# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Laurence K. Thompson' _publ_contact_author_email lk.thompson@mun.ca loop_ _publ_author_name M.U.Anwar L.K.Thompson L.N.Dawe data_MUA435-T2 _database_code_depnum_ccdc_archive 'CCDC 794936' _publ_section_abstract ; Please see full paper. ; # start Validation Reply Form _vrf_CHEMW03_MUA435-T2 ; PROBLEM: WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 RESPONSE: Platon's SQUEEZE application was used in the modeling of this system. Electron density corresponding to five methanol molecules was recovered. These have been included in the formula for the calculation of intensive properties. Please see platon_squeeze_details for further information. ; _vrf_DIFMX01_MUA435-T2 ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 RESPONSE: This does not indicate a model error. The locations of the maximum and minimum residual electron density are: Highest peak 4.17 at -0.0026 0.1635 0.5037 [ 0.86 A from CU1 ] Deepest hole -2.22 at 0.9410 0.1651 0.4528 [ 0.74 A from CU1 ] ; _vrf_PLAT241_MUA435-T2 ; PROBLEM: Check High Ueq as Compared to Neighbors for O37 RESPONSE: This atom is part of a nitrate anion or methanol molecule (since Platon is using this VRF response for different moieties) and does not indicate that an atom as been incorrectly assigned. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H37 Cu6 N17 O25, C30 H38 Cu6 N16 O23, 5(C H4 O)' _chemical_formula_sum 'C65 H95 Cu12 N33 O53' _chemical_formula_weight 2949.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.1537(17) _cell_length_b 16.6970(12) _cell_length_c 23.612(2) _cell_angle_alpha 70.172(10) _cell_angle_beta 82.242(12) _cell_angle_gamma 67.126(9) _cell_volume 5519.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 21375 _cell_measurement_theta_min 2.0163 _cell_measurement_theta_max 28.7304 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Green' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 2.367 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.8230 _exptl_absorpt_correction_T_min 0.5842 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 55342 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.50 _reflns_number_total 20363 _reflns_number_gt 16645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXL-97 (Acta Cryst. 2008. A64, 112-122)' _computing_structure_refinement 'SHELXL-97 (Acta Cryst. 2008. A64, 112-122)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.2000P)^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 20363 _refine_ls_number_parameters 1379 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.1087 _refine_ls_wR_factor_ref 0.3498 _refine_ls_wR_factor_gt 0.3281 _refine_ls_goodness_of_fit_ref 1.413 _refine_ls_restrained_S_all 1.428 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.504 -0.250 0.246 440 92 '5 CH3OH ' 2 0.504 0.250 0.754 440 92 '5 CH3OH ' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 184 electrons per unit cell in two voids (total volume 880 ^A^3); that is 92 electrons per asymmetric unit. Disordered solvent lattice methanol molecules were present prior to the application of Squeeze, however, a satisfactory point atom model could not be achieved. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 0.03796(7) 0.83410(7) 0.52141(5) 0.0635(3) Uani 1 1 d . . . Cu2 Cu 0.25004(6) 0.90717(6) 0.37178(4) 0.0462(3) Uani 1 1 d . . . Cu3 Cu 0.27948(6) 0.92333(7) 0.03080(4) 0.0490(3) Uani 1 1 d . . . Cu4 Cu 0.30331(5) 0.92392(6) 0.23106(4) 0.0430(2) Uani 1 1 d . . . Cu5 Cu 0.59840(5) 1.11688(6) 0.34415(4) 0.0417(2) Uani 1 1 d . . . Cu6 Cu 0.39071(6) 1.00497(8) 0.30302(4) 0.0521(3) Uani 1 1 d . . . Cu7 Cu 0.28041(6) 0.41654(7) 0.52434(5) 0.0521(3) Uani 1 1 d . . . Cu8 Cu 0.29982(6) 0.41309(6) 0.72610(4) 0.0465(3) Uani 1 1 d . . . Cu9 Cu 0.01189(7) 0.33722(7) 1.00639(5) 0.0598(3) Uani 1 1 d . . . Cu10 Cu 0.24336(6) 0.39218(7) 0.86751(4) 0.0508(3) Uani 1 1 d . . . Cu11 Cu 0.59025(5) 0.60882(6) 0.84096(3) 0.0409(2) Uani 1 1 d . . . Cu12 Cu 0.39171(6) 0.48207(8) 0.80307(4) 0.0519(3) Uani 1 1 d . . . O1 O 0.0549(4) 0.8099(4) 0.4423(3) 0.0654(16) Uani 1 1 d . . . O2 O 0.2184(4) 0.8649(4) 0.2663(2) 0.0510(12) Uani 1 1 d . . . O3 O 0.3683(3) 0.9635(3) 0.0543(2) 0.0425(10) Uani 1 1 d . . . O4 O 0.4358(3) 1.0092(4) 0.2226(2) 0.0501(12) Uani 1 1 d . . . O5 O 0.5029(3) 1.0914(4) 0.4019(2) 0.0522(13) Uani 1 1 d . . . O6 O 0.2849(4) 0.9706(5) 0.4138(2) 0.0632(16) Uani 1 1 d . . . O7 O 0.3719(3) 0.4507(4) 0.5510(2) 0.0494(12) Uani 1 1 d . . . O8 O 0.4349(3) 0.4905(4) 0.7220(2) 0.0490(12) Uani 1 1 d . . . O9 O 0.0257(4) 0.3244(4) 0.9250(3) 0.0693(17) Uani 1 1 d . . . O10 O 0.2073(4) 0.3612(4) 0.7581(3) 0.0579(14) Uani 1 1 d . . . O11 O 0.5008(3) 0.5709(5) 0.9024(2) 0.0580(14) Uani 1 1 d . . . O12 O 0.2885(4) 0.4402(5) 0.9140(2) 0.0664(17) Uani 1 1 d . . . O13 O 0.3444(3) 0.9090(4) 0.3099(2) 0.0512(12) Uani 1 1 d . . . O14 O 0.3372(3) 0.3940(4) 0.8063(2) 0.0502(12) Uani 1 1 d . . . O15 O -0.0414(5) 0.7696(5) 0.5646(3) 0.090(2) Uani 1 1 d . . . O16 O -0.1327(6) 0.8818(6) 0.4990(4) 0.111(3) Uani 1 1 d . . . O17 O -0.1774(6) 0.7789(7) 0.5602(5) 0.125(4) Uani 1 1 d . . . O18 O 0.3073(4) 0.9505(5) -0.0556(3) 0.0614(15) Uani 1 1 d . . . O19 O 0.2928(6) 1.0684(8) -0.1325(4) 0.121(4) Uani 1 1 d . . . O20 O 0.2212(6) 1.0872(6) -0.0520(4) 0.095(2) Uani 1 1 d . . . O21 O 0.1849(3) 1.0615(4) 0.2339(3) 0.0617(15) Uani 1 1 d . . . O22 O 0.2499(5) 1.1229(5) 0.2688(4) 0.089(2) Uani 1 1 d . . . O23 O 0.1319(8) 1.2046(7) 0.2196(7) 0.162(6) Uani 1 1 d . . . O24 O 0.6668(3) 1.1351(4) 0.3979(2) 0.0505(12) Uani 1 1 d . . . O25 O 0.6616(5) 1.2315(5) 0.4419(3) 0.0734(17) Uani 1 1 d . . . O26 O 0.5658(4) 1.2706(4) 0.3720(3) 0.0652(15) Uani 1 1 d . . . O27 O 0.7100(4) 0.9780(4) 0.3577(3) 0.0690(16) Uani 1 1 d U . . O28 O 0.6192(8) 0.9059(7) 0.4053(5) 0.126(3) Uani 1 1 d U . . O29 O 0.7598(9) 0.8303(7) 0.3977(7) 0.186(5) Uani 1 1 d U . . O30 O 0.3098(5) 0.4503(6) 0.4393(3) 0.0727(19) Uani 1 1 d . . . O31 O 0.2174(5) 0.5794(6) 0.4435(4) 0.089(2) Uani 1 1 d . . . O32 O 0.2925(6) 0.5679(9) 0.3621(3) 0.126(4) Uani 1 1 d . . . O33 O 0.1939(4) 0.5602(5) 0.7144(4) 0.085(2) Uani 1 1 d U . . O34 O 0.2396(5) 0.5999(6) 0.7776(4) 0.098(3) Uani 1 1 d U . . O35 O 0.1686(8) 0.7000(6) 0.7015(5) 0.138(5) Uani 1 1 d U . . O36 O -0.0867(6) 0.2922(6) 1.0369(4) 0.089(2) Uani 1 1 d U . . O37 O -0.1627(6) 0.4052(7) 0.9628(6) 0.168(5) Uani 1 1 d U . . O38 O -0.2129(5) 0.3019(6) 1.0137(5) 0.127(4) Uani 1 1 d U . . O39 O 0.6638(3) 0.6292(4) 0.8892(2) 0.0519(12) Uani 1 1 d . . . O40 O 0.5490(4) 0.7571(4) 0.8761(3) 0.0657(15) Uani 1 1 d . . . O41 O 0.6603(5) 0.7288(5) 0.9307(3) 0.0761(19) Uani 1 1 d . . . O42 O 0.1453(6) 0.7103(5) 0.5776(4) 0.107(3) Uani 1 1 d . . . O43 O 0.3521(6) 0.7731(6) 0.4322(4) 0.107(3) Uani 1 1 d . . . O44 O 0.3717(5) 0.7781(5) 0.0523(3) 0.083(2) Uani 1 1 d . . . O45 O 0.3633(6) 0.2741(6) 0.5313(5) 0.120(3) Uani 1 1 d U . . O46 O 0.1011(4) 0.1979(4) 1.0519(3) 0.0744(17) Uani 1 1 d . . . O47 O 0.3262(6) 0.2317(6) 0.9032(4) 0.104(3) Uani 1 1 d U . . O48 O 0.7011(6) 0.4690(5) 0.8574(5) 0.121(4) Uani 1 1 d . . . N1 N 0.0386(4) 0.8928(5) 0.5824(3) 0.0600(18) Uani 1 1 d . . . N2 N 0.1219(4) 0.8928(4) 0.4830(3) 0.0524(16) Uani 1 1 d . . . N3 N 0.1512(4) 0.8855(4) 0.4258(3) 0.0483(14) Uani 1 1 d . . . N4 N 0.1936(4) 0.8664(4) 0.3233(3) 0.0513(15) Uani 1 1 d . . . N5 N 0.1650(4) 0.9020(5) 0.0330(3) 0.0574(17) Uani 1 1 d . . . N6 N 0.2465(4) 0.9128(4) 0.1134(3) 0.0459(13) Uani 1 1 d . . . N7 N 0.2973(4) 0.9305(4) 0.1462(3) 0.0447(13) Uani 1 1 d . . . N8 N 0.3935(4) 0.9809(4) 0.1922(3) 0.0453(13) Uani 1 1 d . . . N9 N 0.6488(4) 1.1663(4) 0.2622(3) 0.0442(13) Uani 1 1 d . . . N10 N 0.5280(4) 1.0969(4) 0.2932(3) 0.0470(14) Uani 1 1 d . . . N11 N 0.4643(4) 1.0638(5) 0.3220(3) 0.0499(14) Uani 1 1 d . . . N12 N 0.3511(4) 1.0008(6) 0.3865(3) 0.0574(17) Uani 1 1 d . . . N13 N 0.1629(5) 0.3979(5) 0.5260(3) 0.0598(17) Uani 1 1 d . . . N14 N 0.2484(4) 0.3995(4) 0.6088(3) 0.0482(14) Uani 1 1 d . . . N15 N 0.3011(4) 0.4136(4) 0.6431(3) 0.0482(14) Uani 1 1 d . . . N16 N 0.3941(4) 0.4627(4) 0.6914(3) 0.0478(14) Uani 1 1 d . . . N17 N 0.0181(4) 0.3845(4) 1.0718(3) 0.0583(17) Uani 1 1 d . . . N18 N 0.1072(4) 0.3839(4) 0.9745(3) 0.0553(17) Uani 1 1 d . . . N19 N 0.1383(4) 0.3791(5) 0.9192(3) 0.0517(15) Uani 1 1 d . . . N20 N 0.1809(4) 0.3633(4) 0.8139(3) 0.0515(15) Uani 1 1 d . . . N21 N 0.6348(4) 0.6615(4) 0.7579(2) 0.0415(12) Uani 1 1 d . . . N22 N 0.5213(4) 0.5830(4) 0.7925(2) 0.0415(12) Uani 1 1 d . . . N23 N 0.4609(4) 0.5456(5) 0.8218(2) 0.0456(14) Uani 1 1 d . . . N24 N 0.3519(4) 0.4754(5) 0.8862(3) 0.0561(18) Uani 1 1 d . . . N25 N -0.1200(6) 0.8120(6) 0.5416(4) 0.077(2) Uani 1 1 d . . . N26 N 0.2736(6) 1.0377(7) -0.0821(4) 0.078(2) Uani 1 1 d . . . N27 N 0.1904(5) 1.1298(5) 0.2412(3) 0.0590(16) Uani 1 1 d . . . N28 N 0.6291(4) 1.2160(4) 0.4026(3) 0.0486(14) Uani 1 1 d . . . N29 N 0.2712(5) 0.5375(7) 0.4118(4) 0.072(2) Uani 1 1 d . . . N30 N 0.2018(4) 0.6200(5) 0.7326(3) 0.0581(15) Uani 1 1 d U . . N31 N -0.1573(6) 0.3366(7) 1.0035(6) 0.108(3) Uani 1 1 d U . . N32 N 0.6222(4) 0.7083(5) 0.8996(3) 0.0512(15) Uani 1 1 d . . . N33 N 0.6964(9) 0.9072(7) 0.3870(6) 0.109(3) Uani 1 1 d U . . C1 C -0.0098(6) 0.8932(7) 0.6328(4) 0.074(3) Uani 1 1 d . . . H1 H -0.0555 0.8683 0.6405 0.088 Uiso 1 1 calc R . . C2 C 0.0040(7) 0.9285(9) 0.6743(4) 0.083(3) Uani 1 1 d . . . H2 H -0.0309 0.9270 0.7102 0.099 Uiso 1 1 calc R . . C3 C 0.0698(5) 0.9662(8) 0.6624(4) 0.073(3) Uani 1 1 d . . . H3 H 0.0798 0.9933 0.6890 0.088 Uiso 1 1 calc R . . C4 C 0.1214(6) 0.9630(8) 0.6096(4) 0.071(3) Uani 1 1 d . . . H4 H 0.1692 0.9850 0.6012 0.085 Uiso 1 1 calc R . . C5 C 0.1025(5) 0.9281(6) 0.5702(3) 0.061(2) Uani 1 1 d . . . C6 C 0.1496(5) 0.9274(5) 0.5127(3) 0.0521(17) Uani 1 1 d . . . H6 H 0.1963 0.9507 0.4991 0.063 Uiso 1 1 calc R . . C7 C 0.1099(5) 0.8436(6) 0.4098(4) 0.0566(19) Uani 1 1 d . . . C8 C 0.1320(6) 0.8345(6) 0.3482(4) 0.058(2) Uani 1 1 d . . . C9 C 0.0882(8) 0.7912(9) 0.3220(5) 0.087(4) Uani 1 1 d . . . H9A H 0.0709 0.8288 0.2803 0.105 Uiso 1 1 calc R . . H9B H 0.0346 0.7865 0.3456 0.105 Uiso 1 1 calc R . . H9C H 0.1304 0.7299 0.3228 0.105 Uiso 1 1 calc R . . C10 C 0.1235(7) 0.8963(8) -0.0112(6) 0.081(3) Uani 1 1 d . . . H10 H 0.1499 0.9038 -0.0502 0.097 Uiso 1 1 calc R . . C11 C 0.0453(7) 0.8802(8) -0.0015(6) 0.081(3) Uani 1 1 d . . . H11 H 0.0164 0.8797 -0.0338 0.098 Uiso 1 1 calc R . . C12 C 0.0082(6) 0.8644(7) 0.0562(6) 0.077(3) Uani 1 1 d . . . H12 H -0.0465 0.8537 0.0637 0.093 Uiso 1 1 calc R . . C13 C 0.0521(6) 0.8646(7) 0.1016(5) 0.072(3) Uani 1 1 d . . . H13 H 0.0303 0.8499 0.1417 0.087 Uiso 1 1 calc R . . C14 C 0.1280(5) 0.8861(6) 0.0892(5) 0.061(2) Uani 1 1 d . . . C15 C 0.1764(5) 0.8923(6) 0.1352(4) 0.0529(17) Uani 1 1 d . . . H15 H 0.1584 0.8825 0.1762 0.063 Uiso 1 1 calc R . . C16 C 0.3590(4) 0.9589(4) 0.1104(3) 0.0377(13) Uani 1 1 d . . . C17 C 0.4148(4) 0.9873(5) 0.1367(3) 0.0398(14) Uani 1 1 d . . . C18 C 0.4827(5) 1.0256(5) 0.1037(3) 0.0483(16) Uani 1 1 d . . . H18A H 0.4541 1.0923 0.0871 0.058 Uiso 1 1 calc R . . H18B H 0.5081 0.9996 0.0709 0.058 Uiso 1 1 calc R . . H18C H 0.5307 1.0101 0.1314 0.058 Uiso 1 1 calc R . . C19 C 0.7090(5) 1.2075(5) 0.2490(4) 0.0535(18) Uani 1 1 d . . . H19 H 0.7309 1.2182 0.2801 0.064 Uiso 1 1 calc R . . C20 C 0.7399(6) 1.2349(6) 0.1896(4) 0.063(2) Uani 1 1 d . . . H20 H 0.7799 1.2669 0.1800 0.076 Uiso 1 1 calc R . . C21 C 0.7114(6) 1.2145(7) 0.1452(4) 0.062(2) Uani 1 1 d . . . H21 H 0.7324 1.2312 0.1050 0.075 Uiso 1 1 calc R . . C22 C 0.6513(6) 1.1691(6) 0.1610(4) 0.0562(19) Uani 1 1 d . . . H22 H 0.6327 1.1522 0.1317 0.067 Uiso 1 1 calc R . . C23 C 0.6189(5) 1.1489(5) 0.2190(3) 0.0431(14) Uani 1 1 d . . . C24 C 0.5498(5) 1.1087(5) 0.2377(3) 0.0481(16) Uani 1 1 d . . . H24 H 0.5237 1.0930 0.2113 0.058 Uiso 1 1 calc R . . C25 C 0.4572(5) 1.0628(6) 0.3797(3) 0.0504(17) Uani 1 1 d . . . C26 C 0.3865(5) 1.0327(6) 0.4163(3) 0.0549(19) Uani 1 1 d . . . C27 C 0.3681(6) 1.0311(8) 0.4788(3) 0.068(2) Uani 1 1 d . . . H27A H 0.3316 1.0931 0.4800 0.081 Uiso 1 1 calc R . . H27B H 0.4249 1.0090 0.4998 0.081 Uiso 1 1 calc R . . H27C H 0.3354 0.9902 0.4985 0.081 Uiso 1 1 calc R . . C28 C 0.1220(6) 0.4023(8) 0.4780(5) 0.076(3) Uani 1 1 d . . . H28 H 0.1475 0.4160 0.4389 0.092 Uiso 1 1 calc R . . C29 C 0.0402(7) 0.3859(8) 0.4869(5) 0.080(3) Uani 1 1 d . . . H29 H 0.0087 0.3908 0.4540 0.096 Uiso 1 1 calc R . . C30 C 0.0078(7) 0.3621(8) 0.5461(6) 0.085(3) Uani 1 1 d . . . H30 H -0.0466 0.3508 0.5534 0.102 Uiso 1 1 calc R . . C31 C 0.0526(6) 0.3551(7) 0.5925(5) 0.066(2) Uani 1 1 d . . . H31 H 0.0319 0.3356 0.6325 0.079 Uiso 1 1 calc R . . C32 C 0.1299(5) 0.3768(6) 0.5817(5) 0.063(2) Uani 1 1 d . . . C33 C 0.1780(5) 0.3788(5) 0.6276(4) 0.0539(18) Uani 1 1 d . . . H33 H 0.1597 0.3660 0.6686 0.065 Uiso 1 1 calc R . . C34 C 0.3626(4) 0.4437(5) 0.6063(3) 0.0417(14) Uani 1 1 d . . . C35 C 0.4160(4) 0.4727(5) 0.6361(3) 0.0421(14) Uani 1 1 d . . . C36 C 0.4828(5) 0.5137(5) 0.6034(3) 0.0481(16) Uani 1 1 d . . . H36A H 0.4659 0.5748 0.6070 0.058 Uiso 1 1 calc R . . H36B H 0.4839 0.5184 0.5608 0.058 Uiso 1 1 calc R . . H36C H 0.5425 0.4747 0.6208 0.058 Uiso 1 1 calc R . . C37 C -0.0309(6) 0.3845(6) 1.1224(4) 0.064(2) Uani 1 1 d . . . H37 H -0.0816 0.3672 1.1276 0.077 Uiso 1 1 calc R . . C38 C -0.0098(7) 0.4089(8) 1.1670(5) 0.078(3) Uani 1 1 d . . . H38 H -0.0470 0.4098 1.2018 0.093 Uiso 1 1 calc R . . C39 C 0.0634(7) 0.4317(7) 1.1621(5) 0.072(2) Uani 1 1 d . . . H39 H 0.0777 0.4480 1.1933 0.087 Uiso 1 1 calc R . . C40 C 0.1167(6) 0.4312(6) 1.1117(5) 0.070(2) Uani 1 1 d . . . H40 H 0.1695 0.4447 1.1080 0.084 Uiso 1 1 calc R . . C41 C 0.0904(5) 0.4099(5) 1.0652(4) 0.055(2) Uani 1 1 d . . . C42 C 0.1389(5) 0.4107(5) 1.0091(4) 0.0506(18) Uani 1 1 d . . . H42 H 0.1891 0.4292 0.9986 0.061 Uiso 1 1 calc R . . C43 C 0.0890(5) 0.3467(5) 0.8961(4) 0.0556(19) Uani 1 1 d . . . C44 C 0.1139(5) 0.3398(6) 0.8363(4) 0.0554(19) Uani 1 1 d . . . C45 C 0.0648(7) 0.3083(8) 0.8045(5) 0.080(3) Uani 1 1 d . . . H45A H 0.0756 0.3294 0.7611 0.096 Uiso 1 1 calc R . . H45B H 0.0003 0.3336 0.8127 0.096 Uiso 1 1 calc R . . H45C H 0.0862 0.2413 0.8189 0.096 Uiso 1 1 calc R . . C46 C 0.6925(5) 0.7061(5) 0.7419(4) 0.0530(17) Uani 1 1 d . . . H46 H 0.7140 0.7195 0.7718 0.064 Uiso 1 1 calc R . . C47 C 0.7207(6) 0.7327(6) 0.6834(4) 0.062(2) Uani 1 1 d . . . H47 H 0.7596 0.7660 0.6731 0.074 Uiso 1 1 calc R . . C48 C 0.6939(6) 0.7120(6) 0.6409(4) 0.061(2) Uani 1 1 d . . . H48 H 0.7146 0.7287 0.6005 0.073 Uiso 1 1 calc R . . C49 C 0.6340(6) 0.6645(5) 0.6573(4) 0.0541(18) Uani 1 1 d . . . H49 H 0.6132 0.6488 0.6283 0.065 Uiso 1 1 calc R . . C50 C 0.6070(4) 0.6421(5) 0.7155(3) 0.0397(14) Uani 1 1 d . . . C51 C 0.5406(5) 0.5971(5) 0.7356(3) 0.0439(15) Uani 1 1 d . . . H51 H 0.5149 0.5802 0.7097 0.053 Uiso 1 1 calc R . . C52 C 0.4558(5) 0.5423(6) 0.8795(3) 0.0503(17) Uani 1 1 d . . . C53 C 0.3896(5) 0.5027(7) 0.9170(3) 0.060(2) Uani 1 1 d . . . C54 C 0.3745(6) 0.5001(9) 0.9806(4) 0.076(3) Uani 1 1 d . . . H54A H 0.3370 0.4640 1.0001 0.092 Uiso 1 1 calc R . . H54B H 0.3440 0.5626 0.9826 0.092 Uiso 1 1 calc R . . H54C H 0.4323 0.4719 1.0013 0.092 Uiso 1 1 calc R . . C55 C 0.2027(10) 0.6533(10) 0.5585(7) 0.106(4) Uani 1 1 d . . . H55A H 0.2068 0.5921 0.5845 0.127 Uiso 1 1 calc R . . H55B H 0.2607 0.6596 0.5580 0.127 Uiso 1 1 calc R . . H55C H 0.1873 0.6621 0.5175 0.127 Uiso 1 1 calc R . . C56 C 0.3837(7) 0.6869(7) 0.4298(5) 0.079(3) Uani 1 1 d . . . H56A H 0.3696 0.6876 0.3906 0.094 Uiso 1 1 calc R . . H56B H 0.3555 0.6502 0.4617 0.094 Uiso 1 1 calc R . . H56C H 0.4489 0.6601 0.4355 0.094 Uiso 1 1 calc R . . C57 C 0.4294(8) 0.7355(8) 0.0140(5) 0.092(4) Uani 1 1 d . . . H57A H 0.4062 0.6943 0.0058 0.110 Uiso 1 1 calc R . . H57B H 0.4887 0.7001 0.0327 0.110 Uiso 1 1 calc R . . H57C H 0.4344 0.7816 -0.0239 0.110 Uiso 1 1 calc R . . C58 C 0.3890(7) 0.1853(7) 0.9436(5) 0.081(3) Uani 1 1 d . . . H58A H 0.4452 0.1553 0.9247 0.097 Uiso 1 1 calc R . . H58B H 0.3715 0.1388 0.9752 0.097 Uiso 1 1 calc R . . H58C H 0.3977 0.2267 0.9612 0.097 Uiso 1 1 calc R . . C59 C 0.4488(7) 0.2366(9) 0.5149(5) 0.093(4) Uani 1 1 d . . . H59A H 0.4663 0.2837 0.4839 0.112 Uiso 1 1 calc R . . H59B H 0.4545 0.1878 0.4987 0.112 Uiso 1 1 calc R . . H59C H 0.4880 0.2110 0.5499 0.112 Uiso 1 1 calc R . . C60 C 0.1944(6) 0.1728(7) 1.0584(6) 0.079(3) Uani 1 1 d . . . H60A H 0.2217 0.1900 1.0186 0.095 Uiso 1 1 calc R . . H60B H 0.2219 0.1065 1.0776 0.095 Uiso 1 1 calc R . . H60C H 0.2044 0.2046 1.0834 0.095 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 0.0613(6) 0.0531(6) 0.0750(7) -0.0168(5) 0.0325(5) -0.0333(5) Cu2 0.0365(5) 0.0511(5) 0.0510(5) -0.0098(4) 0.0090(3) -0.0243(4) Cu3 0.0438(5) 0.0575(6) 0.0638(6) -0.0325(4) 0.0100(4) -0.0291(4) Cu4 0.0397(5) 0.0446(5) 0.0489(5) -0.0100(4) 0.0077(3) -0.0266(4) Cu5 0.0379(5) 0.0470(5) 0.0452(5) -0.0114(4) -0.0039(3) -0.0224(4) Cu6 0.0500(5) 0.0800(7) 0.0366(5) -0.0053(4) -0.0011(4) -0.0454(5) Cu7 0.0448(5) 0.0622(6) 0.0706(6) -0.0380(5) 0.0197(4) -0.0336(4) Cu8 0.0413(5) 0.0454(5) 0.0544(5) -0.0099(4) 0.0101(4) -0.0259(4) Cu9 0.0458(5) 0.0525(6) 0.0803(7) -0.0160(5) 0.0230(4) -0.0288(4) Cu10 0.0342(5) 0.0540(5) 0.0546(5) 0.0008(4) 0.0052(4) -0.0232(4) Cu11 0.0372(4) 0.0483(5) 0.0391(4) -0.0085(3) 0.0004(3) -0.0223(4) Cu12 0.0452(5) 0.0795(7) 0.0355(5) -0.0014(4) -0.0013(3) -0.0415(5) O1 0.071(4) 0.072(4) 0.079(4) -0.036(3) 0.039(3) -0.055(3) O2 0.053(3) 0.053(3) 0.057(3) -0.023(2) 0.018(2) -0.031(2) O3 0.038(2) 0.053(3) 0.048(3) -0.021(2) 0.0078(19) -0.027(2) O4 0.052(3) 0.072(3) 0.039(2) -0.013(2) 0.004(2) -0.042(3) O5 0.045(3) 0.082(4) 0.037(2) -0.012(2) -0.0063(19) -0.034(3) O6 0.048(3) 0.106(5) 0.047(3) -0.012(3) 0.006(2) -0.053(3) O7 0.049(3) 0.057(3) 0.051(3) -0.019(2) 0.009(2) -0.031(2) O8 0.048(3) 0.063(3) 0.047(3) -0.009(2) 0.002(2) -0.040(2) O9 0.042(3) 0.063(4) 0.101(5) -0.013(3) 0.018(3) -0.035(3) O10 0.056(3) 0.063(3) 0.065(3) -0.022(3) 0.022(2) -0.039(3) O11 0.043(3) 0.090(4) 0.038(3) -0.005(2) -0.004(2) -0.033(3) O12 0.044(3) 0.114(5) 0.046(3) -0.007(3) 0.004(2) -0.051(3) O13 0.043(3) 0.052(3) 0.054(3) -0.003(2) 0.004(2) -0.026(2) O14 0.035(2) 0.049(3) 0.057(3) -0.003(2) 0.005(2) -0.019(2) O15 0.080(5) 0.085(5) 0.100(5) -0.019(4) 0.041(4) -0.048(4) O16 0.085(5) 0.101(6) 0.122(7) -0.007(5) 0.030(5) -0.041(5) O17 0.088(6) 0.119(7) 0.191(10) -0.057(7) 0.071(6) -0.078(5) O18 0.059(3) 0.081(4) 0.063(3) -0.037(3) 0.007(3) -0.035(3) O19 0.074(5) 0.154(9) 0.089(6) 0.014(6) 0.010(4) -0.041(5) O20 0.094(6) 0.082(5) 0.110(6) -0.027(4) 0.015(5) -0.042(4) O21 0.038(3) 0.059(3) 0.102(4) -0.037(3) 0.000(3) -0.021(2) O22 0.081(5) 0.078(5) 0.111(6) -0.036(4) -0.045(4) -0.014(4) O23 0.159(10) 0.062(5) 0.257(15) -0.043(7) -0.107(10) -0.006(6) O24 0.043(3) 0.047(3) 0.067(3) -0.023(2) -0.009(2) -0.015(2) O25 0.079(4) 0.083(4) 0.082(4) -0.047(4) -0.011(3) -0.034(3) O26 0.066(4) 0.052(3) 0.067(3) -0.022(3) -0.015(3) -0.004(3) O27 0.060(3) 0.045(3) 0.091(4) -0.015(3) -0.012(3) -0.009(2) O28 0.165(6) 0.129(7) 0.128(7) -0.052(6) 0.026(6) -0.097(5) O29 0.172(7) 0.065(4) 0.288(14) -0.015(7) -0.061(9) -0.022(5) O30 0.069(4) 0.114(6) 0.075(4) -0.061(4) 0.027(3) -0.057(4) O31 0.081(5) 0.100(6) 0.090(5) -0.043(4) 0.017(4) -0.031(4) O32 0.075(5) 0.225(12) 0.045(4) -0.011(5) 0.006(3) -0.051(6) O33 0.058(3) 0.064(3) 0.146(6) -0.049(4) -0.033(4) -0.012(3) O34 0.094(5) 0.088(5) 0.089(5) -0.044(4) -0.043(4) 0.017(4) O35 0.185(10) 0.053(3) 0.173(9) -0.013(4) -0.115(8) -0.022(5) O36 0.096(4) 0.096(5) 0.093(4) -0.026(3) 0.033(3) -0.068(4) O37 0.087(6) 0.090(6) 0.246(10) 0.043(6) 0.033(6) -0.042(4) O38 0.059(4) 0.095(5) 0.189(8) 0.011(5) 0.031(4) -0.045(4) O39 0.050(3) 0.049(3) 0.063(3) -0.014(2) -0.005(2) -0.025(2) O40 0.060(3) 0.069(4) 0.069(4) -0.025(3) -0.004(3) -0.022(3) O41 0.088(5) 0.070(4) 0.094(5) -0.036(4) -0.021(4) -0.039(3) O42 0.123(7) 0.065(5) 0.091(5) -0.003(4) 0.007(5) -0.011(5) O43 0.120(6) 0.093(6) 0.097(6) -0.039(4) -0.020(5) -0.013(5) O44 0.097(5) 0.063(4) 0.082(4) -0.033(3) 0.020(4) -0.022(3) O45 0.099(5) 0.077(4) 0.192(7) -0.063(5) 0.063(5) -0.045(4) O46 0.076(4) 0.061(4) 0.089(4) -0.014(3) -0.006(3) -0.033(3) O47 0.094(5) 0.093(5) 0.113(5) -0.001(4) -0.015(4) -0.043(4) O48 0.095(5) 0.048(4) 0.220(10) -0.046(5) -0.089(6) 0.007(4) N1 0.047(4) 0.052(4) 0.055(4) 0.002(3) 0.013(3) -0.012(3) N2 0.036(3) 0.050(3) 0.053(4) -0.001(3) 0.012(2) -0.013(3) N3 0.048(3) 0.052(3) 0.043(3) -0.003(3) 0.007(2) -0.029(3) N4 0.053(4) 0.040(3) 0.065(4) -0.021(3) 0.024(3) -0.025(3) N5 0.050(4) 0.071(4) 0.077(4) -0.042(4) 0.015(3) -0.038(3) N6 0.038(3) 0.047(3) 0.064(4) -0.025(3) 0.007(3) -0.023(2) N7 0.040(3) 0.047(3) 0.056(3) -0.017(3) 0.003(2) -0.025(2) N8 0.043(3) 0.053(3) 0.048(3) -0.010(3) -0.002(2) -0.030(3) N9 0.040(3) 0.030(3) 0.058(3) -0.008(2) 0.003(2) -0.014(2) N10 0.043(3) 0.052(3) 0.044(3) 0.000(2) -0.007(2) -0.025(3) N11 0.043(3) 0.070(4) 0.043(3) -0.009(3) -0.002(2) -0.035(3) N12 0.053(4) 0.092(5) 0.037(3) -0.004(3) -0.004(2) -0.049(4) N13 0.056(4) 0.066(4) 0.081(5) -0.043(4) 0.016(3) -0.035(3) N14 0.032(3) 0.049(3) 0.078(4) -0.035(3) 0.011(3) -0.022(2) N15 0.038(3) 0.046(3) 0.068(4) -0.014(3) 0.003(3) -0.026(2) N16 0.040(3) 0.055(4) 0.042(3) 0.002(3) 0.003(2) -0.026(3) N17 0.049(4) 0.038(3) 0.078(4) -0.012(3) 0.021(3) -0.018(3) N18 0.038(3) 0.038(3) 0.076(4) -0.003(3) 0.012(3) -0.016(2) N19 0.044(3) 0.054(4) 0.057(4) -0.011(3) 0.016(3) -0.030(3) N20 0.044(3) 0.047(3) 0.063(4) -0.008(3) 0.016(3) -0.029(3) N21 0.036(3) 0.052(3) 0.040(3) -0.013(2) 0.002(2) -0.021(2) N22 0.040(3) 0.053(3) 0.034(3) -0.008(2) -0.003(2) -0.024(2) N23 0.039(3) 0.063(4) 0.031(3) 0.000(2) -0.002(2) -0.028(3) N24 0.040(3) 0.091(5) 0.035(3) 0.004(3) -0.003(2) -0.041(3) N25 0.064(5) 0.063(5) 0.111(7) -0.026(4) 0.029(4) -0.040(4) N26 0.062(5) 0.104(7) 0.073(5) -0.012(5) 0.004(4) -0.052(5) N27 0.056(4) 0.047(4) 0.073(4) -0.011(3) -0.011(3) -0.021(3) N28 0.050(3) 0.048(3) 0.047(3) -0.015(3) 0.002(3) -0.018(3) N29 0.042(4) 0.106(7) 0.074(5) -0.024(5) -0.005(3) -0.034(4) N30 0.046(3) 0.048(3) 0.082(4) -0.018(3) -0.017(3) -0.017(3) N31 0.069(4) 0.085(5) 0.148(7) -0.004(4) 0.035(4) -0.044(4) N32 0.052(4) 0.051(4) 0.047(3) -0.009(3) 0.000(3) -0.020(3) N33 0.128(6) 0.070(4) 0.136(7) -0.031(4) 0.000(5) -0.045(4) C1 0.058(5) 0.083(6) 0.051(5) -0.001(4) 0.020(4) -0.021(4) C2 0.058(5) 0.119(9) 0.050(5) -0.016(5) 0.014(4) -0.024(5) C3 0.046(4) 0.126(9) 0.042(4) -0.015(4) -0.001(3) -0.036(5) C4 0.052(5) 0.112(8) 0.046(4) -0.021(4) 0.007(3) -0.034(5) C5 0.045(4) 0.061(5) 0.046(4) 0.003(3) 0.009(3) -0.006(3) C6 0.041(4) 0.055(4) 0.052(4) -0.005(3) -0.002(3) -0.019(3) C7 0.047(4) 0.059(5) 0.069(5) -0.020(4) 0.008(3) -0.029(3) C8 0.060(5) 0.059(5) 0.072(5) -0.029(4) 0.022(4) -0.039(4) C9 0.106(8) 0.116(9) 0.096(7) -0.048(7) 0.034(6) -0.098(8) C10 0.067(6) 0.108(8) 0.117(8) -0.078(7) 0.003(5) -0.048(5) C11 0.075(6) 0.099(8) 0.110(8) -0.061(7) 0.001(6) -0.050(6) C12 0.053(5) 0.083(7) 0.127(9) -0.051(6) -0.002(5) -0.043(5) C13 0.051(5) 0.068(6) 0.113(8) -0.026(5) 0.013(5) -0.045(4) C14 0.043(4) 0.056(5) 0.101(7) -0.033(4) 0.008(4) -0.032(4) C15 0.042(4) 0.065(5) 0.065(5) -0.025(4) 0.005(3) -0.031(3) C16 0.028(3) 0.040(3) 0.044(3) -0.011(3) -0.001(2) -0.014(2) C17 0.039(3) 0.041(3) 0.041(3) -0.003(3) -0.007(2) -0.023(3) C18 0.050(4) 0.056(4) 0.048(4) -0.015(3) 0.006(3) -0.033(3) C19 0.047(4) 0.047(4) 0.069(5) -0.014(3) 0.009(3) -0.027(3) C20 0.054(5) 0.061(5) 0.085(6) -0.016(4) 0.011(4) -0.041(4) C21 0.075(5) 0.077(6) 0.045(4) -0.008(4) 0.009(4) -0.051(5) C22 0.061(5) 0.068(5) 0.054(4) -0.017(4) 0.007(3) -0.043(4) C23 0.043(4) 0.040(3) 0.047(4) -0.009(3) -0.005(3) -0.019(3) C24 0.046(4) 0.061(4) 0.042(4) -0.011(3) -0.002(3) -0.028(3) C25 0.038(4) 0.065(5) 0.053(4) -0.013(3) -0.001(3) -0.029(3) C26 0.040(4) 0.077(5) 0.047(4) -0.006(4) -0.003(3) -0.032(4) C27 0.060(5) 0.104(7) 0.042(4) -0.011(4) -0.004(3) -0.043(5) C28 0.064(5) 0.107(8) 0.111(7) -0.078(7) 0.024(5) -0.056(5) C29 0.075(6) 0.105(8) 0.113(8) -0.075(7) 0.024(5) -0.060(6) C30 0.068(6) 0.105(8) 0.141(10) -0.084(8) 0.027(6) -0.064(6) C31 0.051(5) 0.078(6) 0.093(6) -0.039(5) 0.023(4) -0.045(4) C32 0.046(4) 0.057(5) 0.111(7) -0.046(5) 0.026(4) -0.035(4) C33 0.049(4) 0.048(4) 0.080(5) -0.030(4) 0.015(4) -0.031(3) C34 0.037(3) 0.036(3) 0.053(4) -0.011(3) 0.003(3) -0.018(3) C35 0.035(3) 0.043(3) 0.053(4) -0.015(3) 0.009(3) -0.023(3) C36 0.036(3) 0.047(4) 0.063(4) -0.012(3) 0.011(3) -0.024(3) C37 0.061(5) 0.055(5) 0.081(6) -0.024(4) 0.022(4) -0.030(4) C38 0.072(6) 0.077(6) 0.075(6) -0.024(5) 0.030(5) -0.029(5) C39 0.070(6) 0.075(6) 0.076(6) -0.022(5) 0.012(4) -0.037(5) C40 0.061(5) 0.050(5) 0.087(6) -0.013(4) 0.011(4) -0.020(4) C41 0.047(4) 0.037(4) 0.069(5) -0.011(3) 0.018(3) -0.013(3) C42 0.044(4) 0.041(4) 0.059(4) 0.002(3) 0.004(3) -0.023(3) C43 0.047(4) 0.040(4) 0.074(5) -0.010(3) 0.010(3) -0.020(3) C44 0.049(4) 0.054(4) 0.066(5) -0.010(4) 0.018(3) -0.035(3) C45 0.078(6) 0.099(7) 0.079(6) -0.018(5) 0.025(5) -0.067(6) C46 0.057(4) 0.053(4) 0.063(5) -0.018(3) 0.005(3) -0.037(4) C47 0.072(5) 0.065(5) 0.067(5) -0.027(4) 0.027(4) -0.047(4) C48 0.079(6) 0.058(5) 0.056(4) -0.023(4) 0.030(4) -0.041(4) C49 0.064(5) 0.051(4) 0.055(4) -0.019(3) 0.018(3) -0.032(4) C50 0.034(3) 0.044(3) 0.050(4) -0.018(3) 0.005(3) -0.022(3) C51 0.041(3) 0.048(4) 0.046(4) -0.010(3) -0.004(3) -0.022(3) C52 0.040(4) 0.071(5) 0.039(4) -0.004(3) 0.001(3) -0.031(3) C53 0.045(4) 0.092(6) 0.034(4) 0.007(4) -0.001(3) -0.039(4) C54 0.059(5) 0.130(9) 0.041(4) -0.010(5) 0.006(3) -0.052(5) C55 0.100(9) 0.088(9) 0.109(10) -0.018(7) 0.003(7) -0.025(7) C56 0.077(6) 0.063(6) 0.103(8) -0.034(5) 0.018(5) -0.031(5) C57 0.094(8) 0.072(7) 0.082(7) -0.038(5) 0.016(5) 0.006(5) C58 0.078(6) 0.069(6) 0.077(6) -0.002(5) -0.010(5) -0.023(5) C59 0.055(6) 0.117(9) 0.088(7) -0.044(7) 0.013(5) -0.006(6) C60 0.051(5) 0.051(5) 0.114(8) -0.004(5) 0.006(5) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.928(6) . ? Cu1 O15 1.954(6) . ? Cu1 N1 1.999(9) . ? Cu1 O1 2.003(6) . ? Cu1 O42 2.240(8) . ? Cu2 O6 1.937(6) . ? Cu2 O13 1.966(5) . ? Cu2 N3 1.973(6) . ? Cu2 N4 1.973(7) . ? Cu2 O43 2.317(8) . ? Cu3 N6 1.917(6) . ? Cu3 O18 1.963(6) . ? Cu3 N5 2.006(6) . ? Cu3 O3 2.008(5) . ? Cu3 O44 2.217(7) . ? Cu4 O2 1.932(5) . ? Cu4 O13 1.964(6) . ? Cu4 N7 1.983(6) . ? Cu4 N8 1.998(6) . ? Cu4 O21 2.365(6) . ? Cu5 N10 1.946(6) . ? Cu5 O24 1.956(5) . ? Cu5 O5 1.992(5) . ? Cu5 N9 2.025(6) . ? Cu5 O27 2.265(6) . ? Cu6 O4 1.928(5) . ? Cu6 O13 1.969(5) . ? Cu6 N12 1.974(6) . ? Cu6 N11 1.982(6) . ? Cu6 O22 2.375(7) . ? Cu7 O30 1.938(7) . ? Cu7 N14 1.943(7) . ? Cu7 O7 2.014(5) . ? Cu7 N13 2.033(7) . ? Cu7 O45 2.190(8) . ? Cu8 O14 1.951(6) . ? Cu8 O10 1.953(5) . ? Cu8 N15 1.954(7) . ? Cu8 N16 1.965(6) . ? Cu8 O33 2.331(6) . ? Cu9 N18 1.941(6) . ? Cu9 O36 1.969(7) . ? Cu9 O9 1.978(7) . ? Cu9 N17 1.986(8) . ? Cu9 O46 2.181(6) . ? Cu10 O12 1.909(7) . ? Cu10 O14 1.949(5) . ? Cu10 N19 1.992(6) . ? Cu10 N20 1.998(7) . ? Cu10 O47 2.381(9) . ? Cu11 O39 1.940(5) . ? Cu11 N22 1.946(6) . ? Cu11 N21 2.019(6) . ? Cu11 O11 2.030(5) . ? Cu11 O48 2.264(7) . ? Cu12 O8 1.925(5) . ? Cu12 N24 1.960(6) . ? Cu12 O14 1.963(6) . ? Cu12 N23 1.985(6) . ? O1 C7 1.268(10) . ? O2 N4 1.358(8) . ? O3 C16 1.292(8) . ? O4 N8 1.347(8) . ? O5 C25 1.263(9) . ? O6 N12 1.351(8) . ? O7 C34 1.265(9) . ? O8 N16 1.329(8) . ? O9 C43 1.259(9) . ? O10 N20 1.336(9) . ? O11 C52 1.265(10) . ? O12 N24 1.360(8) . ? O15 N25 1.279(12) . ? O16 N25 1.218(11) . ? O17 N25 1.217(10) . ? O18 N26 1.292(12) . ? O19 N26 1.177(11) . ? O20 N26 1.264(12) . ? O21 N27 1.245(9) . ? O22 N27 1.182(10) . ? O23 N27 1.222(11) . ? O24 N28 1.286(8) . ? O25 N28 1.265(9) . ? O26 N28 1.196(8) . ? O27 N33 1.236(12) . ? O28 N33 1.270(14) . ? O29 N33 1.260(15) . ? O30 N29 1.301(12) . ? O31 N29 1.231(11) . ? O32 N29 1.173(11) . ? O33 N30 1.266(9) . ? O34 N30 1.179(10) . ? O35 N30 1.223(10) . ? O36 N31 1.288(14) . ? O37 N31 1.201(13) . ? O38 N31 1.205(13) . ? O39 N32 1.320(8) . ? O40 N32 1.221(9) . ? O41 N32 1.223(9) . ? O42 C55 1.208(14) . ? O43 C56 1.346(13) . ? O44 C57 1.373(10) . ? O45 C59 1.341(12) . ? O46 C60 1.414(12) . ? O47 C58 1.299(13) . ? N1 C5 1.333(12) . ? N1 C1 1.335(10) . ? N2 C6 1.258(11) . ? N2 N3 1.398(9) . ? N3 C7 1.301(11) . ? N4 C8 1.289(10) . ? N5 C10 1.361(11) . ? N5 C14 1.364(12) . ? N6 C15 1.299(9) . ? N6 N7 1.370(9) . ? N7 C16 1.344(9) . ? N8 C17 1.288(9) . ? N9 C23 1.342(9) . ? N9 C19 1.345(10) . ? N10 C24 1.278(10) . ? N10 N11 1.350(8) . ? N11 C25 1.347(10) . ? N12 C26 1.306(11) . ? N13 C32 1.335(12) . ? N13 C28 1.354(12) . ? N14 C33 1.294(9) . ? N14 N15 1.381(9) . ? N15 C34 1.363(9) . ? N16 C35 1.276(9) . ? N17 C37 1.343(11) . ? N17 C41 1.364(11) . ? N18 C42 1.292(11) . ? N18 N19 1.351(10) . ? N19 C43 1.370(11) . ? N20 C44 1.281(9) . ? N21 C50 1.328(9) . ? N21 C46 1.348(9) . ? N22 C51 1.298(9) . ? N22 N23 1.350(8) . ? N23 C52 1.338(9) . ? N24 C53 1.293(12) . ? C1 C2 1.382(17) . ? C1 H1 0.9500 . ? C2 C3 1.388(15) . ? C2 H2 0.9500 . ? C3 C4 1.407(11) . ? C3 H3 0.9500 . ? C4 C5 1.371(14) . ? C4 H4 0.9500 . ? C5 C6 1.465(11) . ? C6 H6 0.9500 . ? C7 C8 1.494(12) . ? C8 C9 1.492(12) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.367(14) . ? C10 H10 0.9500 . ? C11 C12 1.394(16) . ? C11 H11 0.9500 . ? C12 C13 1.365(15) . ? C12 H12 0.9500 . ? C13 C14 1.375(11) . ? C13 H13 0.9500 . ? C14 C15 1.474(12) . ? C15 H15 0.9500 . ? C16 C17 1.451(9) . ? C17 C18 1.482(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.407(12) . ? C19 H19 0.9500 . ? C20 C21 1.385(13) . ? C20 H20 0.9500 . ? C21 C22 1.392(11) . ? C21 H21 0.9500 . ? C22 C23 1.377(11) . ? C22 H22 0.9500 . ? C23 C24 1.464(10) . ? C24 H24 0.9500 . ? C25 C26 1.481(10) . ? C26 C27 1.458(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.425(12) . ? C28 H28 0.9500 . ? C29 C30 1.403(16) . ? C29 H29 0.9500 . ? C30 C31 1.341(15) . ? C30 H30 0.9500 . ? C31 C32 1.399(11) . ? C31 H31 0.9500 . ? C32 C33 1.432(13) . ? C33 H33 0.9500 . ? C34 C35 1.481(10) . ? C35 C36 1.490(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.374(15) . ? C37 H37 0.9500 . ? C38 C39 1.356(15) . ? C38 H38 0.9500 . ? C39 C40 1.371(13) . ? C39 H39 0.9500 . ? C40 C41 1.422(15) . ? C40 H40 0.9500 . ? C41 C42 1.444(11) . ? C42 H42 0.9500 . ? C43 C44 1.447(12) . ? C44 C45 1.489(14) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.373(11) . ? C46 H46 0.9500 . ? C47 C48 1.336(13) . ? C47 H47 0.9500 . ? C48 C49 1.415(11) . ? C48 H48 0.9500 . ? C49 C50 1.355(10) . ? C49 H49 0.9500 . ? C50 C51 1.480(9) . ? C51 H51 0.9500 . ? C52 C53 1.503(10) . ? C53 C54 1.477(11) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? 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 N2 Cu1 O15 176.3(3) . . ? N2 Cu1 N1 80.6(3) . . ? O15 Cu1 N1 97.8(3) . . ? N2 Cu1 O1 79.7(3) . . ? O15 Cu1 O1 102.2(3) . . ? N1 Cu1 O1 159.2(2) . . ? N2 Cu1 O42 92.6(3) . . ? O15 Cu1 O42 83.8(4) . . ? N1 Cu1 O42 85.8(3) . . ? O1 Cu1 O42 101.8(3) . . ? O6 Cu2 O13 95.2(2) . . ? O6 Cu2 N3 98.0(2) . . ? O13 Cu2 N3 166.6(3) . . ? O6 Cu2 N4 168.3(3) . . ? O13 Cu2 N4 88.3(2) . . ? N3 Cu2 N4 79.3(3) . . ? O6 Cu2 O43 86.8(3) . . ? O13 Cu2 O43 88.2(3) . . ? N3 Cu2 O43 90.1(3) . . ? N4 Cu2 O43 104.5(3) . . ? N6 Cu3 O18 173.0(3) . . ? N6 Cu3 N5 80.7(3) . . ? O18 Cu3 N5 100.5(3) . . ? N6 Cu3 O3 79.4(2) . . ? O18 Cu3 O3 98.0(2) . . ? N5 Cu3 O3 157.8(2) . . ? N6 Cu3 O44 93.5(3) . . ? O18 Cu3 O44 93.3(3) . . ? N5 Cu3 O44 97.1(3) . . ? O3 Cu3 O44 93.9(3) . . ? O2 Cu4 O13 93.0(2) . . ? O2 Cu4 N7 99.0(2) . . ? O13 Cu4 N7 164.3(2) . . ? O2 Cu4 N8 177.3(2) . . ? O13 Cu4 N8 88.7(2) . . ? N7 Cu4 N8 78.9(2) . . ? O2 Cu4 O21 86.0(2) . . ? O13 Cu4 O21 89.6(2) . . ? N7 Cu4 O21 101.1(2) . . ? N8 Cu4 O21 96.2(2) . . ? N10 Cu5 O24 177.9(2) . . ? N10 Cu5 O5 79.5(2) . . ? O24 Cu5 O5 98.4(2) . . ? N10 Cu5 N9 79.8(2) . . ? O24 Cu5 N9 102.3(2) . . ? O5 Cu5 N9 155.2(2) . . ? N10 Cu5 O27 93.9(3) . . ? O24 Cu5 O27 86.1(2) . . ? O5 Cu5 O27 104.4(2) . . ? N9 Cu5 O27 90.6(2) . . ? O4 Cu6 O13 93.0(2) . . ? O4 Cu6 N12 176.7(2) . . ? O13 Cu6 N12 89.4(3) . . ? O4 Cu6 N11 97.3(2) . . ? O13 Cu6 N11 158.3(2) . . ? N12 Cu6 N11 79.7(3) . . ? O4 Cu6 O22 93.4(3) . . ? O13 Cu6 O22 92.0(3) . . ? N12 Cu6 O22 88.8(3) . . ? N11 Cu6 O22 106.4(3) . . ? O30 Cu7 N14 172.3(3) . . ? O30 Cu7 O7 96.4(2) . . ? N14 Cu7 O7 79.3(2) . . ? O30 Cu7 N13 103.1(3) . . ? N14 Cu7 N13 79.9(3) . . ? O7 Cu7 N13 157.1(2) . . ? O30 Cu7 O45 88.4(4) . . ? N14 Cu7 O45 98.5(3) . . ? O7 Cu7 O45 98.8(3) . . ? N13 Cu7 O45 93.7(3) . . ? O14 Cu8 O10 92.6(2) . . ? O14 Cu8 N15 162.8(2) . . ? O10 Cu8 N15 98.4(2) . . ? O14 Cu8 N16 89.2(2) . . ? O10 Cu8 N16 177.6(3) . . ? N15 Cu8 N16 79.5(3) . . ? O14 Cu8 O33 95.1(2) . . ? O10 Cu8 O33 90.5(3) . . ? N15 Cu8 O33 98.1(3) . . ? N16 Cu8 O33 90.9(3) . . ? N18 Cu9 O36 178.5(4) . . ? N18 Cu9 O9 79.7(3) . . ? O36 Cu9 O9 99.4(3) . . ? N18 Cu9 N17 80.6(3) . . ? O36 Cu9 N17 100.1(3) . . ? O9 Cu9 N17 158.6(2) . . ? N18 Cu9 O46 95.4(3) . . ? O36 Cu9 O46 85.9(3) . . ? O9 Cu9 O46 96.2(3) . . ? N17 Cu9 O46 93.9(3) . . ? O12 Cu10 O14 94.2(2) . . ? O12 Cu10 N19 98.2(3) . . ? O14 Cu10 N19 167.6(3) . . ? O12 Cu10 N20 170.4(3) . . ? O14 Cu10 N20 87.8(2) . . ? N19 Cu10 N20 80.0(3) . . ? O12 Cu10 O47 103.7(3) . . ? O14 Cu10 O47 85.0(3) . . ? N19 Cu10 O47 91.8(3) . . ? N20 Cu10 O47 85.8(3) . . ? O39 Cu11 N22 177.2(2) . . ? O39 Cu11 N21 99.8(2) . . ? N22 Cu11 N21 79.9(2) . . ? O39 Cu11 O11 102.2(2) . . ? N22 Cu11 O11 78.7(2) . . ? N21 Cu11 O11 155.8(2) . . ? O39 Cu11 O48 84.6(3) . . ? N22 Cu11 O48 92.7(3) . . ? N21 Cu11 O48 94.2(4) . . ? O11 Cu11 O48 97.9(4) . . ? O8 Cu12 N24 177.4(2) . . ? O8 Cu12 O14 93.4(2) . . ? N24 Cu12 O14 89.0(3) . . ? O8 Cu12 N23 97.3(2) . . ? N24 Cu12 N23 80.2(3) . . ? O14 Cu12 N23 163.9(2) . . ? C7 O1 Cu1 110.0(6) . . ? N4 O2 Cu4 113.5(4) . . ? C16 O3 Cu3 110.7(4) . . ? N8 O4 Cu6 114.3(4) . . ? C25 O5 Cu5 110.0(5) . . ? N12 O6 Cu2 114.3(5) . . ? C34 O7 Cu7 110.9(4) . . ? N16 O8 Cu12 114.6(4) . . ? C43 O9 Cu9 111.9(6) . . ? N20 O10 Cu8 113.5(5) . . ? C52 O11 Cu11 109.6(5) . . ? N24 O12 Cu10 115.3(5) . . ? Cu4 O13 Cu2 112.3(2) . . ? Cu4 O13 Cu6 110.2(2) . . ? Cu2 O13 Cu6 111.3(3) . . ? Cu10 O14 Cu8 114.3(3) . . ? Cu10 O14 Cu12 112.4(3) . . ? Cu8 O14 Cu12 110.2(2) . . ? N25 O15 Cu1 109.9(6) . . ? N26 O18 Cu3 109.8(5) . . ? N27 O21 Cu4 127.9(5) . . ? N27 O22 Cu6 133.7(6) . . ? N28 O24 Cu5 110.8(4) . . ? N33 O27 Cu5 120.6(7) . . ? N29 O30 Cu7 112.7(5) . . ? N30 O33 Cu8 125.9(5) . . ? N31 O36 Cu9 113.4(6) . . ? N32 O39 Cu11 111.2(4) . . ? C55 O42 Cu1 124.6(9) . . ? C56 O43 Cu2 131.1(8) . . ? C57 O44 Cu3 127.8(7) . . ? C59 O45 Cu7 130.6(9) . . ? C60 O46 Cu9 123.3(6) . . ? C58 O47 Cu10 129.7(9) . . ? C5 N1 C1 119.9(9) . . ? C5 N1 Cu1 111.2(5) . . ? C1 N1 Cu1 128.7(8) . . ? C6 N2 N3 126.6(7) . . ? C6 N2 Cu1 118.0(5) . . ? N3 N2 Cu1 115.2(5) . . ? C7 N3 N2 109.8(6) . . ? C7 N3 Cu2 114.7(6) . . ? N2 N3 Cu2 134.8(5) . . ? C8 N4 O2 117.1(7) . . ? C8 N4 Cu2 118.2(6) . . ? O2 N4 Cu2 124.6(4) . . ? C10 N5 C14 117.4(8) . . ? C10 N5 Cu3 130.1(7) . . ? C14 N5 Cu3 112.4(5) . . ? C15 N6 N7 122.9(6) . . ? C15 N6 Cu3 119.5(5) . . ? N7 N6 Cu3 117.5(4) . . ? C16 N7 N6 109.7(6) . . ? C16 N7 Cu4 113.5(5) . . ? N6 N7 Cu4 136.8(5) . . ? C17 N8 O4 118.7(6) . . ? C17 N8 Cu4 118.7(5) . . ? O4 N8 Cu4 122.6(4) . . ? C23 N9 C19 120.3(6) . . ? C23 N9 Cu5 111.9(5) . . ? C19 N9 Cu5 127.8(5) . . ? C24 N10 N11 125.8(6) . . ? C24 N10 Cu5 118.5(5) . . ? N11 N10 Cu5 115.4(4) . . ? C25 N11 N10 110.0(6) . . ? C25 N11 Cu6 113.6(5) . . ? N10 N11 Cu6 135.9(5) . . ? C26 N12 O6 117.4(6) . . ? C26 N12 Cu6 119.4(5) . . ? O6 N12 Cu6 123.0(5) . . ? C32 N13 C28 122.0(8) . . ? C32 N13 Cu7 111.9(6) . . ? C28 N13 Cu7 126.1(6) . . ? C33 N14 N15 125.6(7) . . ? C33 N14 Cu7 117.2(6) . . ? N15 N14 Cu7 117.1(4) . . ? C34 N15 N14 108.4(6) . . ? C34 N15 Cu8 115.2(5) . . ? N14 N15 Cu8 136.0(5) . . ? C35 N16 O8 117.0(6) . . ? C35 N16 Cu8 119.6(5) . . ? O8 N16 Cu8 123.3(4) . . ? C37 N17 C41 118.1(8) . . ? C37 N17 Cu9 129.5(6) . . ? C41 N17 Cu9 111.9(5) . . ? C42 N18 N19 126.1(6) . . ? C42 N18 Cu9 117.7(5) . . ? N19 N18 Cu9 116.0(6) . . ? N18 N19 C43 110.0(6) . . ? N18 N19 Cu10 137.1(6) . . ? C43 N19 Cu10 112.4(5) . . ? C44 N20 O10 118.0(7) . . ? C44 N20 Cu10 117.1(6) . . ? O10 N20 Cu10 124.8(4) . . ? C50 N21 C46 118.1(6) . . ? C50 N21 Cu11 113.0(5) . . ? C46 N21 Cu11 128.7(5) . . ? C51 N22 N23 124.8(6) . . ? C51 N22 Cu11 118.2(5) . . ? N23 N22 Cu11 116.8(4) . . ? C52 N23 N22 109.8(6) . . ? C52 N23 Cu12 113.9(5) . . ? N22 N23 Cu12 135.8(4) . . ? C53 N24 O12 118.0(6) . . ? C53 N24 Cu12 118.8(5) . . ? O12 N24 Cu12 123.2(5) . . ? O17 N25 O16 122.4(11) . . ? O17 N25 O15 119.4(10) . . ? O16 N25 O15 118.0(8) . . ? O19 N26 O20 122.5(12) . . ? O19 N26 O18 119.8(11) . . ? O20 N26 O18 117.7(8) . . ? O22 N27 O23 120.2(9) . . ? O22 N27 O21 121.3(7) . . ? O23 N27 O21 118.5(8) . . ? O26 N28 O25 124.0(7) . . ? O26 N28 O24 120.0(6) . . ? O25 N28 O24 116.0(6) . . ? O32 N29 O31 127.5(12) . . ? O32 N29 O30 118.8(10) . . ? O31 N29 O30 113.6(9) . . ? O34 N30 O35 121.0(8) . . ? O34 N30 O33 121.7(8) . . ? O35 N30 O33 117.2(8) . . ? O37 N31 O38 123.7(13) . . ? O37 N31 O36 120.3(10) . . ? O38 N31 O36 115.9(9) . . ? O40 N32 O41 124.5(7) . . ? O40 N32 O39 117.5(7) . . ? O41 N32 O39 118.0(7) . . ? O27 N33 O29 120.6(13) . . ? O27 N33 O28 123.4(11) . . ? O29 N33 O28 115.9(12) . . ? N1 C1 C2 122.6(10) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 118.5(8) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C2 C3 C4 117.9(10) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C5 C4 C3 120.0(9) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 121.0(7) . . ? N1 C5 C6 115.7(9) . . ? C4 C5 C6 123.3(9) . . ? N2 C6 C5 113.3(8) . . ? N2 C6 H6 123.3 . . ? C5 C6 H6 123.3 . . ? O1 C7 N3 125.2(8) . . ? O1 C7 C8 119.2(8) . . ? N3 C7 C8 115.6(7) . . ? N4 C8 C9 126.6(8) . . ? N4 C8 C7 110.9(7) . . ? C9 C8 C7 122.5(7) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 C11 122.3(10) . . ? N5 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C12 119.5(9) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 118.6(9) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 120.0(10) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? N5 C14 C13 122.0(9) . . ? N5 C14 C15 114.8(7) . . ? C13 C14 C15 123.2(9) . . ? N6 C15 C14 112.4(7) . . ? N6 C15 H15 123.8 . . ? C14 C15 H15 123.8 . . ? O3 C16 N7 122.5(6) . . ? O3 C16 C17 120.2(6) . . ? N7 C16 C17 117.2(6) . . ? N8 C17 C16 111.1(6) . . ? N8 C17 C18 123.6(6) . . ? C16 C17 C18 125.1(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N9 C19 C20 120.6(8) . . ? N9 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 119.3(7) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 118.5(7) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C23 C22 C21 119.8(8) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? N9 C23 C22 121.4(7) . . ? N9 C23 C24 115.6(6) . . ? C22 C23 C24 123.0(7) . . ? N10 C24 C23 113.2(7) . . ? N10 C24 H24 123.4 . . ? C23 C24 H24 123.4 . . ? O5 C25 N11 123.6(7) . . ? O5 C25 C26 119.8(7) . . ? N11 C25 C26 116.4(7) . . ? N12 C26 C27 126.5(7) . . ? N12 C26 C25 110.2(7) . . ? C27 C26 C25 123.0(7) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N13 C28 C29 119.2(9) . . ? N13 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 117.8(10) . . ? C30 C29 H29 121.1 . . ? C28 C29 H29 121.1 . . ? C31 C30 C29 120.8(8) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 119.8(10) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? N13 C32 C31 120.2(9) . . ? N13 C32 C33 115.8(7) . . ? C31 C32 C33 124.0(9) . . ? N14 C33 C32 114.8(8) . . ? N14 C33 H33 122.6 . . ? C32 C33 H33 122.6 . . ? O7 C34 N15 124.1(7) . . ? O7 C34 C35 122.0(6) . . ? N15 C34 C35 113.8(6) . . ? N16 C35 C34 111.8(6) . . ? N16 C35 C36 125.3(7) . . ? C34 C35 C36 122.8(6) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N17 C37 C38 121.9(9) . . ? N17 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C39 C38 C37 120.8(9) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C40 119.7(11) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C39 C40 C41 118.0(9) . . ? C39 C40 H40 121.0 . . ? C41 C40 H40 121.0 . . ? N17 C41 C40 121.4(7) . . ? N17 C41 C42 115.4(8) . . ? C40 C41 C42 123.1(8) . . ? N18 C42 C41 113.3(7) . . ? N18 C42 H42 123.3 . . ? C41 C42 H42 123.3 . . ? O9 C43 N19 122.2(8) . . ? O9 C43 C44 121.9(8) . . ? N19 C43 C44 115.9(7) . . ? N20 C44 C43 113.8(8) . . ? N20 C44 C45 124.1(8) . . ? C43 C44 C45 122.1(7) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N21 C46 C47 121.4(7) . . ? N21 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C48 C47 C46 120.6(8) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 118.4(7) . . ? C47 C48 H48 120.8 . . ? C49 C48 H48 120.8 . . ? C50 C49 C48 118.1(8) . . ? C50 C49 H49 120.9 . . ? C48 C49 H49 120.9 . . ? N21 C50 C49 123.4(7) . . ? N21 C50 C51 115.2(6) . . ? C49 C50 C51 121.4(7) . . ? N22 C51 C50 112.7(6) . . ? N22 C51 H51 123.6 . . ? C50 C51 H51 123.6 . . ? O11 C52 N23 124.5(7) . . ? O11 C52 C53 120.6(7) . . ? N23 C52 C53 114.9(7) . . ? N24 C53 C54 128.6(7) . . ? N24 C53 C52 111.5(6) . . ? C54 C53 C52 119.9(8) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O42 C55 H55A 109.5 . . ? O42 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O42 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O43 C56 H56A 109.5 . . ? O43 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O43 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O44 C57 H57A 109.5 . . ? O44 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O44 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O47 C58 H58A 109.5 . . ? O47 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O47 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O45 C59 H59A 109.5 . . ? O45 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O45 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O46 C60 H60A 109.5 . . ? O46 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O46 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 4.170 _refine_diff_density_min -2.217 _refine_diff_density_rms 0.199