# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'Xiao-Liang Tang' _publ_contact_author_name 'Xiao-Liang Tang' _publ_contact_author_email tangxl0308@yahoo.com.cn data_complex-1 _database_code_depnum_ccdc_archive 'CCDC 676484' #TrackingRef '- complexes.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H15 Ag N8 O3' _chemical_formula_weight 475.23 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' Ag Ag -0.8971 1.1015 '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 9.7616(13) _cell_length_b 9.9673(13) _cell_length_c 11.530(3) _cell_angle_alpha 104.062(3) _cell_angle_beta 99.128(3) _cell_angle_gamma 115.917(2) _cell_volume 932.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2529 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 0.759 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 4777 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.20 _reflns_number_total 3329 _reflns_number_gt 2790 _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^)+(0.0370P)^2^+0.4800P] 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 3329 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Ag1 Ag 0.87270(3) 0.62322(3) 0.72744(3) 0.06994(13) Uani 1 1 d . . . C1 C 0.8446(4) 0.8786(3) 0.6148(3) 0.0470(7) Uani 1 1 d . . . C2 C 0.6822(4) 0.7804(4) 0.5460(3) 0.0596(8) Uani 1 1 d . . . H2 H 0.6259 0.6746 0.5402 0.072 Uiso 1 1 calc R . . C3 C 0.6113(4) 0.8478(4) 0.4883(3) 0.0648(9) Uani 1 1 d . . . H3 H 0.5038 0.7864 0.4416 0.078 Uiso 1 1 calc R . . C4 C 0.6963(5) 1.0079(4) 0.4973(3) 0.0641(9) Uani 1 1 d . . . H4 H 0.6424 1.0486 0.4564 0.077 Uiso 1 1 calc R . . C5 C 0.8545(4) 1.1062(4) 0.5636(3) 0.0530(7) Uani 1 1 d . . . H5 H 0.9096 1.2120 0.5692 0.064 Uiso 1 1 calc R . . C6 C 0.9283(4) 1.0367(3) 0.6228(3) 0.0436(6) Uani 1 1 d . . . C7 C 1.2153(4) 1.2543(4) 0.7482(3) 0.0550(8) Uani 1 1 d . . . H7A H 1.2128 1.3089 0.6894 0.066 Uiso 1 1 calc R . . H7B H 1.3134 1.2494 0.7596 0.066 Uiso 1 1 calc R . . C8 C 1.2142(3) 1.3473(4) 0.8722(3) 0.0516(7) Uani 1 1 d . . . H8A H 1.2177 1.2930 0.9310 0.062 Uiso 1 1 calc R . . H8B H 1.3092 1.4519 0.9058 0.062 Uiso 1 1 calc R . . C9 C 0.8410(3) 1.3489(3) 0.8513(3) 0.0433(6) Uani 1 1 d . . . C10 C 0.6876(4) 1.2936(4) 0.8641(3) 0.0571(8) Uani 1 1 d . . . H10 H 0.6249 1.3374 0.8426 0.069 Uiso 1 1 calc R . . C11 C 0.6346(4) 1.1720(4) 0.9098(3) 0.0675(9) Uani 1 1 d . . . H11 H 0.5338 1.1334 0.9209 0.081 Uiso 1 1 calc R . . C12 C 0.7278(5) 1.1030(4) 0.9408(3) 0.0672(9) Uani 1 1 d . . . H12 H 0.6855 1.0186 0.9697 0.081 Uiso 1 1 calc R . . C13 C 0.8782(4) 1.1562(3) 0.9297(3) 0.0538(7) Uani 1 1 d . . . H13 H 0.9396 1.1109 0.9507 0.065 Uiso 1 1 calc R . . C14 C 0.9345(3) 1.2823(3) 0.8851(2) 0.0401(6) Uani 1 1 d . . . C15 C 0.6872(5) 0.2441(5) 0.2809(4) 0.0793(11) Uani 1 1 d . . . H15A H 0.5772 0.1661 0.2632 0.119 Uiso 1 1 calc R . . H15B H 0.7510 0.1932 0.2807 0.119 Uiso 1 1 calc R . . H15C H 0.6974 0.2926 0.2180 0.119 Uiso 1 1 calc R . . C16 C 0.7405(5) 0.3636(5) 0.4015(4) 0.0734(10) Uani 1 1 d . . . N1 N 0.9492(3) 0.8479(3) 0.6831(2) 0.0526(6) Uani 1 1 d . . . N2 N 1.0892(3) 0.9774(3) 0.7329(2) 0.0529(6) Uani 1 1 d . . . N3 N 1.0784(3) 1.0926(3) 0.6961(2) 0.0469(6) Uani 1 1 d . . . N4 N 0.9288(3) 1.4668(3) 0.8085(2) 0.0475(6) Uani 1 1 d . . . N5 N 1.0672(3) 1.4750(3) 0.8141(2) 0.0468(6) Uani 1 1 d . . . N6 N 1.0731(3) 1.3657(3) 0.8608(2) 0.0425(5) Uani 1 1 d . . . N7 N 0.6197(3) 0.6565(4) 0.8421(3) 0.0592(7) Uani 1 1 d . . . N8 N 0.7791(7) 0.4539(6) 0.4955(4) 0.1258(16) Uani 1 1 d . . . O1 O 0.7636(3) 0.7580(3) 0.8777(3) 0.0798(7) Uani 1 1 d . . . O2 O 0.5688(4) 0.5392(4) 0.7485(3) 0.1073(10) Uani 1 1 d . . . O3 O 0.5359(3) 0.6787(4) 0.9063(3) 0.0938(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 Ag1 0.0827(2) 0.06009(19) 0.0978(2) 0.04575(16) 0.03834(17) 0.04798(16) C1 0.0586(19) 0.0430(16) 0.0513(16) 0.0198(14) 0.0254(15) 0.0305(15) C2 0.061(2) 0.0498(18) 0.066(2) 0.0192(16) 0.0227(17) 0.0255(17) C3 0.058(2) 0.073(2) 0.057(2) 0.0172(18) 0.0104(16) 0.0325(18) C4 0.078(3) 0.076(2) 0.060(2) 0.0302(18) 0.0215(18) 0.053(2) C5 0.069(2) 0.0518(18) 0.0561(18) 0.0268(15) 0.0279(17) 0.0378(17) C6 0.0525(18) 0.0429(15) 0.0436(15) 0.0152(13) 0.0220(14) 0.0281(14) C7 0.0459(17) 0.0480(17) 0.080(2) 0.0270(16) 0.0287(16) 0.0251(15) C8 0.0414(16) 0.0462(16) 0.0638(19) 0.0191(15) 0.0107(14) 0.0208(14) C9 0.0497(17) 0.0355(14) 0.0412(15) 0.0069(12) 0.0142(13) 0.0216(13) C10 0.0473(18) 0.0512(18) 0.068(2) 0.0094(16) 0.0210(16) 0.0251(15) C11 0.056(2) 0.053(2) 0.080(2) 0.0121(18) 0.0341(18) 0.0166(17) C12 0.074(2) 0.0487(19) 0.075(2) 0.0257(17) 0.039(2) 0.0198(18) C13 0.066(2) 0.0421(16) 0.0557(18) 0.0215(14) 0.0211(16) 0.0261(15) C14 0.0439(16) 0.0311(13) 0.0388(14) 0.0087(11) 0.0117(12) 0.0153(12) C15 0.094(3) 0.065(2) 0.073(2) 0.032(2) 0.023(2) 0.031(2) C16 0.079(3) 0.060(2) 0.070(3) 0.023(2) 0.009(2) 0.030(2) N1 0.0593(17) 0.0444(14) 0.0663(16) 0.0251(13) 0.0247(13) 0.0310(14) N2 0.0572(16) 0.0466(14) 0.0699(17) 0.0259(13) 0.0262(13) 0.0330(13) N3 0.0523(15) 0.0417(13) 0.0589(15) 0.0213(12) 0.0249(12) 0.0288(12) N4 0.0539(15) 0.0385(13) 0.0561(14) 0.0180(11) 0.0201(12) 0.0262(12) N5 0.0547(15) 0.0375(12) 0.0547(14) 0.0215(11) 0.0206(12) 0.0241(11) N6 0.0460(14) 0.0360(12) 0.0473(13) 0.0159(10) 0.0152(11) 0.0208(11) N7 0.0545(18) 0.0621(18) 0.077(2) 0.0394(17) 0.0223(15) 0.0335(16) N8 0.164(5) 0.098(3) 0.082(3) 0.005(3) 0.011(3) 0.060(3) O1 0.0585(16) 0.0868(19) 0.0877(18) 0.0361(15) 0.0290(14) 0.0257(15) O2 0.107(2) 0.073(2) 0.101(2) 0.0064(19) 0.0117(19) 0.0297(18) O3 0.0722(18) 0.110(2) 0.137(3) 0.063(2) 0.0616(19) 0.0560(17) _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 Ag1 N4 2.213(2) 1_545 ? Ag1 N1 2.247(2) . ? Ag1 N8 2.553(5) . ? Ag1 O1 2.578(3) . ? C1 N1 1.375(4) . ? C1 C6 1.393(4) . ? C1 C2 1.402(5) . ? C2 C3 1.361(5) . ? C2 H2 0.9300 . ? C3 C4 1.407(5) . ? C3 H3 0.9300 . ? C4 C5 1.367(5) . ? C4 H4 0.9300 . ? C5 C6 1.405(4) . ? C5 H5 0.9300 . ? C6 N3 1.355(4) . ? C7 N3 1.462(4) . ? C7 C8 1.508(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N6 1.457(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N4 1.376(4) . ? C9 C10 1.399(4) . ? C9 C14 1.404(4) . ? C10 C11 1.365(5) . ? C10 H10 0.9300 . ? C11 C12 1.412(5) . ? C11 H11 0.9300 . ? C12 C13 1.366(5) . ? C12 H12 0.9300 . ? C13 C14 1.395(4) . ? C13 H13 0.9300 . ? C14 N6 1.361(4) . ? C15 C16 1.430(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N8 1.108(5) . ? N1 N2 1.309(4) . ? N2 N3 1.356(3) . ? N4 N5 1.307(3) . ? N4 Ag1 2.213(2) 1_565 ? N5 N6 1.345(3) . ? N7 O2 1.220(4) . ? N7 O1 1.240(4) . ? N7 O3 1.240(4) . ? 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 Ag1 N1 151.17(10) 1_545 . ? N4 Ag1 N8 98.65(12) 1_545 . ? N1 Ag1 N8 91.62(13) . . ? N4 Ag1 O1 107.83(9) 1_545 . ? N1 Ag1 O1 81.42(9) . . ? N8 Ag1 O1 136.75(14) . . ? N1 C1 C6 107.7(3) . . ? N1 C1 C2 130.9(3) . . ? C6 C1 C2 121.4(3) . . ? C3 C2 C1 116.6(3) . . ? C3 C2 H2 121.7 . . ? C1 C2 H2 121.7 . . ? C2 C3 C4 121.8(3) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 122.9(3) . . ? C5 C4 H4 118.5 . . ? C3 C4 H4 118.5 . . ? C4 C5 C6 115.5(3) . . ? C4 C5 H5 122.3 . . ? C6 C5 H5 122.3 . . ? N3 C6 C1 104.6(2) . . ? N3 C6 C5 133.4(3) . . ? C1 C6 C5 121.9(3) . . ? N3 C7 C8 111.5(2) . . ? N3 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N3 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N6 C8 C7 112.3(2) . . ? N6 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N6 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N4 C9 C10 131.5(3) . . ? N4 C9 C14 107.5(2) . . ? C10 C9 C14 121.0(3) . . ? C11 C10 C9 116.6(3) . . ? C11 C10 H10 121.7 . . ? C9 C10 H10 121.7 . . ? C10 C11 C12 122.2(3) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 122.0(3) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 116.3(3) . . ? C12 C13 H13 121.9 . . ? C14 C13 H13 121.9 . . ? N6 C14 C13 133.8(3) . . ? N6 C14 C9 104.2(2) . . ? C13 C14 C9 122.0(3) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N8 C16 C15 178.5(5) . . ? N2 N1 C1 109.2(2) . . ? N2 N1 Ag1 126.50(19) . . ? C1 N1 Ag1 123.4(2) . . ? N1 N2 N3 107.8(2) . . ? C6 N3 N2 110.7(2) . . ? C6 N3 C7 130.0(2) . . ? N2 N3 C7 118.9(2) . . ? N5 N4 C9 109.1(2) . . ? N5 N4 Ag1 118.35(17) . 1_565 ? C9 N4 Ag1 132.5(2) . 1_565 ? N4 N5 N6 108.4(2) . . ? N5 N6 C14 110.8(2) . . ? N5 N6 C8 119.0(2) . . ? C14 N6 C8 130.0(2) . . ? O2 N7 O1 118.9(3) . . ? O2 N7 O3 123.5(3) . . ? O1 N7 O3 117.5(3) . . ? C16 N8 Ag1 169.2(4) . . ? N7 O1 Ag1 101.8(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.333 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.055 ################################## data_complex-2 _database_code_depnum_ccdc_archive 'CCDC 676485' #TrackingRef '- complexes-R.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Ag2 N20 O9' _chemical_formula_weight 1264.80 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 15.282(2) _cell_length_b 15.282(2) _cell_length_c 40.377(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8166.7(17) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2854 _cell_measurement_theta_min 2.536 _cell_measurement_theta_max 21.843 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3852 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8086 _exptl_absorpt_correction_T_max 0.8971 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11063 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1545 _reflns_number_gt 962 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1357P)^2^+16.7500P] 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 1545 _refine_ls_number_parameters 127 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.2109 _refine_ls_wR_factor_gt 0.1886 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.061 _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 Ag1 Ag 0.3333 0.6667 0.45612(2) 0.0690(5) Uani 1 3 d S . . N1 N 0.3964(4) 0.8344(4) 0.45509(13) 0.0676(14) Uani 1 1 d . . . N2 N 0.4950(4) 0.8945(4) 0.45357(13) 0.0727(15) Uani 1 1 d . . . N3 N 0.5126(4) 0.9893(4) 0.45627(11) 0.0704(15) Uani 1 1 d . . . N4 N 0.3333(4) 0.6667(4) 0.56492(11) 0.134(7) Uani 0.50 3 d SPRU . 1 O2 O 0.2818(4) 0.6939(4) 0.56493(11) 0.205(8) Uani 0.50 1 d PRU . 1 N4' N 0.3333(4) 0.6667(4) 0.53213(11) 0.106(6) Uani 0.50 3 d SPRU . 2 O2' O 0.2871(4) 0.7003(4) 0.53209(11) 0.205(8) Uani 0.50 1 d PRU . 2 C1 C 0.4247(6) 0.9911(4) 0.45904(12) 0.0660(17) Uani 1 1 d . . . C2 C 0.3487(5) 0.8914(5) 0.45842(12) 0.0632(16) Uani 1 1 d . . . C3 C 0.2492(5) 0.8630(6) 0.46077(15) 0.0746(18) Uani 1 1 d . . . H3 H 0.1989 0.7956 0.4594 0.090 Uiso 1 1 calc R . . C4 C 0.2266(7) 0.9372(6) 0.46511(18) 0.089(2) Uani 1 1 d . . . H4 H 0.1592 0.9197 0.4674 0.106 Uiso 1 1 calc R . . C5 C 0.3020(8) 1.0405(7) 0.4663(2) 0.100(3) Uani 1 1 d . . . H5 H 0.2830 1.0889 0.4698 0.120 Uiso 1 1 calc R . . C6 C 0.4044(7) 1.0717(6) 0.46212(19) 0.093(2) Uani 1 1 d . . . H6 H 0.4548 1.1393 0.4615 0.111 Uiso 1 1 calc R . . C7 C 0.6191(7) 1.0723(5) 0.45553(18) 0.096(3) Uani 1 1 d D . . H7A H 0.6211 1.1330 0.4637 0.115 Uiso 1 1 calc R . . H7B H 0.6572 1.0557 0.4710 0.115 Uiso 1 1 calc R . . C8 C 0.6698(9) 1.0957(9) 0.4246(3) 0.158(4) Uani 1 1 d DU . . H8A H 0.6304 1.1058 0.4078 0.190 Uiso 1 1 calc R . . H8B H 0.7353 1.1566 0.4263 0.190 Uiso 1 1 calc R . . O1 O 0.6809(8) 1.0143(8) 0.4167 0.176(4) Uani 1 2 d SDU . . 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 Ag1 0.0566(5) 0.0566(5) 0.0938(8) 0.000 0.000 0.0283(2) N1 0.071(3) 0.056(3) 0.075(3) 0.004(2) 0.003(2) 0.031(3) N2 0.073(4) 0.058(3) 0.078(3) 0.001(2) -0.003(3) 0.027(3) N3 0.079(4) 0.062(4) 0.061(3) -0.003(2) 0.005(2) 0.028(3) N4 0.125(7) 0.125(7) 0.152(11) 0.000 0.000 0.062(4) O2 0.188(11) 0.205(11) 0.218(11) 0.004(9) -0.006(8) 0.095(8) N4' 0.094(7) 0.094(7) 0.130(10) 0.000 0.000 0.047(3) O2' 0.203(11) 0.197(10) 0.199(11) -0.026(8) 0.016(8) 0.089(8) C1 0.099(5) 0.053(4) 0.045(3) 0.001(2) 0.003(3) 0.038(3) C2 0.084(4) 0.070(4) 0.042(3) 0.000(2) -0.004(3) 0.043(4) C3 0.079(5) 0.076(4) 0.072(4) -0.011(3) -0.007(3) 0.042(4) C4 0.096(5) 0.101(6) 0.089(5) -0.009(4) 0.001(4) 0.064(5) C5 0.134(8) 0.100(6) 0.095(6) -0.006(4) 0.004(5) 0.081(6) C6 0.126(7) 0.066(4) 0.088(5) -0.007(4) -0.004(5) 0.049(5) C7 0.111(6) 0.058(4) 0.076(4) -0.018(3) 0.006(4) 0.010(4) C8 0.136(7) 0.157(8) 0.133(7) -0.013(6) 0.007(6) 0.037(6) O1 0.150(5) 0.150(5) 0.175(8) -0.045(4) 0.045(4) 0.035(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.243(5) . ? Ag1 N1 2.243(5) 2_665 ? Ag1 N1 2.243(5) 3_565 ? Ag1 Ag1 3.1860(18) 10_455 ? N1 N2 1.316(8) . ? N1 C2 1.394(8) . ? N2 N3 1.338(7) . ? N3 C1 1.362(9) . ? N3 C7 1.481(9) . ? N4 O2 1.0589 . ? N4 O2 1.059(10) 3_565 ? N4 O2 1.059(10) 2_665 ? N4' O2' 1.0617 . ? N4' O2' 1.062(10) 3_565 ? N4' O2' 1.062(10) 2_665 ? C1 C2 1.379(9) . ? C1 C6 1.419(10) . ? C2 C3 1.360(9) . ? C3 C4 1.350(10) . ? C3 H3 0.9300 . ? C4 C5 1.416(12) . ? C4 H4 0.9300 . ? C5 C6 1.400(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.419(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.374(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O1 C8 1.374(12) 10_455 ? 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 N1 Ag1 N1 119.966(9) . 2_665 ? N1 Ag1 N1 119.966(11) . 3_565 ? N1 Ag1 N1 119.966(10) 2_665 3_565 ? N1 Ag1 Ag1 88.94(14) . 10_455 ? N1 Ag1 Ag1 88.94(14) 2_665 10_455 ? N1 Ag1 Ag1 88.94(14) 3_565 10_455 ? N2 N1 C2 110.0(5) . . ? N2 N1 Ag1 119.1(4) . . ? C2 N1 Ag1 130.7(4) . . ? N1 N2 N3 107.0(5) . . ? N2 N3 C1 111.2(5) . . ? N2 N3 C7 117.8(6) . . ? C1 N3 C7 131.0(6) . . ? O2 N4 O2 120.0(5) . 3_565 ? O2 N4 O2 120.0(5) . 2_665 ? O2 N4 O2 120.0(6) 3_565 2_665 ? O2' N4' O2' 120.0(5) . 3_565 ? O2' N4' O2' 120.0(5) . 2_665 ? O2' N4' O2' 120.0(6) 3_565 2_665 ? N3 C1 C2 105.7(5) . . ? N3 C1 C6 132.1(7) . . ? C2 C1 C6 122.1(8) . . ? C3 C2 C1 122.7(7) . . ? C3 C2 N1 131.2(6) . . ? C1 C2 N1 106.1(6) . . ? C4 C3 C2 117.1(7) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C3 C4 C5 122.2(8) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 121.6(7) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 114.0(7) . . ? C5 C6 H6 123.0 . . ? C1 C6 H6 123.0 . . ? C8 C7 N3 117.5(7) . . ? C8 C7 H7A 107.9 . . ? N3 C7 H7A 107.9 . . ? C8 C7 H7B 107.9 . . ? N3 C7 H7B 107.9 . . ? H7A C7 H7B 107.2 . . ? O1 C8 C7 106.0(9) . . ? O1 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? O1 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? C8 O1 C8 134.0(14) 10_455 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 N2 -175.7(3) 2_665 . . . ? N1 Ag1 N1 N2 0.6(6) 3_565 . . . ? Ag1 Ag1 N1 N2 -87.5(4) 10_455 . . . ? N1 Ag1 N1 C2 10.1(7) 2_665 . . . ? N1 Ag1 N1 C2 -173.6(3) 3_565 . . . ? Ag1 Ag1 N1 C2 98.2(5) 10_455 . . . ? C2 N1 N2 N3 0.8(6) . . . . ? Ag1 N1 N2 N3 -174.6(4) . . . . ? N1 N2 N3 C1 -1.0(6) . . . . ? N1 N2 N3 C7 179.5(5) . . . . ? N2 N3 C1 C2 0.8(6) . . . . ? C7 N3 C1 C2 -179.9(6) . . . . ? N2 N3 C1 C6 -179.3(6) . . . . ? C7 N3 C1 C6 0.1(10) . . . . ? N3 C1 C2 C3 179.8(5) . . . . ? C6 C1 C2 C3 -0.1(8) . . . . ? N3 C1 C2 N1 -0.3(5) . . . . ? C6 C1 C2 N1 179.8(6) . . . . ? N2 N1 C2 C3 179.6(6) . . . . ? Ag1 N1 C2 C3 -5.7(9) . . . . ? N2 N1 C2 C1 -0.3(6) . . . . ? Ag1 N1 C2 C1 174.3(4) . . . . ? C1 C2 C3 C4 -2.5(9) . . . . ? N1 C2 C3 C4 177.5(6) . . . . ? C2 C3 C4 C5 1.8(10) . . . . ? C3 C4 C5 C6 1.6(12) . . . . ? C4 C5 C6 C1 -4.0(11) . . . . ? N3 C1 C6 C5 -176.5(6) . . . . ? C2 C1 C6 C5 3.3(9) . . . . ? N2 N3 C7 C8 73.3(11) . . . . ? C1 N3 C7 C8 -106.1(10) . . . . ? N3 C7 C8 O1 -68.1(13) . . . . ? C7 C8 O1 C8 -124.9(9) . . . 10_455 ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 2.411 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.115 # Attachment 'complex-3.cif' data_p21c _database_code_depnum_ccdc_archive 'CCDC 676486' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Ag N7 O5' _chemical_formula_weight 522.28 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.302(4) _cell_length_b 9.866(3) _cell_length_c 19.300(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.972(15) _cell_angle_gamma 90.00 _cell_volume 2047.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3687 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.65 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 11391 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.85 _reflns_number_total 4367 _reflns_number_gt 3344 _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^)+(0.0400P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4367 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Ag1 Ag -0.35507(2) 1.10689(2) 0.994821(12) 0.05831(11) Uani 1 1 d . . . C1 C -0.2359(2) 1.0652(2) 0.86876(12) 0.0399(5) Uani 1 1 d . . . C2 C -0.3055(2) 1.1678(3) 0.82440(14) 0.0512(6) Uani 1 1 d . . . H2 H -0.3737 1.2071 0.8338 0.061 Uiso 1 1 calc R . . C3 C -0.2683(2) 1.2069(3) 0.76699(14) 0.0585(7) Uani 1 1 d . . . H3 H -0.3110 1.2762 0.7368 0.070 Uiso 1 1 calc R . . C4 C -0.1672(3) 1.1453(3) 0.75220(14) 0.0606(7) Uani 1 1 d . . . H4 H -0.1458 1.1747 0.7118 0.073 Uiso 1 1 calc R . . C5 C -0.0982(2) 1.0442(3) 0.79414(14) 0.0519(6) Uani 1 1 d . . . H5 H -0.0315 1.0037 0.7835 0.062 Uiso 1 1 calc R . . C6 C -0.1348(2) 1.0060(2) 0.85421(12) 0.0384(5) Uani 1 1 d . . . C7 C 0.0169(2) 0.8256(2) 0.92239(15) 0.0532(6) Uani 1 1 d . . . H7A H 0.0489 0.8042 0.9739 0.064 Uiso 1 1 calc R . . H7B H 0.0825 0.8709 0.9086 0.064 Uiso 1 1 calc R . . C8 C -0.0168(2) 0.6959(2) 0.87966(16) 0.0540(6) Uani 1 1 d . . . H8A H -0.0571 0.7160 0.8286 0.065 Uiso 1 1 calc R . . H8B H 0.0575 0.6432 0.8838 0.065 Uiso 1 1 calc R . . C9 C -0.1288(2) 0.4907(2) 0.87668(14) 0.0509(6) Uani 1 1 d . . . H9A H -0.1559 0.4993 0.8240 0.061 Uiso 1 1 calc R . . H9B H -0.1980 0.4548 0.8907 0.061 Uiso 1 1 calc R . . C10 C -0.0230(2) 0.3917(2) 0.89898(14) 0.0443(6) Uani 1 1 d . . . H10A H 0.0229 0.4046 0.9500 0.053 Uiso 1 1 calc R . . H10B H -0.0554 0.2999 0.8928 0.053 Uiso 1 1 calc R . . C11 C 0.1570(2) 0.3155(2) 0.87222(13) 0.0454(6) Uani 1 1 d . . . H11A H 0.1919 0.3142 0.8322 0.054 Uiso 1 1 calc R . . H11B H 0.1241 0.2259 0.8758 0.054 Uiso 1 1 calc R . . C12 C 0.2599(2) 0.3456(2) 0.94196(14) 0.0468(6) Uani 1 1 d . . . H12A H 0.2254 0.3472 0.9822 0.056 Uiso 1 1 calc R . . H12B H 0.3211 0.2734 0.9511 0.056 Uiso 1 1 calc R . . C13 C 0.40230(19) 0.5078(2) 0.90238(12) 0.0404(5) Uani 1 1 d . . . C14 C 0.4516(2) 0.4358(3) 0.85492(14) 0.0508(6) Uani 1 1 d . . . H14 H 0.4309 0.3458 0.8425 0.061 Uiso 1 1 calc R . . C15 C 0.5319(2) 0.5066(3) 0.82816(15) 0.0575(7) Uani 1 1 d . . . H15 H 0.5660 0.4634 0.7960 0.069 Uiso 1 1 calc R . . C16 C 0.5651(2) 0.6425(3) 0.84736(15) 0.0558(7) Uani 1 1 d . . . H16 H 0.6214 0.6852 0.8282 0.067 Uiso 1 1 calc R . . C17 C 0.5171(2) 0.7128(3) 0.89314(13) 0.0478(6) Uani 1 1 d . . . H17 H 0.5390 0.8025 0.9056 0.057 Uiso 1 1 calc R . . C18 C 0.4329(2) 0.6429(2) 0.92055(12) 0.0396(5) Uani 1 1 d . . . O1 O -0.09813(16) 0.62233(15) 0.90822(10) 0.0517(4) Uani 1 1 d . . . O2 O 0.05813(14) 0.41029(14) 0.85625(9) 0.0422(4) Uani 1 1 d . . . O3 O -0.41448(18) 0.9482(2) 1.07406(11) 0.0676(5) Uani 1 1 d . . . O4 O -0.24953(19) 1.0340(2) 1.14724(12) 0.0787(6) Uani 1 1 d . . . O5 O -0.3610(3) 0.9008(2) 1.18817(13) 0.0999(9) Uani 1 1 d . . . N1 N -0.24586(18) 1.00956(19) 0.93203(11) 0.0462(5) Uani 1 1 d . . . N2 N -0.1557(2) 0.92043(19) 0.95663(12) 0.0487(5) Uani 1 1 d . . . N3 N -0.08895(19) 0.91722(18) 0.91017(11) 0.0441(5) Uani 1 1 d . . . N4 N 0.32115(16) 0.47491(18) 0.93910(10) 0.0406(4) Uani 1 1 d . . . N5 N 0.30068(19) 0.58205(19) 0.97700(11) 0.0452(5) Uani 1 1 d . . . N6 N 0.36791(17) 0.68388(19) 0.96626(10) 0.0431(4) Uani 1 1 d . . . N7 N -0.3416(2) 0.9619(2) 1.13764(12) 0.0496(5) 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 Ag1 0.06265(16) 0.05304(15) 0.07249(17) -0.01612(10) 0.04027(12) -0.00469(9) C1 0.0402(12) 0.0373(12) 0.0447(13) -0.0087(10) 0.0167(10) -0.0045(10) C2 0.0424(13) 0.0516(15) 0.0577(16) -0.0036(13) 0.0125(12) 0.0035(12) C3 0.0581(16) 0.0603(17) 0.0495(15) 0.0052(13) 0.0057(13) -0.0015(14) C4 0.0727(19) 0.0715(18) 0.0403(15) -0.0025(13) 0.0212(13) -0.0128(16) C5 0.0528(15) 0.0572(16) 0.0528(15) -0.0116(13) 0.0267(12) -0.0044(13) C6 0.0398(12) 0.0349(12) 0.0433(13) -0.0093(10) 0.0171(10) -0.0042(10) C7 0.0417(13) 0.0442(14) 0.0752(18) -0.0013(13) 0.0203(12) 0.0052(11) C8 0.0535(15) 0.0408(13) 0.0770(18) -0.0007(13) 0.0337(13) 0.0080(12) C9 0.0376(13) 0.0484(14) 0.0665(17) -0.0107(12) 0.0155(12) -0.0044(11) C10 0.0444(13) 0.0423(13) 0.0487(14) -0.0017(10) 0.0182(11) -0.0014(10) C11 0.0401(12) 0.0358(13) 0.0603(15) -0.0078(11) 0.0155(11) 0.0032(10) C12 0.0388(12) 0.0361(12) 0.0605(16) 0.0041(11) 0.0082(11) 0.0024(10) C13 0.0322(11) 0.0404(13) 0.0446(13) -0.0008(10) 0.0058(10) 0.0066(10) C14 0.0443(14) 0.0451(13) 0.0614(16) -0.0077(12) 0.0140(12) 0.0107(11) C15 0.0506(15) 0.0632(17) 0.0638(17) -0.0064(14) 0.0251(13) 0.0152(13) C16 0.0402(13) 0.0654(17) 0.0657(17) 0.0057(14) 0.0219(12) 0.0065(13) C17 0.0365(12) 0.0489(14) 0.0536(15) -0.0001(12) 0.0077(11) -0.0008(11) C18 0.0320(11) 0.0416(12) 0.0422(13) -0.0024(10) 0.0071(10) 0.0029(10) O1 0.0490(10) 0.0460(10) 0.0673(12) -0.0101(8) 0.0285(9) -0.0016(8) O2 0.0397(9) 0.0416(9) 0.0469(9) 0.0013(7) 0.0157(7) 0.0064(7) O3 0.0592(12) 0.0753(13) 0.0617(13) -0.0019(11) 0.0089(10) -0.0100(10) O4 0.0666(13) 0.0813(15) 0.0836(15) -0.0095(12) 0.0166(11) -0.0242(12) O5 0.147(2) 0.0991(19) 0.0713(16) 0.0044(12) 0.0595(17) -0.0224(15) N1 0.0524(12) 0.0388(11) 0.0556(12) -0.0033(9) 0.0288(10) 0.0025(10) N2 0.0600(13) 0.0400(11) 0.0541(13) -0.0019(9) 0.0292(11) -0.0009(10) N3 0.0451(11) 0.0360(10) 0.0569(13) -0.0043(9) 0.0240(10) 0.0009(8) N4 0.0348(10) 0.0371(10) 0.0485(11) -0.0016(9) 0.0109(9) 0.0033(8) N5 0.0440(11) 0.0410(11) 0.0520(12) -0.0042(9) 0.0167(10) 0.0019(9) N6 0.0440(10) 0.0399(11) 0.0474(11) -0.0047(9) 0.0169(9) -0.0002(9) N7 0.0609(14) 0.0421(12) 0.0525(14) -0.0052(10) 0.0273(11) 0.0034(11) _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 Ag1 N1 2.1994(19) . ? Ag1 N6 2.217(2) 3_577 ? Ag1 O3 2.423(2) . ? Ag1 O3 2.590(2) 3_477 ? C1 N1 1.375(3) . ? C1 C6 1.387(3) . ? C1 C2 1.400(3) . ? C2 C3 1.356(4) . ? C2 H2 0.9300 . ? C3 C4 1.400(4) . ? C3 H3 0.9300 . ? C4 C5 1.367(4) . ? C4 H4 0.9300 . ? C5 C6 1.398(3) . ? C5 H5 0.9300 . ? C6 N3 1.362(3) . ? C7 N3 1.460(3) . ? C7 C8 1.506(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.410(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O1 1.431(3) . ? C9 C10 1.501(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O2 1.421(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O2 1.416(3) . ? C11 C12 1.511(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.461(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.360(3) . ? C13 C18 1.395(3) . ? C13 C14 1.403(3) . ? C14 C15 1.367(4) . ? C14 H14 0.9300 . ? C15 C16 1.411(4) . ? C15 H15 0.9300 . ? C16 C17 1.361(3) . ? C16 H16 0.9300 . ? C17 C18 1.405(3) . ? C17 H17 0.9300 . ? C18 N6 1.371(3) . ? O3 N7 1.256(3) . ? O3 Ag1 2.590(2) 3_477 ? O4 N7 1.227(3) . ? O5 N7 1.222(3) . ? N1 N2 1.318(3) . ? N2 N3 1.339(3) . ? N4 N5 1.345(2) . ? N5 N6 1.314(3) . ? N6 Ag1 2.2167(19) 3_577 ? 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 N1 Ag1 N6 134.41(7) . 3_577 ? N1 Ag1 O3 112.18(7) . . ? N6 Ag1 O3 109.14(7) 3_577 . ? N1 Ag1 O3 105.78(7) . 3_477 ? N6 Ag1 O3 102.06(7) 3_577 3_477 ? O3 Ag1 O3 75.98(7) . 3_477 ? N1 C1 C6 108.0(2) . . ? N1 C1 C2 130.4(2) . . ? C6 C1 C2 121.5(2) . . ? C3 C2 C1 116.7(2) . . ? C3 C2 H2 121.7 . . ? C1 C2 H2 121.7 . . ? C2 C3 C4 121.4(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 123.3(2) . . ? C5 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? C4 C5 C6 115.3(2) . . ? C4 C5 H5 122.4 . . ? C6 C5 H5 122.4 . . ? N3 C6 C1 104.24(19) . . ? N3 C6 C5 133.9(2) . . ? C1 C6 C5 121.8(2) . . ? N3 C7 C8 112.4(2) . . ? N3 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? O1 C8 C7 108.0(2) . . ? O1 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? O1 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? O1 C9 C10 113.65(19) . . ? O1 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? O1 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? O2 C10 C9 110.45(19) . . ? O2 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O2 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O2 C11 C12 113.75(18) . . ? O2 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? O2 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N4 C12 C11 112.38(19) . . ? N4 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? N4 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N4 C13 C18 104.55(19) . . ? N4 C13 C14 133.4(2) . . ? C18 C13 C14 122.0(2) . . ? C15 C14 C13 115.6(2) . . ? C15 C14 H14 122.2 . . ? C13 C14 H14 122.2 . . ? C14 C15 C16 122.7(2) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C17 C16 C15 121.9(2) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 116.5(2) . . ? C16 C17 H17 121.7 . . ? C18 C17 H17 121.7 . . ? N6 C18 C13 107.67(19) . . ? N6 C18 C17 131.1(2) . . ? C13 C18 C17 121.3(2) . . ? C8 O1 C9 113.76(18) . . ? C11 O2 C10 113.29(17) . . ? N7 O3 Ag1 108.76(15) . . ? N7 O3 Ag1 140.89(17) . 3_477 ? Ag1 O3 Ag1 104.02(7) . 3_477 ? N2 N1 C1 108.70(19) . . ? N2 N1 Ag1 126.55(15) . . ? C1 N1 Ag1 121.91(15) . . ? N1 N2 N3 107.90(19) . . ? N2 N3 C6 111.14(18) . . ? N2 N3 C7 120.7(2) . . ? C6 N3 C7 128.2(2) . . ? N5 N4 C13 110.66(18) . . ? N5 N4 C12 120.18(19) . . ? C13 N4 C12 129.16(19) . . ? N6 N5 N4 108.07(18) . . ? N5 N6 C18 109.04(18) . . ? N5 N6 Ag1 123.85(15) . 3_577 ? C18 N6 Ag1 126.63(15) . 3_577 ? O5 N7 O4 121.2(3) . . ? O5 N7 O3 120.1(2) . . ? O4 N7 O3 118.6(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.85 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.292 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.051 # Attachment 'complex-4.cif' data_p-1 _database_code_depnum_ccdc_archive 'CCDC 676487' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Cl2 Cu N6' _chemical_formula_weight 398.74 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' 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 7.7004(14) _cell_length_b 9.5195(18) _cell_length_c 11.112(2) _cell_angle_alpha 79.404(3) _cell_angle_beta 86.652(3) _cell_angle_gamma 80.058(3) _cell_volume 788.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1514 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 26.22 _exptl_crystal_description block _exptl_crystal_colour 'Navy blue' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 402 _exptl_absorpt_coefficient_mu 1.731 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 3987 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2765 _reflns_number_gt 2178 _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^)+(0.0651P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2765 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _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 0.19701(7) 1.25800(5) 0.22442(4) 0.03412(19) Uani 1 1 d . . . C1 C 0.0392(5) 0.9918(4) 0.1984(3) 0.0313(9) Uani 1 1 d . . . C2 C -0.0938(6) 0.9933(5) 0.2884(4) 0.0441(11) Uani 1 1 d . . . H2 H -0.1225 1.0696 0.3314 0.053 Uiso 1 1 calc R . . C3 C -0.1802(6) 0.8766(5) 0.3104(4) 0.0482(11) Uani 1 1 d . . . H3 H -0.2682 0.8722 0.3713 0.058 Uiso 1 1 calc R . . C4 C -0.1387(6) 0.7627(5) 0.2427(4) 0.0438(11) Uani 1 1 d . . . H4 H -0.2015 0.6859 0.2605 0.053 Uiso 1 1 calc R . . C5 C -0.0117(5) 0.7602(4) 0.1532(4) 0.0369(10) Uani 1 1 d . . . H5 H 0.0127 0.6854 0.1083 0.044 Uiso 1 1 calc R . . C6 C 0.0807(5) 0.8779(4) 0.1324(3) 0.0307(9) Uani 1 1 d . . . C7 C 0.3374(6) 0.8192(4) -0.0150(3) 0.0383(10) Uani 1 1 d . . . H7A H 0.3886 0.8800 -0.0827 0.046 Uiso 1 1 calc R . . H7B H 0.2694 0.7595 -0.0486 0.046 Uiso 1 1 calc R . . C8 C 0.4829(6) 0.7232(4) 0.0613(4) 0.0379(10) Uani 1 1 d . . . H8A H 0.5635 0.6695 0.0091 0.045 Uiso 1 1 calc R . . H8B H 0.5486 0.7830 0.0967 0.045 Uiso 1 1 calc R . . C9 C 0.3732(5) 0.6330(4) 0.2789(3) 0.0295(9) Uani 1 1 d . . . C10 C 0.3892(5) 0.7387(4) 0.3480(4) 0.0383(10) Uani 1 1 d . . . H10 H 0.4379 0.8209 0.3154 0.046 Uiso 1 1 calc R . . C11 C 0.3282(6) 0.7128(5) 0.4665(4) 0.0502(12) Uani 1 1 d . . . H11 H 0.3356 0.7799 0.5164 0.060 Uiso 1 1 calc R . . C12 C 0.2546(6) 0.5886(5) 0.5160(4) 0.0515(12) Uani 1 1 d . . . H12 H 0.2183 0.5747 0.5980 0.062 Uiso 1 1 calc R . . C13 C 0.2349(6) 0.4869(5) 0.4465(4) 0.0412(10) Uani 1 1 d . . . H13 H 0.1829 0.4062 0.4785 0.049 Uiso 1 1 calc R . . C14 C 0.2970(5) 0.5116(4) 0.3262(3) 0.0302(9) Uani 1 1 d . . . Cl1 Cl -0.06787(15) 1.38102(11) 0.16815(11) 0.0488(3) Uani 1 1 d . . . Cl2 Cl 0.3950(2) 1.12340(13) 0.35137(14) 0.0746(5) Uani 1 1 d . . . N1 N 0.1583(4) 1.0847(3) 0.1601(3) 0.0337(8) Uani 1 1 d . . . N2 N 0.2679(4) 1.0345(3) 0.0769(3) 0.0334(8) Uani 1 1 d . . . N3 N 0.2214(4) 0.9102(3) 0.0585(3) 0.0297(7) Uani 1 1 d . . . N4 N 0.2938(4) 0.4363(3) 0.2319(3) 0.0338(8) Uani 1 1 d . . . N5 N 0.3625(4) 0.5032(3) 0.1321(3) 0.0362(8) Uani 1 1 d . . . N6 N 0.4132(4) 0.6220(3) 0.1589(3) 0.0309(7) 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 Cu1 0.0455(3) 0.0205(3) 0.0408(3) -0.0132(2) 0.0015(2) -0.0105(2) C1 0.035(2) 0.0196(19) 0.039(2) -0.0048(16) -0.0038(18) -0.0041(16) C2 0.043(3) 0.036(2) 0.055(3) -0.017(2) 0.008(2) -0.006(2) C3 0.041(3) 0.045(3) 0.057(3) -0.008(2) 0.006(2) -0.009(2) C4 0.036(2) 0.032(2) 0.063(3) -0.001(2) -0.002(2) -0.0145(19) C5 0.038(2) 0.026(2) 0.050(3) -0.0073(18) -0.008(2) -0.0092(18) C6 0.038(2) 0.023(2) 0.033(2) -0.0062(16) -0.0044(18) -0.0062(17) C7 0.057(3) 0.032(2) 0.032(2) -0.0141(17) 0.0072(19) -0.015(2) C8 0.046(3) 0.028(2) 0.044(2) -0.0158(18) 0.015(2) -0.0104(19) C9 0.030(2) 0.024(2) 0.038(2) -0.0146(16) 0.0004(17) -0.0042(16) C10 0.041(2) 0.029(2) 0.050(3) -0.0197(19) -0.006(2) -0.0065(19) C11 0.059(3) 0.046(3) 0.053(3) -0.031(2) -0.008(2) -0.003(2) C12 0.068(3) 0.053(3) 0.033(2) -0.015(2) 0.001(2) -0.005(3) C13 0.052(3) 0.033(2) 0.041(2) -0.0065(19) 0.003(2) -0.012(2) C14 0.035(2) 0.0197(19) 0.037(2) -0.0057(16) -0.0009(17) -0.0052(16) Cl1 0.0547(7) 0.0333(6) 0.0630(7) -0.0203(5) -0.0119(6) -0.0039(5) Cl2 0.0938(11) 0.0321(6) 0.1029(11) -0.0199(7) -0.0529(9) 0.0012(7) N1 0.0385(19) 0.0248(17) 0.0409(19) -0.0121(15) -0.0009(16) -0.0076(15) N2 0.045(2) 0.0226(17) 0.0367(18) -0.0110(14) 0.0043(16) -0.0126(15) N3 0.041(2) 0.0183(16) 0.0331(17) -0.0093(13) -0.0007(15) -0.0091(14) N4 0.050(2) 0.0206(17) 0.0351(18) -0.0126(14) 0.0035(16) -0.0104(15) N5 0.050(2) 0.0236(17) 0.0399(19) -0.0147(15) 0.0058(16) -0.0115(16) N6 0.0367(19) 0.0222(17) 0.0380(18) -0.0142(14) 0.0082(15) -0.0097(14) _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 1.985(3) 1_565 ? Cu1 N1 1.987(3) . ? Cu1 Cl2 2.2062(13) . ? Cu1 Cl1 2.2311(13) . ? C1 N1 1.379(5) . ? C1 C2 1.389(6) . ? C1 C6 1.400(5) . ? C2 C3 1.369(6) . ? C2 H2 0.9300 . ? C3 C4 1.413(6) . ? C3 H3 0.9300 . ? C4 C5 1.354(6) . ? C4 H4 0.9300 . ? C5 C6 1.406(5) . ? C5 H5 0.9300 . ? C6 N3 1.364(5) . ? C7 N3 1.457(5) . ? C7 C8 1.510(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N6 1.456(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N6 1.370(5) . ? C9 C14 1.390(5) . ? C9 C10 1.398(5) . ? C10 C11 1.366(6) . ? C10 H10 0.9300 . ? C11 C12 1.406(6) . ? C11 H11 0.9300 . ? C12 C13 1.377(6) . ? C12 H12 0.9300 . ? C13 C14 1.386(5) . ? C13 H13 0.9300 . ? C14 N4 1.378(5) . ? N1 N2 1.315(4) . ? N2 N3 1.346(4) . ? N4 N5 1.305(4) . ? N4 Cu1 1.985(3) 1_545 ? N5 N6 1.344(4) . ? 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 N1 158.18(13) 1_565 . ? N4 Cu1 Cl2 91.97(10) 1_565 . ? N1 Cu1 Cl2 90.86(10) . . ? N4 Cu1 Cl1 93.18(10) 1_565 . ? N1 Cu1 Cl1 92.89(10) . . ? Cl2 Cu1 Cl1 156.24(6) . . ? N1 C1 C2 131.3(4) . . ? N1 C1 C6 106.8(3) . . ? C2 C1 C6 121.7(4) . . ? C3 C2 C1 116.5(4) . . ? C3 C2 H2 121.8 . . ? C1 C2 H2 121.8 . . ? C2 C3 C4 121.5(4) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 123.0(4) . . ? C5 C4 H4 118.5 . . ? C3 C4 H4 118.5 . . ? C4 C5 C6 115.7(4) . . ? C4 C5 H5 122.1 . . ? C6 C5 H5 122.1 . . ? N3 C6 C1 104.9(3) . . ? N3 C6 C5 133.6(4) . . ? C1 C6 C5 121.5(4) . . ? N3 C7 C8 110.9(3) . . ? N3 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? N6 C8 C7 111.6(3) . . ? N6 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N6 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N6 C9 C14 104.7(3) . . ? N6 C9 C10 132.7(4) . . ? C14 C9 C10 122.6(4) . . ? C11 C10 C9 115.3(4) . . ? C11 C10 H10 122.3 . . ? C9 C10 H10 122.3 . . ? C10 C11 C12 122.5(4) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 121.9(4) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 116.1(4) . . ? C12 C13 H13 121.9 . . ? C14 C13 H13 121.9 . . ? N4 C14 C13 131.5(3) . . ? N4 C14 C9 106.9(3) . . ? C13 C14 C9 121.6(4) . . ? N2 N1 C1 109.8(3) . . ? N2 N1 Cu1 120.0(2) . . ? C1 N1 Cu1 129.8(3) . . ? N1 N2 N3 107.7(3) . . ? N2 N3 C6 110.8(3) . . ? N2 N3 C7 119.3(3) . . ? C6 N3 C7 128.9(3) . . ? N5 N4 C14 110.1(3) . . ? N5 N4 Cu1 118.6(2) . 1_545 ? C14 N4 Cu1 131.3(3) . 1_545 ? N4 N5 N6 107.6(3) . . ? N5 N6 C9 110.7(3) . . ? N5 N6 C8 119.3(3) . . ? C9 N6 C8 129.7(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.748 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.087 # Attachment 'complex-5.cif' data_t _database_code_depnum_ccdc_archive 'CCDC 676488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Cl4 Cu2 N12 O2' _chemical_formula_weight 885.58 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' 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 8.7198(7) _cell_length_b 10.1265(9) _cell_length_c 10.9772(9) _cell_angle_alpha 88.4220(10) _cell_angle_beta 73.7320(10) _cell_angle_gamma 72.3070(10) _cell_volume 884.72(13) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2188 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.25 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 1.555 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 4525 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.15 _reflns_number_total 3149 _reflns_number_gt 2646 _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^)+(0.0324P)^2^+0.6000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3149 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _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 0.99768(4) -0.10849(3) 0.12511(3) 0.02894(11) Uani 1 1 d . . . C1 C 0.6334(3) 0.0382(3) 0.2816(2) 0.0307(6) Uani 1 1 d . . . C2 C 0.5435(4) -0.0341(3) 0.2392(3) 0.0406(7) Uani 1 1 d . . . H2 H 0.5953 -0.1015 0.1722 0.049 Uiso 1 1 calc R . . C3 C 0.3748(4) -0.0015(4) 0.3006(3) 0.0499(8) Uani 1 1 d . . . H3 H 0.3111 -0.0475 0.2742 0.060 Uiso 1 1 calc R . . C4 C 0.2964(4) 0.0997(4) 0.4025(3) 0.0571(10) Uani 1 1 d . . . H4 H 0.1823 0.1178 0.4425 0.069 Uiso 1 1 calc R . . C5 C 0.3819(4) 0.1717(4) 0.4444(3) 0.0504(9) Uani 1 1 d . . . H5 H 0.3292 0.2390 0.5114 0.060 Uiso 1 1 calc R . . C6 C 0.5535(4) 0.1397(3) 0.3815(3) 0.0355(7) Uani 1 1 d . . . C7 C 0.6687(4) 0.2874(3) 0.4948(3) 0.0484(8) Uani 1 1 d . . . H7A H 0.7001 0.2370 0.5650 0.058 Uiso 1 1 calc R . . H7B H 0.5540 0.3477 0.5270 0.058 Uiso 1 1 calc R . . C8 C 0.7812(4) 0.3742(3) 0.4463(3) 0.0500(9) Uani 1 1 d . . . H8A H 0.7842 0.4290 0.5162 0.060 Uiso 1 1 calc R . . H8B H 0.8945 0.3150 0.4059 0.060 Uiso 1 1 calc R . . C9 C 0.8406(4) 0.5119(3) 0.2708(3) 0.0469(8) Uani 1 1 d . . . H9A H 0.9445 0.4365 0.2396 0.056 Uiso 1 1 calc R . . H9B H 0.8634 0.5840 0.3126 0.056 Uiso 1 1 calc R . . C10 C 0.7719(4) 0.5687(3) 0.1626(3) 0.0382(7) Uani 1 1 d . . . H10A H 0.6668 0.6427 0.1947 0.046 Uiso 1 1 calc R . . H10B H 0.8505 0.6070 0.1034 0.046 Uiso 1 1 calc R . . C11 C 0.6015(3) 0.4222(3) 0.1154(2) 0.0273(6) Uani 1 1 d . . . C12 C 0.4352(3) 0.4869(3) 0.1857(3) 0.0361(7) Uani 1 1 d . . . H12 H 0.4029 0.5702 0.2336 0.043 Uiso 1 1 calc R . . C13 C 0.3240(4) 0.4201(3) 0.1794(3) 0.0416(7) Uani 1 1 d . . . H13 H 0.2118 0.4588 0.2250 0.050 Uiso 1 1 calc R . . C14 C 0.3721(4) 0.2949(3) 0.1066(3) 0.0408(7) Uani 1 1 d . . . H14 H 0.2911 0.2533 0.1053 0.049 Uiso 1 1 calc R . . C15 C 0.5364(4) 0.2318(3) 0.0370(3) 0.0350(7) Uani 1 1 d . . . H15 H 0.5678 0.1491 -0.0117 0.042 Uiso 1 1 calc R . . C16 C 0.6527(3) 0.2977(3) 0.0430(2) 0.0279(6) Uani 1 1 d . . . Cl1 Cl 1.14082(8) 0.07133(7) 0.03696(6) 0.03181(17) Uani 1 1 d . . . Cl2 Cl 1.06052(10) -0.21763(8) 0.29693(7) 0.0495(2) Uani 1 1 d . . . N1 N 0.7999(3) 0.0307(2) 0.2440(2) 0.0315(5) Uani 1 1 d . . . N2 N 0.8247(3) 0.1207(2) 0.3140(2) 0.0378(6) Uani 1 1 d . . . N3 N 0.6768(3) 0.1877(2) 0.3962(2) 0.0393(6) Uani 1 1 d . . . N4 N 0.8229(3) 0.2653(2) -0.0119(2) 0.0299(5) Uani 1 1 d . . . N5 N 0.8756(3) 0.3637(2) 0.0213(2) 0.0329(5) Uani 1 1 d . . . N6 N 0.7441(3) 0.4584(2) 0.0974(2) 0.0305(5) Uani 1 1 d . . . O1 O 0.7192(2) 0.4632(2) 0.35699(19) 0.0417(5) 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 Cu1 0.02405(18) 0.02575(19) 0.02888(19) -0.00537(13) -0.00155(13) -0.00093(13) C1 0.0281(14) 0.0320(15) 0.0249(14) 0.0038(11) -0.0039(11) -0.0027(12) C2 0.0415(18) 0.0409(17) 0.0360(17) 0.0074(13) -0.0070(14) -0.0121(14) C3 0.0402(18) 0.062(2) 0.051(2) 0.0191(17) -0.0111(16) -0.0235(17) C4 0.0308(18) 0.078(3) 0.047(2) 0.0156(19) 0.0015(15) -0.0078(18) C5 0.0343(18) 0.059(2) 0.0359(18) 0.0015(15) 0.0032(14) 0.0044(16) C6 0.0326(16) 0.0368(16) 0.0283(15) 0.0049(12) -0.0049(12) -0.0016(13) C7 0.067(2) 0.0362(17) 0.0318(17) -0.0089(13) -0.0124(16) -0.0013(16) C8 0.059(2) 0.0432(18) 0.047(2) -0.0130(15) -0.0274(17) -0.0024(16) C9 0.0374(17) 0.0489(19) 0.054(2) -0.0159(16) -0.0048(15) -0.0190(15) C10 0.0353(16) 0.0301(15) 0.0444(18) -0.0089(13) 0.0063(13) -0.0180(13) C11 0.0249(14) 0.0261(14) 0.0277(14) 0.0015(11) -0.0050(11) -0.0055(11) C12 0.0273(15) 0.0326(15) 0.0386(16) -0.0073(13) -0.0012(12) -0.0021(12) C13 0.0216(15) 0.0460(18) 0.0490(19) -0.0007(15) -0.0024(13) -0.0054(13) C14 0.0305(16) 0.0423(18) 0.0545(19) 0.0033(15) -0.0157(14) -0.0151(14) C15 0.0372(16) 0.0282(15) 0.0415(17) 0.0023(12) -0.0166(13) -0.0080(13) C16 0.0232(13) 0.0280(14) 0.0277(14) -0.0010(11) -0.0050(11) -0.0028(11) Cl1 0.0282(4) 0.0311(4) 0.0365(4) -0.0038(3) -0.0093(3) -0.0091(3) Cl2 0.0513(5) 0.0457(5) 0.0351(4) 0.0009(3) -0.0093(3) 0.0057(4) N1 0.0275(12) 0.0286(12) 0.0311(12) -0.0067(10) -0.0041(10) -0.0013(10) N2 0.0331(13) 0.0362(14) 0.0348(14) -0.0097(11) -0.0039(11) -0.0015(11) N3 0.0413(15) 0.0327(13) 0.0294(13) -0.0081(10) -0.0022(11) 0.0027(11) N4 0.0244(12) 0.0272(12) 0.0301(12) -0.0033(10) -0.0001(10) -0.0032(10) N5 0.0259(12) 0.0281(12) 0.0373(13) -0.0036(10) 0.0021(10) -0.0074(10) N6 0.0268(12) 0.0249(12) 0.0324(13) -0.0050(9) 0.0021(10) -0.0065(10) O1 0.0326(11) 0.0469(12) 0.0392(12) -0.0001(10) -0.0069(9) -0.0062(10) _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 2.006(2) 2_755 ? Cu1 N1 2.007(2) . ? Cu1 Cl2 2.2749(8) . ? Cu1 Cl1 2.3783(7) 2_755 ? Cu1 Cl1 2.5333(8) . ? C1 N1 1.372(3) . ? C1 C2 1.393(4) . ? C1 C6 1.393(4) . ? C2 C3 1.374(4) . ? C2 H2 0.9300 . ? C3 C4 1.406(5) . ? C3 H3 0.9300 . ? C4 C5 1.357(5) . ? C4 H4 0.9300 . ? C5 C6 1.400(4) . ? C5 H5 0.9300 . ? C6 N3 1.356(4) . ? C7 N3 1.473(4) . ? C7 C8 1.491(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.421(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O1 1.410(4) . ? C9 C10 1.502(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N6 1.457(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.362(3) . ? C11 C16 1.391(4) . ? C11 C12 1.397(4) . ? C12 C13 1.357(4) . ? C12 H12 0.9300 . ? C13 C14 1.402(4) . ? C13 H13 0.9300 . ? C14 C15 1.379(4) . ? C14 H14 0.9300 . ? C15 C16 1.389(4) . ? C15 H15 0.9300 . ? C16 N4 1.374(3) . ? Cl1 Cu1 2.3783(7) 2_755 ? N1 N2 1.311(3) . ? N2 N3 1.337(3) . ? N4 N5 1.315(3) . ? N4 Cu1 2.006(2) 2_755 ? N5 N6 1.331(3) . ? 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 N1 172.28(9) 2_755 . ? N4 Cu1 Cl2 89.12(7) 2_755 . ? N1 Cu1 Cl2 88.80(7) . . ? N4 Cu1 Cl1 87.70(7) 2_755 2_755 ? N1 Cu1 Cl1 90.73(7) . 2_755 ? Cl2 Cu1 Cl1 152.58(3) . 2_755 ? N4 Cu1 Cl1 93.98(7) 2_755 . ? N1 Cu1 Cl1 93.58(7) . . ? Cl2 Cu1 Cl1 117.21(3) . . ? Cl1 Cu1 Cl1 90.19(2) 2_755 . ? N1 C1 C2 132.2(3) . . ? N1 C1 C6 107.0(2) . . ? C2 C1 C6 120.7(3) . . ? C3 C2 C1 117.1(3) . . ? C3 C2 H2 121.4 . . ? C1 C2 H2 121.4 . . ? C2 C3 C4 121.6(3) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 122.1(3) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 116.6(3) . . ? C4 C5 H5 121.7 . . ? C6 C5 H5 121.7 . . ? N3 C6 C1 104.7(2) . . ? N3 C6 C5 133.4(3) . . ? C1 C6 C5 121.9(3) . . ? N3 C7 C8 112.5(3) . . ? N3 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? O1 C8 C7 108.8(3) . . ? O1 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? O1 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? O1 C9 C10 107.7(2) . . ? O1 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O1 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? N6 C10 C9 109.7(2) . . ? N6 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? N6 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N6 C11 C16 104.7(2) . . ? N6 C11 C12 132.1(2) . . ? C16 C11 C12 123.2(3) . . ? C13 C12 C11 115.6(3) . . ? C13 C12 H12 122.2 . . ? C11 C12 H12 122.2 . . ? C12 C13 C14 122.4(3) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 121.8(3) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 116.8(3) . . ? C14 C15 H15 121.6 . . ? C16 C15 H15 121.6 . . ? N4 C16 C15 132.6(2) . . ? N4 C16 C11 107.1(2) . . ? C15 C16 C11 120.3(2) . . ? Cu1 Cl1 Cu1 89.81(2) 2_755 . ? N2 N1 C1 109.5(2) . . ? N2 N1 Cu1 119.59(17) . . ? C1 N1 Cu1 130.18(18) . . ? N1 N2 N3 107.8(2) . . ? N2 N3 C6 111.0(2) . . ? N2 N3 C7 119.8(3) . . ? C6 N3 C7 128.8(2) . . ? N5 N4 C16 109.2(2) . . ? N5 N4 Cu1 115.03(16) . 2_755 ? C16 N4 Cu1 135.80(19) . 2_755 ? N4 N5 N6 108.1(2) . . ? N5 N6 C11 110.9(2) . . ? N5 N6 C10 119.1(2) . . ? C11 N6 C10 129.3(2) . . ? C9 O1 C8 114.3(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.419 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.058 ################################## data_Complex-6 _database_code_depnum_ccdc_archive 'CCDC 676489' #TrackingRef '- complexes.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 Cl4 Cu2 N14 O6' _chemical_formula_weight 1119.87 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 35.704(6) _cell_length_b 33.360(5) _cell_length_c 8.2196(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9790(3) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2349 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 20.40 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4624 _exptl_absorpt_coefficient_mu 1.149 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 55832 _diffrn_reflns_av_R_equivalents 0.1315 _diffrn_reflns_av_sigmaI/netI 0.1068 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.45 _reflns_number_total 11128 _reflns_number_gt 4991 _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^)+(0.0120P)^2^+67.8778P] 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 11128 _refine_ls_number_parameters 667 _refine_ls_number_restraints 137 _refine_ls_R_factor_all 0.1938 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.1900 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.009 _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 0.38189(3) 0.12797(3) 0.14067(11) 0.0378(2) Uani 1 1 d . . . Cu2 Cu 0.13066(3) 0.12143(3) 0.15489(10) 0.0373(2) Uani 1 1 d . . . Cl1 Cl 0.43432(7) 0.12533(7) -0.0186(3) 0.0744(8) Uani 1 1 d . B . Cl2 Cl 0.38760(7) 0.12732(6) 0.4361(2) 0.0575(6) Uani 1 1 d . B . Cl3 Cl 0.16461(8) 0.12099(7) -0.0750(3) 0.0728(8) Uani 1 1 d . . . Cl4 Cl 0.12957(7) 0.12186(6) 0.4339(2) 0.0525(5) Uani 1 1 d . . . C1 C 0.4101(2) 0.2123(2) 0.1978(9) 0.0349(19) Uani 1 1 d . . . C2 C 0.4424(2) 0.2041(2) 0.2873(10) 0.041(2) Uani 1 1 d . B . H2 H 0.4501 0.1780 0.3083 0.050 Uiso 1 1 calc R . . C3 C 0.4622(2) 0.2364(2) 0.3427(11) 0.045(2) Uani 1 1 d . . . H3 H 0.4839 0.2322 0.4029 0.054 Uiso 1 1 calc R B . C4 C 0.4503(3) 0.2760(2) 0.3105(11) 0.048(2) Uani 1 1 d . B . H4 H 0.4645 0.2970 0.3512 0.058 Uiso 1 1 calc R . . C5 C 0.4193(3) 0.2849(2) 0.2236(11) 0.046(2) Uani 1 1 d . . . H5 H 0.4119 0.3111 0.2025 0.055 Uiso 1 1 calc R B . C6 C 0.3990(2) 0.2517(2) 0.1676(9) 0.0333(18) Uani 1 1 d . B . C7 C 0.3439(3) 0.2796(2) 0.0062(10) 0.046(2) Uani 1 1 d . . . H7A H 0.3261 0.2675 -0.0682 0.056 Uiso 1 1 calc R . . H7B H 0.3599 0.2974 -0.0560 0.056 Uiso 1 1 calc R . . C8 C 0.3230(3) 0.3036(3) 0.1321(12) 0.059(3) Uani 1 1 d . A . H8A H 0.3400 0.3121 0.2175 0.071 Uiso 1 1 calc R . . H8B H 0.3122 0.3273 0.0825 0.071 Uiso 1 1 calc R . . C9' C 0.2752(7) 0.2795(10) 0.352(3) 0.055(6) Uani 0.284(13) 1 d PDU A 2 H9C H 0.2893 0.2936 0.4345 0.066 Uiso 0.284(13) 1 calc PR A 2 H9D H 0.2702 0.2524 0.3885 0.066 Uiso 0.284(13) 1 calc PR A 2 C10' C 0.2397(6) 0.3012(7) 0.310(4) 0.048(6) Uani 0.284(13) 1 d PDU A 2 H10C H 0.2443 0.3229 0.2338 0.058 Uiso 0.284(13) 1 calc PR A 2 H10D H 0.2276 0.3118 0.4060 0.058 Uiso 0.284(13) 1 calc PR A 2 C9 C 0.2721(3) 0.3059(3) 0.2982(15) 0.049(3) Uani 0.716(13) 1 d PDU A 1 H9A H 0.2619 0.3277 0.2342 0.058 Uiso 0.716(13) 1 calc PR A 1 H9B H 0.2869 0.3170 0.3864 0.058 Uiso 0.716(13) 1 calc PR A 1 C10 C 0.2409(4) 0.2792(4) 0.3641(15) 0.058(4) Uani 0.716(13) 1 d PDU A 1 H10A H 0.2515 0.2553 0.4127 0.070 Uiso 0.716(13) 1 calc PR A 1 H10B H 0.2269 0.2934 0.4471 0.070 Uiso 0.716(13) 1 calc PR A 1 C11 C 0.1891(3) 0.2968(3) 0.1747(11) 0.062(3) Uani 1 1 d D A . H11A H 0.2016 0.3200 0.1289 0.075 Uiso 1 1 calc R . . H11B H 0.1735 0.3056 0.2643 0.075 Uiso 1 1 calc R . . C12 C 0.1654(3) 0.2766(2) 0.0466(10) 0.047(2) Uani 1 1 d . . . H12A H 0.1488 0.2963 -0.0019 0.056 Uiso 1 1 calc R . . H12B H 0.1816 0.2663 -0.0385 0.056 Uiso 1 1 calc R . . C13 C 0.1103(2) 0.2457(2) 0.1985(9) 0.0352(18) Uani 1 1 d . . . C14 C 0.0893(3) 0.2780(2) 0.2572(11) 0.046(2) Uani 1 1 d . . . H14 H 0.0967 0.3045 0.2421 0.055 Uiso 1 1 calc R . . C15 C 0.0575(3) 0.2680(2) 0.3377(11) 0.053(2) Uani 1 1 d . . . H15 H 0.0424 0.2885 0.3766 0.063 Uiso 1 1 calc R . . C16 C 0.0463(2) 0.2282(2) 0.3652(10) 0.046(2) Uani 1 1 d . . . H16 H 0.0243 0.2231 0.4218 0.055 Uiso 1 1 calc R . . C17 C 0.0675(2) 0.1968(2) 0.3096(10) 0.039(2) Uani 1 1 d . . . H17 H 0.0602 0.1704 0.3267 0.046 Uiso 1 1 calc R . . C18 C 0.1006(2) 0.2060(2) 0.2261(9) 0.0313(18) Uani 1 1 d . . . C19 C 0.0959(2) 0.0386(2) 0.2230(9) 0.0330(18) Uani 1 1 d . . . C20 C 0.0635(2) 0.0496(2) 0.3065(10) 0.043(2) Uani 1 1 d . . . H20 H 0.0573 0.0763 0.3235 0.052 Uiso 1 1 calc R . . C21 C 0.0414(3) 0.0192(3) 0.3621(11) 0.054(2) Uani 1 1 d . . . H21 H 0.0200 0.0256 0.4213 0.065 Uiso 1 1 calc R . . C22 C 0.0499(3) -0.0215(3) 0.3328(11) 0.052(2) Uani 1 1 d . . . H22 H 0.0337 -0.0411 0.3717 0.062 Uiso 1 1 calc R . . C23 C 0.0812(2) -0.0328(2) 0.2490(10) 0.041(2) Uani 1 1 d . . . H23 H 0.0869 -0.0595 0.2297 0.049 Uiso 1 1 calc R . . C24 C 0.1042(2) -0.0017(2) 0.1939(10) 0.0351(18) Uani 1 1 d . . . C25 C 0.1568(2) -0.0348(2) 0.0343(9) 0.038(2) Uani 1 1 d . . . H25A H 0.1732 -0.0246 -0.0501 0.046 Uiso 1 1 calc R . . H25B H 0.1389 -0.0527 -0.0166 0.046 Uiso 1 1 calc R . . C26 C 0.1797(2) -0.0581(2) 0.1551(11) 0.042(2) Uani 1 1 d . . . H26A H 0.1643 -0.0658 0.2472 0.051 Uiso 1 1 calc R . . H26B H 0.1893 -0.0824 0.1048 0.051 Uiso 1 1 calc R . . C27 C 0.2349(2) -0.0544(3) 0.3131(11) 0.052(2) Uani 1 1 d . . . H27A H 0.2455 -0.0775 0.2577 0.062 Uiso 1 1 calc R . . H27B H 0.2217 -0.0638 0.4089 0.062 Uiso 1 1 calc R . . C28 C 0.2651(2) -0.0265(3) 0.3612(11) 0.053(2) Uani 1 1 d . . . H28A H 0.2540 -0.0042 0.4192 0.064 Uiso 1 1 calc R . . H28B H 0.2818 -0.0403 0.4359 0.064 Uiso 1 1 calc R . . C29 C 0.3108(2) -0.0405(2) 0.1615(10) 0.041(2) Uani 1 1 d . . . H29A H 0.2962 -0.0624 0.1171 0.050 Uiso 1 1 calc R . . H29B H 0.3270 -0.0512 0.2457 0.050 Uiso 1 1 calc R . . C30 C 0.3342(2) -0.0217(2) 0.0287(9) 0.038(2) Uani 1 1 d . B . H30A H 0.3485 -0.0424 -0.0260 0.046 Uiso 1 1 calc R . . H30B H 0.3178 -0.0094 -0.0509 0.046 Uiso 1 1 calc R . . C31 C 0.3918(2) 0.0035(2) 0.1785(10) 0.0322(17) Uani 1 1 d . B . C32 C 0.4108(3) -0.0305(2) 0.2382(11) 0.048(2) Uani 1 1 d . . . H32 H 0.4020 -0.0564 0.2208 0.058 Uiso 1 1 calc R . . C33 C 0.4428(3) -0.0230(2) 0.3232(11) 0.053(2) Uani 1 1 d . . . H33 H 0.4563 -0.0445 0.3648 0.063 Uiso 1 1 calc R . . C34 C 0.4564(3) 0.0159(2) 0.3507(11) 0.052(2) Uani 1 1 d . . . H34 H 0.4782 0.0192 0.4111 0.062 Uiso 1 1 calc R . . C35 C 0.4387(2) 0.0489(2) 0.2915(10) 0.043(2) Uani 1 1 d . B . H35 H 0.4482 0.0746 0.3065 0.051 Uiso 1 1 calc R . . C36 C 0.4052(2) 0.0423(2) 0.2068(10) 0.0318(17) Uani 1 1 d . . . C37 C 0.2992(3) 0.1121(4) 0.2052(17) 0.062(5) Uani 0.640(19) 1 d PDU B 1 H37 H 0.3041 0.0853 0.2289 0.075 Uiso 0.640(19) 1 calc PR B 1 C38 C 0.2387(7) 0.0959(7) 0.314(3) 0.109(7) Uani 0.640(19) 1 d PU B 1 H38A H 0.2196 0.0907 0.2348 0.163 Uiso 0.640(19) 1 calc PR B 1 H38B H 0.2273 0.1057 0.4125 0.163 Uiso 0.640(19) 1 calc PR B 1 H38C H 0.2521 0.0716 0.3372 0.163 Uiso 0.640(19) 1 calc PR B 1 C39 C 0.2538(6) 0.1665(6) 0.249(3) 0.089(6) Uani 0.640(19) 1 d PU B 1 H39A H 0.2742 0.1836 0.2187 0.134 Uiso 0.640(19) 1 calc PR B 1 H39B H 0.2453 0.1736 0.3561 0.134 Uiso 0.640(19) 1 calc PR B 1 H39C H 0.2337 0.1697 0.1729 0.134 Uiso 0.640(19) 1 calc PR B 1 N13 N 0.2656(2) 0.1271(3) 0.2491(9) 0.071(2) Uani 0.640(19) 1 d PD B 1 O5 O 0.32343(19) 0.1311(2) 0.1370(9) 0.0744(19) Uani 0.640(19) 1 d PD B 1 C40 C 0.0652(2) 0.1252(2) -0.0868(11) 0.0438(19) Uani 1 1 d . . . H40 H 0.0869 0.1256 -0.1493 0.053 Uiso 1 1 calc R . . C41 C 0.0308(3) 0.1270(3) -0.3445(10) 0.066(3) Uani 1 1 d . . . H41A H 0.0167 0.1499 -0.3793 0.100 Uiso 1 1 calc R . . H41B H 0.0189 0.1030 -0.3828 0.100 Uiso 1 1 calc R . . H41C H 0.0557 0.1286 -0.3879 0.100 Uiso 1 1 calc R . . C42 C -0.0034(3) 0.1255(3) -0.0768(11) 0.073(3) Uani 1 1 d . . . H42A H 0.0011 0.1186 0.0349 0.109 Uiso 1 1 calc R . . H42B H -0.0198 0.1060 -0.1249 0.109 Uiso 1 1 calc R . . H42C H -0.0150 0.1515 -0.0822 0.109 Uiso 1 1 calc R . . C37' C 0.2972(5) 0.1463(6) 0.205(3) 0.060(8) Uani 0.360(19) 1 d PDU B 2 H37' H 0.2988 0.1736 0.2279 0.072 Uiso 0.360(19) 1 calc PR B 2 C38' C 0.2533(12) 0.0882(12) 0.241(6) 0.103(10) Uani 0.360(19) 1 d PU B 2 H38D H 0.2740 0.0709 0.2162 0.155 Uiso 0.360(19) 1 calc PR B 2 H38E H 0.2347 0.0859 0.1575 0.155 Uiso 0.360(19) 1 calc PR B 2 H38F H 0.2427 0.0807 0.3438 0.155 Uiso 0.360(19) 1 calc PR B 2 C39' C 0.2336(12) 0.1588(12) 0.294(6) 0.109(10) Uani 0.360(19) 1 d PU B 2 H39D H 0.2362 0.1668 0.4058 0.163 Uiso 0.360(19) 1 calc PR B 2 H39E H 0.2095 0.1468 0.2782 0.163 Uiso 0.360(19) 1 calc PR B 2 H39F H 0.2359 0.1820 0.2254 0.163 Uiso 0.360(19) 1 calc PR B 2 N13' N 0.2656(2) 0.1271(3) 0.2491(9) 0.071(2) Uani 0.360(19) 1 d P B 2 O5' O 0.32343(19) 0.1311(2) 0.1370(9) 0.0744(19) Uani 0.360(19) 1 d P B 2 N1 N 0.38310(18) 0.18783(16) 0.1298(8) 0.0344(15) Uani 1 1 d . B . N2 N 0.35784(18) 0.20916(18) 0.0583(8) 0.0370(16) Uani 1 1 d . . . N3 N 0.36673(19) 0.24822(18) 0.0793(8) 0.0372(15) Uani 1 1 d . B . N4 N 0.14316(18) 0.24394(17) 0.1121(7) 0.0333(15) Uani 1 1 d . . . N5 N 0.15289(19) 0.20559(17) 0.0873(8) 0.0379(16) Uani 1 1 d . . . N6 N 0.12755(17) 0.18235(17) 0.1531(8) 0.0329(15) Uani 1 1 d . . . N7 N 0.12450(18) 0.06050(17) 0.1527(8) 0.0371(16) Uani 1 1 d . . . N8 N 0.14918(19) 0.03672(17) 0.0834(7) 0.0358(16) Uani 1 1 d . . . N9 N 0.13655(19) -0.00113(17) 0.1075(8) 0.0355(15) Uani 1 1 d . . . N10 N 0.35987(19) 0.00858(15) 0.0936(8) 0.0341(15) Uani 1 1 d . . . N11 N 0.35242(19) 0.04770(16) 0.0699(8) 0.0374(16) Uani 1 1 d . B . N12 N 0.38000(18) 0.06816(17) 0.1363(8) 0.0376(16) Uani 1 1 d . B . N14 N 0.03255(19) 0.1263(2) -0.1664(8) 0.0480(16) Uani 1 1 d . . . O1 O 0.29475(18) 0.2796(2) 0.1973(8) 0.070(2) Uani 1 1 d D . . O2 O 0.21637(19) 0.2683(2) 0.2318(8) 0.074(2) Uani 1 1 d D . . O3 O 0.20972(16) -0.03392(15) 0.2079(7) 0.0456(14) Uani 1 1 d . . . O4 O 0.28672(16) -0.01123(15) 0.2286(7) 0.0451(14) Uani 1 1 d . . . O6 O 0.06899(16) 0.12393(17) 0.0592(7) 0.0531(14) 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 Cu1 0.0503(6) 0.0253(4) 0.0378(5) 0.0022(4) 0.0013(4) -0.0044(4) Cu2 0.0526(6) 0.0285(4) 0.0309(5) 0.0012(4) 0.0050(4) 0.0021(4) Cl1 0.0899(19) 0.0333(10) 0.1000(19) 0.0012(14) 0.0500(15) -0.0024(13) Cl2 0.1030(18) 0.0344(10) 0.0350(10) 0.0010(10) 0.0059(11) -0.0071(12) Cl3 0.117(2) 0.0402(12) 0.0611(14) -0.0002(11) 0.0481(14) -0.0003(13) Cl4 0.0882(17) 0.0382(10) 0.0312(10) 0.0020(10) -0.0038(10) 0.0036(11) C1 0.050(5) 0.025(4) 0.029(4) -0.007(3) 0.005(4) -0.004(3) C2 0.054(6) 0.031(4) 0.040(5) -0.001(4) -0.002(4) 0.000(4) C3 0.049(6) 0.043(5) 0.043(5) -0.004(4) -0.009(4) -0.006(4) C4 0.057(6) 0.041(5) 0.047(6) -0.009(4) 0.005(5) -0.011(4) C5 0.058(6) 0.025(4) 0.055(6) -0.003(4) 0.012(5) -0.004(4) C6 0.042(5) 0.029(4) 0.029(4) -0.001(3) 0.007(4) 0.000(3) C7 0.050(6) 0.045(5) 0.044(5) 0.008(4) 0.009(4) 0.014(4) C8 0.054(6) 0.050(5) 0.074(7) -0.003(5) 0.011(5) 0.013(4) C9' 0.053(8) 0.061(9) 0.051(8) -0.006(7) -0.003(7) 0.001(7) C10' 0.049(8) 0.052(8) 0.042(8) -0.011(7) 0.001(7) -0.001(7) C9 0.048(6) 0.051(6) 0.047(6) -0.011(5) 0.004(5) -0.005(5) C10 0.061(6) 0.069(7) 0.045(6) -0.008(5) -0.002(5) -0.006(6) C11 0.091(8) 0.057(6) 0.039(6) -0.017(4) 0.013(5) -0.037(5) C12 0.069(7) 0.034(4) 0.036(5) 0.001(4) 0.003(4) -0.010(4) C13 0.046(5) 0.030(4) 0.029(4) 0.002(3) -0.008(4) 0.003(3) C14 0.053(6) 0.026(4) 0.059(6) -0.006(4) -0.006(4) 0.005(4) C15 0.058(6) 0.046(5) 0.054(6) -0.005(4) 0.001(5) 0.022(4) C16 0.048(6) 0.051(5) 0.039(5) 0.000(4) 0.010(4) 0.010(4) C17 0.043(5) 0.037(4) 0.036(5) 0.003(3) 0.004(4) 0.002(3) C18 0.040(5) 0.026(4) 0.028(4) -0.005(3) -0.002(3) 0.006(3) C19 0.039(5) 0.035(4) 0.026(4) 0.006(3) 0.002(4) -0.004(3) C20 0.050(6) 0.043(4) 0.036(5) 0.001(4) 0.005(4) 0.005(4) C21 0.062(7) 0.056(6) 0.045(6) 0.002(5) 0.013(5) 0.000(5) C22 0.053(6) 0.057(5) 0.045(6) 0.011(4) 0.011(5) -0.013(4) C23 0.045(6) 0.036(4) 0.043(5) 0.005(4) 0.000(4) -0.011(4) C24 0.037(5) 0.036(4) 0.033(5) 0.006(3) 0.000(4) -0.003(3) C25 0.048(6) 0.034(4) 0.033(5) -0.001(3) 0.004(4) 0.002(4) C26 0.044(5) 0.032(4) 0.051(5) 0.000(4) 0.003(4) -0.001(3) C27 0.047(6) 0.065(6) 0.043(6) 0.020(4) -0.001(4) -0.007(4) C28 0.039(6) 0.082(7) 0.038(5) 0.007(5) -0.002(4) -0.001(4) C29 0.048(5) 0.031(4) 0.045(5) 0.000(4) -0.001(4) -0.008(3) C30 0.054(6) 0.027(4) 0.034(5) -0.007(3) 0.005(4) -0.006(4) C31 0.033(5) 0.029(4) 0.035(5) -0.001(3) 0.003(4) 0.000(3) C32 0.061(7) 0.030(4) 0.053(6) 0.002(4) -0.001(5) 0.005(4) C33 0.067(7) 0.041(5) 0.051(6) 0.012(4) -0.004(5) 0.011(4) C34 0.052(6) 0.054(5) 0.050(6) 0.003(5) -0.010(5) -0.005(4) C35 0.046(6) 0.035(4) 0.047(5) -0.002(4) 0.003(4) -0.006(4) C36 0.028(4) 0.031(4) 0.036(5) -0.002(3) 0.004(4) -0.001(3) C37 0.083(13) 0.048(9) 0.055(10) 0.004(7) -0.012(9) 0.001(8) C38 0.104(10) 0.109(10) 0.114(10) 0.003(8) 0.016(8) -0.010(8) C39 0.089(10) 0.083(9) 0.096(9) 0.019(7) 0.008(8) 0.014(7) N13 0.057(6) 0.100(7) 0.056(5) 0.000(5) 0.017(4) -0.001(6) O5 0.071(5) 0.073(5) 0.079(5) 0.014(4) 0.009(4) -0.011(4) C40 0.038(5) 0.019(3) 0.075(6) -0.003(4) 0.004(4) -0.005(3) C41 0.085(7) 0.068(6) 0.046(5) -0.004(5) -0.008(5) 0.006(6) C42 0.069(7) 0.090(7) 0.059(6) 0.007(6) 0.009(5) -0.001(6) C37' 0.09(2) 0.030(13) 0.061(17) 0.003(12) 0.010(15) -0.005(13) C38' 0.107(13) 0.098(12) 0.105(13) -0.007(9) 0.005(9) -0.005(9) C39' 0.107(13) 0.105(13) 0.114(13) 0.001(9) 0.005(9) 0.005(9) N13' 0.057(6) 0.100(7) 0.056(5) 0.000(5) 0.017(4) -0.001(6) O5' 0.071(5) 0.073(5) 0.079(5) 0.014(4) 0.009(4) -0.011(4) N1 0.041(4) 0.024(3) 0.038(4) -0.002(3) 0.003(3) 0.000(3) N2 0.033(4) 0.042(4) 0.037(4) 0.014(3) 0.002(3) 0.000(3) N3 0.048(4) 0.029(3) 0.034(4) 0.002(3) 0.004(3) 0.005(3) N4 0.042(4) 0.028(3) 0.030(4) 0.000(3) 0.002(3) -0.006(3) N5 0.044(5) 0.031(3) 0.039(4) 0.002(3) 0.007(3) -0.001(3) N6 0.039(4) 0.032(3) 0.027(4) -0.001(3) -0.001(3) -0.001(3) N7 0.046(4) 0.031(3) 0.035(4) 0.000(3) 0.006(3) 0.004(3) N8 0.052(5) 0.029(3) 0.027(4) 0.007(3) 0.001(3) -0.001(3) N9 0.044(4) 0.025(3) 0.038(4) -0.003(3) 0.002(3) 0.000(3) N10 0.047(4) 0.019(3) 0.036(4) -0.001(3) -0.003(3) 0.000(3) N11 0.052(5) 0.025(3) 0.035(4) 0.004(3) 0.002(3) -0.005(3) N12 0.042(4) 0.032(3) 0.039(4) 0.006(3) -0.003(3) -0.008(3) N14 0.057(5) 0.043(4) 0.044(4) 0.001(4) -0.002(3) -0.002(3) O1 0.049(5) 0.114(6) 0.048(4) -0.028(4) 0.012(3) -0.002(4) O2 0.054(5) 0.115(6) 0.053(5) -0.029(4) -0.002(3) -0.011(4) O3 0.042(4) 0.038(3) 0.056(4) 0.006(3) -0.012(3) -0.004(3) O4 0.042(4) 0.047(3) 0.046(4) -0.004(3) 0.005(3) 0.004(3) O6 0.070(4) 0.042(3) 0.047(3) -0.002(3) -0.006(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N12 1.997(6) . ? Cu1 N1 1.999(5) . ? Cu1 O5 2.090(7) . ? Cu1 Cl1 2.286(2) . ? Cu1 Cl2 2.437(2) . ? Cu2 N6 2.035(6) . ? Cu2 N7 2.044(6) . ? Cu2 Cl3 2.245(2) . ? Cu2 Cl4 2.293(2) . ? Cu2 O6 2.339(6) . ? C1 N1 1.380(9) . ? C1 C2 1.395(11) . ? C1 C6 1.397(10) . ? C2 C3 1.366(10) . ? C2 H2 0.9300 . ? C3 C4 1.412(11) . ? C3 H3 0.9300 . ? C4 C5 1.350(12) . ? C4 H4 0.9300 . ? C5 C6 1.399(10) . ? C5 H5 0.9300 . ? C6 N3 1.368(10) . ? C7 N3 1.455(9) . ? C7 C8 1.507(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O1 1.395(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9' O1 1.447(18) . ? C9' C10' 1.502(18) . ? C9' H9C 0.9700 . ? C9' H9D 0.9700 . ? C10' O2 1.517(16) . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C9 O1 1.453(11) . ? C9 C10 1.527(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O2 1.442(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O2 1.439(11) . ? C11 C12 1.509(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.452(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.371(10) . ? C13 C18 1.389(9) . ? C13 C14 1.398(10) . ? C14 C15 1.356(12) . ? C14 H14 0.9300 . ? C15 C16 1.405(11) . ? C15 H15 0.9300 . ? C16 C17 1.371(10) . ? C16 H16 0.9300 . ? C17 C18 1.399(10) . ? C17 H17 0.9300 . ? C18 N6 1.382(9) . ? C19 N7 1.382(9) . ? C19 C20 1.395(11) . ? C19 C24 1.397(10) . ? C20 C21 1.362(11) . ? C20 H20 0.9300 . ? C21 C22 1.412(11) . ? C21 H21 0.9300 . ? C22 C23 1.367(12) . ? C22 H22 0.9300 . ? C23 C24 1.396(10) . ? C23 H23 0.9300 . ? C24 N9 1.357(10) . ? C25 N9 1.464(9) . ? C25 C26 1.505(10) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O3 1.410(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O3 1.424(9) . ? C27 C28 1.477(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O4 1.430(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O4 1.414(9) . ? C29 C30 1.511(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N10 1.465(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N10 1.349(10) . ? C31 C36 1.399(9) . ? C31 C32 1.410(10) . ? C32 C33 1.365(12) . ? C32 H32 0.9300 . ? C33 C34 1.401(11) . ? C33 H33 0.9300 . ? C34 C35 1.362(11) . ? C34 H34 0.9300 . ? C35 C36 1.399(11) . ? C35 H35 0.9300 . ? C36 N12 1.375(9) . ? C37 O5 1.211(9) . ? C37 N13 1.349(12) . ? C37 H37 0.9300 . ? C38 N13 1.52(2) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N13 1.380(19) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O6 1.209(9) . ? C40 N14 1.338(9) . ? C40 H40 0.9300 . ? C41 N14 1.465(10) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N14 1.481(10) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C37' H37' 0.9300 . ? C38' H38D 0.9600 . ? C38' H38E 0.9600 . ? C38' H38F 0.9600 . ? C39' H39D 0.9600 . ? C39' H39E 0.9600 . ? C39' H39F 0.9600 . ? N1 N2 1.290(8) . ? N2 N3 1.352(8) . ? N4 N5 1.341(8) . ? N5 N6 1.308(8) . ? N7 N8 1.315(8) . ? N8 N9 1.355(8) . ? N10 N11 1.346(7) . ? N11 N12 1.317(8) . ? 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 N12 Cu1 N1 176.4(2) . . ? N12 Cu1 O5 91.0(3) . . ? N1 Cu1 O5 88.3(3) . . ? N12 Cu1 Cl1 88.8(2) . . ? N1 Cu1 Cl1 89.72(19) . . ? O5 Cu1 Cl1 144.2(2) . . ? N12 Cu1 Cl2 90.7(2) . . ? N1 Cu1 Cl2 93.0(2) . . ? O5 Cu1 Cl2 95.7(2) . . ? Cl1 Cu1 Cl2 120.12(10) . . ? N6 Cu2 N7 170.7(2) . . ? N6 Cu2 Cl3 91.71(19) . . ? N7 Cu2 Cl3 92.53(19) . . ? N6 Cu2 Cl4 90.01(19) . . ? N7 Cu2 Cl4 90.8(2) . . ? Cl3 Cu2 Cl4 148.29(11) . . ? N6 Cu2 O6 84.9(2) . . ? N7 Cu2 O6 86.1(2) . . ? Cl3 Cu2 O6 103.03(16) . . ? Cl4 Cu2 O6 108.66(16) . . ? N1 C1 C2 132.5(7) . . ? N1 C1 C6 106.7(7) . . ? C2 C1 C6 120.7(7) . . ? C3 C2 C1 116.7(7) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? C2 C3 C4 121.3(8) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 123.5(8) . . ? C5 C4 H4 118.3 . . ? C3 C4 H4 118.3 . . ? C4 C5 C6 115.1(7) . . ? C4 C5 H5 122.5 . . ? C6 C5 H5 122.5 . . ? N3 C6 C1 104.6(6) . . ? N3 C6 C5 132.7(7) . . ? C1 C6 C5 122.7(8) . . ? N3 C7 C8 112.1(7) . . ? N3 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N3 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O1 C8 C7 108.5(7) . . ? O1 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O1 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? O1 C9' C10' 102(2) . . ? O1 C9' H9C 111.4 . . ? C10' C9' H9C 111.4 . . ? O1 C9' H9D 111.4 . . ? C10' C9' H9D 111.4 . . ? H9C C9' H9D 109.3 . . ? C9' C10' O2 102(2) . . ? C9' C10' H10C 111.3 . . ? O2 C10' H10C 111.3 . . ? C9' C10' H10D 111.3 . . ? O2 C10' H10D 111.3 . . ? H10C C10' H10D 109.2 . . ? O1 C9 C10 104.8(9) . . ? O1 C9 H9A 110.8 . . ? C10 C9 H9A 110.8 . . ? O1 C9 H9B 110.8 . . ? C10 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? O2 C10 C9 108.8(10) . . ? O2 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O2 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O2 C11 C12 108.2(7) . . ? O2 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? O2 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N4 C12 C11 112.5(7) . . ? N4 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? N4 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? N4 C13 C18 105.0(6) . . ? N4 C13 C14 132.1(7) . . ? C18 C13 C14 122.9(8) . . ? C15 C14 C13 115.4(8) . . ? C15 C14 H14 122.3 . . ? C13 C14 H14 122.3 . . ? C14 C15 C16 123.3(8) . . ? C14 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C17 C16 C15 120.7(8) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 117.5(7) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? N6 C18 C13 107.3(7) . . ? N6 C18 C17 132.5(7) . . ? C13 C18 C17 120.1(7) . . ? N7 C19 C20 132.8(7) . . ? N7 C19 C24 106.4(7) . . ? C20 C19 C24 120.8(7) . . ? C21 C20 C19 116.8(8) . . ? C21 C20 H20 121.6 . . ? C19 C20 H20 121.6 . . ? C20 C21 C22 122.2(9) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 121.8(8) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 116.1(8) . . ? C22 C23 H23 122.0 . . ? C24 C23 H23 122.0 . . ? N9 C24 C23 132.9(7) . . ? N9 C24 C19 104.8(6) . . ? C23 C24 C19 122.3(8) . . ? N9 C25 C26 113.2(7) . . ? N9 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? N9 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? O3 C26 C25 108.6(6) . . ? O3 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O3 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? O3 C27 C28 108.7(7) . . ? O3 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? O3 C27 H27B 110.0 . . ? C28 C27 H27B 110.0 . . ? H27A C27 H27B 108.3 . . ? O4 C28 C27 114.5(7) . . ? O4 C28 H28A 108.6 . . ? C27 C28 H28A 108.6 . . ? O4 C28 H28B 108.6 . . ? C27 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? O4 C29 C30 109.4(6) . . ? O4 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? O4 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? N10 C30 C29 111.6(6) . . ? N10 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? N10 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? N10 C31 C36 105.0(6) . . ? N10 C31 C32 133.4(7) . . ? C36 C31 C32 121.6(8) . . ? C33 C32 C31 115.6(8) . . ? C33 C32 H32 122.2 . . ? C31 C32 H32 122.2 . . ? C32 C33 C34 122.9(8) . . ? C32 C33 H33 118.5 . . ? C34 C33 H33 118.5 . . ? C35 C34 C33 122.0(9) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C34 C35 C36 116.6(7) . . ? C34 C35 H35 121.7 . . ? C36 C35 H35 121.7 . . ? N12 C36 C31 106.7(7) . . ? N12 C36 C35 132.0(7) . . ? C31 C36 C35 121.3(7) . . ? O5 C37 N13 124.2(12) . . ? O5 C37 H37 117.9 . . ? N13 C37 H37 117.9 . . ? C37 N13 C39 128.8(13) . . ? C37 N13 C38 113.8(13) . . ? C39 N13 C38 117.3(14) . . ? C37 O5 Cu1 132.8(8) . . ? O6 C40 N14 125.7(8) . . ? O6 C40 H40 117.2 . . ? N14 C40 H40 117.2 . . ? N14 C41 H41A 109.5 . . ? N14 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N14 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N14 C42 H42A 109.5 . . ? N14 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N14 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? H38D C38' H38E 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? H39D C39' H39E 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? N2 N1 C1 110.3(6) . . ? N2 N1 Cu1 123.8(5) . . ? C1 N1 Cu1 125.9(5) . . ? N1 N2 N3 108.0(6) . . ? N2 N3 C6 110.4(6) . . ? N2 N3 C7 120.6(7) . . ? C6 N3 C7 129.0(7) . . ? N5 N4 C13 110.0(6) . . ? N5 N4 C12 121.2(6) . . ? C13 N4 C12 128.8(6) . . ? N6 N5 N4 108.9(6) . . ? N5 N6 C18 108.9(6) . . ? N5 N6 Cu2 123.8(5) . . ? C18 N6 Cu2 127.2(5) . . ? N8 N7 C19 110.9(6) . . ? N8 N7 Cu2 122.1(5) . . ? C19 N7 Cu2 127.0(5) . . ? N7 N8 N9 106.0(6) . . ? N8 N9 C24 111.9(6) . . ? N8 N9 C25 119.4(6) . . ? C24 N9 C25 128.6(6) . . ? N11 N10 C31 111.3(6) . . ? N11 N10 C30 119.5(6) . . ? C31 N10 C30 129.2(6) . . ? N12 N11 N10 107.2(6) . . ? N11 N12 C36 109.8(6) . . ? N11 N12 Cu1 123.4(5) . . ? C36 N12 Cu1 126.7(5) . . ? C40 N14 C41 121.7(7) . . ? C40 N14 C42 120.9(7) . . ? C41 N14 C42 117.4(7) . . ? C8 O1 C9' 133.4(16) . . ? C8 O1 C9 105.9(7) . . ? C9' O1 C9 40.0(11) . . ? C11 O2 C10 119.4(9) . . ? C11 O2 C10' 91.8(9) . . ? C10 O2 C10' 33.7(11) . . ? C26 O3 C27 113.0(6) . . ? C29 O4 C28 112.3(6) . . ? C40 O6 Cu2 116.1(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.046 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.096 ##############END##################