# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_section_title ;Molecular tectonics: ribbons type coordination networks based on porphyrins bearing two pyridine or two pyridine N-oxide units ; _publ_contact_author_name 'Prof. M.Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR loop_ _publ_author_name 'M. Hosseini' 'Veronique Bulach' 'Emmanuel Deiters' # Attachment 'NEW-2-Cu,CuClBF4.cif' data_e136a _database_code_depnum_ccdc_archive 'CCDC 656906' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C84 H52 Cl Cu3 N12 O4), 2(CHCl3), 2(BF4) , 3 (CH3OH)' _chemical_formula_sum 'C173 H118 B2 Cl8 Cu6 F8 N24 O11' _chemical_formula_weight 3547.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7001(3) _cell_length_b 17.1346(5) _cell_length_c 24.9317(8) _cell_angle_alpha 86.6580(10) _cell_angle_beta 79.721(2) _cell_angle_gamma 73.9430(10) _cell_volume 3918.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6986 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.52 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8878 _exptl_absorpt_correction_T_max 0.9323 _exptl_absorpt_process_details sadabs _exptl_special_details ; No hydrogen atoms were introduced on solvant molecules However,the missing hydrogen atoms have been added to the formula ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90211 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.57 _reflns_number_total 17993 _reflns_number_gt 12445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1336P)^2^+10.9270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17993 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2464 _refine_ls_wR_factor_gt 0.2195 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.32477(6) 0.13325(3) 1.00174(2) 0.02550(15) Uani 1 1 d . . . Cu2 Cu 0.54982(7) 0.13475(4) 0.46614(2) 0.03252(17) Uani 1 1 d . . . Cu3 Cu 0.29186(8) 0.59513(4) 0.72485(2) 0.03243(17) Uani 1 1 d . . . Cl1 Cl 0.35320(14) 0.71402(7) 0.71388(5) 0.0315(3) Uani 1 1 d . . . N1 N 0.2672(4) 0.1410(2) 0.92786(15) 0.0246(8) Uani 1 1 d . . . N2 N 0.2945(4) 0.0220(2) 1.01159(15) 0.0254(8) Uani 1 1 d . . . N3 N 0.3679(4) 0.1281(2) 1.07775(15) 0.0237(8) Uani 1 1 d . . . N4 N 0.3577(5) 0.2437(2) 0.99159(16) 0.0275(8) Uani 1 1 d . . . N7 N 0.5976(5) 0.3949(2) 1.17475(16) 0.0288(9) Uani 1 1 d . . . N8 N 0.2867(5) 0.4357(2) 0.76376(17) 0.0345(10) Uani 1 1 d . . . N9 N 0.4201(5) 0.2451(3) 0.45383(16) 0.0302(9) Uani 1 1 d . . . N10 N 0.5190(4) 0.0957(3) 0.39588(16) 0.0286(9) Uani 1 1 d . . . N11 N 0.6754(5) 0.0230(3) 0.47965(16) 0.0304(9) Uani 1 1 d . . . N12 N 0.5963(5) 0.1759(3) 0.53293(17) 0.0316(9) Uani 1 1 d . . . N13 N 0.0468(5) 0.3228(3) 0.26011(18) 0.0354(10) Uani 1 1 d . . . N16 N 0.2899(6) 0.5372(3) 0.62051(18) 0.0401(11) Uani 1 1 d . . . O1 O 0.6539(4) 0.4383(2) 1.20361(15) 0.0354(8) Uani 1 1 d . . . O2 O 0.2846(5) 0.4830(2) 0.71873(15) 0.0457(10) Uani 1 1 d . . . O3 O -0.0525(4) 0.3571(3) 0.22948(16) 0.0465(10) Uani 1 1 d . . . O4 O 0.2396(6) 0.6064(2) 0.65096(15) 0.0504(11) Uani 1 1 d . . . C1 C 0.2554(5) 0.2066(3) 0.89258(18) 0.0263(10) Uani 1 1 d . . . C2 C 0.1969(6) 0.1915(3) 0.84627(19) 0.0293(10) Uani 1 1 d . . . H2 H 0.1788 0.2271 0.8161 0.035 Uiso 1 1 calc R . . C3 C 0.1726(5) 0.1177(3) 0.85352(19) 0.0292(10) Uani 1 1 d . . . H3 H 0.1322 0.0920 0.8299 0.035 Uiso 1 1 calc R . . C4 C 0.2197(5) 0.0850(3) 0.90422(18) 0.0248(9) Uani 1 1 d . . . C5 C 0.2213(5) 0.0066(3) 0.92372(18) 0.0246(9) Uani 1 1 d . . . C6 C 0.2644(5) -0.0228(3) 0.97357(18) 0.0248(9) Uani 1 1 d . . . C7 C 0.2763(6) -0.1048(3) 0.9934(2) 0.0305(10) Uani 1 1 d . . . H7 H 0.2642 -0.1483 0.9744 0.037 Uiso 1 1 calc R . . C8 C 0.3076(6) -0.1077(3) 1.0439(2) 0.0304(10) Uani 1 1 d . . . H8 H 0.3219 -0.1540 1.0673 0.037 Uiso 1 1 calc R . . C9 C 0.3157(5) -0.0292(3) 1.05634(19) 0.0250(9) Uani 1 1 d . . . C10 C 0.3313(5) -0.0056(3) 1.10766(18) 0.0241(9) Uani 1 1 d . . . C11 C 0.3514(5) 0.0692(3) 1.11703(18) 0.0261(9) Uani 1 1 d . . . C12 C 0.3634(6) 0.0958(3) 1.16944(19) 0.0320(11) Uani 1 1 d . . . H12 H 0.3523 0.0676 1.2032 0.038 Uiso 1 1 calc R . . C13 C 0.3935(6) 0.1688(3) 1.16145(19) 0.0328(11) Uani 1 1 d . . . H13 H 0.4087 0.2010 1.1884 0.039 Uiso 1 1 calc R . . C14 C 0.3979(5) 0.1880(3) 1.10432(18) 0.0264(10) Uani 1 1 d . . . C15 C 0.4241(5) 0.2597(3) 1.08003(19) 0.0281(10) Uani 1 1 d . . . C16 C 0.4035(6) 0.2853(3) 1.0275(2) 0.0294(10) Uani 1 1 d . . . C17 C 0.4239(7) 0.3603(3) 1.0037(2) 0.0387(13) Uani 1 1 d . . . H17 H 0.4568 0.3990 1.0199 0.046 Uiso 1 1 calc R . . C18 C 0.3870(7) 0.3652(3) 0.9534(2) 0.0386(12) Uani 1 1 d . . . H18 H 0.3876 0.4087 0.9279 0.046 Uiso 1 1 calc R . . C19 C 0.3466(6) 0.2922(3) 0.94564(19) 0.0284(10) Uani 1 1 d . . . C20 C 0.2983(5) 0.2751(3) 0.89947(18) 0.0264(10) Uani 1 1 d . . . C21 C 0.1721(5) -0.0473(3) 0.89097(19) 0.0261(10) Uani 1 1 d . . . C22 C 0.2430(6) -0.0672(3) 0.8375(2) 0.0306(10) Uani 1 1 d . . . H22 H 0.3237 -0.0472 0.8223 0.037 Uiso 1 1 calc R . . C23 C 0.1953(7) -0.1164(3) 0.8067(2) 0.0397(13) Uani 1 1 d . . . H23 H 0.2428 -0.1294 0.7703 0.048 Uiso 1 1 calc R . . C24 C 0.0800(7) -0.1460(3) 0.8286(3) 0.0429(14) Uani 1 1 d . . . H24 H 0.0478 -0.1796 0.8074 0.052 Uiso 1 1 calc R . . C25 C 0.0106(6) -0.1275(3) 0.8812(3) 0.0401(13) Uani 1 1 d . . . H25 H -0.0696 -0.1482 0.8961 0.048 Uiso 1 1 calc R . . C26 C 0.0574(6) -0.0783(3) 0.9128(2) 0.0327(11) Uani 1 1 d . . . H26 H 0.0101 -0.0663 0.9493 0.039 Uiso 1 1 calc R . . C27 C 0.3217(5) -0.0646(3) 1.15357(18) 0.0274(10) Uani 1 1 d . . . C28 C 0.1982(6) -0.0939(3) 1.1669(2) 0.0349(11) Uani 1 1 d . . . H28 H 0.1203 -0.0751 1.1470 0.042 Uiso 1 1 calc R . . C29 C 0.1884(7) -0.1498(4) 1.2087(2) 0.0413(13) Uani 1 1 d . . . H29 H 0.1043 -0.1693 1.2172 0.050 Uiso 1 1 calc R . . C30 C 0.3008(7) -0.1773(3) 1.2382(2) 0.0433(14) Uani 1 1 d . . . H30 H 0.2942 -0.2160 1.2668 0.052 Uiso 1 1 calc R . . C31 C 0.4243(7) -0.1484(3) 1.2259(2) 0.0390(13) Uani 1 1 d . . . H31 H 0.5012 -0.1670 1.2463 0.047 Uiso 1 1 calc R . . C32 C 0.4342(6) -0.0924(3) 1.18371(19) 0.0307(10) Uani 1 1 d . . . H32 H 0.5183 -0.0730 1.1753 0.037 Uiso 1 1 calc R . . C33 C 0.4829(6) 0.3088(3) 1.11339(19) 0.0280(10) Uani 1 1 d . . . C34 C 0.4004(6) 0.3840(4) 1.1349(2) 0.0392(12) Uani 1 1 d . . . H34 H 0.3035 0.4064 1.1285 0.047 Uiso 1 1 calc R . . C35 C 0.4612(6) 0.4255(3) 1.1656(2) 0.0390(12) Uani 1 1 d . . . H35 H 0.4055 0.4766 1.1806 0.047 Uiso 1 1 calc R . . C36 C 0.6794(6) 0.3231(3) 1.1548(2) 0.0366(12) Uani 1 1 d . . . H36 H 0.7759 0.3023 1.1620 0.044 Uiso 1 1 calc R . . C37 C 0.6239(6) 0.2797(3) 1.1239(2) 0.0366(12) Uani 1 1 d . . . H37 H 0.6828 0.2288 1.1094 0.044 Uiso 1 1 calc R . . C38 C 0.2934(6) 0.3353(3) 0.8531(2) 0.0293(10) Uani 1 1 d . . . C39 C 0.4201(6) 0.3425(3) 0.8206(2) 0.0332(11) Uani 1 1 d . . . H39 H 0.5113 0.3117 0.8292 0.040 Uiso 1 1 calc R . . C40 C 0.4166(7) 0.3937(3) 0.7759(2) 0.0372(12) Uani 1 1 d . . . H40 H 0.5043 0.3992 0.7540 0.045 Uiso 1 1 calc R . . C42 C 0.1629(6) 0.3813(3) 0.8395(2) 0.0395(12) Uani 1 1 d . . . H42 H 0.0735 0.3787 0.8615 0.047 Uiso 1 1 calc R . . C43 C 0.3833(6) 0.3116(3) 0.4870(2) 0.0324(11) Uani 1 1 d . . . C44 C 0.2784(7) 0.3773(3) 0.4663(2) 0.0394(13) Uani 1 1 d . . . H44 H 0.2368 0.4298 0.4817 0.047 Uiso 1 1 calc R . . C45 C 0.2502(7) 0.3503(3) 0.4207(2) 0.0399(13) Uani 1 1 d . . . H45 H 0.1841 0.3801 0.3982 0.048 Uiso 1 1 calc R . . C46 C 0.3391(6) 0.2678(3) 0.4126(2) 0.0327(11) Uani 1 1 d . . . C47 C 0.3470(5) 0.2208(3) 0.36798(19) 0.0288(10) Uani 1 1 d . . . C48 C 0.4391(5) 0.1415(3) 0.35918(19) 0.0289(10) Uani 1 1 d . . . C49 C 0.4644(6) 0.0980(3) 0.3091(2) 0.0350(11) Uani 1 1 d . . . H49 H 0.4229 0.1169 0.2774 0.042 Uiso 1 1 calc R . . C50 C 0.5586(6) 0.0250(3) 0.3159(2) 0.0355(12) Uani 1 1 d . . . H50 H 0.5973 -0.0168 0.2896 0.043 Uiso 1 1 calc R . . C51 C 0.5897(6) 0.0226(3) 0.3709(2) 0.0312(11) Uani 1 1 d . . . C52 C 0.6714(5) -0.0450(3) 0.3955(2) 0.0309(10) Uani 1 1 d . . . C53 C 0.7036(6) -0.0446(3) 0.4481(2) 0.0316(11) Uani 1 1 d . . . C54 C 0.7777(6) -0.1147(3) 0.4761(2) 0.0363(12) Uani 1 1 d . . . H54 H 0.8060 -0.1692 0.4638 0.044 Uiso 1 1 calc R . . C55 C 0.7997(6) -0.0893(3) 0.5231(2) 0.0365(12) Uani 1 1 d . . . H55 H 0.8462 -0.1225 0.5501 0.044 Uiso 1 1 calc R . . C56 C 0.7405(6) -0.0029(3) 0.5250(2) 0.0318(11) Uani 1 1 d . . . C57 C 0.7563(6) 0.0482(3) 0.5636(2) 0.0315(11) Uani 1 1 d . . . C58 C 0.6931(6) 0.1315(3) 0.5656(2) 0.0330(11) Uani 1 1 d . . . C59 C 0.7146(6) 0.1859(3) 0.6036(2) 0.0363(12) Uani 1 1 d . . . H59 H 0.7801 0.1719 0.6289 0.044 Uiso 1 1 calc R . . C60 C 0.6253(6) 0.2601(4) 0.5966(2) 0.0388(12) Uani 1 1 d . . . H60 H 0.6137 0.3075 0.6168 0.047 Uiso 1 1 calc R . . C61 C 0.5499(6) 0.2535(3) 0.5522(2) 0.0324(11) Uani 1 1 d . . . C62 C 0.4458(6) 0.3170(3) 0.5326(2) 0.0333(11) Uani 1 1 d . . . C63 C 0.2485(6) 0.2552(3) 0.32772(19) 0.0301(10) Uani 1 1 d . . . C64 C 0.1391(6) 0.2193(3) 0.3214(2) 0.0355(11) Uani 1 1 d . . . H64 H 0.1332 0.1704 0.3405 0.043 Uiso 1 1 calc R . . C65 C 0.0399(6) 0.2542(4) 0.2878(2) 0.0390(12) Uani 1 1 d . . . H65 H -0.0342 0.2293 0.2843 0.047 Uiso 1 1 calc R . . C66 C 0.1524(6) 0.3584(4) 0.2643(2) 0.0403(13) Uani 1 1 d . . . H66 H 0.1570 0.4066 0.2441 0.048 Uiso 1 1 calc R . . C67 C 0.2548(6) 0.3250(3) 0.2979(2) 0.0359(11) Uani 1 1 d . . . H67 H 0.3290 0.3504 0.3003 0.043 Uiso 1 1 calc R . . C68 C 0.7360(6) -0.1222(3) 0.3636(2) 0.0316(11) Uani 1 1 d . . . C69 C 0.6495(6) -0.1655(3) 0.3475(2) 0.0365(12) Uani 1 1 d . . . H69 H 0.5466 -0.1450 0.3550 0.044 Uiso 1 1 calc R . . C70 C 0.7134(7) -0.2399(4) 0.3198(2) 0.0437(14) Uani 1 1 d . . . H70 H 0.6534 -0.2698 0.3094 0.052 Uiso 1 1 calc R . . C71 C 0.8593(8) -0.2684(4) 0.3082(2) 0.0480(15) Uani 1 1 d . . . H71 H 0.9018 -0.3178 0.2889 0.058 Uiso 1 1 calc R . . C72 C 0.9474(7) -0.2265(4) 0.3241(3) 0.0473(14) Uani 1 1 d . . . H72 H 1.0502 -0.2480 0.3166 0.057 Uiso 1 1 calc R . . C73 C 0.8876(6) -0.1530(3) 0.3511(2) 0.0396(12) Uani 1 1 d . . . H73 H 0.9491 -0.1237 0.3610 0.047 Uiso 1 1 calc R . . C41 C 0.1627(7) 0.4312(3) 0.7939(2) 0.0416(13) Uani 1 1 d . . . H41 H 0.0731 0.4622 0.7842 0.050 Uiso 1 1 calc R . . C74 C 0.8486(6) 0.0107(3) 0.6058(2) 0.0338(11) Uani 1 1 d . . . C75 C 0.9942(6) -0.0319(3) 0.5905(2) 0.0364(12) Uani 1 1 d . . . H75 H 1.0351 -0.0385 0.5530 0.044 Uiso 1 1 calc R . . C76 C 1.0801(6) -0.0647(4) 0.6298(2) 0.0422(13) Uani 1 1 d . . . H76 H 1.1791 -0.0937 0.6189 0.051 Uiso 1 1 calc R . . C77 C 1.0230(7) -0.0555(4) 0.6841(2) 0.0452(14) Uani 1 1 d . . . H77 H 1.0822 -0.0776 0.7107 0.054 Uiso 1 1 calc R . . C78 C 0.8782(7) -0.0137(4) 0.6999(2) 0.0421(13) Uani 1 1 d . . . H78 H 0.8383 -0.0070 0.7376 0.051 Uiso 1 1 calc R . . C79 C 0.7910(6) 0.0184(3) 0.6611(2) 0.0366(12) Uani 1 1 d . . . H79 H 0.6913 0.0459 0.6724 0.044 Uiso 1 1 calc R . . C80 C 0.3920(6) 0.3948(3) 0.5633(2) 0.0339(11) Uani 1 1 d . . . C81 C 0.2505(7) 0.4185(3) 0.5907(2) 0.0383(12) Uani 1 1 d . . . H81 H 0.1877 0.3850 0.5898 0.046 Uiso 1 1 calc R . . C82 C 0.1985(7) 0.4905(3) 0.6198(2) 0.0408(13) Uani 1 1 d . . . H82 H 0.1011 0.5065 0.6387 0.049 Uiso 1 1 calc R . . C83 C 0.4251(7) 0.5177(3) 0.5949(2) 0.0422(14) Uani 1 1 d . . . H83 H 0.4851 0.5525 0.5967 0.051 Uiso 1 1 calc R . . C84 C 0.4813(7) 0.4463(4) 0.5652(2) 0.0413(13) Uani 1 1 d . . . H84 H 0.5789 0.4326 0.5464 0.050 Uiso 1 1 calc R . . B1 B 0.7738(17) 0.4452(9) 0.7078(8) 0.1204(12) Uani 1 1 d . . . F1 F 0.8902(7) 0.4555(4) 0.6749(3) 0.1204(12) Uani 1 1 d . . . F2 F 0.8189(7) 0.4466(4) 0.7630(3) 0.1204(12) Uani 1 1 d . . . F3 F 0.6529(7) 0.5053(4) 0.7093(3) 0.1204(12) Uani 1 1 d . . . F4 F 0.7488(7) 0.3718(4) 0.7017(3) 0.1204(12) Uani 1 1 d . . . C85 C 0.7782(10) 0.3295(5) 0.9553(4) 0.103(4) Uani 1 1 d D . . Cl2A Cl 0.7778(7) 0.3428(6) 0.8852(3) 0.095(2) Uani 0.473(15) 1 d PD A 1 Cl3A Cl 0.9286(10) 0.2587(6) 0.9739(5) 0.095(2) Uani 0.473(15) 1 d PD A 1 Cl4A Cl 0.7463(8) 0.4250(4) 0.9871(4) 0.095(2) Uani 0.473(15) 1 d PD A 1 Cl2B Cl 0.7983(9) 0.3037(6) 0.8882(4) 0.133(2) Uani 0.527(15) 1 d PD A 2 Cl3B Cl 0.9315(13) 0.2692(6) 0.9836(6) 0.133(2) Uani 0.527(15) 1 d PD A 2 Cl4B Cl 0.7826(10) 0.4301(4) 0.9607(5) 0.133(2) Uani 0.527(15) 1 d PD A 2 C86 C 0.1739(15) 0.7448(6) 0.5541(5) 0.049(3) Uani 0.50 1 d P . . O5 O 0.0844(9) 0.6962(5) 0.5750(3) 0.0419(18) Uani 0.50 1 d P . . C87 C 0.0989(15) 0.6089(12) 0.4514(5) 0.067(5) Uani 0.50 1 d P . . O6 O 0.1662(10) 0.5796(5) 0.4958(3) 0.047(2) Uani 0.50 1 d P . . C88 C 1.0092(16) 0.3939(15) 0.0889(5) 0.089(7) Uani 0.50 1 d P . . O7 O 1.0603(8) 0.4140(5) 0.1301(3) 0.0412(19) Uani 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 Cu1 0.0339(3) 0.0276(3) 0.0189(3) 0.0017(2) -0.0086(2) -0.0125(2) Cu2 0.0369(4) 0.0355(3) 0.0265(3) -0.0032(2) -0.0114(3) -0.0076(3) Cu3 0.0556(4) 0.0237(3) 0.0229(3) 0.0016(2) -0.0153(3) -0.0136(3) Cl1 0.0390(7) 0.0221(5) 0.0360(6) -0.0012(4) -0.0048(5) -0.0135(5) N1 0.030(2) 0.026(2) 0.0194(18) 0.0011(15) -0.0071(15) -0.0091(16) N2 0.032(2) 0.026(2) 0.0205(18) 0.0041(15) -0.0107(16) -0.0083(16) N3 0.029(2) 0.029(2) 0.0186(18) 0.0022(15) -0.0076(15) -0.0135(16) N4 0.040(2) 0.028(2) 0.0194(18) 0.0015(15) -0.0105(16) -0.0134(17) N7 0.041(2) 0.026(2) 0.025(2) -0.0009(16) -0.0154(17) -0.0115(18) N8 0.063(3) 0.024(2) 0.025(2) 0.0066(16) -0.020(2) -0.019(2) N9 0.039(2) 0.032(2) 0.0220(19) -0.0020(16) -0.0094(17) -0.0105(18) N10 0.031(2) 0.032(2) 0.023(2) -0.0015(16) -0.0080(16) -0.0074(17) N11 0.033(2) 0.036(2) 0.024(2) 0.0007(17) -0.0107(17) -0.0088(18) N12 0.038(2) 0.033(2) 0.026(2) -0.0010(17) -0.0106(18) -0.0102(18) N13 0.038(2) 0.039(2) 0.027(2) 0.0015(18) -0.0113(18) -0.005(2) N16 0.067(3) 0.030(2) 0.025(2) 0.0006(18) -0.016(2) -0.011(2) O1 0.056(2) 0.0268(18) 0.0336(19) 0.0019(14) -0.0249(17) -0.0181(16) O2 0.094(3) 0.0298(19) 0.0248(18) 0.0085(15) -0.029(2) -0.025(2) O3 0.045(2) 0.059(3) 0.034(2) 0.0099(18) -0.0198(18) -0.0059(19) O4 0.098(4) 0.0256(19) 0.0266(19) -0.0018(15) -0.023(2) -0.008(2) C1 0.033(2) 0.027(2) 0.020(2) 0.0035(17) -0.0106(18) -0.0064(19) C2 0.038(3) 0.031(3) 0.023(2) 0.0045(19) -0.013(2) -0.012(2) C3 0.035(3) 0.036(3) 0.022(2) 0.0030(19) -0.0140(19) -0.014(2) C4 0.029(2) 0.030(2) 0.018(2) 0.0006(18) -0.0085(18) -0.0100(19) C5 0.031(2) 0.026(2) 0.019(2) -0.0013(17) -0.0071(18) -0.0093(19) C6 0.030(2) 0.024(2) 0.020(2) -0.0020(17) -0.0054(18) -0.0067(18) C7 0.042(3) 0.027(2) 0.025(2) -0.0019(19) -0.009(2) -0.012(2) C8 0.044(3) 0.024(2) 0.026(2) 0.0054(18) -0.013(2) -0.012(2) C9 0.030(2) 0.023(2) 0.023(2) 0.0030(17) -0.0064(18) -0.0079(18) C10 0.025(2) 0.029(2) 0.021(2) 0.0041(18) -0.0079(17) -0.0102(18) C11 0.032(2) 0.031(2) 0.018(2) 0.0033(18) -0.0071(18) -0.011(2) C12 0.046(3) 0.039(3) 0.017(2) 0.0052(19) -0.010(2) -0.020(2) C13 0.052(3) 0.035(3) 0.018(2) -0.0005(19) -0.013(2) -0.017(2) C14 0.034(3) 0.030(2) 0.020(2) 0.0001(18) -0.0096(18) -0.013(2) C15 0.037(3) 0.028(2) 0.023(2) -0.0017(18) -0.0100(19) -0.013(2) C16 0.040(3) 0.028(2) 0.025(2) 0.0012(19) -0.009(2) -0.015(2) C17 0.062(4) 0.033(3) 0.031(3) 0.003(2) -0.017(2) -0.025(3) C18 0.063(4) 0.030(3) 0.029(3) 0.007(2) -0.016(2) -0.020(3) C19 0.042(3) 0.023(2) 0.023(2) 0.0043(18) -0.011(2) -0.011(2) C20 0.034(3) 0.028(2) 0.019(2) 0.0055(18) -0.0088(18) -0.0092(19) C21 0.031(2) 0.023(2) 0.025(2) -0.0039(18) -0.0116(19) -0.0042(19) C22 0.038(3) 0.029(2) 0.024(2) -0.0015(19) -0.010(2) -0.006(2) C23 0.052(3) 0.038(3) 0.028(3) -0.007(2) -0.018(2) -0.002(3) C24 0.050(3) 0.035(3) 0.050(3) -0.012(2) -0.032(3) -0.003(2) C25 0.039(3) 0.035(3) 0.054(3) -0.001(2) -0.021(3) -0.014(2) C26 0.036(3) 0.031(3) 0.031(3) -0.001(2) -0.006(2) -0.007(2) C27 0.037(3) 0.031(2) 0.017(2) 0.0032(18) -0.0062(18) -0.014(2) C28 0.038(3) 0.045(3) 0.026(2) 0.006(2) -0.010(2) -0.017(2) C29 0.051(3) 0.046(3) 0.033(3) 0.007(2) -0.002(2) -0.029(3) C30 0.067(4) 0.035(3) 0.027(3) 0.009(2) -0.006(3) -0.015(3) C31 0.053(3) 0.034(3) 0.027(3) 0.002(2) -0.016(2) 0.000(2) C32 0.035(3) 0.035(3) 0.023(2) 0.0019(19) -0.009(2) -0.007(2) C33 0.039(3) 0.030(2) 0.022(2) 0.0026(18) -0.0113(19) -0.016(2) C34 0.039(3) 0.042(3) 0.040(3) -0.013(2) -0.012(2) -0.010(2) C35 0.045(3) 0.033(3) 0.040(3) -0.011(2) -0.013(2) -0.005(2) C36 0.041(3) 0.031(3) 0.042(3) -0.005(2) -0.020(2) -0.008(2) C37 0.045(3) 0.031(3) 0.037(3) -0.007(2) -0.018(2) -0.008(2) C38 0.042(3) 0.025(2) 0.026(2) 0.0032(18) -0.013(2) -0.012(2) C39 0.043(3) 0.029(3) 0.030(3) 0.004(2) -0.012(2) -0.011(2) C40 0.056(3) 0.030(3) 0.031(3) -0.001(2) -0.007(2) -0.020(2) C42 0.042(3) 0.037(3) 0.040(3) 0.012(2) -0.012(2) -0.010(2) C43 0.036(3) 0.034(3) 0.028(2) -0.003(2) -0.008(2) -0.008(2) C44 0.053(3) 0.032(3) 0.030(3) -0.007(2) -0.016(2) 0.000(2) C45 0.050(3) 0.034(3) 0.033(3) -0.003(2) -0.016(2) -0.001(2) C46 0.036(3) 0.036(3) 0.028(2) -0.002(2) -0.012(2) -0.007(2) C47 0.033(3) 0.033(3) 0.022(2) -0.0016(19) -0.0080(19) -0.010(2) C48 0.032(3) 0.033(3) 0.022(2) -0.0006(19) -0.0072(19) -0.009(2) C49 0.046(3) 0.039(3) 0.024(2) -0.002(2) -0.013(2) -0.011(2) C50 0.045(3) 0.036(3) 0.026(2) -0.004(2) -0.012(2) -0.008(2) C51 0.033(3) 0.035(3) 0.027(2) -0.007(2) -0.007(2) -0.010(2) C52 0.032(3) 0.037(3) 0.027(2) -0.004(2) -0.007(2) -0.013(2) C53 0.034(3) 0.036(3) 0.026(2) 0.004(2) -0.008(2) -0.012(2) C54 0.043(3) 0.030(3) 0.036(3) -0.001(2) -0.012(2) -0.008(2) C55 0.043(3) 0.039(3) 0.027(3) 0.007(2) -0.011(2) -0.009(2) C56 0.031(3) 0.041(3) 0.024(2) 0.002(2) -0.0066(19) -0.010(2) C57 0.032(3) 0.040(3) 0.022(2) 0.001(2) -0.0061(19) -0.009(2) C58 0.037(3) 0.041(3) 0.022(2) 0.001(2) -0.010(2) -0.010(2) C59 0.045(3) 0.039(3) 0.029(3) -0.002(2) -0.016(2) -0.012(2) C60 0.049(3) 0.044(3) 0.028(3) -0.003(2) -0.016(2) -0.015(3) C61 0.041(3) 0.035(3) 0.025(2) 0.000(2) -0.010(2) -0.013(2) C62 0.045(3) 0.034(3) 0.024(2) -0.002(2) -0.011(2) -0.013(2) C63 0.035(3) 0.031(3) 0.024(2) -0.0019(19) -0.007(2) -0.006(2) C64 0.044(3) 0.037(3) 0.029(3) 0.002(2) -0.012(2) -0.014(2) C65 0.045(3) 0.047(3) 0.032(3) 0.002(2) -0.015(2) -0.018(3) C66 0.047(3) 0.041(3) 0.032(3) 0.009(2) -0.015(2) -0.008(3) C67 0.040(3) 0.035(3) 0.035(3) 0.002(2) -0.013(2) -0.010(2) C68 0.040(3) 0.032(3) 0.023(2) 0.0016(19) -0.008(2) -0.009(2) C69 0.039(3) 0.032(3) 0.040(3) -0.004(2) -0.012(2) -0.010(2) C70 0.062(4) 0.036(3) 0.038(3) -0.003(2) -0.020(3) -0.014(3) C71 0.071(4) 0.031(3) 0.035(3) -0.005(2) -0.009(3) -0.002(3) C72 0.043(3) 0.041(3) 0.051(4) -0.007(3) 0.000(3) -0.003(3) C73 0.039(3) 0.037(3) 0.042(3) -0.003(2) -0.003(2) -0.011(2) C41 0.049(3) 0.033(3) 0.044(3) 0.008(2) -0.023(3) -0.006(2) C74 0.041(3) 0.038(3) 0.026(2) 0.006(2) -0.011(2) -0.013(2) C75 0.036(3) 0.043(3) 0.031(3) 0.006(2) -0.009(2) -0.013(2) C76 0.038(3) 0.048(3) 0.042(3) 0.008(3) -0.015(2) -0.011(3) C77 0.057(4) 0.048(3) 0.040(3) 0.014(3) -0.027(3) -0.022(3) C78 0.061(4) 0.042(3) 0.030(3) 0.004(2) -0.015(3) -0.022(3) C79 0.042(3) 0.040(3) 0.028(3) 0.002(2) -0.007(2) -0.012(2) C80 0.052(3) 0.031(3) 0.022(2) -0.0006(19) -0.015(2) -0.011(2) C81 0.052(3) 0.037(3) 0.030(3) -0.006(2) -0.013(2) -0.014(2) C82 0.054(4) 0.039(3) 0.029(3) -0.007(2) -0.011(2) -0.008(3) C83 0.069(4) 0.034(3) 0.034(3) 0.004(2) -0.017(3) -0.026(3) C84 0.056(4) 0.040(3) 0.031(3) 0.004(2) -0.011(2) -0.018(3) B1 0.095(2) 0.0823(19) 0.169(3) -0.020(2) 0.023(2) -0.0237(16) F1 0.095(2) 0.0823(19) 0.169(3) -0.020(2) 0.023(2) -0.0237(16) F2 0.095(2) 0.0823(19) 0.169(3) -0.020(2) 0.023(2) -0.0237(16) F3 0.095(2) 0.0823(19) 0.169(3) -0.020(2) 0.023(2) -0.0237(16) F4 0.095(2) 0.0823(19) 0.169(3) -0.020(2) 0.023(2) -0.0237(16) C85 0.071(6) 0.097(8) 0.136(10) -0.048(7) 0.004(6) -0.019(5) Cl2A 0.067(2) 0.086(3) 0.130(4) -0.011(2) -0.0135(19) -0.0204(17) Cl3A 0.067(2) 0.086(3) 0.130(4) -0.011(2) -0.0135(19) -0.0204(17) Cl4A 0.067(2) 0.086(3) 0.130(4) -0.011(2) -0.0135(19) -0.0204(17) Cl2B 0.122(3) 0.071(3) 0.186(5) -0.002(3) 0.012(3) -0.016(2) Cl3B 0.122(3) 0.071(3) 0.186(5) -0.002(3) 0.012(3) -0.016(2) Cl4B 0.122(3) 0.071(3) 0.186(5) -0.002(3) 0.012(3) -0.016(2) C86 0.074(9) 0.016(5) 0.045(7) -0.004(4) 0.028(6) -0.015(5) O5 0.042(4) 0.058(5) 0.022(4) 0.006(3) -0.007(3) -0.008(4) C87 0.051(8) 0.136(15) 0.035(6) 0.018(8) -0.017(6) -0.054(9) O6 0.057(5) 0.043(5) 0.038(4) -0.002(4) -0.015(4) -0.006(4) C88 0.052(8) 0.22(2) 0.021(6) -0.002(9) -0.005(5) -0.082(12) O7 0.027(4) 0.075(6) 0.024(4) 0.013(4) -0.005(3) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.999(4) . ? Cu1 N2 2.003(4) . ? Cu1 N3 2.004(4) . ? Cu1 N1 2.005(4) . ? Cu2 N9 2.002(4) . ? Cu2 N10 2.009(4) . ? Cu2 N11 2.011(4) . ? Cu2 N12 2.013(4) . ? Cu3 O2 1.958(4) . ? Cu3 O1 1.959(3) 2_667 ? Cu3 O4 1.981(4) . ? Cu3 Cl1 2.2641(12) . ? Cu3 O3 2.339(4) 2_566 ? N1 C4 1.374(6) . ? N1 C1 1.379(6) . ? N2 C6 1.371(6) . ? N2 C9 1.387(6) . ? N3 C14 1.375(6) . ? N3 C11 1.386(6) . ? N4 C16 1.377(6) . ? N4 C19 1.377(6) . ? N7 C36 1.334(7) . ? N7 C35 1.336(7) . ? N7 O1 1.341(5) . ? N8 C41 1.319(8) . ? N8 C40 1.344(7) . ? N8 O2 1.345(5) . ? N9 C43 1.373(6) . ? N9 C46 1.377(6) . ? N10 C48 1.374(6) . ? N10 C51 1.376(6) . ? N11 C53 1.374(7) . ? N11 C56 1.384(6) . ? N12 C61 1.367(7) . ? N12 C58 1.388(6) . ? N13 O3 1.324(5) . ? N13 C65 1.341(7) . ? N13 C66 1.350(8) . ? N16 C83 1.313(8) . ? N16 C82 1.351(8) . ? N16 O4 1.369(6) . ? O1 Cu3 1.959(3) 2_667 ? O3 Cu3 2.339(4) 2_566 ? C1 C20 1.378(7) . ? C1 C2 1.440(6) . ? C2 C3 1.345(7) . ? C2 H2 0.9500 . ? C3 C4 1.450(6) . ? C3 H3 0.9500 . ? C4 C5 1.399(7) . ? C5 C6 1.403(6) . ? C5 C21 1.490(6) . ? C6 C7 1.443(7) . ? C7 C8 1.343(7) . ? C7 H7 0.9500 . ? C8 C9 1.423(7) . ? C8 H8 0.9500 . ? C9 C10 1.409(6) . ? C10 C11 1.388(7) . ? C10 C27 1.490(6) . ? C11 C12 1.443(6) . ? C12 C13 1.356(7) . ? C12 H12 0.9500 . ? C13 C14 1.439(6) . ? C13 H13 0.9500 . ? C14 C15 1.406(7) . ? C15 C16 1.388(7) . ? C15 C33 1.497(6) . ? C16 C17 1.433(7) . ? C17 C18 1.356(7) . ? C17 H17 0.9500 . ? C18 C19 1.443(7) . ? C18 H18 0.9500 . ? C19 C20 1.392(6) . ? C20 C38 1.501(6) . ? C21 C26 1.376(7) . ? C21 C22 1.402(7) . ? C22 C23 1.390(7) . ? C22 H22 0.9500 . ? C23 C24 1.368(9) . ? C23 H23 0.9500 . ? C24 C25 1.375(9) . ? C24 H24 0.9500 . ? C25 C26 1.398(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.395(7) . ? C27 C28 1.403(7) . ? C28 C29 1.382(7) . ? C28 H28 0.9500 . ? C29 C30 1.383(9) . ? C29 H29 0.9500 . ? C30 C31 1.398(9) . ? C30 H30 0.9500 . ? C31 C32 1.390(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C37 1.387(7) . ? C33 C34 1.395(8) . ? C34 C35 1.376(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.369(7) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.379(8) . ? C38 C42 1.382(7) . ? C39 C40 1.377(7) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C42 C41 1.383(8) . ? C42 H42 0.9500 . ? C43 C62 1.400(7) . ? C43 C44 1.434(7) . ? C44 C45 1.350(7) . ? C44 H44 0.9500 . ? C45 C46 1.443(8) . ? C45 H45 0.9500 . ? C46 C47 1.390(7) . ? C47 C48 1.408(7) . ? C47 C63 1.493(7) . ? C48 C49 1.440(7) . ? C49 C50 1.351(8) . ? C49 H49 0.9500 . ? C50 C51 1.453(7) . ? C50 H50 0.9500 . ? C51 C52 1.389(7) . ? C52 C53 1.402(7) . ? C52 C68 1.503(7) . ? C53 C54 1.432(7) . ? C54 C55 1.344(8) . ? C54 H54 0.9500 . ? C55 C56 1.432(8) . ? C55 H55 0.9500 . ? C56 C57 1.394(7) . ? C57 C58 1.389(8) . ? C57 C74 1.504(7) . ? C58 C59 1.446(7) . ? C59 C60 1.347(8) . ? C59 H59 0.9500 . ? C60 C61 1.459(7) . ? C60 H60 0.9500 . ? C61 C62 1.396(7) . ? C62 C80 1.492(7) . ? C63 C67 1.382(7) . ? C63 C64 1.401(7) . ? C64 C65 1.376(7) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 C67 1.394(7) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C69 1.384(7) . ? C68 C73 1.401(8) . ? C69 C70 1.413(8) . ? C69 H69 0.9500 . ? C70 C71 1.346(9) . ? C70 H70 0.9500 . ? C71 C72 1.379(9) . ? C71 H71 0.9500 . ? C72 C73 1.389(8) . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C41 H41 0.9500 . ? C74 C79 1.391(7) . ? C74 C75 1.393(8) . ? C75 C76 1.393(7) . ? C75 H75 0.9500 . ? C76 C77 1.367(9) . ? C76 H76 0.9500 . ? C77 C78 1.386(9) . ? C77 H77 0.9500 . ? C78 C79 1.387(8) . ? C78 H78 0.9500 . ? C79 H79 0.9500 . ? C80 C81 1.380(8) . ? C80 C84 1.406(8) . ? C81 C82 1.389(8) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.390(8) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? B1 F1 1.319(15) . ? B1 F3 1.325(16) . ? B1 F4 1.368(16) . ? B1 F2 1.52(2) . ? C85 Cl2B 1.719(11) . ? C85 Cl3A 1.736(12) . ? C85 Cl4B 1.749(11) . ? C85 Cl2A 1.751(11) . ? C85 Cl4A 1.784(10) . ? C85 Cl3B 1.793(13) . ? C86 O5 1.381(14) . ? C87 O6 1.384(15) . ? C88 O7 1.317(15) . ? 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 N4 Cu1 N2 179.26(18) . . ? N4 Cu1 N3 90.05(15) . . ? N2 Cu1 N3 89.92(15) . . ? N4 Cu1 N1 90.37(16) . . ? N2 Cu1 N1 89.70(15) . . ? N3 Cu1 N1 176.10(16) . . ? N9 Cu2 N10 90.66(16) . . ? N9 Cu2 N11 178.42(18) . . ? N10 Cu2 N11 89.39(17) . . ? N9 Cu2 N12 89.76(17) . . ? N10 Cu2 N12 175.08(18) . . ? N11 Cu2 N12 90.33(17) . . ? O2 Cu3 O1 85.62(14) . 2_667 ? O2 Cu3 O4 83.32(15) . . ? O1 Cu3 O4 168.89(15) 2_667 . ? O2 Cu3 Cl1 164.45(15) . . ? O1 Cu3 Cl1 99.81(11) 2_667 . ? O4 Cu3 Cl1 90.64(13) . . ? O2 Cu3 O3 95.66(19) . 2_566 ? O1 Cu3 O3 86.96(15) 2_667 2_566 ? O4 Cu3 O3 95.14(17) . 2_566 ? Cl1 Cu3 O3 99.15(12) . 2_566 ? C4 N1 C1 106.1(4) . . ? C4 N1 Cu1 126.9(3) . . ? C1 N1 Cu1 126.7(3) . . ? C6 N2 C9 105.6(4) . . ? C6 N2 Cu1 127.3(3) . . ? C9 N2 Cu1 126.8(3) . . ? C14 N3 C11 105.5(4) . . ? C14 N3 Cu1 126.9(3) . . ? C11 N3 Cu1 126.9(3) . . ? C16 N4 C19 105.7(4) . . ? C16 N4 Cu1 127.5(3) . . ? C19 N4 Cu1 126.7(3) . . ? C36 N7 C35 121.5(4) . . ? C36 N7 O1 119.5(4) . . ? C35 N7 O1 119.0(4) . . ? C41 N8 C40 122.3(4) . . ? C41 N8 O2 119.5(5) . . ? C40 N8 O2 118.2(5) . . ? C43 N9 C46 105.8(4) . . ? C43 N9 Cu2 127.4(3) . . ? C46 N9 Cu2 126.6(3) . . ? C48 N10 C51 105.8(4) . . ? C48 N10 Cu2 126.3(3) . . ? C51 N10 Cu2 127.2(3) . . ? C53 N11 C56 106.1(4) . . ? C53 N11 Cu2 126.9(3) . . ? C56 N11 Cu2 126.7(3) . . ? C61 N12 C58 106.7(4) . . ? C61 N12 Cu2 127.2(3) . . ? C58 N12 Cu2 125.8(3) . . ? O3 N13 C65 120.0(5) . . ? O3 N13 C66 119.7(5) . . ? C65 N13 C66 120.4(5) . . ? C83 N16 C82 122.9(5) . . ? C83 N16 O4 119.1(5) . . ? C82 N16 O4 118.0(5) . . ? N7 O1 Cu3 123.8(3) . 2_667 ? N8 O2 Cu3 118.4(3) . . ? N13 O3 Cu3 116.4(3) . 2_566 ? N16 O4 Cu3 114.9(3) . . ? C20 C1 N1 125.2(4) . . ? C20 C1 C2 125.0(4) . . ? N1 C1 C2 109.8(4) . . ? C3 C2 C1 107.5(4) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 106.9(4) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 126.4(4) . . ? N1 C4 C3 109.7(4) . . ? C5 C4 C3 123.9(4) . . ? C4 C5 C6 122.6(4) . . ? C4 C5 C21 118.8(4) . . ? C6 C5 C21 118.6(4) . . ? N2 C6 C5 125.8(4) . . ? N2 C6 C7 110.0(4) . . ? C5 C6 C7 124.1(4) . . ? C8 C7 C6 106.7(4) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? C7 C8 C9 108.0(4) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? N2 C9 C10 125.3(4) . . ? N2 C9 C8 109.6(4) . . ? C10 C9 C8 125.0(4) . . ? C11 C10 C9 123.3(4) . . ? C11 C10 C27 119.8(4) . . ? C9 C10 C27 116.9(4) . . ? N3 C11 C10 125.6(4) . . ? N3 C11 C12 109.9(4) . . ? C10 C11 C12 124.5(4) . . ? C13 C12 C11 107.1(4) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? C12 C13 C14 106.8(4) . . ? C12 C13 H13 126.6 . . ? C14 C13 H13 126.6 . . ? N3 C14 C15 125.3(4) . . ? N3 C14 C13 110.6(4) . . ? C15 C14 C13 124.1(4) . . ? C16 C15 C14 124.2(4) . . ? C16 C15 C33 119.4(4) . . ? C14 C15 C33 116.4(4) . . ? N4 C16 C15 125.2(4) . . ? N4 C16 C17 110.7(4) . . ? C15 C16 C17 124.1(5) . . ? C18 C17 C16 106.6(5) . . ? C18 C17 H17 126.7 . . ? C16 C17 H17 126.7 . . ? C17 C18 C19 107.3(4) . . ? C17 C18 H18 126.4 . . ? C19 C18 H18 126.4 . . ? N4 C19 C20 125.3(4) . . ? N4 C19 C18 109.7(4) . . ? C20 C19 C18 124.9(4) . . ? C1 C20 C19 125.1(4) . . ? C1 C20 C38 117.0(4) . . ? C19 C20 C38 117.9(4) . . ? C26 C21 C22 119.3(4) . . ? C26 C21 C5 120.6(4) . . ? C22 C21 C5 120.1(4) . . ? C23 C22 C21 120.0(5) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.2(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.3(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 120.3(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 119.9(5) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C32 C27 C28 118.7(4) . . ? C32 C27 C10 121.4(4) . . ? C28 C27 C10 120.0(4) . . ? C29 C28 C27 120.9(5) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.1(5) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 120.0(5) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 119.8(5) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C27 120.6(5) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? C37 C33 C34 117.8(4) . . ? C37 C33 C15 119.9(5) . . ? C34 C33 C15 122.3(5) . . ? C35 C34 C33 119.1(5) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? N7 C35 C34 121.0(5) . . ? N7 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? N7 C36 C37 119.7(5) . . ? N7 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C33 120.9(5) . . ? C36 C37 H37 119.5 . . ? C33 C37 H37 119.5 . . ? C39 C38 C42 117.8(5) . . ? C39 C38 C20 120.5(5) . . ? C42 C38 C20 121.5(5) . . ? C40 C39 C38 121.0(5) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? N8 C40 C39 118.7(5) . . ? N8 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C38 C42 C41 119.8(5) . . ? C38 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? N9 C43 C62 125.2(5) . . ? N9 C43 C44 110.5(4) . . ? C62 C43 C44 124.1(5) . . ? C45 C44 C43 106.8(5) . . ? C45 C44 H44 126.6 . . ? C43 C44 H44 126.6 . . ? C44 C45 C46 107.3(5) . . ? C44 C45 H45 126.3 . . ? C46 C45 H45 126.4 . . ? N9 C46 C47 125.8(5) . . ? N9 C46 C45 109.6(4) . . ? C47 C46 C45 124.5(5) . . ? C46 C47 C48 124.0(4) . . ? C46 C47 C63 118.2(4) . . ? C48 C47 C63 117.8(4) . . ? N10 C48 C47 125.6(4) . . ? N10 C48 C49 110.6(4) . . ? C47 C48 C49 123.8(4) . . ? C50 C49 C48 106.8(4) . . ? C50 C49 H49 126.6 . . ? C48 C49 H49 126.6 . . ? C49 C50 C51 107.1(5) . . ? C49 C50 H50 126.5 . . ? C51 C50 H50 126.5 . . ? N10 C51 C52 125.3(4) . . ? N10 C51 C50 109.7(4) . . ? C52 C51 C50 124.9(5) . . ? C51 C52 C53 123.5(5) . . ? C51 C52 C68 119.1(4) . . ? C53 C52 C68 117.3(5) . . ? N11 C53 C52 125.6(5) . . ? N11 C53 C54 109.5(4) . . ? C52 C53 C54 124.8(5) . . ? C55 C54 C53 107.4(5) . . ? C55 C54 H54 126.3 . . ? C53 C54 H54 126.3 . . ? C54 C55 C56 107.6(5) . . ? C54 C55 H55 126.2 . . ? C56 C55 H55 126.2 . . ? N11 C56 C57 124.9(5) . . ? N11 C56 C55 109.2(4) . . ? C57 C56 C55 125.7(5) . . ? C58 C57 C56 124.4(5) . . ? C58 C57 C74 117.8(5) . . ? C56 C57 C74 117.8(5) . . ? N12 C58 C57 126.1(5) . . ? N12 C58 C59 108.8(5) . . ? C57 C58 C59 125.0(5) . . ? C60 C59 C58 107.9(5) . . ? C60 C59 H59 126.0 . . ? C58 C59 H59 126.0 . . ? C59 C60 C61 106.7(5) . . ? C59 C60 H60 126.7 . . ? C61 C60 H60 126.7 . . ? N12 C61 C62 125.4(5) . . ? N12 C61 C60 109.7(5) . . ? C62 C61 C60 124.9(5) . . ? C61 C62 C43 124.1(5) . . ? C61 C62 C80 118.5(4) . . ? C43 C62 C80 117.3(5) . . ? C67 C63 C64 117.4(5) . . ? C67 C63 C47 122.4(5) . . ? C64 C63 C47 120.0(5) . . ? C65 C64 C63 120.7(5) . . ? C65 C64 H64 119.7 . . ? C63 C64 H64 119.7 . . ? N13 C65 C64 120.7(5) . . ? N13 C65 H65 119.6 . . ? C64 C65 H65 119.6 . . ? N13 C66 C67 120.7(5) . . ? N13 C66 H66 119.7 . . ? C67 C66 H66 119.7 . . ? C63 C67 C66 120.1(5) . . ? C63 C67 H67 120.0 . . ? C66 C67 H67 119.9 . . ? C69 C68 C73 118.6(5) . . ? C69 C68 C52 121.7(5) . . ? C73 C68 C52 119.7(5) . . ? C68 C69 C70 120.4(5) . . ? C68 C69 H69 119.8 . . ? C70 C69 H69 119.8 . . ? C71 C70 C69 120.0(6) . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C70 C71 C72 120.5(6) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C71 C72 C73 120.7(6) . . ? C71 C72 H72 119.7 . . ? C73 C72 H72 119.7 . . ? C72 C73 C68 119.8(6) . . ? C72 C73 H73 120.1 . . ? C68 C73 H73 120.1 . . ? N8 C41 C42 120.2(5) . . ? N8 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C79 C74 C75 118.4(5) . . ? C79 C74 C57 120.7(5) . . ? C75 C74 C57 120.9(5) . . ? C76 C75 C74 120.6(5) . . ? C76 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? C77 C76 C75 120.5(6) . . ? C77 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? C76 C77 C78 119.6(5) . . ? C76 C77 H77 120.2 . . ? C78 C77 H77 120.2 . . ? C77 C78 C79 120.4(5) . . ? C77 C78 H78 119.8 . . ? C79 C78 H78 119.8 . . ? C78 C79 C74 120.4(5) . . ? C78 C79 H79 119.8 . . ? C74 C79 H79 119.8 . . ? C81 C80 C84 117.8(5) . . ? C81 C80 C62 120.3(5) . . ? C84 C80 C62 121.9(5) . . ? C80 C81 C82 121.1(5) . . ? C80 C81 H81 119.4 . . ? C82 C81 H81 119.5 . . ? N16 C82 C81 118.4(6) . . ? N16 C82 H82 120.8 . . ? C81 C82 H82 120.8 . . ? N16 C83 C84 120.6(5) . . ? N16 C83 H83 119.7 . . ? C84 C83 H83 119.7 . . ? C83 C84 C80 119.2(6) . . ? C83 C84 H84 120.4 . . ? C80 C84 H84 120.4 . . ? F1 B1 F3 116.5(14) . . ? F1 B1 F4 113.3(12) . . ? F3 B1 F4 111.3(13) . . ? F1 B1 F2 100.7(12) . . ? F3 B1 F2 105.1(12) . . ? F4 B1 F2 108.8(13) . . ? Cl2B C85 Cl4B 110.9(7) . . ? Cl3A C85 Cl2A 115.9(6) . . ? Cl3A C85 Cl4A 111.6(6) . . ? Cl2A C85 Cl4A 110.5(6) . . ? Cl2B C85 Cl3B 109.0(7) . . ? Cl4B C85 Cl3B 105.2(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.563 _refine_diff_density_min -1.427 _refine_diff_density_rms 0.146 # Attachment 'NEW1-Cu-CdNO3.cif' data_e412a _database_code_depnum_ccdc_archive 'CCDC 656907' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85.50 H55 Cd Cl3 Cu2 N14 O6.50' _chemical_formula_weight 1728.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 8.7394(4) _cell_length_b 27.7882(16) _cell_length_c 31.3773(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7620.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2941 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 19.53 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3500 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9332 _exptl_absorpt_correction_T_max 0.9802 _exptl_absorpt_process_details sadabs _exptl_special_details ; One nitrate ion is disordered over two positions. No hydrogen atoms were introduced on solvant molecules However,the missing hydrogen atoms have been added to the formula ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55803 _diffrn_reflns_av_R_equivalents 0.1622 _diffrn_reflns_av_sigmaI/netI 0.1450 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8890 _reflns_number_gt 4364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. The large Rint value is due to a small cystal size, a poor crystal quality and a very weak diffracting power. 14 restraints were used in the refinement. For sake of homogeneity, the 3 independant nitrate anions has been refined using the same DFIX restraint for the NO distances. Moreover, one CHCl3 ( C45Cl4Cl5 Cl5$1) appears to be severely disordered,it has been refined isotropically and restraints on distances and angles have been introduced. ; _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^)+(0.1000P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8890 _refine_ls_number_parameters 502 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.2138 _refine_ls_R_factor_gt 0.1123 _refine_ls_wR_factor_ref 0.3157 _refine_ls_wR_factor_gt 0.2858 _refine_ls_goodness_of_fit_ref 1.566 _refine_ls_restrained_S_all 1.583 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.004 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 N6 N 0.4318(9) 0.3626(3) 0.3018(3) 0.033(2) Uani 1 1 d . . . C29 C 0.3324(13) 0.3871(5) 0.3260(4) 0.053(3) Uani 1 1 d . . . C28 C 0.5768(13) 0.3746(5) 0.3079(4) 0.052(4) Uani 1 1 d . . . Cd1 Cd 0.64990(12) 0.80597(4) 0.2500 0.0299(3) Uani 1 2 d S . . Cu2 Cu 0.75710(15) 0.54230(5) 0.46686(4) 0.0322(4) Uani 1 1 d . . . N1 N 0.8241(10) 0.6105(3) 0.4665(2) 0.033(2) Uani 1 1 d . . . N2 N 0.6968(9) 0.5475(3) 0.4063(3) 0.032(2) Uani 1 1 d . . . N3 N 0.6676(9) 0.4773(3) 0.4695(2) 0.033(2) Uani 1 1 d . . . N4 N 0.8389(10) 0.5342(3) 0.5251(2) 0.033(2) Uani 1 1 d . . . C1 C 0.8870(12) 0.6355(4) 0.5000(3) 0.034(3) Uani 1 1 d . . . C2 C 0.9030(15) 0.6856(4) 0.4895(3) 0.050(3) Uani 1 1 d . . . H2 H 0.9436 0.7102 0.5073 0.060 Uiso 1 1 calc R . . C3 C 0.8480(14) 0.6907(4) 0.4491(3) 0.047(3) Uani 1 1 d . . . H3 H 0.8416 0.7199 0.4333 0.056 Uiso 1 1 calc R . . C4 C 0.8018(13) 0.6439(4) 0.4348(3) 0.041(3) Uani 1 1 d . . . C5 C 0.7488(12) 0.6337(4) 0.3939(3) 0.032(2) Uani 1 1 d . . . C6 C 0.7101(12) 0.5885(4) 0.3797(3) 0.034(3) Uani 1 1 d . . . C7 C 0.6696(12) 0.5747(4) 0.3364(3) 0.039(3) Uani 1 1 d . . . H7 H 0.6712 0.5952 0.3121 0.046 Uiso 1 1 calc R . . C8 C 0.6295(12) 0.5282(4) 0.3368(3) 0.037(3) Uani 1 1 d . . . H8 H 0.5978 0.5098 0.3129 0.045 Uiso 1 1 calc R . . C9 C 0.6431(11) 0.5110(4) 0.3801(3) 0.030(2) Uani 1 1 d . . . C10 C 0.5874(12) 0.4676(4) 0.3953(3) 0.034(3) Uani 1 1 d . . . C11 C 0.5865(12) 0.4533(4) 0.4377(3) 0.035(3) Uani 1 1 d . . . C12 C 0.5148(14) 0.4118(4) 0.4543(4) 0.047(3) Uani 1 1 d . . . H12 H 0.4493 0.3903 0.4394 0.056 Uiso 1 1 calc R . . C13 C 0.5581(13) 0.4088(4) 0.4960(4) 0.047(3) Uani 1 1 d . . . H13 H 0.5270 0.3847 0.5156 0.056 Uiso 1 1 calc R . . C14 C 0.6562(13) 0.4472(4) 0.5048(3) 0.038(3) Uani 1 1 d . . . C15 C 0.7453(13) 0.4516(4) 0.5424(3) 0.039(3) Uani 1 1 d . . . C16 C 0.8369(12) 0.4933(4) 0.5499(3) 0.032(2) Uani 1 1 d . . . C17 C 0.9326(12) 0.4979(4) 0.5869(3) 0.039(3) Uani 1 1 d . . . H17 H 0.9540 0.4743 0.6079 0.047 Uiso 1 1 calc R . . C18 C 0.9853(12) 0.5436(5) 0.5849(3) 0.040(3) Uani 1 1 d . . . H18 H 1.0520 0.5578 0.6053 0.049 Uiso 1 1 calc R . . C19 C 0.9271(12) 0.5678(4) 0.5480(3) 0.038(3) Uani 1 1 d . . . C20 C 0.9427(12) 0.6155(4) 0.5374(3) 0.032(2) Uani 1 1 d . . . C21 C 0.6128(14) 0.7046(4) 0.3636(3) 0.048(3) Uani 1 1 d . . . H21 H 0.5338 0.6998 0.3840 0.058 Uiso 1 1 calc R . . C22 C 0.6004(13) 0.7423(4) 0.3342(3) 0.043(3) Uani 1 1 d . . . H22 H 0.5143 0.7631 0.3360 0.051 Uiso 1 1 calc R . . N5 N 0.7031(9) 0.7504(3) 0.3040(3) 0.031(2) Uani 1 1 d . . . C23 C 0.8249(13) 0.7204(5) 0.3043(4) 0.056(4) Uani 1 1 d . . . H23 H 0.9006 0.7256 0.2831 0.068 Uiso 1 1 calc R . . C24 C 0.8499(14) 0.6838(5) 0.3316(4) 0.055(4) Uani 1 1 d . . . H24 H 0.9399 0.6647 0.3298 0.066 Uiso 1 1 calc R . . C25 C 0.7360(13) 0.6746(4) 0.3635(3) 0.038(3) Uani 1 1 d . . . C26 C 0.5308(13) 0.4312(4) 0.3626(3) 0.039(3) Uani 1 1 d . . . C27 C 0.3738(14) 0.4213(6) 0.3569(4) 0.064(4) Uani 1 1 d . . . H27 H 0.2983 0.4372 0.3736 0.077 Uiso 1 1 calc R . . H28 H 0.6490 0.3580 0.2908 0.077 Uiso 1 1 d R . . H29 H 0.2263 0.3809 0.3215 0.077 Uiso 1 1 d R . . C30 C 0.6307(14) 0.4078(5) 0.3362(4) 0.057(4) Uani 1 1 d . . . H30 H 0.7371 0.4147 0.3376 0.069 Uiso 1 1 calc R . . C31 C 0.7414(12) 0.4151(4) 0.5751(3) 0.038(3) Uani 1 1 d . . . C32 C 0.7016(12) 0.4245(5) 0.6167(3) 0.044(3) Uani 1 1 d . . . H32 H 0.6692 0.4561 0.6239 0.053 Uiso 1 1 calc R . . C33 C 0.7065(14) 0.3901(5) 0.6485(4) 0.055(4) Uani 1 1 d . . . H33 H 0.6781 0.3980 0.6769 0.066 Uiso 1 1 calc R . . C34 C 0.7527(14) 0.3448(6) 0.6385(4) 0.063(4) Uani 1 1 d . . . H34 H 0.7577 0.3208 0.6599 0.076 Uiso 1 1 calc R . . C35 C 0.7925(15) 0.3338(5) 0.5968(4) 0.062(4) Uani 1 1 d . . . H35 H 0.8241 0.3021 0.5899 0.074 Uiso 1 1 calc R . . C36 C 0.7870(13) 0.3684(5) 0.5653(4) 0.049(3) Uani 1 1 d . . . H36 H 0.8145 0.3603 0.5369 0.059 Uiso 1 1 calc R . . C37 C 1.0181(18) 0.6466(6) 0.5704(4) 0.083(2) Uani 1 1 d . . . C38 C 0.9369(18) 0.6619(6) 0.6046(4) 0.083(2) Uani 1 1 d . . . H38 H 0.8329 0.6525 0.6076 0.100 Uiso 1 1 calc R . . C39 C 1.0054(18) 0.6922(6) 0.6366(4) 0.083(2) Uani 1 1 d . . . H39 H 0.9465 0.7030 0.6602 0.100 Uiso 1 1 calc R . . C40 C 1.1469(18) 0.7047(6) 0.6331(4) 0.083(2) Uani 1 1 d . . . H40 H 1.1918 0.7245 0.6544 0.100 Uiso 1 1 calc R . . C41 C 1.2350(18) 0.6896(6) 0.5987(4) 0.083(2) Uani 1 1 d . . . H41 H 1.3393 0.6987 0.5963 0.100 Uiso 1 1 calc R . . C42 C 1.1678(18) 0.6611(6) 0.5682(4) 0.083(2) Uani 1 1 d . . . H42 H 1.2277 0.6510 0.5446 0.100 Uiso 1 1 calc R . . N7 N 1.0082(16) 0.8368(6) 0.2500 0.064(5) Uani 1 2 d SD . . O1 O 0.8717(14) 0.8510(5) 0.2500 0.067(4) Uani 1 2 d SD . . O2 O 1.044(2) 0.7933(6) 0.2500 0.097(6) Uani 1 2 d SD . . O3 O 1.1076(15) 0.8684(6) 0.2500 0.107(6) Uani 1 2 d SD . . N8 N 0.354(6) 0.7582(17) 0.2500 0.108(8) Uani 0.50 2 d SPD . . O4 O 0.392(6) 0.7787(17) 0.2500 0.108(8) Uani 0.50 2 d SP . . O5 O 0.284(3) 0.7371(9) 0.2826(3) 0.108(8) Uani 0.50 1 d PD . . N9 N 0.529(2) 0.1462(7) 0.2500 0.040(3) Uani 0.50 2 d SPD . . O6 O 0.626(2) 0.1794(7) 0.2500 0.040(3) Uani 0.50 2 d SPD . . O7 O 0.397(2) 0.1592(7) 0.2500 0.040(3) Uani 0.50 2 d SPD . . O8 O 0.562(2) 0.1031(7) 0.2500 0.040(3) Uani 0.50 2 d SPD . . C43 C 0.892(4) 0.9659(13) 0.2500 0.0467(12) Uani 0.50 2 d SP . . Cl1 Cl 0.9950(7) 0.9832(2) 0.20346(18) 0.0467(12) Uani 0.50 1 d P . . Cl2 Cl 0.7201(10) 0.9957(3) 0.2500 0.0467(12) Uani 0.50 2 d SP . . C44 C 0.975(3) 0.1115(12) 0.2500 0.033(7) Uani 0.50 2 d SP . . O9 O 0.933(2) 0.1573(8) 0.2500 0.038(5) Uani 0.50 2 d SP . . Cl5 Cl 0.5602(11) 0.7184(4) 0.5386(3) 0.033(2) Uiso 0.25 1 d PD . . Cl4 Cl 0.457(2) 0.7059(7) 0.4637(5) 0.113(7) Uiso 0.25 1 d PD . . C45 C 0.472(2) 0.7500 0.5000 0.093(15) Uiso 0.50 2 d SPD . . Cl6 Cl 0.2790(15) 0.7552(8) 0.5097(6) 0.093(6) Uiso 0.25 1 d PD . . 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 N6 0.033(5) 0.035(6) 0.032(5) 0.000(4) -0.003(4) 0.002(4) C29 0.040(7) 0.059(9) 0.060(8) -0.020(7) -0.009(6) 0.002(7) C28 0.035(7) 0.072(10) 0.049(7) -0.023(7) 0.012(6) -0.018(7) Cd1 0.0341(6) 0.0290(6) 0.0266(5) 0.000 0.000 0.0038(6) Cu2 0.0435(8) 0.0276(7) 0.0255(6) 0.0027(5) 0.0005(6) 0.0055(6) N1 0.053(6) 0.029(5) 0.018(4) -0.002(4) -0.006(4) 0.004(5) N2 0.036(5) 0.033(6) 0.028(4) 0.000(4) -0.001(4) 0.004(4) N3 0.038(5) 0.030(5) 0.031(4) 0.007(4) 0.010(4) 0.011(4) N4 0.038(5) 0.030(5) 0.030(4) 0.005(4) 0.001(4) 0.000(4) C1 0.043(6) 0.029(6) 0.031(6) 0.004(5) 0.001(5) 0.005(5) C2 0.089(9) 0.026(7) 0.035(6) 0.000(5) -0.009(6) 0.008(6) C3 0.068(8) 0.034(7) 0.038(6) 0.001(5) -0.016(6) 0.009(7) C4 0.060(7) 0.028(7) 0.036(6) -0.002(5) -0.002(5) 0.008(6) C5 0.042(6) 0.036(6) 0.017(4) -0.003(4) -0.004(4) -0.005(6) C6 0.036(6) 0.035(7) 0.029(5) 0.002(5) -0.006(4) -0.003(5) C7 0.049(7) 0.040(7) 0.026(5) 0.002(5) 0.001(5) 0.001(6) C8 0.053(7) 0.039(7) 0.020(5) -0.003(5) 0.006(5) -0.001(6) C9 0.034(6) 0.028(6) 0.030(5) -0.002(4) 0.000(5) 0.006(5) C10 0.033(6) 0.034(7) 0.035(6) 0.003(5) 0.005(5) 0.006(5) C11 0.042(6) 0.034(7) 0.030(5) 0.001(5) 0.002(5) 0.004(5) C12 0.060(8) 0.037(8) 0.044(7) 0.011(5) 0.004(6) -0.001(6) C13 0.052(8) 0.034(8) 0.054(7) 0.005(6) 0.017(6) 0.004(6) C14 0.044(7) 0.036(7) 0.033(6) -0.002(5) 0.011(5) 0.009(6) C15 0.045(7) 0.046(8) 0.024(5) 0.006(5) 0.006(5) 0.014(6) C16 0.040(6) 0.032(6) 0.024(5) 0.000(4) 0.002(5) 0.013(6) C17 0.040(7) 0.040(8) 0.036(6) 0.005(5) 0.003(5) 0.013(6) C18 0.035(6) 0.059(9) 0.028(5) -0.002(5) 0.000(5) 0.019(6) C19 0.043(7) 0.049(8) 0.021(5) 0.001(5) 0.001(5) 0.011(6) C20 0.045(7) 0.025(6) 0.026(5) 0.000(4) 0.002(5) 0.002(5) C21 0.054(8) 0.049(9) 0.042(7) 0.019(6) 0.017(6) 0.017(6) C22 0.045(7) 0.047(8) 0.036(6) 0.011(5) 0.012(5) 0.008(6) N5 0.036(5) 0.028(5) 0.030(5) 0.005(4) -0.006(4) 0.000(4) C23 0.044(8) 0.071(10) 0.054(7) 0.028(7) 0.023(6) 0.028(7) C24 0.060(8) 0.063(10) 0.042(6) 0.019(6) 0.011(6) 0.027(7) C25 0.059(7) 0.031(6) 0.025(5) -0.002(5) -0.002(5) -0.001(6) C26 0.057(8) 0.024(7) 0.035(6) 0.005(5) -0.005(5) -0.004(6) C27 0.041(8) 0.085(12) 0.068(9) -0.021(8) -0.002(6) 0.017(8) C30 0.048(8) 0.070(10) 0.054(8) -0.026(7) 0.008(6) -0.014(7) C31 0.046(7) 0.032(7) 0.035(6) 0.009(5) 0.007(5) 0.011(6) C32 0.046(7) 0.046(8) 0.039(6) 0.013(6) 0.011(5) 0.009(6) C33 0.060(8) 0.071(11) 0.035(6) 0.017(7) 0.011(6) 0.015(8) C34 0.055(9) 0.072(11) 0.063(9) 0.040(8) 0.004(7) -0.014(8) C35 0.081(10) 0.043(9) 0.061(9) 0.015(7) 0.011(7) 0.010(7) C36 0.054(8) 0.044(8) 0.049(7) 0.009(6) 0.001(6) 0.005(6) C37 0.088(5) 0.105(6) 0.057(4) -0.043(4) 0.000(4) -0.012(5) C38 0.088(5) 0.105(6) 0.057(4) -0.043(4) 0.000(4) -0.012(5) C39 0.088(5) 0.105(6) 0.057(4) -0.043(4) 0.000(4) -0.012(5) C40 0.088(5) 0.105(6) 0.057(4) -0.043(4) 0.000(4) -0.012(5) C41 0.088(5) 0.105(6) 0.057(4) -0.043(4) 0.000(4) -0.012(5) C42 0.088(5) 0.105(6) 0.057(4) -0.043(4) 0.000(4) -0.012(5) N7 0.033(9) 0.098(17) 0.060(10) 0.000 0.000 -0.023(11) O1 0.054(8) 0.093(12) 0.056(8) 0.000 0.000 -0.033(8) O2 0.147(16) 0.047(11) 0.096(12) 0.000 0.000 -0.027(11) O3 0.040(8) 0.067(12) 0.21(2) 0.000 0.000 -0.026(8) N8 0.138(18) 0.12(2) 0.065(9) 0.000 0.000 0.103(15) O4 0.138(18) 0.12(2) 0.065(9) 0.000 0.000 0.103(15) O5 0.138(18) 0.12(2) 0.065(9) 0.000 0.000 0.103(15) N9 0.057(7) 0.026(6) 0.038(6) 0.000 0.000 -0.001(6) O6 0.057(7) 0.026(6) 0.038(6) 0.000 0.000 -0.001(6) O7 0.057(7) 0.026(6) 0.038(6) 0.000 0.000 -0.001(6) O8 0.057(7) 0.026(6) 0.038(6) 0.000 0.000 -0.001(6) C43 0.057(3) 0.039(3) 0.044(3) 0.000 0.000 0.004(2) Cl1 0.057(3) 0.039(3) 0.044(3) 0.000 0.000 0.004(2) Cl2 0.057(3) 0.039(3) 0.044(3) 0.000 0.000 0.004(2) C44 0.022(15) 0.04(2) 0.042(17) 0.000 0.000 -0.016(15) O9 0.048(13) 0.043(15) 0.024(10) 0.000 0.000 0.000(12) _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 N6 C28 1.325(13) . ? N6 C29 1.341(14) . ? N6 Cd1 2.373(8) 3_645 ? C29 C27 1.404(17) . ? C29 H29 0.9539 . ? C28 C30 1.365(16) . ? C28 H28 0.9471 . ? Cd1 O1 2.307(12) . ? Cd1 N5 2.340(8) 6_556 ? Cd1 N5 2.340(8) . ? Cd1 N6 2.373(8) 8_665 ? Cd1 N6 2.373(8) 3_655 ? Cd1 O4 2.38(5) . ? Cu2 N3 1.971(9) . ? Cu2 N4 1.976(8) . ? Cu2 N2 1.978(8) . ? Cu2 N1 1.985(9) . ? N1 C4 1.373(13) . ? N1 C1 1.375(13) . ? N2 C9 1.388(13) . ? N2 C6 1.416(13) . ? N3 C14 1.392(13) . ? N3 C11 1.393(13) . ? N4 C16 1.376(13) . ? N4 C19 1.407(14) . ? C1 C20 1.387(13) . ? C1 C2 1.437(15) . ? C2 C3 1.365(14) . ? C2 H2 0.9500 . ? C3 C4 1.434(16) . ? C3 H3 0.9500 . ? C4 C5 1.395(13) . ? C5 C6 1.376(14) . ? C5 C25 1.485(14) . ? C6 C7 1.455(13) . ? C7 C8 1.339(15) . ? C7 H7 0.9500 . ? C8 C9 1.446(13) . ? C8 H8 0.9500 . ? C9 C10 1.383(14) . ? C10 C11 1.390(14) . ? C10 C26 1.523(15) . ? C11 C12 1.410(15) . ? C12 C13 1.364(15) . ? C12 H12 0.9500 . ? C13 C14 1.395(16) . ? C13 H13 0.9500 . ? C14 C15 1.420(14) . ? C15 C16 1.430(15) . ? C15 C31 1.442(14) . ? C16 C17 1.436(14) . ? C17 C18 1.352(15) . ? C17 H17 0.9500 . ? C18 C19 1.431(14) . ? C18 H18 0.9500 . ? C19 C20 1.375(15) . ? C20 C37 1.500(16) . ? C21 C25 1.362(16) . ? C21 C22 1.402(15) . ? C21 H21 0.9500 . ? C22 N5 1.323(13) . ? C22 H22 0.9500 . ? N5 C23 1.353(13) . ? C23 C24 1.347(16) . ? C23 H23 0.9500 . ? C24 C25 1.435(15) . ? C24 H24 0.9500 . ? C26 C30 1.367(16) . ? C26 C27 1.411(16) . ? C27 H27 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.377(14) . ? C31 C36 1.391(16) . ? C32 C33 1.382(15) . ? C32 H32 0.9500 . ? C33 C34 1.358(18) . ? C33 H33 0.9500 . ? C34 C35 1.386(18) . ? C34 H34 0.9500 . ? C35 C36 1.379(16) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.357(18) . ? C37 C42 1.371(19) . ? C38 C39 1.440(18) . ? C38 H38 0.9500 . ? C39 C40 1.289(19) . ? C39 H39 0.9500 . ? C40 C41 1.393(19) . ? C40 H40 0.9500 . ? C41 C42 1.372(18) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? N7 O3 1.235(14) . ? N7 O2 1.248(15) . ? N7 O1 1.257(14) . ? N8 O4 0.66(7) . ? N8 O5 1.328(19) 6_556 ? N8 O5 1.328(19) . ? O4 O5 1.81(5) 6_556 ? O4 O5 1.81(5) . ? N9 O7 1.208(17) . ? N9 O8 1.233(17) . ? N9 O6 1.253(17) . ? C43 Cl2 1.72(3) . ? C43 Cl1 1.78(2) 6_556 ? C43 Cl1 1.78(2) . ? C44 O9 1.33(4) . ? Cl5 C45 1.682(11) . ? Cl5 Cl4 2.29(2) 4_566 ? Cl4 C45 1.677(13) . ? Cl4 Cl6 2.07(3) 4_566 ? Cl4 Cl5 2.29(2) 4_566 ? C45 Cl4 1.677(13) 4_566 ? C45 Cl5 1.682(11) 4_566 ? C45 Cl6 1.720(18) 4_566 ? C45 Cl6 1.720(18) . ? Cl6 Cl6 0.68(3) 4_566 ? Cl6 Cl4 2.07(3) 4_566 ? 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 C28 N6 C29 114.2(10) . . ? C28 N6 Cd1 123.6(7) . 3_645 ? C29 N6 Cd1 122.1(7) . 3_645 ? N6 C29 C27 124.6(11) . . ? N6 C29 H29 116.9 . . ? C27 C29 H29 118.5 . . ? N6 C28 C30 126.4(11) . . ? N6 C28 H28 115.7 . . ? C30 C28 H28 117.8 . . ? O1 Cd1 N5 101.0(3) . 6_556 ? O1 Cd1 N5 101.0(3) . . ? N5 Cd1 N5 92.9(4) 6_556 . ? O1 Cd1 N6 83.9(3) . 8_665 ? N5 Cd1 N6 173.7(3) 6_556 8_665 ? N5 Cd1 N6 90.1(3) . 8_665 ? O1 Cd1 N6 83.9(3) . 3_655 ? N5 Cd1 N6 90.1(3) 6_556 3_655 ? N5 Cd1 N6 173.7(3) . 3_655 ? N6 Cd1 N6 86.5(4) 8_665 3_655 ? O1 Cd1 O4 165.7(12) . . ? N5 Cd1 O4 88.8(8) 6_556 . ? N5 Cd1 O4 88.8(8) . . ? N6 Cd1 O4 85.8(9) 8_665 . ? N6 Cd1 O4 85.8(9) 3_655 . ? N3 Cu2 N4 90.0(3) . . ? N3 Cu2 N2 90.1(4) . . ? N4 Cu2 N2 173.7(3) . . ? N3 Cu2 N1 173.4(3) . . ? N4 Cu2 N1 90.5(3) . . ? N2 Cu2 N1 90.1(3) . . ? C4 N1 C1 105.6(9) . . ? C4 N1 Cu2 127.5(7) . . ? C1 N1 Cu2 126.6(7) . . ? C9 N2 C6 105.5(8) . . ? C9 N2 Cu2 127.2(7) . . ? C6 N2 Cu2 127.2(7) . . ? C14 N3 C11 104.2(9) . . ? C14 N3 Cu2 127.8(7) . . ? C11 N3 Cu2 127.7(7) . . ? C16 N4 C19 105.4(8) . . ? C16 N4 Cu2 127.8(7) . . ? C19 N4 Cu2 126.5(7) . . ? N1 C1 C20 125.8(10) . . ? N1 C1 C2 110.7(9) . . ? C20 C1 C2 123.2(10) . . ? C3 C2 C1 106.2(10) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? C2 C3 C4 107.2(10) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 125.2(10) . . ? N1 C4 C3 110.3(9) . . ? C5 C4 C3 124.4(10) . . ? C6 C5 C4 124.4(10) . . ? C6 C5 C25 118.2(9) . . ? C4 C5 C25 117.4(10) . . ? C5 C6 N2 124.3(9) . . ? C5 C6 C7 127.0(10) . . ? N2 C6 C7 108.7(9) . . ? C8 C7 C6 107.9(9) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? C7 C8 C9 108.0(9) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? C10 C9 N2 123.6(9) . . ? C10 C9 C8 125.7(10) . . ? N2 C9 C8 109.9(9) . . ? C9 C10 C11 125.5(10) . . ? C9 C10 C26 117.4(9) . . ? C11 C10 C26 116.9(10) . . ? C10 C11 N3 123.0(10) . . ? C10 C11 C12 126.2(11) . . ? N3 C11 C12 110.7(9) . . ? C13 C12 C11 106.3(11) . . ? C13 C12 H12 126.9 . . ? C11 C12 H12 126.8 . . ? C12 C13 C14 108.2(11) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? N3 C14 C13 110.2(10) . . ? N3 C14 C15 124.8(11) . . ? C13 C14 C15 124.6(11) . . ? C14 C15 C16 120.9(10) . . ? C14 C15 C31 121.1(11) . . ? C16 C15 C31 117.9(9) . . ? N4 C16 C15 125.7(9) . . ? N4 C16 C17 112.1(10) . . ? C15 C16 C17 122.1(10) . . ? C18 C17 C16 104.2(10) . . ? C18 C17 H17 127.9 . . ? C16 C17 H17 127.9 . . ? C17 C18 C19 110.9(10) . . ? C17 C18 H18 124.6 . . ? C19 C18 H18 124.6 . . ? C20 C19 N4 124.7(9) . . ? C20 C19 C18 127.8(11) . . ? N4 C19 C18 107.3(10) . . ? C19 C20 C1 123.9(10) . . ? C19 C20 C37 115.6(11) . . ? C1 C20 C37 120.5(11) . . ? C25 C21 C22 121.2(10) . . ? C25 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? N5 C22 C21 123.0(11) . . ? N5 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C22 N5 C23 115.1(9) . . ? C22 N5 Cd1 119.7(7) . . ? C23 N5 Cd1 124.6(7) . . ? C24 C23 N5 126.7(11) . . ? C24 C23 H23 116.7 . . ? N5 C23 H23 116.7 . . ? C23 C24 C25 117.8(11) . . ? C23 C24 H24 121.1 . . ? C25 C24 H24 121.1 . . ? C21 C25 C24 116.1(10) . . ? C21 C25 C5 121.8(10) . . ? C24 C25 C5 122.1(10) . . ? C30 C26 C27 116.8(11) . . ? C30 C26 C10 121.1(10) . . ? C27 C26 C10 122.1(10) . . ? C29 C27 C26 118.0(11) . . ? C29 C27 H27 121.0 . . ? C26 C27 H27 121.0 . . ? C28 C30 C26 119.7(11) . . ? C28 C30 H30 120.1 . . ? C26 C30 H30 120.1 . . ? C32 C31 C36 117.2(10) . . ? C32 C31 C15 123.1(11) . . ? C36 C31 C15 119.6(10) . . ? C31 C32 C33 123.1(12) . . ? C31 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C34 C33 C32 118.8(12) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C33 C34 C35 119.8(12) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 120.9(14) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C31 120.1(12) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C38 C37 C42 116.5(14) . . ? C38 C37 C20 119.8(14) . . ? C42 C37 C20 123.7(12) . . ? C37 C38 C39 121.2(15) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 119.8(14) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 121.0(14) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C42 C41 C40 118.6(15) . . ? C42 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? C37 C42 C41 123.0(14) . . ? C37 C42 H42 118.5 . . ? C41 C42 H42 118.5 . . ? O3 N7 O2 120.9(16) . . ? O3 N7 O1 116.4(16) . . ? O2 N7 O1 122.7(17) . . ? N7 O1 Cd1 128.9(12) . . ? O4 N8 O5 128(3) . 6_556 ? O4 N8 O5 128(3) . . ? O5 N8 O5 101(2) 6_556 . ? O5 O4 O5 69(2) 6_556 . ? N8 O4 Cd1 139(10) . . ? O5 O4 Cd1 134.2(19) 6_556 . ? O5 O4 Cd1 134.2(19) . . ? O7 N9 O8 121(2) . . ? O7 N9 O6 115(2) . . ? O8 N9 O6 124(2) . . ? Cl2 C43 Cl1 108.1(13) . 6_556 ? Cl2 C43 Cl1 108.1(13) . . ? Cl1 C43 Cl1 110.3(19) 6_556 . ? C45 Cl5 Cl4 46.9(4) . 4_566 ? C45 Cl4 Cl6 53.5(9) . 4_566 ? C45 Cl4 Cl5 47.1(6) . 4_566 ? Cl6 Cl4 Cl5 80.2(8) 4_566 4_566 ? Cl4 C45 Cl4 170.9(18) 4_566 . ? Cl4 C45 Cl5 86.0(8) 4_566 . ? Cl4 C45 Cl5 98.2(7) . . ? Cl4 C45 Cl5 98.2(7) 4_566 4_566 ? Cl4 C45 Cl5 86.0(8) . 4_566 ? Cl5 C45 Cl5 125.4(14) . 4_566 ? Cl4 C45 Cl6 96.0(11) 4_566 4_566 ? Cl4 C45 Cl6 74.9(11) . 4_566 ? Cl5 C45 Cl6 122.2(11) . 4_566 ? Cl5 C45 Cl6 111.5(9) 4_566 4_566 ? Cl4 C45 Cl6 74.9(11) 4_566 . ? Cl4 C45 Cl6 96.0(11) . . ? Cl5 C45 Cl6 111.5(9) . . ? Cl5 C45 Cl6 122.2(11) 4_566 . ? Cl6 Cl6 C45 78.6(6) 4_566 . ? Cl6 Cl6 Cl4 126.0(18) 4_566 4_566 ? C45 Cl6 Cl4 51.6(6) . 4_566 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.017 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.211 # Attachment '1-CdBr2.cif' data_e401b _database_code_depnum_ccdc_archive 'CCDC 659598' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H56 Br2 Cd N12, 4(C H Cl3)' _chemical_formula_sum 'C88 H60 Br2 Cd Cl12 N12' _chemical_formula_weight 1983.10 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4956(4) _cell_length_b 14.4774(6) _cell_length_c 16.5058(6) _cell_angle_alpha 82.058(2) _cell_angle_beta 79.919(2) _cell_angle_gamma 74.550(2) _cell_volume 2143.27(15) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7953 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 994 _exptl_absorpt_coefficient_mu 1.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6179 _exptl_absorpt_correction_T_max 0.7938 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38653 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 30.01 _reflns_number_total 12431 _reflns_number_gt 10312 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12431 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1648 _refine_ls_wR_factor_gt 0.1565 _refine_ls_goodness_of_fit_ref 1.234 _refine_ls_restrained_S_all 1.234 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.5000 1.0000 0.5000 0.01583(8) Uani 1 2 d S . . Br1 Br -0.31179(3) 0.937897(19) 0.616849(16) 0.02171(9) Uani 1 1 d . . . N1 N 0.0468(2) 0.60083(16) 0.13637(13) 0.0182(4) Uani 1 1 d . . . H1A H 0.0343 0.5431 0.1346 0.022 Uiso 1 1 calc R . . N2 N -0.0886(2) 0.46705(16) 0.25425(13) 0.0172(4) Uani 1 1 d . . . N3 N 0.0663(2) 0.30591(16) 0.15881(13) 0.0180(4) Uani 1 1 d . . . H3A H 0.0532 0.3688 0.1518 0.022 Uiso 1 1 calc R . . N4 N 0.1867(2) 0.44154(16) 0.03677(13) 0.0178(4) Uani 1 1 d . . . C1 C 0.1373(3) 0.64481(19) 0.07847(16) 0.0193(5) Uani 1 1 d . . . C2 C 0.1303(3) 0.7353(2) 0.10676(17) 0.0229(5) Uani 1 1 d . . . H2 H 0.1833 0.7808 0.0799 0.028 Uiso 1 1 calc R . . C3 C 0.0344(3) 0.7450(2) 0.17888(17) 0.0235(5) Uani 1 1 d . . . H3 H 0.0092 0.7982 0.2110 0.028 Uiso 1 1 calc R . . C4 C -0.0213(3) 0.66044(19) 0.19743(16) 0.0191(5) Uani 1 1 d . . . C5 C -0.1231(3) 0.64006(19) 0.26670(16) 0.0188(5) Uani 1 1 d . . . C6 C -0.1576(3) 0.55039(19) 0.29081(16) 0.0188(5) Uani 1 1 d . . . C7 C -0.2672(3) 0.5329(2) 0.36039(18) 0.0258(6) Uani 1 1 d . . . H7 H -0.3302 0.5793 0.3947 0.031 Uiso 1 1 calc R . . C8 C -0.2624(3) 0.4387(2) 0.36691(18) 0.0263(6) Uani 1 1 d . . . H8 H -0.3209 0.4055 0.4069 0.032 Uiso 1 1 calc R . . C9 C -0.1494(3) 0.39694(19) 0.30035(16) 0.0186(5) Uani 1 1 d . . . C10 C -0.1057(3) 0.29850(18) 0.28890(15) 0.0170(4) Uani 1 1 d . . . C11 C 0.0015(3) 0.25643(19) 0.22581(16) 0.0182(5) Uani 1 1 d . . . C12 C 0.0573(3) 0.1558(2) 0.21492(17) 0.0217(5) Uani 1 1 d . . . H12 H 0.0336 0.1040 0.2519 0.026 Uiso 1 1 calc R . . C13 C 0.1514(3) 0.1481(2) 0.14122(17) 0.0230(5) Uani 1 1 d . . . H13 H 0.2050 0.0898 0.1187 0.028 Uiso 1 1 calc R . . C14 C 0.1542(3) 0.24315(19) 0.10453(16) 0.0184(5) Uani 1 1 d . . . C15 C 0.2279(3) 0.26778(19) 0.02638(16) 0.0192(5) Uani 1 1 d . . . C16 C 0.2351(3) 0.36220(19) -0.00670(16) 0.0181(5) Uani 1 1 d . . . C17 C 0.3037(3) 0.3864(2) -0.09018(16) 0.0220(5) Uani 1 1 d . . . H17 H 0.3428 0.3441 -0.1323 0.026 Uiso 1 1 calc R . . C18 C 0.3008(3) 0.4810(2) -0.09584(16) 0.0212(5) Uani 1 1 d . . . H18 H 0.3374 0.5183 -0.1428 0.025 Uiso 1 1 calc R . . C19 C 0.2307(3) 0.51415(19) -0.01589(15) 0.0171(5) Uani 1 1 d . . . C20 C 0.2178(3) 0.60753(19) 0.00526(16) 0.0182(5) Uani 1 1 d . . . C21 C -0.1989(3) 0.72167(19) 0.31834(16) 0.0189(5) Uani 1 1 d . . . C22 C -0.1866(3) 0.7164(2) 0.40193(17) 0.0232(5) Uani 1 1 d . . . H22 H -0.1273 0.6604 0.4278 0.028 Uiso 1 1 calc R . . C23 C -0.2615(3) 0.7935(2) 0.44705(17) 0.0226(5) Uani 1 1 d . . . H23 H -0.2512 0.7887 0.5038 0.027 Uiso 1 1 calc R . . N5 N -0.3478(3) 0.87440(16) 0.41447(14) 0.0210(4) Uani 1 1 d . . . C24 C -0.3584(3) 0.8797(2) 0.33356(17) 0.0259(6) Uani 1 1 d . . . H24 H -0.4177 0.9367 0.3091 0.031 Uiso 1 1 calc R . . C25 C -0.2870(3) 0.8059(2) 0.28412(17) 0.0250(6) Uani 1 1 d . . . H25 H -0.2982 0.8129 0.2273 0.030 Uiso 1 1 calc R . . C26 C -0.1884(3) 0.23287(19) 0.34363(15) 0.0178(5) Uani 1 1 d . . . C27 C -0.1215(3) 0.1516(2) 0.39218(16) 0.0214(5) Uani 1 1 d . . . H27 H -0.0191 0.1381 0.3957 0.026 Uiso 1 1 calc R . . C28 C -0.2059(3) 0.0906(2) 0.43534(17) 0.0211(5) Uani 1 1 d . . . H28 H -0.1587 0.0357 0.4682 0.025 Uiso 1 1 calc R . . N6 N -0.3510(2) 0.10564(17) 0.43282(14) 0.0201(4) Uani 1 1 d . . . C29 C -0.4160(3) 0.1852(2) 0.38770(17) 0.0212(5) Uani 1 1 d . . . H29 H -0.5192 0.1979 0.3868 0.025 Uiso 1 1 calc R . . C30 C -0.3403(3) 0.24941(19) 0.34250(16) 0.0196(5) Uani 1 1 d . . . H30 H -0.3910 0.3043 0.3110 0.023 Uiso 1 1 calc R . . C31 C 0.3105(3) 0.1859(2) -0.02355(16) 0.0222(5) Uani 1 1 d . . . C32 C 0.4649(3) 0.1683(2) -0.04425(19) 0.0293(6) Uani 1 1 d . . . H32 H 0.5164 0.2092 -0.0282 0.035 Uiso 1 1 calc R . . C33 C 0.5420(4) 0.0898(2) -0.0888(2) 0.0374(8) Uani 1 1 d . . . H33 H 0.6462 0.0775 -0.1028 0.045 Uiso 1 1 calc R . . C34 C 0.4688(5) 0.0304(2) -0.1124(2) 0.0410(9) Uani 1 1 d . . . H34 H 0.5219 -0.0223 -0.1428 0.049 Uiso 1 1 calc R . . C35 C 0.3182(5) 0.0476(2) -0.0917(2) 0.0384(8) Uani 1 1 d . . . H35 H 0.2679 0.0061 -0.1078 0.046 Uiso 1 1 calc R . . C36 C 0.2380(4) 0.1249(2) -0.04760(19) 0.0296(6) Uani 1 1 d . . . H36 H 0.1338 0.1359 -0.0340 0.036 Uiso 1 1 calc R . . C37 C 0.2968(3) 0.67120(19) -0.05389(15) 0.0191(5) Uani 1 1 d . . . C38 C 0.4498(3) 0.6418(2) -0.07769(17) 0.0232(5) Uani 1 1 d . . . H38 H 0.5040 0.5820 -0.0543 0.028 Uiso 1 1 calc R . . C39 C 0.5233(3) 0.6991(3) -0.13515(18) 0.0299(7) Uani 1 1 d . . . H39 H 0.6269 0.6780 -0.1510 0.036 Uiso 1 1 calc R . . C40 C 0.4461(4) 0.7870(2) -0.16946(18) 0.0309(7) Uani 1 1 d . . . H40 H 0.4966 0.8263 -0.2083 0.037 Uiso 1 1 calc R . . C41 C 0.2942(4) 0.8170(2) -0.14646(19) 0.0302(6) Uani 1 1 d . . . H41 H 0.2406 0.8767 -0.1702 0.036 Uiso 1 1 calc R . . C42 C 0.2205(3) 0.7604(2) -0.08918(18) 0.0242(5) Uani 1 1 d . . . H42 H 0.1169 0.7821 -0.0735 0.029 Uiso 1 1 calc R . . C43 C 0.2151(4) 0.4642(3) 0.3283(2) 0.0408(8) Uani 1 1 d . . . H43 H 0.1262 0.4946 0.3004 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.1808(2) 0.50534(13) 0.42616(10) 0.0976(6) Uani 1 1 d . . . Cl2 Cl 0.36673(15) 0.50000(10) 0.26731(10) 0.0753(4) Uani 1 1 d . . . Cl3 Cl 0.24023(10) 0.33879(7) 0.33558(6) 0.0436(2) Uani 1 1 d . . . C44 C 0.7238(6) 0.1824(4) 0.6337(3) 0.0556(12) Uani 1 1 d . . . H44 H 0.6981 0.1222 0.6248 0.067 Uiso 1 1 calc R . . Cl4 Cl 0.6293(2) 0.27796(11) 0.56836(9) 0.0801(4) Uani 1 1 d . . . Cl5 Cl 0.91380(18) 0.1631(2) 0.61170(11) 0.1128(8) Uani 1 1 d . . . Cl6 Cl 0.6607(2) 0.2043(2) 0.73632(8) 0.1244(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01538(13) 0.01436(13) 0.01723(13) -0.00113(9) 0.00093(9) -0.00508(9) Br1 0.02035(14) 0.02229(15) 0.02301(14) -0.00106(10) -0.00529(10) -0.00538(10) N1 0.0185(10) 0.0175(10) 0.0184(9) -0.0025(8) 0.0013(8) -0.0062(8) N2 0.0163(9) 0.0152(10) 0.0190(9) -0.0012(8) 0.0008(7) -0.0042(8) N3 0.0180(10) 0.0168(10) 0.0179(9) -0.0018(8) 0.0031(7) -0.0057(8) N4 0.0183(10) 0.0168(10) 0.0170(9) -0.0012(8) 0.0012(7) -0.0048(8) C1 0.0175(11) 0.0201(12) 0.0195(11) -0.0011(9) 0.0019(9) -0.0069(9) C2 0.0242(13) 0.0202(13) 0.0255(12) -0.0050(10) 0.0024(10) -0.0098(10) C3 0.0252(13) 0.0212(13) 0.0254(13) -0.0070(10) 0.0027(10) -0.0097(10) C4 0.0205(12) 0.0166(11) 0.0187(11) -0.0027(9) 0.0002(9) -0.0038(9) C5 0.0185(11) 0.0178(12) 0.0195(11) -0.0044(9) 0.0006(9) -0.0042(9) C6 0.0175(11) 0.0198(12) 0.0181(11) -0.0037(9) 0.0015(9) -0.0047(9) C7 0.0249(13) 0.0257(14) 0.0256(13) -0.0109(11) 0.0101(10) -0.0087(11) C8 0.0267(13) 0.0259(14) 0.0250(13) -0.0061(11) 0.0105(10) -0.0119(11) C9 0.0174(11) 0.0190(12) 0.0193(11) -0.0032(9) 0.0026(9) -0.0070(9) C10 0.0155(10) 0.0172(11) 0.0180(11) -0.0010(9) 0.0012(8) -0.0062(9) C11 0.0151(10) 0.0189(12) 0.0195(11) -0.0012(9) 0.0007(9) -0.0045(9) C12 0.0232(12) 0.0179(12) 0.0218(12) 0.0012(10) 0.0005(10) -0.0053(10) C13 0.0229(12) 0.0181(12) 0.0234(12) -0.0022(10) 0.0027(10) -0.0008(10) C14 0.0162(11) 0.0175(12) 0.0206(11) -0.0040(9) 0.0019(9) -0.0045(9) C15 0.0181(11) 0.0205(12) 0.0184(11) -0.0038(9) 0.0006(9) -0.0045(9) C16 0.0161(11) 0.0196(12) 0.0185(11) -0.0030(9) -0.0006(9) -0.0048(9) C17 0.0252(13) 0.0230(13) 0.0171(11) -0.0050(10) 0.0014(9) -0.0062(10) C18 0.0229(12) 0.0247(13) 0.0158(11) -0.0016(10) 0.0001(9) -0.0077(10) C19 0.0152(10) 0.0193(12) 0.0172(10) -0.0012(9) 0.0006(8) -0.0072(9) C20 0.0153(11) 0.0187(12) 0.0191(11) -0.0012(9) 0.0003(9) -0.0039(9) C21 0.0185(11) 0.0178(12) 0.0193(11) -0.0041(9) 0.0024(9) -0.0045(9) C22 0.0270(13) 0.0173(12) 0.0217(12) -0.0032(10) -0.0028(10) 0.0009(10) C23 0.0264(13) 0.0195(12) 0.0206(12) -0.0044(10) -0.0026(10) -0.0027(10) N5 0.0234(11) 0.0175(10) 0.0195(10) -0.0050(8) 0.0027(8) -0.0031(8) C24 0.0303(14) 0.0209(13) 0.0213(12) -0.0027(10) -0.0007(10) 0.0008(11) C25 0.0277(14) 0.0235(13) 0.0199(12) -0.0034(10) -0.0009(10) -0.0009(11) C26 0.0184(11) 0.0185(12) 0.0168(10) -0.0018(9) 0.0006(8) -0.0073(9) C27 0.0164(11) 0.0249(13) 0.0213(11) 0.0017(10) -0.0004(9) -0.0057(10) C28 0.0176(11) 0.0203(12) 0.0227(12) 0.0037(10) -0.0019(9) -0.0039(9) N6 0.0171(10) 0.0198(11) 0.0226(10) 0.0001(8) 0.0009(8) -0.0069(8) C29 0.0162(11) 0.0189(12) 0.0272(13) 0.0009(10) -0.0013(9) -0.0051(9) C30 0.0183(11) 0.0169(12) 0.0230(12) 0.0011(9) -0.0010(9) -0.0063(9) C31 0.0280(13) 0.0182(12) 0.0172(11) -0.0024(9) 0.0018(9) -0.0027(10) C32 0.0273(14) 0.0267(15) 0.0272(14) -0.0032(11) 0.0066(11) -0.0018(11) C33 0.0374(17) 0.0294(16) 0.0323(16) -0.0043(13) 0.0104(13) 0.0047(13) C34 0.062(2) 0.0225(15) 0.0266(15) -0.0074(12) 0.0015(14) 0.0079(15) C35 0.058(2) 0.0254(15) 0.0307(16) -0.0069(13) -0.0091(15) -0.0048(15) C36 0.0391(17) 0.0221(14) 0.0272(14) -0.0047(11) -0.0050(12) -0.0056(12) C37 0.0208(12) 0.0210(12) 0.0169(11) -0.0026(9) 0.0000(9) -0.0090(10) C38 0.0209(12) 0.0287(14) 0.0202(12) -0.0031(10) -0.0006(9) -0.0075(11) C39 0.0251(14) 0.0488(19) 0.0223(13) -0.0067(13) 0.0011(10) -0.0215(13) C40 0.0431(17) 0.0391(17) 0.0197(12) -0.0007(12) -0.0016(11) -0.0291(15) C41 0.0453(18) 0.0242(14) 0.0259(13) 0.0021(11) -0.0081(12) -0.0170(13) C42 0.0258(13) 0.0220(13) 0.0255(13) -0.0025(10) -0.0025(10) -0.0081(11) C43 0.0282(16) 0.045(2) 0.0441(19) -0.0001(16) -0.0070(14) -0.0010(14) Cl1 0.1459(17) 0.0771(10) 0.0575(8) -0.0261(7) 0.0142(9) -0.0154(10) Cl2 0.0602(7) 0.0594(7) 0.1013(10) -0.0141(7) 0.0225(7) -0.0250(6) Cl3 0.0391(4) 0.0442(5) 0.0449(5) 0.0032(4) -0.0121(4) -0.0059(4) C44 0.072(3) 0.068(3) 0.042(2) 0.003(2) -0.011(2) -0.047(3) Cl4 0.1106(12) 0.0588(8) 0.0559(7) -0.0029(6) 0.0065(7) -0.0082(7) Cl5 0.0617(8) 0.212(2) 0.0897(11) -0.0656(14) -0.0016(8) -0.0576(12) Cl6 0.0877(11) 0.280(3) 0.0317(5) -0.0071(10) 0.0005(6) -0.1013(15) _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 Cd1 N6 2.388(2) 2_466 ? Cd1 N6 2.388(2) 1_565 ? Cd1 N5 2.446(2) . ? Cd1 N5 2.446(2) 2_476 ? Cd1 Br1 2.7557(3) . ? Cd1 Br1 2.7557(3) 2_476 ? N1 C4 1.376(3) . ? N1 C1 1.376(3) . ? N1 H1A 0.8800 . ? N2 C9 1.374(3) . ? N2 C6 1.375(3) . ? N3 C14 1.373(3) . ? N3 C11 1.375(3) . ? N3 H3A 0.8800 . ? N4 C16 1.370(3) . ? N4 C19 1.374(3) . ? C1 C20 1.405(3) . ? C1 C2 1.432(4) . ? C2 C3 1.365(4) . ? C2 H2 0.9500 . ? C3 C4 1.434(4) . ? C3 H3 0.9500 . ? C4 C5 1.414(3) . ? C5 C6 1.410(4) . ? C5 C21 1.500(4) . ? C6 C7 1.452(4) . ? C7 C8 1.342(4) . ? C7 H7 0.9500 . ? C8 C9 1.466(4) . ? C8 H8 0.9500 . ? C9 C10 1.404(4) . ? C10 C11 1.402(3) . ? C10 C26 1.499(3) . ? C11 C12 1.436(4) . ? C12 C13 1.376(4) . ? C12 H12 0.9500 . ? C13 C14 1.430(4) . ? C13 H13 0.9500 . ? C14 C15 1.404(3) . ? C15 C16 1.415(4) . ? C15 C31 1.500(4) . ? C16 C17 1.456(3) . ? C17 C18 1.353(4) . ? C17 H17 0.9500 . ? C18 C19 1.453(3) . ? C18 H18 0.9500 . ? C19 C20 1.411(4) . ? C20 C37 1.493(3) . ? C21 C25 1.393(4) . ? C21 C22 1.395(4) . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 N5 1.342(4) . ? C23 H23 0.9500 . ? N5 C24 1.347(4) . ? C24 C25 1.388(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.396(4) . ? C26 C30 1.401(4) . ? C27 C28 1.391(4) . ? C27 H27 0.9500 . ? C28 N6 1.344(3) . ? C28 H28 0.9500 . ? N6 C29 1.344(3) . ? N6 Cd1 2.388(2) 1_545 ? C29 C30 1.384(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.388(4) . ? C31 C32 1.408(4) . ? C32 C33 1.404(4) . ? C32 H32 0.9500 . ? C33 C34 1.370(6) . ? C33 H33 0.9500 . ? C34 C35 1.373(6) . ? C34 H34 0.9500 . ? C35 C36 1.393(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.401(4) . ? C37 C42 1.405(4) . ? C38 C39 1.391(4) . ? C38 H38 0.9500 . ? C39 C40 1.387(5) . ? C39 H39 0.9500 . ? C40 C41 1.391(5) . ? C40 H40 0.9500 . ? C41 C42 1.384(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 Cl1 1.746(4) . ? C43 Cl3 1.757(4) . ? C43 Cl2 1.760(4) . ? C43 H43 1.0000 . ? C44 Cl5 1.731(5) . ? C44 Cl6 1.737(5) . ? C44 Cl4 1.774(5) . ? C44 H44 1.0000 . ? 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 N6 Cd1 N6 180.0 2_466 1_565 ? N6 Cd1 N5 90.81(8) 2_466 . ? N6 Cd1 N5 89.20(8) 1_565 . ? N6 Cd1 N5 89.20(8) 2_466 2_476 ? N6 Cd1 N5 90.80(8) 1_565 2_476 ? N5 Cd1 N5 179.998(1) . 2_476 ? N6 Cd1 Br1 90.70(6) 2_466 . ? N6 Cd1 Br1 89.30(6) 1_565 . ? N5 Cd1 Br1 89.84(6) . . ? N5 Cd1 Br1 90.16(6) 2_476 . ? N6 Cd1 Br1 89.30(6) 2_466 2_476 ? N6 Cd1 Br1 90.70(6) 1_565 2_476 ? N5 Cd1 Br1 90.16(6) . 2_476 ? N5 Cd1 Br1 89.84(6) 2_476 2_476 ? Br1 Cd1 Br1 179.999(2) . 2_476 ? C4 N1 C1 110.0(2) . . ? C4 N1 H1A 125.0 . . ? C1 N1 H1A 125.0 . . ? C9 N2 C6 105.4(2) . . ? C14 N3 C11 110.3(2) . . ? C14 N3 H3A 124.8 . . ? C11 N3 H3A 124.8 . . ? C16 N4 C19 104.8(2) . . ? N1 C1 C20 125.8(2) . . ? N1 C1 C2 106.8(2) . . ? C20 C1 C2 127.5(2) . . ? C3 C2 C1 108.4(2) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? C2 C3 C4 107.8(2) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? N1 C4 C5 126.1(2) . . ? N1 C4 C3 107.0(2) . . ? C5 C4 C3 126.8(2) . . ? C6 C5 C4 125.6(2) . . ? C6 C5 C21 118.2(2) . . ? C4 C5 C21 116.2(2) . . ? N2 C6 C5 125.0(2) . . ? N2 C6 C7 110.8(2) . . ? C5 C6 C7 124.2(2) . . ? C8 C7 C6 106.9(2) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C7 C8 C9 106.8(2) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N2 C9 C10 125.5(2) . . ? N2 C9 C8 110.1(2) . . ? C10 C9 C8 124.2(2) . . ? C11 C10 C9 125.6(2) . . ? C11 C10 C26 116.2(2) . . ? C9 C10 C26 118.0(2) . . ? N3 C11 C10 125.4(2) . . ? N3 C11 C12 106.9(2) . . ? C10 C11 C12 127.6(2) . . ? C13 C12 C11 107.6(2) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? C12 C13 C14 108.1(2) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? N3 C14 C15 126.5(2) . . ? N3 C14 C13 107.0(2) . . ? C15 C14 C13 126.5(2) . . ? C14 C15 C16 125.3(2) . . ? C14 C15 C31 116.4(2) . . ? C16 C15 C31 118.3(2) . . ? N4 C16 C15 124.7(2) . . ? N4 C16 C17 111.2(2) . . ? C15 C16 C17 124.1(2) . . ? C18 C17 C16 106.4(2) . . ? C18 C17 H17 126.8 . . ? C16 C17 H17 126.8 . . ? C17 C18 C19 106.4(2) . . ? C17 C18 H18 126.8 . . ? C19 C18 H18 126.8 . . ? N4 C19 C20 125.1(2) . . ? N4 C19 C18 111.2(2) . . ? C20 C19 C18 123.6(2) . . ? C1 C20 C19 124.8(2) . . ? C1 C20 C37 117.4(2) . . ? C19 C20 C37 117.8(2) . . ? C25 C21 C22 117.3(2) . . ? C25 C21 C5 120.6(2) . . ? C22 C21 C5 122.1(2) . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? N5 C23 C22 123.3(3) . . ? N5 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? C23 N5 C24 117.0(2) . . ? C23 N5 Cd1 121.88(17) . . ? C24 N5 Cd1 120.81(18) . . ? N5 C24 C25 123.3(3) . . ? N5 C24 H24 118.3 . . ? C25 C24 H24 118.3 . . ? C24 C25 C21 119.5(3) . . ? C24 C25 H25 120.2 . . ? C21 C25 H25 120.2 . . ? C27 C26 C30 117.2(2) . . ? C27 C26 C10 123.9(2) . . ? C30 C26 C10 118.8(2) . . ? C28 C27 C26 119.5(2) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? N6 C28 C27 123.1(2) . . ? N6 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? C28 N6 C29 117.3(2) . . ? C28 N6 Cd1 124.86(18) . 1_545 ? C29 N6 Cd1 117.80(17) . 1_545 ? N6 C29 C30 123.4(2) . . ? N6 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? C29 C30 C26 119.4(2) . . ? C29 C30 H30 120.3 . . ? C26 C30 H30 120.3 . . ? C36 C31 C32 119.2(3) . . ? C36 C31 C15 121.2(3) . . ? C32 C31 C15 119.6(3) . . ? C33 C32 C31 119.3(3) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C32 120.8(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 119.6(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 121.2(3) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C31 C36 C35 119.9(3) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C42 118.1(2) . . ? C38 C37 C20 120.5(2) . . ? C42 C37 C20 121.4(2) . . ? C39 C38 C37 120.8(3) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 120.4(3) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 119.4(3) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C42 C41 C40 120.5(3) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C37 120.9(3) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? Cl1 C43 Cl3 111.1(2) . . ? Cl1 C43 Cl2 111.1(2) . . ? Cl3 C43 Cl2 111.5(2) . . ? Cl1 C43 H43 107.7 . . ? Cl3 C43 H43 107.7 . . ? Cl2 C43 H43 107.7 . . ? Cl5 C44 Cl6 111.4(3) . . ? Cl5 C44 Cl4 112.8(2) . . ? Cl6 C44 Cl4 109.4(3) . . ? Cl5 C44 H44 107.7 . . ? Cl6 C44 H44 107.7 . . ? Cl4 C44 H44 107.7 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.362 _refine_diff_density_min -1.897 _refine_diff_density_rms 0.123 # Attachment '2-Cu,Cu-CuBr4.cif' data_e139a _database_code_depnum_ccdc_archive 'CCDC 659599' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C42 H26 Br2 Cu2 N6 O2), 3 (H2O)' _chemical_formula_sum 'C84 H58 Br4 Cu4 N12 O7' _chemical_formula_weight 1921.22 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1872(3) _cell_length_b 14.4491(5) _cell_length_c 16.8506(5) _cell_angle_alpha 80.7490(10) _cell_angle_beta 78.4670(10) _cell_angle_gamma 75.4150(10) _cell_volume 1877.34(11) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6562 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 28.35 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 958 _exptl_absorpt_coefficient_mu 3.312 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7120 _exptl_absorpt_correction_T_max 0.8789 _exptl_absorpt_process_details sadabs _exptl_special_details ; No hydrogen atoms were introduced on solvant molecules However,the missing hydrogen atoms have been added to the formula ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50820 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 30.11 _reflns_number_total 11013 _reflns_number_gt 7701 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1800P)^2^+6.7000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11013 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2797 _refine_ls_wR_factor_gt 0.2533 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Cu2 Cu 0.5000 0.5000 0.5000 0.0265(2) Uani 1 2 d S . . Cu1 Cu 0.69338(8) 0.05097(4) 0.07457(3) 0.01920(17) Uani 1 1 d . . . Cu3 Cu 0.0527(3) 0.42587(13) 0.55955(13) 0.0560(6) Uani 0.50 1 d P . . Br1 Br 0.09082(14) 0.27208(8) 0.62968(7) 0.0719(3) Uani 1 1 d . . . Br2 Br 0.11471(10) 0.57419(5) 0.55911(5) 0.0451(2) Uani 1 1 d . . . C1 C 0.6006(7) 0.2247(3) 0.1685(3) 0.0214(9) Uani 1 1 d . . . C2 C 0.5779(8) 0.3281(4) 0.1556(3) 0.0269(10) Uani 1 1 d . . . H2 H 0.5316 0.3711 0.1958 0.032 Uiso 1 1 calc R . . C3 C 0.6350(8) 0.3523(4) 0.0756(3) 0.0274(11) Uani 1 1 d . . . H3 H 0.6357 0.4153 0.0487 0.033 Uiso 1 1 calc R . . C4 C 0.6944(7) 0.2631(3) 0.0394(3) 0.0229(9) Uani 1 1 d . . . C5 C 0.7816(7) 0.2562(3) -0.0414(3) 0.0231(10) Uani 1 1 d . . . C6 C 0.8339(7) 0.1701(4) -0.0770(3) 0.0240(10) Uani 1 1 d . . . C7 C 0.9324(8) 0.1600(4) -0.1571(3) 0.0272(11) Uani 1 1 d . . . H7 H 0.9781 0.2085 -0.1930 0.033 Uiso 1 1 calc R . . C8 C 0.9483(7) 0.0676(4) -0.1720(3) 0.0259(10) Uani 1 1 d . . . H8 H 1.0094 0.0391 -0.2194 0.031 Uiso 1 1 calc R . . C9 C 0.8538(7) 0.0219(4) -0.1012(3) 0.0220(9) Uani 1 1 d . . . C10 C 0.8224(7) -0.0697(3) -0.0957(3) 0.0205(9) Uani 1 1 d . . . C11 C 0.7399(7) -0.1153(4) -0.0243(3) 0.0216(9) Uani 1 1 d . . . C12 C 0.6969(7) -0.2069(4) -0.0177(3) 0.0245(10) Uani 1 1 d . . . H12 H 0.7096 -0.2444 -0.0609 0.029 Uiso 1 1 calc R . . C13 C 0.6342(7) -0.2302(4) 0.0627(3) 0.0260(10) Uani 1 1 d . . . H13 H 0.5941 -0.2865 0.0858 0.031 Uiso 1 1 calc R . . C14 C 0.6407(7) -0.1534(3) 0.1051(3) 0.0216(9) Uani 1 1 d . . . C15 C 0.6007(7) -0.1530(3) 0.1895(3) 0.0219(9) Uani 1 1 d . . . C16 C 0.5951(7) -0.0752(3) 0.2308(3) 0.0211(9) Uani 1 1 d . . . C17 C 0.5628(7) -0.0765(4) 0.3179(3) 0.0255(10) Uani 1 1 d . . . H17 H 0.5477 -0.1300 0.3573 0.031 Uiso 1 1 calc R . . C18 C 0.5582(7) 0.0143(4) 0.3331(3) 0.0250(10) Uani 1 1 d . . . H18 H 0.5395 0.0359 0.3852 0.030 Uiso 1 1 calc R . . C19 C 0.5871(7) 0.0714(3) 0.2551(3) 0.0210(9) Uani 1 1 d . . . C20 C 0.5745(7) 0.1699(3) 0.2450(3) 0.0215(9) Uani 1 1 d . . . C21 C 0.8178(8) 0.3463(4) -0.0926(3) 0.0260(10) Uani 1 1 d . . . C22 C 0.9217(8) 0.3976(4) -0.0703(3) 0.0308(11) Uani 1 1 d . . . H22 H 0.9695 0.3765 -0.0218 0.037 Uiso 1 1 calc R . . C23 C 0.9550(9) 0.4807(4) -0.1202(4) 0.0370(13) Uani 1 1 d . . . H23 H 1.0237 0.5164 -0.1045 0.044 Uiso 1 1 calc R . . C41 C 0.8896(9) 0.5111(4) -0.1913(4) 0.0394(14) Uani 1 1 d . . . H41 H 0.9146 0.5669 -0.2248 0.047 Uiso 1 1 calc R . . C24 C 0.7875(9) 0.4607(4) -0.2143(4) 0.0368(13) Uani 1 1 d . . . H24 H 0.7420 0.4816 -0.2635 0.044 Uiso 1 1 calc R . . C25 C 0.7519(8) 0.3785(4) -0.1645(3) 0.0305(11) Uani 1 1 d . . . H25 H 0.6811 0.3440 -0.1802 0.037 Uiso 1 1 calc R . . C26 C 0.8757(7) -0.1226(4) -0.1686(3) 0.0237(10) Uani 1 1 d . . . C27 C 0.8156(8) -0.0815(4) -0.2413(3) 0.0291(11) Uani 1 1 d . . . H27 H 0.7432 -0.0188 -0.2448 0.035 Uiso 1 1 calc R . . C28 C 0.8633(8) -0.1339(6) -0.3097(4) 0.0382(14) Uani 1 1 d . . . H28 H 0.8228 -0.1062 -0.3592 0.046 Uiso 1 1 calc R . . C42 C 0.9685(9) -0.2252(6) -0.3047(4) 0.0422(16) Uani 1 1 d . . . H42 H 0.9965 -0.2610 -0.3502 0.051 Uiso 1 1 calc R . . C29 C 1.0326(8) -0.2644(5) -0.2345(4) 0.0363(13) Uani 1 1 d . . . H29 H 1.1095 -0.3259 -0.2325 0.044 Uiso 1 1 calc R . . C30 C 0.9858(7) -0.2146(4) -0.1652(4) 0.0283(11) Uani 1 1 d . . . H30 H 1.0283 -0.2431 -0.1164 0.034 Uiso 1 1 calc R . . C31 C 0.5619(7) -0.2421(4) 0.2400(3) 0.0222(9) Uani 1 1 d . . . C32 C 0.6863(7) -0.3287(4) 0.2393(3) 0.0266(10) Uani 1 1 d . . . H32 H 0.7940 -0.3314 0.2048 0.032 Uiso 1 1 calc R . . C33 C 0.6533(8) -0.4105(4) 0.2888(3) 0.0272(11) Uani 1 1 d . . . H33 H 0.7378 -0.4691 0.2880 0.033 Uiso 1 1 calc R . . C34 C 0.3767(7) -0.3255(4) 0.3404(3) 0.0260(10) Uani 1 1 d . . . H34 H 0.2700 -0.3252 0.3753 0.031 Uiso 1 1 calc R . . C35 C 0.4046(7) -0.2416(4) 0.2914(3) 0.0254(10) Uani 1 1 d . . . H35 H 0.3169 -0.1843 0.2929 0.030 Uiso 1 1 calc R . . C36 C 0.5353(7) 0.2207(3) 0.3199(3) 0.0210(9) Uani 1 1 d . . . C37 C 0.6485(7) 0.1977(4) 0.3753(3) 0.0261(10) Uani 1 1 d . . . H37 H 0.7461 0.1459 0.3679 0.031 Uiso 1 1 calc R . . C38 C 0.6208(8) 0.2492(4) 0.4413(3) 0.0277(11) Uani 1 1 d . . . H38 H 0.6998 0.2334 0.4784 0.033 Uiso 1 1 calc R . . C39 C 0.3641(7) 0.3431(4) 0.4030(3) 0.0263(10) Uani 1 1 d . . . H39 H 0.2640 0.3925 0.4140 0.032 Uiso 1 1 calc R . . C40 C 0.3879(7) 0.2936(4) 0.3362(3) 0.0243(10) Uani 1 1 d . . . H40 H 0.3044 0.3091 0.3014 0.029 Uiso 1 1 calc R . . N1 N 0.6665(6) 0.1870(3) 0.0966(2) 0.0203(8) Uani 1 1 d . . . N2 N 0.7907(6) 0.0847(3) -0.0420(2) 0.0213(8) Uani 1 1 d . . . N3 N 0.7008(6) -0.0812(3) 0.0511(2) 0.0220(8) Uani 1 1 d . . . N4 N 0.6148(6) 0.0147(3) 0.1932(2) 0.0207(8) Uani 1 1 d . . . N6 N 0.5001(6) -0.4066(3) 0.3385(2) 0.0247(9) Uani 1 1 d . . . N7 N 0.4818(6) 0.3215(3) 0.4523(3) 0.0241(9) Uani 1 1 d . . . O1 O 0.4718(6) -0.4866(3) 0.3853(2) 0.0301(9) Uani 1 1 d . . . O2 O 0.4574(6) 0.3708(3) 0.5163(2) 0.0317(9) Uani 1 1 d . . . O4 O 0.7183(11) 0.8729(7) 0.4960(5) 0.0354(19) Uani 0.50 1 d P . . O3A O 0.9588(19) 0.1000(14) 0.5839(10) 0.097(6) Uani 0.50 1 d P . . O3B O 0.965(2) 0.1509(10) 0.5185(9) 0.070(4) Uani 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 Cu2 0.0517(6) 0.0178(4) 0.0137(4) -0.0011(3) -0.0039(4) -0.0164(4) Cu1 0.0279(3) 0.0164(3) 0.0143(3) -0.00234(19) -0.0020(2) -0.0076(2) Cu3 0.0617(12) 0.0323(8) 0.0637(12) -0.0221(8) 0.0406(10) -0.0217(8) Br1 0.0694(6) 0.0796(7) 0.0679(6) 0.0052(5) -0.0207(5) -0.0206(5) Br2 0.0462(4) 0.0382(4) 0.0488(4) -0.0094(3) -0.0069(3) -0.0039(3) C1 0.028(2) 0.016(2) 0.021(2) -0.0047(16) -0.0019(18) -0.0065(17) C2 0.037(3) 0.018(2) 0.025(2) -0.0053(18) -0.002(2) -0.007(2) C3 0.039(3) 0.017(2) 0.025(2) -0.0039(18) -0.003(2) -0.005(2) C4 0.034(3) 0.016(2) 0.020(2) -0.0026(16) -0.0045(19) -0.0073(18) C5 0.036(3) 0.016(2) 0.018(2) 0.0000(16) -0.0039(19) -0.0106(19) C6 0.032(3) 0.022(2) 0.019(2) -0.0018(17) -0.0005(19) -0.0105(19) C7 0.037(3) 0.026(2) 0.018(2) -0.0001(18) 0.002(2) -0.014(2) C8 0.033(3) 0.024(2) 0.020(2) -0.0037(18) 0.0017(19) -0.010(2) C9 0.030(3) 0.023(2) 0.0140(19) -0.0039(16) -0.0008(17) -0.0081(19) C10 0.026(2) 0.020(2) 0.0158(19) -0.0035(16) -0.0026(17) -0.0055(17) C11 0.026(2) 0.022(2) 0.018(2) -0.0037(17) -0.0026(17) -0.0089(18) C12 0.035(3) 0.021(2) 0.020(2) -0.0052(17) -0.0023(19) -0.013(2) C13 0.037(3) 0.022(2) 0.022(2) -0.0041(18) -0.003(2) -0.014(2) C14 0.032(3) 0.017(2) 0.017(2) -0.0019(16) -0.0033(18) -0.0082(18) C15 0.030(3) 0.018(2) 0.017(2) 0.0008(16) -0.0025(18) -0.0069(18) C16 0.029(2) 0.018(2) 0.018(2) 0.0003(16) -0.0030(18) -0.0099(18) C17 0.038(3) 0.020(2) 0.018(2) -0.0019(17) -0.0014(19) -0.008(2) C18 0.037(3) 0.022(2) 0.017(2) -0.0019(17) -0.0033(19) -0.009(2) C19 0.028(2) 0.018(2) 0.017(2) -0.0058(16) -0.0011(17) -0.0059(17) C20 0.027(2) 0.021(2) 0.018(2) -0.0058(17) -0.0019(17) -0.0082(18) C21 0.040(3) 0.018(2) 0.020(2) -0.0007(17) -0.002(2) -0.011(2) C22 0.042(3) 0.026(2) 0.027(3) -0.004(2) -0.007(2) -0.012(2) C23 0.046(4) 0.027(3) 0.042(3) -0.004(2) -0.002(3) -0.019(2) C41 0.048(4) 0.025(3) 0.043(3) 0.006(2) -0.004(3) -0.014(3) C24 0.056(4) 0.024(3) 0.029(3) 0.006(2) -0.007(3) -0.012(3) C25 0.045(3) 0.024(2) 0.025(2) 0.002(2) -0.007(2) -0.015(2) C26 0.025(2) 0.027(2) 0.021(2) -0.0076(18) 0.0012(18) -0.0102(19) C27 0.032(3) 0.035(3) 0.021(2) -0.006(2) -0.002(2) -0.010(2) C28 0.031(3) 0.066(4) 0.024(3) -0.018(3) 0.001(2) -0.020(3) C42 0.036(3) 0.061(4) 0.039(3) -0.034(3) 0.009(3) -0.023(3) C29 0.029(3) 0.032(3) 0.050(4) -0.023(3) 0.006(3) -0.011(2) C30 0.028(3) 0.025(2) 0.034(3) -0.008(2) 0.000(2) -0.009(2) C31 0.032(3) 0.021(2) 0.0149(19) -0.0005(16) -0.0017(18) -0.0108(19) C32 0.035(3) 0.022(2) 0.020(2) -0.0013(18) 0.0025(19) -0.008(2) C33 0.038(3) 0.020(2) 0.021(2) 0.0000(18) 0.000(2) -0.007(2) C34 0.032(3) 0.026(2) 0.020(2) -0.0017(18) 0.0000(19) -0.011(2) C35 0.031(3) 0.026(2) 0.020(2) -0.0008(18) -0.0029(19) -0.011(2) C36 0.025(2) 0.020(2) 0.019(2) -0.0060(16) 0.0003(17) -0.0086(18) C37 0.029(3) 0.025(2) 0.026(2) -0.0063(19) -0.004(2) -0.008(2) C38 0.036(3) 0.027(2) 0.024(2) -0.0029(19) -0.007(2) -0.013(2) C39 0.031(3) 0.022(2) 0.026(2) -0.0067(18) 0.001(2) -0.008(2) C40 0.028(3) 0.022(2) 0.025(2) -0.0047(18) -0.0030(19) -0.0090(19) N1 0.030(2) 0.0179(17) 0.0155(17) -0.0022(14) -0.0038(15) -0.0091(15) N2 0.031(2) 0.0158(17) 0.0177(18) -0.0023(14) -0.0005(16) -0.0083(15) N3 0.032(2) 0.0197(18) 0.0158(17) -0.0014(14) -0.0026(16) -0.0098(16) N4 0.029(2) 0.0173(17) 0.0158(17) -0.0026(14) -0.0003(15) -0.0085(15) N6 0.044(3) 0.0194(19) 0.0142(17) 0.0003(14) -0.0035(17) -0.0162(18) N7 0.038(2) 0.0185(18) 0.0178(18) -0.0069(15) 0.0016(17) -0.0131(17) O1 0.056(3) 0.0249(18) 0.0164(16) 0.0032(13) -0.0067(16) -0.0243(18) O2 0.062(3) 0.0215(17) 0.0132(15) -0.0040(13) 0.0021(16) -0.0184(18) O4 0.033(4) 0.053(5) 0.015(3) -0.001(3) 0.002(3) -0.007(4) O3A 0.061(9) 0.143(15) 0.083(10) 0.037(10) 0.005(7) -0.063(10) O3B 0.090(10) 0.056(7) 0.070(8) -0.005(6) -0.035(7) -0.010(7) _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 Cu2 O2 1.952(4) 2_666 ? Cu2 O2 1.952(4) . ? Cu2 O1 1.964(4) 2_656 ? Cu2 O1 1.964(4) 1_565 ? Cu1 N3 1.995(4) . ? Cu1 N2 1.999(4) . ? Cu1 N4 2.001(4) . ? Cu1 N1 2.008(4) . ? Cu3 Br1 2.321(2) . ? Cu3 Br2 2.3223(18) . ? Cu3 Br2 2.641(3) 2_566 ? Cu3 Cu3 2.782(5) 2_566 ? Br2 Cu3 2.641(3) 2_566 ? C1 N1 1.364(6) . ? C1 C20 1.407(7) . ? C1 C2 1.444(7) . ? C2 C3 1.356(7) . ? C2 H2 0.9500 . ? C3 C4 1.445(7) . ? C3 H3 0.9500 . ? C4 N1 1.373(6) . ? C4 C5 1.412(7) . ? C5 C6 1.400(7) . ? C5 C21 1.503(6) . ? C6 N2 1.377(6) . ? C6 C7 1.436(7) . ? C7 C8 1.367(7) . ? C7 H7 0.9500 . ? C8 C9 1.447(7) . ? C8 H8 0.9500 . ? C9 N2 1.391(6) . ? C9 C10 1.395(7) . ? C10 C11 1.408(6) . ? C10 C26 1.485(7) . ? C11 N3 1.384(6) . ? C11 C12 1.436(7) . ? C12 C13 1.368(7) . ? C12 H12 0.9500 . ? C13 C14 1.430(7) . ? C13 H13 0.9500 . ? C14 N3 1.391(6) . ? C14 C15 1.395(7) . ? C15 C16 1.401(7) . ? C15 C31 1.494(6) . ? C16 N4 1.383(6) . ? C16 C17 1.437(7) . ? C17 C18 1.366(7) . ? C17 H17 0.9500 . ? C18 C19 1.445(6) . ? C18 H18 0.9500 . ? C19 N4 1.378(6) . ? C19 C20 1.386(7) . ? C20 C36 1.500(7) . ? C21 C25 1.389(7) . ? C21 C22 1.395(8) . ? C22 C23 1.403(8) . ? C22 H22 0.9500 . ? C23 C41 1.373(10) . ? C23 H23 0.9500 . ? C41 C24 1.380(10) . ? C41 H41 0.9500 . ? C24 C25 1.398(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.397(7) . ? C26 C30 1.406(7) . ? C27 C28 1.416(8) . ? C27 H27 0.9500 . ? C28 C42 1.382(11) . ? C28 H28 0.9500 . ? C42 C29 1.372(11) . ? C42 H42 0.9500 . ? C29 C30 1.406(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C35 1.400(7) . ? C31 C32 1.400(7) . ? C32 C33 1.385(7) . ? C32 H32 0.9500 . ? C33 N6 1.355(7) . ? C33 H33 0.9500 . ? C34 N6 1.341(7) . ? C34 C35 1.394(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.390(7) . ? C36 C40 1.400(7) . ? C37 C38 1.386(7) . ? C37 H37 0.9500 . ? C38 N7 1.342(7) . ? C38 H38 0.9500 . ? C39 N7 1.343(7) . ? C39 C40 1.385(7) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? N6 O1 1.334(5) . ? N7 O2 1.341(5) . ? O1 Cu2 1.964(4) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu2 O2 179.999(1) 2_666 . ? O2 Cu2 O1 90.16(15) 2_666 2_656 ? O2 Cu2 O1 89.83(15) . 2_656 ? O2 Cu2 O1 89.84(15) 2_666 1_565 ? O2 Cu2 O1 90.16(15) . 1_565 ? O1 Cu2 O1 179.998(1) 2_656 1_565 ? N3 Cu1 N2 89.94(16) . . ? N3 Cu1 N4 90.48(16) . . ? N2 Cu1 N4 175.47(18) . . ? N3 Cu1 N1 175.41(18) . . ? N2 Cu1 N1 90.34(16) . . ? N4 Cu1 N1 89.60(16) . . ? Br1 Cu3 Br2 141.18(13) . . ? Br1 Cu3 Br2 106.66(8) . 2_566 ? Br2 Cu3 Br2 112.16(9) . 2_566 ? Br1 Cu3 Cu3 157.29(15) . 2_566 ? Br2 Cu3 Cu3 61.53(6) . 2_566 ? Br2 Cu3 Cu3 50.63(9) 2_566 2_566 ? Cu3 Br2 Cu3 67.84(9) . 2_566 ? N1 C1 C20 124.7(4) . . ? N1 C1 C2 110.0(4) . . ? C20 C1 C2 125.0(5) . . ? C3 C2 C1 107.3(5) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 106.2(4) . . ? C2 C3 H3 126.9 . . ? C4 C3 H3 126.9 . . ? N1 C4 C5 125.7(4) . . ? N1 C4 C3 110.3(4) . . ? C5 C4 C3 123.8(4) . . ? C6 C5 C4 123.5(4) . . ? C6 C5 C21 118.1(4) . . ? C4 C5 C21 118.4(4) . . ? N2 C6 C5 124.8(5) . . ? N2 C6 C7 110.6(4) . . ? C5 C6 C7 124.5(5) . . ? C8 C7 C6 107.2(4) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 106.5(4) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C10 125.3(4) . . ? N2 C9 C8 110.0(4) . . ? C10 C9 C8 124.6(4) . . ? C9 C10 C11 123.5(4) . . ? C9 C10 C26 119.2(4) . . ? C11 C10 C26 117.3(4) . . ? N3 C11 C10 124.4(4) . . ? N3 C11 C12 110.4(4) . . ? C10 C11 C12 125.0(5) . . ? C13 C12 C11 107.1(4) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? C12 C13 C14 106.7(4) . . ? C12 C13 H13 126.6 . . ? C14 C13 H13 126.6 . . ? N3 C14 C15 124.4(4) . . ? N3 C14 C13 110.7(4) . . ? C15 C14 C13 124.8(4) . . ? C14 C15 C16 124.9(4) . . ? C14 C15 C31 117.8(4) . . ? C16 C15 C31 117.3(4) . . ? N4 C16 C15 124.6(4) . . ? N4 C16 C17 110.5(4) . . ? C15 C16 C17 124.9(4) . . ? C18 C17 C16 106.4(4) . . ? C18 C17 H17 126.8 . . ? C16 C17 H17 126.8 . . ? C17 C18 C19 107.3(4) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? N4 C19 C20 125.6(4) . . ? N4 C19 C18 109.7(4) . . ? C20 C19 C18 124.5(4) . . ? C19 C20 C1 123.7(4) . . ? C19 C20 C36 118.2(4) . . ? C1 C20 C36 118.1(4) . . ? C25 C21 C22 118.8(5) . . ? C25 C21 C5 120.2(5) . . ? C22 C21 C5 120.9(5) . . ? C21 C22 C23 119.5(5) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C41 C23 C22 120.9(6) . . ? C41 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C41 C24 120.2(5) . . ? C23 C41 H41 119.9 . . ? C24 C41 H41 119.9 . . ? C41 C24 C25 119.3(6) . . ? C41 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C21 C25 C24 121.3(6) . . ? C21 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C27 C26 C30 119.3(5) . . ? C27 C26 C10 120.2(5) . . ? C30 C26 C10 120.5(5) . . ? C26 C27 C28 119.6(6) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C42 C28 C27 120.3(6) . . ? C42 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C29 C42 C28 120.2(6) . . ? C29 C42 H42 119.9 . . ? C28 C42 H42 119.9 . . ? C42 C29 C30 120.7(6) . . ? C42 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C26 119.8(6) . . ? C29 C30 H30 120.1 . . ? C26 C30 H30 120.1 . . ? C35 C31 C32 117.9(5) . . ? C35 C31 C15 121.8(5) . . ? C32 C31 C15 120.2(5) . . ? C33 C32 C31 120.3(5) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? N6 C33 C32 119.9(5) . . ? N6 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? N6 C34 C35 120.2(5) . . ? N6 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C31 119.9(5) . . ? C34 C35 H35 120.1 . . ? C31 C35 H35 120.1 . . ? C37 C36 C40 117.5(5) . . ? C37 C36 C20 120.2(5) . . ? C40 C36 C20 122.3(5) . . ? C38 C37 C36 120.9(5) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? N7 C38 C37 119.6(5) . . ? N7 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? N7 C39 C40 120.3(5) . . ? N7 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C36 119.9(5) . . ? C39 C40 H40 120.0 . . ? C36 C40 H40 120.0 . . ? C1 N1 C4 106.1(4) . . ? C1 N1 Cu1 127.4(3) . . ? C4 N1 Cu1 126.2(3) . . ? C6 N2 C9 105.5(4) . . ? C6 N2 Cu1 127.2(3) . . ? C9 N2 Cu1 126.6(3) . . ? C11 N3 C14 105.0(4) . . ? C11 N3 Cu1 127.5(3) . . ? C14 N3 Cu1 126.8(3) . . ? C19 N4 C16 105.9(4) . . ? C19 N4 Cu1 126.8(3) . . ? C16 N4 Cu1 127.0(3) . . ? O1 N6 C34 119.7(5) . . ? O1 N6 C33 118.5(5) . . ? C34 N6 C33 121.8(4) . . ? O2 N7 C38 118.7(5) . . ? O2 N7 C39 119.5(5) . . ? C38 N7 C39 121.8(4) . . ? N6 O1 Cu2 117.4(3) . 1_545 ? N7 O2 Cu2 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.490 _refine_diff_density_min -2.953 _refine_diff_density_rms 0.226