Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 #========================================================== data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Peter James Steel' 'Chris Richardson' _publ_contact_author_name 'Prof Peter James Steel' _publ_contact_author_address ; Department of Chemistry University of Canterbury Private Bag 4800 Christchurch NEW ZEALAND ; _publ_contact_author_email P.STEEL@CHEM.CANTERBURY.AC.NZ _publ_section_title ; Benzotriazole as a structural component in chelating and bridging heterocyclic ligands; ruthenium, palladium, copper and silver complexes ; data_3cr11ps(complex14) _database_code_CSD 190038 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H24 Cl4 N8 O Pd2' _chemical_formula_weight 807.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 10.820(2) _cell_length_b 15.273(2) _cell_length_c 17.715(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.210(10) _cell_angle_gamma 90.00 _cell_volume 2904.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.642 _exptl_absorpt_correction_type 'multi scans (SADABS)' _exptl_absorpt_correction_T_min 0.3970 _exptl_absorpt_correction_T_max 0.9524 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4282 _diffrn_reflns_av_R_equivalents 0.1881 _diffrn_reflns_av_sigmaI/netI 0.1840 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3789 _reflns_number_gt 1931 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The atomic displacement parameters of four atoms (C2A', C3A', N1'A and C2'B) were restrained to approximate to isotropic behaviour. ; _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^)+(0.0023P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3789 _refine_ls_number_parameters 363 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0496 _refine_ls_goodness_of_fit_ref 0.674 _refine_ls_restrained_S_all 0.674 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 Pd1 Pd 0.27408(7) -0.41070(5) 0.85171(4) 0.0224(2) Uani 1 1 d . . . Cl1 Cl 0.4243(2) -0.51899(16) 0.87046(13) 0.0346(6) Uani 1 1 d . . . Cl2 Cl 0.1187(2) -0.50839(15) 0.87218(14) 0.0347(7) Uani 1 1 d . . . N1A N 0.0727(6) -0.1832(5) 0.8545(4) 0.0196(19) Uani 1 1 d . . . N2A N 0.1663(7) -0.2392(5) 0.8750(4) 0.029(2) Uani 1 1 d . . . N3A N 0.1444(6) -0.3122(5) 0.8380(4) 0.022(2) Uani 1 1 d . . . C3AA C 0.0351(8) -0.3042(6) 0.7874(5) 0.019(2) Uani 1 1 d . . . C4A C -0.0252(7) -0.3616(6) 0.7325(5) 0.022(3) Uani 1 1 d . . . H4A H 0.0049 -0.4190 0.7255 0.027 Uiso 1 1 calc R . . C5A C -0.1312(8) -0.3293(6) 0.6893(5) 0.026(3) Uani 1 1 d . . . H5A H -0.1731 -0.3654 0.6505 0.031 Uiso 1 1 calc R . . C6A C -0.1797(8) -0.2444(6) 0.7008(5) 0.027(3) Uani 1 1 d . . . H6A H -0.2541 -0.2258 0.6708 0.032 Uiso 1 1 calc R . . C7A C -0.1196(8) -0.1876(6) 0.7558(5) 0.030(3) Uani 1 1 d . . . H7A H -0.1497 -0.1303 0.7635 0.037 Uiso 1 1 calc R . . C7AA C -0.0127(8) -0.2207(6) 0.7984(5) 0.018(2) Uani 1 1 d . . . C1A C 0.0804(7) -0.0917(5) 0.8815(4) 0.017(2) Uani 1 1 d . . . H1A1 H 0.0834 -0.0902 0.9376 0.021 Uiso 1 1 calc R . . H1A2 H 0.0058 -0.0589 0.8591 0.021 Uiso 1 1 calc R . . N1'A N 0.2783(6) -0.0175(5) 0.9154(4) 0.0150(17) Uani 1 1 d U . . C2'A C 0.1957(7) -0.0499(5) 0.8585(5) 0.012(2) Uani 1 1 d U . . C3'A C 0.2202(8) -0.0452(5) 0.7840(5) 0.018(2) Uani 1 1 d U . . H3'A H 0.1607 -0.0676 0.7447 0.022 Uiso 1 1 calc R . . C4'A C 0.3293(7) -0.0087(6) 0.7652(5) 0.027(3) Uani 1 1 d . . . H4'A H 0.3452 -0.0056 0.7137 0.032 Uiso 1 1 calc R . . C5'A C 0.4124(8) 0.0225(6) 0.8220(5) 0.027(2) Uani 1 1 d . . . H5'A H 0.4886 0.0475 0.8111 0.033 Uiso 1 1 calc R . . C6'A C 0.3863(7) 0.0178(6) 0.8954(5) 0.024(2) Uani 1 1 d . . . H6'A H 0.4460 0.0401 0.9346 0.028 Uiso 1 1 calc R . . Pd2 Pd 0.25443(7) -0.02110(5) 1.02831(4) 0.0194(2) Uani 1 1 d . . . Cl3 Cl 0.1769(2) 0.11898(14) 1.01549(13) 0.0295(6) Uani 1 1 d . . . Cl4 Cl 0.2332(2) -0.02268(15) 1.15571(13) 0.0267(6) Uani 1 1 d . . . N1B N 0.4104(7) -0.2637(5) 1.0019(4) 0.021(2) Uani 1 1 d . . . N2B N 0.4066(6) -0.1755(5) 0.9994(4) 0.0202(19) Uani 1 1 d . . . N3B N 0.3084(6) -0.1494(5) 1.0313(4) 0.019(2) Uani 1 1 d . . . C3AB C 0.2429(9) -0.2224(5) 1.0527(5) 0.017(2) Uani 1 1 d . . . C4B C 0.1332(9) -0.2311(6) 1.0842(5) 0.025(3) Uani 1 1 d . . . H4B H 0.0874 -0.1816 1.0975 0.030 Uiso 1 1 calc R . . C5B C 0.0939(9) -0.3137(6) 1.0953(5) 0.028(3) Uani 1 1 d . . . H5B H 0.0171 -0.3217 1.1151 0.034 Uiso 1 1 calc R . . C6B C 0.1619(8) -0.3881(6) 1.0787(5) 0.029(3) Uani 1 1 d . . . H6B H 0.1316 -0.4444 1.0898 0.034 Uiso 1 1 calc R . . C7B C 0.2711(8) -0.3816(6) 1.0471(5) 0.027(3) Uani 1 1 d . . . H7B H 0.3166 -0.4317 1.0347 0.032 Uiso 1 1 calc R . . C7AB C 0.3111(8) -0.2960(6) 1.0342(5) 0.017(2) Uani 1 1 d . . . C1B C 0.5040(8) -0.3113(6) 0.9641(5) 0.026(3) Uani 1 1 d . . . H1B1 H 0.4897 -0.3752 0.9673 0.031 Uiso 1 1 calc R . . H1B2 H 0.5885 -0.2983 0.9899 0.031 Uiso 1 1 calc R . . N1'B N 0.4053(7) -0.3200(5) 0.8281(4) 0.0197(19) Uani 1 1 d . . . C2'B C 0.4943(8) -0.2834(6) 0.8802(5) 0.020(2) Uani 1 1 d U . . C3'B C 0.5708(8) -0.2152(6) 0.8576(5) 0.029(3) Uani 1 1 d . . . H3'B H 0.6341 -0.1907 0.8934 0.035 Uiso 1 1 calc R . . C4'B C 0.5532(8) -0.1837(6) 0.7823(5) 0.028(3) Uani 1 1 d . . . H4'B H 0.6010 -0.1362 0.7669 0.033 Uiso 1 1 calc R . . C5'B C 0.4648(8) -0.2242(6) 0.7320(6) 0.028(3) Uani 1 1 d . . . H5'B H 0.4523 -0.2061 0.6803 0.034 Uiso 1 1 calc R . . C6'B C 0.3944(8) -0.2905(6) 0.7562(5) 0.021(2) Uani 1 1 d . . . H6'B H 0.3340 -0.3173 0.7198 0.026 Uiso 1 1 calc R . . O1C O 0.7585(7) -0.3968(6) 0.9672(5) 0.074(3) Uani 1 1 d . . . H1C H 0.7875 -0.4075 1.0125 0.111 Uiso 1 1 calc R . . C1C C 0.8528(10) -0.3579(7) 0.9288(6) 0.057(4) Uani 1 1 d . . . H1C1 H 0.8167 -0.3397 0.8777 0.086 Uiso 1 1 calc R . . H1C2 H 0.9193 -0.4006 0.9249 0.086 Uiso 1 1 calc R . . H1C3 H 0.8871 -0.3067 0.9575 0.086 Uiso 1 1 calc R . . 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 Pd1 0.0207(4) 0.0153(4) 0.0321(5) -0.0022(4) 0.0072(4) 0.0000(4) Cl1 0.0353(15) 0.0238(13) 0.0448(16) 0.0007(14) 0.0052(13) 0.0138(14) Cl2 0.0374(15) 0.0189(14) 0.0502(17) 0.0004(13) 0.0149(13) -0.0078(12) N1A 0.013(5) 0.018(4) 0.028(5) 0.001(4) 0.003(4) -0.002(4) N2A 0.018(5) 0.025(5) 0.044(6) 0.003(5) -0.004(4) 0.000(4) N3A 0.008(5) 0.012(4) 0.047(6) -0.004(4) 0.004(4) -0.002(4) C3AA 0.009(6) 0.017(5) 0.032(6) 0.002(5) 0.007(5) -0.003(5) C4A 0.006(6) 0.024(6) 0.036(7) -0.004(5) -0.003(5) -0.011(5) C5A 0.020(6) 0.022(6) 0.033(6) -0.010(5) -0.010(5) -0.012(5) C6A 0.015(6) 0.025(6) 0.037(7) -0.002(5) -0.009(5) -0.004(5) C7A 0.024(6) 0.019(6) 0.048(7) 0.008(6) 0.006(6) -0.008(5) C7AA 0.015(6) 0.016(5) 0.025(6) -0.006(5) 0.009(5) -0.003(5) C1A 0.016(5) 0.020(5) 0.015(5) 0.000(5) -0.002(4) 0.007(5) N1'A 0.015(3) 0.007(3) 0.021(3) 0.004(3) -0.003(3) -0.007(3) C2'A 0.007(4) 0.008(4) 0.021(4) 0.002(3) -0.001(3) 0.004(3) C3'A 0.017(4) 0.012(4) 0.025(4) -0.006(3) -0.003(4) -0.003(3) C4'A 0.023(6) 0.040(7) 0.020(6) -0.004(5) 0.012(5) -0.002(5) C5'A 0.021(5) 0.029(5) 0.031(6) 0.010(6) -0.002(5) 0.001(6) C6'A 0.016(5) 0.024(5) 0.028(6) 0.010(5) -0.010(4) -0.002(5) Pd2 0.0193(4) 0.0133(4) 0.0253(5) -0.0012(4) 0.0018(4) 0.0002(4) Cl3 0.0339(15) 0.0150(13) 0.0391(16) -0.0025(12) 0.0021(13) 0.0064(12) Cl4 0.0302(14) 0.0231(12) 0.0274(14) 0.0000(14) 0.0055(11) 0.0055(15) N1B 0.024(5) 0.021(5) 0.018(5) 0.004(4) 0.004(4) 0.000(4) N2B 0.024(5) 0.018(5) 0.020(5) -0.002(4) 0.007(4) -0.002(4) N3B 0.016(5) 0.033(5) 0.007(4) 0.002(4) -0.003(4) -0.005(4) C3AB 0.031(6) 0.001(5) 0.018(6) 0.000(4) 0.003(5) -0.001(5) C4B 0.030(7) 0.024(6) 0.022(6) -0.009(5) 0.007(5) -0.003(5) C5B 0.026(6) 0.018(6) 0.042(7) -0.005(5) 0.011(5) -0.008(5) C6B 0.035(7) 0.016(6) 0.034(7) 0.003(5) -0.001(6) -0.005(5) C7B 0.025(6) 0.029(6) 0.025(6) 0.000(5) -0.007(5) -0.007(5) C7AB 0.028(6) 0.018(5) 0.005(5) -0.004(4) 0.005(5) -0.001(5) C1B 0.027(6) 0.021(6) 0.030(6) -0.006(5) 0.001(5) 0.009(5) N1'B 0.020(5) 0.021(5) 0.019(5) -0.001(4) 0.007(4) 0.001(4) C2'B 0.017(4) 0.017(4) 0.026(4) -0.004(4) 0.006(4) 0.007(4) C3'B 0.023(6) 0.026(6) 0.038(7) -0.017(6) 0.001(5) -0.009(5) C4'B 0.025(6) 0.028(6) 0.031(7) 0.005(5) 0.010(5) 0.004(5) C5'B 0.022(7) 0.026(6) 0.036(7) -0.007(6) 0.007(5) -0.010(5) C6'B 0.015(6) 0.022(6) 0.028(6) -0.005(5) 0.003(5) -0.010(5) O1C 0.052(5) 0.092(7) 0.082(7) 0.038(7) 0.023(5) 0.020(6) C1C 0.063(9) 0.037(8) 0.072(10) 0.020(7) 0.007(8) -0.013(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N3A 2.050(7) . ? Pd1 N1'B 2.063(7) . ? Pd1 Cl2 2.310(2) . ? Pd1 Cl1 2.314(2) . ? N1A N2A 1.340(9) . ? N1A C7AA 1.392(10) . ? N1A C1A 1.476(10) . ? N2A N3A 1.299(9) . ? N3A C3AA 1.398(10) . ? C3AA C7AA 1.400(11) . ? C3AA C4A 1.406(11) . ? C4A C5A 1.387(11) . ? C5A C6A 1.425(11) . ? C6A C7A 1.401(12) . ? C7A C7AA 1.394(11) . ? C1A C2'A 1.502(10) . ? N1'A C2'A 1.354(10) . ? N1'A C6'A 1.374(9) . ? N1'A Pd2 2.049(6) . ? C2'A C3'A 1.380(10) . ? C3'A C4'A 1.384(10) . ? C4'A C5'A 1.350(11) . ? C5'A C6'A 1.365(10) . ? Pd2 N3B 2.044(7) . ? Pd2 Cl4 2.297(2) . ? Pd2 Cl3 2.299(2) . ? N1B N2B 1.349(9) . ? N1B C7AB 1.370(10) . ? N1B C1B 1.475(10) . ? N2B N3B 1.326(9) . ? N3B C3AB 1.398(10) . ? C3AB C4B 1.380(11) . ? C3AB C7AB 1.405(11) . ? C4B C5B 1.353(11) . ? C5B C6B 1.404(11) . ? C6B C7B 1.374(11) . ? C7B C7AB 1.405(11) . ? C1B C2'B 1.538(10) . ? N1'B C6'B 1.344(10) . ? N1'B C2'B 1.367(10) . ? C2'B C3'B 1.418(12) . ? C3'B C4'B 1.409(11) . ? C4'B C5'B 1.370(11) . ? C5'B C6'B 1.367(11) . ? O1C C1C 1.424(10) . ? 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 N3A Pd1 N1'B 87.8(3) . . ? N3A Pd1 Cl2 89.5(2) . . ? N1'B Pd1 Cl2 176.4(2) . . ? N3A Pd1 Cl1 178.0(2) . . ? N1'B Pd1 Cl1 91.2(2) . . ? Cl2 Pd1 Cl1 91.59(9) . . ? N2A N1A C7AA 110.0(7) . . ? N2A N1A C1A 120.5(7) . . ? C7AA N1A C1A 128.7(7) . . ? N3A N2A N1A 109.2(7) . . ? N2A N3A C3AA 109.5(7) . . ? N2A N3A Pd1 119.4(6) . . ? C3AA N3A Pd1 130.7(6) . . ? N3A C3AA C7AA 106.7(8) . . ? N3A C3AA C4A 132.1(8) . . ? C7AA C3AA C4A 121.2(8) . . ? C5A C4A C3AA 116.1(8) . . ? C4A C5A C6A 122.6(9) . . ? C7A C6A C5A 121.0(9) . . ? C7AA C7A C6A 115.8(9) . . ? N1A C7AA C7A 132.0(8) . . ? N1A C7AA C3AA 104.5(8) . . ? C7A C7AA C3AA 123.3(9) . . ? N1A C1A C2'A 109.2(6) . . ? C2'A N1'A C6'A 117.0(7) . . ? C2'A N1'A Pd2 124.4(6) . . ? C6'A N1'A Pd2 118.6(5) . . ? N1'A C2'A C3'A 120.3(8) . . ? N1'A C2'A C1A 116.5(7) . . ? C3'A C2'A C1A 123.2(8) . . ? C4'A C3'A C2'A 121.6(8) . . ? C5'A C4'A C3'A 118.1(8) . . ? C4'A C5'A C6'A 119.6(9) . . ? C5'A C6'A N1'A 123.4(8) . . ? N3B Pd2 N1'A 88.9(3) . . ? N3B Pd2 Cl4 91.6(2) . . ? N1'A Pd2 Cl4 178.2(2) . . ? N3B Pd2 Cl3 174.0(2) . . ? N1'A Pd2 Cl3 88.1(2) . . ? Cl4 Pd2 Cl3 91.53(9) . . ? N2B N1B C7AB 110.6(7) . . ? N2B N1B C1B 119.8(7) . . ? C7AB N1B C1B 129.2(8) . . ? N3B N2B N1B 107.9(7) . . ? N2B N3B C3AB 109.7(7) . . ? N2B N3B Pd2 121.2(5) . . ? C3AB N3B Pd2 128.2(6) . . ? C4B C3AB N3B 132.6(8) . . ? C4B C3AB C7AB 121.4(8) . . ? N3B C3AB C7AB 106.0(8) . . ? C5B C4B C3AB 116.8(9) . . ? C4B C5B C6B 122.8(9) . . ? C7B C6B C5B 121.8(9) . . ? C6B C7B C7AB 115.5(9) . . ? N1B C7AB C3AB 105.8(8) . . ? N1B C7AB C7B 132.5(8) . . ? C3AB C7AB C7B 121.7(8) . . ? N1B C1B C2'B 109.6(7) . . ? C6'B N1'B C2'B 118.2(8) . . ? C6'B N1'B Pd1 115.9(6) . . ? C2'B N1'B Pd1 125.7(6) . . ? N1'B C2'B C3'B 119.9(9) . . ? N1'B C2'B C1B 119.7(8) . . ? C3'B C2'B C1B 120.3(8) . . ? C4'B C3'B C2'B 120.2(9) . . ? C5'B C4'B C3'B 117.5(9) . . ? C6'B C5'B C4'B 120.1(9) . . ? N1'B C6'B C5'B 124.0(9) . . ? 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 C7AA N1A N2A N3A -2.7(10) . . . . ? C1A N1A N2A N3A -173.1(7) . . . . ? N1A N2A N3A C3AA 3.2(10) . . . . ? N1A N2A N3A Pd1 176.9(5) . . . . ? N1'B Pd1 N3A N2A -51.5(7) . . . . ? Cl2 Pd1 N3A N2A 130.8(7) . . . . ? Cl1 Pd1 N3A N2A 6(7) . . . . ? N1'B Pd1 N3A C3AA 120.5(8) . . . . ? Cl2 Pd1 N3A C3AA -57.1(8) . . . . ? Cl1 Pd1 N3A C3AA 178(100) . . . . ? N2A N3A C3AA C7AA -2.6(10) . . . . ? Pd1 N3A C3AA C7AA -175.3(6) . . . . ? N2A N3A C3AA C4A 176.4(9) . . . . ? Pd1 N3A C3AA C4A 3.7(14) . . . . ? N3A C3AA C4A C5A -177.0(9) . . . . ? C7AA C3AA C4A C5A 1.9(12) . . . . ? C3AA C4A C5A C6A -2.0(13) . . . . ? C4A C5A C6A C7A 1.9(15) . . . . ? C5A C6A C7A C7AA -1.3(13) . . . . ? N2A N1A C7AA C7A -175.3(9) . . . . ? C1A N1A C7AA C7A -5.8(16) . . . . ? N2A N1A C7AA C3AA 1.0(10) . . . . ? C1A N1A C7AA C3AA 170.5(8) . . . . ? C6A C7A C7AA N1A 176.9(9) . . . . ? C6A C7A C7AA C3AA 1.2(14) . . . . ? N3A C3AA C7AA N1A 0.9(10) . . . . ? C4A C3AA C7AA N1A -178.2(7) . . . . ? N3A C3AA C7AA C7A 177.6(8) . . . . ? C4A C3AA C7AA C7A -1.5(14) . . . . ? N2A N1A C1A C2'A 56.6(10) . . . . ? C7AA N1A C1A C2'A -111.9(9) . . . . ? C6'A N1'A C2'A C3'A -1.3(12) . . . . ? Pd2 N1'A C2'A C3'A -179.4(6) . . . . ? C6'A N1'A C2'A C1A 177.5(7) . . . . ? Pd2 N1'A C2'A C1A -0.6(10) . . . . ? N1A C1A C2'A N1'A -121.8(8) . . . . ? N1A C1A C2'A C3'A 57.0(10) . . . . ? N1'A C2'A C3'A C4'A 0.8(13) . . . . ? C1A C2'A C3'A C4'A -177.9(8) . . . . ? C2'A C3'A C4'A C5'A 0.2(13) . . . . ? C3'A C4'A C5'A C6'A -0.6(14) . . . . ? C4'A C5'A C6'A N1'A 0.0(15) . . . . ? C2'A N1'A C6'A C5'A 0.9(13) . . . . ? Pd2 N1'A C6'A C5'A 179.1(7) . . . . ? C2'A N1'A Pd2 N3B 78.8(7) . . . . ? C6'A N1'A Pd2 N3B -99.3(6) . . . . ? C2'A N1'A Pd2 Cl4 -175(67) . . . . ? C6'A N1'A Pd2 Cl4 7(7) . . . . ? C2'A N1'A Pd2 Cl3 -96.0(7) . . . . ? C6'A N1'A Pd2 Cl3 85.9(6) . . . . ? C7AB N1B N2B N3B 1.6(10) . . . . ? C1B N1B N2B N3B 174.4(7) . . . . ? N1B N2B N3B C3AB -2.4(9) . . . . ? N1B N2B N3B Pd2 -172.5(5) . . . . ? N1'A Pd2 N3B N2B 45.1(6) . . . . ? Cl4 Pd2 N3B N2B -133.2(6) . . . . ? Cl3 Pd2 N3B N2B 106(2) . . . . ? N1'A Pd2 N3B C3AB -123.0(7) . . . . ? Cl4 Pd2 N3B C3AB 58.7(7) . . . . ? Cl3 Pd2 N3B C3AB -63(2) . . . . ? N2B N3B C3AB C4B -176.5(10) . . . . ? Pd2 N3B C3AB C4B -7.4(15) . . . . ? N2B N3B C3AB C7AB 2.2(10) . . . . ? Pd2 N3B C3AB C7AB 171.4(6) . . . . ? N3B C3AB C4B C5B 177.7(9) . . . . ? C7AB C3AB C4B C5B -0.9(14) . . . . ? C3AB C4B C5B C6B 2.4(15) . . . . ? C4B C5B C6B C7B -2.7(16) . . . . ? C5B C6B C7B C7AB 1.4(14) . . . . ? N2B N1B C7AB C3AB -0.2(10) . . . . ? C1B N1B C7AB C3AB -172.2(8) . . . . ? N2B N1B C7AB C7B 177.4(9) . . . . ? C1B N1B C7AB C7B 5.5(16) . . . . ? C4B C3AB C7AB N1B 177.8(8) . . . . ? N3B C3AB C7AB N1B -1.2(10) . . . . ? C4B C3AB C7AB C7B -0.2(15) . . . . ? N3B C3AB C7AB C7B -179.2(8) . . . . ? C6B C7B C7AB N1B -177.4(9) . . . . ? C6B C7B C7AB C3AB -0.1(13) . . . . ? N2B N1B C1B C2'B -54.5(10) . . . . ? C7AB N1B C1B C2'B 116.8(9) . . . . ? N3A Pd1 N1'B C6'B -69.2(6) . . . . ? Cl2 Pd1 N1'B C6'B -28(4) . . . . ? Cl1 Pd1 N1'B C6'B 112.5(6) . . . . ? N3A Pd1 N1'B C2'B 105.4(7) . . . . ? Cl2 Pd1 N1'B C2'B 146(3) . . . . ? Cl1 Pd1 N1'B C2'B -72.9(7) . . . . ? C6'B N1'B C2'B C3'B 0.9(12) . . . . ? Pd1 N1'B C2'B C3'B -173.6(6) . . . . ? C6'B N1'B C2'B C1B 176.1(7) . . . . ? Pd1 N1'B C2'B C1B 1.5(11) . . . . ? N1B C1B C2'B N1'B -81.3(10) . . . . ? N1B C1B C2'B C3'B 93.9(10) . . . . ? N1'B C2'B C3'B C4'B 1.6(13) . . . . ? C1B C2'B C3'B C4'B -173.6(8) . . . . ? C2'B C3'B C4'B C5'B -3.1(13) . . . . ? C3'B C4'B C5'B C6'B 2.2(13) . . . . ? C2'B N1'B C6'B C5'B -1.8(13) . . . . ? Pd1 N1'B C6'B C5'B 173.2(7) . . . . ? C4'B C5'B C6'B N1'B 0.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.556 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.123 #===END data_3cr1(complex15) _database_code_CSD 190039 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H10 Cl2 Cu N6' _chemical_formula_weight 384.71 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.554(1) _cell_length_b 9.250(1) _cell_length_c 10.322(1) _cell_angle_alpha 88.79(1) _cell_angle_beta 72.78(1) _cell_angle_gamma 65.83(1) _cell_volume 707.01(13) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 55 _cell_measurement_theta_min 10 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.90 _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'siemens P4s' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3558 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2719 _reflns_number_observed 2010 _reflns_observed_criterion >2sigma(I) _computing_data_collection xscans _computing_cell_refinement xscans _computing_data_reduction xscans _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics xp _computing_publication_material xcif _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2719 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _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 0.27850(6) 0.34060(5) 0.30466(4) 0.01946(13) Uani 1 1 d . . . Cl1 Cl 0.18199(12) 0.28786(10) 0.14038(8) 0.0244(2) Uani 1 1 d . . . Cl2 Cl 0.22337(12) 0.44624(9) 0.51270(8) 0.0240(2) Uani 1 1 d . . . N1 N 0.4955(4) -0.1364(3) 0.3124(2) 0.0150(6) Uani 1 1 d . . . N2 N 0.4821(4) 0.0023(3) 0.2638(3) 0.0190(6) Uani 1 1 d . . . N3 N 0.3487(4) 0.1171(3) 0.3529(3) 0.0191(6) Uani 1 1 d . . . C3A C 0.2680(5) 0.0543(4) 0.4607(3) 0.0183(7) Uani 1 1 d . . . C4 C 0.1160(5) 0.1252(4) 0.5758(3) 0.0234(8) Uani 1 1 d . . . H4 H 0.0513 0.2377 0.5959 0.028 Uiso 1 1 calc R . . C5 C 0.0652(5) 0.0231(4) 0.6583(3) 0.0257(8) Uani 1 1 d . . . H5 H -0.0384 0.0666 0.7370 0.031 Uiso 1 1 calc R . . C6 C 0.1621(5) -0.1444(4) 0.6300(3) 0.0232(8) Uani 1 1 d . . . H6 H 0.1205 -0.2100 0.6895 0.028 Uiso 1 1 calc R . . C7 C 0.3137(5) -0.2149(4) 0.5198(3) 0.0205(7) Uani 1 1 d . . . H7 H 0.3810 -0.3274 0.5022 0.025 Uiso 1 1 calc R . . C7A C 0.3635(4) -0.1110(4) 0.4347(3) 0.0147(6) Uani 1 1 d . . . C1 C 0.6123(4) -0.2851(4) 0.2242(3) 0.0159(7) Uani 1 1 d . . . H1A H 0.6887 -0.3621 0.2726 0.019 Uiso 1 1 calc R . . H1B H 0.6925 -0.2659 0.1413 0.019 Uiso 1 1 calc R . . N1' N 0.5010(4) -0.3497(3) 0.1863(3) 0.0152(6) Uani 1 1 d . . . N2' N 0.4750(4) -0.4694(3) 0.2504(3) 0.0167(6) Uani 1 1 d . . . N3' N 0.3515(4) -0.4908(3) 0.2143(3) 0.0187(6) Uani 1 1 d . . . C3A' C 0.2926(5) -0.3816(4) 0.1262(3) 0.0179(7) Uani 1 1 d . . . C4' C 0.1627(5) -0.3533(4) 0.0607(3) 0.0209(7) Uani 1 1 d . . . H4' H 0.0956 -0.4154 0.0715 0.025 Uiso 1 1 calc R . . C5' C 0.1375(5) -0.2312(4) -0.0199(3) 0.0229(8) Uani 1 1 d . . . H5' H 0.0499 -0.2076 -0.0656 0.027 Uiso 1 1 calc R . . C6' C 0.2380(5) -0.1400(4) -0.0366(3) 0.0229(8) Uani 1 1 d . . . H6' H 0.2174 -0.0580 -0.0949 0.028 Uiso 1 1 calc R . . C7' C 0.3635(5) -0.1644(4) 0.0274(3) 0.0196(7) Uani 1 1 d . . . H7' H 0.4291 -0.1009 0.0171 0.024 Uiso 1 1 calc R . . C7A' C 0.3895(4) -0.2890(4) 0.1091(3) 0.0158(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 0.0286(3) 0.0185(2) 0.0192(2) 0.00681(15) -0.01018(18) -0.01600(19) Cl1 0.0323(5) 0.0306(4) 0.0214(4) 0.0052(3) -0.0103(4) -0.0227(4) Cl2 0.0330(5) 0.0255(4) 0.0209(4) 0.0043(3) -0.0113(4) -0.0175(4) N1 0.0153(15) 0.0162(12) 0.0148(13) 0.0027(10) -0.0025(11) -0.0096(11) N2 0.0257(17) 0.0183(13) 0.0181(13) 0.0067(11) -0.0075(13) -0.0139(13) N3 0.0265(17) 0.0153(13) 0.0194(14) 0.0031(11) -0.0058(13) -0.0135(13) C3A 0.0227(19) 0.0212(16) 0.0166(15) 0.0035(13) -0.0071(15) -0.0139(15) C4 0.022(2) 0.0186(16) 0.0254(18) -0.0013(14) -0.0027(15) -0.0077(15) C5 0.023(2) 0.0333(19) 0.0182(16) -0.0008(14) 0.0012(15) -0.0141(17) C6 0.028(2) 0.0277(18) 0.0181(16) 0.0067(14) -0.0054(15) -0.0169(16) C7 0.027(2) 0.0192(16) 0.0196(16) 0.0056(13) -0.0058(15) -0.0148(15) C7A 0.0142(17) 0.0192(15) 0.0140(15) 0.0024(12) -0.0047(13) -0.0102(13) C1 0.0129(18) 0.0200(15) 0.0154(15) 0.0029(12) -0.0033(14) -0.0086(14) N1' 0.0162(15) 0.0140(12) 0.0159(13) 0.0036(10) -0.0043(12) -0.0076(11) N2' 0.0214(16) 0.0139(12) 0.0173(13) 0.0030(10) -0.0057(12) -0.0103(12) N3' 0.0250(17) 0.0184(13) 0.0176(13) 0.0045(11) -0.0089(12) -0.0124(13) C3A' 0.0201(19) 0.0171(15) 0.0158(15) 0.0011(12) -0.0029(14) -0.0090(14) C4' 0.022(2) 0.0215(16) 0.0209(16) -0.0006(13) -0.0052(15) -0.0122(15) C5' 0.022(2) 0.0276(17) 0.0229(17) 0.0031(14) -0.0113(16) -0.0113(15) C6' 0.021(2) 0.0223(17) 0.0237(17) 0.0087(14) -0.0056(15) -0.0091(15) C7' 0.0187(19) 0.0200(16) 0.0184(16) 0.0037(13) -0.0014(15) -0.0097(15) C7A' 0.0136(17) 0.0176(15) 0.0140(14) -0.0003(12) -0.0018(13) -0.0059(13) _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 N3 2.000(2) . ? Cu1 N3' 2.021(3) 1_565 ? Cu1 Cl2 2.2137(9) . ? Cu1 Cl1 2.2335(9) . ? N1 N2 1.340(3) . ? N1 C7A 1.370(4) . ? N1 C1 1.452(4) . ? N2 N3 1.305(4) . ? N3 C3A 1.377(4) . ? C3A C7A 1.394(4) . ? C3A C4 1.397(5) . ? C4 C5 1.374(5) . ? C5 C6 1.413(5) . ? C6 C7 1.366(5) . ? C7 C7A 1.398(4) . ? C1 N1' 1.453(4) . ? N1' N2' 1.341(3) . ? N1' C7A' 1.361(4) . ? N2' N3' 1.304(4) . ? N3' C3A' 1.384(4) . ? N3' Cu1 2.021(3) 1_545 ? C3A' C7A' 1.393(5) . ? C3A' C4' 1.400(5) . ? C4' C5' 1.372(4) . ? C5' C6' 1.407(5) . ? C6' C7' 1.362(5) . ? C7' C7A' 1.397(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 N3 Cu1 N3' 149.31(12) . 1_565 ? N3 Cu1 Cl2 94.72(8) . . ? N3' Cu1 Cl2 93.16(8) 1_565 . ? N3 Cu1 Cl1 91.39(8) . . ? N3' Cu1 Cl1 96.08(8) 1_565 . ? Cl2 Cu1 Cl1 150.66(4) . . ? N2 N1 C7A 110.8(2) . . ? N2 N1 C1 119.6(2) . . ? C7A N1 C1 128.3(3) . . ? N3 N2 N1 107.8(2) . . ? N2 N3 C3A 110.0(2) . . ? N2 N3 Cu1 118.10(19) . . ? C3A N3 Cu1 131.4(2) . . ? N3 C3A C7A 106.8(3) . . ? N3 C3A C4 132.2(3) . . ? C7A C3A C4 120.9(3) . . ? C5 C4 C3A 116.3(3) . . ? C4 C5 C6 122.2(3) . . ? C7 C6 C5 122.0(3) . . ? C6 C7 C7A 115.7(3) . . ? N1 C7A C3A 104.6(3) . . ? N1 C7A C7 132.5(3) . . ? C3A C7A C7 122.8(3) . . ? N1 C1 N1' 108.8(3) . . ? N2' N1' C7A' 111.3(3) . . ? N2' N1' C1 118.9(2) . . ? C7A' N1' C1 128.8(3) . . ? N3' N2' N1' 107.6(2) . . ? N2' N3' C3A' 109.8(3) . . ? N2' N3' Cu1 115.40(19) . 1_545 ? C3A' N3' Cu1 134.7(2) . 1_545 ? N3' C3A' C7A' 106.8(3) . . ? N3' C3A' C4' 132.4(3) . . ? C7A' C3A' C4' 120.8(3) . . ? C5' C4' C3A' 116.5(3) . . ? C4' C5' C6' 121.7(3) . . ? C7' C6' C5' 122.7(3) . . ? C6' C7' C7A' 115.5(3) . . ? N1' C7A' C3A' 104.5(3) . . ? N1' C7A' C7' 132.8(3) . . ? C3A' C7A' C7' 122.7(3) . . ? 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 C7A N1 N2 N3 1.9(4) . . . . ? C1 N1 N2 N3 169.6(3) . . . . ? N1 N2 N3 C3A -2.0(4) . . . . ? N1 N2 N3 Cu1 -174.99(19) . . . . ? N3' Cu1 N3 N2 -37.3(4) 1_565 . . . ? Cl2 Cu1 N3 N2 -141.7(2) . . . . ? Cl1 Cu1 N3 N2 67.1(2) . . . . ? N3' Cu1 N3 C3A 151.4(3) 1_565 . . . ? Cl2 Cu1 N3 C3A 47.1(3) . . . . ? Cl1 Cu1 N3 C3A -104.2(3) . . . . ? N2 N3 C3A C7A 1.3(4) . . . . ? Cu1 N3 C3A C7A 173.1(2) . . . . ? N2 N3 C3A C4 -175.5(4) . . . . ? Cu1 N3 C3A C4 -3.7(6) . . . . ? N3 C3A C4 C5 175.0(3) . . . . ? C7A C3A C4 C5 -1.5(5) . . . . ? C3A C4 C5 C6 0.8(5) . . . . ? C4 C5 C6 C7 0.9(6) . . . . ? C5 C6 C7 C7A -1.9(5) . . . . ? N2 N1 C7A C3A -1.1(3) . . . . ? C1 N1 C7A C3A -167.4(3) . . . . ? N2 N1 C7A C7 175.1(3) . . . . ? C1 N1 C7A C7 8.8(6) . . . . ? N3 C3A C7A N1 -0.1(3) . . . . ? C4 C3A C7A N1 177.1(3) . . . . ? N3 C3A C7A C7 -176.8(3) . . . . ? C4 C3A C7A C7 0.5(5) . . . . ? C6 C7 C7A N1 -174.4(3) . . . . ? C6 C7 C7A C3A 1.2(5) . . . . ? N2 N1 C1 N1' -107.1(3) . . . . ? C7A N1 C1 N1' 58.1(4) . . . . ? N1 C1 N1' N2' -101.6(3) . . . . ? N1 C1 N1' C7A' 65.7(4) . . . . ? C7A' N1' N2' N3' 1.4(3) . . . . ? C1 N1' N2' N3' 170.9(2) . . . . ? N1' N2' N3' C3A' -0.9(3) . . . . ? N1' N2' N3' Cu1 -177.23(17) . . . 1_545 ? N2' N3' C3A' C7A' 0.1(3) . . . . ? Cu1 N3' C3A' C7A' 175.4(2) 1_545 . . . ? N2' N3' C3A' C4' -179.1(3) . . . . ? Cu1 N3' C3A' C4' -3.8(5) 1_545 . . . ? N3' C3A' C4' C5' 179.2(3) . . . . ? C7A' C3A' C4' C5' 0.0(5) . . . . ? C3A' C4' C5' C6' 0.5(5) . . . . ? C4' C5' C6' C7' -1.2(5) . . . . ? C5' C6' C7' C7A' 1.3(5) . . . . ? N2' N1' C7A' C3A' -1.3(3) . . . . ? C1 N1' C7A' C3A' -169.4(3) . . . . ? N2' N1' C7A' C7' 178.6(3) . . . . ? C1 N1' C7A' C7' 10.5(5) . . . . ? N3' C3A' C7A' N1' 0.7(3) . . . . ? C4' C3A' C7A' N1' -179.9(3) . . . . ? N3' C3A' C7A' C7' -179.2(3) . . . . ? C4' C3A' C7A' C7' 0.1(5) . . . . ? C6' C7' C7A' N1' 179.3(3) . . . . ? C6' C7' C7A' C3A' -0.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.773 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.086 #===END data_3cr12(complex16) _database_code_CSD 190040 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 223-225 _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cu N10 O8' _chemical_formula_weight 644.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.720(1) _cell_length_b 12.016(1) _cell_length_c 14.921(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.14(1) _cell_angle_gamma 90.00 _cell_volume 1347.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13 _cell_measurement_theta_max 14 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 0.879 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.68 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Siemens P4s' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.25 _diffrn_reflns_number 3157 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2941 _reflns_number_gt 2007 _reflns_threshold_expression >2sigma(I) _computing_data_collection xscans _computing_cell_refinement xscans _computing_data_reduction xscans _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics xp _computing_publication_material xcif _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^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2941 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.0000 0.0000 0.5000 0.02268(13) Uani 1 2 d S N1 N 0.0874(2) 0.20918(15) 0.42658(12) 0.0201(4) Uani 1 1 d . N2 N 0.1381(3) 0.09979(16) 0.42955(13) 0.0231(4) Uani 1 1 d . N3 N 0.2693(3) 0.08607(17) 0.38896(13) 0.0257(5) Uani 1 1 d . C3A C 0.3071(3) 0.1894(2) 0.35690(15) 0.0234(5) Uani 1 1 d . C4 C 0.4384(3) 0.2178(2) 0.30816(17) 0.0312(6) Uani 1 1 d . H4 H 0.5148 0.1634 0.2916 0.037 Uiso 1 1 calc R C5 C 0.4493(4) 0.3281(2) 0.28609(17) 0.0337(6) Uani 1 1 d . H5 H 0.5349 0.3506 0.2530 0.040 Uiso 1 1 calc R C6 C 0.3360(4) 0.4092(2) 0.31134(17) 0.0319(6) Uani 1 1 d . H6 H 0.3499 0.4847 0.2953 0.038 Uiso 1 1 calc R C7 C 0.2059(3) 0.3832(2) 0.35845(17) 0.0278(6) Uani 1 1 d . H7 H 0.1300 0.4381 0.3747 0.033 Uiso 1 1 calc R C7A C 0.1933(3) 0.26973(19) 0.38069(14) 0.0203(5) Uani 1 1 d . N1' N -0.1151(3) 0.15019(15) 0.51057(13) 0.0224(4) Uani 1 1 d . C2' C -0.0572(3) 0.23690(19) 0.46768(15) 0.0206(5) Uani 1 1 d . C3' C -0.1309(3) 0.3427(2) 0.46317(17) 0.0265(5) Uani 1 1 d . H3' H -0.0876 0.4014 0.4316 0.032 Uiso 1 1 calc R C4' C -0.2704(3) 0.3598(2) 0.50656(17) 0.0291(6) Uani 1 1 d . H4' H -0.3251 0.4309 0.5044 0.035 Uiso 1 1 calc R C5' C -0.3296(3) 0.2724(2) 0.55303(18) 0.0304(6) Uani 1 1 d . H5' H -0.4225 0.2834 0.5843 0.036 Uiso 1 1 calc R C6' C -0.2502(3) 0.1691(2) 0.55273(17) 0.0293(6) Uani 1 1 d . H6' H -0.2922 0.1091 0.5834 0.035 Uiso 1 1 calc R O10 O 0.2020(3) 0.03184(17) 0.63646(13) 0.0384(5) Uani 1 1 d . H10 H 0.208(5) -0.010(3) 0.675(2) 0.058 Uiso 1 1 d . C10 C 0.3491(5) 0.1022(3) 0.6511(2) 0.0602(10) Uani 1 1 d . H10A H 0.4543 0.0598 0.6450 0.090 Uiso 1 1 calc R H10B H 0.3693 0.1339 0.7131 0.090 Uiso 1 1 calc R H10C H 0.3273 0.1623 0.6056 0.090 Uiso 1 1 calc R N10 N 0.2203(3) -0.10148(18) 0.83696(15) 0.0319(5) Uani 1 1 d . O11 O 0.2108(3) -0.11893(17) 0.91821(12) 0.0429(5) Uani 1 1 d . O12 O 0.3533(3) -0.05290(18) 0.82078(15) 0.0537(6) Uani 1 1 d . O13 O 0.0972(3) -0.1295(2) 0.77079(14) 0.0597(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 0.0285(2) 0.01604(19) 0.0285(2) 0.00307(19) 0.01683(17) 0.0023(2) N1 0.0237(10) 0.0161(9) 0.0220(9) 0.0018(7) 0.0085(8) -0.0008(8) N2 0.0270(11) 0.0192(10) 0.0261(10) 0.0006(8) 0.0124(9) 0.0001(9) N3 0.0281(11) 0.0238(11) 0.0289(11) -0.0007(9) 0.0139(9) 0.0009(9) C3A 0.0280(13) 0.0234(12) 0.0197(11) 0.0008(9) 0.0075(10) -0.0033(10) C4 0.0320(14) 0.0355(15) 0.0304(13) -0.0009(11) 0.0161(12) -0.0018(12) C5 0.0346(15) 0.0398(16) 0.0307(13) 0.0057(12) 0.0157(12) -0.0092(12) C6 0.0359(15) 0.0275(14) 0.0325(14) 0.0080(11) 0.0080(12) -0.0063(12) C7 0.0308(14) 0.0244(13) 0.0284(13) 0.0028(10) 0.0072(11) -0.0013(11) C7A 0.0211(12) 0.0240(12) 0.0157(10) -0.0004(9) 0.0039(9) -0.0025(10) N1' 0.0264(10) 0.0176(10) 0.0260(10) 0.0031(8) 0.0120(9) 0.0027(8) C2' 0.0240(12) 0.0200(11) 0.0187(10) -0.0008(9) 0.0070(9) -0.0016(10) C3' 0.0282(13) 0.0193(12) 0.0326(13) 0.0025(10) 0.0084(11) 0.0001(10) C4' 0.0293(14) 0.0200(12) 0.0379(14) -0.0019(10) 0.0075(12) 0.0041(10) C5' 0.0280(14) 0.0286(14) 0.0386(14) -0.0014(11) 0.0157(12) 0.0032(11) C6' 0.0310(14) 0.0243(13) 0.0381(14) 0.0036(11) 0.0192(12) 0.0002(11) O10 0.0428(11) 0.0398(12) 0.0297(10) 0.0080(8) 0.0021(9) -0.0064(9) C10 0.047(2) 0.063(2) 0.065(2) 0.0163(19) 0.0021(17) -0.0182(18) N10 0.0374(13) 0.0276(12) 0.0317(12) -0.0001(9) 0.0101(11) -0.0001(10) O11 0.0494(13) 0.0516(13) 0.0311(10) 0.0043(9) 0.0163(9) -0.0099(10) O12 0.0667(15) 0.0481(13) 0.0579(14) -0.0116(11) 0.0385(12) -0.0231(12) O13 0.0646(16) 0.0609(16) 0.0416(12) -0.0045(11) -0.0127(12) -0.0027(13) _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 N1' 2.0335(19) 3_556 ? Cu1 N1' 2.0335(19) . ? Cu1 N2 2.0467(18) 3_556 ? Cu1 N2 2.0467(18) . ? Cu1 O10 2.2978(19) . ? Cu1 O10 2.2978(19) 3_556 ? N1 N2 1.369(3) . ? N1 C7A 1.386(3) . ? N1 C2' 1.430(3) . ? N2 N3 1.303(3) . ? N3 C3A 1.385(3) . ? C3A C7A 1.404(3) . ? C3A C4 1.417(3) . ? C4 C5 1.373(4) . ? C5 C6 1.416(4) . ? C6 C7 1.387(3) . ? C7 C7A 1.411(3) . ? N1' C2' 1.351(3) . ? N1' C6' 1.354(3) . ? C2' C3' 1.388(3) . ? C3' C4' 1.392(3) . ? C4' C5' 1.391(3) . ? C5' C6' 1.385(3) . ? O10 C10 1.393(4) . ? N10 O11 1.249(3) . ? N10 O13 1.251(3) . ? N10 O12 1.251(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 N1' Cu1 N1' 180.0 3_556 . ? N1' Cu1 N2 78.91(7) 3_556 3_556 ? N1' Cu1 N2 101.09(7) . 3_556 ? N1' Cu1 N2 101.09(7) 3_556 . ? N1' Cu1 N2 78.91(7) . . ? N2 Cu1 N2 180.0 3_556 . ? N1' Cu1 O10 89.77(8) 3_556 . ? N1' Cu1 O10 90.23(8) . . ? N2 Cu1 O10 88.29(8) 3_556 . ? N2 Cu1 O10 91.71(8) . . ? N1' Cu1 O10 90.23(8) 3_556 3_556 ? N1' Cu1 O10 89.77(8) . 3_556 ? N2 Cu1 O10 91.71(8) 3_556 3_556 ? N2 Cu1 O10 88.29(8) . 3_556 ? O10 Cu1 O10 180.0 . 3_556 ? N2 N1 C7A 108.88(18) . . ? N2 N1 C2' 117.06(17) . . ? C7A N1 C2' 134.05(19) . . ? N3 N2 N1 110.67(18) . . ? N3 N2 Cu1 135.66(16) . . ? N1 N2 Cu1 113.61(13) . . ? N2 N3 C3A 107.11(19) . . ? N3 C3A C7A 109.61(19) . . ? N3 C3A C4 128.7(2) . . ? C7A C3A C4 121.7(2) . . ? C5 C4 C3A 116.5(2) . . ? C4 C5 C6 121.7(2) . . ? C7 C6 C5 122.8(2) . . ? C6 C7 C7A 115.7(2) . . ? N1 C7A C3A 103.72(19) . . ? N1 C7A C7 134.7(2) . . ? C3A C7A C7 121.6(2) . . ? C2' N1' C6' 117.6(2) . . ? C2' N1' Cu1 116.76(15) . . ? C6' N1' Cu1 125.55(16) . . ? N1' C2' C3' 123.6(2) . . ? N1' C2' N1 113.47(19) . . ? C3' C2' N1 123.0(2) . . ? C2' C3' C4' 117.7(2) . . ? C5' C4' C3' 119.8(2) . . ? C6' C5' C4' 118.6(2) . . ? N1' C6' C5' 122.7(2) . . ? C10 O10 Cu1 127.23(18) . . ? O11 N10 O13 121.3(2) . . ? O11 N10 O12 119.8(2) . . ? O13 N10 O12 118.9(2) . . ? 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 C7A N1 N2 N3 0.1(3) . . . . ? C2' N1 N2 N3 179.31(18) . . . . ? C7A N1 N2 Cu1 177.70(14) . . . . ? C2' N1 N2 Cu1 -3.1(2) . . . . ? N1' Cu1 N2 N3 -2.6(2) 3_556 . . . ? N1' Cu1 N2 N3 177.4(2) . . . . ? N2 Cu1 N2 N3 -125(6) 3_556 . . . ? O10 Cu1 N2 N3 87.5(2) . . . . ? O10 Cu1 N2 N3 -92.5(2) 3_556 . . . ? N1' Cu1 N2 N1 -179.37(15) 3_556 . . . ? N1' Cu1 N2 N1 0.63(15) . . . . ? N2 Cu1 N2 N1 58(6) 3_556 . . . ? O10 Cu1 N2 N1 -89.27(16) . . . . ? O10 Cu1 N2 N1 90.73(16) 3_556 . . . ? N1 N2 N3 C3A -0.5(2) . . . . ? Cu1 N2 N3 C3A -177.34(18) . . . . ? N2 N3 C3A C7A 0.7(3) . . . . ? N2 N3 C3A C4 -179.9(2) . . . . ? N3 C3A C4 C5 -178.8(2) . . . . ? C7A C3A C4 C5 0.5(4) . . . . ? C3A C4 C5 C6 0.5(4) . . . . ? C4 C5 C6 C7 -1.0(4) . . . . ? C5 C6 C7 C7A 0.4(4) . . . . ? N2 N1 C7A C3A 0.3(2) . . . . ? C2' N1 C7A C3A -178.7(2) . . . . ? N2 N1 C7A C7 -178.5(3) . . . . ? C2' N1 C7A C7 2.5(4) . . . . ? N3 C3A C7A N1 -0.6(2) . . . . ? C4 C3A C7A N1 180.0(2) . . . . ? N3 C3A C7A C7 178.4(2) . . . . ? C4 C3A C7A C7 -1.0(4) . . . . ? C6 C7 C7A N1 179.2(2) . . . . ? C6 C7 C7A C3A 0.5(4) . . . . ? N1' Cu1 N1' C2' -14(57) 3_556 . . . ? N2 Cu1 N1' C2' -177.93(17) 3_556 . . . ? N2 Cu1 N1' C2' 2.07(17) . . . . ? O10 Cu1 N1' C2' 93.77(18) . . . . ? O10 Cu1 N1' C2' -86.23(18) 3_556 . . . ? N1' Cu1 N1' C6' 163(59) 3_556 . . . ? N2 Cu1 N1' C6' -1.5(2) 3_556 . . . ? N2 Cu1 N1' C6' 178.5(2) . . . . ? O10 Cu1 N1' C6' -89.8(2) . . . . ? O10 Cu1 N1' C6' 90.2(2) 3_556 . . . ? C6' N1' C2' C3' -1.3(4) . . . . ? Cu1 N1' C2' C3' 175.40(19) . . . . ? C6' N1' C2' N1 179.0(2) . . . . ? Cu1 N1' C2' N1 -4.2(3) . . . . ? N2 N1 C2' N1' 4.8(3) . . . . ? C7A N1 C2' N1' -176.2(2) . . . . ? N2 N1 C2' C3' -174.8(2) . . . . ? C7A N1 C2' C3' 4.1(4) . . . . ? N1' C2' C3' C4' 0.9(4) . . . . ? N1 C2' C3' C4' -179.5(2) . . . . ? C2' C3' C4' C5' 0.6(4) . . . . ? C3' C4' C5' C6' -1.7(4) . . . . ? C2' N1' C6' C5' 0.2(4) . . . . ? Cu1 N1' C6' C5' -176.2(2) . . . . ? C4' C5' C6' N1' 1.3(4) . . . . ? N1' Cu1 O10 C10 104.4(3) 3_556 . . . ? N1' Cu1 O10 C10 -75.6(3) . . . . ? N2 Cu1 O10 C10 -176.7(3) 3_556 . . . ? N2 Cu1 O10 C10 3.3(3) . . . . ? O10 Cu1 O10 C10 -42(100) 3_556 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.420 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.067 #===END data_3cra(complex17) _database_code_CSD 190041 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H32 Cl4 Cu2 N16' _chemical_formula_weight 1053.74 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.161(3) _cell_length_b 10.464(3) _cell_length_c 11.130(3) _cell_angle_alpha 103.268(3) _cell_angle_beta 107.246(3) _cell_angle_gamma 91.123(3) _cell_volume 1095.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cuboid _exptl_crystal_colour green _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5866 _exptl_absorpt_correction_T_max 0.6239 _exptl_absorpt_process_details 'Blessing, Acta Cyrst. (1995) A57 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'SMART CCD (Siemens)' _diffrn_measurement_method '0.5 degree scans in omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13315 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.30 _reflns_number_total 4319 _reflns_number_gt 4125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT PLUS (Siemens, 1999)' _computing_data_reduction 'SAINT PLUS (Siemens, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Xp _computing_publication_material xcif _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^)+(0.0389P)^2^+0.5157P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4319 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.382470(17) 0.617019(16) 0.512969(15) 0.01823(7) Uani 1 1 d . . . Cl1 Cl 0.58472(4) 0.56786(3) 0.40512(3) 0.02097(9) Uani 1 1 d . . . Cl2 Cl 0.30380(4) 0.80443(4) 0.45979(4) 0.02563(9) Uani 1 1 d . . . N1A N 0.56342(13) 0.81204(12) 0.89542(12) 0.0198(3) Uani 1 1 d . . . N2A N 0.46931(13) 0.72771(13) 0.79231(12) 0.0219(3) Uani 1 1 d . . . N3A N 0.50383(13) 0.72937(12) 0.68860(12) 0.0203(3) Uani 1 1 d . . . C7AA C 0.66265(15) 0.86940(14) 0.85591(14) 0.0195(3) Uani 1 1 d . . . C7A C 0.78144(16) 0.96015(15) 0.92091(15) 0.0240(3) Uani 1 1 d . . . H7A H 0.8104 0.9946 1.0124 0.029 Uiso 1 1 calc R . . C6A C 0.85293(16) 0.99579(16) 0.84358(16) 0.0269(3) Uani 1 1 d . . . H6A H 0.9337 1.0559 0.8834 0.032 Uiso 1 1 calc R . . C5A C 0.80964(17) 0.94557(15) 0.70695(16) 0.0258(3) Uani 1 1 d . . . H5A H 0.8609 0.9745 0.6577 0.031 Uiso 1 1 calc R . . C4A C 0.69404(16) 0.85504(15) 0.64319(15) 0.0232(3) Uani 1 1 d . . . H4A H 0.6654 0.8209 0.5517 0.028 Uiso 1 1 calc R . . C3AA C 0.62140(15) 0.81653(14) 0.72128(14) 0.0190(3) Uani 1 1 d . . . N1A' N 0.63876(15) 0.92376(13) 1.11399(13) 0.0275(3) Uani 1 1 d . . . C2A' C 0.54620(16) 0.83277(15) 1.02145(14) 0.0210(3) Uani 1 1 d . . . C3A' C 0.43925(17) 0.76102(16) 1.03995(16) 0.0274(3) Uani 1 1 d . . . H3A' H 0.3762 0.6979 0.9702 0.033 Uiso 1 1 calc R . . C4A' C 0.42935(19) 0.78617(17) 1.16477(17) 0.0309(4) Uani 1 1 d . . . H4A' H 0.3588 0.7398 1.1825 0.037 Uiso 1 1 calc R . . C5A' C 0.52451(19) 0.88063(17) 1.26436(16) 0.0315(4) Uani 1 1 d . . . H5A' H 0.5196 0.8996 1.3505 0.038 Uiso 1 1 calc R . . C6A' C 0.6259(2) 0.94559(17) 1.23411(16) 0.0320(4) Uani 1 1 d . . . H6A' H 0.6902 1.0094 1.3020 0.038 Uiso 1 1 calc R . . N1B N 0.15216(13) 0.42062(12) 0.14112(12) 0.0198(3) Uani 1 1 d . . . N2B N 0.25792(13) 0.50284(13) 0.23453(12) 0.0219(3) Uani 1 1 d . . . N3B N 0.24298(13) 0.50310(12) 0.34684(12) 0.0211(3) Uani 1 1 d . . . C3BA C 0.12589(15) 0.42058(14) 0.32954(14) 0.0192(3) Uani 1 1 d . . . C4B C 0.06897(16) 0.38738(15) 0.42008(15) 0.0233(3) Uani 1 1 d . . . H4B H 0.1105 0.4225 0.5107 0.028 Uiso 1 1 calc R . . C5B C -0.05054(17) 0.30108(17) 0.37153(17) 0.0285(3) Uani 1 1 d . . . H5B H -0.0915 0.2762 0.4302 0.034 Uiso 1 1 calc R . . C6B C -0.11296(16) 0.24923(17) 0.23582(17) 0.0292(4) Uani 1 1 d . . . H6B H -0.1952 0.1911 0.2062 0.035 Uiso 1 1 calc R . . C7B C -0.05787(16) 0.28059(16) 0.14549(16) 0.0250(3) Uani 1 1 d . . . H7B H -0.0998 0.2457 0.0549 0.030 Uiso 1 1 calc R . . C7BA C 0.06491(15) 0.36783(14) 0.19602(14) 0.0196(3) Uani 1 1 d . . . N1B' N 0.03477(15) 0.32870(14) -0.07710(13) 0.0296(3) Uani 1 1 d . . . C2B' C 0.15136(16) 0.39507(14) 0.00911(14) 0.0210(3) Uani 1 1 d . . . C3B' C 0.26715(17) 0.43602(16) -0.02063(16) 0.0273(3) Uani 1 1 d . . . H3B' H 0.3468 0.4832 0.0452 0.033 Uiso 1 1 calc R . . C4B' C 0.2608(2) 0.40491(18) -0.14980(17) 0.0341(4) Uani 1 1 d . . . H4B' H 0.3363 0.4315 -0.1753 0.041 Uiso 1 1 calc R . . C5B' C 0.1415(2) 0.33352(18) -0.24270(16) 0.0358(4) Uani 1 1 d . . . H5B' H 0.1356 0.3093 -0.3319 0.043 Uiso 1 1 calc R . . C6B' C 0.0320(2) 0.29879(18) -0.20208(17) 0.0365(4) Uani 1 1 d . . . H6B' H -0.0490 0.2515 -0.2659 0.044 Uiso 1 1 calc R . . 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 0.01930(10) 0.01932(11) 0.01203(10) 0.00009(7) 0.00203(7) -0.00354(7) Cl1 0.02291(18) 0.02205(18) 0.01683(17) 0.00298(13) 0.00607(13) -0.00173(13) Cl2 0.0292(2) 0.02304(18) 0.02009(18) 0.00316(14) 0.00251(14) 0.00108(14) N1A 0.0211(6) 0.0191(6) 0.0146(6) -0.0001(5) 0.0024(5) -0.0020(5) N2A 0.0234(6) 0.0227(6) 0.0149(6) 0.0000(5) 0.0028(5) -0.0028(5) N3A 0.0219(6) 0.0207(6) 0.0156(6) 0.0016(5) 0.0041(5) -0.0016(5) C7AA 0.0207(7) 0.0172(7) 0.0190(7) 0.0031(6) 0.0047(6) 0.0029(5) C7A 0.0225(7) 0.0224(7) 0.0204(7) -0.0013(6) 0.0021(6) -0.0023(6) C6A 0.0229(8) 0.0235(8) 0.0294(8) 0.0013(6) 0.0054(6) -0.0047(6) C5A 0.0274(8) 0.0222(7) 0.0292(8) 0.0050(6) 0.0121(7) -0.0005(6) C4A 0.0281(8) 0.0217(7) 0.0185(7) 0.0024(6) 0.0075(6) 0.0011(6) C3AA 0.0197(7) 0.0160(7) 0.0171(7) 0.0008(5) 0.0019(5) -0.0001(5) N1A' 0.0355(8) 0.0256(7) 0.0166(6) -0.0006(5) 0.0055(5) -0.0029(6) C2A' 0.0260(8) 0.0205(7) 0.0158(7) 0.0037(6) 0.0060(6) 0.0048(6) C3A' 0.0299(8) 0.0270(8) 0.0238(8) 0.0039(6) 0.0081(7) -0.0004(6) C4A' 0.0357(9) 0.0345(9) 0.0274(9) 0.0099(7) 0.0152(7) 0.0052(7) C5A' 0.0443(10) 0.0333(9) 0.0198(8) 0.0069(7) 0.0133(7) 0.0119(7) C6A' 0.0432(10) 0.0295(9) 0.0175(8) 0.0000(6) 0.0054(7) 0.0008(7) N1B 0.0194(6) 0.0212(6) 0.0144(6) 0.0009(5) 0.0019(5) -0.0034(5) N2B 0.0232(6) 0.0233(6) 0.0141(6) 0.0013(5) 0.0012(5) -0.0053(5) N3B 0.0231(6) 0.0213(6) 0.0160(6) 0.0018(5) 0.0042(5) -0.0027(5) C3BA 0.0181(7) 0.0176(7) 0.0195(7) 0.0014(5) 0.0048(5) 0.0004(5) C4B 0.0245(7) 0.0261(8) 0.0199(7) 0.0034(6) 0.0091(6) 0.0030(6) C5B 0.0248(8) 0.0328(9) 0.0315(9) 0.0072(7) 0.0144(7) 0.0011(6) C6B 0.0195(7) 0.0303(8) 0.0346(9) 0.0026(7) 0.0081(7) -0.0047(6) C7B 0.0196(7) 0.0250(8) 0.0246(8) -0.0009(6) 0.0035(6) -0.0029(6) C7BA 0.0192(7) 0.0186(7) 0.0190(7) 0.0014(6) 0.0051(6) 0.0014(5) N1B' 0.0309(7) 0.0336(8) 0.0169(6) 0.0017(6) 0.0003(5) -0.0036(6) C2B' 0.0252(7) 0.0202(7) 0.0149(7) 0.0031(5) 0.0033(6) 0.0028(6) C3B' 0.0289(8) 0.0302(8) 0.0229(8) 0.0068(7) 0.0079(6) 0.0019(6) C4B' 0.0437(10) 0.0379(10) 0.0274(9) 0.0118(7) 0.0181(8) 0.0077(8) C5B' 0.0571(12) 0.0340(9) 0.0159(8) 0.0065(7) 0.0099(8) 0.0093(8) C6B' 0.0455(11) 0.0357(9) 0.0180(8) 0.0018(7) -0.0017(7) -0.0012(8) _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 N3A 2.0453(13) . ? Cu1 N3B 2.0535(13) . ? Cu1 Cl2 2.2690(7) . ? Cu1 Cl1 2.3107(6) 2_666 ? Cu1 Cl1 2.6739(7) . ? Cl1 Cu1 2.3107(6) 2_666 ? N1A N2A 1.3644(17) . ? N1A C7AA 1.389(2) . ? N1A C2A' 1.4328(19) . ? N2A N3A 1.3057(18) . ? N3A C3AA 1.3924(19) . ? C7AA C3AA 1.402(2) . ? C7AA C7A 1.416(2) . ? C7A C6A 1.384(2) . ? C6A C5A 1.418(2) . ? C5A C4A 1.391(2) . ? C4A C3AA 1.411(2) . ? N1A' C2A' 1.339(2) . ? N1A' C6A' 1.350(2) . ? C2A' C3A' 1.400(2) . ? C3A' C4A' 1.388(2) . ? C4A' C5A' 1.402(3) . ? C5A' C6A' 1.386(3) . ? N1B N2B 1.3662(17) . ? N1B C7BA 1.386(2) . ? N1B C2B' 1.429(2) . ? N2B N3B 1.3025(19) . ? N3B C3BA 1.3949(19) . ? C3BA C7BA 1.400(2) . ? C3BA C4B 1.403(2) . ? C4B C5B 1.388(2) . ? C5B C6B 1.421(2) . ? C6B C7B 1.382(2) . ? C7B C7BA 1.418(2) . ? N1B' C2B' 1.340(2) . ? N1B' C6B' 1.345(2) . ? C2B' C3B' 1.398(2) . ? C3B' C4B' 1.381(2) . ? C4B' C5B' 1.401(3) . ? C5B' C6B' 1.390(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 N3A Cu1 N3B 173.29(5) . . ? N3A Cu1 Cl2 88.85(4) . . ? N3B Cu1 Cl2 91.12(4) . . ? N3A Cu1 Cl1 89.35(4) . 2_666 ? N3B Cu1 Cl1 88.84(4) . 2_666 ? Cl2 Cu1 Cl1 164.059(17) . 2_666 ? N3A Cu1 Cl1 96.82(4) . . ? N3B Cu1 Cl1 89.70(4) . . ? Cl2 Cu1 Cl1 104.133(17) . . ? Cl1 Cu1 Cl1 91.808(16) 2_666 . ? Cu1 Cl1 Cu1 88.192(16) 2_666 . ? N2A N1A C7AA 110.80(12) . . ? N2A N1A C2A' 119.19(12) . . ? C7AA N1A C2A' 129.97(12) . . ? N3A N2A N1A 107.76(12) . . ? N2A N3A C3AA 109.93(12) . . ? N2A N3A Cu1 118.88(10) . . ? C3AA N3A Cu1 131.15(10) . . ? N1A C7AA C3AA 103.78(12) . . ? N1A C7AA C7A 134.27(14) . . ? C3AA C7AA C7A 121.94(14) . . ? C6A C7A C7AA 116.16(14) . . ? C7A C6A C5A 122.22(15) . . ? C4A C5A C6A 121.66(15) . . ? C5A C4A C3AA 116.62(14) . . ? N3A C3AA C7AA 107.72(13) . . ? N3A C3AA C4A 130.92(14) . . ? C7AA C3AA C4A 121.36(14) . . ? C2A' N1A' C6A' 115.96(15) . . ? N1A' C2A' C3A' 125.34(15) . . ? N1A' C2A' N1A 114.34(14) . . ? C3A' C2A' N1A 120.32(13) . . ? C4A' C3A' C2A' 117.03(15) . . ? C3A' C4A' C5A' 119.32(16) . . ? C6A' C5A' C4A' 118.39(16) . . ? N1A' C6A' C5A' 123.96(16) . . ? N2B N1B C7BA 110.92(12) . . ? N2B N1B C2B' 118.64(12) . . ? C7BA N1B C2B' 130.29(12) . . ? N3B N2B N1B 107.75(12) . . ? N2B N3B C3BA 109.79(12) . . ? N2B N3B Cu1 119.52(10) . . ? C3BA N3B Cu1 130.69(10) . . ? N3B C3BA C7BA 107.83(13) . . ? N3B C3BA C4B 130.95(14) . . ? C7BA C3BA C4B 121.22(14) . . ? C5B C4B C3BA 117.16(14) . . ? C4B C5B C6B 121.36(15) . . ? C7B C6B C5B 122.17(15) . . ? C6B C7B C7BA 116.08(14) . . ? N1B C7BA C3BA 103.69(12) . . ? N1B C7BA C7B 134.29(14) . . ? C3BA C7BA C7B 122.02(14) . . ? C2B' N1B' C6B' 116.02(16) . . ? N1B' C2B' C3B' 125.52(15) . . ? N1B' C2B' N1B 114.28(14) . . ? C3B' C2B' N1B 120.18(13) . . ? C4B' C3B' C2B' 117.15(16) . . ? C3B' C4B' C5B' 119.03(17) . . ? C6B' C5B' C4B' 118.88(16) . . ? N1B' C6B' C5B' 123.39(16) . . ? 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 N3A Cu1 Cl1 Cu1 89.56(4) . . . 2_666 ? N3B Cu1 Cl1 Cu1 -88.83(4) . . . 2_666 ? Cl2 Cu1 Cl1 Cu1 -179.906(14) . . . 2_666 ? Cl1 Cu1 Cl1 Cu1 0.0 2_666 . . 2_666 ? C7AA N1A N2A N3A -0.34(16) . . . . ? C2A' N1A N2A N3A 177.56(12) . . . . ? N1A N2A N3A C3AA -0.64(16) . . . . ? N1A N2A N3A Cu1 -178.56(9) . . . . ? N3B Cu1 N3A N2A 17.3(5) . . . . ? Cl2 Cu1 N3A N2A 107.09(11) . . . . ? Cl1 Cu1 N3A N2A -57.07(11) 2_666 . . . ? Cl1 Cu1 N3A N2A -148.81(10) . . . . ? N3B Cu1 N3A C3AA -160.1(4) . . . . ? Cl2 Cu1 N3A C3AA -70.32(13) . . . . ? Cl1 Cu1 N3A C3AA 125.52(13) 2_666 . . . ? Cl1 Cu1 N3A C3AA 33.78(13) . . . . ? N2A N1A C7AA C3AA 1.13(16) . . . . ? C2A' N1A C7AA C3AA -176.47(14) . . . . ? N2A N1A C7AA C7A -179.11(16) . . . . ? C2A' N1A C7AA C7A 3.3(3) . . . . ? N1A C7AA C7A C6A -178.43(16) . . . . ? C3AA C7AA C7A C6A 1.3(2) . . . . ? C7AA C7A C6A C5A 0.5(2) . . . . ? C7A C6A C5A C4A -1.4(3) . . . . ? C6A C5A C4A C3AA 0.5(2) . . . . ? N2A N3A C3AA C7AA 1.36(16) . . . . ? Cu1 N3A C3AA C7AA 178.95(10) . . . . ? N2A N3A C3AA C4A -177.51(15) . . . . ? Cu1 N3A C3AA C4A 0.1(2) . . . . ? N1A C7AA C3AA N3A -1.47(15) . . . . ? C7A C7AA C3AA N3A 178.74(13) . . . . ? N1A C7AA C3AA C4A 177.53(13) . . . . ? C7A C7AA C3AA C4A -2.3(2) . . . . ? C5A C4A C3AA N3A -179.96(15) . . . . ? C5A C4A C3AA C7AA 1.3(2) . . . . ? C6A' N1A' C2A' C3A' 0.4(2) . . . . ? C6A' N1A' C2A' N1A -179.81(14) . . . . ? N2A N1A C2A' N1A' -175.78(13) . . . . ? C7AA N1A C2A' N1A' 1.7(2) . . . . ? N2A N1A C2A' C3A' 4.1(2) . . . . ? C7AA N1A C2A' C3A' -178.50(14) . . . . ? N1A' C2A' C3A' C4A' -0.4(2) . . . . ? N1A C2A' C3A' C4A' 179.80(14) . . . . ? C2A' C3A' C4A' C5A' 0.3(2) . . . . ? C3A' C4A' C5A' C6A' -0.2(3) . . . . ? C2A' N1A' C6A' C5A' -0.2(3) . . . . ? C4A' C5A' C6A' N1A' 0.1(3) . . . . ? C7BA N1B N2B N3B 0.97(16) . . . . ? C2B' N1B N2B N3B -175.10(12) . . . . ? N1B N2B N3B C3BA -0.13(16) . . . . ? N1B N2B N3B Cu1 -179.61(9) . . . . ? N3A Cu1 N3B N2B 158.5(4) . . . . ? Cl2 Cu1 N3B N2B 68.84(11) . . . . ? Cl1 Cu1 N3B N2B -127.10(11) 2_666 . . . ? Cl1 Cu1 N3B N2B -35.29(11) . . . . ? N3A Cu1 N3B C3BA -20.9(5) . . . . ? Cl2 Cu1 N3B C3BA -110.52(13) . . . . ? Cl1 Cu1 N3B C3BA 53.54(13) 2_666 . . . ? Cl1 Cu1 N3B C3BA 145.35(13) . . . . ? N2B N3B C3BA C7BA -0.72(17) . . . . ? Cu1 N3B C3BA C7BA 178.68(10) . . . . ? N2B N3B C3BA C4B 178.88(15) . . . . ? Cu1 N3B C3BA C4B -1.7(2) . . . . ? N3B C3BA C4B C5B 179.96(15) . . . . ? C7BA C3BA C4B C5B -0.5(2) . . . . ? C3BA C4B C5B C6B -0.4(2) . . . . ? C4B C5B C6B C7B 0.6(3) . . . . ? C5B C6B C7B C7BA 0.0(2) . . . . ? N2B N1B C7BA C3BA -1.36(16) . . . . ? C2B' N1B C7BA C3BA 174.12(14) . . . . ? N2B N1B C7BA C7B 179.21(16) . . . . ? C2B' N1B C7BA C7B -5.3(3) . . . . ? N3B C3BA C7BA N1B 1.23(16) . . . . ? C4B C3BA C7BA N1B -178.42(13) . . . . ? N3B C3BA C7BA C7B -179.25(13) . . . . ? C4B C3BA C7BA C7B 1.1(2) . . . . ? C6B C7B C7BA N1B 178.53(16) . . . . ? C6B C7B C7BA C3BA -0.8(2) . . . . ? C6B' N1B' C2B' C3B' 0.8(2) . . . . ? C6B' N1B' C2B' N1B -177.79(14) . . . . ? N2B N1B C2B' N1B' -171.19(13) . . . . ? C7BA N1B C2B' N1B' 13.6(2) . . . . ? N2B N1B C2B' C3B' 10.2(2) . . . . ? C7BA N1B C2B' C3B' -165.03(15) . . . . ? N1B' C2B' C3B' C4B' -0.3(3) . . . . ? N1B C2B' C3B' C4B' 178.24(15) . . . . ? C2B' C3B' C4B' C5B' -0.9(2) . . . . ? C3B' C4B' C5B' C6B' 1.4(3) . . . . ? C2B' N1B' C6B' C5B' -0.2(3) . . . . ? C4B' C5B' C6B' N1B' -0.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.244 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.061 #===END data_3cr40(complex18) _database_code_CSD 190042 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H20 Cl4 Cu2 N8' _chemical_formula_weight 689.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 8.390(2) _cell_length_b 21.467(6) _cell_length_c 8.328(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.217(8) _cell_angle_gamma 90.00 _cell_volume 1309.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 2.065 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.3963 _exptl_absorpt_correction_T_max 0.8047 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'Siemens SMART CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16369 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 26.44 _reflns_number_total 2663 _reflns_number_gt 2483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1999)' _computing_data_reduction 'SAINT (Siemens, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material Xcif _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^)+(0.0264P)^2^+1.3515P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2663 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.47269(3) 0.603771(10) 0.93756(3) 0.01751(8) Uani 1 1 d . . . Cl1 Cl 0.36446(6) 0.62705(2) 1.13425(7) 0.02484(11) Uani 1 1 d . . . Cl2 Cl 0.44193(7) 0.62787(2) 0.66074(7) 0.02676(12) Uani 1 1 d . . . N1 N 0.8676(2) 0.53785(7) 1.1214(2) 0.0164(3) Uani 1 1 d . . . N2 N 0.6997(2) 0.51530(7) 1.0683(2) 0.0183(3) Uani 1 1 d . . . N3 N 0.7179(2) 0.46410(7) 1.1623(2) 0.0182(3) Uani 1 1 d . . . C3A C 0.9006(2) 0.45303(8) 1.2792(2) 0.0169(4) Uani 1 1 d . . . C4 C 0.9920(3) 0.40408(9) 1.4026(3) 0.0212(4) Uani 1 1 d . . . H4 H 0.9279 0.3707 1.4202 0.025 Uiso 1 1 calc R . . C5 C 1.1801(3) 0.40741(9) 1.4965(3) 0.0236(4) Uani 1 1 d . . . H5 H 1.2472 0.3750 1.5800 0.028 Uiso 1 1 calc R . . C6 C 1.2767(3) 0.45734(10) 1.4730(3) 0.0238(4) Uani 1 1 d . . . H6 H 1.4062 0.4578 1.5436 0.029 Uiso 1 1 calc R . . C7 C 1.1900(3) 0.50516(9) 1.3517(3) 0.0204(4) Uani 1 1 d . . . H7 H 1.2549 0.5385 1.3350 0.024 Uiso 1 1 calc R . . C7A C 0.9987(2) 0.50126(8) 1.2542(2) 0.0160(3) Uani 1 1 d . . . C10 C 0.8901(3) 0.59322(8) 1.0321(3) 0.0179(4) Uani 1 1 d . . . H10A H 0.8038 0.5909 0.8983 0.021 Uiso 1 1 calc R . . H10B H 1.0155 0.5937 1.0494 0.021 Uiso 1 1 calc R . . N1' N 0.6833(2) 0.66527(7) 1.0664(2) 0.0166(3) Uani 1 1 d . . . C2' C 0.8572(2) 0.65296(8) 1.1072(2) 0.0163(3) Uani 1 1 d . . . C3' C 1.0002(3) 0.69392(9) 1.2070(3) 0.0218(4) Uani 1 1 d . . . H3' H 1.1217 0.6831 1.2380 0.026 Uiso 1 1 calc R . . C4' C 0.9632(3) 0.75097(10) 1.2611(3) 0.0268(4) Uani 1 1 d . . . H4' H 1.0588 0.7795 1.3312 0.032 Uiso 1 1 calc R . . C5' C 0.7838(3) 0.76516(9) 1.2102(3) 0.0259(4) Uani 1 1 d . . . H5' H 0.7535 0.8046 1.2394 0.031 Uiso 1 1 calc R . . C6' C 0.6489(3) 0.72120(9) 1.1163(3) 0.0214(4) Uani 1 1 d . . . H6' H 0.5268 0.7309 1.0858 0.026 Uiso 1 1 calc R . . 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 0.01441(12) 0.01867(13) 0.01915(13) -0.00130(9) 0.00797(10) -0.00428(8) Cl1 0.0204(2) 0.0319(3) 0.0264(2) -0.00206(19) 0.0147(2) -0.00268(18) Cl2 0.0259(2) 0.0335(3) 0.0209(2) -0.00125(19) 0.0114(2) -0.00983(19) N1 0.0134(7) 0.0134(7) 0.0222(8) 0.0001(6) 0.0085(6) -0.0004(6) N2 0.0139(7) 0.0171(7) 0.0227(8) 0.0005(6) 0.0081(6) -0.0011(6) N3 0.0148(7) 0.0166(7) 0.0205(8) 0.0016(6) 0.0065(6) -0.0005(6) C3A 0.0137(8) 0.0179(9) 0.0184(9) -0.0030(7) 0.0073(7) -0.0010(7) C4 0.0214(9) 0.0194(9) 0.0215(9) 0.0021(7) 0.0096(8) 0.0009(7) C5 0.0225(10) 0.0246(10) 0.0198(9) 0.0030(8) 0.0071(8) 0.0063(8) C6 0.0133(9) 0.0317(11) 0.0226(10) -0.0030(8) 0.0058(8) 0.0018(7) C7 0.0154(9) 0.0217(9) 0.0233(9) -0.0036(8) 0.0089(8) -0.0025(7) C7A 0.0152(8) 0.0152(8) 0.0171(9) -0.0023(7) 0.0075(7) 0.0011(6) C10 0.0192(9) 0.0137(8) 0.0239(9) 0.0009(7) 0.0130(8) -0.0003(7) N1' 0.0167(7) 0.0152(7) 0.0181(7) 0.0004(6) 0.0086(6) -0.0007(6) C2' 0.0186(9) 0.0141(8) 0.0178(8) 0.0022(7) 0.0102(7) 0.0007(7) C3' 0.0169(9) 0.0220(9) 0.0254(10) -0.0017(8) 0.0095(8) -0.0023(7) C4' 0.0244(10) 0.0234(10) 0.0306(11) -0.0079(8) 0.0118(9) -0.0079(8) C5' 0.0293(10) 0.0178(9) 0.0324(11) -0.0058(8) 0.0165(9) -0.0005(8) C6' 0.0201(9) 0.0195(9) 0.0258(10) 0.0003(7) 0.0121(8) 0.0026(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.0181(16) 3_667 ? Cu1 N1' 2.0408(16) . ? Cu1 Cl2 2.2511(8) . ? Cu1 Cl1 2.2823(7) . ? N1 N2 1.344(2) . ? N1 C7A 1.365(2) . ? N1 C10 1.462(2) . ? N2 N3 1.314(2) . ? N3 C3A 1.377(2) . ? N3 Cu1 2.0181(16) 3_667 ? C3A C7A 1.400(3) . ? C3A C4 1.407(3) . ? C4 C5 1.379(3) . ? C5 C6 1.414(3) . ? C6 C7 1.373(3) . ? C7 C7A 1.404(3) . ? C10 C2' 1.510(2) . ? N1' C6' 1.347(2) . ? N1' C2' 1.353(2) . ? C2' C3' 1.390(3) . ? C3' C4' 1.391(3) . ? C4' C5' 1.384(3) . ? C5' C6' 1.386(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 N3 Cu1 N1' 172.80(6) 3_667 . ? N3 Cu1 Cl2 94.14(5) 3_667 . ? N1' Cu1 Cl2 91.53(5) . . ? N3 Cu1 Cl1 86.63(5) 3_667 . ? N1' Cu1 Cl1 91.53(5) . . ? Cl2 Cu1 Cl1 142.91(2) . . ? N2 N1 C7A 111.09(15) . . ? N2 N1 C10 120.03(15) . . ? C7A N1 C10 128.82(15) . . ? N3 N2 N1 107.90(14) . . ? N2 N3 C3A 109.30(15) . . ? N2 N3 Cu1 121.34(12) . 3_667 ? C3A N3 Cu1 123.45(12) . 3_667 ? N3 C3A C7A 107.43(16) . . ? N3 C3A C4 131.82(17) . . ? C7A C3A C4 120.71(17) . . ? C5 C4 C3A 116.13(18) . . ? C4 C5 C6 122.36(18) . . ? C7 C6 C5 122.33(18) . . ? C6 C7 C7A 115.25(18) . . ? N1 C7A C3A 104.27(16) . . ? N1 C7A C7 132.53(17) . . ? C3A C7A C7 123.19(17) . . ? N1 C10 C2' 112.63(15) . . ? C6' N1' C2' 117.64(16) . . ? C6' N1' Cu1 118.55(13) . . ? C2' N1' Cu1 123.81(12) . . ? N1' C2' C3' 122.48(17) . . ? N1' C2' C10 117.05(16) . . ? C3' C2' C10 120.41(17) . . ? C2' C3' C4' 119.14(18) . . ? C5' C4' C3' 118.42(18) . . ? C4' C5' C6' 119.32(18) . . ? N1' C6' C5' 122.84(18) . . ? 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 C7A N1 N2 N3 -0.7(2) . . . . ? C10 N1 N2 N3 176.75(15) . . . . ? N1 N2 N3 C3A 0.2(2) . . . . ? N1 N2 N3 Cu1 -153.62(12) . . . 3_667 ? N2 N3 C3A C7A 0.4(2) . . . . ? Cu1 N3 C3A C7A 153.54(12) 3_667 . . . ? N2 N3 C3A C4 -177.52(19) . . . . ? Cu1 N3 C3A C4 -24.4(3) 3_667 . . . ? N3 C3A C4 C5 178.55(19) . . . . ? C7A C3A C4 C5 0.8(3) . . . . ? C3A C4 C5 C6 0.8(3) . . . . ? C4 C5 C6 C7 -1.6(3) . . . . ? C5 C6 C7 C7A 0.6(3) . . . . ? N2 N1 C7A C3A 1.0(2) . . . . ? C10 N1 C7A C3A -176.23(17) . . . . ? N2 N1 C7A C7 -179.91(19) . . . . ? C10 N1 C7A C7 2.9(3) . . . . ? N3 C3A C7A N1 -0.82(19) . . . . ? C4 C3A C7A N1 177.41(16) . . . . ? N3 C3A C7A C7 179.94(16) . . . . ? C4 C3A C7A C7 -1.8(3) . . . . ? C6 C7 C7A N1 -177.94(19) . . . . ? C6 C7 C7A C3A 1.1(3) . . . . ? N2 N1 C10 C2' 81.0(2) . . . . ? C7A N1 C10 C2' -102.0(2) . . . . ? N3 Cu1 N1' C6' -117.3(5) 3_667 . . . ? Cl2 Cu1 N1' C6' 100.74(14) . . . . ? Cl1 Cu1 N1' C6' -42.29(14) . . . . ? N3 Cu1 N1' C2' 61.8(5) 3_667 . . . ? Cl2 Cu1 N1' C2' -80.13(14) . . . . ? Cl1 Cu1 N1' C2' 136.84(14) . . . . ? C6' N1' C2' C3' 4.1(3) . . . . ? Cu1 N1' C2' C3' -175.09(14) . . . . ? C6' N1' C2' C10 -173.38(16) . . . . ? Cu1 N1' C2' C10 7.5(2) . . . . ? N1 C10 C2' N1' -70.1(2) . . . . ? N1 C10 C2' C3' 112.41(19) . . . . ? N1' C2' C3' C4' -2.8(3) . . . . ? C10 C2' C3' C4' 174.58(18) . . . . ? C2' C3' C4' C5' -1.0(3) . . . . ? C3' C4' C5' C6' 3.4(3) . . . . ? C2' N1' C6' C5' -1.6(3) . . . . ? Cu1 N1' C6' C5' 177.59(15) . . . . ? C4' C5' C6' N1' -2.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.334 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.059 #===END data_3crq7(complex19) _database_code_CSD 190043 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62.50 H47.50 Cl6 Cu4 N18.50 O6' _chemical_formula_weight 1620.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.585(19) _cell_length_b 13.589(6) _cell_length_c 24.550(11) _cell_angle_alpha 90.00 _cell_angle_beta 109.214(7) _cell_angle_gamma 90.00 _cell_volume 13415(10) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6544 _exptl_absorpt_coefficient_mu 1.556 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6698 _exptl_absorpt_correction_T_max 0.9404 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 60290 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8759 _reflns_number_gt 5735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8759 _refine_ls_number_parameters 884 _refine_ls_number_restraints 395 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.009 _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 0.164321(19) 0.24244(5) 0.17873(3) 0.0226(2) Uani 1 1 d . . . Cu2 Cu 0.131761(19) 0.15452(6) 0.26560(3) 0.0228(2) Uani 1 1 d . . . Cu3 Cu 0.123458(19) 0.04847(5) 0.14872(3) 0.0231(2) Uani 1 1 d . . . Cu4 Cu 0.087647(19) 0.24769(6) 0.14988(3) 0.0261(2) Uani 1 1 d . . . Cl1 Cl 0.11976(5) -0.01846(12) 0.23498(7) 0.0389(5) Uani 1 1 d . . . Cl2 Cl 0.12713(4) 0.38085(12) 0.15263(8) 0.0360(5) Uani 1 1 d . . . Cl3 Cl 0.16926(4) 0.11029(12) 0.11985(7) 0.0306(4) Uani 1 1 d . . . Cl4 Cl 0.07330(4) 0.11927(13) 0.08038(7) 0.0356(5) Uani 1 1 d . . . Cl5 Cl 0.07836(4) 0.22969(13) 0.24242(7) 0.0334(4) Uani 1 1 d . . . Cl6 Cl 0.18520(4) 0.22325(12) 0.28377(7) 0.0280(4) Uani 1 1 d . . . O1 O 0.12680(9) 0.1735(3) 0.18620(16) 0.0200(10) Uani 1 1 d . . . N11 N 0.11245(12) -0.1909(3) 0.04654(18) 0.0256(13) Uani 1 1 d D . . N21 N 0.10549(13) -0.0983(3) 0.0598(2) 0.0264(13) Uani 1 1 d D . . N31 N 0.12388(12) -0.0811(3) 0.1130(2) 0.0231(13) Uani 1 1 d D . . C3A1 C 0.14353(14) -0.1625(4) 0.1362(2) 0.0236(16) Uani 1 1 d D . . C41 C 0.16724(16) -0.1779(5) 0.1905(2) 0.0347(18) Uani 1 1 d D . . H41 H 0.1724 -0.1287 0.2197 0.042 Uiso 1 1 calc R . . C51 C 0.18272(18) -0.2681(5) 0.1995(3) 0.042(2) Uani 1 1 d D . . H51 H 0.1991 -0.2817 0.2357 0.050 Uiso 1 1 calc R . . C61 C 0.17485(17) -0.3405(5) 0.1566(3) 0.040(2) Uani 1 1 d D . . H61 H 0.1856 -0.4026 0.1652 0.048 Uiso 1 1 calc R . . C71 C 0.15241(16) -0.3255(4) 0.1028(3) 0.0354(19) Uani 1 1 d D . . H71 H 0.1476 -0.3750 0.0738 0.043 Uiso 1 1 calc R . . C7A1 C 0.13677(15) -0.2330(4) 0.0926(2) 0.0279(17) Uani 1 1 d D . . C1'1 C 0.09819(14) -0.2283(4) -0.0117(2) 0.0266(16) Uani 1 1 d D . . N2'1 N 0.11816(14) -0.2906(4) -0.0241(2) 0.0392(15) Uani 1 1 d D . . C3'1 C 0.10742(19) -0.3335(6) -0.0774(3) 0.053(2) Uani 1 1 d D . . H3'1 H 0.1211 -0.3818 -0.0865 0.063 Uiso 1 1 calc R . . C4'1 C 0.07778(19) -0.3096(5) -0.1181(3) 0.050(2) Uani 1 1 d D . . H4'1 H 0.0717 -0.3385 -0.1554 0.060 Uiso 1 1 calc R . . C4A1 C 0.05632(16) -0.2429(5) -0.1050(3) 0.0387(19) Uani 1 1 d D . . C5'1 C 0.02515(18) -0.2172(6) -0.1444(3) 0.053(2) Uani 1 1 d D . . H5'1 H 0.0186 -0.2443 -0.1821 0.064 Uiso 1 1 calc R . . C6'1 C 0.00382(18) -0.1539(6) -0.1301(3) 0.055(2) Uani 1 1 d D . . H6'1 H -0.0170 -0.1375 -0.1578 0.066 Uiso 1 1 calc R . . C7'1 C 0.01297(16) -0.1142(6) -0.0747(3) 0.047(2) Uani 1 1 d D . . H7'1 H -0.0020 -0.0723 -0.0643 0.056 Uiso 1 1 calc R . . C8'1 C 0.04370(15) -0.1355(5) -0.0348(3) 0.0365(19) Uani 1 1 d D . . H8'1 H 0.0497 -0.1067 0.0025 0.044 Uiso 1 1 calc R . . C8A1 C 0.06658(14) -0.1994(5) -0.0482(2) 0.0324(18) Uani 1 1 d D . . N12 N 0.00325(12) 0.3741(4) 0.0469(2) 0.0380(16) Uani 1 1 d D . . N22 N 0.03012(13) 0.3136(4) 0.0603(2) 0.0362(15) Uani 1 1 d D . . N32 N 0.04826(12) 0.3304(4) 0.1137(2) 0.0307(14) Uani 1 1 d D . . C3A2 C 0.03398(16) 0.4043(5) 0.1365(3) 0.0349(18) Uani 1 1 d D . . C42 C 0.04503(19) 0.4483(5) 0.1909(3) 0.051(2) Uani 1 1 d D . . H42 H 0.0653 0.4296 0.2194 0.061 Uiso 1 1 calc R . . C52 C 0.0249(2) 0.5200(6) 0.2006(4) 0.075(3) Uani 1 1 d D . . H52 H 0.0309 0.5501 0.2375 0.090 Uiso 1 1 calc R . . C62 C -0.0044(2) 0.5504(7) 0.1576(4) 0.080(3) Uani 1 1 d D . . H62 H -0.0169 0.6029 0.1657 0.097 Uiso 1 1 calc R . . C72 C -0.01537(19) 0.5068(6) 0.1047(4) 0.065(3) Uani 1 1 d D . . H72 H -0.0358 0.5256 0.0765 0.078 Uiso 1 1 calc R . . C7A2 C 0.00486(16) 0.4329(5) 0.0939(3) 0.040(2) Uani 1 1 d D . . C1'2 C -0.02207(16) 0.3703(5) -0.0094(3) 0.044(2) Uani 1 1 d D . . N2'2 N -0.04382(15) 0.4404(4) -0.0151(3) 0.0552(19) Uani 1 1 d D . . C3'2 C -0.07044(19) 0.4435(6) -0.0648(4) 0.066(3) Uani 1 1 d D . . H3'2 H -0.0859 0.4959 -0.0700 0.079 Uiso 1 1 calc R . . C4'2 C -0.07563(19) 0.3748(6) -0.1068(4) 0.067(3) Uani 1 1 d D . . H4'2 H -0.0948 0.3785 -0.1401 0.080 Uiso 1 1 calc R . . C4A2 C -0.05283(17) 0.2986(6) -0.1012(3) 0.055(2) Uani 1 1 d D . . C5'2 C -0.0580(2) 0.2230(7) -0.1421(3) 0.078(3) Uani 1 1 d D . . H5'2 H -0.0779 0.2232 -0.1745 0.093 Uiso 1 1 calc R . . C6'2 C -0.0352(2) 0.1482(7) -0.1368(3) 0.082(3) Uani 1 1 d D . . H6'2 H -0.0394 0.0971 -0.1647 0.098 Uiso 1 1 calc R . . C7'2 C -0.00591(19) 0.1489(6) -0.0899(3) 0.064(3) Uani 1 1 d D . . H7'2 H 0.0103 0.0993 -0.0869 0.077 Uiso 1 1 calc R . . C8'2 C 0.00013(18) 0.2203(5) -0.0474(3) 0.052(2) Uani 1 1 d D . . H8'2 H 0.0203 0.2184 -0.0157 0.063 Uiso 1 1 calc R . . C8A2 C -0.02348(16) 0.2966(5) -0.0506(3) 0.045(2) Uani 1 1 d D . . N13 N 0.16698(11) 0.0993(4) 0.43658(18) 0.0218(13) Uani 1 1 d D . . N23 N 0.16678(12) 0.1439(4) 0.38704(19) 0.0255(13) Uani 1 1 d D . . N33 N 0.13838(12) 0.1247(4) 0.34755(19) 0.0236(13) Uani 1 1 d D . . C3A3 C 0.11881(13) 0.0672(4) 0.3708(2) 0.0235(16) Uani 1 1 d D . . C43 C 0.08687(14) 0.0282(5) 0.3457(3) 0.0302(17) Uani 1 1 d D . . H43 H 0.0742 0.0395 0.3063 0.036 Uiso 1 1 calc R . . C53 C 0.07486(15) -0.0275(5) 0.3814(3) 0.0339(18) Uani 1 1 d D . . H53 H 0.0531 -0.0545 0.3665 0.041 Uiso 1 1 calc R . . C63 C 0.09383(15) -0.0454(5) 0.4392(3) 0.0345(18) Uani 1 1 d D . . H63 H 0.0846 -0.0856 0.4617 0.041 Uiso 1 1 calc R . . C73 C 0.12511(15) -0.0075(4) 0.4646(2) 0.0246(16) Uani 1 1 d D . . H73 H 0.1377 -0.0196 0.5039 0.030 Uiso 1 1 calc R . . C7A3 C 0.13727(13) 0.0504(4) 0.4285(2) 0.0213(15) Uani 1 1 d D . . C1'3 C 0.19573(13) 0.1084(5) 0.4886(2) 0.0249(16) Uani 1 1 d D . . N2'3 N 0.18735(12) 0.1054(4) 0.5353(2) 0.0271(13) Uani 1 1 d D . . C3'3 C 0.21285(16) 0.1152(5) 0.5868(2) 0.0325(18) Uani 1 1 d D . . H3'3 H 0.2077 0.1118 0.6216 0.039 Uiso 1 1 calc R . . C4'3 C 0.24516(16) 0.1294(5) 0.5906(3) 0.0313(18) Uani 1 1 d D . . H4'3 H 0.2617 0.1380 0.6273 0.038 Uiso 1 1 calc R . . C4A3 C 0.25405(14) 0.1313(4) 0.5404(2) 0.0270(17) Uani 1 1 d D . . C5'3 C 0.28716(15) 0.1439(5) 0.5420(3) 0.0356(19) Uani 1 1 d D . . H5'3 H 0.3042 0.1540 0.5780 0.043 Uiso 1 1 calc R . . C6'3 C 0.29532(16) 0.1419(5) 0.4920(3) 0.0340(18) Uani 1 1 d D . . H6'3 H 0.3177 0.1514 0.4937 0.041 Uiso 1 1 calc R . . C7'3 C 0.27067(16) 0.1259(5) 0.4391(3) 0.0327(18) Uani 1 1 d D . . H7'3 H 0.2766 0.1227 0.4051 0.039 Uiso 1 1 calc R . . C8'3 C 0.23797(15) 0.1148(4) 0.4351(3) 0.0291(17) Uani 1 1 d D . . H8'3 H 0.2216 0.1047 0.3983 0.035 Uiso 1 1 calc R . . C8A3 C 0.22812(13) 0.1181(4) 0.4857(2) 0.0247(16) Uani 1 1 d D . . N14 N 0.24470(13) 0.3644(4) 0.1500(3) 0.0444(18) Uani 1 1 d D . . N24 N 0.21954(14) 0.2985(4) 0.1393(2) 0.0388(16) Uani 1 1 d D . . N34 N 0.20327(12) 0.3184(4) 0.1746(2) 0.0263(13) Uani 1 1 d D . . C3A4 C 0.21796(14) 0.3981(4) 0.2092(2) 0.0267(17) Uani 1 1 d D . . C44 C 0.20974(17) 0.4469(4) 0.2527(3) 0.0364(19) Uani 1 1 d D . . H44 H 0.1915 0.4271 0.2644 0.044 Uiso 1 1 calc R . . C54 C 0.22957(19) 0.5254(5) 0.2775(3) 0.049(2) Uani 1 1 d D . . H54 H 0.2247 0.5610 0.3071 0.059 Uiso 1 1 calc R . . C64 C 0.25654(19) 0.5553(5) 0.2611(3) 0.051(2) Uani 1 1 d D . . H64 H 0.2693 0.6103 0.2799 0.061 Uiso 1 1 calc R . . C74 C 0.26522(17) 0.5082(5) 0.2190(3) 0.051(2) Uani 1 1 d D . . H74 H 0.2838 0.5275 0.2082 0.061 Uiso 1 1 calc R . . C7A4 C 0.24456(15) 0.4287(4) 0.1928(3) 0.0337(18) Uani 1 1 d D . . C1'4 C 0.27182(18) 0.3550(6) 0.1261(3) 0.060(3) Uani 1 1 d D . . N2'4 N 0.30101(17) 0.3438(6) 0.1644(3) 0.079(2) Uani 1 1 d D . . C3'4 C 0.3276(2) 0.3371(8) 0.1444(4) 0.093(4) Uani 1 1 d D . . H3'4 H 0.3493 0.3279 0.1712 0.112 Uiso 1 1 calc R . . C4'4 C 0.3233(2) 0.3434(7) 0.0869(4) 0.084(4) Uani 1 1 d D . . H4'4 H 0.3422 0.3378 0.0746 0.100 Uiso 1 1 calc R . . C4A4 C 0.2924(2) 0.3577(6) 0.0461(4) 0.065(3) Uani 1 1 d D . . C5'4 C 0.2858(3) 0.3643(7) -0.0128(5) 0.107(5) Uani 1 1 d D . . H5'4 H 0.3038 0.3577 -0.0273 0.129 Uiso 1 1 calc R . . C6'4 C 0.2538(3) 0.3801(7) -0.0523(4) 0.096(5) Uani 1 1 d D . . H6'4 H 0.2505 0.3853 -0.0924 0.115 Uiso 1 1 calc R . . C7'4 C 0.2271(3) 0.3882(6) -0.0319(4) 0.134(6) Uani 1 1 d D . . H7'4 H 0.2054 0.3994 -0.0582 0.161 Uiso 1 1 calc R . . C8'4 C 0.2319(2) 0.3800(5) 0.0263(3) 0.055(3) Uani 1 1 d D . . H8'4 H 0.2133 0.3849 0.0393 0.066 Uiso 1 1 calc R . . C8A4 C 0.2641(2) 0.3643(5) 0.0674(3) 0.065(3) Uani 1 1 d D . . N91 N 0.0186(6) -0.1718(14) 0.2602(9) 0.25(3) Uani 0.50 1 d PD . . C91 C 0.0525(7) -0.2108(19) 0.2833(12) 0.150(11) Uani 0.50 1 d PDU . . H91A H 0.0555 -0.2634 0.2581 0.225 Uiso 0.50 1 calc PR . . H91B H 0.0563 -0.2371 0.3221 0.225 Uiso 0.50 1 calc PR . . H91C H 0.0685 -0.1579 0.2851 0.225 Uiso 0.50 1 calc PR . . O91 O 0.0000 -0.2420(15) 0.2500 0.208(9) Uani 1 2 d SDU . . O92 O 0.0000 -0.101(2) 0.2500 0.283(14) Uani 1 2 d SDU . . N92 N 0.1352(6) -0.5283(12) -0.1819(7) 0.389(17) Uani 1 1 d DU . . C92 C 0.1272(5) -0.6030(12) -0.2278(7) 0.189(7) Uani 1 1 d DU . . H92A H 0.1478 -0.6343 -0.2287 0.284 Uiso 1 1 calc R . . H92B H 0.1160 -0.5716 -0.2651 0.284 Uiso 1 1 calc R . . H92C H 0.1126 -0.6530 -0.2202 0.284 Uiso 1 1 calc R . . O93 O 0.1642(5) -0.5414(17) -0.1695(9) 0.349(11) Uani 1 1 d DU . . O94 O 0.1077(6) -0.5022(19) -0.1862(10) 0.470(15) Uani 1 1 d DU . . N93 N 0.1153(4) -0.6314(15) -0.0305(10) 1.04(8) Uani 1 1 d DU . . C93 C 0.0945(7) -0.683(2) -0.0827(12) 0.426(19) Uani 1 1 d DU . . H93A H 0.0945 -0.6459 -0.1170 0.639 Uiso 1 1 calc R . . H93B H 0.0716 -0.6880 -0.0820 0.639 Uiso 1 1 calc R . . H93C H 0.1034 -0.7490 -0.0840 0.639 Uiso 1 1 calc R . . O95 O 0.1128(5) -0.6919(15) 0.0038(8) 0.318(9) Uani 1 1 d DU . . O96 O 0.1329(4) -0.5707(13) 0.0014(7) 0.298(8) Uani 1 1 d DU . . 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 0.0253(5) 0.0208(5) 0.0239(4) 0.0001(4) 0.0110(4) -0.0030(4) Cu2 0.0263(5) 0.0249(5) 0.0181(4) 0.0019(4) 0.0084(4) -0.0009(4) Cu3 0.0297(5) 0.0192(5) 0.0216(5) -0.0019(4) 0.0099(4) -0.0013(4) Cu4 0.0258(5) 0.0266(5) 0.0251(5) 0.0021(4) 0.0073(4) 0.0051(4) Cl1 0.0718(14) 0.0229(10) 0.0300(10) -0.0001(8) 0.0277(10) -0.0031(9) Cl2 0.0297(10) 0.0233(10) 0.0515(12) 0.0097(8) 0.0085(9) 0.0039(8) Cl3 0.0336(10) 0.0303(10) 0.0340(10) -0.0103(8) 0.0195(8) -0.0058(8) Cl4 0.0304(10) 0.0376(11) 0.0306(10) -0.0088(8) -0.0013(8) 0.0060(8) Cl5 0.0299(10) 0.0478(12) 0.0254(9) 0.0036(8) 0.0132(8) 0.0095(9) Cl6 0.0274(10) 0.0350(10) 0.0207(9) 0.0052(7) 0.0066(8) -0.0048(8) O1 0.019(2) 0.020(2) 0.020(2) 0.0000(19) 0.0062(19) -0.0038(19) N11 0.030(3) 0.022(3) 0.025(3) -0.006(3) 0.009(3) -0.005(3) N21 0.034(4) 0.022(3) 0.020(3) -0.002(3) 0.005(3) 0.000(3) N31 0.028(3) 0.020(3) 0.024(3) -0.001(3) 0.014(3) 0.001(3) C3A1 0.031(4) 0.021(4) 0.021(4) -0.005(3) 0.010(3) -0.001(3) C41 0.040(5) 0.037(5) 0.025(4) -0.007(3) 0.008(4) -0.004(4) C51 0.047(5) 0.048(5) 0.029(4) 0.002(4) 0.011(4) 0.017(4) C61 0.055(5) 0.032(4) 0.036(5) 0.010(4) 0.020(4) 0.021(4) C71 0.046(5) 0.020(4) 0.045(5) -0.005(3) 0.022(4) -0.001(4) C7A1 0.036(4) 0.027(4) 0.022(4) 0.004(3) 0.012(3) -0.001(3) C1'1 0.036(5) 0.018(4) 0.027(4) 0.001(3) 0.012(4) -0.004(3) N2'1 0.048(4) 0.038(4) 0.033(4) -0.006(3) 0.014(3) -0.001(3) C3'1 0.073(7) 0.052(5) 0.036(5) -0.019(4) 0.021(5) -0.007(5) C4'1 0.077(7) 0.042(5) 0.025(5) -0.006(4) 0.009(5) -0.017(5) C4A1 0.046(5) 0.035(5) 0.030(4) 0.002(4) 0.005(4) -0.019(4) C5'1 0.061(6) 0.059(6) 0.032(5) 0.007(4) 0.004(5) -0.026(5) C6'1 0.032(5) 0.080(7) 0.044(6) 0.019(5) -0.002(4) -0.021(5) C7'1 0.029(5) 0.064(6) 0.049(6) 0.015(5) 0.015(4) -0.004(4) C8'1 0.027(4) 0.049(5) 0.032(4) 0.005(4) 0.008(4) -0.011(4) C8A1 0.038(5) 0.034(4) 0.030(4) 0.001(3) 0.018(4) -0.013(4) N12 0.032(4) 0.036(4) 0.044(4) 0.016(3) 0.011(3) 0.006(3) N22 0.029(4) 0.033(4) 0.041(4) 0.010(3) 0.004(3) 0.006(3) N32 0.026(3) 0.032(4) 0.031(4) 0.005(3) 0.005(3) 0.001(3) C3A2 0.044(5) 0.027(4) 0.040(5) 0.003(4) 0.022(4) 0.006(4) C42 0.058(6) 0.041(5) 0.059(6) 0.003(4) 0.027(5) 0.004(4) C52 0.116(9) 0.051(6) 0.070(7) -0.001(5) 0.049(7) 0.029(6) C62 0.108(9) 0.076(7) 0.068(7) 0.010(6) 0.043(7) 0.054(7) C72 0.054(6) 0.073(7) 0.079(7) 0.021(6) 0.035(6) 0.025(5) C7A2 0.036(5) 0.033(5) 0.058(6) 0.017(4) 0.024(4) 0.009(4) C1'2 0.040(5) 0.038(5) 0.050(5) 0.015(4) 0.008(4) -0.005(4) N2'2 0.040(4) 0.041(4) 0.077(5) 0.028(4) 0.009(4) 0.006(4) C3'2 0.038(6) 0.070(7) 0.082(8) 0.044(6) 0.007(6) 0.010(5) C4'2 0.034(5) 0.092(8) 0.058(7) 0.042(6) -0.006(5) 0.001(6) C4A2 0.034(5) 0.082(7) 0.043(6) 0.023(5) 0.005(4) -0.007(5) C5'2 0.051(7) 0.120(10) 0.045(6) 0.011(6) -0.007(5) -0.025(7) C6'2 0.076(8) 0.112(10) 0.046(6) -0.009(6) 0.006(6) -0.008(7) C7'2 0.044(6) 0.096(8) 0.050(6) -0.009(5) 0.011(5) -0.001(5) C8'2 0.041(5) 0.073(6) 0.043(5) 0.006(5) 0.015(4) -0.001(5) C8A2 0.042(5) 0.049(5) 0.044(5) 0.020(4) 0.016(4) -0.005(4) N13 0.026(3) 0.025(3) 0.016(3) 0.000(2) 0.008(3) 0.001(3) N23 0.030(4) 0.030(3) 0.017(3) 0.002(3) 0.007(3) 0.001(3) N33 0.024(3) 0.028(3) 0.019(3) 0.005(3) 0.008(3) 0.000(3) C3A3 0.032(4) 0.021(4) 0.025(4) 0.001(3) 0.019(3) 0.004(3) C43 0.031(4) 0.038(4) 0.022(4) -0.002(3) 0.008(3) 0.001(4) C53 0.028(4) 0.046(5) 0.030(4) -0.003(4) 0.013(4) -0.004(4) C63 0.043(5) 0.035(4) 0.036(5) 0.005(4) 0.028(4) 0.000(4) C73 0.030(4) 0.024(4) 0.023(4) -0.001(3) 0.014(3) 0.003(3) C7A3 0.024(4) 0.022(4) 0.021(4) -0.003(3) 0.012(3) 0.002(3) C1'3 0.030(4) 0.020(4) 0.025(4) 0.002(3) 0.009(3) -0.001(3) N2'3 0.036(4) 0.032(3) 0.016(3) 0.005(3) 0.012(3) 0.002(3) C3'3 0.051(5) 0.026(4) 0.017(4) 0.006(3) 0.008(4) 0.002(4) C4'3 0.041(5) 0.026(4) 0.022(4) 0.001(3) 0.005(4) 0.006(3) C4A3 0.031(4) 0.015(4) 0.035(4) 0.004(3) 0.011(4) -0.001(3) C5'3 0.036(5) 0.026(4) 0.035(5) -0.004(3) -0.001(4) -0.007(3) C6'3 0.031(4) 0.021(4) 0.053(5) 0.005(4) 0.019(4) 0.001(3) C7'3 0.044(5) 0.022(4) 0.037(5) 0.005(3) 0.020(4) 0.008(3) C8'3 0.035(5) 0.020(4) 0.034(4) 0.000(3) 0.014(4) 0.001(3) C8A3 0.034(4) 0.013(4) 0.027(4) 0.006(3) 0.010(4) 0.002(3) N14 0.041(4) 0.039(4) 0.072(5) 0.007(4) 0.044(4) -0.008(3) N24 0.048(4) 0.032(4) 0.049(4) -0.002(3) 0.033(3) -0.006(3) N34 0.028(3) 0.026(3) 0.028(3) -0.001(3) 0.014(3) -0.006(3) C3A4 0.029(4) 0.019(4) 0.029(4) 0.009(3) 0.005(3) -0.004(3) C44 0.049(5) 0.028(4) 0.029(4) 0.004(3) 0.007(4) -0.011(4) C54 0.068(6) 0.037(5) 0.030(5) 0.004(4) 0.000(4) -0.014(5) C64 0.062(6) 0.035(5) 0.042(5) -0.005(4) -0.002(5) -0.009(5) C74 0.033(5) 0.028(5) 0.080(7) 0.022(5) 0.004(5) -0.011(4) C7A4 0.039(5) 0.020(4) 0.047(5) 0.003(4) 0.021(4) -0.001(4) C1'4 0.080(8) 0.036(5) 0.056(6) -0.009(5) 0.009(6) -0.009(5) N2'4 0.055(5) 0.095(7) 0.094(7) -0.011(5) 0.034(5) -0.014(5) C3'4 0.082(8) 0.092(8) 0.132(11) -0.010(8) 0.073(8) -0.014(7) C4'4 0.125(11) 0.045(6) 0.117(10) -0.012(7) 0.088(9) -0.029(7) C4A4 0.090(8) 0.019(5) 0.116(10) -0.002(5) 0.076(8) -0.009(5) C5'4 0.226(17) 0.028(6) 0.125(11) 0.007(7) 0.135(12) -0.002(8) C6'4 0.207(15) 0.025(6) 0.084(9) 0.001(6) 0.086(10) 0.008(8) C7'4 0.32(2) 0.017(5) 0.088(9) -0.012(5) 0.101(12) -0.035(9) C8'4 0.122(9) 0.018(4) 0.040(5) -0.006(4) 0.045(6) -0.022(5) C8A4 0.103(8) 0.015(5) 0.072(7) -0.008(4) 0.022(7) -0.011(5) N91 0.14(2) 0.56(8) 0.047(15) -0.09(3) 0.048(18) -0.18(4) C91 0.22(2) 0.106(16) 0.131(18) -0.036(14) 0.072(16) -0.029(16) O91 0.214(16) 0.219(15) 0.228(17) 0.000 0.122(14) 0.000 O92 0.31(2) 0.29(2) 0.25(2) 0.000 0.101(17) 0.000 N92 0.32(2) 0.49(3) 0.40(2) -0.027(18) 0.184(19) 0.079(19) C92 0.262(17) 0.163(13) 0.145(12) -0.017(10) 0.070(12) 0.058(12) O93 0.351(18) 0.409(19) 0.335(17) 0.098(14) 0.179(14) -0.090(15) O94 0.50(2) 0.50(2) 0.340(19) -0.058(15) 0.032(15) 0.274(17) N93 1.05(9) 1.03(9) 1.04(9) 0.02(2) 0.33(3) 0.01(2) C93 0.47(3) 0.32(2) 0.44(3) 0.016(19) 0.088(18) 0.073(19) O95 0.427(19) 0.311(15) 0.236(13) -0.093(12) 0.133(13) -0.020(14) O96 0.391(17) 0.266(14) 0.287(14) 0.066(12) 0.179(13) -0.013(13) _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 O1 1.913(4) . ? Cu1 N34 1.984(5) . ? Cu1 Cl3 2.3579(19) . ? Cu1 Cl2 2.4059(19) . ? Cu1 Cl6 2.449(2) . ? Cu2 O1 1.908(4) . ? Cu2 N33 1.980(5) . ? Cu2 Cl6 2.362(2) . ? Cu2 Cl5 2.385(2) . ? Cu2 Cl1 2.470(2) . ? Cu3 O1 1.915(4) . ? Cu3 N31 1.970(5) . ? Cu3 Cl1 2.357(2) . ? Cu3 Cl3 2.4337(19) . ? Cu3 Cl4 2.4379(19) . ? Cu4 O1 1.901(4) . ? Cu4 N32 1.971(5) . ? Cu4 Cl4 2.376(2) . ? Cu4 Cl5 2.443(2) . ? Cu4 Cl2 2.456(2) . ? N11 N21 1.357(5) . ? N11 C7A1 1.380(6) . ? N11 C1'1 1.450(6) . ? N21 N31 1.304(5) . ? N31 C3A1 1.390(6) . ? C3A1 C7A1 1.394(6) . ? C3A1 C41 1.400(6) . ? C41 C51 1.375(7) . ? C51 C61 1.399(7) . ? C61 C71 1.367(7) . ? C71 C7A1 1.407(6) . ? C1'1 N2'1 1.305(6) . ? C1'1 C8A1 1.405(7) . ? N2'1 C3'1 1.366(7) . ? C3'1 C4'1 1.367(7) . ? C4'1 C4A1 1.398(7) . ? C4A1 C5'1 1.405(7) . ? C4A1 C8A1 1.444(7) . ? C5'1 C6'1 1.377(8) . ? C6'1 C7'1 1.394(8) . ? C7'1 C8'1 1.383(7) . ? C8'1 C8A1 1.422(7) . ? N12 N22 1.358(6) . ? N12 C7A2 1.385(6) . ? N12 C1'2 1.447(6) . ? N22 N32 1.306(6) . ? N32 C3A2 1.384(6) . ? C3A2 C7A2 1.390(7) . ? C3A2 C42 1.395(7) . ? C42 C52 1.371(7) . ? C52 C62 1.404(8) . ? C62 C72 1.363(8) . ? C72 C7A2 1.405(7) . ? C1'2 N2'2 1.303(6) . ? C1'2 C8A2 1.410(7) . ? N2'2 C3'2 1.365(7) . ? C3'2 C4'2 1.355(8) . ? C4'2 C4A2 1.395(8) . ? C4A2 C5'2 1.403(8) . ? C4A2 C8A2 1.444(7) . ? C5'2 C6'2 1.383(8) . ? C6'2 C7'2 1.391(8) . ? C7'2 C8'2 1.385(7) . ? C8'2 C8A2 1.429(7) . ? N13 N23 1.356(5) . ? N13 C7A3 1.384(6) . ? N13 C1'3 1.455(6) . ? N23 N33 1.304(5) . ? N33 C3A3 1.394(6) . ? C3A3 C7A3 1.393(6) . ? C3A3 C43 1.400(6) . ? C43 C53 1.378(7) . ? C53 C63 1.404(7) . ? C63 C73 1.372(7) . ? C73 C7A3 1.406(6) . ? C1'3 N2'3 1.309(6) . ? C1'3 C8A3 1.411(6) . ? N2'3 C3'3 1.375(6) . ? C3'3 C4'3 1.362(7) . ? C4'3 C4A3 1.403(7) . ? C4A3 C5'3 1.408(7) . ? C4A3 C8A3 1.443(7) . ? C5'3 C6'3 1.382(7) . ? C6'3 C7'3 1.392(7) . ? C7'3 C8'3 1.372(7) . ? C8'3 C8A3 1.437(7) . ? N14 N24 1.354(6) . ? N14 C7A4 1.369(6) . ? N14 C1'4 1.463(7) . ? N24 N34 1.303(6) . ? N34 C3A4 1.392(6) . ? C3A4 C7A4 1.385(6) . ? C3A4 C44 1.396(7) . ? C44 C54 1.372(7) . ? C54 C64 1.397(7) . ? C64 C74 1.366(7) . ? C74 C7A4 1.408(7) . ? C1'4 N2'4 1.298(7) . ? C1'4 C8A4 1.373(7) . ? N2'4 C3'4 1.376(7) . ? C3'4 C4'4 1.366(8) . ? C4'4 C4A4 1.378(8) . ? C4A4 C5'4 1.381(8) . ? C4A4 C8A4 1.468(7) . ? C5'4 C6'4 1.407(9) . ? C6'4 C7'4 1.388(9) . ? C7'4 C8'4 1.380(8) . ? C8'4 C8A4 1.426(7) . ? N91 O91 1.211(10) . ? N91 O92 1.214(11) . ? N91 N91 1.49(5) 2 ? N91 C91 1.468(10) . ? O91 N91 1.211(10) 2 ? O92 N91 1.214(11) 2 ? N92 O93 1.187(10) . ? N92 O94 1.195(10) . ? N92 C92 1.471(10) . ? N93 O95 1.205(11) . ? N93 O96 1.213(11) . ? N93 C93 1.474(11) . ? 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 O1 Cu1 N34 176.95(19) . . ? O1 Cu1 Cl3 86.07(13) . . ? N34 Cu1 Cl3 96.87(15) . . ? O1 Cu1 Cl2 84.91(13) . . ? N34 Cu1 Cl2 93.90(16) . . ? Cl3 Cu1 Cl2 128.01(7) . . ? O1 Cu1 Cl6 82.65(12) . . ? N34 Cu1 Cl6 95.15(15) . . ? Cl3 Cu1 Cl6 119.32(7) . . ? Cl2 Cu1 Cl6 110.04(7) . . ? O1 Cu2 N33 175.55(19) . . ? O1 Cu2 Cl6 85.16(12) . . ? N33 Cu2 Cl6 94.76(14) . . ? O1 Cu2 Cl5 85.53(12) . . ? N33 Cu2 Cl5 97.81(15) . . ? Cl6 Cu2 Cl5 131.25(7) . . ? O1 Cu2 Cl1 82.83(12) . . ? N33 Cu2 Cl1 93.46(15) . . ? Cl6 Cu2 Cl1 121.58(7) . . ? Cl5 Cu2 Cl1 104.45(7) . . ? O1 Cu3 N31 175.45(19) . . ? O1 Cu3 Cl1 85.81(13) . . ? N31 Cu3 Cl1 93.89(15) . . ? O1 Cu3 Cl3 83.91(12) . . ? N31 Cu3 Cl3 93.07(15) . . ? Cl1 Cu3 Cl3 133.77(7) . . ? O1 Cu3 Cl4 83.71(12) . . ? N31 Cu3 Cl4 100.41(15) . . ? Cl1 Cu3 Cl4 117.91(8) . . ? Cl3 Cu3 Cl4 105.54(7) . . ? O1 Cu4 N32 177.3(2) . . ? O1 Cu4 Cl4 85.74(13) . . ? N32 Cu4 Cl4 96.66(16) . . ? O1 Cu4 Cl5 84.04(13) . . ? N32 Cu4 Cl5 95.82(16) . . ? Cl4 Cu4 Cl5 120.81(7) . . ? O1 Cu4 Cl2 83.75(13) . . ? N32 Cu4 Cl2 93.78(16) . . ? Cl4 Cu4 Cl2 124.95(7) . . ? Cl5 Cu4 Cl2 111.54(7) . . ? Cu3 Cl1 Cu2 80.67(6) . . ? Cu1 Cl2 Cu4 79.40(6) . . ? Cu1 Cl3 Cu3 80.94(6) . . ? Cu4 Cl4 Cu3 80.54(6) . . ? Cu2 Cl5 Cu4 80.29(6) . . ? Cu2 Cl6 Cu1 81.37(5) . . ? Cu4 O1 Cu2 109.64(19) . . ? Cu4 O1 Cu1 109.05(19) . . ? Cu2 O1 Cu1 110.43(19) . . ? Cu4 O1 Cu3 109.28(19) . . ? Cu2 O1 Cu3 109.70(19) . . ? Cu1 O1 Cu3 108.72(19) . . ? N21 N11 C7A1 110.6(4) . . ? N21 N11 C1'1 120.6(4) . . ? C7A1 N11 C1'1 128.3(4) . . ? N31 N21 N11 107.4(4) . . ? N21 N31 C3A1 110.5(4) . . ? N21 N31 Cu3 121.0(4) . . ? C3A1 N31 Cu3 128.4(4) . . ? N31 C3A1 C7A1 106.8(4) . . ? N31 C3A1 C41 131.1(5) . . ? C7A1 C3A1 C41 122.1(5) . . ? C51 C41 C3A1 116.4(5) . . ? C41 C51 C61 121.5(6) . . ? C71 C61 C51 122.8(6) . . ? C61 C71 C7A1 116.4(5) . . ? N11 C7A1 C3A1 104.7(4) . . ? N11 C7A1 C71 134.4(5) . . ? C3A1 C7A1 C71 120.8(5) . . ? N2'1 C1'1 C8A1 126.4(5) . . ? N2'1 C1'1 N11 111.3(5) . . ? C8A1 C1'1 N11 122.2(5) . . ? C1'1 N2'1 C3'1 117.5(5) . . ? C4'1 C3'1 N2'1 122.4(6) . . ? C3'1 C4'1 C4A1 120.2(6) . . ? C4'1 C4A1 C5'1 123.0(6) . . ? C4'1 C4A1 C8A1 118.4(5) . . ? C5'1 C4A1 C8A1 118.6(6) . . ? C6'1 C5'1 C4A1 122.3(6) . . ? C5'1 C6'1 C7'1 119.6(6) . . ? C8'1 C7'1 C6'1 120.4(6) . . ? C7'1 C8'1 C8A1 121.6(6) . . ? C1'1 C8A1 C8'1 127.5(5) . . ? C1'1 C8A1 C4A1 115.0(5) . . ? C8'1 C8A1 C4A1 117.5(5) . . ? N22 N12 C7A2 110.0(4) . . ? N22 N12 C1'2 120.8(5) . . ? C7A2 N12 C1'2 129.2(5) . . ? N32 N22 N12 108.0(5) . . ? N22 N32 C3A2 109.9(5) . . ? N22 N32 Cu4 119.2(4) . . ? C3A2 N32 Cu4 130.8(4) . . ? N32 C3A2 C7A2 107.5(5) . . ? N32 C3A2 C42 130.0(6) . . ? C7A2 C3A2 C42 122.5(5) . . ? C52 C42 C3A2 116.0(6) . . ? C42 C52 C62 122.0(7) . . ? C72 C62 C52 122.0(7) . . ? C62 C72 C7A2 116.9(7) . . ? N12 C7A2 C3A2 104.6(5) . . ? N12 C7A2 C72 134.8(6) . . ? C3A2 C7A2 C72 120.5(6) . . ? N2'2 C1'2 C8A2 125.4(6) . . ? N2'2 C1'2 N12 110.9(5) . . ? C8A2 C1'2 N12 123.6(5) . . ? C1'2 N2'2 C3'2 118.1(6) . . ? C4'2 C3'2 N2'2 122.5(7) . . ? C3'2 C4'2 C4A2 120.2(7) . . ? C4'2 C4A2 C5'2 122.1(7) . . ? C4'2 C4A2 C8A2 118.4(6) . . ? C5'2 C4A2 C8A2 119.4(6) . . ? C6'2 C5'2 C4A2 122.0(7) . . ? C5'2 C6'2 C7'2 119.0(7) . . ? C8'2 C7'2 C6'2 121.4(7) . . ? C7'2 C8'2 C8A2 121.0(6) . . ? C1'2 C8A2 C8'2 127.8(6) . . ? C1'2 C8A2 C4A2 115.1(6) . . ? C8'2 C8A2 C4A2 117.0(6) . . ? N23 N13 C7A3 110.5(4) . . ? N23 N13 C1'3 120.3(4) . . ? C7A3 N13 C1'3 129.2(4) . . ? N33 N23 N13 107.9(4) . . ? N23 N33 C3A3 109.9(4) . . ? N23 N33 Cu2 120.1(3) . . ? C3A3 N33 Cu2 128.8(4) . . ? C7A3 C3A3 N33 107.1(4) . . ? C7A3 C3A3 C43 121.8(5) . . ? N33 C3A3 C43 131.0(5) . . ? C53 C43 C3A3 115.9(5) . . ? C43 C53 C63 121.9(6) . . ? C73 C63 C53 122.9(5) . . ? C63 C73 C7A3 115.3(5) . . ? N13 C7A3 C3A3 104.5(4) . . ? N13 C7A3 C73 133.4(5) . . ? C3A3 C7A3 C73 122.1(5) . . ? N2'3 C1'3 C8A3 126.9(5) . . ? N2'3 C1'3 N13 111.9(5) . . ? C8A3 C1'3 N13 121.1(5) . . ? C1'3 N2'3 C3'3 116.2(5) . . ? C4'3 C3'3 N2'3 123.4(6) . . ? C3'3 C4'3 C4A3 120.1(5) . . ? C4'3 C4A3 C5'3 122.3(5) . . ? C4'3 C4A3 C8A3 118.1(5) . . ? C5'3 C4A3 C8A3 119.6(5) . . ? C6'3 C5'3 C4A3 121.0(6) . . ? C5'3 C6'3 C7'3 120.0(6) . . ? C8'3 C7'3 C6'3 121.3(6) . . ? C7'3 C8'3 C8A3 120.8(5) . . ? C1'3 C8A3 C8'3 127.6(5) . . ? C1'3 C8A3 C4A3 115.1(5) . . ? C8'3 C8A3 C4A3 117.2(5) . . ? N24 N14 C7A4 111.6(4) . . ? N24 N14 C1'4 122.9(5) . . ? C7A4 N14 C1'4 124.6(5) . . ? N34 N24 N14 107.1(4) . . ? N24 N34 C3A4 109.7(4) . . ? N24 N34 Cu1 124.3(4) . . ? C3A4 N34 Cu1 126.1(4) . . ? C7A4 C3A4 N34 107.6(5) . . ? C7A4 C3A4 C44 120.9(5) . . ? N34 C3A4 C44 131.4(5) . . ? C54 C44 C3A4 115.9(6) . . ? C44 C54 C64 122.9(6) . . ? C74 C64 C54 122.3(6) . . ? C64 C74 C7A4 114.9(6) . . ? N14 C7A4 C3A4 104.0(5) . . ? N14 C7A4 C74 132.9(6) . . ? C3A4 C7A4 C74 123.1(5) . . ? N2'4 C1'4 C8A4 127.8(7) . . ? N2'4 C1'4 N14 114.4(6) . . ? C8A4 C1'4 N14 117.6(6) . . ? C1'4 N2'4 C3'4 116.9(7) . . ? C4'4 C3'4 N2'4 121.3(8) . . ? C3'4 C4'4 C4A4 122.1(8) . . ? C4'4 C4A4 C5'4 126.0(8) . . ? C4'4 C4A4 C8A4 116.6(7) . . ? C5'4 C4A4 C8A4 117.4(7) . . ? C4A4 C5'4 C6'4 123.4(8) . . ? C7'4 C6'4 C5'4 119.0(8) . . ? C8'4 C7'4 C6'4 120.5(9) . . ? C7'4 C8'4 C8A4 121.7(7) . . ? C1'4 C8A4 C8'4 126.8(7) . . ? C1'4 C8A4 C4A4 115.3(7) . . ? C8'4 C8A4 C4A4 117.9(6) . . ? O91 N91 O92 104(3) . . ? O91 N91 N91 52.0(14) . 2 ? O92 N91 N91 52.1(14) . 2 ? O91 N91 C91 107(2) . . ? O92 N91 C91 148.9(19) . . ? N91 N91 C91 158.4(14) 2 . ? N91 O91 N91 76(3) . 2 ? N91 O92 N91 76(3) 2 . ? O93 N92 O94 168(3) . . ? O93 N92 C92 93.0(18) . . ? O94 N92 C92 100(2) . . ? O95 N93 O96 101.1(19) . . ? O95 N93 C93 96.8(19) . . ? O96 N93 C93 162(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.256 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.094 #===END data_3cr3(complex20) _database_code_CSD 190044 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 Ag N8 O3' _chemical_formula_weight 461.20 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 9.212(1) _cell_length_b 9.307(1) _cell_length_c 11.849(1) _cell_angle_alpha 92.28(1) _cell_angle_beta 105.92(1) _cell_angle_gamma 115.69(1) _cell_volume 865.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 33 _cell_measurement_theta_max 17 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.74 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'Seimens P4s' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 13 _diffrn_reflns_number 4400 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4150 _reflns_number_observed 3561 _reflns_observed_criterion >2sigma(I) _computing_data_collection xscans _computing_cell_refinement xscans _computing_data_reduction xscans _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics xp _computing_publication_material xcif _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4150 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Ag1 Ag 0.36804(2) 0.59286(2) 0.322942(17) 0.03053(7) Uani 1 1 d . . . N1 N -0.1743(2) 0.3023(2) 0.22550(17) 0.0239(4) Uani 1 1 d . . . N2 N -0.0232(2) 0.3922(2) 0.20846(18) 0.0274(4) Uani 1 1 d . . . N3 N 0.0971(2) 0.4222(2) 0.30832(18) 0.0276(4) Uani 1 1 d . . . C3A C 0.0255(3) 0.3538(3) 0.3935(2) 0.0239(4) Uani 1 1 d . . . C4 C 0.1005(3) 0.3537(3) 0.5135(2) 0.0297(5) Uani 1 1 d . . . H4 H 0.2205 0.4054 0.5505 0.036 Uiso 1 1 calc R . . C5 C -0.0090(3) 0.2749(3) 0.5744(2) 0.0349(5) Uani 1 1 d . . . H5 H 0.0367 0.2720 0.6561 0.042 Uiso 1 1 calc R . . C6 C -0.1868(3) 0.1981(3) 0.5202(2) 0.0347(5) Uani 1 1 d . . . H6 H -0.2571 0.1460 0.5667 0.042 Uiso 1 1 calc R . . C7 C -0.2623(3) 0.1958(3) 0.4023(2) 0.0287(5) Uani 1 1 d . . . H7 H -0.3824 0.1431 0.3654 0.034 Uiso 1 1 calc R . . C7A C -0.1502(3) 0.2764(2) 0.3404(2) 0.0226(4) Uani 1 1 d . . . C1 C -0.3294(3) 0.2738(3) 0.1328(2) 0.0262(4) Uani 1 1 d . . . H1A H -0.3154 0.2626 0.0535 0.031 Uiso 1 1 calc R . . H1B H -0.4250 0.1716 0.1364 0.031 Uiso 1 1 calc R . . N1' N -0.3677(2) 0.4071(2) 0.14814(16) 0.0228(4) Uani 1 1 d . . . N2' N -0.4717(2) 0.3986(2) 0.21212(17) 0.0253(4) Uani 1 1 d . . . N3' N -0.4738(2) 0.5371(2) 0.22320(18) 0.0271(4) Uani 1 1 d . . . C3A' C -0.3679(3) 0.6403(3) 0.1676(2) 0.0247(4) Uani 1 1 d . . . C4' C -0.3248(3) 0.8017(3) 0.1573(2) 0.0305(5) Uani 1 1 d . . . H4' H -0.3715 0.8594 0.1903 0.037 Uiso 1 1 calc R . . C5' C -0.2114(3) 0.8726(3) 0.0970(2) 0.0345(5) Uani 1 1 d . . . H5' H -0.1800 0.9817 0.0871 0.041 Uiso 1 1 calc R . . C6' C -0.1404(3) 0.7876(3) 0.0496(2) 0.0343(5) Uani 1 1 d . . . H6' H -0.0616 0.8421 0.0094 0.041 Uiso 1 1 calc R . . C7' C -0.1803(3) 0.6297(3) 0.0591(2) 0.0296(5) Uani 1 1 d . . . H7' H -0.1317 0.5731 0.0272 0.036 Uiso 1 1 calc R . . C7A' C -0.2978(3) 0.5576(3) 0.11933(19) 0.0230(4) Uani 1 1 d . . . N5 N 0.3154(2) 0.8278(2) 0.16349(17) 0.0249(4) Uani 1 1 d . . . O1 O 0.2540(3) 0.6835(2) 0.11804(17) 0.0406(4) Uani 1 1 d . . . O2 O 0.3813(3) 0.8684(2) 0.27422(16) 0.0414(4) Uani 1 1 d . . . O3 O 0.3147(3) 0.9312(2) 0.10033(17) 0.0401(4) Uani 1 1 d . . . N4 N 0.5576(3) 0.7231(3) 0.5094(2) 0.0435(6) Uani 1 1 d . . . C2 C 0.6589(3) 0.7902(3) 0.5980(2) 0.0342(5) Uani 1 1 d . . . C3 C 0.7912(4) 0.8780(3) 0.7113(2) 0.0388(6) Uani 1 1 d . . . H3A H 0.8111 0.8008 0.7592 0.058 Uiso 1 1 calc R . . H3B H 0.7552 0.9417 0.7545 0.058 Uiso 1 1 calc R . . H3C H 0.8965 0.9509 0.6969 0.058 Uiso 1 1 calc R . . 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 0.02455(10) 0.03180(10) 0.03786(11) 0.01143(7) 0.01405(7) 0.01255(7) N1 0.0204(8) 0.0255(9) 0.0252(9) 0.0051(7) 0.0090(7) 0.0092(7) N2 0.0222(9) 0.0305(10) 0.0311(10) 0.0080(8) 0.0131(8) 0.0107(8) N3 0.0241(9) 0.0283(10) 0.0334(10) 0.0075(8) 0.0131(8) 0.0124(8) C3A 0.0224(10) 0.0233(10) 0.0294(11) 0.0044(9) 0.0099(9) 0.0126(9) C4 0.0266(11) 0.0315(12) 0.0305(12) 0.0042(10) 0.0060(10) 0.0151(10) C5 0.0412(14) 0.0393(13) 0.0278(12) 0.0094(10) 0.0116(11) 0.0212(12) C6 0.0370(13) 0.0366(13) 0.0379(14) 0.0163(11) 0.0212(11) 0.0173(11) C7 0.0262(11) 0.0249(11) 0.0393(13) 0.0099(10) 0.0172(10) 0.0113(9) C7A 0.0231(10) 0.0199(10) 0.0265(11) 0.0042(8) 0.0090(9) 0.0109(8) C1 0.0241(11) 0.0255(11) 0.0252(11) 0.0026(9) 0.0056(9) 0.0097(9) N1' 0.0200(8) 0.0246(9) 0.0209(9) 0.0043(7) 0.0065(7) 0.0077(7) N2' 0.0204(9) 0.0296(10) 0.0259(9) 0.0058(8) 0.0085(7) 0.0109(8) N3' 0.0216(9) 0.0273(9) 0.0321(10) 0.0065(8) 0.0099(8) 0.0102(8) C3A' 0.0181(10) 0.0299(11) 0.0230(10) 0.0066(9) 0.0045(8) 0.0096(9) C4' 0.0251(11) 0.0288(12) 0.0369(13) 0.0070(10) 0.0056(10) 0.0144(10) C5' 0.0314(12) 0.0284(12) 0.0393(14) 0.0141(10) 0.0080(11) 0.0115(10) C6' 0.0323(12) 0.0347(13) 0.0287(12) 0.0107(10) 0.0130(10) 0.0070(10) C7' 0.0293(11) 0.0323(12) 0.0247(11) 0.0050(9) 0.0125(9) 0.0097(10) C7A' 0.0212(10) 0.0236(10) 0.0191(10) 0.0041(8) 0.0039(8) 0.0074(8) N5 0.0232(9) 0.0271(9) 0.0272(10) 0.0059(8) 0.0127(8) 0.0113(8) O1 0.0575(12) 0.0234(8) 0.0365(10) 0.0036(7) 0.0173(9) 0.0139(8) O2 0.0504(12) 0.0436(11) 0.0239(9) 0.0013(8) 0.0061(8) 0.0201(9) O3 0.0585(12) 0.0326(9) 0.0404(10) 0.0196(8) 0.0245(9) 0.0246(9) N4 0.0372(12) 0.0525(14) 0.0386(13) 0.0009(11) 0.0085(11) 0.0217(11) C2 0.0328(13) 0.0357(13) 0.0415(15) 0.0076(11) 0.0157(12) 0.0199(11) C3 0.0387(14) 0.0357(13) 0.0400(14) 0.0001(11) 0.0084(12) 0.0186(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.2554(19) . ? Ag1 N4 2.288(2) . ? Ag1 N3' 2.3108(19) 1_655 ? N1 N2 1.355(2) . ? N1 C7A 1.367(3) . ? N1 C1 1.452(3) . ? N2 N3 1.301(3) . ? N3 C3A 1.382(3) . ? C3A C7A 1.389(3) . ? C3A C4 1.400(3) . ? C4 C5 1.370(3) . ? C5 C6 1.406(4) . ? C6 C7 1.374(4) . ? C7 C7A 1.398(3) . ? C1 N1' 1.447(3) . ? N1' N2' 1.355(2) . ? N1' C7A' 1.367(3) . ? N2' N3' 1.300(3) . ? N3' C3A' 1.378(3) . ? N3' Ag1 2.3108(19) 1_455 ? C3A' C7A' 1.391(3) . ? C3A' C4' 1.398(3) . ? C4' C5' 1.373(4) . ? C5' C6' 1.408(4) . ? C6' C7' 1.370(4) . ? C7' C7A' 1.401(3) . ? N5 O1 1.237(3) . ? N5 O3 1.243(3) . ? N5 O2 1.248(3) . ? N4 C2 1.126(3) . ? C2 C3 1.452(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 N3 Ag1 N4 117.84(8) . . ? N3 Ag1 N3' 124.93(7) . 1_655 ? N4 Ag1 N3' 104.04(8) . 1_655 ? N2 N1 C7A 110.81(18) . . ? N2 N1 C1 118.41(18) . . ? C7A N1 C1 129.76(18) . . ? N3 N2 N1 107.81(18) . . ? N2 N3 C3A 109.40(18) . . ? N2 N3 Ag1 118.72(14) . . ? C3A N3 Ag1 131.32(16) . . ? N3 C3A C7A 107.8(2) . . ? N3 C3A C4 131.1(2) . . ? C7A C3A C4 121.1(2) . . ? C5 C4 C3A 116.2(2) . . ? C4 C5 C6 122.2(2) . . ? C7 C6 C5 122.3(2) . . ? C6 C7 C7A 115.4(2) . . ? N1 C7A C3A 104.21(19) . . ? N1 C7A C7 133.0(2) . . ? C3A C7A C7 122.8(2) . . ? N1' C1 N1 110.17(18) . . ? N2' N1' C7A' 110.53(18) . . ? N2' N1' C1 119.49(18) . . ? C7A' N1' C1 129.47(19) . . ? N3' N2' N1' 108.24(18) . . ? N2' N3' C3A' 109.06(19) . . ? N2' N3' Ag1 123.71(14) . 1_455 ? C3A' N3' Ag1 127.22(15) . 1_455 ? N3' C3A' C7A' 108.1(2) . . ? N3' C3A' C4' 130.8(2) . . ? C7A' C3A' C4' 121.1(2) . . ? C5' C4' C3A' 116.5(2) . . ? C4' C5' C6' 121.7(2) . . ? C7' C6' C5' 122.7(2) . . ? C6' C7' C7A' 115.2(2) . . ? N1' C7A' C3A' 104.03(19) . . ? N1' C7A' C7' 133.2(2) . . ? C3A' C7A' C7' 122.7(2) . . ? O1 N5 O3 120.9(2) . . ? O1 N5 O2 118.6(2) . . ? O3 N5 O2 120.4(2) . . ? C2 N4 Ag1 175.6(2) . . ? N4 C2 C3 179.1(3) . . ? 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 C7A N1 N2 N3 1.1(2) . . . . ? C1 N1 N2 N3 170.65(19) . . . . ? N1 N2 N3 C3A -0.9(2) . . . . ? N1 N2 N3 Ag1 -173.33(13) . . . . ? N4 Ag1 N3 N2 155.87(16) . . . . ? N3' Ag1 N3 N2 -69.43(18) 1_655 . . . ? N4 Ag1 N3 C3A -14.6(2) . . . . ? N3' Ag1 N3 C3A 120.14(19) 1_655 . . . ? N2 N3 C3A C7A 0.4(2) . . . . ? Ag1 N3 C3A C7A 171.54(15) . . . . ? N2 N3 C3A C4 -179.3(2) . . . . ? Ag1 N3 C3A C4 -8.2(4) . . . . ? N3 C3A C4 C5 179.1(2) . . . . ? C7A C3A C4 C5 -0.6(3) . . . . ? C3A C4 C5 C6 0.0(4) . . . . ? C4 C5 C6 C7 0.6(4) . . . . ? C5 C6 C7 C7A -0.6(4) . . . . ? N2 N1 C7A C3A -0.8(2) . . . . ? C1 N1 C7A C3A -168.8(2) . . . . ? N2 N1 C7A C7 178.5(2) . . . . ? C1 N1 C7A C7 10.5(4) . . . . ? N3 C3A C7A N1 0.2(2) . . . . ? C4 C3A C7A N1 -180.0(2) . . . . ? N3 C3A C7A C7 -179.2(2) . . . . ? C4 C3A C7A C7 0.6(3) . . . . ? C6 C7 C7A N1 -179.2(2) . . . . ? C6 C7 C7A C3A 0.0(3) . . . . ? N2 N1 C1 N1' -85.5(2) . . . . ? C7A N1 C1 N1' 81.7(3) . . . . ? N1 C1 N1' N2' -92.7(2) . . . . ? N1 C1 N1' C7A' 78.3(3) . . . . ? C7A' N1' N2' N3' 1.3(2) . . . . ? C1 N1' N2' N3' 173.96(18) . . . . ? N1' N2' N3' C3A' -0.9(2) . . . . ? N1' N2' N3' Ag1 179.47(13) . . . 1_455 ? N2' N3' C3A' C7A' 0.2(3) . . . . ? Ag1 N3' C3A' C7A' 179.81(14) 1_455 . . . ? N2' N3' C3A' C4' -178.4(2) . . . . ? Ag1 N3' C3A' C4' 1.2(3) 1_455 . . . ? N3' C3A' C4' C5' 178.8(2) . . . . ? C7A' C3A' C4' C5' 0.3(3) . . . . ? C3A' C4' C5' C6' -0.9(4) . . . . ? C4' C5' C6' C7' 0.7(4) . . . . ? C5' C6' C7' C7A' 0.2(4) . . . . ? N2' N1' C7A' C3A' -1.1(2) . . . . ? C1 N1' C7A' C3A' -172.8(2) . . . . ? N2' N1' C7A' C7' 177.5(2) . . . . ? C1 N1' C7A' C7' 5.8(4) . . . . ? N3' C3A' C7A' N1' 0.5(2) . . . . ? C4' C3A' C7A' N1' 179.3(2) . . . . ? N3' C3A' C7A' C7' -178.3(2) . . . . ? C4' C3A' C7A' C7' 0.5(3) . . . . ? C6' C7' C7A' N1' -179.2(2) . . . . ? C6' C7' C7A' C3A' -0.8(3) . . . . ? N3 Ag1 N4 C2 169(3) . . . . ? N3' Ag1 N4 C2 26(3) 1_655 . . . ? Ag1 N4 C2 C3 22(23) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.923 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.084 #===END data_3cr35(complex21) _database_code_CSD 190045 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 223-225 _chemical_formula_moiety ? _chemical_formula_sum 'C11 H8 Ag N5 O3' _chemical_formula_weight 366.09 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 8.308(2) _cell_length_b 8.675(2) _cell_length_c 9.664(3) _cell_angle_alpha 102.377(4) _cell_angle_beta 109.288(3) _cell_angle_gamma 107.132(3) _cell_volume 589.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 1.726 _exptl_absorpt_correction_type 'multi scans (SADABS)' _exptl_absorpt_correction_T_min 0.4503 _exptl_absorpt_correction_T_max 0.8328 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'SMART CCD (Siemens 1995)' _diffrn_measurement_method 'Exposures over 0.5\% \f or \w rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7588 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.48 _reflns_number_total 2387 _reflns_number_gt 2206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens 1995)' _computing_cell_refinement 'SAINT (Siemens 1995)' _computing_data_reduction 'SAINT (Siemens 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.2544P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2387 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0562 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Ag1 Ag 0.30748(3) 0.62280(3) 0.05328(2) 0.02893(8) Uani 1 1 d . . . N1 N 0.6492(3) 0.3826(2) 0.2712(2) 0.0203(4) Uani 1 1 d . . . N2 N 0.5324(3) 0.4153(3) 0.1559(2) 0.0227(4) Uani 1 1 d . . . N3 N 0.5069(3) 0.5497(3) 0.2193(2) 0.0222(4) Uani 1 1 d . . . C3A C 0.6077(3) 0.6085(3) 0.3791(3) 0.0205(5) Uani 1 1 d . . . C4 C 0.6252(3) 0.7488(3) 0.4970(3) 0.0254(5) Uani 1 1 d . . . H4 H 0.5639 0.8228 0.4735 0.030 Uiso 1 1 calc R . . C5 C 0.7355(4) 0.7721(3) 0.6474(3) 0.0288(5) Uani 1 1 d . . . H5 H 0.7516 0.8653 0.7304 0.035 Uiso 1 1 calc R . . C6 C 0.8263(3) 0.6612(3) 0.6828(3) 0.0282(5) Uani 1 1 d . . . H6 H 0.8983 0.6805 0.7891 0.034 Uiso 1 1 calc R . . C7 C 0.8138(3) 0.5259(3) 0.5681(3) 0.0230(5) Uani 1 1 d . . . H7 H 0.8781 0.4541 0.5920 0.028 Uiso 1 1 calc R . . C7A C 0.7006(3) 0.5014(3) 0.4149(3) 0.0195(4) Uani 1 1 d . . . N1' N 0.7103(3) 0.2052(2) 0.0937(2) 0.0205(4) Uani 1 1 d . . . C2' C 0.6960(3) 0.2377(3) 0.2297(3) 0.0205(5) Uani 1 1 d . . . C3' C 0.7215(3) 0.1420(3) 0.3259(3) 0.0253(5) Uani 1 1 d . . . H3' H 0.7095 0.1700 0.4216 0.030 Uiso 1 1 calc R . . C4' C 0.7656(4) 0.0027(3) 0.2776(3) 0.0293(5) Uani 1 1 d . . . H4' H 0.7895 -0.0635 0.3425 0.035 Uiso 1 1 calc R . . C5' C 0.7744(3) -0.0385(3) 0.1342(3) 0.0287(5) Uani 1 1 d . . . H5' H 0.7992 -0.1356 0.0972 0.034 Uiso 1 1 calc R . . C6' C 0.7462(3) 0.0654(3) 0.0469(3) 0.0256(5) Uani 1 1 d . . . H6' H 0.7523 0.0375 -0.0513 0.031 Uiso 1 1 calc R . . N10 N 0.0594(3) 0.7257(3) 0.2093(3) 0.0277(5) Uani 1 1 d . . . O11 O 0.2331(3) 0.8040(3) 0.2759(3) 0.0430(5) Uani 1 1 d . . . O12 O -0.0347(3) 0.7096(3) 0.2859(3) 0.0473(6) Uani 1 1 d . . . O13 O -0.0190(3) 0.6642(3) 0.0633(2) 0.0495(6) 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 0.03874(13) 0.03768(12) 0.02309(11) 0.01680(8) 0.01416(9) 0.02615(9) N1 0.0242(10) 0.0217(10) 0.0184(9) 0.0088(8) 0.0089(8) 0.0125(8) N2 0.0274(10) 0.0265(10) 0.0165(9) 0.0088(8) 0.0075(8) 0.0146(9) N3 0.0271(10) 0.0257(10) 0.0182(9) 0.0087(8) 0.0097(8) 0.0151(8) C3A 0.0212(11) 0.0225(11) 0.0188(11) 0.0086(9) 0.0092(9) 0.0081(9) C4 0.0279(13) 0.0217(11) 0.0284(13) 0.0076(10) 0.0158(11) 0.0087(10) C5 0.0274(13) 0.0267(13) 0.0239(12) 0.0010(10) 0.0129(11) 0.0027(10) C6 0.0223(12) 0.0342(14) 0.0167(11) 0.0064(10) 0.0051(10) 0.0014(10) C7 0.0199(11) 0.0272(12) 0.0199(11) 0.0104(9) 0.0074(9) 0.0061(9) C7A 0.0184(11) 0.0211(11) 0.0180(11) 0.0070(9) 0.0083(9) 0.0056(9) N1' 0.0211(9) 0.0203(9) 0.0181(9) 0.0058(8) 0.0053(8) 0.0093(8) C2' 0.0191(11) 0.0177(10) 0.0228(11) 0.0058(9) 0.0067(9) 0.0083(9) C3' 0.0258(12) 0.0278(12) 0.0264(12) 0.0144(10) 0.0117(10) 0.0116(10) C4' 0.0287(13) 0.0248(12) 0.0364(14) 0.0168(11) 0.0119(11) 0.0109(10) C5' 0.0250(12) 0.0198(12) 0.0350(14) 0.0043(10) 0.0075(11) 0.0099(10) C6' 0.0240(12) 0.0226(12) 0.0237(12) 0.0027(10) 0.0063(10) 0.0088(10) N10 0.0349(12) 0.0306(11) 0.0316(12) 0.0179(9) 0.0179(10) 0.0219(10) O11 0.0313(11) 0.0524(13) 0.0454(12) 0.0198(10) 0.0138(10) 0.0172(10) O12 0.0502(13) 0.0793(16) 0.0497(13) 0.0447(12) 0.0357(11) 0.0421(12) O13 0.0539(14) 0.0526(13) 0.0292(11) 0.0091(10) 0.0168(10) 0.0085(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 N3 2.240(2) . ? Ag1 N1' 2.273(2) 2_665 ? Ag1 O13 2.590(2) 2_565 ? N1 N2 1.358(3) . ? N1 C7A 1.381(3) . ? N1 C2' 1.438(3) . ? N2 N3 1.306(3) . ? N3 C3A 1.379(3) . ? C3A C7A 1.401(3) . ? C3A C4 1.412(3) . ? C4 C5 1.370(4) . ? C5 C6 1.417(4) . ? C6 C7 1.382(3) . ? C7 C7A 1.396(3) . ? N1' C2' 1.335(3) . ? N1' C6' 1.353(3) . ? N1' Ag1 2.273(2) 2_665 ? C2' C3' 1.379(3) . ? C3' C4' 1.394(4) . ? C4' C5' 1.387(4) . ? C5' C6' 1.378(4) . ? N10 O12 1.241(3) . ? N10 O13 1.251(3) . ? N10 O11 1.257(3) . ? O13 Ag1 2.590(2) 2_565 ? 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 N3 Ag1 N1' 143.18(7) . 2_665 ? N3 Ag1 O13 98.34(8) . 2_565 ? N1' Ag1 O13 113.97(7) 2_665 2_565 ? N2 N1 C7A 110.19(18) . . ? N2 N1 C2' 118.73(18) . . ? C7A N1 C2' 131.1(2) . . ? N3 N2 N1 108.54(17) . . ? N2 N3 C3A 109.20(19) . . ? N2 N3 Ag1 115.46(14) . . ? C3A N3 Ag1 135.27(16) . . ? N3 C3A C7A 108.13(19) . . ? N3 C3A C4 130.4(2) . . ? C7A C3A C4 121.4(2) . . ? C5 C4 C3A 116.2(2) . . ? C4 C5 C6 122.0(2) . . ? C7 C6 C5 122.3(2) . . ? C6 C7 C7A 115.7(2) . . ? N1 C7A C7 133.8(2) . . ? N1 C7A C3A 103.95(19) . . ? C7 C7A C3A 122.3(2) . . ? C2' N1' C6' 116.9(2) . . ? C2' N1' Ag1 123.81(15) . 2_665 ? C6' N1' Ag1 119.18(16) . 2_665 ? N1' C2' C3' 124.3(2) . . ? N1' C2' N1 115.0(2) . . ? C3' C2' N1 120.8(2) . . ? C2' C3' C4' 117.5(2) . . ? C5' C4' C3' 119.6(2) . . ? C6' C5' C4' 118.2(2) . . ? N1' C6' C5' 123.4(2) . . ? O12 N10 O13 119.8(2) . . ? O12 N10 O11 121.1(2) . . ? O13 N10 O11 119.0(2) . . ? N10 O13 Ag1 115.27(17) . 2_565 ? 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 C7A N1 N2 N3 0.1(3) . . . . ? C2' N1 N2 N3 179.02(19) . . . . ? N1 N2 N3 C3A 0.1(3) . . . . ? N1 N2 N3 Ag1 -177.24(14) . . . . ? N1' Ag1 N3 N2 -94.03(19) 2_665 . . . ? O13 Ag1 N3 N2 57.74(17) 2_565 . . . ? N1' Ag1 N3 C3A 89.6(2) 2_665 . . . ? O13 Ag1 N3 C3A -118.7(2) 2_565 . . . ? N2 N3 C3A C7A -0.2(3) . . . . ? Ag1 N3 C3A C7A 176.36(16) . . . . ? N2 N3 C3A C4 179.9(2) . . . . ? Ag1 N3 C3A C4 -3.5(4) . . . . ? N3 C3A C4 C5 179.0(2) . . . . ? C7A C3A C4 C5 -0.8(3) . . . . ? C3A C4 C5 C6 -0.3(4) . . . . ? C4 C5 C6 C7 1.9(4) . . . . ? C5 C6 C7 C7A -2.1(4) . . . . ? N2 N1 C7A C7 179.3(2) . . . . ? C2' N1 C7A C7 0.6(4) . . . . ? N2 N1 C7A C3A -0.2(2) . . . . ? C2' N1 C7A C3A -179.0(2) . . . . ? C6 C7 C7A N1 -178.5(2) . . . . ? C6 C7 C7A C3A 1.0(3) . . . . ? N3 C3A C7A N1 0.2(2) . . . . ? C4 C3A C7A N1 -179.9(2) . . . . ? N3 C3A C7A C7 -179.4(2) . . . . ? C4 C3A C7A C7 0.5(4) . . . . ? C6' N1' C2' C3' 2.2(3) . . . . ? Ag1 N1' C2' C3' -174.50(18) 2_665 . . . ? C6' N1' C2' N1 -177.2(2) . . . . ? Ag1 N1' C2' N1 6.0(3) 2_665 . . . ? N2 N1 C2' N1' 35.0(3) . . . . ? C7A N1 C2' N1' -146.3(2) . . . . ? N2 N1 C2' C3' -144.5(2) . . . . ? C7A N1 C2' C3' 34.2(4) . . . . ? N1' C2' C3' C4' 0.2(4) . . . . ? N1 C2' C3' C4' 179.6(2) . . . . ? C2' C3' C4' C5' -2.7(4) . . . . ? C3' C4' C5' C6' 2.6(4) . . . . ? C2' N1' C6' C5' -2.3(3) . . . . ? Ag1 N1' C6' C5' 174.59(19) 2_665 . . . ? C4' C5' C6' N1' -0.1(4) . . . . ? O12 N10 O13 Ag1 -35.5(3) . . . 2_565 ? O11 N10 O13 Ag1 145.00(19) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.335 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.079 #===END data_3cr7(complex22) _database_code_CSD 190046 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H20 Ag2 N10 O6' _chemical_formula_weight 760.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.252(2) _cell_length_b 11.020(2) _cell_length_c 14.709(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.98(1) _cell_angle_gamma 90.00 _cell_volume 2614.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 4.64 _cell_measurement_theta_max 17.95 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.560 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5385 _exptl_absorpt_correction_T_max 0.6331 _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.35 _diffrn_reflns_number 2963 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2865 _reflns_number_observed 2365 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2865 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 Ag1 Ag 0.359506(12) 0.607172(17) -0.033704(13) 0.02651(7) Uani 1 1 d . . . N1 N 0.34676(12) 0.98131(18) 0.04337(14) 0.0209(4) Uani 1 1 d . . . N2 N 0.31578(13) 0.87539(18) 0.00900(15) 0.0227(4) Uani 1 1 d . . . N3 N 0.37362(13) 0.79294(19) 0.02479(15) 0.0242(5) Uani 1 1 d . . . C3A C 0.44374(16) 0.8459(2) 0.07031(16) 0.0216(5) Uani 1 1 d . . . C4 C 0.52211(16) 0.7976(2) 0.10085(18) 0.0274(6) Uani 1 1 d . . . H4 H 0.5345 0.7142 0.0933 0.033 Uiso 1 1 calc R . . C5 C 0.57992(17) 0.8771(3) 0.14214(19) 0.0320(6) Uani 1 1 d . . . H5 H 0.6335 0.8478 0.1646 0.038 Uiso 1 1 calc R . . C6 C 0.56180(16) 1.0014(3) 0.15217(18) 0.0297(6) Uani 1 1 d . . . H6 H 0.6041 1.0533 0.1802 0.036 Uiso 1 1 calc R . . C7 C 0.48556(17) 1.0499(2) 0.12304(17) 0.0255(5) Uani 1 1 d . . . H7 H 0.4735 1.1335 0.1300 0.031 Uiso 1 1 calc R . . C7A C 0.42694(15) 0.9680(2) 0.08247(16) 0.0202(5) Uani 1 1 d . . . C1' C 0.29430(16) 1.0893(2) 0.04078(18) 0.0245(5) Uani 1 1 d . . . H1'1 H 0.2501 1.0834 -0.0117 0.029 Uiso 1 1 calc R . . H1'2 H 0.3281 1.1621 0.0317 0.029 Uiso 1 1 calc R . . N1' N 0.19251(13) 1.02640(19) 0.13906(14) 0.0234(4) Uani 1 1 d . . . C2' C 0.25538(15) 1.1028(2) 0.12847(17) 0.0211(5) Uani 1 1 d . . . C3' C 0.28395(16) 1.1880(2) 0.19410(18) 0.0268(5) Uani 1 1 d . . . H3' H 0.3279 1.2414 0.1844 0.032 Uiso 1 1 calc R . . C4' C 0.24717(17) 1.1938(2) 0.27431(17) 0.0302(6) Uani 1 1 d . . . H4' H 0.2660 1.2508 0.3207 0.036 Uiso 1 1 calc R . . C5' C 0.18332(19) 1.1162(2) 0.28577(18) 0.0324(6) Uani 1 1 d . . . H5' H 0.1573 1.1188 0.3402 0.039 Uiso 1 1 calc R . . C6' C 0.15712(17) 1.0337(2) 0.21679(18) 0.0293(6) Uani 1 1 d . . . H6' H 0.1126 0.9805 0.2249 0.035 Uiso 1 1 calc R . . N10 N 0.45418(14) 0.41087(19) 0.09664(16) 0.0261(5) Uani 1 1 d . . . O11 O 0.46565(14) 0.52163(17) 0.08943(16) 0.0436(5) Uani 1 1 d . . . O12 O 0.38451(13) 0.3675(2) 0.07113(18) 0.0477(6) Uani 1 1 d . . . O13 O 0.51238(13) 0.34364(19) 0.12800(16) 0.0411(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 0.03190(12) 0.02092(11) 0.02646(11) -0.00613(8) 0.00245(7) -0.00363(9) N1 0.0221(10) 0.0179(10) 0.0232(10) -0.0021(8) 0.0045(8) -0.0027(8) N2 0.0207(10) 0.0225(11) 0.0248(11) -0.0035(9) 0.0026(8) -0.0030(8) N3 0.0249(11) 0.0208(11) 0.0266(11) -0.0023(9) 0.0017(9) -0.0023(8) C3A 0.0254(13) 0.0203(11) 0.0193(12) 0.0003(9) 0.0034(10) -0.0042(10) C4 0.0284(13) 0.0231(13) 0.0302(14) 0.0036(11) 0.0008(11) 0.0005(11) C5 0.0235(13) 0.0385(16) 0.0326(14) 0.0046(12) -0.0023(11) -0.0009(12) C6 0.0279(14) 0.0335(14) 0.0265(13) -0.0019(11) -0.0019(11) -0.0109(12) C7 0.0313(14) 0.0232(12) 0.0225(12) -0.0040(10) 0.0046(10) -0.0089(11) C7A 0.0218(12) 0.0227(12) 0.0167(11) 0.0004(9) 0.0044(9) -0.0027(10) C1' 0.0267(13) 0.0188(12) 0.0289(13) 0.0020(10) 0.0074(10) 0.0030(10) N1' 0.0275(11) 0.0210(10) 0.0217(10) -0.0026(8) 0.0028(9) 0.0007(9) C2' 0.0222(11) 0.0169(11) 0.0239(12) 0.0004(10) 0.0014(9) 0.0045(10) C3' 0.0286(13) 0.0194(12) 0.0309(14) -0.0026(11) -0.0020(11) 0.0001(11) C4' 0.0373(15) 0.0262(13) 0.0251(13) -0.0077(11) -0.0040(11) 0.0034(12) C5' 0.0415(16) 0.0351(15) 0.0212(12) -0.0045(12) 0.0060(11) 0.0031(13) C6' 0.0345(15) 0.0280(14) 0.0262(13) -0.0021(11) 0.0070(11) -0.0030(12) N10 0.0284(12) 0.0216(11) 0.0291(11) -0.0003(9) 0.0061(9) 0.0001(9) O11 0.0483(13) 0.0197(10) 0.0599(14) 0.0051(10) -0.0051(11) -0.0031(9) O12 0.0318(12) 0.0444(13) 0.0648(16) 0.0021(11) -0.0024(11) -0.0125(10) O13 0.0398(12) 0.0259(10) 0.0560(14) 0.0060(10) -0.0016(10) 0.0047(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.222(2) . ? Ag1 N1' 2.228(2) 7_565 ? Ag1 O11 2.527(2) . ? N1 N2 1.345(3) . ? N1 C7A 1.367(3) . ? N1 C1' 1.462(3) . ? N2 N3 1.308(3) . ? N3 C3A 1.379(3) . ? C3A C7A 1.389(3) . ? C3A C4 1.403(4) . ? C4 C5 1.371(4) . ? C5 C6 1.413(4) . ? C6 C7 1.369(4) . ? C7 C7A 1.393(3) . ? C1' C2' 1.511(3) . ? N1' C6' 1.343(3) . ? N1' C2' 1.348(3) . ? N1' Ag1 2.228(2) 7_565 ? C2' C3' 1.385(3) . ? C3' C4' 1.387(4) . ? C4' C5' 1.371(4) . ? C5' C6' 1.390(4) . ? N10 O11 1.241(3) . ? N10 O12 1.244(3) . ? N10 O13 1.245(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 N3 Ag1 N1' 152.96(8) . 7_565 ? N3 Ag1 O11 92.11(7) . . ? N1' Ag1 O11 114.86(7) 7_565 . ? N2 N1 C7A 111.03(19) . . ? N2 N1 C1' 120.4(2) . . ? C7A N1 C1' 128.4(2) . . ? N3 N2 N1 107.93(19) . . ? N2 N3 C3A 109.0(2) . . ? N2 N3 Ag1 122.22(16) . . ? C3A N3 Ag1 128.19(16) . . ? N3 C3A C7A 108.0(2) . . ? N3 C3A C4 131.2(2) . . ? C7A C3A C4 120.8(2) . . ? C5 C4 C3A 116.5(2) . . ? C4 C5 C6 121.7(3) . . ? C7 C6 C5 122.5(2) . . ? C6 C7 C7A 115.3(2) . . ? N1 C7A C3A 104.0(2) . . ? N1 C7A C7 132.7(2) . . ? C3A C7A C7 123.2(2) . . ? N1 C1' C2' 111.2(2) . . ? C6' N1' C2' 118.0(2) . . ? C6' N1' Ag1 117.77(17) . 7_565 ? C2' N1' Ag1 124.15(16) . 7_565 ? N1' C2' C3' 122.5(2) . . ? N1' C2' C1' 116.0(2) . . ? C3' C2' C1' 121.4(2) . . ? C2' C3' C4' 118.8(2) . . ? C5' C4' C3' 119.1(2) . . ? C4' C5' C6' 119.2(2) . . ? N1' C6' C5' 122.4(3) . . ? O11 N10 O12 119.5(2) . . ? O11 N10 O13 120.1(2) . . ? O12 N10 O13 120.4(2) . . ? N10 O11 Ag1 109.37(17) . . ? 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 C7A N1 N2 N3 0.1(3) . . . . ? C1' N1 N2 N3 -176.3(2) . . . . ? N1 N2 N3 C3A 0.0(3) . . . . ? N1 N2 N3 Ag1 -172.08(14) . . . . ? N1' Ag1 N3 N2 26.8(3) 7_565 . . . ? O11 Ag1 N3 N2 -157.36(19) . . . . ? N1' Ag1 N3 C3A -143.7(2) 7_565 . . . ? O11 Ag1 N3 C3A 32.2(2) . . . . ? N2 N3 C3A C7A -0.1(3) . . . . ? Ag1 N3 C3A C7A 171.35(16) . . . . ? N2 N3 C3A C4 -178.7(3) . . . . ? Ag1 N3 C3A C4 -7.2(4) . . . . ? N3 C3A C4 C5 178.1(3) . . . . ? C7A C3A C4 C5 -0.3(4) . . . . ? C3A C4 C5 C6 -0.9(4) . . . . ? C4 C5 C6 C7 1.2(4) . . . . ? C5 C6 C7 C7A -0.2(4) . . . . ? N2 N1 C7A C3A -0.2(3) . . . . ? C1' N1 C7A C3A 175.9(2) . . . . ? N2 N1 C7A C7 177.0(3) . . . . ? C1' N1 C7A C7 -6.9(4) . . . . ? N3 C3A C7A N1 0.2(3) . . . . ? C4 C3A C7A N1 178.9(2) . . . . ? N3 C3A C7A C7 -177.4(2) . . . . ? C4 C3A C7A C7 1.4(4) . . . . ? C6 C7 C7A N1 -177.9(3) . . . . ? C6 C7 C7A C3A -1.1(4) . . . . ? N2 N1 C1' C2' 93.3(3) . . . . ? C7A N1 C1' C2' -82.4(3) . . . . ? C6' N1' C2' C3' -0.4(4) . . . . ? Ag1 N1' C2' C3' 177.40(18) 7_565 . . . ? C6' N1' C2' C1' 178.8(2) . . . . ? Ag1 N1' C2' C1' -3.4(3) 7_565 . . . ? N1 C1' C2' N1' -74.6(3) . . . . ? N1 C1' C2' C3' 104.6(3) . . . . ? N1' C2' C3' C4' 0.9(4) . . . . ? C1' C2' C3' C4' -178.3(2) . . . . ? C2' C3' C4' C5' -0.7(4) . . . . ? C3' C4' C5' C6' 0.1(4) . . . . ? C2' N1' C6' C5' -0.3(4) . . . . ? Ag1 N1' C6' C5' -178.2(2) 7_565 . . . ? C4' C5' C6' N1' 0.4(4) . . . . ? O12 N10 O11 Ag1 -23.5(3) . . . . ? O13 N10 O11 Ag1 155.5(2) . . . . ? N3 Ag1 O11 N10 157.40(19) . . . . ? N1' Ag1 O11 N10 -24.7(2) 7_565 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.512 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.088 #===END