#------------------------------------------------------------------------------ #$Date: 2024-08-05 20:53:04 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293730 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572002.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_1572002 loop_ _publ_author_name 'Wang, Patrick' 'Fares, Mohamed' 'Eladwy, Radwa A.' 'Bhuyan, Deep J.' 'Wu, Xin' 'Lewis, William' 'Loeb, Stephen J.' 'Macreadie, Lauren K.' 'Gale, Philip A.' _publ_section_title ; Platinum-based metal complexes as chloride transporters that trigger apoptosis. ; _journal_issue 29 _journal_name_full 'Chemical science' _journal_page_first 11584 _journal_page_last 11593 _journal_paper_doi 10.1039/d4sc02115k _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C60 H76 N12 O4 Pt, 2(B F4)' _chemical_formula_sum 'C60 H76 B2 F8 N12 O4 Pt' _chemical_formula_weight 1398.03 _chemical_name_systematic 'Pentyl complex' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2024-02-07 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-02-16 deposited with the CCDC. 2024-06-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.604(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.3731(8) _cell_length_b 14.0167(7) _cell_length_c 17.0490(7) _cell_measurement_reflns_used 10114 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.3270 _cell_measurement_theta_min 2.2670 _cell_volume 3106.1(3) _computing_cell_refinement 'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 5.2930 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 39.00 106.00 1.00 60.00 -- 14.75 178.00-180.00 67 2 \w -26.00 98.00 1.00 60.00 -- 14.75 19.00 -30.00 124 3 \w -61.00 46.00 1.00 60.00 -- 14.75 -57.00-180.00 107 4 \w -42.00 23.00 1.00 60.00 -- -11.78 -77.00 30.00 65 5 \w -47.00 21.00 1.00 60.00 -- -11.78 77.00 -60.00 68 6 \w -15.00 10.00 1.00 60.00 -- -11.78 -99.00 -60.00 25 7 \w -68.00 -7.00 1.00 60.00 -- 14.75 -19.00 -60.00 61 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_unetI/netI 0.0591 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 36390 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.370 _diffrn_reflns_theta_min 1.903 _exptl_absorpt_coefficient_mu 2.339 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'metallic yellowish yellow' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.495 _exptl_crystal_description block _exptl_crystal_F_000 1424 _exptl_crystal_preparation 'Heating platinum complex with isoquinoline urea derivative in acetonitrile' _exptl_crystal_recrystallization_method 'From DMF/ether' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.762 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 396 _refine_ls_number_reflns 6356 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0292 _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^)+(0.0166P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0567 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4534 _reflns_number_total 6356 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02115k2.cif _cod_data_source_block pag22_s2620_sn1001 _cod_depositor_comments 'Adding full bibliography for 1572002--1572006.cif.' _cod_database_code 1572002 _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. ; _shelx_estimated_absorpt_t_max 0.892 _shelx_estimated_absorpt_t_min 0.706 _olex2_refinement_description ; 1.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C45(H45A, H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B) 1.b Aromatic/amide H refined with riding coordinates: C2(H2), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), N11(H11), N14(H14), C32(H32), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), N41(H41), N44(H44) 1.c Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C49(H49A,H49B,H49C) ; _shelx_res_file ; TITL pag22_s2620_sn1001_a.res in P2(1)/c pag22_s2620_sn1001.res created by SHELXL-2018/3 at 14:48:43 on 04-Jul-2023 REM Old TITL pag22_s2620_sn1001 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.082, Rweak 0.003, Alpha 0.033 REM 0.538 for 278 systematic absences, Orientation as input REM Formula found by SHELXT: C66 B2 N2 O8 F8 Pt CELL 0.71073 13.3731 14.0167 17.049 90 103.604 90 ZERR 2 0.0008 0.0007 0.0007 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B F N O Pt UNIT 120 152 4 16 24 8 2 L.S. 12 0 0 PLAN 12 SIZE 0.05 0.07 0.16 TEMP -173 CONF HTAB N11 F62 HTAB N14 F63 HTAB N41 F65 HTAB N44 F65 BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.016600 FVAR 0.26574 PT1 7 0.500000 0.500000 0.500000 10.50000 0.01206 0.01780 = 0.01326 -0.00003 0.00373 0.00007 N1 5 0.439829 0.535278 0.593465 11.00000 0.01156 0.01754 = 0.01661 -0.00332 0.00195 -0.00334 C2 1 0.487139 0.508231 0.667726 11.00000 0.01320 0.01998 = 0.01733 -0.00202 0.00431 -0.00232 AFIX 43 H2 2 0.548090 0.471206 0.674609 11.00000 -1.20000 AFIX 0 C3 1 0.451601 0.531594 0.736081 11.00000 0.02035 0.01801 = 0.01816 -0.00355 0.00519 -0.00539 C4 1 0.505607 0.505880 0.816350 11.00000 0.02238 0.02317 = 0.01718 -0.00441 0.00577 -0.00842 C5 1 0.462830 0.530576 0.878983 11.00000 0.03151 0.03006 = 0.02028 -0.00398 0.00868 -0.00516 AFIX 43 H5 2 0.496313 0.512445 0.932395 11.00000 -1.20000 AFIX 0 C6 1 0.370269 0.582271 0.865712 11.00000 0.03799 0.02944 = 0.02433 -0.00795 0.01947 -0.00569 AFIX 43 H6 2 0.343510 0.599386 0.910682 11.00000 -1.20000 AFIX 0 C7 1 0.317956 0.608479 0.790572 11.00000 0.02190 0.02430 = 0.03146 -0.00700 0.01430 -0.00422 AFIX 43 H7 2 0.255188 0.642861 0.782983 11.00000 -1.20000 AFIX 0 C8 1 0.358153 0.583934 0.724338 11.00000 0.01633 0.01474 = 0.02472 -0.00576 0.00786 -0.00401 C9 1 0.308807 0.610163 0.644830 11.00000 0.01947 0.01616 = 0.02797 -0.00043 0.00712 0.00129 AFIX 43 H9 2 0.245961 0.644691 0.635108 11.00000 -1.20000 AFIX 0 C10 1 0.350430 0.586443 0.581801 11.00000 0.01502 0.01775 = 0.02054 0.00234 0.00178 0.00032 AFIX 43 H10 2 0.316739 0.605797 0.528766 11.00000 -1.20000 AFIX 0 N11 5 0.600660 0.459183 0.826046 11.00000 0.02177 0.04026 = 0.01150 0.00153 0.00389 0.00166 AFIX 43 H11 2 0.631285 0.462862 0.785762 11.00000 -1.20000 AFIX 0 C12 1 0.650683 0.407676 0.893584 11.00000 0.02402 0.03178 = 0.02026 -0.00471 0.00253 -0.00419 O13 6 0.612770 0.393345 0.951080 11.00000 0.02854 0.05202 = 0.02012 0.00690 0.00900 0.00381 N14 5 0.743652 0.374263 0.889365 11.00000 0.02528 0.04010 = 0.01868 0.00280 0.00554 0.00335 AFIX 43 H14 2 0.767318 0.386351 0.846403 11.00000 -1.20000 AFIX 0 C15 1 0.805236 0.318513 0.954946 11.00000 0.02495 0.02908 = 0.02461 -0.00102 0.00572 0.00541 AFIX 23 H15A 2 0.850314 0.275468 0.932630 11.00000 -1.20000 H15B 2 0.758640 0.278106 0.978072 11.00000 -1.20000 AFIX 0 C16 1 0.871767 0.376932 1.022402 11.00000 0.02582 0.02389 = 0.02748 0.00024 0.00238 0.00079 AFIX 23 H16A 2 0.923843 0.412287 1.001176 11.00000 -1.20000 H16B 2 0.828271 0.424178 1.042009 11.00000 -1.20000 AFIX 0 C17 1 0.925490 0.314625 1.091922 11.00000 0.04762 0.02813 = 0.03323 0.00250 -0.00427 0.00480 AFIX 23 H17A 2 0.970520 0.269262 1.071904 11.00000 -1.20000 H17B 2 0.872846 0.276739 1.110332 11.00000 -1.20000 AFIX 0 C18 1 0.989971 0.367425 1.163942 11.00000 0.05898 0.04130 = 0.03332 0.00659 -0.01033 -0.00376 AFIX 23 H18A 2 0.947368 0.417670 1.180792 11.00000 -1.20000 H18B 2 1.011122 0.322239 1.209459 11.00000 -1.20000 AFIX 0 C19 1 1.083946 0.412327 1.146614 11.00000 0.05897 0.06836 = 0.05790 0.00591 -0.01215 -0.00985 AFIX 137 H19A 2 1.125610 0.440587 1.196197 11.00000 -1.50000 H19B 2 1.063445 0.462165 1.105670 11.00000 -1.50000 H19C 2 1.124351 0.363646 1.126621 11.00000 -1.50000 AFIX 0 N31 5 0.586581 0.619309 0.520269 11.00000 0.01687 0.01686 = 0.01396 0.00064 0.00639 0.00120 C32 1 0.687683 0.613116 0.548290 11.00000 0.01601 0.01894 = 0.02003 0.00102 0.00596 0.00383 AFIX 43 H32 2 0.717773 0.551422 0.556291 11.00000 -1.20000 AFIX 0 C33 1 0.752730 0.692858 0.566794 11.00000 0.01430 0.01830 = 0.02199 -0.00062 0.00618 0.00007 C34 1 0.861372 0.684465 0.598906 11.00000 0.02028 0.01978 = 0.03094 -0.00356 0.00651 -0.00087 C35 1 0.919572 0.765735 0.614206 11.00000 0.01607 0.02889 = 0.04611 -0.00450 0.00499 -0.00354 AFIX 43 H35 2 0.991643 0.761365 0.636044 11.00000 -1.20000 AFIX 0 C36 1 0.872890 0.855293 0.597672 11.00000 0.02690 0.02224 = 0.05981 -0.00579 0.01329 -0.00926 AFIX 43 H36 2 0.914713 0.910801 0.607768 11.00000 -1.20000 AFIX 0 C37 1 0.770309 0.865604 0.567819 11.00000 0.02803 0.01623 = 0.05684 -0.00226 0.01273 -0.00172 AFIX 43 H37 2 0.741255 0.927483 0.557342 11.00000 -1.20000 AFIX 0 C38 1 0.706942 0.784480 0.552381 11.00000 0.01821 0.01936 = 0.02991 -0.00076 0.00980 -0.00174 C39 1 0.600393 0.788747 0.523547 11.00000 0.02619 0.01819 = 0.03661 0.00226 0.00688 0.00540 AFIX 43 H39 2 0.567680 0.849229 0.514293 11.00000 -1.20000 AFIX 0 C40 1 0.542407 0.708324 0.508416 11.00000 0.01476 0.02331 = 0.02833 -0.00158 0.00316 0.00469 AFIX 43 H40 2 0.469940 0.713675 0.489276 11.00000 -1.20000 AFIX 0 N41 5 0.902711 0.592850 0.614126 11.00000 0.01590 0.02090 = 0.04414 0.00445 0.00933 -0.00230 AFIX 43 H41 2 0.865129 0.549642 0.631304 11.00000 -1.20000 AFIX 0 C42 1 0.998638 0.564843 0.604187 11.00000 0.02232 0.02920 = 0.03740 -0.00035 0.00278 -0.00099 O43 6 1.063831 0.620743 0.593475 11.00000 0.01771 0.02594 = 0.06279 0.00377 0.01157 -0.00499 N44 5 1.011289 0.468332 0.606716 11.00000 0.01337 0.02286 = 0.06024 0.00303 0.00888 0.00105 AFIX 43 H44 2 0.960398 0.432179 0.613923 11.00000 -1.20000 AFIX 0 C45 1 1.105381 0.423107 0.597981 11.00000 0.01716 0.02837 = 0.04145 0.00211 0.00684 -0.00004 AFIX 23 H45A 2 1.147225 0.470240 0.576500 11.00000 -1.20000 H45B 2 1.088036 0.370543 0.558318 11.00000 -1.20000 AFIX 0 C46 1 1.168306 0.383771 0.676518 11.00000 0.02271 0.03012 = 0.03110 -0.00187 0.00746 -0.00293 AFIX 23 H46A 2 1.126079 0.337524 0.698558 11.00000 -1.20000 H46B 2 1.186894 0.436518 0.715872 11.00000 -1.20000 AFIX 0 C47 1 1.266227 0.334586 0.666657 11.00000 0.02625 0.02210 = 0.03005 -0.00008 0.00690 0.00191 AFIX 23 H47A 2 1.247298 0.280452 0.628772 11.00000 -1.20000 H47B 2 1.306902 0.380210 0.642486 11.00000 -1.20000 AFIX 0 C48 1 1.332457 0.297880 0.745328 11.00000 0.03535 0.03204 = 0.03216 0.00591 0.00310 0.00110 AFIX 23 H48A 2 1.292803 0.249996 0.768148 11.00000 -1.20000 H48B 2 1.348453 0.351484 0.784070 11.00000 -1.20000 AFIX 0 C49 1 1.432239 0.253059 0.736693 11.00000 0.04616 0.04191 = 0.05331 -0.00079 -0.00196 0.01983 AFIX 137 H49A 2 1.417174 0.198361 0.700002 11.00000 -1.50000 H49B 2 1.471658 0.231586 0.789674 11.00000 -1.50000 H49C 2 1.472514 0.300198 0.714809 11.00000 -1.50000 AFIX 0 B61 3 0.751926 0.382418 0.673615 11.00000 0.02206 0.02664 = 0.02168 0.00602 0.00628 0.00079 F62 4 0.730815 0.468152 0.707405 11.00000 0.02963 0.03473 = 0.03189 -0.00455 0.00946 0.00149 F63 4 0.815333 0.327131 0.732080 11.00000 0.03790 0.04146 = 0.03061 0.01025 0.00537 0.01013 F64 4 0.661467 0.335997 0.640037 11.00000 0.02857 0.03468 = 0.04886 0.00124 0.00446 -0.00955 F65 4 0.801943 0.403944 0.611781 11.00000 0.02590 0.02890 = 0.03172 0.00328 0.01275 0.00221 HKLF 4 REM pag22_s2620_sn1001_a.res in P2(1)/c REM wR2 = 0.0567, GooF = S = 1.004, Restrained GooF = 1.004 for all data REM R1 = 0.0292 for 4534 Fo > 4sig(Fo) and 0.0558 for all 6356 data REM 396 parameters refined using 0 restraints END WGHT 0.0164 0.0000 REM Highest difference peak 0.762, deepest hole -0.605, 1-sigma level 0.093 Q1 1 0.5285 0.4999 0.5577 11.00000 0.05 0.76 Q2 1 0.4302 0.5014 0.5090 11.00000 0.05 0.52 Q3 1 0.4596 0.4887 0.5593 11.00000 0.05 0.49 Q4 1 0.4379 0.5524 0.4617 11.00000 0.05 0.46 Q5 1 0.6994 0.4978 0.4984 11.00000 0.05 0.42 Q6 1 0.4568 0.5201 0.6337 11.00000 0.05 0.41 Q7 1 0.5082 0.4360 0.5288 11.00000 0.05 0.40 Q8 1 0.5130 0.4335 0.4599 11.00000 0.05 0.39 Q9 1 0.8571 0.5392 0.6005 11.00000 0.05 0.38 Q10 1 0.6585 0.4618 0.5445 11.00000 0.05 0.37 Q11 1 0.5986 0.6613 0.4209 11.00000 0.05 0.37 Q12 1 0.4731 0.5007 0.7813 11.00000 0.05 0.36 ; _shelx_res_checksum 49547 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Pt1 Pt 0.500000 0.500000 0.500000 0.01425(5) Uani 1 2 d S . P . . N1 N 0.4398(2) 0.53528(17) 0.59346(13) 0.0155(6) Uani 1 1 d . . . . . C2 C 0.4871(2) 0.5082(2) 0.66773(15) 0.0167(6) Uani 1 1 d . . . . . H2 H 0.548090 0.471206 0.674609 0.020 Uiso 1 1 calc R U . . . C3 C 0.4516(3) 0.5316(2) 0.73608(17) 0.0187(7) Uani 1 1 d . . . . . C4 C 0.5056(2) 0.5059(2) 0.81635(16) 0.0207(7) Uani 1 1 d . . . . . C5 C 0.4628(3) 0.5306(2) 0.87898(18) 0.0269(9) Uani 1 1 d . . . . . H5 H 0.496313 0.512445 0.932395 0.032 Uiso 1 1 calc R U . . . C6 C 0.3703(3) 0.5823(2) 0.86571(19) 0.0286(9) Uani 1 1 d . . . . . H6 H 0.343510 0.599386 0.910682 0.034 Uiso 1 1 calc R U . . . C7 C 0.3180(3) 0.6085(2) 0.79057(18) 0.0246(8) Uani 1 1 d . . . . . H7 H 0.255188 0.642861 0.782983 0.029 Uiso 1 1 calc R U . . . C8 C 0.3582(3) 0.5839(2) 0.72434(18) 0.0181(7) Uani 1 1 d . . . . . C9 C 0.3088(3) 0.6102(2) 0.64483(18) 0.0209(8) Uani 1 1 d . . . . . H9 H 0.245961 0.644691 0.635108 0.025 Uiso 1 1 calc R U . . . C10 C 0.3504(2) 0.5864(2) 0.58180(18) 0.0182(7) Uani 1 1 d . . . . . H10 H 0.316739 0.605797 0.528766 0.022 Uiso 1 1 calc R U . . . N11 N 0.6007(2) 0.45918(19) 0.82605(14) 0.0245(7) Uani 1 1 d . . . . . H11 H 0.631285 0.462862 0.785762 0.029 Uiso 1 1 calc R U . . . C12 C 0.6507(3) 0.4077(2) 0.89358(18) 0.0258(8) Uani 1 1 d . . . . . O13 O 0.61277(19) 0.39334(17) 0.95108(12) 0.0330(6) Uani 1 1 d . . . . . N14 N 0.7437(2) 0.37426(19) 0.88936(15) 0.0280(7) Uani 1 1 d . . . . . H14 H 0.767318 0.386351 0.846403 0.034 Uiso 1 1 calc R U . . . C15 C 0.8052(3) 0.3185(2) 0.95495(18) 0.0262(8) Uani 1 1 d . . . . . H15A H 0.850314 0.275468 0.932630 0.031 Uiso 1 1 calc R U . . . H15B H 0.758640 0.278106 0.978072 0.031 Uiso 1 1 calc R U . . . C16 C 0.8718(3) 0.3769(2) 1.02240(18) 0.0264(8) Uani 1 1 d . . . . . H16A H 0.923843 0.412287 1.001176 0.032 Uiso 1 1 calc R U . . . H16B H 0.828271 0.424178 1.042009 0.032 Uiso 1 1 calc R U . . . C17 C 0.9255(3) 0.3146(2) 1.0919(2) 0.0386(10) Uani 1 1 d . . . . . H17A H 0.970520 0.269262 1.071904 0.046 Uiso 1 1 calc R U . . . H17B H 0.872846 0.276739 1.110332 0.046 Uiso 1 1 calc R U . . . C18 C 0.9900(3) 0.3674(3) 1.1639(2) 0.0481(12) Uani 1 1 d . . . . . H18A H 0.947368 0.417670 1.180792 0.058 Uiso 1 1 calc R U . . . H18B H 1.011122 0.322239 1.209459 0.058 Uiso 1 1 calc R U . . . C19 C 1.0839(4) 0.4123(3) 1.1466(3) 0.0660(15) Uani 1 1 d . . . . . H19A H 1.125610 0.440587 1.196197 0.099 Uiso 1 1 calc R U . . . H19B H 1.063445 0.462165 1.105670 0.099 Uiso 1 1 calc R U . . . H19C H 1.124351 0.363646 1.126621 0.099 Uiso 1 1 calc R U . . . N31 N 0.5866(2) 0.61931(17) 0.52027(13) 0.0154(6) Uani 1 1 d . . . . . C32 C 0.6877(3) 0.6131(2) 0.54829(17) 0.0180(7) Uani 1 1 d . . . . . H32 H 0.717773 0.551422 0.556291 0.022 Uiso 1 1 calc R U . . . C33 C 0.7527(2) 0.6929(2) 0.56679(17) 0.0179(7) Uani 1 1 d . . . . . C34 C 0.8614(3) 0.6845(2) 0.59891(19) 0.0236(8) Uani 1 1 d . . . . . C35 C 0.9196(3) 0.7657(2) 0.6142(2) 0.0307(9) Uani 1 1 d . . . . . H35 H 0.991643 0.761365 0.636044 0.037 Uiso 1 1 calc R U . . . C36 C 0.8729(3) 0.8553(2) 0.5977(2) 0.0358(10) Uani 1 1 d . . . . . H36 H 0.914713 0.910801 0.607768 0.043 Uiso 1 1 calc R U . . . C37 C 0.7703(3) 0.8656(2) 0.5678(2) 0.0332(9) Uani 1 1 d . . . . . H37 H 0.741255 0.927483 0.557342 0.040 Uiso 1 1 calc R U . . . C38 C 0.7069(3) 0.7845(2) 0.55238(18) 0.0218(8) Uani 1 1 d . . . . . C39 C 0.6004(3) 0.7887(2) 0.52355(19) 0.0271(8) Uani 1 1 d . . . . . H39 H 0.567680 0.849229 0.514293 0.032 Uiso 1 1 calc R U . . . C40 C 0.5424(3) 0.7083(2) 0.50842(18) 0.0224(8) Uani 1 1 d . . . . . H40 H 0.469940 0.713675 0.489276 0.027 Uiso 1 1 calc R U . . . N41 N 0.9027(2) 0.59285(18) 0.61413(16) 0.0266(7) Uani 1 1 d . . . . . H41 H 0.865129 0.549642 0.631304 0.032 Uiso 1 1 calc R U . . . C42 C 0.9986(3) 0.5648(2) 0.6042(2) 0.0303(9) Uani 1 1 d . . . . . O43 O 1.06383(19) 0.62074(16) 0.59348(15) 0.0351(6) Uani 1 1 d . . . . . N44 N 1.0113(2) 0.46833(19) 0.60672(18) 0.0321(8) Uani 1 1 d . . . . . H44 H 0.960398 0.432179 0.613923 0.039 Uiso 1 1 calc R U . . . C45 C 1.1054(3) 0.4231(2) 0.5980(2) 0.0290(9) Uani 1 1 d . . . . . H45A H 1.147225 0.470240 0.576500 0.035 Uiso 1 1 calc R U . . . H45B H 1.088036 0.370543 0.558318 0.035 Uiso 1 1 calc R U . . . C46 C 1.1683(3) 0.3838(2) 0.67652(19) 0.0278(8) Uani 1 1 d . . . . . H46A H 1.126079 0.337524 0.698558 0.033 Uiso 1 1 calc R U . . . H46B H 1.186894 0.436518 0.715872 0.033 Uiso 1 1 calc R U . . . C47 C 1.2662(3) 0.3346(2) 0.66666(18) 0.0261(8) Uani 1 1 d . . . . . H47A H 1.247298 0.280452 0.628772 0.031 Uiso 1 1 calc R U . . . H47B H 1.306902 0.380210 0.642486 0.031 Uiso 1 1 calc R U . . . C48 C 1.3325(3) 0.2979(2) 0.74533(19) 0.0340(9) Uani 1 1 d . . . . . H48A H 1.292803 0.249996 0.768148 0.041 Uiso 1 1 calc R U . . . H48B H 1.348453 0.351484 0.784070 0.041 Uiso 1 1 calc R U . . . C49 C 1.4322(3) 0.2531(3) 0.7367(2) 0.0494(12) Uani 1 1 d . . . . . H49A H 1.417174 0.198361 0.700002 0.074 Uiso 1 1 calc R U . . . H49B H 1.471658 0.231586 0.789674 0.074 Uiso 1 1 calc R U . . . H49C H 1.472514 0.300198 0.714809 0.074 Uiso 1 1 calc R U . . . B61 B 0.7519(3) 0.3824(3) 0.6736(2) 0.0233(9) Uani 1 1 d . . . . . F62 F 0.73082(15) 0.46815(13) 0.70741(10) 0.0317(5) Uani 1 1 d . . . . . F63 F 0.81533(16) 0.32713(13) 0.73208(11) 0.0371(5) Uani 1 1 d . . . . . F64 F 0.66147(16) 0.33600(13) 0.64004(12) 0.0381(5) Uani 1 1 d . . . . . F65 F 0.80194(15) 0.40394(12) 0.61178(10) 0.0278(5) Uani 1 1 d . . . . . 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 Pt1 0.01206(10) 0.01780(9) 0.01326(8) -0.00003(9) 0.00373(6) 0.00007(10) N1 0.0116(16) 0.0175(13) 0.0166(12) -0.0033(10) 0.0019(11) -0.0033(11) C2 0.0132(17) 0.0200(16) 0.0173(13) -0.0020(15) 0.0043(12) -0.0023(16) C3 0.020(2) 0.0180(16) 0.0182(15) -0.0036(12) 0.0052(14) -0.0054(14) C4 0.0224(19) 0.0232(17) 0.0172(13) -0.0044(16) 0.0058(12) -0.0084(18) C5 0.032(2) 0.030(2) 0.0203(16) -0.0040(14) 0.0087(15) -0.0052(16) C6 0.038(3) 0.029(2) 0.0243(18) -0.0079(15) 0.0195(17) -0.0057(18) C7 0.022(2) 0.0243(18) 0.0315(18) -0.0070(15) 0.0143(16) -0.0042(16) C8 0.016(2) 0.0147(17) 0.0247(16) -0.0058(13) 0.0079(14) -0.0040(14) C9 0.019(2) 0.0162(17) 0.0280(17) -0.0004(14) 0.0071(15) 0.0013(15) C10 0.015(2) 0.0177(17) 0.0205(16) 0.0023(13) 0.0018(14) 0.0003(14) N11 0.0218(18) 0.0403(16) 0.0115(12) 0.0015(12) 0.0039(12) 0.0017(14) C12 0.024(2) 0.032(2) 0.0203(17) -0.0047(15) 0.0025(16) -0.0042(17) O13 0.0285(16) 0.0520(16) 0.0201(12) 0.0069(11) 0.0090(11) 0.0038(13) N14 0.0253(19) 0.0401(18) 0.0187(14) 0.0028(13) 0.0055(13) 0.0034(15) C15 0.025(2) 0.029(2) 0.0246(17) -0.0010(15) 0.0057(15) 0.0054(17) C16 0.026(2) 0.0239(19) 0.0275(18) 0.0002(15) 0.0024(16) 0.0008(16) C17 0.048(3) 0.028(2) 0.033(2) 0.0025(17) -0.0043(19) 0.0048(19) C18 0.059(3) 0.041(2) 0.033(2) 0.0066(18) -0.010(2) -0.004(2) C19 0.059(4) 0.068(3) 0.058(3) 0.006(2) -0.012(3) -0.010(3) N31 0.0169(17) 0.0169(14) 0.0140(12) 0.0006(10) 0.0064(11) 0.0012(12) C32 0.016(2) 0.0189(17) 0.0200(15) 0.0010(13) 0.0060(14) 0.0038(15) C33 0.014(2) 0.0183(17) 0.0220(16) -0.0006(13) 0.0062(14) 0.0001(14) C34 0.020(2) 0.0198(18) 0.0309(18) -0.0036(15) 0.0065(15) -0.0009(16) C35 0.016(2) 0.029(2) 0.046(2) -0.0045(17) 0.0050(17) -0.0035(17) C36 0.027(3) 0.022(2) 0.060(3) -0.0058(18) 0.013(2) -0.0093(18) C37 0.028(3) 0.0162(19) 0.057(2) -0.0023(17) 0.0127(19) -0.0017(17) C38 0.018(2) 0.0194(18) 0.0299(18) -0.0008(14) 0.0098(15) -0.0017(15) C39 0.026(2) 0.0182(18) 0.0366(19) 0.0023(15) 0.0069(17) 0.0054(16) C40 0.0148(19) 0.0233(19) 0.0283(18) -0.0016(14) 0.0032(15) 0.0047(15) N41 0.0159(18) 0.0209(16) 0.0441(17) 0.0045(13) 0.0093(14) -0.0023(13) C42 0.022(2) 0.029(2) 0.037(2) -0.0004(17) 0.0028(17) -0.0010(18) O43 0.0177(16) 0.0259(14) 0.0628(17) 0.0038(12) 0.0116(13) -0.0050(12) N44 0.0134(18) 0.0229(16) 0.060(2) 0.0030(14) 0.0089(15) 0.0010(13) C45 0.017(2) 0.028(2) 0.041(2) 0.0021(16) 0.0068(17) 0.0000(16) C46 0.023(2) 0.030(2) 0.0311(18) -0.0019(16) 0.0075(16) -0.0029(17) C47 0.026(2) 0.0221(18) 0.0301(18) -0.0001(15) 0.0069(16) 0.0019(16) C48 0.035(3) 0.032(2) 0.0322(19) 0.0059(16) 0.0031(18) 0.0011(18) C49 0.046(3) 0.042(3) 0.053(3) -0.001(2) -0.002(2) 0.020(2) B61 0.022(3) 0.027(2) 0.0217(19) 0.0060(17) 0.0063(17) 0.0008(19) F62 0.0296(13) 0.0347(12) 0.0319(10) -0.0046(8) 0.0095(9) 0.0015(9) F63 0.0379(14) 0.0415(12) 0.0306(11) 0.0103(9) 0.0054(10) 0.0101(11) F64 0.0286(14) 0.0347(12) 0.0489(13) 0.0012(10) 0.0045(10) -0.0095(10) F65 0.0259(13) 0.0289(11) 0.0317(10) 0.0033(8) 0.0127(9) 0.0022(9) 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 2 5 0.0660 0 -2 -5 0.0770 1 5 -3 0.0474 -1 -5 3 0.0274 1 0 0 0.0248 -1 0 0 0.0248 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 N1 Pt1 N1 180.0 . 3_666 ? N1 Pt1 N31 88.91(10) 3_666 3_666 ? N1 Pt1 N31 88.91(10) . . ? N1 Pt1 N31 91.09(10) . 3_666 ? N1 Pt1 N31 91.09(10) 3_666 . ? N31 Pt1 N31 180.0 3_666 . ? C2 N1 Pt1 119.7(2) . . ? C2 N1 C10 119.4(3) . . ? C10 N1 Pt1 120.88(19) . . ? N1 C2 H2 118.4 . . ? N1 C2 C3 123.2(3) . . ? C3 C2 H2 118.4 . . ? C2 C3 C4 122.9(3) . . ? C2 C3 C8 117.6(3) . . ? C8 C3 C4 119.5(3) . . ? C5 C4 C3 118.1(3) . . ? C5 C4 N11 124.0(3) . . ? N11 C4 C3 117.9(3) . . ? C4 C5 H5 119.4 . . ? C4 C5 C6 121.2(3) . . ? C6 C5 H5 119.4 . . ? C5 C6 H6 119.0 . . ? C7 C6 C5 122.0(3) . . ? C7 C6 H6 119.0 . . ? C6 C7 H7 120.6 . . ? C6 C7 C8 118.9(3) . . ? C8 C7 H7 120.6 . . ? C7 C8 C3 120.2(3) . . ? C7 C8 C9 121.9(3) . . ? C9 C8 C3 117.8(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 119.7 . . ? N1 C10 H10 119.4 . . ? C9 C10 N1 121.2(3) . . ? C9 C10 H10 119.4 . . ? C4 N11 H11 117.1 . . ? C12 N11 C4 125.8(3) . . ? C12 N11 H11 117.1 . . ? O13 C12 N11 122.7(3) . . ? O13 C12 N14 123.3(3) . . ? N14 C12 N11 114.0(3) . . ? C12 N14 H14 119.7 . . ? C12 N14 C15 120.7(3) . . ? C15 N14 H14 119.7 . . ? N14 C15 H15A 108.6 . . ? N14 C15 H15B 108.6 . . ? N14 C15 C16 114.7(3) . . ? H15A C15 H15B 107.6 . . ? C16 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? C15 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C17 C16 C15 111.6(3) . . ? C17 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? C16 C17 H17A 108.4 . . ? C16 C17 H17B 108.4 . . ? C16 C17 C18 115.3(3) . . ? H17A C17 H17B 107.5 . . ? C18 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? C17 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C19 C18 C17 112.9(4) . . ? C19 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C32 N31 Pt1 120.2(2) . . ? C32 N31 C40 118.6(3) . . ? C40 N31 Pt1 121.2(2) . . ? N31 C32 H32 118.2 . . ? N31 C32 C33 123.6(3) . . ? C33 C32 H32 118.2 . . ? C32 C33 C34 122.6(3) . . ? C32 C33 C38 117.5(3) . . ? C38 C33 C34 119.9(3) . . ? C35 C34 C33 119.0(3) . . ? C35 C34 N41 123.1(3) . . ? N41 C34 C33 117.9(3) . . ? C34 C35 H35 120.0 . . ? C34 C35 C36 120.0(3) . . ? C36 C35 H35 120.0 . . ? C35 C36 H36 118.8 . . ? C37 C36 C35 122.4(3) . . ? C37 C36 H36 118.8 . . ? C36 C37 H37 120.1 . . ? C36 C37 C38 119.8(3) . . ? C38 C37 H37 120.1 . . ? C37 C38 C33 118.9(3) . . ? C39 C38 C33 117.6(3) . . ? C39 C38 C37 123.5(3) . . ? C38 C39 H39 119.3 . . ? C40 C39 C38 121.4(3) . . ? C40 C39 H39 119.3 . . ? N31 C40 H40 119.4 . . ? C39 C40 N31 121.3(3) . . ? C39 C40 H40 119.4 . . ? C34 N41 H41 117.5 . . ? C42 N41 C34 125.0(3) . . ? C42 N41 H41 117.5 . . ? O43 C42 N41 123.4(3) . . ? O43 C42 N44 123.8(4) . . ? N44 C42 N41 112.8(3) . . ? C42 N44 H44 118.8 . . ? C42 N44 C45 122.4(3) . . ? C45 N44 H44 118.8 . . ? N44 C45 H45A 109.1 . . ? N44 C45 H45B 109.1 . . ? N44 C45 C46 112.7(3) . . ? H45A C45 H45B 107.8 . . ? C46 C45 H45A 109.1 . . ? C46 C45 H45B 109.1 . . ? C45 C46 H46A 109.1 . . ? C45 C46 H46B 109.1 . . ? C45 C46 C47 112.5(3) . . ? H46A C46 H46B 107.8 . . ? C47 C46 H46A 109.1 . . ? C47 C46 H46B 109.1 . . ? C46 C47 H47A 108.9 . . ? C46 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? C48 C47 C46 113.3(3) . . ? C48 C47 H47A 108.9 . . ? C48 C47 H47B 108.9 . . ? C47 C48 H48A 108.8 . . ? C47 C48 H48B 108.8 . . ? C47 C48 C49 113.6(3) . . ? H48A C48 H48B 107.7 . . ? C49 C48 H48A 108.8 . . ? C49 C48 H48B 108.8 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? F62 B61 F65 107.7(3) . . ? F63 B61 F62 109.6(3) . . ? F63 B61 F65 109.9(3) . . ? F64 B61 F62 109.7(3) . . ? F64 B61 F63 111.4(3) . . ? F64 B61 F65 108.4(3) . . ? 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 Pt1 N1 2.009(2) . ? Pt1 N1 2.009(2) 3_666 ? Pt1 N31 2.017(2) 3_666 ? Pt1 N31 2.017(2) . ? N1 C2 1.330(3) . ? N1 C10 1.368(4) . ? C2 H2 0.9500 . ? C2 C3 1.397(4) . ? C3 C4 1.435(4) . ? C3 C8 1.422(4) . ? C4 C5 1.369(4) . ? C4 N11 1.405(4) . ? C5 H5 0.9500 . ? C5 C6 1.406(5) . ? C6 H6 0.9500 . ? C6 C7 1.358(4) . ? C7 H7 0.9500 . ? C7 C8 1.403(4) . ? C8 C9 1.410(4) . ? C9 H9 0.9500 . ? C9 C10 1.363(4) . ? C10 H10 0.9500 . ? N11 H11 0.8800 . ? N11 C12 1.390(4) . ? C12 O13 1.222(4) . ? C12 N14 1.346(4) . ? N14 H14 0.8800 . ? N14 C15 1.451(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.518(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.511(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.517(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.496(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N31 C32 1.327(4) . ? N31 C40 1.375(4) . ? C32 H32 0.9500 . ? C32 C33 1.406(4) . ? C33 C34 1.432(4) . ? C33 C38 1.419(4) . ? C34 C35 1.370(4) . ? C34 N41 1.398(4) . ? C35 H35 0.9500 . ? C35 C36 1.401(5) . ? C36 H36 0.9500 . ? C36 C37 1.354(5) . ? C37 H37 0.9500 . ? C37 C38 1.406(4) . ? C38 C39 1.395(5) . ? C39 H39 0.9500 . ? C39 C40 1.358(4) . ? C40 H40 0.9500 . ? N41 H41 0.8800 . ? N41 C42 1.390(5) . ? C42 O43 1.217(4) . ? C42 N44 1.363(4) . ? N44 H44 0.8800 . ? N44 C45 1.448(4) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.508(4) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 C47 1.524(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C48 1.513(4) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C48 C49 1.513(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? B61 F62 1.390(4) . ? B61 F63 1.384(4) . ? B61 F64 1.374(4) . ? B61 F65 1.408(4) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N11 H11 F62 0.88 2.10 2.965(3) 168.8 . yes N14 H14 F63 0.88 2.34 3.123(3) 147.9 . yes N41 H41 F65 0.88 2.21 2.967(3) 144.7 . yes N44 H44 F65 0.88 2.15 2.962(4) 153.7 . yes 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 Pt1 N1 C2 C3 178.6(2) . . . . ? Pt1 N1 C10 C9 179.6(2) . . . . ? Pt1 N31 C32 C33 -177.5(2) . . . . ? Pt1 N31 C40 C39 178.7(2) . . . . ? N1 C2 C3 C4 -177.1(3) . . . . ? N1 C2 C3 C8 2.3(5) . . . . ? C2 N1 C10 C9 -0.1(4) . . . . ? C2 C3 C4 C5 -178.6(3) . . . . ? C2 C3 C4 N11 3.1(5) . . . . ? C2 C3 C8 C7 179.2(3) . . . . ? C2 C3 C8 C9 -1.1(4) . . . . ? C3 C4 C5 C6 -2.0(5) . . . . ? C3 C4 N11 C12 -162.3(3) . . . . ? C3 C8 C9 C10 -0.5(4) . . . . ? C4 C3 C8 C7 -1.3(5) . . . . ? C4 C3 C8 C9 178.3(3) . . . . ? C4 C5 C6 C7 1.3(5) . . . . ? C4 N11 C12 O13 4.2(5) . . . . ? C4 N11 C12 N14 -176.6(3) . . . . ? C5 C4 N11 C12 19.5(5) . . . . ? C5 C6 C7 C8 -0.6(5) . . . . ? C6 C7 C8 C3 0.7(5) . . . . ? C6 C7 C8 C9 -179.0(3) . . . . ? C7 C8 C9 C10 179.1(3) . . . . ? C8 C3 C4 C5 2.0(5) . . . . ? C8 C3 C4 N11 -176.3(3) . . . . ? C8 C9 C10 N1 1.2(5) . . . . ? C10 N1 C2 C3 -1.8(4) . . . . ? N11 C4 C5 C6 176.2(3) . . . . ? N11 C12 N14 C15 -179.6(3) . . . . ? C12 N14 C15 C16 -85.8(4) . . . . ? O13 C12 N14 C15 -0.4(5) . . . . ? N14 C15 C16 C17 174.5(3) . . . . ? C15 C16 C17 C18 -177.3(4) . . . . ? C16 C17 C18 C19 -69.0(5) . . . . ? N31 C32 C33 C34 178.4(3) . . . . ? N31 C32 C33 C38 -1.7(4) . . . . ? C32 N31 C40 C39 1.1(4) . . . . ? C32 C33 C34 C35 179.1(3) . . . . ? C32 C33 C34 N41 -1.8(5) . . . . ? C32 C33 C38 C37 -178.0(3) . . . . ? C32 C33 C38 C39 2.1(4) . . . . ? C33 C34 C35 C36 -0.7(5) . . . . ? C33 C34 N41 C42 144.7(3) . . . . ? C33 C38 C39 C40 -1.1(5) . . . . ? C34 C33 C38 C37 1.9(5) . . . . ? C34 C33 C38 C39 -178.0(3) . . . . ? C34 C35 C36 C37 1.1(6) . . . . ? C34 N41 C42 O43 12.2(5) . . . . ? C34 N41 C42 N44 -167.0(3) . . . . ? C35 C34 N41 C42 -36.1(5) . . . . ? C35 C36 C37 C38 0.0(6) . . . . ? C36 C37 C38 C33 -1.5(5) . . . . ? C36 C37 C38 C39 178.4(3) . . . . ? C37 C38 C39 C40 179.1(3) . . . . ? C38 C33 C34 C35 -0.8(5) . . . . ? C38 C33 C34 N41 178.3(3) . . . . ? C38 C39 C40 N31 -0.6(5) . . . . ? C40 N31 C32 C33 0.1(4) . . . . ? N41 C34 C35 C36 -179.8(3) . . . . ? N41 C42 N44 C45 -179.8(3) . . . . ? C42 N44 C45 C46 106.7(4) . . . . ? O43 C42 N44 C45 1.0(5) . . . . ? N44 C45 C46 C47 178.9(3) . . . . ? C45 C46 C47 C48 177.8(3) . . . . ? C46 C47 C48 C49 -177.3(3) . . . . ?