# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jerry L. Atwood' _publ_contact_author_email ATWOODJ@MISSOURI.EDU _publ_section_title ; Instantaneous formation of metal-organic nano-capsules gives new insight into the self-assembly process ; loop_ _publ_author_name 'Jerry L Atwood' 'Scott Dalgarno' 'Nicholas P Power' 'John E Warren' # Attachment '1.cif' data_C3Cu _database_code_depnum_ccdc_archive 'CCDC 648029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H148.50 Cu12 O50.25' _chemical_formula_weight 3157.37 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 36.361(5) _cell_length_b 32.987(5) _cell_length_c 24.640(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.526(4) _cell_angle_gamma 90.00 _cell_volume 29526(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12948 _exptl_absorpt_coefficient_mu 1.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8158 _exptl_absorpt_correction_T_max 0.8715 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 SMART 1000 CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93490 _diffrn_reflns_av_R_equivalents 0.6463 _diffrn_reflns_av_sigmaI/netI 0.9735 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 27.25 _reflns_number_total 32600 _reflns_number_gt 5722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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. Crystals were very weakly diffracting.The reported and calculated formulae differ due to the missing hydrogen atoms of waters of crystallization and the inability to assign the hydrogen atoms of the remaining upper rim hydroxyl groups. The poor quality of the data meant that all atoms except for Cu were refined isotropically, and resulted in a lack of convergence during refinement. A number of the C-propyl chains of the pyrogallol[4]arenes were disordered over two positions and were modelled at partial occupancy. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _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 32600 _refine_ls_number_parameters 881 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.5401 _refine_ls_R_factor_gt 0.2012 _refine_ls_wR_factor_ref 0.4522 _refine_ls_wR_factor_gt 0.3325 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max '1.531 (H-Tors)' _refine_ls_shift/su_mean 0.018 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 Cu1 Cu 0.13575(9) 0.77148(11) 0.23225(16) 0.0490(12) Uani 1 1 d . . . O1 O 0.2329(5) 0.6026(5) 0.2575(7) 0.043(5) Uiso 1 1 d . . . C1 C 0.2690(8) 0.6338(8) 0.3275(12) 0.045(8) Uiso 1 1 d . . . Cu2 Cu 0.07604(10) 0.71618(12) 0.13256(18) 0.0614(13) Uani 1 1 d . . . O2 O 0.2908(5) 0.5976(6) 0.1972(8) 0.055(6) Uiso 1 1 d . . . C2 C 0.2674(7) 0.6175(8) 0.2790(11) 0.033(7) Uiso 1 1 d . . . Cu3 Cu 0.14574(9) 0.66097(11) 0.21742(17) 0.0527(12) Uani 1 1 d . . . O3 O 0.3576(5) 0.6239(5) 0.2252(7) 0.046(6) Uiso 1 1 d . . . C3 C 0.2970(7) 0.6148(7) 0.2435(11) 0.027(7) Uiso 1 1 d . . . Cu4 Cu 0.24009(9) 0.57800(11) 0.18562(17) 0.0518(12) Uani 1 1 d . . . O4 O 0.4009(5) 0.6797(5) 0.2224(7) 0.038(5) Uiso 1 1 d . . . C4 C 0.3318(7) 0.6304(7) 0.2615(11) 0.028(7) Uiso 1 1 d . . . Cu5 Cu 0.28112(9) 0.53797(11) 0.06262(18) 0.0549(12) Uani 1 1 d . . . O5 O 0.4066(5) 0.7568(5) 0.1866(7) 0.040(5) Uiso 1 1 d . . . C5 C 0.3361(7) 0.6431(7) 0.3136(10) 0.023(7) Uiso 1 1 d . . . Cu6 Cu 0.33921(10) 0.59362(11) 0.16302(19) 0.0631(14) Uani 1 1 d . . . O6 O 0.3879(4) 0.8208(5) 0.2450(7) 0.031(5) Uiso 1 1 d . . . C6 C 0.3066(8) 0.6465(8) 0.3512(12) 0.047(9) Uiso 1 1 d . . . H6 H 0.3105 0.6558 0.3874 0.056 Uiso 1 1 calc R . . Cu7 Cu 0.25706(10) 0.55144(12) -0.11955(18) 0.0644(14) Uani 1 1 d . . . O7 O 0.3378(5) 0.8643(5) 0.2639(7) 0.041(5) Uiso 1 1 d . . . C7 C 0.3754(7) 0.6591(8) 0.3315(11) 0.035(7) Uiso 1 1 d . . . H7 H 0.3938 0.6424 0.3125 0.042 Uiso 1 1 calc R . . Cu8 Cu 0.18786(10) 0.60370(13) -0.20768(19) 0.0714(16) Uani 1 1 d . . . O8 O 0.2668(5) 0.8744(5) 0.2341(8) 0.051(6) Uiso 1 1 d . . . C8 C 0.3785(7) 0.7024(8) 0.3110(11) 0.036(8) Uiso 1 1 d . . . Cu9 Cu 0.28702(10) 0.62045(12) -0.22637(18) 0.0647(14) Uani 1 1 d . . . O9 O 0.2116(6) 0.8421(6) 0.2872(8) 0.063(6) Uiso 1 1 d . . . C9 C 0.3920(8) 0.7087(9) 0.2582(13) 0.049(9) Uiso 1 1 d . . . Cu10 Cu 0.41814(10) 0.70314(10) 0.15556(16) 0.0466(11) Uani 1 1 d . . . O10 O 0.1692(5) 0.7880(5) 0.2952(7) 0.047(5) Uiso 1 1 d . . . C10 C 0.3960(8) 0.7467(9) 0.2379(12) 0.047(9) Uiso 1 1 d . . . Cu11 Cu 0.44872(10) 0.77192(11) 0.04924(16) 0.0499(12) Uani 1 1 d . . . O11 O 0.1517(5) 0.7154(6) 0.2464(8) 0.053(6) Uiso 1 1 d . . . C11 C 0.3837(7) 0.7811(8) 0.2694(11) 0.036(8) Uiso 1 1 d . . . Cu12 Cu 0.40714(9) 0.81289(10) 0.17214(15) 0.0418(11) Uani 1 1 d . . . O12 O 0.1813(5) 0.6459(6) 0.2760(8) 0.048(6) Uiso 1 1 d . . . C12 C 0.3714(7) 0.7774(8) 0.3238(11) 0.029(7) Uiso 1 1 d . . . O13 O 0.2424(4) 0.5107(5) 0.0238(7) 0.030(5) Uiso 1 1 d . . . C13 C 0.3711(7) 0.7377(7) 0.3406(11) 0.031(7) Uiso 1 1 d . . . H13 H 0.3650 0.7335 0.3773 0.037 Uiso 1 1 calc R . . O14 O 0.2449(5) 0.5493(5) 0.1165(8) 0.048(6) Uiso 1 1 d . . . C14 C 0.3597(7) 0.8115(8) 0.3540(11) 0.038(8) Uiso 1 1 d . . . H14 H 0.3736 0.8350 0.3396 0.046 Uiso 1 1 calc R . . O15 O 0.1898(5) 0.5593(5) 0.1828(8) 0.048(6) Uiso 1 1 d . . . C15 C 0.3203(7) 0.8209(8) 0.3409(11) 0.034(7) Uiso 1 1 d . . . O16 O 0.1388(5) 0.6049(5) 0.1992(7) 0.042(5) Uiso 1 1 d . . . C16 C 0.3107(8) 0.8431(9) 0.2970(12) 0.045(8) Uiso 1 1 d . . . O17 O 0.1057(5) 0.6717(5) 0.1653(7) 0.037(5) Uiso 1 1 d . . . C17 C 0.2742(9) 0.8535(9) 0.2861(13) 0.055(9) Uiso 1 1 d . . . O18 O 0.0505(5) 0.6734(5) 0.0869(7) 0.045(5) Uiso 1 1 d . . . C18 C 0.2469(10) 0.8344(10) 0.3123(14) 0.067(10) Uiso 1 1 d . . . O19 O 0.0373(5) 0.6796(6) -0.0081(8) 0.059(6) Uiso 1 1 d . . . C19 C 0.2541(8) 0.8110(8) 0.3555(12) 0.040(8) Uiso 1 1 d . . . O20 O 0.0691(5) 0.6900(6) -0.1027(7) 0.048(6) Uiso 1 1 d . . . C20 C 0.2893(7) 0.8042(7) 0.3712(10) 0.029(7) Uiso 1 1 d . . . H20 H 0.2946 0.7882 0.4027 0.035 Uiso 1 1 calc R . . O21 O 0.0890(5) 0.6277(5) -0.1646(7) 0.040(5) Uiso 1 1 d . . . C21 C 0.2221(8) 0.7916(8) 0.3832(11) 0.039(8) Uiso 1 1 d . . . H21 H 0.2008 0.8106 0.3771 0.047 Uiso 1 1 calc R . . O22 O 0.1401(4) 0.5854(5) -0.1857(7) 0.031(5) Uiso 1 1 d . . . C22 C 0.2100(8) 0.7535(9) 0.3620(12) 0.048(9) Uiso 1 1 d . . . O23 O 0.2096(4) 0.5702(5) -0.1507(7) 0.032(5) Uiso 1 1 d . . . C23 C 0.1865(8) 0.7506(9) 0.3164(12) 0.040(8) Uiso 1 1 d . . . O24 O 0.2299(5) 0.5150(5) -0.0733(7) 0.036(5) Uiso 1 1 d . . . C24 C 0.1765(8) 0.7185(9) 0.2944(12) 0.046(8) Uiso 1 1 d . . . O25 O 0.3903(5) 0.5907(6) 0.1389(8) 0.050(6) Uiso 1 1 d . . . C25 C 0.1922(9) 0.6776(10) 0.3048(14) 0.064(10) Uiso 1 1 d . . . O26 O 0.3226(5) 0.5618(5) 0.0988(7) 0.046(5) Uiso 1 1 d . . . C26 C 0.2174(6) 0.6808(7) 0.3504(10) 0.020(6) Uiso 1 1 d . . . O27 O 0.3132(5) 0.5200(5) 0.0074(7) 0.040(5) Uiso 1 1 d . . . C27 C 0.2257(8) 0.7157(8) 0.3755(11) 0.042(8) Uiso 1 1 d . . . H27 H 0.2436 0.7148 0.4047 0.051 Uiso 1 1 calc R . . O28 O 0.3019(5) 0.5279(6) -0.0882(8) 0.054(6) Uiso 1 1 d . . . C28 C 0.2382(7) 0.6393(8) 0.3651(11) 0.033(7) Uiso 1 1 d . . . H28 H 0.2202 0.6171 0.3563 0.039 Uiso 1 1 calc R . . O29 O 0.2876(5) 0.5817(5) -0.1666(8) 0.052(6) Uiso 1 1 d . . . C29 C 0.3843(8) 0.6559(9) 0.3918(12) 0.054(9) Uiso 1 1 d . . . H29A H 0.3819 0.6271 0.4025 0.065 Uiso 1 1 calc R . . H29B H 0.3656 0.6714 0.4111 0.065 Uiso 1 1 calc R . . O30 O 0.3388(5) 0.6163(5) -0.2253(8) 0.048(6) Uiso 1 1 d . . . C30 C 0.4260(9) 0.6721(10) 0.4137(14) 0.081(12) Uiso 1 1 d . . . H30A H 0.4277 0.7020 0.4113 0.097 Uiso 1 1 calc R . . H30B H 0.4315 0.6637 0.4517 0.097 Uiso 1 1 calc R . . O31 O 0.3820(5) 0.6723(5) -0.2286(7) 0.039(5) Uiso 1 1 d . . . C31 C 0.4523(11) 0.6516(11) 0.3750(16) 0.113(15) Uiso 1 1 d . . . H31A H 0.4476 0.6223 0.3742 0.169 Uiso 1 1 calc R . . H31B H 0.4778 0.6566 0.3878 0.169 Uiso 1 1 calc R . . H31C H 0.4483 0.6628 0.3384 0.169 Uiso 1 1 calc R . . O32 O 0.0976(5) 0.7600(5) 0.1750(7) 0.043(5) Uiso 1 1 d . . . C32 C 0.3707(8) 0.8097(9) 0.4150(12) 0.052(9) Uiso 1 1 d . . . H32A H 0.3567 0.7875 0.4317 0.062 Uiso 1 1 calc R . . H32B H 0.3631 0.8354 0.4320 0.062 Uiso 1 1 calc R . . O33 O 0.4568(4) 0.7434(5) -0.1027(7) 0.029(5) Uiso 1 1 d . . . C33 C 0.4123(9) 0.8030(10) 0.4288(14) 0.074(11) Uiso 1 1 d . . . H33A H 0.4222 0.7837 0.4024 0.088 Uiso 1 1 calc R . . H33B H 0.4255 0.8291 0.4249 0.088 Uiso 1 1 calc R . . O34 O 0.4696(5) 0.7372(6) -0.0034(8) 0.053(6) Uiso 1 1 d . . . C34 C 0.4198(13) 0.7872(14) 0.4846(19) 0.16(2) Uiso 1 1 d . . . H34A H 0.4192 0.8096 0.5106 0.241 Uiso 1 1 calc R . . H34B H 0.4442 0.7744 0.4868 0.241 Uiso 1 1 calc R . . H34C H 0.4011 0.7671 0.4930 0.241 Uiso 1 1 calc R . . O35 O 0.4367(5) 0.7237(5) 0.0872(7) 0.048(6) Uiso 1 1 d . . . C35 C 0.2293(6) 0.7894(7) 0.4462(9) 0.026(7) Uiso 1 1 d . . . H35A H 0.2505 0.7714 0.4546 0.031 Uiso 1 1 calc R . . H35B H 0.2356 0.8168 0.4602 0.031 Uiso 1 1 calc R . . O36 O 0.4292(5) 0.6486(5) 0.1309(8) 0.044(5) Uiso 1 1 d . . . C36 C 0.1953(8) 0.7735(9) 0.4748(12) 0.057(9) Uiso 1 1 d . . . H36A H 0.2015 0.7708 0.5142 0.068 Uiso 1 1 calc R . . H36B H 0.1888 0.7463 0.4605 0.068 Uiso 1 1 calc R . . C37 C 0.1607(9) 0.8032(9) 0.4660(13) 0.077(11) Uiso 1 1 d . . . H37A H 0.1680 0.8309 0.4760 0.116 Uiso 1 1 calc R . . H37B H 0.1409 0.7944 0.4888 0.116 Uiso 1 1 calc R . . H37C H 0.1521 0.8026 0.4277 0.116 Uiso 1 1 calc R . . C38 C 0.2475(7) 0.6360(8) 0.4246(11) 0.040(8) Uiso 1 1 d . . . H38A H 0.2249 0.6410 0.4447 0.048 Uiso 1 1 calc R . . H38B H 0.2655 0.6575 0.4351 0.048 Uiso 1 1 calc R . . C39 C 0.2640(8) 0.5940(8) 0.4424(11) 0.046(8) Uiso 1 1 d . . . H39A H 0.2477 0.5726 0.4265 0.055 Uiso 1 1 calc R . . H39B H 0.2881 0.5911 0.4258 0.055 Uiso 1 1 calc R . . C40 C 0.2696(9) 0.5852(10) 0.5041(13) 0.075(11) Uiso 1 1 d . . . H40A H 0.2802 0.6092 0.5224 0.113 Uiso 1 1 calc R . . H40B H 0.2864 0.5622 0.5095 0.113 Uiso 1 1 calc R . . H40C H 0.2459 0.5788 0.5193 0.113 Uiso 1 1 calc R . . C41 C 0.1757(7) 0.4896(8) 0.0360(11) 0.034(7) Uiso 1 1 d . . . C42 C 0.2105(8) 0.5088(8) 0.0538(12) 0.040(8) Uiso 1 1 d . . . C43 C 0.2090(8) 0.5300(9) 0.0962(12) 0.045(8) Uiso 1 1 d . . . C44 C 0.1817(7) 0.5380(8) 0.1359(12) 0.037(8) Uiso 1 1 d . . . C45 C 0.1480(7) 0.5180(7) 0.1189(10) 0.028(7) Uiso 1 1 d . . . C46 C 0.1481(8) 0.4949(8) 0.0710(11) 0.040(8) Uiso 1 1 d . . . H46 H 0.1258 0.4810 0.0617 0.049 Uiso 1 1 calc R . . C47 C 0.1161(7) 0.5232(8) 0.1554(11) 0.037(8) Uiso 1 1 d . . . H47 H 0.1265 0.5275 0.1933 0.045 Uiso 1 1 calc R . . C48 C 0.0975(8) 0.5617(8) 0.1375(12) 0.042(8) Uiso 1 1 d . . . C49 C 0.1117(7) 0.5991(8) 0.1607(11) 0.037(8) Uiso 1 1 d . . . C50 C 0.0939(8) 0.6370(9) 0.1447(12) 0.042(8) Uiso 1 1 d . . . C51 C 0.0638(9) 0.6351(10) 0.1005(14) 0.066(10) Uiso 1 1 d . . . C52 C 0.0518(7) 0.5996(8) 0.0789(11) 0.033(7) Uiso 1 1 d . . . C53 C 0.0686(7) 0.5637(7) 0.1001(10) 0.027(7) Uiso 1 1 d . . . H53 H 0.0589 0.5386 0.0870 0.033 Uiso 1 1 calc R . . C54 C 0.0220(6) 0.6006(7) 0.0372(10) 0.022(6) Uiso 1 1 d . . . H54 H 0.0073 0.6255 0.0439 0.027 Uiso 1 1 calc R . . C55 C 0.0378(6) 0.6053(7) -0.0178(9) 0.017(6) Uiso 1 1 d . . . C56 C 0.0457(8) 0.6457(9) -0.0356(12) 0.047(9) Uiso 1 1 d . . . C57 C 0.0624(7) 0.6497(8) -0.0872(11) 0.030(7) Uiso 1 1 d . . . C58 C 0.0726(6) 0.6187(7) -0.1189(10) 0.021(6) Uiso 1 1 d . . . C59 C 0.0627(6) 0.5797(7) -0.1040(10) 0.023(6) Uiso 1 1 d . . . C60 C 0.0489(6) 0.5743(7) -0.0537(9) 0.018(6) Uiso 1 1 d . . . H60 H 0.0465 0.5471 -0.0416 0.022 Uiso 1 1 calc R . . C61 C 0.0778(6) 0.5455(7) -0.1342(10) 0.024(7) Uiso 1 1 d . . . H61 H 0.0770 0.5549 -0.1728 0.028 Uiso 1 1 calc R . . C62 C 0.1175(7) 0.5371(8) -0.1212(11) 0.034(7) Uiso 1 1 d . . . C63 C 0.1448(8) 0.5580(8) -0.1458(11) 0.038(8) Uiso 1 1 d . . . C64 C 0.1821(8) 0.5462(8) -0.1282(11) 0.038(8) Uiso 1 1 d . . . C65 C 0.1923(8) 0.5206(9) -0.0855(12) 0.046(8) Uiso 1 1 d . . . C66 C 0.1655(8) 0.5000(8) -0.0589(12) 0.042(8) Uiso 1 1 d . . . C67 C 0.1272(7) 0.5069(7) -0.0781(10) 0.024(7) Uiso 1 1 d . . . H67 H 0.1082 0.4916 -0.0627 0.029 Uiso 1 1 calc R . . C68 C 0.1747(6) 0.4683(6) -0.0176(9) 0.014(6) Uiso 1 1 d . . . H68 H 0.2002 0.4583 -0.0239 0.017 Uiso 1 1 calc R . . C69 C 0.0884(6) 0.4891(7) 0.1573(10) 0.025(7) Uiso 1 1 d . . . H69A H 0.0791 0.4825 0.1199 0.030 Uiso 1 1 calc R . . H69B H 0.0672 0.4977 0.1785 0.030 Uiso 1 1 calc R . . C70 C 0.1068(7) 0.4510(8) 0.1839(11) 0.042(8) Uiso 1 1 d . . . H70A H 0.1180 0.4583 0.2200 0.051 Uiso 1 1 calc R . . H70B H 0.1266 0.4412 0.1610 0.051 Uiso 1 1 calc R . . C71 C 0.0766(8) 0.4150(9) 0.1910(12) 0.061(10) Uiso 1 1 d . . . H71A H 0.0559 0.4255 0.2110 0.091 Uiso 1 1 calc R . . H71B H 0.0881 0.3924 0.2111 0.091 Uiso 1 1 calc R . . H71C H 0.0676 0.4056 0.1551 0.091 Uiso 1 1 calc R . . C72 C -0.0060(7) 0.5633(8) 0.0369(11) 0.045(8) Uiso 1 1 d . . . H72A H -0.0193 0.5639 0.0711 0.054 Uiso 1 1 calc R . . H72B H 0.0084 0.5378 0.0366 0.054 Uiso 1 1 calc R . . C73 C -0.0376(10) 0.5622(11) -0.0160(15) 0.091(13) Uiso 1 1 d . . . H73A H -0.0253 0.5574 -0.0504 0.109 Uiso 1 1 calc R . . H73B H -0.0555 0.5400 -0.0109 0.109 Uiso 1 1 calc R . . C74 C -0.0538(14) 0.5957(15) -0.017(2) 0.17(2) Uiso 1 1 d . . . H74A H -0.0566 0.6055 0.0196 0.255 Uiso 1 1 calc R . . H74B H -0.0781 0.5925 -0.0358 0.255 Uiso 1 1 calc R . . H74C H -0.0393 0.6152 -0.0375 0.255 Uiso 1 1 calc R . . C75 C 0.0534(8) 0.5071(8) -0.1352(12) 0.048(9) Uiso 1 1 d . A . C76 C 0.0183(11) 0.5179(12) -0.1545(17) 0.006(10) Uiso 0.50 1 d P . . H76A H 0.0105 0.5417 -0.1334 0.007 Uiso 0.50 1 calc PR A . H76B H 0.0015 0.4954 -0.1461 0.007 Uiso 0.50 1 calc PR . . C77 C 0.012(3) 0.528(3) -0.214(3) 0.17(4) Uiso 0.50 1 d P A -1 H77A H 0.0096 0.5574 -0.2180 0.252 Uiso 0.50 1 calc PR . . H77B H -0.0102 0.5145 -0.2280 0.252 Uiso 0.50 1 calc PR . . H77C H 0.0333 0.5185 -0.2337 0.252 Uiso 0.50 1 calc PR . . C78 C 0.0597(15) 0.4735(16) -0.185(2) 0.043(17) Uiso 0.50 1 d P . . H78A H 0.0562 0.4880 -0.2196 0.052 Uiso 0.50 1 calc PR A . H78B H 0.0859 0.4650 -0.1817 0.052 Uiso 0.50 1 calc PR . . C79 C 0.0372(15) 0.4358(16) -0.189(2) 0.053(18) Uiso 0.50 1 d P A . H79A H 0.0490 0.4144 -0.1665 0.080 Uiso 0.50 1 calc PR . . H79B H 0.0350 0.4269 -0.2267 0.080 Uiso 0.50 1 calc PR . . H79C H 0.0126 0.4412 -0.1757 0.080 Uiso 0.50 1 calc PR . . C80 C 0.1492(8) 0.4308(8) -0.0146(12) 0.052(9) Uiso 1 1 d . . . H80A H 0.1564 0.4137 0.0171 0.063 Uiso 1 1 calc R . . H80B H 0.1233 0.4393 -0.0115 0.063 Uiso 1 1 calc R . . C81 C 0.1537(8) 0.4085(8) -0.0652(11) 0.040(8) Uiso 1 1 d . . . H81A H 0.1802 0.4085 -0.0726 0.047 Uiso 1 1 calc R . . H81B H 0.1408 0.4239 -0.0948 0.047 Uiso 1 1 calc R . . C82 C 0.1402(10) 0.3645(11) -0.0688(15) 0.099(14) Uiso 1 1 d . . . H82A H 0.1551 0.3476 -0.0436 0.149 Uiso 1 1 calc R . . H82B H 0.1425 0.3545 -0.1060 0.149 Uiso 1 1 calc R . . H82C H 0.1143 0.3633 -0.0593 0.149 Uiso 1 1 calc R . . C83 C 0.4180(8) 0.5597(9) 0.0615(12) 0.047(9) Uiso 1 1 d . . . C84 C 0.3888(8) 0.5702(8) 0.0944(12) 0.044(8) Uiso 1 1 d . . . C85 C 0.3548(8) 0.5517(8) 0.0698(12) 0.043(8) Uiso 1 1 d . . . C86 C 0.3488(8) 0.5321(9) 0.0243(13) 0.050(9) Uiso 1 1 d . . . C87 C 0.3816(7) 0.5183(7) -0.0062(10) 0.027(7) Uiso 1 1 d . . . C88 C 0.4129(6) 0.5381(7) 0.0159(10) 0.020(6) Uiso 1 1 d . . . H88 H 0.4341 0.5358 -0.0051 0.024 Uiso 1 1 calc R . . C89 C 0.3754(6) 0.4990(7) -0.0568(9) 0.019(6) Uiso 1 1 d . . . H89 H 0.3526 0.4824 -0.0528 0.023 Uiso 1 1 calc R . . C90 C 0.3675(8) 0.5248(9) -0.1063(12) 0.051(9) Uiso 1 1 d . . . C91 C 0.3326(9) 0.5414(9) -0.1161(13) 0.054(9) Uiso 1 1 d . . . C92 C 0.3248(8) 0.5700(9) -0.1550(12) 0.048(9) Uiso 1 1 d . . . C93 C 0.3529(8) 0.5886(9) -0.1849(12) 0.045(8) Uiso 1 1 d . . . C94 C 0.3884(8) 0.5742(9) -0.1788(12) 0.048(9) Uiso 1 1 d . . . C95 C 0.3957(9) 0.5457(9) -0.1369(12) 0.058(10) Uiso 1 1 d . . . H95 H 0.4208 0.5396 -0.1279 0.070 Uiso 1 1 calc R . . C96 C 0.4199(8) 0.5930(8) -0.2088(12) 0.048(9) Uiso 1 1 d . . . H96 H 0.4084 0.6013 -0.2447 0.057 Uiso 1 1 calc R . . C97 C 0.4301(8) 0.6335(9) -0.1805(13) 0.055(9) Uiso 1 1 d . . . C98 C 0.4112(7) 0.6698(7) -0.1911(10) 0.024(7) Uiso 1 1 d . . . C99 C 0.4209(8) 0.7038(8) -0.1662(11) 0.040(8) Uiso 1 1 d . . . O100 O 0.3588(12) 0.5286(13) -0.3587(18) 0.076(14) Uiso 0.50 1 d P . . C100 C 0.4506(7) 0.7076(8) -0.1250(11) 0.032(7) Uiso 1 1 d . . . O101 O 0.304(2) 0.525(3) -0.371(3) 0.06(3) Uiso 0.25 1 d P . 1 C101 C 0.4705(8) 0.6732(9) -0.1157(12) 0.045(8) Uiso 1 1 d . . . C102 C 0.4601(7) 0.6378(8) -0.1401(11) 0.034(7) Uiso 1 1 d . . . H102 H 0.4735 0.6140 -0.1300 0.041 Uiso 1 1 calc R . . O103 O 0.3138(14) 0.4598(16) -0.176(2) 0.111(19) Uiso 0.50 1 d P . . C103 C 0.4989(8) 0.6702(9) -0.0682(12) 0.048(9) Uiso 1 1 d . . . H103 H 0.5093 0.6983 -0.0671 0.057 Uiso 1 1 calc R . . O104 O 0.2556(11) 0.4868(12) -0.2062(17) 0.069(13) Uiso 0.50 1 d P B 1 C104 C 0.4841(7) 0.6669(8) -0.0145(11) 0.029(7) Uiso 1 1 d . . . C105 C 0.4693(7) 0.6962(8) 0.0113(11) 0.034(7) Uiso 1 1 d . . . O106 O 0.2093(12) 0.5762(12) -0.3660(17) 0.073(14) Uiso 0.50 1 d P . . C106 C 0.4521(7) 0.6919(7) 0.0588(11) 0.028(7) Uiso 1 1 d . . . O107 O 0.1994(7) 0.5382(8) -0.2762(10) 0.106(9) Uiso 1 1 d . . . C107 C 0.4456(7) 0.6506(8) 0.0839(11) 0.037(8) Uiso 1 1 d . . . O108 O 0.1625(11) 0.4645(12) -0.2046(17) 0.065(13) Uiso 0.50 1 d P C 1 C108 C 0.4633(7) 0.6192(8) 0.0517(12) 0.040(8) Uiso 1 1 d . . . O109 O 0.1118(18) 0.4225(19) -0.204(3) 0.15(2) Uiso 0.50 1 d P . . C109 C 0.4811(7) 0.6266(8) 0.0069(11) 0.039(8) Uiso 1 1 d . . . H109 H 0.4921 0.6047 -0.0115 0.047 Uiso 1 1 calc R . . O110 O 0.5000 0.739(3) -0.2500 0.17(4) Uiso 0.50 2 d SP . . C110 C 0.4555(7) 0.5773(8) 0.0787(12) 0.045(8) Uiso 1 1 d . . . H110 H 0.4556 0.5817 0.1189 0.054 Uiso 1 1 calc R . . O111 O 0.3820(12) 0.6379(13) -0.0451(18) 0.082(15) Uiso 0.50 1 d P . . O112 O 0.2702(16) 0.6023(18) 0.007(3) 0.021(17) Uiso 0.25 1 d P D 1 O113 O 0.262(2) 0.613(3) -0.033(4) 0.08(3) Uiso 0.25 1 d P E 2 O114 O 0.1437(11) 0.6008(11) 0.0052(16) 0.059(12) Uiso 0.50 1 d P . . C114 C 0.4489(8) 0.5659(8) -0.2223(12) 0.045(8) Uiso 1 1 d . . . H11A H 0.4626 0.5580 -0.1883 0.054 Uiso 1 1 calc R . . H11B H 0.4662 0.5808 -0.2450 0.054 Uiso 1 1 calc R . . O115 O 0.002(3) 0.688(2) -0.222(3) 0.21(4) Uiso 0.50 1 d P . . C115 C 0.4373(10) 0.5288(10) -0.2512(14) 0.083(12) Uiso 1 1 d . . . H11C H 0.4229 0.5123 -0.2260 0.099 Uiso 1 1 calc R . . H11D H 0.4597 0.5132 -0.2587 0.099 Uiso 1 1 calc R . . O116 O 0.3839(19) 0.772(2) -0.020(3) 0.04(2) Uiso 0.25 1 d P . . C116 C 0.4137(13) 0.5325(14) -0.3064(18) 0.150(19) Uiso 1 1 d . . . H11E H 0.3934 0.5517 -0.3019 0.225 Uiso 1 1 calc R . . H11F H 0.4036 0.5058 -0.3166 0.225 Uiso 1 1 calc R . . H11G H 0.4293 0.5422 -0.3351 0.225 Uiso 1 1 calc R . . O117 O 0.3506(15) 0.5293(16) 0.228(2) 0.12(2) Uiso 0.50 1 d P . . C117 C 0.5346(7) 0.6440(8) -0.0781(11) 0.039(8) Uiso 1 1 d . F . H11H H 0.5530 0.6497 -0.0483 0.046 Uiso 1 1 calc R . . H11I H 0.5279 0.6150 -0.0756 0.046 Uiso 1 1 calc R . . O118 O 0.3389(16) 0.6877(18) 0.111(2) 0.13(2) Uiso 0.50 1 d P . . C118 C 0.5532(12) 0.6511(12) -0.1336(17) 0.099(14) Uiso 1 1 d . . . O119 O 0.2500 0.7500 0.0000 0.17(4) Uiso 0.50 2 d SP . . C119 C 0.5904(17) 0.6316(19) -0.131(3) 0.07(2) Uiso 0.50 1 d P F 1 H11J H 0.5965 0.6229 -0.1679 0.107 Uiso 0.50 1 calc PR F 1 H11K H 0.5902 0.6079 -0.1073 0.107 Uiso 0.50 1 calc PR F 1 H11L H 0.6088 0.6511 -0.1175 0.107 Uiso 0.50 1 calc PR F 1 O120 O 0.544(2) 0.591(2) 0.245(3) 0.18(3) Uiso 0.50 1 d P . . C120 C 0.5690(18) 0.684(2) -0.131(3) 0.08(2) Uiso 0.50 1 d P F 2 H12A H 0.5822 0.6862 -0.0953 0.113 Uiso 0.50 1 calc PR F 2 H12B H 0.5510 0.7058 -0.1349 0.113 Uiso 0.50 1 calc PR F 2 H12C H 0.5866 0.6857 -0.1596 0.113 Uiso 0.50 1 calc PR F 2 O121 O 0.5122(14) 0.7655(15) 0.103(2) 0.102(17) Uiso 0.50 1 d P . . C121 C 0.4879(8) 0.5483(8) 0.0673(11) 0.045(8) Uiso 1 1 d . G . H1 H 0.5117 0.5625 0.0740 0.054 Uiso 1 1 calc R . . H2 H 0.4863 0.5393 0.0289 0.054 Uiso 1 1 calc R . . O122 O 0.5000 0.653(3) 0.2500 0.16(4) Uiso 0.50 2 d SP . . C122 C 0.4853(10) 0.5096(11) 0.1075(15) 0.071(11) Uiso 1 1 d . . . O123 O 0.4833(11) 0.7120(12) 0.1910(17) 0.072(14) Uiso 0.50 1 d P . . C123 C 0.5000(19) 0.513(2) 0.163(3) 0.09(3) Uiso 0.50 1 d P G 2 H3 H 0.4801 0.5191 0.1874 0.133 Uiso 0.50 1 calc PR G 2 H12D H 0.5188 0.5339 0.1659 0.133 Uiso 0.50 1 calc PR G 2 H12E H 0.5111 0.4866 0.1744 0.133 Uiso 0.50 1 calc PR G 2 O124 O 0.3327(14) 0.8200(15) 0.130(2) 0.103(17) Uiso 0.50 1 d P . . C124 C 0.491(2) 0.483(2) 0.091(3) 0.11(3) Uiso 0.50 1 d P G 1 H12F H 0.5008 0.4873 0.0547 0.162 Uiso 0.50 1 calc PR G 1 H12G H 0.4693 0.4660 0.0881 0.162 Uiso 0.50 1 calc PR G 1 H12H H 0.5103 0.4693 0.1140 0.162 Uiso 0.50 1 calc PR G 1 O125 O 0.2055(13) 0.6612(14) 0.152(2) 0.093(16) Uiso 0.50 1 d P . . C125 C 0.4060(7) 0.4681(7) -0.0677(10) 0.029(7) Uiso 1 1 d . . . H12I H 0.4006 0.4544 -0.1029 0.035 Uiso 1 1 calc R . . H12J H 0.4298 0.4823 -0.0698 0.035 Uiso 1 1 calc R . . O126 O 0.2825(14) 0.7321(15) 0.243(2) 0.104(18) Uiso 0.50 1 d P . . C126 C 0.4086(7) 0.4365(8) -0.0220(11) 0.039(8) Uiso 1 1 d . . . H12K H 0.4231 0.4135 -0.0356 0.047 Uiso 1 1 calc R . . H12L H 0.4235 0.4488 0.0083 0.047 Uiso 1 1 calc R . . O127 O 0.1895(13) 0.7882(14) 0.1590(19) 0.094(16) Uiso 0.50 1 d P . . C127 C 0.3765(8) 0.4194(9) 0.0010(12) 0.061(10) Uiso 1 1 d . . . H12M H 0.3614 0.4412 0.0153 0.092 Uiso 1 1 calc R . . H12N H 0.3840 0.4009 0.0306 0.092 Uiso 1 1 calc R . . H12O H 0.3622 0.4045 -0.0271 0.092 Uiso 1 1 calc R . . O128 O 0.0735(14) 0.7049(15) 0.309(2) 0.105(18) Uiso 0.50 1 d P . . O129 O 0.0256(19) 0.653(2) 0.339(3) 0.17(3) Uiso 0.50 1 d P . . O130 O 0.1732(11) 0.8984(13) 0.3708(16) 0.057(12) Uiso 0.50 1 d P H 2 O131 O 0.184(2) 0.935(3) 0.365(3) 0.20(3) Uiso 0.50 1 d P . 1 O102 O 0.2978(9) 0.5427(10) -0.2979(14) 0.040(10) Uiso 0.50 1 d P I 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 Cu1 0.026(2) 0.049(3) 0.071(3) 0.033(2) -0.004(2) 0.0077(18) Cu2 0.027(2) 0.060(3) 0.096(4) 0.037(3) -0.015(2) 0.000(2) Cu3 0.029(2) 0.055(3) 0.073(3) 0.032(2) -0.014(2) -0.0028(19) Cu4 0.016(2) 0.050(3) 0.089(3) 0.025(2) -0.001(2) -0.0054(18) Cu5 0.019(2) 0.057(3) 0.090(4) 0.008(2) 0.010(2) -0.0071(19) Cu6 0.018(2) 0.049(3) 0.124(4) -0.001(3) 0.017(2) -0.0013(19) Cu7 0.019(2) 0.073(3) 0.101(4) 0.059(3) 0.005(2) 0.004(2) Cu8 0.020(2) 0.092(4) 0.102(4) 0.075(3) -0.004(2) -0.010(2) Cu9 0.020(2) 0.078(3) 0.095(4) 0.063(3) 0.001(2) -0.002(2) Cu10 0.043(3) 0.039(2) 0.059(3) 0.028(2) 0.011(2) 0.0000(19) Cu11 0.035(2) 0.048(3) 0.068(3) 0.034(2) 0.009(2) -0.0086(19) Cu12 0.034(2) 0.038(2) 0.053(3) 0.028(2) 0.000(2) -0.0067(18) _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 Cu1 O31 1.963(17) 7_565 ? Cu1 O11 1.967(19) . ? Cu1 O32 1.971(18) . ? Cu1 O10 2.005(19) . ? O1 C2 1.43(3) . ? O1 Cu4 1.974(18) . ? C1 C2 1.31(3) . ? C1 C28 1.50(3) . ? C1 C6 1.52(4) . ? Cu2 O33 1.914(16) 7_565 ? Cu2 O32 1.930(18) . ? Cu2 O17 1.970(17) . ? Cu2 O18 2.007(18) . ? O2 C3 1.29(3) . ? O2 Cu4 1.96(2) . ? O2 Cu6 1.988(19) . ? C2 C3 1.42(3) . ? Cu3 O16 1.917(17) . ? Cu3 O17 1.933(18) . ? Cu3 O11 1.940(19) . ? Cu3 O12 1.959(19) . ? O3 C4 1.34(3) . ? O3 Cu6 1.924(19) . ? C3 C4 1.42(3) . ? Cu4 O15 1.926(19) . ? Cu4 O14 1.962(19) . ? O4 C9 1.35(3) . ? O4 Cu10 1.948(17) . ? C4 C5 1.35(3) . ? Cu5 O26 1.888(19) . ? Cu5 O13 1.894(17) . ? Cu5 O27 1.924(18) . ? Cu5 O14 1.948(18) . ? O5 C10 1.38(3) . ? O5 Cu12 1.886(17) . ? O5 Cu10 1.979(17) . ? C5 C6 1.45(3) . ? C5 C7 1.57(3) . ? Cu6 O26 1.972(19) . ? Cu6 O25 1.978(19) . ? O6 C11 1.45(3) . ? O6 Cu12 1.972(16) . ? Cu7 O29 1.921(19) . ? Cu7 O28 1.93(2) . ? Cu7 O24 1.954(17) . ? Cu7 O23 1.958(17) . ? O7 C16 1.48(3) . ? O7 Cu8 1.947(18) 7_565 ? C7 C29 1.51(3) . ? C7 C8 1.52(3) . ? Cu8 O23 1.929(17) . ? Cu8 O8 1.939(19) 7_565 ? Cu8 O22 1.940(16) . ? Cu8 O7 1.947(18) 7_565 ? O8 C17 1.47(3) . ? O8 Cu8 1.939(19) 7_565 ? O8 Cu9 1.965(19) 7_565 ? C8 C13 1.41(3) . ? C8 C9 1.42(3) . ? Cu9 O30 1.888(19) . ? Cu9 O9 1.94(2) 7_565 ? Cu9 O29 1.949(19) . ? Cu9 O8 1.966(19) 7_565 ? O9 C18 1.42(4) . ? O9 Cu9 1.94(2) 7_565 ? C9 C10 1.36(4) . ? Cu10 O36 1.945(17) . ? Cu10 O35 1.964(19) . ? O10 C23 1.47(3) . ? C10 C11 1.45(3) . ? Cu11 O35 1.904(18) . ? Cu11 O34 1.913(19) . ? Cu11 O20 1.952(18) 7_565 ? Cu11 O19 1.97(2) 7_565 ? O11 C24 1.46(3) . ? C11 C12 1.44(3) . ? Cu12 O20 1.952(18) 7_565 ? Cu12 O21 1.973(17) 7_565 ? O12 C25 1.32(3) . ? C12 C13 1.37(3) . ? C12 C14 1.42(3) . ? O13 C42 1.40(3) . ? O14 C43 1.52(3) . ? C14 C15 1.49(3) . ? C14 C32 1.54(3) . ? O15 C44 1.38(3) . ? C15 C16 1.34(3) . ? C15 C20 1.48(3) . ? O16 C49 1.35(3) . ? C16 C17 1.39(4) . ? O17 C50 1.32(3) . ? C17 C18 1.36(4) . ? O18 C51 1.39(3) . ? C18 C19 1.33(4) . ? O19 C56 1.35(3) . ? O19 Cu11 1.97(2) 7_565 ? C19 C20 1.34(3) . ? C19 C21 1.52(3) . ? O20 C57 1.41(3) . ? O20 Cu11 1.952(18) 7_565 ? O20 Cu12 1.952(18) 7_565 ? O21 C58 1.33(3) . ? O21 Cu12 1.973(17) 7_565 ? C21 C22 1.42(3) . ? C21 C35 1.56(3) . ? O22 C63 1.34(3) . ? C22 C23 1.38(4) . ? C22 C27 1.41(3) . ? O23 C64 1.41(3) . ? C23 C24 1.24(3) . ? O24 C65 1.40(3) . ? C24 C25 1.48(4) . ? O25 C84 1.29(3) . ? C25 C26 1.42(4) . ? O26 C85 1.44(3) . ? C26 C27 1.33(3) . ? C26 C28 1.60(3) . ? O27 C86 1.40(3) . ? O28 C91 1.41(3) . ? C28 C38 1.49(3) . ? O29 C92 1.42(3) . ? C29 C30 1.67(4) . ? O30 C93 1.43(3) . ? C30 C31 1.54(4) . ? O31 C98 1.38(3) . ? O31 Cu1 1.963(17) 7_565 ? O32 C99 1.38(3) 7_565 ? C32 C33 1.55(4) . ? O33 C100 1.32(3) . ? O33 Cu2 1.914(16) 7_565 ? C33 C34 1.48(5) . ? O34 C105 1.40(3) . ? O35 C106 1.39(3) . ? C35 C36 1.54(3) . ? O36 C107 1.33(3) . ? C36 C37 1.60(4) . ? C38 C39 1.57(3) . ? C39 C40 1.55(4) . ? C41 C46 1.36(3) . ? C41 C42 1.46(3) . ? C41 C68 1.50(3) . ? C42 C43 1.26(3) . ? C43 C44 1.45(3) . ? C44 C45 1.44(3) . ? C45 C46 1.41(3) . ? C45 C47 1.51(3) . ? C47 C48 1.50(3) . ? C47 C69 1.51(3) . ? C48 C53 1.37(3) . ? C48 C49 1.45(3) . ? C49 C50 1.45(3) . ? C50 C51 1.51(4) . ? C51 C52 1.35(4) . ? C52 C53 1.42(3) . ? C52 C54 1.46(3) . ? C54 C55 1.50(3) . ? C54 C72 1.60(3) . ? C55 C60 1.42(3) . ? C55 C56 1.44(3) . ? C56 C57 1.44(3) . ? C57 C58 1.35(3) . ? C58 C59 1.39(3) . ? C59 C60 1.37(3) . ? C59 C61 1.47(3) . ? C61 C62 1.49(3) . ? C61 C75 1.55(3) . ? C62 C63 1.37(3) . ? C62 C67 1.49(3) . ? C63 C64 1.46(4) . ? C64 C65 1.39(3) . ? C65 C66 1.38(3) . ? C66 C67 1.47(3) . ? C66 C68 1.49(3) . ? C68 C80 1.55(3) . ? C69 C70 1.56(3) . ? C70 C71 1.63(3) . ? C72 C73 1.70(4) . ? C73 C74 1.25(5) . ? C75 C76 1.39(4) . ? C75 C78 1.67(6) . ? C76 C77 1.50(8) . ? C78 C79 1.49(7) . ? C80 C81 1.46(3) . ? C81 C82 1.53(4) . ? C83 C88 1.34(3) . ? C83 C84 1.41(3) . ? C83 C110 1.52(4) . ? C84 C85 1.48(4) . ? C85 C86 1.30(4) . ? C86 C87 1.51(3) . ? C87 C88 1.40(3) . ? C87 C89 1.41(3) . ? C89 C90 1.50(3) . ? C89 C125 1.54(3) . ? C90 C91 1.40(4) . ? C90 C95 1.47(4) . ? C91 C92 1.37(4) . ? C92 C93 1.42(4) . ? C93 C94 1.38(4) . ? C94 C95 1.41(4) . ? C94 C96 1.52(4) . ? C96 C114 1.43(3) . ? C96 C97 1.54(4) . ? C97 C98 1.40(3) . ? C97 C102 1.45(4) . ? C98 C99 1.32(3) . ? C99 O32 1.38(3) 7_565 ? C99 C100 1.45(3) . ? C100 C101 1.36(3) . ? O101 O131 1.39(10) 7_565 ? C101 C102 1.36(3) . ? C101 C103 1.53(4) . ? C103 C104 1.45(3) . ? C103 C117 1.59(3) . ? C104 C105 1.29(3) . ? C104 C109 1.44(3) . ? C105 C106 1.36(3) . ? C106 C107 1.52(3) . ? C107 C108 1.47(3) . ? C108 C109 1.33(3) . ? C108 C110 1.57(4) . ? C110 C121 1.55(3) . ? C114 C115 1.47(4) . ? O115 O115 1.37(14) 2_554 ? C115 C116 1.58(5) . ? C117 C118 1.57(4) . ? C118 C120 1.23(6) . ? C118 C119 1.50(6) . ? C121 C122 1.62(4) . ? C122 C124 1.00(7) . ? C122 C123 1.46(7) . ? C125 C126 1.53(3) . ? C126 C127 1.44(3) . ? O131 O101 1.39(10) 7_565 ? 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 O31 Cu1 O11 172.1(8) 7_565 . ? O31 Cu1 O32 86.0(7) 7_565 . ? O11 Cu1 O32 98.0(8) . . ? O31 Cu1 O10 88.0(7) 7_565 . ? O11 Cu1 O10 87.4(8) . . ? O32 Cu1 O10 171.9(8) . . ? C2 O1 Cu4 109.1(15) . . ? C2 C1 C28 128(3) . . ? C2 C1 C6 118(3) . . ? C28 C1 C6 114(2) . . ? O33 Cu2 O32 85.3(7) 7_565 . ? O33 Cu2 O17 174.6(7) 7_565 . ? O32 Cu2 O17 97.7(7) . . ? O33 Cu2 O18 90.5(7) 7_565 . ? O32 Cu2 O18 175.8(8) . . ? O17 Cu2 O18 86.4(7) . . ? C3 O2 Cu4 113.6(17) . . ? C3 O2 Cu6 106.3(17) . . ? Cu4 O2 Cu6 139.5(11) . . ? C1 C2 C3 126(3) . . ? C1 C2 O1 119(3) . . ? C3 C2 O1 115(2) . . ? O16 Cu3 O17 86.1(8) . . ? O16 Cu3 O11 171.9(8) . . ? O17 Cu3 O11 98.3(8) . . ? O16 Cu3 O12 90.3(8) . . ? O17 Cu3 O12 172.0(8) . . ? O11 Cu3 O12 84.5(8) . . ? C4 O3 Cu6 112.7(16) . . ? O2 C3 C2 118(2) . . ? O2 C3 C4 124(2) . . ? C2 C3 C4 118(2) . . ? O15 Cu4 O14 86.2(8) . . ? O15 Cu4 O2 173.7(9) . . ? O14 Cu4 O2 99.5(8) . . ? O15 Cu4 O1 90.1(8) . . ? O14 Cu4 O1 174.9(8) . . ? O2 Cu4 O1 84.0(8) . . ? C9 O4 Cu10 111.6(17) . . ? O3 C4 C5 129(2) . . ? O3 C4 C3 112(2) . . ? C5 C4 C3 118(2) . . ? O26 Cu5 O13 175.0(8) . . ? O26 Cu5 O27 88.0(8) . . ? O13 Cu5 O27 87.6(7) . . ? O26 Cu5 O14 98.5(8) . . ? O13 Cu5 O14 85.7(7) . . ? O27 Cu5 O14 172.1(8) . . ? C10 O5 Cu12 114.5(16) . . ? C10 O5 Cu10 102.3(16) . . ? Cu12 O5 Cu10 143.2(10) . . ? C4 C5 C6 125(2) . . ? C4 C5 C7 116(2) . . ? C6 C5 C7 119(2) . . ? O3 Cu6 O26 177.5(8) . . ? O3 Cu6 O25 88.0(8) . . ? O26 Cu6 O25 89.5(8) . . ? O3 Cu6 O2 85.0(8) . . ? O26 Cu6 O2 97.4(8) . . ? O25 Cu6 O2 172.3(9) . . ? C11 O6 Cu12 107.8(14) . . ? C5 C6 C1 114(3) . . ? O29 Cu7 O28 87.1(8) . . ? O29 Cu7 O24 172.9(8) . . ? O28 Cu7 O24 87.6(8) . . ? O29 Cu7 O23 97.1(8) . . ? O28 Cu7 O23 174.6(8) . . ? O24 Cu7 O23 87.9(7) . . ? C16 O7 Cu8 109.8(15) . 7_565 ? C29 C7 C8 112(2) . . ? C29 C7 C5 114(2) . . ? C8 C7 C5 108(2) . . ? O23 Cu8 O8 97.6(8) . 7_565 ? O23 Cu8 O22 87.8(7) . . ? O8 Cu8 O22 174.6(8) 7_565 . ? O23 Cu8 O7 175.5(7) . 7_565 ? O8 Cu8 O7 86.9(8) 7_565 7_565 ? O22 Cu8 O7 87.7(7) . 7_565 ? C17 O8 Cu8 110.0(17) . 7_565 ? C17 O8 Cu9 105.6(16) . 7_565 ? Cu8 O8 Cu9 142.4(11) 7_565 7_565 ? C13 C8 C9 116(2) . . ? C13 C8 C7 126(3) . . ? C9 C8 C7 118(2) . . ? O30 Cu9 O9 89.9(8) . 7_565 ? O30 Cu9 O29 87.9(8) . . ? O9 Cu9 O29 177.4(9) 7_565 . ? O30 Cu9 O8 175.2(9) . 7_565 ? O9 Cu9 O8 85.9(8) 7_565 7_565 ? O29 Cu9 O8 96.2(8) . 7_565 ? C18 O9 Cu9 113.3(19) . 7_565 ? O4 C9 C10 112(3) . . ? O4 C9 C8 127(3) . . ? C10 C9 C8 121(3) . . ? O36 Cu10 O4 88.7(7) . . ? O36 Cu10 O35 88.1(8) . . ? O4 Cu10 O35 176.8(8) . . ? O36 Cu10 O5 175.4(8) . . ? O4 Cu10 O5 86.9(7) . . ? O35 Cu10 O5 96.3(7) . . ? C23 O10 Cu1 106.3(16) . . ? C9 C10 O5 127(3) . . ? C9 C10 C11 119(3) . . ? O5 C10 C11 114(2) . . ? O35 Cu11 O34 86.5(8) . . ? O35 Cu11 O20 96.7(8) . 7_565 ? O34 Cu11 O20 175.5(8) . 7_565 ? O35 Cu11 O19 177.4(9) . 7_565 ? O34 Cu11 O19 91.0(8) . 7_565 ? O20 Cu11 O19 85.8(8) 7_565 7_565 ? C24 O11 Cu3 114.8(17) . . ? C24 O11 Cu1 104.1(16) . . ? Cu3 O11 Cu1 141.1(11) . . ? C12 C11 O6 120(2) . . ? C12 C11 C10 123(3) . . ? O6 C11 C10 116(2) . . ? O5 Cu12 O20 97.3(8) . 7_565 ? O5 Cu12 O6 87.2(7) . . ? O20 Cu12 O6 172.8(8) 7_565 . ? O5 Cu12 O21 173.7(8) . 7_565 ? O20 Cu12 O21 86.0(7) 7_565 7_565 ? O6 Cu12 O21 89.1(7) . 7_565 ? C25 O12 Cu3 111.8(19) . . ? C13 C12 C14 126(3) . . ? C13 C12 C11 112(2) . . ? C14 C12 C11 122(2) . . ? C42 O13 Cu5 111.7(15) . . ? C12 C13 C8 129(3) . . ? C43 O14 Cu5 106.9(16) . . ? C43 O14 Cu4 112.5(16) . . ? Cu5 O14 Cu4 140.6(10) . . ? C12 C14 C15 111(2) . . ? C12 C14 C32 114(2) . . ? C15 C14 C32 115(2) . . ? C44 O15 Cu4 111.4(16) . . ? C16 C15 C20 116(2) . . ? C16 C15 C14 120(3) . . ? C20 C15 C14 124(2) . . ? C49 O16 Cu3 112.8(16) . . ? C15 C16 C17 120(3) . . ? C15 C16 O7 123(3) . . ? C17 C16 O7 115(3) . . ? C50 O17 Cu3 108.6(17) . . ? C50 O17 Cu2 109.2(17) . . ? Cu3 O17 Cu2 142.3(10) . . ? C18 C17 C16 120(3) . . ? C18 C17 O8 121(3) . . ? C16 C17 O8 115(3) . . ? C51 O18 Cu2 111.0(19) . . ? C19 C18 C17 122(3) . . ? C19 C18 O9 126(3) . . ? C17 C18 O9 112(3) . . ? C56 O19 Cu11 110.1(18) . 7_565 ? C18 C19 C20 119(3) . . ? C18 C19 C21 118(3) . . ? C20 C19 C21 123(3) . . ? C57 O20 Cu11 111.0(15) . 7_565 ? C57 O20 Cu12 106.3(15) . 7_565 ? Cu11 O20 Cu12 142.7(10) 7_565 7_565 ? C19 C20 C15 122(3) . . ? C58 O21 Cu12 109.8(14) . 7_565 ? C22 C21 C19 116(2) . . ? C22 C21 C35 111(2) . . ? C19 C21 C35 112(2) . . ? C63 O22 Cu8 109.0(16) . . ? C23 C22 C27 111(3) . . ? C23 C22 C21 122(3) . . ? C27 C22 C21 126(3) . . ? C64 O23 Cu8 109.5(15) . . ? C64 O23 Cu7 107.3(15) . . ? Cu8 O23 Cu7 142.3(9) . . ? C24 C23 C22 125(3) . . ? C24 C23 O10 117(3) . . ? C22 C23 O10 118(3) . . ? C65 O24 Cu7 107.9(16) . . ? C23 C24 O11 125(3) . . ? C23 C24 C25 127(3) . . ? O11 C24 C25 107(3) . . ? C84 O25 Cu6 106.0(18) . . ? O12 C25 C26 131(3) . . ? O12 C25 C24 122(3) . . ? C26 C25 C24 107(3) . . ? C85 O26 Cu5 108.7(16) . . ? C85 O26 Cu6 107.1(16) . . ? Cu5 O26 Cu6 144.1(10) . . ? C27 C26 C25 124(3) . . ? C27 C26 C28 122(2) . . ? C25 C26 C28 113(2) . . ? C86 O27 Cu5 106.5(17) . . ? C26 C27 C22 125(3) . . ? C91 O28 Cu7 110.5(17) . . ? C38 C28 C1 117(2) . . ? C38 C28 C26 112(2) . . ? C1 C28 C26 109(2) . . ? C92 O29 Cu7 108.0(17) . . ? C92 O29 Cu9 108.0(17) . . ? Cu7 O29 Cu9 144.0(11) . . ? C7 C29 C30 116(2) . . ? C93 O30 Cu9 112.5(16) . . ? C31 C30 C29 104(3) . . ? C98 O31 Cu1 109.3(15) . 7_565 ? C99 O32 Cu2 112.2(17) 7_565 . ? C99 O32 Cu1 105.6(16) 7_565 . ? Cu2 O32 Cu1 142.0(10) . . ? C14 C32 C33 115(2) . . ? C100 O33 Cu2 111.9(16) . 7_565 ? C34 C33 C32 113(3) . . ? C105 O34 Cu11 113.2(16) . . ? C106 O35 Cu11 106.1(15) . . ? C106 O35 Cu10 109.3(16) . . ? Cu11 O35 Cu10 143.6(10) . . ? C36 C35 C21 112(2) . . ? C107 O36 Cu10 109.6(15) . . ? C35 C36 C37 112(2) . . ? C28 C38 C39 114(2) . . ? C40 C39 C38 118(2) . . ? C46 C41 C42 114(3) . . ? C46 C41 C68 129(2) . . ? C42 C41 C68 117(2) . . ? C43 C42 O13 118(3) . . ? C43 C42 C41 115(3) . . ? O13 C42 C41 126(2) . . ? C42 C43 C44 136(3) . . ? C42 C43 O14 116(3) . . ? C44 C43 O14 108(2) . . ? O15 C44 C45 129(2) . . ? O15 C44 C43 122(2) . . ? C45 C44 C43 109(2) . . ? C46 C45 C44 117(2) . . ? C46 C45 C47 126(2) . . ? C44 C45 C47 116(2) . . ? C41 C46 C45 129(3) . . ? C48 C47 C45 106(2) . . ? C48 C47 C69 110(2) . . ? C45 C47 C69 118(2) . . ? C53 C48 C49 118(3) . . ? C53 C48 C47 124(3) . . ? C49 C48 C47 117(3) . . ? O16 C49 C48 129(3) . . ? O16 C49 C50 112(2) . . ? C48 C49 C50 119(3) . . ? O17 C50 C49 121(3) . . ? O17 C50 C51 122(3) . . ? C49 C50 C51 117(3) . . ? C52 C51 O18 126(3) . . ? C52 C51 C50 122(3) . . ? O18 C51 C50 112(3) . . ? C51 C52 C53 117(3) . . ? C51 C52 C54 118(3) . . ? C53 C52 C54 125(2) . . ? C48 C53 C52 126(3) . . ? C52 C54 C55 110(2) . . ? C52 C54 C72 116(2) . . ? C55 C54 C72 110(2) . . ? C60 C55 C56 114(2) . . ? C60 C55 C54 128(2) . . ? C56 C55 C54 117(2) . . ? O19 C56 C55 124(3) . . ? O19 C56 C57 119(3) . . ? C55 C56 C57 117(2) . . ? C58 C57 O20 120(2) . . ? C58 C57 C56 125(3) . . ? O20 C57 C56 114(2) . . ? O21 C58 C57 118(2) . . ? O21 C58 C59 124(2) . . ? C57 C58 C59 118(2) . . ? C60 C59 C58 118(2) . . ? C60 C59 C61 121(2) . . ? C58 C59 C61 118(2) . . ? C59 C60 C55 126(2) . . ? C59 C61 C62 114(2) . . ? C59 C61 C75 114(2) . . ? C62 C61 C75 114(2) . . ? C63 C62 C67 120(2) . . ? C63 C62 C61 122(2) . . ? C67 C62 C61 118(2) . . ? O22 C63 C62 126(3) . . ? O22 C63 C64 119(2) . . ? C62 C63 C64 115(3) . . ? C65 C64 O23 118(2) . . ? C65 C64 C63 127(3) . . ? O23 C64 C63 114(2) . . ? C66 C65 C64 119(3) . . ? C66 C65 O24 123(3) . . ? C64 C65 O24 118(3) . . ? C65 C66 C67 117(3) . . ? C65 C66 C68 122(3) . . ? C67 C66 C68 121(2) . . ? C66 C67 C62 122(2) . . ? C66 C68 C41 106(2) . . ? C66 C68 C80 118(2) . . ? C41 C68 C80 109(2) . . ? C47 C69 C70 110(2) . . ? C69 C70 C71 111(2) . . ? C54 C72 C73 116(2) . . ? C74 C73 C72 108(4) . . ? C76 C75 C61 108(3) . . ? C76 C75 C78 94(3) . . ? C61 C75 C78 117(3) . . ? C75 C76 C77 119(5) . . ? C79 C78 C75 121(4) . . ? C81 C80 C68 106(2) . . ? C80 C81 C82 119(3) . . ? C88 C83 C84 122(3) . . ? C88 C83 C110 122(3) . . ? C84 C83 C110 116(3) . . ? O25 C84 C83 128(3) . . ? O25 C84 C85 125(3) . . ? C83 C84 C85 107(3) . . ? C86 C85 O26 116(3) . . ? C86 C85 C84 131(3) . . ? O26 C85 C84 113(2) . . ? C85 C86 O27 121(3) . . ? C85 C86 C87 118(3) . . ? O27 C86 C87 121(3) . . ? C88 C87 C89 131(2) . . ? C88 C87 C86 108(2) . . ? C89 C87 C86 119(2) . . ? C83 C88 C87 131(3) . . ? C87 C89 C90 119(2) . . ? C87 C89 C125 111(2) . . ? C90 C89 C125 110(2) . . ? C91 C90 C95 112(3) . . ? C91 C90 C89 120(3) . . ? C95 C90 C89 125(3) . . ? C92 C91 C90 123(3) . . ? C92 C91 O28 115(3) . . ? C90 C91 O28 122(3) . . ? C91 C92 O29 120(3) . . ? C91 C92 C93 122(3) . . ? O29 C92 C93 118(3) . . ? C94 C93 C92 119(3) . . ? C94 C93 O30 127(3) . . ? C92 C93 O30 113(3) . . ? C93 C94 C95 117(3) . . ? C93 C94 C96 122(3) . . ? C95 C94 C96 120(3) . . ? C94 C95 C90 125(3) . . ? C114 C96 C94 116(3) . . ? C114 C96 C97 119(3) . . ? C94 C96 C97 108(2) . . ? C98 C97 C102 113(3) . . ? C98 C97 C96 123(3) . . ? C102 C97 C96 123(3) . . ? C99 C98 O31 116(2) . . ? C99 C98 C97 122(3) . . ? O31 C98 C97 122(2) . . ? C98 C99 O32 123(3) . 7_565 ? C98 C99 C100 125(3) . . ? O32 C99 C100 112(2) 7_565 . ? O33 C100 C101 127(3) . . ? O33 C100 C99 118(2) . . ? C101 C100 C99 115(3) . . ? C100 C101 C102 120(3) . . ? C100 C101 C103 121(3) . . ? C102 C101 C103 117(3) . . ? C101 C102 C97 125(3) . . ? C104 C103 C101 116(2) . . ? C104 C103 C117 116(2) . . ? C101 C103 C117 117(2) . . ? C105 C104 C109 118(3) . . ? C105 C104 C103 125(3) . . ? C109 C104 C103 116(2) . . ? C104 C105 C106 125(3) . . ? C104 C105 O34 126(3) . . ? C106 C105 O34 109(2) . . ? C105 C106 O35 124(2) . . ? C105 C106 C107 122(2) . . ? O35 C106 C107 114(2) . . ? O36 C107 C108 131(2) . . ? O36 C107 C106 119(2) . . ? C108 C107 C106 109(2) . . ? C109 C108 C107 124(3) . . ? C109 C108 C110 128(3) . . ? C107 C108 C110 107(2) . . ? C108 C109 C104 122(3) . . ? C83 C110 C121 113(2) . . ? C83 C110 C108 113(2) . . ? C121 C110 C108 108(2) . . ? C96 C114 C115 116(3) . . ? C114 C115 C116 119(3) . . ? C118 C117 C103 116(3) . . ? C120 C118 C119 87(5) . . ? C120 C118 C117 107(4) . . ? C119 C118 C117 109(4) . . ? C110 C121 C122 108(2) . . ? C124 C122 C123 111(7) . . ? C124 C122 C121 115(6) . . ? C123 C122 C121 120(4) . . ? C126 C125 C89 110(2) . . ? C127 C126 C125 122(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.25 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 5.210 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.213 # Attachment '2.cif' data_PgC12EtOAc _database_code_depnum_ccdc_archive 'CCDC 648030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H126 O16.75' _chemical_formula_weight 1367.82 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' O O 0.0106 0.0060 '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 12.017(4) _cell_length_b 13.104(4) _cell_length_c 26.595(7) _cell_angle_alpha 86.693(5) _cell_angle_beta 78.650(5) _cell_angle_gamma 77.855(5) _cell_volume 4013(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9764 _exptl_absorpt_correction_T_max 0.9809 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 SMART 1000 CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19667 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.14 _reflns_number_total 15765 _reflns_number_gt 10157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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 crystals were weakly diffracting. A restraint was applied to the ethyl group of the disordered EtOAc molecule. ; _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^)+(0.1452P)^2^+2.9778P] 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 15765 _refine_ls_number_parameters 975 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2626 _refine_ls_wR_factor_gt 0.2286 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max '0.207 (H-tors)' _refine_ls_shift/su_mean 0.003 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 O1 O 0.01629(16) 0.12706(16) 0.45547(8) 0.0295(5) Uani 1 1 d . . . H101 H 0.0163 0.0660 0.4475 0.035 Uiso 1 1 calc R . . O2 O 0.10462(17) 0.26348(17) 0.50192(8) 0.0338(5) Uani 1 1 d . . . H102 H 0.0344 0.2593 0.5076 0.041 Uiso 1 1 calc R . . O3 O 0.29246(18) 0.33446(17) 0.45599(9) 0.0395(6) Uani 1 1 d . . . H103 H 0.3646 0.3276 0.4469 0.047 Uiso 1 1 calc R . . O4 O 0.52453(19) 0.33894(17) 0.43042(10) 0.0423(6) Uani 1 1 d . . . H104 H 0.5644 0.3496 0.4515 0.051 Uiso 1 1 calc R . . O5 O 0.7308(2) 0.23431(18) 0.45037(10) 0.0445(6) Uani 1 1 d . . . H105 H 0.7905 0.1919 0.4557 0.053 Uiso 1 1 calc R . . O6 O 0.83951(17) 0.05109(16) 0.40474(9) 0.0360(5) Uani 1 1 d . . . H106 H 0.8382 -0.0122 0.4113 0.043 Uiso 1 1 calc R . . O7 O 0.82666(18) -0.16316(16) 0.40351(9) 0.0338(5) Uani 1 1 d . . . H107 H 0.8433 -0.2062 0.4269 0.041 Uiso 1 1 calc R . . O8 O 0.7483(2) -0.34685(17) 0.43546(9) 0.0389(6) Uani 1 1 d . . . H108 H 0.6973 -0.3485 0.4619 0.047 Uiso 1 1 calc R . . O9 O 0.57191(18) -0.39671(15) 0.39590(8) 0.0325(5) Uani 1 1 d . . . H109 H 0.6176 -0.4499 0.3824 0.039 Uiso 1 1 calc R . . O10 O 0.33671(18) -0.37443(16) 0.40910(9) 0.0359(5) Uani 1 1 d . . . H110 H 0.4086 -0.3836 0.4075 0.043 Uiso 1 1 calc R . . O11 O 0.13151(17) -0.27178(16) 0.46384(8) 0.0313(5) Uani 1 1 d . . . H111 H 0.1562 -0.3367 0.4627 0.038 Uiso 1 1 calc R . . O12 O 0.03261(16) -0.07695(15) 0.43859(8) 0.0270(4) Uani 1 1 d . . . H112 H 0.0120 -0.1179 0.4624 0.032 Uiso 1 1 calc R . . O13 O 0.1631(3) -0.4706(2) 0.48933(12) 0.0692(10) Uani 1 1 d . . . O14 O 0.3851(3) 0.52742(18) 0.52442(11) 0.0557(7) Uani 1 1 d . . . O15 O 0.0347(6) -0.4694(6) 0.3434(3) 0.057(2) Uiso 0.50 1 d P A 1 O16 O -0.0042(6) -0.4490(5) 0.3465(3) 0.0527(18) Uiso 0.50 1 d P B 2 O17 O 0.0162(6) -0.5205(5) 0.4284(3) 0.0550(19) Uiso 0.50 1 d P B 2 O18 O -0.0148(9) -0.5201(8) 0.4185(5) 0.090(3) Uiso 0.50 1 d P A 1 O19 O 0.5000 0.0000 0.5000 0.0857(14) Uiso 1 2 d S . . C1 C 0.1712(2) 0.1222(2) 0.37918(11) 0.0218(6) Uani 1 1 d . . . C2 C 0.1150(2) 0.1579(2) 0.42799(11) 0.0244(6) Uani 1 1 d . . . C3 C 0.1562(2) 0.2294(2) 0.45268(11) 0.0267(6) Uani 1 1 d . . . C4 C 0.2537(2) 0.2665(2) 0.42880(12) 0.0288(7) Uani 1 1 d . . . C5 C 0.3104(2) 0.2357(2) 0.37918(11) 0.0251(6) Uani 1 1 d . . . C6 C 0.2681(2) 0.1625(2) 0.35612(11) 0.0237(6) Uani 1 1 d . . . H6 H 0.3074 0.1387 0.3230 0.028 Uiso 1 1 calc R . . C7 C 0.4161(2) 0.2792(2) 0.35346(12) 0.0291(7) Uani 1 1 d . . . H7 H 0.4061 0.3492 0.3689 0.035 Uiso 1 1 calc R . . C8 C 0.5280(2) 0.2141(2) 0.36690(12) 0.0263(6) Uani 1 1 d . . . C9 C 0.5789(2) 0.2490(2) 0.40381(13) 0.0308(7) Uani 1 1 d . . . C10 C 0.6831(2) 0.1937(2) 0.41468(12) 0.0302(7) Uani 1 1 d . . . C11 C 0.7368(2) 0.1004(2) 0.39010(12) 0.0277(6) Uani 1 1 d . . . C12 C 0.6896(2) 0.0633(2) 0.35274(11) 0.0243(6) Uani 1 1 d . . . C13 C 0.5845(2) 0.1213(2) 0.34250(11) 0.0251(6) Uani 1 1 d . . . H13 H 0.5501 0.0961 0.3177 0.030 Uiso 1 1 calc R . . C14 C 0.7528(2) -0.0347(2) 0.32270(11) 0.0261(6) Uani 1 1 d . . . H14 H 0.8333 -0.0500 0.3299 0.031 Uiso 1 1 calc R . . C15 C 0.7017(2) -0.1304(2) 0.34207(11) 0.0230(6) Uani 1 1 d . . . C16 C 0.7427(2) -0.1921(2) 0.38151(11) 0.0241(6) Uani 1 1 d . . . C17 C 0.7008(2) -0.2812(2) 0.39886(11) 0.0259(6) Uani 1 1 d . . . C18 C 0.6142(2) -0.3087(2) 0.37791(11) 0.0245(6) Uani 1 1 d . . . C19 C 0.5675(2) -0.2473(2) 0.33939(11) 0.0232(6) Uani 1 1 d . . . C20 C 0.6141(2) -0.1596(2) 0.32199(11) 0.0244(6) Uani 1 1 d . . . H20 H 0.5848 -0.1179 0.2952 0.029 Uiso 1 1 calc R . . C21 C 0.4672(2) -0.2761(2) 0.31939(11) 0.0248(6) Uani 1 1 d . . . H21 H 0.4733 -0.3528 0.3258 0.030 Uiso 1 1 calc R . . C22 C 0.3503(2) -0.2228(2) 0.35136(11) 0.0232(6) Uani 1 1 d . . . C23 C 0.2953(2) -0.2739(2) 0.39349(12) 0.0264(6) Uani 1 1 d . . . C24 C 0.1890(2) -0.2247(2) 0.42177(11) 0.0252(6) Uani 1 1 d . . . C25 C 0.1372(2) -0.1247(2) 0.40884(11) 0.0240(6) Uani 1 1 d . . . C26 C 0.1888(2) -0.0705(2) 0.36689(11) 0.0212(6) Uani 1 1 d . . . C27 C 0.2955(2) -0.1217(2) 0.33937(11) 0.0235(6) Uani 1 1 d . . . H27 H 0.3328 -0.0859 0.3110 0.028 Uiso 1 1 calc R . . C28 C 0.1296(2) 0.0396(2) 0.35281(11) 0.0236(6) Uani 1 1 d . . . H28 H 0.0449 0.0465 0.3671 0.028 Uiso 1 1 calc R . . C29 C 0.4253(3) 0.2990(3) 0.29668(13) 0.0364(8) Uani 1 1 d . . . H29A H 0.4236 0.2336 0.2802 0.044 Uiso 1 1 calc R . . H29B H 0.5010 0.3180 0.2826 0.044 Uiso 1 1 calc R . . C30 C 0.3281(3) 0.3862(3) 0.28235(15) 0.0490(9) Uani 1 1 d . . . H30A H 0.2590 0.3566 0.2818 0.059 Uiso 1 1 calc R . . H30B H 0.3061 0.4404 0.3089 0.059 Uiso 1 1 calc R . . C31 C 0.3645(4) 0.4367(3) 0.23022(16) 0.0542(10) Uani 1 1 d . . . H31A H 0.3003 0.4936 0.2236 0.065 Uiso 1 1 calc R . . H31B H 0.4321 0.4681 0.2312 0.065 Uiso 1 1 calc R . . C32 C 0.3956(4) 0.3612(3) 0.18694(16) 0.0544(10) Uani 1 1 d . . . H32A H 0.3242 0.3397 0.1822 0.065 Uiso 1 1 calc R . . H32B H 0.4487 0.2980 0.1968 0.065 Uiso 1 1 calc R . . C33 C 0.4531(4) 0.4029(3) 0.13553(16) 0.0546(10) Uani 1 1 d . . . H33A H 0.3987 0.4638 0.1244 0.066 Uiso 1 1 calc R . . H33B H 0.5229 0.4272 0.1403 0.066 Uiso 1 1 calc R . . C34 C 0.4876(4) 0.3226(3) 0.09396(16) 0.0593(11) Uani 1 1 d . . . H34A H 0.4169 0.3012 0.0882 0.071 Uiso 1 1 calc R . . H34B H 0.5381 0.2602 0.1061 0.071 Uiso 1 1 calc R . . C35 C 0.5508(4) 0.3591(3) 0.04300(16) 0.0551(10) Uani 1 1 d . . . H35A H 0.5001 0.4210 0.0304 0.066 Uiso 1 1 calc R . . H35B H 0.6213 0.3810 0.0486 0.066 Uiso 1 1 calc R . . C36 C 0.5853(4) 0.2766(3) 0.00215(16) 0.0591(11) Uani 1 1 d . . . H36A H 0.5146 0.2546 -0.0031 0.071 Uiso 1 1 calc R . . H36B H 0.6359 0.2149 0.0149 0.071 Uiso 1 1 calc R . . C37 C 0.6481(4) 0.3108(3) -0.04920(16) 0.0543(10) Uani 1 1 d . . . H37A H 0.5975 0.3724 -0.0620 0.065 Uiso 1 1 calc R . . H37B H 0.7188 0.3330 -0.0439 0.065 Uiso 1 1 calc R . . C38 C 0.6827(4) 0.2282(3) -0.08977(16) 0.0566(10) Uani 1 1 d . . . H38A H 0.6120 0.2058 -0.0948 0.068 Uiso 1 1 calc R . . H38B H 0.7334 0.1668 -0.0769 0.068 Uiso 1 1 calc R . . C39 C 0.7455(4) 0.2615(3) -0.14163(16) 0.0558(10) Uani 1 1 d . . . H39A H 0.6939 0.3211 -0.1554 0.067 Uiso 1 1 calc R . . H39B H 0.8151 0.2860 -0.1367 0.067 Uiso 1 1 calc R . . C40 C 0.7822(4) 0.1763(4) -0.18043(17) 0.0664(12) Uani 1 1 d . . . H40A H 0.8319 0.1162 -0.1669 0.100 Uiso 1 1 calc R . . H40B H 0.8253 0.2018 -0.2122 0.100 Uiso 1 1 calc R . . H40C H 0.7135 0.1551 -0.1876 0.100 Uiso 1 1 calc R . . C41 C 0.7654(3) -0.0142(2) 0.26545(12) 0.0313(7) Uani 1 1 d . . . H41A H 0.8018 0.0472 0.2568 0.038 Uiso 1 1 calc R . . H41B H 0.6870 0.0042 0.2570 0.038 Uiso 1 1 calc R . . C42 C 0.8365(3) -0.1043(3) 0.23138(13) 0.0377(8) Uani 1 1 d . . . H42A H 0.9066 -0.1360 0.2454 0.045 Uiso 1 1 calc R . . H42B H 0.7901 -0.1586 0.2320 0.045 Uiso 1 1 calc R . . C43 C 0.8729(3) -0.0690(3) 0.17630(13) 0.0367(7) Uani 1 1 d . . . H43A H 0.8049 -0.0238 0.1651 0.044 Uiso 1 1 calc R . . H43B H 0.9322 -0.0262 0.1752 0.044 Uiso 1 1 calc R . . C44 C 0.9213(3) -0.1565(3) 0.13865(13) 0.0383(8) Uani 1 1 d . . . H44A H 0.8589 -0.1935 0.1359 0.046 Uiso 1 1 calc R . . H44B H 0.9827 -0.2071 0.1520 0.046 Uiso 1 1 calc R . . C45 C 0.9718(3) -0.1191(3) 0.08518(13) 0.0404(8) Uani 1 1 d . . . H45A H 0.9123 -0.0639 0.0733 0.049 Uiso 1 1 calc R . . H45B H 1.0384 -0.0874 0.0876 0.049 Uiso 1 1 calc R . . C46 C 1.0122(3) -0.2042(3) 0.04526(13) 0.0405(8) Uani 1 1 d . . . H46A H 0.9448 -0.2332 0.0412 0.049 Uiso 1 1 calc R . . H46B H 1.0685 -0.2614 0.0579 0.049 Uiso 1 1 calc R . . C47 C 1.0684(3) -0.1667(3) -0.00702(13) 0.0434(8) Uani 1 1 d . . . H47A H 1.1379 -0.1408 -0.0032 0.052 Uiso 1 1 calc R . . H47B H 1.0134 -0.1072 -0.0189 0.052 Uiso 1 1 calc R . . C48 C 1.1043(3) -0.2504(3) -0.04810(13) 0.0439(8) Uani 1 1 d . . . H48A H 1.1585 -0.3103 -0.0361 0.053 Uiso 1 1 calc R . . H48B H 1.0346 -0.2756 -0.0523 0.053 Uiso 1 1 calc R . . C49 C 1.1618(4) -0.2132(3) -0.09997(14) 0.0462(9) Uani 1 1 d . . . H49A H 1.2346 -0.1930 -0.0962 0.055 Uiso 1 1 calc R . . H49B H 1.1101 -0.1499 -0.1107 0.055 Uiso 1 1 calc R . . C50 C 1.1896(4) -0.2935(3) -0.14213(14) 0.0463(9) Uani 1 1 d . . . H50A H 1.2445 -0.3554 -0.1322 0.056 Uiso 1 1 calc R . . H50B H 1.1175 -0.3163 -0.1448 0.056 Uiso 1 1 calc R . . C51 C 1.2416(4) -0.2542(3) -0.19428(14) 0.0524(10) Uani 1 1 d . . . H51A H 1.3183 -0.2395 -0.1927 0.063 Uiso 1 1 calc R . . H51B H 1.1914 -0.1874 -0.2022 0.063 Uiso 1 1 calc R . . C52 C 1.2564(4) -0.3295(4) -0.23784(16) 0.0621(12) Uani 1 1 d . . . H52A H 1.3131 -0.3929 -0.2324 0.093 Uiso 1 1 calc R . . H52B H 1.2838 -0.2962 -0.2706 0.093 Uiso 1 1 calc R . . H52C H 1.1818 -0.3480 -0.2385 0.093 Uiso 1 1 calc R . . C53 C 0.4728(3) -0.2586(3) 0.26159(12) 0.0315(7) Uani 1 1 d . . . H53A H 0.4031 -0.2762 0.2525 0.038 Uiso 1 1 calc R . . H53B H 0.4704 -0.1835 0.2535 0.038 Uiso 1 1 calc R . . C54 C 0.5804(3) -0.3223(3) 0.22816(12) 0.0357(7) Uani 1 1 d . . . H54A H 0.6488 -0.2938 0.2311 0.043 Uiso 1 1 calc R . . H54B H 0.5929 -0.3953 0.2412 0.043 Uiso 1 1 calc R . . C55 C 0.5713(3) -0.3216(3) 0.17241(13) 0.0475(9) Uani 1 1 d . . . H55A H 0.5488 -0.2483 0.1609 0.057 Uiso 1 1 calc R . . H55B H 0.5082 -0.3575 0.1693 0.057 Uiso 1 1 calc R . . C56 C 0.6811(3) -0.3732(3) 0.13653(13) 0.0404(8) Uani 1 1 d . . . H56A H 0.7435 -0.3357 0.1385 0.049 Uiso 1 1 calc R . . H56B H 0.7053 -0.4458 0.1487 0.049 Uiso 1 1 calc R . . C57 C 0.6691(3) -0.3753(4) 0.08101(14) 0.0554(11) Uani 1 1 d . . . H57A H 0.6098 -0.4163 0.0789 0.066 Uiso 1 1 calc R . . H57B H 0.6402 -0.3030 0.0696 0.066 Uiso 1 1 calc R . . C58 C 0.7787(3) -0.4204(3) 0.04435(13) 0.0428(8) Uani 1 1 d . . . H58A H 0.8080 -0.4925 0.0560 0.051 Uiso 1 1 calc R . . H58B H 0.8378 -0.3790 0.0463 0.051 Uiso 1 1 calc R . . C59 C 0.7670(3) -0.4235(4) -0.01105(14) 0.0565(11) Uani 1 1 d . . . H59A H 0.7371 -0.3515 -0.0226 0.068 Uiso 1 1 calc R . . H59B H 0.7085 -0.4655 -0.0130 0.068 Uiso 1 1 calc R . . C60 C 0.8776(3) -0.4680(3) -0.04789(13) 0.0433(9) Uani 1 1 d . . . H60A H 0.9359 -0.4259 -0.0459 0.052 Uiso 1 1 calc R . . H60B H 0.9076 -0.5399 -0.0362 0.052 Uiso 1 1 calc R . . C61 C 0.8672(3) -0.4720(4) -0.10344(14) 0.0552(11) Uani 1 1 d . . . H61A H 0.8392 -0.4001 -0.1156 0.066 Uiso 1 1 calc R . . H61B H 0.8081 -0.5131 -0.1056 0.066 Uiso 1 1 calc R . . C62 C 0.9790(3) -0.5190(3) -0.13903(13) 0.0413(8) Uani 1 1 d . . . H62A H 1.0379 -0.4779 -0.1364 0.050 Uiso 1 1 calc R . . H62B H 1.0067 -0.5907 -0.1265 0.050 Uiso 1 1 calc R . . C63 C 0.9731(4) -0.5243(4) -0.19480(15) 0.0615(12) Uani 1 1 d . . . H63A H 0.9138 -0.5647 -0.1977 0.074 Uiso 1 1 calc R . . H63B H 0.9472 -0.4526 -0.2078 0.074 Uiso 1 1 calc R . . C64 C 1.0856(3) -0.5730(3) -0.22857(15) 0.0540(10) Uani 1 1 d . . . H64A H 1.1453 -0.5340 -0.2259 0.081 Uiso 1 1 calc R . . H64B H 1.0750 -0.5712 -0.2642 0.081 Uiso 1 1 calc R . . H64C H 1.1098 -0.6456 -0.2175 0.081 Uiso 1 1 calc R . . C65 C 0.1416(3) 0.0560(2) 0.29467(11) 0.0291(7) Uani 1 1 d . C . H65A H 0.1194 -0.0030 0.2802 0.035 Uiso 1 1 calc R . . H65B H 0.2239 0.0552 0.2796 0.035 Uiso 1 1 calc R . . C66 C 0.0669(3) 0.1590(3) 0.27875(13) 0.0393(8) Uani 1 1 d . . . C67 C 0.0605(6) 0.1536(6) 0.2203(3) 0.0397(16) Uani 0.50 1 d P C 2 H67A H 0.0211 0.0960 0.2167 0.048 Uiso 0.50 1 calc PR C 2 H67B H 0.0100 0.2192 0.2111 0.048 Uiso 0.50 1 calc PR C 2 C68 C 0.1731(8) 0.1379(7) 0.1805(3) 0.037(2) Uani 0.50 1 d P C 2 H68A H 0.2114 0.1972 0.1821 0.045 Uiso 0.50 1 calc PR C 2 H68B H 0.2256 0.0736 0.1897 0.045 Uiso 0.50 1 calc PR C 2 C69 C 0.1569(11) 0.1291(9) 0.1255(5) 0.043(2) Uani 0.50 1 d P C 2 H69A H 0.1118 0.0744 0.1246 0.051 Uiso 0.50 1 calc PR C 2 H69B H 0.1105 0.1961 0.1153 0.051 Uiso 0.50 1 calc PR C 2 C70 C 0.2671(8) 0.1038(7) 0.0867(3) 0.0433(18) Uani 0.50 1 d P C 2 H70A H 0.3164 0.0399 0.0983 0.052 Uiso 0.50 1 calc PR C 2 H70B H 0.3093 0.1614 0.0855 0.052 Uiso 0.50 1 calc PR C 2 C71 C 0.2509(14) 0.0867(10) 0.0325(6) 0.050(3) Uani 0.50 1 d P C 2 H71A H 0.2039 0.1515 0.0204 0.059 Uiso 0.50 1 calc PR C 2 H71B H 0.2063 0.0308 0.0339 0.059 Uiso 0.50 1 calc PR C 2 C72 C 0.3632(8) 0.0574(7) -0.0066(3) 0.0451(18) Uani 0.50 1 d P C 2 H72A H 0.4067 0.1143 -0.0085 0.054 Uiso 0.50 1 calc PR C 2 H72B H 0.4110 -0.0063 0.0060 0.054 Uiso 0.50 1 calc PR C 2 C73 C 0.3476(12) 0.0378(9) -0.0602(5) 0.046(3) Uani 0.50 1 d P C 2 H73A H 0.3033 -0.0185 -0.0581 0.056 Uiso 0.50 1 calc PR C 2 H73B H 0.3003 0.1018 -0.0728 0.056 Uiso 0.50 1 calc PR C 2 C74 C 0.4576(8) 0.0079(6) -0.0991(3) 0.0420(18) Uani 0.50 1 d P C 2 H74A H 0.5046 -0.0569 -0.0870 0.050 Uiso 0.50 1 calc PR C 2 H74B H 0.5027 0.0636 -0.1011 0.050 Uiso 0.50 1 calc PR C 2 C75 C 0.4388(11) -0.0098(9) -0.1530(5) 0.049(3) Uani 0.50 1 d P C 2 H75A H 0.3946 -0.0662 -0.1511 0.059 Uiso 0.50 1 calc PR C 2 H75B H 0.3911 0.0546 -0.1650 0.059 Uiso 0.50 1 calc PR C 2 C76 C 0.5500(9) -0.0387(9) -0.1918(4) 0.052(2) Uani 0.50 1 d P C 2 H76A H 0.5945 0.0166 -0.1939 0.078 Uiso 0.50 1 calc PR C 2 H76B H 0.5316 -0.0469 -0.2255 0.078 Uiso 0.50 1 calc PR C 2 H76C H 0.5959 -0.1045 -0.1813 0.078 Uiso 0.50 1 calc PR C 2 C77 C 0.1026(7) 0.2040(6) 0.2272(3) 0.0403(16) Uani 0.50 1 d P C 1 H77A H 0.1758 0.2280 0.2262 0.048 Uiso 0.50 1 calc PR C 1 H77B H 0.0427 0.2658 0.2215 0.048 Uiso 0.50 1 calc PR C 1 C78 C 0.1200(8) 0.1287(7) 0.1841(3) 0.037(2) Uani 0.50 1 d P C 1 H78A H 0.0447 0.1106 0.1831 0.044 Uiso 0.50 1 calc PR C 1 H78B H 0.1734 0.0638 0.1919 0.044 Uiso 0.50 1 calc PR C 1 C79 C 0.1684(11) 0.1690(9) 0.1315(5) 0.042(2) Uani 0.50 1 d P C 1 H79A H 0.2377 0.1967 0.1339 0.050 Uiso 0.50 1 calc PR C 1 H79B H 0.1099 0.2279 0.1217 0.050 Uiso 0.50 1 calc PR C 1 C80 C 0.2019(9) 0.0888(6) 0.0891(3) 0.0443(18) Uani 0.50 1 d P C 1 H80A H 0.1316 0.0640 0.0855 0.053 Uiso 0.50 1 calc PR C 1 H80B H 0.2570 0.0282 0.0999 0.053 Uiso 0.50 1 calc PR C 1 C81 C 0.2563(12) 0.1268(9) 0.0367(6) 0.041(3) Uani 0.50 1 d P C 1 H81A H 0.1991 0.1840 0.0247 0.049 Uiso 0.50 1 calc PR C 1 H81B H 0.3235 0.1563 0.0406 0.049 Uiso 0.50 1 calc PR C 1 C82 C 0.2968(9) 0.0435(7) -0.0041(3) 0.0456(18) Uani 0.50 1 d P C 1 H82A H 0.3548 -0.0132 0.0078 0.055 Uiso 0.50 1 calc PR C 1 H82B H 0.2298 0.0135 -0.0076 0.055 Uiso 0.50 1 calc PR C 1 C83 C 0.3494(11) 0.0813(8) -0.0561(5) 0.041(2) Uani 0.50 1 d P C 1 H83A H 0.4146 0.1137 -0.0524 0.049 Uiso 0.50 1 calc PR C 1 H83B H 0.2905 0.1361 -0.0686 0.049 Uiso 0.50 1 calc PR C 1 C84 C 0.3938(9) -0.0037(6) -0.0963(3) 0.0430(18) Uani 0.50 1 d P C 1 H84A H 0.4526 -0.0585 -0.0836 0.052 Uiso 0.50 1 calc PR C 1 H84B H 0.3285 -0.0362 -0.0998 0.052 Uiso 0.50 1 calc PR C 1 C85 C 0.4472(10) 0.0328(8) -0.1491(4) 0.039(2) Uani 0.50 1 d P C 1 H85A H 0.3879 0.0857 -0.1626 0.047 Uiso 0.50 1 calc PR C 1 H85B H 0.5113 0.0670 -0.1457 0.047 Uiso 0.50 1 calc PR C 1 C86 C 0.4936(9) -0.0545(9) -0.1876(4) 0.054(3) Uani 0.50 1 d P C 1 H86A H 0.5500 -0.1087 -0.1740 0.082 Uiso 0.50 1 calc PR C 1 H86B H 0.5312 -0.0264 -0.2199 0.082 Uiso 0.50 1 calc PR C 1 H86C H 0.4294 -0.0846 -0.1936 0.082 Uiso 0.50 1 calc PR C 1 C103 C 0.0758(10) -0.3023(8) 0.3141(4) 0.058(3) Uiso 0.50 1 d P B 2 H10D H 0.1206 -0.3401 0.2835 0.087 Uiso 0.50 1 calc PR B 2 H10E H 0.1169 -0.2501 0.3223 0.087 Uiso 0.50 1 calc PR B 2 H10F H -0.0007 -0.2674 0.3077 0.087 Uiso 0.50 1 calc PR B 2 C104 C 0.0630(11) -0.3713(11) 0.3546(5) 0.059(4) Uiso 0.50 1 d P B 2 H10A H 0.0235 -0.3320 0.3860 0.070 Uiso 0.50 1 calc PR B 2 H10B H 0.1406 -0.4082 0.3600 0.070 Uiso 0.50 1 calc PR B 2 C105 C 0.1133(9) -0.3261(8) 0.3075(4) 0.056(3) Uiso 0.50 1 d PD A 1 H10G H 0.1690 -0.3722 0.2823 0.084 Uiso 0.50 1 calc PR A 1 H10H H 0.1471 -0.2677 0.3143 0.084 Uiso 0.50 1 calc PR A 1 H10I H 0.0424 -0.2992 0.2939 0.084 Uiso 0.50 1 calc PR A 1 C106 C 0.0834(11) -0.3887(9) 0.3583(4) 0.047(3) Uiso 0.50 1 d PD A 1 H10C H 0.1540 -0.4181 0.3725 0.057 Uiso 0.50 1 calc PR A 1 H10J H 0.0270 -0.3438 0.3844 0.057 Uiso 0.50 1 calc PR A 1 C107 C -0.0126(9) -0.5228(8) 0.3806(4) 0.043(2) Uiso 0.50 1 d P B 2 C108 C -0.0619(12) -0.6096(10) 0.3701(5) 0.087(3) Uiso 0.50 1 d P B 2 H10X H -0.0008 -0.6727 0.3644 0.131 Uiso 0.50 1 calc PR B 2 H10K H -0.0963 -0.5934 0.3393 0.131 Uiso 0.50 1 calc PR B 2 H10L H -0.1218 -0.6212 0.3993 0.131 Uiso 0.50 1 calc PR B 2 C109 C -0.0437(15) -0.5102(15) 0.3805(8) 0.101(6) Uiso 0.50 1 d P A 1 C110 C -0.1171(10) -0.5783(9) 0.3687(4) 0.070(3) Uiso 0.50 1 d P A 1 H11A H -0.1362 -0.6232 0.3985 0.105 Uiso 0.50 1 calc PR A 1 H11B H -0.0756 -0.6217 0.3393 0.105 Uiso 0.50 1 calc PR A 1 H11C H -0.1886 -0.5355 0.3603 0.105 Uiso 0.50 1 calc PR A 1 C111 C 0.4002(12) 0.0169(10) 0.4834(5) 0.038(3) Uiso 0.25 1 d P D 1 C112 C 0.4758(11) -0.0805(10) 0.4724(5) 0.038(3) Uiso 0.25 1 d P D 2 C113 C 0.3823(8) -0.0557(7) 0.4552(4) 0.063(2) Uiso 0.50 1 d P . . O20 O 0.3260(11) 0.0830(10) 0.5070(5) 0.069(3) Uiso 0.25 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 O1 0.0281(10) 0.0328(11) 0.0281(12) -0.0064(9) 0.0034(8) -0.0139(9) O2 0.0246(10) 0.0460(13) 0.0318(12) -0.0153(10) 0.0007(9) -0.0110(9) O3 0.0276(11) 0.0415(13) 0.0525(15) -0.0206(11) -0.0035(10) -0.0125(9) O4 0.0323(11) 0.0369(12) 0.0603(16) -0.0206(11) -0.0128(11) -0.0035(10) O5 0.0415(13) 0.0385(13) 0.0603(17) -0.0141(12) -0.0255(12) -0.0050(10) O6 0.0287(11) 0.0308(11) 0.0532(15) -0.0018(10) -0.0188(10) -0.0061(9) O7 0.0380(12) 0.0337(11) 0.0367(13) 0.0063(10) -0.0175(10) -0.0153(9) O8 0.0483(13) 0.0405(12) 0.0375(14) 0.0168(10) -0.0217(11) -0.0224(10) O9 0.0339(11) 0.0246(10) 0.0419(14) 0.0029(9) -0.0095(10) -0.0110(9) O10 0.0276(10) 0.0304(11) 0.0431(14) 0.0054(10) 0.0042(9) -0.0031(9) O11 0.0282(10) 0.0276(10) 0.0319(12) 0.0024(9) 0.0066(9) -0.0044(8) O12 0.0225(9) 0.0293(10) 0.0263(11) -0.0004(8) 0.0016(8) -0.0045(8) O13 0.0694(19) 0.0400(14) 0.068(2) 0.0245(13) 0.0266(15) 0.0139(13) O14 0.086(2) 0.0297(12) 0.0618(18) 0.0005(12) -0.0387(15) -0.0132(12) C1 0.0227(13) 0.0228(13) 0.0201(15) -0.0012(11) -0.0047(11) -0.0046(10) C2 0.0213(13) 0.0274(14) 0.0250(16) -0.0026(12) -0.0031(11) -0.0069(11) C3 0.0216(13) 0.0308(15) 0.0269(17) -0.0071(12) -0.0034(11) -0.0029(11) C4 0.0237(14) 0.0273(14) 0.0373(19) -0.0089(13) -0.0059(12) -0.0068(11) C5 0.0206(13) 0.0239(14) 0.0303(17) 0.0007(12) -0.0052(11) -0.0031(11) C6 0.0220(13) 0.0250(14) 0.0232(16) -0.0011(11) -0.0037(11) -0.0031(11) C7 0.0239(14) 0.0253(14) 0.0390(19) 0.0037(13) -0.0070(12) -0.0074(11) C8 0.0206(13) 0.0259(14) 0.0333(18) 0.0016(12) -0.0038(12) -0.0085(11) C9 0.0259(14) 0.0253(14) 0.0418(19) -0.0070(13) -0.0038(13) -0.0072(11) C10 0.0270(14) 0.0315(15) 0.0361(18) -0.0039(13) -0.0092(13) -0.0112(12) C11 0.0228(13) 0.0250(14) 0.0377(19) 0.0032(12) -0.0094(12) -0.0078(11) C12 0.0214(13) 0.0242(13) 0.0271(16) 0.0008(12) -0.0018(11) -0.0073(11) C13 0.0240(13) 0.0282(14) 0.0250(16) -0.0014(12) -0.0051(11) -0.0087(11) C14 0.0211(13) 0.0274(14) 0.0289(17) 0.0007(12) -0.0025(11) -0.0050(11) C15 0.0218(13) 0.0252(14) 0.0209(15) -0.0036(11) -0.0005(11) -0.0046(10) C16 0.0230(13) 0.0265(14) 0.0232(16) -0.0038(12) -0.0033(11) -0.0058(11) C17 0.0288(14) 0.0264(14) 0.0223(16) 0.0001(12) -0.0054(12) -0.0049(11) C18 0.0259(14) 0.0244(14) 0.0234(16) -0.0017(12) -0.0021(11) -0.0077(11) C19 0.0208(13) 0.0259(14) 0.0215(15) -0.0047(11) -0.0009(11) -0.0034(11) C20 0.0230(13) 0.0266(14) 0.0213(16) 0.0001(11) -0.0007(11) -0.0036(11) C21 0.0223(13) 0.0289(14) 0.0233(16) -0.0047(12) -0.0024(11) -0.0058(11) C22 0.0204(13) 0.0303(14) 0.0198(15) -0.0052(12) -0.0025(11) -0.0070(11) C23 0.0252(14) 0.0250(14) 0.0290(17) -0.0031(12) -0.0033(12) -0.0056(11) C24 0.0256(13) 0.0295(15) 0.0218(16) -0.0016(12) -0.0020(11) -0.0105(11) C25 0.0199(13) 0.0271(14) 0.0252(16) -0.0057(12) -0.0024(11) -0.0054(11) C26 0.0214(12) 0.0257(13) 0.0190(15) -0.0031(11) -0.0060(10) -0.0079(10) C27 0.0228(13) 0.0293(14) 0.0201(15) -0.0037(12) -0.0021(11) -0.0100(11) C28 0.0218(13) 0.0293(14) 0.0202(16) -0.0010(12) -0.0029(11) -0.0071(11) C29 0.0285(15) 0.0392(17) 0.040(2) 0.0037(15) -0.0029(14) -0.0068(13) C30 0.0402(19) 0.059(2) 0.043(2) 0.0184(18) -0.0062(16) -0.0054(17) C31 0.049(2) 0.054(2) 0.052(3) 0.0167(19) -0.0075(18) -0.0015(18) C32 0.060(2) 0.051(2) 0.052(3) 0.0096(19) -0.011(2) -0.0102(19) C33 0.055(2) 0.054(2) 0.049(3) 0.0129(19) -0.0053(19) -0.0056(18) C34 0.065(3) 0.055(2) 0.049(3) 0.014(2) -0.004(2) -0.001(2) C35 0.055(2) 0.053(2) 0.049(3) 0.0060(19) -0.0011(19) -0.0036(18) C36 0.063(3) 0.057(2) 0.050(3) 0.008(2) -0.006(2) -0.001(2) C37 0.052(2) 0.055(2) 0.049(3) 0.0049(19) -0.0052(18) -0.0022(18) C38 0.056(2) 0.053(2) 0.054(3) 0.009(2) -0.0086(19) 0.0005(19) C39 0.052(2) 0.059(2) 0.051(3) 0.006(2) -0.0071(19) -0.0034(19) C40 0.071(3) 0.072(3) 0.050(3) 0.005(2) -0.011(2) -0.005(2) C41 0.0310(15) 0.0320(16) 0.0284(18) 0.0003(13) -0.0010(13) -0.0052(12) C42 0.0416(18) 0.0369(17) 0.0300(19) 0.0000(14) 0.0015(14) -0.0056(14) C43 0.0362(17) 0.0371(17) 0.0336(19) -0.0015(14) 0.0038(14) -0.0096(14) C44 0.0414(18) 0.0383(18) 0.0332(19) -0.0030(15) 0.0030(14) -0.0119(14) C45 0.0468(19) 0.0411(18) 0.0307(19) -0.0008(15) 0.0017(15) -0.0114(15) C46 0.049(2) 0.0380(18) 0.032(2) -0.0019(15) 0.0003(15) -0.0102(15) C47 0.052(2) 0.0386(18) 0.036(2) -0.0034(15) 0.0028(16) -0.0122(16) C48 0.055(2) 0.0375(18) 0.034(2) 0.0013(15) 0.0019(16) -0.0104(16) C49 0.059(2) 0.0371(18) 0.038(2) -0.0020(16) 0.0053(17) -0.0140(17) C50 0.060(2) 0.0388(19) 0.035(2) -0.0009(16) 0.0038(17) -0.0097(16) C51 0.065(2) 0.048(2) 0.038(2) -0.0019(17) 0.0102(18) -0.0155(19) C52 0.065(3) 0.074(3) 0.045(2) -0.015(2) 0.012(2) -0.024(2) C53 0.0268(14) 0.0405(17) 0.0269(17) -0.0079(14) -0.0032(12) -0.0058(13) C54 0.0318(16) 0.0406(18) 0.0320(19) -0.0092(14) -0.0002(13) -0.0047(13) C55 0.0364(18) 0.071(3) 0.033(2) -0.0207(18) 0.0000(15) -0.0078(17) C56 0.0359(17) 0.049(2) 0.035(2) -0.0153(16) 0.0012(14) -0.0094(15) C57 0.046(2) 0.083(3) 0.036(2) -0.021(2) 0.0002(17) -0.012(2) C58 0.0415(19) 0.053(2) 0.034(2) -0.0119(16) 0.0008(15) -0.0128(16) C59 0.048(2) 0.085(3) 0.035(2) -0.018(2) 0.0006(17) -0.013(2) C60 0.0446(19) 0.051(2) 0.035(2) -0.0116(16) 0.0012(15) -0.0157(16) C61 0.048(2) 0.082(3) 0.033(2) -0.015(2) -0.0014(17) -0.011(2) C62 0.0429(18) 0.050(2) 0.0312(19) -0.0073(16) -0.0017(15) -0.0143(16) C63 0.053(2) 0.091(3) 0.038(2) -0.010(2) -0.0085(18) -0.007(2) C64 0.057(2) 0.072(3) 0.033(2) -0.0091(19) -0.0016(17) -0.018(2) C65 0.0276(14) 0.0377(16) 0.0232(17) -0.0028(13) -0.0060(12) -0.0073(12) C66 0.0466(19) 0.0419(18) 0.031(2) 0.0049(15) -0.0170(15) -0.0050(15) C67 0.041(4) 0.047(4) 0.033(4) 0.001(3) -0.015(3) -0.007(3) C68 0.038(5) 0.051(5) 0.028(5) 0.005(3) -0.010(4) -0.017(4) C69 0.055(5) 0.054(7) 0.026(5) 0.005(6) -0.018(4) -0.016(5) C70 0.049(5) 0.059(5) 0.026(4) 0.004(3) -0.008(4) -0.019(4) C71 0.064(6) 0.057(8) 0.036(6) 0.006(7) -0.012(4) -0.030(7) C72 0.050(5) 0.052(5) 0.036(5) 0.008(3) -0.009(4) -0.017(4) C73 0.052(5) 0.054(7) 0.039(6) -0.005(7) -0.016(4) -0.018(6) C74 0.040(4) 0.052(5) 0.037(5) 0.002(3) -0.012(4) -0.012(4) C75 0.058(6) 0.050(7) 0.046(6) -0.005(6) -0.011(4) -0.024(6) C76 0.064(7) 0.057(6) 0.033(5) 0.000(4) -0.006(5) -0.012(5) C77 0.047(4) 0.038(4) 0.036(4) 0.002(3) -0.014(3) -0.004(3) C78 0.040(5) 0.043(4) 0.032(5) 0.003(3) -0.007(5) -0.017(4) C79 0.052(5) 0.047(6) 0.032(6) 0.004(5) -0.016(4) -0.017(5) C80 0.052(5) 0.048(4) 0.036(5) 0.000(4) -0.006(4) -0.019(4) C81 0.048(5) 0.045(7) 0.033(6) 0.005(6) -0.011(4) -0.018(5) C82 0.051(5) 0.055(5) 0.033(5) 0.003(4) -0.005(4) -0.020(4) C83 0.051(5) 0.043(6) 0.030(5) -0.001(5) -0.007(3) -0.017(5) C84 0.046(5) 0.045(4) 0.039(5) 0.002(4) -0.008(4) -0.014(4) C85 0.043(4) 0.046(6) 0.033(5) 0.000(5) -0.008(3) -0.017(5) C86 0.055(6) 0.065(6) 0.043(6) -0.003(5) -0.006(5) -0.014(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 O1 C2 1.390(3) . ? O2 C3 1.389(3) . ? O3 C4 1.384(3) . ? O4 C9 1.381(3) . ? O5 C10 1.384(4) . ? O6 C11 1.385(3) . ? O7 C16 1.387(3) . ? O8 C17 1.389(4) . ? O9 C18 1.380(3) . ? O10 C23 1.378(3) . ? O11 C24 1.380(3) . ? O12 C25 1.390(3) . ? O15 C109 1.39(2) . ? O15 C106 1.421(14) . ? O16 C107 1.294(13) . ? O16 C104 1.474(15) . ? O17 C107 1.386(15) . ? O18 C109 1.12(2) . ? O19 C111 1.329(13) . ? O19 C111 1.329(13) 2_656 ? O19 C112 1.427(13) . ? O19 C112 1.427(13) 2_656 ? C1 C6 1.397(4) . ? C1 C2 1.397(4) . ? C1 C28 1.539(4) . ? C2 C3 1.396(4) . ? C3 C4 1.386(4) . ? C4 C5 1.400(4) . ? C5 C6 1.397(4) . ? C5 C7 1.524(4) . ? C7 C29 1.504(5) . ? C7 C8 1.528(4) . ? C8 C13 1.390(4) . ? C8 C9 1.397(4) . ? C9 C10 1.384(4) . ? C10 C11 1.390(4) . ? C11 C12 1.392(4) . ? C12 C13 1.398(4) . ? C12 C14 1.528(4) . ? C14 C41 1.514(4) . ? C14 C15 1.530(4) . ? C15 C16 1.390(4) . ? C15 C20 1.398(4) . ? C16 C17 1.386(4) . ? C17 C18 1.390(4) . ? C18 C19 1.398(4) . ? C19 C20 1.398(4) . ? C19 C21 1.532(4) . ? C21 C53 1.531(4) . ? C21 C22 1.539(4) . ? C22 C23 1.396(4) . ? C22 C27 1.399(4) . ? C23 C24 1.394(4) . ? C24 C25 1.383(4) . ? C25 C26 1.398(4) . ? C26 C27 1.398(4) . ? C26 C28 1.530(4) . ? C28 C65 1.531(4) . ? C29 C30 1.542(5) . ? C30 C31 1.526(5) . ? C31 C32 1.500(6) . ? C32 C33 1.532(6) . ? C33 C34 1.508(6) . ? C34 C35 1.522(6) . ? C35 C36 1.513(6) . ? C36 C37 1.517(6) . ? C37 C38 1.510(6) . ? C38 C39 1.524(6) . ? C39 C40 1.501(6) . ? C41 C42 1.529(4) . ? C42 C43 1.518(5) . ? C43 C44 1.510(4) . ? C44 C45 1.528(5) . ? C45 C46 1.521(5) . ? C46 C47 1.524(5) . ? C47 C48 1.529(5) . ? C48 C49 1.519(5) . ? C49 C50 1.522(5) . ? C50 C51 1.514(5) . ? C51 C52 1.525(5) . ? C53 C54 1.529(4) . ? C54 C55 1.507(5) . ? C55 C56 1.520(4) . ? C56 C57 1.514(5) . ? C57 C58 1.506(5) . ? C58 C59 1.511(5) . ? C59 C60 1.514(5) . ? C60 C61 1.512(5) . ? C61 C62 1.516(5) . ? C62 C63 1.505(5) . ? C63 C64 1.506(5) . ? C65 C66 1.542(4) . ? C66 C77 1.481(8) . ? C66 C67 1.578(8) . ? C67 C68 1.529(11) . ? C68 C69 1.527(14) . ? C69 C70 1.498(15) . ? C70 C71 1.528(16) . ? C71 C72 1.524(18) . ? C72 C73 1.517(15) . ? C73 C74 1.503(16) . ? C74 C75 1.532(14) . ? C75 C76 1.512(17) . ? C77 C78 1.508(11) . ? C78 C79 1.516(15) . ? C79 C80 1.523(13) . ? C80 C81 1.521(17) . ? C81 C82 1.520(14) . ? C82 C83 1.505(15) . ? C83 C84 1.527(13) . ? C84 C85 1.520(14) . ? C85 C86 1.519(15) . ? C103 C104 1.371(15) . ? C105 C106 1.560(13) . ? C107 C108 1.451(16) . ? C109 C110 1.46(2) . ? C111 O20 1.206(17) . ? C111 C113 1.321(16) . ? C112 C113 1.268(16) . ? 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 C109 O15 C106 117.5(10) . . ? C107 O16 C104 117.3(8) . . ? C111 O19 C111 180.0(11) . 2_656 ? C111 O19 C112 61.4(8) . . ? C111 O19 C112 118.6(8) 2_656 . ? C111 O19 C112 118.6(8) . 2_656 ? C111 O19 C112 61.4(8) 2_656 2_656 ? C112 O19 C112 179.999(3) . 2_656 ? C6 C1 C2 117.3(2) . . ? C6 C1 C28 121.6(2) . . ? C2 C1 C28 121.1(2) . . ? O1 C2 C3 115.0(2) . . ? O1 C2 C1 124.2(2) . . ? C3 C2 C1 120.8(2) . . ? C4 C3 O2 117.7(2) . . ? C4 C3 C2 120.2(3) . . ? O2 C3 C2 122.1(3) . . ? O3 C4 C3 117.4(3) . . ? O3 C4 C5 121.6(3) . . ? C3 C4 C5 121.0(2) . . ? C6 C5 C4 117.1(3) . . ? C6 C5 C7 123.0(3) . . ? C4 C5 C7 119.9(2) . . ? C1 C6 C5 123.5(3) . . ? C29 C7 C5 114.5(3) . . ? C29 C7 C8 112.3(2) . . ? C5 C7 C8 111.8(2) . . ? C13 C8 C9 117.7(3) . . ? C13 C8 C7 122.3(3) . . ? C9 C8 C7 120.0(3) . . ? O4 C9 C10 119.1(3) . . ? O4 C9 C8 120.1(3) . . ? C10 C9 C8 120.8(3) . . ? O5 C10 C9 117.9(3) . . ? O5 C10 C11 122.0(3) . . ? C9 C10 C11 120.2(3) . . ? O6 C11 C12 124.1(3) . . ? O6 C11 C10 115.0(3) . . ? C12 C11 C10 120.9(3) . . ? C11 C12 C13 117.5(3) . . ? C11 C12 C14 121.1(2) . . ? C13 C12 C14 121.4(3) . . ? C8 C13 C12 123.0(3) . . ? C41 C14 C12 111.2(2) . . ? C41 C14 C15 114.8(2) . . ? C12 C14 C15 112.4(2) . . ? C16 C15 C20 117.5(3) . . ? C16 C15 C14 119.6(2) . . ? C20 C15 C14 122.9(3) . . ? C17 C16 C15 121.0(3) . . ? C17 C16 O7 120.1(3) . . ? C15 C16 O7 118.9(2) . . ? C16 C17 O8 120.7(3) . . ? C16 C17 C18 120.2(3) . . ? O8 C17 C18 119.0(2) . . ? O9 C18 C17 119.8(3) . . ? O9 C18 C19 119.3(2) . . ? C17 C18 C19 120.9(3) . . ? C20 C19 C18 117.2(3) . . ? C20 C19 C21 123.2(3) . . ? C18 C19 C21 119.6(2) . . ? C19 C20 C15 123.2(3) . . ? C53 C21 C19 114.4(2) . . ? C53 C21 C22 112.8(2) . . ? C19 C21 C22 110.3(2) . . ? C23 C22 C27 117.6(2) . . ? C23 C22 C21 121.0(3) . . ? C27 C22 C21 121.4(3) . . ? O10 C23 C24 115.4(3) . . ? O10 C23 C22 124.4(2) . . ? C24 C23 C22 120.2(3) . . ? O11 C24 C25 117.0(2) . . ? O11 C24 C23 122.3(3) . . ? C25 C24 C23 120.7(3) . . ? C24 C25 O12 119.2(3) . . ? C24 C25 C26 121.2(2) . . ? O12 C25 C26 119.6(2) . . ? C25 C26 C27 116.8(3) . . ? C25 C26 C28 120.5(2) . . ? C27 C26 C28 122.7(3) . . ? C26 C27 C22 123.5(3) . . ? C65 C28 C26 111.8(2) . . ? C65 C28 C1 113.6(2) . . ? C26 C28 C1 110.7(2) . . ? C7 C29 C30 113.9(3) . . ? C31 C30 C29 112.4(3) . . ? C32 C31 C30 113.2(3) . . ? C31 C32 C33 115.1(3) . . ? C34 C33 C32 113.0(3) . . ? C33 C34 C35 114.7(4) . . ? C36 C35 C34 113.6(4) . . ? C35 C36 C37 114.8(4) . . ? C38 C37 C36 114.6(4) . . ? C37 C38 C39 115.3(4) . . ? C40 C39 C38 113.7(4) . . ? C14 C41 C42 115.9(3) . . ? C43 C42 C41 112.3(3) . . ? C44 C43 C42 114.7(3) . . ? C43 C44 C45 113.3(3) . . ? C46 C45 C44 114.5(3) . . ? C45 C46 C47 113.7(3) . . ? C46 C47 C48 114.1(3) . . ? C49 C48 C47 114.0(3) . . ? C48 C49 C50 114.4(3) . . ? C51 C50 C49 114.1(3) . . ? C50 C51 C52 114.4(3) . . ? C54 C53 C21 114.5(3) . . ? C55 C54 C53 113.1(3) . . ? C54 C55 C56 115.2(3) . . ? C57 C56 C55 114.5(3) . . ? C58 C57 C56 115.3(3) . . ? C57 C58 C59 115.5(3) . . ? C58 C59 C60 115.4(3) . . ? C61 C60 C59 116.0(3) . . ? C60 C61 C62 114.6(3) . . ? C63 C62 C61 116.5(3) . . ? C64 C63 C62 114.7(3) . . ? C28 C65 C66 113.8(2) . . ? C77 C66 C65 118.4(4) . . ? C77 C66 C67 36.3(4) . . ? C65 C66 C67 108.8(4) . . ? C68 C67 C66 118.8(6) . . ? C69 C68 C67 114.2(8) . . ? C70 C69 C68 114.9(9) . . ? C69 C70 C71 114.7(10) . . ? C70 C71 C72 114.7(11) . . ? C73 C72 C71 115.0(10) . . ? C74 C73 C72 115.7(9) . . ? C73 C74 C75 114.3(9) . . ? C76 C75 C74 113.8(9) . . ? C66 C77 C78 113.8(6) . . ? C77 C78 C79 114.9(7) . . ? C78 C79 C80 115.3(8) . . ? C79 C80 C81 115.7(8) . . ? C82 C81 C80 114.8(8) . . ? C83 C82 C81 114.9(8) . . ? C82 C83 C84 114.5(8) . . ? C85 C84 C83 115.3(8) . . ? C86 C85 C84 113.8(8) . . ? C103 C104 O16 112.8(11) . . ? O15 C106 C105 103.8(9) . . ? O16 C107 O17 123.4(8) . . ? O16 C107 C108 118.9(10) . . ? O17 C107 C108 117.6(10) . . ? O18 C109 O15 111.3(16) . . ? O18 C109 C110 118.9(17) . . ? O15 C109 C110 123.4(15) . . ? O20 C111 C113 125.6(13) . . ? O20 C111 O19 113.5(12) . . ? C113 C111 O19 117.8(11) . . ? C113 C112 O19 114.6(10) . . ? C112 C113 C111 66.0(9) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.886 _refine_diff_density_max 1.420 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.073 # Attachment '3.cif' data_C13EtOAc _database_code_depnum_ccdc_archive 'CCDC 648031' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H151.50 O18.75' _chemical_formula_weight 1545.62 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' O O 0.0106 0.0060 '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 11.758(4) _cell_length_b 13.555(4) _cell_length_c 30.524(10) _cell_angle_alpha 93.394(6) _cell_angle_beta 95.176(6) _cell_angle_gamma 108.457(5) _cell_volume 4576(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1695 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9774 _exptl_absorpt_correction_T_max 0.9856 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 SMART 1000 CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30900 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.17 _reflns_number_total 19175 _reflns_number_gt 10404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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^)+(0.1326P)^2^+1.0739P] 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 19175 _refine_ls_number_parameters 1020 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1556 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2619 _refine_ls_wR_factor_gt 0.2215 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.6992(2) 0.80379(17) 0.36560(8) 0.0298(6) Uani 1 1 d . . . H300 H -0.7184 0.8489 0.3806 0.036 Uiso 1 1 calc R . . O2 O -0.6058(2) 1.01393(18) 0.37566(8) 0.0355(6) Uani 1 1 d . . . H301 H -0.5621 1.0768 0.3804 0.043 Uiso 1 1 calc R . . O3 O -0.4152(2) 1.11856(17) 0.33348(8) 0.0314(6) Uani 1 1 d . . . H302 H -0.3411 1.1409 0.3309 0.038 Uiso 1 1 calc R . . O4 O -0.1692(2) 1.19497(17) 0.32616(8) 0.0290(6) Uani 1 1 d . . . H303 H -0.1257 1.2450 0.3440 0.035 Uiso 1 1 calc R . . O5 O 0.0329(2) 1.21498(18) 0.38092(8) 0.0369(6) Uani 1 1 d . . . H304 H 0.1032 1.2191 0.3911 0.044 Uiso 1 1 calc R . . O6 O 0.1357(2) 1.06285(17) 0.38292(8) 0.0325(6) Uani 1 1 d . . . H305 H 0.1385 1.0083 0.3940 0.039 Uiso 1 1 calc R . . O7 O 0.15203(19) 0.87524(16) 0.41175(7) 0.0249(5) Uani 1 1 d . . . H306 H 0.1604 0.8895 0.4393 0.030 Uiso 1 1 calc R . . O8 O 0.0761(2) 0.72599(18) 0.46849(7) 0.0304(6) Uani 1 1 d . . . H307 H 0.0435 0.6763 0.4832 0.036 Uiso 1 1 calc R . . O9 O -0.1279(2) 0.56101(17) 0.44790(7) 0.0297(6) Uani 1 1 d . . . H308 H -0.2029 0.5311 0.4450 0.036 Uiso 1 1 calc R . . O10 O -0.3816(2) 0.49131(18) 0.44205(7) 0.0299(6) Uani 1 1 d . . . H309 H -0.4189 0.4848 0.4645 0.036 Uiso 1 1 calc R . . O11 O -0.5781(2) 0.54095(18) 0.45974(7) 0.0305(6) Uani 1 1 d . . . H310 H -0.6396 0.5590 0.4618 0.037 Uiso 1 1 calc R . . O12 O -0.6961(2) 0.62758(18) 0.39917(8) 0.0307(6) Uani 1 1 d . . . H311 H -0.6937 0.6872 0.3922 0.037 Uiso 1 1 calc R . . O13 O -0.0713(2) 0.38332(17) 0.38622(7) 0.0258(5) Uani 1 1 d . . . O14 O -0.0090(2) 0.38208(18) 0.45786(8) 0.0315(6) Uani 1 1 d . . . O15 O -0.5600(4) 0.2189(4) 0.4079(2) 0.0591(13) Uani 0.70 1 d P A 2 O16 O -0.7106(6) 0.2776(4) 0.42398(19) 0.0381(12) Uani 0.70 1 d P A 2 O17 O -0.5822(11) 0.2426(9) 0.4287(4) 0.053(3) Uiso 0.30 1 d P B 1 O18 O -0.7538(12) 0.2796(12) 0.4299(5) 0.047(5) Uiso 0.30 1 d P B 1 O19 O 0.2124(2) 0.55979(19) 0.48124(8) 0.0319(6) Uani 1 1 d . . . C1 C -0.5579(3) 0.7925(2) 0.31584(11) 0.0221(7) Uani 1 1 d . . . C2 C -0.6030(3) 0.8532(3) 0.34273(11) 0.0226(7) Uani 1 1 d . . . C3 C -0.5541(3) 0.9614(3) 0.34814(11) 0.0245(7) Uani 1 1 d . . . C4 C -0.4567(3) 1.0110(2) 0.32565(11) 0.0242(7) Uani 1 1 d . . . C5 C -0.4087(3) 0.9538(2) 0.29741(10) 0.0213(7) Uani 1 1 d . . . C6 C -0.4604(3) 0.8448(2) 0.29360(11) 0.0223(7) Uani 1 1 d . . . H6 H -0.4277 0.8045 0.2751 0.027 Uiso 1 1 calc R . . C7 C -0.3022(3) 1.0077(3) 0.27228(10) 0.0231(7) Uani 1 1 d . . . H7 H -0.3053 1.0793 0.2676 0.028 Uiso 1 1 calc R . . C8 C -0.1827(3) 1.0207(2) 0.30050(10) 0.0209(7) Uani 1 1 d . . . C9 C -0.1225(3) 1.1130(2) 0.32706(10) 0.0218(7) Uani 1 1 d . . . C10 C -0.0193(3) 1.1226(2) 0.35498(11) 0.0254(8) Uani 1 1 d . . . C11 C 0.0304(3) 1.0412(2) 0.35546(11) 0.0239(7) Uani 1 1 d . . . C12 C -0.0249(3) 0.9488(2) 0.32761(10) 0.0214(7) Uani 1 1 d . . . C13 C -0.1316(3) 0.9407(2) 0.30177(10) 0.0217(7) Uani 1 1 d . . . H13 H -0.1721 0.8772 0.2840 0.026 Uiso 1 1 calc R . . C14 C 0.0330(3) 0.8627(2) 0.32485(10) 0.0219(7) Uani 1 1 d . . . H14 H 0.1214 0.8968 0.3341 0.026 Uiso 1 1 calc R . . C15 C -0.0129(3) 0.7818(2) 0.35725(10) 0.0197(7) Uani 1 1 d . . . C16 C 0.0477(3) 0.7904(2) 0.39942(11) 0.0212(7) Uani 1 1 d . . . C17 C 0.0079(3) 0.7151(2) 0.42854(10) 0.0227(7) Uani 1 1 d . . . C18 C -0.0985(3) 0.6312(2) 0.41645(11) 0.0218(7) Uani 1 1 d . . . C19 C -0.1625(3) 0.6193(2) 0.37477(11) 0.0209(7) Uani 1 1 d . . . C20 C -0.1181(3) 0.6962(2) 0.34637(11) 0.0222(7) Uani 1 1 d . . . H20 H -0.1618 0.6900 0.3181 0.027 Uiso 1 1 calc R . . C21 C -0.2764(3) 0.5260(2) 0.36145(10) 0.0220(7) Uani 1 1 d . . . H21 H -0.2717 0.4708 0.3812 0.026 Uiso 1 1 calc R . . C22 C -0.3895(3) 0.5528(2) 0.37017(10) 0.0214(7) Uani 1 1 d . . . C23 C -0.4375(3) 0.5355(2) 0.41036(10) 0.0225(7) Uani 1 1 d . . . C24 C -0.5388(3) 0.5613(2) 0.41906(11) 0.0240(7) Uani 1 1 d . . . C25 C -0.5954(3) 0.6064(2) 0.38745(11) 0.0231(7) Uani 1 1 d . . . C26 C -0.5504(3) 0.6245(2) 0.34670(10) 0.0206(7) Uani 1 1 d . . . C27 C -0.4482(3) 0.5986(2) 0.33941(10) 0.0219(7) Uani 1 1 d . . . H27 H -0.4161 0.6127 0.3121 0.026 Uiso 1 1 calc R . . C28 C -0.6123(3) 0.6730(2) 0.31112(10) 0.0228(7) Uani 1 1 d . . . H28 H -0.6984 0.6561 0.3170 0.027 Uiso 1 1 calc R . . C29 C -0.3119(3) 0.9503(3) 0.22670(11) 0.0266(8) Uani 1 1 d . . . H29A H -0.3959 0.9324 0.2126 0.032 Uiso 1 1 calc R . . H29B H -0.2954 0.8840 0.2307 0.032 Uiso 1 1 calc R . . C30 C -0.2265(3) 1.0114(3) 0.19531(12) 0.0329(9) Uani 1 1 d . . . H30A H -0.2517 1.0714 0.1867 0.040 Uiso 1 1 calc R . . H30B H -0.1436 1.0393 0.2108 0.040 Uiso 1 1 calc R . . C31 C -0.2268(4) 0.9432(3) 0.15424(12) 0.0351(9) Uani 1 1 d . . . H31A H -0.3089 0.8924 0.1467 0.042 Uiso 1 1 calc R . . H31B H -0.1714 0.9030 0.1612 0.042 Uiso 1 1 calc R . . C32 C -0.1901(3) 1.0003(3) 0.11373(12) 0.0330(8) Uani 1 1 d . . . H32A H -0.2440 1.0419 0.1069 0.040 Uiso 1 1 calc R . . H32B H -0.1068 1.0494 0.1206 0.040 Uiso 1 1 calc R . . C33 C -0.1953(4) 0.9281(3) 0.07318(12) 0.0339(9) Uani 1 1 d . . . H33A H -0.2742 0.8716 0.0693 0.041 Uiso 1 1 calc R . . H33B H -0.1315 0.8955 0.0781 0.041 Uiso 1 1 calc R . . C34 C -0.1793(3) 0.9830(3) 0.03097(12) 0.0332(9) Uani 1 1 d . . . H34A H -0.1002 1.0392 0.0348 0.040 Uiso 1 1 calc R . . H34B H -0.2428 1.0160 0.0262 0.040 Uiso 1 1 calc R . . C35 C -0.1854(4) 0.9104(3) -0.01005(12) 0.0349(9) Uani 1 1 d . . . H35A H -0.1203 0.8789 -0.0056 0.042 Uiso 1 1 calc R . . H35B H -0.2635 0.8530 -0.0134 0.042 Uiso 1 1 calc R . . C36 C -0.1728(4) 0.9648(3) -0.05252(12) 0.0348(9) Uani 1 1 d . . . H36A H -0.2385 0.9955 -0.0573 0.042 Uiso 1 1 calc R . . H36B H -0.0951 1.0228 -0.0491 0.042 Uiso 1 1 calc R . . C37 C -0.1773(4) 0.8922(3) -0.09288(12) 0.0344(9) Uani 1 1 d . . . H37A H -0.1120 0.8612 -0.0879 0.041 Uiso 1 1 calc R . . H37B H -0.2551 0.8345 -0.0962 0.041 Uiso 1 1 calc R . . C38 C -0.1643(4) 0.9446(3) -0.13543(12) 0.0367(9) Uani 1 1 d . . . H38A H -0.0877 1.0037 -0.1319 0.044 Uiso 1 1 calc R . . H38B H -0.2312 0.9734 -0.1411 0.044 Uiso 1 1 calc R . . C39 C -0.1650(4) 0.8715(3) -0.17521(12) 0.0389(9) Uani 1 1 d . . . H39A H -0.1000 0.8406 -0.1689 0.047 Uiso 1 1 calc R . . H39B H -0.2427 0.8136 -0.1791 0.047 Uiso 1 1 calc R . . C40 C -0.1481(5) 0.9211(4) -0.21811(14) 0.0613(14) Uani 1 1 d . . . H40A H -0.2160 0.9475 -0.2259 0.074 Uiso 1 1 calc R . . H40B H -0.0727 0.9815 -0.2141 0.074 Uiso 1 1 calc R . . C41 C -0.1418(6) 0.8464(5) -0.25543(18) 0.102(2) Uani 1 1 d . . . H41A H -0.0677 0.8283 -0.2500 0.154 Uiso 1 1 calc R . . H41B H -0.1417 0.8792 -0.2832 0.154 Uiso 1 1 calc R . . H41C H -0.2119 0.7828 -0.2574 0.154 Uiso 1 1 calc R . . C42 C 0.0200(3) 0.8142(3) 0.27694(11) 0.0251(7) Uani 1 1 d . . . H42A H -0.0651 0.7703 0.2685 0.030 Uiso 1 1 calc R . . H42B H 0.0387 0.8711 0.2572 0.030 Uiso 1 1 calc R . . C43 C 0.1009(3) 0.7478(3) 0.26951(12) 0.0325(8) Uani 1 1 d . . . H43A H 0.0949 0.7002 0.2932 0.039 Uiso 1 1 calc R . . H43B H 0.1857 0.7942 0.2717 0.039 Uiso 1 1 calc R . . C44 C 0.0690(4) 0.6829(3) 0.22487(12) 0.0342(9) Uani 1 1 d . . . H44A H -0.0139 0.6333 0.2238 0.041 Uiso 1 1 calc R . . H44B H 0.1242 0.6412 0.2229 0.041 Uiso 1 1 calc R . . C45 C 0.0754(4) 0.7450(3) 0.18421(12) 0.0351(9) Uani 1 1 d . . . H45A H 0.0120 0.7787 0.1834 0.042 Uiso 1 1 calc R . . H45B H 0.1546 0.8009 0.1868 0.042 Uiso 1 1 calc R . . C46 C 0.0590(4) 0.6766(3) 0.14123(12) 0.0379(9) Uani 1 1 d . . . H46A H 0.1242 0.6449 0.1420 0.046 Uiso 1 1 calc R . . H46B H -0.0186 0.6190 0.1396 0.046 Uiso 1 1 calc R . . C47 C 0.0597(4) 0.7326(3) 0.09956(12) 0.0364(9) Uani 1 1 d . . . H47A H 0.1347 0.7932 0.1019 0.044 Uiso 1 1 calc R . . H47B H -0.0093 0.7598 0.0974 0.044 Uiso 1 1 calc R . . C48 C 0.0519(4) 0.6634(3) 0.05743(12) 0.0363(9) Uani 1 1 d . . . H48A H 0.1175 0.6323 0.0606 0.044 Uiso 1 1 calc R . . H48B H -0.0257 0.6055 0.0543 0.044 Uiso 1 1 calc R . . C49 C 0.0608(4) 0.7187(3) 0.01531(12) 0.0357(9) Uani 1 1 d . . . H49A H -0.0067 0.7476 0.0114 0.043 Uiso 1 1 calc R . . H49B H 0.1370 0.7782 0.0188 0.043 Uiso 1 1 calc R . . C50 C 0.0572(4) 0.6496(3) -0.02602(12) 0.0352(9) Uani 1 1 d . . . H50A H -0.0199 0.5910 -0.0299 0.042 Uiso 1 1 calc R . . H50B H 0.1235 0.6195 -0.0219 0.042 Uiso 1 1 calc R . . C51 C 0.0689(4) 0.7056(3) -0.06796(12) 0.0405(10) Uani 1 1 d . . . H51A H 0.1463 0.7639 -0.0640 0.049 Uiso 1 1 calc R . . H51B H 0.0031 0.7365 -0.0718 0.049 Uiso 1 1 calc R . . C52 C 0.0644(4) 0.6377(3) -0.11023(12) 0.0375(9) Uani 1 1 d . . . H52A H 0.1285 0.6051 -0.1062 0.045 Uiso 1 1 calc R . . H52B H -0.0141 0.5808 -0.1148 0.045 Uiso 1 1 calc R . . C53 C 0.0798(5) 0.6947(4) -0.15091(14) 0.0559(12) Uani 1 1 d . . . H53A H 0.1592 0.7505 -0.1466 0.067 Uiso 1 1 calc R . . H53B H 0.0170 0.7288 -0.1544 0.067 Uiso 1 1 calc R . . C54 C 0.0724(5) 0.6273(4) -0.19335(14) 0.0593(13) Uani 1 1 d . . . H54A H 0.1357 0.5946 -0.1907 0.089 Uiso 1 1 calc R . . H54B H 0.0834 0.6709 -0.2181 0.089 Uiso 1 1 calc R . . H54C H -0.0068 0.5729 -0.1986 0.089 Uiso 1 1 calc R . . C55 C -0.6140(3) 0.6256(3) 0.26425(11) 0.0254(8) Uani 1 1 d . . . H55A H -0.5303 0.6323 0.2587 0.030 Uiso 1 1 calc R . . H55B H -0.6451 0.6657 0.2429 0.030 Uiso 1 1 calc R . . C56 C -0.6921(3) 0.5097(3) 0.25609(12) 0.0317(8) Uani 1 1 d . . . H56A H -0.6756 0.4732 0.2818 0.038 Uiso 1 1 calc R . . H56B H -0.7782 0.5048 0.2538 0.038 Uiso 1 1 calc R . . C57 C -0.6697(4) 0.4544(3) 0.21455(12) 0.0363(9) Uani 1 1 d . . . H57A H -0.7224 0.3806 0.2120 0.044 Uiso 1 1 calc R . . H57B H -0.5851 0.4547 0.2181 0.044 Uiso 1 1 calc R . . C58 C -0.6918(4) 0.5009(3) 0.17138(12) 0.0348(9) Uani 1 1 d . . . H58A H -0.7718 0.5110 0.1697 0.042 Uiso 1 1 calc R . . H58B H -0.6300 0.5704 0.1715 0.042 Uiso 1 1 calc R . . C59 C -0.6872(4) 0.4321(3) 0.13045(12) 0.0391(10) Uani 1 1 d . . . H59A H -0.6118 0.4142 0.1342 0.047 Uiso 1 1 calc R . . H59B H -0.7557 0.3661 0.1284 0.047 Uiso 1 1 calc R . . C60 C -0.6926(4) 0.4819(3) 0.08747(12) 0.0363(9) Uani 1 1 d . . . H60A H -0.7662 0.5028 0.0844 0.044 Uiso 1 1 calc R . . H60B H -0.6220 0.5462 0.0889 0.044 Uiso 1 1 calc R . . C61 C -0.6937(4) 0.4119(3) 0.04681(12) 0.0381(9) Uani 1 1 d . . . H61A H -0.7670 0.3496 0.0444 0.046 Uiso 1 1 calc R . . H61B H -0.6228 0.3874 0.0507 0.046 Uiso 1 1 calc R . . C62 C -0.6915(4) 0.4639(3) 0.00362(12) 0.0380(9) Uani 1 1 d . . . H62A H -0.7624 0.4884 -0.0003 0.046 Uiso 1 1 calc R . . H62B H -0.6182 0.5260 0.0060 0.046 Uiso 1 1 calc R . . C63 C -0.6929(4) 0.3936(3) -0.03705(12) 0.0375(9) Uani 1 1 d . . . H63A H -0.6228 0.3682 -0.0329 0.045 Uiso 1 1 calc R . . H63B H -0.7669 0.3320 -0.0397 0.045 Uiso 1 1 calc R . . C64 C -0.6888(4) 0.4451(3) -0.07969(13) 0.0412(10) Uani 1 1 d . . . H64A H -0.6145 0.5064 -0.0772 0.049 Uiso 1 1 calc R . . H64B H -0.7586 0.4710 -0.0838 0.049 Uiso 1 1 calc R . . C65 C -0.6911(4) 0.3736(3) -0.12050(12) 0.0379(9) Uani 1 1 d . . . H65A H -0.6223 0.3466 -0.1160 0.045 Uiso 1 1 calc R . . H65B H -0.7662 0.3130 -0.1232 0.045 Uiso 1 1 calc R . . C66 C -0.6847(4) 0.4236(3) -0.16321(13) 0.0492(11) Uani 1 1 d . . . H66A H -0.6092 0.4837 -0.1609 0.059 Uiso 1 1 calc R . . H66B H -0.7532 0.4508 -0.1679 0.059 Uiso 1 1 calc R . . C67 C -0.6881(4) 0.3496(4) -0.20274(14) 0.0568(12) Uani 1 1 d . . . H67A H -0.6185 0.3245 -0.1989 0.085 Uiso 1 1 calc R . . H67B H -0.6851 0.3861 -0.2296 0.085 Uiso 1 1 calc R . . H67C H -0.7628 0.2900 -0.2054 0.085 Uiso 1 1 calc R . . C68 C -0.2796(3) 0.4796(3) 0.31373(11) 0.0264(8) Uani 1 1 d . . . H68A H -0.2819 0.5333 0.2933 0.032 Uiso 1 1 calc R . . H68B H -0.2040 0.4634 0.3111 0.032 Uiso 1 1 calc R . . C69 C -0.3870(3) 0.3805(3) 0.29887(12) 0.0303(8) Uani 1 1 d . . . H69A H -0.3921 0.3303 0.3215 0.036 Uiso 1 1 calc R . . H69B H -0.4623 0.3988 0.2970 0.036 Uiso 1 1 calc R . . C70 C -0.3778(3) 0.3281(3) 0.25432(13) 0.0359(9) Uani 1 1 d . . . H70A H -0.3651 0.3802 0.2323 0.043 Uiso 1 1 calc R . . H70B H -0.3066 0.3039 0.2570 0.043 Uiso 1 1 calc R . . C71 C -0.4887(4) 0.2362(3) 0.23774(13) 0.0409(10) Uani 1 1 d . . . H71A H -0.5580 0.2621 0.2321 0.049 Uiso 1 1 calc R . . H71B H -0.5066 0.1883 0.2613 0.049 Uiso 1 1 calc R . . C72 C -0.4780(4) 0.1739(3) 0.19549(14) 0.0487(11) Uani 1 1 d . . . H72A H -0.4076 0.1492 0.2009 0.058 Uiso 1 1 calc R . . H72B H -0.5509 0.1114 0.1893 0.058 Uiso 1 1 calc R . . C73 C -0.4638(4) 0.2341(3) 0.15464(13) 0.0441(10) Uani 1 1 d . . . H73A H -0.3873 0.2932 0.1597 0.053 Uiso 1 1 calc R . . H73B H -0.5307 0.2634 0.1503 0.053 Uiso 1 1 calc R . . C74 C -0.4635(4) 0.1671(3) 0.11260(13) 0.0467(11) Uani 1 1 d . . . H74A H -0.3976 0.1367 0.1173 0.056 Uiso 1 1 calc R . . H74B H -0.5406 0.1085 0.1075 0.056 Uiso 1 1 calc R . . C75 C -0.4477(4) 0.2253(3) 0.07140(14) 0.0448(10) Uani 1 1 d . . . H75A H -0.3700 0.2832 0.0762 0.054 Uiso 1 1 calc R . . H75B H -0.5130 0.2564 0.0669 0.054 Uiso 1 1 calc R . . C76 C -0.4492(4) 0.1567(3) 0.02932(14) 0.0452(10) Uani 1 1 d . . . H76A H -0.3839 0.1256 0.0339 0.054 Uiso 1 1 calc R . . H76B H -0.5268 0.0987 0.0246 0.054 Uiso 1 1 calc R . . C77 C -0.4334(4) 0.2139(3) -0.01205(14) 0.0449(10) Uani 1 1 d . . . H77A H -0.4999 0.2435 -0.0170 0.054 Uiso 1 1 calc R . . H77B H -0.3568 0.2730 -0.0070 0.054 Uiso 1 1 calc R . . C78 C -0.4319(4) 0.1476(3) -0.05321(14) 0.0438(10) Uani 1 1 d . . . H78A H -0.5088 0.0890 -0.0584 0.053 Uiso 1 1 calc R . . H78B H -0.3660 0.1174 -0.0481 0.053 Uiso 1 1 calc R . . C79 C -0.4148(4) 0.2049(3) -0.09461(15) 0.0492(11) Uani 1 1 d . . . H79A H -0.4820 0.2334 -0.1003 0.059 Uiso 1 1 calc R . . H79B H -0.3389 0.2646 -0.0893 0.059 Uiso 1 1 calc R . . C80 C -0.4102(4) 0.1378(4) -0.13528(15) 0.0573(12) Uani 1 1 d . . . H80A H -0.3438 0.1093 -0.1300 0.086 Uiso 1 1 calc R . . H80B H -0.3972 0.1803 -0.1604 0.086 Uiso 1 1 calc R . . H80C H -0.4866 0.0804 -0.1418 0.086 Uiso 1 1 calc R . . C81 C 0.0601(4) 0.4538(4) 0.33212(13) 0.0471(11) Uani 1 1 d . . . H81A H 0.0425 0.3823 0.3188 0.071 Uiso 1 1 calc R . . H81B H 0.1422 0.4956 0.3275 0.071 Uiso 1 1 calc R . . H81C H 0.0023 0.4845 0.3183 0.071 Uiso 1 1 calc R . . C82 C 0.0497(3) 0.4524(3) 0.38047(11) 0.0280(8) Uani 1 1 d . . . H82A H 0.1118 0.4265 0.3951 0.034 Uiso 1 1 calc R . . H82B H 0.0620 0.5239 0.3939 0.034 Uiso 1 1 calc R . . C83 C -0.0880(3) 0.3543(3) 0.42723(11) 0.0245(7) Uani 1 1 d . . . C84 C -0.2136(3) 0.2832(3) 0.42973(13) 0.0378(9) Uani 1 1 d . . . H84A H -0.2129 0.2113 0.4310 0.057 Uiso 1 1 calc R . . H84B H -0.2661 0.2871 0.4035 0.057 Uiso 1 1 calc R . . H84C H -0.2438 0.3047 0.4563 0.057 Uiso 1 1 calc R . . C85 C -0.6662(10) 0.2953(9) 0.3555(4) 0.064(3) Uani 0.70 1 d P A 2 H85A H -0.6172 0.3688 0.3556 0.096 Uiso 0.70 1 calc PR A 2 H85B H -0.7520 0.2892 0.3522 0.096 Uiso 0.70 1 calc PR A 2 H85C H -0.6496 0.2543 0.3308 0.096 Uiso 0.70 1 calc PR A 2 C86 C -0.6367(7) 0.2563(5) 0.3968(3) 0.047(2) Uani 0.70 1 d P A 2 C87 C -0.6959(6) 0.2490(5) 0.46915(19) 0.0462(15) Uani 0.70 1 d P A 2 H87A H -0.6160 0.2915 0.4845 0.055 Uiso 0.70 1 calc PR A 2 H87B H -0.7027 0.1743 0.4689 0.055 Uiso 0.70 1 calc PR A 2 C88 C -0.7938(8) 0.2697(7) 0.4915(2) 0.081(3) Uani 0.70 1 d P A 2 H88A H -0.7876 0.3433 0.4904 0.121 Uiso 0.70 1 calc PR A 2 H88B H -0.7863 0.2542 0.5224 0.121 Uiso 0.70 1 calc PR A 2 H88C H -0.8721 0.2254 0.4765 0.121 Uiso 0.70 1 calc PR A 2 C89 C -0.4653(18) 0.1932(16) 0.4925(7) 0.088(6) Uiso 0.30 1 d P B 1 H89A H -0.4684 0.1249 0.4789 0.132 Uiso 0.30 1 calc PR B 1 H89B H -0.4583 0.1926 0.5247 0.132 Uiso 0.30 1 calc PR B 1 H89C H -0.3952 0.2473 0.4841 0.132 Uiso 0.30 1 calc PR B 1 C90 C -0.5925(15) 0.2183(13) 0.4748(5) 0.062(4) Uiso 0.30 1 d P B 1 H90A H -0.6644 0.1568 0.4766 0.074 Uiso 0.30 1 calc PR B 1 H90B H -0.5998 0.2784 0.4931 0.074 Uiso 0.30 1 calc PR B 1 C91 C -0.673(3) 0.271(2) 0.4098(9) 0.048(7) Uiso 0.30 1 d P B 1 C92 C -0.648(3) 0.271(2) 0.3529(10) 0.055(9) Uiso 0.30 1 d P B 1 H92A H -0.7249 0.2569 0.3344 0.083 Uiso 0.30 1 calc PR B 1 H92B H -0.6120 0.2171 0.3455 0.083 Uiso 0.30 1 calc PR B 1 H92C H -0.5929 0.3397 0.3477 0.083 Uiso 0.30 1 calc PR B 1 O200 O -0.0005(13) 1.0441(10) 0.5030(5) 0.073(4) Uiso 0.25 1 d P . 2 C201 C -0.1248(10) 1.0283(9) 0.4824(4) 0.071(3) Uiso 0.50 1 d P C 2 O202 O -0.1464(7) 0.9830(6) 0.4405(3) 0.080(2) Uiso 0.50 1 d P C 2 C203 C -0.3107(8) 0.8562(7) 0.4153(3) 0.049(2) Uiso 0.50 1 d P D 6 C204 C -0.2651(5) 0.9703(4) 0.41750(19) 0.0156(12) Uiso 0.50 1 d P D 6 O205 O -0.3523(6) 1.0158(5) 0.4391(2) 0.0673(18) Uiso 0.50 1 d P D 6 C206 C -0.3271(9) 1.0528(7) 0.4838(3) 0.053(2) Uiso 0.50 1 d P D 6 C207 C -0.2049(8) 1.0369(6) 0.5017(3) 0.0240(19) Uiso 0.50 1 d P C 2 O208 O -0.2414(6) 1.0469(5) 0.5044(2) 0.0424(19) Uiso 0.50 1 d P D 6 C209 C -0.4177(12) 1.1015(11) 0.5006(5) 0.098(4) Uiso 0.50 1 d P D 6 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 O1 0.0297(13) 0.0247(12) 0.0366(14) 0.0054(11) 0.0129(11) 0.0083(10) O2 0.0360(14) 0.0267(13) 0.0465(16) 0.0032(12) 0.0186(12) 0.0102(11) O3 0.0300(13) 0.0203(12) 0.0439(16) 0.0039(11) 0.0111(11) 0.0060(10) O4 0.0287(13) 0.0217(12) 0.0349(14) -0.0005(10) -0.0049(11) 0.0085(10) O5 0.0360(14) 0.0267(13) 0.0423(16) -0.0087(12) -0.0110(12) 0.0083(11) O6 0.0311(13) 0.0250(12) 0.0372(15) 0.0013(11) -0.0139(11) 0.0082(11) O7 0.0263(12) 0.0258(12) 0.0192(12) 0.0022(10) 0.0022(10) 0.0039(10) O8 0.0289(13) 0.0344(13) 0.0205(13) 0.0095(10) -0.0057(10) 0.0008(11) O9 0.0289(13) 0.0301(13) 0.0251(13) 0.0118(11) -0.0003(10) 0.0018(10) O10 0.0301(13) 0.0427(14) 0.0209(13) 0.0145(11) 0.0055(10) 0.0147(11) O11 0.0315(13) 0.0415(14) 0.0239(13) 0.0098(11) 0.0107(10) 0.0159(12) O12 0.0316(14) 0.0349(14) 0.0310(14) 0.0140(11) 0.0099(11) 0.0149(11) O13 0.0261(12) 0.0277(12) 0.0220(12) 0.0022(10) 0.0029(10) 0.0067(10) O14 0.0327(14) 0.0342(14) 0.0261(14) 0.0072(11) 0.0003(11) 0.0087(11) O15 0.040(3) 0.053(3) 0.081(4) -0.022(3) 0.007(3) 0.016(2) O16 0.036(4) 0.037(3) 0.039(3) -0.006(2) 0.006(3) 0.011(3) O19 0.0336(14) 0.0389(14) 0.0242(13) 0.0076(11) 0.0068(11) 0.0113(12) C1 0.0199(16) 0.0253(17) 0.0209(17) 0.0061(14) -0.0020(13) 0.0075(14) C2 0.0172(16) 0.0287(18) 0.0230(18) 0.0094(14) 0.0050(14) 0.0071(14) C3 0.0244(17) 0.0287(18) 0.0248(18) 0.0044(15) 0.0040(14) 0.0141(15) C4 0.0239(17) 0.0219(17) 0.0266(18) 0.0054(14) -0.0002(14) 0.0073(14) C5 0.0220(17) 0.0260(17) 0.0161(16) 0.0061(13) -0.0005(13) 0.0079(14) C6 0.0228(17) 0.0234(17) 0.0212(17) 0.0012(14) 0.0005(14) 0.0089(14) C7 0.0237(17) 0.0246(17) 0.0208(17) 0.0048(14) 0.0035(14) 0.0067(14) C8 0.0222(17) 0.0215(16) 0.0195(17) 0.0053(13) 0.0044(13) 0.0067(14) C9 0.0254(17) 0.0221(17) 0.0207(17) 0.0031(13) 0.0060(14) 0.0107(14) C10 0.0272(18) 0.0190(17) 0.0267(19) -0.0020(14) 0.0034(15) 0.0035(14) C11 0.0215(17) 0.0232(17) 0.0244(18) 0.0071(14) 0.0003(14) 0.0031(14) C12 0.0258(17) 0.0187(16) 0.0202(17) 0.0068(13) 0.0040(14) 0.0066(14) C13 0.0225(17) 0.0211(16) 0.0194(17) 0.0010(13) 0.0029(14) 0.0043(14) C14 0.0210(17) 0.0248(17) 0.0194(17) 0.0062(14) 0.0022(13) 0.0058(14) C15 0.0213(16) 0.0204(16) 0.0179(16) 0.0041(13) 0.0034(13) 0.0066(13) C16 0.0177(16) 0.0179(16) 0.0267(18) 0.0006(13) 0.0023(14) 0.0043(13) C17 0.0239(17) 0.0280(18) 0.0182(17) 0.0035(14) -0.0001(14) 0.0116(15) C18 0.0251(17) 0.0185(16) 0.0235(18) 0.0072(13) 0.0067(14) 0.0076(14) C19 0.0206(16) 0.0195(16) 0.0237(18) 0.0032(13) 0.0019(14) 0.0079(13) C20 0.0245(17) 0.0232(17) 0.0183(17) 0.0028(13) 0.0004(14) 0.0072(14) C21 0.0210(16) 0.0223(16) 0.0202(17) 0.0038(13) 0.0003(13) 0.0036(14) C22 0.0253(17) 0.0176(16) 0.0187(17) 0.0009(13) -0.0004(14) 0.0041(14) C23 0.0259(17) 0.0186(16) 0.0191(17) 0.0041(13) -0.0030(14) 0.0029(14) C24 0.0250(18) 0.0256(17) 0.0185(17) 0.0059(14) 0.0038(14) 0.0032(14) C25 0.0211(17) 0.0226(17) 0.0235(18) 0.0018(14) 0.0013(14) 0.0044(14) C26 0.0211(16) 0.0181(16) 0.0202(17) 0.0019(13) -0.0015(13) 0.0041(13) C27 0.0249(17) 0.0209(16) 0.0171(16) 0.0036(13) 0.0008(14) 0.0036(14) C28 0.0204(16) 0.0235(17) 0.0217(18) 0.0028(14) 0.0010(13) 0.0036(14) C29 0.0274(18) 0.0318(19) 0.0196(18) 0.0060(15) -0.0011(14) 0.0087(15) C30 0.036(2) 0.033(2) 0.029(2) 0.0074(16) 0.0102(16) 0.0078(17) C31 0.041(2) 0.035(2) 0.029(2) 0.0061(16) 0.0114(17) 0.0084(17) C32 0.038(2) 0.032(2) 0.030(2) 0.0038(16) 0.0078(17) 0.0118(17) C33 0.041(2) 0.032(2) 0.030(2) 0.0051(16) 0.0094(17) 0.0122(17) C34 0.040(2) 0.032(2) 0.027(2) 0.0017(16) 0.0041(17) 0.0128(17) C35 0.044(2) 0.030(2) 0.031(2) 0.0040(16) 0.0044(17) 0.0130(17) C36 0.042(2) 0.036(2) 0.029(2) 0.0023(17) 0.0040(17) 0.0173(18) C37 0.047(2) 0.032(2) 0.026(2) 0.0033(16) 0.0055(17) 0.0156(18) C38 0.043(2) 0.034(2) 0.032(2) 0.0049(17) 0.0028(18) 0.0117(18) C39 0.047(2) 0.039(2) 0.027(2) 0.0008(17) 0.0061(18) 0.0092(19) C40 0.069(3) 0.066(3) 0.033(2) 0.006(2) 0.007(2) -0.001(3) C41 0.117(5) 0.105(5) 0.050(3) -0.007(3) 0.035(3) -0.017(4) C42 0.0279(18) 0.0276(18) 0.0197(17) 0.0055(14) 0.0031(14) 0.0080(15) C43 0.036(2) 0.040(2) 0.027(2) 0.0043(16) 0.0032(16) 0.0192(17) C44 0.042(2) 0.037(2) 0.028(2) -0.0007(16) 0.0000(17) 0.0197(18) C45 0.042(2) 0.039(2) 0.026(2) -0.0015(16) 0.0032(17) 0.0168(18) C46 0.051(2) 0.039(2) 0.026(2) -0.0004(17) 0.0004(18) 0.0196(19) C47 0.043(2) 0.039(2) 0.027(2) 0.0031(17) 0.0012(17) 0.0134(18) C48 0.047(2) 0.034(2) 0.028(2) -0.0030(17) -0.0021(17) 0.0157(18) C49 0.046(2) 0.033(2) 0.028(2) -0.0007(16) 0.0005(17) 0.0141(18) C50 0.042(2) 0.032(2) 0.031(2) 0.0035(16) -0.0006(17) 0.0127(17) C51 0.058(3) 0.036(2) 0.028(2) 0.0037(17) 0.0049(19) 0.015(2) C52 0.045(2) 0.037(2) 0.029(2) 0.0007(17) 0.0045(18) 0.0124(18) C53 0.083(3) 0.054(3) 0.035(2) 0.009(2) 0.010(2) 0.027(3) C54 0.072(3) 0.065(3) 0.035(3) 0.000(2) 0.010(2) 0.014(3) C55 0.0262(18) 0.0276(18) 0.0199(17) 0.0032(14) -0.0013(14) 0.0063(15) C56 0.039(2) 0.0265(18) 0.0244(19) 0.0006(15) -0.0008(16) 0.0056(16) C57 0.049(2) 0.0289(19) 0.029(2) 0.0003(16) -0.0015(18) 0.0115(18) C58 0.047(2) 0.0260(19) 0.029(2) -0.0016(16) -0.0013(17) 0.0107(17) C59 0.059(3) 0.036(2) 0.024(2) 0.0012(16) -0.0026(18) 0.0196(19) C60 0.045(2) 0.035(2) 0.028(2) -0.0019(17) -0.0016(17) 0.0137(18) C61 0.053(2) 0.034(2) 0.028(2) -0.0008(17) -0.0031(18) 0.0178(19) C62 0.049(2) 0.034(2) 0.031(2) 0.0054(17) 0.0010(18) 0.0151(19) C63 0.052(2) 0.036(2) 0.027(2) 0.0007(17) 0.0002(18) 0.0191(19) C64 0.057(3) 0.036(2) 0.033(2) 0.0042(18) 0.0059(19) 0.016(2) C65 0.045(2) 0.039(2) 0.031(2) 0.0052(17) 0.0024(18) 0.0162(19) C66 0.066(3) 0.051(3) 0.032(2) 0.010(2) 0.009(2) 0.019(2) C67 0.068(3) 0.070(3) 0.035(3) 0.012(2) 0.014(2) 0.023(3) C68 0.0273(18) 0.0270(18) 0.0247(18) 0.0017(15) 0.0027(15) 0.0087(15) C69 0.032(2) 0.0261(18) 0.030(2) 0.0007(15) 0.0006(16) 0.0069(16) C70 0.035(2) 0.038(2) 0.036(2) -0.0056(17) 0.0014(17) 0.0152(18) C71 0.047(2) 0.035(2) 0.038(2) -0.0044(18) -0.0073(19) 0.0137(19) C72 0.065(3) 0.038(2) 0.041(2) -0.0105(19) -0.014(2) 0.022(2) C73 0.050(3) 0.040(2) 0.043(2) -0.0104(19) -0.009(2) 0.021(2) C74 0.057(3) 0.043(2) 0.041(2) -0.011(2) -0.010(2) 0.024(2) C75 0.047(2) 0.037(2) 0.049(3) -0.009(2) -0.007(2) 0.017(2) C76 0.051(3) 0.042(2) 0.045(3) -0.005(2) -0.007(2) 0.025(2) C77 0.047(2) 0.036(2) 0.052(3) -0.004(2) -0.003(2) 0.0174(19) C78 0.045(2) 0.038(2) 0.049(3) -0.0005(19) -0.005(2) 0.0168(19) C79 0.048(3) 0.042(2) 0.057(3) 0.005(2) -0.004(2) 0.016(2) C80 0.059(3) 0.065(3) 0.044(3) 0.001(2) -0.002(2) 0.017(2) C81 0.039(2) 0.062(3) 0.030(2) 0.009(2) 0.0095(18) 0.000(2) C82 0.0256(18) 0.0272(18) 0.030(2) 0.0048(15) 0.0084(15) 0.0046(15) C83 0.0271(18) 0.0249(17) 0.0213(18) 0.0014(14) 0.0029(15) 0.0085(15) C84 0.039(2) 0.037(2) 0.030(2) 0.0059(17) 0.0062(17) -0.0003(18) C85 0.049(6) 0.054(7) 0.084(7) 0.000(5) 0.019(5) 0.009(5) C86 0.028(4) 0.030(4) 0.068(6) -0.015(4) 0.006(4) -0.008(3) C87 0.057(4) 0.052(4) 0.035(3) 0.008(3) -0.002(3) 0.027(3) C88 0.116(7) 0.125(7) 0.044(4) 0.024(4) 0.029(4) 0.091(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 O1 C2 1.391(4) . ? O2 C3 1.370(4) . ? O3 C4 1.382(4) . ? O4 C9 1.387(4) . ? O5 C10 1.371(4) . ? O6 C11 1.370(4) . ? O7 C16 1.393(4) . ? O8 C17 1.371(4) . ? O9 C18 1.381(4) . ? O10 C23 1.389(4) . ? O11 C24 1.377(4) . ? O12 C25 1.376(4) . ? O13 C83 1.347(4) . ? O13 C82 1.467(4) . ? O14 C83 1.208(4) . ? O15 C86 1.200(9) . ? O16 C86 1.338(10) . ? O16 C87 1.464(8) . ? O17 C91 1.34(4) . ? O17 C90 1.471(19) . ? O18 C91 1.21(3) . ? C1 C2 1.381(5) . ? C1 C6 1.400(4) . ? C1 C28 1.534(4) . ? C2 C3 1.389(5) . ? C3 C4 1.394(5) . ? C4 C5 1.396(5) . ? C5 C6 1.401(4) . ? C5 C7 1.533(4) . ? C7 C29 1.530(5) . ? C7 C8 1.534(4) . ? C8 C9 1.393(4) . ? C8 C13 1.397(4) . ? C9 C10 1.384(5) . ? C10 C11 1.404(5) . ? C11 C12 1.404(4) . ? C12 C13 1.390(4) . ? C12 C14 1.528(4) . ? C14 C15 1.523(4) . ? C14 C42 1.542(4) . ? C15 C16 1.394(4) . ? C15 C20 1.399(4) . ? C16 C17 1.390(4) . ? C17 C18 1.400(4) . ? C18 C19 1.392(4) . ? C19 C20 1.399(4) . ? C19 C21 1.525(4) . ? C21 C22 1.527(5) . ? C21 C68 1.544(5) . ? C22 C23 1.398(5) . ? C22 C27 1.402(4) . ? C23 C24 1.386(5) . ? C24 C25 1.400(4) . ? C25 C26 1.400(5) . ? C26 C27 1.386(5) . ? C26 C28 1.545(4) . ? C28 C55 1.530(5) . ? C29 C30 1.534(5) . ? C30 C31 1.512(5) . ? C31 C32 1.520(5) . ? C32 C33 1.515(5) . ? C33 C34 1.522(5) . ? C34 C35 1.528(5) . ? C35 C36 1.525(5) . ? C36 C37 1.517(5) . ? C37 C38 1.513(5) . ? C38 C39 1.519(5) . ? C39 C40 1.508(6) . ? C40 C41 1.502(7) . ? C42 C43 1.525(5) . ? C43 C44 1.526(5) . ? C44 C45 1.535(5) . ? C45 C46 1.522(5) . ? C46 C47 1.519(5) . ? C47 C48 1.524(5) . ? C48 C49 1.521(5) . ? C49 C50 1.515(5) . ? C50 C51 1.522(5) . ? C51 C52 1.527(5) . ? C52 C53 1.496(5) . ? C53 C54 1.520(6) . ? C55 C56 1.540(5) . ? C56 C57 1.520(5) . ? C57 C58 1.531(5) . ? C58 C59 1.530(5) . ? C59 C60 1.516(5) . ? C60 C61 1.514(5) . ? C61 C62 1.530(5) . ? C62 C63 1.515(5) . ? C63 C64 1.511(5) . ? C64 C65 1.526(5) . ? C65 C66 1.502(5) . ? C66 C67 1.513(6) . ? C68 C69 1.534(5) . ? C69 C70 1.525(5) . ? C70 C71 1.511(5) . ? C71 C72 1.536(6) . ? C72 C73 1.523(6) . ? C73 C74 1.529(5) . ? C74 C75 1.518(6) . ? C75 C76 1.536(6) . ? C76 C77 1.516(6) . ? C77 C78 1.506(6) . ? C78 C79 1.517(6) . ? C79 C80 1.510(6) . ? C81 C82 1.492(5) . ? C83 C84 1.497(5) . ? C85 C86 1.451(15) . ? C87 C88 1.481(9) . ? C89 C90 1.69(3) . ? C91 C92 1.79(4) . ? O200 O200 1.20(3) 2_576 ? O200 C201 1.482(18) . ? C201 C207 1.188(13) . ? C201 O202 1.352(12) . ? C203 C204 1.462(10) . ? C204 O205 1.530(9) . ? O205 C206 1.397(11) . ? C206 O208 1.167(10) . ? C206 C209 1.529(16) . ? 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 C83 O13 C82 116.1(2) . . ? C86 O16 C87 115.8(6) . . ? C91 O17 C90 114.6(16) . . ? C2 C1 C6 117.1(3) . . ? C2 C1 C28 121.0(3) . . ? C6 C1 C28 121.9(3) . . ? C1 C2 C3 122.1(3) . . ? C1 C2 O1 118.6(3) . . ? C3 C2 O1 119.3(3) . . ? O2 C3 C2 117.3(3) . . ? O2 C3 C4 123.4(3) . . ? C2 C3 C4 119.3(3) . . ? O3 C4 C3 114.5(3) . . ? O3 C4 C5 124.4(3) . . ? C3 C4 C5 121.1(3) . . ? C4 C5 C6 117.2(3) . . ? C4 C5 C7 121.5(3) . . ? C6 C5 C7 121.3(3) . . ? C1 C6 C5 123.1(3) . . ? C29 C7 C8 112.6(3) . . ? C29 C7 C5 111.6(3) . . ? C8 C7 C5 110.0(3) . . ? C9 C8 C13 117.3(3) . . ? C9 C8 C7 120.6(3) . . ? C13 C8 C7 122.1(3) . . ? O4 C9 C10 120.0(3) . . ? O4 C9 C8 119.1(3) . . ? C10 C9 C8 120.9(3) . . ? O5 C10 C9 117.4(3) . . ? O5 C10 C11 122.1(3) . . ? C9 C10 C11 120.5(3) . . ? O6 C11 C10 114.5(3) . . ? O6 C11 C12 125.4(3) . . ? C10 C11 C12 120.0(3) . . ? C13 C12 C11 117.3(3) . . ? C13 C12 C14 121.7(3) . . ? C11 C12 C14 120.9(3) . . ? C12 C13 C8 123.8(3) . . ? C15 C14 C12 111.8(3) . . ? C15 C14 C42 113.1(3) . . ? C12 C14 C42 111.3(3) . . ? C16 C15 C20 116.8(3) . . ? C16 C15 C14 121.3(3) . . ? C20 C15 C14 121.8(3) . . ? C17 C16 C15 121.4(3) . . ? C17 C16 O7 120.0(3) . . ? C15 C16 O7 118.7(3) . . ? O8 C17 C16 117.9(3) . . ? O8 C17 C18 122.3(3) . . ? C16 C17 C18 119.8(3) . . ? O9 C18 C19 124.5(3) . . ? O9 C18 C17 114.4(3) . . ? C19 C18 C17 121.0(3) . . ? C18 C19 C20 117.1(3) . . ? C18 C19 C21 120.6(3) . . ? C20 C19 C21 122.3(3) . . ? C19 C20 C15 123.8(3) . . ? C19 C21 C22 111.3(3) . . ? C19 C21 C68 111.3(3) . . ? C22 C21 C68 114.0(3) . . ? C23 C22 C27 116.7(3) . . ? C23 C22 C21 120.9(3) . . ? C27 C22 C21 122.4(3) . . ? C24 C23 O10 119.8(3) . . ? C24 C23 C22 121.5(3) . . ? O10 C23 C22 118.7(3) . . ? O11 C24 C23 116.6(3) . . ? O11 C24 C25 123.1(3) . . ? C23 C24 C25 120.2(3) . . ? O12 C25 C24 115.5(3) . . ? O12 C25 C26 124.5(3) . . ? C24 C25 C26 119.9(3) . . ? C27 C26 C25 118.1(3) . . ? C27 C26 C28 121.1(3) . . ? C25 C26 C28 120.8(3) . . ? C26 C27 C22 123.5(3) . . ? C55 C28 C1 112.4(3) . . ? C55 C28 C26 112.9(3) . . ? C1 C28 C26 111.1(2) . . ? C7 C29 C30 115.0(3) . . ? C31 C30 C29 111.5(3) . . ? C30 C31 C32 115.8(3) . . ? C33 C32 C31 113.6(3) . . ? C32 C33 C34 113.6(3) . . ? C33 C34 C35 113.8(3) . . ? C36 C35 C34 113.7(3) . . ? C37 C36 C35 113.2(3) . . ? C38 C37 C36 114.2(3) . . ? C37 C38 C39 113.4(3) . . ? C40 C39 C38 115.3(3) . . ? C41 C40 C39 112.6(4) . . ? C43 C42 C14 114.3(3) . . ? C42 C43 C44 113.4(3) . . ? C43 C44 C45 115.7(3) . . ? C46 C45 C44 112.4(3) . . ? C47 C46 C45 115.0(3) . . ? C46 C47 C48 113.5(3) . . ? C49 C48 C47 115.0(3) . . ? C50 C49 C48 114.3(3) . . ? C49 C50 C51 114.2(3) . . ? C50 C51 C52 115.4(3) . . ? C53 C52 C51 114.7(3) . . ? C52 C53 C54 115.1(4) . . ? C28 C55 C56 113.2(3) . . ? C57 C56 C55 113.6(3) . . ? C56 C57 C58 115.6(3) . . ? C59 C58 C57 112.8(3) . . ? C60 C59 C58 114.2(3) . . ? C61 C60 C59 114.1(3) . . ? C60 C61 C62 114.4(3) . . ? C63 C62 C61 114.3(3) . . ? C64 C63 C62 114.5(3) . . ? C63 C64 C65 114.1(3) . . ? C66 C65 C64 115.1(3) . . ? C65 C66 C67 113.2(4) . . ? C69 C68 C21 114.6(3) . . ? C70 C69 C68 113.2(3) . . ? C71 C70 C69 113.2(3) . . ? C70 C71 C72 114.9(4) . . ? C73 C72 C71 114.9(3) . . ? C72 C73 C74 113.3(3) . . ? C75 C74 C73 114.6(3) . . ? C74 C75 C76 114.0(3) . . ? C77 C76 C75 114.5(3) . . ? C78 C77 C76 114.7(3) . . ? C77 C78 C79 114.9(3) . . ? C80 C79 C78 114.1(4) . . ? O13 C82 C81 108.1(3) . . ? O14 C83 O13 122.9(3) . . ? O14 C83 C84 124.9(3) . . ? O13 C83 C84 112.2(3) . . ? O15 C86 O16 123.7(8) . . ? O15 C86 C85 131.5(10) . . ? O16 C86 C85 104.6(8) . . ? O16 C87 C88 106.1(5) . . ? O17 C90 C89 106.1(13) . . ? O18 C91 O17 122(3) . . ? O18 C91 C92 135(3) . . ? O17 C91 C92 103(2) . . ? O200 O200 C201 98.6(16) 2_576 . ? C207 C201 O202 120.9(10) . . ? C207 C201 O200 124.9(12) . . ? O202 C201 O200 113.1(11) . . ? C203 C204 O205 109.8(6) . . ? C206 O205 C204 119.4(6) . . ? O208 C206 O205 119.9(9) . . ? O208 C206 C209 126.0(10) . . ? O205 C206 C209 114.1(9) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.17 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.276 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.071 # Attachment '4.cif' data_PgC3CuGa _database_code_depnum_ccdc_archive 'CCDC 648032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122.75 H140.50 Cu8 Ga4 O45.50' _chemical_formula_weight 3131.05 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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 21.206(3) _cell_length_b 21.834(3) _cell_length_c 23.544(5) _cell_angle_alpha 110.972(2) _cell_angle_beta 110.134(2) _cell_angle_gamma 98.955(2) _cell_volume 9060(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3194 _exptl_absorpt_coefficient_mu 1.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8226 _exptl_absorpt_correction_T_max 0.8593 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69070 _diffrn_radiation_type Synchrotron _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Bruker APEX II diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46495 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 20.30 _reflns_number_total 19010 _reflns_number_gt 10888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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. There is severe disorder associated with the solvent molecules. In addition, two of the C-propyl side chains are disordered over two positions and have been modelled as such with appropriate use of restraints on C-C bonds. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _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 19010 _refine_ls_number_parameters 1571 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1179 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.2178 _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_restrained_S_all 1.283 _refine_ls_shift/su_max '1.294 (H-Tors)' _refine_ls_shift/su_mean 0.007 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 Cu1 Cu 0.27576(7) 0.64403(7) 0.22909(7) 0.0643(4) Uani 1 1 d . . . O1 O 0.7814(4) 1.1739(4) 0.8904(3) 0.070(2) Uani 1 1 d . . . C1 C 0.8718(6) 1.1156(5) 0.8933(5) 0.059(3) Uani 1 1 d . . . Cu2 Cu 0.66661(7) 0.72162(7) 0.47372(6) 0.0650(4) Uani 1 1 d . . . O2 O 0.8137(4) 1.2265(4) 0.8116(4) 0.081(2) Uani 1 1 d . . . C2 C 0.8349(6) 1.1581(6) 0.8721(6) 0.066(3) Uani 1 1 d . . . Cu3 Cu 0.40553(7) 0.96027(6) 0.76314(7) 0.0673(4) Uani 1 1 d . . . O3 O 0.9070(4) 1.1930(4) 0.7636(4) 0.070(2) Uani 1 1 d . . . C3 C 0.8502(6) 1.1825(6) 0.8301(6) 0.071(3) Uani 1 1 d . . . C211 C 1.0303(16) 1.0879(17) 0.5697(14) 0.037(9) Uiso 0.25 1 d PD A 2 Cu4 Cu 0.81493(8) 0.90804(7) 0.47712(6) 0.0701(4) Uani 1 1 d . . . O4 O 0.9291(4) 1.1142(4) 0.6717(3) 0.068(2) Uani 1 1 d . C . C4 C 0.8991(6) 1.1671(6) 0.8062(6) 0.064(3) Uani 1 1 d . . . Cu5 Cu 0.59988(7) 1.05406(7) 0.84905(7) 0.0716(4) Uani 1 1 d . . . O5 O 0.8584(4) 1.0001(3) 0.5531(3) 0.068(2) Uani 1 1 d . C . C5 C 0.9378(6) 1.1275(6) 0.8264(6) 0.068(3) Uani 1 1 d . . . Cu6 Cu 0.47552(7) 0.62504(7) 0.38556(7) 0.0683(4) Uani 1 1 d . . . O6 O 0.8429(3) 0.8721(3) 0.5428(3) 0.064(2) Uani 1 1 d . C . C6 C 0.9222(6) 1.1007(6) 0.8676(6) 0.066(3) Uani 1 1 d . . . H6 H 0.9467 1.0708 0.8790 0.079 Uiso 1 1 calc R . . Cu7 Cu 0.53401(7) 0.86172(7) 0.74865(7) 0.0716(4) Uani 1 1 d . . . O7 O 0.7734(4) 0.8154(3) 0.4043(3) 0.063(2) Uani 1 1 d . . . C7 C 0.9921(6) 1.1083(6) 0.8012(5) 0.065(3) Uani 1 1 d . B . H7 H 1.0115 1.1471 0.7925 0.078 Uiso 1 1 calc R . . Cu8 Cu 0.88469(8) 1.09816(7) 0.57680(7) 0.0735(4) Uani 1 1 d . . . O8 O 0.7847(4) 0.9394(3) 0.4070(3) 0.065(2) Uani 1 1 d . . . C8 C 0.9545(5) 1.0440(5) 0.7327(5) 0.058(3) Uani 1 1 d . B . Cu9 Cu 0.56565(7) 0.70424(7) 0.56960(7) 0.0703(4) Uani 1 1 d . . . O9 O 0.7421(4) 0.9579(4) 0.2957(3) 0.064(2) Uani 1 1 d . . . C9 C 0.9252(6) 1.0509(7) 0.6733(6) 0.064(3) Uani 1 1 d . . . Cu10 Cu 0.14785(7) 0.74456(7) 0.24330(7) 0.0654(4) Uani 1 1 d . . . O10 O 0.6364(4) 0.9667(4) 0.2140(4) 0.072(2) Uani 1 1 d . . . C10 C 0.8885(6) 0.9921(6) 0.6100(6) 0.067(3) Uani 1 1 d . C . Cu11 Cu 0.79382(8) 1.02191(7) 0.39306(7) 0.0698(4) Uani 1 1 d . . . O11 O 0.5038(4) 0.9659(4) 0.1838(4) 0.084(2) Uani 1 1 d . . . C11 C 0.8814(5) 0.9267(6) 0.6074(5) 0.054(3) Uani 1 1 d . . . Cu12 Cu 0.25107(7) 0.76149(7) 0.14595(7) 0.0667(4) Uani 1 1 d . . . O12 O 0.3924(4) 0.8482(3) 0.1039(3) 0.070(2) Uani 1 1 d . . . C12 C 0.9090(5) 0.9172(5) 0.6653(6) 0.060(3) Uani 1 1 d . C . O13 O 0.7037(4) 1.0779(4) 0.8882(4) 0.076(2) Uani 1 1 d . . . C13 C 0.9449(5) 0.9761(6) 0.7273(5) 0.064(3) Uani 1 1 d . . . H13 H 0.9637 0.9705 0.7673 0.077 Uiso 1 1 calc R C . O14 O 0.5981(4) 0.9570(4) 0.8083(4) 0.088(3) Uani 1 1 d . . . C14 C 0.8536(6) 1.0858(6) 0.9357(5) 0.070(3) Uani 1 1 d . . . H14 H 0.8350 1.1188 0.9622 0.084 Uiso 1 1 calc R . . O15 O 0.6192(4) 0.8366(4) 0.7579(4) 0.073(2) Uani 1 1 d . . . C15 C 0.9159(6) 1.0797(7) 0.9870(6) 0.081(4) Uani 1 1 d . . . H15A H 0.9339 1.0451 0.9624 0.097 Uiso 1 1 calc R . . H15B H 0.9542 1.1248 1.0124 0.097 Uiso 1 1 calc R . . O16 O 0.6344(3) 0.7538(3) 0.6646(3) 0.0626(19) Uani 1 1 d . . . C16 C 0.9008(6) 1.0598(7) 1.0357(6) 0.087(4) Uani 1 1 d . . . H16A H 0.8620 1.0151 1.0106 0.104 Uiso 1 1 calc R . . H16B H 0.8841 1.0950 1.0614 0.104 Uiso 1 1 calc R . . O17 O 0.6413(4) 0.7366(4) 0.5496(3) 0.070(2) Uani 1 1 d . . . C17 C 0.9626(9) 1.0530(9) 1.0839(7) 0.130(6) Uani 1 1 d . . . H17A H 1.0052 1.0906 1.0984 0.195 Uiso 1 1 calc R . . H17B H 0.9689 1.0084 1.0619 0.195 Uiso 1 1 calc R . . H17C H 0.9548 1.0556 1.1233 0.195 Uiso 1 1 calc R . . O18 O 0.7636(3) 0.7780(3) 0.5430(3) 0.0620(19) Uani 1 1 d . . . C18 C 1.0547(6) 1.1017(6) 0.8517(6) 0.082(4) Uani 1 1 d D . . O19 O 0.6944(3) 0.7171(3) 0.4017(3) 0.0627(19) Uani 1 1 d . . . O20 O 0.5697(4) 0.6714(4) 0.4025(3) 0.071(2) Uani 1 1 d . . . C20 C 1.1645(18) 1.078(2) 0.8853(17) 0.255(17) Uiso 0.75 1 d PD B 1 O21 O 0.4508(4) 0.5971(3) 0.2895(3) 0.0633(19) Uani 1 1 d . . . C21 C 1.1114(9) 1.0891(10) 0.8269(9) 0.101(6) Uiso 0.75 1 d PD B 1 O22 O 0.3478(4) 0.6074(3) 0.2085(3) 0.065(2) Uani 1 1 d . . . C22 C 1.0988(19) 1.1673(15) 0.9183(14) 0.064(12) Uiso 0.25 1 d PD B . O23 O 0.2843(4) 0.6947(4) 0.1762(4) 0.082(2) Uani 1 1 d . . . C23 C 1.156(3) 1.148(3) 0.964(3) 0.107(18) Uiso 0.25 1 d PD B 2 O24 O 0.3123(4) 0.7504(4) 0.0988(3) 0.070(2) Uani 1 1 d . . . C24 C 0.7102(5) 0.6861(5) 0.2764(5) 0.057(3) Uani 1 1 d . . . H24 H 0.7483 0.6923 0.3194 0.068 Uiso 1 1 calc R . . O25 O 0.1105(4) 0.7183(4) 0.2986(3) 0.070(2) Uani 1 1 d . . . C25 C 0.7197(6) 0.7575(5) 0.2791(6) 0.063(3) Uani 1 1 d . . . O26 O 0.2042(4) 0.6821(4) 0.2526(4) 0.082(2) Uani 1 1 d . . . C26 C 0.7492(6) 0.8175(6) 0.3425(5) 0.061(3) Uani 1 1 d . . . O27 O 0.2715(4) 0.5950(4) 0.2823(4) 0.073(2) Uani 1 1 d . . . C27 C 0.7563(6) 0.8819(6) 0.3456(5) 0.057(3) Uani 1 1 d . . . O28 O 0.3749(4) 0.5835(4) 0.3619(3) 0.068(2) Uani 1 1 d . . . C28 C 0.7325(6) 0.8897(5) 0.2883(6) 0.057(3) Uani 1 1 d . . . O29 O 0.4909(4) 0.6577(4) 0.4792(3) 0.082(2) Uani 1 1 d . . . C29 C 0.7019(5) 0.8331(6) 0.2235(5) 0.062(3) Uani 1 1 d . . . O30 O 0.4927(4) 0.6804(4) 0.5984(3) 0.076(2) Uani 1 1 d . . . C30 C 0.6964(5) 0.7681(5) 0.2226(5) 0.055(3) Uani 1 1 d . . . H30 H 0.6750 0.7287 0.1799 0.066 Uiso 1 1 calc R . . O31 O 0.4739(4) 0.7672(3) 0.6904(4) 0.080(2) Uani 1 1 d . . . C31 C 0.6751(6) 0.8448(6) 0.1590(5) 0.064(3) Uani 1 1 d . . . O32 O 0.4453(4) 0.8853(4) 0.7348(4) 0.088(3) Uani 1 1 d . . . C32 C 0.5985(6) 0.8425(6) 0.1413(5) 0.058(3) Uani 1 1 d . . . O33 O 0.3142(4) 0.8904(3) 0.7098(4) 0.073(2) Uani 1 1 d . . . C33 C 0.5827(6) 0.9033(5) 0.1693(5) 0.061(3) Uani 1 1 d . . . O34 O 0.2095(4) 0.8994(3) 0.6284(3) 0.071(2) Uani 1 1 d . . . C34 C 0.5169(6) 0.9040(5) 0.1578(5) 0.058(3) Uani 1 1 d . . . O35 O 0.1649(4) 0.9100(4) 0.5138(4) 0.073(2) Uiso 1 1 d . . . C35 C 0.4590(7) 0.8438(6) 0.1139(6) 0.067(3) Uani 1 1 d . . . O36 O 0.0933(4) 0.8015(4) 0.3917(3) 0.072(2) Uani 1 1 d . . . C36 C 0.4721(6) 0.7805(5) 0.0830(5) 0.065(3) Uani 1 1 d . . . O37 O 0.3274(5) 0.8369(5) 0.2279(5) 0.025(2) Uiso 0.50 1 d P . . C37 C 0.5409(6) 0.7821(5) 0.0993(5) 0.054(3) Uani 1 1 d . . . H37 H 0.5499 0.7398 0.0810 0.065 Uiso 1 1 calc R . . O38 O 0.1722(5) 0.6845(5) 0.0634(5) 0.031(3) Uiso 0.50 1 d P . . C38 C 0.7231(6) 0.6373(5) 0.2199(5) 0.070(3) Uani 1 1 d . . . H38A H 0.6863 0.6295 0.1761 0.084 Uiso 1 1 calc R . . H38B H 0.7696 0.6597 0.2236 0.084 Uiso 1 1 calc R . . O39 O 0.2304(6) 0.8237(6) 0.3290(6) 0.044(3) Uiso 0.50 1 d P . . C39 C 0.7222(8) 0.5679(7) 0.2200(7) 0.113(5) Uani 1 1 d . . . H39A H 0.6752 0.5449 0.2151 0.135 Uiso 1 1 calc R . . H39B H 0.7581 0.5757 0.2643 0.135 Uiso 1 1 calc R . . O40 O 0.0696(5) 0.6664(5) 0.1589(5) 0.029(3) Uiso 0.50 1 d P . . C40 C 0.7372(11) 0.5186(8) 0.1633(8) 0.173(9) Uani 1 1 d . . . H40A H 0.7788 0.5438 0.1621 0.260 Uiso 1 1 calc R . . H40B H 0.6961 0.5012 0.1197 0.260 Uiso 1 1 calc R . . H40C H 0.7462 0.4795 0.1723 0.260 Uiso 1 1 calc R . . O41 O 0.3520(5) 0.7273(5) 0.3134(5) 0.034(3) Uiso 0.50 1 d P . . C41 C 0.6859(7) 0.7911(6) 0.1015(6) 0.080(4) Uani 1 1 d . . . H41A H 0.7365 0.7940 0.1175 0.095 Uiso 1 1 calc R . . H41B H 0.6579 0.7439 0.0893 0.095 Uiso 1 1 calc R . . O42 O 0.1986(5) 0.5645(5) 0.1456(5) 0.024(2) Uiso 0.50 1 d P . . C42 C 0.6631(8) 0.8047(7) 0.0397(6) 0.099(4) Uani 1 1 d . . . H42A H 0.6905 0.8521 0.0515 0.119 Uiso 1 1 calc R . . H42B H 0.6122 0.8006 0.0225 0.119 Uiso 1 1 calc R . . O43 O 0.448(3) 0.737(3) 0.413(3) 0.19(2) Uiso 0.25 1 d P . . C43 C 0.6771(9) 0.7485(9) -0.0171(7) 0.141(6) Uani 1 1 d . . . H43A H 0.6432 0.7028 -0.0347 0.211 Uiso 1 1 calc R . . H43B H 0.7254 0.7471 0.0030 0.211 Uiso 1 1 calc R . . H43C H 0.6714 0.7614 -0.0539 0.211 Uiso 1 1 calc R . . O44 O 0.512(2) 0.791(2) 0.556(2) 0.118(13) Uiso 0.25 1 d P . . C44 C 0.4087(5) 0.7134(5) 0.0383(5) 0.064(3) Uani 1 1 d . . . H44 H 0.3670 0.7270 0.0175 0.077 Uiso 1 1 calc R . . O45 O 0.4961(7) 0.5245(7) 0.3804(7) 0.064(4) Uiso 0.50 1 d P . . C45 C 0.4186(7) 0.6614(6) -0.0211(5) 0.075(3) Uani 1 1 d . . . H45A H 0.4626 0.6504 -0.0028 0.090 Uiso 1 1 calc R . . H45B H 0.3784 0.6179 -0.0457 0.090 Uiso 1 1 calc R . . O46 O 0.6858(5) 0.6222(5) 0.4762(5) 0.033(3) Uiso 0.50 1 d P . . C46 C 0.4228(9) 0.6893(8) -0.0683(8) 0.120(5) Uiso 1 1 d . . . H46A H 0.4614 0.7341 -0.0434 0.144 Uiso 1 1 calc R . . H46B H 0.3778 0.6979 -0.0887 0.144 Uiso 1 1 calc R . . O47 O 0.5972(7) 0.6054(7) 0.5571(7) 0.061(4) Uiso 0.50 1 d P . . C47 C 0.4372(12) 0.6373(11) -0.1271(11) 0.194(9) Uiso 1 1 d . . . H47A H 0.3981 0.5935 -0.1531 0.292 Uiso 1 1 calc R . . H47B H 0.4816 0.6286 -0.1071 0.292 Uiso 1 1 calc R . . H47C H 0.4407 0.6579 -0.1571 0.292 Uiso 1 1 calc R . . O48 O 0.5316(6) 0.8765(6) 0.6654(6) 0.048(3) Uiso 0.50 1 d P . . C48 C 0.7921(6) 1.0165(6) 0.8909(5) 0.067(3) Uani 1 1 d . . . O49 O 0.5972(5) 1.0620(5) 0.7685(5) 0.029(3) Uiso 0.50 1 d P . . C49 C 0.7225(7) 1.0180(6) 0.8708(5) 0.066(3) Uani 1 1 d . . . O50 O 0.3997(6) 0.9718(6) 0.6770(6) 0.049(3) Uiso 0.50 1 d P . . C50 C 0.6686(6) 0.9565(6) 0.8277(6) 0.075(4) Uani 1 1 d . . . O51 O 0.5350(5) 0.8472(5) 0.8292(5) 0.030(3) Uiso 0.50 1 d P . . C51 C 0.6791(6) 0.8936(6) 0.8027(5) 0.075(4) Uani 1 1 d . . . O52 O 0.6031(5) 1.0439(5) 0.9319(5) 0.032(3) Uiso 0.50 1 d P . . C52 C 0.7468(7) 0.8913(6) 0.8232(5) 0.063(3) Uani 1 1 d . . . O53 O 0.4114(5) 0.9481(5) 0.8455(5) 0.034(3) Uiso 0.50 1 d P . . C53 C 0.8036(6) 0.9535(6) 0.8665(5) 0.065(3) Uani 1 1 d . . . H53 H 0.8508 0.9521 0.8792 0.078 Uiso 1 1 calc R . . O54 O 0.9000(5) 1.0261(5) 0.3939(5) 0.028(3) Uiso 0.50 1 d P . . C54 C 0.7626(6) 0.8220(6) 0.7952(5) 0.066(3) Uani 1 1 d . D . H54 H 0.7205 0.7846 0.7847 0.080 Uiso 1 1 calc R . . O55 O 0.9783(8) 1.1036(8) 0.5476(8) 0.084(5) Uiso 0.50 1 d P C 1 C55 C 0.7655(7) 0.8085(5) 0.7292(5) 0.059(3) Uani 1 1 d . . . O56 O 0.7051(16) 0.9062(16) 0.4878(15) 0.079(9) Uiso 0.25 1 d P . . C56 C 0.7018(6) 0.7767(5) 0.6681(6) 0.067(3) Uani 1 1 d . . . C57 C 0.7035(6) 0.7668(6) 0.6074(5) 0.061(3) Uani 1 1 d . . . C58 C 0.7664(6) 0.7880(5) 0.6049(5) 0.053(3) Uani 1 1 d . . . C59 C 0.8323(6) 0.8213(5) 0.6652(5) 0.059(3) Uani 1 1 d . C . C60 C 0.8274(6) 0.8299(5) 0.7237(5) 0.061(3) Uani 1 1 d . . . H60 H 0.8701 0.8526 0.7643 0.074 Uiso 1 1 calc R . . C61 C 0.8254(7) 0.8158(6) 0.8447(6) 0.084(4) Uani 1 1 d D . . C62 C 0.827(2) 0.7419(11) 0.824(2) 0.070(13) Uiso 0.25 1 d PD D 2 H62A H 0.8218 0.7219 0.7769 0.084 Uiso 0.25 1 calc PR D 2 H62B H 0.7870 0.7139 0.8254 0.084 Uiso 0.25 1 calc PR D 2 C63 C 0.897(3) 0.737(4) 0.870(3) 0.16(3) Uiso 0.25 1 d PD D 2 H63A H 0.9020 0.6921 0.8483 0.244 Uiso 0.25 1 calc PR D 2 H63B H 0.8964 0.7437 0.9133 0.244 Uiso 0.25 1 calc PR D 2 H63C H 0.9374 0.7738 0.8785 0.244 Uiso 0.25 1 calc PR D 2 C64 C 0.8095(8) 0.8109(9) 0.9026(7) 0.087(5) Uiso 0.75 1 d PD D 1 H64A H 0.7634 0.7746 0.8824 0.105 Uiso 0.75 1 calc PR D 1 H64B H 0.8044 0.8554 0.9284 0.105 Uiso 0.75 1 calc PR D 1 C65 C 0.8661(11) 0.7945(12) 0.9533(11) 0.148(9) Uiso 0.75 1 d PD D 1 H65A H 0.8729 0.7512 0.9285 0.222 Uiso 0.75 1 calc PR D 1 H65B H 0.8497 0.7897 0.9861 0.222 Uiso 0.75 1 calc PR D 1 H65C H 0.9111 0.8322 0.9770 0.222 Uiso 0.75 1 calc PR D 1 C66 C 0.8998(6) 0.8458(5) 0.6613(5) 0.064(3) Uani 1 1 d . . . H66 H 0.8937 0.8146 0.6153 0.077 Uiso 1 1 calc R C . C67 C 0.9633(6) 0.8400(6) 0.7114(6) 0.075(3) Uani 1 1 d . C . H67A H 1.0060 0.8584 0.7068 0.090 Uiso 1 1 calc R . . H67B H 0.9700 0.8692 0.7576 0.090 Uiso 1 1 calc R . . C68 C 0.9565(8) 0.7677(8) 0.7023(8) 0.118(5) Uiso 1 1 d . . . H68A H 0.9572 0.7397 0.6591 0.141 Uiso 1 1 calc R C . H68B H 0.9108 0.7466 0.7010 0.141 Uiso 1 1 calc R . . C69 C 1.0192(13) 0.7681(13) 0.7622(12) 0.220(11) Uiso 1 1 d . C . H69A H 1.0617 0.8060 0.7770 0.331 Uiso 1 1 calc R . . H69B H 1.0286 0.7239 0.7472 0.331 Uiso 1 1 calc R . . H69C H 1.0066 0.7748 0.7998 0.331 Uiso 1 1 calc R . . C70 C 0.6420(6) 0.6611(5) 0.2785(5) 0.056(3) Uani 1 1 d . . . C71 C 0.6374(6) 0.6768(5) 0.3397(5) 0.054(3) Uani 1 1 d . . . C72 C 0.5734(6) 0.6548(5) 0.3406(5) 0.062(3) Uani 1 1 d . . . C73 C 0.5120(5) 0.6159(5) 0.2820(5) 0.056(3) Uani 1 1 d . . . C74 C 0.5134(6) 0.5980(5) 0.2193(5) 0.063(3) Uani 1 1 d . . . C75 C 0.5773(6) 0.6204(5) 0.2206(5) 0.056(3) Uani 1 1 d . . . H75 H 0.5789 0.6073 0.1782 0.067 Uiso 1 1 calc R . . C76 C 0.4457(5) 0.5584(6) 0.1561(5) 0.061(3) Uani 1 1 d . . . H76 H 0.4136 0.5309 0.1672 0.074 Uiso 1 1 calc R . . C77 C 0.4093(5) 0.6078(5) 0.1368(5) 0.058(3) Uani 1 1 d . . . C78 C 0.3632(6) 0.6279(5) 0.1657(5) 0.057(3) Uani 1 1 d . . . C79 C 0.3316(6) 0.6744(6) 0.1501(6) 0.065(3) Uani 1 1 d . . . O80 O 1.0637(13) 1.0764(14) 0.5228(12) 0.065(8) Uiso 0.25 1 d PD A 2 C80 C 0.3430(6) 0.7008(6) 0.1084(6) 0.067(3) Uani 1 1 d . . . C81 C 0.3908(6) 0.6811(5) 0.0795(4) 0.056(3) Uani 1 1 d . . . C82 C 0.4226(6) 0.6348(5) 0.0956(5) 0.057(3) Uani 1 1 d . . . H82 H 0.4548 0.6212 0.0777 0.068 Uiso 1 1 calc R . . C83 C 0.4540(6) 0.5043(5) 0.0947(5) 0.073(3) Uani 1 1 d . . . H83A H 0.4831 0.5300 0.0804 0.088 Uiso 1 1 calc R . . H83B H 0.4798 0.4752 0.1105 0.088 Uiso 1 1 calc R . . C84 C 0.3859(6) 0.4586(6) 0.0355(5) 0.078(4) Uani 1 1 d . . . H84A H 0.3585 0.4872 0.0206 0.093 Uiso 1 1 calc R . . H84B H 0.3577 0.4302 0.0485 0.093 Uiso 1 1 calc R . . C85 C 0.3979(8) 0.4123(7) -0.0212(7) 0.128(6) Uani 1 1 d . . . H85A H 0.4282 0.4402 -0.0322 0.192 Uiso 1 1 calc R . . H85B H 0.3524 0.3851 -0.0608 0.192 Uiso 1 1 calc R . . H85C H 0.4211 0.3809 -0.0078 0.192 Uiso 1 1 calc R . . C86 C 0.1165(5) 0.6385(6) 0.3472(6) 0.061(3) Uani 1 1 d . . . C87 C 0.1356(6) 0.6677(6) 0.3117(6) 0.065(3) Uani 1 1 d . . . C88 C 0.1856(6) 0.6508(6) 0.2899(5) 0.069(3) Uani 1 1 d . . . C89 C 0.2191(6) 0.6058(6) 0.3040(6) 0.065(3) Uani 1 1 d . . . C90 C 0.1986(6) 0.5726(5) 0.3385(6) 0.064(3) Uani 1 1 d . . . C91 C 0.1489(6) 0.5908(5) 0.3608(5) 0.064(3) Uani 1 1 d . . . H91 H 0.1361 0.5702 0.3863 0.077 Uiso 1 1 calc R . . C92 C 0.2382(6) 0.5246(5) 0.3571(6) 0.074(3) Uani 1 1 d . . . H92 H 0.2534 0.5044 0.3207 0.088 Uiso 1 1 calc R . . C93 C 0.3042(6) 0.5631(5) 0.4202(6) 0.062(3) Uani 1 1 d . . . C94 C 0.3668(6) 0.5899(6) 0.4197(6) 0.070(3) Uani 1 1 d . . . C95 C 0.4284(6) 0.6294(5) 0.4797(6) 0.065(3) Uani 1 1 d . . . C96 C 0.4278(6) 0.6414(5) 0.5419(6) 0.066(3) Uani 1 1 d . . . C97 C 0.3657(7) 0.6162(6) 0.5456(6) 0.073(3) Uani 1 1 d . . . C98 C 0.3047(6) 0.5765(5) 0.4838(6) 0.061(3) Uani 1 1 d . . . H98 H 0.2618 0.5580 0.4850 0.073 Uiso 1 1 calc R . . C99 C 0.3659(6) 0.6307(5) 0.6137(6) 0.066(3) Uani 1 1 d . . . H99 H 0.4152 0.6384 0.6457 0.079 Uiso 1 1 calc R . . C100 C 0.3484(7) 0.6992(6) 0.6404(6) 0.070(3) Uani 1 1 d . . . C101 C 0.4032(6) 0.7614(6) 0.6746(6) 0.071(3) Uani 1 1 d . . . C102 C 0.3892(6) 0.8235(6) 0.6987(6) 0.075(3) Uani 1 1 d . . . C103 C 0.3230(7) 0.8254(6) 0.6867(5) 0.066(3) Uani 1 1 d . . . C104 C 0.2662(6) 0.7637(7) 0.6485(6) 0.069(3) Uani 1 1 d . . . C105 C 0.2799(7) 0.7011(6) 0.6261(6) 0.070(3) Uani 1 1 d . . . H105 H 0.2416 0.6590 0.6006 0.084 Uiso 1 1 calc R . . C106 C 0.1894(6) 0.7653(6) 0.6327(6) 0.072(3) Uani 1 1 d . . . H106 H 0.1928 0.8089 0.6692 0.086 Uiso 1 1 calc R . . C107 C 0.1600(6) 0.7719(6) 0.5685(6) 0.063(3) Uani 1 1 d . . . C108 C 0.1720(6) 0.8365(6) 0.5683(6) 0.067(3) Uani 1 1 d . . . C109 C 0.1496(6) 0.8432(5) 0.5099(6) 0.066(3) Uani 1 1 d . . . C110 C 0.1144(6) 0.7866(6) 0.4464(6) 0.073(3) Uani 1 1 d . . . C111 C 0.0995(6) 0.7217(6) 0.4434(6) 0.068(3) Uani 1 1 d . . . C112 C 0.1252(6) 0.7164(6) 0.5039(7) 0.071(3) Uani 1 1 d . . . H112 H 0.1186 0.6711 0.5010 0.086 Uiso 1 1 calc R . . C113 C 0.0625(6) 0.6583(6) 0.3744(6) 0.076(3) Uani 1 1 d . . . H113 H 0.0315 0.6735 0.3430 0.091 Uiso 1 1 calc R . . C114 C 0.1902(7) 0.4615(6) 0.3559(7) 0.095(4) Uani 1 1 d . . . H11A H 0.1727 0.4789 0.3906 0.115 Uiso 1 1 calc R . . H11B H 0.2192 0.4328 0.3679 0.115 Uiso 1 1 calc R . . C115 C 0.1242(10) 0.4144(10) 0.2847(10) 0.136(6) Uiso 1 1 d . . . C117 C 0.3170(7) 0.5707(6) 0.6121(6) 0.086(4) Uani 1 1 d . . . H11H H 0.3270 0.5275 0.5912 0.103 Uiso 1 1 calc R . . H11I H 0.2671 0.5647 0.5846 0.103 Uiso 1 1 calc R . . C118 C 0.3282(8) 0.5850(8) 0.6838(7) 0.110(5) Uiso 1 1 d . . . H11J H 0.3786 0.5932 0.7117 0.132 Uiso 1 1 calc R . . H11K H 0.3163 0.6272 0.7039 0.132 Uiso 1 1 calc R . . C119 C 0.2823(12) 0.5246(12) 0.6840(12) 0.203(9) Uiso 1 1 d . . . H11L H 0.2365 0.5313 0.6798 0.304 Uiso 1 1 calc R . . H11M H 0.3060 0.5218 0.7264 0.304 Uiso 1 1 calc R . . H11N H 0.2746 0.4816 0.6460 0.304 Uiso 1 1 calc R . . C120 C 0.1433(7) 0.7087(7) 0.6332(7) 0.093(4) Uani 1 1 d . . . H12A H 0.1412 0.6640 0.6000 0.111 Uiso 1 1 calc R . . H12B H 0.0948 0.7120 0.6196 0.111 Uiso 1 1 calc R . . C121 C 0.1720(10) 0.7109(9) 0.7074(9) 0.142(6) Uiso 1 1 d . . . H12C H 0.2226 0.7138 0.7230 0.170 Uiso 1 1 calc R . . H12D H 0.1689 0.7534 0.7391 0.170 Uiso 1 1 calc R . . C122 C 0.1302(13) 0.6466(13) 0.7100(13) 0.230(11) Uiso 1 1 d . . . H12E H 0.0847 0.6512 0.7090 0.345 Uiso 1 1 calc R . . H12F H 0.1580 0.6443 0.7517 0.345 Uiso 1 1 calc R . . H12G H 0.1220 0.6042 0.6710 0.345 Uiso 1 1 calc R . . C123 C 0.0129(7) 0.5993(6) 0.3736(7) 0.103(5) Uani 1 1 d . . . H12H H -0.0166 0.6191 0.3951 0.124 Uiso 1 1 calc R . . H12I H 0.0425 0.5818 0.4029 0.124 Uiso 1 1 calc R . . C124 C -0.0395(15) 0.5338(15) 0.3028(14) 0.237(12) Uiso 1 1 d . . . H12J H -0.0122 0.5073 0.2832 0.284 Uiso 1 1 calc R . . H12K H -0.0730 0.5028 0.3091 0.284 Uiso 1 1 calc R . . C125 C -0.0750(19) 0.5595(19) 0.2619(19) 0.329(19) Uiso 1 1 d . . . H12L H -0.0661 0.6088 0.2884 0.493 Uiso 1 1 calc R . . H12M H -0.1259 0.5348 0.2411 0.493 Uiso 1 1 calc R . . H12N H -0.0587 0.5534 0.2266 0.493 Uiso 1 1 calc R . . C200 C 0.620(2) 0.591(2) 0.596(2) 0.057(11) Uiso 0.25 1 d P . . C201 C 0.567(2) 0.564(2) 0.547(2) 0.058(11) Uiso 0.25 1 d P . . C202 C 0.7554(12) 0.6188(12) 0.5083(12) 0.080(7) Uiso 0.50 1 d P . . C203 C 0.5331(16) 0.5010(16) 0.3527(15) 0.113(10) Uiso 0.50 1 d P . . C204 C 0.5434(16) 0.7832(16) 0.8357(16) 0.116(10) Uiso 0.50 1 d P . . C210 C 0.9164(15) 1.0371(15) 0.3510(15) 0.103(9) Uiso 0.50 1 d P . . C217 C 0.151(3) 0.385(3) 0.243(3) 0.195(18) Uiso 0.50 1 d P . . C218 C 0.061(5) 0.360(4) 0.278(4) 0.34(4) 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 Cu1 0.0737(9) 0.0685(9) 0.0646(9) 0.0249(8) 0.0409(8) 0.0434(8) O1 0.079(5) 0.090(6) 0.063(5) 0.029(4) 0.047(4) 0.055(5) C1 0.065(8) 0.056(7) 0.034(6) 0.009(6) 0.012(6) 0.012(6) Cu2 0.0671(9) 0.0650(9) 0.0452(8) 0.0103(7) 0.0203(7) 0.0200(7) O2 0.093(6) 0.100(6) 0.100(6) 0.060(6) 0.064(5) 0.065(5) C2 0.076(9) 0.074(8) 0.053(7) 0.031(7) 0.023(7) 0.044(7) Cu3 0.0655(9) 0.0452(8) 0.0716(9) 0.0042(7) 0.0281(7) 0.0248(7) O3 0.077(5) 0.073(5) 0.068(5) 0.023(5) 0.038(4) 0.047(4) C3 0.073(8) 0.080(9) 0.060(8) 0.029(7) 0.021(7) 0.050(7) Cu4 0.0921(11) 0.0501(9) 0.0449(8) 0.0038(7) 0.0239(7) 0.0197(7) O4 0.083(5) 0.047(5) 0.050(4) 0.004(4) 0.020(4) 0.026(4) C4 0.069(8) 0.056(7) 0.067(8) 0.021(7) 0.029(7) 0.040(7) Cu5 0.0609(9) 0.0467(8) 0.0788(10) 0.0014(7) 0.0230(8) 0.0268(7) O5 0.085(5) 0.048(5) 0.039(4) -0.002(4) 0.017(4) 0.016(4) C5 0.074(8) 0.062(8) 0.048(7) 0.008(6) 0.018(6) 0.025(7) Cu6 0.0708(10) 0.0683(10) 0.0506(8) 0.0124(7) 0.0246(7) 0.0218(7) O6 0.063(5) 0.050(4) 0.048(4) -0.006(4) 0.016(4) 0.024(4) C6 0.058(8) 0.059(8) 0.053(7) 0.001(6) 0.010(6) 0.036(6) Cu7 0.0659(9) 0.0488(8) 0.0756(10) 0.0038(7) 0.0254(8) 0.0261(7) O7 0.080(5) 0.057(5) 0.042(4) 0.007(4) 0.026(4) 0.031(4) C7 0.061(7) 0.072(8) 0.055(7) 0.011(6) 0.029(6) 0.033(6) Cu8 0.0928(11) 0.0524(9) 0.0523(9) 0.0043(7) 0.0268(8) 0.0219(8) O8 0.081(5) 0.050(5) 0.039(4) -0.001(4) 0.023(4) 0.018(4) C8 0.050(7) 0.053(8) 0.049(7) 0.002(6) 0.014(6) 0.029(6) Cu9 0.0730(10) 0.0701(10) 0.0525(8) 0.0131(8) 0.0255(7) 0.0222(8) O9 0.075(5) 0.051(5) 0.048(4) 0.003(4) 0.026(4) 0.021(4) C9 0.052(7) 0.081(10) 0.059(9) 0.027(8) 0.024(6) 0.028(7) Cu10 0.0734(9) 0.0708(9) 0.0624(9) 0.0227(8) 0.0390(8) 0.0438(8) O10 0.074(5) 0.059(5) 0.073(5) 0.006(4) 0.041(4) 0.030(4) C10 0.070(8) 0.061(9) 0.047(8) 0.005(7) 0.021(6) 0.020(7) Cu11 0.0920(11) 0.0506(9) 0.0510(8) 0.0061(7) 0.0317(8) 0.0213(7) O11 0.069(5) 0.049(5) 0.093(6) -0.004(4) 0.026(4) 0.024(4) C11 0.055(7) 0.058(8) 0.046(7) 0.013(7) 0.027(6) 0.025(6) Cu12 0.0769(10) 0.0770(10) 0.0680(9) 0.0320(8) 0.0433(8) 0.0525(8) O12 0.066(5) 0.055(5) 0.069(5) 0.005(4) 0.025(4) 0.037(4) C12 0.047(7) 0.056(7) 0.063(8) 0.011(7) 0.021(6) 0.025(6) O13 0.071(5) 0.059(5) 0.073(5) 0.002(4) 0.026(4) 0.036(4) C13 0.060(7) 0.073(9) 0.046(7) 0.007(7) 0.021(6) 0.040(6) O14 0.081(6) 0.047(5) 0.089(6) -0.005(4) 0.020(5) 0.027(4) C14 0.075(8) 0.076(8) 0.044(7) 0.013(6) 0.013(6) 0.050(7) O15 0.077(5) 0.063(5) 0.072(5) 0.019(4) 0.032(4) 0.036(4) C15 0.081(9) 0.106(10) 0.050(7) 0.023(7) 0.024(7) 0.055(8) O16 0.063(5) 0.060(5) 0.054(4) 0.016(4) 0.023(4) 0.023(4) C16 0.078(9) 0.109(11) 0.043(7) 0.018(7) 0.007(7) 0.037(8) O17 0.062(5) 0.076(5) 0.048(4) 0.011(4) 0.019(4) 0.011(4) C17 0.157(15) 0.159(15) 0.074(10) 0.040(10) 0.042(10) 0.097(13) O18 0.063(5) 0.055(4) 0.042(4) 0.004(4) 0.011(3) 0.023(4) C18 0.059(8) 0.091(9) 0.057(7) -0.002(7) 0.012(6) 0.037(7) O19 0.059(4) 0.068(5) 0.048(4) 0.011(4) 0.023(4) 0.024(4) O20 0.078(5) 0.080(5) 0.048(4) 0.014(4) 0.032(4) 0.034(4) O21 0.076(5) 0.061(5) 0.046(4) 0.011(4) 0.032(4) 0.022(4) O22 0.078(5) 0.057(5) 0.071(5) 0.023(4) 0.043(4) 0.037(4) O23 0.116(7) 0.086(6) 0.098(6) 0.053(5) 0.075(5) 0.075(5) O24 0.081(5) 0.076(5) 0.063(5) 0.025(4) 0.039(4) 0.050(4) C24 0.068(7) 0.045(7) 0.052(7) 0.010(6) 0.028(6) 0.025(5) O25 0.067(5) 0.070(5) 0.062(5) 0.015(4) 0.029(4) 0.022(4) C25 0.064(8) 0.054(8) 0.055(8) 0.004(7) 0.028(6) 0.026(6) O26 0.100(6) 0.083(6) 0.087(6) 0.036(5) 0.055(5) 0.061(5) C26 0.071(8) 0.071(9) 0.037(7) 0.014(7) 0.025(6) 0.029(6) O27 0.082(5) 0.076(5) 0.076(5) 0.025(4) 0.053(4) 0.040(4) C27 0.082(8) 0.046(8) 0.047(8) 0.018(7) 0.030(6) 0.033(6) O28 0.079(5) 0.065(5) 0.048(4) 0.008(4) 0.033(4) 0.021(4) C28 0.073(8) 0.034(7) 0.059(8) 0.004(6) 0.037(6) 0.024(6) O29 0.074(5) 0.102(6) 0.050(5) 0.021(5) 0.026(4) 0.011(5) C29 0.061(7) 0.047(8) 0.065(8) 0.004(7) 0.031(6) 0.024(6) O30 0.075(5) 0.075(5) 0.056(5) 0.010(4) 0.026(4) 0.019(4) C30 0.064(7) 0.051(8) 0.036(7) 0.003(6) 0.024(6) 0.018(6) O31 0.092(6) 0.044(4) 0.085(6) 0.008(4) 0.042(5) 0.022(4) C31 0.079(8) 0.082(8) 0.031(6) 0.012(6) 0.026(6) 0.050(7) O32 0.081(6) 0.054(5) 0.104(6) 0.001(5) 0.044(5) 0.031(4) C32 0.063(8) 0.068(8) 0.043(6) 0.012(6) 0.027(6) 0.034(7) O33 0.089(5) 0.041(4) 0.089(5) 0.013(4) 0.048(5) 0.030(4) C33 0.059(8) 0.039(7) 0.043(6) -0.011(6) 0.012(6) 0.003(6) O34 0.104(6) 0.047(4) 0.057(5) 0.008(4) 0.044(4) 0.026(4) C34 0.044(7) 0.033(7) 0.060(7) -0.013(6) 0.017(6) 0.015(6) C35 0.085(9) 0.056(8) 0.067(8) 0.019(7) 0.039(7) 0.046(8) O36 0.076(5) 0.063(5) 0.060(5) 0.017(4) 0.024(4) 0.019(4) C36 0.079(9) 0.058(8) 0.046(7) 0.008(6) 0.032(6) 0.023(7) C37 0.055(8) 0.044(7) 0.045(6) -0.001(6) 0.023(6) 0.015(6) C38 0.075(8) 0.054(7) 0.064(8) 0.004(6) 0.032(6) 0.028(6) C39 0.143(13) 0.094(11) 0.096(11) 0.018(9) 0.057(10) 0.070(10) C40 0.22(2) 0.109(13) 0.113(14) -0.017(11) 0.046(14) 0.093(14) C41 0.100(10) 0.072(8) 0.062(8) 0.014(7) 0.040(7) 0.043(7) C42 0.137(12) 0.107(11) 0.059(8) 0.019(8) 0.061(8) 0.052(9) C43 0.173(17) 0.147(15) 0.084(11) 0.025(11) 0.060(11) 0.060(13) C44 0.057(7) 0.058(7) 0.050(7) 0.000(6) 0.019(6) 0.019(6) C45 0.097(9) 0.066(8) 0.046(7) 0.004(6) 0.034(6) 0.032(7) C48 0.064(8) 0.058(8) 0.044(7) -0.001(6) 0.008(6) 0.024(6) C49 0.079(9) 0.070(9) 0.051(7) 0.019(7) 0.031(7) 0.043(7) C50 0.050(7) 0.065(8) 0.075(8) -0.001(7) 0.019(7) 0.026(7) C51 0.069(9) 0.067(8) 0.056(7) 0.001(6) 0.014(6) 0.035(7) C52 0.078(9) 0.056(8) 0.047(7) 0.012(6) 0.025(6) 0.033(7) C53 0.076(8) 0.067(8) 0.047(7) 0.017(7) 0.024(6) 0.038(7) C54 0.086(8) 0.065(8) 0.045(7) 0.016(6) 0.024(6) 0.045(7) C55 0.079(9) 0.054(7) 0.044(7) 0.015(6) 0.024(7) 0.040(6) C56 0.075(8) 0.048(7) 0.060(8) 0.010(6) 0.022(7) 0.030(6) C57 0.075(9) 0.065(8) 0.036(7) 0.013(6) 0.027(6) 0.022(6) C58 0.066(8) 0.053(7) 0.042(7) 0.019(6) 0.024(6) 0.027(6) C59 0.082(9) 0.060(7) 0.049(7) 0.024(6) 0.032(7) 0.050(7) C60 0.058(8) 0.060(7) 0.048(8) 0.010(6) 0.013(6) 0.032(6) C61 0.125(11) 0.093(9) 0.064(8) 0.043(7) 0.048(8) 0.080(9) C66 0.051(7) 0.066(8) 0.049(7) 0.009(6) 0.006(6) 0.028(6) C67 0.078(9) 0.072(8) 0.067(8) 0.021(7) 0.030(7) 0.030(7) C70 0.074(8) 0.045(7) 0.049(7) 0.007(6) 0.034(7) 0.036(6) C71 0.054(7) 0.036(6) 0.048(7) 0.003(5) 0.014(6) 0.013(5) C72 0.077(9) 0.053(7) 0.041(7) 0.001(6) 0.023(7) 0.033(6) C73 0.063(7) 0.045(6) 0.039(7) 0.001(6) 0.013(6) 0.025(6) C74 0.061(8) 0.063(8) 0.042(7) 0.001(6) 0.016(6) 0.031(6) C75 0.062(8) 0.049(7) 0.044(7) 0.004(6) 0.023(6) 0.028(6) C76 0.060(7) 0.071(8) 0.051(7) 0.010(6) 0.034(6) 0.033(6) C77 0.053(7) 0.047(7) 0.047(7) -0.012(6) 0.018(6) 0.031(6) C78 0.068(7) 0.037(6) 0.048(7) 0.008(5) 0.019(6) 0.012(6) C79 0.069(8) 0.071(8) 0.051(7) 0.017(7) 0.033(6) 0.024(7) C80 0.060(7) 0.064(8) 0.065(8) 0.008(7) 0.030(6) 0.036(6) C81 0.073(8) 0.043(6) 0.028(6) -0.002(5) 0.018(5) 0.011(6) C82 0.078(8) 0.052(7) 0.032(6) 0.004(6) 0.027(6) 0.027(6) C83 0.094(9) 0.051(7) 0.062(8) 0.007(6) 0.035(7) 0.030(7) C84 0.073(8) 0.053(7) 0.058(7) -0.013(6) 0.017(7) 0.018(6) C85 0.136(13) 0.089(11) 0.098(11) -0.029(9) 0.066(10) 0.014(9) C86 0.044(7) 0.057(8) 0.056(7) 0.004(6) 0.019(6) 0.010(6) C87 0.071(8) 0.065(8) 0.061(7) 0.018(7) 0.034(7) 0.037(7) C88 0.089(9) 0.066(8) 0.060(7) 0.027(7) 0.038(7) 0.035(7) C89 0.064(8) 0.054(7) 0.059(7) 0.011(6) 0.024(6) 0.016(6) C90 0.071(8) 0.044(7) 0.063(8) 0.013(6) 0.027(7) 0.017(6) C91 0.061(7) 0.046(7) 0.071(8) 0.008(6) 0.035(6) 0.012(6) C92 0.098(10) 0.039(7) 0.074(9) 0.009(7) 0.046(8) 0.019(7) C93 0.076(9) 0.033(6) 0.060(8) 0.006(6) 0.028(7) 0.013(6) C94 0.055(8) 0.045(7) 0.079(9) 0.007(7) 0.018(7) 0.010(6) C95 0.078(9) 0.055(7) 0.066(8) 0.016(7) 0.047(7) 0.021(6) C96 0.076(9) 0.054(7) 0.068(8) 0.017(6) 0.038(7) 0.027(6) C97 0.096(10) 0.047(7) 0.072(9) 0.014(7) 0.043(9) 0.026(7) C98 0.061(8) 0.031(6) 0.073(9) 0.004(6) 0.031(7) 0.008(5) C99 0.078(8) 0.042(7) 0.075(8) 0.018(6) 0.039(7) 0.017(6) C100 0.081(9) 0.045(8) 0.075(8) 0.014(7) 0.038(7) 0.021(7) C101 0.072(8) 0.068(9) 0.080(8) 0.021(7) 0.046(7) 0.034(7) C102 0.063(9) 0.047(8) 0.068(8) -0.005(6) 0.016(6) 0.003(6) C103 0.071(9) 0.068(9) 0.057(7) 0.015(7) 0.038(7) 0.024(7) C104 0.070(9) 0.077(9) 0.069(8) 0.032(7) 0.038(7) 0.031(8) C105 0.078(9) 0.048(7) 0.079(8) 0.012(6) 0.043(7) 0.030(6) C106 0.089(10) 0.053(8) 0.074(9) 0.025(7) 0.041(7) 0.020(7) C107 0.065(8) 0.044(8) 0.068(9) 0.013(7) 0.028(6) 0.016(6) C108 0.076(8) 0.072(9) 0.056(8) 0.021(7) 0.037(6) 0.026(7) C109 0.084(8) 0.037(7) 0.076(9) 0.020(7) 0.040(7) 0.016(6) C110 0.077(8) 0.043(8) 0.073(9) 0.001(7) 0.027(7) 0.019(6) C111 0.075(8) 0.045(8) 0.073(9) 0.007(7) 0.043(7) 0.014(6) C112 0.082(9) 0.045(8) 0.087(10) 0.017(8) 0.049(8) 0.023(6) C113 0.079(8) 0.053(8) 0.076(8) 0.005(7) 0.039(7) 0.017(7) C114 0.092(10) 0.053(8) 0.099(10) 0.004(7) 0.032(8) 0.011(7) C117 0.108(10) 0.065(9) 0.080(9) 0.020(7) 0.043(8) 0.039(8) C120 0.096(10) 0.084(10) 0.094(10) 0.031(8) 0.045(8) 0.032(8) C123 0.102(10) 0.057(9) 0.108(11) -0.012(8) 0.059(9) 0.004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O27 1.931(8) . ? Cu1 O22 1.954(6) . ? Cu1 O23 1.971(8) . ? Cu1 O26 1.985(7) . ? Cu1 O42 2.003(9) . ? Cu1 O41 2.037(10) . ? O1 C2 1.392(13) . ? O1 Cu12 1.989(7) 2_676 ? C1 C2 1.419(14) . ? C1 C6 1.424(15) . ? C1 C14 1.490(15) . ? Cu2 O19 1.955(7) . ? Cu2 O20 1.962(7) . ? Cu2 O18 1.968(6) . ? Cu2 O17 1.972(7) . ? Cu2 O46 2.286(10) . ? O2 C3 1.417(13) . ? O2 Cu12 1.955(7) 2_676 ? O2 Cu10 1.971(8) 2_676 ? C2 C3 1.383(15) . ? Cu3 O33 1.920(7) . ? Cu3 O10 1.944(7) 2_676 ? Cu3 O11 1.948(7) 2_676 ? Cu3 O32 1.966(7) . ? Cu3 O53 2.014(10) . ? Cu3 O50 2.096(12) . ? O3 C4 1.360(13) . ? O3 Cu10 1.939(7) 2_676 ? C3 C4 1.371(15) . ? C211 O80 1.475(18) . ? Cu4 O7 1.932(6) . ? Cu4 O6 1.934(7) . ? Cu4 O5 1.951(6) . ? Cu4 O8 1.954(7) . ? Cu4 O56 2.42(3) . ? O4 C9 1.386(13) . ? O4 Cu8 1.973(7) . ? C4 C5 1.375(15) . ? Cu5 O49 1.947(10) . ? Cu5 O13 1.968(7) . ? Cu5 O12 1.970(6) 2_676 ? Cu5 O14 1.977(7) . ? Cu5 O11 1.979(7) 2_676 ? Cu5 O52 2.021(10) . ? O5 C10 1.359(13) . ? O5 Cu8 1.939(7) . ? C5 C6 1.400(15) . ? C5 C7 1.516(15) . ? Cu6 O20 1.925(7) . ? Cu6 O29 1.945(7) . ? Cu6 O21 1.964(6) . ? Cu6 O28 1.975(7) . ? Cu6 O45 2.273(13) . ? O6 C11 1.394(12) . ? Cu7 O31 1.927(7) . ? Cu7 O15 1.932(7) . ? Cu7 O14 1.965(7) . ? Cu7 O32 1.978(7) . ? Cu7 O51 2.025(10) . ? Cu7 O48 2.082(12) . ? O7 C26 1.388(12) . ? C7 C18 1.514(15) . ? C7 C8 1.533(14) . ? Cu8 O35 1.952(7) 2_676 ? Cu8 O36 1.963(7) 2_676 ? Cu8 O55 2.312(16) . ? O8 C27 1.377(11) . ? O8 Cu11 1.937(7) . ? C8 C9 1.396(14) . ? C8 C13 1.417(14) . ? Cu9 O17 1.922(7) . ? Cu9 O29 1.924(7) . ? Cu9 O16 1.957(7) . ? Cu9 O30 1.962(8) . ? Cu9 O47 2.307(13) . ? Cu9 O44 2.43(4) . ? O9 C28 1.410(12) . ? O9 Cu11 1.977(6) . ? C9 C10 1.413(15) . ? Cu10 O25 1.939(7) . ? Cu10 O3 1.939(7) 2_676 ? Cu10 O26 1.970(7) . ? Cu10 O2 1.971(8) 2_676 ? Cu10 O40 2.009(10) . ? Cu10 O39 2.063(11) . ? O10 C33 1.400(11) . ? O10 Cu3 1.944(7) 2_676 ? C10 C11 1.389(15) . ? Cu11 O35 1.931(7) 2_676 ? Cu11 O34 1.961(7) 2_676 ? Cu11 O54 2.232(10) . ? O11 C34 1.385(11) . ? O11 Cu3 1.948(7) 2_676 ? O11 Cu5 1.978(7) 2_676 ? C11 C12 1.390(14) . ? Cu12 O37 1.949(10) . ? Cu12 O2 1.955(7) 2_676 ? Cu12 O23 1.962(7) . ? Cu12 O24 1.967(7) . ? Cu12 O38 1.988(10) . ? Cu12 O1 1.989(7) 2_676 ? O12 C35 1.374(12) . ? O12 Cu5 1.970(6) 2_676 ? C12 C13 1.397(14) . ? C12 C66 1.507(11) . ? O13 C49 1.389(10) . ? O14 C50 1.409(10) . ? C14 C15 1.514(14) . ? C14 C48 1.550(11) . ? O15 C51 1.385(12) . ? C15 C16 1.476(16) . ? O16 C56 1.403(12) . ? C16 C17 1.478(16) . ? O17 C57 1.371(11) . ? O18 C58 1.373(10) . ? C18 C21 1.527(15) . ? C18 C22 1.533(19) . ? O19 C71 1.379(10) . ? O20 C72 1.404(10) . ? C20 C21 1.573(19) . ? O21 C73 1.388(11) . ? O22 C78 1.351(11) . ? C22 C23 1.55(2) . ? O23 C79 1.396(11) . ? O24 C80 1.394(11) . ? C24 C70 1.489(11) . ? C24 C25 1.515(14) . ? C24 C38 1.519(13) . ? O25 C87 1.382(11) . ? C25 C30 1.369(14) . ? C25 C26 1.427(14) . ? O26 C88 1.406(11) . ? C26 C27 1.363(14) . ? O27 C89 1.392(11) . ? C27 C28 1.351(14) . ? O28 C94 1.389(13) . ? C28 C29 1.411(14) . ? O29 C95 1.380(11) . ? C29 C30 1.397(14) . ? C29 C31 1.557(15) . ? O30 C96 1.397(12) . ? O31 C101 1.388(11) . ? C31 C32 1.519(14) . ? C31 C41 1.556(14) . ? O32 C102 1.394(11) . ? C32 C37 1.394(14) . ? C32 C33 1.406(14) . ? O33 C103 1.396(11) . ? C33 C34 1.330(13) . ? O34 C108 1.421(11) . ? O34 Cu11 1.961(7) 2_676 ? C34 C35 1.398(14) . ? O35 C109 1.405(10) . ? O35 Cu11 1.931(7) 2_676 ? O35 Cu8 1.952(7) 2_676 ? C35 C36 1.434(14) . ? O36 C110 1.382(13) . ? O36 Cu8 1.963(7) 2_676 ? C36 C37 1.366(14) . ? C36 C44 1.540(14) . ? C38 C39 1.512(16) . ? C39 C40 1.555(18) . ? C41 C42 1.520(16) . ? C42 C43 1.611(17) . ? C44 C81 1.495(11) . ? C44 C45 1.560(13) . ? O45 C203 1.24(3) . ? C45 C46 1.467(17) . ? O46 C202 1.44(2) . ? C46 C47 1.60(2) . ? O47 C201 0.91(4) . ? O47 C200 1.05(4) . ? C48 C53 1.385(14) . ? C48 C49 1.394(14) . ? C49 C50 1.374(15) . ? C50 C51 1.375(15) . ? O51 C204 1.49(3) . ? C51 C52 1.365(14) . ? C52 C53 1.410(15) . ? C52 C54 1.558(14) . ? O54 C210 1.26(3) . ? C54 C55 1.499(14) . ? C54 C61 1.501(15) . ? C55 C60 1.387(15) . ? C55 C56 1.426(15) . ? C56 C57 1.380(14) . ? C57 C58 1.370(14) . ? C58 C59 1.441(14) . ? C59 C60 1.366(14) . ? C59 C66 1.492(15) . ? C61 C62 1.521(14) . ? C61 C64 1.547(12) . ? C62 C63 1.549(15) . ? C64 C65 1.565(13) . ? C66 C67 1.511(14) . ? C67 C68 1.493(17) . ? C68 C69 1.57(2) . ? C70 C71 1.397(14) . ? C70 C75 1.412(14) . ? C71 C72 1.378(14) . ? C72 C73 1.378(14) . ? C73 C74 1.400(14) . ? C74 C75 1.354(14) . ? C74 C76 1.497(14) . ? C76 C77 1.527(14) . ? C76 C83 1.591(13) . ? C77 C82 1.383(14) . ? C77 C78 1.410(14) . ? C78 C79 1.387(14) . ? C79 C80 1.372(15) . ? C80 C81 1.439(14) . ? C81 C82 1.392(14) . ? C83 C84 1.481(14) . ? C84 C85 1.490(15) . ? C86 C87 1.341(15) . ? C86 C91 1.403(15) . ? C86 C113 1.540(15) . ? C87 C88 1.373(15) . ? C88 C89 1.366(15) . ? C89 C90 1.392(15) . ? C90 C91 1.382(14) . ? C90 C92 1.533(15) . ? C92 C93 1.476(15) . ? C92 C114 1.564(16) . ? C93 C94 1.371(15) . ? C93 C98 1.417(15) . ? C94 C95 1.397(15) . ? C95 C96 1.398(15) . ? C96 C97 1.389(15) . ? C97 C98 1.412(15) . ? C97 C99 1.517(15) . ? C99 C117 1.519(15) . ? C99 C100 1.560(15) . ? C100 C105 1.384(15) . ? C100 C101 1.388(15) . ? C101 C102 1.393(15) . ? C102 C103 1.343(15) . ? C103 C104 1.398(15) . ? C104 C105 1.396(15) . ? C104 C106 1.549(15) . ? C106 C120 1.457(15) . ? C106 C107 1.492(15) . ? C107 C108 1.398(15) . ? C107 C112 1.399(15) . ? C108 C109 1.360(15) . ? C109 C110 1.394(15) . ? C110 C111 1.371(15) . ? C111 C112 1.395(15) . ? C111 C113 1.531(15) . ? C113 C123 1.520(16) . ? C114 C115 1.59(2) . ? C115 C217 1.32(5) . ? C115 C218 1.56(8) . ? C117 C118 1.525(17) . ? C118 C119 1.52(2) . ? C120 C121 1.62(2) . ? C121 C122 1.57(2) . ? C123 C124 1.61(3) . ? C124 C125 1.35(4) . ? C200 C201 1.15(5) . ? 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 O27 Cu1 O22 92.3(3) . . ? O27 Cu1 O23 177.7(3) . . ? O22 Cu1 O23 85.9(3) . . ? O27 Cu1 O26 86.8(3) . . ? O22 Cu1 O26 178.5(3) . . ? O23 Cu1 O26 95.0(3) . . ? O27 Cu1 O42 91.2(4) . . ? O22 Cu1 O42 90.8(3) . . ? O23 Cu1 O42 90.2(4) . . ? O26 Cu1 O42 90.5(4) . . ? O27 Cu1 O41 90.0(4) . . ? O22 Cu1 O41 91.0(4) . . ? O23 Cu1 O41 88.7(4) . . ? O26 Cu1 O41 87.8(4) . . ? O42 Cu1 O41 177.8(4) . . ? C2 O1 Cu12 107.7(7) . 2_676 ? C2 C1 C6 115.5(11) . . ? C2 C1 C14 120.3(11) . . ? C6 C1 C14 124.1(11) . . ? O19 Cu2 O20 86.6(3) . . ? O19 Cu2 O18 91.2(3) . . ? O20 Cu2 O18 175.4(3) . . ? O19 Cu2 O17 174.1(3) . . ? O20 Cu2 O17 95.8(3) . . ? O18 Cu2 O17 86.0(3) . . ? O19 Cu2 O46 96.8(3) . . ? O20 Cu2 O46 92.4(3) . . ? O18 Cu2 O46 91.9(3) . . ? O17 Cu2 O46 88.5(3) . . ? C3 O2 Cu12 108.4(7) . 2_676 ? C3 O2 Cu10 106.9(7) . 2_676 ? Cu12 O2 Cu10 144.6(4) 2_676 2_676 ? C3 C2 O1 118.7(10) . . ? C3 C2 C1 119.5(11) . . ? O1 C2 C1 121.7(11) . . ? O33 Cu3 O10 92.0(3) . 2_676 ? O33 Cu3 O11 177.4(3) . 2_676 ? O10 Cu3 O11 85.7(3) 2_676 2_676 ? O33 Cu3 O32 86.5(3) . . ? O10 Cu3 O32 176.8(3) 2_676 . ? O11 Cu3 O32 95.7(3) 2_676 . ? O33 Cu3 O53 90.5(3) . . ? O10 Cu3 O53 90.7(3) 2_676 . ? O11 Cu3 O53 90.8(3) 2_676 . ? O32 Cu3 O53 92.2(3) . . ? O33 Cu3 O50 89.3(3) . . ? O10 Cu3 O50 90.0(3) 2_676 . ? O11 Cu3 O50 89.4(3) 2_676 . ? O32 Cu3 O50 87.1(3) . . ? O53 Cu3 O50 179.3(4) . . ? C4 O3 Cu10 110.8(6) . 2_676 ? C4 C3 C2 123.5(11) . . ? C4 C3 O2 118.7(12) . . ? C2 C3 O2 117.8(11) . . ? O7 Cu4 O6 90.8(3) . . ? O7 Cu4 O5 177.8(3) . . ? O6 Cu4 O5 87.0(3) . . ? O7 Cu4 O8 86.2(3) . . ? O6 Cu4 O8 177.0(3) . . ? O5 Cu4 O8 95.9(3) . . ? O7 Cu4 O56 92.2(7) . . ? O6 Cu4 O56 89.5(7) . . ? O5 Cu4 O56 88.1(7) . . ? O8 Cu4 O56 90.7(7) . . ? C9 O4 Cu8 108.8(6) . . ? O3 C4 C3 117.0(10) . . ? O3 C4 C5 123.4(11) . . ? C3 C4 C5 119.6(12) . . ? O49 Cu5 O13 91.3(3) . . ? O49 Cu5 O12 93.3(3) . 2_676 ? O13 Cu5 O12 90.8(3) . 2_676 ? O49 Cu5 O14 89.8(3) . . ? O13 Cu5 O14 85.9(3) . . ? O12 Cu5 O14 175.6(3) 2_676 . ? O49 Cu5 O11 91.9(3) . 2_676 ? O13 Cu5 O11 175.9(3) . 2_676 ? O12 Cu5 O11 86.4(3) 2_676 2_676 ? O14 Cu5 O11 96.6(3) . 2_676 ? O49 Cu5 O52 178.8(4) . . ? O13 Cu5 O52 88.4(3) . . ? O12 Cu5 O52 87.9(3) 2_676 . ? O14 Cu5 O52 89.0(3) . . ? O11 Cu5 O52 88.5(3) 2_676 . ? C10 O5 Cu8 108.6(6) . . ? C10 O5 Cu4 107.3(6) . . ? Cu8 O5 Cu4 143.5(4) . . ? C4 C5 C6 118.1(11) . . ? C4 C5 C7 121.9(12) . . ? C6 C5 C7 119.9(11) . . ? O20 Cu6 O29 97.4(3) . . ? O20 Cu6 O21 86.4(3) . . ? O29 Cu6 O21 173.1(3) . . ? O20 Cu6 O28 173.2(3) . . ? O29 Cu6 O28 86.3(3) . . ? O21 Cu6 O28 89.4(3) . . ? O20 Cu6 O45 95.3(4) . . ? O29 Cu6 O45 92.4(4) . . ? O21 Cu6 O45 93.0(4) . . ? O28 Cu6 O45 90.3(4) . . ? C11 O6 Cu4 109.8(6) . . ? C5 C6 C1 123.7(10) . . ? O31 Cu7 O15 92.4(3) . . ? O31 Cu7 O14 178.1(3) . . ? O15 Cu7 O14 85.6(3) . . ? O31 Cu7 O32 86.1(3) . . ? O15 Cu7 O32 177.4(3) . . ? O14 Cu7 O32 95.9(3) . . ? O31 Cu7 O51 89.2(3) . . ? O15 Cu7 O51 91.0(3) . . ? O14 Cu7 O51 90.8(3) . . ? O32 Cu7 O51 91.0(3) . . ? O31 Cu7 O48 90.5(4) . . ? O15 Cu7 O48 89.7(4) . . ? O14 Cu7 O48 89.5(4) . . ? O32 Cu7 O48 88.3(4) . . ? O51 Cu7 O48 179.3(3) . . ? C26 O7 Cu4 110.2(6) . . ? C18 C7 C5 114.2(9) . . ? C18 C7 C8 113.5(9) . . ? C5 C7 C8 109.1(8) . . ? O5 Cu8 O35 97.4(3) . 2_676 ? O5 Cu8 O36 173.5(3) . 2_676 ? O35 Cu8 O36 86.4(3) 2_676 2_676 ? O5 Cu8 O4 86.8(3) . . ? O35 Cu8 O4 173.3(3) 2_676 . ? O36 Cu8 O4 89.0(3) 2_676 . ? O5 Cu8 O55 97.1(4) . . ? O35 Cu8 O55 81.3(4) 2_676 . ? O36 Cu8 O55 88.7(4) 2_676 . ? O4 Cu8 O55 103.4(4) . . ? C27 O8 Cu11 109.3(6) . . ? C27 O8 Cu4 107.4(6) . . ? Cu11 O8 Cu4 142.3(4) . . ? C9 C8 C13 117.6(10) . . ? C9 C8 C7 120.2(10) . . ? C13 C8 C7 122.1(10) . . ? O17 Cu9 O29 98.5(3) . . ? O17 Cu9 O16 86.4(3) . . ? O29 Cu9 O16 174.3(3) . . ? O17 Cu9 O30 174.1(3) . . ? O29 Cu9 O30 86.2(3) . . ? O16 Cu9 O30 88.8(3) . . ? O17 Cu9 O47 88.3(4) . . ? O29 Cu9 O47 91.1(4) . . ? O16 Cu9 O47 92.1(4) . . ? O30 Cu9 O47 95.4(4) . . ? O17 Cu9 O44 93.7(10) . . ? O29 Cu9 O44 75.5(10) . . ? O16 Cu9 O44 101.2(10) . . ? O30 Cu9 O44 83.9(10) . . ? O47 Cu9 O44 166.6(10) . . ? C28 O9 Cu11 108.2(6) . . ? O4 C9 C8 123.4(10) . . ? O4 C9 C10 115.6(10) . . ? C8 C9 C10 121.0(11) . . ? O25 Cu10 O3 93.1(3) . 2_676 ? O25 Cu10 O26 86.0(3) . . ? O3 Cu10 O26 178.6(3) 2_676 . ? O25 Cu10 O2 178.7(3) . 2_676 ? O3 Cu10 O2 86.1(3) 2_676 2_676 ? O26 Cu10 O2 94.8(3) . 2_676 ? O25 Cu10 O40 91.0(4) . . ? O3 Cu10 O40 90.7(4) 2_676 . ? O26 Cu10 O40 90.3(4) . . ? O2 Cu10 O40 90.0(4) 2_676 . ? O25 Cu10 O39 90.1(4) . . ? O3 Cu10 O39 90.6(4) 2_676 . ? O26 Cu10 O39 88.4(4) . . ? O2 Cu10 O39 88.9(4) 2_676 . ? O40 Cu10 O39 178.3(4) . . ? C33 O10 Cu3 109.6(6) . 2_676 ? O5 C10 C11 121.0(10) . . ? O5 C10 C9 119.8(11) . . ? C11 C10 C9 119.1(11) . . ? O35 Cu11 O8 98.5(3) 2_676 . ? O35 Cu11 O34 85.6(3) 2_676 2_676 ? O8 Cu11 O34 172.9(3) . 2_676 ? O35 Cu11 O9 172.7(3) 2_676 . ? O8 Cu11 O9 85.7(3) . . ? O34 Cu11 O9 89.6(3) 2_676 . ? O35 Cu11 O54 92.3(3) 2_676 . ? O8 Cu11 O54 92.8(3) . . ? O34 Cu11 O54 92.8(3) 2_676 . ? O9 Cu11 O54 93.5(3) . . ? C34 O11 Cu3 108.0(6) . 2_676 ? C34 O11 Cu5 108.1(6) . 2_676 ? Cu3 O11 Cu5 143.9(4) 2_676 2_676 ? C10 C11 C12 122.0(10) . . ? C10 C11 O6 114.7(10) . . ? C12 C11 O6 123.3(10) . . ? O37 Cu12 O2 89.9(4) . 2_676 ? O37 Cu12 O23 89.7(4) . . ? O2 Cu12 O23 96.4(3) 2_676 . ? O37 Cu12 O24 92.0(4) . . ? O2 Cu12 O24 176.5(3) 2_676 . ? O23 Cu12 O24 86.5(3) . . ? O37 Cu12 O38 179.0(4) . . ? O2 Cu12 O38 89.1(4) 2_676 . ? O23 Cu12 O38 90.1(4) . . ? O24 Cu12 O38 89.1(4) . . ? O37 Cu12 O1 92.3(4) . 2_676 ? O2 Cu12 O1 87.0(3) 2_676 2_676 ? O23 Cu12 O1 176.0(3) . 2_676 ? O24 Cu12 O1 89.9(3) . 2_676 ? O38 Cu12 O1 87.9(4) . 2_676 ? C35 O12 Cu5 108.8(6) . 2_676 ? C11 C12 C13 117.9(10) . . ? C11 C12 C66 121.1(9) . . ? C13 C12 C66 121.0(10) . . ? C49 O13 Cu5 109.8(5) . . ? C12 C13 C8 122.4(10) . . ? C50 O14 Cu7 108.9(5) . . ? C50 O14 Cu5 108.1(5) . . ? Cu7 O14 Cu5 143.0(4) . . ? C1 C14 C15 114.7(10) . . ? C1 C14 C48 110.7(7) . . ? C15 C14 C48 112.2(9) . . ? C51 O15 Cu7 111.0(5) . . ? C16 C15 C14 115.3(11) . . ? C56 O16 Cu9 108.8(5) . . ? C15 C16 C17 113.5(12) . . ? C57 O17 Cu9 109.1(5) . . ? C57 O17 Cu2 106.9(5) . . ? Cu9 O17 Cu2 141.4(4) . . ? C58 O18 Cu2 108.4(5) . . ? C7 C18 C21 112.5(12) . . ? C7 C18 C22 115.5(16) . . ? C21 C18 C22 100.4(18) . . ? C71 O19 Cu2 109.9(5) . . ? C72 O20 Cu6 109.0(5) . . ? C72 O20 Cu2 107.0(5) . . ? Cu6 O20 Cu2 143.0(4) . . ? C73 O21 Cu6 109.2(4) . . ? C18 C21 C20 101.0(19) . . ? C78 O22 Cu1 110.9(5) . . ? C18 C22 C23 107(3) . . ? C79 O23 Cu12 108.9(6) . . ? C79 O23 Cu1 107.2(6) . . ? Cu12 O23 Cu1 144.0(4) . . ? C80 O24 Cu12 107.9(5) . . ? C70 C24 C25 109.6(7) . . ? C70 C24 C38 116.4(8) . . ? C25 C24 C38 112.3(9) . . ? C87 O25 Cu10 110.8(5) . . ? C30 C25 C26 116.5(10) . . ? C30 C25 C24 123.0(10) . . ? C26 C25 C24 120.4(11) . . ? C88 O26 Cu10 107.8(5) . . ? C88 O26 Cu1 107.0(5) . . ? Cu10 O26 Cu1 145.2(4) . . ? C27 C26 O7 115.5(9) . . ? C27 C26 C25 121.0(10) . . ? O7 C26 C25 123.6(11) . . ? C89 O27 Cu1 109.4(6) . . ? C28 C27 C26 120.2(10) . . ? C28 C27 O8 119.4(9) . . ? C26 C27 O8 120.4(10) . . ? C94 O28 Cu6 110.0(5) . . ? C27 C28 O9 116.8(9) . . ? C27 C28 C29 122.5(10) . . ? O9 C28 C29 120.6(11) . . ? C95 O29 Cu9 110.1(5) . . ? C95 O29 Cu6 107.8(5) . . ? Cu9 O29 Cu6 141.3(4) . . ? C30 C29 C28 115.4(11) . . ? C30 C29 C31 124.0(9) . . ? C28 C29 C31 120.5(10) . . ? C96 O30 Cu9 109.8(5) . . ? C25 C30 C29 124.3(10) . . ? C101 O31 Cu7 111.2(5) . . ? C32 C31 C41 114.1(9) . . ? C32 C31 C29 106.8(8) . . ? C41 C31 C29 110.7(9) . . ? C102 O32 Cu3 107.0(5) . . ? C102 O32 Cu7 107.6(5) . . ? Cu3 O32 Cu7 144.4(4) . . ? C37 C32 C33 116.1(10) . . ? C37 C32 C31 123.8(9) . . ? C33 C32 C31 120.0(10) . . ? C103 O33 Cu3 109.4(5) . . ? C34 C33 O10 115.9(9) . . ? C34 C33 C32 122.7(10) . . ? O10 C33 C32 121.3(10) . . ? C108 O34 Cu11 109.7(5) . 2_676 ? C33 C34 O11 120.4(9) . . ? C33 C34 C35 120.9(9) . . ? O11 C34 C35 118.4(9) . . ? C109 O35 Cu11 109.7(5) . 2_676 ? C109 O35 Cu8 107.9(5) . 2_676 ? Cu11 O35 Cu8 139.9(4) 2_676 2_676 ? O12 C35 C34 118.0(9) . . ? O12 C35 C36 123.4(11) . . ? C34 C35 C36 118.6(11) . . ? C110 O36 Cu8 109.9(5) . 2_676 ? C37 C36 C35 118.0(10) . . ? C37 C36 C44 123.3(9) . . ? C35 C36 C44 118.5(11) . . ? C36 C37 C32 123.5(10) . . ? C39 C38 C24 114.1(10) . . ? C38 C39 C40 114.1(13) . . ? C42 C41 C31 110.7(9) . . ? C41 C42 C43 108.0(11) . . ? C81 C44 C36 111.5(7) . . ? C81 C44 C45 112.6(8) . . ? C36 C44 C45 112.8(9) . . ? C203 O45 Cu6 120.9(14) . . ? C46 C45 C44 112.0(11) . . ? C202 O46 Cu2 122.5(10) . . ? C45 C46 C47 111.6(14) . . ? C201 O47 C200 71(3) . . ? C201 O47 Cu9 124(3) . . ? C200 O47 Cu9 126(2) . . ? C53 C48 C49 118.7(10) . . ? C53 C48 C14 122.3(10) . . ? C49 C48 C14 118.8(9) . . ? C50 C49 O13 117.2(10) . . ? C50 C49 C48 118.2(10) . . ? O13 C49 C48 124.5(10) . . ? C49 C50 C51 123.9(10) . . ? C49 C50 O14 118.8(9) . . ? C51 C50 O14 117.3(10) . . ? C204 O51 Cu7 121.9(13) . . ? C52 C51 C50 118.4(11) . . ? C52 C51 O15 124.7(9) . . ? C50 C51 O15 116.9(10) . . ? C51 C52 C53 119.2(10) . . ? C51 C52 C54 121.1(10) . . ? C53 C52 C54 119.5(10) . . ? C48 C53 C52 121.5(10) . . ? C210 O54 Cu11 122.5(14) . . ? C55 C54 C61 113.3(9) . . ? C55 C54 C52 110.2(9) . . ? C61 C54 C52 114.5(9) . . ? C60 C55 C56 116.2(10) . . ? C60 C55 C54 123.6(10) . . ? C56 C55 C54 120.1(11) . . ? C57 C56 O16 115.5(9) . . ? C57 C56 C55 120.6(11) . . ? O16 C56 C55 123.9(10) . . ? C58 C57 O17 120.1(9) . . ? C58 C57 C56 120.6(10) . . ? O17 C57 C56 119.2(10) . . ? C57 C58 O18 117.3(9) . . ? C57 C58 C59 121.2(9) . . ? O18 C58 C59 121.5(10) . . ? C60 C59 C58 115.6(11) . . ? C60 C59 C66 124.3(10) . . ? C58 C59 C66 120.1(10) . . ? C59 C60 C55 125.8(10) . . ? C54 C61 C62 113.2(18) . . ? C54 C61 C64 109.9(10) . . ? C62 C61 C64 88(2) . . ? C61 C62 C63 113(4) . . ? C61 C64 C65 115.9(14) . . ? C59 C66 C12 109.0(7) . . ? C59 C66 C67 113.5(10) . . ? C12 C66 C67 113.9(8) . . ? C68 C67 C66 113.4(10) . . ? C67 C68 C69 109.6(15) . . ? C71 C70 C75 114.4(10) . . ? C71 C70 C24 121.5(9) . . ? C75 C70 C24 124.1(9) . . ? C72 C71 O19 116.2(9) . . ? C72 C71 C70 120.6(9) . . ? O19 C71 C70 123.1(10) . . ? C71 C72 C73 122.0(10) . . ? C71 C72 O20 119.9(9) . . ? C73 C72 O20 118.2(10) . . ? C72 C73 O21 116.6(9) . . ? C72 C73 C74 120.0(10) . . ? O21 C73 C74 123.4(9) . . ? C75 C74 C73 116.1(9) . . ? C75 C74 C76 124.4(10) . . ? C73 C74 C76 119.4(11) . . ? C74 C75 C70 126.8(10) . . ? C74 C76 C77 110.5(9) . . ? C74 C76 C83 114.3(9) . . ? C77 C76 C83 112.1(9) . . ? C82 C77 C78 120.5(10) . . ? C82 C77 C76 122.6(9) . . ? C78 C77 C76 116.8(11) . . ? O22 C78 C79 116.4(10) . . ? O22 C78 C77 126.4(10) . . ? C79 C78 C77 117.2(10) . . ? C80 C79 C78 123.2(10) . . ? C80 C79 O23 117.4(10) . . ? C78 C79 O23 119.4(10) . . ? C79 C80 O24 119.1(9) . . ? C79 C80 C81 119.8(10) . . ? O24 C80 C81 120.9(11) . . ? C82 C81 C80 116.7(10) . . ? C82 C81 C44 122.2(9) . . ? C80 C81 C44 120.9(9) . . ? C77 C82 C81 122.6(10) . . ? C84 C83 C76 114.1(9) . . ? C83 C84 C85 111.0(11) . . ? C87 C86 C91 118.2(10) . . ? C87 C86 C113 121.3(11) . . ? C91 C86 C113 120.5(12) . . ? C86 C87 C88 120.1(10) . . ? C86 C87 O25 123.4(10) . . ? C88 C87 O25 116.4(11) . . ? C89 C88 C87 122.8(11) . . ? C89 C88 O26 118.5(10) . . ? C87 C88 O26 118.7(10) . . ? C88 C89 C90 118.5(11) . . ? C88 C89 O27 118.0(11) . . ? C90 C89 O27 123.5(10) . . ? C91 C90 C89 117.9(10) . . ? C91 C90 C92 122.9(12) . . ? C89 C90 C92 118.8(11) . . ? C90 C91 C86 122.4(11) . . ? C93 C92 C90 112.0(9) . . ? C93 C92 C114 113.5(10) . . ? C90 C92 C114 113.6(10) . . ? C94 C93 C98 117.4(10) . . ? C94 C93 C92 121.3(11) . . ? C98 C93 C92 121.2(11) . . ? C93 C94 O28 124.6(10) . . ? C93 C94 C95 121.1(11) . . ? O28 C94 C95 114.2(10) . . ? O29 C95 C96 118.4(10) . . ? O29 C95 C94 121.0(10) . . ? C96 C95 C94 120.6(11) . . ? C97 C96 O30 123.7(10) . . ? C97 C96 C95 120.9(11) . . ? O30 C96 C95 115.4(10) . . ? C96 C97 C98 116.9(11) . . ? C96 C97 C99 120.1(11) . . ? C98 C97 C99 123.1(12) . . ? C97 C98 C93 123.2(11) . . ? C97 C99 C117 113.1(10) . . ? C97 C99 C100 109.1(9) . . ? C117 C99 C100 112.2(10) . . ? C105 C100 C101 118.4(10) . . ? C105 C100 C99 122.9(10) . . ? C101 C100 C99 118.4(11) . . ? C100 C101 O31 124.5(10) . . ? C100 C101 C102 119.7(11) . . ? O31 C101 C102 115.6(10) . . ? C103 C102 C101 121.7(10) . . ? C103 C102 O32 119.3(10) . . ? C101 C102 O32 118.9(11) . . ? C102 C103 O33 117.2(10) . . ? C102 C103 C104 119.7(10) . . ? O33 C103 C104 123.0(10) . . ? C105 C104 C103 119.0(11) . . ? C105 C104 C106 120.8(11) . . ? C103 C104 C106 120.2(11) . . ? C100 C105 C104 121.2(11) . . ? C120 C106 C107 113.3(11) . . ? C120 C106 C104 114.9(10) . . ? C107 C106 C104 108.5(9) . . ? C108 C107 C112 113.5(11) . . ? C108 C107 C106 121.2(10) . . ? C112 C107 C106 125.0(11) . . ? C109 C108 C107 122.0(11) . . ? C109 C108 O34 115.5(10) . . ? C107 C108 O34 122.5(10) . . ? C108 C109 C110 122.7(10) . . ? C108 C109 O35 118.6(10) . . ? C110 C109 O35 118.7(11) . . ? C111 C110 O36 125.6(10) . . ? C111 C110 C109 118.1(11) . . ? O36 C110 C109 116.2(10) . . ? C110 C111 C112 117.8(11) . . ? C110 C111 C113 119.4(12) . . ? C112 C111 C113 122.5(11) . . ? C111 C112 C107 125.7(11) . . ? C123 C113 C111 112.9(10) . . ? C123 C113 C86 115.3(10) . . ? C111 C113 C86 110.7(9) . . ? C92 C114 C115 113.5(12) . . ? C217 C115 C218 111(4) . . ? C217 C115 C114 106(3) . . ? C218 C115 C114 121(3) . . ? C99 C117 C118 109.8(11) . . ? C119 C118 C117 110.9(15) . . ? C106 C120 C121 111.0(12) . . ? C122 C121 C120 114.1(16) . . ? C113 C123 C124 119.3(15) . . ? C125 C124 C123 106(3) . . ? O47 C200 C201 49(3) . . ? O47 C201 C200 60(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 20.30 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.021 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.124