# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Cheng-Yong Su' _publ_contact_author_address ; 135 Xingang West Road Guangzhou 510275 ; _publ_contact_author_email cesscy@mail.sysu.edu.cn _publ_author_name 'Cheng-Yong Su' # Attachment '- Compds.cif' data_1-BF4 _database_code_depnum_ccdc_archive 'CCDC 812762' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H192 B6 Cu6 F24 N42 O42' _chemical_formula_weight 4229.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 27.3936(2) _cell_length_b 27.3936(2) _cell_length_c 27.3936(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20556.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3948 _cell_measurement_theta_min 2.7934 _cell_measurement_theta_max 63.9226 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8712 _exptl_absorpt_coefficient_mu 1.541 _exptl_absorpt_correction_T_min 0.7906 _exptl_absorpt_correction_T_max 0.8866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type '\Gemini S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15467 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 63.94 _reflns_number_total 5623 _reflns_number_gt 3148 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _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. The BF~4~^-^ anion is disordered with F atoms occupying two sets of positions, SADI was used to model the molecule which results in 12 restraints. There are a large amount of free water molecules in the crystal cavity which are distributed over partial sites. SIMU and ISOR were used to refine disordered water molecules which causes 96+126 restraints. The total restraints are 234. ; _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^)+(0.0910P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5623 _refine_ls_number_parameters 502 _refine_ls_number_restraints 234 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1833 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.647715(18) -0.090656(18) 0.846063(18) 0.03510(12) Uani 1 1 d . . . N1 N 0.68957(11) -0.03402(11) 0.81353(11) 0.0390(8) Uani 1 1 d . . . N2 N 0.69407(11) -0.07516(11) 0.90276(11) 0.0406(8) Uani 1 1 d . . . N3 N 0.74521(12) -0.02066(13) 0.93506(12) 0.0514(9) Uani 1 1 d . . . H3A H 0.7633 0.0058 0.9376 0.062 Uiso 1 1 calc R . . N4 N 0.66865(11) -0.12397(11) 0.78278(10) 0.0384(8) Uani 1 1 d . . . N5 N 0.71879(11) -0.12202(12) 0.71954(11) 0.0451(8) Uani 1 1 d . . . H5B H 0.7424 -0.1122 0.7001 0.054 Uiso 1 1 calc R . . N6 N 0.59302(10) -0.03735(10) 0.83537(10) 0.0350(7) Uani 1 1 d . . . N7 N 0.57745(11) 0.03658(11) 0.80453(11) 0.0386(8) Uani 1 1 d . . . C1 C 0.70961(14) -0.00259(14) 0.85291(13) 0.0427(10) Uani 1 1 d . . . H1A H 0.7408 0.0122 0.8423 0.051 Uiso 1 1 calc R . . H1B H 0.6864 0.0241 0.8604 0.051 Uiso 1 1 calc R . . C2 C 0.71758(14) -0.03298(15) 0.89675(14) 0.0444(10) Uani 1 1 d . . . C3 C 0.70777(14) -0.09128(15) 0.94957(14) 0.0446(10) Uani 1 1 d . . . C4 C 0.69454(17) -0.13217(16) 0.97600(15) 0.0571(12) Uani 1 1 d . . . H4A H 0.6729 -0.1559 0.9628 0.069 Uiso 1 1 calc R . . C5 C 0.7141(2) -0.13733(18) 1.02265(17) 0.0688(14) Uani 1 1 d . . . H5A H 0.7055 -0.1651 1.0416 0.083 Uiso 1 1 calc R . . C6 C 0.7458(2) -0.1029(2) 1.04231(17) 0.0745(15) Uani 1 1 d . . . H6A H 0.7585 -0.1075 1.0742 0.089 Uiso 1 1 calc R . . C7 C 0.75894(18) -0.06254(19) 1.01613(17) 0.0666(14) Uani 1 1 d . . . H7A H 0.7805 -0.0390 1.0297 0.080 Uiso 1 1 calc R . . C8 C 0.74037(15) -0.05651(16) 0.96968(15) 0.0497(11) Uani 1 1 d . . . C9 C 0.72865(14) -0.05859(14) 0.78475(14) 0.0441(10) Uani 1 1 d . . . H9A H 0.7418 -0.0362 0.7596 0.053 Uiso 1 1 calc R . . H9B H 0.7557 -0.0689 0.8064 0.053 Uiso 1 1 calc R . . C10 C 0.70550(13) -0.10128(14) 0.76175(13) 0.0422(10) Uani 1 1 d . . . C11 C 0.65684(13) -0.16315(13) 0.75230(13) 0.0382(9) Uani 1 1 d . . . C12 C 0.62165(14) -0.19926(14) 0.75633(14) 0.0459(10) Uani 1 1 d . . . H12A H 0.6000 -0.2002 0.7834 0.055 Uiso 1 1 calc R . . C13 C 0.61888(16) -0.23406(16) 0.71964(16) 0.0545(12) Uani 1 1 d . . . H13A H 0.5954 -0.2595 0.7214 0.065 Uiso 1 1 calc R . . C14 C 0.65146(17) -0.23143(17) 0.67934(16) 0.0629(13) Uani 1 1 d . . . H14A H 0.6490 -0.2553 0.6543 0.075 Uiso 1 1 calc R . . C15 C 0.68564(16) -0.19644(17) 0.67534(15) 0.0544(12) Uani 1 1 d . . . H15A H 0.7072 -0.1953 0.6482 0.065 Uiso 1 1 calc R . . C16 C 0.68814(14) -0.16245(15) 0.71210(14) 0.0460(10) Uani 1 1 d . . . C17 C 0.65693(14) -0.00578(14) 0.78156(14) 0.0428(10) Uani 1 1 d . . . H17A H 0.6525 -0.0227 0.7499 0.051 Uiso 1 1 calc R . . H17B H 0.6707 0.0270 0.7753 0.051 Uiso 1 1 calc R . . C18 C 0.60910(13) -0.00161(13) 0.80774(13) 0.0366(9) Uani 1 1 d . . . C19 C 0.54774(12) -0.02207(12) 0.85291(12) 0.0323(8) Uani 1 1 d . . . C20 C 0.51520(13) -0.04437(13) 0.88413(13) 0.0375(9) Uani 1 1 d . . . H20A H 0.5219 -0.0755 0.8978 0.045 Uiso 1 1 calc R . . C21 C 0.47219(14) -0.01970(14) 0.89500(14) 0.0432(10) Uani 1 1 d . . . H21A H 0.4489 -0.0345 0.9160 0.052 Uiso 1 1 calc R . . C22 C 0.46252(15) 0.02652(14) 0.87560(15) 0.0487(11) Uani 1 1 d . . . H22A H 0.4328 0.0425 0.8837 0.058 Uiso 1 1 calc R . . C23 C 0.49520(14) 0.04944(13) 0.84497(14) 0.0442(10) Uani 1 1 d . . . H23A H 0.4888 0.0810 0.8321 0.053 Uiso 1 1 calc R . . C24 C 0.53768(13) 0.02460(13) 0.83383(13) 0.0375(9) Uani 1 1 d . . . C25 C 0.58762(15) 0.08496(13) 0.78393(13) 0.0428(10) Uani 1 1 d . . . H25A H 0.5563 0.0999 0.7738 0.051 Uiso 1 1 calc R . . H25B H 0.6078 0.0808 0.7542 0.051 Uiso 1 1 calc R . . C26 C 0.61381(13) 0.12024(12) 0.81823(13) 0.0368(9) Uani 1 1 d . . . O1 O 0.62529(8) 0.10424(8) 0.86022(8) 0.0351(6) Uani 1 1 d . . . O2 O 0.62035(10) 0.16221(9) 0.80250(10) 0.0471(7) Uani 1 1 d . . . B1 B 1.02511(18) 0.65987(18) 0.71982(19) 0.0803(12) Uani 1 1 d DU A 1 F1 F 1.04568(19) 0.70460(17) 0.7189(2) 0.0844(14) Uani 0.60 1 d PDU A 1 F2 F 0.97742(18) 0.6644(2) 0.7016(2) 0.0934(15) Uani 0.60 1 d PDU A 1 F3 F 1.0265(2) 0.63754(19) 0.76278(19) 0.0911(15) Uani 0.60 1 d PDU A 1 F4 F 1.0493(2) 0.6300(2) 0.6850(2) 0.0935(15) Uani 0.60 1 d PDU A 1 F1' F 0.9836(3) 0.6814(3) 0.7377(4) 0.106(2) Uani 0.40 1 d PDU B 2 F2' F 1.0166(3) 0.6164(3) 0.6987(3) 0.0996(19) Uani 0.40 1 d PDU C 2 F3' F 1.0537(3) 0.6498(3) 0.7631(3) 0.0860(19) Uani 0.40 1 d PDU D 2 F4' F 1.0524(3) 0.6896(3) 0.6908(3) 0.0854(18) Uani 0.40 1 d PDU E 2 O4W O 1.1342(4) 0.5761(3) 0.6278(3) 0.107(3) Uani 0.50 1 d PU F 1 O5W O 0.9084(3) 0.5286(3) 0.6787(3) 0.105(3) Uani 0.50 1 d PU G 1 O6W O 0.8340(3) -0.0159(4) 0.8394(4) 0.075(3) Uani 0.33 1 d PU H 1 O7W O 1.0361(5) 0.5481(6) 0.5861(5) 0.120(4) Uani 0.33 1 d PU I 1 O8W O 0.7820(2) -0.2180(2) 0.7820(2) 0.137(3) Uani 1 3 d SU J 1 O9W O 1.0454(5) 0.4546(5) 0.5454(5) 0.167(6) Uani 0.50 3 d SPU K 1 O10W O 0.8251(7) -0.1037(7) 0.8981(7) 0.064(3) Uani 0.17 1 d PU L 1 O11W O 0.8301(6) -0.0963(6) 0.8460(7) 0.059(3) Uani 0.17 1 d PU M 2 O12W O 0.9694(5) 0.5538(5) 0.6418(5) 0.180(4) Uani 0.50 1 d PU N 2 O2W O 0.9392(3) 0.4607(3) 0.7014(3) 0.091(2) Uani 0.50 1 d PU O 2 O3W O 0.9303(3) 0.4337(3) 0.7068(3) 0.081(2) Uani 0.50 1 d PU O 2 O1W O 0.6355(2) 0.26020(16) 0.83044(17) 0.1210(17) Uani 1 1 d U . . 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 0.0348(2) 0.0355(2) 0.0350(3) 0.0019(2) 0.0038(2) -0.0001(2) N1 0.0372(15) 0.0405(15) 0.0394(15) 0.0020(14) 0.0052(14) -0.0004(14) N2 0.0367(15) 0.0450(16) 0.0401(16) -0.0010(14) -0.0015(14) 0.0006(14) N3 0.0469(18) 0.056(2) 0.0516(19) -0.0112(17) -0.0126(16) -0.0034(17) N4 0.0374(15) 0.0429(16) 0.0351(15) -0.0015(14) 0.0051(13) 0.0003(14) N5 0.0383(16) 0.0577(19) 0.0393(16) -0.0004(15) 0.0118(14) 0.0063(15) N6 0.0376(14) 0.0334(14) 0.0341(14) 0.0033(12) -0.0011(13) 0.0004(13) N7 0.0446(16) 0.0349(15) 0.0364(15) 0.0056(13) 0.0018(14) 0.0001(14) C1 0.045(2) 0.0402(19) 0.043(2) -0.0016(17) 0.0029(18) -0.0056(17) C2 0.0405(19) 0.050(2) 0.043(2) -0.0023(18) 0.0012(17) 0.0056(18) C3 0.047(2) 0.048(2) 0.0393(19) -0.0005(18) -0.0056(17) 0.0062(19) C4 0.066(3) 0.058(2) 0.047(2) 0.005(2) -0.013(2) 0.000(2) C5 0.093(3) 0.064(3) 0.050(2) 0.007(2) -0.017(3) 0.007(3) C6 0.088(3) 0.089(4) 0.047(2) 0.004(3) -0.031(2) 0.009(3) C7 0.065(3) 0.076(3) 0.059(3) -0.009(2) -0.024(2) 0.004(3) C8 0.047(2) 0.056(2) 0.047(2) -0.004(2) -0.0077(19) 0.000(2) C9 0.0368(19) 0.048(2) 0.048(2) -0.0013(18) 0.0106(17) -0.0026(17) C10 0.0377(18) 0.051(2) 0.0382(19) -0.0016(17) 0.0053(17) 0.0068(17) C11 0.0370(17) 0.0433(19) 0.0342(17) 0.0008(16) 0.0005(15) 0.0056(16) C12 0.044(2) 0.051(2) 0.043(2) -0.0082(18) -0.0012(18) 0.0043(19) C13 0.053(2) 0.050(2) 0.060(2) -0.010(2) -0.012(2) 0.000(2) C14 0.067(3) 0.069(3) 0.052(2) -0.027(2) -0.013(2) 0.016(2) C15 0.053(2) 0.069(3) 0.041(2) -0.009(2) 0.0058(19) 0.007(2) C16 0.0423(19) 0.055(2) 0.0408(19) -0.0072(18) 0.0006(18) 0.0107(18) C17 0.047(2) 0.0405(19) 0.0404(19) 0.0059(17) 0.0055(18) -0.0043(18) C18 0.0397(18) 0.0358(17) 0.0342(18) 0.0036(16) -0.0006(16) -0.0013(16) C19 0.0323(16) 0.0320(16) 0.0327(17) -0.0028(15) -0.0049(15) -0.0017(14) C20 0.0394(18) 0.0328(17) 0.0404(19) 0.0012(16) -0.0011(16) -0.0065(16) C21 0.0399(19) 0.046(2) 0.043(2) -0.0010(18) 0.0068(17) -0.0047(17) C22 0.044(2) 0.044(2) 0.058(2) -0.0091(19) 0.0004(19) 0.0071(18) C23 0.047(2) 0.0344(18) 0.051(2) 0.0061(18) -0.0031(19) 0.0040(17) C24 0.0380(18) 0.0339(17) 0.0407(19) 0.0006(16) -0.0060(16) -0.0027(15) C25 0.052(2) 0.0424(19) 0.0339(18) 0.0079(16) -0.0058(18) -0.0011(19) C26 0.0414(18) 0.0325(17) 0.0364(18) 0.0015(15) -0.0008(16) 0.0021(16) O1 0.0396(12) 0.0318(11) 0.0340(12) 0.0020(10) -0.0089(11) -0.0034(10) O2 0.0568(15) 0.0388(13) 0.0456(14) 0.0074(12) -0.0023(13) -0.0021(12) B1 0.076(2) 0.070(2) 0.095(2) 0.016(2) 0.005(2) 0.005(2) F1 0.088(3) 0.064(2) 0.101(3) 0.025(2) -0.017(2) -0.005(2) F2 0.069(2) 0.094(3) 0.118(3) -0.001(3) -0.003(2) -0.003(2) F3 0.105(3) 0.085(3) 0.083(3) 0.025(2) 0.015(3) 0.005(3) F4 0.092(3) 0.095(3) 0.094(3) -0.001(2) 0.007(2) 0.022(2) F1' 0.088(4) 0.104(4) 0.125(4) 0.011(4) 0.016(4) 0.014(3) F2' 0.096(3) 0.089(3) 0.114(3) -0.002(3) -0.012(3) -0.001(3) F3' 0.090(4) 0.079(3) 0.088(3) 0.016(3) 0.008(3) 0.003(3) F4' 0.075(3) 0.082(3) 0.099(3) 0.022(3) 0.009(3) 0.004(3) O4W 0.131(5) 0.093(5) 0.098(5) -0.029(4) 0.030(4) -0.028(4) O5W 0.109(5) 0.108(5) 0.097(5) -0.005(4) -0.011(4) 0.016(4) O6W 0.046(4) 0.113(6) 0.066(5) -0.009(5) 0.006(4) -0.025(4) O7W 0.109(7) 0.127(7) 0.124(7) 0.005(6) -0.007(6) 0.025(6) O8W 0.137(3) 0.137(3) 0.137(3) 0.019(3) 0.019(3) 0.019(3) O9W 0.167(6) 0.167(6) 0.167(6) 0.008(4) -0.008(4) 0.008(4) O10W 0.059(5) 0.063(5) 0.071(5) -0.014(5) 0.000(5) 0.000(5) O11W 0.056(5) 0.055(5) 0.065(5) -0.003(5) -0.012(5) -0.001(5) O12W 0.169(7) 0.198(7) 0.174(7) 0.030(6) -0.082(6) -0.031(6) O2W 0.077(4) 0.112(4) 0.084(4) 0.011(4) -0.008(3) 0.010(4) O3W 0.070(4) 0.088(4) 0.083(4) 0.020(4) -0.010(3) -0.001(3) O1W 0.193(4) 0.078(2) 0.093(3) 0.000(2) 0.000(3) -0.029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.961(2) 24_647 ? Cu1 N4 2.041(3) . ? Cu1 N2 2.051(3) . ? Cu1 N6 2.112(3) . ? Cu1 N1 2.125(3) . ? N1 C17 1.472(5) . ? N1 C1 1.486(5) . ? N1 C9 1.490(5) . ? N2 C2 1.333(5) . ? N2 C3 1.407(5) . ? N3 C2 1.337(5) . ? N3 C8 1.372(5) . ? N3 H3A 0.8800 . ? N4 C10 1.318(5) . ? N4 C11 1.398(5) . ? N5 C10 1.339(5) . ? N5 C16 1.405(5) . ? N5 H5B 0.8800 . ? N6 C18 1.314(4) . ? N6 C19 1.394(4) . ? N7 C18 1.362(5) . ? N7 C24 1.392(5) . ? N7 C25 1.467(5) . ? C1 C2 1.477(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.382(6) . ? C3 C8 1.417(6) . ? C4 C5 1.393(6) . ? C4 H4A 0.9500 . ? C5 C6 1.392(7) . ? C5 H5A 0.9500 . ? C6 C7 1.366(7) . ? C6 H6A 0.9500 . ? C7 C8 1.380(6) . ? C7 H7A 0.9500 . ? C9 C10 1.472(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.386(5) . ? C11 C16 1.396(5) . ? C12 C13 1.387(6) . ? C12 H12A 0.9500 . ? C13 C14 1.422(6) . ? C13 H13A 0.9500 . ? C14 C15 1.344(6) . ? C14 H14A 0.9500 . ? C15 C16 1.373(6) . ? C15 H15A 0.9500 . ? C17 C18 1.498(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.378(5) . ? C19 C24 1.409(5) . ? C20 C21 1.391(5) . ? C20 H20A 0.9500 . ? C21 C22 1.399(5) . ? C21 H21A 0.9500 . ? C22 C23 1.378(6) . ? C22 H22A 0.9500 . ? C23 C24 1.382(5) . ? C23 H23A 0.9500 . ? C25 C26 1.527(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O2 1.241(4) . ? C26 O1 1.270(4) . ? O1 Cu1 1.961(2) 18_756 ? B1 F3 1.327(7) . ? B1 F1 1.349(6) . ? B1 F2 1.404(7) . ? B1 F4 1.421(7) . ? O2W O3W 0.793(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N4 101.75(11) 24_647 . ? O1 Cu1 N2 102.42(11) 24_647 . ? N4 Cu1 N2 124.18(12) . . ? O1 Cu1 N6 95.69(10) 24_647 . ? N4 Cu1 N6 112.99(11) . . ? N2 Cu1 N6 113.65(12) . . ? O1 Cu1 N1 175.25(11) 24_647 . ? N4 Cu1 N1 79.55(12) . . ? N2 Cu1 N1 80.35(12) . . ? N6 Cu1 N1 79.63(11) . . ? C17 N1 C1 110.6(3) . . ? C17 N1 C9 111.0(3) . . ? C1 N1 C9 112.4(3) . . ? C17 N1 Cu1 107.8(2) . . ? C1 N1 Cu1 108.5(2) . . ? C9 N1 Cu1 106.3(2) . . ? C2 N2 C3 104.8(3) . . ? C2 N2 Cu1 112.6(2) . . ? C3 N2 Cu1 142.2(3) . . ? C2 N3 C8 107.9(3) . . ? C2 N3 H3A 126.1 . . ? C8 N3 H3A 126.1 . . ? C10 N4 C11 106.2(3) . . ? C10 N4 Cu1 112.1(2) . . ? C11 N4 Cu1 141.8(2) . . ? C10 N5 C16 107.3(3) . . ? C10 N5 H5B 126.3 . . ? C16 N5 H5B 126.3 . . ? C18 N6 C19 105.9(3) . . ? C18 N6 Cu1 110.9(2) . . ? C19 N6 Cu1 142.2(2) . . ? C18 N7 C24 106.3(3) . . ? C18 N7 C25 126.7(3) . . ? C24 N7 C25 125.7(3) . . ? C2 C1 N1 108.6(3) . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? N1 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N2 C2 N3 113.3(3) . . ? N2 C2 C1 121.2(3) . . ? N3 C2 C1 125.4(4) . . ? C4 C3 N2 131.4(4) . . ? C4 C3 C8 120.4(4) . . ? N2 C3 C8 108.1(3) . . ? C3 C4 C5 117.5(4) . . ? C3 C4 H4A 121.2 . . ? C5 C4 H4A 121.2 . . ? C6 C5 C4 121.8(5) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C7 C6 C5 120.6(4) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C6 C7 C8 119.0(5) . . ? C6 C7 H7A 120.5 . . ? C8 C7 H7A 120.5 . . ? N3 C8 C7 133.4(4) . . ? N3 C8 C3 105.9(3) . . ? C7 C8 C3 120.7(4) . . ? C10 C9 N1 106.0(3) . . ? C10 C9 H9A 110.5 . . ? N1 C9 H9A 110.5 . . ? C10 C9 H9B 110.5 . . ? N1 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? N4 C10 N5 112.7(3) . . ? N4 C10 C9 121.2(3) . . ? N5 C10 C9 126.1(3) . . ? C12 C11 C16 120.0(3) . . ? C12 C11 N4 131.4(3) . . ? C16 C11 N4 108.6(3) . . ? C11 C12 C13 118.1(4) . . ? C11 C12 H12A 120.9 . . ? C13 C12 H12A 121.0 . . ? C12 C13 C14 119.6(4) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C15 C14 C13 122.5(4) . . ? C15 C14 H14A 118.8 . . ? C13 C14 H14A 118.8 . . ? C14 C15 C16 117.3(4) . . ? C14 C15 H15A 121.4 . . ? C16 C15 H15A 121.4 . . ? C15 C16 C11 122.6(4) . . ? C15 C16 N5 132.1(4) . . ? C11 C16 N5 105.3(3) . . ? N1 C17 C18 106.7(3) . . ? N1 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? N1 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? N6 C18 N7 113.3(3) . . ? N6 C18 C17 120.8(3) . . ? N7 C18 C17 125.8(3) . . ? C20 C19 N6 131.0(3) . . ? C20 C19 C24 120.4(3) . . ? N6 C19 C24 108.6(3) . . ? C19 C20 C21 117.7(3) . . ? C19 C20 H20A 121.1 . . ? C21 C20 H20A 121.1 . . ? C20 C21 C22 121.3(4) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C23 C22 C21 121.4(4) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C24 117.2(3) . . ? C22 C23 H23A 121.4 . . ? C24 C23 H23A 121.4 . . ? C23 C24 N7 132.1(3) . . ? C23 C24 C19 122.0(3) . . ? N7 C24 C19 106.0(3) . . ? N7 C25 C26 115.1(3) . . ? N7 C25 H25A 108.5 . . ? C26 C25 H25A 108.5 . . ? N7 C25 H25B 108.5 . . ? C26 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? O2 C26 O1 126.8(3) . . ? O2 C26 C25 116.1(3) . . ? O1 C26 C25 117.1(3) . . ? C26 O1 Cu1 120.7(2) . 18_756 ? F3 B1 F1 115.1(5) . . ? F3 B1 F2 112.5(5) . . ? F1 B1 F2 107.5(5) . . ? F3 B1 F4 108.5(5) . . ? F1 B1 F4 108.4(5) . . ? F2 B1 F4 104.2(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 63.94 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.792 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.089 #============# data_2-sif6 _database_code_depnum_ccdc_archive 'CCDC 812763' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C324 H356 Cu12 F36 N88 O60 Si6' _chemical_formula_weight 8057.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 26.5623(4) _cell_length_b 17.5464(2) _cell_length_c 42.0801(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.125(2) _cell_angle_gamma 90.00 _cell_volume 19019.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29381 _cell_measurement_theta_min 2.8502 _cell_measurement_theta_max 29.8373 _exptl_crystal_description block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8304 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6759 _exptl_absorpt_correction_T_max 0.7737 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_method '\w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76960 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 28.00 _reflns_number_total 22833 _reflns_number_gt 15881 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _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. The C-O bond of solvated MeOH molecules is constrained to a reasonable by DFIX which results in 1 restraint. The large mount of free water molecules are refined isotropically with fractional occupancy due to server disorder. ; _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^)+(0.0913P)^2^+22.7398P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22833 _refine_ls_number_parameters 1213 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1663 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.273406(14) 0.12707(2) 0.663035(10) 0.02252(10) Uani 1 1 d . . . Cu2 Cu 0.336170(17) 0.51934(2) 0.662596(11) 0.03009(11) Uani 1 1 d . . . Cu3 Cu 0.504684(17) 0.24814(3) 0.623885(12) 0.03484(12) Uani 1 1 d . . . N1 N 0.20835(10) 0.22683(16) 0.63653(7) 0.0276(6) Uani 1 1 d . . . N2 N 0.26424(10) 0.11341(16) 0.61466(7) 0.0260(6) Uani 1 1 d . . . N3 N 0.25653(12) 0.16622(19) 0.56586(7) 0.0366(7) Uani 1 1 d . . . H3A H 0.2480 0.1995 0.5498 0.044 Uiso 1 1 calc R . . N4 N 0.20510(10) 0.08602(15) 0.66623(6) 0.0234(6) Uani 1 1 d . . . N5 N 0.11956(10) 0.07608(16) 0.65270(7) 0.0290(6) Uani 1 1 d . . . H5B H 0.0869 0.0867 0.6435 0.035 Uiso 1 1 calc R . . N6 N 0.27862(10) 0.20478(15) 0.69795(7) 0.0248(6) Uani 1 1 d . . . N7 N 0.26843(11) 0.32114(15) 0.71649(7) 0.0268(6) Uani 1 1 d . . . N8 N 0.38263(13) 0.53493(18) 0.61796(8) 0.0387(7) Uani 1 1 d . . . N9 N 0.28219(13) 0.50292(17) 0.62067(7) 0.0332(7) Uani 1 1 d . . . N10 N 0.26083(13) 0.44465(18) 0.57265(8) 0.0396(8) Uani 1 1 d . . . H10A H 0.2642 0.4247 0.5541 0.048 Uiso 1 1 calc R . . N11 N 0.34548(12) 0.63177(16) 0.65967(7) 0.0340(7) Uani 1 1 d . . . N12 N 0.37338(13) 0.73756(17) 0.64054(8) 0.0389(8) Uani 1 1 d . . . H12B H 0.3869 0.7675 0.6280 0.047 Uiso 1 1 calc R . . N13 N 0.40941(12) 0.49681(16) 0.68531(7) 0.0310(7) Uani 1 1 d . . . N14 N 0.49104(12) 0.46690(17) 0.68575(8) 0.0367(7) Uani 1 1 d . . . N15 N 0.44648(12) 0.14754(18) 0.59526(8) 0.0373(7) Uani 1 1 d . . . N16 N 0.46719(12) 0.29644(19) 0.58148(8) 0.0376(7) Uani 1 1 d . . . N17 N 0.39384(13) 0.3120(2) 0.54388(8) 0.0424(8) Uani 1 1 d . . . H17C H 0.3628 0.3017 0.5314 0.051 Uiso 1 1 calc R . . N18 N 0.55256(13) 0.1777(2) 0.60746(8) 0.0434(8) Uani 1 1 d . . . N19 N 0.57009(16) 0.0695(2) 0.58539(10) 0.0552(10) Uani 1 1 d . . . H19A H 0.5651 0.0268 0.5741 0.066 Uiso 1 1 calc R . . N20 N 0.49675(11) 0.18105(17) 0.66054(8) 0.0329(7) Uani 1 1 d . . . N21 N 0.45442(10) 0.09213(16) 0.68141(7) 0.0296(6) Uani 1 1 d . . . C1 C 0.22657(14) 0.2442(2) 0.60730(9) 0.0331(8) Uani 1 1 d . . . H1A H 0.2537 0.2841 0.6124 0.040 Uiso 1 1 calc R . . H1B H 0.1974 0.2636 0.5898 0.040 Uiso 1 1 calc R . . C2 C 0.24822(13) 0.1737(2) 0.59590(9) 0.0292(7) Uani 1 1 d . . . C3 C 0.28546(13) 0.0633(2) 0.59558(9) 0.0289(7) Uani 1 1 d . . . C4 C 0.31041(13) -0.0064(2) 0.60325(9) 0.0341(8) Uani 1 1 d . . . H4A H 0.3139 -0.0295 0.6241 0.041 Uiso 1 1 calc R . . C5 C 0.32999(15) -0.0408(2) 0.57915(11) 0.0438(10) Uani 1 1 d . . . H5A H 0.3473 -0.0884 0.5836 0.053 Uiso 1 1 calc R . . C6 C 0.32484(17) -0.0068(3) 0.54834(11) 0.0507(11) Uani 1 1 d . . . H6A H 0.3388 -0.0322 0.5325 0.061 Uiso 1 1 calc R . . C7 C 0.30021(16) 0.0620(3) 0.54025(10) 0.0450(10) Uani 1 1 d . . . H7A H 0.2965 0.0845 0.5193 0.054 Uiso 1 1 calc R . . C8 C 0.28098(14) 0.0970(2) 0.56464(9) 0.0330(8) Uani 1 1 d . . . C9 C 0.15803(12) 0.1865(2) 0.62909(9) 0.0312(8) Uani 1 1 d . . . H9A H 0.1482 0.1727 0.6056 0.037 Uiso 1 1 calc R . . H9B H 0.1309 0.2207 0.6335 0.037 Uiso 1 1 calc R . . C10 C 0.16115(12) 0.11591(19) 0.64945(8) 0.0258(7) Uani 1 1 d . . . C11 C 0.19150(12) 0.02220(18) 0.68213(8) 0.0250(7) Uani 1 1 d . . . C12 C 0.22218(15) -0.02884(19) 0.70374(9) 0.0322(8) Uani 1 1 d . . . H12A H 0.2589 -0.0238 0.7100 0.039 Uiso 1 1 calc R . . C13 C 0.19719(17) -0.0870(2) 0.71567(10) 0.0414(9) Uani 1 1 d . . . H13A H 0.2171 -0.1228 0.7305 0.050 Uiso 1 1 calc R . . C14 C 0.14278(17) -0.0946(2) 0.70636(11) 0.0471(10) Uani 1 1 d . . . H14A H 0.1270 -0.1355 0.7151 0.057 Uiso 1 1 calc R . . C15 C 0.11159(16) -0.0441(2) 0.68483(10) 0.0397(9) Uani 1 1 d . . . H15A H 0.0749 -0.0494 0.6784 0.048 Uiso 1 1 calc R . . C16 C 0.13756(13) 0.0149(2) 0.67332(9) 0.0307(8) Uani 1 1 d . . . C17 C 0.21343(14) 0.28866(19) 0.66052(9) 0.0322(8) Uani 1 1 d . . . H17A H 0.1795 0.2973 0.6658 0.039 Uiso 1 1 calc R . . H17B H 0.2233 0.3362 0.6509 0.039 Uiso 1 1 calc R . . C18 C 0.25380(12) 0.27022(18) 0.69162(8) 0.0251(7) Uani 1 1 d . . . C19 C 0.31239(12) 0.21265(19) 0.72897(8) 0.0251(7) Uani 1 1 d . . . C20 C 0.34810(13) 0.1617(2) 0.74745(9) 0.0305(7) Uani 1 1 d . . . H20A H 0.3511 0.1110 0.7402 0.037 Uiso 1 1 calc R . . C21 C 0.37902(15) 0.1879(2) 0.77678(9) 0.0359(8) Uani 1 1 d . . . H21A H 0.4042 0.1549 0.7897 0.043 Uiso 1 1 calc R . . C22 C 0.37396(15) 0.2623(2) 0.78773(9) 0.0384(9) Uani 1 1 d . . . H22A H 0.3961 0.2785 0.8079 0.046 Uiso 1 1 calc R . . C23 C 0.33793(15) 0.3123(2) 0.77021(9) 0.0346(8) Uani 1 1 d . . . H23A H 0.3343 0.3624 0.7779 0.042 Uiso 1 1 calc R . . C24 C 0.30714(13) 0.28612(19) 0.74078(8) 0.0273(7) Uani 1 1 d . . . C25 C 0.25203(14) 0.40017(18) 0.71673(9) 0.0308(8) Uani 1 1 d . . . H25A H 0.2568 0.4167 0.7398 0.037 Uiso 1 1 calc R . . H25B H 0.2145 0.4033 0.7060 0.037 Uiso 1 1 calc R . . C26 C 0.28122(14) 0.45531(19) 0.69953(8) 0.0280(7) Uani 1 1 d . . . C27 C 0.35371(17) 0.4836(2) 0.59295(10) 0.0436(10) Uani 1 1 d . . . H27A H 0.3698 0.4324 0.5959 0.052 Uiso 1 1 calc R . . H27B H 0.3548 0.5026 0.5710 0.052 Uiso 1 1 calc R . . C28 C 0.29854(17) 0.4782(2) 0.59529(9) 0.0372(9) Uani 1 1 d . . . C29 C 0.22960(15) 0.4840(2) 0.61378(9) 0.0351(8) Uani 1 1 d . . . C30 C 0.19278(16) 0.4983(2) 0.63149(10) 0.0432(10) Uani 1 1 d . . . H30A H 0.2014 0.5259 0.6515 0.052 Uiso 1 1 calc R . . C31 C 0.14290(17) 0.4706(3) 0.61877(13) 0.0582(13) Uani 1 1 d . . . H31A H 0.1170 0.4794 0.6304 0.070 Uiso 1 1 calc R . . C32 C 0.12997(18) 0.4303(3) 0.58930(12) 0.0622(14) Uani 1 1 d . . . H32A H 0.0957 0.4110 0.5816 0.075 Uiso 1 1 calc R . . C33 C 0.16614(18) 0.4179(3) 0.57113(11) 0.0524(12) Uani 1 1 d . . . H33A H 0.1574 0.3908 0.5510 0.063 Uiso 1 1 calc R . . C34 C 0.21581(16) 0.4468(2) 0.58351(9) 0.0384(9) Uani 1 1 d . . . C35 C 0.37656(19) 0.6160(2) 0.60927(10) 0.0455(10) Uani 1 1 d . . . H35A H 0.3474 0.6224 0.5897 0.055 Uiso 1 1 calc R . . H35B H 0.4085 0.6348 0.6038 0.055 Uiso 1 1 calc R . . C36 C 0.36636(15) 0.6611(2) 0.63681(9) 0.0366(9) Uani 1 1 d . . . C37 C 0.33813(14) 0.69302(19) 0.67945(9) 0.0323(8) Uani 1 1 d . . . C38 C 0.31705(15) 0.6946(2) 0.70615(10) 0.0382(9) Uani 1 1 d . . . H38A H 0.3053 0.6494 0.7145 0.046 Uiso 1 1 calc R . . C39 C 0.31361(16) 0.7655(2) 0.72040(12) 0.0467(10) Uani 1 1 d . . . H39A H 0.2994 0.7687 0.7390 0.056 Uiso 1 1 calc R . . C40 C 0.33068(17) 0.8326(2) 0.70781(12) 0.0496(11) Uani 1 1 d . . . H40A H 0.3272 0.8801 0.7179 0.060 Uiso 1 1 calc R . . C41 C 0.35220(14) 0.8306(2) 0.68144(10) 0.0384(9) Uani 1 1 d . . . H41A H 0.3643 0.8757 0.6732 0.046 Uiso 1 1 calc R . . C42 C 0.35576(14) 0.7601(2) 0.66708(10) 0.0333(8) Uani 1 1 d . . . C43 C 0.43640(17) 0.5128(3) 0.63256(11) 0.0497(11) Uani 1 1 d . . . H43A H 0.4597 0.5553 0.6303 0.060 Uiso 1 1 calc R . . H43B H 0.4455 0.4683 0.6206 0.060 Uiso 1 1 calc R . . C44 C 0.44470(15) 0.4930(2) 0.66787(10) 0.0357(8) Uani 1 1 d . . . C45 C 0.43398(14) 0.46949(19) 0.71651(9) 0.0320(8) Uani 1 1 d . . . C46 C 0.41568(15) 0.4605(2) 0.74424(9) 0.0372(9) Uani 1 1 d . . . H46A H 0.3817 0.4764 0.7448 0.045 Uiso 1 1 calc R . . C47 C 0.44877(16) 0.4273(2) 0.77130(10) 0.0412(9) Uani 1 1 d . . . H47A H 0.4371 0.4199 0.7907 0.049 Uiso 1 1 calc R . . C48 C 0.49903(16) 0.4046(2) 0.77064(10) 0.0412(9) Uani 1 1 d . . . H48A H 0.5203 0.3803 0.7893 0.049 Uiso 1 1 calc R . . C49 C 0.51812(16) 0.4165(2) 0.74376(10) 0.0397(9) Uani 1 1 d . . . H49A H 0.5526 0.4028 0.7435 0.048 Uiso 1 1 calc R . . C50 C 0.48471(15) 0.4494(2) 0.71701(9) 0.0342(8) Uani 1 1 d . . . C51 C 0.53729(16) 0.4538(2) 0.67388(12) 0.0452(10) Uani 1 1 d . . . H51A H 0.5679 0.4534 0.6928 0.054 Uiso 1 1 calc R . . H51B H 0.5415 0.4968 0.6596 0.054 Uiso 1 1 calc R . . C52 C 0.53665(17) 0.3795(2) 0.65482(10) 0.0428(9) Uani 1 1 d . . . C53 C 0.40245(16) 0.1916(2) 0.57678(11) 0.0461(10) Uani 1 1 d . . . H53A H 0.3774 0.2004 0.5904 0.055 Uiso 1 1 calc R . . H53B H 0.3845 0.1630 0.5570 0.055 Uiso 1 1 calc R . . C54 C 0.42150(15) 0.2669(2) 0.56698(10) 0.0388(9) Uani 1 1 d . . . C55 C 0.46845(15) 0.3670(2) 0.56643(10) 0.0394(9) Uani 1 1 d . . . C56 C 0.50682(18) 0.4227(3) 0.57114(11) 0.0537(12) Uani 1 1 d . . . H56A H 0.5389 0.4162 0.5869 0.064 Uiso 1 1 calc R . . C57 C 0.4967(2) 0.4872(3) 0.55227(13) 0.0714(16) Uani 1 1 d . . . H57A H 0.5224 0.5261 0.5552 0.086 Uiso 1 1 calc R . . C58 C 0.4494(2) 0.4979(3) 0.52858(13) 0.0680(15) Uani 1 1 d . . . H58A H 0.4437 0.5436 0.5161 0.082 Uiso 1 1 calc R . . C59 C 0.41116(19) 0.4425(3) 0.52337(11) 0.0546(12) Uani 1 1 d . . . H59A H 0.3793 0.4486 0.5074 0.066 Uiso 1 1 calc R . . C60 C 0.42181(16) 0.3773(2) 0.54273(10) 0.0419(9) Uani 1 1 d . . . C61 C 0.47559(18) 0.1099(3) 0.57449(11) 0.0499(11) Uani 1 1 d . . . H61A H 0.4669 0.1332 0.5524 0.060 Uiso 1 1 calc R . . H61B H 0.4663 0.0552 0.5722 0.060 Uiso 1 1 calc R . . C62 C 0.53292(18) 0.1184(2) 0.58986(11) 0.0465(10) Uani 1 1 d . . . C63 C 0.60628(16) 0.1673(3) 0.61578(10) 0.0464(11) Uani 1 1 d . . . C64 C 0.64561(17) 0.2116(4) 0.63488(12) 0.0618(14) Uani 1 1 d . . . H64A H 0.6384 0.2579 0.6446 0.074 Uiso 1 1 calc R . . C65 C 0.6957(2) 0.1848(4) 0.63891(15) 0.0786(18) Uani 1 1 d . . . H65A H 0.7238 0.2141 0.6514 0.094 Uiso 1 1 calc R . . C66 C 0.7061(2) 0.1170(5) 0.62537(17) 0.087(2) Uani 1 1 d . . . H66A H 0.7411 0.1003 0.6292 0.104 Uiso 1 1 calc R . . C67 C 0.6689(3) 0.0743(4) 0.60718(15) 0.0775(19) Uani 1 1 d . . . H67A H 0.6769 0.0279 0.5979 0.093 Uiso 1 1 calc R . . C68 C 0.61753(19) 0.0994(3) 0.60204(12) 0.0546(12) Uani 1 1 d . . . C69 C 0.43464(16) 0.0972(2) 0.62066(10) 0.0414(9) Uani 1 1 d . . . H69A H 0.4455 0.0444 0.6173 0.050 Uiso 1 1 calc R . . H69B H 0.3968 0.0970 0.6188 0.050 Uiso 1 1 calc R . . C70 C 0.46241(13) 0.1240(2) 0.65412(9) 0.0317(8) Uani 1 1 d . . . C71 C 0.51137(12) 0.1863(2) 0.69461(9) 0.0307(8) Uani 1 1 d . . . C72 C 0.54658(14) 0.2356(2) 0.71511(11) 0.0392(9) Uani 1 1 d . . . H72A H 0.5656 0.2728 0.7065 0.047 Uiso 1 1 calc R . . C73 C 0.55212(15) 0.2272(2) 0.74851(10) 0.0427(10) Uani 1 1 d . . . H73A H 0.5755 0.2599 0.7631 0.051 Uiso 1 1 calc R . . C74 C 0.52473(17) 0.1727(2) 0.76158(11) 0.0460(10) Uani 1 1 d . . . H74A H 0.5298 0.1693 0.7847 0.055 Uiso 1 1 calc R . . C75 C 0.49024(15) 0.1235(2) 0.74150(10) 0.0395(9) Uani 1 1 d . . . H75A H 0.4712 0.0864 0.7501 0.047 Uiso 1 1 calc R . . C76 C 0.48518(12) 0.13148(19) 0.70811(9) 0.0306(8) Uani 1 1 d . . . C77 C 0.41750(13) 0.03281(19) 0.68322(9) 0.0316(8) Uani 1 1 d . . . H77A H 0.4289 0.0069 0.7047 0.038 Uiso 1 1 calc R . . H77B H 0.4180 -0.0054 0.6660 0.038 Uiso 1 1 calc R . . C78 C 0.36204(12) 0.06042(18) 0.67918(8) 0.0252(7) Uani 1 1 d . . . O1 O 0.31016(9) 0.42815(13) 0.68257(6) 0.0301(5) Uani 1 1 d . . . O2 O 0.27401(11) 0.52440(13) 0.70309(7) 0.0398(6) Uani 1 1 d . . . O3 O 0.49478(11) 0.34077(15) 0.64843(7) 0.0413(6) Uani 1 1 d . . . O4 O 0.57651(13) 0.3616(2) 0.64693(10) 0.0707(11) Uani 1 1 d . . . O5 O 0.35029(8) 0.12723(12) 0.66784(6) 0.0265(5) Uani 1 1 d . . . O6 O 0.33054(10) 0.01579(14) 0.68618(7) 0.0379(6) Uani 1 1 d . . . Si1 Si 0.47819(4) 0.86466(6) 0.62283(3) 0.0344(2) Uani 1 1 d . . . Si2 Si 0.2500 0.31248(8) 0.5000 0.0279(3) Uani 1 2 d S . . F1 F 0.50030(11) 0.81305(14) 0.65689(6) 0.0564(7) Uani 1 1 d . . . F2 F 0.45656(9) 0.91449(14) 0.58786(6) 0.0496(6) Uani 1 1 d . . . F3 F 0.42528(9) 0.88755(14) 0.63511(6) 0.0488(6) Uani 1 1 d . . . F4 F 0.50936(9) 0.94214(14) 0.64125(7) 0.0564(7) Uani 1 1 d . . . F5 F 0.53191(9) 0.84033(14) 0.61038(7) 0.0536(6) Uani 1 1 d . . . F6 F 0.44703(9) 0.78592(13) 0.60401(6) 0.0453(6) Uani 1 1 d . . . F7 F 0.22617(9) 0.31098(13) 0.53330(5) 0.0410(5) Uani 1 1 d . . . F8 F 0.29334(8) 0.24426(12) 0.51680(5) 0.0402(5) Uani 1 1 d . . . F9 F 0.29273(8) 0.38063(12) 0.51724(5) 0.0401(5) Uani 1 1 d . . . N22 N 0.35278(17) 0.3087(2) 0.62507(11) 0.0621(11) Uani 1 1 d . . . C79 C 0.37331(16) 0.3022(2) 0.65218(13) 0.0442(10) Uani 1 1 d . . . C80 C 0.39907(14) 0.2941(2) 0.68662(10) 0.0372(9) Uani 1 1 d . . . H80A H 0.4364 0.3029 0.6897 0.056 Uiso 1 1 calc R . . H80B H 0.3934 0.2425 0.6940 0.056 Uiso 1 1 calc R . . H80C H 0.3849 0.3314 0.6994 0.056 Uiso 1 1 calc R . . O1W O 0.51468(17) 0.6585(2) 0.65501(11) 0.0846(12) Uani 1 1 d D . . H1W H 0.5126 0.7041 0.6606 0.127 Uiso 1 1 calc R . . C1W C 0.5435(2) 0.6543(3) 0.63523(17) 0.0784(17) Uani 1 1 d D . . H1W1 H 0.5485 0.7053 0.6270 0.118 Uiso 1 1 calc R . . H1W2 H 0.5272 0.6213 0.6168 0.118 Uiso 1 1 calc R . . H1W3 H 0.5773 0.6330 0.6465 0.118 Uiso 1 1 calc R . . O2W O 0.6671(3) 0.4252(4) 0.71269(17) 0.0589(17) Uiso 0.50 1 d P A 1 O4W O 0.0422(4) 0.0692(5) 0.5578(2) 0.072(2) Uiso 0.50 1 d P B 1 O6W O 0.1279(4) 0.1225(6) 0.5516(3) 0.108(3) Uiso 0.50 1 d P C 1 O8W O 0.3848(6) 0.8114(9) 0.5366(4) 0.159(5) Uiso 0.50 1 d P D 1 O10W O 0.4776(7) 0.6964(9) 0.5602(4) 0.075(4) Uiso 0.25 1 d P E 1 O11W O 0.1445(9) 0.6413(13) 0.5632(5) 0.114(7) Uiso 0.25 1 d P F 1 O12W O 0.2769(8) 0.6003(12) 0.5322(5) 0.101(6) Uiso 0.25 1 d P G 1 O13W O 0.2536(7) 0.6629(10) 0.5712(4) 0.086(5) Uiso 0.25 1 d P H 1 O18W O 0.1646(10) 0.6009(15) 0.5275(6) 0.136(8) Uiso 0.25 1 d P I 1 O20W O 0.2940(9) -0.1423(14) 0.4700(6) 0.131(8) Uiso 0.25 1 d P J 1 O23W O 0.4188(8) 0.8900(13) 0.5217(5) 0.114(7) Uiso 0.25 1 d P K 1 O24W O 0.2923(10) 0.7395(16) 0.5524(6) 0.146(9) Uiso 0.25 1 d P L 1 O5W O 0.6818(3) 0.3499(5) 0.6998(2) 0.086(2) Uiso 0.50 1 d P M 2 O9W O 0.6395(5) 0.4755(8) 0.7336(3) 0.151(5) Uiso 0.50 1 d P N 2 O14W O 0.1246(7) 0.1713(11) 0.5227(4) 0.090(5) Uiso 0.25 1 d P O 2 O16W O 0.2500 0.5711(14) 0.5000 0.182(8) Uiso 0.50 2 d SP P 2 O17W O 0.0199(4) 0.0676(6) 0.5470(3) 0.034(2) Uiso 0.25 1 d P Q 2 O19W O 0.5103(8) 0.7097(11) 0.5544(5) 0.095(5) Uiso 0.25 1 d P R 2 O21W O 0.3719(8) 0.6810(13) 0.5275(5) 0.111(6) Uiso 0.25 1 d P S 2 O22W O 0.2109(11) 0.6568(15) 0.5766(6) 0.140(8) Uiso 0.25 1 d P T 2 O7W O 0.7002(6) 0.3970(9) 0.7226(4) 0.157(5) Uiso 0.50 1 d P U 3 O15W O 0.0906(7) 0.2082(11) 0.5527(5) 0.098(5) Uiso 0.25 1 d P V 3 O25W O 0.3514(10) 0.7568(15) 0.5381(6) 0.131(8) Uiso 0.25 1 d P W 3 O26W O 0.4746(11) 0.9194(18) 0.4969(7) 0.162(10) Uiso 0.25 1 d P X 3 O27W O 0.0907(10) 0.0739(14) 0.5617(6) 0.128(8) Uiso 0.25 1 d P Y 3 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 0.01813(18) 0.01813(19) 0.0295(2) 0.00172(15) 0.00234(15) -0.00113(15) Cu2 0.0401(3) 0.0201(2) 0.0322(2) 0.00109(17) 0.01276(19) -0.00816(17) Cu3 0.0276(2) 0.0361(3) 0.0428(3) -0.0102(2) 0.01233(19) -0.00595(19) N1 0.0229(14) 0.0205(13) 0.0377(16) 0.0057(12) 0.0040(12) 0.0015(11) N2 0.0199(13) 0.0235(14) 0.0327(15) 0.0040(11) 0.0028(11) 0.0018(11) N3 0.0363(17) 0.0399(18) 0.0333(17) 0.0116(14) 0.0078(14) 0.0045(14) N4 0.0214(13) 0.0196(13) 0.0273(14) 0.0010(11) 0.0023(11) -0.0013(10) N5 0.0190(13) 0.0302(15) 0.0371(16) -0.0046(13) 0.0053(12) -0.0040(11) N6 0.0209(13) 0.0172(13) 0.0351(15) 0.0012(11) 0.0047(11) -0.0017(10) N7 0.0313(15) 0.0180(13) 0.0354(16) -0.0003(11) 0.0162(12) -0.0035(11) N8 0.051(2) 0.0317(17) 0.0377(18) 0.0006(14) 0.0185(15) -0.0095(15) N9 0.0474(18) 0.0242(15) 0.0296(16) -0.0014(12) 0.0126(14) -0.0031(13) N10 0.056(2) 0.0329(17) 0.0284(16) -0.0049(13) 0.0071(15) -0.0003(15) N11 0.0452(18) 0.0222(14) 0.0370(17) 0.0004(13) 0.0146(14) -0.0086(13) N12 0.0463(19) 0.0238(15) 0.0437(19) 0.0091(13) 0.0057(15) -0.0116(14) N13 0.0366(16) 0.0230(14) 0.0360(16) -0.0030(12) 0.0137(13) -0.0097(12) N14 0.0395(18) 0.0278(16) 0.0464(19) -0.0075(14) 0.0175(15) -0.0097(13) N15 0.0355(17) 0.0354(17) 0.0427(18) -0.0097(14) 0.0131(14) -0.0045(14) N16 0.0290(16) 0.0423(19) 0.0439(19) -0.0079(15) 0.0134(14) -0.0068(14) N17 0.0336(17) 0.049(2) 0.0421(19) -0.0047(16) 0.0047(14) -0.0104(15) N18 0.0402(18) 0.050(2) 0.046(2) -0.0048(16) 0.0218(16) 0.0051(16) N19 0.075(3) 0.042(2) 0.063(2) 0.0045(18) 0.044(2) 0.018(2) N20 0.0217(14) 0.0297(16) 0.0472(19) -0.0102(13) 0.0083(13) -0.0027(12) N21 0.0194(13) 0.0228(14) 0.0429(17) -0.0012(13) 0.0007(12) 0.0026(11) C1 0.0323(18) 0.0259(18) 0.042(2) 0.0132(15) 0.0105(16) 0.0071(14) C2 0.0233(16) 0.0293(18) 0.0345(19) 0.0070(15) 0.0065(14) 0.0010(13) C3 0.0234(16) 0.0278(17) 0.0324(18) -0.0027(14) 0.0010(14) -0.0046(13) C4 0.0287(18) 0.0286(18) 0.039(2) -0.0044(15) -0.0034(15) -0.0026(14) C5 0.037(2) 0.038(2) 0.053(3) -0.0146(19) 0.0039(18) -0.0011(17) C6 0.047(2) 0.055(3) 0.051(3) -0.022(2) 0.014(2) -0.002(2) C7 0.043(2) 0.055(3) 0.037(2) -0.0095(19) 0.0094(18) -0.006(2) C8 0.0273(17) 0.036(2) 0.0338(19) -0.0020(16) 0.0039(15) -0.0028(15) C9 0.0188(15) 0.0291(18) 0.041(2) 0.0073(15) -0.0009(14) 0.0010(13) C10 0.0228(15) 0.0254(17) 0.0287(17) -0.0035(13) 0.0058(13) -0.0007(13) C11 0.0268(16) 0.0195(15) 0.0301(17) -0.0034(13) 0.0095(14) -0.0050(13) C12 0.0358(19) 0.0236(17) 0.038(2) 0.0011(15) 0.0117(16) -0.0016(14) C13 0.055(2) 0.0253(19) 0.050(2) 0.0086(17) 0.024(2) 0.0011(17) C14 0.056(3) 0.030(2) 0.065(3) -0.0003(19) 0.032(2) -0.0140(19) C15 0.039(2) 0.032(2) 0.055(2) -0.0064(18) 0.0240(19) -0.0130(17) C16 0.0292(17) 0.0261(17) 0.038(2) -0.0102(15) 0.0115(15) -0.0073(14) C17 0.0319(18) 0.0219(17) 0.040(2) 0.0042(15) 0.0042(15) 0.0076(14) C18 0.0203(15) 0.0199(15) 0.0367(19) 0.0036(13) 0.0102(13) -0.0012(12) C19 0.0233(16) 0.0241(16) 0.0301(17) 0.0005(13) 0.0109(13) -0.0047(13) C20 0.0296(18) 0.0280(18) 0.0347(19) 0.0009(15) 0.0093(15) 0.0007(14) C21 0.036(2) 0.041(2) 0.0302(19) 0.0039(16) 0.0067(15) 0.0009(16) C22 0.043(2) 0.042(2) 0.0304(19) -0.0035(16) 0.0100(16) -0.0079(18) C23 0.046(2) 0.0295(19) 0.0325(19) -0.0041(15) 0.0166(17) -0.0082(16) C24 0.0287(17) 0.0240(16) 0.0325(18) 0.0019(14) 0.0136(14) -0.0055(13) C25 0.0373(19) 0.0184(16) 0.042(2) -0.0004(14) 0.0203(16) 0.0005(14) C26 0.0347(18) 0.0221(16) 0.0279(17) 0.0028(13) 0.0088(14) -0.0045(14) C27 0.059(3) 0.037(2) 0.043(2) -0.0046(18) 0.028(2) -0.0092(19) C28 0.058(2) 0.0234(18) 0.0314(19) 0.0000(15) 0.0124(18) -0.0050(17) C29 0.043(2) 0.0220(17) 0.037(2) 0.0003(15) 0.0045(17) 0.0058(15) C30 0.044(2) 0.038(2) 0.044(2) -0.0046(18) 0.0051(18) 0.0090(18) C31 0.036(2) 0.067(3) 0.068(3) -0.012(3) 0.005(2) 0.016(2) C32 0.037(2) 0.075(4) 0.064(3) -0.015(3) -0.008(2) 0.015(2) C33 0.052(3) 0.049(3) 0.045(2) -0.012(2) -0.010(2) 0.017(2) C34 0.049(2) 0.0283(19) 0.033(2) -0.0008(15) 0.0006(17) 0.0092(17) C35 0.067(3) 0.034(2) 0.039(2) 0.0030(17) 0.019(2) -0.017(2) C36 0.045(2) 0.0270(18) 0.038(2) 0.0062(16) 0.0099(17) -0.0116(16) C37 0.0301(18) 0.0165(15) 0.046(2) 0.0026(14) 0.0015(16) -0.0013(13) C38 0.044(2) 0.0190(17) 0.053(2) -0.0014(16) 0.0162(19) -0.0006(15) C39 0.045(2) 0.028(2) 0.073(3) -0.0017(19) 0.025(2) 0.0063(17) C40 0.046(2) 0.0204(18) 0.085(3) -0.003(2) 0.020(2) 0.0073(17) C41 0.0332(19) 0.0166(16) 0.062(3) 0.0095(16) 0.0046(18) 0.0008(14) C42 0.0297(18) 0.0227(17) 0.044(2) 0.0054(15) 0.0026(16) -0.0032(14) C43 0.050(3) 0.056(3) 0.050(3) 0.008(2) 0.025(2) -0.003(2) C44 0.044(2) 0.0253(18) 0.042(2) -0.0039(15) 0.0185(18) -0.0129(16) C45 0.040(2) 0.0208(16) 0.0358(19) -0.0042(14) 0.0092(16) -0.0093(14) C46 0.041(2) 0.0304(19) 0.041(2) -0.0056(16) 0.0108(17) -0.0097(16) C47 0.054(2) 0.033(2) 0.036(2) -0.0051(16) 0.0077(18) -0.0086(18) C48 0.048(2) 0.031(2) 0.042(2) -0.0067(17) 0.0044(19) -0.0071(17) C49 0.041(2) 0.0250(18) 0.050(2) -0.0096(17) 0.0052(18) -0.0063(16) C50 0.041(2) 0.0212(17) 0.043(2) -0.0076(15) 0.0143(17) -0.0114(15) C51 0.039(2) 0.036(2) 0.065(3) -0.004(2) 0.023(2) -0.0117(18) C52 0.048(2) 0.038(2) 0.048(2) -0.0017(18) 0.023(2) -0.0069(19) C53 0.037(2) 0.040(2) 0.059(3) -0.012(2) 0.0069(19) -0.0128(18) C54 0.0313(19) 0.041(2) 0.044(2) -0.0097(18) 0.0096(17) -0.0043(17) C55 0.039(2) 0.047(2) 0.036(2) -0.0051(17) 0.0137(17) -0.0075(18) C56 0.043(2) 0.066(3) 0.050(3) 0.003(2) 0.008(2) -0.024(2) C57 0.072(4) 0.075(4) 0.063(3) 0.009(3) 0.008(3) -0.042(3) C58 0.079(4) 0.070(3) 0.055(3) 0.016(3) 0.015(3) -0.021(3) C59 0.055(3) 0.064(3) 0.044(2) -0.001(2) 0.010(2) -0.010(2) C60 0.041(2) 0.048(2) 0.039(2) -0.0059(18) 0.0146(18) -0.0070(19) C61 0.059(3) 0.042(2) 0.053(3) -0.016(2) 0.022(2) -0.004(2) C62 0.056(3) 0.042(2) 0.051(3) 0.003(2) 0.031(2) 0.009(2) C63 0.038(2) 0.066(3) 0.042(2) 0.012(2) 0.0222(19) 0.013(2) C64 0.038(2) 0.095(4) 0.057(3) 0.006(3) 0.020(2) 0.009(3) C65 0.041(3) 0.122(6) 0.075(4) 0.016(4) 0.018(3) 0.022(3) C66 0.047(3) 0.129(6) 0.089(5) 0.030(4) 0.025(3) 0.039(4) C67 0.088(4) 0.081(4) 0.076(4) 0.030(3) 0.044(4) 0.049(4) C68 0.058(3) 0.061(3) 0.054(3) 0.017(2) 0.032(2) 0.020(2) C69 0.042(2) 0.037(2) 0.046(2) -0.0124(18) 0.0114(18) -0.0146(17) C70 0.0191(15) 0.0285(18) 0.047(2) -0.0083(16) 0.0068(15) 0.0026(14) C71 0.0183(15) 0.0294(18) 0.042(2) -0.0068(15) 0.0029(14) 0.0053(13) C72 0.0226(17) 0.0311(19) 0.059(3) -0.0078(18) 0.0011(17) 0.0027(15) C73 0.038(2) 0.033(2) 0.048(2) -0.0100(18) -0.0071(18) 0.0082(17) C74 0.053(3) 0.033(2) 0.044(2) 0.0013(18) -0.0048(19) 0.0101(19) C75 0.039(2) 0.0278(19) 0.047(2) 0.0050(17) -0.0002(17) 0.0066(16) C76 0.0195(15) 0.0227(16) 0.046(2) -0.0018(15) 0.0003(14) 0.0068(13) C77 0.0243(17) 0.0210(16) 0.047(2) 0.0012(15) 0.0033(15) 0.0022(13) C78 0.0230(16) 0.0181(15) 0.0318(18) -0.0028(13) 0.0019(13) -0.0006(12) O1 0.0360(13) 0.0242(12) 0.0342(13) 0.0008(10) 0.0162(11) -0.0046(10) O2 0.0634(18) 0.0158(12) 0.0440(15) 0.0002(10) 0.0204(14) 0.0000(11) O3 0.0480(16) 0.0324(14) 0.0483(16) -0.0088(12) 0.0211(13) -0.0059(12) O4 0.056(2) 0.063(2) 0.109(3) -0.019(2) 0.051(2) -0.0048(17) O5 0.0210(11) 0.0197(11) 0.0365(13) 0.0010(10) 0.0023(9) 0.0007(9) O6 0.0304(13) 0.0217(12) 0.0617(18) 0.0062(12) 0.0118(12) -0.0018(10) Si1 0.0298(5) 0.0290(5) 0.0409(6) -0.0008(4) 0.0020(4) -0.0033(4) Si2 0.0341(7) 0.0258(7) 0.0211(6) 0.000 0.0013(5) 0.000 F1 0.0781(18) 0.0400(14) 0.0413(14) 0.0010(11) -0.0045(12) 0.0108(13) F2 0.0453(13) 0.0523(15) 0.0520(14) 0.0172(12) 0.0131(11) 0.0036(11) F3 0.0486(14) 0.0474(14) 0.0538(15) -0.0011(11) 0.0193(12) -0.0001(11) F4 0.0431(13) 0.0364(13) 0.0815(19) -0.0149(12) -0.0005(12) -0.0061(11) F5 0.0354(12) 0.0450(14) 0.0825(18) -0.0056(13) 0.0182(12) 0.0010(11) F6 0.0485(13) 0.0417(13) 0.0464(13) -0.0092(11) 0.0129(11) -0.0169(11) F7 0.0555(14) 0.0375(12) 0.0327(11) 0.0002(9) 0.0161(10) 0.0013(10) F8 0.0410(12) 0.0338(12) 0.0432(13) 0.0072(10) 0.0050(10) 0.0071(9) F9 0.0424(12) 0.0335(12) 0.0409(12) -0.0057(9) 0.0034(10) -0.0072(10) N22 0.067(3) 0.056(3) 0.064(3) 0.001(2) 0.018(2) -0.005(2) C79 0.039(2) 0.028(2) 0.070(3) -0.006(2) 0.020(2) -0.0033(16) C80 0.0306(19) 0.0232(18) 0.060(3) -0.0075(17) 0.0149(18) -0.0059(14) O1W 0.085(3) 0.045(2) 0.111(3) -0.001(2) -0.001(3) -0.001(2) C1W 0.072(4) 0.047(3) 0.119(5) 0.005(3) 0.029(4) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 1.984(3) . ? Cu1 N4 1.987(3) . ? Cu1 O5 2.003(2) . ? Cu1 N2 2.005(3) . ? Cu1 O6 2.519(2) . ? Cu2 N13 1.987(3) . ? Cu2 N11 1.996(3) . ? Cu2 N9 2.004(3) . ? Cu2 O1 2.007(2) . ? Cu2 O2 2.648(3) . ? Cu3 O3 1.977(3) . ? Cu3 N20 1.992(3) . ? Cu3 N16 2.007(3) . ? Cu3 N18 2.013(3) . ? Cu3 N15 2.459(3) . ? Cu3 O4 2.765(4) . ? N1 C1 1.460(5) . ? N1 C17 1.465(4) . ? N1 C9 1.477(4) . ? N2 C2 1.326(4) . ? N2 C3 1.398(4) . ? N3 C2 1.342(5) . ? N3 C8 1.383(5) . ? N3 H3A 0.8800 . ? N4 C10 1.317(4) . ? N4 C11 1.397(4) . ? N5 C10 1.342(4) . ? N5 C16 1.389(5) . ? N5 H5B 0.8800 . ? N6 C18 1.319(4) . ? N6 C19 1.399(4) . ? N7 C18 1.359(4) . ? N7 C24 1.402(4) . ? N7 C25 1.454(4) . ? N8 C27 1.454(5) . ? N8 C43 1.463(6) . ? N8 C35 1.467(5) . ? N9 C28 1.320(5) . ? N9 C29 1.396(5) . ? N10 C28 1.339(5) . ? N10 C34 1.381(5) . ? N10 H10A 0.8800 . ? N11 C36 1.327(5) . ? N11 C37 1.402(5) . ? N12 C36 1.358(5) . ? N12 C42 1.370(5) . ? N12 H12B 0.8800 . ? N13 C44 1.325(5) . ? N13 C45 1.401(5) . ? N14 C44 1.356(5) . ? N14 C50 1.400(5) . ? N14 C51 1.453(5) . ? N15 C53 1.458(5) . ? N15 C61 1.459(5) . ? N15 C69 1.479(5) . ? N16 C54 1.324(5) . ? N16 C55 1.394(5) . ? N17 C54 1.327(5) . ? N17 C60 1.374(5) . ? N17 H17C 0.8800 . ? N18 C62 1.309(6) . ? N18 C63 1.396(5) . ? N19 C62 1.356(5) . ? N19 C68 1.387(7) . ? N19 H19A 0.8800 . ? N20 C70 1.337(4) . ? N20 C71 1.394(5) . ? N21 C70 1.340(5) . ? N21 C76 1.399(4) . ? N21 C77 1.445(4) . ? C1 C2 1.492(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.391(5) . ? C3 C8 1.408(5) . ? C4 C5 1.386(6) . ? C4 H4A 0.9500 . ? C5 C6 1.403(6) . ? C5 H5A 0.9500 . ? C6 C7 1.377(6) . ? C6 H6A 0.9500 . ? C7 C8 1.395(5) . ? C7 H7A 0.9500 . ? C9 C10 1.497(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.390(5) . ? C11 C16 1.395(5) . ? C12 C13 1.378(5) . ? C12 H12A 0.9500 . ? C13 C14 1.408(6) . ? C13 H13A 0.9500 . ? C14 C15 1.388(6) . ? C14 H14A 0.9500 . ? C15 C16 1.396(5) . ? C15 H15A 0.9500 . ? C17 C18 1.511(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.394(5) . ? C19 C24 1.401(5) . ? C20 C21 1.384(5) . ? C20 H20A 0.9500 . ? C21 C22 1.401(5) . ? C21 H21A 0.9500 . ? C22 C23 1.373(6) . ? C22 H22A 0.9500 . ? C23 C24 1.385(5) . ? C23 H23A 0.9500 . ? C25 C26 1.528(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O2 1.242(4) . ? C26 O1 1.263(4) . ? C27 C28 1.496(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C29 C30 1.389(6) . ? C29 C34 1.398(5) . ? C30 C31 1.390(6) . ? C30 H30A 0.9500 . ? C31 C32 1.396(7) . ? C31 H31A 0.9500 . ? C32 C33 1.383(7) . ? C32 H32A 0.9500 . ? C33 C34 1.390(6) . ? C33 H33A 0.9500 . ? C35 C36 1.482(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C37 C38 1.372(5) . ? C37 C42 1.413(5) . ? C38 C39 1.394(5) . ? C38 H38A 0.9500 . ? C39 C40 1.411(6) . ? C39 H39A 0.9500 . ? C40 C41 1.367(6) . ? C40 H40A 0.9500 . ? C41 C42 1.389(5) . ? C41 H41A 0.9500 . ? C43 C44 1.489(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C45 C46 1.378(5) . ? C45 C50 1.388(5) . ? C46 C47 1.386(6) . ? C46 H46A 0.9500 . ? C47 C48 1.400(6) . ? C47 H47A 0.9500 . ? C48 C49 1.364(6) . ? C48 H48A 0.9500 . ? C49 C50 1.379(6) . ? C49 H49A 0.9500 . ? C51 C52 1.528(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O4 1.225(5) . ? C52 O3 1.275(5) . ? C53 C54 1.507(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C55 C56 1.391(6) . ? C55 C60 1.400(6) . ? C56 C57 1.372(7) . ? C56 H56A 0.9500 . ? C57 C58 1.414(8) . ? C57 H57A 0.9500 . ? C58 C59 1.384(7) . ? C58 H58A 0.9500 . ? C59 C60 1.392(6) . ? C59 H59A 0.9500 . ? C61 C62 1.510(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C63 C68 1.387(7) . ? C63 C64 1.390(7) . ? C64 C65 1.383(7) . ? C64 H64A 0.9500 . ? C65 C66 1.376(10) . ? C65 H65A 0.9500 . ? C66 C67 1.325(9) . ? C66 H66A 0.9500 . ? C67 C68 1.401(7) . ? C67 H67A 0.9500 . ? C69 C70 1.497(5) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C71 C76 1.388(5) . ? C71 C72 1.405(5) . ? C72 C73 1.385(6) . ? C72 H72A 0.9500 . ? C73 C74 1.394(6) . ? C73 H73A 0.9500 . ? C74 C75 1.386(6) . ? C74 H74A 0.9500 . ? C75 C76 1.386(5) . ? C75 H75A 0.9500 . ? C77 C78 1.521(4) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 O6 1.233(4) . ? C78 O5 1.275(4) . ? Si1 F3 1.661(3) . ? Si1 F1 1.676(3) . ? Si1 F4 1.680(3) . ? Si1 F2 1.688(2) . ? Si1 F5 1.691(3) . ? Si1 F6 1.703(2) . ? Si2 F7 1.673(2) 2_556 ? Si2 F7 1.673(2) . ? Si2 F9 1.686(2) . ? Si2 F9 1.686(2) 2_556 ? Si2 F8 1.691(2) 2_556 ? Si2 F8 1.691(2) . ? N22 C79 1.144(6) . ? C79 C80 1.451(6) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? O1W C1W 1.264(6) . ? O1W H1W 0.8400 . ? C1W H1W1 0.9800 . ? C1W H1W2 0.9800 . ? C1W H1W3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Cu1 N4 95.68(11) . . ? N6 Cu1 O5 92.24(10) . . ? N4 Cu1 O5 156.82(10) . . ? N6 Cu1 N2 143.45(11) . . ? N4 Cu1 N2 97.97(11) . . ? O5 Cu1 N2 88.33(10) . . ? N6 Cu1 O6 108.65(10) . . ? N4 Cu1 O6 99.60(9) . . ? O5 Cu1 O6 57.22(8) . . ? N2 Cu1 O6 102.26(10) . . ? N13 Cu2 N11 96.01(13) . . ? N13 Cu2 N9 143.23(13) . . ? N11 Cu2 N9 99.24(12) . . ? N13 Cu2 O1 92.11(11) . . ? N11 Cu2 O1 150.98(11) . . ? N9 Cu2 O1 90.49(11) . . ? N13 Cu2 O2 112.85(11) . . ? N11 Cu2 O2 96.47(10) . . ? N9 Cu2 O2 98.44(11) . . ? O1 Cu2 O2 54.88(8) . . ? O3 Cu3 N20 91.65(12) . . ? O3 Cu3 N16 90.96(13) . . ? N20 Cu3 N16 144.57(12) . . ? O3 Cu3 N18 149.29(13) . . ? N20 Cu3 N18 95.63(13) . . ? N16 Cu3 N18 99.90(14) . . ? O3 Cu3 N15 134.26(11) . . ? N20 Cu3 N15 77.43(11) . . ? N16 Cu3 N15 75.60(12) . . ? N18 Cu3 N15 76.43(13) . . ? O3 Cu3 O4 52.63(10) . . ? N20 Cu3 O4 110.40(12) . . ? N16 Cu3 O4 99.08(13) . . ? N18 Cu3 O4 97.07(12) . . ? N15 Cu3 O4 170.52(11) . . ? C1 N1 C17 115.6(3) . . ? C1 N1 C9 113.0(3) . . ? C17 N1 C9 115.3(3) . . ? C2 N2 C3 106.0(3) . . ? C2 N2 Cu1 116.8(2) . . ? C3 N2 Cu1 133.8(2) . . ? C2 N3 C8 107.9(3) . . ? C2 N3 H3A 126.1 . . ? C8 N3 H3A 126.1 . . ? C10 N4 C11 106.1(3) . . ? C10 N4 Cu1 121.6(2) . . ? C11 N4 Cu1 132.1(2) . . ? C10 N5 C16 107.4(3) . . ? C10 N5 H5B 126.3 . . ? C16 N5 H5B 126.3 . . ? C18 N6 C19 106.1(3) . . ? C18 N6 Cu1 120.5(2) . . ? C19 N6 Cu1 132.2(2) . . ? C18 N7 C24 107.1(3) . . ? C18 N7 C25 127.1(3) . . ? C24 N7 C25 125.5(3) . . ? C27 N8 C43 115.4(3) . . ? C27 N8 C35 114.4(3) . . ? C43 N8 C35 113.5(3) . . ? C28 N9 C29 105.3(3) . . ? C28 N9 Cu2 117.0(3) . . ? C29 N9 Cu2 133.0(2) . . ? C28 N10 C34 108.1(3) . . ? C28 N10 H10A 126.0 . . ? C34 N10 H10A 126.0 . . ? C36 N11 C37 106.0(3) . . ? C36 N11 Cu2 120.6(3) . . ? C37 N11 Cu2 133.1(2) . . ? C36 N12 C42 108.4(3) . . ? C36 N12 H12B 125.8 . . ? C42 N12 H12B 125.8 . . ? C44 N13 C45 105.7(3) . . ? C44 N13 Cu2 119.1(3) . . ? C45 N13 Cu2 134.1(2) . . ? C44 N14 C50 107.1(3) . . ? C44 N14 C51 126.3(3) . . ? C50 N14 C51 126.4(4) . . ? C53 N15 C61 113.2(3) . . ? C53 N15 C69 114.7(3) . . ? C61 N15 C69 113.6(3) . . ? C53 N15 Cu3 102.0(2) . . ? C61 N15 Cu3 104.9(2) . . ? C69 N15 Cu3 107.1(2) . . ? C54 N16 C55 105.0(3) . . ? C54 N16 Cu3 116.4(3) . . ? C55 N16 Cu3 135.8(3) . . ? C54 N17 C60 108.4(3) . . ? C54 N17 H17C 125.8 . . ? C60 N17 H17C 125.8 . . ? C62 N18 C63 106.2(4) . . ? C62 N18 Cu3 119.0(3) . . ? C63 N18 Cu3 133.4(3) . . ? C62 N19 C68 107.0(4) . . ? C62 N19 H19A 126.5 . . ? C68 N19 H19A 126.5 . . ? C70 N20 C71 105.2(3) . . ? C70 N20 Cu3 118.8(3) . . ? C71 N20 Cu3 134.6(2) . . ? C70 N21 C76 107.4(3) . . ? C70 N21 C77 126.7(3) . . ? C76 N21 C77 125.7(3) . . ? N1 C1 C2 109.3(3) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 112.4(3) . . ? N2 C2 C1 124.3(3) . . ? N3 C2 C1 123.3(3) . . ? C4 C3 N2 130.9(3) . . ? C4 C3 C8 120.8(3) . . ? N2 C3 C8 108.2(3) . . ? C5 C4 C3 117.1(4) . . ? C5 C4 H4A 121.5 . . ? C3 C4 H4A 121.5 . . ? C4 C5 C6 121.5(4) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C7 C6 C5 122.3(4) . . ? C7 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? C6 C7 C8 116.2(4) . . ? C6 C7 H7A 121.9 . . ? C8 C7 H7A 121.9 . . ? N3 C8 C7 132.3(4) . . ? N3 C8 C3 105.6(3) . . ? C7 C8 C3 122.1(4) . . ? N1 C9 C10 110.8(3) . . ? N1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N4 C10 N5 112.5(3) . . ? N4 C10 C9 123.7(3) . . ? N5 C10 C9 123.9(3) . . ? C12 C11 C16 121.0(3) . . ? C12 C11 N4 130.6(3) . . ? C16 C11 N4 108.4(3) . . ? C13 C12 C11 117.3(4) . . ? C13 C12 H12A 121.4 . . ? C11 C12 H12A 121.4 . . ? C12 C13 C14 121.4(4) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C15 C14 C13 122.0(4) . . ? C15 C14 H14A 119.0 . . ? C13 C14 H14A 119.0 . . ? C14 C15 C16 115.7(4) . . ? C14 C15 H15A 122.2 . . ? C16 C15 H15A 122.2 . . ? N5 C16 C11 105.7(3) . . ? N5 C16 C15 131.8(3) . . ? C11 C16 C15 122.6(4) . . ? N1 C17 C18 111.4(3) . . ? N1 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N1 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? N6 C18 N7 112.5(3) . . ? N6 C18 C17 125.2(3) . . ? N7 C18 C17 122.4(3) . . ? C20 C19 N6 130.6(3) . . ? C20 C19 C24 120.4(3) . . ? N6 C19 C24 109.0(3) . . ? C21 C20 C19 117.3(3) . . ? C21 C20 H20A 121.3 . . ? C19 C20 H20A 121.3 . . ? C20 C21 C22 121.3(4) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C23 C22 C21 121.9(4) . . ? C23 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C22 C23 C24 116.8(3) . . ? C22 C23 H23A 121.6 . . ? C24 C23 H23A 121.6 . . ? C23 C24 C19 122.3(3) . . ? C23 C24 N7 132.4(3) . . ? C19 C24 N7 105.3(3) . . ? N7 C25 C26 114.4(3) . . ? N7 C25 H25A 108.7 . . ? C26 C25 H25A 108.7 . . ? N7 C25 H25B 108.7 . . ? C26 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? O2 C26 O1 124.7(3) . . ? O2 C26 C25 116.7(3) . . ? O1 C26 C25 118.5(3) . . ? N8 C27 C28 110.1(3) . . ? N8 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? N8 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? N9 C28 N10 112.5(4) . . ? N9 C28 C27 123.6(3) . . ? N10 C28 C27 123.8(4) . . ? C30 C29 N9 130.2(4) . . ? C30 C29 C34 120.7(4) . . ? N9 C29 C34 109.1(3) . . ? C29 C30 C31 117.4(4) . . ? C29 C30 H30A 121.3 . . ? C31 C30 H30A 121.3 . . ? C30 C31 C32 121.6(4) . . ? C30 C31 H31A 119.2 . . ? C32 C31 H31A 119.2 . . ? C33 C32 C31 121.1(5) . . ? C33 C32 H32A 119.4 . . ? C31 C32 H32A 119.4 . . ? C32 C33 C34 117.4(4) . . ? C32 C33 H33A 121.3 . . ? C34 C33 H33A 121.3 . . ? N10 C34 C33 133.3(4) . . ? N10 C34 C29 105.0(3) . . ? C33 C34 C29 121.7(4) . . ? N8 C35 C36 110.7(3) . . ? N8 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? N8 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? N11 C36 N12 111.7(4) . . ? N11 C36 C35 123.2(3) . . ? N12 C36 C35 124.9(3) . . ? C38 C37 N11 130.2(3) . . ? C38 C37 C42 121.6(3) . . ? N11 C37 C42 108.3(3) . . ? C37 C38 C39 116.9(4) . . ? C37 C38 H38A 121.5 . . ? C39 C38 H38A 121.5 . . ? C38 C39 C40 121.5(4) . . ? C38 C39 H39A 119.2 . . ? C40 C39 H39A 119.2 . . ? C41 C40 C39 121.3(4) . . ? C41 C40 H40A 119.4 . . ? C39 C40 H40A 119.4 . . ? C40 C41 C42 117.6(3) . . ? C40 C41 H41A 121.2 . . ? C42 C41 H41A 121.2 . . ? N12 C42 C41 133.2(3) . . ? N12 C42 C37 105.6(3) . . ? C41 C42 C37 121.1(4) . . ? N8 C43 C44 111.9(3) . . ? N8 C43 H43A 109.2 . . ? C44 C43 H43A 109.2 . . ? N8 C43 H43B 109.2 . . ? C44 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? N13 C44 N14 112.3(3) . . ? N13 C44 C43 126.0(4) . . ? N14 C44 C43 121.7(3) . . ? C46 C45 C50 120.0(4) . . ? C46 C45 N13 130.8(4) . . ? C50 C45 N13 109.2(3) . . ? C45 C46 C47 117.4(4) . . ? C45 C46 H46A 121.3 . . ? C47 C46 H46A 121.3 . . ? C46 C47 C48 121.3(4) . . ? C46 C47 H47A 119.3 . . ? C48 C47 H47A 119.3 . . ? C49 C48 C47 121.5(4) . . ? C49 C48 H48A 119.3 . . ? C47 C48 H48A 119.3 . . ? C48 C49 C50 116.5(4) . . ? C48 C49 H49A 121.8 . . ? C50 C49 H49A 121.8 . . ? C49 C50 C45 123.2(4) . . ? C49 C50 N14 131.2(4) . . ? C45 C50 N14 105.6(3) . . ? N14 C51 C52 114.4(3) . . ? N14 C51 H51A 108.7 . . ? C52 C51 H51A 108.7 . . ? N14 C51 H51B 108.7 . . ? C52 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? O4 C52 O3 125.0(4) . . ? O4 C52 C51 117.4(4) . . ? O3 C52 C51 117.6(4) . . ? N15 C53 C54 109.4(3) . . ? N15 C53 H53A 109.8 . . ? C54 C53 H53A 109.8 . . ? N15 C53 H53B 109.8 . . ? C54 C53 H53B 109.8 . . ? H53A C53 H53B 108.3 . . ? N16 C54 N17 112.6(4) . . ? N16 C54 C53 123.3(4) . . ? N17 C54 C53 124.1(3) . . ? C56 C55 N16 131.0(4) . . ? C56 C55 C60 120.1(4) . . ? N16 C55 C60 108.9(3) . . ? C57 C56 C55 117.7(4) . . ? C57 C56 H56A 121.2 . . ? C55 C56 H56A 121.2 . . ? C56 C57 C58 122.2(5) . . ? C56 C57 H57A 118.9 . . ? C58 C57 H57A 118.9 . . ? C59 C58 C57 120.7(5) . . ? C59 C58 H58A 119.7 . . ? C57 C58 H58A 119.7 . . ? C58 C59 C60 116.6(5) . . ? C58 C59 H59A 121.7 . . ? C60 C59 H59A 121.7 . . ? N17 C60 C59 132.2(4) . . ? N17 C60 C55 105.0(4) . . ? C59 C60 C55 122.8(4) . . ? N15 C61 C62 109.0(3) . . ? N15 C61 H61A 109.9 . . ? C62 C61 H61A 109.9 . . ? N15 C61 H61B 109.9 . . ? C62 C61 H61B 109.9 . . ? H61A C61 H61B 108.3 . . ? N18 C62 N19 112.3(4) . . ? N18 C62 C61 122.8(4) . . ? N19 C62 C61 124.8(4) . . ? C68 C63 C64 120.9(4) . . ? C68 C63 N18 108.6(4) . . ? C64 C63 N18 130.5(4) . . ? C65 C64 C63 116.5(6) . . ? C65 C64 H64A 121.8 . . ? C63 C64 H64A 121.8 . . ? C66 C65 C64 121.9(6) . . ? C66 C65 H65A 119.1 . . ? C64 C65 H65A 119.1 . . ? C67 C66 C65 122.1(5) . . ? C67 C66 H66A 118.9 . . ? C65 C66 H66A 118.9 . . ? C66 C67 C68 118.2(6) . . ? C66 C67 H67A 120.9 . . ? C68 C67 H67A 120.9 . . ? N19 C68 C63 105.9(4) . . ? N19 C68 C67 133.6(5) . . ? C63 C68 C67 120.5(6) . . ? N15 C69 C70 110.4(3) . . ? N15 C69 H69A 109.6 . . ? C70 C69 H69A 109.6 . . ? N15 C69 H69B 109.6 . . ? C70 C69 H69B 109.6 . . ? H69A C69 H69B 108.1 . . ? N20 C70 N21 112.5(3) . . ? N20 C70 C69 125.5(4) . . ? N21 C70 C69 122.0(3) . . ? C76 C71 N20 109.5(3) . . ? C76 C71 C72 120.0(4) . . ? N20 C71 C72 130.5(4) . . ? C73 C72 C71 116.6(4) . . ? C73 C72 H72A 121.7 . . ? C71 C72 H72A 121.7 . . ? C72 C73 C74 122.5(4) . . ? C72 C73 H73A 118.8 . . ? C74 C73 H73A 118.8 . . ? C75 C74 C73 121.2(4) . . ? C75 C74 H74A 119.4 . . ? C73 C74 H74A 119.4 . . ? C76 C75 C74 116.2(4) . . ? C76 C75 H75A 121.9 . . ? C74 C75 H75A 121.9 . . ? C75 C76 C71 123.4(3) . . ? C75 C76 N21 131.1(3) . . ? C71 C76 N21 105.4(3) . . ? N21 C77 C78 114.6(3) . . ? N21 C77 H77A 108.6 . . ? C78 C77 H77A 108.6 . . ? N21 C77 H77B 108.6 . . ? C78 C77 H77B 108.6 . . ? H77A C77 H77B 107.6 . . ? O6 C78 O5 123.7(3) . . ? O6 C78 C77 117.8(3) . . ? O5 C78 C77 118.5(3) . . ? C26 O1 Cu2 104.8(2) . . ? C26 O2 Cu2 75.6(2) . . ? C52 O3 Cu3 109.2(3) . . ? C52 O4 Cu3 73.2(3) . . ? C78 O5 Cu1 100.8(2) . . ? C78 O6 Cu1 78.18(19) . . ? F3 Si1 F1 90.65(14) . . ? F3 Si1 F4 91.15(13) . . ? F1 Si1 F4 90.71(14) . . ? F3 Si1 F2 90.70(13) . . ? F1 Si1 F2 178.22(15) . . ? F4 Si1 F2 90.43(14) . . ? F3 Si1 F5 179.37(15) . . ? F1 Si1 F5 89.00(14) . . ? F4 Si1 F5 89.37(13) . . ? F2 Si1 F5 89.64(13) . . ? F3 Si1 F6 89.36(13) . . ? F1 Si1 F6 89.34(13) . . ? F4 Si1 F6 179.49(16) . . ? F2 Si1 F6 89.51(13) . . ? F5 Si1 F6 90.12(13) . . ? F7 Si2 F7 178.20(18) 2_556 . ? F7 Si2 F9 91.09(11) 2_556 . ? F7 Si2 F9 90.19(11) . . ? F7 Si2 F9 90.19(11) 2_556 2_556 ? F7 Si2 F9 91.09(11) . 2_556 ? F9 Si2 F9 89.66(16) . 2_556 ? F7 Si2 F8 89.83(11) 2_556 2_556 ? F7 Si2 F8 88.90(11) . 2_556 ? F9 Si2 F8 179.08(11) . 2_556 ? F9 Si2 F8 90.23(11) 2_556 2_556 ? F7 Si2 F8 88.90(11) 2_556 . ? F7 Si2 F8 89.83(11) . . ? F9 Si2 F8 90.23(11) . . ? F9 Si2 F8 179.08(11) 2_556 . ? F8 Si2 F8 89.90(16) 2_556 . ? N22 C79 C80 179.7(5) . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C1W O1W H1W 109.5 . . ? O1W C1W H1W1 109.5 . . ? O1W C1W H1W2 109.5 . . ? H1W1 C1W H1W2 109.5 . . ? O1W C1W H1W3 109.5 . . ? H1W1 C1W H1W3 109.5 . . ? H1W2 C1W H1W3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Cu1 N2 C2 -14.3(3) . . . . ? N4 Cu1 N2 C2 96.6(2) . . . . ? O5 Cu1 N2 C2 -105.8(2) . . . . ? O6 Cu1 N2 C2 -161.7(2) . . . . ? N6 Cu1 N2 C3 141.4(3) . . . . ? N4 Cu1 N2 C3 -107.7(3) . . . . ? O5 Cu1 N2 C3 49.9(3) . . . . ? O6 Cu1 N2 C3 -6.0(3) . . . . ? N6 Cu1 N4 C10 87.6(3) . . . . ? O5 Cu1 N4 C10 -163.0(2) . . . . ? N2 Cu1 N4 C10 -58.4(3) . . . . ? O6 Cu1 N4 C10 -162.4(2) . . . . ? N6 Cu1 N4 C11 -98.5(3) . . . . ? O5 Cu1 N4 C11 10.9(5) . . . . ? N2 Cu1 N4 C11 115.5(3) . . . . ? O6 Cu1 N4 C11 11.5(3) . . . . ? N4 Cu1 N6 C18 -80.6(3) . . . . ? O5 Cu1 N6 C18 121.3(2) . . . . ? N2 Cu1 N6 C18 31.0(3) . . . . ? O6 Cu1 N6 C18 177.3(2) . . . . ? N4 Cu1 N6 C19 113.5(3) . . . . ? O5 Cu1 N6 C19 -44.6(3) . . . . ? N2 Cu1 N6 C19 -134.8(3) . . . . ? O6 Cu1 N6 C19 11.4(3) . . . . ? N13 Cu2 N9 C28 -14.7(4) . . . . ? N11 Cu2 N9 C28 98.6(3) . . . . ? O1 Cu2 N9 C28 -108.9(3) . . . . ? O2 Cu2 N9 C28 -163.4(3) . . . . ? N13 Cu2 N9 C29 136.8(3) . . . . ? N11 Cu2 N9 C29 -109.9(3) . . . . ? O1 Cu2 N9 C29 42.6(3) . . . . ? O2 Cu2 N9 C29 -11.9(3) . . . . ? N13 Cu2 N11 C36 79.2(3) . . . . ? N9 Cu2 N11 C36 -67.3(3) . . . . ? O1 Cu2 N11 C36 -175.4(3) . . . . ? O2 Cu2 N11 C36 -166.9(3) . . . . ? N13 Cu2 N11 C37 -94.5(3) . . . . ? N9 Cu2 N11 C37 119.0(3) . . . . ? O1 Cu2 N11 C37 10.9(5) . . . . ? O2 Cu2 N11 C37 19.4(3) . . . . ? N11 Cu2 N13 C44 -80.1(3) . . . . ? N9 Cu2 N13 C44 34.2(4) . . . . ? O1 Cu2 N13 C44 127.8(3) . . . . ? O2 Cu2 N13 C44 -179.7(2) . . . . ? N11 Cu2 N13 C45 113.7(3) . . . . ? N9 Cu2 N13 C45 -132.1(3) . . . . ? O1 Cu2 N13 C45 -38.4(3) . . . . ? O2 Cu2 N13 C45 14.1(3) . . . . ? O3 Cu3 N15 C53 45.2(3) . . . . ? N20 Cu3 N15 C53 125.1(3) . . . . ? N16 Cu3 N15 C53 -31.7(2) . . . . ? N18 Cu3 N15 C53 -135.9(3) . . . . ? O4 Cu3 N15 C53 -88.5(7) . . . . ? O3 Cu3 N15 C61 163.4(3) . . . . ? N20 Cu3 N15 C61 -116.7(3) . . . . ? N16 Cu3 N15 C61 86.5(3) . . . . ? N18 Cu3 N15 C61 -17.7(3) . . . . ? O4 Cu3 N15 C61 29.7(8) . . . . ? O3 Cu3 N15 C69 -75.6(3) . . . . ? N20 Cu3 N15 C69 4.3(2) . . . . ? N16 Cu3 N15 C69 -152.5(3) . . . . ? N18 Cu3 N15 C69 103.3(3) . . . . ? O4 Cu3 N15 C69 150.7(6) . . . . ? O3 Cu3 N16 C54 -111.7(3) . . . . ? N20 Cu3 N16 C54 -17.5(4) . . . . ? N18 Cu3 N16 C54 97.1(3) . . . . ? N15 Cu3 N16 C54 24.0(3) . . . . ? O4 Cu3 N16 C54 -164.0(3) . . . . ? O3 Cu3 N16 C55 46.1(4) . . . . ? N20 Cu3 N16 C55 140.3(3) . . . . ? N18 Cu3 N16 C55 -105.1(4) . . . . ? N15 Cu3 N16 C55 -178.2(4) . . . . ? O4 Cu3 N16 C55 -6.2(4) . . . . ? O3 Cu3 N18 C62 -179.2(3) . . . . ? N20 Cu3 N18 C62 78.0(3) . . . . ? N16 Cu3 N18 C62 -70.1(3) . . . . ? N15 Cu3 N18 C62 2.4(3) . . . . ? O4 Cu3 N18 C62 -170.6(3) . . . . ? O3 Cu3 N18 C63 16.4(6) . . . . ? N20 Cu3 N18 C63 -86.5(4) . . . . ? N16 Cu3 N18 C63 125.5(4) . . . . ? N15 Cu3 N18 C63 -162.1(4) . . . . ? O4 Cu3 N18 C63 24.9(4) . . . . ? O3 Cu3 N20 C70 127.7(3) . . . . ? N16 Cu3 N20 C70 33.8(4) . . . . ? N18 Cu3 N20 C70 -82.1(3) . . . . ? N15 Cu3 N20 C70 -7.4(2) . . . . ? O4 Cu3 N20 C70 178.2(2) . . . . ? O3 Cu3 N20 C71 -36.5(3) . . . . ? N16 Cu3 N20 C71 -130.5(3) . . . . ? N18 Cu3 N20 C71 113.6(3) . . . . ? N15 Cu3 N20 C71 -171.7(3) . . . . ? O4 Cu3 N20 C71 13.9(3) . . . . ? C17 N1 C1 C2 147.1(3) . . . . ? C9 N1 C1 C2 -77.1(3) . . . . ? C3 N2 C2 N3 1.1(4) . . . . ? Cu1 N2 C2 N3 163.1(2) . . . . ? C3 N2 C2 C1 -175.1(3) . . . . ? Cu1 N2 C2 C1 -13.1(4) . . . . ? C8 N3 C2 N2 -1.6(4) . . . . ? C8 N3 C2 C1 174.7(3) . . . . ? N1 C1 C2 N2 -20.6(5) . . . . ? N1 C1 C2 N3 163.6(3) . . . . ? C2 N2 C3 C4 176.1(4) . . . . ? Cu1 N2 C3 C4 18.6(5) . . . . ? C2 N2 C3 C8 -0.2(4) . . . . ? Cu1 N2 C3 C8 -157.7(2) . . . . ? N2 C3 C4 C5 -176.3(3) . . . . ? C8 C3 C4 C5 -0.4(5) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C4 C5 C6 C7 0.0(6) . . . . ? C5 C6 C7 C8 0.7(6) . . . . ? C2 N3 C8 C7 -177.1(4) . . . . ? C2 N3 C8 C3 1.3(4) . . . . ? C6 C7 C8 N3 177.0(4) . . . . ? C6 C7 C8 C3 -1.3(6) . . . . ? C4 C3 C8 N3 -177.5(3) . . . . ? N2 C3 C8 N3 -0.7(4) . . . . ? C4 C3 C8 C7 1.2(5) . . . . ? N2 C3 C8 C7 177.9(3) . . . . ? C1 N1 C9 C10 128.3(3) . . . . ? C17 N1 C9 C10 -95.7(3) . . . . ? C11 N4 C10 N5 -0.9(4) . . . . ? Cu1 N4 C10 N5 174.4(2) . . . . ? C11 N4 C10 C9 179.0(3) . . . . ? Cu1 N4 C10 C9 -5.7(5) . . . . ? C16 N5 C10 N4 0.0(4) . . . . ? C16 N5 C10 C9 -179.9(3) . . . . ? N1 C9 C10 N4 -13.3(5) . . . . ? N1 C9 C10 N5 166.6(3) . . . . ? C10 N4 C11 C12 -177.8(4) . . . . ? Cu1 N4 C11 C12 7.6(5) . . . . ? C10 N4 C11 C16 1.3(4) . . . . ? Cu1 N4 C11 C16 -173.3(2) . . . . ? C16 C11 C12 C13 0.8(5) . . . . ? N4 C11 C12 C13 179.8(3) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C12 C13 C14 C15 -0.1(7) . . . . ? C13 C14 C15 C16 -0.6(6) . . . . ? C10 N5 C16 C11 0.8(4) . . . . ? C10 N5 C16 C15 -179.8(4) . . . . ? C12 C11 C16 N5 177.9(3) . . . . ? N4 C11 C16 N5 -1.3(4) . . . . ? C12 C11 C16 C15 -1.6(5) . . . . ? N4 C11 C16 C15 179.2(3) . . . . ? C14 C15 C16 N5 -177.9(4) . . . . ? C14 C15 C16 C11 1.5(6) . . . . ? C1 N1 C17 C18 -111.4(3) . . . . ? C9 N1 C17 C18 113.8(3) . . . . ? C19 N6 C18 N7 -0.5(4) . . . . ? Cu1 N6 C18 N7 -169.7(2) . . . . ? C19 N6 C18 C17 179.5(3) . . . . ? Cu1 N6 C18 C17 10.3(4) . . . . ? C24 N7 C18 N6 1.5(4) . . . . ? C25 N7 C18 N6 174.9(3) . . . . ? C24 N7 C18 C17 -178.4(3) . . . . ? C25 N7 C18 C17 -5.1(5) . . . . ? N1 C17 C18 N6 -5.3(5) . . . . ? N1 C17 C18 N7 174.7(3) . . . . ? C18 N6 C19 C20 -179.1(3) . . . . ? Cu1 N6 C19 C20 -11.8(5) . . . . ? C18 N6 C19 C24 -0.7(4) . . . . ? Cu1 N6 C19 C24 166.7(2) . . . . ? N6 C19 C20 C21 175.6(3) . . . . ? C24 C19 C20 C21 -2.7(5) . . . . ? C19 C20 C21 C22 1.1(5) . . . . ? C20 C21 C22 C23 0.7(6) . . . . ? C21 C22 C23 C24 -0.9(6) . . . . ? C22 C23 C24 C19 -0.6(5) . . . . ? C22 C23 C24 N7 -177.6(3) . . . . ? C20 C19 C24 C23 2.5(5) . . . . ? N6 C19 C24 C23 -176.1(3) . . . . ? C20 C19 C24 N7 -179.8(3) . . . . ? N6 C19 C24 N7 1.6(3) . . . . ? C18 N7 C24 C23 175.5(4) . . . . ? C25 N7 C24 C23 2.0(6) . . . . ? C18 N7 C24 C19 -1.9(3) . . . . ? C25 N7 C24 C19 -175.4(3) . . . . ? C18 N7 C25 C26 -80.9(4) . . . . ? C24 N7 C25 C26 91.3(4) . . . . ? N7 C25 C26 O2 -170.0(3) . . . . ? N7 C25 C26 O1 10.8(5) . . . . ? C43 N8 C27 C28 143.3(3) . . . . ? C35 N8 C27 C28 -82.3(4) . . . . ? C29 N9 C28 N10 -0.3(4) . . . . ? Cu2 N9 C28 N10 158.5(3) . . . . ? C29 N9 C28 C27 -177.2(3) . . . . ? Cu2 N9 C28 C27 -18.4(5) . . . . ? C34 N10 C28 N9 0.0(4) . . . . ? C34 N10 C28 C27 177.0(4) . . . . ? N8 C27 C28 N9 -13.8(5) . . . . ? N8 C27 C28 N10 169.6(3) . . . . ? C28 N9 C29 C30 -177.9(4) . . . . ? Cu2 N9 C29 C30 28.3(6) . . . . ? C28 N9 C29 C34 0.4(4) . . . . ? Cu2 N9 C29 C34 -153.4(3) . . . . ? N9 C29 C30 C31 -178.5(4) . . . . ? C34 C29 C30 C31 3.4(6) . . . . ? C29 C30 C31 C32 -0.3(7) . . . . ? C30 C31 C32 C33 -1.7(8) . . . . ? C31 C32 C33 C34 0.5(7) . . . . ? C28 N10 C34 C33 -176.5(4) . . . . ? C28 N10 C34 C29 0.3(4) . . . . ? C32 C33 C34 N10 179.0(4) . . . . ? C32 C33 C34 C29 2.7(6) . . . . ? C30 C29 C34 N10 178.1(3) . . . . ? N9 C29 C34 N10 -0.4(4) . . . . ? C30 C29 C34 C33 -4.7(6) . . . . ? N9 C29 C34 C33 176.8(4) . . . . ? C27 N8 C35 C36 133.5(4) . . . . ? C43 N8 C35 C36 -91.3(4) . . . . ? C37 N11 C36 N12 0.4(4) . . . . ? Cu2 N11 C36 N12 -174.8(2) . . . . ? C37 N11 C36 C35 -175.1(4) . . . . ? Cu2 N11 C36 C35 9.6(5) . . . . ? C42 N12 C36 N11 -0.6(4) . . . . ? C42 N12 C36 C35 174.8(4) . . . . ? N8 C35 C36 N11 -24.7(6) . . . . ? N8 C35 C36 N12 160.4(4) . . . . ? C36 N11 C37 C38 178.7(4) . . . . ? Cu2 N11 C37 C38 -6.9(6) . . . . ? C36 N11 C37 C42 0.0(4) . . . . ? Cu2 N11 C37 C42 174.4(3) . . . . ? N11 C37 C38 C39 -178.3(4) . . . . ? C42 C37 C38 C39 0.3(6) . . . . ? C37 C38 C39 C40 0.4(6) . . . . ? C38 C39 C40 C41 -1.2(7) . . . . ? C39 C40 C41 C42 1.2(6) . . . . ? C36 N12 C42 C41 -178.1(4) . . . . ? C36 N12 C42 C37 0.6(4) . . . . ? C40 C41 C42 N12 178.1(4) . . . . ? C40 C41 C42 C37 -0.5(6) . . . . ? C38 C37 C42 N12 -179.2(3) . . . . ? N11 C37 C42 N12 -0.3(4) . . . . ? C38 C37 C42 C41 -0.3(6) . . . . ? N11 C37 C42 C41 178.5(3) . . . . ? C27 N8 C43 C44 -114.0(4) . . . . ? C35 N8 C43 C44 111.1(4) . . . . ? C45 N13 C44 N14 -1.6(4) . . . . ? Cu2 N13 C44 N14 -171.4(2) . . . . ? C45 N13 C44 C43 177.3(4) . . . . ? Cu2 N13 C44 C43 7.5(5) . . . . ? C50 N14 C44 N13 2.6(4) . . . . ? C51 N14 C44 N13 178.0(3) . . . . ? C50 N14 C44 C43 -176.3(3) . . . . ? C51 N14 C44 C43 -0.9(6) . . . . ? N8 C43 C44 N13 -2.4(6) . . . . ? N8 C43 C44 N14 176.4(3) . . . . ? C44 N13 C45 C46 -179.7(4) . . . . ? Cu2 N13 C45 C46 -12.2(6) . . . . ? C44 N13 C45 C50 0.0(4) . . . . ? Cu2 N13 C45 C50 167.5(2) . . . . ? C50 C45 C46 C47 -3.4(5) . . . . ? N13 C45 C46 C47 176.2(3) . . . . ? C45 C46 C47 C48 0.7(5) . . . . ? C46 C47 C48 C49 2.3(6) . . . . ? C47 C48 C49 C50 -2.3(5) . . . . ? C48 C49 C50 C45 -0.5(5) . . . . ? C48 C49 C50 N14 -177.7(4) . . . . ? C46 C45 C50 C49 3.4(5) . . . . ? N13 C45 C50 C49 -176.3(3) . . . . ? C46 C45 C50 N14 -178.7(3) . . . . ? N13 C45 C50 N14 1.6(4) . . . . ? C44 N14 C50 C49 175.1(4) . . . . ? C51 N14 C50 C49 -0.3(6) . . . . ? C44 N14 C50 C45 -2.5(4) . . . . ? C51 N14 C50 C45 -177.9(3) . . . . ? C44 N14 C51 C52 -78.9(5) . . . . ? C50 N14 C51 C52 95.6(5) . . . . ? N14 C51 C52 O4 -173.1(4) . . . . ? N14 C51 C52 O3 6.7(6) . . . . ? C61 N15 C53 C54 -79.4(4) . . . . ? C69 N15 C53 C54 148.1(3) . . . . ? Cu3 N15 C53 C54 32.7(4) . . . . ? C55 N16 C54 N17 0.6(4) . . . . ? Cu3 N16 C54 N17 164.7(3) . . . . ? C55 N16 C54 C53 -177.1(4) . . . . ? Cu3 N16 C54 C53 -12.9(5) . . . . ? C60 N17 C54 N16 -1.1(5) . . . . ? C60 N17 C54 C53 176.5(4) . . . . ? N15 C53 C54 N16 -19.1(5) . . . . ? N15 C53 C54 N17 163.5(4) . . . . ? C54 N16 C55 C56 -178.8(5) . . . . ? Cu3 N16 C55 C56 21.7(7) . . . . ? C54 N16 C55 C60 0.1(4) . . . . ? Cu3 N16 C55 C60 -159.4(3) . . . . ? N16 C55 C56 C57 179.9(5) . . . . ? C60 C55 C56 C57 1.0(7) . . . . ? C55 C56 C57 C58 -0.4(9) . . . . ? C56 C57 C58 C59 -0.5(9) . . . . ? C57 C58 C59 C60 0.6(8) . . . . ? C54 N17 C60 C59 -179.8(5) . . . . ? C54 N17 C60 C55 1.1(4) . . . . ? C58 C59 C60 N17 -179.0(5) . . . . ? C58 C59 C60 C55 0.0(7) . . . . ? C56 C55 C60 N17 178.4(4) . . . . ? N16 C55 C60 N17 -0.7(4) . . . . ? C56 C55 C60 C59 -0.9(7) . . . . ? N16 C55 C60 C59 -179.9(4) . . . . ? C53 N15 C61 C62 137.6(4) . . . . ? C69 N15 C61 C62 -89.3(4) . . . . ? Cu3 N15 C61 C62 27.3(4) . . . . ? C63 N18 C62 N19 -1.0(5) . . . . ? Cu3 N18 C62 N19 -169.3(3) . . . . ? C63 N18 C62 C61 -176.8(4) . . . . ? Cu3 N18 C62 C61 14.9(6) . . . . ? C68 N19 C62 N18 1.0(5) . . . . ? C68 N19 C62 C61 176.7(4) . . . . ? N15 C61 C62 N18 -31.3(6) . . . . ? N15 C61 C62 N19 153.4(4) . . . . ? C62 N18 C63 C68 0.5(5) . . . . ? Cu3 N18 C63 C68 166.4(3) . . . . ? C62 N18 C63 C64 -178.0(5) . . . . ? Cu3 N18 C63 C64 -12.1(7) . . . . ? C68 C63 C64 C65 0.7(7) . . . . ? N18 C63 C64 C65 179.1(5) . . . . ? C63 C64 C65 C66 -1.4(8) . . . . ? C64 C65 C66 C67 1.4(10) . . . . ? C65 C66 C67 C68 -0.6(9) . . . . ? C62 N19 C68 C63 -0.6(5) . . . . ? C62 N19 C68 C67 177.9(5) . . . . ? C64 C63 C68 N19 178.8(4) . . . . ? N18 C63 C68 N19 0.1(5) . . . . ? C64 C63 C68 C67 0.0(7) . . . . ? N18 C63 C68 C67 -178.7(4) . . . . ? C66 C67 C68 N19 -178.5(5) . . . . ? C66 C67 C68 C63 -0.1(8) . . . . ? C53 N15 C69 C70 -113.2(4) . . . . ? C61 N15 C69 C70 114.4(4) . . . . ? Cu3 N15 C69 C70 -0.9(4) . . . . ? C71 N20 C70 N21 -0.6(4) . . . . ? Cu3 N20 C70 N21 -169.0(2) . . . . ? C71 N20 C70 C69 178.9(3) . . . . ? Cu3 N20 C70 C69 10.4(5) . . . . ? C76 N21 C70 N20 0.9(4) . . . . ? C77 N21 C70 N20 175.7(3) . . . . ? C76 N21 C70 C69 -178.6(3) . . . . ? C77 N21 C70 C69 -3.7(5) . . . . ? N15 C69 C70 N20 -5.5(5) . . . . ? N15 C69 C70 N21 173.8(3) . . . . ? C70 N20 C71 C76 0.1(4) . . . . ? Cu3 N20 C71 C76 165.8(2) . . . . ? C70 N20 C71 C72 179.5(4) . . . . ? Cu3 N20 C71 C72 -14.7(6) . . . . ? C76 C71 C72 C73 -1.6(5) . . . . ? N20 C71 C72 C73 179.0(3) . . . . ? C71 C72 C73 C74 0.4(6) . . . . ? C72 C73 C74 C75 0.1(6) . . . . ? C73 C74 C75 C76 0.5(6) . . . . ? C74 C75 C76 C71 -1.8(5) . . . . ? C74 C75 C76 N21 -179.9(3) . . . . ? N20 C71 C76 C75 -178.1(3) . . . . ? C72 C71 C76 C75 2.4(5) . . . . ? N20 C71 C76 N21 0.4(4) . . . . ? C72 C71 C76 N21 -179.1(3) . . . . ? C70 N21 C76 C75 177.6(4) . . . . ? C77 N21 C76 C75 2.7(6) . . . . ? C70 N21 C76 C71 -0.8(4) . . . . ? C77 N21 C76 C71 -175.7(3) . . . . ? C70 N21 C77 C78 -80.1(4) . . . . ? C76 N21 C77 C78 93.8(4) . . . . ? N21 C77 C78 O6 -167.4(3) . . . . ? N21 C77 C78 O5 14.8(5) . . . . ? O2 C26 O1 Cu2 -2.7(4) . . . . ? C25 C26 O1 Cu2 176.4(3) . . . . ? N13 Cu2 O1 C26 118.0(2) . . . . ? N11 Cu2 O1 C26 11.6(4) . . . . ? N9 Cu2 O1 C26 -98.7(2) . . . . ? O2 Cu2 O1 C26 1.3(2) . . . . ? O1 C26 O2 Cu2 2.1(3) . . . . ? C25 C26 O2 Cu2 -177.0(3) . . . . ? N13 Cu2 O2 C26 -77.0(2) . . . . ? N11 Cu2 O2 C26 -176.3(2) . . . . ? N9 Cu2 O2 C26 83.3(2) . . . . ? O1 Cu2 O2 C26 -1.3(2) . . . . ? O4 C52 O3 Cu3 -0.1(6) . . . . ? C51 C52 O3 Cu3 -179.8(3) . . . . ? N20 Cu3 O3 C52 114.7(3) . . . . ? N16 Cu3 O3 C52 -100.7(3) . . . . ? N18 Cu3 O3 C52 10.7(4) . . . . ? N15 Cu3 O3 C52 -171.4(3) . . . . ? O4 Cu3 O3 C52 0.0(3) . . . . ? O3 C52 O4 Cu3 0.1(4) . . . . ? C51 C52 O4 Cu3 179.8(4) . . . . ? O3 Cu3 O4 C52 0.0(3) . . . . ? N20 Cu3 O4 C52 -75.8(3) . . . . ? N16 Cu3 O4 C52 84.2(3) . . . . ? N18 Cu3 O4 C52 -174.5(3) . . . . ? N15 Cu3 O4 C52 139.3(6) . . . . ? O6 C78 O5 Cu1 -4.1(4) . . . . ? C77 C78 O5 Cu1 173.6(3) . . . . ? N6 Cu1 O5 C78 112.8(2) . . . . ? N4 Cu1 O5 C78 2.8(4) . . . . ? N2 Cu1 O5 C78 -103.8(2) . . . . ? O6 Cu1 O5 C78 2.00(19) . . . . ? O5 C78 O6 Cu1 3.3(3) . . . . ? C77 C78 O6 Cu1 -174.4(3) . . . . ? N6 Cu1 O6 C78 -82.4(2) . . . . ? N4 Cu1 O6 C78 178.2(2) . . . . ? O5 Cu1 O6 C78 -2.1(2) . . . . ? N2 Cu1 O6 C78 77.8(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A F7 0.88 2.11 2.905(4) 150.0 . N3 H3A F8 0.88 2.19 2.842(4) 130.1 . N5 H5B F4 0.88 2.10 2.866(4) 145.0 6_565 N5 H5B F5 0.88 2.17 2.953(4) 147.6 6_565 N10 H10A F9 0.88 2.04 2.895(4) 164.4 . N10 H10A F7 0.88 2.31 2.889(4) 123.4 . N12 H12B F6 0.88 2.11 2.895(4) 147.6 . N12 H12B F3 0.88 2.33 3.006(4) 134.0 . N17 H17C F8 0.88 2.06 2.890(4) 156.5 . N17 H17C F9 0.88 2.28 2.907(4) 128.1 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.931 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.100 #==========# data_3-OTs _database_code_depnum_ccdc_archive 'CCDC 812764' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H33 Cu N7 O6 S' _chemical_formula_weight 731.27 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9659(5) _cell_length_b 13.2766(5) _cell_length_c 18.0272(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.667(3) _cell_angle_gamma 90.00 _cell_volume 3233.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3873 _cell_measurement_theta_min 2.8720 _cell_measurement_theta_max 30.1779 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7406 _exptl_absorpt_correction_T_max 0.9612 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _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 'OXFORD Gemini' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16427 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.1427 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6288 _reflns_number_gt 3215 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _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. ; _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^)+(0.0180P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6288 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.57631(3) 0.16205(3) 0.22376(2) 0.02765(13) Uani 1 1 d . . . S1 S 0.24948(7) 0.50074(8) 0.04806(5) 0.0387(3) Uani 1 1 d . . . N1 N 0.58701(17) 0.0176(2) 0.27752(14) 0.0232(7) Uani 1 1 d . . . N2 N 0.53133(18) 0.1961(2) 0.32217(15) 0.0252(7) Uani 1 1 d . . . N3 N 0.44447(18) 0.1374(2) 0.40063(15) 0.0289(7) Uani 1 1 d . . . H3A H 0.4162 0.0939 0.4252 0.035 Uiso 1 1 calc R . . N4 N 0.48707(17) 0.0795(2) 0.13712(15) 0.0255(7) Uani 1 1 d . . . N5 N 0.4417(2) -0.0727(2) 0.09157(16) 0.0385(8) Uani 1 1 d . . . H5B H 0.4380 -0.1389 0.0893 0.046 Uiso 1 1 calc R . . N6 N 0.72405(18) 0.1284(2) 0.23702(15) 0.0243(7) Uani 1 1 d . . . N7 N 0.85532(19) 0.0458(2) 0.30641(15) 0.0255(7) Uani 1 1 d . . . C1 C 0.5101(2) 0.0129(2) 0.32150(18) 0.0253(9) Uani 1 1 d . . . H1A H 0.4469 -0.0118 0.2882 0.030 Uiso 1 1 calc R . . H1B H 0.5312 -0.0337 0.3655 0.030 Uiso 1 1 calc R . . C2 C 0.4971(2) 0.1155(3) 0.34912(18) 0.0249(9) Uani 1 1 d . . . C3 C 0.5007(2) 0.2773(3) 0.35913(19) 0.0274(9) Uani 1 1 d . . . C4 C 0.5156(2) 0.3811(3) 0.35513(19) 0.0314(9) Uani 1 1 d . . . H4A H 0.5550 0.4077 0.3239 0.038 Uiso 1 1 calc R . . C5 C 0.4720(2) 0.4433(3) 0.3973(2) 0.0397(10) Uani 1 1 d . . . H5A H 0.4822 0.5139 0.3956 0.048 Uiso 1 1 calc R . . C6 C 0.4122(3) 0.4056(3) 0.4434(2) 0.0432(11) Uani 1 1 d . . . H6A H 0.3817 0.4512 0.4711 0.052 Uiso 1 1 calc R . . C7 C 0.3978(3) 0.3039(3) 0.4489(2) 0.0400(10) Uani 1 1 d . . . H7A H 0.3580 0.2775 0.4799 0.048 Uiso 1 1 calc R . . C8 C 0.4437(2) 0.2424(3) 0.40724(19) 0.0279(9) Uani 1 1 d . . . C9 C 0.5702(2) -0.0592(2) 0.21646(18) 0.0296(9) Uani 1 1 d . . . H9A H 0.5440 -0.1217 0.2339 0.036 Uiso 1 1 calc R . . H9B H 0.6333 -0.0754 0.2036 0.036 Uiso 1 1 calc R . . C10 C 0.4979(2) -0.0181(3) 0.14809(19) 0.0270(9) Uani 1 1 d . . . C11 C 0.4183(2) 0.0891(3) 0.0661(2) 0.0303(9) Uani 1 1 d . . . C12 C 0.3792(2) 0.1737(3) 0.0246(2) 0.0391(10) Uani 1 1 d . . . H12A H 0.3976 0.2395 0.0437 0.047 Uiso 1 1 calc R . . C13 C 0.3126(3) 0.1593(4) -0.0456(2) 0.0490(11) Uani 1 1 d . . . H13A H 0.2846 0.2159 -0.0755 0.059 Uiso 1 1 calc R . . C14 C 0.2862(3) 0.0623(4) -0.0728(2) 0.0538(13) Uani 1 1 d . . . H14A H 0.2408 0.0547 -0.1216 0.065 Uiso 1 1 calc R . . C15 C 0.3228(3) -0.0219(3) -0.0325(2) 0.0494(12) Uani 1 1 d . . . H15A H 0.3033 -0.0876 -0.0512 0.059 Uiso 1 1 calc R . . C16 C 0.3903(2) -0.0061(3) 0.0374(2) 0.0356(10) Uani 1 1 d . . . C17 C 0.6868(2) 0.0110(3) 0.32971(17) 0.0269(9) Uani 1 1 d . . . H17A H 0.7056 -0.0603 0.3410 0.032 Uiso 1 1 calc R . . H17B H 0.6886 0.0459 0.3786 0.032 Uiso 1 1 calc R . . C18 C 0.7565(2) 0.0608(3) 0.28958(19) 0.0235(8) Uani 1 1 d . . . C19 C 0.8070(2) 0.1599(3) 0.21374(18) 0.0242(8) Uani 1 1 d . . . C20 C 0.8155(2) 0.2276(3) 0.1573(2) 0.0304(9) Uani 1 1 d . . . H20A H 0.7594 0.2622 0.1273 0.036 Uiso 1 1 calc R . . C21 C 0.9091(3) 0.2430(3) 0.1464(2) 0.0352(10) Uani 1 1 d . . . H21A H 0.9172 0.2870 0.1069 0.042 Uiso 1 1 calc R . . C22 C 0.9913(3) 0.1949(3) 0.1924(2) 0.0420(11) Uani 1 1 d . . . H22A H 1.0548 0.2101 0.1852 0.050 Uiso 1 1 calc R . . C23 C 0.9845(2) 0.1262(3) 0.2481(2) 0.0383(10) Uani 1 1 d . . . H23A H 1.0412 0.0929 0.2784 0.046 Uiso 1 1 calc R . . C24 C 0.8901(2) 0.1082(3) 0.25759(19) 0.0250(9) Uani 1 1 d . . . C25 C 0.9080(2) -0.0404(2) 0.34828(19) 0.0299(9) Uani 1 1 d . . . H25A H 0.8898 -0.0475 0.3977 0.036 Uiso 1 1 calc R . . H25B H 0.9801 -0.0279 0.3597 0.036 Uiso 1 1 calc R . . C26 C 0.8836(3) -0.1393(3) 0.3024(2) 0.0281(9) Uani 1 1 d . . . C27 C 0.2401(2) 0.3856(3) 0.0951(2) 0.0321(10) Uani 1 1 d . . . C28 C 0.2956(3) 0.3690(3) 0.1692(2) 0.0500(12) Uani 1 1 d . . . H28A H 0.3350 0.4213 0.1974 0.060 Uiso 1 1 calc R . . C29 C 0.2929(3) 0.2758(4) 0.2016(2) 0.0569(13) Uani 1 1 d . . . H29A H 0.3300 0.2657 0.2530 0.068 Uiso 1 1 calc R . . C30 C 0.2392(2) 0.1961(3) 0.1633(2) 0.0389(11) Uani 1 1 d . . . C31 C 0.1810(2) 0.2153(3) 0.0887(2) 0.0401(11) Uani 1 1 d . . . H31A H 0.1409 0.1632 0.0609 0.048 Uiso 1 1 calc R . . C32 C 0.1813(2) 0.3089(3) 0.0552(2) 0.0398(11) Uani 1 1 d . . . H32A H 0.1413 0.3207 0.0049 0.048 Uiso 1 1 calc R . . C33 C 0.2443(3) 0.0935(3) 0.1984(2) 0.0571(13) Uani 1 1 d . . . H33A H 0.2869 0.0501 0.1764 0.086 Uiso 1 1 calc R . . H33B H 0.1777 0.0645 0.1878 0.086 Uiso 1 1 calc R . . H33C H 0.2718 0.0986 0.2540 0.086 Uiso 1 1 calc R . . C34 C 0.4634(4) -0.3238(4) 0.0369(3) 0.121(2) Uani 1 1 d . . . H34A H 0.4536 -0.3010 -0.0162 0.181 Uiso 1 1 calc R . . H34B H 0.4494 -0.3961 0.0374 0.181 Uiso 1 1 calc R . . H34C H 0.5320 -0.3112 0.0653 0.181 Uiso 1 1 calc R . . O1 O 0.94133(16) -0.21151(18) 0.32982(12) 0.0317(6) Uani 1 1 d . . . O2 O 0.81341(16) -0.14032(17) 0.24546(13) 0.0347(6) Uani 1 1 d . . . O3 O 0.29193(17) 0.57344(19) 0.10845(13) 0.0500(7) Uani 1 1 d . . . O4 O 0.14734(15) 0.52769(17) 0.00624(12) 0.0376(6) Uani 1 1 d . . . O5 O 0.31243(15) 0.47992(18) -0.00308(12) 0.0409(7) Uani 1 1 d . . . O6 O 0.3999(3) -0.2718(2) 0.0711(2) 0.1016(13) Uani 1 1 d . . . H6 H 0.3619 -0.3127 0.0850 0.152 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 0.0271(2) 0.0294(3) 0.0258(2) 0.0013(3) 0.00535(18) -0.0023(2) S1 0.0369(6) 0.0510(7) 0.0294(6) -0.0071(6) 0.0103(5) -0.0060(6) N1 0.0213(15) 0.0264(19) 0.0216(16) 0.0001(14) 0.0052(13) 0.0002(14) N2 0.0239(16) 0.0257(19) 0.0269(17) -0.0027(16) 0.0079(13) -0.0024(15) N3 0.0297(17) 0.037(2) 0.0232(17) 0.0022(16) 0.0121(13) -0.0003(15) N4 0.0220(16) 0.030(2) 0.0221(17) -0.0010(16) 0.0004(13) -0.0003(15) N5 0.0436(19) 0.036(2) 0.034(2) -0.0064(18) 0.0065(16) -0.0117(18) N6 0.0236(16) 0.0244(19) 0.0246(17) -0.0008(15) 0.0059(13) -0.0022(14) N7 0.0243(17) 0.0248(19) 0.0277(17) 0.0001(15) 0.0072(13) 0.0029(15) C1 0.027(2) 0.023(2) 0.027(2) -0.0001(18) 0.0091(16) 0.0002(18) C2 0.0198(19) 0.035(2) 0.018(2) 0.0035(19) 0.0008(15) 0.0010(18) C3 0.023(2) 0.035(3) 0.023(2) -0.002(2) 0.0030(17) 0.0043(19) C4 0.034(2) 0.034(3) 0.029(2) 0.003(2) 0.0124(18) 0.001(2) C5 0.044(2) 0.031(3) 0.043(3) -0.001(2) 0.010(2) -0.001(2) C6 0.057(3) 0.042(3) 0.035(3) -0.006(2) 0.021(2) 0.012(2) C7 0.039(2) 0.053(3) 0.031(2) 0.001(2) 0.0134(18) 0.005(2) C8 0.027(2) 0.034(3) 0.019(2) -0.002(2) 0.0005(16) 0.002(2) C9 0.031(2) 0.027(2) 0.031(2) -0.003(2) 0.0068(17) -0.007(2) C10 0.025(2) 0.035(3) 0.022(2) -0.003(2) 0.0063(17) -0.010(2) C11 0.021(2) 0.046(3) 0.025(2) 0.003(2) 0.0086(17) 0.001(2) C12 0.035(2) 0.051(3) 0.031(2) 0.000(2) 0.0079(18) 0.008(2) C13 0.039(2) 0.080(4) 0.031(3) 0.017(3) 0.0125(19) 0.019(3) C14 0.034(2) 0.101(4) 0.023(2) -0.005(3) -0.0002(19) 0.000(3) C15 0.043(3) 0.071(4) 0.033(3) -0.011(3) 0.008(2) -0.017(3) C16 0.029(2) 0.049(3) 0.027(2) 0.003(2) 0.0049(18) -0.012(2) C17 0.026(2) 0.029(2) 0.026(2) 0.0059(19) 0.0078(16) 0.0017(18) C18 0.023(2) 0.026(2) 0.022(2) -0.0069(19) 0.0077(16) -0.0016(19) C19 0.031(2) 0.019(2) 0.026(2) -0.009(2) 0.0135(17) -0.006(2) C20 0.033(2) 0.023(2) 0.038(2) -0.011(2) 0.0149(18) -0.0012(18) C21 0.050(3) 0.030(3) 0.033(2) -0.006(2) 0.023(2) -0.006(2) C22 0.036(2) 0.038(3) 0.061(3) -0.010(2) 0.027(2) -0.009(2) C23 0.032(2) 0.037(3) 0.050(3) -0.011(2) 0.0165(19) 0.003(2) C24 0.028(2) 0.020(2) 0.029(2) -0.0076(18) 0.0103(18) -0.0030(18) C25 0.025(2) 0.033(2) 0.031(2) 0.004(2) 0.0069(17) 0.0028(19) C26 0.025(2) 0.037(3) 0.026(2) -0.002(2) 0.0137(18) -0.006(2) C27 0.028(2) 0.043(3) 0.026(2) -0.009(2) 0.0091(18) 0.001(2) C28 0.045(3) 0.060(4) 0.036(3) 0.005(2) -0.008(2) -0.014(2) C29 0.045(3) 0.074(4) 0.039(3) 0.001(3) -0.011(2) -0.010(3) C30 0.021(2) 0.054(3) 0.043(3) 0.005(3) 0.0126(19) 0.004(2) C31 0.035(2) 0.050(3) 0.035(3) 0.002(2) 0.0089(19) -0.012(2) C32 0.029(2) 0.062(3) 0.026(2) -0.006(2) 0.0034(17) -0.006(2) C33 0.035(2) 0.064(3) 0.069(3) 0.013(3) 0.009(2) 0.007(2) C34 0.161(6) 0.130(6) 0.075(4) -0.003(4) 0.038(4) -0.091(5) O1 0.0310(14) 0.0311(16) 0.0300(15) -0.0035(13) 0.0021(11) 0.0062(13) O2 0.0354(14) 0.0404(18) 0.0253(14) -0.0036(13) 0.0018(12) 0.0030(13) O3 0.0573(17) 0.0538(19) 0.0385(16) -0.0168(15) 0.0114(13) -0.0198(15) O4 0.0365(15) 0.0464(18) 0.0308(15) -0.0010(13) 0.0103(12) 0.0052(13) O5 0.0340(14) 0.0612(19) 0.0329(15) 0.0003(14) 0.0184(12) -0.0015(14) O6 0.157(4) 0.063(3) 0.105(3) -0.019(2) 0.069(3) -0.044(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.921(2) 2_655 ? Cu1 N4 2.051(3) . ? Cu1 N6 2.065(2) . ? Cu1 N2 2.076(3) . ? Cu1 N1 2.136(3) . ? S1 O5 1.452(2) . ? S1 O3 1.463(2) . ? S1 O4 1.479(2) . ? S1 C27 1.768(4) . ? N1 C17 1.473(3) . ? N1 C9 1.475(4) . ? N1 C1 1.489(3) . ? N2 C2 1.313(4) . ? N2 C3 1.391(4) . ? N3 C2 1.354(4) . ? N3 C8 1.399(4) . ? N3 H3A 0.8800 . ? N4 C10 1.314(4) . ? N4 C11 1.399(4) . ? N5 C10 1.333(4) . ? N5 C16 1.377(4) . ? N5 H5B 0.8800 . ? N6 C18 1.301(4) . ? N6 C19 1.393(3) . ? N7 C18 1.350(3) . ? N7 C24 1.383(4) . ? N7 C25 1.462(4) . ? C1 C2 1.477(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.399(4) . ? C3 C8 1.397(4) . ? C4 C5 1.365(4) . ? C4 H4A 0.9500 . ? C5 C6 1.410(4) . ? C5 H5A 0.9500 . ? C6 C7 1.372(5) . ? C6 H6A 0.9500 . ? C7 C8 1.373(4) . ? C7 H7A 0.9500 . ? C9 C10 1.485(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.383(5) . ? C11 C16 1.384(5) . ? C12 C13 1.380(5) . ? C12 H12A 0.9500 . ? C13 C14 1.394(5) . ? C13 H13A 0.9500 . ? C14 C15 1.360(5) . ? C14 H14A 0.9500 . ? C15 C16 1.386(5) . ? C15 H15A 0.9500 . ? C17 C18 1.505(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.385(4) . ? C19 C24 1.406(4) . ? C20 C21 1.385(4) . ? C20 H20A 0.9500 . ? C21 C22 1.390(5) . ? C21 H21A 0.9500 . ? C22 C23 1.377(5) . ? C22 H22A 0.9500 . ? C23 C24 1.392(4) . ? C23 H23A 0.9500 . ? C25 C26 1.544(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O2 1.226(4) . ? C26 O1 1.269(4) . ? C27 C28 1.383(5) . ? C27 C32 1.390(4) . ? C28 C29 1.372(5) . ? C28 H28A 0.9500 . ? C29 C30 1.378(5) . ? C29 H29A 0.9500 . ? C30 C31 1.407(5) . ? C30 C33 1.496(5) . ? C31 C32 1.381(5) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 O6 1.386(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O1 Cu1 1.921(2) 2_645 ? O6 H6 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N4 96.21(11) 2_655 . ? O1 Cu1 N6 104.13(10) 2_655 . ? N4 Cu1 N6 111.67(10) . . ? O1 Cu1 N2 102.21(10) 2_655 . ? N4 Cu1 N2 120.66(10) . . ? N6 Cu1 N2 117.25(10) . . ? O1 Cu1 N1 175.98(10) 2_655 . ? N4 Cu1 N1 79.93(11) . . ? N6 Cu1 N1 78.49(10) . . ? N2 Cu1 N1 79.00(10) . . ? O5 S1 O3 113.67(14) . . ? O5 S1 O4 112.54(13) . . ? O3 S1 O4 112.12(14) . . ? O5 S1 C27 105.67(15) . . ? O3 S1 C27 106.18(16) . . ? O4 S1 C27 105.92(15) . . ? C17 N1 C9 112.4(2) . . ? C17 N1 C1 110.5(2) . . ? C9 N1 C1 111.6(2) . . ? C17 N1 Cu1 106.83(19) . . ? C9 N1 Cu1 107.61(18) . . ? C1 N1 Cu1 107.59(19) . . ? C2 N2 C3 105.6(3) . . ? C2 N2 Cu1 110.9(2) . . ? C3 N2 Cu1 140.7(2) . . ? C2 N3 C8 106.8(3) . . ? C2 N3 H3A 126.6 . . ? C8 N3 H3A 126.6 . . ? C10 N4 C11 104.7(3) . . ? C10 N4 Cu1 112.8(2) . . ? C11 N4 Cu1 142.4(3) . . ? C10 N5 C16 107.0(3) . . ? C10 N5 H5B 126.5 . . ? C16 N5 H5B 126.5 . . ? C18 N6 C19 105.2(3) . . ? C18 N6 Cu1 112.8(2) . . ? C19 N6 Cu1 141.6(2) . . ? C18 N7 C24 105.8(3) . . ? C18 N7 C25 125.6(3) . . ? C24 N7 C25 125.8(3) . . ? C2 C1 N1 107.9(3) . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1B 110.1 . . ? N1 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 N3 113.0(3) . . ? N2 C2 C1 122.6(3) . . ? N3 C2 C1 124.2(3) . . ? N2 C3 C4 132.2(3) . . ? N2 C3 C8 109.4(3) . . ? C4 C3 C8 118.4(3) . . ? C5 C4 C3 118.3(3) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C4 C5 C6 121.9(4) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C7 C6 C5 120.7(4) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C6 C7 C8 116.7(3) . . ? C6 C7 H7A 121.6 . . ? C8 C7 H7A 121.6 . . ? C7 C8 N3 130.9(3) . . ? C7 C8 C3 124.0(4) . . ? N3 C8 C3 105.1(3) . . ? N1 C9 C10 108.1(3) . . ? N1 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? N1 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N4 C10 N5 113.5(3) . . ? N4 C10 C9 121.1(3) . . ? N5 C10 C9 125.4(3) . . ? C12 C11 C16 120.3(3) . . ? C12 C11 N4 130.9(4) . . ? C16 C11 N4 108.8(3) . . ? C11 C12 C13 117.7(4) . . ? C11 C12 H12A 121.2 . . ? C13 C12 H12A 121.2 . . ? C12 C13 C14 120.5(4) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 122.7(4) . . ? C15 C14 H14A 118.6 . . ? C13 C14 H14A 118.6 . . ? C14 C15 C16 116.0(4) . . ? C14 C15 H15A 122.0 . . ? C16 C15 H15A 122.0 . . ? N5 C16 C11 106.0(3) . . ? N5 C16 C15 131.3(4) . . ? C11 C16 C15 122.7(4) . . ? N1 C17 C18 106.8(2) . . ? N1 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? N1 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? N6 C18 N7 114.4(3) . . ? N6 C18 C17 120.3(3) . . ? N7 C18 C17 125.2(3) . . ? C20 C19 N6 130.4(3) . . ? C20 C19 C24 121.2(3) . . ? N6 C19 C24 108.4(3) . . ? C19 C20 C21 117.3(3) . . ? C19 C20 H20A 121.3 . . ? C21 C20 H20A 121.3 . . ? C20 C21 C22 121.0(3) . . ? C20 C21 H21A 119.5 . . ? C22 C21 H21A 119.5 . . ? C23 C22 C21 122.6(3) . . ? C23 C22 H22A 118.7 . . ? C21 C22 H22A 118.7 . . ? C22 C23 C24 116.5(3) . . ? C22 C23 H23A 121.8 . . ? C24 C23 H23A 121.8 . . ? N7 C24 C23 132.6(3) . . ? N7 C24 C19 106.1(3) . . ? C23 C24 C19 121.3(3) . . ? N7 C25 C26 112.0(3) . . ? N7 C25 H25A 109.2 . . ? C26 C25 H25A 109.2 . . ? N7 C25 H25B 109.2 . . ? C26 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? O2 C26 O1 127.8(3) . . ? O2 C26 C25 118.6(3) . . ? O1 C26 C25 113.6(3) . . ? C28 C27 C32 119.7(4) . . ? C28 C27 S1 120.7(3) . . ? C32 C27 S1 119.5(3) . . ? C29 C28 C27 119.1(4) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C28 C29 C30 123.3(4) . . ? C28 C29 H29A 118.3 . . ? C30 C29 H29A 118.3 . . ? C29 C30 C31 116.7(4) . . ? C29 C30 C33 121.7(4) . . ? C31 C30 C33 121.6(4) . . ? C32 C31 C30 121.1(4) . . ? C32 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C31 C32 C27 120.0(3) . . ? C31 C32 H32A 120.0 . . ? C27 C32 H32A 120.0 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O6 C34 H34A 109.5 . . ? O6 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O6 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C26 O1 Cu1 118.4(2) . 2_645 ? C34 O6 H6 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 N1 C17 164.3(13) 2_655 . . . ? N4 Cu1 N1 C17 148.0(2) . . . . ? N6 Cu1 N1 C17 33.21(18) . . . . ? N2 Cu1 N1 C17 -87.82(19) . . . . ? O1 Cu1 N1 C9 43.4(14) 2_655 . . . ? N4 Cu1 N1 C9 27.07(18) . . . . ? N6 Cu1 N1 C9 -87.69(19) . . . . ? N2 Cu1 N1 C9 151.27(19) . . . . ? O1 Cu1 N1 C1 -77.0(14) 2_655 . . . ? N4 Cu1 N1 C1 -93.3(2) . . . . ? N6 Cu1 N1 C1 151.9(2) . . . . ? N2 Cu1 N1 C1 30.86(19) . . . . ? O1 Cu1 N2 C2 152.4(2) 2_655 . . . ? N4 Cu1 N2 C2 47.6(3) . . . . ? N6 Cu1 N2 C2 -94.4(2) . . . . ? N1 Cu1 N2 C2 -23.6(2) . . . . ? O1 Cu1 N2 C3 -4.7(3) 2_655 . . . ? N4 Cu1 N2 C3 -109.6(3) . . . . ? N6 Cu1 N2 C3 108.4(3) . . . . ? N1 Cu1 N2 C3 179.2(3) . . . . ? O1 Cu1 N4 C10 166.4(2) 2_655 . . . ? N6 Cu1 N4 C10 58.5(2) . . . . ? N2 Cu1 N4 C10 -85.4(2) . . . . ? N1 Cu1 N4 C10 -14.7(2) . . . . ? O1 Cu1 N4 C11 -10.2(3) 2_655 . . . ? N6 Cu1 N4 C11 -118.1(3) . . . . ? N2 Cu1 N4 C11 97.9(3) . . . . ? N1 Cu1 N4 C11 168.6(3) . . . . ? O1 Cu1 N6 C18 162.3(2) 2_655 . . . ? N4 Cu1 N6 C18 -95.0(2) . . . . ? N2 Cu1 N6 C18 50.2(3) . . . . ? N1 Cu1 N6 C18 -20.9(2) . . . . ? O1 Cu1 N6 C19 -9.5(4) 2_655 . . . ? N4 Cu1 N6 C19 93.3(3) . . . . ? N2 Cu1 N6 C19 -121.5(3) . . . . ? N1 Cu1 N6 C19 167.4(3) . . . . ? C17 N1 C1 C2 84.1(3) . . . . ? C9 N1 C1 C2 -150.0(3) . . . . ? Cu1 N1 C1 C2 -32.2(3) . . . . ? C3 N2 C2 N3 1.0(4) . . . . ? Cu1 N2 C2 N3 -164.3(2) . . . . ? C3 N2 C2 C1 177.2(3) . . . . ? Cu1 N2 C2 C1 12.0(4) . . . . ? C8 N3 C2 N2 0.6(4) . . . . ? C8 N3 C2 C1 -175.6(3) . . . . ? N1 C1 C2 N2 14.6(4) . . . . ? N1 C1 C2 N3 -169.6(3) . . . . ? C2 N2 C3 C4 178.9(4) . . . . ? Cu1 N2 C3 C4 -23.2(6) . . . . ? C2 N2 C3 C8 -2.1(4) . . . . ? Cu1 N2 C3 C8 155.7(3) . . . . ? N2 C3 C4 C5 177.6(3) . . . . ? C8 C3 C4 C5 -1.3(5) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 C7 1.6(6) . . . . ? C5 C6 C7 C8 -0.3(6) . . . . ? C6 C7 C8 N3 179.6(3) . . . . ? C6 C7 C8 C3 -1.8(5) . . . . ? C2 N3 C8 C7 176.9(3) . . . . ? C2 N3 C8 C3 -1.8(4) . . . . ? N2 C3 C8 C7 -176.4(3) . . . . ? C4 C3 C8 C7 2.7(5) . . . . ? N2 C3 C8 N3 2.5(4) . . . . ? C4 C3 C8 N3 -178.4(3) . . . . ? C17 N1 C9 C10 -150.9(3) . . . . ? C1 N1 C9 C10 84.3(3) . . . . ? Cu1 N1 C9 C10 -33.5(3) . . . . ? C11 N4 C10 N5 -1.0(4) . . . . ? Cu1 N4 C10 N5 -178.9(2) . . . . ? C11 N4 C10 C9 176.6(3) . . . . ? Cu1 N4 C10 C9 -1.3(4) . . . . ? C16 N5 C10 N4 1.3(4) . . . . ? C16 N5 C10 C9 -176.2(3) . . . . ? N1 C9 C10 N4 24.7(4) . . . . ? N1 C9 C10 N5 -158.0(3) . . . . ? C10 N4 C11 C12 -179.2(3) . . . . ? Cu1 N4 C11 C12 -2.4(6) . . . . ? C10 N4 C11 C16 0.3(3) . . . . ? Cu1 N4 C11 C16 177.1(3) . . . . ? C16 C11 C12 C13 -0.3(5) . . . . ? N4 C11 C12 C13 179.1(3) . . . . ? C11 C12 C13 C14 0.2(5) . . . . ? C12 C13 C14 C15 0.7(6) . . . . ? C13 C14 C15 C16 -1.3(6) . . . . ? C10 N5 C16 C11 -1.1(4) . . . . ? C10 N5 C16 C15 179.3(3) . . . . ? C12 C11 C16 N5 180.0(3) . . . . ? N4 C11 C16 N5 0.5(4) . . . . ? C12 C11 C16 C15 -0.3(5) . . . . ? N4 C11 C16 C15 -179.8(3) . . . . ? C14 C15 C16 N5 -179.3(4) . . . . ? C14 C15 C16 C11 1.1(5) . . . . ? C9 N1 C17 C18 79.2(3) . . . . ? C1 N1 C17 C18 -155.3(3) . . . . ? Cu1 N1 C17 C18 -38.6(3) . . . . ? C19 N6 C18 N7 2.4(4) . . . . ? Cu1 N6 C18 N7 -172.3(2) . . . . ? C19 N6 C18 C17 178.6(3) . . . . ? Cu1 N6 C18 C17 3.9(4) . . . . ? C24 N7 C18 N6 -2.2(4) . . . . ? C25 N7 C18 N6 -164.3(3) . . . . ? C24 N7 C18 C17 -178.2(3) . . . . ? C25 N7 C18 C17 19.7(5) . . . . ? N1 C17 C18 N6 24.7(4) . . . . ? N1 C17 C18 N7 -159.5(3) . . . . ? C18 N6 C19 C20 177.1(3) . . . . ? Cu1 N6 C19 C20 -10.8(6) . . . . ? C18 N6 C19 C24 -1.6(3) . . . . ? Cu1 N6 C19 C24 170.5(3) . . . . ? N6 C19 C20 C21 -179.2(3) . . . . ? C24 C19 C20 C21 -0.6(5) . . . . ? C19 C20 C21 C22 -2.3(5) . . . . ? C20 C21 C22 C23 3.4(5) . . . . ? C21 C22 C23 C24 -1.3(5) . . . . ? C18 N7 C24 C23 179.7(4) . . . . ? C25 N7 C24 C23 -18.3(6) . . . . ? C18 N7 C24 C19 1.0(4) . . . . ? C25 N7 C24 C19 163.0(3) . . . . ? C22 C23 C24 N7 179.9(3) . . . . ? C22 C23 C24 C19 -1.6(5) . . . . ? C20 C19 C24 N7 -178.5(3) . . . . ? N6 C19 C24 N7 0.4(4) . . . . ? C20 C19 C24 C23 2.6(5) . . . . ? N6 C19 C24 C23 -178.5(3) . . . . ? C18 N7 C25 C26 67.5(4) . . . . ? C24 N7 C25 C26 -91.1(4) . . . . ? N7 C25 C26 O2 -12.7(4) . . . . ? N7 C25 C26 O1 167.2(2) . . . . ? O5 S1 C27 C28 101.4(3) . . . . ? O3 S1 C27 C28 -19.6(3) . . . . ? O4 S1 C27 C28 -139.0(3) . . . . ? O5 S1 C27 C32 -74.2(3) . . . . ? O3 S1 C27 C32 164.7(3) . . . . ? O4 S1 C27 C32 45.4(3) . . . . ? C32 C27 C28 C29 1.3(6) . . . . ? S1 C27 C28 C29 -174.4(3) . . . . ? C27 C28 C29 C30 1.5(6) . . . . ? C28 C29 C30 C31 -3.3(6) . . . . ? C28 C29 C30 C33 175.2(4) . . . . ? C29 C30 C31 C32 2.3(5) . . . . ? C33 C30 C31 C32 -176.2(3) . . . . ? C30 C31 C32 C27 0.3(5) . . . . ? C28 C27 C32 C31 -2.2(5) . . . . ? S1 C27 C32 C31 173.6(3) . . . . ? O2 C26 O1 Cu1 2.6(4) . . . 2_645 ? C25 C26 O1 Cu1 -177.32(18) . . . 2_645 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.666 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.069 #==============# data_3-Clo4-Phno2 _database_code_depnum_ccdc_archive 'CCDC 812765' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H118 Cl4 Cu4 N30 O38' _chemical_formula_weight 2936.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.7325(8) _cell_length_b 12.9895(7) _cell_length_c 20.3885(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.252(4) _cell_angle_gamma 90.00 _cell_volume 6319.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4256 _cell_measurement_theta_min 2.2450 _cell_measurement_theta_max 60.4594 _exptl_crystal_description plate _exptl_crystal_colour Blue _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 2.345 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7503 _exptl_absorpt_correction_T_max 0.9330 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type 'Oxford Germini S Ultra' _diffrn_measurement_method '\w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14966 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 60.63 _reflns_number_total 4701 _reflns_number_gt 2994 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _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. The O atoms of NO~2~ group and water molecules are disordered, which were treated to occupy partial positions. Isotropically simulated refinement is applied for all the solvents and anions by SIMU/ISOR which results in 78+108 restaints. ; _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^)+(0.1158P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4701 _refine_ls_number_parameters 471 _refine_ls_number_restraints 186 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1811 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.679759(18) -0.44696(4) 0.63672(2) 0.04898(15) Uani 1 1 d . . . N1 N 0.65123(10) -0.3001(2) 0.66617(13) 0.0472(8) Uani 1 1 d . . . N2 N 0.68626(10) -0.3513(3) 0.55449(14) 0.0530(8) Uani 1 1 d . . . N3 N 0.67987(11) -0.1930(3) 0.51365(14) 0.0544(9) Uani 1 1 d . . . H3A H 0.6771 -0.1255 0.5126 0.065 Uiso 1 1 calc R . . N4 N 0.59689(10) -0.4755(2) 0.61228(13) 0.0474(8) Uani 1 1 d . . . N5 N 0.51124(11) -0.4205(3) 0.60376(14) 0.0531(9) Uani 1 1 d . . . H5A H 0.4837 -0.3784 0.6054 0.064 Uiso 1 1 calc R . . N6 N 0.74116(10) -0.4118(2) 0.72053(14) 0.0480(8) Uani 1 1 d . . . N7 N 0.76519(11) -0.3350(2) 0.82175(14) 0.0509(8) Uani 1 1 d . . . C1 C 0.67968(14) -0.2182(3) 0.63666(17) 0.0517(10) Uani 1 1 d . . . H1A H 0.7180 -0.2067 0.6659 0.062 Uiso 1 1 calc R . . H1B H 0.6586 -0.1528 0.6333 0.062 Uiso 1 1 calc R . . C2 C 0.68208(13) -0.2530(3) 0.56711(17) 0.0485(10) Uani 1 1 d . . . C3 C 0.68712(13) -0.3553(4) 0.48645(19) 0.0627(12) Uani 1 1 d . . . C4 C 0.68888(17) -0.4394(4) 0.4443(2) 0.0871(15) Uani 1 1 d . . . H4A H 0.6917 -0.5082 0.4607 0.105 Uiso 1 1 calc R . . C5 C 0.68630(17) -0.4162(5) 0.3767(2) 0.1018(16) Uani 1 1 d . . . H5B H 0.6875 -0.4715 0.3466 0.122 Uiso 1 1 calc R . . C6 C 0.68214(17) -0.3178(5) 0.3514(2) 0.0993(19) Uani 1 1 d . . . H6A H 0.6804 -0.3071 0.3048 0.119 Uiso 1 1 calc R . . C7 C 0.68050(15) -0.2357(5) 0.3916(2) 0.0792(16) Uani 1 1 d . . . H7A H 0.6780 -0.1675 0.3743 0.095 Uiso 1 1 calc R . . C8 C 0.68267(14) -0.2554(4) 0.46055(18) 0.0597(12) Uani 1 1 d . . . C9 C 0.58885(13) -0.2931(3) 0.63937(19) 0.0541(10) Uani 1 1 d . . . H9A H 0.5724 -0.2643 0.6747 0.065 Uiso 1 1 calc R . . H9B H 0.5792 -0.2468 0.5994 0.065 Uiso 1 1 calc R . . C10 C 0.56594(13) -0.3965(3) 0.61982(16) 0.0475(10) Uani 1 1 d . . . C11 C 0.56015(12) -0.5573(3) 0.58953(16) 0.0441(9) Uani 1 1 d . . . C12 C 0.56844(13) -0.6572(3) 0.57208(18) 0.0498(10) Uani 1 1 d . . . H12A H 0.6050 -0.6816 0.5737 0.060 Uiso 1 1 calc R . . C13 C 0.52290(14) -0.7206(3) 0.5523(2) 0.0586(11) Uani 1 1 d . . . H13A H 0.5279 -0.7897 0.5398 0.070 Uiso 1 1 calc R . . C14 C 0.46868(15) -0.6847(4) 0.55016(19) 0.0621(12) Uani 1 1 d . . . H14A H 0.4379 -0.7309 0.5377 0.074 Uiso 1 1 calc R . . C15 C 0.45928(14) -0.5858(3) 0.56536(18) 0.0572(11) Uani 1 1 d . . . H15A H 0.4226 -0.5616 0.5631 0.069 Uiso 1 1 calc R . . C16 C 0.50567(12) -0.5212(3) 0.58449(16) 0.0476(10) Uani 1 1 d . . . C17 C 0.66949(14) -0.2976(3) 0.74144(17) 0.0520(10) Uani 1 1 d . . . H17A H 0.6426 -0.3355 0.7608 0.062 Uiso 1 1 calc R . . H17B H 0.6719 -0.2257 0.7580 0.062 Uiso 1 1 calc R . . C18 C 0.72572(13) -0.3475(3) 0.76157(16) 0.0472(9) Uani 1 1 d . . . C19 C 0.79525(13) -0.4434(3) 0.75400(18) 0.0499(10) Uani 1 1 d . . . C20 C 0.83301(14) -0.5058(3) 0.7325(2) 0.0534(10) Uani 1 1 d . . . H20A H 0.8234 -0.5371 0.6888 0.064 Uiso 1 1 calc R . . C21 C 0.88481(14) -0.5202(3) 0.7770(2) 0.0592(11) Uani 1 1 d . . . H21A H 0.9116 -0.5620 0.7638 0.071 Uiso 1 1 calc R . . C22 C 0.89886(15) -0.4745(3) 0.8416(2) 0.0635(12) Uani 1 1 d . . . H22A H 0.9346 -0.4882 0.8716 0.076 Uiso 1 1 calc R . . C23 C 0.86238(15) -0.4101(3) 0.8629(2) 0.0630(12) Uani 1 1 d . . . H23A H 0.8725 -0.3780 0.9062 0.076 Uiso 1 1 calc R . . C24 C 0.81031(14) -0.3946(3) 0.81782(18) 0.0519(10) Uani 1 1 d . . . C25 C 0.76562(15) -0.2512(3) 0.86981(18) 0.0553(11) Uani 1 1 d . . . H25A H 0.7899 -0.2706 0.9149 0.066 Uiso 1 1 calc R . . H25B H 0.7272 -0.2408 0.8746 0.066 Uiso 1 1 calc R . . C26 C 0.78724(13) -0.1488(3) 0.84631(18) 0.0519(10) Uani 1 1 d . . . O1 O 0.79773(12) -0.1456(2) 0.79268(13) 0.0707(8) Uani 1 1 d . . . O2 O 0.79104(9) -0.0762(2) 0.88987(12) 0.0567(7) Uani 1 1 d . . . Cl1 Cl 0.60683(5) 0.23994(11) 0.40763(6) 0.0901(4) Uani 1 1 d U . . O3 O 0.6163(2) 0.3460(3) 0.4062(3) 0.154(2) Uani 1 1 d U . . O4 O 0.62596(13) 0.1863(3) 0.35729(16) 0.1005(11) Uani 1 1 d U . . O5 O 0.63379(18) 0.1967(4) 0.47324(17) 0.1195(14) Uani 1 1 d U . . O6 O 0.54643(14) 0.2225(4) 0.39272(19) 0.1137(13) Uani 1 1 d U . . O7 O 0.5502(3) 0.4467(6) 0.2562(4) 0.088(2) Uani 0.50 1 d PU A 1 N8 N 0.5000 0.4794(5) 0.2500 0.0819(17) Uani 1 2 d SU . 1 C27 C 0.5000 0.5935(6) 0.2500 0.0684(17) Uani 1 2 d SU . 1 C28 C 0.54767(19) 0.6448(5) 0.2452(2) 0.0890(16) Uani 1 1 d U B 1 H28A H 0.5803 0.6084 0.2422 0.107 Uiso 1 1 calc R B 1 C29 C 0.5462(2) 0.7527(5) 0.2450(3) 0.1048(19) Uani 1 1 d U B 1 H29A H 0.5784 0.7897 0.2413 0.126 Uiso 1 1 calc R B 1 C30 C 0.5000 0.8063(9) 0.2500 0.128(3) Uani 1 2 d SU . 1 H30A H 0.5000 0.8795 0.2500 0.153 Uiso 1 2 calc SR . 1 O7' O 0.4585(3) 0.4225(7) 0.2374(4) 0.081(2) Uani 0.50 1 d PU C 2 O1W O 0.5666(4) -0.0488(7) 0.3951(5) 0.137(3) Uani 0.50 1 d PU D 1 O3W O 0.7040(2) 0.0260(6) 0.4749(4) 0.096(2) Uani 0.50 1 d PU E 1 O5W O 1.0000 -0.6607(13) 0.7500 0.150(5) Uani 0.50 2 d SPU F 1 O2W O 0.5665(4) -0.0246(7) 0.4642(4) 0.123(3) Uani 0.50 1 d PU G 2 O4W O 0.6425(3) -0.0095(6) 0.4739(5) 0.130(3) Uani 0.50 1 d PU H 2 O6W O 0.5244(7) 0.0480(14) 0.4711(8) 0.115(5) Uani 0.25 1 d PU I 3 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 0.0381(2) 0.0527(3) 0.0511(3) -0.0042(2) 0.0027(2) 0.0051(2) N1 0.0438(13) 0.0520(18) 0.0430(15) -0.0031(13) 0.0065(11) 0.0001(13) N2 0.0401(12) 0.065(2) 0.0552(16) -0.0146(15) 0.0151(12) -0.0043(14) N3 0.0454(13) 0.068(2) 0.0484(16) 0.0007(15) 0.0093(12) 0.0088(14) N4 0.0422(13) 0.0526(18) 0.0453(15) 0.0016(14) 0.0077(11) 0.0054(13) N5 0.0408(13) 0.071(2) 0.0460(15) -0.0036(15) 0.0095(12) 0.0087(14) N6 0.0403(13) 0.0514(18) 0.0485(15) 0.0025(14) 0.0048(12) 0.0006(13) N7 0.0498(14) 0.0559(19) 0.0430(15) -0.0011(14) 0.0053(12) -0.0110(14) C1 0.0515(17) 0.053(2) 0.0495(19) -0.0011(18) 0.0105(15) 0.0047(18) C2 0.0371(15) 0.062(2) 0.0419(18) -0.0027(18) 0.0018(14) 0.0084(16) C3 0.0379(15) 0.092(3) 0.061(2) -0.024(2) 0.0181(14) -0.0159(19) C4 0.074(2) 0.108(4) 0.093(3) -0.045(3) 0.045(2) -0.036(2) C5 0.079(2) 0.148(4) 0.097(3) -0.076(3) 0.0560(19) -0.067(3) C6 0.060(2) 0.171(5) 0.074(3) -0.042(3) 0.0298(19) -0.050(3) C7 0.0445(18) 0.135(5) 0.056(2) -0.006(3) 0.0111(17) -0.009(2) C8 0.0398(16) 0.092(3) 0.045(2) -0.006(2) 0.0063(15) -0.0108(19) C9 0.0417(16) 0.057(2) 0.057(2) -0.0037(19) 0.0025(15) 0.0133(17) C10 0.0414(16) 0.058(2) 0.0397(17) -0.0013(17) 0.0049(14) 0.0057(17) C11 0.0357(14) 0.053(2) 0.0398(17) 0.0020(16) 0.0034(13) 0.0028(16) C12 0.0382(15) 0.053(2) 0.056(2) 0.0025(18) 0.0088(14) 0.0015(16) C13 0.0487(18) 0.055(2) 0.067(2) -0.003(2) 0.0058(17) 0.0013(18) C14 0.0448(17) 0.078(3) 0.058(2) -0.002(2) 0.0033(16) -0.011(2) C15 0.0433(17) 0.078(3) 0.0476(19) 0.002(2) 0.0078(15) -0.0018(19) C16 0.0389(15) 0.065(3) 0.0376(17) 0.0025(17) 0.0081(13) 0.0010(17) C17 0.0518(17) 0.056(2) 0.0452(19) -0.0010(18) 0.0079(15) -0.0020(18) C18 0.0475(16) 0.052(2) 0.0425(17) 0.0029(17) 0.0121(14) -0.0102(17) C19 0.0429(16) 0.047(2) 0.054(2) 0.0082(18) 0.0032(15) -0.0059(16) C20 0.0470(16) 0.047(2) 0.062(2) 0.0132(18) 0.0072(16) -0.0047(17) C21 0.0429(16) 0.052(2) 0.079(2) 0.017(2) 0.0104(17) 0.0007(17) C22 0.0474(17) 0.062(3) 0.069(2) 0.020(2) -0.0060(17) -0.0131(19) C23 0.0545(19) 0.063(3) 0.061(2) 0.009(2) -0.0033(18) -0.014(2) C24 0.0461(16) 0.055(2) 0.0479(19) 0.0091(18) 0.0013(15) -0.0081(18) C25 0.0543(18) 0.062(3) 0.0447(19) 0.0009(18) 0.0038(15) -0.0176(18) C26 0.0363(15) 0.060(2) 0.049(2) -0.0028(19) -0.0084(15) 0.0009(17) O1 0.0935(16) 0.0659(19) 0.0622(15) 0.0093(14) 0.0370(13) -0.0008(15) O2 0.0511(12) 0.0640(17) 0.0479(13) 0.0004(13) 0.0006(11) -0.0115(12) Cl1 0.1166(8) 0.0856(8) 0.0663(6) 0.0082(6) 0.0210(6) 0.0406(7) O3 0.192(4) 0.071(3) 0.165(4) 0.007(3) -0.015(3) 0.032(3) O4 0.0987(17) 0.135(3) 0.0858(18) -0.0052(19) 0.0565(15) 0.028(2) O5 0.153(3) 0.137(3) 0.0618(19) 0.014(2) 0.0163(19) 0.063(3) O6 0.096(2) 0.145(3) 0.101(2) 0.013(2) 0.0294(18) 0.055(2) O7 0.093(4) 0.093(5) 0.075(4) 0.008(4) 0.015(3) 0.012(4) N8 0.095(3) 0.106(4) 0.043(2) 0.000 0.015(2) 0.000 C27 0.070(3) 0.094(4) 0.039(3) 0.000 0.011(2) 0.000 C28 0.077(2) 0.132(4) 0.052(2) 0.011(3) 0.006(2) -0.004(3) C29 0.101(3) 0.125(4) 0.075(3) 0.015(3) 0.000(3) -0.025(3) C30 0.129(6) 0.138(7) 0.095(5) 0.000 -0.007(5) 0.000 O7' 0.082(4) 0.110(6) 0.059(3) -0.007(3) 0.033(3) -0.008(4) O1W 0.174(6) 0.108(6) 0.141(6) -0.010(5) 0.062(5) 0.008(5) O3W 0.067(3) 0.100(5) 0.123(4) 0.034(4) 0.032(3) 0.010(3) O5W 0.106(7) 0.167(11) 0.163(10) 0.000 0.013(7) 0.000 O2W 0.162(5) 0.090(5) 0.106(5) -0.017(4) 0.018(4) 0.030(5) O4W 0.088(4) 0.091(5) 0.176(6) 0.050(5) -0.029(4) 0.007(4) O6W 0.127(8) 0.107(9) 0.109(8) -0.011(7) 0.025(7) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.960(3) 4_646 ? Cu1 N4 2.012(2) . ? Cu1 N6 2.017(3) . ? Cu1 N2 2.127(3) . ? Cu1 N1 2.173(3) . ? N1 C17 1.482(4) . ? N1 C1 1.487(5) . ? N1 C9 1.498(4) . ? N2 C2 1.312(5) . ? N2 C3 1.394(5) . ? N3 C2 1.329(5) . ? N3 C8 1.368(5) . ? N3 H3A 0.8800 . ? N4 C10 1.313(5) . ? N4 C11 1.396(4) . ? N5 C10 1.342(4) . ? N5 C16 1.363(5) . ? N5 H5A 0.8800 . ? N6 C18 1.308(5) . ? N6 C19 1.394(4) . ? N7 C18 1.362(4) . ? N7 C24 1.378(5) . ? N7 C25 1.462(5) . ? C1 C2 1.504(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C8 1.394(6) . ? C3 C4 1.398(7) . ? C4 C5 1.397(7) . ? C4 H4A 0.9500 . ? C5 C6 1.372(8) . ? C5 H5B 0.9500 . ? C6 C7 1.352(8) . ? C6 H6A 0.9500 . ? C7 C8 1.416(6) . ? C7 H7A 0.9500 . ? C9 C10 1.471(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.375(5) . ? C11 C16 1.405(5) . ? C12 C13 1.367(5) . ? C12 H12A 0.9500 . ? C13 C14 1.410(5) . ? C13 H13A 0.9500 . ? C14 C15 1.355(6) . ? C14 H14A 0.9500 . ? C15 C16 1.392(5) . ? C15 H15A 0.9500 . ? C17 C18 1.491(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.392(5) . ? C19 C24 1.407(5) . ? C20 C21 1.374(5) . ? C20 H20A 0.9500 . ? C21 C22 1.402(6) . ? C21 H21A 0.9500 . ? C22 C23 1.381(6) . ? C22 H22A 0.9500 . ? C23 C24 1.386(5) . ? C23 H23A 0.9500 . ? C25 C26 1.556(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O1 1.189(5) . ? C26 O2 1.281(5) . ? O2 Cu1 1.960(3) 4_656 ? Cl1 O3 1.399(5) . ? Cl1 O4 1.421(4) . ? Cl1 O5 1.442(4) . ? Cl1 O6 1.462(4) . ? O7 N8 1.287(8) . ? N8 O7 1.287(8) 2_655 ? N8 C27 1.482(10) . ? C27 C28 1.380(6) . ? C27 C28 1.380(6) 2_655 ? C28 C29 1.402(9) . ? C28 H28A 0.9500 . ? C29 C30 1.364(9) . ? C29 H29A 0.9500 . ? C30 C29 1.364(9) 2_655 ? C30 H30A 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 O2 Cu1 N4 101.48(11) 4_646 . ? O2 Cu1 N6 100.28(11) 4_646 . ? N4 Cu1 N6 137.92(12) . . ? O2 Cu1 N2 99.96(12) 4_646 . ? N4 Cu1 N2 101.29(11) . . ? N6 Cu1 N2 109.82(11) . . ? O2 Cu1 N1 177.21(11) 4_646 . ? N4 Cu1 N1 81.18(11) . . ? N6 Cu1 N1 78.09(11) . . ? N2 Cu1 N1 78.59(11) . . ? C17 N1 C1 110.8(3) . . ? C17 N1 C9 112.4(3) . . ? C1 N1 C9 111.2(3) . . ? C17 N1 Cu1 105.8(2) . . ? C1 N1 Cu1 107.1(2) . . ? C9 N1 Cu1 109.3(2) . . ? C2 N2 C3 104.7(3) . . ? C2 N2 Cu1 112.8(2) . . ? C3 N2 Cu1 141.9(3) . . ? C2 N3 C8 107.6(3) . . ? C2 N3 H3A 126.2 . . ? C8 N3 H3A 126.2 . . ? C10 N4 C11 106.6(3) . . ? C10 N4 Cu1 114.5(2) . . ? C11 N4 Cu1 138.9(2) . . ? C10 N5 C16 108.2(3) . . ? C10 N5 H5A 125.9 . . ? C16 N5 H5A 125.9 . . ? C18 N6 C19 106.2(3) . . ? C18 N6 Cu1 113.9(2) . . ? C19 N6 Cu1 139.4(3) . . ? C18 N7 C24 106.2(3) . . ? C18 N7 C25 124.8(3) . . ? C24 N7 C25 126.4(3) . . ? N1 C1 C2 107.9(3) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 N3 113.4(3) . . ? N2 C2 C1 120.1(3) . . ? N3 C2 C1 126.4(4) . . ? N2 C3 C8 108.8(4) . . ? N2 C3 C4 130.7(4) . . ? C8 C3 C4 120.5(4) . . ? C5 C4 C3 115.9(5) . . ? C5 C4 H4A 122.1 . . ? C3 C4 H4A 122.0 . . ? C6 C5 C4 123.5(5) . . ? C6 C5 H5B 118.2 . . ? C4 C5 H5B 118.2 . . ? C7 C6 C5 121.2(5) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C6 C7 C8 117.4(5) . . ? C6 C7 H7A 121.3 . . ? C8 C7 H7A 121.3 . . ? N3 C8 C3 105.5(3) . . ? N3 C8 C7 133.0(5) . . ? C3 C8 C7 121.5(4) . . ? C10 C9 N1 109.3(3) . . ? C10 C9 H9A 109.8 . . ? N1 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? N1 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? N4 C10 N5 111.8(3) . . ? N4 C10 C9 123.4(3) . . ? N5 C10 C9 124.7(3) . . ? C12 C11 N4 132.5(3) . . ? C12 C11 C16 120.1(3) . . ? N4 C11 C16 107.3(3) . . ? C13 C12 C11 118.5(3) . . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? C12 C13 C14 120.8(4) . . ? C12 C13 H13A 119.6 . . ? C14 C13 H13A 119.6 . . ? C15 C14 C13 121.7(4) . . ? C15 C14 H14A 119.1 . . ? C13 C14 H14A 119.1 . . ? C14 C15 C16 117.2(3) . . ? C14 C15 H15A 121.4 . . ? C16 C15 H15A 121.4 . . ? N5 C16 C15 132.3(3) . . ? N5 C16 C11 106.1(3) . . ? C15 C16 C11 121.5(4) . . ? N1 C17 C18 106.5(3) . . ? N1 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? N1 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? N6 C18 N7 113.1(3) . . ? N6 C18 C17 120.7(3) . . ? N7 C18 C17 126.3(3) . . ? C20 C19 N6 130.9(3) . . ? C20 C19 C24 121.2(3) . . ? N6 C19 C24 107.8(3) . . ? C21 C20 C19 117.2(4) . . ? C21 C20 H20A 121.4 . . ? C19 C20 H20A 121.4 . . ? C20 C21 C22 121.4(4) . . ? C20 C21 H21A 119.3 . . ? C22 C21 H21A 119.3 . . ? C23 C22 C21 122.0(3) . . ? C23 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C22 C23 C24 116.7(4) . . ? C22 C23 H23A 121.6 . . ? C24 C23 H23A 121.6 . . ? N7 C24 C23 131.9(4) . . ? N7 C24 C19 106.6(3) . . ? C23 C24 C19 121.4(4) . . ? N7 C25 C26 111.9(3) . . ? N7 C25 H25A 109.2 . . ? C26 C25 H25A 109.2 . . ? N7 C25 H25B 109.2 . . ? C26 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? O1 C26 O2 128.2(4) . . ? O1 C26 C25 119.2(4) . . ? O2 C26 C25 112.6(3) . . ? C26 O2 Cu1 113.8(2) . 4_656 ? O3 Cl1 O4 112.2(3) . . ? O3 Cl1 O5 111.3(3) . . ? O4 Cl1 O5 108.6(2) . . ? O3 Cl1 O6 108.5(3) . . ? O4 Cl1 O6 106.9(2) . . ? O5 Cl1 O6 109.3(3) . . ? O7 N8 O7 141.5(9) . 2_655 ? O7 N8 C27 109.3(5) . . ? O7 N8 C27 109.3(5) 2_655 . ? C28 C27 C28 122.2(7) . 2_655 ? C28 C27 N8 118.9(4) . . ? C28 C27 N8 118.9(4) 2_655 . ? C27 C28 C29 117.4(5) . . ? C27 C28 H28A 121.3 . . ? C29 C28 H28A 121.3 . . ? C30 C29 C28 122.2(7) . . ? C30 C29 H29A 118.9 . . ? C28 C29 H29A 118.9 . . ? C29 C30 C29 118.6(10) . 2_655 ? C29 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 2_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cu1 N1 C17 -88(2) 4_646 . . . ? N4 Cu1 N1 C17 109.4(2) . . . . ? N6 Cu1 N1 C17 -33.8(2) . . . . ? N2 Cu1 N1 C17 -147.1(2) . . . . ? O2 Cu1 N1 C1 30(2) 4_646 . . . ? N4 Cu1 N1 C1 -132.34(19) . . . . ? N6 Cu1 N1 C1 84.50(19) . . . . ? N2 Cu1 N1 C1 -28.83(18) . . . . ? O2 Cu1 N1 C9 150(2) 4_646 . . . ? N4 Cu1 N1 C9 -11.8(2) . . . . ? N6 Cu1 N1 C9 -155.0(2) . . . . ? N2 Cu1 N1 C9 91.7(2) . . . . ? O2 Cu1 N2 C2 -164.5(2) 4_646 . . . ? N4 Cu1 N2 C2 91.5(2) . . . . ? N6 Cu1 N2 C2 -59.7(2) . . . . ? N1 Cu1 N2 C2 13.1(2) . . . . ? O2 Cu1 N2 C3 26.0(3) 4_646 . . . ? N4 Cu1 N2 C3 -78.0(3) . . . . ? N6 Cu1 N2 C3 130.8(3) . . . . ? N1 Cu1 N2 C3 -156.4(3) . . . . ? O2 Cu1 N4 C10 -174.6(2) 4_646 . . . ? N6 Cu1 N4 C10 65.6(3) . . . . ? N2 Cu1 N4 C10 -71.8(3) . . . . ? N1 Cu1 N4 C10 4.5(2) . . . . ? O2 Cu1 N4 C11 6.6(4) 4_646 . . . ? N6 Cu1 N4 C11 -113.2(3) . . . . ? N2 Cu1 N4 C11 109.3(3) . . . . ? N1 Cu1 N4 C11 -174.3(4) . . . . ? O2 Cu1 N6 C18 -159.4(3) 4_646 . . . ? N4 Cu1 N6 C18 -39.2(3) . . . . ? N2 Cu1 N6 C18 96.0(3) . . . . ? N1 Cu1 N6 C18 22.9(2) . . . . ? O2 Cu1 N6 C19 10.9(4) 4_646 . . . ? N4 Cu1 N6 C19 131.1(4) . . . . ? N2 Cu1 N6 C19 -93.7(4) . . . . ? N1 Cu1 N6 C19 -166.8(4) . . . . ? C17 N1 C1 C2 153.6(3) . . . . ? C9 N1 C1 C2 -80.6(3) . . . . ? Cu1 N1 C1 C2 38.6(3) . . . . ? C3 N2 C2 N3 0.3(4) . . . . ? Cu1 N2 C2 N3 -173.0(2) . . . . ? C3 N2 C2 C1 179.7(3) . . . . ? Cu1 N2 C2 C1 6.4(4) . . . . ? C8 N3 C2 N2 0.1(4) . . . . ? C8 N3 C2 C1 -179.3(3) . . . . ? N1 C1 C2 N2 -31.7(4) . . . . ? N1 C1 C2 N3 147.7(3) . . . . ? C2 N2 C3 C8 -0.6(3) . . . . ? Cu1 N2 C3 C8 169.4(3) . . . . ? C2 N2 C3 C4 -177.3(4) . . . . ? Cu1 N2 C3 C4 -7.3(6) . . . . ? N2 C3 C4 C5 176.7(3) . . . . ? C8 C3 C4 C5 0.4(5) . . . . ? C3 C4 C5 C6 -0.1(6) . . . . ? C4 C5 C6 C7 0.3(6) . . . . ? C5 C6 C7 C8 -0.6(6) . . . . ? C2 N3 C8 C3 -0.5(3) . . . . ? C2 N3 C8 C7 177.8(4) . . . . ? N2 C3 C8 N3 0.7(4) . . . . ? C4 C3 C8 N3 177.7(3) . . . . ? N2 C3 C8 C7 -177.8(3) . . . . ? C4 C3 C8 C7 -0.8(5) . . . . ? C6 C7 C8 N3 -177.2(4) . . . . ? C6 C7 C8 C3 0.9(5) . . . . ? C17 N1 C9 C10 -100.9(4) . . . . ? C1 N1 C9 C10 134.2(3) . . . . ? Cu1 N1 C9 C10 16.2(3) . . . . ? C11 N4 C10 N5 0.1(4) . . . . ? Cu1 N4 C10 N5 -179.1(2) . . . . ? C11 N4 C10 C9 -176.3(3) . . . . ? Cu1 N4 C10 C9 4.5(4) . . . . ? C16 N5 C10 N4 0.0(4) . . . . ? C16 N5 C10 C9 176.4(3) . . . . ? N1 C9 C10 N4 -14.8(5) . . . . ? N1 C9 C10 N5 169.3(3) . . . . ? C10 N4 C11 C12 178.7(4) . . . . ? Cu1 N4 C11 C12 -2.4(6) . . . . ? C10 N4 C11 C16 -0.2(4) . . . . ? Cu1 N4 C11 C16 178.7(3) . . . . ? N4 C11 C12 C13 178.9(4) . . . . ? C16 C11 C12 C13 -2.3(5) . . . . ? C11 C12 C13 C14 -0.4(6) . . . . ? C12 C13 C14 C15 2.2(6) . . . . ? C13 C14 C15 C16 -1.2(6) . . . . ? C10 N5 C16 C15 177.3(4) . . . . ? C10 N5 C16 C11 -0.2(4) . . . . ? C14 C15 C16 N5 -178.7(4) . . . . ? C14 C15 C16 C11 -1.6(5) . . . . ? C12 C11 C16 N5 -178.8(3) . . . . ? N4 C11 C16 N5 0.2(4) . . . . ? C12 C11 C16 C15 3.4(5) . . . . ? N4 C11 C16 C15 -177.6(3) . . . . ? C1 N1 C17 C18 -78.1(4) . . . . ? C9 N1 C17 C18 156.8(3) . . . . ? Cu1 N1 C17 C18 37.6(3) . . . . ? C19 N6 C18 N7 -1.5(4) . . . . ? Cu1 N6 C18 N7 172.0(2) . . . . ? C19 N6 C18 C17 179.6(3) . . . . ? Cu1 N6 C18 C17 -7.0(4) . . . . ? C24 N7 C18 N6 1.6(4) . . . . ? C25 N7 C18 N6 164.4(3) . . . . ? C24 N7 C18 C17 -179.5(4) . . . . ? C25 N7 C18 C17 -16.7(6) . . . . ? N1 C17 C18 N6 -22.8(5) . . . . ? N1 C17 C18 N7 158.4(3) . . . . ? C18 N6 C19 C20 -175.3(4) . . . . ? Cu1 N6 C19 C20 13.9(7) . . . . ? C18 N6 C19 C24 0.8(4) . . . . ? Cu1 N6 C19 C24 -170.1(3) . . . . ? N6 C19 C20 C21 177.7(4) . . . . ? C24 C19 C20 C21 2.1(6) . . . . ? C19 C20 C21 C22 0.3(6) . . . . ? C20 C21 C22 C23 -2.2(6) . . . . ? C21 C22 C23 C24 1.6(6) . . . . ? C18 N7 C24 C23 178.3(4) . . . . ? C25 N7 C24 C23 15.9(7) . . . . ? C18 N7 C24 C19 -1.0(4) . . . . ? C25 N7 C24 C19 -163.4(3) . . . . ? C22 C23 C24 N7 -178.4(4) . . . . ? C22 C23 C24 C19 0.9(6) . . . . ? C20 C19 C24 N7 176.7(3) . . . . ? N6 C19 C24 N7 0.2(4) . . . . ? C20 C19 C24 C23 -2.8(6) . . . . ? N6 C19 C24 C23 -179.3(4) . . . . ? C18 N7 C25 C26 -77.6(4) . . . . ? C24 N7 C25 C26 81.8(4) . . . . ? N7 C25 C26 O1 4.2(4) . . . . ? N7 C25 C26 O2 -176.1(3) . . . . ? O1 C26 O2 Cu1 -2.1(4) . . . 4_656 ? C25 C26 O2 Cu1 178.3(2) . . . 4_656 ? O7 N8 C27 C28 10.2(4) . . . . ? O7 N8 C27 C28 -169.8(4) 2_655 . . . ? O7 N8 C27 C28 -169.8(4) . . . 2_655 ? O7 N8 C27 C28 10.2(4) 2_655 . . 2_655 ? C28 C27 C28 C29 -0.3(3) 2_655 . . . ? N8 C27 C28 C29 179.7(3) . . . . ? C27 C28 C29 C30 0.7(7) . . . . ? C28 C29 C30 C29 -0.4(3) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 60.63 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.877 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.087 #============# data_3-no3-Phno2 _database_code_depnum_ccdc_archive 'CCDC 812766' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H34 Cu N8.50 O10.25' _chemical_formula_weight 729.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.6794(10) _cell_length_b 12.4257(5) _cell_length_c 21.1689(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.994(4) _cell_angle_gamma 90.00 _cell_volume 6270.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2563 _cell_measurement_theta_min 2.4534 _cell_measurement_theta_max 60.5685 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3028 _exptl_absorpt_coefficient_mu 1.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6254 _exptl_absorpt_correction_T_max 0.7379 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type 'Oxford Germini S Ultra' _diffrn_measurement_method '\w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11979 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 60.42 _reflns_number_total 4607 _reflns_number_gt 2584 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _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. The NO~3~^-^ anion was constrained by SADI to make all N-O bonds resembling, which cause 3 restraint. The C37-C28 bond was fixed by DIFX which gives rise to 1 restraint. The free water molecules are disordered in the crystal lattice and are treated with partial-occupancy sites. Isotropically simulated refinement is applied for all the solvents and anions by SIMU/ISOR which results in 84+120 restraints. In total the restraints are 208. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4607 _refine_ls_number_parameters 489 _refine_ls_number_restraints 208 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.013 _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 0.67856(3) 0.46229(6) 0.12745(4) 0.0585(3) Uani 1 1 d . . . N1 N 0.65271(18) 0.3109(3) 0.1604(2) 0.0573(11) Uani 1 1 d . . . N2 N 0.68634(18) 0.3558(4) 0.0484(2) 0.0650(12) Uani 1 1 d . . . N3 N 0.67702(18) 0.1862(4) 0.0157(2) 0.0687(13) Uani 1 1 d . . . H3A H 0.6731 0.1159 0.0171 0.082 Uiso 1 1 calc R . . N4 N 0.59676(18) 0.4883(4) 0.1031(2) 0.0578(11) Uani 1 1 d . . . N5 N 0.51122(19) 0.4325(4) 0.1011(2) 0.0630(12) Uani 1 1 d . . . H5A H 0.4840 0.3895 0.1051 0.076 Uiso 1 1 calc R . . N6 N 0.74388(18) 0.4296(4) 0.2031(2) 0.0620(12) Uani 1 1 d . . . N7 N 0.7715(2) 0.3606(4) 0.3027(2) 0.0662(13) Uani 1 1 d . . . C1 C 0.6813(2) 0.2236(4) 0.1327(3) 0.0597(14) Uani 1 1 d . . . H1A H 0.7202 0.2140 0.1598 0.072 Uiso 1 1 calc R . . H1B H 0.6610 0.1547 0.1319 0.072 Uiso 1 1 calc R . . C2 C 0.6816(2) 0.2558(5) 0.0650(3) 0.0597(14) Uani 1 1 d . . . C3 C 0.6858(2) 0.3528(6) -0.0168(3) 0.0700(17) Uani 1 1 d . . . C4 C 0.6880(2) 0.4355(7) -0.0607(3) 0.088(2) Uani 1 1 d . . . H4A H 0.6918 0.5088 -0.0476 0.105 Uiso 1 1 calc R . . C5 C 0.6844(3) 0.4049(10) -0.1234(4) 0.110(3) Uani 1 1 d . . . H5B H 0.6867 0.4591 -0.1543 0.132 Uiso 1 1 calc R . . C6 C 0.6776(3) 0.3001(11) -0.1443(4) 0.116(3) Uani 1 1 d . . . H6A H 0.6743 0.2847 -0.1891 0.139 Uiso 1 1 calc R . . C7 C 0.6755(3) 0.2178(8) -0.1029(3) 0.100(3) Uani 1 1 d . . . H7A H 0.6715 0.1450 -0.1170 0.120 Uiso 1 1 calc R . . C8 C 0.6797(2) 0.2473(6) -0.0382(3) 0.0735(18) Uani 1 1 d . . . C9 C 0.5909(2) 0.3008(4) 0.1380(3) 0.0656(15) Uani 1 1 d . . . H9A H 0.5759 0.2758 0.1746 0.079 Uiso 1 1 calc R . . H9B H 0.5807 0.2472 0.1023 0.079 Uiso 1 1 calc R . . C10 C 0.5662(2) 0.4077(4) 0.1143(3) 0.0575(14) Uani 1 1 d . . . C11 C 0.5598(2) 0.5744(5) 0.0811(3) 0.0597(14) Uani 1 1 d . . . C12 C 0.5687(2) 0.6785(5) 0.0628(3) 0.0684(16) Uani 1 1 d . . . H12A H 0.6049 0.7028 0.0614 0.082 Uiso 1 1 calc R . . C13 C 0.5225(3) 0.7454(5) 0.0465(3) 0.0817(19) Uani 1 1 d . . . H13A H 0.5273 0.8178 0.0346 0.098 Uiso 1 1 calc R . . C14 C 0.4700(3) 0.7104(6) 0.0470(3) 0.0846(19) Uani 1 1 d . . . H14A H 0.4396 0.7595 0.0355 0.102 Uiso 1 1 calc R . . C15 C 0.4599(3) 0.6082(6) 0.0634(3) 0.0785(18) Uani 1 1 d . . . H15A H 0.4232 0.5850 0.0633 0.094 Uiso 1 1 calc R . . C16 C 0.5057(2) 0.5384(5) 0.0803(3) 0.0626(14) Uani 1 1 d . . . C17 C 0.6741(3) 0.3159(5) 0.2328(3) 0.0669(15) Uani 1 1 d . . . H17A H 0.6772 0.2426 0.2517 0.080 Uiso 1 1 calc R . . H17B H 0.6483 0.3586 0.2518 0.080 Uiso 1 1 calc R . . C18 C 0.7305(2) 0.3681(4) 0.2473(3) 0.0592(14) Uani 1 1 d . . . C19 C 0.7979(2) 0.4664(4) 0.2305(3) 0.0645(15) Uani 1 1 d . . . C20 C 0.8331(3) 0.5305(5) 0.2058(4) 0.0804(19) Uani 1 1 d . . . H20A H 0.8213 0.5601 0.1631 0.096 Uiso 1 1 calc R . . C21 C 0.8860(3) 0.5502(5) 0.2455(4) 0.090(2) Uani 1 1 d . . . H21A H 0.9110 0.5948 0.2299 0.108 Uiso 1 1 calc R . . C22 C 0.9036(3) 0.5051(6) 0.3090(4) 0.092(2) Uani 1 1 d . . . H22A H 0.9407 0.5192 0.3345 0.111 Uiso 1 1 calc R . . C23 C 0.8690(3) 0.4416(5) 0.3350(4) 0.0815(19) Uani 1 1 d . . . H23A H 0.8804 0.4131 0.3781 0.098 Uiso 1 1 calc R . . C24 C 0.8161(3) 0.4223(4) 0.2936(3) 0.0678(16) Uani 1 1 d . . . C25 C 0.7728(3) 0.2856(5) 0.3568(3) 0.0707(16) Uani 1 1 d . . . H25A H 0.7345 0.2782 0.3631 0.085 Uiso 1 1 calc R . . H25B H 0.7975 0.3146 0.3977 0.085 Uiso 1 1 calc R . . C26 C 0.7941(2) 0.1754(4) 0.3424(3) 0.0597(14) Uani 1 1 d . . . O1 O 0.79634(14) 0.1069(3) 0.38951(18) 0.0605(9) Uani 1 1 d . . . O2 O 0.80689(19) 0.1572(3) 0.2918(2) 0.0784(12) Uani 1 1 d . . . N8 N 0.5000 0.4647(10) 0.2500 0.115(3) Uani 1 2 d SU . . O3 O 0.5469(3) 0.4201(6) 0.2566(3) 0.139(2) Uani 1 1 d U . . C27 C 0.5000 0.5861(9) 0.2500 0.092(3) Uani 1 2 d SDU . . C28 C 0.5463(3) 0.6395(8) 0.2411(3) 0.099(2) Uani 1 1 d DU . . H28A H 0.5779 0.6010 0.2353 0.119 Uiso 1 1 calc R . . C29 C 0.5454(4) 0.7463(9) 0.2409(5) 0.119(3) Uani 1 1 d U . . H29A H 0.5768 0.7848 0.2344 0.143 Uiso 1 1 calc R . . C30 C 0.5000 0.8021(12) 0.2500 0.128(4) Uani 1 2 d SU . . H30A H 0.5000 0.8786 0.2500 0.154 Uiso 1 2 calc SR . . N9 N 0.4059(6) 0.2688(17) 0.1089(11) 0.295(7) Uani 1 1 d DU . . O4 O 0.3527(6) 0.2395(14) 0.1133(8) 0.355(7) Uani 1 1 d DU . . O5 O 0.3991(8) 0.3687(17) 0.0921(11) 0.378(9) Uani 1 1 d DU . . O6 O 0.4566(4) 0.2378(8) 0.1318(5) 0.195(4) Uani 1 1 d DU . . O1W O 0.6443(7) -0.035(2) 0.0066(11) 0.122(6) Uani 0.50 1 d PU A 1 O3W O 0.7258(6) 0.1662(9) 0.4637(6) 0.109(3) Uani 0.50 1 d PU B 1 O4W O 0.5483(7) 0.0267(15) 0.0136(10) 0.157(5) Uani 0.50 1 d PU C 1 O5W O 0.5587(7) -0.0503(14) -0.0697(7) 0.125(5) Uani 0.50 1 d PU D 1 O2W O 0.5000 0.208(2) 0.2500 0.197(9) Uani 0.50 2 d SPU E 1 O1W' O 0.6713(6) -0.0343(17) 0.0178(9) 0.099(5) Uani 0.50 1 d PU F 2 O3W' O 0.7686(9) 0.1602(12) 0.5033(8) 0.080(4) Uani 0.30 1 d PU G 2 O4W' O 0.5224(11) 0.0460(16) 0.0496(10) 0.189(7) Uani 0.50 1 d PU . 2 O5W' O 0.5377(8) -0.0352(15) -0.0458(10) 0.148(5) Uani 0.50 1 d PU . 2 O3W" O 0.8152(13) 0.179(2) 0.5196(13) 0.100(7) Uani 0.20 1 d PU H 3 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 0.0649(5) 0.0430(5) 0.0642(5) 0.0053(4) 0.0105(4) 0.0043(4) N1 0.068(3) 0.046(3) 0.057(3) -0.002(2) 0.012(2) 0.001(2) N2 0.067(3) 0.061(3) 0.064(3) 0.012(3) 0.011(2) 0.010(2) N3 0.071(3) 0.072(3) 0.058(3) -0.007(3) 0.008(2) 0.020(2) N4 0.068(3) 0.046(3) 0.058(3) -0.002(2) 0.013(2) 0.005(2) N5 0.060(3) 0.061(3) 0.064(3) -0.003(2) 0.007(2) -0.005(2) N6 0.067(3) 0.044(3) 0.069(3) 0.004(2) 0.006(2) 0.004(2) N7 0.087(3) 0.041(3) 0.060(3) -0.004(2) 0.001(3) 0.009(3) C1 0.075(3) 0.039(3) 0.063(4) -0.004(3) 0.013(3) 0.007(3) C2 0.061(3) 0.060(4) 0.056(3) -0.001(3) 0.012(3) 0.017(3) C3 0.053(3) 0.101(5) 0.055(4) 0.013(4) 0.011(3) 0.026(3) C4 0.066(4) 0.129(6) 0.069(5) 0.032(5) 0.020(3) 0.024(4) C5 0.070(4) 0.183(10) 0.081(6) 0.052(6) 0.025(4) 0.041(6) C6 0.082(5) 0.203(11) 0.059(5) 0.009(7) 0.011(4) 0.039(6) C7 0.085(5) 0.153(8) 0.061(5) -0.013(5) 0.015(4) 0.039(5) C8 0.057(3) 0.107(6) 0.054(4) 0.000(4) 0.009(3) 0.030(3) C9 0.071(4) 0.049(3) 0.075(4) -0.002(3) 0.016(3) -0.004(3) C10 0.066(4) 0.047(3) 0.060(3) -0.002(3) 0.016(3) -0.002(3) C11 0.062(4) 0.052(3) 0.056(3) -0.007(3) 0.000(3) 0.009(3) C12 0.065(4) 0.048(4) 0.083(4) 0.003(3) 0.002(3) 0.008(3) C13 0.076(5) 0.060(4) 0.093(5) 0.001(4) -0.007(3) 0.014(3) C14 0.074(5) 0.074(5) 0.093(5) -0.003(4) -0.002(4) 0.022(4) C15 0.061(4) 0.093(6) 0.075(4) -0.007(4) 0.006(3) 0.004(4) C16 0.059(4) 0.067(4) 0.057(3) -0.010(3) 0.006(3) 0.004(3) C17 0.090(4) 0.047(3) 0.064(4) -0.003(3) 0.018(3) 0.000(3) C18 0.074(4) 0.038(3) 0.063(4) -0.005(3) 0.012(3) 0.005(3) C19 0.069(4) 0.033(3) 0.085(4) 0.001(3) 0.008(3) 0.008(3) C20 0.070(4) 0.049(4) 0.111(5) 0.004(4) 0.003(4) 0.010(3) C21 0.077(4) 0.046(4) 0.142(7) -0.004(4) 0.017(5) 0.002(3) C22 0.078(4) 0.056(4) 0.124(7) -0.009(4) -0.011(4) 0.018(4) C23 0.082(4) 0.050(4) 0.094(5) -0.008(4) -0.010(4) 0.009(3) C24 0.082(4) 0.034(3) 0.076(4) -0.005(3) 0.000(3) 0.014(3) C25 0.087(4) 0.058(4) 0.058(4) -0.011(3) 0.003(3) 0.014(3) C26 0.071(4) 0.045(3) 0.058(4) -0.005(3) 0.009(3) -0.002(3) O1 0.073(2) 0.047(2) 0.056(2) -0.0044(19) 0.0072(18) -0.0046(18) O2 0.130(4) 0.050(2) 0.061(3) -0.003(2) 0.034(2) 0.004(2) N8 0.124(7) 0.145(8) 0.080(5) 0.000 0.032(5) 0.000 O3 0.130(5) 0.173(6) 0.120(5) 0.026(4) 0.044(4) 0.048(4) C27 0.104(7) 0.106(7) 0.062(5) 0.000 0.012(5) 0.000 C28 0.084(4) 0.141(7) 0.072(4) 0.015(5) 0.019(4) 0.012(5) C29 0.094(5) 0.142(7) 0.116(6) 0.035(6) 0.016(5) -0.018(5) C30 0.112(9) 0.108(8) 0.146(10) 0.000 -0.001(8) 0.000 N9 0.284(11) 0.314(12) 0.309(11) 0.003(11) 0.117(10) -0.064(11) O4 0.299(11) 0.407(13) 0.397(14) 0.087(11) 0.158(10) -0.145(10) O5 0.377(13) 0.364(15) 0.383(15) -0.019(14) 0.083(12) -0.054(12) O6 0.207(7) 0.175(7) 0.239(9) -0.029(6) 0.121(7) -0.068(6) O1W 0.140(13) 0.115(9) 0.111(11) -0.004(8) 0.031(11) 0.019(11) O3W 0.145(9) 0.092(7) 0.104(8) -0.006(6) 0.056(7) -0.009(7) O4W 0.173(10) 0.135(9) 0.150(11) 0.062(9) 0.016(9) 0.053(8) O5W 0.153(10) 0.123(9) 0.117(9) -0.012(7) 0.069(7) 0.005(7) O2W 0.159(14) 0.179(16) 0.255(19) 0.000 0.055(14) 0.000 O1W' 0.120(11) 0.082(7) 0.076(7) 0.003(6) -0.010(8) 0.042(9) O3W' 0.112(10) 0.074(8) 0.059(8) -0.006(7) 0.031(8) -0.001(9) O4W' 0.228(14) 0.146(11) 0.166(13) 0.059(10) 0.003(11) 0.023(11) O5W' 0.163(11) 0.112(9) 0.144(11) 0.038(9) -0.006(9) 0.008(9) O3W" 0.118(13) 0.082(12) 0.092(12) 0.002(10) 0.015(11) 0.016(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.964(4) 4_655 ? Cu1 N4 1.977(4) . ? Cu1 N6 1.998(5) . ? Cu1 N1 2.159(4) . ? Cu1 N2 2.180(5) . ? N1 C9 1.481(7) . ? N1 C17 1.488(7) . ? N1 C1 1.494(7) . ? N2 C2 1.305(7) . ? N2 C3 1.378(7) . ? N3 C2 1.338(7) . ? N3 C8 1.385(8) . ? N3 H3A 0.8800 . ? N4 C10 1.312(7) . ? N4 C11 1.405(7) . ? N5 C10 1.348(7) . ? N5 C16 1.383(7) . ? N5 H5A 0.8800 . ? N6 C18 1.315(7) . ? N6 C19 1.386(7) . ? N7 C18 1.339(7) . ? N7 C24 1.395(8) . ? N7 C25 1.471(8) . ? C1 C2 1.489(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C8 1.382(9) . ? C3 C4 1.395(9) . ? C4 C5 1.360(11) . ? C4 H4A 0.9500 . ? C5 C6 1.372(13) . ? C5 H5B 0.9500 . ? C6 C7 1.357(12) . ? C6 H6A 0.9500 . ? C7 C8 1.396(9) . ? C7 H7A 0.9500 . ? C9 C10 1.494(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.384(8) . ? C11 C16 1.403(8) . ? C12 C13 1.380(8) . ? C12 H12A 0.9500 . ? C13 C14 1.369(9) . ? C13 H13A 0.9500 . ? C14 C15 1.356(9) . ? C14 H14A 0.9500 . ? C15 C16 1.395(8) . ? C15 H15A 0.9500 . ? C17 C18 1.493(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.378(9) . ? C19 C24 1.405(8) . ? C20 C21 1.379(9) . ? C20 H20A 0.9500 . ? C21 C22 1.417(11) . ? C21 H21A 0.9500 . ? C22 C23 1.378(10) . ? C22 H22A 0.9500 . ? C23 C24 1.393(9) . ? C23 H23A 0.9500 . ? C25 C26 1.525(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O2 1.214(7) . ? C26 O1 1.301(7) . ? O1 Cu1 1.964(4) 4_645 ? N8 O3 1.257(7) . ? N8 O3 1.257(7) 2_655 ? N8 C27 1.509(15) . ? C27 C28 1.375(7) . ? C27 C28 1.375(7) 2_655 ? C28 C29 1.328(12) . ? C28 H28A 0.9500 . ? C29 C30 1.373(12) . ? C29 H29A 0.9500 . ? C30 C29 1.373(12) 2_655 ? C30 H30A 0.9500 . ? N9 O6 1.279(12) . ? N9 O5 1.290(15) . ? N9 O4 1.388(13) . ? O4W' O5W' 1.47(3) 5_655 ? O5W' O4W' 1.47(3) 5_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N4 98.75(17) 4_655 . ? O1 Cu1 N6 96.05(17) 4_655 . ? N4 Cu1 N6 143.10(19) . . ? O1 Cu1 N1 171.80(16) 4_655 . ? N4 Cu1 N1 81.91(17) . . ? N6 Cu1 N1 78.97(18) . . ? O1 Cu1 N2 108.69(17) 4_655 . ? N4 Cu1 N2 100.73(17) . . ? N6 Cu1 N2 106.18(18) . . ? N1 Cu1 N2 79.10(17) . . ? C9 N1 C17 113.2(4) . . ? C9 N1 C1 111.5(4) . . ? C17 N1 C1 110.9(4) . . ? C9 N1 Cu1 109.7(3) . . ? C17 N1 Cu1 103.9(3) . . ? C1 N1 Cu1 107.3(3) . . ? C2 N2 C3 105.4(5) . . ? C2 N2 Cu1 109.8(4) . . ? C3 N2 Cu1 143.7(4) . . ? C2 N3 C8 106.0(5) . . ? C2 N3 H3A 127.0 . . ? C8 N3 H3A 127.0 . . ? C10 N4 C11 106.6(4) . . ? C10 N4 Cu1 115.2(4) . . ? C11 N4 Cu1 137.9(4) . . ? C10 N5 C16 107.1(4) . . ? C10 N5 H5A 126.4 . . ? C16 N5 H5A 126.4 . . ? C18 N6 C19 106.5(5) . . ? C18 N6 Cu1 112.9(4) . . ? C19 N6 Cu1 139.3(4) . . ? C18 N7 C24 106.6(5) . . ? C18 N7 C25 125.8(5) . . ? C24 N7 C25 126.7(5) . . ? C2 C1 N1 107.6(4) . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1B 110.2 . . ? N1 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 N3 113.6(5) . . ? N2 C2 C1 122.6(5) . . ? N3 C2 C1 123.8(5) . . ? N2 C3 C8 109.0(6) . . ? N2 C3 C4 130.9(7) . . ? C8 C3 C4 120.0(6) . . ? C5 C4 C3 116.1(8) . . ? C5 C4 H4A 122.0 . . ? C3 C4 H4A 122.0 . . ? C4 C5 C6 123.5(9) . . ? C4 C5 H5B 118.3 . . ? C6 C5 H5B 118.3 . . ? C7 C6 C5 121.9(8) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C6 C7 C8 115.5(9) . . ? C6 C7 H7A 122.2 . . ? C8 C7 H7A 122.2 . . ? C3 C8 N3 106.0(5) . . ? C3 C8 C7 122.9(8) . . ? N3 C8 C7 131.0(8) . . ? N1 C9 C10 109.2(4) . . ? N1 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? N1 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? N4 C10 N5 112.5(5) . . ? N4 C10 C9 122.4(5) . . ? N5 C10 C9 125.1(5) . . ? C12 C11 C16 120.9(5) . . ? C12 C11 N4 131.9(5) . . ? C16 C11 N4 107.2(5) . . ? C13 C12 C11 116.9(6) . . ? C13 C12 H12A 121.6 . . ? C11 C12 H12A 121.6 . . ? C14 C13 C12 121.9(6) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C15 C14 C13 122.4(6) . . ? C15 C14 H14A 118.8 . . ? C13 C14 H14A 118.8 . . ? C14 C15 C16 117.2(6) . . ? C14 C15 H15A 121.4 . . ? C16 C15 H15A 121.4 . . ? N5 C16 C15 132.8(6) . . ? N5 C16 C11 106.5(5) . . ? C15 C16 C11 120.6(6) . . ? N1 C17 C18 107.1(5) . . ? N1 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? N1 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.5 . . ? N6 C18 N7 113.0(5) . . ? N6 C18 C17 119.9(5) . . ? N7 C18 C17 127.1(5) . . ? C20 C19 N6 131.6(6) . . ? C20 C19 C24 120.6(6) . . ? N6 C19 C24 107.8(5) . . ? C19 C20 C21 117.5(7) . . ? C19 C20 H20A 121.2 . . ? C21 C20 H20A 121.2 . . ? C20 C21 C22 121.1(7) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C23 C22 C21 122.4(7) . . ? C23 C22 H22A 118.8 . . ? C21 C22 H22A 118.8 . . ? C22 C23 C24 115.1(7) . . ? C22 C23 H23A 122.5 . . ? C24 C23 H23A 122.5 . . ? C23 C24 N7 130.7(6) . . ? C23 C24 C19 123.3(6) . . ? N7 C24 C19 106.0(5) . . ? N7 C25 C26 110.6(5) . . ? N7 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? N7 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? O2 C26 O1 125.8(5) . . ? O2 C26 C25 121.7(5) . . ? O1 C26 C25 112.5(5) . . ? C26 O1 Cu1 114.3(3) . 4_645 ? O3 N8 O3 127.7(12) . 2_655 ? O3 N8 C27 116.2(6) . . ? O3 N8 C27 116.2(6) 2_655 . ? C28 C27 C28 122.3(11) . 2_655 ? C28 C27 N8 118.8(5) . . ? C28 C27 N8 118.8(5) 2_655 . ? C29 C28 C27 118.0(8) . . ? C29 C28 H28A 121.0 . . ? C27 C28 H28A 121.0 . . ? C28 C29 C30 121.2(9) . . ? C28 C29 H29A 119.4 . . ? C30 C29 H29A 119.4 . . ? C29 C30 C29 119.3(13) . 2_655 ? C29 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 2_655 . ? O6 N9 O5 116.1(18) . . ? O6 N9 O4 138.1(18) . . ? O5 N9 O4 102.3(16) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 60.42 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.462 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.081 #==================# data_3-no3-PhMe _database_code_depnum_ccdc_archive 'CCDC 812767' #TrackingRef '- Compds.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H116 Cu4 N32 O26' _chemical_formula_weight 2616.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.4796(8) _cell_length_b 12.5996(5) _cell_length_c 23.1723(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.953(5) _cell_angle_gamma 90.00 _cell_volume 5776.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3029 _cell_measurement_theta_min 2.5817 _cell_measurement_theta_max 30.3700 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8873 _exptl_absorpt_correction_T_max 0.9603 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type Oxford _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25524 _diffrn_reflns_av_R_equivalents 0.1171 _diffrn_reflns_av_sigmaI/netI 0.3585 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11201 _reflns_number_gt 3724 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. The toluene molecule is symmetrically disordered over inversion center to occupy two half positions. The C6 ring is fixed as a hexagon by AFIX 66 and the methyl group is modeled by DFIX and SADI which cause 2 restraints. Isotropically simulated refinement is applied for all the solvents and anions by SIMU/ISOR which results in 84+120 restraints. In total the restraints are 206. ; _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^)+(0.0121P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11201 _refine_ls_number_parameters 814 _refine_ls_number_restraints 206 _refine_ls_R_factor_all 0.2455 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.066 _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 0.37109(4) -0.06984(7) 0.81395(4) 0.0371(3) Uani 1 1 d . . . Cu2 Cu 0.64595(4) 0.49037(7) 0.66471(4) 0.0414(3) Uani 1 1 d . . . N1 N 0.1662(3) 0.2845(4) 0.6557(3) 0.0285(16) Uani 1 1 d . . . N2 N 0.0513(3) 0.3200(5) 0.6945(3) 0.0359(17) Uani 1 1 d . . . N3 N 0.0182(3) 0.1498(5) 0.6784(2) 0.0377(17) Uani 1 1 d . . . H3A H 0.0206 0.0810 0.6726 0.045 Uiso 1 1 calc R . . N4 N 0.1039(3) 0.4593(5) 0.5995(3) 0.0415(19) Uani 1 1 d . . . N5 N 0.1237(3) 0.4222(5) 0.5115(3) 0.0372(17) Uani 1 1 d . . . H5B H 0.1371 0.3865 0.4840 0.045 Uiso 1 1 calc R . . N6 N 0.2083(3) 0.4010(4) 0.7566(3) 0.0316(17) Uani 1 1 d . . . N7 N 0.3119(3) 0.3355(5) 0.7838(3) 0.0393(18) Uani 1 1 d . . . N8 N 0.6814(3) 0.6417(4) 0.6470(3) 0.0364(17) Uani 1 1 d . . . N9 N 0.5679(3) 0.5805(5) 0.6750(2) 0.0374(17) Uani 1 1 d . . . N10 N 0.5208(3) 0.7382(5) 0.6678(3) 0.0448(18) Uani 1 1 d . . . H10A H 0.5158 0.8074 0.6637 0.054 Uiso 1 1 calc R . . N11 N 0.6794(3) 0.4564(5) 0.5900(3) 0.0365(17) Uani 1 1 d . . . N12 N 0.7088(3) 0.5284(5) 0.5125(3) 0.0418(18) Uani 1 1 d . . . H12B H 0.7164 0.5782 0.4884 0.050 Uiso 1 1 calc R . . N13 N 0.7225(3) 0.5262(5) 0.7456(3) 0.0375(17) Uani 1 1 d . . . N14 N 0.8225(3) 0.5960(5) 0.7791(3) 0.0395(18) Uani 1 1 d . . . C1 C 0.1390(4) 0.1951(5) 0.6842(3) 0.041(2) Uani 1 1 d . . . H1A H 0.1672 0.1841 0.7255 0.050 Uiso 1 1 calc R . . H1B H 0.1393 0.1289 0.6613 0.050 Uiso 1 1 calc R . . C2 C 0.0682(4) 0.2230(6) 0.6851(3) 0.030(2) Uani 1 1 d . . . C3 C -0.0169(4) 0.3132(6) 0.6932(3) 0.032(2) Uani 1 1 d . . . C4 C -0.0632(4) 0.3925(6) 0.6990(3) 0.043(2) Uani 1 1 d . . . H4A H -0.0502 0.4645 0.7068 0.051 Uiso 1 1 calc R . . C5 C -0.1288(4) 0.3583(7) 0.6926(3) 0.055(3) Uani 1 1 d . . . H5A H -0.1613 0.4097 0.6966 0.066 Uiso 1 1 calc R . . C6 C -0.1505(4) 0.2554(8) 0.6808(3) 0.054(3) Uani 1 1 d . . . H6A H -0.1968 0.2382 0.6758 0.065 Uiso 1 1 calc R . . C7 C -0.1053(4) 0.1778(7) 0.6763(3) 0.047(2) Uani 1 1 d . . . H7A H -0.1188 0.1058 0.6691 0.057 Uiso 1 1 calc R . . C8 C -0.0382(4) 0.2093(6) 0.6827(3) 0.035(2) Uani 1 1 d . . . C9 C 0.1453(3) 0.2814(6) 0.5895(3) 0.040(2) Uani 1 1 d . . . H9A H 0.1065 0.2325 0.5758 0.048 Uiso 1 1 calc R . . H9B H 0.1831 0.2555 0.5739 0.048 Uiso 1 1 calc R . . C10 C 0.1257(3) 0.3909(6) 0.5670(4) 0.033(2) Uani 1 1 d . . . C11 C 0.0840(4) 0.5439(6) 0.5614(4) 0.036(2) Uani 1 1 d . . . C12 C 0.0517(4) 0.6384(7) 0.5703(4) 0.045(2) Uani 1 1 d . . . H12A H 0.0415 0.6540 0.6071 0.054 Uiso 1 1 calc R . . C13 C 0.0355(4) 0.7078(6) 0.5223(5) 0.055(3) Uani 1 1 d . . . H13A H 0.0126 0.7719 0.5262 0.066 Uiso 1 1 calc R . . C14 C 0.0517(4) 0.6869(7) 0.4688(4) 0.053(3) Uani 1 1 d . . . H14A H 0.0426 0.7389 0.4380 0.064 Uiso 1 1 calc R . . C15 C 0.0802(4) 0.5932(8) 0.4598(4) 0.063(3) Uani 1 1 d . . . H15A H 0.0890 0.5769 0.4225 0.075 Uiso 1 1 calc R . . C16 C 0.0957(4) 0.5228(7) 0.5066(4) 0.045(2) Uani 1 1 d . . . C17 C 0.2401(3) 0.2930(5) 0.6815(3) 0.039(2) Uani 1 1 d . . . H17A H 0.2609 0.2215 0.6849 0.047 Uiso 1 1 calc R . . H17B H 0.2605 0.3367 0.6552 0.047 Uiso 1 1 calc R . . C18 C 0.2526(4) 0.3424(6) 0.7411(4) 0.034(2) Uani 1 1 d . . . C19 C 0.2377(4) 0.4367(6) 0.8140(4) 0.033(2) Uani 1 1 d . . . C20 C 0.2137(4) 0.5015(6) 0.8512(4) 0.042(2) Uani 1 1 d . . . H20A H 0.1696 0.5309 0.8392 0.050 Uiso 1 1 calc R . . C21 C 0.2552(4) 0.5222(6) 0.9060(4) 0.047(2) Uani 1 1 d . . . H21A H 0.2393 0.5667 0.9326 0.057 Uiso 1 1 calc R . . C22 C 0.3197(4) 0.4807(6) 0.9243(3) 0.044(2) Uani 1 1 d . . . H22A H 0.3471 0.4965 0.9631 0.053 Uiso 1 1 calc R . . C23 C 0.3445(4) 0.4168(6) 0.8869(4) 0.041(2) Uani 1 1 d . . . H23A H 0.3890 0.3889 0.8988 0.049 Uiso 1 1 calc R . . C24 C 0.3028(4) 0.3948(6) 0.8320(4) 0.035(2) Uani 1 1 d . . . C25 C 0.3678(4) 0.2560(6) 0.7835(3) 0.049(2) Uani 1 1 d . . . H25A H 0.4086 0.2746 0.8153 0.059 Uiso 1 1 calc R . . H25B H 0.3795 0.2598 0.7447 0.059 Uiso 1 1 calc R . . C26 C 0.3458(4) 0.1416(6) 0.7936(3) 0.036(2) Uani 1 1 d . . . C27 C 0.6452(3) 0.7248(5) 0.6705(3) 0.032(2) Uani 1 1 d . . . H27A H 0.6403 0.7889 0.6450 0.038 Uiso 1 1 calc R . . H27B H 0.6707 0.7445 0.7115 0.038 Uiso 1 1 calc R . . C28 C 0.5780(4) 0.6831(6) 0.6710(3) 0.038(2) Uani 1 1 d . . . C29 C 0.5011(4) 0.5667(7) 0.6772(3) 0.039(2) Uani 1 1 d . . . C30 C 0.4646(4) 0.4790(7) 0.6829(3) 0.051(2) Uani 1 1 d . . . H30A H 0.4840 0.4100 0.6869 0.062 Uiso 1 1 calc R . . C31 C 0.3966(4) 0.4956(8) 0.6826(3) 0.057(3) Uani 1 1 d . . . H31A H 0.3701 0.4359 0.6872 0.068 Uiso 1 1 calc R . . C32 C 0.3661(4) 0.5952(8) 0.6759(3) 0.054(3) Uani 1 1 d . . . H32A H 0.3196 0.6018 0.6747 0.064 Uiso 1 1 calc R . . C33 C 0.4028(4) 0.6830(7) 0.6710(3) 0.053(3) Uani 1 1 d . . . H33A H 0.3834 0.7519 0.6672 0.064 Uiso 1 1 calc R . . C34 C 0.4717(4) 0.6662(7) 0.6719(3) 0.041(2) Uani 1 1 d . . . C35 C 0.6682(4) 0.6498(5) 0.5826(3) 0.038(2) Uani 1 1 d . . . H35A H 0.6963 0.7063 0.5715 0.046 Uiso 1 1 calc R . . H35B H 0.6200 0.6666 0.5645 0.046 Uiso 1 1 calc R . . C36 C 0.6859(4) 0.5437(6) 0.5615(4) 0.036(2) Uani 1 1 d . . . C37 C 0.7009(4) 0.3759(6) 0.5570(4) 0.040(2) Uani 1 1 d . . . C38 C 0.7034(4) 0.2645(6) 0.5648(4) 0.046(2) Uani 1 1 d . . . H38A H 0.6910 0.2314 0.5973 0.055 Uiso 1 1 calc R . . C39 C 0.7245(4) 0.2069(6) 0.5229(4) 0.057(3) Uani 1 1 d . . . H39A H 0.7260 0.1318 0.5264 0.068 Uiso 1 1 calc R . . C40 C 0.7436(4) 0.2528(7) 0.4759(4) 0.051(3) Uani 1 1 d . . . H40A H 0.7596 0.2085 0.4493 0.061 Uiso 1 1 calc R . . C41 C 0.7404(4) 0.3607(7) 0.4660(4) 0.050(2) Uani 1 1 d . . . H41A H 0.7526 0.3924 0.4330 0.060 Uiso 1 1 calc R . . C42 C 0.7185(4) 0.4186(7) 0.5069(4) 0.041(2) Uani 1 1 d . . . C43 C 0.7554(3) 0.6441(5) 0.6755(3) 0.040(2) Uani 1 1 d . . . H43A H 0.7801 0.6064 0.6500 0.048 Uiso 1 1 calc R . . H43B H 0.7717 0.7184 0.6805 0.048 Uiso 1 1 calc R . . C44 C 0.7673(4) 0.5922(6) 0.7334(4) 0.042(2) Uani 1 1 d . . . C45 C 0.7480(4) 0.4934(6) 0.8035(4) 0.032(2) Uani 1 1 d . . . C46 C 0.7201(4) 0.4285(6) 0.8416(4) 0.045(2) Uani 1 1 d . . . H46A H 0.6770 0.3967 0.8269 0.054 Uiso 1 1 calc R . . C47 C 0.7556(4) 0.4124(6) 0.8991(4) 0.049(2) Uani 1 1 d . . . H47A H 0.7363 0.3717 0.9250 0.059 Uiso 1 1 calc R . . C48 C 0.8198(5) 0.4549(6) 0.9204(4) 0.054(3) Uani 1 1 d . . . H48A H 0.8443 0.4403 0.9604 0.065 Uiso 1 1 calc R . . C49 C 0.8489(4) 0.5174(6) 0.8853(4) 0.055(3) Uani 1 1 d . . . H49A H 0.8928 0.5468 0.9001 0.066 Uiso 1 1 calc R . . C50 C 0.8113(4) 0.5355(6) 0.8273(4) 0.045(2) Uani 1 1 d . . . C51 C 0.8750(4) 0.6791(6) 0.7852(4) 0.057(3) Uani 1 1 d . . . H51A H 0.8886 0.6853 0.7473 0.068 Uiso 1 1 calc R . . H51B H 0.9154 0.6589 0.8171 0.068 Uiso 1 1 calc R . . C52 C 0.8474(5) 0.7875(6) 0.8006(4) 0.045(3) Uani 1 1 d . . . O1 O 0.3916(2) 0.0738(4) 0.7895(2) 0.0368(13) Uani 1 1 d . . . O2 O 0.2927(3) 0.1245(4) 0.8056(2) 0.0539(17) Uani 1 1 d . . . O3 O 0.8924(2) 0.8570(4) 0.8209(2) 0.0492(16) Uani 1 1 d . . . O4 O 0.7855(3) 0.7965(4) 0.7892(2) 0.0507(17) Uani 1 1 d . . . N15 N 0.6569(4) 0.7448(6) 0.4180(4) 0.064(2) Uani 1 1 d U . . O5 O 0.6284(4) 0.7812(6) 0.4549(3) 0.138(3) Uani 1 1 d U . . O6 O 0.6298(3) 0.7623(5) 0.3663(3) 0.073(2) Uani 1 1 d U . . O7 O 0.7095(3) 0.6950(5) 0.4375(3) 0.084(2) Uani 1 1 d U . . N16 N 0.1060(7) 0.2661(12) 0.3920(7) 0.137(4) Uani 1 1 d U . . O8 O 0.1202(5) 0.2276(9) 0.4397(4) 0.168(4) Uani 1 1 d U . . O9 O 0.0720(4) 0.2238(6) 0.3418(4) 0.136(3) Uani 1 1 d U . . O10 O 0.1261(5) 0.3576(7) 0.3884(5) 0.188(4) Uani 1 1 d U . . O11 O 0.0080(3) 0.0522(5) 0.3711(3) 0.093(2) Uani 1 1 d U . . C53 C 0.0341(5) 0.0149(8) 0.4316(4) 0.120(4) Uani 1 1 d U . . H53A H 0.0752 -0.0268 0.4343 0.181 Uiso 1 1 calc R . . H53B H 0.0002 -0.0297 0.4428 0.181 Uiso 1 1 calc R . . H53C H 0.0447 0.0757 0.4587 0.181 Uiso 1 1 calc R . . O12 O 0.4945(3) 0.9456(5) 0.6400(3) 0.108(2) Uani 1 1 d U . . C54 C 0.4528(5) 0.9488(9) 0.5770(5) 0.161(5) Uani 1 1 d U . . H54A H 0.4107 0.9875 0.5751 0.242 Uiso 1 1 calc R . . H54B H 0.4421 0.8762 0.5624 0.242 Uiso 1 1 calc R . . H54C H 0.4780 0.9849 0.5521 0.242 Uiso 1 1 calc R . . C1W C 0.4766(8) 0.7144(13) 0.4712(9) 0.154(10) Uani 0.50 1 d PDU A -1 C2W C 0.4912(15) 0.5769(11) 0.4925(10) 0.169(9) Uani 0.50 1 d PGDU A -1 C3W C 0.4608(13) 0.5280(10) 0.5327(9) 0.149(9) Uani 0.50 1 d PGDU A -1 C4W C 0.4692(10) 0.4197(9) 0.5435(7) 0.147(8) Uani 0.50 1 d PGU A -1 C5W C 0.5080(10) 0.3603(10) 0.5141(6) 0.147(9) Uani 0.50 1 d PGU A -1 C6W C 0.5383(12) 0.4092(12) 0.4739(8) 0.154(8) Uani 0.50 1 d PGU A -1 C7W C 0.5299(14) 0.5175(12) 0.4631(9) 0.161(9) Uani 0.50 1 d PGDU A -1 O1W O 0.4663(2) 0.1044(4) 0.7029(3) 0.093(2) Uani 1 1 d GU A -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 0.0359(6) 0.0320(6) 0.0413(7) 0.0016(6) 0.0062(5) -0.0022(5) Cu2 0.0405(6) 0.0302(6) 0.0505(7) 0.0015(6) 0.0062(5) -0.0003(6) N1 0.023(4) 0.029(4) 0.033(5) 0.001(3) 0.007(3) -0.001(3) N2 0.041(5) 0.022(4) 0.040(5) 0.005(4) 0.002(4) 0.009(4) N3 0.025(4) 0.042(4) 0.041(5) -0.003(4) -0.001(3) 0.003(4) N4 0.047(4) 0.036(5) 0.046(5) -0.016(4) 0.018(4) 0.001(4) N5 0.045(4) 0.036(5) 0.028(5) 0.000(4) 0.005(3) 0.005(4) N6 0.032(4) 0.020(4) 0.044(5) 0.001(3) 0.012(4) 0.010(3) N7 0.033(4) 0.035(4) 0.050(6) 0.007(4) 0.010(4) 0.012(4) N8 0.030(4) 0.032(4) 0.047(5) -0.002(4) 0.010(4) -0.006(3) N9 0.040(4) 0.029(4) 0.042(5) 0.002(4) 0.008(3) -0.001(4) N10 0.049(5) 0.024(4) 0.056(5) 0.005(4) 0.003(4) 0.004(4) N11 0.039(4) 0.018(4) 0.051(5) -0.005(4) 0.007(4) -0.005(3) N12 0.047(4) 0.037(5) 0.037(5) 0.008(4) 0.004(4) 0.002(4) N13 0.043(4) 0.032(4) 0.032(5) -0.006(4) 0.001(4) 0.001(4) N14 0.032(4) 0.021(4) 0.058(6) -0.007(4) -0.001(4) -0.004(4) C1 0.056(6) 0.024(5) 0.046(6) 0.005(5) 0.016(5) 0.003(5) C2 0.020(5) 0.035(5) 0.032(5) 0.006(4) 0.001(4) -0.002(5) C3 0.024(5) 0.038(6) 0.031(5) -0.002(4) 0.000(4) -0.008(5) C4 0.050(6) 0.046(6) 0.035(6) 0.003(4) 0.016(5) 0.011(5) C5 0.025(6) 0.078(8) 0.063(7) 0.003(6) 0.011(5) 0.022(6) C6 0.042(6) 0.073(7) 0.046(7) -0.004(6) 0.009(5) 0.000(6) C7 0.050(6) 0.057(7) 0.034(6) -0.004(5) 0.008(5) -0.018(6) C8 0.040(6) 0.038(6) 0.023(5) 0.005(4) 0.002(4) -0.013(5) C9 0.035(5) 0.049(6) 0.032(6) -0.009(5) 0.002(4) -0.012(5) C10 0.021(5) 0.038(6) 0.036(6) 0.008(5) 0.001(4) -0.005(4) C11 0.036(5) 0.025(6) 0.042(7) 0.009(5) 0.000(5) 0.002(4) C12 0.039(5) 0.046(6) 0.034(6) -0.009(5) -0.017(4) -0.012(5) C13 0.042(6) 0.034(6) 0.074(8) -0.005(6) -0.012(6) -0.003(5) C14 0.051(6) 0.056(7) 0.040(7) 0.013(6) -0.011(5) -0.010(5) C15 0.071(7) 0.068(7) 0.051(8) -0.001(6) 0.019(6) 0.001(6) C16 0.040(5) 0.053(7) 0.033(6) 0.002(6) -0.005(5) -0.007(5) C17 0.024(5) 0.035(5) 0.059(7) 0.004(5) 0.010(5) 0.007(4) C18 0.040(6) 0.024(5) 0.038(6) -0.003(5) 0.011(5) -0.010(5) C19 0.045(6) 0.025(5) 0.025(6) 0.000(5) 0.002(5) -0.006(5) C20 0.058(6) 0.028(5) 0.036(6) -0.002(5) 0.005(5) 0.007(5) C21 0.062(6) 0.022(5) 0.060(7) 0.001(5) 0.019(5) 0.009(5) C22 0.059(6) 0.027(5) 0.040(6) 0.004(5) 0.000(5) -0.012(5) C23 0.045(6) 0.038(6) 0.036(6) 0.010(5) 0.003(5) 0.000(5) C24 0.027(5) 0.026(5) 0.049(7) -0.002(5) 0.004(5) -0.004(4) C25 0.060(6) 0.055(6) 0.026(6) 0.000(5) 0.000(5) -0.019(5) C26 0.037(6) 0.023(5) 0.036(6) 0.017(4) -0.012(4) 0.002(5) C27 0.035(5) 0.019(5) 0.038(6) 0.013(4) 0.004(4) 0.012(4) C28 0.043(6) 0.028(5) 0.044(6) 0.007(5) 0.013(5) 0.018(5) C29 0.034(5) 0.028(5) 0.052(6) 0.000(5) 0.006(4) 0.000(5) C30 0.043(6) 0.054(7) 0.055(6) -0.005(5) 0.009(5) -0.004(5) C31 0.047(6) 0.073(8) 0.048(6) 0.013(6) 0.006(5) -0.011(6) C32 0.045(6) 0.073(8) 0.039(6) 0.002(5) 0.003(5) -0.002(6) C33 0.054(7) 0.060(7) 0.037(6) 0.002(5) -0.003(5) 0.011(6) C34 0.041(6) 0.048(7) 0.033(6) 0.000(5) 0.007(5) 0.004(6) C35 0.058(6) 0.019(5) 0.038(6) -0.010(4) 0.014(5) -0.001(4) C36 0.040(5) 0.029(6) 0.043(6) -0.008(5) 0.018(5) -0.015(4) C37 0.034(5) 0.023(5) 0.052(7) -0.008(5) -0.009(5) -0.005(5) C38 0.061(6) 0.030(5) 0.045(6) -0.003(5) 0.008(5) 0.002(5) C39 0.065(7) 0.044(6) 0.056(7) -0.007(6) 0.006(5) 0.004(5) C40 0.071(7) 0.034(6) 0.048(7) -0.003(5) 0.017(6) 0.008(6) C41 0.057(6) 0.056(7) 0.036(6) -0.015(5) 0.012(5) -0.002(6) C42 0.036(5) 0.045(6) 0.041(6) -0.006(5) 0.009(5) -0.007(5) C43 0.045(6) 0.031(5) 0.033(6) 0.005(4) -0.009(5) 0.001(4) C44 0.021(5) 0.039(6) 0.060(7) -0.025(5) -0.004(5) -0.015(5) C45 0.028(5) 0.024(5) 0.044(6) -0.014(5) 0.009(5) -0.012(4) C46 0.047(6) 0.030(5) 0.051(7) -0.001(5) -0.001(5) 0.002(5) C47 0.054(6) 0.032(6) 0.053(7) -0.007(5) -0.001(5) -0.002(5) C48 0.082(8) 0.027(6) 0.042(7) 0.003(5) -0.003(6) 0.013(5) C49 0.045(6) 0.030(6) 0.076(8) -0.007(6) -0.008(6) 0.003(5) C50 0.040(6) 0.028(6) 0.058(7) -0.004(5) -0.001(5) 0.008(5) C51 0.039(5) 0.038(6) 0.087(8) 0.006(5) 0.004(5) 0.011(5) C52 0.058(7) 0.025(6) 0.054(7) 0.003(5) 0.021(6) 0.015(5) O1 0.033(3) 0.030(3) 0.042(4) -0.002(3) -0.002(3) -0.007(3) O2 0.042(4) 0.033(4) 0.087(5) -0.005(3) 0.016(4) -0.010(3) O3 0.038(3) 0.032(4) 0.070(5) -0.014(3) -0.001(3) 0.000(3) O4 0.040(3) 0.043(4) 0.067(5) 0.000(3) 0.010(3) 0.002(3) N15 0.070(6) 0.075(6) 0.053(6) 0.017(5) 0.027(5) 0.005(5) O5 0.131(6) 0.200(8) 0.082(6) -0.021(5) 0.028(5) 0.042(5) O6 0.071(4) 0.095(5) 0.055(5) 0.022(4) 0.020(4) 0.016(4) O7 0.053(4) 0.107(5) 0.090(5) 0.046(4) 0.014(4) 0.006(4) N16 0.149(8) 0.120(9) 0.177(10) -0.027(9) 0.105(8) -0.010(7) O8 0.165(7) 0.180(9) 0.136(9) -0.072(7) -0.001(7) 0.077(7) O9 0.157(7) 0.132(7) 0.125(7) -0.057(6) 0.043(6) -0.016(5) O10 0.215(8) 0.152(8) 0.257(9) -0.067(8) 0.169(7) -0.063(7) O11 0.069(4) 0.083(5) 0.120(6) -0.017(5) 0.011(4) 0.004(4) C53 0.126(8) 0.148(9) 0.064(7) -0.011(8) -0.017(7) 0.073(7) O12 0.112(5) 0.090(5) 0.119(6) 0.033(5) 0.025(5) 0.028(4) C54 0.133(9) 0.175(10) 0.160(11) 0.036(10) 0.007(8) 0.037(8) C1W 0.024(10) 0.160(17) 0.235(19) -0.124(15) -0.045(12) 0.035(11) C2W 0.123(13) 0.209(15) 0.155(14) -0.020(13) -0.002(11) -0.034(13) C3W 0.112(12) 0.190(15) 0.129(13) -0.029(12) 0.002(11) -0.028(12) C4W 0.105(12) 0.189(15) 0.131(13) -0.038(12) 0.001(10) -0.032(12) C5W 0.088(13) 0.180(15) 0.152(13) -0.044(12) -0.007(11) 0.008(13) C6W 0.108(12) 0.200(15) 0.140(13) -0.029(12) 0.010(11) -0.006(12) C7W 0.125(13) 0.210(15) 0.138(13) -0.039(12) 0.014(11) -0.029(13) O1W 0.058(4) 0.078(5) 0.153(6) 0.017(4) 0.042(4) 0.010(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 N4 1.972(6) 2_546 ? Cu1 O1 1.973(4) . ? Cu1 N6 2.019(6) 2_546 ? Cu1 N2 2.157(6) 2_546 ? Cu1 N1 2.173(5) 2_546 ? Cu2 O3 1.920(5) 2_646 ? Cu2 N9 2.024(6) . ? Cu2 N11 2.064(6) . ? Cu2 N8 2.118(5) . ? Cu2 N13 2.158(6) . ? N1 C17 1.480(7) . ? N1 C9 1.482(7) . ? N1 C1 1.486(7) . ? N1 Cu1 2.173(5) 2_556 ? N2 C2 1.304(7) . ? N2 C3 1.390(8) . ? N2 Cu1 2.157(6) 2_556 ? N3 C2 1.356(7) . ? N3 C8 1.402(8) . ? N3 H3A 0.8800 . ? N4 C10 1.297(8) . ? N4 C11 1.378(8) . ? N4 Cu1 1.972(6) 2_556 ? N5 C10 1.335(8) . ? N5 C16 1.383(9) . ? N5 H5B 0.8800 . ? N6 C18 1.292(8) . ? N6 C19 1.385(8) . ? N6 Cu1 2.019(6) 2_556 ? N7 C18 1.358(9) . ? N7 C24 1.396(9) . ? N7 C25 1.522(8) . ? N8 C35 1.450(8) . ? N8 C27 1.467(7) . ? N8 C43 1.489(8) . ? N9 C28 1.316(8) . ? N9 C29 1.393(8) . ? N10 C28 1.346(8) . ? N10 C34 1.376(8) . ? N10 H10A 0.8800 . ? N11 C36 1.307(8) . ? N11 C37 1.408(8) . ? N12 C36 1.350(7) . ? N12 C42 1.408(8) . ? N12 H12B 0.8800 . ? N13 C44 1.323(8) . ? N13 C45 1.371(8) . ? N14 C44 1.336(8) . ? N14 C50 1.420(9) . ? N14 C51 1.480(8) . ? C1 C2 1.498(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C8 1.382(9) . ? C3 C4 1.407(9) . ? C4 C5 1.382(9) . ? C4 H4A 0.9500 . ? C5 C6 1.375(9) . ? C5 H5A 0.9500 . ? C6 C7 1.369(9) . ? C6 H6A 0.9500 . ? C7 C8 1.400(9) . ? C7 H7A 0.9500 . ? C9 C10 1.493(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C16 1.377(9) . ? C11 C12 1.403(9) . ? C12 C13 1.386(9) . ? C12 H12A 0.9500 . ? C13 C14 1.389(10) . ? C13 H13A 0.9500 . ? C14 C15 1.357(9) . ? C14 H14A 0.9500 . ? C15 C16 1.375(10) . ? C15 H15A 0.9500 . ? C17 C18 1.475(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.369(9) . ? C19 C24 1.393(9) . ? C20 C21 1.358(9) . ? C20 H20A 0.9500 . ? C21 C22 1.382(9) . ? C21 H21A 0.9500 . ? C22 C23 1.372(9) . ? C22 H22A 0.9500 . ? C23 C24 1.365(9) . ? C23 H23A 0.9500 . ? C25 C26 1.546(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O2 1.209(7) . ? C26 O1 1.291(8) . ? C27 C28 1.476(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C29 C30 1.361(9) . ? C29 C34 1.382(9) . ? C30 C31 1.406(9) . ? C30 H30A 0.9500 . ? C31 C32 1.392(9) . ? C31 H31A 0.9500 . ? C32 C33 1.357(9) . ? C32 H32A 0.9500 . ? C33 C34 1.423(9) . ? C33 H33A 0.9500 . ? C35 C36 1.499(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C37 C42 1.409(9) . ? C37 C38 1.414(9) . ? C38 C39 1.369(9) . ? C38 H38A 0.9500 . ? C39 C40 1.376(9) . ? C39 H39A 0.9500 . ? C40 C41 1.378(9) . ? C40 H40A 0.9500 . ? C41 C42 1.360(9) . ? C41 H41A 0.9500 . ? C43 C44 1.456(9) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C45 C50 1.377(9) . ? C45 C46 1.427(9) . ? C46 C47 1.358(9) . ? C46 H46A 0.9500 . ? C47 C48 1.387(9) . ? C47 H47A 0.9500 . ? C48 C49 1.374(9) . ? C48 H48A 0.9500 . ? C49 C50 1.384(10) . ? C49 H49A 0.9500 . ? C51 C52 1.555(9) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O4 1.232(8) . ? C52 O3 1.269(8) . ? O3 Cu2 1.920(5) 2_656 ? N15 O6 1.203(8) . ? N15 O7 1.230(8) . ? N15 O5 1.242(8) . ? N16 O8 1.172(14) . ? N16 O10 1.234(13) . ? N16 O9 1.306(15) . ? O11 C53 1.445(8) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O12 C54 1.490(10) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C1W C2W 1.805(18) . ? C2W C3W 1.3900 . ? C2W C7W 1.3900 . ? C3W C4W 1.3900 . ? C4W C5W 1.3900 . ? C5W C6W 1.3900 . ? C6W C7W 1.3900 . ? 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 N4 Cu1 O1 95.9(2) 2_546 . ? N4 Cu1 N6 143.2(2) 2_546 2_546 ? O1 Cu1 N6 96.9(2) . 2_546 ? N4 Cu1 N2 102.0(2) 2_546 2_546 ? O1 Cu1 N2 110.3(2) . 2_546 ? N6 Cu1 N2 105.5(2) 2_546 2_546 ? N4 Cu1 N1 81.3(2) 2_546 2_546 ? O1 Cu1 N1 170.3(2) . 2_546 ? N6 Cu1 N1 80.3(2) 2_546 2_546 ? N2 Cu1 N1 79.3(2) 2_546 2_546 ? O3 Cu2 N9 95.7(2) 2_646 . ? O3 Cu2 N11 101.7(2) 2_646 . ? N9 Cu2 N11 131.2(2) . . ? O3 Cu2 N8 176.1(2) 2_646 . ? N9 Cu2 N8 80.7(2) . . ? N11 Cu2 N8 79.6(2) . . ? O3 Cu2 N13 105.6(2) 2_646 . ? N9 Cu2 N13 101.4(2) . . ? N11 Cu2 N13 116.6(2) . . ? N8 Cu2 N13 76.8(2) . . ? C17 N1 C9 114.4(5) . . ? C17 N1 C1 109.6(6) . . ? C9 N1 C1 113.5(5) . . ? C17 N1 Cu1 102.5(4) . 2_556 ? C9 N1 Cu1 109.0(4) . 2_556 ? C1 N1 Cu1 107.0(4) . 2_556 ? C2 N2 C3 104.3(6) . . ? C2 N2 Cu1 110.7(5) . 2_556 ? C3 N2 Cu1 142.8(5) . 2_556 ? C2 N3 C8 103.8(6) . . ? C2 N3 H3A 128.1 . . ? C8 N3 H3A 128.1 . . ? C10 N4 C11 103.4(6) . . ? C10 N4 Cu1 115.4(6) . 2_556 ? C11 N4 Cu1 138.8(6) . 2_556 ? C10 N5 C16 105.0(7) . . ? C10 N5 H5B 127.5 . . ? C16 N5 H5B 127.5 . . ? C18 N6 C19 106.8(6) . . ? C18 N6 Cu1 110.8(6) . 2_556 ? C19 N6 Cu1 141.1(5) . 2_556 ? C18 N7 C24 105.7(6) . . ? C18 N7 C25 124.8(7) . . ? C24 N7 C25 127.8(7) . . ? C35 N8 C27 110.8(6) . . ? C35 N8 C43 110.6(6) . . ? C27 N8 C43 112.1(6) . . ? C35 N8 Cu2 106.3(4) . . ? C27 N8 Cu2 109.9(4) . . ? C43 N8 Cu2 107.0(4) . . ? C28 N9 C29 107.3(6) . . ? C28 N9 Cu2 113.6(5) . . ? C29 N9 Cu2 138.3(5) . . ? C28 N10 C34 107.3(6) . . ? C28 N10 H10A 126.4 . . ? C34 N10 H10A 126.4 . . ? C36 N11 C37 104.2(6) . . ? C36 N11 Cu2 110.4(5) . . ? C37 N11 Cu2 145.4(5) . . ? C36 N12 C42 107.8(6) . . ? C36 N12 H12B 126.1 . . ? C42 N12 H12B 126.1 . . ? C44 N13 C45 106.7(7) . . ? C44 N13 Cu2 109.5(5) . . ? C45 N13 Cu2 142.6(6) . . ? C44 N14 C50 109.2(7) . . ? C44 N14 C51 123.1(7) . . ? C50 N14 C51 124.6(7) . . ? N1 C1 C2 107.7(6) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 N3 115.6(6) . . ? N2 C2 C1 121.5(7) . . ? N3 C2 C1 122.9(7) . . ? C8 C3 N2 109.4(7) . . ? C8 C3 C4 120.0(7) . . ? N2 C3 C4 130.6(8) . . ? C5 C4 C3 115.4(7) . . ? C5 C4 H4A 122.3 . . ? C3 C4 H4A 122.3 . . ? C6 C5 C4 124.8(8) . . ? C6 C5 H5A 117.6 . . ? C4 C5 H5A 117.6 . . ? C7 C6 C5 119.9(8) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C6 C7 C8 117.0(8) . . ? C6 C7 H7A 121.5 . . ? C8 C7 H7A 121.5 . . ? C3 C8 C7 123.0(8) . . ? C3 C8 N3 106.9(6) . . ? C7 C8 N3 130.1(8) . . ? N1 C9 C10 108.4(6) . . ? N1 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? N1 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N4 C10 N5 115.7(7) . . ? N4 C10 C9 120.9(7) . . ? N5 C10 C9 123.2(8) . . ? C16 C11 N4 110.4(7) . . ? C16 C11 C12 120.0(8) . . ? N4 C11 C12 129.5(8) . . ? C13 C12 C11 116.2(8) . . ? C13 C12 H12A 121.9 . . ? C11 C12 H12A 121.9 . . ? C12 C13 C14 122.3(8) . . ? C12 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? C15 C14 C13 120.9(8) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C14 C15 C16 117.5(8) . . ? C14 C15 H15A 121.3 . . ? C16 C15 H15A 121.3 . . ? C15 C16 C11 122.9(9) . . ? C15 C16 N5 131.6(9) . . ? C11 C16 N5 105.6(8) . . ? C18 C17 N1 108.8(6) . . ? C18 C17 H17A 109.9 . . ? N1 C17 H17A 109.9 . . ? C18 C17 H17B 109.9 . . ? N1 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N6 C18 N7 113.2(7) . . ? N6 C18 C17 122.5(8) . . ? N7 C18 C17 124.2(8) . . ? C20 C19 N6 131.3(8) . . ? C20 C19 C24 120.5(8) . . ? N6 C19 C24 108.2(7) . . ? C21 C20 C19 117.7(8) . . ? C21 C20 H20A 121.1 . . ? C19 C20 H20A 121.1 . . ? C20 C21 C22 122.1(8) . . ? C20 C21 H21A 119.0 . . ? C22 C21 H21A 119.0 . . ? C23 C22 C21 120.6(8) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 117.6(7) . . ? C24 C23 H23A 121.2 . . ? C22 C23 H23A 121.2 . . ? C23 C24 C19 121.5(8) . . ? C23 C24 N7 132.4(8) . . ? C19 C24 N7 106.1(8) . . ? N7 C25 C26 111.3(6) . . ? N7 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? N7 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? O2 C26 O1 127.9(7) . . ? O2 C26 C25 121.0(7) . . ? O1 C26 C25 111.1(7) . . ? N8 C27 C28 108.0(6) . . ? N8 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? N8 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? N9 C28 N10 111.1(7) . . ? N9 C28 C27 120.9(7) . . ? N10 C28 C27 127.9(7) . . ? C30 C29 C34 120.5(8) . . ? C30 C29 N9 132.4(8) . . ? C34 C29 N9 107.0(7) . . ? C29 C30 C31 116.5(8) . . ? C29 C30 H30A 121.7 . . ? C31 C30 H30A 121.7 . . ? C32 C31 C30 123.3(8) . . ? C32 C31 H31A 118.3 . . ? C30 C31 H31A 118.3 . . ? C33 C32 C31 120.1(8) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 116.5(8) . . ? C32 C33 H33A 121.7 . . ? C34 C33 H33A 121.7 . . ? N10 C34 C29 107.2(7) . . ? N10 C34 C33 129.9(8) . . ? C29 C34 C33 122.9(8) . . ? N8 C35 C36 106.0(6) . . ? N8 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? N8 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? N11 C36 N12 114.1(6) . . ? N11 C36 C35 121.4(7) . . ? N12 C36 C35 124.5(7) . . ? N11 C37 C42 110.8(7) . . ? N11 C37 C38 130.7(8) . . ? C42 C37 C38 118.4(8) . . ? C39 C38 C37 116.3(8) . . ? C39 C38 H38A 121.8 . . ? C37 C38 H38A 121.8 . . ? C38 C39 C40 123.0(8) . . ? C38 C39 H39A 118.5 . . ? C40 C39 H39A 118.5 . . ? C39 C40 C41 122.4(8) . . ? C39 C40 H40A 118.8 . . ? C41 C40 H40A 118.8 . . ? C42 C41 C40 115.0(8) . . ? C42 C41 H41A 122.5 . . ? C40 C41 H41A 122.5 . . ? C41 C42 N12 132.1(8) . . ? C41 C42 C37 124.8(9) . . ? N12 C42 C37 103.1(7) . . ? C44 C43 N8 108.0(6) . . ? C44 C43 H43A 110.1 . . ? N8 C43 H43A 110.1 . . ? C44 C43 H43B 110.1 . . ? N8 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? N13 C44 N14 110.2(8) . . ? N13 C44 C43 121.3(7) . . ? N14 C44 C43 128.4(8) . . ? N13 C45 C50 111.0(7) . . ? N13 C45 C46 131.8(8) . . ? C50 C45 C46 117.2(8) . . ? C47 C46 C45 119.7(8) . . ? C47 C46 H46A 120.2 . . ? C45 C46 H46A 120.2 . . ? C46 C47 C48 120.6(8) . . ? C46 C47 H47A 119.7 . . ? C48 C47 H47A 119.7 . . ? C49 C48 C47 121.8(8) . . ? C49 C48 H48A 119.1 . . ? C47 C48 H48A 119.1 . . ? C48 C49 C50 116.8(8) . . ? C48 C49 H49A 121.6 . . ? C50 C49 H49A 121.6 . . ? C45 C50 C49 123.8(9) . . ? C45 C50 N14 102.6(8) . . ? C49 C50 N14 133.5(8) . . ? N14 C51 C52 110.2(6) . . ? N14 C51 H51A 109.6 . . ? C52 C51 H51A 109.6 . . ? N14 C51 H51B 109.6 . . ? C52 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? O4 C52 O3 128.6(7) . . ? O4 C52 C51 116.5(8) . . ? O3 C52 C51 114.8(7) . . ? C26 O1 Cu1 111.9(4) . . ? C52 O3 Cu2 112.3(5) . 2_656 ? O6 N15 O7 126.6(9) . . ? O6 N15 O5 116.2(9) . . ? O7 N15 O5 117.2(9) . . ? O8 N16 O10 116.4(18) . . ? O8 N16 O9 128.1(17) . . ? O10 N16 O9 115.5(16) . . ? O11 C53 H53A 109.5 . . ? O11 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O11 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O12 C54 H54A 109.5 . . ? O12 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O12 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C3W C2W C7W 120.0 . . ? C3W C2W C1W 122.5(7) . . ? C7W C2W C1W 117.2(7) . . ? C2W C3W C4W 120.0 . . ? C5W C4W C3W 120.0 . . ? C4W C5W C6W 120.0 . . ? C7W C6W C5W 120.0 . . ? C6W C7W C2W 120.0 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.815 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.082 #====================END