# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' #TrackingRef '- 891817.cif' _journal_coden_cambridge 1475 #send to: deposit@ccdc.cam.ac.uk _publ_contact_author ; Stephen J. Loeb Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; _publ_contact_author_phone '+ 519 253-3000 ext 3529' _publ_contact_author_fax '+ 519 973-7098 ' _publ_contact_author_email loeb@uwindsor.ca _publ_requested_coeditor_name ? _publ_contact_letter ; This structure is part of a study on a new type templating motif for preparing [2]rotaxane moelcular shuttles with rigid compact structures. ; _publ_section_title ; Bis(benzimidazolium) axles and crown ether wheels: a versatile templating pair for the formation of [2]rotaxane molecular shuttles ; loop_ _publ_author_address ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; _publ_contact_author_name 'Stephen J. Loeb' _publ_author_name S.J.Loeb data_kz35 _database_code_depnum_ccdc_archive 'CCDC 891917' #TrackingRef '- 891817.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H74 B F4 N3 O8' _chemical_formula_weight 1136.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.2420(13) _cell_length_b 18.9077(16) _cell_length_c 19.5236(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.3180(10) _cell_angle_gamma 90.00 _cell_volume 5978.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 642 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9822 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56650 _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10527 _reflns_number_gt 5789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The BF4- anion was disordered with SOF of 1/3 and 2/3. Each PART was treated as a rigid group with SADI, DELU and SIMU 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^)+(0.1143P)^2^+3.9213P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10527 _refine_ls_number_parameters 794 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.1417 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2443 _refine_ls_wR_factor_gt 0.1953 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _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 N1 N 0.06917(19) 0.30427(15) 0.12967(15) 0.0340(7) Uani 1 1 d . . . H1A H 0.0214 0.2974 0.1063 0.041 Uiso 1 1 calc R . . N2 N 0.19395(19) 0.34005(16) 0.15575(16) 0.0372(8) Uani 1 1 d . . . H2A H 0.2425 0.3598 0.1521 0.045 Uiso 1 1 calc R . . C1 C -0.3322(3) 0.1179(4) 0.2388(3) 0.090(2) Uani 1 1 d . . . H1B H -0.3017 0.0732 0.2390 0.136 Uiso 1 1 calc R . . H1C H -0.3913 0.1086 0.2290 0.136 Uiso 1 1 calc R . . H1D H -0.3230 0.1407 0.2837 0.136 Uiso 1 1 calc R . . C2 C -0.3489(3) 0.2362(3) 0.1858(4) 0.096(2) Uani 1 1 d . . . H2B H -0.3298 0.2680 0.1507 0.144 Uiso 1 1 calc R . . H2C H -0.3387 0.2579 0.2312 0.144 Uiso 1 1 calc R . . H2D H -0.4082 0.2275 0.1766 0.144 Uiso 1 1 calc R . . C3 C -0.3223(3) 0.1341(4) 0.1134(3) 0.096(2) Uani 1 1 d . . . H3A H -0.2926 0.0892 0.1100 0.144 Uiso 1 1 calc R . . H3B H -0.3053 0.1668 0.0782 0.144 Uiso 1 1 calc R . . H3C H -0.3818 0.1255 0.1065 0.144 Uiso 1 1 calc R . . C4 C -0.3022(3) 0.1660(3) 0.1840(2) 0.0539(12) Uani 1 1 d . . . C5 C -0.2104(2) 0.1811(2) 0.1989(2) 0.0392(10) Uani 1 1 d . . . C6 C -0.1517(3) 0.1683(2) 0.1520(2) 0.0443(10) Uani 1 1 d . . . H6A H -0.1685 0.1459 0.1097 0.053 Uiso 1 1 calc R . . C7 C -0.0698(2) 0.1868(2) 0.16501(19) 0.0383(9) Uani 1 1 d . . . H7A H -0.0317 0.1773 0.1315 0.046 Uiso 1 1 calc R . . C8 C -0.0422(2) 0.21934(19) 0.22653(19) 0.0344(9) Uani 1 1 d . . . C9 C -0.1003(2) 0.2302(2) 0.2744(2) 0.0389(9) Uani 1 1 d . . . H9A H -0.0832 0.2510 0.3174 0.047 Uiso 1 1 calc R . . C10 C -0.1813(2) 0.2116(2) 0.2612(2) 0.0417(10) Uani 1 1 d . . . H10A H -0.2189 0.2196 0.2954 0.050 Uiso 1 1 calc R . . C11 C 0.0439(2) 0.24374(19) 0.24194(19) 0.0360(9) Uani 1 1 d . . . C12 C 0.0887(2) 0.2822(2) 0.19652(19) 0.0355(9) Uani 1 1 d . . . C13 C 0.1686(2) 0.3069(2) 0.21396(19) 0.0364(9) Uani 1 1 d . . . C14 C 0.2091(2) 0.2975(2) 0.2790(2) 0.0430(10) Uani 1 1 d . . . C15 C 0.1645(2) 0.2582(2) 0.3237(2) 0.0471(11) Uani 1 1 d . . . H15A H 0.1889 0.2487 0.3685 0.056 Uiso 1 1 calc R . . C16 C 0.0857(2) 0.2321(2) 0.3056(2) 0.0442(10) Uani 1 1 d . . . H16A H 0.0592 0.2050 0.3385 0.053 Uiso 1 1 calc R . . C17 C 0.2911(2) 0.3270(2) 0.3002(2) 0.0451(10) Uani 1 1 d . . . C18 C 0.3145(2) 0.3940(2) 0.2790(2) 0.0488(11) Uani 1 1 d . . . H18A H 0.2769 0.4215 0.2505 0.059 Uiso 1 1 calc R . . C19 C 0.3915(3) 0.4210(3) 0.2990(2) 0.0554(12) Uani 1 1 d . . . H19A H 0.4054 0.4668 0.2837 0.067 Uiso 1 1 calc R . . C20 C 0.4488(3) 0.3841(3) 0.3402(2) 0.0568(12) Uani 1 1 d . . . C21 C 0.4252(3) 0.3171(3) 0.3612(2) 0.0621(13) Uani 1 1 d . . . H21A H 0.4631 0.2899 0.3897 0.075 Uiso 1 1 calc R . . C22 C 0.3489(3) 0.2893(3) 0.3422(2) 0.0548(12) Uani 1 1 d . . . H22A H 0.3352 0.2436 0.3580 0.066 Uiso 1 1 calc R . . C23 C 0.5352(3) 0.4142(3) 0.3583(3) 0.0730(16) Uani 1 1 d . . . C24 C 0.5861(4) 0.4010(6) 0.2986(5) 0.166(4) Uani 1 1 d . . . H24A H 0.5928 0.3500 0.2924 0.249 Uiso 1 1 calc R . . H24B H 0.6405 0.4230 0.3075 0.249 Uiso 1 1 calc R . . H24C H 0.5583 0.4214 0.2569 0.249 Uiso 1 1 calc R . . C25 C 0.5337(4) 0.4931(5) 0.3608(6) 0.163(4) Uani 1 1 d . . . H25A H 0.5010 0.5085 0.3982 0.244 Uiso 1 1 calc R . . H25B H 0.5089 0.5115 0.3171 0.244 Uiso 1 1 calc R . . H25C H 0.5903 0.5110 0.3687 0.244 Uiso 1 1 calc R . . C26 C 0.5723(5) 0.3875(6) 0.4246(5) 0.221(7) Uani 1 1 d . . . H26A H 0.5720 0.3356 0.4242 0.331 Uiso 1 1 calc R . . H26B H 0.5403 0.4045 0.4619 0.331 Uiso 1 1 calc R . . H26C H 0.6293 0.4045 0.4319 0.331 Uiso 1 1 calc R . . C27 C 0.1331(2) 0.33727(19) 0.10625(19) 0.0341(9) Uani 1 1 d . . . C28 C 0.1370(2) 0.36681(19) 0.03727(19) 0.0344(9) Uani 1 1 d . . . C29 C 0.0744(2) 0.4103(2) 0.0097(2) 0.0396(10) Uani 1 1 d . . . H29A H 0.0281 0.4202 0.0351 0.048 Uiso 1 1 calc R . . C30 C 0.0797(3) 0.4392(2) -0.0547(2) 0.0441(10) Uani 1 1 d . . . H30A H 0.0367 0.4688 -0.0740 0.053 Uiso 1 1 calc R . . C31 C 0.1471(3) 0.4253(2) -0.0908(2) 0.0466(11) Uani 1 1 d . . . H31A H 0.1505 0.4456 -0.1350 0.056 Uiso 1 1 calc R . . C32 C 0.2099(3) 0.3823(2) -0.0638(2) 0.0483(11) Uani 1 1 d . . . H32A H 0.2564 0.3731 -0.0892 0.058 Uiso 1 1 calc R . . C33 C 0.2048(2) 0.3528(2) 0.0002(2) 0.0427(10) Uani 1 1 d . . . H33A H 0.2477 0.3229 0.0190 0.051 Uiso 1 1 calc R . . O1 O 0.21604(18) 0.17934(16) 0.09979(17) 0.0582(8) Uani 1 1 d . . . O2 O 0.0392(2) 0.19301(18) 0.02412(16) 0.0689(10) Uani 1 1 d . . . O3 O -0.07165(16) 0.30172(15) 0.03284(13) 0.0447(7) Uani 1 1 d . . . O4 O -0.08101(15) 0.40189(13) 0.13717(13) 0.0396(7) Uani 1 1 d . . . O5 O 0.04658(16) 0.47331(14) 0.18505(13) 0.0423(7) Uani 1 1 d . . . O6 O 0.22165(17) 0.49846(14) 0.14440(14) 0.0463(7) Uani 1 1 d . . . O7 O 0.34136(17) 0.40339(16) 0.10984(16) 0.0553(8) Uani 1 1 d . . . O8 O 0.34701(19) 0.25634(17) 0.1241(2) 0.0756(11) Uani 1 1 d . . . C34 C 0.3408(3) 0.1999(2) 0.1673(3) 0.0607(13) Uani 1 1 d . . . C35 C 0.3966(3) 0.1832(2) 0.2201(3) 0.0642(14) Uani 1 1 d . . . H35A H 0.4455 0.2106 0.2273 0.077 Uiso 1 1 calc R . . C36 C 0.3838(3) 0.1262(2) 0.2643(3) 0.0550(12) Uani 1 1 d . . . C37 C 0.4391(3) 0.1096(3) 0.3218(3) 0.0677(14) Uani 1 1 d . . . H37A H 0.4870 0.1378 0.3315 0.081 Uiso 1 1 calc R . . C38 C 0.4244(3) 0.0532(3) 0.3635(3) 0.0669(14) Uani 1 1 d . . . H38A H 0.4619 0.0430 0.4020 0.080 Uiso 1 1 calc R . . C39 C 0.3552(3) 0.0112(3) 0.3498(3) 0.0670(14) Uani 1 1 d . . . H39A H 0.3458 -0.0280 0.3786 0.080 Uiso 1 1 calc R . . C40 C 0.3006(3) 0.0260(2) 0.2952(3) 0.0578(12) Uani 1 1 d . . . H40A H 0.2536 -0.0034 0.2862 0.069 Uiso 1 1 calc R . . C41 C 0.3125(3) 0.0838(2) 0.2520(2) 0.0494(11) Uani 1 1 d . . . C42 C 0.2556(3) 0.1017(2) 0.1959(2) 0.0493(11) Uani 1 1 d . . . H42A H 0.2077 0.0733 0.1868 0.059 Uiso 1 1 calc R . . C43 C 0.2678(3) 0.1584(2) 0.1549(3) 0.0515(11) Uani 1 1 d . . . C44 C 0.1531(3) 0.1299(2) 0.0773(2) 0.0574(12) Uani 1 1 d . . . H44A H 0.1121 0.1260 0.1122 0.069 Uiso 1 1 calc R . . H44B H 0.1778 0.0826 0.0713 0.069 Uiso 1 1 calc R . . C45 C 0.1117(3) 0.1546(3) 0.0107(3) 0.0691(14) Uani 1 1 d . . . H45A H 0.1496 0.1854 -0.0133 0.083 Uiso 1 1 calc R . . H45B H 0.0969 0.1135 -0.0192 0.083 Uiso 1 1 calc R . . C46 C -0.0022(3) 0.2201(3) -0.0342(2) 0.0649(14) Uani 1 1 d . . . H46A H -0.0130 0.1814 -0.0678 0.078 Uiso 1 1 calc R . . H46B H 0.0338 0.2551 -0.0551 0.078 Uiso 1 1 calc R . . C47 C -0.0799(3) 0.2539(3) -0.0216(2) 0.0704(15) Uani 1 1 d . . . H47A H -0.1014 0.2791 -0.0637 0.085 Uiso 1 1 calc R . . H47B H -0.1206 0.2171 -0.0113 0.085 Uiso 1 1 calc R . . C48 C -0.1407(3) 0.3478(2) 0.0361(2) 0.0482(11) Uani 1 1 d . . . H48A H -0.1908 0.3251 0.0141 0.058 Uiso 1 1 calc R . . H48B H -0.1308 0.3922 0.0111 0.058 Uiso 1 1 calc R . . C49 C -0.1529(2) 0.3639(2) 0.1091(2) 0.0449(10) Uani 1 1 d . . . H49A H -0.2031 0.3931 0.1123 0.054 Uiso 1 1 calc R . . H49B H -0.1597 0.3195 0.1350 0.054 Uiso 1 1 calc R . . C50 C -0.0788(2) 0.41611(19) 0.2063(2) 0.0363(9) Uani 1 1 d . . . C51 C -0.1369(2) 0.3962(2) 0.2482(2) 0.0403(10) Uani 1 1 d . . . H51A H -0.1837 0.3704 0.2300 0.048 Uiso 1 1 calc R . . C52 C -0.1290(2) 0.4134(2) 0.3191(2) 0.0408(10) Uani 1 1 d . . . C53 C -0.1878(3) 0.3910(2) 0.3648(2) 0.0505(11) Uani 1 1 d . . . H53A H -0.2335 0.3632 0.3478 0.061 Uiso 1 1 calc R . . C54 C -0.1800(3) 0.4085(3) 0.4323(2) 0.0551(12) Uani 1 1 d . . . H54A H -0.2203 0.3936 0.4620 0.066 Uiso 1 1 calc R . . C55 C -0.1125(3) 0.4485(3) 0.4575(2) 0.0630(13) Uani 1 1 d . . . H55A H -0.1071 0.4609 0.5048 0.076 Uiso 1 1 calc R . . C56 C -0.0539(3) 0.4703(3) 0.4156(2) 0.0554(12) Uani 1 1 d . . . H56A H -0.0080 0.4971 0.4341 0.066 Uiso 1 1 calc R . . C57 C -0.0608(2) 0.4533(2) 0.3451(2) 0.0420(10) Uani 1 1 d . . . C58 C -0.0006(3) 0.4747(2) 0.3000(2) 0.0447(10) Uani 1 1 d . . . H58A H 0.0457 0.5017 0.3174 0.054 Uiso 1 1 calc R . . C59 C -0.0083(2) 0.4567(2) 0.2322(2) 0.0386(9) Uani 1 1 d . . . C60 C 0.1049(3) 0.5280(2) 0.2050(2) 0.0455(10) Uani 1 1 d . . . H60A H 0.1422 0.5120 0.2444 0.055 Uiso 1 1 calc R . . H60B H 0.0756 0.5709 0.2190 0.055 Uiso 1 1 calc R . . C61 C 0.1536(3) 0.5442(2) 0.1452(2) 0.0441(10) Uani 1 1 d . . . H61A H 0.1181 0.5389 0.1021 0.053 Uiso 1 1 calc R . . H61B H 0.1731 0.5938 0.1482 0.053 Uiso 1 1 calc R . . C62 C 0.2694(3) 0.5130(2) 0.0880(2) 0.0517(11) Uani 1 1 d . . . H62A H 0.2769 0.5648 0.0835 0.062 Uiso 1 1 calc R . . H62B H 0.2403 0.4954 0.0450 0.062 Uiso 1 1 calc R . . C63 C 0.3514(3) 0.4781(2) 0.0988(3) 0.0593(13) Uani 1 1 d . . . H63A H 0.3832 0.4857 0.0582 0.071 Uiso 1 1 calc R . . H63B H 0.3828 0.4992 0.1392 0.071 Uiso 1 1 calc R . . C64 C 0.4115(3) 0.3634(3) 0.0949(3) 0.0795(17) Uani 1 1 d . . . H64A H 0.4617 0.3929 0.1024 0.095 Uiso 1 1 calc R . . H64B H 0.4063 0.3487 0.0461 0.095 Uiso 1 1 calc R . . C65 C 0.4195(3) 0.3017(3) 0.1381(4) 0.091(2) Uani 1 1 d . . . H65A H 0.4240 0.3161 0.1870 0.109 Uiso 1 1 calc R . . H65B H 0.4702 0.2754 0.1287 0.109 Uiso 1 1 calc R . . B1A B 0.6202(7) 0.1845(6) 0.4828(6) 0.114(4) Uani 0.67 1 d PDU A -1 F1A F 0.6839(4) 0.2329(5) 0.4818(6) 0.165(3) Uani 0.67 1 d PDU A -1 F2A F 0.6503(7) 0.1315(5) 0.5233(5) 0.146(3) Uani 0.67 1 d PDU A -1 F3A F 0.6028(7) 0.1591(8) 0.4191(5) 0.191(6) Uani 0.67 1 d PDU A -1 F4A F 0.5522(6) 0.2153(5) 0.5063(6) 0.106(3) Uani 0.67 1 d PDU A -1 B1B B 0.6087(11) 0.1641(9) 0.4858(9) 0.103(7) Uani 0.33 1 d PDU B -2 F1B F 0.5719(8) 0.1012(6) 0.4907(8) 0.133(5) Uani 0.33 1 d PDU B -2 F2B F 0.6617(10) 0.1724(11) 0.5422(9) 0.151(8) Uani 0.33 1 d PDU B -2 F3B F 0.6500(15) 0.1742(11) 0.4293(11) 0.179(9) Uani 0.33 1 d PDU B -2 F4B F 0.5522(14) 0.2172(10) 0.4818(16) 0.173(12) Uani 0.33 1 d PDU B -2 N1S N 0.1859(5) 0.4739(4) 0.3993(4) 0.134(2) Uani 1 1 d . . . C1S C 0.2455(6) 0.4544(5) 0.4344(4) 0.108(3) Uani 1 1 d . . . C2S C 0.3151(5) 0.4285(4) 0.4765(4) 0.114(3) Uani 1 1 d . . . H1SA H 0.3139 0.3767 0.4772 0.172 Uiso 1 1 calc R . . H1SB H 0.3128 0.4466 0.5234 0.172 Uiso 1 1 calc R . . H1SC H 0.3662 0.4446 0.4578 0.172 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 N1 0.0323(17) 0.0366(18) 0.0319(17) 0.0037(14) -0.0059(14) -0.0010(14) N2 0.0293(17) 0.0399(19) 0.0415(19) 0.0072(15) -0.0035(15) -0.0028(14) C1 0.046(3) 0.122(5) 0.102(5) 0.035(4) -0.006(3) -0.028(3) C2 0.049(3) 0.097(5) 0.139(6) 0.011(4) -0.017(3) 0.026(3) C3 0.047(3) 0.155(6) 0.082(4) -0.025(4) -0.013(3) -0.023(3) C4 0.037(2) 0.064(3) 0.060(3) 0.010(2) -0.005(2) 0.000(2) C5 0.029(2) 0.046(2) 0.042(2) 0.0108(19) -0.0031(18) -0.0001(18) C6 0.047(3) 0.046(2) 0.038(2) 0.0008(19) -0.008(2) -0.005(2) C7 0.040(2) 0.041(2) 0.035(2) -0.0002(18) 0.0035(18) -0.0011(18) C8 0.039(2) 0.030(2) 0.034(2) 0.0060(16) 0.0014(18) -0.0002(17) C9 0.039(2) 0.042(2) 0.035(2) 0.0038(18) 0.0006(18) 0.0023(18) C10 0.041(2) 0.045(2) 0.040(2) 0.0068(19) 0.0070(19) 0.0042(19) C11 0.038(2) 0.032(2) 0.038(2) 0.0012(17) -0.0003(18) -0.0006(17) C12 0.037(2) 0.034(2) 0.034(2) 0.0048(17) -0.0029(17) 0.0040(17) C13 0.031(2) 0.039(2) 0.039(2) 0.0085(18) 0.0001(17) -0.0002(17) C14 0.035(2) 0.046(2) 0.046(2) 0.008(2) -0.0081(19) 0.0009(19) C15 0.042(2) 0.057(3) 0.041(2) 0.009(2) -0.0097(19) -0.002(2) C16 0.040(2) 0.053(3) 0.039(2) 0.0113(19) -0.0021(19) -0.006(2) C17 0.038(2) 0.054(3) 0.042(2) 0.007(2) -0.0085(19) -0.003(2) C18 0.037(2) 0.053(3) 0.054(3) 0.008(2) -0.013(2) -0.004(2) C19 0.045(3) 0.064(3) 0.056(3) 0.004(2) -0.003(2) -0.012(2) C20 0.035(2) 0.076(4) 0.058(3) 0.003(3) -0.009(2) -0.003(2) C21 0.040(3) 0.079(4) 0.064(3) 0.009(3) -0.020(2) 0.004(2) C22 0.044(3) 0.058(3) 0.059(3) 0.016(2) -0.012(2) 0.001(2) C23 0.033(3) 0.096(4) 0.088(4) -0.002(3) -0.014(3) -0.007(3) C24 0.060(4) 0.289(13) 0.152(8) -0.060(8) 0.025(5) -0.045(6) C25 0.078(5) 0.126(7) 0.273(12) -0.012(7) -0.062(6) -0.041(5) C26 0.131(7) 0.276(13) 0.231(11) 0.163(10) -0.139(8) -0.131(8) C27 0.036(2) 0.032(2) 0.035(2) 0.0054(17) 0.0036(18) 0.0037(17) C28 0.037(2) 0.033(2) 0.033(2) 0.0033(17) 0.0028(17) -0.0024(17) C29 0.041(2) 0.040(2) 0.037(2) 0.0007(18) -0.0001(18) -0.0032(18) C30 0.049(3) 0.041(2) 0.041(2) 0.0052(19) -0.004(2) 0.002(2) C31 0.058(3) 0.050(3) 0.032(2) 0.0022(19) 0.005(2) -0.006(2) C32 0.054(3) 0.049(3) 0.043(3) -0.001(2) 0.013(2) -0.004(2) C33 0.039(2) 0.040(2) 0.049(3) -0.0022(19) 0.004(2) -0.0007(19) O1 0.0470(18) 0.0502(19) 0.077(2) 0.0048(16) 0.0025(16) 0.0051(15) O2 0.072(2) 0.075(2) 0.058(2) -0.0178(17) -0.0083(17) 0.0229(19) O3 0.0427(16) 0.0546(18) 0.0354(15) -0.0104(13) -0.0059(12) -0.0012(14) O4 0.0388(15) 0.0414(16) 0.0371(15) -0.0036(12) -0.0067(12) -0.0030(12) O5 0.0431(16) 0.0421(16) 0.0410(16) -0.0023(13) -0.0016(13) -0.0089(13) O6 0.0467(17) 0.0475(17) 0.0445(17) 0.0074(13) 0.0022(13) -0.0029(14) O7 0.0371(16) 0.056(2) 0.073(2) 0.0140(16) 0.0051(15) -0.0023(14) O8 0.0411(18) 0.056(2) 0.130(3) 0.033(2) 0.0084(19) 0.0044(16) C34 0.035(2) 0.046(3) 0.101(4) 0.016(3) 0.009(3) 0.006(2) C35 0.033(2) 0.044(3) 0.115(4) 0.011(3) 0.002(3) -0.003(2) C36 0.034(2) 0.045(3) 0.086(4) -0.002(2) 0.004(2) 0.009(2) C37 0.045(3) 0.053(3) 0.104(4) -0.002(3) 0.000(3) 0.007(2) C38 0.053(3) 0.069(4) 0.078(4) -0.001(3) -0.001(3) 0.020(3) C39 0.058(3) 0.066(3) 0.079(4) 0.010(3) 0.013(3) 0.009(3) C40 0.051(3) 0.052(3) 0.071(3) -0.006(3) 0.010(3) 0.001(2) C41 0.042(2) 0.040(3) 0.068(3) -0.004(2) 0.014(2) 0.008(2) C42 0.035(2) 0.045(3) 0.069(3) -0.009(2) 0.007(2) -0.003(2) C43 0.035(2) 0.041(3) 0.079(3) -0.005(2) 0.008(2) 0.008(2) C44 0.057(3) 0.047(3) 0.069(3) -0.007(2) 0.004(2) 0.009(2) C45 0.071(3) 0.069(3) 0.067(3) -0.010(3) 0.007(3) 0.020(3) C46 0.092(4) 0.071(3) 0.032(2) -0.007(2) 0.002(3) 0.014(3) C47 0.085(4) 0.065(3) 0.057(3) -0.028(3) -0.021(3) 0.017(3) C48 0.046(3) 0.050(3) 0.046(3) -0.008(2) -0.016(2) 0.002(2) C49 0.037(2) 0.044(2) 0.052(3) -0.008(2) -0.0085(19) -0.0003(19) C50 0.037(2) 0.033(2) 0.038(2) -0.0027(17) -0.0075(18) 0.0038(17) C51 0.033(2) 0.039(2) 0.048(3) -0.0040(19) -0.0037(19) 0.0027(18) C52 0.038(2) 0.042(2) 0.043(2) 0.0003(19) -0.0002(19) 0.0069(19) C53 0.039(2) 0.057(3) 0.054(3) -0.002(2) 0.000(2) 0.004(2) C54 0.049(3) 0.065(3) 0.052(3) 0.006(2) 0.007(2) 0.007(2) C55 0.071(3) 0.078(4) 0.039(3) 0.000(2) 0.001(2) -0.001(3) C56 0.059(3) 0.066(3) 0.039(3) -0.004(2) -0.005(2) -0.009(2) C57 0.039(2) 0.042(2) 0.044(2) 0.0031(19) -0.0031(19) 0.0022(19) C58 0.046(2) 0.045(2) 0.041(2) -0.0018(19) -0.007(2) -0.009(2) C59 0.037(2) 0.036(2) 0.043(2) 0.0007(18) -0.0023(19) -0.0003(18) C60 0.047(2) 0.041(2) 0.049(3) -0.009(2) -0.001(2) -0.013(2) C61 0.045(2) 0.035(2) 0.051(3) 0.0025(19) 0.000(2) -0.0023(19) C62 0.057(3) 0.046(3) 0.053(3) 0.007(2) 0.008(2) -0.008(2) C63 0.052(3) 0.052(3) 0.076(3) 0.004(2) 0.014(2) -0.015(2) C64 0.045(3) 0.060(3) 0.137(5) 0.015(3) 0.025(3) 0.003(3) C65 0.028(3) 0.074(4) 0.171(6) 0.042(4) 0.010(3) 0.001(3) B1A 0.094(8) 0.098(9) 0.140(11) -0.064(7) -0.063(9) 0.049(6) F1A 0.088(4) 0.169(7) 0.231(9) 0.030(7) -0.021(5) 0.028(4) F2A 0.159(9) 0.127(7) 0.148(7) 0.004(6) -0.011(6) 0.056(6) F3A 0.159(8) 0.275(13) 0.126(6) -0.101(7) -0.069(6) 0.099(8) F4A 0.105(6) 0.085(5) 0.133(6) -0.014(4) 0.035(5) 0.014(4) B1B 0.14(2) 0.070(11) 0.085(13) -0.046(14) -0.046(10) 0.046(9) F1B 0.121(10) 0.093(7) 0.180(13) -0.072(8) -0.032(9) 0.027(7) F2B 0.095(10) 0.193(19) 0.152(12) -0.063(14) -0.071(9) 0.021(11) F3B 0.25(3) 0.152(17) 0.139(12) 0.035(13) 0.016(15) 0.118(15) F4B 0.135(16) 0.137(12) 0.24(3) 0.035(16) -0.026(13) 0.090(13) N1S 0.105(5) 0.164(7) 0.137(6) -0.004(5) 0.028(5) -0.014(5) C1S 0.085(5) 0.136(7) 0.108(6) -0.029(5) 0.039(5) -0.032(5) C2S 0.092(5) 0.168(7) 0.089(5) -0.025(5) 0.043(4) -0.044(5) _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 N1 C27 1.322(5) . ? N1 C12 1.384(4) . ? N1 H1A 0.8800 . ? N2 C27 1.330(5) . ? N2 C13 1.387(5) . ? N2 H2A 0.8800 . ? C1 C4 1.512(7) . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 C4 1.529(7) . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.517(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.525(5) . ? C5 C6 1.392(6) . ? C5 C10 1.396(5) . ? C6 C7 1.381(5) . ? C6 H6A 0.9500 . ? C7 C8 1.393(5) . ? C7 H7A 0.9500 . ? C8 C9 1.392(5) . ? C8 C11 1.482(5) . ? C9 C10 1.368(5) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C16 1.388(5) . ? C11 C12 1.394(5) . ? C12 C13 1.397(5) . ? C13 C14 1.396(5) . ? C14 C15 1.390(6) . ? C14 C17 1.475(5) . ? C15 C16 1.392(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C22 1.394(5) . ? C17 C18 1.395(6) . ? C18 C19 1.379(6) . ? C18 H18A 0.9500 . ? C19 C20 1.374(6) . ? C19 H19A 0.9500 . ? C20 C21 1.394(7) . ? C20 C23 1.530(6) . ? C21 C22 1.371(6) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C26 1.477(9) . ? C23 C25 1.492(9) . ? C23 C24 1.499(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.464(5) . ? C28 C29 1.383(5) . ? C28 C33 1.389(5) . ? C29 C30 1.380(5) . ? C29 H29A 0.9500 . ? C30 C31 1.371(6) . ? C30 H30A 0.9500 . ? C31 C32 1.378(6) . ? C31 H31A 0.9500 . ? C32 C33 1.377(6) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? O1 C43 1.373(5) . ? O1 C44 1.430(5) . ? O2 C46 1.377(5) . ? O2 C45 1.424(5) . ? O3 C47 1.394(5) . ? O3 C48 1.425(5) . ? O4 C50 1.375(4) . ? O4 C49 1.444(4) . ? O5 C59 1.366(5) . ? O5 C60 1.437(4) . ? O6 C61 1.405(5) . ? O6 C62 1.422(5) . ? O7 C64 1.416(6) . ? O7 C63 1.439(5) . ? O8 C34 1.368(5) . ? O8 C65 1.466(6) . ? C34 C35 1.358(7) . ? C34 C43 1.427(6) . ? C35 C36 1.406(7) . ? C35 H35A 0.9500 . ? C36 C41 1.415(6) . ? C36 C37 1.418(7) . ? C37 C38 1.373(7) . ? C37 H37A 0.9500 . ? C38 C39 1.386(7) . ? C38 H38A 0.9500 . ? C39 C40 1.363(7) . ? C39 H39A 0.9500 . ? C40 C41 1.403(6) . ? C40 H40A 0.9500 . ? C41 C42 1.419(6) . ? C42 C43 1.363(6) . ? C42 H42A 0.9500 . ? C44 C45 1.494(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.452(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.485(6) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.347(5) . ? C50 C59 1.438(5) . ? C51 C52 1.418(5) . ? C51 H51A 0.9500 . ? C52 C57 1.403(5) . ? C52 C53 1.420(6) . ? C53 C54 1.354(6) . ? C53 H53A 0.9500 . ? C54 C55 1.392(6) . ? C54 H54A 0.9500 . ? C55 C56 1.364(6) . ? C55 H55A 0.9500 . ? C56 C57 1.410(6) . ? C56 H56A 0.9500 . ? C57 C58 1.423(6) . ? C58 C59 1.363(5) . ? C58 H58A 0.9500 . ? C60 C61 1.490(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.487(6) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.438(7) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? B1A F3A 1.343(12) . ? B1A F2A 1.346(11) . ? B1A F4A 1.359(11) . ? B1A F1A 1.382(12) . ? B1B F1B 1.338(15) . ? B1B F3B 1.348(15) . ? B1B F4B 1.357(15) . ? B1B F2B 1.355(15) . ? N1S C1S 1.201(10) . ? C1S C2S 1.433(11) . ? C2S H1SA 0.9800 . ? C2S H1SB 0.9800 . ? C2S H1SC 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 C27 N1 C12 109.7(3) . . ? C27 N1 H1A 125.1 . . ? C12 N1 H1A 125.1 . . ? C27 N2 C13 109.1(3) . . ? C27 N2 H2A 125.5 . . ? C13 N2 H2A 125.5 . . ? C4 C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C4 C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 C3 110.1(5) . . ? C1 C4 C5 109.9(4) . . ? C3 C4 C5 112.8(4) . . ? C1 C4 C2 108.6(5) . . ? C3 C4 C2 107.1(5) . . ? C5 C4 C2 108.2(4) . . ? C6 C5 C10 116.2(4) . . ? C6 C5 C4 123.4(4) . . ? C10 C5 C4 120.3(4) . . ? C7 C6 C5 122.2(4) . . ? C7 C6 H6A 118.9 . . ? C5 C6 H6A 118.9 . . ? C6 C7 C8 120.9(4) . . ? C6 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C9 C8 C7 117.0(4) . . ? C9 C8 C11 119.6(3) . . ? C7 C8 C11 123.3(3) . . ? C10 C9 C8 121.7(4) . . ? C10 C9 H9A 119.1 . . ? C8 C9 H9A 119.1 . . ? C9 C10 C5 121.9(4) . . ? C9 C10 H10A 119.1 . . ? C5 C10 H10A 119.1 . . ? C16 C11 C12 114.1(3) . . ? C16 C11 C8 121.5(3) . . ? C12 C11 C8 124.3(3) . . ? N1 C12 C11 131.6(3) . . ? N1 C12 C13 105.8(3) . . ? C11 C12 C13 122.7(3) . . ? N2 C13 C14 130.8(3) . . ? N2 C13 C12 106.2(3) . . ? C14 C13 C12 123.0(4) . . ? C15 C14 C13 114.0(3) . . ? C15 C14 C17 121.8(4) . . ? C13 C14 C17 124.1(4) . . ? C16 C15 C14 122.8(4) . . ? C16 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? C11 C16 C15 123.3(4) . . ? C11 C16 H16A 118.3 . . ? C15 C16 H16A 118.3 . . ? C22 C17 C18 116.9(4) . . ? C22 C17 C14 121.8(4) . . ? C18 C17 C14 121.3(4) . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C20 C19 C18 122.6(4) . . ? C20 C19 H19A 118.7 . . ? C18 C19 H19A 118.7 . . ? C19 C20 C21 116.3(4) . . ? C19 C20 C23 121.1(5) . . ? C21 C20 C23 122.5(4) . . ? C22 C21 C20 122.1(4) . . ? C22 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? C21 C22 C17 121.2(4) . . ? C21 C22 H22A 119.4 . . ? C17 C22 H22A 119.4 . . ? C26 C23 C25 108.7(7) . . ? C26 C23 C24 114.4(7) . . ? C25 C23 C24 101.7(7) . . ? C26 C23 C20 112.4(5) . . ? C25 C23 C20 111.2(5) . . ? C24 C23 C20 107.9(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 C27 N2 109.1(3) . . ? N1 C27 C28 126.0(3) . . ? N2 C27 C28 124.9(3) . . ? C29 C28 C33 119.9(4) . . ? C29 C28 C27 120.2(3) . . ? C33 C28 C27 119.8(3) . . ? C30 C29 C28 119.7(4) . . ? C30 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? C31 C30 C29 120.0(4) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.9(4) . . ? C30 C31 H31A 119.6 . . ? C32 C31 H31A 119.6 . . ? C33 C32 C31 119.5(4) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C32 C33 C28 120.0(4) . . ? C32 C33 H33A 120.0 . . ? C28 C33 H33A 120.0 . . ? C43 O1 C44 115.7(3) . . ? C46 O2 C45 113.3(4) . . ? C47 O3 C48 113.6(3) . . ? C50 O4 C49 115.5(3) . . ? C59 O5 C60 115.7(3) . . ? C61 O6 C62 111.4(3) . . ? C64 O7 C63 113.0(3) . . ? C34 O8 C65 115.9(4) . . ? C35 C34 O8 125.0(4) . . ? C35 C34 C43 120.0(4) . . ? O8 C34 C43 115.0(4) . . ? C34 C35 C36 121.5(4) . . ? C34 C35 H35A 119.2 . . ? C36 C35 H35A 119.2 . . ? C35 C36 C41 119.1(4) . . ? C35 C36 C37 122.8(4) . . ? C41 C36 C37 118.1(4) . . ? C38 C37 C36 120.9(5) . . ? C38 C37 H37A 119.5 . . ? C36 C37 H37A 119.5 . . ? C37 C38 C39 120.3(5) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C40 C39 C38 120.3(5) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C39 C40 C41 121.3(5) . . ? C39 C40 H40A 119.3 . . ? C41 C40 H40A 119.3 . . ? C40 C41 C36 119.1(4) . . ? C40 C41 C42 122.6(4) . . ? C36 C41 C42 118.3(4) . . ? C43 C42 C41 121.7(4) . . ? C43 C42 H42A 119.2 . . ? C41 C42 H42A 119.2 . . ? C42 C43 O1 125.4(4) . . ? C42 C43 C34 119.3(4) . . ? O1 C43 C34 115.3(4) . . ? O1 C44 C45 109.1(4) . . ? O1 C44 H44A 109.9 . . ? C45 C44 H44A 109.9 . . ? O1 C44 H44B 109.9 . . ? C45 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? O2 C45 C44 108.9(4) . . ? O2 C45 H45A 109.9 . . ? C44 C45 H45A 109.9 . . ? O2 C45 H45B 109.9 . . ? C44 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? O2 C46 C47 113.5(4) . . ? O2 C46 H46A 108.9 . . ? C47 C46 H46A 108.9 . . ? O2 C46 H46B 108.9 . . ? C47 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? O3 C47 C46 112.3(4) . . ? O3 C47 H47A 109.1 . . ? C46 C47 H47A 109.1 . . ? O3 C47 H47B 109.1 . . ? C46 C47 H47B 109.1 . . ? H47A C47 H47B 107.9 . . ? O3 C48 C49 109.3(3) . . ? O3 C48 H48A 109.8 . . ? C49 C48 H48A 109.8 . . ? O3 C48 H48B 109.8 . . ? C49 C48 H48B 109.8 . . ? H48A C48 H48B 108.3 . . ? O4 C49 C48 107.7(3) . . ? O4 C49 H49A 110.2 . . ? C48 C49 H49A 110.2 . . ? O4 C49 H49B 110.2 . . ? C48 C49 H49B 110.2 . . ? H49A C49 H49B 108.5 . . ? C51 C50 O4 125.0(3) . . ? C51 C50 C59 120.7(4) . . ? O4 C50 C59 114.2(3) . . ? C50 C51 C52 120.8(4) . . ? C50 C51 H51A 119.6 . . ? C52 C51 H51A 119.6 . . ? C57 C52 C51 119.1(4) . . ? C57 C52 C53 118.9(4) . . ? C51 C52 C53 122.0(4) . . ? C54 C53 C52 121.4(4) . . ? C54 C53 H53A 119.3 . . ? C52 C53 H53A 119.3 . . ? C53 C54 C55 119.4(4) . . ? C53 C54 H54A 120.3 . . ? C55 C54 H54A 120.3 . . ? C56 C55 C54 121.2(4) . . ? C56 C55 H55A 119.4 . . ? C54 C55 H55A 119.4 . . ? C55 C56 C57 120.6(4) . . ? C55 C56 H56A 119.7 . . ? C57 C56 H56A 119.7 . . ? C52 C57 C56 118.5(4) . . ? C52 C57 C58 119.4(4) . . ? C56 C57 C58 122.1(4) . . ? C59 C58 C57 120.8(4) . . ? C59 C58 H58A 119.6 . . ? C57 C58 H58A 119.6 . . ? C58 C59 O5 125.4(4) . . ? C58 C59 C50 119.1(4) . . ? O5 C59 C50 115.4(3) . . ? O5 C60 C61 108.3(3) . . ? O5 C60 H60A 110.0 . . ? C61 C60 H60A 110.0 . . ? O5 C60 H60B 110.0 . . ? C61 C60 H60B 110.0 . . ? H60A C60 H60B 108.4 . . ? O6 C61 C60 110.3(3) . . ? O6 C61 H61A 109.6 . . ? C60 C61 H61A 109.6 . . ? O6 C61 H61B 109.6 . . ? C60 C61 H61B 109.6 . . ? H61A C61 H61B 108.1 . . ? O6 C62 C63 109.8(4) . . ? O6 C62 H62A 109.7 . . ? C63 C62 H62A 109.7 . . ? O6 C62 H62B 109.7 . . ? C63 C62 H62B 109.7 . . ? H62A C62 H62B 108.2 . . ? O7 C63 C62 110.3(3) . . ? O7 C63 H63A 109.6 . . ? C62 C63 H63A 109.6 . . ? O7 C63 H63B 109.6 . . ? C62 C63 H63B 109.6 . . ? H63A C63 H63B 108.1 . . ? O7 C64 C65 110.6(4) . . ? O7 C64 H64A 109.5 . . ? C65 C64 H64A 109.5 . . ? O7 C64 H64B 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? C64 C65 O8 109.3(5) . . ? C64 C65 H65A 109.8 . . ? O8 C65 H65A 109.8 . . ? C64 C65 H65B 109.8 . . ? O8 C65 H65B 109.8 . . ? H65A C65 H65B 108.3 . . ? F3A B1A F2A 108.7(9) . . ? F3A B1A F4A 110.4(9) . . ? F2A B1A F4A 112.8(10) . . ? F3A B1A F1A 109.2(10) . . ? F2A B1A F1A 105.1(8) . . ? F4A B1A F1A 110.4(9) . . ? F1B B1B F3B 115.9(13) . . ? F1B B1B F4B 111.0(13) . . ? F3B B1B F4B 102.9(19) . . ? F1B B1B F2B 107.7(12) . . ? F3B B1B F2B 108.9(12) . . ? F4B B1B F2B 110.4(13) . . ? N1S C1S C2S 177.9(9) . . ? C1S C2S H1SA 109.5 . . ? C1S C2S H1SB 109.5 . . ? H1SA C2S H1SB 109.5 . . ? C1S C2S H1SC 109.5 . . ? H1SA C2S H1SC 109.5 . . ? H1SB C2S H1SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.659 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.056 # Attachment '- 891818.cif' data_kz88 _database_code_depnum_ccdc_archive 'CCDC 891918' #TrackingRef '- 891818.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H114 N4 O10' _chemical_formula_weight 1531.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1231(17) _cell_length_b 23.130(3) _cell_length_c 26.377(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.575(2) _cell_angle_gamma 90.00 _cell_volume 8470.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 222 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9774 _exptl_absorpt_correction_T_max 0.9962 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 61059 _diffrn_reflns_av_R_equivalents 0.1301 _diffrn_reflns_av_sigmaI/netI 0.1168 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 23.26 _reflns_number_total 12142 _reflns_number_gt 7094 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _refine_special_details ; ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 723 176 ' ' 2 0.000 0.500 0.500 723 176 ' ' _platon_squeeze_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Crystals were very weakly diffracting; a cut-off at 0.8 A was applied in XPEP to improve data set statistics and allow for a solution. This allowed the location of all axle and wheel atom psoitions. Electron density in the lattice appeared to be THF molecules (H-bonded to the open benzimidazolium NH group) but no satisfactory model could be devised. The unit cell was calculated to contain an estimated 8 molecules of THF which were treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. Three ISOR commands were necessary to restrain C27 (axle), C72 (crown) and C75 (crown) to have approximate isotropic behaviour. A single AFIX 66 commands was used to restrain one of the outer rings of a naphthyl unit to be an idealized hexagon with C-C and bonds equal to 1.39 A. ; _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^)+(0.1365P)^2^+51.9337P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12142 _refine_ls_number_parameters 925 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.2292 _refine_ls_R_factor_gt 0.1690 _refine_ls_wR_factor_ref 0.4070 _refine_ls_wR_factor_gt 0.3701 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _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 N1 N 0.3650(4) -0.0877(3) 0.6412(2) 0.0271(15) Uani 1 1 d . . . H1D H 0.3736 -0.0798 0.6743 0.032 Uiso 1 1 calc R . . N2 N 0.3097(4) -0.0808(3) 0.5569(2) 0.0259(15) Uani 1 1 d . . . N3 N 0.1210(4) 0.1719(3) 0.6867(2) 0.0295(15) Uani 1 1 d . . . H3D H 0.1514 0.1559 0.7154 0.035 Uiso 1 1 calc R . . N4 N 0.0602(4) 0.1851(3) 0.6040(2) 0.0276(15) Uani 1 1 d . . . C1 C 0.6829(12) -0.2652(7) 0.8641(5) 0.135(7) Uani 1 1 d . . . H1A H 0.7108 -0.2716 0.9005 0.203 Uiso 1 1 calc R . . H1B H 0.7337 -0.2680 0.8434 0.203 Uiso 1 1 calc R . . H1C H 0.6337 -0.2947 0.8527 0.203 Uiso 1 1 calc R . . C2 C 0.5676(12) -0.2054(11) 0.8941(4) 0.189(12) Uani 1 1 d . . . H2A H 0.6018 -0.2125 0.9294 0.283 Uiso 1 1 calc R . . H2B H 0.5186 -0.2354 0.8843 0.283 Uiso 1 1 calc R . . H2C H 0.5365 -0.1674 0.8924 0.283 Uiso 1 1 calc R . . C3 C 0.7215(16) -0.1669(10) 0.8735(5) 0.184(10) Uani 1 1 d . . . H3A H 0.7497 -0.1735 0.9098 0.275 Uiso 1 1 calc R . . H3B H 0.6992 -0.1267 0.8689 0.275 Uiso 1 1 calc R . . H3C H 0.7701 -0.1741 0.8521 0.275 Uiso 1 1 calc R . . C4 C 0.6382(8) -0.2068(6) 0.8577(4) 0.070(4) Uani 1 1 d . . . C5 C 0.5949(7) -0.1955(4) 0.8015(3) 0.052(3) Uani 1 1 d . . . C6 C 0.5005(7) -0.1821(4) 0.7858(3) 0.056(3) Uani 1 1 d . . . H6A H 0.4605 -0.1786 0.8110 0.067 Uiso 1 1 calc R . . C7 C 0.4604(6) -0.1732(4) 0.7346(3) 0.048(2) Uani 1 1 d . . . H7A H 0.3942 -0.1631 0.7255 0.058 Uiso 1 1 calc R . . C8 C 0.5144(5) -0.1787(3) 0.6968(3) 0.034(2) Uani 1 1 d . . . C9 C 0.6108(6) -0.1925(4) 0.7128(3) 0.049(2) Uani 1 1 d . . . H9A H 0.6507 -0.1958 0.6876 0.058 Uiso 1 1 calc R . . C10 C 0.6510(6) -0.2019(5) 0.7643(3) 0.063(3) Uani 1 1 d . . . H10A H 0.7168 -0.2126 0.7737 0.075 Uiso 1 1 calc R . . C11 C 0.4744(6) -0.1733(4) 0.6403(3) 0.038(2) Uani 1 1 d . . . C12 C 0.4070(5) -0.1322(3) 0.6191(3) 0.0202(16) Uani 1 1 d . . . C13 C 0.3721(4) -0.1275(3) 0.5669(3) 0.0228(17) Uani 1 1 d . . . C14 C 0.3985(6) -0.1688(4) 0.5309(3) 0.039(2) Uani 1 1 d . . . C15 C 0.4674(6) -0.2088(4) 0.5528(3) 0.044(2) Uani 1 1 d . . . H15A H 0.4907 -0.2360 0.5311 0.052 Uiso 1 1 calc R . . C16 C 0.5027(5) -0.2101(4) 0.6044(3) 0.036(2) Uani 1 1 d . . . H16A H 0.5502 -0.2384 0.6167 0.044 Uiso 1 1 calc R . . C17 C 0.3593(5) -0.1674(3) 0.4747(3) 0.0269(17) Uani 1 1 d . . . C18 C 0.3281(6) -0.1193(3) 0.4474(3) 0.036(2) Uani 1 1 d . . . H18A H 0.3296 -0.0831 0.4645 0.043 Uiso 1 1 calc R . . C19 C 0.2941(6) -0.1221(4) 0.3947(4) 0.046(2) Uani 1 1 d . . . H19A H 0.2725 -0.0874 0.3769 0.055 Uiso 1 1 calc R . . C20 C 0.2900(6) -0.1725(4) 0.3670(3) 0.041(2) Uani 1 1 d . . . C21 C 0.3207(7) -0.2210(4) 0.3951(3) 0.050(3) Uani 1 1 d . . . H21A H 0.3201 -0.2571 0.3779 0.060 Uiso 1 1 calc R . . C22 C 0.3518(7) -0.2187(4) 0.4469(3) 0.052(3) Uani 1 1 d . . . H22A H 0.3693 -0.2537 0.4650 0.062 Uiso 1 1 calc R . . C23 C 0.2509(8) -0.1734(4) 0.3092(3) 0.057(3) Uani 1 1 d . . . C24 C 0.1491(10) -0.1643(11) 0.2993(5) 0.201(13) Uani 1 1 d . . . H24A H 0.1249 -0.1653 0.2620 0.302 Uiso 1 1 calc R . . H24B H 0.1347 -0.1266 0.3130 0.302 Uiso 1 1 calc R . . H24C H 0.1179 -0.1948 0.3161 0.302 Uiso 1 1 calc R . . C25 C 0.2962(10) -0.1284(8) 0.2820(3) 0.132(7) Uani 1 1 d . . . H25A H 0.2701 -0.1304 0.2450 0.197 Uiso 1 1 calc R . . H25B H 0.3660 -0.1346 0.2879 0.197 Uiso 1 1 calc R . . H25C H 0.2825 -0.0902 0.2952 0.197 Uiso 1 1 calc R . . C26 C 0.277(3) -0.2295(8) 0.2870(5) 0.32(2) Uani 1 1 d . . . H26A H 0.2519 -0.2300 0.2498 0.480 Uiso 1 1 calc R . . H26B H 0.2486 -0.2615 0.3034 0.480 Uiso 1 1 calc R . . H26C H 0.3471 -0.2337 0.2932 0.480 Uiso 1 1 calc R . . C27 C 0.3082(5) -0.0583(3) 0.6034(3) 0.0260(17) Uani 1 1 d U . . C28 C 0.2545(5) -0.0060(3) 0.6120(3) 0.0280(18) Uani 1 1 d . . . C29 C 0.2404(7) 0.0081(4) 0.6603(3) 0.047(2) Uani 1 1 d . . . H29A H 0.2649 -0.0165 0.6885 0.056 Uiso 1 1 calc R . . C30 C 0.1918(7) 0.0569(4) 0.6686(3) 0.042(2) Uani 1 1 d . . . H30A H 0.1798 0.0649 0.7022 0.050 Uiso 1 1 calc R . . C31 C 0.1599(5) 0.0945(3) 0.6292(3) 0.0303(19) Uani 1 1 d . . . C32 C 0.1731(5) 0.0800(3) 0.5801(3) 0.0288(18) Uani 1 1 d . . . H32A H 0.1502 0.1052 0.5521 0.035 Uiso 1 1 calc R . . C33 C 0.2182(5) 0.0304(3) 0.5713(3) 0.0223(16) Uani 1 1 d . . . H33A H 0.2250 0.0205 0.5371 0.027 Uiso 1 1 calc R . . C34 C 0.1114(5) 0.1500(3) 0.6397(3) 0.0247(18) Uani 1 1 d . . . C35 C 0.2922(10) 0.2387(10) 0.9557(4) 0.150(9) Uani 1 1 d . . . H35A H 0.3135 0.2329 0.9929 0.225 Uiso 1 1 calc R . . H35B H 0.3093 0.2779 0.9464 0.225 Uiso 1 1 calc R . . H35C H 0.3237 0.2104 0.9368 0.225 Uiso 1 1 calc R . . C36 C 0.1643(15) 0.1723(10) 0.9598(5) 0.187(12) Uani 1 1 d . . . H36A H 0.1875 0.1679 0.9970 0.281 Uiso 1 1 calc R . . H36B H 0.1939 0.1427 0.9412 0.281 Uiso 1 1 calc R . . H36C H 0.0941 0.1679 0.9522 0.281 Uiso 1 1 calc R . . C37 C 0.1344(14) 0.2706(11) 0.9710(5) 0.183(11) Uani 1 1 d . . . H37A H 0.1555 0.2656 1.0082 0.274 Uiso 1 1 calc R . . H37B H 0.0658 0.2612 0.9615 0.274 Uiso 1 1 calc R . . H37C H 0.1447 0.3109 0.9617 0.274 Uiso 1 1 calc R . . C38 C 0.1910(7) 0.2316(6) 0.9429(4) 0.065(3) Uani 1 1 d . . . C39 C 0.1578(7) 0.2405(6) 0.8850(4) 0.063(3) Uani 1 1 d . . . C40 C 0.1619(7) 0.2911(5) 0.8621(3) 0.060(3) Uani 1 1 d . . . H40A H 0.1858 0.3230 0.8833 0.072 Uiso 1 1 calc R . . C41 C 0.1344(8) 0.3011(4) 0.8102(4) 0.065(3) Uani 1 1 d . . . H41A H 0.1391 0.3391 0.7972 0.078 Uiso 1 1 calc R . . C42 C 0.1002(5) 0.2571(4) 0.7769(3) 0.035(2) Uani 1 1 d . . . C43 C 0.0965(7) 0.2038(5) 0.7996(3) 0.054(3) Uani 1 1 d . . . H43A H 0.0747 0.1718 0.7781 0.065 Uiso 1 1 calc R . . C44 C 0.1227(7) 0.1945(5) 0.8519(4) 0.062(3) Uani 1 1 d . . . H44A H 0.1170 0.1569 0.8657 0.074 Uiso 1 1 calc R . . C45 C 0.0685(6) 0.2663(4) 0.7201(4) 0.042(2) Uani 1 1 d . . . C46 C 0.0255(5) 0.3171(4) 0.7013(3) 0.042(2) Uani 1 1 d . . . H46A H 0.0220 0.3479 0.7247 0.050 Uiso 1 1 calc R . . C47 C -0.0140(6) 0.3255(4) 0.6486(3) 0.040(2) Uani 1 1 d . . . H47A H -0.0438 0.3613 0.6376 0.048 Uiso 1 1 calc R . . C48 C -0.0096(5) 0.2818(4) 0.6124(3) 0.036(2) Uani 1 1 d . . . C49 C 0.0375(5) 0.2326(3) 0.6308(3) 0.0267(18) Uani 1 1 d . . . C50 C 0.0760(5) 0.2226(3) 0.6823(3) 0.0303(18) Uani 1 1 d . . . C51 C -0.0570(5) 0.2930(4) 0.5573(3) 0.035(2) Uani 1 1 d . . . C52 C -0.0426(7) 0.3437(4) 0.5315(3) 0.051(2) Uani 1 1 d . . . H52A H -0.0001 0.3725 0.5485 0.061 Uiso 1 1 calc R . . C53 C -0.0890(9) 0.3525(5) 0.4821(4) 0.072(3) Uani 1 1 d . . . H53A H -0.0772 0.3875 0.4655 0.087 Uiso 1 1 calc R . . C54 C -0.1531(7) 0.3126(5) 0.4545(3) 0.056(3) Uani 1 1 d . . . C55 C -0.1653(7) 0.2634(4) 0.4810(4) 0.058(3) Uani 1 1 d . . . H55A H -0.2080 0.2348 0.4640 0.069 Uiso 1 1 calc R . . C56 C -0.1199(7) 0.2528(4) 0.5303(4) 0.053(3) Uani 1 1 d . . . H56A H -0.1313 0.2174 0.5464 0.063 Uiso 1 1 calc R . . C57 C -0.1973(9) 0.3250(6) 0.3980(4) 0.079(4) Uani 1 1 d . . . C58 C -0.2421(14) 0.3831(8) 0.3915(6) 0.140(7) Uani 1 1 d . . . H58A H -0.2936 0.3856 0.4118 0.211 Uiso 1 1 calc R . . H58B H -0.2691 0.3895 0.3550 0.211 Uiso 1 1 calc R . . H58C H -0.1933 0.4126 0.4034 0.211 Uiso 1 1 calc R . . C59 C -0.2728(12) 0.2799(9) 0.3782(5) 0.148(8) Uani 1 1 d . . . H59A H -0.3219 0.2795 0.4001 0.222 Uiso 1 1 calc R . . H59B H -0.2422 0.2418 0.3791 0.222 Uiso 1 1 calc R . . H59C H -0.3030 0.2892 0.3427 0.222 Uiso 1 1 calc R . . C60 C -0.1190(9) 0.3239(10) 0.3665(5) 0.146(8) Uani 1 1 d . . . H60A H -0.1469 0.3310 0.3302 0.220 Uiso 1 1 calc R . . H60B H -0.0876 0.2859 0.3698 0.220 Uiso 1 1 calc R . . H60C H -0.0714 0.3539 0.3788 0.220 Uiso 1 1 calc R . . O1 O 0.2529(5) -0.0934(4) 0.7467(3) 0.096(3) Uani 1 1 d . . . O2 O 0.1151(7) -0.1209(5) 0.6513(6) 0.120(4) Uani 1 1 d . . . O3 O 0.0383(12) -0.1084(13) 0.5150(8) 0.321(17) Uani 1 1 d . . . O4 O 0.1442(5) -0.0145(4) 0.4489(3) 0.088(3) Uani 1 1 d . . . O5 O 0.2898(6) 0.0505(4) 0.4537(3) 0.079(2) Uani 1 1 d . . . O6 O 0.4339(5) 0.0653(3) 0.5470(3) 0.062(2) Uani 1 1 d . . . O7 O 0.4834(5) 0.0334(3) 0.6803(3) 0.072(2) Uani 1 1 d . . . O8 O 0.4147(5) -0.0363(3) 0.7584(3) 0.078(2) Uani 1 1 d . . . C61 C 0.3906(9) -0.0562(6) 0.8020(5) 0.078(4) Uani 1 1 d . . . C62 C 0.4436(11) -0.0474(5) 0.8482(5) 0.084(4) Uani 1 1 d . . . H62A H 0.5022 -0.0263 0.8519 0.101 Uiso 1 1 calc R . . C63 C 0.4108(14) -0.0704(7) 0.8936(6) 0.105(5) Uani 1 1 d . . . C64 C 0.4676(19) -0.0607(7) 0.9411(8) 0.170(10) Uani 1 1 d . . . H64A H 0.5227 -0.0367 0.9432 0.204 Uiso 1 1 calc R . . C65 C 0.447(2) -0.0853(10) 0.9869(8) 0.225(15) Uani 1 1 d . . . H65A H 0.4860 -0.0791 1.0198 0.270 Uiso 1 1 calc R . . C66 C 0.364(2) -0.1193(8) 0.9801(6) 0.209(15) Uani 1 1 d . . . H66A H 0.3481 -0.1387 1.0092 0.251 Uiso 1 1 calc R . . C67 C 0.3059(17) -0.1259(7) 0.9352(7) 0.146(8) Uani 1 1 d . . . H67A H 0.2484 -0.1476 0.9338 0.175 Uiso 1 1 calc R . . C68 C 0.3268(13) -0.1010(5) 0.8869(6) 0.091(4) Uani 1 1 d . . . C69 C 0.2763(10) -0.1099(6) 0.8393(6) 0.088(4) Uani 1 1 d . . . H69A H 0.2196 -0.1328 0.8359 0.106 Uiso 1 1 calc R . . C70 C 0.3012(7) -0.0880(4) 0.7954(5) 0.060(3) Uani 1 1 d . . . C71 C 0.1627(8) -0.1219(8) 0.7416(8) 0.177(11) Uani 1 1 d . . . H71A H 0.1352 -0.1168 0.7732 0.213 Uiso 1 1 calc R . . H71B H 0.1702 -0.1638 0.7357 0.213 Uiso 1 1 calc R . . C72 C 0.100(2) -0.0956(13) 0.6972(10) 0.207(11) Uani 1 1 d U . . H72A H 0.0316 -0.1008 0.7006 0.249 Uiso 1 1 calc R . . H72B H 0.1130 -0.0536 0.6965 0.249 Uiso 1 1 calc R . . C73 C 0.0488(15) -0.0989(11) 0.6040(13) 0.232(16) Uani 1 1 d . . . H73A H -0.0189 -0.1098 0.6043 0.278 Uiso 1 1 calc R . . H73B H 0.0533 -0.0564 0.6010 0.278 Uiso 1 1 calc R . . C74 C 0.0805(13) -0.1244(16) 0.5678(11) 0.25(2) Uani 1 1 d . . . H74A H 0.0713 -0.1665 0.5716 0.305 Uiso 1 1 calc R . . H74B H 0.1507 -0.1173 0.5727 0.305 Uiso 1 1 calc R . . C75 C 0.0861(15) -0.0858(10) 0.4923(9) 0.156(7) Uani 1 1 d U . . H75A H 0.1371 -0.1146 0.4902 0.187 Uiso 1 1 calc R . . H75B H 0.1176 -0.0556 0.5161 0.187 Uiso 1 1 calc R . . C76 C 0.0729(9) -0.0602(9) 0.4466(5) 0.131(7) Uani 1 1 d . . . H76A H 0.0071 -0.0437 0.4383 0.157 Uiso 1 1 calc R . . H76B H 0.0805 -0.0886 0.4195 0.157 Uiso 1 1 calc R . . C77 C 0.1601(9) 0.0038(6) 0.4037(4) 0.074(3) Uani 1 1 d . . . C78 C 0.1022(9) -0.0085(7) 0.3587(5) 0.096(5) Uani 1 1 d . . . H78A H 0.0465 -0.0311 0.3601 0.115 Uiso 1 1 calc R . . C79 C 0.1166(8) 0.0087(5) 0.3100(4) 0.103(5) Uani 1 1 d G . . C80 C 0.0595(8) -0.0062(6) 0.2631(5) 0.165(9) Uani 1 1 d G . . H80A H 0.0035 -0.0292 0.2625 0.198 Uiso 1 1 calc R . . C81 C 0.0842(10) 0.0124(6) 0.2172(4) 0.179(10) Uani 1 1 d G . . H81A H 0.0452 0.0022 0.1852 0.215 Uiso 1 1 calc R . . C82 C 0.1661(11) 0.0460(6) 0.2181(3) 0.144(8) Uani 1 1 d G . . H82A H 0.1830 0.0588 0.1867 0.173 Uiso 1 1 calc R . . C83 C 0.2232(8) 0.0610(4) 0.2649(4) 0.145(7) Uani 1 1 d G . . H83A H 0.2792 0.0840 0.2655 0.175 Uiso 1 1 calc R . . C84 C 0.1985(7) 0.0424(4) 0.3109(3) 0.084(4) Uani 1 1 d G . . C85 C 0.2630(11) 0.0574(5) 0.3591(5) 0.094(5) Uani 1 1 d . . . H85A H 0.3194 0.0796 0.3586 0.112 Uiso 1 1 calc R . . C86 C 0.2416(9) 0.0392(5) 0.4048(5) 0.075(4) Uani 1 1 d . . . C87 C 0.3743(9) 0.0850(7) 0.4602(5) 0.104(5) Uani 1 1 d . . . H87A H 0.3656 0.1171 0.4349 0.125 Uiso 1 1 calc R . . H87B H 0.4298 0.0613 0.4544 0.125 Uiso 1 1 calc R . . C88 C 0.3935(10) 0.1097(7) 0.5165(5) 0.094(4) Uani 1 1 d . . . H88A H 0.4379 0.1432 0.5193 0.113 Uiso 1 1 calc R . . H88B H 0.3324 0.1222 0.5265 0.113 Uiso 1 1 calc R . . C89 C 0.4512(8) 0.0811(5) 0.6063(5) 0.084(4) Uani 1 1 d . . . H89A H 0.4905 0.1167 0.6134 0.101 Uiso 1 1 calc R . . H89B H 0.3893 0.0870 0.6181 0.101 Uiso 1 1 calc R . . C90 C 0.4998(9) 0.0338(6) 0.6302(6) 0.094(4) Uani 1 1 d . . . H90A H 0.5696 0.0370 0.6299 0.113 Uiso 1 1 calc R . . H90B H 0.4753 -0.0022 0.6122 0.113 Uiso 1 1 calc R . . C91 C 0.5400(9) -0.0099(7) 0.7138(5) 0.099(5) Uani 1 1 d . . . H91A H 0.6095 -0.0009 0.7180 0.118 Uiso 1 1 calc R . . H91B H 0.5290 -0.0488 0.6981 0.118 Uiso 1 1 calc R . . C92 C 0.5093(10) -0.0089(8) 0.7647(5) 0.122(6) Uani 1 1 d . . . H92A H 0.5562 -0.0302 0.7905 0.146 Uiso 1 1 calc R . . H92B H 0.5057 0.0314 0.7767 0.146 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 N1 0.030(3) 0.039(4) 0.008(3) -0.011(3) -0.006(3) -0.003(3) N2 0.026(3) 0.043(4) 0.006(3) -0.002(3) -0.002(2) -0.003(3) N3 0.024(3) 0.038(4) 0.026(4) 0.006(3) 0.006(3) 0.010(3) N4 0.021(3) 0.034(4) 0.029(3) 0.005(3) 0.008(3) -0.002(3) C1 0.176(16) 0.174(16) 0.061(8) 0.078(10) 0.036(9) 0.100(14) C2 0.152(15) 0.39(3) 0.021(6) 0.038(11) 0.019(8) 0.152(19) C3 0.20(2) 0.27(3) 0.055(9) 0.017(13) -0.058(11) -0.05(2) C4 0.050(6) 0.113(10) 0.045(6) 0.041(6) 0.004(5) 0.040(7) C5 0.047(6) 0.072(7) 0.039(5) 0.014(5) 0.007(4) 0.023(5) C6 0.063(6) 0.082(7) 0.019(4) -0.004(5) -0.004(4) 0.042(6) C7 0.020(4) 0.073(7) 0.053(6) -0.011(5) 0.010(4) 0.017(4) C8 0.019(4) 0.029(5) 0.051(5) 0.009(4) -0.001(4) 0.008(3) C9 0.041(5) 0.080(7) 0.033(5) 0.013(5) 0.027(4) 0.006(5) C10 0.023(5) 0.122(10) 0.041(5) 0.032(6) 0.000(4) 0.018(5) C11 0.037(5) 0.048(5) 0.029(4) -0.009(4) 0.005(4) -0.020(4) C12 0.016(4) 0.015(4) 0.029(4) -0.002(3) 0.001(3) -0.005(3) C13 0.006(3) 0.034(4) 0.024(4) 0.006(3) -0.006(3) -0.001(3) C14 0.025(4) 0.059(6) 0.033(5) 0.011(4) 0.006(4) -0.006(4) C15 0.043(5) 0.057(6) 0.035(5) -0.002(4) 0.018(4) 0.010(5) C16 0.021(4) 0.056(6) 0.033(5) 0.011(4) 0.005(3) 0.007(4) C17 0.027(4) 0.021(4) 0.033(4) 0.001(4) 0.006(3) -0.002(3) C18 0.050(5) 0.020(4) 0.036(5) -0.010(4) 0.002(4) 0.001(4) C19 0.025(5) 0.057(6) 0.056(6) 0.001(5) 0.008(4) 0.006(4) C20 0.052(6) 0.051(6) 0.023(4) -0.017(4) 0.011(4) -0.007(4) C21 0.101(8) 0.033(5) 0.013(4) -0.007(4) 0.000(4) -0.007(5) C22 0.074(7) 0.036(5) 0.049(6) -0.005(5) 0.020(5) 0.030(5) C23 0.098(8) 0.053(6) 0.022(5) -0.014(4) 0.016(5) -0.029(6) C24 0.071(10) 0.48(4) 0.044(8) -0.012(14) -0.026(7) -0.122(17) C25 0.134(12) 0.25(2) 0.004(5) 0.021(7) -0.007(6) -0.116(13) C26 0.74(7) 0.127(16) 0.035(8) -0.031(9) -0.075(19) 0.18(3) C27 0.025(4) 0.030(4) 0.017(4) 0.008(3) -0.013(3) -0.004(3) C28 0.029(4) 0.034(5) 0.024(4) -0.010(4) 0.015(3) -0.006(4) C29 0.070(6) 0.037(5) 0.032(5) 0.007(4) 0.004(4) 0.009(5) C30 0.072(6) 0.036(5) 0.024(4) 0.009(4) 0.027(4) 0.004(5) C31 0.025(4) 0.024(4) 0.047(5) 0.006(4) 0.021(4) -0.003(3) C32 0.037(4) 0.034(5) 0.014(4) -0.011(3) 0.001(3) -0.012(4) C33 0.013(4) 0.037(5) 0.015(4) -0.010(3) -0.001(3) -0.010(3) C34 0.022(4) 0.044(5) 0.012(4) -0.005(3) 0.014(3) -0.015(4) C35 0.086(10) 0.31(3) 0.041(7) 0.030(11) -0.016(7) -0.061(13) C36 0.23(2) 0.25(3) 0.060(9) 0.049(12) -0.027(11) -0.17(2) C37 0.168(17) 0.33(3) 0.039(8) -0.017(12) 0.003(9) 0.114(19) C38 0.036(5) 0.114(10) 0.044(6) 0.003(6) 0.005(5) -0.015(6) C39 0.038(6) 0.102(9) 0.053(6) 0.016(7) 0.019(5) 0.002(6) C40 0.072(7) 0.082(8) 0.024(5) -0.017(5) 0.001(5) -0.005(6) C41 0.079(8) 0.038(6) 0.080(8) -0.007(6) 0.018(6) 0.003(5) C42 0.029(4) 0.040(5) 0.039(5) -0.007(4) 0.016(4) -0.008(4) C43 0.047(6) 0.072(7) 0.039(6) -0.009(5) -0.004(4) 0.003(5) C44 0.051(6) 0.079(8) 0.057(7) 0.005(6) 0.012(5) 0.002(6) C45 0.024(4) 0.036(5) 0.063(6) 0.001(5) 0.003(4) -0.001(4) C46 0.024(4) 0.060(6) 0.042(5) -0.016(5) 0.006(4) -0.003(4) C47 0.041(5) 0.027(5) 0.048(5) -0.006(4) 0.003(4) 0.009(4) C48 0.021(4) 0.051(6) 0.042(5) -0.019(4) 0.022(4) -0.004(4) C49 0.029(4) 0.011(4) 0.048(5) -0.009(4) 0.025(4) 0.004(3) C50 0.023(4) 0.031(5) 0.041(5) -0.003(4) 0.016(4) 0.002(3) C51 0.020(4) 0.044(5) 0.043(5) -0.012(4) 0.012(4) 0.001(4) C52 0.080(7) 0.032(5) 0.038(5) 0.002(4) 0.004(5) -0.007(5) C53 0.096(9) 0.071(8) 0.046(6) 0.009(6) 0.004(6) -0.015(7) C54 0.060(6) 0.080(8) 0.028(5) -0.024(5) 0.007(5) 0.012(6) C55 0.059(6) 0.056(6) 0.053(6) 0.008(5) 0.000(5) -0.026(5) C56 0.063(6) 0.053(6) 0.045(6) 0.012(5) 0.016(5) -0.016(5) C57 0.085(9) 0.100(10) 0.045(6) 0.008(7) -0.006(6) -0.023(8) C58 0.175(18) 0.154(17) 0.086(11) 0.045(11) 0.008(11) 0.009(14) C59 0.117(13) 0.24(2) 0.080(10) 0.045(12) -0.009(9) -0.077(14) C60 0.057(8) 0.33(3) 0.054(8) 0.011(12) 0.019(6) -0.036(12) O1 0.048(5) 0.140(8) 0.098(6) 0.082(6) 0.008(4) -0.003(5) O2 0.062(6) 0.106(8) 0.196(12) 0.069(8) 0.033(7) 0.020(5) O3 0.136(14) 0.59(4) 0.26(2) 0.31(3) 0.100(14) 0.140(19) O4 0.044(4) 0.161(9) 0.056(5) -0.009(5) 0.006(4) -0.043(5) O5 0.078(5) 0.108(7) 0.056(5) -0.008(5) 0.028(4) -0.029(5) O6 0.043(4) 0.053(4) 0.094(6) -0.016(4) 0.022(4) -0.027(3) O7 0.052(4) 0.065(5) 0.103(6) 0.050(4) 0.028(4) -0.002(4) O8 0.067(5) 0.089(6) 0.087(6) 0.043(5) 0.037(4) -0.013(4) C61 0.083(9) 0.087(9) 0.066(8) 0.036(7) 0.020(7) 0.043(7) C62 0.127(11) 0.047(7) 0.097(10) 0.029(7) 0.066(9) 0.003(7) C63 0.161(16) 0.075(10) 0.087(10) -0.006(8) 0.046(11) 0.005(10) C64 0.30(3) 0.091(13) 0.136(16) -0.006(12) 0.099(19) -0.078(16) C65 0.42(4) 0.16(2) 0.099(14) -0.023(14) 0.065(19) -0.17(3) C66 0.48(5) 0.098(14) 0.053(10) -0.021(10) 0.067(17) -0.08(2) C67 0.25(2) 0.108(13) 0.098(13) -0.001(11) 0.084(15) -0.035(14) C68 0.147(14) 0.043(7) 0.091(10) 0.005(7) 0.040(10) -0.031(8) C69 0.077(9) 0.086(10) 0.114(11) 0.032(9) 0.048(9) 0.008(7) C70 0.034(5) 0.045(6) 0.113(9) 0.048(6) 0.048(6) 0.009(4) C71 0.029(7) 0.23(2) 0.27(2) 0.216(18) 0.019(9) -0.020(9) C72 0.195(14) 0.211(14) 0.216(14) 0.019(10) 0.040(10) -0.016(9) C73 0.129(19) 0.19(2) 0.43(5) 0.11(3) 0.20(3) 0.046(16) C74 0.051(11) 0.49(6) 0.23(3) -0.16(3) 0.033(14) 0.023(19) C75 0.134(10) 0.164(11) 0.171(11) 0.029(9) 0.031(9) -0.052(8) C76 0.055(8) 0.26(2) 0.069(9) 0.014(11) -0.014(7) -0.075(11) C77 0.071(8) 0.105(10) 0.045(7) -0.030(7) 0.007(6) -0.014(7) C78 0.069(8) 0.140(13) 0.087(10) 0.023(9) 0.036(8) 0.010(8) C79 0.082(10) 0.096(11) 0.129(14) -0.011(10) 0.012(9) -0.028(8) C80 0.19(2) 0.22(2) 0.077(11) 0.013(14) -0.003(13) -0.020(18) C81 0.21(3) 0.19(3) 0.126(19) -0.007(17) 0.003(17) 0.02(2) C82 0.24(3) 0.148(17) 0.048(9) -0.012(10) 0.041(12) -0.003(16) C83 0.24(2) 0.088(11) 0.118(14) -0.049(11) 0.063(15) 0.036(13) C84 0.127(12) 0.098(10) 0.032(6) -0.011(6) 0.032(7) 0.047(9) C85 0.137(12) 0.059(8) 0.109(11) -0.003(7) 0.085(10) -0.002(8) C86 0.085(9) 0.059(7) 0.098(10) -0.007(7) 0.058(8) 0.001(6) C87 0.074(9) 0.153(14) 0.084(9) 0.013(9) 0.009(7) -0.064(9) C88 0.089(10) 0.103(11) 0.088(10) 0.012(9) 0.008(8) -0.011(8) C89 0.050(7) 0.057(8) 0.140(12) -0.015(8) 0.003(7) 0.005(6) C90 0.069(8) 0.085(10) 0.145(13) 0.009(9) 0.064(9) -0.028(7) C91 0.058(8) 0.126(12) 0.114(11) 0.027(10) 0.019(7) -0.036(8) C92 0.106(11) 0.178(16) 0.093(10) 0.030(10) 0.050(9) -0.066(11) _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 N1 C27 1.344(9) . ? N1 C12 1.369(9) . ? N1 H1D 0.8800 . ? N2 C27 1.339(9) . ? N2 C13 1.388(9) . ? N3 C34 1.323(9) . ? N3 C50 1.330(9) . ? N3 H3D 0.8800 . ? N4 C34 1.350(9) . ? N4 C49 1.375(9) . ? C1 C4 1.489(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.507(16) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.49(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.520(13) . ? C5 C6 1.357(12) . ? C5 C10 1.379(12) . ? C6 C7 1.381(12) . ? C6 H6A 0.9500 . ? C7 C8 1.368(11) . ? C7 H7A 0.9500 . ? C8 C9 1.386(11) . ? C8 C11 1.500(11) . ? C9 C10 1.389(12) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C16 1.386(11) . ? C11 C12 1.388(11) . ? C12 C13 1.379(10) . ? C13 C14 1.443(11) . ? C14 C15 1.389(12) . ? C14 C17 1.484(11) . ? C15 C16 1.360(11) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.355(10) . ? C17 C22 1.389(11) . ? C18 C19 1.386(12) . ? C18 H18A 0.9500 . ? C19 C20 1.371(12) . ? C19 H19A 0.9500 . ? C20 C21 1.369(12) . ? C20 C23 1.524(11) . ? C21 C22 1.359(12) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.429(18) . ? C23 C25 1.474(14) . ? C23 C26 1.497(19) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.466(10) . ? C28 C29 1.366(11) . ? C28 C33 1.387(10) . ? C29 C30 1.358(12) . ? C29 H29A 0.9500 . ? C30 C31 1.369(11) . ? C30 H30A 0.9500 . ? C31 C32 1.384(10) . ? C31 C34 1.503(11) . ? C32 C33 1.352(10) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C35 C38 1.416(15) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.510(19) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.490(19) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.528(14) . ? C39 C40 1.323(15) . ? C39 C44 1.408(15) . ? C40 C41 1.371(14) . ? C40 H40A 0.9500 . ? C41 C42 1.374(12) . ? C41 H41A 0.9500 . ? C42 C43 1.375(13) . ? C42 C45 1.498(12) . ? C43 C44 1.379(13) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.373(12) . ? C45 C50 1.437(11) . ? C46 C47 1.413(12) . ? C46 H46A 0.9500 . ? C47 C48 1.399(11) . ? C47 H47A 0.9500 . ? C48 C49 1.362(11) . ? C48 C51 1.507(12) . ? C49 C50 1.388(11) . ? C51 C56 1.388(12) . ? C51 C52 1.391(12) . ? C52 C53 1.362(13) . ? C52 H52A 0.9500 . ? C53 C54 1.400(14) . ? C53 H53A 0.9500 . ? C54 C55 1.361(14) . ? C54 C57 1.534(14) . ? C55 C56 1.364(13) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C58 1.48(2) . ? C57 C60 1.502(17) . ? C57 C59 1.515(18) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O1 C70 1.345(14) . ? O1 C71 1.418(13) . ? O2 C72 1.40(3) . ? O2 C73 1.50(3) . ? O3 C75 1.11(2) . ? O3 C74 1.46(3) . ? O4 C77 1.322(13) . ? O4 C76 1.453(15) . ? O5 C86 1.369(14) . ? O5 C87 1.420(13) . ? O6 C88 1.364(14) . ? O6 C89 1.583(14) . ? O7 C90 1.384(14) . ? O7 C91 1.471(14) . ? O8 C61 1.341(13) . ? O8 C92 1.460(14) . ? C61 C62 1.324(17) . ? C61 C70 1.443(16) . ? C62 C63 1.460(17) . ? C62 H62A 0.9500 . ? C63 C68 1.36(2) . ? C63 C64 1.38(2) . ? C64 C65 1.41(2) . ? C64 H64A 0.9500 . ? C65 C66 1.40(3) . ? C65 H65A 0.9500 . ? C66 C67 1.32(3) . ? C66 H66A 0.9500 . ? C67 C68 1.477(18) . ? C67 H67A 0.9500 . ? C68 C69 1.340(18) . ? C69 C70 1.368(15) . ? C69 H69A 0.9500 . ? C71 C72 1.46(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.27(3) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.32(2) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.342(16) . ? C77 C86 1.408(16) . ? C78 C79 1.395(14) . ? C78 H78A 0.9500 . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C80 C81 1.3900 . ? C80 H80A 0.9500 . ? C81 C82 1.3900 . ? C81 H81A 0.9500 . ? C82 C83 1.3900 . ? C82 H82A 0.9500 . ? C83 C84 1.3900 . ? C83 H83A 0.9500 . ? C84 C85 1.465(16) . ? C85 C86 1.361(16) . ? C85 H85A 0.9500 . ? C87 C88 1.568(17) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.381(16) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.486(17) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? 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 C27 N1 C12 108.3(6) . . ? C27 N1 H1D 125.9 . . ? C12 N1 H1D 125.9 . . ? C27 N2 C13 104.2(5) . . ? C34 N3 C50 107.0(6) . . ? C34 N3 H3D 126.5 . . ? C50 N3 H3D 126.5 . . ? C34 N4 C49 105.5(6) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 C3 103.6(13) . . ? C1 C4 C2 105.3(12) . . ? C3 C4 C2 112.9(15) . . ? C1 C4 C5 110.7(11) . . ? C3 C4 C5 108.7(10) . . ? C2 C4 C5 115.0(9) . . ? C6 C5 C10 117.9(8) . . ? C6 C5 C4 122.3(8) . . ? C10 C5 C4 119.7(8) . . ? C5 C6 C7 122.4(9) . . ? C5 C6 H6A 118.8 . . ? C7 C6 H6A 118.8 . . ? C8 C7 C6 121.0(8) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C7 C8 C9 116.6(7) . . ? C7 C8 C11 123.9(7) . . ? C9 C8 C11 119.4(7) . . ? C8 C9 C10 122.4(8) . . ? C8 C9 H9A 118.8 . . ? C10 C9 H9A 118.8 . . ? C5 C10 C9 119.6(8) . . ? C5 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C16 C11 C12 114.2(7) . . ? C16 C11 C8 121.7(8) . . ? C12 C11 C8 124.2(7) . . ? N1 C12 C13 105.1(6) . . ? N1 C12 C11 131.5(7) . . ? C13 C12 C11 123.2(7) . . ? C12 C13 N2 110.5(6) . . ? C12 C13 C14 121.1(7) . . ? N2 C13 C14 128.3(6) . . ? C15 C14 C13 114.3(7) . . ? C15 C14 C17 122.4(8) . . ? C13 C14 C17 123.3(7) . . ? C16 C15 C14 122.1(8) . . ? C16 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C15 C16 C11 124.7(8) . . ? C15 C16 H16A 117.6 . . ? C11 C16 H16A 117.6 . . ? C18 C17 C22 115.8(7) . . ? C18 C17 C14 125.1(7) . . ? C22 C17 C14 119.1(7) . . ? C17 C18 C19 121.0(8) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C20 C19 C18 123.1(9) . . ? C20 C19 H19A 118.4 . . ? C18 C19 H19A 118.4 . . ? C21 C20 C19 115.5(7) . . ? C21 C20 C23 123.4(8) . . ? C19 C20 C23 121.1(9) . . ? C22 C21 C20 121.6(8) . . ? C22 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? C21 C22 C17 123.0(9) . . ? C21 C22 H22A 118.5 . . ? C17 C22 H22A 118.5 . . ? C24 C23 C25 108.6(13) . . ? C24 C23 C26 111.5(17) . . ? C25 C23 C26 105.3(15) . . ? C24 C23 C20 110.3(9) . . ? C25 C23 C20 111.5(8) . . ? C26 C23 C20 109.5(10) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 N1 111.9(6) . . ? N2 C27 C28 124.0(6) . . ? N1 C27 C28 124.0(6) . . ? C29 C28 C33 118.8(7) . . ? C29 C28 C27 120.6(7) . . ? C33 C28 C27 120.6(6) . . ? C30 C29 C28 121.0(8) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C31 120.7(7) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C30 C31 C32 118.3(7) . . ? C30 C31 C34 120.0(7) . . ? C32 C31 C34 121.7(7) . . ? C33 C32 C31 121.1(7) . . ? C33 C32 H32A 119.5 . . ? C31 C32 H32A 119.5 . . ? C32 C33 C28 120.0(7) . . ? C32 C33 H33A 120.0 . . ? C28 C33 H33A 120.0 . . ? N3 C34 N4 111.9(7) . . ? N3 C34 C31 121.9(7) . . ? N4 C34 C31 126.0(6) . . ? C38 C35 H35A 109.5 . . ? C38 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C38 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 H36A 109.5 . . ? C38 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C38 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 C37 114.8(14) . . ? C35 C38 C36 109.4(14) . . ? C37 C38 C36 102.6(14) . . ? C35 C38 C39 109.5(9) . . ? C37 C38 C39 108.7(10) . . ? C36 C38 C39 111.8(10) . . ? C40 C39 C44 115.2(10) . . ? C40 C39 C38 123.1(11) . . ? C44 C39 C38 121.7(11) . . ? C39 C40 C41 125.3(10) . . ? C39 C40 H40A 117.4 . . ? C41 C40 H40A 117.4 . . ? C40 C41 C42 121.0(10) . . ? C40 C41 H41A 119.5 . . ? C42 C41 H41A 119.5 . . ? C41 C42 C43 115.0(8) . . ? C41 C42 C45 122.6(8) . . ? C43 C42 C45 122.3(8) . . ? C42 C43 C44 123.5(10) . . ? C42 C43 H43A 118.3 . . ? C44 C43 H43A 118.3 . . ? C43 C44 C39 120.1(11) . . ? C43 C44 H44A 120.0 . . ? C39 C44 H44A 120.0 . . ? C46 C45 C50 115.8(8) . . ? C46 C45 C42 121.0(8) . . ? C50 C45 C42 123.1(8) . . ? C45 C46 C47 122.8(8) . . ? C45 C46 H46A 118.6 . . ? C47 C46 H46A 118.6 . . ? C48 C47 C46 120.9(8) . . ? C48 C47 H47A 119.6 . . ? C46 C47 H47A 119.6 . . ? C49 C48 C47 116.2(8) . . ? C49 C48 C51 126.0(7) . . ? C47 C48 C51 117.8(8) . . ? C48 C49 N4 129.0(7) . . ? C48 C49 C50 124.4(7) . . ? N4 C49 C50 106.6(6) . . ? N3 C50 C49 109.0(7) . . ? N3 C50 C45 130.9(8) . . ? C49 C50 C45 119.9(7) . . ? C56 C51 C52 116.8(8) . . ? C56 C51 C48 120.6(8) . . ? C52 C51 C48 122.5(8) . . ? C53 C52 C51 120.4(9) . . ? C53 C52 H52A 119.8 . . ? C51 C52 H52A 119.8 . . ? C52 C53 C54 123.5(10) . . ? C52 C53 H53A 118.3 . . ? C54 C53 H53A 118.3 . . ? C55 C54 C53 114.5(9) . . ? C55 C54 C57 126.0(10) . . ? C53 C54 C57 119.4(10) . . ? C54 C55 C56 123.9(9) . . ? C54 C55 H55A 118.0 . . ? C56 C55 H55A 118.0 . . ? C55 C56 C51 120.9(9) . . ? C55 C56 H56A 119.6 . . ? C51 C56 H56A 119.6 . . ? C58 C57 C60 107.1(13) . . ? C58 C57 C59 109.0(14) . . ? C60 C57 C59 109.8(13) . . ? C58 C57 C54 111.9(11) . . ? C60 C57 C54 109.0(10) . . ? C59 C57 C54 109.9(11) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C70 O1 C71 115.1(10) . . ? C72 O2 C73 114.0(17) . . ? C75 O3 C74 117(3) . . ? C77 O4 C76 115.3(9) . . ? C86 O5 C87 118.9(9) . . ? C88 O6 C89 112.4(9) . . ? C90 O7 C91 114.2(10) . . ? C61 O8 C92 115.0(10) . . ? C62 C61 O8 123.2(13) . . ? C62 C61 C70 121.6(11) . . ? O8 C61 C70 115.2(11) . . ? C61 C62 C63 119.1(14) . . ? C61 C62 H62A 120.4 . . ? C63 C62 H62A 120.4 . . ? C68 C63 C64 123.3(16) . . ? C68 C63 C62 118.8(15) . . ? C64 C63 C62 117.8(17) . . ? C63 C64 C65 122(2) . . ? C63 C64 H64A 118.8 . . ? C65 C64 H64A 118.8 . . ? C66 C65 C64 115(2) . . ? C66 C65 H65A 122.7 . . ? C64 C65 H65A 122.7 . . ? C67 C66 C65 123.3(19) . . ? C67 C66 H66A 118.4 . . ? C65 C66 H66A 118.4 . . ? C66 C67 C68 123(2) . . ? C66 C67 H67A 118.6 . . ? C68 C67 H67A 118.6 . . ? C69 C68 C63 120.1(14) . . ? C69 C68 C67 126.3(15) . . ? C63 C68 C67 113.4(16) . . ? C68 C69 C70 124.1(13) . . ? C68 C69 H69A 117.9 . . ? C70 C69 H69A 117.9 . . ? O1 C70 C69 127.6(11) . . ? O1 C70 C61 116.3(9) . . ? C69 C70 C61 116.2(12) . . ? O1 C71 C72 106.6(13) . . ? O1 C71 H71A 110.4 . . ? C72 C71 H71A 110.4 . . ? O1 C71 H71B 110.4 . . ? C72 C71 H71B 110.4 . . ? H71A C71 H71B 108.6 . . ? O2 C72 C71 111(2) . . ? O2 C72 H72A 109.5 . . ? C71 C72 H72A 109.5 . . ? O2 C72 H72B 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 108.1 . . ? C74 C73 O2 102(2) . . ? C74 C73 H73A 111.3 . . ? O2 C73 H73A 111.3 . . ? C74 C73 H73B 111.3 . . ? O2 C73 H73B 111.3 . . ? H73A C73 H73B 109.2 . . ? C73 C74 O3 117(3) . . ? C73 C74 H74A 107.9 . . ? O3 C74 H74A 107.9 . . ? C73 C74 H74B 107.9 . . ? O3 C74 H74B 107.9 . . ? H74A C74 H74B 107.2 . . ? O3 C75 C76 135(2) . . ? O3 C75 H75A 103.5 . . ? C76 C75 H75A 103.5 . . ? O3 C75 H75B 103.5 . . ? C76 C75 H75B 103.5 . . ? H75A C75 H75B 105.3 . . ? C75 C76 O4 107.9(12) . . ? C75 C76 H76A 110.1 . . ? O4 C76 H76A 110.1 . . ? C75 C76 H76B 110.1 . . ? O4 C76 H76B 110.1 . . ? H76A C76 H76B 108.4 . . ? O4 C77 C78 123.6(12) . . ? O4 C77 C86 116.2(10) . . ? C78 C77 C86 120.2(13) . . ? C77 C78 C79 125.8(13) . . ? C77 C78 H78A 117.1 . . ? C79 C78 H78A 117.1 . . ? C80 C79 C84 120.0 . . ? C80 C79 C78 126.0(10) . . ? C84 C79 C78 114.0(10) . . ? C81 C80 C79 120.0 . . ? C81 C80 H80A 120.0 . . ? C79 C80 H80A 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81A 120.0 . . ? C82 C81 H81A 120.0 . . ? C81 C82 C83 120.0 . . ? C81 C82 H82A 120.0 . . ? C83 C82 H82A 120.0 . . ? C84 C83 C82 120.0 . . ? C84 C83 H83A 120.0 . . ? C82 C83 H83A 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 C85 117.9(9) . . ? C79 C84 C85 122.0(9) . . ? C86 C85 C84 119.4(12) . . ? C86 C85 H85A 120.3 . . ? C84 C85 H85A 120.3 . . ? C85 C86 O5 128.4(12) . . ? C85 C86 C77 118.4(13) . . ? O5 C86 C77 113.2(10) . . ? O5 C87 C88 108.3(10) . . ? O5 C87 H87A 110.0 . . ? C88 C87 H87A 110.0 . . ? O5 C87 H87B 110.0 . . ? C88 C87 H87B 110.0 . . ? H87A C87 H87B 108.4 . . ? O6 C88 C87 105.4(12) . . ? O6 C88 H88A 110.7 . . ? C87 C88 H88A 110.7 . . ? O6 C88 H88B 110.7 . . ? C87 C88 H88B 110.7 . . ? H88A C88 H88B 108.8 . . ? C90 C89 O6 104.0(10) . . ? C90 C89 H89A 111.0 . . ? O6 C89 H89A 111.0 . . ? C90 C89 H89B 111.0 . . ? O6 C89 H89B 111.0 . . ? H89A C89 H89B 109.0 . . ? C89 C90 O7 106.5(12) . . ? C89 C90 H90A 110.4 . . ? O7 C90 H90A 110.4 . . ? C89 C90 H90B 110.4 . . ? O7 C90 H90B 110.4 . . ? H90A C90 H90B 108.6 . . ? O7 C91 C92 108.3(12) . . ? O7 C91 H91A 110.0 . . ? C92 C91 H91A 110.0 . . ? O7 C91 H91B 110.0 . . ? C92 C91 H91B 110.0 . . ? H91A C91 H91B 108.4 . . ? O8 C92 C91 107.6(11) . . ? O8 C92 H92A 110.2 . . ? C91 C92 H92A 110.2 . . ? O8 C92 H92B 110.2 . . ? C91 C92 H92B 110.2 . . ? H92A C92 H92B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.871 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.082 # Attachment '- 891819.cif' data_kz92 _database_code_depnum_ccdc_archive 'CCDC 891919' #TrackingRef '- 891819.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76.50 H96.50 B2 Cl1.50 F8 N4 O8' _chemical_formula_weight 1426.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.833(2) _cell_length_b 29.043(4) _cell_length_c 38.755(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.751(2) _cell_angle_gamma 90.00 _cell_volume 15428(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 681 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6040 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9669 _exptl_absorpt_correction_T_max 0.9805 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 70770 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13565 _reflns_number_gt 7009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _refine_special_details ; ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.032 0.250 35 2 ' ' 2 0.500 0.202 0.750 129 46 ' ' 3 0.966 0.200 0.686 15 0 ' ' 4 0.034 0.200 0.814 15 0 ' ' 5 0.750 0.250 0.500 52 7 ' ' 6 0.250 0.250 1.000 52 7 ' ' 7 0.000 0.298 0.250 129 46 ' ' 8 0.466 0.300 0.186 15 0 ' ' 9 0.534 0.300 0.314 15 0 ' ' 10 0.500 0.468 0.750 35 2 ' ' 11 0.500 0.532 0.250 35 2 ' ' 12 0.000 0.702 0.750 129 46 ' ' 13 0.466 0.700 0.686 15 0 ' ' 14 0.534 0.700 0.814 15 0 ' ' 15 0.250 0.750 0.500 52 7 ' ' 16 0.750 0.750 1.000 52 7 ' ' 17 0.500 0.798 0.250 129 46 ' ' 18 0.966 0.800 0.186 15 0 ' ' 19 0.034 0.800 0.314 15 0 ' ' 20 0.000 0.968 0.750 35 2 ' ' _platon_squeeze_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Both BF4- anoins were treated as rigid groups using DFIX, SADI, DELU and SIMU restraints. One of the BF4- anions was disordered over two sites and refined with sofs of 1/3 nd 2/3. Residual electron density in the lattice appeared to be CHCL3 but could not be modeled satisfactorily. The unit cell was calculated to contain an estimated 4 molecules of CHCL3 which were treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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^)+(0.1939P)^2^+35.8923P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13565 _refine_ls_number_parameters 928 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.2103 _refine_ls_R_factor_gt 0.1356 _refine_ls_wR_factor_ref 0.3923 _refine_ls_wR_factor_gt 0.3416 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _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 N1 N 0.5696(4) 0.90533(15) 0.08738(12) 0.0379(12) Uani 1 1 d . . . H1D H 0.5409 0.8810 0.0770 0.045 Uiso 1 1 calc R . . N2 N 0.6706(4) 0.94662(15) 0.12136(12) 0.0371(12) Uani 1 1 d . . . H2D H 0.7181 0.9545 0.1377 0.044 Uiso 1 1 calc R . . N3 N 0.7669(4) 0.69827(16) 0.17501(13) 0.0425(13) Uani 1 1 d . . . H3D H 0.7416 0.6901 0.1538 0.051 Uiso 1 1 calc R . . N4 N 0.8179(4) 0.74053(16) 0.22004(13) 0.0475(14) Uani 1 1 d . . . H4A H 0.8327 0.7649 0.2332 0.057 Uiso 1 1 calc R . . C1 C 0.0636(7) 0.8765(5) -0.0060(3) 0.111(4) Uani 1 1 d . . . H1A H 0.0509 0.9093 -0.0103 0.166 Uiso 1 1 calc R . . H1B H 0.0719 0.8706 0.0191 0.166 Uiso 1 1 calc R . . H1C H 0.0085 0.8584 -0.0174 0.166 Uiso 1 1 calc R . . C2 C 0.1423(7) 0.8691(3) -0.0595(2) 0.087(3) Uani 1 1 d . . . H2A H 0.1311 0.9018 -0.0650 0.130 Uiso 1 1 calc R . . H2B H 0.0860 0.8511 -0.0700 0.130 Uiso 1 1 calc R . . H2C H 0.2009 0.8587 -0.0690 0.130 Uiso 1 1 calc R . . C3 C 0.1737(10) 0.8107(3) -0.0134(3) 0.131(5) Uani 1 1 d . . . H3A H 0.2330 0.8010 -0.0227 0.196 Uiso 1 1 calc R . . H3B H 0.1178 0.7931 -0.0248 0.196 Uiso 1 1 calc R . . H3C H 0.1812 0.8053 0.0117 0.196 Uiso 1 1 calc R . . C4 C 0.1563(5) 0.8627(2) -0.02072(17) 0.0550(18) Uani 1 1 d . . . C5 C 0.2410(5) 0.8900(2) -0.00211(14) 0.0380(14) Uani 1 1 d . . . C6 C 0.2783(4) 0.8795(2) 0.03193(16) 0.0403(14) Uani 1 1 d . . . H6A H 0.2519 0.8541 0.0429 0.048 Uiso 1 1 calc R . . C7 C 0.3523(4) 0.9046(2) 0.05059(15) 0.0403(14) Uani 1 1 d . . . H7A H 0.3756 0.8965 0.0740 0.048 Uiso 1 1 calc R . . C8 C 0.3929(4) 0.9420(2) 0.03508(15) 0.0373(14) Uani 1 1 d . . . C9 C 0.3553(5) 0.9530(2) 0.00135(15) 0.0437(15) Uani 1 1 d . . . H9A H 0.3800 0.9790 -0.0095 0.052 Uiso 1 1 calc R . . C10 C 0.2821(5) 0.9268(2) -0.01684(16) 0.0466(16) Uani 1 1 d . . . H10A H 0.2594 0.9346 -0.0404 0.056 Uiso 1 1 calc R . . C11 C 0.4701(5) 0.96992(19) 0.05555(15) 0.0397(14) Uani 1 1 d . . . C12 C 0.5452(5) 0.95084(19) 0.07884(15) 0.0388(14) Uani 1 1 d . . . C13 C 0.6128(4) 0.97724(19) 0.09945(15) 0.0372(14) Uani 1 1 d . . . C14 C 0.6154(4) 1.02568(19) 0.09773(15) 0.0357(13) Uani 1 1 d . . . C15 C 0.5418(5) 1.04475(19) 0.07470(16) 0.0414(15) Uani 1 1 d . . . H15A H 0.5390 1.0773 0.0723 0.050 Uiso 1 1 calc R . . C16 C 0.4715(5) 1.0183(2) 0.05487(17) 0.0477(16) Uani 1 1 d . . . H16A H 0.4215 1.0337 0.0400 0.057 Uiso 1 1 calc R . . C17 C 0.6913(5) 1.05421(18) 0.11809(16) 0.0388(14) Uani 1 1 d . . . C18 C 0.7888(5) 1.0419(2) 0.12346(15) 0.0408(15) Uani 1 1 d . . . H18A H 0.8078 1.0135 0.1142 0.049 Uiso 1 1 calc R . . C19 C 0.8592(5) 1.06924(19) 0.14163(15) 0.0395(14) Uani 1 1 d . . . H19A H 0.9254 1.0595 0.1443 0.047 Uiso 1 1 calc R . . C20 C 0.8355(5) 1.11051(19) 0.15604(15) 0.0402(14) Uani 1 1 d . . . C21 C 0.7382(5) 1.1236(2) 0.15031(16) 0.0434(15) Uani 1 1 d . . . H21A H 0.7201 1.1525 0.1590 0.052 Uiso 1 1 calc R . . C22 C 0.6675(5) 1.09650(19) 0.13260(16) 0.0430(15) Uani 1 1 d . . . H22A H 0.6015 1.1063 0.1300 0.052 Uiso 1 1 calc R . . C23 C 0.9114(5) 1.1417(2) 0.17724(17) 0.0494(17) Uani 1 1 d . . . C24 C 1.0127(6) 1.1218(3) 0.1812(2) 0.076(2) Uani 1 1 d . . . H24A H 1.0128 1.0917 0.1927 0.114 Uiso 1 1 calc R . . H24B H 1.0577 1.1425 0.1953 0.114 Uiso 1 1 calc R . . H24C H 1.0335 1.1181 0.1582 0.114 Uiso 1 1 calc R . . C25 C 0.8812(6) 1.1500(3) 0.2132(2) 0.068(2) Uani 1 1 d . . . H25A H 0.8796 1.1206 0.2255 0.103 Uiso 1 1 calc R . . H25B H 0.8164 1.1641 0.2107 0.103 Uiso 1 1 calc R . . H25C H 0.9285 1.1706 0.2266 0.103 Uiso 1 1 calc R . . C26 C 0.9128(7) 1.1889(3) 0.1591(2) 0.075(2) Uani 1 1 d . . . H26A H 0.9611 1.2089 0.1726 0.112 Uiso 1 1 calc R . . H26B H 0.8481 1.2031 0.1577 0.112 Uiso 1 1 calc R . . H26C H 0.9301 1.1848 0.1356 0.112 Uiso 1 1 calc R . . C27 C 0.6420(4) 0.90396(18) 0.11336(14) 0.0357(13) Uani 1 1 d . . . C28 C 0.6807(4) 0.86239(18) 0.13107(15) 0.0371(14) Uani 1 1 d . . . C29 C 0.7046(4) 0.82356(19) 0.11322(15) 0.0384(14) Uani 1 1 d . . . H29A H 0.6977 0.8237 0.0885 0.046 Uiso 1 1 calc R . . C30 C 0.7384(5) 0.7847(2) 0.13135(17) 0.0440(15) Uani 1 1 d . . . H30A H 0.7574 0.7587 0.1190 0.053 Uiso 1 1 calc R . . C31 C 0.7449(5) 0.78303(19) 0.16724(16) 0.0408(14) Uani 1 1 d . . . C32 C 0.7209(6) 0.8225(2) 0.18502(17) 0.0573(19) Uani 1 1 d . . . H32A H 0.7260 0.8221 0.2097 0.069 Uiso 1 1 calc R . . C33 C 0.6902(5) 0.8613(2) 0.16732(17) 0.0518(18) Uani 1 1 d . . . H33A H 0.6751 0.8879 0.1798 0.062 Uiso 1 1 calc R . . C34 C 0.7768(5) 0.7415(2) 0.18696(17) 0.0447(15) Uani 1 1 d . . . C35 C 0.5364(6) 0.5207(3) 0.0807(2) 0.082(3) Uani 1 1 d . . . H35A H 0.5001 0.5040 0.0611 0.122 Uiso 1 1 calc R . . H35B H 0.5284 0.5539 0.0768 0.122 Uiso 1 1 calc R . . H35C H 0.5114 0.5121 0.1023 0.122 Uiso 1 1 calc R . . C36 C 0.6804(7) 0.5204(3) 0.0495(2) 0.075(2) Uani 1 1 d . . . H36A H 0.6447 0.5022 0.0306 0.113 Uiso 1 1 calc R . . H36B H 0.7502 0.5134 0.0512 0.113 Uiso 1 1 calc R . . H36C H 0.6698 0.5532 0.0446 0.113 Uiso 1 1 calc R . . C37 C 0.6574(6) 0.4568(3) 0.0900(2) 0.069(2) Uani 1 1 d . . . H37A H 0.6237 0.4397 0.0701 0.103 Uiso 1 1 calc R . . H37B H 0.6300 0.4483 0.1112 0.103 Uiso 1 1 calc R . . H37C H 0.7271 0.4493 0.0929 0.103 Uiso 1 1 calc R . . C38 C 0.6440(5) 0.5083(2) 0.0835(2) 0.0583(19) Uani 1 1 d . . . C39 C 0.6968(5) 0.5355(2) 0.11463(18) 0.0532(18) Uani 1 1 d . . . C40 C 0.6769(5) 0.5260(2) 0.14796(18) 0.0522(17) Uani 1 1 d . . . H40A H 0.6362 0.5006 0.1515 0.063 Uiso 1 1 calc R . . C41 C 0.7150(5) 0.5525(2) 0.17611(19) 0.0539(18) Uani 1 1 d . . . H41A H 0.7007 0.5447 0.1987 0.065 Uiso 1 1 calc R . . C42 C 0.7734(5) 0.5902(2) 0.17216(17) 0.0440(15) Uani 1 1 d . . . C43 C 0.7966(5) 0.5993(2) 0.13878(18) 0.0522(17) Uani 1 1 d . . . H43A H 0.8385 0.6242 0.1352 0.063 Uiso 1 1 calc R . . C44 C 0.7586(5) 0.5718(2) 0.11085(18) 0.0503(17) Uani 1 1 d . . . H44A H 0.7757 0.5783 0.0884 0.060 Uiso 1 1 calc R . . C45 C 0.8101(5) 0.6194(2) 0.20224(17) 0.0450(16) Uani 1 1 d . . . C46 C 0.8501(5) 0.6019(2) 0.23385(18) 0.0534(18) Uani 1 1 d . . . H46A H 0.8585 0.5695 0.2358 0.064 Uiso 1 1 calc R . . C47 C 0.8791(5) 0.6285(2) 0.26309(17) 0.0510(17) Uani 1 1 d . . . H47A H 0.9052 0.6134 0.2841 0.061 Uiso 1 1 calc R . . C48 C 0.8715(5) 0.6770(2) 0.26302(17) 0.0470(16) Uani 1 1 d . . . C49 C 0.8338(5) 0.6946(2) 0.23062(17) 0.0454(16) Uani 1 1 d . . . C50 C 0.8035(5) 0.6683(2) 0.20171(16) 0.0428(15) Uani 1 1 d . . . C51 C 0.8929(5) 0.7030(2) 0.29537(17) 0.0485(16) Uani 1 1 d . . . C52 C 0.9686(5) 0.6898(2) 0.32179(17) 0.0495(16) Uani 1 1 d . . . H52A H 1.0130 0.6665 0.3170 0.059 Uiso 1 1 calc R . . C53 C 0.9797(5) 0.7099(3) 0.35426(18) 0.0561(18) Uani 1 1 d . . . H53A H 1.0308 0.6996 0.3714 0.067 Uiso 1 1 calc R . . C54 C 0.9181(5) 0.7446(2) 0.36257(19) 0.0565(18) Uani 1 1 d . . . C55 C 0.8459(6) 0.7593(2) 0.33604(19) 0.0567(18) Uani 1 1 d . . . H55A H 0.8044 0.7841 0.3404 0.068 Uiso 1 1 calc R . . C56 C 0.8337(5) 0.7385(2) 0.30350(18) 0.0552(18) Uani 1 1 d . . . H56A H 0.7830 0.7490 0.2863 0.066 Uiso 1 1 calc R . . C57 C 0.9262(6) 0.7647(3) 0.3993(2) 0.067(2) Uani 1 1 d . . . C58 C 0.8843(11) 0.7286(4) 0.4218(3) 0.132(5) Uani 1 1 d . . . H58A H 0.8165 0.7221 0.4122 0.198 Uiso 1 1 calc R . . H58B H 0.8866 0.7404 0.4456 0.198 Uiso 1 1 calc R . . H58C H 0.9229 0.7003 0.4221 0.198 Uiso 1 1 calc R . . C59 C 1.0323(7) 0.7756(4) 0.4138(3) 0.093(3) Uani 1 1 d . . . H59A H 1.0719 0.7476 0.4133 0.140 Uiso 1 1 calc R . . H59B H 1.0354 0.7866 0.4378 0.140 Uiso 1 1 calc R . . H59C H 1.0574 0.7994 0.3994 0.140 Uiso 1 1 calc R . . C60 C 0.8681(6) 0.8093(3) 0.4006(2) 0.092(3) Uani 1 1 d . . . H60A H 0.7996 0.8036 0.3915 0.137 Uiso 1 1 calc R . . H60B H 0.8947 0.8328 0.3863 0.137 Uiso 1 1 calc R . . H60C H 0.8728 0.8201 0.4247 0.137 Uiso 1 1 calc R . . O1 O 0.5138(4) 0.82157(18) 0.05352(17) 0.0871(19) Uani 1 1 d . . . O2 O 0.6708(6) 0.8623(3) 0.02720(16) 0.096(2) Uani 1 1 d . . . O3 O 0.8214(5) 0.9031(2) 0.07543(18) 0.0909(19) Uani 1 1 d . . . O4 O 0.8827(5) 0.9343(2) 0.14711(19) 0.091(2) Uani 1 1 d . . . O5 O 0.7591(6) 0.97014(18) 0.19141(14) 0.090(2) Uani 1 1 d . . . O6 O 0.5464(10) 0.9713(3) 0.1997(3) 0.162(4) Uani 1 1 d . . . O7 O 0.4471(5) 0.9152(3) 0.14660(16) 0.097(2) Uani 1 1 d . . . O8 O 0.4206(4) 0.8300(2) 0.11148(19) 0.095(2) Uani 1 1 d . . . C61 C 0.5258(11) 0.8156(5) 0.0186(4) 0.137(6) Uani 1 1 d . . . H61A H 0.4613 0.8128 0.0042 0.164 Uiso 1 1 calc R . . H61B H 0.5631 0.7870 0.0158 0.164 Uiso 1 1 calc R . . C62 C 0.5764(13) 0.8538(6) 0.0078(3) 0.148(6) Uani 1 1 d . . . H62A H 0.5355 0.8816 0.0092 0.177 Uiso 1 1 calc R . . H62B H 0.5846 0.8495 -0.0170 0.177 Uiso 1 1 calc R . . C63 C 0.7225(12) 0.8996(5) 0.0206(3) 0.132(5) Uani 1 1 d . . . H63A H 0.6885 0.9273 0.0276 0.158 Uiso 1 1 calc R . . H63B H 0.7236 0.9016 -0.0049 0.158 Uiso 1 1 calc R . . C64 C 0.8204(10) 0.9004(5) 0.0375(3) 0.136(5) Uani 1 1 d . . . H64A H 0.8550 0.9273 0.0294 0.164 Uiso 1 1 calc R . . H64B H 0.8548 0.8722 0.0315 0.164 Uiso 1 1 calc R . . C65 C 0.9154(7) 0.9057(3) 0.0923(3) 0.099(3) Uani 1 1 d . . . H65A H 0.9414 0.9369 0.0887 0.119 Uiso 1 1 calc R . . H65B H 0.9564 0.8833 0.0816 0.119 Uiso 1 1 calc R . . C66 C 0.9239(7) 0.8966(4) 0.1300(3) 0.100(3) Uani 1 1 d . . . H66A H 0.8890 0.8678 0.1342 0.120 Uiso 1 1 calc R . . H66B H 0.9934 0.8927 0.1397 0.120 Uiso 1 1 calc R . . C67 C 0.9049(8) 0.9296(3) 0.1841(3) 0.111(4) Uani 1 1 d . . . H67A H 0.9764 0.9292 0.1911 0.133 Uiso 1 1 calc R . . H67B H 0.8774 0.9005 0.1919 0.133 Uiso 1 1 calc R . . C68 C 0.8602(10) 0.9705(3) 0.2006(3) 0.126(5) Uani 1 1 d . . . H68A H 0.8762 0.9689 0.2262 0.152 Uiso 1 1 calc R . . H68B H 0.8874 0.9995 0.1925 0.152 Uiso 1 1 calc R . . C69 C 0.7059(11) 1.0039(3) 0.2095(2) 0.134(6) Uani 1 1 d . . . H69A H 0.7356 1.0348 0.2085 0.161 Uiso 1 1 calc R . . H69B H 0.7066 0.9952 0.2342 0.161 Uiso 1 1 calc R . . C70 C 0.5924(8) 1.0039(4) 0.1888(3) 0.105(4) Uani 1 1 d . . . H70A H 0.5600 1.0334 0.1929 0.126 Uiso 1 1 calc R . . H70B H 0.5935 1.0005 0.1634 0.126 Uiso 1 1 calc R . . C71 C 0.4522(13) 0.9761(6) 0.1891(5) 0.182(8) Uani 1 1 d . . . H71A H 0.4349 1.0089 0.1918 0.219 Uiso 1 1 calc R . . H71B H 0.4159 0.9580 0.2048 0.219 Uiso 1 1 calc R . . C72 C 0.4210(8) 0.9633(5) 0.1560(3) 0.119(4) Uani 1 1 d . . . H72A H 0.4485 0.9850 0.1401 0.143 Uiso 1 1 calc R . . H72B H 0.3491 0.9665 0.1518 0.143 Uiso 1 1 calc R . . C73 C 0.3860(9) 0.8838(6) 0.1557(3) 0.122(5) Uani 1 1 d . . . H73A H 0.3205 0.8888 0.1425 0.146 Uiso 1 1 calc R . . H73B H 0.3805 0.8870 0.1808 0.146 Uiso 1 1 calc R . . C74 C 0.4200(9) 0.8369(7) 0.1488(3) 0.160(8) Uani 1 1 d . . . H74A H 0.4867 0.8323 0.1612 0.192 Uiso 1 1 calc R . . H74B H 0.3765 0.8140 0.1576 0.192 Uiso 1 1 calc R . . C75 C 0.4568(8) 0.7876(4) 0.1010(5) 0.126(5) Uani 1 1 d . . . H75A H 0.4176 0.7620 0.1088 0.151 Uiso 1 1 calc R . . H75B H 0.5252 0.7835 0.1119 0.151 Uiso 1 1 calc R . . C76 C 0.4523(8) 0.7862(3) 0.0638(4) 0.117(5) Uani 1 1 d . . . H76A H 0.4744 0.7558 0.0563 0.140 Uiso 1 1 calc R . . H76B H 0.3843 0.7912 0.0527 0.140 Uiso 1 1 calc R . . B1 B 0.6929(7) 0.6836(3) 0.0767(2) 0.094(3) Uani 1 1 d DU . . F1 F 0.6605(4) 0.68184(17) 0.10960(13) 0.0966(16) Uani 1 1 d DU . . F2 F 0.6565(4) 0.64676(18) 0.05691(14) 0.1061(18) Uani 1 1 d DU . . F3 F 0.6616(6) 0.72418(19) 0.06068(14) 0.151(3) Uani 1 1 d DU . . F4 F 0.7950(5) 0.6827(2) 0.08297(17) 0.127(2) Uani 1 1 d DU . . B2A B 0.8031(9) 0.8986(5) 0.2857(3) 0.136(6) Uani 0.67 1 d PDU A -1 F5A F 0.8754(9) 0.9021(4) 0.2659(3) 0.148(5) Uani 0.67 1 d PDU A -1 F6A F 0.7393(10) 0.8651(5) 0.2732(4) 0.246(8) Uani 0.67 1 d PDU A -1 F7A F 0.7591(10) 0.9408(4) 0.2853(3) 0.186(5) Uani 0.67 1 d PDU A -1 F8A F 0.8405(8) 0.8887(6) 0.3191(3) 0.224(8) Uani 0.67 1 d PDU A -1 B2B B 0.868(2) 0.8647(5) 0.2728(5) 0.214(15) Uani 0.33 1 d PDU B -2 F5B F 0.8737(13) 0.8220(3) 0.2562(3) 0.139(8) Uani 0.33 1 d PDU B -2 F6B F 0.858(2) 0.8600(5) 0.3081(4) 0.237(16) Uani 0.33 1 d PDU B -2 F7B F 0.792(3) 0.8928(6) 0.2569(5) 0.239(17) Uani 0.33 1 d PDU B -2 F8B F 0.957(2) 0.8878(10) 0.2709(9) 0.37(2) Uani 0.33 1 d PDU B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.057(3) 0.018(2) 0.040(3) -0.002(2) 0.010(2) -0.009(2) N2 0.047(3) 0.024(2) 0.038(3) 0.002(2) -0.003(2) 0.000(2) N3 0.057(3) 0.028(3) 0.043(3) 0.003(2) 0.010(3) 0.005(2) N4 0.078(4) 0.026(3) 0.038(3) 0.003(2) 0.005(3) 0.002(3) C1 0.066(6) 0.192(12) 0.073(6) -0.030(7) 0.003(5) -0.037(7) C2 0.100(7) 0.109(7) 0.047(5) -0.008(5) -0.003(5) -0.041(6) C3 0.217(14) 0.053(5) 0.098(8) -0.006(5) -0.066(8) -0.048(7) C4 0.069(5) 0.057(4) 0.036(4) -0.005(3) -0.006(3) -0.016(4) C5 0.052(4) 0.037(3) 0.025(3) -0.004(2) 0.004(3) -0.001(3) C6 0.047(4) 0.029(3) 0.044(4) -0.003(3) 0.004(3) -0.009(3) C7 0.050(4) 0.047(4) 0.024(3) 0.007(3) 0.009(3) -0.002(3) C8 0.042(3) 0.038(3) 0.033(3) -0.006(3) 0.009(3) 0.000(3) C9 0.059(4) 0.038(3) 0.033(3) 0.003(3) -0.002(3) -0.010(3) C10 0.060(4) 0.049(4) 0.030(3) 0.006(3) 0.001(3) -0.002(3) C11 0.051(4) 0.026(3) 0.041(4) 0.001(3) 0.005(3) -0.005(3) C12 0.054(4) 0.030(3) 0.034(3) -0.002(3) 0.011(3) 0.000(3) C13 0.047(4) 0.028(3) 0.037(3) -0.001(2) 0.008(3) -0.001(3) C14 0.037(3) 0.030(3) 0.040(3) -0.006(2) 0.005(3) -0.001(2) C15 0.057(4) 0.022(3) 0.045(4) -0.004(3) 0.005(3) -0.008(3) C16 0.060(4) 0.037(3) 0.046(4) 0.006(3) 0.007(3) 0.004(3) C17 0.053(4) 0.020(3) 0.045(4) 0.004(2) 0.015(3) -0.003(3) C18 0.055(4) 0.026(3) 0.042(4) -0.003(3) 0.013(3) 0.009(3) C19 0.044(4) 0.031(3) 0.043(4) 0.004(3) 0.002(3) -0.004(3) C20 0.054(4) 0.028(3) 0.038(3) 0.005(2) 0.008(3) 0.001(3) C21 0.058(4) 0.026(3) 0.044(4) -0.010(3) 0.000(3) -0.003(3) C22 0.046(4) 0.030(3) 0.052(4) -0.003(3) 0.003(3) 0.010(3) C23 0.054(4) 0.043(4) 0.049(4) 0.001(3) -0.001(3) -0.011(3) C24 0.056(5) 0.069(5) 0.098(7) -0.024(5) -0.004(4) -0.014(4) C25 0.067(5) 0.074(5) 0.061(5) -0.008(4) -0.004(4) -0.015(4) C26 0.094(6) 0.048(4) 0.080(6) 0.001(4) 0.001(5) -0.020(4) C27 0.049(4) 0.027(3) 0.030(3) -0.003(2) 0.000(3) -0.005(3) C28 0.046(4) 0.023(3) 0.042(4) 0.001(2) 0.008(3) -0.001(2) C29 0.052(4) 0.033(3) 0.030(3) -0.003(2) 0.005(3) -0.007(3) C30 0.054(4) 0.029(3) 0.051(4) -0.003(3) 0.015(3) -0.004(3) C31 0.057(4) 0.026(3) 0.041(4) 0.006(3) 0.013(3) 0.000(3) C32 0.096(6) 0.042(4) 0.035(4) -0.003(3) 0.011(4) 0.003(4) C33 0.086(5) 0.022(3) 0.050(4) -0.001(3) 0.016(4) 0.010(3) C34 0.054(4) 0.031(3) 0.051(4) 0.000(3) 0.013(3) 0.004(3) C35 0.079(6) 0.075(6) 0.087(6) -0.015(5) 0.000(5) 0.010(5) C36 0.103(7) 0.065(5) 0.059(5) -0.017(4) 0.015(5) -0.015(5) C37 0.079(6) 0.056(5) 0.072(5) -0.020(4) 0.010(4) 0.008(4) C38 0.055(4) 0.053(4) 0.070(5) -0.007(4) 0.021(4) 0.001(3) C39 0.062(4) 0.044(4) 0.058(4) -0.004(3) 0.021(4) 0.009(3) C40 0.064(5) 0.034(3) 0.062(5) 0.003(3) 0.022(4) -0.003(3) C41 0.069(5) 0.035(4) 0.061(5) 0.007(3) 0.022(4) 0.000(3) C42 0.054(4) 0.032(3) 0.049(4) 0.002(3) 0.018(3) 0.011(3) C43 0.068(5) 0.040(4) 0.051(4) 0.001(3) 0.015(3) -0.012(3) C44 0.054(4) 0.050(4) 0.051(4) 0.007(3) 0.020(3) -0.001(3) C45 0.056(4) 0.031(3) 0.051(4) 0.002(3) 0.017(3) 0.009(3) C46 0.074(5) 0.029(3) 0.058(4) 0.012(3) 0.012(4) 0.015(3) C47 0.070(5) 0.045(4) 0.038(4) 0.008(3) 0.007(3) 0.019(3) C48 0.058(4) 0.038(4) 0.045(4) 0.003(3) 0.007(3) 0.012(3) C49 0.059(4) 0.028(3) 0.052(4) 0.004(3) 0.021(3) 0.007(3) C50 0.052(4) 0.036(3) 0.042(4) 0.008(3) 0.013(3) 0.005(3) C51 0.068(5) 0.033(3) 0.048(4) 0.002(3) 0.021(3) 0.003(3) C52 0.046(4) 0.052(4) 0.052(4) -0.003(3) 0.012(3) 0.000(3) C53 0.057(4) 0.065(5) 0.047(4) 0.000(3) 0.009(3) -0.001(4) C54 0.058(4) 0.056(4) 0.058(5) -0.006(4) 0.020(4) -0.009(4) C55 0.072(5) 0.043(4) 0.059(5) -0.006(3) 0.021(4) 0.002(3) C56 0.070(5) 0.044(4) 0.050(4) 0.007(3) 0.003(4) 0.011(3) C57 0.071(5) 0.078(6) 0.055(5) -0.017(4) 0.017(4) -0.012(4) C58 0.210(14) 0.132(10) 0.059(6) -0.006(6) 0.039(7) -0.047(9) C59 0.084(7) 0.101(7) 0.092(7) -0.044(6) 0.005(5) -0.003(5) C60 0.074(6) 0.112(8) 0.091(7) -0.051(6) 0.022(5) -0.003(5) O1 0.095(4) 0.046(3) 0.109(5) -0.035(3) -0.026(4) 0.002(3) O2 0.114(6) 0.116(6) 0.057(4) 0.006(4) 0.014(4) 0.026(4) O3 0.073(4) 0.105(5) 0.099(5) 0.034(4) 0.030(4) -0.003(3) O4 0.088(4) 0.054(4) 0.118(5) 0.009(3) -0.030(4) -0.003(3) O5 0.147(6) 0.054(3) 0.056(3) 0.007(3) -0.032(4) -0.026(4) O6 0.221(12) 0.088(6) 0.176(10) -0.016(6) 0.026(9) 0.034(7) O7 0.072(4) 0.157(7) 0.064(4) -0.003(4) 0.018(3) 0.004(4) O8 0.078(4) 0.075(4) 0.127(6) 0.055(4) -0.006(4) -0.013(3) C61 0.174(13) 0.103(9) 0.116(11) -0.076(9) -0.043(9) 0.007(9) C62 0.203(17) 0.179(15) 0.054(7) -0.014(8) -0.006(9) 0.048(13) C63 0.155(13) 0.174(14) 0.074(8) 0.057(8) 0.040(8) 0.017(11) C64 0.117(10) 0.191(14) 0.116(10) 0.085(9) 0.070(8) 0.027(9) C65 0.073(7) 0.076(6) 0.153(11) 0.037(7) 0.035(7) 0.001(5) C66 0.065(6) 0.076(7) 0.152(11) 0.029(7) -0.013(6) -0.007(5) C67 0.107(8) 0.070(7) 0.134(10) 0.028(6) -0.062(7) -0.001(6) C68 0.206(14) 0.060(6) 0.086(7) 0.025(5) -0.081(8) -0.034(7) C69 0.285(18) 0.059(6) 0.046(5) -0.032(4) -0.027(8) 0.027(8) C70 0.102(8) 0.104(8) 0.116(9) 0.064(7) 0.041(7) 0.015(6) C71 0.162(15) 0.206(18) 0.168(16) -0.064(13) -0.011(12) 0.112(14) C72 0.103(8) 0.194(13) 0.061(6) -0.007(7) 0.012(6) 0.065(9) C73 0.098(9) 0.209(16) 0.063(7) 0.054(8) 0.028(6) 0.023(10) C74 0.098(9) 0.27(2) 0.110(10) 0.144(13) -0.011(7) -0.070(11) C75 0.080(7) 0.055(7) 0.233(16) 0.063(9) -0.015(9) -0.028(5) C76 0.081(7) 0.036(5) 0.220(15) -0.024(7) -0.031(9) -0.018(5) B1 0.133(8) 0.060(6) 0.080(6) -0.027(5) -0.025(6) 0.041(6) F1 0.114(4) 0.078(3) 0.091(3) -0.015(3) -0.010(3) 0.004(3) F2 0.124(4) 0.085(3) 0.099(4) -0.024(3) -0.022(3) 0.002(3) F3 0.274(9) 0.088(4) 0.077(4) 0.001(3) -0.025(4) 0.060(5) F4 0.126(4) 0.108(5) 0.145(6) 0.036(4) 0.008(4) -0.022(4) B2A 0.064(11) 0.203(15) 0.139(13) 0.004(17) 0.003(8) 0.036(9) F5A 0.187(11) 0.123(10) 0.146(11) 0.000(8) 0.071(10) 0.008(8) F6A 0.209(13) 0.298(15) 0.264(16) -0.183(15) 0.147(11) -0.070(12) F7A 0.223(14) 0.173(10) 0.172(11) 0.025(8) 0.068(10) 0.050(9) F8A 0.097(8) 0.40(2) 0.174(9) 0.164(13) 0.013(7) -0.007(10) B2B 0.41(4) 0.09(2) 0.124(17) -0.018(18) -0.06(3) -0.045(18) F5B 0.28(2) 0.025(6) 0.073(8) 0.034(5) -0.132(11) -0.065(8) F6B 0.54(5) 0.036(9) 0.092(11) -0.010(8) -0.122(16) -0.058(16) F7B 0.59(5) 0.036(10) 0.077(13) 0.020(9) -0.02(2) 0.035(18) F8B 0.55(5) 0.17(3) 0.39(5) -0.10(3) 0.02(4) -0.21(3) _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 N1 C27 1.322(7) . ? N1 C12 1.393(7) . ? N1 H1D 0.8800 . ? N2 C27 1.325(7) . ? N2 C13 1.403(7) . ? N2 H2D 0.8800 . ? N3 C34 1.339(7) . ? N3 C50 1.394(7) . ? N3 H3D 0.8800 . ? N4 C34 1.330(8) . ? N4 C49 1.403(7) . ? N4 H4A 0.8800 . ? C1 C4 1.525(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.503(10) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.547(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.516(9) . ? C5 C10 1.370(8) . ? C5 C6 1.384(8) . ? C6 C7 1.379(8) . ? C6 H6A 0.9500 . ? C7 C8 1.394(8) . ? C7 H7A 0.9500 . ? C8 C9 1.378(8) . ? C8 C11 1.483(8) . ? C9 C10 1.381(8) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.396(8) . ? C11 C16 1.405(8) . ? C12 C13 1.378(8) . ? C13 C14 1.409(8) . ? C14 C15 1.377(8) . ? C14 C17 1.479(8) . ? C15 C16 1.388(9) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.383(8) . ? C17 C22 1.408(8) . ? C18 C19 1.374(8) . ? C18 H18A 0.9500 . ? C19 C20 1.380(8) . ? C19 H19A 0.9500 . ? C20 C21 1.388(9) . ? C20 C23 1.537(9) . ? C21 C22 1.366(8) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.505(10) . ? C23 C25 1.527(10) . ? C23 C26 1.542(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.455(8) . ? C28 C29 1.386(8) . ? C28 C33 1.394(9) . ? C29 C30 1.376(8) . ? C29 H29A 0.9500 . ? C30 C31 1.382(8) . ? C30 H30A 0.9500 . ? C31 C32 1.401(9) . ? C31 C34 1.464(8) . ? C32 C33 1.356(9) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C35 C38 1.521(11) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.516(10) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.523(10) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.541(10) . ? C39 C44 1.377(9) . ? C39 C40 1.385(9) . ? C40 C41 1.381(9) . ? C40 H40A 0.9500 . ? C41 C42 1.380(9) . ? C41 H41A 0.9500 . ? C42 C43 1.399(9) . ? C42 C45 1.477(9) . ? C43 C44 1.390(9) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.373(9) . ? C45 C50 1.422(8) . ? C46 C47 1.385(9) . ? C46 H46A 0.9500 . ? C47 C48 1.412(8) . ? C47 H47A 0.9500 . ? C48 C49 1.391(9) . ? C48 C51 1.460(9) . ? C49 C50 1.375(9) . ? C51 C56 1.379(9) . ? C51 C52 1.415(9) . ? C52 C53 1.376(9) . ? C52 H52A 0.9500 . ? C53 C54 1.385(10) . ? C53 H53A 0.9500 . ? C54 C55 1.401(10) . ? C54 C57 1.528(10) . ? C55 C56 1.388(9) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C58 1.526(13) . ? C57 C60 1.530(12) . ? C57 C59 1.531(11) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O1 C61 1.396(15) . ? O1 C76 1.423(13) . ? O2 C63 1.342(14) . ? O2 C62 1.438(17) . ? O3 C65 1.377(11) . ? O3 C64 1.471(13) . ? O4 C67 1.432(12) . ? O4 C66 1.436(12) . ? O5 C68 1.396(14) . ? O5 C69 1.461(12) . ? O6 C70 1.247(13) . ? O6 C71 1.320(16) . ? O7 C73 1.324(15) . ? O7 C72 1.501(14) . ? O8 C75 1.410(14) . ? O8 C74 1.461(16) . ? C61 C62 1.407(19) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.423(16) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.474(14) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.518(16) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.664(16) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.351(16) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.48(2) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.436(16) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? B1 F2 1.372(8) . ? B1 F3 1.376(8) . ? B1 F4 1.402(9) . ? B1 F1 1.407(9) . ? B2A F5A 1.343(11) . ? B2A F8A 1.356(11) . ? B2A F6A 1.359(11) . ? B2A F7A 1.367(11) . ? B2B F6B 1.400(13) . ? B2B F5B 1.404(13) . ? B2B F7B 1.408(13) . ? B2B F8B 1.416(13) . ? 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 C27 N1 C12 110.1(5) . . ? C27 N1 H1D 125.0 . . ? C12 N1 H1D 125.0 . . ? C27 N2 C13 108.9(5) . . ? C27 N2 H2D 125.6 . . ? C13 N2 H2D 125.6 . . ? C34 N3 C50 108.6(5) . . ? C34 N3 H3D 125.7 . . ? C50 N3 H3D 125.7 . . ? C34 N4 C49 109.4(5) . . ? C34 N4 H4A 125.3 . . ? C49 N4 H4A 125.3 . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C5 113.4(6) . . ? C2 C4 C1 109.9(7) . . ? C5 C4 C1 108.6(6) . . ? C2 C4 C3 107.4(7) . . ? C5 C4 C3 109.4(6) . . ? C1 C4 C3 107.8(9) . . ? C10 C5 C6 116.5(5) . . ? C10 C5 C4 123.2(5) . . ? C6 C5 C4 120.2(5) . . ? C7 C6 C5 122.6(6) . . ? C7 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 . . ? C6 C7 C8 119.9(5) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 117.8(5) . . ? C9 C8 C11 122.2(5) . . ? C7 C8 C11 119.9(5) . . ? C8 C9 C10 120.9(6) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C5 C10 C9 122.2(6) . . ? C5 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? C12 C11 C16 113.5(5) . . ? C12 C11 C8 123.2(5) . . ? C16 C11 C8 123.2(6) . . ? C13 C12 N1 105.5(5) . . ? C13 C12 C11 122.8(5) . . ? N1 C12 C11 131.7(5) . . ? C12 C13 N2 106.5(5) . . ? C12 C13 C14 123.2(5) . . ? N2 C13 C14 130.2(5) . . ? C15 C14 C13 114.3(5) . . ? C15 C14 C17 122.0(5) . . ? C13 C14 C17 123.7(5) . . ? C14 C15 C16 122.6(5) . . ? C14 C15 H15A 118.7 . . ? C16 C15 H15A 118.7 . . ? C15 C16 C11 123.6(6) . . ? C15 C16 H16A 118.2 . . ? C11 C16 H16A 118.2 . . ? C18 C17 C22 116.1(5) . . ? C18 C17 C14 122.9(5) . . ? C22 C17 C14 121.0(5) . . ? C19 C18 C17 122.5(5) . . ? C19 C18 H18A 118.7 . . ? C17 C18 H18A 118.7 . . ? C18 C19 C20 121.2(6) . . ? C18 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? C19 C20 C21 116.8(6) . . ? C19 C20 C23 123.1(6) . . ? C21 C20 C23 120.1(5) . . ? C22 C21 C20 122.4(6) . . ? C22 C21 H21A 118.8 . . ? C20 C21 H21A 118.8 . . ? C21 C22 C17 120.9(6) . . ? C21 C22 H22A 119.5 . . ? C17 C22 H22A 119.5 . . ? C24 C23 C25 109.4(6) . . ? C24 C23 C20 112.7(6) . . ? C25 C23 C20 109.3(5) . . ? C24 C23 C26 108.6(6) . . ? C25 C23 C26 107.3(6) . . ? C20 C23 C26 109.3(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 C27 N2 108.8(5) . . ? N1 C27 C28 125.3(5) . . ? N2 C27 C28 125.9(5) . . ? C29 C28 C33 119.2(5) . . ? C29 C28 C27 122.5(5) . . ? C33 C28 C27 118.3(5) . . ? C30 C29 C28 119.9(6) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 121.0(6) . . ? C29 C30 H30A 119.5 . . ? C31 C30 H30A 119.5 . . ? C30 C31 C32 118.6(6) . . ? C30 C31 C34 122.0(5) . . ? C32 C31 C34 119.5(6) . . ? C33 C32 C31 120.6(6) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C28 120.7(6) . . ? C32 C33 H33A 119.7 . . ? C28 C33 H33A 119.7 . . ? N4 C34 N3 108.9(5) . . ? N4 C34 C31 125.5(5) . . ? N3 C34 C31 125.6(6) . . ? C38 C35 H35A 109.5 . . ? C38 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C38 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 H36A 109.5 . . ? C38 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C38 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 C35 108.6(7) . . ? C36 C38 C37 108.8(6) . . ? C35 C38 C37 109.9(7) . . ? C36 C38 C39 112.6(6) . . ? C35 C38 C39 107.0(6) . . ? C37 C38 C39 109.9(6) . . ? C44 C39 C40 117.2(6) . . ? C44 C39 C38 123.0(6) . . ? C40 C39 C38 119.6(6) . . ? C41 C40 C39 121.5(6) . . ? C41 C40 H40A 119.3 . . ? C39 C40 H40A 119.3 . . ? C42 C41 C40 121.4(6) . . ? C42 C41 H41A 119.3 . . ? C40 C41 H41A 119.3 . . ? C41 C42 C43 117.6(6) . . ? C41 C42 C45 120.8(6) . . ? C43 C42 C45 121.6(6) . . ? C44 C43 C42 120.1(6) . . ? C44 C43 H43A 119.9 . . ? C42 C43 H43A 119.9 . . ? C39 C44 C43 122.1(6) . . ? C39 C44 H44A 119.0 . . ? C43 C44 H44A 119.0 . . ? C46 C45 C50 113.7(6) . . ? C46 C45 C42 123.0(5) . . ? C50 C45 C42 123.2(6) . . ? C45 C46 C47 124.1(6) . . ? C45 C46 H46A 118.0 . . ? C47 C46 H46A 118.0 . . ? C46 C47 C48 122.8(6) . . ? C46 C47 H47A 118.6 . . ? C48 C47 H47A 118.6 . . ? C49 C48 C47 112.9(6) . . ? C49 C48 C51 126.3(6) . . ? C47 C48 C51 120.6(6) . . ? C50 C49 C48 124.5(6) . . ? C50 C49 N4 105.8(5) . . ? C48 C49 N4 129.7(6) . . ? C49 C50 N3 107.3(5) . . ? C49 C50 C45 122.1(6) . . ? N3 C50 C45 130.6(6) . . ? C56 C51 C52 116.2(6) . . ? C56 C51 C48 121.7(6) . . ? C52 C51 C48 121.7(6) . . ? C53 C52 C51 121.8(6) . . ? C53 C52 H52A 119.1 . . ? C51 C52 H52A 119.1 . . ? C52 C53 C54 121.6(7) . . ? C52 C53 H53A 119.2 . . ? C54 C53 H53A 119.2 . . ? C53 C54 C55 116.9(7) . . ? C53 C54 C57 121.6(7) . . ? C55 C54 C57 121.5(7) . . ? C56 C55 C54 121.4(7) . . ? C56 C55 H55A 119.3 . . ? C54 C55 H55A 119.3 . . ? C51 C56 C55 122.0(7) . . ? C51 C56 H56A 119.0 . . ? C55 C56 H56A 119.0 . . ? C58 C57 C54 106.6(7) . . ? C58 C57 C60 108.7(8) . . ? C54 C57 C60 112.4(7) . . ? C58 C57 C59 110.6(9) . . ? C54 C57 C59 111.5(7) . . ? C60 C57 C59 107.2(7) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C61 O1 C76 109.5(9) . . ? C63 O2 C62 120.6(11) . . ? C65 O3 C64 111.0(8) . . ? C67 O4 C66 110.3(8) . . ? C68 O5 C69 115.2(8) . . ? C70 O6 C71 109.9(13) . . ? C73 O7 C72 113.2(10) . . ? C75 O8 C74 117.1(11) . . ? O1 C61 C62 108.6(8) . . ? O1 C61 H61A 110.0 . . ? C62 C61 H61A 110.0 . . ? O1 C61 H61B 110.0 . . ? C62 C61 H61B 110.0 . . ? H61A C61 H61B 108.3 . . ? C61 C62 O2 115.6(12) . . ? C61 C62 H62A 108.4 . . ? O2 C62 H62A 108.4 . . ? C61 C62 H62B 108.4 . . ? O2 C62 H62B 108.4 . . ? H62A C62 H62B 107.4 . . ? O2 C63 C64 115.1(11) . . ? O2 C63 H63A 108.5 . . ? C64 C63 H63A 108.5 . . ? O2 C63 H63B 108.5 . . ? C64 C63 H63B 108.5 . . ? H63A C63 H63B 107.5 . . ? C63 C64 O3 110.0(9) . . ? C63 C64 H64A 109.7 . . ? O3 C64 H64A 109.7 . . ? C63 C64 H64B 109.7 . . ? O3 C64 H64B 109.7 . . ? H64A C64 H64B 108.2 . . ? O3 C65 C66 113.8(8) . . ? O3 C65 H65A 108.8 . . ? C66 C65 H65A 108.8 . . ? O3 C65 H65B 108.8 . . ? C66 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? O4 C66 C65 109.7(8) . . ? O4 C66 H66A 109.7 . . ? C65 C66 H66A 109.7 . . ? O4 C66 H66B 109.7 . . ? C65 C66 H66B 109.7 . . ? H66A C66 H66B 108.2 . . ? O4 C67 C68 107.6(7) . . ? O4 C67 H67A 110.2 . . ? C68 C67 H67A 110.2 . . ? O4 C67 H67B 110.2 . . ? C68 C67 H67B 110.2 . . ? H67A C67 H67B 108.5 . . ? O5 C68 C67 109.8(8) . . ? O5 C68 H68A 109.7 . . ? C67 C68 H68A 109.7 . . ? O5 C68 H68B 109.7 . . ? C67 C68 H68B 109.7 . . ? H68A C68 H68B 108.2 . . ? O5 C69 C70 105.8(7) . . ? O5 C69 H69A 110.6 . . ? C70 C69 H69A 110.6 . . ? O5 C69 H69B 110.6 . . ? C70 C69 H69B 110.6 . . ? H69A C69 H69B 108.7 . . ? O6 C70 C69 109.2(10) . . ? O6 C70 H70A 109.8 . . ? C69 C70 H70A 109.8 . . ? O6 C70 H70B 109.8 . . ? C69 C70 H70B 109.8 . . ? H70A C70 H70B 108.3 . . ? O6 C71 C72 116.2(13) . . ? O6 C71 H71A 108.2 . . ? C72 C71 H71A 108.2 . . ? O6 C71 H71B 108.2 . . ? C72 C71 H71B 108.2 . . ? H71A C71 H71B 107.4 . . ? C71 C72 O7 115.5(11) . . ? C71 C72 H72A 108.4 . . ? O7 C72 H72A 108.4 . . ? C71 C72 H72B 108.4 . . ? O7 C72 H72B 108.4 . . ? H72A C72 H72B 107.5 . . ? O7 C73 C74 110.9(10) . . ? O7 C73 H73A 109.5 . . ? C74 C73 H73A 109.5 . . ? O7 C73 H73B 109.5 . . ? C74 C73 H73B 109.5 . . ? H73A C73 H73B 108.1 . . ? O8 C74 C73 110.6(9) . . ? O8 C74 H74A 109.5 . . ? C73 C74 H74A 109.5 . . ? O8 C74 H74B 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 108.1 . . ? O8 C75 C76 110.2(9) . . ? O8 C75 H75A 109.6 . . ? C76 C75 H75A 109.6 . . ? O8 C75 H75B 109.6 . . ? C76 C75 H75B 109.6 . . ? H75A C75 H75B 108.1 . . ? O1 C76 C75 108.3(8) . . ? O1 C76 H76A 110.0 . . ? C75 C76 H76A 110.0 . . ? O1 C76 H76B 110.0 . . ? C75 C76 H76B 110.0 . . ? H76A C76 H76B 108.4 . . ? F2 B1 F3 110.2(6) . . ? F2 B1 F4 111.6(6) . . ? F3 B1 F4 110.0(8) . . ? F2 B1 F1 110.0(7) . . ? F3 B1 F1 108.7(6) . . ? F4 B1 F1 106.2(6) . . ? F5A B2A F8A 110.1(10) . . ? F5A B2A F6A 110.4(10) . . ? F8A B2A F6A 109.4(11) . . ? F5A B2A F7A 106.9(10) . . ? F8A B2A F7A 108.3(10) . . ? F6A B2A F7A 111.7(10) . . ? F6B B2B F5B 112.3(11) . . ? F6B B2B F7B 108.4(11) . . ? F5B B2B F7B 113.2(11) . . ? F6B B2B F8B 107.5(11) . . ? F5B B2B F8B 107.1(11) . . ? F7B B2B F8B 108.1(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.399 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.084 # Attachment '- 891821.cif' data_kz90z _database_code_depnum_ccdc_archive 'CCDC 891920' #TrackingRef '- 891821.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89.50 H107.50 B2 Cl1.50 F8 N5 O12' _chemical_formula_weight 1672.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.517(3) _cell_length_b 39.753(5) _cell_length_c 11.1884(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.934(2) _cell_angle_gamma 90.00 _cell_volume 9501(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 452 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 20.91 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3532 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9628 _exptl_absorpt_correction_T_max 0.9937 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48976 _diffrn_reflns_av_R_equivalents 0.1358 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 20.91 _reflns_number_total 9999 _reflns_number_gt 6600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal was very weakly diffracting and a cut-off at 1.0 A was applied in XPREP in order find a solution. Both BF4- anions were treated as rigid groups with DFIX 1.38, SADI,DELU and SIMU restraints.The lattice contains both CHCL3 and CH3NO2 solvent molecules. The CHCL3 was 1/2 occupancy and disordered over two positions with 1/3 and 2/3 sof. THe CH3NO2 was refined as full sof but disordered equally with sof of 1/3 over three different positions.DFIX, SADI, DELU and SIMU restraints were employed for all solvent molecules to achieve chemically reasonable geomteries.All of these factors contributed to high residuals in the fianl cycles of refinment but the structure of the cationic portion of the molecule is well behaved and provides sensible metric parameters. ; _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^)+(0.0378P)^2^+107.4031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9999 _refine_ls_number_parameters 1089 _refine_ls_number_restraints 184 _refine_ls_R_factor_all 0.2158 _refine_ls_R_factor_gt 0.1563 _refine_ls_wR_factor_ref 0.3319 _refine_ls_wR_factor_gt 0.2932 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.000 _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 N1 N -0.2508(4) 0.9522(2) 0.0062(7) 0.034(2) Uani 1 1 d . . . H1A H -0.2677 0.9343 -0.0304 0.041 Uiso 1 1 calc R . . N2 N -0.1909(4) 0.9836(2) 0.1316(8) 0.034(2) Uani 1 1 d . . . H2A H -0.1615 0.9896 0.1893 0.041 Uiso 1 1 calc R . . N3 N -0.0995(4) 0.8150(2) 0.3733(8) 0.042(2) Uani 1 1 d . . . H3A H -0.1336 0.8187 0.4077 0.050 Uiso 1 1 calc R . . N4 N -0.0262(4) 0.8226(2) 0.2625(8) 0.036(2) Uani 1 1 d . . . H4A H -0.0029 0.8320 0.2125 0.043 Uiso 1 1 calc R . . C1 C -0.5016(8) 0.9411(5) -0.5576(15) 0.129(8) Uani 1 1 d . . . H1B H -0.5260 0.9278 -0.6203 0.194 Uiso 1 1 calc R . . H1C H -0.4775 0.9582 -0.5952 0.194 Uiso 1 1 calc R . . H1D H -0.5300 0.9521 -0.5076 0.194 Uiso 1 1 calc R . . C2 C -0.4954(9) 0.8935(5) -0.4155(16) 0.145(9) Uani 1 1 d . . . H2B H -0.4678 0.8785 -0.3636 0.217 Uiso 1 1 calc R . . H2C H -0.5215 0.8802 -0.4757 0.217 Uiso 1 1 calc R . . H2D H -0.5222 0.9061 -0.3664 0.217 Uiso 1 1 calc R . . C3 C -0.4177(7) 0.9011(4) -0.5590(14) 0.103(6) Uani 1 1 d . . . H3B H -0.3878 0.8861 -0.5124 0.154 Uiso 1 1 calc R . . H3C H -0.3948 0.9181 -0.5999 0.154 Uiso 1 1 calc R . . H3D H -0.4445 0.8880 -0.6188 0.154 Uiso 1 1 calc R . . C4 C -0.4563(6) 0.9178(4) -0.4781(12) 0.068(4) Uani 1 1 d . . . C5 C -0.4190(6) 0.9391(3) -0.3817(10) 0.047(3) Uani 1 1 d . . . C6 C -0.3553(5) 0.9338(3) -0.3467(10) 0.046(3) Uani 1 1 d . . . H6A H -0.3345 0.9165 -0.3853 0.055 Uiso 1 1 calc R . . C7 C -0.3217(5) 0.9527(3) -0.2582(10) 0.050(3) Uani 1 1 d . . . H7A H -0.2785 0.9480 -0.2359 0.060 Uiso 1 1 calc R . . C8 C -0.3499(5) 0.9783(3) -0.2014(10) 0.042(3) Uani 1 1 d . . . C9 C -0.4134(6) 0.9836(3) -0.2316(11) 0.053(3) Uani 1 1 d . . . H9A H -0.4342 1.0004 -0.1910 0.064 Uiso 1 1 calc R . . C10 C -0.4467(6) 0.9644(3) -0.3210(11) 0.055(3) Uani 1 1 d . . . H10A H -0.4902 0.9688 -0.3414 0.066 Uiso 1 1 calc R . . C11 C -0.3126(5) 0.9990(3) -0.1082(10) 0.045(3) Uani 1 1 d . . . C12 C -0.2684(5) 0.9860(3) -0.0196(9) 0.035(3) Uani 1 1 d . . . C13 C -0.2315(5) 1.0055(3) 0.0631(10) 0.034(3) Uani 1 1 d . . . C14 C -0.2367(5) 1.0404(3) 0.0685(10) 0.042(3) Uani 1 1 d . . . C15 C -0.2815(5) 1.0536(3) -0.0195(11) 0.051(3) Uani 1 1 d . . . H15A H -0.2877 1.0773 -0.0218 0.061 Uiso 1 1 calc R . . C16 C -0.3179(5) 1.0339(3) -0.1046(11) 0.045(3) Uani 1 1 d . . . H16A H -0.3474 1.0447 -0.1622 0.054 Uiso 1 1 calc R . . C17 C -0.1984(5) 1.0612(3) 0.1589(10) 0.040(3) Uani 1 1 d . . . C18 C -0.1852(5) 1.0513(3) 0.2770(11) 0.043(3) Uani 1 1 d . . . H18A H -0.2040 1.0313 0.3024 0.052 Uiso 1 1 calc R . . C19 C -0.1455(5) 1.0692(3) 0.3605(10) 0.039(3) Uani 1 1 d . . . H19A H -0.1374 1.0613 0.4409 0.047 Uiso 1 1 calc R . . C20 C -0.1174(6) 1.0987(3) 0.3281(10) 0.043(3) Uani 1 1 d . . . C21 C -0.1326(6) 1.1092(3) 0.2094(11) 0.047(3) Uani 1 1 d . . . H21A H -0.1149 1.1296 0.1845 0.056 Uiso 1 1 calc R . . C22 C -0.1718(5) 1.0916(3) 0.1278(10) 0.043(3) Uani 1 1 d . . . H22A H -0.1812 1.1001 0.0483 0.052 Uiso 1 1 calc R . . C23 C -0.0692(7) 1.1184(3) 0.4130(10) 0.054(4) Uani 1 1 d . . . C24 C -0.0735(7) 1.1094(3) 0.5448(11) 0.077(5) Uani 1 1 d . . . H24A H -0.1150 1.1156 0.5655 0.115 Uiso 1 1 calc R . . H24B H -0.0413 1.1218 0.5967 0.115 Uiso 1 1 calc R . . H24C H -0.0670 1.0852 0.5565 0.115 Uiso 1 1 calc R . . C25 C -0.0037(7) 1.1084(4) 0.3845(13) 0.087(5) Uani 1 1 d . . . H25A H 0.0004 1.1138 0.3003 0.131 Uiso 1 1 calc R . . H25B H 0.0025 1.0842 0.3976 0.131 Uiso 1 1 calc R . . H25C H 0.0280 1.1209 0.4374 0.131 Uiso 1 1 calc R . . C26 C -0.0763(8) 1.1558(3) 0.3982(13) 0.096(6) Uani 1 1 d . . . H26A H -0.0738 1.1619 0.3141 0.145 Uiso 1 1 calc R . . H26B H -0.0428 1.1672 0.4501 0.145 Uiso 1 1 calc R . . H26C H -0.1170 1.1627 0.4209 0.145 Uiso 1 1 calc R . . C27 C -0.2040(5) 0.9524(3) 0.0956(9) 0.030(3) Uani 1 1 d . . . C28 C -0.1709(5) 0.9219(3) 0.1449(9) 0.034(3) Uani 1 1 d . . . C29 C -0.2044(5) 0.8963(3) 0.1902(9) 0.038(3) Uani 1 1 d . . . H29A H -0.2485 0.8980 0.1883 0.045 Uiso 1 1 calc R . . C30 C -0.1731(5) 0.8682(2) 0.2382(9) 0.035(3) Uani 1 1 d . . . H30A H -0.1960 0.8501 0.2672 0.042 Uiso 1 1 calc R . . C31 C -0.1085(5) 0.8661(3) 0.2445(9) 0.033(3) Uani 1 1 d . . . C32 C -0.0750(5) 0.8925(3) 0.2010(9) 0.033(3) Uani 1 1 d . . . H32A H -0.0307 0.8912 0.2061 0.040 Uiso 1 1 calc R . . C33 C -0.1059(5) 0.9202(3) 0.1509(9) 0.035(3) Uani 1 1 d . . . H33A H -0.0831 0.9381 0.1205 0.041 Uiso 1 1 calc R . . C34 C -0.0777(5) 0.8352(2) 0.2924(10) 0.034(3) Uani 1 1 d . . . C35 C -0.3139(14) 0.7704(6) 0.733(4) 0.37(3) Uani 1 1 d . . . H35A H -0.3225 0.7833 0.6582 0.554 Uiso 1 1 calc R . . H35B H -0.2852 0.7830 0.7909 0.554 Uiso 1 1 calc R . . H35C H -0.3532 0.7663 0.7667 0.554 Uiso 1 1 calc R . . C36 C -0.3273(10) 0.7181(11) 0.640(2) 0.34(3) Uani 1 1 d . . . H36A H -0.3051 0.6991 0.6081 0.517 Uiso 1 1 calc R . . H36B H -0.3485 0.7311 0.5722 0.517 Uiso 1 1 calc R . . H36C H -0.3583 0.7096 0.6894 0.517 Uiso 1 1 calc R . . C37 C -0.2729(10) 0.7233(8) 0.8244(18) 0.216(15) Uani 1 1 d . . . H37A H -0.2589 0.7000 0.8165 0.324 Uiso 1 1 calc R . . H37B H -0.3111 0.7235 0.8641 0.324 Uiso 1 1 calc R . . H37C H -0.2400 0.7361 0.8728 0.324 Uiso 1 1 calc R . . C38 C -0.2854(8) 0.7382(4) 0.7073(14) 0.076(4) Uani 1 1 d . . . C39 C -0.2240(6) 0.7418(4) 0.6548(12) 0.061(4) Uani 1 1 d . . . C40 C -0.1989(7) 0.7172(3) 0.5890(12) 0.065(4) Uani 1 1 d . . . H40A H -0.2187 0.6958 0.5835 0.078 Uiso 1 1 calc R . . C41 C -0.1475(6) 0.7217(3) 0.5314(11) 0.058(4) Uani 1 1 d . . . H41A H -0.1321 0.7034 0.4888 0.070 Uiso 1 1 calc R . . C42 C -0.1171(6) 0.7527(3) 0.5340(11) 0.054(4) Uani 1 1 d . . . C43 C -0.1399(7) 0.7771(3) 0.6058(11) 0.065(4) Uani 1 1 d . . . H43A H -0.1188 0.7981 0.6154 0.078 Uiso 1 1 calc R . . C44 C -0.1920(7) 0.7718(4) 0.6636(11) 0.063(4) Uani 1 1 d . . . H44A H -0.2063 0.7894 0.7108 0.075 Uiso 1 1 calc R . . C45 C -0.0655(6) 0.7585(3) 0.4609(10) 0.050(3) Uani 1 1 d . . . C46 C -0.0191(6) 0.7343(3) 0.4474(12) 0.063(4) Uani 1 1 d . . . H46A H -0.0208 0.7135 0.4891 0.075 Uiso 1 1 calc R . . C47 C 0.0293(6) 0.7390(3) 0.3759(12) 0.062(4) Uani 1 1 d . . . H47A H 0.0589 0.7215 0.3710 0.074 Uiso 1 1 calc R . . C48 C 0.0354(6) 0.7686(3) 0.3116(11) 0.047(3) Uani 1 1 d . . . C49 C -0.0131(5) 0.7918(3) 0.3211(10) 0.041(3) Uani 1 1 d . . . C50 C -0.0602(5) 0.7876(3) 0.3947(10) 0.041(3) Uani 1 1 d . . . C51 C 0.0853(5) 0.7727(3) 0.2366(12) 0.048(3) Uani 1 1 d . . . C52 C 0.1030(6) 0.7466(3) 0.1697(13) 0.065(4) Uani 1 1 d . . . H52A H 0.0820 0.7256 0.1726 0.077 Uiso 1 1 calc R . . C53 C 0.1510(7) 0.7496(4) 0.0968(14) 0.077(4) Uani 1 1 d . . . H53A H 0.1604 0.7313 0.0476 0.093 Uiso 1 1 calc R . . C54 C 0.1848(6) 0.7789(4) 0.0959(13) 0.068(4) Uani 1 1 d . . . C55 C 0.1654(7) 0.8052(4) 0.1604(14) 0.074(4) Uani 1 1 d . . . H55A H 0.1853 0.8264 0.1557 0.089 Uiso 1 1 calc R . . C56 C 0.1173(6) 0.8021(4) 0.2331(13) 0.068(4) Uani 1 1 d . . . H56A H 0.1068 0.8207 0.2804 0.081 Uiso 1 1 calc R . . C57 C 0.2374(7) 0.7837(4) 0.0182(16) 0.080(5) Uani 1 1 d . . . C58 C 0.2493(10) 0.7534(5) -0.058(2) 0.155(9) Uani 1 1 d . . . H58A H 0.2597 0.7339 -0.0058 0.232 Uiso 1 1 calc R . . H58B H 0.2842 0.7582 -0.1042 0.232 Uiso 1 1 calc R . . H58C H 0.2116 0.7485 -0.1136 0.232 Uiso 1 1 calc R . . C59 C 0.2959(8) 0.7896(8) 0.092(2) 0.207(14) Uani 1 1 d . . . H59A H 0.3039 0.7714 0.1507 0.310 Uiso 1 1 calc R . . H59B H 0.2939 0.8111 0.1342 0.310 Uiso 1 1 calc R . . H59C H 0.3298 0.7904 0.0408 0.310 Uiso 1 1 calc R . . C60 C 0.2218(11) 0.8112(6) -0.073(2) 0.201(13) Uani 1 1 d . . . H60A H 0.1820 0.8061 -0.1218 0.302 Uiso 1 1 calc R . . H60B H 0.2551 0.8128 -0.1255 0.302 Uiso 1 1 calc R . . H60C H 0.2182 0.8327 -0.0314 0.302 Uiso 1 1 calc R . . O1 O -0.0679(3) 1.00031(17) 0.0481(6) 0.0352(18) Uani 1 1 d . . . O2 O -0.0782(3) 0.98857(17) 0.2917(6) 0.0370(18) Uani 1 1 d . . . O3 O -0.1766(4) 0.9752(2) 0.4178(7) 0.054(2) Uani 1 1 d . . . O4 O -0.2648(4) 1.0089(2) 0.5278(8) 0.068(3) Uani 1 1 d . . . O5 O -0.3625(5) 1.0422(3) 0.3520(12) 0.104(4) Uani 1 1 d . . . O6 O -0.4322(6) 1.0135(5) 0.1686(13) 0.126(5) Uani 1 1 d . . . O7 O -0.3795(8) 0.9345(4) 0.098(2) 0.243(13) Uani 1 1 d . . . O8 O -0.3126(4) 0.8868(2) -0.0339(7) 0.061(2) Uani 1 1 d . . . O9 O -0.2052(4) 0.89944(18) -0.1410(7) 0.049(2) Uani 1 1 d . . . O10 O -0.1263(3) 0.96024(17) -0.1112(6) 0.0374(19) Uani 1 1 d . . . C61 C -0.1231(5) 0.9937(3) -0.1449(9) 0.036(3) Uani 1 1 d . . . C62 C -0.1497(5) 1.0056(3) -0.2524(9) 0.046(3) Uani 1 1 d . . . H62A H -0.1712 0.9908 -0.3101 0.056 Uiso 1 1 calc R . . C63 C -0.1451(6) 1.0399(3) -0.2771(11) 0.057(4) Uani 1 1 d . . . H63A H -0.1635 1.0486 -0.3523 0.069 Uiso 1 1 calc R . . C64 C -0.1136(6) 1.0616(3) -0.1920(11) 0.052(3) Uani 1 1 d . . . H64A H -0.1106 1.0849 -0.2093 0.062 Uiso 1 1 calc R . . C65 C -0.0869(5) 1.0490(3) -0.0825(10) 0.041(3) Uani 1 1 d . . . H65A H -0.0649 1.0635 -0.0247 0.049 Uiso 1 1 calc R . . C66 C -0.0924(5) 1.0150(3) -0.0574(9) 0.036(3) Uani 1 1 d . . . C67 C -0.0403(5) 1.0227(3) 0.1402(9) 0.036(3) Uani 1 1 d . . . H67A H -0.0703 1.0406 0.1547 0.043 Uiso 1 1 calc R . . H67B H -0.0023 1.0333 0.1150 0.043 Uiso 1 1 calc R . . C68 C -0.0237(5) 1.0028(3) 0.2513(9) 0.041(3) Uani 1 1 d . . . H68A H 0.0056 0.9846 0.2354 0.049 Uiso 1 1 calc R . . H68B H -0.0024 1.0175 0.3150 0.049 Uiso 1 1 calc R . . C69 C -0.0698(6) 0.9766(3) 0.4109(9) 0.050(3) Uani 1 1 d . . . H69A H -0.0642 0.9959 0.4668 0.060 Uiso 1 1 calc R . . H69B H -0.0311 0.9629 0.4230 0.060 Uiso 1 1 calc R . . C70 C -0.1225(6) 0.9563(3) 0.4399(10) 0.051(3) Uani 1 1 d . . . H70A H -0.1261 0.9357 0.3898 0.061 Uiso 1 1 calc R . . H70B H -0.1158 0.9495 0.5256 0.061 Uiso 1 1 calc R . . C71 C -0.2313(6) 0.9591(3) 0.4489(11) 0.057(4) Uani 1 1 d . . . H71A H -0.2237 0.9504 0.5322 0.068 Uiso 1 1 calc R . . H71B H -0.2426 0.9400 0.3939 0.068 Uiso 1 1 calc R . . C72 C -0.2830(6) 0.9841(4) 0.4390(12) 0.065(4) Uani 1 1 d . . . H72A H -0.2888 0.9943 0.3577 0.078 Uiso 1 1 calc R . . H72B H -0.3228 0.9733 0.4543 0.078 Uiso 1 1 calc R . . C73 C -0.3141(7) 1.0310(4) 0.5462(14) 0.084(5) Uani 1 1 d . . . H73A H -0.3037 1.0425 0.6245 0.101 Uiso 1 1 calc R . . H73B H -0.3526 1.0177 0.5507 0.101 Uiso 1 1 calc R . . C74 C -0.3269(8) 1.0569(4) 0.4499(15) 0.089(5) Uani 1 1 d . . . H74A H -0.3499 1.0761 0.4799 0.107 Uiso 1 1 calc R . . H74B H -0.2870 1.0654 0.4257 0.107 Uiso 1 1 calc R . . C75 C -0.3795(7) 1.0622(6) 0.2585(18) 0.087(6) Uani 1 1 d . . . C76 C -0.3651(9) 1.0960(5) 0.238(2) 0.121(7) Uani 1 1 d . . . H76A H -0.3393 1.1080 0.2990 0.146 Uiso 1 1 calc R . . C77 C -0.3871(11) 1.1123(6) 0.134(2) 0.132(9) Uani 1 1 d . . . H77A H -0.3769 1.1354 0.1243 0.158 Uiso 1 1 calc R . . C78 C -0.4235(11) 1.0961(9) 0.042(3) 0.158(12) Uani 1 1 d . . . H78A H -0.4392 1.1078 -0.0289 0.189 Uiso 1 1 calc R . . C79 C -0.4373(10) 1.0619(8) 0.056(2) 0.128(8) Uani 1 1 d . . . H79A H -0.4613 1.0492 -0.0051 0.154 Uiso 1 1 calc R . . C80 C -0.4134(10) 1.0482(6) 0.164(2) 0.099(6) Uani 1 1 d . . . C81 C -0.4035(13) 0.9909(6) 0.141(3) 0.204(17) Uani 1 1 d . . . H81A H -0.3634 0.9936 0.1944 0.244 Uiso 1 1 calc R . . H81B H -0.3938 0.9974 0.0603 0.244 Uiso 1 1 calc R . . C82 C -0.4089(8) 0.9576(6) 0.1321(17) 0.103(6) Uani 1 1 d . . . H82A H -0.4151 0.9508 0.2150 0.124 Uiso 1 1 calc R . . H82B H -0.4505 0.9548 0.0845 0.124 Uiso 1 1 calc R . . C83 C -0.3924(7) 0.9008(5) 0.0868(16) 0.107(7) Uani 1 1 d . . . H83A H -0.4374 0.8974 0.0933 0.128 Uiso 1 1 calc R . . H83B H -0.3683 0.8888 0.1546 0.128 Uiso 1 1 calc R . . C84 C -0.3777(6) 0.8859(4) -0.0276(13) 0.078(5) Uani 1 1 d . . . H84A H -0.3925 0.8623 -0.0332 0.093 Uiso 1 1 calc R . . H84B H -0.3997 0.8985 -0.0963 0.093 Uiso 1 1 calc R . . C85 C -0.2941(7) 0.8660(3) -0.1263(12) 0.068(4) Uani 1 1 d . . . H85A H -0.3130 0.8744 -0.2057 0.081 Uiso 1 1 calc R . . H85B H -0.3091 0.8428 -0.1163 0.081 Uiso 1 1 calc R . . C86 C -0.2252(7) 0.8662(3) -0.1207(12) 0.063(4) Uani 1 1 d . . . H86A H -0.2061 0.8582 -0.0408 0.076 Uiso 1 1 calc R . . H86B H -0.2119 0.8509 -0.1828 0.076 Uiso 1 1 calc R . . C87 C -0.1418(6) 0.9013(3) -0.1604(10) 0.050(3) Uani 1 1 d . . . H87A H -0.1326 0.8841 -0.2194 0.060 Uiso 1 1 calc R . . H87B H -0.1145 0.8973 -0.0841 0.060 Uiso 1 1 calc R . . C88 C -0.1300(6) 0.9356(3) -0.2072(9) 0.046(3) Uani 1 1 d . . . H88A H -0.0903 0.9355 -0.2436 0.055 Uiso 1 1 calc R . . H88B H -0.1642 0.9418 -0.2707 0.055 Uiso 1 1 calc R . . B1 B 0.0121(5) 0.8586(2) -0.0130(10) 0.077(4) Uani 1 1 d DU . . F1 F 0.0444(4) 0.83879(17) -0.0854(8) 0.108(3) Uani 1 1 d DU . . F2 F 0.0450(4) 0.8604(2) 0.1008(7) 0.108(3) Uani 1 1 d DU . . F3 F -0.0457(4) 0.84467(18) -0.0015(7) 0.101(3) Uani 1 1 d DU . . F4 F 0.0044(3) 0.89038(15) -0.0610(6) 0.068(2) Uani 1 1 d DU . . B2 B -0.2385(5) 0.8617(3) 0.5167(9) 0.074(4) Uani 1 1 d DU . . F5 F -0.2074(7) 0.8879(3) 0.5711(10) 0.234(8) Uani 1 1 d DU . . F6 F -0.2731(4) 0.8470(2) 0.5936(8) 0.130(4) Uani 1 1 d DU . . F7 F -0.1973(5) 0.8390(3) 0.4832(8) 0.143(4) Uani 1 1 d DU . . F8 F -0.2726(4) 0.8736(2) 0.4157(7) 0.091(3) Uani 1 1 d DU . . C1S C -0.2719(13) 1.1545(9) 0.598(3) 0.177(12) Uiso 0.33 1 d PDU A -1 H1SA H -0.2508 1.1740 0.6422 0.213 Uiso 0.33 1 calc PR A -1 Cl1 Cl -0.2481(10) 1.1182(5) 0.6729(18) 0.185(7) Uiso 0.33 1 d PDU A -1 Cl2 Cl -0.3515(10) 1.1589(6) 0.596(2) 0.208(8) Uiso 0.33 1 d PDU A -1 Cl3 Cl -0.2514(10) 1.1539(6) 0.4546(18) 0.201(8) Uiso 0.33 1 d PDU A -1 C2S C -0.359(2) 1.1371(15) 0.631(4) 0.253(19) Uiso 0.17 1 d PDU B -2 H2SA H -0.3832 1.1179 0.5898 0.303 Uiso 0.17 1 calc PR B -2 Cl4 Cl -0.412(2) 1.1603(15) 0.705(5) 0.266(17) Uiso 0.17 1 d PDU B -2 Cl5 Cl -0.329(3) 1.1606(16) 0.518(4) 0.256(17) Uiso 0.17 1 d PDU B -2 Cl6 Cl -0.300(2) 1.1198(13) 0.731(5) 0.249(17) Uiso 0.17 1 d PDU B -2 O1N O -0.491(8) 1.246(2) 0.096(13) 0.47(7) Uiso 0.33 1 d PDU C -3 O2N O -0.489(5) 1.195(2) 0.032(8) 0.35(4) Uiso 0.33 1 d PDU C -3 N1N N -0.480(6) 1.216(2) 0.112(7) 0.45(6) Uiso 0.33 1 d PDU C -3 C1N C -0.482(12) 1.204(5) 0.236(8) 0.49(8) Uiso 0.33 1 d PDU C -3 H1NA H -0.4723 1.1794 0.2400 0.739 Uiso 0.33 1 calc PR C -3 H1NB H -0.5242 1.2070 0.2598 0.739 Uiso 0.33 1 calc PR C -3 H1NC H -0.4515 1.2158 0.2916 0.739 Uiso 0.33 1 calc PR C -3 O3N O -0.514(4) 1.193(2) 0.168(9) 0.30(4) Uiso 0.33 1 d PDU D -4 O4N O -0.424(4) 1.205(3) 0.262(11) 0.46(6) Uiso 0.33 1 d PDU D -4 N2N N -0.469(5) 1.212(2) 0.190(11) 0.44(6) Uiso 0.33 1 d PDU D -4 C2N C -0.479(10) 1.247(2) 0.15(2) 0.44(9) Uiso 0.33 1 d PDU D -4 H2NA H -0.4394 1.2594 0.1723 0.665 Uiso 0.33 1 calc PR D -4 H2NB H -0.5110 1.2571 0.1976 0.665 Uiso 0.33 1 calc PR D -4 H2NC H -0.4924 1.2483 0.0668 0.665 Uiso 0.33 1 calc PR D -4 O5N O -0.518(4) 1.300(2) 0.087(6) 0.36(4) Uiso 0.33 1 d PDU E -5 O6N O -0.482(6) 1.2667(16) 0.224(9) 0.42(6) Uiso 0.33 1 d PDU E -5 N3N N -0.494(5) 1.2950(15) 0.188(6) 0.33(4) Uiso 0.33 1 d PDU E -5 C3N C -0.493(4) 1.3218(17) 0.278(6) 0.19(3) Uiso 0.33 1 d PDU E -5 H3NA H -0.5023 1.3434 0.2376 0.282 Uiso 0.33 1 calc PR E -5 H3NB H -0.4517 1.3229 0.3257 0.282 Uiso 0.33 1 calc PR E -5 H3NC H -0.5249 1.3171 0.3318 0.282 Uiso 0.33 1 calc PR E -5 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 N1 0.045(6) 0.027(6) 0.029(5) 0.000(4) -0.001(5) -0.004(4) N2 0.040(6) 0.024(6) 0.039(6) -0.004(5) 0.007(5) -0.008(5) N3 0.047(6) 0.040(6) 0.038(6) 0.003(5) 0.009(5) 0.013(5) N4 0.042(6) 0.023(5) 0.041(6) 0.004(4) 0.005(5) 0.007(5) C1 0.097(14) 0.161(19) 0.111(14) -0.062(14) -0.062(12) 0.036(13) C2 0.17(2) 0.16(2) 0.112(15) -0.058(14) 0.043(14) -0.113(17) C3 0.073(11) 0.145(16) 0.091(12) -0.070(12) 0.013(9) -0.023(11) C4 0.038(8) 0.114(13) 0.050(9) -0.009(9) 0.003(7) -0.001(8) C5 0.043(8) 0.056(8) 0.043(8) -0.008(7) 0.002(6) 0.000(6) C6 0.039(8) 0.054(8) 0.048(8) 0.004(7) 0.014(6) 0.001(6) C7 0.025(7) 0.075(10) 0.046(8) 0.009(7) -0.016(6) -0.008(7) C8 0.043(8) 0.045(8) 0.035(7) 0.014(6) 0.000(6) -0.004(6) C9 0.044(9) 0.058(9) 0.056(9) 0.000(7) 0.002(7) -0.001(7) C10 0.041(8) 0.062(9) 0.062(9) -0.020(8) 0.002(7) 0.004(7) C11 0.046(8) 0.042(8) 0.044(8) 0.020(6) 0.001(6) 0.005(6) C12 0.049(8) 0.029(7) 0.029(7) -0.004(6) 0.010(6) -0.007(6) C13 0.026(6) 0.036(7) 0.042(7) 0.017(6) 0.011(5) -0.002(6) C14 0.036(7) 0.050(8) 0.039(7) 0.005(6) 0.005(6) 0.005(6) C15 0.040(8) 0.033(7) 0.076(9) 0.004(7) -0.007(7) -0.007(6) C16 0.035(7) 0.038(8) 0.058(8) 0.010(6) -0.009(6) 0.009(6) C17 0.044(8) 0.029(7) 0.047(8) -0.002(6) 0.001(6) 0.005(6) C18 0.054(8) 0.033(7) 0.047(8) 0.002(6) 0.019(7) -0.003(6) C19 0.054(8) 0.037(7) 0.027(7) -0.001(6) 0.012(6) 0.005(6) C20 0.072(9) 0.024(7) 0.036(8) -0.003(6) 0.019(7) 0.003(6) C21 0.065(9) 0.022(6) 0.055(9) -0.002(6) 0.012(7) -0.011(6) C22 0.050(8) 0.035(7) 0.043(7) 0.005(6) 0.000(6) 0.013(6) C23 0.088(11) 0.037(8) 0.037(8) -0.005(6) 0.000(7) -0.012(7) C24 0.114(13) 0.069(10) 0.042(8) -0.002(7) -0.010(8) -0.030(9) C25 0.071(11) 0.116(14) 0.074(11) -0.010(10) 0.006(9) -0.018(10) C26 0.163(17) 0.035(9) 0.079(11) -0.010(8) -0.036(11) -0.034(9) C27 0.038(7) 0.031(7) 0.023(6) 0.007(5) 0.012(6) -0.004(5) C28 0.053(8) 0.028(7) 0.020(6) 0.005(5) 0.004(6) 0.009(6) C29 0.045(7) 0.033(7) 0.039(7) -0.001(6) 0.018(6) 0.003(6) C30 0.050(8) 0.016(6) 0.038(7) -0.004(5) 0.004(6) 0.009(5) C31 0.036(7) 0.033(7) 0.030(6) -0.006(5) 0.003(5) 0.011(6) C32 0.041(7) 0.028(7) 0.032(6) 0.000(5) 0.009(5) -0.004(6) C33 0.046(8) 0.028(7) 0.030(6) -0.007(5) 0.006(6) -0.001(6) C34 0.043(8) 0.019(6) 0.041(7) -0.005(6) 0.013(6) 0.008(6) C35 0.24(3) 0.12(2) 0.83(9) 0.16(4) 0.39(5) 0.11(2) C36 0.080(16) 0.77(9) 0.21(3) -0.28(4) 0.101(18) -0.19(3) C37 0.13(2) 0.43(5) 0.090(17) 0.06(2) 0.045(14) -0.06(3) C38 0.094(13) 0.073(11) 0.067(11) 0.019(8) 0.028(9) 0.021(9) C39 0.064(10) 0.059(10) 0.064(9) 0.023(8) 0.023(8) 0.023(8) C40 0.068(10) 0.049(9) 0.081(10) 0.018(8) 0.020(9) 0.021(8) C41 0.062(10) 0.054(9) 0.063(9) 0.010(7) 0.024(8) 0.014(7) C42 0.077(10) 0.033(8) 0.054(9) 0.022(7) 0.014(7) 0.019(7) C43 0.100(12) 0.045(9) 0.051(9) -0.006(7) 0.010(9) 0.011(8) C44 0.079(11) 0.082(12) 0.030(8) 0.001(7) 0.022(7) 0.017(9) C45 0.074(10) 0.034(8) 0.042(8) 0.016(6) 0.005(7) 0.000(7) C46 0.077(10) 0.034(8) 0.076(10) 0.005(7) 0.004(8) 0.020(7) C47 0.043(8) 0.056(9) 0.089(11) 0.013(8) 0.023(8) 0.009(7) C48 0.050(8) 0.035(8) 0.056(8) 0.001(6) 0.008(7) -0.003(6) C49 0.051(8) 0.022(7) 0.048(8) -0.001(6) 0.001(7) 0.009(6) C50 0.035(7) 0.036(8) 0.051(8) 0.000(6) 0.003(6) 0.012(6) C51 0.041(8) 0.017(7) 0.082(10) 0.005(7) -0.005(7) 0.016(6) C52 0.066(10) 0.042(9) 0.088(11) 0.013(8) 0.019(9) 0.013(7) C53 0.077(11) 0.052(10) 0.105(13) -0.010(9) 0.022(10) 0.011(9) C54 0.039(9) 0.067(11) 0.097(12) 0.002(9) 0.011(8) 0.026(8) C55 0.069(10) 0.049(9) 0.104(12) 0.010(9) 0.012(9) -0.001(8) C56 0.065(10) 0.060(10) 0.081(11) -0.015(8) 0.020(8) 0.022(8) C57 0.065(11) 0.074(11) 0.108(13) 0.010(10) 0.032(10) 0.013(9) C58 0.16(2) 0.15(2) 0.18(2) -0.042(17) 0.114(18) -0.008(16) C59 0.042(12) 0.41(4) 0.17(2) -0.05(3) 0.014(13) -0.035(19) C60 0.17(2) 0.20(3) 0.27(3) 0.09(2) 0.15(2) 0.03(2) O1 0.042(5) 0.037(4) 0.026(4) 0.000(4) -0.001(4) -0.001(4) O2 0.048(5) 0.045(5) 0.017(4) 0.001(3) 0.001(3) -0.004(4) O3 0.049(6) 0.056(5) 0.060(6) 0.016(4) 0.014(4) -0.007(5) O4 0.054(6) 0.085(7) 0.063(6) -0.012(5) 0.002(5) 0.011(5) O5 0.080(8) 0.132(11) 0.095(9) 0.029(9) -0.011(7) 0.012(8) O6 0.107(10) 0.139(14) 0.144(12) 0.002(11) 0.062(9) 0.041(10) O7 0.148(14) 0.152(14) 0.47(3) -0.173(18) 0.219(19) -0.104(12) O8 0.064(6) 0.063(6) 0.060(6) -0.024(5) 0.019(5) -0.027(5) O9 0.055(6) 0.044(5) 0.050(5) -0.008(4) 0.014(4) -0.013(4) O10 0.052(5) 0.035(5) 0.025(4) -0.008(4) 0.001(3) -0.009(4) C61 0.048(7) 0.036(7) 0.028(7) 0.005(6) 0.015(6) 0.002(6) C62 0.043(8) 0.069(10) 0.023(7) 0.010(6) -0.010(6) -0.008(6) C63 0.073(10) 0.064(10) 0.036(8) 0.017(7) 0.010(7) 0.009(8) C64 0.070(9) 0.036(7) 0.053(9) 0.014(7) 0.021(7) 0.001(7) C65 0.054(8) 0.035(7) 0.034(7) 0.008(6) 0.007(6) -0.002(6) C66 0.047(7) 0.032(7) 0.030(7) 0.004(6) 0.013(6) 0.006(6) C67 0.042(7) 0.028(6) 0.039(7) -0.011(6) 0.006(6) -0.005(5) C68 0.044(8) 0.043(7) 0.034(7) 0.006(6) -0.003(6) -0.007(6) C69 0.067(9) 0.062(8) 0.019(7) 0.008(6) 0.001(6) 0.002(7) C70 0.056(9) 0.064(9) 0.034(7) 0.015(6) 0.010(6) -0.016(8) C71 0.055(9) 0.067(9) 0.049(8) -0.001(7) 0.008(7) -0.028(8) C72 0.058(10) 0.087(11) 0.049(9) -0.002(8) 0.004(7) -0.032(9) C73 0.058(10) 0.119(14) 0.075(11) -0.004(10) 0.009(8) 0.018(10) C74 0.075(12) 0.098(13) 0.094(13) 0.007(11) 0.007(10) 0.011(10) C75 0.036(9) 0.139(19) 0.083(13) -0.001(14) -0.006(9) 0.029(10) C76 0.119(17) 0.096(15) 0.15(2) 0.047(15) 0.032(14) 0.021(13) C77 0.12(2) 0.13(2) 0.14(2) 0.070(18) 0.031(16) 0.068(17) C78 0.084(18) 0.23(4) 0.16(3) 0.06(3) 0.025(17) 0.06(2) C79 0.103(17) 0.18(2) 0.102(18) 0.018(18) 0.008(13) 0.021(18) C80 0.093(15) 0.115(18) 0.094(16) 0.036(14) 0.040(13) 0.042(13) C81 0.20(3) 0.11(2) 0.34(4) -0.10(2) 0.19(3) -0.10(2) C82 0.070(12) 0.137(19) 0.112(15) 0.000(13) 0.045(11) -0.013(13) C83 0.081(12) 0.136(17) 0.115(14) -0.055(12) 0.061(11) -0.073(11) C84 0.052(10) 0.091(12) 0.093(12) -0.006(9) 0.018(8) -0.041(8) C85 0.099(12) 0.050(9) 0.057(9) -0.019(7) 0.025(8) -0.038(8) C86 0.100(12) 0.029(8) 0.062(9) -0.008(6) 0.021(8) -0.011(8) C87 0.058(9) 0.051(9) 0.042(8) -0.011(6) 0.008(6) -0.001(7) C88 0.060(8) 0.049(8) 0.028(7) -0.006(6) 0.006(6) -0.006(6) B1 0.121(12) 0.025(7) 0.093(10) -0.010(8) 0.046(9) 0.005(8) F1 0.167(9) 0.040(4) 0.137(7) -0.011(5) 0.100(7) -0.011(5) F2 0.124(7) 0.112(7) 0.092(6) 0.015(5) 0.029(5) 0.052(6) F3 0.144(7) 0.056(5) 0.120(7) -0.017(5) 0.083(6) -0.026(5) F4 0.092(6) 0.036(4) 0.078(5) 0.004(3) 0.018(4) -0.008(4) B2 0.133(15) 0.051(10) 0.042(9) -0.005(7) 0.028(7) 0.007(7) F5 0.43(2) 0.113(8) 0.129(10) 0.023(7) -0.092(11) -0.104(10) F6 0.142(9) 0.154(9) 0.108(7) 0.055(6) 0.075(6) 0.056(6) F7 0.162(9) 0.167(8) 0.120(8) 0.089(6) 0.097(7) 0.111(7) F8 0.085(6) 0.112(7) 0.080(5) 0.022(5) 0.029(4) 0.031(5) _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 N1 C27 1.330(12) . ? N1 C12 1.417(13) . ? N1 H1A 0.8800 . ? N2 C27 1.326(12) . ? N2 C13 1.395(13) . ? N2 H2A 0.8800 . ? N3 C34 1.335(13) . ? N3 C50 1.384(13) . ? N3 H3A 0.8800 . ? N4 C34 1.296(12) . ? N4 C49 1.401(13) . ? N4 H4A 0.8800 . ? C1 C4 1.55(2) . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 C4 1.51(2) . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.459(18) . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 C5 1.521(17) . ? C5 C10 1.388(15) . ? C5 C6 1.395(15) . ? C6 C7 1.378(15) . ? C6 H6A 0.9500 . ? C7 C8 1.379(16) . ? C7 H7A 0.9500 . ? C8 C9 1.384(15) . ? C8 C11 1.484(16) . ? C9 C10 1.387(16) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.387(15) . ? C11 C16 1.394(15) . ? C12 C13 1.383(14) . ? C13 C14 1.395(15) . ? C14 C15 1.396(15) . ? C14 C17 1.477(15) . ? C15 C16 1.398(15) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.375(15) . ? C17 C22 1.400(15) . ? C18 C19 1.385(15) . ? C18 H18A 0.9500 . ? C19 C20 1.386(15) . ? C19 H19A 0.9500 . ? C20 C21 1.393(15) . ? C20 C23 1.535(16) . ? C21 C22 1.360(15) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C26 1.503(16) . ? C23 C24 1.531(16) . ? C23 C25 1.534(18) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.477(14) . ? C28 C29 1.379(14) . ? C28 C33 1.395(14) . ? C29 C30 1.381(14) . ? C29 H29A 0.9500 . ? C30 C31 1.387(14) . ? C30 H30A 0.9500 . ? C31 C32 1.392(14) . ? C31 C34 1.465(14) . ? C32 C33 1.371(14) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C35 C38 1.46(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.36(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.43(2) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.516(19) . ? C39 C40 1.372(17) . ? C39 C44 1.376(18) . ? C40 C41 1.357(17) . ? C40 H40A 0.9500 . ? C41 C42 1.395(17) . ? C41 H41A 0.9500 . ? C42 C43 1.386(16) . ? C42 C45 1.474(17) . ? C43 C44 1.377(18) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C50 1.385(15) . ? C45 C46 1.408(16) . ? C46 C47 1.400(17) . ? C46 H46A 0.9500 . ? C47 C48 1.392(16) . ? C47 H47A 0.9500 . ? C48 C49 1.407(15) . ? C48 C51 1.449(16) . ? C49 C50 1.391(15) . ? C51 C56 1.361(17) . ? C51 C52 1.361(16) . ? C52 C53 1.396(18) . ? C52 H52A 0.9500 . ? C53 C54 1.375(18) . ? C53 H53A 0.9500 . ? C54 C55 1.366(18) . ? C54 C57 1.520(19) . ? C55 C56 1.397(18) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C59 1.44(2) . ? C57 C60 1.51(2) . ? C57 C58 1.51(2) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O1 C66 1.366(12) . ? O1 C67 1.434(11) . ? O2 C69 1.407(12) . ? O2 C68 1.423(12) . ? O3 C70 1.384(13) . ? O3 C71 1.418(13) . ? O4 C73 1.411(15) . ? O4 C72 1.421(14) . ? O5 C75 1.33(2) . ? O5 C74 1.388(18) . ? O6 C81 1.15(2) . ? O6 C80 1.44(2) . ? O7 C82 1.21(2) . ? O7 C83 1.37(2) . ? O8 C84 1.411(14) . ? O8 C85 1.416(14) . ? O9 C87 1.409(13) . ? O9 C86 1.417(13) . ? O10 C61 1.387(12) . ? O10 C88 1.450(12) . ? C61 C62 1.353(14) . ? C61 C66 1.397(15) . ? C62 C63 1.400(16) . ? C62 H62A 0.9500 . ? C63 C64 1.397(16) . ? C63 H63A 0.9500 . ? C64 C65 1.384(15) . ? C64 H64A 0.9500 . ? C65 C66 1.387(14) . ? C65 H65A 0.9500 . ? C67 C68 1.479(14) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.460(15) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.486(17) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.492(19) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C80 1.33(2) . ? C75 C76 1.40(2) . ? C76 C77 1.37(2) . ? C76 H76A 0.9500 . ? C77 C78 1.37(3) . ? C77 H77A 0.9500 . ? C78 C79 1.41(3) . ? C78 H78A 0.9500 . ? C79 C80 1.37(3) . ? C79 H79A 0.9500 . ? C81 C82 1.33(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.481(18) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.477(17) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.492(15) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? B1 F4 1.374(10) . ? B1 F1 1.378(10) . ? B1 F3 1.382(10) . ? B1 F2 1.383(10) . ? B2 F6 1.338(10) . ? B2 F5 1.344(10) . ? B2 F7 1.349(10) . ? B2 F8 1.355(10) . ? C1S Cl3 1.713(15) . ? C1S Cl1 1.715(15) . ? C1S Cl2 1.720(15) . ? C1S H1SA 1.0000 . ? C2S Cl6 1.743(16) . ? C2S Cl4 1.746(16) . ? C2S Cl5 1.748(16) . ? C2S H2SA 1.0000 . ? O1N N1N 1.217(17) . ? O2N N1N 1.216(17) . ? N1N C1N 1.48(2) . ? C1N H1NA 0.9800 . ? C1N H1NB 0.9800 . ? C1N H1NC 0.9800 . ? O3N N2N 1.214(16) . ? O4N N2N 1.213(17) . ? N2N C2N 1.47(2) . ? C2N H2NA 0.9800 . ? C2N H2NB 0.9800 . ? C2N H2NC 0.9800 . ? O5N N3N 1.209(10) . ? O6N N3N 1.210(9) . ? N3N C3N 1.467(10) . ? C3N H3NA 0.9800 . ? C3N H3NB 0.9800 . ? C3N H3NC 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 C27 N1 C12 108.0(8) . . ? C27 N1 H1A 126.0 . . ? C12 N1 H1A 126.0 . . ? C27 N2 C13 108.7(9) . . ? C27 N2 H2A 125.6 . . ? C13 N2 H2A 125.6 . . ? C34 N3 C50 109.5(9) . . ? C34 N3 H3A 125.3 . . ? C50 N3 H3A 125.3 . . ? C34 N4 C49 110.3(9) . . ? C34 N4 H4A 124.9 . . ? C49 N4 H4A 124.9 . . ? C4 C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C4 C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C4 C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C3 C4 C2 112.8(15) . . ? C3 C4 C5 113.7(11) . . ? C2 C4 C5 107.7(11) . . ? C3 C4 C1 106.4(13) . . ? C2 C4 C1 107.6(14) . . ? C5 C4 C1 108.4(12) . . ? C10 C5 C6 116.1(11) . . ? C10 C5 C4 121.9(11) . . ? C6 C5 C4 122.0(11) . . ? C7 C6 C5 122.1(11) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C6 C7 C8 120.8(11) . . ? C6 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C7 C8 C9 118.5(11) . . ? C7 C8 C11 120.1(11) . . ? C9 C8 C11 121.3(11) . . ? C8 C9 C10 120.1(12) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C9 C10 C5 122.4(12) . . ? C9 C10 H10A 118.8 . . ? C5 C10 H10A 118.8 . . ? C12 C11 C16 113.6(11) . . ? C12 C11 C8 124.2(10) . . ? C16 C11 C8 122.2(10) . . ? C13 C12 C11 124.0(10) . . ? C13 C12 N1 106.0(9) . . ? C11 C12 N1 129.9(10) . . ? C12 C13 C14 123.0(10) . . ? C12 C13 N2 106.8(9) . . ? C14 C13 N2 130.2(10) . . ? C13 C14 C15 113.3(10) . . ? C13 C14 C17 123.0(10) . . ? C15 C14 C17 123.7(11) . . ? C14 C15 C16 123.5(11) . . ? C14 C15 H15A 118.2 . . ? C16 C15 H15A 118.2 . . ? C11 C16 C15 122.5(11) . . ? C11 C16 H16A 118.7 . . ? C15 C16 H16A 118.7 . . ? C18 C17 C22 116.3(11) . . ? C18 C17 C14 122.1(10) . . ? C22 C17 C14 121.5(11) . . ? C17 C18 C19 122.6(11) . . ? C17 C18 H18A 118.7 . . ? C19 C18 H18A 118.7 . . ? C18 C19 C20 120.8(10) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C21 116.4(11) . . ? C19 C20 C23 123.6(10) . . ? C21 C20 C23 120.0(10) . . ? C22 C21 C20 122.7(11) . . ? C22 C21 H21A 118.7 . . ? C20 C21 H21A 118.7 . . ? C21 C22 C17 121.1(11) . . ? C21 C22 H22A 119.4 . . ? C17 C22 H22A 119.4 . . ? C26 C23 C24 108.6(11) . . ? C26 C23 C25 108.5(12) . . ? C24 C23 C25 107.8(12) . . ? C26 C23 C20 112.6(11) . . ? C24 C23 C20 111.2(10) . . ? C25 C23 C20 108.1(10) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 N1 110.3(9) . . ? N2 C27 C28 125.3(10) . . ? N1 C27 C28 124.3(10) . . ? C29 C28 C33 120.7(10) . . ? C29 C28 C27 119.5(10) . . ? C33 C28 C27 119.7(10) . . ? C28 C29 C30 119.3(11) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? C29 C30 C31 120.4(10) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C30 C31 C32 119.7(10) . . ? C30 C31 C34 118.3(10) . . ? C32 C31 C34 122.0(10) . . ? C33 C32 C31 120.2(10) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C28 119.6(10) . . ? C32 C33 H33A 120.2 . . ? C28 C33 H33A 120.2 . . ? N4 C34 N3 108.9(9) . . ? N4 C34 C31 126.3(10) . . ? N3 C34 C31 124.8(10) . . ? C38 C35 H35A 109.5 . . ? C38 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C38 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 H36A 109.5 . . ? C38 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C38 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 C37 108(2) . . ? C36 C38 C35 111(2) . . ? C37 C38 C35 103(2) . . ? C36 C38 C39 112.8(15) . . ? C37 C38 C39 108.4(15) . . ? C35 C38 C39 113.5(15) . . ? C40 C39 C44 115.4(13) . . ? C40 C39 C38 124.1(14) . . ? C44 C39 C38 120.4(13) . . ? C41 C40 C39 124.0(14) . . ? C41 C40 H40A 118.0 . . ? C39 C40 H40A 118.0 . . ? C40 C41 C42 120.8(13) . . ? C40 C41 H41A 119.6 . . ? C42 C41 H41A 119.6 . . ? C43 C42 C41 115.6(12) . . ? C43 C42 C45 123.6(12) . . ? C41 C42 C45 120.7(11) . . ? C44 C43 C42 122.1(14) . . ? C44 C43 H43A 118.9 . . ? C42 C43 H43A 118.9 . . ? C39 C44 C43 121.8(13) . . ? C39 C44 H44A 119.1 . . ? C43 C44 H44A 119.1 . . ? C50 C45 C46 114.1(12) . . ? C50 C45 C42 123.0(11) . . ? C46 C45 C42 122.8(11) . . ? C47 C46 C45 123.7(12) . . ? C47 C46 H46A 118.2 . . ? C45 C46 H46A 118.2 . . ? C48 C47 C46 122.2(12) . . ? C48 C47 H47A 118.9 . . ? C46 C47 H47A 118.9 . . ? C47 C48 C49 113.4(11) . . ? C47 C48 C51 121.1(11) . . ? C49 C48 C51 125.3(11) . . ? C50 C49 N4 105.2(9) . . ? C50 C49 C48 124.4(10) . . ? N4 C49 C48 130.4(11) . . ? N3 C50 C45 131.5(11) . . ? N3 C50 C49 106.0(10) . . ? C45 C50 C49 122.0(10) . . ? C56 C51 C52 117.6(13) . . ? C56 C51 C48 121.8(11) . . ? C52 C51 C48 120.6(11) . . ? C51 C52 C53 122.1(13) . . ? C51 C52 H52A 118.9 . . ? C53 C52 H52A 118.9 . . ? C54 C53 C52 120.5(13) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C55 C54 C53 116.7(13) . . ? C55 C54 C57 120.2(14) . . ? C53 C54 C57 122.8(14) . . ? C54 C55 C56 122.4(14) . . ? C54 C55 H55A 118.8 . . ? C56 C55 H55A 118.8 . . ? C51 C56 C55 120.4(13) . . ? C51 C56 H56A 119.8 . . ? C55 C56 H56A 119.8 . . ? C59 C57 C60 112.1(19) . . ? C59 C57 C58 105.0(17) . . ? C60 C57 C58 103.5(17) . . ? C59 C57 C54 110.7(16) . . ? C60 C57 C54 110.9(13) . . ? C58 C57 C54 114.2(14) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C66 O1 C67 116.1(8) . . ? C69 O2 C68 114.8(8) . . ? C70 O3 C71 114.7(9) . . ? C73 O4 C72 112.7(11) . . ? C75 O5 C74 116.2(15) . . ? C81 O6 C80 125.2(17) . . ? C82 O7 C83 131.8(15) . . ? C84 O8 C85 112.9(10) . . ? C87 O9 C86 113.1(9) . . ? C61 O10 C88 116.6(8) . . ? C62 C61 O10 123.1(10) . . ? C62 C61 C66 121.7(11) . . ? O10 C61 C66 115.2(9) . . ? C61 C62 C63 118.8(11) . . ? C61 C62 H62A 120.6 . . ? C63 C62 H62A 120.6 . . ? C64 C63 C62 120.5(11) . . ? C64 C63 H63A 119.7 . . ? C62 C63 H63A 119.7 . . ? C65 C64 C63 119.6(11) . . ? C65 C64 H64A 120.2 . . ? C63 C64 H64A 120.2 . . ? C64 C65 C66 119.7(11) . . ? C64 C65 H65A 120.1 . . ? C66 C65 H65A 120.1 . . ? O1 C66 C65 123.9(10) . . ? O1 C66 C61 116.5(9) . . ? C65 C66 C61 119.5(10) . . ? O1 C67 C68 108.1(8) . . ? O1 C67 H67A 110.1 . . ? C68 C67 H67A 110.1 . . ? O1 C67 H67B 110.1 . . ? C68 C67 H67B 110.1 . . ? H67A C67 H67B 108.4 . . ? O2 C68 C67 110.8(9) . . ? O2 C68 H68A 109.5 . . ? C67 C68 H68A 109.5 . . ? O2 C68 H68B 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? O2 C69 C70 112.5(10) . . ? O2 C69 H69A 109.1 . . ? C70 C69 H69A 109.1 . . ? O2 C69 H69B 109.1 . . ? C70 C69 H69B 109.1 . . ? H69A C69 H69B 107.8 . . ? O3 C70 C69 108.7(10) . . ? O3 C70 H70A 110.0 . . ? C69 C70 H70A 110.0 . . ? O3 C70 H70B 110.0 . . ? C69 C70 H70B 110.0 . . ? H70A C70 H70B 108.3 . . ? O3 C71 C72 108.5(10) . . ? O3 C71 H71A 110.0 . . ? C72 C71 H71A 110.0 . . ? O3 C71 H71B 110.0 . . ? C72 C71 H71B 110.0 . . ? H71A C71 H71B 108.4 . . ? O4 C72 C71 105.7(10) . . ? O4 C72 H72A 110.6 . . ? C71 C72 H72A 110.6 . . ? O4 C72 H72B 110.6 . . ? C71 C72 H72B 110.6 . . ? H72A C72 H72B 108.7 . . ? O4 C73 C74 113.7(12) . . ? O4 C73 H73A 108.8 . . ? C74 C73 H73A 108.8 . . ? O4 C73 H73B 108.8 . . ? C74 C73 H73B 108.8 . . ? H73A C73 H73B 107.7 . . ? O5 C74 C73 108.3(14) . . ? O5 C74 H74A 110.0 . . ? C73 C74 H74A 110.0 . . ? O5 C74 H74B 110.0 . . ? C73 C74 H74B 110.0 . . ? H74A C74 H74B 108.4 . . ? O5 C75 C80 117(2) . . ? O5 C75 C76 130.8(19) . . ? C80 C75 C76 113(2) . . ? C77 C76 C75 122(2) . . ? C77 C76 H76A 119.1 . . ? C75 C76 H76A 119.1 . . ? C78 C77 C76 121(3) . . ? C78 C77 H77A 119.3 . . ? C76 C77 H77A 119.3 . . ? C77 C78 C79 119(3) . . ? C77 C78 H78A 120.5 . . ? C79 C78 H78A 120.5 . . ? C80 C79 C78 115(3) . . ? C80 C79 H79A 122.7 . . ? C78 C79 H79A 122.7 . . ? C75 C80 C79 130(2) . . ? C75 C80 O6 120.0(19) . . ? C79 C80 O6 110(2) . . ? O6 C81 C82 139(2) . . ? O6 C81 H81A 102.4 . . ? C82 C81 H81A 102.4 . . ? O6 C81 H81B 102.4 . . ? C82 C81 H81B 102.4 . . ? H81A C81 H81B 104.9 . . ? O7 C82 C81 137.7(19) . . ? O7 C82 H82A 102.7 . . ? C81 C82 H82A 102.7 . . ? O7 C82 H82B 102.7 . . ? C81 C82 H82B 102.7 . . ? H82A C82 H82B 105.0 . . ? O7 C83 C84 114.3(15) . . ? O7 C83 H83A 108.7 . . ? C84 C83 H83A 108.7 . . ? O7 C83 H83B 108.7 . . ? C84 C83 H83B 108.7 . . ? H83A C83 H83B 107.6 . . ? O8 C84 C83 110.5(12) . . ? O8 C84 H84A 109.6 . . ? C83 C84 H84A 109.6 . . ? O8 C84 H84B 109.6 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 108.1 . . ? O8 C85 C86 109.6(10) . . ? O8 C85 H85A 109.7 . . ? C86 C85 H85A 109.7 . . ? O8 C85 H85B 109.7 . . ? C86 C85 H85B 109.7 . . ? H85A C85 H85B 108.2 . . ? O9 C86 C85 108.6(11) . . ? O9 C86 H86A 110.0 . . ? C85 C86 H86A 110.0 . . ? O9 C86 H86B 110.0 . . ? C85 C86 H86B 110.0 . . ? H86A C86 H86B 108.3 . . ? O9 C87 C88 108.2(10) . . ? O9 C87 H87A 110.0 . . ? C88 C87 H87A 110.0 . . ? O9 C87 H87B 110.0 . . ? C88 C87 H87B 110.0 . . ? H87A C87 H87B 108.4 . . ? O10 C88 C87 110.7(9) . . ? O10 C88 H88A 109.5 . . ? C87 C88 H88A 109.5 . . ? O10 C88 H88B 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 108.1 . . ? F4 B1 F1 110.0(8) . . ? F4 B1 F3 109.8(8) . . ? F1 B1 F3 110.5(8) . . ? F4 B1 F2 109.6(8) . . ? F1 B1 F2 109.4(9) . . ? F3 B1 F2 107.6(9) . . ? F6 B2 F5 109.5(9) . . ? F6 B2 F7 108.7(8) . . ? F5 B2 F7 109.7(10) . . ? F6 B2 F8 113.7(9) . . ? F5 B2 F8 107.3(9) . . ? F7 B2 F8 108.0(8) . . ? Cl3 C1S Cl1 110.6(16) . . ? Cl3 C1S Cl2 110.7(16) . . ? Cl1 C1S Cl2 109.4(16) . . ? Cl3 C1S H1SA 108.7 . . ? Cl1 C1S H1SA 108.7 . . ? Cl2 C1S H1SA 108.7 . . ? Cl6 C2S Cl4 111.7(19) . . ? Cl6 C2S Cl5 112(2) . . ? Cl4 C2S Cl5 112.0(19) . . ? Cl6 C2S H2SA 107.0 . . ? Cl4 C2S H2SA 107.0 . . ? Cl5 C2S H2SA 107.0 . . ? O2N N1N O1N 123(5) . . ? O2N N1N C1N 117(4) . . ? O1N N1N C1N 116(4) . . ? N1N C1N H1NA 109.5 . . ? N1N C1N H1NB 109.5 . . ? H1NA C1N H1NB 109.5 . . ? N1N C1N H1NC 109.5 . . ? H1NA C1N H1NC 109.5 . . ? H1NB C1N H1NC 109.5 . . ? O4N N2N O3N 124(5) . . ? O4N N2N C2N 117(4) . . ? O3N N2N C2N 116(4) . . ? N2N C2N H2NA 109.5 . . ? N2N C2N H2NB 109.5 . . ? H2NA C2N H2NB 109.5 . . ? N2N C2N H2NC 109.5 . . ? H2NA C2N H2NC 109.5 . . ? H2NB C2N H2NC 109.5 . . ? O5N N3N O6N 121(4) . . ? O5N N3N C3N 119(3) . . ? O6N N3N C3N 118(3) . . ? N3N C3N H3NA 109.5 . . ? N3N C3N H3NB 109.5 . . ? H3NA C3N H3NB 109.5 . . ? N3N C3N H3NC 109.5 . . ? H3NA C3N H3NC 109.5 . . ? H3NB C3N H3NC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 20.91 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.450 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.080 # Attachment '- 891820.cif' data_kz68a _database_code_depnum_ccdc_archive 'CCDC 891921' #TrackingRef '- 891820.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H111 B2 F8 N9 O18' _chemical_formula_weight 1768.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.951(3) _cell_length_b 16.589(3) _cell_length_c 9.3553(16) _cell_angle_alpha 100.333(2) _cell_angle_beta 92.296(2) _cell_angle_gamma 91.691(2) _cell_volume 2279.3(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 463 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9545 _exptl_absorpt_correction_T_max 0.9735 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20664 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7969 _reflns_number_gt 5945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The BF4- anion was disordered over two sites with sofs of 1/3 and 2/3. Each PART was treated as a rigid group with SADI, DELU and SIMU restraints. Three molecules of nitromethane were located in the lattice; two were refined with full sof, the other with 1/2 sof. ; _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^)+(0.1489P)^2^+4.2121P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7969 _refine_ls_number_parameters 685 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.1228 _refine_ls_R_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.2861 _refine_ls_wR_factor_gt 0.2636 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _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 N1 N 0.32436(18) 0.10377(16) 0.2439(3) 0.0265(6) Uani 1 1 d . A . H1A H 0.3636 0.1446 0.2728 0.032 Uiso 1 1 calc R . . N2 N 0.26544(18) -0.01313(16) 0.1333(3) 0.0276(6) Uani 1 1 d . A . H2A H 0.2595 -0.0618 0.0773 0.033 Uiso 1 1 calc R . . C1A C 0.2656(8) 0.5118(7) 0.7866(17) 0.112(5) Uani 0.67 1 d P A -1 H1AA H 0.2334 0.5326 0.7081 0.168 Uiso 0.67 1 calc PR A -1 H1AB H 0.2892 0.5581 0.8599 0.168 Uiso 0.67 1 calc PR A -1 H1AC H 0.2245 0.4777 0.8315 0.168 Uiso 0.67 1 calc PR A -1 C2A C 0.4039(8) 0.4426(6) 0.8420(13) 0.097(3) Uani 0.67 1 d P A -1 H2AA H 0.4604 0.4247 0.7994 0.146 Uiso 0.67 1 calc PR A -1 H2AB H 0.3772 0.3988 0.8860 0.146 Uiso 0.67 1 calc PR A -1 H2AC H 0.4155 0.4918 0.9168 0.146 Uiso 0.67 1 calc PR A -1 C3A C 0.3948(12) 0.5107(8) 0.6289(13) 0.131(6) Uani 0.67 1 d P A -1 H3AA H 0.3781 0.4897 0.5264 0.197 Uiso 0.67 1 calc PR A -1 H3AB H 0.4590 0.5045 0.6465 0.197 Uiso 0.67 1 calc PR A -1 H3AC H 0.3811 0.5689 0.6527 0.197 Uiso 0.67 1 calc PR A -1 C1B C 0.3301(15) 0.4652(11) 0.9026(18) 0.081(6) Uani 0.33 1 d P A -2 H1BA H 0.3781 0.4348 0.9407 0.122 Uiso 0.33 1 calc PR A -2 H1BB H 0.2719 0.4403 0.9184 0.122 Uiso 0.33 1 calc PR A -2 H1BC H 0.3339 0.5224 0.9532 0.122 Uiso 0.33 1 calc PR A -2 C2B C 0.4376(14) 0.4674(13) 0.714(3) 0.103(8) Uani 0.33 1 d P A -2 H2BA H 0.4513 0.4661 0.6118 0.155 Uiso 0.33 1 calc PR A -2 H2BB H 0.4648 0.4210 0.7482 0.155 Uiso 0.33 1 calc PR A -2 H2BC H 0.4617 0.5188 0.7729 0.155 Uiso 0.33 1 calc PR A -2 C3B C 0.288(2) 0.5323(11) 0.687(3) 0.111(10) Uani 0.33 1 d P A -2 H3BA H 0.2903 0.5320 0.5821 0.166 Uiso 0.33 1 calc PR A -2 H3BB H 0.3137 0.5844 0.7409 0.166 Uiso 0.33 1 calc PR A -2 H3BC H 0.2254 0.5258 0.7120 0.166 Uiso 0.33 1 calc PR A -2 C4 C 0.3410(3) 0.4620(3) 0.7260(5) 0.0541(11) Uani 1 1 d . . . C5 C 0.3015(3) 0.3815(2) 0.6358(4) 0.0400(9) Uani 1 1 d . A . C6 C 0.3008(3) 0.3656(2) 0.4839(5) 0.0407(9) Uani 1 1 d . . . H6A H 0.3246 0.4061 0.4345 0.049 Uiso 1 1 calc R A . C7 C 0.2665(2) 0.2925(2) 0.4039(4) 0.0352(8) Uani 1 1 d . A . H7A H 0.2685 0.2829 0.3009 0.042 Uiso 1 1 calc R . . C8 C 0.2290(2) 0.2327(2) 0.4721(4) 0.0314(8) Uani 1 1 d . . . C9 C 0.2276(3) 0.2488(2) 0.6233(4) 0.0366(9) Uani 1 1 d . A . H9A H 0.2010 0.2095 0.6725 0.044 Uiso 1 1 calc R . . C10 C 0.2644(3) 0.3215(2) 0.7025(4) 0.0417(9) Uani 1 1 d . . . H10A H 0.2641 0.3304 0.8056 0.050 Uiso 1 1 calc R A . C11 C 0.1903(2) 0.1539(2) 0.3903(4) 0.0305(8) Uani 1 1 d . A . C12 C 0.2370(2) 0.1001(2) 0.2883(4) 0.0271(7) Uani 1 1 d . . . C13 C 0.1993(2) 0.0247(2) 0.2176(4) 0.0287(7) Uani 1 1 d . A . C14 C 0.1140(2) -0.0033(2) 0.2421(4) 0.0329(8) Uani 1 1 d . . . C15 C 0.0678(2) 0.0497(2) 0.3434(4) 0.0381(9) Uani 1 1 d . A . H15A H 0.0091 0.0338 0.3655 0.046 Uiso 1 1 calc R . . C16 C 0.1046(2) 0.1255(2) 0.4137(4) 0.0369(9) Uani 1 1 d . . . H16A H 0.0694 0.1593 0.4807 0.044 Uiso 1 1 calc R A . C17 C 0.0770(2) -0.0849(2) 0.1695(4) 0.0336(8) Uani 1 1 d . A . C18 C 0.0638(3) -0.1043(3) 0.0201(4) 0.0439(10) Uani 1 1 d . . . H18A H 0.0783 -0.0646 -0.0378 0.053 Uiso 1 1 calc R A . C19 C 0.0295(3) -0.1816(3) -0.0464(5) 0.0517(11) Uani 1 1 d . A . H19A H 0.0199 -0.1934 -0.1492 0.062 Uiso 1 1 calc R . . C20 C 0.0092(2) -0.2415(2) 0.0343(5) 0.0477(11) Uani 1 1 d . . . C21 C 0.0217(3) -0.2209(3) 0.1840(6) 0.0521(11) Uani 1 1 d . A . H21A H 0.0074 -0.2605 0.2421 0.063 Uiso 1 1 calc R . . C22 C 0.0545(3) -0.1441(2) 0.2509(5) 0.0432(9) Uani 1 1 d . . . H22A H 0.0618 -0.1317 0.3539 0.052 Uiso 1 1 calc R A . C23 C -0.0236(3) -0.3284(3) -0.0416(7) 0.0676(15) Uani 1 1 d . A . C24A C 0.044(2) -0.3700(17) -0.124(3) 0.077(6) Uani 0.50 1 d P A -1 H24A H 0.0884 -0.3884 -0.0583 0.116 Uiso 0.50 1 calc PR A -1 H24B H 0.0730 -0.3328 -0.1798 0.116 Uiso 0.50 1 calc PR A -1 H24C H 0.0169 -0.4176 -0.1908 0.116 Uiso 0.50 1 calc PR A -1 C25A C -0.1143(7) -0.3253(6) -0.1106(13) 0.063(3) Uani 0.50 1 d P A -1 H25A H -0.1594 -0.3255 -0.0373 0.094 Uiso 0.50 1 calc PR A -1 H25B H -0.1251 -0.3733 -0.1881 0.094 Uiso 0.50 1 calc PR A -1 H25C H -0.1184 -0.2752 -0.1518 0.094 Uiso 0.50 1 calc PR A -1 C26A C -0.0451(7) -0.3855(5) 0.0904(11) 0.056(2) Uani 0.50 1 d P A -1 H26A H -0.0112 -0.3615 0.1806 0.084 Uiso 0.50 1 calc PR A -1 H26B H -0.0271 -0.4419 0.0580 0.084 Uiso 0.50 1 calc PR A -1 H26C H -0.1093 -0.3855 0.1078 0.084 Uiso 0.50 1 calc PR A -1 C26B C -0.0983(7) -0.3559(6) 0.0099(15) 0.072(3) Uani 0.50 1 d P A -2 H26D H -0.0880 -0.3584 0.1131 0.108 Uiso 0.50 1 calc PR A -2 H26E H -0.1150 -0.4108 -0.0444 0.108 Uiso 0.50 1 calc PR A -2 H26F H -0.1467 -0.3186 -0.0013 0.108 Uiso 0.50 1 calc PR A -2 C25B C -0.0489(9) -0.3255(6) -0.2222(12) 0.077(3) Uani 0.50 1 d P A -2 H25D H -0.0161 -0.2791 -0.2500 0.115 Uiso 0.50 1 calc PR A -2 H25E H -0.1134 -0.3192 -0.2364 0.115 Uiso 0.50 1 calc PR A -2 H25F H -0.0315 -0.3767 -0.2827 0.115 Uiso 0.50 1 calc PR A -2 C24B C 0.0587(19) -0.3807(16) -0.060(3) 0.087(8) Uani 0.50 1 d P A -2 H24D H 0.0835 -0.3870 0.0355 0.131 Uiso 0.50 1 calc PR A -2 H24E H 0.1039 -0.3539 -0.1108 0.131 Uiso 0.50 1 calc PR A -2 H24F H 0.0416 -0.4348 -0.1175 0.131 Uiso 0.50 1 calc PR A -2 C27 C 0.3394(2) 0.0349(2) 0.1495(3) 0.0260(7) Uani 1 1 d . . . C28 C 0.4223(2) 0.01636(19) 0.0742(4) 0.0265(7) Uani 1 1 d . . . C29 C 0.5041(2) 0.0515(2) 0.1352(4) 0.0293(8) Uani 1 1 d . . . H29A H 0.5067 0.0864 0.2278 0.035 Uiso 1 1 calc R A . C30 C 0.5810(2) 0.0356(2) 0.0609(4) 0.0285(7) Uani 1 1 d . . . H30A H 0.6367 0.0601 0.1017 0.034 Uiso 1 1 calc R . . O1 O 0.34107(17) 0.22058(17) 0.0291(3) 0.0427(7) Uani 1 1 d . . . O2 O 0.45684(17) 0.23493(15) 0.2829(3) 0.0393(6) Uani 1 1 d . . . O3 O 0.5634(4) 0.1452(2) 0.4615(4) 0.1038(18) Uani 1 1 d . . . O4 O 0.3693(3) 0.0215(2) -0.3942(4) 0.0761(11) Uani 1 1 d . . . C31 C 0.3556(3) 0.1220(2) -0.1921(5) 0.0451(10) Uani 1 1 d . . . H31A H 0.4164 0.1379 -0.2009 0.054 Uiso 1 1 calc R . . C32 C 0.3133(4) 0.0587(3) -0.2930(5) 0.0582(13) Uani 1 1 d . . . C33 C 0.2220(4) 0.0381(3) -0.2814(7) 0.0717(17) Uani 1 1 d . . . H33A H 0.1929 -0.0046 -0.3502 0.086 Uiso 1 1 calc R . . C34 C 0.1754(4) 0.0805(4) -0.1692(7) 0.0705(16) Uani 1 1 d . . . H34A H 0.1135 0.0678 -0.1632 0.085 Uiso 1 1 calc R . . C35 C 0.2162(3) 0.1395(3) -0.0681(6) 0.0582(13) Uani 1 1 d . . . H35A H 0.1837 0.1667 0.0104 0.070 Uiso 1 1 calc R . . C36 C 0.3071(3) 0.1608(2) -0.0794(5) 0.0414(9) Uani 1 1 d . . . C37 C 0.4349(2) 0.2419(2) 0.0318(4) 0.0399(9) Uani 1 1 d . . . H37A H 0.4468 0.2760 -0.0424 0.048 Uiso 1 1 calc R . . H37B H 0.4697 0.1917 0.0101 0.048 Uiso 1 1 calc R . . C38 C 0.4615(3) 0.2883(2) 0.1797(5) 0.0455(10) Uani 1 1 d . . . H38A H 0.5234 0.3114 0.1802 0.055 Uiso 1 1 calc R . . H38B H 0.4211 0.3342 0.2061 0.055 Uiso 1 1 calc R . . C39 C 0.5016(3) 0.2691(2) 0.4190(5) 0.0458(10) Uani 1 1 d . . . H39A H 0.4704 0.3183 0.4649 0.055 Uiso 1 1 calc R . . H39B H 0.5637 0.2864 0.4023 0.055 Uiso 1 1 calc R . . C40 C 0.5034(3) 0.2088(3) 0.5175(5) 0.0571(12) Uani 1 1 d . . . H40A H 0.5245 0.2360 0.6166 0.068 Uiso 1 1 calc R . . H40B H 0.4425 0.1849 0.5228 0.068 Uiso 1 1 calc R . . C41 C 0.6009(5) 0.1001(4) 0.5522(7) 0.096(2) Uani 1 1 d . . . H41A H 0.5529 0.0660 0.5847 0.116 Uiso 1 1 calc R . . H41B H 0.6263 0.1379 0.6394 0.116 Uiso 1 1 calc R . . C42 C 0.3315(6) -0.0482(3) -0.4955(7) 0.100(3) Uani 1 1 d . . . H42A H 0.2887 -0.0790 -0.4457 0.120 Uiso 1 1 calc R . . H42B H 0.2983 -0.0290 -0.5760 0.120 Uiso 1 1 calc R . . B1A B 0.6882(8) 0.2376(8) 1.0301(16) 0.068(4) Uani 0.33 1 d PDU B -1 F1A F 0.7592(9) 0.2920(7) 1.067(2) 0.145(7) Uani 0.33 1 d PDU B -1 F2A F 0.6473(6) 0.2231(6) 1.1513(9) 0.077(2) Uani 0.33 1 d PDU B -1 F3A F 0.6293(10) 0.2702(16) 0.942(2) 0.186(10) Uani 0.33 1 d PDU B -1 F4A F 0.7175(14) 0.1665(10) 0.955(2) 0.137(9) Uani 0.33 1 d PDU B -1 B1B B 0.6877(6) 0.2234(5) 0.9202(11) 0.081(3) Uani 0.67 1 d PDU C -2 F1B F 0.7336(4) 0.2280(4) 0.7972(7) 0.114(2) Uani 0.67 1 d PDU C -2 F2B F 0.6062(4) 0.1881(5) 0.8807(8) 0.120(2) Uani 0.67 1 d PDU C -2 F3B F 0.6815(10) 0.2981(4) 1.0082(10) 0.181(5) Uani 0.67 1 d PDU C -2 F4B F 0.7339(5) 0.1745(4) 1.0038(9) 0.090(2) Uani 0.67 1 d PDU C -2 O1S O 0.9199(7) 0.2708(5) 0.4660(10) 0.207(4) Uani 1 1 d . . . O2S O 0.8638(4) 0.1570(4) 0.3934(7) 0.1185(18) Uani 1 1 d . . . N1S N 0.8583(4) 0.2289(4) 0.4224(6) 0.0839(15) Uani 1 1 d . . . C1S C 0.7772(8) 0.2649(7) 0.376(2) 0.237(9) Uani 1 1 d . . . H1SA H 0.7297 0.2222 0.3502 0.355 Uiso 1 1 calc R . . H1SB H 0.7890 0.2898 0.2906 0.355 Uiso 1 1 calc R . . H1SC H 0.7583 0.3071 0.4548 0.355 Uiso 1 1 calc R . . O3S O 0.6545(11) 0.5111(10) 0.7696(15) 0.258(6) Uani 1 1 d . . . O4S O 0.6439(8) 0.3855(8) 0.6418(10) 0.248(6) Uani 1 1 d . . . N2S N 0.6880(13) 0.4361(10) 0.7278(11) 0.204(6) Uani 1 1 d . . . C2S C 0.7680(9) 0.4142(12) 0.7877(14) 0.248(10) Uani 1 1 d . . . H2SA H 0.7954 0.4617 0.8543 0.373 Uiso 1 1 calc R . . H2SB H 0.8087 0.3959 0.7099 0.373 Uiso 1 1 calc R . . H2SC H 0.7564 0.3697 0.8413 0.373 Uiso 1 1 calc R . . O5S O 0.9708(9) 0.4294(8) 0.6939(15) 0.136(4) Uani 0.50 1 d P D -3 O6S O 0.9262(9) 0.4716(8) 0.5108(15) 0.134(5) Uani 0.50 1 d P D -3 N3S N 0.9813(9) 0.4459(8) 0.5758(13) 0.096(4) Uani 0.50 1 d P D -3 C3S C 1.0682(10) 0.4298(13) 0.5187(17) 0.117(6) Uani 0.50 1 d P D -3 H3SA H 1.0714 0.4482 0.4252 0.175 Uiso 0.50 1 calc PR D -3 H3SB H 1.0781 0.3708 0.5049 0.175 Uiso 0.50 1 calc PR D -3 H3SC H 1.1144 0.4594 0.5873 0.175 Uiso 0.50 1 calc PR D -3 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 N1 0.0228(14) 0.0239(14) 0.0301(15) -0.0028(11) 0.0028(11) 0.0004(11) N2 0.0244(14) 0.0258(14) 0.0296(15) -0.0036(11) 0.0037(11) 0.0002(11) C1A 0.101(8) 0.055(6) 0.152(13) -0.058(8) -0.001(9) 0.007(6) C2A 0.105(8) 0.078(6) 0.094(8) -0.010(6) -0.035(7) -0.033(6) C3A 0.215(17) 0.072(7) 0.088(8) -0.024(6) 0.031(9) -0.096(10) C1B 0.100(14) 0.062(10) 0.063(10) -0.036(8) 0.005(10) -0.041(10) C2B 0.086(14) 0.053(11) 0.15(2) -0.026(13) 0.022(14) -0.041(10) C3B 0.19(3) 0.024(8) 0.103(18) -0.024(10) -0.001(19) 0.008(11) C4 0.064(3) 0.036(2) 0.056(3) -0.007(2) 0.005(2) -0.008(2) C5 0.039(2) 0.0285(19) 0.048(2) -0.0065(17) 0.0090(17) 0.0022(16) C6 0.039(2) 0.0306(19) 0.053(2) 0.0059(17) 0.0142(18) 0.0027(16) C7 0.0346(19) 0.0357(19) 0.034(2) 0.0003(15) 0.0079(15) 0.0052(15) C8 0.0254(17) 0.0298(18) 0.037(2) -0.0014(15) 0.0064(14) 0.0058(14) C9 0.041(2) 0.0303(18) 0.037(2) -0.0005(15) 0.0114(16) 0.0000(15) C10 0.048(2) 0.037(2) 0.036(2) -0.0059(16) 0.0059(17) 0.0030(17) C11 0.0281(18) 0.0310(18) 0.0303(18) -0.0012(14) 0.0053(14) 0.0034(14) C12 0.0237(16) 0.0280(17) 0.0286(17) 0.0025(14) -0.0001(13) 0.0001(13) C13 0.0274(17) 0.0294(17) 0.0277(17) 0.0010(14) 0.0017(14) 0.0022(14) C14 0.0249(18) 0.039(2) 0.0329(19) 0.0019(15) 0.0027(14) -0.0020(15) C15 0.0261(18) 0.042(2) 0.043(2) -0.0026(17) 0.0107(16) -0.0039(15) C16 0.0298(19) 0.040(2) 0.037(2) -0.0055(16) 0.0130(15) 0.0050(15) C17 0.0206(17) 0.0357(19) 0.041(2) -0.0021(16) 0.0038(14) -0.0025(14) C18 0.043(2) 0.046(2) 0.041(2) 0.0019(18) 0.0050(17) -0.0079(18) C19 0.042(2) 0.055(3) 0.049(3) -0.015(2) -0.0021(19) -0.0036(19) C20 0.0242(19) 0.035(2) 0.076(3) -0.008(2) -0.0020(19) -0.0005(16) C21 0.043(2) 0.037(2) 0.076(3) 0.010(2) -0.004(2) -0.0045(18) C22 0.039(2) 0.044(2) 0.046(2) 0.0060(18) 0.0017(17) -0.0055(17) C23 0.047(3) 0.038(2) 0.104(4) -0.020(3) -0.011(3) 0.001(2) C24A 0.076(13) 0.053(10) 0.091(15) -0.018(9) 0.003(10) 0.011(8) C25A 0.069(7) 0.043(5) 0.070(7) 0.003(5) -0.024(5) -0.020(4) C26A 0.061(6) 0.033(4) 0.070(6) -0.003(4) 0.002(5) -0.005(4) C26B 0.054(6) 0.051(6) 0.101(9) -0.011(6) 0.011(6) -0.022(5) C25B 0.103(9) 0.053(6) 0.062(7) -0.012(5) -0.016(6) -0.025(6) C24B 0.066(10) 0.041(8) 0.14(2) -0.021(13) 0.004(14) 0.007(7) C27 0.0234(16) 0.0290(17) 0.0243(16) 0.0011(13) 0.0019(13) 0.0005(13) C28 0.0230(16) 0.0255(16) 0.0304(18) 0.0029(14) 0.0029(13) 0.0029(13) C29 0.0287(18) 0.0282(17) 0.0278(17) -0.0039(14) 0.0036(14) -0.0009(14) C30 0.0221(16) 0.0278(17) 0.0323(18) -0.0027(14) -0.0004(13) -0.0006(13) O1 0.0310(14) 0.0507(16) 0.0470(16) 0.0094(13) 0.0050(12) 0.0017(12) O2 0.0402(15) 0.0303(13) 0.0424(15) -0.0053(11) 0.0012(12) -0.0055(11) O3 0.215(5) 0.059(2) 0.0309(18) -0.0111(16) -0.018(2) 0.051(3) O4 0.102(3) 0.0500(19) 0.067(2) -0.0113(17) -0.026(2) 0.0192(19) C31 0.047(2) 0.036(2) 0.053(3) 0.0120(18) -0.0080(19) -0.0004(17) C32 0.077(3) 0.040(2) 0.056(3) 0.010(2) -0.021(2) 0.006(2) C33 0.078(4) 0.050(3) 0.088(4) 0.032(3) -0.046(3) -0.026(3) C34 0.052(3) 0.090(4) 0.076(4) 0.039(3) -0.016(3) -0.019(3) C35 0.038(2) 0.081(3) 0.063(3) 0.037(3) -0.007(2) -0.008(2) C36 0.039(2) 0.044(2) 0.046(2) 0.0202(18) -0.0037(17) -0.0028(17) C37 0.034(2) 0.037(2) 0.049(2) 0.0092(17) 0.0093(17) 0.0003(16) C38 0.045(2) 0.032(2) 0.057(3) 0.0015(18) 0.0076(19) -0.0071(17) C39 0.037(2) 0.037(2) 0.054(3) -0.0152(19) -0.0058(18) 0.0032(17) C40 0.067(3) 0.058(3) 0.037(2) -0.014(2) -0.004(2) -0.003(2) C41 0.105(5) 0.083(4) 0.082(4) -0.032(4) -0.024(4) 0.022(4) C42 0.166(7) 0.052(3) 0.071(4) -0.012(3) -0.063(4) 0.025(4) B1A 0.044(8) 0.046(9) 0.110(13) -0.004(8) 0.040(8) -0.010(6) F1A 0.106(9) 0.051(7) 0.26(2) -0.031(9) 0.069(10) -0.039(7) F2A 0.061(5) 0.084(6) 0.075(5) -0.015(5) 0.017(4) 0.000(4) F3A 0.086(9) 0.30(3) 0.24(2) 0.19(2) 0.083(9) 0.043(12) F4A 0.19(2) 0.042(7) 0.153(16) -0.057(8) 0.075(13) -0.036(8) B1B 0.073(6) 0.052(6) 0.115(8) -0.009(5) 0.044(6) 0.019(4) F1B 0.078(4) 0.121(5) 0.141(5) 0.013(4) 0.043(3) -0.014(3) F2B 0.063(3) 0.151(6) 0.166(6) 0.072(5) 0.038(3) 0.014(3) F3B 0.322(16) 0.043(3) 0.172(8) -0.015(4) 0.047(9) 0.064(6) F4B 0.083(4) 0.033(3) 0.132(6) -0.043(3) 0.017(4) -0.007(3) O1S 0.239(10) 0.172(7) 0.198(8) 0.034(6) -0.075(7) -0.086(7) O2S 0.113(4) 0.096(4) 0.144(5) 0.013(3) 0.007(3) 0.008(3) N1S 0.091(4) 0.077(4) 0.077(3) -0.003(3) 0.009(3) -0.022(3) C1S 0.144(10) 0.132(9) 0.48(3) 0.146(13) 0.112(13) 0.070(8) O3S 0.319(17) 0.266(15) 0.202(12) 0.084(11) 0.008(10) -0.014(13) O4S 0.258(11) 0.302(13) 0.152(7) -0.005(8) -0.076(7) -0.111(10) N2S 0.298(18) 0.215(13) 0.093(7) 0.041(8) -0.049(9) -0.100(13) C2S 0.132(10) 0.44(3) 0.125(9) -0.055(13) -0.029(8) -0.077(13) O5S 0.136(10) 0.150(11) 0.117(10) 0.014(8) 0.023(8) -0.010(8) O6S 0.133(10) 0.123(9) 0.139(10) 0.003(8) -0.033(8) 0.046(8) N3S 0.102(9) 0.113(9) 0.057(6) -0.021(6) -0.010(6) 0.004(7) C3S 0.074(9) 0.177(18) 0.092(10) 0.005(11) 0.012(8) 0.000(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 N1 C27 1.343(4) . ? N1 C12 1.389(4) . ? N1 H1A 0.8800 . ? N2 C27 1.331(4) . ? N2 C13 1.383(4) . ? N2 H2A 0.8800 . ? C1A C4 1.488(12) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C2A C4 1.492(11) . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C3A C4 1.552(11) . ? C3A H3AA 0.9800 . ? C3A H3AB 0.9800 . ? C3A H3AC 0.9800 . ? C1B C4 1.658(18) . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? C2B C4 1.45(2) . ? C2B H2BA 0.9800 . ? C2B H2BB 0.9800 . ? C2B H2BC 0.9800 . ? C3B C4 1.52(2) . ? C3B H3BA 0.9800 . ? C3B H3BB 0.9800 . ? C3B H3BC 0.9800 . ? C4 C5 1.533(5) . ? C5 C10 1.381(6) . ? C5 C6 1.397(6) . ? C6 C7 1.378(5) . ? C6 H6A 0.9500 . ? C7 C8 1.389(5) . ? C7 H7A 0.9500 . ? C8 C9 1.392(5) . ? C8 C11 1.480(5) . ? C9 C10 1.383(5) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C16 1.391(5) . ? C11 C12 1.407(5) . ? C12 C13 1.398(5) . ? C13 C14 1.386(5) . ? C14 C15 1.393(5) . ? C14 C17 1.481(5) . ? C15 C16 1.396(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.382(5) . ? C17 C22 1.388(6) . ? C18 C19 1.394(6) . ? C18 H18A 0.9500 . ? C19 C20 1.386(7) . ? C19 H19A 0.9500 . ? C20 C21 1.385(7) . ? C20 C23 1.545(6) . ? C21 C22 1.380(6) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C26B 1.334(11) . ? C23 C24A 1.41(3) . ? C23 C25A 1.486(11) . ? C23 C24B 1.52(3) . ? C23 C26A 1.720(12) . ? C23 C25B 1.726(13) . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C27 C28 1.464(4) . ? C28 C30 1.394(5) 2_655 ? C28 C29 1.395(5) . ? C29 C30 1.375(5) . ? C29 H29A 0.9500 . ? C30 C28 1.394(5) 2_655 ? C30 H30A 0.9500 . ? O1 C36 1.357(5) . ? O1 C37 1.434(4) . ? O2 C38 1.424(5) . ? O2 C39 1.429(5) . ? O3 C41 1.345(8) . ? O3 C40 1.446(6) . ? O4 C32 1.365(6) . ? O4 C42 1.442(6) . ? C31 C36 1.378(6) . ? C31 C32 1.396(6) . ? C31 H31A 0.9500 . ? C32 C33 1.411(8) . ? C33 C34 1.380(8) . ? C33 H33A 0.9500 . ? C34 C35 1.346(8) . ? C34 H34A 0.9500 . ? C35 C36 1.406(6) . ? C35 H35A 0.9500 . ? C37 C38 1.490(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.477(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.405(9) 2_655 ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C41 1.405(9) 2_655 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? B1A F4A 1.356(14) . ? B1A F2A 1.364(13) . ? B1A F1A 1.365(13) . ? B1A F3A 1.370(14) . ? B1B F2B 1.345(10) . ? B1B F3B 1.366(9) . ? B1B F1B 1.376(10) . ? B1B F4B 1.402(11) . ? O1S N1S 1.152(8) . ? O2S N1S 1.181(7) . ? N1S C1S 1.454(13) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? O3S N2S 1.352(18) . ? O4S N2S 1.213(12) . ? N2S C2S 1.39(2) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? O5S N3S 1.200(16) . ? O6S N3S 1.142(15) . ? N3S C3S 1.438(18) . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 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 C27 N1 C12 109.0(3) . . ? C27 N1 H1A 125.5 . . ? C12 N1 H1A 125.5 . . ? C27 N2 C13 110.0(3) . . ? C27 N2 H2A 125.0 . . ? C13 N2 H2A 125.0 . . ? C4 C1A H1AA 109.5 . . ? C4 C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? C4 C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C4 C2A H2AA 109.5 . . ? C4 C2A H2AB 109.5 . . ? H2AA C2A H2AB 109.5 . . ? C4 C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? C4 C3A H3AA 109.5 . . ? C4 C3A H3AB 109.5 . . ? H3AA C3A H3AB 109.5 . . ? C4 C3A H3AC 109.5 . . ? H3AA C3A H3AC 109.5 . . ? H3AB C3A H3AC 109.5 . . ? C4 C1B H1BA 109.5 . . ? C4 C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? C4 C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? C4 C2B H2BA 109.5 . . ? C4 C2B H2BB 109.5 . . ? H2BA C2B H2BB 109.5 . . ? C4 C2B H2BC 109.5 . . ? H2BA C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? C4 C3B H3BA 109.5 . . ? C4 C3B H3BB 109.5 . . ? H3BA C3B H3BB 109.5 . . ? C4 C3B H3BC 109.5 . . ? H3BA C3B H3BC 109.5 . . ? H3BB C3B H3BC 109.5 . . ? C2B C4 C1A 141.0(9) . . ? C2B C4 C2A 58.5(14) . . ? C1A C4 C2A 112.4(9) . . ? C2B C4 C3B 116.9(17) . . ? C1A C4 C3B 43.2(11) . . ? C2A C4 C3B 140.9(10) . . ? C2B C4 C5 110.6(8) . . ? C1A C4 C5 108.1(5) . . ? C2A C4 C5 109.0(5) . . ? C3B C4 C5 108.4(10) . . ? C2B C4 C3A 52.0(12) . . ? C1A C4 C3A 109.0(10) . . ? C2A C4 C3A 107.9(9) . . ? C3B C4 C3A 68.7(14) . . ? C5 C4 C3A 110.4(5) . . ? C2B C4 C1B 103.0(15) . . ? C1A C4 C1B 66.2(10) . . ? C2A C4 C1B 48.2(9) . . ? C3B C4 C1B 106.1(13) . . ? C5 C4 C1B 111.7(6) . . ? C3A C4 C1B 136.8(7) . . ? C10 C5 C6 117.0(3) . . ? C10 C5 C4 120.8(4) . . ? C6 C5 C4 122.2(4) . . ? C7 C6 C5 121.7(4) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C8 120.8(4) . . ? C6 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C7 C8 C9 117.9(3) . . ? C7 C8 C11 122.5(3) . . ? C9 C8 C11 119.6(3) . . ? C10 C9 C8 120.7(4) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C5 C10 C9 121.8(4) . . ? C5 C10 H10A 119.1 . . ? C9 C10 H10A 119.1 . . ? C16 C11 C12 114.4(3) . . ? C16 C11 C8 121.8(3) . . ? C12 C11 C8 123.8(3) . . ? N1 C12 C13 106.4(3) . . ? N1 C12 C11 131.5(3) . . ? C13 C12 C11 122.0(3) . . ? N2 C13 C14 130.7(3) . . ? N2 C13 C12 106.0(3) . . ? C14 C13 C12 123.2(3) . . ? C13 C14 C15 114.9(3) . . ? C13 C14 C17 122.1(3) . . ? C15 C14 C17 123.0(3) . . ? C14 C15 C16 122.3(3) . . ? C14 C15 H15A 118.8 . . ? C16 C15 H15A 118.8 . . ? C11 C16 C15 123.2(3) . . ? C11 C16 H16A 118.4 . . ? C15 C16 H16A 118.4 . . ? C18 C17 C22 118.2(3) . . ? C18 C17 C14 121.4(4) . . ? C22 C17 C14 120.4(3) . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C19 C18 121.3(4) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C19 C20 C21 117.4(4) . . ? C19 C20 C23 120.7(4) . . ? C21 C20 C23 121.8(4) . . ? C22 C21 C20 121.6(4) . . ? C22 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? C21 C22 C17 120.9(4) . . ? C21 C22 H22A 119.6 . . ? C17 C22 H22A 119.6 . . ? C26B C23 C24A 131.5(14) . . ? C26B C23 C25A 56.1(7) . . ? C24A C23 C25A 119.2(10) . . ? C26B C23 C24B 121.0(13) . . ? C24A C23 C24B 26.5(13) . . ? C25A C23 C24B 139.2(11) . . ? C26B C23 C20 114.4(6) . . ? C24A C23 C20 111.7(13) . . ? C25A C23 C20 109.9(5) . . ? C24B C23 C20 107.0(10) . . ? C26B C23 C26A 46.0(7) . . ? C24A C23 C26A 105.3(11) . . ? C25A C23 C26A 101.4(7) . . ? C24B C23 C26A 82.7(12) . . ? C20 C23 C26A 108.2(5) . . ? C26B C23 C25B 105.8(8) . . ? C24A C23 C25B 72.6(9) . . ? C25A C23 C25B 53.4(6) . . ? C24B C23 C25B 98.8(11) . . ? C20 C23 C25B 108.0(5) . . ? C26A C23 C25B 141.4(5) . . ? C23 C24A H24A 109.5 . . ? C23 C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23 C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C23 C25A H25A 109.5 . . ? C23 C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C23 C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C23 C26A H26A 109.5 . . ? C23 C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C23 C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C23 C26B H26D 109.5 . . ? C23 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C23 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C23 C25B H25D 109.5 . . ? C23 C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C23 C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C23 C24B H24D 109.5 . . ? C23 C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23 C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? N2 C27 N1 108.6(3) . . ? N2 C27 C28 125.5(3) . . ? N1 C27 C28 125.9(3) . . ? C30 C28 C29 119.9(3) 2_655 . ? C30 C28 C27 119.6(3) 2_655 . ? C29 C28 C27 120.5(3) . . ? C30 C29 C28 119.8(3) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C28 120.3(3) . 2_655 ? C29 C30 H30A 119.9 . . ? C28 C30 H30A 119.9 2_655 . ? C36 O1 C37 118.1(3) . . ? C38 O2 C39 112.5(3) . . ? C41 O3 C40 119.4(4) . . ? C32 O4 C42 116.1(5) . . ? C36 C31 C32 118.4(4) . . ? C36 C31 H31A 120.8 . . ? C32 C31 H31A 120.8 . . ? O4 C32 C31 113.2(5) . . ? O4 C32 C33 126.8(5) . . ? C31 C32 C33 120.0(5) . . ? C34 C33 C32 119.5(5) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C35 C34 C33 121.2(5) . . ? C35 C34 H34A 119.4 . . ? C33 C34 H34A 119.4 . . ? C34 C35 C36 119.7(5) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? O1 C36 C31 124.4(4) . . ? O1 C36 C35 114.5(4) . . ? C31 C36 C35 121.2(4) . . ? O1 C37 C38 108.0(3) . . ? O1 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O1 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? O2 C38 C37 109.6(3) . . ? O2 C38 H38A 109.7 . . ? C37 C38 H38A 109.7 . . ? O2 C38 H38B 109.7 . . ? C37 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? O2 C39 C40 110.9(3) . . ? O2 C39 H39A 109.5 . . ? C40 C39 H39A 109.5 . . ? O2 C39 H39B 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? O3 C40 C39 108.3(4) . . ? O3 C40 H40A 110.0 . . ? C39 C40 H40A 110.0 . . ? O3 C40 H40B 110.0 . . ? C39 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? O3 C41 C42 116.2(6) . 2_655 ? O3 C41 H41A 108.2 . . ? C42 C41 H41A 108.2 2_655 . ? O3 C41 H41B 108.2 . . ? C42 C41 H41B 108.2 2_655 . ? H41A C41 H41B 107.4 . . ? C41 C42 O4 110.7(6) 2_655 . ? C41 C42 H42A 109.5 2_655 . ? O4 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 2_655 . ? O4 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? F4A B1A F2A 109.9(11) . . ? F4A B1A F1A 109.1(11) . . ? F2A B1A F1A 110.8(11) . . ? F4A B1A F3A 108.6(12) . . ? F2A B1A F3A 110.4(10) . . ? F1A B1A F3A 108.0(11) . . ? F2B B1B F3B 111.3(9) . . ? F2B B1B F1B 109.0(8) . . ? F3B B1B F1B 112.7(8) . . ? F2B B1B F4B 108.4(7) . . ? F3B B1B F4B 106.0(8) . . ? F1B B1B F4B 109.3(7) . . ? O1S N1S O2S 121.3(8) . . ? O1S N1S C1S 119.4(9) . . ? O2S N1S C1S 118.3(8) . . ? N1S C1S H1SA 109.5 . . ? N1S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? N1S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O4S N2S O3S 118.6(19) . . ? O4S N2S C2S 119.5(18) . . ? O3S N2S C2S 121.8(14) . . ? N2S C2S H2SA 109.5 . . ? N2S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? N2S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O6S N3S O5S 122.9(16) . . ? O6S N3S C3S 121.4(15) . . ? O5S N3S C3S 115.6(15) . . ? N3S C3S H3SA 109.5 . . ? N3S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? N3S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.766 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.069