# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Andrey Yakovenko' _publ_contact_author_email ayakovenko@mail.chem.tamu.edu loop_ _publ_author_name 'Weigang Lu' 'Daqiang Yuan' 'Andrey A. Yakovenko' 'Hong-Cai Zhou' data_MOP1a _database_code_depnum_ccdc_archive 'CCDC 797901' #TrackingRef 'MOP-1a_luke05.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H30 Cu2 O11' _chemical_formula_weight 933.82 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' 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 13.9831(9) _cell_length_b 30.543(2) _cell_length_c 27.9915(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.349(3) _cell_angle_gamma 90.00 _cell_volume 11720.9(13) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4301 _cell_measurement_theta_min 2.392 _cell_measurement_theta_max 20.042 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3808 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8485 _exptl_absorpt_correction_T_max 0.8800 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54362 _diffrn_reflns_av_R_equivalents 0.0915 _diffrn_reflns_av_sigmaI/netI 0.1101 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.54 _reflns_number_total 12065 _reflns_number_gt 6088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.1026P)^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 12065 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1669 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 0.800 _refine_ls_restrained_S_all 0.800 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.004 2140 834 ' ' 2 1.000 0.500 -0.082 2140 834 ' ' _platon_squeeze_details ; ; 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 0.25831(4) 0.053943(14) 0.651350(17) 0.03727(16) Uani 1 1 d . . . Cu2 Cu 0.25636(4) 0.123904(14) 0.597828(17) 0.03684(16) Uani 1 1 d . . . O1 O 0.1960(2) 0.02739(8) 0.58910(9) 0.0454(7) Uani 1 1 d . . . O2 O 0.2070(2) 0.08636(8) 0.54316(9) 0.0431(7) Uani 1 1 d . . . O3 O 0.2507(2) 0.00601(9) 0.18837(10) 0.0515(8) Uani 1 1 d . . . H3A H 0.2932 0.0189 0.2076 0.062 Uiso 1 1 d R . . O4 O 0.1957(2) 0.34842(8) 0.33954(10) 0.0420(7) Uani 1 1 d . . . O5 O 0.1781(2) 0.40949(8) 0.29401(9) 0.0427(7) Uani 1 1 d . . . O6 O 0.3872(2) 0.04277(8) 0.63547(10) 0.0438(7) Uani 1 1 d . . . O7 O 0.3889(2) 0.10573(8) 0.59420(9) 0.0388(7) Uani 1 1 d . . . O8 O 1.0597(3) 0.19449(14) 0.41400(19) 0.1165(16) Uani 1 1 d . . . H8A H 1.1130 0.1875 0.4083 0.140 Uiso 1 1 d R . . O9 O 0.3766(2) 0.36798(9) 0.39151(10) 0.0464(7) Uani 1 1 d . . . O10 O 0.3676(2) 0.42431(8) 0.33851(10) 0.0436(7) Uani 1 1 d . . . O11 O 0.2610(2) 0.18227(9) 0.55501(11) 0.0635(9) Uani 1 1 d . . . H11A H 0.3136 0.1958 0.5538 0.076 Uiso 1 1 d R . . H11B H 0.2256 0.2045 0.5571 0.076 Uiso 1 1 d R . . C1 C 0.1865(3) 0.04655(13) 0.54857(15) 0.0407(10) Uani 1 1 d . . . C2 C 0.1329(3) 0.04275(13) 0.45907(14) 0.0410(10) Uani 1 1 d . . . H2 H 0.1555 0.0720 0.4577 0.049 Uiso 1 1 calc R . . C3 C 0.1429(3) 0.02211(12) 0.50350(15) 0.0422(10) Uani 1 1 d . . . C4 C 0.1080(3) -0.02042(13) 0.50538(16) 0.0488(11) Uani 1 1 d . . . H4 H 0.1159 -0.0352 0.5357 0.059 Uiso 1 1 calc R . . C5 C 0.0621(3) -0.04103(14) 0.46348(16) 0.0489(12) Uani 1 1 d . . . H5 H 0.0368 -0.0697 0.4652 0.059 Uiso 1 1 calc R . . C6 C 0.0524(3) -0.02045(13) 0.41888(16) 0.0480(11) Uani 1 1 d . . . H6 H 0.0199 -0.0350 0.3902 0.058 Uiso 1 1 calc R . . C7 C 0.0899(3) 0.02133(14) 0.41561(15) 0.0442(11) Uani 1 1 d . . . C8 C 0.0898(3) 0.04128(13) 0.37032(16) 0.0472(11) Uani 1 1 d . . . C9 C 0.1007(4) 0.05739(13) 0.33343(16) 0.0517(12) Uani 1 1 d . . . C10 C 0.1177(3) 0.07550(13) 0.28854(15) 0.0480(11) Uani 1 1 d . . . C11 C 0.1355(4) 0.04900(13) 0.25195(16) 0.0544(13) Uani 1 1 d . . . H11 H 0.1361 0.0182 0.2564 0.065 Uiso 1 1 calc R . . C12 C 0.1528(4) 0.06587(14) 0.20870(16) 0.0540(13) Uani 1 1 d . . . C13 C 0.1498(3) 0.11071(13) 0.20174(16) 0.0513(12) Uani 1 1 d . . . H13 H 0.1619 0.1226 0.1722 0.062 Uiso 1 1 calc R . . C14 C 0.1291(3) 0.13848(13) 0.23789(15) 0.0480(11) Uani 1 1 d . . . C15 C 0.1154(3) 0.12124(13) 0.28178(16) 0.0492(12) Uani 1 1 d . . . H15 H 0.1045 0.1401 0.3072 0.059 Uiso 1 1 calc R . . C16 C 0.1747(4) 0.03524(14) 0.17005(15) 0.0678(16) Uani 1 1 d . . . H16A H 0.1152 0.0183 0.1563 0.081 Uiso 1 1 calc R . . H16B H 0.1928 0.0526 0.1433 0.081 Uiso 1 1 calc R . . C17 C 0.1233(4) 0.18478(13) 0.22977(16) 0.0539(13) Uani 1 1 d . . . C18 C 0.1142(4) 0.22333(14) 0.22485(15) 0.0526(12) Uani 1 1 d . . . C19 C 0.1379(3) 0.29660(12) 0.25921(15) 0.0443(11) Uani 1 1 d . . . H19 H 0.1658 0.2836 0.2896 0.053 Uiso 1 1 calc R . . C20 C 0.1032(3) 0.27029(13) 0.21982(16) 0.0472(11) Uani 1 1 d . . . C21 C 0.0585(3) 0.28982(13) 0.17570(16) 0.0472(11) Uani 1 1 d . . . H21 H 0.0326 0.2721 0.1483 0.057 Uiso 1 1 calc R . . C22 C 0.0520(3) 0.33459(13) 0.17202(15) 0.0435(10) Uani 1 1 d . . . H22 H 0.0210 0.3477 0.1422 0.052 Uiso 1 1 calc R . . C23 C 0.0903(3) 0.36078(13) 0.21135(15) 0.0392(10) Uani 1 1 d . . . H23 H 0.0875 0.3917 0.2082 0.047 Uiso 1 1 calc R . . C24 C 0.1329(3) 0.34192(11) 0.25546(14) 0.0333(9) Uani 1 1 d . . . C25 C 0.1711(3) 0.36888(13) 0.29960(15) 0.0364(9) Uani 1 1 d . . . C26 C 0.4277(3) 0.07111(13) 0.61357(14) 0.0386(10) Uani 1 1 d . . . C27 C 0.5745(3) 0.08967(13) 0.57974(15) 0.0426(10) Uani 1 1 d . . . H27 H 0.5367 0.1115 0.5605 0.051 Uiso 1 1 calc R . . C28 C 0.5311(3) 0.06307(13) 0.60992(15) 0.0430(11) Uani 1 1 d . . . C29 C 0.5870(4) 0.03132(14) 0.63779(18) 0.0590(13) Uani 1 1 d . . . H29 H 0.5573 0.0125 0.6577 0.071 Uiso 1 1 calc R . . C30 C 0.6829(4) 0.02652(17) 0.63719(19) 0.0701(15) Uani 1 1 d . . . H30 H 0.7208 0.0052 0.6572 0.084 Uiso 1 1 calc R . . C31 C 0.7256(4) 0.05314(16) 0.6069(2) 0.0695(15) Uani 1 1 d . . . H31 H 0.7929 0.0499 0.6063 0.083 Uiso 1 1 calc R . . C32 C 0.6700(4) 0.08480(14) 0.57736(17) 0.0533(12) Uani 1 1 d . . . C33 C 0.7150(3) 0.11203(15) 0.54524(19) 0.0557(13) Uani 1 1 d . . . C34 C 0.7490(4) 0.13393(15) 0.51746(19) 0.0613(14) Uani 1 1 d . . . C35 C 0.7888(4) 0.15881(16) 0.4814(2) 0.0662(15) Uani 1 1 d . . . C36 C 0.8757(4) 0.14695(16) 0.4692(2) 0.0721(16) Uani 1 1 d . . . H36 H 0.9103 0.1224 0.4848 0.086 Uiso 1 1 calc R . . C37 C 0.9137(4) 0.16987(17) 0.4349(2) 0.0818(18) Uani 1 1 d . . . C38 C 0.8595(4) 0.20401(16) 0.4112(2) 0.0782(17) Uani 1 1 d . . . H38 H 0.8823 0.2189 0.3857 0.094 Uiso 1 1 calc R . . C39 C 0.7733(4) 0.21699(15) 0.4235(2) 0.0634(14) Uani 1 1 d . . . C40 C 0.7355(4) 0.19421(15) 0.45830(19) 0.0602(13) Uani 1 1 d . . . H40 H 0.6750 0.2024 0.4663 0.072 Uiso 1 1 calc R . . C41 C 1.0096(5) 0.15774(19) 0.4232(3) 0.119(3) Uani 1 1 d . . . H41A H 1.0487 0.1415 0.4509 0.142 Uiso 1 1 calc R . . H41B H 0.9991 0.1383 0.3943 0.142 Uiso 1 1 calc R . . C42 C 0.7229(4) 0.25447(17) 0.4000(2) 0.0701(16) Uani 1 1 d . . . C43 C 0.6828(4) 0.28591(17) 0.38019(19) 0.0624(14) Uani 1 1 d . . . C44 C 0.5497(3) 0.33975(14) 0.37040(16) 0.0528(12) Uani 1 1 d . . . H44 H 0.5234 0.3250 0.3948 0.063 Uiso 1 1 calc R . . C45 C 0.6354(3) 0.32425(14) 0.35785(17) 0.0505(12) Uani 1 1 d . . . C46 C 0.6746(4) 0.34666(15) 0.32267(17) 0.0582(13) Uani 1 1 d . . . H46 H 0.7325 0.3364 0.3135 0.070 Uiso 1 1 calc R . . C47 C 0.6291(4) 0.38368(16) 0.30140(18) 0.0606(13) Uani 1 1 d . . . H47 H 0.6571 0.3993 0.2782 0.073 Uiso 1 1 calc R . . C48 C 0.5432(3) 0.39856(14) 0.31319(15) 0.0479(11) Uani 1 1 d . . . H48 H 0.5119 0.4239 0.2978 0.057 Uiso 1 1 calc R . . C49 C 0.5030(3) 0.37597(13) 0.34794(15) 0.0415(10) Uani 1 1 d . . . C50 C 0.4087(3) 0.39024(13) 0.36014(15) 0.0413(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0453(3) 0.0268(2) 0.0412(3) 0.0057(2) 0.0120(2) -0.0001(2) Cu2 0.0447(3) 0.0282(2) 0.0398(3) 0.0061(2) 0.0137(2) 0.0014(2) O1 0.062(2) 0.0360(15) 0.0383(17) 0.0039(12) 0.0090(15) -0.0002(14) O2 0.053(2) 0.0374(16) 0.0392(16) 0.0064(12) 0.0094(14) -0.0081(13) O3 0.049(2) 0.0436(16) 0.059(2) -0.0293(14) 0.0037(16) 0.0058(14) O4 0.055(2) 0.0297(14) 0.0421(17) 0.0007(12) 0.0109(14) 0.0004(13) O5 0.053(2) 0.0278(14) 0.0464(17) 0.0060(12) 0.0088(14) 0.0009(13) O6 0.0481(19) 0.0359(15) 0.0511(18) 0.0050(13) 0.0185(15) 0.0027(13) O7 0.0459(18) 0.0317(14) 0.0428(16) 0.0054(12) 0.0184(14) 0.0062(13) O8 0.073(3) 0.096(3) 0.195(5) 0.026(3) 0.063(3) 0.004(2) O9 0.047(2) 0.0448(17) 0.0507(18) 0.0111(14) 0.0164(15) 0.0010(14) O10 0.0484(19) 0.0353(15) 0.0481(17) 0.0060(13) 0.0116(15) 0.0029(13) O11 0.071(2) 0.0455(18) 0.077(2) 0.0184(16) 0.0223(19) -0.0075(16) C1 0.044(3) 0.039(2) 0.042(3) 0.0048(19) 0.017(2) -0.001(2) C2 0.047(3) 0.033(2) 0.044(2) -0.0012(18) 0.012(2) 0.0047(19) C3 0.051(3) 0.034(2) 0.044(3) 0.0030(18) 0.018(2) -0.001(2) C4 0.060(3) 0.045(3) 0.044(3) 0.007(2) 0.016(2) -0.004(2) C5 0.059(3) 0.037(2) 0.050(3) -0.003(2) 0.009(2) -0.004(2) C6 0.059(3) 0.040(2) 0.047(3) -0.004(2) 0.015(2) -0.001(2) C7 0.046(3) 0.050(3) 0.039(2) -0.004(2) 0.013(2) 0.003(2) C8 0.060(3) 0.040(2) 0.042(3) -0.008(2) 0.011(2) -0.001(2) C9 0.075(4) 0.040(2) 0.044(3) -0.003(2) 0.022(3) -0.002(2) C10 0.068(3) 0.042(2) 0.034(2) -0.0005(18) 0.009(2) 0.003(2) C11 0.083(4) 0.032(2) 0.049(3) -0.006(2) 0.014(3) 0.007(2) C12 0.082(4) 0.040(2) 0.040(3) -0.0046(19) 0.015(3) 0.015(2) C13 0.077(4) 0.035(2) 0.046(3) -0.0025(19) 0.022(2) 0.009(2) C14 0.064(3) 0.036(2) 0.044(3) -0.0050(19) 0.011(2) 0.005(2) C15 0.067(3) 0.037(2) 0.046(3) -0.0096(19) 0.017(2) 0.000(2) C16 0.132(5) 0.040(2) 0.037(3) 0.000(2) 0.030(3) 0.029(3) C17 0.082(4) 0.033(2) 0.049(3) -0.0025(19) 0.019(3) 0.007(2) C18 0.083(4) 0.038(3) 0.039(3) -0.0060(19) 0.019(2) -0.001(2) C19 0.062(3) 0.034(2) 0.041(2) 0.0005(18) 0.021(2) 0.005(2) C20 0.065(3) 0.035(2) 0.046(3) -0.0070(19) 0.024(2) -0.005(2) C21 0.054(3) 0.045(3) 0.045(3) -0.011(2) 0.013(2) 0.000(2) C22 0.043(3) 0.047(3) 0.045(3) 0.004(2) 0.017(2) 0.002(2) C23 0.045(3) 0.032(2) 0.045(2) 0.0011(18) 0.019(2) -0.0018(18) C24 0.039(3) 0.0268(19) 0.037(2) 0.0010(16) 0.015(2) -0.0018(17) C25 0.027(2) 0.039(2) 0.045(3) -0.0007(19) 0.012(2) 0.0003(18) C26 0.046(3) 0.034(2) 0.036(2) -0.0053(18) 0.011(2) -0.005(2) C27 0.045(3) 0.042(2) 0.045(3) 0.0031(19) 0.019(2) 0.003(2) C28 0.048(3) 0.037(2) 0.045(3) -0.0003(19) 0.012(2) 0.003(2) C29 0.063(4) 0.047(3) 0.073(3) 0.013(2) 0.027(3) 0.008(2) C30 0.059(4) 0.076(4) 0.082(4) 0.023(3) 0.031(3) 0.012(3) C31 0.056(4) 0.064(3) 0.094(4) 0.012(3) 0.027(3) 0.016(3) C32 0.051(3) 0.049(3) 0.064(3) 0.000(2) 0.022(3) 0.006(2) C33 0.042(3) 0.052(3) 0.077(4) 0.002(2) 0.020(3) 0.006(2) C34 0.056(3) 0.048(3) 0.083(4) 0.020(3) 0.020(3) 0.004(2) C35 0.053(3) 0.058(3) 0.098(4) 0.020(3) 0.041(3) 0.001(3) C36 0.069(4) 0.051(3) 0.105(4) 0.025(3) 0.038(3) 0.012(3) C37 0.062(4) 0.061(3) 0.136(5) 0.029(3) 0.052(4) 0.024(3) C38 0.078(4) 0.055(3) 0.118(5) 0.026(3) 0.058(4) 0.008(3) C39 0.054(3) 0.052(3) 0.092(4) 0.015(3) 0.034(3) 0.008(2) C40 0.044(3) 0.053(3) 0.090(4) 0.017(3) 0.027(3) 0.002(2) C41 0.112(6) 0.059(4) 0.216(8) 0.049(4) 0.108(6) 0.033(4) C42 0.058(4) 0.055(3) 0.110(5) 0.018(3) 0.049(3) 0.012(3) C43 0.048(3) 0.065(3) 0.083(4) 0.015(3) 0.034(3) 0.010(3) C44 0.051(3) 0.052(3) 0.057(3) 0.006(2) 0.014(3) 0.000(2) C45 0.040(3) 0.050(3) 0.064(3) 0.011(2) 0.017(2) 0.015(2) C46 0.050(3) 0.063(3) 0.067(3) 0.016(3) 0.026(3) 0.017(2) C47 0.051(3) 0.069(3) 0.066(3) 0.017(3) 0.023(3) 0.005(3) C48 0.049(3) 0.046(2) 0.049(3) 0.011(2) 0.010(2) 0.009(2) C49 0.043(3) 0.040(2) 0.043(2) -0.0014(19) 0.012(2) 0.001(2) C50 0.043(3) 0.036(2) 0.045(3) -0.0111(19) 0.010(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O10 1.955(3) 7_556 ? Cu1 O5 1.960(3) 7_556 ? Cu1 O1 1.964(3) . ? Cu1 O6 1.969(3) . ? Cu1 O3 2.117(2) 6_556 ? Cu1 Cu2 2.6067(6) . ? Cu2 O2 1.928(3) . ? Cu2 O4 1.943(3) 7_556 ? Cu2 O7 1.956(3) . ? Cu2 O9 1.956(3) 7_556 ? Cu2 O11 2.156(3) . ? O1 C1 1.260(4) . ? O2 C1 1.265(4) . ? O3 C16 1.406(5) . ? O3 Cu1 2.117(2) 6 ? O3 H3A 0.8200 . ? O4 C25 1.268(4) . ? O4 Cu2 1.943(3) 7_556 ? O5 C25 1.256(4) . ? O5 Cu1 1.960(3) 7_556 ? O6 C26 1.258(4) . ? O7 C26 1.262(4) . ? O8 C41 1.374(6) . ? O8 H8A 0.8200 . ? O9 C50 1.261(5) . ? O9 Cu2 1.956(3) 7_556 ? O10 C50 1.281(5) . ? O10 Cu1 1.955(3) 7_556 ? O11 H11A 0.8499 . ? O11 H11B 0.8502 . ? C1 C3 1.489(6) . ? C2 C3 1.377(5) . ? C2 C7 1.408(5) . ? C2 H2 0.9500 . ? C3 C4 1.392(5) . ? C4 C5 1.374(6) . ? C4 H4 0.9500 . ? C5 C6 1.380(6) . ? C5 H5 0.9500 . ? C6 C7 1.389(6) . ? C6 H6 0.9500 . ? C7 C8 1.406(6) . ? C8 C9 1.181(6) . ? C9 C10 1.435(6) . ? C10 C11 1.366(5) . ? C10 C15 1.409(5) . ? C11 C12 1.380(6) . ? C11 H11 0.9500 . ? C12 C13 1.383(5) . ? C12 C16 1.506(5) . ? C13 C14 1.394(5) . ? C13 H13 0.9500 . ? C14 C15 1.384(6) . ? C14 C17 1.432(6) . ? C15 H15 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.189(5) . ? C18 C20 1.446(6) . ? C19 C20 1.373(5) . ? C19 C24 1.389(5) . ? C19 H19 0.9500 . ? C20 C21 1.403(6) . ? C21 C22 1.373(5) . ? C21 H21 0.9500 . ? C22 C23 1.381(5) . ? C22 H22 0.9500 . ? C23 C24 1.386(5) . ? C23 H23 0.9500 . ? C24 C25 1.493(5) . ? C26 C28 1.489(6) . ? C27 C32 1.358(6) . ? C27 C28 1.394(5) . ? C27 H27 0.9500 . ? C28 C29 1.385(6) . ? C29 C30 1.353(6) . ? C29 H29 0.9500 . ? C30 C31 1.390(7) . ? C30 H30 0.9500 . ? C31 C32 1.404(6) . ? C31 H31 0.9500 . ? C32 C33 1.456(6) . ? C33 C34 1.193(6) . ? C34 C35 1.459(6) . ? C35 C36 1.373(6) . ? C35 C40 1.397(6) . ? C36 C37 1.376(7) . ? C36 H36 0.9500 . ? C37 C38 1.381(7) . ? C37 C41 1.488(7) . ? C38 C39 1.376(6) . ? C38 H38 0.9500 . ? C39 C40 1.385(6) . ? C39 C42 1.434(7) . ? C40 H40 0.9500 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.192(6) . ? C43 C45 1.427(6) . ? C44 C49 1.373(6) . ? C44 C45 1.397(6) . ? C44 H44 0.9500 . ? C45 C46 1.397(6) . ? C46 C47 1.374(6) . ? C46 H46 0.9500 . ? C47 C48 1.384(6) . ? C47 H47 0.9500 . ? C48 C49 1.397(5) . ? C48 H48 0.9500 . ? C49 C50 1.491(6) . ? 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 O10 Cu1 O5 88.65(12) 7_556 7_556 ? O10 Cu1 O1 90.81(12) 7_556 . ? O5 Cu1 O1 169.02(11) 7_556 . ? O10 Cu1 O6 169.28(11) 7_556 . ? O5 Cu1 O6 88.86(12) 7_556 . ? O1 Cu1 O6 89.66(12) . . ? O10 Cu1 O3 95.14(11) 7_556 6_556 ? O5 Cu1 O3 99.77(11) 7_556 6_556 ? O1 Cu1 O3 91.20(11) . 6_556 ? O6 Cu1 O3 95.56(11) . 6_556 ? O10 Cu1 Cu2 84.09(8) 7_556 . ? O5 Cu1 Cu2 86.17(7) 7_556 . ? O1 Cu1 Cu2 82.87(8) . . ? O6 Cu1 Cu2 85.35(8) . . ? O3 Cu1 Cu2 174.00(8) 6_556 . ? O2 Cu2 O4 168.81(11) . 7_556 ? O2 Cu2 O7 89.15(12) . . ? O4 Cu2 O7 90.47(12) 7_556 . ? O2 Cu2 O9 89.63(12) . 7_556 ? O4 Cu2 O9 88.66(12) 7_556 7_556 ? O7 Cu2 O9 169.28(11) . 7_556 ? O2 Cu2 O11 95.50(11) . . ? O4 Cu2 O11 95.68(11) 7_556 . ? O7 Cu2 O11 94.21(12) . . ? O9 Cu2 O11 96.51(12) 7_556 . ? O2 Cu2 Cu1 86.00(8) . . ? O4 Cu2 Cu1 82.84(8) 7_556 . ? O7 Cu2 Cu1 83.94(7) . . ? O9 Cu2 Cu1 85.35(8) 7_556 . ? O11 Cu2 Cu1 177.61(9) . . ? C1 O1 Cu1 123.9(3) . . ? C1 O2 Cu2 122.1(3) . . ? C16 O3 Cu1 118.6(3) . 6 ? C16 O3 H3A 109.4 . . ? Cu1 O3 H3A 129.6 6 . ? C25 O4 Cu2 124.5(2) . 7_556 ? C25 O5 Cu1 120.0(3) . 7_556 ? C26 O6 Cu1 120.7(3) . . ? C26 O7 Cu2 123.2(3) . . ? C41 O8 H8A 109.9 . . ? C50 O9 Cu2 121.2(3) . 7_556 ? C50 O10 Cu1 122.7(3) . 7_556 ? Cu2 O11 H11A 123.0 . . ? Cu2 O11 H11B 122.8 . . ? H11A O11 H11B 97.8 . . ? O1 C1 O2 124.6(4) . . ? O1 C1 C3 118.9(3) . . ? O2 C1 C3 116.4(3) . . ? C3 C2 C7 121.2(4) . . ? C3 C2 H2 119.4 . . ? C7 C2 H2 119.4 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 C1 119.2(3) . . ? C4 C3 C1 121.6(4) . . ? C5 C4 C3 120.2(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 120.5(4) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C8 121.6(4) . . ? C6 C7 C2 118.2(4) . . ? C8 C7 C2 120.1(4) . . ? C9 C8 C7 172.6(5) . . ? C8 C9 C10 177.3(5) . . ? C11 C10 C15 119.3(4) . . ? C11 C10 C9 120.9(4) . . ? C15 C10 C9 119.8(4) . . ? C10 C11 C12 121.7(4) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C13 119.2(4) . . ? C11 C12 C16 119.6(4) . . ? C13 C12 C16 121.2(4) . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 119.8(4) . . ? C15 C14 C17 120.2(4) . . ? C13 C14 C17 119.9(4) . . ? C14 C15 C10 119.5(4) . . ? C14 C15 H15 120.2 . . ? C10 C15 H15 120.2 . . ? O3 C16 C12 112.2(4) . . ? O3 C16 H16A 109.2 . . ? C12 C16 H16A 109.2 . . ? O3 C16 H16B 109.2 . . ? C12 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C14 175.8(5) . . ? C17 C18 C20 179.0(4) . . ? C20 C19 C24 121.2(4) . . ? C20 C19 H19 119.4 . . ? C24 C19 H19 119.4 . . ? C19 C20 C21 118.9(4) . . ? C19 C20 C18 119.2(4) . . ? C21 C20 C18 121.8(4) . . ? C22 C21 C20 120.1(4) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.5(4) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 119.2(4) . . ? C23 C24 C25 121.9(3) . . ? C19 C24 C25 118.8(4) . . ? O5 C25 O4 125.6(4) . . ? O5 C25 C24 117.7(3) . . ? O4 C25 C24 116.7(3) . . ? O6 C26 O7 126.1(4) . . ? O6 C26 C28 117.2(4) . . ? O7 C26 C28 116.8(4) . . ? C32 C27 C28 121.0(4) . . ? C32 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 119.0(4) . . ? C29 C28 C26 121.6(4) . . ? C27 C28 C26 119.3(4) . . ? C30 C29 C28 121.3(4) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 119.3(5) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 120.5(5) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C27 C32 C31 118.8(4) . . ? C27 C32 C33 121.1(4) . . ? C31 C32 C33 120.1(5) . . ? C34 C33 C32 177.4(6) . . ? C33 C34 C35 176.8(6) . . ? C36 C35 C40 120.5(4) . . ? C36 C35 C34 120.7(5) . . ? C40 C35 C34 118.8(4) . . ? C37 C36 C35 121.4(5) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C38 118.0(5) . . ? C36 C37 C41 121.0(5) . . ? C38 C37 C41 121.0(5) . . ? C39 C38 C37 121.5(5) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C38 C39 C40 120.4(5) . . ? C38 C39 C42 119.4(4) . . ? C40 C39 C42 120.2(4) . . ? C39 C40 C35 118.1(4) . . ? C39 C40 H40 120.9 . . ? C35 C40 H40 120.9 . . ? O8 C41 C37 110.7(5) . . ? O8 C41 H41A 109.5 . . ? C37 C41 H41A 109.5 . . ? O8 C41 H41B 109.5 . . ? C37 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C43 C42 C39 178.6(5) . . ? C42 C43 C45 178.3(6) . . ? C49 C44 C45 120.8(4) . . ? C49 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 119.1(4) . . ? C46 C45 C43 119.9(4) . . ? C44 C45 C43 121.0(4) . . ? C47 C46 C45 119.8(4) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C48 121.1(4) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C47 C48 C49 119.4(4) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? C44 C49 C48 119.8(4) . . ? C44 C49 C50 119.5(4) . . ? C48 C49 C50 120.7(4) . . ? O9 C50 O10 125.4(4) . . ? O9 C50 C49 117.0(4) . . ? O10 C50 C49 117.6(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.54 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.384 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.080 # Attachment 'MOP-1b_luke07.cif' data_MOP1b _database_code_depnum_ccdc_archive 'CCDC 797902' #TrackingRef 'MOP-1b_luke07.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H72 Cu4 O24 S2' _chemical_formula_sum 'C104 H72 Cu4 O24 S2' _chemical_formula_weight 2023.90 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' S S 0.1246 0.1234 '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 tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 25.160(3) _cell_length_b 25.160(3) _cell_length_c 25.726(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16285(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3463 _cell_measurement_theta_min 2.2645 _cell_measurement_theta_max 20.227 _exptl_crystal_description neddle _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8441 _exptl_absorpt_correction_T_max 0.9602 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48691 _diffrn_reflns_av_R_equivalents 0.1608 _diffrn_reflns_av_sigmaI/netI 0.1696 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.99 _reflns_number_total 7171 _reflns_number_gt 2789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0818P)^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 7171 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1510 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 0.795 _refine_ls_restrained_S_all 0.795 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.050 -0.026 -0.011 8394 3073 ' ' _platon_squeeze_details ; ; 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 0.22185(3) 0.09097(3) 0.5000 0.0501(3) Uani 1 2 d S . . Cu2 Cu 0.32401(3) 0.06921(3) 0.5000 0.0489(3) Uani 1 2 d S . . S1 S 0.10633(9) 0.12963(10) 0.47124(12) 0.0596(9) Uani 0.50 1 d P . . O1 O 0.23683(12) 0.14458(11) 0.55316(14) 0.0481(9) Uani 1 1 d . . . O2 O 0.32299(12) 0.12359(12) 0.55304(15) 0.0591(11) Uani 1 1 d . . . O3 O 0.57023(12) 0.36070(13) 0.80871(16) 0.0705(12) Uani 1 1 d . . . H3A H 0.5758 0.3800 0.8348 0.085 Uiso 1 1 d R . . O4 O 0.69261(13) -0.01628(12) 0.55228(15) 0.0617(11) Uani 1 1 d . . . O5 O 0.77802(13) -0.03585(12) 0.55380(15) 0.0572(10) Uani 1 1 d . . . O6 O 0.40753(18) 0.0619(2) 0.5000 0.091(2) Uani 1 2 d S . . H6A H 0.4189 0.0472 0.4724 0.12(3) Uiso 1 1 d R . . O7 O 0.13867(18) 0.09662(19) 0.5000 0.087(2) Uani 1 2 d S . . C1 C 0.2836(2) 0.15040(19) 0.5692(2) 0.0503(15) Uani 1 1 d . . . C2 C 0.29327(18) 0.18965(18) 0.6093(2) 0.0474(14) Uani 1 1 d . . . C3 C 0.25371(19) 0.22219(19) 0.6296(2) 0.0573(16) Uani 1 1 d . . . H3 H 0.2181 0.2188 0.6178 0.069 Uiso 1 1 calc R . . C4 C 0.2668(2) 0.2607(2) 0.6681(3) 0.076(2) Uani 1 1 d . . . H4 H 0.2397 0.2836 0.6807 0.091 Uiso 1 1 calc R . . C5 C 0.31619(19) 0.2656(2) 0.6873(2) 0.0630(17) Uani 1 1 d . . . H5 H 0.3234 0.2906 0.7141 0.076 Uiso 1 1 calc R . . C6 C 0.35739(19) 0.2334(2) 0.6673(2) 0.0573(16) Uani 1 1 d . . . C7 C 0.34519(18) 0.19478(19) 0.6299(2) 0.0505(15) Uani 1 1 d . . . H7 H 0.3724 0.1715 0.6182 0.061 Uiso 1 1 calc R . . C8 C 0.4109(2) 0.2347(2) 0.6891(3) 0.0734(19) Uani 1 1 d . . . C9 C 0.4564(2) 0.2337(2) 0.7019(3) 0.0695(19) Uani 1 1 d . . . C10 C 0.50915(19) 0.2334(2) 0.7216(3) 0.0618(17) Uani 1 1 d . . . C11 C 0.5254(2) 0.2700(2) 0.7576(3) 0.0684(19) Uani 1 1 d . . . H11 H 0.5007 0.2956 0.7700 0.082 Uiso 1 1 calc R . . C12 C 0.57653(19) 0.2706(2) 0.7761(2) 0.0606(17) Uani 1 1 d . . . C13 C 0.61273(19) 0.2330(2) 0.7570(3) 0.0620(18) Uani 1 1 d . . . H13 H 0.6479 0.2326 0.7704 0.074 Uiso 1 1 calc R . . C14 C 0.59899(19) 0.1979(2) 0.7206(3) 0.073(2) Uani 1 1 d . . . C15 C 0.5466(2) 0.1968(2) 0.7019(2) 0.0674(18) Uani 1 1 d . . . H15 H 0.5365 0.1717 0.6762 0.081 Uiso 1 1 calc R . . C16 C 0.59244(19) 0.3098(2) 0.8176(2) 0.0658(17) Uani 1 1 d . . . H16A H 0.5805 0.2965 0.8519 0.079 Uiso 1 1 calc R . . H16B H 0.6317 0.3128 0.8184 0.079 Uiso 1 1 calc R . . C17 C 0.6379(2) 0.1621(2) 0.6983(3) 0.077(2) Uani 1 1 d . . . C18 C 0.6711(2) 0.1335(2) 0.6828(3) 0.0630(17) Uani 1 1 d . . . C19 C 0.71655(19) 0.10168(19) 0.6623(2) 0.0590(16) Uani 1 1 d . . . C20 C 0.7684(2) 0.11217(19) 0.6799(3) 0.0666(18) Uani 1 1 d . . . H20 H 0.7750 0.1400 0.7040 0.080 Uiso 1 1 calc R . . C21 C 0.8085(2) 0.0821(2) 0.6621(3) 0.0695(19) Uani 1 1 d . . . H21 H 0.8435 0.0888 0.6742 0.083 Uiso 1 1 calc R . . C22 C 0.80052(19) 0.04233(19) 0.6271(3) 0.0652(19) Uani 1 1 d . . . H22 H 0.8297 0.0218 0.6151 0.078 Uiso 1 1 calc R . . C23 C 0.74913(19) 0.03189(18) 0.6091(2) 0.0520(15) Uani 1 1 d . . . C24 C 0.70666(19) 0.06117(18) 0.6269(2) 0.0540(16) Uani 1 1 d . . . H24 H 0.6716 0.0539 0.6152 0.065 Uiso 1 1 calc R . . C25 C 0.7389(2) -0.01068(19) 0.5695(2) 0.0573(16) Uani 1 1 d . . . C26 C 0.1146(3) 0.1961(3) 0.5000 0.092(3) Uani 1 2 d S . . H26A H 0.1483 0.2112 0.4905 0.138 Uiso 0.50 1 d PR . . H26B H 0.0865 0.2187 0.4877 0.138 Uiso 0.50 1 d PR . . H26C H 0.1125 0.1931 0.5371 0.138 Uiso 0.50 1 d PR . . C27 C 0.0388(3) 0.1196(3) 0.5000 0.116(5) Uani 1 2 d S . . H27A H 0.0251 0.0855 0.4901 0.174 Uiso 0.50 1 d PR . . H27B H 0.0415 0.1214 0.5372 0.174 Uiso 0.50 1 d PR . . H27C H 0.0155 0.1470 0.4878 0.174 Uiso 0.50 1 d PR . . 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 0.0256(5) 0.0289(5) 0.0958(8) 0.000 0.000 -0.0005(4) Cu2 0.0240(5) 0.0331(5) 0.0896(8) 0.000 0.000 0.0003(4) S1 0.0357(14) 0.0465(15) 0.097(2) -0.0168(15) -0.0211(15) 0.0025(11) O1 0.0325(19) 0.0404(19) 0.072(3) -0.0062(18) 0.0005(19) -0.0069(15) O2 0.0300(19) 0.042(2) 0.105(3) -0.018(2) -0.002(2) -0.0037(15) O3 0.054(2) 0.053(2) 0.104(4) -0.018(2) -0.012(2) 0.0051(18) O4 0.036(2) 0.047(2) 0.103(3) -0.010(2) -0.013(2) 0.0034(16) O5 0.040(2) 0.041(2) 0.090(3) -0.008(2) -0.009(2) 0.0012(16) O6 0.031(3) 0.075(4) 0.168(7) 0.000 0.000 0.015(3) O7 0.027(3) 0.058(3) 0.177(7) 0.000 0.000 0.000(3) C1 0.046(3) 0.034(3) 0.071(4) 0.008(3) -0.002(3) -0.010(3) C2 0.036(3) 0.038(3) 0.068(4) -0.001(3) 0.005(3) -0.003(2) C3 0.036(3) 0.045(3) 0.090(5) -0.003(3) -0.006(3) 0.001(2) C4 0.067(4) 0.050(4) 0.111(6) -0.008(4) -0.032(4) 0.015(3) C5 0.030(3) 0.069(4) 0.090(5) -0.026(3) -0.007(3) -0.003(3) C6 0.033(3) 0.060(4) 0.078(5) -0.025(3) 0.000(3) -0.001(3) C7 0.032(3) 0.052(3) 0.068(4) 0.000(3) -0.006(3) 0.004(2) C8 0.049(4) 0.068(4) 0.103(6) -0.029(4) -0.001(4) -0.006(3) C9 0.034(3) 0.063(4) 0.112(6) -0.023(4) -0.004(4) -0.004(3) C10 0.041(3) 0.052(3) 0.093(5) -0.017(4) 0.000(3) 0.003(3) C11 0.036(3) 0.054(3) 0.115(6) -0.021(4) -0.007(3) 0.006(3) C12 0.040(3) 0.046(3) 0.096(5) -0.016(3) -0.006(3) -0.002(2) C13 0.032(3) 0.042(3) 0.112(6) 0.000(4) 0.013(3) -0.001(2) C14 0.027(3) 0.056(4) 0.136(7) -0.027(4) 0.005(4) -0.003(3) C15 0.056(4) 0.054(3) 0.092(5) -0.035(3) -0.022(4) 0.010(3) C16 0.041(3) 0.060(4) 0.096(5) -0.004(4) -0.009(3) 0.005(3) C17 0.044(3) 0.037(3) 0.150(7) -0.015(4) 0.008(4) -0.010(3) C18 0.060(4) 0.034(3) 0.095(5) -0.007(3) -0.004(4) 0.003(3) C19 0.042(3) 0.041(3) 0.094(5) -0.002(3) 0.011(3) -0.002(2) C20 0.055(4) 0.037(3) 0.108(6) -0.007(3) 0.005(4) -0.001(3) C21 0.040(3) 0.039(3) 0.130(6) -0.010(4) -0.016(4) -0.001(3) C22 0.042(3) 0.025(3) 0.129(6) -0.003(3) 0.000(4) 0.000(2) C23 0.035(3) 0.032(3) 0.089(5) 0.011(3) 0.001(3) 0.001(2) C24 0.044(3) 0.030(3) 0.089(5) -0.008(3) 0.007(3) 0.000(2) C25 0.036(3) 0.037(3) 0.099(5) 0.001(3) 0.003(4) -0.006(2) C26 0.042(5) 0.045(5) 0.189(11) 0.000 0.000 0.001(4) C27 0.026(4) 0.063(6) 0.259(15) 0.000 0.000 0.006(4) _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 O1 1.957(3) 11_556 ? Cu1 O1 1.957(3) . ? Cu1 O5 1.959(3) 3_655 ? Cu1 O5 1.959(3) 9_656 ? Cu1 O7 2.098(5) . ? Cu1 Cu2 2.6281(10) . ? Cu2 O2 1.932(4) 11_556 ? Cu2 O2 1.933(4) . ? Cu2 O4 1.938(3) 3_655 ? Cu2 O4 1.938(3) 9_656 ? Cu2 O6 2.109(5) . ? S1 O7 1.378(4) . ? S1 S1 1.480(6) 11_556 ? S1 C26 1.841(6) . ? S1 C27 1.869(7) . ? O1 C1 1.257(5) . ? O2 C1 1.268(6) . ? O3 C16 1.415(5) . ? O3 H3A 0.8402 . ? O4 C25 1.255(5) . ? O4 Cu2 1.938(3) 9_656 ? O5 C25 1.238(5) . ? O5 Cu1 1.959(3) 9_656 ? O6 H6A 0.8499 . ? O7 S1 1.378(4) 11_556 ? C1 C2 1.448(7) . ? C2 C3 1.391(6) . ? C2 C7 1.416(6) . ? C3 C4 1.424(7) . ? C3 H3 0.9500 . ? C4 C5 1.343(7) . ? C4 H4 0.9500 . ? C5 C6 1.414(6) . ? C5 H5 0.9500 . ? C6 C7 1.401(6) . ? C6 C8 1.460(7) . ? C7 H7 0.9500 . ? C8 C9 1.192(7) . ? C9 C10 1.420(7) . ? C10 C11 1.369(7) . ? C10 C15 1.411(7) . ? C11 C12 1.372(6) . ? C11 H11 0.9500 . ? C12 C13 1.400(7) . ? C12 C16 1.509(7) . ? C13 C14 1.333(7) . ? C13 H13 0.9500 . ? C14 C15 1.403(7) . ? C14 C17 1.448(8) . ? C15 H15 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.173(7) . ? C18 C19 1.493(7) . ? C19 C24 1.391(7) . ? C19 C20 1.407(7) . ? C20 C21 1.341(7) . ? C20 H20 0.9500 . ? C21 C22 1.360(7) . ? C21 H21 0.9500 . ? C22 C23 1.399(6) . ? C22 H22 0.9500 . ? C23 C24 1.376(6) . ? C23 C25 1.500(7) . ? C24 H24 0.9500 . ? C26 S1 1.841(6) 11_556 ? C26 H26A 0.9602 . ? C26 H26B 0.9598 . ? C26 H26C 0.9599 . ? C27 S1 1.869(7) 11_556 ? C27 H27A 0.9599 . ? C27 H27B 0.9601 . ? C27 H27C 0.9597 . ? 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 O1 Cu1 O1 88.64(19) 11_556 . ? O1 Cu1 O5 168.79(14) 11_556 3_655 ? O1 Cu1 O5 89.65(14) . 3_655 ? O1 Cu1 O5 89.65(14) 11_556 9_656 ? O1 Cu1 O5 168.78(14) . 9_656 ? O5 Cu1 O5 89.9(2) 3_655 9_656 ? O1 Cu1 O7 98.36(13) 11_556 . ? O1 Cu1 O7 98.37(13) . . ? O5 Cu1 O7 92.85(13) 3_655 . ? O5 Cu1 O7 92.85(13) 9_656 . ? O1 Cu1 Cu2 87.43(9) 11_556 . ? O1 Cu1 Cu2 87.43(9) . . ? O5 Cu1 Cu2 81.42(10) 3_655 . ? O5 Cu1 Cu2 81.42(10) 9_656 . ? O7 Cu1 Cu2 171.86(14) . . ? O2 Cu2 O2 89.8(2) 11_556 . ? O2 Cu2 O4 166.78(14) 11_556 3_655 ? O2 Cu2 O4 89.64(15) . 3_655 ? O2 Cu2 O4 89.64(15) 11_556 9_656 ? O2 Cu2 O4 166.78(14) . 9_656 ? O4 Cu2 O4 87.9(2) 3_655 9_656 ? O2 Cu2 O6 94.29(14) 11_556 . ? O2 Cu2 O6 94.28(14) . . ? O4 Cu2 O6 98.93(14) 3_655 . ? O4 Cu2 O6 98.92(14) 9_656 . ? O2 Cu2 Cu1 80.76(10) 11_556 . ? O2 Cu2 Cu1 80.77(10) . . ? O4 Cu2 Cu1 86.11(10) 3_655 . ? O4 Cu2 Cu1 86.11(10) 9_656 . ? O6 Cu2 Cu1 172.96(15) . . ? O7 S1 S1 57.53(16) . 11_556 ? O7 S1 C26 105.4(3) . . ? S1 S1 C26 66.31(13) 11_556 . ? O7 S1 C27 104.0(3) . . ? S1 S1 C27 66.68(12) 11_556 . ? C26 S1 C27 93.8(3) . . ? C1 O1 Cu1 119.4(3) . . ? C1 O2 Cu2 128.2(3) . . ? C16 O3 H3A 109.2 . . ? C25 O4 Cu2 121.5(3) . 9_656 ? C25 O5 Cu1 126.5(3) . 9_656 ? Cu2 O6 H6A 111.9 . . ? S1 O7 S1 64.9(3) 11_556 . ? S1 O7 Cu1 129.0(3) 11_556 . ? S1 O7 Cu1 129.0(3) . . ? O1 C1 O2 124.2(5) . . ? O1 C1 C2 118.0(5) . . ? O2 C1 C2 117.8(5) . . ? C3 C2 C7 117.8(5) . . ? C3 C2 C1 123.3(5) . . ? C7 C2 C1 118.9(5) . . ? C2 C3 C4 119.7(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 122.2(5) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 119.4(5) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 119.2(5) . . ? C7 C6 C8 118.8(5) . . ? C5 C6 C8 121.6(5) . . ? C6 C7 C2 121.5(5) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? C9 C8 C6 173.0(7) . . ? C8 C9 C10 175.1(7) . . ? C11 C10 C15 118.8(5) . . ? C11 C10 C9 121.1(5) . . ? C15 C10 C9 120.0(5) . . ? C10 C11 C12 121.4(5) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 118.8(5) . . ? C11 C12 C16 120.0(5) . . ? C13 C12 C16 121.1(5) . . ? C14 C13 C12 121.6(5) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 C17 121.0(5) . . ? C15 C14 C17 119.1(6) . . ? C14 C15 C10 119.5(5) . . ? C14 C15 H15 120.3 . . ? C10 C15 H15 120.3 . . ? O3 C16 C12 111.9(4) . . ? O3 C16 H16A 109.2 . . ? C12 C16 H16A 109.2 . . ? O3 C16 H16B 109.2 . . ? C12 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C14 176.2(8) . . ? C17 C18 C19 174.6(6) . . ? C24 C19 C20 121.0(5) . . ? C24 C19 C18 119.2(5) . . ? C20 C19 C18 119.8(5) . . ? C21 C20 C19 118.8(5) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 122.0(5) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C21 C22 C23 119.6(5) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 120.5(5) . . ? C24 C23 C25 118.3(5) . . ? C22 C23 C25 121.2(5) . . ? C23 C24 C19 118.1(5) . . ? C23 C24 H24 120.9 . . ? C19 C24 H24 120.9 . . ? O5 C25 O4 124.4(5) . . ? O5 C25 C23 116.8(5) . . ? O4 C25 C23 118.6(5) . . ? S1 C26 S1 47.4(3) 11_556 . ? S1 C26 H26A 124.0 11_556 . ? S1 C26 H26A 110.8 . . ? S1 C26 H26B 125.9 11_556 . ? S1 C26 H26B 108.8 . . ? H26A C26 H26B 109.5 . . ? S1 C26 H26C 61.5 11_556 . ? S1 C26 H26C 108.8 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S1 C27 S1 46.6(2) . 11_556 ? S1 C27 H27A 110.1 . . ? S1 C27 H27A 123.7 11_556 . ? S1 C27 H27B 109.0 . . ? S1 C27 H27B 62.4 11_556 . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.3 . . ? S1 C27 H27C 126.1 11_556 . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.510 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.064 # Attachment 'MOP-2_luke23_sq_fs.cif' data_MOP2 _database_code_depnum_ccdc_archive 'CCDC 797903' #TrackingRef 'MOP-2_luke23_sq_fs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H64 Cu4 O26, 2(C5 H11 N O)' _chemical_formula_sum 'C118 H86 Cu4 N2 O28' _chemical_formula_weight 2234.05 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.852(3) _cell_length_b 16.673(3) _cell_length_c 17.458(6) _cell_angle_alpha 110.385(4) _cell_angle_beta 103.907(4) _cell_angle_gamma 108.850(3) _cell_volume 3518.6(15) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2346 _cell_measurement_theta_min 2.2308 _cell_measurement_theta_max 19.6666 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8800 _exptl_absorpt_correction_T_max 0.9373 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27594 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.1716 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13625 _reflns_number_gt 5835 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0300P)^2^+2.5000P] 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 13625 _refine_ls_number_parameters 574 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1458 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _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 Cu1 Cu -0.33064(5) 0.47710(4) 1.34482(4) 0.0290(2) Uani 1 1 d . . . Cu2 Cu -0.40413(5) 0.30515(4) 1.21315(4) 0.0300(2) Uani 1 1 d . . . O1 O -0.4733(3) 0.4601(2) 1.3068(2) 0.0303(9) Uani 1 1 d . C . O2 O -0.5376(3) 0.3093(2) 1.2026(2) 0.0368(10) Uani 1 1 d . . . O3 O -0.8010(3) -0.4724(3) 0.6373(2) 0.0428(11) Uani 1 1 d . . . O4 O -0.7414(3) -0.3293(3) 0.7557(2) 0.0410(10) Uani 1 1 d . . . O5 O -1.3698(3) -0.0194(3) 0.8060(3) 0.0686(14) Uani 1 1 d . C . O6 O -1.3345(4) -0.0236(4) 0.6889(3) 0.0882(18) Uani 1 1 d . C . O7 O -0.3170(3) 0.5203(3) 1.2555(2) 0.0416(10) Uani 1 1 d . C . O8 O -0.3903(3) 0.3721(3) 1.1414(2) 0.0436(11) Uani 1 1 d . . . O9 O -0.6454(3) -0.4103(2) 0.5832(2) 0.0325(9) Uani 1 1 d . . . O10 O -0.5943(3) -0.2648(2) 0.6945(2) 0.0356(10) Uani 1 1 d . . . C1 C -0.5466(4) 0.3836(4) 1.2428(3) 0.0289(14) Uani 1 1 d . C . C2 C -0.6508(2) 0.3792(2) 1.2107(2) 0.0280(13) Uani 1 1 d G . . C3 C -0.7309(3) 0.29618(19) 1.1378(2) 0.0312(14) Uani 1 1 d G C . H3A H -0.7190 0.2426 1.1106 0.037 Uiso 1 1 calc R . . C4 C -0.8285(2) 0.2915(2) 1.1049(2) 0.0350(14) Uani 1 1 d G C . C5 C -0.8459(2) 0.3700(3) 1.1448(3) 0.059(2) Uani 1 1 d G C . H5A H -0.9125 0.3668 1.1222 0.071 Uiso 1 1 calc R . . C6 C -0.7657(3) 0.4530(2) 1.2176(3) 0.063(2) Uani 1 1 d G C . H6A H -0.7776 0.5066 1.2448 0.075 Uiso 1 1 calc R . . C7 C -0.6682(2) 0.45766(19) 1.2505(2) 0.0443(16) Uani 1 1 d G C . H7A H -0.6134 0.5144 1.3003 0.053 Uiso 1 1 calc R . . C8 C -0.9123(4) 0.2025(4) 1.0324(4) 0.0427(16) Uani 1 1 d . . . C9 C -0.9790(5) 0.1265(4) 0.9744(4) 0.0480(17) Uani 1 1 d . C . C10 C -1.0581(3) 0.03322(19) 0.9081(2) 0.0457(16) Uani 1 1 d G . . C11 C -1.1620(3) 0.0137(2) 0.8835(2) 0.0457(17) Uani 1 1 d G C . H11A H -1.1808 0.0624 0.9107 0.055 Uiso 1 1 calc R . . C12 C -1.2385(2) -0.0770(3) 0.8191(3) 0.0450(16) Uani 1 1 d G C . C13 C -1.2110(2) -0.14817(19) 0.7794(2) 0.0413(15) Uani 1 1 d G C . H13A H -1.2633 -0.2102 0.7354 0.050 Uiso 1 1 calc R . . C14 C -1.1071(3) -0.1287(2) 0.8040(2) 0.0407(15) Uani 1 1 d G C . C15 C -1.0306(2) -0.0380(3) 0.8684(3) 0.0426(16) Uani 1 1 d G C . H15A H -0.9596 -0.0246 0.8852 0.051 Uiso 1 1 calc R . . C16 C -1.0786(5) -0.2023(5) 0.7646(4) 0.0503(17) Uani 1 1 d . . . C17 C -1.0587(4) -0.2674(5) 0.7302(5) 0.0533(18) Uani 1 1 d . C . C18 C -1.0400(3) -0.3466(3) 0.6861(3) 0.0470(17) Uani 1 1 d G . . C19 C -0.9395(3) -0.3372(2) 0.7090(2) 0.0414(15) Uani 1 1 d G C . H19A H -0.8831 -0.2785 0.7548 0.050 Uiso 1 1 calc R . . C20 C -0.9214(2) -0.4138(3) 0.6648(3) 0.0414(15) Uani 1 1 d G C . C21 C -1.0039(3) -0.4998(2) 0.5977(2) 0.0493(17) Uani 1 1 d G C . H21A H -0.9915 -0.5521 0.5675 0.059 Uiso 1 1 calc R . . C22 C -1.1044(3) -0.5091(2) 0.5748(2) 0.060(2) Uani 1 1 d G C . H22A H -1.1608 -0.5678 0.5290 0.072 Uiso 1 1 calc R . . C23 C -1.1224(2) -0.4325(3) 0.6190(3) 0.0542(18) Uani 1 1 d G C . H23A H -1.1911 -0.4389 0.6034 0.065 Uiso 1 1 calc R . . C24 C -0.8128(4) -0.4044(5) 0.6875(4) 0.0368(15) Uani 1 1 d . . . C25 C -1.3514(4) -0.1016(4) 0.7931(4) 0.0593(19) Uani 1 1 d . . . H25A H -1.3901 -0.1501 0.7297 0.071 Uiso 1 1 calc R C . H25B H -1.3780 -0.1300 0.8291 0.071 Uiso 1 1 calc R . . C26 C -1.3584(6) 0.0131(6) 0.7473(6) 0.075(3) Uani 1 1 d . . . C27 C -1.3746(6) 0.1001(5) 0.7682(5) 0.106(3) Uani 1 1 d . C . H27A H -1.3648 0.1231 0.7248 0.159 Uiso 1 1 calc R . . H27B H -1.3244 0.1500 0.8282 0.159 Uiso 1 1 calc R . . H27C H -1.4451 0.0850 0.7654 0.159 Uiso 1 1 calc R . . C28 C -0.3517(4) 0.4626(4) 1.1741(4) 0.0369(15) Uani 1 1 d . C . C29 C -0.3509(3) 0.5019(3) 1.1093(2) 0.0389(15) Uani 1 1 d G . . C30 C -0.3056(3) 0.6002(2) 1.13918(17) 0.0478(17) Uani 1 1 d G C . H30A H -0.2729 0.6427 1.2013 0.057 Uiso 1 1 calc R . . C31 C -0.3079(3) 0.63616(18) 1.0783(2) 0.061(2) Uani 1 1 d G C . H31A H -0.2769 0.7033 1.0987 0.074 Uiso 1 1 calc R . . C32 C -0.3557(3) 0.5739(3) 0.9874(2) 0.0543(19) Uani 1 1 d G C . H32A H -0.3573 0.5985 0.9458 0.065 Uiso 1 1 calc R . . C33 C -0.4011(3) 0.4756(2) 0.95752(17) 0.0368(15) Uani 1 1 d G C . C34 C -0.3987(3) 0.43965(18) 1.0184(2) 0.0365(15) Uani 1 1 d G C . H34A H -0.4297 0.3725 0.9980 0.044 Uiso 1 1 calc R . . C35 C -0.4532(5) 0.4090(4) 0.8637(4) 0.0424(16) Uani 1 1 d . . . C36 C -0.4971(4) 0.3525(4) 0.7870(4) 0.0383(15) Uani 1 1 d . A . C43 C -0.6065(5) 0.0215(4) 0.5664(4) 0.0498(17) Uani 1 1 d . . . C44 C -0.6099(5) -0.0541(4) 0.5479(4) 0.0463(17) Uani 1 1 d . A . C45 C -0.6189(3) -0.15015(18) 0.5193(2) 0.0403(15) Uani 1 1 d G . . C46 C -0.6117(3) -0.1879(2) 0.57881(17) 0.0371(15) Uani 1 1 d G A . H46A H -0.5994 -0.1503 0.6389 0.045 Uiso 1 1 calc R . . C47 C -0.6225(3) -0.2807(2) 0.5504(2) 0.0292(13) Uani 1 1 d G A . C48 C -0.6405(3) -0.33572(18) 0.4625(2) 0.0366(15) Uani 1 1 d G A . H48A H -0.6478 -0.3991 0.4431 0.044 Uiso 1 1 calc R . . C49 C -0.6477(3) -0.2980(2) 0.40300(17) 0.0496(18) Uani 1 1 d G A . H49A H -0.6599 -0.3356 0.3429 0.060 Uiso 1 1 calc R . . C50 C -0.6369(3) -0.2052(2) 0.4314(2) 0.0512(18) Uani 1 1 d G A . H50A H -0.6418 -0.1794 0.3908 0.061 Uiso 1 1 calc R . . C51 C -0.6196(4) -0.3213(4) 0.6146(4) 0.0299(14) Uani 1 1 d . . . C37 C -0.5468(8) 0.2774(8) 0.6929(5) 0.0391(8) Uani 0.50 1 d PGD A 1 C38 C -0.5665(7) 0.3046(6) 0.6263(7) 0.0391(8) Uani 0.50 1 d PGD A 1 H38A H -0.5557 0.3684 0.6413 0.047 Uiso 0.50 1 calc PR A 1 C39 C -0.6019(5) 0.2384(7) 0.5377(6) 0.0391(8) Uani 0.50 1 d PGD A 1 C40 C -0.6177(7) 0.1450(6) 0.5157(5) 0.0391(8) Uani 0.50 1 d PGD A 1 H40A H -0.6419 0.0997 0.4551 0.047 Uiso 0.50 1 calc PR A 1 C41 C -0.5980(9) 0.1178(7) 0.5823(7) 0.0391(8) Uani 0.50 1 d PGD A 1 C42 C -0.5626(9) 0.1840(9) 0.6709(6) 0.0391(8) Uani 0.50 1 d PGD A 1 H42A H -0.5491 0.1654 0.7164 0.047 Uiso 0.50 1 calc PR A 1 O11 O -0.5524(4) 0.3626(3) 0.4974(4) 0.0422(9) Uani 0.50 1 d PD . 1 O12 O -0.6531(4) 0.3755(4) 0.3941(4) 0.0422(9) Uani 0.50 1 d PD B 1 C52 C -0.6246(6) 0.2639(4) 0.4626(5) 0.0422(9) Uani 0.50 1 d PD A 1 H52A H -0.6153 0.2225 0.4117 0.051 Uiso 0.50 1 calc PR A 1 H52B H -0.6968 0.2554 0.4422 0.051 Uiso 0.50 1 calc PR A 1 C53 C -0.5723(4) 0.4151(3) 0.4581(3) 0.0422(9) Uani 0.50 1 d PD . 1 C54 C -0.4938(7) 0.5168(4) 0.4965(7) 0.0422(9) Uani 0.50 1 d PD . 1 H54A H -0.5178 0.5456 0.4623 0.063 Uiso 0.50 1 d PR . 1 H54B H -0.4845 0.5512 0.5571 0.063 Uiso 0.50 1 d PR . 1 H54C H -0.4290 0.5188 0.4949 0.063 Uiso 0.50 1 d PR . 1 C37' C -0.5446(8) 0.2808(8) 0.6976(5) 0.0391(8) Uani 0.50 1 d PGD A 2 C38' C -0.5904(7) 0.2956(6) 0.6277(7) 0.0391(8) Uani 0.50 1 d PGD A 2 H38B H -0.5882 0.3564 0.6391 0.047 Uiso 0.50 1 calc PR A 2 C39' C -0.6394(4) 0.2215(7) 0.5411(6) 0.0391(8) Uani 0.50 1 d PGD A 2 C40' C -0.6426(7) 0.1325(6) 0.5244(5) 0.0391(8) Uani 0.50 1 d PGD A 2 H40B H -0.6761 0.0819 0.4652 0.047 Uiso 0.50 1 calc PR A 2 C41' C -0.5969(9) 0.1178(7) 0.5943(7) 0.0391(8) Uani 0.50 1 d PGD A 2 C42' C -0.5479(8) 0.1919(9) 0.6809(6) 0.0391(8) Uani 0.50 1 d PGD A 2 H42B H -0.5166 0.1818 0.7287 0.047 Uiso 0.50 1 calc PR A 2 O11' O -0.7898(4) 0.2290(4) 0.4608(4) 0.0422(9) Uani 0.50 1 d PD A 2 O12' O -0.7258(7) 0.3820(4) 0.5449(8) 0.0422(9) Uani 0.50 1 d PD . 2 C52' C -0.6898(5) 0.2353(7) 0.4637(6) 0.0422(9) Uani 0.50 1 d PD A 2 H52C H -0.6456 0.2986 0.4710 0.051 Uiso 0.50 1 calc PR A 2 H52D H -0.6981 0.1854 0.4073 0.051 Uiso 0.50 1 calc PR A 2 C53' C -0.8014(5) 0.3057(4) 0.5078(4) 0.0422(9) Uani 0.50 1 d PD A 2 C54' C -0.9055(6) 0.2901(7) 0.5100(8) 0.0422(9) Uani 0.50 1 d PD A 2 H54D H -0.9027 0.3516 0.5464 0.063 Uiso 0.50 1 calc PR A 2 H54E H -0.9250 0.2470 0.5359 0.063 Uiso 0.50 1 calc PR A 2 H54F H -0.9571 0.2616 0.4493 0.063 Uiso 0.50 1 calc PR A 2 O1S O -0.2583(11) 0.6224(9) 1.4491(12) 0.095(2) Uani 0.50 1 d P C 1 N1S N -0.0924(8) 0.7380(8) 1.4957(7) 0.095(2) Uani 0.50 1 d PD C 1 C1S C -0.1671(13) 0.6758(11) 1.5028(11) 0.095(2) Uani 0.50 1 d P C 1 H1SA H -0.1485 0.6711 1.5565 0.114 Uiso 0.50 1 calc PR C 1 C2S C -0.1101(11) 0.7181(9) 1.3973(9) 0.095(2) Uani 0.50 1 d PD C 1 H2SA H -0.0445 0.7286 1.3888 0.114 Uiso 0.50 1 calc PR C 1 H2SB H -0.1621 0.6512 1.3552 0.114 Uiso 0.50 1 calc PR C 1 C3S C -0.1484(11) 0.7868(9) 1.3815(8) 0.095(2) Uani 0.50 1 d PD C 1 H3SA H -0.1620 0.7759 1.3201 0.143 Uiso 0.50 1 calc PR C 1 H3SB H -0.0956 0.8527 1.4228 0.143 Uiso 0.50 1 calc PR C 1 H3SC H -0.2125 0.7766 1.3915 0.143 Uiso 0.50 1 calc PR C 1 C4S C 0.0057(10) 0.8006(9) 1.5605(8) 0.095(2) Uani 0.50 1 d PD C 1 H4SA H 0.0008 0.8094 1.6167 0.114 Uiso 0.30 1 d PR C 1 H4SB H 0.0237 0.8611 1.5603 0.114 Uiso 0.30 1 d PR C 1 H4SC H 0.0258 0.8586 1.5526 0.114 Uiso 0.20 1 d PR C 1 H4SD H 0.0506 0.7738 1.5459 0.114 Uiso 0.20 1 d PR C 1 C5S C 0.0916(10) 0.7721(15) 1.5560(15) 0.095(2) Uani 0.30 1 d PD C 1 H5SA H 0.1044 0.7709 1.5032 0.143 Uiso 0.30 1 calc PR C 1 H5SB H 0.0714 0.7083 1.5523 0.143 Uiso 0.30 1 calc PR C 1 H5SC H 0.1550 0.8184 1.6095 0.143 Uiso 0.30 1 calc PR C 1 C5S' C 0.021(2) 0.827(2) 1.6562(7) 0.095(2) Uani 0.20 1 d PD C 1 H5SD H -0.0363 0.8395 1.6667 0.143 Uiso 0.20 1 calc PR C 1 H5SE H 0.0867 0.8843 1.6958 0.143 Uiso 0.20 1 calc PR C 1 H5SF H 0.0218 0.7739 1.6681 0.143 Uiso 0.20 1 calc PR C 1 O3S O -0.0029(6) 0.5222(7) 1.1990(6) 0.0717(16) Uani 0.50 1 d PD D 2 N3S N -0.1383(7) 0.3993(6) 1.0698(5) 0.0717(16) Uani 0.50 1 d PD D 2 C11S C -0.0973(7) 0.4827(7) 1.1483(6) 0.0717(16) Uani 0.50 1 d PD D 2 H11B H -0.1409 0.5106 1.1642 0.086 Uiso 0.50 1 calc PR D 2 C13S C -0.2338(9) 0.2229(6) 0.9883(7) 0.0717(16) Uani 0.50 1 d PD D 2 H13B H -0.2792 0.1671 0.9909 0.108 Uiso 0.50 1 calc PR D 2 H13C H -0.1680 0.2206 0.9912 0.108 Uiso 0.50 1 calc PR D 2 H13D H -0.2675 0.2225 0.9324 0.108 Uiso 0.50 1 calc PR D 2 C12S C -0.2132(9) 0.3131(7) 1.0659(7) 0.0717(16) Uani 0.50 1 d PD D 2 H12A H -0.2792 0.3173 1.0606 0.086 Uiso 0.50 1 calc PR D 2 H12B H -0.1860 0.3102 1.1220 0.086 Uiso 0.50 1 calc PR D 2 C15S C -0.1916(9) 0.4029(10) 0.9262(6) 0.0717(16) Uani 0.50 1 d PD D 2 H15B H -0.1717 0.4005 0.8761 0.108 Uiso 0.50 1 calc PR D 2 H15C H -0.1907 0.4650 0.9571 0.108 Uiso 0.50 1 calc PR D 2 H15D H -0.2615 0.3517 0.9039 0.108 Uiso 0.50 1 calc PR D 2 C14S C -0.1158(8) 0.3900(11) 0.9902(7) 0.0717(16) Uani 0.50 1 d PD D 2 H14A H -0.1192 0.3261 0.9596 0.086 Uiso 0.50 1 calc PR D 2 H14B H -0.0445 0.4387 1.0087 0.086 Uiso 0.50 1 calc PR D 2 O2S O -0.4708(3) 0.1620(2) 1.1093(3) 0.0693(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0320(4) 0.0243(4) 0.0192(4) 0.0036(3) 0.0057(3) 0.0099(3) Cu2 0.0349(4) 0.0248(4) 0.0203(4) 0.0038(3) 0.0066(3) 0.0126(3) O1 0.033(2) 0.0241(19) 0.020(2) 0.0037(16) 0.0031(17) 0.0105(17) O2 0.033(2) 0.030(2) 0.031(2) 0.0007(18) 0.0030(18) 0.0162(18) O3 0.039(3) 0.045(2) 0.033(2) 0.005(2) 0.014(2) 0.020(2) O4 0.034(2) 0.042(2) 0.032(2) 0.009(2) 0.007(2) 0.014(2) O5 0.045(3) 0.047(3) 0.078(4) 0.005(3) 0.003(3) 0.021(2) O6 0.104(4) 0.094(4) 0.046(3) 0.014(3) 0.004(3) 0.060(4) O7 0.054(3) 0.037(2) 0.027(2) 0.0125(19) 0.019(2) 0.012(2) O8 0.060(3) 0.036(2) 0.028(2) 0.016(2) 0.010(2) 0.018(2) O9 0.051(3) 0.024(2) 0.022(2) 0.0075(17) 0.0138(18) 0.0198(18) O10 0.043(2) 0.025(2) 0.020(2) 0.0039(17) 0.0035(18) 0.0089(18) C1 0.042(4) 0.022(3) 0.018(3) 0.011(2) 0.006(3) 0.012(3) C2 0.034(3) 0.025(3) 0.025(3) 0.010(2) 0.010(3) 0.014(3) C3 0.033(3) 0.026(3) 0.026(3) 0.010(3) 0.006(3) 0.011(3) C4 0.035(4) 0.031(3) 0.029(3) 0.013(3) 0.004(3) 0.012(3) C5 0.046(4) 0.054(4) 0.063(5) 0.024(4) -0.001(4) 0.027(4) C6 0.044(4) 0.037(4) 0.084(5) 0.009(4) 0.009(4) 0.024(3) C7 0.034(4) 0.032(3) 0.048(4) 0.009(3) 0.004(3) 0.013(3) C8 0.031(4) 0.048(4) 0.049(4) 0.026(3) 0.010(3) 0.018(3) C9 0.042(4) 0.036(4) 0.048(4) 0.020(3) 0.000(3) 0.009(3) C10 0.041(4) 0.039(4) 0.039(4) 0.019(3) -0.001(3) 0.009(3) C11 0.039(4) 0.035(3) 0.047(4) 0.015(3) 0.002(3) 0.014(3) C12 0.037(4) 0.035(3) 0.053(4) 0.020(3) 0.010(3) 0.011(3) C13 0.032(4) 0.036(3) 0.050(4) 0.023(3) 0.007(3) 0.011(3) C14 0.038(4) 0.035(3) 0.056(4) 0.026(3) 0.018(3) 0.020(3) C15 0.026(3) 0.039(4) 0.048(4) 0.022(3) -0.001(3) 0.007(3) C16 0.037(4) 0.048(4) 0.057(5) 0.025(4) 0.007(3) 0.017(3) C17 0.030(4) 0.056(4) 0.071(5) 0.033(4) 0.013(3) 0.017(3) C18 0.043(4) 0.054(4) 0.059(4) 0.032(4) 0.020(4) 0.032(4) C19 0.042(4) 0.042(4) 0.040(4) 0.018(3) 0.015(3) 0.020(3) C20 0.035(4) 0.051(4) 0.037(4) 0.021(3) 0.013(3) 0.019(3) C21 0.044(4) 0.053(4) 0.048(4) 0.019(3) 0.019(3) 0.024(3) C22 0.032(4) 0.062(5) 0.053(4) 0.014(4) 0.002(3) 0.010(3) C23 0.036(4) 0.050(4) 0.074(5) 0.027(4) 0.018(4) 0.021(3) C24 0.032(4) 0.058(4) 0.035(4) 0.029(3) 0.020(3) 0.024(3) C25 0.036(4) 0.035(3) 0.077(5) 0.009(4) 0.007(4) 0.012(3) C26 0.061(6) 0.066(6) 0.052(6) 0.007(5) -0.021(4) 0.030(4) C27 0.148(8) 0.091(6) 0.059(5) 0.025(5) -0.006(5) 0.076(6) C28 0.034(4) 0.054(4) 0.029(4) 0.025(3) 0.012(3) 0.022(3) C29 0.041(4) 0.035(3) 0.038(4) 0.018(3) 0.015(3) 0.013(3) C30 0.054(4) 0.047(4) 0.027(3) 0.022(3) 0.009(3) 0.007(3) C31 0.079(5) 0.043(4) 0.041(4) 0.018(3) 0.019(4) 0.007(4) C32 0.075(5) 0.050(4) 0.031(4) 0.024(3) 0.019(3) 0.016(4) C33 0.046(4) 0.036(3) 0.029(3) 0.018(3) 0.017(3) 0.015(3) C34 0.046(4) 0.032(3) 0.028(3) 0.013(3) 0.015(3) 0.016(3) C35 0.051(4) 0.050(4) 0.034(4) 0.026(3) 0.016(3) 0.024(3) C36 0.047(4) 0.036(3) 0.038(4) 0.023(3) 0.014(3) 0.021(3) C43 0.072(5) 0.038(4) 0.033(4) 0.016(3) 0.017(3) 0.021(3) C44 0.060(4) 0.033(3) 0.045(4) 0.019(3) 0.019(3) 0.021(3) C45 0.048(4) 0.037(3) 0.031(4) 0.018(3) 0.008(3) 0.017(3) C46 0.040(4) 0.028(3) 0.028(3) 0.005(3) 0.008(3) 0.010(3) C47 0.039(3) 0.026(3) 0.018(3) 0.006(2) 0.008(3) 0.016(3) C48 0.049(4) 0.029(3) 0.033(3) 0.017(3) 0.018(3) 0.015(3) C49 0.075(5) 0.023(3) 0.035(4) 0.007(3) 0.015(3) 0.016(3) C50 0.077(5) 0.037(4) 0.033(4) 0.018(3) 0.013(3) 0.023(3) C51 0.030(3) 0.022(3) 0.028(3) 0.008(3) 0.005(3) 0.010(3) C37 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C38 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C39 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C40 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C41 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C42 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) O11 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) O12 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) C52 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) C53 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) C54 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) C37' 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C38' 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C39' 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C40' 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C41' 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) C42' 0.0512(19) 0.0329(15) 0.0293(17) 0.0118(13) 0.0083(15) 0.0230(15) O11' 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) O12' 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) C52' 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) C53' 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) C54' 0.056(2) 0.0322(17) 0.0298(18) 0.0125(15) 0.0041(16) 0.0211(17) O1S 0.101(5) 0.061(4) 0.063(4) 0.016(3) -0.007(4) 0.011(3) N1S 0.101(5) 0.061(4) 0.063(4) 0.016(3) -0.007(4) 0.011(3) C1S 0.101(5) 0.061(4) 0.063(4) 0.016(3) -0.007(4) 0.011(3) C2S 0.101(5) 0.061(4) 0.063(4) 0.016(3) -0.007(4) 0.011(3) C3S 0.101(5) 0.061(4) 0.063(4) 0.016(3) -0.007(4) 0.011(3) C4S 0.101(5) 0.061(4) 0.063(4) 0.016(3) -0.007(4) 0.011(3) C5S 0.101(5) 0.061(4) 0.063(4) 0.016(3) -0.007(4) 0.011(3) C5S' 0.101(5) 0.061(4) 0.063(4) 0.016(3) -0.007(4) 0.011(3) O3S 0.060(3) 0.133(5) 0.066(4) 0.073(4) 0.040(3) 0.053(3) N3S 0.060(3) 0.133(5) 0.066(4) 0.073(4) 0.040(3) 0.053(3) C11S 0.060(3) 0.133(5) 0.066(4) 0.073(4) 0.040(3) 0.053(3) C13S 0.060(3) 0.133(5) 0.066(4) 0.073(4) 0.040(3) 0.053(3) C12S 0.060(3) 0.133(5) 0.066(4) 0.073(4) 0.040(3) 0.053(3) C15S 0.060(3) 0.133(5) 0.066(4) 0.073(4) 0.040(3) 0.053(3) C14S 0.060(3) 0.133(5) 0.066(4) 0.073(4) 0.040(3) 0.053(3) O2S 0.093(4) 0.022(2) 0.065(3) -0.003(2) 0.036(3) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.936(4) 2_457 ? Cu1 O1 1.952(3) . ? Cu1 O7 1.957(4) . ? Cu1 O9 1.971(3) 2_457 ? Cu1 O1S 2.155(12) . ? Cu1 O12' 2.174(7) 2_467 ? Cu1 Cu2 2.6221(10) . ? Cu2 O8 1.952(4) . ? Cu2 O10 1.954(4) 2_457 ? Cu2 O4 1.963(4) 2_457 ? Cu2 O2 1.972(4) . ? Cu2 O2S 2.135(4) . ? O1 C1 1.259(5) . ? O2 C1 1.262(6) . ? O3 C24 1.263(6) . ? O3 Cu1 1.936(4) 2_457 ? O4 C24 1.267(6) . ? O4 Cu2 1.963(4) 2_457 ? O5 C26 1.335(9) . ? O5 C25 1.435(7) . ? O6 C26 1.192(9) . ? O7 C28 1.259(6) . ? O8 C28 1.270(6) . ? O9 C51 1.270(5) . ? O9 Cu1 1.970(3) 2_457 ? O10 C51 1.257(5) . ? O10 Cu2 1.954(4) 2_457 ? C1 C2 1.481(6) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 C8 1.447(6) . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 C7 1.3900 . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.193(7) . ? C9 C10 1.432(6) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9500 . ? C12 C13 1.3900 . ? C12 C25 1.499(6) . ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 C15 1.3900 . ? C14 C16 1.431(7) . ? C15 H15A 0.9500 . ? C16 C17 1.209(8) . ? C17 C18 1.431(8) . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9500 . ? C20 C21 1.3900 . ? C20 C24 1.507(6) . ? C21 C22 1.3900 . ? C21 H21A 0.9500 . ? C22 C23 1.3900 . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.481(10) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.494(6) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C30 H30A 0.9500 . ? C31 C32 1.3900 . ? C31 H31A 0.9500 . ? C32 C33 1.3900 . ? C32 H32A 0.9500 . ? C33 C34 1.3900 . ? C33 C35 1.444(6) . ? C34 H34A 0.9500 . ? C35 C36 1.187(7) . ? C36 C37' 1.410(10) . ? C36 C37 1.483(10) . ? C43 C44 1.167(7) . ? C43 C41' 1.452(11) . ? C43 C41 1.488(10) . ? C44 C45 1.451(6) . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C46 H46A 0.9500 . ? C47 C48 1.3900 . ? C47 C51 1.496(6) . ? C48 C49 1.3900 . ? C48 H48A 0.9500 . ? C49 C50 1.3900 . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C38 C39 1.3900 . ? C38 H38A 0.9500 . ? C39 C40 1.3900 . ? C39 C52 1.5100(11) . ? C40 C41 1.3900 . ? C40 H40A 0.9500 . ? C41 C42 1.3900 . ? C42 H42A 0.9500 . ? O11 C53 1.3472(9) . ? O11 C52 1.4408(11) . ? O11 C54 1.859(9) 2_466 ? O12 C53 1.2058(9) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.078(9) 2_466 ? C53 C54 1.4960(9) . ? C54 C54 0.594(11) 2_466 ? C54 C53 1.077(9) 2_466 ? C54 O11 1.859(9) 2_466 ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C37' C38' 1.3900 . ? C37' C42' 1.3900 . ? C38' C39' 1.3900 . ? C38' H38B 0.9500 . ? C39' C40' 1.3900 . ? C39' C52' 1.5101(11) . ? C40' C41' 1.3900 . ? C40' H40B 0.9500 . ? C41' C42' 1.3900 . ? C42' H42B 0.9500 . ? O11' C53' 1.3474(9) . ? O11' C52' 1.4415(11) . ? O12' C53' 1.2058(9) . ? O12' Cu1 2.174(7) 2_467 ? C52' H52C 0.9900 . ? C52' H52D 0.9900 . ? C53' C54' 1.4959(9) . ? C54' H54D 0.9800 . ? C54' H54E 0.9800 . ? C54' H54F 0.9800 . ? O1S C1S 1.239(19) . ? N1S C1S 1.316(19) . ? N1S C4S 1.376(13) . ? N1S C2S 1.569(17) . ? C1S H1SA 0.9500 . ? C2S C3S 1.5100(11) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C4S C5S 1.5100(11) . ? C4S C5S' 1.5101(12) . ? C4S H4SA 0.9648 . ? C4S H4SB 0.9564 . ? C4S H4SC 0.9825 . ? C4S H4SD 0.9521 . ? C5S H4SD 0.6054 . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? C5S' H4SA 0.5947 . ? C5S' H5SD 0.9800 . ? C5S' H5SE 0.9800 . ? C5S' H5SF 0.9800 . ? O3S C11S 1.2594(11) . ? N3S C11S 1.3807(11) . ? N3S C12S 1.4735(11) . ? N3S C14S 1.4751(11) . ? C11S H11B 0.9500 . ? C13S C12S 1.5082(11) . ? C13S H13B 0.9800 . ? C13S H13C 0.9800 . ? C13S H13D 0.9800 . ? C12S H12A 0.9900 . ? C12S H12B 0.9900 . ? C15S C14S 1.5098(11) . ? C15S H15B 0.9800 . ? C15S H15C 0.9800 . ? C15S H15D 0.9800 . ? C14S H14A 0.9900 . ? C14S H14B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 O1 169.49(15) 2_457 . ? O3 Cu1 O7 90.03(16) 2_457 . ? O1 Cu1 O7 87.54(15) . . ? O3 Cu1 O9 88.91(15) 2_457 2_457 ? O1 Cu1 O9 91.65(14) . 2_457 ? O7 Cu1 O9 169.65(14) . 2_457 ? O3 Cu1 O1S 92.4(5) 2_457 . ? O1 Cu1 O1S 97.9(5) . . ? O7 Cu1 O1S 91.5(6) . . ? O9 Cu1 O1S 98.8(5) 2_457 . ? O3 Cu1 O12' 97.9(3) 2_457 2_467 ? O1 Cu1 O12' 92.6(3) . 2_467 ? O7 Cu1 O12' 96.4(4) . 2_467 ? O9 Cu1 O12' 93.9(4) 2_457 2_467 ? O1S Cu1 O12' 7.4(6) . 2_467 ? O3 Cu1 Cu2 83.58(11) 2_457 . ? O1 Cu1 Cu2 86.02(10) . . ? O7 Cu1 Cu2 84.83(11) . . ? O9 Cu1 Cu2 84.82(10) 2_457 . ? O1S Cu1 Cu2 174.6(4) . . ? O12' Cu1 Cu2 178.1(3) 2_467 . ? O8 Cu2 O10 168.10(15) . 2_457 ? O8 Cu2 O4 90.09(16) . 2_457 ? O10 Cu2 O4 88.57(15) 2_457 2_457 ? O8 Cu2 O2 88.12(16) . . ? O10 Cu2 O2 90.65(15) 2_457 . ? O4 Cu2 O2 167.62(15) 2_457 . ? O8 Cu2 O2S 98.65(17) . . ? O10 Cu2 O2S 93.26(16) 2_457 . ? O4 Cu2 O2S 97.05(17) 2_457 . ? O2 Cu2 O2S 95.33(16) . . ? O8 Cu2 Cu1 84.02(11) . . ? O10 Cu2 Cu1 84.08(10) 2_457 . ? O4 Cu2 Cu1 85.36(11) 2_457 . ? O2 Cu2 Cu1 82.27(10) . . ? O2S Cu2 Cu1 176.38(12) . . ? C1 O1 Cu1 121.7(3) . . ? C1 O2 Cu2 124.5(3) . . ? C24 O3 Cu1 124.2(4) . 2_457 ? C24 O4 Cu2 120.7(4) . 2_457 ? C26 O5 C25 115.0(6) . . ? C28 O7 Cu1 122.1(4) . . ? C28 O8 Cu2 123.2(4) . . ? C51 O9 Cu1 121.2(3) . 2_457 ? C51 O10 Cu2 123.5(3) . 2_457 ? O1 C1 O2 124.2(5) . . ? O1 C1 C2 119.0(4) . . ? O2 C1 C2 116.8(4) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 119.0(3) . . ? C7 C2 C1 120.9(3) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 C8 120.8(3) . . ? C3 C4 C8 119.1(3) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C9 C8 C4 176.4(6) . . ? C8 C9 C10 176.9(6) . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 120.2(4) . . ? C15 C10 C9 119.8(4) . . ? C12 C11 C10 120.0 . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 C25 121.5(3) . . ? C13 C12 C25 118.5(3) . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 C16 119.8(3) . . ? C13 C14 C16 120.2(3) . . ? C14 C15 C10 120.0 . . ? C14 C15 H15A 120.0 . . ? C10 C15 H15A 120.0 . . ? C17 C16 C14 177.2(6) . . ? C16 C17 C18 177.3(7) . . ? C19 C18 C23 120.0 . . ? C19 C18 C17 120.2(4) . . ? C23 C18 C17 119.8(4) . . ? C20 C19 C18 120.0 . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 C24 120.7(4) . . ? C21 C20 C24 119.3(4) . . ? C22 C21 C20 120.0 . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 H23A 120.0 . . ? C18 C23 H23A 120.0 . . ? O3 C24 O4 125.8(5) . . ? O3 C24 C20 117.1(5) . . ? O4 C24 C20 117.2(5) . . ? O5 C25 C12 112.1(4) . . ? O5 C25 H25A 109.2 . . ? C12 C25 H25A 109.2 . . ? O5 C25 H25B 109.2 . . ? C12 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? O6 C26 O5 122.1(8) . . ? O6 C26 C27 126.7(10) . . ? O5 C26 C27 111.1(8) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O7 C28 O8 125.4(5) . . ? O7 C28 C29 118.3(5) . . ? O8 C28 C29 116.3(5) . . ? C30 C29 C34 120.0 . . ? C30 C29 C28 120.4(3) . . ? C34 C29 C28 119.6(3) . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 C35 118.5(3) . . ? C32 C33 C35 121.4(3) . . ? C33 C34 C29 120.0 . . ? C33 C34 H34A 120.0 . . ? C29 C34 H34A 120.0 . . ? C36 C35 C33 178.4(6) . . ? C35 C36 C37' 174.9(8) . . ? C35 C36 C37 175.0(8) . . ? C44 C43 C41' 176.6(8) . . ? C44 C43 C41 173.8(8) . . ? C43 C44 C45 176.4(7) . . ? C46 C45 C50 120.0 . . ? C46 C45 C44 120.4(3) . . ? C50 C45 C44 119.6(3) . . ? C45 C46 C47 120.0 . . ? C45 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 C51 121.0(3) . . ? C46 C47 C51 118.9(3) . . ? C47 C48 C49 120.0 . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 H50A 120.0 . . ? C45 C50 H50A 120.0 . . ? O10 C51 O9 125.7(5) . . ? O10 C51 C47 117.1(4) . . ? O9 C51 C47 117.2(4) . . ? C38 C37 C42 120.0 . . ? C38 C37 C36 118.4(8) . . ? C42 C37 C36 121.2(8) . . ? C39 C38 C37 120.0 . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 C52 117.7(7) . . ? C38 C39 C52 122.3(7) . . ? C39 C40 C41 120.0 . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 C43 124.2(7) . . ? C42 C41 C43 115.7(7) . . ? C41 C42 C37 120.0 . . ? C41 C42 H42A 120.0 . . ? C37 C42 H42A 120.0 . . ? C53 O11 C52 120.6(4) . . ? C52 O11 C54 155.4(6) . 2_466 ? O11 C52 C39 106.6(5) . . ? O11 C52 H52A 110.4 . . ? C39 C52 H52A 110.4 . . ? O11 C52 H52B 110.4 . . ? C39 C52 H52B 110.4 . . ? H52A C52 H52B 108.6 . . ? C54 C53 O12 143.7(8) 2_466 . ? C54 C53 O11 99.5(8) 2_466 . ? O12 C53 O11 116.56(10) . . ? O12 C53 C54 125.22(10) . . ? O11 C53 C54 118.22(9) . . ? C54 C54 C53 124(2) 2_466 2_466 ? C53 C54 C53 160.9(8) 2_466 . ? C54 C54 O11 167(3) 2_466 2_466 ? C53 C54 O11 152.9(5) . 2_466 ? C54 C54 H54A 144.6 2_466 . ? C53 C54 H54A 89.2 2_466 . ? C53 C54 H54A 109.5 . . ? C54 C54 H54B 83.5 2_466 . ? C53 C54 H54B 58.5 2_466 . ? C53 C54 H54B 109.3 . . ? O11 C54 H54B 83.4 2_466 . ? H54A C54 H54B 109.5 . . ? C54 C54 H54C 95.9 2_466 . ? C53 C54 H54C 65.8 2_466 . ? C53 C54 H54C 109.6 . . ? O11 C54 H54C 87.1 2_466 . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C38' C37' C42' 120.0 . . ? C38' C37' C36 122.3(8) . . ? C42' C37' C36 117.6(8) . . ? C37' C38' C39' 120.0 . . ? C37' C38' H38B 120.0 . . ? C39' C38' H38B 120.0 . . ? C40' C39' C38' 120.0 . . ? C40' C39' C52' 118.7(7) . . ? C38' C39' C52' 121.3(7) . . ? C41' C40' C39' 120.0 . . ? C41' C40' H40B 120.0 . . ? C39' C40' H40B 120.0 . . ? C40' C41' C42' 120.0 . . ? C40' C41' C43 113.6(7) . . ? C42' C41' C43 126.4(7) . . ? C41' C42' C37' 120.0 . . ? C41' C42' H42B 120.0 . . ? C37' C42' H42B 120.0 . . ? C53' O11' C52' 122.1(6) . . ? C53' O12' Cu1 138.0(5) . 2_467 ? O11' C52' C39' 108.9(5) . . ? O11' C52' H52C 109.9 . . ? C39' C52' H52C 109.9 . . ? O11' C52' H52D 109.9 . . ? C39' C52' H52D 109.9 . . ? H52C C52' H52D 108.3 . . ? O12' C53' O11' 116.53(10) . . ? O12' C53' C54' 125.18(10) . . ? O11' C53' C54' 118.29(9) . . ? C53' C54' H54D 109.5 . . ? C53' C54' H54E 109.5 . . ? H54D C54' H54E 109.5 . . ? C53' C54' H54F 109.5 . . ? H54D C54' H54F 109.5 . . ? H54E C54' H54F 109.5 . . ? C1S O1S Cu1 131.1(16) . . ? C1S N1S C4S 126.5(11) . . ? C1S N1S C2S 114.0(11) . . ? C4S N1S C2S 117.5(11) . . ? O1S C1S N1S 129.0(17) . . ? O1S C1S H1SA 115.5 . . ? N1S C1S H1SA 115.5 . . ? C3S C2S N1S 106.7(9) . . ? C3S C2S H2SA 110.4 . . ? N1S C2S H2SA 110.4 . . ? C3S C2S H2SB 110.4 . . ? N1S C2S H2SB 110.4 . . ? H2SA C2S H2SB 108.6 . . ? C2S C3S H3SA 109.5 . . ? C2S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C2S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? N1S C4S C5S 117.7(9) . . ? N1S C4S C5S' 117.6(9) . . ? C5S C4S C5S' 101(2) . . ? N1S C4S H4SA 106.4 . . ? C5S C4S H4SA 107.8 . . ? N1S C4S H4SB 108.1 . . ? C5S C4S H4SB 109.3 . . ? C5S' C4S H4SB 102.3 . . ? H4SA C4S H4SB 107.2 . . ? N1S C4S H4SC 105.9 . . ? C5S C4S H4SC 104.4 . . ? C5S' C4S H4SC 109.9 . . ? H4SA C4S H4SC 115.1 . . ? N1S C4S H4SD 106.9 . . ? C5S' C4S H4SD 109.8 . . ? H4SA C4S H4SD 115.8 . . ? H4SB C4S H4SD 112.2 . . ? H4SC C4S H4SD 106.0 . . ? C4S C5S H5SA 109.5 . . ? H4SD C5S H5SA 97.6 . . ? C4S C5S H5SB 109.5 . . ? H4SD C5S H5SB 102.5 . . ? H5SA C5S H5SB 109.5 . . ? C4S C5S H5SC 109.5 . . ? H4SD C5S H5SC 127.0 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? C4S C5S' H5SD 109.5 . . ? H4SA C5S' H5SD 95.4 . . ? C4S C5S' H5SE 109.5 . . ? H4SA C5S' H5SE 126.9 . . ? H5SD C5S' H5SE 109.5 . . ? C4S C5S' H5SF 109.5 . . ? H4SA C5S' H5SF 104.7 . . ? H5SD C5S' H5SF 109.5 . . ? H5SE C5S' H5SF 109.5 . . ? C11S N3S C12S 116.0(7) . . ? C11S N3S C14S 126.0(10) . . ? C12S N3S C14S 118.0(7) . . ? O3S C11S N3S 120.7(10) . . ? O3S C11S H11B 119.7 . . ? N3S C11S H11B 119.7 . . ? C12S C13S H13B 109.5 . . ? C12S C13S H13C 109.5 . . ? H13B C13S H13C 109.5 . . ? C12S C13S H13D 109.5 . . ? H13B C13S H13D 109.5 . . ? H13C C13S H13D 109.5 . . ? N3S C12S C13S 111.91(11) . . ? N3S C12S H12A 109.2 . . ? C13S C12S H12A 109.2 . . ? N3S C12S H12B 109.2 . . ? C13S C12S H12B 109.2 . . ? H12A C12S H12B 107.9 . . ? C14S C15S H15B 109.5 . . ? C14S C15S H15C 109.5 . . ? H15B C15S H15C 109.5 . . ? C14S C15S H15D 109.5 . . ? H15B C15S H15D 109.5 . . ? H15C C15S H15D 109.5 . . ? N3S C14S C15S 111.67(11) . . ? N3S C14S H14A 109.3 . . ? C15S C14S H14A 109.3 . . ? N3S C14S H14B 109.3 . . ? C15S C14S H14B 109.3 . . ? H14A C14S H14B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.968 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.085 _publ_section_references ; Bruker (2001). SAINTP+ for NT. Data Reduction and Correction Program v. 6.2, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005). APEX2 software package. Bruker Molecular Analysis Research Tool, v. 2008.4 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SADABS-2008/1, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SHELXTL 2008/4, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.086 0.000 0.414 920 285 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT366_MOP2 ; PROBLEM: Short? C(sp?)-C(sp?) Bond C35 - C36 ... 1.19 Ang. RESPONSE:Bonds C35-C36 and C43-C44 are normal C(sp)-C(sp) triple bonds. ; _vrf_PLAT413_MOP2 ; PROBLEM: Short Inter XH3 .. XHn H13D .. H27B .. 1.60 Ang. RESPONSE:Since the structure is highly disordered it is very problematic to find correct positions of hydrogen atoms. Even use of the refinement with AFIX 137 do not give any results. ; # end Validation Reply Form # Attachment 'MOP-3_luke22_sq_fs.cif' data_MOP3 _database_code_depnum_ccdc_archive 'CCDC 797904' #TrackingRef 'MOP-3_luke22_sq_fs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C124 H96 Cu4 O28' _chemical_formula_sum 'C124 H96 Cu4 O28' _chemical_formula_weight 2288.17 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 'C 2/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 26.047(5) _cell_length_b 18.101(3) _cell_length_c 33.213(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.478(2) _cell_angle_gamma 90.00 _cell_volume 15091(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4127 _cell_measurement_theta_min 2.1774 _cell_measurement_theta_max 19.6967 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4720 _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8375 _exptl_absorpt_correction_T_max 0.9413 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56618 _diffrn_reflns_av_R_equivalents 0.1011 _diffrn_reflns_av_sigmaI/netI 0.1453 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14663 _reflns_number_gt 6129 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0300P)^2^+110.0000P] 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 14663 _refine_ls_number_parameters 494 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1718 _refine_ls_R_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.2195 _refine_ls_wR_factor_gt 0.2008 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.88899(3) 0.65671(5) 0.60512(2) 0.0450(2) Uani 1 1 d . . . Cu2 Cu 0.96465(3) 0.59746(5) 0.66486(2) 0.0459(2) Uani 1 1 d . . . O1 O 0.9039(2) 0.5739(3) 0.57258(13) 0.0583(14) Uani 1 1 d . . . O2 O 0.97459(19) 0.5313(3) 0.62194(13) 0.0568(13) Uani 1 1 d . . . O3 O 0.61109(17) 0.7694(2) 0.35149(13) 0.0482(12) Uani 1 1 d . . . O4 O 0.55245(17) 0.8280(3) 0.29909(13) 0.0477(12) Uani 1 1 d . . . O5 O 0.83992(18) 0.5952(3) 0.62604(14) 0.0577(13) Uani 1 1 d . . . O6 O 0.9060(2) 0.5362(3) 0.67275(14) 0.0594(13) Uani 1 1 d . . . O7 O 0.55253(18) 0.7893(3) 0.40850(13) 0.0508(12) Uani 1 1 d . . . O8 O 0.48943(17) 0.8292(3) 0.35225(13) 0.0496(12) Uani 1 1 d . . . O9 O 0.8285(2) 0.7082(4) 0.55608(17) 0.103(2) Uani 1 1 d . . . O10 O 1.0231(2) 0.5426(4) 0.71475(16) 0.104(2) Uani 1 1 d . . . C1 C 0.9437(4) 0.5316(4) 0.5850(2) 0.062(2) Uani 1 1 d . . . C2 C 0.9554(2) 0.4781(3) 0.55467(12) 0.0771(11) Uani 1 1 d G . . C3 C 0.9268(2) 0.4839(3) 0.51299(14) 0.0771(11) Uani 1 1 d G . . H3A H 0.8995 0.5200 0.5048 0.092 Uiso 1 1 calc R . . C4 C 0.9381(2) 0.4370(3) 0.48337(10) 0.0771(11) Uani 1 1 d GD . . C5 C 0.9781(2) 0.3842(3) 0.49543(12) 0.0771(11) Uani 1 1 d G . . H5A H 0.9858 0.3521 0.4752 0.092 Uiso 1 1 calc R . . C6 C 1.00670(19) 0.3784(3) 0.53711(14) 0.0771(11) Uani 1 1 d G . . H6A H 1.0340 0.3424 0.5454 0.092 Uiso 1 1 calc R . . C7 C 0.9954(2) 0.4254(3) 0.56673(10) 0.0771(11) Uani 1 1 d G . . H7A H 1.0149 0.4214 0.5952 0.092 Uiso 1 1 calc R . . C8 C 0.9090(3) 0.4432(5) 0.44005(11) 0.071(2) Uani 1 1 d D . . C9 C 0.8838(3) 0.4506(4) 0.40440(12) 0.070(2) Uani 1 1 d D . . C10 C 0.85383(18) 0.4531(3) 0.36116(10) 0.062(2) Uani 1 1 d GD . . C11 C 0.8053(2) 0.4899(3) 0.34959(13) 0.071(2) Uani 1 1 d G . . H11A H 0.7927 0.5157 0.3700 0.085 Uiso 1 1 calc R . . C12 C 0.77514(16) 0.4891(3) 0.30817(15) 0.066(2) Uani 1 1 d GD . . C13 C 0.79358(19) 0.4514(3) 0.27833(10) 0.069(2) Uani 1 1 d G . . H13A H 0.7730 0.4508 0.2500 0.083 Uiso 1 1 calc R . . C14 C 0.8422(2) 0.4146(3) 0.28990(12) 0.066(2) Uani 1 1 d G B . C15 C 0.87228(16) 0.4155(3) 0.33132(14) 0.064(2) Uani 1 1 d G . . H15A H 0.9055 0.3903 0.3392 0.077 Uiso 1 1 calc R . . C16 C 0.7255(2) 0.5288(4) 0.2951(2) 0.069(2) Uani 1 1 d D . . C17 C 0.6850(2) 0.5630(4) 0.2837(2) 0.069(2) Uani 1 1 d D . . C18 C 0.63960(16) 0.6111(2) 0.27051(15) 0.057(2) Uani 1 1 d GD . . C19 C 0.63156(16) 0.6652(3) 0.29792(10) 0.0468(17) Uani 1 1 d G . . H19A H 0.6533 0.6663 0.3259 0.056 Uiso 1 1 calc R . . C20 C 0.59176(17) 0.7177(2) 0.28441(12) 0.0430(16) Uani 1 1 d G . . C21 C 0.56001(15) 0.7162(2) 0.24349(13) 0.0495(18) Uani 1 1 d G . . H21A H 0.5328 0.7521 0.2343 0.059 Uiso 1 1 calc R . . C22 C 0.56804(17) 0.6622(3) 0.21608(10) 0.064(2) Uani 1 1 d G . . H22A H 0.5463 0.6611 0.1881 0.077 Uiso 1 1 calc R . . C23 C 0.60784(19) 0.6096(2) 0.22959(14) 0.071(2) Uani 1 1 d G . . H23A H 0.6133 0.5727 0.2109 0.085 Uiso 1 1 calc R . . C24 C 0.5847(3) 0.7763(4) 0.3140(2) 0.0411(16) Uani 1 1 d . . . C25 C 0.8632(3) 0.3734(5) 0.2583(2) 0.079(3) Uani 1 1 d D . . H25A H 0.8840 0.4076 0.2455 0.095 Uiso 1 1 calc R A 1 H25B H 0.8873 0.3335 0.2725 0.095 Uiso 1 1 calc R A 1 O11 O 0.8205(5) 0.3418(7) 0.2259(4) 0.1417(18) Uani 0.70 1 d PD B 1 O12 O 0.8085(7) 0.2587(9) 0.2729(3) 0.1417(18) Uani 0.70 1 d PD B 1 C26 C 0.7960(6) 0.2830(9) 0.2376(3) 0.1417(18) Uani 0.70 1 d PD B 1 C27 C 0.7491(5) 0.2456(7) 0.2079(3) 0.1417(18) Uani 0.70 1 d PD B 1 H27A H 0.7572 0.1926 0.2054 0.170 Uiso 0.70 1 calc PR B 1 H27B H 0.7174 0.2492 0.2189 0.170 Uiso 0.70 1 calc PR B 1 C28 C 0.7377(4) 0.2820(7) 0.1655(3) 0.1417(18) Uani 0.70 1 d PD B 1 H28A H 0.7680 0.2741 0.1534 0.170 Uiso 0.70 1 calc PR B 1 H28B H 0.7331 0.3358 0.1685 0.170 Uiso 0.70 1 calc PR B 1 C29 C 0.6876(5) 0.2496(7) 0.1370(3) 0.1417(18) Uani 0.70 1 d PD B 1 H29A H 0.6930 0.1964 0.1327 0.170 Uiso 0.70 1 calc PR B 1 H29B H 0.6578 0.2547 0.1501 0.170 Uiso 0.70 1 calc PR B 1 C30 C 0.6742(5) 0.2894(7) 0.0956(3) 0.1417(18) Uani 0.70 1 d PD B 1 H30A H 0.6663 0.3419 0.0997 0.170 Uiso 0.70 1 calc PR B 1 H30B H 0.7051 0.2874 0.0835 0.170 Uiso 0.70 1 calc PR B 1 C31 C 0.6265(5) 0.2535(8) 0.0660(3) 0.1417(18) Uani 0.70 1 d PD B 1 H31A H 0.6171 0.2808 0.0395 0.213 Uiso 0.70 1 calc PR B 1 H31B H 0.5964 0.2542 0.0784 0.213 Uiso 0.70 1 calc PR B 1 H31C H 0.6352 0.2023 0.0608 0.213 Uiso 0.70 1 calc PR B 1 O11' O 0.8208(9) 0.3426(12) 0.2254(7) 0.1417(18) Uani 0.30 1 d PD B 2 O12' O 0.8009(14) 0.2595(19) 0.2636(7) 0.1417(18) Uani 0.30 1 d PD B 2 C26' C 0.7875(8) 0.2874(11) 0.2293(6) 0.1417(18) Uani 0.30 1 d PD B 2 C27' C 0.7395(6) 0.2629(11) 0.1954(7) 0.1417(18) Uani 0.30 1 d PD B 2 H27C H 0.7122 0.2426 0.2081 0.170 Uiso 0.30 1 calc PR B 2 H27D H 0.7238 0.3057 0.1778 0.170 Uiso 0.30 1 calc PR B 2 C28' C 0.7557(8) 0.2045(16) 0.1687(7) 0.1417(18) Uani 0.30 1 d PD B 2 H28C H 0.7854 0.2231 0.1582 0.170 Uiso 0.30 1 calc PR B 2 H28D H 0.7680 0.1598 0.1856 0.170 Uiso 0.30 1 calc PR B 2 C29' C 0.7089(7) 0.1854(18) 0.1323(6) 0.1417(18) Uani 0.30 1 d PD B 2 H29C H 0.6829 0.2266 0.1269 0.170 Uiso 0.30 1 calc PR B 2 H29D H 0.6908 0.1407 0.1390 0.170 Uiso 0.30 1 calc PR B 2 C30' C 0.7279(8) 0.171(2) 0.0938(6) 0.1417(18) Uani 0.30 1 d PD B 2 H30C H 0.7508 0.1269 0.0981 0.170 Uiso 0.30 1 calc PR B 2 H30D H 0.7493 0.2140 0.0888 0.170 Uiso 0.30 1 calc PR B 2 C31' C 0.6806(11) 0.160(2) 0.0565(5) 0.1417(18) Uani 0.30 1 d PD B 2 H31D H 0.6931 0.1464 0.0322 0.213 Uiso 0.30 1 calc PR B 2 H31E H 0.6602 0.2064 0.0505 0.213 Uiso 0.30 1 calc PR B 2 H31F H 0.6579 0.1210 0.0625 0.213 Uiso 0.30 1 calc PR B 2 C32 C 0.8568(3) 0.5475(4) 0.6545(2) 0.058(2) Uani 1 1 d D . . O13 O 0.4422(6) 0.4531(7) 0.6604(4) 0.578(13) Uani 0.50 1 d PD C 1 O14 O 0.3806(6) 0.5293(11) 0.6279(5) 0.578(13) Uani 0.50 1 d PD C 1 C33 C 0.8149(4) 0.5030(7) 0.6675(4) 0.0660(11) Uani 0.50 1 d PGD C 1 C34 C 0.7609(5) 0.5109(5) 0.6478(3) 0.0660(11) Uani 0.50 1 d PGD C 1 H34A H 0.7493 0.5479 0.6271 0.079 Uiso 0.50 1 calc PR C 1 C35 C 0.7240(2) 0.4648(6) 0.6585(3) 0.0660(11) Uani 0.50 1 d PGD C 1 C36 C 0.7410(4) 0.4106(6) 0.6888(4) 0.0660(11) Uani 0.50 1 d PGD C 1 H36A H 0.7158 0.3791 0.6961 0.079 Uiso 0.50 1 calc PR C 1 C37 C 0.7950(5) 0.4027(6) 0.7085(3) 0.0660(11) Uani 0.50 1 d PGD C 1 H37A H 0.8066 0.3657 0.7292 0.079 Uiso 0.50 1 calc PR C 1 C38 C 0.8319(2) 0.4489(7) 0.6978(3) 0.0660(11) Uani 0.50 1 d PGD C 1 H38A H 0.8688 0.4435 0.7112 0.079 Uiso 0.50 1 calc PR C 1 C39 C 0.6685(3) 0.4754(9) 0.6372(4) 0.071(3) Uani 0.50 1 d PD C 1 C40 C 0.6220(2) 0.4849(7) 0.6230(4) 0.071(3) Uani 0.50 1 d PD C 1 C41 C 0.5661(2) 0.4876(5) 0.6015(3) 0.0988(19) Uani 0.50 1 d PGD C 1 C42 C 0.5480(3) 0.5237(4) 0.5634(3) 0.0988(19) Uani 0.50 1 d PGD C 1 H42A H 0.5727 0.5471 0.5510 0.119 Uiso 0.50 1 calc PR C 1 C43 C 0.4939(4) 0.5254(4) 0.54334(19) 0.0988(19) Uani 0.50 1 d PGD C 1 C44 C 0.4578(2) 0.4910(5) 0.5614(3) 0.0988(19) Uani 0.50 1 d PGD C 1 H44A H 0.4208 0.4922 0.5477 0.119 Uiso 0.50 1 calc PR C 1 C45 C 0.4758(3) 0.4549(4) 0.5995(3) 0.0988(19) Uani 0.50 1 d PGD C 1 C46 C 0.5300(4) 0.4532(4) 0.61956(18) 0.0988(19) Uani 0.50 1 d PGD C 1 H46A H 0.5423 0.4286 0.6456 0.119 Uiso 0.50 1 calc PR C 1 C47 C 0.4748(7) 0.5626(6) 0.5038(2) 0.094(3) Uani 0.50 1 d PD C 1 C48 C 0.4618(6) 0.5980(7) 0.4725(3) 0.094(3) Uani 0.50 1 d PD C 1 C49 C 0.4448(4) 0.6456(5) 0.43666(19) 0.0668(15) Uani 0.50 1 d PGD C 1 C50 C 0.4809(4) 0.6962(6) 0.4285(3) 0.0668(15) Uani 0.50 1 d PGD C 1 H50A H 0.5160 0.6989 0.4464 0.080 Uiso 0.50 1 calc PR C 1 C51 C 0.4656(5) 0.7428(6) 0.3941(3) 0.0668(15) Uani 0.50 1 d PGD C 1 C52 C 0.4142(5) 0.7388(5) 0.3679(2) 0.0668(15) Uani 0.50 1 d PGD C 1 H52A H 0.4038 0.7706 0.3443 0.080 Uiso 0.50 1 calc PR C 1 C53 C 0.3781(4) 0.6882(6) 0.3760(3) 0.0668(15) Uani 0.50 1 d PGD C 1 H53A H 0.3430 0.6854 0.3581 0.080 Uiso 0.50 1 calc PR C 1 C54 C 0.3934(4) 0.6416(5) 0.4104(3) 0.0668(15) Uani 0.50 1 d PGD C 1 H54A H 0.3688 0.6070 0.4160 0.080 Uiso 0.50 1 calc PR C 1 C55 C 0.5026(14) 0.7990(9) 0.3833(14) 0.037(5) Uani 0.50 1 d PD C 1 C56 C 0.4395(6) 0.4162(7) 0.6214(5) 0.578(13) Uani 0.50 1 d PD C 1 H56A H 0.4025 0.4170 0.6035 0.693 Uiso 0.50 1 calc PR C 1 H56B H 0.4507 0.3640 0.6268 0.693 Uiso 0.50 1 calc PR C 1 C57 C 0.4129(5) 0.5145(7) 0.6602(4) 0.578(13) Uani 0.50 1 d PD C 1 C58 C 0.4227(6) 0.5588(12) 0.6998(7) 0.578(13) Uani 0.50 1 d PD C 1 H58A H 0.4386 0.6071 0.6958 0.693 Uiso 0.50 1 calc PR C 1 H58B H 0.4483 0.5323 0.7227 0.693 Uiso 0.50 1 calc PR C 1 C59 C 0.3712(10) 0.5709(15) 0.7114(8) 0.578(13) Uani 0.50 1 d PD C 1 H59A H 0.3636 0.5277 0.7272 0.693 Uiso 0.50 1 calc PR C 1 H59B H 0.3415 0.5762 0.6858 0.693 Uiso 0.50 1 calc PR C 1 C60 C 0.3753(12) 0.6397(10) 0.7378(8) 0.578(13) Uani 0.50 1 d PD C 1 H60A H 0.3433 0.6707 0.7272 0.693 Uiso 0.50 1 calc PR C 1 H60B H 0.4069 0.6688 0.7361 0.693 Uiso 0.50 1 calc PR C 1 C61 C 0.3803(15) 0.6186(17) 0.7827(6) 0.578(13) Uani 0.50 1 d PD C 1 H61A H 0.3644 0.5692 0.7838 0.693 Uiso 0.50 1 calc PR C 1 H61B H 0.4184 0.6162 0.7983 0.693 Uiso 0.50 1 calc PR C 1 C62 C 0.352(2) 0.675(2) 0.8026(13) 0.578(13) Uani 0.50 1 d PD C 1 H62A H 0.3640 0.6700 0.8331 0.867 Uiso 0.50 1 calc PR C 1 H62B H 0.3135 0.6668 0.7931 0.867 Uiso 0.50 1 calc PR C 1 H62C H 0.3604 0.7248 0.7946 0.867 Uiso 0.50 1 calc PR C 1 O13' O 0.4301(6) 0.6367(8) 0.6828(7) 0.578(13) Uani 0.50 1 d PD C 2 O14' O 0.4182(10) 0.6947(14) 0.7362(7) 0.578(13) Uani 0.50 1 d PD C 2 C33' C 0.8152(4) 0.4997(7) 0.6658(4) 0.0660(11) Uani 0.50 1 d PGD C 2 C34' C 0.7623(5) 0.5226(4) 0.6541(3) 0.0660(11) Uani 0.50 1 d PGD C 2 H34B H 0.7524 0.5655 0.6374 0.079 Uiso 0.50 1 calc PR C 2 C35' C 0.7240(2) 0.4827(6) 0.6671(3) 0.0660(11) Uani 0.50 1 d PGD C 2 C36' C 0.7385(4) 0.4200(7) 0.6916(4) 0.0660(11) Uani 0.50 1 d PGD C 2 H36B H 0.7123 0.3927 0.7004 0.079 Uiso 0.50 1 calc PR C 2 C37' C 0.7913(5) 0.3971(5) 0.7032(4) 0.0660(11) Uani 0.50 1 d PGD C 2 H37B H 0.8012 0.3543 0.7200 0.079 Uiso 0.50 1 calc PR C 2 C38' C 0.8297(2) 0.4370(7) 0.6903(4) 0.0660(11) Uani 0.50 1 d PGD C 2 H38B H 0.8658 0.4214 0.6982 0.079 Uiso 0.50 1 calc PR C 2 C39' C 0.6691(3) 0.5062(9) 0.6551(4) 0.071(3) Uani 0.50 1 d PD C 2 C40' C 0.6255(3) 0.5318(5) 0.6471(5) 0.071(3) Uani 0.50 1 d PD C 2 C41' C 0.5770(2) 0.5745(4) 0.6364(3) 0.0988(19) Uani 0.50 1 d PGD C 2 C42' C 0.5527(4) 0.5862(4) 0.5943(3) 0.0988(19) Uani 0.50 1 d PGD C 2 H42B H 0.5681 0.5663 0.5737 0.119 Uiso 0.50 1 calc PR C 2 C43' C 0.5059(4) 0.6269(5) 0.58219(19) 0.0988(19) Uani 0.50 1 d PGD C 2 C44' C 0.4833(2) 0.6560(4) 0.6123(3) 0.0988(19) Uani 0.50 1 d PGD C 2 H44B H 0.4513 0.6838 0.6040 0.119 Uiso 0.50 1 calc PR C 2 C45' C 0.5076(3) 0.6443(4) 0.6544(3) 0.0988(19) Uani 0.50 1 d PGD C 2 C46' C 0.5544(3) 0.6035(5) 0.66649(18) 0.0988(19) Uani 0.50 1 d PGD C 2 H46B H 0.5710 0.5955 0.6953 0.119 Uiso 0.50 1 calc PR C 2 C47' C 0.4789(6) 0.6409(9) 0.5390(2) 0.094(3) Uani 0.50 1 d PD C 2 C48' C 0.4621(6) 0.6523(7) 0.50252(19) 0.094(3) Uani 0.50 1 d PD C 2 C49' C 0.4442(4) 0.6816(5) 0.46075(16) 0.0668(15) Uani 0.50 1 d PGD C 2 C50' C 0.4811(4) 0.7152(6) 0.4432(3) 0.0668(15) Uani 0.50 1 d PGD C 2 H50B H 0.5174 0.7186 0.4587 0.080 Uiso 0.50 1 calc PR C 2 C51' C 0.4649(5) 0.7440(6) 0.4030(3) 0.0668(15) Uani 0.50 1 d PGD C 2 C52' C 0.4118(5) 0.7390(6) 0.3803(2) 0.0668(15) Uani 0.50 1 d PGD C 2 H52B H 0.4007 0.7587 0.3528 0.080 Uiso 0.50 1 calc PR C 2 C53' C 0.3749(4) 0.7053(6) 0.3978(3) 0.0668(15) Uani 0.50 1 d PGD C 2 H53B H 0.3386 0.7020 0.3823 0.080 Uiso 0.50 1 calc PR C 2 C54' C 0.3911(4) 0.6766(5) 0.4381(2) 0.0668(15) Uani 0.50 1 d PGD C 2 H54B H 0.3659 0.6536 0.4500 0.080 Uiso 0.50 1 calc PR C 2 C55' C 0.5080(14) 0.7794(10) 0.3869(15) 0.037(5) Uani 0.50 1 d PD C 2 C56' C 0.4734(11) 0.6826(10) 0.6782(13) 0.578(13) Uani 0.50 1 d PD C 2 H56C H 0.4957 0.6965 0.7063 0.693 Uiso 0.50 1 calc PR C 2 H56D H 0.4587 0.7285 0.6634 0.693 Uiso 0.50 1 calc PR C 2 C57' C 0.3965(6) 0.6627(7) 0.7042(6) 0.578(13) Uani 0.50 1 d PD C 2 C58' C 0.3369(6) 0.6522(13) 0.6890(9) 0.578(13) Uani 0.50 1 d PD C 2 H58C H 0.3288 0.6022 0.6769 0.693 Uiso 0.50 1 calc PR C 2 H58D H 0.3209 0.6566 0.7128 0.693 Uiso 0.50 1 calc PR C 2 C59' C 0.3133(7) 0.7098(16) 0.6565(10) 0.578(13) Uani 0.50 1 d PD C 2 H59C H 0.3292 0.7053 0.6327 0.693 Uiso 0.50 1 calc PR C 2 H59D H 0.3214 0.7598 0.6687 0.693 Uiso 0.50 1 calc PR C 2 C60' C 0.2537(6) 0.6995(19) 0.6414(9) 0.578(13) Uani 0.50 1 d PD C 2 H60C H 0.2355 0.7469 0.6433 0.693 Uiso 0.50 1 calc PR C 2 H60D H 0.2420 0.6630 0.6593 0.693 Uiso 0.50 1 calc PR C 2 C61' C 0.2387(13) 0.673(2) 0.5967(9) 0.578(13) Uani 0.50 1 d PD C 2 H61C H 0.2452 0.7126 0.5782 0.693 Uiso 0.50 1 calc PR C 2 H61D H 0.2004 0.6601 0.5880 0.693 Uiso 0.50 1 calc PR C 2 C62' C 0.272(3) 0.606(2) 0.5929(16) 0.578(13) Uani 0.50 1 d PD C 2 H62D H 0.2632 0.5903 0.5636 0.867 Uiso 0.50 1 calc PR C 2 H62E H 0.2631 0.5654 0.6098 0.867 Uiso 0.50 1 calc PR C 2 H62F H 0.3095 0.6179 0.6028 0.867 Uiso 0.50 1 calc PR C 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 0.0439(5) 0.0622(6) 0.0269(4) 0.0011(4) 0.0061(3) 0.0021(4) Cu2 0.0486(5) 0.0587(5) 0.0281(4) -0.0007(4) 0.0064(4) 0.0074(4) O1 0.068(4) 0.072(4) 0.030(3) -0.007(2) 0.006(2) 0.008(3) O2 0.076(4) 0.060(3) 0.031(3) -0.005(2) 0.008(2) 0.009(3) O3 0.050(3) 0.061(3) 0.033(3) -0.005(2) 0.009(2) 0.006(2) O4 0.038(3) 0.065(3) 0.039(3) -0.007(2) 0.009(2) 0.012(2) O5 0.059(3) 0.069(3) 0.047(3) -0.006(3) 0.016(2) -0.011(3) O6 0.059(3) 0.067(3) 0.053(3) 0.005(3) 0.016(3) -0.003(3) O7 0.045(3) 0.067(3) 0.038(3) 0.011(2) 0.008(2) 0.004(3) O8 0.045(3) 0.065(3) 0.037(3) 0.004(2) 0.008(2) 0.011(2) O9 0.063(4) 0.156(6) 0.066(4) 0.012(4) -0.021(3) 0.029(4) O10 0.084(4) 0.177(7) 0.047(3) 0.045(4) 0.012(3) 0.046(4) C1 0.095(7) 0.051(5) 0.041(5) 0.000(4) 0.020(5) -0.004(5) C2 0.100(3) 0.080(3) 0.0465(18) -0.0150(17) 0.0117(19) 0.018(2) C3 0.100(3) 0.080(3) 0.0465(18) -0.0150(17) 0.0117(19) 0.018(2) C4 0.100(3) 0.080(3) 0.0465(18) -0.0150(17) 0.0117(19) 0.018(2) C5 0.100(3) 0.080(3) 0.0465(18) -0.0150(17) 0.0117(19) 0.018(2) C6 0.100(3) 0.080(3) 0.0465(18) -0.0150(17) 0.0117(19) 0.018(2) C7 0.100(3) 0.080(3) 0.0465(18) -0.0150(17) 0.0117(19) 0.018(2) C8 0.072(6) 0.095(7) 0.041(4) -0.016(4) 0.005(4) 0.012(5) C9 0.068(6) 0.078(6) 0.066(5) -0.018(5) 0.020(5) 0.018(5) C10 0.067(5) 0.071(5) 0.045(4) -0.004(4) 0.011(4) 0.018(4) C11 0.092(7) 0.075(6) 0.050(5) -0.008(4) 0.027(5) 0.020(5) C12 0.071(6) 0.070(5) 0.055(5) -0.008(4) 0.012(4) 0.031(4) C13 0.084(6) 0.076(6) 0.045(4) -0.007(4) 0.012(4) 0.028(5) C14 0.085(6) 0.078(6) 0.033(4) 0.004(4) 0.013(4) 0.039(5) C15 0.073(5) 0.079(6) 0.045(4) 0.001(4) 0.022(4) 0.037(5) C16 0.065(6) 0.077(6) 0.069(5) -0.015(5) 0.029(5) 0.023(5) C17 0.060(5) 0.083(6) 0.064(5) -0.025(5) 0.018(4) 0.011(5) C18 0.045(4) 0.059(5) 0.068(5) -0.001(4) 0.018(4) 0.016(4) C19 0.050(4) 0.054(5) 0.037(4) -0.003(3) 0.013(3) 0.002(4) C20 0.038(4) 0.053(4) 0.043(4) -0.008(3) 0.017(3) -0.004(3) C21 0.034(4) 0.070(5) 0.047(4) -0.008(4) 0.015(3) 0.003(4) C22 0.056(5) 0.089(6) 0.041(4) -0.023(4) 0.005(4) 0.001(5) C23 0.060(5) 0.088(6) 0.062(5) -0.026(5) 0.013(4) 0.012(5) C24 0.030(4) 0.060(5) 0.039(4) -0.009(3) 0.019(3) -0.010(4) C25 0.096(7) 0.099(7) 0.042(4) -0.003(4) 0.016(5) 0.039(5) O11 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) O12 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C26 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C27 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C28 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C29 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C30 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C31 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) O11' 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) O12' 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C26' 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C27' 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C28' 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C29' 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C30' 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C31' 0.151(4) 0.161(4) 0.099(3) -0.038(3) 0.010(3) 0.049(3) C32 0.071(6) 0.060(5) 0.047(5) -0.012(4) 0.024(4) -0.001(5) O13 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) O14 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C33 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C34 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C35 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C36 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C37 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C38 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C39 0.069(5) 0.094(9) 0.048(7) 0.009(5) 0.011(6) -0.019(6) C40 0.069(5) 0.094(9) 0.048(7) 0.009(5) 0.011(6) -0.019(6) C41 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C42 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C43 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C44 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C45 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C46 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C47 0.078(6) 0.134(9) 0.070(6) 0.030(6) 0.022(6) -0.022(7) C48 0.078(6) 0.134(9) 0.070(6) 0.030(6) 0.022(6) -0.022(7) C49 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C50 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C51 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C52 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C53 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C54 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C55 0.050(7) 0.020(10) 0.040(7) 0.009(12) 0.012(7) 0.022(10) C56 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C57 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C58 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C59 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C60 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C61 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C62 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) O13' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) O14' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C33' 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C34' 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C35' 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C36' 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C37' 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C38' 0.076(2) 0.066(3) 0.055(2) -0.0049(18) 0.017(2) -0.020(2) C39' 0.069(5) 0.094(9) 0.048(7) 0.009(5) 0.011(6) -0.019(6) C40' 0.069(5) 0.094(9) 0.048(7) 0.009(5) 0.011(6) -0.019(6) C41' 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C42' 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C43' 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C44' 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C45' 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C46' 0.089(4) 0.136(5) 0.072(4) 0.033(3) 0.023(3) -0.001(4) C47' 0.078(6) 0.134(9) 0.070(6) 0.030(6) 0.022(6) -0.022(7) C48' 0.078(6) 0.134(9) 0.070(6) 0.030(6) 0.022(6) -0.022(7) C49' 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C50' 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C51' 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C52' 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C53' 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C54' 0.054(2) 0.080(3) 0.068(4) 0.015(3) 0.019(3) -0.005(2) C55' 0.050(7) 0.020(10) 0.040(7) 0.009(12) 0.012(7) 0.022(10) C56' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C57' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C58' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C59' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C60' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C61' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) C62' 0.82(3) 0.315(15) 0.91(3) 0.102(19) 0.77(3) -0.042(17) _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 O1 1.946(5) . ? Cu1 O5 1.957(5) . ? Cu1 O7 1.962(5) 7_666 ? Cu1 O3 1.966(4) 7_666 ? Cu1 O9 2.153(5) . ? Cu1 Cu2 2.6237(11) . ? Cu2 O2 1.932(4) . ? Cu2 O4 1.933(4) 7_666 ? Cu2 O6 1.962(5) . ? Cu2 O8 1.969(5) 7_666 ? Cu2 O10 2.169(5) . ? O1 C1 1.267(9) . ? O2 C1 1.274(8) . ? O3 C24 1.258(7) . ? O3 Cu1 1.966(4) 7_666 ? O4 C24 1.266(8) . ? O4 Cu2 1.933(4) 7_666 ? O5 C32 1.269(8) . ? O6 C32 1.279(8) . ? O7 C55' 1.20(4) . ? O7 C55 1.36(5) . ? O7 Cu1 1.962(5) 7_666 ? O8 C55 1.14(5) . ? O8 C55' 1.44(4) . ? O8 Cu2 1.969(5) 7_666 ? C1 C2 1.486(8) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 C8 1.441(5) . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 C7 1.3900 . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.198(4) . ? C9 C10 1.441(5) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9500 . ? C12 C13 1.3900 . ? C12 C16 1.441(8) . ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 C15 1.3900 . ? C14 C25 1.506(8) . ? C15 H15A 0.9500 . ? C16 C17 1.194(5) . ? C17 C18 1.439(8) . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9500 . ? C20 C21 1.3900 . ? C20 C24 1.490(7) . ? C21 C22 1.3900 . ? C21 H21A 0.9500 . ? C22 C23 1.3900 . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C25 O11' 1.4410(10) . ? C25 O11 1.4413(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? O11 C26 1.3513(10) . ? O12 C26 1.2104(10) . ? C26 C27 1.5101(10) . ? C27 C28 1.5097(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.5104(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.5101(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.5098(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O11' C26' 1.3508(10) . ? O12' C26' 1.2099(10) . ? C26' C27' 1.5099(10) . ? C27' C28' 1.5101(10) . ? C27' H27C 0.9900 . ? C27' H27D 0.9900 . ? C28' C29' 1.5100(10) . ? C28' H28C 0.9900 . ? C28' H28D 0.9900 . ? C29' C30' 1.5100(10) . ? C29' H29C 0.9900 . ? C29' H29D 0.9900 . ? C30' C31' 1.5101(10) . ? C30' H30C 0.9900 . ? C30' H30D 0.9900 . ? C31' H31D 0.9800 . ? C31' H31E 0.9800 . ? C31' H31F 0.9800 . ? C32 C33' 1.5100(10) . ? C32 C33 1.5101(10) . ? O13 C57 1.3471(9) . ? O13 C56 1.4433(10) . ? O14 C57 1.2033(9) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C35 C39 1.4415(11) . ? C36 C37 1.3900 . ? C36 H36A 0.9500 . ? C37 C38 1.3900 . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.1904(10) . ? C40 C41 1.4414(10) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 H42A 0.9500 . ? C43 C44 1.3900 . ? C43 C47 1.4410(10) . ? C44 C45 1.3900 . ? C44 H44A 0.9500 . ? C45 C46 1.3900 . ? C45 C56 1.5104(10) . ? C46 H46A 0.9500 . ? C47 C48 1.1900(10) . ? C48 C49 1.4411(10) . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C50 H50A 0.9500 . ? C51 C52 1.3900 . ? C51 C55 1.5102(11) . ? C52 C53 1.3900 . ? C52 H52A 0.9500 . ? C53 C54 1.3900 . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.5011(9) . ? C58 C59 1.5099(11) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.5101(10) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.5100(11) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.5100(10) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O13' C57' 1.3512(10) . ? O13' C56' 1.4411(11) . ? O14' C57' 1.2102(10) . ? C33' C34' 1.3900 . ? C33' C38' 1.3900 . ? C34' C35' 1.3900 . ? C34' H34B 0.9500 . ? C35' C36' 1.3900 . ? C35' C39' 1.4414(11) . ? C36' C37' 1.3900 . ? C36' H36B 0.9500 . ? C37' C38' 1.3900 . ? C37' H37B 0.9500 . ? C38' H38B 0.9500 . ? C39' C40' 1.1903(10) . ? C40' C41' 1.4413(10) . ? C41' C42' 1.3900 . ? C41' C46' 1.3900 . ? C42' C43' 1.3900 . ? C42' H42B 0.9500 . ? C43' C44' 1.3900 . ? C43' C47' 1.4416(10) . ? C44' C45' 1.3900 . ? C44' H44B 0.9500 . ? C45' C46' 1.3900 . ? C45' C56' 1.5101(10) . ? C46' H46B 0.9500 . ? C47' C48' 1.1906(10) . ? C48' C49' 1.4415(10) . ? C49' C50' 1.3900 . ? C49' C54' 1.3900 . ? C50' C51' 1.3900 . ? C50' H50B 0.9500 . ? C51' C52' 1.3900 . ? C51' C55' 1.5102(11) . ? C52' C53' 1.3900 . ? C52' H52B 0.9500 . ? C53' C54' 1.3900 . ? C53' H53B 0.9500 . ? C54' H54B 0.9500 . ? C56' H56C 0.9900 . ? C56' H56D 0.9900 . ? C57' C58' 1.5101(11) . ? C58' C59' 1.5098(10) . ? C58' H58C 0.9900 . ? C58' H58D 0.9900 . ? C59' C60' 1.5100(11) . ? C59' H59C 0.9900 . ? C59' H59D 0.9900 . ? C60' C61' 1.5101(11) . ? C60' H60C 0.9900 . ? C60' H60D 0.9900 . ? C61' C62' 1.5101(10) . ? C61' H61C 0.9900 . ? C61' H61D 0.9900 . ? C62' H62D 0.9800 . ? C62' H62E 0.9800 . ? C62' H62F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O5 90.3(2) . . ? O1 Cu1 O7 88.5(2) . 7_666 ? O5 Cu1 O7 170.5(2) . 7_666 ? O1 Cu1 O3 165.91(19) . 7_666 ? O5 Cu1 O3 89.87(19) . 7_666 ? O7 Cu1 O3 89.03(19) 7_666 7_666 ? O1 Cu1 O9 97.3(2) . . ? O5 Cu1 O9 95.7(2) . . ? O7 Cu1 O9 93.8(2) 7_666 . ? O3 Cu1 O9 96.7(2) 7_666 . ? O1 Cu1 Cu2 83.36(14) . . ? O5 Cu1 Cu2 85.93(15) . . ? O7 Cu1 Cu2 84.56(13) 7_666 . ? O3 Cu1 Cu2 82.59(13) 7_666 . ? O9 Cu1 Cu2 178.22(19) . . ? O2 Cu2 O4 171.25(19) . 7_666 ? O2 Cu2 O6 90.6(2) . . ? O4 Cu2 O6 89.7(2) 7_666 . ? O2 Cu2 O8 89.6(2) . 7_666 ? O4 Cu2 O8 88.09(19) 7_666 7_666 ? O6 Cu2 O8 167.0(2) . 7_666 ? O2 Cu2 O10 94.3(2) . . ? O4 Cu2 O10 94.4(2) 7_666 . ? O6 Cu2 O10 93.0(2) . . ? O8 Cu2 O10 99.9(2) 7_666 . ? O2 Cu2 Cu1 85.23(14) . . ? O4 Cu2 Cu1 86.14(13) 7_666 . ? O6 Cu2 Cu1 82.96(15) . . ? O8 Cu2 Cu1 84.13(13) 7_666 . ? O10 Cu2 Cu1 175.90(19) . . ? C1 O1 Cu1 123.5(4) . . ? C1 O2 Cu2 122.2(5) . . ? C24 O3 Cu1 123.4(4) . 7_666 ? C24 O4 Cu2 120.8(4) . 7_666 ? C32 O5 Cu1 121.5(4) . . ? C32 O6 Cu2 124.2(4) . . ? C55' O7 Cu1 128.4(14) . 7_666 ? C55 O7 Cu1 117.9(9) . 7_666 ? C55 O8 Cu2 121.7(13) . 7_666 ? C55' O8 Cu2 123.5(11) . 7_666 ? O1 C1 O2 124.6(7) . . ? O1 C1 C2 118.1(6) . . ? O2 C1 C2 117.3(7) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 118.3(5) . . ? C7 C2 C1 121.7(5) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 C8 119.7(5) . . ? C3 C4 C8 120.3(5) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C9 C8 C4 177.5(9) . . ? C8 C9 C10 175.4(9) . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 120.2(4) . . ? C15 C10 C9 119.8(4) . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 C16 118.8(4) . . ? C11 C12 C16 121.1(4) . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 C25 121.2(4) . . ? C15 C14 C25 118.8(4) . . ? C14 C15 C10 120.0 . . ? C14 C15 H15A 120.0 . . ? C10 C15 H15A 120.0 . . ? C17 C16 C12 178.3(10) . . ? C16 C17 C18 174.0(9) . . ? C19 C18 C23 120.0 . . ? C19 C18 C17 118.8(4) . . ? C23 C18 C17 120.8(4) . . ? C18 C19 C20 120.0 . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 C24 120.8(4) . . ? C19 C20 C24 119.1(4) . . ? C20 C21 C22 120.0 . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 H23A 120.0 . . ? C18 C23 H23A 120.0 . . ? O3 C24 O4 126.2(6) . . ? O3 C24 C20 116.8(6) . . ? O4 C24 C20 117.0(5) . . ? O11' C25 C14 111.9(14) . . ? O11 C25 C14 111.4(8) . . ? O11' C25 H25A 108.3 . . ? O11 C25 H25A 109.3 . . ? C14 C25 H25A 109.3 . . ? O11' C25 H25B 109.8 . . ? O11 C25 H25B 109.3 . . ? C14 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C26 O11 C25 115.3(10) . . ? O12 C26 O11 122.7(11) . . ? O12 C26 C27 115.5(9) . . ? O11 C26 C27 121.8(5) . . ? C28 C27 C26 109.76(10) . . ? C28 C27 H27A 109.7 . . ? C26 C27 H27A 109.7 . . ? C28 C27 H27B 109.7 . . ? C26 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C27 C28 C29 109.76(10) . . ? C27 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? C27 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C28 109.72(10) . . ? C30 C29 H29A 109.7 . . ? C28 C29 H29A 109.7 . . ? C30 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 109.76(10) . . ? C31 C30 H30A 109.7 . . ? C29 C30 H30A 109.7 . . ? C31 C30 H30B 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26' O11' C25 126.5(16) . . ? O12' C26' O11' 111.58(13) . . ? O12' C26' C27' 123.50(15) . . ? O11' C26' C27' 124.9(2) . . ? C28' C27' C26' 109.74(10) . . ? C28' C27' H27C 109.7 . . ? C26' C27' H27C 109.7 . . ? C28' C27' H27D 109.7 . . ? C26' C27' H27D 109.7 . . ? H27C C27' H27D 108.2 . . ? C29' C28' C27' 109.74(10) . . ? C29' C28' H28C 109.7 . . ? C27' C28' H28C 109.7 . . ? C29' C28' H28D 109.7 . . ? C27' C28' H28D 109.7 . . ? H28C C28' H28D 108.2 . . ? C28' C29' C30' 109.75(10) . . ? C28' C29' H29C 109.7 . . ? C30' C29' H29C 109.7 . . ? C28' C29' H29D 109.7 . . ? C30' C29' H29D 109.7 . . ? H29C C29' H29D 108.2 . . ? C29' C30' C31' 109.74(10) . . ? C29' C30' H30C 109.7 . . ? C31' C30' H30C 109.7 . . ? C29' C30' H30D 109.7 . . ? C31' C30' H30D 109.7 . . ? H30C C30' H30D 108.2 . . ? C30' C31' H31D 109.5 . . ? C30' C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C30' C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? O5 C32 O6 124.5(4) . . ? O5 C32 C33' 116.5(8) . . ? O6 C32 C33' 119.0(8) . . ? O5 C32 C33 116.3(8) . . ? O6 C32 C33 119.2(8) . . ? C57 O13 C56 119.11(9) . . ? C34 C33 C38 120.0 . . ? C34 C33 C32 121.9(10) . . ? C38 C33 C32 117.9(10) . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 C39 122.3(12) . . ? C34 C35 C39 117.7(12) . . ? C37 C36 C35 120.0 . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38A 120.0 . . ? C33 C38 H38A 120.0 . . ? C40 C39 C35 174.2(13) . . ? C39 C40 C41 171.3(10) . . ? C42 C41 C46 120.0 . . ? C42 C41 C40 121.3(9) . . ? C46 C41 C40 118.7(9) . . ? C43 C42 C41 120.0 . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 C47 119.6(10) . . ? C42 C43 C47 120.4(10) . . ? C43 C44 C45 120.0 . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 C56 116.4(9) . . ? C44 C45 C56 123.6(9) . . ? C45 C46 C41 120.0 . . ? C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? C48 C47 C43 174.6(16) . . ? C47 C48 C49 175.4(11) . . ? C50 C49 C54 120.0 . . ? C50 C49 C48 118.8(9) . . ? C54 C49 C48 121.2(9) . . ? C49 C50 C51 120.0 . . ? C49 C50 H50A 120.0 . . ? C51 C50 H50A 120.0 . . ? C50 C51 C52 120.0 . . ? C50 C51 C55 123(2) . . ? C52 C51 C55 117(2) . . ? C51 C52 C53 120.0 . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 H54A 120.0 . . ? C49 C54 H54A 120.0 . . ? O8 C55 O7 129.1(9) . . ? O8 C55 C51 119(3) . . ? O7 C55 C51 109(3) . . ? O13 C56 C45 109.29(10) . . ? O13 C56 H56A 109.8 . . ? C45 C56 H56A 109.8 . . ? O13 C56 H56B 109.8 . . ? C45 C56 H56B 109.8 . . ? H56A C56 H56B 108.3 . . ? O14 C57 O13 116.60(8) . . ? O14 C57 C58 125.24(9) . . ? O13 C57 C58 118.15(9) . . ? C57 C58 C59 110.24(10) . . ? C57 C58 H58A 109.6 . . ? C59 C58 H58A 109.6 . . ? C57 C58 H58B 109.6 . . ? C59 C58 H58B 109.6 . . ? H58A C58 H58B 108.1 . . ? C58 C59 C60 109.75(11) . . ? C58 C59 H59A 109.7 . . ? C60 C59 H59A 109.7 . . ? C58 C59 H59B 109.7 . . ? C60 C59 H59B 109.7 . . ? H59A C59 H59B 108.2 . . ? C59 C60 C61 109.74(10) . . ? C59 C60 H60A 109.7 . . ? C61 C60 H60A 109.7 . . ? C59 C60 H60B 109.7 . . ? C61 C60 H60B 109.7 . . ? H60A C60 H60B 108.2 . . ? C62 C61 C60 109.75(10) . . ? C62 C61 H61A 109.7 . . ? C60 C61 H61A 109.7 . . ? C62 C61 H61B 109.7 . . ? C60 C61 H61B 109.7 . . ? H61A C61 H61B 108.2 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C57' O13' C56' 119.31(13) . . ? C34' C33' C38' 120.0 . . ? C34' C33' C32 119.0(11) . . ? C38' C33' C32 120.8(11) . . ? C33' C34' C35' 120.0 . . ? C33' C34' H34B 120.0 . . ? C35' C34' H34B 120.0 . . ? C36' C35' C34' 120.0 . . ? C36' C35' C39' 119.8(13) . . ? C34' C35' C39' 120.2(13) . . ? C37' C36' C35' 120.0 . . ? C37' C36' H36B 120.0 . . ? C35' C36' H36B 120.0 . . ? C38' C37' C36' 120.0 . . ? C38' C37' H37B 120.0 . . ? C36' C37' H37B 120.0 . . ? C37' C38' C33' 120.0 . . ? C37' C38' H38B 120.0 . . ? C33' C38' H38B 120.0 . . ? C40' C39' C35' 173.7(13) . . ? C39' C40' C41' 170.2(11) . . ? C42' C41' C46' 120.0 . . ? C42' C41' C40' 117.6(9) . . ? C46' C41' C40' 122.4(9) . . ? C41' C42' C43' 120.0 . . ? C41' C42' H42B 120.0 . . ? C43' C42' H42B 120.0 . . ? C42' C43' C44' 120.0 . . ? C42' C43' C47' 122.5(11) . . ? C44' C43' C47' 117.5(11) . . ? C45' C44' C43' 120.0 . . ? C45' C44' H44B 120.0 . . ? C43' C44' H44B 120.0 . . ? C44' C45' C46' 120.0 . . ? C44' C45' C56' 106.5(19) . . ? C46' C45' C56' 133.5(19) . . ? C45' C46' C41' 120.0 . . ? C45' C46' H46B 120.0 . . ? C41' C46' H46B 120.0 . . ? C48' C47' C43' 172.7(18) . . ? C47' C48' C49' 168.3(13) . . ? C50' C49' C54' 120.0 . . ? C50' C49' C48' 118.8(9) . . ? C54' C49' C48' 121.2(9) . . ? C51' C50' C49' 120.0 . . ? C51' C50' H50B 120.0 . . ? C49' C50' H50B 120.0 . . ? C50' C51' C52' 120.0 . . ? C50' C51' C55' 116(2) . . ? C52' C51' C55' 124(2) . . ? C53' C52' C51' 120.0 . . ? C53' C52' H52B 120.0 . . ? C51' C52' H52B 120.0 . . ? C54' C53' C52' 120.0 . . ? C54' C53' H53B 120.0 . . ? C52' C53' H53B 120.0 . . ? C53' C54' C49' 120.0 . . ? C53' C54' H54B 120.0 . . ? C49' C54' H54B 120.0 . . ? O7 C55' O8 116.6(8) . . ? O7 C55' C51' 123(3) . . ? O8 C55' C51' 115(3) . . ? O13' C56' C45' 112.21(11) . . ? O13' C56' H56C 109.2 . . ? C45' C56' H56C 109.2 . . ? O13' C56' H56D 109.2 . . ? C45' C56' H56D 109.2 . . ? H56C C56' H56D 107.9 . . ? O14' C57' O13' 114.3(14) . . ? O14' C57' C58' 123.44(15) . . ? O13' C57' C58' 122.2(14) . . ? C59' C58' C57' 109.75(10) . . ? C59' C58' H58C 109.7 . . ? C57' C58' H58C 109.7 . . ? C59' C58' H58D 109.7 . . ? C57' C58' H58D 109.7 . . ? H58C C58' H58D 108.2 . . ? C58' C59' C60' 109.75(11) . . ? C58' C59' H59C 109.7 . . ? C60' C59' H59C 109.7 . . ? C58' C59' H59D 109.7 . . ? C60' C59' H59D 109.7 . . ? H59C C59' H59D 108.2 . . ? C59' C60' C61' 109.74(10) . . ? C59' C60' H60C 109.7 . . ? C61' C60' H60C 109.7 . . ? C59' C60' H60D 109.7 . . ? C61' C60' H60D 109.7 . . ? H60C C60' H60D 108.2 . . ? C60' C61' C62' 109.73(10) . . ? C60' C61' H61C 109.7 . . ? C62' C61' H61C 109.7 . . ? C60' C61' H61D 109.7 . . ? C62' C61' H61D 109.7 . . ? H61C C61' H61D 108.2 . . ? C61' C62' H62D 109.5 . . ? C61' C62' H62E 109.5 . . ? H62D C62' H62E 109.5 . . ? C61' C62' H62F 109.5 . . ? H62D C62' H62F 109.5 . . ? H62E C62' H62F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.300 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.096 _publ_section_references ; Bruker (2001). SAINTP+ for NT. Data Reduction and Correction Program v. 6.2, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005). APEX2 software package. Bruker Molecular Analysis Research Tool, v. 2008.4 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SADABS-2008/1, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SHELXTL 2008/4, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.273 0.250 0.023 1742 533 ' ' 2 0.633 -0.250 -0.117 1742 533 ' ' 3 0.000 0.062 0.250 7 1 ' ' 4 0.500 0.437 0.750 7 1 ' ' 5 0.500 0.562 0.250 7 1 ' ' 6 0.000 0.937 0.750 7 1 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT220_MOP3 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE:Hexatyric-ester groups are highly disordered. Full disorder can not be fully resolved due to its complexity. Hence thermal parameters of atoms in these groups have high values. ; _vrf_PLAT222_MOP3 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uso(min) ... 10.00 Rati RESPONSE:Hexatyric-ester groups are highly disordered. Full disorder can not be fully resolved due to its complexity. Hence thermal parameters of atoms in these groups have high values. ; _vrf_PLAT242_MOP3 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C45 RESPONSE:Atoms C45, C45' and C25, C25' are directly connected to the disordered hexatyric-ester groups. ; # end Validation Reply Form # Attachment 'MOP-4_luke12_sq_fs.cif' data_MOP4 _database_code_depnum_ccdc_archive 'CCDC 797905' #TrackingRef 'MOP-4_luke12_sq_fs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C164 H180 Cu4 N3 O28, C5 H11 N O' _chemical_formula_sum 'C169 H191 Cu4 N4 O29' _chemical_formula_weight 2996.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.2237(9) _cell_length_b 28.9086(17) _cell_length_c 36.303(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.6440(10) _cell_angle_gamma 90.00 _cell_volume 15701.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9719 _cell_measurement_theta_min 2.1531 _cell_measurement_theta_max 13.4258 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6324 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9308 _exptl_absorpt_correction_T_max 0.9588 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 200441 _diffrn_reflns_av_R_equivalents 0.1037 _diffrn_reflns_av_sigmaI/netI 0.0939 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 27217 _reflns_number_gt 15871 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0100P)^2^+190.5000P] 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 SHELXL _refine_ls_extinction_coef 0.00042(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 27217 _refine_ls_number_parameters 1510 _refine_ls_number_restraints 155 _refine_ls_R_factor_all 0.1755 _refine_ls_R_factor_gt 0.1167 _refine_ls_wR_factor_ref 0.2461 _refine_ls_wR_factor_gt 0.2248 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _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 Cu1 Cu -0.53813(7) 1.22772(3) 0.36787(3) 0.0346(3) Uani 1 1 d . . . Cu2 Cu -0.56170(7) 1.18712(3) 0.43001(3) 0.0357(3) Uani 1 1 d . . . Cu3 Cu -0.49416(6) 1.32432(3) 0.13220(3) 0.0302(2) Uani 1 1 d . . . Cu4 Cu -0.46720(7) 1.36463(3) 0.07053(3) 0.0320(3) Uani 1 1 d . . . O1 O -0.5556(4) 1.16724(19) 0.34378(14) 0.0368(14) Uani 1 1 d . . . O2 O -0.5782(4) 1.1332(2) 0.39672(15) 0.0407(14) Uani 1 1 d . . . O3 O -0.5088(4) 1.27059(19) 0.09917(15) 0.0375(14) Uani 1 1 d . . . O4 O -0.4966(4) 1.30534(17) 0.04537(14) 0.0354(13) Uani 1 1 d . . . O7 O -0.4122(4) 1.2105(2) 0.38726(16) 0.0411(14) Uani 1 1 d . . . O8 O -0.4343(4) 1.1750(2) 0.44001(16) 0.0450(15) Uani 1 1 d . . . O11 O -0.3648(4) 1.31319(18) 0.14261(14) 0.0348(13) Uani 1 1 d . . . O12 O -0.3441(4) 1.34136(19) 0.08678(15) 0.0391(14) Uani 1 1 d . . . O13 O -0.6852(4) 1.2061(2) 0.41410(16) 0.0437(15) Uani 1 1 d . . . O14 O -0.6673(4) 1.2376(2) 0.35973(15) 0.0417(14) Uani 1 1 d . . . O17 O -0.6199(4) 1.34131(18) 0.11442(14) 0.0348(13) Uani 1 1 d . . . O18 O -0.5945(4) 1.37999(18) 0.06376(14) 0.0345(13) Uani 1 1 d . . . O19 O -0.5363(4) 1.24735(19) 0.45414(15) 0.0433(15) Uani 1 1 d . . . O20 O -0.5215(4) 1.28209(19) 0.39998(16) 0.0424(15) Uani 1 1 d . . . O23 O -0.4762(4) 1.38599(17) 0.15542(15) 0.0331(13) Uani 1 1 d . . . O24 O -0.4424(4) 1.41793(18) 0.10363(16) 0.0380(14) Uani 1 1 d . . . C1 C -0.5678(5) 1.1323(3) 0.3634(2) 0.039(2) Uani 1 1 d . . . C2 C -0.5669(5) 1.0856(3) 0.3454(2) 0.0341(19) Uani 1 1 d . . . C3 C -0.5747(6) 1.0467(3) 0.3671(2) 0.038(2) Uani 1 1 d . . . H3A H -0.5848 1.0497 0.3920 0.046 Uiso 1 1 calc R . . C4 C -0.5676(6) 1.0036(3) 0.3514(3) 0.046(2) Uani 1 1 d . . . H4A H -0.5724 0.9768 0.3661 0.055 Uiso 1 1 calc R . . C5 C -0.5538(6) 0.9983(3) 0.3157(2) 0.040(2) Uani 1 1 d . . . H5A H -0.5486 0.9682 0.3057 0.048 Uiso 1 1 calc R . . C6 C -0.5475(5) 1.0369(3) 0.2938(2) 0.037(2) Uani 1 1 d . . . C7 C -0.5544(5) 1.0812(3) 0.3086(2) 0.0320(18) Uani 1 1 d . . . H7A H -0.5505 1.1078 0.2937 0.038 Uiso 1 1 calc R . . C8 C -0.5358(5) 1.0310(3) 0.2549(2) 0.0328(19) Uani 1 1 d . . . C9 C -0.5285(5) 1.0224(3) 0.2239(2) 0.0349(19) Uani 1 1 d . . . C10 C -0.5202(3) 1.0107(3) 0.1866(2) 0.0333(19) Uani 1 1 d D . . C11 C -0.5150(3) 0.9649(3) 0.1755(2) 0.038(2) Uani 1 1 d D . . H11A H -0.5156 0.9411 0.1936 0.046 Uiso 1 1 calc R . . C12 C -0.5091(2) 0.9526(2) 0.1390(2) 0.048(2) Uani 1 1 d D . . C13 C -0.5085(3) 0.9882(3) 0.1131(2) 0.045(2) Uani 1 1 d D . . H13A H -0.5045 0.9807 0.0880 0.054 Uiso 1 1 calc R . . C14 C -0.5136(4) 1.0346(3) 0.1231(2) 0.037(2) Uani 1 1 d D . . C15 C -0.5193(3) 1.0453(3) 0.1596(2) 0.036(2) Uani 1 1 d D . . H15A H -0.5228 1.0768 0.1666 0.043 Uiso 1 1 calc R . . C16 C -0.5164(6) 1.0706(3) 0.0954(2) 0.039(2) Uani 1 1 d . . . C17 C -0.5168(6) 1.1016(3) 0.0736(2) 0.041(2) Uani 1 1 d . . . C18 C -0.5178(5) 1.1846(3) 0.0665(2) 0.036(2) Uani 1 1 d . . . H18A H -0.5222 1.1872 0.0922 0.044 Uiso 1 1 calc R . . C19 C -0.5158(6) 1.1414(3) 0.0505(2) 0.039(2) Uani 1 1 d . . . C20 C -0.5099(7) 1.1377(3) 0.0120(2) 0.052(3) Uani 1 1 d . . . H20A H -0.5079 1.1082 0.0007 0.062 Uiso 1 1 calc R . . C21 C -0.5071(8) 1.1771(3) -0.0086(3) 0.058(3) Uani 1 1 d . . . H21A H -0.5037 1.1746 -0.0344 0.070 Uiso 1 1 calc R . . C22 C -0.5090(7) 1.2207(3) 0.0074(2) 0.048(2) Uani 1 1 d . . . H22A H -0.5075 1.2476 -0.0076 0.057 Uiso 1 1 calc R . . C23 C -0.5132(6) 1.2250(3) 0.0451(2) 0.037(2) Uani 1 1 d . . . C24 C -0.5057(6) 1.2709(3) 0.0650(2) 0.038(2) Uani 1 1 d . . . C25 C -0.5036(4) 0.9026(2) 0.1276(3) 0.074(4) Uani 1 1 d D . . H25A H -0.4734 0.9002 0.1057 0.089 Uiso 1 1 calc R . . H25B H -0.4688 0.8845 0.1484 0.089 Uiso 1 1 calc R . . C38 C -0.3862(6) 1.1887(3) 0.4181(2) 0.0350(19) Uani 1 1 d . . . C39 C -0.2878(5) 1.1789(3) 0.4275(2) 0.0356(19) Uani 1 1 d . . . C40 C -0.2498(6) 1.1644(3) 0.4640(2) 0.039(2) Uani 1 1 d . . . H40A H -0.2856 1.1614 0.4827 0.047 Uiso 1 1 calc R . . C41 C -0.1599(6) 1.1545(3) 0.4721(2) 0.042(2) Uani 1 1 d . . . H41A H -0.1333 1.1459 0.4969 0.050 Uiso 1 1 calc R . . C42 C -0.1075(6) 1.1568(3) 0.4448(2) 0.041(2) Uani 1 1 d . . . H42A H -0.0457 1.1494 0.4508 0.050 Uiso 1 1 calc R . . C43 C -0.1453(6) 1.1698(3) 0.4088(2) 0.0345(19) Uani 1 1 d . . . C44 C -0.2352(5) 1.1818(3) 0.4004(2) 0.0347(19) Uani 1 1 d . . . H44A H -0.2607 1.1920 0.3759 0.042 Uiso 1 1 calc R . . C45 C -0.0941(6) 1.1705(3) 0.3794(2) 0.037(2) Uani 1 1 d . . . C46 C -0.0536(6) 1.1707(3) 0.3544(2) 0.036(2) Uani 1 1 d . . . C47 C -0.0054(5) 1.1720(3) 0.3238(2) 0.0337(19) Uani 1 1 d . . . C48 C 0.0782(5) 1.1513(3) 0.3270(2) 0.0354(19) Uani 1 1 d . . . H48A H 0.1036 1.1361 0.3497 0.042 Uiso 1 1 calc R . . C49 C 0.1244(5) 1.1523(3) 0.2983(2) 0.038(2) Uani 1 1 d . . . C50 C 0.0881(6) 1.1748(3) 0.2647(2) 0.042(2) Uani 1 1 d . . . H50A H 0.1203 1.1761 0.2447 0.051 Uiso 1 1 calc R . . C51 C 0.0028(5) 1.1957(3) 0.2612(2) 0.0346(19) Uani 1 1 d . . . C52 C -0.0428(5) 1.1943(3) 0.2902(2) 0.0328(19) Uani 1 1 d . . . H52A H -0.1000 1.2083 0.2876 0.039 Uiso 1 1 calc R . . C53 C -0.0348(6) 1.2193(3) 0.2272(2) 0.036(2) Uani 1 1 d . . . C54 C -0.0683(6) 1.2392(3) 0.1990(2) 0.0354(19) Uani 1 1 d . . . C55 C -0.1910(6) 1.2798(3) 0.1583(2) 0.035(2) Uani 1 1 d . . . H55A H -0.2277 1.2751 0.1765 0.042 Uiso 1 1 calc R . . C56 C -0.1034(5) 1.2639(2) 0.1652(2) 0.0296(18) Uani 1 1 d . . . C57 C -0.0496(6) 1.2692(3) 0.1382(2) 0.0354(19) Uani 1 1 d . . . H57A H 0.0096 1.2572 0.1425 0.043 Uiso 1 1 calc R . . C58 C -0.0835(6) 1.2921(3) 0.1050(2) 0.036(2) Uani 1 1 d . . . H58A H -0.0473 1.2962 0.0866 0.043 Uiso 1 1 calc R . . C59 C -0.1700(6) 1.3089(3) 0.0987(2) 0.036(2) Uani 1 1 d . . . H59A H -0.1919 1.3251 0.0762 0.043 Uiso 1 1 calc R . . C60 C -0.2254(5) 1.3027(2) 0.1246(2) 0.0313(18) Uani 1 1 d . . . C61 C -0.3188(6) 1.3200(3) 0.1178(2) 0.0331(19) Uani 1 1 d . . . C62 C 0.2155(6) 1.1295(3) 0.3025(3) 0.051(2) Uani 1 1 d . . . H62A H 0.2609 1.1526 0.2988 0.061 Uiso 1 1 calc R . . H62B H 0.2328 1.1165 0.3281 0.061 Uiso 1 1 calc R . . C75 C -0.7125(6) 1.2275(3) 0.3846(2) 0.0345(19) Uani 1 1 d . . . C76 C -0.8081(6) 1.2447(3) 0.3783(2) 0.0354(19) Uani 1 1 d . . . C77 C -0.8562(6) 1.2402(3) 0.4067(2) 0.038(2) Uani 1 1 d . . . H77A H -0.8304 1.2249 0.4293 0.046 Uiso 1 1 calc R . . C78 C -0.9422(6) 1.2577(3) 0.4024(2) 0.039(2) Uani 1 1 d . . . H78A H -0.9750 1.2550 0.4222 0.047 Uiso 1 1 calc R . . C79 C -0.9801(6) 1.2790(3) 0.3695(2) 0.036(2) Uani 1 1 d . . . H79A H -1.0397 1.2903 0.3662 0.043 Uiso 1 1 calc R . . C80 C -0.9306(6) 1.2842(3) 0.3408(2) 0.035(2) Uani 1 1 d . . . C81 C -0.8454(5) 1.2664(3) 0.3452(2) 0.0325(19) Uani 1 1 d . . . H81A H -0.8123 1.2690 0.3255 0.039 Uiso 1 1 calc R . . C82 C -0.9696(6) 1.3066(3) 0.3065(2) 0.0351(19) Uani 1 1 d . . . C83 C -1.0005(5) 1.3256(3) 0.2775(2) 0.0356(19) Uani 1 1 d . . . C84 C -1.0362(6) 1.3487(3) 0.2431(2) 0.039(2) Uani 1 1 d . . . C85 C -1.1240(6) 1.3649(3) 0.2375(2) 0.044(2) Uani 1 1 d . . . H85A H -1.1584 1.3617 0.2567 0.052 Uiso 1 1 calc R . . C86 C -1.1608(6) 1.3862(3) 0.2034(3) 0.047(2) Uani 1 1 d . . . C87 C -1.1122(6) 1.3905(3) 0.1761(2) 0.043(2) Uani 1 1 d . . . H87A H -1.1381 1.4050 0.1532 0.052 Uiso 1 1 calc R . . C88 C -1.0237(6) 1.3738(3) 0.1808(2) 0.036(2) Uani 1 1 d . . . C89 C -0.9871(5) 1.3527(3) 0.2150(2) 0.0348(19) Uani 1 1 d . . . H89A H -0.9277 1.3411 0.2188 0.042 Uiso 1 1 calc R . . C90 C -0.9734(6) 1.3790(3) 0.1520(3) 0.039(2) Uani 1 1 d . . . C91 C -0.9317(6) 1.3837(3) 0.1271(2) 0.037(2) Uani 1 1 d . . . C92 C -0.7914(5) 1.3728(3) 0.1040(2) 0.036(2) Uani 1 1 d . . . H92A H -0.7687 1.3544 0.1253 0.043 Uiso 1 1 calc R . . C93 C -0.8802(5) 1.3905(3) 0.0990(2) 0.0343(19) Uani 1 1 d . . . C94 C -0.9098(6) 1.4172(3) 0.0676(2) 0.046(2) Uani 1 1 d . . . H94A H -0.9686 1.4297 0.0638 0.055 Uiso 1 1 calc R . . C95 C -0.8565(6) 1.4262(3) 0.0418(2) 0.049(2) Uani 1 1 d . . . H95A H -0.8792 1.4444 0.0204 0.059 Uiso 1 1 calc R . . C96 C -0.7712(6) 1.4094(3) 0.0466(2) 0.040(2) Uani 1 1 d . . . H96A H -0.7345 1.4160 0.0288 0.049 Uiso 1 1 calc R . . C97 C -0.7389(5) 1.3825(2) 0.0781(2) 0.0277(17) Uani 1 1 d . . . C98 C -0.6423(5) 1.3666(3) 0.0858(2) 0.0302(18) Uani 1 1 d . . . C99 C -1.2556(6) 1.4031(4) 0.1977(3) 0.060(3) Uani 1 1 d . . . H99A H -1.2720 1.4178 0.1727 0.072 Uiso 1 1 calc R . . H99B H -1.2966 1.3768 0.1989 0.072 Uiso 1 1 calc R . . C112 C -0.5248(6) 1.2829(3) 0.4347(2) 0.039(2) Uani 1 1 d . . . C113 C -0.5118(6) 1.3287(3) 0.4540(2) 0.042(2) Uani 1 1 d . . . C114 C -0.5104(8) 1.3320(3) 0.4918(3) 0.063(3) Uani 1 1 d . . . H11B H -0.5172 1.3050 0.5060 0.076 Uiso 1 1 calc R . . C115 C -0.4993(9) 1.3744(4) 0.5091(3) 0.076(4) Uani 1 1 d . . . H11C H -0.4972 1.3767 0.5354 0.091 Uiso 1 1 calc R . . C116 C -0.4911(9) 1.4142(4) 0.4883(3) 0.074(4) Uani 1 1 d . . . H11D H -0.4852 1.4437 0.5002 0.089 Uiso 1 1 calc R . . C117 C -0.4914(7) 1.4107(3) 0.4500(3) 0.055(3) Uani 1 1 d . . . C118 C -0.5014(6) 1.3676(3) 0.4332(2) 0.042(2) Uani 1 1 d . . . H11E H -0.5011 1.3648 0.4072 0.050 Uiso 1 1 calc R . . C119 C -0.4866(7) 1.4504(3) 0.4272(3) 0.052(2) Uani 1 1 d . . . C120 C -0.4837(6) 1.4811(3) 0.4057(3) 0.051(3) Uani 1 1 d . . . C121 C -0.4836(3) 1.5190(3) 0.3790(3) 0.045(2) Uani 1 1 d D . . C122 C -0.4873(3) 1.5645(3) 0.3897(3) 0.045(2) Uani 1 1 d D . . H12A H -0.4900 1.5720 0.4149 0.054 Uiso 1 1 calc R . . C123 C -0.4870(2) 1.5995(2) 0.3636(3) 0.049(2) Uani 1 1 d D D . C124 C -0.4829(3) 1.5884(3) 0.3265(3) 0.048(2) Uani 1 1 d D . . H12B H -0.4827 1.6125 0.3087 0.058 Uiso 1 1 calc R . . C125 C -0.4792(4) 1.5427(3) 0.3154(3) 0.043(2) Uani 1 1 d D . . C126 C -0.4795(3) 1.5077(3) 0.3415(3) 0.046(2) Uani 1 1 d D . . H12C H -0.4769 1.4763 0.3341 0.055 Uiso 1 1 calc R . . C127 C -0.4719(5) 1.5314(3) 0.2778(3) 0.042(2) Uani 1 1 d . . . C128 C -0.4647(6) 1.5228(3) 0.2461(3) 0.043(2) Uani 1 1 d . . . C129 C -0.4611(5) 1.4724(3) 0.1918(2) 0.034(2) Uani 1 1 d . . . H12D H -0.4733 1.4461 0.2057 0.041 Uiso 1 1 calc R . . C130 C -0.4553(5) 1.5153(3) 0.2084(2) 0.038(2) Uani 1 1 d . . . C131 C -0.4392(6) 1.5537(3) 0.1868(3) 0.049(2) Uani 1 1 d . . . H13B H -0.4361 1.5836 0.1977 0.059 Uiso 1 1 calc R . . C132 C -0.4278(6) 1.5488(3) 0.1501(3) 0.049(2) Uani 1 1 d . . . H13C H -0.4170 1.5751 0.1359 0.059 Uiso 1 1 calc R . . C133 C -0.4323(6) 1.5049(3) 0.1340(3) 0.042(2) Uani 1 1 d . . . H13D H -0.4238 1.5012 0.1089 0.051 Uiso 1 1 calc R . . C134 C -0.4493(5) 1.4666(3) 0.1547(2) 0.0340(19) Uani 1 1 d . . . C135 C -0.4573(5) 1.4200(2) 0.1365(2) 0.0306(18) Uani 1 1 d . . . C136 C -0.4910(3) 1.64949(18) 0.3751(3) 0.063(3) Uani 1 1 d D . . H13E H -0.4522 1.6543 0.3999 0.076 Uiso 1 1 calc R A 1 H13F H -0.4691 1.6696 0.3567 0.076 Uiso 1 1 calc R A 1 O5 O -0.6025(5) 0.9023(3) 0.05929(18) 0.1100(15) Uani 1 1 d D . . O6 O -0.5933(4) 0.8846(3) 0.11803(17) 0.1100(15) Uani 1 1 d D . . C26 C -0.6406(3) 0.88663(18) 0.08282(16) 0.1100(15) Uani 1 1 d D C . C27 C -0.7349(4) 0.8695(3) 0.0758(2) 0.1100(15) Uani 1 1 d D . . H27A H -0.7386 0.8400 0.0618 0.132 Uiso 0.65 1 calc PR B 1 H27B H -0.7740 0.8923 0.0604 0.132 Uiso 0.65 1 calc PR B 1 H27C H -0.7402 0.8441 0.0923 0.132 Uiso 0.35 1 d PR B 2 H27D H -0.7515 0.8587 0.0505 0.132 Uiso 0.35 1 d PR B 2 C28 C -0.7667(5) 0.8622(3) 0.1124(3) 0.1100(15) Uani 0.65 1 d PD C 1 H28A H -0.8230 0.8442 0.1079 0.132 Uiso 0.65 1 calc PR C 1 H28B H -0.7214 0.8445 0.1299 0.132 Uiso 0.65 1 calc PR C 1 C29 C -0.7822(10) 0.9084(4) 0.1296(3) 0.1100(15) Uani 0.65 1 d PD C 1 H29A H -0.8083 0.9304 0.1096 0.132 Uiso 0.65 1 calc PR C 1 H29B H -0.7245 0.9212 0.1426 0.132 Uiso 0.65 1 calc PR C 1 C30 C -0.8448(8) 0.9026(5) 0.1570(3) 0.1100(15) Uani 0.65 1 d PD C 1 H30A H -0.8560 0.9330 0.1678 0.132 Uiso 0.65 1 calc PR C 1 H30B H -0.9027 0.8901 0.1438 0.132 Uiso 0.65 1 calc PR C 1 C31 C -0.8042(11) 0.8699(4) 0.1879(3) 0.1100(15) Uani 0.65 1 d PD C 1 H31A H -0.7843 0.8413 0.1770 0.132 Uiso 0.65 1 calc PR C 1 H31B H -0.8496 0.8615 0.2031 0.132 Uiso 0.65 1 calc PR C 1 C32 C -0.7256(8) 0.8928(5) 0.2126(3) 0.1100(15) Uani 0.65 1 d PD C 1 H32A H -0.6966 0.8707 0.2319 0.132 Uiso 0.65 1 calc PR C 1 H32B H -0.6811 0.9022 0.1973 0.132 Uiso 0.65 1 calc PR C 1 C33 C -0.7567(12) 0.9348(4) 0.2314(2) 0.1100(15) Uani 0.65 1 d PD C 1 H33A H -0.8146 0.9456 0.2168 0.132 Uiso 0.65 1 calc PR C 1 H33B H -0.7127 0.9601 0.2320 0.132 Uiso 0.65 1 calc PR C 1 C34 C -0.7673(18) 0.9227(3) 0.2708(4) 0.1100(15) Uani 0.65 1 d PD C 1 H34A H -0.7108 0.9095 0.2847 0.132 Uiso 0.65 1 calc PR C 1 H34B H -0.8150 0.8993 0.2700 0.132 Uiso 0.65 1 calc PR C 1 C35 C -0.7910(16) 0.9657(4) 0.2906(3) 0.1100(15) Uani 0.65 1 d PD C 1 H35A H -0.7440 0.9894 0.2908 0.132 Uiso 0.65 1 calc PR C 1 H35B H -0.8482 0.9785 0.2770 0.132 Uiso 0.65 1 calc PR C 1 C36 C -0.7993(17) 0.9538(4) 0.3303(3) 0.1100(15) Uani 0.65 1 d PD C 1 H36A H -0.7449 0.9374 0.3428 0.132 Uiso 0.65 1 calc PR C 1 H36B H -0.8513 0.9332 0.3301 0.132 Uiso 0.65 1 calc PR C 1 C37 C -0.8114(19) 0.9976(5) 0.3515(4) 0.1100(15) Uani 0.65 1 d PD C 1 H37A H -0.8118 0.9900 0.3778 0.165 Uiso 0.65 1 calc PR C 1 H37B H -0.8683 1.0122 0.3404 0.165 Uiso 0.65 1 calc PR C 1 H37C H -0.7621 1.0189 0.3501 0.165 Uiso 0.65 1 calc PR C 1 C28' C -0.7976(4) 0.9072(5) 0.0837(4) 0.1100(15) Uani 0.35 1 d PD C 2 H28C H -0.7693 0.9378 0.0822 0.132 Uiso 0.35 1 calc PR C 2 H28D H -0.8533 0.9062 0.0647 0.132 Uiso 0.35 1 calc PR C 2 C29' C -0.8195(14) 0.9005(6) 0.1223(6) 0.1100(15) Uani 0.35 1 d PD C 2 H29C H -0.7939 0.8708 0.1330 0.132 Uiso 0.35 1 calc PR C 2 H29D H -0.8851 0.8992 0.1205 0.132 Uiso 0.35 1 calc PR C 2 C30' C -0.781(2) 0.9400(7) 0.1474(4) 0.1100(15) Uani 0.35 1 d PD C 2 H30C H -0.7160 0.9421 0.1482 0.132 Uiso 0.35 1 calc PR C 2 H30D H -0.8090 0.9694 0.1374 0.132 Uiso 0.35 1 calc PR C 2 C31' C -0.7991(18) 0.9320(8) 0.1865(4) 0.1100(15) Uani 0.35 1 d PD C 2 H31C H -0.8639 0.9273 0.1855 0.132 Uiso 0.35 1 calc PR C 2 H31D H -0.7803 0.9595 0.2023 0.132 Uiso 0.35 1 calc PR C 2 C32' C -0.748(2) 0.8900(8) 0.2035(5) 0.1100(15) Uani 0.35 1 d PD C 2 H32C H -0.6854 0.8919 0.1999 0.132 Uiso 0.35 1 calc PR C 2 H32D H -0.7752 0.8617 0.1908 0.132 Uiso 0.35 1 calc PR C 2 C33' C -0.751(2) 0.8876(6) 0.2448(5) 0.1100(15) Uani 0.35 1 d PD C 2 H33C H -0.7955 0.8642 0.2492 0.132 Uiso 0.35 1 calc PR C 2 H33D H -0.6918 0.8781 0.2589 0.132 Uiso 0.35 1 calc PR C 2 C34' C -0.776(3) 0.9343(6) 0.2584(5) 0.1100(15) Uani 0.35 1 d PD C 2 H34C H -0.7286 0.9570 0.2562 0.132 Uiso 0.35 1 calc PR C 2 H34D H -0.8324 0.9450 0.2428 0.132 Uiso 0.35 1 calc PR C 2 C35' C -0.787(3) 0.9308(6) 0.2988(6) 0.1100(15) Uani 0.35 1 d PD C 2 H35C H -0.7340 0.9153 0.3138 0.132 Uiso 0.35 1 calc PR C 2 H35D H -0.8403 0.9121 0.3006 0.132 Uiso 0.35 1 calc PR C 2 C36' C -0.797(3) 0.9786(7) 0.3143(6) 0.1100(15) Uani 0.35 1 d PD C 2 H36C H -0.8540 0.9924 0.3018 0.132 Uiso 0.35 1 calc PR C 2 H36D H -0.7474 0.9987 0.3094 0.132 Uiso 0.35 1 calc PR C 2 C37' C -0.795(4) 0.9757(10) 0.3560(6) 0.1100(15) Uani 0.35 1 d PD C 2 H37D H -0.7335 0.9805 0.3695 0.165 Uiso 0.35 1 calc PR C 2 H37E H -0.8157 0.9451 0.3622 0.165 Uiso 0.35 1 calc PR C 2 H37F H -0.8339 0.9996 0.3634 0.165 Uiso 0.35 1 calc PR C 2 O9 O 0.2114(4) 1.0926(2) 0.2747(2) 0.0558(18) Uani 1 1 d . . . O10 O 0.2756(5) 1.1403(3) 0.2390(2) 0.070(2) Uani 1 1 d . . . C63 C 0.2420(6) 1.1028(4) 0.2434(3) 0.059(3) Uani 1 1 d . . . C64 C 0.2330(10) 1.0626(4) 0.21294(18) 0.1052(15) Uani 1 1 d D . . H64A H 0.2782 1.0384 0.2215 0.126 Uiso 1 1 calc R . . H64B H 0.1731 1.0482 0.2104 0.126 Uiso 1 1 calc R . . C65 C 0.2458(10) 1.0807(3) 0.17529(18) 0.1052(15) Uani 1 1 d D . . H65A H 0.3064 1.0941 0.1775 0.126 Uiso 1 1 calc R . . H65B H 0.2016 1.1054 0.1668 0.126 Uiso 1 1 calc R . . C66 C 0.2341(10) 1.0419(2) 0.14700(17) 0.1052(15) Uani 1 1 d D . . H66A H 0.1754 1.0268 0.1463 0.126 Uiso 1 1 calc R . . H66B H 0.2814 1.0184 0.1544 0.126 Uiso 1 1 calc R . . C67 C 0.2392(10) 1.0608(2) 0.10867(17) 0.1052(15) Uani 1 1 d D . . H67A H 0.1900 1.0831 0.1008 0.126 Uiso 1 1 calc R . . H67B H 0.2966 1.0773 0.1096 0.126 Uiso 1 1 calc R . . C68 C 0.2322(10) 1.0217(2) 0.08073(17) 0.1052(15) Uani 1 1 d D . . H68A H 0.1735 1.0062 0.0788 0.126 Uiso 1 1 calc R . . H68B H 0.2795 0.9986 0.0893 0.126 Uiso 1 1 calc R . . C69 C 0.2421(10) 1.0403(2) 0.04283(18) 0.1052(15) Uani 1 1 d D . . H69A H 0.1953 1.0637 0.0344 0.126 Uiso 1 1 calc R . . H69B H 0.3012 1.0553 0.0447 0.126 Uiso 1 1 calc R . . C70 C 0.2336(9) 1.0012(3) 0.01479(19) 0.1052(15) Uani 1 1 d D . . H70A H 0.2756 0.9761 0.0246 0.126 Uiso 1 1 calc R . . H70B H 0.1721 0.9885 0.0108 0.126 Uiso 1 1 calc R . . C71 C 0.2541(10) 1.0186(2) -0.02190(19) 0.1052(15) Uani 1 1 d D . . H71A H 0.3139 1.0334 -0.0176 0.126 Uiso 1 1 calc R . . H71B H 0.2094 1.0421 -0.0327 0.126 Uiso 1 1 calc R . . C72 C 0.2522(9) 0.9788(3) -0.04898(18) 0.1052(15) Uani 1 1 d D . . H72A H 0.2974 0.9555 -0.0383 0.126 Uiso 1 1 calc R . . H72B H 0.1927 0.9639 -0.0531 0.126 Uiso 1 1 calc R . . C73 C 0.2718(7) 0.9963(3) -0.08582(18) 0.1052(15) Uani 1 1 d D . . H73A H 0.2670 0.9705 -0.1040 0.126 Uiso 1 1 calc R . . H73B H 0.3334 1.0086 -0.0821 0.126 Uiso 1 1 calc R . . C74 C 0.2061(8) 1.0339(4) -0.1010(3) 0.1052(15) Uani 1 1 d D . . H74A H 0.1585 1.0209 -0.1200 0.158 Uiso 1 1 calc R . . H74B H 0.2372 1.0584 -0.1122 0.158 Uiso 1 1 calc R . . H74C H 0.1801 1.0469 -0.0805 0.158 Uiso 1 1 calc R . . O15 O -1.2637(6) 1.4360(4) 0.2263(3) 0.087(3) Uani 1 1 d . . . O16 O -1.2080(6) 1.4875(3) 0.1902(3) 0.090(3) Uani 1 1 d . . . C100 C -1.2335(8) 1.4754(6) 0.2194(4) 0.082(4) Uani 1 1 d . . . C101 C -1.2280(9) 1.5083(3) 0.2499(3) 0.1017(14) Uani 1 1 d D . . H10A H -1.2348 1.4972 0.2738 0.122 Uiso 1 1 calc R . . C102 C -1.2122(10) 1.5594(3) 0.2455(2) 0.1017(14) Uani 1 1 d D . . H10B H -1.1552 1.5642 0.2366 0.122 Uiso 1 1 calc R . . H10C H -1.2611 1.5727 0.2266 0.122 Uiso 1 1 calc R . . C103 C -1.2086(10) 1.5835(3) 0.28263(17) 0.1017(14) Uani 1 1 d D . . H10D H -1.2621 1.5754 0.2931 0.122 Uiso 1 1 calc R . . H10E H -1.1551 1.5732 0.3005 0.122 Uiso 1 1 calc R . . C104 C -1.2048(6) 1.6352(2) 0.27732(16) 0.1017(14) Uani 1 1 d D . . H10F H -1.2657 1.6473 0.2679 0.122 Uiso 1 1 calc R . . H10G H -1.1672 1.6425 0.2585 0.122 Uiso 1 1 calc R . . C105 C -1.1662(6) 1.6581(3) 0.3141(2) 0.1017(14) Uani 1 1 d D . . H10H H -1.1118 1.6414 0.3263 0.122 Uiso 1 1 calc R . . H10I H -1.1493 1.6904 0.3096 0.122 Uiso 1 1 calc R . . C106 C -1.2343(5) 1.6578(5) 0.3395(2) 0.1017(14) Uani 1 1 d D . . H10J H -1.2540 1.6256 0.3428 0.122 Uiso 1 1 calc R . . H10K H -1.2873 1.6761 0.3281 0.122 Uiso 1 1 calc R . . C107 C -1.1938(5) 1.6781(5) 0.3772(2) 0.1017(14) Uani 1 1 d D . . H10L H -1.1415 1.6594 0.3889 0.122 Uiso 1 1 calc R . . H10M H -1.1732 1.7100 0.3738 0.122 Uiso 1 1 calc R . . C108 C -1.2624(6) 1.6785(5) 0.4024(2) 0.1017(14) Uani 1 1 d D . . H10N H -1.2813 1.6465 0.4065 0.122 Uiso 1 1 calc R . . H10O H -1.3158 1.6961 0.3902 0.122 Uiso 1 1 calc R . . C109 C -1.2231(7) 1.7006(5) 0.4395(2) 0.1017(14) Uani 1 1 d D . . H10P H -1.1698 1.6828 0.4514 0.122 Uiso 1 1 calc R . . H10Q H -1.2036 1.7324 0.4350 0.122 Uiso 1 1 calc R . . C110 C -1.2877(8) 1.7021(5) 0.4650(2) 0.1017(14) Uani 1 1 d D . . H11F H -1.2975 1.6703 0.4736 0.122 Uiso 1 1 calc R . . H11G H -1.3455 1.7139 0.4513 0.122 Uiso 1 1 calc R . . C111 C -1.2557(8) 1.7325(5) 0.4986(2) 0.1017(14) Uani 1 1 d D . . H11H H -1.3002 1.7325 0.5150 0.153 Uiso 1 1 calc R . . H11I H -1.2473 1.7641 0.4902 0.153 Uiso 1 1 calc R . . H11J H -1.1988 1.7206 0.5125 0.153 Uiso 1 1 calc R . . O21 O -0.5819(3) 1.6615(2) 0.3771(3) 0.143(3) Uani 0.50 1 d PD D 1 O22 O -0.5334(6) 1.7122(6) 0.4203(5) 0.143(3) Uani 0.50 1 d PD D 1 C137 C -0.5979(5) 1.6947(3) 0.4011(3) 0.143(3) Uani 0.50 1 d PD D 1 C138 C -0.6930(5) 1.7070(7) 0.4020(6) 0.143(3) Uani 0.50 1 d PD D 1 H13G H -0.7227 1.6806 0.4120 0.172 Uiso 0.50 1 calc PR D 1 H13H H -0.7252 1.7133 0.3762 0.172 Uiso 0.50 1 calc PR D 1 C139 C -0.6971(9) 1.7491(4) 0.4263(4) 0.143(3) Uani 0.50 1 d PD D 1 H13I H -0.6360 1.7580 0.4386 0.172 Uiso 0.50 1 calc PR D 1 H13J H -0.7238 1.7753 0.4105 0.172 Uiso 0.50 1 calc PR D 1 C140 C -0.7529(9) 1.7385(8) 0.4556(4) 0.143(3) Uani 0.50 1 d PD D 1 H14A H -0.8123 1.7269 0.4433 0.172 Uiso 0.50 1 calc PR D 1 H14B H -0.7617 1.7671 0.4694 0.172 Uiso 0.50 1 calc PR D 1 C141 C -0.7065(16) 1.7026(7) 0.4825(6) 0.143(3) Uani 0.50 1 d PD D 1 H14C H -0.6410 1.7049 0.4841 0.172 Uiso 0.50 1 calc PR D 1 H14D H -0.7257 1.6713 0.4733 0.172 Uiso 0.50 1 calc PR D 1 C142 C -0.729(2) 1.7100(5) 0.5208(4) 0.143(3) Uani 0.50 1 d PD D 1 H14E H -0.6828 1.7293 0.5362 0.172 Uiso 0.50 1 calc PR D 1 H14F H -0.7872 1.7265 0.5183 0.172 Uiso 0.50 1 calc PR D 1 C143 C -0.736(2) 1.6639(4) 0.5398(5) 0.143(3) Uani 0.50 1 d PD D 1 H14G H -0.7812 1.6444 0.5241 0.172 Uiso 0.50 1 calc PR D 1 H14H H -0.6773 1.6478 0.5428 0.172 Uiso 0.50 1 calc PR D 1 C144 C -0.7606(18) 1.6713(6) 0.5777(6) 0.143(3) Uani 0.50 1 d PD D 1 H14I H -0.8258 1.6763 0.5747 0.172 Uiso 0.50 1 calc PR D 1 H14J H -0.7299 1.6992 0.5897 0.172 Uiso 0.50 1 calc PR D 1 C145 C -0.7337(17) 1.6296(6) 0.6022(6) 0.143(3) Uani 0.50 1 d PD D 1 H14K H -0.7612 1.6014 0.5895 0.172 Uiso 0.50 1 calc PR D 1 H14L H -0.6679 1.6258 0.6065 0.172 Uiso 0.50 1 calc PR D 1 C146 C -0.7640(19) 1.6356(5) 0.6392(5) 0.143(3) Uani 0.50 1 d PD D 1 H14M H -0.7197 1.6544 0.6563 0.172 Uiso 0.50 1 calc PR D 1 H14N H -0.8219 1.6522 0.6353 0.172 Uiso 0.50 1 calc PR D 1 C147 C -0.7740(15) 1.5889(6) 0.6566(7) 0.143(3) Uani 0.50 1 d PD D 1 H14O H -0.7723 1.5924 0.6838 0.172 Uiso 0.50 1 calc PR D 1 H14P H -0.8323 1.5752 0.6452 0.172 Uiso 0.50 1 calc PR D 1 C148 C -0.6993(18) 1.5574(7) 0.6501(11) 0.143(3) Uani 0.50 1 d PD . 1 H14Q H -0.7246 1.5290 0.6376 0.215 Uiso 0.50 1 calc PR . 1 H14R H -0.6616 1.5495 0.6742 0.215 Uiso 0.50 1 calc PR . 1 H14S H -0.6631 1.5731 0.6342 0.215 Uiso 0.50 1 calc PR . 1 O221 O -0.5729(5) 1.6577(3) 0.3886(3) 0.143(3) Uani 0.50 1 d PD D 2 O222 O -0.6283(8) 1.6916(6) 0.3361(4) 0.143(3) Uani 0.50 1 d PD D 2 C237 C -0.6411(4) 1.6795(3) 0.3664(4) 0.143(3) Uani 0.50 1 d PD D 2 C238 C -0.7257(5) 1.6870(4) 0.3810(7) 0.143(3) Uani 0.50 1 d PD D 2 H23A H -0.7261 1.6667 0.4030 0.172 Uiso 0.50 1 calc PR D 2 H23B H -0.7775 1.6786 0.3614 0.172 Uiso 0.50 1 calc PR D 2 C239 C -0.7336(11) 1.7369(4) 0.3923(7) 0.143(3) Uani 0.50 1 d PD D 2 H23C H -0.7335 1.7572 0.3703 0.172 Uiso 0.50 1 calc PR D 2 H23D H -0.6819 1.7453 0.4119 0.172 Uiso 0.50 1 calc PR D 2 C240 C -0.8193(11) 1.7437(6) 0.4070(5) 0.143(3) Uani 0.50 1 d PD D 2 H24A H -0.8704 1.7455 0.3857 0.172 Uiso 0.50 1 calc PR D 2 H24B H -0.8165 1.7730 0.4212 0.172 Uiso 0.50 1 calc PR D 2 C241 C -0.8327(11) 1.7037(7) 0.4322(6) 0.143(3) Uani 0.50 1 d PD D 2 H24C H -0.8756 1.7127 0.4484 0.172 Uiso 0.50 1 calc PR D 2 H24D H -0.8578 1.6769 0.4168 0.172 Uiso 0.50 1 calc PR D 2 C242 C -0.7444(13) 1.6905(7) 0.4562(4) 0.143(3) Uani 0.50 1 d PD D 2 H24E H -0.7402 1.6565 0.4586 0.172 Uiso 0.50 1 calc PR D 2 H24F H -0.6947 1.7014 0.4442 0.172 Uiso 0.50 1 calc PR D 2 C243 C -0.7367(18) 1.7121(6) 0.4945(5) 0.143(3) Uani 0.50 1 d PD D 2 H24G H -0.6774 1.7269 0.5019 0.172 Uiso 0.50 1 calc PR D 2 H24H H -0.7830 1.7363 0.4939 0.172 Uiso 0.50 1 calc PR D 2 C244 C -0.749(2) 1.6754(5) 0.5228(4) 0.143(3) Uani 0.50 1 d PD D 2 H24I H -0.8000 1.6554 0.5125 0.172 Uiso 0.50 1 calc PR D 2 H24J H -0.6944 1.6557 0.5281 0.172 Uiso 0.50 1 calc PR D 2 C245 C -0.7642(16) 1.6979(6) 0.5585(5) 0.143(3) Uani 0.50 1 d PD D 2 H24K H -0.7426 1.7303 0.5596 0.172 Uiso 0.50 1 calc PR D 2 H24L H -0.8290 1.6984 0.5591 0.172 Uiso 0.50 1 calc PR D 2 C246 C -0.7152(15) 1.6714(7) 0.5920(4) 0.143(3) Uani 0.50 1 d PD D 2 H24M H -0.7097 1.6908 0.6148 0.172 Uiso 0.50 1 calc PR D 2 H24N H -0.6543 1.6636 0.5880 0.172 Uiso 0.50 1 calc PR D 2 C247 C -0.7656(17) 1.6276(8) 0.5971(8) 0.143(3) Uani 0.50 1 d PD D 2 H24O H -0.7662 1.6070 0.5753 0.172 Uiso 0.50 1 calc PR D 2 H24P H -0.8282 1.6352 0.5986 0.172 Uiso 0.50 1 calc PR D 2 C248 C -0.721(2) 1.6033(8) 0.6325(7) 0.143(3) Uani 0.50 1 d PD D 2 H24Q H -0.7657 1.5847 0.6423 0.215 Uiso 0.50 1 calc PR D 2 H24R H -0.6958 1.6264 0.6513 0.215 Uiso 0.50 1 calc PR D 2 H24S H -0.6737 1.5831 0.6270 0.215 Uiso 0.50 1 calc PR D 2 O25 O -0.5090(5) 1.2665(3) 0.3209(2) 0.0718(11) Uani 1 1 d . . . N1 N -0.4036(6) 1.2996(3) 0.2908(3) 0.0718(11) Uani 1 1 d . . . C149 C -0.4286(8) 1.2711(4) 0.3161(3) 0.0718(11) Uani 1 1 d . . . H14T H -0.3837 1.2533 0.3313 0.086 Uiso 1 1 calc R . . C150 C -0.3106(8) 1.2996(4) 0.2849(3) 0.0718(11) Uani 1 1 d . . . H15B H -0.2714 1.2867 0.3074 0.086 Uiso 1 1 calc R . . H15C H -0.2915 1.3319 0.2817 0.086 Uiso 1 1 calc R . . C151 C -0.2992(8) 1.2716(4) 0.2509(3) 0.0718(11) Uani 1 1 d . . . H15D H -0.2367 1.2729 0.2478 0.108 Uiso 1 1 calc R . . H15E H -0.3377 1.2843 0.2286 0.108 Uiso 1 1 calc R . . H15F H -0.3160 1.2394 0.2544 0.108 Uiso 1 1 calc R . . C152 C -0.4668(8) 1.3298(4) 0.2674(3) 0.0718(11) Uani 1 1 d . . . H15G H -0.5283 1.3183 0.2668 0.086 Uiso 1 1 calc R . . H15H H -0.4552 1.3293 0.2414 0.086 Uiso 1 1 calc R . . C153 C -0.4594(8) 1.3798(4) 0.2821(3) 0.0718(11) Uani 1 1 d . . . H15I H -0.5027 1.3993 0.2658 0.108 Uiso 1 1 calc R . . H15J H -0.3988 1.3914 0.2823 0.108 Uiso 1 1 calc R . . H15K H -0.4718 1.3804 0.3077 0.108 Uiso 1 1 calc R . . O26 O -0.5856(4) 1.1498(2) 0.47886(15) 0.0424(14) Uani 1 1 d . . . H26A H -0.6172 1.1253 0.4767 0.051 Uiso 1 1 d R . . C164 C -0.5482(9) 1.1679(4) 0.5140(3) 0.076(4) Uani 1 1 d . . . H16K H -0.5643 1.1482 0.5337 0.114 Uiso 1 1 calc R . . H16L H -0.5710 1.1992 0.5164 0.114 Uiso 1 1 calc R . . H16M H -0.4830 1.1689 0.5166 0.114 Uiso 1 1 calc R . . O27 O -0.5237(5) 1.2871(2) 0.17978(19) 0.0582(9) Uani 1 1 d . . . N2 N -0.6290(6) 1.2546(3) 0.2083(2) 0.0582(9) Uani 1 1 d . . . C154 C -0.6001(7) 1.2855(4) 0.1871(3) 0.0582(9) Uani 1 1 d . . . H15L H -0.6412 1.3087 0.1764 0.070 Uiso 1 1 calc R . . C155 C -0.5657(7) 1.2164(3) 0.2250(3) 0.0582(9) Uani 1 1 d . . . H15M H -0.5053 1.2296 0.2333 0.070 Uiso 1 1 calc R . . H15N H -0.5860 1.2036 0.2473 0.070 Uiso 1 1 calc R . . C156 C -0.5608(7) 1.1793(3) 0.1984(3) 0.0582(9) Uani 1 1 d . . . H15O H -0.5184 1.1557 0.2102 0.087 Uiso 1 1 calc R . . H15P H -0.5405 1.1918 0.1763 0.087 Uiso 1 1 calc R . . H15Q H -0.6200 1.1653 0.1908 0.087 Uiso 1 1 calc R . . C157 C -0.7192(7) 1.2543(4) 0.2159(3) 0.0582(9) Uani 1 1 d . . . H15R H -0.7455 1.2234 0.2091 0.070 Uiso 1 1 calc R . . H15S H -0.7549 1.2772 0.1991 0.070 Uiso 1 1 calc R . . C158 C -0.7295(7) 1.2644(4) 0.2543(3) 0.0582(9) Uani 1 1 d . . . H15T H -0.7932 1.2643 0.2557 0.087 Uiso 1 1 calc R . . H15U H -0.7041 1.2949 0.2616 0.087 Uiso 1 1 calc R . . H15V H -0.6983 1.2408 0.2712 0.087 Uiso 1 1 calc R . . O28 O -0.4449(5) 1.4011(3) 0.0214(2) 0.0787(12) Uani 1 1 d . . . N3 N -0.3704(7) 1.4147(4) -0.0240(3) 0.0787(12) Uani 1 1 d . . . C159 C -0.3862(8) 1.3907(5) 0.0061(3) 0.0787(12) Uani 1 1 d . . . H15W H -0.3493 1.3650 0.0149 0.094 Uiso 1 1 calc R . . C160 C -0.2932(8) 1.4055(4) -0.0377(3) 0.0787(12) Uani 1 1 d . . . H16A H -0.2560 1.3831 -0.0210 0.094 Uiso 1 1 calc R . . H16B H -0.2583 1.4344 -0.0379 0.094 Uiso 1 1 calc R . . C161 C -0.3142(8) 1.3865(4) -0.0758(3) 0.0787(12) Uani 1 1 d . . . H16C H -0.2586 1.3800 -0.0848 0.118 Uiso 1 1 calc R . . H16D H -0.3497 1.4091 -0.0925 0.118 Uiso 1 1 calc R . . H16E H -0.3485 1.3579 -0.0756 0.118 Uiso 1 1 calc R . . C162 C -0.4287(8) 1.4531(4) -0.0381(3) 0.0787(12) Uani 1 1 d . . . H16F H -0.4886 1.4478 -0.0320 0.094 Uiso 1 1 calc R . . H16G H -0.4353 1.4545 -0.0657 0.094 Uiso 1 1 calc R . . C163 C -0.3932(8) 1.4988(4) -0.0218(3) 0.0787(12) Uani 1 1 d . . . H16H H -0.4349 1.5235 -0.0317 0.118 Uiso 1 1 calc R . . H16I H -0.3348 1.5048 -0.0285 0.118 Uiso 1 1 calc R . . H16J H -0.3868 1.4977 0.0056 0.118 Uiso 1 1 calc R . . O29 O -0.0637(5) 0.5133(2) 0.0459(2) 0.0659(10) Uani 1 1 d . . . N4 N -0.1635(6) 0.5258(3) 0.0847(3) 0.0659(10) Uani 1 1 d . . . C165 C -0.1125(8) 0.5395(4) 0.0611(3) 0.0659(10) Uani 1 1 d . . . H16N H -0.1126 0.5715 0.0552 0.079 Uiso 1 1 calc R . . C166 C -0.1598(8) 0.4771(3) 0.0973(3) 0.0659(10) Uani 1 1 d . . . H16O H -0.1708 0.4758 0.1234 0.079 Uiso 1 1 calc R . . H16P H -0.0993 0.4646 0.0973 0.079 Uiso 1 1 calc R . . C167 C -0.2271(7) 0.4477(4) 0.0728(3) 0.0659(10) Uani 1 1 d . . . H16Q H -0.2224 0.4158 0.0821 0.099 Uiso 1 1 calc R . . H16R H -0.2160 0.4485 0.0471 0.099 Uiso 1 1 calc R . . H16S H -0.2873 0.4595 0.0733 0.099 Uiso 1 1 calc R . . C168 C -0.2246(8) 0.5570(4) 0.0999(3) 0.0659(10) Uani 1 1 d . . . H16T H -0.2785 0.5397 0.1035 0.079 Uiso 1 1 calc R . . H16U H -0.2437 0.5824 0.0820 0.079 Uiso 1 1 calc R . . C169 C -0.1778(8) 0.5772(4) 0.1374(3) 0.0659(10) Uani 1 1 d . . . H16V H -0.2187 0.5981 0.1472 0.099 Uiso 1 1 calc R . . H16W H -0.1246 0.5943 0.1338 0.099 Uiso 1 1 calc R . . H16X H -0.1602 0.5520 0.1553 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0410(6) 0.0341(6) 0.0279(5) -0.0012(4) 0.0047(5) 0.0041(5) Cu2 0.0420(6) 0.0351(6) 0.0293(5) -0.0011(4) 0.0051(5) 0.0047(5) Cu3 0.0370(6) 0.0249(5) 0.0284(5) 0.0060(4) 0.0051(4) 0.0031(4) Cu4 0.0396(6) 0.0267(5) 0.0291(5) 0.0070(4) 0.0046(4) 0.0017(4) O1 0.047(4) 0.039(3) 0.022(3) 0.001(3) 0.002(3) 0.007(3) O2 0.048(4) 0.044(4) 0.030(3) -0.005(3) 0.009(3) 0.002(3) O3 0.051(4) 0.035(3) 0.027(3) 0.004(3) 0.008(3) 0.001(3) O4 0.051(4) 0.025(3) 0.030(3) 0.003(2) 0.007(3) 0.004(3) O7 0.042(4) 0.044(4) 0.035(3) 0.001(3) 0.004(3) 0.003(3) O8 0.045(4) 0.055(4) 0.035(3) 0.002(3) 0.008(3) 0.007(3) O11 0.040(3) 0.036(3) 0.029(3) 0.005(2) 0.008(3) 0.007(3) O12 0.045(4) 0.040(3) 0.033(3) 0.014(3) 0.007(3) 0.008(3) O13 0.046(4) 0.047(4) 0.038(4) 0.002(3) 0.008(3) 0.008(3) O14 0.048(4) 0.045(4) 0.031(3) 0.000(3) 0.006(3) 0.007(3) O17 0.042(3) 0.032(3) 0.028(3) 0.011(2) -0.001(3) -0.002(3) O18 0.044(3) 0.033(3) 0.027(3) 0.003(2) 0.009(3) 0.003(3) O19 0.065(4) 0.033(3) 0.033(3) -0.006(3) 0.011(3) -0.002(3) O20 0.056(4) 0.035(3) 0.035(3) -0.004(3) 0.006(3) 0.003(3) O23 0.037(3) 0.025(3) 0.036(3) 0.002(2) 0.003(3) 0.001(2) O24 0.043(3) 0.031(3) 0.041(4) 0.003(3) 0.012(3) -0.003(3) C1 0.026(4) 0.050(6) 0.039(5) 0.008(4) 0.004(4) 0.019(4) C2 0.028(4) 0.037(5) 0.038(5) -0.005(4) 0.006(4) 0.001(4) C3 0.045(5) 0.037(5) 0.034(5) 0.000(4) 0.011(4) 0.005(4) C4 0.051(6) 0.034(5) 0.052(6) 0.005(4) 0.006(5) 0.001(4) C5 0.053(6) 0.028(5) 0.036(5) -0.003(4) 0.002(4) 0.005(4) C6 0.024(4) 0.048(5) 0.038(5) -0.015(4) 0.002(4) 0.000(4) C7 0.028(4) 0.032(4) 0.035(5) 0.000(4) 0.003(4) 0.003(3) C8 0.031(5) 0.029(4) 0.039(5) 0.001(4) 0.006(4) 0.005(3) C9 0.026(4) 0.036(5) 0.041(5) 0.002(4) 0.003(4) 0.006(4) C10 0.030(4) 0.030(4) 0.040(5) -0.005(4) 0.006(4) 0.000(3) C11 0.044(5) 0.028(4) 0.044(5) 0.007(4) 0.014(4) 0.003(4) C12 0.078(7) 0.026(5) 0.043(5) 0.002(4) 0.024(5) 0.017(4) C13 0.057(6) 0.040(5) 0.042(5) -0.007(4) 0.020(5) 0.005(4) C14 0.037(5) 0.026(4) 0.052(6) 0.006(4) 0.014(4) 0.001(4) C15 0.031(5) 0.030(5) 0.046(5) -0.007(4) 0.005(4) -0.003(4) C16 0.043(5) 0.028(5) 0.045(5) -0.003(4) 0.010(4) -0.004(4) C17 0.055(6) 0.027(5) 0.039(5) -0.001(4) 0.004(4) -0.005(4) C18 0.040(5) 0.037(5) 0.031(5) 0.004(4) 0.004(4) 0.000(4) C19 0.053(6) 0.025(4) 0.039(5) -0.005(4) 0.004(4) -0.010(4) C20 0.088(8) 0.028(5) 0.037(5) 0.002(4) 0.007(5) -0.003(5) C21 0.099(8) 0.040(6) 0.033(5) -0.005(4) 0.006(5) -0.009(5) C22 0.070(7) 0.036(5) 0.034(5) 0.010(4) 0.002(5) -0.010(5) C23 0.048(5) 0.032(5) 0.031(5) 0.002(4) 0.006(4) -0.009(4) C24 0.042(5) 0.028(5) 0.044(5) 0.013(4) 0.005(4) 0.012(4) C25 0.141(12) 0.039(6) 0.054(7) 0.017(5) 0.046(7) 0.034(7) C38 0.045(5) 0.029(4) 0.028(5) -0.005(4) -0.001(4) 0.004(4) C39 0.039(5) 0.029(4) 0.038(5) -0.009(4) 0.002(4) -0.004(4) C40 0.048(6) 0.044(5) 0.025(4) -0.001(4) 0.008(4) -0.008(4) C41 0.046(6) 0.041(5) 0.035(5) 0.006(4) -0.004(4) -0.003(4) C42 0.036(5) 0.044(5) 0.040(5) 0.005(4) -0.007(4) -0.005(4) C43 0.045(5) 0.021(4) 0.037(5) 0.004(3) 0.006(4) 0.000(4) C44 0.035(5) 0.031(4) 0.036(5) 0.006(4) 0.000(4) 0.002(4) C45 0.035(5) 0.031(5) 0.042(5) 0.007(4) -0.004(4) -0.002(4) C46 0.042(5) 0.024(4) 0.037(5) 0.005(4) -0.003(4) -0.003(4) C47 0.041(5) 0.023(4) 0.034(5) 0.001(3) -0.001(4) -0.009(4) C48 0.036(5) 0.032(5) 0.036(5) 0.007(4) 0.001(4) -0.001(4) C49 0.034(5) 0.036(5) 0.042(5) 0.010(4) -0.001(4) 0.004(4) C50 0.043(5) 0.049(5) 0.037(5) 0.006(4) 0.012(4) 0.008(4) C51 0.037(5) 0.030(4) 0.034(5) -0.002(4) -0.001(4) 0.006(4) C52 0.031(4) 0.034(5) 0.033(5) -0.005(4) 0.004(4) 0.001(4) C53 0.042(5) 0.030(5) 0.036(5) -0.003(4) 0.010(4) 0.004(4) C54 0.039(5) 0.033(5) 0.036(5) 0.001(4) 0.011(4) 0.005(4) C55 0.053(6) 0.025(4) 0.030(4) 0.007(3) 0.013(4) 0.005(4) C56 0.032(4) 0.021(4) 0.034(5) 0.002(3) 0.004(4) 0.007(3) C57 0.042(5) 0.028(4) 0.036(5) 0.000(4) 0.006(4) 0.003(4) C58 0.045(5) 0.035(5) 0.032(5) 0.003(4) 0.014(4) 0.000(4) C59 0.042(5) 0.039(5) 0.025(4) -0.001(4) 0.004(4) 0.003(4) C60 0.042(5) 0.021(4) 0.032(4) 0.001(3) 0.010(4) 0.001(3) C61 0.047(5) 0.020(4) 0.030(5) -0.001(3) 0.001(4) 0.003(4) C62 0.044(6) 0.056(6) 0.052(6) 0.018(5) 0.007(5) 0.018(5) C75 0.045(5) 0.028(4) 0.030(5) -0.010(4) 0.006(4) 0.006(4) C76 0.043(5) 0.032(4) 0.031(5) -0.010(4) 0.007(4) -0.002(4) C77 0.050(6) 0.030(5) 0.035(5) -0.007(4) 0.007(4) 0.009(4) C78 0.052(6) 0.035(5) 0.030(5) -0.006(4) 0.009(4) 0.003(4) C79 0.036(5) 0.027(4) 0.047(5) -0.007(4) 0.011(4) -0.001(4) C80 0.042(5) 0.020(4) 0.039(5) -0.010(4) 0.003(4) 0.006(4) C81 0.040(5) 0.026(4) 0.032(5) -0.010(4) 0.008(4) 0.001(4) C82 0.039(5) 0.030(4) 0.035(5) -0.006(4) 0.003(4) 0.001(4) C83 0.034(5) 0.038(5) 0.035(5) 0.000(4) 0.008(4) 0.008(4) C84 0.036(5) 0.033(5) 0.046(5) -0.001(4) 0.003(4) 0.000(4) C85 0.039(5) 0.050(6) 0.042(5) 0.003(4) 0.010(4) 0.005(4) C86 0.047(6) 0.046(6) 0.046(6) 0.005(4) 0.002(5) 0.004(4) C87 0.042(5) 0.044(5) 0.039(5) 0.008(4) -0.003(4) 0.008(4) C88 0.045(5) 0.026(4) 0.038(5) 0.006(4) 0.009(4) 0.004(4) C89 0.029(4) 0.031(4) 0.042(5) 0.004(4) -0.001(4) 0.005(3) C90 0.038(5) 0.032(5) 0.044(5) 0.008(4) -0.002(4) -0.002(4) C91 0.032(5) 0.034(5) 0.042(5) 0.003(4) -0.001(4) -0.001(4) C92 0.040(5) 0.029(4) 0.035(5) -0.003(4) 0.001(4) 0.002(4) C93 0.040(5) 0.020(4) 0.042(5) -0.004(4) 0.002(4) 0.003(4) C94 0.046(6) 0.047(5) 0.041(5) 0.007(4) -0.006(4) 0.014(4) C95 0.050(6) 0.068(7) 0.030(5) 0.013(5) 0.007(4) 0.025(5) C96 0.051(6) 0.043(5) 0.028(5) 0.004(4) 0.011(4) 0.007(4) C97 0.029(4) 0.021(4) 0.031(4) -0.002(3) 0.000(4) 0.003(3) C98 0.031(4) 0.030(4) 0.031(5) -0.011(4) 0.008(4) -0.003(3) C99 0.043(6) 0.073(7) 0.062(7) -0.007(6) 0.007(5) 0.024(5) C112 0.045(5) 0.029(5) 0.042(5) -0.012(4) 0.008(4) 0.004(4) C113 0.049(6) 0.031(5) 0.046(5) -0.009(4) 0.007(4) -0.009(4) C114 0.110(9) 0.037(6) 0.047(6) -0.016(5) 0.030(6) -0.010(6) C115 0.135(11) 0.057(7) 0.041(6) -0.012(5) 0.029(7) -0.009(7) C116 0.115(10) 0.049(7) 0.063(7) -0.030(6) 0.028(7) -0.012(6) C117 0.058(7) 0.050(6) 0.062(7) -0.003(5) 0.021(5) 0.000(5) C118 0.055(6) 0.034(5) 0.038(5) -0.009(4) 0.013(4) -0.002(4) C119 0.058(7) 0.037(6) 0.063(7) -0.005(5) 0.020(5) -0.003(5) C120 0.049(6) 0.044(6) 0.059(7) -0.020(5) 0.006(5) -0.008(5) C121 0.041(5) 0.033(5) 0.064(6) -0.017(5) 0.016(5) -0.010(4) C122 0.049(6) 0.038(5) 0.052(6) -0.011(4) 0.021(5) -0.009(4) C123 0.051(6) 0.032(5) 0.063(7) -0.022(5) 0.010(5) -0.004(4) C124 0.038(5) 0.033(5) 0.068(7) -0.003(5) -0.003(5) -0.001(4) C125 0.034(5) 0.041(5) 0.049(6) -0.012(4) -0.006(4) -0.003(4) C126 0.039(5) 0.032(5) 0.066(7) -0.015(5) 0.010(5) -0.002(4) C127 0.026(5) 0.031(5) 0.065(7) -0.010(5) -0.001(4) 0.000(4) C128 0.029(5) 0.033(5) 0.063(7) -0.009(5) 0.001(5) 0.005(4) C129 0.024(4) 0.028(4) 0.048(5) 0.000(4) -0.003(4) 0.006(3) C130 0.034(5) 0.027(5) 0.050(6) -0.001(4) 0.001(4) 0.008(4) C131 0.051(6) 0.033(5) 0.059(6) -0.014(5) -0.004(5) 0.007(4) C132 0.050(6) 0.027(5) 0.067(7) 0.005(5) 0.000(5) -0.004(4) C133 0.044(5) 0.036(5) 0.044(5) 0.002(4) 0.000(4) 0.001(4) C134 0.031(5) 0.023(4) 0.046(5) 0.007(4) 0.000(4) 0.004(3) C135 0.030(4) 0.015(4) 0.045(5) -0.001(4) 0.003(4) 0.003(3) C136 0.062(7) 0.033(5) 0.094(9) -0.017(5) 0.012(6) -0.004(5) O5 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) O6 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C26 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C27 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C28 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C29 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C30 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C31 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C32 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C33 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C34 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C35 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C36 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C37 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C28' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C29' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C30' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C31' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C32' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C33' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C34' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C35' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C36' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) C37' 0.146(4) 0.076(3) 0.095(3) -0.003(2) -0.009(3) -0.012(3) O9 0.043(4) 0.063(4) 0.066(5) 0.020(4) 0.020(3) 0.015(3) O10 0.064(5) 0.069(5) 0.081(5) 0.010(4) 0.022(4) -0.014(4) C63 0.037(6) 0.055(7) 0.086(8) 0.028(6) 0.011(5) 0.009(5) C64 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C65 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C66 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C67 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C68 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C69 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C70 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C71 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C72 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C73 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) C74 0.086(3) 0.113(4) 0.117(4) -0.011(3) 0.019(3) -0.002(3) O15 0.058(5) 0.111(8) 0.090(7) 0.025(6) 0.011(5) 0.029(5) O16 0.068(6) 0.077(6) 0.120(8) -0.011(6) 0.005(6) 0.020(5) C100 0.037(7) 0.146(15) 0.062(8) -0.002(9) 0.006(6) 0.047(8) C101 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C102 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C103 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C104 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C105 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C106 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C107 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C108 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C109 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C110 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) C111 0.095(3) 0.112(3) 0.096(3) -0.009(3) 0.010(2) 0.010(3) O21 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) O22 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C137 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C138 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C139 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C140 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C141 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C142 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C143 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C144 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C145 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C146 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C147 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C148 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) O221 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) O222 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C237 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C238 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C239 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C240 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C241 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C242 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C243 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C244 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C245 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C246 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C247 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) C248 0.109(5) 0.091(4) 0.225(8) -0.030(4) 0.019(5) -0.001(3) O25 0.074(3) 0.080(3) 0.065(3) 0.009(2) 0.025(2) -0.002(2) N1 0.074(3) 0.080(3) 0.065(3) 0.009(2) 0.025(2) -0.002(2) C149 0.074(3) 0.080(3) 0.065(3) 0.009(2) 0.025(2) -0.002(2) C150 0.074(3) 0.080(3) 0.065(3) 0.009(2) 0.025(2) -0.002(2) C151 0.074(3) 0.080(3) 0.065(3) 0.009(2) 0.025(2) -0.002(2) C152 0.074(3) 0.080(3) 0.065(3) 0.009(2) 0.025(2) -0.002(2) C153 0.074(3) 0.080(3) 0.065(3) 0.009(2) 0.025(2) -0.002(2) O26 0.048(4) 0.046(4) 0.034(3) 0.000(3) 0.012(3) 0.000(3) C164 0.134(11) 0.057(7) 0.037(6) -0.009(5) 0.015(7) 0.013(7) O27 0.060(2) 0.059(2) 0.060(2) 0.0043(17) 0.0228(19) -0.0032(18) N2 0.060(2) 0.059(2) 0.060(2) 0.0043(17) 0.0228(19) -0.0032(18) C154 0.060(2) 0.059(2) 0.060(2) 0.0043(17) 0.0228(19) -0.0032(18) C155 0.060(2) 0.059(2) 0.060(2) 0.0043(17) 0.0228(19) -0.0032(18) C156 0.060(2) 0.059(2) 0.060(2) 0.0043(17) 0.0228(19) -0.0032(18) C157 0.060(2) 0.059(2) 0.060(2) 0.0043(17) 0.0228(19) -0.0032(18) C158 0.060(2) 0.059(2) 0.060(2) 0.0043(17) 0.0228(19) -0.0032(18) O28 0.073(3) 0.086(3) 0.076(3) 0.017(2) 0.010(2) 0.017(2) N3 0.073(3) 0.086(3) 0.076(3) 0.017(2) 0.010(2) 0.017(2) C159 0.073(3) 0.086(3) 0.076(3) 0.017(2) 0.010(2) 0.017(2) C160 0.073(3) 0.086(3) 0.076(3) 0.017(2) 0.010(2) 0.017(2) C161 0.073(3) 0.086(3) 0.076(3) 0.017(2) 0.010(2) 0.017(2) C162 0.073(3) 0.086(3) 0.076(3) 0.017(2) 0.010(2) 0.017(2) C163 0.073(3) 0.086(3) 0.076(3) 0.017(2) 0.010(2) 0.017(2) O29 0.076(3) 0.052(2) 0.069(3) 0.0140(19) 0.012(2) 0.0014(19) N4 0.076(3) 0.052(2) 0.069(3) 0.0140(19) 0.012(2) 0.0014(19) C165 0.076(3) 0.052(2) 0.069(3) 0.0140(19) 0.012(2) 0.0014(19) C166 0.076(3) 0.052(2) 0.069(3) 0.0140(19) 0.012(2) 0.0014(19) C167 0.076(3) 0.052(2) 0.069(3) 0.0140(19) 0.012(2) 0.0014(19) C168 0.076(3) 0.052(2) 0.069(3) 0.0140(19) 0.012(2) 0.0014(19) C169 0.076(3) 0.052(2) 0.069(3) 0.0140(19) 0.012(2) 0.0014(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O20 1.945(6) . ? Cu1 O1 1.951(6) . ? Cu1 O14 1.955(6) . ? Cu1 O7 1.980(6) . ? Cu1 O25 2.154(7) . ? Cu1 Cu2 2.6258(14) . ? Cu2 O8 1.939(6) . ? Cu2 O13 1.942(6) . ? Cu2 O19 1.955(6) . ? Cu2 O2 1.959(6) . ? Cu2 O26 2.164(6) . ? Cu3 O3 1.949(5) . ? Cu3 O11 1.962(5) . ? Cu3 O17 1.967(5) . ? Cu3 O23 1.969(5) . ? Cu3 O27 2.152(6) . ? Cu3 Cu4 2.6225(13) . ? Cu4 O24 1.947(6) . ? Cu4 O4 1.955(5) . ? Cu4 O18 1.959(6) . ? Cu4 O12 1.976(6) . ? Cu4 O28 2.151(8) . ? O1 C1 1.267(10) . ? O2 C1 1.251(10) . ? O3 C24 1.249(10) . ? O4 C24 1.249(9) . ? O7 C38 1.282(9) . ? O8 C38 1.241(10) . ? O11 C61 1.256(9) . ? O12 C61 1.278(9) . ? O13 C75 1.239(10) . ? O14 C75 1.266(10) . ? O17 C98 1.265(9) . ? O18 C98 1.238(9) . ? O19 C112 1.276(10) . ? O20 C112 1.272(10) . ? O23 C135 1.264(9) . ? O24 C135 1.256(9) . ? C1 C2 1.500(12) . ? C2 C7 1.390(11) . ? C2 C3 1.390(11) . ? C3 C4 1.383(12) . ? C3 H3A 0.9500 . ? C4 C5 1.362(12) . ? C4 H4A 0.9500 . ? C5 C6 1.383(12) . ? C5 H5A 0.9500 . ? C6 C7 1.399(11) . ? C6 C8 1.468(11) . ? C7 H7A 0.9500 . ? C8 C9 1.176(11) . ? C9 C10 1.426(12) . ? C10 C11 1.392(11) . ? C10 C15 1.400(11) . ? C11 C12 1.392(11) . ? C11 H11A 0.9500 . ? C12 C13 1.397(12) . ? C12 C25 1.510(9) . ? C13 C14 1.395(11) . ? C13 H13A 0.9500 . ? C14 C15 1.380(11) . ? C14 C16 1.439(12) . ? C15 H15A 0.9500 . ? C16 C17 1.196(11) . ? C17 C19 1.427(12) . ? C18 C19 1.381(11) . ? C18 C23 1.411(11) . ? C18 H18A 0.9500 . ? C19 C20 1.419(12) . ? C20 C21 1.368(12) . ? C20 H20A 0.9500 . ? C21 C22 1.389(12) . ? C21 H21A 0.9500 . ? C22 C23 1.391(11) . ? C22 H22A 0.9500 . ? C23 C24 1.504(11) . ? C25 O6 1.443(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C38 C39 1.500(12) . ? C39 C44 1.380(11) . ? C39 C40 1.409(11) . ? C40 C41 1.375(12) . ? C40 H40A 0.9500 . ? C41 C42 1.384(12) . ? C41 H41A 0.9500 . ? C42 C43 1.380(11) . ? C42 H42A 0.9500 . ? C43 C44 1.390(11) . ? C43 C45 1.435(12) . ? C44 H44A 0.9500 . ? C45 C46 1.188(12) . ? C46 C47 1.438(12) . ? C47 C48 1.391(11) . ? C47 C52 1.406(11) . ? C48 C49 1.361(11) . ? C48 H48A 0.9500 . ? C49 C50 1.401(11) . ? C49 C62 1.518(12) . ? C50 C51 1.417(11) . ? C50 H50A 0.9500 . ? C51 C52 1.365(11) . ? C51 C53 1.433(11) . ? C52 H52A 0.9500 . ? C53 C54 1.202(11) . ? C54 C56 1.436(11) . ? C55 C56 1.388(11) . ? C55 C60 1.404(11) . ? C55 H55A 0.9500 . ? C56 C57 1.396(11) . ? C57 C58 1.388(11) . ? C57 H57A 0.9500 . ? C58 C59 1.382(11) . ? C58 H58A 0.9500 . ? C59 C60 1.387(11) . ? C59 H59A 0.9500 . ? C60 C61 1.483(11) . ? C62 O9 1.464(11) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C75 C76 1.515(12) . ? C76 C77 1.377(11) . ? C76 C81 1.382(11) . ? C77 C78 1.386(12) . ? C77 H77A 0.9500 . ? C78 C79 1.372(11) . ? C78 H78A 0.9500 . ? C79 C80 1.404(11) . ? C79 H79A 0.9500 . ? C80 C81 1.377(11) . ? C80 C82 1.432(12) . ? C81 H81A 0.9500 . ? C82 C83 1.202(11) . ? C83 C84 1.432(12) . ? C84 C89 1.376(12) . ? C84 C85 1.395(12) . ? C85 C86 1.402(12) . ? C85 H85A 0.9500 . ? C86 C87 1.348(12) . ? C86 C99 1.502(12) . ? C87 C88 1.411(12) . ? C87 H87A 0.9500 . ? C88 C89 1.403(11) . ? C88 C90 1.414(12) . ? C89 H89A 0.9500 . ? C90 C91 1.204(12) . ? C91 C93 1.412(12) . ? C92 C97 1.372(11) . ? C92 C93 1.425(11) . ? C92 H92A 0.9500 . ? C93 C94 1.380(11) . ? C94 C95 1.373(12) . ? C94 H94A 0.9500 . ? C95 C96 1.367(12) . ? C95 H95A 0.9500 . ? C96 C97 1.394(11) . ? C96 H96A 0.9500 . ? C97 C98 1.517(10) . ? C99 O15 1.429(13) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C112 C113 1.495(11) . ? C113 C114 1.373(12) . ? C113 C118 1.379(12) . ? C114 C115 1.375(13) . ? C114 H11B 0.9500 . ? C115 C116 1.395(15) . ? C115 H11C 0.9500 . ? C116 C117 1.393(14) . ? C116 H11D 0.9500 . ? C117 C118 1.381(12) . ? C117 C119 1.426(14) . ? C118 H11E 0.9500 . ? C119 C120 1.188(13) . ? C120 C121 1.462(14) . ? C121 C122 1.375(12) . ? C121 C126 1.415(12) . ? C122 C123 1.384(12) . ? C122 H12A 0.9500 . ? C123 C124 1.399(12) . ? C123 C136 1.509(9) . ? C124 C125 1.385(12) . ? C124 H12B 0.9500 . ? C125 C126 1.386(13) . ? C125 C127 1.429(13) . ? C126 H12C 0.9500 . ? C127 C128 1.199(13) . ? C128 C130 1.420(13) . ? C129 C130 1.376(11) . ? C129 C134 1.400(11) . ? C129 H12D 0.9500 . ? C130 C131 1.405(13) . ? C131 C132 1.382(13) . ? C131 H13B 0.9500 . ? C132 C133 1.392(12) . ? C132 H13C 0.9500 . ? C133 C134 1.390(11) . ? C133 H13D 0.9500 . ? C134 C135 1.494(11) . ? C136 O221 1.4409(10) . ? C136 O21 1.4412(10) . ? C136 H13E 0.9900 . ? C136 H13F 0.9900 . ? O5 C26 1.206(9) . ? O6 C26 1.347(9) . ? C26 C27 1.495(8) . ? C27 C28 1.5097(10) . ? C27 C28' 1.5101(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 H27C 0.9599 . ? C27 H27D 0.9600 . ? C28 C29 1.5096(10) . ? C28 H27C 1.0379 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.5097(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.5095(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.5097(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.5095(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.5099(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.5101(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.5098(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.5102(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C28' C29' 1.5100(10) . ? C28' H28C 0.9900 . ? C28' H28D 0.9900 . ? C29' C30' 1.5100(10) . ? C29' H29C 0.9900 . ? C29' H29D 0.9900 . ? C30' C31' 1.5099(10) . ? C30' H30C 0.9900 . ? C30' H30D 0.9900 . ? C31' C32' 1.5100(10) . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? C32' C33' 1.5102(10) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33' C34' 1.5101(10) . ? C33' H33C 0.9900 . ? C33' H33D 0.9900 . ? C34' C35' 1.5100(10) . ? C34' H34C 0.9900 . ? C34' H34D 0.9900 . ? C35' C36' 1.5100(10) . ? C35' H35C 0.9900 . ? C35' H35D 0.9900 . ? C36' C37' 1.5101(10) . ? C36' H36C 0.9900 . ? C36' H36D 0.9900 . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? O9 C63 1.338(12) . ? O10 C63 1.223(12) . ? C63 C64 1.593(14) . ? C64 C65 1.509(11) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.509(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.510(10) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.509(8) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.511(10) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.511(10) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.509(12) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.510(10) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.510(10) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.510(10) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? O15 C100 1.272(18) . ? O16 C100 1.245(15) . ? C100 C101 1.450(16) . ? C101 C102 1.510(13) . ? C101 H10A 0.9500 . ? C102 C103 1.510(13) . ? C102 H10B 0.9900 . ? C102 H10C 0.9900 . ? C103 C104 1.510(13) . ? C103 H10D 0.9900 . ? C103 H10E 0.9900 . ? C104 C105 1.510(13) . ? C104 H10F 0.9900 . ? C104 H10G 0.9900 . ? C105 C106 1.510(13) . ? C105 H10H 0.9900 . ? C105 H10I 0.9900 . ? C106 C107 1.510(13) . ? C106 H10J 0.9900 . ? C106 H10K 0.9900 . ? C107 C108 1.510(13) . ? C107 H10L 0.9900 . ? C107 H10M 0.9900 . ? C108 C109 1.510(13) . ? C108 H10N 0.9900 . ? C108 H10O 0.9900 . ? C109 C110 1.471(10) . ? C109 H10P 0.9900 . ? C109 H10Q 0.9900 . ? C110 C111 1.509(15) . ? C110 H11F 0.9900 . ? C110 H11G 0.9900 . ? C111 H11H 0.9800 . ? C111 H11I 0.9800 . ? C111 H11J 0.9800 . ? O21 C137 1.3469(9) . ? O22 C137 1.2060(9) . ? C137 C138 1.4962(9) . ? C138 C139 1.5102(10) . ? C138 H13G 0.9900 . ? C138 H13H 0.9900 . ? C139 C140 1.5095(11) . ? C139 H13I 0.9900 . ? C139 H13J 0.9900 . ? C140 C141 1.5096(10) . ? C140 H14A 0.9900 . ? C140 H14B 0.9900 . ? C141 C142 1.5100(10) . ? C141 H14C 0.9900 . ? C141 H14D 0.9900 . ? C142 C143 1.5100(10) . ? C142 H14E 0.9900 . ? C142 H14F 0.9900 . ? C143 C144 1.5099(10) . ? C143 H14G 0.9900 . ? C143 H14H 0.9900 . ? C144 C145 1.5101(10) . ? C144 H14I 0.9900 . ? C144 H14J 0.9900 . ? C145 C146 1.5101(10) . ? C145 H14K 0.9900 . ? C145 H14L 0.9900 . ? C146 C147 1.5099(11) . ? C146 H14M 0.9900 . ? C146 H14N 0.9900 . ? C147 C148 1.5098(11) . ? C147 H14O 0.9900 . ? C147 H14P 0.9900 . ? C148 C74 1.89(4) 2_455 ? C148 H14Q 0.9800 . ? C148 H14R 0.9800 . ? C148 H14S 0.9800 . ? O221 C237 1.3474(9) . ? O222 C237 1.2060(9) . ? C237 C238 1.4957(9) . ? C238 C239 1.5100(10) . ? C238 H23A 0.9900 . ? C238 H23B 0.9900 . ? C239 C240 1.5103(10) . ? C239 H23C 0.9900 . ? C239 H23D 0.9900 . ? C240 C241 1.5104(10) . ? C240 H24A 0.9900 . ? C240 H24B 0.9900 . ? C241 C242 1.5103(11) . ? C241 H24C 0.9900 . ? C241 H24D 0.9900 . ? C242 C243 1.5101(10) . ? C242 H24E 0.9900 . ? C242 H24F 0.9900 . ? C243 C244 1.5100(10) . ? C243 H24G 0.9900 . ? C243 H24H 0.9900 . ? C244 C245 1.5099(10) . ? C244 H24I 0.9900 . ? C244 H24J 0.9900 . ? C245 C246 1.5099(10) . ? C245 H24K 0.9900 . ? C245 H24L 0.9900 . ? C246 C247 1.5099(11) . ? C246 H24M 0.9900 . ? C246 H24N 0.9900 . ? C247 C248 1.5100(10) . ? C247 H24O 0.9900 . ? C247 H24P 0.9900 . ? C248 H24Q 0.9800 . ? C248 H24R 0.9800 . ? C248 H24S 0.9800 . ? O25 C149 1.274(12) . ? N1 C149 1.338(13) . ? N1 C152 1.453(14) . ? N1 C150 1.472(14) . ? C149 H14T 0.9500 . ? C150 C151 1.512(15) . ? C150 H15B 0.9900 . ? C150 H15C 0.9900 . ? C151 H15D 0.9800 . ? C151 H15E 0.9800 . ? C151 H15F 0.9800 . ? C152 C153 1.536(15) . ? C152 H15G 0.9900 . ? C152 H15H 0.9900 . ? C153 H15I 0.9800 . ? C153 H15J 0.9800 . ? C153 H15K 0.9800 . ? O26 C164 1.401(11) . ? O26 H26A 0.8500 . ? C164 H16K 0.9800 . ? C164 H16L 0.9800 . ? C164 H16M 0.9800 . ? O27 C154 1.241(11) . ? N2 C154 1.308(12) . ? N2 C157 1.451(12) . ? N2 C155 1.515(13) . ? C154 H15L 0.9500 . ? C155 C156 1.454(13) . ? C155 H15M 0.9900 . ? C155 H15N 0.9900 . ? C156 H15O 0.9800 . ? C156 H15P 0.9800 . ? C156 H15Q 0.9800 . ? C157 C158 1.460(13) . ? C157 H15R 0.9900 . ? C157 H15S 0.9900 . ? C158 H15T 0.9800 . ? C158 H15U 0.9800 . ? C158 H15V 0.9800 . ? O28 C159 1.177(13) . ? N3 C159 1.352(14) . ? N3 C160 1.385(14) . ? N3 C162 1.456(14) . ? C159 H15W 0.9500 . ? C160 C161 1.467(16) . ? C160 H16A 0.9900 . ? C160 H16B 0.9900 . ? C161 H16C 0.9800 . ? C161 H16D 0.9800 . ? C161 H16E 0.9800 . ? C162 C163 1.506(16) . ? C162 H16F 0.9900 . ? C162 H16G 0.9900 . ? C163 H16H 0.9800 . ? C163 H16I 0.9800 . ? C163 H16J 0.9800 . ? O29 C165 1.258(12) . ? N4 C165 1.320(13) . ? N4 C168 1.475(13) . ? N4 C166 1.478(12) . ? C165 H16N 0.9500 . ? C166 C167 1.491(14) . ? C166 H16O 0.9900 . ? C166 H16P 0.9900 . ? C167 H16Q 0.9800 . ? C167 H16R 0.9800 . ? C167 H16S 0.9800 . ? C168 C169 1.530(14) . ? C168 H16T 0.9900 . ? C168 H16U 0.9900 . ? C169 H16V 0.9800 . ? C169 H16W 0.9800 . ? C169 H16X 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O20 Cu1 O1 169.9(2) . . ? O20 Cu1 O14 89.3(2) . . ? O1 Cu1 O14 90.7(2) . . ? O20 Cu1 O7 88.9(2) . . ? O1 Cu1 O7 88.7(2) . . ? O14 Cu1 O7 166.3(2) . . ? O20 Cu1 O25 91.8(3) . . ? O1 Cu1 O25 98.2(3) . . ? O14 Cu1 O25 98.8(3) . . ? O7 Cu1 O25 94.8(3) . . ? O20 Cu1 Cu2 82.50(18) . . ? O1 Cu1 Cu2 87.45(16) . . ? O14 Cu1 Cu2 84.36(17) . . ? O7 Cu1 Cu2 81.91(17) . . ? O25 Cu1 Cu2 173.5(2) . . ? O8 Cu2 O13 170.9(3) . . ? O8 Cu2 O19 88.2(3) . . ? O13 Cu2 O19 89.0(3) . . ? O8 Cu2 O2 89.0(2) . . ? O13 Cu2 O2 92.0(2) . . ? O19 Cu2 O2 167.6(2) . . ? O8 Cu2 O26 94.1(2) . . ? O13 Cu2 O26 94.8(2) . . ? O19 Cu2 O26 97.3(2) . . ? O2 Cu2 O26 95.0(2) . . ? O8 Cu2 Cu1 87.18(18) . . ? O13 Cu2 Cu1 84.07(18) . . ? O19 Cu2 Cu1 86.55(17) . . ? O2 Cu2 Cu1 81.25(17) . . ? O26 Cu2 Cu1 176.03(16) . . ? O3 Cu3 O11 89.1(2) . . ? O3 Cu3 O17 90.2(2) . . ? O11 Cu3 O17 170.4(2) . . ? O3 Cu3 O23 167.3(2) . . ? O11 Cu3 O23 90.6(2) . . ? O17 Cu3 O23 87.9(2) . . ? O3 Cu3 O27 94.5(2) . . ? O11 Cu3 O27 96.6(2) . . ? O17 Cu3 O27 93.0(2) . . ? O23 Cu3 O27 98.2(2) . . ? O3 Cu3 Cu4 81.22(16) . . ? O11 Cu3 Cu4 85.85(16) . . ? O17 Cu3 Cu4 84.56(15) . . ? O23 Cu3 Cu4 86.09(16) . . ? O27 Cu3 Cu4 175.05(19) . . ? O24 Cu4 O4 169.6(2) . . ? O24 Cu4 O18 88.4(2) . . ? O4 Cu4 O18 90.2(2) . . ? O24 Cu4 O12 91.2(2) . . ? O4 Cu4 O12 87.9(2) . . ? O18 Cu4 O12 167.5(2) . . ? O24 Cu4 O28 94.6(3) . . ? O4 Cu4 O28 95.8(3) . . ? O18 Cu4 O28 95.1(3) . . ? O12 Cu4 O28 97.3(3) . . ? O24 Cu4 Cu3 82.41(17) . . ? O4 Cu4 Cu3 87.18(16) . . ? O18 Cu4 Cu3 84.30(15) . . ? O12 Cu4 Cu3 83.30(16) . . ? O28 Cu4 Cu3 177.0(2) . . ? C1 O1 Cu1 119.0(5) . . ? C1 O2 Cu2 126.1(6) . . ? C24 O3 Cu3 125.8(5) . . ? C24 O4 Cu4 118.2(5) . . ? C38 O7 Cu1 123.8(6) . . ? C38 O8 Cu2 120.7(5) . . ? C61 O11 Cu3 120.6(5) . . ? C61 O12 Cu4 122.8(5) . . ? C75 O13 Cu2 123.3(6) . . ? C75 O14 Cu1 121.5(5) . . ? C98 O17 Cu3 120.8(5) . . ? C98 O18 Cu4 122.2(5) . . ? C112 O19 Cu2 120.4(5) . . ? C112 O20 Cu1 125.7(5) . . ? C135 O23 Cu3 120.0(5) . . ? C135 O24 Cu4 125.2(5) . . ? O2 C1 O1 125.8(8) . . ? O2 C1 C2 116.9(8) . . ? O1 C1 C2 117.3(7) . . ? C7 C2 C3 120.6(8) . . ? C7 C2 C1 121.0(8) . . ? C3 C2 C1 118.3(7) . . ? C4 C3 C2 118.5(8) . . ? C4 C3 H3A 120.8 . . ? C2 C3 H3A 120.8 . . ? C5 C4 C3 122.0(8) . . ? C5 C4 H4A 119.0 . . ? C3 C4 H4A 119.0 . . ? C4 C5 C6 119.7(8) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C5 C6 C7 120.0(8) . . ? C5 C6 C8 119.5(7) . . ? C7 C6 C8 120.5(8) . . ? C2 C7 C6 119.1(8) . . ? C2 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? C9 C8 C6 174.3(9) . . ? C8 C9 C10 178.4(9) . . ? C11 C10 C15 118.1(8) . . ? C11 C10 C9 121.3(8) . . ? C15 C10 C9 120.6(7) . . ? C10 C11 C12 122.3(7) . . ? C10 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? C11 C12 C13 117.5(7) . . ? C11 C12 C25 121.6(8) . . ? C13 C12 C25 120.9(8) . . ? C14 C13 C12 121.8(8) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C15 C14 C13 118.8(8) . . ? C15 C14 C16 120.7(7) . . ? C13 C14 C16 120.5(8) . . ? C14 C15 C10 121.5(7) . . ? C14 C15 H15A 119.3 . . ? C10 C15 H15A 119.2 . . ? C17 C16 C14 177.3(9) . . ? C16 C17 C19 174.6(9) . . ? C19 C18 C23 120.6(8) . . ? C19 C18 H18A 119.7 . . ? C23 C18 H18A 119.7 . . ? C18 C19 C20 119.5(8) . . ? C18 C19 C17 118.6(8) . . ? C20 C19 C17 121.9(8) . . ? C21 C20 C19 119.4(8) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C22 121.3(9) . . ? C20 C21 H21A 119.3 . . ? C22 C21 H21A 119.3 . . ? C21 C22 C23 120.1(8) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C22 C23 C18 119.0(8) . . ? C22 C23 C24 122.6(7) . . ? C18 C23 C24 118.2(7) . . ? O4 C24 O3 126.9(8) . . ? O4 C24 C23 115.9(8) . . ? O3 C24 C23 117.2(7) . . ? O6 C25 C12 108.2(5) . . ? O6 C25 H25A 110.1 . . ? C12 C25 H25A 110.1 . . ? O6 C25 H25B 110.1 . . ? C12 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? O8 C38 O7 126.4(8) . . ? O8 C38 C39 118.4(7) . . ? O7 C38 C39 115.2(8) . . ? C44 C39 C40 119.7(8) . . ? C44 C39 C38 120.8(8) . . ? C40 C39 C38 119.4(8) . . ? C41 C40 C39 118.9(8) . . ? C41 C40 H40A 120.5 . . ? C39 C40 H40A 120.5 . . ? C40 C41 C42 121.2(8) . . ? C40 C41 H41A 119.4 . . ? C42 C41 H41A 119.4 . . ? C43 C42 C41 119.8(8) . . ? C43 C42 H42A 120.1 . . ? C41 C42 H42A 120.1 . . ? C42 C43 C44 119.8(8) . . ? C42 C43 C45 121.3(8) . . ? C44 C43 C45 118.9(7) . . ? C39 C44 C43 120.4(8) . . ? C39 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? C46 C45 C43 178.3(9) . . ? C45 C46 C47 178.7(9) . . ? C48 C47 C52 119.1(8) . . ? C48 C47 C46 121.0(7) . . ? C52 C47 C46 119.9(8) . . ? C49 C48 C47 121.4(8) . . ? C49 C48 H48A 119.3 . . ? C47 C48 H48A 119.3 . . ? C48 C49 C50 120.0(8) . . ? C48 C49 C62 120.2(8) . . ? C50 C49 C62 119.8(8) . . ? C49 C50 C51 119.0(8) . . ? C49 C50 H50A 120.5 . . ? C51 C50 H50A 120.5 . . ? C52 C51 C50 120.3(8) . . ? C52 C51 C53 120.0(7) . . ? C50 C51 C53 119.7(8) . . ? C51 C52 C47 120.1(8) . . ? C51 C52 H52A 119.9 . . ? C47 C52 H52A 119.9 . . ? C54 C53 C51 178.4(9) . . ? C53 C54 C56 176.8(9) . . ? C56 C55 C60 120.3(8) . . ? C56 C55 H55A 119.8 . . ? C60 C55 H55A 119.8 . . ? C55 C56 C57 120.4(7) . . ? C55 C56 C54 120.8(7) . . ? C57 C56 C54 118.7(7) . . ? C58 C57 C56 119.2(8) . . ? C58 C57 H57A 120.4 . . ? C56 C57 H57A 120.4 . . ? C59 C58 C57 120.1(8) . . ? C59 C58 H58A 119.9 . . ? C57 C58 H58A 119.9 . . ? C58 C59 C60 121.6(8) . . ? C58 C59 H59A 119.2 . . ? C60 C59 H59A 119.2 . . ? C59 C60 C55 118.3(8) . . ? C59 C60 C61 121.8(7) . . ? C55 C60 C61 119.9(7) . . ? O11 C61 O12 126.2(8) . . ? O11 C61 C60 118.1(7) . . ? O12 C61 C60 115.7(7) . . ? O9 C62 C49 109.0(7) . . ? O9 C62 H62A 109.9 . . ? C49 C62 H62A 109.9 . . ? O9 C62 H62B 109.9 . . ? C49 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? O13 C75 O14 126.3(8) . . ? O13 C75 C76 116.9(8) . . ? O14 C75 C76 116.7(7) . . ? C77 C76 C81 120.3(8) . . ? C77 C76 C75 119.0(8) . . ? C81 C76 C75 120.6(8) . . ? C76 C77 C78 120.1(8) . . ? C76 C77 H77A 119.9 . . ? C78 C77 H77A 119.9 . . ? C79 C78 C77 120.0(8) . . ? C79 C78 H78A 120.0 . . ? C77 C78 H78A 120.0 . . ? C78 C79 C80 119.8(8) . . ? C78 C79 H79A 120.1 . . ? C80 C79 H79A 120.1 . . ? C81 C80 C79 119.8(8) . . ? C81 C80 C82 120.1(8) . . ? C79 C80 C82 120.0(8) . . ? C80 C81 C76 119.9(8) . . ? C80 C81 H81A 120.1 . . ? C76 C81 H81A 120.1 . . ? C83 C82 C80 178.5(10) . . ? C82 C83 C84 179.2(10) . . ? C89 C84 C85 120.1(8) . . ? C89 C84 C83 121.0(8) . . ? C85 C84 C83 118.9(8) . . ? C84 C85 C86 119.5(9) . . ? C84 C85 H85A 120.3 . . ? C86 C85 H85A 120.3 . . ? C87 C86 C85 120.3(9) . . ? C87 C86 C99 120.8(9) . . ? C85 C86 C99 118.9(9) . . ? C86 C87 C88 121.5(8) . . ? C86 C87 H87A 119.3 . . ? C88 C87 H87A 119.3 . . ? C89 C88 C87 118.0(8) . . ? C89 C88 C90 121.3(8) . . ? C87 C88 C90 120.7(8) . . ? C84 C89 C88 120.7(8) . . ? C84 C89 H89A 119.6 . . ? C88 C89 H89A 119.6 . . ? C91 C90 C88 179.0(10) . . ? C90 C91 C93 177.4(9) . . ? C97 C92 C93 119.9(8) . . ? C97 C92 H92A 120.1 . . ? C93 C92 H92A 120.1 . . ? C94 C93 C91 122.3(8) . . ? C94 C93 C92 117.7(8) . . ? C91 C93 C92 119.8(8) . . ? C95 C94 C93 121.6(8) . . ? C95 C94 H94A 119.2 . . ? C93 C94 H94A 119.2 . . ? C96 C95 C94 120.9(8) . . ? C96 C95 H95A 119.6 . . ? C94 C95 H95A 119.6 . . ? C95 C96 C97 119.1(8) . . ? C95 C96 H96A 120.5 . . ? C97 C96 H96A 120.5 . . ? C92 C97 C96 120.9(7) . . ? C92 C97 C98 118.7(7) . . ? C96 C97 C98 120.2(7) . . ? O18 C98 O17 127.7(7) . . ? O18 C98 C97 116.8(7) . . ? O17 C98 C97 115.5(7) . . ? O15 C99 C86 108.9(8) . . ? O15 C99 H99A 109.9 . . ? C86 C99 H99A 109.9 . . ? O15 C99 H99B 109.9 . . ? C86 C99 H99B 109.9 . . ? H99A C99 H99B 108.3 . . ? O20 C112 O19 124.6(7) . . ? O20 C112 C113 117.0(8) . . ? O19 C112 C113 118.4(8) . . ? C114 C113 C118 120.7(8) . . ? C114 C113 C112 120.3(8) . . ? C118 C113 C112 119.0(8) . . ? C113 C114 C115 119.7(9) . . ? C113 C114 H11B 120.2 . . ? C115 C114 H11B 120.2 . . ? C114 C115 C116 120.4(9) . . ? C114 C115 H11C 119.8 . . ? C116 C115 H11C 119.8 . . ? C117 C116 C115 119.7(9) . . ? C117 C116 H11D 120.2 . . ? C115 C116 H11D 120.2 . . ? C118 C117 C116 119.2(9) . . ? C118 C117 C119 118.8(9) . . ? C116 C117 C119 121.9(9) . . ? C113 C118 C117 120.4(8) . . ? C113 C118 H11E 119.8 . . ? C117 C118 H11E 119.8 . . ? C120 C119 C117 174.7(11) . . ? C119 C120 C121 178.0(11) . . ? C122 C121 C126 120.2(9) . . ? C122 C121 C120 121.6(9) . . ? C126 C121 C120 118.1(8) . . ? C121 C122 C123 120.0(8) . . ? C121 C122 H12A 120.0 . . ? C123 C122 H12A 120.0 . . ? C122 C123 C124 119.9(6) . . ? C122 C123 C136 120.3(7) . . ? C124 C123 C136 119.8(8) . . ? C125 C124 C123 120.6(9) . . ? C125 C124 H12B 119.7 . . ? C123 C124 H12B 119.7 . . ? C124 C125 C126 119.5(9) . . ? C124 C125 C127 120.7(9) . . ? C126 C125 C127 119.8(8) . . ? C125 C126 C121 119.7(8) . . ? C125 C126 H12C 120.1 . . ? C121 C126 H12C 120.1 . . ? C128 C127 C125 178.6(10) . . ? C127 C128 C130 176.7(10) . . ? C130 C129 C134 121.4(8) . . ? C130 C129 H12D 119.3 . . ? C134 C129 H12D 119.3 . . ? C129 C130 C131 118.0(8) . . ? C129 C130 C128 123.4(8) . . ? C131 C130 C128 118.6(8) . . ? C132 C131 C130 121.6(8) . . ? C132 C131 H13B 119.2 . . ? C130 C131 H13B 119.2 . . ? C131 C132 C133 119.5(9) . . ? C131 C132 H13C 120.2 . . ? C133 C132 H13C 120.2 . . ? C134 C133 C132 119.9(9) . . ? C134 C133 H13D 120.1 . . ? C132 C133 H13D 120.1 . . ? C133 C134 C129 119.6(8) . . ? C133 C134 C135 119.1(8) . . ? C129 C134 C135 121.2(7) . . ? O24 C135 O23 125.3(7) . . ? O24 C135 C134 116.7(7) . . ? O23 C135 C134 118.0(7) . . ? O221 C136 C123 109.50(11) . . ? O21 C136 C123 109.49(10) . . ? O221 C136 H13E 94.4 . . ? O21 C136 H13E 109.8 . . ? C123 C136 H13E 109.8 . . ? O221 C136 H13F 123.7 . . ? O21 C136 H13F 109.8 . . ? C123 C136 H13F 109.8 . . ? H13E C136 H13F 108.2 . . ? C26 O6 C25 121.9(6) . . ? O5 C26 O6 116.5(6) . . ? O5 C26 C27 125.2(6) . . ? O6 C26 C27 118.3(5) . . ? C26 C27 C28 110.58(10) . . ? C26 C27 C28' 110.51(10) . . ? C28 C27 C28' 67.5(7) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C28' C27 H27A 137.8 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? C28' C27 H27B 45.0 . . ? H27A C27 H27B 108.1 . . ? C26 C27 H27C 109.7 . . ? C28' C27 H27C 107.7 . . ? H27A C27 H27C 70.0 . . ? H27B C27 H27C 138.7 . . ? C26 C27 H27D 110.1 . . ? C28 C27 H27D 136.6 . . ? C28' C27 H27D 110.6 . . ? H27B C27 H27D 69.4 . . ? H27C C27 H27D 108.1 . . ? C29 C28 C27 109.81(10) . . ? C29 C28 H27C 147.8 . . ? C29 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? H27C C28 H28A 93.2 . . ? C29 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H27C C28 H28B 82.7 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C30 109.81(10) . . ? C28 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? C28 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 109.82(10) . . ? C31 C30 H30A 109.7 . . ? C29 C30 H30A 109.7 . . ? C31 C30 H30B 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C30 C31 C32 109.80(10) . . ? C30 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? C30 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C33 C32 C31 109.81(10) . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32B 109.7 . . ? C31 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C32 C33 C34 109.81(10) . . ? C32 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? C32 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C33 C34 C35 109.74(10) . . ? C33 C34 H34A 109.7 . . ? C35 C34 H34A 109.7 . . ? C33 C34 H34B 109.7 . . ? C35 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? C36 C35 C34 109.77(10) . . ? C36 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? C36 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C35 C36 C37 109.76(10) . . ? C35 C36 H36A 109.7 . . ? C37 C36 H36A 109.7 . . ? C35 C36 H36B 109.7 . . ? C37 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? C29' C28' C27 109.74(10) . . ? C29' C28' H28C 109.7 . . ? C27 C28' H28C 109.7 . . ? C29' C28' H28D 109.7 . . ? C27 C28' H28D 109.7 . . ? H28C C28' H28D 108.2 . . ? C28' C29' C30' 109.75(10) . . ? C28' C29' H29C 109.7 . . ? C30' C29' H29C 109.7 . . ? C28' C29' H29D 109.7 . . ? C30' C29' H29D 109.7 . . ? H29C C29' H29D 108.2 . . ? C31' C30' C29' 109.74(10) . . ? C31' C30' H30C 109.7 . . ? C29' C30' H30C 109.7 . . ? C31' C30' H30D 109.7 . . ? C29' C30' H30D 109.7 . . ? H30C C30' H30D 108.2 . . ? C30' C31' C32' 109.75(10) . . ? C30' C31' H31C 109.7 . . ? C32' C31' H31C 109.7 . . ? C30' C31' H31D 109.7 . . ? C32' C31' H31D 109.7 . . ? H31C C31' H31D 108.2 . . ? C31' C32' C33' 109.72(10) . . ? C31' C32' H32C 109.7 . . ? C33' C32' H32C 109.7 . . ? C31' C32' H32D 109.7 . . ? C33' C32' H32D 109.7 . . ? H32C C32' H32D 108.2 . . ? C34' C33' C32' 109.73(10) . . ? C34' C33' H33C 109.7 . . ? C32' C33' H33C 109.7 . . ? C34' C33' H33D 109.7 . . ? C32' C33' H33D 109.7 . . ? H33C C33' H33D 108.2 . . ? C35' C34' C33' 109.74(10) . . ? C35' C34' H34C 109.7 . . ? C33' C34' H34C 109.7 . . ? C35' C34' H34D 109.7 . . ? C33' C34' H34D 109.7 . . ? H34C C34' H34D 108.2 . . ? C34' C35' C36' 109.75(10) . . ? C34' C35' H35C 109.7 . . ? C36' C35' H35C 109.7 . . ? C34' C35' H35D 109.7 . . ? C36' C35' H35D 109.7 . . ? H35C C35' H35D 108.2 . . ? C35' C36' C37' 109.74(10) . . ? C35' C36' H36C 109.7 . . ? C37' C36' H36C 109.7 . . ? C35' C36' H36D 109.7 . . ? C37' C36' H36D 109.7 . . ? H36C C36' H36D 108.2 . . ? C36' C37' H37D 109.5 . . ? C36' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C36' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C63 O9 C62 116.6(8) . . ? O10 C63 O9 121.9(11) . . ? O10 C63 C64 122.7(10) . . ? O9 C63 C64 115.4(8) . . ? C65 C64 C63 111.5(6) . . ? C65 C64 H64A 109.3 . . ? C63 C64 H64A 109.3 . . ? C65 C64 H64B 109.3 . . ? C63 C64 H64B 109.3 . . ? H64A C64 H64B 108.0 . . ? C64 C65 C66 109.9(8) . . ? C64 C65 H65A 109.7 . . ? C66 C65 H65A 109.7 . . ? C64 C65 H65B 109.7 . . ? C66 C65 H65B 109.7 . . ? H65A C65 H65B 108.2 . . ? C65 C66 C67 109.8(5) . . ? C65 C66 H66A 109.7 . . ? C67 C66 H66A 109.7 . . ? C65 C66 H66B 109.7 . . ? C67 C66 H66B 109.7 . . ? H66A C66 H66B 108.2 . . ? C68 C67 C66 109.8(5) . . ? C68 C67 H67A 109.7 . . ? C66 C67 H67A 109.7 . . ? C68 C67 H67B 109.7 . . ? C66 C67 H67B 109.7 . . ? H67A C67 H67B 108.2 . . ? C67 C68 C69 109.8(5) . . ? C67 C68 H68A 109.7 . . ? C69 C68 H68A 109.7 . . ? C67 C68 H68B 109.7 . . ? C69 C68 H68B 109.7 . . ? H68A C68 H68B 108.2 . . ? C70 C69 C68 109.7(6) . . ? C70 C69 H69A 109.7 . . ? C68 C69 H69A 109.7 . . ? C70 C69 H69B 109.7 . . ? C68 C69 H69B 109.7 . . ? H69A C69 H69B 108.2 . . ? C71 C70 C69 109.8(6) . . ? C71 C70 H70A 109.7 . . ? C69 C70 H70A 109.7 . . ? C71 C70 H70B 109.7 . . ? C69 C70 H70B 109.7 . . ? H70A C70 H70B 108.2 . . ? C70 C71 C72 109.7(7) . . ? C70 C71 H71A 109.7 . . ? C72 C71 H71A 109.7 . . ? C70 C71 H71B 109.7 . . ? C72 C71 H71B 109.7 . . ? H71A C71 H71B 108.2 . . ? C73 C72 C71 109.7(7) . . ? C73 C72 H72A 109.7 . . ? C71 C72 H72A 109.7 . . ? C73 C72 H72B 109.7 . . ? C71 C72 H72B 109.7 . . ? H72A C72 H72B 108.2 . . ? C72 C73 C74 109.8(9) . . ? C72 C73 H73A 109.7 . . ? C74 C73 H73A 109.7 . . ? C72 C73 H73B 109.7 . . ? C74 C73 H73B 109.7 . . ? H73A C73 H73B 108.2 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C100 O15 C99 111.7(11) . . ? O16 C100 O15 126.9(14) . . ? O16 C100 C101 118.9(17) . . ? O15 C100 C101 114.1(13) . . ? C100 C101 C102 123.3(10) . . ? C100 C101 H10A 118.4 . . ? C102 C101 H10A 118.4 . . ? C103 C102 C101 109.7(7) . . ? C103 C102 H10B 109.7 . . ? C101 C102 H10B 109.7 . . ? C103 C102 H10C 109.7 . . ? C101 C102 H10C 109.7 . . ? H10B C102 H10C 108.2 . . ? C104 C103 C102 109.8(7) . . ? C104 C103 H10D 109.7 . . ? C102 C103 H10D 109.7 . . ? C104 C103 H10E 109.7 . . ? C102 C103 H10E 109.7 . . ? H10D C103 H10E 108.2 . . ? C103 C104 C105 109.8(7) . . ? C103 C104 H10F 109.7 . . ? C105 C104 H10F 109.7 . . ? C103 C104 H10G 109.7 . . ? C105 C104 H10G 109.7 . . ? H10F C104 H10G 108.2 . . ? C106 C105 C104 109.8(7) . . ? C106 C105 H10H 109.7 . . ? C104 C105 H10H 109.7 . . ? C106 C105 H10I 109.7 . . ? C104 C105 H10I 109.7 . . ? H10H C105 H10I 108.2 . . ? C105 C106 C107 109.8(7) . . ? C105 C106 H10J 109.7 . . ? C107 C106 H10J 109.7 . . ? C105 C106 H10K 109.7 . . ? C107 C106 H10K 109.7 . . ? H10J C106 H10K 108.2 . . ? C108 C107 C106 109.8(7) . . ? C108 C107 H10L 109.7 . . ? C106 C107 H10L 109.7 . . ? C108 C107 H10M 109.7 . . ? C106 C107 H10M 109.7 . . ? H10L C107 H10M 108.2 . . ? C107 C108 C109 109.8(7) . . ? C107 C108 H10N 109.7 . . ? C109 C108 H10N 109.7 . . ? C107 C108 H10O 109.7 . . ? C109 C108 H10O 109.7 . . ? H10N C108 H10O 108.2 . . ? C110 C109 C108 111.9(6) . . ? C110 C109 H10P 109.2 . . ? C108 C109 H10P 109.2 . . ? C110 C109 H10Q 109.2 . . ? C108 C109 H10Q 109.2 . . ? H10P C109 H10Q 107.9 . . ? C109 C110 C111 111.9(6) . . ? C109 C110 H11F 109.2 . . ? C111 C110 H11F 109.2 . . ? C109 C110 H11G 109.2 . . ? C111 C110 H11G 109.2 . . ? H11F C110 H11G 107.9 . . ? C110 C111 H11H 109.5 . . ? C110 C111 H11I 109.5 . . ? H11H C111 H11I 109.5 . . ? C110 C111 H11J 109.5 . . ? H11H C111 H11J 109.5 . . ? H11I C111 H11J 109.5 . . ? C137 O21 C136 119.60(13) . . ? O22 C137 O21 116.52(10) . . ? O22 C137 C138 125.13(10) . . ? O21 C137 C138 118.34(9) . . ? C137 C138 C139 110.45(10) . . ? C137 C138 H13G 109.6 . . ? C139 C138 H13G 109.6 . . ? C137 C138 H13H 109.6 . . ? C139 C138 H13H 109.6 . . ? H13G C138 H13H 108.1 . . ? C140 C139 C138 109.79(11) . . ? C140 C139 H13I 109.7 . . ? C138 C139 H13I 109.7 . . ? C140 C139 H13J 109.7 . . ? C138 C139 H13J 109.7 . . ? H13I C139 H13J 108.2 . . ? C139 C140 C141 109.81(11) . . ? C139 C140 H14A 109.7 . . ? C141 C140 H14A 109.7 . . ? C139 C140 H14B 109.7 . . ? C141 C140 H14B 109.7 . . ? H14A C140 H14B 108.2 . . ? C140 C141 C142 109.78(11) . . ? C140 C141 H14C 109.7 . . ? C142 C141 H14C 109.7 . . ? C140 C141 H14D 109.7 . . ? C142 C141 H14D 109.7 . . ? H14C C141 H14D 108.2 . . ? C143 C142 C141 109.75(10) . . ? C143 C142 H14E 109.7 . . ? C141 C142 H14E 109.7 . . ? C143 C142 H14F 109.7 . . ? C141 C142 H14F 109.7 . . ? H14E C142 H14F 108.2 . . ? C144 C143 C142 109.77(10) . . ? C144 C143 H14G 109.7 . . ? C142 C143 H14G 109.7 . . ? C144 C143 H14H 109.7 . . ? C142 C143 H14H 109.7 . . ? H14G C143 H14H 108.2 . . ? C143 C144 C145 109.76(10) . . ? C143 C144 H14I 109.7 . . ? C145 C144 H14I 109.7 . . ? C143 C144 H14J 109.7 . . ? C145 C144 H14J 109.7 . . ? H14I C144 H14J 108.2 . . ? C146 C145 C144 109.73(10) . . ? C146 C145 H14K 109.7 . . ? C144 C145 H14K 109.7 . . ? C146 C145 H14L 109.7 . . ? C144 C145 H14L 109.7 . . ? H14K C145 H14L 108.2 . . ? C147 C146 C145 109.76(10) . . ? C147 C146 H14M 109.7 . . ? C145 C146 H14M 109.7 . . ? C147 C146 H14N 109.7 . . ? C145 C146 H14N 109.7 . . ? H14M C146 H14N 108.2 . . ? C148 C147 C146 109.76(11) . . ? C148 C147 H14O 109.7 . . ? C146 C147 H14O 109.7 . . ? C148 C147 H14P 109.7 . . ? C146 C147 H14P 109.7 . . ? H14O C147 H14P 108.2 . . ? C147 C148 C74 117(2) . 2_455 ? C147 C148 H14Q 109.5 . . ? C74 C148 H14Q 47.0 2_455 . ? C147 C148 H14R 109.5 . . ? C74 C148 H14R 132.9 2_455 . ? H14Q C148 H14R 109.5 . . ? C147 C148 H14S 109.5 . . ? C74 C148 H14S 63.3 2_455 . ? H14Q C148 H14S 109.5 . . ? H14R C148 H14S 109.5 . . ? C237 O221 C136 119.55(13) . . ? O222 C237 O221 116.47(10) . . ? O222 C237 C238 125.23(10) . . ? O221 C237 C238 118.30(9) . . ? C237 C238 C239 110.53(10) . . ? C237 C238 H23A 109.5 . . ? C239 C238 H23A 109.5 . . ? C237 C238 H23B 109.5 . . ? C239 C238 H23B 109.5 . . ? H23A C238 H23B 108.1 . . ? C238 C239 C240 109.71(11) . . ? C238 C239 H23C 109.7 . . ? C240 C239 H23C 109.7 . . ? C238 C239 H23D 109.7 . . ? C240 C239 H23D 109.7 . . ? H23C C239 H23D 108.2 . . ? C239 C240 C241 109.69(10) . . ? C239 C240 H24A 109.7 . . ? C241 C240 H24A 109.7 . . ? C239 C240 H24B 109.7 . . ? C241 C240 H24B 109.7 . . ? H24A C240 H24B 108.2 . . ? C242 C241 C240 109.69(11) . . ? C242 C241 H24C 109.7 . . ? C240 C241 H24C 109.7 . . ? C242 C241 H24D 109.7 . . ? C240 C241 H24D 109.7 . . ? H24C C241 H24D 108.2 . . ? C243 C242 C241 109.72(11) . . ? C243 C242 H24E 109.7 . . ? C241 C242 H24E 109.7 . . ? C243 C242 H24F 109.7 . . ? C241 C242 H24F 109.7 . . ? H24E C242 H24F 108.2 . . ? C244 C243 C242 109.74(10) . . ? C244 C243 H24G 109.7 . . ? C242 C243 H24G 109.7 . . ? C244 C243 H24H 109.7 . . ? C242 C243 H24H 109.7 . . ? H24G C243 H24H 108.2 . . ? C245 C244 C243 109.75(10) . . ? C245 C244 H24I 109.7 . . ? C243 C244 H24I 109.7 . . ? C245 C244 H24J 109.7 . . ? C243 C244 H24J 109.7 . . ? H24I C244 H24J 108.2 . . ? C246 C245 C244 109.76(10) . . ? C246 C245 H24K 109.7 . . ? C244 C245 H24K 109.7 . . ? C246 C245 H24L 109.7 . . ? C244 C245 H24L 109.7 . . ? H24K C245 H24L 108.2 . . ? C245 C246 C247 109.77(11) . . ? C245 C246 H24M 109.7 . . ? C247 C246 H24M 109.7 . . ? C245 C246 H24N 109.7 . . ? C247 C246 H24N 109.7 . . ? H24M C246 H24N 108.2 . . ? C246 C247 C248 109.76(11) . . ? C246 C247 H24O 109.7 . . ? C248 C247 H24O 109.7 . . ? C246 C247 H24P 109.7 . . ? C248 C247 H24P 109.7 . . ? H24O C247 H24P 108.2 . . ? C247 C248 H24Q 109.5 . . ? C247 C248 H24R 109.5 . . ? H24Q C248 H24R 109.5 . . ? C247 C248 H24S 109.5 . . ? H24Q C248 H24S 109.5 . . ? H24R C248 H24S 109.5 . . ? C149 O25 Cu1 120.5(7) . . ? C149 N1 C152 122.0(10) . . ? C149 N1 C150 120.2(10) . . ? C152 N1 C150 117.7(9) . . ? O25 C149 N1 124.1(12) . . ? O25 C149 H14T 117.9 . . ? N1 C149 H14T 117.9 . . ? N1 C150 C151 112.2(10) . . ? N1 C150 H15B 109.2 . . ? C151 C150 H15B 109.2 . . ? N1 C150 H15C 109.2 . . ? C151 C150 H15C 109.2 . . ? H15B C150 H15C 107.9 . . ? C150 C151 H15D 109.5 . . ? C150 C151 H15E 109.5 . . ? H15D C151 H15E 109.5 . . ? C150 C151 H15F 109.5 . . ? H15D C151 H15F 109.5 . . ? H15E C151 H15F 109.5 . . ? N1 C152 C153 111.2(10) . . ? N1 C152 H15G 109.4 . . ? C153 C152 H15G 109.4 . . ? N1 C152 H15H 109.4 . . ? C153 C152 H15H 109.4 . . ? H15G C152 H15H 108.0 . . ? C152 C153 H15I 109.5 . . ? C152 C153 H15J 109.5 . . ? H15I C153 H15J 109.5 . . ? C152 C153 H15K 109.5 . . ? H15I C153 H15K 109.5 . . ? H15J C153 H15K 109.5 . . ? C164 O26 Cu2 117.3(6) . . ? C164 O26 H26A 121.6 . . ? Cu2 O26 H26A 121.1 . . ? O26 C164 H16K 109.5 . . ? O26 C164 H16L 109.5 . . ? H16K C164 H16L 109.5 . . ? O26 C164 H16M 109.5 . . ? H16K C164 H16M 109.5 . . ? H16L C164 H16M 109.5 . . ? C154 O27 Cu3 122.2(7) . . ? C154 N2 C157 123.2(9) . . ? C154 N2 C155 118.4(9) . . ? C157 N2 C155 118.4(8) . . ? O27 C154 N2 125.5(10) . . ? O27 C154 H15L 117.2 . . ? N2 C154 H15L 117.2 . . ? C156 C155 N2 112.4(9) . . ? C156 C155 H15M 109.1 . . ? N2 C155 H15M 109.1 . . ? C156 C155 H15N 109.1 . . ? N2 C155 H15N 109.1 . . ? H15M C155 H15N 107.9 . . ? C155 C156 H15O 109.5 . . ? C155 C156 H15P 109.5 . . ? H15O C156 H15P 109.5 . . ? C155 C156 H15Q 109.5 . . ? H15O C156 H15Q 109.5 . . ? H15P C156 H15Q 109.5 . . ? N2 C157 C158 116.9(9) . . ? N2 C157 H15R 108.1 . . ? C158 C157 H15R 108.1 . . ? N2 C157 H15S 108.1 . . ? C158 C157 H15S 108.1 . . ? H15R C157 H15S 107.3 . . ? C157 C158 H15T 109.5 . . ? C157 C158 H15U 109.5 . . ? H15T C158 H15U 109.5 . . ? C157 C158 H15V 109.5 . . ? H15T C158 H15V 109.5 . . ? H15U C158 H15V 109.5 . . ? C159 O28 Cu4 121.1(8) . . ? C159 N3 C160 118.8(10) . . ? C159 N3 C162 119.3(11) . . ? C160 N3 C162 121.5(10) . . ? O28 C159 N3 120.9(12) . . ? O28 C159 H15W 119.5 . . ? N3 C159 H15W 119.5 . . ? N3 C160 C161 111.0(11) . . ? N3 C160 H16A 109.4 . . ? C161 C160 H16A 109.4 . . ? N3 C160 H16B 109.4 . . ? C161 C160 H16B 109.4 . . ? H16A C160 H16B 108.0 . . ? C160 C161 H16C 109.5 . . ? C160 C161 H16D 109.5 . . ? H16C C161 H16D 109.5 . . ? C160 C161 H16E 109.5 . . ? H16C C161 H16E 109.5 . . ? H16D C161 H16E 109.5 . . ? N3 C162 C163 112.3(10) . . ? N3 C162 H16F 109.1 . . ? C163 C162 H16F 109.1 . . ? N3 C162 H16G 109.1 . . ? C163 C162 H16G 109.1 . . ? H16F C162 H16G 107.9 . . ? C162 C163 H16H 109.5 . . ? C162 C163 H16I 109.5 . . ? H16H C163 H16I 109.5 . . ? C162 C163 H16J 109.5 . . ? H16H C163 H16J 109.5 . . ? H16I C163 H16J 109.5 . . ? C165 N4 C168 123.1(9) . . ? C165 N4 C166 119.6(10) . . ? C168 N4 C166 117.2(9) . . ? O29 C165 N4 124.7(10) . . ? O29 C165 H16N 117.6 . . ? N4 C165 H16N 117.6 . . ? N4 C166 C167 112.0(9) . . ? N4 C166 H16O 109.2 . . ? C167 C166 H16O 109.2 . . ? N4 C166 H16P 109.2 . . ? C167 C166 H16P 109.2 . . ? H16O C166 H16P 107.9 . . ? C166 C167 H16Q 109.5 . . ? C166 C167 H16R 109.5 . . ? H16Q C167 H16R 109.5 . . ? C166 C167 H16S 109.5 . . ? H16Q C167 H16S 109.5 . . ? H16R C167 H16S 109.5 . . ? N4 C168 C169 110.2(9) . . ? N4 C168 H16T 109.6 . . ? C169 C168 H16T 109.6 . . ? N4 C168 H16U 109.6 . . ? C169 C168 H16U 109.6 . . ? H16T C168 H16U 108.1 . . ? C168 C169 H16V 109.5 . . ? C168 C169 H16W 109.5 . . ? H16V C169 H16W 109.5 . . ? C168 C169 H16X 109.5 . . ? H16V C169 H16X 109.5 . . ? H16W C169 H16X 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.712 _refine_diff_density_min -2.096 _refine_diff_density_rms 0.117 _publ_section_references ; Bruker (2001). SAINTP+ for NT. Data Reduction and Correction Program v. 6.2, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005). APEX2 software package. Bruker Molecular Analysis Research Tool, v. 2008.4 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SADABS-2008/1, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2008). SHELXTL 2008/4, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 47 13 ' ' 2 0.397 0.037 0.470 14 9 ' ' 3 0.668 0.168 0.303 37 10 ' ' 4 0.168 0.332 0.803 37 10 ' ' 5 0.897 0.463 0.970 14 9 ' ' 6 0.000 0.500 0.500 47 13 ' ' 7 0.103 0.537 0.030 14 9 ' ' 8 0.832 0.668 0.197 38 10 ' ' 9 0.332 0.832 0.697 37 10 ' ' 10 0.603 0.963 0.530 14 9 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT220_MOP4 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.11 Ratio RESPONSE:C11H23COO-ester groups are highly disordered and carbon and oxygen atoms in these groups have very high values Ueq parameters, on the other hand the core of the MOP is ordered, hence atoms there have low Ueq values. ; _vrf_PLAT410_MOP4 ; PROBLEM: Short Intra H...H Contact H14K .. H74B .. 1.50 Ang. RESPONSE:Since the alkane chains in the structure are highly disordered it is very problematic to find correct positions of hydrogen atoms. ; _vrf_PLAT411_MOP4 ; PROBLEM: Short Inter H...H Contact H66A .. H30D .. 1.72 Ang. RESPONSE:Since the alkane chains in the structure are highly disordered it is very problematic to find correct positions of hydrogen atoms. ; _vrf_PLAT413_MOP4 ; PROBLEM: Short Inter XH3 .. XHn H18A .. H24D .. 1.82 Ang. RESPONSE:Since the alkane chains in the structure are highly disordered it is very problematic to find correct positions of hydrogen atoms. Even refinement using AFIX 137 do not give any results. ; # end Validation Reply Form