#------------------------------------------------------------------------------ #$Date: 2021-09-30 04:04:22 +0300 (Thu, 30 Sep 2021) $ #$Revision: 269394 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/83/7158326.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_7158326 loop_ _publ_author_name 'Shen, Jinhui' 'Yu, Aimin' 'Meng, Xiangtai' _publ_section_title ; Stereoselective [4+3] annulation of azadienes and ethyl 4-bromo-3-oxobutanoate: construction of benzindeno-fused azepine derivatives ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB01749G _journal_year 2021 _chemical_formula_moiety '2(C29 H29 N O5 S)' _chemical_formula_sum 'C58 H58 N2 O10 S2' _chemical_formula_weight 1007.18 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2021-08-03 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-09-07 deposited with the CCDC. 2021-09-29 downloaded from the CCDC. ; _cell_angle_alpha 81.9160(10) _cell_angle_beta 82.2550(10) _cell_angle_gamma 78.7780(10) _cell_formula_units_Z 2 _cell_length_a 11.71540(10) _cell_length_b 12.19970(10) _cell_length_c 18.5760(2) _cell_measurement_reflns_used 15397 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 68.0440 _cell_measurement_theta_min 2.4230 _cell_volume 2562.51(4) _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.3 (Bourhis et al., 2015)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_device_type 'XtaLAB Pro II AFC12 (RINC): Kappa single' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_unetI/netI 0.0229 _diffrn_reflns_Laue_measured_fraction_full 0.962 _diffrn_reflns_Laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 24249 _diffrn_reflns_point_group_measured_fraction_full 0.962 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.212 _diffrn_reflns_theta_min 2.417 _exptl_absorpt_coefficient_mu 1.450 _exptl_crystal_density_diffrn 1.305 _exptl_crystal_description block _exptl_crystal_F_000 1064 _refine_diff_density_max 0.220 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.031 _refine_ls_extinction_coef 0.00200(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 712 _refine_ls_number_reflns 8960 _refine_ls_number_restraints 50 _refine_ls_restrained_S_all 1.110 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0397 _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^)+(0.0571P)^2^+0.4334P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1099 _refine_ls_wR_factor_ref 0.1133 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7774 _reflns_number_total 8960 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob01749g2.cif _cod_data_source_block 1 _cod_database_code 7158326 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. 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, All O(H) groups 2. Restrained distances C3-C2 1.45 with sigma of 0.02 H01I-C01I 1.45 with sigma of 0.02 3. Rigid bond restraints C2, C7, C3, C6, O00N, O6 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O00E, C1, C4, C5 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C01U, C01V with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005 4. Uiso/Uaniso restraints and constraints C7 \\sim O6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A C3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A C2 \\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A 5. Rigid body (RIGU) restrains O00N, C6, C7, C012 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O6, C3, C2, C012 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(H1BC)=Sof(H1BD)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=1-FVAR(1) Sof(H1AA)=Sof(H1AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1) Sof(O6)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=1-FVAR(2) Sof(O00N)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(2) 7.a Ternary CH refined with riding coordinates: C00I(H00I), C00J(H00J), C00L(H00L), C00R(H00R), C00X(H00X), C013(H013) 7.b Secondary CH2 refined with riding coordinates: C00Q(H00A,H00B), C01F(H01A,H01B), C6(H6A,H6B), C1(H1BC,H1BD), C1(H1AA,H1AB), C3(H3A,H3B) 7.c Aromatic/amide H refined with riding coordinates: C00S(H00S), C00T(H00T), C00V(H00V), C00W(H00W), C00Y(H00Y), C014(H014), C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01N), C01C(H01R), C01D(H01D), C01G(H01G), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01U), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01Z), C01S(H01S), C01T(H01T), C01V(H01V) 7.d Idealised Me refined as rotating group: C01N(H01W,H01X,H01Y), C01Y(H01F,H01H,H01M), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C) 7.e Idealised tetrahedral OH refined as rotating group: O003(H003), O008(H008) ; _shelx_res_file ; TITL 20210801-mxt-1_auto_a.res in P-1 1.res created by SHELXL-2018/3 at 21:59:16 on 03-Aug-2021 REM Old TITL 20210801-mxt-1_auto_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.196, Rweak 0.012, Alpha 0.054, Orientation as input REM Formula found by SHELXT: C56 Cl2 N6 O7 CELL 1.54184 11.7154 12.1997 18.576 81.916 82.255 78.778 ZERR 2 0.0001 0.0001 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H N O S UNIT 116 116 4 20 4 SIMU 0.04 0.08 1.7 C7 O6 SIMU 0.04 0.08 1.7 C3 SIMU 0.04 0.08 1.7 C2 C7 DELU C2 C7 C3 C6 O00N O6 DELU O00E C1 C4 C5 DFIX 1.45 C3 C2 RIGU O00N C6 C7 C012 RIGU O6 C3 C2 C012 DFIX 1.45 H01I C01I DELU 0.0005 0.0005 C01U C01V L.S. 100 PLAN 5 CONF BOND $H list 4 MORE -1 fmap 2 acta OMIT 3 1 1 OMIT 4 3 0 OMIT 1 0 1 OMIT 2 1 0 OMIT 1 -1 5 OMIT 4 -1 1 OMIT 0 -5 1 OMIT 0 -4 5 OMIT 1 1 0 OMIT 4 -1 2 OMIT 3 0 1 OMIT 0 4 6 OMIT -3 4 1 OMIT 0 0 2 OMIT 0 1 4 OMIT 4 1 0 OMIT -2 -4 5 OMIT 6 4 0 OMIT 2 0 0 OMIT 4 2 5 OMIT 0 -4 7 OMIT -1 -2 1 OMIT 1 0 6 OMIT 3 1 0 OMIT 4 0 2 OMIT -2 3 3 OMIT 3 -2 2 OMIT 1 -1 1 OMIT 6 1 1 OMIT 0 0 7 OMIT 0 -2 1 OMIT 3 0 5 OMIT -2 4 6 OMIT -5 2 5 OMIT 1 -4 2 OMIT 1 5 6 OMIT -1 1 0 OMIT -1 4 6 OMIT 3 -1 2 OMIT 1 2 7 OMIT -3 1 6 OMIT -2 -6 5 OMIT 4 0 1 OMIT 7 0 2 OMIT 7 3 6 OMIT 2 0 1 OMIT -2 -4 8 OMIT -1 -1 5 OMIT 3 0 0 OMIT 4 2 1 OMIT 0 1 2 OMIT 1 1 2 OMIT 2 3 3 OMIT 2 1 2 OMIT 2 0 3 OMIT 2 4 5 OMIT -1 -3 3 OMIT 3 0 3 OMIT -1 -1 2 OMIT -5 -4 2 OMIT -1 -2 2 OMIT 0 -1 2 OMIT -1 -2 11 OMIT 4 0 3 OMIT 2 3 2 OMIT -1 1 5 OMIT 3 1 4 OMIT -2 -2 1 OMIT 5 5 8 OMIT 0 3 5 OMIT -3 1 1 OMIT 2 4 1 OMIT -3 2 3 OMIT 3 2 8 OMIT 2 3 4 OMIT 0 5 4 OMIT 4 1 3 OMIT 1 1 8 OMIT 4 4 2 OMIT 8 2 7 REM REM REM WGHT 0.057100 0.433400 EXTI 0.002005 FVAR 0.53823 0.38815 0.75256 S01 5 1.043742 0.080561 0.641535 11.00000 0.03835 0.04914 = 0.05671 0.00746 -0.00520 -0.00374 S02 5 -0.061443 0.524883 0.841051 11.00000 0.04131 0.08635 = 0.06325 0.00793 -0.00050 0.00375 O003 4 0.692673 0.357511 0.697597 11.00000 0.04406 0.06713 = 0.06196 -0.01624 0.00764 -0.00247 AFIX 147 H003 2 0.627782 0.349184 0.717888 11.00000 -1.50000 AFIX 0 O004 4 1.113107 0.053212 0.575237 11.00000 0.05047 0.05180 = 0.07702 0.00177 0.01393 0.00156 O005 4 0.518993 0.299118 0.610097 11.00000 0.03537 0.07492 = 0.09304 -0.00494 0.00470 -0.00452 O006 4 1.098778 0.077942 0.705880 11.00000 0.05748 0.07965 = 0.07538 0.01734 -0.02827 -0.01494 N007 3 0.968791 0.207107 0.623319 11.00000 0.03480 0.04746 = 0.04324 0.00230 -0.00062 -0.00397 O008 4 0.279551 0.343759 0.689990 11.00000 0.04897 0.13376 = 0.05775 -0.02889 0.00720 -0.02087 AFIX 147 H008 2 0.346800 0.353866 0.676984 11.00000 -1.50000 AFIX 0 O009 4 -0.114601 0.486203 0.911242 11.00000 0.05594 0.09327 = 0.07208 -0.00353 0.01943 -0.00666 O00A 4 0.473558 0.341893 0.781982 11.00000 0.04160 0.10769 = 0.09901 -0.02988 0.01927 -0.01857 N00B 3 0.022958 0.414297 0.810381 11.00000 0.03700 0.08176 = 0.04817 0.00717 0.00311 -0.00427 C00C 1 0.882912 0.318582 0.516366 11.00000 0.03427 0.04061 = 0.04522 -0.00216 -0.00346 -0.00763 C00D 1 1.083804 0.303294 0.514969 11.00000 0.03396 0.04138 = 0.04662 -0.00461 -0.00082 -0.00915 O00E 4 0.586116 0.114413 0.618459 11.00000 0.05080 0.06783 = 0.15380 0.01306 -0.01876 -0.02568 C00F 1 1.054543 0.372889 0.451048 11.00000 0.03884 0.04198 = 0.04760 -0.00315 -0.00114 -0.01051 C00G 1 0.975389 0.268732 0.552378 11.00000 0.03533 0.03874 = 0.04332 -0.00205 -0.00164 -0.00759 O00H 4 -0.133078 0.580355 0.785979 11.00000 0.06143 0.11636 = 0.09688 0.01485 -0.02682 0.01459 C00I 1 0.727316 0.230516 0.601662 11.00000 0.03196 0.04643 = 0.05291 -0.00351 -0.00026 -0.00752 AFIX 13 H00I 2 0.773525 0.157684 0.590446 11.00000 -1.20000 AFIX 0 C00J 1 0.753662 0.319543 0.537351 11.00000 0.03345 0.04361 = 0.04876 -0.00282 -0.00194 -0.00563 AFIX 13 H00J 2 0.719178 0.393443 0.552968 11.00000 -1.20000 AFIX 0 C10 1 0.925239 0.387636 0.447790 11.00000 0.03906 0.04965 = 0.04640 0.00308 -0.00442 -0.01023 C00L 1 0.755763 0.252632 0.676456 11.00000 0.03789 0.05219 = 0.04756 -0.00074 0.00320 -0.00846 AFIX 13 H00L 2 0.734295 0.192306 0.713452 11.00000 -1.20000 AFIX 0 C00M 1 0.698053 0.309117 0.469739 11.00000 0.02988 0.05488 = 0.05176 0.00023 -0.00184 -0.00984 PART 3 O00N 4 0.403080 0.500555 0.831276 31.00000 0.05281 0.09212 = 0.08642 -0.02355 -0.00267 -0.02073 PART 0 C00O 1 0.599088 0.221064 0.610200 11.00000 0.03795 0.06129 = 0.05657 0.00251 -0.00168 -0.01288 C00P 1 0.939263 -0.008192 0.664025 11.00000 0.04850 0.04416 = 0.05185 0.00601 -0.00453 -0.00435 C00Q 1 0.883855 0.258747 0.679607 11.00000 0.04063 0.05631 = 0.04548 -0.00502 -0.00004 -0.00726 AFIX 23 H00A 2 0.890493 0.337355 0.676382 11.00000 -1.20000 H00B 2 0.905473 0.223045 0.727085 11.00000 -1.20000 AFIX 0 C00R 1 0.266678 0.386417 0.816766 11.00000 0.03560 0.07684 = 0.04893 -0.00773 0.00203 -0.00735 AFIX 13 H00R 2 0.219525 0.437903 0.849893 11.00000 -1.20000 AFIX 0 C00S 1 1.196528 0.282678 0.533934 11.00000 0.03817 0.05337 = 0.05695 -0.00206 -0.00694 -0.00962 AFIX 43 H00S 2 1.215274 0.238289 0.577149 11.00000 -1.20000 AFIX 0 C00T 1 1.253630 0.394845 0.422416 11.00000 0.04302 0.05487 = 0.06722 -0.00553 0.00880 -0.02012 AFIX 43 H00T 2 1.312142 0.423790 0.390920 11.00000 -1.20000 AFIX 0 C00U 1 0.034700 0.305458 0.850380 11.00000 0.03667 0.07913 = 0.04501 -0.00165 -0.00123 -0.00963 C00V 1 0.903173 -0.055897 0.609565 11.00000 0.06109 0.05009 = 0.05295 -0.00462 0.00269 -0.00782 AFIX 43 H00V 2 0.937360 -0.045325 0.561522 11.00000 -1.20000 AFIX 0 C00W 1 1.140357 0.417514 0.403995 11.00000 0.04656 0.04787 = 0.05320 0.00080 0.00177 -0.01446 AFIX 43 H00W 2 1.122101 0.461995 0.360721 11.00000 -1.20000 AFIX 0 C00X 1 0.259426 0.265507 0.850459 11.00000 0.03424 0.07444 = 0.05458 -0.00735 0.00138 -0.00392 AFIX 13 H00X 2 0.306839 0.214934 0.816852 11.00000 -1.20000 AFIX 0 C00Y 1 1.281283 0.329810 0.486936 11.00000 0.03558 0.06065 = 0.07315 -0.00695 -0.00310 -0.01530 AFIX 43 H00Y 2 1.357609 0.317459 0.499027 11.00000 -1.20000 AFIX 0 C00Z 1 0.137596 0.238615 0.862205 11.00000 0.03871 0.07501 = 0.05267 -0.00253 -0.00147 -0.00945 C010 1 -0.061769 0.241287 0.871275 11.00000 0.04145 0.09087 = 0.04252 -0.00444 -0.00079 -0.01570 C011 1 0.311670 0.238525 0.923464 11.00000 0.03420 0.07110 = 0.06024 -0.00133 -0.00338 -0.00441 C012 1 0.392465 0.402871 0.810261 11.00000 0.03995 0.08413 = 0.05346 -0.00864 0.00029 -0.01207 C013 1 0.224548 0.420076 0.740024 11.00000 0.04225 0.08583 = 0.04618 -0.00298 0.00277 -0.01617 AFIX 13 H013 2 0.242191 0.494774 0.721098 11.00000 -1.20000 AFIX 0 C014 1 0.624249 0.400486 0.437536 11.00000 0.03654 0.06817 = 0.06290 0.00733 -0.00591 -0.00828 AFIX 43 H014 2 0.606194 0.467466 0.458545 11.00000 -1.20000 AFIX 0 C015 1 0.763444 -0.135865 0.698542 11.00000 0.05275 0.04693 = 0.07369 -0.00177 -0.00105 -0.00813 C016 1 0.815509 -0.119519 0.627677 11.00000 0.06555 0.04964 = 0.06806 -0.01045 -0.00716 -0.01003 AFIX 43 H016 2 0.791187 -0.151935 0.591308 11.00000 -1.20000 AFIX 0 C017 1 -0.180821 0.270350 0.865959 11.00000 0.04197 0.10994 = 0.05591 -0.00481 0.00015 -0.01769 AFIX 43 H017 2 -0.213992 0.343062 0.848188 11.00000 -1.20000 AFIX 0 C018 1 0.889193 -0.024495 0.735476 11.00000 0.06952 0.06095 = 0.05034 0.00421 -0.00773 -0.01909 AFIX 43 H018 2 0.914056 0.006941 0.772095 11.00000 -1.20000 AFIX 0 C019 1 0.801670 -0.088156 0.751754 11.00000 0.07208 0.06499 = 0.05671 0.00512 0.00526 -0.02184 AFIX 43 H019 2 0.767676 -0.099109 0.799817 11.00000 -1.20000 AFIX 0 C01A 1 0.722863 0.210481 0.437711 11.00000 0.06110 0.06692 = 0.06490 -0.01133 -0.01024 -0.01339 AFIX 43 H01N 2 0.772309 0.148566 0.458627 11.00000 -1.20000 AFIX 0 C01B 1 0.031624 0.616812 0.852125 11.00000 0.05487 0.06899 = 0.06646 0.00768 0.00436 0.00387 C01C 1 0.577446 0.392630 0.374525 11.00000 0.04573 0.11227 = 0.07013 0.02412 -0.01660 -0.02306 AFIX 43 H01R 2 0.528526 0.454441 0.353059 11.00000 -1.20000 AFIX 0 C01D 1 0.419222 0.169207 0.929716 11.00000 0.03875 0.08955 = 0.07310 -0.00535 -0.00268 0.00210 AFIX 43 H01D 2 0.460910 0.137856 0.889038 11.00000 -1.20000 AFIX 0 C01E 1 -0.012591 0.132303 0.896843 11.00000 0.05235 0.08834 = 0.05450 -0.00454 -0.00161 -0.02062 C01F 1 0.093290 0.423200 0.738874 11.00000 0.04179 0.10695 = 0.04617 0.00610 -0.00074 -0.01411 AFIX 23 H01A 2 0.061308 0.493078 0.710889 11.00000 -1.20000 H01B 2 0.084301 0.362137 0.713046 11.00000 -1.20000 AFIX 0 C01G 1 0.079935 0.606128 0.917329 11.00000 0.07079 0.07878 = 0.06526 0.00236 0.00236 -0.00633 AFIX 43 H01G 2 0.060162 0.552868 0.955571 11.00000 -1.20000 AFIX 0 C01H 1 0.117946 0.122168 0.890894 11.00000 0.05163 0.07862 = 0.07820 0.00467 -0.00791 -0.01191 C01I 1 0.252685 0.281683 0.985119 11.00000 0.05812 0.09366 = 0.06046 -0.00809 -0.00573 0.01396 AFIX 43 H01I 2 0.179946 0.328026 0.982259 11.00000 -1.20000 AFIX 0 C01J 1 0.465138 0.146251 0.996222 11.00000 0.04493 0.10456 = 0.08926 0.00839 -0.01740 0.00202 AFIX 43 H01J 2 0.538079 0.100458 0.999560 11.00000 -1.20000 AFIX 0 C01K 1 -0.249039 0.188697 0.887695 11.00000 0.04984 0.13327 = 0.07001 -0.01260 0.00026 -0.03337 AFIX 43 H01K 2 -0.329114 0.206859 0.884188 11.00000 -1.20000 AFIX 0 C01L 1 -0.081835 0.050883 0.918767 11.00000 0.07031 0.09325 = 0.06992 -0.00605 -0.00041 -0.03025 AFIX 43 H01L 2 -0.049042 -0.022229 0.935976 11.00000 -1.20000 AFIX 0 C01M 1 0.675378 0.202651 0.375279 11.00000 0.09433 0.10097 = 0.06974 -0.01981 -0.00998 -0.04005 AFIX 43 H01U 2 0.692310 0.135486 0.354494 11.00000 -1.20000 AFIX 0 C01N 1 0.667799 -0.205126 0.717579 11.00000 0.06783 0.07018 = 0.10492 -0.00638 0.00245 -0.02547 AFIX 137 H01W 2 0.629031 -0.204042 0.675063 11.00000 -1.50000 H01X 2 0.612217 -0.174180 0.755635 11.00000 -1.50000 H01Y 2 0.701236 -0.281266 0.734163 11.00000 -1.50000 AFIX 0 C01O 1 -0.201292 0.081309 0.914366 11.00000 0.06669 0.12351 = 0.07380 -0.01675 0.00596 -0.04731 AFIX 43 H01O 2 -0.249540 0.028348 0.929658 11.00000 -1.20000 AFIX 0 C01P 1 0.156932 0.673843 0.925779 11.00000 0.08364 0.08274 = 0.08915 -0.01668 -0.00129 -0.00771 AFIX 43 H01P 2 0.188508 0.665635 0.969965 11.00000 -1.20000 AFIX 0 C01Q 1 0.405055 0.189738 1.056723 11.00000 0.06899 0.11102 = 0.06880 0.00382 -0.02122 -0.01168 AFIX 43 H01Q 2 0.436050 0.173192 1.101336 11.00000 -1.20000 AFIX 0 C01R 1 0.602896 0.293877 0.343471 11.00000 0.08282 0.14679 = 0.06486 0.00247 -0.02483 -0.06091 AFIX 43 H01Z 2 0.571232 0.288646 0.301047 11.00000 -1.20000 AFIX 0 C01S 1 0.298663 0.257992 1.051164 11.00000 0.08142 0.10489 = 0.06051 -0.01104 -0.00816 0.00459 AFIX 43 H01S 2 0.257089 0.288598 1.092127 11.00000 -1.20000 AFIX 0 C01T 1 0.058158 0.699466 0.795976 11.00000 0.08180 0.08220 = 0.08036 0.01774 -0.00255 0.00146 AFIX 43 H01T 2 0.024255 0.709951 0.752471 11.00000 -1.20000 AFIX 0 C01U 1 0.188437 0.753264 0.870704 11.00000 0.08211 0.06691 = 0.12069 -0.01938 0.01269 -0.00387 C01V 1 0.137572 0.766459 0.806996 11.00000 0.09795 0.06715 = 0.10944 0.01352 0.01337 -0.01092 AFIX 43 H01V 2 0.156340 0.821684 0.769826 11.00000 -1.20000 AFIX 0 C01Y 1 0.277676 0.823584 0.879295 11.00000 0.12859 0.08930 = 0.20867 -0.04323 0.00437 -0.03333 AFIX 137 H01F 2 0.351886 0.775499 0.885293 11.00000 -1.50000 H01H 2 0.252309 0.862938 0.921519 11.00000 -1.50000 H01M 2 0.285483 0.876953 0.836525 11.00000 -1.50000 AFIX 0 H10A 2 0.910207 0.360661 0.404285 11.00000 0.05374 H10B 2 0.886572 0.470561 0.445683 11.00000 0.05909 H01C 2 0.144928 0.099186 0.937318 11.00000 0.07289 H01E 2 0.159080 0.064120 0.857548 11.00000 0.09474 PART 3 C6 1 0.520499 0.524595 0.830860 31.00000 0.06338 0.11413 = 0.11907 -0.03439 -0.01127 -0.03480 AFIX 23 H6A 2 0.576124 0.476845 0.799868 31.00000 -1.20000 H6B 2 0.522175 0.602420 0.811448 31.00000 -1.20000 AFIX 0 PART 0 C1 1 0.468214 0.089777 0.627055 11.00000 0.06614 0.10940 = 0.17804 0.01148 -0.01532 -0.04870 PART 2 AFIX 23 H1BC 2 0.466490 0.026742 0.600932 -21.00000 -1.20000 H1BD 2 0.414702 0.154515 0.607168 -21.00000 -1.20000 AFIX 23 PART 1 H1AA 2 0.410469 0.156806 0.635163 21.00000 -1.20000 H1AB 2 0.457985 0.032221 0.667875 21.00000 -1.20000 AFIX 0 PART 2 C4 1 0.432739 0.062343 0.705280 -21.00000 0.09006 0.12505 = 0.17093 -0.02517 0.03857 -0.02655 AFIX 137 H4A 2 0.489787 0.002412 0.725429 -21.00000 -1.50000 H4B 2 0.357925 0.039134 0.711651 -21.00000 -1.50000 H4C 2 0.427283 0.127527 0.729965 -21.00000 -1.50000 AFIX 0 PART 1 C5 1 0.457122 0.048533 0.555569 21.00000 0.10947 0.13691 = 0.26129 -0.01983 -0.06848 -0.05461 AFIX 137 H5A 2 0.464000 0.107819 0.516239 21.00000 -1.50000 H5B 2 0.382244 0.026479 0.558028 21.00000 -1.50000 H5C 2 0.518090 -0.014847 0.547123 21.00000 -1.50000 AFIX 0 PART 3 C7 1 0.552376 0.504013 0.904938 31.00000 0.10203 0.19171 = 0.16066 -0.04496 -0.05083 -0.03261 AFIX 137 H7A 2 0.623931 0.530615 0.906152 31.00000 -1.50000 H7B 2 0.563091 0.424740 0.920975 31.00000 -1.50000 H7C 2 0.491221 0.543053 0.936750 31.00000 -1.50000 AFIX 0 PART 4 O6 4 0.403860 0.464249 0.860360 -31.00000 0.05505 0.09000 = 0.07609 -0.00571 -0.01338 -0.02313 C3 1 0.527553 0.468584 0.865618 -31.00000 0.07537 0.11641 = 0.12420 -0.00086 -0.03713 -0.04643 AFIX 23 H3A 2 0.549730 0.433662 0.913128 -31.00000 -1.20000 H3B 2 0.578327 0.429167 0.828142 -31.00000 -1.20000 AFIX 0 C2 1 0.537153 0.583724 0.855673 -31.00000 0.15230 0.12159 = 0.36505 0.10190 -0.15180 -0.08244 AFIX 137 H2A 2 0.532973 0.612799 0.805132 -31.00000 -1.50000 H2B 2 0.610703 0.591596 0.869855 -31.00000 -1.50000 H2C 2 0.474295 0.624884 0.885285 -31.00000 -1.50000 AFIX 0 HKLF 4 REM 20210801-mxt-1_auto_a.res in P-1 REM wR2 = 0.1133, GooF = S = 1.071, Restrained GooF = 1.110 for all data REM R1 = 0.0397 for 7774 Fo > 4sig(Fo) and 0.0447 for all 8960 data REM 712 parameters refined using 50 restraints END WGHT 0.0571 0.4333 REM Highest difference peak 0.220, deepest hole -0.269, 1-sigma level 0.031 Q1 1 0.5899 0.1487 0.6666 11.00000 0.05 0.22 Q2 1 0.4446 0.1485 0.6691 11.00000 0.05 0.20 Q3 1 0.1047 0.7532 0.7659 11.00000 0.05 0.19 Q4 1 1.0462 0.0743 0.5800 11.00000 0.05 0.19 Q5 1 0.5592 0.5261 0.7683 11.00000 0.05 0.19 ; _shelx_res_checksum 44123 _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 S01 S 1.04374(3) 0.08056(3) 0.64154(2) 0.04997(12) Uani 1 1 d . . . . . S02 S -0.06144(4) 0.52488(5) 0.84105(3) 0.06784(15) Uani 1 1 d . . . . . O003 O 0.69267(10) 0.35751(10) 0.69760(7) 0.0592(3) Uani 1 1 d . . . . . H003 H 0.627782 0.349184 0.717888 0.089 Uiso 1 1 calc R U . . . O004 O 1.11311(10) 0.05321(10) 0.57524(7) 0.0641(3) Uani 1 1 d . . . . . O005 O 0.51899(10) 0.29912(12) 0.61010(8) 0.0701(4) Uani 1 1 d . . . . . O006 O 1.09878(12) 0.07794(12) 0.70588(8) 0.0711(4) Uani 1 1 d . . . . . N007 N 0.96879(10) 0.20711(10) 0.62332(7) 0.0434(3) Uani 1 1 d . . . . . O008 O 0.27955(12) 0.34376(15) 0.68999(8) 0.0790(4) Uani 1 1 d . . . . . H008 H 0.346800 0.353866 0.676984 0.119 Uiso 1 1 calc R U . . . O009 O -0.11460(12) 0.48620(13) 0.91124(8) 0.0778(4) Uani 1 1 d . . . . . O00A O 0.47356(11) 0.34189(14) 0.78198(9) 0.0829(4) Uani 1 1 d . . . . . N00B N 0.02296(12) 0.41430(14) 0.81038(8) 0.0587(4) Uani 1 1 d . . . . . C00C C 0.88291(12) 0.31858(12) 0.51637(8) 0.0403(3) Uani 1 1 d . . . . . C00D C 1.08380(12) 0.30329(12) 0.51497(8) 0.0407(3) Uani 1 1 d . . . . . O00E O 0.58612(12) 0.11441(12) 0.61846(11) 0.0906(5) Uani 1 1 d . U . . . C00F C 1.05454(13) 0.37289(12) 0.45105(8) 0.0429(3) Uani 1 1 d . . . . . C00G C 0.97539(12) 0.26873(12) 0.55238(8) 0.0395(3) Uani 1 1 d . . . . . O00H O -0.13308(14) 0.58035(16) 0.78598(10) 0.0967(5) Uani 1 1 d . . . . . C00I C 0.72732(13) 0.23052(13) 0.60166(9) 0.0443(3) Uani 1 1 d . . . . . H00I H 0.773525 0.157684 0.590446 0.053 Uiso 1 1 calc R U . . . C00J C 0.75366(12) 0.31954(12) 0.53735(8) 0.0426(3) Uani 1 1 d . . . . . H00J H 0.719178 0.393443 0.552968 0.051 Uiso 1 1 calc R U . . . C10 C 0.92524(14) 0.38764(14) 0.44779(9) 0.0456(3) Uani 1 1 d . . . . . C00L C 0.75576(13) 0.25263(13) 0.67646(9) 0.0471(4) Uani 1 1 d . . . . . H00L H 0.734295 0.192306 0.713452 0.056 Uiso 1 1 calc R U . . . C00M C 0.69805(13) 0.30912(13) 0.46974(9) 0.0461(4) Uani 1 1 d . . . . . O00N O 0.4031(3) 0.5006(4) 0.8313(3) 0.0753(10) Uani 0.753(10) 1 d . U P A 3 C00O C 0.59909(14) 0.22106(15) 0.61020(9) 0.0526(4) Uani 1 1 d . . . . . C00P C 0.93926(15) -0.00819(13) 0.66403(9) 0.0499(4) Uani 1 1 d . . . . . C00Q C 0.88385(13) 0.25875(14) 0.67961(9) 0.0482(4) Uani 1 1 d . . . . . H00A H 0.890493 0.337355 0.676382 0.058 Uiso 1 1 calc R U . . . H00B H 0.905473 0.223045 0.727085 0.058 Uiso 1 1 calc R U . . . C00R C 0.26668(14) 0.38642(16) 0.81677(9) 0.0548(4) Uani 1 1 d . . . . . H00R H 0.219525 0.437903 0.849893 0.066 Uiso 1 1 calc R U . . . C00S C 1.19653(13) 0.28268(14) 0.53393(9) 0.0496(4) Uani 1 1 d . . . . . H00S H 1.215274 0.238289 0.577149 0.059 Uiso 1 1 calc R U . . . C00T C 1.25363(15) 0.39485(14) 0.42242(10) 0.0550(4) Uani 1 1 d . . . . . H00T H 1.312142 0.423790 0.390920 0.066 Uiso 1 1 calc R U . . . C00U C 0.03470(14) 0.30546(16) 0.85038(9) 0.0546(4) Uani 1 1 d . . . . . C00V C 0.90317(16) -0.05590(14) 0.60956(10) 0.0560(4) Uani 1 1 d . . . . . H00V H 0.937360 -0.045325 0.561522 0.067 Uiso 1 1 calc R U . . . C00W C 1.14036(14) 0.41751(13) 0.40400(9) 0.0497(4) Uani 1 1 d . . . . . H00W H 1.122101 0.461995 0.360721 0.060 Uiso 1 1 calc R U . . . C00X C 0.25943(14) 0.26551(16) 0.85046(10) 0.0558(4) Uani 1 1 d . . . . . H00X H 0.306839 0.214934 0.816852 0.067 Uiso 1 1 calc R U . . . C00Y C 1.28128(15) 0.32981(15) 0.48694(11) 0.0559(4) Uani 1 1 d . . . . . H00Y H 1.357609 0.317459 0.499027 0.067 Uiso 1 1 calc R U . . . C00Z C 0.13760(14) 0.23862(16) 0.86221(10) 0.0564(4) Uani 1 1 d . . . . . C010 C -0.06177(15) 0.24129(18) 0.87128(9) 0.0584(4) Uani 1 1 d . . . . . C011 C 0.31167(14) 0.23852(16) 0.92346(10) 0.0567(4) Uani 1 1 d . . . . . C012 C 0.39246(15) 0.40287(18) 0.81026(10) 0.0595(4) Uani 1 1 d . . . . . C013 C 0.22455(15) 0.42008(18) 0.74002(9) 0.0586(4) Uani 1 1 d . . . . . H013 H 0.242191 0.494774 0.721098 0.070 Uiso 1 1 calc R U . . . C014 C 0.62425(14) 0.40049(16) 0.43754(10) 0.0575(4) Uani 1 1 d . . . . . H014 H 0.606194 0.467466 0.458545 0.069 Uiso 1 1 calc R U . . . C015 C 0.76344(16) -0.13586(14) 0.69854(11) 0.0590(4) Uani 1 1 d . . . . . C016 C 0.81551(17) -0.11952(15) 0.62768(11) 0.0608(4) Uani 1 1 d . . . . . H016 H 0.791187 -0.151935 0.591308 0.073 Uiso 1 1 calc R U . . . C017 C -0.18082(16) 0.2704(2) 0.86596(10) 0.0697(5) Uani 1 1 d . . . . . H017 H -0.213992 0.343062 0.848188 0.084 Uiso 1 1 calc R U . . . C018 C 0.88919(17) -0.02449(15) 0.73548(10) 0.0602(4) Uani 1 1 d . . . . . H018 H 0.914056 0.006941 0.772095 0.072 Uiso 1 1 calc R U . . . C019 C 0.80167(18) -0.08816(16) 0.75175(11) 0.0656(5) Uani 1 1 d . . . . . H019 H 0.767676 -0.099109 0.799817 0.079 Uiso 1 1 calc R U . . . C01A C 0.72286(17) 0.21048(17) 0.43771(11) 0.0634(5) Uani 1 1 d . . . . . H01N H 0.772309 0.148566 0.458627 0.076 Uiso 1 1 calc R U . . . C01B C 0.03162(17) 0.61681(17) 0.85212(11) 0.0681(5) Uani 1 1 d . . . . . C01C C 0.57745(17) 0.3926(2) 0.37453(12) 0.0773(6) Uani 1 1 d . . . . . H01R H 0.528526 0.454441 0.353059 0.093 Uiso 1 1 calc R U . . . C01D C 0.41922(16) 0.16921(18) 0.92972(12) 0.0697(5) Uani 1 1 d . . . . . H01D H 0.460910 0.137856 0.889038 0.084 Uiso 1 1 calc R U . . . C01E C -0.01259(17) 0.13230(19) 0.89684(10) 0.0647(5) Uani 1 1 d . . . . . C01F C 0.09329(15) 0.4232(2) 0.73887(10) 0.0667(5) Uani 1 1 d . . . . . H01A H 0.061308 0.493078 0.710889 0.080 Uiso 1 1 calc R U . . . H01B H 0.084301 0.362137 0.713046 0.080 Uiso 1 1 calc R U . . . C01G C 0.07993(19) 0.60613(19) 0.91733(12) 0.0746(6) Uani 1 1 d . . . . . H01G H 0.060162 0.552868 0.955571 0.089 Uiso 1 1 calc R U . . . C01H C 0.11795(18) 0.1222(2) 0.89089(14) 0.0707(5) Uani 1 1 d . . . . . C01I C 0.25269(19) 0.2817(2) 0.98512(11) 0.0747(6) Uani 1 1 d D . . . . H01I H 0.179946 0.328026 0.982259 0.090 Uiso 1 1 calc DR U . . . C01J C 0.46514(18) 0.1463(2) 0.99622(14) 0.0827(6) Uani 1 1 d . . . . . H01J H 0.538079 0.100458 0.999560 0.099 Uiso 1 1 calc R U . . . C01K C -0.24904(19) 0.1887(3) 0.88770(12) 0.0826(7) Uani 1 1 d . . . . . H01K H -0.329114 0.206859 0.884188 0.099 Uiso 1 1 calc R U . . . C01L C -0.0818(2) 0.0509(2) 0.91877(12) 0.0767(6) Uani 1 1 d . . . . . H01L H -0.049042 -0.022229 0.935976 0.092 Uiso 1 1 calc R U . . . C01M C 0.6754(2) 0.2027(2) 0.37528(13) 0.0842(7) Uani 1 1 d . . . . . H01U H 0.692310 0.135486 0.354494 0.101 Uiso 1 1 calc R U . . . C01N C 0.6678(2) -0.20513(19) 0.71758(15) 0.0807(6) Uani 1 1 d . . . . . H01W H 0.629031 -0.204042 0.675063 0.121 Uiso 1 1 calc R U . . . H01X H 0.612217 -0.174180 0.755635 0.121 Uiso 1 1 calc R U . . . H01Y H 0.701236 -0.281266 0.734163 0.121 Uiso 1 1 calc R U . . . C01O C -0.2013(2) 0.0813(3) 0.91437(13) 0.0846(7) Uani 1 1 d . . . . . H01O H -0.249540 0.028348 0.929658 0.102 Uiso 1 1 calc R U . . . C01P C 0.1569(2) 0.6738(2) 0.92578(15) 0.0863(7) Uani 1 1 d . . . . . H01P H 0.188508 0.665635 0.969965 0.104 Uiso 1 1 calc R U . . . C01Q C 0.4051(2) 0.1897(2) 1.05672(13) 0.0837(6) Uani 1 1 d . . . . . H01Q H 0.436050 0.173192 1.101336 0.100 Uiso 1 1 calc R U . . . C01R C 0.6029(2) 0.2939(3) 0.34347(13) 0.0925(8) Uani 1 1 d . . . . . H01Z H 0.571232 0.288646 0.301047 0.111 Uiso 1 1 calc R U . . . C01S C 0.2987(2) 0.2580(2) 1.05116(12) 0.0850(7) Uani 1 1 d . . . . . H01S H 0.257089 0.288598 1.092127 0.102 Uiso 1 1 calc R U . . . C01T C 0.0582(2) 0.6995(2) 0.79598(14) 0.0869(7) Uani 1 1 d . . . . . H01T H 0.024255 0.709951 0.752471 0.104 Uiso 1 1 calc R U . . . C01U C 0.1884(2) 0.7533(2) 0.87070(17) 0.0926(7) Uani 1 1 d . U . . . C01V C 0.1376(3) 0.7665(2) 0.80700(17) 0.0967(7) Uani 1 1 d . U . . . H01V H 0.156340 0.821684 0.769826 0.116 Uiso 1 1 calc R U . . . C01Y C 0.2777(3) 0.8236(3) 0.8793(3) 0.1399(14) Uani 1 1 d . . . . . H01F H 0.351886 0.775499 0.885293 0.210 Uiso 1 1 calc R U . . . H01H H 0.252309 0.862938 0.921519 0.210 Uiso 1 1 calc R U . . . H01M H 0.285483 0.876953 0.836525 0.210 Uiso 1 1 calc R U . . . H10A H 0.9102(15) 0.3607(15) 0.4043(10) 0.054(5) Uiso 1 1 d . . . . . H10B H 0.8866(16) 0.4706(16) 0.4457(10) 0.059(5) Uiso 1 1 d . . . . . H01C H 0.1449(19) 0.0992(18) 0.9373(13) 0.073(6) Uiso 1 1 d . . . . . H01E H 0.159(2) 0.064(2) 0.8575(14) 0.095(8) Uiso 1 1 d . . . . . C6 C 0.5205(4) 0.5246(6) 0.8309(3) 0.0941(16) Uani 0.753(10) 1 d . U P A 3 H6A H 0.576124 0.476845 0.799868 0.113 Uiso 0.753(10) 1 calc R U P A 3 H6B H 0.522175 0.602420 0.811448 0.113 Uiso 0.753(10) 1 calc R U P A 3 C1 C 0.4682(2) 0.0898(3) 0.6271(2) 0.1160(11) Uani 1 1 d . U . . . H1BC H 0.466490 0.026742 0.600932 0.139 Uiso 0.612(7) 1 calc R U P B 2 H1BD H 0.414702 0.154515 0.607168 0.139 Uiso 0.612(7) 1 calc R U P B 2 H1AA H 0.410469 0.156806 0.635163 0.139 Uiso 0.388(7) 1 calc R U P B 1 H1AB H 0.457985 0.032221 0.667875 0.139 Uiso 0.388(7) 1 calc R U P B 1 C4 C 0.4327(5) 0.0623(5) 0.7053(4) 0.132(2) Uani 0.612(7) 1 d . U P B 2 H4A H 0.489787 0.002412 0.725429 0.198 Uiso 0.612(7) 1 calc R U P B 2 H4B H 0.357925 0.039134 0.711651 0.198 Uiso 0.612(7) 1 calc R U P B 2 H4C H 0.427283 0.127527 0.729965 0.198 Uiso 0.612(7) 1 calc R U P B 2 C5 C 0.4571(9) 0.0485(9) 0.5556(7) 0.161(5) Uani 0.388(7) 1 d . U P B 1 H5A H 0.464000 0.107819 0.516239 0.241 Uiso 0.388(7) 1 calc R U P B 1 H5B H 0.382244 0.026479 0.558028 0.241 Uiso 0.388(7) 1 calc R U P B 1 H5C H 0.518090 -0.014847 0.547123 0.241 Uiso 0.388(7) 1 calc R U P B 1 C7 C 0.5524(5) 0.5040(7) 0.9049(3) 0.145(3) Uani 0.753(10) 1 d . U P A 3 H7A H 0.623931 0.530615 0.906152 0.217 Uiso 0.753(10) 1 calc R U P A 3 H7B H 0.563091 0.424740 0.920975 0.217 Uiso 0.753(10) 1 calc R U P A 3 H7C H 0.491221 0.543053 0.936750 0.217 Uiso 0.753(10) 1 calc R U P A 3 O6 O 0.4039(10) 0.4642(12) 0.8604(7) 0.072(3) Uani 0.247(10) 1 d . U P A 4 C3 C 0.5276(12) 0.4686(14) 0.8656(12) 0.100(5) Uani 0.247(10) 1 d D U P A 4 H3A H 0.549730 0.433662 0.913128 0.120 Uiso 0.247(10) 1 calc R U P A 4 H3B H 0.578327 0.429167 0.828142 0.120 Uiso 0.247(10) 1 calc R U P A 4 C2 C 0.5372(17) 0.5837(14) 0.8557(18) 0.206(12) Uani 0.247(10) 1 d D U P A 4 H2A H 0.532973 0.612799 0.805132 0.309 Uiso 0.247(10) 1 calc R U P A 4 H2B H 0.610703 0.591596 0.869855 0.309 Uiso 0.247(10) 1 calc R U P A 4 H2C H 0.474295 0.624884 0.885285 0.309 Uiso 0.247(10) 1 calc R U P A 4 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 S01 0.0383(2) 0.0491(2) 0.0567(2) 0.00746(17) -0.00520(16) -0.00374(15) S02 0.0413(2) 0.0864(3) 0.0633(3) 0.0079(2) -0.00050(19) 0.0038(2) O003 0.0441(7) 0.0671(7) 0.0620(7) -0.0162(6) 0.0076(5) -0.0025(5) O004 0.0505(7) 0.0518(7) 0.0770(8) 0.0018(6) 0.0139(6) 0.0016(5) O005 0.0354(7) 0.0749(9) 0.0930(10) -0.0049(7) 0.0047(6) -0.0045(6) O006 0.0575(8) 0.0797(9) 0.0754(9) 0.0173(7) -0.0283(6) -0.0149(6) N007 0.0348(7) 0.0475(7) 0.0432(7) 0.0023(5) -0.0006(5) -0.0040(5) O008 0.0490(8) 0.1338(13) 0.0578(8) -0.0289(8) 0.0072(6) -0.0209(8) O009 0.0559(8) 0.0933(10) 0.0721(9) -0.0035(7) 0.0194(7) -0.0067(7) O00A 0.0416(7) 0.1077(11) 0.0990(11) -0.0299(9) 0.0193(7) -0.0186(7) N00B 0.0370(7) 0.0818(10) 0.0482(8) 0.0072(7) 0.0031(6) -0.0043(6) C00C 0.0343(8) 0.0406(7) 0.0452(8) -0.0022(6) -0.0035(6) -0.0076(6) C00D 0.0340(8) 0.0414(7) 0.0466(8) -0.0046(6) -0.0008(6) -0.0092(6) O00E 0.0508(8) 0.0678(9) 0.1538(16) 0.0131(9) -0.0188(9) -0.0257(7) C00F 0.0388(8) 0.0420(8) 0.0476(8) -0.0031(6) -0.0011(6) -0.0105(6) C00G 0.0353(8) 0.0387(7) 0.0433(8) -0.0021(6) -0.0016(6) -0.0076(6) O00H 0.0614(9) 0.1164(13) 0.0969(12) 0.0149(10) -0.0268(8) 0.0146(8) C00I 0.0320(8) 0.0464(8) 0.0529(9) -0.0035(7) -0.0003(6) -0.0075(6) C00J 0.0334(8) 0.0436(8) 0.0488(8) -0.0028(6) -0.0019(6) -0.0056(6) C10 0.0391(8) 0.0497(9) 0.0464(9) 0.0031(7) -0.0044(6) -0.0102(6) C00L 0.0379(8) 0.0522(9) 0.0476(9) -0.0007(7) 0.0032(6) -0.0085(6) C00M 0.0299(8) 0.0549(9) 0.0518(9) 0.0002(7) -0.0018(6) -0.0098(6) O00N 0.0528(12) 0.092(2) 0.086(3) -0.0235(17) -0.0027(16) -0.0207(15) C00O 0.0379(9) 0.0613(10) 0.0566(10) 0.0025(8) -0.0017(7) -0.0129(7) C00P 0.0485(9) 0.0442(8) 0.0518(9) 0.0060(7) -0.0045(7) -0.0043(7) C00Q 0.0406(8) 0.0563(9) 0.0455(8) -0.0050(7) 0.0000(6) -0.0073(7) C00R 0.0356(9) 0.0768(11) 0.0489(9) -0.0077(8) 0.0020(7) -0.0074(7) C00S 0.0382(9) 0.0534(9) 0.0570(10) -0.0021(7) -0.0069(7) -0.0096(7) C00T 0.0430(9) 0.0549(9) 0.0672(11) -0.0055(8) 0.0088(8) -0.0201(7) C00U 0.0367(9) 0.0791(12) 0.0450(9) -0.0016(8) -0.0012(6) -0.0096(7) C00V 0.0611(11) 0.0501(9) 0.0529(10) -0.0046(7) 0.0027(8) -0.0078(8) C00W 0.0466(9) 0.0479(8) 0.0532(9) 0.0008(7) 0.0018(7) -0.0145(7) C00X 0.0342(9) 0.0744(11) 0.0546(10) -0.0074(8) 0.0014(7) -0.0039(7) C00Y 0.0356(9) 0.0607(10) 0.0731(12) -0.0069(8) -0.0031(7) -0.0153(7) C00Z 0.0387(9) 0.0750(11) 0.0527(9) -0.0025(8) -0.0015(7) -0.0094(8) C010 0.0414(9) 0.0909(13) 0.0425(9) -0.0044(8) -0.0008(7) -0.0157(8) C011 0.0342(9) 0.0711(11) 0.0602(10) -0.0013(8) -0.0034(7) -0.0044(7) C012 0.0399(9) 0.0841(13) 0.0535(10) -0.0086(9) 0.0003(7) -0.0121(8) C013 0.0422(9) 0.0858(13) 0.0462(9) -0.0030(8) 0.0028(7) -0.0162(8) C014 0.0365(9) 0.0682(11) 0.0629(11) 0.0073(8) -0.0059(7) -0.0083(7) C015 0.0528(10) 0.0469(9) 0.0737(12) -0.0018(8) -0.0010(9) -0.0081(7) C016 0.0656(12) 0.0496(9) 0.0681(12) -0.0104(8) -0.0072(9) -0.0100(8) C017 0.0420(10) 0.1099(16) 0.0559(11) -0.0048(10) 0.0001(8) -0.0177(10) C018 0.0695(12) 0.0610(10) 0.0503(10) 0.0042(8) -0.0077(8) -0.0191(9) C019 0.0721(13) 0.0650(11) 0.0567(11) 0.0051(9) 0.0053(9) -0.0218(9) C01A 0.0611(11) 0.0669(11) 0.0649(11) -0.0113(9) -0.0102(9) -0.0134(9) C01B 0.0549(11) 0.0690(12) 0.0665(12) 0.0077(9) 0.0044(9) 0.0039(9) C01C 0.0457(11) 0.1123(18) 0.0701(13) 0.0241(13) -0.0166(9) -0.0231(11) C01D 0.0387(10) 0.0895(14) 0.0731(13) -0.0054(10) -0.0027(8) 0.0021(9) C01E 0.0524(11) 0.0883(14) 0.0545(10) -0.0045(9) -0.0016(8) -0.0206(9) C01F 0.0418(10) 0.1069(15) 0.0462(9) 0.0061(9) -0.0007(7) -0.0141(9) C01G 0.0708(14) 0.0788(14) 0.0653(12) 0.0024(10) 0.0024(10) -0.0063(10) C01H 0.0516(11) 0.0786(14) 0.0782(14) 0.0047(11) -0.0079(10) -0.0119(9) C01I 0.0581(12) 0.0937(15) 0.0605(12) -0.0081(10) -0.0057(9) 0.0140(10) C01J 0.0449(11) 0.1046(17) 0.0893(16) 0.0084(13) -0.0174(10) 0.0020(10) C01K 0.0498(12) 0.133(2) 0.0700(13) -0.0126(14) 0.0003(10) -0.0334(13) C01L 0.0703(14) 0.0932(15) 0.0699(13) -0.0060(11) -0.0004(10) -0.0302(11) C01M 0.0943(18) 0.1010(17) 0.0697(14) -0.0198(12) -0.0100(12) -0.0401(14) C01N 0.0678(13) 0.0702(13) 0.1049(17) -0.0064(12) 0.0025(12) -0.0255(10) C01O 0.0667(15) 0.124(2) 0.0738(14) -0.0168(14) 0.0060(11) -0.0473(14) C01P 0.0836(16) 0.0827(15) 0.0892(16) -0.0167(13) -0.0013(13) -0.0077(12) C01Q 0.0690(14) 0.1110(18) 0.0688(14) 0.0038(12) -0.0212(11) -0.0117(12) C01R 0.0828(17) 0.147(3) 0.0649(13) 0.0025(15) -0.0248(12) -0.0609(17) C01S 0.0814(16) 0.1049(17) 0.0605(12) -0.0110(12) -0.0082(11) 0.0046(13) C01T 0.0818(16) 0.0822(15) 0.0804(15) 0.0177(12) -0.0026(12) 0.0015(12) C01U 0.0821(16) 0.0669(13) 0.1207(18) -0.0194(14) 0.0127(13) -0.0039(11) C01V 0.0979(19) 0.0671(13) 0.1094(17) 0.0135(13) 0.0134(13) -0.0109(13) C01Y 0.129(3) 0.089(2) 0.209(4) -0.043(2) 0.004(3) -0.0333(19) C6 0.063(2) 0.114(4) 0.119(4) -0.034(3) -0.011(2) -0.035(2) C1 0.0661(16) 0.109(2) 0.178(3) 0.011(2) -0.0153(18) -0.0487(15) C4 0.090(4) 0.125(4) 0.171(5) -0.025(4) 0.039(4) -0.027(3) C5 0.109(7) 0.137(8) 0.261(11) -0.020(8) -0.068(8) -0.055(6) C7 0.102(4) 0.192(7) 0.161(5) -0.045(5) -0.051(3) -0.033(4) O6 0.055(4) 0.090(6) 0.076(6) -0.006(4) -0.013(4) -0.023(4) C3 0.075(6) 0.116(10) 0.124(13) -0.001(9) -0.037(8) -0.046(7) C2 0.152(15) 0.122(10) 0.37(3) 0.102(16) -0.152(18) -0.082(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O004 S01 O006 119.85(9) . . ? O004 S01 N007 106.30(7) . . ? O004 S01 C00P 109.17(8) . . ? O006 S01 N007 108.25(8) . . ? O006 S01 C00P 106.87(8) . . ? N007 S01 C00P 105.57(7) . . ? O009 S02 N00B 105.88(8) . . ? O009 S02 C01B 108.85(10) . . ? N00B S02 C01B 106.34(9) . . ? O00H S02 O009 119.70(10) . . ? O00H S02 N00B 108.61(10) . . ? O00H S02 C01B 106.76(11) . . ? C00L O003 H003 109.5 . . ? C00G N007 S01 122.90(10) . . ? C00G N007 C00Q 116.71(12) . . ? C00Q N007 S01 120.22(10) . . ? C013 O008 H008 109.5 . . ? C00U N00B S02 123.12(11) . . ? C00U N00B C01F 115.93(15) . . ? C01F N00B S02 120.94(13) . . ? C00G C00C C00J 130.34(13) . . ? C00G C00C C10 109.02(12) . . ? C10 C00C C00J 120.51(12) . . ? C00F C00D C00G 107.09(12) . . ? C00S C00D C00F 120.94(14) . . ? C00S C00D C00G 131.91(14) . . ? C00O O00E C1 118.44(18) . . ? C00D C00F C10 109.18(13) . . ? C00W C00F C00D 120.03(14) . . ? C00W C00F C10 130.77(14) . . ? N007 C00G C00D 122.98(12) . . ? C00C C00G N007 125.29(13) . . ? C00C C00G C00D 110.86(13) . . ? C00J C00I H00I 108.0 . . ? C00J C00I C00L 115.08(12) . . ? C00L C00I H00I 108.0 . . ? C00O C00I H00I 108.0 . . ? C00O C00I C00J 110.36(13) . . ? C00O C00I C00L 107.14(13) . . ? C00C C00J C00I 113.38(12) . . ? C00C C00J H00J 107.2 . . ? C00C C00J C00M 108.90(12) . . ? C00I C00J H00J 107.2 . . ? C00M C00J C00I 112.55(12) . . ? C00M C00J H00J 107.2 . . ? C00C C10 H10A 112.0(11) . . ? C00C C10 H10B 112.5(10) . . ? C00F C10 C00C 103.76(12) . . ? C00F C10 H10A 110.1(11) . . ? C00F C10 H10B 111.4(11) . . ? H10A C10 H10B 107.1(15) . . ? O003 C00L C00I 112.25(13) . . ? O003 C00L H00L 108.4 . . ? O003 C00L C00Q 104.36(13) . . ? C00I C00L H00L 108.4 . . ? C00Q C00L C00I 114.75(13) . . ? C00Q C00L H00L 108.4 . . ? C014 C00M C00J 120.31(15) . . ? C01A C00M C00J 121.02(15) . . ? C01A C00M C014 118.63(16) . . ? C012 O00N C6 118.5(4) . . ? O005 C00O O00E 123.88(15) . . ? O005 C00O C00I 125.06(16) . . ? O00E C00O C00I 111.06(14) . . ? C00V C00P S01 119.93(13) . . ? C018 C00P S01 119.41(14) . . ? C018 C00P C00V 120.56(16) . . ? N007 C00Q C00L 116.48(13) . . ? N007 C00Q H00A 108.2 . . ? N007 C00Q H00B 108.2 . . ? C00L C00Q H00A 108.2 . . ? C00L C00Q H00B 108.2 . . ? H00A C00Q H00B 107.3 . . ? C00X C00R H00R 108.3 . . ? C00X C00R C013 115.35(15) . . ? C012 C00R H00R 108.3 . . ? C012 C00R C00X 109.01(14) . . ? C012 C00R C013 107.33(14) . . ? C013 C00R H00R 108.3 . . ? C00D C00S H00S 120.8 . . ? C00D C00S C00Y 118.36(16) . . ? C00Y C00S H00S 120.8 . . ? C00W C00T H00T 119.5 . . ? C00W C00T C00Y 120.97(15) . . ? C00Y C00T H00T 119.5 . . ? N00B C00U C010 124.38(15) . . ? C00Z C00U N00B 124.41(15) . . ? C00Z C00U C010 110.11(17) . . ? C00P C00V H00V 120.5 . . ? C016 C00V C00P 119.02(17) . . ? C016 C00V H00V 120.5 . . ? C00F C00W H00W 120.6 . . ? C00T C00W C00F 118.83(15) . . ? C00T C00W H00W 120.6 . . ? C00R C00X H00X 107.5 . . ? C00Z C00X C00R 114.56(14) . . ? C00Z C00X H00X 107.5 . . ? C00Z C00X C011 108.53(14) . . ? C011 C00X C00R 110.93(15) . . ? C011 C00X H00X 107.5 . . ? C00S C00Y H00Y 119.6 . . ? C00T C00Y C00S 120.79(16) . . ? C00T C00Y H00Y 119.6 . . ? C00U C00Z C00X 129.86(17) . . ? C00U C00Z C01H 109.66(16) . . ? C01H C00Z C00X 120.47(16) . . ? C017 C010 C00U 131.98(19) . . ? C017 C010 C01E 120.56(19) . . ? C01E C010 C00U 107.38(16) . . ? C01D C011 C00X 121.27(17) . . ? C01I C011 C00X 120.95(16) . . ? C01I C011 C01D 117.77(18) . . ? O00A C012 O00N 122.4(2) . . ? O00A C012 C00R 124.15(18) . . ? O00A C012 O6 122.6(6) . . ? O00N C012 C00R 112.9(2) . . ? O6 C012 C00R 109.2(6) . . ? O008 C013 C00R 112.53(16) . . ? O008 C013 H013 108.6 . . ? O008 C013 C01F 104.29(15) . . ? C00R C013 H013 108.6 . . ? C01F C013 C00R 114.05(14) . . ? C01F C013 H013 108.6 . . ? C00M C014 H014 119.8 . . ? C01C C014 C00M 120.4(2) . . ? C01C C014 H014 119.8 . . ? C016 C015 C01N 120.89(19) . . ? C019 C015 C016 118.40(17) . . ? C019 C015 C01N 120.72(19) . . ? C00V C016 H016 119.3 . . ? C015 C016 C00V 121.37(18) . . ? C015 C016 H016 119.3 . . ? C010 C017 H017 120.8 . . ? C01K C017 C010 118.3(2) . . ? C01K C017 H017 120.8 . . ? C00P C018 H018 120.5 . . ? C019 C018 C00P 119.02(18) . . ? C019 C018 H018 120.5 . . ? C015 C019 C018 121.63(18) . . ? C015 C019 H019 119.2 . . ? C018 C019 H019 119.2 . . ? C00M C01A H01N 119.6 . . ? C01M C01A C00M 120.8(2) . . ? C01M C01A H01N 119.6 . . ? C01G C01B S02 119.46(16) . . ? C01G C01B C01T 119.6(2) . . ? C01T C01B S02 120.89(19) . . ? C014 C01C H01R 119.9 . . ? C01R C01C C014 120.2(2) . . ? C01R C01C H01R 119.9 . . ? C011 C01D H01D 119.8 . . ? C011 C01D C01J 120.3(2) . . ? C01J C01D H01D 119.8 . . ? C010 C01E C01H 109.23(17) . . ? C01L C01E C010 120.74(19) . . ? C01L C01E C01H 129.9(2) . . ? N00B C01F C013 116.24(15) . . ? N00B C01F H01A 108.2 . . ? N00B C01F H01B 108.2 . . ? C013 C01F H01A 108.2 . . ? C013 C01F H01B 108.2 . . ? H01A C01F H01B 107.4 . . ? C01B C01G H01G 119.9 . . ? C01P C01G C01B 120.3(2) . . ? C01P C01G H01G 119.9 . . ? C00Z C01H C01E 103.57(17) . . ? C00Z C01H H01C 111.3(13) . . ? C00Z C01H H01E 112.8(15) . . ? C01E C01H H01C 110.4(14) . . ? C01E C01H H01E 111.5(15) . . ? H01C C01H H01E 107(2) . . ? C011 C01I H01I 119.2 . . ? C011 C01I C01S 121.54(19) . . ? C01S C01I H01I 119.2 . . ? C01D C01J H01J 119.5 . . ? C01Q C01J C01D 120.9(2) . . ? C01Q C01J H01J 119.5 . . ? C017 C01K H01K 119.3 . . ? C01O C01K C017 121.4(2) . . ? C01O C01K H01K 119.3 . . ? C01E C01L H01L 120.9 . . ? C01E C01L C01O 118.3(2) . . ? C01O C01L H01L 120.9 . . ? C01A C01M H01U 119.9 . . ? C01A C01M C01R 120.2(2) . . ? C01R C01M H01U 119.9 . . ? C015 C01N H01W 109.5 . . ? C015 C01N H01X 109.5 . . ? C015 C01N H01Y 109.5 . . ? H01W C01N H01X 109.5 . . ? H01W C01N H01Y 109.5 . . ? H01X C01N H01Y 109.5 . . ? C01K C01O C01L 120.7(2) . . ? C01K C01O H01O 119.7 . . ? C01L C01O H01O 119.7 . . ? C01G C01P H01P 119.2 . . ? C01U C01P C01G 121.7(3) . . ? C01U C01P H01P 119.2 . . ? C01J C01Q H01Q 120.4 . . ? C01J C01Q C01S 119.2(2) . . ? C01S C01Q H01Q 120.4 . . ? C01C C01R C01M 119.8(2) . . ? C01C C01R H01Z 120.1 . . ? C01M C01R H01Z 120.1 . . ? C01I C01S H01S 119.9 . . ? C01Q C01S C01I 120.2(2) . . ? C01Q C01S H01S 119.9 . . ? C01B C01T H01T 121.0 . . ? C01B C01T C01V 118.0(2) . . ? C01V C01T H01T 121.0 . . ? C01P C01U C01Y 121.2(3) . . ? C01V C01U C01P 118.1(3) . . ? C01V C01U C01Y 120.7(3) . . ? C01T C01V H01V 118.9 . . ? C01U C01V C01T 122.2(2) . . ? C01U C01V H01V 118.9 . . ? C01U C01Y H01F 109.5 . . ? C01U C01Y H01H 109.5 . . ? C01U C01Y H01M 109.5 . . ? H01F C01Y H01H 109.5 . . ? H01F C01Y H01M 109.5 . . ? H01H C01Y H01M 109.5 . . ? O00N C6 H6A 109.8 . . ? O00N C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C7 C6 O00N 109.2(5) . . ? C7 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? O00E C1 H1BC 110.0 . . ? O00E C1 H1BD 110.0 . . ? O00E C1 H1AA 110.9 . . ? O00E C1 H1AB 110.9 . . ? O00E C1 C4 108.4(3) . . ? O00E C1 C5 104.5(5) . . ? H1BC C1 H1BD 108.4 . . ? H1AA C1 H1AB 108.9 . . ? C4 C1 H1BC 110.0 . . ? C4 C1 H1BD 110.0 . . ? C5 C1 H1AA 110.9 . . ? C5 C1 H1AB 110.9 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? 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 . . ? C012 O6 C3 112.4(11) . . ? O6 C3 H3A 110.4 . . ? O6 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C2 C3 O6 106.7(13) . . ? C2 C3 H3A 110.4 . . ? C2 C3 H3B 110.4 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S01 O004 1.4243(13) . ? S01 O006 1.4263(14) . ? S01 N007 1.6354(13) . ? S01 C00P 1.7595(17) . ? S02 O009 1.4259(14) . ? S02 N00B 1.6333(16) . ? S02 O00H 1.4228(15) . ? S02 C01B 1.758(2) . ? O003 H003 0.8200 . ? O003 C00L 1.4257(19) . ? O005 C00O 1.200(2) . ? N007 C00G 1.4228(19) . ? N007 C00Q 1.463(2) . ? O008 H008 0.8200 . ? O008 C013 1.412(2) . ? O00A C012 1.197(2) . ? N00B C00U 1.419(2) . ? N00B C01F 1.468(2) . ? C00C C00G 1.347(2) . ? C00C C00J 1.510(2) . ? C00C C10 1.506(2) . ? C00D C00F 1.400(2) . ? C00D C00G 1.4704(19) . ? C00D C00S 1.379(2) . ? O00E C00O 1.324(2) . ? O00E C1 1.453(3) . ? C00F C10 1.499(2) . ? C00F C00W 1.383(2) . ? C00I H00I 0.9800 . ? C00I C00J 1.539(2) . ? C00I C00L 1.543(2) . ? C00I C00O 1.514(2) . ? C00J H00J 0.9800 . ? C00J C00M 1.522(2) . ? C10 H10A 0.963(19) . ? C10 H10B 1.022(19) . ? C00L H00L 0.9800 . ? C00L C00Q 1.526(2) . ? C00M C014 1.387(2) . ? C00M C01A 1.380(2) . ? O00N C012 1.338(4) . ? O00N C6 1.460(5) . ? C00P C00V 1.385(3) . ? C00P C018 1.381(2) . ? C00Q H00A 0.9700 . ? C00Q H00B 0.9700 . ? C00R H00R 0.9800 . ? C00R C00X 1.533(3) . ? C00R C012 1.512(2) . ? C00R C013 1.546(2) . ? C00S H00S 0.9300 . ? C00S C00Y 1.388(2) . ? C00T H00T 0.9300 . ? C00T C00W 1.381(2) . ? C00T C00Y 1.381(3) . ? C00U C00Z 1.343(2) . ? C00U C010 1.477(2) . ? C00V H00V 0.9300 . ? C00V C016 1.383(3) . ? C00W H00W 0.9300 . ? C00X H00X 0.9800 . ? C00X C00Z 1.507(2) . ? C00X C011 1.530(2) . ? C00Y H00Y 0.9300 . ? C00Z C01H 1.495(3) . ? C010 C017 1.384(3) . ? C010 C01E 1.387(3) . ? C011 C01D 1.383(2) . ? C011 C01I 1.372(3) . ? C012 O6 1.309(12) . ? C013 H013 0.9800 . ? C013 C01F 1.534(2) . ? C014 H014 0.9300 . ? C014 C01C 1.380(3) . ? C015 C016 1.379(3) . ? C015 C019 1.378(3) . ? C015 C01N 1.507(3) . ? C016 H016 0.9300 . ? C017 H017 0.9300 . ? C017 C01K 1.380(3) . ? C018 H018 0.9300 . ? C018 C019 1.381(3) . ? C019 H019 0.9300 . ? C01A H01N 0.9300 . ? C01A C01M 1.375(3) . ? C01B C01G 1.384(3) . ? C01B C01T 1.393(3) . ? C01C H01R 0.9300 . ? C01C C01R 1.372(4) . ? C01D H01D 0.9300 . ? C01D C01J 1.385(3) . ? C01E C01H 1.500(3) . ? C01E C01L 1.386(3) . ? C01F H01A 0.9700 . ? C01F H01B 0.9700 . ? C01G H01G 0.9300 . ? C01G C01P 1.373(3) . ? C01H H01C 0.95(2) . ? C01H H01E 1.01(3) . ? C01I H01I 0.9300 . ? C01I C01S 1.377(3) . ? C01J H01J 0.9300 . ? C01J C01Q 1.360(3) . ? C01K H01K 0.9300 . ? C01K C01O 1.372(4) . ? C01L H01L 0.9300 . ? C01L C01O 1.387(3) . ? C01M H01U 0.9300 . ? C01M C01R 1.375(4) . ? C01N H01W 0.9600 . ? C01N H01X 0.9600 . ? C01N H01Y 0.9600 . ? C01O H01O 0.9300 . ? C01P H01P 0.9300 . ? C01P C01U 1.371(4) . ? C01Q H01Q 0.9300 . ? C01Q C01S 1.365(3) . ? C01R H01Z 0.9300 . ? C01S H01S 0.9300 . ? C01T H01T 0.9300 . ? C01T C01V 1.403(4) . ? C01U C01V 1.371(4) . ? C01U C01Y 1.512(4) . ? C01V H01V 0.9300 . ? C01Y H01F 0.9600 . ? C01Y H01H 0.9600 . ? C01Y H01M 0.9600 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C7 1.449(9) . ? C1 H1BC 0.9700 . ? C1 H1BD 0.9700 . ? C1 H1AA 0.9700 . ? C1 H1AB 0.9700 . ? C1 C4 1.467(7) . ? C1 C5 1.514(12) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? O6 C3 1.477(17) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C2 1.415(18) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S01 N007 C00G C00C 128.98(14) . . . . ? S01 N007 C00G C00D -62.68(18) . . . . ? S01 N007 C00Q C00L -98.65(15) . . . . ? S01 C00P C00V C016 -175.87(13) . . . . ? S01 C00P C018 C019 175.70(14) . . . . ? S02 N00B C00U C00Z -130.09(17) . . . . ? S02 N00B C00U C010 63.1(2) . . . . ? S02 N00B C01F C013 103.90(19) . . . . ? S02 C01B C01G C01P 177.08(17) . . . . ? S02 C01B C01T C01V -176.90(18) . . . . ? O003 C00L C00Q N007 -143.24(13) . . . . ? O004 S01 N007 C00G 1.90(14) . . . . ? O004 S01 N007 C00Q 177.18(12) . . . . ? O004 S01 C00P C00V -25.05(16) . . . . ? O004 S01 C00P C018 158.56(14) . . . . ? O006 S01 N007 C00G 131.87(12) . . . . ? O006 S01 N007 C00Q -52.85(14) . . . . ? O006 S01 C00P C00V -156.04(14) . . . . ? O006 S01 C00P C018 27.57(16) . . . . ? N007 S01 C00P C00V 88.85(15) . . . . ? N007 S01 C00P C018 -87.53(15) . . . . ? O008 C013 C01F N00B 133.65(18) . . . . ? O009 S02 N00B C00U -0.19(16) . . . . ? O009 S02 N00B C01F -179.28(14) . . . . ? O009 S02 C01B C01G 26.19(19) . . . . ? O009 S02 C01B C01T -154.39(17) . . . . ? O00A C012 O6 C3 12.5(13) . . . . ? N00B S02 C01B C01G -87.48(17) . . . . ? N00B S02 C01B C01T 91.94(18) . . . . ? N00B C00U C00Z C00X 12.5(3) . . . . ? N00B C00U C00Z C01H -167.19(18) . . . . ? N00B C00U C010 C017 -7.8(3) . . . . ? N00B C00U C010 C01E 168.77(17) . . . . ? C00C C00J C00M C014 -108.85(16) . . . . ? C00C C00J C00M C01A 68.87(18) . . . . ? C00D C00F C10 C00C -0.35(17) . . . . ? C00D C00F C00W C00T -1.9(2) . . . . ? C00D C00S C00Y C00T -0.6(3) . . . . ? C00F C00D C00G N007 -173.12(13) . . . . ? C00F C00D C00G C00C -3.29(17) . . . . ? C00F C00D C00S C00Y -2.0(2) . . . . ? C00G N007 C00Q C00L 76.91(17) . . . . ? C00G C00C C00J C00I -14.0(2) . . . . ? C00G C00C C00J C00M -140.14(16) . . . . ? C00G C00C C10 C00F -1.69(17) . . . . ? C00G C00D C00F C10 2.08(17) . . . . ? C00G C00D C00F C00W -179.34(14) . . . . ? C00G C00D C00S C00Y -178.62(16) . . . . ? O00H S02 N00B C00U -129.93(15) . . . . ? O00H S02 N00B C01F 50.98(17) . . . . ? O00H S02 C01B C01G 156.70(17) . . . . ? O00H S02 C01B C01T -23.9(2) . . . . ? C00I C00J C00M C014 124.54(15) . . . . ? C00I C00J C00M C01A -57.74(19) . . . . ? C00I C00L C00Q N007 -20.0(2) . . . . ? C00J C00C C00G N007 -3.0(3) . . . . ? C00J C00C C00G C00D -172.58(14) . . . . ? C00J C00C C10 C00F 174.46(13) . . . . ? C00J C00I C00L O003 59.06(17) . . . . ? C00J C00I C00L C00Q -59.86(18) . . . . ? C00J C00I C00O O005 -47.0(2) . . . . ? C00J C00I C00O O00E 133.43(16) . . . . ? C00J C00M C014 C01C 177.38(15) . . . . ? C00J C00M C01A C01M -177.88(17) . . . . ? C10 C00C C00G N007 172.61(14) . . . . ? C10 C00C C00G C00D 3.07(17) . . . . ? C10 C00C C00J C00I 170.77(14) . . . . ? C10 C00C C00J C00M 44.64(18) . . . . ? C10 C00F C00W C00T 176.33(16) . . . . ? C00L C00I C00J C00C 69.46(17) . . . . ? C00L C00I C00J C00M -166.37(13) . . . . ? C00L C00I C00O O005 78.9(2) . . . . ? C00L C00I C00O O00E -100.58(17) . . . . ? C00M C014 C01C C01R 0.5(3) . . . . ? C00M C01A C01M C01R 0.5(3) . . . . ? C00O O00E C1 C4 -98.3(3) . . . . ? C00O O00E C1 C5 108.3(5) . . . . ? C00O C00I C00J C00C -169.15(13) . . . . ? C00O C00I C00J C00M -44.99(17) . . . . ? C00O C00I C00L O003 -64.05(16) . . . . ? C00O C00I C00L C00Q 177.02(13) . . . . ? C00P S01 N007 C00G -113.98(12) . . . . ? C00P S01 N007 C00Q 61.29(13) . . . . ? C00P C00V C016 C015 0.2(3) . . . . ? C00P C018 C019 C015 0.2(3) . . . . ? C00Q N007 C00G C00C -46.5(2) . . . . ? C00Q N007 C00G C00D 121.89(15) . . . . ? C00R C00X C00Z C00U -3.0(3) . . . . ? C00R C00X C00Z C01H 176.68(18) . . . . ? C00R C00X C011 C01D -106.4(2) . . . . ? C00R C00X C011 C01I 74.1(2) . . . . ? C00R C012 O6 C3 170.6(9) . . . . ? C00R C013 C01F N00B 10.5(3) . . . . ? C00S C00D C00F C10 -175.32(14) . . . . ? C00S C00D C00F C00W 3.3(2) . . . . ? C00S C00D C00G N007 3.9(3) . . . . ? C00S C00D C00G C00C 173.71(16) . . . . ? C00U N00B C01F C013 -75.3(2) . . . . ? C00U C00Z C01H C01E -2.2(2) . . . . ? C00U C010 C017 C01K 177.12(19) . . . . ? C00U C010 C01E C01H -1.8(2) . . . . ? C00U C010 C01E C01L -178.18(18) . . . . ? C00V C00P C018 C019 -0.7(3) . . . . ? C00W C00F C10 C00C -178.73(16) . . . . ? C00W C00T C00Y C00S 2.0(3) . . . . ? C00X C00R C012 O00A 51.6(2) . . . . ? C00X C00R C012 O00N -136.2(3) . . . . ? C00X C00R C012 O6 -106.1(7) . . . . ? C00X C00R C013 O008 -52.58(19) . . . . ? C00X C00R C013 C01F 66.0(2) . . . . ? C00X C00Z C01H C01E 178.11(17) . . . . ? C00X C011 C01D C01J 179.7(2) . . . . ? C00X C011 C01I C01S 179.9(2) . . . . ? C00Y C00T C00W C00F -0.7(3) . . . . ? C00Z C00U C010 C017 -176.2(2) . . . . ? C00Z C00U C010 C01E 0.4(2) . . . . ? C00Z C00X C011 C01D 126.89(19) . . . . ? C00Z C00X C011 C01I -52.6(2) . . . . ? C010 C00U C00Z C00X -179.12(17) . . . . ? C010 C00U C00Z C01H 1.2(2) . . . . ? C010 C017 C01K C01O 0.4(3) . . . . ? C010 C01E C01H C00Z 2.4(2) . . . . ? C010 C01E C01L C01O 0.1(3) . . . . ? C011 C00X C00Z C00U 121.6(2) . . . . ? C011 C00X C00Z C01H -58.8(2) . . . . ? C011 C01D C01J C01Q 1.0(4) . . . . ? C011 C01I C01S C01Q -0.3(4) . . . . ? C012 O00N C6 C7 -101.5(6) . . . . ? C012 C00R C00X C00Z 178.23(15) . . . . ? C012 C00R C00X C011 54.94(18) . . . . ? C012 C00R C013 O008 69.11(19) . . . . ? C012 C00R C013 C01F -172.35(17) . . . . ? C012 O6 C3 C2 124(2) . . . . ? C013 C00R C00X C00Z -61.0(2) . . . . ? C013 C00R C00X C011 175.72(14) . . . . ? C013 C00R C012 O00A -74.0(2) . . . . ? C013 C00R C012 O00N 98.2(3) . . . . ? C013 C00R C012 O6 128.4(7) . . . . ? C014 C00M C01A C01M -0.1(3) . . . . ? C014 C01C C01R C01M -0.1(3) . . . . ? C016 C015 C019 C018 0.5(3) . . . . ? C017 C010 C01E C01H 175.26(19) . . . . ? C017 C010 C01E C01L -1.1(3) . . . . ? C017 C01K C01O C01L -1.4(4) . . . . ? C018 C00P C00V C016 0.5(3) . . . . ? C019 C015 C016 C00V -0.7(3) . . . . ? C01A C00M C014 C01C -0.4(2) . . . . ? C01A C01M C01R C01C -0.4(4) . . . . ? C01B S02 N00B C00U 115.50(15) . . . . ? C01B S02 N00B C01F -63.60(16) . . . . ? C01B C01G C01P C01U -0.1(3) . . . . ? C01B C01T C01V C01U -0.3(4) . . . . ? C01D C011 C01I C01S 0.5(3) . . . . ? C01D C01J C01Q C01S -0.8(4) . . . . ? C01E C010 C017 C01K 0.9(3) . . . . ? C01E C01L C01O C01K 1.2(3) . . . . ? C01F N00B C00U C00Z 49.0(2) . . . . ? C01F N00B C00U C010 -117.72(18) . . . . ? C01G C01B C01T C01V 2.5(3) . . . . ? C01G C01P C01U C01V 2.2(4) . . . . ? C01G C01P C01U C01Y -177.1(2) . . . . ? C01H C01E C01L C01O -175.5(2) . . . . ? C01I C011 C01D C01J -0.8(3) . . . . ? C01J C01Q C01S C01I 0.4(4) . . . . ? C01L C01E C01H C00Z 178.4(2) . . . . ? C01N C015 C016 C00V 179.85(18) . . . . ? C01N C015 C019 C018 179.96(18) . . . . ? C01P C01U C01V C01T -2.0(4) . . . . ? C01T C01B C01G C01P -2.4(3) . . . . ? C01Y C01U C01V C01T 177.3(3) . . . . ? C6 O00N C012 O00A -10.4(5) . . . . ? C6 O00N C012 C00R 177.2(3) . . . . ? C1 O00E C00O O005 0.8(3) . . . . ? C1 O00E C00O C00I -179.7(2) . . . . ?