# Supplementary Material (ESI) for CrystEngcomm # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Sasankasekhar Mohanta' _publ_contact_author_address ; 92 A. P. C. Road Kolkata West Bengal India 700009 ; _publ_contact_author_email 'sm cu chem@yahoo.co.in' loop_ _publ_author_name S.Sasmal S.Majumder S.Hazra H.Sparkes J.Howard M.Nayak ; S.Mohanta ; data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H26 Cu Li N2 O6, 2(C20 H22 Cu N2 O4), Cl O4' _chemical_formula_sum 'C60 H70 Cl Cu3 Li N6 O18' _chemical_formula_weight 1396.23 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' 'Li' 'Li' -0.0003 0.0001 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1205(4) _cell_length_b 15.5520(5) _cell_length_c 17.3547(6) _cell_angle_alpha 85.886(3) _cell_angle_beta 71.153(3) _cell_angle_gamma 78.266(3) _cell_volume 3031.17(17) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7697 _cell_measurement_theta_min 2.4906 _cell_measurement_theta_max 29.0401 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1446 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.90227 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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_measurement_method ? _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25656 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.1221 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10701 _reflns_number_gt 6469 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0192P)^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 10701 _refine_ls_number_parameters 824 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.826 _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 0.36628(4) 0.05735(3) 0.54128(3) 0.01590(12) Uani 1 1 d . . . Cu2 Cu 0.16661(4) 0.32788(3) 0.67674(3) 0.01762(12) Uani 1 1 d . . . Cu3 Cu 0.08786(4) 0.48384(3) 0.90345(3) 0.01604(12) Uani 1 1 d . . . Cl1 Cl 0.03511(8) 0.75381(5) 0.61646(5) 0.0214(2) Uani 1 1 d . . . O1 O 0.5537(2) -0.04816(15) 0.72099(14) 0.0209(6) Uani 1 1 d . . . O2 O 0.44681(18) -0.00225(13) 0.61306(12) 0.0154(6) Uani 1 1 d U . . O3 O 0.41879(19) 0.16120(14) 0.55324(13) 0.0172(6) Uani 1 1 d . . . O4 O 0.5311(2) 0.27571(15) 0.57650(14) 0.0224(6) Uani 1 1 d . . . O5 O 0.4274(2) 0.14501(17) 0.72044(15) 0.0212(6) Uani 1 1 d D . . O6 O 0.1880(2) 0.06176(14) 0.78531(14) 0.0222(6) Uani 1 1 d . . . O7 O 0.1580(2) 0.21362(14) 0.72015(13) 0.0195(6) Uani 1 1 d . . . O8 O 0.26721(19) 0.32787(14) 0.74061(13) 0.0185(6) Uani 1 1 d . . . O9 O 0.39184(19) 0.29755(14) 0.83802(13) 0.0196(6) Uani 1 1 d . . . O10 O 0.1445(2) 0.22890(17) 0.89741(17) 0.0225(6) Uani 1 1 d D . . O11 O -0.1046(2) 0.28235(15) 0.87026(14) 0.0228(6) Uani 1 1 d . . . O12 O 0.00562(19) 0.40531(14) 0.87624(13) 0.0173(6) Uani 1 1 d . . . O13 O 0.13297(19) 0.39845(14) 0.97659(13) 0.0185(6) Uani 1 1 d . . . O14 O 0.17545(19) 0.26112(14) 1.06242(13) 0.0202(6) Uani 1 1 d . . . O15 O 0.1430(2) 0.70041(16) 0.62176(16) 0.0409(8) Uani 1 1 d U . . O16 O -0.0231(3) 0.80352(17) 0.68830(16) 0.0558(9) Uani 1 1 d U . . O17 O 0.0590(2) 0.81197(15) 0.54814(13) 0.0345(7) Uani 1 1 d U . . O18 O -0.0400(2) 0.69722(16) 0.60641(17) 0.0443(8) Uani 1 1 d U . . N1 N 0.3107(2) -0.04654(18) 0.52567(16) 0.0166(7) Uani 1 1 d . . . N2 N 0.2782(2) 0.11345(18) 0.46979(16) 0.0176(7) Uani 1 1 d . . . N3 N 0.0675(2) 0.32441(19) 0.61128(16) 0.0187(7) Uani 1 1 d . . . N4 N 0.1783(2) 0.44448(18) 0.63370(16) 0.0188(7) Uani 1 1 d . . . N5 N 0.0463(2) 0.57437(18) 0.82924(16) 0.0149(7) Uani 1 1 d . . . N6 N 0.1652(2) 0.56845(18) 0.93267(16) 0.0154(7) Uani 1 1 d . . . C1 C 0.6789(3) 0.0046(2) 0.7781(2) 0.0293(10) Uani 1 1 d . . . H1A H 0.7478 0.0005 0.7287 0.044 Uiso 1 1 calc R . . H1B H 0.7057 -0.0001 0.8261 0.044 Uiso 1 1 calc R . . H1C H 0.6254 0.0612 0.7786 0.044 Uiso 1 1 calc R . . C2 C 0.6144(3) -0.0685(2) 0.7794(2) 0.0286(10) Uani 1 1 d . . . H2A H 0.6714 -0.1249 0.7659 0.034 Uiso 1 1 calc R . . H2B H 0.5571 -0.0740 0.8343 0.034 Uiso 1 1 calc R . . C3 C 0.4870(3) -0.1053(2) 0.7110(2) 0.0189(9) Uani 1 1 d . . . C4 C 0.4710(3) -0.1823(2) 0.7541(2) 0.0226(10) Uani 1 1 d . . . H4 H 0.5088 -0.1994 0.7945 0.027 Uiso 1 1 calc R . . C5 C 0.4005(3) -0.2351(2) 0.7393(2) 0.0244(10) Uani 1 1 d . . . H5 H 0.3889 -0.2873 0.7701 0.029 Uiso 1 1 calc R . . C6 C 0.3481(3) -0.2119(2) 0.6805(2) 0.0224(10) Uani 1 1 d . . . H6 H 0.3007 -0.2486 0.6701 0.027 Uiso 1 1 calc R . . C7 C 0.3631(3) -0.1338(2) 0.6348(2) 0.0172(9) Uani 1 1 d . . . C8 C 0.4301(3) -0.0776(2) 0.6504(2) 0.0154(9) Uani 1 1 d . . . C9 C 0.3116(3) -0.1165(2) 0.5691(2) 0.0185(9) Uani 1 1 d . . . H9 H 0.2757 -0.1608 0.5574 0.022 Uiso 1 1 calc R . . C10 C 0.2696(3) -0.0387(2) 0.4552(2) 0.0211(9) Uani 1 1 d . . . H10A H 0.2129 -0.0784 0.4612 0.025 Uiso 1 1 calc RD . . H10B H 0.3376 -0.0550 0.4052 0.025 Uiso 1 1 calc RD . . C11 C 0.2089(3) 0.0567(2) 0.4496(2) 0.0221(9) Uani 1 1 d . . . H11A H 0.2048 0.0699 0.3938 0.027 Uiso 1 1 calc R . . H11B H 0.1270 0.0668 0.4881 0.027 Uiso 1 1 calc R . . C12 C 0.2791(3) 0.1918(2) 0.4405(2) 0.0213(10) Uani 1 1 d . . . H12 H 0.2363 0.2098 0.4031 0.026 Uiso 1 1 calc R . . C13 C 0.3379(3) 0.2540(2) 0.4590(2) 0.0162(9) Uani 1 1 d . . . C14 C 0.3307(3) 0.3378(2) 0.4199(2) 0.0252(10) Uani 1 1 d . . . H14 H 0.2864 0.3505 0.3829 0.030 Uiso 1 1 calc R . . C15 C 0.3854(3) 0.3992(2) 0.4342(2) 0.0256(10) Uani 1 1 d . . . H15 H 0.3774 0.4550 0.4084 0.031 Uiso 1 1 calc R . . C16 C 0.4540(3) 0.3813(2) 0.4870(2) 0.0254(10) Uani 1 1 d . . . H16 H 0.4934 0.4245 0.4963 0.030 Uiso 1 1 calc R . . C17 C 0.4637(3) 0.3009(2) 0.5250(2) 0.0201(9) Uani 1 1 d . . . C18 C 0.4055(3) 0.2354(2) 0.5131(2) 0.0140(9) Uani 1 1 d . . . C19 C 0.6080(3) 0.3310(2) 0.5824(2) 0.0277(10) Uani 1 1 d . . . H19A H 0.5613 0.3866 0.6098 0.033 Uiso 1 1 calc R . . H19B H 0.6588 0.3450 0.5276 0.033 Uiso 1 1 calc R . . C20 C 0.6829(3) 0.2817(2) 0.6313(2) 0.0331(11) Uani 1 1 d . . . H20A H 0.6316 0.2684 0.6855 0.050 Uiso 1 1 calc R . . H20B H 0.7376 0.3178 0.6367 0.050 Uiso 1 1 calc R . . H20C H 0.7285 0.2269 0.6036 0.050 Uiso 1 1 calc R . . C21 C 0.2700(3) -0.0063(2) 0.8853(2) 0.0293(10) Uani 1 1 d . . . H21A H 0.3478 0.0036 0.8499 0.044 Uiso 1 1 calc R . . H21B H 0.2805 -0.0595 0.9180 0.044 Uiso 1 1 calc R . . H21C H 0.2306 0.0442 0.9213 0.044 Uiso 1 1 calc R . . C22 C 0.1943(3) -0.0173(2) 0.8333(2) 0.0230(10) Uani 1 1 d . . . H22A H 0.2313 -0.0693 0.7978 0.028 Uiso 1 1 calc R . . H22B H 0.1140 -0.0246 0.8680 0.028 Uiso 1 1 calc R . . C23 C 0.1192(3) 0.0711(2) 0.7348(2) 0.0180(9) Uani 1 1 d . . . C24 C 0.0674(3) 0.0082(2) 0.7177(2) 0.0215(9) Uani 1 1 d . . . H24 H 0.0787 -0.0489 0.7408 0.026 Uiso 1 1 calc R . . C25 C -0.0024(3) 0.0271(2) 0.6662(2) 0.0259(10) Uani 1 1 d . . . H25 H -0.0388 -0.0168 0.6546 0.031 Uiso 1 1 calc R . . C26 C -0.0183(3) 0.1095(2) 0.6321(2) 0.0254(10) Uani 1 1 d . . . H26 H -0.0665 0.1220 0.5976 0.031 Uiso 1 1 calc R . . C27 C 0.0356(3) 0.1754(2) 0.6475(2) 0.0173(9) Uani 1 1 d . . . C28 C 0.1051(3) 0.1577(2) 0.6999(2) 0.0157(9) Uani 1 1 d . . . C29 C 0.0203(3) 0.2586(2) 0.6058(2) 0.0213(9) Uani 1 1 d . . . H29 H -0.0283 0.2656 0.5716 0.026 Uiso 1 1 calc R . . C30 C 0.0485(3) 0.4042(2) 0.5627(2) 0.0298(10) Uani 1 1 d . . . H30A H -0.0379 0.4268 0.5752 0.036 Uiso 1 1 calc R . . H30B H 0.0817 0.3894 0.5041 0.036 Uiso 1 1 calc R . . C31 C 0.1066(3) 0.4750(2) 0.5802(2) 0.0252(10) Uani 1 1 d . . . H31A H 0.1577 0.4956 0.5281 0.030 Uiso 1 1 calc R . . H31B H 0.0442 0.5256 0.6058 0.030 Uiso 1 1 calc R . . C32 C 0.2446(3) 0.4914(2) 0.6475(2) 0.0193(9) Uani 1 1 d . . . H32 H 0.2469 0.5463 0.6198 0.023 Uiso 1 1 calc R . . C33 C 0.3167(3) 0.4701(2) 0.7007(2) 0.0160(9) Uani 1 1 d . . . C34 C 0.3847(3) 0.5311(2) 0.7075(2) 0.0216(10) Uani 1 1 d . . . H34 H 0.3822 0.5843 0.6772 0.026 Uiso 1 1 calc R . . C35 C 0.4534(3) 0.5149(2) 0.7566(2) 0.0233(9) Uani 1 1 d . . . H35 H 0.4985 0.5570 0.7601 0.028 Uiso 1 1 calc R . . C36 C 0.4594(3) 0.4367(2) 0.8024(2) 0.0185(9) Uani 1 1 d . . . H36 H 0.5078 0.4259 0.8369 0.022 Uiso 1 1 calc R . . C37 C 0.3944(3) 0.3763(2) 0.7966(2) 0.0168(9) Uani 1 1 d . . . C38 C 0.3227(3) 0.3895(2) 0.7447(2) 0.0165(9) Uani 1 1 d . . . C39 C 0.4753(3) 0.2699(2) 0.8811(2) 0.0228(10) Uani 1 1 d . . . H39A H 0.4622 0.3120 0.9247 0.027 Uiso 1 1 calc R . . H39B H 0.5575 0.2659 0.8436 0.027 Uiso 1 1 calc R . . C40 C 0.4554(3) 0.1810(2) 0.9168(2) 0.0286(10) Uani 1 1 d . . . H40A H 0.3742 0.1862 0.9543 0.043 Uiso 1 1 calc R . . H40B H 0.5120 0.1584 0.9464 0.043 Uiso 1 1 calc R . . H40C H 0.4671 0.1404 0.8729 0.043 Uiso 1 1 calc R . . C41 C -0.1228(3) 0.1405(2) 0.9229(2) 0.0340(11) Uani 1 1 d . . . H41A H -0.0361 0.1234 0.9027 0.051 Uiso 1 1 calc R . . H41B H -0.1585 0.0894 0.9227 0.051 Uiso 1 1 calc R . . H41C H -0.1474 0.1626 0.9786 0.051 Uiso 1 1 calc R . . C42 C -0.1632(3) 0.2110(2) 0.8692(2) 0.0271(10) Uani 1 1 d . . . H42A H -0.1413 0.1890 0.8130 0.033 Uiso 1 1 calc R . . H42B H -0.2505 0.2305 0.8900 0.033 Uiso 1 1 calc R . . C43 C -0.1269(3) 0.3565(2) 0.8255(2) 0.0195(9) Uani 1 1 d . . . C44 C -0.2032(3) 0.3692(2) 0.7805(2) 0.0244(10) Uani 1 1 d . . . H44 H -0.2437 0.3238 0.7776 0.029 Uiso 1 1 calc R . . C45 C -0.2222(3) 0.4486(2) 0.7385(2) 0.0224(9) Uani 1 1 d . . . H45 H -0.2749 0.4571 0.7071 0.027 Uiso 1 1 calc R . . C46 C -0.1640(3) 0.5133(2) 0.7435(2) 0.0235(10) Uani 1 1 d . . . H46 H -0.1779 0.5672 0.7156 0.028 Uiso 1 1 calc R . . C47 C -0.0848(3) 0.5031(2) 0.7880(2) 0.0165(9) Uani 1 1 d . . . C48 C -0.0645(3) 0.4228(2) 0.8315(2) 0.0156(9) Uani 1 1 d . . . C49 C -0.0258(3) 0.5738(2) 0.7906(2) 0.0174(9) Uani 1 1 d . . . H49 H -0.0428 0.6252 0.7602 0.021 Uiso 1 1 calc R . . C50 C 0.1047(3) 0.6501(2) 0.8246(2) 0.0186(9) Uani 1 1 d . . . H50A H 0.0538 0.7046 0.8133 0.022 Uiso 1 1 calc R . . H50B H 0.1815 0.6414 0.7802 0.022 Uiso 1 1 calc R . . C51 C 0.1249(3) 0.6574(2) 0.9058(2) 0.0211(9) Uani 1 1 d . . . H51A H 0.1856 0.6937 0.8996 0.025 Uiso 1 1 calc R . . H51B H 0.0502 0.6854 0.9466 0.025 Uiso 1 1 calc R . . C52 C 0.2379(3) 0.5532(2) 0.9734(2) 0.0209(10) Uani 1 1 d . . . H52 H 0.2733 0.6003 0.9798 0.025 Uiso 1 1 calc R . . C53 C 0.2708(3) 0.4694(2) 1.0107(2) 0.0181(9) Uani 1 1 d . . . C54 C 0.3563(3) 0.4628(2) 1.0507(2) 0.0211(9) Uani 1 1 d . . . H54 H 0.3950 0.5108 1.0483 0.025 Uiso 1 1 calc R . . C55 C 0.3846(3) 0.3890(2) 1.0928(2) 0.0240(10) Uani 1 1 d . . . H55 H 0.4445 0.3844 1.1180 0.029 Uiso 1 1 calc R . . C56 C 0.3243(3) 0.3197(2) 1.0986(2) 0.0234(10) Uani 1 1 d . . . H56 H 0.3419 0.2687 1.1294 0.028 Uiso 1 1 calc R . . C57 C 0.2403(3) 0.3243(2) 1.0604(2) 0.0161(9) Uani 1 1 d . . . C58 C 0.2126(3) 0.3997(2) 1.0126(2) 0.0150(9) Uani 1 1 d . . . C59 C 0.1894(3) 0.1850(2) 1.1126(2) 0.0246(10) Uani 1 1 d . . . H59A H 0.1703 0.2025 1.1698 0.030 Uiso 1 1 calc R . . H59B H 0.2724 0.1523 1.0938 0.030 Uiso 1 1 calc R . . C60 C 0.1063(3) 0.1286(2) 1.1060(2) 0.0261(10) Uani 1 1 d . . . H60A H 0.0243 0.1607 1.1268 0.039 Uiso 1 1 calc R . . H60B H 0.1160 0.0748 1.1382 0.039 Uiso 1 1 calc R . . H60C H 0.1243 0.1133 1.0489 0.039 Uiso 1 1 calc R . . Li1 Li 0.2666(6) 0.2053(4) 0.7875(4) 0.0280(17) Uani 1 1 d D . . H10C H 0.160(3) 0.259(2) 0.9272(19) 0.038(14) Uiso 1 1 d D . . H5A H 0.451(2) 0.1739(16) 0.6790(13) 0.019(11) Uiso 1 1 d D . . H10D H 0.084(2) 0.257(2) 0.888(2) 0.045(15) Uiso 1 1 d D . . H5B H 0.423(3) 0.0994(16) 0.700(2) 0.070(17) Uiso 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 0.0173(3) 0.0131(2) 0.0195(3) 0.0014(2) -0.0072(2) -0.0060(2) Cu2 0.0198(3) 0.0156(2) 0.0195(3) 0.0034(2) -0.0082(2) -0.0059(2) Cu3 0.0162(2) 0.0156(3) 0.0185(3) 0.0023(2) -0.0066(2) -0.0068(2) Cl1 0.0259(5) 0.0165(5) 0.0226(5) 0.0027(4) -0.0091(4) -0.0047(4) O1 0.0242(14) 0.0214(14) 0.0242(14) 0.0080(12) -0.0168(12) -0.0080(12) O2 0.0184(12) 0.0095(12) 0.0213(13) 0.0084(10) -0.0079(10) -0.0095(10) O3 0.0253(14) 0.0122(13) 0.0190(13) 0.0033(11) -0.0126(11) -0.0064(11) O4 0.0263(15) 0.0160(14) 0.0289(15) -0.0032(12) -0.0090(13) -0.0115(12) O5 0.0302(16) 0.0127(14) 0.0226(16) 0.0012(13) -0.0081(13) -0.0095(12) O6 0.0292(15) 0.0162(14) 0.0231(14) 0.0073(12) -0.0103(12) -0.0079(12) O7 0.0260(14) 0.0151(13) 0.0233(14) 0.0058(11) -0.0137(12) -0.0095(12) O8 0.0206(14) 0.0161(13) 0.0240(14) 0.0060(11) -0.0122(11) -0.0086(12) O9 0.0216(14) 0.0178(14) 0.0221(14) 0.0046(11) -0.0102(12) -0.0061(11) O10 0.0294(17) 0.0206(16) 0.0219(16) -0.0011(13) -0.0130(13) -0.0066(14) O11 0.0263(15) 0.0189(14) 0.0289(15) 0.0028(12) -0.0115(12) -0.0134(12) O12 0.0196(14) 0.0155(14) 0.0223(14) 0.0067(11) -0.0117(12) -0.0093(11) O13 0.0194(14) 0.0223(14) 0.0204(14) 0.0016(11) -0.0125(12) -0.0090(11) O14 0.0257(14) 0.0160(13) 0.0222(14) 0.0090(11) -0.0130(12) -0.0057(12) O15 0.0311(14) 0.0329(15) 0.0628(17) 0.0082(13) -0.0255(13) -0.0010(12) O16 0.0780(19) 0.0384(16) 0.0320(15) -0.0064(13) 0.0038(14) -0.0011(15) O17 0.0460(15) 0.0336(14) 0.0252(14) 0.0121(12) -0.0118(12) -0.0139(12) O18 0.0415(15) 0.0351(15) 0.0704(18) 0.0144(14) -0.0327(14) -0.0189(13) N1 0.0173(16) 0.0152(17) 0.0177(17) -0.0006(14) -0.0048(14) -0.0047(14) N2 0.0159(17) 0.0169(17) 0.0157(16) 0.0006(14) -0.0008(14) -0.0005(14) N3 0.0202(17) 0.0213(18) 0.0167(16) 0.0016(14) -0.0090(14) -0.0038(15) N4 0.0205(17) 0.0162(17) 0.0163(17) 0.0024(14) -0.0038(14) -0.0005(15) N5 0.0136(16) 0.0164(17) 0.0149(16) -0.0006(14) -0.0045(14) -0.0028(14) N6 0.0155(16) 0.0157(17) 0.0163(17) 0.0007(14) -0.0049(14) -0.0062(14) C1 0.026(2) 0.041(3) 0.027(2) -0.002(2) -0.0155(19) -0.008(2) C2 0.024(2) 0.036(3) 0.030(2) 0.006(2) -0.0154(19) -0.008(2) C3 0.015(2) 0.017(2) 0.021(2) 0.0001(18) -0.0043(17) 0.0014(17) C4 0.023(2) 0.020(2) 0.023(2) 0.0080(18) -0.0071(18) -0.0026(18) C5 0.027(2) 0.014(2) 0.028(2) 0.0058(18) -0.0031(19) -0.0044(18) C6 0.024(2) 0.010(2) 0.029(2) -0.0011(18) -0.0024(19) -0.0053(17) C7 0.016(2) 0.012(2) 0.019(2) -0.0030(17) -0.0002(17) -0.0027(17) C8 0.0107(19) 0.015(2) 0.015(2) 0.0007(17) 0.0000(16) 0.0029(16) C9 0.015(2) 0.019(2) 0.021(2) -0.0093(18) -0.0016(17) -0.0067(17) C10 0.022(2) 0.026(2) 0.020(2) -0.0018(18) -0.0064(17) -0.0148(18) C11 0.017(2) 0.034(2) 0.019(2) 0.0014(18) -0.0103(17) -0.0072(18) C12 0.018(2) 0.032(2) 0.0096(19) 0.0014(18) -0.0046(16) 0.0062(19) C13 0.0127(19) 0.014(2) 0.017(2) 0.0016(17) 0.0006(17) 0.0002(16) C14 0.026(2) 0.025(2) 0.021(2) 0.0063(18) -0.0047(18) -0.0012(19) C15 0.026(2) 0.011(2) 0.027(2) 0.0050(18) 0.0042(19) 0.0033(18) C16 0.023(2) 0.012(2) 0.031(2) -0.0028(18) 0.005(2) -0.0034(18) C17 0.016(2) 0.016(2) 0.022(2) -0.0030(18) 0.0018(18) -0.0026(17) C18 0.015(2) 0.011(2) 0.0126(19) 0.0002(16) -0.0006(16) 0.0004(16) C19 0.029(2) 0.019(2) 0.034(2) -0.0098(19) 0.000(2) -0.0135(19) C20 0.030(2) 0.029(2) 0.042(3) -0.012(2) -0.014(2) -0.004(2) C21 0.039(2) 0.025(2) 0.023(2) 0.0046(18) -0.013(2) -0.003(2) C22 0.027(2) 0.017(2) 0.021(2) 0.0080(17) -0.0026(18) -0.0051(18) C23 0.016(2) 0.025(2) 0.011(2) -0.0001(17) -0.0013(17) -0.0059(18) C24 0.020(2) 0.016(2) 0.025(2) 0.0020(18) -0.0017(18) -0.0062(18) C25 0.021(2) 0.028(2) 0.028(2) -0.0077(19) 0.0013(19) -0.0131(19) C26 0.020(2) 0.041(3) 0.019(2) -0.005(2) -0.0067(18) -0.0098(19) C27 0.015(2) 0.020(2) 0.015(2) -0.0013(17) -0.0016(17) -0.0042(17) C28 0.014(2) 0.018(2) 0.012(2) -0.0014(17) 0.0020(17) -0.0068(17) C29 0.012(2) 0.037(2) 0.017(2) -0.0082(19) -0.0064(17) -0.0034(19) C30 0.034(2) 0.031(2) 0.029(2) 0.004(2) -0.018(2) -0.004(2) C31 0.028(2) 0.023(2) 0.022(2) 0.0007(18) -0.0089(19) 0.0029(19) C32 0.025(2) 0.010(2) 0.018(2) 0.0031(17) -0.0004(18) -0.0033(18) C33 0.0127(19) 0.014(2) 0.017(2) -0.0010(17) -0.0007(17) 0.0018(16) C34 0.021(2) 0.013(2) 0.027(2) 0.0031(18) -0.0008(19) -0.0065(17) C35 0.022(2) 0.017(2) 0.030(2) -0.0057(18) -0.0033(19) -0.0080(17) C36 0.017(2) 0.020(2) 0.019(2) -0.0042(17) -0.0048(17) -0.0046(17) C37 0.015(2) 0.014(2) 0.017(2) -0.0006(17) -0.0017(17) 0.0005(17) C38 0.015(2) 0.017(2) 0.016(2) -0.0049(17) -0.0027(17) -0.0011(17) C39 0.021(2) 0.030(2) 0.020(2) 0.0017(18) -0.0110(18) -0.0035(18) C40 0.032(2) 0.028(2) 0.028(2) 0.0015(19) -0.0159(19) 0.001(2) C41 0.044(3) 0.021(2) 0.038(2) 0.000(2) -0.007(2) -0.020(2) C42 0.026(2) 0.024(2) 0.033(2) -0.0057(19) -0.0053(19) -0.0133(19) C43 0.019(2) 0.023(2) 0.017(2) -0.0029(18) -0.0040(17) -0.0069(17) C44 0.017(2) 0.030(2) 0.025(2) -0.0078(19) -0.0024(18) -0.0083(18) C45 0.020(2) 0.034(2) 0.017(2) -0.0034(18) -0.0123(17) -0.0032(19) C46 0.021(2) 0.029(2) 0.021(2) 0.0010(18) -0.0088(18) -0.0020(19) C47 0.0117(19) 0.023(2) 0.0130(19) -0.0032(17) -0.0023(16) -0.0008(17) C48 0.0117(19) 0.019(2) 0.013(2) 0.0005(17) -0.0017(17) -0.0002(16) C49 0.015(2) 0.020(2) 0.014(2) 0.0033(17) -0.0034(17) 0.0032(17) C50 0.0136(19) 0.012(2) 0.027(2) 0.0030(17) -0.0022(17) -0.0037(16) C51 0.017(2) 0.020(2) 0.023(2) -0.0005(18) -0.0018(17) -0.0048(17) C52 0.015(2) 0.022(2) 0.022(2) -0.0059(18) 0.0037(18) -0.0091(18) C53 0.014(2) 0.020(2) 0.018(2) -0.0021(17) -0.0047(17) -0.0003(17) C54 0.017(2) 0.028(2) 0.021(2) -0.0035(18) -0.0054(17) -0.0103(18) C55 0.015(2) 0.039(3) 0.023(2) 0.0005(19) -0.0121(17) -0.0063(19) C56 0.022(2) 0.025(2) 0.020(2) 0.0050(18) -0.0067(18) 0.0010(18) C57 0.016(2) 0.018(2) 0.015(2) -0.0001(17) -0.0066(17) -0.0023(17) C58 0.0119(19) 0.020(2) 0.0095(19) 0.0011(16) -0.0001(16) -0.0015(17) C59 0.027(2) 0.021(2) 0.020(2) 0.0083(18) -0.0058(18) 0.0010(18) C60 0.033(2) 0.015(2) 0.023(2) 0.0053(17) -0.0007(19) -0.0040(18) Li1 0.031(4) 0.022(4) 0.035(4) -0.001(3) -0.014(3) -0.007(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 O3 1.900(2) . ? Cu1 O2 1.901(2) . ? Cu1 N1 1.939(3) . ? Cu1 N2 1.940(3) . ? Cu2 O7 1.889(2) . ? Cu2 O8 1.894(2) . ? Cu2 N3 1.911(3) . ? Cu2 N4 1.926(3) . ? Cu2 Li1 2.972(6) . ? Cu3 O13 1.893(2) . ? Cu3 O12 1.895(2) . ? Cu3 N5 1.940(3) . ? Cu3 N6 1.942(3) . ? Cl1 O16 1.414(3) . ? Cl1 O15 1.426(2) . ? Cl1 O17 1.428(2) . ? Cl1 O18 1.444(3) . ? O1 C3 1.370(4) . ? O1 C2 1.418(4) . ? O2 C8 1.319(4) . ? O3 C18 1.314(4) . ? O4 C17 1.382(4) . ? O4 C19 1.421(4) . ? O5 Li1 1.996(6) . ? O5 H5A 0.820(17) . ? O5 H5B 0.835(18) . ? O6 C23 1.375(4) . ? O6 C22 1.438(4) . ? O6 Li1 2.607(7) . ? O7 C28 1.306(4) . ? O7 Li1 2.004(8) . ? O8 C38 1.296(4) . ? O8 Li1 2.018(6) . ? O9 C37 1.376(4) . ? O9 C39 1.425(4) . ? O9 Li1 2.656(8) . ? O10 Li1 2.004(6) . ? O10 H10C 0.814(18) . ? O10 H10D 0.833(18) . ? O11 C43 1.373(4) . ? O11 C42 1.439(4) . ? O12 C48 1.305(4) . ? O13 C58 1.312(4) . ? O14 C57 1.370(4) . ? O14 C59 1.433(3) . ? N1 C9 1.279(4) . ? N1 C10 1.451(4) . ? N2 C12 1.287(4) . ? N2 C11 1.464(4) . ? N3 C29 1.292(4) . ? N3 C30 1.471(4) . ? N4 C32 1.275(5) . ? N4 C31 1.460(4) . ? N5 C49 1.263(4) . ? N5 C50 1.477(4) . ? N6 C52 1.274(4) . ? N6 C51 1.465(4) . ? C1 C2 1.501(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.379(4) . ? C3 C8 1.432(5) . ? C4 C5 1.389(5) . ? C4 H4 0.9500 . ? C5 C6 1.359(5) . ? C5 H5 0.9500 . ? C6 C7 1.414(4) . ? C6 H6 0.9500 . ? C7 C8 1.400(5) . ? C7 C9 1.452(5) . ? C9 H9 0.9500 . ? C10 C11 1.527(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.421(5) . ? C12 H12 0.9500 . ? C13 C18 1.413(5) . ? C13 C14 1.425(4) . ? C14 C15 1.345(5) . ? C14 H14 0.9500 . ? C15 C16 1.404(5) . ? C15 H15 0.9500 . ? C16 C17 1.373(4) . ? C16 H16 0.9500 . ? C17 C18 1.412(5) . ? C19 C20 1.500(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.518(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.362(5) . ? C23 C28 1.438(5) . ? C24 C25 1.396(5) . ? C24 H24 0.9500 . ? C25 C26 1.374(5) . ? C25 H25 0.9500 . ? C26 C27 1.405(5) . ? C26 H26 0.9500 . ? C27 C28 1.406(5) . ? C27 C29 1.445(4) . ? C29 H29 0.9500 . ? C30 C31 1.519(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.443(5) . ? C32 H32 0.9500 . ? C33 C34 1.411(5) . ? C33 C38 1.422(4) . ? C34 C35 1.350(5) . ? C34 H34 0.9500 . ? C35 C36 1.407(4) . ? C35 H35 0.9500 . ? C36 C37 1.372(5) . ? C36 H36 0.9500 . ? C37 C38 1.419(5) . ? C39 C40 1.508(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.497(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.369(5) . ? C43 C48 1.424(5) . ? C44 C45 1.404(4) . ? C44 H44 0.9500 . ? C45 C46 1.363(5) . ? C45 H45 0.9500 . ? C46 C47 1.394(5) . ? C46 H46 0.9500 . ? C47 C48 1.431(4) . ? C47 C49 1.439(5) . ? C49 H49 0.9500 . ? C50 C51 1.522(5) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.453(4) . ? C52 H52 0.9500 . ? C53 C58 1.402(5) . ? C53 C54 1.407(5) . ? C54 C55 1.361(4) . ? C54 H54 0.9500 . ? C55 C56 1.401(5) . ? C55 H55 0.9500 . ? C56 C57 1.371(5) . ? C56 H56 0.9500 . ? C57 C58 1.434(4) . ? C59 C60 1.498(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 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 O3 Cu1 O2 89.44(10) . . ? O3 Cu1 N1 177.82(11) . . ? O2 Cu1 N1 92.70(11) . . ? O3 Cu1 N2 93.47(11) . . ? O2 Cu1 N2 176.79(11) . . ? N1 Cu1 N2 84.40(12) . . ? O7 Cu2 O8 83.81(10) . . ? O7 Cu2 N3 94.96(12) . . ? O8 Cu2 N3 178.29(11) . . ? O7 Cu2 N4 178.60(13) . . ? O8 Cu2 N4 94.80(12) . . ? N3 Cu2 N4 86.43(13) . . ? O7 Cu2 Li1 41.69(16) . . ? O8 Cu2 Li1 42.14(15) . . ? N3 Cu2 Li1 136.59(16) . . ? N4 Cu2 Li1 136.92(17) . . ? O13 Cu3 O12 89.16(10) . . ? O13 Cu3 N5 177.48(12) . . ? O12 Cu3 N5 93.33(11) . . ? O13 Cu3 N6 92.37(11) . . ? O12 Cu3 N6 177.29(10) . . ? N5 Cu3 N6 85.16(12) . . ? O16 Cl1 O15 109.98(18) . . ? O16 Cl1 O17 109.26(15) . . ? O15 Cl1 O17 110.30(15) . . ? O16 Cl1 O18 109.67(18) . . ? O15 Cl1 O18 108.48(15) . . ? O17 Cl1 O18 109.13(16) . . ? C3 O1 C2 118.8(3) . . ? C8 O2 Cu1 126.1(2) . . ? C18 O3 Cu1 126.8(2) . . ? C17 O4 C19 118.4(3) . . ? Li1 O5 H5A 109.4(18) . . ? Li1 O5 H5B 111(2) . . ? H5A O5 H5B 100(3) . . ? C23 O6 C22 117.8(3) . . ? C23 O6 Li1 110.8(3) . . ? C22 O6 Li1 131.0(3) . . ? C28 O7 Cu2 126.0(2) . . ? C28 O7 Li1 134.0(3) . . ? Cu2 O7 Li1 99.5(2) . . ? C38 O8 Cu2 127.1(2) . . ? C38 O8 Li1 133.9(3) . . ? Cu2 O8 Li1 98.8(2) . . ? C37 O9 C39 118.1(3) . . ? C37 O9 Li1 109.5(3) . . ? C39 O9 Li1 130.1(2) . . ? Li1 O10 H10C 115(3) . . ? Li1 O10 H10D 105(3) . . ? H10C O10 H10D 107(3) . . ? C43 O11 C42 118.4(3) . . ? C48 O12 Cu3 126.7(2) . . ? C58 O13 Cu3 126.7(2) . . ? C57 O14 C59 118.4(3) . . ? C9 N1 C10 121.6(3) . . ? C9 N1 Cu1 126.1(3) . . ? C10 N1 Cu1 112.3(2) . . ? C12 N2 C11 121.3(3) . . ? C12 N2 Cu1 125.5(3) . . ? C11 N2 Cu1 113.2(2) . . ? C29 N3 C30 119.5(3) . . ? C29 N3 Cu2 125.6(2) . . ? C30 N3 Cu2 114.9(2) . . ? C32 N4 C31 121.6(3) . . ? C32 N4 Cu2 124.4(3) . . ? C31 N4 Cu2 114.1(3) . . ? C49 N5 C50 121.5(3) . . ? C49 N5 Cu3 126.1(3) . . ? C50 N5 Cu3 112.3(2) . . ? C52 N6 C51 121.7(3) . . ? C52 N6 Cu3 126.7(3) . . ? C51 N6 Cu3 111.5(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 107.7(3) . . ? O1 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O1 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O1 C3 C4 125.8(4) . . ? O1 C3 C8 113.6(3) . . ? C4 C3 C8 120.6(4) . . ? C3 C4 C5 120.9(4) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.7(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 120.6(4) . . ? C8 C7 C9 121.7(3) . . ? C6 C7 C9 117.6(4) . . ? O2 C8 C7 125.5(3) . . ? O2 C8 C3 117.4(3) . . ? C7 C8 C3 117.1(3) . . ? N1 C9 C7 125.3(4) . . ? N1 C9 H9 117.4 . . ? C7 C9 H9 117.4 . . ? N1 C10 C11 107.7(3) . . ? N1 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? N1 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? N2 C11 C10 108.2(3) . . ? N2 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? N2 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N2 C12 C13 126.2(4) . . ? N2 C12 H12 116.9 . . ? C13 C12 H12 116.9 . . ? C18 C13 C12 122.7(3) . . ? C18 C13 C14 118.7(4) . . ? C12 C13 C14 118.6(4) . . ? C15 C14 C13 121.5(4) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 120.5(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 119.5(4) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 O4 124.2(4) . . ? C16 C17 C18 121.8(4) . . ? O4 C17 C18 114.0(3) . . ? O3 C18 C17 117.1(3) . . ? O3 C18 C13 124.8(3) . . ? C17 C18 C13 118.1(3) . . ? O4 C19 C20 106.9(3) . . ? O4 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O4 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 C21 105.4(3) . . ? O6 C22 H22A 110.7 . . ? C21 C22 H22A 110.7 . . ? O6 C22 H22B 110.7 . . ? C21 C22 H22B 110.7 . . ? H22A C22 H22B 108.8 . . ? C24 C23 O6 126.2(3) . . ? C24 C23 C28 121.3(4) . . ? O6 C23 C28 112.5(3) . . ? C23 C24 C25 120.2(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.0(4) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 121.2(4) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C28 119.6(3) . . ? C26 C27 C29 117.9(4) . . ? C28 C27 C29 122.4(4) . . ? O7 C28 C27 125.6(3) . . ? O7 C28 C23 116.8(3) . . ? C27 C28 C23 117.7(4) . . ? N3 C29 C27 125.2(4) . . ? N3 C29 H29 117.4 . . ? C27 C29 H29 117.4 . . ? N3 C30 C31 111.5(3) . . ? N3 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? N3 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? N4 C31 C30 112.8(3) . . ? N4 C31 H31A 109.0 . . ? C30 C31 H31A 109.0 . . ? N4 C31 H31B 109.0 . . ? C30 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? N4 C32 C33 127.0(3) . . ? N4 C32 H32 116.5 . . ? C33 C32 H32 116.5 . . ? C34 C33 C38 119.4(4) . . ? C34 C33 C32 118.4(3) . . ? C38 C33 C32 122.2(4) . . ? C35 C34 C33 121.1(3) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 121.0(4) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C37 C36 C35 119.0(4) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 O9 125.0(3) . . ? C36 C37 C38 122.1(3) . . ? O9 C37 C38 112.9(3) . . ? O8 C38 C37 118.2(3) . . ? O8 C38 C33 124.4(4) . . ? C37 C38 C33 117.4(4) . . ? O9 C39 C40 106.3(3) . . ? O9 C39 H39A 110.5 . . ? C40 C39 H39A 110.5 . . ? O9 C39 H39B 110.5 . . ? C40 C39 H39B 110.5 . . ? H39A C39 H39B 108.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O11 C42 C41 106.4(3) . . ? O11 C42 H42A 110.4 . . ? C41 C42 H42A 110.4 . . ? O11 C42 H42B 110.4 . . ? C41 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C44 C43 O11 125.1(4) . . ? C44 C43 C48 121.5(3) . . ? O11 C43 C48 113.4(3) . . ? C43 C44 C45 120.6(4) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 119.1(4) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C45 C46 C47 122.3(3) . . ? C45 C46 H46 118.9 . . ? C47 C46 H46 118.9 . . ? C46 C47 C48 119.5(4) . . ? C46 C47 C49 119.7(3) . . ? C48 C47 C49 120.8(3) . . ? O12 C48 C43 117.3(3) . . ? O12 C48 C47 125.7(4) . . ? C43 C48 C47 117.0(3) . . ? N5 C49 C47 126.6(3) . . ? N5 C49 H49 116.7 . . ? C47 C49 H49 116.7 . . ? N5 C50 C51 108.2(3) . . ? N5 C50 H50A 110.1 . . ? C51 C50 H50A 110.1 . . ? N5 C50 H50B 110.1 . . ? C51 C50 H50B 110.1 . . ? H50A C50 H50B 108.4 . . ? N6 C51 C50 107.9(3) . . ? N6 C51 H51A 110.1 . . ? C50 C51 H51A 110.1 . . ? N6 C51 H51B 110.1 . . ? C50 C51 H51B 110.1 . . ? H51A C51 H51B 108.4 . . ? N6 C52 C53 125.1(4) . . ? N6 C52 H52 117.5 . . ? C53 C52 H52 117.5 . . ? C58 C53 C54 120.9(3) . . ? C58 C53 C52 121.2(3) . . ? C54 C53 C52 117.7(4) . . ? C55 C54 C53 121.2(4) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C56 119.2(4) . . ? C54 C55 H55 120.4 . . ? C56 C55 H55 120.4 . . ? C57 C56 C55 120.9(3) . . ? C57 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? O14 C57 C56 125.9(3) . . ? O14 C57 C58 113.0(3) . . ? C56 C57 C58 121.1(4) . . ? O13 C58 C53 125.9(3) . . ? O13 C58 C57 117.4(3) . . ? C53 C58 C57 116.7(3) . . ? O14 C59 C60 107.6(3) . . ? O14 C59 H59A 110.2 . . ? C60 C59 H59A 110.2 . . ? O14 C59 H59B 110.2 . . ? C60 C59 H59B 110.2 . . ? H59A C59 H59B 108.5 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O5 Li1 O7 107.4(3) . . ? O5 Li1 O10 148.8(4) . . ? O7 Li1 O10 99.1(3) . . ? O5 Li1 O8 99.9(3) . . ? O7 Li1 O8 77.8(2) . . ? O10 Li1 O8 101.5(3) . . ? O5 Li1 O6 88.9(2) . . ? O7 Li1 O6 65.8(2) . . ? O10 Li1 O6 87.3(2) . . ? O8 Li1 O6 143.5(4) . . ? O5 Li1 O9 82.7(2) . . ? O7 Li1 O9 142.8(3) . . ? O10 Li1 O9 86.0(3) . . ? O8 Li1 O9 65.1(2) . . ? O6 Li1 O9 151.4(3) . . ? O5 Li1 Cu2 106.8(2) . . ? O7 Li1 Cu2 38.81(13) . . ? O10 Li1 Cu2 104.2(2) . . ? O8 Li1 Cu2 39.03(14) . . ? O6 Li1 Cu2 104.5(2) . . ? O9 Li1 Cu2 104.1(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 O5 H5B O1 0.835(18) 2.58(3) 3.083(3) 120(3) . O5 H5B O2 0.835(18) 2.18(2) 2.980(3) 162(3) . O5 H5A O3 0.820(17) 2.36(3) 2.928(3) 127(3) . O5 H5A O4 0.820(17) 2.392(18) 3.199(3) 168(3) . O10 H10D O11 0.833(18) 2.35(2) 3.142(4) 158(4) . O10 H10D O12 0.833(18) 2.33(3) 2.979(3) 135(3) . O10 H10C O13 0.814(18) 2.31(3) 3.018(4) 147(3) . O10 H10C O14 0.814(18) 2.42(3) 3.093(4) 141(3) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.506 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.073 #==== end data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H26 Cu N2 Na O6, 2(C20 H22 Cu N2 O4), C2 N3' _chemical_formula_sum 'C62 H70 Cu3 N9 Na O14' _chemical_formula_weight 1378.88 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' 'Na' 'Na' 0.0362 0.0249 '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 12.0391(3) _cell_length_b 16.6189(3) _cell_length_c 16.6213(3) _cell_angle_alpha 86.908(2) _cell_angle_beta 69.870(2) _cell_angle_gamma 82.251(2) _cell_volume 3093.78(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 19396 _cell_measurement_theta_min 2.5673 _cell_measurement_theta_max 32.6070 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1430 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.54756 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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_measurement_method ? _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59302 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 32.70 _reflns_number_total 20591 _reflns_number_gt 12631 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0338P)^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 20591 _refine_ls_number_parameters 827 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 0.853 _refine_ls_restrained_S_all 0.854 _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 0.86698(2) 0.495824(13) 0.077918(13) 0.01542(5) Uani 1 1 d . . . Cu2 Cu 0.69457(2) 0.841575(13) 0.144220(13) 0.01616(5) Uani 1 1 d . . . Cu3 Cu 0.58785(2) 0.984086(13) 0.397811(13) 0.01542(5) Uani 1 1 d . . . Na1 Na 0.76980(7) 0.71983(4) 0.28620(4) 0.01987(16) Uani 1 1 d D . . O1 O 1.04259(12) 0.46954(8) 0.27613(8) 0.0235(3) Uani 1 1 d . . . O2 O 0.92672(11) 0.47524(7) 0.17066(7) 0.0175(3) Uani 1 1 d . . . O3 O 0.93006(12) 0.59723(7) 0.05507(8) 0.0215(3) Uani 1 1 d . . . O4 O 1.00995(12) 0.73256(7) 0.06147(8) 0.0220(3) Uani 1 1 d . . . O5 O 0.94672(13) 0.63621(9) 0.22141(9) 0.0235(3) Uani 1 1 d D . . O6 O 0.65419(12) 0.59878(7) 0.27170(8) 0.0202(3) Uani 1 1 d . . . O7 O 0.66633(11) 0.73713(7) 0.19128(7) 0.0179(3) Uani 1 1 d . . . O8 O 0.78314(11) 0.84807(7) 0.21816(7) 0.0182(3) Uani 1 1 d . . . O9 O 0.89392(12) 0.82738(8) 0.32704(8) 0.0201(3) Uani 1 1 d . . . O10 O 0.61439(14) 0.74979(8) 0.41304(9) 0.0227(3) Uani 1 1 d D . . O11 O 0.39425(12) 0.78683(8) 0.36075(8) 0.0226(3) Uani 1 1 d . . . O12 O 0.50482(11) 0.90664(7) 0.36937(8) 0.0189(3) Uani 1 1 d . . . O13 O 0.62510(11) 0.90956(7) 0.47942(8) 0.0186(3) Uani 1 1 d . . . O14 O 0.66510(12) 0.78548(7) 0.57045(8) 0.0202(3) Uani 1 1 d . . . N1 N 0.79327(13) 0.39581(9) 0.09917(9) 0.0169(3) Uani 1 1 d . . . N2 N 0.80756(13) 0.50997(9) -0.01657(9) 0.0170(3) Uani 1 1 d . . . N3 N 0.59895(14) 0.83975(9) 0.07306(9) 0.0180(3) Uani 1 1 d . . . N4 N 0.72998(14) 0.94548(9) 0.09050(9) 0.0183(3) Uani 1 1 d . . . N5 N 0.55582(13) 1.06411(9) 0.31675(9) 0.0170(3) Uani 1 1 d . . . N6 N 0.66422(13) 1.06795(9) 0.42759(9) 0.0173(3) Uani 1 1 d . . . N7 N 0.65423(19) 0.16840(11) 0.07174(13) 0.0501(6) Uani 1 1 d . A . N9 N 0.39797(16) 0.38466(11) 0.17140(11) 0.0305(4) Uani 1 1 d . A . N8A N 0.45882(19) 0.23706(11) 0.15462(15) 0.0355(6) Uani 0.76 1 d PD A 1 N8B N 0.5168(5) 0.2588(3) 0.1768(3) 0.0355(6) Uani 0.24 1 d PD A 2 C1 C 1.1896(2) 0.53734(13) 0.29965(14) 0.0341(5) Uani 1 1 d . . . H1A H 1.2370 0.5349 0.2385 0.051 Uiso 1 1 calc R . . H1B H 1.2426 0.5365 0.3332 0.051 Uiso 1 1 calc R . . H1C H 1.1338 0.5875 0.3113 0.051 Uiso 1 1 calc R . . C2 C 1.12110(19) 0.46549(13) 0.32410(13) 0.0299(5) Uani 1 1 d . . . H2A H 1.1767 0.4145 0.3113 0.036 Uiso 1 1 calc R . . H2B H 1.0749 0.4665 0.3862 0.036 Uiso 1 1 calc R . . C3 C 0.98633(17) 0.40328(11) 0.27712(11) 0.0189(4) Uani 1 1 d . . . C4 C 0.98603(18) 0.33673(12) 0.33005(12) 0.0234(4) Uani 1 1 d . . . H4 H 1.0250 0.3355 0.3711 0.028 Uiso 1 1 calc R . . C5 C 0.92828(18) 0.27050(12) 0.32359(12) 0.0260(4) Uani 1 1 d . . . H5 H 0.9285 0.2245 0.3600 0.031 Uiso 1 1 calc R . . C6 C 0.87212(17) 0.27250(11) 0.26502(12) 0.0224(4) Uani 1 1 d . . . H6 H 0.8348 0.2270 0.2602 0.027 Uiso 1 1 calc R . . C7 C 0.86805(16) 0.34092(11) 0.21099(11) 0.0170(4) Uani 1 1 d . . . C8 C 0.92535(16) 0.40858(10) 0.21656(11) 0.0161(4) Uani 1 1 d . . . C9 C 0.80529(16) 0.33884(11) 0.15197(11) 0.0186(4) Uani 1 1 d . . . H9 H 0.7695 0.2913 0.1519 0.022 Uiso 1 1 calc R . . C10 C 0.72194(17) 0.38800(11) 0.04455(11) 0.0194(4) Uani 1 1 d . . . H10A H 0.6380 0.4109 0.0738 0.023 Uiso 1 1 calc R . . H10B H 0.7239 0.3301 0.0324 0.023 Uiso 1 1 calc R . . C11 C 0.77529(18) 0.43442(11) -0.03880(11) 0.0209(4) Uani 1 1 d . . . H11A H 0.8468 0.4016 -0.0773 0.025 Uiso 1 1 calc R . . H11B H 0.7164 0.4465 -0.0686 0.025 Uiso 1 1 calc R . . C12 C 0.79926(16) 0.57492(11) -0.06070(11) 0.0191(4) Uani 1 1 d . . . H12 H 0.7635 0.5734 -0.1033 0.023 Uiso 1 1 calc R . . C13 C 0.84012(16) 0.64951(11) -0.05018(11) 0.0185(4) Uani 1 1 d . . . C14 C 0.82122(17) 0.71676(12) -0.10243(11) 0.0225(4) Uani 1 1 d . . . H14 H 0.7788 0.7118 -0.1403 0.027 Uiso 1 1 calc R . . C15 C 0.86299(18) 0.78823(12) -0.09909(12) 0.0252(5) Uani 1 1 d . . . H15 H 0.8497 0.8326 -0.1345 0.030 Uiso 1 1 calc R . . C16 C 0.92535(17) 0.79641(11) -0.04367(12) 0.0234(4) Uani 1 1 d . . . H16 H 0.9533 0.8467 -0.0410 0.028 Uiso 1 1 calc R . . C17 C 0.94685(17) 0.73201(11) 0.00738(11) 0.0191(4) Uani 1 1 d . . . C18 C 0.90369(16) 0.65591(11) 0.00612(11) 0.0181(4) Uani 1 1 d . . . C19 C 1.06622(18) 0.80349(11) 0.06148(12) 0.0245(4) Uani 1 1 d . . . H19A H 1.0055 0.8517 0.0789 0.029 Uiso 1 1 calc R . . H19B H 1.1223 0.8136 0.0034 0.029 Uiso 1 1 calc R . . C20 C 1.1321(2) 0.78801(13) 0.12401(13) 0.0316(5) Uani 1 1 d . . . H20A H 1.0763 0.7755 0.1806 0.047 Uiso 1 1 calc R . . H20B H 1.1682 0.8365 0.1278 0.047 Uiso 1 1 calc R . . H20C H 1.1946 0.7420 0.1045 0.047 Uiso 1 1 calc R . . C21 C 0.7071(2) 0.52849(13) 0.38385(12) 0.0321(5) Uani 1 1 d . . . H21A H 0.7908 0.5365 0.3546 0.048 Uiso 1 1 calc R . . H21B H 0.7031 0.4779 0.4172 0.048 Uiso 1 1 calc R . . H21C H 0.6664 0.5741 0.4223 0.048 Uiso 1 1 calc R . . C22 C 0.64729(19) 0.52378(11) 0.31828(12) 0.0235(4) Uani 1 1 d . . . H22A H 0.6880 0.4780 0.2788 0.028 Uiso 1 1 calc R . . H22B H 0.5629 0.5150 0.3471 0.028 Uiso 1 1 calc R . . C23 C 0.60110(16) 0.60817(11) 0.21027(11) 0.0178(4) Uani 1 1 d . . . C24 C 0.54316(17) 0.55097(12) 0.18926(12) 0.0224(4) Uani 1 1 d . . . H24 H 0.5392 0.4997 0.2177 0.027 Uiso 1 1 calc R . . C25 C 0.48990(18) 0.56764(12) 0.12627(13) 0.0262(4) Uani 1 1 d . . . H25 H 0.4511 0.5276 0.1115 0.031 Uiso 1 1 calc R . . C26 C 0.49407(18) 0.64169(12) 0.08625(12) 0.0249(4) Uani 1 1 d . . . H26 H 0.4572 0.6530 0.0440 0.030 Uiso 1 1 calc R . . C27 C 0.55258(17) 0.70201(11) 0.10684(11) 0.0193(4) Uani 1 1 d . . . C28 C 0.60876(16) 0.68585(11) 0.16869(11) 0.0169(4) Uani 1 1 d . . . C29 C 0.54833(17) 0.77915(12) 0.06377(11) 0.0209(4) Uani 1 1 d . . . H29 H 0.5047 0.7859 0.0254 0.025 Uiso 1 1 calc R . . C30 C 0.58207(18) 0.91779(11) 0.02985(12) 0.0232(4) Uani 1 1 d . . . H30A H 0.5081 0.9507 0.0652 0.028 Uiso 1 1 calc R . . H30B H 0.5745 0.9081 -0.0262 0.028 Uiso 1 1 calc R . . C31 C 0.68882(18) 0.96319(11) 0.01665(11) 0.0214(4) Uani 1 1 d . . . H31A H 0.7536 0.9454 -0.0371 0.026 Uiso 1 1 calc R . . H31B H 0.6657 1.0223 0.0124 0.026 Uiso 1 1 calc R . . C32 C 0.78848(17) 0.99552(11) 0.11079(11) 0.0199(4) Uani 1 1 d . . . H32 H 0.7970 1.0455 0.0801 0.024 Uiso 1 1 calc R . . C33 C 0.84204(17) 0.98174(11) 0.17628(11) 0.0182(4) Uani 1 1 d . . . C34 C 0.90712(18) 1.04237(11) 0.18805(12) 0.0240(4) Uani 1 1 d . . . H34 H 0.9094 1.0912 0.1554 0.029 Uiso 1 1 calc R . . C35 C 0.96643(19) 1.03225(12) 0.24504(12) 0.0269(5) Uani 1 1 d . . . H35 H 1.0096 1.0737 0.2518 0.032 Uiso 1 1 calc R . . C36 C 0.96369(17) 0.96042(12) 0.29384(12) 0.0225(4) Uani 1 1 d . . . H36 H 1.0056 0.9532 0.3333 0.027 Uiso 1 1 calc R . . C37 C 0.90055(16) 0.90048(11) 0.28476(11) 0.0179(4) Uani 1 1 d . . . C38 C 0.83740(16) 0.90905(11) 0.22535(11) 0.0166(4) Uani 1 1 d . . . C39 C 0.96974(17) 0.80749(12) 0.37747(12) 0.0234(4) Uani 1 1 d . . . H39A H 0.9480 0.8462 0.4253 0.028 Uiso 1 1 calc R . . H39B H 1.0541 0.8099 0.3417 0.028 Uiso 1 1 calc R . . C40 C 0.9518(2) 0.72261(12) 0.41168(12) 0.0302(5) Uani 1 1 d . . . H40A H 0.8677 0.7209 0.4462 0.045 Uiso 1 1 calc R . . H40B H 1.0013 0.7068 0.4474 0.045 Uiso 1 1 calc R . . H40C H 0.9747 0.6849 0.3637 0.045 Uiso 1 1 calc R . . C41 C 0.3509(2) 0.66130(13) 0.42889(14) 0.0344(5) Uani 1 1 d . . . H41A H 0.4367 0.6451 0.4153 0.052 Uiso 1 1 calc R . . H41B H 0.3116 0.6131 0.4300 0.052 Uiso 1 1 calc R . . H41C H 0.3178 0.6873 0.4851 0.052 Uiso 1 1 calc R . . C42 C 0.33053(18) 0.72007(12) 0.36176(13) 0.0250(4) Uani 1 1 d . . . H42A H 0.3603 0.6938 0.3050 0.030 Uiso 1 1 calc R . . H42B H 0.2444 0.7389 0.3761 0.030 Uiso 1 1 calc R . . C43 C 0.37936(16) 0.85288(11) 0.31078(11) 0.0180(4) Uani 1 1 d . . . C44 C 0.31118(17) 0.85961(12) 0.25856(11) 0.0229(4) Uani 1 1 d . . . H44 H 0.2733 0.8147 0.2528 0.027 Uiso 1 1 calc R . . C45 C 0.29706(18) 0.93220(12) 0.21365(12) 0.0251(4) Uani 1 1 d . . . H45 H 0.2487 0.9369 0.1785 0.030 Uiso 1 1 calc R . . C46 C 0.35365(17) 0.99582(12) 0.22109(11) 0.0224(4) Uani 1 1 d . . . H46 H 0.3430 1.0451 0.1914 0.027 Uiso 1 1 calc R . . C47 C 0.42770(16) 0.99034(11) 0.27175(11) 0.0177(4) Uani 1 1 d . . . C48 C 0.44193(16) 0.91820(11) 0.31875(11) 0.0166(4) Uani 1 1 d . . . C49 C 0.48570(16) 1.05985(11) 0.27428(11) 0.0183(4) Uani 1 1 d . . . H49 H 0.4709 1.1064 0.2419 0.022 Uiso 1 1 calc R . . C50 C 0.61455(17) 1.13728(11) 0.31100(11) 0.0198(4) Uani 1 1 d . . . H50A H 0.5658 1.1853 0.2971 0.024 Uiso 1 1 calc R . . H50B H 0.6937 1.1310 0.2653 0.024 Uiso 1 1 calc R . . C51 C 0.62827(17) 1.14854(11) 0.39712(11) 0.0195(4) Uani 1 1 d . . . H51A H 0.6896 1.1849 0.3908 0.023 Uiso 1 1 calc R . . H51B H 0.5518 1.1731 0.4385 0.023 Uiso 1 1 calc R . . C52 C 0.73311(16) 1.05910(11) 0.47229(11) 0.0193(4) Uani 1 1 d . . . H52 H 0.7675 1.1054 0.4791 0.023 Uiso 1 1 calc R . . C53 C 0.76262(16) 0.98460(11) 0.51303(11) 0.0169(4) Uani 1 1 d . . . C54 C 0.84721(17) 0.98354(12) 0.55482(11) 0.0218(4) Uani 1 1 d . . . H54 H 0.8864 1.0301 0.5518 0.026 Uiso 1 1 calc R . . C55 C 0.87342(18) 0.91658(12) 0.59939(12) 0.0250(4) Uani 1 1 d . . . H55 H 0.9326 0.9160 0.6253 0.030 Uiso 1 1 calc R . . C56 C 0.81284(17) 0.84857(12) 0.60691(11) 0.0213(4) Uani 1 1 d . . . H56 H 0.8293 0.8026 0.6394 0.026 Uiso 1 1 calc R . . C57 C 0.72968(16) 0.84830(11) 0.56725(11) 0.0174(4) Uani 1 1 d . . . C58 C 0.70358(16) 0.91571(11) 0.51678(11) 0.0167(4) Uani 1 1 d . . . C59 C 0.68488(19) 0.71503(12) 0.61962(12) 0.0242(4) Uani 1 1 d . . . H59A H 0.6690 0.7302 0.6797 0.029 Uiso 1 1 calc R . . H59B H 0.7686 0.6896 0.5954 0.029 Uiso 1 1 calc R . . C60 C 0.6013(2) 0.65678(12) 0.61611(13) 0.0324(5) Uani 1 1 d . . . H60A H 0.5188 0.6809 0.6443 0.049 Uiso 1 1 calc R . . H60B H 0.6169 0.6061 0.6456 0.049 Uiso 1 1 calc R . . H60C H 0.6138 0.6453 0.5562 0.049 Uiso 1 1 calc R . . C61 C 0.57166(18) 0.20643(11) 0.11160(12) 0.0240(4) Uani 1 1 d D . . C62 C 0.43799(19) 0.31857(12) 0.16265(12) 0.0302(5) Uani 1 1 d D . . H5A H 0.936(2) 0.5905(9) 0.2270(15) 0.068(10) Uiso 1 1 d D . . H5B H 0.9656(19) 0.6486(13) 0.1707(10) 0.046(8) Uiso 1 1 d D . . H10C H 0.5641(16) 0.7730(15) 0.3968(13) 0.058(9) Uiso 1 1 d D . . H10D H 0.6371(19) 0.7806(13) 0.4376(12) 0.044(8) Uiso 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 0.01429(12) 0.01427(11) 0.01953(11) 0.00135(8) -0.00778(9) -0.00315(9) Cu2 0.01736(12) 0.01422(11) 0.01889(11) 0.00218(8) -0.00912(9) -0.00171(9) Cu3 0.01297(11) 0.01596(11) 0.01875(11) 0.00098(8) -0.00693(9) -0.00294(9) Na1 0.0216(4) 0.0185(4) 0.0205(4) 0.0004(3) -0.0094(3) -0.0001(3) O1 0.0262(8) 0.0198(7) 0.0323(7) 0.0018(6) -0.0198(6) -0.0040(6) O2 0.0197(7) 0.0131(6) 0.0220(6) 0.0006(5) -0.0097(5) -0.0034(5) O3 0.0222(7) 0.0177(7) 0.0290(7) 0.0063(5) -0.0142(6) -0.0052(6) O4 0.0223(7) 0.0154(7) 0.0295(7) 0.0014(5) -0.0085(6) -0.0073(6) O5 0.0279(8) 0.0183(8) 0.0244(8) -0.0006(6) -0.0087(6) -0.0036(6) O6 0.0248(8) 0.0164(7) 0.0224(6) 0.0039(5) -0.0114(6) -0.0048(6) O7 0.0226(7) 0.0159(6) 0.0204(6) 0.0035(5) -0.0130(6) -0.0058(5) O8 0.0209(7) 0.0149(6) 0.0233(6) 0.0020(5) -0.0125(6) -0.0049(5) O9 0.0210(7) 0.0206(7) 0.0219(6) 0.0007(5) -0.0117(6) -0.0020(6) O10 0.0233(8) 0.0228(8) 0.0251(7) -0.0026(6) -0.0126(6) -0.0008(6) O11 0.0224(7) 0.0192(7) 0.0317(7) 0.0027(6) -0.0145(6) -0.0078(6) O12 0.0182(7) 0.0195(7) 0.0225(6) 0.0015(5) -0.0116(5) -0.0028(5) O13 0.0169(7) 0.0200(7) 0.0228(6) 0.0018(5) -0.0109(5) -0.0046(5) O14 0.0211(7) 0.0195(7) 0.0229(7) 0.0030(5) -0.0114(6) -0.0033(6) N1 0.0133(8) 0.0172(8) 0.0197(7) -0.0042(6) -0.0047(6) -0.0007(6) N2 0.0133(8) 0.0185(8) 0.0192(7) -0.0025(6) -0.0053(6) -0.0013(6) N3 0.0165(8) 0.0187(8) 0.0179(7) 0.0023(6) -0.0060(6) 0.0005(6) N4 0.0195(8) 0.0162(8) 0.0193(7) 0.0017(6) -0.0085(7) 0.0014(6) N5 0.0147(8) 0.0166(8) 0.0178(7) -0.0013(6) -0.0028(6) -0.0030(6) N6 0.0137(8) 0.0190(8) 0.0176(7) -0.0012(6) -0.0032(6) -0.0018(6) N7 0.0441(13) 0.0244(10) 0.0579(13) 0.0079(9) 0.0082(11) 0.0053(10) N9 0.0294(10) 0.0274(10) 0.0327(9) -0.0003(8) -0.0091(8) -0.0001(8) N8A 0.0243(14) 0.0222(12) 0.0473(14) 0.0063(10) 0.0014(11) 0.0011(10) N8B 0.0243(14) 0.0222(12) 0.0473(14) 0.0063(10) 0.0014(11) 0.0011(10) C1 0.0299(13) 0.0333(12) 0.0450(13) -0.0084(10) -0.0198(11) -0.0019(10) C2 0.0283(12) 0.0378(13) 0.0312(11) -0.0004(9) -0.0200(10) -0.0033(10) C3 0.0164(9) 0.0166(9) 0.0220(9) -0.0031(7) -0.0048(8) 0.0004(7) C4 0.0236(11) 0.0267(11) 0.0209(9) 0.0028(8) -0.0107(8) 0.0004(9) C5 0.0283(12) 0.0215(10) 0.0260(10) 0.0092(8) -0.0084(9) -0.0013(9) C6 0.0215(10) 0.0163(9) 0.0258(10) 0.0031(8) -0.0034(8) -0.0039(8) C7 0.0141(9) 0.0158(9) 0.0182(9) 0.0003(7) -0.0021(7) -0.0015(7) C8 0.0136(9) 0.0145(9) 0.0170(8) -0.0011(7) -0.0021(7) 0.0014(7) C9 0.0153(9) 0.0151(9) 0.0227(9) -0.0026(7) -0.0016(8) -0.0045(7) C10 0.0161(9) 0.0186(9) 0.0252(9) -0.0032(7) -0.0087(8) -0.0026(7) C11 0.0217(10) 0.0213(10) 0.0224(9) -0.0029(7) -0.0110(8) -0.0021(8) C12 0.0128(9) 0.0248(10) 0.0182(9) -0.0016(7) -0.0045(7) 0.0017(8) C13 0.0129(9) 0.0192(9) 0.0190(9) 0.0012(7) -0.0017(7) 0.0020(7) C14 0.0179(10) 0.0250(10) 0.0196(9) 0.0019(8) -0.0034(8) 0.0056(8) C15 0.0232(11) 0.0208(10) 0.0226(10) 0.0062(8) 0.0001(8) 0.0042(8) C16 0.0204(10) 0.0141(9) 0.0277(10) 0.0017(8) 0.0009(8) 0.0002(8) C17 0.0160(9) 0.0159(9) 0.0214(9) 0.0004(7) -0.0012(8) -0.0020(7) C18 0.0140(9) 0.0160(9) 0.0204(9) 0.0003(7) -0.0020(7) 0.0006(7) C19 0.0243(11) 0.0156(9) 0.0290(10) -0.0042(8) -0.0002(9) -0.0092(8) C20 0.0323(13) 0.0273(11) 0.0353(12) -0.0097(9) -0.0069(10) -0.0129(10) C21 0.0423(14) 0.0271(11) 0.0268(11) 0.0067(9) -0.0143(10) 0.0003(10) C22 0.0258(11) 0.0161(9) 0.0251(10) 0.0042(8) -0.0060(9) 0.0004(8) C23 0.0156(9) 0.0175(9) 0.0191(9) -0.0003(7) -0.0049(7) -0.0008(7) C24 0.0185(10) 0.0180(10) 0.0282(10) -0.0010(8) -0.0046(8) -0.0020(8) C25 0.0209(11) 0.0240(11) 0.0369(11) -0.0046(9) -0.0120(9) -0.0059(8) C26 0.0206(10) 0.0282(11) 0.0309(11) -0.0020(8) -0.0155(9) -0.0014(8) C27 0.0166(10) 0.0224(10) 0.0192(9) -0.0013(7) -0.0061(8) -0.0031(8) C28 0.0137(9) 0.0183(9) 0.0166(8) -0.0010(7) -0.0029(7) -0.0009(7) C29 0.0181(10) 0.0278(11) 0.0186(9) 0.0005(8) -0.0101(8) 0.0006(8) C30 0.0258(11) 0.0214(10) 0.0243(10) 0.0045(8) -0.0134(9) 0.0012(8) C31 0.0274(11) 0.0161(9) 0.0209(9) 0.0035(7) -0.0107(8) 0.0018(8) C32 0.0202(10) 0.0129(9) 0.0227(9) 0.0019(7) -0.0038(8) 0.0009(7) C33 0.0168(9) 0.0152(9) 0.0201(9) -0.0022(7) -0.0030(8) -0.0006(7) C34 0.0264(11) 0.0159(9) 0.0276(10) -0.0016(8) -0.0055(9) -0.0053(8) C35 0.0272(11) 0.0245(11) 0.0289(10) -0.0033(8) -0.0056(9) -0.0128(9) C36 0.0183(10) 0.0270(11) 0.0232(10) -0.0056(8) -0.0072(8) -0.0040(8) C37 0.0144(9) 0.0207(10) 0.0169(9) -0.0021(7) -0.0033(7) -0.0014(7) C38 0.0134(9) 0.0168(9) 0.0170(9) -0.0033(7) -0.0026(7) 0.0011(7) C39 0.0160(10) 0.0356(12) 0.0194(9) -0.0009(8) -0.0083(8) 0.0006(8) C40 0.0337(13) 0.0309(12) 0.0255(10) 0.0001(9) -0.0134(9) 0.0063(10) C41 0.0383(14) 0.0253(11) 0.0460(13) 0.0049(10) -0.0201(11) -0.0122(10) C42 0.0209(11) 0.0228(10) 0.0344(11) -0.0029(8) -0.0109(9) -0.0082(8) C43 0.0139(9) 0.0215(10) 0.0181(9) -0.0027(7) -0.0041(7) -0.0028(7) C44 0.0187(10) 0.0285(11) 0.0232(10) -0.0045(8) -0.0074(8) -0.0066(8) C45 0.0224(11) 0.0342(12) 0.0221(10) -0.0020(8) -0.0117(8) -0.0035(9) C46 0.0230(11) 0.0277(11) 0.0168(9) 0.0023(8) -0.0081(8) -0.0012(8) C47 0.0147(9) 0.0218(10) 0.0148(8) -0.0015(7) -0.0029(7) -0.0017(7) C48 0.0122(9) 0.0209(9) 0.0151(8) -0.0025(7) -0.0026(7) -0.0013(7) C49 0.0190(10) 0.0196(9) 0.0133(8) 0.0014(7) -0.0029(7) -0.0003(8) C50 0.0173(10) 0.0155(9) 0.0242(9) 0.0024(7) -0.0039(8) -0.0040(7) C51 0.0170(10) 0.0169(9) 0.0235(9) 0.0004(7) -0.0050(8) -0.0035(7) C52 0.0143(9) 0.0218(10) 0.0201(9) -0.0053(7) -0.0020(7) -0.0047(8) C53 0.0100(9) 0.0226(10) 0.0169(8) -0.0039(7) -0.0034(7) 0.0001(7) C54 0.0154(10) 0.0266(11) 0.0252(10) -0.0074(8) -0.0080(8) -0.0032(8) C55 0.0195(10) 0.0336(12) 0.0254(10) -0.0057(8) -0.0125(8) 0.0003(9) C56 0.0193(10) 0.0269(10) 0.0182(9) -0.0035(7) -0.0082(8) 0.0019(8) C57 0.0140(9) 0.0207(9) 0.0156(8) -0.0039(7) -0.0030(7) 0.0006(7) C58 0.0106(9) 0.0226(10) 0.0153(8) -0.0053(7) -0.0026(7) 0.0004(7) C59 0.0276(11) 0.0246(10) 0.0199(9) 0.0054(8) -0.0094(8) 0.0001(9) C60 0.0452(15) 0.0246(11) 0.0301(11) 0.0051(9) -0.0165(10) -0.0057(10) C61 0.0303(12) 0.0182(10) 0.0223(10) 0.0064(8) -0.0085(9) -0.0026(9) C62 0.0290(12) 0.0284(12) 0.0229(10) 0.0084(8) 0.0003(9) 0.0041(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.9075(13) . ? Cu1 O2 1.9106(12) . ? Cu1 N2 1.9292(15) . ? Cu1 N1 1.9477(15) . ? Cu2 O7 1.8894(12) . ? Cu2 O8 1.8991(12) . ? Cu2 N3 1.9172(15) . ? Cu2 N4 1.9317(15) . ? Cu3 O12 1.9018(13) . ? Cu3 O13 1.9139(12) . ? Cu3 N5 1.9388(15) . ? Cu3 N6 1.9406(15) . ? Na1 O7 2.3088(14) . ? Na1 O10 2.3110(16) . ? Na1 O5 2.3264(16) . ? Na1 O8 2.3566(14) . ? Na1 O6 2.6610(15) . ? Na1 O9 2.7272(15) . ? Na1 H5B 2.650(18) . ? Na1 H10C 2.597(18) . ? Na1 H10D 2.641(17) . ? O1 C3 1.365(2) . ? O1 C2 1.425(2) . ? O2 C8 1.309(2) . ? O3 C18 1.312(2) . ? O4 C17 1.363(2) . ? O4 C19 1.437(2) . ? O5 H5A 0.783(15) . ? O5 H5B 0.816(15) . ? O6 C23 1.371(2) . ? O6 C22 1.428(2) . ? O7 C28 1.312(2) . ? O8 C38 1.309(2) . ? O9 C37 1.368(2) . ? O9 C39 1.435(2) . ? O10 H10C 0.791(15) . ? O10 H10D 0.800(15) . ? O11 C43 1.370(2) . ? O11 C42 1.428(2) . ? O12 C48 1.304(2) . ? O13 C58 1.313(2) . ? O14 C57 1.372(2) . ? O14 C59 1.432(2) . ? N1 C9 1.284(2) . ? N1 C10 1.469(2) . ? N2 C12 1.284(2) . ? N2 C11 1.464(2) . ? N3 C29 1.287(2) . ? N3 C30 1.472(2) . ? N4 C32 1.286(2) . ? N4 C31 1.476(2) . ? N5 C49 1.284(2) . ? N5 C50 1.470(2) . ? N6 C52 1.281(2) . ? N6 C51 1.469(2) . ? N7 C61 1.118(2) . ? N9 C62 1.134(2) . ? N8A C61 1.342(2) . ? N8A C62 1.349(2) . ? N8B C62 1.349(3) . ? N8B C61 1.349(3) . ? C1 C2 1.501(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.375(2) . ? C3 C8 1.429(3) . ? C4 C5 1.406(3) . ? C4 H4 0.9500 . ? C5 C6 1.360(3) . ? C5 H5 0.9500 . ? C6 C7 1.417(2) . ? C6 H6 0.9500 . ? C7 C8 1.419(3) . ? C7 C9 1.434(3) . ? C9 H9 0.9500 . ? C10 C11 1.527(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.434(3) . ? C12 H12 0.9500 . ? C13 C18 1.414(3) . ? C13 C14 1.420(2) . ? C14 C15 1.362(3) . ? C14 H14 0.9500 . ? C15 C16 1.396(3) . ? C15 H15 0.9500 . ? C16 C17 1.382(2) . ? C16 H16 0.9500 . ? C17 C18 1.434(3) . ? C19 C20 1.503(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.509(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.376(3) . ? C23 C28 1.430(2) . ? C24 C25 1.402(3) . ? C24 H24 0.9500 . ? C25 C26 1.366(3) . ? C25 H25 0.9500 . ? C26 C27 1.418(3) . ? C26 H26 0.9500 . ? C27 C28 1.409(2) . ? C27 C29 1.438(3) . ? C29 H29 0.9500 . ? C30 C31 1.523(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.439(3) . ? C32 H32 0.9500 . ? C33 C34 1.417(3) . ? C33 C38 1.417(2) . ? C34 C35 1.361(3) . ? C34 H34 0.9500 . ? C35 C36 1.404(3) . ? C35 H35 0.9500 . ? C36 C37 1.376(3) . ? C36 H36 0.9500 . ? C37 C38 1.430(2) . ? C39 C40 1.507(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.505(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.377(3) . ? C43 C48 1.438(2) . ? C44 C45 1.406(3) . ? C44 H44 0.9500 . ? C45 C46 1.365(3) . ? C45 H45 0.9500 . ? C46 C47 1.414(3) . ? C46 H46 0.9500 . ? C47 C48 1.419(2) . ? C47 C49 1.438(3) . ? C49 H49 0.9500 . ? C50 C51 1.520(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.440(3) . ? C52 H52 0.9500 . ? C53 C54 1.414(3) . ? C53 C58 1.415(3) . ? C54 C55 1.365(3) . ? C54 H54 0.9500 . ? C55 C56 1.403(3) . ? C55 H55 0.9500 . ? C56 C57 1.376(3) . ? C56 H56 0.9500 . ? C57 C58 1.429(2) . ? C59 C60 1.504(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 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 O3 Cu1 O2 90.49(5) . . ? O3 Cu1 N2 92.40(6) . . ? O2 Cu1 N2 176.71(6) . . ? O3 Cu1 N1 176.07(6) . . ? O2 Cu1 N1 92.67(6) . . ? N2 Cu1 N1 84.51(6) . . ? O7 Cu2 O8 86.97(5) . . ? O7 Cu2 N3 94.31(6) . . ? O8 Cu2 N3 176.86(6) . . ? O7 Cu2 N4 176.81(6) . . ? O8 Cu2 N4 93.75(6) . . ? N3 Cu2 N4 85.13(6) . . ? O12 Cu3 O13 90.13(5) . . ? O12 Cu3 N5 93.35(6) . . ? O13 Cu3 N5 176.51(6) . . ? O12 Cu3 N6 176.53(6) . . ? O13 Cu3 N6 92.12(6) . . ? N5 Cu3 N6 84.40(6) . . ? O7 Na1 O10 99.78(6) . . ? O7 Na1 O5 107.68(5) . . ? O10 Na1 O5 144.96(6) . . ? O7 Na1 O8 67.94(5) . . ? O10 Na1 O8 101.59(5) . . ? O5 Na1 O8 108.59(6) . . ? O7 Na1 O6 62.40(4) . . ? O10 Na1 O6 86.10(5) . . ? O5 Na1 O6 87.70(5) . . ? O8 Na1 O6 130.33(5) . . ? O7 Na1 O9 128.33(5) . . ? O10 Na1 O9 89.61(5) . . ? O5 Na1 O9 90.09(5) . . ? O8 Na1 O9 60.40(4) . . ? O6 Na1 O9 169.09(5) . . ? O7 Na1 H5B 93.2(4) . . ? O10 Na1 H5B 162.2(4) . . ? O5 Na1 H5B 17.4(4) . . ? O8 Na1 H5B 94.6(4) . . ? O6 Na1 H5B 89.2(5) . . ? O9 Na1 H5B 91.8(5) . . ? O7 Na1 H10C 83.3(4) . . ? O10 Na1 H10C 17.3(4) . . ? O5 Na1 H10C 160.3(5) . . ? O8 Na1 H10C 90.6(5) . . ? O6 Na1 H10C 83.0(6) . . ? O9 Na1 H10C 95.8(5) . . ? H5B Na1 H10C 172.2(8) . . ? O7 Na1 H10D 110.9(5) . . ? O10 Na1 H10D 17.0(4) . . ? O5 Na1 H10D 140.4(5) . . ? O8 Na1 H10D 93.7(5) . . ? O6 Na1 H10D 102.6(4) . . ? O9 Na1 H10D 72.7(4) . . ? H5B Na1 H10D 155.8(7) . . ? H10C Na1 H10D 28.8(5) . . ? C3 O1 C2 118.08(15) . . ? C8 O2 Cu1 127.14(12) . . ? C18 O3 Cu1 126.07(12) . . ? C17 O4 C19 117.82(14) . . ? Na1 O5 H5A 110.5(17) . . ? Na1 O5 H5B 104.4(14) . . ? H5A O5 H5B 109(2) . . ? C23 O6 C22 117.10(14) . . ? C23 O6 Na1 116.29(10) . . ? C22 O6 Na1 126.52(11) . . ? C28 O7 Cu2 126.64(11) . . ? C28 O7 Na1 129.61(11) . . ? Cu2 O7 Na1 103.55(6) . . ? C38 O8 Cu2 127.00(11) . . ? C38 O8 Na1 131.49(11) . . ? Cu2 O8 Na1 101.50(6) . . ? C37 O9 C39 117.35(15) . . ? C37 O9 Na1 117.30(11) . . ? C39 O9 Na1 124.35(11) . . ? Na1 O10 H10C 102.3(15) . . ? Na1 O10 H10D 105.6(15) . . ? H10C O10 H10D 110(2) . . ? C43 O11 C42 117.77(15) . . ? C48 O12 Cu3 126.62(11) . . ? C58 O13 Cu3 126.37(12) . . ? C57 O14 C59 117.47(15) . . ? C9 N1 C10 120.44(16) . . ? C9 N1 Cu1 126.54(14) . . ? C10 N1 Cu1 112.98(11) . . ? C12 N2 C11 120.21(16) . . ? C12 N2 Cu1 127.37(13) . . ? C11 N2 Cu1 112.36(11) . . ? C29 N3 C30 120.46(16) . . ? C29 N3 Cu2 125.92(13) . . ? C30 N3 Cu2 113.58(12) . . ? C32 N4 C31 120.06(15) . . ? C32 N4 Cu2 126.33(13) . . ? C31 N4 Cu2 113.53(12) . . ? C49 N5 C50 120.26(16) . . ? C49 N5 Cu3 126.33(13) . . ? C50 N5 Cu3 113.29(12) . . ? C52 N6 C51 121.08(16) . . ? C52 N6 Cu3 126.85(13) . . ? C51 N6 Cu3 111.96(12) . . ? C61 N8A C62 115.9(2) . . ? C62 N8B C61 115.5(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 108.15(17) . . ? O1 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O1 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O1 C3 C4 125.05(18) . . ? O1 C3 C8 113.41(15) . . ? C4 C3 C8 121.54(18) . . ? C3 C4 C5 120.22(18) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.82(17) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.45(18) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C8 119.72(17) . . ? C6 C7 C9 118.04(17) . . ? C8 C7 C9 122.25(16) . . ? O2 C8 C7 125.19(17) . . ? O2 C8 C3 117.62(16) . . ? C7 C8 C3 117.20(16) . . ? N1 C9 C7 125.56(17) . . ? N1 C9 H9 117.2 . . ? C7 C9 H9 117.2 . . ? N1 C10 C11 107.81(15) . . ? N1 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? N1 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.5 . . ? N2 C11 C10 107.52(14) . . ? N2 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? N2 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N2 C12 C13 124.63(18) . . ? N2 C12 H12 117.7 . . ? C13 C12 H12 117.7 . . ? C18 C13 C14 120.09(18) . . ? C18 C13 C12 122.02(16) . . ? C14 C13 C12 117.78(18) . . ? C15 C14 C13 121.03(19) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.09(18) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.57(18) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? O4 C17 C16 125.37(17) . . ? O4 C17 C18 113.60(15) . . ? C16 C17 C18 121.02(19) . . ? O3 C18 C13 125.47(17) . . ? O3 C18 C17 117.30(17) . . ? C13 C18 C17 117.18(16) . . ? O4 C19 C20 107.38(15) . . ? O4 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O4 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 C21 107.70(16) . . ? O6 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? O6 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? O6 C23 C24 125.37(16) . . ? O6 C23 C28 113.50(16) . . ? C24 C23 C28 121.12(17) . . ? C23 C24 C25 120.60(18) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 119.73(18) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.96(18) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C28 C27 C26 120.16(17) . . ? C28 C27 C29 122.87(17) . . ? C26 C27 C29 116.95(17) . . ? O7 C28 C27 124.72(16) . . ? O7 C28 C23 117.88(16) . . ? C27 C28 C23 117.40(17) . . ? N3 C29 C27 125.19(17) . . ? N3 C29 H29 117.4 . . ? C27 C29 H29 117.4 . . ? N3 C30 C31 109.06(15) . . ? N3 C30 H30A 109.9 . . ? C31 C30 H30A 109.9 . . ? N3 C30 H30B 109.9 . . ? C31 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? N4 C31 C30 108.25(14) . . ? N4 C31 H31A 110.0 . . ? C30 C31 H31A 110.0 . . ? N4 C31 H31B 110.0 . . ? C30 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? N4 C32 C33 125.15(17) . . ? N4 C32 H32 117.4 . . ? C33 C32 H32 117.4 . . ? C34 C33 C38 119.51(17) . . ? C34 C33 C32 117.62(16) . . ? C38 C33 C32 122.79(17) . . ? C35 C34 C33 121.52(18) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 C35 C36 119.87(18) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C36 C35 120.29(18) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? O9 C37 C36 125.48(17) . . ? O9 C37 C38 113.17(16) . . ? C36 C37 C38 121.31(17) . . ? O8 C38 C33 124.84(17) . . ? O8 C38 C37 117.62(16) . . ? C33 C38 C37 117.50(17) . . ? O9 C39 C40 106.77(16) . . ? O9 C39 H39A 110.4 . . ? C40 C39 H39A 110.4 . . ? O9 C39 H39B 110.4 . . ? C40 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O11 C42 C41 106.69(16) . . ? O11 C42 H42A 110.4 . . ? C41 C42 H42A 110.4 . . ? O11 C42 H42B 110.4 . . ? C41 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? O11 C43 C44 125.62(17) . . ? O11 C43 C48 112.91(16) . . ? C44 C43 C48 121.46(17) . . ? C43 C44 C45 120.66(18) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 119.24(18) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C47 121.79(18) . . ? C45 C46 H46 119.1 . . ? C47 C46 H46 119.1 . . ? C46 C47 C48 120.05(17) . . ? C46 C47 C49 117.88(16) . . ? C48 C47 C49 122.06(17) . . ? O12 C48 C47 125.76(17) . . ? O12 C48 C43 117.48(16) . . ? C47 C48 C43 116.75(17) . . ? N5 C49 C47 125.25(17) . . ? N5 C49 H49 117.4 . . ? C47 C49 H49 117.4 . . ? N5 C50 C51 107.94(14) . . ? N5 C50 H50A 110.1 . . ? C51 C50 H50A 110.1 . . ? N5 C50 H50B 110.1 . . ? C51 C50 H50B 110.1 . . ? H50A C50 H50B 108.4 . . ? N6 C51 C50 107.47(14) . . ? N6 C51 H51A 110.2 . . ? C50 C51 H51A 110.2 . . ? N6 C51 H51B 110.2 . . ? C50 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? N6 C52 C53 125.21(17) . . ? N6 C52 H52 117.4 . . ? C53 C52 H52 117.4 . . ? C54 C53 C58 120.22(17) . . ? C54 C53 C52 118.06(17) . . ? C58 C53 C52 121.58(17) . . ? C55 C54 C53 121.00(18) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? C54 C55 C56 119.95(19) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C57 C56 C55 120.11(18) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? O14 C57 C56 125.08(17) . . ? O14 C57 C58 113.25(16) . . ? C56 C57 C58 121.66(18) . . ? O13 C58 C53 125.36(17) . . ? O13 C58 C57 117.68(16) . . ? C53 C58 C57 116.95(17) . . ? O14 C59 C60 107.49(16) . . ? O14 C59 H59A 110.2 . . ? C60 C59 H59A 110.2 . . ? O14 C59 H59B 110.2 . . ? C60 C59 H59B 110.2 . . ? H59A C59 H59B 108.5 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N7 C61 N8A 165.3(3) . . ? N7 C61 N8B 149.4(3) . . ? N9 C62 N8B 147.9(3) . . ? N9 C62 N8A 166.3(3) . . ? 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 O5 H5A O1 0.783(15) 2.49(2) 3.0693(19) 132(2) . O5 H5A O2 0.783(15) 2.209(19) 2.9125(18) 150(2) . O5 H5B O3 0.816(15) 2.33(2) 2.9519(19) 133(2) . O5 H5B O4 0.816(15) 2.189(17) 2.9475(19) 155(2) . O10 H10C O11 0.791(15) 2.302(17) 3.041(2) 156(3) . O10 H10C O12 0.791(15) 2.31(2) 2.9308(19) 136(2) . O10 H10D O13 0.800(15) 2.260(18) 2.9649(19) 147(2) . O10 H10D O14 0.800(15) 2.353(18) 2.9890(19) 137(2) . _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.684 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.078 #==== end data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H26 Cu Mg N2 O7, 2(C20 H22 Cu N2 O4), 2(N O3), O' _chemical_formula_sum 'C60 H70 Cu3 Mg N8 O22' _chemical_formula_weight 1470.17 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' 'Mg' 'Mg' 0.0486 0.0363 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7379(14) _cell_length_b 15.5892(19) _cell_length_c 16.265(2) _cell_angle_alpha 85.814(10) _cell_angle_beta 73.400(10) _cell_angle_gamma 85.944(9) _cell_volume 3082.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5518 _cell_measurement_theta_min 2.6072 _cell_measurement_theta_max 30.7403 _exptl_crystal_description block _exptl_crystal_colour 'red-brown' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1522 _exptl_absorpt_coefficient_mu 1.123 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) 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 120(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_measurement_method ? _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26411 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.1241 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10885 _reflns_number_gt 6267 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0523P)^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 10885 _refine_ls_number_parameters 865 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.912 _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 0.87205(5) 0.53830(4) 0.02544(4) 0.02057(17) Uani 1 1 d . . . Cu2 Cu 0.68881(5) 0.81813(4) 0.13943(4) 0.01973(17) Uani 1 1 d . . . Cu3 Cu 0.60287(5) 1.00055(4) 0.40991(4) 0.02176(17) Uani 1 1 d . . . Mg1 Mg 0.78743(12) 0.71962(11) 0.27494(10) 0.0175(4) Uani 1 1 d D . . O1 O 1.0442(3) 0.5181(2) 0.2339(2) 0.0239(8) Uani 1 1 d . . . O2 O 0.9528(2) 0.5136(2) 0.1095(2) 0.0231(8) Uani 1 1 d . . . O3 O 0.8998(2) 0.6571(2) 0.0206(2) 0.0213(8) Uani 1 1 d . . . O4 O 0.9864(3) 0.8009(2) 0.0203(2) 0.0267(9) Uani 1 1 d . . . O5 O 0.9253(3) 0.6779(2) 0.1861(2) 0.0222(8) Uani 1 1 d D . . H5A H 0.946(3) 0.6262(16) 0.191(2) 0.033 Uiso 1 1 d D . . H5B H 0.933(3) 0.698(3) 0.1354(14) 0.033 Uiso 1 1 d D . . O6 O 0.7193(2) 0.5639(2) 0.2758(2) 0.0220(8) Uani 1 1 d . . . O7 O 0.6911(2) 0.7057(2) 0.1924(2) 0.0189(8) Uani 1 1 d . . . O8 O 0.7849(2) 0.8372(2) 0.2051(2) 0.0175(8) Uani 1 1 d . . . O9 O 0.8919(2) 0.8343(2) 0.3168(2) 0.0209(8) Uani 1 1 d . . . O10 O 0.8265(3) 0.6636(3) 0.3792(3) 0.0515(12) Uani 1 1 d U . . O11 O 0.6537(3) 0.7650(2) 0.3689(2) 0.0276(9) Uani 1 1 d D . . H11C H 0.603(3) 0.791(3) 0.353(2) 0.041 Uiso 1 1 d D . . H11D H 0.666(3) 0.787(3) 0.411(2) 0.041 Uiso 1 1 d D . . O12 O 0.4537(2) 0.7971(2) 0.3129(2) 0.0254(8) Uani 1 1 d . . . O13 O 0.5412(2) 0.9243(2) 0.3528(2) 0.0246(9) Uani 1 1 d . . . O14 O 0.6558(2) 0.9036(2) 0.4701(2) 0.0227(8) Uani 1 1 d . . . O15 O 0.7108(3) 0.7561(2) 0.5459(2) 0.0298(9) Uani 1 1 d . . . O16 O 0.1467(4) 0.7480(3) 0.4950(3) 0.0622(13) Uani 1 1 d U . . O17 O 0.1824(3) 0.6109(3) 0.4929(3) 0.0466(12) Uani 1 1 d . . . O18 O 0.0164(3) 0.6628(2) 0.5088(2) 0.0366(10) Uani 1 1 d . . . O19 O 0.6240(3) 0.2528(3) 0.1763(3) 0.0618(13) Uani 1 1 d U . . O20 O 0.4796(3) 0.2736(3) 0.1325(3) 0.0559(13) Uani 1 1 d . . . O21 O 0.6263(3) 0.2129(3) 0.0524(3) 0.0647(14) Uani 1 1 d . . . O22 O 0.8985(3) 0.5434(3) 0.4671(3) 0.0624(13) Uani 1 1 d U . . N1 N 0.8335(3) 0.4200(3) 0.0307(2) 0.0205(10) Uani 1 1 d . . . N2 N 0.7844(3) 0.5575(3) -0.0563(3) 0.0238(10) Uani 1 1 d . . . N3 N 0.6019(3) 0.7939(3) 0.0668(2) 0.0200(10) Uani 1 1 d . . . N4 N 0.6740(3) 0.9359(3) 0.1002(2) 0.0200(10) Uani 1 1 d . . . N5 N 0.5534(3) 1.1011(3) 0.3503(3) 0.0240(10) Uani 1 1 d . . . N6 N 0.6584(3) 1.0828(3) 0.4674(3) 0.0257(11) Uani 1 1 d . . . N7 N 0.1160(4) 0.6735(3) 0.4990(3) 0.0373(12) Uani 1 1 d . . . N8 N 0.5771(4) 0.2474(3) 0.1193(3) 0.0389(13) Uani 1 1 d . . . C1 C 1.1541(4) 0.6043(3) 0.2866(3) 0.0348(14) Uani 1 1 d . . . H1A H 1.1999 0.6188 0.2284 0.052 Uiso 1 1 calc R . . H1B H 1.1976 0.6058 0.3274 0.052 Uiso 1 1 calc R . . H1C H 1.0915 0.6463 0.3017 0.052 Uiso 1 1 calc R . . C2 C 1.1129(4) 0.5151(3) 0.2905(3) 0.0270(13) Uani 1 1 d . . . H2A H 1.1753 0.4726 0.2719 0.032 Uiso 1 1 calc R . . H2B H 1.0704 0.4983 0.3499 0.032 Uiso 1 1 calc R . . C3 C 0.9921(4) 0.4438(3) 0.2317(3) 0.0204(12) Uani 1 1 d . . . C4 C 0.9864(4) 0.3755(3) 0.2904(3) 0.0225(12) Uani 1 1 d . . . H4 H 1.0202 0.3773 0.3352 0.027 Uiso 1 1 calc R . . C5 C 0.9309(4) 0.3032(3) 0.2843(3) 0.0242(12) Uani 1 1 d . . . H5 H 0.9258 0.2558 0.3251 0.029 Uiso 1 1 calc R . . C6 C 0.8837(4) 0.3016(3) 0.2183(3) 0.0271(13) Uani 1 1 d . . . H6 H 0.8467 0.2521 0.2138 0.032 Uiso 1 1 calc R . . C7 C 0.8883(4) 0.3709(3) 0.1572(3) 0.0198(12) Uani 1 1 d . . . C8 C 0.9434(4) 0.4453(3) 0.1627(3) 0.0160(11) Uani 1 1 d . . . C9 C 0.8423(4) 0.3618(3) 0.0863(3) 0.0236(12) Uani 1 1 d . . . H9 H 0.8166 0.3071 0.0817 0.028 Uiso 1 1 calc R . . C10 C 0.7934(4) 0.4019(3) -0.0429(3) 0.0270(11) Uani 1 1 d U . . H10A H 0.7471 0.3514 -0.0281 0.032 Uiso 1 1 calc R . . H10B H 0.8561 0.3891 -0.0934 0.032 Uiso 1 1 calc R . . C11 C 0.7265(4) 0.4816(3) -0.0629(3) 0.0263(11) Uani 1 1 d U . . H11A H 0.7186 0.4803 -0.1216 0.032 Uiso 1 1 calc R . . H11B H 0.6524 0.4834 -0.0216 0.032 Uiso 1 1 calc R . . C12 C 0.7753(4) 0.6283(4) -0.1012(3) 0.0240(13) Uani 1 1 d . . . H12 H 0.7324 0.6277 -0.1403 0.029 Uiso 1 1 calc R . . C13 C 0.8241(4) 0.7075(3) -0.0973(3) 0.0219(12) Uani 1 1 d . . . C14 C 0.8142(4) 0.7745(4) -0.1568(3) 0.0316(14) Uani 1 1 d . . . H14 H 0.7756 0.7662 -0.1974 0.038 Uiso 1 1 calc R . . C15 C 0.8594(4) 0.8526(4) -0.1578(3) 0.0329(14) Uani 1 1 d . . . H15 H 0.8530 0.8977 -0.1990 0.039 Uiso 1 1 calc R . . C16 C 0.9152(4) 0.8639(3) -0.0963(3) 0.0276(13) Uani 1 1 d . . . H16 H 0.9443 0.9181 -0.0948 0.033 Uiso 1 1 calc R . . C17 C 0.9283(4) 0.7979(3) -0.0385(3) 0.0206(12) Uani 1 1 d . . . C18 C 0.8835(4) 0.7157(3) -0.0356(3) 0.0188(12) Uani 1 1 d . . . C19 C 1.0327(4) 0.8811(3) 0.0252(3) 0.0309(14) Uani 1 1 d . . . H19A H 0.9738 0.9260 0.0458 0.037 Uiso 1 1 calc R . . H19B H 1.0791 0.9008 -0.0321 0.037 Uiso 1 1 calc R . . C20 C 1.1005(5) 0.8655(4) 0.0871(4) 0.0411(15) Uani 1 1 d . . . H20A H 1.0547 0.8429 0.1426 0.062 Uiso 1 1 calc R . . H20B H 1.1300 0.9198 0.0949 0.062 Uiso 1 1 calc R . . H20C H 1.1612 0.8237 0.0644 0.062 Uiso 1 1 calc R . . C21 C 0.6207(4) 0.4865(4) 0.4098(3) 0.0345(14) Uani 1 1 d . . . H21A H 0.6089 0.5401 0.4398 0.052 Uiso 1 1 calc R . . H21B H 0.6292 0.4379 0.4496 0.052 Uiso 1 1 calc R . . H21C H 0.5575 0.4785 0.3887 0.052 Uiso 1 1 calc R . . C22 C 0.7232(4) 0.4909(3) 0.3348(3) 0.0244(12) Uani 1 1 d . . . H22A H 0.7875 0.4942 0.3570 0.029 Uiso 1 1 calc R . . H22B H 0.7331 0.4374 0.3036 0.029 Uiso 1 1 calc R . . C23 C 0.6558(4) 0.5611(3) 0.2198(3) 0.0197(9) Uani 1 1 d U . . C24 C 0.6046(4) 0.4878(3) 0.2083(3) 0.0253(10) Uani 1 1 d U . . H24 H 0.6144 0.4346 0.2383 0.030 Uiso 1 1 calc R . . C25 C 0.5387(4) 0.4942(3) 0.1520(3) 0.0267(10) Uani 1 1 d U . . H25 H 0.5022 0.4454 0.1448 0.032 Uiso 1 1 calc R . . C26 C 0.5268(4) 0.5697(3) 0.1078(3) 0.0253(10) Uani 1 1 d U . . H26 H 0.4825 0.5724 0.0695 0.030 Uiso 1 1 calc R . . C27 C 0.5782(4) 0.6448(3) 0.1168(3) 0.0223(9) Uani 1 1 d U . . C28 C 0.6422(4) 0.6395(3) 0.1757(3) 0.0207(9) Uani 1 1 d U . . C29 C 0.5624(4) 0.7205(3) 0.0638(3) 0.0231(10) Uani 1 1 d U . . H29 H 0.5205 0.7160 0.0246 0.028 Uiso 1 1 calc R . . C30 C 0.5908(4) 0.8670(3) 0.0064(3) 0.0294(13) Uani 1 1 d . . . H30A H 0.5196 0.8662 -0.0067 0.035 Uiso 1 1 calc R . . H30B H 0.6502 0.8625 -0.0480 0.035 Uiso 1 1 calc R . . C31 C 0.5971(4) 0.9499(4) 0.0470(3) 0.0324(14) Uani 1 1 d . . . H31A H 0.6228 0.9958 0.0016 0.039 Uiso 1 1 calc R . . H31B H 0.5235 0.9684 0.0831 0.039 Uiso 1 1 calc R . . C32 C 0.7107(4) 1.0001(3) 0.1271(3) 0.0202(12) Uani 1 1 d . . . H32 H 0.6938 1.0563 0.1061 0.024 Uiso 1 1 calc R . . C33 C 0.7757(4) 0.9924(3) 0.1870(3) 0.0170(11) Uani 1 1 d . . . C34 C 0.8045(4) 1.0702(3) 0.2115(3) 0.0216(12) Uani 1 1 d . . . H34 H 0.7820 1.1237 0.1882 0.026 Uiso 1 1 calc R . . C35 C 0.8657(4) 1.0686(3) 0.2696(3) 0.0246(12) Uani 1 1 d . . . H35 H 0.8868 1.1212 0.2846 0.029 Uiso 1 1 calc R . . C36 C 0.8968(4) 0.9912(3) 0.3065(3) 0.0204(12) Uani 1 1 d . . . H36 H 0.9373 0.9912 0.3473 0.024 Uiso 1 1 calc R . . C37 C 0.8685(4) 0.9142(3) 0.2837(3) 0.0203(12) Uani 1 1 d . . . C38 C 0.8081(4) 0.9143(3) 0.2226(3) 0.0173(11) Uani 1 1 d . . . C39 C 0.9687(4) 0.8260(3) 0.3681(3) 0.0235(12) Uani 1 1 d . . . H39A H 0.9634 0.7686 0.3989 0.028 Uiso 1 1 calc R . . H39B H 0.9484 0.8700 0.4116 0.028 Uiso 1 1 calc R . . C40 C 1.0848(4) 0.8367(3) 0.3144(3) 0.0275(13) Uani 1 1 d . . . H40A H 1.1056 0.7927 0.2717 0.041 Uiso 1 1 calc R . . H40B H 1.1339 0.8302 0.3515 0.041 Uiso 1 1 calc R . . H40C H 1.0909 0.8940 0.2850 0.041 Uiso 1 1 calc R . . C41 C 0.4245(4) 0.6528(3) 0.3644(3) 0.0289(13) Uani 1 1 d . . . H41A H 0.5042 0.6419 0.3439 0.043 Uiso 1 1 calc R . . H41B H 0.3879 0.6008 0.3599 0.043 Uiso 1 1 calc R . . H41C H 0.4041 0.6681 0.4245 0.043 Uiso 1 1 calc R . . C42 C 0.3898(4) 0.7256(3) 0.3106(3) 0.0250(13) Uani 1 1 d . . . H42A H 0.4034 0.7089 0.2507 0.030 Uiso 1 1 calc R . . H42B H 0.3107 0.7411 0.3340 0.030 Uiso 1 1 calc R . . C43 C 0.4248(4) 0.8755(3) 0.2807(3) 0.0216(12) Uani 1 1 d . . . C44 C 0.3542(4) 0.8905(3) 0.2305(3) 0.0254(13) Uani 1 1 d . . . H44 H 0.3220 0.8434 0.2149 0.031 Uiso 1 1 calc R . . C45 C 0.3291(4) 0.9746(4) 0.2018(3) 0.0277(13) Uani 1 1 d . . . H45 H 0.2814 0.9844 0.1663 0.033 Uiso 1 1 calc R . . C46 C 0.3744(4) 1.0421(4) 0.2259(3) 0.0292(13) Uani 1 1 d . . . H46 H 0.3562 1.0992 0.2080 0.035 Uiso 1 1 calc R . . C47 C 0.4478(4) 1.0286(3) 0.2769(3) 0.0209(12) Uani 1 1 d . . . C48 C 0.4741(4) 0.9458(3) 0.3059(3) 0.0226(12) Uani 1 1 d . . . C49 C 0.4910(4) 1.1037(3) 0.3008(3) 0.0262(13) Uani 1 1 d . . . H49 H 0.4715 1.1585 0.2782 0.031 Uiso 1 1 calc R . . C50 C 0.5957(4) 1.1820(3) 0.3680(3) 0.0288(13) Uani 1 1 d . . . H50A H 0.5424 1.2308 0.3659 0.035 Uiso 1 1 calc R . . H50B H 0.6658 1.1942 0.3243 0.035 Uiso 1 1 calc R . . C51 C 0.6131(4) 1.1709(3) 0.4553(3) 0.0317(14) Uani 1 1 d . . . H51A H 0.6646 1.2133 0.4609 0.038 Uiso 1 1 calc R . . H51B H 0.5425 1.1808 0.4998 0.038 Uiso 1 1 calc R . . C52 C 0.7312(4) 1.0666(3) 0.5074(3) 0.0247(13) Uani 1 1 d . . . H52 H 0.7616 1.1146 0.5232 0.030 Uiso 1 1 calc R . . C53 C 0.7712(4) 0.9832(3) 0.5304(3) 0.0216(12) Uani 1 1 d . . . C54 C 0.8533(4) 0.9786(3) 0.5729(3) 0.0282(13) Uani 1 1 d . . . H54 H 0.8845 1.0302 0.5799 0.034 Uiso 1 1 calc R . . C55 C 0.8897(4) 0.9024(4) 0.6042(3) 0.0301(13) Uani 1 1 d . . . H55 H 0.9467 0.9010 0.6313 0.036 Uiso 1 1 calc R . . C56 C 0.8429(4) 0.8265(3) 0.5963(3) 0.0269(13) Uani 1 1 d . . . H56 H 0.8663 0.7732 0.6193 0.032 Uiso 1 1 calc R . . C57 C 0.7612(4) 0.8297(3) 0.5544(3) 0.0206(12) Uani 1 1 d . . . C58 C 0.7270(4) 0.9061(3) 0.5163(3) 0.0182(11) Uani 1 1 d . . . C59 C 0.7112(4) 0.6868(4) 0.6092(4) 0.0342(14) Uani 1 1 d . . . H59A H 0.6861 0.7091 0.6675 0.041 Uiso 1 1 calc R . . H59B H 0.7866 0.6610 0.6005 0.041 Uiso 1 1 calc R . . C60 C 0.6361(4) 0.6197(4) 0.6012(4) 0.0451(17) Uani 1 1 d . . . H60A H 0.5655 0.6475 0.5990 0.068 Uiso 1 1 calc R . . H60B H 0.6247 0.5784 0.6510 0.068 Uiso 1 1 calc R . . H60C H 0.6693 0.5894 0.5485 0.068 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 0.0206(3) 0.0217(4) 0.0257(4) -0.0039(3) -0.0134(3) -0.0110(3) Cu2 0.0197(3) 0.0193(4) 0.0270(4) -0.0042(3) -0.0158(3) -0.0052(3) Cu3 0.0224(4) 0.0174(4) 0.0283(4) -0.0045(3) -0.0092(3) -0.0079(3) Mg1 0.0168(9) 0.0159(10) 0.0249(9) -0.0045(8) -0.0124(7) -0.0049(7) O1 0.033(2) 0.018(2) 0.030(2) -0.0005(16) -0.0219(16) -0.0124(16) O2 0.030(2) 0.018(2) 0.030(2) -0.0029(17) -0.0198(16) -0.0116(16) O3 0.0260(19) 0.015(2) 0.029(2) -0.0039(16) -0.0157(16) -0.0056(15) O4 0.036(2) 0.018(2) 0.031(2) -0.0030(17) -0.0159(17) -0.0125(17) O5 0.0189(19) 0.015(2) 0.037(2) -0.0029(18) -0.0140(17) -0.0027(15) O6 0.0263(19) 0.020(2) 0.028(2) -0.0031(16) -0.0188(16) -0.0087(15) O7 0.0171(18) 0.016(2) 0.030(2) -0.0049(16) -0.0150(15) -0.0067(15) O8 0.0232(18) 0.0086(19) 0.0288(19) -0.0025(15) -0.0186(15) -0.0048(15) O9 0.0225(18) 0.017(2) 0.033(2) 0.0001(16) -0.0212(16) -0.0087(15) O10 0.058(2) 0.050(2) 0.063(2) 0.0060(18) -0.0412(18) -0.0206(18) O11 0.024(2) 0.032(2) 0.033(2) -0.0104(18) -0.0141(17) -0.0100(17) O12 0.0220(19) 0.017(2) 0.045(2) -0.0005(18) -0.0191(17) -0.0100(16) O13 0.027(2) 0.021(2) 0.032(2) -0.0064(17) -0.0173(17) -0.0063(16) O14 0.0235(19) 0.019(2) 0.031(2) -0.0075(17) -0.0141(16) -0.0069(16) O15 0.043(2) 0.015(2) 0.044(2) 0.0032(18) -0.0315(18) -0.0125(17) O16 0.079(2) 0.058(3) 0.057(2) -0.001(2) -0.0254(19) -0.027(2) O17 0.027(2) 0.054(3) 0.058(3) 0.006(2) -0.014(2) 0.000(2) O18 0.033(2) 0.038(3) 0.046(2) 0.000(2) -0.0216(19) -0.0071(19) O19 0.060(2) 0.077(3) 0.061(2) 0.012(2) -0.0355(19) -0.028(2) O20 0.048(3) 0.059(3) 0.075(3) -0.017(3) -0.037(2) 0.004(2) O21 0.051(3) 0.082(4) 0.067(3) -0.019(3) -0.020(3) -0.018(3) O22 0.071(2) 0.059(3) 0.074(2) 0.000(2) -0.049(2) 0.0002(19) N1 0.020(2) 0.023(3) 0.023(2) -0.004(2) -0.0092(18) -0.0122(19) N2 0.016(2) 0.029(3) 0.031(3) -0.010(2) -0.0111(19) -0.009(2) N3 0.024(2) 0.020(3) 0.021(2) -0.002(2) -0.0141(18) -0.0026(19) N4 0.014(2) 0.024(3) 0.026(2) 0.000(2) -0.0123(18) -0.0042(19) N5 0.026(2) 0.014(3) 0.035(3) -0.004(2) -0.011(2) -0.0103(19) N6 0.025(2) 0.025(3) 0.029(3) -0.013(2) -0.007(2) -0.006(2) N7 0.064(4) 0.028(3) 0.027(3) 0.006(2) -0.022(3) -0.020(3) N8 0.051(4) 0.037(3) 0.042(3) 0.008(3) -0.033(3) -0.025(3) C1 0.051(4) 0.028(4) 0.038(3) -0.009(3) -0.028(3) -0.014(3) C2 0.035(3) 0.027(3) 0.028(3) -0.001(3) -0.023(3) -0.009(3) C3 0.025(3) 0.013(3) 0.028(3) -0.005(2) -0.013(2) -0.008(2) C4 0.026(3) 0.017(3) 0.029(3) -0.006(2) -0.012(2) -0.002(2) C5 0.034(3) 0.013(3) 0.026(3) 0.001(2) -0.010(2) -0.002(2) C6 0.039(3) 0.014(3) 0.031(3) -0.007(3) -0.010(3) -0.009(2) C7 0.024(3) 0.013(3) 0.024(3) -0.008(2) -0.006(2) -0.009(2) C8 0.022(3) 0.011(3) 0.018(3) -0.002(2) -0.010(2) -0.001(2) C9 0.019(3) 0.018(3) 0.035(3) -0.009(3) -0.006(2) -0.011(2) C10 0.027(2) 0.034(3) 0.025(2) -0.009(2) -0.011(2) -0.016(2) C11 0.028(3) 0.035(3) 0.022(2) -0.009(2) -0.011(2) -0.014(2) C12 0.018(3) 0.033(4) 0.026(3) -0.010(3) -0.012(2) -0.005(2) C13 0.022(3) 0.024(3) 0.022(3) -0.009(2) -0.010(2) 0.003(2) C14 0.031(3) 0.033(4) 0.035(3) -0.012(3) -0.018(3) 0.011(3) C15 0.033(3) 0.031(4) 0.033(3) -0.006(3) -0.008(3) 0.007(3) C16 0.035(3) 0.019(3) 0.029(3) -0.005(3) -0.009(3) -0.002(2) C17 0.020(3) 0.019(3) 0.022(3) -0.004(2) -0.004(2) -0.002(2) C18 0.016(3) 0.016(3) 0.026(3) -0.005(2) -0.007(2) -0.002(2) C19 0.037(3) 0.022(3) 0.033(3) -0.006(3) -0.006(3) -0.012(3) C20 0.053(4) 0.030(4) 0.050(4) -0.005(3) -0.025(3) -0.019(3) C21 0.034(3) 0.037(4) 0.035(3) 0.003(3) -0.014(3) -0.009(3) C22 0.022(3) 0.019(3) 0.036(3) -0.001(3) -0.013(2) -0.005(2) C23 0.0154(18) 0.024(2) 0.024(2) -0.0124(17) -0.0075(16) -0.0065(17) C24 0.0216(19) 0.027(2) 0.030(2) -0.0101(18) -0.0071(17) -0.0093(17) C25 0.0224(19) 0.030(2) 0.033(2) -0.0120(18) -0.0116(17) -0.0113(18) C26 0.0194(19) 0.030(2) 0.034(2) -0.0136(18) -0.0136(17) -0.0080(18) C27 0.0156(17) 0.026(2) 0.0307(19) -0.0132(16) -0.0111(15) -0.0049(16) C28 0.0146(18) 0.024(2) 0.027(2) -0.0129(17) -0.0079(16) -0.0051(17) C29 0.016(2) 0.030(3) 0.030(2) -0.014(2) -0.0150(18) -0.001(2) C30 0.033(3) 0.033(4) 0.031(3) -0.002(3) -0.021(3) -0.005(3) C31 0.032(3) 0.034(4) 0.042(4) -0.001(3) -0.027(3) -0.004(3) C32 0.017(3) 0.021(3) 0.022(3) -0.003(2) -0.004(2) -0.001(2) C33 0.014(3) 0.018(3) 0.020(3) -0.006(2) -0.005(2) -0.001(2) C34 0.028(3) 0.011(3) 0.027(3) -0.001(2) -0.010(2) -0.001(2) C35 0.027(3) 0.021(3) 0.032(3) -0.008(3) -0.015(2) -0.007(2) C36 0.018(3) 0.021(3) 0.028(3) -0.009(2) -0.013(2) -0.004(2) C37 0.020(3) 0.016(3) 0.029(3) -0.008(2) -0.011(2) -0.002(2) C38 0.015(3) 0.015(3) 0.024(3) -0.008(2) -0.007(2) -0.004(2) C39 0.023(3) 0.028(3) 0.026(3) -0.006(2) -0.016(2) -0.008(2) C40 0.027(3) 0.028(3) 0.036(3) -0.010(3) -0.020(2) 0.000(2) C41 0.024(3) 0.018(3) 0.045(4) -0.005(3) -0.009(3) -0.007(2) C42 0.019(3) 0.024(3) 0.036(3) -0.008(3) -0.011(2) -0.008(2) C43 0.016(3) 0.020(3) 0.029(3) -0.004(2) -0.006(2) -0.007(2) C44 0.015(3) 0.028(3) 0.036(3) -0.004(3) -0.011(2) -0.005(2) C45 0.021(3) 0.035(4) 0.032(3) -0.009(3) -0.013(2) -0.001(3) C46 0.025(3) 0.026(3) 0.038(3) -0.001(3) -0.012(3) 0.003(3) C47 0.019(3) 0.016(3) 0.029(3) -0.005(2) -0.007(2) -0.003(2) C48 0.014(3) 0.028(3) 0.023(3) 0.000(2) 0.000(2) -0.003(2) C49 0.024(3) 0.021(3) 0.031(3) -0.002(3) -0.004(2) 0.003(2) C50 0.033(3) 0.016(3) 0.038(3) -0.011(3) -0.008(3) -0.003(2) C51 0.038(3) 0.020(3) 0.038(3) -0.011(3) -0.007(3) -0.007(3) C52 0.032(3) 0.018(3) 0.024(3) -0.006(2) -0.003(2) -0.016(2) C53 0.025(3) 0.020(3) 0.021(3) -0.006(2) -0.003(2) -0.014(2) C54 0.038(3) 0.025(3) 0.028(3) -0.009(3) -0.015(3) -0.017(3) C55 0.032(3) 0.034(4) 0.033(3) -0.006(3) -0.018(3) -0.016(3) C56 0.036(3) 0.027(3) 0.026(3) -0.004(3) -0.020(2) -0.010(3) C57 0.023(3) 0.014(3) 0.029(3) -0.009(2) -0.010(2) -0.008(2) C58 0.020(3) 0.014(3) 0.022(3) -0.008(2) -0.006(2) -0.004(2) C59 0.041(3) 0.025(4) 0.044(4) -0.003(3) -0.023(3) -0.010(3) C60 0.034(3) 0.034(4) 0.073(5) -0.009(3) -0.021(3) -0.012(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 O3 1.901(3) . ? Cu1 N1 1.932(4) . ? Cu1 O2 1.936(3) . ? Cu1 N2 1.961(4) . ? Cu2 O8 1.891(3) . ? Cu2 O7 1.897(3) . ? Cu2 N3 1.907(4) . ? Cu2 N4 1.913(4) . ? Cu2 Mg1 3.0998(17) . ? Cu3 O13 1.898(3) . ? Cu3 N6 1.924(4) . ? Cu3 O14 1.927(3) . ? Cu3 N5 1.945(4) . ? Mg1 O10 2.023(4) . ? Mg1 O5 2.031(4) . ? Mg1 O11 2.058(4) . ? Mg1 O8 2.088(3) . ? Mg1 O7 2.092(3) . ? Mg1 O9 2.542(3) . ? Mg1 O6 2.632(4) . ? O1 C3 1.383(6) . ? O1 C2 1.436(5) . ? O2 C8 1.312(5) . ? O3 C18 1.293(6) . ? O4 C17 1.370(5) . ? O4 C19 1.437(6) . ? O5 H5A 0.836(18) . ? O5 H5B 0.842(18) . ? O6 C23 1.385(5) . ? O6 C22 1.442(6) . ? O7 C28 1.325(5) . ? O8 C38 1.326(5) . ? O9 C37 1.368(6) . ? O9 C39 1.449(5) . ? O11 H11C 0.828(18) . ? O11 H11D 0.841(19) . ? O12 C43 1.363(6) . ? O12 C42 1.434(6) . ? O13 C48 1.312(5) . ? O14 C58 1.337(5) . ? O15 C57 1.388(6) . ? O15 C59 1.437(6) . ? O16 N7 1.243(6) . ? O17 N7 1.236(6) . ? O18 N7 1.254(5) . ? O19 N8 1.249(5) . ? O20 N8 1.243(5) . ? O21 N8 1.230(6) . ? N1 C9 1.256(6) . ? N1 C10 1.479(6) . ? N2 C12 1.295(6) . ? N2 C11 1.464(6) . ? N3 C29 1.290(6) . ? N3 C30 1.475(6) . ? N4 C32 1.289(6) . ? N4 C31 1.477(6) . ? N5 C49 1.280(6) . ? N5 C50 1.484(6) . ? N6 C52 1.279(6) . ? N6 C51 1.473(6) . ? C1 C2 1.512(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.368(7) . ? C3 C8 1.427(6) . ? C4 C5 1.397(7) . ? C4 H4 0.9500 . ? C5 C6 1.375(6) . ? C5 H5 0.9500 . ? C6 C7 1.406(7) . ? C6 H6 0.9500 . ? C7 C8 1.418(6) . ? C7 C9 1.455(7) . ? C9 H9 0.9500 . ? C10 C11 1.526(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.434(7) . ? C12 H12 0.9500 . ? C13 C14 1.395(7) . ? C13 C18 1.436(6) . ? C14 C15 1.380(8) . ? C14 H14 0.9500 . ? C15 C16 1.409(7) . ? C15 H15 0.9500 . ? C16 C17 1.377(7) . ? C16 H16 0.9500 . ? C17 C18 1.432(7) . ? C19 C20 1.500(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.513(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.396(7) . ? C23 C24 1.404(7) . ? C24 C25 1.403(6) . ? C24 H24 0.9500 . ? C25 C26 1.356(7) . ? C25 H25 0.9500 . ? C26 C27 1.417(7) . ? C26 H26 0.9500 . ? C27 C28 1.419(6) . ? C27 C29 1.448(7) . ? C29 H29 0.9500 . ? C30 C31 1.510(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.442(6) . ? C32 H32 0.9500 . ? C33 C38 1.397(7) . ? C33 C34 1.408(7) . ? C34 C35 1.385(6) . ? C34 H34 0.9500 . ? C35 C36 1.391(7) . ? C35 H35 0.9500 . ? C36 C37 1.382(7) . ? C36 H36 0.9500 . ? C37 C38 1.420(6) . ? C39 C40 1.502(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.502(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.376(6) . ? C43 C48 1.439(7) . ? C44 C45 1.405(7) . ? C44 H44 0.9500 . ? C45 C46 1.367(7) . ? C45 H45 0.9500 . ? C46 C47 1.414(7) . ? C46 H46 0.9500 . ? C47 C48 1.393(7) . ? C47 C49 1.450(7) . ? C49 H49 0.9500 . ? C50 C51 1.494(7) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.426(7) . ? C52 H52 0.9500 . ? C53 C54 1.403(7) . ? C53 C58 1.424(6) . ? C54 C55 1.361(7) . ? C54 H54 0.9500 . ? C55 C56 1.392(7) . ? C55 H55 0.9500 . ? C56 C57 1.393(6) . ? C56 H56 0.9500 . ? C57 C58 1.402(7) . ? C59 C60 1.502(7) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 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 O3 Cu1 N1 176.04(15) . . ? O3 Cu1 O2 90.47(14) . . ? N1 Cu1 O2 92.35(15) . . ? O3 Cu1 N2 92.53(16) . . ? N1 Cu1 N2 84.56(18) . . ? O2 Cu1 N2 176.46(16) . . ? O8 Cu2 O7 82.39(13) . . ? O8 Cu2 N3 175.20(15) . . ? O7 Cu2 N3 96.43(15) . . ? O8 Cu2 N4 95.79(15) . . ? O7 Cu2 N4 172.49(15) . . ? N3 Cu2 N4 85.98(17) . . ? O8 Cu2 Mg1 41.16(10) . . ? O7 Cu2 Mg1 41.35(9) . . ? N3 Cu2 Mg1 137.77(13) . . ? N4 Cu2 Mg1 135.93(12) . . ? O13 Cu3 N6 176.57(16) . . ? O13 Cu3 O14 89.90(14) . . ? N6 Cu3 O14 93.04(16) . . ? O13 Cu3 N5 92.15(16) . . ? N6 Cu3 N5 84.93(18) . . ? O14 Cu3 N5 177.83(16) . . ? O10 Mg1 O5 96.77(16) . . ? O10 Mg1 O11 81.19(16) . . ? O5 Mg1 O11 176.49(16) . . ? O10 Mg1 O8 142.54(17) . . ? O5 Mg1 O8 90.99(14) . . ? O11 Mg1 O8 88.95(15) . . ? O10 Mg1 O7 142.51(17) . . ? O5 Mg1 O7 91.69(14) . . ? O11 Mg1 O7 91.65(13) . . ? O8 Mg1 O7 73.29(13) . . ? O10 Mg1 O9 76.98(15) . . ? O5 Mg1 O9 90.84(13) . . ? O11 Mg1 O9 85.92(13) . . ? O8 Mg1 O9 66.28(12) . . ? O7 Mg1 O9 139.53(14) . . ? O10 Mg1 O6 79.64(15) . . ? O5 Mg1 O6 85.79(13) . . ? O11 Mg1 O6 96.61(14) . . ? O8 Mg1 O6 137.62(13) . . ? O7 Mg1 O6 64.60(12) . . ? O9 Mg1 O6 155.81(12) . . ? O10 Mg1 Cu2 169.45(14) . . ? O5 Mg1 Cu2 93.78(11) . . ? O11 Mg1 Cu2 88.26(11) . . ? O8 Mg1 Cu2 36.59(8) . . ? O7 Mg1 Cu2 36.80(9) . . ? O9 Mg1 Cu2 102.73(9) . . ? O6 Mg1 Cu2 101.40(8) . . ? C3 O1 C2 116.7(4) . . ? C8 O2 Cu1 125.5(3) . . ? C18 O3 Cu1 126.7(3) . . ? C17 O4 C19 117.4(4) . . ? Mg1 O5 H5A 117(3) . . ? Mg1 O5 H5B 116(2) . . ? H5A O5 H5B 116(4) . . ? C23 O6 C22 118.8(4) . . ? C23 O6 Mg1 111.3(3) . . ? C22 O6 Mg1 128.9(3) . . ? C28 O7 Cu2 125.1(3) . . ? C28 O7 Mg1 133.0(3) . . ? Cu2 O7 Mg1 101.85(15) . . ? C38 O8 Cu2 124.6(3) . . ? C38 O8 Mg1 129.1(3) . . ? Cu2 O8 Mg1 102.25(15) . . ? C37 O9 C39 118.8(4) . . ? C37 O9 Mg1 111.4(3) . . ? C39 O9 Mg1 129.8(3) . . ? Mg1 O11 H11C 117(3) . . ? Mg1 O11 H11D 117(3) . . ? H11C O11 H11D 113(4) . . ? C43 O12 C42 118.0(4) . . ? C48 O13 Cu3 126.4(3) . . ? C58 O14 Cu3 125.9(3) . . ? C57 O15 C59 116.1(4) . . ? C9 N1 C10 121.2(4) . . ? C9 N1 Cu1 127.0(4) . . ? C10 N1 Cu1 111.8(3) . . ? C12 N2 C11 121.0(4) . . ? C12 N2 Cu1 126.1(4) . . ? C11 N2 Cu1 112.9(3) . . ? C29 N3 C30 121.4(4) . . ? C29 N3 Cu2 125.6(4) . . ? C30 N3 Cu2 112.7(3) . . ? C32 N4 C31 120.8(4) . . ? C32 N4 Cu2 125.2(4) . . ? C31 N4 Cu2 113.1(3) . . ? C49 N5 C50 119.8(4) . . ? C49 N5 Cu3 127.8(4) . . ? C50 N5 Cu3 112.5(3) . . ? C52 N6 C51 122.1(4) . . ? C52 N6 Cu3 125.6(4) . . ? C51 N6 Cu3 112.1(3) . . ? O17 N7 O16 120.7(5) . . ? O17 N7 O18 120.4(5) . . ? O16 N7 O18 118.9(5) . . ? O21 N8 O20 120.8(5) . . ? O21 N8 O19 119.7(5) . . ? O20 N8 O19 119.4(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 107.1(4) . . ? O1 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O1 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C4 C3 O1 123.5(4) . . ? C4 C3 C8 123.0(5) . . ? O1 C3 C8 113.5(4) . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.0(5) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 122.1(5) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C6 C7 C8 119.8(5) . . ? C6 C7 C9 118.5(4) . . ? C8 C7 C9 121.6(5) . . ? O2 C8 C7 125.0(4) . . ? O2 C8 C3 118.8(4) . . ? C7 C8 C3 116.2(4) . . ? N1 C9 C7 125.7(5) . . ? N1 C9 H9 117.2 . . ? C7 C9 H9 117.2 . . ? N1 C10 C11 107.6(4) . . ? N1 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? N1 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? N2 C11 C10 107.9(4) . . ? N2 C11 H11A 110.1 . . ? C10 C11 H11A 110.1 . . ? N2 C11 H11B 110.1 . . ? C10 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? N2 C12 C13 125.9(5) . . ? N2 C12 H12 117.0 . . ? C13 C12 H12 117.0 . . ? C14 C13 C12 117.7(5) . . ? C14 C13 C18 121.8(5) . . ? C12 C13 C18 120.5(5) . . ? C15 C14 C13 121.4(5) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 118.4(5) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 121.2(5) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? O4 C17 C16 125.6(5) . . ? O4 C17 C18 112.2(4) . . ? C16 C17 C18 122.2(5) . . ? O3 C18 C17 118.3(4) . . ? O3 C18 C13 126.7(5) . . ? C17 C18 C13 115.0(4) . . ? O4 C19 C20 107.1(4) . . ? O4 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O4 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 C21 112.7(4) . . ? O6 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? O6 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? O6 C23 C28 114.5(4) . . ? O6 C23 C24 124.6(5) . . ? C28 C23 C24 120.9(5) . . ? C23 C24 C25 119.0(5) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 120.3(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 122.3(5) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C28 C27 C26 117.7(5) . . ? C28 C27 C29 125.3(5) . . ? C26 C27 C29 117.0(4) . . ? O7 C28 C23 116.7(4) . . ? O7 C28 C27 123.7(5) . . ? C23 C28 C27 119.7(5) . . ? N3 C29 C27 123.8(4) . . ? N3 C29 H29 118.1 . . ? C27 C29 H29 118.1 . . ? N3 C30 C31 108.9(4) . . ? N3 C30 H30A 109.9 . . ? C31 C30 H30A 109.9 . . ? N3 C30 H30B 109.9 . . ? C31 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? N4 C31 C30 109.1(4) . . ? N4 C31 H31A 109.9 . . ? C30 C31 H31A 109.9 . . ? N4 C31 H31B 109.9 . . ? C30 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? N4 C32 C33 124.4(5) . . ? N4 C32 H32 117.8 . . ? C33 C32 H32 117.8 . . ? C38 C33 C34 119.5(4) . . ? C38 C33 C32 124.4(5) . . ? C34 C33 C32 116.1(4) . . ? C35 C34 C33 119.8(5) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 121.1(5) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C37 C36 C35 119.9(5) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? O9 C37 C36 125.3(4) . . ? O9 C37 C38 114.7(4) . . ? C36 C37 C38 119.9(5) . . ? O8 C38 C33 124.9(4) . . ? O8 C38 C37 115.3(4) . . ? C33 C38 C37 119.8(4) . . ? O9 C39 C40 112.2(4) . . ? O9 C39 H39A 109.2 . . ? C40 C39 H39A 109.2 . . ? O9 C39 H39B 109.2 . . ? C40 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O12 C42 C41 106.9(4) . . ? O12 C42 H42A 110.3 . . ? C41 C42 H42A 110.3 . . ? O12 C42 H42B 110.3 . . ? C41 C42 H42B 110.3 . . ? H42A C42 H42B 108.6 . . ? O12 C43 C44 125.9(5) . . ? O12 C43 C48 113.3(4) . . ? C44 C43 C48 120.7(5) . . ? C43 C44 C45 120.9(5) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 119.1(5) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C45 C46 C47 121.2(5) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C48 C47 C46 120.7(5) . . ? C48 C47 C49 121.4(5) . . ? C46 C47 C49 117.8(5) . . ? O13 C48 C47 126.9(5) . . ? O13 C48 C43 115.8(5) . . ? C47 C48 C43 117.4(5) . . ? N5 C49 C47 124.4(5) . . ? N5 C49 H49 117.8 . . ? C47 C49 H49 117.8 . . ? N5 C50 C51 108.1(4) . . ? N5 C50 H50A 110.1 . . ? C51 C50 H50A 110.1 . . ? N5 C50 H50B 110.1 . . ? C51 C50 H50B 110.1 . . ? H50A C50 H50B 108.4 . . ? N6 C51 C50 109.0(4) . . ? N6 C51 H51A 109.9 . . ? C50 C51 H51A 109.9 . . ? N6 C51 H51B 109.9 . . ? C50 C51 H51B 109.9 . . ? H51A C51 H51B 108.3 . . ? N6 C52 C53 126.2(5) . . ? N6 C52 H52 116.9 . . ? C53 C52 H52 116.9 . . ? C54 C53 C58 119.6(5) . . ? C54 C53 C52 117.8(5) . . ? C58 C53 C52 122.5(5) . . ? C55 C54 C53 122.0(5) . . ? C55 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? C54 C55 C56 119.7(5) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C55 C56 C57 119.2(5) . . ? C55 C56 H56 120.4 . . ? C57 C56 H56 120.4 . . ? O15 C57 C56 121.5(4) . . ? O15 C57 C58 115.8(4) . . ? C56 C57 C58 122.7(5) . . ? O14 C58 C57 119.8(4) . . ? O14 C58 C53 123.8(4) . . ? C57 C58 C53 116.5(4) . . ? O15 C59 C60 109.3(4) . . ? O15 C59 H59A 109.8 . . ? C60 C59 H59A 109.8 . . ? O15 C59 H59B 109.8 . . ? C60 C59 H59B 109.8 . . ? H59A C59 H59B 108.3 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? 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 O5 H5A O1 0.836(18) 2.22(3) 2.994(5) 154(5) . O5 H5A O2 0.836(18) 2.26(4) 2.886(5) 132(4) . O5 H5B O3 0.842(18) 2.18(4) 2.846(5) 136(5) . O5 H5B O4 0.842(18) 2.35(3) 3.132(5) 155(5) . O11 H11C O12 0.828(18) 2.18(3) 2.940(4) 153(5) . O11 H11C O13 0.828(18) 2.17(4) 2.811(5) 134(5) . O11 H11D O14 0.841(19) 2.10(3) 2.816(5) 143(4) . O11 H11D O15 0.841(19) 2.43(3) 3.157(5) 145(5) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.349 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.095 #==== end data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H66 Cl Cu3 K2 N6 O16, C40 H44 Cu2 K N4 O8, 2(Cl O4)' _chemical_formula_sum 'C100 H110 Cl3 Cu5 K3 N10 O32' _chemical_formula_weight 2505.33 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' 'K' 'K' 0.2009 0.2494 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 21.4852(3) _cell_length_b 25.7356(3) _cell_length_c 18.6849(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.9020(10) _cell_angle_gamma 90.00 _cell_volume 10325.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 26835 _cell_measurement_theta_min 2.5501 _cell_measurement_theta_max 32.6483 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5156 _exptl_absorpt_coefficient_mu 1.299 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.93069 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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_measurement_method ? _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59985 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10549 _reflns_number_gt 8163 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0537P)^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 10549 _refine_ls_number_parameters 708 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.086 _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 0.367706(14) 0.117365(11) 0.811493(15) 0.01767(8) Uani 1 1 d . . . Cu2 Cu 0.234949(13) 0.161152(11) 0.715887(15) 0.01615(8) Uani 1 1 d . . . Cu3 Cu 0.0000 0.211785(17) 0.7500 0.02916(13) Uani 1 2 d S . . K1 K 0.5000 0.18030(3) 0.7500 0.02647(19) Uani 1 2 d S . . K2 K 0.10172(3) 0.09326(2) 0.79241(3) 0.02379(13) Uani 1 1 d . . . Cl1 Cl 0.0000 -0.03360(3) 0.7500 0.0320(2) Uani 1 2 d S . . Cl2 Cl 0.32702(3) 0.12090(2) 0.42008(3) 0.02646(15) Uani 1 1 d D . . O1 O 0.48321(8) 0.09914(6) 0.62053(9) 0.0238(4) Uani 1 1 d . . . O2 O 0.41969(8) 0.10106(6) 0.73543(9) 0.0188(4) Uani 1 1 d . . . O3 O 0.38486(8) 0.18862(6) 0.79396(9) 0.0208(4) Uani 1 1 d . . . O4 O 0.41758(8) 0.27707(6) 0.74258(9) 0.0228(4) Uani 1 1 d . . . O5 O 0.11040(8) 0.17983(6) 0.89945(9) 0.0211(4) Uani 1 1 d . . . O6 O 0.17732(8) 0.17772(6) 0.78702(9) 0.0198(4) Uani 1 1 d . . . O7 O 0.22557(8) 0.09042(6) 0.74196(9) 0.0189(4) Uani 1 1 d . . . O8 O 0.19477(8) 0.00048(6) 0.79141(9) 0.0224(4) Uani 1 1 d . . . O9 O -0.09183(8) 0.07538(7) 0.85137(9) 0.0250(4) Uani 1 1 d . . . O10 O -0.03904(8) 0.15863(6) 0.80365(10) 0.0268(4) Uani 1 1 d . . . O11 O 0.04277(11) -0.00106(9) 0.78915(14) 0.0589(7) Uani 1 1 d U . . O12 O 0.03257(10) -0.06567(8) 0.70112(12) 0.0463(6) Uani 1 1 d U . . O13A O 0.3800(2) 0.1420(2) 0.4592(4) 0.0947(18) Uani 0.52 1 d PDU A 1 O14A O 0.3140(2) 0.07004(8) 0.4475(2) 0.0440(8) Uani 0.52 1 d PDU A 1 O15A O 0.2802(2) 0.15985(17) 0.4310(5) 0.0576(14) Uani 0.52 1 d PDU A 1 O16A O 0.3257(5) 0.1141(5) 0.34350(11) 0.0395(15) Uani 0.52 1 d PDU A 1 O13B O 0.3879(2) 0.1129(3) 0.4526(5) 0.0947(18) Uani 0.48 1 d PDU A 2 O14B O 0.27929(17) 0.08711(16) 0.4464(3) 0.0440(8) Uani 0.48 1 d PDU A 2 O15B O 0.3071(3) 0.17254(12) 0.4379(5) 0.0576(14) Uani 0.48 1 d PDU A 2 O16B O 0.3441(5) 0.1228(6) 0.34622(17) 0.0395(15) Uani 0.48 1 d PDU A 2 N1 N 0.35563(9) 0.04617(8) 0.83837(11) 0.0208(5) Uani 1 1 d . . . N2 N 0.30926(10) 0.13400(9) 0.88502(11) 0.0237(5) Uani 1 1 d . . . N3 N 0.24780(9) 0.23285(8) 0.68929(11) 0.0183(4) Uani 1 1 d . . . N4 N 0.29572(9) 0.14595(8) 0.64556(11) 0.0178(4) Uani 1 1 d . . . N5 N -0.03058(12) 0.26727(9) 0.80949(16) 0.0392(7) Uani 1 1 d U . . C1 C 0.51527(14) 0.15665(12) 0.53114(15) 0.0363(7) Uani 1 1 d . . . H1A H 0.4759 0.1754 0.5351 0.054 Uiso 1 1 calc R . . H1B H 0.5295 0.1594 0.4820 0.054 Uiso 1 1 calc R . . H1C H 0.5466 0.1718 0.5643 0.054 Uiso 1 1 calc R . . C2 C 0.50584(12) 0.10097(11) 0.54941(14) 0.0260(6) Uani 1 1 d . . . H2A H 0.4753 0.0849 0.5153 0.031 Uiso 1 1 calc R . . H2B H 0.5456 0.0818 0.5470 0.031 Uiso 1 1 calc R . . C3 C 0.46439(11) 0.05171(10) 0.64538(13) 0.0208(5) Uani 1 1 d . . . C4 C 0.47695(12) 0.00447(10) 0.61452(14) 0.0255(6) Uani 1 1 d . . . H4 H 0.4999 0.0032 0.5719 0.031 Uiso 1 1 calc R . . C5 C 0.45620(13) -0.04182(10) 0.64541(16) 0.0302(6) Uani 1 1 d . . . H5 H 0.4651 -0.0743 0.6238 0.036 Uiso 1 1 calc R . . C6 C 0.42329(12) -0.04016(10) 0.70622(15) 0.0271(6) Uani 1 1 d . . . H6 H 0.4094 -0.0717 0.7267 0.033 Uiso 1 1 calc R . . C7 C 0.40921(11) 0.00746(9) 0.73969(14) 0.0208(5) Uani 1 1 d . . . C8 C 0.43003(11) 0.05474(9) 0.70928(13) 0.0177(5) Uani 1 1 d . . . C9 C 0.37362(12) 0.00619(10) 0.80361(14) 0.0244(6) Uani 1 1 d . . . H9 H 0.3625 -0.0270 0.8215 0.029 Uiso 1 1 calc R . . C10 C 0.32017(12) 0.04124(11) 0.90414(14) 0.0291(6) Uani 1 1 d . . . H10A H 0.3490 0.0410 0.9466 0.035 Uiso 1 1 calc R . . H10B H 0.2964 0.0083 0.9034 0.035 Uiso 1 1 calc R . . C11 C 0.27591(12) 0.08705(11) 0.90806(14) 0.0286(6) Uani 1 1 d . . . H11A H 0.2388 0.0810 0.8764 0.034 Uiso 1 1 calc R . . H11B H 0.2620 0.0915 0.9577 0.034 Uiso 1 1 calc R . . C12 C 0.29484(12) 0.17923(11) 0.90729(13) 0.0259(6) Uani 1 1 d . . . H12 H 0.2646 0.1811 0.9432 0.031 Uiso 1 1 calc R . . C13 C 0.32035(11) 0.22750(10) 0.88288(13) 0.0223(6) Uani 1 1 d . . . C14 C 0.29988(13) 0.27434(11) 0.91348(14) 0.0290(6) Uani 1 1 d . . . H14 H 0.2716 0.2731 0.9515 0.035 Uiso 1 1 calc R . . C15 C 0.31972(13) 0.32143(11) 0.88970(15) 0.0309(7) Uani 1 1 d . . . H15 H 0.3062 0.3524 0.9120 0.037 Uiso 1 1 calc R . . C16 C 0.36004(12) 0.32401(10) 0.83237(14) 0.0262(6) Uani 1 1 d . . . H16 H 0.3737 0.3568 0.8156 0.031 Uiso 1 1 calc R . . C17 C 0.37980(11) 0.27912(10) 0.80033(13) 0.0201(5) Uani 1 1 d . . . C18 C 0.36226(11) 0.22921(10) 0.82591(13) 0.0184(5) Uani 1 1 d . . . C19 C 0.42339(13) 0.32395(10) 0.70129(15) 0.0270(6) Uani 1 1 d . . . H19A H 0.4474 0.3503 0.7292 0.032 Uiso 1 1 calc R . . H19B H 0.3817 0.3384 0.6889 0.032 Uiso 1 1 calc R . . C20 C 0.45652(13) 0.31032(11) 0.63456(15) 0.0328(7) Uani 1 1 d . . . H20A H 0.4982 0.2972 0.6474 0.049 Uiso 1 1 calc R . . H20B H 0.4600 0.3413 0.6045 0.049 Uiso 1 1 calc R . . H20C H 0.4330 0.2835 0.6081 0.049 Uiso 1 1 calc R . . C21 C 0.05510(15) 0.12382(11) 0.97340(17) 0.0372(7) Uani 1 1 d . . . H21A H 0.0325 0.1090 0.9318 0.056 Uiso 1 1 calc R . . H21B H 0.0292 0.1215 1.0155 0.056 Uiso 1 1 calc R . . H21C H 0.0939 0.1045 0.9824 0.056 Uiso 1 1 calc R . . C22 C 0.06996(11) 0.17965(10) 0.95896(14) 0.0222(6) Uani 1 1 d . . . H22A H 0.0314 0.1994 0.9471 0.027 Uiso 1 1 calc R . . H22B H 0.0909 0.1957 1.0015 0.027 Uiso 1 1 calc R . . C23 C 0.13067(11) 0.22711(9) 0.87549(13) 0.0184(5) Uani 1 1 d . . . C24 C 0.11983(11) 0.27415(10) 0.90832(14) 0.0223(6) Uani 1 1 d . . . H24 H 0.0975 0.2752 0.9513 0.027 Uiso 1 1 calc R . . C25 C 0.14177(12) 0.32045(10) 0.87836(15) 0.0258(6) Uani 1 1 d . . . H25 H 0.1341 0.3527 0.9010 0.031 Uiso 1 1 calc R . . C26 C 0.17402(11) 0.31919(10) 0.81697(14) 0.0231(6) Uani 1 1 d . . . H26 H 0.1872 0.3508 0.7962 0.028 Uiso 1 1 calc R . . C27 C 0.18823(11) 0.27133(9) 0.78348(13) 0.0192(5) Uani 1 1 d . . . C28 C 0.16663(11) 0.22410(9) 0.81249(13) 0.0174(5) Uani 1 1 d . . . C29 C 0.22685(11) 0.27293(10) 0.72182(13) 0.0200(5) Uani 1 1 d . . . H29 H 0.2376 0.3062 0.7039 0.024 Uiso 1 1 calc R . . C30 C 0.28613(12) 0.23855(10) 0.62597(13) 0.0210(5) Uani 1 1 d . . . H30A H 0.3102 0.2713 0.6289 0.025 Uiso 1 1 calc R . . H30B H 0.2593 0.2394 0.5819 0.025 Uiso 1 1 calc R . . C31 C 0.33029(11) 0.19220(10) 0.62415(14) 0.0214(5) Uani 1 1 d . . . H31A H 0.3459 0.1876 0.5753 0.026 Uiso 1 1 calc R . . H31B H 0.3664 0.1980 0.6575 0.026 Uiso 1 1 calc R . . C32 C 0.30718(11) 0.10082(9) 0.61919(12) 0.0178(5) Uani 1 1 d . . . H32 H 0.3358 0.0990 0.5816 0.021 Uiso 1 1 calc R . . C33 C 0.27977(11) 0.05302(9) 0.64255(13) 0.0177(5) Uani 1 1 d . . . C34 C 0.29339(11) 0.00718(10) 0.60433(13) 0.0205(5) Uani 1 1 d . . . H34 H 0.3168 0.0093 0.5622 0.025 Uiso 1 1 calc R . . C35 C 0.27328(12) -0.04024(10) 0.62723(14) 0.0229(6) Uani 1 1 d . . . H35 H 0.2818 -0.0706 0.6003 0.027 Uiso 1 1 calc R . . C36 C 0.24033(12) -0.04412(9) 0.69001(14) 0.0208(5) Uani 1 1 d . . . H36 H 0.2275 -0.0772 0.7064 0.025 Uiso 1 1 calc R . . C37 C 0.22628(11) -0.00008(9) 0.72855(13) 0.0177(5) Uani 1 1 d . . . C38 C 0.24356(11) 0.05012(9) 0.70463(12) 0.0158(5) Uani 1 1 d . . . C39 C 0.17875(14) -0.04922(10) 0.82116(15) 0.0295(6) Uani 1 1 d . . . H39A H 0.2161 -0.0717 0.8251 0.035 Uiso 1 1 calc R . . H39B H 0.1471 -0.0667 0.7899 0.035 Uiso 1 1 calc R . . C40 C 0.15338(16) -0.03971(12) 0.89400(16) 0.0422(8) Uani 1 1 d . . . H40A H 0.1849 -0.0221 0.9243 0.063 Uiso 1 1 calc R . . H40B H 0.1426 -0.0730 0.9159 0.063 Uiso 1 1 calc R . . H40C H 0.1161 -0.0179 0.8894 0.063 Uiso 1 1 calc R . . C41 C -0.06172(13) 0.01431(11) 0.94481(15) 0.0305(6) Uani 1 1 d . . . H41A H -0.0202 0.0098 0.9255 0.046 Uiso 1 1 calc R . . H41B H -0.0743 -0.0179 0.9684 0.046 Uiso 1 1 calc R . . H41C H -0.0607 0.0428 0.9797 0.046 Uiso 1 1 calc R . . C42 C -0.10748(12) 0.02689(10) 0.88499(14) 0.0246(6) Uani 1 1 d . . . H42A H -0.1075 -0.0013 0.8490 0.030 Uiso 1 1 calc R . . H42B H -0.1498 0.0293 0.9040 0.030 Uiso 1 1 calc R . . C43 C -0.10617(12) 0.12077(10) 0.88571(14) 0.0256(5) Uani 1 1 d U . . C44 C -0.14576(13) 0.12447(12) 0.94148(15) 0.0316(6) Uani 1 1 d U . . H44 H -0.1649 0.0941 0.9594 0.038 Uiso 1 1 calc R . . C45 C -0.15823(14) 0.17300(13) 0.97230(17) 0.0402(7) Uani 1 1 d U . . H45 H -0.1852 0.1753 1.0114 0.048 Uiso 1 1 calc R . . C46 C -0.13177(14) 0.21640(12) 0.94621(17) 0.0418(7) Uani 1 1 d U . . H46 H -0.1403 0.2490 0.9676 0.050 Uiso 1 1 calc R . . C47 C -0.09149(13) 0.21425(11) 0.88759(17) 0.0342(6) Uani 1 1 d U . . C48 C -0.07698(12) 0.16553(10) 0.85677(15) 0.0275(6) Uani 1 1 d U . . C49 C -0.06686(14) 0.26253(11) 0.86178(19) 0.0407(7) Uani 1 1 d U . . H49 H -0.0786 0.2934 0.8857 0.049 Uiso 1 1 calc R . . C50 C -0.00616(16) 0.31906(11) 0.78945(19) 0.0497(9) Uani 1 1 d U . . H50A H 0.0328 0.3265 0.8173 0.060 Uiso 1 1 calc R . . H50B H -0.0369 0.3463 0.8003 0.060 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 0.02058(16) 0.01643(16) 0.01633(15) 0.00327(12) 0.00571(12) -0.00115(12) Cu2 0.01957(16) 0.01144(15) 0.01764(15) 0.00031(12) 0.00392(12) -0.00258(11) Cu3 0.0248(3) 0.0094(2) 0.0524(3) 0.000 -0.0129(2) 0.000 K1 0.0206(4) 0.0147(4) 0.0449(5) 0.000 0.0127(4) 0.000 K2 0.0341(3) 0.0147(3) 0.0230(3) -0.0015(2) 0.0071(2) -0.0038(2) Cl1 0.0277(5) 0.0117(4) 0.0574(7) 0.000 0.0132(5) 0.000 Cl2 0.0387(4) 0.0208(3) 0.0201(3) -0.0016(3) 0.0051(3) -0.0001(3) O1 0.0339(10) 0.0185(9) 0.0197(9) 0.0017(7) 0.0091(8) 0.0005(8) O2 0.0239(9) 0.0117(8) 0.0211(9) 0.0018(7) 0.0067(7) -0.0014(7) O3 0.0258(9) 0.0144(9) 0.0229(9) 0.0014(7) 0.0113(7) 0.0032(7) O4 0.0311(10) 0.0132(9) 0.0246(9) 0.0024(7) 0.0078(8) 0.0028(7) O5 0.0238(9) 0.0143(9) 0.0259(9) -0.0015(7) 0.0102(8) 0.0000(7) O6 0.0262(9) 0.0102(8) 0.0236(9) -0.0031(7) 0.0076(8) -0.0032(7) O7 0.0253(9) 0.0123(8) 0.0196(9) -0.0013(7) 0.0070(7) -0.0001(7) O8 0.0316(10) 0.0137(9) 0.0225(9) 0.0006(7) 0.0102(8) -0.0048(7) O9 0.0351(11) 0.0177(9) 0.0224(9) -0.0017(8) 0.0032(8) 0.0054(8) O10 0.0262(10) 0.0142(9) 0.0400(11) -0.0051(8) -0.0002(9) 0.0031(7) O11 0.0517(14) 0.0471(14) 0.0779(17) -0.0069(12) 0.0021(12) -0.0229(11) O12 0.0546(13) 0.0233(10) 0.0626(14) 0.0021(10) 0.0276(11) 0.0093(9) O13A 0.0351(19) 0.195(5) 0.054(2) 0.057(4) 0.0016(18) 0.044(3) O14A 0.0665(19) 0.0273(15) 0.0379(13) 0.0047(12) -0.0023(15) -0.0077(13) O15A 0.067(3) 0.055(2) 0.052(2) -0.001(2) 0.028(3) 0.016(2) O16A 0.083(5) 0.016(4) 0.0200(11) -0.0007(10) 0.0113(15) 0.005(3) O13B 0.0351(19) 0.195(5) 0.054(2) 0.057(4) 0.0016(18) 0.044(3) O14B 0.0665(19) 0.0273(15) 0.0379(13) 0.0047(12) -0.0023(15) -0.0077(13) O15B 0.067(3) 0.055(2) 0.052(2) -0.001(2) 0.028(3) 0.016(2) O16B 0.083(5) 0.016(4) 0.0200(11) -0.0007(10) 0.0113(15) 0.005(3) N1 0.0189(11) 0.0212(12) 0.0222(11) 0.0067(9) 0.0015(9) -0.0042(9) N2 0.0223(11) 0.0319(13) 0.0171(11) 0.0030(10) 0.0049(9) -0.0044(10) N3 0.0179(10) 0.0171(11) 0.0198(11) 0.0027(9) -0.0006(8) -0.0043(8) N4 0.0180(10) 0.0168(11) 0.0188(10) 0.0026(9) 0.0017(8) -0.0027(8) N5 0.0352(14) 0.0124(11) 0.0682(18) -0.0086(12) -0.0266(13) 0.0039(10) C1 0.0407(18) 0.0420(18) 0.0267(15) 0.0049(13) 0.0090(13) -0.0163(14) C2 0.0236(14) 0.0347(16) 0.0202(13) -0.0014(12) 0.0078(11) 0.0009(11) C3 0.0225(13) 0.0177(13) 0.0222(13) 0.0016(10) -0.0011(11) 0.0019(10) C4 0.0296(15) 0.0215(14) 0.0253(14) -0.0052(11) 0.0007(11) 0.0062(11) C5 0.0378(16) 0.0161(14) 0.0361(16) -0.0058(12) -0.0065(13) 0.0044(11) C6 0.0317(15) 0.0134(13) 0.0358(16) 0.0043(11) -0.0060(12) -0.0012(11) C7 0.0224(13) 0.0149(12) 0.0247(13) 0.0032(11) -0.0050(11) -0.0009(10) C8 0.0192(13) 0.0149(12) 0.0188(12) 0.0017(10) -0.0012(10) 0.0013(10) C9 0.0235(14) 0.0202(14) 0.0289(15) 0.0113(11) -0.0050(11) -0.0084(11) C10 0.0278(15) 0.0349(16) 0.0246(14) 0.0150(12) 0.0028(12) -0.0093(12) C11 0.0259(14) 0.0388(17) 0.0216(14) 0.0047(12) 0.0085(11) -0.0057(12) C12 0.0232(14) 0.0398(17) 0.0152(12) -0.0028(12) 0.0061(11) 0.0032(12) C13 0.0204(13) 0.0307(15) 0.0159(12) -0.0014(11) 0.0004(10) 0.0052(11) C14 0.0283(15) 0.0399(17) 0.0190(13) -0.0081(12) 0.0043(11) 0.0110(13) C15 0.0331(16) 0.0292(16) 0.0299(15) -0.0142(13) -0.0052(12) 0.0153(12) C16 0.0284(15) 0.0206(14) 0.0291(15) -0.0035(12) -0.0063(12) 0.0060(11) C17 0.0216(13) 0.0197(13) 0.0189(13) -0.0025(10) -0.0020(10) 0.0059(10) C18 0.0176(12) 0.0213(13) 0.0161(12) -0.0007(10) -0.0005(10) 0.0059(10) C19 0.0323(15) 0.0133(13) 0.0353(16) 0.0060(11) -0.0033(12) -0.0035(11) C20 0.0318(16) 0.0342(17) 0.0326(16) 0.0122(13) 0.0029(13) -0.0067(13) C21 0.0443(18) 0.0299(16) 0.0388(17) -0.0010(13) 0.0231(15) -0.0083(13) C22 0.0190(13) 0.0231(14) 0.0249(14) -0.0057(11) 0.0064(11) -0.0002(10) C23 0.0158(12) 0.0149(12) 0.0243(13) -0.0020(10) -0.0007(10) 0.0010(9) C24 0.0199(13) 0.0191(13) 0.0281(14) -0.0036(11) 0.0037(11) 0.0032(10) C25 0.0248(14) 0.0133(13) 0.0394(16) -0.0056(12) 0.0003(12) 0.0035(10) C26 0.0224(13) 0.0122(12) 0.0345(15) 0.0007(11) -0.0028(11) -0.0001(10) C27 0.0182(13) 0.0160(12) 0.0233(13) 0.0000(10) -0.0033(10) -0.0003(10) C28 0.0158(12) 0.0160(12) 0.0203(12) -0.0024(10) -0.0023(10) 0.0005(9) C29 0.0187(13) 0.0155(13) 0.0253(13) 0.0020(11) -0.0052(10) -0.0033(10) C30 0.0230(13) 0.0174(13) 0.0227(13) 0.0044(11) 0.0026(11) -0.0055(10) C31 0.0209(13) 0.0219(14) 0.0216(13) 0.0023(11) 0.0046(10) -0.0053(10) C32 0.0175(12) 0.0219(13) 0.0141(12) 0.0011(10) 0.0007(10) -0.0016(10) C33 0.0171(12) 0.0192(13) 0.0166(12) -0.0003(10) -0.0005(10) 0.0021(10) C34 0.0213(13) 0.0226(13) 0.0177(12) -0.0025(10) 0.0031(10) 0.0027(10) C35 0.0267(14) 0.0197(13) 0.0222(13) -0.0085(11) 0.0010(11) 0.0049(11) C36 0.0253(13) 0.0129(12) 0.0240(13) 0.0011(10) -0.0007(11) 0.0005(10) C37 0.0186(12) 0.0172(13) 0.0175(12) -0.0009(10) 0.0028(10) 0.0006(10) C38 0.0166(12) 0.0149(12) 0.0159(12) -0.0013(10) -0.0011(9) -0.0001(9) C39 0.0448(17) 0.0155(13) 0.0287(15) 0.0045(11) 0.0094(13) -0.0050(12) C40 0.061(2) 0.0350(18) 0.0320(17) 0.0054(14) 0.0193(16) -0.0150(15) C41 0.0263(15) 0.0314(16) 0.0336(16) 0.0086(13) -0.0029(12) -0.0042(12) C42 0.0249(14) 0.0232(14) 0.0259(14) -0.0002(11) 0.0033(11) -0.0023(11) C43 0.0244(12) 0.0270(13) 0.0250(12) -0.0084(10) -0.0064(10) 0.0096(10) C44 0.0289(13) 0.0384(14) 0.0270(13) -0.0087(11) -0.0070(11) 0.0111(11) C45 0.0340(14) 0.0501(16) 0.0359(14) -0.0181(13) -0.0080(12) 0.0191(12) C46 0.0352(14) 0.0413(15) 0.0476(15) -0.0294(13) -0.0171(12) 0.0236(12) C47 0.0280(12) 0.0270(12) 0.0465(14) -0.0201(11) -0.0171(11) 0.0129(10) C48 0.0236(12) 0.0229(12) 0.0351(13) -0.0110(11) -0.0114(11) 0.0090(10) C49 0.0343(15) 0.0238(14) 0.0623(19) -0.0226(14) -0.0269(15) 0.0155(12) C50 0.0496(19) 0.0129(13) 0.084(2) -0.0066(14) -0.0370(19) 0.0014(13) _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 1.8838(16) . ? Cu1 O3 1.9010(16) . ? Cu1 N1 1.920(2) . ? Cu1 N2 1.940(2) . ? Cu1 K1 3.4984(5) . ? Cu2 O6 1.8950(16) . ? Cu2 O7 1.8968(16) . ? Cu2 N4 1.9231(19) . ? Cu2 N3 1.933(2) . ? Cu3 O10 1.9067(18) . ? Cu3 O10 1.9067(18) 2_556 ? Cu3 N5 1.938(3) 2_556 ? Cu3 N5 1.938(3) . ? K1 O3 2.6411(16) . ? K1 O3 2.6411(16) 2_656 ? K1 O2 2.6794(17) 2_656 ? K1 O2 2.6794(17) . ? K1 O4 3.0564(18) 2_656 ? K1 O4 3.0564(17) . ? K1 O1 3.2073(18) . ? K1 O1 3.2073(18) 2_656 ? K1 Cu1 3.4984(4) 2_656 ? K2 O6 2.7173(17) . ? K2 O9 2.7270(18) 2_556 ? K2 O11 2.738(2) . ? K2 O10 2.7756(19) 2_556 ? K2 O7 2.8532(17) . ? K2 O5 2.9955(17) . ? K2 O8 3.1148(18) . ? K2 C48 3.378(3) 2_556 ? K2 C43 3.407(3) 2_556 ? Cl1 O11 1.427(2) . ? Cl1 O11 1.427(2) 2_556 ? Cl1 O12 1.431(2) . ? Cl1 O12 1.431(2) 2_556 ? Cl2 O14A 1.4363(10) . ? Cl2 O13B 1.4382(10) . ? Cl2 O15A 1.4389(10) . ? Cl2 O15B 1.4389(10) . ? Cl2 O13A 1.4393(11) . ? Cl2 O16B 1.4407(10) . ? Cl2 O16A 1.4407(10) . ? Cl2 O14B 1.4430(10) . ? O1 C3 1.372(3) . ? O1 C2 1.431(3) . ? O2 C8 1.310(3) . ? O3 C18 1.305(3) . ? O4 C17 1.373(3) . ? O4 C19 1.440(3) . ? O5 C23 1.372(3) . ? O5 C22 1.434(3) . ? O6 C28 1.308(3) . ? O7 C38 1.315(3) . ? O8 C37 1.375(3) . ? O8 C39 1.441(3) . ? O9 C43 1.373(3) . ? O9 C42 1.442(3) . ? O9 K2 2.7270(18) 2_556 ? O10 C48 1.317(3) . ? O10 K2 2.7756(19) 2_556 ? N1 C9 1.283(3) . ? N1 C10 1.473(3) . ? N2 C12 1.278(3) . ? N2 C11 1.476(3) . ? N3 C29 1.286(3) . ? N3 C30 1.471(3) . ? N4 C32 1.288(3) . ? N4 C31 1.466(3) . ? N5 C49 1.276(4) . ? N5 C50 1.485(4) . ? C1 C2 1.488(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.376(3) . ? C3 C8 1.427(3) . ? C4 C5 1.403(4) . ? C4 H4 0.9500 . ? C5 C6 1.359(4) . ? C5 H5 0.9500 . ? C6 C7 1.413(4) . ? C6 H6 0.9500 . ? C7 C8 1.421(3) . ? C7 C9 1.440(4) . ? C9 H9 0.9500 . ? C10 C11 1.518(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.438(4) . ? C12 H12 0.9500 . ? C13 C14 1.411(4) . ? C13 C18 1.418(3) . ? C14 C15 1.364(4) . ? C14 H14 0.9500 . ? C15 C16 1.402(4) . ? C15 H15 0.9500 . ? C16 C17 1.375(3) . ? C16 H16 0.9500 . ? C17 C18 1.426(3) . ? C19 C20 1.498(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.498(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.381(3) . ? C23 C28 1.431(3) . ? C24 C25 1.405(4) . ? C24 H24 0.9500 . ? C25 C26 1.360(4) . ? C25 H25 0.9500 . ? C26 C27 1.419(3) . ? C26 H26 0.9500 . ? C27 C28 1.416(3) . ? C27 C29 1.443(3) . ? C29 H29 0.9500 . ? C30 C31 1.525(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.438(3) . ? C32 H32 0.9500 . ? C33 C34 1.415(3) . ? C33 C38 1.420(3) . ? C34 C35 1.368(4) . ? C34 H34 0.9500 . ? C35 C36 1.394(3) . ? C35 H35 0.9500 . ? C36 C37 1.382(3) . ? C36 H36 0.9500 . ? C37 C38 1.421(3) . ? C39 C40 1.503(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.499(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.370(4) . ? C43 C48 1.426(4) . ? C43 K2 3.407(3) 2_556 ? C44 C45 1.405(4) . ? C44 H44 0.9500 . ? C45 C46 1.351(5) . ? C45 H45 0.9500 . ? C46 C47 1.419(4) . ? C46 H46 0.9500 . ? C47 C48 1.419(4) . ? C47 C49 1.440(4) . ? C48 K2 3.378(3) 2_556 ? C49 H49 0.9500 . ? C50 C50 1.507(7) 2_556 ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? 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 O3 87.81(7) . . ? O2 Cu1 N1 94.21(8) . . ? O3 Cu1 N1 173.94(9) . . ? O2 Cu1 N2 175.97(8) . . ? O3 Cu1 N2 92.46(8) . . ? N1 Cu1 N2 85.93(9) . . ? O2 Cu1 K1 49.22(5) . . ? O3 Cu1 K1 48.13(5) . . ? N1 Cu1 K1 130.25(6) . . ? N2 Cu1 K1 133.05(7) . . ? O6 Cu2 O7 87.61(7) . . ? O6 Cu2 N4 177.84(8) . . ? O7 Cu2 N4 93.48(8) . . ? O6 Cu2 N3 93.88(8) . . ? O7 Cu2 N3 177.88(8) . . ? N4 Cu2 N3 84.98(8) . . ? O6 Cu2 K2 45.58(5) . . ? O7 Cu2 K2 49.79(5) . . ? N4 Cu2 K2 136.29(6) . . ? N3 Cu2 K2 132.23(6) . . ? O10 Cu3 O10 88.30(10) . 2_556 ? O10 Cu3 N5 173.59(9) . 2_556 ? O10 Cu3 N5 93.66(10) 2_556 2_556 ? O10 Cu3 N5 93.66(10) . . ? O10 Cu3 N5 173.59(9) 2_556 . ? N5 Cu3 N5 85.06(17) 2_556 . ? O10 Cu3 K2 43.74(6) . 2_556 ? O10 Cu3 K2 64.95(5) 2_556 2_556 ? N5 Cu3 K2 132.22(8) 2_556 2_556 ? N5 Cu3 K2 120.32(8) . 2_556 ? O10 Cu3 K2 64.95(5) . . ? O10 Cu3 K2 43.74(6) 2_556 . ? N5 Cu3 K2 120.32(8) 2_556 . ? N5 Cu3 K2 132.22(8) . . ? K2 Cu3 K2 74.031(19) 2_556 . ? O3 K1 O3 170.70(8) . 2_656 ? O3 K1 O2 129.56(5) . 2_656 ? O3 K1 O2 59.11(5) 2_656 2_656 ? O3 K1 O2 59.11(5) . . ? O3 K1 O2 129.56(5) 2_656 . ? O2 K1 O2 80.88(7) 2_656 . ? O3 K1 O4 117.84(5) . 2_656 ? O3 K1 O4 53.18(5) 2_656 2_656 ? O2 K1 O4 104.21(5) 2_656 2_656 ? O2 K1 O4 174.27(5) . 2_656 ? O3 K1 O4 53.18(5) . . ? O3 K1 O4 117.84(5) 2_656 . ? O2 K1 O4 174.27(5) 2_656 . ? O2 K1 O4 104.21(5) . . ? O4 K1 O4 70.85(7) 2_656 . ? O3 K1 O1 101.79(5) . . ? O3 K1 O1 84.34(5) 2_656 . ? O2 K1 O1 68.71(5) 2_656 . ? O2 K1 O1 51.08(5) . . ? O4 K1 O1 127.98(4) 2_656 . ? O4 K1 O1 116.48(5) . . ? O3 K1 O1 84.34(5) . 2_656 ? O3 K1 O1 101.79(5) 2_656 2_656 ? O2 K1 O1 51.08(5) 2_656 2_656 ? O2 K1 O1 68.71(5) . 2_656 ? O4 K1 O1 116.48(5) 2_656 2_656 ? O4 K1 O1 127.98(4) . 2_656 ? O1 K1 O1 98.74(6) . 2_656 ? O3 K1 Cu1 156.82(5) . 2_656 ? O3 K1 Cu1 32.41(4) 2_656 2_656 ? O2 K1 Cu1 32.17(3) 2_656 2_656 ? O2 K1 Cu1 98.15(4) . 2_656 ? O4 K1 Cu1 85.20(3) 2_656 2_656 ? O4 K1 Cu1 146.95(3) . 2_656 ? O1 K1 Cu1 61.52(3) . 2_656 ? O1 K1 Cu1 82.76(3) 2_656 2_656 ? O3 K1 Cu1 32.41(4) . . ? O3 K1 Cu1 156.82(5) 2_656 . ? O2 K1 Cu1 98.15(4) 2_656 . ? O2 K1 Cu1 32.17(3) . . ? O4 K1 Cu1 146.95(3) 2_656 . ? O4 K1 Cu1 85.20(3) . . ? O1 K1 Cu1 82.76(3) . . ? O1 K1 Cu1 61.52(3) 2_656 . ? Cu1 K1 Cu1 124.85(2) 2_656 . ? O6 K2 O9 97.22(5) . 2_556 ? O6 K2 O11 170.09(7) . . ? O9 K2 O11 78.91(7) 2_556 . ? O6 K2 O10 76.65(5) . 2_556 ? O9 K2 O10 56.29(5) 2_556 2_556 ? O11 K2 O10 107.99(7) . 2_556 ? O6 K2 O7 56.16(5) . . ? O9 K2 O7 73.34(5) 2_556 . ? O11 K2 O7 113.94(6) . . ? O10 K2 O7 103.87(5) 2_556 . ? O6 K2 O5 53.54(5) . . ? O9 K2 O5 141.66(5) 2_556 . ? O11 K2 O5 133.85(6) . . ? O10 K2 O5 89.95(5) 2_556 . ? O7 K2 O5 101.62(5) . . ? O6 K2 O8 103.20(5) . . ? O9 K2 O8 83.90(5) 2_556 . ? O11 K2 O8 67.46(6) . . ? O10 K2 O8 139.33(5) 2_556 . ? O7 K2 O8 51.14(4) . . ? O5 K2 O8 123.26(5) . . ? O6 K2 C48 66.86(6) . 2_556 ? O9 K2 C48 43.53(6) 2_556 2_556 ? O11 K2 C48 114.19(8) . 2_556 ? O10 K2 C48 22.05(6) 2_556 2_556 ? O7 K2 C48 82.21(6) . 2_556 ? O5 K2 C48 98.40(6) . 2_556 ? O8 K2 C48 120.03(6) . 2_556 ? O6 K2 C43 76.20(6) . 2_556 ? O9 K2 C43 22.56(6) 2_556 2_556 ? O11 K2 C43 100.98(7) . 2_556 ? O10 K2 C43 43.21(6) 2_556 2_556 ? O7 K2 C43 68.03(6) . 2_556 ? O5 K2 C43 119.64(6) . 2_556 ? O8 K2 C43 96.58(6) . 2_556 ? C48 K2 C43 24.27(7) 2_556 2_556 ? O6 K2 Cu2 29.87(3) . . ? O9 K2 Cu2 74.56(4) 2_556 . ? O11 K2 Cu2 140.99(6) . . ? O10 K2 Cu2 80.10(4) 2_556 . ? O7 K2 Cu2 30.51(3) . . ? O5 K2 Cu2 82.78(3) . . ? O8 K2 Cu2 81.60(3) . . ? C48 K2 Cu2 61.41(4) 2_556 . ? C43 K2 Cu2 58.32(4) 2_556 . ? O6 K2 Cu3 72.07(4) . . ? O9 K2 Cu3 84.55(4) 2_556 . ? O11 K2 Cu3 116.25(6) . . ? O10 K2 Cu3 28.36(4) 2_556 . ? O7 K2 Cu3 119.03(4) . . ? O5 K2 Cu3 64.35(4) . . ? O8 K2 Cu3 166.85(4) . . ? C48 K2 Cu3 46.85(5) 2_556 . ? C43 K2 Cu3 70.48(5) 2_556 . ? Cu2 K2 Cu3 89.275(13) . . ? O6 K2 K2 123.34(4) . 2_556 ? O9 K2 K2 67.57(4) 2_556 2_556 ? O11 K2 K2 63.82(6) . 2_556 ? O10 K2 K2 48.86(4) 2_556 2_556 ? O7 K2 K2 140.55(4) . 2_556 ? O5 K2 K2 105.51(4) . 2_556 ? O8 K2 K2 126.92(3) . 2_556 ? C48 K2 K2 66.05(5) 2_556 2_556 ? C43 K2 K2 73.78(5) 2_556 2_556 ? Cu2 K2 K2 127.460(18) . 2_556 ? Cu3 K2 K2 52.984(9) . 2_556 ? O11 Cl1 O11 108.1(2) . 2_556 ? O11 Cl1 O12 110.21(14) . . ? O11 Cl1 O12 109.37(14) 2_556 . ? O11 Cl1 O12 109.37(14) . 2_556 ? O11 Cl1 O12 110.21(14) 2_556 2_556 ? O12 Cl1 O12 109.54(18) . 2_556 ? O14A Cl2 O15A 116.0(3) . . ? O13B Cl2 O15B 107.9(5) . . ? O14A Cl2 O13A 108.9(4) . . ? O15A Cl2 O13A 102.1(4) . . ? O13B Cl2 O16B 98.7(6) . . ? O15B Cl2 O16B 106.2(7) . . ? O14A Cl2 O16A 104.2(5) . . ? O15A Cl2 O16A 103.6(7) . . ? O13A Cl2 O16A 122.6(5) . . ? O13B Cl2 O14B 114.6(4) . . ? O15B Cl2 O14B 104.9(3) . . ? O16B Cl2 O14B 123.6(4) . . ? C3 O1 C2 117.17(19) . . ? C3 O1 K1 110.56(13) . . ? C2 O1 K1 130.23(14) . . ? C8 O2 Cu1 126.60(14) . . ? C8 O2 K1 127.87(14) . . ? Cu1 O2 K1 98.61(7) . . ? C18 O3 Cu1 128.04(15) . . ? C18 O3 K1 125.02(15) . . ? Cu1 O3 K1 99.46(7) . . ? C17 O4 C19 116.95(18) . . ? C17 O4 K1 110.64(13) . . ? C19 O4 K1 130.30(14) . . ? C23 O5 C22 117.57(18) . . ? C23 O5 K2 117.06(13) . . ? C22 O5 K2 119.31(13) . . ? C28 O6 Cu2 125.97(14) . . ? C28 O6 K2 127.15(14) . . ? Cu2 O6 K2 104.55(7) . . ? C38 O7 Cu2 125.79(15) . . ? C38 O7 K2 119.29(14) . . ? Cu2 O7 K2 99.70(6) . . ? C37 O8 C39 116.80(18) . . ? C37 O8 K2 110.33(13) . . ? C39 O8 K2 121.10(14) . . ? C43 O9 C42 118.3(2) . . ? C43 O9 K2 107.79(15) . 2_556 ? C42 O9 K2 124.30(14) . 2_556 ? C48 O10 Cu3 126.40(16) . . ? C48 O10 K2 105.65(15) . 2_556 ? Cu3 O10 K2 107.90(8) . 2_556 ? Cl1 O11 K2 145.21(16) . . ? C9 N1 C10 121.7(2) . . ? C9 N1 Cu1 125.97(17) . . ? C10 N1 Cu1 112.26(16) . . ? C12 N2 C11 121.7(2) . . ? C12 N2 Cu1 126.97(18) . . ? C11 N2 Cu1 110.97(16) . . ? C29 N3 C30 120.9(2) . . ? C29 N3 Cu2 126.07(17) . . ? C30 N3 Cu2 112.98(15) . . ? C32 N4 C31 121.5(2) . . ? C32 N4 Cu2 125.97(16) . . ? C31 N4 Cu2 112.52(15) . . ? C49 N5 C50 120.6(3) . . ? C49 N5 Cu3 126.6(2) . . ? C50 N5 Cu3 112.8(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 107.3(2) . . ? O1 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O1 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? O1 C3 C4 125.5(2) . . ? O1 C3 C8 113.6(2) . . ? C4 C3 C8 120.9(2) . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 119.9(2) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 121.5(2) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C8 119.4(2) . . ? C6 C7 C9 118.3(2) . . ? C8 C7 C9 122.3(2) . . ? O2 C8 C7 124.8(2) . . ? O2 C8 C3 117.4(2) . . ? C7 C8 C3 117.8(2) . . ? N1 C9 C7 125.4(2) . . ? N1 C9 H9 117.3 . . ? C7 C9 H9 117.3 . . ? N1 C10 C11 108.4(2) . . ? N1 C10 H10A 110.0 . . ? C11 C10 H10A 110.0 . . ? N1 C10 H10B 110.0 . . ? C11 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? N2 C11 C10 108.1(2) . . ? N2 C11 H11A 110.1 . . ? C10 C11 H11A 110.1 . . ? N2 C11 H11B 110.1 . . ? C10 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? N2 C12 C13 125.8(2) . . ? N2 C12 H12 117.1 . . ? C13 C12 H12 117.1 . . ? C14 C13 C18 119.5(2) . . ? C14 C13 C12 118.8(2) . . ? C18 C13 C12 121.5(2) . . ? C15 C14 C13 121.5(2) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 119.9(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? O4 C17 C16 125.0(2) . . ? O4 C17 C18 113.5(2) . . ? C16 C17 C18 121.5(2) . . ? O3 C18 C13 125.0(2) . . ? O3 C18 C17 117.5(2) . . ? C13 C18 C17 117.5(2) . . ? O4 C19 C20 107.6(2) . . ? O4 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O4 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 C21 106.32(19) . . ? O5 C22 H22A 110.5 . . ? C21 C22 H22A 110.5 . . ? O5 C22 H22B 110.5 . . ? C21 C22 H22B 110.5 . . ? H22A C22 H22B 108.7 . . ? O5 C23 C24 124.9(2) . . ? O5 C23 C28 114.0(2) . . ? C24 C23 C28 121.1(2) . . ? C23 C24 C25 120.2(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.2(2) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 121.0(2) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C28 C27 C26 119.9(2) . . ? C28 C27 C29 122.3(2) . . ? C26 C27 C29 117.7(2) . . ? O6 C28 C27 125.5(2) . . ? O6 C28 C23 117.0(2) . . ? C27 C28 C23 117.5(2) . . ? N3 C29 C27 125.0(2) . . ? N3 C29 H29 117.5 . . ? C27 C29 H29 117.5 . . ? N3 C30 C31 107.77(19) . . ? N3 C30 H30A 110.2 . . ? C31 C30 H30A 110.2 . . ? N3 C30 H30B 110.2 . . ? C31 C30 H30B 110.2 . . ? H30A C30 H30B 108.5 . . ? N4 C31 C30 107.93(19) . . ? N4 C31 H31A 110.1 . . ? C30 C31 H31A 110.1 . . ? N4 C31 H31B 110.1 . . ? C30 C31 H31B 110.1 . . ? H31A C31 H31B 108.4 . . ? N4 C32 C33 124.7(2) . . ? N4 C32 H32 117.6 . . ? C33 C32 H32 117.6 . . ? C34 C33 C38 119.8(2) . . ? C34 C33 C32 117.8(2) . . ? C38 C33 C32 122.3(2) . . ? C35 C34 C33 120.9(2) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 120.1(2) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 120.4(2) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? O8 C37 C36 125.2(2) . . ? O8 C37 C38 113.6(2) . . ? C36 C37 C38 121.2(2) . . ? O7 C38 C33 124.8(2) . . ? O7 C38 C37 117.8(2) . . ? C33 C38 C37 117.4(2) . . ? O8 C39 C40 107.7(2) . . ? O8 C39 H39A 110.2 . . ? C40 C39 H39A 110.2 . . ? O8 C39 H39B 110.2 . . ? C40 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O9 C42 C41 110.8(2) . . ? O9 C42 H42A 109.5 . . ? C41 C42 H42A 109.5 . . ? O9 C42 H42B 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? C44 C43 O9 124.7(3) . . ? C44 C43 C48 121.6(2) . . ? O9 C43 C48 113.7(2) . . ? C44 C43 K2 142.72(19) . 2_556 ? O9 C43 K2 49.65(12) . 2_556 ? C48 C43 K2 76.73(15) . 2_556 ? C43 C44 C45 120.3(3) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C46 C45 C44 119.9(3) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 121.4(3) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C48 C47 C46 119.7(3) . . ? C48 C47 C49 122.6(3) . . ? C46 C47 C49 117.7(3) . . ? O10 C48 C47 125.1(3) . . ? O10 C48 C43 117.9(2) . . ? C47 C48 C43 117.0(3) . . ? O10 C48 K2 52.29(12) . 2_556 ? C47 C48 K2 142.25(19) . 2_556 ? C43 C48 K2 79.00(15) . 2_556 ? N5 C49 C47 125.4(3) . . ? N5 C49 H49 117.3 . . ? C47 C49 H49 117.3 . . ? N5 C50 C50 108.77(19) . 2_556 ? N5 C50 H50A 109.9 . . ? C50 C50 H50A 109.9 2_556 . ? N5 C50 H50B 109.9 . . ? C50 C50 H50B 109.9 2_556 . ? H50A C50 H50B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.128 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.066 #==== end data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 Cu F6 K N2 O4 P' _chemical_formula_sum 'C20 H22 Cu F6 K N2 O4 P' _chemical_formula_weight 602.01 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.1687(2) _cell_length_b 13.7862(4) _cell_length_c 23.3747(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2310.10(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4890 _cell_measurement_theta_min 2.6096 _cell_measurement_theta_max 32.4432 _exptl_crystal_description block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.78941 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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_measurement_method ? _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10437 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 32.51 _reflns_number_total 6871 _reflns_number_gt 5250 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0203P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(9) _refine_ls_number_reflns 6871 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 0.865 _refine_ls_restrained_S_all 0.865 _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 0.23799(4) 0.582516(19) 0.969258(9) 0.01542(6) Uani 1 1 d . . . K1 K 0.22604(7) 0.52602(3) 1.120687(17) 0.01774(10) Uani 1 1 d . . . P1 P 0.70728(8) 0.50616(5) 1.20254(2) 0.01974(13) Uani 1 1 d . . . F1 F 0.5844(2) 0.50985(15) 1.14567(8) 0.0551(5) Uani 1 1 d . . . F2 F 0.88728(18) 0.52950(14) 1.16511(7) 0.0433(5) Uani 1 1 d . . . F3 F 0.7381(2) 0.39314(9) 1.19325(5) 0.0343(3) Uani 1 1 d . . . F4 F 0.5254(2) 0.48352(14) 1.23877(9) 0.0649(6) Uani 1 1 d . . . F5 F 0.6754(2) 0.61960(11) 1.21051(7) 0.0467(5) Uani 1 1 d . . . F6 F 0.8314(2) 0.50310(14) 1.25833(6) 0.0582(5) Uani 1 1 d . . . O1 O 0.2409(2) 0.72624(10) 1.14236(5) 0.0177(3) Uani 1 1 d . . . O2 O 0.2419(2) 0.65703(10) 1.03821(5) 0.0160(3) Uani 1 1 d . . . O3 O 0.2117(2) 0.46740(10) 1.01400(5) 0.0164(3) Uani 1 1 d . . . O4 O 0.1673(2) 0.33345(12) 1.09181(6) 0.0181(3) Uani 1 1 d . . . N1 N 0.2548(3) 0.69583(13) 0.92072(6) 0.0162(4) Uani 1 1 d . . . N2 N 0.2493(3) 0.51100(13) 0.89785(6) 0.0177(4) Uani 1 1 d . . . C1 C 0.2047(3) 0.68173(17) 1.24031(9) 0.0235(5) Uani 1 1 d . . . H1A H 0.0907 0.6469 1.2297 0.035 Uiso 1 1 calc R . . H1B H 0.1924 0.7067 1.2794 0.035 Uiso 1 1 calc R . . H1C H 0.3114 0.6374 1.2384 0.035 Uiso 1 1 calc R . . C2 C 0.2347(3) 0.76458(15) 1.19983(7) 0.0159(4) Uani 1 1 d . . . H2A H 0.1316 0.8120 1.2034 0.019 Uiso 1 1 calc R . . H2B H 0.3533 0.7980 1.2089 0.019 Uiso 1 1 calc R . . C3 C 0.2585(3) 0.79322(15) 1.09880(8) 0.0149(4) Uani 1 1 d . . . C4 C 0.2776(3) 0.89114(16) 1.10685(8) 0.0172(5) Uani 1 1 d . . . H4 H 0.2811 0.9168 1.1446 0.021 Uiso 1 1 calc R . . C5 C 0.2922(3) 0.95389(17) 1.05974(9) 0.0206(5) Uani 1 1 d . . . H5 H 0.3057 1.0217 1.0656 0.025 Uiso 1 1 calc R . . C6 C 0.2869(3) 0.91714(18) 1.00553(9) 0.0199(5) Uani 1 1 d . . . H6 H 0.2955 0.9599 0.9738 0.024 Uiso 1 1 calc R . . C7 C 0.2688(3) 0.81646(16) 0.99598(8) 0.0172(4) Uani 1 1 d . . . C8 C 0.2564(3) 0.75147(15) 1.04255(7) 0.0139(4) Uani 1 1 d . . . C9 C 0.2660(3) 0.78445(17) 0.93719(8) 0.0194(5) Uani 1 1 d . . . H9 H 0.2731 0.8329 0.9084 0.023 Uiso 1 1 calc R . . C10 C 0.2406(3) 0.67475(16) 0.85900(7) 0.0198(5) Uani 1 1 d . . . H10A H 0.3201 0.7203 0.8371 0.024 Uiso 1 1 calc R . . H10B H 0.1100 0.6829 0.8461 0.024 Uiso 1 1 calc R . . C11 C 0.3041(3) 0.57099(18) 0.84857(8) 0.0216(5) Uani 1 1 d . . . H11A H 0.2457 0.5455 0.8133 0.026 Uiso 1 1 calc R . . H11B H 0.4412 0.5691 0.8437 0.026 Uiso 1 1 calc R . . C12 C 0.2114(3) 0.42144(18) 0.89129(8) 0.0191(5) Uani 1 1 d . . . H12 H 0.2082 0.3976 0.8532 0.023 Uiso 1 1 calc R . . C13 C 0.1731(3) 0.35287(18) 0.93629(9) 0.0173(5) Uani 1 1 d . . . C14 C 0.1405(3) 0.25563(19) 0.92021(10) 0.0208(5) Uani 1 1 d . . . H14 H 0.1366 0.2390 0.8808 0.025 Uiso 1 1 calc R . . C15 C 0.1148(3) 0.18552(19) 0.96012(10) 0.0230(6) Uani 1 1 d . . . H15 H 0.0928 0.1203 0.9488 0.028 Uiso 1 1 calc R . . C16 C 0.1211(3) 0.21044(18) 1.01864(10) 0.0191(5) Uani 1 1 d . . . H16 H 0.1024 0.1616 1.0467 0.023 Uiso 1 1 calc R . . C17 C 0.1534(3) 0.30341(18) 1.03543(10) 0.0159(5) Uani 1 1 d . . . C18 C 0.1788(3) 0.37955(18) 0.99498(9) 0.0154(5) Uani 1 1 d . . . C19 C 0.1656(3) 0.25842(18) 1.13417(9) 0.0202(5) Uani 1 1 d . . . H19A H 0.2603 0.2085 1.1249 0.024 Uiso 1 1 calc R . . H19B H 0.0416 0.2269 1.1354 0.024 Uiso 1 1 calc R . . C20 C 0.2093(4) 0.30483(18) 1.19140(9) 0.0266(6) Uani 1 1 d . . . H20A H 0.3336 0.3343 1.1900 0.040 Uiso 1 1 calc R . . H20B H 0.2064 0.2552 1.2214 0.040 Uiso 1 1 calc R . . H20C H 0.1162 0.3549 1.1998 0.040 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 0.02040(12) 0.01574(12) 0.01012(10) -0.00001(11) 0.00040(11) -0.00080(14) K1 0.0249(2) 0.0146(2) 0.01376(19) 0.00045(18) 0.0022(2) -0.0004(2) P1 0.0198(3) 0.0172(3) 0.0222(3) 0.0012(3) 0.0016(2) -0.0022(3) F1 0.0533(9) 0.0439(13) 0.0682(12) 0.0133(12) -0.0444(9) -0.0049(10) F2 0.0273(7) 0.0552(14) 0.0474(10) 0.0135(10) 0.0163(7) -0.0015(8) F3 0.0471(8) 0.0185(7) 0.0372(7) -0.0009(6) 0.0009(8) 0.0055(9) F4 0.0595(10) 0.0344(12) 0.1010(16) -0.0089(12) 0.0576(10) -0.0107(10) F5 0.0604(10) 0.0172(8) 0.0625(11) -0.0030(9) 0.0152(9) -0.0029(8) F6 0.0996(13) 0.0470(12) 0.0280(8) 0.0108(9) -0.0309(9) -0.0238(12) O1 0.0294(8) 0.0123(7) 0.0114(6) -0.0008(6) 0.0011(7) 0.0009(9) O2 0.0253(7) 0.0119(7) 0.0109(6) 0.0000(6) 0.0005(8) -0.0021(9) O3 0.0261(8) 0.0105(8) 0.0125(6) -0.0019(6) 0.0003(6) 0.0001(7) O4 0.0262(8) 0.0137(9) 0.0144(7) 0.0014(7) 0.0007(6) -0.0006(7) N1 0.0171(9) 0.0221(10) 0.0093(7) 0.0019(7) 0.0000(8) -0.0028(11) N2 0.0187(8) 0.0239(10) 0.0106(7) -0.0016(7) 0.0012(8) -0.0003(11) C1 0.0348(13) 0.0204(13) 0.0154(10) 0.0015(10) 0.0024(10) 0.0056(12) C2 0.0200(11) 0.0156(10) 0.0122(8) -0.0050(8) 0.0012(10) 0.0005(11) C3 0.0138(9) 0.0165(11) 0.0146(8) 0.0033(8) -0.0003(10) 0.0001(12) C4 0.0187(10) 0.0156(11) 0.0172(9) -0.0018(9) -0.0005(9) 0.0019(11) C5 0.0234(11) 0.0120(11) 0.0265(11) -0.0008(10) -0.0001(9) -0.0019(10) C6 0.0220(11) 0.0150(11) 0.0228(10) 0.0069(10) 0.0007(9) -0.0001(12) C7 0.0155(10) 0.0187(11) 0.0173(9) 0.0023(9) -0.0006(9) 0.0005(11) C8 0.0118(9) 0.0146(10) 0.0155(9) -0.0014(8) -0.0001(9) -0.0008(12) C9 0.0189(11) 0.0245(12) 0.0147(9) 0.0090(9) 0.0002(10) 0.0003(13) C10 0.0209(10) 0.0284(12) 0.0101(8) 0.0031(9) 0.0006(10) -0.0008(13) C11 0.0221(11) 0.0307(14) 0.0121(9) 0.0001(10) 0.0021(8) -0.0051(12) C12 0.0159(10) 0.0267(13) 0.0147(9) -0.0050(10) -0.0011(8) 0.0017(12) C13 0.0149(10) 0.0204(14) 0.0167(10) -0.0060(10) -0.0004(8) -0.0015(10) C14 0.0180(11) 0.0238(15) 0.0207(11) -0.0098(12) -0.0009(9) 0.0011(11) C15 0.0194(11) 0.0170(13) 0.0325(14) -0.0118(12) -0.0013(10) -0.0004(11) C16 0.0184(10) 0.0150(13) 0.0238(13) -0.0001(11) -0.0013(9) 0.0009(10) C17 0.0144(9) 0.0165(12) 0.0168(11) -0.0025(10) 0.0013(9) 0.0018(9) C18 0.0128(10) 0.0163(12) 0.0172(10) -0.0026(10) 0.0000(8) 0.0010(9) C19 0.0230(11) 0.0162(13) 0.0215(11) 0.0069(11) 0.0001(9) -0.0041(10) C20 0.0358(14) 0.0227(13) 0.0213(11) 0.0062(10) 0.0004(10) -0.0020(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.9100(14) . ? Cu1 O2 1.9115(12) . ? Cu1 N1 1.9345(17) . ? Cu1 N2 1.9403(15) . ? K1 O3 2.6235(14) . ? K1 F2 2.6417(14) 1_455 ? K1 F1 2.6440(15) . ? K1 O2 2.6442(13) . ? K1 O4 2.7716(17) . ? K1 O1 2.8083(14) . ? P1 F6 1.5792(16) . ? P1 F4 1.5858(15) . ? P1 F3 1.5886(15) . ? P1 F5 1.5914(17) . ? P1 F2 1.5918(14) . ? P1 F1 1.5953(16) . ? F2 K1 2.6417(13) 1_655 ? O1 C3 1.380(2) . ? O1 C2 1.444(2) . ? O2 C8 1.310(2) . ? O3 C18 1.311(3) . ? O4 C17 1.385(3) . ? O4 C19 1.432(3) . ? N1 C9 1.284(3) . ? N1 C10 1.475(2) . ? N2 C12 1.273(3) . ? N2 C11 1.471(3) . ? C1 C2 1.499(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.370(3) . ? C3 C8 1.435(2) . ? C4 C5 1.404(3) . ? C4 H4 0.9500 . ? C5 C6 1.365(3) . ? C5 H5 0.9500 . ? C6 C7 1.412(3) . ? C6 H6 0.9500 . ? C7 C8 1.413(3) . ? C7 C9 1.443(3) . ? C9 H9 0.9500 . ? C10 C11 1.521(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.441(3) . ? C12 H12 0.9500 . ? C13 C14 1.412(3) . ? C13 C18 1.421(3) . ? C14 C15 1.356(3) . ? C14 H14 0.9500 . ? C15 C16 1.411(3) . ? C15 H15 0.9500 . ? C16 C17 1.360(3) . ? C16 H16 0.9500 . ? C17 C18 1.424(3) . ? C19 C20 1.515(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 O3 Cu1 O2 89.22(6) . . ? O3 Cu1 N1 176.67(7) . . ? O2 Cu1 N1 93.42(6) . . ? O3 Cu1 N2 93.03(7) . . ? O2 Cu1 N2 176.23(8) . . ? N1 Cu1 N2 84.45(7) . . ? O3 Cu1 K1 44.32(4) . . ? O2 Cu1 K1 44.97(4) . . ? N1 Cu1 K1 138.38(5) . . ? N2 Cu1 K1 137.03(5) . . ? O3 K1 F2 110.07(5) . 1_455 ? O3 K1 F1 102.84(6) . . ? F2 K1 F1 143.90(6) 1_455 . ? O3 K1 O2 61.25(4) . . ? F2 K1 O2 108.29(5) 1_455 . ? F1 K1 O2 100.19(6) . . ? O3 K1 O4 57.82(5) . . ? F2 K1 O4 88.47(5) 1_455 . ? F1 K1 O4 96.93(6) . . ? O2 K1 O4 118.90(4) . . ? O3 K1 O1 118.41(4) . . ? F2 K1 O1 86.91(6) 1_455 . ? F1 K1 O1 90.36(6) . . ? O2 K1 O1 57.22(4) . . ? O4 K1 O1 172.38(5) . . ? O3 K1 Cu1 30.57(3) . . ? F2 K1 Cu1 113.68(4) 1_455 . ? F1 K1 Cu1 102.17(4) . . ? O2 K1 Cu1 30.73(3) . . ? O4 K1 Cu1 88.37(3) . . ? O1 K1 Cu1 87.94(3) . . ? F6 P1 F4 90.96(11) . . ? F6 P1 F3 90.48(9) . . ? F4 P1 F3 89.66(10) . . ? F6 P1 F5 90.60(10) . . ? F4 P1 F5 90.72(10) . . ? F3 P1 F5 178.84(9) . . ? F6 P1 F2 90.16(9) . . ? F4 P1 F2 178.85(11) . . ? F3 P1 F2 90.60(10) . . ? F5 P1 F2 88.99(10) . . ? F6 P1 F1 179.19(11) . . ? F4 P1 F1 89.84(11) . . ? F3 P1 F1 89.66(10) . . ? F5 P1 F1 89.25(10) . . ? F2 P1 F1 89.04(9) . . ? P1 F1 K1 136.32(11) . . ? P1 F2 K1 163.25(11) . 1_655 ? C3 O1 C2 116.37(15) . . ? C3 O1 K1 121.86(11) . . ? C2 O1 K1 121.76(11) . . ? C8 O2 Cu1 126.91(11) . . ? C8 O2 K1 128.74(11) . . ? Cu1 O2 K1 104.30(6) . . ? C18 O3 Cu1 126.83(13) . . ? C18 O3 K1 127.87(13) . . ? Cu1 O3 K1 105.11(6) . . ? C17 O4 C19 116.20(18) . . ? C17 O4 K1 121.94(13) . . ? C19 O4 K1 121.65(13) . . ? C9 N1 C10 119.03(17) . . ? C9 N1 Cu1 126.63(13) . . ? C10 N1 Cu1 114.21(13) . . ? C12 N2 C11 120.51(17) . . ? C12 N2 Cu1 125.97(14) . . ? C11 N2 Cu1 113.51(14) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 108.22(16) . . ? O1 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O1 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C4 C3 O1 124.54(17) . . ? C4 C3 C8 121.47(18) . . ? O1 C3 C8 113.99(17) . . ? C3 C4 C5 120.46(19) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.8(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.9(2) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C8 120.50(18) . . ? C6 C7 C9 116.89(19) . . ? C8 C7 C9 122.61(19) . . ? O2 C8 C7 125.14(16) . . ? O2 C8 C3 118.06(17) . . ? C7 C8 C3 116.80(18) . . ? N1 C9 C7 125.27(19) . . ? N1 C9 H9 117.4 . . ? C7 C9 H9 117.4 . . ? N1 C10 C11 108.75(17) . . ? N1 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N1 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N2 C11 C10 108.87(17) . . ? N2 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? N2 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N2 C12 C13 126.08(19) . . ? N2 C12 H12 117.0 . . ? C13 C12 H12 117.0 . . ? C14 C13 C18 120.5(2) . . ? C14 C13 C12 117.4(2) . . ? C18 C13 C12 122.0(2) . . ? C15 C14 C13 121.1(2) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.3(2) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 121.0(2) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 O4 124.6(2) . . ? C16 C17 C18 121.7(2) . . ? O4 C17 C18 113.7(2) . . ? O3 C18 C13 124.9(2) . . ? O3 C18 C17 118.58(19) . . ? C13 C18 C17 116.5(2) . . ? O4 C19 C20 107.7(2) . . ? O4 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O4 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.532 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.072 #==== end data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H144 B2 Cu4 N8 O20 Rb2' _chemical_formula_weight 2633.3 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' 'Rb' 'Rb' -0.9393 2.9676 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0693(5) _cell_length_b 14.9039(6) _cell_length_c 16.9493(5) _cell_angle_alpha 115.765(4) _cell_angle_beta 106.404(3) _cell_angle_gamma 91.471(3) _cell_volume 3024.78(19) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 18944 _cell_measurement_theta_min 2.5759 _cell_measurement_theta_max 32.6345 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 0.742 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) 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 120(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_measurement_method ? _diffrn_detector_area_resol_mean 16.1511 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33356 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12322 _reflns_number_gt 9646 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0327P)^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 12322 _refine_ls_number_parameters 784 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.955 _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 Rb1 Rb 0.097913(13) 0.740482(12) 0.400690(11) 0.01814(5) Uani 1 1 d . . . Cu1 Cu -0.006016(16) 0.625793(16) 0.519693(14) 0.01980(6) Uani 1 1 d . . . Cu2 Cu 0.071317(15) 0.943636(15) 0.625561(13) 0.01488(5) Uani 1 1 d . A . O1 O 0.29811(8) 0.76420(9) 0.55076(8) 0.0217(3) Uani 1 1 d . . . O2 O 0.12426(8) 0.69388(9) 0.54808(7) 0.0199(3) Uani 1 1 d . . . O3 O -0.02190(8) 0.58080(9) 0.39230(8) 0.0196(3) Uani 1 1 d . . . O4 O -0.00417(9) 0.53434(9) 0.23026(8) 0.0247(3) Uani 1 1 d . . . O5 O 0.22160(8) 0.93023(9) 0.42183(7) 0.0189(3) Uani 1 1 d . . . O6 O 0.15057(8) 0.94316(8) 0.54983(7) 0.0164(2) Uani 1 1 d . . . O7 O -0.03507(8) 0.85177(8) 0.51488(7) 0.0179(3) Uani 1 1 d . . . O8 O -0.16100(8) 0.74536(9) 0.34933(7) 0.0204(3) Uani 1 1 d . A . O9 O 0.00537(9) 1.08878(9) 0.61997(8) 0.0191(3) Uani 1 1 d D . . H9A H -0.0485(11) 1.0624(12) 0.5784(11) 0.029 Uiso 1 1 d D . . H9B H 0.0407(12) 1.1146(13) 0.6028(12) 0.029 Uiso 1 1 d D . . O10 O 0.34839(14) 0.71198(14) 0.20947(13) 0.0693(5) Uani 1 1 d U . . N1 N 0.00631(12) 0.66868(12) 0.64747(11) 0.0260(4) Uani 1 1 d . . . N2 N -0.13490(12) 0.55128(12) 0.49242(11) 0.0267(4) Uani 1 1 d . . . N3 N 0.18224(11) 1.01963(11) 0.74011(9) 0.0197(3) Uani 1 1 d . . . N4 N -0.00121(11) 0.93984(11) 0.70657(9) 0.0230(3) Uani 1 1 d . . . C1 C 0.39074(14) 0.76729(14) 0.45430(13) 0.0283(4) Uani 1 1 d . . . H1A H 0.3721 0.6936 0.4176 0.042 Uiso 1 1 calc R . . H1B H 0.4566 0.7891 0.4534 0.042 Uiso 1 1 calc R . . H1C H 0.3403 0.7995 0.4278 0.042 Uiso 1 1 calc R . . C2 C 0.39578(13) 0.79731(14) 0.55209(13) 0.0260(4) Uani 1 1 d . . . H2A H 0.4468 0.7654 0.5796 0.031 Uiso 1 1 calc R . . H2B H 0.4149 0.8716 0.5899 0.031 Uiso 1 1 calc R . . C3 C 0.28906(13) 0.78241(13) 0.63518(11) 0.0209(4) Uani 1 1 d . . . C4 C 0.36489(15) 0.83501(14) 0.71914(12) 0.0287(4) Uani 1 1 d . . . H4 H 0.4277 0.8625 0.7212 0.034 Uiso 1 1 calc R . . C5 C 0.34949(17) 0.84799(15) 0.80125(13) 0.0355(5) Uani 1 1 d . . . H5 H 0.4020 0.8838 0.8588 0.043 Uiso 1 1 calc R . . C6 C 0.25942(17) 0.80940(15) 0.79878(12) 0.0335(5) Uani 1 1 d . . . H6 H 0.2500 0.8181 0.8549 0.040 Uiso 1 1 calc R . . C7 C 0.17944(15) 0.75642(13) 0.71412(12) 0.0247(4) Uani 1 1 d . . . C8 C 0.19318(13) 0.74225(13) 0.62997(11) 0.0193(4) Uani 1 1 d . . . C9 C 0.08659(16) 0.71844(14) 0.71741(13) 0.0282(5) Uani 1 1 d . . . H9 H 0.0839 0.7311 0.7767 0.034 Uiso 1 1 calc R . . C10 C -0.08562(15) 0.63958(16) 0.66232(14) 0.0347(5) Uani 1 1 d . . . H10A H -0.1215 0.6977 0.6807 0.042 Uiso 1 1 calc R . . H10B H -0.0674 0.6202 0.7130 0.042 Uiso 1 1 calc R . . C11 C -0.15384(16) 0.55093(16) 0.57352(15) 0.0354(5) Uani 1 1 d . . . H11A H -0.1410 0.4866 0.5751 0.043 Uiso 1 1 calc R . . H11B H -0.2251 0.5560 0.5687 0.043 Uiso 1 1 calc R . . C12 C -0.20235(14) 0.50313(14) 0.41207(15) 0.0317(5) Uani 1 1 d . . . H12 H -0.2651 0.4751 0.4098 0.038 Uiso 1 1 calc R . . C13 C -0.19152(13) 0.48788(14) 0.32570(14) 0.0266(4) Uani 1 1 d . . . C14 C -0.27300(15) 0.42831(15) 0.24314(16) 0.0374(5) Uani 1 1 d . . . H14 H -0.3347 0.4066 0.2473 0.045 Uiso 1 1 calc R . . C15 C -0.26394(16) 0.40197(16) 0.15845(16) 0.0422(6) Uani 1 1 d . . . H15 H -0.3187 0.3615 0.1039 0.051 Uiso 1 1 calc R . . C16 C -0.17386(15) 0.43455(15) 0.15195(14) 0.0349(5) Uani 1 1 d . . . H16 H -0.1671 0.4145 0.0927 0.042 Uiso 1 1 calc R . . C17 C -0.09444(14) 0.49568(13) 0.23072(12) 0.0255(4) Uani 1 1 d . . . C18 C -0.10070(13) 0.52441(13) 0.32055(12) 0.0218(4) Uani 1 1 d . . . C19 C 0.01159(17) 0.49767(16) 0.14244(13) 0.0369(5) Uani 1 1 d . . . H19A H -0.0406 0.5142 0.1001 0.044 Uiso 1 1 calc R . . H19B H 0.0072 0.4233 0.1141 0.044 Uiso 1 1 calc R . . C20 C 0.11359(17) 0.54687(17) 0.15760(14) 0.0420(6) Uani 1 1 d . . . H20A H 0.1171 0.6204 0.1853 0.063 Uiso 1 1 calc R . . H20B H 0.1257 0.5226 0.0981 0.063 Uiso 1 1 calc R . . H20C H 0.1648 0.5299 0.1993 0.063 Uiso 1 1 calc R . . C21 C 0.16734(15) 0.86403(15) 0.25939(12) 0.0306(5) Uani 1 1 d . . . H21A H 0.1728 0.7936 0.2450 0.046 Uiso 1 1 calc R . . H21B H 0.1738 0.8761 0.2086 0.046 Uiso 1 1 calc R . . H21C H 0.1018 0.8772 0.2671 0.046 Uiso 1 1 calc R . . C22 C 0.24961(13) 0.93326(14) 0.34753(11) 0.0213(4) Uani 1 1 d . . . H22A H 0.3148 0.9099 0.3469 0.026 Uiso 1 1 calc R . . H22B H 0.2559 1.0030 0.3549 0.026 Uiso 1 1 calc R . . C23 C 0.28474(12) 0.98996(12) 0.51113(11) 0.0167(4) Uani 1 1 d . . . C24 C 0.37942(13) 1.04085(13) 0.53464(12) 0.0209(4) Uani 1 1 d . . . H24 H 0.4048 1.0386 0.4876 0.025 Uiso 1 1 calc R . . C25 C 0.43834(13) 1.09608(13) 0.62836(12) 0.0240(4) Uani 1 1 d . . . H25 H 0.5037 1.1315 0.6450 0.029 Uiso 1 1 calc R . . C26 C 0.40128(13) 1.09859(13) 0.69543(12) 0.0222(4) Uani 1 1 d . A . H26 H 0.4422 1.1347 0.7586 0.027 Uiso 1 1 calc R . . C27 C 0.30345(13) 1.04867(13) 0.67304(11) 0.0176(4) Uani 1 1 d . . . C28 C 0.24243(12) 0.99273(12) 0.57927(11) 0.0153(3) Uani 1 1 d . A . C29 C 0.26990(13) 1.05722(13) 0.74875(11) 0.0206(4) Uani 1 1 d . A . H29 H 0.3164 1.0935 0.8097 0.025 Uiso 1 1 calc R . . C30A C 0.1631(2) 1.0237(2) 0.82285(19) 0.0208(6) Uani 0.71 1 d P A 1 H30A H 0.2005 1.0870 0.8787 0.025 Uiso 0.71 1 calc PR A 1 H30B H 0.1844 0.9655 0.8327 0.025 Uiso 0.71 1 calc PR A 1 C31A C 0.0501(2) 1.0198(2) 0.8040(2) 0.0238(7) Uani 0.71 1 d P A 1 H31A H 0.0293 1.0030 0.8479 0.029 Uiso 0.71 1 calc PR A 1 H31B H 0.0319 1.0861 0.8117 0.029 Uiso 0.71 1 calc PR A 1 C32 C -0.08948(14) 0.89095(14) 0.68192(12) 0.0233(4) Uani 1 1 d . A . H32 H -0.1156 0.8975 0.7297 0.028 Uiso 1 1 calc R . . C33 C -0.15253(13) 0.82669(13) 0.58743(12) 0.0197(4) Uani 1 1 d . . . C34 C -0.24881(14) 0.77923(14) 0.57319(13) 0.0253(4) Uani 1 1 d . A . H34 H -0.2680 0.7886 0.6253 0.030 Uiso 1 1 calc R . . C35 C -0.31425(14) 0.72059(14) 0.48635(14) 0.0285(4) Uani 1 1 d . . . H35 H -0.3781 0.6885 0.4781 0.034 Uiso 1 1 calc R A . C36 C -0.28684(13) 0.70777(14) 0.40904(13) 0.0248(4) Uani 1 1 d . A . H36 H -0.3328 0.6676 0.3484 0.030 Uiso 1 1 calc R . . C37 C -0.19448(12) 0.75263(13) 0.42034(11) 0.0186(4) Uani 1 1 d . . . C38 C -0.12264(12) 0.81277(12) 0.51002(11) 0.0170(4) Uani 1 1 d . A . C39 C -0.23243(14) 0.69586(14) 0.25694(11) 0.0250(4) Uani 1 1 d . . . H39A H -0.2920 0.7297 0.2537 0.030 Uiso 1 1 calc R A . H39B H -0.2549 0.6242 0.2393 0.030 Uiso 1 1 calc R . . C40 C -0.18074(15) 0.70234(15) 0.19274(12) 0.0307(5) Uani 1 1 d . A . H40A H -0.1556 0.7734 0.2129 0.046 Uiso 1 1 calc R . . H40B H -0.2286 0.6726 0.1296 0.046 Uiso 1 1 calc R . . H40C H -0.1243 0.6652 0.1938 0.046 Uiso 1 1 calc R . . C41 C 0.34497(13) 0.31350(13) 0.21498(11) 0.0199(4) Uani 1 1 d . . . C42 C 0.44783(13) 0.33697(14) 0.26876(12) 0.0246(4) Uani 1 1 d . . . H42 H 0.4913 0.2915 0.2468 0.030 Uiso 1 1 calc R . . C43 C 0.48765(14) 0.42440(15) 0.35268(12) 0.0282(4) Uani 1 1 d . . . H43 H 0.5567 0.4362 0.3878 0.034 Uiso 1 1 calc R . . C44 C 0.42794(15) 0.49409(15) 0.38534(12) 0.0285(4) Uani 1 1 d . . . H44 H 0.4552 0.5538 0.4426 0.034 Uiso 1 1 calc R . . C45 C 0.32729(14) 0.47550(14) 0.33316(12) 0.0250(4) Uani 1 1 d . . . H45 H 0.2855 0.5237 0.3537 0.030 Uiso 1 1 calc R . . C46 C 0.28721(14) 0.38603(13) 0.25051(12) 0.0219(4) Uani 1 1 d . . . H46 H 0.2176 0.3740 0.2170 0.026 Uiso 1 1 calc R . . C47 C 0.31054(12) 0.10866(13) 0.13593(11) 0.0192(4) Uani 1 1 d . . . C48 C 0.35778(13) 0.11229(15) 0.22225(12) 0.0234(4) Uani 1 1 d . . . H48 H 0.3841 0.1766 0.2748 0.028 Uiso 1 1 calc R . . C49 C 0.36786(14) 0.02622(15) 0.23450(13) 0.0279(4) Uani 1 1 d . . . H49 H 0.4008 0.0328 0.2945 0.033 Uiso 1 1 calc R . . C50 C 0.33019(13) -0.06890(15) 0.15996(13) 0.0270(4) Uani 1 1 d . . . H50 H 0.3378 -0.1280 0.1677 0.032 Uiso 1 1 calc R . . C51 C 0.28098(14) -0.07589(14) 0.07353(13) 0.0261(4) Uani 1 1 d . . . H51 H 0.2537 -0.1404 0.0215 0.031 Uiso 1 1 calc R . . C52 C 0.27137(13) 0.01083(14) 0.06275(12) 0.0234(4) Uani 1 1 d . . . H52 H 0.2366 0.0037 0.0029 0.028 Uiso 1 1 calc R . . C53 C 0.18189(13) 0.20651(13) 0.06669(11) 0.0199(4) Uani 1 1 d . . . C54 C 0.10404(13) 0.16017(15) 0.08038(12) 0.0262(4) Uani 1 1 d . . . H54 H 0.1212 0.1255 0.1167 0.031 Uiso 1 1 calc R . . C55 C 0.00299(14) 0.16262(16) 0.04328(13) 0.0313(5) Uani 1 1 d . . . H55 H -0.0469 0.1299 0.0544 0.038 Uiso 1 1 calc R . . C56 C -0.02503(14) 0.21256(14) -0.00980(12) 0.0280(4) Uani 1 1 d . . . H56 H -0.0939 0.2146 -0.0353 0.034 Uiso 1 1 calc R . . C57 C 0.04882(14) 0.25917(14) -0.02485(12) 0.0256(4) Uani 1 1 d . . . H57 H 0.0309 0.2938 -0.0611 0.031 Uiso 1 1 calc R . . C58 C 0.14970(13) 0.25598(13) 0.01268(11) 0.0221(4) Uani 1 1 d . . . H58 H 0.1989 0.2889 0.0011 0.027 Uiso 1 1 calc R . . C59 C 0.37262(12) 0.20942(13) 0.05478(11) 0.0199(4) Uani 1 1 d . . . C60 C 0.41838(13) 0.12939(14) 0.00913(11) 0.0200(4) Uani 1 1 d . . . H60 H 0.4047 0.0671 0.0099 0.024 Uiso 1 1 calc R . . C61 C 0.48298(13) 0.13666(14) -0.03731(11) 0.0240(4) Uani 1 1 d . . . H61 H 0.5131 0.0803 -0.0664 0.029 Uiso 1 1 calc R . . C62 C 0.50363(13) 0.22494(15) -0.04147(12) 0.0261(4) Uani 1 1 d . . . H62 H 0.5476 0.2301 -0.0734 0.031 Uiso 1 1 calc R . . C63 C 0.45930(14) 0.30604(15) 0.00161(12) 0.0284(4) Uani 1 1 d . . . H63 H 0.4720 0.3673 -0.0012 0.034 Uiso 1 1 calc R . . C64 C 0.39627(14) 0.29796(14) 0.04893(12) 0.0253(4) Uani 1 1 d . . . H64 H 0.3677 0.3552 0.0789 0.030 Uiso 1 1 calc R . . C65 C 0.3321(2) 0.5667(2) 0.07016(16) 0.0656(8) Uani 1 1 d . . . H65A H 0.2824 0.5986 0.0426 0.098 Uiso 1 1 calc R . . H65B H 0.2992 0.5015 0.0591 0.098 Uiso 1 1 calc R . . H65C H 0.3854 0.5558 0.0419 0.098 Uiso 1 1 calc R . . C66 C 0.37612(16) 0.63319(17) 0.17120(15) 0.0372(5) Uani 1 1 d . . . C67 C 0.45563(17) 0.59751(19) 0.22415(15) 0.0495(6) Uani 1 1 d . . . H67A H 0.4875 0.6522 0.2872 0.074 Uiso 1 1 calc R . . H67B H 0.5064 0.5774 0.1932 0.074 Uiso 1 1 calc R . . H67C H 0.4254 0.5394 0.2269 0.074 Uiso 1 1 calc R . . B1 B 0.30152(15) 0.20793(15) 0.11753(13) 0.0192(4) Uani 1 1 d . . . C30B C 0.1418(7) 1.0599(6) 0.8215(6) 0.0208(6) Uani 0.29 1 d P A 2 H30C H 0.1967 1.0776 0.8801 0.025 Uiso 0.29 1 calc PR A 2 H30D H 0.1130 1.1214 0.8267 0.025 Uiso 0.29 1 calc PR A 2 C31B C 0.0618(7) 0.9781(6) 0.8038(6) 0.0238(7) Uani 0.29 1 d P A 2 H31C H 0.0925 0.9234 0.8141 0.029 Uiso 0.29 1 calc PR A 2 H31D H 0.0214 1.0058 0.8456 0.029 Uiso 0.29 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rb1 0.02266(9) 0.01374(9) 0.01604(8) 0.00605(7) 0.00503(7) 0.00071(7) Cu1 0.01870(12) 0.02158(12) 0.02493(12) 0.01419(10) 0.00956(9) 0.00479(9) Cu2 0.01538(11) 0.01635(11) 0.01179(10) 0.00548(8) 0.00455(8) 0.00202(8) O1 0.0150(6) 0.0241(7) 0.0208(6) 0.0082(5) 0.0021(5) -0.0007(5) O2 0.0187(6) 0.0234(7) 0.0167(6) 0.0105(5) 0.0026(5) 0.0008(5) O3 0.0150(6) 0.0186(7) 0.0211(6) 0.0086(5) 0.0016(5) -0.0016(5) O4 0.0265(7) 0.0213(7) 0.0177(6) 0.0045(5) 0.0029(6) 0.0002(6) O5 0.0178(6) 0.0221(7) 0.0138(6) 0.0058(5) 0.0054(5) -0.0038(5) O6 0.0131(6) 0.0177(6) 0.0140(6) 0.0046(5) 0.0032(5) -0.0006(5) O7 0.0146(6) 0.0199(7) 0.0166(6) 0.0065(5) 0.0051(5) -0.0017(5) O8 0.0166(6) 0.0223(7) 0.0164(6) 0.0066(5) 0.0010(5) -0.0017(5) O9 0.0156(7) 0.0227(7) 0.0207(7) 0.0124(6) 0.0046(5) 0.0023(5) O10 0.0594(11) 0.0452(11) 0.0891(13) 0.0243(10) 0.0146(10) 0.0140(9) N1 0.0331(9) 0.0297(9) 0.0320(9) 0.0223(8) 0.0202(8) 0.0158(8) N2 0.0234(9) 0.0262(9) 0.0450(10) 0.0241(8) 0.0187(8) 0.0097(7) N3 0.0226(8) 0.0205(8) 0.0126(7) 0.0054(6) 0.0045(6) 0.0037(7) N4 0.0250(9) 0.0273(9) 0.0172(8) 0.0093(7) 0.0091(7) 0.0045(7) C1 0.0253(10) 0.0214(10) 0.0395(12) 0.0124(9) 0.0150(9) 0.0043(8) C2 0.0160(9) 0.0224(10) 0.0363(11) 0.0133(9) 0.0043(8) 0.0020(8) C3 0.0245(10) 0.0157(9) 0.0192(9) 0.0076(7) 0.0027(8) 0.0051(8) C4 0.0266(10) 0.0221(11) 0.0269(11) 0.0094(8) -0.0032(8) 0.0032(8) C5 0.0458(13) 0.0234(11) 0.0197(10) 0.0053(8) -0.0064(9) 0.0041(10) C6 0.0557(14) 0.0235(11) 0.0158(10) 0.0078(8) 0.0056(10) 0.0104(10) C7 0.0376(11) 0.0176(10) 0.0213(10) 0.0112(8) 0.0090(9) 0.0111(8) C8 0.0250(10) 0.0135(9) 0.0168(9) 0.0067(7) 0.0031(8) 0.0069(8) C9 0.0475(13) 0.0251(11) 0.0247(10) 0.0167(9) 0.0204(10) 0.0189(10) C10 0.0403(13) 0.0457(14) 0.0473(13) 0.0355(11) 0.0314(11) 0.0233(11) C11 0.0335(12) 0.0391(13) 0.0621(14) 0.0368(11) 0.0329(11) 0.0180(10) C12 0.0168(10) 0.0228(11) 0.0643(15) 0.0262(10) 0.0153(10) 0.0066(8) C13 0.0173(10) 0.0169(10) 0.0437(12) 0.0156(9) 0.0043(9) 0.0017(8) C14 0.0171(10) 0.0232(11) 0.0637(15) 0.0214(11) -0.0005(10) -0.0018(8) C15 0.0304(12) 0.0257(12) 0.0441(14) 0.0104(10) -0.0149(10) -0.0092(9) C16 0.0355(12) 0.0215(11) 0.0318(12) 0.0088(9) -0.0054(9) -0.0009(9) C17 0.0242(10) 0.0138(10) 0.0283(10) 0.0072(8) -0.0016(8) 0.0017(8) C18 0.0171(9) 0.0137(9) 0.0300(10) 0.0107(8) -0.0001(8) 0.0023(7) C19 0.0516(14) 0.0285(12) 0.0210(10) 0.0036(9) 0.0110(10) 0.0061(10) C20 0.0565(15) 0.0398(13) 0.0310(12) 0.0126(10) 0.0224(11) 0.0074(11) C21 0.0306(11) 0.0403(12) 0.0183(10) 0.0099(9) 0.0108(9) -0.0017(9) C22 0.0216(10) 0.0255(10) 0.0216(9) 0.0124(8) 0.0113(8) 0.0045(8) C23 0.0153(9) 0.0143(9) 0.0167(9) 0.0051(7) 0.0032(7) 0.0041(7) C24 0.0172(9) 0.0200(10) 0.0260(10) 0.0103(8) 0.0083(8) 0.0021(7) C25 0.0142(9) 0.0199(10) 0.0320(11) 0.0094(8) 0.0037(8) -0.0019(8) C26 0.0163(9) 0.0186(10) 0.0200(9) 0.0036(7) -0.0021(7) -0.0001(7) C27 0.0178(9) 0.0151(9) 0.0180(9) 0.0069(7) 0.0042(7) 0.0050(7) C28 0.0132(8) 0.0120(9) 0.0192(9) 0.0067(7) 0.0040(7) 0.0043(7) C29 0.0201(10) 0.0183(10) 0.0135(9) 0.0031(7) -0.0017(7) 0.0021(8) C30A 0.0281(17) 0.021(2) 0.0125(10) 0.0061(13) 0.0071(11) 0.0075(13) C31A 0.0298(15) 0.026(2) 0.0133(10) 0.0055(15) 0.0092(10) 0.0053(16) C32 0.0260(10) 0.0295(11) 0.0224(10) 0.0148(8) 0.0143(8) 0.0078(8) C33 0.0197(9) 0.0182(10) 0.0277(10) 0.0134(8) 0.0122(8) 0.0077(7) C34 0.0248(10) 0.0241(10) 0.0363(11) 0.0168(9) 0.0183(9) 0.0087(8) C35 0.0157(10) 0.0264(11) 0.0479(13) 0.0188(10) 0.0141(9) 0.0045(8) C36 0.0180(10) 0.0194(10) 0.0303(10) 0.0082(8) 0.0037(8) 0.0022(8) C37 0.0158(9) 0.0163(9) 0.0242(9) 0.0093(8) 0.0068(7) 0.0055(7) C38 0.0169(9) 0.0126(9) 0.0232(9) 0.0090(7) 0.0074(7) 0.0042(7) C39 0.0232(10) 0.0198(10) 0.0208(10) 0.0062(8) -0.0034(8) 0.0026(8) C40 0.0376(12) 0.0269(11) 0.0195(10) 0.0084(8) 0.0019(9) 0.0036(9) C41 0.0186(9) 0.0241(10) 0.0201(9) 0.0121(8) 0.0081(8) 0.0006(8) C42 0.0206(10) 0.0283(11) 0.0238(10) 0.0102(8) 0.0088(8) 0.0027(8) C43 0.0207(10) 0.0336(12) 0.0228(10) 0.0112(9) 0.0004(8) -0.0047(9) C44 0.0347(12) 0.0254(11) 0.0184(10) 0.0053(8) 0.0074(9) -0.0063(9) C45 0.0289(11) 0.0228(10) 0.0248(10) 0.0087(8) 0.0149(9) 0.0014(8) C46 0.0190(9) 0.0243(10) 0.0232(10) 0.0112(8) 0.0083(8) -0.0005(8) C47 0.0131(9) 0.0254(10) 0.0193(9) 0.0090(8) 0.0081(7) 0.0016(7) C48 0.0171(9) 0.0318(11) 0.0230(10) 0.0129(8) 0.0087(8) 0.0005(8) C49 0.0196(10) 0.0437(13) 0.0308(11) 0.0250(10) 0.0103(8) 0.0043(9) C50 0.0218(10) 0.0340(12) 0.0394(12) 0.0247(10) 0.0172(9) 0.0074(9) C51 0.0242(10) 0.0254(11) 0.0301(11) 0.0106(8) 0.0146(9) 0.0011(8) C52 0.0204(10) 0.0294(11) 0.0216(10) 0.0120(8) 0.0083(8) 0.0037(8) C53 0.0200(9) 0.0200(10) 0.0130(9) 0.0016(7) 0.0058(7) 0.0020(7) C54 0.0211(10) 0.0363(12) 0.0219(10) 0.0139(9) 0.0072(8) 0.0030(9) C55 0.0189(10) 0.0422(13) 0.0272(11) 0.0102(9) 0.0092(8) -0.0002(9) C56 0.0176(10) 0.0323(12) 0.0187(10) 0.0011(8) 0.0015(8) 0.0070(8) C57 0.0294(11) 0.0233(11) 0.0181(9) 0.0054(8) 0.0055(8) 0.0090(8) C58 0.0228(10) 0.0192(10) 0.0190(9) 0.0040(8) 0.0073(8) 0.0021(8) C59 0.0148(9) 0.0256(10) 0.0140(9) 0.0073(8) 0.0006(7) -0.0007(8) C60 0.0171(9) 0.0236(10) 0.0148(9) 0.0071(7) 0.0019(7) 0.0006(8) C61 0.0160(9) 0.0324(11) 0.0159(9) 0.0052(8) 0.0041(7) 0.0023(8) C62 0.0175(9) 0.0375(12) 0.0161(9) 0.0068(8) 0.0054(8) -0.0059(8) C63 0.0270(11) 0.0296(11) 0.0277(10) 0.0127(9) 0.0093(9) -0.0045(9) C64 0.0250(10) 0.0236(10) 0.0262(10) 0.0088(8) 0.0112(8) 0.0017(8) C65 0.0672(19) 0.086(2) 0.0435(15) 0.0390(15) 0.0028(14) 0.0049(16) C66 0.0298(12) 0.0346(13) 0.0480(14) 0.0208(11) 0.0116(10) -0.0021(10) C67 0.0409(14) 0.0519(16) 0.0405(13) 0.0142(12) 0.0034(11) 0.0079(12) B1 0.0173(10) 0.0228(11) 0.0165(10) 0.0079(8) 0.0061(8) 0.0015(8) C30B 0.0281(17) 0.021(2) 0.0125(10) 0.0061(13) 0.0071(11) 0.0075(13) C31B 0.0298(15) 0.026(2) 0.0133(10) 0.0055(15) 0.0092(10) 0.0053(16) _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 Rb1 O2 2.8034(11) . ? Rb1 O3 2.8090(11) . ? Rb1 O6 2.8727(11) . ? Rb1 O9 3.0637(12) 2_576 ? Rb1 O7 3.0678(11) . ? Rb1 O4 3.0920(12) . ? Rb1 O1 3.1063(11) . ? Rb1 O5 3.1094(11) . ? Rb1 O8 3.5086(12) . ? Cu1 O2 1.8981(11) . ? Cu1 O3 1.9033(11) . ? Cu1 N1 1.9255(14) . ? Cu1 N2 1.9267(15) . ? Cu2 O6 1.9214(11) . ? Cu2 O7 1.9262(11) . ? Cu2 N3 1.9427(14) . ? Cu2 N4 1.9456(14) . ? Cu2 O9 2.4044(12) . ? O1 C3 1.3800(19) . ? O1 C2 1.439(2) . ? O2 C8 1.3118(19) . ? O3 C18 1.310(2) . ? O4 C17 1.385(2) . ? O4 C19 1.431(2) . ? O5 C23 1.3788(19) . ? O5 C22 1.4395(18) . ? O6 C28 1.3158(19) . ? O7 C38 1.314(2) . ? O8 C37 1.3754(19) . ? O8 C39 1.440(2) . ? O9 Rb1 3.0637(12) 2_576 ? O9 H9A 0.817(14) . ? O9 H9B 0.807(14) . ? O10 C66 1.207(3) . ? N1 C9 1.291(2) . ? N1 C10 1.474(2) . ? N2 C12 1.287(2) . ? N2 C11 1.474(2) . ? N3 C29 1.284(2) . ? N3 C30A 1.478(3) . ? N3 C30B 1.526(8) . ? N4 C32 1.282(2) . ? N4 C31B 1.470(9) . ? N4 C31A 1.497(3) . ? C1 C2 1.497(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.381(2) . ? C3 C8 1.425(3) . ? C4 C5 1.400(3) . ? C4 H4 0.9500 . ? C5 C6 1.360(3) . ? C5 H5 0.9500 . ? C6 C7 1.416(3) . ? C6 H6 0.9500 . ? C7 C8 1.419(2) . ? C7 C9 1.435(3) . ? C9 H9 0.9500 . ? C10 C11 1.524(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.434(3) . ? C12 H12 0.9500 . ? C13 C18 1.416(3) . ? C13 C14 1.422(3) . ? C14 C15 1.359(3) . ? C14 H14 0.9500 . ? C15 C16 1.396(3) . ? C15 H15 0.9500 . ? C16 C17 1.382(2) . ? C16 H16 0.9500 . ? C17 C18 1.421(3) . ? C19 C20 1.496(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.503(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.376(2) . ? C23 C28 1.428(2) . ? C24 C25 1.404(2) . ? C24 H24 0.9500 . ? C25 C26 1.365(2) . ? C25 H25 0.9500 . ? C26 C27 1.414(2) . ? C26 H26 0.9500 . ? C27 C28 1.414(2) . ? C27 C29 1.445(2) . ? C29 H29 0.9500 . ? C30A C31A 1.525(4) . ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32 C33 1.446(2) . ? C32 H32 0.9500 . ? C33 C34 1.418(2) . ? C33 C38 1.421(2) . ? C34 C35 1.361(3) . ? C34 H34 0.9500 . ? C35 C36 1.405(3) . ? C35 H35 0.9500 . ? C36 C37 1.370(2) . ? C36 H36 0.9500 . ? C37 C38 1.427(2) . ? C39 C40 1.502(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C46 1.395(2) . ? C41 C42 1.414(2) . ? C41 B1 1.643(3) . ? C42 C43 1.391(2) . ? C42 H42 0.9500 . ? C43 C44 1.378(3) . ? C43 H43 0.9500 . ? C44 C45 1.387(3) . ? C44 H44 0.9500 . ? C45 C46 1.396(2) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.402(2) . ? C47 C52 1.403(2) . ? C47 B1 1.640(3) . ? C48 C49 1.390(3) . ? C48 H48 0.9500 . ? C49 C50 1.383(3) . ? C49 H49 0.9500 . ? C50 C51 1.388(3) . ? C50 H50 0.9500 . ? C51 C52 1.386(3) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C58 1.399(2) . ? C53 C54 1.405(2) . ? C53 B1 1.655(3) . ? C54 C55 1.391(3) . ? C54 H54 0.9500 . ? C55 C56 1.384(3) . ? C55 H55 0.9500 . ? C56 C57 1.376(3) . ? C56 H56 0.9500 . ? C57 C58 1.393(2) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.398(2) . ? C59 C64 1.404(2) . ? C59 B1 1.659(2) . ? C60 C61 1.389(2) . ? C60 H60 0.9500 . ? C61 C62 1.376(3) . ? C61 H61 0.9500 . ? C62 C63 1.383(3) . ? C62 H62 0.9500 . ? C63 C64 1.387(2) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C66 1.481(3) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.489(3) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C30B C31B 1.505(13) . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? 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 Rb1 O3 55.93(3) . . ? O2 Rb1 O6 81.64(3) . . ? O3 Rb1 O6 124.64(3) . . ? O2 Rb1 O9 125.91(3) . 2_576 ? O3 Rb1 O9 117.44(3) . 2_576 ? O6 Rb1 O9 58.77(3) . 2_576 ? O2 Rb1 O7 70.71(3) . . ? O3 Rb1 O7 77.67(3) . . ? O6 Rb1 O7 53.86(3) . . ? O9 Rb1 O7 56.65(3) 2_576 . ? O2 Rb1 O4 102.20(3) . . ? O3 Rb1 O4 52.30(3) . . ? O6 Rb1 O4 167.69(3) . . ? O9 Rb1 O4 110.65(3) 2_576 . ? O7 Rb1 O4 116.01(3) . . ? O2 Rb1 O1 52.26(3) . . ? O3 Rb1 O1 101.81(3) . . ? O6 Rb1 O1 69.75(3) . . ? O9 Rb1 O1 126.73(3) 2_576 . ? O7 Rb1 O1 103.29(3) . . ? O4 Rb1 O1 121.89(3) . . ? O2 Rb1 O5 122.22(3) . . ? O3 Rb1 O5 174.94(3) . . ? O6 Rb1 O5 50.73(3) . . ? O9 Rb1 O5 59.14(3) 2_576 . ? O7 Rb1 O5 97.28(3) . . ? O4 Rb1 O5 131.63(3) . . ? O1 Rb1 O5 78.80(3) . . ? O2 Rb1 O8 97.73(3) . . ? O3 Rb1 O8 63.39(3) . . ? O6 Rb1 O8 93.14(3) . . ? O9 Rb1 O8 54.25(3) 2_576 . ? O7 Rb1 O8 45.77(3) . . ? O4 Rb1 O8 74.81(3) . . ? O1 Rb1 O8 146.22(3) . . ? O5 Rb1 O8 113.38(3) . . ? O2 Rb1 C18 73.21(4) . . ? O3 Rb1 C18 17.33(3) . . ? O6 Rb1 C18 133.92(4) . . ? O9 Rb1 C18 107.59(4) 2_576 . ? O7 Rb1 C18 81.26(4) . . ? O4 Rb1 C18 39.50(4) . . ? O1 Rb1 C18 117.82(3) . . ? O5 Rb1 C18 163.28(3) . . ? O8 Rb1 C18 54.21(3) . . ? O2 Rb1 Cu1 30.16(2) . . ? O3 Rb1 Cu1 30.29(2) . . ? O6 Rb1 Cu1 96.22(2) . . ? O9 Rb1 Cu1 114.56(2) 2_576 . ? O7 Rb1 Cu1 60.21(2) . . ? O4 Rb1 Cu1 82.36(2) . . ? O1 Rb1 Cu1 82.14(2) . . ? O5 Rb1 Cu1 146.01(2) . . ? O8 Rb1 Cu1 70.665(19) . . ? C18 Rb1 Cu1 46.13(3) . . ? O2 Rb1 C28 85.66(3) . . ? O3 Rb1 C28 137.30(3) . . ? O6 Rb1 C28 18.11(3) . . ? O9 Rb1 C28 68.09(3) 2_576 . ? O7 Rb1 C28 71.89(3) . . ? O4 Rb1 C28 170.23(3) . . ? O1 Rb1 C28 58.65(3) . . ? O5 Rb1 C28 38.96(3) . . ? O8 Rb1 C28 110.20(3) . . ? C18 Rb1 C28 150.19(4) . . ? Cu1 Rb1 C28 107.10(3) . . ? O2 Cu1 O3 87.63(5) . . ? O2 Cu1 N1 94.08(6) . . ? O3 Cu1 N1 178.27(6) . . ? O2 Cu1 N2 176.92(6) . . ? O3 Cu1 N2 93.15(6) . . ? N1 Cu1 N2 85.13(7) . . ? O2 Cu1 Rb1 47.90(3) . . ? O3 Cu1 Rb1 48.11(3) . . ? N1 Cu1 Rb1 133.49(5) . . ? N2 Cu1 Rb1 134.24(5) . . ? O6 Cu2 O7 88.98(5) . . ? O6 Cu2 N3 93.07(5) . . ? O7 Cu2 N3 171.83(6) . . ? O6 Cu2 N4 175.71(6) . . ? O7 Cu2 N4 93.03(5) . . ? N3 Cu2 N4 84.42(6) . . ? O6 Cu2 O9 91.12(4) . . ? O7 Cu2 O9 92.09(5) . . ? N3 Cu2 O9 95.78(5) . . ? N4 Cu2 O9 92.59(5) . . ? O6 Cu2 Rb1 46.64(3) . . ? O7 Cu2 Rb1 52.58(3) . . ? N3 Cu2 Rb1 124.63(4) . . ? N4 Cu2 Rb1 132.70(5) . . ? O9 Cu2 Rb1 116.84(3) . . ? C3 O1 C2 116.34(13) . . ? C3 O1 Rb1 114.71(10) . . ? C2 O1 Rb1 124.01(10) . . ? C8 O2 Cu1 127.17(10) . . ? C8 O2 Rb1 125.65(10) . . ? Cu1 O2 Rb1 101.94(4) . . ? C18 O3 Cu1 127.48(11) . . ? C18 O3 Rb1 123.00(10) . . ? Cu1 O3 Rb1 101.60(4) . . ? C17 O4 C19 116.95(14) . . ? C17 O4 Rb1 113.46(10) . . ? C19 O4 Rb1 125.36(11) . . ? C23 O5 C22 117.63(12) . . ? C23 O5 Rb1 112.91(9) . . ? C22 O5 Rb1 123.21(9) . . ? C28 O6 Cu2 126.38(10) . . ? C28 O6 Rb1 119.17(9) . . ? Cu2 O6 Rb1 104.27(4) . . ? C38 O7 Cu2 126.85(10) . . ? C38 O7 Rb1 126.26(10) . . ? Cu2 O7 Rb1 97.51(4) . . ? C37 O8 C39 117.16(13) . . ? C37 O8 Rb1 112.06(9) . . ? C39 O8 Rb1 123.86(9) . . ? Cu2 O9 Rb1 174.37(5) . 2_576 ? Cu2 O9 H9A 101.6(11) . . ? Rb1 O9 H9A 72.9(11) 2_576 . ? Cu2 O9 H9B 108.3(12) . . ? Rb1 O9 H9B 74.7(11) 2_576 . ? H9A O9 H9B 108.2(18) . . ? C9 N1 C10 120.00(15) . . ? C9 N1 Cu1 125.36(13) . . ? C10 N1 Cu1 114.64(13) . . ? C12 N2 C11 119.32(17) . . ? C12 N2 Cu1 126.19(13) . . ? C11 N2 Cu1 114.49(13) . . ? C29 N3 C30A 118.80(18) . . ? C29 N3 C30B 120.9(4) . . ? C29 N3 Cu2 126.98(12) . . ? C30A N3 Cu2 113.92(15) . . ? C30B N3 Cu2 109.3(4) . . ? C32 N4 C31B 117.2(4) . . ? C32 N4 C31A 121.35(18) . . ? C32 N4 Cu2 126.95(12) . . ? C31B N4 Cu2 114.2(4) . . ? C31A N4 Cu2 110.57(15) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 107.98(14) . . ? O1 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O1 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C4 C3 O1 124.25(17) . . ? C4 C3 C8 121.26(16) . . ? O1 C3 C8 114.49(14) . . ? C3 C4 C5 120.24(19) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 120.11(18) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 121.20(18) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C8 119.76(18) . . ? C6 C7 C9 117.81(16) . . ? C8 C7 C9 122.42(17) . . ? O2 C8 C7 124.49(16) . . ? O2 C8 C3 118.10(14) . . ? C7 C8 C3 117.41(16) . . ? C7 C8 Rb1 150.15(12) . . ? C3 C8 Rb1 85.89(10) . . ? N1 C9 C7 126.20(16) . . ? N1 C9 H9 116.9 . . ? C7 C9 H9 116.9 . . ? N1 C10 C11 109.78(15) . . ? N1 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N1 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C10 110.04(16) . . ? N2 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N2 C12 C13 126.01(17) . . ? N2 C12 H12 117.0 . . ? C13 C12 H12 117.0 . . ? C18 C13 C14 120.00(18) . . ? C18 C13 C12 121.92(17) . . ? C14 C13 C12 117.94(18) . . ? C15 C14 C13 121.00(19) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.79(19) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.8(2) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 O4 124.36(17) . . ? C16 C17 C18 121.14(18) . . ? O4 C17 C18 114.50(15) . . ? O3 C18 C13 124.75(16) . . ? O3 C18 C17 118.01(16) . . ? C13 C18 C17 117.23(16) . . ? C13 C18 Rb1 148.19(12) . . ? C17 C18 Rb1 85.91(10) . . ? O4 C19 C20 108.33(16) . . ? O4 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? O4 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 C21 106.36(13) . . ? O5 C22 H22A 110.5 . . ? C21 C22 H22A 110.5 . . ? O5 C22 H22B 110.5 . . ? C21 C22 H22B 110.5 . . ? H22A C22 H22B 108.6 . . ? C24 C23 O5 125.11(15) . . ? C24 C23 C28 122.19(15) . . ? O5 C23 C28 112.69(14) . . ? C23 C24 C25 119.78(16) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 119.69(16) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 121.54(16) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C26 C27 C28 119.95(15) . . ? C26 C27 C29 117.63(15) . . ? C28 C27 C29 122.42(15) . . ? O6 C28 C27 125.58(15) . . ? O6 C28 C23 117.59(14) . . ? C27 C28 C23 116.83(15) . . ? C27 C28 Rb1 143.91(11) . . ? C23 C28 Rb1 85.66(9) . . ? N3 C29 C27 125.15(15) . . ? N3 C29 H29 117.4 . . ? C27 C29 H29 117.4 . . ? N3 C30A C31A 106.2(2) . . ? N3 C30A H30A 110.5 . . ? C31A C30A H30A 110.5 . . ? N3 C30A H30B 110.5 . . ? C31A C30A H30B 110.5 . . ? H30A C30A H30B 108.7 . . ? N4 C31A C30A 107.3(2) . . ? N4 C31A H31A 110.3 . . ? C30A C31A H31A 110.3 . . ? N4 C31A H31B 110.3 . . ? C30A C31A H31B 110.3 . . ? H31A C31A H31B 108.5 . . ? N4 C32 C33 125.42(16) . . ? N4 C32 H32 117.3 . . ? C33 C32 H32 117.3 . . ? C34 C33 C38 119.88(16) . . ? C34 C33 C32 117.61(15) . . ? C38 C33 C32 122.48(15) . . ? C35 C34 C33 121.31(17) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C34 C35 C36 119.60(17) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C37 C36 C35 120.58(17) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 O8 124.97(16) . . ? C36 C37 C38 121.71(16) . . ? O8 C37 C38 113.31(14) . . ? O7 C38 C33 125.15(15) . . ? O7 C38 C37 117.96(14) . . ? C33 C38 C37 116.89(15) . . ? O8 C39 C40 107.41(14) . . ? O8 C39 H39A 110.2 . . ? C40 C39 H39A 110.2 . . ? O8 C39 H39B 110.2 . . ? C40 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C46 C41 C42 115.15(16) . . ? C46 C41 B1 124.61(15) . . ? C42 C41 B1 120.24(16) . . ? C43 C42 C41 122.31(17) . . ? C43 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? C44 C43 C42 120.65(17) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 118.83(17) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C44 C45 C46 120.12(18) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 122.87(17) . . ? C41 C46 H46 118.6 . . ? C45 C46 H46 118.6 . . ? C48 C47 C52 114.55(17) . . ? C48 C47 B1 124.67(16) . . ? C52 C47 B1 120.77(15) . . ? C49 C48 C47 123.07(17) . . ? C49 C48 H48 118.5 . . ? C47 C48 H48 118.5 . . ? C50 C49 C48 120.43(17) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 118.38(18) . . ? C49 C50 H50 120.8 . . ? C51 C50 H50 120.8 . . ? C52 C51 C50 120.34(18) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C47 123.19(17) . . ? C51 C52 H52 118.4 . . ? C47 C52 H52 118.4 . . ? C58 C53 C54 114.50(16) . . ? C58 C53 B1 123.86(15) . . ? C54 C53 B1 121.50(15) . . ? C55 C54 C53 123.13(18) . . ? C55 C54 H54 118.4 . . ? C53 C54 H54 118.4 . . ? C56 C55 C54 120.15(18) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C57 C56 C55 118.68(17) . . ? C57 C56 H56 120.7 . . ? C55 C56 H56 120.7 . . ? C56 C57 C58 120.51(18) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C57 C58 C53 123.03(17) . . ? C57 C58 H58 118.5 . . ? C53 C58 H58 118.5 . . ? C60 C59 C64 114.41(16) . . ? C60 C59 B1 125.25(16) . . ? C64 C59 B1 120.22(15) . . ? C61 C60 C59 123.12(17) . . ? C61 C60 H60 118.4 . . ? C59 C60 H60 118.4 . . ? C62 C61 C60 120.37(17) . . ? C62 C61 H61 119.8 . . ? C60 C61 H61 119.8 . . ? C61 C62 C63 118.82(17) . . ? C61 C62 H62 120.6 . . ? C63 C62 H62 120.6 . . ? C62 C63 C64 120.02(19) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C59 123.25(18) . . ? C63 C64 H64 118.4 . . ? C59 C64 H64 118.4 . . ? C66 C65 H65A 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C66 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? O10 C66 C65 122.0(2) . . ? O10 C66 C67 121.2(2) . . ? C65 C66 C67 116.8(2) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C47 B1 C41 111.36(14) . . ? C47 B1 C53 109.07(14) . . ? C41 B1 C53 108.86(14) . . ? C47 B1 C59 110.13(14) . . ? C41 B1 C59 105.38(14) . . ? C53 B1 C59 112.02(14) . . ? C31B C30B N3 107.6(6) . . ? C31B C30B H30C 110.2 . . ? N3 C30B H30C 110.2 . . ? C31B C30B H30D 110.2 . . ? N3 C30B H30D 110.2 . . ? H30C C30B H30D 108.5 . . ? N4 C31B C30B 105.6(6) . . ? N4 C31B H31C 110.6 . . ? C30B C31B H31C 110.6 . . ? N4 C31B H31D 110.6 . . ? C30B C31B H31D 110.6 . . ? H31C C31B H31D 108.7 . . ? 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 O9 H9A O5 0.817(14) 2.439(16) 3.0464(17) 131.9(16) 2_576 O9 H9A O6 0.817(14) 2.206(15) 2.9175(16) 145.6(16) 2_576 O9 H9B O7 0.807(14) 2.239(16) 2.9093(16) 140.8(16) 2_576 O9 H9B O8 0.807(14) 2.334(16) 3.0224(17) 143.8(17) 2_576 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.306 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.050