Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Reedijk, Jan' 'Driessen, Willem L.' 'Gamez, Patrick' 'Hoog, Paul de' 'Lutz, Martin' 'Roubeau, Olivier' 'Spek, A.' _publ_contact_author_name 'Prof Jan Reedijk' _publ_contact_author_address ; LIC Leiden University P.O. Box 9502 Leiden 2300RA NETHERLANDS ; _publ_contact_author_email 'REEDIJK@CHEM.LEIDENUNIV.NL' _publ_contact_author_fax '[+31] 30 2533940' _publ_contact_author_phone '[+31] 30 2533902' _publ_requested_journal 'Chemical Communications' _publ_section_title ; An unprecedented 1D ladder coordination polymer based on a pentanuclear copper(II) 2,4,6-(di-pyridin-2-yl-amino)-[1,3,5]triazine building block ; data_s2564a _database_code_CSD 183664 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H54 Cu5 N36 O30, 7(C2 H3 N)' _chemical_formula_sum 'C84 H75 Cu5 N43 O30' _chemical_formula_weight 2484.57 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.052(2) _cell_length_b 14.0863(18) _cell_length_c 16.425(4) _cell_angle_alpha 79.047(11) _cell_angle_beta 73.946(15) _cell_angle_gamma 82.334(11) _cell_volume 2621.3(9) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1265 _exptl_absorpt_coefficient_mu 1.096 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ? _exptl_special_details ; The crystal appeared to be a non-merohedral twin with a twofold rotation around hkl=(101) as twin operation. Indexing and determination of the twin law was performed with the program DIRAX (Duisenberg, 1992) based on accurately measured reflection positions from the PhiChi routine (Duisenberg, Hooft, Schreurs & Kroon, 2000). The intenties were obtained using the EVAL program (Duisenberg, 1998).Equivalent reflections were merged after the absorption correction using a locally written program. The reflections belonging to the two twin domains were kept separate in a HKLF5 file. The structure was solved with direct methods (SIR-97, Altomare et al., 1997), based on the non-overlapping reflections of the major domain. The refinement was performed with SHELXL-97 (Sheldrick, 1997) with twinned data. The refined twin ratio was 0.2520(7):0.7480(7). ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56928 _diffrn_reflns_av_R_equivalents 0.08 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.00 _reflns_number_total 12741 _reflns_number_gt 8894 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'DIRAX (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998)' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+8.7612P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12741 _refine_ls_number_parameters 687 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.028 _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 Cu3 Cu 0.13012(6) 0.82961(5) 0.23945(4) 0.02226(18) Uani 1 1 d . . . Cu1 Cu 0.5000 0.5000 0.5000 0.0263(3) Uani 1 2 d S . . Cu2 Cu 0.21245(6) 0.22483(5) 0.17257(4) 0.02261(18) Uani 1 1 d . . . N1 N 0.4952(4) 0.4895(3) 0.3188(3) 0.0216(11) Uani 1 1 d . . . N2 N 0.1765(4) 0.3736(3) 0.2816(3) 0.0188(10) Uani 1 1 d . . . N3 N 0.2747(4) 0.6786(3) 0.1488(3) 0.0214(11) Uani 1 1 d . . . N11 N 0.3384(4) 0.4289(3) 0.3000(3) 0.0214(10) Uani 1 1 d . . . C12 C 0.2511(5) 0.4455(4) 0.2641(3) 0.0189(12) Uani 1 1 d . . . N13 N 0.2260(4) 0.5255(3) 0.2124(3) 0.0198(10) Uani 1 1 d . . . C14 C 0.2979(5) 0.5935(4) 0.2007(3) 0.0188(12) Uani 1 1 d . . . N15 N 0.3871(4) 0.5877(3) 0.2335(3) 0.0193(10) Uani 1 1 d . . . C16 C 0.4035(4) 0.5034(4) 0.2811(3) 0.0202(13) Uani 1 1 d . . . N21 N 0.5721(4) 0.5842(3) 0.3891(3) 0.0254(11) Uani 1 1 d . . . C22 C 0.5609(5) 0.5688(4) 0.3135(4) 0.0241(13) Uani 1 1 d . . . C23 C 0.6106(5) 0.6210(4) 0.2361(4) 0.0296(14) Uani 1 1 d . . . H23 H 0.6018 0.6064 0.1842 0.036 Uiso 1 1 calc R . . C24 C 0.6744(5) 0.6961(4) 0.2355(4) 0.0375(16) Uani 1 1 d . . . H24 H 0.7077 0.7357 0.1830 0.045 Uiso 1 1 calc R . . C25 C 0.6890(5) 0.7128(4) 0.3119(4) 0.0344(15) Uani 1 1 d . . . H25 H 0.7329 0.7636 0.3127 0.041 Uiso 1 1 calc R . . C26 C 0.6391(5) 0.6549(4) 0.3860(4) 0.0314(15) Uani 1 1 d . . . H26 H 0.6522 0.6648 0.4381 0.038 Uiso 1 1 calc R . . N31 N 0.5461(4) 0.3878(3) 0.4354(3) 0.0251(11) Uani 1 1 d . . . C32 C 0.5320(5) 0.3961(4) 0.3568(4) 0.0237(13) Uani 1 1 d . . . C33 C 0.5583(5) 0.3200(4) 0.3096(4) 0.0352(15) Uani 1 1 d . . . H33 H 0.5478 0.3288 0.2534 0.042 Uiso 1 1 calc R . . C34 C 0.5995(6) 0.2324(4) 0.3469(4) 0.0421(17) Uani 1 1 d . . . H34 H 0.6163 0.1784 0.3172 0.051 Uiso 1 1 calc R . . C35 C 0.6166(6) 0.2227(4) 0.4280(4) 0.0394(17) Uani 1 1 d . . . H35 H 0.6454 0.1621 0.4546 0.047 Uiso 1 1 calc R . . C36 C 0.5920(5) 0.3005(4) 0.4689(4) 0.0329(15) Uani 1 1 d . . . H36 H 0.6074 0.2940 0.5234 0.040 Uiso 1 1 calc R . . N41 N 0.2168(4) 0.2051(3) 0.2947(3) 0.0198(10) Uani 1 1 d . . . C42 C 0.2011(5) 0.2832(4) 0.3328(3) 0.0204(12) Uani 1 1 d . . . C43 C 0.2042(5) 0.2779(4) 0.4162(3) 0.0282(14) Uani 1 1 d . . . H43 H 0.1908 0.3347 0.4420 0.034 Uiso 1 1 calc R . . C44 C 0.2273(5) 0.1883(4) 0.4618(4) 0.0339(15) Uani 1 1 d . . . H44 H 0.2315 0.1825 0.5195 0.041 Uiso 1 1 calc R . . C45 C 0.2444(6) 0.1066(4) 0.4227(4) 0.0348(15) Uani 1 1 d . . . H45 H 0.2615 0.0441 0.4527 0.042 Uiso 1 1 calc R . . C46 C 0.2360(5) 0.1183(4) 0.3402(4) 0.0268(14) Uani 1 1 d . . . H46 H 0.2441 0.0622 0.3140 0.032 Uiso 1 1 calc R . . N51 N 0.0733(4) 0.3173(3) 0.2026(3) 0.0223(11) Uani 1 1 d . . . C52 C 0.0792(4) 0.3859(4) 0.2473(3) 0.0196(12) Uani 1 1 d . . . C53 C -0.0037(5) 0.4602(4) 0.2607(4) 0.0304(14) Uani 1 1 d . . . H53 H 0.0033 0.5081 0.2921 0.037 Uiso 1 1 calc R . . C54 C -0.0977(5) 0.4653(5) 0.2285(4) 0.0425(17) Uani 1 1 d . . . H54 H -0.1557 0.5179 0.2360 0.051 Uiso 1 1 calc R . . C55 C -0.1078(6) 0.3935(5) 0.1849(4) 0.0437(17) Uani 1 1 d . . . H55 H -0.1735 0.3949 0.1633 0.052 Uiso 1 1 calc R . . C56 C -0.0213(5) 0.3204(4) 0.1736(4) 0.0316(15) Uani 1 1 d . . . H56 H -0.0280 0.2703 0.1443 0.038 Uiso 1 1 calc R . . N61 N 0.0954(4) 0.7638(3) 0.1527(3) 0.0207(11) Uani 1 1 d . . . C62 C 0.1717(5) 0.6945(4) 0.1212(3) 0.0221(13) Uani 1 1 d . . . C63 C 0.1513(5) 0.6402(4) 0.0664(4) 0.0293(14) Uani 1 1 d . . . H63 H 0.2075 0.5913 0.0440 0.035 Uiso 1 1 calc R . . C64 C 0.0475(5) 0.6585(4) 0.0452(4) 0.0331(15) Uani 1 1 d . . . H64 H 0.0295 0.6198 0.0099 0.040 Uiso 1 1 calc R . . C65 C -0.0311(5) 0.7329(4) 0.0747(4) 0.0304(15) Uani 1 1 d . . . H65 H -0.1016 0.7483 0.0580 0.036 Uiso 1 1 calc R . . C66 C -0.0044(5) 0.7837(4) 0.1290(4) 0.0273(14) Uani 1 1 d . . . H66 H -0.0580 0.8346 0.1505 0.033 Uiso 1 1 calc R . . N71 N 0.2907(4) 0.8363(3) 0.1662(3) 0.0210(10) Uani 1 1 d . . . C72 C 0.3438(5) 0.7579(4) 0.1325(3) 0.0214(13) Uani 1 1 d . . . C73 C 0.4567(5) 0.7533(4) 0.0840(4) 0.0287(14) Uani 1 1 d . . . H73 H 0.4914 0.6963 0.0609 0.034 Uiso 1 1 calc R . . C74 C 0.5189(5) 0.8333(4) 0.0696(4) 0.0321(15) Uani 1 1 d . . . H74 H 0.5977 0.8319 0.0375 0.038 Uiso 1 1 calc R . . C75 C 0.4645(5) 0.9144(4) 0.1025(4) 0.0280(14) Uani 1 1 d . . . H75 H 0.5050 0.9706 0.0927 0.034 Uiso 1 1 calc R . . C76 C 0.3515(5) 0.9146(4) 0.1495(4) 0.0255(13) Uani 1 1 d . . . H76 H 0.3145 0.9719 0.1713 0.031 Uiso 1 1 calc R . . N80 N 0.3069(5) 0.5234(4) 0.4778(3) 0.0375(13) Uani 1 1 d . . . C81 C 0.2130(7) 0.5532(5) 0.4942(4) 0.0425(17) Uani 1 1 d . . . C82 C 0.0948(7) 0.5916(10) 0.5151(5) 0.125(5) Uani 1 1 d . . . H82A H 0.0486 0.5452 0.5595 0.188 Uiso 1 1 calc R . . H82B H 0.0656 0.6029 0.4637 0.188 Uiso 1 1 calc R . . H82C H 0.0890 0.6530 0.5364 0.188 Uiso 1 1 calc R . . N90 N 0.2391(5) 0.3554(4) 0.0204(4) 0.0475(15) Uani 1 1 d . . . O91 O 0.2183(4) 0.2626(3) 0.0495(2) 0.0367(10) Uani 1 1 d . . . O92 O 0.2617(5) 0.4022(3) 0.0694(3) 0.0569(14) Uani 1 1 d . . . O93 O 0.2338(6) 0.3924(4) -0.0517(3) 0.083(2) Uani 1 1 d . . . N94 N 0.4473(5) 0.1860(4) 0.1461(3) 0.0339(12) Uani 1 1 d . . . O95 O 0.3604(3) 0.1432(3) 0.1444(3) 0.0324(10) Uani 1 1 d . . . O96 O 0.4302(4) 0.2706(3) 0.1573(3) 0.0547(13) Uani 1 1 d . . . O97 O 0.5420(4) 0.1400(4) 0.1362(3) 0.0616(14) Uani 1 1 d . . . N98 N 0.0712(4) 0.0554(4) 0.1577(3) 0.0309(12) Uani 1 1 d . . . O99 O 0.1331(3) 0.0828(3) 0.1969(3) 0.0322(10) Uani 1 1 d . . . O910 O 0.0506(4) -0.0315(3) 0.1721(3) 0.0367(11) Uani 1 1 d . . . O911 O 0.0340(5) 0.1124(3) 0.1039(4) 0.082(2) Uani 1 1 d . . . N912 N -0.0206(5) 0.7078(4) 0.3479(3) 0.0297(12) Uani 1 1 d . . . O913 O 0.0695(4) 0.6570(3) 0.3246(3) 0.0397(11) Uani 1 1 d . . . O914 O -0.0238(3) 0.8000(3) 0.3191(2) 0.0314(10) Uani 1 1 d . . . O915 O -0.1090(4) 0.6747(3) 0.3970(3) 0.0403(11) Uani 1 1 d . . . N916 N 0.2338(4) 0.8391(4) 0.3679(3) 0.0332(12) Uani 1 1 d . . . O917 O 0.1659(3) 0.8911(3) 0.3251(2) 0.0302(10) Uani 1 1 d . . . O918 O 0.2651(5) 0.7556(3) 0.3558(3) 0.0587(14) Uani 1 1 d . . . O919 O 0.2626(4) 0.8753(3) 0.4193(3) 0.0503(13) Uani 1 1 d . . . N1A N 0.7422(6) 0.9155(5) 0.1310(5) 0.082(2) Uiso 1 1 d D . . C2A C 0.7739(6) 0.9861(5) 0.0884(4) 0.0488(18) Uiso 1 1 d D . . C3A C 0.8118(6) 1.0739(5) 0.0387(4) 0.055(2) Uiso 1 1 d D . . H3A H 0.7468 1.1227 0.0409 0.050 Uiso 1 1 d . . . H3B H 0.8468 1.0636 -0.0202 0.050 Uiso 1 1 d . . . H3C H 0.8698 1.0949 0.0615 0.050 Uiso 1 1 d . . . N1B N 0.6492(7) 0.9742(6) 0.4000(5) 0.098(3) Uiso 1 1 d D . . C2B C 0.5898(7) 0.9623(6) 0.3602(5) 0.066(2) Uiso 1 1 d D . . C3B C 0.5191(7) 0.9507(6) 0.3085(5) 0.067(2) Uiso 1 1 d D . . H3D H 0.5209 1.0070 0.2635 0.050 Uiso 1 1 d . . . H3E H 0.4393 0.9453 0.3440 0.050 Uiso 1 1 d . . . H3F H 0.5464 0.8921 0.2834 0.050 Uiso 1 1 d . . . N1C N 0.9329(9) 0.2188(6) 0.3904(6) 0.124(3) Uiso 1 1 d D . . C2C C 0.9312(9) 0.1381(7) 0.3865(6) 0.086(3) Uiso 1 1 d D . . C3C C 0.9300(9) 0.0392(6) 0.3855(7) 0.097(3) Uiso 1 1 d D . . H3G H 0.9190 0.0035 0.4426 0.050 Uiso 1 1 d . . . H3H H 1.0040 0.0169 0.3485 0.050 Uiso 1 1 d . . . H3I H 0.8674 0.0309 0.3608 0.050 Uiso 1 1 d . . . N1D N 0.517(3) 0.511(3) -0.0218(16) 0.172(10) Uiso 0.50 1 d PD . . C2D C 0.5289(17) 0.4788(16) 0.0479(13) 0.093(6) Uiso 0.50 1 d PD . . C3D C 0.5963(15) 0.4475(13) 0.1076(10) 0.075(5) Uiso 0.50 1 d PD . . H3J H 0.6298 0.3795 0.0989 0.050 Uiso 0.50 1 d P . . H3K H 0.5476 0.4449 0.1644 0.050 Uiso 0.50 1 d P . . H3L H 0.6582 0.4876 0.0957 0.050 Uiso 0.50 1 d P . . 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 Cu3 0.0248(4) 0.0191(4) 0.0258(4) -0.0050(3) -0.0106(3) -0.0011(3) Cu1 0.0390(6) 0.0168(5) 0.0288(6) 0.0008(4) -0.0198(5) -0.0053(4) Cu2 0.0289(4) 0.0178(4) 0.0240(4) -0.0056(3) -0.0115(3) 0.0009(3) N1 0.026(3) 0.016(2) 0.026(3) 0.000(2) -0.015(2) -0.003(2) N2 0.027(3) 0.010(2) 0.021(2) 0.000(2) -0.011(2) 0.001(2) N3 0.032(3) 0.010(2) 0.026(3) 0.000(2) -0.015(2) -0.004(2) N11 0.028(3) 0.017(2) 0.024(3) -0.002(2) -0.015(2) -0.001(2) C12 0.029(3) 0.012(3) 0.016(3) -0.006(2) -0.004(3) -0.001(2) N13 0.025(3) 0.013(2) 0.024(3) -0.006(2) -0.011(2) 0.002(2) C14 0.025(3) 0.017(3) 0.015(3) -0.007(2) -0.003(2) 0.001(3) N15 0.024(3) 0.015(2) 0.023(2) 0.000(2) -0.013(2) -0.004(2) C16 0.019(3) 0.023(3) 0.021(3) -0.010(3) -0.006(2) 0.002(3) N21 0.031(3) 0.018(3) 0.034(3) 0.000(2) -0.021(2) -0.006(2) C22 0.018(3) 0.018(3) 0.037(4) 0.000(3) -0.013(3) 0.002(2) C23 0.025(3) 0.033(4) 0.030(3) 0.004(3) -0.012(3) -0.003(3) C24 0.031(4) 0.033(4) 0.044(4) 0.010(3) -0.012(3) -0.007(3) C25 0.029(4) 0.027(3) 0.049(4) 0.000(3) -0.015(3) -0.006(3) C26 0.039(4) 0.022(3) 0.040(4) 0.000(3) -0.022(3) -0.006(3) N31 0.031(3) 0.021(3) 0.027(3) 0.001(2) -0.016(2) -0.002(2) C32 0.022(3) 0.020(3) 0.031(3) 0.000(3) -0.014(3) -0.001(2) C33 0.039(4) 0.034(4) 0.040(4) -0.013(3) -0.021(3) 0.005(3) C34 0.057(5) 0.021(4) 0.060(5) -0.015(3) -0.036(4) 0.009(3) C35 0.052(4) 0.021(3) 0.051(4) -0.002(3) -0.030(4) 0.005(3) C36 0.043(4) 0.018(3) 0.045(4) 0.004(3) -0.027(3) -0.003(3) N41 0.023(3) 0.016(3) 0.022(2) -0.003(2) -0.008(2) -0.001(2) C42 0.021(3) 0.020(3) 0.020(3) -0.003(3) -0.005(2) -0.002(2) C43 0.041(4) 0.020(3) 0.025(3) -0.005(3) -0.010(3) 0.000(3) C44 0.047(4) 0.034(4) 0.022(3) 0.001(3) -0.014(3) -0.006(3) C45 0.056(4) 0.018(3) 0.031(4) 0.001(3) -0.018(3) 0.000(3) C46 0.041(4) 0.014(3) 0.030(3) -0.006(3) -0.016(3) 0.002(3) N51 0.026(3) 0.017(3) 0.025(3) -0.001(2) -0.010(2) -0.001(2) C52 0.022(3) 0.013(3) 0.023(3) 0.002(2) -0.008(2) -0.001(2) C53 0.031(4) 0.021(3) 0.040(4) -0.009(3) -0.010(3) 0.002(3) C54 0.027(4) 0.038(4) 0.063(5) -0.010(4) -0.016(3) 0.008(3) C55 0.032(4) 0.046(4) 0.060(5) -0.004(4) -0.026(3) -0.002(3) C56 0.033(4) 0.028(3) 0.040(4) -0.005(3) -0.021(3) -0.003(3) N61 0.029(3) 0.015(2) 0.023(3) 0.002(2) -0.014(2) -0.007(2) C62 0.035(4) 0.015(3) 0.021(3) 0.000(3) -0.015(3) -0.007(3) C63 0.039(4) 0.021(3) 0.031(3) -0.005(3) -0.017(3) 0.006(3) C64 0.049(4) 0.026(3) 0.032(4) -0.004(3) -0.024(3) -0.002(3) C65 0.033(4) 0.030(3) 0.035(4) 0.003(3) -0.022(3) -0.009(3) C66 0.029(4) 0.022(3) 0.034(3) -0.002(3) -0.014(3) -0.004(3) N71 0.026(3) 0.016(2) 0.025(3) 0.000(2) -0.014(2) -0.001(2) C72 0.030(4) 0.013(3) 0.022(3) 0.007(2) -0.015(3) -0.002(3) C73 0.037(4) 0.022(3) 0.027(3) -0.002(3) -0.011(3) 0.002(3) C74 0.031(4) 0.032(4) 0.029(3) 0.003(3) -0.003(3) -0.008(3) C75 0.036(4) 0.017(3) 0.033(3) 0.004(3) -0.013(3) -0.013(3) C76 0.031(4) 0.017(3) 0.030(3) 0.004(3) -0.014(3) -0.008(3) N80 0.040(4) 0.039(3) 0.037(3) -0.003(3) -0.017(3) -0.004(3) C81 0.046(5) 0.059(5) 0.023(3) -0.005(3) -0.015(3) 0.005(4) C82 0.050(6) 0.239(14) 0.050(5) 0.003(7) -0.006(4) 0.064(7) N90 0.045(4) 0.055(4) 0.045(4) -0.011(3) -0.015(3) -0.004(3) O91 0.050(3) 0.036(3) 0.028(2) -0.009(2) -0.014(2) -0.002(2) O92 0.081(4) 0.049(3) 0.047(3) -0.010(3) -0.019(3) -0.018(3) O93 0.131(5) 0.100(5) 0.021(3) 0.022(3) -0.030(3) -0.040(4) N94 0.037(4) 0.030(3) 0.034(3) -0.001(2) -0.013(3) 0.003(3) O95 0.027(2) 0.025(2) 0.048(3) -0.015(2) -0.010(2) -0.0014(19) O96 0.049(3) 0.037(3) 0.078(4) -0.019(3) -0.007(3) -0.012(2) O97 0.027(3) 0.062(3) 0.090(4) -0.009(3) -0.014(3) 0.009(3) N98 0.035(3) 0.025(3) 0.040(3) -0.007(3) -0.023(3) 0.002(2) O99 0.041(3) 0.022(2) 0.041(2) -0.0034(19) -0.024(2) -0.0054(19) O910 0.046(3) 0.013(2) 0.060(3) -0.001(2) -0.031(2) -0.0051(19) O911 0.137(5) 0.031(3) 0.117(5) 0.015(3) -0.108(5) -0.022(3) N912 0.038(3) 0.033(3) 0.022(3) -0.003(2) -0.012(3) -0.010(3) O913 0.040(3) 0.029(2) 0.039(3) -0.003(2) 0.001(2) 0.008(2) O914 0.033(2) 0.027(2) 0.034(2) -0.0050(19) -0.0077(19) -0.0018(19) O915 0.035(3) 0.054(3) 0.031(2) -0.001(2) -0.005(2) -0.014(2) N916 0.042(3) 0.030(3) 0.030(3) -0.001(3) -0.015(3) -0.002(3) O917 0.037(2) 0.026(2) 0.034(2) -0.0088(19) -0.020(2) 0.0051(19) O918 0.097(4) 0.028(3) 0.062(3) -0.008(2) -0.048(3) 0.015(3) O919 0.078(4) 0.043(3) 0.049(3) -0.004(2) -0.043(3) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu3 O917 1.952(4) . ? Cu3 N71 1.981(4) . ? Cu3 O914 1.996(4) . ? Cu3 N61 2.000(4) . ? Cu3 O910 2.288(4) 1_565 ? Cu1 N31 2.002(5) 2_666 ? Cu1 N31 2.002(5) . ? Cu1 N21 2.015(4) . ? Cu1 N21 2.015(4) 2_666 ? Cu1 N80 2.425(6) 2_666 ? Cu1 N80 2.425(6) . ? Cu2 O91 1.974(4) . ? Cu2 O95 1.978(4) . ? Cu2 N41 1.986(4) . ? Cu2 N51 1.989(4) . ? Cu2 O99 2.253(4) . ? N1 C16 1.385(6) . ? N1 C32 1.415(7) . ? N1 C22 1.430(7) . ? N2 C12 1.381(6) . ? N2 C52 1.413(7) . ? N2 C42 1.431(6) . ? N3 C14 1.376(6) . ? N3 C62 1.412(7) . ? N3 C72 1.423(7) . ? N11 C12 1.318(7) . ? N11 C16 1.331(7) . ? C12 N13 1.331(6) . ? N13 C14 1.329(6) . ? C14 N15 1.316(7) . ? N15 C16 1.316(7) . ? N21 C22 1.345(7) . ? N21 C26 1.348(7) . ? C22 C23 1.363(8) . ? C23 C24 1.384(8) . ? C23 H23 0.9500 . ? C24 C25 1.381(8) . ? C24 H24 0.9500 . ? C25 C26 1.363(8) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? N31 C32 1.329(7) . ? N31 C36 1.361(7) . ? C32 C33 1.393(8) . ? C33 C34 1.363(8) . ? C33 H33 0.9500 . ? C34 C35 1.383(9) . ? C34 H34 0.9500 . ? C35 C36 1.350(8) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? N41 C42 1.334(7) . ? N41 C46 1.334(7) . ? C42 C43 1.369(7) . ? C43 C44 1.376(8) . ? C43 H43 0.9500 . ? C44 C45 1.387(8) . ? C44 H44 0.9500 . ? C45 C46 1.365(8) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? N51 C52 1.339(7) . ? N51 C56 1.345(7) . ? C52 C53 1.353(7) . ? C53 C54 1.364(8) . ? C53 H53 0.9500 . ? C54 C55 1.382(9) . ? C54 H54 0.9500 . ? C55 C56 1.364(8) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? N61 C62 1.325(7) . ? N61 C66 1.343(7) . ? C62 C63 1.376(7) . ? C63 C64 1.369(8) . ? C63 H63 0.9500 . ? C64 C65 1.381(8) . ? C64 H64 0.9500 . ? C65 C66 1.369(8) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? N71 C72 1.335(7) . ? N71 C76 1.348(7) . ? C72 C73 1.373(8) . ? C73 C74 1.384(8) . ? C73 H73 0.9500 . ? C74 C75 1.366(8) . ? C74 H74 0.9500 . ? C75 C76 1.367(8) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? N80 C81 1.129(8) . ? C81 C82 1.426(11) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? N90 O93 1.214(7) . ? N90 O92 1.237(7) . ? N90 O91 1.336(7) . ? N94 O97 1.221(6) . ? N94 O96 1.222(6) . ? N94 O95 1.285(6) . ? N98 O911 1.216(6) . ? N98 O99 1.247(6) . ? N98 O910 1.247(6) . ? O910 Cu3 2.288(4) 1_545 ? N912 O913 1.227(6) . ? N912 O915 1.232(6) . ? N912 O914 1.294(6) . ? N916 O919 1.211(6) . ? N916 O918 1.223(6) . ? N916 O917 1.291(6) . ? N1A C2A 1.146(6) . ? C2A C3A 1.402(6) . ? C3A H3A 0.9682 . ? C3A H3B 0.9726 . ? C3A H3C 0.9786 . ? N1B C2B 1.139(6) . ? C2B C3B 1.403(7) . ? C3B H3D 0.9736 . ? C3B H3E 0.9826 . ? C3B H3F 0.9688 . ? N1C C2C 1.153(7) . ? C2C C3C 1.400(7) . ? C3C H3G 0.9595 . ? C3C H3H 0.9797 . ? C3C H3I 0.9785 . ? N1D C2D 1.186(9) . ? C2D C3D 1.413(9) . ? C3D H3J 1.0092 . ? C3D H3K 0.9520 . ? C3D H3L 0.9509 . ? 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 O917 Cu3 N71 91.64(17) . . ? O917 Cu3 O914 90.30(16) . . ? N71 Cu3 O914 170.59(17) . . ? O917 Cu3 N61 178.71(17) . . ? N71 Cu3 N61 88.04(18) . . ? O914 Cu3 N61 89.82(17) . . ? O917 Cu3 O910 95.62(15) . 1_565 ? N71 Cu3 O910 97.44(16) . 1_565 ? O914 Cu3 O910 91.53(16) . 1_565 ? N61 Cu3 O910 85.66(16) . 1_565 ? N31 Cu1 N31 179.997(2) 2_666 . ? N31 Cu1 N21 93.09(18) 2_666 . ? N31 Cu1 N21 86.91(18) . . ? N31 Cu1 N21 86.91(18) 2_666 2_666 ? N31 Cu1 N21 93.09(18) . 2_666 ? N21 Cu1 N21 179.999(1) . 2_666 ? N31 Cu1 N80 92.85(18) 2_666 2_666 ? N31 Cu1 N80 87.15(18) . 2_666 ? N21 Cu1 N80 85.21(17) . 2_666 ? N21 Cu1 N80 94.79(17) 2_666 2_666 ? N31 Cu1 N80 87.16(18) 2_666 . ? N31 Cu1 N80 92.85(18) . . ? N21 Cu1 N80 94.79(17) . . ? N21 Cu1 N80 85.21(17) 2_666 . ? N80 Cu1 N80 180.0 2_666 . ? O91 Cu2 O95 90.67(17) . . ? O91 Cu2 N41 171.53(17) . . ? O95 Cu2 N41 90.29(17) . . ? O91 Cu2 N51 90.48(18) . . ? O95 Cu2 N51 173.98(17) . . ? N41 Cu2 N51 87.71(18) . . ? O91 Cu2 O99 98.73(16) . . ? O95 Cu2 O99 83.70(15) . . ? N41 Cu2 O99 89.74(16) . . ? N51 Cu2 O99 101.97(16) . . ? C16 N1 C32 121.3(4) . . ? C16 N1 C22 120.0(4) . . ? C32 N1 C22 118.4(4) . . ? C12 N2 C52 121.5(4) . . ? C12 N2 C42 119.1(4) . . ? C52 N2 C42 119.4(4) . . ? C14 N3 C62 120.4(4) . . ? C14 N3 C72 121.0(4) . . ? C62 N3 C72 117.9(4) . . ? C12 N11 C16 113.1(4) . . ? N11 C12 N13 126.7(5) . . ? N11 C12 N2 117.6(4) . . ? N13 C12 N2 115.7(5) . . ? C14 N13 C12 112.9(4) . . ? N15 C14 N13 126.9(5) . . ? N15 C14 N3 117.7(5) . . ? N13 C14 N3 115.3(4) . . ? C16 N15 C14 113.3(4) . . ? N15 C16 N11 126.9(5) . . ? N15 C16 N1 118.1(5) . . ? N11 C16 N1 114.9(5) . . ? C22 N21 C26 116.6(5) . . ? C22 N21 Cu1 121.2(3) . . ? C26 N21 Cu1 122.1(4) . . ? N21 C22 C23 124.1(5) . . ? N21 C22 N1 115.1(5) . . ? C23 C22 N1 120.8(5) . . ? C22 C23 C24 117.9(6) . . ? C22 C23 H23 121.1 . . ? C24 C23 H23 121.1 . . ? C25 C24 C23 119.4(6) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 118.7(6) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? N21 C26 C25 123.2(6) . . ? N21 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C32 N31 C36 117.0(5) . . ? C32 N31 Cu1 120.5(4) . . ? C36 N31 Cu1 122.6(4) . . ? N31 C32 C33 123.4(5) . . ? N31 C32 N1 116.9(5) . . ? C33 C32 N1 119.6(5) . . ? C34 C33 C32 117.8(6) . . ? C34 C33 H33 121.1 . . ? C32 C33 H33 121.1 . . ? C33 C34 C35 119.7(6) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 119.1(6) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 N31 122.9(5) . . ? C35 C36 H36 118.5 . . ? N31 C36 H36 118.5 . . ? C42 N41 C46 118.3(4) . . ? C42 N41 Cu2 118.0(3) . . ? C46 N41 Cu2 123.6(4) . . ? N41 C42 C43 122.8(5) . . ? N41 C42 N2 115.6(4) . . ? C43 C42 N2 121.6(5) . . ? C42 C43 C44 118.4(5) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? C43 C44 C45 119.3(5) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C46 C45 C44 118.3(5) . . ? C46 C45 H45 120.8 . . ? C44 C45 H45 120.8 . . ? N41 C46 C45 122.8(5) . . ? N41 C46 H46 118.6 . . ? C45 C46 H46 118.6 . . ? C52 N51 C56 118.4(5) . . ? C52 N51 Cu2 117.7(3) . . ? C56 N51 Cu2 123.5(4) . . ? N51 C52 C53 122.4(5) . . ? N51 C52 N2 115.3(4) . . ? C53 C52 N2 122.3(5) . . ? C52 C53 C54 119.2(6) . . ? C52 C53 H53 120.4 . . ? C54 C53 H53 120.4 . . ? C53 C54 C55 119.5(6) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C56 C55 C54 118.5(6) . . ? C56 C55 H55 120.8 . . ? C54 C55 H55 120.8 . . ? N51 C56 C55 121.9(6) . . ? N51 C56 H56 119.0 . . ? C55 C56 H56 119.0 . . ? C62 N61 C66 119.3(5) . . ? C62 N61 Cu3 118.1(3) . . ? C66 N61 Cu3 122.5(4) . . ? N61 C62 C63 122.2(5) . . ? N61 C62 N3 115.8(5) . . ? C63 C62 N3 122.0(5) . . ? C64 C63 C62 118.1(6) . . ? C64 C63 H63 121.0 . . ? C62 C63 H63 121.0 . . ? C63 C64 C65 120.4(6) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C66 C65 C64 117.9(5) . . ? C66 C65 H65 121.0 . . ? C64 C65 H65 121.0 . . ? N61 C66 C65 122.0(6) . . ? N61 C66 H66 119.0 . . ? C65 C66 H66 119.0 . . ? C72 N71 C76 117.5(5) . . ? C72 N71 Cu3 118.4(3) . . ? C76 N71 Cu3 124.1(4) . . ? N71 C72 C73 123.1(5) . . ? N71 C72 N3 115.4(5) . . ? C73 C72 N3 121.4(5) . . ? C72 C73 C74 118.6(6) . . ? C72 C73 H73 120.7 . . ? C74 C73 H73 120.7 . . ? C75 C74 C73 118.5(6) . . ? C75 C74 H74 120.7 . . ? C73 C74 H74 120.7 . . ? C74 C75 C76 119.9(5) . . ? C74 C75 H75 120.1 . . ? C76 C75 H75 120.1 . . ? N71 C76 C75 122.3(5) . . ? N71 C76 H76 118.9 . . ? C75 C76 H76 118.9 . . ? C81 N80 Cu1 152.1(5) . . ? N80 C81 C82 179.4(10) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O93 N90 O92 121.6(6) . . ? O93 N90 O91 120.5(6) . . ? O92 N90 O91 117.9(5) . . ? N90 O91 Cu2 112.6(3) . . ? O97 N94 O96 123.9(6) . . ? O97 N94 O95 118.2(5) . . ? O96 N94 O95 118.0(5) . . ? N94 O95 Cu2 112.3(3) . . ? O911 N98 O99 120.3(5) . . ? O911 N98 O910 120.1(5) . . ? O99 N98 O910 119.5(5) . . ? N98 O99 Cu2 129.3(3) . . ? N98 O910 Cu3 133.6(3) . 1_545 ? O913 N912 O915 122.7(5) . . ? O913 N912 O914 118.9(5) . . ? O915 N912 O914 118.3(5) . . ? N912 O914 Cu3 108.5(3) . . ? O919 N916 O918 123.0(5) . . ? O919 N916 O917 118.1(5) . . ? O918 N916 O917 118.9(5) . . ? N916 O917 Cu3 115.5(3) . . ? N1A C2A C3A 178.2(8) . . ? C2A C3A H3A 109.7 . . ? C2A C3A H3B 108.9 . . ? H3A C3A H3B 110.2 . . ? C2A C3A H3C 108.9 . . ? H3A C3A H3C 109.8 . . ? H3B C3A H3C 109.4 . . ? N1B C2B C3B 177.5(10) . . ? C2B C3B H3D 109.4 . . ? C2B C3B H3E 109.0 . . ? H3D C3B H3E 109.2 . . ? C2B C3B H3F 109.6 . . ? H3D C3B H3F 110.3 . . ? H3E C3B H3F 109.3 . . ? N1C C2C C3C 177.4(12) . . ? C2C C3C H3G 110.1 . . ? C2C C3C H3H 108.3 . . ? H3G C3C H3H 110.5 . . ? C2C C3C H3I 108.5 . . ? H3G C3C H3I 110.7 . . ? H3H C3C H3I 108.8 . . ? N1D C2D C3D 152.9(19) . . ? C2D C3D H3J 106.0 . . ? C2D C3D H3K 109.6 . . ? H3J C3D H3K 108.5 . . ? C2D C3D H3L 110.1 . . ? H3J C3D H3L 108.7 . . ? H3K C3D H3L 113.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 N11 C12 N13 1.2(8) . . . . ? C16 N11 C12 N2 -178.3(4) . . . . ? C52 N2 C12 N11 178.8(5) . . . . ? C42 N2 C12 N11 -3.9(7) . . . . ? C52 N2 C12 N13 -0.9(7) . . . . ? C42 N2 C12 N13 176.5(4) . . . . ? N11 C12 N13 C14 -2.2(8) . . . . ? N2 C12 N13 C14 177.4(4) . . . . ? C12 N13 C14 N15 0.8(8) . . . . ? C12 N13 C14 N3 -178.9(4) . . . . ? C62 N3 C14 N15 -171.3(5) . . . . ? C72 N3 C14 N15 -1.0(7) . . . . ? C62 N3 C14 N13 8.4(7) . . . . ? C72 N3 C14 N13 178.8(5) . . . . ? N13 C14 N15 C16 1.3(8) . . . . ? N3 C14 N15 C16 -179.0(5) . . . . ? C14 N15 C16 N11 -2.4(8) . . . . ? C14 N15 C16 N1 180.0(5) . . . . ? C12 N11 C16 N15 1.3(8) . . . . ? C12 N11 C16 N1 178.9(4) . . . . ? C32 N1 C16 N15 -167.8(5) . . . . ? C22 N1 C16 N15 7.0(7) . . . . ? C32 N1 C16 N11 14.3(7) . . . . ? C22 N1 C16 N11 -170.9(5) . . . . ? N31 Cu1 N21 C22 -141.1(4) 2_666 . . . ? N31 Cu1 N21 C22 38.9(4) . . . . ? N80 Cu1 N21 C22 126.3(4) 2_666 . . . ? N80 Cu1 N21 C22 -53.7(4) . . . . ? N31 Cu1 N21 C26 42.8(4) 2_666 . . . ? N31 Cu1 N21 C26 -137.2(4) . . . . ? N80 Cu1 N21 C26 -49.8(4) 2_666 . . . ? N80 Cu1 N21 C26 130.2(4) . . . . ? C26 N21 C22 C23 -1.5(8) . . . . ? Cu1 N21 C22 C23 -177.8(4) . . . . ? C26 N21 C22 N1 176.3(5) . . . . ? Cu1 N21 C22 N1 0.0(6) . . . . ? C16 N1 C22 N21 127.5(5) . . . . ? C32 N1 C22 N21 -57.5(7) . . . . ? C16 N1 C22 C23 -54.6(7) . . . . ? C32 N1 C22 C23 120.3(6) . . . . ? N21 C22 C23 C24 -1.5(9) . . . . ? N1 C22 C23 C24 -179.2(5) . . . . ? C22 C23 C24 C25 2.5(9) . . . . ? C23 C24 C25 C26 -0.5(9) . . . . ? C22 N21 C26 C25 3.6(8) . . . . ? Cu1 N21 C26 C25 179.9(5) . . . . ? C24 C25 C26 N21 -2.7(9) . . . . ? N21 Cu1 N31 C32 -42.5(4) . . . . ? N21 Cu1 N31 C32 137.5(4) 2_666 . . . ? N80 Cu1 N31 C32 -127.8(4) 2_666 . . . ? N80 Cu1 N31 C32 52.2(4) . . . . ? N21 Cu1 N31 C36 137.9(4) . . . . ? N21 Cu1 N31 C36 -42.1(4) 2_666 . . . ? N80 Cu1 N31 C36 52.5(4) 2_666 . . . ? N80 Cu1 N31 C36 -127.5(4) . . . . ? C36 N31 C32 C33 2.1(8) . . . . ? Cu1 N31 C32 C33 -177.6(4) . . . . ? C36 N31 C32 N1 -173.9(5) . . . . ? Cu1 N31 C32 N1 6.5(6) . . . . ? C16 N1 C32 N31 -130.8(5) . . . . ? C22 N1 C32 N31 54.3(7) . . . . ? C16 N1 C32 C33 53.1(7) . . . . ? C22 N1 C32 C33 -121.8(6) . . . . ? N31 C32 C33 C34 0.7(9) . . . . ? N1 C32 C33 C34 176.5(5) . . . . ? C32 C33 C34 C35 -1.7(10) . . . . ? C33 C34 C35 C36 0.1(10) . . . . ? C34 C35 C36 N31 2.9(10) . . . . ? C32 N31 C36 C35 -3.9(9) . . . . ? Cu1 N31 C36 C35 175.8(5) . . . . ? O95 Cu2 N41 C42 130.0(4) . . . . ? N51 Cu2 N41 C42 -44.4(4) . . . . ? O99 Cu2 N41 C42 -146.3(4) . . . . ? O95 Cu2 N41 C46 -49.2(4) . . . . ? N51 Cu2 N41 C46 136.5(4) . . . . ? O99 Cu2 N41 C46 34.5(4) . . . . ? C46 N41 C42 C43 0.2(8) . . . . ? Cu2 N41 C42 C43 -179.0(4) . . . . ? C46 N41 C42 N2 -177.6(5) . . . . ? Cu2 N41 C42 N2 3.1(6) . . . . ? C12 N2 C42 N41 -119.5(5) . . . . ? C52 N2 C42 N41 57.9(6) . . . . ? C12 N2 C42 C43 62.6(7) . . . . ? C52 N2 C42 C43 -120.0(6) . . . . ? N41 C42 C43 C44 1.6(9) . . . . ? N2 C42 C43 C44 179.3(5) . . . . ? C42 C43 C44 C45 -1.2(9) . . . . ? C43 C44 C45 C46 -0.9(9) . . . . ? C42 N41 C46 C45 -2.5(8) . . . . ? Cu2 N41 C46 C45 176.7(5) . . . . ? C44 C45 C46 N41 2.8(9) . . . . ? O91 Cu2 N51 C52 -122.6(4) . . . . ? N41 Cu2 N51 C52 49.1(4) . . . . ? O99 Cu2 N51 C52 138.4(4) . . . . ? O91 Cu2 N51 C56 50.7(4) . . . . ? N41 Cu2 N51 C56 -137.6(4) . . . . ? O99 Cu2 N51 C56 -48.3(5) . . . . ? C56 N51 C52 C53 -3.0(8) . . . . ? Cu2 N51 C52 C53 170.6(4) . . . . ? C56 N51 C52 N2 175.1(5) . . . . ? Cu2 N51 C52 N2 -11.3(6) . . . . ? C12 N2 C52 N51 124.6(5) . . . . ? C42 N2 C52 N51 -52.7(6) . . . . ? C12 N2 C52 C53 -57.2(7) . . . . ? C42 N2 C52 C53 125.4(6) . . . . ? N51 C52 C53 C54 0.7(9) . . . . ? N2 C52 C53 C54 -177.3(5) . . . . ? C52 C53 C54 C55 1.7(9) . . . . ? C53 C54 C55 C56 -1.6(10) . . . . ? C52 N51 C56 C55 3.1(8) . . . . ? Cu2 N51 C56 C55 -170.2(5) . . . . ? C54 C55 C56 N51 -0.8(10) . . . . ? N71 Cu3 N61 C62 44.2(4) . . . . ? O914 Cu3 N61 C62 -126.7(4) . . . . ? O910 Cu3 N61 C62 141.8(4) 1_565 . . . ? N71 Cu3 N61 C66 -139.5(4) . . . . ? O914 Cu3 N61 C66 49.7(4) . . . . ? O910 Cu3 N61 C66 -41.8(4) 1_565 . . . ? C66 N61 C62 C63 -1.6(8) . . . . ? Cu3 N61 C62 C63 174.9(4) . . . . ? C66 N61 C62 N3 179.6(4) . . . . ? Cu3 N61 C62 N3 -4.0(6) . . . . ? C14 N3 C62 N61 112.3(5) . . . . ? C72 N3 C62 N61 -58.3(6) . . . . ? C14 N3 C62 C63 -66.5(7) . . . . ? C72 N3 C62 C63 122.9(6) . . . . ? N61 C62 C63 C64 -0.8(8) . . . . ? N3 C62 C63 C64 177.9(5) . . . . ? C62 C63 C64 C65 3.3(9) . . . . ? C63 C64 C65 C66 -3.3(9) . . . . ? C62 N61 C66 C65 1.6(8) . . . . ? Cu3 N61 C66 C65 -174.7(4) . . . . ? C64 C65 C66 N61 0.8(8) . . . . ? O917 Cu3 N71 C72 134.8(4) . . . . ? N61 Cu3 N71 C72 -43.9(4) . . . . ? O910 Cu3 N71 C72 -129.3(4) 1_565 . . . ? O917 Cu3 N71 C76 -43.5(4) . . . . ? N61 Cu3 N71 C76 137.7(4) . . . . ? O910 Cu3 N71 C76 52.3(4) 1_565 . . . ? C76 N71 C72 C73 1.5(7) . . . . ? Cu3 N71 C72 C73 -177.0(4) . . . . ? C76 N71 C72 N3 -177.5(4) . . . . ? Cu3 N71 C72 N3 4.1(6) . . . . ? C14 N3 C72 N71 -112.2(5) . . . . ? C62 N3 C72 N71 58.4(6) . . . . ? C14 N3 C72 C73 68.9(7) . . . . ? C62 N3 C72 C73 -120.5(6) . . . . ? N71 C72 C73 C74 0.3(8) . . . . ? N3 C72 C73 C74 179.2(5) . . . . ? C72 C73 C74 C75 -1.5(8) . . . . ? C73 C74 C75 C76 0.9(8) . . . . ? C72 N71 C76 C75 -2.1(7) . . . . ? Cu3 N71 C76 C75 176.3(4) . . . . ? C74 C75 C76 N71 0.9(8) . . . . ? N31 Cu1 N80 C81 -18.7(11) 2_666 . . . ? N31 Cu1 N80 C81 161.3(11) . . . . ? N21 Cu1 N80 C81 -111.5(11) . . . . ? N21 Cu1 N80 C81 68.5(11) 2_666 . . . ? O93 N90 O91 Cu2 -172.6(5) . . . . ? O92 N90 O91 Cu2 6.2(7) . . . . ? O95 Cu2 O91 N90 -109.8(4) . . . . ? N51 Cu2 O91 N90 64.3(4) . . . . ? O99 Cu2 O91 N90 166.4(4) . . . . ? O97 N94 O95 Cu2 174.5(4) . . . . ? O96 N94 O95 Cu2 -5.7(6) . . . . ? O91 Cu2 O95 N94 99.4(4) . . . . ? N41 Cu2 O95 N94 -72.2(4) . . . . ? O99 Cu2 O95 N94 -161.9(4) . . . . ? O911 N98 O99 Cu2 -9.2(8) . . . . ? O910 N98 O99 Cu2 168.7(4) . . . . ? O91 Cu2 O99 N98 -24.7(5) . . . . ? O95 Cu2 O99 N98 -114.4(5) . . . . ? N41 Cu2 O99 N98 155.3(5) . . . . ? N51 Cu2 O99 N98 67.7(5) . . . . ? O911 N98 O910 Cu3 163.4(5) . . . 1_545 ? O99 N98 O910 Cu3 -14.5(8) . . . 1_545 ? O913 N912 O914 Cu3 0.9(6) . . . . ? O915 N912 O914 Cu3 -178.5(4) . . . . ? O917 Cu3 O914 N912 -107.2(3) . . . . ? N61 Cu3 O914 N912 71.5(3) . . . . ? O910 Cu3 O914 N912 157.2(3) 1_565 . . . ? O919 N916 O917 Cu3 177.0(4) . . . . ? O918 N916 O917 Cu3 -3.9(7) . . . . ? N71 Cu3 O917 N916 -69.6(4) . . . . ? O914 Cu3 O917 N916 101.2(4) . . . . ? O910 Cu3 O917 N916 -167.2(4) 1_565 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.083 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.124 #===END