# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Jian Zhang' 'Yan-Xi Tan' 'Juan Liu' 'Fei Wang' 'Yao Kang' _publ_contact_author_name 'Dr Jian Zhang,' _publ_contact_author_email zhj@fjirsm.ac.cn data_a _database_code_depnum_ccdc_archive 'CCDC 846750' #TrackingRef '- a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H68 Cu3 N6 O16' _chemical_formula_weight 1572.03 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.3011(12) _cell_length_b 20.084(2) _cell_length_c 25.5200(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7842.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5081 _cell_measurement_theta_min 2.3078 _cell_measurement_theta_max 28.7660 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max .21 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3244 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 16981 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12315 _reflns_number_gt 6705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1098P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(2) _refine_ls_number_reflns 12315 _refine_ls_number_parameters 955 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1279 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1955 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.006 _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 0.76798(6) 2.00631(6) 1.78628(4) 0.0486(3) Uani 1 1 d . . . Cu2 Cu 1.57485(8) 1.79433(6) 1.54872(4) 0.0589(3) Uani 1 1 d . . . Cu3 Cu -0.07037(8) 2.16750(7) 1.53783(4) 0.0642(4) Uani 1 1 d . . . O1 O -0.0193(5) 2.0511(5) 1.6276(3) 0.091(3) Uani 1 1 d . . . O1W O 0.7818(4) 2.0050(3) 1.6950(2) 0.0659(18) Uani 1 1 d . . . H10B H 0.7382 2.0235 1.6742 0.079 Uiso 1 1 d R . . H10C H 0.8309 1.9860 1.6795 0.079 Uiso 1 1 d R . . O2 O 0.0039(4) 2.1520(5) 1.5985(3) 0.083(2) Uani 1 1 d . . . O3 O 0.6561(4) 2.0518(3) 1.7776(2) 0.0532(16) Uani 1 1 d . . . O4 O 0.6334(4) 2.0456(5) 1.8635(2) 0.090(3) Uani 1 1 d . . . O5 O 0.2644(4) 2.1531(4) 1.7874(2) 0.073(2) Uani 1 1 d . . . O6 O 1.5031(5) 1.7942(4) 1.6083(2) 0.0692(19) Uani 1 1 d . . . O7 O 1.5189(6) 1.8995(5) 1.6291(3) 0.096(3) Uani 1 1 d . . . O8 O 0.8798(4) 1.9585(3) 1.7825(2) 0.0551(17) Uani 1 1 d . . . O9 O 0.8910(4) 1.9493(4) 1.8702(3) 0.084(2) Uani 1 1 d . . . O10 O 1.2471(4) 1.8133(4) 1.8019(2) 0.090(3) Uani 1 1 d . . . O11 O 1.8873(4) 1.2272(4) 1.4826(2) 0.0557(17) Uani 1 1 d . . . O12 O 1.9848(4) 1.2904(4) 1.5211(2) 0.078(2) Uani 1 1 d . . . O13 O 1.6295(5) 1.7502(4) 1.4892(2) 0.073(2) Uani 1 1 d . . . O14 O 1.5494(5) 1.6786(4) 1.5292(3) 0.090(3) Uani 1 1 d . . . O15 O 1.7835(5) 1.4988(3) 1.3753(2) 0.083(2) Uani 1 1 d . . . N1 N 1.3115(6) 2.3096(4) 1.9164(3) 0.063(2) Uani 1 1 d . . . N2 N 0.8343(4) 2.0917(4) 1.8005(3) 0.0464(18) Uani 1 1 d . . . N3 N 0.7028(4) 1.9220(4) 1.7967(3) 0.0488(19) Uani 1 1 d . . . N4 N 0.1841(5) 1.6775(4) 1.9233(3) 0.054(2) Uani 1 1 d . . . N5 N 1.4927(6) 1.8458(5) 1.5015(3) 0.061(2) Uani 1 1 d . . . N6 N 1.0205(5) 2.1322(4) 1.4881(3) 0.055(2) Uani 1 1 d . . . C1 C 1.2358(10) 2.3302(7) 1.9457(5) 0.106(5) Uani 1 1 d . . . H1A H 1.2423 2.3303 1.9819 0.128 Uiso 1 1 calc R . . C2 C 1.1582(7) 2.3491(8) 1.9282(5) 0.094(5) Uani 1 1 d . . . H2A H 1.1142 2.3648 1.9500 0.113 Uiso 1 1 calc R . . C3 C 1.1488(7) 2.3433(7) 1.8748(5) 0.081(3) Uani 1 1 d . . . C4 C 1.2129(9) 2.3229(7) 1.8450(5) 0.095(4) Uani 1 1 d . . . H4A H 1.2040 2.3175 1.8092 0.114 Uiso 1 1 calc R . . C5 C 1.2943(7) 2.3091(6) 1.8667(4) 0.070(3) Uani 1 1 d . . . H5A H 1.3396 2.2989 1.8438 0.084 Uiso 1 1 calc R . . C6 C 0.9078(9) 2.1060(6) 1.7757(5) 0.102(5) Uani 1 1 d . . . H6A H 0.9255 2.0789 1.7481 0.122 Uiso 1 1 calc R . . C7 C 0.9562(10) 2.1568(10) 1.7887(8) 0.199(11) Uani 1 1 d . . . H7A H 1.0028 2.1665 1.7666 0.239 Uiso 1 1 calc R . . C8 C 0.9461(9) 2.1951(9) 1.8290(8) 0.136(7) Uani 1 1 d . . . C9 C 0.8719(11) 2.1771(7) 1.8548(5) 0.109(5) Uani 1 1 d . . . H9A H 0.8575 2.2006 1.8850 0.131 Uiso 1 1 calc R . . C10 C 0.8178(10) 2.1275(6) 1.8397(5) 0.106(5) Uani 1 1 d . . . H10A H 0.7670 2.1197 1.8588 0.127 Uiso 1 1 calc R . . C11 C 1.0065(11) 2.2456(9) 1.8495(8) 0.163(8) Uani 1 1 d D . . H11A H 0.9986 2.2475 1.8872 0.195 Uiso 1 1 calc R . . H11B H 1.0655 2.2299 1.8432 0.195 Uiso 1 1 calc R . . C12 C 1.0014(13) 2.3080(10) 1.8312(9) 0.203(11) Uani 1 1 d D . . H12A H 0.9413 2.3223 1.8357 0.244 Uiso 1 1 calc R . . H12B H 1.0119 2.3058 1.7937 0.244 Uiso 1 1 calc R . . C13 C 1.0596(11) 2.3636(7) 1.8528(7) 0.162(8) Uani 1 1 d . . . H13A H 1.0275 2.3863 1.8803 0.195 Uiso 1 1 calc R . . H13B H 1.0693 2.3957 1.8249 0.195 Uiso 1 1 calc R . . C14 C 0.6518(7) 1.8966(7) 1.7581(4) 0.078(3) Uani 1 1 d . . . H14A H 0.6446 1.9204 1.7272 0.093 Uiso 1 1 calc R . . C15 C 0.6102(6) 1.8357(6) 1.7642(4) 0.065(3) Uani 1 1 d . . . H15B H 0.5789 1.8179 1.7364 0.077 Uiso 1 1 calc R . . C16 C 0.6143(6) 1.8020(5) 1.8099(4) 0.052(2) Uani 1 1 d . . . C17 C 0.6584(8) 1.8276(5) 1.8477(4) 0.076(3) Uani 1 1 d . . . H17A H 0.6611 1.8053 1.8796 0.091 Uiso 1 1 calc R . . C18 C 0.7020(7) 1.8874(7) 1.8421(4) 0.077(4) Uani 1 1 d . . . H18A H 0.7321 1.9046 1.8708 0.093 Uiso 1 1 calc R . . C19 C 0.1975(7) 1.6595(5) 1.8715(4) 0.070(3) Uani 1 1 d . . . H19A H 0.1477 1.6470 1.8531 0.084 Uiso 1 1 calc R . . C20 C 0.2686(6) 1.6577(6) 1.8454(3) 0.065(3) Uani 1 1 d . . . H20D H 0.2695 1.6449 1.8104 0.078 Uiso 1 1 calc R . . C21 C 0.3464(8) 1.6763(5) 1.8722(4) 0.070(3) Uani 1 1 d . . . C22 C 0.3338(9) 1.6952(6) 1.9242(4) 0.094(4) Uani 1 1 d . . . H22B H 0.3817 1.7092 1.9438 0.113 Uiso 1 1 calc R . . C23 C 0.2532(5) 1.6939(6) 1.9474(4) 0.075(4) Uani 1 1 d . . . H23A H 0.2489 1.7056 1.9826 0.090 Uiso 1 1 calc R . . C24 C 0.5614(7) 1.7372(5) 1.8145(4) 0.065(3) Uani 1 1 d . . . H24B H 0.5480 1.7216 1.7795 0.079 Uiso 1 1 calc R . . H24C H 0.5980 1.7039 1.8310 0.079 Uiso 1 1 calc R . . C25 C 0.4787(6) 1.7421(5) 1.8444(4) 0.057(3) Uani 1 1 d . . . H25B H 0.4391 1.7728 1.8272 0.068 Uiso 1 1 calc R . . H25C H 0.4903 1.7585 1.8795 0.068 Uiso 1 1 calc R . . C26 C 0.4377(6) 1.6733(5) 1.8472(4) 0.064(3) Uani 1 1 d . . . H26B H 0.4748 1.6441 1.8677 0.077 Uiso 1 1 calc R . . H26C H 0.4331 1.6549 1.8121 0.077 Uiso 1 1 calc R . . C27 C 1.4084(8) 1.8231(7) 1.4892(5) 0.093(4) Uani 1 1 d . . . H27A H 1.3865 1.7847 1.5048 0.111 Uiso 1 1 calc R . . C28 C 1.3612(8) 1.8562(7) 1.4558(5) 0.099(4) Uani 1 1 d . . . H28A H 1.3052 1.8406 1.4486 0.119 Uiso 1 1 calc R . . C29 C 1.3894(7) 1.9138(6) 1.4298(4) 0.064(3) Uani 1 1 d . . . C30 C 1.4715(8) 1.9349(7) 1.4419(4) 0.089(4) Uani 1 1 d . . . H30A H 1.4943 1.9734 1.4270 0.107 Uiso 1 1 calc R . . C31 C 1.5213(8) 1.8970(7) 1.4778(5) 0.089(4) Uani 1 1 d . . . H31B H 1.5785 1.9103 1.4844 0.106 Uiso 1 1 calc R . . C32 C 0.9976(7) 2.0910(6) 1.4499(4) 0.074(3) Uani 1 1 d . . . H32A H 0.9385 2.0816 1.4456 0.089 Uiso 1 1 calc R . . C33 C 1.0522(8) 2.0632(6) 1.4183(4) 0.078(3) Uani 1 1 d . . . H33B H 1.0310 2.0362 1.3916 0.093 Uiso 1 1 calc R . . C34 C 1.1428(7) 2.0723(5) 1.4230(4) 0.063(3) Uani 1 1 d . . . C35 C 1.1658(6) 2.1148(6) 1.4618(3) 0.063(3) Uani 1 1 d . . . H35A H 1.2244 2.1251 1.4667 0.076 Uiso 1 1 calc R . . C36 C 1.1033(7) 2.1432(6) 1.4942(4) 0.072(3) Uani 1 1 d . . . H36A H 1.1214 2.1711 1.5211 0.086 Uiso 1 1 calc R . . C37 C 1.3336(8) 1.9515(6) 1.3918(4) 0.080(3) Uani 1 1 d . . . H37A H 1.3051 1.9207 1.3680 0.096 Uiso 1 1 calc R . . H37B H 1.3695 1.9816 1.3713 0.096 Uiso 1 1 calc R . . C38 C 1.2631(7) 1.9921(6) 1.4232(4) 0.083(3) Uani 1 1 d . . . H38A H 1.2267 1.9611 1.4426 0.099 Uiso 1 1 calc R . . H38B H 1.2927 2.0202 1.4485 0.099 Uiso 1 1 calc R . . C39 C 1.2062(7) 2.0343(6) 1.3902(4) 0.085(4) Uani 1 1 d . . . H39A H 1.1746 2.0066 1.3655 0.102 Uiso 1 1 calc R . . H39B H 1.2419 2.0652 1.3703 0.102 Uiso 1 1 calc R . . C40 C 0.0813(7) 2.1199(7) 1.6710(3) 0.073(4) Uani 1 1 d . . . C41 C 0.1160(6) 2.0631(6) 1.7004(3) 0.071(3) Uani 1 1 d . . . H41A H 0.0977 2.0194 1.6950 0.085 Uiso 1 1 calc R . . C42 C 0.1833(7) 2.0823(7) 1.7395(4) 0.079(4) Uani 1 1 d . . . H42A H 0.2073 2.0491 1.7604 0.094 Uiso 1 1 calc R . . C43 C 0.2097(6) 2.1413(5) 1.7461(4) 0.047(2) Uani 1 1 d . . . C44 C 0.1786(6) 2.1924(5) 1.7194(3) 0.059(3) Uani 1 1 d . . . H44A H 0.1995 2.2350 1.7263 0.071 Uiso 1 1 calc R . . C45 C 0.1146(6) 2.1833(5) 1.6808(4) 0.057(3) Uani 1 1 d . . . H45A H 0.0943 2.2195 1.6617 0.068 Uiso 1 1 calc R . . C46 C 0.0156(7) 2.1043(6) 1.6269(4) 0.059(3) Uani 1 1 d . . . C47 C 0.5142(5) 2.0806(4) 1.8093(3) 0.039(2) Uani 1 1 d . . . C48 C 0.4724(6) 2.1123(5) 1.8467(4) 0.059(3) Uani 1 1 d . . . H48A H 0.4999 2.1181 1.8789 0.071 Uiso 1 1 calc R . . C49 C 0.3876(6) 2.1380(5) 1.8399(3) 0.061(3) Uani 1 1 d . . . H49A H 0.3602 2.1621 1.8664 0.073 Uiso 1 1 calc R . . C50 C 0.3458(6) 2.1259(5) 1.7920(3) 0.047(2) Uani 1 1 d . . . C51 C 0.3867(6) 2.0921(5) 1.7537(3) 0.057(3) Uani 1 1 d . . . H51B H 0.3579 2.0833 1.7224 0.069 Uiso 1 1 calc R . . C52 C 0.4730(5) 2.0703(5) 1.7610(3) 0.046(2) Uani 1 1 d . . . H52A H 0.5026 2.0490 1.7339 0.055 Uiso 1 1 calc R . . C53 C 0.6099(6) 2.0580(5) 1.8199(4) 0.060(3) Uani 1 1 d . . . C54 C 1.4231(6) 1.8379(6) 1.6799(3) 0.056(2) Uani 1 1 d . . . C55 C 1.4033(6) 1.8923(6) 1.7133(4) 0.072(3) Uani 1 1 d . . . H55A H 1.4305 1.9333 1.7085 0.087 Uiso 1 1 calc R . . C56 C 1.3429(8) 1.8833(8) 1.7529(4) 0.090(4) Uani 1 1 d . . . H56A H 1.3303 1.9185 1.7753 0.107 Uiso 1 1 calc R . . C57 C 1.3008(7) 1.8230(7) 1.7599(4) 0.064(3) Uani 1 1 d . . . C58 C 1.3206(7) 1.7732(6) 1.7280(4) 0.075(3) Uani 1 1 d . . . H58A H 1.2903 1.7334 1.7319 0.089 Uiso 1 1 calc R . . C59 C 1.3834(8) 1.7766(6) 1.6892(4) 0.068(3) Uani 1 1 d . . . H59A H 1.3987 1.7391 1.6698 0.082 Uiso 1 1 calc R . . C60 C 1.4862(7) 1.8456(6) 1.6348(4) 0.060(3) Uani 1 1 d . . . C61 C 1.0084(6) 1.9079(5) 1.8192(4) 0.051(2) Uani 1 1 d . . . C62 C 1.0451(6) 1.8675(6) 1.8581(3) 0.069(3) Uani 1 1 d . . . H62A H 1.0140 1.8590 1.8886 0.082 Uiso 1 1 calc R . . C63 C 1.1239(6) 1.8414(6) 1.8518(4) 0.072(3) Uani 1 1 d . . . H63A H 1.1501 1.8189 1.8795 0.087 Uiso 1 1 calc R . . C64 C 1.1671(7) 1.8471(6) 1.8052(4) 0.075(3) Uani 1 1 d . . . C65 C 1.1317(6) 1.8881(6) 1.7644(4) 0.065(3) Uani 1 1 d . . . H65A H 1.1619 1.8939 1.7331 0.078 Uiso 1 1 calc R . . C66 C 1.0533(6) 1.9183(5) 1.7723(3) 0.057(3) Uani 1 1 d . . . H66A H 1.0298 1.9458 1.7466 0.068 Uiso 1 1 calc R . . C67 C 0.9152(6) 1.9410(5) 1.8230(5) 0.061(3) Uani 1 1 d . . . C68 C 1.8888(6) 1.3394(5) 1.4600(3) 0.046(2) Uani 1 1 d . . . C69 C 1.9271(8) 1.4015(6) 1.4614(4) 0.087(3) Uani 1 1 d . . . H69A H 1.9768 1.4078 1.4818 0.104 Uiso 1 1 calc R . . C70 C 1.8938(9) 1.4554(6) 1.4331(4) 0.089(4) Uani 1 1 d . . . H70A H 1.9199 1.4972 1.4334 0.107 Uiso 1 1 calc R . . C71 C 1.8197(8) 1.4420(6) 1.4048(3) 0.064(3) Uani 1 1 d . . . C72 C 1.7812(7) 1.3845(5) 1.4013(4) 0.061(3) Uani 1 1 d . . . H72A H 1.7320 1.3787 1.3804 0.073 Uiso 1 1 calc R . . C73 C 1.8150(7) 1.3342(5) 1.4289(4) 0.061(3) Uani 1 1 d . . . H73A H 1.7872 1.2931 1.4271 0.073 Uiso 1 1 calc R . . C74 C 1.9231(6) 1.2846(5) 1.4894(3) 0.048(2) Uani 1 1 d . . . C75 C 1.6490(6) 1.6388(5) 1.4607(3) 0.050(2) Uani 1 1 d . . . C76 C 1.7105(8) 1.6575(6) 1.4274(4) 0.091(4) Uani 1 1 d . . . H76A H 1.7246 1.7024 1.4244 0.109 Uiso 1 1 calc R . . C77 C 1.7554(9) 1.6099(6) 1.3963(5) 0.100(4) Uani 1 1 d . . . H77A H 1.7961 1.6226 1.3711 0.120 Uiso 1 1 calc R . . C78 C 1.7349(8) 1.5427(5) 1.4053(3) 0.059(3) Uani 1 1 d . . . C79 C 1.6700(8) 1.5260(6) 1.4365(4) 0.080(3) Uani 1 1 d . . . H79A H 1.6529 1.4817 1.4398 0.096 Uiso 1 1 calc R . . C80 C 1.6280(7) 1.5751(5) 1.4641(4) 0.072(3) Uani 1 1 d . . . H80A H 1.5824 1.5630 1.4863 0.087 Uiso 1 1 calc R . . C81 C 1.6033(7) 1.6896(5) 1.4941(4) 0.060(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0416(5) 0.0584(7) 0.0458(6) 0.0066(6) 0.0036(5) 0.0063(6) Cu2 0.0583(7) 0.0724(8) 0.0459(6) 0.0005(6) 0.0134(6) 0.0170(7) Cu3 0.0528(7) 0.0948(10) 0.0452(6) 0.0111(6) -0.0075(5) 0.0190(7) O1 0.090(6) 0.080(6) 0.102(6) -0.004(5) -0.045(5) 0.008(5) O1W 0.072(4) 0.077(5) 0.048(4) 0.009(3) 0.007(3) 0.009(4) O2 0.053(4) 0.134(7) 0.062(4) 0.037(5) -0.016(3) 0.010(5) O3 0.048(4) 0.046(4) 0.065(4) 0.009(3) 0.000(3) 0.004(3) O4 0.072(5) 0.162(8) 0.035(4) 0.019(5) -0.017(3) 0.028(5) O5 0.048(4) 0.106(6) 0.066(4) -0.013(4) -0.022(3) 0.024(4) O6 0.085(5) 0.077(5) 0.046(4) -0.006(4) 0.011(3) 0.020(4) O7 0.093(6) 0.080(6) 0.116(7) -0.005(5) 0.022(5) 0.003(5) O8 0.054(4) 0.053(4) 0.059(4) 0.010(4) -0.010(3) 0.010(3) O9 0.049(4) 0.100(6) 0.103(6) 0.002(5) 0.008(4) 0.021(4) O10 0.068(5) 0.136(7) 0.067(5) 0.032(4) 0.028(4) 0.064(5) O11 0.042(4) 0.073(5) 0.052(4) 0.003(3) -0.005(3) 0.010(4) O12 0.062(5) 0.111(6) 0.060(4) 0.004(4) -0.016(4) 0.001(5) O13 0.087(5) 0.076(5) 0.056(4) -0.016(4) 0.024(4) 0.015(5) O14 0.105(6) 0.075(5) 0.091(5) 0.001(4) 0.054(5) 0.017(5) O15 0.143(6) 0.054(4) 0.052(4) 0.003(4) 0.003(4) 0.031(5) N1 0.074(6) 0.072(7) 0.043(5) 0.010(4) 0.013(4) -0.018(5) N2 0.042(4) 0.042(5) 0.056(5) -0.006(4) -0.001(3) 0.008(4) N3 0.026(4) 0.064(5) 0.057(5) 0.010(4) 0.001(3) 0.024(4) N4 0.038(4) 0.086(7) 0.038(4) -0.001(4) -0.018(3) -0.009(4) N5 0.072(6) 0.057(6) 0.054(5) 0.003(5) 0.009(4) 0.016(5) N6 0.037(5) 0.069(6) 0.060(5) 0.006(5) -0.002(4) 0.011(4) C1 0.139(13) 0.116(10) 0.064(7) -0.037(8) 0.014(9) -0.048(10) C2 0.038(6) 0.164(14) 0.079(8) 0.000(9) -0.017(6) -0.006(8) C3 0.047(7) 0.091(9) 0.105(10) 0.020(8) 0.001(7) -0.006(7) C4 0.097(11) 0.122(12) 0.065(7) -0.012(7) -0.028(7) -0.018(9) C5 0.065(7) 0.099(10) 0.047(6) -0.007(6) 0.015(5) -0.017(6) C6 0.114(11) 0.064(8) 0.128(11) -0.029(8) 0.063(9) -0.027(8) C7 0.101(12) 0.183(18) 0.31(2) -0.166(19) 0.125(15) -0.100(13) C8 0.060(9) 0.143(15) 0.204(17) -0.086(14) -0.010(10) -0.026(10) C9 0.137(14) 0.096(11) 0.095(9) -0.057(9) 0.004(9) 0.016(11) C10 0.160(13) 0.054(8) 0.105(10) -0.056(8) 0.063(10) -0.023(9) C11 0.118(14) 0.141(17) 0.23(2) -0.046(17) -0.057(15) 0.011(14) C12 0.139(16) 0.151(19) 0.32(3) 0.077(19) -0.125(18) -0.069(15) C13 0.158(16) 0.093(11) 0.237(19) 0.070(12) -0.077(15) -0.051(12) C14 0.060(7) 0.114(11) 0.058(7) 0.019(7) -0.002(6) 0.007(7) C15 0.052(6) 0.071(8) 0.070(7) -0.004(6) -0.013(5) -0.016(6) C16 0.042(5) 0.068(7) 0.045(5) -0.006(6) -0.004(4) 0.013(5) C17 0.121(10) 0.046(7) 0.061(7) 0.014(6) -0.001(7) -0.033(7) C18 0.068(7) 0.128(11) 0.036(6) 0.007(6) -0.013(5) -0.011(7) C19 0.065(7) 0.067(8) 0.079(7) -0.020(6) -0.042(6) -0.014(6) C20 0.041(5) 0.107(9) 0.046(5) -0.010(6) 0.016(5) -0.027(6) C21 0.090(8) 0.044(6) 0.076(7) 0.011(6) 0.017(6) -0.016(6) C22 0.110(10) 0.132(12) 0.040(6) -0.035(7) -0.029(6) 0.015(9) C23 0.021(5) 0.159(12) 0.045(5) -0.022(6) 0.003(4) -0.005(6) C24 0.090(8) 0.045(6) 0.061(6) 0.003(5) -0.003(6) -0.004(6) C25 0.057(6) 0.052(7) 0.061(6) -0.005(5) 0.000(5) -0.001(5) C26 0.052(6) 0.073(7) 0.068(6) -0.012(5) 0.011(5) 0.000(6) C27 0.069(8) 0.109(10) 0.100(9) 0.049(8) -0.017(7) 0.016(8) C28 0.059(7) 0.112(11) 0.127(11) 0.058(10) -0.003(7) 0.003(7) C29 0.049(6) 0.091(9) 0.052(6) -0.005(6) 0.006(5) 0.024(6) C30 0.087(9) 0.111(11) 0.070(7) 0.043(7) -0.012(6) -0.019(8) C31 0.057(7) 0.106(10) 0.104(9) 0.035(8) -0.021(7) 0.000(7) C32 0.042(6) 0.114(10) 0.066(7) -0.032(7) -0.006(5) 0.018(6) C33 0.092(9) 0.084(9) 0.057(6) -0.016(6) -0.035(6) 0.003(7) C34 0.052(6) 0.065(7) 0.071(7) 0.009(6) -0.010(5) 0.007(6) C35 0.043(6) 0.098(8) 0.048(5) -0.014(6) 0.004(4) -0.009(6) C36 0.071(8) 0.068(8) 0.076(7) 0.002(6) -0.003(6) -0.001(6) C37 0.097(9) 0.072(8) 0.070(7) 0.014(6) 0.019(6) 0.027(7) C38 0.079(7) 0.119(10) 0.051(6) -0.010(6) -0.008(5) 0.030(8) C39 0.073(8) 0.101(10) 0.081(8) -0.013(7) -0.032(6) 0.033(7) C40 0.057(6) 0.131(11) 0.031(5) 0.022(6) 0.011(5) 0.036(8) C41 0.060(6) 0.109(9) 0.043(6) 0.021(6) -0.008(5) 0.014(6) C42 0.058(7) 0.131(12) 0.048(6) 0.048(7) 0.008(5) 0.040(8) C43 0.050(6) 0.041(6) 0.049(6) 0.003(5) -0.001(4) -0.004(5) C44 0.047(5) 0.076(8) 0.055(6) 0.001(6) -0.014(5) -0.003(5) C45 0.056(6) 0.049(7) 0.064(6) 0.000(5) 0.009(5) 0.000(5) C46 0.055(7) 0.054(7) 0.068(7) -0.005(6) -0.019(5) 0.010(6) C47 0.039(5) 0.045(6) 0.035(5) 0.003(4) 0.001(4) 0.009(4) C48 0.044(5) 0.084(8) 0.049(6) -0.016(6) -0.017(4) 0.004(6) C49 0.046(6) 0.089(8) 0.047(6) -0.015(6) -0.006(4) 0.013(6) C50 0.048(5) 0.052(6) 0.041(5) 0.003(5) -0.007(4) 0.006(5) C51 0.061(6) 0.076(8) 0.034(5) 0.011(5) -0.002(4) -0.011(6) C52 0.040(5) 0.061(7) 0.037(5) -0.008(4) 0.005(4) 0.007(5) C53 0.057(6) 0.055(7) 0.067(7) -0.006(6) 0.016(6) 0.004(5) C54 0.042(5) 0.087(8) 0.040(5) -0.012(5) 0.002(4) 0.004(6) C55 0.049(6) 0.078(8) 0.090(8) -0.024(7) 0.010(6) 0.004(6) C56 0.093(9) 0.130(13) 0.046(6) -0.032(7) 0.019(6) 0.042(9) C57 0.053(6) 0.094(9) 0.045(6) 0.004(6) 0.014(5) 0.033(7) C58 0.064(7) 0.095(9) 0.064(7) 0.032(7) 0.011(6) 0.006(7) C59 0.095(8) 0.058(7) 0.052(6) -0.006(5) 0.001(6) 0.012(7) C60 0.078(8) 0.047(7) 0.057(6) 0.008(6) -0.018(6) 0.005(6) C61 0.051(6) 0.045(6) 0.057(6) -0.008(5) 0.011(5) 0.005(5) C62 0.052(6) 0.110(9) 0.044(5) 0.014(6) 0.022(4) 0.022(6) C63 0.053(6) 0.102(9) 0.062(6) 0.024(7) 0.020(5) 0.025(6) C64 0.058(7) 0.112(10) 0.055(6) 0.000(7) -0.005(5) 0.011(7) C65 0.046(6) 0.095(9) 0.053(6) 0.006(6) 0.004(4) 0.008(6) C66 0.044(6) 0.071(7) 0.055(6) 0.011(5) -0.005(4) 0.013(5) C67 0.038(6) 0.064(7) 0.080(7) -0.017(6) 0.035(6) 0.003(5) C68 0.045(5) 0.049(6) 0.046(5) -0.002(5) 0.006(4) -0.002(5) C69 0.083(8) 0.091(9) 0.086(8) -0.010(8) -0.003(7) -0.007(8) C70 0.120(11) 0.050(7) 0.097(9) 0.020(7) -0.032(8) -0.004(7) C71 0.101(9) 0.054(7) 0.038(5) 0.011(5) 0.004(5) 0.030(7) C72 0.078(7) 0.033(6) 0.071(7) -0.017(5) -0.022(6) 0.012(6) C73 0.071(7) 0.036(6) 0.076(7) -0.012(6) -0.021(5) -0.007(6) C74 0.027(5) 0.060(7) 0.055(5) 0.004(5) 0.001(4) 0.009(5) C75 0.059(6) 0.040(6) 0.052(5) 0.005(5) 0.015(5) 0.001(5) C76 0.100(9) 0.058(7) 0.113(9) 0.000(7) 0.066(8) 0.015(7) C77 0.106(11) 0.082(10) 0.112(10) -0.027(8) 0.035(8) 0.022(9) C78 0.093(8) 0.035(6) 0.050(6) 0.000(5) 0.010(5) 0.027(6) C79 0.104(9) 0.060(8) 0.077(8) 0.003(6) 0.020(7) -0.026(7) C80 0.081(8) 0.057(7) 0.078(7) 0.016(6) 0.035(6) -0.007(6) C81 0.063(7) 0.056(7) 0.061(6) -0.003(6) 0.010(5) -0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.954(6) . ? Cu1 O8 1.965(6) . ? Cu1 N3 1.984(8) . ? Cu1 N2 2.026(7) . ? Cu1 O1W 2.339(6) . ? Cu2 O6 1.877(6) . ? Cu2 O13 1.948(6) . ? Cu2 N1 1.978(9) 4_848 ? Cu2 N5 2.025(8) . ? Cu2 O14 2.409(8) . ? Cu3 O2 1.947(6) . ? Cu3 O11 1.961(6) 1_365 ? Cu3 N4 2.013(7) 4_558 ? Cu3 N6 2.013(8) 1_455 ? O1 C46 1.195(12) . ? O1W H10B 0.9300 . ? O1W H10C 0.9299 . ? O2 C46 1.212(12) . ? O3 C53 1.297(11) . ? O4 C53 1.195(11) . ? O5 C50 1.366(10) . ? O5 C43 1.367(10) . ? O6 C60 1.259(12) . ? O7 C60 1.201(12) . ? O8 C67 1.218(12) . ? O9 C67 1.272(11) . ? O10 C57 1.365(11) . ? O10 C64 1.402(12) . ? O11 C74 1.287(10) . ? O11 Cu3 1.961(6) 1_745 ? O12 C74 1.248(10) . ? O13 C81 1.288(11) . ? O14 C81 1.237(11) . ? O15 C78 1.384(11) . ? O15 C71 1.475(11) . ? N1 C5 1.296(11) . ? N1 C1 1.439(15) . ? N1 Cu2 1.978(9) 4_858 ? N2 C10 1.257(12) . ? N2 C6 1.322(13) . ? N3 C18 1.351(12) . ? N3 C14 1.355(13) . ? N4 C23 1.267(10) . ? N4 C19 1.386(12) . ? N4 Cu3 2.013(7) 4_548 ? N5 C31 1.272(13) . ? N5 C27 1.403(14) . ? N6 C36 1.295(12) . ? N6 C32 1.326(12) . ? N6 Cu3 2.013(8) 1_655 ? C1 C2 1.323(17) . ? C1 H1A 0.9300 . ? C2 C3 1.374(16) . ? C2 H2A 0.9300 . ? C3 C4 1.307(16) . ? C3 C13 1.533(18) . ? C4 C5 1.390(15) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.303(17) . ? C6 H6A 0.9300 . ? C7 C8 1.29(2) . ? C7 H7A 0.9300 . ? C8 C9 1.36(2) . ? C8 C11 1.47(2) . ? C9 C10 1.352(18) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.340(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.53(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.388(14) . ? C14 H14A 0.9300 . ? C15 C16 1.349(13) . ? C15 H15B 0.9300 . ? C16 C17 1.286(13) . ? C16 C24 1.536(13) . ? C17 C18 1.382(15) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.276(13) . ? C19 H19A 0.9300 . ? C20 C21 1.423(14) . ? C20 H20D 0.9300 . ? C21 C22 1.394(14) . ? C21 C26 1.536(13) . ? C22 C23 1.369(14) . ? C22 H22B 0.9300 . ? C23 H23A 0.9300 . ? C24 C25 1.481(13) . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.519(13) . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 C28 1.301(14) . ? C27 H27A 0.9300 . ? C28 C29 1.403(16) . ? C28 H28A 0.9300 . ? C29 C30 1.361(15) . ? C29 C37 1.497(14) . ? C30 C31 1.413(15) . ? C30 H30A 0.9300 . ? C31 H31B 0.9300 . ? C32 C33 1.287(13) . ? C32 H32A 0.9300 . ? C33 C34 1.403(15) . ? C33 H33B 0.9300 . ? C34 C35 1.353(13) . ? C34 C39 1.492(14) . ? C35 C36 1.387(13) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C38 1.572(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.480(14) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C45 1.393(14) . ? C40 C41 1.464(14) . ? C40 C46 1.543(14) . ? C41 C42 1.487(15) . ? C41 H41A 0.9300 . ? C42 C43 1.262(14) . ? C42 H42A 0.9300 . ? C43 C44 1.321(12) . ? C44 C45 1.400(13) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C47 C48 1.314(11) . ? C47 C52 1.400(11) . ? C47 C53 1.556(13) . ? C48 C49 1.406(12) . ? C48 H48A 0.9300 . ? C49 C50 1.401(12) . ? C49 H49A 0.9300 . ? C50 C51 1.345(12) . ? C51 C52 1.403(12) . ? C51 H51B 0.9300 . ? C52 H52A 0.9300 . ? C54 C59 1.393(14) . ? C54 C55 1.418(13) . ? C54 C60 1.512(14) . ? C55 C56 1.382(15) . ? C55 H55A 0.9300 . ? C56 C57 1.383(16) . ? C56 H56A 0.9300 . ? C57 C58 1.327(14) . ? C58 C59 1.381(13) . ? C58 H58A 0.9300 . ? C59 H59A 0.9300 . ? C61 C66 1.396(12) . ? C61 C62 1.399(13) . ? C61 C67 1.575(13) . ? C62 C63 1.323(12) . ? C62 H62A 0.9300 . ? C63 C64 1.366(13) . ? C63 H63A 0.9300 . ? C64 C65 1.433(14) . ? C65 C66 1.359(12) . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C68 C69 1.380(14) . ? C68 C73 1.384(12) . ? C68 C74 1.432(12) . ? C69 C70 1.397(15) . ? C69 H69A 0.9300 . ? C70 C71 1.370(15) . ? C70 H70A 0.9300 . ? C71 C72 1.300(14) . ? C72 C73 1.336(12) . ? C72 H72A 0.9300 . ? C73 H73A 0.9300 . ? C75 C76 1.323(12) . ? C75 C80 1.322(13) . ? C75 C81 1.501(13) . ? C76 C77 1.421(14) . ? C76 H76A 0.9300 . ? C77 C78 1.404(15) . ? C77 H77A 0.9300 . ? C78 C79 1.317(14) . ? C79 C80 1.372(14) . ? C79 H79A 0.9300 . ? C80 H80A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 O8 170.6(3) . . ? O3 Cu1 N3 88.5(3) . . ? O8 Cu1 N3 91.6(3) . . ? O3 Cu1 N2 93.6(3) . . ? O8 Cu1 N2 89.2(3) . . ? N3 Cu1 N2 162.0(3) . . ? O3 Cu1 O1W 88.4(2) . . ? O8 Cu1 O1W 82.4(2) . . ? N3 Cu1 O1W 99.8(3) . . ? N2 Cu1 O1W 98.2(3) . . ? O6 Cu2 O13 152.0(4) . . ? O6 Cu2 N1 98.6(3) . 4_848 ? O13 Cu2 N1 92.5(3) . 4_848 ? O6 Cu2 N5 96.8(3) . . ? O13 Cu2 N5 92.0(3) . . ? N1 Cu2 N5 137.3(4) 4_848 . ? O6 Cu2 O14 94.1(3) . . ? O13 Cu2 O14 57.9(3) . . ? N1 Cu2 O14 112.6(3) 4_848 . ? N5 Cu2 O14 105.6(3) . . ? O2 Cu3 O11 149.7(4) . 1_365 ? O2 Cu3 N4 97.4(3) . 4_558 ? O11 Cu3 N4 90.5(3) 1_365 4_558 ? O2 Cu3 N6 92.4(3) . 1_455 ? O11 Cu3 N6 89.4(3) 1_365 1_455 ? N4 Cu3 N6 160.6(4) 4_558 1_455 ? Cu1 O1W H10B 119.9 . . ? Cu1 O1W H10C 120.1 . . ? H10B O1W H10C 120.0 . . ? C46 O2 Cu3 133.4(8) . . ? C53 O3 Cu1 115.4(6) . . ? C50 O5 C43 123.7(7) . . ? C60 O6 Cu2 123.6(7) . . ? C67 O8 Cu1 119.2(6) . . ? C57 O10 C64 120.2(8) . . ? C74 O11 Cu3 108.0(5) . 1_745 ? C81 O13 Cu2 102.7(6) . . ? C81 O14 Cu2 82.5(6) . . ? C78 O15 C71 114.3(7) . . ? C5 N1 C1 110.3(10) . . ? C5 N1 Cu2 128.2(7) . 4_858 ? C1 N1 Cu2 121.2(7) . 4_858 ? C10 N2 C6 115.3(10) . . ? C10 N2 Cu1 121.7(8) . . ? C6 N2 Cu1 121.6(7) . . ? C18 N3 C14 115.2(9) . . ? C18 N3 Cu1 123.9(7) . . ? C14 N3 Cu1 120.9(7) . . ? C23 N4 C19 114.0(8) . . ? C23 N4 Cu3 120.5(6) . 4_548 ? C19 N4 Cu3 124.9(6) . 4_548 ? C31 N5 C27 118.2(9) . . ? C31 N5 Cu2 118.8(8) . . ? C27 N5 Cu2 122.5(8) . . ? C36 N6 C32 117.0(9) . . ? C36 N6 Cu3 122.6(8) . 1_655 ? C32 N6 Cu3 120.1(7) . 1_655 ? C2 C1 N1 129.0(11) . . ? C2 C1 H1A 115.5 . . ? N1 C1 H1A 115.5 . . ? C1 C2 C3 113.8(12) . . ? C1 C2 H2A 123.1 . . ? C3 C2 H2A 123.1 . . ? C4 C3 C2 121.7(11) . . ? C4 C3 C13 122.5(14) . . ? C2 C3 C13 115.8(14) . . ? C3 C4 C5 120.2(11) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? N1 C5 C4 124.8(10) . . ? N1 C5 H5A 117.6 . . ? C4 C5 H5A 117.6 . . ? C7 C6 N2 122.2(12) . . ? C7 C6 H6A 118.9 . . ? N2 C6 H6A 118.9 . . ? C8 C7 C6 126.8(15) . . ? C8 C7 H7A 116.6 . . ? C6 C7 H7A 116.6 . . ? C7 C8 C9 109.1(13) . . ? C7 C8 C11 128.2(17) . . ? C9 C8 C11 122.4(18) . . ? C10 C9 C8 124.6(13) . . ? C10 C9 H9A 117.7 . . ? C8 C9 H9A 117.6 . . ? N2 C10 C9 121.7(13) . . ? N2 C10 H10A 119.2 . . ? C9 C10 H10A 119.1 . . ? C12 C11 C8 119.0(17) . . ? C12 C11 H11A 107.6 . . ? C8 C11 H11A 107.6 . . ? C12 C11 H11B 107.4 . . ? C8 C11 H11B 107.6 . . ? H11A C11 H11B 107.0 . . ? C11 C12 C13 121.5(16) . . ? C11 C12 H12A 106.9 . . ? C13 C12 H12A 106.9 . . ? C11 C12 H12B 107.1 . . ? C13 C12 H12B 106.9 . . ? H12A C12 H12B 106.7 . . ? C12 C13 C3 117.1(14) . . ? C12 C13 H13A 108.0 . . ? C3 C13 H13A 108.0 . . ? C12 C13 H13B 108.1 . . ? C3 C13 H13B 108.0 . . ? H13A C13 H13B 107.2 . . ? N3 C14 C15 120.9(10) . . ? N3 C14 H14A 119.5 . . ? C15 C14 H14A 119.6 . . ? C16 C15 C14 121.2(10) . . ? C16 C15 H15B 119.4 . . ? C14 C15 H15B 119.4 . . ? C17 C16 C15 118.2(10) . . ? C17 C16 C24 123.9(9) . . ? C15 C16 C24 117.9(9) . . ? C16 C17 C18 121.5(10) . . ? C16 C17 H17A 119.2 . . ? C18 C17 H17A 119.2 . . ? N3 C18 C17 122.7(10) . . ? N3 C18 H18A 118.6 . . ? C17 C18 H18A 118.7 . . ? C20 C19 N4 129.2(8) . . ? C20 C19 H19A 115.4 . . ? N4 C19 H19A 115.4 . . ? C19 C20 C21 117.0(9) . . ? C19 C20 H20D 121.5 . . ? C21 C20 H20D 121.5 . . ? C22 C21 C20 114.4(10) . . ? C22 C21 C26 122.1(11) . . ? C20 C21 C26 123.4(9) . . ? C23 C22 C21 122.1(11) . . ? C23 C22 H22B 119.0 . . ? C21 C22 H22B 118.9 . . ? N4 C23 C22 123.1(9) . . ? N4 C23 H23A 118.4 . . ? C22 C23 H23A 118.4 . . ? C25 C24 C16 115.7(8) . . ? C25 C24 H24B 108.4 . . ? C16 C24 H24B 108.4 . . ? C25 C24 H24C 108.3 . . ? C16 C24 H24C 108.4 . . ? H24B C24 H24C 107.4 . . ? C24 C25 C26 108.5(8) . . ? C24 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? C24 C25 H25C 110.0 . . ? C26 C25 H25C 110.0 . . ? H25B C25 H25C 108.4 . . ? C25 C26 C21 111.1(8) . . ? C25 C26 H26B 109.4 . . ? C21 C26 H26B 109.4 . . ? C25 C26 H26C 109.4 . . ? C21 C26 H26C 109.4 . . ? H26B C26 H26C 108.0 . . ? C28 C27 N5 119.4(12) . . ? C28 C27 H27A 120.3 . . ? N5 C27 H27A 120.3 . . ? C27 C28 C29 124.0(12) . . ? C27 C28 H28A 118.0 . . ? C29 C28 H28A 118.0 . . ? C30 C29 C28 115.7(10) . . ? C30 C29 C37 121.1(12) . . ? C28 C29 C37 123.1(11) . . ? C29 C30 C31 118.5(12) . . ? C29 C30 H30A 120.7 . . ? C31 C30 H30A 120.7 . . ? N5 C31 C30 123.9(11) . . ? N5 C31 H31B 118.0 . . ? C30 C31 H31B 118.1 . . ? C33 C32 N6 123.9(10) . . ? C33 C32 H32A 118.0 . . ? N6 C32 H32A 118.0 . . ? C32 C33 C34 122.1(10) . . ? C32 C33 H33B 118.9 . . ? C34 C33 H33B 119.0 . . ? C35 C34 C33 113.7(10) . . ? C35 C34 C39 124.3(10) . . ? C33 C34 C39 121.9(10) . . ? C34 C35 C36 121.1(10) . . ? C34 C35 H35A 119.5 . . ? C36 C35 H35A 119.5 . . ? N6 C36 C35 122.1(11) . . ? N6 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C29 C37 C38 108.8(8) . . ? C29 C37 H37A 109.9 . . ? C38 C37 H37A 109.9 . . ? C29 C37 H37B 109.9 . . ? C38 C37 H37B 109.9 . . ? H37A C37 H37B 108.3 . . ? C39 C38 C37 114.2(9) . . ? C39 C38 H38A 108.7 . . ? C37 C38 H38A 108.7 . . ? C39 C38 H38B 108.7 . . ? C37 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C38 C39 C34 110.8(9) . . ? C38 C39 H39A 109.5 . . ? C34 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? C45 C40 C41 119.2(10) . . ? C45 C40 C46 123.7(10) . . ? C41 C40 C46 116.8(11) . . ? C40 C41 C42 113.1(11) . . ? C40 C41 H41A 123.5 . . ? C42 C41 H41A 123.5 . . ? C43 C42 C41 123.7(10) . . ? C43 C42 H42A 118.2 . . ? C41 C42 H42A 118.1 . . ? C42 C43 C44 123.0(10) . . ? C42 C43 O5 117.5(10) . . ? C44 C43 O5 118.9(9) . . ? C43 C44 C45 120.9(10) . . ? C43 C44 H44A 119.6 . . ? C45 C44 H44A 119.6 . . ? C40 C45 C44 120.1(10) . . ? C40 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? O1 C46 O2 130.5(10) . . ? O1 C46 C40 117.5(11) . . ? O2 C46 C40 111.8(10) . . ? C48 C47 C52 119.4(8) . . ? C48 C47 C53 118.2(8) . . ? C52 C47 C53 122.3(8) . . ? C47 C48 C49 122.5(9) . . ? C47 C48 H48A 118.7 . . ? C49 C48 H48A 118.7 . . ? C50 C49 C48 117.7(9) . . ? C50 C49 H49A 121.2 . . ? C48 C49 H49A 121.2 . . ? C51 C50 O5 124.3(8) . . ? C51 C50 C49 120.7(9) . . ? O5 C50 C49 115.0(8) . . ? C50 C51 C52 119.9(9) . . ? C50 C51 H51B 120.1 . . ? C52 C51 H51B 120.0 . . ? C47 C52 C51 119.7(8) . . ? C47 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? O4 C53 O3 126.2(9) . . ? O4 C53 C47 120.4(8) . . ? O3 C53 C47 113.3(9) . . ? C59 C54 C55 119.1(9) . . ? C59 C54 C60 119.9(9) . . ? C55 C54 C60 120.9(10) . . ? C56 C55 C54 118.8(11) . . ? C56 C55 H55A 120.6 . . ? C54 C55 H55A 120.6 . . ? C57 C56 C55 121.4(11) . . ? C57 C56 H56A 119.3 . . ? C55 C56 H56A 119.3 . . ? C58 C57 O10 120.8(12) . . ? C58 C57 C56 118.3(9) . . ? O10 C57 C56 120.5(11) . . ? C57 C58 C59 124.2(11) . . ? C57 C58 H58A 117.9 . . ? C59 C58 H58A 117.9 . . ? C58 C59 C54 117.9(10) . . ? C58 C59 H59A 121.0 . . ? C54 C59 H59A 121.0 . . ? O7 C60 O6 126.1(11) . . ? O7 C60 C54 116.7(11) . . ? O6 C60 C54 117.0(10) . . ? C66 C61 C62 119.7(8) . . ? C66 C61 C67 115.8(8) . . ? C62 C61 C67 124.4(8) . . ? C63 C62 C61 120.7(9) . . ? C63 C62 H62A 119.7 . . ? C61 C62 H62A 119.7 . . ? C62 C63 C64 120.9(10) . . ? C62 C63 H63A 119.6 . . ? C64 C63 H63A 119.6 . . ? C63 C64 O10 115.8(9) . . ? C63 C64 C65 119.8(10) . . ? O10 C64 C65 124.3(8) . . ? C66 C65 C64 118.8(9) . . ? C66 C65 H65A 120.6 . . ? C64 C65 H65A 120.6 . . ? C65 C66 C61 119.7(9) . . ? C65 C66 H66A 120.1 . . ? C61 C66 H66A 120.1 . . ? O8 C67 O9 129.4(9) . . ? O8 C67 C61 118.2(8) . . ? O9 C67 C61 112.2(10) . . ? C69 C68 C73 115.5(10) . . ? C69 C68 C74 121.7(9) . . ? C73 C68 C74 122.8(9) . . ? C68 C69 C70 122.1(11) . . ? C68 C69 H69A 118.9 . . ? C70 C69 H69A 118.9 . . ? C71 C70 C69 115.0(11) . . ? C71 C70 H70A 122.5 . . ? C69 C70 H70A 122.5 . . ? C72 C71 C70 125.8(10) . . ? C72 C71 O15 118.8(10) . . ? C70 C71 O15 115.4(11) . . ? C71 C72 C73 117.4(10) . . ? C71 C72 H72A 121.3 . . ? C73 C72 H72A 121.3 . . ? C72 C73 C68 124.1(10) . . ? C72 C73 H73A 117.9 . . ? C68 C73 H73A 117.9 . . ? O12 C74 O11 119.6(9) . . ? O12 C74 C68 123.0(10) . . ? O11 C74 C68 117.4(8) . . ? C76 C75 C80 119.3(10) . . ? C76 C75 C81 120.2(9) . . ? C80 C75 C81 120.5(9) . . ? C75 C76 C77 120.8(11) . . ? C75 C76 H76A 119.6 . . ? C77 C76 H76A 119.6 . . ? C78 C77 C76 116.6(11) . . ? C78 C77 H77A 121.7 . . ? C76 C77 H77A 121.7 . . ? C79 C78 O15 125.2(10) . . ? C79 C78 C77 120.8(10) . . ? O15 C78 C77 113.7(10) . . ? C78 C79 C80 118.7(10) . . ? C78 C79 H79A 120.7 . . ? C80 C79 H79A 120.7 . . ? C75 C80 C79 123.3(9) . . ? C75 C80 H80A 118.4 . . ? C79 C80 H80A 118.4 . . ? O14 C81 O13 116.5(10) . . ? O14 C81 C75 126.8(10) . . ? O13 C81 C75 116.2(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Cu3 O2 C46 179.6(8) 1_365 . . . ? N4 Cu3 O2 C46 75.9(10) 4_558 . . . ? N6 Cu3 O2 C46 -87.4(10) 1_455 . . . ? O8 Cu1 O3 C53 161.6(15) . . . . ? N3 Cu1 O3 C53 71.1(7) . . . . ? N2 Cu1 O3 C53 -91.0(7) . . . . ? O1W Cu1 O3 C53 170.9(7) . . . . ? O13 Cu2 O6 C60 -176.8(7) . . . . ? N1 Cu2 O6 C60 70.8(8) 4_848 . . . ? N5 Cu2 O6 C60 -69.2(8) . . . . ? O14 Cu2 O6 C60 -175.6(8) . . . . ? O3 Cu1 O8 C67 -170.3(14) . . . . ? N3 Cu1 O8 C67 -80.1(8) . . . . ? N2 Cu1 O8 C67 81.9(7) . . . . ? O1W Cu1 O8 C67 -179.7(8) . . . . ? O6 Cu2 O13 C81 -1.7(11) . . . . ? N1 Cu2 O13 C81 112.1(7) 4_848 . . . ? N5 Cu2 O13 C81 -110.4(7) . . . . ? O14 Cu2 O13 C81 -3.2(6) . . . . ? O6 Cu2 O14 C81 -176.1(6) . . . . ? O13 Cu2 O14 C81 3.2(6) . . . . ? N1 Cu2 O14 C81 -75.0(7) 4_848 . . . ? N5 Cu2 O14 C81 85.6(7) . . . . ? O3 Cu1 N2 C10 62.9(10) . . . . ? O8 Cu1 N2 C10 -126.0(10) . . . . ? N3 Cu1 N2 C10 -33.3(15) . . . . ? O1W Cu1 N2 C10 151.8(10) . . . . ? O3 Cu1 N2 C6 -130.9(9) . . . . ? O8 Cu1 N2 C6 40.1(9) . . . . ? N3 Cu1 N2 C6 132.8(11) . . . . ? O1W Cu1 N2 C6 -42.0(9) . . . . ? O3 Cu1 N3 C18 -114.6(8) . . . . ? O8 Cu1 N3 C18 74.8(8) . . . . ? N2 Cu1 N3 C18 -17.6(13) . . . . ? O1W Cu1 N3 C18 157.3(7) . . . . ? O3 Cu1 N3 C14 62.4(7) . . . . ? O8 Cu1 N3 C14 -108.2(7) . . . . ? N2 Cu1 N3 C14 159.4(9) . . . . ? O1W Cu1 N3 C14 -25.7(7) . . . . ? O6 Cu2 N5 C31 127.7(9) . . . . ? O13 Cu2 N5 C31 -78.9(9) . . . . ? N1 Cu2 N5 C31 17.1(11) 4_848 . . . ? O14 Cu2 N5 C31 -136.0(9) . . . . ? O6 Cu2 N5 C27 -59.9(9) . . . . ? O13 Cu2 N5 C27 93.6(9) . . . . ? N1 Cu2 N5 C27 -170.5(8) 4_848 . . . ? O14 Cu2 N5 C27 36.4(9) . . . . ? C5 N1 C1 C2 -2.1(19) . . . . ? Cu2 N1 C1 C2 172.3(13) 4_858 . . . ? N1 C1 C2 C3 5(2) . . . . ? C1 C2 C3 C4 -2(2) . . . . ? C1 C2 C3 C13 179.1(13) . . . . ? C2 C3 C4 C5 -3(2) . . . . ? C13 C3 C4 C5 175.9(12) . . . . ? C1 N1 C5 C4 -3.5(16) . . . . ? Cu2 N1 C5 C4 -177.4(9) 4_858 . . . ? C3 C4 C5 N1 6(2) . . . . ? C10 N2 C6 C7 -5(2) . . . . ? Cu1 N2 C6 C7 -172.0(16) . . . . ? N2 C6 C7 C8 8(4) . . . . ? C6 C7 C8 C9 -4(3) . . . . ? C6 C7 C8 C11 169(2) . . . . ? C7 C8 C9 C10 -1(3) . . . . ? C11 C8 C9 C10 -174.8(16) . . . . ? C6 N2 C10 C9 0(2) . . . . ? Cu1 N2 C10 C9 167.2(11) . . . . ? C8 C9 C10 N2 3(3) . . . . ? C7 C8 C11 C12 89(3) . . . . ? C9 C8 C11 C12 -98(3) . . . . ? C8 C11 C12 C13 177.1(19) . . . . ? C11 C12 C13 C3 28(3) . . . . ? C4 C3 C13 C12 71(2) . . . . ? C2 C3 C13 C12 -110(2) . . . . ? C18 N3 C14 C15 -6.5(14) . . . . ? Cu1 N3 C14 C15 176.2(8) . . . . ? N3 C14 C15 C16 4.5(16) . . . . ? C14 C15 C16 C17 -0.5(16) . . . . ? C14 C15 C16 C24 176.1(9) . . . . ? C15 C16 C17 C18 -1.0(17) . . . . ? C24 C16 C17 C18 -177.4(10) . . . . ? C14 N3 C18 C17 5.1(15) . . . . ? Cu1 N3 C18 C17 -177.7(9) . . . . ? C16 C17 C18 N3 -1.4(19) . . . . ? C23 N4 C19 C20 -0.4(18) . . . . ? Cu3 N4 C19 C20 -172.2(11) 4_548 . . . ? N4 C19 C20 C21 0.3(19) . . . . ? C19 C20 C21 C22 -0.9(16) . . . . ? C19 C20 C21 C26 176.7(11) . . . . ? C20 C21 C22 C23 1.8(18) . . . . ? C26 C21 C22 C23 -175.9(11) . . . . ? C19 N4 C23 C22 1.3(17) . . . . ? Cu3 N4 C23 C22 173.5(10) 4_548 . . . ? C21 C22 C23 N4 -2(2) . . . . ? C17 C16 C24 C25 74.1(13) . . . . ? C15 C16 C24 C25 -102.3(11) . . . . ? C16 C24 C25 C26 -177.3(8) . . . . ? C24 C25 C26 C21 -173.4(8) . . . . ? C22 C21 C26 C25 -64.7(14) . . . . ? C20 C21 C26 C25 117.8(11) . . . . ? C31 N5 C27 C28 -2.7(18) . . . . ? Cu2 N5 C27 C28 -175.2(10) . . . . ? N5 C27 C28 C29 1(2) . . . . ? C27 C28 C29 C30 -0.6(19) . . . . ? C27 C28 C29 C37 -179.4(12) . . . . ? C28 C29 C30 C31 1.6(17) . . . . ? C37 C29 C30 C31 -179.5(10) . . . . ? C27 N5 C31 C30 4.0(18) . . . . ? Cu2 N5 C31 C30 176.8(10) . . . . ? C29 C30 C31 N5 -4(2) . . . . ? C36 N6 C32 C33 -1.7(17) . . . . ? Cu3 N6 C32 C33 -175.9(10) 1_655 . . . ? N6 C32 C33 C34 2.5(19) . . . . ? C32 C33 C34 C35 -2.8(17) . . . . ? C32 C33 C34 C39 173.2(11) . . . . ? C33 C34 C35 C36 2.5(15) . . . . ? C39 C34 C35 C36 -173.4(11) . . . . ? C32 N6 C36 C35 1.4(16) . . . . ? Cu3 N6 C36 C35 175.4(8) 1_655 . . . ? C34 C35 C36 N6 -2.0(17) . . . . ? C30 C29 C37 C38 -103.5(12) . . . . ? C28 C29 C37 C38 75.3(14) . . . . ? C29 C37 C38 C39 177.1(11) . . . . ? C37 C38 C39 C34 -178.6(10) . . . . ? C35 C34 C39 C38 58.1(16) . . . . ? C33 C34 C39 C38 -117.6(12) . . . . ? C45 C40 C41 C42 1.8(12) . . . . ? C46 C40 C41 C42 176.0(8) . . . . ? C40 C41 C42 C43 -1.7(14) . . . . ? C41 C42 C43 C44 1.5(17) . . . . ? C41 C42 C43 O5 172.6(8) . . . . ? C50 O5 C43 C42 63.7(13) . . . . ? C50 O5 C43 C44 -124.8(10) . . . . ? C42 C43 C44 C45 -1.4(16) . . . . ? O5 C43 C44 C45 -172.4(8) . . . . ? C41 C40 C45 C44 -1.9(14) . . . . ? C46 C40 C45 C44 -175.6(8) . . . . ? C43 C44 C45 C40 1.6(14) . . . . ? Cu3 O2 C46 O1 -4(2) . . . . ? Cu3 O2 C46 C40 -178.4(6) . . . . ? C45 C40 C46 O1 -167.8(10) . . . . ? C41 C40 C46 O1 18.4(14) . . . . ? C45 C40 C46 O2 7.3(14) . . . . ? C41 C40 C46 O2 -166.5(9) . . . . ? C52 C47 C48 C49 -1.4(16) . . . . ? C53 C47 C48 C49 176.5(9) . . . . ? C47 C48 C49 C50 3.1(16) . . . . ? C43 O5 C50 C51 9.7(15) . . . . ? C43 O5 C50 C49 -173.0(9) . . . . ? C48 C49 C50 C51 -1.4(15) . . . . ? C48 C49 C50 O5 -178.8(9) . . . . ? O5 C50 C51 C52 175.4(9) . . . . ? C49 C50 C51 C52 -1.8(15) . . . . ? C48 C47 C52 C51 -1.8(14) . . . . ? C53 C47 C52 C51 -179.7(8) . . . . ? C50 C51 C52 C47 3.5(14) . . . . ? Cu1 O3 C53 O4 9.1(14) . . . . ? Cu1 O3 C53 C47 -167.8(6) . . . . ? C48 C47 C53 O4 28.5(15) . . . . ? C52 C47 C53 O4 -153.7(10) . . . . ? C48 C47 C53 O3 -154.4(9) . . . . ? C52 C47 C53 O3 23.4(13) . . . . ? C59 C54 C55 C56 -2.2(15) . . . . ? C60 C54 C55 C56 177.8(9) . . . . ? C54 C55 C56 C57 -1.1(16) . . . . ? C64 O10 C57 C58 -117.6(12) . . . . ? C64 O10 C57 C56 69.1(14) . . . . ? C55 C56 C57 C58 0.9(17) . . . . ? C55 C56 C57 O10 174.3(9) . . . . ? O10 C57 C58 C59 -170.7(9) . . . . ? C56 C57 C58 C59 2.7(16) . . . . ? C57 C58 C59 C54 -5.9(15) . . . . ? C55 C54 C59 C58 5.4(14) . . . . ? C60 C54 C59 C58 -174.6(8) . . . . ? Cu2 O6 C60 O7 -7.4(15) . . . . ? Cu2 O6 C60 C54 176.6(6) . . . . ? C59 C54 C60 O7 -179.3(10) . . . . ? C55 C54 C60 O7 0.7(14) . . . . ? C59 C54 C60 O6 -2.9(13) . . . . ? C55 C54 C60 O6 177.1(9) . . . . ? C66 C61 C62 C63 3.0(16) . . . . ? C67 C61 C62 C63 179.8(10) . . . . ? C61 C62 C63 C64 -7.2(19) . . . . ? C62 C63 C64 O10 -175.4(11) . . . . ? C62 C63 C64 C65 7.2(19) . . . . ? C57 O10 C64 C63 -171.1(11) . . . . ? C57 O10 C64 C65 6.2(18) . . . . ? C63 C64 C65 C66 -2.9(17) . . . . ? O10 C64 C65 C66 180.0(10) . . . . ? C64 C65 C66 C61 -1.2(16) . . . . ? C62 C61 C66 C65 1.3(15) . . . . ? C67 C61 C66 C65 -175.8(9) . . . . ? Cu1 O8 C67 O9 -0.7(15) . . . . ? Cu1 O8 C67 C61 -175.2(6) . . . . ? C66 C61 C67 O8 17.6(13) . . . . ? C62 C61 C67 O8 -159.3(10) . . . . ? C66 C61 C67 O9 -157.8(9) . . . . ? C62 C61 C67 O9 25.3(14) . . . . ? C73 C68 C69 C70 -0.3(16) . . . . ? C74 C68 C69 C70 -179.6(10) . . . . ? C68 C69 C70 C71 1.1(17) . . . . ? C69 C70 C71 C72 -2.1(18) . . . . ? C69 C70 C71 O15 179.3(9) . . . . ? C78 O15 C71 C72 101.7(11) . . . . ? C78 O15 C71 C70 -79.6(12) . . . . ? C70 C71 C72 C73 2.2(17) . . . . ? O15 C71 C72 C73 -179.3(8) . . . . ? C71 C72 C73 C68 -1.2(16) . . . . ? C69 C68 C73 C72 0.3(15) . . . . ? C74 C68 C73 C72 179.6(9) . . . . ? Cu3 O11 C74 O12 11.5(10) 1_745 . . . ? Cu3 O11 C74 C68 -167.9(6) 1_745 . . . ? C69 C68 C74 O12 5.9(14) . . . . ? C73 C68 C74 O12 -173.3(8) . . . . ? C69 C68 C74 O11 -174.7(9) . . . . ? C73 C68 C74 O11 6.1(13) . . . . ? C80 C75 C76 C77 -1.4(18) . . . . ? C81 C75 C76 C77 178.9(11) . . . . ? C75 C76 C77 C78 -4.1(19) . . . . ? C71 O15 C78 C79 -51.9(15) . . . . ? C71 O15 C78 C77 133.8(11) . . . . ? C76 C77 C78 C79 8.0(18) . . . . ? C76 C77 C78 O15 -177.4(10) . . . . ? O15 C78 C79 C80 179.8(10) . . . . ? C77 C78 C79 C80 -6.3(18) . . . . ? C76 C75 C80 C79 3.5(18) . . . . ? C81 C75 C80 C79 -176.9(10) . . . . ? C78 C79 C80 C75 0.4(19) . . . . ? Cu2 O14 C81 O13 -4.6(9) . . . . ? Cu2 O14 C81 C75 167.8(11) . . . . ? Cu2 O13 C81 O14 5.8(11) . . . . ? Cu2 O13 C81 C75 -167.5(7) . . . . ? C76 C75 C81 O14 -174.5(11) . . . . ? C80 C75 C81 O14 5.8(17) . . . . ? C76 C75 C81 O13 -2.0(15) . . . . ? C80 C75 C81 O13 178.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.580 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.083