Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dimitris Kessissoglou' _publ_contact_author_address ; Department of Chemistry Aristotle University of Thessaloniki Thessaloniki 54124 GREECE ; _publ_contact_author_email KESSISOG@CHEM.AUTH.GR _publ_section_title ; Di-2-Pyridyl Ketone Oxime in Copper Chemistry: di-, tri-, penta- and hexanuclear Clusters ; loop_ _publ_author_name 'Dimitris Kessissoglou' 'Tereza Afrati' 'Catherine Dendrinou-Samara' 'Jeff W Kampf' 'Gellert Mezei' ; V.L.Pecoraro ; 'Curtis M. Zaleski' # Attachment 'cz514.cif' data_temp _database_code_depnum_ccdc_archive 'CCDC 633711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C66 H50 Cl2 Cu6 N18 O8, 2(C24 H20 B), 4(C3 H7 N O), 2(C H4 0) ; _chemical_formula_sum 'C128 H126 B2 Cl2 Cu6 N22 O14' _chemical_formula_weight 2670.27 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.904(5) _cell_length_b 16.2272(19) _cell_length_c 20.398(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.941(2) _cell_angle_gamma 90.00 _cell_volume 12700(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8872 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 27.04 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5512 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7484 _exptl_absorpt_correction_T_max 0.9270 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_special_details ; 3949 frames x 30 sec. @ 4.980 cm; , 0.2 deg. steps in omega & phi ; _diffrn_ambient_temperature 123(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69494 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.42 _reflns_number_total 14346 _reflns_number_gt 10526 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-1K' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Use of the SQUEEZE subroutine of the PLATON program suite (PLATON Reference : A.L.Spek (2007) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands.) indicated the presence of eight solvent accessible voids in the crystal lattice. The toatl volume was 1290.2 A^3 with an estimated contribution of 141 electrons due to diffuse solvent scattering. This has been included as a total of eight methanol lattice solvates per unit cell. These have ben included as such in all derived crystal quanities however they exact composition of the diffuse solvent is not known precisely. Two ligands are disorderd by a rotation that brings a carbon and nitrogen position into coincidence. The atoms affected are N9/C30 and N3/C9. These were modeled as partial contributions of both N and C scattering with a free variable (contrained to sum to unity) assigned to refine the ratio. 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^)+(0.0955P)^2^+8.8884P] 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 14346 _refine_ls_number_parameters 776 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Cl1 Cl 0.50596(2) 0.19023(5) -0.06135(4) 0.03271(17) Uani 1 1 d . . . Cu1 Cu 0.527244(9) 0.16454(2) 0.073022(19) 0.02981(11) Uani 1 1 d . . . Cu2 Cu 0.534278(10) 0.35747(2) 0.040574(19) 0.02966(11) Uani 1 1 d . . . Cu3 Cu 0.462871(10) 0.25575(2) -0.010184(19) 0.02894(11) Uani 1 1 d . . . O1 O 0.57777(6) 0.29549(13) 0.07791(12) 0.0362(5) Uani 1 1 d . . . O2 O 0.46290(5) 0.36272(13) -0.05180(11) 0.0293(5) Uani 1 1 d . . . O3 O 0.48399(5) 0.10828(14) 0.07086(11) 0.0335(5) Uani 1 1 d . . . O4 O 0.50629(6) 0.27536(14) 0.06989(10) 0.0303(5) Uani 1 1 d D . . H4 H 0.5012(13) 0.277(3) 0.1129(13) 0.077(15) Uiso 1 1 d D . . O5 O 0.41396(13) 0.2829(4) 0.1611(4) 0.143(2) Uani 1 1 d . . . O6 O 0.20705(12) 0.3902(3) -0.0216(3) 0.1040(15) Uani 1 1 d . . . N1 N 0.55732(7) 0.06610(17) 0.10164(13) 0.0314(6) Uani 1 1 d . . . N2 N 0.57375(7) 0.21615(17) 0.08903(13) 0.0314(6) Uani 1 1 d . . . N3 N 0.64346(10) 0.2427(2) 0.06013(19) 0.0467(10) Uani 0.55(4) 1 d P A 1 C9A C 0.64346(10) 0.2427(2) 0.06013(19) 0.0467(10) Uani 0.45(4) 1 d P A 2 H9AA H 0.6252 0.2534 0.0200 0.056 Uiso 0.45(4) 1 calc PR A 2 N4 N 0.55911(7) 0.43677(17) -0.00244(14) 0.0333(6) Uani 1 1 d . . . N5 N 0.49484(6) 0.39489(15) -0.03633(13) 0.0275(5) Uani 1 1 d . . . N7 N 0.41134(6) 0.25019(14) -0.03663(12) 0.0254(5) Uani 1 1 d . . . N8 N 0.45678(7) 0.15279(16) 0.03621(13) 0.0305(6) Uani 1 1 d . . . N9 N 0.43068(9) -0.0196(2) 0.05731(17) 0.0357(8) Uani 0.10(3) 1 d P B 1 C30A C 0.43068(9) -0.0196(2) 0.05731(17) 0.0357(8) Uani 0.90(3) 1 d P B 2 H30B H 0.4470 -0.0235 0.0312 0.043 Uiso 0.90(3) 1 calc PR B 2 N10 N 0.36109(14) 0.2438(3) 0.1631(3) 0.0935(15) Uani 1 1 d . . . N11 N 0.21487(13) 0.4762(3) 0.0672(2) 0.0780(13) Uani 1 1 d . . . C1 C 0.54654(9) -0.0111(2) 0.10817(17) 0.0364(7) Uani 1 1 d . . . H1A H 0.5223 -0.0229 0.0936 0.044 Uiso 1 1 calc R . . C2 C 0.56952(9) -0.0744(2) 0.13547(18) 0.0408(8) Uani 1 1 d . . . H2A H 0.5612 -0.1286 0.1395 0.049 Uiso 1 1 calc R . . C3 C 0.60477(10) -0.0568(2) 0.15670(19) 0.0447(9) Uani 1 1 d . . . H3B H 0.6211 -0.0986 0.1766 0.054 Uiso 1 1 calc R . . C4 C 0.61625(9) 0.0226(2) 0.14875(18) 0.0413(8) Uani 1 1 d . . . H4A H 0.6404 0.0352 0.1625 0.050 Uiso 1 1 calc R . . C5 C 0.59210(8) 0.0832(2) 0.12064(16) 0.0324(7) Uani 1 1 d . . . C6 C 0.60067(8) 0.1681(2) 0.10797(16) 0.0319(7) Uani 1 1 d . A . C7 C 0.63702(9) 0.1983(2) 0.11335(18) 0.0365(7) Uani 1 1 d . . . C8 C 0.66147(8) 0.1794(2) 0.16941(19) 0.0442(9) Uani 1 1 d . A . H8A H 0.6566 0.1474 0.2047 0.053 Uiso 1 1 calc R C 1 C9 C 0.69396(11) 0.2079(3) 0.1740(3) 0.0788(16) Uani 0.55(4) 1 d P A 1 H9B H 0.7120 0.1951 0.2139 0.095 Uiso 0.55(4) 1 calc PR A 1 N3A N 0.69396(11) 0.2079(3) 0.1740(3) 0.0788(16) Uani 0.45(4) 1 d P A 2 C10 C 0.70233(11) 0.2542(3) 0.1246(3) 0.0583(11) Uani 1 1 d . . . H10A H 0.7254 0.2740 0.1309 0.070 Uiso 1 1 calc R A 1 C11 C 0.67693(11) 0.2713(2) 0.0663(2) 0.0507(10) Uani 1 1 d . A . H11A H 0.6820 0.3022 0.0307 0.061 Uiso 1 1 calc R D 1 C12 C 0.59313(9) 0.4541(2) 0.01731(19) 0.0430(9) Uani 1 1 d . . . H12A H 0.6080 0.4223 0.0526 0.052 Uiso 1 1 calc R . . C13 C 0.60749(10) 0.5180(3) -0.0125(2) 0.0519(11) Uani 1 1 d . . . H13A H 0.6318 0.5292 0.0024 0.062 Uiso 1 1 calc R . . C14 C 0.58598(10) 0.5643(3) -0.0634(2) 0.0483(10) Uani 1 1 d . . . H14A H 0.5952 0.6086 -0.0834 0.058 Uiso 1 1 calc R . . C15 C 0.55069(10) 0.5457(2) -0.08527(18) 0.0412(8) Uani 1 1 d . . . H15A H 0.5356 0.5764 -0.1211 0.049 Uiso 1 1 calc R . . C16 C 0.53778(9) 0.4814(2) -0.05391(16) 0.0334(7) Uani 1 1 d . . . C17 C 0.50138(8) 0.45433(18) -0.07340(15) 0.0280(6) Uani 1 1 d . . . C23 C 0.38923(8) 0.30561(18) -0.07546(15) 0.0286(6) Uani 1 1 d . . . H23A H 0.3985 0.3483 -0.0972 0.034 Uiso 1 1 calc R . . C24 C 0.35378(8) 0.3021(2) -0.08445(16) 0.0335(7) Uani 1 1 d . . . H24A H 0.3387 0.3421 -0.1114 0.040 Uiso 1 1 calc R . . C25 C 0.34059(9) 0.2390(2) -0.05328(18) 0.0371(7) Uani 1 1 d . . . H25A H 0.3162 0.2352 -0.0587 0.045 Uiso 1 1 calc R . . C26 C 0.36296(8) 0.1812(2) -0.01415(16) 0.0326(7) Uani 1 1 d . . . H26A H 0.3541 0.1372 0.0069 0.039 Uiso 1 1 calc R . . C27 C 0.39857(8) 0.18864(18) -0.00612(15) 0.0272(6) Uani 1 1 d . . . C28 C 0.42514(8) 0.13089(18) 0.03396(16) 0.0280(6) Uani 1 1 d . B . C29 C 0.41642(8) 0.05562(18) 0.06652(15) 0.0283(6) Uani 1 1 d . . . C30 C 0.39399(7) 0.06474(17) 0.10455(14) 0.0331(7) Uani 0.10(3) 1 d P B 1 H30A H 0.3846 0.1171 0.1107 0.040 Uiso 0.10(3) 1 calc PR B 1 N9A N 0.39399(7) 0.06474(17) 0.10455(14) 0.0331(7) Uani 0.90(3) 1 d P B 2 C31 C 0.38542(9) -0.0032(2) 0.1334(2) 0.0456(9) Uani 1 1 d . . . H31A H 0.3698 0.0023 0.1608 0.055 Uiso 1 1 calc R B 1 C32 C 0.39793(9) -0.0804(2) 0.1257(2) 0.0479(10) Uani 1 1 d . B . H32A H 0.3909 -0.1269 0.1469 0.057 Uiso 1 1 calc R . . C33 C 0.42092(10) -0.0889(2) 0.0866(2) 0.0454(9) Uani 1 1 d . . . H33A H 0.4299 -0.1416 0.0799 0.054 Uiso 1 1 calc R B 1 C34 C 0.12355(8) 0.19485(18) 0.31803(15) 0.0278(6) Uani 1 1 d . . . C35 C 0.10981(8) 0.18417(17) 0.37401(15) 0.0276(6) Uani 1 1 d . . . H35A H 0.1246 0.1635 0.4154 0.033 Uiso 1 1 calc R . . C36 C 0.07542(8) 0.20268(18) 0.37122(16) 0.0293(6) Uani 1 1 d . . . H36A H 0.0673 0.1945 0.4104 0.035 Uiso 1 1 calc R . . C37 C 0.05286(8) 0.23295(17) 0.31183(16) 0.0294(6) Uani 1 1 d . . . H37A H 0.0294 0.2460 0.3098 0.035 Uiso 1 1 calc R . . C38 C 0.06552(8) 0.24377(17) 0.25525(16) 0.0300(6) Uani 1 1 d . . . H38A H 0.0505 0.2638 0.2138 0.036 Uiso 1 1 calc R . . C39 C 0.09985(8) 0.22548(18) 0.25903(15) 0.0289(6) Uani 1 1 d . . . H39A H 0.1078 0.2341 0.2197 0.035 Uiso 1 1 calc R . . C40 C 0.18710(8) 0.13755(19) 0.39207(16) 0.0309(7) Uani 1 1 d . . . C41 C 0.17686(9) 0.0619(2) 0.41320(18) 0.0358(7) Uani 1 1 d . . . H41A H 0.1560 0.0373 0.3864 0.043 Uiso 1 1 calc R . . C42 C 0.19578(9) 0.0207(2) 0.47163(19) 0.0399(8) Uani 1 1 d . . . H42A H 0.1877 -0.0304 0.4841 0.048 Uiso 1 1 calc R . . C43 C 0.22664(9) 0.0550(2) 0.51162(18) 0.0398(8) Uani 1 1 d . . . H43A H 0.2397 0.0278 0.5517 0.048 Uiso 1 1 calc R . . C44 C 0.23788(9) 0.1288(2) 0.49208(17) 0.0367(7) Uani 1 1 d . . . H44A H 0.2589 0.1527 0.5189 0.044 Uiso 1 1 calc R . . C45 C 0.21851(8) 0.1689(2) 0.43299(16) 0.0333(7) Uani 1 1 d . . . H45A H 0.2271 0.2194 0.4203 0.040 Uiso 1 1 calc R . . C46 C 0.16813(9) 0.1130(2) 0.26177(16) 0.0334(7) Uani 1 1 d . . . C47 C 0.14126(10) 0.0601(2) 0.22820(17) 0.0379(7) Uani 1 1 d . . . H47A H 0.1189 0.0672 0.2353 0.045 Uiso 1 1 calc R . . C48 C 0.14576(12) -0.0024(2) 0.1850(2) 0.0518(10) Uani 1 1 d . . . H48A H 0.1268 -0.0377 0.1643 0.062 Uiso 1 1 calc R . . C49 C 0.17740(12) -0.0137(3) 0.1717(2) 0.0574(11) Uani 1 1 d . . . H49A H 0.1802 -0.0553 0.1409 0.069 Uiso 1 1 calc R . . C50 C 0.20481(11) 0.0359(3) 0.20358(19) 0.0501(10) Uani 1 1 d . . . H50A H 0.2269 0.0281 0.1955 0.060 Uiso 1 1 calc R . . C51 C 0.20023(10) 0.0978(3) 0.24791(18) 0.0441(9) Uani 1 1 d . . . H51A H 0.2197 0.1312 0.2697 0.053 Uiso 1 1 calc R . . C52 C 0.17943(8) 0.27146(19) 0.30740(16) 0.0298(6) Uani 1 1 d . . . C53 C 0.18214(8) 0.3346(2) 0.35529(17) 0.0334(7) Uani 1 1 d . . . H53A H 0.1767 0.3224 0.3968 0.040 Uiso 1 1 calc R . . C54 C 0.19239(9) 0.4144(2) 0.34506(19) 0.0392(8) Uani 1 1 d . . . H54A H 0.1944 0.4550 0.3795 0.047 Uiso 1 1 calc R . . C55 C 0.19970(10) 0.4346(2) 0.2841(2) 0.0455(9) Uani 1 1 d . . . H55A H 0.2065 0.4890 0.2763 0.055 Uiso 1 1 calc R . . C56 C 0.19695(11) 0.3745(3) 0.2354(2) 0.0502(10) Uani 1 1 d . . . H56A H 0.2018 0.3875 0.1935 0.060 Uiso 1 1 calc R . . C57 C 0.18703(9) 0.2943(2) 0.24712(18) 0.0400(8) Uani 1 1 d . . . H57A H 0.1854 0.2539 0.2127 0.048 Uiso 1 1 calc R . . C58 C 0.3392(2) 0.1742(5) 0.1744(5) 0.137(3) Uani 1 1 d . . . H58A H 0.3250 0.1537 0.1304 0.206 Uiso 1 1 calc R . . H58B H 0.3240 0.1930 0.2018 0.206 Uiso 1 1 calc R . . H58C H 0.3543 0.1297 0.1986 0.206 Uiso 1 1 calc R . . C59 C 0.3422(2) 0.3141(5) 0.1275(5) 0.138(3) Uani 1 1 d . . . H59A H 0.3323 0.3456 0.1587 0.207 Uiso 1 1 calc R . . H59B H 0.3234 0.2950 0.0887 0.207 Uiso 1 1 calc R . . H59C H 0.3582 0.3493 0.1111 0.207 Uiso 1 1 calc R . . C60 C 0.39650(18) 0.2368(3) 0.1720(3) 0.0812(17) Uani 1 1 d . . . H60A H 0.4068 0.1858 0.1896 0.097 Uiso 1 1 calc R . . C61 C 0.2378(2) 0.5026(5) 0.1323(3) 0.123(3) Uani 1 1 d . . . H61A H 0.2576 0.4645 0.1463 0.184 Uiso 1 1 calc R . . H61B H 0.2249 0.5029 0.1668 0.184 Uiso 1 1 calc R . . H61C H 0.2465 0.5582 0.1277 0.184 Uiso 1 1 calc R . . C62 C 0.18447(14) 0.5265(3) 0.0357(3) 0.0691(13) Uani 1 1 d . . . H62A H 0.1707 0.4995 -0.0060 0.104 Uiso 1 1 calc R . . H62B H 0.1921 0.5808 0.0244 0.104 Uiso 1 1 calc R . . H62C H 0.1702 0.5330 0.0675 0.104 Uiso 1 1 calc R . . C63 C 0.22415(17) 0.4120(4) 0.0347(4) 0.0870(18) Uani 1 1 d . . . H63A H 0.2448 0.3825 0.0564 0.104 Uiso 1 1 calc R . . B1 B 0.16468(9) 0.1798(2) 0.31989(18) 0.0291(7) Uani 1 1 d . . . C18 C 0.47617(8) 0.48656(18) -0.13577(15) 0.0283(6) Uani 1 1 d . . . C19 C 0.46874(10) 0.4402(2) -0.19483(16) 0.0390(8) Uani 1 1 d . . . H19A H 0.4788 0.3871 -0.1949 0.047 Uiso 1 1 calc R . . C20 C 0.44644(11) 0.4719(2) -0.25383(17) 0.0442(9) Uani 1 1 d . . . H20A H 0.4409 0.4410 -0.2950 0.053 Uiso 1 1 calc R . . C21 C 0.43255(10) 0.5486(2) -0.25158(17) 0.0392(8) Uani 1 1 d . . . H21A H 0.4174 0.5722 -0.2914 0.047 Uiso 1 1 calc R . . C22 C 0.44074(9) 0.5910(2) -0.19082(17) 0.0383(8) Uani 1 1 d . . . H22A H 0.4307 0.6440 -0.1898 0.046 Uiso 1 1 calc R . . N6 N 0.46217(7) 0.56126(17) -0.13288(13) 0.0323(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0379(4) 0.0318(4) 0.0325(4) 0.0020(3) 0.0166(3) 0.0042(3) Cu1 0.0262(2) 0.0327(2) 0.0302(2) 0.00124(15) 0.00725(16) 0.00444(15) Cu2 0.0276(2) 0.0315(2) 0.0282(2) -0.00456(15) 0.00479(15) 0.00196(15) Cu3 0.0263(2) 0.0293(2) 0.0311(2) 0.00980(15) 0.00779(16) 0.00080(14) O1 0.0309(12) 0.0301(12) 0.0458(14) -0.0020(10) 0.0075(10) 0.0034(9) O2 0.0281(11) 0.0285(11) 0.0301(11) 0.0042(9) 0.0062(9) -0.0016(8) O3 0.0257(11) 0.0374(12) 0.0373(12) 0.0162(10) 0.0085(9) 0.0067(9) O4 0.0295(11) 0.0372(12) 0.0245(11) -0.0010(9) 0.0079(9) 0.0059(9) O5 0.076(3) 0.150(5) 0.202(6) -0.050(5) 0.039(4) -0.032(3) O6 0.112(3) 0.107(3) 0.119(4) -0.045(3) 0.075(3) -0.050(3) N1 0.0285(13) 0.0400(15) 0.0256(13) 0.0088(11) 0.0071(11) 0.0044(11) N2 0.0288(13) 0.0356(14) 0.0295(13) -0.0029(11) 0.0075(11) 0.0034(11) N3 0.048(2) 0.0426(19) 0.055(2) -0.0005(15) 0.0220(17) -0.0004(15) C9A 0.048(2) 0.0426(19) 0.055(2) -0.0005(15) 0.0220(17) -0.0004(15) N4 0.0293(14) 0.0350(14) 0.0341(14) -0.0143(11) 0.0062(11) -0.0021(11) N5 0.0274(13) 0.0282(13) 0.0274(13) -0.0062(10) 0.0085(10) -0.0021(10) N7 0.0282(13) 0.0242(12) 0.0240(12) 0.0020(9) 0.0073(10) 0.0005(9) N8 0.0264(13) 0.0358(14) 0.0297(14) 0.0089(11) 0.0084(11) 0.0045(11) N9 0.0399(19) 0.0340(17) 0.0354(18) 0.0066(13) 0.0140(14) 0.0021(14) C30A 0.0399(19) 0.0340(17) 0.0354(18) 0.0066(13) 0.0140(14) 0.0021(14) N10 0.086(4) 0.087(4) 0.105(4) 0.011(3) 0.023(3) 0.002(3) N11 0.097(3) 0.075(3) 0.070(3) -0.008(2) 0.038(3) -0.042(3) C1 0.0350(18) 0.0390(18) 0.0355(18) 0.0080(14) 0.0103(14) 0.0039(14) C2 0.042(2) 0.0412(19) 0.0406(19) 0.0118(15) 0.0129(16) 0.0070(15) C3 0.046(2) 0.044(2) 0.044(2) 0.0131(16) 0.0108(17) 0.0126(16) C4 0.0331(18) 0.053(2) 0.0378(19) 0.0084(16) 0.0089(15) 0.0091(15) C5 0.0304(16) 0.0411(18) 0.0270(16) 0.0036(13) 0.0099(13) 0.0050(13) C6 0.0262(15) 0.0429(18) 0.0260(15) 0.0039(13) 0.0064(12) 0.0031(13) C7 0.0305(17) 0.0400(18) 0.0402(19) 0.0019(15) 0.0116(14) 0.0046(14) C8 0.0220(16) 0.063(2) 0.042(2) 0.0189(17) -0.0001(14) 0.0026(15) C9 0.042(2) 0.092(4) 0.089(4) 0.008(3) -0.005(2) 0.008(2) N3A 0.042(2) 0.092(4) 0.089(4) 0.008(3) -0.005(2) 0.008(2) C10 0.039(2) 0.056(3) 0.085(3) 0.000(2) 0.025(2) -0.0026(18) C11 0.047(2) 0.044(2) 0.070(3) -0.0006(19) 0.031(2) -0.0003(17) C12 0.0312(18) 0.050(2) 0.048(2) -0.0249(17) 0.0102(16) -0.0055(15) C13 0.037(2) 0.066(3) 0.056(2) -0.033(2) 0.0182(18) -0.0165(18) C14 0.048(2) 0.061(2) 0.041(2) -0.0169(18) 0.0208(18) -0.0242(19) C15 0.046(2) 0.049(2) 0.0320(17) -0.0147(15) 0.0169(15) -0.0211(16) C16 0.0367(18) 0.0357(17) 0.0294(16) -0.0143(13) 0.0119(14) -0.0076(14) C17 0.0325(16) 0.0274(15) 0.0248(14) -0.0061(12) 0.0090(12) -0.0031(12) C23 0.0336(16) 0.0248(14) 0.0247(15) 0.0029(11) 0.0039(12) 0.0018(12) C24 0.0330(17) 0.0316(16) 0.0307(16) 0.0036(13) -0.0001(13) 0.0017(13) C25 0.0272(16) 0.0399(18) 0.0408(19) 0.0063(14) 0.0036(14) -0.0010(13) C26 0.0311(16) 0.0347(17) 0.0320(16) 0.0073(13) 0.0085(13) -0.0012(13) C27 0.0304(16) 0.0269(14) 0.0250(15) 0.0006(11) 0.0089(12) -0.0001(12) C28 0.0290(16) 0.0279(15) 0.0291(15) 0.0040(12) 0.0111(13) 0.0026(12) C29 0.0285(15) 0.0313(15) 0.0268(15) 0.0046(12) 0.0108(12) 0.0008(12) C30 0.0318(15) 0.0364(15) 0.0341(15) 0.0111(12) 0.0145(12) 0.0031(11) N9A 0.0318(15) 0.0364(15) 0.0341(15) 0.0111(12) 0.0145(12) 0.0031(11) C31 0.0310(18) 0.059(2) 0.051(2) 0.0262(18) 0.0192(16) 0.0044(16) C32 0.0347(19) 0.046(2) 0.062(2) 0.0292(18) 0.0110(17) -0.0001(15) C33 0.043(2) 0.0301(17) 0.059(2) 0.0109(16) 0.0075(18) 0.0011(15) C34 0.0317(16) 0.0227(14) 0.0299(15) -0.0067(12) 0.0100(13) -0.0034(12) C35 0.0328(16) 0.0231(14) 0.0257(15) -0.0022(11) 0.0059(12) 0.0006(12) C36 0.0357(17) 0.0241(14) 0.0303(16) -0.0029(12) 0.0126(13) -0.0033(12) C37 0.0285(16) 0.0214(14) 0.0380(17) -0.0021(12) 0.0086(13) 0.0004(11) C38 0.0353(17) 0.0219(14) 0.0303(16) -0.0014(12) 0.0047(13) -0.0005(12) C39 0.0360(17) 0.0246(14) 0.0271(15) -0.0032(12) 0.0103(13) -0.0016(12) C40 0.0316(16) 0.0317(16) 0.0317(16) -0.0065(12) 0.0126(13) 0.0048(12) C41 0.0285(16) 0.0330(17) 0.0430(19) -0.0016(14) 0.0051(14) 0.0018(13) C42 0.0364(19) 0.0377(18) 0.046(2) 0.0051(15) 0.0117(16) 0.0062(15) C43 0.0357(18) 0.045(2) 0.0370(18) -0.0001(15) 0.0063(15) 0.0154(15) C44 0.0321(17) 0.0381(18) 0.0356(17) -0.0089(14) 0.0021(14) 0.0048(14) C45 0.0335(17) 0.0347(17) 0.0321(17) -0.0055(13) 0.0098(14) 0.0028(13) C46 0.0382(18) 0.0342(16) 0.0283(16) -0.0002(13) 0.0099(14) 0.0068(13) C47 0.0435(19) 0.0327(17) 0.0394(18) -0.0094(14) 0.0146(15) -0.0008(14) C48 0.062(3) 0.040(2) 0.056(2) -0.0175(18) 0.019(2) -0.0008(18) C49 0.076(3) 0.049(2) 0.045(2) -0.0142(18) 0.013(2) 0.018(2) C50 0.049(2) 0.060(2) 0.044(2) -0.0048(18) 0.0160(18) 0.0225(19) C51 0.0377(19) 0.058(2) 0.0355(19) -0.0074(16) 0.0078(15) 0.0092(16) C52 0.0258(15) 0.0333(16) 0.0301(16) -0.0011(12) 0.0076(13) 0.0007(12) C53 0.0311(17) 0.0357(17) 0.0343(17) -0.0016(13) 0.0106(14) 0.0021(13) C54 0.0322(17) 0.0348(17) 0.048(2) -0.0031(15) 0.0071(15) 0.0026(14) C55 0.039(2) 0.043(2) 0.053(2) 0.0029(17) 0.0105(17) -0.0075(15) C56 0.057(2) 0.053(2) 0.045(2) 0.0028(18) 0.0211(19) -0.0148(19) C57 0.045(2) 0.0403(19) 0.0365(18) -0.0050(15) 0.0145(16) -0.0081(15) C58 0.177(8) 0.114(6) 0.157(8) -0.003(5) 0.107(7) -0.030(6) C59 0.116(6) 0.092(5) 0.212(10) 0.033(6) 0.055(6) 0.035(5) C60 0.090(4) 0.042(3) 0.093(4) -0.014(2) -0.006(3) -0.023(3) C61 0.153(6) 0.141(6) 0.066(4) 0.003(4) 0.018(4) -0.100(5) C62 0.078(3) 0.059(3) 0.081(3) -0.014(3) 0.040(3) -0.015(3) C63 0.090(4) 0.083(4) 0.103(5) -0.016(4) 0.053(4) -0.041(3) B1 0.0297(18) 0.0299(17) 0.0283(17) -0.0034(13) 0.0088(14) -0.0005(13) C18 0.0342(16) 0.0276(15) 0.0241(15) -0.0026(11) 0.0100(12) -0.0110(12) C19 0.064(2) 0.0264(15) 0.0261(16) -0.0034(12) 0.0115(16) -0.0089(15) C20 0.069(3) 0.0362(18) 0.0226(16) -0.0045(13) 0.0040(16) -0.0143(17) C21 0.047(2) 0.0420(19) 0.0254(16) 0.0019(14) 0.0037(14) -0.0077(15) C22 0.0383(18) 0.0412(18) 0.0327(18) -0.0063(14) 0.0053(14) 0.0013(15) N6 0.0314(14) 0.0380(15) 0.0256(13) -0.0067(11) 0.0045(11) 0.0009(11) _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 Cl1 Cu3 2.4824(9) . ? Cl1 Cu1 2.6700(9) . ? Cu1 O3 1.942(2) . ? Cu1 O4 1.977(2) . ? Cu1 N2 1.980(3) . ? Cu1 N1 1.987(3) . ? Cu1 Cu3 3.0455(6) . ? Cu2 O4 1.936(2) . ? Cu2 O1 1.969(2) . ? Cu2 N4 1.971(3) . ? Cu2 N5 1.988(3) . ? Cu2 N6 2.271(3) 5_665 ? Cu3 O2 1.932(2) . ? Cu3 N8 1.968(3) . ? Cu3 N7 1.979(3) . ? Cu3 O4 2.053(2) . ? O1 N2 1.325(4) . ? O2 N5 1.332(3) . ? O3 N8 1.333(3) . ? O5 C60 1.085(7) . ? O6 C63 1.216(7) . ? N1 C1 1.344(4) . ? N1 C5 1.363(4) . ? N2 C6 1.298(4) . ? N3 C7 1.385(5) . ? N3 C11 1.386(5) . ? N4 C12 1.335(4) . ? N4 C16 1.364(4) . ? N5 C17 1.296(4) . ? N7 C27 1.349(4) . ? N7 C23 1.353(4) . ? N8 C28 1.300(4) . ? N9 C33 1.379(5) . ? N9 C29 1.381(4) . ? N10 C60 1.379(8) . ? N10 C59 1.447(8) . ? N10 C58 1.484(8) . ? N11 C63 1.339(7) . ? N11 C61 1.456(7) . ? N11 C62 1.457(7) . ? C1 C2 1.387(5) . ? C2 C3 1.383(5) . ? C3 C4 1.392(5) . ? C4 C5 1.386(5) . ? C5 C6 1.459(5) . ? C6 C7 1.506(5) . ? C7 C8 1.319(5) . ? C8 C9 1.355(6) . ? C9 C10 1.369(7) . ? C10 C11 1.362(6) . ? C12 C13 1.401(6) . ? C13 C14 1.375(6) . ? C14 C15 1.388(5) . ? C15 C16 1.395(5) . ? C16 C17 1.464(4) . ? C17 C18 1.484(4) . ? C23 C24 1.377(4) . ? C24 C25 1.384(5) . ? C25 C26 1.386(4) . ? C26 C27 1.390(4) . ? C27 C28 1.482(4) . ? C28 C29 1.477(4) . ? C29 C30 1.344(4) . ? C30 C31 1.337(4) . ? C31 C32 1.373(6) . ? C32 C33 1.379(6) . ? C34 C39 1.402(4) . ? C34 C35 1.407(4) . ? C34 B1 1.650(5) . ? C35 C36 1.390(4) . ? C36 C37 1.386(4) . ? C37 C38 1.392(5) . ? C38 C39 1.383(4) . ? C40 C45 1.397(4) . ? C40 C41 1.399(5) . ? C40 B1 1.648(5) . ? C41 C42 1.393(5) . ? C42 C43 1.392(5) . ? C43 C44 1.376(5) . ? C44 C45 1.401(5) . ? C46 C47 1.397(5) . ? C46 C51 1.407(5) . ? C46 B1 1.640(5) . ? C47 C48 1.387(5) . ? C48 C49 1.374(6) . ? C49 C50 1.369(6) . ? C50 C51 1.397(5) . ? C52 C57 1.395(5) . ? C52 C53 1.400(4) . ? C52 B1 1.645(5) . ? C53 C54 1.391(5) . ? C54 C55 1.392(5) . ? C55 C56 1.375(6) . ? C56 C57 1.400(5) . ? C18 N6 1.343(4) . ? C18 C19 1.382(4) . ? C19 C20 1.385(5) . ? C20 C21 1.368(5) . ? C21 C22 1.377(5) . ? C22 N6 1.344(4) . ? N6 Cu2 2.271(3) 5_665 ? 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 Cu3 Cl1 Cu1 72.36(2) . . ? O3 Cu1 O4 93.53(9) . . ? O3 Cu1 N2 171.69(10) . . ? O4 Cu1 N2 89.40(10) . . ? O3 Cu1 N1 95.16(10) . . ? O4 Cu1 N1 163.11(10) . . ? N2 Cu1 N1 80.13(11) . . ? O3 Cu1 Cl1 91.15(7) . . ? O4 Cu1 Cl1 79.18(6) . . ? N2 Cu1 Cl1 97.05(8) . . ? N1 Cu1 Cl1 115.04(8) . . ? O3 Cu1 Cu3 66.89(6) . . ? O4 Cu1 Cu3 41.87(6) . . ? N2 Cu1 Cu3 119.69(8) . . ? N1 Cu1 Cu3 154.61(8) . . ? Cl1 Cu1 Cu3 50.968(19) . . ? O4 Cu2 O1 92.92(9) . . ? O4 Cu2 N4 171.94(10) . . ? O1 Cu2 N4 90.47(11) . . ? O4 Cu2 N5 93.16(10) . . ? O1 Cu2 N5 152.13(10) . . ? N4 Cu2 N5 80.51(11) . . ? O4 Cu2 N6 93.07(9) . 5_665 ? O1 Cu2 N6 97.37(10) . 5_665 ? N4 Cu2 N6 93.76(10) . 5_665 ? N5 Cu2 N6 109.42(10) . 5_665 ? O2 Cu3 N8 171.48(10) . . ? O2 Cu3 N7 92.70(9) . . ? N8 Cu3 N7 80.57(10) . . ? O2 Cu3 O4 96.21(9) . . ? N8 Cu3 O4 86.42(10) . . ? N7 Cu3 O4 144.12(9) . . ? O2 Cu3 Cl1 96.66(7) . . ? N8 Cu3 Cl1 91.71(8) . . ? N7 Cu3 Cl1 130.82(7) . . ? O4 Cu3 Cl1 82.54(6) . . ? O2 Cu3 Cu1 125.40(6) . . ? N8 Cu3 Cu1 61.05(7) . . ? N7 Cu3 Cu1 141.61(7) . . ? O4 Cu3 Cu1 39.98(6) . . ? Cl1 Cu3 Cu1 56.67(2) . . ? N2 O1 Cu2 115.30(18) . . ? N5 O2 Cu3 111.33(17) . . ? N8 O3 Cu1 110.27(17) . . ? Cu2 O4 Cu1 111.19(10) . . ? Cu2 O4 Cu3 107.05(10) . . ? Cu1 O4 Cu3 98.15(10) . . ? C1 N1 C5 119.4(3) . . ? C1 N1 Cu1 126.5(2) . . ? C5 N1 Cu1 113.9(2) . . ? C6 N2 O1 120.4(3) . . ? C6 N2 Cu1 117.2(2) . . ? O1 N2 Cu1 122.35(19) . . ? C7 N3 C11 119.0(4) . . ? C12 N4 C16 119.2(3) . . ? C12 N4 Cu2 126.7(3) . . ? C16 N4 Cu2 113.9(2) . . ? C17 N5 O2 119.1(3) . . ? C17 N5 Cu2 116.4(2) . . ? O2 N5 Cu2 124.45(19) . . ? C27 N7 C23 119.6(3) . . ? C27 N7 Cu3 113.83(19) . . ? C23 N7 Cu3 126.2(2) . . ? C28 N8 O3 120.8(3) . . ? C28 N8 Cu3 117.5(2) . . ? O3 N8 Cu3 121.65(19) . . ? C33 N9 C29 119.1(3) . . ? C60 N10 C59 120.3(6) . . ? C60 N10 C58 122.8(6) . . ? C59 N10 C58 115.5(7) . . ? C63 N11 C61 119.3(6) . . ? C63 N11 C62 121.8(5) . . ? C61 N11 C62 118.4(5) . . ? N1 C1 C2 122.4(3) . . ? C3 C2 C1 118.4(3) . . ? C2 C3 C4 119.6(3) . . ? C5 C4 C3 119.4(3) . . ? N1 C5 C4 120.7(3) . . ? N1 C5 C6 114.3(3) . . ? C4 C5 C6 124.9(3) . . ? N2 C6 C5 113.9(3) . . ? N2 C6 C7 121.9(3) . . ? C5 C6 C7 124.2(3) . . ? C8 C7 N3 123.2(3) . . ? C8 C7 C6 117.1(3) . . ? N3 C7 C6 119.6(3) . . ? C7 C8 C9 116.5(4) . . ? C8 C9 C10 123.9(4) . . ? C11 C10 C9 118.7(4) . . ? C10 C11 N3 118.6(4) . . ? N4 C12 C13 121.9(4) . . ? C14 C13 C12 119.1(4) . . ? C13 C14 C15 119.5(4) . . ? C14 C15 C16 119.0(4) . . ? N4 C16 C15 121.3(3) . . ? N4 C16 C17 114.4(3) . . ? C15 C16 C17 124.3(3) . . ? N5 C17 C16 114.1(3) . . ? N5 C17 C18 124.4(3) . . ? C16 C17 C18 121.0(3) . . ? N7 C23 C24 122.1(3) . . ? C23 C24 C25 118.4(3) . . ? C24 C25 C26 120.0(3) . . ? C25 C26 C27 119.0(3) . . ? N7 C27 C26 120.9(3) . . ? N7 C27 C28 114.8(3) . . ? C26 C27 C28 124.3(3) . . ? N8 C28 C29 123.8(3) . . ? N8 C28 C27 112.8(3) . . ? C29 C28 C27 123.4(3) . . ? C30 C29 N9 122.7(3) . . ? C30 C29 C28 116.4(3) . . ? N9 C29 C28 120.8(3) . . ? C31 C30 C29 117.0(3) . . ? C30 C31 C32 123.8(3) . . ? C31 C32 C33 118.6(3) . . ? C32 C33 N9 118.7(3) . . ? C39 C34 C35 114.8(3) . . ? C39 C34 B1 120.3(3) . . ? C35 C34 B1 124.8(3) . . ? C36 C35 C34 122.7(3) . . ? C37 C36 C35 120.6(3) . . ? C36 C37 C38 118.2(3) . . ? C39 C38 C37 120.4(3) . . ? C38 C39 C34 123.3(3) . . ? C45 C40 C41 115.2(3) . . ? C45 C40 B1 124.0(3) . . ? C41 C40 B1 120.5(3) . . ? C42 C41 C40 123.3(3) . . ? C43 C42 C41 119.6(3) . . ? C44 C43 C42 118.9(3) . . ? C43 C44 C45 120.5(3) . . ? C40 C45 C44 122.5(3) . . ? C47 C46 C51 114.4(3) . . ? C47 C46 B1 123.7(3) . . ? C51 C46 B1 121.5(3) . . ? C48 C47 C46 123.0(3) . . ? C49 C48 C47 120.6(4) . . ? C50 C49 C48 119.1(4) . . ? C49 C50 C51 120.0(4) . . ? C50 C51 C46 122.9(4) . . ? C57 C52 C53 115.2(3) . . ? C57 C52 B1 123.4(3) . . ? C53 C52 B1 121.1(3) . . ? C54 C53 C52 123.1(3) . . ? C53 C54 C55 119.7(3) . . ? C56 C55 C54 119.0(3) . . ? C55 C56 C57 120.3(3) . . ? C52 C57 C56 122.6(3) . . ? O5 C60 N10 127.5(7) . . ? O6 C63 N11 122.2(7) . . ? C46 B1 C52 112.4(3) . . ? C46 B1 C40 103.8(2) . . ? C52 B1 C40 112.7(3) . . ? C46 B1 C34 111.2(3) . . ? C52 B1 C34 105.0(2) . . ? C40 B1 C34 112.0(3) . . ? N6 C18 C19 122.5(3) . . ? N6 C18 C17 118.2(3) . . ? C19 C18 C17 119.2(3) . . ? C18 C19 C20 119.2(3) . . ? C21 C20 C19 118.6(3) . . ? C20 C21 C22 119.2(3) . . ? N6 C22 C21 123.2(3) . . ? C18 N6 C22 117.2(3) . . ? C18 N6 Cu2 128.9(2) . 5_665 ? C22 N6 Cu2 113.6(2) . 5_665 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.975 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.093 # Attachment 'f16b1.cif' data_f16b _database_code_depnum_ccdc_archive 'CCDC 633712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C77 H56 Cu5 N21 O7, 2(C H4 O), 3(Cl O4), 2(H2 O)' _chemical_formula_sum 'C79 H68 Cl3 Cu5 N21 O23' _chemical_formula_weight 2103.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.0171(15) _cell_length_b 17.4816(16) _cell_length_c 18.7802(18) _cell_angle_alpha 67.822(5) _cell_angle_beta 63.093(5) _cell_angle_gamma 62.629(5) _cell_volume 4321.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 108(2) _cell_measurement_reflns_used 8494 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.01 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2138 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6646 _exptl_absorpt_correction_T_max 0.7684 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_special_details ; 4095 frames x 45 sec. @ 4.969 cm; 0.5 deg. steps in omega & phi ; _diffrn_ambient_temperature 108(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 133448 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.62 _reflns_number_total 21550 _reflns_number_gt 15858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-1K' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Use of the SQUEEZE sub-routine of the PLATON program suite - (PLATON Reference : Spek, A.L. (2003), J. Appl Cryst. 2003, 36, 7-13) indicated the presence of 4 solvent accessible voids with a total volume of 146 A^3 and containing the contribution of 44 electrons due to diffuse solvent scattering. This has been included as two water molecules per copper complex. One perchlorate anion was refined with restraints (SAME) to maintain reasonable chemical geometry. Two ligands are disorderd by a rotation that brings a carbon and nitrogen position into coincidence. The atoms affected are N21/C74 and N15/C52. These were modeled as partial contributions of both N and C scattering with a free variable (contrained to sum to unity) assigned to refine the ratio. 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^)+(0.0726P)^2^+3.8348P] 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 21550 _refine_ls_number_parameters 1168 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.140 _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 0.81494(2) 0.33577(2) 0.28537(2) 0.01959(9) Uani 1 1 d . . . Cu2 Cu 0.68496(2) 0.12706(2) 0.50633(2) 0.01987(9) Uani 1 1 d . . . Cu3 Cu 0.92491(2) 0.10554(2) 0.37763(2) 0.02124(9) Uani 1 1 d . . . Cu4 Cu 0.91404(3) 0.12869(2) 0.18777(2) 0.02269(9) Uani 1 1 d . . . Cu5 Cu 0.98627(3) 0.31570(2) 0.12014(2) 0.02121(9) Uani 1 1 d . . . O1 O 0.84226(14) 0.19186(14) 0.45013(13) 0.0215(4) Uani 1 1 d . . . O2 O 0.88133(15) 0.00862(14) 0.44196(14) 0.0254(5) Uani 1 1 d . . . O3 O 0.83240(14) 0.15109(13) 0.31086(13) 0.0209(4) Uani 1 1 d . . . O4 O 0.95090(14) 0.27200(13) 0.26336(13) 0.0213(4) Uani 1 1 d . . . O5 O 1.06501(15) 0.20574(15) 0.08605(15) 0.0274(5) Uani 1 1 d . . . O6 O 0.86415(15) 0.32079(14) 0.13120(14) 0.0242(5) Uani 1 1 d . . . O7 O 0.84658(14) 0.44272(14) 0.22104(13) 0.0219(4) Uani 1 1 d . . . N1 N 0.78187(18) 0.38481(16) 0.40408(16) 0.0206(5) Uani 1 1 d . . . N2 N 0.75118(17) 0.20961(16) 0.47809(15) 0.0192(5) Uani 1 1 d . . . N3 N 0.57364(17) 0.23872(16) 0.52395(16) 0.0200(5) Uani 1 1 d . . . N4 N 0.62783(18) 0.04200(17) 0.60673(16) 0.0219(5) Uani 1 1 d . . . N5 N 0.79760(18) 0.01733(17) 0.49947(16) 0.0228(5) Uani 1 1 d . . . N6 N 0.93486(19) -0.16477(17) 0.54942(18) 0.0258(6) Uani 1 1 d . . . N7 N 0.65135(18) 0.12097(17) 0.40988(16) 0.0224(5) Uani 1 1 d . . . N8 N 0.77431(17) 0.23539(16) 0.31286(15) 0.0199(5) Uani 1 1 d . . . N9 N 0.67868(18) 0.40177(17) 0.29542(16) 0.0212(5) Uani 1 1 d . . . N10 N 1.05688(17) 0.02169(17) 0.35646(16) 0.0213(5) Uani 1 1 d . . . N11 N 0.99166(17) 0.18705(16) 0.29586(15) 0.0197(5) Uani 1 1 d . . . N12 N 1.22309(19) 0.1753(2) 0.16359(18) 0.0296(6) Uani 1 1 d . . . N13 N 0.98610(18) 0.00518(17) 0.22644(17) 0.0241(5) Uani 1 1 d . . . N14 N 1.04373(18) 0.13404(17) 0.13019(16) 0.0236(5) Uani 1 1 d . . . N15 N 1.2800(2) -0.0095(2) 0.0921(2) 0.0318(8) Uani 0.54(3) 1 d P A 1 C52A C 1.2800(2) -0.0095(2) 0.0921(2) 0.0318(8) Uani 0.46(3) 1 d P A 2 H52A H 1.2704 -0.0445 0.1461 0.038 Uiso 0.46(3) 1 calc PR A 2 N16 N 0.82191(19) 0.10430(18) 0.16304(18) 0.0267(6) Uani 1 1 d . . . N17 N 0.85371(18) 0.24844(17) 0.13357(16) 0.0227(5) Uani 1 1 d . . . N18 N 0.6487(2) 0.3819(2) 0.1269(2) 0.0417(8) Uani 1 1 d . . . N19 N 1.08844(18) 0.36663(18) 0.05311(16) 0.0231(5) Uani 1 1 d . . . N20 N 0.92765(17) 0.42670(17) 0.15891(15) 0.0212(5) Uani 1 1 d . . . N21A N 0.8602(2) 0.6093(2) 0.1926(2) 0.0282(8) Uani 0.08(3) 1 d P B 2 C74 C 0.8602(2) 0.6093(2) 0.1926(2) 0.0282(8) Uani 0.92(3) 1 d P B 1 H74A H 0.8099 0.6016 0.1898 0.034 Uiso 0.92(3) 1 calc PR B 1 C1 C 0.8167(2) 0.4459(2) 0.3904(2) 0.0241(6) Uani 1 1 d . . . H1A H 0.8509 0.4674 0.3357 0.029 Uiso 1 1 calc R . . C2 C 0.8053(2) 0.4794(2) 0.4524(2) 0.0265(7) Uani 1 1 d . . . H2A H 0.8297 0.5238 0.4399 0.032 Uiso 1 1 calc R . . C3 C 0.7575(2) 0.4466(2) 0.5329(2) 0.0285(7) Uani 1 1 d . . . H3A H 0.7498 0.4672 0.5765 0.034 Uiso 1 1 calc R . . C4 C 0.7213(2) 0.3833(2) 0.5479(2) 0.0238(6) Uani 1 1 d . . . H4A H 0.6882 0.3597 0.6021 0.029 Uiso 1 1 calc R . . C5 C 0.7341(2) 0.35456(19) 0.48225(19) 0.0194(6) Uani 1 1 d . . . C6 C 0.6961(2) 0.28739(18) 0.49544(18) 0.0181(6) Uani 1 1 d . . . C7 C 0.5957(2) 0.30496(19) 0.52170(18) 0.0198(6) Uani 1 1 d . . . C8 C 0.5260(2) 0.3852(2) 0.53849(19) 0.0229(6) Uani 1 1 d . . . H8A H 0.5421 0.4315 0.5365 0.027 Uiso 1 1 calc R . . C9 C 0.4335(2) 0.3965(2) 0.5580(2) 0.0249(6) Uani 1 1 d . . . H9A H 0.3850 0.4501 0.5715 0.030 Uiso 1 1 calc R . . C10 C 0.4113(2) 0.3297(2) 0.5580(2) 0.0252(6) Uani 1 1 d . . . H10A H 0.3480 0.3372 0.5696 0.030 Uiso 1 1 calc R . . C11 C 0.4838(2) 0.2514(2) 0.54048(19) 0.0231(6) Uani 1 1 d . . . H11A H 0.4693 0.2052 0.5402 0.028 Uiso 1 1 calc R . . C12 C 0.5448(2) 0.0598(2) 0.6675(2) 0.0251(6) Uani 1 1 d . . . H12B H 0.5014 0.1186 0.6637 0.030 Uiso 1 1 calc R . . C13 C 0.5197(2) -0.0038(2) 0.7354(2) 0.0284(7) Uani 1 1 d . . . H13A H 0.4600 0.0110 0.7770 0.034 Uiso 1 1 calc R . . C14 C 0.5833(2) -0.0895(2) 0.7413(2) 0.0277(7) Uani 1 1 d . . . H14A H 0.5681 -0.1343 0.7875 0.033 Uiso 1 1 calc R . . C15 C 0.6692(2) -0.1090(2) 0.6793(2) 0.0264(7) Uani 1 1 d . . . H15B H 0.7135 -0.1675 0.6819 0.032 Uiso 1 1 calc R . . C16 C 0.6901(2) -0.0416(2) 0.6127(2) 0.0231(6) Uani 1 1 d . . . C17 C 0.7824(2) -0.0545(2) 0.5481(2) 0.0228(6) Uani 1 1 d . . . C18 C 0.8537(2) -0.1441(2) 0.5397(2) 0.0244(6) Uani 1 1 d . . . C19 C 0.8337(3) -0.2006(2) 0.5203(3) 0.0378(9) Uani 1 1 d . . . H19A H 0.7746 -0.1837 0.5150 0.045 Uiso 1 1 calc R . . C20 C 0.9022(3) -0.2830(3) 0.5087(3) 0.0462(11) Uani 1 1 d . . . H20A H 0.8909 -0.3233 0.4952 0.055 Uiso 1 1 calc R . . C21 C 0.9864(3) -0.3046(2) 0.5171(3) 0.0385(9) Uani 1 1 d . . . H21B H 1.0351 -0.3597 0.5083 0.046 Uiso 1 1 calc R . . C22 C 0.9992(2) -0.2446(2) 0.5388(2) 0.0309(7) Uani 1 1 d . . . H22A H 1.0568 -0.2610 0.5466 0.037 Uiso 1 1 calc R . . C23 C 0.6174(2) 0.0595(2) 0.4228(2) 0.0264(7) Uani 1 1 d . . . H23A H 0.6213 0.0120 0.4690 0.032 Uiso 1 1 calc R . . C24 C 0.5772(2) 0.0616(2) 0.3723(2) 0.0314(7) Uani 1 1 d . . . H24A H 0.5546 0.0162 0.3834 0.038 Uiso 1 1 calc R . . C25 C 0.5702(2) 0.1309(2) 0.3050(2) 0.0303(7) Uani 1 1 d . . . H25A H 0.5417 0.1345 0.2700 0.036 Uiso 1 1 calc R . . C26 C 0.6057(2) 0.1950(2) 0.2900(2) 0.0263(7) Uani 1 1 d . . . H26A H 0.6025 0.2430 0.2442 0.032 Uiso 1 1 calc R . . C27 C 0.6460(2) 0.1874(2) 0.34314(19) 0.0216(6) Uani 1 1 d . . . C28 C 0.6863(2) 0.2544(2) 0.32673(18) 0.0201(6) Uani 1 1 d . . . C29 C 0.6293(2) 0.3487(2) 0.31918(18) 0.0208(6) Uani 1 1 d . . . C30 C 0.5330(2) 0.3829(2) 0.3331(2) 0.0244(6) Uani 1 1 d . . . H30A H 0.4985 0.3450 0.3521 0.029 Uiso 1 1 calc R . . C31 C 0.4890(2) 0.4737(2) 0.3185(2) 0.0283(7) Uani 1 1 d . . . H31A H 0.4237 0.4987 0.3263 0.034 Uiso 1 1 calc R . . C32 C 0.5399(2) 0.5278(2) 0.2927(2) 0.0281(7) Uani 1 1 d . . . H32A H 0.5104 0.5901 0.2824 0.034 Uiso 1 1 calc R . . C33 C 0.6347(2) 0.4893(2) 0.2821(2) 0.0247(6) Uani 1 1 d . . . H33A H 0.6699 0.5262 0.2648 0.030 Uiso 1 1 calc R . . C34 C 1.0837(2) -0.0652(2) 0.3882(2) 0.0252(6) Uani 1 1 d . . . H34A H 1.0372 -0.0905 0.4260 0.030 Uiso 1 1 calc R . . C35 C 1.1775(2) -0.1191(2) 0.3674(2) 0.0277(7) Uani 1 1 d . . . H35A H 1.1949 -0.1809 0.3888 0.033 Uiso 1 1 calc R . . C36 C 1.2450(2) -0.0819(2) 0.3153(2) 0.0299(7) Uani 1 1 d . . . H36A H 1.3097 -0.1177 0.3008 0.036 Uiso 1 1 calc R . . C37 C 1.2177(2) 0.0085(2) 0.2843(2) 0.0291(7) Uani 1 1 d . . . H37A H 1.2636 0.0353 0.2492 0.035 Uiso 1 1 calc R . . C38 C 1.1230(2) 0.0591(2) 0.3050(2) 0.0225(6) Uani 1 1 d . . . C39 C 1.0834(2) 0.1553(2) 0.27382(19) 0.0209(6) Uani 1 1 d . . . C40 C 1.1448(2) 0.2100(2) 0.2226(2) 0.0243(6) Uani 1 1 d . . . C41 C 1.1218(2) 0.2895(2) 0.2396(2) 0.0275(7) Uani 1 1 d . . . H41A H 1.0648 0.3125 0.2810 0.033 Uiso 1 1 calc R . . C42 C 1.1845(3) 0.3353(2) 0.1945(2) 0.0342(8) Uani 1 1 d . . . H42A H 1.1720 0.3893 0.2053 0.041 Uiso 1 1 calc R . . C43 C 1.2656(3) 0.2997(3) 0.1333(2) 0.0371(9) Uani 1 1 d . . . H43A H 1.3095 0.3294 0.1011 0.045 Uiso 1 1 calc R . . C44 C 1.2813(3) 0.2208(3) 0.1202(2) 0.0366(8) Uani 1 1 d . . . H44A H 1.3367 0.1974 0.0779 0.044 Uiso 1 1 calc R . . C45 C 0.9510(2) -0.0553(2) 0.2838(2) 0.0280(7) Uani 1 1 d . . . H45A H 0.8867 -0.0372 0.3173 0.034 Uiso 1 1 calc R . . C46 C 1.0059(3) -0.1444(2) 0.2959(2) 0.0340(8) Uani 1 1 d . . . H46A H 0.9798 -0.1868 0.3370 0.041 Uiso 1 1 calc R . . C47 C 1.0987(3) -0.1693(2) 0.2471(3) 0.0388(9) Uani 1 1 d . . . H47A H 1.1373 -0.2299 0.2534 0.047 Uiso 1 1 calc R . . C48 C 1.1363(2) -0.1062(2) 0.1885(2) 0.0334(8) Uani 1 1 d . . . H48A H 1.2007 -0.1232 0.1548 0.040 Uiso 1 1 calc R . . C49 C 1.0789(2) -0.0183(2) 0.1797(2) 0.0256(7) Uani 1 1 d . . . C50 C 1.1099(2) 0.0569(2) 0.1231(2) 0.0257(7) Uani 1 1 d . A . C51 C 1.2072(2) 0.0463(2) 0.0656(2) 0.0265(7) Uani 1 1 d . . . C52 C 1.2179(3) 0.0934(3) -0.0126(2) 0.0472(11) Uani 0.54(3) 1 d P A 1 H52B H 1.1653 0.1284 -0.0304 0.057 Uiso 0.54(3) 1 calc PR A 1 N15A N 1.2179(3) 0.0934(3) -0.0126(2) 0.0472(11) Uani 0.46(3) 1 d P A 2 C53 C 1.3075(4) 0.0886(3) -0.0646(3) 0.0543(13) Uani 1 1 d . . . H53A H 1.3166 0.1233 -0.1187 0.065 Uiso 1 1 calc R A 1 C54 C 1.3841(3) 0.0347(3) -0.0404(3) 0.0464(11) Uani 1 1 d . A . H54A H 1.4459 0.0312 -0.0770 0.056 Uiso 1 1 calc R . . C55 C 1.3691(3) -0.0137(3) 0.0375(3) 0.0437(10) Uani 1 1 d . . . H55A H 1.4217 -0.0517 0.0549 0.052 Uiso 1 1 calc R A 1 C56 C 0.8091(3) 0.0293(2) 0.1778(2) 0.0324(8) Uani 1 1 d . . . H56A H 0.8396 -0.0220 0.2109 0.039 Uiso 1 1 calc R . . C57 C 0.7528(3) 0.0236(3) 0.1463(3) 0.0402(9) Uani 1 1 d . . . H57A H 0.7438 -0.0303 0.1588 0.048 Uiso 1 1 calc R . . C58 C 0.7102(3) 0.0967(3) 0.0969(3) 0.0425(9) Uani 1 1 d . . . H58A H 0.6726 0.0934 0.0739 0.051 Uiso 1 1 calc R . . C59 C 0.7225(3) 0.1761(3) 0.0809(2) 0.0348(8) Uani 1 1 d . . . H59A H 0.6936 0.2276 0.0469 0.042 Uiso 1 1 calc R . . C60 C 0.7778(2) 0.1776(2) 0.1159(2) 0.0267(7) Uani 1 1 d . . . C61 C 0.7911(2) 0.2589(2) 0.1063(2) 0.0254(6) Uani 1 1 d . . . C62 C 0.7315(2) 0.3463(2) 0.0716(2) 0.0288(7) Uani 1 1 d . . . C63 C 0.7588(3) 0.3851(3) -0.0104(2) 0.0359(8) Uani 1 1 d . . . H63A H 0.8180 0.3571 -0.0472 0.043 Uiso 1 1 calc R . . C64 C 0.6976(3) 0.4661(3) -0.0381(3) 0.0462(10) Uani 1 1 d . . . H64A H 0.7140 0.4947 -0.0942 0.055 Uiso 1 1 calc R . . C65 C 0.6128(3) 0.5037(3) 0.0177(3) 0.0485(11) Uani 1 1 d . . . H65A H 0.5695 0.5590 0.0008 0.058 Uiso 1 1 calc R . . C66 C 0.5918(3) 0.4602(3) 0.0978(3) 0.0519(11) Uani 1 1 d . . . H66A H 0.5330 0.4872 0.1355 0.062 Uiso 1 1 calc R . . C67 C 1.1684(2) 0.3324(2) -0.0047(2) 0.0261(7) Uani 1 1 d . . . H67A H 1.1835 0.2753 -0.0110 0.031 Uiso 1 1 calc R . . C68 C 1.2302(2) 0.3782(2) -0.0560(2) 0.0286(7) Uani 1 1 d . . . H68A H 1.2876 0.3520 -0.0954 0.034 Uiso 1 1 calc R . . C69 C 1.2061(2) 0.4625(2) -0.0484(2) 0.0291(7) Uani 1 1 d . . . H69A H 1.2455 0.4961 -0.0840 0.035 Uiso 1 1 calc R . . C70 C 1.1232(2) 0.4975(2) 0.01230(19) 0.0252(6) Uani 1 1 d . . . H70A H 1.1059 0.5551 0.0188 0.030 Uiso 1 1 calc R . . C71 C 1.0660(2) 0.4477(2) 0.06327(19) 0.0223(6) Uani 1 1 d . . . C72 C 0.9770(2) 0.4773(2) 0.13020(18) 0.0215(6) Uani 1 1 d . B . C73 C 0.9525(2) 0.5526(2) 0.16393(19) 0.0249(6) Uani 1 1 d . . . N21 N 1.0259(2) 0.5607(2) 0.16704(19) 0.0340(8) Uani 0.92(3) 1 d P B 1 C74A C 1.0259(2) 0.5607(2) 0.16704(19) 0.0340(8) Uani 0.08(3) 1 d P B 2 H74B H 1.0884 0.5216 0.1474 0.041 Uiso 0.08(3) 1 calc PR B 2 C75 C 1.0061(3) 0.6271(3) 0.1995(3) 0.0493(11) Uani 1 1 d . . . H75A H 1.0569 0.6339 0.2022 0.059 Uiso 1 1 calc R B 1 C76 C 0.9172(3) 0.6854(3) 0.2288(3) 0.0541(12) Uani 1 1 d . B . H76A H 0.9072 0.7308 0.2513 0.065 Uiso 1 1 calc R . . C77 C 0.8427(3) 0.6769(3) 0.2251(2) 0.0391(9) Uani 1 1 d . . . H77A H 0.7805 0.7166 0.2445 0.047 Uiso 1 1 calc R B 1 Cl1 Cl 0.52054(7) 0.77667(7) 0.21750(6) 0.0466(2) Uani 1 1 d . . . O8 O 0.4743(3) 0.8635(2) 0.1835(2) 0.0667(10) Uani 1 1 d . . . O9 O 0.5961(3) 0.7790(5) 0.2310(3) 0.119(2) Uani 1 1 d . . . O10 O 0.5555(3) 0.7208(3) 0.1663(3) 0.113(2) Uani 1 1 d . . . O11 O 0.4551(2) 0.7508(2) 0.2947(2) 0.0694(11) Uani 1 1 d . . . Cl2 Cl 0.71912(6) 0.82764(6) 0.38225(6) 0.03311(19) Uani 1 1 d D . . O12 O 0.7832(2) 0.8738(2) 0.35026(19) 0.0494(7) Uani 1 1 d D . . O13 O 0.67954(19) 0.84525(18) 0.32323(17) 0.0421(6) Uani 1 1 d D . . O14 O 0.76814(18) 0.73474(16) 0.40328(18) 0.0411(6) Uani 1 1 d D . . O15 O 0.64457(18) 0.85570(18) 0.45641(17) 0.0398(6) Uani 1 1 d D . . O101 O 0.6202(4) 0.7177(4) 0.6034(4) 0.1193(19) Uani 1 1 d . . . H101 H 0.6324 0.7631 0.5722 0.179 Uiso 1 1 calc R . . C101 C 0.7028(5) 0.6470(4) 0.6010(7) 0.143(5) Uani 1 1 d . . . H10E H 0.7413 0.6591 0.6187 0.215 Uiso 1 1 calc R . . H10F H 0.7372 0.6375 0.5451 0.215 Uiso 1 1 calc R . . H10G H 0.6886 0.5942 0.6377 0.215 Uiso 1 1 calc R . . O102 O 0.5134(3) 0.7471(3) 0.8603(3) 0.0902(16) Uani 1 1 d . . . H102 H 0.4926 0.7277 0.9109 0.135 Uiso 1 1 calc R . . C102 C 0.5631(6) 0.6759(4) 0.8194(6) 0.124(4) Uani 1 1 d . . . H10H H 0.6030 0.6264 0.8491 0.187 Uiso 1 1 calc R . . H10I H 0.6024 0.6949 0.7637 0.187 Uiso 1 1 calc R . . H10J H 0.5181 0.6573 0.8172 0.187 Uiso 1 1 calc R . . Cl3 Cl 0.28304(10) 0.59596(10) 0.21193(9) 0.0761(4) Uani 1 1 d D . . O19 O 0.2794(4) 0.6276(4) 0.2733(3) 0.153(3) Uani 1 1 d D . . O18 O 0.3716(3) 0.5467(5) 0.1712(5) 0.201(5) Uani 1 1 d D . . O17 O 0.2411(6) 0.6681(3) 0.1580(4) 0.213(5) Uani 1 1 d D . . O16 O 0.2149(5) 0.5480(6) 0.2509(7) 0.312(7) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01365(17) 0.01659(17) 0.02727(19) -0.00416(14) -0.00701(14) -0.00466(14) Cu2 0.01513(17) 0.01398(17) 0.0278(2) -0.00406(14) -0.00637(14) -0.00423(14) Cu3 0.01397(17) 0.01502(17) 0.0296(2) -0.00423(14) -0.00609(14) -0.00279(14) Cu4 0.01587(18) 0.02097(19) 0.0316(2) -0.00747(15) -0.00917(15) -0.00419(14) Cu5 0.01638(18) 0.02076(18) 0.0266(2) -0.00653(14) -0.00680(14) -0.00592(14) O1 0.0128(10) 0.0226(11) 0.0288(11) -0.0072(9) -0.0056(8) -0.0060(8) O2 0.0141(10) 0.0187(11) 0.0359(12) -0.0054(9) -0.0048(9) -0.0036(8) O3 0.0170(10) 0.0152(10) 0.0290(11) -0.0066(8) -0.0093(9) -0.0016(8) O4 0.0154(10) 0.0164(10) 0.0295(11) -0.0030(8) -0.0093(8) -0.0033(8) O5 0.0194(11) 0.0248(12) 0.0371(13) -0.0110(10) -0.0052(9) -0.0080(9) O6 0.0211(11) 0.0200(11) 0.0344(12) -0.0056(9) -0.0121(9) -0.0070(9) O7 0.0152(10) 0.0204(10) 0.0248(11) -0.0043(8) -0.0032(8) -0.0059(8) N1 0.0190(12) 0.0174(12) 0.0256(13) -0.0028(10) -0.0102(10) -0.0053(10) N2 0.0138(11) 0.0189(12) 0.0228(12) -0.0034(9) -0.0057(9) -0.0055(10) N3 0.0167(12) 0.0147(11) 0.0269(13) -0.0035(9) -0.0078(10) -0.0046(10) N4 0.0188(12) 0.0176(12) 0.0281(14) -0.0035(10) -0.0093(10) -0.0052(10) N5 0.0172(12) 0.0172(12) 0.0306(14) -0.0049(10) -0.0069(10) -0.0047(10) N6 0.0232(13) 0.0202(13) 0.0375(15) -0.0038(11) -0.0151(12) -0.0074(11) N7 0.0155(12) 0.0197(12) 0.0297(14) -0.0089(10) -0.0053(10) -0.0039(10) N8 0.0150(12) 0.0172(12) 0.0245(13) -0.0048(10) -0.0068(10) -0.0029(10) N9 0.0173(12) 0.0197(12) 0.0251(13) -0.0043(10) -0.0076(10) -0.0054(10) N10 0.0159(12) 0.0183(12) 0.0278(13) -0.0062(10) -0.0083(10) -0.0027(10) N11 0.0159(12) 0.0174(12) 0.0255(13) -0.0054(10) -0.0078(10) -0.0040(10) N12 0.0156(13) 0.0337(16) 0.0340(15) -0.0042(12) -0.0075(11) -0.0076(11) N13 0.0187(13) 0.0216(13) 0.0344(15) -0.0100(11) -0.0101(11) -0.0047(10) N14 0.0208(13) 0.0239(13) 0.0289(14) -0.0102(11) -0.0077(11) -0.0072(11) N15 0.0254(16) 0.0333(17) 0.0327(17) -0.0094(13) -0.0106(13) -0.0044(13) C52A 0.0254(16) 0.0333(17) 0.0327(17) -0.0094(13) -0.0106(13) -0.0044(13) N16 0.0203(13) 0.0273(14) 0.0355(15) -0.0091(11) -0.0098(11) -0.0086(11) N17 0.0184(12) 0.0229(13) 0.0280(14) -0.0063(10) -0.0085(10) -0.0068(10) N18 0.0278(16) 0.0426(19) 0.0437(19) -0.0065(15) -0.0163(14) -0.0018(14) N19 0.0188(12) 0.0251(13) 0.0251(13) -0.0047(10) -0.0088(10) -0.0066(11) N20 0.0174(12) 0.0217(13) 0.0218(12) -0.0035(10) -0.0063(10) -0.0060(10) N21A 0.0289(17) 0.0252(16) 0.0284(17) -0.0029(13) -0.0074(13) -0.0124(14) C74 0.0289(17) 0.0252(16) 0.0284(17) -0.0029(13) -0.0074(13) -0.0124(14) C1 0.0185(14) 0.0232(15) 0.0311(17) -0.0022(12) -0.0100(12) -0.0090(12) C2 0.0234(16) 0.0223(15) 0.0379(18) -0.0054(13) -0.0123(14) -0.0102(13) C3 0.0246(16) 0.0282(17) 0.0371(19) -0.0139(14) -0.0085(14) -0.0092(14) C4 0.0184(14) 0.0222(15) 0.0273(16) -0.0069(12) -0.0052(12) -0.0055(12) C5 0.0131(13) 0.0159(13) 0.0283(15) -0.0066(11) -0.0084(11) -0.0016(11) C6 0.0169(14) 0.0146(13) 0.0224(14) -0.0016(10) -0.0080(11) -0.0056(11) C7 0.0165(14) 0.0157(13) 0.0233(15) -0.0024(11) -0.0058(11) -0.0049(11) C8 0.0191(14) 0.0165(14) 0.0316(16) -0.0042(12) -0.0081(12) -0.0062(12) C9 0.0185(15) 0.0186(14) 0.0327(17) -0.0068(12) -0.0078(12) -0.0027(12) C10 0.0171(14) 0.0224(15) 0.0332(17) -0.0040(13) -0.0081(13) -0.0066(12) C11 0.0185(14) 0.0212(15) 0.0289(16) -0.0043(12) -0.0071(12) -0.0081(12) C12 0.0223(15) 0.0237(15) 0.0294(16) -0.0030(12) -0.0097(13) -0.0093(13) C13 0.0248(16) 0.0317(18) 0.0295(17) -0.0041(13) -0.0086(13) -0.0130(14) C14 0.0299(17) 0.0280(17) 0.0302(17) 0.0016(13) -0.0134(14) -0.0171(14) C15 0.0237(16) 0.0193(15) 0.0374(18) 0.0013(13) -0.0156(14) -0.0092(13) C16 0.0215(15) 0.0197(15) 0.0307(16) -0.0025(12) -0.0129(13) -0.0077(12) C17 0.0192(14) 0.0192(14) 0.0313(16) -0.0054(12) -0.0109(12) -0.0055(12) C18 0.0202(15) 0.0164(14) 0.0361(17) -0.0030(12) -0.0127(13) -0.0050(12) C19 0.0288(18) 0.0244(17) 0.070(3) -0.0130(17) -0.0285(18) -0.0034(15) C20 0.036(2) 0.0255(19) 0.092(3) -0.022(2) -0.035(2) -0.0025(16) C21 0.0270(18) 0.0209(17) 0.070(3) -0.0135(17) -0.0246(18) 0.0011(14) C22 0.0223(16) 0.0209(16) 0.049(2) -0.0021(14) -0.0196(15) -0.0046(13) C23 0.0217(15) 0.0220(15) 0.0346(18) -0.0072(13) -0.0068(13) -0.0088(13) C24 0.0283(17) 0.0307(18) 0.043(2) -0.0111(15) -0.0110(15) -0.0153(15) C25 0.0251(17) 0.0326(18) 0.043(2) -0.0109(15) -0.0167(15) -0.0104(14) C26 0.0207(15) 0.0264(16) 0.0335(17) -0.0070(13) -0.0122(13) -0.0061(13) C27 0.0146(13) 0.0194(14) 0.0298(16) -0.0084(12) -0.0068(12) -0.0035(11) C28 0.0150(13) 0.0201(14) 0.0252(15) -0.0068(11) -0.0070(11) -0.0044(11) C29 0.0176(14) 0.0215(15) 0.0229(15) -0.0048(11) -0.0075(11) -0.0059(12) C30 0.0162(14) 0.0240(15) 0.0315(17) -0.0064(12) -0.0068(12) -0.0068(12) C31 0.0168(15) 0.0248(16) 0.0378(18) -0.0079(13) -0.0095(13) -0.0019(13) C32 0.0219(16) 0.0198(15) 0.0380(18) -0.0061(13) -0.0115(14) -0.0023(13) C33 0.0230(15) 0.0193(15) 0.0292(16) -0.0030(12) -0.0085(13) -0.0074(12) C34 0.0215(15) 0.0192(15) 0.0319(17) -0.0049(12) -0.0116(13) -0.0028(12) C35 0.0245(16) 0.0212(15) 0.0390(19) -0.0079(13) -0.0162(14) -0.0027(13) C36 0.0180(15) 0.0268(17) 0.046(2) -0.0128(15) -0.0146(14) -0.0006(13) C37 0.0170(15) 0.0261(17) 0.046(2) -0.0105(14) -0.0126(14) -0.0050(13) C38 0.0192(14) 0.0208(15) 0.0314(16) -0.0074(12) -0.0119(12) -0.0053(12) C39 0.0172(14) 0.0213(15) 0.0262(15) -0.0068(12) -0.0093(12) -0.0050(12) C40 0.0177(14) 0.0270(16) 0.0303(16) -0.0030(13) -0.0115(12) -0.0086(13) C41 0.0234(16) 0.0244(16) 0.0340(18) -0.0019(13) -0.0134(13) -0.0077(13) C42 0.036(2) 0.0305(18) 0.044(2) 0.0038(15) -0.0240(17) -0.0176(16) C43 0.0281(18) 0.041(2) 0.045(2) 0.0079(16) -0.0192(16) -0.0213(16) C44 0.0225(17) 0.046(2) 0.0359(19) -0.0005(16) -0.0099(14) -0.0144(16) C45 0.0229(16) 0.0267(17) 0.0344(18) -0.0087(13) -0.0095(13) -0.0073(13) C46 0.0309(18) 0.0238(17) 0.048(2) -0.0057(15) -0.0168(16) -0.0087(14) C47 0.0300(19) 0.0243(17) 0.061(3) -0.0141(17) -0.0169(18) -0.0028(15) C48 0.0205(16) 0.0261(17) 0.048(2) -0.0144(15) -0.0080(15) -0.0025(13) C49 0.0197(15) 0.0237(16) 0.0350(18) -0.0124(13) -0.0099(13) -0.0036(12) C50 0.0204(15) 0.0288(17) 0.0303(17) -0.0130(13) -0.0082(13) -0.0058(13) C51 0.0193(15) 0.0265(16) 0.0347(18) -0.0147(13) -0.0079(13) -0.0037(13) C52 0.041(2) 0.043(2) 0.0341(19) -0.0184(16) -0.0148(16) 0.0143(17) N15A 0.041(2) 0.043(2) 0.0341(19) -0.0184(16) -0.0148(16) 0.0143(17) C53 0.068(3) 0.029(2) 0.029(2) -0.0110(16) -0.0003(19) 0.001(2) C54 0.035(2) 0.052(3) 0.051(2) -0.030(2) 0.0128(18) -0.027(2) C55 0.0208(17) 0.057(3) 0.058(3) -0.034(2) -0.0163(17) 0.0016(17) C56 0.0296(18) 0.0265(17) 0.046(2) -0.0099(15) -0.0160(16) -0.0091(14) C57 0.036(2) 0.035(2) 0.063(3) -0.0162(18) -0.0230(19) -0.0121(17) C58 0.039(2) 0.041(2) 0.062(3) -0.0132(19) -0.028(2) -0.0142(18) C59 0.0325(19) 0.0354(19) 0.045(2) -0.0099(16) -0.0188(16) -0.0120(16) C60 0.0220(16) 0.0295(17) 0.0328(17) -0.0084(13) -0.0114(13) -0.0089(13) C61 0.0198(15) 0.0264(16) 0.0292(16) -0.0084(13) -0.0083(13) -0.0057(13) C62 0.0244(16) 0.0295(17) 0.0380(19) -0.0056(14) -0.0167(14) -0.0088(14) C63 0.0346(19) 0.037(2) 0.042(2) -0.0033(16) -0.0180(16) -0.0158(16) C64 0.061(3) 0.040(2) 0.050(2) 0.0074(18) -0.037(2) -0.023(2) C65 0.048(3) 0.035(2) 0.071(3) 0.002(2) -0.042(2) -0.0107(19) C66 0.032(2) 0.041(2) 0.071(3) -0.012(2) -0.024(2) 0.0039(18) C67 0.0189(15) 0.0308(17) 0.0278(16) -0.0073(13) -0.0080(12) -0.0072(13) C68 0.0198(15) 0.0384(19) 0.0246(16) -0.0072(14) -0.0057(12) -0.0093(14) C69 0.0236(16) 0.0382(19) 0.0249(16) -0.0012(13) -0.0079(13) -0.0150(14) C70 0.0236(16) 0.0283(16) 0.0249(16) -0.0034(12) -0.0096(13) -0.0105(13) C71 0.0181(14) 0.0258(15) 0.0249(15) -0.0043(12) -0.0091(12) -0.0083(12) C72 0.0184(14) 0.0240(15) 0.0226(15) -0.0051(12) -0.0078(12) -0.0069(12) C73 0.0253(16) 0.0260(16) 0.0251(16) -0.0041(12) -0.0067(12) -0.0132(13) N21 0.0278(16) 0.0442(19) 0.0387(17) -0.0192(14) -0.0049(13) -0.0176(14) C74A 0.0278(16) 0.0442(19) 0.0387(17) -0.0192(14) -0.0049(13) -0.0176(14) C75 0.034(2) 0.068(3) 0.064(3) -0.038(2) -0.0033(19) -0.027(2) C76 0.050(3) 0.063(3) 0.065(3) -0.042(2) 0.004(2) -0.032(2) C77 0.036(2) 0.0317(19) 0.046(2) -0.0173(16) -0.0009(17) -0.0144(16) Cl1 0.0364(5) 0.0380(5) 0.0403(5) -0.0047(4) 0.0033(4) -0.0122(4) O8 0.074(2) 0.0414(18) 0.060(2) 0.0059(15) -0.0083(18) -0.0274(17) O9 0.043(2) 0.206(6) 0.094(3) -0.041(4) -0.016(2) -0.033(3) O10 0.087(3) 0.113(4) 0.130(4) -0.092(3) 0.051(3) -0.061(3) O11 0.0435(18) 0.0429(18) 0.054(2) 0.0068(15) 0.0079(15) 0.0008(14) Cl2 0.0224(4) 0.0331(4) 0.0481(5) -0.0140(4) -0.0073(3) -0.0134(3) O12 0.0369(15) 0.0544(18) 0.0642(19) -0.0109(15) -0.0082(14) -0.0320(14) O13 0.0355(15) 0.0432(16) 0.0546(17) -0.0163(13) -0.0171(13) -0.0128(12) O14 0.0325(14) 0.0301(14) 0.0583(18) -0.0138(12) -0.0140(13) -0.0071(11) O15 0.0298(13) 0.0376(15) 0.0520(16) -0.0202(12) -0.0025(12) -0.0146(12) O101 0.104(4) 0.113(4) 0.124(5) -0.014(4) -0.014(3) -0.059(4) C101 0.090(5) 0.064(4) 0.279(12) 0.071(6) -0.124(7) -0.054(4) O102 0.045(2) 0.053(2) 0.123(4) 0.028(2) -0.019(2) -0.0243(18) C102 0.131(6) 0.048(3) 0.256(11) 0.025(5) -0.163(8) -0.030(4) Cl3 0.0648(8) 0.0672(9) 0.0695(9) -0.0236(7) -0.0303(7) 0.0125(7) O19 0.153(5) 0.157(5) 0.107(4) -0.087(4) -0.096(4) 0.076(4) O18 0.069(3) 0.276(9) 0.330(10) -0.254(9) -0.093(5) 0.057(4) O17 0.284(9) 0.143(6) 0.224(8) -0.131(6) -0.215(8) 0.115(6) O16 0.132(7) 0.429(19) 0.433(19) -0.061(15) -0.122(10) -0.143(10) _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 O7 1.969(2) . ? Cu1 O4 1.969(2) . ? Cu1 N8 1.983(3) . ? Cu1 N9 2.013(3) . ? Cu1 N1 2.426(3) . ? Cu2 N5 1.988(3) . ? Cu2 N2 2.003(2) . ? Cu2 N3 2.007(2) . ? Cu2 N4 2.065(3) . ? Cu2 N7 2.181(3) . ? Cu3 O2 1.918(2) . ? Cu3 N11 1.984(3) . ? Cu3 N10 1.989(2) . ? Cu3 O1 1.994(2) . ? Cu3 O3 2.137(2) . ? Cu4 N17 1.958(3) . ? Cu4 N13 1.970(3) . ? Cu4 N14 2.001(3) . ? Cu4 N16 2.068(3) . ? Cu4 O3 2.169(2) . ? Cu5 O5 1.920(2) . ? Cu5 O6 1.955(2) . ? Cu5 N20 1.980(3) . ? Cu5 N19 1.999(3) . ? Cu5 O4 2.364(2) . ? O1 N2 1.311(3) . ? O2 N5 1.323(3) . ? O3 N8 1.349(3) . ? O4 N11 1.346(3) . ? O5 N14 1.323(3) . ? O6 N17 1.338(3) . ? O7 N20 1.333(3) . ? N1 C1 1.339(4) . ? N1 C5 1.351(4) . ? N2 C6 1.312(4) . ? N3 C11 1.339(4) . ? N3 C7 1.353(4) . ? N4 C12 1.341(4) . ? N4 C16 1.353(4) . ? N5 C17 1.303(4) . ? N6 C18 1.338(4) . ? N6 C22 1.339(4) . ? N7 C23 1.340(4) . ? N7 C27 1.354(4) . ? N8 C28 1.294(4) . ? N9 C33 1.338(4) . ? N9 C29 1.353(4) . ? N10 C34 1.341(4) . ? N10 C38 1.357(4) . ? N11 C39 1.306(4) . ? N12 C44 1.335(4) . ? N12 C40 1.341(4) . ? N13 C45 1.332(4) . ? N13 C49 1.362(4) . ? N14 C50 1.307(4) . ? N15 C51 1.347(5) . ? N15 C55 1.379(5) . ? N16 C56 1.334(4) . ? N16 C60 1.360(4) . ? N17 C61 1.293(4) . ? N18 C66 1.344(5) . ? N18 C62 1.345(5) . ? N19 C67 1.339(4) . ? N19 C71 1.353(4) . ? N20 C72 1.300(4) . ? N21A C77 1.383(5) . ? N21A C73 1.396(5) . ? C1 C2 1.394(5) . ? C2 C3 1.392(5) . ? C3 C4 1.385(4) . ? C4 C5 1.393(4) . ? C5 C6 1.481(4) . ? C6 C7 1.458(4) . ? C7 C8 1.392(4) . ? C8 C9 1.378(4) . ? C9 C10 1.383(4) . ? C10 C11 1.387(4) . ? C12 C13 1.385(4) . ? C13 C14 1.386(5) . ? C14 C15 1.383(5) . ? C15 C16 1.397(4) . ? C16 C17 1.464(4) . ? C17 C18 1.489(4) . ? C18 C19 1.385(5) . ? C19 C20 1.394(5) . ? C20 C21 1.372(5) . ? C21 C22 1.388(5) . ? C23 C24 1.382(5) . ? C24 C25 1.387(5) . ? C25 C26 1.389(5) . ? C26 C27 1.384(4) . ? C27 C28 1.489(4) . ? C28 C29 1.467(4) . ? C29 C30 1.393(4) . ? C30 C31 1.385(4) . ? C31 C32 1.381(5) . ? C32 C33 1.381(4) . ? C34 C35 1.385(4) . ? C35 C36 1.375(5) . ? C36 C37 1.388(5) . ? C37 C38 1.384(4) . ? C38 C39 1.483(4) . ? C39 C40 1.500(4) . ? C40 C41 1.382(5) . ? C41 C42 1.396(5) . ? C42 C43 1.387(6) . ? C43 C44 1.375(6) . ? C45 C46 1.391(5) . ? C46 C47 1.372(5) . ? C47 C48 1.391(5) . ? C48 C49 1.385(5) . ? C49 C50 1.487(5) . ? C50 C51 1.480(4) . ? C51 C52 1.360(5) . ? C52 C53 1.371(6) . ? C53 C54 1.370(7) . ? C54 C55 1.359(6) . ? C56 C57 1.387(5) . ? C57 C58 1.371(6) . ? C58 C59 1.398(5) . ? C59 C60 1.385(5) . ? C60 C61 1.473(5) . ? C61 C62 1.486(5) . ? C62 C63 1.379(5) . ? C63 C64 1.392(6) . ? C64 C65 1.376(7) . ? C65 C66 1.367(7) . ? C67 C68 1.396(5) . ? C68 C69 1.383(5) . ? C69 C70 1.393(5) . ? C70 C71 1.390(4) . ? C71 C72 1.479(4) . ? C72 C73 1.481(4) . ? C73 N21 1.348(4) . ? N21 C75 1.350(5) . ? C75 C76 1.372(6) . ? C76 C77 1.377(6) . ? Cl1 O10 1.374(4) . ? Cl1 O8 1.399(3) . ? Cl1 O11 1.432(3) . ? Cl1 O9 1.438(5) . ? Cl2 O13 1.416(3) . ? Cl2 O12 1.433(2) . ? Cl2 O14 1.434(3) . ? Cl2 O15 1.461(3) . ? O101 C101 1.375(8) . ? O102 C102 1.421(10) . ? Cl3 O18 1.364(4) . ? Cl3 O17 1.409(4) . ? Cl3 O19 1.423(4) . ? Cl3 O16 1.499(5) . ? 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 O7 Cu1 O4 86.68(9) . . ? O7 Cu1 N8 158.67(10) . . ? O4 Cu1 N8 99.47(9) . . ? O7 Cu1 N9 91.53(10) . . ? O4 Cu1 N9 173.94(10) . . ? N8 Cu1 N9 80.20(10) . . ? O7 Cu1 N1 85.58(9) . . ? O4 Cu1 N1 97.35(9) . . ? N8 Cu1 N1 113.55(10) . . ? N9 Cu1 N1 88.28(10) . . ? N5 Cu2 N2 96.84(10) . . ? N5 Cu2 N3 173.46(11) . . ? N2 Cu2 N3 80.35(10) . . ? N5 Cu2 N4 80.29(10) . . ? N2 Cu2 N4 139.34(10) . . ? N3 Cu2 N4 97.95(10) . . ? N5 Cu2 N7 96.21(10) . . ? N2 Cu2 N7 117.60(10) . . ? N3 Cu2 N7 90.33(10) . . ? N4 Cu2 N7 102.99(10) . . ? O2 Cu3 N11 167.41(10) . . ? O2 Cu3 N10 89.48(10) . . ? N11 Cu3 N10 80.52(10) . . ? O2 Cu3 O1 100.49(9) . . ? N11 Cu3 O1 91.97(9) . . ? N10 Cu3 O1 133.89(10) . . ? O2 Cu3 O3 90.24(9) . . ? N11 Cu3 O3 90.40(9) . . ? N10 Cu3 O3 130.12(10) . . ? O1 Cu3 O3 95.06(8) . . ? N17 Cu4 N13 171.80(11) . . ? N17 Cu4 N14 94.31(11) . . ? N13 Cu4 N14 81.05(11) . . ? N17 Cu4 N16 81.24(11) . . ? N13 Cu4 N16 97.54(11) . . ? N14 Cu4 N16 137.21(11) . . ? N17 Cu4 O3 95.22(9) . . ? N13 Cu4 O3 92.97(10) . . ? N14 Cu4 O3 121.72(9) . . ? N16 Cu4 O3 101.07(10) . . ? O5 Cu5 O6 99.84(9) . . ? O5 Cu5 N20 168.38(10) . . ? O6 Cu5 N20 91.47(10) . . ? O5 Cu5 N19 91.98(10) . . ? O6 Cu5 N19 144.96(10) . . ? N20 Cu5 N19 80.06(11) . . ? O5 Cu5 O4 102.22(9) . . ? O6 Cu5 O4 91.34(8) . . ? N20 Cu5 O4 74.66(9) . . ? N19 Cu5 O4 118.34(9) . . ? N2 O1 Cu3 118.73(17) . . ? N5 O2 Cu3 123.44(18) . . ? N8 O3 Cu3 112.49(16) . . ? N8 O3 Cu4 113.19(16) . . ? Cu3 O3 Cu4 109.42(9) . . ? N11 O4 Cu1 125.99(17) . . ? N11 O4 Cu5 118.55(17) . . ? Cu1 O4 Cu5 92.97(8) . . ? N14 O5 Cu5 119.49(18) . . ? N17 O6 Cu5 120.07(17) . . ? N20 O7 Cu1 112.65(17) . . ? C1 N1 C5 117.5(3) . . ? C1 N1 Cu1 116.4(2) . . ? C5 N1 Cu1 126.1(2) . . ? O1 N2 C6 117.7(2) . . ? O1 N2 Cu2 127.04(19) . . ? C6 N2 Cu2 115.02(19) . . ? C11 N3 C7 119.4(3) . . ? C11 N3 Cu2 127.3(2) . . ? C7 N3 Cu2 113.21(19) . . ? C12 N4 C16 118.4(3) . . ? C12 N4 Cu2 129.5(2) . . ? C16 N4 Cu2 111.7(2) . . ? C17 N5 O2 117.4(3) . . ? C17 N5 Cu2 115.7(2) . . ? O2 N5 Cu2 125.85(19) . . ? C18 N6 C22 116.8(3) . . ? C23 N7 C27 117.2(3) . . ? C23 N7 Cu2 119.8(2) . . ? C27 N7 Cu2 121.8(2) . . ? C28 N8 O3 118.1(2) . . ? C28 N8 Cu1 116.6(2) . . ? O3 N8 Cu1 125.01(18) . . ? C33 N9 C29 119.3(3) . . ? C33 N9 Cu1 127.1(2) . . ? C29 N9 Cu1 113.6(2) . . ? C34 N10 C38 119.6(3) . . ? C34 N10 Cu3 125.8(2) . . ? C38 N10 Cu3 114.6(2) . . ? C39 N11 O4 117.7(2) . . ? C39 N11 Cu3 116.4(2) . . ? O4 N11 Cu3 125.91(18) . . ? C44 N12 C40 117.1(3) . . ? C45 N13 C49 120.5(3) . . ? C45 N13 Cu4 126.6(2) . . ? C49 N13 Cu4 112.4(2) . . ? C50 N14 O5 118.8(3) . . ? C50 N14 Cu4 113.6(2) . . ? O5 N14 Cu4 126.0(2) . . ? C51 N15 C55 117.2(3) . . ? C56 N16 C60 118.8(3) . . ? C56 N16 Cu4 130.6(2) . . ? C60 N16 Cu4 110.1(2) . . ? C61 N17 O6 117.8(3) . . ? C61 N17 Cu4 116.8(2) . . ? O6 N17 Cu4 124.99(19) . . ? C66 N18 C62 115.8(4) . . ? C67 N19 C71 119.9(3) . . ? C67 N19 Cu5 125.9(2) . . ? C71 N19 Cu5 113.8(2) . . ? C72 N20 O7 120.5(3) . . ? C72 N20 Cu5 117.7(2) . . ? O7 N20 Cu5 121.02(19) . . ? C77 N21A C73 119.2(3) . . ? N1 C1 C2 123.2(3) . . ? C3 C2 C1 118.8(3) . . ? C4 C3 C2 118.5(3) . . ? C3 C4 C5 119.1(3) . . ? N1 C5 C4 122.9(3) . . ? N1 C5 C6 116.3(3) . . ? C4 C5 C6 120.9(3) . . ? N2 C6 C7 115.1(3) . . ? N2 C6 C5 121.8(3) . . ? C7 C6 C5 122.9(3) . . ? N3 C7 C8 120.9(3) . . ? N3 C7 C6 115.0(3) . . ? C8 C7 C6 123.9(3) . . ? C9 C8 C7 119.1(3) . . ? C8 C9 C10 119.9(3) . . ? C9 C10 C11 118.2(3) . . ? N3 C11 C10 122.3(3) . . ? N4 C12 C13 122.9(3) . . ? C12 C13 C14 118.7(3) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 119.1(3) . . ? N4 C16 C15 121.7(3) . . ? N4 C16 C17 115.5(3) . . ? C15 C16 C17 122.7(3) . . ? N5 C17 C16 115.5(3) . . ? N5 C17 C18 122.7(3) . . ? C16 C17 C18 121.8(3) . . ? N6 C18 C19 123.6(3) . . ? N6 C18 C17 117.9(3) . . ? C19 C18 C17 118.5(3) . . ? C18 C19 C20 118.5(3) . . ? C21 C20 C19 118.7(3) . . ? C20 C21 C22 118.7(3) . . ? N6 C22 C21 123.7(3) . . ? N7 C23 C24 123.3(3) . . ? C23 C24 C25 119.0(3) . . ? C24 C25 C26 118.7(3) . . ? C27 C26 C25 118.6(3) . . ? N7 C27 C26 123.2(3) . . ? N7 C27 C28 117.6(3) . . ? C26 C27 C28 119.2(3) . . ? N8 C28 C29 115.2(3) . . ? N8 C28 C27 123.2(3) . . ? C29 C28 C27 121.5(3) . . ? N9 C29 C30 121.5(3) . . ? N9 C29 C28 114.2(3) . . ? C30 C29 C28 124.3(3) . . ? C31 C30 C29 118.2(3) . . ? C32 C31 C30 120.1(3) . . ? C31 C32 C33 118.5(3) . . ? N9 C33 C32 122.3(3) . . ? N10 C34 C35 121.7(3) . . ? C36 C35 C34 119.1(3) . . ? C35 C36 C37 119.4(3) . . ? C38 C37 C36 119.3(3) . . ? N10 C38 C37 120.8(3) . . ? N10 C38 C39 113.8(3) . . ? C37 C38 C39 125.3(3) . . ? N11 C39 C38 114.1(3) . . ? N11 C39 C40 124.0(3) . . ? C38 C39 C40 121.9(3) . . ? N12 C40 C41 123.5(3) . . ? N12 C40 C39 116.2(3) . . ? C41 C40 C39 120.2(3) . . ? C40 C41 C42 118.4(3) . . ? C43 C42 C41 118.4(3) . . ? C44 C43 C42 118.8(3) . . ? N12 C44 C43 123.8(4) . . ? N13 C45 C46 121.8(3) . . ? C47 C46 C45 118.3(3) . . ? C46 C47 C48 120.2(3) . . ? C49 C48 C47 119.2(3) . . ? N13 C49 C48 119.9(3) . . ? N13 C49 C50 114.6(3) . . ? C48 C49 C50 125.5(3) . . ? N14 C50 C51 122.7(3) . . ? N14 C50 C49 113.7(3) . . ? C51 C50 C49 123.6(3) . . ? N15 C51 C52 123.3(3) . . ? N15 C51 C50 119.4(3) . . ? C52 C51 C50 117.3(3) . . ? C51 C52 C53 117.6(4) . . ? C54 C53 C52 121.4(4) . . ? C55 C54 C53 118.2(4) . . ? C54 C55 N15 122.1(4) . . ? N16 C56 C57 122.1(3) . . ? C58 C57 C56 119.4(4) . . ? C57 C58 C59 119.4(4) . . ? C60 C59 C58 118.2(4) . . ? N16 C60 C59 122.1(3) . . ? N16 C60 C61 115.5(3) . . ? C59 C60 C61 122.4(3) . . ? N17 C61 C60 115.4(3) . . ? N17 C61 C62 123.8(3) . . ? C60 C61 C62 120.7(3) . . ? N18 C62 C63 123.9(3) . . ? N18 C62 C61 113.8(3) . . ? C63 C62 C61 122.3(3) . . ? C62 C63 C64 118.5(4) . . ? C65 C64 C63 118.5(4) . . ? C66 C65 C64 118.9(4) . . ? N18 C66 C65 124.5(4) . . ? N19 C67 C68 121.9(3) . . ? C69 C68 C67 118.7(3) . . ? C68 C69 C70 119.1(3) . . ? C71 C70 C69 119.6(3) . . ? N19 C71 C70 120.8(3) . . ? N19 C71 C72 114.7(3) . . ? C70 C71 C72 124.5(3) . . ? N20 C72 C71 112.8(3) . . ? N20 C72 C73 124.7(3) . . ? C71 C72 C73 122.3(3) . . ? N21 C73 N21A 122.5(3) . . ? N21 C73 C72 114.9(3) . . ? N21A C73 C72 122.6(3) . . ? C73 N21 C75 116.7(3) . . ? N21 C75 C76 124.1(4) . . ? C75 C76 C77 118.8(4) . . ? C76 C77 N21A 118.8(4) . . ? O10 Cl1 O8 111.8(3) . . ? O10 Cl1 O11 111.9(3) . . ? O8 Cl1 O11 107.5(2) . . ? O10 Cl1 O9 110.2(3) . . ? O8 Cl1 O9 106.0(3) . . ? O11 Cl1 O9 109.1(3) . . ? O13 Cl2 O12 109.80(18) . . ? O13 Cl2 O14 109.92(17) . . ? O12 Cl2 O14 109.53(17) . . ? O13 Cl2 O15 109.82(17) . . ? O12 Cl2 O15 109.63(17) . . ? O14 Cl2 O15 108.11(17) . . ? O18 Cl3 O17 111.7(4) . . ? O18 Cl3 O19 113.4(3) . . ? O17 Cl3 O19 108.9(3) . . ? O18 Cl3 O16 113.1(5) . . ? O17 Cl3 O16 101.0(4) . . ? O19 Cl3 O16 108.0(5) . . ? 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 O101 H101 O15 0.84 2.15 2.910(7) 149.7 . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.717 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.098