#------------------------------------------------------------------------------ #$Date: 2021-07-06 06:56:50 +0300 (Tue, 06 Jul 2021) $ #$Revision: 267272 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/81/7158161.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_7158161 loop_ _publ_author_name 'Kulkarni, Pradnya' 'Datta, Dhrubajyoti' 'Ramabhadran, Raghunath Ozhapakkam' 'Ganesh, Krishna' _publ_section_title ; Gemdimethyl Peptide Nucleic Acid (\a/\b/\g-gdm-PNA) Monomers: Synthesis and the Role of gdm-Substituents in Preferential Stabilisation of Z/E-Rotamers ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB01097B _journal_year 2021 _chemical_formula_moiety 'C19 H30 N4 O7, 5(O)' _chemical_formula_sum 'C19 H30 N4 O12' _chemical_formula_weight 506.47 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-01-08 deposited with the CCDC. 2021-07-05 downloaded from the CCDC. ; _cell_angle_alpha 89.931(4) _cell_angle_beta 89.940(4) _cell_angle_gamma 89.969(5) _cell_formula_units_Z 8 _cell_length_a 8.694(2) _cell_length_b 18.217(4) _cell_length_c 34.494(9) _cell_measurement_reflns_used 2433 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 20.56 _cell_measurement_theta_min 2.36 _cell_volume 5463(2) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.3248 _diffrn_reflns_av_unetI/netI 0.4966 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_number 112152 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.164 _diffrn_reflns_theta_min 1.118 _exptl_absorpt_coefficient_mu 0.103 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.232 _exptl_crystal_description rodshape _exptl_crystal_F_000 2144.0 _refine_diff_density_max 0.483 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1289 _refine_ls_number_reflns 32012 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.912 _refine_ls_R_factor_all 0.3769 _refine_ls_R_factor_gt 0.1058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.3571P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2067 _refine_ls_wR_factor_ref 0.3326 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7947 _reflns_number_total 32012 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob01097b2.cif _cod_data_source_block tri_a _cod_database_code 7158161 _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_res_file ; tri_a.res created by SHELXL-2014/7 TITL tri_a.res in P-1 CELL 0.71073 8.6942 18.2167 34.4938 89.931 89.940 89.969 ZERR 109.000 0.0021 0.0044 0.0085 0.004 0.004 0.005 LATT 1 SFAC C H N O UNIT 109 109 109 109 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 TEMP 23.000 WGHT 0.100000 0.357050 FVAR 0.22126 O28 4 0.357385 0.428372 0.150422 11.00000 0.01998 0.02122 = 0.03811 0.00331 -0.00040 -0.00237 O5 4 0.142210 0.428485 0.849652 11.00000 0.01917 0.02509 = 0.04054 0.00008 0.00208 0.00041 O10 4 0.642355 0.071793 0.650506 11.00000 0.01969 0.02865 = 0.03552 -0.00235 0.00162 -0.00270 O20 4 0.857680 0.071375 0.349487 11.00000 0.01913 0.02612 = 0.03911 0.00293 -0.00055 0.00052 O15 4 0.272278 0.118532 0.312495 11.00000 0.01805 0.02780 = 0.04737 -0.00310 0.00188 -0.00186 O49 4 0.417479 0.100677 0.843872 11.00000 0.02334 0.02491 = 0.04481 0.00817 -0.00159 0.00473 O18 4 0.582577 0.398972 0.343763 11.00000 0.02344 0.02395 = 0.04297 -0.00185 -0.00272 0.00346 O4 4 0.727389 0.381162 0.812097 11.00000 0.01877 0.02904 = 0.04428 0.00774 -0.00240 0.00077 O8 4 1.227362 0.118852 0.687440 11.00000 0.01889 0.02821 = 0.04194 0.00530 -0.00015 0.00222 O2 4 0.417079 0.171186 0.788846 11.00000 0.03572 0.02636 = 0.03809 0.00494 0.00563 0.00540 O24 4 0.082132 0.170833 0.211154 11.00000 0.03345 0.02466 = 0.03807 -0.00277 0.00914 -0.00712 O14 4 0.917470 0.399205 0.656108 11.00000 0.02026 0.02962 = 0.04387 0.00711 -0.00363 -0.00350 O17 4 0.581797 0.328858 0.288919 11.00000 0.03287 0.02699 = 0.04038 -0.00334 -0.00333 0.00409 O16 4 0.483747 0.071137 0.284044 11.00000 0.02309 0.03026 = 0.04587 -0.00822 -0.00051 0.00647 O13 4 0.917017 0.329066 0.710955 11.00000 0.03445 0.02653 = 0.03713 -0.00111 -0.00735 -0.00606 O25 4 0.083221 0.100765 0.156388 11.00000 0.02415 0.02604 = 0.04719 -0.00488 0.00352 -0.00576 O3 4 0.515924 0.428715 0.784120 11.00000 0.02232 0.03185 = 0.04278 0.00594 0.00272 0.00456 O22 4 -0.227512 0.382227 0.187517 11.00000 0.01952 0.03070 = 0.04296 -0.00201 -0.00417 0.00182 O23 4 -0.016140 0.428922 0.215647 11.00000 0.02431 0.03071 = 0.04289 -0.00236 0.00207 -0.00404 O11 4 0.719268 0.122000 0.566936 11.00000 0.04862 0.02755 = 0.03778 0.00193 0.00012 0.00121 O27 4 0.281353 0.377814 0.067071 11.00000 0.04594 0.02527 = 0.03808 0.00028 0.00110 0.00427 O9 4 1.016153 0.071497 0.715672 11.00000 0.02571 0.02848 = 0.04423 0.00570 0.00091 -0.00272 O6 4 0.218628 0.377638 0.933019 11.00000 0.04418 0.02675 = 0.04230 0.00328 -0.00064 -0.00270 O12 4 0.553104 -0.090713 0.512994 11.00000 0.04418 0.03366 = 0.03589 -0.00120 -0.00621 0.00307 O7 4 0.052474 0.591292 0.986827 11.00000 0.04136 0.03338 = 0.03914 -0.00625 0.01210 -0.00205 O19 4 0.780426 0.122189 0.433278 11.00000 0.04325 0.03046 = 0.04481 0.00157 -0.00099 -0.00596 O21 4 0.948091 -0.091097 0.486964 11.00000 0.03741 0.03870 = 0.03993 0.00198 -0.00949 -0.00091 O26 4 0.447474 0.591380 0.013078 11.00000 0.04505 0.03523 = 0.03585 0.00204 0.00999 0.00053 N12 3 0.640667 0.014483 0.540131 11.00000 0.03233 0.02125 = 0.02687 0.00690 -0.00125 0.00392 AFIX 43 H12 2 0.585445 0.038382 0.523736 11.00000 -1.20000 AFIX 0 N10 3 0.826226 0.153797 0.667514 11.00000 0.01646 0.02145 = 0.03397 -0.00360 -0.00069 -0.00067 N15 3 0.325807 0.345319 0.832486 11.00000 0.01964 0.01672 = 0.03319 -0.00036 -0.00197 -0.00103 N7 3 0.672974 0.154429 0.332235 11.00000 0.01910 0.01775 = 0.03308 0.00770 0.00101 0.00147 N106 3 0.754275 0.311131 0.338228 11.00000 0.02584 0.02598 = 0.02763 -0.00382 0.00004 0.00056 AFIX 43 H106 2 0.769881 0.320865 0.362294 11.00000 -1.20000 AFIX 0 O44 4 0.152138 0.141177 0.919975 11.00000 0.05357 0.05197 = 0.04085 0.00226 0.00325 -0.00184 N3 3 0.173394 0.346008 0.167921 11.00000 0.02293 0.01749 = 0.03043 0.00296 0.00306 0.00185 N1 3 0.360699 0.485419 0.040234 11.00000 0.03063 0.01973 = 0.02954 0.00080 0.00602 0.00821 AFIX 43 H1 2 0.417243 0.461726 0.024044 11.00000 -1.20000 AFIX 0 N13 3 0.140210 0.485433 0.959605 11.00000 0.03244 0.02610 = 0.02601 0.00331 0.00609 -0.00487 AFIX 43 H13 2 0.084240 0.461485 0.975835 11.00000 -1.20000 AFIX 0 N105 3 0.254446 0.188990 0.161983 11.00000 0.02772 0.01771 = 0.02774 -0.00149 -0.00123 0.00449 AFIX 43 H105 2 0.271200 0.178651 0.138027 11.00000 -1.20000 AFIX 0 N108 3 0.245805 0.188757 0.838120 11.00000 0.02284 0.02331 = 0.03526 0.00163 0.00303 -0.00023 AFIX 43 H108 2 0.229382 0.179102 0.862182 11.00000 -1.20000 AFIX 0 N2 3 0.189850 0.485523 0.091631 11.00000 0.02290 0.02279 = 0.02971 0.00202 0.00413 0.00247 N107 3 0.745947 0.311234 0.662237 11.00000 0.02827 0.02063 = 0.02928 0.00012 0.00019 -0.00331 AFIX 43 H107 2 0.729371 0.321730 0.638288 11.00000 -1.20000 AFIX 0 O37 4 0.652465 0.358408 0.580014 11.00000 0.05751 0.04391 = 0.04907 0.00203 -0.00377 0.00486 N14 3 0.310686 0.484995 0.908389 11.00000 0.02634 0.02113 = 0.02652 0.00151 0.00250 -0.00357 N11 3 0.810800 0.015017 0.591908 11.00000 0.02312 0.02857 = 0.02562 0.00168 0.00012 0.00628 O48 4 0.320688 0.035548 0.963416 11.00000 0.06266 0.04460 = 0.05538 0.00354 -0.00165 0.00119 N5 3 0.860254 0.014184 0.459527 11.00000 0.03131 0.02743 = 0.02488 0.00071 -0.00289 -0.00678 AFIX 43 H5 2 0.917082 0.037871 0.475614 11.00000 -1.20000 AFIX 0 O34 4 0.847191 0.358977 0.420076 11.00000 0.06164 0.04521 = 0.04088 -0.00193 -0.00113 -0.00237 O31 4 0.348231 0.140932 0.079893 11.00000 0.05455 0.04636 = 0.04919 0.00221 -0.00008 0.00252 O39 4 0.678139 0.464283 0.463028 11.00000 0.05626 0.04879 = 0.05298 0.00130 0.00064 0.00394 O41 4 0.360700 0.383403 0.546333 11.00000 0.04777 0.05468 = 0.06733 0.00086 0.00002 -0.00095 N6 3 0.689525 0.015203 0.408250 11.00000 0.03247 0.02429 = 0.02367 0.00591 0.00278 -0.00506 O30 4 0.640596 0.116542 0.046555 11.00000 0.05702 0.05126 = 0.07113 -0.00258 -0.00064 -0.00118 O33 4 0.179491 0.035611 0.036764 11.00000 0.05848 0.04773 = 0.05959 0.00554 -0.00380 -0.00100 O40 4 0.450322 0.356818 0.469581 11.00000 0.05765 0.05792 = 0.07495 0.00078 0.00734 -0.00931 O38 4 0.821403 0.463747 0.536659 11.00000 0.05600 0.04823 = 0.06282 0.00124 0.00105 -0.00310 O47 4 0.860985 0.116157 0.953600 11.00000 0.05019 0.05759 = 0.07125 0.00110 0.00053 -0.00476 O29 4 0.951341 0.143389 0.030531 11.00000 0.05299 0.05418 = 0.08263 -0.00562 -0.00398 -0.00036 O43 4 0.138990 0.383480 0.453904 11.00000 0.05717 0.05757 = 0.07178 -0.00271 0.00021 -0.00324 O46 4 0.548247 0.143081 0.969186 11.00000 0.05399 0.05626 = 0.08142 0.00594 -0.00380 -0.00581 C67 1 0.575369 0.386050 0.805967 11.00000 0.01925 0.01889 = 0.02843 -0.00149 0.00194 0.00449 C49 1 1.076373 0.113800 0.694008 11.00000 0.01221 0.01970 = 0.03576 -0.01351 0.00569 -0.00854 O42 4 0.047837 0.356697 0.530503 11.00000 0.05813 0.05915 = 0.07206 0.00502 0.00583 0.00553 C30 1 0.425362 0.113657 0.305915 11.00000 0.01496 0.02565 = 0.03257 0.01134 -0.00275 -0.00185 C24 1 0.634724 0.344881 0.320132 11.00000 0.02542 0.01285 = 0.04126 0.00209 0.00428 -0.00150 C62 1 0.366863 0.154281 0.820793 11.00000 0.02591 0.01372 = 0.04442 -0.00093 -0.00020 -0.00530 C11 1 -0.076691 0.386066 0.193548 11.00000 0.01969 0.02038 = 0.03443 0.00678 -0.00152 -0.00325 C51 1 0.774927 0.095376 0.648270 11.00000 0.02294 0.02067 = 0.03087 0.00257 0.00177 0.00221 C32 1 0.725950 0.095286 0.352026 11.00000 0.02300 0.01956 = 0.03071 0.00015 0.00057 -0.00341 C9 1 0.273995 0.310065 0.196538 11.00000 0.02725 0.01999 = 0.03026 0.00280 0.00166 -0.00179 AFIX 23 H9A 2 0.212261 0.295138 0.218618 11.00000 -1.20000 H9B 2 0.348986 0.345461 0.205645 11.00000 -1.20000 AFIX 0 C28 1 0.772912 0.190471 0.303780 11.00000 0.02714 0.02088 = 0.02614 0.00536 0.00284 0.00307 AFIX 23 H28A 2 0.710735 0.205171 0.281763 11.00000 -1.20000 H28B 2 0.847611 0.154947 0.294579 11.00000 -1.20000 AFIX 0 C43 1 0.865275 0.344879 0.679601 11.00000 0.02466 0.01528 = 0.04049 -0.00173 0.00610 0.00063 C53 1 0.723573 0.055204 0.565811 11.00000 0.03171 0.02488 = 0.02453 -0.00393 0.00424 -0.00361 C70 1 0.274398 0.405416 0.851989 11.00000 0.02637 0.01604 = 0.03401 0.00361 -0.00524 -0.00223 C29 1 0.508900 0.170922 0.329950 11.00000 0.02060 0.02783 = 0.03585 0.00335 -0.00290 0.00313 AFIX 23 H29A 2 0.494568 0.218970 0.318350 11.00000 -1.20000 H29B 2 0.465591 0.172080 0.355870 11.00000 -1.20000 AFIX 0 C41 1 1.069747 0.432158 0.662752 11.00000 0.01890 0.02050 = 0.04902 0.00285 -0.00219 -0.00384 C48 1 0.990552 0.170621 0.670471 11.00000 0.02413 0.02395 = 0.03238 -0.00484 -0.00149 -0.00443 AFIX 23 H48A 2 1.003178 0.218383 0.682452 11.00000 -1.20000 H48B 2 1.034537 0.172999 0.644646 11.00000 -1.20000 AFIX 0 C13 1 0.227022 0.404828 0.147998 11.00000 0.02306 0.01590 = 0.03033 -0.00141 0.00269 0.00268 C44 1 0.640812 0.257755 0.680775 11.00000 0.01915 0.02228 = 0.03837 -0.00051 0.00678 -0.00498 C10 1 0.009946 0.329228 0.169794 11.00000 0.02057 0.02582 = 0.03629 0.00184 0.00324 -0.00249 AFIX 23 H10C 2 -0.004176 0.281124 0.181345 11.00000 -1.20000 H10D 2 -0.031878 0.327871 0.143745 11.00000 -1.20000 AFIX 0 C74 1 0.233901 0.599891 0.934720 11.00000 0.03096 0.02883 = 0.02512 0.00156 -0.00080 -0.01030 C5 1 0.133773 0.155321 0.179378 11.00000 0.02327 0.01988 = 0.04666 0.00131 0.00148 0.00030 C66 1 0.139804 0.241557 0.819041 11.00000 0.01709 0.02148 = 0.04099 -0.00194 -0.00484 0.00236 C38 1 0.863103 -0.061778 0.462114 11.00000 0.02929 0.02526 = 0.02940 -0.00368 0.00785 -0.00493 C16 1 0.363864 0.561369 0.037686 11.00000 0.02992 0.03195 = 0.02474 0.00533 -0.00103 0.00145 C47 1 0.726653 0.190581 0.696363 11.00000 0.02552 0.01989 = 0.03360 -0.00439 -0.00079 -0.00223 AFIX 23 H47A 2 0.789539 0.205667 0.718153 11.00000 -1.20000 H47B 2 0.651920 0.155405 0.705919 11.00000 -1.20000 AFIX 0 C6 1 0.360179 0.242115 0.180637 11.00000 0.02367 0.02149 = 0.03340 0.00845 -0.00174 -0.00422 C36 1 0.768310 -0.099882 0.434950 11.00000 0.02882 0.02265 = 0.02881 0.00387 -0.00182 -0.00143 C34 1 0.776891 0.054837 0.434188 11.00000 0.03163 0.02929 = 0.02860 0.00008 0.00114 -0.00169 C54 1 0.636149 -0.060331 0.537721 11.00000 0.02608 0.04111 = 0.02454 -0.00312 0.00110 -0.00264 C45 1 0.524663 0.237005 0.649668 11.00000 0.02154 0.02975 = 0.04280 -0.00503 -0.00487 -0.00763 AFIX 137 H45A 2 0.476344 0.280611 0.639844 11.00000 -1.50000 H45B 2 0.447989 0.205249 0.660638 11.00000 -1.50000 H45C 2 0.576414 0.212070 0.628904 11.00000 -1.50000 AFIX 0 C68 1 0.489313 0.329487 0.829850 11.00000 0.01654 0.01800 = 0.03978 0.00104 0.00276 0.00249 AFIX 23 H68A 2 0.503380 0.281450 0.818269 11.00000 -1.20000 H68B 2 0.532517 0.327994 0.855755 11.00000 -1.20000 AFIX 0 C2 1 -0.070865 0.067788 0.162378 11.00000 0.02014 0.02208 = 0.04896 0.00406 -0.00457 -0.00481 C73 1 0.312523 0.560317 0.909418 11.00000 0.02783 0.03000 = 0.02545 0.00301 -0.00372 -0.00576 AFIX 43 H73 2 0.372562 0.584947 0.891262 11.00000 -1.20000 AFIX 0 C18 1 0.187575 0.560403 0.090687 11.00000 0.02462 0.02484 = 0.03587 -0.00480 -0.00126 0.00672 AFIX 43 H18 2 0.127517 0.585025 0.108823 11.00000 -1.20000 AFIX 0 C15 1 0.277491 0.444627 0.065665 11.00000 0.02610 0.03152 = 0.03082 -0.00175 -0.00427 -0.00366 C7 1 0.475758 0.263441 0.149755 11.00000 0.02290 0.02790 = 0.04025 -0.00392 0.00581 -0.00232 AFIX 137 H7A 2 0.525596 0.220138 0.140070 11.00000 -1.50000 H7B 2 0.551228 0.295752 0.160724 11.00000 -1.50000 H7C 2 0.423730 0.287954 0.128892 11.00000 -1.50000 AFIX 0 C26 1 0.859843 0.258245 0.318775 11.00000 0.01980 0.02339 = 0.03624 -0.00481 0.00521 0.00022 O45 4 0.310598 0.244343 0.962404 11.00000 0.10246 0.04428 = 0.12770 0.00442 -0.04677 0.00109 C65 1 0.227399 0.309677 0.803812 11.00000 0.02697 0.02043 = 0.03441 0.00253 0.00444 0.00773 AFIX 23 H65A 2 0.290410 0.294960 0.781935 11.00000 -1.20000 H65B 2 0.153013 0.345210 0.794455 11.00000 -1.20000 AFIX 0 C57 1 0.813203 -0.061204 0.590555 11.00000 0.02672 0.02848 = 0.02887 -0.00322 0.00602 0.00877 AFIX 43 H57 2 0.873775 -0.086237 0.608423 11.00000 -1.20000 AFIX 0 C14 1 0.111179 0.442881 0.120900 11.00000 0.02221 0.02293 = 0.03823 0.00674 -0.00025 0.00429 AFIX 23 H14A 2 0.047281 0.406163 0.108489 11.00000 -1.20000 H14B 2 0.044812 0.474796 0.135970 11.00000 -1.20000 AFIX 0 C55 1 0.733608 -0.099932 0.565112 11.00000 0.03329 0.03031 = 0.02557 -0.00261 -0.00016 0.00352 C72 1 0.223474 0.444529 0.933849 11.00000 0.03720 0.02479 = 0.03029 -0.00442 -0.00224 -0.00465 C71 1 0.390259 0.442137 0.879090 11.00000 0.02567 0.02554 = 0.03474 -0.00130 0.00221 0.00153 AFIX 23 H71A 2 0.452968 0.404913 0.891540 11.00000 -1.20000 H71B 2 0.457664 0.473876 0.864189 11.00000 -1.20000 AFIX 0 C75 1 0.136164 0.561058 0.962407 11.00000 0.03826 0.03074 = 0.03084 -0.00122 -0.00408 -0.00221 C69 1 0.822718 0.431417 0.789640 11.00000 0.02511 0.02915 = 0.04518 -0.00124 0.00850 -0.00759 AFIX 137 H69A 2 0.828956 0.414606 0.763319 11.00000 -1.50000 H69B 2 0.924052 0.433165 0.800627 11.00000 -1.50000 H69C 2 0.777958 0.479591 0.790178 11.00000 -1.50000 AFIX 0 C64 1 0.024646 0.263463 0.850823 11.00000 0.02550 0.03175 = 0.04410 -0.00152 0.00658 -0.00020 AFIX 137 H64A 2 -0.030178 0.220727 0.859461 11.00000 -1.50000 H64B 2 -0.046876 0.298661 0.840601 11.00000 -1.50000 H64C 2 0.079057 0.284684 0.872259 11.00000 -1.50000 AFIX 0 C27 1 0.976177 0.236687 0.349904 11.00000 0.01941 0.02629 = 0.04527 -0.00012 -0.00213 -0.00431 AFIX 137 H27A 2 1.027095 0.279890 0.359295 11.00000 -1.50000 H27B 2 1.050798 0.203730 0.339032 11.00000 -1.50000 H27C 2 0.923788 0.212887 0.370957 11.00000 -1.50000 AFIX 0 C35 1 0.687467 -0.060909 0.409587 11.00000 0.02504 0.02877 = 0.03298 -0.00542 0.00305 -0.00451 AFIX 43 H35 2 0.626429 -0.085869 0.391835 11.00000 -1.20000 AFIX 0 O32 4 0.188198 0.244810 0.038124 11.00000 0.09765 0.04406 = 0.12658 -0.00545 -0.05085 0.00168 C58 1 0.572502 0.068283 0.837563 11.00000 0.02071 0.02540 = 0.05282 0.00792 0.00185 0.00378 C63 1 0.060426 0.206031 0.784979 11.00000 0.04001 0.02484 = 0.05119 -0.00443 -0.01615 -0.00104 AFIX 137 H63A 2 0.135833 0.191413 0.766156 11.00000 -1.50000 H63B 2 -0.009594 0.240433 0.773427 11.00000 -1.50000 H63C 2 0.004569 0.163657 0.793695 11.00000 -1.50000 AFIX 0 O36 4 0.810396 0.255501 0.538143 11.00000 0.10064 0.03926 = 0.12573 0.00757 0.05002 -0.00295 C22 1 0.428901 0.432058 0.337201 11.00000 0.02476 0.03210 = 0.04287 0.00093 -0.00153 0.00757 C17 1 0.267066 0.600040 0.065091 11.00000 0.03525 0.02367 = 0.03159 0.00030 0.00349 0.00300 C31 1 0.177126 0.069031 0.289310 11.00000 0.02836 0.03155 = 0.04829 -0.00613 -0.00812 -0.01326 AFIX 137 H31A 2 0.175303 0.085745 0.262909 11.00000 -1.50000 H31B 2 0.074301 0.068509 0.299475 11.00000 -1.50000 H31C 2 0.219348 0.020364 0.290333 11.00000 -1.50000 AFIX 0 C52 1 0.890761 0.057198 0.621329 11.00000 0.02724 0.02837 = 0.03304 -0.00423 0.00208 0.00091 AFIX 23 H52A 2 0.955534 0.093732 0.608975 11.00000 -1.20000 H52B 2 0.956211 0.024861 0.636409 11.00000 -1.20000 AFIX 0 C8 1 0.440058 0.206176 0.215053 11.00000 0.03127 0.03691 = 0.04938 0.00780 -0.01122 -0.00520 AFIX 137 H8C 2 0.364320 0.190020 0.233446 11.00000 -1.50000 H8D 2 0.507331 0.241056 0.227154 11.00000 -1.50000 H8E 2 0.498874 0.164798 0.206253 11.00000 -1.50000 AFIX 0 C46 1 0.560841 0.293691 0.715281 11.00000 0.03519 0.02957 = 0.04889 -0.00771 0.01649 0.00336 AFIX 137 H46A 2 0.635998 0.306537 0.734476 11.00000 -1.50000 H46B 2 0.487994 0.259978 0.726280 11.00000 -1.50000 H46C 2 0.508214 0.337167 0.706795 11.00000 -1.50000 AFIX 0 C50 1 1.322794 0.069186 0.710539 11.00000 0.02133 0.03496 = 0.05023 0.00665 -0.00050 0.01013 AFIX 137 H50A 2 1.325531 0.085955 0.736903 11.00000 -1.50000 H50B 2 1.425311 0.068400 0.700182 11.00000 -1.50000 H50C 2 1.280154 0.020615 0.709688 11.00000 -1.50000 AFIX 0 C33 1 0.610055 0.056898 0.378800 11.00000 0.01842 0.02959 = 0.03904 0.00325 -0.00206 -0.00146 AFIX 23 H33A 2 0.544474 0.093275 0.390993 11.00000 -1.20000 H33B 2 0.545440 0.024366 0.363669 11.00000 -1.20000 AFIX 0 O35 4 0.688445 0.255126 0.462167 11.00000 0.10487 0.04769 = 0.12317 -0.00307 0.04121 -0.00020 C25 1 0.941265 0.293433 0.284640 11.00000 0.03990 0.03174 = 0.04659 0.01321 0.01277 -0.00188 AFIX 137 H25A 2 0.866992 0.307093 0.265358 11.00000 -1.50000 H25B 2 1.013051 0.259139 0.273710 11.00000 -1.50000 H25C 2 0.995347 0.336364 0.293223 11.00000 -1.50000 AFIX 0 C12 1 -0.324248 0.431832 0.210440 11.00000 0.02933 0.03197 = 0.05094 -0.00151 0.01286 0.01020 AFIX 137 H12A 2 -0.324353 0.416218 0.237031 11.00000 -1.50000 H12B 2 -0.427435 0.430913 0.200574 11.00000 -1.50000 H12C 2 -0.284311 0.480851 0.208727 11.00000 -1.50000 AFIX 0 C42 1 1.191983 0.372677 0.660837 11.00000 0.02968 0.03419 = 0.08229 -0.00142 0.00495 0.00269 AFIX 137 H42A 2 1.177088 0.338648 0.681778 11.00000 -1.50000 H42B 2 1.291997 0.394610 0.662943 11.00000 -1.50000 H42C 2 1.184127 0.347176 0.636581 11.00000 -1.50000 AFIX 0 C20 1 0.423725 0.473614 0.299629 11.00000 0.04288 0.03992 = 0.05876 0.01044 0.00049 0.01411 AFIX 137 H20A 2 0.512154 0.504956 0.297742 11.00000 -1.50000 H20B 2 0.331934 0.502876 0.298713 11.00000 -1.50000 H20C 2 0.423775 0.439589 0.278397 11.00000 -1.50000 AFIX 0 C39 1 1.084749 0.484566 0.629197 11.00000 0.03729 0.04083 = 0.06342 0.01147 -0.00218 -0.01357 AFIX 137 H39A 2 1.073753 0.458137 0.605299 11.00000 -1.50000 H39B 2 1.184005 0.507581 0.629950 11.00000 -1.50000 H39C 2 1.006059 0.521407 0.630938 11.00000 -1.50000 AFIX 0 C56 1 0.740644 -0.182036 0.562708 11.00000 0.06041 0.02223 = 0.04233 -0.00115 -0.01462 0.00636 AFIX 137 H56A 2 0.802765 -0.200678 0.583504 11.00000 -1.50000 H56B 2 0.785039 -0.196178 0.538340 11.00000 -1.50000 H56C 2 0.638633 -0.201824 0.564741 11.00000 -1.50000 AFIX 0 C59 1 0.576340 0.026576 0.799610 11.00000 0.04424 0.03451 = 0.06641 -0.00770 0.00000 0.02058 AFIX 137 H59A 2 0.485252 -0.002871 0.797367 11.00000 -1.50000 H59B 2 0.665410 -0.004570 0.798983 11.00000 -1.50000 H59C 2 0.580789 0.060738 0.778425 11.00000 -1.50000 AFIX 0 C76 1 0.242008 0.682321 0.937530 11.00000 0.06826 0.02877 = 0.04208 -0.00073 0.01633 -0.00974 AFIX 137 H76A 2 0.306400 0.701018 0.917167 11.00000 -1.50000 H76B 2 0.284261 0.695911 0.962199 11.00000 -1.50000 H76C 2 0.140529 0.702559 0.935014 11.00000 -1.50000 AFIX 0 C61 1 0.587062 0.016246 0.871652 11.00000 0.03653 0.04747 = 0.05849 0.00652 -0.00448 0.00770 AFIX 137 H61A 2 0.588910 0.043889 0.895324 11.00000 -1.50000 H61B 2 0.680587 -0.011433 0.869283 11.00000 -1.50000 H61C 2 0.500917 -0.016695 0.871952 11.00000 -1.50000 AFIX 0 C3 1 -0.086500 0.015562 0.128783 11.00000 0.03169 0.04216 = 0.06170 -0.00814 0.00331 -0.00781 AFIX 137 H3A 2 -0.082304 0.042576 0.104892 11.00000 -1.50000 H3B 2 -0.183132 -0.009695 0.130581 11.00000 -1.50000 H3C 2 -0.004027 -0.019476 0.129467 11.00000 -1.50000 AFIX 0 C40 1 1.076006 0.473878 0.700547 11.00000 0.04858 0.03758 = 0.06136 -0.00822 0.00229 -0.01796 AFIX 137 H40A 2 0.987177 0.504943 0.702678 11.00000 -1.50000 H40B 2 1.167373 0.503418 0.701192 11.00000 -1.50000 H40C 2 1.077446 0.439782 0.721786 11.00000 -1.50000 AFIX 0 C21 1 0.308400 0.372012 0.339600 11.00000 0.02416 0.03564 = 0.09028 -0.00136 0.00171 -0.00546 AFIX 137 H21A 2 0.308997 0.344106 0.316009 11.00000 -1.50000 H21B 2 0.208783 0.393704 0.343246 11.00000 -1.50000 H21C 2 0.331172 0.340232 0.361063 11.00000 -1.50000 AFIX 0 C23 1 0.414377 0.484840 0.371153 11.00000 0.03815 0.04578 = 0.05765 -0.01074 0.00006 0.00838 AFIX 137 H23A 2 0.417710 0.457759 0.395031 11.00000 -1.50000 H23B 2 0.318452 0.510748 0.369386 11.00000 -1.50000 H23C 2 0.497802 0.519321 0.370470 11.00000 -1.50000 AFIX 0 C19 1 0.260909 0.682469 0.062429 11.00000 0.05724 0.02880 = 0.04757 0.00156 0.01468 0.00090 AFIX 137 H19A 2 0.210081 0.696550 0.038870 11.00000 -1.50000 H19B 2 0.363599 0.701811 0.062500 11.00000 -1.50000 H19C 2 0.205122 0.701618 0.084220 11.00000 -1.50000 AFIX 0 C4 1 -0.192622 0.127498 0.159923 11.00000 0.02702 0.02985 = 0.09391 0.00106 -0.00079 -0.00161 AFIX 137 H4C 2 -0.184730 0.158991 0.182126 11.00000 -1.50000 H4D 2 -0.292828 0.105421 0.159343 11.00000 -1.50000 H4E 2 -0.177220 0.155801 0.136748 11.00000 -1.50000 AFIX 0 C60 1 0.691702 0.127359 0.839776 11.00000 0.02801 0.03557 = 0.09337 0.00535 -0.00635 -0.00265 AFIX 137 H60A 2 0.686745 0.157222 0.816861 11.00000 -1.50000 H60B 2 0.791868 0.105465 0.841708 11.00000 -1.50000 H60C 2 0.672958 0.157286 0.862179 11.00000 -1.50000 AFIX 0 C37 1 0.759572 -0.182186 0.437276 11.00000 0.06512 0.02833 = 0.05415 0.00339 -0.01227 0.00259 AFIX 137 H37A 2 0.710334 -0.196242 0.461075 11.00000 -1.50000 H37B 2 0.861550 -0.202367 0.436493 11.00000 -1.50000 H37C 2 0.701252 -0.200507 0.415746 11.00000 -1.50000 AFIX 0 C1 1 -0.077148 0.026131 0.200785 11.00000 0.04675 0.03590 = 0.06879 0.00246 0.00385 -0.01301 AFIX 137 H1A 2 0.013193 -0.003794 0.203368 11.00000 -1.50000 H1B 2 -0.166919 -0.004517 0.201309 11.00000 -1.50000 H1C 2 -0.081670 0.060513 0.221826 11.00000 -1.50000 AFIX 0 HKLF 4 REM tri_a.res in P-1 REM R1 = 0.1058 for 7947 Fo > 4sig(Fo) and 0.3769 for all 32012 data REM 1289 parameters refined using 0 restraints END WGHT 0.0930 0.0000 REM Highest difference peak 0.483, deepest hole -0.449, 1-sigma level 0.118 Q1 1 0.5157 0.3776 0.5730 11.00000 0.05 0.48 Q2 1 0.6274 0.2782 0.4201 11.00000 0.05 0.48 Q3 1 0.6258 0.2390 0.5216 11.00000 0.05 0.47 Q4 1 0.7744 0.1352 0.0299 11.00000 0.05 0.46 Q5 1 0.0929 0.0113 0.0020 11.00000 0.05 0.46 Q6 1 0.1561 -0.0243 0.0425 11.00000 0.05 0.46 Q7 1 0.7760 0.4225 0.4846 11.00000 0.05 0.46 Q8 1 0.3696 0.2652 0.0242 11.00000 0.05 0.45 Q9 1 0.3712 0.2239 0.9148 11.00000 0.05 0.45 Q10 1 0.7908 0.5310 0.4822 11.00000 0.05 0.44 Q11 1 0.3446 0.2663 1.0079 11.00000 0.05 0.44 Q12 1 0.4801 0.2563 1.0070 11.00000 0.05 0.44 Q13 1 0.1388 0.2226 -0.0049 11.00000 0.05 0.44 Q14 1 0.6470 0.3064 0.5624 11.00000 0.05 0.44 Q15 1 0.2924 0.0894 0.0670 11.00000 0.05 0.44 Q16 1 0.9188 0.2393 0.4904 11.00000 0.05 0.44 Q17 1 0.5548 0.3942 0.4818 11.00000 0.05 0.43 Q18 1 0.9040 0.2693 0.4909 11.00000 0.05 0.43 Q19 1 0.2312 0.0935 0.9363 11.00000 0.05 0.43 Q20 1 0.6854 0.4078 0.5602 11.00000 0.05 0.43 ; _shelx_res_checksum 60745 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 O28 O 0.3574(4) 0.4284(2) 0.15042(12) 0.0264(10) Uani 1 1 d . . . . . O5 O 0.1422(4) 0.4285(2) 0.84965(12) 0.0283(10) Uani 1 1 d . . . . . O10 O 0.6424(4) 0.0718(2) 0.65051(12) 0.0280(10) Uani 1 1 d . . . . . O20 O 0.8577(4) 0.0714(2) 0.34949(12) 0.0281(10) Uani 1 1 d . . . . . O15 O 0.2723(4) 0.1185(2) 0.31249(13) 0.0311(10) Uani 1 1 d . . . . . O49 O 0.4175(4) 0.1007(2) 0.84387(13) 0.0310(10) Uani 1 1 d . . . . . O18 O 0.5826(4) 0.3990(2) 0.34376(12) 0.0301(10) Uani 1 1 d . . . . . O4 O 0.7274(4) 0.3812(2) 0.81210(13) 0.0307(10) Uani 1 1 d . . . . . O8 O 1.2274(4) 0.1189(2) 0.68744(12) 0.0297(10) Uani 1 1 d . . . . . O2 O 0.4171(5) 0.1712(2) 0.78885(13) 0.0334(10) Uani 1 1 d . . . . . O24 O 0.0821(5) 0.1708(2) 0.21115(13) 0.0321(10) Uani 1 1 d . . . . . O14 O 0.9175(4) 0.3992(2) 0.65611(13) 0.0312(10) Uani 1 1 d . . . . . O17 O 0.5818(5) 0.3289(2) 0.28892(13) 0.0334(10) Uani 1 1 d . . . . . O16 O 0.4837(4) 0.0711(2) 0.28404(13) 0.0331(11) Uani 1 1 d . . . . . O13 O 0.9170(5) 0.3291(2) 0.71096(14) 0.0327(10) Uani 1 1 d . . . . . O25 O 0.0832(4) 0.1008(2) 0.15639(13) 0.0325(10) Uani 1 1 d . . . . . O3 O 0.5159(4) 0.4287(2) 0.78412(13) 0.0323(10) Uani 1 1 d . . . . . O22 O -0.2275(4) 0.3822(2) 0.18752(12) 0.0311(10) Uani 1 1 d . . . . . O23 O -0.0161(4) 0.4289(2) 0.21565(13) 0.0326(10) Uani 1 1 d . . . . . O11 O 0.7193(5) 0.1220(2) 0.56694(13) 0.0380(11) Uani 1 1 d . . . . . O27 O 0.2814(5) 0.3778(2) 0.06707(13) 0.0364(11) Uani 1 1 d . . . . . O9 O 1.0162(4) 0.0715(2) 0.71567(13) 0.0328(10) Uani 1 1 d . . . . . O6 O 0.2186(5) 0.3776(2) 0.93302(13) 0.0377(11) Uani 1 1 d . . . . . O12 O 0.5531(5) -0.0907(2) 0.51299(13) 0.0379(11) Uani 1 1 d . . . . . O7 O 0.0525(5) 0.5913(2) 0.98683(13) 0.0380(11) Uani 1 1 d . . . . . O19 O 0.7804(5) 0.1222(2) 0.43328(13) 0.0395(11) Uani 1 1 d . . . . . O21 O 0.9481(5) -0.0911(2) 0.48696(13) 0.0387(11) Uani 1 1 d . . . . . O26 O 0.4475(5) 0.5914(2) 0.01308(13) 0.0387(11) Uani 1 1 d . . . . . N12 N 0.6407(5) 0.0145(3) 0.54013(14) 0.0268(12) Uani 1 1 d . . . . . H12 H 0.5854 0.0384 0.5237 0.032 Uiso 1 1 calc R U . . . N10 N 0.8262(5) 0.1538(2) 0.66751(14) 0.0240(11) Uani 1 1 d . . . . . N15 N 0.3258(5) 0.3453(2) 0.83249(14) 0.0232(11) Uani 1 1 d . . . . . N7 N 0.6730(5) 0.1544(2) 0.33223(14) 0.0233(11) Uani 1 1 d . . . . . N106 N 0.7543(5) 0.3111(2) 0.33823(15) 0.0265(12) Uani 1 1 d . . . . . H106 H 0.7699 0.3209 0.3623 0.032 Uiso 1 1 calc R U . . . O44 O 0.1521(5) 0.1412(3) 0.91997(14) 0.0488(13) Uani 1 1 d . . . . . N3 N 0.1734(5) 0.3460(2) 0.16792(14) 0.0236(11) Uani 1 1 d . . . . . N1 N 0.3607(5) 0.4854(2) 0.04023(14) 0.0266(12) Uani 1 1 d . . . . . H1 H 0.4172 0.4617 0.0240 0.032 Uiso 1 1 calc R U . . . N13 N 0.1402(5) 0.4854(3) 0.95961(14) 0.0282(12) Uani 1 1 d . . . . . H13 H 0.0842 0.4615 0.9758 0.034 Uiso 1 1 calc R U . . . N105 N 0.2544(5) 0.1890(2) 0.16198(15) 0.0244(11) Uani 1 1 d . . . . . H105 H 0.2712 0.1787 0.1380 0.029 Uiso 1 1 calc R U . . . N108 N 0.2458(5) 0.1888(2) 0.83812(15) 0.0271(12) Uani 1 1 d . . . . . H108 H 0.2294 0.1791 0.8622 0.033 Uiso 1 1 calc R U . . . N2 N 0.1899(5) 0.4855(3) 0.09163(14) 0.0251(12) Uani 1 1 d . . . . . N107 N 0.7459(5) 0.3112(2) 0.66224(15) 0.0261(12) Uani 1 1 d . . . . . H107 H 0.7294 0.3217 0.6383 0.031 Uiso 1 1 calc R U . . . O37 O 0.6525(5) 0.3584(3) 0.58001(14) 0.0502(13) Uani 1 1 d . . . . . N14 N 0.3107(5) 0.4850(2) 0.90839(14) 0.0247(11) Uani 1 1 d . . . . . N11 N 0.8108(5) 0.0150(3) 0.59191(14) 0.0258(12) Uani 1 1 d . . . . . O48 O 0.3207(6) 0.0355(3) 0.96342(15) 0.0542(14) Uani 1 1 d . . . . . N5 N 0.8603(5) 0.0142(3) 0.45953(14) 0.0279(12) Uani 1 1 d . . . . . H5 H 0.9171 0.0379 0.4756 0.033 Uiso 1 1 calc R U . . . O34 O 0.8472(5) 0.3590(3) 0.42008(14) 0.0492(13) Uani 1 1 d . . . . . O31 O 0.3482(5) 0.1409(3) 0.07989(14) 0.0500(13) Uani 1 1 d . . . . . O39 O 0.6781(6) 0.4643(3) 0.46303(15) 0.0527(13) Uani 1 1 d . . . . . O41 O 0.3607(5) 0.3834(3) 0.54633(16) 0.0566(14) Uani 1 1 d . . . . . N6 N 0.6895(5) 0.0152(3) 0.40825(14) 0.0268(12) Uani 1 1 d . . . . . O30 O 0.6406(6) 0.1165(3) 0.04655(16) 0.0598(15) Uani 1 1 d . . . . . O33 O 0.1795(6) 0.0356(3) 0.03676(15) 0.0553(14) Uani 1 1 d . . . . . O40 O 0.4503(6) 0.3568(3) 0.46958(17) 0.0635(15) Uani 1 1 d . . . . . O38 O 0.8214(6) 0.4637(3) 0.53666(15) 0.0557(14) Uani 1 1 d . . . . . O47 O 0.8610(6) 0.1162(3) 0.95360(16) 0.0597(15) Uani 1 1 d . . . . . O29 O 0.9513(6) 0.1434(3) 0.03053(17) 0.0633(15) Uani 1 1 d . . . . . O43 O 0.1390(6) 0.3835(3) 0.45390(16) 0.0622(15) Uani 1 1 d . . . . . O46 O 0.5482(6) 0.1431(3) 0.96919(17) 0.0639(15) Uani 1 1 d . . . . . C67 C 0.5754(6) 0.3860(3) 0.80597(18) 0.0222(13) Uani 1 1 d . . . . . C49 C 1.0764(6) 0.1138(3) 0.69401(18) 0.0225(14) Uani 1 1 d . . . . . O42 O 0.0478(6) 0.3567(3) 0.53050(16) 0.0631(15) Uani 1 1 d . . . . . C30 C 0.4254(6) 0.1137(3) 0.30592(18) 0.0244(14) Uani 1 1 d . . . . . C24 C 0.6347(7) 0.3449(3) 0.3201(2) 0.0265(14) Uani 1 1 d . . . . . C62 C 0.3669(7) 0.1543(3) 0.8208(2) 0.0280(15) Uani 1 1 d . . . . . C11 C -0.0767(6) 0.3861(3) 0.19355(18) 0.0248(14) Uani 1 1 d . . . . . C51 C 0.7749(6) 0.0954(3) 0.64827(18) 0.0248(14) Uani 1 1 d . . . . . C32 C 0.7260(6) 0.0953(3) 0.35203(18) 0.0244(14) Uani 1 1 d . . . . . C9 C 0.2740(6) 0.3101(3) 0.19654(18) 0.0258(14) Uani 1 1 d . . . . . H9A H 0.2123 0.2951 0.2186 0.031 Uiso 1 1 calc R U . . . H9B H 0.3490 0.3455 0.2056 0.031 Uiso 1 1 calc R U . . . C28 C 0.7729(6) 0.1905(3) 0.30378(17) 0.0247(14) Uani 1 1 d . . . . . H28A H 0.7107 0.2052 0.2818 0.030 Uiso 1 1 calc R U . . . H28B H 0.8476 0.1549 0.2946 0.030 Uiso 1 1 calc R U . . . C43 C 0.8653(7) 0.3449(3) 0.6796(2) 0.0268(14) Uani 1 1 d . . . . . C53 C 0.7236(7) 0.0552(3) 0.56581(18) 0.0270(14) Uani 1 1 d . . . . . C70 C 0.2744(7) 0.4054(3) 0.85199(18) 0.0255(14) Uani 1 1 d . . . . . C29 C 0.5089(6) 0.1709(3) 0.32995(19) 0.0281(14) Uani 1 1 d . . . . . H29A H 0.4946 0.2190 0.3183 0.034 Uiso 1 1 calc R U . . . H29B H 0.4656 0.1721 0.3559 0.034 Uiso 1 1 calc R U . . . C41 C 1.0697(6) 0.4322(3) 0.66275(19) 0.0295(15) Uani 1 1 d . . . . . C48 C 0.9906(6) 0.1706(3) 0.67047(18) 0.0268(14) Uani 1 1 d . . . . . H48A H 1.0032 0.2184 0.6825 0.032 Uiso 1 1 calc R U . . . H48B H 1.0345 0.1730 0.6446 0.032 Uiso 1 1 calc R U . . . C13 C 0.2270(6) 0.4048(3) 0.14800(17) 0.0231(13) Uani 1 1 d . . . . . C44 C 0.6408(6) 0.2578(3) 0.68078(18) 0.0266(14) Uani 1 1 d . . . . . C10 C 0.0099(6) 0.3292(3) 0.16979(19) 0.0276(14) Uani 1 1 d . . . . . H10C H -0.0042 0.2811 0.1813 0.033 Uiso 1 1 calc R U . . . H10D H -0.0319 0.3279 0.1437 0.033 Uiso 1 1 calc R U . . . C74 C 0.2339(7) 0.5999(3) 0.93472(18) 0.0283(15) Uani 1 1 d . . . . . C5 C 0.1338(7) 0.1553(3) 0.1794(2) 0.0299(15) Uani 1 1 d . . . . . C66 C 0.1398(6) 0.2416(3) 0.81904(18) 0.0265(14) Uani 1 1 d . . . . . C38 C 0.8631(7) -0.0618(3) 0.46211(19) 0.0280(15) Uani 1 1 d . . . . . C16 C 0.3639(7) 0.5614(3) 0.03769(18) 0.0289(15) Uani 1 1 d . . . . . C47 C 0.7267(6) 0.1906(3) 0.69636(18) 0.0263(14) Uani 1 1 d . . . . . H47A H 0.7895 0.2057 0.7182 0.032 Uiso 1 1 calc R U . . . H47B H 0.6519 0.1554 0.7059 0.032 Uiso 1 1 calc R U . . . C6 C 0.3602(6) 0.2421(3) 0.18064(18) 0.0262(14) Uani 1 1 d . . . . . C36 C 0.7683(7) -0.0999(3) 0.43495(18) 0.0268(14) Uani 1 1 d . . . . . C34 C 0.7769(7) 0.0548(3) 0.43419(19) 0.0298(15) Uani 1 1 d . . . . . C54 C 0.6361(7) -0.0603(4) 0.53772(18) 0.0306(15) Uani 1 1 d . . . . . C45 C 0.5247(6) 0.2370(3) 0.64967(19) 0.0314(15) Uani 1 1 d . . . . . H45A H 0.4763 0.2806 0.6398 0.047 Uiso 1 1 calc R U . . . H45B H 0.4480 0.2052 0.6606 0.047 Uiso 1 1 calc R U . . . H45C H 0.5764 0.2121 0.6289 0.047 Uiso 1 1 calc R U . . . C68 C 0.4893(6) 0.3295(3) 0.82985(19) 0.0248(14) Uani 1 1 d . . . . . H68A H 0.5034 0.2815 0.8183 0.030 Uiso 1 1 calc R U . . . H68B H 0.5325 0.3280 0.8558 0.030 Uiso 1 1 calc R U . . . C2 C -0.0709(6) 0.0678(3) 0.1624(2) 0.0304(15) Uani 1 1 d . . . . . C73 C 0.3125(7) 0.5603(3) 0.90942(18) 0.0278(14) Uani 1 1 d . . . . . H73 H 0.3726 0.5849 0.8913 0.033 Uiso 1 1 calc R U . . . C18 C 0.1876(6) 0.5604(3) 0.09069(19) 0.0284(15) Uani 1 1 d . . . . . H18 H 0.1275 0.5850 0.1088 0.034 Uiso 1 1 calc R U . . . C15 C 0.2775(7) 0.4446(3) 0.06567(19) 0.0295(15) Uani 1 1 d . . . . . C7 C 0.4758(6) 0.2634(3) 0.14976(19) 0.0304(15) Uani 1 1 d . . . . . H7A H 0.5256 0.2201 0.1401 0.046 Uiso 1 1 calc R U . . . H7B H 0.5512 0.2958 0.1607 0.046 Uiso 1 1 calc R U . . . H7C H 0.4237 0.2880 0.1289 0.046 Uiso 1 1 calc R U . . . C26 C 0.8598(6) 0.2582(3) 0.31877(18) 0.0265(14) Uani 1 1 d . . . . . O45 O 0.3106(7) 0.2443(3) 0.9624(2) 0.091(2) Uani 1 1 d . . . . . C65 C 0.2274(7) 0.3097(3) 0.80381(18) 0.0273(14) Uani 1 1 d . . . . . H65A H 0.2904 0.2950 0.7819 0.033 Uiso 1 1 calc R U . . . H65B H 0.1530 0.3452 0.7945 0.033 Uiso 1 1 calc R U . . . C57 C 0.8132(7) -0.0612(3) 0.59056(18) 0.0280(14) Uani 1 1 d . . . . . H57 H 0.8738 -0.0862 0.6084 0.034 Uiso 1 1 calc R U . . . C14 C 0.1112(6) 0.4429(3) 0.12090(18) 0.0278(14) Uani 1 1 d . . . . . H14A H 0.0473 0.4062 0.1085 0.033 Uiso 1 1 calc R U . . . H14B H 0.0448 0.4748 0.1360 0.033 Uiso 1 1 calc R U . . . C55 C 0.7336(7) -0.0999(3) 0.56511(18) 0.0297(15) Uani 1 1 d . . . . . C72 C 0.2235(7) 0.4445(3) 0.93385(19) 0.0308(15) Uani 1 1 d . . . . . C71 C 0.3903(6) 0.4421(3) 0.87909(18) 0.0287(14) Uani 1 1 d . . . . . H71A H 0.4530 0.4049 0.8915 0.034 Uiso 1 1 calc R U . . . H71B H 0.4577 0.4739 0.8642 0.034 Uiso 1 1 calc R U . . . C75 C 0.1362(7) 0.5611(3) 0.96241(19) 0.0333(16) Uani 1 1 d . . . . . C69 C 0.8227(7) 0.4314(3) 0.7896(2) 0.0331(16) Uani 1 1 d . . . . . H69A H 0.8290 0.4146 0.7633 0.050 Uiso 1 1 calc R U . . . H69B H 0.9241 0.4332 0.8006 0.050 Uiso 1 1 calc R U . . . H69C H 0.7780 0.4796 0.7902 0.050 Uiso 1 1 calc R U . . . C64 C 0.0246(7) 0.2635(3) 0.85082(19) 0.0338(16) Uani 1 1 d . . . . . H64A H -0.0302 0.2207 0.8595 0.051 Uiso 1 1 calc R U . . . H64B H -0.0469 0.2987 0.8406 0.051 Uiso 1 1 calc R U . . . H64C H 0.0791 0.2847 0.8723 0.051 Uiso 1 1 calc R U . . . C27 C 0.9762(6) 0.2367(3) 0.34990(19) 0.0303(15) Uani 1 1 d . . . . . H27A H 1.0271 0.2799 0.3593 0.045 Uiso 1 1 calc R U . . . H27B H 1.0508 0.2037 0.3390 0.045 Uiso 1 1 calc R U . . . H27C H 0.9238 0.2129 0.3710 0.045 Uiso 1 1 calc R U . . . C35 C 0.6875(7) -0.0609(3) 0.40959(19) 0.0289(15) Uani 1 1 d . . . . . H35 H 0.6264 -0.0859 0.3918 0.035 Uiso 1 1 calc R U . . . O32 O 0.1882(7) 0.2448(3) 0.0381(2) 0.089(2) Uani 1 1 d . . . . . C58 C 0.5725(6) 0.0683(3) 0.8376(2) 0.0330(16) Uani 1 1 d . . . . . C63 C 0.0604(7) 0.2060(3) 0.7850(2) 0.0387(17) Uani 1 1 d . . . . . H63A H 0.1358 0.1914 0.7662 0.058 Uiso 1 1 calc R U . . . H63B H -0.0096 0.2404 0.7734 0.058 Uiso 1 1 calc R U . . . H63C H 0.0046 0.1637 0.7937 0.058 Uiso 1 1 calc R U . . . O36 O 0.8104(7) 0.2555(3) 0.5381(2) 0.089(2) Uani 1 1 d . . . . . C22 C 0.4289(7) 0.4321(3) 0.3372(2) 0.0332(16) Uani 1 1 d . . . . . C17 C 0.2671(7) 0.6000(3) 0.06509(19) 0.0302(15) Uani 1 1 d . . . . . C31 C 0.1771(7) 0.0690(3) 0.2893(2) 0.0361(16) Uani 1 1 d . . . . . H31A H 0.1753 0.0857 0.2629 0.054 Uiso 1 1 calc R U . . . H31B H 0.0743 0.0685 0.2995 0.054 Uiso 1 1 calc R U . . . H31C H 0.2193 0.0204 0.2903 0.054 Uiso 1 1 calc R U . . . C52 C 0.8908(7) 0.0572(3) 0.62133(18) 0.0295(15) Uani 1 1 d . . . . . H52A H 0.9555 0.0937 0.6090 0.035 Uiso 1 1 calc R U . . . H52B H 0.9562 0.0249 0.6364 0.035 Uiso 1 1 calc R U . . . C8 C 0.4401(7) 0.2062(4) 0.2151(2) 0.0392(17) Uani 1 1 d . . . . . H8C H 0.3643 0.1900 0.2334 0.059 Uiso 1 1 calc R U . . . H8D H 0.5073 0.2411 0.2272 0.059 Uiso 1 1 calc R U . . . H8E H 0.4989 0.1648 0.2063 0.059 Uiso 1 1 calc R U . . . C46 C 0.5608(7) 0.2937(3) 0.7153(2) 0.0379(17) Uani 1 1 d . . . . . H46A H 0.6360 0.3065 0.7345 0.057 Uiso 1 1 calc R U . . . H46B H 0.4880 0.2600 0.7263 0.057 Uiso 1 1 calc R U . . . H46C H 0.5082 0.3372 0.7068 0.057 Uiso 1 1 calc R U . . . C50 C 1.3228(6) 0.0692(3) 0.7105(2) 0.0355(16) Uani 1 1 d . . . . . H50A H 1.3255 0.0860 0.7369 0.053 Uiso 1 1 calc R U . . . H50B H 1.4253 0.0684 0.7002 0.053 Uiso 1 1 calc R U . . . H50C H 1.2802 0.0206 0.7097 0.053 Uiso 1 1 calc R U . . . C33 C 0.6101(6) 0.0569(3) 0.37880(18) 0.0290(15) Uani 1 1 d . . . . . H33A H 0.5445 0.0933 0.3910 0.035 Uiso 1 1 calc R U . . . H33B H 0.5454 0.0244 0.3637 0.035 Uiso 1 1 calc R U . . . O35 O 0.6884(7) 0.2551(3) 0.4622(2) 0.092(2) Uani 1 1 d . . . . . C25 C 0.9413(7) 0.2934(3) 0.2846(2) 0.0394(17) Uani 1 1 d . . . . . H25A H 0.8670 0.3071 0.2654 0.059 Uiso 1 1 calc R U . . . H25B H 1.0131 0.2591 0.2737 0.059 Uiso 1 1 calc R U . . . H25C H 0.9953 0.3364 0.2932 0.059 Uiso 1 1 calc R U . . . C12 C -0.3242(7) 0.4318(3) 0.2104(2) 0.0374(17) Uani 1 1 d . . . . . H12A H -0.3244 0.4162 0.2370 0.056 Uiso 1 1 calc R U . . . H12B H -0.4274 0.4309 0.2006 0.056 Uiso 1 1 calc R U . . . H12C H -0.2843 0.4809 0.2087 0.056 Uiso 1 1 calc R U . . . C42 C 1.1920(7) 0.3727(4) 0.6608(2) 0.049(2) Uani 1 1 d . . . . . H42A H 1.1771 0.3386 0.6818 0.073 Uiso 1 1 calc R U . . . H42B H 1.2920 0.3946 0.6629 0.073 Uiso 1 1 calc R U . . . H42C H 1.1841 0.3472 0.6366 0.073 Uiso 1 1 calc R U . . . C20 C 0.4237(8) 0.4736(4) 0.2996(2) 0.0472(19) Uani 1 1 d . . . . . H20A H 0.5122 0.5050 0.2977 0.071 Uiso 1 1 calc R U . . . H20B H 0.3319 0.5029 0.2987 0.071 Uiso 1 1 calc R U . . . H20C H 0.4238 0.4396 0.2784 0.071 Uiso 1 1 calc R U . . . C39 C 1.0847(8) 0.4846(4) 0.6292(2) 0.0472(19) Uani 1 1 d . . . . . H39A H 1.0738 0.4581 0.6053 0.071 Uiso 1 1 calc R U . . . H39B H 1.1840 0.5076 0.6299 0.071 Uiso 1 1 calc R U . . . H39C H 1.0061 0.5214 0.6309 0.071 Uiso 1 1 calc R U . . . C56 C 0.7406(8) -0.1820(3) 0.5627(2) 0.0416(18) Uani 1 1 d . . . . . H56A H 0.8028 -0.2007 0.5835 0.062 Uiso 1 1 calc R U . . . H56B H 0.7850 -0.1962 0.5383 0.062 Uiso 1 1 calc R U . . . H56C H 0.6386 -0.2018 0.5647 0.062 Uiso 1 1 calc R U . . . C59 C 0.5763(8) 0.0266(4) 0.7996(2) 0.048(2) Uani 1 1 d . . . . . H59A H 0.4853 -0.0029 0.7974 0.073 Uiso 1 1 calc R U . . . H59B H 0.6654 -0.0046 0.7990 0.073 Uiso 1 1 calc R U . . . H59C H 0.5808 0.0607 0.7784 0.073 Uiso 1 1 calc R U . . . C76 C 0.2420(9) 0.6823(3) 0.9375(2) 0.0464(19) Uani 1 1 d . . . . . H76A H 0.3064 0.7010 0.9172 0.070 Uiso 1 1 calc R U . . . H76B H 0.2843 0.6959 0.9622 0.070 Uiso 1 1 calc R U . . . H76C H 0.1405 0.7026 0.9350 0.070 Uiso 1 1 calc R U . . . C61 C 0.5871(8) 0.0162(4) 0.8717(2) 0.0475(19) Uani 1 1 d . . . . . H61A H 0.5889 0.0439 0.8953 0.071 Uiso 1 1 calc R U . . . H61B H 0.6806 -0.0114 0.8693 0.071 Uiso 1 1 calc R U . . . H61C H 0.5009 -0.0167 0.8720 0.071 Uiso 1 1 calc R U . . . C3 C -0.0865(7) 0.0156(4) 0.1288(2) 0.0452(19) Uani 1 1 d . . . . . H3A H -0.0823 0.0426 0.1049 0.068 Uiso 1 1 calc R U . . . H3B H -0.1831 -0.0097 0.1306 0.068 Uiso 1 1 calc R U . . . H3C H -0.0040 -0.0195 0.1295 0.068 Uiso 1 1 calc R U . . . C40 C 1.0760(8) 0.4739(4) 0.7005(2) 0.049(2) Uani 1 1 d . . . . . H40A H 0.9872 0.5049 0.7027 0.074 Uiso 1 1 calc R U . . . H40B H 1.1674 0.5034 0.7012 0.074 Uiso 1 1 calc R U . . . H40C H 1.0774 0.4398 0.7218 0.074 Uiso 1 1 calc R U . . . C21 C 0.3084(7) 0.3720(4) 0.3396(2) 0.050(2) Uani 1 1 d . . . . . H21A H 0.3090 0.3441 0.3160 0.075 Uiso 1 1 calc R U . . . H21B H 0.2088 0.3937 0.3432 0.075 Uiso 1 1 calc R U . . . H21C H 0.3312 0.3402 0.3611 0.075 Uiso 1 1 calc R U . . . C23 C 0.4144(8) 0.4848(4) 0.3712(2) 0.0472(19) Uani 1 1 d . . . . . H23A H 0.4177 0.4578 0.3950 0.071 Uiso 1 1 calc R U . . . H23B H 0.3185 0.5107 0.3694 0.071 Uiso 1 1 calc R U . . . H23C H 0.4978 0.5193 0.3705 0.071 Uiso 1 1 calc R U . . . C19 C 0.2609(8) 0.6825(3) 0.0624(2) 0.0446(19) Uani 1 1 d . . . . . H19A H 0.2101 0.6965 0.0389 0.067 Uiso 1 1 calc R U . . . H19B H 0.3636 0.7018 0.0625 0.067 Uiso 1 1 calc R U . . . H19C H 0.2051 0.7016 0.0842 0.067 Uiso 1 1 calc R U . . . C4 C -0.1926(7) 0.1275(4) 0.1599(3) 0.050(2) Uani 1 1 d . . . . . H4C H -0.1847 0.1590 0.1821 0.075 Uiso 1 1 calc R U . . . H4D H -0.2928 0.1054 0.1593 0.075 Uiso 1 1 calc R U . . . H4E H -0.1772 0.1558 0.1367 0.075 Uiso 1 1 calc R U . . . C60 C 0.6917(7) 0.1274(4) 0.8398(3) 0.052(2) Uani 1 1 d . . . . . H60A H 0.6867 0.1572 0.8169 0.078 Uiso 1 1 calc R U . . . H60B H 0.7919 0.1055 0.8417 0.078 Uiso 1 1 calc R U . . . H60C H 0.6730 0.1573 0.8622 0.078 Uiso 1 1 calc R U . . . C37 C 0.7596(9) -0.1822(3) 0.4373(2) 0.049(2) Uani 1 1 d . . . . . H37A H 0.7103 -0.1962 0.4611 0.074 Uiso 1 1 calc R U . . . H37B H 0.8615 -0.2024 0.4365 0.074 Uiso 1 1 calc R U . . . H37C H 0.7013 -0.2005 0.4157 0.074 Uiso 1 1 calc R U . . . C1 C -0.0771(8) 0.0261(4) 0.2008(2) 0.050(2) Uani 1 1 d . . . . . H1A H 0.0132 -0.0038 0.2034 0.076 Uiso 1 1 calc R U . . . H1B H -0.1669 -0.0045 0.2013 0.076 Uiso 1 1 calc R U . . . H1C H -0.0817 0.0605 0.2218 0.076 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O28 0.020(2) 0.021(2) 0.038(3) 0.0033(19) -0.0004(18) -0.0024(17) O5 0.019(2) 0.025(2) 0.041(3) 0.000(2) 0.0021(19) 0.0004(18) O10 0.020(2) 0.029(2) 0.036(3) -0.0024(19) 0.0016(18) -0.0027(18) O20 0.019(2) 0.026(2) 0.039(3) 0.003(2) -0.0006(18) 0.0005(18) O15 0.018(2) 0.028(2) 0.047(3) -0.003(2) 0.0019(19) -0.0019(17) O49 0.023(2) 0.025(2) 0.045(3) 0.008(2) -0.0016(19) 0.0047(18) O18 0.023(2) 0.024(2) 0.043(3) -0.002(2) -0.0027(19) 0.0035(18) O4 0.019(2) 0.029(2) 0.044(3) 0.008(2) -0.0024(19) 0.0008(18) O8 0.019(2) 0.028(2) 0.042(3) 0.005(2) -0.0002(19) 0.0022(18) O2 0.036(2) 0.026(2) 0.038(3) 0.005(2) 0.006(2) 0.0054(19) O24 0.033(2) 0.025(2) 0.038(3) -0.003(2) 0.009(2) -0.0071(19) O14 0.020(2) 0.030(2) 0.044(3) 0.007(2) -0.0036(19) -0.0035(18) O17 0.033(2) 0.027(2) 0.040(3) -0.003(2) -0.003(2) 0.0041(19) O16 0.023(2) 0.030(2) 0.046(3) -0.008(2) -0.001(2) 0.0065(19) O13 0.034(2) 0.027(2) 0.037(3) -0.001(2) -0.007(2) -0.0061(19) O25 0.024(2) 0.026(2) 0.047(3) -0.005(2) 0.004(2) -0.0058(18) O3 0.022(2) 0.032(2) 0.043(3) 0.006(2) 0.003(2) 0.0046(19) O22 0.020(2) 0.031(2) 0.043(3) -0.002(2) -0.0042(19) 0.0018(18) O23 0.024(2) 0.031(2) 0.043(3) -0.002(2) 0.002(2) -0.0040(19) O11 0.049(3) 0.028(3) 0.038(3) 0.002(2) 0.000(2) 0.001(2) O27 0.046(3) 0.025(3) 0.038(3) 0.000(2) 0.001(2) 0.004(2) O9 0.026(2) 0.028(2) 0.044(3) 0.006(2) 0.001(2) -0.0027(19) O6 0.044(3) 0.027(3) 0.042(3) 0.003(2) -0.001(2) -0.003(2) O12 0.044(3) 0.034(3) 0.036(3) -0.001(2) -0.006(2) 0.003(2) O7 0.041(3) 0.033(2) 0.039(3) -0.006(2) 0.012(2) -0.002(2) O19 0.043(3) 0.030(3) 0.045(3) 0.002(2) -0.001(2) -0.006(2) O21 0.037(3) 0.039(3) 0.040(3) 0.002(2) -0.009(2) -0.001(2) O26 0.045(3) 0.035(3) 0.036(3) 0.002(2) 0.010(2) 0.001(2) N12 0.032(3) 0.021(3) 0.027(3) 0.007(2) -0.001(2) 0.004(2) N10 0.016(2) 0.021(3) 0.034(3) -0.004(2) -0.001(2) -0.001(2) N15 0.020(3) 0.017(2) 0.033(3) 0.000(2) -0.002(2) -0.001(2) N7 0.019(2) 0.018(2) 0.033(3) 0.008(2) 0.001(2) 0.001(2) N106 0.026(3) 0.026(3) 0.028(3) -0.004(2) 0.000(2) 0.001(2) O44 0.054(3) 0.052(3) 0.041(3) 0.002(2) 0.003(2) -0.002(2) N3 0.023(3) 0.017(2) 0.030(3) 0.003(2) 0.003(2) 0.002(2) N1 0.031(3) 0.020(3) 0.030(3) 0.001(2) 0.006(2) 0.008(2) N13 0.032(3) 0.026(3) 0.026(3) 0.003(2) 0.006(2) -0.005(2) N105 0.028(3) 0.018(2) 0.028(3) -0.001(2) -0.001(2) 0.004(2) N108 0.023(3) 0.023(3) 0.035(3) 0.002(2) 0.003(2) 0.000(2) N2 0.023(3) 0.023(3) 0.030(3) 0.002(2) 0.004(2) 0.002(2) N107 0.028(3) 0.021(3) 0.029(3) 0.000(2) 0.000(2) -0.003(2) O37 0.058(3) 0.044(3) 0.049(3) 0.002(2) -0.004(2) 0.005(2) N14 0.026(3) 0.021(3) 0.027(3) 0.002(2) 0.002(2) -0.004(2) N11 0.023(3) 0.029(3) 0.026(3) 0.002(2) 0.000(2) 0.006(2) O48 0.063(3) 0.045(3) 0.055(4) 0.004(3) -0.002(3) 0.001(3) N5 0.031(3) 0.027(3) 0.025(3) 0.001(2) -0.003(2) -0.007(2) O34 0.062(3) 0.045(3) 0.041(3) -0.002(2) -0.001(2) -0.002(2) O31 0.055(3) 0.046(3) 0.049(3) 0.002(2) 0.000(2) 0.003(2) O39 0.056(3) 0.049(3) 0.053(4) 0.001(3) 0.001(3) 0.004(2) O41 0.048(3) 0.055(3) 0.067(4) 0.001(3) 0.000(3) -0.001(2) N6 0.032(3) 0.024(3) 0.024(3) 0.006(2) 0.003(2) -0.005(2) O30 0.057(3) 0.051(3) 0.071(4) -0.003(3) -0.001(3) -0.001(3) O33 0.058(3) 0.048(3) 0.060(4) 0.006(3) -0.004(3) -0.001(2) O40 0.058(3) 0.058(3) 0.075(4) 0.001(3) 0.007(3) -0.009(3) O38 0.056(3) 0.048(3) 0.063(4) 0.001(3) 0.001(3) -0.003(2) O47 0.050(3) 0.058(3) 0.071(4) 0.001(3) 0.001(3) -0.005(3) O29 0.053(3) 0.054(3) 0.083(4) -0.006(3) -0.004(3) 0.000(3) O43 0.057(3) 0.058(3) 0.072(4) -0.003(3) 0.000(3) -0.003(3) O46 0.054(3) 0.056(3) 0.081(4) 0.006(3) -0.004(3) -0.006(3) C67 0.019(3) 0.019(3) 0.028(4) -0.001(3) 0.002(3) 0.004(2) C49 0.012(3) 0.020(3) 0.036(4) -0.014(3) 0.006(3) -0.009(2) O42 0.058(3) 0.059(3) 0.072(4) 0.005(3) 0.006(3) 0.006(3) C30 0.015(3) 0.026(3) 0.033(4) 0.011(3) -0.003(3) -0.002(3) C24 0.025(3) 0.013(3) 0.041(4) 0.002(3) 0.004(3) -0.002(3) C62 0.026(3) 0.014(3) 0.044(5) -0.001(3) 0.000(3) -0.005(3) C11 0.020(3) 0.020(3) 0.034(4) 0.007(3) -0.002(3) -0.003(3) C51 0.023(3) 0.021(3) 0.031(4) 0.003(3) 0.002(3) 0.002(3) C32 0.023(3) 0.020(3) 0.031(4) 0.000(3) 0.001(3) -0.003(3) C9 0.027(3) 0.020(3) 0.030(4) 0.003(3) 0.002(3) -0.002(3) C28 0.027(3) 0.021(3) 0.026(4) 0.005(3) 0.003(3) 0.003(3) C43 0.025(3) 0.015(3) 0.040(4) -0.002(3) 0.006(3) 0.001(3) C53 0.032(3) 0.025(3) 0.025(4) -0.004(3) 0.004(3) -0.004(3) C70 0.026(3) 0.016(3) 0.034(4) 0.004(3) -0.005(3) -0.002(3) C29 0.021(3) 0.028(3) 0.036(4) 0.003(3) -0.003(3) 0.003(3) C41 0.019(3) 0.021(3) 0.049(5) 0.003(3) -0.002(3) -0.004(3) C48 0.024(3) 0.024(3) 0.032(4) -0.005(3) -0.001(3) -0.004(3) C13 0.023(3) 0.016(3) 0.030(4) -0.001(3) 0.003(3) 0.003(2) C44 0.019(3) 0.022(3) 0.038(4) -0.001(3) 0.007(3) -0.005(2) C10 0.021(3) 0.026(3) 0.036(4) 0.002(3) 0.003(3) -0.002(3) C74 0.031(3) 0.029(3) 0.025(4) 0.002(3) -0.001(3) -0.010(3) C5 0.023(3) 0.020(3) 0.047(5) 0.001(3) 0.001(3) 0.000(3) C66 0.017(3) 0.021(3) 0.041(4) -0.002(3) -0.005(3) 0.002(2) C38 0.029(3) 0.025(3) 0.029(4) -0.004(3) 0.008(3) -0.005(3) C16 0.030(3) 0.032(4) 0.025(4) 0.005(3) -0.001(3) 0.001(3) C47 0.026(3) 0.020(3) 0.034(4) -0.004(3) -0.001(3) -0.002(3) C6 0.024(3) 0.021(3) 0.033(4) 0.008(3) -0.002(3) -0.004(3) C36 0.029(3) 0.023(3) 0.029(4) 0.004(3) -0.002(3) -0.001(3) C34 0.032(4) 0.029(4) 0.029(4) 0.000(3) 0.001(3) -0.002(3) C54 0.026(3) 0.041(4) 0.025(4) -0.003(3) 0.001(3) -0.003(3) C45 0.022(3) 0.030(3) 0.043(4) -0.005(3) -0.005(3) -0.008(3) C68 0.017(3) 0.018(3) 0.040(4) 0.001(3) 0.003(3) 0.002(2) C2 0.020(3) 0.022(3) 0.049(5) 0.004(3) -0.005(3) -0.005(3) C73 0.028(3) 0.030(3) 0.025(4) 0.003(3) -0.004(3) -0.006(3) C18 0.025(3) 0.025(3) 0.036(4) -0.005(3) -0.001(3) 0.007(3) C15 0.026(3) 0.032(4) 0.031(4) -0.002(3) -0.004(3) -0.004(3) C7 0.023(3) 0.028(3) 0.040(4) -0.004(3) 0.006(3) -0.002(3) C26 0.020(3) 0.023(3) 0.036(4) -0.005(3) 0.005(3) 0.000(2) O45 0.102(5) 0.044(3) 0.128(6) 0.004(4) -0.047(4) 0.001(3) C65 0.027(3) 0.020(3) 0.034(4) 0.003(3) 0.004(3) 0.008(3) C57 0.027(3) 0.028(3) 0.029(4) -0.003(3) 0.006(3) 0.009(3) C14 0.022(3) 0.023(3) 0.038(4) 0.007(3) 0.000(3) 0.004(3) C55 0.033(4) 0.030(4) 0.026(4) -0.003(3) 0.000(3) 0.004(3) C72 0.037(4) 0.025(4) 0.030(4) -0.004(3) -0.002(3) -0.005(3) C71 0.026(3) 0.026(3) 0.035(4) -0.001(3) 0.002(3) 0.002(3) C75 0.038(4) 0.031(4) 0.031(4) -0.001(3) -0.004(3) -0.002(3) C69 0.025(3) 0.029(3) 0.045(4) -0.001(3) 0.008(3) -0.008(3) C64 0.025(3) 0.032(4) 0.044(4) -0.002(3) 0.007(3) 0.000(3) C27 0.019(3) 0.026(3) 0.045(4) 0.000(3) -0.002(3) -0.004(3) C35 0.025(3) 0.029(3) 0.033(4) -0.005(3) 0.003(3) -0.005(3) O32 0.098(5) 0.044(3) 0.127(6) -0.005(4) -0.051(4) 0.002(3) C58 0.021(3) 0.025(3) 0.053(5) 0.008(3) 0.002(3) 0.004(3) C63 0.040(4) 0.025(3) 0.051(5) -0.004(3) -0.016(3) -0.001(3) O36 0.101(5) 0.039(3) 0.126(6) 0.008(3) 0.050(4) -0.003(3) C22 0.025(3) 0.032(4) 0.043(5) 0.001(3) -0.002(3) 0.008(3) C17 0.035(4) 0.024(3) 0.032(4) 0.000(3) 0.003(3) 0.003(3) C31 0.028(3) 0.032(4) 0.048(5) -0.006(3) -0.008(3) -0.013(3) C52 0.027(3) 0.028(3) 0.033(4) -0.004(3) 0.002(3) 0.001(3) C8 0.031(4) 0.037(4) 0.049(5) 0.008(3) -0.011(3) -0.005(3) C46 0.035(4) 0.030(4) 0.049(5) -0.008(3) 0.016(3) 0.003(3) C50 0.021(3) 0.035(4) 0.050(5) 0.007(3) 0.000(3) 0.010(3) C33 0.018(3) 0.030(3) 0.039(4) 0.003(3) -0.002(3) -0.001(3) O35 0.105(5) 0.048(4) 0.123(6) -0.003(4) 0.041(4) 0.000(3) C25 0.040(4) 0.032(4) 0.047(5) 0.013(3) 0.013(3) -0.002(3) C12 0.029(4) 0.032(4) 0.051(5) -0.002(3) 0.013(3) 0.010(3) C42 0.030(4) 0.034(4) 0.082(6) -0.001(4) 0.005(4) 0.003(3) C20 0.043(4) 0.040(4) 0.059(6) 0.010(4) 0.000(4) 0.014(3) C39 0.037(4) 0.041(4) 0.063(6) 0.011(4) -0.002(4) -0.014(3) C56 0.060(5) 0.022(3) 0.042(5) -0.001(3) -0.015(4) 0.006(3) C59 0.044(4) 0.035(4) 0.066(6) -0.008(4) 0.000(4) 0.021(3) C76 0.068(5) 0.029(4) 0.042(5) -0.001(3) 0.016(4) -0.010(3) C61 0.037(4) 0.047(4) 0.058(5) 0.007(4) -0.004(4) 0.008(3) C3 0.032(4) 0.042(4) 0.062(5) -0.008(4) 0.003(3) -0.008(3) C40 0.049(5) 0.038(4) 0.061(6) -0.008(4) 0.002(4) -0.018(3) C21 0.024(4) 0.036(4) 0.090(7) -0.001(4) 0.002(4) -0.005(3) C23 0.038(4) 0.046(4) 0.058(5) -0.011(4) 0.000(4) 0.008(3) C19 0.057(5) 0.029(4) 0.048(5) 0.002(3) 0.015(4) 0.001(3) C4 0.027(4) 0.030(4) 0.094(7) 0.001(4) -0.001(4) -0.002(3) C60 0.028(4) 0.036(4) 0.093(7) 0.005(4) -0.006(4) -0.003(3) C37 0.065(5) 0.028(4) 0.054(5) 0.003(3) -0.012(4) 0.003(3) C1 0.047(4) 0.036(4) 0.069(6) 0.002(4) 0.004(4) -0.013(3) 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' 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 C30 O15 C31 115.1(5) . . ? C62 O49 C58 120.1(5) . . ? C24 O18 C22 120.2(5) . . ? C67 O4 C69 115.8(5) . . ? C49 O8 C50 115.0(4) . . ? C43 O14 C41 120.3(5) . . ? C5 O25 C2 120.9(5) . . ? C11 O22 C12 116.6(5) . . ? C53 N12 C54 126.8(5) . . ? C53 N12 H12 116.6 . . ? C54 N12 H12 116.6 . . ? C51 N10 C48 122.0(5) . . ? C51 N10 C47 120.1(4) . . ? C48 N10 C47 115.3(4) . . ? C70 N15 C68 120.7(5) . . ? C70 N15 C65 120.1(5) . . ? C68 N15 C65 116.3(4) . . ? C32 N7 C29 121.5(5) . . ? C32 N7 C28 119.4(4) . . ? C29 N7 C28 116.8(5) . . ? C24 N106 C26 123.8(5) . . ? C24 N106 H106 118.1 . . ? C26 N106 H106 118.1 . . ? C13 N3 C10 121.6(5) . . ? C13 N3 C9 119.1(5) . . ? C10 N3 C9 117.2(4) . . ? C15 N1 C16 126.7(5) . . ? C15 N1 H1 116.7 . . ? C16 N1 H1 116.7 . . ? C72 N13 C75 127.1(5) . . ? C72 N13 H13 116.5 . . ? C75 N13 H13 116.5 . . ? C5 N105 C6 125.7(5) . . ? C5 N105 H105 117.1 . . ? C6 N105 H105 117.1 . . ? C62 N108 C66 125.7(5) . . ? C62 N108 H108 117.2 . . ? C66 N108 H108 117.2 . . ? C18 N2 C15 121.9(5) . . ? C18 N2 C14 123.1(5) . . ? C15 N2 C14 114.9(5) . . ? C43 N107 C44 125.7(5) . . ? C43 N107 H107 117.2 . . ? C44 N107 H107 117.2 . . ? C73 N14 C72 121.7(5) . . ? C73 N14 C71 123.4(5) . . ? C72 N14 C71 114.7(5) . . ? C53 N11 C57 120.9(5) . . ? C53 N11 C52 115.9(5) . . ? C57 N11 C52 123.1(5) . . ? C34 N5 C38 126.5(5) . . ? C34 N5 H5 116.7 . . ? C38 N5 H5 116.7 . . ? C34 N6 C35 120.6(5) . . ? C34 N6 C33 116.4(5) . . ? C35 N6 C33 122.8(5) . . ? O3 C67 O4 124.5(5) . . ? O3 C67 C68 124.6(5) . . ? O4 C67 C68 110.8(5) . . ? O9 C49 O8 125.6(6) . . ? O9 C49 C48 124.1(5) . . ? O8 C49 C48 110.3(5) . . ? O16 C30 O15 124.4(5) . . ? O16 C30 C29 126.0(5) . . ? O15 C30 C29 109.5(5) . . ? O17 C24 O18 125.8(6) . . ? O17 C24 N106 126.3(6) . . ? O18 C24 N106 107.9(6) . . ? O2 C62 O49 127.1(6) . . ? O2 C62 N108 123.6(6) . . ? O49 C62 N108 109.3(6) . . ? O23 C11 O22 124.2(5) . . ? O23 C11 C10 124.3(5) . . ? O22 C11 C10 111.6(5) . . ? O10 C51 N10 124.2(5) . . ? O10 C51 C52 119.5(5) . . ? N10 C51 C52 116.4(5) . . ? O20 C32 N7 124.2(5) . . ? O20 C32 C33 119.6(5) . . ? N7 C32 C33 116.2(5) . . ? N3 C9 C6 113.9(5) . . ? N3 C9 H9A 108.8 . . ? C6 C9 H9A 108.8 . . ? N3 C9 H9B 108.8 . . ? C6 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N7 C28 C26 115.2(5) . . ? N7 C28 H28A 108.5 . . ? C26 C28 H28A 108.5 . . ? N7 C28 H28B 108.5 . . ? C26 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? O13 C43 N107 125.4(6) . . ? O13 C43 O14 125.7(6) . . ? N107 C43 O14 108.9(6) . . ? O11 C53 N12 123.3(6) . . ? O11 C53 N11 121.5(6) . . ? N12 C53 N11 115.1(5) . . ? O5 C70 N15 123.4(5) . . ? O5 C70 C71 120.5(5) . . ? N15 C70 C71 116.0(5) . . ? N7 C29 C30 110.9(5) . . ? N7 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? N7 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? O14 C41 C39 102.5(5) . . ? O14 C41 C40 111.9(5) . . ? C39 C41 C40 109.9(5) . . ? O14 C41 C42 109.3(5) . . ? C39 C41 C42 111.0(5) . . ? C40 C41 C42 111.8(6) . . ? N10 C48 C49 112.1(4) . . ? N10 C48 H48A 109.2 . . ? C49 C48 H48A 109.2 . . ? N10 C48 H48B 109.2 . . ? C49 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? O28 C13 N3 124.4(5) . . ? O28 C13 C14 119.6(5) . . ? N3 C13 C14 116.0(5) . . ? N107 C44 C45 105.6(5) . . ? N107 C44 C46 109.6(5) . . ? C45 C44 C46 110.8(5) . . ? N107 C44 C47 112.1(4) . . ? C45 C44 C47 111.9(5) . . ? C46 C44 C47 106.9(5) . . ? N3 C10 C11 111.3(5) . . ? N3 C10 H10C 109.4 . . ? C11 C10 H10C 109.4 . . ? N3 C10 H10D 109.4 . . ? C11 C10 H10D 109.4 . . ? H10C C10 H10D 108.0 . . ? C73 C74 C75 117.9(6) . . ? C73 C74 C76 124.2(6) . . ? C75 C74 C76 117.9(6) . . ? O24 C5 O25 125.6(5) . . ? O24 C5 N105 125.3(6) . . ? O25 C5 N105 109.1(6) . . ? N108 C66 C63 110.6(5) . . ? N108 C66 C64 104.8(5) . . ? C63 C66 C64 111.7(5) . . ? N108 C66 C65 111.3(4) . . ? C63 C66 C65 107.8(5) . . ? C64 C66 C65 110.7(5) . . ? O21 C38 N5 118.6(6) . . ? O21 C38 C36 125.7(6) . . ? N5 C38 C36 115.7(6) . . ? O26 C16 N1 119.5(5) . . ? O26 C16 C17 124.8(6) . . ? N1 C16 C17 115.7(5) . . ? N10 C47 C44 114.3(5) . . ? N10 C47 H47A 108.7 . . ? C44 C47 H47A 108.7 . . ? N10 C47 H47B 108.7 . . ? C44 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? N105 C6 C7 105.9(5) . . ? N105 C6 C8 110.0(5) . . ? C7 C6 C8 110.8(5) . . ? N105 C6 C9 112.1(4) . . ? C7 C6 C9 111.4(5) . . ? C8 C6 C9 106.7(5) . . ? C35 C36 C38 118.6(6) . . ? C35 C36 C37 122.7(6) . . ? C38 C36 C37 118.7(6) . . ? O19 C34 N5 123.2(6) . . ? O19 C34 N6 121.4(6) . . ? N5 C34 N6 115.3(5) . . ? O12 C54 N12 120.1(6) . . ? O12 C54 C55 124.0(6) . . ? N12 C54 C55 115.8(6) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N15 C68 C67 112.4(5) . . ? N15 C68 H68A 109.1 . . ? C67 C68 H68A 109.1 . . ? N15 C68 H68B 109.1 . . ? C67 C68 H68B 109.1 . . ? H68A C68 H68B 107.8 . . ? O25 C2 C3 103.4(5) . . ? O25 C2 C4 109.4(5) . . ? C3 C2 C4 110.3(6) . . ? O25 C2 C1 110.7(5) . . ? C3 C2 C1 110.5(5) . . ? C4 C2 C1 112.3(6) . . ? C74 C73 N14 123.8(6) . . ? C74 C73 H73 118.1 . . ? N14 C73 H73 118.1 . . ? C17 C18 N2 123.3(6) . . ? C17 C18 H18 118.3 . . ? N2 C18 H18 118.3 . . ? O27 C15 N1 123.9(6) . . ? O27 C15 N2 121.6(6) . . ? N1 C15 N2 114.4(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N106 C26 C25 111.3(5) . . ? N106 C26 C27 104.9(5) . . ? C25 C26 C27 110.2(5) . . ? N106 C26 C28 111.6(4) . . ? C25 C26 C28 107.9(5) . . ? C27 C26 C28 110.9(5) . . ? N15 C65 C66 114.6(5) . . ? N15 C65 H65A 108.6 . . ? C66 C65 H65A 108.6 . . ? N15 C65 H65B 108.6 . . ? C66 C65 H65B 108.6 . . ? H65A C65 H65B 107.6 . . ? C55 C57 N11 123.3(6) . . ? C55 C57 H57 118.4 . . ? N11 C57 H57 118.4 . . ? N2 C14 C13 110.9(5) . . ? N2 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C57 C55 C54 118.1(6) . . ? C57 C55 C56 123.3(6) . . ? C54 C55 C56 118.7(6) . . ? O6 C72 N13 122.8(6) . . ? O6 C72 N14 122.7(6) . . ? N13 C72 N14 114.5(5) . . ? N14 C71 C70 110.3(5) . . ? N14 C71 H71A 109.6 . . ? C70 C71 H71A 109.6 . . ? N14 C71 H71B 109.6 . . ? C70 C71 H71B 109.6 . . ? H71A C71 H71B 108.1 . . ? O7 C75 N13 120.3(6) . . ? O7 C75 C74 124.7(6) . . ? N13 C75 C74 115.0(6) . . ? O4 C69 H69A 109.5 . . ? O4 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? O4 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C66 C64 H64A 109.5 . . ? C66 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C66 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C36 C35 N6 123.3(6) . . ? C36 C35 H35 118.4 . . ? N6 C35 H35 118.4 . . ? O49 C58 C60 109.6(5) . . ? O49 C58 C59 110.2(5) . . ? C60 C58 C59 113.0(6) . . ? O49 C58 C61 102.2(5) . . ? C60 C58 C61 110.6(6) . . ? C59 C58 C61 110.8(6) . . ? C66 C63 H63A 109.5 . . ? C66 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C66 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O18 C22 C20 111.3(5) . . ? O18 C22 C21 108.7(5) . . ? C20 C22 C21 112.9(6) . . ? O18 C22 C23 102.3(5) . . ? C20 C22 C23 110.1(6) . . ? C21 C22 C23 111.0(6) . . ? C18 C17 C16 118.0(6) . . ? C18 C17 C19 124.2(6) . . ? C16 C17 C19 117.8(5) . . ? O15 C31 H31A 109.5 . . ? O15 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O15 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N11 C52 C51 110.4(5) . . ? N11 C52 H52A 109.6 . . ? C51 C52 H52A 109.6 . . ? N11 C52 H52B 109.6 . . ? C51 C52 H52B 109.6 . . ? H52A C52 H52B 108.1 . . ? C6 C8 H8C 109.5 . . ? C6 C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? C6 C8 H8E 109.5 . . ? H8C C8 H8E 109.5 . . ? H8D C8 H8E 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O8 C50 H50A 109.5 . . ? O8 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O8 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N6 C33 C32 110.4(5) . . ? N6 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? N6 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O22 C12 H12A 109.5 . . ? O22 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O22 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C22 C20 H20A 109.5 . . ? C22 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C22 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C41 C39 H39A 109.5 . . ? C41 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C41 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C58 C61 H61A 109.5 . . ? C58 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C58 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C2 C4 H4C 109.5 . . ? C2 C4 H4D 109.5 . . ? H4C C4 H4D 109.5 . . ? C2 C4 H4E 109.5 . . ? H4C C4 H4E 109.5 . . ? H4D C4 H4E 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 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 O28 C13 1.215(6) . ? O5 C70 1.226(6) . ? O10 C51 1.233(6) . ? O20 C32 1.228(6) . ? O15 C30 1.353(6) . ? O15 C31 1.463(7) . ? O49 C62 1.334(7) . ? O49 C58 1.487(7) . ? O18 C24 1.357(7) . ? O18 C22 1.483(7) . ? O4 C67 1.342(7) . ? O4 C69 1.457(7) . ? O8 C49 1.335(6) . ? O8 C50 1.463(7) . ? O2 C62 1.224(7) . ? O24 C5 1.218(7) . ? O14 C43 1.356(7) . ? O14 C41 1.472(7) . ? O17 C24 1.208(7) . ? O16 C30 1.195(7) . ? O13 C43 1.206(7) . ? O25 C5 1.346(7) . ? O25 C2 1.483(6) . ? O3 C67 1.199(7) . ? O22 C11 1.330(6) . ? O22 C12 1.466(7) . ? O23 C11 1.213(7) . ? O11 C53 1.218(7) . ? O27 C15 1.218(7) . ? O9 C49 1.194(7) . ? O6 C72 1.220(7) . ? O12 C54 1.248(7) . ? O7 C75 1.242(7) . ? O19 C34 1.228(7) . ? O21 C38 1.251(7) . ? O26 C16 1.243(7) . ? N12 C53 1.363(7) . ? N12 C54 1.366(8) . ? N12 H12 0.8600 . ? N10 C51 1.332(7) . ? N10 C48 1.465(7) . ? N10 C47 1.479(7) . ? N15 C70 1.361(7) . ? N15 C68 1.453(7) . ? N15 C65 1.461(7) . ? N7 C32 1.355(7) . ? N7 C29 1.460(7) . ? N7 C28 1.465(7) . ? N106 C24 1.359(8) . ? N106 C26 1.490(7) . ? N106 H106 0.8600 . ? N3 C13 1.355(7) . ? N3 C10 1.455(7) . ? N3 C9 1.472(7) . ? N1 C15 1.357(7) . ? N1 C16 1.387(7) . ? N1 H1 0.8600 . ? N13 C72 1.367(7) . ? N13 C75 1.382(8) . ? N13 H13 0.8600 . ? N105 C5 1.355(7) . ? N105 C6 1.483(7) . ? N105 H105 0.8600 . ? N108 C62 1.363(7) . ? N108 C66 1.485(7) . ? N108 H108 0.8600 . ? N2 C18 1.365(7) . ? N2 C15 1.392(8) . ? N2 C14 1.445(7) . ? N107 C43 1.347(8) . ? N107 C44 1.480(7) . ? N107 H107 0.8600 . ? N14 C73 1.373(7) . ? N14 C72 1.374(8) . ? N14 C71 1.452(7) . ? N11 C53 1.386(8) . ? N11 C57 1.389(7) . ? N11 C52 1.452(7) . ? N5 C34 1.355(8) . ? N5 C38 1.387(7) . ? N5 H5 0.8600 . ? N6 C34 1.379(8) . ? N6 C35 1.387(7) . ? N6 C33 1.444(8) . ? C67 C68 1.516(8) . ? C49 C48 1.512(8) . ? C30 C29 1.519(8) . ? C11 C10 1.520(8) . ? C51 C52 1.536(8) . ? C32 C33 1.534(8) . ? C9 C6 1.547(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C28 C26 1.538(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C70 C71 1.530(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C41 C39 1.505(9) . ? C41 C40 1.511(9) . ? C41 C42 1.519(8) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C13 C14 1.539(8) . ? C44 C45 1.522(8) . ? C44 C46 1.526(8) . ? C44 C47 1.530(8) . ? C10 H10C 0.9700 . ? C10 H10D 0.9700 . ? C74 C73 1.322(8) . ? C74 C75 1.460(9) . ? C74 C76 1.507(8) . ? C66 C63 1.510(8) . ? C66 C64 1.537(8) . ? C66 C65 1.547(8) . ? C38 C36 1.429(8) . ? C16 C17 1.448(8) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C6 C7 1.514(8) . ? C6 C8 1.523(9) . ? C36 C35 1.328(8) . ? C36 C37 1.503(8) . ? C54 C55 1.460(9) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C2 C3 1.507(9) . ? C2 C4 1.520(8) . ? C2 C1 1.527(9) . ? C73 H73 0.9300 . ? C18 C17 1.333(8) . ? C18 H18 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C26 C25 1.515(8) . ? C26 C27 1.527(8) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C57 C55 1.323(8) . ? C57 H57 0.9300 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C55 C56 1.499(8) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C35 H35 0.9300 . ? C58 C60 1.497(8) . ? C58 C59 1.515(9) . ? C58 C61 1.515(9) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C22 C20 1.501(9) . ? C22 C21 1.517(8) . ? C22 C23 1.521(9) . ? C17 C19 1.505(8) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C8 H8E 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C4 H4C 0.9600 . ? C4 H4D 0.9600 . ? C4 H4E 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ?