# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 loop_ _publ_author_name 'Paul D. Beer' 'Michael G. B. Drew' 'Vitor Felix' 'Susan E. Matthews' _publ_contact_author_name 'Prof Paul D. Beer' _publ_contact_author_address ; Chemistry University Of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email PAUL.BEER@CHEM.OX.AC.UK _publ_section_title ; Halo-Derivatised Calix[4]tube ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; data_11 _database_code_CSD 198704 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81.50 H93 Cl4 I4 N0 O11.50' _chemical_formula_weight 1905.96 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' I I -0.4742 1.8119 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.413(17) _cell_length_b 13.296(17) _cell_length_c 32.14(4) _cell_angle_alpha 81.631(10) _cell_angle_beta 81.645(10) _cell_angle_gamma 67.077(10) _cell_volume 4423(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 1.583 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.635 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 5 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19032 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.1158 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 22.40 _reflns_number_total 10452 _reflns_number_gt 7311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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. ; _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^)+(0.1650P)^2^+3.6530P] 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 10452 _refine_ls_number_parameters 938 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2674 _refine_ls_wR_factor_gt 0.2436 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.009 _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 I1 I 0.32865(8) 0.44326(8) 0.50298(2) 0.1012(3) Uani 1 1 d . . . I3 I -0.00782(9) 0.48204(10) 0.43793(3) 0.1227(4) Uani 1 1 d . . . I2 I 0.50657(16) -0.11733(9) 0.45472(3) 0.1475(5) Uani 1 1 d . . . I4 I 0.09057(10) 0.99308(8) 0.36428(4) 0.1298(4) Uani 1 1 d . . . C81 C 0.7273(9) 0.6216(8) 0.1688(3) 0.066(2) Uani 1 1 d . . . C82 C 0.7394(10) 0.6995(9) 0.1357(3) 0.076(3) Uani 1 1 d . . . H82 H 0.8000 0.7299 0.1361 0.092 Uiso 1 1 calc R . . C83 C 0.6632(11) 0.7326(8) 0.1022(3) 0.076(3) Uani 1 1 d . . . C84 C 0.5770(9) 0.6821(8) 0.1015(3) 0.067(2) Uani 1 1 d . . . H84 H 0.5277 0.7007 0.0788 0.080 Uiso 1 1 calc R . . C85 C 0.5626(8) 0.6044(7) 0.1340(3) 0.061(2) Uani 1 1 d . . . C86 C 0.6366(8) 0.5779(7) 0.1675(3) 0.059(2) Uani 1 1 d . . . C87 C 0.4714(9) 0.5474(7) 0.1305(3) 0.066(2) Uani 1 1 d . . . H87A H 0.4183 0.5483 0.1571 0.079 Uiso 1 1 calc R . . H87B H 0.4157 0.5878 0.1087 0.079 Uiso 1 1 calc R . . C71 C 0.5422(8) 0.4294(7) 0.1202(3) 0.061(2) Uani 1 1 d . . . C72 C 0.6073(9) 0.4078(8) 0.0808(3) 0.066(2) Uani 1 1 d . . . H72 H 0.6037 0.4673 0.0611 0.080 Uiso 1 1 calc R . . C73 C 0.6772(9) 0.3041(8) 0.0688(3) 0.071(2) Uani 1 1 d . . . C74 C 0.6904(8) 0.2166(8) 0.1014(3) 0.066(2) Uani 1 1 d . . . H74 H 0.7426 0.1456 0.0955 0.079 Uiso 1 1 calc R . . C75 C 0.6275(8) 0.2337(7) 0.1423(3) 0.060(2) Uani 1 1 d . . . C76 C 0.5474(8) 0.3402(7) 0.1502(3) 0.057(2) Uani 1 1 d . . . C77 C 0.6545(8) 0.1363(7) 0.1756(3) 0.067(2) Uani 1 1 d . . . H77A H 0.6354 0.0793 0.1656 0.080 Uiso 1 1 calc R . . H77B H 0.5990 0.1586 0.2012 0.080 Uiso 1 1 calc R . . C61 C 0.7945(9) 0.0900(7) 0.1855(3) 0.067(2) Uani 1 1 d . . . C62 C 0.8854(10) -0.0024(8) 0.1667(3) 0.075(3) Uani 1 1 d . . . H62 H 0.8584 -0.0356 0.1485 0.090 Uiso 1 1 calc R . . C63 C 1.0146(10) -0.0464(8) 0.1742(3) 0.074(3) Uani 1 1 d . . . C64 C 1.0504(10) 0.0104(9) 0.1994(3) 0.080(3) Uani 1 1 d . . . H64 H 1.1364 -0.0149 0.2038 0.096 Uiso 1 1 calc R . . C65 C 0.9665(9) 0.1032(7) 0.2190(3) 0.067(2) Uani 1 1 d . . . C66 C 0.8382(9) 0.1401(7) 0.2115(3) 0.062(2) Uani 1 1 d . . . C67 C 1.0161(10) 0.1675(8) 0.2426(3) 0.078(3) Uani 1 1 d . . . H67A H 1.1031 0.1233 0.2490 0.093 Uiso 1 1 calc R . . H67B H 0.9634 0.1856 0.2691 0.093 Uiso 1 1 calc R . . C51 C 1.0124(8) 0.2724(8) 0.2152(3) 0.067(2) Uani 1 1 d . . . C52 C 1.0828(10) 0.2635(10) 0.1757(3) 0.080(3) Uani 1 1 d . . . H52 H 1.1370 0.1941 0.1684 0.096 Uiso 1 1 calc R . . C53 C 1.0759(10) 0.3528(10) 0.1469(3) 0.082(3) Uani 1 1 d . . . C54 C 0.9903(9) 0.4570(9) 0.1588(3) 0.075(3) Uani 1 1 d . . . H54 H 0.9831 0.5186 0.1399 0.089 Uiso 1 1 calc R . . C55 C 0.9179(8) 0.4707(8) 0.1970(3) 0.065(2) Uani 1 1 d . . . C56 C 0.9334(7) 0.3767(7) 0.2265(3) 0.059(2) Uani 1 1 d . . . C57 C 0.8164(9) 0.5822(8) 0.2041(3) 0.070(2) Uani 1 1 d . . . H57A H 0.8565 0.6341 0.2048 0.084 Uiso 1 1 calc R . . H57B H 0.7673 0.5781 0.2311 0.084 Uiso 1 1 calc R . . C41 C 0.4132(10) 0.6833(8) 0.3454(3) 0.072(2) Uani 1 1 d . . . C42 C 0.3319(11) 0.7850(9) 0.3582(3) 0.081(3) Uani 1 1 d . . . H42 H 0.3602 0.8185 0.3759 0.098 Uiso 1 1 calc R . . C43 C 0.2094(12) 0.8386(10) 0.3453(4) 0.092(3) Uani 1 1 d . . . C44 C 0.1640(11) 0.7854(9) 0.3205(4) 0.087(3) Uani 1 1 d . . . H44 H 0.0807 0.8185 0.3130 0.105 Uiso 1 1 calc R . . C45 C 0.2426(9) 0.6835(8) 0.3070(3) 0.072(2) Uani 1 1 d . . . C46 C 0.3699(9) 0.6361(8) 0.3185(3) 0.068(2) Uani 1 1 d . . . C47 C 0.1941(9) 0.6180(8) 0.2838(3) 0.078(3) Uani 1 1 d . . . H47A H 0.1123 0.6652 0.2738 0.093 Uiso 1 1 calc R . . H47B H 0.2538 0.5910 0.2595 0.093 Uiso 1 1 calc R . . C31 C 0.1789(9) 0.5223(9) 0.3126(3) 0.072(3) Uani 1 1 d . . . C32 C 0.1082(9) 0.5371(10) 0.3507(3) 0.078(3) Uani 1 1 d . . . H32 H 0.0607 0.6081 0.3578 0.094 Uiso 1 1 calc R . . C33 C 0.1052(11) 0.4501(13) 0.3788(3) 0.092(3) Uani 1 1 d . . . C34 C 0.1716(10) 0.3431(10) 0.3696(3) 0.081(3) Uani 1 1 d . . . H34 H 0.1669 0.2851 0.3888 0.097 Uiso 1 1 calc R . . C35 C 0.2451(8) 0.3236(9) 0.3314(3) 0.069(2) Uani 1 1 d . . . C36 C 0.2456(8) 0.4129(8) 0.3015(3) 0.065(2) Uani 1 1 d . . . C37 C 0.3231(10) 0.2049(9) 0.3231(3) 0.078(3) Uani 1 1 d . . . H37A H 0.3620 0.2025 0.2942 0.093 Uiso 1 1 calc R . . H37B H 0.2668 0.1647 0.3265 0.093 Uiso 1 1 calc R . . C21 C 0.4285(10) 0.1491(8) 0.3534(3) 0.072(2) Uani 1 1 d . . . C22 C 0.4204(12) 0.0651(9) 0.3835(4) 0.086(3) Uani 1 1 d . . . H22 H 0.3550 0.0396 0.3839 0.103 Uiso 1 1 calc R . . C23 C 0.5094(14) 0.0192(10) 0.4128(3) 0.092(3) Uani 1 1 d . . . C24 C 0.5995(12) 0.0612(10) 0.4147(3) 0.089(3) Uani 1 1 d . . . H24 H 0.6549 0.0324 0.4358 0.106 Uiso 1 1 calc R . . C25 C 0.6104(10) 0.1470(8) 0.3855(3) 0.074(3) Uani 1 1 d . . . C26 C 0.5263(9) 0.1860(8) 0.3542(3) 0.068(2) Uani 1 1 d . . . C27 C 0.7016(10) 0.2036(9) 0.3879(3) 0.082(3) Uani 1 1 d . . . H27A H 0.7479 0.2088 0.3604 0.098 Uiso 1 1 calc R . . H22B H 0.7633 0.1607 0.4078 0.098 Uiso 1 1 calc R . . C11 C 0.6273(8) 0.3186(8) 0.4020(3) 0.068(2) Uani 1 1 d . . . C12 C 0.5419(10) 0.3287(9) 0.4379(3) 0.077(3) Uani 1 1 d . . . H12 H 0.5395 0.2665 0.4549 0.092 Uiso 1 1 calc R . . C13 C 0.4605(10) 0.4318(10) 0.4484(3) 0.080(3) Uani 1 1 d . . . C14 C 0.4633(10) 0.5247(9) 0.4243(3) 0.075(3) Uani 1 1 d . . . H14 H 0.4065 0.5932 0.4317 0.091 Uiso 1 1 calc R . . C15 C 0.5498(9) 0.5172(9) 0.3892(3) 0.071(2) Uani 1 1 d . . . C16 C 0.6347(8) 0.4120(8) 0.3780(3) 0.065(2) Uani 1 1 d . . . C17 C 0.5437(10) 0.6242(8) 0.3623(3) 0.076(3) Uani 1 1 d . . . H17A H 0.5590 0.6715 0.3794 0.091 Uiso 1 1 calc R . . H17B H 0.6099 0.6079 0.3389 0.091 Uiso 1 1 calc R . . O850 O 0.6227(5) 0.5035(5) 0.20061(18) 0.0634(14) Uani 1 1 d . . . C851 C 0.5064(9) 0.5430(9) 0.2302(3) 0.073(2) Uani 1 1 d . . . H85A H 0.4524 0.6171 0.2205 0.087 Uiso 1 1 calc R . . H85B H 0.4584 0.4960 0.2319 0.087 Uiso 1 1 calc R . . C852 C 0.5463(10) 0.5407(11) 0.2712(3) 0.085(3) Uani 1 1 d . . . H85C H 0.5643 0.6058 0.2722 0.102 Uiso 1 1 calc R . . H85D H 0.6241 0.4770 0.2755 0.102 Uiso 1 1 calc R . . O450 O 0.4464(6) 0.5364(5) 0.30464(19) 0.0708(16) Uani 1 1 d . . . O750 O 0.4732(5) 0.3605(5) 0.18902(16) 0.0590(13) Uani 1 1 d . . . O350 O 0.3229(5) 0.3907(5) 0.26449(17) 0.0653(15) Uani 1 1 d . . . O650 O 0.7517(6) 0.2331(5) 0.22867(18) 0.0656(15) Uani 1 1 d . . . C651 C 0.7215(10) 0.2214(10) 0.2746(4) 0.086(3) Uani 1 1 d . . . H65A H 0.7742 0.1492 0.2866 0.104 Uiso 1 1 calc R . . H65B H 0.7365 0.2762 0.2876 0.104 Uiso 1 1 calc R . . C652 C 0.5869(10) 0.2366(10) 0.2817(3) 0.087(3) Uani 1 1 d . . . H65C H 0.5776 0.1686 0.2787 0.105 Uiso 1 1 calc R . . H65D H 0.5396 0.2924 0.2608 0.105 Uiso 1 1 calc R . . O250 O 0.5350(6) 0.2703(5) 0.32464(18) 0.0685(15) Uani 1 1 d . . . O550 O 0.8608(5) 0.3862(5) 0.26579(17) 0.0613(14) Uani 1 1 d . . . C551 C 0.8985(10) 0.4190(12) 0.2994(3) 0.090(3) Uani 1 1 d . . . H55A H 0.8745 0.4979 0.2953 0.108 Uiso 1 1 calc R . . H55B H 0.9909 0.3859 0.2986 0.108 Uiso 1 1 calc R . . C552 C 0.8443(9) 0.3905(11) 0.3408(3) 0.088(3) Uani 1 1 d . . . H55C H 0.8924 0.3143 0.3500 0.106 Uiso 1 1 calc R . . H55D H 0.8511 0.4354 0.3609 0.106 Uiso 1 1 calc R . . O150 O 0.7138(6) 0.4065(5) 0.34043(18) 0.0683(15) Uani 1 1 d . . . C800 C 0.6795(13) 0.8189(11) 0.0668(4) 0.096(3) Uani 1 1 d . . . C801 C 0.616(3) 0.828(2) 0.0294(6) 0.242(16) Uani 1 1 d . . . H80A H 0.5310 0.8289 0.0380 0.290 Uiso 1 1 calc R . . H80B H 0.6634 0.7657 0.0137 0.290 Uiso 1 1 calc R . . H80C H 0.6108 0.8940 0.0120 0.290 Uiso 1 1 calc R . . C802 C 0.676(5) 0.914(2) 0.0833(7) 0.31(3) Uani 1 1 d . . . C803 C 0.821(3) 0.782(4) 0.0493(11) 0.28(2) Uani 1 1 d . . . C700 C 0.7361(11) 0.2783(9) 0.0240(3) 0.082(3) Uani 1 1 d . . . C701 C 0.857(2) 0.1771(18) 0.0218(5) 0.177(9) Uani 1 1 d . . . H70A H 0.9125 0.1783 0.0412 0.213 Uiso 1 1 calc R . . H70B H 0.8988 0.1755 -0.0064 0.213 Uiso 1 1 calc R . . H70C H 0.8359 0.1130 0.0291 0.213 Uiso 1 1 calc R . . C702 C 0.780(3) 0.3667(19) 0.0025(6) 0.212(13) Uani 1 1 d . . . H70D H 0.7155 0.4173 -0.0148 0.255 Uiso 1 1 calc R . . H70E H 0.8580 0.3348 -0.0150 0.255 Uiso 1 1 calc R . . H70F H 0.7934 0.4048 0.0233 0.255 Uiso 1 1 calc R . . C703 C 0.640(2) 0.260(3) 0.0022(5) 0.189(11) Uani 1 1 d . . . H70G H 0.6263 0.1955 0.0154 0.227 Uiso 1 1 calc R . . H70H H 0.6702 0.2514 -0.0270 0.227 Uiso 1 1 calc R . . H70I H 0.5603 0.3224 0.0041 0.227 Uiso 1 1 calc R . . C751 C 0.3579(10) 0.3370(11) 0.1945(3) 0.084(3) Uani 1 1 d . . . H75A H 0.3795 0.2591 0.2025 0.101 Uiso 1 1 calc R . . H25B H 0.3200 0.3555 0.1680 0.101 Uiso 1 1 calc R . . C752 C 0.2654(9) 0.3988(11) 0.2269(3) 0.083(3) Uani 1 1 d . . . H25C H 0.2283 0.4754 0.2160 0.099 Uiso 1 1 calc R . . H25D H 0.1971 0.3713 0.2337 0.099 Uiso 1 1 calc R . . C600 C 1.1077(11) -0.1458(10) 0.1530(4) 0.098(4) Uani 1 1 d . . . C601 C 1.235(2) -0.190(2) 0.1723(11) 0.245(17) Uani 1 1 d . . . H60A H 1.2759 -0.1380 0.1649 0.294 Uiso 1 1 calc R . . H60B H 1.2885 -0.2584 0.1618 0.294 Uiso 1 1 calc R . . H60C H 1.2194 -0.2001 0.2025 0.294 Uiso 1 1 calc R . . C602 C 1.063(3) -0.241(3) 0.1594(18) 0.34(3) Uani 1 1 d . . . H60D H 1.0122 -0.2396 0.1861 0.413 Uiso 1 1 calc R . . H60E H 1.1361 -0.3092 0.1593 0.413 Uiso 1 1 calc R . . H60F H 1.0129 -0.2358 0.1371 0.413 Uiso 1 1 calc R . . C603 C 1.117(4) -0.116(3) 0.1078(8) 0.37(3) Uani 1 1 d . . . H60G H 1.1448 -0.1811 0.0933 0.446 Uiso 1 1 calc R . . H60H H 1.1778 -0.0813 0.1004 0.446 Uiso 1 1 calc R . . H60I H 1.0350 -0.0666 0.0996 0.446 Uiso 1 1 calc R . . C503 C 1.043(2) 0.350(4) 0.0735(6) 0.32(3) Uani 1 1 d . . . H50A H 0.9617 0.3638 0.0900 0.382 Uiso 1 1 calc R . . H50B H 1.0675 0.2836 0.0604 0.382 Uiso 1 1 calc R . . H50C H 1.0355 0.4102 0.0522 0.382 Uiso 1 1 calc R . . C500 C 1.1397(14) 0.3394(14) 0.1012(4) 0.114(4) Uani 1 1 d . . . C501 C 1.265(2) 0.2315(19) 0.0979(6) 0.169(8) Uani 1 1 d . . . C502 C 1.197(3) 0.425(2) 0.0872(7) 0.229(13) Uani 1 1 d . . . H50G H 1.2850 0.3900 0.0766 0.275 Uiso 1 1 calc R . . H50H H 1.1918 0.4641 0.1107 0.275 Uiso 1 1 calc R . . H50I H 1.1509 0.4756 0.0652 0.275 Uiso 1 1 calc R . . C91 C 0.4691(18) -0.0462(17) 0.2336(6) 0.27(2) Uiso 0.50 1 d PD A 1 H91 H 0.4562 0.0094 0.2526 0.326 Uiso 0.50 1 calc PR A 1 Cl92 Cl 0.6340(11) -0.1187(12) 0.2219(4) 0.196(5) Uiso 0.50 1 d PD A 1 Cl93 Cl 0.3872(17) -0.1311(16) 0.2565(6) 0.261(8) Uiso 0.50 1 d PD A 1 Cl94 Cl 0.4008(10) 0.0212(9) 0.1840(4) 0.158(3) Uiso 0.50 1 d PD A 1 C92 C 0.4691(18) -0.0462(17) 0.2336(6) 0.27(2) Uiso 0.25 1 d P B 2 H92 H 0.5393 -0.0195 0.2279 0.326 Uiso 0.25 1 calc PR B 2 Cl95 Cl 0.547(2) -0.1676(17) 0.2106(8) 0.190(9) Uiso 0.25 1 d PD B 2 Cl96 Cl 0.459(5) -0.055(3) 0.2888(7) 0.31(2) Uiso 0.25 1 d PD B 2 Cl97 Cl 0.3621(17) 0.0594(14) 0.2079(6) 0.143(6) Uiso 0.25 1 d PD B 2 C98 C 0.765(4) -0.150(2) 0.3301(11) 0.178(16) Uiso 0.50 1 d PD C 3 H98A H 0.7836 -0.0946 0.3100 0.213 Uiso 0.50 1 calc PR C 3 H98B H 0.6740 -0.1223 0.3383 0.213 Uiso 0.50 1 calc PR C 3 Cl99 Cl 0.810(2) -0.2728(19) 0.3052(7) 0.264(8) Uiso 0.50 1 d PD C 3 Cl89 Cl 0.8464(19) -0.1691(16) 0.3755(6) 0.239(7) Uiso 0.50 1 d PD C 3 C81' C -0.053(4) 1.218(4) 0.4977(12) 0.14(2) Uiso 0.25 1 d PD D 4 H81 H -0.0782 1.2958 0.4879 0.173 Uiso 0.25 1 calc PR D 4 Cl82 Cl 0.047(5) 1.194(8) 0.5381(16) 0.44(4) Uiso 0.25 1 d PD D 4 Cl83 Cl 0.027(4) 1.147(4) 0.4530(12) 0.236(16) Uiso 0.25 1 d PD D 4 Cl84 Cl -0.196(3) 1.198(3) 0.5160(12) 0.229(13) Uiso 0.25 1 d PD D 4 O81 O 0.811(2) -0.0672(18) 0.2994(7) 0.118(6) Uiso 0.50 1 d P E 5 O82 O 0.8252(18) -0.0889(17) 0.2780(7) 0.109(5) Uiso 0.50 1 d P E 5 O83 O -0.208(3) 0.774(3) 0.3649(10) 0.115(8) Uiso 0.33 1 d P . 5 O84 O -0.036(5) 1.197(4) 0.4456(15) 0.146(13) Uiso 0.33 1 d P F 5 O85 O -0.068(4) 1.245(3) 0.5476(13) 0.155(12) Uiso 0.33 1 d P G 5 O86 O 0.769(4) -0.252(4) 0.3394(16) 0.132(13) Uiso 0.25 1 d P . 5 O87 O 0.595(6) -0.138(5) 0.3166(19) 0.176(19) Uiso 0.25 1 d P H 5 O88 O -0.143(6) 1.221(5) 0.4892(19) 0.153(16) Uiso 0.25 1 d P F 5 O89 O -0.066(6) 1.180(5) 0.469(2) 0.148(17) Uiso 0.25 1 d P F 5 O90 O 0.124(7) 1.110(6) 0.488(2) 0.18(2) Uiso 0.25 1 d P I 5 O91 O 0.161(7) 1.172(6) 0.488(2) 0.19(2) Uiso 0.25 1 d P I 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 I1 0.0928(6) 0.1285(7) 0.0796(5) -0.0132(4) 0.0054(4) -0.0422(5) I3 0.1089(7) 0.1834(11) 0.0821(5) -0.0331(5) 0.0176(4) -0.0642(7) I2 0.2385(14) 0.1191(8) 0.1128(7) 0.0390(6) -0.0477(8) -0.1044(9) I4 0.1231(7) 0.0778(6) 0.1733(10) -0.0423(6) -0.0048(6) -0.0143(5) C81 0.073(6) 0.065(5) 0.069(5) 0.007(4) -0.018(4) -0.035(5) C82 0.076(6) 0.083(7) 0.084(6) -0.005(5) -0.016(5) -0.044(6) C83 0.096(7) 0.059(5) 0.074(6) -0.003(4) -0.017(5) -0.027(6) C84 0.074(6) 0.068(6) 0.068(5) -0.010(4) -0.020(4) -0.031(5) C85 0.066(5) 0.060(5) 0.057(5) 0.002(4) -0.010(4) -0.024(4) C86 0.057(5) 0.062(5) 0.062(5) 0.000(4) -0.011(4) -0.027(4) C87 0.064(5) 0.062(5) 0.073(5) -0.001(4) -0.022(4) -0.021(5) C71 0.059(5) 0.065(5) 0.068(5) 0.004(4) -0.019(4) -0.033(4) C72 0.067(5) 0.071(6) 0.066(5) -0.002(4) -0.011(4) -0.032(5) C73 0.070(5) 0.078(7) 0.068(5) -0.006(5) -0.010(4) -0.031(5) C74 0.057(5) 0.061(5) 0.075(6) -0.008(4) -0.014(4) -0.015(4) C75 0.057(5) 0.062(6) 0.068(5) -0.013(4) -0.015(4) -0.025(5) C76 0.049(4) 0.063(6) 0.065(5) -0.010(4) -0.011(4) -0.024(4) C77 0.063(5) 0.055(5) 0.080(6) -0.007(4) -0.006(4) -0.019(4) C61 0.062(5) 0.060(5) 0.071(5) 0.002(4) -0.008(4) -0.017(5) C62 0.080(7) 0.060(6) 0.083(6) -0.009(5) -0.011(5) -0.020(5) C63 0.085(7) 0.050(5) 0.080(6) -0.010(4) -0.014(5) -0.015(5) C64 0.068(6) 0.070(6) 0.090(6) 0.000(5) -0.017(5) -0.013(5) C65 0.062(5) 0.055(5) 0.078(6) -0.005(4) -0.011(4) -0.015(5) C66 0.066(6) 0.048(5) 0.069(5) -0.013(4) -0.003(4) -0.016(5) C67 0.072(6) 0.065(6) 0.085(6) -0.002(5) -0.020(5) -0.012(5) C51 0.054(5) 0.080(7) 0.073(5) 0.000(5) -0.015(4) -0.032(5) C52 0.068(6) 0.089(7) 0.083(7) -0.017(6) -0.009(5) -0.026(5) C53 0.070(6) 0.111(9) 0.070(6) 0.000(6) -0.007(5) -0.043(6) C54 0.064(5) 0.094(7) 0.074(6) 0.005(5) -0.016(5) -0.040(6) C55 0.058(5) 0.082(6) 0.065(5) 0.009(4) -0.023(4) -0.038(5) C56 0.046(4) 0.064(6) 0.072(5) -0.010(4) -0.014(4) -0.021(4) C57 0.073(6) 0.066(6) 0.083(6) -0.005(4) -0.023(5) -0.035(5) C41 0.077(6) 0.063(6) 0.080(6) -0.012(5) 0.004(5) -0.033(5) C42 0.098(8) 0.068(7) 0.083(6) -0.013(5) -0.008(5) -0.036(6) C43 0.092(8) 0.077(7) 0.102(8) -0.015(6) -0.006(6) -0.026(7) C44 0.080(7) 0.080(8) 0.101(7) -0.011(6) -0.010(6) -0.027(6) C45 0.069(6) 0.060(6) 0.081(6) -0.011(5) -0.009(5) -0.017(5) C46 0.073(6) 0.063(6) 0.069(5) -0.010(4) 0.004(4) -0.028(5) C47 0.051(5) 0.081(7) 0.090(6) 0.001(5) -0.018(4) -0.013(5) C31 0.057(5) 0.095(8) 0.073(6) -0.010(5) -0.015(4) -0.036(5) C32 0.064(5) 0.098(7) 0.077(6) -0.011(6) -0.008(5) -0.033(5) C33 0.082(7) 0.145(12) 0.063(6) -0.018(7) -0.005(5) -0.056(8) C34 0.075(6) 0.099(8) 0.079(6) -0.009(6) -0.012(5) -0.042(6) C35 0.053(5) 0.098(7) 0.066(5) -0.012(5) -0.007(4) -0.037(5) C36 0.051(4) 0.080(7) 0.068(5) -0.010(5) -0.013(4) -0.027(5) C37 0.085(6) 0.091(7) 0.078(6) -0.007(5) -0.007(5) -0.056(6) C21 0.080(6) 0.072(6) 0.073(5) -0.005(5) -0.010(5) -0.039(5) C22 0.100(8) 0.068(6) 0.096(7) -0.003(6) -0.010(6) -0.041(6) C23 0.133(10) 0.083(7) 0.075(6) 0.005(5) -0.018(7) -0.058(8) C24 0.102(8) 0.087(7) 0.073(6) 0.015(5) -0.023(5) -0.034(7) C25 0.072(6) 0.068(6) 0.078(6) -0.001(5) -0.008(5) -0.024(5) C26 0.067(5) 0.071(6) 0.064(5) -0.001(4) -0.005(4) -0.025(5) C27 0.073(6) 0.074(7) 0.084(6) -0.007(5) -0.017(5) -0.009(5) C11 0.061(5) 0.088(7) 0.062(5) -0.005(5) -0.017(4) -0.032(5) C12 0.082(6) 0.086(7) 0.072(6) 0.001(5) -0.019(5) -0.040(6) C13 0.084(7) 0.094(8) 0.065(5) -0.019(5) -0.002(5) -0.037(7) C14 0.073(6) 0.092(7) 0.072(6) -0.017(5) -0.010(5) -0.039(6) C15 0.066(5) 0.085(7) 0.071(5) -0.013(5) -0.011(4) -0.036(5) C16 0.058(5) 0.079(6) 0.061(5) -0.007(4) -0.015(4) -0.026(5) C17 0.083(6) 0.079(6) 0.080(6) -0.013(5) -0.008(5) -0.044(6) O850 0.064(3) 0.060(3) 0.067(3) 0.003(3) -0.012(3) -0.025(3) C851 0.071(6) 0.075(6) 0.073(6) -0.003(4) -0.010(4) -0.028(5) C852 0.064(6) 0.103(8) 0.085(7) -0.014(6) -0.016(5) -0.025(6) O450 0.064(3) 0.069(4) 0.076(4) -0.015(3) -0.006(3) -0.020(3) O750 0.059(3) 0.063(3) 0.061(3) -0.008(2) -0.009(2) -0.028(3) O350 0.054(3) 0.086(4) 0.061(3) -0.007(3) -0.010(3) -0.031(3) O650 0.064(3) 0.060(4) 0.071(4) -0.007(3) -0.005(3) -0.022(3) C651 0.075(6) 0.087(7) 0.098(7) 0.001(6) -0.016(5) -0.033(6) C652 0.079(7) 0.097(8) 0.090(7) 0.019(6) -0.025(5) -0.041(6) O250 0.067(4) 0.080(4) 0.062(3) 0.005(3) -0.007(3) -0.035(3) O550 0.053(3) 0.072(4) 0.067(3) -0.004(3) -0.014(3) -0.030(3) C551 0.072(6) 0.137(10) 0.085(7) -0.028(6) -0.012(5) -0.057(7) C552 0.068(6) 0.143(10) 0.066(6) 0.005(6) -0.025(5) -0.052(6) O150 0.060(3) 0.082(4) 0.070(4) -0.008(3) -0.018(3) -0.030(3) C800 0.113(9) 0.106(9) 0.084(7) 0.028(6) -0.030(6) -0.064(7) C801 0.46(5) 0.29(3) 0.113(12) 0.102(16) -0.11(2) -0.30(3) C802 0.75(9) 0.19(2) 0.124(15) 0.051(15) -0.11(3) -0.31(4) C803 0.20(2) 0.40(5) 0.23(3) 0.17(3) -0.01(2) -0.16(3) C700 0.088(7) 0.077(7) 0.072(6) -0.022(5) -0.005(5) -0.016(6) C701 0.178(17) 0.180(19) 0.102(11) -0.024(11) 0.023(11) 0.001(14) C702 0.35(3) 0.20(2) 0.099(11) -0.039(12) 0.107(17) -0.15(2) C703 0.165(16) 0.33(3) 0.099(11) -0.089(16) -0.006(10) -0.104(19) C751 0.076(6) 0.115(9) 0.089(7) -0.025(6) 0.000(5) -0.063(7) C752 0.057(5) 0.128(9) 0.073(6) -0.017(6) -0.011(4) -0.040(6) C600 0.080(7) 0.064(7) 0.127(10) -0.028(6) -0.018(6) 0.006(6) C601 0.147(17) 0.17(2) 0.37(4) -0.16(3) -0.08(2) 0.059(16) C602 0.17(2) 0.19(3) 0.71(10) -0.28(5) 0.02(4) -0.05(2) C603 0.49(6) 0.21(3) 0.137(19) -0.043(18) 0.11(3) 0.13(3) C503 0.169(19) 0.73(8) 0.108(13) -0.15(3) -0.001(13) -0.19(3) C500 0.112(9) 0.145(12) 0.077(7) 0.001(7) -0.010(7) -0.045(9) C501 0.178(17) 0.170(18) 0.118(12) -0.038(11) 0.046(11) -0.033(14) C502 0.22(2) 0.28(3) 0.126(15) 0.044(16) 0.077(16) -0.09(2) _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 I1 C13 2.121(10) . ? I3 C33 2.133(10) . ? I2 C23 2.105(11) . ? I4 C43 2.094(11) . ? C81 C86 1.379(12) . ? C81 C82 1.403(14) . ? C81 C57 1.531(13) . ? C82 C83 1.395(15) . ? C83 C84 1.395(14) . ? C83 C800 1.538(15) . ? C84 C85 1.397(13) . ? C85 C86 1.385(12) . ? C85 C87 1.531(13) . ? C86 O850 1.381(10) . ? C87 C71 1.520(13) . ? C71 C72 1.379(13) . ? C71 C76 1.403(13) . ? C72 C73 1.377(14) . ? C73 C74 1.424(14) . ? C73 C700 1.526(14) . ? C74 C75 1.405(13) . ? C75 C76 1.391(12) . ? C75 C77 1.516(13) . ? C76 O750 1.400(10) . ? C77 C61 1.536(14) . ? C61 C66 1.392(14) . ? C61 C62 1.412(13) . ? C62 C63 1.402(15) . ? C63 C64 1.382(15) . ? C63 C600 1.516(15) . ? C64 C65 1.402(14) . ? C65 C66 1.397(13) . ? C65 C67 1.523(15) . ? C66 O650 1.377(10) . ? C67 C51 1.527(14) . ? C51 C56 1.395(13) . ? C51 C52 1.396(14) . ? C52 C53 1.379(16) . ? C53 C54 1.418(16) . ? C53 C500 1.542(17) . ? C54 C55 1.369(13) . ? C55 C56 1.424(13) . ? C55 C57 1.508(14) . ? C56 O550 1.398(10) . ? C41 C46 1.383(14) . ? C41 C42 1.390(14) . ? C41 C17 1.527(15) . ? C42 C43 1.393(17) . ? C43 C44 1.404(17) . ? C44 C45 1.391(15) . ? C45 C46 1.420(14) . ? C45 C47 1.519(15) . ? C46 O450 1.369(11) . ? C47 C31 1.511(15) . ? C31 C32 1.359(14) . ? C31 C36 1.425(14) . ? C32 C33 1.370(18) . ? C33 C34 1.379(17) . ? C34 C35 1.378(14) . ? C35 C36 1.416(14) . ? C35 C37 1.521(15) . ? C36 O350 1.369(10) . ? C37 C21 1.543(15) . ? C21 C26 1.387(14) . ? C21 C22 1.390(15) . ? C22 C23 1.386(17) . ? C23 C24 1.360(17) . ? C24 C25 1.401(15) . ? C25 C26 1.396(14) . ? C25 C27 1.519(15) . ? C26 O250 1.384(11) . ? C27 C11 1.531(15) . ? C11 C12 1.385(14) . ? C11 C16 1.388(14) . ? C12 C13 1.381(15) . ? C13 C14 1.368(16) . ? C14 C15 1.375(14) . ? C15 C16 1.419(14) . ? C15 C17 1.535(15) . ? C16 O150 1.392(11) . ? O850 C851 1.475(11) . ? C851 C852 1.448(14) . ? C852 O450 1.462(12) . ? O750 C751 1.448(11) . ? O350 C752 1.426(11) . ? O650 C651 1.466(13) . ? C651 C652 1.457(15) . ? C652 O250 1.482(13) . ? O550 C551 1.401(12) . ? C551 C552 1.447(15) . ? C552 O150 1.422(12) . ? C800 C802 1.43(2) . ? C800 C801 1.46(2) . ? C800 C803 1.53(3) . ? C700 C702 1.49(2) . ? C700 C703 1.50(2) . ? C700 C701 1.51(2) . ? C751 C752 1.459(14) . ? C600 C603 1.45(3) . ? C600 C602 1.52(3) . ? C600 C601 1.52(3) . ? C503 C500 1.47(2) . ? C500 C502 1.51(3) . ? C500 C501 1.59(3) . ? C91 Cl93 1.753(18) . ? C91 Cl92 1.761(17) . ? C91 Cl94 1.831(16) . ? C92 Cl97 1.664(15) . ? C92 Cl95 1.727(17) . ? C92 Cl96 1.749(17) . ? C98 Cl89 1.773(19) . ? C98 Cl99 1.788(19) . ? C81 Cl84 1.76(2) . ? C81 Cl83 1.76(2) . ? C81 Cl82 1.76(2) . ? O81 O82 0.76(2) . ? O83 O86 1.04(5) 1_465 ? O84 O89 0.82(6) . ? O84 O88 1.70(8) . ? O86 O83 1.04(5) 1_645 ? O88 O89 1.03(6) . ? O90 O91 1.06(8) . ? 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 C86 C81 C82 117.9(8) . . ? C86 C81 C57 120.9(8) . . ? C82 C81 C57 121.2(8) . . ? C83 C82 C81 122.0(9) . . ? C82 C83 C84 117.6(9) . . ? C82 C83 C800 120.0(10) . . ? C84 C83 C800 122.4(9) . . ? C85 C84 C83 121.7(8) . . ? C86 C85 C84 118.4(8) . . ? C86 C85 C87 122.1(8) . . ? C84 C85 C87 119.5(8) . . ? C81 C86 O850 117.8(7) . . ? C81 C86 C85 122.3(8) . . ? O850 C86 C85 119.9(8) . . ? C71 C87 C85 112.2(7) . . ? C72 C71 C76 118.2(9) . . ? C72 C71 C87 119.8(8) . . ? C76 C71 C87 121.9(8) . . ? C73 C72 C71 124.3(9) . . ? C72 C73 C74 115.5(8) . . ? C72 C73 C700 124.9(9) . . ? C74 C73 C700 119.5(9) . . ? C75 C74 C73 122.5(9) . . ? C76 C75 C74 117.9(8) . . ? C76 C75 C77 123.7(8) . . ? C74 C75 C77 118.4(8) . . ? C75 C76 O750 120.3(8) . . ? C75 C76 C71 121.0(8) . . ? O750 C76 C71 118.7(8) . . ? C75 C77 C61 111.6(7) . . ? C66 C61 C62 117.3(9) . . ? C66 C61 C77 121.7(8) . . ? C62 C61 C77 120.9(9) . . ? C63 C62 C61 122.9(10) . . ? C64 C63 C62 115.8(9) . . ? C64 C63 C600 123.7(10) . . ? C62 C63 C600 120.4(10) . . ? C63 C64 C65 124.8(10) . . ? C66 C65 C64 116.4(9) . . ? C66 C65 C67 122.0(8) . . ? C64 C65 C67 121.2(9) . . ? O650 C66 C61 118.0(8) . . ? O650 C66 C65 119.2(8) . . ? C61 C66 C65 122.6(8) . . ? C65 C67 C51 109.1(8) . . ? C56 C51 C52 118.5(9) . . ? C56 C51 C67 122.7(8) . . ? C52 C51 C67 118.6(10) . . ? C53 C52 C51 123.1(11) . . ? C52 C53 C54 116.7(9) . . ? C52 C53 C500 121.8(12) . . ? C54 C53 C500 120.7(11) . . ? C55 C54 C53 122.8(9) . . ? C54 C55 C56 118.4(9) . . ? C54 C55 C57 118.5(9) . . ? C56 C55 C57 122.8(8) . . ? C51 C56 O550 118.8(8) . . ? C51 C56 C55 120.3(8) . . ? O550 C56 C55 120.6(8) . . ? C55 C57 C81 110.3(7) . . ? C46 C41 C42 117.9(10) . . ? C46 C41 C17 121.5(9) . . ? C42 C41 C17 120.6(9) . . ? C41 C42 C43 122.2(10) . . ? C42 C43 C44 118.9(11) . . ? C42 C43 I4 121.1(9) . . ? C44 C43 I4 120.0(9) . . ? C45 C44 C43 120.6(11) . . ? C44 C45 C46 118.2(9) . . ? C44 C45 C47 122.4(9) . . ? C46 C45 C47 119.2(9) . . ? O450 C46 C41 120.3(9) . . ? O450 C46 C45 117.6(8) . . ? C41 C46 C45 121.9(9) . . ? C31 C47 C45 110.8(8) . . ? C32 C31 C36 118.1(10) . . ? C32 C31 C47 121.3(10) . . ? C36 C31 C47 120.5(8) . . ? C31 C32 C33 121.6(11) . . ? C32 C33 C34 121.7(10) . . ? C32 C33 I3 118.7(10) . . ? C34 C33 I3 119.6(9) . . ? C35 C34 C33 119.0(11) . . ? C34 C35 C36 119.7(10) . . ? C34 C35 C37 117.9(10) . . ? C36 C35 C37 122.4(8) . . ? O350 C36 C35 118.2(9) . . ? O350 C36 C31 121.7(8) . . ? C35 C36 C31 119.6(8) . . ? C35 C37 C21 111.8(8) . . ? C26 C21 C22 118.1(9) . . ? C26 C21 C37 122.2(8) . . ? C22 C21 C37 119.5(9) . . ? C23 C22 C21 120.3(11) . . ? C24 C23 C22 120.6(10) . . ? C24 C23 I2 119.4(9) . . ? C22 C23 I2 120.0(9) . . ? C23 C24 C25 121.2(10) . . ? C26 C25 C24 117.1(10) . . ? C26 C25 C27 118.9(9) . . ? C24 C25 C27 123.9(10) . . ? O250 C26 C21 118.8(8) . . ? O250 C26 C25 118.6(9) . . ? C21 C26 C25 122.4(9) . . ? C25 C27 C11 110.1(8) . . ? C12 C11 C16 119.8(10) . . ? C12 C11 C27 117.8(9) . . ? C16 C11 C27 122.1(8) . . ? C11 C12 C13 119.5(10) . . ? C14 C13 C12 121.4(9) . . ? C14 C13 I1 120.4(8) . . ? C12 C13 I1 118.3(8) . . ? C13 C14 C15 120.3(10) . . ? C14 C15 C16 119.1(10) . . ? C14 C15 C17 117.6(9) . . ? C16 C15 C17 123.1(8) . . ? C11 C16 O150 122.1(8) . . ? C11 C16 C15 119.7(8) . . ? O150 C16 C15 117.9(8) . . ? C41 C17 C15 110.6(8) . . ? C86 O850 C851 116.2(7) . . ? C852 C851 O850 107.6(8) . . ? C851 C852 O450 110.5(8) . . ? C46 O450 C852 114.3(8) . . ? C76 O750 C751 116.5(6) . . ? C36 O350 C752 118.5(6) . . ? C66 O650 C651 115.5(7) . . ? C652 C651 O650 106.2(9) . . ? C651 C652 O250 109.7(9) . . ? C26 O250 C652 114.3(8) . . ? C56 O550 C551 120.4(7) . . ? O550 C551 C552 114.8(9) . . ? O150 C552 C551 111.3(8) . . ? C16 O150 C552 120.5(6) . . ? C802 C800 C801 121.3(19) . . ? C802 C800 C803 95(3) . . ? C801 C800 C803 102(2) . . ? C802 C800 C83 111.9(12) . . ? C801 C800 C83 114.0(11) . . ? C803 C800 C83 108.9(14) . . ? C702 C700 C703 114.6(18) . . ? C702 C700 C701 102.8(16) . . ? C703 C700 C701 107.7(16) . . ? C702 C700 C73 110.2(10) . . ? C703 C700 C73 107.4(10) . . ? C701 C700 C73 114.3(10) . . ? O750 C751 C752 111.4(8) . . ? O350 C752 C751 111.8(8) . . ? C603 C600 C602 106(3) . . ? C603 C600 C63 108.5(13) . . ? C602 C600 C63 113.1(15) . . ? C603 C600 C601 115(3) . . ? C602 C600 C601 105(2) . . ? C63 C600 C601 110.0(13) . . ? C503 C500 C502 111(2) . . ? C503 C500 C53 108.6(13) . . ? C502 C500 C53 110.0(14) . . ? C503 C500 C501 115(2) . . ? C502 C500 C501 99.7(16) . . ? C53 C500 C501 112.6(12) . . ? Cl93 C91 Cl92 113.2(12) . . ? Cl93 C91 Cl94 107.3(12) . . ? Cl92 C91 Cl94 108.0(11) . . ? Cl97 C92 Cl95 119.6(13) . . ? Cl97 C92 Cl96 119.3(13) . . ? Cl95 C92 Cl96 116.6(13) . . ? Cl89 C98 Cl99 113.0(16) . . ? Cl84 C81 Cl83 112.3(17) . . ? Cl84 C81 Cl82 113.1(18) . . ? Cl83 C81 Cl82 113.6(18) . . ? _refine_diff_density_max 0.843 _refine_diff_density_min -1.120 _refine_diff_density_rms 0.128 data_12 _database_code_CSD 198705 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C109 H114 Br4 O7' _chemical_formula_weight 1855.64 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' Br Br -0.2901 2.4595 '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 32.85(4) _cell_length_b 13.692(19) _cell_length_c 47.55(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.546(10) _cell_angle_gamma 90.00 _cell_volume 21151(49) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7712 _exptl_absorpt_coefficient_mu 1.572 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.441 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 5 min.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21071 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.3211 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 22.60 _reflns_number_total 12553 _reflns_number_gt 3433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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. ; _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^)+(0.1553P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00025(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12553 _refine_ls_number_parameters 830 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.2825 _refine_ls_R_factor_gt 0.1262 _refine_ls_wR_factor_ref 0.3511 _refine_ls_wR_factor_gt 0.3100 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.102 _refine_ls_shift/su_mean 0.013 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 Br1 Br 0.01593(7) 0.51714(16) 0.04123(5) 0.1371(10) Uani 1 1 d . . . Br2 Br 0.06991(10) 0.0108(2) 0.07519(7) 0.2120(15) Uani 1 1 d . . . Br3 Br 0.09585(7) 0.38843(17) -0.03631(5) 0.1568(11) Uani 1 1 d . . . Br4 Br 0.15105(8) 0.89466(17) -0.00978(6) 0.1666(12) Uani 1 1 d . . . C11 C 0.1255(5) 0.6082(10) 0.0889(3) 0.054(4) Uani 1 1 d . . . C12 C 0.0904(6) 0.6007(12) 0.0699(4) 0.078(5) Uani 1 1 d . . . H12 H 0.0843 0.6503 0.0566 0.093 Uiso 1 1 calc R . . C13 C 0.0640(5) 0.5253(14) 0.0694(3) 0.063(4) Uani 1 1 d . . . C14 C 0.0731(5) 0.4418(12) 0.0853(3) 0.060(5) Uani 1 1 d . . . H14 H 0.0564 0.3867 0.0830 0.072 Uiso 1 1 calc R . . C15 C 0.1070(7) 0.4448(12) 0.1042(4) 0.079(5) Uani 1 1 d . . . C16 C 0.1347(6) 0.5281(13) 0.1078(3) 0.068(5) Uani 1 1 d . . . C17 C 0.1243(4) 0.3507(10) 0.1212(3) 0.071(5) Uani 1 1 d . . . H17A H 0.1503 0.3663 0.1328 0.085 Uiso 1 1 calc R . . H17B H 0.1051 0.3308 0.1338 0.085 Uiso 1 1 calc R . . C21 C 0.1303(7) 0.2700(12) 0.1022(3) 0.071(5) Uani 1 1 d . . . C22 C 0.1012(7) 0.1963(15) 0.0980(4) 0.125(7) Uani 1 1 d . . . H22 H 0.0779 0.1953 0.1069 0.149 Uiso 1 1 calc R . . C23 C 0.1110(8) 0.1158(15) 0.0774(6) 0.121(9) Uani 1 1 d . . . C24 C 0.1395(8) 0.1248(16) 0.0625(4) 0.107(7) Uani 1 1 d . . . H24 H 0.1406 0.0775 0.0486 0.129 Uiso 1 1 calc R . . C25 C 0.1691(6) 0.1961(13) 0.0643(4) 0.075(5) Uani 1 1 d . . . C26 C 0.1641(6) 0.2680(15) 0.0866(4) 0.082(6) Uani 1 1 d . . . C27 C 0.1987(5) 0.2077(12) 0.0452(4) 0.092(6) Uani 1 1 d . . . H27A H 0.1971 0.1507 0.0329 0.110 Uiso 1 1 calc R . . H27B H 0.2259 0.2081 0.0563 0.110 Uiso 1 1 calc R . . C31 C 0.1946(7) 0.3035(16) 0.0252(3) 0.085(6) Uani 1 1 d . . . C32 C 0.1546(5) 0.3080(12) 0.0057(4) 0.066(5) Uani 1 1 d . . . H32 H 0.1354 0.2578 0.0044 0.079 Uiso 1 1 calc R . . C33 C 0.1484(6) 0.3921(17) -0.0101(4) 0.088(7) Uani 1 1 d . . . C34 C 0.1705(8) 0.4627(17) -0.0064(4) 0.093(6) Uani 1 1 d . . . H34 H 0.1618 0.5185 -0.0168 0.111 Uiso 1 1 calc R . . C35 C 0.2094(7) 0.4694(17) 0.0126(4) 0.095(6) Uani 1 1 d . . . C36 C 0.2177(7) 0.3848(16) 0.0285(4) 0.090(6) Uani 1 1 d . . . C37 C 0.2331(5) 0.5537(13) 0.0164(3) 0.077(5) Uani 1 1 d . . . H37A H 0.2424 0.5702 -0.0015 0.093 Uiso 1 1 calc R . . H37B H 0.2573 0.5408 0.0302 0.093 Uiso 1 1 calc R . . C41 C 0.2113(5) 0.6363(14) 0.0259(5) 0.081(5) Uani 1 1 d . . . C42 C 0.1915(7) 0.7257(18) 0.0086(4) 0.111(7) Uani 1 1 d . . . H42 H 0.1979 0.7353 -0.0096 0.133 Uiso 1 1 calc R . . C43 C 0.1659(7) 0.7893(13) 0.0182(6) 0.093(7) Uani 1 1 d . . . C44 C 0.1535(6) 0.7808(14) 0.0423(5) 0.097(6) Uani 1 1 d . . . H44 H 0.1332 0.8220 0.0473 0.116 Uiso 1 1 calc R . . C45 C 0.1707(6) 0.7087(14) 0.0610(4) 0.080(6) Uani 1 1 d . . . C46 C 0.1976(6) 0.6422(12) 0.0526(4) 0.072(5) Uani 1 1 d . . . C47 C 0.1539(5) 0.6980(12) 0.0892(4) 0.093(6) Uani 1 1 d . . . H47A H 0.1387 0.7563 0.0926 0.112 Uiso 1 1 calc R . . H47B H 0.1767 0.6914 0.1045 0.112 Uiso 1 1 calc R . . C51 C 0.3097(5) 0.6356(9) 0.1851(3) 0.053(4) Uani 1 1 d . . . C52 C 0.3447(5) 0.6377(13) 0.2064(4) 0.075(5) Uani 1 1 d . . . H52 H 0.3628 0.6901 0.2072 0.090 Uiso 1 1 calc R . . C53 C 0.3521(5) 0.5662(14) 0.2252(3) 0.060(4) Uani 1 1 d . . . C54 C 0.3261(6) 0.4886(13) 0.2247(4) 0.090(6) Uani 1 1 d . . . H54 H 0.3320 0.4406 0.2385 0.108 Uiso 1 1 calc R . . C55 C 0.2909(6) 0.4771(10) 0.2044(4) 0.068(5) Uani 1 1 d . . . C56 C 0.2772(5) 0.5499(9) 0.1842(4) 0.061(5) Uani 1 1 d . . . C57 C 0.2654(5) 0.3852(11) 0.2031(3) 0.086(5) Uani 1 1 d . . . H57A H 0.2399 0.3956 0.1903 0.103 Uiso 1 1 calc R . . H57B H 0.2585 0.3713 0.2218 0.103 Uiso 1 1 calc R . . C61 C 0.2888(4) 0.2935(10) 0.1924(4) 0.065(5) Uani 1 1 d . . . C62 C 0.3016(4) 0.2161(11) 0.2121(3) 0.076(5) Uani 1 1 d D . . H62 H 0.2938 0.2198 0.2301 0.091 Uiso 1 1 calc R . . C63 C 0.3243(5) 0.1378(9) 0.2062(3) 0.078(5) Uani 1 1 d D . . C64 C 0.3372(5) 0.1423(11) 0.1793(4) 0.081(5) Uani 1 1 d D . . H64 H 0.3560 0.0957 0.1751 0.097 Uiso 1 1 calc R . . C65 C 0.3236(5) 0.2126(12) 0.1584(4) 0.067(5) Uani 1 1 d . . . C66 C 0.2990(5) 0.2905(13) 0.1646(4) 0.070(5) Uani 1 1 d . . . C67 C 0.3377(5) 0.2181(10) 0.1292(3) 0.074(5) Uani 1 1 d . . . H67A H 0.3136 0.2286 0.1151 0.088 Uiso 1 1 calc R . . H67B H 0.3491 0.1550 0.1253 0.088 Uiso 1 1 calc R . . C71 C 0.3696(6) 0.2969(13) 0.1250(4) 0.069(5) Uani 1 1 d . . . C72 C 0.4094(7) 0.2982(11) 0.1439(3) 0.066(5) Uani 1 1 d . . . H72 H 0.4158 0.2477 0.1569 0.080 Uiso 1 1 calc R . . C73 C 0.4355(5) 0.3670(14) 0.1429(3) 0.065(5) Uani 1 1 d . . . C74 C 0.4268(6) 0.4485(11) 0.1237(4) 0.082(5) Uani 1 1 d . . . H74 H 0.4458 0.4984 0.1229 0.098 Uiso 1 1 calc R . . C75 C 0.3876(7) 0.4488(14) 0.1061(4) 0.076(5) Uani 1 1 d . . . C76 C 0.3641(5) 0.3711(13) 0.1055(4) 0.051(4) Uani 1 1 d . . . C77 C 0.3774(4) 0.5375(10) 0.0881(3) 0.068(4) Uani 1 1 d . . . H77A H 0.3988 0.5478 0.0763 0.082 Uiso 1 1 calc R . . H77B H 0.3518 0.5265 0.0755 0.082 Uiso 1 1 calc R . . C81 C 0.3735(6) 0.6268(13) 0.1053(4) 0.074(5) Uani 1 1 d . . . C82 C 0.4030(5) 0.7065(11) 0.1098(3) 0.082(5) Uani 1 1 d D . . H82 H 0.4257 0.7013 0.1002 0.098 Uiso 1 1 calc R . . C83 C 0.4019(5) 0.7902(10) 0.1267(3) 0.104(8) Uani 1 1 d D . . C84 C 0.3688(5) 0.7845(9) 0.1425(3) 0.083(6) Uani 1 1 d D . . H84 H 0.3667 0.8361 0.1550 0.099 Uiso 1 1 calc R . . C85 C 0.3358(5) 0.7042(11) 0.1419(3) 0.067(5) Uani 1 1 d . . . C86 C 0.3432(6) 0.6294(9) 0.1221(3) 0.059(5) Uani 1 1 d . . . C87 C 0.3025(5) 0.7085(9) 0.1609(3) 0.061(4) Uani 1 1 d . . . H87A H 0.3016 0.7739 0.1686 0.073 Uiso 1 1 calc R . . H87B H 0.2760 0.6954 0.1495 0.073 Uiso 1 1 calc R . . C151 C 0.1701(5) 0.5686(11) 0.1569(4) 0.092(5) Uiso 1 1 d . . . H15A H 0.1502 0.6211 0.1566 0.111 Uiso 1 1 calc R . . H15B H 0.1603 0.5139 0.1669 0.111 Uiso 1 1 calc R . . C152 C 0.2076(5) 0.5996(10) 0.1712(3) 0.076(5) Uiso 1 1 d . . . H15C H 0.2069 0.5957 0.1915 0.091 Uiso 1 1 calc R . . H15D H 0.2117 0.6675 0.1665 0.091 Uiso 1 1 calc R . . C251 C 0.2291(6) 0.3158(12) 0.1062(4) 0.101(6) Uiso 1 1 d . . . H25A H 0.2506 0.3386 0.0959 0.121 Uiso 1 1 calc R . . H25B H 0.2301 0.2450 0.1062 0.121 Uiso 1 1 calc R . . C252 C 0.2386(5) 0.3472(11) 0.1341(4) 0.096(6) Uiso 1 1 d . . . H25C H 0.2260 0.3024 0.1461 0.115 Uiso 1 1 calc R . . H25D H 0.2260 0.4106 0.1356 0.115 Uiso 1 1 calc R . . C351 C 0.2938(6) 0.3501(12) 0.0369(4) 0.112(6) Uiso 1 1 d . . . H35A H 0.3038 0.4082 0.0285 0.134 Uiso 1 1 calc R . . H35B H 0.2886 0.3004 0.0223 0.134 Uiso 1 1 calc R . . C352 C 0.3256(4) 0.3140(10) 0.0608(3) 0.074(4) Uiso 1 1 d . . . H35C H 0.3200 0.2463 0.0648 0.088 Uiso 1 1 calc R . . H35D H 0.3527 0.3171 0.0550 0.088 Uiso 1 1 calc R . . C451 C 0.2418(6) 0.5998(14) 0.0995(5) 0.152(8) Uiso 1 1 d . . . H45A H 0.2408 0.6697 0.1025 0.182 Uiso 1 1 calc R . . H45B H 0.2366 0.5652 0.1164 0.182 Uiso 1 1 calc R . . C452 C 0.2786(6) 0.5696(12) 0.0900(4) 0.119(6) Uiso 1 1 d . . . H45C H 0.2875 0.6167 0.0770 0.142 Uiso 1 1 calc R . . H45D H 0.2753 0.5062 0.0808 0.142 Uiso 1 1 calc R . . C500 C 0.3873(6) 0.5802(13) 0.2501(4) 0.106(6) Uiso 1 1 d . . . C501 C 0.4258(7) 0.6147(17) 0.2360(5) 0.220(11) Uiso 1 1 d . . . H50A H 0.4193 0.6746 0.2259 0.264 Uiso 1 1 calc R . . H50B H 0.4325 0.5654 0.2231 0.264 Uiso 1 1 calc R . . H50C H 0.4489 0.6250 0.2506 0.264 Uiso 1 1 calc R . . C502 C 0.4063(8) 0.4927(19) 0.2610(6) 0.233(12) Uiso 1 1 d . . . H50D H 0.4324 0.5074 0.2722 0.280 Uiso 1 1 calc R . . H50E H 0.4104 0.4506 0.2456 0.280 Uiso 1 1 calc R . . H50F H 0.3889 0.4607 0.2728 0.280 Uiso 1 1 calc R . . C503 C 0.3859(8) 0.6679(19) 0.2651(6) 0.217(11) Uiso 1 1 d . . . H50G H 0.3847 0.7201 0.2512 0.260 Uiso 1 1 calc R . . H50H H 0.4122 0.6742 0.2773 0.260 Uiso 1 1 calc R . . C504 C 0.3484(8) 0.6917(17) 0.2857(6) 0.168(9) Uiso 1 1 d . . . C505 C 0.3039(7) 0.6697(15) 0.2722(5) 0.185(9) Uiso 1 1 d . . . H50I H 0.2852 0.6954 0.2840 0.221 Uiso 1 1 calc R . . H50J H 0.3001 0.6003 0.2703 0.221 Uiso 1 1 calc R . . H50K H 0.2985 0.6996 0.2537 0.221 Uiso 1 1 calc R . . C506 C 0.3595(6) 0.8007(12) 0.2915(4) 0.145(7) Uiso 1 1 d . . . H50L H 0.3463 0.8398 0.2760 0.174 Uiso 1 1 calc R . . H50M H 0.3888 0.8090 0.2933 0.174 Uiso 1 1 calc R . . H50N H 0.3502 0.8210 0.3088 0.174 Uiso 1 1 calc R . . C507 C 0.3605(12) 0.634(3) 0.3100(9) 0.38(2) Uiso 1 1 d . . . H50O H 0.3365 0.6088 0.3167 0.458 Uiso 1 1 calc R . . H50P H 0.3760 0.6735 0.3245 0.458 Uiso 1 1 calc R . . H50Q H 0.3773 0.5811 0.3052 0.458 Uiso 1 1 calc R . . C600 C 0.3324(4) 0.0455(9) 0.2254(3) 0.094(5) Uiso 1 1 d D . . C601 C 0.3254(6) -0.0460(11) 0.2064(4) 0.221(11) Uiso 1 1 d D . . H60A H 0.3256 -0.1031 0.2182 0.265 Uiso 1 1 calc R . . H60B H 0.3469 -0.0510 0.1949 0.265 Uiso 1 1 calc R . . H60C H 0.2993 -0.0410 0.1944 0.265 Uiso 1 1 calc R . . C602 C 0.3785(5) 0.0450(12) 0.2381(4) 0.251(13) Uiso 1 1 d D . . H60D H 0.3847 -0.0146 0.2489 0.301 Uiso 1 1 calc R . . H60E H 0.3950 0.0458 0.2228 0.301 Uiso 1 1 calc R . . C603 C 0.3039(6) 0.0408(14) 0.2478(4) 0.219(11) Uiso 1 1 d D . . C604 C 0.3897(6) 0.1324(15) 0.2574(4) 0.300 Uiso 1 1 d D . . C605 C 0.4061(6) 0.2178(13) 0.2413(4) 0.221(12) Uiso 1 1 d D . . H60I H 0.3957 0.2125 0.2214 0.265 Uiso 1 1 calc R . . H60J H 0.4356 0.2157 0.2440 0.265 Uiso 1 1 calc R . . H60K H 0.3972 0.2785 0.2485 0.265 Uiso 1 1 calc R . . C606 C 0.3496(6) 0.1742(16) 0.2689(5) 0.300 Uiso 1 1 d D . . C607 C 0.4192(7) 0.1036(18) 0.2845(4) 0.300 Uiso 1 1 d D . . H60O H 0.4442 0.0781 0.2792 0.360 Uiso 1 1 calc R . . H60P H 0.4064 0.0547 0.2947 0.360 Uiso 1 1 calc R . . H60Q H 0.4252 0.1601 0.2963 0.360 Uiso 1 1 calc R . . C700 C 0.4751(6) 0.3598(13) 0.1632(5) 0.120(6) Uiso 1 1 d . . . C701 C 0.5009(5) 0.2652(12) 0.1592(4) 0.115(6) Uiso 1 1 d . . . H70A H 0.5247 0.2669 0.1740 0.139 Uiso 1 1 calc R . . H70B H 0.4843 0.2101 0.1635 0.139 Uiso 1 1 calc R . . C702 C 0.5070(6) 0.4553(13) 0.1594(4) 0.149(8) Uiso 1 1 d . . . H70C H 0.5285 0.4576 0.1755 0.179 Uiso 1 1 calc R . . H70D H 0.4917 0.5151 0.1584 0.179 Uiso 1 1 calc R . . H70E H 0.5190 0.4470 0.1423 0.179 Uiso 1 1 calc R . . C703 C 0.4718(8) 0.3809(19) 0.1934(6) 0.259(14) Uiso 1 1 d . . . H70F H 0.4626 0.3234 0.2022 0.311 Uiso 1 1 calc R . . H70G H 0.4524 0.4328 0.1944 0.311 Uiso 1 1 calc R . . H70H H 0.4982 0.4001 0.2033 0.311 Uiso 1 1 calc R . . C704 C 0.5170(7) 0.2399(13) 0.1315(5) 0.124(7) Uiso 1 1 d . . . C705 C 0.4849(8) 0.2452(18) 0.1096(5) 0.222(12) Uiso 1 1 d . . . H70I H 0.4822 0.1841 0.0996 0.266 Uiso 1 1 calc R . . H70J H 0.4900 0.2964 0.0968 0.266 Uiso 1 1 calc R . . H70K H 0.4599 0.2588 0.1171 0.266 Uiso 1 1 calc R . . C706 C 0.5343(6) 0.1319(13) 0.1391(4) 0.160(8) Uiso 1 1 d . . . H70L H 0.5167 0.0991 0.1505 0.192 Uiso 1 1 calc R . . H70M H 0.5616 0.1361 0.1495 0.192 Uiso 1 1 calc R . . H70N H 0.5350 0.0959 0.1219 0.192 Uiso 1 1 calc R . . C707 C 0.5641(9) 0.280(2) 0.1313(6) 0.272(15) Uiso 1 1 d . . . H70O H 0.5817 0.2260 0.1282 0.327 Uiso 1 1 calc R . . H70P H 0.5740 0.3102 0.1492 0.327 Uiso 1 1 calc R . . H70Q H 0.5641 0.3266 0.1162 0.327 Uiso 1 1 calc R . . C800 C 0.4275(5) 0.8867(11) 0.1370(3) 0.136(7) Uiso 1 1 d D . . C801 C 0.4177(7) 0.9059(18) 0.1694(4) 0.300 Uiso 1 1 d D . . C802 C 0.4710(5) 0.8647(14) 0.1404(4) 0.300 Uiso 1 1 d D . . H80D H 0.4861 0.9253 0.1394 0.360 Uiso 1 1 calc R . . H80E H 0.4763 0.8239 0.1247 0.360 Uiso 1 1 calc R . . C803 C 0.4056(5) 0.9711(10) 0.1210(4) 0.164(8) Uiso 1 1 d D . . H80F H 0.4248 1.0235 0.1199 0.197 Uiso 1 1 calc R . . H80G H 0.3837 0.9932 0.1307 0.197 Uiso 1 1 calc R . . H80H H 0.3945 0.9504 0.1021 0.197 Uiso 1 1 calc R . . C804 C 0.4883(5) 0.8112(12) 0.1693(4) 0.177(9) Uiso 1 1 d D . . C805 C 0.4851(7) 0.8675(17) 0.1966(4) 0.300 Uiso 1 1 d D . . C806 C 0.5357(5) 0.8049(18) 0.1670(5) 0.300 Uiso 1 1 d D . . H80L H 0.5448 0.8660 0.1603 0.360 Uiso 1 1 calc R . . H80M H 0.5402 0.7539 0.1540 0.360 Uiso 1 1 calc R . . H80N H 0.5509 0.7909 0.1854 0.360 Uiso 1 1 calc R . . C807 C 0.4695(5) 0.7102(10) 0.1708(3) 0.114(6) Uiso 1 1 d D . . O150 O 0.1730(3) 0.5390(6) 0.1274(2) 0.065(3) Uani 1 1 d . . . O250 O 0.1924(3) 0.3437(6) 0.09157(18) 0.061(3) Uani 1 1 d . . . O350 O 0.2548(4) 0.3731(6) 0.0483(2) 0.071(3) Uani 1 1 d . . . O450 O 0.2123(3) 0.5651(6) 0.0716(2) 0.062(3) Uani 1 1 d . . . O550 O 0.2413(3) 0.5442(6) 0.16460(19) 0.066(3) Uani 1 1 d . . . O650 O 0.2817(3) 0.3552(6) 0.1454(2) 0.060(3) Uani 1 1 d . . . O750 O 0.3256(3) 0.3712(6) 0.0862(2) 0.072(3) Uani 1 1 d . . . O850 O 0.3099(3) 0.5646(6) 0.11910(18) 0.063(3) Uani 1 1 d . . . O980 O 0.4024(8) 0.4026(17) 0.0219(5) 0.144(9) Uiso 0.50 1 d P . . O981 O 0.2904(7) 0.0161(15) 0.0750(5) 0.120(8) Uiso 0.50 1 d P . . O982 O 0.0405(7) 0.7981(16) 0.0159(5) 0.135(9) Uiso 0.50 1 d P . . O983 O 0.2508(10) 0.890(2) 0.0836(7) 0.192(12) Uiso 0.50 1 d P . . O984 O 0.2985(10) 0.850(2) 0.0716(7) 0.189(12) Uiso 0.50 1 d P . . O985 O 0.2791(10) 0.981(2) 0.1161(7) 0.206(13) Uiso 0.50 1 d P . . O986 O -0.0297(12) 0.771(3) -0.0187(8) 0.252(17) Uiso 0.50 1 d P . . O987 O 0.0587(11) 0.704(2) -0.0127(8) 0.227(14) Uiso 0.50 1 d P . . O988 O 0.2351(10) 1.030(2) 0.1509(7) 0.211(14) Uiso 0.50 1 d P . . O989 O 0.0293(11) 0.779(2) -0.0506(8) 0.234(15) Uiso 0.50 1 d P . . O990 O 0.4530(12) 0.386(3) 0.0361(8) 0.244(16) Uiso 0.50 1 d P . . O991 O 0.1694(10) 0.942(2) 0.1357(7) 0.220(14) Uiso 0.50 1 d P . . 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 Br1 0.1090(19) 0.1582(19) 0.131(2) 0.0182(15) -0.0250(15) -0.0061(14) Br2 0.234(3) 0.162(2) 0.240(4) -0.029(2) 0.037(3) -0.074(2) Br3 0.135(2) 0.176(2) 0.141(2) -0.0123(17) -0.0400(17) 0.0175(16) Br4 0.157(2) 0.167(2) 0.176(3) 0.0934(19) 0.0250(19) 0.0163(17) C11 0.046(13) 0.059(11) 0.060(12) 0.014(9) 0.019(10) 0.003(9) C12 0.069(15) 0.065(12) 0.093(15) 0.023(10) -0.005(12) -0.009(11) C13 0.068(13) 0.073(12) 0.040(11) 0.010(9) -0.016(9) 0.013(11) C14 0.037(12) 0.093(14) 0.045(12) -0.009(10) -0.011(9) -0.010(10) C15 0.094(17) 0.069(13) 0.088(16) 0.015(11) 0.056(14) -0.005(13) C16 0.083(16) 0.076(13) 0.054(13) 0.012(10) 0.043(12) 0.040(12) C17 0.081(13) 0.071(11) 0.065(12) -0.006(10) 0.024(10) -0.018(9) C21 0.088(17) 0.080(14) 0.040(12) -0.009(10) -0.006(11) -0.006(12) C22 0.14(2) 0.104(15) 0.131(19) -0.038(14) 0.028(15) -0.043(15) C23 0.13(2) 0.094(16) 0.13(2) 0.010(16) 0.004(16) -0.072(15) C24 0.14(2) 0.118(18) 0.060(16) 0.014(12) -0.003(14) -0.036(17) C25 0.095(17) 0.063(12) 0.069(15) -0.025(10) 0.013(12) -0.025(12) C26 0.067(16) 0.115(18) 0.059(15) 0.039(14) -0.001(13) 0.013(13) C27 0.089(16) 0.095(14) 0.096(16) -0.032(12) 0.027(13) -0.013(11) C31 0.109(19) 0.101(17) 0.042(13) -0.014(12) 0.002(13) 0.047(14) C32 0.069(15) 0.054(12) 0.078(14) -0.010(10) 0.023(12) -0.014(10) C33 0.055(15) 0.069(14) 0.132(19) -0.033(15) -0.011(12) 0.006(12) C34 0.11(2) 0.13(2) 0.051(14) 0.003(13) 0.023(15) 0.036(16) C35 0.11(2) 0.12(2) 0.053(14) 0.014(14) 0.008(14) 0.009(15) C36 0.12(2) 0.082(15) 0.066(16) 0.017(13) 0.022(14) -0.023(15) C37 0.060(13) 0.081(12) 0.087(14) -0.025(11) -0.003(10) 0.010(12) C41 0.088(15) 0.085(14) 0.073(16) 0.026(13) 0.018(12) -0.022(11) C42 0.13(2) 0.14(2) 0.063(15) 0.013(16) 0.021(15) -0.088(16) C43 0.108(19) 0.071(13) 0.10(2) 0.018(13) 0.028(15) 0.029(12) C44 0.098(17) 0.104(15) 0.089(18) 0.018(15) 0.014(15) 0.033(12) C45 0.075(15) 0.063(12) 0.093(18) -0.011(13) -0.012(13) 0.005(11) C46 0.081(15) 0.062(13) 0.065(16) -0.016(12) -0.014(12) -0.019(12) C47 0.087(15) 0.112(14) 0.086(16) 0.034(11) 0.033(12) -0.002(12) C51 0.072(13) 0.030(9) 0.071(13) 0.019(8) 0.054(11) 0.015(9) C52 0.054(14) 0.095(14) 0.070(14) -0.006(11) -0.011(11) -0.009(10) C53 0.042(12) 0.086(12) 0.043(12) -0.012(10) -0.021(9) 0.005(11) C54 0.108(18) 0.077(13) 0.074(15) 0.001(11) -0.025(13) -0.001(13) C55 0.121(17) 0.019(9) 0.068(14) -0.009(9) 0.031(12) -0.006(10) C56 0.093(15) 0.024(9) 0.073(13) -0.010(9) 0.035(11) 0.020(10) C57 0.109(15) 0.095(13) 0.052(12) -0.002(9) 0.004(10) 0.026(12) C61 0.037(11) 0.052(10) 0.110(16) 0.005(11) 0.026(11) 0.005(8) C62 0.094(14) 0.076(12) 0.058(12) 0.015(10) 0.007(10) 0.019(10) C63 0.096(14) 0.056(10) 0.081(15) -0.019(10) 0.010(11) 0.041(10) C64 0.108(15) 0.075(11) 0.067(14) 0.034(11) 0.036(11) 0.047(10) C65 0.067(13) 0.072(11) 0.068(14) -0.014(11) 0.032(11) 0.004(10) C66 0.084(14) 0.077(13) 0.060(15) -0.009(11) 0.043(12) -0.008(11) C67 0.077(14) 0.067(10) 0.085(15) -0.001(9) 0.039(11) 0.021(10) C71 0.082(16) 0.073(13) 0.049(12) -0.007(10) -0.006(11) -0.016(11) C72 0.109(18) 0.036(10) 0.056(13) -0.002(8) 0.021(13) 0.017(11) C73 0.051(13) 0.070(12) 0.070(13) -0.022(11) -0.007(10) 0.012(11) C74 0.100(18) 0.066(12) 0.080(14) 0.002(11) 0.018(13) 0.024(11) C75 0.078(17) 0.084(15) 0.068(14) 0.027(11) 0.013(12) 0.020(13) C76 0.060(14) 0.042(11) 0.055(13) -0.019(10) 0.017(11) 0.020(10) C77 0.058(12) 0.081(11) 0.067(12) -0.009(11) 0.013(9) -0.014(9) C81 0.075(15) 0.087(15) 0.067(14) -0.018(11) 0.029(11) 0.019(11) C82 0.097(15) 0.088(12) 0.072(13) -0.017(10) 0.047(11) -0.010(12) C83 0.076(15) 0.21(2) 0.028(11) -0.036(12) 0.006(10) 0.096(14) C84 0.128(17) 0.038(9) 0.067(13) -0.031(8) -0.035(12) 0.028(11) C85 0.067(13) 0.067(12) 0.058(13) 0.017(10) -0.014(10) -0.030(10) C86 0.110(17) 0.013(8) 0.050(12) -0.001(8) -0.006(11) 0.003(10) C87 0.072(13) 0.058(10) 0.052(11) -0.014(9) 0.006(10) -0.034(9) O150 0.058(8) 0.083(7) 0.055(8) -0.015(5) 0.013(6) 0.011(6) O250 0.062(8) 0.059(6) 0.062(7) -0.012(5) 0.001(6) -0.014(6) O350 0.080(9) 0.081(7) 0.047(7) 0.002(5) -0.007(7) 0.006(6) O450 0.071(8) 0.056(6) 0.055(7) 0.009(5) -0.001(5) 0.010(5) O550 0.067(8) 0.081(7) 0.044(7) -0.008(5) -0.016(6) -0.003(6) O650 0.089(9) 0.040(5) 0.050(7) 0.013(5) 0.004(6) 0.009(5) O750 0.088(9) 0.072(7) 0.056(7) -0.012(6) 0.011(7) -0.002(6) O850 0.078(8) 0.050(6) 0.062(8) -0.003(5) 0.019(6) -0.006(6) _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 Br1 C13 1.915(14) . ? Br2 C23 1.963(19) . ? Br3 C33 1.972(19) . ? Br4 C43 1.97(2) . ? C11 C12 1.358(17) . ? C11 C16 1.422(17) . ? C11 C47 1.542(18) . ? C12 C13 1.348(17) . ? C13 C14 1.379(17) . ? C14 C15 1.322(19) . ? C15 C16 1.45(2) . ? C15 C17 1.582(19) . ? C16 O150 1.456(18) . ? C17 C21 1.459(18) . ? C21 C22 1.38(2) . ? C21 C26 1.42(2) . ? C22 C23 1.54(3) . ? C23 C24 1.26(2) . ? C24 C25 1.37(2) . ? C25 C27 1.44(2) . ? C25 C26 1.47(2) . ? C26 O250 1.388(18) . ? C27 C31 1.61(2) . ? C31 C36 1.34(2) . ? C31 C32 1.490(19) . ? C32 C33 1.38(2) . ? C33 C34 1.21(2) . ? C34 C35 1.46(2) . ? C35 C36 1.39(2) . ? C35 C37 1.39(2) . ? C36 O350 1.44(2) . ? C37 C41 1.45(2) . ? C41 C46 1.41(2) . ? C41 C42 1.56(2) . ? C42 C43 1.33(2) . ? C43 C44 1.28(2) . ? C44 C45 1.39(2) . ? C45 C46 1.37(2) . ? C45 C47 1.53(2) . ? C46 O450 1.424(17) . ? C51 C52 1.414(18) . ? C51 C87 1.517(17) . ? C51 C56 1.582(19) . ? C52 C53 1.325(18) . ? C53 C54 1.361(19) . ? C53 C500 1.54(2) . ? C54 C55 1.40(2) . ? C55 C56 1.410(18) . ? C55 C57 1.509(18) . ? C56 O550 1.394(16) . ? C57 C61 1.595(18) . ? C61 C66 1.413(18) . ? C61 C62 1.434(17) . ? C62 C63 1.358(13) . ? C63 C64 1.406(13) . ? C63 C600 1.559(13) . ? C64 C65 1.408(18) . ? C65 C66 1.395(18) . ? C65 C67 1.529(18) . ? C66 O650 1.337(17) . ? C67 C71 1.539(19) . ? C71 C76 1.369(19) . ? C71 C72 1.473(19) . ? C72 C73 1.280(17) . ? C73 C74 1.441(19) . ? C73 C700 1.50(2) . ? C74 C75 1.43(2) . ? C75 C76 1.314(19) . ? C75 C77 1.496(19) . ? C76 O750 1.448(16) . ? C77 C81 1.487(18) . ? C81 C86 1.365(18) . ? C81 C82 1.456(19) . ? C82 C83 1.405(14) . ? C83 C84 1.412(14) . ? C83 C800 1.603(15) . ? C84 C85 1.544(18) . ? C85 C86 1.437(19) . ? C85 C87 1.519(18) . ? C86 O850 1.400(16) . ? C151 C152 1.383(17) . ? C151 O150 1.476(16) . ? C152 O550 1.414(15) . ? C251 O250 1.355(16) . ? C251 C252 1.386(18) . ? C252 O650 1.441(16) . ? C351 O350 1.495(17) . ? C351 C352 1.509(18) . ? C352 O750 1.439(14) . ? C451 C452 1.41(2) . ? C451 O450 1.60(2) . ? C452 O850 1.598(18) . ? C500 C503 1.40(2) . ? C500 C502 1.41(2) . ? C500 C501 1.59(3) . ? C503 C504 1.72(3) . ? C504 C507 1.40(4) . ? C504 C505 1.54(3) . ? C504 C506 1.55(2) . ? C600 C603 1.520(14) . ? C600 C601 1.541(13) . ? C600 C602 1.544(14) . ? C602 C604 1.519(15) . ? C604 C605 1.538(17) . ? C604 C607 1.543(16) . ? C604 C606 1.603(17) . ? C700 C703 1.49(3) . ? C700 C701 1.58(2) . ? C700 C702 1.70(2) . ? C701 C704 1.53(2) . ? C704 C705 1.37(2) . ? C704 C706 1.61(2) . ? C704 C707 1.64(3) . ? C800 C802 1.448(14) . ? C800 C803 1.505(13) . ? C800 C801 1.640(16) . ? C802 C804 1.585(15) . ? C804 C807 1.521(15) . ? C804 C805 1.525(16) . ? C804 C806 1.579(15) . ? 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 C12 C11 C16 116.1(15) . . ? C12 C11 C47 121.2(15) . . ? C16 C11 C47 122.6(17) . . ? C13 C12 C11 123.5(15) . . ? C12 C13 C14 122.5(14) . . ? C12 C13 Br1 121.3(14) . . ? C14 C13 Br1 115.2(14) . . ? C15 C14 C13 116.1(15) . . ? C14 C15 C16 123.7(16) . . ? C14 C15 C17 121.6(18) . . ? C16 C15 C17 114.1(17) . . ? C11 C16 C15 117.4(17) . . ? C11 C16 O150 114.0(17) . . ? C15 C16 O150 128.5(15) . . ? C21 C17 C15 111.8(13) . . ? C22 C21 C26 119.1(18) . . ? C22 C21 C17 119(2) . . ? C26 C21 C17 121.6(18) . . ? C21 C22 C23 114.2(18) . . ? C24 C23 C22 122(2) . . ? C24 C23 Br2 127(2) . . ? C22 C23 Br2 110.6(19) . . ? C23 C24 C25 128(2) . . ? C24 C25 C27 125.3(19) . . ? C24 C25 C26 111.6(19) . . ? C27 C25 C26 122.7(17) . . ? O250 C26 C21 117(2) . . ? O250 C26 C25 118.5(19) . . ? C21 C26 C25 124.5(19) . . ? C25 C27 C31 117.3(15) . . ? C36 C31 C32 117.9(18) . . ? C36 C31 C27 127.5(18) . . ? C32 C31 C27 113(2) . . ? C33 C32 C31 114.9(15) . . ? C34 C33 C32 124(2) . . ? C34 C33 Br3 124(2) . . ? C32 C33 Br3 111.7(17) . . ? C33 C34 C35 127(2) . . ? C36 C35 C37 124(2) . . ? C36 C35 C34 112(2) . . ? C37 C35 C34 124(2) . . ? C31 C36 C35 125(2) . . ? C31 C36 O350 113.2(19) . . ? C35 C36 O350 122(2) . . ? C35 C37 C41 113.3(15) . . ? C46 C41 C37 124.3(17) . . ? C46 C41 C42 105.3(17) . . ? C37 C41 C42 130(2) . . ? C43 C42 C41 124.6(18) . . ? C44 C43 C42 123(2) . . ? C44 C43 Br4 126.2(19) . . ? C42 C43 Br4 111(2) . . ? C43 C44 C45 119(2) . . ? C46 C45 C44 121(2) . . ? C46 C45 C47 121.4(18) . . ? C44 C45 C47 118(2) . . ? C45 C46 C41 127.2(18) . . ? C45 C46 O450 118.9(19) . . ? C41 C46 O450 113.8(18) . . ? C45 C47 C11 111.5(14) . . ? C52 C51 C87 123.3(15) . . ? C52 C51 C56 120.5(13) . . ? C87 C51 C56 116.1(15) . . ? C53 C52 C51 121.1(15) . . ? C52 C53 C54 120.8(15) . . ? C52 C53 C500 118.0(18) . . ? C54 C53 C500 120.7(18) . . ? C53 C54 C55 123.6(15) . . ? C54 C55 C56 122.5(15) . . ? C54 C55 C57 121.4(16) . . ? C56 C55 C57 116.2(17) . . ? O550 C56 C55 124.8(15) . . ? O550 C56 C51 124.0(14) . . ? C55 C56 C51 111.1(15) . . ? C55 C57 C61 112.3(12) . . ? C66 C61 C62 120.2(14) . . ? C66 C61 C57 120.9(14) . . ? C62 C61 C57 118.8(15) . . ? C63 C62 C61 124.4(14) . . ? C62 C63 C64 113.7(12) . . ? C62 C63 C600 124.8(13) . . ? C64 C63 C600 121.2(12) . . ? C63 C64 C65 124.4(13) . . ? C66 C65 C64 120.5(16) . . ? C66 C65 C67 114.5(15) . . ? C64 C65 C67 124.6(15) . . ? O650 C66 C65 124.4(16) . . ? O650 C66 C61 118.9(15) . . ? C65 C66 C61 116.3(16) . . ? C65 C67 C71 117.2(13) . . ? C76 C71 C72 114.9(15) . . ? C76 C71 C67 125.7(17) . . ? C72 C71 C67 119.3(17) . . ? C73 C72 C71 121.7(15) . . ? C72 C73 C74 121.5(16) . . ? C72 C73 C700 116.5(19) . . ? C74 C73 C700 122.0(19) . . ? C75 C74 C73 116.8(16) . . ? C76 C75 C74 119.1(16) . . ? C76 C75 C77 124.4(19) . . ? C74 C75 C77 116.5(18) . . ? C75 C76 C71 124.6(17) . . ? C75 C76 O750 117.9(17) . . ? C71 C76 O750 116.5(17) . . ? C81 C77 C75 112.5(13) . . ? C86 C81 C82 114.9(15) . . ? C86 C81 C77 118.4(16) . . ? C82 C81 C77 125.9(16) . . ? C83 C82 C81 128.5(14) . . ? C82 C83 C84 110.4(13) . . ? C82 C83 C800 142.2(15) . . ? C84 C83 C800 107.0(11) . . ? C83 C84 C85 128.6(13) . . ? C86 C85 C87 128.8(14) . . ? C86 C85 C84 109.4(15) . . ? C87 C85 C84 121.9(15) . . ? C81 C86 O850 123.3(15) . . ? C81 C86 C85 127.9(16) . . ? O850 C86 C85 108.1(16) . . ? C51 C87 C85 112.4(12) . . ? C152 C151 O150 111.9(14) . . ? C151 C152 O550 113.4(13) . . ? O250 C251 C252 117.5(15) . . ? C251 C252 O650 116.7(15) . . ? O350 C351 C352 109.3(14) . . ? O750 C352 C351 111.5(13) . . ? C452 C451 O450 95.0(15) . . ? C451 C452 O850 102.0(15) . . ? C503 C500 C502 126(2) . . ? C503 C500 C53 114.8(18) . . ? C502 C500 C53 114.6(19) . . ? C503 C500 C501 92.7(17) . . ? C502 C500 C501 94.1(18) . . ? C53 C500 C501 105.5(16) . . ? C500 C503 C504 122(2) . . ? C507 C504 C505 112(3) . . ? C507 C504 C506 111(3) . . ? C505 C504 C506 116(2) . . ? C507 C504 C503 103(2) . . ? C505 C504 C503 116(2) . . ? C506 C504 C503 96.6(18) . . ? C603 C600 C601 108.8(11) . . ? C603 C600 C602 113.2(12) . . ? C601 C600 C602 106.2(11) . . ? C603 C600 C63 112.0(12) . . ? C601 C600 C63 108.6(11) . . ? C602 C600 C63 107.8(11) . . ? C604 C602 C600 111.7(11) . . ? C602 C604 C605 111.8(14) . . ? C602 C604 C607 111.6(14) . . ? C605 C604 C607 112.7(13) . . ? C602 C604 C606 110.4(13) . . ? C605 C604 C606 105.3(14) . . ? C607 C604 C606 104.7(14) . . ? C703 C700 C73 115.4(19) . . ? C703 C700 C701 113.2(19) . . ? C73 C700 C701 114.0(16) . . ? C703 C700 C702 95.0(17) . . ? C73 C700 C702 111.7(16) . . ? C701 C700 C702 105.5(15) . . ? C704 C701 C700 123.5(16) . . ? C705 C704 C701 108(2) . . ? C705 C704 C706 115.3(19) . . ? C701 C704 C706 99.9(16) . . ? C705 C704 C707 127(2) . . ? C701 C704 C707 112.2(18) . . ? C706 C704 C707 90.3(16) . . ? C802 C800 C803 127.3(14) . . ? C802 C800 C83 109.1(12) . . ? C803 C800 C83 106.8(11) . . ? C802 C800 C801 104.8(12) . . ? C803 C800 C801 101.9(11) . . ? C83 C800 C801 104.5(12) . . ? C800 C802 C804 114.5(11) . . ? C807 C804 C805 109.8(13) . . ? C807 C804 C806 111.5(13) . . ? C805 C804 C806 106.2(13) . . ? C807 C804 C802 111.5(12) . . ? C805 C804 C802 116.2(13) . . ? C806 C804 C802 101.3(12) . . ? C16 O150 C151 117.6(11) . . ? C251 O250 C26 113.6(12) . . ? C36 O350 C351 118.4(12) . . ? C46 O450 C451 114.4(11) . . ? C56 O550 C152 115.8(11) . . ? C66 O650 C252 119.9(11) . . ? C352 O750 C76 115.1(10) . . ? C86 O850 C452 117.0(10) . . ? _refine_diff_density_max 0.839 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.105