# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'A. Addison' _publ_contact_author_email ADDISONA@DREXEL.EDU _publ_section_title ; A novel copper(II) complex of a tripodal ligand with phenolate-phenol interligand intra-dimer hydrogen bonding ; loop_ _publ_author_name 'A. Addison' 'K. Travis Holman' 'Vaidyanathan Mathrubootham' 'Ekkehard Sinn' 'L. Thompson' # Attachment '692208 B.txt' data_692208 _database_code_depnum_ccdc_archive 'CCDC 692208' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C32 H35 Cu2 N6 O4, Cl O4, C2 H3 N' _chemical_formula_sum 'C34 H38 Cl Cu2 N7 O8' _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour 'dark blue/green' _diffrn_ambient_temperature 185(2) _chemical_formula_weight 835.24 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6923(10) _cell_length_b 13.9323(13) _cell_length_c 13.9809(13) _cell_angle_alpha 115.514(2) _cell_angle_beta 101.644(2) _cell_angle_gamma 99.473(2) _cell_volume 1764.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 7655 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.20 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5532 _exptl_absorpt_correction_T_max 0.8555 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens SMART 1K CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART 1K CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18616 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7661 _reflns_number_gt 5976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-SEED, L.Barbour (1999); http://x-seed.net/' _computing_publication_material 'SHELXL-97-2, G. Sheldrick (1997)' _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^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7661 _refine_ls_number_parameters 512 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.054 _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 Cu1 Cu 0.25557(3) 0.29737(2) 0.20992(2) 0.02042(9) Uani 1 1 d . . . Cu2 Cu 0.30166(3) 0.34376(2) 0.48631(2) 0.02030(9) Uani 1 1 d . . . Cl1 Cl 0.21909(7) 0.65115(6) 0.12913(6) 0.03278(17) Uani 1 1 d D . . O1A O 0.15472(17) 0.13585(14) 0.19827(14) 0.0231(4) Uani 1 1 d . . . O2A O 0.15573(17) 0.36845(15) 0.40566(13) 0.0233(4) Uani 1 1 d . . . N1A N 0.1438(2) 0.35852(16) 0.30343(16) 0.0201(4) Uani 1 1 d . . . N2A N 0.1005(2) 0.27852(17) 0.08448(17) 0.0221(5) Uani 1 1 d . . . N3A N 0.3480(2) 0.26772(18) 0.09329(18) 0.0269(5) Uani 1 1 d . . . C1A C 0.0217(3) 0.1105(2) 0.1710(2) 0.0229(5) Uani 1 1 d . . . C2A C -0.0484(3) 0.0757(2) 0.2307(2) 0.0285(6) Uani 1 1 d . . . H2A H -0.0009 0.0722 0.2937 0.034 Uiso 1 1 calc R . . C3A C -0.1854(3) 0.0467(2) 0.1983(3) 0.0378(7) Uani 1 1 d . . . H3A H -0.2315 0.0228 0.2391 0.045 Uiso 1 1 calc R . . C4A C -0.2574(3) 0.0519(3) 0.1069(3) 0.0386(7) Uani 1 1 d . . . H4A H -0.3520 0.0309 0.0845 0.046 Uiso 1 1 calc R . . C5A C -0.1894(3) 0.0878(2) 0.0496(2) 0.0312(6) Uani 1 1 d . . . H5A H -0.2380 0.0923 -0.0125 0.037 Uiso 1 1 calc R . . C6A C -0.0509(3) 0.1180(2) 0.0801(2) 0.0244(6) Uani 1 1 d . . . C7A C 0.0212(3) 0.1583(2) 0.0173(2) 0.0261(6) Uani 1 1 d . . . H7A1 H -0.0444 0.1475 -0.0502 0.031 Uiso 1 1 calc R . . H7A2 H 0.0820 0.1129 -0.0073 0.031 Uiso 1 1 calc R . . C8A C 0.0187(3) 0.3490(2) 0.1372(2) 0.0246(6) Uani 1 1 d . . . H8A1 H -0.0758 0.3150 0.0905 0.029 Uiso 1 1 calc R . . H8A2 H 0.0488 0.4230 0.1432 0.029 Uiso 1 1 calc R . . C9A C 0.0311(3) 0.3611(2) 0.2512(2) 0.0217(5) Uani 1 1 d . . . C10A C -0.0820(3) 0.3713(2) 0.2981(2) 0.0294(6) Uani 1 1 d . . . H10A H -0.1218 0.3010 0.2949 0.044 Uiso 1 1 calc R . . H10B H -0.1492 0.3892 0.2546 0.044 Uiso 1 1 calc R . . H10C H -0.0497 0.4305 0.3757 0.044 Uiso 1 1 calc R . . C11A C 0.1603(3) 0.3120(2) 0.0128(2) 0.0297(6) Uani 1 1 d . . . H11A H 0.1816 0.3935 0.0441 0.036 Uiso 1 1 calc R . . H11B H 0.0957 0.2771 -0.0626 0.036 Uiso 1 1 calc R . . C12A C 0.2849(3) 0.2768(2) 0.0055(2) 0.0270(6) Uani 1 1 d . . . C13A C 0.3368(3) 0.2608(2) -0.0809(2) 0.0336(7) Uani 1 1 d . . . H13A H 0.2892 0.2645 -0.1437 0.040 Uiso 1 1 calc R . . C14A C 0.4586(3) 0.2391(2) -0.0753(3) 0.0405(8) Uani 1 1 d . . . H14A H 0.4968 0.2296 -0.1333 0.049 Uiso 1 1 calc R . . C15A C 0.5235(3) 0.2315(3) 0.0150(3) 0.0402(7) Uani 1 1 d . . . H15A H 0.6081 0.2176 0.0206 0.048 Uiso 1 1 calc R . . C16A C 0.4659(3) 0.2441(2) 0.0976(2) 0.0334(7) Uani 1 1 d . . . H16A H 0.5098 0.2360 0.1588 0.040 Uiso 1 1 calc R . . O1B O 0.25884(17) 0.15973(14) 0.38195(14) 0.0233(4) Uani 1 1 d . . . O2B O 0.42660(17) 0.34017(15) 0.31405(14) 0.0242(4) Uani 1 1 d . . . N1B N 0.4436(2) 0.35959(17) 0.41973(16) 0.0203(4) Uani 1 1 d . . . N2B N 0.4516(2) 0.34968(17) 0.60680(16) 0.0222(5) Uani 1 1 d . . . N3B N 0.2072(2) 0.36289(17) 0.60108(17) 0.0245(5) Uani 1 1 d . . . C1B C 0.3685(3) 0.1235(2) 0.3863(2) 0.0233(5) Uani 1 1 d . . . C2B C 0.3946(3) 0.0543(2) 0.2901(2) 0.0324(6) Uani 1 1 d . . . H2B H 0.3346 0.0322 0.2193 0.039 Uiso 1 1 calc R . . C3B C 0.5067(3) 0.0176(2) 0.2966(3) 0.0385(7) Uani 1 1 d . . . H3B H 0.5235 -0.0293 0.2303 0.046 Uiso 1 1 calc R . . C4B C 0.5953(3) 0.0491(2) 0.3998(2) 0.0378(7) Uani 1 1 d . . . H4B H 0.6719 0.0231 0.4044 0.045 Uiso 1 1 calc R . . C5B C 0.5706(3) 0.1185(2) 0.4955(2) 0.0306(6) Uani 1 1 d . . . H5B H 0.6309 0.1400 0.5660 0.037 Uiso 1 1 calc R . . C6B C 0.4590(3) 0.1573(2) 0.4904(2) 0.0236(6) Uani 1 1 d . . . C7B C 0.4357(3) 0.2359(2) 0.5954(2) 0.0242(6) Uani 1 1 d . . . H7B1 H 0.3447 0.2064 0.5949 0.029 Uiso 1 1 calc R . . H7B2 H 0.4997 0.2409 0.6605 0.029 Uiso 1 1 calc R . . C8B C 0.5806(3) 0.3914(2) 0.5933(2) 0.0271(6) Uani 1 1 d . . . H8B1 H 0.6453 0.3544 0.6127 0.033 Uiso 1 1 calc R . . H8B2 H 0.6172 0.4722 0.6444 0.033 Uiso 1 1 calc R . . C9B C 0.5610(2) 0.3688(2) 0.4754(2) 0.0221(5) Uani 1 1 d . . . C10B C 0.6750(3) 0.3592(2) 0.4299(2) 0.0317(6) Uani 1 1 d . . . H10D H 0.6783 0.2821 0.3977 0.048 Uiso 1 1 calc R . . H10E H 0.7581 0.4073 0.4898 0.048 Uiso 1 1 calc R . . H10F H 0.6639 0.3819 0.3721 0.048 Uiso 1 1 calc R . . C11B C 0.4358(3) 0.4263(2) 0.7146(2) 0.0292(6) Uani 1 1 d . . . H11C H 0.4742 0.5041 0.7332 0.035 Uiso 1 1 calc R . . H11D H 0.4840 0.4140 0.7747 0.035 Uiso 1 1 calc R . . C12B C 0.2905(3) 0.4058(2) 0.7059(2) 0.0264(6) Uani 1 1 d . . . C13B C 0.2424(3) 0.4308(2) 0.7955(2) 0.0326(7) Uani 1 1 d . . . H13B H 0.3022 0.4629 0.8687 0.039 Uiso 1 1 calc R . . C14B C 0.1072(3) 0.4089(2) 0.7781(3) 0.0356(7) Uani 1 1 d . . . H14B H 0.0727 0.4255 0.8391 0.043 Uiso 1 1 calc R . . C15B C 0.0220(3) 0.3626(2) 0.6711(2) 0.0346(7) Uani 1 1 d . . . H15B H -0.0718 0.3455 0.6575 0.041 Uiso 1 1 calc R . . C16B C 0.0751(3) 0.3414(2) 0.5842(2) 0.0293(6) Uani 1 1 d . . . H16B H 0.0168 0.3110 0.5107 0.035 Uiso 1 1 calc R . . O1C O 0.0863(4) 0.5745(4) 0.0481(3) 0.0481(12) Uani 0.50 1 d PD A 1 O3D O 0.2137(7) 0.5991(5) 0.1987(5) 0.0506(15) Uani 0.50 1 d PD A 2 O2C O 0.3134(5) 0.5895(5) 0.0921(5) 0.0480(15) Uani 0.50 1 d PD A 1 O2D O 0.3202(4) 0.7622(3) 0.2029(3) 0.0420(11) Uani 0.50 1 d PD A 2 O1D O 0.0971(4) 0.6753(5) 0.1054(5) 0.0735(17) Uani 0.50 1 d PD A 2 O3C O 0.2184(6) 0.6684(6) 0.2324(4) 0.068(2) Uani 0.50 1 d PD A 1 O4D O 0.2576(7) 0.5933(5) 0.0401(4) 0.081(2) Uani 0.50 1 d PD A 2 O4C O 0.2405(5) 0.7445(4) 0.1153(5) 0.0645(15) Uani 0.50 1 d PD A 1 N1S N 0.1404(3) 0.1114(2) 0.6409(2) 0.0531(7) Uani 1 1 d . . . C1S C -0.1056(3) 0.0883(3) 0.6397(3) 0.0554(9) Uani 1 1 d . . . H1S1 H -0.1086 0.1399 0.7133 0.083 Uiso 1 1 calc R . . H1S2 H -0.1466 0.0120 0.6222 0.083 Uiso 1 1 calc R . . H1S3 H -0.1545 0.1042 0.5836 0.083 Uiso 1 1 calc R . . C2S C 0.0338(3) 0.1015(3) 0.6399(3) 0.0399(7) Uani 1 1 d . . . H1B H 0.217(4) 0.153(3) 0.298(3) 0.088(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02072(17) 0.02336(17) 0.01894(16) 0.01079(13) 0.00736(13) 0.00720(13) Cu2 0.01942(17) 0.02456(18) 0.01942(16) 0.01169(13) 0.00716(13) 0.00771(13) Cl1 0.0274(4) 0.0437(4) 0.0333(4) 0.0226(3) 0.0121(3) 0.0099(3) O1A 0.0231(10) 0.0232(9) 0.0243(9) 0.0127(8) 0.0067(8) 0.0070(8) O2A 0.0230(10) 0.0322(10) 0.0177(9) 0.0127(8) 0.0076(7) 0.0112(8) N1A 0.0218(11) 0.0194(11) 0.0205(11) 0.0103(9) 0.0072(9) 0.0063(9) N2A 0.0246(12) 0.0206(11) 0.0233(11) 0.0117(9) 0.0084(9) 0.0075(9) N3A 0.0271(13) 0.0285(12) 0.0258(12) 0.0120(10) 0.0122(10) 0.0075(10) C1A 0.0252(14) 0.0167(13) 0.0226(13) 0.0076(10) 0.0051(11) 0.0037(11) C2A 0.0287(15) 0.0269(15) 0.0326(15) 0.0178(12) 0.0086(12) 0.0053(12) C3A 0.0332(17) 0.0405(18) 0.0441(18) 0.0253(15) 0.0146(14) 0.0041(14) C4A 0.0199(15) 0.0410(18) 0.0480(18) 0.0201(15) 0.0055(13) 0.0009(13) C5A 0.0267(15) 0.0289(15) 0.0288(15) 0.0121(12) -0.0013(12) 0.0029(12) C6A 0.0260(14) 0.0194(13) 0.0233(13) 0.0083(11) 0.0043(11) 0.0048(11) C7A 0.0302(15) 0.0235(14) 0.0222(13) 0.0098(11) 0.0055(11) 0.0086(12) C8A 0.0281(15) 0.0252(14) 0.0245(13) 0.0139(11) 0.0071(11) 0.0132(12) C9A 0.0248(14) 0.0182(13) 0.0261(13) 0.0123(11) 0.0097(11) 0.0090(11) C10A 0.0238(14) 0.0359(16) 0.0353(15) 0.0200(13) 0.0119(12) 0.0136(13) C11A 0.0363(16) 0.0329(16) 0.0279(14) 0.0198(13) 0.0128(12) 0.0113(13) C12A 0.0343(16) 0.0206(14) 0.0249(14) 0.0110(11) 0.0105(12) 0.0028(12) C13A 0.0451(19) 0.0305(16) 0.0308(15) 0.0182(13) 0.0162(14) 0.0087(14) C14A 0.051(2) 0.0357(17) 0.0389(17) 0.0153(14) 0.0297(16) 0.0090(15) C15A 0.0382(18) 0.0396(18) 0.0434(18) 0.0157(15) 0.0241(15) 0.0104(14) C16A 0.0275(16) 0.0360(17) 0.0340(15) 0.0129(13) 0.0122(13) 0.0099(13) O1B 0.0223(10) 0.0235(9) 0.0248(9) 0.0126(8) 0.0049(8) 0.0078(8) O2B 0.0213(9) 0.0336(10) 0.0209(9) 0.0151(8) 0.0087(7) 0.0070(8) N1B 0.0197(11) 0.0212(11) 0.0209(11) 0.0108(9) 0.0070(9) 0.0050(9) N2B 0.0221(11) 0.0234(11) 0.0206(11) 0.0101(9) 0.0065(9) 0.0068(9) N3B 0.0267(12) 0.0262(12) 0.0268(12) 0.0147(10) 0.0112(10) 0.0131(10) C1B 0.0235(14) 0.0206(13) 0.0307(14) 0.0150(11) 0.0106(11) 0.0074(11) C2B 0.0351(17) 0.0288(15) 0.0267(14) 0.0084(12) 0.0067(12) 0.0108(13) C3B 0.0419(19) 0.0343(17) 0.0391(17) 0.0121(14) 0.0182(15) 0.0194(15) C4B 0.0330(17) 0.0404(18) 0.0468(18) 0.0201(15) 0.0175(14) 0.0230(15) C5B 0.0285(15) 0.0339(16) 0.0343(15) 0.0192(13) 0.0084(12) 0.0142(13) C6B 0.0233(14) 0.0238(14) 0.0272(14) 0.0144(11) 0.0094(11) 0.0073(11) C7B 0.0258(14) 0.0282(14) 0.0252(13) 0.0175(12) 0.0075(11) 0.0104(12) C8B 0.0201(14) 0.0274(15) 0.0280(14) 0.0119(12) 0.0021(11) 0.0026(11) C9B 0.0187(13) 0.0203(13) 0.0258(13) 0.0104(11) 0.0062(11) 0.0041(11) C10B 0.0213(14) 0.0413(17) 0.0309(15) 0.0167(13) 0.0075(12) 0.0077(13) C11B 0.0339(16) 0.0344(16) 0.0189(13) 0.0119(12) 0.0068(12) 0.0127(13) C12B 0.0386(16) 0.0228(14) 0.0257(14) 0.0145(11) 0.0137(12) 0.0151(12) C13B 0.052(2) 0.0302(16) 0.0276(14) 0.0175(13) 0.0194(14) 0.0228(14) C14B 0.054(2) 0.0374(17) 0.0413(17) 0.0288(15) 0.0323(16) 0.0281(15) C15B 0.0390(18) 0.0360(17) 0.0513(19) 0.0306(15) 0.0285(15) 0.0206(14) C16B 0.0294(15) 0.0336(16) 0.0340(15) 0.0207(13) 0.0143(12) 0.0129(13) O1C 0.037(3) 0.057(3) 0.033(2) 0.013(2) -0.002(2) 0.008(2) O3D 0.065(4) 0.058(4) 0.043(3) 0.036(3) 0.016(3) 0.021(3) O2C 0.041(3) 0.050(3) 0.061(4) 0.029(3) 0.021(3) 0.022(3) O2D 0.036(3) 0.035(2) 0.033(2) 0.0049(19) 0.008(2) -0.006(2) O1D 0.028(3) 0.117(5) 0.094(4) 0.073(4) 0.003(3) 0.023(3) O3C 0.045(3) 0.125(6) 0.024(3) 0.033(4) 0.009(2) 0.015(4) O4D 0.099(6) 0.064(4) 0.044(4) -0.007(3) 0.054(4) -0.008(4) O4C 0.062(4) 0.046(3) 0.105(5) 0.048(3) 0.033(3) 0.021(3) N1S 0.0416(18) 0.057(2) 0.0614(19) 0.0302(16) 0.0158(15) 0.0114(15) C1S 0.037(2) 0.051(2) 0.081(3) 0.035(2) 0.0130(19) 0.0132(17) C2S 0.044(2) 0.0359(18) 0.0389(17) 0.0211(14) 0.0077(15) 0.0080(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 Cu1 O2B 1.9072(17) . ? Cu1 N1A 1.967(2) . ? Cu1 N3A 2.002(2) . ? Cu1 N2A 2.044(2) . ? Cu1 O1A 2.2513(17) . ? Cu2 O2A 1.9040(17) . ? Cu2 N1B 1.963(2) . ? Cu2 N3B 2.010(2) . ? Cu2 N2B 2.040(2) . ? Cu2 O1B 2.2435(17) . ? Cl1 O4D 1.349(5) . ? Cl1 O3C 1.360(5) . ? Cl1 O4C 1.385(4) . ? Cl1 O1D 1.411(4) . ? Cl1 O3D 1.446(5) . ? Cl1 O2C 1.461(5) . ? Cl1 O1C 1.500(4) . ? Cl1 O2D 1.500(4) . ? O1A C1A 1.339(3) . ? O1A H1B 1.32(4) . ? O2A N1A 1.352(2) . ? N1A C9A 1.291(3) . ? N2A C11A 1.481(3) . ? N2A C8A 1.481(3) . ? N2A C7A 1.504(3) . ? N3A C12A 1.344(3) . ? N3A C16A 1.351(3) . ? C1A C6A 1.403(3) . ? C1A C2A 1.405(3) . ? C2A C3A 1.376(4) . ? C2A H2A 0.9500 . ? C3A C4A 1.390(4) . ? C3A H3A 0.9500 . ? C4A C5A 1.372(4) . ? C4A H4A 0.9500 . ? C5A C6A 1.391(4) . ? C5A H5A 0.9500 . ? C6A C7A 1.496(3) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A C9A 1.505(3) . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C9A C10A 1.486(3) . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C11A C12A 1.500(4) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A C13A 1.377(4) . ? C13A C14A 1.378(4) . ? C13A H13A 0.9500 . ? C14A C15A 1.368(4) . ? C14A H14A 0.9500 . ? C15A C16A 1.377(4) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? O1B C1B 1.352(3) . ? O1B H1B 1.12(4) . ? O2B N1B 1.349(2) . ? N1B C9B 1.291(3) . ? N2B C8B 1.488(3) . ? N2B C11B 1.488(3) . ? N2B C7B 1.499(3) . ? N3B C16B 1.344(3) . ? N3B C12B 1.357(3) . ? C1B C2B 1.392(4) . ? C1B C6B 1.403(4) . ? C2B C3B 1.380(4) . ? C2B H2B 0.9500 . ? C3B C4B 1.393(4) . ? C3B H3B 0.9500 . ? C4B C5B 1.380(4) . ? C4B H4B 0.9500 . ? C5B C6B 1.390(4) . ? C5B H5B 0.9500 . ? C6B C7B 1.506(3) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C8B C9B 1.500(3) . ? C8B H8B1 0.9900 . ? C8B H8B2 0.9900 . ? C9B C10B 1.484(3) . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B C12B 1.503(4) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B C13B 1.378(4) . ? C13B C14B 1.376(4) . ? C13B H13B 0.9500 . ? C14B C15B 1.382(4) . ? C14B H14B 0.9500 . ? C15B C16B 1.383(4) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? N1S C2S 1.121(4) . ? C1S C2S 1.471(5) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2B Cu1 N1A 104.10(8) . . ? O2B Cu1 N3A 86.95(8) . . ? N1A Cu1 N3A 160.24(9) . . ? O2B Cu1 N2A 164.11(8) . . ? N1A Cu1 N2A 83.56(8) . . ? N3A Cu1 N2A 82.02(9) . . ? O2B Cu1 O1A 102.62(7) . . ? N1A Cu1 O1A 84.31(7) . . ? N3A Cu1 O1A 109.56(8) . . ? N2A Cu1 O1A 91.88(7) . . ? O2A Cu2 N1B 105.10(8) . . ? O2A Cu2 N3B 87.73(8) . . ? N1B Cu2 N3B 160.69(9) . . ? O2A Cu2 N2B 165.28(8) . . ? N1B Cu2 N2B 83.37(8) . . ? N3B Cu2 N2B 81.27(8) . . ? O2A Cu2 O1B 100.08(7) . . ? N1B Cu2 O1B 87.05(7) . . ? N3B Cu2 O1B 105.14(8) . . ? N2B Cu2 O1B 92.26(7) . . ? O4D Cl1 O3C 145.0(5) . . ? O4D Cl1 O4C 92.1(4) . . ? O3C Cl1 O4C 116.2(4) . . ? O4D Cl1 O1D 115.7(4) . . ? O3C Cl1 O1D 94.0(4) . . ? O4C Cl1 O1D 70.6(3) . . ? O4D Cl1 O3D 112.8(4) . . ? O3C Cl1 O3D 35.5(3) . . ? O4C Cl1 O3D 151.3(3) . . ? O1D Cl1 O3D 108.2(3) . . ? O4D Cl1 O2C 35.7(3) . . ? O3C Cl1 O2C 110.9(4) . . ? O4C Cl1 O2C 109.9(3) . . ? O1D Cl1 O2C 150.2(3) . . ? O3D Cl1 O2C 85.5(3) . . ? O4D Cl1 O1C 80.3(3) . . ? O3C Cl1 O1C 108.1(3) . . ? O4C Cl1 O1C 107.1(3) . . ? O1D Cl1 O1C 50.8(3) . . ? O3D Cl1 O1C 91.7(3) . . ? O2C Cl1 O1C 103.9(3) . . ? O4D Cl1 O2D 109.4(3) . . ? O3C Cl1 O2D 77.9(3) . . ? O4C Cl1 O2D 50.7(3) . . ? O1D Cl1 O2D 104.9(3) . . ? O3D Cl1 O2D 105.0(3) . . ? O2C Cl1 O2D 96.5(3) . . ? O1C Cl1 O2D 154.6(3) . . ? C1A O1A Cu1 115.05(15) . . ? C1A O1A H1B 115.9(17) . . ? Cu1 O1A H1B 99.9(17) . . ? N1A O2A Cu2 122.93(13) . . ? C9A N1A O2A 116.41(19) . . ? C9A N1A Cu1 115.21(16) . . ? O2A N1A Cu1 125.71(15) . . ? C11A N2A C8A 113.46(19) . . ? C11A N2A C7A 108.99(19) . . ? C8A N2A C7A 111.3(2) . . ? C11A N2A Cu1 106.49(16) . . ? C8A N2A Cu1 107.15(15) . . ? C7A N2A Cu1 109.25(15) . . ? C12A N3A C16A 119.2(2) . . ? C12A N3A Cu1 114.35(18) . . ? C16A N3A Cu1 126.38(19) . . ? O1A C1A C6A 119.7(2) . . ? O1A C1A C2A 121.8(2) . . ? C6A C1A C2A 118.5(2) . . ? C3A C2A C1A 120.4(3) . . ? C3A C2A H2A 119.8 . . ? C1A C2A H2A 119.8 . . ? C2A C3A C4A 121.0(3) . . ? C2A C3A H3A 119.5 . . ? C4A C3A H3A 119.5 . . ? C5A C4A C3A 118.8(3) . . ? C5A C4A H4A 120.6 . . ? C3A C4A H4A 120.6 . . ? C4A C5A C6A 121.7(3) . . ? C4A C5A H5A 119.1 . . ? C6A C5A H5A 119.1 . . ? C5A C6A C1A 119.5(2) . . ? C5A C6A C7A 120.8(2) . . ? C1A C6A C7A 119.7(2) . . ? C6A C7A N2A 113.3(2) . . ? C6A C7A H7A1 108.9 . . ? N2A C7A H7A1 108.9 . . ? C6A C7A H7A2 108.9 . . ? N2A C7A H7A2 108.9 . . ? H7A1 C7A H7A2 107.7 . . ? N2A C8A C9A 110.0(2) . . ? N2A C8A H8A1 109.7 . . ? C9A C8A H8A1 109.7 . . ? N2A C8A H8A2 109.7 . . ? C9A C8A H8A2 109.7 . . ? H8A1 C8A H8A2 108.2 . . ? N1A C9A C10A 122.7(2) . . ? N1A C9A C8A 115.9(2) . . ? C10A C9A C8A 121.4(2) . . ? C9A C10A H10A 109.5 . . ? C9A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C9A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? N2A C11A C12A 110.2(2) . . ? N2A C11A H11A 109.6 . . ? C12A C11A H11A 109.6 . . ? N2A C11A H11B 109.6 . . ? C12A C11A H11B 109.6 . . ? H11A C11A H11B 108.1 . . ? N3A C12A C13A 121.4(3) . . ? N3A C12A C11A 115.1(2) . . ? C13A C12A C11A 123.5(3) . . ? C12A C13A C14A 119.4(3) . . ? C12A C13A H13A 120.3 . . ? C14A C13A H13A 120.3 . . ? C15A C14A C13A 119.1(3) . . ? C15A C14A H14A 120.5 . . ? C13A C14A H14A 120.5 . . ? C14A C15A C16A 119.7(3) . . ? C14A C15A H15A 120.1 . . ? C16A C15A H15A 120.1 . . ? N3A C16A C15A 121.1(3) . . ? N3A C16A H16A 119.4 . . ? C15A C16A H16A 119.4 . . ? C1B O1B Cu2 113.87(15) . . ? C1B O1B H1B 110(2) . . ? Cu2 O1B H1B 99(2) . . ? N1B O2B Cu1 122.88(14) . . ? C9B N1B O2B 116.5(2) . . ? C9B N1B Cu2 115.90(17) . . ? O2B N1B Cu2 126.22(15) . . ? C8B N2B C11B 112.3(2) . . ? C8B N2B C7B 111.0(2) . . ? C11B N2B C7B 110.17(19) . . ? C8B N2B Cu2 108.15(15) . . ? C11B N2B Cu2 105.64(15) . . ? C7B N2B Cu2 109.35(15) . . ? C16B N3B C12B 119.2(2) . . ? C16B N3B Cu2 126.95(18) . . ? C12B N3B Cu2 113.79(17) . . ? O1B C1B C2B 121.7(2) . . ? O1B C1B C6B 119.1(2) . . ? C2B C1B C6B 119.2(2) . . ? C3B C2B C1B 120.7(3) . . ? C3B C2B H2B 119.7 . . ? C1B C2B H2B 119.7 . . ? C2B C3B C4B 120.3(3) . . ? C2B C3B H3B 119.9 . . ? C4B C3B H3B 119.9 . . ? C5B C4B C3B 119.3(3) . . ? C5B C4B H4B 120.4 . . ? C3B C4B H4B 120.4 . . ? C4B C5B C6B 121.2(3) . . ? C4B C5B H5B 119.4 . . ? C6B C5B H5B 119.4 . . ? C5B C6B C1B 119.3(2) . . ? C5B C6B C7B 120.6(2) . . ? C1B C6B C7B 120.1(2) . . ? N2B C7B C6B 111.9(2) . . ? N2B C7B H7B1 109.2 . . ? C6B C7B H7B1 109.2 . . ? N2B C7B H7B2 109.2 . . ? C6B C7B H7B2 109.2 . . ? H7B1 C7B H7B2 107.9 . . ? N2B C8B C9B 110.2(2) . . ? N2B C8B H8B1 109.6 . . ? C9B C8B H8B1 109.6 . . ? N2B C8B H8B2 109.6 . . ? C9B C8B H8B2 109.6 . . ? H8B1 C8B H8B2 108.1 . . ? N1B C9B C10B 124.0(2) . . ? N1B C9B C8B 116.7(2) . . ? C10B C9B C8B 119.4(2) . . ? C9B C10B H10D 109.5 . . ? C9B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C9B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? N2B C11B C12B 109.6(2) . . ? N2B C11B H11C 109.8 . . ? C12B C11B H11C 109.8 . . ? N2B C11B H11D 109.8 . . ? C12B C11B H11D 109.8 . . ? H11C C11B H11D 108.2 . . ? N3B C12B C13B 121.3(3) . . ? N3B C12B C11B 114.5(2) . . ? C13B C12B C11B 124.2(3) . . ? C14B C13B C12B 119.4(3) . . ? C14B C13B H13B 120.3 . . ? C12B C13B H13B 120.3 . . ? C13B C14B C15B 119.4(3) . . ? C13B C14B H14B 120.3 . . ? C15B C14B H14B 120.3 . . ? C14B C15B C16B 119.0(3) . . ? C14B C15B H15B 120.5 . . ? C16B C15B H15B 120.5 . . ? N3B C16B C15B 121.6(3) . . ? N3B C16B H16B 119.2 . . ? C15B C16B H16B 119.2 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? N1S C2S C1S 179.4(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.417 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.072