# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Myoung Soo Lah' _publ_contact_author_email MSLAH@HANYANG.AC.KR _publ_section_title ; Edge-directed [(M2)2L4] Tetragonal Metal-Organic Polyhedra Decorated Using a Square Paddle-wheel Secondary Building Unit ; loop_ _publ_author_name 'Myoung Soo Lah' 'Kwi Nam Han' 'Xinfang Liu' 'Minhak Oh' 'M. Jaya Prakash' 'Gi Hun Seong' # Attachment 'mslah_rev2.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 744143' #TrackingRef 'mslah_rev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H90 Cu4 N6 O22' _chemical_formula_weight 2150.08 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 17.475(4) _cell_length_b 18.723(4) _cell_length_c 18.789(4) _cell_angle_alpha 82.05(3) _cell_angle_beta 62.82(3) _cell_angle_gamma 87.67(3) _cell_volume 5414.3(19) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 227040 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 31.81 _exptl_crystal_description block _exptl_crystal_colour greenish-blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7853 _exptl_absorpt_correction_T_max 0.9201 _exptl_absorpt_process_details HKL2000-Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.72999 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Fixed gap multipole wiggler beamline' _diffrn_radiation_monochromator 'Pt coated Si double crystal' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67393 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 31.81 _reflns_number_total 33839 _reflns_number_gt 27707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.1704P)^2^+2.6493P] 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 0.0143(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 33839 _refine_ls_number_parameters 1212 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2534 _refine_ls_wR_factor_gt 0.2427 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.002 _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 0.454841(18) 0.203503(17) 0.539937(16) 0.02583(9) Uani 1 1 d . . . Cu2 Cu 0.377366(17) 0.210467(15) 0.695486(15) 0.02135(8) Uani 1 1 d . . . Cu3 Cu 0.028579(18) 0.210986(17) 1.393650(16) 0.02525(9) Uani 1 1 d . . . Cu4 Cu 0.107534(17) 0.212641(15) 1.236341(15) 0.02168(8) Uani 1 1 d . . . O1A O 0.43125(13) 0.30712(11) 0.52674(11) 0.0342(4) Uani 1 1 d . . . O2A O 0.34505(12) 0.30565(10) 0.66015(11) 0.0307(4) Uani 1 1 d . . . O3A O 0.00743(12) 0.31381(11) 1.36757(11) 0.0328(4) Uani 1 1 d . . . O4A O 0.06062(13) 0.30900(10) 1.23392(11) 0.0311(4) Uani 1 1 d . . . C1A C 0.38151(17) 0.33638(14) 0.58804(16) 0.0308(5) Uani 1 1 d . . . C2A C 0.3657(2) 0.41532(15) 0.5745(2) 0.0406(6) Uani 1 1 d . . . C3A C 0.3092(2) 0.44903(15) 0.6389(2) 0.0427(7) Uani 1 1 d . . . H3A H 0.2784 0.4218 0.6907 0.051 Uiso 1 1 calc R . . C4A C 0.2973(3) 0.52345(17) 0.6278(3) 0.0557(9) Uani 1 1 d . . . C5A C 0.3451(4) 0.5625(2) 0.5497(3) 0.0788(15) Uani 1 1 d . . . H5A H 0.3393 0.6133 0.5416 0.095 Uiso 1 1 calc R . . C6A C 0.3990(4) 0.5282(2) 0.4865(3) 0.0860(17) Uani 1 1 d . . . H6A H 0.4283 0.5553 0.4344 0.103 Uiso 1 1 calc R . . C7A C 0.4125(3) 0.4544(2) 0.4962(3) 0.0614(10) Uani 1 1 d . . . H7A H 0.4514 0.4311 0.4521 0.074 Uiso 1 1 calc R . . C8A C 0.2378(3) 0.55837(17) 0.6968(3) 0.0626(12) Uani 1 1 d . . . C9A C 0.1890(3) 0.58564(16) 0.7552(3) 0.0599(11) Uani 1 1 d . . . C10A C 0.1303(3) 0.61871(16) 0.8240(3) 0.0566(10) Uani 1 1 d . . . C11A C 0.1060(3) 0.58442(17) 0.9018(3) 0.0596(11) Uani 1 1 d . . . H11A H 0.1297 0.5392 0.9096 0.071 Uiso 1 1 calc R . . C12A C 0.0467(4) 0.61566(18) 0.9694(3) 0.0693(13) Uani 1 1 d . . . C13A C 0.0110(5) 0.6823(2) 0.9569(3) 0.100(2) Uani 1 1 d . . . H13A H -0.0301 0.7036 1.0018 0.120 Uiso 1 1 calc R . . C14A C 0.0357(5) 0.7164(2) 0.8795(3) 0.097(2) Uani 1 1 d . . . H14A H 0.0117 0.7614 0.8714 0.116 Uiso 1 1 calc R . . C15A C 0.0957(3) 0.68561(19) 0.8129(3) 0.0641(12) Uani 1 1 d . . . H15A H 0.1130 0.7101 0.7599 0.077 Uiso 1 1 calc R . . C16A C 0.0224(3) 0.58105(18) 1.0491(3) 0.0694(13) Uani 1 1 d . . . C17A C 0.0050(3) 0.55326(17) 1.1165(3) 0.0594(11) Uani 1 1 d . . . C18A C -0.0112(2) 0.52023(16) 1.1951(3) 0.0497(8) Uani 1 1 d . . . C19A C 0.01498(19) 0.44972(15) 1.2067(2) 0.0388(6) Uani 1 1 d . . . H19A H 0.0444 0.4241 1.1618 0.047 Uiso 1 1 calc R . . C20A C -0.00204(18) 0.41689(15) 1.28419(18) 0.0353(5) Uani 1 1 d . . . C21A C -0.0438(2) 0.45539(18) 1.3495(2) 0.0484(7) Uani 1 1 d . . . H21A H -0.0552 0.4338 1.4023 0.058 Uiso 1 1 calc R . . C22A C -0.0688(3) 0.5258(2) 1.3369(3) 0.0649(11) Uani 1 1 d . . . H22A H -0.0970 0.5520 1.3815 0.078 Uiso 1 1 calc R . . C23A C -0.0537(3) 0.55742(19) 1.2625(3) 0.0630(11) Uani 1 1 d . . . H23A H -0.0720 0.6052 1.2555 0.076 Uiso 1 1 calc R . . C24A C 0.02391(16) 0.34093(14) 1.29622(15) 0.0284(4) Uani 1 1 d . . . O1B O 0.55948(12) 0.23098(12) 0.54540(11) 0.0346(4) Uani 1 1 d . . . O2B O 0.48851(11) 0.25354(10) 0.67485(11) 0.0275(3) Uani 1 1 d . . . O3B O 0.14241(11) 0.23887(12) 1.37985(11) 0.0338(4) Uani 1 1 d . . . O4B O 0.20507(11) 0.25588(10) 1.24371(10) 0.0276(3) Uani 1 1 d . . . C1B C 0.55572(15) 0.25135(14) 0.60855(14) 0.0274(4) Uani 1 1 d . . . C2B C 0.63954(15) 0.27439(13) 0.60369(14) 0.0259(4) Uani 1 1 d . . . C3B C 0.64247(15) 0.29096(13) 0.67229(14) 0.0266(4) Uani 1 1 d . . . H3B H 0.5912 0.2882 0.7220 0.032 Uiso 1 1 calc R . . C4B C 0.72064(15) 0.31169(14) 0.66862(14) 0.0285(4) Uani 1 1 d . . . C5B C 0.79586(16) 0.31512(15) 0.59492(16) 0.0320(5) Uani 1 1 d . . . H5B H 0.8490 0.3295 0.5917 0.038 Uiso 1 1 calc R . . C6B C 0.79319(16) 0.29763(15) 0.52640(15) 0.0317(5) Uani 1 1 d . . . H6B H 0.8444 0.2996 0.4768 0.038 Uiso 1 1 calc R . . C7B C 0.71551(16) 0.27729(14) 0.53065(15) 0.0284(4) Uani 1 1 d . . . H7B H 0.7138 0.2653 0.4839 0.034 Uiso 1 1 calc R . . C8B C 0.72290(16) 0.32864(15) 0.73946(16) 0.0326(5) Uani 1 1 d . . . C9B C 0.72248(17) 0.34363(16) 0.79996(16) 0.0342(5) Uani 1 1 d . . . C10B C 0.72025(17) 0.36418(16) 0.87125(16) 0.0342(5) Uani 1 1 d . . . C11B C 0.64873(17) 0.34583(15) 0.94620(16) 0.0327(5) Uani 1 1 d . . . H11B H 0.6023 0.3184 0.9497 0.039 Uiso 1 1 calc R . . C12B C 0.64504(18) 0.36747(17) 1.01596(16) 0.0369(6) Uani 1 1 d . . . C13B C 0.7133(2) 0.4084(2) 1.01000(19) 0.0530(9) Uani 1 1 d . . . H13B H 0.7113 0.4232 1.0572 0.064 Uiso 1 1 calc R . . C14B C 0.7830(2) 0.4273(3) 0.9367(2) 0.0614(11) Uani 1 1 d . . . H14B H 0.8280 0.4565 0.9333 0.074 Uiso 1 1 calc R . . C15B C 0.7887(2) 0.4044(2) 0.86698(18) 0.0479(8) Uani 1 1 d . . . H15B H 0.8387 0.4158 0.8169 0.057 Uiso 1 1 calc R . . C16B C 0.57199(19) 0.34844(17) 1.09265(17) 0.0384(6) Uani 1 1 d . . . C17B C 0.51173(18) 0.33261(16) 1.15756(16) 0.0355(5) Uani 1 1 d . . . C18B C 0.43692(17) 0.31556(14) 1.23384(15) 0.0301(5) Uani 1 1 d . . . C19B C 0.36025(16) 0.29434(13) 1.23589(14) 0.0274(4) Uani 1 1 d . . . H19B H 0.3581 0.2904 1.1870 0.033 Uiso 1 1 calc R . . C20B C 0.28677(15) 0.27891(13) 1.30958(13) 0.0255(4) Uani 1 1 d . . . C21B C 0.29040(17) 0.28379(14) 1.38191(14) 0.0285(4) Uani 1 1 d . . . H21B H 0.2404 0.2733 1.4322 0.034 Uiso 1 1 calc R . . C22B C 0.36710(18) 0.30404(15) 1.38014(15) 0.0319(5) Uani 1 1 d . . . H22B H 0.3697 0.3065 1.4291 0.038 Uiso 1 1 calc R . . C23B C 0.43993(18) 0.32068(15) 1.30639(16) 0.0335(5) Uani 1 1 d . . . H23B H 0.4919 0.3356 1.3051 0.040 Uiso 1 1 calc R . . C24B C 0.20514(15) 0.25623(13) 1.31141(14) 0.0266(4) Uani 1 1 d . . . O1C O 0.47056(13) 0.10380(11) 0.57846(11) 0.0324(4) Uani 1 1 d . . . O2C O 0.42532(11) 0.11646(9) 0.70932(10) 0.0257(3) Uani 1 1 d . . . O3C O 0.06594(12) 0.11008(11) 1.39057(10) 0.0305(4) Uani 1 1 d . . . O4C O 0.15096(11) 0.11824(9) 1.25608(9) 0.0255(3) Uani 1 1 d . . . C1C C 0.46466(14) 0.08395(13) 0.64818(13) 0.0251(4) Uani 1 1 d . . . C2C C 0.51124(14) 0.01674(13) 0.65714(13) 0.0245(4) Uani 1 1 d . . . C3C C 0.51517(14) -0.00527(13) 0.72966(13) 0.0250(4) Uani 1 1 d . . . H3C H 0.4856 0.0207 0.7743 0.030 Uiso 1 1 calc R . . C4C C 0.56259(15) -0.06541(13) 0.73630(14) 0.0267(4) Uani 1 1 d . . . C5C C 0.60725(16) -0.10248(14) 0.66958(16) 0.0313(5) Uani 1 1 d . . . H5C H 0.6414 -0.1423 0.6732 0.038 Uiso 1 1 calc R . . C6C C 0.60185(16) -0.08145(14) 0.59839(15) 0.0310(5) Uani 1 1 d . . . H6C H 0.6312 -0.1075 0.5539 0.037 Uiso 1 1 calc R . . C7C C 0.55365(15) -0.02238(14) 0.59184(14) 0.0279(4) Uani 1 1 d . . . H7C H 0.5494 -0.0085 0.5432 0.034 Uiso 1 1 calc R . . C8C C 0.56299(16) -0.09107(13) 0.81153(15) 0.0294(4) Uani 1 1 d . . . C9C C 0.56093(16) -0.11489(14) 0.87511(15) 0.0296(5) Uani 1 1 d . . . C10C C 0.55411(15) -0.14140(13) 0.95322(15) 0.0278(4) Uani 1 1 d . . . C11C C 0.48963(16) -0.11523(14) 1.02173(15) 0.0284(4) Uani 1 1 d . . . H11C H 0.4515 -0.0801 1.0157 0.034 Uiso 1 1 calc R . . C12C C 0.48094(15) -0.14038(13) 1.09868(15) 0.0289(4) Uani 1 1 d . . . C13C C 0.53865(17) -0.19092(15) 1.10787(15) 0.0344(5) Uani 1 1 d . . . H13C H 0.5345 -0.2069 1.1598 0.041 Uiso 1 1 calc R . . C14C C 0.60207(18) -0.21714(16) 1.03969(16) 0.0370(6) Uani 1 1 d . . . H14C H 0.6405 -0.2520 1.0457 0.044 Uiso 1 1 calc R . . C15C C 0.61021(17) -0.19320(14) 0.96279(16) 0.0325(5) Uani 1 1 d . . . H15C H 0.6536 -0.2119 0.9171 0.039 Uiso 1 1 calc R . . C16C C 0.41200(16) -0.11421(14) 1.16735(15) 0.0306(5) Uani 1 1 d . . . C17C C 0.35251(16) -0.09211(13) 1.22280(15) 0.0292(4) Uani 1 1 d . . . C18C C 0.27914(15) -0.06708(13) 1.28904(13) 0.0261(4) Uani 1 1 d . . . C19C C 0.23807(14) -0.00437(12) 1.27623(13) 0.0241(4) Uani 1 1 d . . . H19C H 0.2596 0.0227 1.2240 0.029 Uiso 1 1 calc R . . C20C C 0.16536(14) 0.01826(12) 1.34058(13) 0.0235(4) Uani 1 1 d . . . C21C C 0.13282(15) -0.02224(14) 1.41712(13) 0.0273(4) Uani 1 1 d . . . H21C H 0.0825 -0.0075 1.4606 0.033 Uiso 1 1 calc R . . C22C C 0.17418(17) -0.08408(15) 1.42959(14) 0.0325(5) Uani 1 1 d . . . H22C H 0.1521 -0.1115 1.4817 0.039 Uiso 1 1 calc R . . C23C C 0.24750(17) -0.10593(14) 1.36637(15) 0.0321(5) Uani 1 1 d . . . H23C H 0.2764 -0.1475 1.3757 0.039 Uiso 1 1 calc R . . C24C C 0.12395(14) 0.08702(13) 1.32783(13) 0.0242(4) Uani 1 1 d . . . O1D O 0.34018(11) 0.17867(10) 0.55555(10) 0.0261(3) Uani 1 1 d . . . O2D O 0.28083(11) 0.16328(9) 0.69168(9) 0.0249(3) Uani 1 1 d . . . O3D O -0.07398(11) 0.18315(10) 1.38636(10) 0.0258(3) Uani 1 1 d . . . O4D O -0.00113(10) 0.16775(10) 1.25472(9) 0.0260(3) Uani 1 1 d . . . C1D C 0.27988(15) 0.15888(12) 0.62537(13) 0.0238(4) Uani 1 1 d . . . C2D C 0.20023(14) 0.12728(12) 0.62936(13) 0.0237(4) Uani 1 1 d . . . C3D C 0.13535(15) 0.09642(12) 0.70306(13) 0.0244(4) Uani 1 1 d . . . H3D H 0.1412 0.0958 0.7510 0.029 Uiso 1 1 calc R . . C4D C 0.06148(15) 0.06624(13) 0.70670(14) 0.0267(4) Uani 1 1 d . . . C5D C 0.05404(16) 0.06649(14) 0.63532(15) 0.0297(5) Uani 1 1 d . . . H5D H 0.0049 0.0447 0.6373 0.036 Uiso 1 1 calc R . . C6D C 0.11792(16) 0.09838(15) 0.56213(15) 0.0312(5) Uani 1 1 d . . . H6D H 0.1119 0.0994 0.5142 0.037 Uiso 1 1 calc R . . C7D C 0.19051(15) 0.12878(14) 0.55892(14) 0.0269(4) Uani 1 1 d . . . H7D H 0.2341 0.1508 0.5087 0.032 Uiso 1 1 calc R . . C8D C -0.00779(16) 0.03831(14) 0.78357(15) 0.0307(5) Uani 1 1 d . . . C9D C -0.06773(18) 0.01899(15) 0.84719(16) 0.0335(5) Uani 1 1 d . . . C10D C -0.14182(17) 0.00043(15) 0.92399(15) 0.0321(5) Uani 1 1 d . . . C11D C -0.14305(17) 0.01939(14) 0.99368(15) 0.0311(5) Uani 1 1 d . . . H11D H -0.0939 0.0424 0.9904 0.037 Uiso 1 1 calc R . . C12D C -0.21644(18) 0.00475(15) 1.06882(15) 0.0334(5) Uani 1 1 d . . . C13D C -0.28995(18) -0.02734(17) 1.07275(17) 0.0384(6) Uani 1 1 d . . . H13D H -0.3403 -0.0365 1.1229 0.046 Uiso 1 1 calc R . . C14D C -0.28857(19) -0.04556(18) 1.00308(17) 0.0403(6) Uani 1 1 d . . . H14D H -0.3385 -0.0667 1.0058 0.048 Uiso 1 1 calc R . . C15D C -0.21505(18) -0.03330(17) 0.92928(16) 0.0377(6) Uani 1 1 d . . . H15D H -0.2143 -0.0477 0.8824 0.045 Uiso 1 1 calc R . . C16D C -0.21702(17) 0.02529(15) 1.13959(15) 0.0329(5) Uani 1 1 d . . . C17D C -0.21762(17) 0.04460(14) 1.19828(16) 0.0320(5) Uani 1 1 d . . . C18D C -0.21926(16) 0.07091(13) 1.26739(14) 0.0277(4) Uani 1 1 d . . . C19D C -0.14586(15) 0.10235(13) 1.26188(13) 0.0257(4) Uani 1 1 d . . . H19D H -0.0939 0.1050 1.2128 0.031 Uiso 1 1 calc R . . C20D C -0.14792(15) 0.13009(12) 1.32802(13) 0.0245(4) Uani 1 1 d . . . C21D C -0.22526(16) 0.12686(14) 1.39985(14) 0.0283(4) Uani 1 1 d . . . H21D H -0.2274 0.1463 1.4448 0.034 Uiso 1 1 calc R . . C22D C -0.29851(17) 0.09533(16) 1.40546(15) 0.0343(5) Uani 1 1 d . . . H22D H -0.3505 0.0928 1.4544 0.041 Uiso 1 1 calc R . . C23D C -0.29613(16) 0.06740(15) 1.33975(15) 0.0321(5) Uani 1 1 d . . . H23D H -0.3465 0.0459 1.3438 0.038 Uiso 1 1 calc R . . C24D C -0.06824(14) 0.16254(13) 1.32270(13) 0.0241(4) Uani 1 1 d . . . O1L O 0.52086(12) 0.19443(12) 0.41440(11) 0.0345(4) Uani 1 1 d D . . N1L N 0.62453(17) 0.22902(14) 0.28833(14) 0.0423(6) Uani 1 1 d D . . C1L C 0.58313(18) 0.23183(16) 0.36741(15) 0.0374(6) Uani 1 1 d D . . H1L H 0.6038 0.2655 0.3885 0.045 Uiso 1 1 calc R . . C2L C 0.7036(4) 0.2690(3) 0.2386(4) 0.0890(15) Uiso 1 1 d D . . H2L1 H 0.7273 0.2840 0.2727 0.134 Uiso 1 1 calc R . . H2L2 H 0.6928 0.3118 0.2084 0.134 Uiso 1 1 calc R . . H2L3 H 0.7449 0.2386 0.2007 0.134 Uiso 1 1 calc R . . C3L C 0.59902(18) 0.17878(16) 0.25116(15) 0.0351(5) Uani 1 1 d D . . H3L1 H 0.5521 0.1473 0.2930 0.053 Uiso 1 1 calc R . . H3L2 H 0.6481 0.1495 0.2212 0.053 Uiso 1 1 calc R . . H3L3 H 0.5795 0.2054 0.2140 0.053 Uiso 1 1 calc R . . O2L O 0.30027(14) 0.22695(11) 0.82215(11) 0.0374(4) Uani 1 1 d . . . N2L N 0.15448(18) 0.20460(15) 0.87179(16) 0.0473(6) Uani 1 1 d . . . C4L C 0.2313(2) 0.19460(17) 0.87002(18) 0.0454(7) Uani 1 1 d . . . H4L H 0.2336 0.1586 0.9099 0.054 Uiso 1 1 calc R . . C5L C 0.1424(2) 0.25686(19) 0.8138(2) 0.0466(7) Uani 1 1 d . . . H5L1 H 0.1976 0.2811 0.7760 0.070 Uiso 1 1 calc R . . H5L2 H 0.1012 0.2927 0.8421 0.070 Uiso 1 1 calc R . . H5L3 H 0.1202 0.2323 0.7839 0.070 Uiso 1 1 calc R . . C6L C 0.0802(3) 0.1583(2) 0.9271(3) 0.0700(12) Uani 1 1 d . . . H6L1 H 0.0727 0.1212 0.8986 0.105 Uiso 1 1 calc R . . H6L2 H 0.0285 0.1874 0.9474 0.105 Uiso 1 1 calc R . . H6L3 H 0.0895 0.1351 0.9725 0.105 Uiso 1 1 calc R . . O3L O -0.02938(12) 0.20948(12) 1.52093(10) 0.0339(4) Uani 1 1 d . . . N3L N -0.03073(16) 0.23701(14) 1.63512(13) 0.0356(5) Uani 1 1 d . . . C7L C 0.00258(18) 0.24121(15) 1.55520(14) 0.0328(5) Uani 1 1 d . . . H7L H 0.0534 0.2699 1.5228 0.039 Uiso 1 1 calc R . . C8L C -0.1061(2) 0.19166(19) 1.68858(15) 0.0419(7) Uani 1 1 d . . . H8L1 H -0.1270 0.1692 1.6564 0.063 Uiso 1 1 calc R . . H8L2 H -0.1513 0.2212 1.7241 0.063 Uiso 1 1 calc R . . H8L3 H -0.0907 0.1541 1.7213 0.063 Uiso 1 1 calc R . . C9L C 0.0110(3) 0.2746(2) 1.6719(2) 0.0558(9) Uani 1 1 d . . . H9L1 H 0.0603 0.3034 1.6294 0.084 Uiso 1 1 calc R . . H9L2 H 0.0308 0.2393 1.7030 0.084 Uiso 1 1 calc R . . H9L3 H -0.0302 0.3064 1.7078 0.084 Uiso 1 1 calc R . . O4L O 0.16984(13) 0.22114(11) 1.10498(10) 0.0345(4) Uani 1 1 d D . . N4L N 0.1962(4) 0.3363(4) 1.0343(4) 0.1148(18) Uiso 1 1 d D . . C10L C 0.1666(4) 0.2675(3) 1.0538(3) 0.0914(17) Uani 1 1 d D . . H10L H 0.1397 0.2532 1.0239 0.110 Uiso 1 1 calc R . . C11L C 0.1800(9) 0.3865(7) 0.9737(7) 0.199(5) Uiso 1 1 d D . . H11E H 0.1299 0.3688 0.9703 0.298 Uiso 1 1 calc R . . H11F H 0.2306 0.3887 0.9207 0.298 Uiso 1 1 calc R . . H11G H 0.1689 0.4348 0.9903 0.298 Uiso 1 1 calc R . . C12L C 0.2562(5) 0.3545(4) 1.0539(4) 0.112(2) Uiso 1 1 d D . . H12A H 0.2702 0.4062 1.0367 0.169 Uiso 1 1 calc R . . H12B H 0.3080 0.3268 1.0268 0.169 Uiso 1 1 calc R . . H12C H 0.2347 0.3439 1.1125 0.169 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 0.02403(15) 0.03647(17) 0.01649(14) -0.00285(10) -0.00918(11) 0.00290(11) Cu2 0.02245(14) 0.02386(14) 0.01774(13) -0.00355(9) -0.00930(10) 0.00479(10) Cu3 0.02236(14) 0.03790(17) 0.01556(13) -0.00693(10) -0.00829(10) 0.00717(11) Cu4 0.02224(14) 0.02784(15) 0.01473(13) -0.00312(9) -0.00863(10) 0.00674(10) O1A 0.0382(10) 0.0370(10) 0.0292(8) 0.0034(7) -0.0189(8) -0.0033(8) O2A 0.0319(8) 0.0263(8) 0.0333(9) 0.0005(6) -0.0160(7) 0.0050(6) O3A 0.0322(9) 0.0381(10) 0.0284(8) -0.0109(7) -0.0127(7) 0.0056(7) O4A 0.0387(9) 0.0314(9) 0.0273(8) -0.0071(6) -0.0188(7) 0.0135(7) C1A 0.0332(11) 0.0286(11) 0.0372(12) 0.0033(9) -0.0236(10) -0.0010(9) C2A 0.0531(16) 0.0279(12) 0.0548(17) 0.0063(11) -0.0397(15) -0.0013(11) C3A 0.0406(14) 0.0269(12) 0.070(2) 0.0028(12) -0.0354(15) 0.0021(10) C4A 0.066(2) 0.0268(13) 0.097(3) -0.0001(15) -0.059(2) 0.0070(13) C5A 0.126(4) 0.0294(16) 0.101(4) 0.009(2) -0.075(3) 0.009(2) C6A 0.145(5) 0.041(2) 0.083(3) 0.020(2) -0.068(4) -0.008(3) C7A 0.093(3) 0.0410(17) 0.059(2) 0.0118(15) -0.046(2) -0.0087(18) C8A 0.065(2) 0.0234(13) 0.130(4) -0.0091(18) -0.072(3) 0.0108(14) C9A 0.059(2) 0.0231(13) 0.129(4) -0.0143(17) -0.070(2) 0.0114(13) C10A 0.071(2) 0.0258(13) 0.114(3) -0.0138(16) -0.077(2) 0.0113(13) C11A 0.075(2) 0.0233(12) 0.121(3) -0.0051(16) -0.080(3) 0.0066(14) C12A 0.123(4) 0.0300(15) 0.114(3) -0.0150(18) -0.104(3) 0.0210(19) C13A 0.213(7) 0.051(2) 0.096(3) -0.033(2) -0.122(5) 0.066(3) C14A 0.207(7) 0.046(2) 0.103(4) -0.034(2) -0.125(4) 0.065(3) C15A 0.109(3) 0.0350(16) 0.098(3) -0.0229(17) -0.087(3) 0.0283(18) C16A 0.114(4) 0.0299(15) 0.117(4) -0.0057(18) -0.099(3) 0.0132(18) C17A 0.080(2) 0.0276(13) 0.109(3) -0.0076(16) -0.078(3) 0.0107(15) C18A 0.0556(18) 0.0294(13) 0.089(3) -0.0108(14) -0.0540(19) 0.0075(12) C19A 0.0410(14) 0.0301(12) 0.0585(17) -0.0099(11) -0.0337(13) 0.0084(10) C20A 0.0342(12) 0.0306(12) 0.0488(15) -0.0139(10) -0.0238(11) 0.0091(9) C21A 0.0536(18) 0.0391(16) 0.0574(19) -0.0217(14) -0.0263(16) 0.0114(13) C22A 0.079(3) 0.0399(18) 0.086(3) -0.0358(19) -0.041(2) 0.0206(18) C23A 0.072(2) 0.0307(15) 0.113(4) -0.0270(19) -0.061(3) 0.0174(15) C24A 0.0270(10) 0.0317(11) 0.0308(11) -0.0096(9) -0.0158(9) 0.0075(8) O1B 0.0241(8) 0.0561(12) 0.0252(8) -0.0105(8) -0.0113(7) 0.0026(8) O2B 0.0205(7) 0.0334(9) 0.0282(8) -0.0070(6) -0.0099(6) 0.0013(6) O3B 0.0230(8) 0.0575(12) 0.0215(8) -0.0064(7) -0.0104(6) 0.0012(8) O4B 0.0283(8) 0.0356(9) 0.0225(7) -0.0005(6) -0.0155(6) 0.0003(7) C1B 0.0257(10) 0.0310(11) 0.0261(10) -0.0036(8) -0.0128(8) 0.0057(8) C2B 0.0236(9) 0.0288(11) 0.0244(10) -0.0018(8) -0.0110(8) 0.0050(8) C3B 0.0243(10) 0.0299(11) 0.0244(10) -0.0023(8) -0.0107(8) 0.0032(8) C4B 0.0265(10) 0.0310(11) 0.0270(10) -0.0017(8) -0.0120(9) 0.0032(8) C5B 0.0238(10) 0.0375(13) 0.0335(12) -0.0031(9) -0.0129(9) 0.0047(9) C6B 0.0229(10) 0.0396(13) 0.0256(10) -0.0012(9) -0.0062(8) 0.0048(9) C7B 0.0269(10) 0.0319(11) 0.0239(10) -0.0019(8) -0.0103(8) 0.0060(9) C8B 0.0275(11) 0.0392(13) 0.0313(11) -0.0032(9) -0.0142(9) 0.0028(9) C9B 0.0285(11) 0.0413(14) 0.0314(12) -0.0015(10) -0.0132(9) -0.0002(10) C10B 0.0307(11) 0.0426(14) 0.0307(12) -0.0014(10) -0.0160(10) -0.0006(10) C11B 0.0305(11) 0.0370(13) 0.0312(11) -0.0004(9) -0.0155(10) -0.0026(9) C12B 0.0356(13) 0.0457(15) 0.0287(11) 0.0020(10) -0.0152(10) -0.0070(11) C13B 0.0490(17) 0.081(2) 0.0318(13) -0.0027(14) -0.0199(13) -0.0248(17) C14B 0.0475(17) 0.102(3) 0.0354(15) -0.0010(16) -0.0189(14) -0.035(2) C15B 0.0326(13) 0.080(2) 0.0307(13) -0.0014(13) -0.0142(11) -0.0134(14) C16B 0.0385(13) 0.0436(15) 0.0327(12) -0.0004(10) -0.0167(11) -0.0061(11) C17B 0.0364(13) 0.0407(14) 0.0306(12) -0.0010(10) -0.0169(10) -0.0043(10) C18B 0.0327(11) 0.0307(11) 0.0272(11) -0.0010(8) -0.0145(9) -0.0011(9) C19B 0.0319(11) 0.0292(11) 0.0228(10) -0.0019(8) -0.0145(9) 0.0025(9) C20B 0.0300(10) 0.0278(10) 0.0210(9) -0.0026(7) -0.0141(8) 0.0048(8) C21B 0.0339(11) 0.0312(11) 0.0224(10) -0.0037(8) -0.0151(9) 0.0055(9) C22B 0.0379(12) 0.0377(13) 0.0249(10) -0.0056(9) -0.0182(10) 0.0018(10) C23B 0.0353(12) 0.0391(13) 0.0290(11) -0.0041(9) -0.0171(10) -0.0019(10) C24B 0.0276(10) 0.0316(11) 0.0237(10) -0.0054(8) -0.0144(8) 0.0081(8) O1C 0.0372(9) 0.0379(10) 0.0251(8) -0.0066(7) -0.0169(7) 0.0108(7) O2C 0.0293(8) 0.0264(8) 0.0219(7) -0.0061(6) -0.0119(6) 0.0079(6) O3C 0.0291(8) 0.0394(10) 0.0209(7) -0.0054(6) -0.0100(6) 0.0121(7) O4C 0.0273(7) 0.0279(8) 0.0182(7) -0.0016(6) -0.0086(6) 0.0074(6) C1C 0.0237(9) 0.0300(11) 0.0228(9) -0.0063(8) -0.0113(8) 0.0048(8) C2C 0.0232(9) 0.0279(10) 0.0239(9) -0.0064(8) -0.0117(8) 0.0054(8) C3C 0.0243(9) 0.0282(10) 0.0235(9) -0.0089(8) -0.0106(8) 0.0055(8) C4C 0.0262(10) 0.0279(10) 0.0291(10) -0.0067(8) -0.0152(8) 0.0074(8) C5C 0.0297(11) 0.0306(12) 0.0359(12) -0.0118(9) -0.0157(10) 0.0113(9) C6C 0.0302(11) 0.0336(12) 0.0280(11) -0.0131(9) -0.0103(9) 0.0076(9) C7C 0.0266(10) 0.0348(12) 0.0217(9) -0.0087(8) -0.0094(8) 0.0044(9) C8C 0.0294(11) 0.0285(11) 0.0338(11) -0.0080(9) -0.0170(9) 0.0077(8) C9C 0.0300(11) 0.0303(11) 0.0323(11) -0.0075(9) -0.0173(9) 0.0078(9) C10C 0.0279(10) 0.0273(11) 0.0298(11) -0.0044(8) -0.0145(9) 0.0044(8) C11C 0.0264(10) 0.0284(11) 0.0306(11) -0.0040(8) -0.0134(9) 0.0053(8) C12C 0.0247(10) 0.0266(11) 0.0303(11) -0.0014(8) -0.0092(9) 0.0044(8) C13C 0.0314(11) 0.0361(13) 0.0277(11) 0.0031(9) -0.0093(9) 0.0083(10) C14C 0.0349(12) 0.0370(13) 0.0350(12) 0.0000(10) -0.0149(10) 0.0149(10) C15C 0.0334(12) 0.0322(12) 0.0303(11) -0.0066(9) -0.0131(9) 0.0098(9) C16C 0.0278(10) 0.0298(11) 0.0299(11) 0.0001(9) -0.0110(9) 0.0048(9) C17C 0.0276(10) 0.0287(11) 0.0292(11) 0.0011(8) -0.0128(9) 0.0041(8) C18C 0.0247(9) 0.0281(10) 0.0234(9) 0.0003(8) -0.0104(8) 0.0034(8) C19C 0.0239(9) 0.0289(10) 0.0186(8) -0.0008(7) -0.0100(7) 0.0038(8) C20C 0.0227(9) 0.0290(10) 0.0206(9) -0.0020(7) -0.0118(8) 0.0030(8) C21C 0.0249(10) 0.0359(12) 0.0193(9) -0.0002(8) -0.0094(8) 0.0011(8) C22C 0.0337(12) 0.0368(13) 0.0226(10) 0.0057(9) -0.0116(9) 0.0010(10) C23C 0.0318(11) 0.0325(12) 0.0294(11) 0.0042(9) -0.0144(9) 0.0059(9) C24C 0.0224(9) 0.0305(11) 0.0194(9) -0.0020(7) -0.0102(7) 0.0055(8) O1D 0.0227(7) 0.0352(9) 0.0197(7) -0.0037(6) -0.0091(6) 0.0018(6) O2D 0.0246(7) 0.0324(8) 0.0188(7) -0.0035(6) -0.0106(6) 0.0000(6) O3D 0.0223(7) 0.0362(9) 0.0195(7) -0.0050(6) -0.0102(6) 0.0050(6) O4D 0.0203(7) 0.0379(9) 0.0183(7) -0.0033(6) -0.0078(6) 0.0014(6) C1D 0.0250(9) 0.0264(10) 0.0215(9) -0.0039(7) -0.0120(8) 0.0052(8) C2D 0.0254(9) 0.0250(10) 0.0214(9) -0.0041(7) -0.0113(8) 0.0060(8) C3D 0.0268(10) 0.0261(10) 0.0210(9) -0.0033(7) -0.0117(8) 0.0035(8) C4D 0.0269(10) 0.0271(10) 0.0259(10) -0.0037(8) -0.0122(8) 0.0046(8) C5D 0.0281(10) 0.0337(12) 0.0304(11) -0.0084(9) -0.0152(9) 0.0040(9) C6D 0.0297(11) 0.0425(14) 0.0258(10) -0.0073(9) -0.0158(9) 0.0043(10) C7D 0.0266(10) 0.0336(11) 0.0213(9) -0.0054(8) -0.0117(8) 0.0060(8) C8D 0.0304(11) 0.0326(12) 0.0300(11) -0.0035(9) -0.0148(9) 0.0003(9) C9D 0.0356(12) 0.0362(13) 0.0302(11) -0.0028(9) -0.0165(10) -0.0019(10) C10D 0.0303(11) 0.0366(13) 0.0269(11) -0.0027(9) -0.0111(9) -0.0025(9) C11D 0.0299(11) 0.0344(12) 0.0278(11) -0.0040(9) -0.0119(9) -0.0033(9) C12D 0.0347(12) 0.0373(13) 0.0277(11) -0.0054(9) -0.0132(10) -0.0029(10) C13D 0.0330(12) 0.0469(15) 0.0303(12) -0.0056(10) -0.0093(10) -0.0074(11) C14D 0.0338(13) 0.0507(16) 0.0354(13) -0.0051(11) -0.0141(11) -0.0101(11) C15D 0.0369(13) 0.0472(15) 0.0289(11) -0.0044(10) -0.0145(10) -0.0081(11) C16D 0.0322(11) 0.0360(13) 0.0295(11) -0.0061(9) -0.0127(9) -0.0001(9) C17D 0.0311(11) 0.0337(12) 0.0316(11) -0.0041(9) -0.0147(9) 0.0006(9) C18D 0.0300(11) 0.0278(11) 0.0251(10) -0.0022(8) -0.0129(9) 0.0019(8) C19D 0.0260(10) 0.0287(11) 0.0205(9) -0.0025(7) -0.0096(8) 0.0045(8) C20D 0.0266(10) 0.0265(10) 0.0204(9) -0.0021(7) -0.0114(8) 0.0057(8) C21D 0.0273(10) 0.0338(12) 0.0213(9) -0.0030(8) -0.0092(8) 0.0030(9) C22D 0.0277(11) 0.0454(15) 0.0240(10) -0.0026(9) -0.0072(9) -0.0017(10) C23D 0.0284(11) 0.0374(13) 0.0277(11) -0.0007(9) -0.0110(9) -0.0043(9) C24D 0.0242(9) 0.0286(10) 0.0197(9) -0.0016(7) -0.0111(8) 0.0062(8) O1L 0.0309(9) 0.0491(11) 0.0206(8) -0.0059(7) -0.0087(7) -0.0004(8) N1L 0.0418(12) 0.0411(13) 0.0270(10) -0.0101(9) 0.0012(9) -0.0084(10) C1L 0.0369(13) 0.0410(14) 0.0246(11) -0.0133(9) -0.0033(10) -0.0009(10) C3L 0.0375(13) 0.0429(14) 0.0221(10) -0.0067(9) -0.0106(9) 0.0022(11) O2L 0.0484(11) 0.0373(10) 0.0237(8) -0.0100(7) -0.0133(8) 0.0121(8) N2L 0.0467(14) 0.0374(13) 0.0410(13) -0.0068(10) -0.0055(11) 0.0058(11) C4L 0.0586(19) 0.0387(15) 0.0312(13) -0.0060(11) -0.0145(13) 0.0136(13) C5L 0.0411(15) 0.0450(16) 0.0477(16) -0.0114(13) -0.0142(13) 0.0083(12) C6L 0.062(2) 0.062(2) 0.053(2) -0.0091(18) 0.0030(18) 0.0017(19) O3L 0.0304(8) 0.0552(12) 0.0167(7) -0.0101(7) -0.0101(6) 0.0066(8) N3L 0.0432(12) 0.0459(13) 0.0216(9) -0.0112(8) -0.0173(9) 0.0119(10) C7L 0.0367(12) 0.0422(14) 0.0194(9) -0.0083(9) -0.0126(9) 0.0126(10) C8L 0.0426(15) 0.0615(19) 0.0191(10) -0.0097(11) -0.0118(10) 0.0141(13) C9L 0.074(2) 0.069(2) 0.0341(14) -0.0206(14) -0.0293(16) 0.0039(18) O4L 0.0383(9) 0.0404(10) 0.0185(7) -0.0017(7) -0.0089(7) 0.0124(8) C10L 0.119(5) 0.089(4) 0.064(3) -0.012(3) -0.039(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1D 1.9539(17) . ? Cu1 O1C 1.962(2) . ? Cu1 O1B 1.9701(19) . ? Cu1 O1A 1.972(2) . ? Cu1 O1L 2.129(2) . ? Cu1 Cu2 2.6206(10) . ? Cu2 O2C 1.9546(18) . ? Cu2 O2A 1.9671(19) . ? Cu2 O2D 1.9699(17) . ? Cu2 O2B 1.9814(18) . ? Cu2 O2L 2.194(2) . ? Cu3 O3D 1.9551(17) . ? Cu3 O3B 1.9679(19) . ? Cu3 O3C 1.973(2) . ? Cu3 O3A 1.982(2) . ? Cu3 O3L 2.1252(19) . ? Cu3 Cu4 2.6255(10) . ? Cu4 O4C 1.9505(17) . ? Cu4 O4A 1.9546(19) . ? Cu4 O4D 1.9702(18) . ? Cu4 O4B 1.9845(18) . ? Cu4 O4L 2.1802(19) . ? O1A C1A 1.266(3) . ? O2A C1A 1.264(3) . ? O3A C24A 1.268(3) . ? O4A C24A 1.271(3) . ? C1A C2A 1.501(4) . ? C2A C3A 1.381(5) . ? C2A C7A 1.421(5) . ? C3A C4A 1.401(4) . ? C4A C5A 1.421(6) . ? C4A C8A 1.462(7) . ? C5A C6A 1.360(8) . ? C6A C7A 1.394(6) . ? C8A C9A 1.207(7) . ? C9A C10A 1.437(6) . ? C10A C11A 1.387(6) . ? C10A C15A 1.400(4) . ? C11A C12A 1.408(7) . ? C12A C13A 1.410(5) . ? C12A C16A 1.420(6) . ? C13A C14A 1.379(7) . ? C14A C15A 1.397(7) . ? C16A C17A 1.201(6) . ? C17A C18A 1.423(6) . ? C18A C19A 1.401(4) . ? C18A C23A 1.408(6) . ? C19A C20A 1.399(4) . ? C20A C21A 1.394(4) . ? C20A C24A 1.494(4) . ? C21A C22A 1.396(5) . ? C22A C23A 1.349(7) . ? O1B C1B 1.269(3) . ? O2B C1B 1.267(3) . ? O3B C24B 1.259(3) . ? O4B C24B 1.273(3) . ? C1B C2B 1.503(3) . ? C2B C3B 1.390(3) . ? C2B C7B 1.403(3) . ? C3B C4B 1.404(3) . ? C4B C5B 1.403(3) . ? C4B C8B 1.428(4) . ? C5B C6B 1.393(4) . ? C6B C7B 1.389(4) . ? C8B C9B 1.205(4) . ? C9B C10B 1.427(4) . ? C10B C11B 1.399(4) . ? C10B C15B 1.405(4) . ? C11B C12B 1.398(4) . ? C12B C13B 1.397(4) . ? C12B C16B 1.431(4) . ? C13B C14B 1.368(4) . ? C14B C15B 1.394(5) . ? C16B C17B 1.198(4) . ? C17B C18B 1.436(4) . ? C18B C19B 1.395(4) . ? C18B C23B 1.404(3) . ? C19B C20B 1.394(3) . ? C20B C21B 1.405(3) . ? C20B C24B 1.489(3) . ? C21B C22B 1.392(4) . ? C22B C23B 1.392(4) . ? O1C C1C 1.269(3) . ? O2C C1C 1.265(3) . ? O3C C24C 1.272(3) . ? O4C C24C 1.267(3) . ? C1C C2C 1.503(3) . ? C2C C3C 1.400(3) . ? C2C C7C 1.402(3) . ? C3C C4C 1.396(3) . ? C4C C5C 1.402(3) . ? C4C C8C 1.432(3) . ? C5C C6C 1.385(4) . ? C6C C7C 1.389(4) . ? C8C C9C 1.201(4) . ? C9C C10C 1.434(3) . ? C10C C15C 1.404(3) . ? C10C C11C 1.404(3) . ? C11C C12C 1.397(3) . ? C12C C13C 1.407(4) . ? C12C C16C 1.436(3) . ? C13C C14C 1.394(4) . ? C14C C15C 1.395(4) . ? C16C C17C 1.197(4) . ? C17C C18C 1.438(3) . ? C18C C23C 1.397(3) . ? C18C C19C 1.401(3) . ? C19C C20C 1.396(3) . ? C20C C21C 1.397(3) . ? C20C C24C 1.495(3) . ? C21C C22C 1.389(4) . ? C22C C23C 1.386(4) . ? O1D C1D 1.266(3) . ? O2D C1D 1.268(3) . ? O3D C24D 1.267(3) . ? O4D C24D 1.274(3) . ? C1D C2D 1.501(3) . ? C2D C3D 1.391(3) . ? C2D C7D 1.406(3) . ? C3D C4D 1.399(3) . ? C4D C5D 1.405(3) . ? C4D C8D 1.439(3) . ? C5D C6D 1.385(4) . ? C6D C7D 1.384(3) . ? C8D C9D 1.193(4) . ? C9D C10D 1.439(4) . ? C10D C11D 1.394(4) . ? C10D C15D 1.407(4) . ? C11D C12D 1.407(4) . ? C12D C13D 1.407(4) . ? C12D C16D 1.430(4) . ? C13D C14D 1.387(4) . ? C14D C15D 1.391(4) . ? C16D C17D 1.203(4) . ? C17D C18D 1.439(3) . ? C18D C19D 1.388(3) . ? C18D C23D 1.404(3) . ? C19D C20D 1.397(3) . ? C20D C21D 1.403(3) . ? C20D C24D 1.498(3) . ? C21D C22D 1.385(4) . ? C22D C23D 1.389(4) . ? O1L C1L 1.211(3) . ? N1L C1L 1.331(3) . ? N1L C2L 1.434(6) . ? N1L C3L 1.439(4) . ? O2L C4L 1.244(4) . ? N2L C4L 1.334(5) . ? N2L C5L 1.445(5) . ? N2L C6L 1.459(5) . ? O3L C7L 1.241(3) . ? N3L C7L 1.331(3) . ? N3L C8L 1.452(4) . ? N3L C9L 1.463(4) . ? O4L C10L 1.223(6) . ? N4L C12L 1.328(8) . ? N4L C10L 1.345(8) . ? N4L C11L 1.497(11) . ? 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 O1D Cu1 O1C 91.06(9) . . ? O1D Cu1 O1B 169.41(7) . . ? O1C Cu1 O1B 88.14(9) . . ? O1D Cu1 O1A 90.48(8) . . ? O1C Cu1 O1A 166.96(8) . . ? O1B Cu1 O1A 87.97(9) . . ? O1D Cu1 O1L 96.55(8) . . ? O1C Cu1 O1L 96.67(9) . . ? O1B Cu1 O1L 94.03(8) . . ? O1A Cu1 O1L 96.01(9) . . ? O1D Cu1 Cu2 84.56(6) . . ? O1C Cu1 Cu2 81.25(6) . . ? O1B Cu1 Cu2 84.89(6) . . ? O1A Cu1 Cu2 86.01(7) . . ? O1L Cu1 Cu2 177.68(6) . . ? O2C Cu2 O2A 169.23(7) . . ? O2C Cu2 O2D 90.43(8) . . ? O2A Cu2 O2D 91.22(8) . . ? O2C Cu2 O2B 87.02(8) . . ? O2A Cu2 O2B 89.10(8) . . ? O2D Cu2 O2B 167.57(7) . . ? O2C Cu2 O2L 100.26(8) . . ? O2A Cu2 O2L 90.28(8) . . ? O2D Cu2 O2L 93.01(8) . . ? O2B Cu2 O2L 99.42(9) . . ? O2C Cu2 Cu1 87.18(6) . . ? O2A Cu2 Cu1 82.43(7) . . ? O2D Cu2 Cu1 83.70(6) . . ? O2B Cu2 Cu1 84.03(6) . . ? O2L Cu2 Cu1 171.91(6) . . ? O3D Cu3 O3B 169.69(7) . . ? O3D Cu3 O3C 90.11(8) . . ? O3B Cu3 O3C 88.19(9) . . ? O3D Cu3 O3A 89.75(8) . . ? O3B Cu3 O3A 89.43(9) . . ? O3C Cu3 O3A 165.91(7) . . ? O3D Cu3 O3L 97.47(8) . . ? O3B Cu3 O3L 92.84(8) . . ? O3C Cu3 O3L 97.59(8) . . ? O3A Cu3 O3L 96.39(9) . . ? O3D Cu3 Cu4 85.19(6) . . ? O3B Cu3 Cu4 84.50(6) . . ? O3C Cu3 Cu4 81.54(6) . . ? O3A Cu3 Cu4 84.41(6) . . ? O3L Cu3 Cu4 177.21(5) . . ? O4C Cu4 O4A 170.90(7) . . ? O4C Cu4 O4D 90.69(8) . . ? O4A Cu4 O4D 91.26(8) . . ? O4C Cu4 O4B 87.62(8) . . ? O4A Cu4 O4B 88.57(8) . . ? O4D Cu4 O4B 167.58(7) . . ? O4C Cu4 O4L 96.80(8) . . ? O4A Cu4 O4L 91.80(8) . . ? O4D Cu4 O4L 96.63(8) . . ? O4B Cu4 O4L 95.79(8) . . ? O4C Cu4 Cu3 86.99(6) . . ? O4A Cu4 Cu3 84.41(6) . . ? O4D Cu4 Cu3 83.45(6) . . ? O4B Cu4 Cu3 84.17(6) . . ? O4L Cu4 Cu3 176.21(5) . . ? C1A O1A Cu1 119.49(16) . . ? C1A O2A Cu2 123.36(18) . . ? C24A O3A Cu3 121.49(17) . . ? C24A O4A Cu4 122.85(17) . . ? O2A C1A O1A 126.1(2) . . ? O2A C1A C2A 116.6(3) . . ? O1A C1A C2A 117.3(2) . . ? C3A C2A C7A 121.5(3) . . ? C3A C2A C1A 119.4(3) . . ? C7A C2A C1A 119.0(3) . . ? C2A C3A C4A 119.9(3) . . ? C3A C4A C5A 118.5(4) . . ? C3A C4A C8A 119.2(4) . . ? C5A C4A C8A 122.4(3) . . ? C6A C5A C4A 120.9(4) . . ? C5A C6A C7A 121.6(4) . . ? C6A C7A C2A 117.6(5) . . ? C9A C8A C4A 178.2(4) . . ? C8A C9A C10A 179.1(4) . . ? C11A C10A C15A 119.3(4) . . ? C11A C10A C9A 120.7(3) . . ? C15A C10A C9A 119.9(4) . . ? C10A C11A C12A 121.0(3) . . ? C11A C12A C13A 118.9(4) . . ? C11A C12A C16A 121.1(3) . . ? C13A C12A C16A 120.0(5) . . ? C14A C13A C12A 119.9(5) . . ? C13A C14A C15A 120.8(4) . . ? C14A C15A C10A 120.1(4) . . ? C17A C16A C12A 177.1(4) . . ? C16A C17A C18A 177.1(4) . . ? C19A C18A C23A 118.8(4) . . ? C19A C18A C17A 120.3(3) . . ? C23A C18A C17A 120.9(3) . . ? C20A C19A C18A 120.3(3) . . ? C21A C20A C19A 119.4(3) . . ? C21A C20A C24A 120.7(3) . . ? C19A C20A C24A 119.8(2) . . ? C20A C21A C22A 119.6(4) . . ? C23A C22A C21A 121.2(4) . . ? C22A C23A C18A 120.6(3) . . ? O3A C24A O4A 125.6(2) . . ? O3A C24A C20A 117.3(2) . . ? O4A C24A C20A 117.1(2) . . ? C1B O1B Cu1 121.41(16) . . ? C1B O2B Cu2 121.61(16) . . ? C24B O3B Cu3 122.46(16) . . ? C24B O4B Cu4 121.40(16) . . ? O2B C1B O1B 126.3(2) . . ? O2B C1B C2B 117.5(2) . . ? O1B C1B C2B 116.3(2) . . ? C3B C2B C7B 119.7(2) . . ? C3B C2B C1B 120.0(2) . . ? C7B C2B C1B 120.3(2) . . ? C2B C3B C4B 120.4(2) . . ? C5B C4B C3B 119.2(2) . . ? C5B C4B C8B 120.9(2) . . ? C3B C4B C8B 120.0(2) . . ? C6B C5B C4B 120.5(2) . . ? C7B C6B C5B 119.9(2) . . ? C6B C7B C2B 120.3(2) . . ? C9B C8B C4B 178.2(3) . . ? C8B C9B C10B 177.6(3) . . ? C11B C10B C15B 119.1(3) . . ? C11B C10B C9B 120.2(2) . . ? C15B C10B C9B 120.6(2) . . ? C12B C11B C10B 120.6(2) . . ? C13B C12B C11B 119.3(3) . . ? C13B C12B C16B 120.2(3) . . ? C11B C12B C16B 120.5(3) . . ? C14B C13B C12B 120.5(3) . . ? C13B C14B C15B 120.9(3) . . ? C14B C15B C10B 119.6(3) . . ? C17B C16B C12B 178.8(3) . . ? C16B C17B C18B 177.2(3) . . ? C19B C18B C23B 119.7(2) . . ? C19B C18B C17B 119.7(2) . . ? C23B C18B C17B 120.7(2) . . ? C20B C19B C18B 120.2(2) . . ? C19B C20B C21B 119.8(2) . . ? C19B C20B C24B 119.9(2) . . ? C21B C20B C24B 120.2(2) . . ? C22B C21B C20B 120.2(2) . . ? C23B C22B C21B 119.8(2) . . ? C22B C23B C18B 120.3(2) . . ? O3B C24B O4B 125.9(2) . . ? O3B C24B C20B 117.0(2) . . ? O4B C24B C20B 117.1(2) . . ? C1C O1C Cu1 123.45(17) . . ? C1C O2C Cu2 118.46(15) . . ? C24C O3C Cu3 123.62(16) . . ? C24C O4C Cu4 119.55(15) . . ? O2C C1C O1C 126.0(2) . . ? O2C C1C C2C 117.9(2) . . ? O1C C1C C2C 116.1(2) . . ? C3C C2C C7C 119.9(2) . . ? C3C C2C C1C 120.0(2) . . ? C7C C2C C1C 120.0(2) . . ? C4C C3C C2C 119.9(2) . . ? C3C C4C C5C 119.6(2) . . ? C3C C4C C8C 120.5(2) . . ? C5C C4C C8C 119.9(2) . . ? C6C C5C C4C 120.4(2) . . ? C5C C6C C7C 120.3(2) . . ? C6C C7C C2C 119.9(2) . . ? C9C C8C C4C 177.2(3) . . ? C8C C9C C10C 176.9(3) . . ? C15C C10C C11C 119.2(2) . . ? C15C C10C C9C 121.5(2) . . ? C11C C10C C9C 119.3(2) . . ? C12C C11C C10C 120.7(2) . . ? C11C C12C C13C 120.0(2) . . ? C11C C12C C16C 118.8(2) . . ? C13C C12C C16C 121.2(2) . . ? C14C C13C C12C 119.0(2) . . ? C13C C14C C15C 121.3(2) . . ? C14C C15C C10C 119.8(2) . . ? C17C C16C C12C 177.2(3) . . ? C16C C17C C18C 178.1(3) . . ? C23C C18C C19C 119.6(2) . . ? C23C C18C C17C 120.1(2) . . ? C19C C18C C17C 120.3(2) . . ? C20C C19C C18C 119.8(2) . . ? C19C C20C C21C 120.1(2) . . ? C19C C20C C24C 119.78(19) . . ? C21C C20C C24C 120.1(2) . . ? C22C C21C C20C 119.9(2) . . ? C23C C22C C21C 120.3(2) . . ? C22C C23C C18C 120.3(2) . . ? O4C C24C O3C 125.6(2) . . ? O4C C24C C20C 117.5(2) . . ? O3C C24C C20C 116.82(19) . . ? C1D O1D Cu1 121.09(15) . . ? C1D O2D Cu2 121.64(15) . . ? C24D O3D Cu3 121.06(15) . . ? C24D O4D Cu4 122.59(15) . . ? O1D C1D O2D 126.0(2) . . ? O1D C1D C2D 116.56(19) . . ? O2D C1D C2D 117.4(2) . . ? C3D C2D C7D 119.6(2) . . ? C3D C2D C1D 120.1(2) . . ? C7D C2D C1D 120.4(2) . . ? C2D C3D C4D 120.1(2) . . ? C3D C4D C5D 119.5(2) . . ? C3D C4D C8D 119.9(2) . . ? C5D C4D C8D 120.5(2) . . ? C6D C5D C4D 120.4(2) . . ? C7D C6D C5D 119.9(2) . . ? C6D C7D C2D 120.5(2) . . ? C9D C8D C4D 176.0(3) . . ? C8D C9D C10D 176.3(3) . . ? C11D C10D C15D 119.3(2) . . ? C11D C10D C9D 119.7(2) . . ? C15D C10D C9D 120.9(2) . . ? C10D C11D C12D 120.6(2) . . ? C13D C12D C11D 119.3(2) . . ? C13D C12D C16D 120.7(2) . . ? C11D C12D C16D 119.9(2) . . ? C14D C13D C12D 119.8(2) . . ? C13D C14D C15D 120.9(3) . . ? C14D C15D C10D 120.0(3) . . ? C17D C16D C12D 178.1(3) . . ? C16D C17D C18D 177.4(3) . . ? C19D C18D C23D 119.7(2) . . ? C19D C18D C17D 120.2(2) . . ? C23D C18D C17D 120.0(2) . . ? C18D C19D C20D 120.4(2) . . ? C19D C20D C21D 119.4(2) . . ? C19D C20D C24D 120.4(2) . . ? C21D C20D C24D 120.2(2) . . ? C22D C21D C20D 120.2(2) . . ? C21D C22D C23D 120.2(2) . . ? C22D C23D C18D 120.0(2) . . ? O3D C24D O4D 125.7(2) . . ? O3D C24D C20D 116.8(2) . . ? O4D C24D C20D 117.5(2) . . ? C1L O1L Cu1 122.86(18) . . ? C1L N1L C2L 120.7(3) . . ? C1L N1L C3L 121.8(2) . . ? C2L N1L C3L 117.0(3) . . ? O1L C1L N1L 124.5(3) . . ? C4L O2L Cu2 125.1(2) . . ? C4L N2L C5L 121.9(3) . . ? C4L N2L C6L 121.6(3) . . ? C5L N2L C6L 116.3(3) . . ? O2L C4L N2L 127.5(3) . . ? C7L O3L Cu3 123.04(18) . . ? C7L N3L C8L 121.4(2) . . ? C7L N3L C9L 120.7(3) . . ? C8L N3L C9L 117.8(2) . . ? O3L C7L N3L 123.3(3) . . ? C10L O4L Cu4 131.2(3) . . ? C12L N4L C10L 119.1(7) . . ? C12L N4L C11L 118.8(8) . . ? C10L N4L C11L 120.2(8) . . ? O4L C10L N4L 128.5(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 31.81 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.843 _refine_diff_density_min -2.362 _refine_diff_density_rms 0.142 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 1 0.003 0.500 0.497 772.2 83.6 2 0.205 0.803 0.034 156.1 18.4 3 0.034 0.939 0.917 6.4 -0.6 4 0.794 0.197 -0.033 156.3 18.3 5 0.965 0.061 0.083 6.3 -0.6 _platon_squeeze_details ; ; #===END data_1b _database_code_depnum_ccdc_archive 'CCDC 744144' #TrackingRef 'mslah_rev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H38 Cu2 N2 O10' _chemical_formula_weight 1001.94 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 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 11.245(2) _cell_length_b 37.235(7) _cell_length_c 28.875(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.01(3) _cell_angle_gamma 90.00 _cell_volume 11972(4) _cell_formula_units_Z 8 _cell_measurement_temperature 99(2) _cell_measurement_reflns_used 235087 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 30.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.6184 _exptl_absorpt_correction_T_max 0.7986 _exptl_absorpt_process_details 'hkl2000 scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 99(2) _diffrn_radiation_wavelength 0.75000 __diffrn_radiation_type synchrotron _diffrn_radiation_source 'bending magnet 6b mx beamline' _diffrn_radiation_monochromator 'si(111) double crystal monochromator' _diffrn_measurement_device_type 'ccd area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53617 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.00 _reflns_number_total 14391 _reflns_number_gt 12173 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'adsc quantum-210 adx program' _computing_cell_refinement hkl2000 _computing_data_reduction hkl2000 _computing_structure_solution 'wingx sir-92' _computing_structure_refinement 'bruker shelxtl' _computing_molecular_graphics ortep3 _computing_publication_material wingx _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^)+(0.1428P)^2^+25.2440P] 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 0.0044(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14391 _refine_ls_number_parameters 754 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2452 _refine_ls_wR_factor_gt 0.2357 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.028 _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 0.19763(4) 0.061073(11) 0.428579(18) 0.05013(17) Uani 1 1 d . . . Cu2 Cu 0.22574(3) 0.127457(9) 0.460428(15) 0.04158(16) Uani 1 1 d . B . O1 O 0.3667(2) 0.05467(7) 0.45538(12) 0.0592(7) Uani 1 1 d . . . O2 O 0.3953(2) 0.11302(7) 0.47301(10) 0.0506(6) Uani 1 1 d . . . O3 O 0.0312(2) 0.07640(7) 0.40768(11) 0.0584(7) Uani 1 1 d . . . O4 O 0.0522(2) 0.13103(6) 0.44172(10) 0.0498(6) Uani 1 1 d . . . O5 O 0.2501(3) 0.08385(7) 0.37274(11) 0.0613(7) Uani 1 1 d . . . O6 O 0.2495(2) 0.14121(7) 0.39696(10) 0.0525(6) Uani 1 1 d . . . O7 O 0.1527(2) 0.04945(7) 0.49034(11) 0.0559(6) Uani 1 1 d . . . O8 O 0.1992(2) 0.10462(6) 0.51974(9) 0.0499(6) Uani 1 1 d . B . C1 C 0.4311(3) 0.08108(10) 0.47015(14) 0.0502(8) Uani 1 1 d . . . C2 C 0.5626(3) 0.07499(9) 0.48510(14) 0.0486(8) Uani 1 1 d . . . C3 C 0.6359(3) 0.10347(10) 0.49915(14) 0.0500(8) Uani 1 1 d . . . H3 H 0.6025 0.1269 0.4994 0.060 Uiso 1 1 calc R . . C4 C 0.7588(3) 0.09871(11) 0.51305(14) 0.0539(8) Uani 1 1 d . . . C5 C 0.8061(4) 0.06395(12) 0.51172(17) 0.0629(11) Uani 1 1 d . . . H5 H 0.8900 0.0603 0.5197 0.075 Uiso 1 1 calc R . . C6 C 0.7327(4) 0.03512(11) 0.49909(17) 0.0631(11) Uani 1 1 d . . . H6 H 0.7656 0.0116 0.4999 0.076 Uiso 1 1 calc R . . C7 C 0.6103(3) 0.04015(10) 0.48504(16) 0.0566(9) Uani 1 1 d . . . H7 H 0.5597 0.0203 0.4755 0.068 Uiso 1 1 calc R . . C8 C 0.8332(3) 0.12890(11) 0.52810(15) 0.0568(9) Uani 1 1 d . . . C9 C 0.8903(3) 0.15488(12) 0.54091(15) 0.0575(9) Uani 1 1 d . . . C10 C 0.9581(3) 0.18636(11) 0.55812(14) 0.0537(8) Uani 1 1 d . . . C11 C 0.9011(3) 0.21921(11) 0.56336(14) 0.0552(9) Uani 1 1 d . . . H11 H 0.8170 0.2212 0.5540 0.066 Uiso 1 1 calc R . . C12 C 0.9641(3) 0.24844(12) 0.58160(16) 0.0585(9) Uani 1 1 d . . . C13 C 1.0892(4) 0.24536(13) 0.59576(19) 0.0701(12) Uani 1 1 d . . . H13 H 1.1339 0.2653 0.6095 0.084 Uiso 1 1 calc R . . C14 C 1.1463(4) 0.21297(13) 0.5894(2) 0.0745(13) Uani 1 1 d . . . H14 H 1.2306 0.2110 0.5984 0.089 Uiso 1 1 calc R . . C15 C 1.0832(3) 0.18396(12) 0.57053(18) 0.0635(10) Uani 1 1 d . . . H15 H 1.1237 0.1622 0.5658 0.076 Uiso 1 1 calc R . . C16 C -0.4062(3) 0.21761(12) 0.41294(17) 0.0618(10) Uani 1 1 d . . . C17 C -0.3593(3) 0.18887(12) 0.40833(15) 0.0572(9) Uani 1 1 d . . . C18 C -0.3098(3) 0.15446(11) 0.40145(14) 0.0509(8) Uani 1 1 d . . . C19 C -0.1870(3) 0.14739(10) 0.41312(14) 0.0498(8) Uani 1 1 d . . . H19 H -0.1346 0.1660 0.4260 0.060 Uiso 1 1 calc R . . C20 C -0.1411(3) 0.11352(10) 0.40611(13) 0.0486(7) Uani 1 1 d . . . C21 C -0.2182(3) 0.08592(11) 0.38804(15) 0.0554(8) Uani 1 1 d . . . H21 H -0.1874 0.0626 0.3837 0.067 Uiso 1 1 calc R . . C22 C -0.3407(4) 0.09281(12) 0.37643(15) 0.0599(9) Uani 1 1 d . . . H22 H -0.3931 0.0742 0.3637 0.072 Uiso 1 1 calc R . . C23 C -0.3865(3) 0.12660(12) 0.38331(16) 0.0589(9) Uani 1 1 d . . . H23 H -0.4702 0.1309 0.3757 0.071 Uiso 1 1 calc R . . C24 C -0.0085(3) 0.10652(9) 0.41964(13) 0.0480(7) Uani 1 1 d . . . C25 C 0.2619(3) 0.11730(10) 0.36706(14) 0.0500(8) Uani 1 1 d . . . C26 C 0.2934(3) 0.12956(10) 0.32118(14) 0.0490(8) Uani 1 1 d . . . C27 C 0.2980(4) 0.16563(11) 0.31124(15) 0.0578(9) Uani 1 1 d . A . H27 H 0.2826 0.1827 0.3341 0.069 Uiso 1 1 calc R . . C28 C 0.3250(5) 0.17745(12) 0.26810(16) 0.0683(11) Uani 1 1 d . . . C29 C 0.3474(4) 0.15188(13) 0.23530(17) 0.0670(11) Uani 1 1 d . A . H29 H 0.3653 0.1594 0.2056 0.080 Uiso 1 1 calc R . . C30 C 0.3439(4) 0.11592(13) 0.24515(17) 0.0648(10) Uani 1 1 d . . . H30 H 0.3603 0.0989 0.2224 0.078 Uiso 1 1 calc R A . C31 C 0.3168(3) 0.10417(12) 0.28776(15) 0.0583(9) Uani 1 1 d . A . H31 H 0.3141 0.0792 0.2944 0.070 Uiso 1 1 calc R . . C321 C 0.3596(10) 0.2153(3) 0.2613(4) 0.062(2) Uani 0.50 1 d P A 1 C331 C 0.3687(12) 0.2465(3) 0.2517(4) 0.072(3) Uani 0.50 1 d P A 1 C341 C 0.3812(12) 0.2831(3) 0.2383(3) 0.077(3) Uani 0.50 1 d PD A 1 C351 C 0.3802(11) 0.3109(2) 0.2702(4) 0.081(3) Uani 0.50 1 d PD A 1 H351 H 0.3714 0.3058 0.3018 0.097 Uiso 0.50 1 calc PR A 1 C361 C 0.3920(13) 0.3461(2) 0.2562(4) 0.088(4) Uani 0.50 1 d PD . 1 C371 C 0.4096(16) 0.3540(3) 0.2107(4) 0.105(5) Uani 0.50 1 d PD A 1 H371 H 0.4172 0.3781 0.2008 0.126 Uiso 0.50 1 calc PR A 1 C381 C 0.4157(17) 0.3257(4) 0.1801(5) 0.113(5) Uani 0.50 1 d PD A 1 H38 H 0.4318 0.3305 0.1493 0.136 Uiso 0.50 1 calc PR A 1 C391 C 0.3990(15) 0.2905(3) 0.1930(4) 0.097(4) Uani 0.50 1 d PD A 1 H391 H 0.3998 0.2716 0.1709 0.116 Uiso 0.50 1 calc PR A 1 C322 C 0.3016(8) 0.2136(3) 0.2538(3) 0.0511(19) Uani 0.50 1 d P A 2 C332 C 0.2935(10) 0.2454(3) 0.2418(3) 0.063(2) Uani 0.50 1 d P A 2 C342 C 0.2905(9) 0.2820(2) 0.2266(3) 0.063(2) Uani 0.50 1 d PD A 2 C352 C 0.2891(9) 0.3103(2) 0.2578(3) 0.070(2) Uani 0.50 1 d PD A 2 H352 H 0.2868 0.3050 0.2899 0.084 Uiso 0.50 1 calc PR A 2 C362 C 0.2909(11) 0.3462(3) 0.2439(3) 0.078(3) Uani 0.50 1 d PD . 2 C372 C 0.2967(15) 0.3529(3) 0.1970(3) 0.097(4) Uani 0.50 1 d PD A 2 H372 H 0.2996 0.3769 0.1863 0.116 Uiso 0.50 1 calc PR A 2 C382 C 0.2983(18) 0.3252(3) 0.1661(4) 0.115(6) Uani 0.50 1 d PD A 2 H382 H 0.3036 0.3306 0.1343 0.138 Uiso 0.50 1 calc PR A 2 C392 C 0.2923(13) 0.2890(3) 0.1794(3) 0.083(3) Uani 0.50 1 d PD A 2 H392 H 0.2897 0.2701 0.1571 0.099 Uiso 0.50 1 calc PR A 2 C401 C 0.1070(15) 0.1245(3) 0.7106(4) 0.088(4) Uani 0.50 1 d P . 1 C411 C 0.0989(12) 0.1005(3) 0.6814(4) 0.077(3) Uani 0.50 1 d P B 1 C421 C 0.0993(10) 0.0741(3) 0.6467(5) 0.071(3) Uani 0.50 1 d PD B 1 C431 C 0.1376(13) 0.0854(5) 0.6051(5) 0.080(5) Uani 0.50 1 d PD B 1 H431 H 0.1595 0.1097 0.6010 0.097 Uiso 0.50 1 calc PR B 1 C441 C 0.1429(4) 0.06029(9) 0.57019(17) 0.0626(11) Uani 0.50 1 d PD B 1 C451 C 0.1011(12) 0.0244(3) 0.5718(7) 0.054(4) Uani 0.50 1 d PD B 1 H451 H 0.0937 0.0084 0.5459 0.065 Uiso 0.50 1 calc PR B 1 C461 C 0.072(2) 0.0151(5) 0.6159(6) 0.072(4) Uani 0.50 1 d PD B 1 H461 H 0.0493 -0.0092 0.6201 0.086 Uiso 0.50 1 calc PR B 1 C471 C 0.0725(13) 0.0381(3) 0.6545(7) 0.081(4) Uani 0.50 1 d PD B 1 H471 H 0.0559 0.0298 0.6841 0.097 Uiso 0.50 1 calc PR B 1 C402 C 0.2034(15) 0.1254(3) 0.7235(4) 0.085(4) Uani 0.50 1 d P . 2 C412 C 0.1902(14) 0.1018(3) 0.6937(4) 0.079(3) Uani 0.50 1 d P B 2 C422 C 0.1726(12) 0.0753(3) 0.6568(4) 0.079(4) Uani 0.50 1 d PD B 2 C432 C 0.1732(13) 0.0840(5) 0.6088(4) 0.071(4) Uani 0.50 1 d PD B 2 H432 H 0.1958 0.1078 0.6019 0.085 Uiso 0.50 1 calc PR B 2 C442 C 0.1429(4) 0.06029(9) 0.57019(17) 0.0626(11) Uani 0.50 1 d PD B 2 C452 C 0.112(2) 0.0254(4) 0.5833(8) 0.077(6) Uani 0.50 1 d PD B 2 H452 H 0.0927 0.0082 0.5591 0.092 Uiso 0.50 1 calc PR B 2 C462 C 0.107(2) 0.0143(6) 0.6289(6) 0.100(9) Uani 0.50 1 d PD B 2 H462 H 0.0809 -0.0091 0.6359 0.119 Uiso 0.50 1 calc PR B 2 C472 C 0.1418(18) 0.0400(3) 0.6645(7) 0.117(8) Uani 0.50 1 d PD B 2 H472 H 0.1444 0.0324 0.6960 0.140 Uiso 0.50 1 calc PR B 2 C48 C 0.1666(3) 0.07233(9) 0.52308(14) 0.0487(8) Uani 1 1 d . . . O1D O 0.1933(4) 0.00896(8) 0.39797(13) 0.0818(10) Uani 1 1 d . . . N1D N 0.1954(8) -0.03111(17) 0.3392(2) 0.140(3) Uani 1 1 d . . . C1D C 0.1872(7) 0.00244(17) 0.3578(3) 0.103(2) Uani 1 1 d . . . H1D H 0.1758 0.0221 0.3366 0.124 Uiso 1 1 calc R . . C2D C 0.2146(14) -0.0609(2) 0.3679(3) 0.197(6) Uani 1 1 d . . . H2D1 H 0.2985 -0.0613 0.3827 0.295 Uiso 1 1 calc R . . H2D2 H 0.1973 -0.0828 0.3493 0.295 Uiso 1 1 calc R . . H2D3 H 0.1617 -0.0598 0.3921 0.295 Uiso 1 1 calc R . . C3D C 0.1888(13) -0.0373(3) 0.2916(4) 0.192(6) Uani 1 1 d . . . H3D1 H 0.1774 -0.0144 0.2748 0.288 Uiso 1 1 calc R . . H3D2 H 0.1210 -0.0532 0.2813 0.288 Uiso 1 1 calc R . . H3D3 H 0.2635 -0.0485 0.2851 0.288 Uiso 1 1 calc R . . O2D O 0.2707(3) 0.17955(8) 0.49005(12) 0.0681(8) Uani 1 1 d D . . N21D N 0.4593(6) 0.18325(18) 0.5404(3) 0.0583(15) Uani 0.50 1 d PDU C -1 C41D C 0.3769(5) 0.18990(15) 0.5038(2) 0.0908(17) Uani 0.50 1 d PD C -1 H41D H 0.4045 0.2065 0.4827 0.109 Uiso 0.50 1 calc PR C -1 C51D C 0.5602(13) 0.2115(4) 0.5408(5) 0.209(6) Uiso 0.50 1 d PDU C -1 H51A H 0.6222 0.2072 0.5676 0.313 Uiso 0.50 1 calc PR C -1 H51B H 0.5266 0.2356 0.5432 0.313 Uiso 0.50 1 calc PR C -1 H51C H 0.5958 0.2097 0.5117 0.313 Uiso 0.50 1 calc PR C -1 C61D C 0.4313(8) 0.1566(3) 0.5739(4) 0.078(3) Uani 0.50 1 d PD C -1 H61A H 0.4992 0.1543 0.5990 0.117 Uiso 0.50 1 calc PR C -1 H61B H 0.4163 0.1334 0.5581 0.117 Uiso 0.50 1 calc PR C -1 H61C H 0.3597 0.1641 0.5872 0.117 Uiso 0.50 1 calc PR C -1 N22D N 0.4153(10) 0.2182(3) 0.5199(4) 0.095(3) Uiso 0.50 1 d PDU C -2 C42D C 0.3769(5) 0.18990(15) 0.5038(2) 0.0908(17) Uani 0.50 1 d PD C -2 H42D H 0.4368 0.1724 0.5009 0.109 Uiso 0.50 1 calc PR C -2 C52D C 0.5602(13) 0.2115(4) 0.5408(5) 0.209(6) Uiso 0.50 1 d PDU C -2 H52A H 0.5953 0.2339 0.5542 0.313 Uiso 0.50 1 calc PR C -2 H52B H 0.6035 0.2038 0.5153 0.313 Uiso 0.50 1 calc PR C -2 H52C H 0.5666 0.1929 0.5650 0.313 Uiso 0.50 1 calc PR C -2 C62D C 0.3394(16) 0.2490(5) 0.5181(7) 0.142(6) Uiso 0.50 1 d PD C -2 H62A H 0.3852 0.2695 0.5325 0.213 Uiso 0.50 1 calc PR C -2 H62B H 0.2716 0.2440 0.5350 0.213 Uiso 0.50 1 calc PR C -2 H62C H 0.3092 0.2547 0.4854 0.213 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 0.0516(3) 0.0271(2) 0.0719(3) -0.00599(16) 0.0092(2) 0.00506(15) Cu2 0.0403(2) 0.0256(2) 0.0591(3) -0.00105(14) 0.00761(16) 0.00591(13) O1 0.0509(14) 0.0354(12) 0.093(2) 0.0064(12) 0.0165(13) 0.0096(10) O2 0.0447(12) 0.0374(12) 0.0706(16) 0.0014(11) 0.0109(10) 0.0114(9) O3 0.0523(14) 0.0374(13) 0.0831(19) -0.0082(12) 0.0011(12) 0.0056(10) O4 0.0419(12) 0.0368(12) 0.0699(16) -0.0034(10) 0.0052(10) 0.0063(9) O5 0.0755(18) 0.0369(13) 0.0728(18) -0.0048(12) 0.0153(14) 0.0034(12) O6 0.0606(14) 0.0356(12) 0.0627(15) -0.0005(10) 0.0132(11) 0.0073(10) O7 0.0566(14) 0.0323(12) 0.0810(19) 0.0023(11) 0.0169(12) 0.0034(10) O8 0.0549(13) 0.0329(11) 0.0637(15) 0.0051(10) 0.0140(11) 0.0039(9) C1 0.0492(18) 0.0406(17) 0.064(2) 0.0081(14) 0.0199(15) 0.0117(13) C2 0.0455(16) 0.0382(16) 0.065(2) 0.0110(14) 0.0182(14) 0.0140(13) C3 0.0447(16) 0.0415(17) 0.068(2) 0.0092(15) 0.0204(14) 0.0132(13) C4 0.0429(17) 0.052(2) 0.070(2) 0.0100(17) 0.0183(15) 0.0110(14) C5 0.0474(19) 0.060(2) 0.084(3) 0.014(2) 0.0183(18) 0.0199(16) C6 0.059(2) 0.0432(19) 0.090(3) 0.0159(19) 0.0226(19) 0.0223(16) C7 0.0537(19) 0.0353(17) 0.085(3) 0.0145(16) 0.0237(17) 0.0142(14) C8 0.0454(18) 0.059(2) 0.069(2) 0.0094(17) 0.0184(16) 0.0124(16) C9 0.0465(18) 0.062(2) 0.067(2) 0.0108(18) 0.0178(16) 0.0120(16) C10 0.0424(16) 0.061(2) 0.060(2) 0.0124(17) 0.0155(14) 0.0074(14) C11 0.0380(16) 0.063(2) 0.065(2) 0.0073(17) 0.0092(14) 0.0090(15) C12 0.0410(17) 0.063(2) 0.073(3) 0.0107(19) 0.0119(15) 0.0114(15) C13 0.0450(19) 0.064(3) 0.101(4) -0.001(2) 0.0080(19) 0.0072(17) C14 0.0410(19) 0.068(3) 0.114(4) 0.010(3) 0.010(2) 0.0154(18) C15 0.0467(19) 0.053(2) 0.093(3) 0.010(2) 0.0177(18) 0.0124(16) C16 0.0394(17) 0.065(2) 0.080(3) 0.008(2) 0.0072(16) 0.0088(16) C17 0.0423(17) 0.060(2) 0.069(2) 0.0057(18) 0.0067(15) 0.0048(15) C18 0.0426(16) 0.053(2) 0.058(2) 0.0082(15) 0.0079(13) 0.0050(14) C19 0.0434(16) 0.0458(18) 0.060(2) 0.0048(15) 0.0074(14) 0.0024(13) C20 0.0416(16) 0.0434(17) 0.061(2) 0.0036(14) 0.0060(13) 0.0010(13) C21 0.0522(19) 0.0442(19) 0.070(2) 0.0006(16) 0.0101(16) -0.0011(14) C22 0.0509(19) 0.061(2) 0.068(2) 0.0031(19) 0.0057(16) -0.0117(16) C23 0.0405(17) 0.065(2) 0.071(3) 0.0112(19) 0.0076(15) -0.0025(15) C24 0.0455(16) 0.0354(16) 0.063(2) 0.0018(14) 0.0075(14) 0.0051(12) C25 0.0441(16) 0.0405(17) 0.064(2) -0.0030(15) 0.0021(14) 0.0046(13) C26 0.0382(15) 0.0466(18) 0.061(2) -0.0043(14) 0.0042(13) 0.0052(12) C27 0.069(2) 0.0448(19) 0.060(2) -0.0023(16) 0.0115(17) 0.0087(16) C28 0.096(3) 0.051(2) 0.062(3) 0.0011(18) 0.027(2) 0.008(2) C29 0.074(3) 0.068(3) 0.062(3) -0.009(2) 0.0181(19) -0.002(2) C30 0.064(2) 0.062(3) 0.070(3) -0.016(2) 0.0155(19) -0.0007(19) C31 0.056(2) 0.051(2) 0.069(3) -0.0130(17) 0.0117(17) 0.0000(16) C321 0.064(6) 0.056(5) 0.066(6) -0.007(4) 0.015(5) -0.006(5) C331 0.097(8) 0.070(6) 0.054(5) -0.002(4) 0.033(5) 0.004(6) C341 0.125(9) 0.059(5) 0.056(5) 0.011(4) 0.043(6) 0.011(6) C351 0.138(10) 0.046(5) 0.072(6) 0.019(4) 0.059(7) 0.019(6) C361 0.166(12) 0.047(5) 0.061(6) 0.014(4) 0.051(7) 0.005(6) C371 0.178(15) 0.076(8) 0.069(7) 0.026(6) 0.042(8) 0.000(9) C381 0.164(14) 0.125(13) 0.061(7) 0.003(7) 0.052(8) -0.014(11) C391 0.147(12) 0.082(8) 0.070(7) 0.006(6) 0.046(7) 0.010(8) C322 0.050(5) 0.052(4) 0.052(5) -0.002(3) 0.012(4) -0.008(4) C332 0.072(6) 0.065(6) 0.055(5) -0.001(4) 0.023(4) -0.012(5) C342 0.087(6) 0.057(5) 0.050(5) 0.008(3) 0.025(4) 0.011(4) C352 0.093(7) 0.068(6) 0.055(5) 0.014(4) 0.029(5) 0.015(5) C362 0.128(9) 0.057(5) 0.052(5) 0.008(4) 0.027(5) 0.015(6) C372 0.190(14) 0.058(6) 0.050(6) 0.019(4) 0.046(7) 0.016(7) C382 0.256(19) 0.061(6) 0.043(5) 0.010(4) 0.073(9) 0.011(9) C392 0.143(11) 0.056(5) 0.056(6) 0.008(4) 0.036(6) 0.017(6) C401 0.157(12) 0.039(5) 0.079(7) 0.023(4) 0.058(8) 0.022(6) C411 0.109(8) 0.048(5) 0.084(7) 0.027(5) 0.045(6) 0.019(5) C421 0.095(7) 0.034(4) 0.094(8) 0.016(4) 0.044(7) 0.011(5) C431 0.112(10) 0.033(6) 0.105(11) 0.017(6) 0.048(8) 0.026(7) C441 0.071(2) 0.0343(17) 0.090(3) 0.0128(17) 0.037(2) 0.0172(16) C451 0.043(4) 0.038(6) 0.086(10) 0.016(5) 0.028(5) 0.005(3) C461 0.104(9) 0.035(5) 0.082(11) 0.024(6) 0.031(8) 0.003(5) C471 0.117(10) 0.040(5) 0.100(9) 0.015(5) 0.062(9) -0.003(6) C402 0.147(11) 0.058(6) 0.059(6) 0.013(4) 0.044(7) 0.025(7) C412 0.127(10) 0.052(5) 0.067(6) 0.020(4) 0.041(6) 0.019(6) C422 0.130(10) 0.041(5) 0.077(7) 0.012(4) 0.055(8) 0.018(7) C432 0.120(10) 0.029(5) 0.076(8) 0.021(5) 0.059(7) 0.030(6) C442 0.071(2) 0.0343(17) 0.090(3) 0.0128(17) 0.037(2) 0.0172(16) C452 0.133(15) 0.037(6) 0.070(9) -0.001(5) 0.048(9) 0.014(6) C462 0.19(3) 0.054(7) 0.071(10) 0.018(7) 0.066(13) 0.030(10) C472 0.22(2) 0.044(6) 0.116(14) 0.017(7) 0.119(16) 0.015(10) C48 0.0402(15) 0.0323(15) 0.076(2) 0.0072(14) 0.0145(14) 0.0071(12) O1D 0.127(3) 0.0375(15) 0.082(2) -0.0167(14) 0.019(2) 0.0067(16) N1D 0.254(9) 0.071(4) 0.111(5) -0.029(3) 0.079(5) -0.018(4) C1D 0.145(6) 0.066(3) 0.104(5) -0.004(3) 0.034(4) -0.016(3) C2D 0.43(2) 0.056(4) 0.120(7) -0.016(4) 0.084(9) 0.045(7) C3D 0.339(18) 0.109(7) 0.144(8) -0.059(6) 0.091(9) -0.028(8) O2D 0.0748(19) 0.0406(14) 0.095(2) -0.0203(14) 0.0322(16) -0.0148(12) N21D 0.054(3) 0.045(3) 0.075(4) -0.011(3) 0.003(3) -0.002(3) C41D 0.083(4) 0.065(3) 0.128(5) -0.018(3) 0.026(3) -0.004(3) C61D 0.059(5) 0.073(6) 0.103(8) 0.006(5) 0.012(5) 0.007(4) C42D 0.083(4) 0.065(3) 0.128(5) -0.018(3) 0.026(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.965(3) . ? Cu1 O7 1.968(3) . ? Cu1 O3 1.969(3) . ? Cu1 O5 1.983(3) . ? Cu1 O1D 2.130(3) . ? Cu1 Cu2 2.6409(7) . ? Cu2 O4 1.955(2) . ? Cu2 O6 1.957(3) . ? Cu2 O2 1.966(2) . ? Cu2 O8 1.972(3) . ? Cu2 O2D 2.151(3) . ? O1 C1 1.260(5) . ? O2 C1 1.262(4) . ? O3 C24 1.273(4) . ? O4 C24 1.259(4) . ? O5 C25 1.266(4) . ? O6 C25 1.261(4) . ? O7 C48 1.266(5) . ? O8 C48 1.265(4) . ? C1 C2 1.498(5) . ? C2 C3 1.370(5) . ? C2 C7 1.403(4) . ? C3 C4 1.395(5) . ? C4 C5 1.402(5) . ? C4 C8 1.432(6) . ? C5 C6 1.372(7) . ? C6 C7 1.392(5) . ? C8 C9 1.191(6) . ? C9 C10 1.448(6) . ? C10 C11 1.399(5) . ? C10 C15 1.405(5) . ? C11 C12 1.364(6) . ? C12 C13 1.414(5) . ? C12 C16 1.440(6) 7_556 ? C13 C14 1.390(6) . ? C14 C15 1.364(7) . ? C16 C17 1.209(6) . ? C16 C12 1.440(6) 7_556 ? C17 C18 1.422(5) . ? C18 C19 1.399(5) . ? C18 C23 1.403(6) . ? C19 C20 1.388(5) . ? C20 C21 1.398(5) . ? C20 C24 1.511(5) . ? C21 C22 1.396(5) . ? C22 C23 1.384(6) . ? C25 C26 1.490(6) . ? C26 C27 1.376(5) . ? C26 C31 1.402(5) . ? C27 C28 1.394(6) . ? C28 C29 1.390(6) . ? C28 C322 1.421(11) . ? C28 C321 1.484(12) . ? C29 C30 1.370(7) . ? C30 C31 1.379(6) . ? C321 C331 1.202(15) . ? C331 C341 1.426(14) . ? C341 C391 1.379(12) . ? C341 C351 1.389(12) . ? C351 C361 1.384(11) . ? C361 C371 1.387(12) . ? C361 C401 1.453(16) 7_556 ? C371 C381 1.385(14) . ? C381 C391 1.382(14) . ? C322 C332 1.235(14) . ? C332 C342 1.431(13) . ? C342 C352 1.386(11) . ? C342 C392 1.392(11) . ? C352 C362 1.399(11) . ? C362 C372 1.387(11) . ? C362 C402 1.411(15) 7_556 ? C372 C382 1.365(12) . ? C382 C392 1.406(12) . ? C401 C411 1.227(17) . ? C401 C361 1.453(16) 7_556 ? C411 C421 1.404(17) . ? C421 C431 1.395(16) . ? C421 C471 1.399(13) . ? C431 C441 1.383(16) . ? C441 C451 1.421(12) . ? C441 C48 1.491(6) . ? C451 C461 1.402(15) . ? C461 C471 1.406(16) . ? C402 C412 1.221(16) . ? C402 C362 1.411(15) 7_556 ? C412 C422 1.446(17) . ? C422 C472 1.385(13) . ? C422 C432 1.424(14) . ? C452 C462 1.388(16) . ? C462 C472 1.420(17) . ? O1D C1D 1.179(7) . ? N1D C1D 1.368(8) . ? N1D C3D 1.384(11) . ? N1D C2D 1.385(11) . ? O2D C41D 1.265(7) . ? N21D C41D 1.329(9) . ? N21D C61D 1.450(13) . ? N21D C51D 1.547(15) . ? N22D C62D 1.43(2) . ? 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 O7 88.47(13) . . ? O1 Cu1 O3 169.13(11) . . ? O7 Cu1 O3 89.31(12) . . ? O1 Cu1 O5 89.48(13) . . ? O7 Cu1 O5 166.85(11) . . ? O3 Cu1 O5 90.26(13) . . ? O1 Cu1 O1D 91.03(14) . . ? O7 Cu1 O1D 100.47(13) . . ? O3 Cu1 O1D 99.84(14) . . ? O5 Cu1 O1D 92.55(13) . . ? O1 Cu1 Cu2 85.07(8) . . ? O7 Cu1 Cu2 85.62(8) . . ? O3 Cu1 Cu2 84.15(8) . . ? O5 Cu1 Cu2 81.26(8) . . ? O1D Cu1 Cu2 172.70(11) . . ? O4 Cu2 O6 89.13(12) . . ? O4 Cu2 O2 167.09(10) . . ? O6 Cu2 O2 89.38(11) . . ? O4 Cu2 O8 90.20(11) . . ? O6 Cu2 O8 169.53(10) . . ? O2 Cu2 O8 88.95(11) . . ? O4 Cu2 O2D 102.63(11) . . ? O6 Cu2 O2D 94.66(12) . . ? O2 Cu2 O2D 90.28(12) . . ? O8 Cu2 O2D 95.69(12) . . ? O4 Cu2 Cu1 84.32(7) . . ? O6 Cu2 Cu1 86.80(8) . . ? O2 Cu2 Cu1 82.79(8) . . ? O8 Cu2 Cu1 82.74(8) . . ? O2D Cu2 Cu1 172.90(10) . . ? C1 O1 Cu1 121.2(2) . . ? C1 O2 Cu2 123.8(2) . . ? C24 O3 Cu1 121.8(2) . . ? C24 O4 Cu2 122.7(2) . . ? C25 O5 Cu1 125.1(3) . . ? C25 O6 Cu2 119.9(2) . . ? C48 O7 Cu1 120.5(2) . . ? C48 O8 Cu2 123.8(3) . . ? O1 C1 O2 125.7(3) . . ? O1 C1 C2 118.5(3) . . ? O2 C1 C2 115.8(3) . . ? C3 C2 C7 120.1(3) . . ? C3 C2 C1 119.8(3) . . ? C7 C2 C1 120.1(3) . . ? C2 C3 C4 121.2(3) . . ? C3 C4 C5 118.3(4) . . ? C3 C4 C8 120.1(3) . . ? C5 C4 C8 121.7(3) . . ? C6 C5 C4 120.9(4) . . ? C5 C6 C7 120.4(3) . . ? C6 C7 C2 119.1(4) . . ? C9 C8 C4 176.9(4) . . ? C8 C9 C10 177.9(4) . . ? C11 C10 C15 119.0(4) . . ? C11 C10 C9 121.2(3) . . ? C15 C10 C9 119.8(4) . . ? C12 C11 C10 121.3(3) . . ? C11 C12 C13 119.3(4) . . ? C11 C12 C16 121.6(3) . 7_556 ? C13 C12 C16 119.1(4) . 7_556 ? C14 C13 C12 119.4(4) . . ? C15 C14 C13 121.1(4) . . ? C14 C15 C10 119.9(4) . . ? C17 C16 C12 179.0(4) . 7_556 ? C16 C17 C18 177.0(4) . . ? C19 C18 C23 119.0(4) . . ? C19 C18 C17 121.9(4) . . ? C23 C18 C17 119.1(3) . . ? C20 C19 C18 120.7(3) . . ? C19 C20 C21 119.9(3) . . ? C19 C20 C24 119.5(3) . . ? C21 C20 C24 120.6(3) . . ? C22 C21 C20 119.7(4) . . ? C23 C22 C21 120.4(4) . . ? C22 C23 C18 120.3(3) . . ? O4 C24 O3 126.2(3) . . ? O4 C24 C20 116.9(3) . . ? O3 C24 C20 116.9(3) . . ? O6 C25 O5 125.6(4) . . ? O6 C25 C26 117.1(3) . . ? O5 C25 C26 117.3(3) . . ? C27 C26 C31 119.9(4) . . ? C27 C26 C25 120.4(3) . . ? C31 C26 C25 119.7(3) . . ? C26 C27 C28 120.9(4) . . ? C29 C28 C27 118.4(4) . . ? C29 C28 C322 119.6(5) . . ? C27 C28 C322 120.3(5) . . ? C29 C28 C321 119.1(6) . . ? C27 C28 C321 120.8(6) . . ? C322 C28 C321 26.2(4) . . ? C30 C29 C28 121.0(4) . . ? C29 C30 C31 120.7(4) . . ? C30 C31 C26 119.1(4) . . ? C331 C321 C28 169.0(13) . . ? C321 C331 C341 177.4(10) . . ? C391 C341 C351 119.7(9) . . ? C391 C341 C331 118.8(9) . . ? C351 C341 C331 121.4(8) . . ? C361 C351 C341 120.2(9) . . ? C351 C361 C371 120.7(10) . . ? C351 C361 C401 120.7(8) . 7_556 ? C371 C361 C401 118.5(9) . 7_556 ? C381 C371 C361 118.0(11) . . ? C391 C381 C371 122.0(11) . . ? C341 C391 C381 119.3(11) . . ? C332 C322 C28 173.6(10) . . ? C322 C332 C342 176.6(11) . . ? C352 C342 C392 120.0(8) . . ? C352 C342 C332 121.7(8) . . ? C392 C342 C332 118.3(8) . . ? C342 C352 C362 122.5(8) . . ? C372 C362 C352 117.1(9) . . ? C372 C362 C402 120.8(9) . 7_556 ? C352 C362 C402 121.8(8) . 7_556 ? C382 C372 C362 120.7(9) . . ? C372 C382 C392 122.7(9) . . ? C342 C392 C382 116.9(9) . . ? C411 C401 C361 175.9(17) . 7_556 ? C401 C411 C421 174.9(14) . . ? C431 C421 C471 121.9(14) . . ? C431 C421 C411 115.7(11) . . ? C471 C421 C411 122.1(11) . . ? C441 C431 C421 118.2(16) . . ? C431 C441 C451 124.3(12) . . ? C431 C441 C48 119.6(9) . . ? C451 C441 C48 114.5(9) . . ? C461 C451 C441 112.5(15) . . ? C451 C461 C471 126.5(16) . . ? C421 C471 C461 115.6(14) . . ? C412 C402 C362 175.0(16) . 7_556 ? C402 C412 C422 177.2(11) . . ? C472 C422 C432 113.9(14) . . ? C472 C422 C412 122.8(11) . . ? C432 C422 C412 123.0(10) . . ? C452 C462 C472 116(2) . . ? C422 C472 C462 125.1(17) . . ? O8 C48 O7 126.1(4) . . ? O8 C48 C441 116.5(4) . . ? O7 C48 C441 117.4(3) . . ? C1D O1D Cu1 126.2(4) . . ? C1D N1D C3D 122.9(8) . . ? C1D N1D C2D 120.7(7) . . ? C3D N1D C2D 116.4(7) . . ? O1D C1D N1D 125.2(7) . . ? C41D O2D Cu2 124.0(3) . . ? C41D N21D C61D 117.8(7) . . ? C41D N21D C51D 108.0(8) . . ? C61D N21D C51D 133.5(9) . . ? O2D C41D N21D 135.7(7) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.337 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.098 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 1 0.849 0.431 0.250 1591.5 78.2 2 0.338 0.058 0.750 1591.5 78.3 _platon_squeeze_details ; ; #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 744145' #TrackingRef 'mslah_rev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72.25 H76.50 Cu2 N7.50 O17.75' _chemical_formula_weight 1460.99 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 p2(1)/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 13.187(3) _cell_length_b 29.985(6) _cell_length_c 18.713(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.93(3) _cell_angle_gamma 90.00 _cell_volume 7382(3) _cell_formula_units_Z 4 _cell_measurement_temperature 99(2) _cell_measurement_reflns_used 81351 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 31.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3050 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.7954 _exptl_absorpt_correction_T_max 0.8293 _exptl_absorpt_process_details 'hkl2000 scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 99(2) _diffrn_radiation_wavelength 0.75000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'bending magnet 6b mx beamline' _diffrn_radiation_monochromator 'si(111) double crystal monochromator' _diffrn_measurement_device_type 'ccd area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61282 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 31.00 _reflns_number_total 19718 _reflns_number_gt 16424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'adsc quantum-210 adx program' _computing_cell_refinement hkl2000 _computing_data_reduction hkl2000 _computing_structure_solution 'wingx sir-92' _computing_structure_refinement 'bruker shelxtl' _computing_molecular_graphics ortep3 _computing_publication_material wingx _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^)+(0.1278P)^2^+7.5494P] 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 0.0191(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 19718 _refine_ls_number_parameters 983 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2153 _refine_ls_wR_factor_gt 0.2019 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.003 _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 0.55079(3) 0.835320(10) 0.713534(15) 0.03293(11) Uani 1 1 d . . . Cu2 Cu 0.54325(3) 0.896908(10) 0.812182(15) 0.03305(11) Uani 1 1 d . . . O1 O 0.58379(19) 0.79530(7) 0.79462(10) 0.0444(5) Uani 1 1 d . . . O2 O 0.58558(18) 0.84937(7) 0.87827(10) 0.0424(4) Uani 1 1 d . B . O3 O 0.51839(16) 0.88544(6) 0.64690(10) 0.0368(4) Uani 1 1 d . . . O4 O 0.50133(19) 0.93679(7) 0.73267(10) 0.0435(5) Uani 1 1 d . B . O9 O 0.76642(19) 0.69379(7) 1.07086(10) 0.0472(5) Uani 1 1 d . . . O10 O 0.2818(2) 1.03812(8) 0.47330(12) 0.0563(6) Uani 1 1 d . . . C1 C 0.5993(2) 0.80975(9) 0.85790(14) 0.0371(5) Uani 1 1 d . B . C2 C 0.6383(2) 0.77757(9) 0.91391(14) 0.0372(5) Uani 1 1 d . . . C3 C 0.6575(2) 0.79181(9) 0.98418(14) 0.0360(5) Uani 1 1 d . B . H3 H 0.6414 0.8216 0.9965 0.043 Uiso 1 1 calc R . . C4 C 0.6997(2) 0.76343(9) 1.03674(13) 0.0369(5) Uani 1 1 d . . . C5 C 0.7226(2) 0.71907(10) 1.01768(14) 0.0416(6) Uani 1 1 d . B . C6 C 0.7017(3) 0.70442(10) 0.94705(15) 0.0467(7) Uani 1 1 d . . . H6 H 0.7159 0.6745 0.9343 0.056 Uiso 1 1 calc R B . C7 C 0.6603(3) 0.73366(10) 0.89628(15) 0.0430(6) Uani 1 1 d . B . H7 H 0.6465 0.7237 0.8484 0.052 Uiso 1 1 calc R . . C8 C 0.7250(2) 0.77888(9) 1.10815(14) 0.0379(5) Uani 1 1 d . B . C9 C 0.7477(2) 0.79323(9) 1.16703(14) 0.0385(5) Uani 1 1 d . . . C10 C 0.7764(2) 0.80834(9) 1.23797(14) 0.0384(5) Uani 1 1 d . B . C11 C 0.7347(2) 0.84754(10) 1.26459(15) 0.0413(6) Uani 1 1 d . . . H11 H 0.6870 0.8643 1.2352 0.050 Uiso 1 1 calc R B . C12 C 0.7630(3) 0.86211(10) 1.33418(15) 0.0440(6) Uani 1 1 d . . . C13 C 0.8340(3) 0.83714(11) 1.37692(16) 0.0492(7) Uani 1 1 d . . . H13 H 0.8539 0.8468 1.4241 0.059 Uiso 1 1 calc R B . C14 C 0.8750(3) 0.79865(11) 1.35062(16) 0.0492(7) Uani 1 1 d . B . H14 H 0.9226 0.7819 1.3801 0.059 Uiso 1 1 calc R . . C15 C 0.8475(2) 0.78404(10) 1.28158(15) 0.0429(6) Uani 1 1 d . . . H15 H 0.8768 0.7576 1.2639 0.052 Uiso 1 1 calc R B . C16 C 0.2804(3) 1.09811(11) 0.63806(16) 0.0480(7) Uani 1 1 d . . . C17 C 0.3154(3) 1.06507(10) 0.61327(15) 0.0462(7) Uani 1 1 d . . . C18 C 0.3580(2) 1.02469(9) 0.58807(15) 0.0403(6) Uani 1 1 d . . . C19 C 0.4137(2) 0.99661(9) 0.63562(14) 0.0376(5) Uani 1 1 d . B . H19 H 0.4270 1.0057 0.6840 0.045 Uiso 1 1 calc R . . C20 C 0.4502(2) 0.95571(9) 0.61376(13) 0.0345(5) Uani 1 1 d . . . C21 C 0.4350(2) 0.94342(9) 0.54206(14) 0.0359(5) Uani 1 1 d . B . H21 H 0.4624 0.9161 0.5263 0.043 Uiso 1 1 calc R . . C22 C 0.3805(2) 0.97044(9) 0.49351(14) 0.0396(6) Uani 1 1 d . . . H22 H 0.3707 0.9616 0.4448 0.048 Uiso 1 1 calc R B . C23 C 0.3400(3) 1.01062(9) 0.51576(15) 0.0421(6) Uani 1 1 d . B . C24 C 0.4944(2) 0.92370(9) 0.66827(13) 0.0348(5) Uani 1 1 d . B . C49 C 0.8036(3) 0.65065(11) 1.05143(17) 0.0504(7) Uani 1 1 d . . . H49A H 0.7463 0.6317 1.0345 0.076 Uiso 1 1 calc R . . H49B H 0.8395 0.6368 1.0933 0.076 Uiso 1 1 calc R . . H49C H 0.8503 0.6540 1.0133 0.076 Uiso 1 1 calc R . . C50 C 0.2540(4) 1.02328(13) 0.40184(18) 0.0654(11) Uani 1 1 d . . . H50A H 0.3148 1.0216 0.3747 0.098 Uiso 1 1 calc R . . H50B H 0.2055 1.0443 0.3785 0.098 Uiso 1 1 calc R . . H50C H 0.2226 0.9937 0.4035 0.098 Uiso 1 1 calc R . . O5 O 0.40467(16) 0.82998(7) 0.72948(10) 0.0399(4) Uani 1 1 d . . . O6 O 0.40099(16) 0.87967(7) 0.81893(11) 0.0423(4) Uani 1 1 d . B . O7 O 0.69550(16) 0.85084(7) 0.71112(11) 0.0408(4) Uani 1 1 d . . . O8 O 0.68490(17) 0.90602(8) 0.79129(11) 0.0447(5) Uani 1 1 d . B . O11 O -0.04956(17) 0.80888(8) 0.81475(12) 0.0457(5) Uani 1 1 d . . . O12 O 1.12288(18) 0.94896(8) 0.70278(13) 0.0522(5) Uani 1 1 d . . . C25 C 0.3598(2) 0.85072(9) 0.77684(13) 0.0360(5) Uani 1 1 d . B . C26 C 0.2511(2) 0.84028(9) 0.78428(14) 0.0363(5) Uani 1 1 d . . . C27 C 0.1976(2) 0.86118(9) 0.83709(14) 0.0378(5) Uani 1 1 d . B . H27 H 0.2307 0.8829 0.8674 0.045 Uiso 1 1 calc R . . C28 C 0.0968(2) 0.85054(9) 0.84555(14) 0.0385(5) Uani 1 1 d . . . C29 C 0.0480(2) 0.81756(10) 0.80109(15) 0.0402(6) Uani 1 1 d . B . C30 C 0.1004(2) 0.79739(10) 0.74777(15) 0.0408(6) Uani 1 1 d . . . H30 H 0.0676 0.7758 0.7170 0.049 Uiso 1 1 calc R B . C31 C 0.2010(2) 0.80895(9) 0.73979(14) 0.0394(6) Uani 1 1 d . B . H31 H 0.2363 0.7952 0.7031 0.047 Uiso 1 1 calc R . . C32 C 0.0416(2) 0.87159(10) 0.89946(15) 0.0417(6) Uani 1 1 d . B . C33 C -0.0072(2) 0.88816(11) 0.94396(16) 0.0443(6) Uani 1 1 d . . . C34 C -0.0659(3) 0.90393(11) 1.00019(17) 0.0456(7) Uani 1 1 d . B . C35 C -0.0311(2) 0.93876(10) 1.04481(16) 0.0436(6) Uani 1 1 d . . . H35 H 0.0286 0.9545 1.0345 0.052 Uiso 1 1 calc R B . C36 C -0.0829(3) 0.95059(11) 1.10405(18) 0.0493(7) Uani 1 1 d . . . C37 C -0.1703(3) 0.92737(12) 1.1191(2) 0.0579(9) Uani 1 1 d . . . H37 H -0.2043 0.9343 1.1608 0.069 Uiso 1 1 calc R B . C38 C -0.2073(3) 0.89423(13) 1.0735(2) 0.0652(11) Uani 1 1 d . B . H38 H -0.2684 0.8793 1.0831 0.078 Uiso 1 1 calc R . . C39 C -0.1571(3) 0.88234(13) 1.0140(2) 0.0620(10) Uani 1 1 d . . . H39 H -0.1840 0.8597 0.9826 0.074 Uiso 1 1 calc R B . C40 C 1.0470(3) 1.01330(11) 0.84990(18) 0.0511(7) Uani 1 1 d . . . C41 C 1.0177(3) 0.98365(11) 0.81115(18) 0.0487(7) Uani 1 1 d . . . C42 C 0.9758(2) 0.94881(10) 0.76631(16) 0.0433(6) Uani 1 1 d . . . C43 C 0.8802(2) 0.93219(10) 0.77753(15) 0.0415(6) Uani 1 1 d . B . H43 H 0.8438 0.9441 0.8152 0.050 Uiso 1 1 calc R . . C44 C 0.8364(2) 0.89850(9) 0.73490(14) 0.0369(5) Uani 1 1 d . . . C45 C 0.8908(2) 0.88105(10) 0.67992(15) 0.0394(6) Uani 1 1 d . B . H45 H 0.8618 0.8578 0.6507 0.047 Uiso 1 1 calc R . . C46 C 0.9867(2) 0.89713(10) 0.66727(16) 0.0418(6) Uani 1 1 d . . . H46 H 1.0226 0.8852 0.6294 0.050 Uiso 1 1 calc R B . C47 C 1.0299(2) 0.93088(10) 0.71045(16) 0.0424(6) Uani 1 1 d . B . C48 C 0.7315(2) 0.88368(9) 0.74651(14) 0.0374(5) Uani 1 1 d . B . C51 C -0.1032(3) 0.77550(12) 0.7720(2) 0.0533(8) Uani 1 1 d . . . H51A H -0.0975 0.7821 0.7211 0.080 Uiso 1 1 calc R . . H51B H -0.1750 0.7755 0.7824 0.080 Uiso 1 1 calc R . . H51C H -0.0737 0.7461 0.7832 0.080 Uiso 1 1 calc R . . C52 C 1.1824(3) 0.92935(13) 0.6492(2) 0.0546(8) Uani 1 1 d . . . H52A H 1.1922 0.8975 0.6593 0.082 Uiso 1 1 calc R . . H52B H 1.2487 0.9442 0.6498 0.082 Uiso 1 1 calc R . . H52C H 1.1467 0.9330 0.6018 0.082 Uiso 1 1 calc R . . O1L O 0.5585(2) 0.78421(8) 0.63486(12) 0.0557(6) Uani 1 1 d . . . N1L N 0.5327(4) 0.74431(15) 0.5341(2) 0.0345(9) Uani 0.50 1 d P A 1 C1L C 0.5065(4) 0.76916(15) 0.5890(2) 0.0297(9) Uani 0.50 1 d P A 1 H1L H 0.4360 0.7752 0.5905 0.036 Uiso 0.50 1 calc PR A 1 C2L C 0.6361(5) 0.73167(19) 0.5243(3) 0.0402(11) Uani 0.50 1 d P A 1 H2L1 H 0.6791 0.7396 0.5672 0.060 Uiso 0.50 1 calc PR A 1 H2L2 H 0.6600 0.7474 0.4828 0.060 Uiso 0.50 1 calc PR A 1 H2L3 H 0.6395 0.6994 0.5163 0.060 Uiso 0.50 1 calc PR A 1 C3L C 0.4574(6) 0.7343(2) 0.4744(4) 0.0492(14) Uani 0.50 1 d P A 1 H3L1 H 0.3889 0.7402 0.4894 0.074 Uiso 0.50 1 calc PR A 1 H3L2 H 0.4629 0.7029 0.4609 0.074 Uiso 0.50 1 calc PR A 1 H3L3 H 0.4704 0.7532 0.4332 0.074 Uiso 0.50 1 calc PR A 1 N12L N 0.5244(12) 0.7134(5) 0.6096(9) 0.072(4) Uiso 0.25 1 d P A 2 C12L C 0.5543(16) 0.7471(6) 0.6522(9) 0.071(4) Uani 0.25 1 d P A 2 H12L H 0.5739 0.7402 0.7007 0.085 Uiso 0.25 1 calc PR A 2 C22L C 0.4763(17) 0.7188(8) 0.5383(12) 0.077(5) Uiso 0.25 1 d P A 2 H22A H 0.4139 0.7363 0.5407 0.116 Uiso 0.25 1 calc PR A 2 H22B H 0.4596 0.6894 0.5178 0.116 Uiso 0.25 1 calc PR A 2 H22C H 0.5228 0.7343 0.5080 0.116 Uiso 0.25 1 calc PR A 2 C32L C 0.526(2) 0.6667(8) 0.6364(14) 0.094(6) Uiso 0.25 1 d P A 2 H32A H 0.5931 0.6537 0.6313 0.141 Uiso 0.25 1 calc PR A 2 H32B H 0.4744 0.6492 0.6086 0.141 Uiso 0.25 1 calc PR A 2 H32C H 0.5111 0.6665 0.6870 0.141 Uiso 0.25 1 calc PR A 2 N13L N 0.5492(17) 0.7747(8) 0.5102(12) 0.100(6) Uiso 0.25 1 d P A 3 C13L C 0.568(2) 0.7983(8) 0.5681(11) 0.104(9) Uani 0.25 1 d P A 3 H13L H 0.5905 0.8281 0.5621 0.124 Uiso 0.25 1 calc PR A 3 C23L C 0.4887(19) 0.7354(8) 0.5111(16) 0.073(5) Uiso 0.25 1 d P A 3 H23A H 0.5330 0.7092 0.5144 0.109 Uiso 0.25 1 calc PR A 3 H23B H 0.4442 0.7339 0.4671 0.109 Uiso 0.25 1 calc PR A 3 H23C H 0.4473 0.7363 0.5526 0.109 Uiso 0.25 1 calc PR A 3 C33L C 0.630(4) 0.7703(16) 0.449(2) 0.175(16) Uiso 0.25 1 d P A 3 H33A H 0.6894 0.7892 0.4615 0.263 Uiso 0.25 1 calc PR A 3 H33B H 0.5981 0.7799 0.4026 0.263 Uiso 0.25 1 calc PR A 3 H33C H 0.6522 0.7392 0.4454 0.263 Uiso 0.25 1 calc PR A 3 O21L O 0.54996(19) 0.94924(8) 0.89218(12) 0.0510(5) Uani 0.50 1 d P B 1 N21L N 0.6834(5) 0.9953(2) 0.8974(4) 0.0616(16) Uani 0.50 1 d P B 1 C41L C 0.6301(3) 0.96388(14) 0.9172(2) 0.0634(9) Uani 0.50 1 d P B 1 H41L H 0.6570 0.9489 0.9591 0.076 Uiso 0.50 1 calc PR B 1 C51L C 0.7642(6) 1.0119(3) 0.9587(5) 0.126(2) Uiso 0.50 1 d P B 1 C61L C 0.6621(8) 1.0120(3) 0.8296(5) 0.076(2) Uani 0.50 1 d P B 1 H61A H 0.6054 0.9953 0.8059 0.114 Uiso 0.50 1 calc PR B 1 H61B H 0.7221 1.0091 0.8019 0.114 Uiso 0.50 1 calc PR B 1 H61C H 0.6434 1.0436 0.8328 0.114 Uiso 0.50 1 calc PR B 1 O22L O 0.54996(19) 0.94924(8) 0.89218(12) 0.0510(5) Uani 0.50 1 d P B 2 N22L N 0.6566(5) 0.9993(2) 0.9535(3) 0.0572(14) Uani 0.50 1 d P B 2 C42L C 0.6301(3) 0.96388(14) 0.9172(2) 0.0634(9) Uani 0.50 1 d P B 2 H42L H 0.6862 0.9453 0.9083 0.076 Uiso 0.50 1 calc PR B 2 C52L C 0.7642(6) 1.0119(3) 0.9587(5) 0.126(2) Uiso 0.50 1 d P B 2 C62L C 0.5843(16) 1.0296(7) 0.9693(11) 0.157(7) Uiso 0.50 1 d P B 2 H62A H 0.5380 1.0347 0.9269 0.236 Uiso 0.50 1 calc PR B 2 H62B H 0.6172 1.0577 0.9841 0.236 Uiso 0.50 1 calc PR B 2 H62C H 0.5459 1.0181 1.0084 0.236 Uiso 0.50 1 calc PR B 2 O1S O -0.0588(4) 0.1117(2) 0.5039(3) 0.142(2) Uani 1 1 d . . . N1S N -0.0018(5) 0.06924(19) 0.5911(4) 0.1143(18) Uani 1 1 d . . . C1S C -0.0478(7) 0.1022(3) 0.5652(4) 0.127(3) Uani 1 1 d . . . H1S H -0.0771 0.1218 0.5979 0.153 Uiso 1 1 calc R . . C2S C 0.0440(12) 0.0354(6) 0.5530(8) 0.243(7) Uiso 1 1 d . . . H2S1 H 0.0025 0.0292 0.5087 0.365 Uiso 1 1 calc R . . H2S2 H 0.0495 0.0083 0.5824 0.365 Uiso 1 1 calc R . . H2S3 H 0.1120 0.0450 0.5414 0.365 Uiso 1 1 calc R . . C3S C 0.0103(8) 0.0593(4) 0.6627(5) 0.151(3) Uiso 1 1 d . . . H3S1 H 0.0762 0.0705 0.6825 0.227 Uiso 1 1 calc R . . H3S2 H 0.0074 0.0269 0.6692 0.227 Uiso 1 1 calc R . . H3S3 H -0.0442 0.0734 0.6878 0.227 Uiso 1 1 calc R . . O2S O 0.7497(4) 0.62113(19) 0.6175(3) 0.0964(15) Uiso 0.75 1 d P C 1 N2S N 0.6471(3) 0.66521(14) 0.6786(2) 0.0526(9) Uani 0.75 1 d P C 1 C4S C 0.6679(5) 0.63024(19) 0.6397(3) 0.0664(13) Uani 0.75 1 d P C 1 H4S H 0.6136 0.6102 0.6278 0.080 Uiso 0.75 1 calc PR C 1 C5S C 0.7268(5) 0.6952(2) 0.7043(3) 0.0694(14) Uani 0.75 1 d P C 1 H5S1 H 0.7451 0.6892 0.7550 0.104 Uiso 0.75 1 calc PR C 1 H5S2 H 0.7032 0.7261 0.6985 0.104 Uiso 0.75 1 calc PR C 1 H5S3 H 0.7865 0.6907 0.6767 0.104 Uiso 0.75 1 calc PR C 1 C6S C 0.5484(4) 0.6715(2) 0.7055(4) 0.0761(17) Uani 0.75 1 d P C 1 H6S1 H 0.4994 0.6514 0.6802 0.114 Uiso 0.75 1 calc PR C 1 H6S2 H 0.5267 0.7024 0.6978 0.114 Uiso 0.75 1 calc PR C 1 H6S3 H 0.5518 0.6647 0.7569 0.114 Uiso 0.75 1 calc PR C 1 O3S O 0.5385(5) 0.2311(2) 0.8857(3) 0.1431(19) Uiso 0.50 1 d P D 1 N3S N 0.5640(4) 0.1714(2) 0.9566(3) 0.1066(18) Uani 0.50 1 d P D 1 C7S C 0.5269(6) 0.1857(3) 0.8974(3) 0.078(2) Uani 0.706(9) 1 d P D 1 H7S H 0.4930 0.1668 0.8628 0.093 Uiso 0.706(9) 1 calc PR D 1 C8S C 0.5437(8) 0.1191(3) 0.9729(5) 0.107(3) Uani 0.706(9) 1 d P D 1 C9S C 0.6210(5) 0.1890(3) 1.0165(4) 0.077(2) Uani 0.706(9) 1 d P D 1 O32S O 0.5385(5) 0.2311(2) 0.8857(3) 0.1431(19) Uiso 0.50 1 d P D 2 N32S N 0.5640(4) 0.1714(2) 0.9566(3) 0.1066(18) Uani 0.50 1 d P D 2 C72S C 0.5777(13) 0.2219(6) 0.9507(10) 0.078(5) Uiso 0.294(9) 1 d P D 2 H72S H 0.6074 0.2418 0.9856 0.093 Uiso 0.294(9) 1 calc PR D 2 C82S C 0.5243(13) 0.1510(7) 0.8970(10) 0.078(5) Uiso 0.294(9) 1 d P D 2 C92S C 0.6307(17) 0.1562(9) 1.0114(12) 0.094(6) Uiso 0.294(9) 1 d P D 2 N1A N 0.5851(3) -0.05632(15) 0.1750(3) 0.0846(11) Uani 1 1 d . . . C1A C 0.6274(4) -0.02218(17) 0.1727(3) 0.0768(12) Uani 1 1 d . . . C2A C 0.6823(3) 0.01941(15) 0.1758(3) 0.0821(15) Uani 1 1 d . . . H2A1 H 0.6394 0.0428 0.1944 0.123 Uiso 1 1 calc R . . H2A2 H 0.7007 0.0275 0.1276 0.123 Uiso 1 1 calc R . . H2A3 H 0.7442 0.0162 0.2075 0.123 Uiso 1 1 calc R . . N2A N 0.5291(4) 0.83947(19) 0.4479(3) 0.0741(13) Uani 0.75 1 d P E 1 C3A C 0.6010(4) 0.84450(17) 0.4837(3) 0.0553(11) Uani 0.75 1 d P E 1 C4A C 0.6924(4) 0.85139(17) 0.5313(2) 0.0549(11) Uani 0.75 1 d P E 1 O4S O 0.7840(8) 1.1082(4) 0.6565(6) 0.129(4) Uani 0.50 1 d P F 2 N4S N 0.6689(7) 1.0716(3) 0.7202(5) 0.088(2) Uiso 0.50 1 d PD F 2 C10S C 0.7639(12) 1.0811(5) 0.6985(8) 0.112(4) Uiso 0.50 1 d P F 2 H10S H 0.8187 1.0639 0.7196 0.134 Uiso 0.50 1 calc PR F 2 C11S C 0.5829(12) 1.0979(5) 0.6974(9) 0.119(5) Uiso 0.50 1 d PD F 2 H11A H 0.5454 1.0832 0.6569 0.178 Uiso 0.50 1 calc PR F 2 H11B H 0.6055 1.1274 0.6825 0.178 Uiso 0.50 1 calc PR F 2 H11C H 0.5385 1.1011 0.7370 0.178 Uiso 0.50 1 calc PR F 2 C12S C 0.6607(11) 1.0387(5) 0.7647(7) 0.103(4) Uani 0.50 1 d P F 2 H12A H 0.6925 1.0120 0.7460 0.155 Uiso 0.50 1 calc PR F 2 H12B H 0.5887 1.0327 0.7706 0.155 Uiso 0.50 1 calc PR F 2 H12C H 0.6947 1.0465 0.8112 0.155 Uiso 0.50 1 calc PR F 2 N3A N 0.7079(14) 1.1028(6) 0.6565(10) 0.148(6) Uiso 0.50 1 d PDU G 1 C5A C 0.6429(12) 1.1063(5) 0.6872(9) 0.110(4) Uiso 0.50 1 d PDU G 1 C6A C 0.5543(10) 1.1228(5) 0.7194(7) 0.101(4) Uiso 0.50 1 d PDU G 1 O1W O 0.0680(5) 0.1892(2) 0.4594(4) 0.0748(16) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0458(2) 0.02956(17) 0.02383(16) 0.00019(10) 0.00547(12) -0.00025(12) Cu2 0.0447(2) 0.03088(17) 0.02401(16) -0.00016(11) 0.00532(12) -0.00057(12) O1 0.0695(14) 0.0357(10) 0.0275(9) 0.0028(7) -0.0008(9) 0.0006(9) O2 0.0619(12) 0.0378(10) 0.0274(8) 0.0034(7) 0.0035(8) 0.0071(9) O3 0.0497(10) 0.0320(9) 0.0293(8) 0.0023(7) 0.0064(7) 0.0029(8) O4 0.0697(13) 0.0328(9) 0.0275(9) 0.0003(7) 0.0002(8) 0.0025(9) O9 0.0732(14) 0.0399(10) 0.0288(9) 0.0046(8) 0.0059(9) 0.0199(10) O10 0.0908(18) 0.0420(12) 0.0349(10) 0.0016(9) -0.0040(11) 0.0222(12) C1 0.0485(14) 0.0350(12) 0.0282(11) 0.0045(10) 0.0048(10) 0.0015(11) C2 0.0486(14) 0.0346(12) 0.0290(11) 0.0030(10) 0.0058(10) 0.0004(11) C3 0.0450(13) 0.0324(12) 0.0314(12) 0.0025(9) 0.0074(10) 0.0020(10) C4 0.0489(14) 0.0358(12) 0.0269(11) 0.0015(9) 0.0078(10) 0.0038(11) C5 0.0570(16) 0.0398(14) 0.0285(12) 0.0058(10) 0.0071(11) 0.0094(12) C6 0.073(2) 0.0364(14) 0.0316(13) 0.0014(11) 0.0074(12) 0.0111(13) C7 0.0640(18) 0.0375(14) 0.0274(11) 0.0009(10) 0.0029(11) 0.0036(12) C8 0.0513(15) 0.0320(12) 0.0312(12) 0.0036(10) 0.0083(10) 0.0052(11) C9 0.0529(15) 0.0324(12) 0.0310(12) 0.0026(10) 0.0088(10) 0.0054(11) C10 0.0532(15) 0.0341(12) 0.0285(11) 0.0015(10) 0.0073(10) 0.0043(11) C11 0.0576(16) 0.0351(13) 0.0318(12) 0.0013(10) 0.0062(11) 0.0062(12) C12 0.0635(18) 0.0363(13) 0.0331(13) -0.0020(11) 0.0089(12) 0.0058(12) C13 0.069(2) 0.0458(16) 0.0323(13) -0.0060(12) 0.0010(13) 0.0097(14) C14 0.0658(19) 0.0447(16) 0.0365(14) -0.0014(12) -0.0012(13) 0.0103(14) C15 0.0575(16) 0.0377(14) 0.0341(13) -0.0009(11) 0.0067(11) 0.0084(12) C16 0.072(2) 0.0401(15) 0.0322(13) -0.0026(11) 0.0054(13) 0.0089(14) C17 0.070(2) 0.0366(14) 0.0326(13) -0.0010(11) 0.0053(12) 0.0071(13) C18 0.0591(16) 0.0309(12) 0.0318(12) -0.0017(10) 0.0082(11) 0.0018(11) C19 0.0521(15) 0.0319(12) 0.0294(11) -0.0001(9) 0.0075(10) -0.0011(11) C20 0.0455(13) 0.0300(11) 0.0285(11) 0.0026(9) 0.0059(9) -0.0023(10) C21 0.0494(14) 0.0296(11) 0.0293(11) 0.0009(9) 0.0083(10) -0.0011(10) C22 0.0610(17) 0.0319(12) 0.0263(11) 0.0006(9) 0.0066(11) 0.0020(11) C23 0.0624(17) 0.0334(13) 0.0305(12) 0.0043(10) 0.0038(11) 0.0053(12) C24 0.0451(13) 0.0311(11) 0.0287(11) 0.0023(9) 0.0052(9) -0.0019(10) C49 0.075(2) 0.0406(15) 0.0366(14) 0.0064(12) 0.0089(13) 0.0179(15) C50 0.105(3) 0.054(2) 0.0344(15) 0.0037(14) -0.0091(17) 0.026(2) O5 0.0471(10) 0.0428(10) 0.0310(9) -0.0037(8) 0.0111(8) -0.0051(8) O6 0.0453(10) 0.0441(11) 0.0382(10) -0.0072(8) 0.0073(8) -0.0040(8) O7 0.0460(10) 0.0366(10) 0.0402(10) -0.0035(8) 0.0042(8) 0.0002(8) O8 0.0468(11) 0.0485(11) 0.0402(10) -0.0097(9) 0.0127(8) -0.0063(9) O11 0.0458(11) 0.0457(11) 0.0463(11) -0.0063(9) 0.0092(9) -0.0077(9) O12 0.0492(12) 0.0512(12) 0.0583(13) -0.0139(11) 0.0181(10) -0.0085(10) C25 0.0467(14) 0.0345(12) 0.0274(11) 0.0026(9) 0.0067(9) -0.0016(10) C26 0.0465(14) 0.0334(12) 0.0298(11) 0.0005(9) 0.0081(10) -0.0001(10) C27 0.0487(14) 0.0353(12) 0.0300(11) -0.0015(10) 0.0066(10) -0.0017(11) C28 0.0476(14) 0.0360(13) 0.0328(12) -0.0014(10) 0.0088(10) 0.0003(11) C29 0.0462(14) 0.0376(13) 0.0371(13) 0.0011(11) 0.0063(11) -0.0038(11) C30 0.0516(15) 0.0352(13) 0.0358(13) -0.0048(10) 0.0050(11) -0.0030(11) C31 0.0516(15) 0.0350(13) 0.0324(12) -0.0022(10) 0.0080(11) 0.0001(11) C32 0.0491(15) 0.0406(14) 0.0362(13) -0.0045(11) 0.0077(11) -0.0043(12) C33 0.0493(15) 0.0442(15) 0.0402(14) -0.0069(12) 0.0095(12) -0.0055(12) C34 0.0512(16) 0.0445(15) 0.0428(15) -0.0095(12) 0.0152(12) -0.0080(12) C35 0.0517(16) 0.0379(14) 0.0423(14) -0.0045(11) 0.0114(12) -0.0072(12) C36 0.0616(18) 0.0416(15) 0.0461(16) -0.0113(13) 0.0147(14) -0.0087(13) C37 0.068(2) 0.0512(18) 0.0580(19) -0.0159(15) 0.0294(17) -0.0104(16) C38 0.066(2) 0.054(2) 0.080(3) -0.0239(18) 0.035(2) -0.0169(17) C39 0.062(2) 0.0553(19) 0.072(2) -0.0297(18) 0.0285(18) -0.0217(16) C40 0.0600(18) 0.0462(16) 0.0489(17) -0.0098(13) 0.0173(14) -0.0079(14) C41 0.0551(17) 0.0465(16) 0.0460(16) -0.0093(13) 0.0144(13) -0.0055(13) C42 0.0501(15) 0.0399(14) 0.0409(14) -0.0066(11) 0.0105(12) -0.0027(12) C43 0.0503(15) 0.0401(14) 0.0351(13) -0.0013(11) 0.0096(11) -0.0014(12) C44 0.0442(14) 0.0349(13) 0.0321(12) 0.0023(10) 0.0062(10) 0.0019(10) C45 0.0468(14) 0.0367(13) 0.0351(13) -0.0027(10) 0.0051(10) 0.0023(11) C46 0.0503(15) 0.0393(14) 0.0368(13) -0.0038(11) 0.0087(11) 0.0029(11) C47 0.0471(15) 0.0405(14) 0.0405(14) -0.0036(11) 0.0104(11) -0.0032(12) C48 0.0468(14) 0.0336(12) 0.0320(12) 0.0033(10) 0.0049(10) 0.0015(11) C51 0.0514(17) 0.0511(18) 0.0578(19) -0.0100(15) 0.0062(14) -0.0105(14) C52 0.0523(17) 0.0560(19) 0.0576(19) -0.0110(15) 0.0200(15) -0.0054(15) O1L 0.0894(18) 0.0406(11) 0.0395(11) -0.0115(9) 0.0210(11) -0.0131(11) N1L 0.046(2) 0.030(2) 0.029(2) -0.0083(17) 0.0091(18) -0.0017(18) C1L 0.043(2) 0.0229(19) 0.0239(19) -0.0045(16) 0.0103(17) -0.0015(17) C2L 0.050(3) 0.036(3) 0.036(3) -0.007(2) 0.014(2) 0.007(2) C3L 0.055(4) 0.051(4) 0.041(3) -0.018(3) 0.005(3) -0.009(3) C12L 0.100(13) 0.056(9) 0.057(9) -0.009(7) 0.000(8) -0.008(9) C13L 0.14(2) 0.101(15) 0.074(12) -0.040(11) 0.060(13) -0.062(15) O21L 0.0590(13) 0.0531(13) 0.0406(11) -0.0159(10) 0.0009(9) 0.0019(10) N21L 0.068(4) 0.059(4) 0.056(3) -0.016(3) -0.007(3) 0.000(3) C41L 0.071(2) 0.053(2) 0.065(2) -0.0130(17) -0.0034(18) -0.0033(18) C61L 0.093(6) 0.054(4) 0.083(6) 0.007(4) 0.018(5) -0.001(4) O22L 0.0590(13) 0.0531(13) 0.0406(11) -0.0159(10) 0.0009(9) 0.0019(10) N22L 0.066(4) 0.062(4) 0.045(3) -0.013(3) 0.012(3) -0.014(3) C42L 0.071(2) 0.053(2) 0.065(2) -0.0130(17) -0.0034(18) -0.0033(18) O1S 0.140(4) 0.208(6) 0.075(3) -0.026(3) -0.018(3) 0.031(4) N1S 0.126(5) 0.079(3) 0.134(5) -0.002(3) -0.018(4) -0.006(3) C1S 0.146(7) 0.134(6) 0.099(5) 0.023(4) -0.015(5) 0.036(5) N2S 0.0494(19) 0.059(2) 0.050(2) -0.0114(17) 0.0118(16) -0.0074(16) C4S 0.078(3) 0.060(3) 0.063(3) -0.013(2) 0.019(3) 0.000(3) C5S 0.075(3) 0.072(3) 0.062(3) -0.021(3) 0.014(3) -0.020(3) C6S 0.058(3) 0.078(4) 0.095(5) -0.004(3) 0.030(3) -0.003(3) N3S 0.088(3) 0.167(6) 0.065(3) -0.016(3) 0.012(2) 0.024(3) C7S 0.088(5) 0.092(5) 0.055(3) 0.005(3) 0.013(3) -0.012(4) C8S 0.139(8) 0.074(5) 0.115(7) 0.007(4) 0.071(6) -0.008(5) C9S 0.072(4) 0.096(6) 0.064(4) 0.013(3) 0.005(3) -0.008(4) N32S 0.088(3) 0.167(6) 0.065(3) -0.016(3) 0.012(2) 0.024(3) N1A 0.085(3) 0.067(2) 0.103(3) -0.011(2) 0.013(2) -0.001(2) C1A 0.066(2) 0.071(3) 0.094(3) -0.025(2) 0.014(2) 0.009(2) C2A 0.059(2) 0.057(2) 0.132(4) -0.026(3) 0.019(3) 0.0039(18) N2A 0.077(3) 0.079(3) 0.067(3) 0.010(2) 0.008(2) -0.017(3) C3A 0.071(3) 0.050(2) 0.046(2) 0.0076(19) 0.019(2) 0.001(2) C4A 0.072(3) 0.055(3) 0.040(2) 0.0035(18) 0.0163(19) 0.000(2) O4S 0.110(7) 0.160(9) 0.122(7) 0.077(7) 0.038(6) 0.022(6) C12S 0.115(9) 0.106(9) 0.088(8) 0.002(7) 0.008(7) 0.022(7) _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 1.960(2) . ? Cu1 O7 1.968(2) . ? Cu1 O5 1.976(2) . ? Cu1 O3 1.9806(19) . ? Cu1 O1L 2.132(2) . ? Cu1 Cu2 2.6178(6) . ? Cu2 O2 1.944(2) . ? Cu2 O8 1.954(2) . ? Cu2 O6 1.958(2) . ? Cu2 O4 1.959(2) . ? Cu2 O21L 2.166(2) . ? O1 C1 1.264(3) . ? O2 C1 1.265(3) . ? O3 C24 1.262(3) . ? O4 C24 1.265(3) . ? O9 C5 1.349(3) . ? O9 C49 1.439(4) . ? O10 C23 1.348(4) . ? O10 C50 1.433(4) . ? C1 C2 1.490(4) . ? C2 C3 1.389(4) . ? C2 C7 1.392(4) . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.415(4) . ? C4 C8 1.432(4) . ? C5 C6 1.402(4) . ? C6 C7 1.378(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.201(4) . ? C9 C10 1.429(4) . ? C10 C11 1.403(4) . ? C10 C15 1.404(4) . ? C11 C12 1.400(4) . ? C11 H11 0.9500 . ? C12 C13 1.406(4) . ? C12 C16 1.436(4) 3_677 ? C13 C14 1.379(4) . ? C13 H13 0.9500 . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.200(4) . ? C16 C12 1.436(4) 3_677 ? C17 C18 1.428(4) . ? C18 C19 1.397(4) . ? C18 C23 1.422(4) . ? C19 C20 1.389(4) . ? C19 H19 0.9500 . ? C20 C21 1.393(3) . ? C20 C24 1.490(4) . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 C23 1.393(4) . ? C22 H22 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O5 C25 1.263(3) . ? O6 C25 1.269(3) . ? O7 C48 1.261(3) . ? O8 C48 1.265(3) . ? O11 C29 1.355(4) . ? O11 C51 1.438(4) . ? O12 C47 1.357(4) . ? O12 C52 1.441(4) . ? C25 C26 1.483(4) . ? C26 C31 1.392(4) . ? C26 C27 1.401(4) . ? C27 C28 1.386(4) . ? C27 H27 0.9500 . ? C28 C29 1.418(4) . ? C28 C32 1.431(4) . ? C29 C30 1.390(4) . ? C30 C31 1.388(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.196(4) . ? C33 C34 1.429(4) . ? C34 C35 1.395(4) . ? C34 C39 1.405(5) . ? C35 C36 1.388(4) . ? C35 H35 0.9500 . ? C36 C37 1.391(5) . ? C36 C40 1.443(4) 3_677 ? C37 C38 1.378(5) . ? C37 H37 0.9500 . ? C38 C39 1.381(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.195(5) . ? C40 C36 1.443(4) 3_677 ? C41 C42 1.427(4) . ? C42 C43 1.385(4) . ? C42 C47 1.412(4) . ? C43 C44 1.388(4) . ? C43 H43 0.9500 . ? C44 C45 1.396(4) . ? C44 C48 1.482(4) . ? C45 C46 1.388(4) . ? C45 H45 0.9500 . ? C46 C47 1.392(4) . ? C46 H46 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O1L C1L 1.153(5) . ? O1L C12L 1.162(18) . ? O1L C13L 1.33(2) . ? N1L C1L 1.334(6) . ? N1L C2L 1.439(7) . ? N1L C3L 1.473(8) . ? C1L H1L 0.9500 . ? C2L H2L1 0.9800 . ? C2L H2L2 0.9800 . ? C2L H2L3 0.9800 . ? C3L H3L1 0.9800 . ? C3L H3L2 0.9800 . ? C3L H3L3 0.9800 . ? N12L C12L 1.33(2) . ? N12L C22L 1.45(3) . ? N12L C32L 1.49(3) . ? C12L H12L 0.9500 . ? C22L H22A 0.9800 . ? C22L H22B 0.9800 . ? C22L H22C 0.9800 . ? C32L H32A 0.9800 . ? C32L H32B 0.9800 . ? C32L H32C 0.9800 . ? N13L C13L 1.30(3) . ? N13L C23L 1.42(3) . ? N13L C33L 1.63(5) . ? C13L H13L 0.9500 . ? C23L H23A 0.9800 . ? C23L H23B 0.9800 . ? C23L H23C 0.9800 . ? C33L H33A 0.9800 . ? C33L H33B 0.9800 . ? C33L H33C 0.9800 . ? O21L C41L 1.209(5) . ? N21L C41L 1.247(8) . ? N21L C61L 1.376(12) . ? N21L C51L 1.591(10) . ? C41L H41L 0.9500 . ? C61L H61A 0.9800 . ? C61L H61B 0.9800 . ? C61L H61C 0.9800 . ? N22L C62L 1.36(2) . ? C62L H62A 0.9800 . ? C62L H62B 0.9800 . ? C62L H62C 0.9800 . ? O1S C1S 1.181(8) . ? N1S C1S 1.241(8) . ? N1S C3S 1.373(10) . ? N1S C2S 1.400(15) . ? C1S H1S 0.9500 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? O2S C4S 1.212(7) . ? N2S C4S 1.317(6) . ? N2S C6S 1.440(6) . ? N2S C5S 1.440(6) . ? C4S H4S 0.9500 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? O3S C7S 1.389(10) . ? N3S C7S 1.255(8) . ? N3S C9S 1.409(9) . ? N3S C8S 1.624(10) . ? C7S H7S 0.9500 . ? C72S H72S 0.9500 . ? N1A C1A 1.168(6) . ? C1A C2A 1.441(7) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? N2A C3A 1.134(7) . ? C3A C4A 1.464(8) . ? O4S C10S 1.175(17) . ? N4S C12S 1.302(15) . ? N4S C10S 1.372(18) . ? N4S C11S 1.421(14) . ? C10S H10S 0.9500 . ? C11S H11A 0.9800 . ? C11S H11B 0.9800 . ? C11S H11C 0.9800 . ? C12S H12A 0.9800 . ? C12S H12B 0.9800 . ? C12S H12C 0.9800 . ? N3A C5A 1.069(14) . ? C5A C6A 1.438(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O7 89.91(10) . . ? O1 Cu1 O5 90.03(10) . . ? O7 Cu1 O5 168.42(8) . . ? O1 Cu1 O3 168.20(8) . . ? O7 Cu1 O3 88.50(9) . . ? O5 Cu1 O3 89.20(9) . . ? O1 Cu1 O1L 94.35(9) . . ? O7 Cu1 O1L 93.55(10) . . ? O5 Cu1 O1L 98.00(10) . . ? O3 Cu1 O1L 97.42(9) . . ? O1 Cu1 Cu2 84.44(6) . . ? O7 Cu1 Cu2 86.16(6) . . ? O5 Cu1 Cu2 82.31(6) . . ? O3 Cu1 Cu2 83.79(6) . . ? O1L Cu1 Cu2 178.76(8) . . ? O2 Cu2 O8 89.60(10) . . ? O2 Cu2 O6 90.01(10) . . ? O8 Cu2 O6 169.46(9) . . ? O2 Cu2 O4 170.00(8) . . ? O8 Cu2 O4 89.23(10) . . ? O6 Cu2 O4 89.33(10) . . ? O2 Cu2 O21L 95.46(9) . . ? O8 Cu2 O21L 92.44(9) . . ? O6 Cu2 O21L 98.08(9) . . ? O4 Cu2 O21L 94.52(9) . . ? O2 Cu2 Cu1 84.74(6) . . ? O8 Cu2 Cu1 82.80(7) . . ? O6 Cu2 Cu1 86.68(6) . . ? O4 Cu2 Cu1 85.26(6) . . ? O21L Cu2 Cu1 175.24(7) . . ? C1 O1 Cu1 121.90(18) . . ? C1 O2 Cu2 122.54(17) . . ? C24 O3 Cu1 122.55(17) . . ? C24 O4 Cu2 122.19(18) . . ? C5 O9 C49 117.0(2) . . ? C23 O10 C50 117.3(2) . . ? O1 C1 O2 125.9(2) . . ? O1 C1 C2 117.6(2) . . ? O2 C1 C2 116.5(2) . . ? C3 C2 C7 119.2(2) . . ? C3 C2 C1 119.9(2) . . ? C7 C2 C1 120.9(2) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 C8 121.3(3) . . ? C5 C4 C8 120.0(2) . . ? O9 C5 C6 124.5(3) . . ? O9 C5 C4 115.5(2) . . ? C6 C5 C4 120.0(3) . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C2 121.1(3) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? C9 C8 C4 177.6(3) . . ? C8 C9 C10 177.4(3) . . ? C11 C10 C15 119.4(3) . . ? C11 C10 C9 120.7(3) . . ? C15 C10 C9 120.0(2) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.2(3) . . ? C11 C12 C16 120.6(3) . 3_677 ? C13 C12 C16 120.2(3) . 3_677 ? C14 C13 C12 120.3(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.8(3) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 119.9(3) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? C17 C16 C12 178.4(4) . 3_677 ? C16 C17 C18 176.5(3) . . ? C19 C18 C23 118.3(2) . . ? C19 C18 C17 120.1(3) . . ? C23 C18 C17 121.5(3) . . ? C20 C19 C18 121.5(2) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 119.2(2) . . ? C19 C20 C24 119.6(2) . . ? C21 C20 C24 120.9(2) . . ? C22 C21 C20 120.8(2) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.2(2) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? O10 C23 C22 124.6(3) . . ? O10 C23 C18 115.5(3) . . ? C22 C23 C18 119.9(3) . . ? O3 C24 O4 125.5(2) . . ? O3 C24 C20 117.6(2) . . ? O4 C24 C20 116.9(2) . . ? O9 C49 H49A 109.5 . . ? O9 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O9 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O10 C50 H50A 109.5 . . ? O10 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O10 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C25 O5 Cu1 125.09(19) . . ? C25 O6 Cu2 120.79(18) . . ? C48 O7 Cu1 120.24(19) . . ? C48 O8 Cu2 125.0(2) . . ? C29 O11 C51 117.8(2) . . ? C47 O12 C52 116.7(3) . . ? O5 C25 O6 124.8(3) . . ? O5 C25 C26 117.7(2) . . ? O6 C25 C26 117.5(2) . . ? C31 C26 C27 118.8(3) . . ? C31 C26 C25 120.6(2) . . ? C27 C26 C25 120.6(2) . . ? C28 C27 C26 120.7(3) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 119.6(2) . . ? C27 C28 C32 121.1(3) . . ? C29 C28 C32 119.3(3) . . ? O11 C29 C30 125.2(3) . . ? O11 C29 C28 115.0(3) . . ? C30 C29 C28 119.8(3) . . ? C31 C30 C29 119.6(3) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C26 121.5(3) . . ? C30 C31 H31 119.3 . . ? C26 C31 H31 119.3 . . ? C33 C32 C28 177.7(3) . . ? C32 C33 C34 174.6(4) . . ? C35 C34 C39 119.0(3) . . ? C35 C34 C33 121.1(3) . . ? C39 C34 C33 119.7(3) . . ? C36 C35 C34 120.7(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.6(3) . . ? C35 C36 C40 120.6(3) . 3_677 ? C37 C36 C40 119.8(3) . 3_677 ? C38 C37 C36 119.9(3) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 121.1(3) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C38 C39 C34 119.5(3) . . ? C38 C39 H39 120.2 . . ? C34 C39 H39 120.2 . . ? C41 C40 C36 179.3(4) . 3_677 ? C40 C41 C42 176.1(4) . . ? C43 C42 C47 119.1(3) . . ? C43 C42 C41 119.6(3) . . ? C47 C42 C41 121.3(3) . . ? C42 C43 C44 121.5(3) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C43 C44 C45 118.8(3) . . ? C43 C44 C48 119.3(2) . . ? C45 C44 C48 121.8(3) . . ? C46 C45 C44 121.0(3) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 119.7(3) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? O12 C47 C46 124.5(3) . . ? O12 C47 C42 115.6(3) . . ? C46 C47 C42 119.9(3) . . ? O7 C48 O8 125.4(3) . . ? O7 C48 C44 118.6(2) . . ? O8 C48 C44 116.0(2) . . ? O11 C51 H51A 109.5 . . ? O11 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O11 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O12 C52 H52A 109.5 . . ? O12 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O12 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C1L O1L C12L 78.2(9) . . ? C1L O1L C13L 61.0(10) . . ? C12L O1L C13L 125.1(13) . . ? C1L O1L Cu1 137.8(3) . . ? C12L O1L Cu1 119.4(9) . . ? C13L O1L Cu1 115.6(10) . . ? C1L N1L C2L 122.8(5) . . ? C1L N1L C3L 120.1(5) . . ? C2L N1L C3L 116.5(5) . . ? O1L C1L N1L 128.4(5) . . ? O1L C1L H1L 115.8 . . ? N1L C1L H1L 115.8 . . ? C12L N12L C22L 124.3(17) . . ? C12L N12L C32L 121.0(18) . . ? C22L N12L C32L 114.3(18) . . ? O1L C12L N12L 125.3(17) . . ? O1L C12L H12L 117.4 . . ? N12L C12L H12L 117.4 . . ? N12L C22L H22A 109.5 . . ? N12L C22L H22B 109.5 . . ? H22A C22L H22B 109.5 . . ? N12L C22L H22C 109.5 . . ? H22A C22L H22C 109.5 . . ? H22B C22L H22C 109.5 . . ? N12L C32L H32A 109.5 . . ? N12L C32L H32B 109.5 . . ? H32A C32L H32B 109.5 . . ? N12L C32L H32C 109.5 . . ? H32A C32L H32C 109.5 . . ? H32B C32L H32C 109.5 . . ? C13L N13L C23L 121(2) . . ? C13L N13L C33L 122(3) . . ? C23L N13L C33L 110(2) . . ? N13L C13L O1L 126(2) . . ? N13L C13L H13L 117.2 . . ? O1L C13L H13L 117.2 . . ? C41L O21L Cu2 121.6(3) . . ? C41L N21L C61L 117.8(7) . . ? C41L N21L C51L 112.7(6) . . ? C61L N21L C51L 129.4(7) . . ? O21L C41L N21L 130.9(5) . . ? O21L C41L H41L 114.5 . . ? N21L C41L H41L 114.5 . . ? N22L C62L H62A 109.5 . . ? N22L C62L H62B 109.5 . . ? H62A C62L H62B 109.5 . . ? N22L C62L H62C 109.5 . . ? H62A C62L H62C 109.5 . . ? H62B C62L H62C 109.5 . . ? C1S N1S C3S 125.2(8) . . ? C1S N1S C2S 126.5(10) . . ? C3S N1S C2S 108.3(9) . . ? O1S C1S N1S 126.5(10) . . ? O1S C1S H1S 116.7 . . ? N1S C1S H1S 116.7 . . ? N1S C2S H2S1 109.5 . . ? N1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? N1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N1S C3S H3S1 109.5 . . ? N1S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? N1S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C4S N2S C6S 121.6(5) . . ? C4S N2S C5S 120.4(5) . . ? C6S N2S C5S 117.4(5) . . ? O2S C4S N2S 126.3(6) . . ? O2S C4S H4S 116.8 . . ? N2S C4S H4S 116.8 . . ? C7S N3S C9S 136.8(8) . . ? C7S N3S C8S 115.9(7) . . ? C9S N3S C8S 107.3(6) . . ? N3S C7S O3S 115.7(7) . . ? N3S C7S H7S 122.2 . . ? O3S C7S H7S 122.2 . . ? N1A C1A C2A 175.4(6) . . ? C1A C2A H2A1 109.5 . . ? C1A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C1A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? N2A C3A C4A 178.6(6) . . ? C12S N4S C10S 117.6(12) . . ? C12S N4S C11S 120.9(13) . . ? C10S N4S C11S 121.5(13) . . ? O4S C10S N4S 126.4(15) . . ? O4S C10S H10S 116.8 . . ? N4S C10S H10S 116.8 . . ? N4S C11S H11A 109.5 . . ? N4S C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? N4S C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 109.5 . . ? N4S C12S H12A 109.5 . . ? N4S C12S H12B 109.5 . . ? H12A C12S H12B 109.5 . . ? N4S C12S H12C 109.5 . . ? H12A C12S H12C 109.5 . . ? H12B C12S H12C 109.5 . . ? N3A C5A C6A 164(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.035 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.092 #===END