# 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 'Hardie, Michaele' _publ_contact_author_email m.j.hardie@leeds.ac.uk _publ_section_title ; Bow-tie metallo-cryptophanes from a carboxylate derived cavitand ; loop_ _publ_author_name M.Hardie T.Ronson H.Nowell A.Westcott # Attachment 'compound1-776456-.CIF.txt' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 776456' #TrackingRef 'compound1-776456-.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; di{tris[3,5-bis(methyl)benzoate]cyclotricatechylene}- tris(dimethylformamide)tricopper(ii) dimethylformamide clathrate ; _chemical_name_common ; di(tris(3,5-bis(methyl)benzoate)cyclotricatechylene)- tris(dimethylformamide)tricopper(ii) dimethylformamide clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C111 H101 Cu3 N5 O29' _chemical_formula_weight 2159.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0641(11) _cell_length_b 18.8982(17) _cell_length_c 22.4670(19) _cell_angle_alpha 94.765(4) _cell_angle_beta 91.139(4) _cell_angle_gamma 92.562(5) _cell_volume 5098.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9367 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.55 _exptl_crystal_description plate _exptl_crystal_colour green-blue _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2242 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type multi-scan' _exptl_absorpt_correction_T_min 0.7113 _exptl_absorpt_correction_T_max 0.9590 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS (Sheldrick, G. M. 2003) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 187717 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.50 _reflns_number_total 23414 _reflns_number_gt 20056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _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^)+(0.0466P)^2^+4.0593P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23414 _refine_ls_number_parameters 1366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.200163(16) 0.083726(10) 0.823077(9) 0.01564(5) Uani 1 1 d . . . Cu2 Cu -0.019721(17) -0.007348(10) 0.744764(9) 0.01670(5) Uani 1 1 d . . . Cu3 Cu 0.246678(16) -0.003642(10) 0.685818(8) 0.01532(5) Uani 1 1 d . . . O1 O 0.28049(11) 0.42234(7) 0.77814(6) 0.0240(3) Uani 1 1 d . . . O2 O 0.08231(11) 0.42073(7) 0.82321(6) 0.0271(3) Uani 1 1 d . . . O3 O -0.33497(11) 0.24314(7) 0.67066(7) 0.0291(3) Uani 1 1 d . . . O4 O -0.30639(11) 0.17624(7) 0.56576(7) 0.0289(3) Uani 1 1 d . . . O5 O 0.20225(11) 0.18087(7) 0.45143(6) 0.0254(3) Uani 1 1 d . . . O6 O 0.36634(11) 0.24867(7) 0.51256(5) 0.0243(3) Uani 1 1 d . . . O7 O 0.06669(10) 0.14007(7) 0.83196(6) 0.0240(3) Uani 1 1 d . . . O8 O -0.04955(11) 0.09342(6) 0.75690(6) 0.0264(3) Uani 1 1 d . . . O9 O -0.02454(11) 0.00542(7) 0.65890(5) 0.0245(3) Uani 1 1 d . . . O10 O 0.14884(11) 0.04296(7) 0.63476(6) 0.0293(3) Uani 1 1 d . . . O11 O 0.33395(10) 0.08764(6) 0.69529(6) 0.0226(3) Uani 1 1 d . . . O12 O 0.25087(11) 0.15304(7) 0.76943(6) 0.0264(3) Uani 1 1 d . . . O13 O -0.10430(11) -0.33616(7) 0.81058(6) 0.0262(3) Uani 1 1 d . . . O14 O -0.13879(10) -0.27214(7) 0.91696(6) 0.0243(3) Uani 1 1 d . . . O15 O 0.29145(10) -0.08556(6) 1.05477(5) 0.0213(2) Uani 1 1 d . . . O16 O 0.49196(10) -0.08547(6) 1.01153(5) 0.0195(2) Uani 1 1 d . . . O17 O 0.57034(11) -0.26374(7) 0.74565(5) 0.0228(3) Uani 1 1 d . . . O18 O 0.39905(11) -0.33193(7) 0.68900(5) 0.0246(3) Uani 1 1 d . . . O19 O 0.17391(11) -0.10008(6) 0.67095(6) 0.0228(3) Uani 1 1 d . . . O20 O 0.03090(12) -0.10319(7) 0.73502(6) 0.0303(3) Uani 1 1 d . . . O21 O -0.03304(11) -0.02367(7) 0.83078(5) 0.0234(3) Uani 1 1 d . . . O22 O 0.14189(11) 0.00641(8) 0.86538(7) 0.0325(3) Uani 1 1 d . . . O23 O 0.34199(10) 0.03575(6) 0.82657(5) 0.0206(2) Uani 1 1 d . . . O24 O 0.33058(11) -0.04674(7) 0.74719(6) 0.0258(3) Uani 1 1 d . . . O25 O 0.37140(11) -0.03705(7) 0.61310(6) 0.0278(3) Uani 1 1 d . . . O26 O 0.27060(12) 0.16676(8) 0.90422(6) 0.0310(3) Uani 1 1 d . . . O27 O -0.21225(12) -0.03773(8) 0.73136(7) 0.0341(3) Uani 1 1 d . . . N1 N 0.51085(15) -0.11571(10) 0.59874(7) 0.0314(4) Uani 1 1 d . . . N2 N 0.39433(15) 0.26029(9) 0.89096(7) 0.0311(4) Uani 1 1 d . . . N3 N -0.34409(13) 0.04544(9) 0.74985(8) 0.0298(4) Uani 1 1 d . . . C1 C 0.13678(17) 0.45576(10) 0.57331(9) 0.0272(4) Uani 1 1 d . . . H1A H 0.2067 0.4846 0.5703 0.033 Uiso 1 1 calc R . . H1B H 0.0763 0.4813 0.5554 0.033 Uiso 1 1 calc R . . C2 C 0.11297(16) 0.44890(9) 0.63954(9) 0.0241(4) Uani 1 1 d . . . C3 C 0.20596(15) 0.44153(9) 0.67802(8) 0.0227(4) Uani 1 1 d . . . H3 H 0.2784 0.4438 0.6623 0.027 Uiso 1 1 calc R . . C4 C 0.19349(15) 0.43103(9) 0.73832(8) 0.0225(4) Uani 1 1 d . . . C5 C 0.08570(16) 0.43009(9) 0.76275(8) 0.0243(4) Uani 1 1 d . . . C6 C -0.00535(16) 0.44004(9) 0.72525(9) 0.0262(4) Uani 1 1 d . . . H6 H -0.0773 0.4413 0.7417 0.031 Uiso 1 1 calc R . . C7 C 0.00651(16) 0.44837(9) 0.66337(9) 0.0256(4) Uani 1 1 d . . . C8 C -0.09970(17) 0.45457(10) 0.62546(10) 0.0300(4) Uani 1 1 d . . . H8A H -0.0814 0.4811 0.5905 0.036 Uiso 1 1 calc R . . H8B H -0.1535 0.4820 0.6495 0.036 Uiso 1 1 calc R . . C9 C -0.15394(16) 0.38127(10) 0.60349(9) 0.0275(4) Uani 1 1 d . . . C10 C -0.22261(15) 0.34806(10) 0.64438(10) 0.0279(4) Uani 1 1 d . . . H10 H -0.2371 0.3733 0.6816 0.033 Uiso 1 1 calc R . . C11 C -0.26975(15) 0.27934(10) 0.63181(9) 0.0268(4) Uani 1 1 d . . . C12 C -0.25305(15) 0.24329(10) 0.57514(9) 0.0271(4) Uani 1 1 d . . . C13 C -0.18901(15) 0.27686(10) 0.53363(9) 0.0274(4) Uani 1 1 d . . . H13 H -0.1804 0.2534 0.4951 0.033 Uiso 1 1 calc R . . C14 C -0.13621(15) 0.34554(10) 0.54758(9) 0.0272(4) Uani 1 1 d . . . C15 C -0.05909(17) 0.37451(10) 0.50057(9) 0.0289(4) Uani 1 1 d . . . H15A H -0.0915 0.3606 0.4602 0.035 Uiso 1 1 calc R . . H15B H -0.0546 0.4271 0.5063 0.035 Uiso 1 1 calc R . . C16 C 0.05870(16) 0.34694(10) 0.50419(8) 0.0247(4) Uani 1 1 d . . . C17 C 0.07737(16) 0.27965(10) 0.47417(8) 0.0250(4) Uani 1 1 d . . . H17 H 0.0191 0.2561 0.4501 0.030 Uiso 1 1 calc R . . C18 C 0.17834(16) 0.24677(10) 0.47875(7) 0.0225(4) Uani 1 1 d . . . C19 C 0.26708(15) 0.28363(10) 0.51239(8) 0.0220(3) Uani 1 1 d . . . C20 C 0.25101(15) 0.35136(10) 0.53971(8) 0.0228(4) Uani 1 1 d . . . H20 H 0.3116 0.3768 0.5605 0.027 Uiso 1 1 calc R . . C21 C 0.14695(16) 0.38345(9) 0.53736(8) 0.0243(4) Uani 1 1 d . . . C22 C -0.02494(16) 0.40892(10) 0.84983(9) 0.0279(4) Uani 1 1 d . . . H22A H -0.0728 0.4484 0.8418 0.033 Uiso 1 1 calc R . . H22B H -0.0147 0.4089 0.8937 0.033 Uiso 1 1 calc R . . C23 C -0.08262(15) 0.33846(9) 0.82528(8) 0.0235(4) Uani 1 1 d . . . C24 C -0.02663(14) 0.27473(9) 0.82595(8) 0.0207(3) Uani 1 1 d . . . H24 H 0.0431 0.2743 0.8463 0.025 Uiso 1 1 calc R . . C25 C -0.07418(14) 0.21170(9) 0.79649(8) 0.0187(3) Uani 1 1 d . . . C26 C -0.17621(14) 0.21230(9) 0.76557(8) 0.0207(3) Uani 1 1 d . . . H26 H -0.2059 0.1701 0.7440 0.025 Uiso 1 1 calc R . . C27 C -0.23494(14) 0.27504(10) 0.76623(9) 0.0236(4) Uani 1 1 d . . . C28 C -0.18782(15) 0.33727(10) 0.79696(9) 0.0263(4) Uani 1 1 d . . . H28 H -0.2279 0.3795 0.7987 0.032 Uiso 1 1 calc R . . C29 C -0.34395(15) 0.27575(11) 0.73064(10) 0.0291(4) Uani 1 1 d . . . H29A H -0.4030 0.2500 0.7513 0.035 Uiso 1 1 calc R . . H29B H -0.3655 0.3255 0.7289 0.035 Uiso 1 1 calc R . . C30 C -0.01330(14) 0.14275(9) 0.79493(7) 0.0179(3) Uani 1 1 d . . . C31 C -0.27631(15) 0.13089(10) 0.51354(9) 0.0269(4) Uani 1 1 d . . . H31A H -0.2888 0.1560 0.4772 0.032 Uiso 1 1 calc R . . H31B H -0.3251 0.0871 0.5103 0.032 Uiso 1 1 calc R . . C32 C -0.15569(15) 0.11053(9) 0.51641(8) 0.0212(3) Uani 1 1 d . . . C33 C -0.11406(15) 0.08048(9) 0.56700(8) 0.0197(3) Uani 1 1 d . . . H33 H -0.1624 0.0692 0.5981 0.024 Uiso 1 1 calc R . . C34 C -0.00045(14) 0.06724(9) 0.57139(7) 0.0178(3) Uani 1 1 d . . . C35 C 0.07232(14) 0.08480(9) 0.52609(7) 0.0191(3) Uani 1 1 d . . . H35 H 0.1493 0.0773 0.5301 0.023 Uiso 1 1 calc R . . C36 C 0.03068(15) 0.11351(9) 0.47478(7) 0.0206(3) Uani 1 1 d . . . C37 C -0.08347(15) 0.12510(9) 0.47045(8) 0.0227(4) Uani 1 1 d . . . H37 H -0.1123 0.1433 0.4355 0.027 Uiso 1 1 calc R . . C38 C 0.10974(16) 0.13487(10) 0.42647(8) 0.0252(4) Uani 1 1 d . . . H38A H 0.1388 0.0916 0.4057 0.030 Uiso 1 1 calc R . . H38B H 0.0685 0.1599 0.3967 0.030 Uiso 1 1 calc R . . C39 C 0.04444(14) 0.03571(8) 0.62623(7) 0.0180(3) Uani 1 1 d . . . C40 C 0.45647(15) 0.27852(10) 0.55184(8) 0.0228(4) Uani 1 1 d . . . H40A H 0.4742 0.3281 0.5429 0.027 Uiso 1 1 calc R . . H40B H 0.5233 0.2509 0.5443 0.027 Uiso 1 1 calc R . . C41 C 0.42682(14) 0.27757(9) 0.61739(7) 0.0190(3) Uani 1 1 d . . . C42 C 0.38973(14) 0.21364(9) 0.63973(7) 0.0182(3) Uani 1 1 d . . . H42 H 0.3899 0.1702 0.6151 0.022 Uiso 1 1 calc R . . C43 C 0.35228(13) 0.21414(9) 0.69872(7) 0.0170(3) Uani 1 1 d . . . C44 C 0.35118(14) 0.27857(9) 0.73499(7) 0.0178(3) Uani 1 1 d . . . H44 H 0.3225 0.2790 0.7741 0.021 Uiso 1 1 calc R . . C45 C 0.39216(14) 0.34219(9) 0.71377(7) 0.0185(3) Uani 1 1 d . . . C46 C 0.43088(14) 0.34081(9) 0.65498(8) 0.0197(3) Uani 1 1 d . . . H46 H 0.4603 0.3834 0.6405 0.024 Uiso 1 1 calc R . . C47 C 0.38887(15) 0.41234(9) 0.75284(8) 0.0228(4) Uani 1 1 d . . . H47A H 0.4451 0.4129 0.7856 0.027 Uiso 1 1 calc R . . H47B H 0.4081 0.4523 0.7285 0.027 Uiso 1 1 calc R . . C48 C 0.30926(13) 0.14568(9) 0.72276(7) 0.0168(3) Uani 1 1 d . . . C49 C 0.25766(15) -0.42856(9) 0.87592(8) 0.0223(4) Uani 1 1 d . . . H49A H 0.2352 -0.4716 0.8496 0.027 Uiso 1 1 calc R . . H49B H 0.2903 -0.4442 0.9131 0.027 Uiso 1 1 calc R . . C50 C 0.15381(15) -0.38684(9) 0.89140(8) 0.0211(3) Uani 1 1 d . . . C51 C 0.07171(15) -0.38372(9) 0.84582(8) 0.0231(4) Uani 1 1 d . . . H51 H 0.0809 -0.4098 0.8084 0.028 Uiso 1 1 calc R . . C52 C -0.02247(15) -0.34357(9) 0.85387(8) 0.0228(4) Uani 1 1 d . . . C53 C -0.04028(15) -0.30814(9) 0.91080(8) 0.0223(4) Uani 1 1 d . . . C54 C 0.03831(15) -0.31296(9) 0.95654(8) 0.0224(4) Uani 1 1 d . . . H54 H 0.0254 -0.2904 0.9950 0.027 Uiso 1 1 calc R . . C55 C 0.13688(15) -0.35043(9) 0.94753(8) 0.0205(3) Uani 1 1 d . . . C56 C 0.22240(15) -0.34615(9) 0.99952(8) 0.0219(3) Uani 1 1 d . . . H56A H 0.1827 -0.3459 1.0377 0.026 Uiso 1 1 calc R . . H56B H 0.2669 -0.3890 0.9959 0.026 Uiso 1 1 calc R . . C57 C 0.30072(14) -0.27960(9) 1.00103(7) 0.0190(3) Uani 1 1 d . . . C58 C 0.26231(14) -0.21513(9) 1.02892(7) 0.0198(3) Uani 1 1 d . . . H58 H 0.1921 -0.2158 1.0473 0.024 Uiso 1 1 calc R . . C59 C 0.32490(14) -0.15084(9) 1.03010(7) 0.0186(3) Uani 1 1 d . . . C60 C 0.43268(14) -0.15049(9) 1.00575(7) 0.0178(3) Uani 1 1 d . . . C61 C 0.47207(14) -0.21420(9) 0.97987(7) 0.0183(3) Uani 1 1 d . . . H61 H 0.5450 -0.2142 0.9646 0.022 Uiso 1 1 calc R . . C62 C 0.40654(14) -0.27894(9) 0.97566(7) 0.0187(3) Uani 1 1 d . . . C63 C 0.45678(15) -0.34427(9) 0.94277(8) 0.0206(3) Uani 1 1 d . . . H63A H 0.5376 -0.3429 0.9517 0.025 Uiso 1 1 calc R . . H63B H 0.4234 -0.3879 0.9579 0.025 Uiso 1 1 calc R . . C64 C 0.43759(15) -0.34765(9) 0.87485(8) 0.0199(3) Uani 1 1 d . . . C65 C 0.51396(15) -0.30809(9) 0.84170(8) 0.0208(3) Uani 1 1 d . . . H65 H 0.5771 -0.2847 0.8619 0.025 Uiso 1 1 calc R . . C66 C 0.49933(15) -0.30240(9) 0.78037(8) 0.0204(3) Uani 1 1 d . . . C67 C 0.40730(15) -0.33969(9) 0.75002(8) 0.0214(3) Uani 1 1 d . . . C68 C 0.33507(15) -0.38170(9) 0.78195(8) 0.0220(3) Uani 1 1 d . . . H68 H 0.2763 -0.4089 0.7610 0.026 Uiso 1 1 calc R . . C70 C 0.34682(15) -0.38504(9) 0.84463(8) 0.0208(3) Uani 1 1 d . . . C71 C 0.29960(16) -0.36151(9) 0.65694(8) 0.0238(4) Uani 1 1 d . . . H71A H 0.2894 -0.4124 0.6639 0.029 Uiso 1 1 calc R . . H71B H 0.3095 -0.3584 0.6136 0.029 Uiso 1 1 calc R . . C72 C 0.19538(16) -0.32325(9) 0.67602(8) 0.0217(3) Uani 1 1 d . . . C73 C 0.19359(15) -0.24876(9) 0.67567(7) 0.0207(3) Uani 1 1 d . . . H73 H 0.2543 -0.2230 0.6601 0.025 Uiso 1 1 calc R . . C74 C 0.10208(15) -0.21238(9) 0.69837(7) 0.0198(3) Uani 1 1 d . . . C75 C 0.01200(15) -0.25010(9) 0.72185(8) 0.0216(3) Uani 1 1 d . . . H75 H -0.0487 -0.2252 0.7380 0.026 Uiso 1 1 calc R . . C76 C 0.01186(15) -0.32456(9) 0.72141(8) 0.0219(4) Uani 1 1 d . . . C77 C 0.10308(16) -0.36054(9) 0.69789(8) 0.0237(4) Uani 1 1 d . . . H77 H 0.1024 -0.4109 0.6967 0.028 Uiso 1 1 calc R . . C78 C -0.08392(16) -0.36449(10) 0.74992(8) 0.0261(4) Uani 1 1 d . . . H78A H -0.1522 -0.3619 0.7252 0.031 Uiso 1 1 calc R . . H78B H -0.0667 -0.4152 0.7502 0.031 Uiso 1 1 calc R . . C79 C 0.10287(15) -0.13160(9) 0.70133(7) 0.0193(3) Uani 1 1 d . . . C80 C -0.14839(14) -0.22425(9) 0.97049(8) 0.0213(3) Uani 1 1 d . . . H80A H -0.1357 -0.2506 1.0061 0.026 Uiso 1 1 calc R . . H80B H -0.2246 -0.2070 0.9722 0.026 Uiso 1 1 calc R . . C81 C -0.06536(14) -0.16073(9) 0.97195(8) 0.0190(3) Uani 1 1 d . . . C82 C -0.05370(14) -0.12095(9) 0.92197(7) 0.0188(3) Uani 1 1 d . . . H82 H -0.1028 -0.1303 0.8884 0.023 Uiso 1 1 calc R . . C83 C 0.03110(14) -0.06723(9) 0.92195(7) 0.0181(3) Uani 1 1 d . . . C84 C 0.10556(14) -0.05415(9) 0.97094(7) 0.0188(3) Uani 1 1 d . . . H84 H 0.1642 -0.0190 0.9700 0.023 Uiso 1 1 calc R . . C85 C 0.09341(14) -0.09299(9) 1.02127(7) 0.0185(3) Uani 1 1 d . . . C86 C 0.00627(14) -0.14481(9) 1.02177(7) 0.0200(3) Uani 1 1 d . . . H86 H -0.0044 -0.1696 1.0565 0.024 Uiso 1 1 calc R . . C87 C 0.17671(15) -0.08066(10) 1.07341(8) 0.0220(3) Uani 1 1 d . . . H87A H 0.1672 -0.0330 1.0939 0.026 Uiso 1 1 calc R . . H87B H 0.1609 -0.1163 1.1024 0.026 Uiso 1 1 calc R . . C88 C 0.04700(14) -0.02459(9) 0.86822(7) 0.0190(3) Uani 1 1 d . . . C89 C 0.59419(14) -0.07821(9) 0.97840(7) 0.0184(3) Uani 1 1 d . . . H89A H 0.6462 -0.1140 0.9900 0.022 Uiso 1 1 calc R . . H89B H 0.6298 -0.0305 0.9889 0.022 Uiso 1 1 calc R . . C90 C 0.57160(13) -0.08831(9) 0.91120(7) 0.0171(3) Uani 1 1 d . . . C91 C 0.48888(14) -0.04938(9) 0.88557(7) 0.0170(3) Uani 1 1 d . . . H91 H 0.4527 -0.0139 0.9094 0.020 Uiso 1 1 calc R . . C92 C 0.45978(13) -0.06293(9) 0.82475(7) 0.0163(3) Uani 1 1 d . . . C93 C 0.51264(14) -0.11609(9) 0.78936(7) 0.0178(3) Uani 1 1 d . . . H93 H 0.4909 -0.1262 0.7486 0.021 Uiso 1 1 calc R . . C94 C 0.59706(14) -0.15421(9) 0.81398(7) 0.0176(3) Uani 1 1 d . . . C95 C 0.62636(13) -0.13912(9) 0.87463(7) 0.0181(3) Uani 1 1 d . . . H95 H 0.6846 -0.1638 0.8914 0.022 Uiso 1 1 calc R . . C96 C 0.65193(14) -0.21361(9) 0.77649(8) 0.0209(3) Uani 1 1 d . . . H96A H 0.6997 -0.1925 0.7467 0.025 Uiso 1 1 calc R . . H96B H 0.6998 -0.2394 0.8028 0.025 Uiso 1 1 calc R . . C97 C 0.37026(13) -0.02096(9) 0.79758(7) 0.0164(3) Uani 1 1 d . . . C98 C 0.41878(16) -0.09141(10) 0.62469(8) 0.0246(4) Uani 1 1 d . . . H98 H 0.3872 -0.1183 0.6546 0.030 Uiso 1 1 calc R . . C99 C 0.5635(3) -0.17810(16) 0.61926(11) 0.0591(8) Uani 1 1 d . . . H99A H 0.6354 -0.1634 0.6386 0.089 Uiso 1 1 calc R . . H99B H 0.5748 -0.2124 0.5850 0.089 Uiso 1 1 calc R . . H99C H 0.5156 -0.2002 0.6479 0.089 Uiso 1 1 calc R . . C100 C 0.5666(2) -0.07745(14) 0.55228(10) 0.0413(5) Uani 1 1 d . . . H10A H 0.5285 -0.0337 0.5467 0.062 Uiso 1 1 calc R . . H10B H 0.5644 -0.1077 0.5146 0.062 Uiso 1 1 calc R . . H10C H 0.6440 -0.0655 0.5647 0.062 Uiso 1 1 calc R . . C101 C 0.36399(17) 0.19075(11) 0.89157(8) 0.0290(4) Uani 1 1 d . . . H101 H 0.4186 0.1574 0.8815 0.035 Uiso 1 1 calc R . . C102 C 0.5074(2) 0.28354(14) 0.87693(10) 0.0429(6) Uani 1 1 d . . . H10D H 0.5535 0.2422 0.8720 0.064 Uiso 1 1 calc R . . H10E H 0.5382 0.3167 0.9096 0.064 Uiso 1 1 calc R . . H10F H 0.5061 0.3074 0.8398 0.064 Uiso 1 1 calc R . . C103 C 0.3148(3) 0.31547(13) 0.90561(11) 0.0490(6) Uani 1 1 d . . . H10G H 0.2409 0.2931 0.9099 0.074 Uiso 1 1 calc R . . H10H H 0.3126 0.3475 0.8735 0.074 Uiso 1 1 calc R . . H10I H 0.3380 0.3426 0.9432 0.074 Uiso 1 1 calc R . . C104 C -0.26723(16) 0.00088(11) 0.76608(9) 0.0299(4) Uani 1 1 d . . . H104 H -0.2537 -0.0013 0.8077 0.036 Uiso 1 1 calc R . . C105 C -0.3718(2) 0.05285(13) 0.68719(10) 0.0411(5) Uani 1 1 d . . . H10J H -0.3294 0.0197 0.6618 0.062 Uiso 1 1 calc R . . H10K H -0.3531 0.1017 0.6779 0.062 Uiso 1 1 calc R . . H10L H -0.4513 0.0422 0.6799 0.062 Uiso 1 1 calc R . . C106 C -0.39954(18) 0.09144(12) 0.79522(11) 0.0375(5) Uani 1 1 d . . . H10M H -0.3882 0.0739 0.8346 0.056 Uiso 1 1 calc R . . H10N H -0.4792 0.0908 0.7856 0.056 Uiso 1 1 calc R . . H10O H -0.3681 0.1402 0.7956 0.056 Uiso 1 1 calc R . . N4 N 0.6736(2) 0.52376(11) 0.90088(12) 0.0551(6) Uani 1 1 d . . . C108 C 0.7418(4) 0.5512(2) 0.9507(2) 0.0910(12) Uani 1 1 d . A . H10P H 0.8093 0.5244 0.9520 0.136 Uiso 1 1 calc R . . H10Q H 0.7011 0.5468 0.9876 0.136 Uiso 1 1 calc R . . H10R H 0.7619 0.6014 0.9468 0.136 Uiso 1 1 calc R . . C109 C 0.7013(4) 0.5396(2) 0.8443(2) 0.0984(14) Uani 0.50 1 d P A 1 H109 H 0.7340 0.5857 0.8410 0.118 Uiso 0.50 1 calc PR A 1 C107 C 0.5782(4) 0.4847(3) 0.9108(2) 0.1092(17) Uani 0.50 1 d P A 1 H10S H 0.5186 0.4978 0.8842 0.164 Uiso 0.50 1 calc PR A 1 H10T H 0.5569 0.4943 0.9524 0.164 Uiso 0.50 1 calc PR A 1 H10U H 0.5911 0.4339 0.9029 0.164 Uiso 0.50 1 calc PR A 1 O28 O 0.6885(7) 0.4999(4) 0.7954(3) 0.135(3) Uani 0.50 1 d P A 1 O28A O 0.5384(4) 0.4777(2) 0.9642(2) 0.0828(15) Uani 0.50 1 d P A 2 N203 N 0.6222(3) 0.56448(13) 0.62427(13) 0.0731(8) Uani 1 1 d . . . C111 C 0.6189(3) 0.54186(16) 0.68200(14) 0.0591(7) Uani 0.50 1 d P B 2 H11A H 0.5506 0.5128 0.6862 0.089 Uiso 0.50 1 calc PR B 2 H11B H 0.6204 0.5834 0.7113 0.089 Uiso 0.50 1 calc PR B 2 H11C H 0.6833 0.5136 0.6889 0.089 Uiso 0.50 1 calc PR B 2 O29 O 0.6184(3) 0.48303(17) 0.69989(18) 0.0528(9) Uani 0.50 1 d P B 1 C110 C 0.6563(4) 0.63539(18) 0.61614(15) 0.0824(12) Uani 1 1 d . B . H11D H 0.6502 0.6648 0.6539 0.124 Uiso 1 1 calc R . . H11E H 0.6088 0.6535 0.5855 0.124 Uiso 1 1 calc R . . H11F H 0.7335 0.6371 0.6034 0.124 Uiso 1 1 calc R . . C113 C 0.6359(5) 0.5091(3) 0.5753(3) 0.0557(14) Uani 0.50 1 d P B 1 H11G H 0.6507 0.4640 0.5919 0.084 Uiso 0.50 1 calc PR B 1 H11H H 0.6983 0.5231 0.5508 0.084 Uiso 0.50 1 calc PR B 1 H11I H 0.5679 0.5033 0.5504 0.084 Uiso 0.50 1 calc PR B 1 O29A O 0.4503(5) 0.4933(3) 0.5876(3) 0.0916(17) Uani 0.50 1 d P B 2 C112 C 0.5240(11) 0.5441(4) 0.5830(4) 0.123(4) Uani 0.50 1 d P B 2 H112 H 0.5153 0.5718 0.5499 0.148 Uiso 0.50 1 calc PR B 2 C19A C 0.7013(4) 0.5396(2) 0.8443(2) 0.0984(14) Uani 0.50 1 d P A 2 H19A H 0.7419 0.5858 0.8464 0.148 Uiso 0.50 1 calc PR A 2 H19B H 0.6335 0.5413 0.8198 0.148 Uiso 0.50 1 calc PR A 2 H19C H 0.7481 0.5028 0.8264 0.148 Uiso 0.50 1 calc PR A 2 C17A C 0.5782(4) 0.4847(3) 0.9108(2) 0.1092(17) Uani 0.50 1 d P A 2 H17A H 0.5387 0.4613 0.8772 0.131 Uiso 0.50 1 calc PR A 2 C11A C 0.6189(3) 0.54186(16) 0.68200(14) 0.0591(7) Uani 0.50 1 d P B 1 H11J H 0.6166 0.5794 0.7127 0.071 Uiso 0.50 1 calc PR B 1 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 0.01541(10) 0.01477(10) 0.01767(10) 0.00540(7) 0.00146(7) 0.00302(7) Cu2 0.02303(11) 0.01238(10) 0.01521(10) 0.00282(7) 0.00045(8) 0.00350(8) Cu3 0.01862(10) 0.01256(9) 0.01489(9) 0.00233(7) -0.00429(7) 0.00167(7) O1 0.0263(7) 0.0211(6) 0.0236(6) -0.0032(5) -0.0027(5) 0.0017(5) O2 0.0289(7) 0.0225(6) 0.0285(7) -0.0024(5) 0.0008(5) -0.0045(5) O3 0.0185(6) 0.0268(7) 0.0418(8) 0.0034(6) -0.0037(6) -0.0007(5) O4 0.0193(6) 0.0225(7) 0.0443(8) 0.0006(6) -0.0036(6) -0.0008(5) O5 0.0270(7) 0.0266(7) 0.0216(6) -0.0018(5) 0.0003(5) -0.0037(5) O6 0.0245(6) 0.0299(7) 0.0181(6) -0.0006(5) -0.0003(5) 0.0007(5) O7 0.0209(6) 0.0241(6) 0.0270(6) 0.0008(5) -0.0015(5) 0.0054(5) O8 0.0334(7) 0.0156(6) 0.0299(7) -0.0001(5) -0.0074(6) 0.0055(5) O9 0.0284(7) 0.0265(7) 0.0193(6) 0.0057(5) -0.0008(5) 0.0029(5) O10 0.0259(7) 0.0309(7) 0.0326(7) 0.0157(6) -0.0096(6) -0.0009(5) O11 0.0249(6) 0.0180(6) 0.0247(6) 0.0007(5) 0.0019(5) -0.0010(5) O12 0.0345(7) 0.0208(6) 0.0253(6) 0.0076(5) 0.0089(6) 0.0035(5) O13 0.0240(6) 0.0283(7) 0.0261(7) 0.0027(5) -0.0018(5) -0.0010(5) O14 0.0196(6) 0.0246(6) 0.0286(7) 0.0018(5) 0.0003(5) 0.0005(5) O15 0.0207(6) 0.0201(6) 0.0222(6) -0.0036(5) 0.0006(5) 0.0034(5) O16 0.0207(6) 0.0188(6) 0.0184(6) -0.0019(5) -0.0001(5) 0.0009(5) O17 0.0277(7) 0.0219(6) 0.0186(6) -0.0010(5) 0.0050(5) 0.0007(5) O18 0.0296(7) 0.0262(7) 0.0178(6) -0.0006(5) 0.0021(5) 0.0017(5) O19 0.0286(7) 0.0165(6) 0.0231(6) 0.0009(5) -0.0008(5) -0.0007(5) O20 0.0433(8) 0.0172(6) 0.0320(7) 0.0059(5) 0.0114(6) 0.0084(6) O21 0.0272(7) 0.0246(6) 0.0191(6) 0.0055(5) 0.0015(5) 0.0015(5) O22 0.0228(7) 0.0358(8) 0.0421(8) 0.0239(6) 0.0020(6) -0.0004(6) O23 0.0196(6) 0.0218(6) 0.0205(6) 0.0005(5) -0.0013(5) 0.0068(5) O24 0.0338(7) 0.0225(6) 0.0209(6) 0.0000(5) -0.0114(5) 0.0086(5) O25 0.0310(7) 0.0260(7) 0.0266(7) 0.0007(5) 0.0024(6) 0.0058(6) O26 0.0325(8) 0.0355(8) 0.0244(7) -0.0011(6) -0.0002(6) -0.0001(6) O27 0.0286(7) 0.0337(8) 0.0389(8) -0.0020(6) -0.0002(6) -0.0010(6) N1 0.0375(9) 0.0373(9) 0.0208(8) 0.0038(7) 0.0056(7) 0.0143(8) N2 0.0378(9) 0.0338(9) 0.0217(8) 0.0043(7) -0.0045(7) 0.0003(7) N3 0.0218(8) 0.0304(9) 0.0375(9) 0.0068(7) -0.0012(7) -0.0042(7) C1 0.0327(10) 0.0169(8) 0.0326(10) 0.0094(7) -0.0067(8) -0.0015(7) C2 0.0309(10) 0.0096(7) 0.0317(9) 0.0026(7) -0.0049(8) -0.0001(7) C3 0.0261(9) 0.0114(8) 0.0302(9) 0.0007(7) -0.0022(7) -0.0008(6) C4 0.0271(9) 0.0113(8) 0.0283(9) -0.0025(6) -0.0044(7) 0.0004(6) C5 0.0310(10) 0.0118(8) 0.0292(9) -0.0018(7) -0.0010(8) -0.0009(7) C6 0.0269(9) 0.0127(8) 0.0384(10) -0.0002(7) -0.0005(8) 0.0001(7) C7 0.0298(10) 0.0090(7) 0.0378(10) 0.0022(7) -0.0062(8) 0.0010(7) C8 0.0294(10) 0.0171(9) 0.0442(11) 0.0065(8) -0.0069(9) 0.0043(7) C9 0.0231(9) 0.0181(9) 0.0420(11) 0.0074(8) -0.0108(8) 0.0051(7) C10 0.0222(9) 0.0213(9) 0.0405(11) 0.0038(8) -0.0069(8) 0.0057(7) C11 0.0154(8) 0.0246(9) 0.0414(11) 0.0072(8) -0.0059(7) 0.0043(7) C12 0.0172(8) 0.0207(9) 0.0434(11) 0.0043(8) -0.0100(8) 0.0026(7) C13 0.0227(9) 0.0225(9) 0.0374(10) 0.0059(8) -0.0097(8) 0.0038(7) C14 0.0230(9) 0.0209(9) 0.0389(11) 0.0099(8) -0.0104(8) 0.0048(7) C15 0.0332(10) 0.0212(9) 0.0333(10) 0.0109(8) -0.0124(8) 0.0016(8) C16 0.0289(9) 0.0226(9) 0.0239(9) 0.0117(7) -0.0057(7) -0.0010(7) C17 0.0295(9) 0.0240(9) 0.0216(8) 0.0078(7) -0.0057(7) -0.0050(7) C18 0.0294(9) 0.0233(9) 0.0149(8) 0.0043(6) -0.0002(7) -0.0032(7) C19 0.0238(9) 0.0264(9) 0.0164(8) 0.0067(7) -0.0003(7) -0.0016(7) C20 0.0262(9) 0.0225(9) 0.0197(8) 0.0064(7) -0.0034(7) -0.0045(7) C21 0.0326(10) 0.0185(8) 0.0226(8) 0.0094(7) -0.0034(7) -0.0025(7) C22 0.0296(10) 0.0188(9) 0.0342(10) -0.0051(7) 0.0044(8) 0.0015(7) C23 0.0232(9) 0.0177(8) 0.0290(9) -0.0027(7) 0.0049(7) 0.0011(7) C24 0.0186(8) 0.0192(8) 0.0243(8) 0.0010(7) 0.0018(7) 0.0016(6) C25 0.0175(8) 0.0161(8) 0.0230(8) 0.0023(6) 0.0038(6) 0.0024(6) C26 0.0166(8) 0.0166(8) 0.0288(9) 0.0018(7) 0.0017(7) 0.0001(6) C27 0.0154(8) 0.0221(9) 0.0336(10) 0.0026(7) 0.0019(7) 0.0031(7) C28 0.0217(9) 0.0183(8) 0.0395(11) 0.0005(7) 0.0051(8) 0.0077(7) C29 0.0160(8) 0.0268(10) 0.0450(12) 0.0040(8) 0.0012(8) 0.0052(7) C30 0.0185(8) 0.0158(8) 0.0200(8) 0.0047(6) 0.0034(6) 0.0022(6) C31 0.0221(9) 0.0237(9) 0.0345(10) 0.0034(8) -0.0112(8) -0.0007(7) C32 0.0219(8) 0.0181(8) 0.0230(8) 0.0009(6) -0.0090(7) -0.0004(6) C33 0.0224(8) 0.0167(8) 0.0200(8) 0.0026(6) -0.0035(6) 0.0000(6) C34 0.0233(8) 0.0133(7) 0.0165(7) 0.0012(6) -0.0045(6) 0.0013(6) C35 0.0213(8) 0.0173(8) 0.0184(8) 0.0008(6) -0.0040(6) 0.0013(6) C36 0.0273(9) 0.0176(8) 0.0160(8) -0.0006(6) -0.0042(7) -0.0019(7) C37 0.0299(9) 0.0202(8) 0.0176(8) 0.0028(6) -0.0104(7) -0.0002(7) C38 0.0313(10) 0.0271(9) 0.0163(8) 0.0000(7) -0.0032(7) -0.0043(8) C39 0.0240(8) 0.0122(7) 0.0176(8) 0.0008(6) -0.0052(6) 0.0016(6) C40 0.0211(8) 0.0282(9) 0.0192(8) 0.0044(7) 0.0021(7) -0.0028(7) C41 0.0162(8) 0.0238(9) 0.0174(8) 0.0041(6) -0.0006(6) -0.0004(6) C42 0.0176(8) 0.0187(8) 0.0181(8) 0.0009(6) -0.0014(6) 0.0005(6) C43 0.0153(7) 0.0171(8) 0.0189(8) 0.0038(6) -0.0016(6) 0.0015(6) C44 0.0178(8) 0.0196(8) 0.0160(7) 0.0024(6) -0.0024(6) 0.0008(6) C45 0.0169(8) 0.0184(8) 0.0200(8) 0.0013(6) -0.0044(6) -0.0001(6) C46 0.0181(8) 0.0183(8) 0.0227(8) 0.0057(6) -0.0022(6) -0.0036(6) C47 0.0235(9) 0.0198(8) 0.0241(9) -0.0006(7) -0.0042(7) -0.0039(7) C48 0.0155(7) 0.0175(8) 0.0177(7) 0.0041(6) -0.0028(6) 0.0021(6) C49 0.0282(9) 0.0136(8) 0.0253(9) 0.0014(6) 0.0014(7) 0.0019(7) C50 0.0235(9) 0.0138(8) 0.0262(9) 0.0041(6) 0.0030(7) -0.0013(6) C51 0.0282(9) 0.0170(8) 0.0238(9) 0.0014(7) 0.0009(7) -0.0028(7) C52 0.0232(9) 0.0189(8) 0.0261(9) 0.0044(7) -0.0013(7) -0.0049(7) C53 0.0204(8) 0.0174(8) 0.0294(9) 0.0052(7) 0.0031(7) -0.0022(7) C54 0.0242(9) 0.0184(8) 0.0246(9) 0.0037(7) 0.0034(7) -0.0019(7) C55 0.0225(8) 0.0152(8) 0.0242(8) 0.0052(6) 0.0014(7) -0.0021(6) C56 0.0267(9) 0.0183(8) 0.0217(8) 0.0051(6) 0.0022(7) 0.0031(7) C57 0.0231(8) 0.0181(8) 0.0165(8) 0.0044(6) -0.0019(6) 0.0032(7) C58 0.0196(8) 0.0231(9) 0.0173(8) 0.0032(6) 0.0008(6) 0.0042(7) C59 0.0227(8) 0.0190(8) 0.0142(7) -0.0002(6) -0.0022(6) 0.0054(6) C60 0.0204(8) 0.0188(8) 0.0141(7) 0.0020(6) -0.0039(6) 0.0010(6) C61 0.0188(8) 0.0215(8) 0.0150(7) 0.0027(6) -0.0007(6) 0.0045(6) C62 0.0233(8) 0.0176(8) 0.0158(7) 0.0039(6) -0.0021(6) 0.0050(6) C63 0.0239(9) 0.0173(8) 0.0213(8) 0.0041(6) 0.0003(7) 0.0058(7) C64 0.0249(9) 0.0140(8) 0.0215(8) 0.0014(6) 0.0021(7) 0.0075(6) C65 0.0243(9) 0.0161(8) 0.0222(8) 0.0002(6) 0.0012(7) 0.0042(7) C66 0.0239(8) 0.0148(8) 0.0228(8) 0.0004(6) 0.0052(7) 0.0055(6) C67 0.0287(9) 0.0177(8) 0.0181(8) -0.0014(6) 0.0026(7) 0.0084(7) C68 0.0264(9) 0.0159(8) 0.0235(9) -0.0019(6) 0.0002(7) 0.0039(7) C70 0.0255(9) 0.0134(8) 0.0238(8) 0.0010(6) 0.0028(7) 0.0064(7) C71 0.0330(10) 0.0179(8) 0.0199(8) -0.0041(6) 0.0005(7) 0.0046(7) C72 0.0313(9) 0.0156(8) 0.0174(8) -0.0030(6) -0.0026(7) 0.0029(7) C73 0.0282(9) 0.0165(8) 0.0169(8) 0.0000(6) -0.0011(7) 0.0000(7) C74 0.0287(9) 0.0141(8) 0.0162(8) 0.0001(6) -0.0037(7) 0.0015(7) C75 0.0253(9) 0.0182(8) 0.0212(8) 0.0002(6) -0.0025(7) 0.0029(7) C76 0.0263(9) 0.0185(8) 0.0202(8) 0.0005(6) -0.0045(7) -0.0030(7) C77 0.0337(10) 0.0130(8) 0.0235(9) -0.0022(6) -0.0041(7) 0.0004(7) C78 0.0283(9) 0.0215(9) 0.0274(9) 0.0011(7) -0.0040(7) -0.0050(7) C79 0.0282(9) 0.0154(8) 0.0143(7) 0.0011(6) -0.0056(6) 0.0040(7) C80 0.0193(8) 0.0224(9) 0.0233(8) 0.0065(7) 0.0037(7) 0.0027(7) C81 0.0180(8) 0.0201(8) 0.0196(8) 0.0040(6) 0.0049(6) 0.0032(6) C82 0.0186(8) 0.0209(8) 0.0176(8) 0.0037(6) 0.0014(6) 0.0035(6) C83 0.0197(8) 0.0171(8) 0.0184(8) 0.0036(6) 0.0043(6) 0.0050(6) C84 0.0187(8) 0.0172(8) 0.0208(8) 0.0015(6) 0.0027(6) 0.0026(6) C85 0.0201(8) 0.0196(8) 0.0160(7) -0.0003(6) 0.0025(6) 0.0060(6) C86 0.0227(8) 0.0218(8) 0.0166(8) 0.0050(6) 0.0052(6) 0.0059(7) C87 0.0229(9) 0.0251(9) 0.0179(8) -0.0022(7) 0.0019(7) 0.0063(7) C88 0.0215(8) 0.0166(8) 0.0200(8) 0.0048(6) 0.0052(6) 0.0055(6) C89 0.0171(8) 0.0204(8) 0.0177(8) 0.0009(6) -0.0030(6) 0.0014(6) C90 0.0163(8) 0.0178(8) 0.0172(7) 0.0022(6) -0.0024(6) -0.0005(6) C91 0.0179(8) 0.0156(8) 0.0174(8) 0.0003(6) -0.0016(6) 0.0020(6) C92 0.0161(7) 0.0156(8) 0.0173(7) 0.0022(6) -0.0018(6) 0.0009(6) C93 0.0202(8) 0.0186(8) 0.0146(7) 0.0017(6) -0.0008(6) 0.0013(6) C94 0.0162(8) 0.0174(8) 0.0192(8) 0.0018(6) 0.0017(6) 0.0011(6) C95 0.0151(7) 0.0198(8) 0.0199(8) 0.0042(6) -0.0021(6) 0.0031(6) C96 0.0198(8) 0.0218(8) 0.0213(8) 0.0010(7) 0.0031(7) 0.0045(7) C97 0.0165(8) 0.0160(8) 0.0172(7) 0.0050(6) -0.0008(6) 0.0000(6) C98 0.0294(9) 0.0262(9) 0.0175(8) -0.0015(7) 0.0003(7) 0.0009(7) C99 0.082(2) 0.0695(18) 0.0343(12) 0.0219(12) 0.0255(13) 0.0516(16) C100 0.0412(12) 0.0529(14) 0.0328(11) 0.0118(10) 0.0113(9) 0.0140(11) C101 0.0346(11) 0.0316(10) 0.0204(9) 0.0003(7) -0.0072(8) 0.0044(8) C102 0.0417(13) 0.0520(14) 0.0352(12) 0.0146(10) -0.0132(10) -0.0102(11) C103 0.0762(19) 0.0365(13) 0.0362(12) 0.0047(10) 0.0178(12) 0.0126(12) C104 0.0259(9) 0.0296(10) 0.0335(10) 0.0036(8) -0.0019(8) -0.0054(8) C105 0.0388(12) 0.0436(13) 0.0406(12) 0.0062(10) -0.0101(10) -0.0033(10) C106 0.0273(10) 0.0327(11) 0.0526(13) 0.0046(10) 0.0096(9) -0.0028(8) N4 0.0601(14) 0.0328(11) 0.0735(16) 0.0130(10) 0.0010(12) -0.0031(10) C108 0.089(3) 0.061(2) 0.117(3) -0.014(2) -0.016(2) -0.0123(19) C109 0.137(4) 0.070(2) 0.093(3) 0.022(2) 0.047(3) 0.012(2) C107 0.102(3) 0.122(4) 0.105(3) 0.058(3) -0.029(3) -0.056(3) O28 0.191(8) 0.105(5) 0.123(6) 0.050(4) 0.066(5) 0.078(5) O28A 0.099(4) 0.056(3) 0.102(4) 0.047(3) 0.038(3) 0.012(2) N203 0.113(2) 0.0422(13) 0.0643(16) 0.0056(12) 0.0317(16) -0.0093(14) C111 0.0650(18) 0.0516(16) 0.0639(18) 0.0135(14) 0.0272(15) 0.0107(14) O29 0.068(2) 0.0260(16) 0.066(2) 0.0123(15) 0.0220(19) -0.0047(16) C110 0.137(3) 0.061(2) 0.0482(17) 0.0036(14) 0.027(2) -0.020(2) C113 0.050(3) 0.050(3) 0.066(4) 0.001(3) -0.022(3) 0.008(2) O29A 0.084(4) 0.059(3) 0.131(5) 0.024(3) -0.007(3) -0.023(3) C112 0.239(14) 0.049(4) 0.079(5) 0.011(4) -0.025(7) -0.021(6) C19A 0.137(4) 0.070(2) 0.093(3) 0.022(2) 0.047(3) 0.012(2) C17A 0.102(3) 0.122(4) 0.105(3) 0.058(3) -0.029(3) -0.056(3) C11A 0.0650(18) 0.0516(16) 0.0639(18) 0.0135(14) 0.0272(15) 0.0107(14) _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 O22 1.9231(13) . ? Cu1 O12 1.9398(13) . ? Cu1 O7 1.9742(12) . ? Cu1 O23 1.9750(12) . ? Cu1 O26 2.4191(14) . ? Cu2 O20 1.9339(13) . ? Cu2 O8 1.9518(12) . ? Cu2 O9 1.9640(12) . ? Cu2 O21 1.9905(12) . ? Cu2 O27 2.3748(15) . ? Cu3 O10 1.9214(12) . ? Cu3 O24 1.9478(12) . ? Cu3 O11 1.9741(12) . ? Cu3 O19 1.9870(12) . ? Cu3 O25 2.3115(14) . ? O1 C4 1.390(2) . ? O1 C47 1.450(2) . ? O2 C5 1.385(2) . ? O2 C22 1.452(2) . ? O3 C11 1.388(2) . ? O3 C29 1.443(3) . ? O4 C12 1.393(2) . ? O4 C31 1.456(2) . ? O5 C18 1.387(2) . ? O5 C38 1.457(2) . ? O6 C19 1.393(2) . ? O6 C40 1.450(2) . ? O7 C30 1.267(2) . ? O8 C30 1.267(2) . ? O9 C39 1.269(2) . ? O10 C39 1.270(2) . ? O11 C48 1.264(2) . ? O12 C48 1.276(2) . ? O13 C52 1.392(2) . ? O13 C78 1.452(2) . ? O14 C53 1.399(2) . ? O14 C80 1.454(2) . ? O15 C59 1.390(2) . ? O15 C87 1.459(2) . ? O16 C60 1.389(2) . ? O16 C89 1.460(2) . ? O17 C66 1.393(2) . ? O17 C96 1.458(2) . ? O18 C67 1.393(2) . ? O18 C71 1.452(2) . ? O19 C79 1.265(2) . ? O20 C79 1.271(2) . ? O21 C88 1.270(2) . ? O22 C88 1.268(2) . ? O23 C97 1.271(2) . ? O24 C97 1.271(2) . ? O25 C98 1.241(2) . ? O26 C101 1.243(3) . ? O27 C104 1.245(3) . ? N1 C98 1.346(3) . ? N1 C99 1.467(3) . ? N1 C100 1.475(3) . ? N2 C101 1.350(3) . ? N2 C102 1.463(3) . ? N2 C103 1.470(3) . ? N3 C104 1.345(3) . ? N3 C105 1.460(3) . ? N3 C106 1.474(3) . ? C1 C2 1.536(3) . ? C1 C21 1.540(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.401(3) . ? C2 C3 1.421(3) . ? C3 C4 1.396(3) . ? C3 H3 0.9500 . ? C4 C5 1.421(3) . ? C5 C6 1.400(3) . ? C6 C7 1.421(3) . ? C6 H6 0.9500 . ? C7 C8 1.539(3) . ? C8 C9 1.544(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.401(3) . ? C9 C10 1.416(3) . ? C10 C11 1.399(3) . ? C10 H10 0.9500 . ? C11 C12 1.416(3) . ? C12 C13 1.397(3) . ? C13 C14 1.428(3) . ? C13 H13 0.9500 . ? C14 C15 1.540(3) . ? C15 C16 1.538(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.408(3) . ? C16 C17 1.419(3) . ? C17 C18 1.398(3) . ? C17 H17 0.9500 . ? C18 C19 1.420(2) . ? C19 C20 1.396(3) . ? C20 C21 1.420(3) . ? C20 H20 0.9500 . ? C22 C23 1.530(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.407(3) . ? C23 C24 1.408(2) . ? C24 C25 1.407(2) . ? C24 H24 0.9500 . ? C25 C26 1.402(2) . ? C25 C30 1.522(2) . ? C26 C27 1.407(2) . ? C26 H26 0.9500 . ? C27 C28 1.404(3) . ? C27 C29 1.527(3) . ? C28 H28 0.9500 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C32 1.523(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C37 1.401(3) . ? C32 C33 1.406(2) . ? C33 C34 1.407(2) . ? C33 H33 0.9500 . ? C34 C35 1.408(2) . ? C34 C39 1.513(2) . ? C35 C36 1.407(2) . ? C35 H35 0.9500 . ? C36 C37 1.407(3) . ? C36 C38 1.526(3) . ? C37 H37 0.9500 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C40 C41 1.524(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.403(2) . ? C41 C42 1.405(2) . ? C42 C43 1.408(2) . ? C42 H42 0.9500 . ? C43 C44 1.409(2) . ? C43 C48 1.517(2) . ? C44 C45 1.403(2) . ? C44 H44 0.9500 . ? C45 C46 1.408(2) . ? C45 C47 1.530(2) . ? C46 H46 0.9500 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C49 C50 1.540(2) . ? C49 C70 1.541(2) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C55 1.408(3) . ? C50 C51 1.417(3) . ? C51 C52 1.401(3) . ? C51 H51 0.9500 . ? C52 C53 1.418(3) . ? C53 C54 1.396(3) . ? C54 C55 1.420(3) . ? C54 H54 0.9500 . ? C55 C56 1.538(2) . ? C56 C57 1.537(2) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C62 1.408(2) . ? C57 C58 1.424(2) . ? C58 C59 1.400(2) . ? C58 H58 0.9500 . ? C59 C60 1.421(2) . ? C60 C61 1.400(2) . ? C61 C62 1.422(2) . ? C61 H61 0.9500 . ? C62 C63 1.540(2) . ? C63 C64 1.534(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C70 1.408(3) . ? C64 C65 1.422(3) . ? C65 C66 1.399(2) . ? C65 H65 0.9500 . ? C66 C67 1.419(3) . ? C67 C68 1.401(3) . ? C68 C70 1.419(2) . ? C68 H68 0.9500 . ? C71 C72 1.529(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.410(2) . ? C72 C77 1.410(3) . ? C73 C74 1.408(3) . ? C73 H73 0.9500 . ? C74 C75 1.408(3) . ? C74 C79 1.522(2) . ? C75 C76 1.406(2) . ? C75 H75 0.9500 . ? C76 C77 1.408(3) . ? C76 C78 1.532(3) . ? C77 H77 0.9500 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C80 C81 1.526(2) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C86 1.405(2) . ? C81 C82 1.408(2) . ? C82 C83 1.409(2) . ? C82 H82 0.9500 . ? C83 C84 1.405(2) . ? C83 C88 1.517(2) . ? C84 C85 1.405(2) . ? C84 H84 0.9500 . ? C85 C86 1.405(2) . ? C85 C87 1.524(2) . ? C86 H86 0.9500 . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C89 C90 1.523(2) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 C95 1.407(2) . ? C90 C91 1.408(2) . ? C91 C92 1.404(2) . ? C91 H91 0.9500 . ? C92 C93 1.412(2) . ? C92 C97 1.516(2) . ? C93 C94 1.404(2) . ? C93 H93 0.9500 . ? C94 C95 1.404(2) . ? C94 C96 1.529(2) . ? C95 H95 0.9500 . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C98 H98 0.9500 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C101 H101 0.9500 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C103 H10G 0.9800 . ? C103 H10H 0.9800 . ? C103 H10I 0.9800 . ? C104 H104 0.9500 . ? C105 H10J 0.9800 . ? C105 H10K 0.9800 . ? C105 H10L 0.9800 . ? C106 H10M 0.9800 . ? C106 H10N 0.9800 . ? C106 H10O 0.9800 . ? N4 C107 1.372(4) . ? N4 C109 1.374(5) . ? N4 C108 1.424(4) . ? C108 H10P 0.9800 . ? C108 H10Q 0.9800 . ? C108 H10R 0.9800 . ? C109 O28 1.279(9) . ? C109 H109 0.9500 . ? C107 H10S 0.9800 . ? C107 H10T 0.9800 . ? C107 H10U 0.9800 . ? N203 C111 1.400(4) . ? N203 C110 1.412(4) . ? N203 C113 1.472(6) . ? N203 C112 1.506(11) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C110 H11D 0.9800 . ? C110 H11E 0.9800 . ? C110 H11F 0.9800 . ? C113 H11G 0.9800 . ? C113 H11H 0.9800 . ? C113 H11I 0.9800 . ? O29A C112 1.291(11) . ? C112 H112 0.9500 . ? 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 O22 Cu1 O12 171.23(6) . . ? O22 Cu1 O7 95.02(6) . . ? O12 Cu1 O7 85.83(6) . . ? O22 Cu1 O23 85.02(6) . . ? O12 Cu1 O23 95.55(5) . . ? O7 Cu1 O23 170.69(5) . . ? O22 Cu1 O26 101.73(6) . . ? O12 Cu1 O26 87.04(5) . . ? O7 Cu1 O26 82.70(5) . . ? O23 Cu1 O26 88.17(5) . . ? O20 Cu2 O8 172.15(6) . . ? O20 Cu2 O9 94.90(6) . . ? O8 Cu2 O9 86.27(6) . . ? O20 Cu2 O21 85.62(6) . . ? O8 Cu2 O21 94.10(5) . . ? O9 Cu2 O21 173.49(5) . . ? O20 Cu2 O27 96.84(6) . . ? O8 Cu2 O27 90.99(5) . . ? O9 Cu2 O27 84.76(5) . . ? O21 Cu2 O27 88.73(5) . . ? O10 Cu3 O24 171.32(6) . . ? O10 Cu3 O11 86.07(6) . . ? O24 Cu3 O11 94.50(5) . . ? O10 Cu3 O19 96.38(6) . . ? O24 Cu3 O19 84.03(5) . . ? O11 Cu3 O19 173.21(5) . . ? O10 Cu3 O25 96.40(6) . . ? O24 Cu3 O25 92.28(5) . . ? O11 Cu3 O25 85.80(5) . . ? O19 Cu3 O25 87.63(5) . . ? C4 O1 C47 116.80(14) . . ? C5 O2 C22 118.62(15) . . ? C11 O3 C29 117.12(15) . . ? C12 O4 C31 117.70(15) . . ? C18 O5 C38 117.76(14) . . ? C19 O6 C40 118.42(14) . . ? C30 O7 Cu1 128.03(11) . . ? C30 O8 Cu2 132.65(11) . . ? C39 O9 Cu2 131.02(11) . . ? C39 O10 Cu3 130.85(12) . . ? C48 O11 Cu3 128.77(11) . . ? C48 O12 Cu1 130.40(11) . . ? C52 O13 C78 117.51(14) . . ? C53 O14 C80 116.95(13) . . ? C59 O15 C87 118.08(13) . . ? C60 O16 C89 118.36(13) . . ? C66 O17 C96 117.85(13) . . ? C67 O18 C71 117.73(14) . . ? C79 O19 Cu3 129.82(11) . . ? C79 O20 Cu2 131.94(12) . . ? C88 O21 Cu2 125.82(11) . . ? C88 O22 Cu1 134.37(12) . . ? C97 O23 Cu1 129.00(11) . . ? C97 O24 Cu3 131.17(11) . . ? C98 O25 Cu3 111.54(12) . . ? C101 O26 Cu1 109.16(12) . . ? C104 O27 Cu2 110.45(12) . . ? C98 N1 C99 120.70(18) . . ? C98 N1 C100 121.18(17) . . ? C99 N1 C100 117.96(18) . . ? C101 N2 C102 121.49(19) . . ? C101 N2 C103 120.83(19) . . ? C102 N2 C103 117.7(2) . . ? C104 N3 C105 121.76(19) . . ? C104 N3 C106 120.65(18) . . ? C105 N3 C106 117.52(18) . . ? C2 C1 C21 113.03(14) . . ? C2 C1 H1A 109.0 . . ? C21 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? C21 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C7 C2 C3 119.05(17) . . ? C7 C2 C1 124.12(17) . . ? C3 C2 C1 116.83(17) . . ? C4 C3 C2 121.66(18) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? O1 C4 C3 124.64(17) . . ? O1 C4 C5 115.78(16) . . ? C3 C4 C5 119.57(17) . . ? O2 C5 C6 126.21(18) . . ? O2 C5 C4 115.16(16) . . ? C6 C5 C4 118.62(18) . . ? C5 C6 C7 122.02(18) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C2 C7 C6 119.01(17) . . ? C2 C7 C8 123.20(18) . . ? C6 C7 C8 117.77(18) . . ? C7 C8 C9 112.36(14) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? C14 C9 C10 119.12(18) . . ? C14 C9 C8 124.42(19) . . ? C10 C9 C8 116.42(18) . . ? C11 C10 C9 122.12(19) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? O3 C11 C10 124.86(19) . . ? O3 C11 C12 116.20(17) . . ? C10 C11 C12 118.92(19) . . ? O4 C12 C13 125.79(19) . . ? O4 C12 C11 114.95(18) . . ? C13 C12 C11 119.23(17) . . ? C12 C13 C14 121.81(19) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C9 C14 C13 118.66(19) . . ? C9 C14 C15 123.95(17) . . ? C13 C14 C15 117.35(18) . . ? C16 C15 C14 112.78(14) . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 118.67(17) . . ? C21 C16 C15 123.65(17) . . ? C17 C16 C15 117.63(16) . . ? C18 C17 C16 122.41(17) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? O5 C18 C17 125.70(16) . . ? O5 C18 C19 115.56(16) . . ? C17 C18 C19 118.71(17) . . ? O6 C19 C20 125.55(16) . . ? O6 C19 C18 115.20(16) . . ? C20 C19 C18 119.18(17) . . ? C19 C20 C21 122.12(17) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 118.77(17) . . ? C16 C21 C1 123.82(17) . . ? C20 C21 C1 117.38(16) . . ? O2 C22 C23 112.04(15) . . ? O2 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? O2 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C28 C23 C24 119.06(16) . . ? C28 C23 C22 120.54(16) . . ? C24 C23 C22 120.15(16) . . ? C25 C24 C23 119.87(16) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.30(15) . . ? C26 C25 C30 118.91(15) . . ? C24 C25 C30 120.72(15) . . ? C25 C26 C27 120.43(16) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 118.71(16) . . ? C28 C27 C29 121.20(16) . . ? C26 C27 C29 119.98(16) . . ? C27 C28 C23 121.48(16) . . ? C27 C28 H28 119.3 . . ? C23 C28 H28 119.3 . . ? O3 C29 C27 111.80(15) . . ? O3 C29 H29A 109.3 . . ? C27 C29 H29A 109.3 . . ? O3 C29 H29B 109.3 . . ? C27 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? O7 C30 O8 126.80(15) . . ? O7 C30 C25 117.20(15) . . ? O8 C30 C25 116.00(15) . . ? O4 C31 C32 112.39(14) . . ? O4 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? O4 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? C37 C32 C33 119.18(16) . . ? C37 C32 C31 120.61(16) . . ? C33 C32 C31 120.11(17) . . ? C32 C33 C34 119.68(16) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C33 C34 C35 120.69(15) . . ? C33 C34 C39 119.58(15) . . ? C35 C34 C39 119.71(15) . . ? C36 C35 C34 119.85(16) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 118.80(16) . . ? C37 C36 C38 121.10(15) . . ? C35 C36 C38 120.04(16) . . ? C32 C37 C36 121.73(15) . . ? C32 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? O5 C38 C36 111.71(14) . . ? O5 C38 H38A 109.3 . . ? C36 C38 H38A 109.3 . . ? O5 C38 H38B 109.3 . . ? C36 C38 H38B 109.3 . . ? H38A C38 H38B 107.9 . . ? O9 C39 O10 126.70(15) . . ? O9 C39 C34 117.74(15) . . ? O10 C39 C34 115.56(15) . . ? O6 C40 C41 111.70(14) . . ? O6 C40 H40A 109.3 . . ? C41 C40 H40A 109.3 . . ? O6 C40 H40B 109.3 . . ? C41 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C46 C41 C42 119.59(15) . . ? C46 C41 C40 120.44(15) . . ? C42 C41 C40 119.88(15) . . ? C41 C42 C43 119.72(15) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C42 C43 C44 120.12(15) . . ? C42 C43 C48 120.14(15) . . ? C44 C43 C48 119.71(15) . . ? C45 C44 C43 120.44(15) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 118.83(15) . . ? C44 C45 C47 120.33(15) . . ? C46 C45 C47 120.76(15) . . ? C41 C46 C45 121.16(15) . . ? C41 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? O1 C47 C45 111.86(14) . . ? O1 C47 H47A 109.2 . . ? C45 C47 H47A 109.2 . . ? O1 C47 H47B 109.2 . . ? C45 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? O11 C48 O12 126.44(16) . . ? O11 C48 C43 117.87(15) . . ? O12 C48 C43 115.68(14) . . ? C50 C49 C70 113.28(14) . . ? C50 C49 H49A 108.9 . . ? C70 C49 H49A 108.9 . . ? C50 C49 H49B 108.9 . . ? C70 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C55 C50 C51 118.24(16) . . ? C55 C50 C49 124.00(16) . . ? C51 C50 C49 117.75(16) . . ? C52 C51 C50 122.47(17) . . ? C52 C51 H51 118.8 . . ? C50 C51 H51 118.8 . . ? O13 C52 C51 125.54(17) . . ? O13 C52 C53 115.41(16) . . ? C51 C52 C53 119.02(16) . . ? C54 C53 O14 124.84(16) . . ? C54 C53 C52 118.78(16) . . ? O14 C53 C52 116.35(16) . . ? C53 C54 C55 122.23(17) . . ? C53 C54 H54 118.9 . . ? C55 C54 H54 118.9 . . ? C50 C55 C54 119.12(16) . . ? C50 C55 C56 123.34(16) . . ? C54 C55 C56 117.49(16) . . ? C57 C56 C55 112.65(14) . . ? C57 C56 H56A 109.1 . . ? C55 C56 H56A 109.1 . . ? C57 C56 H56B 109.1 . . ? C55 C56 H56B 109.1 . . ? H56A C56 H56B 107.8 . . ? C62 C57 C58 118.83(16) . . ? C62 C57 C56 123.67(15) . . ? C58 C57 C56 117.49(15) . . ? C59 C58 C57 122.00(16) . . ? C59 C58 H58 119.0 . . ? C57 C58 H58 119.0 . . ? O15 C59 C58 125.24(15) . . ? O15 C59 C60 115.64(15) . . ? C58 C59 C60 119.11(15) . . ? O16 C60 C61 125.29(15) . . ? O16 C60 C59 115.69(14) . . ? C61 C60 C59 118.99(15) . . ? C60 C61 C62 122.14(16) . . ? C60 C61 H61 118.9 . . ? C62 C61 H61 118.9 . . ? C57 C62 C61 118.80(15) . . ? C57 C62 C63 124.15(15) . . ? C61 C62 C63 117.04(15) . . ? C64 C63 C62 112.64(13) . . ? C64 C63 H63A 109.1 . . ? C62 C63 H63A 109.1 . . ? C64 C63 H63B 109.1 . . ? C62 C63 H63B 109.1 . . ? H63A C63 H63B 107.8 . . ? C70 C64 C65 119.03(16) . . ? C70 C64 C63 123.59(16) . . ? C65 C64 C63 117.33(16) . . ? C66 C65 C64 122.21(17) . . ? C66 C65 H65 118.9 . . ? C64 C65 H65 118.9 . . ? O17 C66 C65 124.88(16) . . ? O17 C66 C67 116.45(15) . . ? C65 C66 C67 118.65(16) . . ? O18 C67 C68 125.48(16) . . ? O18 C67 C66 115.23(16) . . ? C68 C67 C66 119.27(16) . . ? C67 C68 C70 122.16(17) . . ? C67 C68 H68 118.9 . . ? C70 C68 H68 118.9 . . ? C64 C70 C68 118.52(16) . . ? C64 C70 C49 123.68(16) . . ? C68 C70 C49 117.79(16) . . ? O18 C71 C72 112.73(14) . . ? O18 C71 H71A 109.0 . . ? C72 C71 H71A 109.0 . . ? O18 C71 H71B 109.0 . . ? C72 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? C73 C72 C77 118.90(16) . . ? C73 C72 C71 119.82(16) . . ? C77 C72 C71 121.14(15) . . ? C74 C73 C72 120.20(17) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C75 C74 C73 120.27(16) . . ? C75 C74 C79 119.35(16) . . ? C73 C74 C79 120.28(16) . . ? C76 C75 C74 120.06(17) . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C75 C76 C77 119.23(17) . . ? C75 C76 C78 119.44(16) . . ? C77 C76 C78 121.22(16) . . ? C76 C77 C72 121.28(16) . . ? C76 C77 H77 119.4 . . ? C72 C77 H77 119.4 . . ? O13 C78 C76 112.85(14) . . ? O13 C78 H78A 109.0 . . ? C76 C78 H78A 109.0 . . ? O13 C78 H78B 109.0 . . ? C76 C78 H78B 109.0 . . ? H78A C78 H78B 107.8 . . ? O19 C79 O20 127.11(16) . . ? O19 C79 C74 117.72(15) . . ? O20 C79 C74 115.17(16) . . ? O14 C80 C81 111.94(14) . . ? O14 C80 H80A 109.2 . . ? C81 C80 H80A 109.2 . . ? O14 C80 H80B 109.2 . . ? C81 C80 H80B 109.2 . . ? H80A C80 H80B 107.9 . . ? C86 C81 C82 119.23(16) . . ? C86 C81 C80 119.89(15) . . ? C82 C81 C80 120.71(15) . . ? C81 C82 C83 119.76(16) . . ? C81 C82 H82 120.1 . . ? C83 C82 H82 120.1 . . ? C84 C83 C82 120.41(15) . . ? C84 C83 C88 118.68(15) . . ? C82 C83 C88 120.86(15) . . ? C85 C84 C83 120.07(16) . . ? C85 C84 H84 120.0 . . ? C83 C84 H84 120.0 . . ? C84 C85 C86 119.14(15) . . ? C84 C85 C87 120.02(16) . . ? C86 C85 C87 120.81(15) . . ? C81 C86 C85 121.27(15) . . ? C81 C86 H86 119.4 . . ? C85 C86 H86 119.4 . . ? O15 C87 C85 112.80(13) . . ? O15 C87 H87A 109.0 . . ? C85 C87 H87A 109.0 . . ? O15 C87 H87B 109.0 . . ? C85 C87 H87B 109.0 . . ? H87A C87 H87B 107.8 . . ? O22 C88 O21 126.54(16) . . ? O22 C88 C83 115.02(15) . . ? O21 C88 C83 118.44(15) . . ? O16 C89 C90 111.41(13) . . ? O16 C89 H89A 109.3 . . ? C90 C89 H89A 109.3 . . ? O16 C89 H89B 109.3 . . ? C90 C89 H89B 109.3 . . ? H89A C89 H89B 108.0 . . ? C95 C90 C91 119.03(15) . . ? C95 C90 C89 121.48(14) . . ? C91 C90 C89 119.36(15) . . ? C92 C91 C90 120.03(15) . . ? C92 C91 H91 120.0 . . ? C90 C91 H91 120.0 . . ? C91 C92 C93 120.04(15) . . ? C91 C92 C97 119.67(14) . . ? C93 C92 C97 120.29(14) . . ? C94 C93 C92 120.55(15) . . ? C94 C93 H93 119.7 . . ? C92 C93 H93 119.7 . . ? C95 C94 C93 118.60(15) . . ? C95 C94 C96 120.50(15) . . ? C93 C94 C96 120.83(15) . . ? C94 C95 C90 121.67(15) . . ? C94 C95 H95 119.2 . . ? C90 C95 H95 119.2 . . ? O17 C96 C94 112.01(13) . . ? O17 C96 H96A 109.2 . . ? C94 C96 H96A 109.2 . . ? O17 C96 H96B 109.2 . . ? C94 C96 H96B 109.2 . . ? H96A C96 H96B 107.9 . . ? O24 C97 O23 126.27(15) . . ? O24 C97 C92 115.68(14) . . ? O23 C97 C92 118.05(14) . . ? O25 C98 N1 125.86(18) . . ? O25 C98 H98 117.1 . . ? N1 C98 H98 117.1 . . ? N1 C99 H99A 109.5 . . ? N1 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? N1 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? N1 C100 H10A 109.5 . . ? N1 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? N1 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O26 C101 N2 125.43(19) . . ? O26 C101 H101 117.3 . . ? N2 C101 H101 117.3 . . ? N2 C102 H10D 109.5 . . ? N2 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? N2 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? N2 C103 H10G 109.5 . . ? N2 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? N2 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? O27 C104 N3 125.7(2) . . ? O27 C104 H104 117.1 . . ? N3 C104 H104 117.1 . . ? N3 C105 H10J 109.5 . . ? N3 C105 H10K 109.5 . . ? H10J C105 H10K 109.5 . . ? N3 C105 H10L 109.5 . . ? H10J C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? N3 C106 H10M 109.5 . . ? N3 C106 H10N 109.5 . . ? H10M C106 H10N 109.5 . . ? N3 C106 H10O 109.5 . . ? H10M C106 H10O 109.5 . . ? H10N C106 H10O 109.5 . . ? C107 N4 C109 121.2(4) . . ? C107 N4 C108 118.9(3) . . ? C109 N4 C108 119.8(3) . . ? N4 C108 H10P 109.5 . . ? N4 C108 H10Q 109.5 . . ? H10P C108 H10Q 109.5 . . ? N4 C108 H10R 109.5 . . ? H10P C108 H10R 109.5 . . ? H10Q C108 H10R 109.5 . . ? O28 C109 N4 128.1(5) . . ? O28 C109 H109 115.9 . . ? N4 C109 H109 115.9 . . ? N4 C107 H10S 109.5 . . ? N4 C107 H10T 109.5 . . ? H10S C107 H10T 109.5 . . ? N4 C107 H10U 109.5 . . ? H10S C107 H10U 109.5 . . ? H10T C107 H10U 109.5 . . ? C111 N203 C110 119.7(3) . . ? C111 N203 C113 116.4(3) . . ? C110 N203 C113 119.0(3) . . ? C111 N203 C112 117.6(5) . . ? C110 N203 C112 107.9(4) . . ? C113 N203 C112 62.2(5) . . ? N203 C111 H11A 109.5 . . ? N203 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? N203 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? N203 C110 H11D 109.5 . . ? N203 C110 H11E 109.5 . . ? H11D C110 H11E 109.5 . . ? N203 C110 H11F 109.5 . . ? H11D C110 H11F 109.5 . . ? H11E C110 H11F 109.5 . . ? N203 C113 H11G 109.5 . . ? N203 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? N203 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? O29A C112 N203 127.2(7) . . ? O29A C112 H112 116.4 . . ? N203 C112 H112 116.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.808 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.060 # Attachment 'compound2-776458-.CIF.txt' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 776457' #TrackingRef 'compound2-776458-.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; di{Tris[3,5-bis(methyl)benzoate]cyclotricatechylene}- tris(diethylformamide)tricopper(ii) diethylformamide clathrate ; _chemical_name_common ; di(Tris(3,5-bis(methyl)benzoate)cyclotricatechylene)- tris(diethylformamide)tricopper(ii) diethylformamide clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H110 Cu3 N4 O28' _chemical_formula_weight 2198.70 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 16.129(3) _cell_length_b 17.520(3) _cell_length_c 19.048(3) _cell_angle_alpha 88.520(10) _cell_angle_beta 83.420(10) _cell_angle_gamma 88.020(10) _cell_volume 5342.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9909 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.55 _exptl_crystal_description block _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2290 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8831 _exptl_absorpt_correction_T_max 0.9119 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS (Sheldrick, G. M. 2003) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86359 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.41 _reflns_number_total 42057 _reflns_number_gt 32894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _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. High residual e-densities are < 1 A from heavy metal sites ; _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^)+(0.0183P)^2^+201.1465P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 42057 _refine_ls_number_parameters 628 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2123 _refine_ls_R_factor_gt 0.1666 _refine_ls_wR_factor_ref 0.4079 _refine_ls_wR_factor_gt 0.3584 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.555 _refine_ls_shift/su_mean 0.014 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 0.72299(10) 0.14707(9) 0.06818(9) 0.0246(4) Uani 1 1 d . . . Cu2 Cu 0.71788(11) 0.34754(9) 0.06829(9) 0.0238(4) Uani 1 1 d . . . Cu3 Cu 0.88643(10) 0.25068(10) 0.12824(9) 0.0318(4) Uani 1 1 d . . . O1 O 0.8705(8) 0.3166(7) 0.4637(7) 0.055(3) Uiso 1 1 d . . . O2 O 0.8772(9) 0.1654(8) 0.4626(7) 0.068(4) Uiso 1 1 d . . . O3 O 0.5587(6) -0.0251(6) 0.3601(5) 0.033(2) Uiso 1 1 d . . . O4 O 0.4291(6) 0.0513(6) 0.3190(5) 0.033(2) Uiso 1 1 d . . . O5 O 0.4140(7) 0.4369(7) 0.3172(6) 0.048(3) Uiso 1 1 d . . . O6 O 0.5403(8) 0.5111(7) 0.3598(7) 0.059(3) Uiso 1 1 d . . . O7 O 0.8327(7) 0.1888(6) 0.2049(5) 0.040(3) Uiso 1 1 d . . . O8 O 0.7554(6) 0.1015(5) 0.1571(5) 0.028(2) Uiso 1 1 d . . . O9 O 0.6221(7) 0.1832(6) 0.1257(5) 0.040(3) Uiso 1 1 d . . . O10 O 0.6059(6) 0.3100(5) 0.1058(5) 0.030(2) Uiso 1 1 d . . . O11 O 0.7267(6) 0.3704(6) 0.1674(5) 0.038(3) Uiso 1 1 d . . . O12 O 0.8589(7) 0.3371(7) 0.1909(6) 0.049(3) Uiso 1 1 d . . . O13 O 0.7626(6) 0.4419(6) -0.2750(5) 0.036(3) Uiso 1 1 d . . . O14 O 0.8764(7) 0.5253(6) -0.2290(5) 0.040(3) Uiso 1 1 d . . . O15 O 1.2093(7) 0.3463(6) -0.1040(6) 0.046(3) Uiso 1 1 d . . . O16 O 1.2128(7) 0.1950(6) -0.0977(6) 0.044(3) Uiso 1 1 d . . . O17 O 0.9245(7) -0.0161(6) -0.2246(6) 0.041(3) Uiso 1 1 d . . . O18 O 0.7961(6) 0.0586(6) -0.2694(5) 0.034(2) Uiso 1 1 d . . . O19 O 0.8196(6) 0.3977(6) 0.0303(5) 0.036(3) Uiso 1 1 d . . . O20 O 0.9270(6) 0.3129(6) 0.0474(5) 0.038(3) Uiso 1 1 d . . . O21 O 0.7150(6) 0.3133(6) -0.0265(5) 0.035(2) Uiso 1 1 d . . . O22 O 0.6858(6) 0.1862(5) -0.0196(5) 0.033(2) Uiso 1 1 d . . . O23 O 0.8265(7) 0.1192(6) 0.0129(6) 0.041(3) Uiso 1 1 d . . . O24 O 0.9268(7) 0.1631(7) 0.0717(6) 0.051(3) Uiso 1 1 d . . . O25 O 1.0209(7) 0.2382(7) 0.1683(6) 0.053(3) Uiso 1 1 d . . . O26 O 0.6507(7) 0.4645(6) 0.0524(6) 0.047(3) Uiso 1 1 d . . . O27 O 0.6613(6) 0.0325(6) 0.0532(5) 0.031(2) Uiso 1 1 d . . . O201 O 0.8090(16) 0.9470(14) 0.5795(14) 0.163(9) Uiso 1 1 d . . . N1 N 0.5541(14) 0.5464(13) 0.1086(13) 0.104(7) Uiso 1 1 d . . . N2 N 1.1595(8) 0.2325(9) 0.1201(7) 0.053(4) Uiso 1 1 d . . . N3 N 0.9020(18) 0.8474(19) 0.6005(15) 0.137(9) Uiso 1 1 d . . . N75 N 0.5684(10) -0.0536(9) 0.1085(8) 0.052(4) Uiso 1 1 d . . . C1 C 0.5672(11) 0.3269(10) 0.5613(9) 0.051(5) Uiso 1 1 d . . . H1A H 0.5796 0.3723 0.5878 0.061 Uiso 1 1 calc R . . H1B H 0.5293 0.2945 0.5929 0.061 Uiso 1 1 calc R . . C2 C 0.6465(10) 0.2829(10) 0.5387(9) 0.045(4) Uiso 1 1 d . . . C3 C 0.7206(11) 0.3204(10) 0.5135(9) 0.050(5) Uiso 1 1 d . . . H3 H 0.7198 0.3746 0.5139 0.060 Uiso 1 1 calc R . . C4 C 0.7942(12) 0.2824(11) 0.4883(10) 0.059(5) Uiso 1 1 d . . . C5 C 0.8038(12) 0.1986(11) 0.4879(10) 0.052(5) Uiso 1 1 d . . . C6 C 0.7287(10) 0.1622(9) 0.5142(8) 0.037(4) Uiso 1 1 d . . . H6 H 0.7302 0.1079 0.5158 0.045 Uiso 1 1 calc R . . C7 C 0.6544(12) 0.1982(11) 0.5373(10) 0.052(5) Uiso 1 1 d . . . C8 C 0.5769(11) 0.1498(10) 0.5610(9) 0.048(5) Uiso 1 1 d . . . H8A H 0.5950 0.1031 0.5862 0.058 Uiso 1 1 calc R . . H8B H 0.5379 0.1795 0.5947 0.058 Uiso 1 1 calc R . . C9 C 0.5300(10) 0.1262(9) 0.4992(8) 0.037(4) Uiso 1 1 d . . . C10 C 0.5641(10) 0.0619(9) 0.4607(8) 0.038(4) Uiso 1 1 d . . . H10 H 0.6113 0.0348 0.4756 0.045 Uiso 1 1 calc R . . C11 C 0.5296(9) 0.0376(8) 0.4010(8) 0.032(4) Uiso 1 1 d . . . C12 C 0.4637(10) 0.0778(9) 0.3790(8) 0.033(4) Uiso 1 1 d . . . C13 C 0.4251(9) 0.1419(8) 0.4169(7) 0.028(3) Uiso 1 1 d . . . H13 H 0.3766 0.1675 0.4027 0.033 Uiso 1 1 calc R . . C14 C 0.4622(10) 0.1656(9) 0.4765(9) 0.039(4) Uiso 1 1 d . . . C15 C 0.4220(10) 0.2409(10) 0.5122(9) 0.052(4) Uiso 1 1 d . . . H15A H 0.3608 0.2409 0.5112 0.063 Uiso 1 1 calc R . . H15B H 0.4328 0.2403 0.5623 0.063 Uiso 1 1 calc R . . C16 C 0.4554(11) 0.3150(10) 0.4762(9) 0.044(4) Uiso 1 1 d . . . C17 C 0.4156(10) 0.3418(10) 0.4169(9) 0.043(4) Uiso 1 1 d . . . H17 H 0.3681 0.3171 0.4042 0.051 Uiso 1 1 calc R . . C18 C 0.4482(12) 0.4071(11) 0.3762(10) 0.055(5) Uiso 1 1 d . . . C19 C 0.5143(12) 0.4460(11) 0.4005(11) 0.057(5) Uiso 1 1 d . . . C20 C 0.5516(14) 0.4221(12) 0.4618(12) 0.071(6) Uiso 1 1 d . . . H20 H 0.5929 0.4516 0.4792 0.086 Uiso 1 1 calc R . . C21 C 0.5251(11) 0.3522(10) 0.4968(10) 0.050(5) Uiso 1 1 d . . . C22 C 0.8799(13) 0.0833(11) 0.4506(11) 0.066(6) Uiso 1 1 d . . . H22A H 0.8614 0.0555 0.4953 0.080 Uiso 1 1 calc R . . H22B H 0.9379 0.0659 0.4344 0.080 Uiso 1 1 calc R . . C23 C 0.8237(10) 0.0663(9) 0.3956(8) 0.038(4) Uiso 1 1 d . . . C24 C 0.8310(9) 0.1059(8) 0.3302(8) 0.032(4) Uiso 1 1 d . . . H24 H 0.8696 0.1457 0.3215 0.038 Uiso 1 1 calc R . . C25 C 0.7808(9) 0.0866(8) 0.2766(7) 0.025(3) Uiso 1 1 d . . . C26 C 0.7218(9) 0.0317(7) 0.2914(7) 0.024(3) Uiso 1 1 d . . . H26 H 0.6875 0.0201 0.2560 0.029 Uiso 1 1 calc R . . C27 C 0.7101(9) -0.0083(8) 0.3575(8) 0.033(4) Uiso 1 1 d . . . C28 C 0.7633(9) 0.0077(9) 0.4094(8) 0.034(4) Uiso 1 1 d . . . H28 H 0.7590 -0.0202 0.4531 0.041 Uiso 1 1 calc R . . C29 C 0.6372(9) -0.0619(9) 0.3745(8) 0.034(4) Uiso 1 1 d . . . H29A H 0.6476 -0.1082 0.3457 0.041 Uiso 1 1 calc R . . H29B H 0.6333 -0.0779 0.4249 0.041 Uiso 1 1 calc R . . C30 C 0.7885(8) 0.1305(8) 0.2067(7) 0.024(3) Uiso 1 1 d . . . C31 C 0.3644(10) 0.0995(8) 0.2894(8) 0.035(4) Uiso 1 1 d . . . H31A H 0.3177 0.1095 0.3268 0.042 Uiso 1 1 calc R . . H31B H 0.3423 0.0718 0.2513 0.042 Uiso 1 1 calc R . . C32 C 0.3987(9) 0.1765(9) 0.2594(8) 0.032(4) Uiso 1 1 d . . . C33 C 0.4726(9) 0.1757(8) 0.2100(7) 0.026(3) Uiso 1 1 d . . . H33 H 0.5002 0.1292 0.1949 0.031 Uiso 1 1 calc R . . C34 C 0.5025(8) 0.2472(8) 0.1847(7) 0.030(3) Uiso 1 1 d . . . C35 C 0.4663(9) 0.3157(8) 0.2105(8) 0.032(4) Uiso 1 1 d . . . H35 H 0.4908 0.3627 0.1953 0.038 Uiso 1 1 calc R . . C36 C 0.3928(10) 0.3155(9) 0.2598(8) 0.035(4) Uiso 1 1 d . . . C37 C 0.3588(8) 0.2457(9) 0.2811(7) 0.032(3) Uiso 1 1 d . . . H37 H 0.3074 0.2448 0.3110 0.038 Uiso 1 1 calc R . . C38 C 0.3538(11) 0.3913(10) 0.2896(10) 0.050(5) Uiso 1 1 d . . . H38A H 0.3290 0.4206 0.2516 0.060 Uiso 1 1 calc R . . H38B H 0.3084 0.3800 0.3275 0.060 Uiso 1 1 calc R . . C39 C 0.5817(8) 0.2479(8) 0.1351(6) 0.026(3) Uiso 1 1 d . . . C40 C 0.6135(12) 0.5470(11) 0.3744(11) 0.057(5) Uiso 1 1 d . . . H40A H 0.6080 0.5607 0.4248 0.068 Uiso 1 1 calc R . . H40B H 0.6202 0.5947 0.3456 0.068 Uiso 1 1 calc R . . C41 C 0.6892(13) 0.4959(12) 0.3583(11) 0.062(5) Uiso 1 1 d . . . C42 C 0.7069(11) 0.4591(10) 0.2914(9) 0.046(4) Uiso 1 1 d . . . H42 H 0.6705 0.4695 0.2563 0.056 Uiso 1 1 calc R . . C43 C 0.7726(11) 0.4106(10) 0.2763(9) 0.045(4) Uiso 1 1 d . . . C44 C 0.8271(10) 0.3918(9) 0.3286(8) 0.039(4) Uiso 1 1 d . . . H44 H 0.8724 0.3561 0.3194 0.046 Uiso 1 1 calc R . . C45 C 0.8118(12) 0.4277(11) 0.3936(10) 0.054(5) Uiso 1 1 d . . . C46 C 0.7447(11) 0.4794(10) 0.4072(10) 0.049(5) Uiso 1 1 d . . . H46 H 0.7369 0.5040 0.4514 0.059 Uiso 1 1 calc R . . C47 C 0.7886(10) 0.3669(9) 0.2044(8) 0.035(4) Uiso 1 1 d . . . C48 C 0.8687(12) 0.4010(11) 0.4537(10) 0.059(5) Uiso 1 1 d . . . H48A H 0.9263 0.4184 0.4405 0.070 Uiso 1 1 calc R . . H48B H 0.8467 0.4251 0.4988 0.070 Uiso 1 1 calc R . . C51 C 0.9727(9) 0.2598(9) -0.3975(7) 0.037(4) Uiso 1 1 d . . . H51A H 0.9319 0.2597 -0.4326 0.045 Uiso 1 1 calc R . . H51B H 1.0291 0.2619 -0.4240 0.045 Uiso 1 1 calc R . . C52 C 0.9667(10) 0.1845(9) -0.3543(8) 0.037(4) Uiso 1 1 d . . . C53 C 0.8850(10) 0.1544(9) -0.3358(8) 0.041(4) Uiso 1 1 d . . . H53 H 0.8382 0.1791 -0.3537 0.049 Uiso 1 1 calc R . . C54 C 0.8729(9) 0.0877(8) -0.2908(8) 0.032(3) Uiso 1 1 d . . . C55 C 0.9444(10) 0.0518(9) -0.2674(9) 0.042(4) Uiso 1 1 d . . . C56 C 1.0211(10) 0.0796(9) -0.2847(8) 0.037(4) Uiso 1 1 d . . . H56 H 1.0684 0.0539 -0.2684 0.045 Uiso 1 1 calc R . . C57 C 1.0318(10) 0.1472(10) -0.3274(9) 0.042(4) Uiso 1 1 d . . . C58 C 1.1251(11) 0.1750(10) -0.3384(9) 0.051(5) Uiso 1 1 d . . . H58A H 1.1632 0.1294 -0.3416 0.061 Uiso 1 1 calc R . . H58B H 1.1339 0.2033 -0.3842 0.061 Uiso 1 1 calc R . . C59 C 1.1498(9) 0.2262(9) -0.2803(8) 0.038(4) Uiso 1 1 d . . . C60 C 1.1736(10) 0.1896(9) -0.2191(8) 0.040(4) Uiso 1 1 d . . . H60 H 1.1772 0.1353 -0.2172 0.048 Uiso 1 1 calc R . . C61 C 1.1913(9) 0.2285(9) -0.1629(8) 0.041(4) Uiso 1 1 d . . . C62 C 1.1883(10) 0.3085(9) -0.1629(8) 0.039(4) Uiso 1 1 d . . . C63 C 1.1648(10) 0.3469(10) -0.2249(8) 0.042(4) Uiso 1 1 d . . . H63 H 1.1643 0.4012 -0.2273 0.051 Uiso 1 1 calc R . . C64 C 1.1427(10) 0.3071(9) -0.2817(9) 0.041(4) Uiso 1 1 d . . . C65 C 1.1113(10) 0.3551(10) -0.3428(9) 0.043(4) Uiso 1 1 d . . . H65A H 1.1435 0.4023 -0.3499 0.052 Uiso 1 1 calc R . . H65B H 1.1212 0.3258 -0.3868 0.052 Uiso 1 1 calc R . . C66 C 1.0182(10) 0.3768(9) -0.3286(8) 0.035(4) Uiso 1 1 d . . . C67 C 0.9945(11) 0.4400(10) -0.2890(9) 0.044(4) Uiso 1 1 d . . . H67 H 1.0364 0.4704 -0.2736 0.053 Uiso 1 1 calc R . . C68 C 0.9075(9) 0.4615(9) -0.2700(8) 0.033(4) Uiso 1 1 d . . . C69 C 0.8465(9) 0.4158(8) -0.2954(7) 0.028(3) Uiso 1 1 d . . . C70 C 0.8712(8) 0.3560(8) -0.3379(7) 0.024(3) Uiso 1 1 d . . . H70 H 0.8300 0.3291 -0.3582 0.028 Uiso 1 1 calc R . . C71 C 0.9566(8) 0.3325(7) -0.3532(7) 0.020(3) Uiso 1 1 d . . . C72 C 0.9910(11) -0.0440(10) -0.1848(9) 0.047(4) Uiso 1 1 d . . . H72A H 1.0416 -0.0548 -0.2180 0.057 Uiso 1 1 calc R . . H72B H 0.9744 -0.0927 -0.1604 0.057 Uiso 1 1 calc R . . C73 C 1.0120(11) 0.0123(10) -0.1300(9) 0.048(4) Uiso 1 1 d . . . C74 C 0.9463(10) 0.0443(9) -0.0826(8) 0.039(4) Uiso 1 1 d . . . H74 H 0.8899 0.0310 -0.0837 0.047 Uiso 1 1 calc R . . C75 C 0.9694(10) 0.0976(9) -0.0333(9) 0.041(4) Uiso 1 1 d . . . C76 C 1.0520(9) 0.1184(9) -0.0341(8) 0.035(4) Uiso 1 1 d . . . H76 H 1.0665 0.1531 -0.0003 0.042 Uiso 1 1 calc R . . C77 C 1.1137(10) 0.0886(9) -0.0842(8) 0.040(4) Uiso 1 1 d . . . C78 C 1.0916(10) 0.0347(9) -0.1298(8) 0.036(4) Uiso 1 1 d . . . H78 H 1.1340 0.0124 -0.1625 0.044 Uiso 1 1 calc R . . C79 C 0.9027(10) 0.1293(9) 0.0216(8) 0.036(4) Uiso 1 1 d . . . C80 C 1.2042(11) 0.1140(10) -0.0886(9) 0.046(4) Uiso 1 1 d . . . H80A H 1.2277 0.0970 -0.0448 0.055 Uiso 1 1 calc R . . H80B H 1.2373 0.0882 -0.1287 0.055 Uiso 1 1 calc R . . C81 C 1.1874(11) 0.4276(10) -0.0962(10) 0.047(4) Uiso 1 1 d . . . H81A H 1.2154 0.4566 -0.1370 0.057 Uiso 1 1 calc R . . H81B H 1.2077 0.4459 -0.0527 0.057 Uiso 1 1 calc R . . C82 C 1.0932(10) 0.4425(9) -0.0922(9) 0.039(4) Uiso 1 1 d . . . C83 C 1.0377(9) 0.4016(8) -0.0425(8) 0.034(4) Uiso 1 1 d . . . H83 H 1.0595 0.3639 -0.0121 0.041 Uiso 1 1 calc R . . C84 C 0.9516(9) 0.4161(8) -0.0378(8) 0.033(4) Uiso 1 1 d . . . C85 C 0.9206(10) 0.4664(9) -0.0833(8) 0.038(4) Uiso 1 1 d . . . H85 H 0.8619 0.4758 -0.0796 0.046 Uiso 1 1 calc R . . C86 C 0.9716(10) 0.5058(9) -0.1361(8) 0.038(4) Uiso 1 1 d . . . C87 C 1.0567(10) 0.4942(9) -0.1369(8) 0.036(4) Uiso 1 1 d . . . H87 H 1.0923 0.5232 -0.1699 0.044 Uiso 1 1 calc R . . C88 C 0.9374(9) 0.5617(8) -0.1897(8) 0.034(4) Uiso 1 1 d . . . H88A H 0.9102 0.6063 -0.1646 0.040 Uiso 1 1 calc R . . H88B H 0.9841 0.5802 -0.2233 0.040 Uiso 1 1 calc R . . C89 C 0.8939(10) 0.3702(9) 0.0168(8) 0.036(4) Uiso 1 1 d . . . C90 C 0.6992(9) 0.3936(8) -0.2887(8) 0.030(3) Uiso 1 1 d . . . H90A H 0.7056 0.3828 -0.3398 0.036 Uiso 1 1 calc R . . H90B H 0.6445 0.4206 -0.2773 0.036 Uiso 1 1 calc R . . C91 C 0.6988(9) 0.3178(8) -0.2470(8) 0.029(3) Uiso 1 1 d . . . C92 C 0.7000(9) 0.3186(8) -0.1719(7) 0.026(3) Uiso 1 1 d . . . H92 H 0.6979 0.3656 -0.1479 0.032 Uiso 1 1 calc R . . C93 C 0.7043(7) 0.2498(8) -0.1347(6) 0.022(3) Uiso 1 1 d . . . C94 C 0.7061(8) 0.1769(8) -0.1681(7) 0.024(3) Uiso 1 1 d . . . H94 H 0.7064 0.1302 -0.1416 0.029 Uiso 1 1 calc R . . C95 C 0.7071(9) 0.1785(8) -0.2439(7) 0.027(3) Uiso 1 1 d . . . C96 C 0.7021(9) 0.2445(9) -0.2809(8) 0.041(4) Uiso 1 1 d . . . H96 H 0.7007 0.2431 -0.3306 0.049 Uiso 1 1 calc R . . C97 C 0.7006(7) 0.2478(8) -0.0515(6) 0.023(3) Uiso 1 1 d . . . C98 C 0.7204(9) 0.1046(8) -0.2853(8) 0.030(3) Uiso 1 1 d . . . H98A H 0.6706 0.0731 -0.2742 0.036 Uiso 1 1 calc R . . H98B H 0.7255 0.1175 -0.3365 0.036 Uiso 1 1 calc R . . C99 C 0.6137(11) 0.0114(10) 0.1052(9) 0.044(4) Uiso 1 1 d . . . H99 H 0.6081 0.0425 0.1456 0.053 Uiso 1 1 calc R . . C100 C 0.5108(17) -0.0750(15) 0.1757(14) 0.095(8) Uiso 1 1 d . . . H10A H 0.4541 -0.0843 0.1635 0.114 Uiso 1 1 calc R . . H10B H 0.5069 -0.0326 0.2094 0.114 Uiso 1 1 calc R . . C101 C 0.549(2) -0.1513(18) 0.2112(17) 0.136(12) Uiso 1 1 d . . . H10C H 0.5582 -0.1914 0.1760 0.204 Uiso 1 1 calc R . . H10D H 0.5099 -0.1687 0.2510 0.204 Uiso 1 1 calc R . . H10E H 0.6024 -0.1399 0.2281 0.204 Uiso 1 1 calc R . . C102 C 0.580(2) -0.1065(18) 0.0461(17) 0.125(11) Uiso 1 1 d . . . H10F H 0.6154 -0.0823 0.0060 0.151 Uiso 1 1 calc R . . H10G H 0.6086 -0.1551 0.0593 0.151 Uiso 1 1 calc R . . C103 C 0.504(2) -0.1201(17) 0.0274(17) 0.125(11) Uiso 1 1 d . . . H10H H 0.4634 -0.0810 0.0475 0.188 Uiso 1 1 calc R . . H10I H 0.4862 -0.1706 0.0455 0.188 Uiso 1 1 calc R . . H10J H 0.5056 -0.1184 -0.0242 0.188 Uiso 1 1 calc R . . C104 C 0.6071(11) 0.4844(10) 0.1060(10) 0.047(4) Uiso 1 1 d . . . H104 H 0.6104 0.4549 0.1482 0.056 Uiso 1 1 calc R . . C105 C 0.5208(19) 0.5740(16) 0.1781(15) 0.109(10) Uiso 1 1 d D . . H10K H 0.5283 0.5313 0.2121 0.131 Uiso 1 1 calc R . . H10L H 0.4599 0.5819 0.1772 0.131 Uiso 1 1 calc R . . C106 C 0.552(2) 0.6461(18) 0.211(2) 0.173(16) Uiso 1 1 d D . . H10M H 0.5889 0.6734 0.1747 0.260 Uiso 1 1 calc R . . H10N H 0.5822 0.6313 0.2506 0.260 Uiso 1 1 calc R . . H10O H 0.5038 0.6796 0.2268 0.260 Uiso 1 1 calc R . . C107 C 0.5840(16) 0.6158(14) 0.0559(13) 0.086(7) Uiso 1 1 d . . . H10P H 0.6058 0.6579 0.0816 0.103 Uiso 1 1 calc R . . H10Q H 0.6270 0.5987 0.0178 0.103 Uiso 1 1 calc R . . C108 C 0.510(2) 0.6374(19) 0.0298(18) 0.149(13) Uiso 1 1 d . . . H10R H 0.4992 0.6025 -0.0074 0.224 Uiso 1 1 calc R . . H10S H 0.5134 0.6896 0.0102 0.224 Uiso 1 1 calc R . . H10T H 0.4636 0.6354 0.0681 0.224 Uiso 1 1 calc R . . C110 C 0.949(3) 0.805(2) 0.661(2) 0.199(19) Uiso 1 1 d . . . H11A H 0.9368 0.8343 0.7051 0.239 Uiso 1 1 calc R . . H11B H 1.0099 0.8063 0.6467 0.239 Uiso 1 1 calc R . . C111 C 0.920(3) 0.712(2) 0.677(2) 0.197(18) Uiso 1 1 d . . . H11C H 0.8601 0.7107 0.6913 0.295 Uiso 1 1 calc R . . H11D H 0.9502 0.6900 0.7154 0.295 Uiso 1 1 calc R . . H11E H 0.9349 0.6824 0.6344 0.295 Uiso 1 1 calc R . . C112 C 0.890(2) 0.782(2) 0.561(2) 0.182(16) Uiso 1 1 d . . . H11F H 0.9266 0.7857 0.5160 0.219 Uiso 1 1 calc R . . H11G H 0.9117 0.7368 0.5876 0.219 Uiso 1 1 calc R . . C113 C 0.8029(12) 0.7639(13) 0.5448(10) 0.076(6) Uiso 1 1 d . . . H11H H 0.7627 0.8017 0.5670 0.114 Uiso 1 1 calc R . . H11I H 0.7884 0.7128 0.5632 0.114 Uiso 1 1 calc R . . H11J H 0.8014 0.7660 0.4935 0.114 Uiso 1 1 calc R . . C114 C 1.0799(11) 0.2516(11) 0.1221(9) 0.058(5) Uiso 1 1 d . . . H114 H 1.0650 0.2802 0.0821 0.069 Uiso 1 1 calc R . . C115 C 1.1893(14) 0.1665(12) 0.1696(11) 0.075(6) Uiso 1 1 d . . . H11K H 1.2280 0.1881 0.2001 0.090 Uiso 1 1 calc R . . H11L H 1.1401 0.1488 0.2008 0.090 Uiso 1 1 calc R . . C117 C 1.2313(15) 0.0996(13) 0.1342(12) 0.084(7) Uiso 1 1 d . . . H11M H 1.1909 0.0721 0.1105 0.126 Uiso 1 1 calc R . . H11N H 1.2544 0.0657 0.1693 0.126 Uiso 1 1 calc R . . H11O H 1.2766 0.1166 0.0991 0.126 Uiso 1 1 calc R . . C118 C 1.2236(13) 0.2617(14) 0.0672(11) 0.078(6) Uiso 1 1 d . . . H11P H 1.1969 0.2902 0.0298 0.094 Uiso 1 1 calc R . . H11Q H 1.2572 0.2185 0.0450 0.094 Uiso 1 1 calc R . . C119 C 1.2814(16) 0.3151(13) 0.1012(13) 0.096(8) Uiso 1 1 d . . . H11R H 1.2533 0.3326 0.1466 0.145 Uiso 1 1 calc R . . H11S H 1.2939 0.3594 0.0697 0.145 Uiso 1 1 calc R . . H11T H 1.3334 0.2873 0.1088 0.145 Uiso 1 1 calc R . . C109 C 0.872(3) 0.912(3) 0.615(2) 0.197(18) Uiso 1 1 d . . . H109 H 0.8932 0.9386 0.6515 0.236 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 0.0241(9) 0.0224(8) 0.0257(9) 0.0103(7) 0.0024(8) -0.0036(7) Cu2 0.0286(9) 0.0200(8) 0.0225(9) 0.0032(7) -0.0008(8) -0.0084(7) Cu3 0.0322(9) 0.0252(9) 0.0374(9) 0.0216(9) -0.0025(8) -0.0150(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O23 1.923(11) . ? Cu1 O22 1.941(10) . ? Cu1 O9 1.951(11) . ? Cu1 O8 1.972(9) . ? Cu1 O27 2.308(10) . ? Cu2 O21 1.924(10) . ? Cu2 O19 1.946(10) . ? Cu2 O11 1.963(10) . ? Cu2 O10 1.992(10) . ? Cu2 O26 2.313(12) . ? Cu3 O20 1.929(10) . ? Cu3 O7 1.937(10) . ? Cu3 O24 1.947(12) . ? Cu3 O12 1.960(12) . ? Cu3 O25 2.381(11) . ? O1 C4 1.41(2) . ? O1 C48 1.49(2) . ? O2 C5 1.34(2) . ? O2 C22 1.46(2) . ? O3 C11 1.401(17) . ? O3 C29 1.451(17) . ? O4 C12 1.424(18) . ? O4 C31 1.473(18) . ? O5 C18 1.39(2) . ? O5 C38 1.43(2) . ? O6 C19 1.41(2) . ? O6 C40 1.41(2) . ? O7 C30 1.264(16) . ? O8 C30 1.262(16) . ? O9 C39 1.293(17) . ? O10 C39 1.264(16) . ? O11 C47 1.285(18) . ? O12 C47 1.234(18) . ? O13 C90 1.400(17) . ? O13 C69 1.427(17) . ? O14 C68 1.424(18) . ? O14 C88 1.473(17) . ? O15 C62 1.398(19) . ? O15 C81 1.461(19) . ? O16 C61 1.433(18) . ? O16 C80 1.436(18) . ? O17 C72 1.448(19) . ? O17 C55 1.448(19) . ? O18 C54 1.370(17) . ? O18 C98 1.496(17) . ? O19 C89 1.276(18) . ? O20 C89 1.279(18) . ? O21 C97 1.291(16) . ? O22 C97 1.242(16) . ? O23 C79 1.279(18) . ? O24 C79 1.242(18) . ? O25 C114 1.244(19) . ? O26 C104 1.224(19) . ? O27 C99 1.238(18) . ? O201 C109 1.40(4) . ? N1 C104 1.36(3) . ? N1 C105 1.46(3) . ? N1 C107 1.61(3) . ? N2 C114 1.31(2) . ? N2 C118 1.46(2) . ? N2 C115 1.57(2) . ? N3 C109 1.23(4) . ? N3 C112 1.42(4) . ? N3 C110 1.60(4) . ? N75 C99 1.37(2) . ? N75 C102 1.52(3) . ? N75 C100 1.54(3) . ? C1 C2 1.50(2) . ? C1 C21 1.52(2) . ? C2 C3 1.41(2) . ? C2 C7 1.49(2) . ? C3 C4 1.38(3) . ? C4 C5 1.47(2) . ? C5 C6 1.42(2) . ? C6 C7 1.37(2) . ? C7 C8 1.55(2) . ? C8 C9 1.54(2) . ? C9 C14 1.38(2) . ? C9 C10 1.42(2) . ? C10 C11 1.40(2) . ? C11 C12 1.35(2) . ? C12 C13 1.44(2) . ? C13 C14 1.42(2) . ? C14 C15 1.58(2) . ? C15 C16 1.54(2) . ? C16 C17 1.43(2) . ? C16 C21 1.42(2) . ? C17 C18 1.44(2) . ? C18 C19 1.41(3) . ? C19 C20 1.42(3) . ? C20 C21 1.43(3) . ? C22 C23 1.50(2) . ? C23 C24 1.41(2) . ? C23 C28 1.44(2) . ? C24 C25 1.43(2) . ? C25 C26 1.378(19) . ? C25 C30 1.515(19) . ? C26 C27 1.42(2) . ? C27 C28 1.42(2) . ? C27 C29 1.53(2) . ? C31 C32 1.55(2) . ? C32 C37 1.40(2) . ? C32 C33 1.43(2) . ? C33 C34 1.411(19) . ? C34 C35 1.39(2) . ? C34 C39 1.500(17) . ? C35 C36 1.43(2) . ? C36 C37 1.39(2) . ? C36 C38 1.54(2) . ? C40 C41 1.50(3) . ? C41 C46 1.38(3) . ? C41 C42 1.44(3) . ? C42 C43 1.34(2) . ? C43 C44 1.43(2) . ? C43 C47 1.58(2) . ? C44 C45 1.40(2) . ? C45 C46 1.39(2) . ? C45 C48 1.60(3) . ? C51 C52 1.54(2) . ? C51 C71 1.544(19) . ? C52 C57 1.36(2) . ? C52 C53 1.44(2) . ? C53 C54 1.44(2) . ? C54 C55 1.41(2) . ? C55 C56 1.35(2) . ? C56 C57 1.42(2) . ? C57 C58 1.59(2) . ? C58 C59 1.54(2) . ? C59 C60 1.40(2) . ? C59 C64 1.42(2) . ? C60 C61 1.35(2) . ? C61 C62 1.40(2) . ? C62 C63 1.43(2) . ? C63 C64 1.39(2) . ? C64 C65 1.54(2) . ? C65 C66 1.53(2) . ? C66 C67 1.38(2) . ? C66 C71 1.41(2) . ? C67 C68 1.45(2) . ? C68 C69 1.42(2) . ? C69 C70 1.361(19) . ? C70 C71 1.424(18) . ? C72 C73 1.53(2) . ? C73 C78 1.36(2) . ? C73 C74 1.42(2) . ? C74 C75 1.43(2) . ? C75 C76 1.39(2) . ? C75 C79 1.51(2) . ? C76 C77 1.39(2) . ? C77 C78 1.38(2) . ? C77 C80 1.53(2) . ? C81 C82 1.53(2) . ? C82 C87 1.39(2) . ? C82 C83 1.42(2) . ? C83 C84 1.40(2) . ? C84 C85 1.34(2) . ? C84 C89 1.54(2) . ? C85 C86 1.41(2) . ? C86 C87 1.38(2) . ? C86 C88 1.53(2) . ? C90 C91 1.530(19) . ? C91 C92 1.43(2) . ? C91 C96 1.45(2) . ? C92 C93 1.387(19) . ? C93 C94 1.440(18) . ? C93 C97 1.578(16) . ? C94 C95 1.442(19) . ? C95 C96 1.34(2) . ? C95 C98 1.528(19) . ? C100 C101 1.62(3) . ? C102 C103 1.36(4) . ? C105 C106 1.544(18) . ? C107 C108 1.39(4) . ? C110 C111 1.73(4) . ? C112 C113 1.53(4) . ? C115 C117 1.47(3) . ? C118 C119 1.55(3) . ? 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 O23 Cu1 O22 86.5(4) . . ? O23 Cu1 O9 175.3(5) . . ? O22 Cu1 O9 93.7(4) . . ? O23 Cu1 O8 94.8(4) . . ? O22 Cu1 O8 176.0(4) . . ? O9 Cu1 O8 85.3(4) . . ? O23 Cu1 O27 94.6(4) . . ? O22 Cu1 O27 89.9(4) . . ? O9 Cu1 O27 90.1(4) . . ? O8 Cu1 O27 86.2(4) . . ? O21 Cu2 O19 85.4(4) . . ? O21 Cu2 O11 173.2(4) . . ? O19 Cu2 O11 95.7(4) . . ? O21 Cu2 O10 95.7(4) . . ? O19 Cu2 O10 172.2(4) . . ? O11 Cu2 O10 84.2(4) . . ? O21 Cu2 O26 96.2(4) . . ? O19 Cu2 O26 86.0(4) . . ? O11 Cu2 O26 90.7(4) . . ? O10 Cu2 O26 86.2(4) . . ? O20 Cu3 O7 173.1(5) . . ? O20 Cu3 O24 86.4(5) . . ? O7 Cu3 O24 94.0(5) . . ? O20 Cu3 O12 94.8(5) . . ? O7 Cu3 O12 85.7(5) . . ? O24 Cu3 O12 172.7(5) . . ? O20 Cu3 O25 92.6(4) . . ? O7 Cu3 O25 94.3(4) . . ? O24 Cu3 O25 82.9(4) . . ? O12 Cu3 O25 89.8(4) . . ? C4 O1 C48 117.1(14) . . ? C5 O2 C22 118.1(15) . . ? C11 O3 C29 117.4(11) . . ? C12 O4 C31 118.2(11) . . ? C18 O5 C38 116.4(14) . . ? C19 O6 C40 118.7(15) . . ? C30 O7 Cu3 133.0(10) . . ? C30 O8 Cu1 130.9(9) . . ? C39 O9 Cu1 136.0(9) . . ? C39 O10 Cu2 133.0(9) . . ? C47 O11 Cu2 132.1(10) . . ? C47 O12 Cu3 125.1(11) . . ? C90 O13 C69 116.8(11) . . ? C68 O14 C88 115.8(11) . . ? C62 O15 C81 119.4(12) . . ? C61 O16 C80 116.7(12) . . ? C72 O17 C55 114.1(12) . . ? C54 O18 C98 118.0(11) . . ? C89 O19 Cu2 129.9(10) . . ? C89 O20 Cu3 131.5(10) . . ? C97 O21 Cu2 132.5(9) . . ? C97 O22 Cu1 129.6(9) . . ? C79 O23 Cu1 132.4(10) . . ? C79 O24 Cu3 135.4(11) . . ? C114 O25 Cu3 114.5(11) . . ? C104 O26 Cu2 111.9(11) . . ? C99 O27 Cu1 113.9(10) . . ? C104 N1 C105 118(2) . . ? C104 N1 C107 115(2) . . ? C105 N1 C107 111(2) . . ? C114 N2 C118 123.7(16) . . ? C114 N2 C115 120.4(16) . . ? C118 N2 C115 115.4(15) . . ? C109 N3 C112 143(4) . . ? C109 N3 C110 115(4) . . ? C112 N3 C110 97(3) . . ? C99 N75 C102 118.3(18) . . ? C99 N75 C100 120.9(16) . . ? C102 N75 C100 120.7(19) . . ? C2 C1 C21 109.8(15) . . ? C3 C2 C7 114.2(17) . . ? C3 C2 C1 121.3(16) . . ? C7 C2 C1 124.4(16) . . ? C4 C3 C2 123.6(18) . . ? C3 C4 O1 126.2(18) . . ? C3 C4 C5 123.0(18) . . ? O1 C4 C5 110.7(17) . . ? O2 C5 C6 127.8(17) . . ? O2 C5 C4 119.9(17) . . ? C6 C5 C4 112.2(17) . . ? C7 C6 C5 126.0(17) . . ? C6 C7 C2 120.9(17) . . ? C6 C7 C8 119.5(16) . . ? C2 C7 C8 119.7(17) . . ? C9 C8 C7 113.5(14) . . ? C14 C9 C10 118.8(15) . . ? C14 C9 C8 124.9(15) . . ? C10 C9 C8 116.2(15) . . ? C11 C10 C9 121.4(15) . . ? C12 C11 O3 115.7(14) . . ? C12 C11 C10 118.9(15) . . ? O3 C11 C10 125.4(14) . . ? C11 C12 O4 117.8(13) . . ? C11 C12 C13 122.2(14) . . ? O4 C12 C13 119.8(13) . . ? C14 C13 C12 117.3(14) . . ? C9 C14 C13 121.3(15) . . ? C9 C14 C15 123.5(15) . . ? C13 C14 C15 115.1(14) . . ? C16 C15 C14 113.9(13) . . ? C17 C16 C21 121.1(16) . . ? C17 C16 C15 115.8(15) . . ? C21 C16 C15 122.9(16) . . ? C16 C17 C18 119.2(16) . . ? O5 C18 C19 118.1(17) . . ? O5 C18 C17 123.3(16) . . ? C19 C18 C17 118.4(17) . . ? C20 C19 O6 122.2(18) . . ? C20 C19 C18 122.7(19) . . ? O6 C19 C18 115.1(17) . . ? C19 C20 C21 118(2) . . ? C16 C21 C20 119.8(18) . . ? C16 C21 C1 122.6(16) . . ? C20 C21 C1 117.1(17) . . ? O2 C22 C23 109.5(16) . . ? C24 C23 C28 119.7(14) . . ? C24 C23 C22 120.6(15) . . ? C28 C23 C22 119.7(15) . . ? C23 C24 C25 120.5(14) . . ? C26 C25 C24 119.0(13) . . ? C26 C25 C30 120.9(12) . . ? C24 C25 C30 119.9(12) . . ? C25 C26 C27 122.6(13) . . ? C28 C27 C26 118.4(13) . . ? C28 C27 C29 120.9(13) . . ? C26 C27 C29 120.5(13) . . ? C27 C28 C23 119.7(14) . . ? O3 C29 C27 111.5(12) . . ? O8 C30 O7 128.8(13) . . ? O8 C30 C25 116.4(12) . . ? O7 C30 C25 114.6(12) . . ? O4 C31 C32 112.0(12) . . ? C37 C32 C33 120.8(14) . . ? C37 C32 C31 120.5(13) . . ? C33 C32 C31 118.7(13) . . ? C34 C33 C32 116.9(13) . . ? C35 C34 C33 121.9(12) . . ? C35 C34 C39 119.8(13) . . ? C33 C34 C39 117.9(13) . . ? C34 C35 C36 120.3(14) . . ? C37 C36 C35 118.4(14) . . ? C37 C36 C38 121.4(14) . . ? C35 C36 C38 120.2(14) . . ? C36 C37 C32 121.3(13) . . ? O5 C38 C36 112.1(14) . . ? O10 C39 O9 123.8(12) . . ? O10 C39 C34 119.6(12) . . ? O9 C39 C34 116.6(12) . . ? O6 C40 C41 111.3(16) . . ? C46 C41 C42 116.0(18) . . ? C46 C41 C40 122.3(18) . . ? C42 C41 C40 121.6(18) . . ? C43 C42 C41 123.1(17) . . ? C42 C43 C44 119.9(16) . . ? C42 C43 C47 122.7(16) . . ? C44 C43 C47 117.2(14) . . ? C45 C44 C43 118.0(16) . . ? C46 C45 C44 120.9(17) . . ? C46 C45 C48 121.5(17) . . ? C44 C45 C48 117.3(16) . . ? C41 C46 C45 122.0(18) . . ? O12 C47 O11 129.8(15) . . ? O12 C47 C43 115.8(14) . . ? O11 C47 C43 114.3(13) . . ? O1 C48 C45 111.3(15) . . ? C52 C51 C71 114.6(11) . . ? C57 C52 C53 117.2(15) . . ? C57 C52 C51 125.0(14) . . ? C53 C52 C51 117.6(14) . . ? C54 C53 C52 121.3(15) . . ? O18 C54 C55 119.2(13) . . ? O18 C54 C53 123.5(14) . . ? C55 C54 C53 117.3(14) . . ? C56 C55 C54 121.7(15) . . ? C56 C55 O17 126.3(15) . . ? C54 C55 O17 112.1(13) . . ? C55 C56 C57 120.4(16) . . ? C52 C57 C56 122.1(15) . . ? C52 C57 C58 124.1(15) . . ? C56 C57 C58 113.7(14) . . ? C59 C58 C57 115.5(14) . . ? C60 C59 C64 118.2(15) . . ? C60 C59 C58 117.0(15) . . ? C64 C59 C58 124.6(15) . . ? C61 C60 C59 122.3(16) . . ? C60 C61 C62 121.6(16) . . ? C60 C61 O16 125.4(15) . . ? C62 C61 O16 113.0(14) . . ? C61 C62 O15 119.4(15) . . ? C61 C62 C63 117.0(15) . . ? O15 C62 C63 123.6(14) . . ? C64 C63 C62 121.7(16) . . ? C63 C64 C59 119.1(16) . . ? C63 C64 C65 116.7(15) . . ? C59 C64 C65 124.2(15) . . ? C66 C65 C64 112.4(13) . . ? C67 C66 C71 119.5(15) . . ? C67 C66 C65 118.6(14) . . ? C71 C66 C65 121.8(14) . . ? C66 C67 C68 121.6(16) . . ? C69 C68 O14 116.2(13) . . ? C69 C68 C67 117.7(14) . . ? O14 C68 C67 126.1(14) . . ? C70 C69 C68 119.7(13) . . ? C70 C69 O13 126.5(13) . . ? C68 C69 O13 113.7(12) . . ? C69 C70 C71 122.3(13) . . ? C66 C71 C70 118.7(13) . . ? C66 C71 C51 125.9(12) . . ? C70 C71 C51 115.4(12) . . ? O17 C72 C73 113.1(13) . . ? C78 C73 C74 120.8(16) . . ? C78 C73 C72 120.0(16) . . ? C74 C73 C72 119.0(15) . . ? C75 C74 C73 116.6(15) . . ? C76 C75 C74 121.0(15) . . ? C76 C75 C79 120.2(15) . . ? C74 C75 C79 118.7(14) . . ? C75 C76 C77 120.3(15) . . ? C78 C77 C76 118.4(15) . . ? C78 C77 C80 120.3(15) . . ? C76 C77 C80 121.3(15) . . ? C73 C78 C77 122.7(16) . . ? O24 C79 O23 125.2(15) . . ? O24 C79 C75 117.0(14) . . ? O23 C79 C75 117.7(14) . . ? O16 C80 C77 113.8(13) . . ? O15 C81 C82 111.5(13) . . ? C87 C82 C83 116.5(15) . . ? C87 C82 C81 122.9(15) . . ? C83 C82 C81 120.6(14) . . ? C84 C83 C82 120.7(15) . . ? C85 C84 C83 119.5(15) . . ? C85 C84 C89 121.5(14) . . ? C83 C84 C89 118.9(14) . . ? C84 C85 C86 122.6(15) . . ? C87 C86 C85 117.0(15) . . ? C87 C86 C88 119.6(14) . . ? C85 C86 C88 123.4(14) . . ? C86 C87 C82 123.5(15) . . ? O14 C88 C86 111.4(12) . . ? O19 C89 O20 127.3(14) . . ? O19 C89 C84 115.5(13) . . ? O20 C89 C84 116.9(13) . . ? O13 C90 C91 113.9(12) . . ? C92 C91 C96 118.3(13) . . ? C92 C91 C90 119.2(13) . . ? C96 C91 C90 122.4(13) . . ? C93 C92 C91 119.1(13) . . ? C92 C93 C94 122.8(11) . . ? C92 C93 C97 120.8(12) . . ? C94 C93 C97 116.3(12) . . ? C93 C94 C95 116.5(12) . . ? C96 C95 C94 121.7(14) . . ? C96 C95 C98 117.8(13) . . ? C94 C95 C98 120.4(12) . . ? C95 C96 C91 121.7(13) . . ? O22 C97 O21 129.2(11) . . ? O22 C97 C93 118.2(12) . . ? O21 C97 C93 112.6(11) . . ? O18 C98 C95 113.4(11) . . ? O27 C99 N75 124.9(16) . . ? N75 C100 C101 109(2) . . ? C103 C102 N75 107(3) . . ? O26 C104 N1 123.6(19) . . ? N1 C105 C106 123(3) . . ? C108 C107 N1 101(2) . . ? N3 C110 C111 113(3) . . ? C113 C112 N3 119(3) . . ? O25 C114 N2 130.0(18) . . ? C117 C115 N2 116.3(18) . . ? N2 C118 C119 110.7(17) . . ? O201 C109 N3 123(4) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 24.41 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 4.262 _refine_diff_density_min -3.164 _refine_diff_density_rms 0.287 # Attachment 'compound3-776458-.CIF.txt' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 776458' #TrackingRef 'compound3-776458-.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; di{tris[3,5-bis(methyl)benzoate]cyclotricatechylene}- aquo(dimethylformamide)tricopper(ii)-1,2-bis(4-pyridyl)ethylene- di{tris[3,5-bis(methyl)benzoate]cyclotricatechylene}- aquo(dimethylformamide)tricopper(ii) dimethylformamide clathrate ; _chemical_name_common ; di(tris(3,5-bis(methyl)benzoate)cyclotricatechylene)- aquo(dimethylformamide)tricopper(ii)-1,2-bis(4-pyridyl)ethylene- di(tris(3,5-bis(methyl)benzoate)cyclotricatechylene)- aquo(dimethylformamide)tricopper(ii) dimethylformamide clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C111 H94 Cu3 N4 O28' _chemical_formula_weight 2122.52 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 17.140(4) _cell_length_b 18.030(4) _cell_length_c 20.805(5) _cell_angle_alpha 86.235(12) _cell_angle_beta 80.028(12) _cell_angle_gamma 64.703(6) _cell_volume 5725(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10649 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 32.1 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2198 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 0.791 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond Light Source station I19' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Rigaku Saturn CCD' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26820 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.1528 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 22.50 _reflns_number_total 16099 _reflns_number_gt 10527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. One solvent DMF was refined with group ADPs. SQUEEZE routine was applied to data due to significant voids and diffuse residual e-density. ; _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^)+(0.1323P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16099 _refine_ls_number_parameters 1291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2289 _refine_ls_wR_factor_gt 0.2093 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 0.64402(4) 0.10244(4) 0.15145(3) 0.0284(2) Uani 1 1 d . . . Cu2 Cu 0.53040(5) 0.18714(4) 0.30702(3) 0.0306(2) Uani 1 1 d . . . Cu3 Cu 0.51553(4) 0.02176(4) 0.24726(3) 0.0291(2) Uani 1 1 d . . . O1 O 0.2252(3) 0.5400(3) 0.2373(3) 0.0550(13) Uani 1 1 d . . . O2 O 0.1302(3) 0.4790(3) 0.3114(2) 0.0511(13) Uani 1 1 d . . . O3 O 0.1122(3) 0.1479(3) 0.2113(3) 0.0538(13) Uani 1 1 d . . . O4 O 0.1946(3) 0.0822(3) 0.0988(3) 0.0573(14) Uani 1 1 d . . . O5 O 0.4269(3) 0.2485(3) -0.0972(2) 0.0529(13) Uani 1 1 d . . . O6 O 0.4376(3) 0.3747(3) -0.0532(2) 0.0539(13) Uani 1 1 d . . . O7 O 0.4084(3) 0.2038(2) 0.3271(2) 0.0381(10) Uani 1 1 d . . . O8 O 0.4043(3) 0.1165(3) 0.2578(2) 0.0483(12) Uani 1 1 d . . . O9 O 0.5030(3) 0.0211(3) 0.1577(2) 0.0373(10) Uani 1 1 d . A . O10 O 0.5508(3) 0.1103(2) 0.1058(2) 0.0420(11) Uani 1 1 d . A . O11 O 0.5896(3) 0.2236(2) 0.1487(2) 0.0372(10) Uani 1 1 d . A . O12 O 0.4915(3) 0.2673(2) 0.2394(2) 0.0390(10) Uani 1 1 d . A . O13 O 1.0555(3) -0.0668(2) 0.1963(2) 0.0399(11) Uani 1 1 d . . . O14 O 1.0429(3) -0.1898(2) 0.1492(2) 0.0350(10) Uani 1 1 d . . . O15 O 0.7852(3) -0.3463(2) 0.3196(2) 0.0374(10) Uani 1 1 d . . . O16 O 0.6977(3) -0.2847(3) 0.4325(2) 0.0463(12) Uani 1 1 d . . . O17 O 0.7332(3) 0.0271(3) 0.5601(2) 0.0494(13) Uani 1 1 d . . . O18 O 0.8292(3) 0.0894(3) 0.4874(2) 0.0460(12) Uani 1 1 d . . . O19 O 0.7047(3) -0.0180(2) 0.1483(2) 0.0339(10) Uani 1 1 d . A . O20 O 0.6360(3) -0.0593(3) 0.2342(2) 0.0416(11) Uani 1 1 d . A . O21 O 0.5200(3) 0.0087(2) 0.33975(19) 0.0371(10) Uani 1 1 d . . . O22 O 0.5718(3) 0.0963(3) 0.3654(2) 0.0448(11) Uani 1 1 d . . . O23 O 0.6502(3) 0.1766(3) 0.2915(2) 0.0412(11) Uani 1 1 d . A . O24 O 0.7284(3) 0.0939(3) 0.2055(2) 0.0420(11) Uani 1 1 d . A . N1 N 0.5059(4) 0.2828(3) 0.3830(3) 0.0466(15) Uani 1 1 d . . . C1 C 0.1222(4) 0.5047(4) 0.0391(3) 0.0445(17) Uani 1 1 d . . . H1A H 0.1266 0.5567 0.0255 0.053 Uiso 1 1 calc R . . H1B H 0.0669 0.5083 0.0277 0.053 Uiso 1 1 calc R . . C2 C 0.1172(4) 0.4976(3) 0.1122(3) 0.0388(16) Uani 1 1 d . . . C3 C 0.1706(4) 0.5250(3) 0.1391(3) 0.0385(16) Uani 1 1 d . . . H3 H 0.2041 0.5488 0.1117 0.046 Uiso 1 1 calc R . . C4 C 0.1742(4) 0.5175(4) 0.2050(4) 0.0442(18) Uani 1 1 d . . . C5 C 0.1226(4) 0.4840(4) 0.2459(3) 0.0403(16) Uani 1 1 d . . . C6 C 0.0699(4) 0.4596(4) 0.2190(3) 0.0388(16) Uani 1 1 d . . . H6 H 0.0336 0.4392 0.2470 0.047 Uiso 1 1 calc R . . C7 C 0.0672(4) 0.4634(3) 0.1518(3) 0.0363(15) Uani 1 1 d . . . C8 C 0.0108(4) 0.4302(4) 0.1258(3) 0.0414(16) Uani 1 1 d . . . H8A H -0.0071 0.4590 0.0850 0.050 Uiso 1 1 calc R . . H8B H -0.0428 0.4415 0.1580 0.050 Uiso 1 1 calc R . . C9 C 0.0590(4) 0.3379(4) 0.1122(3) 0.0383(16) Uani 1 1 d . . . C10 C 0.0602(4) 0.2864(4) 0.1653(4) 0.0392(16) Uani 1 1 d . . . H10 H 0.0281 0.3101 0.2064 0.047 Uiso 1 1 calc R . . C11 C 0.1058(4) 0.2032(4) 0.1603(4) 0.0441(17) Uani 1 1 d . . . C12 C 0.1503(4) 0.1675(4) 0.0990(4) 0.0473(19) Uani 1 1 d . . . C13 C 0.1474(4) 0.2170(4) 0.0456(4) 0.0466(18) Uani 1 1 d . . . H13 H 0.1757 0.1929 0.0038 0.056 Uiso 1 1 calc R . . C14 C 0.1026(4) 0.3038(4) 0.0520(4) 0.0431(17) Uani 1 1 d . . . C15 C 0.1095(4) 0.3532(4) -0.0097(3) 0.0420(16) Uani 1 1 d . . . H15A H 0.0584 0.4072 -0.0057 0.050 Uiso 1 1 calc R . . H15B H 0.1074 0.3240 -0.0476 0.050 Uiso 1 1 calc R . . C16 C 0.1941(4) 0.3666(4) -0.0225(3) 0.0400(16) Uani 1 1 d . . . C17 C 0.2689(4) 0.3053(4) -0.0565(3) 0.0433(17) Uani 1 1 d . . . H17 H 0.2638 0.2607 -0.0744 0.052 Uiso 1 1 calc R . . C18 C 0.3500(4) 0.3067(4) -0.0652(3) 0.0462(18) Uani 1 1 d . . . C19 C 0.3552(4) 0.3759(4) -0.0418(3) 0.0474(18) Uani 1 1 d . . . C20 C 0.2795(4) 0.4398(4) -0.0120(3) 0.0431(17) Uani 1 1 d . . . H20 H 0.2821 0.4882 0.0007 0.052 Uiso 1 1 calc R . . C21 C 0.1990(4) 0.4338(4) -0.0005(3) 0.0370(15) Uani 1 1 d . . . C22 C 0.0928(4) 0.4333(4) 0.3531(3) 0.0470(18) Uani 1 1 d . . . H22A H 0.0301 0.4542 0.3496 0.056 Uiso 1 1 calc R . . H22B H 0.0970 0.4409 0.3988 0.056 Uiso 1 1 calc R . . C23 C 0.1389(4) 0.3420(4) 0.3355(3) 0.0354(15) Uani 1 1 d . . . C24 C 0.2283(4) 0.3008(3) 0.3290(3) 0.0304(14) Uani 1 1 d . . . H24 H 0.2609 0.3276 0.3407 0.037 Uiso 1 1 calc R . . C25 C 0.2713(4) 0.2219(3) 0.3059(3) 0.0283(13) Uani 1 1 d . . . C26 C 0.2220(4) 0.1821(4) 0.2873(3) 0.0345(14) Uani 1 1 d . . . H26 H 0.2510 0.1283 0.2692 0.041 Uiso 1 1 calc R . . C27 C 0.1330(4) 0.2218(4) 0.2957(3) 0.0406(16) Uani 1 1 d . . . C28 C 0.0905(4) 0.3023(4) 0.3193(3) 0.0451(17) Uani 1 1 d . . . H28 H 0.0285 0.3301 0.3243 0.054 Uiso 1 1 calc R . . C29 C 0.0801(5) 0.1807(5) 0.2767(4) 0.054(2) Uani 1 1 d . . . H29A H 0.0826 0.1358 0.3076 0.065 Uiso 1 1 calc R . . H29B H 0.0182 0.2210 0.2798 0.065 Uiso 1 1 calc R . . C30 C 0.3697(4) 0.1769(4) 0.2960(3) 0.0307(14) Uani 1 1 d . . . C31 C 0.2528(5) 0.0431(5) 0.0421(5) 0.065(2) Uani 1 1 d . . . H31A H 0.2208 0.0577 0.0045 0.078 Uiso 1 1 calc R . . H31B H 0.2760 -0.0170 0.0477 0.078 Uiso 1 1 calc R . . C32 C 0.3285(4) 0.0676(4) 0.0276(4) 0.0448(18) Uani 1 1 d . . . C33 C 0.3825(4) 0.0562(4) 0.0734(3) 0.0402(16) Uani 1 1 d . . . H33 H 0.3741 0.0300 0.1134 0.048 Uiso 1 1 calc R . . C34 C 0.4485(4) 0.0825(4) 0.0616(3) 0.0339(15) Uani 1 1 d . A . C35 C 0.4641(4) 0.1185(4) 0.0032(3) 0.0385(16) Uani 1 1 d . . . H35 H 0.5092 0.1369 -0.0045 0.046 Uiso 1 1 calc R . . C36 C 0.4120(4) 0.1273(4) -0.0448(3) 0.0439(18) Uani 1 1 d . . . C37 C 0.3479(4) 0.1013(4) -0.0331(4) 0.050(2) Uani 1 1 d . . . H37 H 0.3149 0.1057 -0.0665 0.060 Uiso 1 1 calc R . . C38 C 0.4285(5) 0.1709(5) -0.1096(3) 0.062(2) Uani 1 1 d . . . H38A H 0.4860 0.1356 -0.1348 0.074 Uiso 1 1 calc R . . H38B H 0.3830 0.1789 -0.1363 0.074 Uiso 1 1 calc R . . C39 C 0.5054(4) 0.0694(4) 0.1131(3) 0.0326(15) Uani 1 1 d . . . C40 C 0.4489(5) 0.4383(5) -0.0223(4) 0.053(2) Uani 1 1 d . . . H40A H 0.4056 0.4924 -0.0344 0.063 Uiso 1 1 calc R . . H40B H 0.5079 0.4350 -0.0394 0.063 Uiso 1 1 calc R . . C41 C 0.4384(4) 0.4327(4) 0.0509(4) 0.0430(17) Uani 1 1 d . . . C42 C 0.4865(4) 0.3610(4) 0.0818(3) 0.0383(16) Uani 1 1 d . . . H42 H 0.5298 0.3155 0.0564 0.046 Uiso 1 1 calc R . . C43 C 0.4722(4) 0.3552(4) 0.1489(3) 0.0356(15) Uani 1 1 d . A . C44 C 0.4071(4) 0.4207(3) 0.1865(3) 0.0352(15) Uani 1 1 d . . . H44 H 0.3954 0.4154 0.2325 0.042 Uiso 1 1 calc R . . C45 C 0.3596(4) 0.4936(4) 0.1566(3) 0.0381(16) Uani 1 1 d . . . C46 C 0.3759(4) 0.4975(4) 0.0908(4) 0.0478(19) Uani 1 1 d . . . H46 H 0.3430 0.5472 0.0705 0.057 Uiso 1 1 calc R . . C47 C 0.2883(5) 0.5640(4) 0.1971(4) 0.061(2) Uani 1 1 d . . . H47A H 0.3149 0.5855 0.2255 0.073 Uiso 1 1 calc R . . H47B H 0.2579 0.6087 0.1678 0.073 Uiso 1 1 calc R . . C48 C 0.5221(4) 0.2748(3) 0.1823(3) 0.0286(13) Uani 1 1 d . . . C50 C 1.0672(4) -0.1831(4) 0.4180(3) 0.0360(15) Uani 1 1 d . . . H50A H 1.1067 -0.1568 0.4208 0.043 Uiso 1 1 calc R . . H50B H 1.0923 -0.2384 0.4372 0.043 Uiso 1 1 calc R . . C51 C 1.0629(4) -0.1917(4) 0.3464(3) 0.0311(14) Uani 1 1 d . . . C52 C 1.0636(4) -0.1276(4) 0.3048(3) 0.0360(15) Uani 1 1 d . . . H52 H 1.0690 -0.0825 0.3216 0.043 Uiso 1 1 calc R . . C53 C 1.0565(4) -0.1290(4) 0.2398(3) 0.0350(15) Uani 1 1 d . . . C54 C 1.0493(4) -0.1950(3) 0.2144(3) 0.0287(14) Uani 1 1 d . . . C55 C 1.0519(4) -0.2594(3) 0.2542(3) 0.0286(13) Uani 1 1 d . . . H55 H 1.0497 -0.3056 0.2365 0.034 Uiso 1 1 calc R . . C56 C 1.0577(4) -0.2586(3) 0.3216(3) 0.0292(14) Uani 1 1 d . . . C57 C 1.0519(4) -0.3294(4) 0.3636(3) 0.0327(14) Uani 1 1 d . . . H57A H 1.0841 -0.3810 0.3379 0.039 Uiso 1 1 calc R . . H57B H 1.0810 -0.3346 0.4018 0.039 Uiso 1 1 calc R . . C58 C 0.9584(4) -0.3190(3) 0.3875(3) 0.0279(13) Uani 1 1 d . . . C59 C 0.9173(4) -0.3418(3) 0.3449(3) 0.0299(14) Uani 1 1 d . . . H59 H 0.9501 -0.3675 0.3045 0.036 Uiso 1 1 calc R . . C60 C 0.8314(4) -0.3281(4) 0.3598(3) 0.0344(15) Uani 1 1 d . . . C61 C 0.7838(4) -0.2944(4) 0.4212(3) 0.0402(16) Uani 1 1 d . . . C62 C 0.8250(4) -0.2774(4) 0.4648(3) 0.0377(15) Uani 1 1 d . . . H62 H 0.7941 -0.2585 0.5074 0.045 Uiso 1 1 calc R . . C63 C 0.9130(4) -0.2871(4) 0.4483(3) 0.0351(15) Uani 1 1 d . . . C64 C 0.9494(4) -0.2582(4) 0.4989(3) 0.0367(15) Uani 1 1 d . . . H64A H 0.9270 -0.2717 0.5431 0.044 Uiso 1 1 calc R . . H64B H 1.0139 -0.2883 0.4918 0.044 Uiso 1 1 calc R . . C65 C 0.9247(4) -0.1670(4) 0.4956(3) 0.0365(15) Uani 1 1 d . . . C66 C 0.8446(4) -0.1118(4) 0.5300(3) 0.0400(16) Uani 1 1 d . . . H66 H 0.8100 -0.1340 0.5578 0.048 Uiso 1 1 calc R . . C67 C 0.8133(4) -0.0286(4) 0.5261(3) 0.0407(17) Uani 1 1 d . . . C68 C 0.8645(4) 0.0054(4) 0.4883(3) 0.0414(18) Uani 1 1 d . . . C69 C 0.9458(4) -0.0459(4) 0.4559(3) 0.0371(16) Uani 1 1 d . . . H69 H 0.9818 -0.0225 0.4315 0.045 Uiso 1 1 calc R . . C70 C 0.9772(4) -0.1322(4) 0.4580(3) 0.0367(16) Uani 1 1 d . . . C71 C 1.0185(4) -0.2483(3) 0.1226(3) 0.0312(14) Uani 1 1 d . . . H71A H 1.0614 -0.3047 0.1303 0.037 Uiso 1 1 calc R . . H71B H 1.0211 -0.2406 0.0749 0.037 Uiso 1 1 calc R . . C72 C 0.9292(4) -0.2392(4) 0.1521(3) 0.0309(14) Uani 1 1 d . . . C73 C 0.8575(4) -0.1636(3) 0.1533(3) 0.0264(13) Uani 1 1 d . . . H73 H 0.8646 -0.1187 0.1310 0.032 Uiso 1 1 calc R . . C74 C 0.7766(4) -0.1528(3) 0.1861(3) 0.0269(13) Uani 1 1 d . A . C75 C 0.7652(4) -0.2187(3) 0.2184(3) 0.0292(13) Uani 1 1 d . . . H75 H 0.7093 -0.2106 0.2416 0.035 Uiso 1 1 calc R . . C76 C 0.8347(4) -0.2965(3) 0.2169(3) 0.0297(14) Uani 1 1 d . . . C77 C 0.9163(4) -0.3051(3) 0.1828(3) 0.0302(14) Uani 1 1 d . . . H77 H 0.9644 -0.3576 0.1805 0.036 Uiso 1 1 calc R . . C78 C 0.8249(4) -0.3660(4) 0.2531(3) 0.0381(15) Uani 1 1 d . . . H78A H 0.7889 -0.3840 0.2313 0.046 Uiso 1 1 calc R . . H78B H 0.8833 -0.4125 0.2517 0.046 Uiso 1 1 calc R . . C79 C 0.6985(4) -0.0694(4) 0.1902(3) 0.0292(14) Uani 1 1 d . . . C80 C 0.6408(4) -0.2368(4) 0.4895(4) 0.0480(18) Uani 1 1 d . . . H80A H 0.6660 -0.2624 0.5291 0.058 Uiso 1 1 calc R . . H80B H 0.5831 -0.2381 0.4933 0.058 Uiso 1 1 calc R . . C81 C 0.6285(4) -0.1497(4) 0.4869(3) 0.0365(15) Uani 1 1 d . . . C82 C 0.5976(4) -0.1001(4) 0.4345(3) 0.0384(16) Uani 1 1 d . . . H82 H 0.5813 -0.1212 0.4010 0.046 Uiso 1 1 calc R . . C83 C 0.5901(4) -0.0204(4) 0.4307(3) 0.0317(14) Uani 1 1 d . . . C84 C 0.6128(4) 0.0096(4) 0.4808(3) 0.0443(17) Uani 1 1 d . . . H84 H 0.6081 0.0641 0.4784 0.053 Uiso 1 1 calc R . . C85 C 0.6417(4) -0.0374(4) 0.5339(3) 0.0435(17) Uani 1 1 d . . . C86 C 0.6476(4) -0.1170(4) 0.5363(3) 0.0452(18) Uani 1 1 d . . . H86 H 0.6654 -0.1496 0.5733 0.054 Uiso 1 1 calc R . . C87 C 0.6696(4) -0.0036(5) 0.5867(3) 0.054(2) Uani 1 1 d . . . H87A H 0.6175 0.0411 0.6107 0.065 Uiso 1 1 calc R . . H87B H 0.6946 -0.0476 0.6182 0.065 Uiso 1 1 calc R . . C88 C 0.5583(4) 0.0325(4) 0.3748(3) 0.0342(15) Uani 1 1 d . . . C90 C 0.8748(5) 0.1270(4) 0.4442(4) 0.053(2) Uani 1 1 d . . . H90A H 0.9355 0.1058 0.4531 0.064 Uiso 1 1 calc R . . H90B H 0.8465 0.1869 0.4528 0.064 Uiso 1 1 calc R . . C91 C 0.8771(4) 0.1116(4) 0.3722(3) 0.0377(16) Uani 1 1 d . . . C92 C 0.8012(4) 0.1302(4) 0.3470(3) 0.0349(15) Uani 1 1 d . . . H92 H 0.7462 0.1575 0.3740 0.042 Uiso 1 1 calc R . . C93 C 0.8038(4) 0.1100(4) 0.2837(3) 0.0352(15) Uani 1 1 d . A . C94 C 0.8840(4) 0.0700(3) 0.2437(3) 0.0362(15) Uani 1 1 d . . . H94 H 0.8861 0.0540 0.2006 0.043 Uiso 1 1 calc R . . C95 C 0.9618(4) 0.0532(3) 0.2674(3) 0.0329(15) Uani 1 1 d . . . C96 C 0.9569(4) 0.0729(4) 0.3295(3) 0.0376(16) Uani 1 1 d . . . H96 H 1.0098 0.0601 0.3456 0.045 Uiso 1 1 calc R . . C97 C 1.0487(4) 0.0072(4) 0.2236(3) 0.0398(16) Uani 1 1 d . . . H97A H 1.0561 0.0436 0.1877 0.048 Uiso 1 1 calc R . . H97B H 1.0966 -0.0066 0.2492 0.048 Uiso 1 1 calc R . . C98 C 0.7204(4) 0.1286(3) 0.2582(3) 0.0328(14) Uani 1 1 d . . . C100 C 0.5597(6) 0.2647(6) 0.4278(4) 0.068(2) Uani 1 1 d . . . H100 H 0.5976 0.2086 0.4327 0.082 Uiso 1 1 calc R . . C101 C 0.5640(6) 0.3207(7) 0.4667(5) 0.084(3) Uani 1 1 d . . . H101 H 0.6015 0.3044 0.4987 0.101 Uiso 1 1 calc R . . C102 C 0.5098(8) 0.4040(8) 0.4569(5) 0.099(4) Uani 1 1 d . . . C103 C 0.4551(8) 0.4249(6) 0.4102(5) 0.095(4) Uani 1 1 d . . . H103 H 0.4188 0.4806 0.4024 0.114 Uiso 1 1 calc R . . C104 C 0.4549(7) 0.3607(5) 0.3746(4) 0.077(3) Uani 1 1 d . . . H104 H 0.4166 0.3744 0.3434 0.092 Uiso 1 1 calc R . . C105 C 0.5226(7) 0.4641(7) 0.5017(6) 0.111(4) Uani 1 1 d . . . H105 H 0.5647 0.4440 0.5303 0.133 Uiso 1 1 calc R . . O120 O 0.2398(5) 0.6478(4) 1.0051(4) 0.102(3) Uani 1 1 d . . . N120 N 0.1845(6) 0.7202(5) 0.9188(4) 0.084(3) Uani 1 1 d . . . C122 C 0.2447(7) 0.6912(6) 0.9584(6) 0.093(4) Uani 1 1 d . . . H122 H 0.2932 0.7049 0.9498 0.111 Uiso 1 1 calc R . . C121 C 0.1056(8) 0.7069(8) 0.9306(6) 0.120(4) Uani 1 1 d . . . H12A H 0.0554 0.7582 0.9240 0.180 Uiso 1 1 calc R . . H12B H 0.0969 0.6885 0.9756 0.180 Uiso 1 1 calc R . . H12C H 0.1113 0.6649 0.9003 0.180 Uiso 1 1 calc R . . C120 C 0.1902(12) 0.7746(10) 0.8652(8) 0.187(9) Uani 1 1 d . . . H12D H 0.1565 0.8317 0.8799 0.280 Uiso 1 1 calc R . . H12E H 0.1664 0.7644 0.8289 0.280 Uiso 1 1 calc R . . H12F H 0.2515 0.7642 0.8507 0.280 Uiso 1 1 calc R . . O25 O 0.7303(4) 0.1078(3) 0.0556(3) 0.0681(16) Uani 1 1 d . A 1 N2 N 0.7068(5) 0.1754(5) -0.0469(5) 0.097(3) Uani 1 1 d . A 1 C106 C 0.6794(7) 0.1531(6) 0.0130(5) 0.080(3) Uani 1 1 d . A 1 H106 H 0.6181 0.1714 0.0258 0.096 Uiso 1 1 calc R A 1 C107 C 0.8037(8) 0.1439(10) -0.0652(7) 0.163(7) Uani 1 1 d . A 1 H10A H 0.8304 0.1324 -0.0255 0.244 Uiso 1 1 calc R A 1 H10B H 0.8180 0.1853 -0.0909 0.244 Uiso 1 1 calc R A 1 H10C H 0.8263 0.0935 -0.0911 0.244 Uiso 1 1 calc R A 1 C108 C 0.6523(8) 0.2229(8) -0.0933(9) 0.169(8) Uani 1 1 d . A 1 H10D H 0.6656 0.2699 -0.1069 0.253 Uiso 1 1 calc R A 1 H10E H 0.5907 0.2426 -0.0732 0.253 Uiso 1 1 calc R A 1 H10F H 0.6633 0.1886 -0.1314 0.253 Uiso 1 1 calc R A 1 O130 O 0.2498(8) 0.6430(8) 0.5109(7) 0.192(3) Uani 1 1 d . . . N130 N 0.1821(10) 0.5488(10) 0.5078(9) 0.192(3) Uani 1 1 d . . . C131 C 0.1014(11) 0.5342(10) 0.5286(10) 0.192(3) Uani 1 1 d . . . H13A H 0.0532 0.5847 0.5476 0.288 Uiso 1 1 calc R . . H13B H 0.1128 0.4906 0.5611 0.288 Uiso 1 1 calc R . . H13C H 0.0856 0.5178 0.4906 0.288 Uiso 1 1 calc R . . C132 C 0.1977(13) 0.6226(14) 0.5206(12) 0.192(3) Uani 1 1 d . . . H132 H 0.1465 0.6635 0.5442 0.230 Uiso 1 1 calc R . . C130 C 0.2364(11) 0.4956(10) 0.4381(10) 0.192(3) Uani 1 1 d . . . H13D H 0.1961 0.4840 0.4168 0.288 Uiso 1 1 calc R . . H13E H 0.2839 0.4439 0.4481 0.288 Uiso 1 1 calc R . . H13F H 0.2607 0.5281 0.4089 0.288 Uiso 1 1 calc R . . O30 O 0.4591(4) -0.0774(4) 0.2602(3) 0.0792(18) 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 0.0275(4) 0.0192(4) 0.0356(4) -0.0055(3) -0.0113(3) -0.0040(3) Cu2 0.0270(4) 0.0259(4) 0.0366(5) -0.0074(3) -0.0090(3) -0.0064(3) Cu3 0.0261(4) 0.0238(4) 0.0318(4) -0.0056(3) -0.0090(3) -0.0028(3) O1 0.039(3) 0.033(3) 0.085(4) -0.027(2) -0.005(3) -0.006(2) O2 0.053(3) 0.031(3) 0.058(3) -0.013(2) -0.009(2) -0.006(2) O3 0.046(3) 0.041(3) 0.087(4) 0.011(3) -0.021(3) -0.029(2) O4 0.038(3) 0.033(3) 0.102(4) -0.004(3) -0.023(3) -0.011(2) O5 0.040(3) 0.061(3) 0.033(3) -0.008(2) -0.006(2) 0.002(2) O6 0.036(3) 0.054(3) 0.060(3) 0.001(2) 0.001(2) -0.011(2) O7 0.028(2) 0.035(3) 0.047(3) -0.007(2) -0.012(2) -0.0072(19) O8 0.034(3) 0.044(3) 0.048(3) -0.020(2) -0.015(2) 0.007(2) O9 0.033(3) 0.041(3) 0.037(3) 0.000(2) -0.0126(19) -0.012(2) O10 0.048(3) 0.028(2) 0.052(3) 0.006(2) -0.028(2) -0.012(2) O11 0.037(3) 0.019(2) 0.050(3) -0.0011(19) -0.008(2) -0.006(2) O12 0.033(3) 0.036(3) 0.039(3) -0.0016(19) -0.006(2) -0.005(2) O13 0.036(3) 0.029(2) 0.052(3) 0.002(2) -0.001(2) -0.014(2) O14 0.033(2) 0.033(2) 0.036(3) -0.0065(18) -0.0001(18) -0.0127(19) O15 0.033(2) 0.036(3) 0.046(3) 0.0020(19) -0.015(2) -0.015(2) O16 0.030(3) 0.048(3) 0.055(3) 0.000(2) -0.002(2) -0.013(2) O17 0.038(3) 0.047(3) 0.044(3) -0.027(2) -0.010(2) 0.006(2) O18 0.042(3) 0.033(3) 0.054(3) -0.021(2) -0.017(2) -0.001(2) O19 0.033(2) 0.022(2) 0.039(3) -0.0080(19) -0.0073(19) -0.0031(18) O20 0.033(3) 0.034(3) 0.042(3) 0.0022(19) -0.012(2) 0.002(2) O21 0.037(3) 0.037(3) 0.031(2) -0.0045(18) -0.0072(19) -0.009(2) O22 0.054(3) 0.042(3) 0.046(3) 0.003(2) -0.021(2) -0.023(2) O23 0.030(3) 0.044(3) 0.047(3) -0.011(2) -0.014(2) -0.009(2) O24 0.029(3) 0.039(3) 0.054(3) -0.008(2) -0.016(2) -0.006(2) N1 0.047(4) 0.038(4) 0.050(4) -0.023(3) -0.002(3) -0.013(3) C1 0.037(4) 0.027(4) 0.056(5) 0.003(3) -0.008(3) -0.001(3) C2 0.027(4) 0.016(3) 0.054(4) -0.005(3) -0.001(3) 0.008(3) C3 0.032(4) 0.017(3) 0.056(5) -0.006(3) -0.003(3) -0.001(3) C4 0.028(4) 0.020(3) 0.078(6) -0.020(3) -0.004(3) -0.002(3) C5 0.046(4) 0.015(3) 0.046(4) -0.011(3) -0.006(3) 0.002(3) C6 0.024(4) 0.018(3) 0.062(5) -0.005(3) -0.003(3) 0.002(3) C7 0.031(4) 0.014(3) 0.058(5) -0.006(3) -0.007(3) -0.002(3) C8 0.022(3) 0.035(4) 0.058(5) 0.003(3) -0.009(3) -0.004(3) C9 0.020(3) 0.031(4) 0.063(5) 0.001(3) -0.019(3) -0.006(3) C10 0.030(4) 0.026(4) 0.068(5) -0.003(3) -0.020(3) -0.013(3) C11 0.031(4) 0.044(4) 0.070(5) 0.007(4) -0.021(3) -0.024(3) C12 0.035(4) 0.034(4) 0.083(6) 0.004(4) -0.032(4) -0.016(3) C13 0.030(4) 0.036(4) 0.074(5) -0.014(4) -0.018(3) -0.009(3) C14 0.026(4) 0.042(4) 0.061(5) -0.005(3) -0.025(3) -0.006(3) C15 0.032(4) 0.036(4) 0.055(4) -0.005(3) -0.022(3) -0.005(3) C16 0.036(4) 0.039(4) 0.035(4) 0.004(3) -0.014(3) -0.003(3) C17 0.033(4) 0.044(4) 0.043(4) 0.005(3) -0.018(3) -0.003(3) C18 0.034(4) 0.045(4) 0.042(4) 0.003(3) -0.010(3) 0.000(3) C19 0.029(4) 0.054(5) 0.046(4) 0.011(3) -0.003(3) -0.007(3) C20 0.041(4) 0.038(4) 0.041(4) 0.010(3) -0.001(3) -0.012(3) C21 0.028(4) 0.038(4) 0.038(4) 0.012(3) -0.014(3) -0.006(3) C22 0.039(4) 0.036(4) 0.048(4) -0.012(3) 0.000(3) 0.000(3) C23 0.025(4) 0.035(4) 0.035(4) -0.007(3) 0.001(3) -0.003(3) C24 0.034(4) 0.017(3) 0.034(3) 0.000(2) -0.004(3) -0.005(3) C25 0.027(3) 0.024(3) 0.029(3) 0.001(2) -0.004(2) -0.006(3) C26 0.033(4) 0.023(3) 0.043(4) -0.002(3) -0.006(3) -0.008(3) C27 0.035(4) 0.036(4) 0.055(4) 0.010(3) -0.014(3) -0.018(3) C28 0.032(4) 0.044(4) 0.043(4) 0.007(3) 0.002(3) -0.006(3) C29 0.038(4) 0.054(5) 0.075(6) 0.022(4) -0.014(4) -0.027(4) C30 0.029(3) 0.027(3) 0.031(3) 0.001(3) -0.017(3) -0.003(3) C31 0.055(5) 0.039(4) 0.102(7) -0.014(4) -0.041(5) -0.010(4) C32 0.034(4) 0.026(4) 0.068(5) -0.016(3) -0.026(3) 0.003(3) C33 0.030(4) 0.031(4) 0.050(4) -0.009(3) -0.015(3) 0.000(3) C34 0.030(4) 0.024(3) 0.040(4) -0.012(3) -0.014(3) 0.001(3) C35 0.031(4) 0.033(4) 0.041(4) -0.012(3) -0.015(3) 0.002(3) C36 0.032(4) 0.042(4) 0.035(4) -0.017(3) -0.016(3) 0.011(3) C37 0.034(4) 0.044(4) 0.056(5) -0.027(4) -0.028(3) 0.009(3) C38 0.055(5) 0.061(5) 0.037(4) -0.015(4) -0.018(4) 0.012(4) C39 0.026(3) 0.019(3) 0.041(4) -0.014(3) -0.006(3) 0.004(3) C40 0.032(4) 0.055(5) 0.069(5) 0.022(4) -0.004(3) -0.021(4) C41 0.020(3) 0.035(4) 0.069(5) 0.011(3) -0.004(3) -0.008(3) C42 0.024(3) 0.028(4) 0.060(5) -0.001(3) -0.006(3) -0.009(3) C43 0.026(4) 0.032(4) 0.048(4) 0.002(3) -0.011(3) -0.011(3) C44 0.027(3) 0.020(3) 0.056(4) -0.009(3) -0.002(3) -0.008(3) C45 0.037(4) 0.026(4) 0.055(5) -0.004(3) -0.008(3) -0.017(3) C46 0.033(4) 0.023(4) 0.090(6) 0.017(3) -0.021(4) -0.014(3) C47 0.040(4) 0.018(4) 0.111(7) -0.017(4) -0.008(4) 0.001(3) C48 0.030(4) 0.015(3) 0.043(4) -0.002(3) -0.013(3) -0.008(3) C50 0.035(4) 0.037(4) 0.036(4) -0.012(3) -0.009(3) -0.012(3) C51 0.024(3) 0.026(3) 0.039(4) -0.007(3) -0.006(3) -0.005(3) C52 0.025(3) 0.028(4) 0.056(5) -0.007(3) -0.009(3) -0.010(3) C53 0.030(4) 0.028(4) 0.042(4) -0.002(3) -0.006(3) -0.008(3) C54 0.021(3) 0.024(3) 0.038(4) -0.008(3) -0.002(3) -0.007(3) C55 0.026(3) 0.023(3) 0.032(3) -0.008(2) 0.004(2) -0.009(3) C56 0.018(3) 0.024(3) 0.040(4) -0.008(3) -0.008(2) 0.000(2) C57 0.036(4) 0.031(4) 0.029(3) -0.006(3) -0.005(3) -0.011(3) C58 0.027(3) 0.016(3) 0.031(3) -0.001(2) -0.004(3) 0.000(2) C59 0.032(4) 0.032(3) 0.022(3) -0.003(2) -0.003(2) -0.009(3) C60 0.032(4) 0.034(4) 0.037(4) 0.004(3) -0.012(3) -0.012(3) C61 0.029(4) 0.036(4) 0.048(4) 0.009(3) -0.003(3) -0.009(3) C62 0.036(4) 0.034(4) 0.035(4) 0.006(3) -0.011(3) -0.006(3) C63 0.037(4) 0.032(4) 0.034(4) 0.006(3) -0.008(3) -0.012(3) C64 0.034(4) 0.042(4) 0.027(3) 0.001(3) -0.008(3) -0.008(3) C65 0.025(3) 0.043(4) 0.033(4) -0.012(3) -0.009(3) -0.002(3) C66 0.028(4) 0.051(5) 0.032(4) -0.013(3) -0.010(3) -0.004(3) C67 0.036(4) 0.048(4) 0.029(4) -0.013(3) -0.017(3) -0.003(3) C68 0.039(4) 0.037(4) 0.041(4) -0.019(3) -0.026(3) 0.000(3) C69 0.036(4) 0.038(4) 0.037(4) -0.015(3) -0.022(3) -0.008(3) C70 0.025(3) 0.041(4) 0.040(4) -0.015(3) -0.018(3) -0.003(3) C71 0.039(4) 0.019(3) 0.029(3) -0.010(2) -0.006(3) -0.004(3) C72 0.030(4) 0.030(3) 0.027(3) -0.015(3) -0.001(3) -0.006(3) C73 0.030(4) 0.020(3) 0.028(3) -0.003(2) -0.012(3) -0.006(3) C74 0.028(3) 0.024(3) 0.027(3) -0.007(2) -0.013(3) -0.005(3) C75 0.031(3) 0.031(4) 0.025(3) -0.006(2) -0.009(2) -0.010(3) C76 0.031(4) 0.024(3) 0.033(3) -0.008(2) -0.013(3) -0.006(3) C77 0.033(4) 0.024(3) 0.027(3) -0.008(2) -0.015(3) -0.001(3) C78 0.036(4) 0.030(4) 0.049(4) -0.005(3) -0.012(3) -0.012(3) C79 0.026(3) 0.034(4) 0.024(3) -0.007(3) -0.009(3) -0.006(3) C80 0.028(4) 0.052(5) 0.054(5) 0.010(3) -0.002(3) -0.010(3) C81 0.025(3) 0.043(4) 0.031(4) 0.001(3) 0.001(3) -0.006(3) C82 0.033(4) 0.037(4) 0.033(4) -0.003(3) -0.001(3) -0.004(3) C83 0.026(3) 0.034(4) 0.024(3) -0.005(3) -0.005(2) -0.001(3) C84 0.024(4) 0.050(4) 0.042(4) -0.005(3) 0.001(3) -0.001(3) C85 0.026(4) 0.057(5) 0.031(4) -0.003(3) -0.007(3) 0.000(3) C86 0.030(4) 0.050(5) 0.031(4) 0.012(3) -0.006(3) 0.005(3) C87 0.031(4) 0.067(5) 0.034(4) -0.014(3) -0.013(3) 0.012(4) C88 0.027(3) 0.043(4) 0.030(4) -0.011(3) -0.008(3) -0.010(3) C90 0.046(4) 0.036(4) 0.074(5) -0.031(4) -0.027(4) -0.003(3) C91 0.035(4) 0.020(3) 0.063(5) -0.006(3) -0.017(3) -0.012(3) C92 0.025(3) 0.025(3) 0.054(4) -0.011(3) -0.017(3) -0.005(3) C93 0.025(3) 0.025(3) 0.055(4) -0.001(3) -0.013(3) -0.008(3) C94 0.042(4) 0.022(3) 0.049(4) 0.002(3) -0.015(3) -0.016(3) C95 0.026(3) 0.015(3) 0.057(4) -0.002(3) -0.007(3) -0.009(3) C96 0.032(4) 0.026(3) 0.063(5) -0.005(3) -0.015(3) -0.017(3) C97 0.035(4) 0.027(4) 0.061(5) 0.004(3) -0.008(3) -0.017(3) C98 0.038(4) 0.020(3) 0.046(4) -0.004(3) -0.013(3) -0.014(3) C100 0.066(6) 0.081(6) 0.063(6) -0.037(5) -0.012(4) -0.031(5) C101 0.075(6) 0.089(8) 0.097(7) -0.059(6) -0.004(5) -0.038(6) C102 0.140(10) 0.130(11) 0.073(7) -0.060(7) 0.020(6) -0.107(9) C103 0.154(10) 0.046(5) 0.076(7) -0.029(5) 0.013(7) -0.040(6) C104 0.100(7) 0.052(6) 0.066(6) -0.015(4) -0.008(5) -0.021(5) C105 0.071(8) 0.112(10) 0.111(9) 0.008(8) 0.008(7) -0.010(7) O120 0.155(7) 0.044(4) 0.106(6) 0.030(4) -0.078(5) -0.024(4) N120 0.123(7) 0.085(6) 0.091(6) 0.055(5) -0.065(5) -0.079(5) C122 0.121(9) 0.061(6) 0.130(9) 0.031(6) -0.088(8) -0.050(6) C121 0.126(10) 0.167(12) 0.114(10) 0.052(9) -0.050(8) -0.102(10) C120 0.27(2) 0.247(18) 0.177(15) 0.130(14) -0.097(14) -0.230(17) O25 0.091(4) 0.039(3) 0.059(4) -0.005(3) 0.007(3) -0.020(3) N2 0.055(5) 0.092(6) 0.116(7) -0.001(5) 0.025(5) -0.019(4) C106 0.076(7) 0.080(7) 0.076(7) -0.010(5) 0.029(5) -0.041(6) C107 0.107(11) 0.197(16) 0.157(14) -0.010(11) 0.067(9) -0.071(10) C108 0.083(9) 0.099(10) 0.27(2) 0.112(12) -0.034(10) -0.004(7) O130 0.127(6) 0.154(6) 0.259(8) 0.019(6) -0.009(6) -0.037(5) N130 0.127(6) 0.154(6) 0.259(8) 0.019(6) -0.009(6) -0.037(5) C131 0.127(6) 0.154(6) 0.259(8) 0.019(6) -0.009(6) -0.037(5) C132 0.127(6) 0.154(6) 0.259(8) 0.019(6) -0.009(6) -0.037(5) C130 0.127(6) 0.154(6) 0.259(8) 0.019(6) -0.009(6) -0.037(5) O30 0.094(5) 0.110(5) 0.054(3) -0.040(3) 0.020(3) -0.069(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O24 1.932(4) . ? Cu1 O10 1.946(4) . ? Cu1 O19 1.966(4) . ? Cu1 O11 1.976(4) . ? Cu1 O25 2.290(5) . ? Cu2 O22 1.924(4) . ? Cu2 O12 1.937(4) . ? Cu2 O23 1.949(4) . ? Cu2 O7 1.953(4) . ? Cu2 N1 2.272(5) . ? Cu3 O9 1.913(4) . ? Cu3 O8 1.929(4) . ? Cu3 O21 1.934(4) . ? Cu3 O20 1.937(4) . ? Cu3 O30 2.351(6) . ? O1 C4 1.387(8) . ? O1 C47 1.447(9) . ? O2 C5 1.385(8) . ? O2 C22 1.415(8) . ? O3 C11 1.392(8) . ? O3 C29 1.440(9) . ? O4 C12 1.394(8) . ? O4 C31 1.408(10) . ? O5 C18 1.374(8) . ? O5 C38 1.427(10) . ? O6 C19 1.384(8) . ? O6 C40 1.446(9) . ? O7 C30 1.251(7) . ? O8 C30 1.251(7) . ? O9 C39 1.239(7) . ? O10 C39 1.267(8) . ? O11 C48 1.255(7) . ? O12 C48 1.235(7) . ? O13 C53 1.389(7) . ? O13 C97 1.437(7) . ? O14 C54 1.374(7) . ? O14 C71 1.459(7) . ? O15 C60 1.385(7) . ? O15 C78 1.427(8) . ? O16 C61 1.388(8) . ? O16 C80 1.456(8) . ? O17 C67 1.405(8) . ? O17 C87 1.439(10) . ? O18 C68 1.370(8) . ? O18 C90 1.417(9) . ? O19 C79 1.256(7) . ? O20 C79 1.239(7) . ? O21 C88 1.262(7) . ? O22 C88 1.266(8) . ? O23 C98 1.256(7) . ? O24 C98 1.255(7) . ? N1 C104 1.319(10) . ? N1 C100 1.352(9) . ? C1 C2 1.509(9) . ? C1 C21 1.539(9) . ? C2 C7 1.390(9) . ? C2 C3 1.413(9) . ? C3 C4 1.377(10) . ? C4 C5 1.413(10) . ? C5 C6 1.368(9) . ? C6 C7 1.404(9) . ? C7 C8 1.516(9) . ? C8 C9 1.529(9) . ? C9 C14 1.375(9) . ? C9 C10 1.392(9) . ? C10 C11 1.366(9) . ? C11 C12 1.405(11) . ? C12 C13 1.373(10) . ? C13 C14 1.423(9) . ? C14 C15 1.530(10) . ? C15 C16 1.546(9) . ? C16 C21 1.362(9) . ? C16 C17 1.394(9) . ? C17 C18 1.382(10) . ? C18 C19 1.410(10) . ? C19 C20 1.390(9) . ? C20 C21 1.408(9) . ? C22 C23 1.529(9) . ? C23 C24 1.373(8) . ? C23 C28 1.398(9) . ? C24 C25 1.367(8) . ? C25 C26 1.431(8) . ? C25 C30 1.508(8) . ? C26 C27 1.363(9) . ? C27 C28 1.393(9) . ? C27 C29 1.505(9) . ? C31 C32 1.517(11) . ? C32 C33 1.389(9) . ? C32 C37 1.413(11) . ? C33 C34 1.383(9) . ? C34 C35 1.378(9) . ? C34 C39 1.512(8) . ? C35 C36 1.410(9) . ? C36 C37 1.349(10) . ? C36 C38 1.560(11) . ? C40 C41 1.505(10) . ? C41 C42 1.388(9) . ? C41 C46 1.396(10) . ? C42 C43 1.380(9) . ? C43 C44 1.394(8) . ? C43 C48 1.527(8) . ? C44 C45 1.390(9) . ? C45 C46 1.354(10) . ? C45 C47 1.507(9) . ? C50 C51 1.526(8) . ? C50 C70 1.536(8) . ? C51 C56 1.384(8) . ? C51 C52 1.401(9) . ? C52 C53 1.382(9) . ? C53 C54 1.395(8) . ? C54 C55 1.371(8) . ? C55 C56 1.423(8) . ? C56 C57 1.529(8) . ? C57 C58 1.526(8) . ? C58 C63 1.382(8) . ? C58 C59 1.401(8) . ? C59 C60 1.366(8) . ? C60 C61 1.409(9) . ? C61 C62 1.365(9) . ? C62 C63 1.424(9) . ? C63 C64 1.531(9) . ? C64 C65 1.513(9) . ? C65 C66 1.405(8) . ? C65 C70 1.409(9) . ? C66 C67 1.363(9) . ? C67 C68 1.386(10) . ? C68 C69 1.381(9) . ? C69 C70 1.412(9) . ? C71 C72 1.489(8) . ? C72 C73 1.390(8) . ? C72 C77 1.393(9) . ? C73 C74 1.372(8) . ? C74 C75 1.398(8) . ? C74 C79 1.522(8) . ? C75 C76 1.398(8) . ? C76 C77 1.403(8) . ? C76 C78 1.476(9) . ? C80 C81 1.491(10) . ? C81 C86 1.367(10) . ? C81 C82 1.391(9) . ? C82 C83 1.385(9) . ? C83 C84 1.388(9) . ? C83 C88 1.478(8) . ? C84 C85 1.376(9) . ? C85 C86 1.394(10) . ? C85 C87 1.524(10) . ? C90 C91 1.532(10) . ? C91 C92 1.385(8) . ? C91 C96 1.410(9) . ? C92 C93 1.378(9) . ? C93 C94 1.392(9) . ? C93 C98 1.506(8) . ? C94 C95 1.406(8) . ? C95 C96 1.342(9) . ? C95 C97 1.520(9) . ? C100 C101 1.368(11) . ? C101 C102 1.411(15) . ? C102 C103 1.390(15) . ? C102 C105 1.581(16) . ? C103 C104 1.414(12) . ? C105 C105 1.19(2) 2_666 ? O120 C122 1.221(12) . ? N120 C122 1.339(10) . ? N120 C121 1.450(12) . ? N120 C120 1.453(12) . ? O25 C106 1.335(11) . ? N2 C106 1.351(12) . ? N2 C108 1.435(14) . ? N2 C107 1.492(14) . ? O130 C132 1.09(2) . ? N130 C131 1.50(2) . ? N130 C132 1.51(3) . ? N130 C130 1.69(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 O24 Cu1 O10 173.7(2) . . ? O24 Cu1 O19 84.25(17) . . ? O10 Cu1 O19 95.68(17) . . ? O24 Cu1 O11 95.60(18) . . ? O10 Cu1 O11 84.95(17) . . ? O19 Cu1 O11 175.54(18) . . ? O24 Cu1 O25 94.4(2) . . ? O10 Cu1 O25 91.9(2) . . ? O19 Cu1 O25 89.51(18) . . ? O11 Cu1 O25 86.06(18) . . ? O22 Cu2 O12 172.08(19) . . ? O22 Cu2 O23 85.51(19) . . ? O12 Cu2 O23 95.23(19) . . ? O22 Cu2 O7 94.95(19) . . ? O12 Cu2 O7 84.88(18) . . ? O23 Cu2 O7 175.89(18) . . ? O22 Cu2 N1 94.1(2) . . ? O12 Cu2 N1 93.8(2) . . ? O23 Cu2 N1 85.12(19) . . ? O7 Cu2 N1 90.77(19) . . ? O9 Cu3 O8 86.45(18) . . ? O9 Cu3 O21 170.21(19) . . ? O8 Cu3 O21 94.56(18) . . ? O9 Cu3 O20 94.22(18) . . ? O8 Cu3 O20 169.9(2) . . ? O21 Cu3 O20 86.50(18) . . ? O9 Cu3 O30 84.68(19) . . ? O8 Cu3 O30 96.6(2) . . ? O21 Cu3 O30 85.53(19) . . ? O20 Cu3 O30 93.5(2) . . ? C4 O1 C47 116.8(6) . . ? C5 O2 C22 118.7(6) . . ? C11 O3 C29 117.8(5) . . ? C12 O4 C31 118.2(6) . . ? C18 O5 C38 117.2(6) . . ? C19 O6 C40 117.2(5) . . ? C30 O7 Cu2 127.3(4) . . ? C30 O8 Cu3 133.6(4) . . ? C39 O9 Cu3 130.6(4) . . ? C39 O10 Cu1 129.9(4) . . ? C48 O11 Cu1 130.3(4) . . ? C48 O12 Cu2 134.8(4) . . ? C53 O13 C97 116.7(5) . . ? C54 O14 C71 117.6(4) . . ? C60 O15 C78 117.0(5) . . ? C61 O16 C80 117.6(5) . . ? C67 O17 C87 117.5(6) . . ? C68 O18 C90 117.7(5) . . ? C79 O19 Cu1 129.4(4) . . ? C79 O20 Cu3 132.1(4) . . ? C88 O21 Cu3 130.2(4) . . ? C88 O22 Cu2 132.2(4) . . ? C98 O23 Cu2 134.5(4) . . ? C98 O24 Cu1 131.8(4) . . ? C104 N1 C100 117.8(7) . . ? C104 N1 Cu2 120.5(5) . . ? C100 N1 Cu2 119.6(5) . . ? C2 C1 C21 115.1(5) . . ? C7 C2 C3 120.5(6) . . ? C7 C2 C1 123.9(6) . . ? C3 C2 C1 115.5(6) . . ? C4 C3 C2 120.2(6) . . ? C3 C4 O1 126.0(6) . . ? C3 C4 C5 119.8(6) . . ? O1 C4 C5 114.2(7) . . ? C6 C5 O2 125.2(6) . . ? C6 C5 C4 119.0(6) . . ? O2 C5 C4 115.8(6) . . ? C5 C6 C7 122.7(6) . . ? C2 C7 C6 117.7(6) . . ? C2 C7 C8 123.3(6) . . ? C6 C7 C8 119.0(6) . . ? C7 C8 C9 111.9(5) . . ? C14 C9 C10 119.0(6) . . ? C14 C9 C8 124.1(6) . . ? C10 C9 C8 116.9(6) . . ? C11 C10 C9 122.4(7) . . ? C10 C11 O3 125.8(7) . . ? C10 C11 C12 119.1(7) . . ? O3 C11 C12 115.1(6) . . ? C13 C12 O4 125.6(7) . . ? C13 C12 C11 119.4(6) . . ? O4 C12 C11 114.9(7) . . ? C12 C13 C14 120.8(7) . . ? C9 C14 C13 119.2(7) . . ? C9 C14 C15 124.4(6) . . ? C13 C14 C15 116.4(6) . . ? C14 C15 C16 113.1(5) . . ? C21 C16 C17 119.3(7) . . ? C21 C16 C15 123.0(6) . . ? C17 C16 C15 117.6(6) . . ? C18 C17 C16 122.7(7) . . ? O5 C18 C17 126.4(7) . . ? O5 C18 C19 115.7(6) . . ? C17 C18 C19 117.8(6) . . ? O6 C19 C20 125.3(7) . . ? O6 C19 C18 115.2(6) . . ? C20 C19 C18 119.4(7) . . ? C19 C20 C21 120.9(7) . . ? C16 C21 C20 119.5(6) . . ? C16 C21 C1 124.7(6) . . ? C20 C21 C1 115.8(6) . . ? O2 C22 C23 111.4(5) . . ? C24 C23 C28 119.5(6) . . ? C24 C23 C22 120.7(6) . . ? C28 C23 C22 119.4(6) . . ? C25 C24 C23 121.5(6) . . ? C24 C25 C26 119.0(5) . . ? C24 C25 C30 122.1(5) . . ? C26 C25 C30 118.8(5) . . ? C27 C26 C25 119.7(6) . . ? C26 C27 C28 120.3(6) . . ? C26 C27 C29 120.4(6) . . ? C28 C27 C29 119.3(6) . . ? C27 C28 C23 120.0(6) . . ? O3 C29 C27 111.4(6) . . ? O8 C30 O7 126.5(6) . . ? O8 C30 C25 117.2(5) . . ? O7 C30 C25 116.3(5) . . ? O4 C31 C32 112.0(6) . . ? C33 C32 C37 117.3(7) . . ? C33 C32 C31 120.9(7) . . ? C37 C32 C31 121.8(6) . . ? C34 C33 C32 120.9(7) . . ? C35 C34 C33 120.9(6) . . ? C35 C34 C39 120.0(6) . . ? C33 C34 C39 119.1(6) . . ? C34 C35 C36 118.8(7) . . ? C37 C36 C35 120.0(7) . . ? C37 C36 C38 121.9(6) . . ? C35 C36 C38 118.0(7) . . ? C36 C37 C32 122.0(6) . . ? O5 C38 C36 111.3(5) . . ? O9 C39 O10 126.7(6) . . ? O9 C39 C34 117.8(6) . . ? O10 C39 C34 115.4(6) . . ? O6 C40 C41 113.7(6) . . ? C42 C41 C46 117.0(7) . . ? C42 C41 C40 121.4(6) . . ? C46 C41 C40 121.5(6) . . ? C43 C42 C41 120.6(6) . . ? C42 C43 C44 120.3(6) . . ? C42 C43 C48 120.4(6) . . ? C44 C43 C48 119.1(6) . . ? C45 C44 C43 119.8(6) . . ? C46 C45 C44 118.3(6) . . ? C46 C45 C47 121.7(6) . . ? C44 C45 C47 120.0(7) . . ? C45 C46 C41 123.9(6) . . ? O1 C47 C45 112.2(5) . . ? O12 C48 O11 127.2(5) . . ? O12 C48 C43 116.5(5) . . ? O11 C48 C43 116.2(6) . . ? C51 C50 C70 112.8(5) . . ? C56 C51 C52 119.6(6) . . ? C56 C51 C50 123.3(5) . . ? C52 C51 C50 117.1(5) . . ? C53 C52 C51 120.9(6) . . ? C52 C53 O13 123.7(6) . . ? C52 C53 C54 120.2(6) . . ? O13 C53 C54 116.1(5) . . ? C55 C54 O14 125.7(5) . . ? C55 C54 C53 119.2(6) . . ? O14 C54 C53 115.0(5) . . ? C54 C55 C56 121.4(5) . . ? C51 C56 C55 118.6(5) . . ? C51 C56 C57 123.5(5) . . ? C55 C56 C57 117.8(5) . . ? C58 C57 C56 113.8(5) . . ? C63 C58 C59 119.4(6) . . ? C63 C58 C57 122.9(5) . . ? C59 C58 C57 117.7(5) . . ? C60 C59 C58 121.9(5) . . ? C59 C60 O15 125.6(6) . . ? C59 C60 C61 119.3(6) . . ? O15 C60 C61 115.1(6) . . ? C62 C61 O16 125.6(6) . . ? C62 C61 C60 119.2(6) . . ? O16 C61 C60 115.2(6) . . ? C61 C62 C63 121.8(6) . . ? C58 C63 C62 118.2(6) . . ? C58 C63 C64 124.7(6) . . ? C62 C63 C64 117.0(5) . . ? C65 C64 C63 112.6(5) . . ? C66 C65 C70 116.4(6) . . ? C66 C65 C64 119.9(6) . . ? C70 C65 C64 123.7(5) . . ? C67 C66 C65 124.4(7) . . ? C66 C67 C68 118.9(6) . . ? C66 C67 O17 124.9(7) . . ? C68 C67 O17 116.1(6) . . ? O18 C68 C69 125.3(7) . . ? O18 C68 C67 115.6(6) . . ? C69 C68 C67 119.1(6) . . ? C68 C69 C70 122.1(7) . . ? C65 C70 C69 119.0(6) . . ? C65 C70 C50 123.5(6) . . ? C69 C70 C50 117.5(6) . . ? O14 C71 C72 112.8(4) . . ? C73 C72 C77 118.2(5) . . ? C73 C72 C71 120.8(5) . . ? C77 C72 C71 120.8(5) . . ? C74 C73 C72 121.2(5) . . ? C73 C74 C75 119.9(5) . . ? C73 C74 C79 121.7(5) . . ? C75 C74 C79 118.4(5) . . ? C76 C75 C74 121.0(6) . . ? C75 C76 C77 117.3(5) . . ? C75 C76 C78 121.7(6) . . ? C77 C76 C78 120.8(5) . . ? C72 C77 C76 122.3(5) . . ? O15 C78 C76 113.1(5) . . ? O20 C79 O19 127.0(5) . . ? O20 C79 C74 117.1(5) . . ? O19 C79 C74 115.9(5) . . ? O16 C80 C81 113.1(5) . . ? C86 C81 C82 118.7(6) . . ? C86 C81 C80 120.3(6) . . ? C82 C81 C80 121.0(6) . . ? C83 C82 C81 120.9(6) . . ? C82 C83 C84 118.6(6) . . ? C82 C83 C88 121.3(5) . . ? C84 C83 C88 120.1(6) . . ? C85 C84 C83 121.8(7) . . ? C84 C85 C86 117.9(6) . . ? C84 C85 C87 120.3(7) . . ? C86 C85 C87 121.7(6) . . ? C81 C86 C85 122.1(6) . . ? O17 C87 C85 112.2(6) . . ? O21 C88 O22 125.3(6) . . ? O21 C88 C83 116.0(6) . . ? O22 C88 C83 118.6(5) . . ? O18 C90 C91 113.1(5) . . ? C92 C91 C96 116.9(6) . . ? C92 C91 C90 121.5(6) . . ? C96 C91 C90 121.5(6) . . ? C93 C92 C91 121.4(6) . . ? C92 C93 C94 119.9(6) . . ? C92 C93 C98 120.3(6) . . ? C94 C93 C98 119.7(6) . . ? C93 C94 C95 119.7(6) . . ? C96 C95 C94 118.8(6) . . ? C96 C95 C97 122.2(6) . . ? C94 C95 C97 118.8(6) . . ? C95 C96 C91 123.2(6) . . ? O13 C97 C95 113.0(5) . . ? O24 C98 O23 126.6(6) . . ? O24 C98 C93 116.2(5) . . ? O23 C98 C93 117.2(5) . . ? N1 C100 C101 125.2(9) . . ? C100 C101 C102 116.5(9) . . ? C103 C102 C101 119.7(8) . . ? C103 C102 C105 127.4(12) . . ? C101 C102 C105 112.8(10) . . ? C102 C103 C104 118.1(9) . . ? N1 C104 C103 122.6(10) . . ? C105 C105 C102 117.6(18) 2_666 . ? C122 N120 C121 122.3(8) . . ? C122 N120 C120 121.5(9) . . ? C121 N120 C120 115.9(8) . . ? O120 C122 N120 122.8(10) . . ? C106 O25 Cu1 109.1(5) . . ? C106 N2 C108 126.2(10) . . ? C106 N2 C107 114.8(10) . . ? C108 N2 C107 119.0(10) . . ? O25 C106 N2 126.1(9) . . ? C131 N130 C132 129.1(17) . . ? C131 N130 C130 108.0(16) . . ? C132 N130 C130 117.1(16) . . ? O130 C132 N130 139(2) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.142 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.124 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 127 54 ' ' 2 0.463 0.389 0.712 542 193 ' ' 3 0.188 0.092 0.661 57 11 ' ' 4 0.537 0.612 0.288 542 192 ' ' 5 0.303 0.283 0.135 57 3 ' ' 6 0.696 0.717 0.865 57 3 ' ' 7 0.812 0.908 0.339 57 11 ' ' _platon_squeeze_details ; ; # Attachment 'complex4-776459-.CIF.txt' data_complex4 _database_code_depnum_ccdc_archive 'CCDC 776459' #TrackingRef 'complex4-776459-.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; di{tris[3,5-bis(methyl)benzoate]cyclotricatechylene}- tetraacetobis(dimethylformamide)oxoheptacobalt(ii) dimethylformamide clathrate hydrate ; _chemical_name_common ; di(tris(3,5-bis(methyl)benzoate)cyclotricatechylene)- tetraacetobis(dimethylformamide)oxoheptacobalt(ii) dimethylformamide clathrate hydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C113 H103 Co7 N3 O38' _chemical_formula_weight 2523.49 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' Co Co 0.3494 0.9721 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.811(3) _cell_length_b 12.2580(15) _cell_length_c 29.620(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.087(7) _cell_angle_gamma 90.00 _cell_volume 6744.2(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9740 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 24.96 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2590 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7780 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS (Sheldrick, G. M. 2003) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 273527 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16788 _reflns_number_gt 12651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _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^)+(0.1446P)^2^+13.9334P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16788 _refine_ls_number_parameters 745 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2401 _refine_ls_wR_factor_gt 0.2191 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Co1 Co 0.07520(5) 0.83407(7) 0.05819(3) 0.0252(2) Uani 1 1 d . A 1 Co2 Co 0.14951(5) 1.08396(7) 0.06210(3) 0.0292(2) Uani 1 1 d . A 1 Co3 Co 0.00830(4) 1.04201(6) 0.10909(3) 0.0222(2) Uani 1 1 d . A 1 Co4 Co 0.0000 1.0000 0.0000 0.0253(3) Uani 1 2 d S . 1 O1 O 0.0651(2) 0.9474(4) 0.33452(15) 0.0349(11) Uani 1 1 d . A 1 O2 O 0.1185(2) 1.1439(4) 0.33306(15) 0.0338(11) Uani 1 1 d . A 1 O3 O 0.4071(3) 1.2324(4) 0.23126(19) 0.0440(13) Uani 1 1 d . A 1 O4 O 0.4596(3) 1.0686(4) 0.19071(17) 0.0373(11) Uani 1 1 d . A 1 O5 O 0.3279(3) 0.5678(4) 0.19484(16) 0.0358(11) Uani 1 1 d . A 1 O6 O 0.2124(3) 0.5356(4) 0.23471(16) 0.0362(11) Uani 1 1 d . A 1 O7 O 0.0685(2) 1.1418(4) 0.15239(15) 0.0359(11) Uani 1 1 d . A 1 O8 O 0.1680(3) 1.1695(4) 0.11911(16) 0.0484(14) Uani 1 1 d . A 1 O9 O 0.2359(3) 0.9906(4) 0.06614(17) 0.0432(13) Uani 1 1 d . A 1 O10 O 0.1867(2) 0.8254(4) 0.07602(15) 0.0356(11) Uani 1 1 d . A 1 O11 O 0.0639(3) 0.7970(4) 0.12507(15) 0.0401(12) Uani 1 1 d . A 1 O12 O -0.0035(2) 0.9244(4) 0.15332(15) 0.0337(11) Uani 1 1 d . A 1 O13 O 0.0625(2) 1.0003(3) 0.06168(13) 0.0233(9) Uani 1 1 d . A 1 O14 O -0.0415(3) 0.8544(4) 0.02988(15) 0.0347(11) Uani 1 1 d . . 1 O15 O 0.0753(3) 0.8760(4) -0.01385(14) 0.0331(11) Uani 1 1 d . . 1 O16 O -0.0840(2) 1.1236(4) 0.08845(14) 0.0346(11) Uani 1 1 d . A 1 O17 O 0.1490(3) 1.1881(4) 0.01020(15) 0.0385(11) Uani 1 1 d . A 1 O18 O 0.0726(3) 0.6635(4) 0.04709(16) 0.0406(12) Uani 1 1 d . A 1 O101 O 0.3661(9) 0.3269(13) 0.3815(4) 0.078(5) Uani 0.50 1 d P B 1 O201 O 0.3624(12) 1.2614(18) 0.1053(8) 0.131(7) Uiso 0.50 1 d P C 1 O202 O 0.3865(17) 1.239(3) 0.0642(12) 0.201(12) Uiso 0.50 1 d P D 2 N1 N 0.1089(5) 0.5047(6) 0.0852(3) 0.063(2) Uani 1 1 d . A 1 N101 N 0.3268(12) 0.456(2) 0.4358(6) 0.096(7) Uani 0.50 1 d P B 1 C1 C 0.3078(3) 0.7733(5) 0.3682(2) 0.0301(15) Uani 1 1 d . A 1 H1A H 0.2840 0.7210 0.3865 0.036 Uiso 1 1 calc R A 1 H1B H 0.3553 0.7916 0.3860 0.036 Uiso 1 1 calc R A 1 C2 C 0.2621(4) 0.8776(6) 0.3612(2) 0.0318(15) Uani 1 1 d . A 1 C3 C 0.1867(4) 0.8656(5) 0.3530(2) 0.0288(14) Uani 1 1 d . A 1 H3 H 0.1669 0.7946 0.3543 0.035 Uiso 1 1 calc R A 1 C4 C 0.1397(3) 0.9539(6) 0.3430(2) 0.0279(14) Uani 1 1 d . A 1 C5 C 0.1686(4) 1.0602(5) 0.3426(2) 0.0284(15) Uani 1 1 d . A 1 C6 C 0.2433(4) 1.0731(6) 0.3523(2) 0.0355(16) Uani 1 1 d . A 1 H6 H 0.2628 1.1447 0.3534 0.043 Uiso 1 1 calc R A 1 C7 C 0.2912(4) 0.9827(6) 0.3607(2) 0.0306(15) Uani 1 1 d . A 1 C8 C 0.3722(4) 1.0072(6) 0.3666(2) 0.0349(16) Uani 1 1 d . A 1 H8A H 0.3818 1.0762 0.3839 0.042 Uiso 1 1 calc R A 1 H8B H 0.3987 0.9483 0.3849 0.042 Uiso 1 1 calc R A 1 C9 C 0.4013(3) 1.0173(6) 0.3216(2) 0.0317(15) Uani 1 1 d . A 1 C10 C 0.3938(4) 1.1188(6) 0.2987(2) 0.0330(15) Uiso 1 1 d . A 1 H10 H 0.3754 1.1790 0.3134 0.040 Uiso 1 1 calc R A 1 C11 C 0.4124(4) 1.1348(5) 0.2551(3) 0.0371(17) Uani 1 1 d . A 1 C12 C 0.4430(3) 1.0455(5) 0.2337(2) 0.0319(15) Uani 1 1 d . A 1 C13 C 0.4530(3) 0.9479(5) 0.2568(2) 0.0318(15) Uani 1 1 d . A 1 H13 H 0.4751 0.8896 0.2431 0.038 Uiso 1 1 calc R A 1 C14 C 0.4318(3) 0.9302(5) 0.3001(2) 0.0306(15) Uani 1 1 d . A 1 C15 C 0.4415(4) 0.8135(5) 0.3210(2) 0.0311(15) Uani 1 1 d . A 1 H15A H 0.4877 0.7827 0.3148 0.037 Uiso 1 1 calc R A 1 H15B H 0.4440 0.8184 0.3546 0.037 Uiso 1 1 calc R A 1 C16 C 0.3808(3) 0.7370(5) 0.3019(2) 0.0285(14) Uani 1 1 d . A 1 C17 C 0.3834(4) 0.6842(5) 0.2591(2) 0.0304(15) Uani 1 1 d . A 1 H17 H 0.4252 0.6937 0.2452 0.036 Uiso 1 1 calc R A 1 C18 C 0.3280(4) 0.6197(5) 0.2369(2) 0.0297(15) Uani 1 1 d . A 1 C19 C 0.2657(4) 0.6014(5) 0.2586(2) 0.0319(16) Uani 1 1 d . A 1 C20 C 0.2637(4) 0.6483(5) 0.3011(2) 0.0294(15) Uiso 1 1 d . A 1 H20 H 0.2237 0.6334 0.3160 0.035 Uiso 1 1 calc R A 1 C21 C 0.3192(4) 0.7174(5) 0.3230(2) 0.0307(15) Uani 1 1 d . A 1 C22 C 0.1454(4) 1.2484(6) 0.3235(2) 0.0329(15) Uani 1 1 d . A 1 H22A H 0.1821 1.2709 0.3496 0.040 Uiso 1 1 calc R A 1 H22B H 0.1055 1.3018 0.3209 0.040 Uiso 1 1 calc R A 1 C23 C 0.1791(3) 1.2522(5) 0.2796(2) 0.0276(14) Uani 1 1 d . A 1 C24 C 0.1413(3) 1.2123(5) 0.2381(2) 0.0247(13) Uani 1 1 d . A 1 H24 H 0.0937 1.1854 0.2368 0.030 Uiso 1 1 calc R A 1 C25 C 0.1744(3) 1.2124(5) 0.1982(2) 0.0275(14) Uani 1 1 d . A 1 C26 C 0.1334(4) 1.1712(5) 0.1533(2) 0.0299(15) Uani 1 1 d . A 1 C27 C 0.2453(4) 1.2482(5) 0.2007(2) 0.0313(15) Uani 1 1 d . A 1 H27 H 0.2676 1.2471 0.1741 0.038 Uiso 1 1 calc R A 1 C29 C 0.2838(3) 1.2856(5) 0.2419(2) 0.0303(15) Uani 1 1 d . A 1 C30 C 0.2496(4) 1.2890(5) 0.2810(2) 0.0328(16) Uani 1 1 d . A 1 H30 H 0.2751 1.3169 0.3088 0.039 Uiso 1 1 calc R A 1 C31 C 0.3623(4) 1.3186(5) 0.2461(3) 0.0400(18) Uani 1 1 d . A 1 H31A H 0.3660 1.3847 0.2275 0.048 Uiso 1 1 calc R A 1 H31B H 0.3806 1.3371 0.2784 0.048 Uiso 1 1 calc R A 1 C32 C 0.4885(4) 0.9798(6) 0.1656(3) 0.0383(17) Uani 1 1 d . A 1 H32A H 0.5285 0.9434 0.1858 0.046 Uiso 1 1 calc R A 1 H32B H 0.5079 1.0102 0.1391 0.046 Uiso 1 1 calc R A 1 C33 C 0.4294(4) 0.8963(6) 0.1490(2) 0.0352(16) Uani 1 1 d . A 1 C34 C 0.3651(4) 0.9309(6) 0.1217(2) 0.0325(15) Uani 1 1 d . A 1 H34 H 0.3594 1.0048 0.1121 0.039 Uiso 1 1 calc R A 1 C35 C 0.3085(4) 0.8538(6) 0.1085(2) 0.0327(16) Uani 1 1 d . A 1 C36 C 0.2384(4) 0.8928(6) 0.0816(2) 0.0341(16) Uani 1 1 d . A 1 C37 C 0.3171(4) 0.7466(6) 0.1239(2) 0.0337(16) Uani 1 1 d . A 1 H37 H 0.2790 0.6960 0.1156 0.040 Uiso 1 1 calc R A 1 C38 C 0.3804(4) 0.7114(5) 0.1515(2) 0.0307(15) Uani 1 1 d . A 1 C39 C 0.4362(4) 0.7858(6) 0.1628(2) 0.0352(16) Uani 1 1 d . A 1 H39 H 0.4800 0.7618 0.1804 0.042 Uiso 1 1 calc R A 1 C40 C 0.3856(4) 0.5930(6) 0.1697(2) 0.0384(17) Uani 1 1 d . A 1 H40A H 0.3839 0.5419 0.1437 0.046 Uiso 1 1 calc R A 1 H40B H 0.4324 0.5829 0.1899 0.046 Uiso 1 1 calc R A 1 C41 C 0.1462(4) 0.5235(6) 0.2528(2) 0.0373(17) Uani 1 1 d . A 1 H41A H 0.1572 0.5009 0.2852 0.045 Uiso 1 1 calc R A 1 H41B H 0.1170 0.4652 0.2358 0.045 Uiso 1 1 calc R A 1 C42 C 0.1027(4) 0.6283(5) 0.2494(2) 0.0337(16) Uani 1 1 d . A 1 C43 C 0.0853(4) 0.6819(5) 0.2068(2) 0.0313(15) Uani 1 1 d . A 1 H43 H 0.0968 0.6478 0.1801 0.038 Uiso 1 1 calc R A 1 C44 C 0.0516(3) 0.7841(5) 0.2031(2) 0.0278(14) Uani 1 1 d . A 1 C45 C 0.0356(3) 0.8392(5) 0.1569(2) 0.0290(15) Uani 1 1 d . A 1 C46 C 0.0340(3) 0.8343(6) 0.2424(2) 0.0284(14) Uani 1 1 d . A 1 H46 H 0.0119 0.9042 0.2400 0.034 Uiso 1 1 calc R A 1 C47 C 0.0487(3) 0.7823(6) 0.2851(2) 0.0310(15) Uani 1 1 d . A 1 C48 C 0.0821(4) 0.6798(5) 0.2883(2) 0.0309(15) Uani 1 1 d . A 1 H48 H 0.0911 0.6440 0.3171 0.037 Uiso 1 1 calc R A 1 C49 C 0.0328(4) 0.8405(6) 0.3285(2) 0.0328(16) Uani 1 1 d . A 1 H49A H -0.0200 0.8476 0.3269 0.039 Uiso 1 1 calc R A 1 H49B H 0.0510 0.7951 0.3555 0.039 Uiso 1 1 calc R A 1 C50 C -0.1043(4) 1.1566(5) 0.0473(2) 0.0312(15) Uani 1 1 d . . 1 C51 C -0.1655(5) 1.2376(8) 0.0380(3) 0.061(3) Uani 1 1 d . E 1 H51A H -0.1823 1.2561 0.0667 0.091 Uiso 1 1 calc R E 1 H51B H -0.2052 1.2053 0.0168 0.091 Uiso 1 1 calc R E 1 H51C H -0.1488 1.3038 0.0244 0.091 Uiso 1 1 calc R E 1 C52 C 0.0974(4) 1.2035(6) -0.0235(2) 0.0343(16) Uani 1 1 d . . 1 C53 C 0.1048(5) 1.2962(8) -0.0563(3) 0.059(2) Uani 1 1 d . F 1 H53A H 0.0613 1.3003 -0.0794 0.089 Uiso 1 1 calc R F 1 H53B H 0.1467 1.2831 -0.0715 0.089 Uiso 1 1 calc R F 1 H53C H 0.1112 1.3651 -0.0394 0.089 Uiso 1 1 calc R F 1 C54 C 0.1140(4) 0.6096(6) 0.0781(3) 0.0454(19) Uani 1 1 d . A 1 H54 H 0.1507 0.6487 0.0972 0.054 Uiso 1 1 calc R A 1 C55 C 0.1590(6) 0.4527(8) 0.1226(4) 0.080(3) Uani 1 1 d . A 1 H55A H 0.1897 0.4004 0.1097 0.120 Uiso 1 1 calc R A 1 H55B H 0.1314 0.4144 0.1432 0.120 Uiso 1 1 calc R A 1 H55C H 0.1891 0.5087 0.1398 0.120 Uiso 1 1 calc R A 1 C56 C 0.0459(9) 0.4381(9) 0.0629(4) 0.116(5) Uani 1 1 d . A 1 H56A H 0.0016 0.4810 0.0615 0.174 Uiso 1 1 calc R A 1 H56B H 0.0420 0.3718 0.0809 0.174 Uiso 1 1 calc R A 1 H56C H 0.0529 0.4180 0.0319 0.174 Uiso 1 1 calc R A 1 C100 C 0.354(2) 0.534(3) 0.4719(9) 0.146(13) Uani 0.50 1 d P B 1 H10D H 0.3138 0.5585 0.4870 0.220 Uiso 0.50 1 calc PR B 1 H10E H 0.3749 0.5969 0.4585 0.220 Uiso 0.50 1 calc PR B 1 H10F H 0.3903 0.4986 0.4943 0.220 Uiso 0.50 1 calc PR B 1 C101 C 0.2562(15) 0.4551(19) 0.4262(9) 0.097(8) Uani 0.50 1 d P B 1 H10A H 0.2360 0.4952 0.4498 0.145 Uiso 0.50 1 calc PR B 1 H10B H 0.2392 0.3795 0.4252 0.145 Uiso 0.50 1 calc PR B 1 H10C H 0.2409 0.4897 0.3964 0.145 Uiso 0.50 1 calc PR B 1 C102 C 0.3653(18) 0.397(3) 0.4021(15) 0.148(15) Uani 0.50 1 d P B 1 H102 H 0.4050 0.4415 0.3973 0.178 Uiso 0.50 1 calc PR B 1 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 Co1 0.0302(5) 0.0252(4) 0.0188(4) 0.0000(3) -0.0002(4) 0.0049(4) Co2 0.0337(5) 0.0285(5) 0.0264(5) -0.0004(4) 0.0080(4) 0.0022(4) Co3 0.0224(4) 0.0281(4) 0.0151(4) 0.0006(3) -0.0005(3) 0.0021(4) Co4 0.0333(7) 0.0266(6) 0.0146(5) -0.0016(4) -0.0011(5) 0.0054(5) O1 0.028(3) 0.045(3) 0.032(2) 0.005(2) 0.005(2) 0.002(2) O2 0.033(3) 0.038(3) 0.030(2) -0.006(2) 0.005(2) 0.007(2) O3 0.036(3) 0.026(3) 0.071(4) 0.016(2) 0.013(3) 0.001(2) O4 0.030(3) 0.036(3) 0.046(3) 0.010(2) 0.006(2) -0.002(2) O5 0.039(3) 0.031(2) 0.037(3) 0.002(2) 0.003(2) 0.003(2) O6 0.038(3) 0.029(2) 0.041(3) 0.000(2) 0.004(2) -0.003(2) O7 0.028(3) 0.049(3) 0.028(2) -0.020(2) -0.003(2) 0.001(2) O8 0.068(4) 0.052(3) 0.028(3) -0.014(2) 0.016(3) -0.022(3) O9 0.034(3) 0.047(3) 0.048(3) 0.020(2) 0.004(2) 0.010(2) O10 0.028(3) 0.040(3) 0.036(3) 0.005(2) -0.005(2) 0.006(2) O11 0.047(3) 0.048(3) 0.024(2) 0.012(2) 0.004(2) 0.011(2) O12 0.035(3) 0.039(3) 0.027(2) 0.0108(19) 0.004(2) 0.006(2) O13 0.026(2) 0.026(2) 0.016(2) -0.0010(16) -0.0043(17) 0.0034(18) O14 0.033(3) 0.033(3) 0.034(3) 0.004(2) -0.006(2) -0.001(2) O15 0.042(3) 0.038(2) 0.019(2) -0.0001(19) 0.005(2) 0.019(2) O16 0.032(3) 0.052(3) 0.018(2) -0.002(2) -0.0025(19) 0.013(2) O17 0.034(3) 0.050(3) 0.030(3) 0.012(2) -0.001(2) -0.004(2) O18 0.052(3) 0.032(2) 0.036(3) 0.001(2) -0.001(2) 0.013(2) O101 0.110(12) 0.082(10) 0.028(6) -0.027(6) -0.028(7) 0.004(9) N1 0.088(6) 0.039(4) 0.056(5) 0.002(3) -0.005(4) 0.010(4) N101 0.087(15) 0.16(2) 0.044(10) -0.013(11) 0.022(10) -0.031(14) C1 0.023(3) 0.037(4) 0.028(4) 0.009(3) -0.001(3) 0.001(3) C2 0.035(4) 0.038(4) 0.021(3) 0.002(3) 0.001(3) 0.000(3) C3 0.035(4) 0.030(3) 0.021(3) 0.005(3) 0.003(3) -0.005(3) C4 0.020(3) 0.044(4) 0.020(3) 0.002(3) 0.004(3) 0.005(3) C5 0.031(4) 0.036(4) 0.018(3) 0.001(3) 0.003(3) 0.007(3) C6 0.036(4) 0.039(4) 0.030(4) 0.002(3) 0.002(3) 0.008(3) C7 0.025(4) 0.041(4) 0.024(3) -0.001(3) -0.003(3) 0.004(3) C8 0.026(4) 0.038(4) 0.037(4) -0.003(3) -0.006(3) -0.001(3) C9 0.017(3) 0.037(4) 0.040(4) -0.002(3) -0.001(3) -0.004(3) C11 0.023(4) 0.026(4) 0.061(5) 0.001(3) -0.001(3) -0.004(3) C12 0.011(3) 0.037(4) 0.046(4) 0.000(3) 0.003(3) -0.004(3) C13 0.014(3) 0.033(4) 0.046(4) -0.002(3) -0.003(3) 0.000(3) C14 0.018(3) 0.032(4) 0.039(4) 0.003(3) -0.003(3) -0.001(3) C15 0.029(4) 0.030(3) 0.032(4) 0.004(3) -0.002(3) 0.003(3) C16 0.024(3) 0.025(3) 0.033(4) 0.009(3) -0.006(3) 0.004(3) C17 0.026(3) 0.027(3) 0.038(4) 0.008(3) 0.003(3) 0.007(3) C18 0.033(4) 0.022(3) 0.034(4) 0.007(3) 0.003(3) 0.007(3) C19 0.038(4) 0.017(3) 0.038(4) 0.008(3) -0.004(3) 0.002(3) C21 0.035(4) 0.024(3) 0.031(4) 0.010(3) -0.002(3) 0.006(3) C22 0.032(4) 0.038(4) 0.027(4) -0.007(3) 0.000(3) 0.010(3) C23 0.025(3) 0.031(3) 0.025(3) -0.005(3) -0.003(3) 0.010(3) C24 0.024(3) 0.024(3) 0.025(3) 0.000(2) 0.001(3) 0.004(3) C25 0.031(4) 0.022(3) 0.029(3) -0.003(3) 0.001(3) -0.001(3) C26 0.040(4) 0.025(3) 0.025(3) -0.005(3) 0.008(3) -0.001(3) C27 0.037(4) 0.023(3) 0.035(4) 0.001(3) 0.009(3) -0.003(3) C29 0.030(4) 0.019(3) 0.040(4) 0.002(3) 0.000(3) 0.002(3) C30 0.030(4) 0.031(3) 0.033(4) -0.007(3) -0.011(3) 0.003(3) C31 0.033(4) 0.024(4) 0.060(5) -0.005(3) 0.001(3) 0.002(3) C32 0.025(4) 0.044(4) 0.047(4) 0.007(3) 0.006(3) 0.002(3) C33 0.026(4) 0.044(4) 0.036(4) 0.005(3) 0.006(3) 0.007(3) C34 0.025(4) 0.035(4) 0.038(4) 0.009(3) 0.006(3) 0.007(3) C35 0.026(4) 0.044(4) 0.027(3) 0.009(3) 0.003(3) 0.012(3) C36 0.031(4) 0.040(4) 0.032(4) 0.005(3) 0.008(3) 0.006(3) C37 0.028(4) 0.035(4) 0.039(4) 0.003(3) 0.007(3) 0.004(3) C38 0.029(4) 0.034(4) 0.028(3) 0.003(3) 0.002(3) 0.010(3) C39 0.025(4) 0.045(4) 0.036(4) 0.008(3) 0.003(3) 0.010(3) C40 0.042(4) 0.041(4) 0.032(4) 0.003(3) 0.005(3) 0.014(3) C41 0.040(4) 0.034(4) 0.037(4) 0.008(3) 0.003(3) -0.009(3) C42 0.034(4) 0.028(3) 0.037(4) 0.011(3) 0.002(3) -0.010(3) C43 0.032(4) 0.036(4) 0.025(3) 0.006(3) 0.002(3) -0.006(3) C44 0.024(3) 0.036(4) 0.022(3) 0.009(3) 0.001(3) -0.003(3) C45 0.027(3) 0.037(4) 0.022(3) 0.006(3) 0.001(3) 0.000(3) C46 0.018(3) 0.040(4) 0.025(3) 0.008(3) -0.003(3) 0.002(3) C47 0.021(3) 0.047(4) 0.025(3) 0.009(3) 0.004(3) -0.001(3) C48 0.032(4) 0.036(4) 0.025(3) 0.010(3) 0.004(3) -0.007(3) C49 0.026(4) 0.047(4) 0.025(3) 0.010(3) 0.003(3) 0.000(3) C50 0.033(4) 0.038(4) 0.020(3) -0.004(3) -0.003(3) 0.011(3) C51 0.064(5) 0.082(6) 0.036(4) 0.004(4) 0.006(4) 0.047(5) C52 0.033(4) 0.041(4) 0.031(4) 0.005(3) 0.010(3) 0.000(3) C53 0.050(5) 0.074(6) 0.051(5) 0.030(5) 0.001(4) -0.008(5) C54 0.049(5) 0.037(4) 0.049(5) 0.005(4) 0.003(4) 0.006(4) C55 0.101(8) 0.053(5) 0.081(7) 0.019(5) -0.002(6) 0.026(6) C56 0.188(15) 0.068(7) 0.071(8) 0.010(6) -0.041(9) -0.008(8) C100 0.20(4) 0.18(3) 0.055(16) -0.054(18) 0.020(18) 0.00(3) C101 0.11(2) 0.083(16) 0.088(17) 0.003(13) -0.005(15) -0.047(15) C102 0.11(2) 0.18(4) 0.17(4) 0.08(3) 0.06(3) -0.05(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 Co1 O13 2.057(4) . ? Co1 O11 2.076(5) . ? Co1 O10 2.083(5) . ? Co1 O18 2.116(5) . ? Co1 O15 2.195(4) . ? Co1 O14 2.236(5) . ? Co1 Co4 2.8878(8) . ? Co2 O13 1.930(4) . ? Co2 O8 1.972(5) . ? Co2 O9 1.976(5) . ? Co2 O17 1.997(4) . ? Co3 O13 1.930(4) . ? Co3 O12 1.984(4) . ? Co3 O7 1.992(4) . ? Co3 O16 2.013(4) . ? Co4 O13 2.010(4) . ? Co4 O13 2.010(4) 3_575 ? Co4 O15 2.161(4) 3_575 ? Co4 O15 2.161(4) . ? Co4 O14 2.190(5) . ? Co4 O14 2.190(5) 3_575 ? Co4 Co1 2.8878(8) 3_575 ? O1 C4 1.388(8) . ? O1 C49 1.444(8) . ? O2 C5 1.390(8) . ? O2 C22 1.422(8) . ? O3 C11 1.385(8) . ? O3 C31 1.462(8) . ? O4 C12 1.388(8) . ? O4 C32 1.470(9) . ? O5 C18 1.399(8) . ? O5 C40 1.443(9) . ? O6 C19 1.389(8) . ? O6 C41 1.440(8) . ? O7 C26 1.269(8) . ? O8 C26 1.288(8) . ? O9 C36 1.281(8) . ? O10 C36 1.268(8) . ? O11 C45 1.263(8) . ? O12 C45 1.272(8) . ? O14 C52 1.258(8) 3_575 ? O15 C50 1.269(8) 3_575 ? O16 C50 1.282(8) . ? O17 C52 1.292(8) . ? O18 C54 1.289(9) . ? O101 C102 1.06(5) . ? N1 C54 1.308(10) . ? N1 C55 1.481(12) . ? N1 C56 1.505(14) . ? N101 C101 1.31(3) . ? N101 C100 1.46(3) . ? N101 C102 1.51(5) . ? C1 C2 1.536(9) . ? C1 C21 1.548(9) . ? C2 C7 1.400(10) . ? C2 C3 1.409(9) . ? C3 C4 1.400(9) . ? C4 C5 1.412(9) . ? C5 C6 1.399(10) . ? C6 C7 1.425(10) . ? C7 C8 1.537(9) . ? C8 C9 1.520(10) . ? C9 C14 1.411(10) . ? C9 C10 1.415(10) . ? C10 C11 1.403(10) . ? C11 C12 1.429(10) . ? C12 C13 1.376(9) . ? C13 C14 1.419(10) . ? C14 C15 1.558(9) . ? C15 C16 1.517(9) . ? C16 C21 1.422(9) . ? C16 C17 1.430(9) . ? C17 C18 1.388(9) . ? C18 C19 1.440(10) . ? C19 C20 1.389(9) . ? C20 C21 1.420(9) . ? C22 C23 1.535(9) . ? C23 C30 1.395(9) . ? C23 C24 1.407(8) . ? C24 C25 1.421(9) . ? C25 C27 1.395(9) . ? C25 C26 1.515(9) . ? C27 C29 1.394(9) . ? C29 C30 1.410(10) . ? C29 C31 1.517(9) . ? C32 C33 1.535(10) . ? C33 C34 1.412(9) . ? C33 C39 1.414(10) . ? C34 C35 1.431(10) . ? C35 C37 1.392(10) . ? C35 C36 1.505(9) . ? C37 C38 1.401(9) . ? C38 C39 1.391(10) . ? C38 C40 1.546(9) . ? C41 C42 1.518(10) . ? C42 C43 1.414(9) . ? C42 C48 1.420(10) . ? C43 C44 1.400(9) . ? C44 C46 1.400(9) . ? C44 C45 1.515(9) . ? C46 C47 1.406(9) . ? C47 C48 1.401(10) . ? C47 C49 1.540(10) . ? C50 O15 1.269(8) 3_575 ? C50 C51 1.514(9) . ? C52 O14 1.258(8) 3_575 ? C52 C53 1.517(10) . ? 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 O13 Co1 O11 97.98(18) . . ? O13 Co1 O10 99.11(17) . . ? O11 Co1 O10 89.87(19) . . ? O13 Co1 O18 170.78(18) . . ? O11 Co1 O18 85.9(2) . . ? O10 Co1 O18 89.22(19) . . ? O13 Co1 O15 80.50(16) . . ? O11 Co1 O15 174.16(19) . . ? O10 Co1 O15 95.93(18) . . ? O18 Co1 O15 94.80(18) . . ? O13 Co1 O14 78.07(16) . . ? O11 Co1 O14 98.04(19) . . ? O10 Co1 O14 171.89(18) . . ? O18 Co1 O14 93.13(18) . . ? O15 Co1 O14 76.15(17) . . ? O13 Co1 Co4 44.11(10) . . ? O11 Co1 Co4 127.55(14) . . ? O10 Co1 Co4 124.47(13) . . ? O18 Co1 Co4 127.31(13) . . ? O15 Co1 Co4 47.96(11) . . ? O14 Co1 Co4 48.58(12) . . ? O13 Co2 O8 108.8(2) . . ? O13 Co2 O9 112.43(19) . . ? O8 Co2 O9 103.0(2) . . ? O13 Co2 O17 115.68(18) . . ? O8 Co2 O17 107.3(2) . . ? O9 Co2 O17 108.7(2) . . ? O13 Co3 O12 114.52(18) . . ? O13 Co3 O7 108.63(18) . . ? O12 Co3 O7 97.6(2) . . ? O13 Co3 O16 116.08(17) . . ? O12 Co3 O16 112.4(2) . . ? O7 Co3 O16 105.40(19) . . ? O13 Co4 O13 180.0 . 3_575 ? O13 Co4 O15 97.62(16) . 3_575 ? O13 Co4 O15 82.38(16) 3_575 3_575 ? O13 Co4 O15 82.38(16) . . ? O13 Co4 O15 97.62(16) 3_575 . ? O15 Co4 O15 180.0(2) 3_575 . ? O13 Co4 O14 80.14(16) . . ? O13 Co4 O14 99.86(16) 3_575 . ? O15 Co4 O14 102.17(18) 3_575 . ? O15 Co4 O14 77.83(17) . . ? O13 Co4 O14 99.86(16) . 3_575 ? O13 Co4 O14 80.14(16) 3_575 3_575 ? O15 Co4 O14 77.83(17) 3_575 3_575 ? O15 Co4 O14 102.17(17) . 3_575 ? O14 Co4 O14 180.0(2) . 3_575 ? O13 Co4 Co1 45.41(11) . . ? O13 Co4 Co1 134.59(11) 3_575 . ? O15 Co4 Co1 131.01(11) 3_575 . ? O15 Co4 Co1 48.99(11) . . ? O14 Co4 Co1 49.97(12) . . ? O14 Co4 Co1 130.03(12) 3_575 . ? O13 Co4 Co1 134.59(11) . 3_575 ? O13 Co4 Co1 45.41(11) 3_575 3_575 ? O15 Co4 Co1 48.99(11) 3_575 3_575 ? O15 Co4 Co1 131.01(11) . 3_575 ? O14 Co4 Co1 130.03(12) . 3_575 ? O14 Co4 Co1 49.97(12) 3_575 3_575 ? Co1 Co4 Co1 180.0 . 3_575 ? C4 O1 C49 117.9(5) . . ? C5 O2 C22 117.0(5) . . ? C11 O3 C31 118.0(6) . . ? C12 O4 C32 117.9(5) . . ? C18 O5 C40 117.9(5) . . ? C19 O6 C41 117.9(5) . . ? C26 O7 Co3 129.4(4) . . ? C26 O8 Co2 129.7(4) . . ? C36 O9 Co2 123.2(4) . . ? C36 O10 Co1 136.2(4) . . ? C45 O11 Co1 137.8(4) . . ? C45 O12 Co3 121.8(4) . . ? Co3 O13 Co2 113.55(19) . . ? Co3 O13 Co4 111.21(19) . . ? Co2 O13 Co4 112.37(19) . . ? Co3 O13 Co1 112.21(19) . . ? Co2 O13 Co1 114.92(19) . . ? Co4 O13 Co1 90.48(15) . . ? C52 O14 Co4 137.9(4) 3_575 . ? C52 O14 Co1 137.8(4) 3_575 . ? Co4 O14 Co1 81.44(16) . . ? C50 O15 Co4 138.1(4) 3_575 . ? C50 O15 Co1 138.8(4) 3_575 . ? Co4 O15 Co1 83.05(15) . . ? C50 O16 Co3 123.9(4) . . ? C52 O17 Co2 126.9(4) . . ? C54 O18 Co1 113.5(5) . . ? C54 N1 C55 119.3(8) . . ? C54 N1 C56 122.4(8) . . ? C55 N1 C56 117.3(8) . . ? C101 N101 C100 113(2) . . ? C101 N101 C102 115(2) . . ? C100 N101 C102 131(3) . . ? C2 C1 C21 113.7(5) . . ? C7 C2 C3 118.6(6) . . ? C7 C2 C1 123.8(6) . . ? C3 C2 C1 117.5(6) . . ? C4 C3 C2 122.7(6) . . ? O1 C4 C3 125.5(6) . . ? O1 C4 C5 115.5(6) . . ? C3 C4 C5 119.0(6) . . ? O2 C5 C6 125.8(6) . . ? O2 C5 C4 115.7(6) . . ? C6 C5 C4 118.5(6) . . ? C5 C6 C7 122.4(7) . . ? C2 C7 C6 118.7(6) . . ? C2 C7 C8 124.1(6) . . ? C6 C7 C8 117.1(6) . . ? C9 C8 C7 113.8(5) . . ? C14 C9 C10 117.7(6) . . ? C14 C9 C8 124.2(6) . . ? C10 C9 C8 118.0(6) . . ? C11 C10 C9 123.0(6) . . ? O3 C11 C10 125.5(6) . . ? O3 C11 C12 115.9(7) . . ? C10 C11 C12 118.5(6) . . ? C13 C12 O4 126.9(6) . . ? C13 C12 C11 118.6(7) . . ? O4 C12 C11 114.5(6) . . ? C12 C13 C14 123.1(6) . . ? C9 C14 C13 119.0(6) . . ? C9 C14 C15 123.1(6) . . ? C13 C14 C15 117.9(6) . . ? C16 C15 C14 112.6(5) . . ? C21 C16 C17 117.3(6) . . ? C21 C16 C15 123.9(6) . . ? C17 C16 C15 118.8(6) . . ? C18 C17 C16 123.3(6) . . ? C17 C18 O5 125.1(6) . . ? C17 C18 C19 118.8(6) . . ? O5 C18 C19 116.1(6) . . ? C20 C19 O6 125.6(6) . . ? C20 C19 C18 118.6(6) . . ? O6 C19 C18 115.8(6) . . ? C19 C20 C21 122.7(6) . . ? C20 C21 C16 119.3(6) . . ? C20 C21 C1 117.9(6) . . ? C16 C21 C1 122.7(6) . . ? O2 C22 C23 113.8(5) . . ? C30 C23 C24 119.0(6) . . ? C30 C23 C22 120.2(6) . . ? C24 C23 C22 120.7(6) . . ? C23 C24 C25 119.9(6) . . ? C27 C25 C24 119.7(6) . . ? C27 C25 C26 120.1(6) . . ? C24 C25 C26 120.1(6) . . ? O7 C26 O8 125.7(6) . . ? O7 C26 C25 117.9(6) . . ? O8 C26 C25 116.5(6) . . ? C29 C27 C25 120.7(6) . . ? C27 C29 C30 119.1(6) . . ? C27 C29 C31 121.6(6) . . ? C30 C29 C31 119.3(6) . . ? C23 C30 C29 121.4(6) . . ? O3 C31 C29 112.5(5) . . ? O4 C32 C33 110.4(5) . . ? C34 C33 C39 118.9(6) . . ? C34 C33 C32 119.7(6) . . ? C39 C33 C32 121.3(6) . . ? C33 C34 C35 119.4(6) . . ? C37 C35 C34 119.4(6) . . ? C37 C35 C36 121.3(6) . . ? C34 C35 C36 119.0(6) . . ? O10 C36 O9 125.3(6) . . ? O10 C36 C35 116.8(6) . . ? O9 C36 C35 117.8(6) . . ? C35 C37 C38 121.7(7) . . ? C39 C38 C37 118.6(6) . . ? C39 C38 C40 121.8(6) . . ? C37 C38 C40 119.6(6) . . ? C38 C39 C33 121.9(6) . . ? O5 C40 C38 111.7(5) . . ? O6 C41 C42 112.2(5) . . ? C43 C42 C48 117.5(6) . . ? C43 C42 C41 119.9(6) . . ? C48 C42 C41 122.5(6) . . ? C44 C43 C42 121.6(6) . . ? C46 C44 C43 119.4(6) . . ? C46 C44 C45 121.0(6) . . ? C43 C44 C45 119.5(6) . . ? O11 C45 O12 125.5(6) . . ? O11 C45 C44 116.4(6) . . ? O12 C45 C44 118.0(6) . . ? C44 C46 C47 120.7(6) . . ? C48 C47 C46 119.2(6) . . ? C48 C47 C49 120.2(6) . . ? C46 C47 C49 120.4(6) . . ? C47 C48 C42 121.4(6) . . ? O1 C49 C47 112.9(5) . . ? O15 C50 O16 122.9(6) 3_575 . ? O15 C50 C51 118.2(6) 3_575 . ? O16 C50 C51 119.0(6) . . ? O14 C52 O17 122.8(6) 3_575 . ? O14 C52 C53 119.1(6) 3_575 . ? O17 C52 C53 118.1(6) . . ? O18 C54 N1 124.5(8) . . ? O101 C102 N101 146(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.484 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.166