(12) C17' H17C 0.9900 C17' H17D 0.9900 C17' C18' 1.503(14) C18' H18D 0.9800 C18' H18E 0.9800 C18' H18F 0.9800 C19' H19C 0.9900 C19' H19D 0.9900 C19' H19E 0.9900 C19' H19F 0.9900 C19' C20' 1.5399(13) C19' C20S 1.5402(13) C20' H20C 0.9900 C20' H20D 0.9900 C20' C21' 1.5399(13) C20S H20E 0.9900 C20S H20F 0.9900 C20S C21S 1.5400(13) C21' H21C 0.9900 C21' H21D 0.9900 C21' C22' 1.5403(13) C21S H21E 0.9900 C21S H21F 0.9900 C21S C22S 1.5402(13) C22' H22D 0.9800 C22' H22E 0.9800 C22' H22F 0.9800 C22S H22G 0.9800 C22S H22H 0.9800 C22S H22I 0.9800 C23' C24' 1.332(10) C23' C25' 1.505(10) C24' C27' 1.492(9) C26' H26D 0.9800 C26' H26E 0.9800 C26' H26F 0.9800 C28' H28D 0.9800 C28' H28E 0.9800 C28' H28F 0.9800 C29 C30 1.3900 C29 C34 1.3900 C29 C35 1.384(16) C30 H30 0.9500 C30 C31 1.3900 C31 H31 0.9500 C31 C32 1.3900 C32 H32 0.9500 C32 C33 1.3900 C33 H33 0.9500 C33 C34 1.3900 C34 H34 0.9500 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.4413(14) 2 0.5587(14)