#------------------------------------------------------------------------------ #$Date: 2021-10-16 01:59:07 +0300 (Sat, 16 Oct 2021) $ #$Revision: 269973 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708572.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_7708572 loop_ _publ_author_name 'Swaminathan, Srividya' 'Haribabu, Jebiti' 'Mohamed Kasim, Mohamed Subarkhan' 'dasararaju, gayathri' 'Balakrishnan, Nithya' 'Bhuvanesh, Nattamai' 'Echeverria, Cesar' 'Karvembu, R.' _publ_section_title ; Impact of aliphatic acyl and aromatic thioamide substituents on the anticancer activity of Ru(II)-p-cymene complexes carrying acylthiourea ligands -- In vitro and in vivo studies ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02611A _journal_year 2021 _chemical_formula_moiety 'C14 H20 N2 O S' _chemical_formula_sum 'C14 H20 N2 O S' _chemical_formula_weight 264.38 _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 _atom_sites_solution_primary dual _audit_creation_date 2018-10-12 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-09-18 deposited with the CCDC. 2021-10-15 downloaded from the CCDC. ; _cell_angle_alpha 96.577(4) _cell_angle_beta 99.785(4) _cell_angle_gamma 96.172(4) _cell_formula_units_Z 4 _cell_length_a 9.5041(11) _cell_length_b 10.2883(11) _cell_length_c 15.1931(17) _cell_measurement_reflns_used 9926 _cell_measurement_temperature 110.0 _cell_measurement_theta_max 25.758 _cell_measurement_theta_min 2.275 _cell_volume 1442.1(3) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS, 2016)' _computing_data_collection 'APEX 3 (Bruker AXS)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 110.0 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_unetI/netI 0.0566 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9748 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 22.500 _diffrn_reflns_theta_max 22.500 _diffrn_reflns_theta_min 2.193 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.5685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1416 before and 0.0861 after correction. The Ratio of minimum to maximum transmission is 0.7628. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.218 _exptl_crystal_description block _exptl_crystal_F_000 568 _exptl_crystal_size_max 0.241 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.124 _refine_diff_density_max 1.172 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 393 _refine_ls_number_reflns 3710 _refine_ls_number_restraints 334 _refine_ls_restrained_S_all 1.161 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0770 _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^)+(0.0334P)^2^+6.0505P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1586 _refine_ls_wR_factor_ref 0.1719 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3017 _reflns_number_total 3710 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02611a2.cif _cod_data_source_block svshcan _cod_database_code 7708572 _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 0.974 _shelx_estimated_absorpt_t_min 0.950 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C13B-C14B = C13B-C12B = C11B-C12B = C11B-C10B = C10B-C9B 1.54 with sigma of 0.005 C9B-C11B = C10B-C12B = C11B-C13B = C12B-C14B 2.5 with sigma of 0.005 C10-C12 = C9-C11 = C11-C13 = C9-C11A = C10-C12A = C11A-C13 2.5 with sigma of 0.02 C11A-C10 \\sim C11-C10 \\sim C12A-C11A \\sim C12-C11 \\sim C13-C12 \\sim C13-C12A with sigma of 0.01 3. Uiso/Uaniso restraints and constraints C10 \\sim C13 \\sim C14 \\sim C11 \\sim C12 \\sim C11A \\sim C12A \\sim C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim C14B \\sim C10C \\sim C11C \\sim C12C \\sim C13C \\sim C14C: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Rigid body (RIGU) restrains C10, C13, C14, C11, C12, C11A, C12A, C9B, C10B, C11B, C12B, C13B, C14B, C10C, C11C, C12C, C13C, C14C with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Same fragment restrains {C10B, C11B, C12B, C13B, C14B} sigma for 1-2: 0.005, 1-3: 0.04 as {C10C, C11C, C12C, C13C, C14C} 6. Others Sof(H9BC)=Sof(H9BD)=Sof(C10C)=Sof(H10C)=Sof(H10D)=Sof(C11C)=Sof(H11C)= Sof(H11D)=Sof(C12C)=Sof(H12C)=Sof(H12D)=Sof(C13C)=Sof(H13C)=Sof(H13D)= Sof(C14C)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1) Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(C11B)=Sof(H11A)= Sof(H11B)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(C13B)=Sof(H13A)=Sof(H13B)= Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1) Sof(H10G)=Sof(H10H)=Sof(H13G)=Sof(H13H)=Sof(C11A)=Sof(H11G)=Sof(H11H)= Sof(C12A)=Sof(H12G)=Sof(H12H)=1-FVAR(2) Sof(H10E)=Sof(H10F)=Sof(H13E)=Sof(H13F)=Sof(C11)=Sof(H11E)=Sof(H11F)=Sof(C12)= Sof(H12E)=Sof(H12F)=FVAR(2) 7.a Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C10(H10E,H10F), C10(H10G,H10H), C13(H13E,H13F), C13(H13G,H13H), C11(H11E,H11F), C12(H12E,H12F), C11A(H11G,H11H), C12A(H12G,H12H), C9B(H9BA, H9BB), C9B(H9BC,H9BD), C10B(H10A,H10B), C11B(H11A,H11B), C12B(H12A,H12B), C13B(H13A,H13B), C10C(H10C,H10D), C11C(H11C,H11D), C12C(H12C,H12D), C13C(H13C, H13D) 7.b Aromatic/amide H refined with riding coordinates: N1(H1), N2(H2), C2(H2A), C3(H3), C4(H4), C5(H5), C6(H6), N1B(H1B), N2B(H2B), C2B(H2BA), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B) 7.c Idealised Me refined as rotating group: C14(H14G,H14H,H14I), C14B(H14A,H14B,H14C), C14C(H14D,H14E,H14F) ; _shelx_res_file ; TITL svshcan_a.res in P-1 svshcan.res created by SHELXL-2018/3 at 09:27:22 on 12-Oct-2018 REM Old TITL SVSHCAN in P-1 REM SHELXT solution in P-1: R1 0.208, Rweak 0.037, Alpha 0.091 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C29 N3 O3 S2 CELL 0.71073 9.5041 10.2883 15.1931 96.577 99.785 96.172 ZERR 4 0.0011 0.0011 0.0017 0.004 0.004 0.004 LATT 1 SFAC C H N O S UNIT 56 80 8 4 4 EQIV $1 +X,1+Y,+Z EQIV $2 +X,-1+Y,+Z DFIX 1.54 0.005 C13B C14B C13B C12B C11B C12B C11B C10B C10B C9B DFIX 2.5 0.005 C9B C11B C10B C12B C11B C13B C12B C14B DFIX 2.5 C10 C12 C9 C11 C11 C13 C9 C11A C10 C12A C11A C13 SADI 0.01 C11A C10 C11 C10 C12A C11A C12 C11 C13 C12 C13 C12A SIMU 0.01 0.02 2 C10 > C12A C9B > C14C RIGU 0.01 0.01 C10 > C12A C9B > C14C L.S. 10 PLAN 20 SIZE 0.124 0.153 0.241 TEMP -163.15 HTAB N1 O1 HTAB N1 O3B HTAB N2 S2_$1 HTAB N1B O1 HTAB N1B O3B HTAB N2B S1_$2 BOND $H more -1 wpdb -1 htab conf acta OMIT -4 45 OMIT -2 0 2 REM REM REM WGHT 0.033400 6.050500 FVAR 0.66985 0.51100 0.61544 S1 5 0.556677 1.118074 0.714251 11.00000 0.02112 0.02269 = 0.02982 0.00262 -0.00500 -0.00145 O1 4 0.245810 0.759530 0.570652 11.00000 0.02459 0.02027 = 0.02019 0.00599 0.00068 0.00385 N1 3 0.468447 0.861042 0.702587 11.00000 0.02328 0.01791 = 0.01689 -0.00160 -0.00128 0.00482 AFIX 43 H1 2 0.412588 0.789902 0.673628 11.00000 -1.20000 AFIX 0 N2 3 0.365448 0.967733 0.586752 11.00000 0.01673 0.01937 = 0.02171 0.00913 -0.00033 0.00157 AFIX 43 H2 2 0.370256 1.039792 0.560704 11.00000 -1.20000 AFIX 0 C1 1 0.562898 0.848634 0.784737 11.00000 0.01759 0.02045 = 0.01789 0.00377 -0.00030 -0.00082 C2 1 0.544526 0.912362 0.866186 11.00000 0.02935 0.03093 = 0.02473 -0.00117 0.00662 0.01119 AFIX 43 H2A 2 0.470049 0.966613 0.868423 11.00000 -1.20000 AFIX 0 C3 1 0.635218 0.896701 0.944450 11.00000 0.03985 0.04973 = 0.01321 -0.00188 -0.00045 0.00841 AFIX 43 H3 2 0.624397 0.941802 1.000577 11.00000 -1.20000 AFIX 0 C4 1 0.741561 0.815682 0.941345 11.00000 0.03210 0.04493 = 0.02136 0.00386 -0.00712 0.00369 AFIX 43 H4 2 0.802554 0.803744 0.995414 11.00000 -1.20000 AFIX 0 C5 1 0.759145 0.752298 0.859979 11.00000 0.02419 0.04239 = 0.02690 0.00345 -0.00401 0.01177 AFIX 43 H5 2 0.833238 0.697525 0.858191 11.00000 -1.20000 AFIX 0 C6 1 0.669916 0.767371 0.780380 11.00000 0.02884 0.03152 = 0.01772 -0.00037 0.00355 0.00972 AFIX 43 H6 2 0.681768 0.723133 0.724223 11.00000 -1.20000 AFIX 0 C7 1 0.459943 0.972996 0.667474 11.00000 0.01483 0.02189 = 0.01570 -0.00239 0.00515 0.00507 C8 1 0.264312 0.864325 0.541426 11.00000 0.01393 0.01893 = 0.01839 0.00097 0.00485 0.00187 C9 1 0.182005 0.893347 0.453362 11.00000 0.01854 0.02283 = 0.01941 0.00671 0.00016 0.00053 AFIX 23 H9A 2 0.237283 0.871763 0.405166 11.00000 -1.20000 H9B 2 0.174515 0.989040 0.458111 11.00000 -1.20000 AFIX 0 C10 1 0.031295 0.817585 0.426141 11.00000 0.02282 0.03922 = 0.03207 0.02208 -0.00489 -0.00719 PART 1 AFIX 23 H10E 2 -0.033452 0.857883 0.462847 31.00000 -1.20000 H10F 2 0.033996 0.725219 0.438119 31.00000 -1.20000 AFIX 23 PART 0 PART 2 H10G 2 -0.009418 0.805378 0.480884 -31.00000 -1.20000 H10H 2 0.036628 0.729189 0.394390 -31.00000 -1.20000 AFIX 0 PART 0 C13 1 -0.125230 0.947604 0.203360 11.00000 0.03956 0.05880 = 0.02973 0.01020 -0.00848 0.00524 PART 1 AFIX 23 H13E 2 -0.068307 0.905705 0.161849 31.00000 -1.20000 H13F 2 -0.222866 0.897612 0.193282 31.00000 -1.20000 AFIX 23 PART 0 PART 2 H13G 2 -0.114855 0.907306 0.142813 -31.00000 -1.20000 H13H 2 -0.224439 0.915082 0.209633 -31.00000 -1.20000 AFIX 0 PART 0 C14 1 -0.130588 1.089676 0.193741 11.00000 0.05224 0.05179 = 0.10618 -0.01498 0.02834 -0.01167 AFIX 137 H14G 2 -0.180868 1.129595 0.239061 11.00000 -1.50000 H14H 2 -0.182089 1.097374 0.133336 11.00000 -1.50000 H14I 2 -0.032328 1.135445 0.202503 11.00000 -1.50000 AFIX 0 PART 1 C11 1 -0.029167 0.819124 0.323617 31.00000 0.02031 0.03030 = 0.03168 0.00788 -0.00423 -0.00175 AFIX 23 H11E 2 0.038020 0.782514 0.287184 31.00000 -1.20000 H11F 2 -0.122989 0.762197 0.306244 31.00000 -1.20000 AFIX 0 C12 1 -0.048866 0.959758 0.303063 31.00000 0.02173 0.03504 = 0.02570 0.00061 0.00083 0.00390 AFIX 23 H12E 2 0.045805 1.014909 0.312382 31.00000 -1.20000 H12F 2 -0.108070 1.001068 0.343316 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C11A 1 -0.069045 0.891770 0.363805 -31.00000 0.01778 0.03389 = 0.02919 0.01085 -0.00084 0.00049 AFIX 23 H11G 2 -0.170922 0.855425 0.360274 -31.00000 -1.20000 H11H 2 -0.056551 0.986715 0.387820 -31.00000 -1.20000 AFIX 0 C12A 1 -0.028130 0.873320 0.269352 -31.00000 0.02652 0.03900 = 0.02685 0.00281 -0.00304 0.00568 AFIX 23 H12G 2 -0.041017 0.778181 0.245818 -31.00000 -1.20000 H12H 2 0.074347 0.908341 0.273673 -31.00000 -1.20000 AFIX 0 PART 0 S2 5 0.348180 0.238414 0.478522 11.00000 0.02479 0.02043 = 0.01894 0.00183 0.00311 0.00605 O3B 4 0.344125 0.574894 0.699412 11.00000 0.03073 0.02653 = 0.02081 0.00105 -0.00277 0.00924 N1B 3 0.263173 0.469484 0.527562 11.00000 0.02086 0.01640 = 0.01849 -0.00048 0.00048 0.00474 AFIX 43 H1B 2 0.258555 0.533975 0.569922 11.00000 -1.20000 AFIX 0 N2B 3 0.379344 0.368406 0.642559 11.00000 0.01841 0.02323 = 0.01651 0.00424 0.00244 0.00534 AFIX 43 H2B 2 0.410656 0.295388 0.658211 11.00000 -1.20000 AFIX 0 C1B 1 0.201508 0.479963 0.435841 11.00000 0.02069 0.01388 = 0.01282 -0.00062 0.00187 0.00459 C2B 1 0.069133 0.410106 0.396418 11.00000 0.01931 0.02023 = 0.02368 0.00589 0.00187 0.00016 AFIX 43 H2BA 2 0.019713 0.352314 0.428842 11.00000 -1.20000 AFIX 0 C3B 1 0.009431 0.425264 0.309270 11.00000 0.02268 0.01980 = 0.02821 -0.00137 -0.00498 -0.00359 AFIX 43 H3B 2 -0.081181 0.377013 0.281526 11.00000 -1.20000 AFIX 0 C4B 1 0.079676 0.509066 0.262720 11.00000 0.03364 0.02114 = 0.02016 0.00382 -0.00350 0.00504 AFIX 43 H4B 2 0.037693 0.519058 0.202909 11.00000 -1.20000 AFIX 0 C5B 1 0.212090 0.579539 0.302596 11.00000 0.03795 0.02107 = 0.02355 0.00434 0.01013 -0.00373 AFIX 43 H5B 2 0.261167 0.637063 0.269840 11.00000 -1.20000 AFIX 0 C6B 1 0.273195 0.566255 0.390331 11.00000 0.01667 0.02510 = 0.02098 -0.00275 0.00453 -0.00224 AFIX 43 H6B 2 0.362896 0.615797 0.418526 11.00000 -1.20000 AFIX 0 C7B 1 0.326707 0.366790 0.551050 11.00000 0.01151 0.01805 = 0.01959 0.00365 0.00238 -0.00555 C8B 1 0.388606 0.470272 0.711915 11.00000 0.01615 0.03053 = 0.01689 0.00109 0.00202 0.00571 C9B 1 0.457836 0.441426 0.802481 11.00000 0.04446 0.04317 = 0.01762 0.00119 -0.00137 0.02247 PART 1 AFIX 23 H9BA 2 0.562199 0.440965 0.803453 21.00000 -1.20000 H9BB 2 0.417360 0.351900 0.810884 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H9BC 2 0.542263 0.508001 0.828291 -21.00000 -1.20000 H9BD 2 0.490414 0.353110 0.797256 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C10B 1 0.438198 0.538870 0.881308 21.00000 0.04172 0.04623 = 0.00769 -0.00224 -0.00331 0.02218 AFIX 23 H10A 2 0.448405 0.629472 0.865108 21.00000 -1.20000 H10B 2 0.513971 0.535248 0.934123 21.00000 -1.20000 AFIX 0 C11B 1 0.289152 0.506634 0.905943 21.00000 0.05526 0.07766 = 0.01755 0.00041 0.00329 0.02914 AFIX 23 H11A 2 0.287282 0.429800 0.939641 21.00000 -1.20000 H11B 2 0.213757 0.486314 0.850923 21.00000 -1.20000 AFIX 0 C12B 1 0.264129 0.632944 0.965904 21.00000 0.07707 0.09318 = 0.03017 0.00757 0.01123 0.00889 AFIX 23 H12A 2 0.349485 0.662219 1.014104 21.00000 -1.20000 H12B 2 0.250172 0.705116 0.928710 21.00000 -1.20000 AFIX 0 C13B 1 0.131855 0.602401 1.007572 21.00000 0.07808 0.10849 = 0.05212 -0.00211 0.00975 0.02287 AFIX 23 H13A 2 0.142689 0.526225 1.041371 21.00000 -1.20000 H13B 2 0.045126 0.579552 0.959640 21.00000 -1.20000 AFIX 0 C14B 1 0.115378 0.724693 1.071616 21.00000 0.07761 0.07424 = 0.05936 0.00163 -0.00652 0.05072 AFIX 137 H14A 2 0.114725 0.801694 1.039155 21.00000 -1.50000 H14B 2 0.196159 0.740516 1.122724 21.00000 -1.50000 H14C 2 0.024759 0.709749 1.093756 21.00000 -1.50000 AFIX 0 SAME 0.005 0.04 C10B > C14B PART 0 PART 2 C10C 1 0.329430 0.446853 0.870308 -21.00000 0.06339 0.05797 = 0.02770 0.00512 -0.01176 0.01701 AFIX 23 H10C 2 0.231773 0.417636 0.834368 -21.00000 -1.20000 H10D 2 0.347932 0.389767 0.918121 -21.00000 -1.20000 AFIX 0 C11C 1 0.344184 0.591660 0.911079 -21.00000 0.06154 0.07386 = 0.02705 0.00569 0.00187 0.01133 AFIX 23 H11C 2 0.315807 0.647767 0.863998 -21.00000 -1.20000 H11D 2 0.444428 0.623570 0.941834 -21.00000 -1.20000 AFIX 0 C12C 1 0.238767 0.592885 0.980400 -21.00000 0.05984 0.10684 = 0.02488 0.00209 0.02373 0.01149 AFIX 23 H12C 2 0.137931 0.563157 0.949920 -21.00000 -1.20000 H12D 2 0.266118 0.536515 1.027493 -21.00000 -1.20000 AFIX 0 C13C 1 0.259542 0.738100 1.019781 -21.00000 0.07012 0.09818 = 0.04883 0.01362 0.02460 0.02829 AFIX 23 H13C 2 0.256974 0.792672 0.970069 -21.00000 -1.20000 H13D 2 0.355592 0.760041 1.059062 -21.00000 -1.20000 AFIX 0 C14C 1 0.144468 0.772580 1.074470 -21.00000 0.04568 0.06972 = 0.05681 0.02148 0.01418 0.00443 AFIX 137 H14D 2 0.049085 0.751239 1.035912 -21.00000 -1.50000 H14E 2 0.161395 0.867037 1.097239 -21.00000 -1.50000 H14F 2 0.149157 0.721568 1.125316 -21.00000 -1.50000 AFIX 0 HKLF 4 REM svshcan_a.res in P-1 REM wR2 = 0.1719, GooF = S = 1.142, Restrained GooF = 1.161 for all data REM R1 = 0.0770 for 3017 Fo > 4sig(Fo) and 0.0939 for all 3710 data REM 393 parameters refined using 334 restraints END WGHT 0.0334 6.0506 REM Instructions for potential hydrogen bonds HTAB N1 O1 HTAB N1 O3B HTAB N2 S2_$1 EQIV $3 -x+1, -y+2, -z+1 HTAB C9 S1_$3 HTAB C9 S2_$1 HTAB N1B O1 HTAB N1B O3B HTAB N2B S1_$2 HTAB C9B S1_$2 REM Highest difference peak 1.172, deepest hole -0.641, 1-sigma level 0.082 Q1 1 0.1795 0.6753 0.9690 11.00000 0.05 1.17 Q2 1 0.2196 0.5135 0.9840 11.00000 0.05 0.99 Q3 1 0.2598 0.4545 0.9008 11.00000 0.05 0.73 Q4 1 0.1667 0.7559 1.0466 11.00000 0.05 0.37 Q5 1 0.1441 0.5884 0.9216 11.00000 0.05 0.32 Q6 1 0.2645 0.7630 1.0449 11.00000 0.05 0.31 Q7 1 0.2413 0.9153 0.2332 11.00000 0.05 0.27 Q8 1 -0.0445 0.8321 0.2976 11.00000 0.05 0.26 Q9 1 0.4938 1.0786 0.7423 11.00000 0.05 0.26 Q10 1 -0.0632 1.1203 0.1564 11.00000 0.05 0.25 Q11 1 0.3318 0.7344 0.3026 11.00000 0.05 0.24 Q12 1 0.5525 0.6722 0.8714 11.00000 0.05 0.24 Q13 1 0.2433 1.0880 0.4674 11.00000 0.05 0.24 Q14 1 0.3304 0.5837 0.2792 11.00000 0.05 0.24 Q15 1 0.3423 0.2973 0.9603 11.00000 0.05 0.24 Q16 1 0.1057 0.6840 0.4832 11.00000 0.05 0.23 Q17 1 0.0382 0.7093 0.4197 11.00000 0.05 0.23 Q18 1 0.1905 0.5679 0.4434 11.00000 0.05 0.22 Q19 1 0.4937 0.5591 0.6427 11.00000 0.05 0.22 Q20 1 0.2625 0.4814 0.3966 11.00000 0.05 0.22 ; _shelx_res_checksum 55026 _shelx_hkl_file ; 1 0 0 1557.74 73.59 -2 0 0 230.58 11.60 -2 0 0 216.88 11.50 2 0 0 216.88 11.50 2 0 0 221.08 11.70 -3 0 0 673.73 32.10 -3 0 0 642.84 32.80 3 0 0 672.53 32.50 3 0 0 615.74 31.90 -4 0 0 56.39 5.70 -4 0 0 63.49 5.20 4 0 0 60.19 5.30 4 0 0 63.49 5.50 -5 0 0 40.20 5.30 -5 0 0 50.89 5.30 5 0 0 48.00 5.80 5 0 0 32.70 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40.90 6.90 -5 -4 5 29.80 7.70 -5 -4 5 21.80 8.20 4 4 -5 209.98 14.90 -4 -4 5 196.28 14.90 -4 -4 5 229.88 14.70 3 4 -5 31.50 5.50 -3 -4 5 25.80 6.30 -3 -4 5 37.80 5.40 2 4 -5 130.29 9.90 2 4 -5 143.59 10.00 -2 -4 5 138.09 10.60 -2 -4 5 144.89 9.50 1 4 -5 10.10 3.20 -1 -4 5 0.80 1.50 -1 -4 5 0.30 1.10 0 4 -5 82.49 6.80 0 4 -5 76.19 6.70 0 -4 5 78.59 5.50 0 -4 5 79.49 7.50 -1 4 -5 22.30 2.90 -1 4 -5 16.30 3.80 1 -4 5 23.60 2.20 -2 4 -5 281.47 17.10 2 -4 5 297.87 17.80 -3 4 -5 160.18 11.20 3 -4 5 143.29 11.80 -4 4 -5 -1.60 1.50 4 -4 5 1.70 2.10 -5 4 -5 308.47 19.80 -5 4 -5 274.67 15.40 5 -4 5 301.47 19.40 5 -4 5 320.47 15.80 -6 4 -5 1.70 1.50 -6 4 -5 2.50 2.40 6 -4 5 -1.20 2.20 6 -4 5 0.40 3.00 -7 4 -5 109.49 8.80 -7 4 -5 110.99 12.20 7 -4 5 105.19 10.00 7 -4 5 97.59 13.90 -8 4 -5 149.59 12.30 -8 4 -5 183.98 17.60 8 -4 5 179.98 14.10 9 -4 5 53.79 12.40 -10 4 -5 -8.00 5.30 -9 -3 5 19.70 10.20 8 3 -5 766.02 43.30 -8 -3 5 683.53 38.90 7 3 -5 267.97 20.80 -7 -3 5 298.27 18.80 -7 -3 5 298.97 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4.10 0 1 -16 111.19 10.90 0 1 -16 107.59 15.00 -1 1 -16 32.20 8.20 -2 1 -16 35.00 8.70 -3 1 -16 36.30 16.00 -4 1 -16 10.10 6.30 7 0 -16 85.59 14.10 6 0 -16 30.50 11.20 5 0 -16 41.70 11.30 5 0 -16 43.30 9.50 4 0 -16 1.00 3.00 4 0 -16 1.20 3.20 3 0 -16 28.40 10.60 2 0 -16 17.20 9.40 1 0 -16 89.49 10.10 1 0 -16 83.99 13.70 0 0 -16 49.80 9.30 0 0 -16 46.80 13.30 -1 0 -16 137.69 12.70 -2 0 -16 11.60 5.40 -2 0 -16 8.50 4.00 -3 0 -16 47.90 16.50 7 -1 -16 0.30 4.30 6 -1 -16 31.90 11.30 6 -1 -16 33.10 12.70 5 -1 -16 -0.60 2.90 5 -1 -16 -4.10 3.40 4 -1 -16 141.69 14.40 4 -1 -16 122.59 13.70 -4 1 16 123.39 21.20 3 -1 -16 50.69 11.20 2 -1 -16 2.30 3.90 2 -1 -16 5.90 3.20 1 -1 -16 22.30 9.40 0 -1 -16 3.40 3.70 0 -1 -16 -1.70 3.80 -1 -1 -16 45.20 15.90 -2 -1 -16 135.49 18.80 -2 -1 -16 115.69 22.20 -3 -1 -16 157.08 22.80 -3 -1 -16 160.18 17.40 7 -2 -16 101.09 15.40 6 -2 -16 132.29 16.10 5 -2 -16 7.40 4.00 5 -2 -16 3.20 3.30 4 -2 -16 -5.10 3.10 3 -2 -16 83.79 10.70 3 -2 -16 58.69 12.10 2 -2 -16 63.99 12.70 1 -2 -16 93.99 15.20 1 -2 -16 119.49 14.70 0 -2 -16 -3.70 4.50 0 -2 -16 8.20 4.90 -1 -2 -16 82.19 16.90 -2 -2 -16 100.69 18.10 -2 -2 -16 55.79 15.30 6 -3 -16 15.50 4.80 5 -3 -16 9.40 4.30 4 -3 -16 -2.80 3.20 4 -3 -16 4.00 4.20 3 -3 -16 4.20 3.90 3 -3 -16 5.80 3.60 2 -3 -16 85.69 13.10 2 -3 -16 84.19 13.80 1 -3 -16 9.90 4.90 1 -3 -16 8.10 4.30 0 -3 -16 0.00 4.90 0 -3 -16 6.50 4.80 -1 -3 -16 66.79 16.50 -1 -3 -16 58.29 17.80 -2 -3 -16 137.69 23.40 -2 -3 -16 133.39 20.30 5 -4 -16 127.29 15.30 4 -4 -16 4.40 4.90 3 -4 -16 106.19 14.60 3 -4 -16 134.29 14.90 2 -4 -16 25.20 13.90 1 -4 -16 110.99 17.40 1 -4 -16 112.79 17.10 0 -4 -16 41.40 17.20 0 -4 -16 55.49 17.60 3 -5 -16 63.59 16.30 2 -5 -16 -5.50 5.80 2 -5 -16 4.50 4.60 2 6 -17 50.29 15.50 1 6 -17 -3.70 4.70 0 6 -17 16.80 5.60 4 5 -17 81.09 18.40 4 5 -17 70.69 13.50 3 5 -17 33.00 13.80 2 5 -17 10.30 3.80 2 5 -17 11.80 5.40 1 5 -17 -5.20 4.70 1 5 -17 -4.30 3.30 0 5 -17 1.50 4.70 -1 5 -17 12.00 5.20 5 4 -17 2.50 4.50 5 4 -17 8.70 5.10 4 4 -17 4.90 4.00 4 4 -17 2.20 4.30 3 4 -17 94.69 15.50 3 4 -17 97.69 14.00 2 4 -17 16.90 5.20 2 4 -17 39.50 9.70 1 4 -17 32.20 8.70 1 4 -17 39.60 13.60 0 4 -17 7.80 4.90 0 4 -17 -0.90 3.10 -1 4 -17 60.09 16.90 -2 4 -17 28.70 15.40 5 3 -17 -1.10 4.40 5 3 -17 5.70 4.10 4 3 -17 20.30 11.00 4 3 -17 51.99 14.50 3 3 -17 30.80 13.60 3 3 -17 32.40 9.20 2 3 -17 22.00 8.60 1 3 -17 97.49 10.50 1 3 -17 75.99 15.80 0 3 -17 12.70 5.30 0 3 -17 29.00 8.00 -1 3 -17 7.60 4.90 -2 3 -17 147.99 19.90 6 2 -17 85.49 16.20 6 2 -17 83.49 15.00 5 2 -17 179.68 19.50 5 2 -17 209.38 18.00 4 2 -17 82.89 11.80 4 2 -17 77.89 14.60 3 2 -17 25.30 13.00 2 2 -17 26.30 12.90 2 2 -17 27.00 13.10 1 2 -17 33.30 12.10 1 2 -17 23.80 8.60 0 2 -17 -4.70 3.80 -1 2 -17 3.30 2.60 -1 2 -17 -1.80 5.00 -2 2 -17 -3.10 5.30 6 1 -17 29.50 13.30 5 1 -17 36.40 11.80 5 1 -17 33.90 13.10 4 1 -17 -4.70 3.40 4 1 -17 6.10 4.00 3 1 -17 5.20 3.10 3 1 -17 -5.90 3.70 2 1 -17 -4.00 2.90 2 1 -17 -0.60 4.00 1 1 -17 129.29 12.70 1 1 -17 85.49 16.00 0 1 -17 72.59 10.20 -1 1 -17 7.50 5.10 -1 1 -17 -1.10 3.00 -2 1 -17 2.30 3.10 -2 1 -17 8.40 5.40 6 0 -17 10.70 4.80 6 0 -17 7.40 4.40 5 0 -17 0.30 3.50 5 0 -17 1.50 3.70 4 0 -17 1.50 3.50 3 0 -17 28.90 12.90 2 0 -17 4.60 3.10 2 0 -17 -1.10 4.10 1 0 -17 123.89 16.70 1 0 -17 117.19 12.20 0 0 -17 78.99 15.70 0 0 -17 49.60 10.70 -1 0 -17 83.79 15.90 -2 0 -17 -5.50 5.40 6 -1 -17 2.20 3.90 5 -1 -17 34.80 12.30 5 -1 -17 16.00 4.70 4 -1 -17 67.49 13.70 4 -1 -17 93.99 13.10 3 -1 -17 30.50 10.90 2 -1 -17 2.10 3.90 2 -1 -17 2.10 3.60 1 -1 -17 14.40 4.10 1 -1 -17 36.50 12.40 0 -1 -17 -1.30 4.40 0 -1 -17 -0.70 3.50 -1 -1 -17 -3.40 4.30 -1 -1 -17 -8.10 4.50 -2 -1 -17 13.80 5.30 5 -2 -17 -1.50 4.20 4 -2 -17 -1.40 3.80 4 -2 -17 -5.20 3.70 3 -2 -17 4.40 4.10 3 -2 -17 2.30 3.90 2 -2 -17 0.60 4.20 2 -2 -17 0.30 4.00 1 -2 -17 32.50 12.10 0 -2 -17 47.90 14.10 -1 -2 -17 5.80 5.10 -1 -2 -17 13.40 5.90 4 -3 -17 8.00 4.70 3 -3 -17 -5.70 4.20 3 -3 -17 3.30 4.20 2 -3 -17 40.40 13.20 1 -3 -17 33.10 13.80 0 -3 -17 -5.40 5.10 0 -3 -17 -3.70 5.60 3 4 -18 98.89 13.40 3 4 -18 88.39 17.30 2 4 -18 4.90 3.90 2 4 -18 4.00 5.30 1 4 -18 -6.60 5.00 4 3 -18 4.30 5.10 4 3 -18 27.60 11.10 3 3 -18 70.79 15.40 3 3 -18 51.29 10.80 2 3 -18 1.70 3.90 2 3 -18 2.00 5.30 1 3 -18 2.60 3.00 1 3 -18 4.60 4.90 0 3 -18 -2.20 5.00 4 2 -18 1.40 4.70 4 2 -18 23.20 11.00 3 2 -18 36.80 14.70 2 2 -18 5.90 5.00 2 2 -18 3.70 3.50 1 2 -18 -8.30 4.50 0 2 -18 2.80 5.30 0 2 -18 -3.70 3.00 4 1 -18 3.00 3.70 4 1 -18 3.70 4.70 3 1 -18 25.80 10.30 2 1 -18 -1.60 3.10 2 1 -18 -1.30 4.50 1 1 -18 24.50 9.20 1 1 -18 32.90 15.30 0 1 -18 0.80 4.80 4 0 -18 7.60 4.50 4 0 -18 0.60 4.00 3 0 -18 10.50 4.10 3 0 -18 15.20 5.20 2 0 -18 93.09 17.10 2 0 -18 104.79 12.30 1 0 -18 7.70 5.00 1 0 -18 1.10 3.50 0 0 -18 11.60 5.90 0 0 -18 10.60 4.00 4 -1 -18 3.90 4.40 3 -1 -18 42.20 11.60 2 -1 -18 -0.80 4.90 1 -1 -18 9.80 4.10 1 -1 -18 6.90 5.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 58130 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.55668(13) 1.11807(13) 0.71425(9) 0.0261(4) Uani 1 1 d . . . . . O1 O 0.2458(3) 0.7595(3) 0.5707(2) 0.0218(8) Uani 1 1 d . . . . . N1 N 0.4684(4) 0.8610(4) 0.7026(2) 0.0201(9) Uani 1 1 d . . . . . H1 H 0.412588 0.789902 0.673628 0.024 Uiso 1 1 calc R . . . . N2 N 0.3654(4) 0.9677(4) 0.5868(3) 0.0193(9) Uani 1 1 d . . . . . H2 H 0.370256 1.039792 0.560704 0.023 Uiso 1 1 calc R . . . . C1 C 0.5629(5) 0.8486(5) 0.7847(3) 0.0192(11) Uani 1 1 d . . . . . C2 C 0.5445(6) 0.9124(5) 0.8662(3) 0.0280(13) Uani 1 1 d . . . . . H2A H 0.470049 0.966613 0.868423 0.034 Uiso 1 1 calc R . . . . C3 C 0.6352(6) 0.8967(6) 0.9444(3) 0.0352(14) Uani 1 1 d . . . . . H3 H 0.624397 0.941802 1.000577 0.042 Uiso 1 1 calc R . . . . C4 C 0.7416(6) 0.8157(6) 0.9413(3) 0.0344(14) Uani 1 1 d . . . . . H4 H 0.802554 0.803744 0.995414 0.041 Uiso 1 1 calc R . . . . C5 C 0.7591(6) 0.7523(6) 0.8600(3) 0.0317(13) Uani 1 1 d . . . . . H5 H 0.833238 0.697525 0.858191 0.038 Uiso 1 1 calc R . . . . C6 C 0.6699(5) 0.7674(5) 0.7804(3) 0.0260(12) Uani 1 1 d . . . . . H6 H 0.681768 0.723133 0.724223 0.031 Uiso 1 1 calc R . . . . C7 C 0.4599(5) 0.9730(5) 0.6675(3) 0.0174(11) Uani 1 1 d . . . . . C8 C 0.2643(5) 0.8643(5) 0.5414(3) 0.0170(11) Uani 1 1 d . . . . . C9 C 0.1820(5) 0.8933(5) 0.4534(3) 0.0205(11) Uani 1 1 d D . . . . H9A H 0.237283 0.871763 0.405166 0.025 Uiso 1 1 calc R . . . . H9B H 0.174515 0.989040 0.458111 0.025 Uiso 1 1 calc R . . . . C10 C 0.0313(5) 0.8176(5) 0.4261(3) 0.0320(13) Uani 1 1 d D U . . . H10E H -0.033452 0.857883 0.462847 0.038 Uiso 0.615(8) 1 calc R . P A 1 H10F H 0.033996 0.725219 0.438119 0.038 Uiso 0.615(8) 1 calc R . P A 1 H10G H -0.009418 0.805378 0.480884 0.038 Uiso 0.385(8) 1 calc R . P A 2 H10H H 0.036628 0.729189 0.394390 0.038 Uiso 0.385(8) 1 calc R . P A 2 C13 C -0.1252(6) 0.9476(6) 0.2034(3) 0.0442(15) Uani 1 1 d D U . . . H13E H -0.068307 0.905705 0.161849 0.053 Uiso 0.615(8) 1 calc R . P A 1 H13F H -0.222866 0.897612 0.193282 0.053 Uiso 0.615(8) 1 calc R . P A 1 H13G H -0.114855 0.907306 0.142813 0.053 Uiso 0.385(8) 1 calc R . P A 2 H13H H -0.224439 0.915082 0.209633 0.053 Uiso 0.385(8) 1 calc R . P A 2 C14 C -0.1306(8) 1.0897(7) 0.1937(6) 0.072(2) Uani 1 1 d . U . . . H14G H -0.180868 1.129595 0.239061 0.108 Uiso 1 1 calc GR . . . . H14H H -0.182089 1.097374 0.133336 0.108 Uiso 1 1 calc GR . . . . H14I H -0.032328 1.135445 0.202503 0.108 Uiso 1 1 calc GR . . . . C11 C -0.0292(9) 0.8191(7) 0.3236(5) 0.0286(19) Uani 0.615(8) 1 d D U P A 1 H11E H 0.038020 0.782514 0.287184 0.034 Uiso 0.615(8) 1 calc R . P A 1 H11F H -0.122989 0.762197 0.306244 0.034 Uiso 0.615(8) 1 calc R . P A 1 C12 C -0.0489(9) 0.9598(8) 0.3031(4) 0.0282(19) Uani 0.615(8) 1 d D U P A 1 H12E H 0.045805 1.014909 0.312382 0.034 Uiso 0.615(8) 1 calc R . P A 1 H12F H -0.108070 1.001068 0.343316 0.034 Uiso 0.615(8) 1 calc R . P A 1 C11A C -0.0690(11) 0.8918(13) 0.3638(6) 0.027(2) Uani 0.385(8) 1 d D U P A 2 H11G H -0.170922 0.855425 0.360274 0.033 Uiso 0.385(8) 1 calc R . P A 2 H11H H -0.056551 0.986715 0.387820 0.033 Uiso 0.385(8) 1 calc R . P A 2 C12A C -0.0281(14) 0.8733(14) 0.2694(6) 0.032(3) Uani 0.385(8) 1 d D U P A 2 H12G H -0.041017 0.778181 0.245818 0.038 Uiso 0.385(8) 1 calc R . P A 2 H12H H 0.074347 0.908341 0.273673 0.038 Uiso 0.385(8) 1 calc R . P A 2 S2 S 0.34818(13) 0.23841(12) 0.47852(8) 0.0213(3) Uani 1 1 d . . . . . O3B O 0.3441(4) 0.5749(3) 0.6994(2) 0.0267(8) Uani 1 1 d . . . . . N1B N 0.2632(4) 0.4695(4) 0.5276(2) 0.0190(9) Uani 1 1 d . . . . . H1B H 0.258555 0.533975 0.569922 0.023 Uiso 1 1 calc R . . . . N2B N 0.3793(4) 0.3684(4) 0.6426(2) 0.0192(9) Uani 1 1 d . . . . . H2B H 0.410656 0.295388 0.658211 0.023 Uiso 1 1 calc R . . . . C1B C 0.2015(5) 0.4800(4) 0.4358(3) 0.0160(11) Uani 1 1 d . . . . . C2B C 0.0691(5) 0.4101(5) 0.3964(3) 0.0213(11) Uani 1 1 d . . . . . H2BA H 0.019713 0.352314 0.428842 0.026 Uiso 1 1 calc R . . . . C3B C 0.0094(5) 0.4253(5) 0.3093(3) 0.0256(12) Uani 1 1 d . . . . . H3B H -0.081181 0.377013 0.281526 0.031 Uiso 1 1 calc R . . . . C4B C 0.0797(6) 0.5091(5) 0.2627(3) 0.0258(12) Uani 1 1 d . . . . . H4B H 0.037693 0.519058 0.202909 0.031 Uiso 1 1 calc R . . . . C5B C 0.2121(6) 0.5795(5) 0.3026(3) 0.0275(12) Uani 1 1 d . . . . . H5B H 0.261167 0.637063 0.269840 0.033 Uiso 1 1 calc R . . . . C6B C 0.2732(5) 0.5663(5) 0.3903(3) 0.0216(11) Uani 1 1 d . . . . . H6B H 0.362896 0.615797 0.418526 0.026 Uiso 1 1 calc R . . . . C7B C 0.3267(5) 0.3668(5) 0.5510(3) 0.0169(11) Uani 1 1 d . . . . . C8B C 0.3886(5) 0.4703(5) 0.7119(3) 0.0213(12) Uani 1 1 d . . . . . C9B C 0.4578(6) 0.4414(6) 0.8025(3) 0.0349(13) Uani 1 1 d D U . . . H9BA H 0.562199 0.440965 0.803453 0.042 Uiso 0.511(6) 1 calc R . P B 1 H9BB H 0.417360 0.351900 0.810884 0.042 Uiso 0.511(6) 1 calc R . P B 1 H9BC H 0.542263 0.508001 0.828291 0.042 Uiso 0.489(6) 1 calc R . P B 2 H9BD H 0.490414 0.353110 0.797256 0.042 Uiso 0.489(6) 1 calc R . P B 2 C10B C 0.4382(8) 0.5389(9) 0.8813(5) 0.032(2) Uani 0.511(6) 1 d D U P B 1 H10A H 0.448405 0.629472 0.865108 0.038 Uiso 0.511(6) 1 calc R . P B 1 H10B H 0.513971 0.535248 0.934123 0.038 Uiso 0.511(6) 1 calc R . P B 1 C11B C 0.2892(9) 0.5066(10) 0.9059(7) 0.050(2) Uani 0.511(6) 1 d D U P B 1 H11A H 0.287282 0.429800 0.939641 0.059 Uiso 0.511(6) 1 calc R . P B 1 H11B H 0.213757 0.486314 0.850923 0.059 Uiso 0.511(6) 1 calc R . P B 1 C12B C 0.2641(14) 0.6329(10) 0.9659(11) 0.067(3) Uani 0.511(6) 1 d D U P B 1 H12A H 0.349485 0.662219 1.014104 0.080 Uiso 0.511(6) 1 calc R . P B 1 H12B H 0.250172 0.705116 0.928710 0.080 Uiso 0.511(6) 1 calc R . P B 1 C13B C 0.1319(12) 0.6024(12) 1.0076(9) 0.080(3) Uani 0.511(6) 1 d D U P B 1 H13A H 0.142689 0.526225 1.041371 0.096 Uiso 0.511(6) 1 calc R . P B 1 H13B H 0.045126 0.579552 0.959640 0.096 Uiso 0.511(6) 1 calc R . P B 1 C14B C 0.115(2) 0.7247(15) 1.0716(13) 0.070(5) Uani 0.511(6) 1 d D U P B 1 H14A H 0.114725 0.801694 1.039155 0.105 Uiso 0.511(6) 1 calc GR . P B 1 H14B H 0.196159 0.740516 1.122724 0.105 Uiso 0.511(6) 1 calc GR . P B 1 H14C H 0.024759 0.709749 1.093756 0.105 Uiso 0.511(6) 1 calc GR . P B 1 C10C C 0.3294(15) 0.4469(11) 0.8703(8) 0.051(3) Uani 0.489(6) 1 d D U P B 2 H10C H 0.231773 0.417636 0.834368 0.062 Uiso 0.489(6) 1 calc R . P B 2 H10D H 0.347932 0.389767 0.918121 0.062 Uiso 0.489(6) 1 calc R . P B 2 C11C C 0.3442(14) 0.5917(11) 0.9111(8) 0.055(3) Uani 0.489(6) 1 d D U P B 2 H11C H 0.315807 0.647767 0.863998 0.066 Uiso 0.489(6) 1 calc R . P B 2 H11D H 0.444428 0.623570 0.941834 0.066 Uiso 0.489(6) 1 calc R . P B 2 C12C C 0.2388(19) 0.5929(13) 0.9804(11) 0.062(3) Uani 0.489(6) 1 d D U P B 2 H12C H 0.137931 0.563157 0.949920 0.075 Uiso 0.489(6) 1 calc R . P B 2 H12D H 0.266118 0.536515 1.027493 0.075 Uiso 0.489(6) 1 calc R . P B 2 C13C C 0.2595(15) 0.7381(13) 1.0198(9) 0.069(3) Uani 0.489(6) 1 d D U P B 2 H13C H 0.256974 0.792672 0.970069 0.083 Uiso 0.489(6) 1 calc R . P B 2 H13D H 0.355592 0.760041 1.059062 0.083 Uiso 0.489(6) 1 calc R . P B 2 C14C C 0.144(2) 0.7726(19) 1.0745(15) 0.056(4) Uani 0.489(6) 1 d D U P B 2 H14D H 0.049085 0.751239 1.035912 0.084 Uiso 0.489(6) 1 calc GR . P B 2 H14E H 0.161395 0.867037 1.097239 0.084 Uiso 0.489(6) 1 calc GR . P B 2 H14F H 0.149157 0.721568 1.125316 0.084 Uiso 0.489(6) 1 calc GR . P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0211(7) 0.0227(8) 0.0298(7) 0.0026(6) -0.0050(6) -0.0014(6) O1 0.0246(19) 0.020(2) 0.0202(18) 0.0060(15) 0.0007(15) 0.0039(15) N1 0.023(2) 0.018(2) 0.017(2) -0.0016(18) -0.0013(18) 0.0048(18) N2 0.017(2) 0.019(2) 0.022(2) 0.0091(18) -0.0003(18) 0.0016(18) C1 0.018(3) 0.020(3) 0.018(3) 0.004(2) 0.000(2) -0.001(2) C2 0.029(3) 0.031(3) 0.025(3) -0.001(2) 0.007(2) 0.011(3) C3 0.040(3) 0.050(4) 0.013(3) -0.002(3) 0.000(2) 0.008(3) C4 0.032(3) 0.045(4) 0.021(3) 0.004(3) -0.007(2) 0.004(3) C5 0.024(3) 0.042(4) 0.027(3) 0.003(3) -0.004(2) 0.012(3) C6 0.029(3) 0.032(3) 0.018(3) 0.000(2) 0.004(2) 0.010(2) C7 0.015(2) 0.022(3) 0.016(2) -0.002(2) 0.005(2) 0.005(2) C8 0.014(2) 0.019(3) 0.018(3) 0.001(2) 0.005(2) 0.002(2) C9 0.019(3) 0.023(3) 0.019(3) 0.007(2) 0.000(2) 0.001(2) C10 0.023(3) 0.039(3) 0.032(3) 0.022(2) -0.005(2) -0.007(2) C13 0.040(3) 0.059(4) 0.030(3) 0.010(3) -0.008(3) 0.005(3) C14 0.052(4) 0.052(4) 0.106(6) -0.015(4) 0.028(4) -0.012(4) C11 0.020(4) 0.030(4) 0.032(4) 0.008(3) -0.004(3) -0.002(3) C12 0.022(4) 0.035(4) 0.026(4) 0.001(3) 0.001(3) 0.004(3) C11A 0.018(4) 0.034(5) 0.029(5) 0.011(4) -0.001(4) 0.000(4) C12A 0.027(5) 0.039(5) 0.027(5) 0.003(4) -0.003(4) 0.006(4) S2 0.0248(7) 0.0204(7) 0.0189(7) 0.0018(5) 0.0031(5) 0.0060(5) O3B 0.031(2) 0.027(2) 0.0208(19) 0.0011(15) -0.0028(15) 0.0092(17) N1B 0.021(2) 0.016(2) 0.018(2) -0.0005(17) 0.0005(17) 0.0047(18) N2B 0.018(2) 0.023(2) 0.017(2) 0.0042(18) 0.0024(17) 0.0053(18) C1B 0.021(3) 0.014(3) 0.013(2) -0.001(2) 0.002(2) 0.005(2) C2B 0.019(3) 0.020(3) 0.024(3) 0.006(2) 0.002(2) 0.000(2) C3B 0.023(3) 0.020(3) 0.028(3) -0.001(2) -0.005(2) -0.004(2) C4B 0.034(3) 0.021(3) 0.020(3) 0.004(2) -0.003(2) 0.005(2) C5B 0.038(3) 0.021(3) 0.024(3) 0.004(2) 0.010(2) -0.004(2) C6B 0.017(3) 0.025(3) 0.021(3) -0.003(2) 0.005(2) -0.002(2) C7B 0.012(2) 0.018(3) 0.020(3) 0.004(2) 0.002(2) -0.006(2) C8B 0.016(3) 0.031(3) 0.017(3) 0.001(2) 0.002(2) 0.006(2) C9B 0.044(3) 0.043(3) 0.018(3) 0.001(2) -0.001(2) 0.022(3) C10B 0.042(4) 0.046(5) 0.008(4) -0.002(4) -0.003(4) 0.022(4) C11B 0.055(5) 0.078(6) 0.018(4) 0.000(4) 0.003(4) 0.029(4) C12B 0.077(5) 0.093(6) 0.030(5) 0.008(5) 0.011(4) 0.009(5) C13B 0.078(6) 0.108(7) 0.052(5) -0.002(5) 0.010(5) 0.023(6) C14B 0.078(10) 0.074(11) 0.059(8) 0.002(8) -0.007(8) 0.051(8) C10C 0.063(5) 0.058(5) 0.028(5) 0.005(4) -0.012(4) 0.017(4) C11C 0.062(5) 0.074(5) 0.027(4) 0.006(4) 0.002(4) 0.011(5) C12C 0.060(5) 0.107(6) 0.025(5) 0.002(5) 0.024(4) 0.011(5) C13C 0.070(6) 0.098(6) 0.049(5) 0.014(5) 0.025(5) 0.028(5) C14C 0.046(8) 0.070(10) 0.057(8) 0.021(8) 0.014(7) 0.004(8) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 H1 117.9 . . ? C7 N1 H1 117.9 . . ? C7 N1 C1 124.2(4) . . ? C7 N2 H2 115.6 . . ? C7 N2 C8 128.7(4) . . ? C8 N2 H2 115.6 . . ? C2 C1 N1 120.7(4) . . ? C2 C1 C6 121.0(4) . . ? C6 C1 N1 118.3(4) . . ? C1 C2 H2A 120.2 . . ? C1 C2 C3 119.5(5) . . ? C3 C2 H2A 120.2 . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.2(5) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 119.6 . . ? C4 C5 C6 120.8(5) . . ? C6 C5 H5 119.6 . . ? C1 C6 H6 120.8 . . ? C5 C6 C1 118.5(4) . . ? C5 C6 H6 120.8 . . ? N1 C7 S1 124.3(3) . . ? N1 C7 N2 117.0(4) . . ? N2 C7 S1 118.7(3) . . ? O1 C8 N2 122.2(4) . . ? O1 C8 C9 123.9(4) . . ? N2 C8 C9 113.9(4) . . ? C8 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? C8 C9 C10 114.0(4) . . ? H9A C9 H9B 107.6 . . ? C10 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C9 C10 H10E 109.5 . . ? C9 C10 H10F 109.5 . . ? C9 C10 H10G 109.4 . . ? C9 C10 H10H 109.4 . . ? C9 C10 C11 110.9(5) . . ? C9 C10 C11A 111.2(6) . . ? H10E C10 H10F 108.0 . . ? H10G C10 H10H 108.0 . . ? C11 C10 H10E 109.5 . . ? C11 C10 H10F 109.5 . . ? C11A C10 H10G 109.4 . . ? C11A C10 H10H 109.4 . . ? H13E C13 H13F 109.5 . . ? H13G C13 H13H 105.4 . . ? C14 C13 H13E 111.7 . . ? C14 C13 H13F 111.7 . . ? C14 C13 H13G 103.8 . . ? C14 C13 H13H 103.8 . . ? C14 C13 C12 100.2(6) . . ? C14 C13 C12A 133.5(8) . . ? C12 C13 H13E 111.7 . . ? C12 C13 H13F 111.7 . . ? C12A C13 H13G 103.8 . . ? C12A C13 H13H 103.8 . . ? C13 C14 H14G 109.5 . . ? C13 C14 H14H 109.5 . . ? C13 C14 H14I 109.5 . . ? H14G C14 H14H 109.5 . . ? H14G C14 H14I 109.5 . . ? H14H C14 H14I 109.5 . . ? C10 C11 H11E 109.3 . . ? C10 C11 H11F 109.3 . . ? H11E C11 H11F 108.0 . . ? C12 C11 C10 111.5(6) . . ? C12 C11 H11E 109.3 . . ? C12 C11 H11F 109.3 . . ? C13 C12 H12E 110.3 . . ? C13 C12 H12F 110.3 . . ? C11 C12 C13 107.0(6) . . ? C11 C12 H12E 110.3 . . ? C11 C12 H12F 110.3 . . ? H12E C12 H12F 108.6 . . ? C10 C11A H11G 110.2 . . ? C10 C11A H11H 110.2 . . ? H11G C11A H11H 108.5 . . ? C12A C11A C10 107.7(7) . . ? C12A C11A H11G 110.2 . . ? C12A C11A H11H 110.2 . . ? C13 C12A H12G 109.7 . . ? C13 C12A H12H 109.7 . . ? C11A C12A C13 110.0(7) . . ? C11A C12A H12G 109.7 . . ? C11A C12A H12H 109.7 . . ? H12G C12A H12H 108.2 . . ? C1B N1B H1B 118.6 . . ? C7B N1B H1B 118.6 . . ? C7B N1B C1B 122.8(4) . . ? C7B N2B H2B 115.9 . . ? C8B N2B H2B 115.9 . . ? C8B N2B C7B 128.2(4) . . ? C2B C1B N1B 120.2(4) . . ? C6B C1B N1B 118.7(4) . . ? C6B C1B C2B 121.1(4) . . ? C1B C2B H2BA 120.4 . . ? C1B C2B C3B 119.2(4) . . ? C3B C2B H2BA 120.4 . . ? C2B C3B H3B 119.7 . . ? C4B C3B C2B 120.5(5) . . ? C4B C3B H3B 119.7 . . ? C3B C4B H4B 119.9 . . ? C3B C4B C5B 120.1(5) . . ? C5B C4B H4B 119.9 . . ? C4B C5B H5B 119.9 . . ? C4B C5B C6B 120.1(5) . . ? C6B C5B H5B 119.9 . . ? C1B C6B C5B 118.9(5) . . ? C1B C6B H6B 120.6 . . ? C5B C6B H6B 120.6 . . ? N1B C7B S2 124.5(4) . . ? N1B C7B N2B 116.7(4) . . ? N2B C7B S2 118.8(3) . . ? O3B C8B N2B 122.2(4) . . ? O3B C8B C9B 123.3(4) . . ? N2B C8B C9B 114.5(4) . . ? C8B C9B H9BA 108.6 . . ? C8B C9B H9BB 108.6 . . ? C8B C9B H9BC 110.3 . . ? C8B C9B H9BD 110.3 . . ? C8B C9B C10B 114.5(5) . . ? C8B C9B C10C 106.9(5) . . ? H9BA C9B H9BB 107.6 . . ? H9BC C9B H9BD 108.6 . . ? C10B C9B H9BA 108.6 . . ? C10B C9B H9BB 108.6 . . ? C10C C9B H9BC 110.3 . . ? C10C C9B H9BD 110.3 . . ? C9B C10B H10A 109.5 . . ? C9B C10B H10B 109.5 . . ? C9B C10B C11B 110.7(4) . . ? H10A C10B H10B 108.1 . . ? C11B C10B H10A 109.5 . . ? C11B C10B H10B 109.5 . . ? C10B C11B H11A 110.6 . . ? C10B C11B H11B 110.6 . . ? C10B C11B C12B 105.7(4) . . ? H11A C11B H11B 108.7 . . ? C12B C11B H11A 110.6 . . ? C12B C11B H11B 110.6 . . ? C11B C12B H12A 109.8 . . ? C11B C12B H12B 109.8 . . ? H12A C12B H12B 108.2 . . ? C13B C12B C11B 109.5(5) . . ? C13B C12B H12A 109.8 . . ? C13B C12B H12B 109.8 . . ? C12B C13B H13A 109.9 . . ? C12B C13B H13B 109.9 . . ? C12B C13B C14B 108.7(5) . . ? H13A C13B H13B 108.3 . . ? C14B C13B H13A 109.9 . . ? C14B C13B H13B 109.9 . . ? C13B C14B H14A 109.5 . . ? C13B C14B H14B 109.5 . . ? C13B C14B H14C 109.5 . . ? H14A C14B H14B 109.5 . . ? H14A C14B H14C 109.5 . . ? H14B C14B H14C 109.5 . . ? C9B C10C H10C 110.8 . . ? C9B C10C H10D 110.8 . . ? H10C C10C H10D 108.9 . . ? C11C C10C C9B 104.7(9) . . ? C11C C10C H10C 110.8 . . ? C11C C10C H10D 110.8 . . ? C10C C11C H11C 110.9 . . ? C10C C11C H11D 110.9 . . ? C10C C11C C12C 104.2(9) . . ? H11C C11C H11D 108.9 . . ? C12C C11C H11C 110.9 . . ? C12C C11C H11D 110.9 . . ? C11C C12C H12C 111.4 . . ? C11C C12C H12D 111.4 . . ? H12C C12C H12D 109.2 . . ? C13C C12C C11C 102.0(9) . . ? C13C C12C H12C 111.4 . . ? C13C C12C H12D 111.4 . . ? C12C C13C H13C 109.1 . . ? C12C C13C H13D 109.1 . . ? C12C C13C C14C 112.6(11) . . ? H13C C13C H13D 107.8 . . ? C14C C13C H13C 109.1 . . ? C14C C13C H13D 109.1 . . ? C13C C14C H14D 109.5 . . ? C13C C14C H14E 109.5 . . ? C13C C14C H14F 109.5 . . ? H14D C14C H14E 109.5 . . ? H14D C14C H14F 109.5 . . ? H14E C14C H14F 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 S1 C7 1.679(5) . ? O1 C8 1.219(5) . ? N1 H1 0.8800 . ? N1 C1 1.435(6) . ? N1 C7 1.328(6) . ? N2 H2 0.8800 . ? N2 C7 1.383(6) . ? N2 C8 1.385(6) . ? C1 C2 1.380(7) . ? C1 C6 1.390(7) . ? C2 H2A 0.9500 . ? C2 C3 1.381(7) . ? C3 H3 0.9500 . ? C3 C4 1.381(8) . ? C4 H4 0.9500 . ? C4 C5 1.375(7) . ? C5 H5 0.9500 . ? C5 C6 1.389(7) . ? C6 H6 0.9500 . ? C8 C9 1.509(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.522(7) . ? C10 H10E 0.9900 . ? C10 H10F 0.9900 . ? C10 H10G 0.9900 . ? C10 H10H 0.9900 . ? C10 C11 1.568(6) . ? C10 C11A 1.550(7) . ? C13 H13E 0.9900 . ? C13 H13F 0.9900 . ? C13 H13G 0.9900 . ? C13 H13H 0.9900 . ? C13 C14 1.491(9) . ? C13 C12 1.549(7) . ? C13 C12A 1.566(8) . ? C14 H14G 0.9800 . ? C14 H14H 0.9800 . ? C14 H14I 0.9800 . ? C11 H11E 0.9900 . ? C11 H11F 0.9900 . ? C11 C12 1.539(7) . ? C12 H12E 0.9900 . ? C12 H12F 0.9900 . ? C11A H11G 0.9900 . ? C11A H11H 0.9900 . ? C11A C12A 1.546(8) . ? C12A H12G 0.9900 . ? C12A H12H 0.9900 . ? S2 C7B 1.674(5) . ? O3B C8B 1.221(6) . ? N1B H1B 0.8800 . ? N1B C1B 1.438(6) . ? N1B C7B 1.326(6) . ? N2B H2B 0.8800 . ? N2B C7B 1.393(6) . ? N2B C8B 1.383(6) . ? C1B C2B 1.382(7) . ? C1B C6B 1.379(7) . ? C2B H2BA 0.9500 . ? C2B C3B 1.382(7) . ? C3B H3B 0.9500 . ? C3B C4B 1.366(7) . ? C4B H4B 0.9500 . ? C4B C5B 1.386(7) . ? C5B H5B 0.9500 . ? C5B C6B 1.389(7) . ? C6B H6B 0.9500 . ? C8B C9B 1.497(7) . ? C9B H9BA 0.9900 . ? C9B H9BB 0.9900 . ? C9B H9BC 0.9900 . ? C9B H9BD 0.9900 . ? C9B C10B 1.522(5) . ? C9B C10C 1.727(14) . ? C10B H10A 0.9900 . ? C10B H10B 0.9900 . ? C10B C11B 1.538(5) . ? C11B H11A 0.9900 . ? C11B H11B 0.9900 . ? C11B C12B 1.563(5) . ? C12B H12A 0.9900 . ? C12B H12B 0.9900 . ? C12B C13B 1.520(5) . ? C13B H13A 0.9900 . ? C13B H13B 0.9900 . ? C13B C14B 1.539(5) . ? C14B H14A 0.9800 . ? C14B H14B 0.9800 . ? C14B H14C 0.9800 . ? C10C H10C 0.9900 . ? C10C H10D 0.9900 . ? C10C C11C 1.529(7) . ? C11C H11C 0.9900 . ? C11C H11D 0.9900 . ? C11C C12C 1.572(7) . ? C12C H12C 0.9900 . ? C12C H12D 0.9900 . ? C12C C13C 1.523(7) . ? C13C H13C 0.9900 . ? C13C H13D 0.9900 . ? C13C C14C 1.529(7) . ? C14C H14D 0.9800 . ? C14C H14E 0.9800 . ? C14C H14F 0.9800 . ? 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 N1 H1 O1 0.88 2.00 2.681(5) 133.4 . yes N1 H1 O3B 0.88 2.33 3.044(5) 137.9 . yes N2 H2 S2 0.88 2.52 3.397(4) 172.3 1_565 yes N1B H1B O1 0.88 2.34 3.009(5) 133.4 . yes N1B H1B O3B 0.88 1.98 2.660(5) 133.6 . yes N2B H2B S1 0.88 2.55 3.408(4) 166.8 1_545 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 O1 C8 C9 C10 28.7(7) . . . . ? N1 C1 C2 C3 178.8(5) . . . . ? N1 C1 C6 C5 -178.3(5) . . . . ? N2 C8 C9 C10 -151.9(4) . . . . ? C1 N1 C7 S1 -0.8(6) . . . . ? C1 N1 C7 N2 178.7(4) . . . . ? C1 C2 C3 C4 -1.3(9) . . . . ? C2 C1 C6 C5 -0.5(8) . . . . ? C2 C3 C4 C5 1.2(9) . . . . ? C3 C4 C5 C6 -0.8(9) . . . . ? C4 C5 C6 C1 0.4(8) . . . . ? C6 C1 C2 C3 1.0(8) . . . . ? C7 N1 C1 C2 65.5(6) . . . . ? C7 N1 C1 C6 -116.6(5) . . . . ? C7 N2 C8 O1 0.7(7) . . . . ? C7 N2 C8 C9 -178.7(4) . . . . ? C8 N2 C7 S1 -172.1(4) . . . . ? C8 N2 C7 N1 8.4(7) . . . . ? C8 C9 C10 C11 -163.1(5) . . . . ? C8 C9 C10 C11A 154.5(6) . . . . ? C9 C10 C11 C12 -64.4(8) . . . . ? C9 C10 C11A C12A 75.3(11) . . . . ? C10 C11 C12 C13 -173.4(6) . . . . ? C10 C11A C12A C13 -179.4(9) . . . . ? C14 C13 C12 C11 -177.9(6) . . . . ? C14 C13 C12A C11A 73.0(14) . . . . ? O3B C8B C9B C10B 13.4(7) . . . . ? O3B C8B C9B C10C 62.8(7) . . . . ? N1B C1B C2B C3B 177.7(4) . . . . ? N1B C1B C6B C5B -178.2(4) . . . . ? N2B C8B C9B C10B -166.9(5) . . . . ? N2B C8B C9B C10C -117.5(5) . . . . ? C1B N1B C7B S2 1.7(6) . . . . ? C1B N1B C7B N2B -178.8(4) . . . . ? C1B C2B C3B C4B -0.5(7) . . . . ? C2B C1B C6B C5B -1.8(7) . . . . ? C2B C3B C4B C5B 0.2(8) . . . . ? C3B C4B C5B C6B -0.7(8) . . . . ? C4B C5B C6B C1B 1.4(7) . . . . ? C6B C1B C2B C3B 1.3(7) . . . . ? C7B N1B C1B C2B 77.7(6) . . . . ? C7B N1B C1B C6B -105.9(5) . . . . ? C7B N2B C8B O3B 2.6(7) . . . . ? C7B N2B C8B C9B -177.1(4) . . . . ? C8B N2B C7B S2 171.6(4) . . . . ? C8B N2B C7B N1B -7.9(7) . . . . ? C8B C9B C10B C11B 80.5(9) . . . . ? C8B C9B C10C C11C -87.8(9) . . . . ? C9B C10B C11B C12B -163.8(10) . . . . ? C9B C10C C11C C12C -174.2(11) . . . . ? C10B C11B C12B C13B -169.9(12) . . . . ? C11B C12B C13B C14B 176.0(15) . . . . ? C10C C11C C12C C13C 179.1(12) . . . . ? C11C C12C C13C C14C 167.2(16) . . . . ?