Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. #TrackingRef 'CCDC770342-yamChemCom-3a.cif.txt' _journal_coden_Cambridge 0182 _publ_contact_author_name 'B. Schweizer' _publ_contact_author_address ; ; _publ_contact_author_email schweizer@org.chem.ethz.ch _publ_contact_author_phone ' ' _publ_contact_author_fax ' ' loop_ _publ_author_name _publ_author_address M.Yamada ;Laboratorium fur Organische Chemie, ETH Zurich 8093 Zurich, Switzerland ; W.B.Schweizer ;Laboratorium fur Organische Chemie, ETH Zurich 8093 Zurich, Switzerland ; F.Schoenebeck ;Laboratorium fur Organische Chemie, ETH Zurich 8093 Zurich, Switzerland ; F.Diederich ;Laboratorium fur Organische Chemie, ETH Zurich 8093 Zurich, Switzerland ; _audit_creation_method maXus _publ_section_title ; Unprecedented Thermal Rearrangement of Push-Pull-Chromophore--[60]Fullerene Conjugates: Formation of Chiral 1,2,9,12-Tetrakis-Adducts ; _publ_section_comment ; Structure contains three Chlorobenzene molecules, two disordered refined with constraints. Geometries are tabulated below. All diagrams and calculations were performed using maXus (Bruker Nonius, Delft & MacScience, Japan). ; _publ_section_synopsis ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; # CIF Copied by cif2cif, version 0.0.8 - beta ( 2 Apr 98) data_3a _database_code_depnum_ccdc_archive 'CCDC 770342' #TrackingRef 'CCDC770342-yamChemCom-3a.cif.txt' _publ_section_comment ; Structure contains 1.5 Cl-Bz solvent molecules. One of them refined with constrained geometry and two-fold disorder at a symmetry centre. No H-aatoms included for the disordered Chlorobenzene. ; _chemical_compound_source 'LOC ETH Zurich' _exptl_crystal_description plate _exptl_crystal_size_max .27 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .042 _exptl_crystal_F_000 2420.0 _exptl_crystal_colour brown _diffrn_ambient_temperature 123 _cell_measurement_temperature 123 _refine_ls_hydrogen_treatment mixed # Submission details _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 -0.05100 _diffrn_orient_matrix_UB_12 0.00105 _diffrn_orient_matrix_UB_13 0.03773 _diffrn_orient_matrix_UB_21 -0.01641 _diffrn_orient_matrix_UB_22 -0.04644 _diffrn_orient_matrix_UB_23 -0.02089 _diffrn_orient_matrix_UB_31 0.02279 _diffrn_orient_matrix_UB_32 -0.02903 _diffrn_orient_matrix_UB_33 0.04661 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1190.851 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z '-X,+Y+ 1/2,-Z+ 1/2' '+X,-Y+ 1/2,+Z+ 1/2' _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_cell_setting Monoclinic _chemical_formula_moiety 'C78 H15 N5 , 1.5 (C6 H5 Cl)' _chemical_formula_sum 'C87 H22.5 Cl1.5 N5 ' _chemical_name_systematic ; ? ; _cell_length_a 15.9413(3) _cell_length_b 18.6916(3) _cell_length_c 17.0131(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.6182(6) _cell_angle_gamma 90.00 _cell_volume 5012.1(2) _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_number 19793 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 5.91 _diffrn_reflns_theta_full 27.48 _cell_measurement_reflns_used 143610 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 27.485 _diffrn_measurement_method CCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97(Altomare et al., J. Appl. Cryst.,1999)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' Cl Cl 0.1484 0.1585 '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' _exptl_absorpt_coefficient_mu 0.170 _reflns_number_total 10912 _reflns_number_gt 8574 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Structure contains 1.5 Cl-Bz solvent molecules. One of them refined with constrained geometry and two-fold disorder at a symmetry centre. No H-aatoms included for the disordered Chlorobenzene. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10912 _refine_ls_number_parameters 902 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.2032 _refine_ls_wR_factor_gt 0.1874 _refine_ls_goodness_of_fit_ref 1.441 _refine_ls_restrained_S_all 1.441 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl89 Cl 0.65314(4) 0.33608(4) 0.32586(5) 0.0459(2) Uani 1 1 d . . . N64 N 0.50085(14) 0.62065(13) 0.26999(14) 0.0379(5) Uani 1 1 d . . . N66 N 0.48182(16) 0.81728(13) 0.37353(16) 0.0439(6) Uani 1 1 d . . . N70 N 0.13305(14) 0.70855(13) 0.55728(15) 0.0390(5) Uani 1 1 d . . . N77 N 0.38635(16) 0.99038(11) 0.54486(14) 0.0390(5) Uani 1 1 d . . . N90 N 0.02907(15) 0.68987(14) 0.36106(18) 0.0490(6) Uani 1 1 d . . . C1 C 0.29628(13) 0.59589(11) 0.36381(13) 0.0223(4) Uani 1 1 d . . . C2 C 0.21998(13) 0.59665(11) 0.41899(13) 0.0228(4) Uani 1 1 d . . . C3 C 0.25278(13) 0.54770(11) 0.48856(12) 0.0224(4) Uani 1 1 d . . . C4 C 0.20348(14) 0.50704(12) 0.53096(13) 0.0246(4) Uani 1 1 d . . . C5 C 0.23859(15) 0.44483(12) 0.57363(13) 0.0265(4) Uani 1 1 d . . . C6 C 0.17430(15) 0.38916(13) 0.56643(13) 0.0285(5) Uani 1 1 d . . . C7 C 0.19659(15) 0.31822(13) 0.55854(14) 0.0294(5) Uani 1 1 d . . . C8 C 0.28521(16) 0.29942(13) 0.55860(14) 0.0310(5) Uani 1 1 d . . . C9 C 0.28758(15) 0.24228(12) 0.50214(16) 0.0321(5) Uani 1 1 d . . . C10 C 0.20137(16) 0.22509(12) 0.46677(16) 0.0327(5) Uani 1 1 d . . . C11 C 0.18280(16) 0.20732(12) 0.38668(17) 0.0339(5) Uani 1 1 d . . . C12 C 0.25027(17) 0.20530(13) 0.33841(17) 0.0360(6) Uani 1 1 d . . . C13 C 0.21620(18) 0.23231(13) 0.26019(16) 0.0373(6) Uani 1 1 d . . . C14 C 0.26679(18) 0.27418(14) 0.21814(17) 0.0391(6) Uani 1 1 d . . . C15 C 0.23088(19) 0.33649(15) 0.17518(15) 0.0383(6) Uani 1 1 d . . . C16 C 0.29550(18) 0.39226(15) 0.18352(14) 0.0366(6) Uani 1 1 d . . . C17 C 0.27347(17) 0.46326(14) 0.19364(14) 0.0335(5) Uani 1 1 d . . . C18 C 0.32578(15) 0.51110(12) 0.24716(14) 0.0281(5) Uani 1 1 d . . . C19 C 0.27133(14) 0.57315(12) 0.27188(13) 0.0264(5) Uani 1 1 d . . . C20 C 0.18412(14) 0.53766(12) 0.25369(13) 0.0271(5) Uani 1 1 d . . . C21 C 0.12021(14) 0.54002(12) 0.29803(14) 0.0270(5) Uani 1 1 d . . . C22 C 0.12565(13) 0.57576(12) 0.37927(14) 0.0264(5) Uani 1 1 d . . . C23 C 0.08204(13) 0.51706(12) 0.42441(14) 0.0261(5) Uani 1 1 d . . . C24 C 0.11495(14) 0.49055(12) 0.49728(14) 0.0261(4) Uani 1 1 d . . . C25 C 0.09822(14) 0.41744(13) 0.51855(14) 0.0281(5) Uani 1 1 d . . . C26 C 0.04856(13) 0.37268(13) 0.46486(15) 0.0285(5) Uani 1 1 d . . . C27 C 0.07177(14) 0.29860(13) 0.45585(15) 0.0295(5) Uani 1 1 d . . . C28 C 0.14507(15) 0.27195(13) 0.50244(15) 0.0309(5) Uani 1 1 d . . . C29 C 0.05292(14) 0.28016(13) 0.37261(16) 0.0320(5) Uani 1 1 d . . . C30 C 0.10712(16) 0.23513(13) 0.33846(16) 0.0346(5) Uani 1 1 d . . . C31 C 0.12802(17) 0.25060(14) 0.26012(16) 0.0367(6) Uani 1 1 d . . . C32 C 0.09365(17) 0.31041(15) 0.21926(15) 0.0369(6) Uani 1 1 d . . . C33 C 0.14597(18) 0.35435(15) 0.17579(15) 0.0375(6) Uani 1 1 d . . . C34 C 0.12305(17) 0.42876(14) 0.18592(14) 0.0348(5) Uani 1 1 d . . . C35 C 0.18570(16) 0.48108(14) 0.19646(13) 0.0325(5) Uani 1 1 d . . . C36 C 0.39595(14) 0.48261(13) 0.29292(15) 0.0288(5) Uani 1 1 d . . . C37 C 0.41919(15) 0.40831(13) 0.28525(16) 0.0326(5) Uani 1 1 d . . . C38 C 0.37089(17) 0.36386(14) 0.23059(16) 0.0368(6) Uani 1 1 d . . . C39 C 0.35350(18) 0.29049(14) 0.25271(17) 0.0380(6) Uani 1 1 d . . . C40 C 0.38605(16) 0.26471(13) 0.32757(18) 0.0368(6) Uani 1 1 d . . . C41 C 0.43700(15) 0.31064(14) 0.38447(18) 0.0355(6) Uani 1 1 d . . . C42 C 0.41701(15) 0.29555(13) 0.46322(17) 0.0343(5) Uani 1 1 d . . . C43 C 0.35271(15) 0.23993(12) 0.45492(17) 0.0335(5) Uani 1 1 d . . . C44 C 0.33365(17) 0.22114(13) 0.37179(17) 0.0361(6) Uani 1 1 d . . . C45 C 0.41438(14) 0.35009(13) 0.51787(15) 0.0318(5) Uani 1 1 d . . . C46 C 0.34698(15) 0.35196(13) 0.56646(14) 0.0309(5) Uani 1 1 d . . . C47 C 0.32325(15) 0.42622(12) 0.57437(13) 0.0276(5) Uani 1 1 d . . . C48 C 0.37488(14) 0.46943(12) 0.53039(14) 0.0266(5) Uani 1 1 d . . . C49 C 0.33869(13) 0.52836(11) 0.48687(13) 0.0229(4) Uani 1 1 d . . . C50 C 0.36053(13) 0.54507(11) 0.41091(13) 0.0228(4) Uani 1 1 d . . . C51 C 0.41437(13) 0.50085(12) 0.37767(14) 0.0261(5) Uani 1 1 d . . . C52 C 0.44963(13) 0.43836(12) 0.42035(15) 0.0282(5) Uani 1 1 d . . . C53 C 0.45281(14) 0.38118(14) 0.36371(16) 0.0331(5) Uani 1 1 d . . . C54 C 0.43145(13) 0.42316(13) 0.49600(15) 0.0292(5) Uani 1 1 d . . . C55 C 0.01509(13) 0.40013(13) 0.38684(15) 0.0304(5) Uani 1 1 d . . . C56 C 0.01758(14) 0.34265(14) 0.32980(16) 0.0327(5) Uani 1 1 d . . . C57 C 0.03762(15) 0.35750(14) 0.25470(16) 0.0347(5) Uani 1 1 d . . . C58 C 0.05661(15) 0.43093(14) 0.23436(15) 0.0337(5) Uani 1 1 d . . . C59 C 0.05639(14) 0.48481(13) 0.29000(15) 0.0304(5) Uani 1 1 d . . . C60 C 0.03370(13) 0.47022(13) 0.36737(15) 0.0293(5) Uani 1 1 d . . . C61 C 0.33518(13) 0.67135(12) 0.37781(13) 0.0242(4) Uani 1 1 d . . . C62 C 0.40751(14) 0.69464(12) 0.35228(13) 0.0260(4) Uani 1 1 d . . . C63 C 0.45764(14) 0.65161(13) 0.30617(14) 0.0295(5) Uani 1 1 d . . . C65 C 0.44471(15) 0.76444(13) 0.36759(15) 0.0308(5) Uani 1 1 d . . . C67 C 0.28965(13) 0.71200(12) 0.43092(14) 0.0254(4) Uani 1 1 d . . . C68 C 0.22610(13) 0.67226(12) 0.45209(13) 0.0253(4) Uani 1 1 d . . . C69 C 0.17458(14) 0.69422(12) 0.51032(15) 0.0298(5) Uani 1 1 d . . . C71 C 0.31303(13) 0.78453(12) 0.46172(14) 0.0253(4) Uani 1 1 d . . . C72 C 0.27151(17) 0.84529(14) 0.42787(16) 0.0349(5) Uani 1 1 d . . . C73 C 0.29532(18) 0.91286(14) 0.45493(16) 0.0365(5) Uani 1 1 d . . . C74 C 0.36211(16) 0.92284(12) 0.51815(14) 0.0294(5) Uani 1 1 d . . . C75 C 0.40312(15) 0.86194(13) 0.55323(15) 0.0302(5) Uani 1 1 d . . . C76 C 0.37810(14) 0.79499(13) 0.52549(14) 0.0281(5) Uani 1 1 d . . . C78 C 0.46427(19) 1.00050(15) 0.59873(17) 0.0389(6) Uani 1 1 d . . . C79 C 0.3452(3) 1.05279(15) 0.50554(19) 0.0460(7) Uani 1 1 d . . . C80 C 0.26811(17) 0.63683(14) 0.21211(14) 0.0321(5) Uani 1 1 d . . . C81 C 0.20106(18) 0.69352(15) 0.22239(17) 0.0377(6) Uani 1 1 d . . . C82 C 0.07120(14) 0.64046(13) 0.36948(16) 0.0318(5) Uani 1 1 d . . . C83 C 0.69769(16) 0.40959(15) 0.28496(15) 0.0343(5) Uani 1 1 d . . . C84 C 0.78422(15) 0.40939(15) 0.28068(16) 0.0353(5) Uani 1 1 d . . . C85 C 0.81912(17) 0.46806(16) 0.24931(17) 0.0399(6) Uani 1 1 d . . . C86 C 0.76995(18) 0.52688(16) 0.22349(17) 0.0407(6) Uani 1 1 d . . . C87 C 0.68395(18) 0.52653(16) 0.22826(16) 0.0388(6) Uani 1 1 d . . . C88 C 0.64645(17) 0.46761(15) 0.25858(15) 0.0354(5) Uani 1 1 d . . . Cl90 Cl -0.0314(5) 0.3821(4) -0.0481(5) 0.1036(10) Uiso 0.218(3) 1 d PG . 1 C91 C -0.0419(17) 0.5612(9) 0.0849(15) 0.1036(10) Uiso 0.218(3) 1 d PG . 1 C92 C 0.0219(15) 0.6035(7) 0.0619(14) 0.1036(10) Uiso 0.218(3) 1 d PG . 1 C93 C 0.0694(15) 0.5786(8) 0.0055(15) 0.1036(10) Uiso 0.218(3) 1 d PG . 1 C94 C 0.0532(13) 0.5112(7) -0.0280(13) 0.1036(10) Uiso 0.218(3) 1 d PG . 1 C95 C -0.0105(7) 0.4688(5) -0.0050(7) 0.1036(10) Uiso 0.218(3) 1 d PG . 1 C96 C -0.0581(13) 0.4938(8) 0.0514(12) 0.1036(10) Uiso 0.218(3) 1 d PG . 1 Cl90a Cl 0.0089(4) 0.4102(3) -0.0933(4) 0.1036(10) Uiso 0.282(3) 1 d PG . 2 C91a C -0.0481(12) 0.5514(9) 0.0720(11) 0.1036(10) Uiso 0.282(3) 1 d PG . 2 C92a C 0.0120(11) 0.6049(6) 0.0695(10) 0.1036(10) Uiso 0.282(3) 1 d PG . 2 C93a C 0.0712(12) 0.5992(6) 0.0176(11) 0.1036(10) Uiso 0.282(3) 1 d PG . 2 C94a C 0.0703(9) 0.5400(6) -0.0319(10) 0.1036(10) Uiso 0.282(3) 1 d PG . 2 C95a C 0.0101(5) 0.4865(3) -0.0295(4) 0.1036(10) Uiso 0.282(3) 1 d PG . 2 C96a C -0.0490(10) 0.4922(7) 0.0225(10) 0.1036(10) Uiso 0.282(3) 1 d PG . 2 H86 H 0.7958 0.5686 0.2019 0.081(13) Uiso 1 1 calc R . . H78A H 0.456(2) 0.9791(18) 0.648(2) 0.040(8) Uiso 1 1 d . . . H75 H 0.450(2) 0.8665(18) 0.597(2) 0.043(8) Uiso 1 1 d . . . H80A H 0.2569(16) 0.6153(14) 0.1617(17) 0.019(6) Uiso 1 1 d . . . H76 H 0.403(2) 0.760(2) 0.552(2) 0.051(10) Uiso 1 1 d . . . H73 H 0.273(3) 0.954(3) 0.432(3) 0.067(12) Uiso 1 1 d . . . H80B H 0.320(2) 0.6623(17) 0.2128(19) 0.035(7) Uiso 1 1 d . . . H72 H 0.224(2) 0.8421(19) 0.382(2) 0.049(9) Uiso 1 1 d . . . H88 H 0.5866(19) 0.4675(15) 0.2613(18) 0.029(7) Uiso 1 1 d . . . H81A H 0.141(2) 0.6733(18) 0.216(2) 0.040(8) Uiso 1 1 d . . . H81B H 0.207(3) 0.725(2) 0.181(3) 0.061(11) Uiso 1 1 d . . . H87 H 0.652(2) 0.566(2) 0.212(2) 0.047(9) Uiso 1 1 d . . . H79A H 0.354(2) 1.0556(19) 0.448(2) 0.045(9) Uiso 1 1 d . . . H81C H 0.214(2) 0.7171(19) 0.273(2) 0.046(9) Uiso 1 1 d . . . H78B H 0.470(2) 1.050(2) 0.614(2) 0.052(9) Uiso 1 1 d . . . H79B H 0.279(3) 1.051(2) 0.503(3) 0.064(11) Uiso 1 1 d . . . H85 H 0.889(3) 0.462(2) 0.245(3) 0.061(10) Uiso 1 1 d . . . H79C H 0.372(3) 1.091(2) 0.532(3) 0.063(11) Uiso 1 1 d . . . H84 H 0.821(3) 0.368(2) 0.303(3) 0.067(11) Uiso 1 1 d . . . H78C H 0.518(3) 0.984(2) 0.575(2) 0.059(10) Uiso 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 Cl89 0.0363(3) 0.0446(4) 0.0588(4) 0.0052(3) 0.0140(3) -0.0031(3) N64 0.0359(11) 0.0406(12) 0.0394(12) -0.0057(9) 0.0126(9) -0.0071(9) N66 0.0472(13) 0.0375(12) 0.0511(14) -0.0073(10) 0.0212(11) -0.0143(10) N70 0.0313(10) 0.0430(13) 0.0449(13) -0.0119(10) 0.0122(9) -0.0028(9) N77 0.0560(13) 0.0218(10) 0.0383(12) -0.0015(8) 0.0041(10) -0.0040(9) N90 0.0392(12) 0.0402(13) 0.0638(17) 0.0034(11) -0.0046(11) 0.0121(10) C1 0.0228(9) 0.0214(10) 0.0235(10) 0.0005(8) 0.0058(8) -0.0026(8) C2 0.0213(9) 0.0221(10) 0.0251(10) -0.0013(8) 0.0044(8) -0.0001(8) C3 0.0260(10) 0.0203(10) 0.0205(10) -0.0040(7) 0.0027(8) -0.0009(8) C4 0.0281(10) 0.0250(11) 0.0216(10) -0.0047(8) 0.0065(8) 0.0000(8) C5 0.0344(11) 0.0264(11) 0.0189(10) -0.0006(8) 0.0049(8) -0.0031(9) C6 0.0339(11) 0.0313(12) 0.0221(10) 0.0006(9) 0.0101(8) -0.0042(9) C7 0.0349(11) 0.0283(11) 0.0267(11) 0.0057(9) 0.0100(9) -0.0062(9) C8 0.0362(12) 0.0269(11) 0.0294(12) 0.0094(9) 0.0035(9) 0.0001(9) C9 0.0352(12) 0.0206(11) 0.0408(13) 0.0070(9) 0.0070(10) 0.0004(9) C10 0.0366(12) 0.0214(11) 0.0410(14) 0.0061(9) 0.0087(10) -0.0044(9) C11 0.0389(12) 0.0187(10) 0.0459(14) -0.0043(10) 0.0123(11) -0.0068(9) C12 0.0443(13) 0.0201(11) 0.0460(15) -0.0086(10) 0.0151(11) -0.0026(10) C13 0.0484(14) 0.0259(12) 0.0398(14) -0.0158(10) 0.0139(11) -0.0076(10) C14 0.0499(14) 0.0315(13) 0.0387(14) -0.0171(10) 0.0162(11) -0.0065(11) C15 0.0564(16) 0.0361(14) 0.0245(12) -0.0121(10) 0.0131(11) -0.0097(12) C16 0.0508(14) 0.0387(14) 0.0239(11) -0.0081(10) 0.0177(10) -0.0073(11) C17 0.0476(14) 0.0376(13) 0.0174(10) -0.0012(9) 0.0115(9) -0.0089(11) C18 0.0354(11) 0.0271(11) 0.0244(11) -0.0014(8) 0.0132(9) -0.0072(9) C19 0.0290(10) 0.0287(11) 0.0217(10) 0.0019(8) 0.0047(8) -0.0036(8) C20 0.0308(11) 0.0269(11) 0.0223(10) 0.0047(8) -0.0002(8) -0.0028(8) C21 0.0246(10) 0.0280(11) 0.0265(11) 0.0036(8) -0.0022(8) 0.0011(8) C22 0.0211(9) 0.0249(11) 0.0327(12) 0.0004(9) 0.0028(8) 0.0011(8) C23 0.0197(9) 0.0238(11) 0.0364(12) -0.0016(9) 0.0093(8) 0.0007(8) C24 0.0247(10) 0.0269(11) 0.0292(11) -0.0048(9) 0.0122(8) 0.0005(8) C25 0.0277(10) 0.0303(12) 0.0293(11) 0.0000(9) 0.0139(9) -0.0010(9) C26 0.0203(9) 0.0302(12) 0.0373(12) 0.0013(9) 0.0120(9) -0.0050(8) C27 0.0255(10) 0.0262(11) 0.0390(13) 0.0007(9) 0.0123(9) -0.0078(8) C28 0.0345(11) 0.0240(11) 0.0361(13) 0.0050(9) 0.0111(10) -0.0053(9) C29 0.0262(10) 0.0278(12) 0.0419(14) -0.0016(10) 0.0051(9) -0.0121(9) C30 0.0375(12) 0.0240(11) 0.0426(14) -0.0076(10) 0.0074(10) -0.0139(9) C31 0.0433(13) 0.0277(12) 0.0388(13) -0.0135(10) 0.0057(11) -0.0135(10) C32 0.0390(13) 0.0390(14) 0.0309(12) -0.0110(10) -0.0009(10) -0.0141(11) C33 0.0517(15) 0.0369(14) 0.0231(11) -0.0115(10) 0.0025(10) -0.0132(11) C34 0.0416(13) 0.0389(13) 0.0208(11) -0.0016(9) -0.0054(9) -0.0078(10) C35 0.0420(13) 0.0357(13) 0.0187(10) 0.0014(9) 0.0013(9) -0.0073(10) C36 0.0281(10) 0.0282(11) 0.0336(12) -0.0023(9) 0.0163(9) -0.0047(9) C37 0.0309(11) 0.0301(12) 0.0413(13) -0.0045(10) 0.0207(10) -0.0002(9) C38 0.0423(13) 0.0335(13) 0.0411(14) -0.0097(10) 0.0275(11) -0.0009(10) C39 0.0440(13) 0.0303(13) 0.0450(15) -0.0142(11) 0.0241(11) -0.0022(10) C40 0.0366(12) 0.0251(12) 0.0528(16) -0.0075(10) 0.0207(11) 0.0052(10) C41 0.0246(10) 0.0287(12) 0.0557(16) -0.0023(11) 0.0141(10) 0.0060(9) C42 0.0246(10) 0.0278(12) 0.0503(15) 0.0057(10) 0.0052(10) 0.0058(9) C43 0.0334(12) 0.0200(11) 0.0471(14) 0.0042(10) 0.0062(10) 0.0071(9) C44 0.0408(13) 0.0196(11) 0.0510(16) -0.0024(10) 0.0168(11) 0.0050(9) C45 0.0227(10) 0.0305(12) 0.0394(13) 0.0067(10) -0.0046(9) 0.0025(9) C46 0.0329(11) 0.0286(12) 0.0286(12) 0.0076(9) -0.0035(9) 0.0017(9) C47 0.0320(11) 0.0285(11) 0.0207(10) 0.0013(8) -0.0009(8) -0.0013(9) C48 0.0247(10) 0.0272(11) 0.0257(11) -0.0009(8) -0.0033(8) -0.0030(8) C49 0.0220(9) 0.0220(10) 0.0238(10) -0.0023(8) 0.0003(8) -0.0042(7) C50 0.0195(9) 0.0205(10) 0.0280(11) -0.0022(8) 0.0022(8) -0.0039(7) C51 0.0206(9) 0.0242(11) 0.0345(12) -0.0019(9) 0.0074(8) -0.0050(8) C52 0.0162(9) 0.0278(11) 0.0409(13) -0.0018(9) 0.0048(8) -0.0006(8) C53 0.0216(10) 0.0319(12) 0.0490(14) -0.0031(10) 0.0161(10) 0.0007(9) C54 0.0180(9) 0.0292(12) 0.0380(12) 0.0034(9) -0.0036(8) -0.0006(8) C55 0.0186(9) 0.0338(12) 0.0391(13) -0.0007(10) 0.0050(9) -0.0059(8) C56 0.0227(10) 0.0344(13) 0.0401(13) -0.0027(10) 0.0015(9) -0.0110(9) C57 0.0282(11) 0.0372(13) 0.0355(13) -0.0053(10) -0.0054(9) -0.0107(10) C58 0.0297(11) 0.0390(13) 0.0289(12) 0.0011(10) -0.0071(9) -0.0076(10) C59 0.0216(10) 0.0320(12) 0.0347(12) 0.0040(9) -0.0055(9) -0.0012(9) C60 0.0165(9) 0.0321(12) 0.0386(13) 0.0002(9) 0.0015(8) -0.0001(8) C61 0.0260(10) 0.0221(10) 0.0240(10) 0.0017(8) 0.0023(8) -0.0024(8) C62 0.0271(10) 0.0240(11) 0.0266(11) 0.0004(8) 0.0038(8) -0.0030(8) C63 0.0286(11) 0.0306(12) 0.0299(11) -0.0017(9) 0.0065(9) -0.0087(9) C65 0.0313(11) 0.0315(13) 0.0318(12) -0.0002(9) 0.0118(9) -0.0043(9) C67 0.0246(10) 0.0231(11) 0.0281(11) -0.0001(8) 0.0027(8) 0.0006(8) C68 0.0254(10) 0.0240(11) 0.0264(11) 0.0001(8) 0.0034(8) 0.0005(8) C69 0.0267(10) 0.0244(11) 0.0384(13) -0.0051(9) 0.0050(9) -0.0020(8) C71 0.0258(10) 0.0215(10) 0.0298(11) -0.0014(8) 0.0076(8) -0.0013(8) C72 0.0379(12) 0.0298(12) 0.0350(13) -0.0004(10) -0.0013(10) 0.0005(10) C73 0.0463(14) 0.0230(12) 0.0380(13) 0.0028(10) -0.0008(11) 0.0046(10) C74 0.0392(12) 0.0219(11) 0.0297(12) -0.0029(9) 0.0132(9) -0.0041(9) C75 0.0296(11) 0.0313(12) 0.0295(12) -0.0005(9) 0.0038(9) -0.0027(9) C76 0.0274(10) 0.0261(11) 0.0301(11) 0.0036(9) 0.0024(9) -0.0008(9) C78 0.0525(16) 0.0302(13) 0.0360(14) -0.0085(11) 0.0130(12) -0.0148(11) C79 0.077(2) 0.0221(13) 0.0394(16) 0.0022(11) 0.0110(14) 0.0006(13) C80 0.0402(13) 0.0316(12) 0.0244(12) 0.0053(9) 0.0043(9) -0.0086(10) C81 0.0433(14) 0.0340(13) 0.0336(14) 0.0097(11) -0.0018(10) -0.0015(11) C82 0.0242(10) 0.0298(12) 0.0404(13) 0.0014(10) 0.0018(9) 0.0005(9) C83 0.0330(12) 0.0400(13) 0.0304(12) -0.0051(10) 0.0063(9) -0.0023(10) C84 0.0290(11) 0.0391(14) 0.0376(13) 0.0014(11) 0.0036(10) 0.0033(10) C85 0.0322(12) 0.0468(16) 0.0399(14) -0.0019(11) 0.0021(10) -0.0039(11) C86 0.0452(14) 0.0397(14) 0.0370(14) -0.0004(11) 0.0056(11) -0.0036(11) C87 0.0419(14) 0.0436(15) 0.0307(13) -0.0004(11) 0.0051(10) 0.0089(12) C88 0.0330(12) 0.0430(15) 0.0303(12) -0.0024(10) 0.0049(9) 0.0070(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cl89 C83 1.739(3) . ? N64 C63 1.147(3) . ? N66 C65 1.148(3) . ? N70 C69 1.143(3) . ? N77 C74 1.377(3) . ? N77 C78 1.441(4) . ? N77 C79 1.452(4) . ? N90 C82 1.138(3) . ? C1 C50 1.532(3) . ? C1 C61 1.545(3) . ? C1 C19 1.612(3) . ? C1 C2 1.644(3) . ? C2 C68 1.519(3) . ? C2 C3 1.525(3) . ? C2 C22 1.602(3) . ? C3 C4 1.373(3) . ? C3 C49 1.421(3) . ? C4 C5 1.439(3) . ? C4 C24 1.474(3) . ? C5 C47 1.392(3) . ? C5 C6 1.453(3) . ? C6 C7 1.384(3) . ? C6 C25 1.455(3) . ? C7 C28 1.449(3) . ? C7 C8 1.456(3) . ? C8 C46 1.383(3) . ? C8 C9 1.441(4) . ? C9 C43 1.405(4) . ? C9 C10 1.451(4) . ? C10 C11 1.391(4) . ? C10 C28 1.451(4) . ? C11 C12 1.448(4) . ? C11 C30 1.450(4) . ? C12 C44 1.397(4) . ? C12 C13 1.451(4) . ? C13 C14 1.396(4) . ? C13 C31 1.446(4) . ? C14 C15 1.447(4) . ? C14 C39 1.451(4) . ? C15 C33 1.396(4) . ? C15 C16 1.457(4) . ? C16 C17 1.390(4) . ? C16 C38 1.442(4) . ? C17 C35 1.446(4) . ? C17 C18 1.448(3) . ? C18 C36 1.371(4) . ? C18 C19 1.544(3) . ? C19 C20 1.530(3) . ? C19 C80 1.561(3) . ? C20 C21 1.356(3) . ? C20 C35 1.440(3) . ? C21 C59 1.441(3) . ? C21 C22 1.526(3) . ? C22 C82 1.483(3) . ? C22 C23 1.561(3) . ? C23 C24 1.365(3) . ? C23 C60 1.441(3) . ? C24 C25 1.449(3) . ? C25 C26 1.394(3) . ? C26 C27 1.447(3) . ? C26 C55 1.448(4) . ? C27 C28 1.401(4) . ? C27 C29 1.445(4) . ? C29 C30 1.394(4) . ? C29 C56 1.445(4) . ? C30 C31 1.451(4) . ? C31 C32 1.385(4) . ? C32 C57 1.448(4) . ? C32 C33 1.450(4) . ? C33 C34 1.455(4) . ? C34 C35 1.390(4) . ? C34 C58 1.437(4) . ? C36 C37 1.448(3) . ? C36 C51 1.468(3) . ? C37 C38 1.390(4) . ? C37 C53 1.453(4) . ? C38 C39 1.460(4) . ? C39 C40 1.388(4) . ? C40 C41 1.449(4) . ? C40 C44 1.454(4) . ? C41 C53 1.398(4) . ? C41 C42 1.451(4) . ? C42 C45 1.385(4) . ? C42 C43 1.452(3) . ? C43 C44 1.445(4) . ? C45 C46 1.451(4) . ? C45 C54 1.452(3) . ? C46 C47 1.450(3) . ? C47 C48 1.440(3) . ? C48 C49 1.402(3) . ? C48 C54 1.436(3) . ? C49 C50 1.423(3) . ? C50 C51 1.373(3) . ? C51 C52 1.444(3) . ? C52 C54 1.390(4) . ? C52 C53 1.445(3) . ? C55 C60 1.394(3) . ? C55 C56 1.452(4) . ? C56 C57 1.391(4) . ? C57 C58 1.458(4) . ? C58 C59 1.383(4) . ? C59 C60 1.442(4) . ? C61 C62 1.363(3) . ? C61 C67 1.455(3) . ? C62 C65 1.441(3) . ? C62 C63 1.445(3) . ? C67 C68 1.348(3) . ? C67 C71 1.481(3) . ? C68 C69 1.438(3) . ? C71 C72 1.395(3) . ? C71 C76 1.398(3) . ? C72 C73 1.378(4) . ? C73 C74 1.408(4) . ? C74 C75 1.401(4) . ? C75 C76 1.375(3) . ? C80 C81 1.534(4) . ? C83 C88 1.391(4) . ? C83 C84 1.392(3) . ? C84 C85 1.373(4) . ? C85 C86 1.383(4) . ? C86 C87 1.385(4) . ? C87 C88 1.389(4) . ? Cl90 C95 1.7900 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? Cl90a C95a 1.7900 . ? C91a C92a 1.3900 . ? C91a C96a 1.3900 . ? C92a C93a 1.3900 . ? C93a C94a 1.3900 . ? C94a C95a 1.3900 . ? C95a C96a 1.3900 . ? C72 H72 1.01(4) . ? C73 H73 0.91(5) . ? C75 H75 0.97(4) . ? C76 H76 0.85(4) . ? C78 H78A 0.95(4) . ? C78 H78B 0.96(4) . ? C78 H78C 1.04(4) . ? C79 H79A 1.00(4) . ? C79 H79B 1.05(4) . ? C79 H79C 0.91(5) . ? C80 H80A 0.94(3) . ? C80 H80B 0.96(3) . ? C81 H81A 1.02(3) . ? C81 H81B 0.94(5) . ? C81 H81C 0.96(4) . ? C84 H84 1.01(5) . ? C85 H85 1.12(4) . ? C86 H86 0.9800 . ? C87 H87 0.93(4) . ? C88 H88 0.96(3) . ? 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 C74 N77 C78 120.2(2) . . ? C74 N77 C79 120.0(2) . . ? C78 N77 C79 118.3(2) . . ? C50 C1 C61 105.31(16) . . ? C50 C1 C19 113.10(17) . . ? C61 C1 C19 115.17(17) . . ? C50 C1 C2 101.57(16) . . ? C61 C1 C2 102.61(16) . . ? C19 C1 C2 117.40(16) . . ? C68 C2 C3 105.95(17) . . ? C68 C2 C22 112.78(17) . . ? C3 C2 C22 111.85(17) . . ? C68 C2 C1 101.99(16) . . ? C3 C2 C1 103.95(16) . . ? C22 C2 C1 119.02(17) . . ? C4 C3 C49 119.9(2) . . ? C4 C3 C2 125.67(19) . . ? C49 C3 C2 110.88(18) . . ? C3 C4 C5 120.2(2) . . ? C3 C4 C24 120.1(2) . . ? C5 C4 C24 107.73(19) . . ? C47 C5 C4 120.6(2) . . ? C47 C5 C6 119.5(2) . . ? C4 C5 C6 108.7(2) . . ? C7 C6 C5 120.4(2) . . ? C7 C6 C25 119.9(2) . . ? C5 C6 C25 107.8(2) . . ? C6 C7 C28 120.5(2) . . ? C6 C7 C8 119.6(2) . . ? C28 C7 C8 108.1(2) . . ? C46 C8 C9 120.1(2) . . ? C46 C8 C7 120.4(2) . . ? C9 C8 C7 107.5(2) . . ? C43 C9 C8 120.0(2) . . ? C43 C9 C10 119.4(2) . . ? C8 C9 C10 108.8(2) . . ? C11 C10 C28 120.0(2) . . ? C11 C10 C9 120.6(2) . . ? C28 C10 C9 107.4(2) . . ? C10 C11 C12 119.7(2) . . ? C10 C11 C30 120.4(2) . . ? C12 C11 C30 108.3(2) . . ? C44 C12 C11 120.4(2) . . ? C44 C12 C13 120.1(2) . . ? C11 C12 C13 107.7(2) . . ? C14 C13 C31 120.2(3) . . ? C14 C13 C12 120.0(2) . . ? C31 C13 C12 108.3(2) . . ? C13 C14 C15 119.7(3) . . ? C13 C14 C39 119.9(3) . . ? C15 C14 C39 108.4(2) . . ? C33 C15 C14 120.0(2) . . ? C33 C15 C16 120.0(2) . . ? C14 C15 C16 107.8(3) . . ? C17 C16 C38 119.2(2) . . ? C17 C16 C15 120.5(2) . . ? C38 C16 C15 108.0(2) . . ? C16 C17 C35 119.2(2) . . ? C16 C17 C18 122.4(2) . . ? C35 C17 C18 107.8(2) . . ? C36 C18 C17 117.5(2) . . ? C36 C18 C19 125.5(2) . . ? C17 C18 C19 109.9(2) . . ? C20 C19 C18 98.64(18) . . ? C20 C19 C80 104.99(18) . . ? C18 C19 C80 111.11(18) . . ? C20 C19 C1 113.28(17) . . ? C18 C19 C1 113.28(18) . . ? C80 C19 C1 114.21(19) . . ? C21 C20 C35 119.4(2) . . ? C21 C20 C19 127.5(2) . . ? C35 C20 C19 110.4(2) . . ? C20 C21 C59 120.2(2) . . ? C20 C21 C22 124.9(2) . . ? C59 C21 C22 110.1(2) . . ? C82 C22 C21 107.60(19) . . ? C82 C22 C23 109.39(18) . . ? C21 C22 C23 99.71(18) . . ? C82 C22 C2 110.20(18) . . ? C21 C22 C2 114.28(18) . . ? C23 C22 C2 115.02(18) . . ? C24 C23 C60 119.0(2) . . ? C24 C23 C22 124.28(19) . . ? C60 C23 C22 109.2(2) . . ? C23 C24 C25 120.6(2) . . ? C23 C24 C4 119.50(19) . . ? C25 C24 C4 107.54(19) . . ? C26 C25 C24 120.7(2) . . ? C26 C25 C6 119.5(2) . . ? C24 C25 C6 108.27(19) . . ? C25 C26 C27 121.0(2) . . ? C25 C26 C55 118.9(2) . . ? C27 C26 C55 107.9(2) . . ? C28 C27 C29 120.2(2) . . ? C28 C27 C26 119.0(2) . . ? C29 C27 C26 108.2(2) . . ? C27 C28 C7 120.2(2) . . ? C27 C28 C10 119.6(2) . . ? C7 C28 C10 108.1(2) . . ? C30 C29 C27 120.1(2) . . ? C30 C29 C56 119.8(2) . . ? C27 C29 C56 108.0(2) . . ? C29 C30 C11 119.7(2) . . ? C29 C30 C31 120.3(2) . . ? C11 C30 C31 107.8(2) . . ? C32 C31 C13 120.2(2) . . ? C32 C31 C30 119.6(2) . . ? C13 C31 C30 108.0(2) . . ? C31 C32 C57 120.3(2) . . ? C31 C32 C33 119.9(2) . . ? C57 C32 C33 107.8(2) . . ? C15 C33 C32 120.1(3) . . ? C15 C33 C34 119.4(2) . . ? C32 C33 C34 107.9(2) . . ? C35 C34 C58 118.9(2) . . ? C35 C34 C33 120.0(2) . . ? C58 C34 C33 108.3(2) . . ? C34 C35 C20 121.3(2) . . ? C34 C35 C17 120.9(2) . . ? C20 C35 C17 107.9(2) . . ? C18 C36 C37 121.3(2) . . ? C18 C36 C51 119.6(2) . . ? C37 C36 C51 107.2(2) . . ? C38 C37 C36 120.7(2) . . ? C38 C37 C53 119.8(2) . . ? C36 C37 C53 108.4(2) . . ? C37 C38 C16 118.9(2) . . ? C37 C38 C39 119.8(3) . . ? C16 C38 C39 108.3(2) . . ? C40 C39 C14 120.1(2) . . ? C40 C39 C38 120.2(2) . . ? C14 C39 C38 107.4(3) . . ? C39 C40 C41 120.2(2) . . ? C39 C40 C44 120.3(2) . . ? C41 C40 C44 107.1(2) . . ? C53 C41 C40 119.6(3) . . ? C53 C41 C42 119.3(2) . . ? C40 C41 C42 108.9(2) . . ? C45 C42 C41 120.7(2) . . ? C45 C42 C43 120.0(2) . . ? C41 C42 C43 107.4(2) . . ? C9 C43 C44 120.1(2) . . ? C9 C43 C42 119.5(2) . . ? C44 C43 C42 108.1(2) . . ? C12 C44 C43 119.8(2) . . ? C12 C44 C40 119.6(3) . . ? C43 C44 C40 108.5(2) . . ? C42 C45 C46 120.0(2) . . ? C42 C45 C54 119.7(2) . . ? C46 C45 C54 107.9(2) . . ? C8 C46 C47 119.8(2) . . ? C8 C46 C45 120.3(2) . . ? C47 C46 C45 107.5(2) . . ? C5 C47 C48 118.9(2) . . ? C5 C47 C46 120.3(2) . . ? C48 C47 C46 108.1(2) . . ? C49 C48 C54 119.5(2) . . ? C49 C48 C47 119.5(2) . . ? C54 C48 C47 108.5(2) . . ? C48 C49 C3 120.7(2) . . ? C48 C49 C50 121.0(2) . . ? C3 C49 C50 109.29(18) . . ? C51 C50 C49 119.7(2) . . ? C51 C50 C1 124.6(2) . . ? C49 C50 C1 112.07(18) . . ? C50 C51 C52 120.0(2) . . ? C50 C51 C36 119.9(2) . . ? C52 C51 C36 108.2(2) . . ? C54 C52 C51 120.7(2) . . ? C54 C52 C53 119.9(2) . . ? C51 C52 C53 108.2(2) . . ? C41 C53 C52 120.2(2) . . ? C41 C53 C37 120.4(2) . . ? C52 C53 C37 108.0(2) . . ? C52 C54 C48 119.0(2) . . ? C52 C54 C45 120.2(2) . . ? C48 C54 C45 108.0(2) . . ? C60 C55 C26 119.2(2) . . ? C60 C55 C56 120.6(2) . . ? C26 C55 C56 107.9(2) . . ? C57 C56 C29 119.9(2) . . ? C57 C56 C55 120.0(2) . . ? C29 C56 C55 108.0(2) . . ? C56 C57 C32 120.1(2) . . ? C56 C57 C58 119.4(2) . . ? C32 C57 C58 108.1(2) . . ? C59 C58 C34 119.4(2) . . ? C59 C58 C57 120.1(2) . . ? C34 C58 C57 107.9(2) . . ? C58 C59 C21 120.8(2) . . ? C58 C59 C60 120.9(2) . . ? C21 C59 C60 108.6(2) . . ? C55 C60 C23 121.5(2) . . ? C55 C60 C59 119.1(2) . . ? C23 C60 C59 108.52(19) . . ? C62 C61 C67 123.7(2) . . ? C62 C61 C1 125.6(2) . . ? C67 C61 C1 110.28(17) . . ? C61 C62 C65 125.2(2) . . ? C61 C62 C63 123.9(2) . . ? C65 C62 C63 110.86(19) . . ? N64 C63 C62 176.0(2) . . ? N66 C65 C62 171.1(3) . . ? C68 C67 C61 110.05(19) . . ? C68 C67 C71 124.7(2) . . ? C61 C67 C71 125.13(19) . . ? C67 C68 C69 123.8(2) . . ? C67 C68 C2 115.00(19) . . ? C69 C68 C2 120.62(19) . . ? N70 C69 C68 177.0(3) . . ? C72 C71 C76 117.2(2) . . ? C72 C71 C67 121.4(2) . . ? C76 C71 C67 121.4(2) . . ? C73 C72 C71 121.2(2) . . ? C72 C73 C74 121.0(2) . . ? N77 C74 C75 121.0(2) . . ? N77 C74 C73 121.1(2) . . ? C75 C74 C73 118.0(2) . . ? C76 C75 C74 120.0(2) . . ? C75 C76 C71 122.5(2) . . ? C81 C80 C19 114.1(2) . . ? N90 C82 C22 179.2(3) . . ? C88 C83 C84 121.6(2) . . ? C88 C83 Cl89 119.3(2) . . ? C84 C83 Cl89 119.1(2) . . ? C85 C84 C83 118.7(3) . . ? C84 C85 C86 121.0(3) . . ? C85 C86 C87 119.8(3) . . ? C86 C87 C88 120.7(3) . . ? C87 C88 C83 118.3(2) . . ? C92 C91 C96 120.0 . . ? C91 C92 C93 120.0 . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C96 C95 C94 120.0 . . ? C96 C95 Cl90 120.0 . . ? C94 C95 Cl90 120.0 . . ? C95 C96 C91 120.0 . . ? C92a C91a C96a 120.0 . . ? C93a C92a C91a 120.0 . . ? C94a C93a C92a 120.0 . . ? C93a C94a C95a 120.0 . . ? C96a C95a C94a 120.0 . . ? C96a C95a Cl90a 120.0 . . ? C94a C95a Cl90a 120.0 . . ? C95a C96a C91a 120.0 . . ? C73 C72 H72 117(2) . . ? C71 C72 H72 122(2) . . ? C72 C73 H73 124(3) . . ? C74 C73 H73 115(3) . . ? C76 C75 H75 119(2) . . ? C74 C75 H75 121(2) . . ? C75 C76 H76 115(3) . . ? C71 C76 H76 122(3) . . ? N77 C78 H78A 106(2) . . ? N77 C78 H78B 110(2) . . ? H78A C78 H78B 101(3) . . ? N77 C78 H78C 113(2) . . ? H78A C78 H78C 116(3) . . ? H78B C78 H78C 110(3) . . ? N77 C79 H79A 112(2) . . ? N77 C79 H79B 112(2) . . ? H79A C79 H79B 104(3) . . ? N77 C79 H79C 105(3) . . ? H79A C79 H79C 108(3) . . ? H79B C79 H79C 116(4) . . ? C81 C80 H80A 111.1(15) . . ? C19 C80 H80A 104.5(16) . . ? C81 C80 H80B 106.0(18) . . ? C19 C80 H80B 115.2(19) . . ? H80A C80 H80B 106(2) . . ? C80 C81 H81A 112.9(19) . . ? C80 C81 H81B 101(2) . . ? H81A C81 H81B 110(3) . . ? C80 C81 H81C 111(2) . . ? H81A C81 H81C 110(3) . . ? H81B C81 H81C 111(3) . . ? C85 C84 H84 121(2) . . ? C83 C84 H84 120(2) . . ? C84 C85 H85 114(2) . . ? C86 C85 H85 125(2) . . ? C85 C86 H86 120.1 . . ? C87 C86 H86 120.1 . . ? C86 C87 H87 119(2) . . ? C88 C87 H87 120(2) . . ? C87 C88 H88 120.3(17) . . ? C83 C88 H88 121.4(18) . . ? 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 C50 C1 C2 C68 110.81(17) . . . . ? C61 C1 C2 C68 2.0(2) . . . . ? C19 C1 C2 C68 -125.33(19) . . . . ? C50 C1 C2 C3 0.8(2) . . . . ? C61 C1 C2 C3 -107.98(17) . . . . ? C19 C1 C2 C3 124.66(19) . . . . ? C50 C1 C2 C22 -124.40(19) . . . . ? C61 C1 C2 C22 126.82(19) . . . . ? C19 C1 C2 C22 -0.5(3) . . . . ? C68 C2 C3 C4 102.6(2) . . . . ? C22 C2 C3 C4 -20.7(3) . . . . ? C1 C2 C3 C4 -150.4(2) . . . . ? C68 C2 C3 C49 -98.83(19) . . . . ? C22 C2 C3 C49 137.91(18) . . . . ? C1 C2 C3 C49 8.3(2) . . . . ? C49 C3 C4 C5 -0.1(3) . . . . ? C2 C3 C4 C5 156.8(2) . . . . ? C49 C3 C4 C24 -138.1(2) . . . . ? C2 C3 C4 C24 18.7(3) . . . . ? C3 C4 C5 C47 1.8(3) . . . . ? C24 C4 C5 C47 144.4(2) . . . . ? C3 C4 C5 C6 -141.8(2) . . . . ? C24 C4 C5 C6 0.9(2) . . . . ? C47 C5 C6 C7 -1.5(3) . . . . ? C4 C5 C6 C7 142.6(2) . . . . ? C47 C5 C6 C25 -144.1(2) . . . . ? C4 C5 C6 C25 0.0(2) . . . . ? C5 C6 C7 C28 -137.7(2) . . . . ? C25 C6 C7 C28 0.5(3) . . . . ? C5 C6 C7 C8 0.9(3) . . . . ? C25 C6 C7 C8 139.0(2) . . . . ? C6 C7 C8 C46 0.0(3) . . . . ? C28 C7 C8 C46 143.1(2) . . . . ? C6 C7 C8 C9 -142.6(2) . . . . ? C28 C7 C8 C9 0.5(3) . . . . ? C46 C8 C9 C43 -0.1(4) . . . . ? C7 C8 C9 C43 142.7(2) . . . . ? C46 C8 C9 C10 -142.8(2) . . . . ? C7 C8 C9 C10 0.0(3) . . . . ? C43 C9 C10 C11 -0.8(3) . . . . ? C8 C9 C10 C11 142.1(2) . . . . ? C43 C9 C10 C28 -143.4(2) . . . . ? C8 C9 C10 C28 -0.4(3) . . . . ? C28 C10 C11 C12 138.6(2) . . . . ? C9 C10 C11 C12 0.6(3) . . . . ? C28 C10 C11 C30 -0.3(3) . . . . ? C9 C10 C11 C30 -138.2(2) . . . . ? C10 C11 C12 C44 -0.1(4) . . . . ? C30 C11 C12 C44 143.2(2) . . . . ? C10 C11 C12 C13 -143.0(2) . . . . ? C30 C11 C12 C13 0.3(3) . . . . ? C44 C12 C13 C14 0.0(3) . . . . ? C11 C12 C13 C14 143.1(2) . . . . ? C44 C12 C13 C31 -143.3(2) . . . . ? C11 C12 C13 C31 -0.3(3) . . . . ? C31 C13 C14 C15 0.7(4) . . . . ? C12 C13 C14 C15 -138.3(3) . . . . ? C31 C13 C14 C39 139.1(3) . . . . ? C12 C13 C14 C39 0.1(3) . . . . ? C13 C14 C15 C33 -0.1(4) . . . . ? C39 C14 C15 C33 -142.8(2) . . . . ? C13 C14 C15 C16 142.2(2) . . . . ? C39 C14 C15 C16 -0.4(3) . . . . ? C33 C15 C16 C17 1.2(4) . . . . ? C14 C15 C16 C17 -141.1(2) . . . . ? C33 C15 C16 C38 143.0(2) . . . . ? C14 C15 C16 C38 0.7(3) . . . . ? C38 C16 C17 C35 -137.1(2) . . . . ? C15 C16 C17 C35 0.5(4) . . . . ? C38 C16 C17 C18 3.1(3) . . . . ? C15 C16 C17 C18 140.7(2) . . . . ? C16 C17 C18 C36 -4.7(3) . . . . ? C35 C17 C18 C36 139.3(2) . . . . ? C16 C17 C18 C19 -157.0(2) . . . . ? C35 C17 C18 C19 -12.9(3) . . . . ? C36 C18 C19 C20 -128.3(2) . . . . ? C17 C18 C19 C20 21.2(2) . . . . ? C36 C18 C19 C80 121.9(2) . . . . ? C17 C18 C19 C80 -88.6(2) . . . . ? C36 C18 C19 C1 -8.3(3) . . . . ? C17 C18 C19 C1 141.24(19) . . . . ? C50 C1 C19 C20 103.6(2) . . . . ? C61 C1 C19 C20 -135.28(19) . . . . ? C2 C1 C19 C20 -14.3(3) . . . . ? C50 C1 C19 C18 -7.7(2) . . . . ? C61 C1 C19 C18 113.4(2) . . . . ? C2 C1 C19 C18 -125.55(19) . . . . ? C50 C1 C19 C80 -136.3(2) . . . . ? C61 C1 C19 C80 -15.1(3) . . . . ? C2 C1 C19 C80 105.9(2) . . . . ? C18 C19 C20 C21 138.2(2) . . . . ? C80 C19 C20 C21 -107.1(3) . . . . ? C1 C19 C20 C21 18.1(3) . . . . ? C18 C19 C20 C35 -22.7(2) . . . . ? C80 C19 C20 C35 92.0(2) . . . . ? C1 C19 C20 C35 -142.72(19) . . . . ? C35 C20 C21 C59 2.4(3) . . . . ? C19 C20 C21 C59 -157.0(2) . . . . ? C35 C20 C21 C22 155.2(2) . . . . ? C19 C20 C21 C22 -4.1(4) . . . . ? C20 C21 C22 C82 109.9(2) . . . . ? C59 C21 C22 C82 -94.9(2) . . . . ? C20 C21 C22 C23 -136.0(2) . . . . ? C59 C21 C22 C23 19.2(2) . . . . ? C20 C21 C22 C2 -12.8(3) . . . . ? C59 C21 C22 C2 142.39(19) . . . . ? C68 C2 C22 C82 11.9(3) . . . . ? C3 C2 C22 C82 131.3(2) . . . . ? C1 C2 C22 C82 -107.4(2) . . . . ? C68 C2 C22 C21 133.24(19) . . . . ? C3 C2 C22 C21 -107.4(2) . . . . ? C1 C2 C22 C21 13.9(3) . . . . ? C68 C2 C22 C23 -112.3(2) . . . . ? C3 C2 C22 C23 7.1(3) . . . . ? C1 C2 C22 C23 128.4(2) . . . . ? C82 C22 C23 C24 -116.7(2) . . . . ? C21 C22 C23 C24 130.7(2) . . . . ? C2 C22 C23 C24 8.0(3) . . . . ? C82 C22 C23 C60 94.2(2) . . . . ? C21 C22 C23 C60 -18.4(2) . . . . ? C2 C22 C23 C60 -141.14(19) . . . . ? C60 C23 C24 C25 -3.0(3) . . . . ? C22 C23 C24 C25 -149.3(2) . . . . ? C60 C23 C24 C4 134.6(2) . . . . ? C22 C23 C24 C4 -11.8(3) . . . . ? C3 C4 C24 C23 -1.2(3) . . . . ? C5 C4 C24 C23 -143.8(2) . . . . ? C3 C4 C24 C25 141.3(2) . . . . ? C5 C4 C24 C25 -1.4(2) . . . . ? C23 C24 C25 C26 0.3(3) . . . . ? C4 C24 C25 C26 -141.6(2) . . . . ? C23 C24 C25 C6 143.3(2) . . . . ? C4 C24 C25 C6 1.4(2) . . . . ? C7 C6 C25 C26 -0.2(3) . . . . ? C5 C6 C25 C26 142.6(2) . . . . ? C7 C6 C25 C24 -143.7(2) . . . . ? C5 C6 C25 C24 -0.9(2) . . . . ? C24 C25 C26 C27 138.7(2) . . . . ? C6 C25 C26 C27 -0.2(3) . . . . ? C24 C25 C26 C55 1.0(3) . . . . ? C6 C25 C26 C55 -137.9(2) . . . . ? C25 C26 C27 C28 0.4(3) . . . . ? C55 C26 C27 C28 142.1(2) . . . . ? C25 C26 C27 C29 -141.6(2) . . . . ? C55 C26 C27 C29 0.1(2) . . . . ? C29 C27 C28 C7 137.3(2) . . . . ? C26 C27 C28 C7 -0.1(3) . . . . ? C29 C27 C28 C10 -0.7(3) . . . . ? C26 C27 C28 C10 -138.2(2) . . . . ? C6 C7 C28 C27 -0.3(3) . . . . ? C8 C7 C28 C27 -143.1(2) . . . . ? C6 C7 C28 C10 142.0(2) . . . . ? C8 C7 C28 C10 -0.8(3) . . . . ? C11 C10 C28 C27 0.5(3) . . . . ? C9 C10 C28 C27 143.3(2) . . . . ? C11 C10 C28 C7 -142.1(2) . . . . ? C9 C10 C28 C7 0.8(3) . . . . ? C28 C27 C29 C30 0.7(3) . . . . ? C26 C27 C29 C30 142.2(2) . . . . ? C28 C27 C29 C56 -141.8(2) . . . . ? C26 C27 C29 C56 -0.3(2) . . . . ? C27 C29 C30 C11 -0.5(3) . . . . ? C56 C29 C30 C11 137.6(2) . . . . ? C27 C29 C30 C31 -138.3(2) . . . . ? C56 C29 C30 C31 -0.2(3) . . . . ? C10 C11 C30 C29 0.3(3) . . . . ? C12 C11 C30 C29 -142.7(2) . . . . ? C10 C11 C30 C31 142.8(2) . . . . ? C12 C11 C30 C31 -0.2(3) . . . . ? C14 C13 C31 C32 -1.0(4) . . . . ? C12 C13 C31 C32 142.3(2) . . . . ? C14 C13 C31 C30 -143.1(2) . . . . ? C12 C13 C31 C30 0.1(3) . . . . ? C29 C30 C31 C32 -0.1(3) . . . . ? C11 C30 C31 C32 -142.3(2) . . . . ? C29 C30 C31 C13 142.3(2) . . . . ? C11 C30 C31 C13 0.0(3) . . . . ? C13 C31 C32 C57 -137.4(2) . . . . ? C30 C31 C32 C57 0.4(3) . . . . ? C13 C31 C32 C33 0.6(4) . . . . ? C30 C31 C32 C33 138.5(2) . . . . ? C14 C15 C33 C32 -0.2(3) . . . . ? C16 C15 C33 C32 -138.0(3) . . . . ? C14 C15 C33 C34 137.0(3) . . . . ? C16 C15 C33 C34 -0.9(4) . . . . ? C31 C32 C33 C15 -0.1(3) . . . . ? C57 C32 C33 C15 142.6(2) . . . . ? C31 C32 C33 C34 -141.6(2) . . . . ? C57 C32 C33 C34 1.1(3) . . . . ? C15 C33 C34 C35 -1.3(4) . . . . ? C32 C33 C34 C35 140.5(2) . . . . ? C15 C33 C34 C58 -142.5(2) . . . . ? C32 C33 C34 C58 -0.6(3) . . . . ? C58 C34 C35 C20 -1.1(4) . . . . ? C33 C34 C35 C20 -138.3(2) . . . . ? C58 C34 C35 C17 140.2(2) . . . . ? C33 C34 C35 C17 3.1(3) . . . . ? C21 C20 C35 C34 -0.1(3) . . . . ? C19 C20 C35 C34 162.5(2) . . . . ? C21 C20 C35 C17 -145.9(2) . . . . ? C19 C20 C35 C17 16.7(3) . . . . ? C16 C17 C35 C34 -2.7(3) . . . . ? C18 C17 C35 C34 -148.1(2) . . . . ? C16 C17 C35 C20 143.2(2) . . . . ? C18 C17 C35 C20 -2.2(3) . . . . ? C17 C18 C36 C37 2.9(3) . . . . ? C19 C18 C36 C37 150.4(2) . . . . ? C17 C18 C36 C51 -134.9(2) . . . . ? C19 C18 C36 C51 12.5(3) . . . . ? C18 C36 C37 C38 0.4(3) . . . . ? C51 C36 C37 C38 142.8(2) . . . . ? C18 C36 C37 C53 -143.3(2) . . . . ? C51 C36 C37 C53 -0.9(2) . . . . ? C36 C37 C38 C16 -2.1(3) . . . . ? C53 C37 C38 C16 137.5(2) . . . . ? C36 C37 C38 C39 -139.0(2) . . . . ? C53 C37 C38 C39 0.7(3) . . . . ? C17 C16 C38 C37 0.4(3) . . . . ? C15 C16 C38 C37 -142.0(2) . . . . ? C17 C16 C38 C39 141.7(2) . . . . ? C15 C16 C38 C39 -0.7(3) . . . . ? C13 C14 C39 C40 -0.2(4) . . . . ? C15 C14 C39 C40 142.4(2) . . . . ? C13 C14 C39 C38 -142.6(2) . . . . ? C15 C14 C39 C38 0.0(3) . . . . ? C37 C38 C39 C40 -1.0(3) . . . . ? C16 C38 C39 C40 -141.9(2) . . . . ? C37 C38 C39 C14 141.3(2) . . . . ? C16 C38 C39 C14 0.4(3) . . . . ? C14 C39 C40 C41 -137.1(2) . . . . ? C38 C39 C40 C41 0.5(3) . . . . ? C14 C39 C40 C44 0.1(3) . . . . ? C38 C39 C40 C44 137.7(2) . . . . ? C39 C40 C41 C53 0.3(3) . . . . ? C44 C40 C41 C53 -141.8(2) . . . . ? C39 C40 C41 C42 142.5(2) . . . . ? C44 C40 C41 C42 0.4(3) . . . . ? C53 C41 C42 C45 -0.7(3) . . . . ? C40 C41 C42 C45 -143.0(2) . . . . ? C53 C41 C42 C43 142.0(2) . . . . ? C40 C41 C42 C43 -0.3(3) . . . . ? C8 C9 C43 C44 -138.3(2) . . . . ? C10 C9 C43 C44 0.5(3) . . . . ? C8 C9 C43 C42 -0.3(4) . . . . ? C10 C9 C43 C42 138.5(2) . . . . ? C45 C42 C43 C9 0.6(4) . . . . ? C41 C42 C43 C9 -142.4(2) . . . . ? C45 C42 C43 C44 143.0(2) . . . . ? C41 C42 C43 C44 0.1(3) . . . . ? C11 C12 C44 C43 -0.2(4) . . . . ? C13 C12 C44 C43 138.1(2) . . . . ? C11 C12 C44 C40 -138.5(2) . . . . ? C13 C12 C44 C40 -0.1(3) . . . . ? C9 C43 C44 C12 0.0(3) . . . . ? C42 C43 C44 C12 -142.2(2) . . . . ? C9 C43 C44 C40 142.4(2) . . . . ? C42 C43 C44 C40 0.2(3) . . . . ? C39 C40 C44 C12 0.1(3) . . . . ? C41 C40 C44 C12 142.1(2) . . . . ? C39 C40 C44 C43 -142.4(2) . . . . ? C41 C40 C44 C43 -0.3(3) . . . . ? C41 C42 C45 C46 137.7(2) . . . . ? C43 C42 C45 C46 -0.4(3) . . . . ? C41 C42 C45 C54 0.3(3) . . . . ? C43 C42 C45 C54 -137.8(2) . . . . ? C9 C8 C46 C47 137.7(2) . . . . ? C7 C8 C46 C47 -0.3(3) . . . . ? C9 C8 C46 C45 0.2(3) . . . . ? C7 C8 C46 C45 -137.8(2) . . . . ? C42 C45 C46 C8 0.1(3) . . . . ? C54 C45 C46 C8 141.9(2) . . . . ? C42 C45 C46 C47 -142.0(2) . . . . ? C54 C45 C46 C47 -0.2(3) . . . . ? C4 C5 C47 C48 -1.2(3) . . . . ? C6 C5 C47 C48 138.5(2) . . . . ? C4 C5 C47 C46 -138.5(2) . . . . ? C6 C5 C47 C46 1.2(3) . . . . ? C8 C46 C47 C5 -0.4(3) . . . . ? C45 C46 C47 C5 142.0(2) . . . . ? C8 C46 C47 C48 -141.7(2) . . . . ? C45 C46 C47 C48 0.6(2) . . . . ? C5 C47 C48 C49 -1.1(3) . . . . ? C46 C47 C48 C49 140.9(2) . . . . ? C5 C47 C48 C54 -142.8(2) . . . . ? C46 C47 C48 C54 -0.8(2) . . . . ? C54 C48 C49 C3 140.4(2) . . . . ? C47 C48 C49 C3 2.8(3) . . . . ? C54 C48 C49 C50 -3.2(3) . . . . ? C47 C48 C49 C50 -140.8(2) . . . . ? C4 C3 C49 C48 -2.3(3) . . . . ? C2 C3 C49 C48 -162.26(19) . . . . ? C4 C3 C49 C50 145.1(2) . . . . ? C2 C3 C49 C50 -14.9(2) . . . . ? C48 C49 C50 C51 3.5(3) . . . . ? C3 C49 C50 C51 -143.8(2) . . . . ? C48 C49 C50 C1 162.96(19) . . . . ? C3 C49 C50 C1 15.7(2) . . . . ? C61 C1 C50 C51 -104.7(2) . . . . ? C19 C1 C50 C51 21.9(3) . . . . ? C2 C1 C50 C51 148.6(2) . . . . ? C61 C1 C50 C49 96.97(19) . . . . ? C19 C1 C50 C49 -136.44(18) . . . . ? C2 C1 C50 C49 -9.7(2) . . . . ? C49 C50 C51 C52 -1.0(3) . . . . ? C1 C50 C51 C52 -157.8(2) . . . . ? C49 C50 C51 C36 137.4(2) . . . . ? C1 C50 C51 C36 -19.4(3) . . . . ? C18 C36 C51 C50 1.3(3) . . . . ? C37 C36 C51 C50 -141.9(2) . . . . ? C18 C36 C51 C52 144.0(2) . . . . ? C37 C36 C51 C52 0.9(2) . . . . ? C50 C51 C52 C54 -1.6(3) . . . . ? C36 C51 C52 C54 -144.4(2) . . . . ? C50 C51 C52 C53 142.2(2) . . . . ? C36 C51 C52 C53 -0.5(2) . . . . ? C40 C41 C53 C52 138.6(2) . . . . ? C42 C41 C53 C52 0.3(3) . . . . ? C40 C41 C53 C37 -0.6(3) . . . . ? C42 C41 C53 C37 -138.9(2) . . . . ? C54 C52 C53 C41 0.5(3) . . . . ? C51 C52 C53 C41 -143.7(2) . . . . ? C54 C52 C53 C37 144.1(2) . . . . ? C51 C52 C53 C37 -0.1(2) . . . . ? C38 C37 C53 C41 0.1(3) . . . . ? C36 C37 C53 C41 144.2(2) . . . . ? C38 C37 C53 C52 -143.5(2) . . . . ? C36 C37 C53 C52 0.6(2) . . . . ? C51 C52 C54 C48 1.8(3) . . . . ? C53 C52 C54 C48 -137.9(2) . . . . ? C51 C52 C54 C45 138.8(2) . . . . ? C53 C52 C54 C45 -0.9(3) . . . . ? C49 C48 C54 C52 0.6(3) . . . . ? C47 C48 C54 C52 142.3(2) . . . . ? C49 C48 C54 C45 -141.1(2) . . . . ? C47 C48 C54 C45 0.7(2) . . . . ? C42 C45 C54 C52 0.5(3) . . . . ? C46 C45 C54 C52 -141.4(2) . . . . ? C42 C45 C54 C48 141.7(2) . . . . ? C46 C45 C54 C48 -0.3(3) . . . . ? C25 C26 C55 C60 0.3(3) . . . . ? C27 C26 C55 C60 -142.3(2) . . . . ? C25 C26 C55 C56 142.8(2) . . . . ? C27 C26 C55 C56 0.1(2) . . . . ? C30 C29 C56 C57 0.2(3) . . . . ? C27 C29 C56 C57 142.7(2) . . . . ? C30 C29 C56 C55 -142.2(2) . . . . ? C27 C29 C56 C55 0.4(2) . . . . ? C60 C55 C56 C57 -0.8(3) . . . . ? C26 C55 C56 C57 -142.7(2) . . . . ? C60 C55 C56 C29 141.5(2) . . . . ? C26 C55 C56 C29 -0.3(2) . . . . ? C29 C56 C57 C32 0.1(3) . . . . ? C55 C56 C57 C32 138.1(2) . . . . ? C29 C56 C57 C58 -137.5(2) . . . . ? C55 C56 C57 C58 0.5(3) . . . . ? C31 C32 C57 C56 -0.4(3) . . . . ? C33 C32 C57 C56 -142.9(2) . . . . ? C31 C32 C57 C58 141.4(2) . . . . ? C33 C32 C57 C58 -1.1(3) . . . . ? C35 C34 C58 C59 0.1(4) . . . . ? C33 C34 C58 C59 141.8(2) . . . . ? C35 C34 C58 C57 -141.7(2) . . . . ? C33 C34 C58 C57 -0.1(3) . . . . ? C56 C57 C58 C59 1.4(4) . . . . ? C32 C57 C58 C59 -140.8(2) . . . . ? C56 C57 C58 C34 142.9(2) . . . . ? C32 C57 C58 C34 0.7(3) . . . . ? C34 C58 C59 C21 2.1(4) . . . . ? C57 C58 C59 C21 139.3(2) . . . . ? C34 C58 C59 C60 -140.1(2) . . . . ? C57 C58 C59 C60 -2.9(3) . . . . ? C20 C21 C59 C58 -3.4(3) . . . . ? C22 C21 C59 C58 -160.0(2) . . . . ? C20 C21 C59 C60 142.9(2) . . . . ? C22 C21 C59 C60 -13.7(3) . . . . ? C26 C55 C60 C23 -3.0(3) . . . . ? C56 C55 C60 C23 -140.7(2) . . . . ? C26 C55 C60 C59 137.0(2) . . . . ? C56 C55 C60 C59 -0.7(3) . . . . ? C24 C23 C60 C55 4.4(3) . . . . ? C22 C23 C60 C55 155.4(2) . . . . ? C24 C23 C60 C59 -139.3(2) . . . . ? C22 C23 C60 C59 11.7(2) . . . . ? C58 C59 C60 C55 2.5(3) . . . . ? C21 C59 C60 C55 -143.7(2) . . . . ? C58 C59 C60 C23 147.3(2) . . . . ? C21 C59 C60 C23 1.0(3) . . . . ? C50 C1 C61 C62 65.9(3) . . . . ? C19 C1 C61 C62 -59.4(3) . . . . ? C2 C1 C61 C62 171.8(2) . . . . ? C50 C1 C61 C67 -106.97(19) . . . . ? C19 C1 C61 C67 127.72(19) . . . . ? C2 C1 C61 C67 -1.0(2) . . . . ? C67 C61 C62 C65 -6.1(4) . . . . ? C1 C61 C62 C65 -178.1(2) . . . . ? C67 C61 C62 C63 173.5(2) . . . . ? C1 C61 C62 C63 1.5(4) . . . . ? C61 C62 C63 N64 -174(4) . . . . ? C65 C62 C63 N64 5(4) . . . . ? C61 C62 C65 N66 -175.5(17) . . . . ? C63 C62 C65 N66 4.9(19) . . . . ? C62 C61 C67 C68 -173.6(2) . . . . ? C1 C61 C67 C68 -0.5(3) . . . . ? C62 C61 C67 C71 2.6(4) . . . . ? C1 C61 C67 C71 175.6(2) . . . . ? C61 C67 C68 C69 173.5(2) . . . . ? C71 C67 C68 C69 -2.7(4) . . . . ? C61 C67 C68 C2 2.1(3) . . . . ? C71 C67 C68 C2 -174.1(2) . . . . ? C3 C2 C68 C67 105.8(2) . . . . ? C22 C2 C68 C67 -131.5(2) . . . . ? C1 C2 C68 C67 -2.7(2) . . . . ? C3 C2 C68 C69 -65.8(2) . . . . ? C22 C2 C68 C69 56.8(3) . . . . ? C1 C2 C68 C69 -174.3(2) . . . . ? C67 C68 C69 N70 -153(5) . . . . ? C2 C68 C69 N70 18(5) . . . . ? C68 C67 C71 C72 -84.6(3) . . . . ? C61 C67 C71 C72 99.8(3) . . . . ? C68 C67 C71 C76 96.0(3) . . . . ? C61 C67 C71 C76 -79.6(3) . . . . ? C76 C71 C72 C73 1.7(4) . . . . ? C67 C71 C72 C73 -177.8(2) . . . . ? C71 C72 C73 C74 -0.4(4) . . . . ? C78 N77 C74 C75 11.9(4) . . . . ? C79 N77 C74 C75 177.6(2) . . . . ? C78 N77 C74 C73 -168.2(2) . . . . ? C79 N77 C74 C73 -2.6(4) . . . . ? C72 C73 C74 N77 179.5(3) . . . . ? C72 C73 C74 C75 -0.6(4) . . . . ? N77 C74 C75 C76 -179.8(2) . . . . ? C73 C74 C75 C76 0.3(3) . . . . ? C74 C75 C76 C71 1.0(4) . . . . ? C72 C71 C76 C75 -2.0(4) . . . . ? C67 C71 C76 C75 177.5(2) . . . . ? C20 C19 C80 C81 62.2(3) . . . . ? C18 C19 C80 C81 167.9(2) . . . . ? C1 C19 C80 C81 -62.4(3) . . . . ? C88 C83 C84 C85 -0.2(4) . . . . ? Cl89 C83 C84 C85 -179.1(2) . . . . ? C83 C84 C85 C86 1.0(4) . . . . ? C84 C85 C86 C87 -0.8(4) . . . . ? C85 C86 C87 C88 -0.1(4) . . . . ? C86 C87 C88 C83 0.9(4) . . . . ? C84 C83 C88 C87 -0.7(4) . . . . ? Cl89 C83 C88 C87 178.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.038 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.061 _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # Attachment 'CCDC770343-yamChemCom-2a.cif.txt' # CIF Copied by cif2cif, version 0.0.8 - beta ( 2 Apr 98) # CIF Copied by cif2cif, version 0.0.8 - beta ( 2 Apr 98) data_2a _database_code_depnum_ccdc_archive 'CCDC 770343' #TrackingRef 'CCDC770343-yamChemCom-2a.cif.txt' _publ_section_comment ; Two disordered CS2 refined over two positions with restraints. ; _chemical_compound_source 'LOC ETH Zurich' _exptl_crystal_description Cube _exptl_crystal_size_max .57 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .012 _exptl_crystal_F_000 1264.0 _exptl_crystal_colour 'dark brown' _diffrn_ambient_temperature 123 _cell_measurement_temperature 123 _refine_ls_hydrogen_treatment constr # Submission details _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 -0.07604 _diffrn_orient_matrix_UB_12 0.02529 _diffrn_orient_matrix_UB_13 0.00339 _diffrn_orient_matrix_UB_21 0.01616 _diffrn_orient_matrix_UB_22 -0.01331 _diffrn_orient_matrix_UB_23 0.07552 _diffrn_orient_matrix_UB_31 0.02972 _diffrn_orient_matrix_UB_32 0.05753 _diffrn_orient_matrix_UB_33 -0.01211 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1250.430 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting Triclinic _chemical_formula_moiety 'C78 H15 N5 , 3( C S2 ) ' _chemical_formula_sum 'C81 H15 N5 S6 ' _chemical_name_systematic ; ? ; _cell_length_a 13.0651(3) _cell_length_b 13.5710(3) _cell_length_c 15.9971(5) _cell_angle_alpha 74.0161(11) _cell_angle_beta 77.3303(12) _cell_angle_gamma 75.1841(12) _cell_volume 2602.02(12) _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_number 19258 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_full 27.46 _cell_measurement_reflns_used 62527 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 27.485 _diffrn_measurement_method CCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97(Altomare et al., J. Appl. Cryst.,1999)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 0.325 _reflns_number_total 11674 _reflns_number_gt 8566 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Two disordered CS2 refined over two positions with restraints ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11674 _refine_ls_number_parameters 893 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2294 _refine_ls_wR_factor_gt 0.2109 _refine_ls_goodness_of_fit_ref 1.509 _refine_ls_restrained_S_all 1.514 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S73 S 0.64304(11) 0.11046(14) 0.33401(13) 0.1011(5) Uani 1 1 d . . . S84 S 0.48414(14) 0.13170(12) 0.51015(10) 0.0654(5) Uani 0.715(3) 1 d P . . S86 S 0.68055(8) 0.18641(10) 0.06888(8) 0.0675(3) Uani 1 1 d . . . S88 S 0.63023(18) 0.41797(11) 0.07135(14) 0.1335(9) Uani 1 1 d . . . S94 S 0.0930(3) 0.2958(4) 0.7593(2) 0.0770(15) Uani 0.285(3) 1 d PD A 1 C95 C 0.1861(12) 0.3521(12) 0.7436(9) 0.092(8) Uani 0.285(3) 1 d PD A 1 S96 S 0.2722(16) 0.4104(17) 0.7396(16) 0.36(2) Uani 0.285(3) 1 d PD A 1 S92 S 0.34675(18) 0.1615(3) 0.73125(13) 0.1020(9) Uani 0.715(3) 1 d PD A 2 C91 C 0.3063(5) 0.2828(5) 0.7336(4) 0.093(3) Uani 0.715(3) 1 d PD A 2 S93 S 0.2758(2) 0.4017(2) 0.74021(14) 0.0828(7) Uani 0.715(3) 1 d PD A 2 C851 C 0.6588(13) 0.0252(16) 0.2844(15) 0.087(5) Uani 0.285(3) 1 d P A 1 S841 S 0.6828(4) -0.0756(5) 0.2454(4) 0.0882(17) Uani 0.285(3) 1 d P A 1 N73 N 0.1109(2) 0.70337(19) 0.39018(18) 0.0414(6) Uani 1 1 d . . . N75 N -0.0955(2) 0.4927(2) 0.42196(18) 0.0421(6) Uani 1 1 d . . . N78 N 0.4600(3) 0.6669(3) 0.1617(2) 0.0581(8) Uani 1 1 d . . . N80 N 0.1383(2) 0.6762(2) 0.12723(18) 0.0441(6) Uani 1 1 d . . . N81 N 0.6083(2) 0.3382(2) 0.50406(17) 0.0417(6) Uani 1 1 d . . . C1 C 0.1733(2) 0.36721(19) 0.29689(16) 0.0262(5) Uani 1 1 d . . . C2 C 0.1626(2) 0.26728(19) 0.38034(16) 0.0272(5) Uani 1 1 d . . . C3 C 0.0629(2) 0.2227(2) 0.38660(16) 0.0295(5) Uani 1 1 d . . . C4 C -0.0212(2) 0.2718(2) 0.34157(17) 0.0302(5) Uani 1 1 d . . . C5 C -0.0837(2) 0.2105(2) 0.31992(19) 0.0336(6) Uani 1 1 d . . . C6 C -0.0601(2) 0.1017(2) 0.34550(19) 0.0349(6) Uani 1 1 d . . . C7 C 0.0288(2) 0.0502(2) 0.39185(18) 0.0342(6) Uani 1 1 d . . . C8 C 0.0896(2) 0.1106(2) 0.41026(17) 0.0309(6) Uani 1 1 d . . . C9 C 0.2055(2) 0.0772(2) 0.39976(17) 0.0300(5) Uani 1 1 d . . . C10 C 0.0826(2) 0.39830(19) 0.24137(17) 0.0285(5) Uani 1 1 d . . . C11 C 0.1262(2) 0.42609(19) 0.14908(17) 0.0309(6) Uani 1 1 d . . . C12 C 0.2411(2) 0.3931(2) 0.13912(17) 0.0306(6) Uani 1 1 d . . . C13 C 0.2709(2) 0.3451(2) 0.22465(17) 0.0285(5) Uani 1 1 d . . . C14 C 0.3535(2) 0.2584(2) 0.23432(18) 0.0298(5) Uani 1 1 d . . . C15 C 0.4111(2) 0.2190(2) 0.15874(19) 0.0338(6) Uani 1 1 d . . . C16 C 0.3855(2) 0.2681(2) 0.07490(19) 0.0345(6) Uani 1 1 d . . . C17 C 0.2987(2) 0.3567(2) 0.06490(18) 0.0341(6) Uani 1 1 d . . . C18 C 0.2415(3) 0.3514(2) -0.00184(18) 0.0372(6) Uani 1 1 d . . . C19 C 0.2944(2) 0.2574(2) -0.03204(17) 0.0369(6) Uani 1 1 d . . . C20 C 0.3840(2) 0.2055(2) 0.01484(18) 0.0368(6) Uani 1 1 d . . . C21 C 0.4086(2) 0.0964(2) 0.04107(19) 0.0376(6) Uani 1 1 d . . . C22 C 0.3454(2) 0.0354(2) 0.02023(19) 0.0372(6) Uani 1 1 d . . . C23 C 0.2598(3) 0.0851(2) -0.02494(18) 0.0382(6) Uani 1 1 d . . . C24 C 0.2334(3) 0.1985(2) -0.05179(18) 0.0389(7) Uani 1 1 d . . . C25 C 0.1177(3) 0.2319(2) -0.04174(18) 0.0387(6) Uani 1 1 d . . . C26 C 0.2400(2) -0.0900(2) 0.1198(2) 0.0370(6) Uani 1 1 d . . . C27 C 0.1604(2) 0.0480(2) 0.00177(19) 0.0380(6) Uani 1 1 d . . . C28 C 0.1504(2) -0.0378(2) 0.0726(2) 0.0378(6) Uani 1 1 d . . . C29 C 0.0525(2) -0.0368(2) 0.1362(2) 0.0371(6) Uani 1 1 d . . . C30 C -0.0316(2) 0.0508(2) 0.1263(2) 0.0377(6) Uani 1 1 d . . . C31 C -0.0215(2) 0.1399(2) 0.0526(2) 0.0380(6) Uani 1 1 d . . . C32 C -0.0737(2) 0.2346(2) 0.0830(2) 0.0383(6) Uani 1 1 d . . . C33 C -0.1161(2) 0.2032(2) 0.1761(2) 0.0375(6) Uani 1 1 d . . . C34 C -0.0900(2) 0.0892(2) 0.2028(2) 0.0371(6) Uani 1 1 d . . . C35 C -0.0628(2) 0.0399(2) 0.2862(2) 0.0366(6) Uani 1 1 d . . . C36 C 0.0243(2) -0.0509(2) 0.2962(2) 0.0362(6) Uani 1 1 d . . . C37 C 0.0816(2) -0.0884(2) 0.2223(2) 0.0360(6) Uani 1 1 d . . . C38 C 0.1968(2) -0.1211(2) 0.2119(2) 0.0364(6) Uani 1 1 d . . . C39 C 0.0725(3) 0.1389(2) -0.00902(19) 0.0394(7) Uani 1 1 d . . . C40 C 0.3355(2) -0.0544(2) 0.0949(2) 0.0376(6) Uani 1 1 d . . . C41 C 0.3921(2) -0.0478(2) 0.1602(2) 0.0371(6) Uani 1 1 d . . . C42 C 0.3519(2) -0.0783(2) 0.2494(2) 0.0356(6) Uani 1 1 d . . . C43 C 0.2515(2) -0.1148(2) 0.2758(2) 0.0360(6) Uani 1 1 d . . . C44 C 0.1916(2) -0.0762(2) 0.35255(18) 0.0347(6) Uani 1 1 d . . . C45 C 0.0818(2) -0.0444(2) 0.36166(18) 0.0351(6) Uani 1 1 d . . . C46 C 0.2560(2) -0.0150(2) 0.37230(18) 0.0333(6) Uani 1 1 d . . . C47 C 0.3532(2) -0.0161(2) 0.30941(19) 0.0345(6) Uani 1 1 d . . . C48 C 0.3956(2) 0.0741(2) 0.27802(19) 0.0332(6) Uani 1 1 d . . . C49 C 0.3429(2) 0.1680(2) 0.30960(18) 0.0308(5) Uani 1 1 d . . . C50 C 0.2503(2) 0.1691(2) 0.36937(17) 0.0283(5) Uani 1 1 d . . . C51 C -0.0107(2) 0.3621(2) 0.26636(18) 0.0300(5) Uani 1 1 d . . . C52 C -0.0673(2) 0.3555(2) 0.20047(19) 0.0331(6) Uani 1 1 d . . . C53 C -0.1124(2) 0.2621(2) 0.2334(2) 0.0353(6) Uani 1 1 d . . . C54 C -0.0276(2) 0.3854(2) 0.11076(19) 0.0350(6) Uani 1 1 d . . . C55 C 0.0709(2) 0.4219(2) 0.08523(18) 0.0342(6) Uani 1 1 d . . . C56 C 0.1312(3) 0.3839(2) 0.00794(17) 0.0360(6) Uani 1 1 d . . . C57 C 0.0675(3) 0.3225(2) -0.01268(18) 0.0377(6) Uani 1 1 d . . . C58 C -0.0307(2) 0.3236(2) 0.05144(19) 0.0373(6) Uani 1 1 d . . . C59 C 0.4368(2) 0.0456(2) 0.1274(2) 0.0369(6) Uani 1 1 d . . . C60 C 0.4378(2) 0.1053(2) 0.18531(19) 0.0338(6) Uani 1 1 d . . . C61 C 0.1651(2) 0.2923(2) 0.46950(17) 0.0341(6) Uani 1 1 d . . . C62 C 0.1594(3) 0.2007(2) 0.55058(19) 0.0400(7) Uani 1 1 d . . . C63 C 0.1784(2) 0.46935(19) 0.32114(16) 0.0271(5) Uani 1 1 d . . . C64 C 0.2822(2) 0.5069(2) 0.29157(17) 0.0280(5) Uani 1 1 d . . . C65 C 0.3667(2) 0.4583(2) 0.34543(17) 0.0294(5) Uani 1 1 d . . . C66 C 0.3422(2) 0.4463(2) 0.43782(18) 0.0318(6) Uani 1 1 d . . . C67 C 0.4214(2) 0.4076(2) 0.48975(18) 0.0342(6) Uani 1 1 d . . . C68 C 0.5301(2) 0.3767(2) 0.45252(19) 0.0357(6) Uani 1 1 d . . . C69 C 0.5539(2) 0.3881(2) 0.36003(19) 0.0368(6) Uani 1 1 d . . . C70 C 0.4741(2) 0.4283(2) 0.30817(18) 0.0339(6) Uani 1 1 d . . . C71 C 0.0936(2) 0.5313(2) 0.36034(17) 0.0294(5) Uani 1 1 d . . . C72 C 0.1047(2) 0.6275(2) 0.37572(18) 0.0322(6) Uani 1 1 d . . . C74 C -0.0116(2) 0.5069(2) 0.39249(18) 0.0325(6) Uani 1 1 d . . . C76 C 0.2923(2) 0.5852(2) 0.21713(18) 0.0320(6) Uani 1 1 d . . . C77 C 0.3874(2) 0.6293(2) 0.1872(2) 0.0403(7) Uani 1 1 d . . . C79 C 0.2067(2) 0.6340(2) 0.16632(18) 0.0353(6) Uani 1 1 d . . . C82 C 0.7187(2) 0.3044(3) 0.4654(2) 0.0479(8) Uani 1 1 d . . . C83 C 0.5811(3) 0.3218(3) 0.5992(2) 0.0455(7) Uani 1 1 d . . . C85 C 0.5674(4) 0.1186(4) 0.4226(4) 0.0507(12) Uani 0.715(3) 1 d P A . C87 C 0.6545(3) 0.3019(4) 0.0696(3) 0.0633(11) Uani 1 1 d . . . H61A H 0.2380 0.3191 0.4634 0.040(8) Uiso 1 1 calc R . . H61B H 0.0986 0.3560 0.4805 0.046(9) Uiso 1 1 calc R . . H62A H 0.0888 0.1705 0.5559 0.045(9) Uiso 1 1 calc R . . H62B H 0.1553 0.2277 0.6090 0.060(11) Uiso 1 1 calc R . . H62C H 0.2300 0.1395 0.5439 0.065(12) Uiso 1 1 calc R . . H66 H 0.2675 0.4658 0.4654 0.031(8) Uiso 1 1 calc R . . H67 H 0.4023 0.4014 0.5535 0.032(8) Uiso 1 1 calc R . . H69 H 0.6282 0.3670 0.3323 0.053(10) Uiso 1 1 calc R . . H70 H 0.4929 0.4361 0.2443 0.026(7) Uiso 1 1 calc R . . H82A H 0.7255 0.2374 0.4391 0.064(12) Uiso 1 1 calc R . . H82B H 0.7695 0.2832 0.5153 0.075(13) Uiso 1 1 calc R . . H82C H 0.7435 0.3674 0.4130 0.086(15) Uiso 1 1 calc R . . H83A H 0.5348 0.3939 0.6160 0.067(12) Uiso 1 1 calc R . . H83B H 0.6538 0.2978 0.6277 0.061(11) Uiso 1 1 calc R . . H83C H 0.5346 0.2615 0.6246 0.081(14) Uiso 1 1 calc R . . 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 S73 0.0654(7) 0.1136(12) 0.1374(13) -0.0596(10) 0.0156(8) -0.0356(8) S84 0.0821(11) 0.0545(8) 0.0673(9) -0.0153(6) -0.0238(7) -0.0164(7) S86 0.0395(5) 0.0841(8) 0.0915(7) -0.0475(6) 0.0038(5) -0.0175(5) S88 0.1607(17) 0.0589(8) 0.1367(14) -0.0200(8) 0.0771(14) -0.0342(9) S94 0.065(2) 0.103(3) 0.053(2) -0.002(2) -0.0172(17) -0.011(2) C95 0.18(2) 0.045(8) 0.052(8) -0.013(6) -0.075(12) 0.020(11) S96 0.30(3) 0.41(4) 0.193(17) 0.04(2) -0.096(16) 0.16(3) S92 0.0828(13) 0.165(3) 0.0602(10) -0.0424(13) -0.0006(9) -0.0211(15) C91 0.055(3) 0.159(8) 0.040(3) -0.004(4) -0.001(2) -0.002(4) S93 0.0785(14) 0.0945(16) 0.0498(9) 0.0105(10) -0.0012(10) -0.0104(13) C851 0.056(9) 0.090(13) 0.124(15) -0.040(11) -0.003(9) -0.024(9) S841 0.080(3) 0.090(4) 0.091(3) -0.034(3) -0.029(2) 0.015(3) N73 0.0440(14) 0.0294(12) 0.0536(15) -0.0125(11) -0.0079(12) -0.0095(11) N75 0.0374(14) 0.0425(14) 0.0495(14) -0.0211(12) 0.0018(11) -0.0101(11) N78 0.0481(16) 0.0546(18) 0.0671(19) 0.0038(15) -0.0052(14) -0.0256(15) N80 0.0537(16) 0.0336(13) 0.0466(14) -0.0009(11) -0.0175(13) -0.0132(12) N81 0.0341(13) 0.0471(15) 0.0419(13) -0.0133(11) -0.0123(10) 0.0035(11) C1 0.0272(12) 0.0205(11) 0.0312(12) -0.0061(9) -0.0033(10) -0.0064(9) C2 0.0286(12) 0.0225(12) 0.0296(11) -0.0058(9) -0.0027(10) -0.0057(10) C3 0.0293(13) 0.0280(13) 0.0290(12) -0.0078(10) 0.0030(10) -0.0074(10) C4 0.0258(12) 0.0281(13) 0.0341(12) -0.0103(10) 0.0018(10) -0.0034(10) C5 0.0215(12) 0.0361(14) 0.0405(14) -0.0114(11) 0.0027(10) -0.0052(11) C6 0.0272(13) 0.0373(15) 0.0405(14) -0.0102(12) 0.0047(11) -0.0145(11) C7 0.0359(14) 0.0283(13) 0.0361(13) -0.0046(11) 0.0048(11) -0.0148(11) C8 0.0327(13) 0.0283(13) 0.0274(11) -0.0033(10) 0.0005(10) -0.0068(11) C9 0.0335(13) 0.0240(12) 0.0297(12) -0.0008(10) -0.0072(10) -0.0053(10) C10 0.0323(13) 0.0190(11) 0.0335(12) -0.0070(9) -0.0073(10) -0.0017(10) C11 0.0398(14) 0.0173(11) 0.0330(12) -0.0034(9) -0.0055(11) -0.0040(10) C12 0.0365(14) 0.0228(12) 0.0321(12) -0.0028(10) -0.0029(11) -0.0115(11) C13 0.0294(13) 0.0240(12) 0.0324(12) -0.0071(10) 0.0011(10) -0.0104(10) C14 0.0241(12) 0.0304(13) 0.0372(13) -0.0088(11) -0.0029(10) -0.0101(10) C15 0.0246(12) 0.0333(14) 0.0433(14) -0.0106(12) 0.0016(11) -0.0100(11) C16 0.0308(13) 0.0343(14) 0.0378(13) -0.0091(11) 0.0044(11) -0.0136(11) C17 0.0391(15) 0.0296(13) 0.0317(12) -0.0029(11) 0.0039(11) -0.0162(12) C18 0.0478(16) 0.0328(14) 0.0285(12) -0.0010(11) -0.0012(12) -0.0147(13) C19 0.0453(16) 0.0366(15) 0.0273(12) -0.0068(11) 0.0027(12) -0.0138(13) C20 0.0353(14) 0.0383(15) 0.0348(13) -0.0111(12) 0.0083(11) -0.0130(12) C21 0.0294(13) 0.0407(15) 0.0412(14) -0.0193(12) 0.0082(11) -0.0061(12) C22 0.0354(14) 0.0346(14) 0.0394(14) -0.0179(12) 0.0057(12) -0.0031(12) C23 0.0470(16) 0.0360(15) 0.0326(13) -0.0163(12) 0.0012(12) -0.0076(13) C24 0.0482(17) 0.0395(15) 0.0275(12) -0.0089(11) -0.0016(12) -0.0094(13) C25 0.0477(17) 0.0386(15) 0.0327(13) -0.0081(12) -0.0119(12) -0.0095(13) C26 0.0433(16) 0.0223(13) 0.0460(15) -0.0139(11) -0.0049(13) -0.0034(11) C27 0.0415(16) 0.0390(15) 0.0390(14) -0.0195(12) -0.0068(12) -0.0068(13) C28 0.0426(16) 0.0321(14) 0.0458(15) -0.0207(12) -0.0088(13) -0.0066(12) C29 0.0410(15) 0.0297(14) 0.0474(15) -0.0143(12) -0.0079(13) -0.0126(12) C30 0.0339(14) 0.0405(15) 0.0471(15) -0.0180(13) -0.0095(12) -0.0114(12) C31 0.0379(15) 0.0375(15) 0.0462(15) -0.0141(13) -0.0174(12) -0.0075(12) C32 0.0344(14) 0.0355(15) 0.0474(16) -0.0118(12) -0.0166(12) -0.0008(12) C33 0.0236(12) 0.0390(16) 0.0528(16) -0.0138(13) -0.0085(12) -0.0061(11) C34 0.0284(13) 0.0382(15) 0.0499(16) -0.0144(13) -0.0052(12) -0.0122(12) C35 0.0275(13) 0.0350(14) 0.0481(15) -0.0103(12) 0.0031(12) -0.0151(11) C36 0.0381(15) 0.0267(13) 0.0455(15) -0.0066(11) -0.0010(12) -0.0160(12) C37 0.0392(15) 0.0260(13) 0.0460(15) -0.0084(11) -0.0057(12) -0.0135(12) C38 0.0415(15) 0.0194(12) 0.0480(15) -0.0091(11) -0.0052(13) -0.0058(11) C39 0.0492(17) 0.0385(16) 0.0366(14) -0.0122(12) -0.0139(13) -0.0098(13) C40 0.0318(14) 0.0302(14) 0.0491(16) -0.0185(12) 0.0013(12) -0.0003(11) C41 0.0269(13) 0.0319(14) 0.0499(16) -0.0172(12) -0.0012(12) 0.0028(11) C42 0.0311(14) 0.0220(12) 0.0493(16) -0.0075(11) -0.0073(12) 0.0021(10) C43 0.0408(15) 0.0198(12) 0.0433(14) -0.0032(11) -0.0091(12) -0.0016(11) C44 0.0437(15) 0.0198(12) 0.0376(13) 0.0003(10) -0.0078(12) -0.0076(11) C45 0.0416(15) 0.0237(12) 0.0369(13) -0.0012(11) -0.0007(12) -0.0129(11) C46 0.0385(15) 0.0221(12) 0.0366(13) -0.0003(10) -0.0111(11) -0.0043(11) C47 0.0315(13) 0.0238(13) 0.0446(14) -0.0045(11) -0.0125(12) 0.0026(10) C48 0.0258(12) 0.0302(13) 0.0443(14) -0.0104(11) -0.0100(11) -0.0014(10) C49 0.0271(12) 0.0267(13) 0.0390(13) -0.0072(11) -0.0095(11) -0.0033(10) C50 0.0303(13) 0.0225(12) 0.0317(12) -0.0024(10) -0.0110(10) -0.0038(10) C51 0.0254(12) 0.0251(12) 0.0370(13) -0.0112(10) -0.0036(10) 0.0020(10) C52 0.0254(12) 0.0284(13) 0.0444(14) -0.0113(11) -0.0094(11) 0.0024(10) C53 0.0219(12) 0.0354(15) 0.0486(15) -0.0145(12) -0.0045(11) -0.0019(11) C54 0.0346(14) 0.0249(13) 0.0433(14) -0.0080(11) -0.0142(12) 0.0045(11) C55 0.0446(16) 0.0204(12) 0.0341(13) -0.0018(10) -0.0127(12) 0.0002(11) C56 0.0501(17) 0.0256(13) 0.0300(12) 0.0000(10) -0.0101(12) -0.0077(12) C57 0.0457(16) 0.0331(14) 0.0332(13) -0.0035(11) -0.0146(12) -0.0034(12) C58 0.0396(15) 0.0317(14) 0.0408(14) -0.0060(12) -0.0189(12) 0.0002(12) C59 0.0243(12) 0.0350(14) 0.0481(15) -0.0151(12) 0.0011(11) -0.0005(11) C60 0.0219(12) 0.0318(14) 0.0453(15) -0.0113(12) -0.0019(11) -0.0020(10) C61 0.0429(15) 0.0314(14) 0.0296(12) -0.0073(11) -0.0055(11) -0.0106(12) C62 0.0504(17) 0.0349(15) 0.0318(13) -0.0053(11) -0.0042(12) -0.0083(13) C63 0.0311(13) 0.0227(11) 0.0283(11) -0.0046(9) -0.0076(10) -0.0061(10) C64 0.0266(12) 0.0251(12) 0.0351(12) -0.0103(10) -0.0048(10) -0.0069(10) C65 0.0283(13) 0.0267(12) 0.0338(12) -0.0070(10) -0.0051(10) -0.0068(10) C66 0.0275(13) 0.0299(13) 0.0347(13) -0.0081(11) -0.0015(10) -0.0026(10) C67 0.0335(14) 0.0333(14) 0.0335(13) -0.0082(11) -0.0063(11) -0.0016(11) C68 0.0300(13) 0.0343(14) 0.0415(14) -0.0109(12) -0.0071(11) -0.0010(11) C69 0.0276(13) 0.0390(15) 0.0417(14) -0.0131(12) -0.0027(11) -0.0020(11) C70 0.0323(14) 0.0311(14) 0.0368(13) -0.0105(11) -0.0008(11) -0.0048(11) C71 0.0309(13) 0.0248(12) 0.0330(12) -0.0067(10) -0.0045(10) -0.0069(10) C72 0.0322(13) 0.0258(13) 0.0368(13) -0.0048(11) -0.0065(11) -0.0048(11) C74 0.0341(14) 0.0271(13) 0.0366(13) -0.0135(11) -0.0007(11) -0.0043(11) C76 0.0319(13) 0.0279(13) 0.0375(13) -0.0077(11) -0.0042(11) -0.0096(11) C77 0.0392(16) 0.0337(15) 0.0454(15) -0.0019(12) -0.0063(13) -0.0111(13) C79 0.0446(16) 0.0280(13) 0.0349(13) -0.0054(11) -0.0056(13) -0.0131(12) C82 0.0305(15) 0.055(2) 0.0575(18) -0.0164(16) -0.0132(13) 0.0020(14) C83 0.0449(17) 0.0461(18) 0.0438(16) -0.0073(14) -0.0188(14) -0.0004(14) C85 0.039(2) 0.043(2) 0.072(3) -0.008(2) -0.017(2) -0.0108(19) C87 0.049(2) 0.078(3) 0.057(2) -0.0172(19) 0.0133(17) -0.0194(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 S73 C851 1.52(2) . ? S73 C85 1.554(6) . ? S84 C85 1.595(6) . ? S86 C87 1.519(5) . ? S88 C87 1.532(5) . ? S94 C95 1.536(10) . ? C95 S96 1.515(10) . ? S92 C91 1.603(6) . ? C91 S93 1.588(7) . ? C851 S841 1.59(2) . ? N73 C72 1.141(4) . ? N75 C74 1.136(4) . ? N78 C77 1.136(4) . ? N80 C79 1.141(4) . ? N81 C68 1.362(4) . ? N81 C82 1.449(4) . ? N81 C83 1.452(4) . ? C1 C10 1.540(4) . ? C1 C13 1.549(3) . ? C1 C63 1.559(3) . ? C1 C2 1.631(3) . ? C2 C50 1.542(4) . ? C2 C3 1.545(4) . ? C2 C61 1.563(4) . ? C3 C4 1.371(4) . ? C3 C8 1.431(4) . ? C4 C5 1.452(4) . ? C4 C51 1.473(4) . ? C5 C6 1.390(4) . ? C5 C53 1.452(4) . ? C6 C7 1.436(4) . ? C6 C35 1.440(4) . ? C7 C8 1.400(4) . ? C7 C45 1.449(4) . ? C8 C9 1.451(4) . ? C9 C46 1.396(4) . ? C9 C50 1.430(4) . ? C10 C51 1.368(4) . ? C10 C11 1.443(4) . ? C11 C55 1.395(4) . ? C11 C12 1.439(4) . ? C12 C17 1.400(4) . ? C12 C13 1.435(4) . ? C13 C14 1.377(4) . ? C14 C15 1.437(4) . ? C14 C49 1.474(4) . ? C15 C16 1.394(4) . ? C15 C60 1.453(4) . ? C16 C17 1.427(4) . ? C16 C20 1.453(4) . ? C17 C18 1.457(4) . ? C18 C56 1.382(4) . ? C18 C19 1.442(4) . ? C19 C24 1.396(4) . ? C19 C20 1.450(5) . ? C20 C21 1.394(4) . ? C21 C59 1.445(4) . ? C21 C22 1.450(4) . ? C22 C23 1.389(5) . ? C22 C40 1.462(4) . ? C23 C27 1.447(4) . ? C23 C24 1.449(4) . ? C24 C25 1.449(4) . ? C25 C57 1.389(4) . ? C25 C39 1.447(4) . ? C26 C40 1.391(4) . ? C26 C38 1.442(4) . ? C26 C28 1.452(4) . ? C27 C28 1.394(4) . ? C27 C39 1.455(4) . ? C28 C29 1.449(4) . ? C29 C30 1.396(4) . ? C29 C37 1.447(4) . ? C30 C34 1.446(4) . ? C30 C31 1.449(4) . ? C31 C39 1.395(4) . ? C31 C32 1.450(4) . ? C32 C58 1.385(4) . ? C32 C33 1.454(4) . ? C33 C53 1.387(4) . ? C33 C34 1.457(4) . ? C34 C35 1.396(4) . ? C35 C36 1.447(4) . ? C36 C37 1.402(4) . ? C36 C45 1.449(4) . ? C37 C38 1.442(4) . ? C38 C43 1.400(4) . ? C40 C41 1.440(5) . ? C41 C42 1.393(4) . ? C41 C59 1.449(4) . ? C42 C47 1.447(4) . ? C42 C43 1.456(4) . ? C43 C44 1.455(4) . ? C44 C45 1.375(4) . ? C44 C46 1.455(4) . ? C46 C47 1.437(4) . ? C47 C48 1.394(4) . ? C48 C60 1.449(4) . ? C48 C49 1.452(4) . ? C49 C50 1.368(4) . ? C51 C52 1.447(4) . ? C52 C54 1.398(4) . ? C52 C53 1.453(4) . ? C54 C55 1.433(4) . ? C54 C58 1.442(4) . ? C55 C56 1.460(4) . ? C56 C57 1.457(4) . ? C57 C58 1.456(4) . ? C59 C60 1.393(4) . ? C61 C62 1.533(4) . ? C63 C71 1.356(4) . ? C63 C64 1.504(4) . ? C64 C76 1.368(4) . ? C64 C65 1.460(4) . ? C65 C70 1.401(4) . ? C65 C66 1.414(4) . ? C66 C67 1.377(4) . ? C67 C68 1.418(4) . ? C68 C69 1.417(4) . ? C69 C70 1.383(4) . ? C71 C72 1.442(4) . ? C71 C74 1.446(4) . ? C76 C79 1.440(4) . ? C76 C77 1.447(4) . ? C61 H61A 1.0800 . ? C61 H61B 1.0800 . ? C62 H62A 1.0800 . ? C62 H62B 1.0800 . ? C62 H62C 1.0800 . ? C66 H66 0.9800 . ? C67 H67 0.9800 . ? C69 H69 0.9800 . ? C70 H70 0.9800 . ? C82 H82A 1.0800 . ? C82 H82B 1.0800 . ? C82 H82C 1.0800 . ? C83 H83A 1.0800 . ? C83 H83B 1.0800 . ? C83 H83C 1.0800 . ? 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 C851 S73 C85 126.2(7) . . ? S96 C95 S94 172.7(17) . . ? S93 C91 S92 174.6(5) . . ? S73 C851 S841 171.1(17) . . ? C68 N81 C82 120.4(3) . . ? C68 N81 C83 120.5(2) . . ? C82 N81 C83 118.9(3) . . ? C10 C1 C13 99.4(2) . . ? C10 C1 C63 105.9(2) . . ? C13 C1 C63 107.2(2) . . ? C10 C1 C2 114.2(2) . . ? C13 C1 C2 113.73(19) . . ? C63 C1 C2 114.9(2) . . ? C50 C2 C3 98.9(2) . . ? C50 C2 C61 108.4(2) . . ? C3 C2 C61 110.8(2) . . ? C50 C2 C1 112.93(19) . . ? C3 C2 C1 112.6(2) . . ? C61 C2 C1 112.5(2) . . ? C4 C3 C8 119.3(3) . . ? C4 C3 C2 125.3(2) . . ? C8 C3 C2 109.9(2) . . ? C3 C4 C5 120.1(2) . . ? C3 C4 C51 120.2(2) . . ? C5 C4 C51 107.3(2) . . ? C6 C5 C53 119.9(3) . . ? C6 C5 C4 120.6(3) . . ? C53 C5 C4 108.3(2) . . ? C5 C6 C7 119.2(3) . . ? C5 C6 C35 120.3(3) . . ? C7 C6 C35 107.9(3) . . ? C8 C7 C6 119.3(2) . . ? C8 C7 C45 119.9(3) . . ? C6 C7 C45 108.5(3) . . ? C7 C8 C3 121.4(3) . . ? C7 C8 C9 119.5(2) . . ? C3 C8 C9 108.6(2) . . ? C46 C9 C50 121.6(2) . . ? C46 C9 C8 120.3(3) . . ? C50 C9 C8 107.9(2) . . ? C51 C10 C11 119.5(2) . . ? C51 C10 C1 124.7(2) . . ? C11 C10 C1 109.8(2) . . ? C55 C11 C12 120.5(2) . . ? C55 C11 C10 120.5(3) . . ? C12 C11 C10 108.6(2) . . ? C17 C12 C13 121.0(3) . . ? C17 C12 C11 120.2(3) . . ? C13 C12 C11 108.6(2) . . ? C14 C13 C12 119.3(2) . . ? C14 C13 C1 124.7(2) . . ? C12 C13 C1 109.9(2) . . ? C13 C14 C15 120.0(2) . . ? C13 C14 C49 120.2(2) . . ? C15 C14 C49 108.0(2) . . ? C16 C15 C14 121.0(3) . . ? C16 C15 C60 119.9(3) . . ? C14 C15 C60 108.4(2) . . ? C15 C16 C17 119.2(3) . . ? C15 C16 C20 120.0(3) . . ? C17 C16 C20 108.1(3) . . ? C12 C17 C16 119.5(3) . . ? C12 C17 C18 119.7(3) . . ? C16 C17 C18 108.6(3) . . ? C56 C18 C19 120.9(3) . . ? C56 C18 C17 119.7(3) . . ? C19 C18 C17 107.3(3) . . ? C24 C19 C18 119.6(3) . . ? C24 C19 C20 120.2(3) . . ? C18 C19 C20 108.4(3) . . ? C21 C20 C19 119.9(3) . . ? C21 C20 C16 119.9(3) . . ? C19 C20 C16 107.6(3) . . ? C20 C21 C59 120.2(3) . . ? C20 C21 C22 119.8(3) . . ? C59 C21 C22 108.2(3) . . ? C23 C22 C21 120.3(3) . . ? C23 C22 C40 120.2(3) . . ? C21 C22 C40 107.5(3) . . ? C22 C23 C27 120.0(3) . . ? C22 C23 C24 120.1(3) . . ? C27 C23 C24 108.0(3) . . ? C19 C24 C25 120.0(3) . . ? C19 C24 C23 119.7(3) . . ? C25 C24 C23 108.3(3) . . ? C57 C25 C39 120.3(3) . . ? C57 C25 C24 120.0(3) . . ? C39 C25 C24 107.8(3) . . ? C40 C26 C38 120.0(3) . . ? C40 C26 C28 120.2(3) . . ? C38 C26 C28 107.7(3) . . ? C28 C27 C23 120.2(3) . . ? C28 C27 C39 120.3(3) . . ? C23 C27 C39 107.8(3) . . ? C27 C28 C29 120.2(3) . . ? C27 C28 C26 119.9(3) . . ? C29 C28 C26 108.0(3) . . ? C30 C29 C37 120.4(3) . . ? C30 C29 C28 119.6(3) . . ? C37 C29 C28 107.8(3) . . ? C29 C30 C34 119.5(3) . . ? C29 C30 C31 120.3(3) . . ? C34 C30 C31 108.4(3) . . ? C39 C31 C30 120.2(3) . . ? C39 C31 C32 119.6(3) . . ? C30 C31 C32 108.2(3) . . ? C58 C32 C31 120.4(3) . . ? C58 C32 C33 120.1(3) . . ? C31 C32 C33 107.6(3) . . ? C53 C33 C32 119.9(3) . . ? C53 C33 C34 119.7(3) . . ? C32 C33 C34 108.2(3) . . ? C35 C34 C30 120.6(3) . . ? C35 C34 C33 119.9(3) . . ? C30 C34 C33 107.6(3) . . ? C34 C35 C6 120.0(3) . . ? C34 C35 C36 119.7(3) . . ? C6 C35 C36 108.3(3) . . ? C37 C36 C35 120.1(3) . . ? C37 C36 C45 119.5(3) . . ? C35 C36 C45 107.7(3) . . ? C36 C37 C38 120.2(3) . . ? C36 C37 C29 119.8(3) . . ? C38 C37 C29 108.1(3) . . ? C43 C38 C37 119.8(3) . . ? C43 C38 C26 119.6(3) . . ? C37 C38 C26 108.4(3) . . ? C31 C39 C25 120.0(3) . . ? C31 C39 C27 119.4(3) . . ? C25 C39 C27 108.2(3) . . ? C26 C40 C41 120.6(3) . . ? C26 C40 C22 119.5(3) . . ? C41 C40 C22 108.0(3) . . ? C42 C41 C40 120.0(3) . . ? C42 C41 C59 120.1(3) . . ? C40 C41 C59 108.2(3) . . ? C41 C42 C47 120.2(3) . . ? C41 C42 C43 119.6(3) . . ? C47 C42 C43 107.4(2) . . ? C38 C43 C44 119.8(3) . . ? C38 C43 C42 120.2(3) . . ? C44 C43 C42 108.6(3) . . ? C45 C44 C43 120.1(3) . . ? C45 C44 C46 120.5(3) . . ? C43 C44 C46 106.8(2) . . ? C44 C45 C7 120.4(3) . . ? C44 C45 C36 120.5(3) . . ? C7 C45 C36 107.5(3) . . ? C9 C46 C47 118.9(2) . . ? C9 C46 C44 119.4(3) . . ? C47 C46 C44 108.9(3) . . ? C48 C47 C46 119.5(3) . . ? C48 C47 C42 120.0(3) . . ? C46 C47 C42 108.4(2) . . ? C47 C48 C60 119.8(3) . . ? C47 C48 C49 120.4(2) . . ? C60 C48 C49 108.3(2) . . ? C50 C49 C48 120.1(2) . . ? C50 C49 C14 120.2(2) . . ? C48 C49 C14 107.2(2) . . ? C49 C50 C9 119.5(2) . . ? C49 C50 C2 125.4(2) . . ? C9 C50 C2 110.3(2) . . ? C10 C51 C52 120.2(2) . . ? C10 C51 C4 120.3(2) . . ? C52 C51 C4 108.0(2) . . ? C54 C52 C51 120.7(3) . . ? C54 C52 C53 119.5(3) . . ? C51 C52 C53 108.1(2) . . ? C33 C53 C5 120.2(3) . . ? C33 C53 C52 120.1(3) . . ? C5 C53 C52 108.2(3) . . ? C52 C54 C55 118.7(3) . . ? C52 C54 C58 120.2(3) . . ? C55 C54 C58 108.6(3) . . ? C11 C55 C54 120.3(2) . . ? C11 C55 C56 119.1(3) . . ? C54 C55 C56 108.5(3) . . ? C18 C56 C57 119.6(3) . . ? C18 C56 C55 120.8(3) . . ? C57 C56 C55 107.0(3) . . ? C25 C57 C58 119.7(3) . . ? C25 C57 C56 120.0(3) . . ? C58 C57 C56 108.0(3) . . ? C32 C58 C54 120.1(3) . . ? C32 C58 C57 120.0(3) . . ? C54 C58 C57 107.8(3) . . ? C60 C59 C21 120.1(3) . . ? C60 C59 C41 119.6(3) . . ? C21 C59 C41 108.2(3) . . ? C59 C60 C48 120.4(3) . . ? C59 C60 C15 120.0(3) . . ? C48 C60 C15 108.1(2) . . ? C62 C61 C2 115.4(2) . . ? C71 C63 C64 117.6(2) . . ? C71 C63 C1 124.6(2) . . ? C64 C63 C1 117.6(2) . . ? C76 C64 C65 123.4(2) . . ? C76 C64 C63 119.0(2) . . ? C65 C64 C63 117.6(2) . . ? C70 C65 C66 118.0(2) . . ? C70 C65 C64 122.1(2) . . ? C66 C65 C64 119.8(2) . . ? C67 C66 C65 121.2(2) . . ? C66 C67 C68 121.1(3) . . ? N81 C68 C69 121.6(3) . . ? N81 C68 C67 121.0(3) . . ? C69 C68 C67 117.4(3) . . ? C70 C69 C68 121.2(3) . . ? C69 C70 C65 121.1(3) . . ? C63 C71 C72 120.6(2) . . ? C63 C71 C74 124.6(2) . . ? C72 C71 C74 114.7(2) . . ? N73 C72 C71 177.8(3) . . ? N75 C74 C71 174.8(3) . . ? C64 C76 C79 122.4(2) . . ? C64 C76 C77 122.2(3) . . ? C79 C76 C77 115.3(2) . . ? N78 C77 C76 177.6(3) . . ? N80 C79 C76 177.2(3) . . ? S73 C85 S84 176.4(4) . . ? S86 C87 S88 178.8(4) . . ? C62 C61 H61A 108.4 . . ? C2 C61 H61A 108.4 . . ? C62 C61 H61B 108.4 . . ? C2 C61 H61B 108.4 . . ? H61A C61 H61B 107.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C67 C66 H66 119.4 . . ? C65 C66 H66 119.4 . . ? C66 C67 H67 119.5 . . ? C68 C67 H67 119.5 . . ? C70 C69 H69 119.4 . . ? C68 C69 H69 119.4 . . ? C69 C70 H70 119.4 . . ? C65 C70 H70 119.4 . . ? N81 C82 H82A 109.5 . . ? N81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N81 C83 H83A 109.5 . . ? N81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? 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 C85 S73 C851 S841 -65(8) . . . . ? C10 C1 C2 C50 111.4(2) . . . . ? C13 C1 C2 C50 -1.8(3) . . . . ? C63 C1 C2 C50 -125.9(2) . . . . ? C10 C1 C2 C3 0.5(3) . . . . ? C13 C1 C2 C3 -112.7(2) . . . . ? C63 C1 C2 C3 123.2(2) . . . . ? C10 C1 C2 C61 -125.6(2) . . . . ? C13 C1 C2 C61 121.3(2) . . . . ? C63 C1 C2 C61 -2.8(3) . . . . ? C50 C2 C3 C4 -133.3(3) . . . . ? C61 C2 C3 C4 113.1(3) . . . . ? C1 C2 C3 C4 -13.8(3) . . . . ? C50 C2 C3 C8 19.9(3) . . . . ? C61 C2 C3 C8 -93.7(2) . . . . ? C1 C2 C3 C8 139.4(2) . . . . ? C8 C3 C4 C5 1.3(4) . . . . ? C2 C3 C4 C5 152.2(2) . . . . ? C8 C3 C4 C51 -136.1(3) . . . . ? C2 C3 C4 C51 14.8(4) . . . . ? C3 C4 C5 C6 0.9(4) . . . . ? C51 C4 C5 C6 143.1(2) . . . . ? C3 C4 C5 C53 -142.8(2) . . . . ? C51 C4 C5 C53 -0.6(3) . . . . ? C53 C5 C6 C7 138.1(3) . . . . ? C4 C5 C6 C7 -1.6(4) . . . . ? C53 C5 C6 C35 0.7(4) . . . . ? C4 C5 C6 C35 -138.9(3) . . . . ? C5 C6 C7 C8 0.0(4) . . . . ? C35 C6 C7 C8 142.1(3) . . . . ? C5 C6 C7 C45 -142.2(3) . . . . ? C35 C6 C7 C45 -0.1(3) . . . . ? C6 C7 C8 C3 2.2(4) . . . . ? C45 C7 C8 C3 140.1(3) . . . . ? C6 C7 C8 C9 -138.5(3) . . . . ? C45 C7 C8 C9 -0.6(4) . . . . ? C4 C3 C8 C7 -2.9(4) . . . . ? C2 C3 C8 C7 -157.9(2) . . . . ? C4 C3 C8 C9 141.6(2) . . . . ? C2 C3 C8 C9 -13.4(3) . . . . ? C7 C8 C9 C46 -0.6(4) . . . . ? C3 C8 C9 C46 -145.9(2) . . . . ? C7 C8 C9 C50 145.2(2) . . . . ? C3 C8 C9 C50 -0.1(3) . . . . ? C13 C1 C10 C51 134.0(3) . . . . ? C63 C1 C10 C51 -115.0(3) . . . . ? C2 C1 C10 C51 12.5(3) . . . . ? C13 C1 C10 C11 -18.5(3) . . . . ? C63 C1 C10 C11 92.6(2) . . . . ? C2 C1 C10 C11 -139.9(2) . . . . ? C51 C10 C11 C55 3.6(4) . . . . ? C1 C10 C11 C55 157.7(2) . . . . ? C51 C10 C11 C12 -141.4(2) . . . . ? C1 C10 C11 C12 12.8(3) . . . . ? C55 C11 C12 C17 0.1(4) . . . . ? C10 C11 C12 C17 145.1(2) . . . . ? C55 C11 C12 C13 -145.3(2) . . . . ? C10 C11 C12 C13 -0.4(3) . . . . ? C17 C12 C13 C14 -3.6(4) . . . . ? C11 C12 C13 C14 141.6(2) . . . . ? C17 C12 C13 C1 -157.3(2) . . . . ? C11 C12 C13 C1 -12.1(3) . . . . ? C10 C1 C13 C14 -133.6(3) . . . . ? C63 C1 C13 C14 116.3(3) . . . . ? C2 C1 C13 C14 -11.8(4) . . . . ? C10 C1 C13 C12 18.3(3) . . . . ? C63 C1 C13 C12 -91.7(2) . . . . ? C2 C1 C13 C12 140.1(2) . . . . ? C12 C13 C14 C15 2.0(4) . . . . ? C1 C13 C14 C15 151.5(3) . . . . ? C12 C13 C14 C49 -136.5(3) . . . . ? C1 C13 C14 C49 13.0(4) . . . . ? C13 C14 C15 C16 0.8(4) . . . . ? C49 C14 C15 C16 143.7(3) . . . . ? C13 C14 C15 C60 -143.4(3) . . . . ? C49 C14 C15 C60 -0.5(3) . . . . ? C14 C15 C16 C17 -2.0(4) . . . . ? C60 C15 C16 C17 138.2(3) . . . . ? C14 C15 C16 C20 -139.2(3) . . . . ? C60 C15 C16 C20 1.0(4) . . . . ? C13 C12 C17 C16 2.4(4) . . . . ? C11 C12 C17 C16 -138.8(3) . . . . ? C13 C12 C17 C18 140.6(3) . . . . ? C11 C12 C17 C18 -0.6(4) . . . . ? C15 C16 C17 C12 0.4(4) . . . . ? C20 C16 C17 C12 142.1(3) . . . . ? C15 C16 C17 C18 -142.0(3) . . . . ? C20 C16 C17 C18 -0.3(3) . . . . ? C12 C17 C18 C56 1.0(4) . . . . ? C16 C17 C18 C56 143.3(3) . . . . ? C12 C17 C18 C19 -141.8(3) . . . . ? C16 C17 C18 C19 0.5(3) . . . . ? C56 C18 C19 C24 0.1(4) . . . . ? C17 C18 C19 C24 142.4(3) . . . . ? C56 C18 C19 C20 -142.9(3) . . . . ? C17 C18 C19 C20 -0.5(3) . . . . ? C24 C19 C20 C21 -0.7(4) . . . . ? C18 C19 C20 C21 142.0(3) . . . . ? C24 C19 C20 C16 -142.3(3) . . . . ? C18 C19 C20 C16 0.4(3) . . . . ? C15 C16 C20 C21 -0.4(4) . . . . ? C17 C16 C20 C21 -141.7(3) . . . . ? C15 C16 C20 C19 141.3(3) . . . . ? C17 C16 C20 C19 -0.1(3) . . . . ? C19 C20 C21 C59 -137.6(3) . . . . ? C16 C20 C21 C59 -0.6(4) . . . . ? C19 C20 C21 C22 0.9(4) . . . . ? C16 C20 C21 C22 137.9(3) . . . . ? C20 C21 C22 C23 -0.7(4) . . . . ? C59 C21 C22 C23 142.2(3) . . . . ? C20 C21 C22 C40 -143.3(3) . . . . ? C59 C21 C22 C40 -0.3(3) . . . . ? C21 C22 C23 C27 -138.0(3) . . . . ? C40 C22 C23 C27 -0.1(4) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? C40 C22 C23 C24 138.1(3) . . . . ? C18 C19 C24 C25 -0.1(4) . . . . ? C20 C19 C24 C25 138.5(3) . . . . ? C18 C19 C24 C23 -138.4(3) . . . . ? C20 C19 C24 C23 0.2(4) . . . . ? C22 C23 C24 C19 0.0(4) . . . . ? C27 C23 C24 C19 142.6(3) . . . . ? C22 C23 C24 C25 -142.6(3) . . . . ? C27 C23 C24 C25 0.0(3) . . . . ? C19 C24 C25 C57 0.2(4) . . . . ? C23 C24 C25 C57 142.6(3) . . . . ? C19 C24 C25 C39 -142.7(3) . . . . ? C23 C24 C25 C39 -0.3(3) . . . . ? C22 C23 C27 C28 -0.2(4) . . . . ? C24 C23 C27 C28 -142.8(3) . . . . ? C22 C23 C27 C39 142.9(3) . . . . ? C24 C23 C27 C39 0.2(3) . . . . ? C23 C27 C28 C29 138.4(3) . . . . ? C39 C27 C28 C29 -0.2(4) . . . . ? C23 C27 C28 C26 0.0(4) . . . . ? C39 C27 C28 C26 -138.5(3) . . . . ? C40 C26 C28 C27 0.4(4) . . . . ? C38 C26 C28 C27 142.9(3) . . . . ? C40 C26 C28 C29 -142.5(3) . . . . ? C38 C26 C28 C29 0.1(3) . . . . ? C27 C28 C29 C30 -0.4(4) . . . . ? C26 C28 C29 C30 142.4(3) . . . . ? C27 C28 C29 C37 -142.8(3) . . . . ? C26 C28 C29 C37 0.0(3) . . . . ? C37 C29 C30 C34 -0.5(4) . . . . ? C28 C29 C30 C34 -138.2(3) . . . . ? C37 C29 C30 C31 138.2(3) . . . . ? C28 C29 C30 C31 0.5(4) . . . . ? C29 C30 C31 C39 -0.1(4) . . . . ? C34 C30 C31 C39 142.6(3) . . . . ? C29 C30 C31 C32 -142.7(3) . . . . ? C34 C30 C31 C32 0.0(3) . . . . ? C39 C31 C32 C58 -0.2(4) . . . . ? C30 C31 C32 C58 142.7(3) . . . . ? C39 C31 C32 C33 -142.8(3) . . . . ? C30 C31 C32 C33 0.0(3) . . . . ? C58 C32 C33 C53 -0.7(4) . . . . ? C31 C32 C33 C53 142.2(3) . . . . ? C58 C32 C33 C34 -142.9(3) . . . . ? C31 C32 C33 C34 -0.1(3) . . . . ? C29 C30 C34 C35 0.3(4) . . . . ? C31 C30 C34 C35 -142.8(3) . . . . ? C29 C30 C34 C33 143.0(3) . . . . ? C31 C30 C34 C33 -0.1(3) . . . . ? C53 C33 C34 C35 0.8(4) . . . . ? C32 C33 C34 C35 143.1(3) . . . . ? C53 C33 C34 C30 -142.2(3) . . . . ? C32 C33 C34 C30 0.1(3) . . . . ? C30 C34 C35 C6 138.0(3) . . . . ? C33 C34 C35 C6 -0.2(4) . . . . ? C30 C34 C35 C36 -0.4(4) . . . . ? C33 C34 C35 C36 -138.6(3) . . . . ? C5 C6 C35 C34 -0.5(4) . . . . ? C7 C6 C35 C34 -142.1(3) . . . . ? C5 C6 C35 C36 142.0(3) . . . . ? C7 C6 C35 C36 0.4(3) . . . . ? C34 C35 C36 C37 0.6(4) . . . . ? C6 C35 C36 C37 -142.1(3) . . . . ? C34 C35 C36 C45 142.1(3) . . . . ? C6 C35 C36 C45 -0.6(3) . . . . ? C35 C36 C37 C38 137.6(3) . . . . ? C45 C36 C37 C38 0.5(4) . . . . ? C35 C36 C37 C29 -0.8(4) . . . . ? C45 C36 C37 C29 -137.8(3) . . . . ? C30 C29 C37 C36 0.7(4) . . . . ? C28 C29 C37 C36 142.8(3) . . . . ? C30 C29 C37 C38 -142.1(3) . . . . ? C28 C29 C37 C38 0.0(3) . . . . ? C36 C37 C38 C43 -0.3(4) . . . . ? C29 C37 C38 C43 142.3(3) . . . . ? C36 C37 C38 C26 -142.5(3) . . . . ? C29 C37 C38 C26 0.1(3) . . . . ? C40 C26 C38 C43 0.2(4) . . . . ? C28 C26 C38 C43 -142.4(3) . . . . ? C40 C26 C38 C37 142.5(3) . . . . ? C28 C26 C38 C37 -0.1(3) . . . . ? C30 C31 C39 C25 -138.0(3) . . . . ? C32 C31 C39 C25 0.4(4) . . . . ? C30 C31 C39 C27 -0.4(4) . . . . ? C32 C31 C39 C27 138.0(3) . . . . ? C57 C25 C39 C31 -0.5(4) . . . . ? C24 C25 C39 C31 142.2(3) . . . . ? C57 C25 C39 C27 -142.4(3) . . . . ? C24 C25 C39 C27 0.4(3) . . . . ? C28 C27 C39 C31 0.6(4) . . . . ? C23 C27 C39 C31 -142.5(3) . . . . ? C28 C27 C39 C25 142.6(3) . . . . ? C23 C27 C39 C25 -0.4(3) . . . . ? C38 C26 C40 C41 -0.2(4) . . . . ? C28 C26 C40 C41 137.8(3) . . . . ? C38 C26 C40 C22 -138.6(3) . . . . ? C28 C26 C40 C22 -0.6(4) . . . . ? C23 C22 C40 C26 0.5(4) . . . . ? C21 C22 C40 C26 143.1(3) . . . . ? C23 C22 C40 C41 -142.6(3) . . . . ? C21 C22 C40 C41 0.0(3) . . . . ? C26 C40 C41 C42 0.7(4) . . . . ? C22 C40 C41 C42 143.3(3) . . . . ? C26 C40 C41 C59 -142.3(3) . . . . ? C22 C40 C41 C59 0.3(3) . . . . ? C40 C41 C42 C47 -137.8(3) . . . . ? C59 C41 C42 C47 0.8(4) . . . . ? C40 C41 C42 C43 -1.2(4) . . . . ? C59 C41 C42 C43 137.4(3) . . . . ? C37 C38 C43 C44 0.5(4) . . . . ? C26 C38 C43 C44 138.6(3) . . . . ? C37 C38 C43 C42 -138.8(3) . . . . ? C26 C38 C43 C42 -0.7(4) . . . . ? C41 C42 C43 C38 1.2(4) . . . . ? C47 C42 C43 C38 142.7(3) . . . . ? C41 C42 C43 C44 -142.2(3) . . . . ? C47 C42 C43 C44 -0.6(3) . . . . ? C38 C43 C44 C45 -1.1(4) . . . . ? C42 C43 C44 C45 142.4(3) . . . . ? C38 C43 C44 C46 -143.0(3) . . . . ? C42 C43 C44 C46 0.5(3) . . . . ? C43 C44 C45 C7 -137.3(3) . . . . ? C46 C44 C45 C7 -0.6(4) . . . . ? C43 C44 C45 C36 1.4(4) . . . . ? C46 C44 C45 C36 138.1(3) . . . . ? C8 C7 C45 C44 1.2(4) . . . . ? C6 C7 C45 C44 143.2(3) . . . . ? C8 C7 C45 C36 -142.1(3) . . . . ? C6 C7 C45 C36 -0.2(3) . . . . ? C37 C36 C45 C44 -1.1(4) . . . . ? C35 C36 C45 C44 -142.8(3) . . . . ? C37 C36 C45 C7 142.2(3) . . . . ? C35 C36 C45 C7 0.5(3) . . . . ? C50 C9 C46 C47 -2.4(4) . . . . ? C8 C9 C46 C47 138.7(3) . . . . ? C50 C9 C46 C44 -139.8(3) . . . . ? C8 C9 C46 C44 1.3(4) . . . . ? C45 C44 C46 C9 -0.7(4) . . . . ? C43 C44 C46 C9 141.1(3) . . . . ? C45 C44 C46 C47 -141.9(3) . . . . ? C43 C44 C46 C47 -0.1(3) . . . . ? C9 C46 C47 C48 0.7(4) . . . . ? C44 C46 C47 C48 142.2(3) . . . . ? C9 C46 C47 C42 -141.7(3) . . . . ? C44 C46 C47 C42 -0.3(3) . . . . ? C41 C42 C47 C48 -0.4(4) . . . . ? C43 C42 C47 C48 -141.7(3) . . . . ? C41 C42 C47 C46 141.8(3) . . . . ? C43 C42 C47 C46 0.5(3) . . . . ? C46 C47 C48 C60 -138.0(3) . . . . ? C42 C47 C48 C60 0.1(4) . . . . ? C46 C47 C48 C49 1.0(4) . . . . ? C42 C47 C48 C49 139.1(3) . . . . ? C47 C48 C49 C50 -1.1(4) . . . . ? C60 C48 C49 C50 142.0(3) . . . . ? C47 C48 C49 C14 -143.1(3) . . . . ? C60 C48 C49 C14 0.0(3) . . . . ? C13 C14 C49 C50 1.2(4) . . . . ? C15 C14 C49 C50 -141.7(3) . . . . ? C13 C14 C49 C48 143.2(3) . . . . ? C15 C14 C49 C48 0.3(3) . . . . ? C48 C49 C50 C9 -0.5(4) . . . . ? C14 C49 C50 C9 136.6(3) . . . . ? C48 C49 C50 C2 -153.3(3) . . . . ? C14 C49 C50 C2 -16.2(4) . . . . ? C46 C9 C50 C49 2.3(4) . . . . ? C8 C9 C50 C49 -142.9(3) . . . . ? C46 C9 C50 C2 158.9(2) . . . . ? C8 C9 C50 C2 13.7(3) . . . . ? C3 C2 C50 C49 134.8(3) . . . . ? C61 C2 C50 C49 -109.6(3) . . . . ? C1 C2 C50 C49 15.6(4) . . . . ? C3 C2 C50 C9 -20.1(3) . . . . ? C61 C2 C50 C9 95.4(3) . . . . ? C1 C2 C50 C9 -139.3(2) . . . . ? C11 C10 C51 C52 -2.3(4) . . . . ? C1 C10 C51 C52 -152.3(2) . . . . ? C11 C10 C51 C4 136.7(3) . . . . ? C1 C10 C51 C4 -13.3(4) . . . . ? C3 C4 C51 C10 -0.7(4) . . . . ? C5 C4 C51 C10 -142.8(2) . . . . ? C3 C4 C51 C52 142.8(2) . . . . ? C5 C4 C51 C52 0.6(3) . . . . ? C10 C51 C52 C54 0.3(4) . . . . ? C4 C51 C52 C54 -143.2(3) . . . . ? C10 C51 C52 C53 143.2(2) . . . . ? C4 C51 C52 C53 -0.3(3) . . . . ? C32 C33 C53 C5 -138.5(3) . . . . ? C34 C33 C53 C5 -0.5(4) . . . . ? C32 C33 C53 C52 0.6(4) . . . . ? C34 C33 C53 C52 138.6(3) . . . . ? C6 C5 C53 C33 -0.2(4) . . . . ? C4 C5 C53 C33 143.9(3) . . . . ? C6 C5 C53 C52 -143.7(3) . . . . ? C4 C5 C53 C52 0.4(3) . . . . ? C54 C52 C53 C33 -0.1(4) . . . . ? C51 C52 C53 C33 -143.5(3) . . . . ? C54 C52 C53 C5 143.4(3) . . . . ? C51 C52 C53 C5 0.0(3) . . . . ? C51 C52 C54 C55 0.5(4) . . . . ? C53 C52 C54 C55 -138.2(3) . . . . ? C51 C52 C54 C58 138.4(3) . . . . ? C53 C52 C54 C58 -0.4(4) . . . . ? C12 C11 C55 C54 138.0(3) . . . . ? C10 C11 C55 C54 -2.8(4) . . . . ? C12 C11 C55 C56 -0.2(4) . . . . ? C10 C11 C55 C56 -141.0(3) . . . . ? C52 C54 C55 C11 0.7(4) . . . . ? C58 C54 C55 C11 -141.5(3) . . . . ? C52 C54 C55 C56 142.9(3) . . . . ? C58 C54 C55 C56 0.6(3) . . . . ? C19 C18 C56 C57 -0.1(4) . . . . ? C17 C18 C56 C57 -137.9(3) . . . . ? C19 C18 C56 C55 136.7(3) . . . . ? C17 C18 C56 C55 -1.0(4) . . . . ? C11 C55 C56 C18 0.6(4) . . . . ? C54 C55 C56 C18 -142.0(3) . . . . ? C11 C55 C56 C57 142.2(3) . . . . ? C54 C55 C56 C57 -0.5(3) . . . . ? C39 C25 C57 C58 0.4(4) . . . . ? C24 C25 C57 C58 -137.9(3) . . . . ? C39 C25 C57 C56 138.1(3) . . . . ? C24 C25 C57 C56 -0.2(4) . . . . ? C18 C56 C57 C25 0.2(4) . . . . ? C55 C56 C57 C25 -141.9(3) . . . . ? C18 C56 C57 C58 142.2(3) . . . . ? C55 C56 C57 C58 0.1(3) . . . . ? C31 C32 C58 C54 -137.9(3) . . . . ? C33 C32 C58 C54 0.1(4) . . . . ? C31 C32 C58 C57 0.0(4) . . . . ? C33 C32 C58 C57 138.1(3) . . . . ? C52 C54 C58 C32 0.4(4) . . . . ? C55 C54 C58 C32 142.0(3) . . . . ? C52 C54 C58 C57 -142.1(3) . . . . ? C55 C54 C58 C57 -0.5(3) . . . . ? C25 C57 C58 C32 -0.1(4) . . . . ? C56 C57 C58 C32 -142.3(3) . . . . ? C25 C57 C58 C54 142.4(3) . . . . ? C56 C57 C58 C54 0.2(3) . . . . ? C20 C21 C59 C60 0.9(4) . . . . ? C22 C21 C59 C60 -141.8(3) . . . . ? C20 C21 C59 C41 143.3(3) . . . . ? C22 C21 C59 C41 0.6(3) . . . . ? C42 C41 C59 C60 -0.9(4) . . . . ? C40 C41 C59 C60 142.0(3) . . . . ? C42 C41 C59 C21 -143.5(3) . . . . ? C40 C41 C59 C21 -0.5(3) . . . . ? C21 C59 C60 C48 138.7(3) . . . . ? C41 C59 C60 C48 0.6(4) . . . . ? C21 C59 C60 C15 -0.3(4) . . . . ? C41 C59 C60 C15 -138.4(3) . . . . ? C47 C48 C60 C59 -0.2(4) . . . . ? C49 C48 C60 C59 -143.6(3) . . . . ? C47 C48 C60 C15 143.1(3) . . . . ? C49 C48 C60 C15 -0.3(3) . . . . ? C16 C15 C60 C59 -0.7(4) . . . . ? C14 C15 C60 C59 143.9(3) . . . . ? C16 C15 C60 C48 -144.2(3) . . . . ? C14 C15 C60 C48 0.5(3) . . . . ? C50 C2 C61 C62 -52.4(3) . . . . ? C3 C2 C61 C62 55.1(3) . . . . ? C1 C2 C61 C62 -177.9(2) . . . . ? C10 C1 C63 C71 53.5(3) . . . . ? C13 C1 C63 C71 159.0(2) . . . . ? C2 C1 C63 C71 -73.6(3) . . . . ? C10 C1 C63 C64 -120.7(2) . . . . ? C13 C1 C63 C64 -15.2(3) . . . . ? C2 C1 C63 C64 112.3(2) . . . . ? C71 C63 C64 C76 -75.5(3) . . . . ? C1 C63 C64 C76 99.0(3) . . . . ? C71 C63 C64 C65 103.5(3) . . . . ? C1 C63 C64 C65 -81.9(3) . . . . ? C76 C64 C65 C70 -44.6(4) . . . . ? C63 C64 C65 C70 136.4(3) . . . . ? C76 C64 C65 C66 131.4(3) . . . . ? C63 C64 C65 C66 -47.6(3) . . . . ? C70 C65 C66 C67 0.8(4) . . . . ? C64 C65 C66 C67 -175.3(3) . . . . ? C65 C66 C67 C68 -1.2(4) . . . . ? C82 N81 C68 C69 -2.0(5) . . . . ? C83 N81 C68 C69 -176.5(3) . . . . ? C82 N81 C68 C67 178.4(3) . . . . ? C83 N81 C68 C67 3.9(5) . . . . ? C66 C67 C68 N81 -179.8(3) . . . . ? C66 C67 C68 C69 0.6(4) . . . . ? N81 C68 C69 C70 -179.3(3) . . . . ? C67 C68 C69 C70 0.3(4) . . . . ? C68 C69 C70 C65 -0.7(5) . . . . ? C66 C65 C70 C69 0.1(4) . . . . ? C64 C65 C70 C69 176.1(3) . . . . ? C64 C63 C71 C72 -2.3(4) . . . . ? C1 C63 C71 C72 -176.5(2) . . . . ? C64 C63 C71 C74 180.0(2) . . . . ? C1 C63 C71 C74 5.8(4) . . . . ? C63 C71 C72 N73 -152(8) . . . . ? C74 C71 C72 N73 26(8) . . . . ? C63 C71 C74 N75 156(3) . . . . ? C72 C71 C74 N75 -22(3) . . . . ? C65 C64 C76 C79 -178.3(3) . . . . ? C63 C64 C76 C79 0.7(4) . . . . ? C65 C64 C76 C77 -2.3(4) . . . . ? C63 C64 C76 C77 176.6(3) . . . . ? C64 C76 C77 N78 -164(9) . . . . ? C79 C76 C77 N78 12(9) . . . . ? C64 C76 C79 N80 110(6) . . . . ? C77 C76 C79 N80 -67(6) . . . . ? C851 S73 C85 S84 -95(6) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.806 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.070 _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # Attachment 'CCDC770541-yamChemCom-3b.cif.txt' # CIF Copied by cif2cif, version 0.0.8 - beta ( 2 Apr 98) data_3b _database_code_depnum_ccdc_archive 'CCDC 770541' #TrackingRef 'CCDC770541-yamChemCom-3b.cif.txt' _chemical_compound_source 'LOC ETH Zurich' _exptl_crystal_description needle _exptl_crystal_size_max .27 _exptl_crystal_size_mid .075 _exptl_crystal_size_min .012 _exptl_crystal_F_000 1400.0 _exptl_crystal_colour black _diffrn_ambient_temperature 123 _cell_measurement_temperature 123 _refine_ls_hydrogen_treatment constr # Submission details _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.06892 _diffrn_orient_matrix_UB_12 0.04088 _diffrn_orient_matrix_UB_13 0.06135 _diffrn_orient_matrix_UB_21 0.01591 _diffrn_orient_matrix_UB_22 0.03680 _diffrn_orient_matrix_UB_23 -0.04764 _diffrn_orient_matrix_UB_31 -0.04635 _diffrn_orient_matrix_UB_32 0.01934 _diffrn_orient_matrix_UB_33 0.03328 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1373.717 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting Triclinic _chemical_formula_moiety 'C79 H17 N5 , 3( C6 H5 Cl)' _chemical_formula_sum 'C97 H32 Cl3 N5 ' _chemical_name_systematic ; ? ; _cell_length_a 9.9620(7) _cell_length_b 17.8492(9) _cell_length_c 18.4538(12) _cell_angle_alpha 64.282(3) _cell_angle_beta 84.813(2) _cell_angle_gamma 85.112(2) _cell_volume 2940.3(3) _diffrn_reflns_av_R_equivalents 0.145 _diffrn_reflns_number 9701 _diffrn_reflns_theta_max 20.68 _diffrn_reflns_theta_min 4.92 _diffrn_reflns_theta_full 20.68 _cell_measurement_reflns_used 9747 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 20.600 _diffrn_measurement_method CCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97(Altomare et al., J. Appl. Cryst.,1999)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' Cl Cl 0.1484 0.1585 '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' _exptl_absorpt_coefficient_mu 0.222 _reflns_number_total 5697 _reflns_number_gt 3469 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Structure contains three Chlorobenzene molecules of which two are disordered (refined with constraints). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5697 _refine_ls_number_parameters 882 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1841 _refine_ls_R_factor_gt 0.1200 _refine_ls_wR_factor_ref 0.2873 _refine_ls_wR_factor_gt 0.2542 _refine_ls_goodness_of_fit_ref 1.432 _refine_ls_restrained_S_all 1.432 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl85 Cl 0.1589(4) 0.2945(3) 0.2323(2) 0.0782(12) Uani 1 1 d . . . Cl92 Cl 0.2427(5) 0.1195(3) 0.4103(4) 0.1118(18) Uani 1 1 d . . . Cl93 Cl -0.2539(7) 0.5589(4) 0.4470(3) 0.149(3) Uani 1 1 d . . . N66 N 0.0018(11) 0.0397(6) 0.2260(6) 0.041(2) Uani 1 1 d . . . N68 N -0.2923(9) -0.0479(6) 0.2001(6) 0.036(2) Uani 1 1 d . . . N73 N -0.4516(10) 0.3336(6) 0.2941(7) 0.052(3) Uani 1 1 d . . . N75 N -0.5897(11) 0.4195(7) 0.0672(7) 0.048(3) Uani 1 1 d . . . N82 N -0.2524(11) 0.0857(7) 0.5438(7) 0.062(3) Uani 1 1 d . . . C1 C -0.2381(11) 0.1680(6) 0.0833(6) 0.032(3) Uani 1 1 d . . . C2 C -0.3611(10) 0.2368(6) 0.0710(6) 0.028(3) Uani 1 1 d . . . C3 C -0.5033(10) 0.2251(6) 0.0433(6) 0.030(3) Uani 1 1 d . . . C4 C -0.4899(10) 0.1593(6) 0.0104(6) 0.031(3) Uani 1 1 d . . . C5 C -0.3904(9) 0.0999(6) 0.0206(6) 0.024(2) Uani 1 1 d . . . C6 C -0.2615(10) 0.0897(6) 0.0651(7) 0.030(3) Uani 1 1 d . . . C7 C -0.1555(10) 0.0704(6) 0.0077(7) 0.030(3) Uani 1 1 d . . . C8 C -0.2195(10) 0.0461(6) -0.0440(7) 0.030(3) Uani 1 1 d . . . C9 C -0.3641(11) 0.0628(6) -0.0357(6) 0.029(3) Uani 1 1 d . . . C10 C -0.4428(10) 0.0855(6) -0.1003(7) 0.032(3) Uani 1 1 d . . . C11 C -0.3838(11) 0.0964(6) -0.1777(6) 0.028(3) Uani 1 1 d . . . C12 C -0.2456(11) 0.0829(6) -0.1873(7) 0.032(3) Uani 1 1 d . . . C13 C -0.1616(10) 0.0568(6) -0.1183(7) 0.029(3) Uani 1 1 d . . . C14 C -0.0370(10) 0.0985(6) -0.1492(7) 0.033(3) Uani 1 1 d . . . C15 C -0.0396(10) 0.1504(6) -0.2331(6) 0.026(2) Uani 1 1 d . . . C16 C -0.1719(11) 0.1411(6) -0.2583(6) 0.031(3) Uani 1 1 d . . . C17 C -0.2380(11) 0.2087(6) -0.3147(6) 0.032(3) Uani 1 1 d . . . C18 C -0.3843(11) 0.2230(6) -0.3063(6) 0.031(3) Uani 1 1 d . . . C19 C -0.4572(10) 0.1693(6) -0.2384(6) 0.028(3) Uani 1 1 d . . . C20 C -0.5591(10) 0.1996(6) -0.1986(6) 0.026(2) Uani 1 1 d . . . C21 C -0.5883(11) 0.2851(6) -0.2265(7) 0.033(3) Uiso 1 1 d . . . C22 C -0.5149(10) 0.3414(6) -0.2956(6) 0.033(3) Uani 1 1 d . . . C23 C -0.4133(11) 0.3118(6) -0.3351(6) 0.034(3) Uani 1 1 d . . . C24 C -0.2845(11) 0.3535(7) -0.3639(7) 0.037(3) Uani 1 1 d . . . C25 C -0.1787(11) 0.2899(7) -0.3522(6) 0.035(3) Uani 1 1 d . . . C26 C -0.0555(10) 0.3001(6) -0.3278(6) 0.030(3) Uani 1 1 d . . . C27 C -0.0340(10) 0.3719(6) -0.3156(7) 0.034(3) Uani 1 1 d . . . C28 C -0.1383(11) 0.4324(6) -0.3263(6) 0.032(3) Uani 1 1 d . . . C29 C -0.2670(11) 0.4230(6) -0.3506(6) 0.033(3) Uani 1 1 d . . . C30 C -0.3065(12) 0.4823(6) -0.2586(7) 0.036(3) Uani 1 1 d . . . C31 C -0.1619(11) 0.4696(6) -0.2712(7) 0.038(3) Uani 1 1 d . . . C32 C -0.3711(12) 0.4542(6) -0.3106(6) 0.037(3) Uani 1 1 d . . . C33 C -0.4934(10) 0.4137(6) -0.2824(7) 0.036(3) Uani 1 1 d . . . C34 C -0.5542(10) 0.4021(6) -0.2057(7) 0.033(3) Uani 1 1 d . . . C35 C -0.4930(11) 0.4270(6) -0.1557(6) 0.034(3) Uani 1 1 d . . . C36 C -0.3650(11) 0.4699(6) -0.1858(7) 0.035(3) Uani 1 1 d . . . C37 C -0.2822(11) 0.4417(6) -0.1161(6) 0.029(3) Uani 1 1 d . . . C38 C -0.3561(11) 0.3855(6) -0.0454(6) 0.030(3) Uani 1 1 d . . . C39 C -0.2944(11) 0.3170(6) 0.0111(6) 0.029(3) Uani 1 1 d . . . C40 C -0.1488(10) 0.3021(6) -0.0003(6) 0.026(3) Uani 1 1 d . . . C41 C -0.0747(10) 0.3589(6) -0.0657(7) 0.031(3) Uani 1 1 d . . . C42 C -0.1419(11) 0.4294(6) -0.1243(7) 0.032(3) Uani 1 1 d . . . C43 C -0.0825(11) 0.4439(6) -0.2041(7) 0.032(3) Uani 1 1 d . . . C44 C 0.0248(10) 0.3824(6) -0.1935(7) 0.032(3) Uani 1 1 d . . . C45 C 0.0520(10) 0.3451(7) -0.2466(6) 0.030(3) Uani 1 1 d . . . C46 C 0.0791(9) 0.2552(7) -0.2155(7) 0.031(3) Uani 1 1 d . . . C47 C 0.0138(11) 0.2267(7) -0.2665(7) 0.037(3) Uani 1 1 d . . . C48 C 0.0832(10) 0.2068(6) -0.1357(6) 0.029(3) Uani 1 1 d . . . C49 C 0.0235(10) 0.1257(6) -0.0993(7) 0.029(3) Uani 1 1 d . . . C50 C -0.0376(10) 0.1125(6) -0.0210(6) 0.027(3) Uani 1 1 d . . . C51 C -0.0181(10) 0.1863(6) -0.0076(7) 0.032(3) Uani 1 1 d . . . C52 C 0.0542(9) 0.2443(7) -0.0792(6) 0.027(3) Uani 1 1 d . . . C53 C 0.0298(9) 0.3294(6) -0.1072(6) 0.027(3) Uani 1 1 d . . . C54 C -0.4915(10) 0.3761(6) -0.0712(7) 0.033(3) Uani 1 1 d . . . C55 C -0.5478(10) 0.2996(6) -0.0347(7) 0.029(3) Uani 1 1 d . . . C56 C -0.6053(9) 0.2714(6) -0.0873(7) 0.030(3) Uani 1 1 d . . . C57 C -0.6115(10) 0.3211(6) -0.1694(7) 0.035(3) Uani 1 1 d . . . C58 C -0.5525(10) 0.1482(6) -0.1120(7) 0.031(3) Uani 1 1 d . . . C59 C -0.5703(9) 0.1831(6) -0.0576(6) 0.028(3) Uani 1 1 d . . . C60 C -0.1177(9) 0.2157(6) 0.0300(6) 0.021(2) Uani 1 1 d . . . C61 C -0.6149(10) 0.1980(7) 0.1128(7) 0.035(3) Uani 1 1 d . . . C62 C -0.7580(10) 0.1999(7) 0.0836(8) 0.041(3) Uani 1 1 d . . . C63 C -0.5838(11) 0.1119(6) 0.1803(7) 0.036(3) Uani 1 1 d . . . C64 C -0.2041(10) 0.1406(6) 0.1701(7) 0.032(3) Uani 1 1 d . . . C65 C -0.0923(12) 0.0820(7) 0.2040(7) 0.031(3) Uani 1 1 d . . . C67 C -0.2775(10) 0.0121(7) 0.1425(8) 0.030(3) Uani 1 1 d . . . C69 C -0.2787(10) 0.1783(6) 0.2096(6) 0.026(2) Uani 1 1 d . . . C70 C -0.3713(10) 0.2413(6) 0.1543(7) 0.034(3) Uani 1 1 d . . . C71 C -0.4382(11) 0.3052(6) 0.1678(7) 0.035(3) Uani 1 1 d . . . C72 C -0.4386(10) 0.3150(6) 0.2406(8) 0.033(3) Uani 1 1 d . . . C74 C -0.5203(12) 0.3679(7) 0.1101(8) 0.036(3) Uani 1 1 d . . . C76 C -0.2707(11) 0.1580(6) 0.2961(7) 0.033(3) Uani 1 1 d . . . C77 C -0.3855(12) 0.1369(7) 0.3490(8) 0.042(3) Uani 1 1 d . . . C78 C -0.3836(12) 0.1130(7) 0.4301(7) 0.042(3) Uani 1 1 d . . . C79 C -0.2581(12) 0.1079(7) 0.4640(7) 0.043(3) Uani 1 1 d . . . C80 C -0.1417(12) 0.1282(7) 0.4100(8) 0.047(3) Uani 1 1 d . . . C81 C -0.1489(12) 0.1506(7) 0.3301(7) 0.041(3) Uani 1 1 d . . . C83 C -0.1202(15) 0.0690(11) 0.5817(9) 0.074(5) Uani 1 1 d . . . C84 C -0.3780(15) 0.0723(9) 0.5968(8) 0.062(4) Uani 1 1 d . . . C86 C 0.0194(13) 0.3619(7) 0.1894(9) 0.051(3) Uani 1 1 d . . . C87 C 0.0047(15) 0.3890(8) 0.1106(9) 0.058(4) Uani 1 1 d . . . C88 C -0.1071(15) 0.4424(10) 0.0777(11) 0.070(4) Uani 1 1 d . . . C89 C -0.1977(14) 0.4661(9) 0.1265(12) 0.068(5) Uani 1 1 d . . . C90 C -0.1735(17) 0.4354(11) 0.2080(12) 0.077(5) Uani 1 1 d . . . C91 C -0.0656(15) 0.3826(9) 0.2402(9) 0.058(4) Uani 1 1 d . . . C94 C -0.2209(11) 0.4661(6) 0.4462(8) 0.082(4) Uiso 1 1 d G . . C95 C -0.3259(10) 0.4234(9) 0.4396(10) 0.157(9) Uiso 1 1 d G . . C96 C -0.3008(15) 0.3442(9) 0.4428(12) 0.139(8) Uiso 1 1 d G . . C97 C -0.1707(17) 0.3078(7) 0.4526(12) 0.168(10) Uiso 1 1 d G . . C98 C -0.0656(12) 0.3506(8) 0.4592(10) 0.137(8) Uiso 1 1 d G . . C99 C -0.0907(10) 0.4298(7) 0.4560(8) 0.066(4) Uiso 1 1 d G . . C100 C 0.2592(14) 0.1638(7) 0.4702(8) 0.089(5) Uiso 1 1 d G . . C101 C 0.2993(14) 0.2449(7) 0.4424(7) 0.089(5) Uiso 1 1 d G . . C102 C 0.3148(18) 0.2779(7) 0.4967(10) 0.165(10) Uiso 1 1 d G . . C103 C 0.2902(19) 0.2299(10) 0.5788(9) 0.148(9) Uiso 1 1 d G . . C104 C 0.2501(18) 0.1489(10) 0.6066(7) 0.152(9) Uiso 1 1 d G . . C105 C 0.2346(16) 0.1158(7) 0.5523(8) 0.126(7) Uiso 1 1 d G . . H61 H -0.6195 0.2421 0.1387 0.07(4) Uiso 1 1 calc R . . H62A H -0.7593 0.1538 0.0605 0.05(3) Uiso 1 1 calc R . . H62B H -0.7815 0.2609 0.0366 0.04(3) Uiso 1 1 calc R . . H62C H -0.8321 0.1863 0.1335 0.03(2) Uiso 1 1 calc R . . H63A H -0.5936 0.0649 0.1593 0.05(3) Uiso 1 1 calc R . . H63B H -0.6539 0.1015 0.2316 0.09(4) Uiso 1 1 calc R . . H63C H -0.4821 0.1085 0.1978 0.07(4) Uiso 1 1 calc R . . H77 H -0.4722 0.1394 0.3268 0.051 Uiso 1 1 calc R . . H78 H -0.4673 0.0995 0.4644 0.09(5) Uiso 1 1 calc R . . H80 H -0.0538 0.1259 0.4310 0.04(3) Uiso 1 1 calc R . . H81 H -0.0655 0.1618 0.2955 0.06(4) Uiso 1 1 calc R . . H83A H -0.0580 0.0255 0.5652 0.08(4) Uiso 1 1 calc R . . H83B H -0.1373 0.0428 0.6465 0.07(4) Uiso 1 1 calc R . . H83C H -0.0696 0.1265 0.5609 0.10(5) Uiso 1 1 calc R . . H84A H -0.4472 0.1259 0.5716 0.14(7) Uiso 1 1 calc R . . H84B H -0.3540 0.0634 0.6560 0.08(4) Uiso 1 1 calc R . . H84C H -0.4243 0.0177 0.6014 0.09(4) Uiso 1 1 calc R . . H87 H 0.0702 0.3719 0.0769 0.07(4) Uiso 1 1 calc R . . H88 H -0.1213 0.4631 0.0202 0.16(9) Uiso 1 1 calc R . . H89 H -0.2766 0.5033 0.1043 0.12(6) Uiso 1 1 calc R . . H90 H -0.2359 0.4523 0.2430 0.04(3) Uiso 1 1 calc R . . H91 H -0.0500 0.3604 0.2976 0.07(4) Uiso 1 1 calc R . . H95 H -0.4177 0.4490 0.4328 0.188 Uiso 1 1 calc R . . H96 H -0.3749 0.3141 0.4382 0.167 Uiso 1 1 calc R . . H97 H -0.1530 0.2520 0.4549 0.202 Uiso 1 1 calc R . . H98 H 0.0261 0.3249 0.4661 0.165 Uiso 1 1 calc R . . H99 H -0.0166 0.4599 0.4606 0.079 Uiso 1 1 calc R . . H101 H 0.3166 0.2787 0.3845 0.107 Uiso 1 1 calc R . . H102 H 0.3431 0.3350 0.4771 0.198 Uiso 1 1 calc R . . H103 H 0.3012 0.2532 0.6171 0.177 Uiso 1 1 calc R . . H104 H 0.2328 0.1151 0.6645 0.183 Uiso 1 1 calc R . . H105 H 0.2064 0.0587 0.5720 0.151 Uiso 1 1 calc R . . 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 Cl85 0.061(2) 0.101(3) 0.069(3) -0.034(2) -0.007(2) 0.003(2) Cl92 0.070(3) 0.095(3) 0.163(5) -0.051(3) -0.006(3) 0.007(2) Cl93 0.134(5) 0.139(5) 0.089(4) 0.015(3) 0.017(3) 0.056(4) N66 0.046(7) 0.048(6) 0.039(6) -0.027(5) -0.013(5) 0.002(5) N68 0.048(6) 0.033(6) 0.021(6) -0.004(5) -0.002(5) -0.009(4) N73 0.065(8) 0.053(6) 0.050(7) -0.032(6) -0.007(6) 0.000(5) N75 0.053(7) 0.047(6) 0.049(7) -0.026(6) -0.006(6) 0.014(6) N82 0.071(8) 0.074(7) 0.045(8) -0.034(6) -0.013(7) 0.026(6) C1 0.044(7) 0.043(6) 0.018(6) -0.019(5) -0.008(5) 0.002(5) C2 0.029(6) 0.036(6) 0.020(6) -0.015(5) 0.004(5) -0.003(5) C3 0.022(6) 0.034(6) 0.029(7) -0.007(5) 0.003(5) -0.008(5) C4 0.022(6) 0.038(6) 0.032(7) -0.014(5) -0.001(5) -0.006(5) C5 0.017(6) 0.025(6) 0.024(6) -0.004(5) -0.002(5) -0.013(5) C6 0.018(6) 0.035(6) 0.042(7) -0.019(6) -0.010(5) -0.001(4) C7 0.026(7) 0.030(6) 0.038(7) -0.017(5) -0.008(5) 0.006(5) C8 0.031(7) 0.022(6) 0.037(8) -0.012(5) -0.006(6) 0.005(4) C9 0.034(7) 0.025(6) 0.028(7) -0.011(5) 0.004(6) -0.016(5) C10 0.019(6) 0.035(6) 0.042(8) -0.016(5) -0.007(6) -0.004(5) C11 0.040(8) 0.033(6) 0.020(7) -0.019(5) -0.007(5) -0.001(5) C12 0.032(7) 0.033(6) 0.041(8) -0.023(6) 0.005(6) -0.009(5) C13 0.021(6) 0.032(6) 0.035(8) -0.015(5) -0.009(6) 0.007(5) C14 0.029(7) 0.036(6) 0.040(8) -0.023(6) 0.002(5) 0.009(5) C15 0.023(6) 0.040(7) 0.019(7) -0.015(6) -0.003(5) -0.002(5) C16 0.036(7) 0.032(6) 0.031(7) -0.021(6) -0.001(6) 0.009(5) C17 0.041(8) 0.032(7) 0.029(7) -0.018(6) -0.003(6) 0.001(6) C18 0.039(7) 0.041(7) 0.017(7) -0.015(5) -0.014(6) 0.004(5) C19 0.023(6) 0.042(6) 0.021(7) -0.012(6) -0.009(5) -0.005(5) C20 0.020(6) 0.053(7) 0.011(6) -0.016(5) -0.008(5) -0.008(5) C22 0.029(7) 0.045(7) 0.029(7) -0.019(6) -0.026(5) 0.011(5) C23 0.043(8) 0.040(7) 0.022(6) -0.015(5) -0.005(5) -0.004(5) C24 0.035(7) 0.041(7) 0.029(7) -0.009(5) 0.006(5) -0.011(6) C25 0.036(8) 0.052(8) 0.021(6) -0.020(6) 0.000(5) 0.007(6) C26 0.014(6) 0.044(7) 0.024(7) -0.007(5) 0.008(5) -0.002(5) C27 0.026(7) 0.026(6) 0.042(8) -0.008(5) 0.012(6) -0.006(5) C28 0.033(7) 0.042(7) 0.017(6) -0.011(5) 0.005(5) -0.008(5) C29 0.048(8) 0.021(6) 0.019(6) 0.004(5) -0.006(6) -0.004(5) C30 0.055(9) 0.020(6) 0.023(7) 0.002(5) -0.008(6) -0.001(5) C31 0.027(7) 0.027(6) 0.051(9) -0.009(6) 0.006(6) -0.002(5) C32 0.052(8) 0.018(6) 0.028(7) 0.002(5) -0.021(6) 0.015(5) C33 0.016(6) 0.035(6) 0.048(9) -0.010(6) -0.008(6) 0.009(5) C34 0.022(6) 0.037(7) 0.037(8) -0.015(6) -0.008(6) 0.017(5) C35 0.043(7) 0.023(6) 0.024(7) -0.003(5) -0.008(6) 0.019(5) C36 0.034(7) 0.016(5) 0.048(9) -0.009(5) 0.002(6) 0.003(5) C37 0.038(8) 0.026(6) 0.026(7) -0.011(5) -0.010(6) -0.004(5) C38 0.045(7) 0.020(6) 0.024(7) -0.009(5) -0.008(6) 0.008(5) C39 0.039(7) 0.028(6) 0.018(6) -0.010(5) 0.013(5) -0.006(5) C40 0.020(6) 0.035(7) 0.025(7) -0.013(5) -0.011(5) -0.002(5) C41 0.028(6) 0.034(6) 0.039(7) -0.022(6) -0.005(6) -0.010(5) C42 0.026(7) 0.035(7) 0.038(8) -0.019(6) 0.001(6) -0.011(5) C43 0.034(7) 0.023(6) 0.038(8) -0.009(5) 0.001(6) -0.009(5) C44 0.028(6) 0.026(6) 0.032(8) -0.004(5) -0.006(5) -0.005(5) C45 0.015(6) 0.054(8) 0.017(6) -0.013(6) 0.001(5) -0.005(5) C46 0.010(6) 0.046(7) 0.045(8) -0.027(7) -0.002(5) -0.004(5) C47 0.038(7) 0.047(8) 0.026(7) -0.019(6) 0.008(6) 0.003(6) C48 0.016(6) 0.042(7) 0.020(7) -0.008(6) -0.003(5) 0.008(5) C49 0.022(6) 0.034(6) 0.037(7) -0.020(6) -0.008(5) 0.009(5) C50 0.027(7) 0.025(6) 0.027(7) -0.009(5) -0.013(5) 0.009(5) C51 0.020(6) 0.043(7) 0.031(7) -0.011(6) -0.012(5) -0.001(5) C52 0.007(5) 0.049(7) 0.033(7) -0.026(6) -0.009(5) 0.001(5) C53 0.006(5) 0.036(7) 0.036(7) -0.013(6) 0.000(5) -0.004(4) C54 0.027(7) 0.033(7) 0.045(8) -0.024(6) -0.007(5) 0.016(5) C55 0.021(6) 0.030(6) 0.043(7) -0.023(6) 0.005(5) 0.005(5) C56 0.012(6) 0.040(7) 0.037(8) -0.017(6) 0.002(5) -0.003(5) C57 0.024(6) 0.032(7) 0.039(8) -0.005(6) -0.007(5) 0.008(5) C58 0.013(6) 0.045(7) 0.047(8) -0.030(6) 0.000(5) -0.009(5) C59 0.009(6) 0.041(7) 0.037(7) -0.018(6) -0.001(5) -0.005(4) C60 0.011(5) 0.030(6) 0.023(6) -0.013(5) -0.001(5) -0.001(4) C61 0.026(6) 0.052(7) 0.034(7) -0.025(6) -0.006(5) 0.001(5) C62 0.014(6) 0.062(8) 0.047(8) -0.022(7) -0.007(5) -0.002(5) C63 0.037(7) 0.032(6) 0.039(7) -0.014(6) -0.001(6) -0.009(5) C64 0.028(6) 0.040(6) 0.032(7) -0.018(6) -0.006(5) -0.001(5) C65 0.026(7) 0.040(7) 0.031(7) -0.018(6) -0.007(6) 0.008(6) C67 0.023(6) 0.030(7) 0.044(9) -0.021(7) -0.010(6) 0.002(5) C69 0.019(6) 0.035(6) 0.022(7) -0.010(5) 0.000(5) -0.003(5) C70 0.026(6) 0.042(7) 0.039(8) -0.019(6) 0.001(6) -0.013(5) C71 0.033(7) 0.035(7) 0.051(8) -0.032(6) -0.006(6) 0.000(5) C72 0.031(7) 0.026(6) 0.046(8) -0.022(6) 0.000(6) -0.001(5) C74 0.034(7) 0.033(7) 0.043(8) -0.019(7) 0.000(7) 0.008(6) C76 0.032(7) 0.035(6) 0.029(7) -0.011(5) -0.002(6) 0.000(5) C77 0.042(8) 0.050(7) 0.045(9) -0.029(6) -0.008(7) -0.005(6) C78 0.039(8) 0.058(8) 0.030(8) -0.021(6) -0.002(6) 0.007(6) C79 0.043(8) 0.060(8) 0.028(8) -0.021(6) -0.012(7) 0.020(6) C80 0.041(8) 0.065(8) 0.054(10) -0.043(7) -0.025(7) 0.011(6) C81 0.032(8) 0.063(8) 0.040(8) -0.035(6) -0.010(6) 0.010(6) C83 0.067(10) 0.126(14) 0.047(9) -0.057(10) -0.036(8) 0.051(10) C84 0.083(11) 0.072(9) 0.023(8) -0.017(7) 0.012(7) 0.004(8) C86 0.049(8) 0.049(7) 0.064(11) -0.032(7) -0.012(7) 0.003(6) C87 0.066(10) 0.063(9) 0.055(11) -0.035(8) -0.013(8) 0.012(8) C88 0.065(10) 0.091(11) 0.086(13) -0.068(10) 0.000(9) -0.010(9) C89 0.047(9) 0.056(9) 0.119(16) -0.053(10) -0.008(10) 0.000(7) C90 0.057(11) 0.105(13) 0.086(14) -0.059(11) 0.015(10) -0.019(10) C91 0.060(10) 0.068(9) 0.044(10) -0.024(8) 0.015(8) -0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cl85 C86 1.759(14) . ? Cl92 C100 1.641(12) . ? Cl93 C94 1.667(12) . ? N66 C65 1.138(13) . ? N68 C67 1.145(13) . ? N73 C72 1.165(14) . ? N75 C74 1.145(15) . ? N82 C79 1.354(15) . ? N82 C84 1.486(17) . ? N82 C83 1.494(17) . ? C1 C64 1.519(15) . ? C1 C60 1.538(14) . ? C1 C6 1.613(14) . ? C1 C2 1.616(15) . ? C2 C39 1.540(14) . ? C2 C70 1.567(15) . ? C2 C3 1.608(14) . ? C3 C4 1.531(15) . ? C3 C55 1.547(15) . ? C3 C61 1.553(15) . ? C4 C5 1.350(14) . ? C4 C59 1.434(15) . ? C5 C9 1.451(14) . ? C5 C6 1.542(14) . ? C6 C67 1.505(18) . ? C6 C7 1.551(15) . ? C7 C50 1.384(14) . ? C7 C8 1.422(14) . ? C8 C13 1.378(15) . ? C8 C9 1.453(15) . ? C9 C10 1.376(15) . ? C10 C11 1.432(15) . ? C10 C58 1.455(15) . ? C11 C12 1.386(15) . ? C11 C19 1.484(15) . ? C12 C16 1.451(15) . ? C12 C13 1.466(15) . ? C13 C14 1.442(15) . ? C14 C49 1.410(15) . ? C14 C15 1.419(15) . ? C15 C47 1.360(14) . ? C15 C16 1.482(15) . ? C16 C17 1.369(15) . ? C17 C25 1.459(15) . ? C17 C18 1.465(15) . ? C18 C19 1.388(15) . ? C18 C23 1.448(14) . ? C19 C20 1.408(14) . ? C20 C21 1.396(14) . ? C20 C58 1.461(15) . ? C21 C22 1.420(15) . ? C21 C57 1.447(15) . ? C22 C23 1.394(15) . ? C22 C33 1.449(15) . ? C23 C24 1.476(15) . ? C24 C29 1.392(14) . ? C24 C25 1.439(16) . ? C25 C26 1.398(15) . ? C26 C27 1.429(14) . ? C26 C47 1.475(16) . ? C27 C28 1.394(15) . ? C27 C45 1.477(15) . ? C28 C31 1.431(15) . ? C28 C29 1.441(15) . ? C29 C32 1.432(16) . ? C30 C36 1.347(15) . ? C30 C31 1.453(16) . ? C30 C32 1.474(15) . ? C31 C43 1.411(16) . ? C32 C33 1.409(15) . ? C33 C34 1.424(16) . ? C34 C35 1.387(15) . ? C34 C57 1.447(15) . ? C35 C54 1.425(15) . ? C35 C36 1.480(15) . ? C36 C37 1.466(15) . ? C37 C42 1.402(14) . ? C37 C38 1.437(15) . ? C38 C39 1.357(15) . ? C38 C54 1.516(15) . ? C39 C40 1.466(14) . ? C40 C41 1.391(15) . ? C40 C60 1.410(13) . ? C41 C42 1.416(16) . ? C41 C53 1.436(14) . ? C42 C43 1.457(15) . ? C43 C44 1.427(15) . ? C44 C45 1.403(15) . ? C44 C53 1.460(15) . ? C45 C46 1.459(15) . ? C46 C48 1.348(15) . ? C46 C47 1.467(15) . ? C48 C49 1.459(14) . ? C48 C52 1.462(14) . ? C49 C50 1.444(15) . ? C50 C51 1.474(14) . ? C51 C60 1.359(14) . ? C51 C52 1.450(15) . ? C52 C53 1.382(14) . ? C54 C55 1.376(14) . ? C55 C56 1.448(14) . ? C56 C57 1.389(15) . ? C56 C59 1.449(14) . ? C58 C59 1.386(15) . ? C61 C63 1.528(16) . ? C61 C62 1.561(14) . ? C64 C69 1.334(14) . ? C64 C65 1.445(17) . ? C69 C70 1.468(15) . ? C69 C76 1.484(15) . ? C70 C71 1.377(15) . ? C71 C74 1.422(19) . ? C71 C72 1.427(18) . ? C76 C81 1.386(15) . ? C76 C77 1.398(16) . ? C77 C78 1.367(16) . ? C78 C79 1.427(17) . ? C79 C80 1.421(17) . ? C80 C81 1.356(16) . ? C86 C87 1.336(18) . ? C86 C91 1.354(18) . ? C87 C88 1.40(2) . ? C88 C89 1.39(2) . ? C89 C90 1.40(2) . ? C90 C91 1.36(2) . ? C94 C95 1.3900 . ? C94 C99 1.3900 . ? C95 C96 1.3900 . ? C96 C97 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.3900 . ? C100 C101 1.3900 . ? C100 C105 1.3900 . ? C101 C102 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C61 H61 1.0800 . ? C62 H62A 1.0800 . ? C62 H62B 1.0800 . ? C62 H62C 1.0800 . ? C63 H63A 1.0800 . ? C63 H63B 1.0800 . ? C63 H63C 1.0800 . ? C77 H77 0.9800 . ? C78 H78 0.9800 . ? C80 H80 0.9800 . ? C81 H81 0.9800 . ? C83 H83A 1.0800 . ? C83 H83B 1.0800 . ? C83 H83C 1.0800 . ? C84 H84A 1.0800 . ? C84 H84B 1.0800 . ? C84 H84C 1.0800 . ? C87 H87 0.9800 . ? C88 H88 0.9800 . ? C89 H89 0.9800 . ? C90 H90 0.9800 . ? C91 H91 0.9800 . ? C95 H95 0.9800 . ? C96 H96 0.9800 . ? C97 H97 0.9800 . ? C98 H98 0.9800 . ? C99 H99 0.9800 . ? C101 H101 0.9800 . ? C102 H102 0.9800 . ? C103 H103 0.9800 . ? C104 H104 0.9800 . ? C105 H105 0.9800 . ? 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 C79 N82 C84 120.5(11) . . ? C79 N82 C83 121.1(11) . . ? C84 N82 C83 118.2(11) . . ? C64 C1 C60 106.6(8) . . ? C64 C1 C6 111.8(8) . . ? C60 C1 C6 109.8(8) . . ? C64 C1 C2 103.6(8) . . ? C60 C1 C2 106.1(8) . . ? C6 C1 C2 118.2(8) . . ? C39 C2 C70 105.4(7) . . ? C39 C2 C3 113.0(8) . . ? C70 C2 C3 113.8(8) . . ? C39 C2 C1 101.5(8) . . ? C70 C2 C1 101.3(8) . . ? C3 C2 C1 120.1(7) . . ? C4 C3 C55 97.2(8) . . ? C4 C3 C61 107.2(7) . . ? C55 C3 C61 113.8(8) . . ? C4 C3 C2 111.3(8) . . ? C55 C3 C2 113.0(8) . . ? C61 C3 C2 113.0(8) . . ? C5 C4 C59 117.3(9) . . ? C5 C4 C3 128.3(9) . . ? C59 C4 C3 111.3(9) . . ? C4 C5 C9 121.4(9) . . ? C4 C5 C6 125.0(8) . . ? C9 C5 C6 108.9(9) . . ? C67 C6 C5 105.5(7) . . ? C67 C6 C7 108.8(8) . . ? C5 C6 C7 99.9(8) . . ? C67 C6 C1 110.5(8) . . ? C5 C6 C1 113.6(8) . . ? C7 C6 C1 117.5(8) . . ? C50 C7 C8 118.4(9) . . ? C50 C7 C6 122.3(8) . . ? C8 C7 C6 110.6(8) . . ? C13 C8 C7 121.8(9) . . ? C13 C8 C9 118.9(10) . . ? C7 C8 C9 108.2(9) . . ? C10 C9 C5 120.8(10) . . ? C10 C9 C8 120.5(9) . . ? C5 C9 C8 108.9(8) . . ? C9 C10 C11 121.0(9) . . ? C9 C10 C58 119.0(9) . . ? C11 C10 C58 108.4(9) . . ? C12 C11 C10 119.3(9) . . ? C12 C11 C19 121.2(9) . . ? C10 C11 C19 106.8(9) . . ? C11 C12 C16 119.2(10) . . ? C11 C12 C13 119.9(9) . . ? C16 C12 C13 108.3(9) . . ? C8 C13 C14 121.0(9) . . ? C8 C13 C12 120.2(9) . . ? C14 C13 C12 106.3(9) . . ? C49 C14 C15 119.6(9) . . ? C49 C14 C13 117.0(9) . . ? C15 C14 C13 111.1(9) . . ? C47 C15 C14 121.4(9) . . ? C47 C15 C16 119.1(9) . . ? C14 C15 C16 106.7(9) . . ? C17 C16 C12 120.4(10) . . ? C17 C16 C15 119.7(9) . . ? C12 C16 C15 107.6(9) . . ? C16 C17 C25 121.1(10) . . ? C16 C17 C18 121.1(9) . . ? C25 C17 C18 107.6(9) . . ? C19 C18 C23 118.8(9) . . ? C19 C18 C17 119.8(9) . . ? C23 C18 C17 107.9(8) . . ? C18 C19 C20 121.2(9) . . ? C18 C19 C11 118.3(9) . . ? C20 C19 C11 109.1(9) . . ? C21 C20 C19 120.3(9) . . ? C21 C20 C58 119.2(8) . . ? C19 C20 C58 107.9(9) . . ? C20 C21 C22 119.6(9) . . ? C20 C21 C57 119.6(10) . . ? C22 C21 C57 108.3(8) . . ? C23 C22 C21 120.4(9) . . ? C23 C22 C33 119.6(9) . . ? C21 C22 C33 107.7(9) . . ? C22 C23 C18 119.7(10) . . ? C22 C23 C24 120.7(9) . . ? C18 C23 C24 108.0(9) . . ? C29 C24 C25 121.7(10) . . ? C29 C24 C23 118.4(10) . . ? C25 C24 C23 107.6(9) . . ? C26 C25 C24 118.0(9) . . ? C26 C25 C17 119.8(10) . . ? C24 C25 C17 108.8(9) . . ? C25 C26 C27 121.3(9) . . ? C25 C26 C47 118.3(9) . . ? C27 C26 C47 109.1(9) . . ? C28 C27 C26 119.9(10) . . ? C28 C27 C45 120.2(9) . . ? C26 C27 C45 107.7(9) . . ? C27 C28 C31 120.3(10) . . ? C27 C28 C29 120.1(9) . . ? C31 C28 C29 108.3(9) . . ? C24 C29 C32 121.2(10) . . ? C24 C29 C28 119.0(10) . . ? C32 C29 C28 108.5(9) . . ? C36 C30 C31 122.2(10) . . ? C36 C30 C32 120.0(10) . . ? C31 C30 C32 106.4(9) . . ? C43 C31 C28 120.5(10) . . ? C43 C31 C30 117.7(10) . . ? C28 C31 C30 108.8(9) . . ? C33 C32 C29 120.2(9) . . ? C33 C32 C30 118.9(10) . . ? C29 C32 C30 108.0(10) . . ? C32 C33 C34 120.1(10) . . ? C32 C33 C22 119.8(10) . . ? C34 C33 C22 108.7(9) . . ? C35 C34 C33 121.4(10) . . ? C35 C34 C57 117.6(10) . . ? C33 C34 C57 107.5(9) . . ? C34 C35 C54 121.2(10) . . ? C34 C35 C36 118.2(10) . . ? C54 C35 C36 110.1(9) . . ? C30 C36 C37 119.9(10) . . ? C30 C36 C35 121.4(10) . . ? C37 C36 C35 106.2(9) . . ? C42 C37 C38 119.6(9) . . ? C42 C37 C36 120.9(9) . . ? C38 C37 C36 109.5(9) . . ? C39 C38 C37 121.4(10) . . ? C39 C38 C54 118.0(9) . . ? C37 C38 C54 107.4(9) . . ? C38 C39 C40 118.5(9) . . ? C38 C39 C2 126.9(10) . . ? C40 C39 C2 111.2(9) . . ? C41 C40 C60 121.5(9) . . ? C41 C40 C39 120.6(9) . . ? C60 C40 C39 109.4(8) . . ? C40 C41 C42 119.7(9) . . ? C40 C41 C53 119.6(9) . . ? C42 C41 C53 107.7(10) . . ? C37 C42 C41 120.0(9) . . ? C37 C42 C43 117.5(10) . . ? C41 C42 C43 109.1(9) . . ? C31 C43 C44 119.2(9) . . ? C31 C43 C42 121.9(10) . . ? C44 C43 C42 107.3(10) . . ? C45 C44 C43 122.0(10) . . ? C45 C44 C53 118.1(9) . . ? C43 C44 C53 107.6(9) . . ? C44 C45 C46 120.3(9) . . ? C44 C45 C27 117.8(9) . . ? C46 C45 C27 108.2(8) . . ? C48 C46 C45 121.1(9) . . ? C48 C46 C47 120.0(9) . . ? C45 C46 C47 107.7(9) . . ? C15 C47 C46 119.6(10) . . ? C15 C47 C26 121.9(10) . . ? C46 C47 C26 107.2(9) . . ? C46 C48 C49 120.6(9) . . ? C46 C48 C52 119.5(9) . . ? C49 C48 C52 107.1(9) . . ? C14 C49 C50 121.1(9) . . ? C14 C49 C48 118.8(10) . . ? C50 C49 C48 108.6(8) . . ? C7 C50 C49 120.4(9) . . ? C7 C50 C51 120.2(9) . . ? C49 C50 C51 108.3(8) . . ? C60 C51 C52 119.5(9) . . ? C60 C51 C50 120.3(9) . . ? C52 C51 C50 107.0(9) . . ? C53 C52 C51 121.4(9) . . ? C53 C52 C48 120.4(10) . . ? C51 C52 C48 109.1(8) . . ? C52 C53 C41 118.0(9) . . ? C52 C53 C44 120.5(9) . . ? C41 C53 C44 108.3(9) . . ? C55 C54 C35 122.5(9) . . ? C55 C54 C38 118.8(9) . . ? C35 C54 C38 106.7(9) . . ? C54 C55 C56 116.4(10) . . ? C54 C55 C3 126.3(9) . . ? C56 C55 C3 111.0(8) . . ? C57 C56 C55 121.8(9) . . ? C57 C56 C59 120.4(9) . . ? C55 C56 C59 106.9(9) . . ? C56 C57 C34 120.3(10) . . ? C56 C57 C21 120.6(9) . . ? C34 C57 C21 107.7(9) . . ? C59 C58 C10 117.5(10) . . ? C59 C58 C20 121.2(9) . . ? C10 C58 C20 107.8(9) . . ? C58 C59 C4 123.9(9) . . ? C58 C59 C56 118.8(10) . . ? C4 C59 C56 107.8(8) . . ? C51 C60 C40 119.7(9) . . ? C51 C60 C1 126.7(8) . . ? C40 C60 C1 109.7(8) . . ? C63 C61 C3 112.9(9) . . ? C63 C61 C62 109.0(9) . . ? C3 C61 C62 113.2(9) . . ? C69 C64 C65 123.4(10) . . ? C69 C64 C1 115.3(9) . . ? C65 C64 C1 121.2(9) . . ? N66 C65 C64 174.9(12) . . ? N68 C67 C6 177.7(10) . . ? C64 C69 C70 109.0(9) . . ? C64 C69 C76 125.1(9) . . ? C70 C69 C76 125.8(9) . . ? C71 C70 C69 124.6(10) . . ? C71 C70 C2 123.9(10) . . ? C69 C70 C2 110.5(8) . . ? C70 C71 C74 122.5(10) . . ? C70 C71 C72 125.0(10) . . ? C74 C71 C72 112.4(9) . . ? N73 C72 C71 169.6(11) . . ? N75 C74 C71 176.0(12) . . ? C81 C76 C77 116.5(11) . . ? C81 C76 C69 122.3(10) . . ? C77 C76 C69 120.9(10) . . ? C78 C77 C76 123.8(11) . . ? C77 C78 C79 119.1(11) . . ? N82 C79 C80 122.4(11) . . ? N82 C79 C78 120.9(11) . . ? C80 C79 C78 116.7(11) . . ? C81 C80 C79 121.8(11) . . ? C80 C81 C76 122.0(11) . . ? C87 C86 C91 125.0(13) . . ? C87 C86 Cl85 118.8(11) . . ? C91 C86 Cl85 116.2(12) . . ? C86 C87 C88 117.9(13) . . ? C89 C88 C87 119.9(17) . . ? C88 C89 C90 118.2(16) . . ? C91 C90 C89 121.8(15) . . ? C86 C91 C90 117.2(15) . . ? C95 C94 C99 120.0 . . ? C95 C94 Cl93 119.4(8) . . ? C99 C94 Cl93 120.5(8) . . ? C94 C95 C96 120.0 . . ? C97 C96 C95 120.0 . . ? C98 C97 C96 120.0 . . ? C97 C98 C99 120.0 . . ? C98 C99 C94 120.0 . . ? C101 C100 C105 120.0 . . ? C101 C100 Cl92 122.9(8) . . ? C105 C100 Cl92 117.0(8) . . ? C100 C101 C102 120.0 . . ? C103 C102 C101 120.0 . . ? C102 C103 C104 120.0 . . ? C105 C104 C103 120.0 . . ? C104 C105 C100 120.0 . . ? C63 C61 H61 107.2 . . ? C3 C61 H61 107.2 . . ? C62 C61 H61 107.2 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C78 C77 H77 118.1 . . ? C76 C77 H77 118.1 . . ? C77 C78 H78 120.4 . . ? C79 C78 H78 120.4 . . ? C81 C80 H80 119.1 . . ? C79 C80 H80 119.1 . . ? C80 C81 H81 119.0 . . ? C76 C81 H81 119.0 . . ? N82 C83 H83A 109.5 . . ? N82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N82 C84 H84A 109.5 . . ? N82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C87 H87 121.1 . . ? C88 C87 H87 121.1 . . ? C89 C88 H88 120.0 . . ? C87 C88 H88 120.0 . . ? C88 C89 H89 120.9 . . ? C90 C89 H89 120.9 . . ? C91 C90 H90 119.1 . . ? C89 C90 H90 119.1 . . ? C86 C91 H91 121.4 . . ? C90 C91 H91 121.4 . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C97 C96 H96 120.0 . . ? C95 C96 H96 120.0 . . ? C98 C97 H97 120.0 . . ? C96 C97 H97 120.0 . . ? C97 C98 H98 120.0 . . ? C99 C98 H98 120.0 . . ? C98 C99 H99 120.0 . . ? C94 C99 H99 120.0 . . ? C100 C101 H101 120.0 . . ? C102 C101 H101 120.0 . . ? C103 C102 H102 120.0 . . ? C101 C102 H102 120.0 . . ? C102 C103 H103 120.0 . . ? C104 C103 H103 120.0 . . ? C105 C104 H104 120.0 . . ? C103 C104 H104 120.0 . . ? C104 C105 H105 120.0 . . ? C100 C105 H105 120.0 . . ? 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 C64 C1 C2 C39 111.9(8) . . . . ? C60 C1 C2 C39 -0.1(9) . . . . ? C6 C1 C2 C39 -123.9(9) . . . . ? C64 C1 C2 C70 3.4(9) . . . . ? C60 C1 C2 C70 -108.6(8) . . . . ? C6 C1 C2 C70 127.7(9) . . . . ? C64 C1 C2 C3 -122.8(9) . . . . ? C60 C1 C2 C3 125.2(9) . . . . ? C6 C1 C2 C3 1.4(13) . . . . ? C39 C2 C3 C4 104.4(9) . . . . ? C70 C2 C3 C4 -135.6(9) . . . . ? C1 C2 C3 C4 -15.3(12) . . . . ? C39 C2 C3 C55 -3.8(11) . . . . ? C70 C2 C3 C55 116.2(9) . . . . ? C1 C2 C3 C55 -123.5(9) . . . . ? C39 C2 C3 C61 -134.9(8) . . . . ? C70 C2 C3 C61 -14.8(11) . . . . ? C1 C2 C3 C61 105.4(10) . . . . ? C55 C3 C4 C5 136.1(11) . . . . ? C61 C3 C4 C5 -106.2(12) . . . . ? C2 C3 C4 C5 17.9(14) . . . . ? C55 C3 C4 C59 -23.1(9) . . . . ? C61 C3 C4 C59 94.6(10) . . . . ? C2 C3 C4 C59 -141.3(8) . . . . ? C59 C4 C5 C9 1.1(13) . . . . ? C3 C4 C5 C9 -157.1(9) . . . . ? C59 C4 C5 C6 154.3(9) . . . . ? C3 C4 C5 C6 -3.9(17) . . . . ? C4 C5 C6 C67 108.9(11) . . . . ? C9 C5 C6 C67 -95.2(9) . . . . ? C4 C5 C6 C7 -138.3(10) . . . . ? C9 C5 C6 C7 17.6(9) . . . . ? C4 C5 C6 C1 -12.2(14) . . . . ? C9 C5 C6 C1 143.7(8) . . . . ? C64 C1 C6 C67 14.0(11) . . . . ? C60 C1 C6 C67 132.1(8) . . . . ? C2 C1 C6 C67 -106.1(10) . . . . ? C64 C1 C6 C5 132.3(9) . . . . ? C60 C1 C6 C5 -109.6(9) . . . . ? C2 C1 C6 C5 12.2(13) . . . . ? C64 C1 C6 C7 -111.5(10) . . . . ? C60 C1 C6 C7 6.5(12) . . . . ? C2 C1 C6 C7 128.4(9) . . . . ? C67 C6 C7 C50 -119.9(10) . . . . ? C5 C6 C7 C50 129.8(10) . . . . ? C1 C6 C7 C50 6.5(14) . . . . ? C67 C6 C7 C8 93.1(10) . . . . ? C5 C6 C7 C8 -17.2(10) . . . . ? C1 C6 C7 C8 -140.5(9) . . . . ? C50 C7 C8 C13 5.7(14) . . . . ? C6 C7 C8 C13 154.1(9) . . . . ? C50 C7 C8 C9 -137.8(9) . . . . ? C6 C7 C8 C9 10.6(11) . . . . ? C4 C5 C9 C10 -1.8(14) . . . . ? C6 C5 C9 C10 -158.8(9) . . . . ? C4 C5 C9 C8 144.2(9) . . . . ? C6 C5 C9 C8 -12.8(11) . . . . ? C13 C8 C9 C10 2.7(13) . . . . ? C7 C8 C9 C10 147.5(9) . . . . ? C13 C8 C9 C5 -143.4(9) . . . . ? C7 C8 C9 C5 1.4(11) . . . . ? C5 C9 C10 C11 139.6(9) . . . . ? C8 C9 C10 C11 -2.5(13) . . . . ? C5 C9 C10 C58 0.6(14) . . . . ? C8 C9 C10 C58 -141.5(9) . . . . ? C9 C10 C11 C12 0.8(14) . . . . ? C58 C10 C11 C12 143.6(9) . . . . ? C9 C10 C11 C19 -141.3(9) . . . . ? C58 C10 C11 C19 1.5(10) . . . . ? C10 C11 C12 C16 -136.8(9) . . . . ? C19 C11 C12 C16 -0.2(13) . . . . ? C10 C11 C12 C13 0.6(13) . . . . ? C19 C11 C12 C13 137.3(9) . . . . ? C7 C8 C13 C14 -4.2(15) . . . . ? C9 C8 C13 C14 135.6(10) . . . . ? C7 C8 C13 C12 -141.1(10) . . . . ? C9 C8 C13 C12 -1.3(13) . . . . ? C11 C12 C13 C8 -0.4(13) . . . . ? C16 C12 C13 C8 141.2(9) . . . . ? C11 C12 C13 C14 -142.8(9) . . . . ? C16 C12 C13 C14 -1.2(10) . . . . ? C8 C13 C14 C49 1.4(14) . . . . ? C12 C13 C14 C49 143.4(9) . . . . ? C8 C13 C14 C15 -140.8(9) . . . . ? C12 C13 C14 C15 1.3(11) . . . . ? C49 C14 C15 C47 -0.9(15) . . . . ? C13 C14 C15 C47 140.2(10) . . . . ? C49 C14 C15 C16 -141.9(9) . . . . ? C13 C14 C15 C16 -0.8(10) . . . . ? C11 C12 C16 C17 0.5(13) . . . . ? C13 C12 C16 C17 -141.4(9) . . . . ? C11 C12 C16 C15 142.6(9) . . . . ? C13 C12 C16 C15 0.7(10) . . . . ? C47 C15 C16 C17 0.3(14) . . . . ? C14 C15 C16 C17 142.5(9) . . . . ? C47 C15 C16 C12 -142.1(9) . . . . ? C14 C15 C16 C12 0.1(10) . . . . ? C12 C16 C17 C25 139.1(10) . . . . ? C15 C16 C17 C25 1.5(14) . . . . ? C12 C16 C17 C18 -1.7(14) . . . . ? C15 C16 C17 C18 -139.3(9) . . . . ? C16 C17 C18 C19 2.8(13) . . . . ? C25 C17 C18 C19 -142.7(9) . . . . ? C16 C17 C18 C23 143.0(9) . . . . ? C25 C17 C18 C23 -2.4(10) . . . . ? C23 C18 C19 C20 1.0(13) . . . . ? C17 C18 C19 C20 137.0(9) . . . . ? C23 C18 C19 C11 -138.4(9) . . . . ? C17 C18 C19 C11 -2.4(13) . . . . ? C12 C11 C19 C18 1.2(13) . . . . ? C10 C11 C19 C18 142.5(9) . . . . ? C12 C11 C19 C20 -142.7(8) . . . . ? C10 C11 C19 C20 -1.4(10) . . . . ? C18 C19 C20 C21 -0.5(13) . . . . ? C11 C19 C20 C21 142.2(9) . . . . ? C18 C19 C20 C58 -141.9(9) . . . . ? C11 C19 C20 C58 0.8(10) . . . . ? C19 C20 C21 C22 0.3(14) . . . . ? C58 C20 C21 C22 137.5(10) . . . . ? C19 C20 C21 C57 -137.3(10) . . . . ? C58 C20 C21 C57 -0.1(14) . . . . ? C20 C21 C22 C23 -0.6(14) . . . . ? C57 C21 C22 C23 141.2(9) . . . . ? C20 C21 C22 C33 -142.6(9) . . . . ? C57 C21 C22 C33 -0.8(11) . . . . ? C21 C22 C23 C18 1.1(14) . . . . ? C33 C22 C23 C18 138.7(10) . . . . ? C21 C22 C23 C24 -137.8(11) . . . . ? C33 C22 C23 C24 -0.2(15) . . . . ? C19 C18 C23 C22 -1.3(13) . . . . ? C17 C18 C23 C22 -142.0(9) . . . . ? C19 C18 C23 C24 142.3(9) . . . . ? C17 C18 C23 C24 1.6(11) . . . . ? C22 C23 C24 C29 0.0(16) . . . . ? C18 C23 C24 C29 -143.1(10) . . . . ? C22 C23 C24 C25 143.0(10) . . . . ? C18 C23 C24 C25 -0.1(11) . . . . ? C29 C24 C25 C26 -0.8(15) . . . . ? C23 C24 C25 C26 -142.3(10) . . . . ? C29 C24 C25 C17 140.1(10) . . . . ? C23 C24 C25 C17 -1.4(11) . . . . ? C16 C17 C25 C26 -3.0(14) . . . . ? C18 C17 C25 C26 142.5(9) . . . . ? C16 C17 C25 C24 -143.0(10) . . . . ? C18 C17 C25 C24 2.4(11) . . . . ? C24 C25 C26 C27 -0.7(15) . . . . ? C17 C25 C26 C27 -137.2(10) . . . . ? C24 C25 C26 C47 139.0(10) . . . . ? C17 C25 C26 C47 2.5(14) . . . . ? C25 C26 C27 C28 1.5(15) . . . . ? C47 C26 C27 C28 -141.5(10) . . . . ? C25 C26 C27 C45 143.9(10) . . . . ? C47 C26 C27 C45 1.0(11) . . . . ? C26 C27 C28 C31 138.5(10) . . . . ? C45 C27 C28 C31 0.7(14) . . . . ? C26 C27 C28 C29 -0.7(15) . . . . ? C45 C27 C28 C29 -138.5(10) . . . . ? C25 C24 C29 C32 -138.0(11) . . . . ? C23 C24 C29 C32 -0.4(16) . . . . ? C25 C24 C29 C28 1.5(15) . . . . ? C23 C24 C29 C28 139.1(10) . . . . ? C27 C28 C29 C24 -0.7(15) . . . . ? C31 C28 C29 C24 -144.3(10) . . . . ? C27 C28 C29 C32 143.5(10) . . . . ? C31 C28 C29 C32 -0.1(12) . . . . ? C27 C28 C31 C43 -1.9(14) . . . . ? C29 C28 C31 C43 141.6(9) . . . . ? C27 C28 C31 C30 -142.1(10) . . . . ? C29 C28 C31 C30 1.4(12) . . . . ? C36 C30 C31 C43 -0.4(14) . . . . ? C32 C30 C31 C43 -143.6(9) . . . . ? C36 C30 C31 C28 141.2(10) . . . . ? C32 C30 C31 C28 -2.0(11) . . . . ? C24 C29 C32 C33 1.1(15) . . . . ? C28 C29 C32 C33 -142.2(10) . . . . ? C24 C29 C32 C30 142.1(10) . . . . ? C28 C29 C32 C30 -1.1(11) . . . . ? C36 C30 C32 C33 -0.6(14) . . . . ? C31 C30 C32 C33 143.6(9) . . . . ? C36 C30 C32 C29 -142.2(10) . . . . ? C31 C30 C32 C29 1.9(11) . . . . ? C29 C32 C33 C34 138.2(10) . . . . ? C30 C32 C33 C34 1.3(14) . . . . ? C29 C32 C33 C22 -1.3(15) . . . . ? C30 C32 C33 C22 -138.2(10) . . . . ? C23 C22 C33 C32 0.9(16) . . . . ? C21 C22 C33 C32 143.2(10) . . . . ? C23 C22 C33 C34 -142.7(10) . . . . ? C21 C22 C33 C34 -0.4(11) . . . . ? C32 C33 C34 C35 -2.5(15) . . . . ? C22 C33 C34 C35 141.0(9) . . . . ? C32 C33 C34 C57 -142.1(9) . . . . ? C22 C33 C34 C57 1.4(11) . . . . ? C33 C34 C35 C54 -138.3(10) . . . . ? C57 C34 C35 C54 -2.5(14) . . . . ? C33 C34 C35 C36 2.9(14) . . . . ? C57 C34 C35 C36 138.7(10) . . . . ? C31 C30 C36 C37 -0.7(13) . . . . ? C32 C30 C36 C37 137.7(9) . . . . ? C31 C30 C36 C35 -137.4(10) . . . . ? C32 C30 C36 C35 1.1(15) . . . . ? C34 C35 C36 C30 -2.2(14) . . . . ? C54 C35 C36 C30 143.0(10) . . . . ? C34 C35 C36 C37 -143.9(9) . . . . ? C54 C35 C36 C37 1.3(10) . . . . ? C30 C36 C37 C42 1.6(13) . . . . ? C35 C36 C37 C42 144.0(9) . . . . ? C30 C36 C37 C38 -143.7(9) . . . . ? C35 C36 C37 C38 -1.3(10) . . . . ? C42 C37 C38 C39 -4.8(14) . . . . ? C36 C37 C38 C39 141.1(10) . . . . ? C42 C37 C38 C54 -144.9(8) . . . . ? C36 C37 C38 C54 0.9(10) . . . . ? C37 C38 C39 C40 1.3(14) . . . . ? C54 C38 C39 C40 137.5(9) . . . . ? C37 C38 C39 C2 -155.9(9) . . . . ? C54 C38 C39 C2 -19.7(15) . . . . ? C70 C2 C39 C38 -104.7(11) . . . . ? C3 C2 C39 C38 20.1(13) . . . . ? C1 C2 C39 C38 150.0(10) . . . . ? C70 C2 C39 C40 96.8(9) . . . . ? C3 C2 C39 C40 -138.4(8) . . . . ? C1 C2 C39 C40 -8.5(9) . . . . ? C38 C39 C40 C41 3.0(13) . . . . ? C2 C39 C40 C41 163.5(8) . . . . ? C38 C39 C40 C60 -145.6(9) . . . . ? C2 C39 C40 C60 15.0(11) . . . . ? C60 C40 C41 C42 141.0(9) . . . . ? C39 C40 C41 C42 -3.7(13) . . . . ? C60 C40 C41 C53 4.4(14) . . . . ? C39 C40 C41 C53 -140.3(9) . . . . ? C38 C37 C42 C41 4.0(13) . . . . ? C36 C37 C42 C41 -138.0(10) . . . . ? C38 C37 C42 C43 140.6(9) . . . . ? C36 C37 C42 C43 -1.3(13) . . . . ? C40 C41 C42 C37 0.2(14) . . . . ? C53 C41 C42 C37 141.4(9) . . . . ? C40 C41 C42 C43 -139.6(9) . . . . ? C53 C41 C42 C43 1.5(11) . . . . ? C28 C31 C43 C44 2.3(14) . . . . ? C30 C31 C43 C44 139.2(10) . . . . ? C28 C31 C43 C42 -136.3(10) . . . . ? C30 C31 C43 C42 0.6(13) . . . . ? C37 C42 C43 C31 0.2(13) . . . . ? C41 C42 C43 C31 141.2(9) . . . . ? C37 C42 C43 C44 -142.5(9) . . . . ? C41 C42 C43 C44 -1.5(11) . . . . ? C31 C43 C44 C45 -1.6(14) . . . . ? C42 C43 C44 C45 142.3(9) . . . . ? C31 C43 C44 C53 -143.0(9) . . . . ? C42 C43 C44 C53 0.9(10) . . . . ? C43 C44 C45 C46 -135.3(10) . . . . ? C53 C44 C45 C46 2.4(13) . . . . ? C43 C44 C45 C27 0.5(14) . . . . ? C53 C44 C45 C27 138.1(9) . . . . ? C28 C27 C45 C44 -0.1(14) . . . . ? C26 C27 C45 C44 -142.4(9) . . . . ? C28 C27 C45 C46 140.6(9) . . . . ? C26 C27 C45 C46 -1.7(11) . . . . ? C44 C45 C46 C48 -2.3(14) . . . . ? C27 C45 C46 C48 -141.8(9) . . . . ? C44 C45 C46 C47 141.2(10) . . . . ? C27 C45 C46 C47 1.8(11) . . . . ? C14 C15 C47 C46 1.8(15) . . . . ? C16 C15 C47 C46 138.3(10) . . . . ? C14 C15 C47 C26 -137.2(10) . . . . ? C16 C15 C47 C26 -0.7(14) . . . . ? C48 C46 C47 C15 -1.5(15) . . . . ? C45 C46 C47 C15 -145.5(10) . . . . ? C48 C46 C47 C26 142.9(10) . . . . ? C45 C46 C47 C26 -1.2(11) . . . . ? C25 C26 C47 C15 -0.7(15) . . . . ? C27 C26 C47 C15 143.5(9) . . . . ? C25 C26 C47 C46 -144.1(9) . . . . ? C27 C26 C47 C46 0.1(11) . . . . ? C45 C46 C48 C49 139.4(9) . . . . ? C47 C46 C48 C49 0.2(14) . . . . ? C45 C46 C48 C52 2.7(14) . . . . ? C47 C46 C48 C52 -136.5(10) . . . . ? C15 C14 C49 C50 138.6(10) . . . . ? C13 C14 C49 C50 -0.2(14) . . . . ? C15 C14 C49 C48 -0.5(14) . . . . ? C13 C14 C49 C48 -139.3(10) . . . . ? C46 C48 C49 C14 0.8(14) . . . . ? C52 C48 C49 C14 142.1(9) . . . . ? C46 C48 C49 C50 -142.9(10) . . . . ? C52 C48 C49 C50 -1.6(11) . . . . ? C8 C7 C50 C49 -4.4(14) . . . . ? C6 C7 C50 C49 -149.0(9) . . . . ? C8 C7 C50 C51 135.3(10) . . . . ? C6 C7 C50 C51 -9.3(15) . . . . ? C14 C49 C50 C7 1.9(14) . . . . ? C48 C49 C50 C7 144.6(9) . . . . ? C14 C49 C50 C51 -142.1(9) . . . . ? C48 C49 C50 C51 0.7(11) . . . . ? C7 C50 C51 C60 -2.7(15) . . . . ? C49 C50 C51 C60 141.4(10) . . . . ? C7 C50 C51 C52 -143.5(9) . . . . ? C49 C50 C51 C52 0.6(11) . . . . ? C60 C51 C52 C53 4.1(13) . . . . ? C50 C51 C52 C53 145.3(9) . . . . ? C60 C51 C52 C48 -142.8(9) . . . . ? C50 C51 C52 C48 -1.6(11) . . . . ? C46 C48 C52 C53 -3.5(14) . . . . ? C49 C48 C52 C53 -145.3(9) . . . . ? C46 C48 C52 C51 143.8(9) . . . . ? C49 C48 C52 C51 2.0(11) . . . . ? C51 C52 C53 C41 -3.2(13) . . . . ? C48 C52 C53 C41 140.0(9) . . . . ? C51 C52 C53 C44 -139.6(9) . . . . ? C48 C52 C53 C44 3.6(13) . . . . ? C40 C41 C53 C52 -1.0(13) . . . . ? C42 C41 C53 C52 -142.1(9) . . . . ? C40 C41 C53 C44 140.3(9) . . . . ? C42 C41 C53 C44 -0.9(10) . . . . ? C45 C44 C53 C52 -3.1(14) . . . . ? C43 C44 C53 C52 140.1(9) . . . . ? C45 C44 C53 C41 -143.2(9) . . . . ? C43 C44 C53 C41 0.0(10) . . . . ? C34 C35 C54 C55 1.1(15) . . . . ? C36 C35 C54 C55 -142.8(9) . . . . ? C34 C35 C54 C38 143.2(9) . . . . ? C36 C35 C54 C38 -0.7(10) . . . . ? C39 C38 C54 C55 1.9(14) . . . . ? C37 C38 C54 C55 143.7(9) . . . . ? C39 C38 C54 C35 -141.9(9) . . . . ? C37 C38 C54 C35 -0.1(10) . . . . ? C35 C54 C55 C56 2.2(13) . . . . ? C38 C54 C55 C56 -135.6(9) . . . . ? C35 C54 C55 C3 151.8(10) . . . . ? C38 C54 C55 C3 13.9(14) . . . . ? C4 C3 C55 C54 -128.9(10) . . . . ? C61 C3 C55 C54 118.7(10) . . . . ? C2 C3 C55 C54 -12.0(13) . . . . ? C4 C3 C55 C56 22.0(9) . . . . ? C61 C3 C55 C56 -90.4(9) . . . . ? C2 C3 C55 C56 138.9(8) . . . . ? C54 C55 C56 C57 -4.2(14) . . . . ? C3 C55 C56 C57 -158.3(9) . . . . ? C54 C55 C56 C59 140.0(9) . . . . ? C3 C55 C56 C59 -14.0(11) . . . . ? C55 C56 C57 C34 2.9(15) . . . . ? C59 C56 C57 C34 -136.7(10) . . . . ? C55 C56 C57 C21 142.0(10) . . . . ? C59 C56 C57 C21 2.4(15) . . . . ? C35 C34 C57 C56 0.5(14) . . . . ? C33 C34 C57 C56 141.9(10) . . . . ? C35 C34 C57 C21 -143.2(10) . . . . ? C33 C34 C57 C21 -1.8(12) . . . . ? C20 C21 C57 C56 -0.1(15) . . . . ? C22 C21 C57 C56 -142.0(10) . . . . ? C20 C21 C57 C34 143.5(9) . . . . ? C22 C21 C57 C34 1.6(12) . . . . ? C9 C10 C58 C59 1.2(14) . . . . ? C11 C10 C58 C59 -142.5(9) . . . . ? C9 C10 C58 C20 142.6(9) . . . . ? C11 C10 C58 C20 -1.0(10) . . . . ? C21 C20 C58 C59 -2.1(14) . . . . ? C19 C20 C58 C59 139.9(9) . . . . ? C21 C20 C58 C10 -141.8(9) . . . . ? C19 C20 C58 C10 0.2(10) . . . . ? C10 C58 C59 C4 -1.9(14) . . . . ? C20 C58 C59 C4 -138.0(10) . . . . ? C10 C58 C59 C56 140.3(10) . . . . ? C20 C58 C59 C56 4.3(13) . . . . ? C5 C4 C59 C58 0.8(14) . . . . ? C3 C4 C59 C58 162.5(9) . . . . ? C5 C4 C59 C56 -144.9(9) . . . . ? C3 C4 C59 C56 16.8(11) . . . . ? C57 C56 C59 C58 -4.5(13) . . . . ? C55 C56 C59 C58 -149.3(8) . . . . ? C57 C56 C59 C4 143.3(9) . . . . ? C55 C56 C59 C4 -1.6(11) . . . . ? C52 C51 C60 C40 -0.7(13) . . . . ? C50 C51 C60 C40 -136.7(9) . . . . ? C52 C51 C60 C1 154.8(9) . . . . ? C50 C51 C60 C1 18.8(16) . . . . ? C41 C40 C60 C51 -3.6(13) . . . . ? C39 C40 C60 C51 144.6(9) . . . . ? C41 C40 C60 C1 -162.9(9) . . . . ? C39 C40 C60 C1 -14.8(11) . . . . ? C64 C1 C60 C51 101.6(11) . . . . ? C6 C1 C60 C51 -19.7(14) . . . . ? C2 C1 C60 C51 -148.5(10) . . . . ? C64 C1 C60 C40 -100.9(9) . . . . ? C6 C1 C60 C40 137.9(8) . . . . ? C2 C1 C60 C40 9.0(10) . . . . ? C4 C3 C61 C63 58.5(11) . . . . ? C55 C3 C61 C63 164.7(8) . . . . ? C2 C3 C61 C63 -64.6(10) . . . . ? C4 C3 C61 C62 -65.9(11) . . . . ? C55 C3 C61 C62 40.3(11) . . . . ? C2 C3 C61 C62 171.0(8) . . . . ? C60 C1 C64 C69 111.2(10) . . . . ? C6 C1 C64 C69 -128.8(9) . . . . ? C2 C1 C64 C69 -0.4(11) . . . . ? C60 C1 C64 C65 -64.7(11) . . . . ? C6 C1 C64 C65 55.3(12) . . . . ? C2 C1 C64 C65 -176.3(9) . . . . ? C69 C64 C65 N66 -122(12) . . . . ? C1 C64 C65 N66 53(12) . . . . ? C65 C64 C69 C70 172.7(9) . . . . ? C1 C64 C69 C70 -3.2(12) . . . . ? C65 C64 C69 C76 -8.5(16) . . . . ? C1 C64 C69 C76 175.7(8) . . . . ? C64 C69 C70 C71 -163.0(10) . . . . ? C76 C69 C70 C71 18.1(15) . . . . ? C64 C69 C70 C2 5.6(11) . . . . ? C76 C69 C70 C2 -173.2(8) . . . . ? C39 C2 C70 C71 57.9(12) . . . . ? C3 C2 C70 C71 -66.4(12) . . . . ? C1 C2 C70 C71 163.3(9) . . . . ? C39 C2 C70 C69 -110.8(9) . . . . ? C3 C2 C70 C69 124.9(8) . . . . ? C1 C2 C70 C69 -5.4(10) . . . . ? C69 C70 C71 C74 176.0(9) . . . . ? C2 C70 C71 C74 8.8(15) . . . . ? C69 C70 C71 C72 -6.7(16) . . . . ? C2 C70 C71 C72 -173.8(9) . . . . ? C74 C71 C72 N73 -1(6) . . . . ? C70 C71 C74 N75 164(17) . . . . ? C72 C71 C74 N75 -14(18) . . . . ? C64 C69 C76 C81 48.7(14) . . . . ? C70 C69 C76 C81 -132.7(11) . . . . ? C64 C69 C76 C77 -124.5(11) . . . . ? C70 C69 C76 C77 54.2(14) . . . . ? C81 C76 C77 C78 2.6(15) . . . . ? C69 C76 C77 C78 176.1(9) . . . . ? C76 C77 C78 C79 -0.8(16) . . . . ? C84 N82 C79 C80 174.6(11) . . . . ? C83 N82 C79 C80 -9.3(17) . . . . ? C84 N82 C79 C78 -4.5(16) . . . . ? C83 N82 C79 C78 171.5(12) . . . . ? C77 C78 C79 N82 178.9(10) . . . . ? C77 C78 C79 C80 -0.3(15) . . . . ? N82 C79 C80 C81 -179.7(10) . . . . ? C78 C79 C80 C81 -0.5(16) . . . . ? C79 C80 C81 C76 2.5(16) . . . . ? C77 C76 C81 C80 -3.4(15) . . . . ? C69 C76 C81 C80 -176.8(10) . . . . ? C91 C86 C87 C88 -0.3(19) . . . . ? Cl85 C86 C87 C88 179.9(9) . . . . ? C86 C87 C88 C89 0.5(19) . . . . ? C87 C88 C89 C90 0.2(19) . . . . ? C88 C89 C90 C91 -1(2) . . . . ? C87 C86 C91 C90 -0.5(19) . . . . ? Cl85 C86 C91 C90 179.3(10) . . . . ? C89 C90 C91 C86 1(2) . . . . ? C99 C94 C95 C96 0.0 . . . . ? Cl93 C94 C95 C96 -176.8(11) . . . . ? C94 C95 C96 C97 0.0 . . . . ? C95 C96 C97 C98 0.0 . . . . ? C96 C97 C98 C99 0.0 . . . . ? C97 C98 C99 C94 0.0 . . . . ? C95 C94 C99 C98 0.0 . . . . ? Cl93 C94 C99 C98 176.8(11) . . . . ? C105 C100 C101 C102 0.0 . . . . ? Cl92 C100 C101 C102 -178.3(12) . . . . ? C100 C101 C102 C103 0.0 . . . . ? C101 C102 C103 C104 0.0 . . . . ? C102 C103 C104 C105 0.0 . . . . ? C103 C104 C105 C100 0.0 . . . . ? C101 C100 C105 C104 0.0 . . . . ? Cl92 C100 C105 C104 178.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.924 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.084 _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ;