# 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 _publ_contact_author_name 'Armando J. L. Pombeiro' _publ_contact_author_address ; Instituto Superior Tecnico Av. Rovisco Pais, Lisboa 1049-001 ; _publ_contact_author_email pombeiro@ist.utl.pt _publ_author_name 'Armando J. L. Pombeiro' # Attachment '- Compound1.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 777426' #TrackingRef '- Compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Cu2 N4 O4 S2' _chemical_formula_sum 'C12 H24 Cu2 N4 O4 S2' _chemical_formula_weight 479.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 13.4911(5) _cell_length_b 17.2845(7) _cell_length_c 19.2434(6) _cell_angle_alpha 99.775(2) _cell_angle_beta 109.903(2) _cell_angle_gamma 103.164(2) _cell_volume 3955.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3791 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 21.68 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 2.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5253 _exptl_absorpt_correction_T_max 0.7795 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40857 _diffrn_reflns_av_R_equivalents 0.0952 _diffrn_reflns_av_sigmaI/netI 0.1552 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.35 _reflns_number_total 13461 _reflns_number_gt 6240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^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 13461 _refine_ls_number_parameters 889 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1601 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.930 _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 0.000 0.000 0.000 137 48 ' ' 2 0.486 0.345 0.104 7 2 ' ' 3 0.514 0.655 0.896 7 2 ' ' _platon_squeeze_details ; ; 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 C2 C 0.5133(8) 0.3324(8) 0.9245(5) 0.056(3) Uani 1 1 d . . . C3 C 0.4520(6) 0.1845(5) 0.4618(5) 0.030(2) Uani 1 1 d . . . C4 C -0.0179(7) -0.0376(6) 0.5831(4) 0.035(2) Uani 1 1 d . . . C5 C 0.0612(7) 0.4156(6) 0.5097(5) 0.039(2) Uani 1 1 d . . . C6 C -0.0510(8) 0.6693(8) 0.2056(7) 0.067(4) Uani 1 1 d . . . C7 C 1.1830(10) 0.8546(6) 0.9509(5) 0.060(3) Uani 1 1 d . . . C8 C 0.5456(8) 0.5725(8) 0.7391(6) 0.063(3) Uani 1 1 d . . . C11 C 0.7537(7) 0.1854(6) 0.8055(6) 0.048(3) Uani 1 1 d . . . H11A H 0.7188 0.1895 0.7525 0.058 Uiso 1 1 calc R . . H11B H 0.8330 0.2182 0.8267 0.058 Uiso 1 1 calc R . . C12 C 0.6985(7) 0.2191(6) 0.8535(5) 0.047(3) Uani 1 1 d . . . H12A H 0.7367 0.2203 0.9078 0.057 Uiso 1 1 calc R . . H12B H 0.6984 0.2758 0.8506 0.057 Uiso 1 1 calc R . . C13 C 0.7283(7) 0.0449(6) 0.7307(5) 0.042(2) Uani 1 1 d . . . H13A H 0.7288 -0.0108 0.7366 0.050 Uiso 1 1 calc R . . H13B H 0.7920 0.0679 0.7178 0.050 Uiso 1 1 calc R . . C14 C 0.6226(6) 0.0369(6) 0.6647(4) 0.042(3) Uani 1 1 d . . . H14A H 0.6274 0.0895 0.6501 0.051 Uiso 1 1 calc R . . H14B H 0.6104 -0.0070 0.6195 0.051 Uiso 1 1 calc R . . C15 C 0.8425(8) 0.0936(6) 0.8669(5) 0.057(3) Uani 1 1 d . . . H15A H 0.8528 0.1295 0.9158 0.085 Uiso 1 1 calc R . . H15B H 0.9082 0.1121 0.8556 0.085 Uiso 1 1 calc R . . H15C H 0.8318 0.0367 0.8706 0.085 Uiso 1 1 calc R . . C21 C 0.3281(10) 0.0290(9) 0.8884(6) 0.078(4) Uani 1 1 d . . . H21A H 0.2635 0.0117 0.8387 0.093 Uiso 1 1 calc R . . H21B H 0.3036 0.0067 0.9260 0.093 Uiso 1 1 calc R . . C22 C 0.4195(8) -0.0046(7) 0.8790(6) 0.065(3) Uani 1 1 d . . . H22A H 0.4796 0.0049 0.9296 0.078 Uiso 1 1 calc R . . H22B H 0.3896 -0.0646 0.8535 0.078 Uiso 1 1 calc R . . C23 C 0.2812(10) 0.1584(9) 0.8866(6) 0.088(4) Uani 1 1 d . . . H23A H 0.3102 0.2187 0.9105 0.106 Uiso 1 1 calc R . . H23B H 0.2189 0.1352 0.9009 0.106 Uiso 1 1 calc R . . C24 C 0.2397(10) 0.1408(9) 0.7982(6) 0.088(5) Uani 1 1 d . . . H24A H 0.1998 0.0813 0.7735 0.106 Uiso 1 1 calc R . . H24B H 0.1883 0.1725 0.7794 0.106 Uiso 1 1 calc R . . C25 C 0.4166(12) 0.1483(10) 1.0018(6) 0.118(6) Uani 1 1 d . . . H25A H 0.4458 0.2087 1.0186 0.177 Uiso 1 1 calc R . . H25B H 0.4763 0.1251 1.0237 0.177 Uiso 1 1 calc R . . H25C H 0.3573 0.1299 1.0194 0.177 Uiso 1 1 calc R . . C31 C 0.2591(8) 0.2594(7) 0.6396(5) 0.051(3) Uani 1 1 d . . . H31A H 0.3002 0.2777 0.6960 0.062 Uiso 1 1 calc R . . H31B H 0.2128 0.2955 0.6246 0.062 Uiso 1 1 calc R . . C32 C 0.1889(7) 0.1727(7) 0.6157(5) 0.053(3) Uani 1 1 d . . . H32A H 0.1417 0.1660 0.6454 0.063 Uiso 1 1 calc R . . H32B H 0.1399 0.1573 0.5606 0.063 Uiso 1 1 calc R . . C33 C 0.4477(7) 0.3255(7) 0.6506(6) 0.065(3) Uani 1 1 d . . . H33A H 0.4372 0.3791 0.6685 0.078 Uiso 1 1 calc R . . H33B H 0.4929 0.3337 0.6197 0.078 Uiso 1 1 calc R . . C34 C 0.5095(8) 0.2991(7) 0.7194(6) 0.065(3) Uani 1 1 d . . . H34A H 0.5855 0.3381 0.7470 0.078 Uiso 1 1 calc R . . H34B H 0.4712 0.2998 0.7551 0.078 Uiso 1 1 calc R . . C35 C 0.2901(8) 0.2880(7) 0.5294(6) 0.070(4) Uani 1 1 d . . . H35A H 0.3412 0.2914 0.5033 0.105 Uiso 1 1 calc R . . H35B H 0.2786 0.3418 0.5418 0.105 Uiso 1 1 calc R . . H35C H 0.2190 0.2465 0.4958 0.105 Uiso 1 1 calc R . . C41 C 0.3170(7) -0.1068(7) 0.5249(5) 0.058(3) Uani 1 1 d . . . H41A H 0.3013 -0.1499 0.4781 0.069 Uiso 1 1 calc R . . H41B H 0.3752 -0.1148 0.5686 0.069 Uiso 1 1 calc R . . C42 C 0.3561(7) -0.0228(7) 0.5144(5) 0.053(3) Uani 1 1 d . . . H42A H 0.4305 -0.0128 0.5129 0.064 Uiso 1 1 calc R . . H42B H 0.3042 -0.0178 0.4658 0.064 Uiso 1 1 calc R . . C43 C 0.2111(8) -0.1638(7) 0.5961(6) 0.060(3) Uani 1 1 d . . . H43A H 0.1371 -0.1754 0.5983 0.073 Uiso 1 1 calc R . . H43B H 0.2210 -0.2174 0.5773 0.073 Uiso 1 1 calc R . . C44 C 0.2977(7) -0.1219(7) 0.6753(5) 0.053(3) Uani 1 1 d . . . H44A H 0.2868 -0.1545 0.7112 0.064 Uiso 1 1 calc R . . H44B H 0.3724 -0.1169 0.6754 0.064 Uiso 1 1 calc R . . C45 C 0.1155(7) -0.1551(7) 0.4666(5) 0.067(3) Uani 1 1 d . . . H45A H 0.0481 -0.1584 0.4762 0.100 Uiso 1 1 calc R . . H45B H 0.1160 -0.2109 0.4461 0.100 Uiso 1 1 calc R . . H45C H 0.1174 -0.1232 0.4293 0.100 Uiso 1 1 calc R . . C51 C 0.2669(7) 0.6237(6) 0.3946(5) 0.056(3) Uani 1 1 d . . . H51A H 0.3106 0.6020 0.3684 0.067 Uiso 1 1 calc R . . H51B H 0.3115 0.6805 0.4269 0.067 Uiso 1 1 calc R . . C52 C 0.1603(7) 0.6253(6) 0.3357(6) 0.055(3) Uani 1 1 d . . . H52A H 0.1214 0.6546 0.3610 0.066 Uiso 1 1 calc R . . H52B H 0.1755 0.6540 0.2984 0.066 Uiso 1 1 calc R . . C53 C 0.3258(7) 0.5253(6) 0.4642(5) 0.059(3) Uani 1 1 d . . . H53A H 0.4016 0.5648 0.4866 0.071 Uiso 1 1 calc R . . H53B H 0.3155 0.4985 0.5039 0.071 Uiso 1 1 calc R . . C54 C 0.3145(7) 0.4623(7) 0.3981(5) 0.056(3) Uani 1 1 d . . . H54A H 0.3378 0.4894 0.3624 0.067 Uiso 1 1 calc R . . H54B H 0.3635 0.4287 0.4157 0.067 Uiso 1 1 calc R . . C55 C 0.2449(7) 0.6206(6) 0.5142(5) 0.052(3) Uani 1 1 d . . . H55A H 0.2290 0.5840 0.5454 0.078 Uiso 1 1 calc R . . H55B H 0.1886 0.6490 0.5015 0.078 Uiso 1 1 calc R . . H55C H 0.3182 0.6615 0.5433 0.078 Uiso 1 1 calc R . . C61 C -0.2505(7) 0.3768(6) 0.2290(5) 0.050(3) Uani 1 1 d . . . H61A H -0.3226 0.3692 0.2340 0.059 Uiso 1 1 calc R . . H61B H -0.2526 0.3242 0.1977 0.059 Uiso 1 1 calc R . . C62 C -0.1567(6) 0.4013(6) 0.3080(5) 0.041(2) Uani 1 1 d . . . H62A H -0.1621 0.4484 0.3423 0.049 Uiso 1 1 calc R . . H62B H -0.1605 0.3544 0.3314 0.049 Uiso 1 1 calc R . . C63 C -0.2647(7) 0.4112(7) 0.1071(5) 0.052(3) Uani 1 1 d . . . H63A H -0.2647 0.4568 0.0822 0.062 Uiso 1 1 calc R . . H63B H -0.3415 0.3733 0.0858 0.062 Uiso 1 1 calc R . . C64 C -0.1912(7) 0.3652(7) 0.0880(5) 0.055(3) Uani 1 1 d . . . H64A H -0.1986 0.3147 0.1061 0.066 Uiso 1 1 calc R . . H64B H -0.2131 0.3487 0.0318 0.066 Uiso 1 1 calc R . . C65 C -0.2934(7) 0.5022(7) 0.2047(6) 0.060(3) Uani 1 1 d . . . H65A H -0.2680 0.5261 0.2601 0.091 Uiso 1 1 calc R . . H65B H -0.3725 0.4712 0.1835 0.091 Uiso 1 1 calc R . . H65C H -0.2817 0.5465 0.1799 0.091 Uiso 1 1 calc R . . C71 C 0.8157(7) 0.7894(6) 0.7026(5) 0.043(3) Uani 1 1 d . . . H71A H 0.8236 0.7546 0.6595 0.051 Uiso 1 1 calc R . . H71B H 0.7793 0.8296 0.6831 0.051 Uiso 1 1 calc R . . C72 C 0.7455(7) 0.7356(6) 0.7347(5) 0.042(2) Uani 1 1 d . . . H72A H 0.7288 0.7702 0.7730 0.051 Uiso 1 1 calc R . . H72B H 0.6749 0.6994 0.6930 0.051 Uiso 1 1 calc R . . C73 C 1.0163(8) 0.8427(7) 0.7363(7) 0.075(4) Uani 1 1 d . . . H73A H 0.9987 0.8691 0.6937 0.090 Uiso 1 1 calc R . . H73B H 1.0858 0.8801 0.7782 0.090 Uiso 1 1 calc R . . C74 C 1.0349(8) 0.7647(7) 0.7093(6) 0.058(3) Uani 1 1 d . . . H74A H 0.9708 0.7303 0.6618 0.070 Uiso 1 1 calc R . . H74B H 1.1018 0.7760 0.6975 0.070 Uiso 1 1 calc R . . C75 C 0.9287(11) 0.9165(7) 0.8029(7) 0.103(5) Uani 1 1 d . . . H75A H 0.8675 0.9111 0.8201 0.154 Uiso 1 1 calc R . . H75B H 0.9212 0.9505 0.7667 0.154 Uiso 1 1 calc R . . H75C H 0.9993 0.9425 0.8473 0.154 Uiso 1 1 calc R . . C81 C 0.9232(9) 0.6110(8) 0.9861(5) 0.068(4) Uani 1 1 d . . . H81A H 0.9616 0.5711 0.9747 0.082 Uiso 1 1 calc R . . H81B H 0.9313 0.6182 1.0401 0.082 Uiso 1 1 calc R . . C82 C 0.9757(8) 0.6932(7) 0.9753(5) 0.055(3) Uani 1 1 d . . . H82A H 0.9448 0.7359 0.9926 0.067 Uiso 1 1 calc R . . H82B H 1.0570 0.7120 1.0041 0.067 Uiso 1 1 calc R . . C83 C 0.7678(10) 0.4885(8) 0.9065(6) 0.070(4) Uani 1 1 d . . . H83A H 0.6864 0.4684 0.8779 0.084 Uiso 1 1 calc R . . H83B H 0.7858 0.4648 0.9509 0.084 Uiso 1 1 calc R . . C84 C 0.8229(9) 0.4585(7) 0.8542(6) 0.069(3) Uani 1 1 d . . . H84A H 0.9040 0.4740 0.8833 0.083 Uiso 1 1 calc R . . H84B H 0.7934 0.3977 0.8339 0.083 Uiso 1 1 calc R . . C85 C 0.7331(9) 0.6038(7) 0.9725(6) 0.072(3) Uani 1 1 d . . . H85A H 0.7587 0.6640 0.9927 0.107 Uiso 1 1 calc R . . H85B H 0.7377 0.5782 1.0147 0.107 Uiso 1 1 calc R . . H85C H 0.6562 0.5859 0.9351 0.107 Uiso 1 1 calc R . . N1 N 0.6275(10) -0.0476(6) 0.8377(6) 0.093(3) Uani 1 1 d U . . N2 N 0.5355(8) 0.2722(6) 0.9249(4) 0.076(3) Uani 1 1 d . . . N3 N 0.4376(6) 0.1664(6) 0.5131(5) 0.058(3) Uani 1 1 d . . . N4 N 0.0704(6) -0.0261(5) 0.5851(4) 0.050(2) Uani 1 1 d . . . N5 N 0.0706(6) 0.4406(5) 0.4596(4) 0.042(2) Uani 1 1 d . . . N6 N -0.0682(6) 0.6009(6) 0.2012(4) 0.051(2) Uani 1 1 d . . . N7 N 1.0881(9) 0.8403(6) 0.9195(5) 0.086(4) Uani 1 1 d . . . N8 N 0.6292(7) 0.5890(6) 0.7922(5) 0.065(3) Uani 1 1 d . . . N10 N 0.7434(5) 0.0976(4) 0.8044(4) 0.0377(19) Uani 1 1 d . . . N20 N 0.3713(8) 0.1196(7) 0.9154(4) 0.068(3) Uani 1 1 d . . . N30 N 0.3376(6) 0.2642(5) 0.6011(4) 0.056(2) Uani 1 1 d . . . N40 N 0.2148(5) -0.1138(5) 0.5400(4) 0.049(2) Uani 1 1 d . . . N50 N 0.2432(5) 0.5716(5) 0.4429(4) 0.044(2) Uani 1 1 d . . . N60 N -0.2296(5) 0.4455(5) 0.1906(4) 0.048(2) Uani 1 1 d . . . N70 N 0.9258(7) 0.8336(5) 0.7646(4) 0.057(2) Uani 1 1 d . . . N80 N 0.8041(7) 0.5784(6) 0.9344(4) 0.055(2) Uani 1 1 d . . . O11 O 0.5336(5) 0.0167(4) 0.6892(3) 0.0462(19) Uani 1 1 d . . . O12 O 0.5885(4) 0.1642(4) 0.8217(3) 0.0384(15) Uani 1 1 d . . . O21 O 0.3320(6) 0.1645(5) 0.7805(3) 0.062(2) Uani 1 1 d . . . O22 O 0.4599(5) 0.0397(4) 0.8324(3) 0.0473(18) Uani 1 1 d . . . O31 O 0.5143(5) 0.2183(4) 0.6946(4) 0.0486(17) Uani 1 1 d D . . O32 O 0.2572(4) 0.1204(4) 0.6288(3) 0.0376(16) Uani 1 1 d . . . O41 O 0.2879(5) -0.0419(5) 0.6985(4) 0.0491(19) Uani 1 1 d . . . O42 O 0.3600(4) 0.0356(4) 0.5790(3) 0.0413(16) Uani 1 1 d . . . O51 O 0.2025(5) 0.4099(4) 0.3588(3) 0.0413(17) Uani 1 1 d . . . O52 O 0.0943(4) 0.5418(4) 0.2979(3) 0.0374(15) Uani 1 1 d . . . O61 O -0.0784(5) 0.4183(4) 0.1251(3) 0.0450(17) Uani 1 1 d D . . O62 O -0.0552(4) 0.4238(4) 0.2972(3) 0.0376(15) Uani 1 1 d . . . O71 O 1.0487(5) 0.7219(4) 0.7667(3) 0.0428(16) Uani 1 1 d D . . O72 O 0.8118(4) 0.6867(4) 0.7702(3) 0.0369(15) Uani 1 1 d . . . O81 O 0.7988(5) 0.4970(5) 0.7915(4) 0.0551(19) Uani 1 1 d D . . O82 O 0.9470(5) 0.6758(4) 0.8929(3) 0.0444(17) Uani 1 1 d . . . S2 S 0.4820(3) 0.4166(2) 0.9271(2) 0.1015(13) Uani 1 1 d . . . S3 S 0.4715(2) 0.2081(2) 0.39118(15) 0.0716(10) Uani 1 1 d . . . S4 S -0.14187(18) -0.05553(19) 0.58246(13) 0.0560(8) Uani 1 1 d . . . S5 S 0.0485(2) 0.38156(18) 0.57978(14) 0.0542(8) Uani 1 1 d . . . S6 S -0.0271(4) 0.7658(3) 0.2078(5) 0.203(3) Uani 1 1 d . . . S7 S 1.3143(3) 0.8774(2) 0.99633(17) 0.0873(11) Uani 1 1 d . . . S8 S 0.4330(2) 0.5514(3) 0.66600(17) 0.0876(12) Uani 1 1 d . . . Cu1 Cu 0.60037(9) 0.05323(7) 0.81949(6) 0.0392(3) Uani 1 1 d . . . Cu2 Cu 0.48540(10) 0.15703(8) 0.87247(6) 0.0513(4) Uani 1 1 d . . . Cu3 Cu 0.36244(8) 0.15072(8) 0.58259(6) 0.0458(4) Uani 1 1 d . . . Cu4 Cu 0.21912(8) 0.00170(8) 0.58867(6) 0.0414(3) Uani 1 1 d . . . Cu5 Cu 0.09095(8) 0.48740(7) 0.37864(5) 0.0365(3) Uani 1 1 d . . . Cu6 Cu -0.06475(8) 0.50378(7) 0.23715(6) 0.0377(3) Uani 1 1 d . . . Cu7 Cu 0.95526(10) 0.76141(8) 0.83900(6) 0.0511(4) Uani 1 1 d . . . Cu8 Cu 0.78724(9) 0.62423(8) 0.84137(6) 0.0437(3) Uani 1 1 d . . . S1 S 0.5215(4) -0.2218(3) 0.8038(2) 0.1223(15) Uani 1 1 d . . . C1 C 0.5682(10) -0.1142(10) 0.8159(7) 0.086(4) Uani 1 1 d U . . H31 H 0.553(8) 0.186(5) 0.714(6) 0.104 Uiso 1 1 d D . . H11 H 0.469(9) 0.018(7) 0.652(6) 0.104 Uiso 1 1 d . . . H21 H 0.321(10) 0.163(8) 0.739(6) 0.104 Uiso 1 1 d . . . H41 H 0.356(9) -0.018(7) 0.737(6) 0.104 Uiso 1 1 d . . . H51 H 0.184(10) 0.386(8) 0.317(6) 0.104 Uiso 1 1 d . . . H61 H -0.033(8) 0.388(6) 0.127(6) 0.104 Uiso 1 1 d D . . H71 H 1.048(9) 0.670(3) 0.755(6) 0.104 Uiso 1 1 d D . . H81 H 0.838(8) 0.487(7) 0.763(5) 0.104 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 C2 0.041(6) 0.077(9) 0.032(6) 0.003(6) -0.005(4) 0.026(6) C3 0.025(5) 0.032(6) 0.039(5) 0.018(5) 0.015(4) 0.012(4) C4 0.031(5) 0.046(7) 0.022(5) 0.007(4) 0.005(4) 0.011(5) C5 0.029(5) 0.055(7) 0.023(5) -0.003(5) -0.002(4) 0.025(5) C6 0.044(6) 0.065(9) 0.131(11) 0.046(9) 0.058(7) 0.036(7) C7 0.094(9) 0.037(7) 0.023(5) 0.003(5) -0.002(6) 0.016(7) C8 0.051(7) 0.118(11) 0.062(7) 0.061(7) 0.042(6) 0.044(7) C11 0.018(5) 0.040(7) 0.071(7) 0.023(6) -0.001(5) 0.005(5) C12 0.033(5) 0.037(6) 0.051(6) 0.010(5) -0.008(5) 0.011(5) C13 0.035(5) 0.055(7) 0.045(6) 0.022(5) 0.018(4) 0.022(5) C14 0.032(5) 0.077(8) 0.026(5) 0.022(5) 0.014(4) 0.021(5) C15 0.074(7) 0.038(7) 0.036(5) 0.002(5) -0.009(5) 0.029(6) C21 0.082(9) 0.117(13) 0.064(8) 0.040(8) 0.055(7) 0.034(9) C22 0.062(7) 0.085(9) 0.052(7) 0.030(6) 0.027(6) 0.014(7) C23 0.096(9) 0.149(14) 0.061(8) 0.044(8) 0.046(7) 0.081(10) C24 0.087(9) 0.177(15) 0.054(7) 0.052(8) 0.061(7) 0.071(9) C25 0.172(14) 0.210(17) 0.038(7) 0.051(9) 0.059(8) 0.138(13) C31 0.041(6) 0.067(8) 0.051(6) 0.020(6) 0.017(5) 0.024(6) C32 0.030(5) 0.106(10) 0.040(6) 0.039(6) 0.019(4) 0.033(6) C33 0.037(6) 0.056(8) 0.094(8) 0.036(7) 0.010(6) 0.011(6) C34 0.033(6) 0.073(9) 0.073(8) 0.033(7) 0.001(5) 0.010(6) C35 0.048(6) 0.105(10) 0.079(8) 0.074(8) 0.021(6) 0.033(7) C41 0.032(6) 0.094(10) 0.042(6) 0.000(6) 0.012(5) 0.028(6) C42 0.030(5) 0.113(11) 0.020(5) 0.003(6) 0.013(4) 0.032(6) C43 0.045(6) 0.061(8) 0.062(7) 0.002(6) 0.019(5) 0.006(6) C44 0.035(6) 0.064(8) 0.052(6) 0.009(6) 0.018(5) 0.002(6) C45 0.022(5) 0.086(9) 0.056(7) -0.016(6) -0.003(5) 0.006(5) C51 0.029(5) 0.049(7) 0.061(7) 0.004(6) 0.003(5) -0.007(5) C52 0.044(6) 0.045(7) 0.068(7) 0.018(6) 0.013(5) 0.012(5) C53 0.033(5) 0.064(8) 0.057(7) -0.015(6) -0.002(5) 0.024(5) C54 0.032(5) 0.069(8) 0.059(7) 0.011(6) 0.009(5) 0.023(5) C55 0.058(6) 0.051(7) 0.033(5) -0.007(5) 0.003(5) 0.025(6) C61 0.028(5) 0.067(8) 0.054(6) 0.030(6) 0.009(4) 0.016(5) C62 0.031(5) 0.058(7) 0.044(6) 0.033(5) 0.015(4) 0.017(5) C63 0.037(5) 0.069(8) 0.029(5) 0.008(5) -0.001(4) 0.003(5) C64 0.050(6) 0.067(8) 0.034(6) 0.012(5) 0.001(5) 0.013(6) C65 0.042(6) 0.081(9) 0.068(7) 0.038(6) 0.018(5) 0.029(6) C71 0.040(5) 0.050(7) 0.036(5) 0.026(5) 0.003(4) 0.018(5) C72 0.043(5) 0.054(7) 0.040(5) 0.022(5) 0.013(4) 0.029(5) C73 0.036(6) 0.076(10) 0.098(9) 0.059(8) -0.003(6) 0.009(6) C74 0.041(6) 0.084(9) 0.082(8) 0.063(7) 0.030(5) 0.035(6) C75 0.142(12) 0.055(9) 0.074(9) 0.009(7) -0.007(8) 0.047(9) C81 0.084(8) 0.114(11) 0.031(6) 0.030(7) 0.029(6) 0.058(8) C82 0.071(7) 0.077(9) 0.020(5) 0.007(5) 0.014(5) 0.037(7) C83 0.089(9) 0.100(11) 0.048(7) 0.039(7) 0.042(6) 0.040(8) C84 0.078(8) 0.060(8) 0.081(8) 0.036(7) 0.033(7) 0.028(7) C85 0.092(9) 0.093(10) 0.060(7) 0.030(7) 0.054(7) 0.042(8) N1 0.144(8) 0.042(6) 0.109(7) 0.006(5) 0.095(6) -0.001(5) N2 0.104(8) 0.064(7) 0.040(5) -0.007(5) -0.007(5) 0.061(6) N3 0.031(4) 0.100(8) 0.051(5) 0.040(5) 0.017(4) 0.021(5) N4 0.029(4) 0.063(6) 0.041(5) -0.001(4) 0.007(4) 0.005(4) N5 0.049(5) 0.048(6) 0.028(4) 0.001(4) 0.010(4) 0.029(4) N6 0.039(5) 0.059(7) 0.056(5) 0.023(5) 0.012(4) 0.021(5) N7 0.099(8) 0.060(7) 0.046(6) 0.007(5) -0.021(5) 0.012(6) N8 0.047(5) 0.104(8) 0.063(6) 0.051(6) 0.027(5) 0.030(5) N10 0.037(4) 0.034(5) 0.032(4) 0.010(4) 0.002(3) 0.010(4) N20 0.094(7) 0.101(9) 0.035(5) 0.027(5) 0.036(5) 0.052(7) N30 0.041(5) 0.084(7) 0.048(5) 0.040(5) 0.011(4) 0.022(5) N40 0.022(4) 0.067(6) 0.043(5) -0.012(4) 0.009(3) 0.008(4) N50 0.032(4) 0.044(5) 0.047(5) 0.003(4) 0.007(4) 0.018(4) N60 0.027(4) 0.056(6) 0.050(5) 0.019(4) 0.000(4) 0.015(4) N70 0.059(6) 0.047(6) 0.053(5) 0.011(5) 0.002(4) 0.025(5) N80 0.064(6) 0.076(7) 0.046(5) 0.027(5) 0.034(5) 0.036(5) O11 0.025(3) 0.079(5) 0.023(3) 0.003(3) 0.008(3) 0.004(3) O12 0.030(3) 0.041(4) 0.037(3) 0.013(3) 0.003(3) 0.013(3) O21 0.058(4) 0.110(7) 0.029(4) 0.023(4) 0.017(4) 0.046(4) O22 0.051(4) 0.057(5) 0.032(3) 0.014(3) 0.020(3) 0.006(4) O31 0.035(4) 0.048(5) 0.056(4) 0.024(4) 0.001(3) 0.019(3) O32 0.020(3) 0.058(5) 0.035(3) 0.018(3) 0.010(2) 0.009(3) O41 0.032(4) 0.061(5) 0.047(4) 0.005(4) 0.019(3) 0.002(4) O42 0.022(3) 0.074(5) 0.031(3) 0.018(3) 0.012(3) 0.017(3) O51 0.030(3) 0.054(5) 0.025(3) -0.002(3) 0.002(3) 0.010(3) O52 0.032(3) 0.038(4) 0.036(3) 0.011(3) 0.007(3) 0.007(3) O61 0.046(4) 0.048(5) 0.039(4) 0.014(3) 0.011(3) 0.016(3) O62 0.032(3) 0.048(4) 0.031(3) 0.016(3) 0.006(3) 0.014(3) O71 0.034(3) 0.042(4) 0.051(4) 0.026(4) 0.008(3) 0.014(3) O72 0.044(3) 0.050(4) 0.025(3) 0.014(3) 0.012(3) 0.031(3) O81 0.061(5) 0.073(5) 0.050(4) 0.027(4) 0.032(3) 0.033(4) O82 0.049(4) 0.061(5) 0.030(3) 0.017(3) 0.013(3) 0.031(3) S2 0.076(2) 0.074(3) 0.156(3) 0.027(2) 0.030(2) 0.052(2) S3 0.0359(14) 0.142(3) 0.0599(17) 0.066(2) 0.0223(13) 0.0372(17) S4 0.0217(12) 0.108(3) 0.0455(15) 0.0328(16) 0.0166(11) 0.0194(14) S5 0.0509(15) 0.076(2) 0.0565(16) 0.0401(15) 0.0250(13) 0.0352(15) S6 0.142(4) 0.083(3) 0.516(11) 0.137(5) 0.233(6) 0.079(3) S7 0.080(2) 0.105(3) 0.066(2) 0.034(2) 0.0021(17) 0.041(2) S8 0.0475(17) 0.152(4) 0.078(2) 0.064(2) 0.0164(15) 0.045(2) Cu1 0.0497(7) 0.0355(8) 0.0300(6) 0.0080(5) 0.0160(5) 0.0091(6) Cu2 0.0589(8) 0.0660(10) 0.0299(6) 0.0104(6) 0.0111(6) 0.0324(7) Cu3 0.0241(6) 0.0819(10) 0.0386(7) 0.0314(7) 0.0124(5) 0.0186(6) Cu4 0.0186(5) 0.0652(9) 0.0344(6) 0.0041(6) 0.0119(5) 0.0067(6) Cu5 0.0305(6) 0.0505(8) 0.0277(6) 0.0097(5) 0.0070(5) 0.0188(6) Cu6 0.0308(6) 0.0455(8) 0.0362(6) 0.0164(6) 0.0069(5) 0.0164(6) Cu7 0.0562(8) 0.0482(9) 0.0304(6) 0.0084(6) -0.0060(5) 0.0194(6) Cu8 0.0449(7) 0.0651(9) 0.0305(6) 0.0204(6) 0.0155(5) 0.0277(6) S1 0.153(4) 0.097(3) 0.127(3) 0.032(3) 0.071(3) 0.032(3) C1 0.072(7) 0.103(8) 0.079(7) 0.014(6) 0.024(5) 0.034(6) _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 C2 N2 1.147(12) . ? C2 S2 1.603(12) . ? C3 N3 1.148(9) . ? C3 S3 1.571(9) . ? C4 N4 1.149(10) . ? C4 S4 1.626(9) . ? C5 N5 1.154(10) . ? C5 S5 1.605(10) . ? C6 N6 1.134(12) . ? C6 S6 1.616(13) . ? C7 N7 1.159(13) . ? C7 S7 1.602(12) . ? C8 N8 1.170(11) . ? C8 S8 1.593(11) . ? C11 N10 1.488(11) . ? C11 C12 1.494(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O12 1.422(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N10 1.472(10) . ? C13 C14 1.511(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O11 1.428(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N10 1.488(10) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C21 N20 1.472(14) . ? C21 C22 1.528(14) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O22 1.436(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N20 1.508(13) . ? C23 C24 1.549(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O21 1.392(12) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N20 1.509(12) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C31 C32 1.475(13) . ? C31 N30 1.482(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O32 1.424(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N30 1.488(11) . ? C33 C34 1.512(12) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O31 1.421(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N30 1.481(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C41 N40 1.486(11) . ? C41 C42 1.501(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O42 1.440(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.497(12) . ? C43 N40 1.500(12) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O41 1.430(12) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 N40 1.494(10) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C51 N50 1.461(11) . ? C51 C52 1.508(11) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O52 1.422(10) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.468(12) . ? C53 N50 1.503(11) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O51 1.429(10) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 N50 1.476(11) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C61 C62 1.524(11) . ? C61 N60 1.525(11) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O62 1.432(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 N60 1.478(11) . ? C63 C64 1.502(13) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 O61 1.439(10) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N60 1.493(12) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C71 N70 1.477(10) . ? C71 C72 1.528(11) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 O72 1.449(9) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.469(15) . ? C73 N70 1.485(13) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 O71 1.415(10) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 N70 1.480(13) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C81 N80 1.483(12) . ? C81 C82 1.519(14) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 O82 1.456(9) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 N80 1.461(13) . ? C83 C84 1.530(14) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 O81 1.453(11) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 N80 1.485(12) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? N1 C1 1.153(14) . ? N1 Cu1 1.924(11) . ? N2 Cu2 1.918(9) . ? N3 Cu3 1.952(8) . ? N4 Cu4 1.927(8) . ? N5 Cu5 1.943(8) . ? N6 Cu6 1.925(9) . ? N7 Cu7 1.936(9) . ? N8 Cu8 1.911(8) . ? N10 Cu1 2.044(7) . ? N20 Cu2 2.016(9) . ? N30 Cu3 2.056(9) . ? N40 Cu4 2.035(8) . ? N50 Cu5 2.040(7) . ? N60 Cu6 2.020(7) . ? N70 Cu7 2.052(8) . ? N80 Cu8 2.042(7) . ? O11 Cu1 2.272(5) . ? O11 H11 0.93(11) . ? O12 Cu2 1.948(6) . ? O12 Cu1 1.956(6) . ? O21 Cu2 2.267(6) . ? O21 H21 0.76(11) . ? O22 Cu2 1.949(7) . ? O22 Cu1 1.962(6) . ? O31 Cu3 2.293(6) . ? O31 H31 0.897(15) . ? O32 Cu3 1.939(5) . ? O32 Cu4 1.945(6) . ? O41 Cu4 2.328(7) . ? O41 H41 0.91(11) . ? O42 Cu4 1.939(5) . ? O42 Cu3 1.971(7) . ? O51 Cu5 2.310(6) . ? O51 H51 0.76(11) . ? O52 Cu6 1.947(5) . ? O52 Cu5 1.957(5) . ? O61 Cu6 2.322(6) . ? O61 H61 0.89(2) . ? O62 Cu6 1.945(5) . ? O62 Cu5 1.969(5) . ? O71 Cu7 2.293(7) . ? O71 H71 0.89(2) . ? O72 Cu7 1.924(5) . ? O72 Cu8 1.950(5) . ? O81 Cu8 2.307(7) . ? O81 H81 0.91(2) . ? O82 Cu8 1.947(6) . ? O82 Cu7 1.951(6) . ? Cu1 Cu2 2.8962(17) . ? Cu3 Cu4 2.8940(16) . ? Cu5 Cu6 2.9231(13) . ? Cu7 Cu8 2.9020(17) . ? S1 C1 1.770(16) . ? 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 C2 S2 177.8(10) . . ? N3 C3 S3 179.3(9) . . ? N4 C4 S4 178.1(9) . . ? N5 C5 S5 179.6(9) . . ? N6 C6 S6 177.3(12) . . ? N7 C7 S7 178.0(11) . . ? N8 C8 S8 178.8(10) . . ? N10 C11 C12 110.0(8) . . ? N10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O12 C12 C11 104.8(7) . . ? O12 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? O12 C12 H12B 110.8 . . ? C11 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? N10 C13 C14 114.2(7) . . ? N10 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? N10 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? O11 C14 C13 107.7(6) . . ? O11 C14 H14A 110.2 . . ? C13 C14 H14A 110.2 . . ? O11 C14 H14B 110.2 . . ? C13 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? N10 C15 H15A 109.5 . . ? N10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N20 C21 C22 108.9(10) . . ? N20 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? N20 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O22 C22 C21 105.7(9) . . ? O22 C22 H22A 110.6 . . ? C21 C22 H22A 110.6 . . ? O22 C22 H22B 110.6 . . ? C21 C22 H22B 110.6 . . ? H22A C22 H22B 108.7 . . ? N20 C23 C24 109.4(9) . . ? N20 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? N20 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? O21 C24 C23 107.6(9) . . ? O21 C24 H24A 110.2 . . ? C23 C24 H24A 110.2 . . ? O21 C24 H24B 110.2 . . ? C23 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? N20 C25 H25A 109.5 . . ? N20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C32 C31 N30 107.7(8) . . ? C32 C31 H31A 110.2 . . ? N30 C31 H31A 110.2 . . ? C32 C31 H31B 110.2 . . ? N30 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? O32 C32 C31 109.5(7) . . ? O32 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? O32 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? N30 C33 C34 112.6(8) . . ? N30 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? N30 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? O31 C34 C33 109.5(9) . . ? O31 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? O31 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? N30 C35 H35A 109.5 . . ? N30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N40 C41 C42 108.6(9) . . ? N40 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? N40 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.3 . . ? O42 C42 C41 106.5(7) . . ? O42 C42 H42A 110.4 . . ? C41 C42 H42A 110.4 . . ? O42 C42 H42B 110.4 . . ? C41 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C44 C43 N40 113.2(8) . . ? C44 C43 H43A 108.9 . . ? N40 C43 H43A 108.9 . . ? C44 C43 H43B 108.9 . . ? N40 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? O41 C44 C43 108.0(8) . . ? O41 C44 H44A 110.1 . . ? C43 C44 H44A 110.1 . . ? O41 C44 H44B 110.1 . . ? C43 C44 H44B 110.1 . . ? H44A C44 H44B 108.4 . . ? N40 C45 H45A 109.5 . . ? N40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N50 C51 C52 110.1(7) . . ? N50 C51 H51A 109.6 . . ? C52 C51 H51A 109.6 . . ? N50 C51 H51B 109.6 . . ? C52 C51 H51B 109.6 . . ? H51A C51 H51B 108.2 . . ? O52 C52 C51 106.9(8) . . ? O52 C52 H52A 110.3 . . ? C51 C52 H52A 110.3 . . ? O52 C52 H52B 110.3 . . ? C51 C52 H52B 110.3 . . ? H52A C52 H52B 108.6 . . ? C54 C53 N50 112.3(7) . . ? C54 C53 H53A 109.2 . . ? N50 C53 H53A 109.2 . . ? C54 C53 H53B 109.2 . . ? N50 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? O51 C54 C53 110.7(8) . . ? O51 C54 H54A 109.5 . . ? C53 C54 H54A 109.5 . . ? O51 C54 H54B 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? N50 C55 H55A 109.5 . . ? N50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C62 C61 N60 107.9(7) . . ? C62 C61 H61A 110.1 . . ? N60 C61 H61A 110.1 . . ? C62 C61 H61B 110.1 . . ? N60 C61 H61B 110.1 . . ? H61A C61 H61B 108.4 . . ? O62 C62 C61 106.8(7) . . ? O62 C62 H62A 110.4 . . ? C61 C62 H62A 110.4 . . ? O62 C62 H62B 110.4 . . ? C61 C62 H62B 110.4 . . ? H62A C62 H62B 108.6 . . ? N60 C63 C64 113.1(7) . . ? N60 C63 H63A 109.0 . . ? C64 C63 H63A 109.0 . . ? N60 C63 H63B 109.0 . . ? C64 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? O61 C64 C63 108.6(8) . . ? O61 C64 H64A 110.0 . . ? C63 C64 H64A 110.0 . . ? O61 C64 H64B 110.0 . . ? C63 C64 H64B 110.0 . . ? H64A C64 H64B 108.4 . . ? N60 C65 H65A 109.5 . . ? N60 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N60 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N70 C71 C72 108.6(7) . . ? N70 C71 H71A 110.0 . . ? C72 C71 H71A 110.0 . . ? N70 C71 H71B 110.0 . . ? C72 C71 H71B 110.0 . . ? H71A C71 H71B 108.4 . . ? O72 C72 C71 105.6(6) . . ? O72 C72 H72A 110.6 . . ? C71 C72 H72A 110.6 . . ? O72 C72 H72B 110.6 . . ? C71 C72 H72B 110.6 . . ? H72A C72 H72B 108.7 . . ? C74 C73 N70 114.2(9) . . ? C74 C73 H73A 108.7 . . ? N70 C73 H73A 108.7 . . ? C74 C73 H73B 108.7 . . ? N70 C73 H73B 108.7 . . ? H73A C73 H73B 107.6 . . ? O71 C74 C73 109.6(9) . . ? O71 C74 H74A 109.8 . . ? C73 C74 H74A 109.8 . . ? O71 C74 H74B 109.8 . . ? C73 C74 H74B 109.8 . . ? H74A C74 H74B 108.2 . . ? N70 C75 H75A 109.5 . . ? N70 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N70 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N80 C81 C82 110.1(8) . . ? N80 C81 H81A 109.6 . . ? C82 C81 H81A 109.6 . . ? N80 C81 H81B 109.6 . . ? C82 C81 H81B 109.6 . . ? H81A C81 H81B 108.2 . . ? O82 C82 C81 103.8(8) . . ? O82 C82 H82A 111.0 . . ? C81 C82 H82A 111.0 . . ? O82 C82 H82B 111.0 . . ? C81 C82 H82B 111.0 . . ? H82A C82 H82B 109.0 . . ? N80 C83 C84 112.2(9) . . ? N80 C83 H83A 109.2 . . ? C84 C83 H83A 109.2 . . ? N80 C83 H83B 109.2 . . ? C84 C83 H83B 109.2 . . ? H83A C83 H83B 107.9 . . ? O81 C84 C83 107.8(8) . . ? O81 C84 H84A 110.2 . . ? C83 C84 H84A 110.2 . . ? O81 C84 H84B 110.2 . . ? C83 C84 H84B 110.2 . . ? H84A C84 H84B 108.5 . . ? N80 C85 H85A 109.5 . . ? N80 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? N80 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C1 N1 Cu1 130.4(12) . . ? C2 N2 Cu2 143.4(8) . . ? C3 N3 Cu3 157.0(7) . . ? C4 N4 Cu4 175.8(9) . . ? C5 N5 Cu5 177.3(8) . . ? C6 N6 Cu6 156.9(10) . . ? C7 N7 Cu7 144.3(10) . . ? C8 N8 Cu8 153.1(8) . . ? C13 N10 C11 114.3(7) . . ? C13 N10 C15 109.9(7) . . ? C11 N10 C15 109.3(6) . . ? C13 N10 Cu1 105.6(5) . . ? C11 N10 Cu1 105.4(5) . . ? C15 N10 Cu1 112.4(6) . . ? C21 N20 C25 110.8(9) . . ? C21 N20 C23 111.4(10) . . ? C25 N20 C23 106.0(9) . . ? C21 N20 Cu2 107.7(7) . . ? C25 N20 Cu2 113.0(8) . . ? C23 N20 Cu2 107.9(7) . . ? C35 N30 C33 109.2(8) . . ? C35 N30 C31 108.5(7) . . ? C33 N30 C31 111.9(8) . . ? C35 N30 Cu3 113.3(7) . . ? C33 N30 Cu3 106.9(6) . . ? C31 N30 Cu3 107.1(6) . . ? C41 N40 C45 109.4(7) . . ? C41 N40 C43 110.8(8) . . ? C45 N40 C43 108.7(8) . . ? C41 N40 Cu4 108.0(6) . . ? C45 N40 Cu4 112.5(6) . . ? C43 N40 Cu4 107.5(6) . . ? C51 N50 C55 111.6(8) . . ? C51 N50 C53 111.3(8) . . ? C55 N50 C53 108.3(7) . . ? C51 N50 Cu5 106.5(5) . . ? C55 N50 Cu5 111.2(6) . . ? C53 N50 Cu5 108.0(6) . . ? C63 N60 C65 110.0(7) . . ? C63 N60 C61 110.7(8) . . ? C65 N60 C61 108.3(7) . . ? C63 N60 Cu6 108.6(6) . . ? C65 N60 Cu6 111.8(6) . . ? C61 N60 Cu6 107.3(5) . . ? C71 N70 C75 110.5(8) . . ? C71 N70 C73 112.4(8) . . ? C75 N70 C73 109.0(10) . . ? C71 N70 Cu7 106.9(6) . . ? C75 N70 Cu7 112.1(7) . . ? C73 N70 Cu7 105.9(6) . . ? C83 N80 C81 111.4(9) . . ? C83 N80 C85 109.3(9) . . ? C81 N80 C85 111.9(8) . . ? C83 N80 Cu8 107.4(6) . . ? C81 N80 Cu8 106.7(6) . . ? C85 N80 Cu8 110.1(6) . . ? C14 O11 Cu1 109.9(4) . . ? C14 O11 H11 109(7) . . ? Cu1 O11 H11 133(7) . . ? C12 O12 Cu2 125.0(5) . . ? C12 O12 Cu1 106.7(5) . . ? Cu2 O12 Cu1 95.8(2) . . ? C24 O21 Cu2 110.9(6) . . ? C24 O21 H21 117(9) . . ? Cu2 O21 H21 129(9) . . ? C22 O22 Cu2 109.0(6) . . ? C22 O22 Cu1 128.9(6) . . ? Cu2 O22 Cu1 95.6(3) . . ? C34 O31 Cu3 107.9(5) . . ? C34 O31 H31 137(7) . . ? Cu3 O31 H31 114(7) . . ? C32 O32 Cu3 106.7(5) . . ? C32 O32 Cu4 129.7(5) . . ? Cu3 O32 Cu4 96.3(3) . . ? C44 O41 Cu4 107.8(5) . . ? C44 O41 H41 98(8) . . ? Cu4 O41 H41 125(7) . . ? C42 O42 Cu4 108.3(5) . . ? C42 O42 Cu3 124.7(6) . . ? Cu4 O42 Cu3 95.5(3) . . ? C54 O51 Cu5 107.0(5) . . ? C54 O51 H51 118(9) . . ? Cu5 O51 H51 114(9) . . ? C52 O52 Cu6 125.8(5) . . ? C52 O52 Cu5 106.4(5) . . ? Cu6 O52 Cu5 97.0(2) . . ? C64 O61 Cu6 106.5(5) . . ? C64 O61 H61 109(8) . . ? Cu6 O61 H61 120(7) . . ? C62 O62 Cu6 107.6(5) . . ? C62 O62 Cu5 125.3(5) . . ? Cu6 O62 Cu5 96.6(3) . . ? C74 O71 Cu7 107.7(5) . . ? C74 O71 H71 119(8) . . ? Cu7 O71 H71 121(8) . . ? C72 O72 Cu7 107.6(5) . . ? C72 O72 Cu8 126.7(5) . . ? Cu7 O72 Cu8 97.0(2) . . ? C84 O81 Cu8 106.0(6) . . ? C84 O81 H81 110(7) . . ? Cu8 O81 H81 126(8) . . ? C82 O82 Cu8 107.7(5) . . ? C82 O82 Cu7 123.4(6) . . ? Cu8 O82 Cu7 96.2(2) . . ? O12 Cu1 O22 80.3(3) . . ? O12 Cu1 N1 169.3(4) . . ? O22 Cu1 N1 99.9(4) . . ? O12 Cu1 N10 84.5(3) . . ? O22 Cu1 N10 164.8(3) . . ? N1 Cu1 N10 95.2(4) . . ? O12 Cu1 O11 91.3(2) . . ? O22 Cu1 O11 99.1(2) . . ? N1 Cu1 O11 99.2(4) . . ? N10 Cu1 O11 80.2(2) . . ? O12 Cu1 Cu2 41.99(17) . . ? O22 Cu1 Cu2 42.04(19) . . ? N1 Cu1 Cu2 133.7(3) . . ? N10 Cu1 Cu2 123.8(2) . . ? O11 Cu1 Cu2 110.30(17) . . ? N2 Cu2 O12 96.0(4) . . ? N2 Cu2 O22 169.6(3) . . ? O12 Cu2 O22 80.8(2) . . ? N2 Cu2 N20 97.8(4) . . ? O12 Cu2 N20 165.9(4) . . ? O22 Cu2 N20 85.1(4) . . ? N2 Cu2 O21 94.2(3) . . ? O12 Cu2 O21 101.8(2) . . ? O22 Cu2 O21 96.2(3) . . ? N20 Cu2 O21 79.6(3) . . ? N2 Cu2 Cu1 130.7(3) . . ? O12 Cu2 Cu1 42.21(17) . . ? O22 Cu2 Cu1 42.39(17) . . ? N20 Cu2 Cu1 124.4(3) . . ? O21 Cu2 Cu1 115.54(19) . . ? O32 Cu3 N3 166.1(3) . . ? O32 Cu3 O42 80.2(2) . . ? N3 Cu3 O42 96.8(3) . . ? O32 Cu3 N30 84.7(3) . . ? N3 Cu3 N30 98.1(4) . . ? O42 Cu3 N30 164.9(3) . . ? O32 Cu3 O31 97.0(2) . . ? N3 Cu3 O31 96.8(3) . . ? O42 Cu3 O31 100.1(2) . . ? N30 Cu3 O31 80.8(3) . . ? O32 Cu3 Cu4 41.92(19) . . ? N3 Cu3 Cu4 129.7(3) . . ? O42 Cu3 Cu4 41.84(15) . . ? N30 Cu3 Cu4 124.0(2) . . ? O31 Cu3 Cu4 114.43(17) . . ? N4 Cu4 O42 171.4(3) . . ? N4 Cu4 O32 96.9(3) . . ? O42 Cu4 O32 80.8(2) . . ? N4 Cu4 N40 97.6(3) . . ? O42 Cu4 N40 84.2(3) . . ? O32 Cu4 N40 164.9(3) . . ? N4 Cu4 O41 93.3(3) . . ? O42 Cu4 O41 95.2(2) . . ? O32 Cu4 O41 103.2(2) . . ? N40 Cu4 O41 80.1(3) . . ? N4 Cu4 Cu3 132.0(3) . . ? O42 Cu4 Cu3 42.69(19) . . ? O32 Cu4 Cu3 41.76(16) . . ? N40 Cu4 Cu3 123.5(2) . . ? O41 Cu4 Cu3 115.49(16) . . ? N5 Cu5 O52 171.5(3) . . ? N5 Cu5 O62 97.0(3) . . ? O52 Cu5 O62 79.7(2) . . ? N5 Cu5 N50 97.8(3) . . ? O52 Cu5 N50 85.1(3) . . ? O62 Cu5 N50 164.7(3) . . ? N5 Cu5 O51 93.4(3) . . ? O52 Cu5 O51 95.0(2) . . ? O62 Cu5 O51 102.7(2) . . ? N50 Cu5 O51 80.2(3) . . ? N5 Cu5 Cu6 132.7(2) . . ? O52 Cu5 Cu6 41.38(15) . . ? O62 Cu5 Cu6 41.37(16) . . ? N50 Cu5 Cu6 123.6(2) . . ? O51 Cu5 Cu6 113.71(13) . . ? N6 Cu6 O62 165.9(3) . . ? N6 Cu6 O52 95.3(3) . . ? O62 Cu6 O52 80.5(2) . . ? N6 Cu6 N60 97.8(3) . . ? O62 Cu6 N60 85.6(3) . . ? O52 Cu6 N60 166.1(3) . . ? N6 Cu6 O61 97.2(3) . . ? O62 Cu6 O61 96.8(2) . . ? O52 Cu6 O61 102.2(2) . . ? N60 Cu6 O61 80.7(3) . . ? N6 Cu6 Cu5 128.9(2) . . ? O62 Cu6 Cu5 41.98(15) . . ? O52 Cu6 Cu5 41.64(16) . . ? N60 Cu6 Cu5 124.7(2) . . ? O61 Cu6 Cu5 114.86(15) . . ? O72 Cu7 N7 170.8(4) . . ? O72 Cu7 O82 80.9(2) . . ? N7 Cu7 O82 96.0(3) . . ? O72 Cu7 N70 85.2(3) . . ? N7 Cu7 N70 97.6(4) . . ? O82 Cu7 N70 166.0(3) . . ? O72 Cu7 O71 95.9(2) . . ? N7 Cu7 O71 93.2(4) . . ? O82 Cu7 O71 101.5(2) . . ? N70 Cu7 O71 80.5(3) . . ? O72 Cu7 Cu8 41.84(16) . . ? N7 Cu7 Cu8 132.2(3) . . ? O82 Cu7 Cu8 41.85(17) . . ? N70 Cu7 Cu8 124.6(2) . . ? O71 Cu7 Cu8 113.21(16) . . ? N8 Cu8 O82 172.0(4) . . ? N8 Cu8 O72 95.4(3) . . ? O82 Cu8 O72 80.3(2) . . ? N8 Cu8 N80 99.1(3) . . ? O82 Cu8 N80 84.6(3) . . ? O72 Cu8 N80 164.5(3) . . ? N8 Cu8 O81 93.0(3) . . ? O82 Cu8 O81 94.6(2) . . ? O72 Cu8 O81 103.3(2) . . ? N80 Cu8 O81 81.2(3) . . ? N8 Cu8 Cu7 131.8(3) . . ? O82 Cu8 Cu7 41.93(17) . . ? O72 Cu8 Cu7 41.15(16) . . ? N80 Cu8 Cu7 123.4(3) . . ? O81 Cu8 Cu7 113.34(17) . . ? N1 C1 S1 159.3(13) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.044 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.116 # Attachment '- CIF-Compound-2_corrected.cif' data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 777427' #TrackingRef '- CIF-Compound-2_corrected.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H84 Cu6 N24 O12, C12 H28 Cu2 N8 O4, H2 O' _chemical_formula_sum 'C48 H114 Cu8 N32 O17' _chemical_formula_weight 1920.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 17.7735(10) _cell_length_b 19.9819(11) _cell_length_c 21.8189(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7748.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4997 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 23.56 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3976 _exptl_absorpt_coefficient_mu 2.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5737 _exptl_absorpt_correction_T_max 0.7913 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26786 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0935 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.35 _reflns_number_total 13924 _reflns_number_gt 10977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+8.6356P] 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_abs_structure_details 'Flack (1983), 6281 Friedel pairs' _refine_ls_abs_structure_Flack 0.472(17) _refine_ls_number_reflns 13924 _refine_ls_number_parameters 972 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.000 _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 C11 C 0.2655(4) 0.5950(4) 0.5754(4) 0.0276(17) Uani 1 1 d . . . H11A H 0.2493 0.5477 0.5735 0.033 Uiso 1 1 calc R . . H11B H 0.2203 0.6227 0.5833 0.033 Uiso 1 1 calc R . . C12 C 0.2976(4) 0.6142(4) 0.5152(4) 0.0291(18) Uani 1 1 d . . . H12A H 0.3403 0.5845 0.5047 0.035 Uiso 1 1 calc R . . H12B H 0.2589 0.6100 0.4828 0.035 Uiso 1 1 calc R . . C13 C 0.3835(4) 0.5543(3) 0.6232(4) 0.0260(17) Uani 1 1 d . . . H13A H 0.3894 0.5391 0.5803 0.031 Uiso 1 1 calc R . . H13B H 0.3733 0.5147 0.6492 0.031 Uiso 1 1 calc R . . C14 C 0.4547(4) 0.5889(3) 0.6445(4) 0.0247(17) Uani 1 1 d . . . H14A H 0.4520 0.5983 0.6890 0.030 Uiso 1 1 calc R . . H14B H 0.4990 0.5600 0.6368 0.030 Uiso 1 1 calc R . . C15 C 0.2810(5) 0.5957(3) 0.6876(4) 0.0274(18) Uani 1 1 d . . . H15A H 0.2455 0.6334 0.6928 0.033 Uiso 1 1 calc R . . H15B H 0.3193 0.5993 0.7204 0.033 Uiso 1 1 calc R . . C16 C 0.2378(5) 0.5302(4) 0.6965(4) 0.039(2) Uani 1 1 d . . . H16A H 0.2157 0.5292 0.7376 0.059 Uiso 1 1 calc R . . H16B H 0.2723 0.4923 0.6918 0.059 Uiso 1 1 calc R . . H16C H 0.1977 0.5270 0.6658 0.059 Uiso 1 1 calc R . . C21 C 0.6297(4) 0.8277(4) 0.6101(4) 0.034(2) Uani 1 1 d . . . H21A H 0.6711 0.7998 0.6264 0.041 Uiso 1 1 calc R . . H21B H 0.6470 0.8748 0.6104 0.041 Uiso 1 1 calc R . . C22 C 0.6144(4) 0.8073(4) 0.5451(4) 0.0309(19) Uani 1 1 d . . . H22A H 0.5779 0.8386 0.5263 0.037 Uiso 1 1 calc R . . H22B H 0.6615 0.8090 0.5210 0.037 Uiso 1 1 calc R . . C23 C 0.5025(4) 0.8693(3) 0.6346(4) 0.0230(17) Uani 1 1 d . . . H23A H 0.5083 0.8839 0.5915 0.028 Uiso 1 1 calc R . . H23B H 0.5052 0.9093 0.6612 0.028 Uiso 1 1 calc R . . C24 C 0.4277(4) 0.8348(3) 0.6430(3) 0.0237(16) Uani 1 1 d . . . H24A H 0.4186 0.8252 0.6869 0.028 Uiso 1 1 calc R . . H24B H 0.3864 0.8635 0.6276 0.028 Uiso 1 1 calc R . . C25 C 0.5839(5) 0.8298(4) 0.7183(4) 0.041(2) Uani 1 1 d . . . H25A H 0.5376 0.8243 0.7430 0.049 Uiso 1 1 calc R . . H25B H 0.6192 0.7937 0.7302 0.049 Uiso 1 1 calc R . . C26 C 0.6189(6) 0.8959(5) 0.7336(5) 0.061(3) Uani 1 1 d . . . H26A H 0.6303 0.8975 0.7776 0.091 Uiso 1 1 calc R . . H26B H 0.5838 0.9320 0.7232 0.091 Uiso 1 1 calc R . . H26C H 0.6655 0.9014 0.7102 0.091 Uiso 1 1 calc R . . C31 C 0.5758(4) 0.5404(3) 0.4376(3) 0.0234(17) Uani 1 1 d . . . H31A H 0.6261 0.5191 0.4395 0.028 Uiso 1 1 calc R . . H31B H 0.5398 0.5068 0.4217 0.028 Uiso 1 1 calc R . . C32 C 0.5523(4) 0.5606(4) 0.5014(3) 0.0241(17) Uani 1 1 d . . . H32A H 0.5447 0.5202 0.5270 0.029 Uiso 1 1 calc R . . H32B H 0.5923 0.5881 0.5206 0.029 Uiso 1 1 calc R . . C33 C 0.6373(4) 0.6481(3) 0.4127(4) 0.0239(16) Uani 1 1 d . . . H33A H 0.6495 0.6428 0.4567 0.029 Uiso 1 1 calc R . . H33B H 0.6838 0.6403 0.3888 0.029 Uiso 1 1 calc R . . C34 C 0.6088(4) 0.7187(3) 0.4009(3) 0.0227(16) Uani 1 1 d . . . H34A H 0.6435 0.7519 0.4192 0.027 Uiso 1 1 calc R . . H34B H 0.6056 0.7273 0.3563 0.027 Uiso 1 1 calc R . . C35 C 0.5884(4) 0.5757(4) 0.3302(3) 0.0264(17) Uani 1 1 d . . . H35A H 0.5954 0.6157 0.3040 0.032 Uiso 1 1 calc R . . H35B H 0.5414 0.5534 0.3169 0.032 Uiso 1 1 calc R . . C36 C 0.6538(5) 0.5281(4) 0.3188(4) 0.036(2) Uani 1 1 d . . . H36A H 0.6555 0.5163 0.2752 0.055 Uiso 1 1 calc R . . H36B H 0.6469 0.4874 0.3433 0.055 Uiso 1 1 calc R . . H36C H 0.7010 0.5499 0.3305 0.055 Uiso 1 1 calc R . . C41 C 0.3472(5) 0.8881(4) 0.4327(4) 0.0325(19) Uani 1 1 d . . . H41A H 0.2955 0.9061 0.4290 0.039 Uiso 1 1 calc R . . H41B H 0.3826 0.9261 0.4290 0.039 Uiso 1 1 calc R . . C42 C 0.3562(4) 0.8568(4) 0.4950(3) 0.0303(18) Uani 1 1 d . . . H42A H 0.3489 0.8910 0.5274 0.036 Uiso 1 1 calc R . . H42B H 0.3182 0.8211 0.5009 0.036 Uiso 1 1 calc R . . C43 C 0.3013(4) 0.7878(3) 0.3801(3) 0.0227(16) Uani 1 1 d . . . H43A H 0.2653 0.7979 0.3468 0.027 Uiso 1 1 calc R . . H43B H 0.2733 0.7879 0.4193 0.027 Uiso 1 1 calc R . . C44 C 0.3353(4) 0.7195(3) 0.3698(3) 0.0245(16) Uani 1 1 d . . . H44A H 0.2968 0.6843 0.3760 0.029 Uiso 1 1 calc R . . H44B H 0.3547 0.7159 0.3274 0.029 Uiso 1 1 calc R . . C45 C 0.3624(5) 0.8810(4) 0.3247(4) 0.0321(19) Uani 1 1 d . . . H45A H 0.3153 0.9073 0.3222 0.039 Uiso 1 1 calc R . . H45B H 0.4047 0.9132 0.3272 0.039 Uiso 1 1 calc R . . C46 C 0.3705(5) 0.8420(4) 0.2679(4) 0.041(2) Uani 1 1 d . . . H46A H 0.3719 0.8725 0.2327 0.061 Uiso 1 1 calc R . . H46B H 0.3277 0.8115 0.2637 0.061 Uiso 1 1 calc R . . H46C H 0.4173 0.8161 0.2695 0.061 Uiso 1 1 calc R . . C51 C 0.4634(4) 0.0745(3) 0.5339(3) 0.0237(16) Uani 1 1 d . . . H51A H 0.4373 0.0332 0.5472 0.028 Uiso 1 1 calc R . . H51B H 0.5178 0.0643 0.5310 0.028 Uiso 1 1 calc R . . C52 C 0.4350(4) 0.0941(4) 0.4719(4) 0.0263(17) Uani 1 1 d . . . H52A H 0.4664 0.1307 0.4550 0.032 Uiso 1 1 calc R . . H52B H 0.4379 0.0555 0.4436 0.032 Uiso 1 1 calc R . . C53 C 0.4993(3) 0.1881(3) 0.5689(4) 0.0203(16) Uani 1 1 d . . . H53A H 0.5121 0.1901 0.5248 0.024 Uiso 1 1 calc R . . H53B H 0.5467 0.1852 0.5925 0.024 Uiso 1 1 calc R . . C54 C 0.4569(4) 0.2500(3) 0.5870(3) 0.0203(15) Uani 1 1 d . . . H54A H 0.4492 0.2510 0.6319 0.024 Uiso 1 1 calc R . . H54B H 0.4855 0.2905 0.5749 0.024 Uiso 1 1 calc R . . C55 C 0.4664(4) 0.1011(4) 0.6448(4) 0.0280(17) Uani 1 1 d . . . H55A H 0.4283 0.0664 0.6540 0.034 Uiso 1 1 calc R . . H55B H 0.4588 0.1381 0.6743 0.034 Uiso 1 1 calc R . . C56 C 0.5444(5) 0.0710(4) 0.6559(4) 0.040(2) Uani 1 1 d . . . H56A H 0.5476 0.0546 0.6982 0.060 Uiso 1 1 calc R . . H56B H 0.5829 0.1054 0.6493 0.060 Uiso 1 1 calc R . . H56C H 0.5527 0.0338 0.6275 0.060 Uiso 1 1 calc R . . C61 C 0.1717(5) 0.3848(4) 0.5575(4) 0.036(2) Uani 1 1 d . . . H61A H 0.2019 0.4244 0.5696 0.043 Uiso 1 1 calc R . . H61B H 0.1179 0.3970 0.5611 0.043 Uiso 1 1 calc R . . C62 C 0.1888(5) 0.3677(5) 0.4917(4) 0.043(2) Uani 1 1 d . . . H62A H 0.1539 0.3325 0.4772 0.051 Uiso 1 1 calc R . . H62B H 0.1818 0.4078 0.4656 0.051 Uiso 1 1 calc R . . C63 C 0.1389(4) 0.2699(3) 0.5909(4) 0.0241(17) Uani 1 1 d . . . H63A H 0.0971 0.2708 0.6208 0.029 Uiso 1 1 calc R . . H63B H 0.1171 0.2710 0.5492 0.029 Uiso 1 1 calc R . . C64 C 0.1839(4) 0.2076(3) 0.5991(3) 0.0229(15) Uani 1 1 d . . . H64A H 0.1984 0.2025 0.6427 0.027 Uiso 1 1 calc R . . H64B H 0.1535 0.1681 0.5871 0.027 Uiso 1 1 calc R . . C65 C 0.1859(4) 0.3516(4) 0.6664(4) 0.033(2) Uani 1 1 d . . . H65A H 0.1917 0.3116 0.6928 0.039 Uiso 1 1 calc R . . H65B H 0.2297 0.3810 0.6740 0.039 Uiso 1 1 calc R . . C66 C 0.1172(6) 0.3874(5) 0.6854(5) 0.061(3) Uani 1 1 d . . . H66A H 0.1211 0.3996 0.7287 0.091 Uiso 1 1 calc R . . H66B H 0.0734 0.3584 0.6794 0.091 Uiso 1 1 calc R . . H66C H 0.1115 0.4280 0.6606 0.091 Uiso 1 1 calc R . . C71 C 0.1383(4) 0.0913(3) 0.3920(4) 0.0251(17) Uani 1 1 d . . . H71A H 0.0903 0.1140 0.3824 0.030 Uiso 1 1 calc R . . H71B H 0.1289 0.0424 0.3913 0.030 Uiso 1 1 calc R . . C72 C 0.1627(4) 0.1110(3) 0.4545(3) 0.0233(16) Uani 1 1 d . . . H72A H 0.1220 0.1015 0.4843 0.028 Uiso 1 1 calc R . . H72B H 0.2076 0.0849 0.4665 0.028 Uiso 1 1 calc R . . C73 C 0.2637(4) 0.0684(3) 0.3488(3) 0.0178(15) Uani 1 1 d . . . H73A H 0.2613 0.0295 0.3208 0.021 Uiso 1 1 calc R . . H73B H 0.2691 0.0514 0.3912 0.021 Uiso 1 1 calc R . . C74 C 0.3308(4) 0.1120(3) 0.3324(4) 0.0212(16) Uani 1 1 d . . . H74A H 0.3784 0.0877 0.3406 0.025 Uiso 1 1 calc R . . H74B H 0.3293 0.1242 0.2885 0.025 Uiso 1 1 calc R . . C75 C 0.1596(4) 0.1021(3) 0.2810(3) 0.0244(17) Uani 1 1 d . . . H75A H 0.1983 0.1142 0.2503 0.029 Uiso 1 1 calc R . . H75B H 0.1187 0.1355 0.2778 0.029 Uiso 1 1 calc R . . C76 C 0.1276(5) 0.0337(4) 0.2639(4) 0.040(2) Uani 1 1 d . . . H76A H 0.1071 0.0354 0.2223 0.059 Uiso 1 1 calc R . . H76B H 0.0875 0.0217 0.2927 0.059 Uiso 1 1 calc R . . H76C H 0.1677 0.0000 0.2658 0.059 Uiso 1 1 calc R . . C81 C 0.4696(4) 0.3670(4) 0.3758(3) 0.0259(17) Uani 1 1 d . . . H81A H 0.4804 0.4156 0.3762 0.031 Uiso 1 1 calc R . . H81B H 0.5139 0.3439 0.3582 0.031 Uiso 1 1 calc R . . C82 C 0.4582(4) 0.3432(4) 0.4414(3) 0.0284(18) Uani 1 1 d . . . H82A H 0.5056 0.3482 0.4648 0.034 Uiso 1 1 calc R . . H82B H 0.4190 0.3706 0.4616 0.034 Uiso 1 1 calc R . . C83 C 0.3357(4) 0.3930(3) 0.3551(3) 0.0215(16) Uani 1 1 d . . . H83A H 0.3398 0.4053 0.3990 0.026 Uiso 1 1 calc R . . H83B H 0.3326 0.4347 0.3309 0.026 Uiso 1 1 calc R . . C84 C 0.2658(4) 0.3518(3) 0.3452(4) 0.0235(16) Uani 1 1 d . . . H84A H 0.2212 0.3755 0.3617 0.028 Uiso 1 1 calc R . . H84B H 0.2578 0.3438 0.3009 0.028 Uiso 1 1 calc R . . C85 C 0.4216(4) 0.3672(3) 0.2705(3) 0.0231(16) Uani 1 1 d . . . H85A H 0.3753 0.3604 0.2460 0.028 Uiso 1 1 calc R . . H85B H 0.4590 0.3337 0.2568 0.028 Uiso 1 1 calc R . . C86 C 0.4528(4) 0.4381(3) 0.2568(3) 0.0247(17) Uani 1 1 d . . . H86A H 0.4633 0.4422 0.2128 0.037 Uiso 1 1 calc R . . H86B H 0.4993 0.4452 0.2800 0.037 Uiso 1 1 calc R . . H86C H 0.4155 0.4718 0.2688 0.037 Uiso 1 1 calc R . . N1 N 0.3191(3) 0.6033(3) 0.6277(3) 0.0211(14) Uani 1 1 d . . . N2 N 0.5641(3) 0.8215(3) 0.6510(3) 0.0243(14) Uani 1 1 d . . . N3 N 0.5788(3) 0.5982(3) 0.3947(3) 0.0222(14) Uani 1 1 d . . . N4 N 0.3610(3) 0.8407(3) 0.3819(3) 0.0240(14) Uani 1 1 d . . . N5 N 0.4519(3) 0.1275(3) 0.5812(3) 0.0223(13) Uani 1 1 d . . . N6 N 0.1882(3) 0.3292(3) 0.6002(3) 0.0246(14) Uani 1 1 d . . . N7 N 0.1941(3) 0.1079(3) 0.3436(3) 0.0172(12) Uani 1 1 d . . . N8 N 0.4036(3) 0.3543(3) 0.3363(3) 0.0182(13) Uani 1 1 d . . . N11 N 0.2757(3) 0.7501(3) 0.6434(3) 0.0279(14) Uani 1 1 d . . . N12 N 0.2509(3) 0.7586(3) 0.6934(3) 0.0148(12) Uani 1 1 d . . . N13 N 0.2228(3) 0.7680(3) 0.7402(3) 0.0267(14) Uani 1 1 d . . . N21 N 0.6042(3) 0.6791(3) 0.6769(3) 0.0278(15) Uani 1 1 d . . . N22 N 0.6331(3) 0.6320(3) 0.6504(3) 0.0256(14) Uani 1 1 d . . . N23 N 0.6636(4) 0.5878(3) 0.6278(3) 0.0338(17) Uani 1 1 d . . . N31 N 0.4188(4) 0.5715(3) 0.3688(3) 0.0298(16) Uani 1 1 d . . . N32 N 0.3542(4) 0.5651(3) 0.3645(3) 0.0355(17) Uani 1 1 d . . . N33 N 0.2888(4) 0.5557(4) 0.3620(5) 0.066(3) Uani 1 1 d . . . N41 N 0.5301(4) 0.8622(3) 0.3827(3) 0.0301(15) Uani 1 1 d . . . N42 N 0.5454(4) 0.9091(3) 0.4134(3) 0.0297(15) Uani 1 1 d . . . N43 N 0.5621(5) 0.9563(4) 0.4402(5) 0.069(3) Uani 1 1 d . . . N51 N 0.2916(4) 0.0841(3) 0.6125(3) 0.0329(16) Uani 1 1 d . A . N61 N 0.3432(4) 0.3789(3) 0.6097(3) 0.0304(16) Uani 1 1 d . . . N62 N 0.4031(4) 0.3991(3) 0.5921(3) 0.0279(15) Uani 1 1 d . . . N63 N 0.4609(4) 0.4209(3) 0.5774(4) 0.0396(18) Uani 1 1 d . . . N71 N 0.1262(3) 0.2477(3) 0.3367(3) 0.0228(13) Uani 1 1 d . . . N72 N 0.1082(3) 0.2702(3) 0.2889(3) 0.0194(13) Uani 1 1 d . . . N73 N 0.0873(4) 0.2926(3) 0.2436(3) 0.0339(16) Uani 1 1 d . . . N81 N 0.4647(3) 0.2156(3) 0.3132(3) 0.0260(14) Uani 1 1 d . . . N82 N 0.4846(3) 0.2128(3) 0.2612(3) 0.0217(13) Uani 1 1 d . . . N83 N 0.5081(4) 0.2090(3) 0.2119(3) 0.0338(16) Uani 1 1 d . . . O10 O 0.6822(4) 0.6903(3) 0.7940(3) 0.0542(18) Uani 1 1 d . . . O11 O 0.3232(3) 0.6828(2) 0.5194(2) 0.0246(12) Uani 1 1 d D . . O12 O 0.4613(2) 0.6502(2) 0.6108(2) 0.0169(10) Uani 1 1 d . . . O21 O 0.5846(3) 0.7410(2) 0.5443(2) 0.0247(11) Uani 1 1 d D . . O22 O 0.4310(2) 0.7738(2) 0.6087(2) 0.0162(10) Uani 1 1 d . . . O31 O 0.4838(3) 0.5982(2) 0.4984(2) 0.0225(11) Uani 1 1 d D . . O32 O 0.5366(2) 0.7242(2) 0.4280(2) 0.0187(10) Uani 1 1 d . . . O41 O 0.4299(3) 0.8296(2) 0.4987(2) 0.0236(11) Uani 1 1 d D . . O42 O 0.3952(2) 0.7114(2) 0.4128(2) 0.0201(10) Uani 1 1 d . . . O51 O 0.3583(3) 0.1161(2) 0.4775(2) 0.0218(11) Uani 1 1 d . . . O52 O 0.3863(2) 0.2482(2) 0.5560(2) 0.0169(10) Uani 1 1 d . . . O61 O 0.2651(3) 0.3445(2) 0.4871(2) 0.0268(12) Uani 1 1 d . . . O62 O 0.2488(2) 0.2115(2) 0.5623(2) 0.0188(10) Uani 1 1 d . . . O71 O 0.1800(3) 0.1810(2) 0.4551(2) 0.0220(11) Uani 1 1 d . . . H71 H 0.1748 0.2109 0.4887 0.026 Uiso 1 1 calc R . . O72 O 0.3264(2) 0.1701(2) 0.3693(2) 0.0171(10) Uani 1 1 d . . . O81 O 0.4360(3) 0.2749(3) 0.4409(2) 0.0256(12) Uani 1 1 d D . . O82 O 0.2769(2) 0.2900(2) 0.3766(2) 0.0166(10) Uani 1 1 d . . . Cu1 Cu 0.36447(4) 0.69712(4) 0.62020(4) 0.01745(19) Uani 1 1 d . . . Cu2 Cu 0.52234(5) 0.72703(4) 0.63479(4) 0.01876(19) Uani 1 1 d . . . Cu3 Cu 0.47659(5) 0.64648(4) 0.40273(4) 0.01834(19) Uani 1 1 d . . . Cu4 Cu 0.46023(4) 0.79070(4) 0.40492(4) 0.01899(19) Uani 1 1 d . . . Cu5 Cu 0.34203(5) 0.16004(4) 0.57273(4) 0.01807(19) Uani 1 1 d . . . Cu6 Cu 0.29557(4) 0.29876(4) 0.57818(4) 0.01767(18) Uani 1 1 d . . . Cu7 Cu 0.22318(4) 0.20660(4) 0.35819(4) 0.01639(18) Uani 1 1 d . . . Cu8 Cu 0.37554(4) 0.25520(4) 0.34962(4) 0.01713(19) Uani 1 1 d . . . N52 N 0.2906(5) 0.0322(4) 0.5918(5) 0.072(3) Uani 1 1 d . . . N53A N 0.2695(11) -0.0141(8) 0.5515(12) 0.042(8) Uani 0.47(3) 1 d P A 1 N53B N 0.3096(15) -0.0253(8) 0.5970(14) 0.073(11) Uani 0.53(3) 1 d P A 2 H11 H 0.357(6) 0.693(6) 0.487(4) 0.109 Uiso 1 1 d D . . H21 H 0.571(6) 0.738(6) 0.5025(17) 0.109 Uiso 1 1 d D . . H31 H 0.476(7) 0.614(5) 0.538(2) 0.109 Uiso 1 1 d D . . H41 H 0.428(7) 0.809(5) 0.538(3) 0.109 Uiso 1 1 d D . . H51 H 0.3455 0.1374 0.4451 0.109 Uiso 1 1 d . . . H61 H 0.2663 0.3127 0.4469 0.109 Uiso 1 1 d . . . H81 H 0.421(7) 0.273(6) 0.4821(19) 0.109 Uiso 1 1 d D . . H10A H 0.6628 0.6990 0.7524 0.087 Uiso 1 1 d . . . H10B H 0.6838 0.6478 0.7992 0.087 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.022(4) 0.021(4) 0.040(5) -0.003(3) 0.004(4) -0.003(3) C12 0.028(4) 0.025(4) 0.034(5) -0.006(3) -0.004(4) -0.003(3) C13 0.029(4) 0.020(4) 0.029(4) 0.004(3) 0.009(4) 0.003(3) C14 0.023(4) 0.021(4) 0.030(4) 0.003(3) 0.009(3) 0.005(3) C15 0.038(5) 0.019(4) 0.025(4) 0.001(3) 0.012(4) 0.000(3) C16 0.045(5) 0.022(4) 0.050(6) 0.005(4) 0.024(5) -0.010(4) C21 0.023(4) 0.031(4) 0.048(6) -0.003(4) -0.006(4) -0.009(3) C22 0.023(4) 0.027(4) 0.042(5) 0.001(3) 0.010(4) -0.009(3) C23 0.030(4) 0.010(3) 0.029(4) -0.001(3) -0.002(3) 0.001(3) C24 0.032(4) 0.020(4) 0.019(4) -0.009(3) 0.003(3) -0.001(3) C25 0.051(6) 0.028(5) 0.044(6) -0.008(4) -0.031(5) 0.006(4) C26 0.080(8) 0.064(7) 0.038(6) -0.017(5) -0.024(6) 0.003(6) C31 0.024(4) 0.022(4) 0.024(4) 0.003(3) 0.006(3) 0.001(3) C32 0.032(4) 0.024(4) 0.016(4) -0.003(3) -0.002(3) 0.003(3) C33 0.013(3) 0.028(4) 0.031(4) 0.000(3) 0.004(3) -0.006(3) C34 0.021(4) 0.020(4) 0.028(4) -0.003(3) 0.000(3) -0.004(3) C35 0.031(4) 0.029(4) 0.019(4) 0.002(3) 0.007(3) 0.008(3) C36 0.048(5) 0.036(5) 0.026(5) 0.000(3) 0.013(4) 0.015(4) C41 0.040(5) 0.020(4) 0.037(5) -0.003(3) -0.015(4) 0.010(3) C42 0.029(4) 0.040(5) 0.023(4) -0.009(3) 0.001(3) 0.014(4) C43 0.020(4) 0.017(4) 0.030(4) 0.003(3) -0.003(3) -0.006(3) C44 0.026(4) 0.024(4) 0.024(4) -0.002(3) -0.003(3) 0.000(3) C45 0.036(5) 0.030(4) 0.030(5) 0.014(3) -0.012(4) -0.007(4) C46 0.053(6) 0.044(5) 0.025(4) 0.019(4) -0.004(4) 0.002(4) C51 0.030(4) 0.013(4) 0.028(4) -0.003(3) -0.004(3) 0.005(3) C52 0.024(4) 0.021(4) 0.033(5) -0.002(3) -0.001(4) 0.008(3) C53 0.007(3) 0.020(4) 0.033(4) 0.000(3) -0.005(3) 0.002(3) C54 0.021(4) 0.020(4) 0.020(4) -0.001(3) -0.005(3) -0.003(3) C55 0.032(4) 0.029(4) 0.023(4) 0.009(3) -0.009(4) 0.001(3) C56 0.041(5) 0.031(5) 0.047(6) -0.006(4) -0.022(4) 0.000(4) C61 0.026(4) 0.040(5) 0.042(5) -0.002(4) 0.013(4) 0.008(4) C62 0.030(5) 0.058(6) 0.039(5) 0.015(4) 0.007(4) 0.018(4) C63 0.017(4) 0.028(4) 0.028(4) -0.014(3) 0.011(3) -0.008(3) C64 0.025(4) 0.026(4) 0.017(4) -0.005(3) 0.004(3) -0.010(3) C65 0.037(5) 0.028(4) 0.033(5) -0.020(3) 0.018(4) -0.010(4) C66 0.063(7) 0.048(6) 0.071(8) -0.019(5) 0.030(6) -0.011(5) C71 0.026(4) 0.013(4) 0.036(5) 0.001(3) 0.001(4) -0.007(3) C72 0.027(4) 0.020(4) 0.023(4) 0.002(3) 0.004(3) -0.005(3) C73 0.021(4) 0.013(3) 0.020(4) 0.000(3) 0.002(3) 0.001(3) C74 0.017(4) 0.012(4) 0.035(5) -0.001(3) 0.001(3) -0.002(3) C75 0.036(4) 0.020(4) 0.018(4) -0.005(3) -0.008(3) 0.001(3) C76 0.044(5) 0.045(5) 0.030(5) 0.000(4) -0.019(4) -0.015(4) C81 0.028(4) 0.032(4) 0.018(4) -0.006(3) -0.005(3) -0.008(3) C82 0.027(4) 0.030(4) 0.027(4) 0.000(3) -0.003(3) -0.011(3) C83 0.032(4) 0.017(4) 0.015(4) -0.005(3) 0.008(3) 0.000(3) C84 0.019(4) 0.022(4) 0.030(4) 0.003(3) 0.003(3) 0.003(3) C85 0.032(4) 0.026(4) 0.011(4) -0.007(3) 0.001(3) -0.001(3) C86 0.025(4) 0.022(4) 0.028(4) -0.001(3) 0.007(3) -0.003(3) N1 0.018(3) 0.021(3) 0.024(4) 0.001(2) 0.010(3) 0.005(2) N2 0.027(3) 0.021(3) 0.025(4) 0.000(3) -0.006(3) 0.003(2) N3 0.020(3) 0.023(3) 0.023(4) -0.004(3) 0.008(3) -0.006(3) N4 0.031(4) 0.018(3) 0.022(3) 0.001(2) -0.007(3) -0.002(3) N5 0.020(3) 0.025(3) 0.022(3) -0.003(2) -0.007(3) 0.000(2) N6 0.020(3) 0.025(3) 0.029(4) -0.003(3) 0.008(3) -0.002(3) N7 0.018(3) 0.016(3) 0.017(3) 0.000(2) 0.002(3) 0.002(2) N8 0.024(3) 0.014(3) 0.017(3) 0.005(2) -0.003(3) 0.001(2) N11 0.023(3) 0.029(3) 0.032(4) -0.004(3) 0.000(3) 0.007(3) N12 0.012(3) 0.016(3) 0.016(3) -0.001(2) 0.001(3) 0.002(2) N13 0.022(3) 0.029(4) 0.029(4) -0.005(3) 0.002(3) 0.001(3) N21 0.025(3) 0.036(4) 0.023(4) -0.003(3) -0.011(3) 0.009(3) N22 0.020(3) 0.022(4) 0.034(4) 0.007(3) -0.014(3) -0.002(3) N23 0.033(4) 0.019(4) 0.050(5) 0.001(3) -0.008(4) 0.004(3) N31 0.022(4) 0.024(4) 0.043(4) -0.011(3) -0.007(3) -0.003(3) N32 0.041(5) 0.018(3) 0.048(5) -0.015(3) -0.015(4) 0.003(3) N33 0.035(5) 0.029(4) 0.134(9) -0.032(5) -0.025(5) 0.010(4) N41 0.039(4) 0.026(4) 0.025(4) -0.001(3) 0.004(3) -0.007(3) N42 0.030(4) 0.020(4) 0.039(4) 0.007(3) 0.004(3) 0.001(3) N43 0.081(7) 0.040(5) 0.087(7) -0.023(5) 0.012(6) -0.025(5) N51 0.042(4) 0.025(4) 0.033(4) 0.007(3) 0.005(3) -0.015(3) N61 0.031(4) 0.028(4) 0.032(4) -0.014(3) 0.004(3) -0.004(3) N62 0.030(4) 0.016(3) 0.038(4) -0.001(3) 0.005(3) 0.002(3) N63 0.022(4) 0.028(4) 0.069(6) -0.003(3) 0.011(4) -0.003(3) N71 0.013(3) 0.033(3) 0.023(3) 0.010(3) 0.003(3) 0.003(3) N72 0.020(3) 0.016(3) 0.022(4) -0.002(2) -0.002(3) 0.003(2) N73 0.041(4) 0.035(4) 0.026(4) -0.001(3) -0.002(3) 0.015(3) N81 0.020(3) 0.039(4) 0.019(3) 0.003(3) 0.009(3) 0.008(3) N82 0.016(3) 0.015(3) 0.034(4) -0.006(3) 0.003(3) -0.006(3) N83 0.041(4) 0.032(4) 0.028(4) -0.004(3) 0.010(3) -0.004(3) O10 0.056(4) 0.063(4) 0.043(4) 0.004(3) -0.019(3) -0.005(3) O11 0.027(3) 0.026(3) 0.020(3) -0.001(2) 0.006(2) 0.000(2) O12 0.017(2) 0.018(2) 0.016(3) 0.0080(18) 0.002(2) 0.000(2) O21 0.021(3) 0.030(3) 0.023(3) -0.004(2) 0.004(2) -0.006(2) O22 0.018(2) 0.016(2) 0.015(2) -0.0029(18) 0.001(2) 0.0028(18) O31 0.020(3) 0.026(3) 0.022(3) -0.001(2) 0.003(2) 0.003(2) O32 0.017(2) 0.022(2) 0.018(2) 0.0000(19) 0.005(2) -0.0008(19) O41 0.028(3) 0.028(3) 0.015(3) 0.002(2) -0.003(2) 0.006(2) O42 0.018(2) 0.020(3) 0.022(3) -0.003(2) 0.003(2) 0.001(2) O51 0.018(3) 0.025(3) 0.022(3) -0.004(2) -0.006(2) 0.005(2) O52 0.013(2) 0.021(3) 0.016(2) -0.0012(19) 0.0014(19) -0.001(2) O61 0.025(3) 0.034(3) 0.021(3) 0.001(2) 0.001(2) 0.006(2) O62 0.014(2) 0.024(3) 0.019(2) 0.004(2) -0.0016(19) -0.004(2) O71 0.027(3) 0.023(3) 0.017(3) -0.0022(19) 0.002(2) -0.003(2) O72 0.018(2) 0.017(2) 0.016(3) -0.0011(19) 0.000(2) -0.0006(19) O81 0.024(3) 0.033(3) 0.019(3) -0.001(2) -0.005(2) -0.007(2) O82 0.015(2) 0.016(2) 0.019(2) 0.001(2) -0.0005(19) 0.0008(19) Cu1 0.0153(4) 0.0156(4) 0.0214(4) 0.0014(3) 0.0042(3) 0.0029(3) Cu2 0.0171(4) 0.0191(4) 0.0200(5) -0.0001(3) -0.0031(4) 0.0031(3) Cu3 0.0176(4) 0.0164(4) 0.0211(4) -0.0036(3) 0.0022(4) 0.0000(3) Cu4 0.0210(4) 0.0169(4) 0.0191(4) 0.0007(3) 0.0002(3) -0.0020(4) Cu5 0.0179(4) 0.0168(4) 0.0195(4) 0.0002(3) -0.0016(4) -0.0026(3) Cu6 0.0154(4) 0.0195(4) 0.0181(4) -0.0026(3) 0.0011(3) -0.0019(3) Cu7 0.0143(4) 0.0159(4) 0.0189(4) 0.0003(3) -0.0003(3) 0.0004(3) Cu8 0.0152(4) 0.0179(4) 0.0183(4) 0.0005(3) 0.0024(4) -0.0006(3) N52 0.059(6) 0.024(5) 0.133(10) -0.009(5) 0.068(6) -0.005(4) N53A 0.049(12) 0.019(9) 0.059(16) -0.019(8) 0.019(11) 0.003(7) N53B 0.096(19) 0.032(10) 0.09(2) -0.006(9) 0.053(17) 0.007(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 C11 C12 1.483(11) . ? C11 N1 1.495(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O11 1.446(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N1 1.508(9) . ? C13 C14 1.516(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O12 1.433(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N1 1.480(9) . ? C15 C16 1.531(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 N2 1.475(10) . ? C21 C22 1.500(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O21 1.427(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N2 1.495(9) . ? C23 C24 1.510(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O22 1.431(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.498(12) . ? C25 N2 1.518(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 N3 1.488(9) . ? C31 C32 1.509(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O31 1.431(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.521(9) . ? C33 N3 1.494(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O32 1.417(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N3 1.487(9) . ? C35 C36 1.521(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C41 N4 1.479(9) . ? C41 C42 1.504(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O41 1.421(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 N4 1.498(8) . ? C43 C44 1.509(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O42 1.429(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.470(11) . ? C45 N4 1.486(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C51 N5 1.493(9) . ? C51 C52 1.497(10) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O51 1.437(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 N5 1.499(8) . ? C53 C54 1.502(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O52 1.426(8) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 N5 1.506(9) . ? C55 C56 1.531(10) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C61 N6 1.479(10) . ? C61 C62 1.507(12) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O61 1.437(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.491(10) . ? C63 N6 1.487(8) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 O62 1.409(8) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.474(11) . ? C65 N6 1.512(9) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 C72 1.485(10) . ? C71 N7 1.486(9) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 O71 1.433(8) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 N7 1.471(8) . ? C73 C74 1.521(9) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 O72 1.415(8) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 N7 1.502(9) . ? C75 C76 1.527(10) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C81 N8 1.478(9) . ? C81 C82 1.522(10) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 O81 1.419(9) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.506(9) . ? C83 N8 1.489(9) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 O82 1.428(8) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 N8 1.494(9) . ? C85 C86 1.550(10) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? N1 Cu1 2.048(6) . ? N2 Cu2 2.060(6) . ? N3 Cu3 2.064(6) . ? N4 Cu4 2.089(6) . ? N5 Cu5 2.067(6) . ? N6 Cu6 2.059(6) . ? N7 Cu7 2.062(5) . ? N8 Cu8 2.063(5) . ? N11 N12 1.190(8) . ? N11 Cu1 1.967(6) . ? N12 N13 1.151(8) . ? N21 N22 1.217(9) . ? N21 Cu2 1.970(6) . ? N22 N23 1.148(9) . ? N31 N32 1.161(9) . ? N31 Cu3 1.961(6) . ? N32 N33 1.179(10) . ? N41 N42 1.184(9) . ? N41 Cu4 1.954(6) . ? N42 N43 1.149(10) . ? N51 N52 1.132(9) . ? N51 Cu5 1.965(6) . ? N61 N62 1.202(9) . ? N61 Cu6 1.936(6) . ? N62 N63 1.160(9) . ? N71 N72 1.180(8) . ? N71 Cu7 1.966(6) . ? N72 N73 1.146(8) . ? N81 N82 1.189(8) . ? N81 Cu8 1.941(6) . ? N82 N83 1.157(8) . ? O10 H10A 0.987 . ? O10 H10B 0.857 . ? O11 Cu1 2.336(5) . ? O11 H11 0.94(2) . ? O12 Cu2 1.952(4) . ? O12 Cu1 1.970(4) . ? O21 Cu2 2.281(5) . ? O21 H21 0.94(2) . ? O22 Cu2 1.958(4) . ? O22 Cu1 1.951(4) . ? O31 Cu3 2.302(5) . ? O31 H31 0.94(2) . ? O32 Cu4 1.965(4) . ? O32 Cu3 1.963(4) . ? O41 Cu4 2.254(5) . ? O41 H41 0.95(2) . ? O42 Cu4 1.968(5) . ? O42 Cu3 1.956(4) . ? O51 Cu5 2.274(5) . ? O51 H51 0.855 . ? O52 Cu5 1.962(4) . ? O52 Cu6 1.964(4) . ? O61 Cu6 2.253(5) . ? O61 H61 1.084 . ? O62 Cu5 1.963(4) . ? O62 Cu6 1.962(4) . ? O71 Cu7 2.306(5) . ? O71 H71 0.9500 . ? O72 Cu8 1.960(4) . ? O72 Cu7 1.989(4) . ? O81 Cu8 2.297(5) . ? O81 H81 0.94(2) . ? O82 Cu7 1.961(4) . ? O82 Cu8 1.976(4) . ? Cu1 Cu2 2.8864(12) . ? Cu3 Cu4 2.8968(11) . ? Cu5 Cu6 2.8947(12) . ? Cu7 Cu8 2.8830(11) . ? N52 N53A 1.33(2) . ? N52 N53B 1.203(19) . ? 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 C12 C11 N1 113.7(6) . . ? C12 C11 H11A 108.8 . . ? N1 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? N1 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? O11 C12 C11 108.0(6) . . ? O11 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O11 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? N1 C13 C14 108.5(5) . . ? N1 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? N1 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? O12 C14 C13 107.5(6) . . ? O12 C14 H14A 110.2 . . ? C13 C14 H14A 110.2 . . ? O12 C14 H14B 110.2 . . ? C13 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? N1 C15 C16 115.4(6) . . ? N1 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? N1 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C21 C22 113.9(6) . . ? N2 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N2 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? O21 C22 C21 109.4(6) . . ? O21 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? O21 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? N2 C23 C24 108.9(5) . . ? N2 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? N2 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O22 C24 C23 106.8(6) . . ? O22 C24 H24A 110.4 . . ? C23 C24 H24A 110.4 . . ? O22 C24 H24B 110.4 . . ? C23 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C26 C25 N2 114.1(7) . . ? C26 C25 H25A 108.7 . . ? N2 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? N2 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C31 C32 112.5(6) . . ? N3 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? N3 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? O31 C32 C31 109.4(6) . . ? O31 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? O31 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? C34 C33 N3 110.1(6) . . ? C34 C33 H33A 109.6 . . ? N3 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? N3 C33 H33B 109.6 . . ? H33A C33 H33B 108.2 . . ? O32 C34 C33 107.6(5) . . ? O32 C34 H34A 110.2 . . ? C33 C34 H34A 110.2 . . ? O32 C34 H34B 110.2 . . ? C33 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? N3 C35 C36 115.6(6) . . ? N3 C35 H35A 108.4 . . ? C36 C35 H35A 108.4 . . ? N3 C35 H35B 108.4 . . ? C36 C35 H35B 108.4 . . ? H35A C35 H35B 107.4 . . ? 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 . . ? N4 C41 C42 113.3(6) . . ? N4 C41 H41A 108.9 . . ? C42 C41 H41A 108.9 . . ? N4 C41 H41B 108.9 . . ? C42 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? O41 C42 C41 107.9(6) . . ? O41 C42 H42A 110.1 . . ? C41 C42 H42A 110.1 . . ? O41 C42 H42B 110.1 . . ? C41 C42 H42B 110.1 . . ? H42A C42 H42B 108.4 . . ? N4 C43 C44 111.0(6) . . ? N4 C43 H43A 109.4 . . ? C44 C43 H43A 109.4 . . ? N4 C43 H43B 109.4 . . ? C44 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? O42 C44 C43 107.6(6) . . ? O42 C44 H44A 110.2 . . ? C43 C44 H44A 110.2 . . ? O42 C44 H44B 110.2 . . ? C43 C44 H44B 110.2 . . ? H44A C44 H44B 108.5 . . ? C46 C45 N4 115.0(6) . . ? C46 C45 H45A 108.5 . . ? N4 C45 H45A 108.5 . . ? C46 C45 H45B 108.5 . . ? N4 C45 H45B 108.5 . . ? H45A C45 H45B 107.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N5 C51 C52 113.1(6) . . ? N5 C51 H51A 109.0 . . ? C52 C51 H51A 109.0 . . ? N5 C51 H51B 109.0 . . ? C52 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? O51 C52 C51 108.9(6) . . ? O51 C52 H52A 109.9 . . ? C51 C52 H52A 109.9 . . ? O51 C52 H52B 109.9 . . ? C51 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? N5 C53 C54 109.7(5) . . ? N5 C53 H53A 109.7 . . ? C54 C53 H53A 109.7 . . ? N5 C53 H53B 109.7 . . ? C54 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? O52 C54 C53 107.2(5) . . ? O52 C54 H54A 110.3 . . ? C53 C54 H54A 110.3 . . ? O52 C54 H54B 110.3 . . ? C53 C54 H54B 110.3 . . ? H54A C54 H54B 108.5 . . ? N5 C55 C56 116.0(7) . . ? N5 C55 H55A 108.3 . . ? C56 C55 H55A 108.3 . . ? N5 C55 H55B 108.3 . . ? C56 C55 H55B 108.3 . . ? H55A C55 H55B 107.4 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N6 C61 C62 112.9(7) . . ? N6 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? N6 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? O61 C62 C61 109.2(7) . . ? O61 C62 H62A 109.8 . . ? C61 C62 H62A 109.8 . . ? O61 C62 H62B 109.8 . . ? C61 C62 H62B 109.8 . . ? H62A C62 H62B 108.3 . . ? C64 C63 N6 109.5(6) . . ? C64 C63 H63A 109.8 . . ? N6 C63 H63A 109.8 . . ? C64 C63 H63B 109.8 . . ? N6 C63 H63B 109.8 . . ? H63A C63 H63B 108.2 . . ? O62 C64 C63 108.9(6) . . ? O62 C64 H64A 109.9 . . ? C63 C64 H64A 109.9 . . ? O62 C64 H64B 109.9 . . ? C63 C64 H64B 109.9 . . ? H64A C64 H64B 108.3 . . ? C66 C65 N6 115.8(8) . . ? C66 C65 H65A 108.3 . . ? N6 C65 H65A 108.3 . . ? C66 C65 H65B 108.3 . . ? N6 C65 H65B 108.3 . . ? H65A C65 H65B 107.4 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C71 N7 113.5(6) . . ? C72 C71 H71A 108.9 . . ? N7 C71 H71A 108.9 . . ? C72 C71 H71B 108.9 . . ? N7 C71 H71B 108.9 . . ? H71A C71 H71B 107.7 . . ? O71 C72 C71 109.3(6) . . ? O71 C72 H72A 109.8 . . ? C71 C72 H72A 109.8 . . ? O71 C72 H72B 109.8 . . ? C71 C72 H72B 109.8 . . ? H72A C72 H72B 108.3 . . ? N7 C73 C74 109.4(5) . . ? N7 C73 H73A 109.8 . . ? C74 C73 H73A 109.8 . . ? N7 C73 H73B 109.8 . . ? C74 C73 H73B 109.8 . . ? H73A C73 H73B 108.2 . . ? O72 C74 C73 107.0(6) . . ? O72 C74 H74A 110.3 . . ? C73 C74 H74A 110.3 . . ? O72 C74 H74B 110.3 . . ? C73 C74 H74B 110.3 . . ? H74A C74 H74B 108.6 . . ? N7 C75 C76 116.4(6) . . ? N7 C75 H75A 108.2 . . ? C76 C75 H75A 108.2 . . ? N7 C75 H75B 108.2 . . ? C76 C75 H75B 108.2 . . ? H75A C75 H75B 107.3 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N8 C81 C82 112.9(6) . . ? N8 C81 H81A 109.0 . . ? C82 C81 H81A 109.0 . . ? N8 C81 H81B 109.0 . . ? C82 C81 H81B 109.0 . . ? H81A C81 H81B 107.8 . . ? O81 C82 C81 109.2(6) . . ? O81 C82 H82A 109.8 . . ? C81 C82 H82A 109.8 . . ? O81 C82 H82B 109.8 . . ? C81 C82 H82B 109.8 . . ? H82A C82 H82B 108.3 . . ? C84 C83 N8 110.2(5) . . ? C84 C83 H83A 109.6 . . ? N8 C83 H83A 109.6 . . ? C84 C83 H83B 109.6 . . ? N8 C83 H83B 109.6 . . ? H83A C83 H83B 108.1 . . ? O82 C84 C83 106.8(5) . . ? O82 C84 H84A 110.4 . . ? C83 C84 H84A 110.4 . . ? O82 C84 H84B 110.4 . . ? C83 C84 H84B 110.4 . . ? H84A C84 H84B 108.6 . . ? N8 C85 C86 114.8(5) . . ? N8 C85 H85A 108.6 . . ? C86 C85 H85A 108.6 . . ? N8 C85 H85B 108.6 . . ? C86 C85 H85B 108.6 . . ? H85A C85 H85B 107.5 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C11 N1 C13 111.2(6) . . ? C11 N1 C15 111.8(6) . . ? C13 N1 C15 109.8(6) . . ? C11 N1 Cu1 106.9(4) . . ? C13 N1 Cu1 106.9(4) . . ? C15 N1 Cu1 110.1(4) . . ? C23 N2 C21 112.3(6) . . ? C23 N2 C25 109.4(6) . . ? C21 N2 C25 113.1(6) . . ? C23 N2 Cu2 106.3(4) . . ? C21 N2 Cu2 104.9(4) . . ? C25 N2 Cu2 110.4(5) . . ? C35 N3 C31 111.4(5) . . ? C35 N3 C33 111.8(6) . . ? C31 N3 C33 112.1(6) . . ? C35 N3 Cu3 108.9(4) . . ? C31 N3 Cu3 106.2(4) . . ? C33 N3 Cu3 106.1(4) . . ? C41 N4 C45 106.7(6) . . ? C41 N4 C43 110.7(6) . . ? C45 N4 C43 112.0(6) . . ? C41 N4 Cu4 105.4(4) . . ? C45 N4 Cu4 116.5(5) . . ? C43 N4 Cu4 105.4(4) . . ? C53 N5 C51 111.8(6) . . ? C53 N5 C55 110.6(5) . . ? C51 N5 C55 111.4(5) . . ? C53 N5 Cu5 105.1(4) . . ? C51 N5 Cu5 106.9(4) . . ? C55 N5 Cu5 110.8(4) . . ? C61 N6 C63 113.3(6) . . ? C61 N6 C65 111.9(6) . . ? C63 N6 C65 110.4(6) . . ? C61 N6 Cu6 105.0(4) . . ? C63 N6 Cu6 106.2(4) . . ? C65 N6 Cu6 109.6(5) . . ? C73 N7 C71 112.7(5) . . ? C73 N7 C75 111.8(5) . . ? C71 N7 C75 110.8(6) . . ? C73 N7 Cu7 107.0(4) . . ? C71 N7 Cu7 105.8(4) . . ? C75 N7 Cu7 108.5(4) . . ? C85 N8 C83 110.4(5) . . ? C85 N8 C81 111.2(5) . . ? C83 N8 C81 113.2(5) . . ? C85 N8 Cu8 110.6(4) . . ? C83 N8 Cu8 105.3(4) . . ? C81 N8 Cu8 105.9(4) . . ? N12 N11 Cu1 127.6(5) . . ? N13 N12 N11 175.7(7) . . ? N22 N21 Cu2 117.8(5) . . ? N23 N22 N21 176.2(7) . . ? N32 N31 Cu3 129.3(5) . . ? N33 N32 N31 176.6(9) . . ? N42 N41 Cu4 125.8(6) . . ? N43 N42 N41 176.0(9) . . ? N52 N51 Cu5 122.6(7) . . ? N62 N61 Cu6 123.6(5) . . ? N63 N62 N61 176.8(8) . . ? N72 N71 Cu7 127.5(5) . . ? N73 N72 N71 176.7(7) . . ? N82 N81 Cu8 130.7(5) . . ? N83 N82 N81 175.9(8) . . ? H10A O10 H10B 108.0 . . ? C12 O11 Cu1 106.0(4) . . ? C12 O11 H11 111(7) . . ? Cu1 O11 H11 119(8) . . ? C14 O12 Cu2 125.4(4) . . ? C14 O12 Cu1 106.4(4) . . ? Cu2 O12 Cu1 94.77(19) . . ? C22 O21 Cu2 106.4(4) . . ? C22 O21 H21 100(7) . . ? Cu2 O21 H21 135(7) . . ? C24 O22 Cu2 106.8(4) . . ? C24 O22 Cu1 125.3(4) . . ? Cu2 O22 Cu1 95.22(18) . . ? C32 O31 Cu3 108.0(4) . . ? C32 O31 H31 105(8) . . ? Cu3 O31 H31 134(7) . . ? C34 O32 Cu4 124.8(4) . . ? C34 O32 Cu3 108.3(4) . . ? Cu4 O32 Cu3 95.04(19) . . ? C42 O41 Cu4 107.5(4) . . ? C42 O41 H41 101(8) . . ? Cu4 O41 H41 132(7) . . ? C44 O42 Cu4 106.8(4) . . ? C44 O42 Cu3 123.5(4) . . ? Cu4 O42 Cu3 95.17(19) . . ? C52 O51 Cu5 108.4(4) . . ? C52 O51 H51 109.5 . . ? Cu5 O51 H51 122.0 . . ? C54 O52 Cu5 106.8(4) . . ? C54 O52 Cu6 126.4(4) . . ? Cu5 O52 Cu6 95.01(18) . . ? C62 O61 Cu6 107.2(4) . . ? C62 O61 H61 105.3 . . ? Cu6 O61 H61 118.1 . . ? C64 O62 Cu5 126.6(4) . . ? C64 O62 Cu6 107.2(4) . . ? Cu5 O62 Cu6 95.05(18) . . ? C72 O71 Cu7 106.2(4) . . ? C72 O71 H71 126.9 . . ? Cu7 O71 H71 126.9 . . ? C74 O72 Cu8 124.2(4) . . ? C74 O72 Cu7 106.4(4) . . ? Cu8 O72 Cu7 93.76(18) . . ? C82 O81 Cu8 107.6(4) . . ? C82 O81 H81 96(7) . . ? Cu8 O81 H81 134(8) . . ? C84 O82 Cu7 124.8(4) . . ? C84 O82 Cu8 106.5(4) . . ? Cu7 O82 Cu8 94.14(18) . . ? O22 Cu1 N11 95.5(2) . . ? O22 Cu1 O12 80.29(18) . . ? N11 Cu1 O12 169.7(2) . . ? O22 Cu1 N1 165.4(2) . . ? N11 Cu1 N1 99.0(2) . . ? O12 Cu1 N1 85.2(2) . . ? O22 Cu1 O11 99.58(18) . . ? N11 Cu1 O11 93.2(2) . . ? O12 Cu1 O11 96.79(18) . . ? N1 Cu1 O11 80.7(2) . . ? O22 Cu1 Cu2 42.49(13) . . ? N11 Cu1 Cu2 129.80(18) . . ? O12 Cu1 Cu2 42.37(13) . . ? N1 Cu1 Cu2 124.29(16) . . ? O11 Cu1 Cu2 115.78(12) . . ? O12 Cu2 O22 80.57(18) . . ? O12 Cu2 N21 98.8(2) . . ? O22 Cu2 N21 168.6(2) . . ? O12 Cu2 N2 165.4(2) . . ? O22 Cu2 N2 84.9(2) . . ? N21 Cu2 N2 95.7(3) . . ? O12 Cu2 O21 97.69(18) . . ? O22 Cu2 O21 95.33(18) . . ? N21 Cu2 O21 96.0(2) . . ? N2 Cu2 O21 82.1(2) . . ? O12 Cu2 Cu1 42.86(13) . . ? O22 Cu2 Cu1 42.30(13) . . ? N21 Cu2 Cu1 132.0(2) . . ? N2 Cu2 Cu1 123.98(17) . . ? O21 Cu2 Cu1 113.67(13) . . ? O42 Cu3 O32 81.09(18) . . ? O42 Cu3 N31 99.4(2) . . ? O32 Cu3 N31 174.1(3) . . ? O42 Cu3 N3 166.1(2) . . ? O32 Cu3 N3 85.2(2) . . ? N31 Cu3 N3 94.1(2) . . ? O42 Cu3 O31 102.56(18) . . ? O32 Cu3 O31 92.67(19) . . ? N31 Cu3 O31 93.0(2) . . ? N3 Cu3 O31 80.4(2) . . ? O42 Cu3 Cu4 42.58(13) . . ? O32 Cu3 Cu4 42.50(13) . . ? N31 Cu3 Cu4 135.54(19) . . ? N3 Cu3 Cu4 123.70(16) . . ? O31 Cu3 Cu4 114.02(12) . . ? O42 Cu4 O32 80.75(18) . . ? O42 Cu4 N41 169.5(2) . . ? O32 Cu4 N41 96.8(2) . . ? O42 Cu4 N4 84.8(2) . . ? O32 Cu4 N4 165.6(2) . . ? N41 Cu4 N4 97.3(3) . . ? O42 Cu4 O41 93.30(19) . . ? O32 Cu4 O41 99.55(18) . . ? N41 Cu4 O41 97.2(2) . . ? N4 Cu4 O41 81.5(2) . . ? O42 Cu4 Cu3 42.25(13) . . ? O32 Cu4 Cu3 42.46(13) . . ? N41 Cu4 Cu3 131.2(2) . . ? N4 Cu4 Cu3 123.83(16) . . ? O41 Cu4 Cu3 112.45(13) . . ? O62 Cu5 O52 81.17(18) . . ? O62 Cu5 N5 166.6(2) . . ? O52 Cu5 N5 85.4(2) . . ? O62 Cu5 N51 94.1(2) . . ? O52 Cu5 N51 163.3(2) . . ? N5 Cu5 N51 98.5(3) . . ? O62 Cu5 O51 101.74(18) . . ? O52 Cu5 O51 97.22(18) . . ? N5 Cu5 O51 80.8(2) . . ? N51 Cu5 O51 99.4(2) . . ? O62 Cu5 Cu6 42.46(13) . . ? O52 Cu5 Cu6 42.51(13) . . ? N5 Cu5 Cu6 124.56(16) . . ? N51 Cu5 Cu6 126.3(2) . . ? O51 Cu5 Cu6 116.31(12) . . ? N61 Cu6 O62 169.2(2) . . ? N61 Cu6 O52 98.9(2) . . ? O62 Cu6 O52 81.17(18) . . ? N61 Cu6 N6 94.5(3) . . ? O62 Cu6 N6 84.9(2) . . ? O52 Cu6 N6 166.0(2) . . ? N61 Cu6 O61 94.7(2) . . ? O62 Cu6 O61 95.90(19) . . ? O52 Cu6 O61 100.91(18) . . ? N6 Cu6 O61 82.1(2) . . ? N61 Cu6 Cu5 133.0(2) . . ? O62 Cu6 Cu5 42.49(13) . . ? O52 Cu6 Cu5 42.48(13) . . ? N6 Cu6 Cu5 123.82(16) . . ? O61 Cu6 Cu5 114.88(13) . . ? O82 Cu7 N71 96.9(2) . . ? O82 Cu7 O72 80.68(17) . . ? N71 Cu7 O72 172.3(2) . . ? O82 Cu7 N7 164.8(2) . . ? N71 Cu7 N7 98.2(2) . . ? O72 Cu7 N7 84.19(19) . . ? O82 Cu7 O71 99.33(17) . . ? N71 Cu7 O71 91.1(2) . . ? O72 Cu7 O71 96.49(18) . . ? N7 Cu7 O71 81.17(19) . . ? O82 Cu7 Cu8 43.13(12) . . ? N71 Cu7 Cu8 131.87(17) . . ? O72 Cu7 Cu8 42.73(12) . . ? N7 Cu7 Cu8 123.16(16) . . ? O71 Cu7 Cu8 116.51(12) . . ? N81 Cu8 O72 95.7(2) . . ? N81 Cu8 O82 171.8(2) . . ? O72 Cu8 O82 81.02(18) . . ? N81 Cu8 N8 97.9(2) . . ? O72 Cu8 N8 166.3(2) . . ? O82 Cu8 N8 85.3(2) . . ? N81 Cu8 O81 92.5(2) . . ? O72 Cu8 O81 99.62(19) . . ? O82 Cu8 O81 95.54(18) . . ? N8 Cu8 O81 81.0(2) . . ? N81 Cu8 Cu7 130.99(19) . . ? O72 Cu8 Cu7 43.51(13) . . ? O82 Cu8 Cu7 42.72(13) . . ? N8 Cu8 Cu7 124.01(16) . . ? O81 Cu8 Cu7 116.16(13) . . ? N51 N52 N53A 155.0(16) . . ? N51 N52 N53B 146(2) . . ? N53A N52 N53B 58.5(12) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.984 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.100