Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'A. Amoroso' _publ_contact_author_address ; Department of Chemistry Cardiff University of Wales Main Building Park Place Cardiff CF1 3TB UNITED KINGDOM ; _publ_contact_author_email AMOROSOAJ@CF.AC.UK _publ_section_title ; The Synthesis and Structure of Terpyridine-N-Oxide Complexes of Cu(II)Perchlorate ; loop_ _publ_author_name 'A. Amoroso' 'Miles W. Burrows' 'Simon Coles' 'Robert D. Farley' 'Robert Haigh' 'M. Hursthouse' ; M.Jones ; 'K. M. Abdul Malik' 'Damien M. Murphy' data_1 _database_code_depnum_ccdc_archive 'CCDC 659290' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H26 Cl2 Cu N6 O11' _chemical_formula_weight 793.02 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 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 6.9303(2) _cell_length_b 12.0952(3) _cell_length_c 38.2470(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.4265(9) _cell_angle_gamma 90.00 _cell_volume 3203.12(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod-like _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7694 _exptl_absorpt_correction_T_max 0.9299 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 14163 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.1226 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.02 _reflns_number_total 5879 _reflns_number_gt 3837 _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. ; _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^)+(0.0261P)^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 SHELXL _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5879 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 0.48621(6) 0.22352(4) 0.122202(11) 0.01748(15) Uani 1 1 d . . . O1 O 0.2105(3) 0.28993(19) 0.11383(6) 0.0240(6) Uani 1 1 d . . . O2 O 0.3508(3) 0.10752(19) 0.08316(6) 0.0254(6) Uani 1 1 d . . . N1 N 0.1517(4) 0.3474(2) 0.14125(8) 0.0213(7) Uani 1 1 d . . . N2 N 0.3747(4) 0.1518(2) 0.16348(7) 0.0153(7) Uani 1 1 d . . . N3 N 0.6969(4) 0.1076(2) 0.13296(7) 0.0180(7) Uani 1 1 d . . . N4 N 0.4838(4) 0.0585(2) 0.06443(7) 0.0199(7) Uani 1 1 d . . . N5 N 0.5836(4) 0.2936(2) 0.07792(7) 0.0147(7) Uani 1 1 d . . . N6 N 0.5810(4) 0.3812(2) 0.14168(7) 0.0209(7) Uani 1 1 d . . . C1 C 0.0986(5) 0.4546(3) 0.13596(10) 0.0222(9) Uani 1 1 d . . . H1 H 0.1044 0.4855 0.1132 0.027 Uiso 1 1 calc R . . C2 C 0.0372(5) 0.5184(3) 0.16270(10) 0.0239(9) Uani 1 1 d . . . H2 H 0.0008 0.5932 0.1586 0.029 Uiso 1 1 calc R . . C3 C 0.0285(5) 0.4728(3) 0.19608(10) 0.0256(9) Uani 1 1 d . . . H3 H -0.0133 0.5159 0.2151 0.031 Uiso 1 1 calc R . . C4 C 0.0818(4) 0.3635(3) 0.20091(9) 0.0213(9) Uani 1 1 d . . . H4 H 0.0741 0.3313 0.2235 0.026 Uiso 1 1 calc R . . C5 C 0.1459(5) 0.3003(3) 0.17380(9) 0.0176(8) Uani 1 1 d . . . C6 C 0.2143(5) 0.1857(3) 0.17959(9) 0.0174(8) Uani 1 1 d . . . C7 C 0.1243(5) 0.1187(3) 0.20323(9) 0.0200(8) Uani 1 1 d . . . H7 H 0.0110 0.1431 0.2141 0.024 Uiso 1 1 calc R . . C8 C 0.2018(5) 0.0150(3) 0.21096(9) 0.0279(10) Uani 1 1 d . . . H8 H 0.1400 -0.0329 0.2267 0.033 Uiso 1 1 calc R . . C9 C 0.3689(5) -0.0178(3) 0.19561(9) 0.0214(9) Uani 1 1 d . . . H9 H 0.4263 -0.0871 0.2013 0.026 Uiso 1 1 calc R . . C10 C 0.4523(5) 0.0521(3) 0.17163(9) 0.0167(8) Uani 1 1 d . . . C11 C 0.6350(5) 0.0267(3) 0.15403(8) 0.0175(8) Uani 1 1 d . . . C12 C 0.7335(5) -0.0717(3) 0.15875(9) 0.0211(9) Uani 1 1 d . . . H12 H 0.6864 -0.1276 0.1736 0.025 Uiso 1 1 calc R . . C13 C 0.9031(5) -0.0872(3) 0.14132(9) 0.0263(9) Uani 1 1 d . . . H13 H 0.9728 -0.1546 0.1437 0.032 Uiso 1 1 calc R . . C14 C 0.9692(5) -0.0031(3) 0.12047(9) 0.0245(9) Uani 1 1 d . . . H14 H 1.0864 -0.0116 0.1088 0.029 Uiso 1 1 calc R . . C15 C 0.8640(5) 0.0924(3) 0.11684(9) 0.0225(9) Uani 1 1 d . . . H15 H 0.9104 0.1498 0.1025 0.027 Uiso 1 1 calc R . . C16 C 0.4924(5) -0.0535(3) 0.06477(9) 0.0235(9) Uani 1 1 d . . . H16 H 0.4059 -0.0942 0.0785 0.028 Uiso 1 1 calc R . . C17 C 0.6236(5) -0.1084(3) 0.04568(10) 0.0275(10) Uani 1 1 d . . . H17 H 0.6305 -0.1868 0.0467 0.033 Uiso 1 1 calc R . . C18 C 0.7462(5) -0.0510(3) 0.02484(9) 0.0247(9) Uani 1 1 d . . . H18 H 0.8344 -0.0887 0.0107 0.030 Uiso 1 1 calc R . . C19 C 0.7374(5) 0.0629(3) 0.02509(9) 0.0212(9) Uani 1 1 d . . . H19 H 0.8215 0.1038 0.0110 0.025 Uiso 1 1 calc R . . C20 C 0.6090(5) 0.1192(3) 0.04538(9) 0.0173(8) Uani 1 1 d . . . C21 C 0.6085(4) 0.2416(3) 0.04714(9) 0.0160(8) Uani 1 1 d . . . C22 C 0.6519(5) 0.3010(3) 0.01734(9) 0.0197(9) Uani 1 1 d . . . H22 H 0.6668 0.2638 -0.0043 0.024 Uiso 1 1 calc R . . C23 C 0.6732(4) 0.4149(3) 0.01932(9) 0.0211(9) Uani 1 1 d . . . H23 H 0.7025 0.4564 -0.0009 0.025 Uiso 1 1 calc R . . C24 C 0.6514(4) 0.4671(3) 0.05086(9) 0.0202(9) Uani 1 1 d . . . H24 H 0.6671 0.5450 0.0527 0.024 Uiso 1 1 calc R . . C25 C 0.6065(4) 0.4053(3) 0.07993(9) 0.0169(8) Uani 1 1 d . . . C26 C 0.5842(4) 0.4552(3) 0.11511(9) 0.0163(8) Uani 1 1 d . . . C27 C 0.5694(5) 0.5681(3) 0.12057(9) 0.0213(9) Uani 1 1 d . . . H27 H 0.5733 0.6186 0.1016 0.026 Uiso 1 1 calc R . . C28 C 0.5487(4) 0.6054(3) 0.15463(10) 0.0270(10) Uani 1 1 d . . . H28 H 0.5338 0.6821 0.1591 0.032 Uiso 1 1 calc R . . C29 C 0.5498(5) 0.5309(3) 0.18185(10) 0.0262(9) Uani 1 1 d . . . H29 H 0.5405 0.5552 0.2053 0.031 Uiso 1 1 calc R . . C30 C 0.5649(5) 0.4200(3) 0.17407(10) 0.0256(9) Uani 1 1 d . . . H30 H 0.5638 0.3684 0.1928 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.88104(13) 0.29056(8) -0.07539(2) 0.0247(2) Uani 1 1 d . . . O3 O 0.8953(4) 0.2059(2) -0.04909(7) 0.0358(7) Uani 1 1 d . . . O4 O 0.7707(4) 0.2493(2) -0.10513(7) 0.0358(7) Uani 1 1 d . . . O5 O 1.0702(4) 0.3216(2) -0.08566(8) 0.0516(9) Uani 1 1 d . . . O6 O 0.7847(4) 0.3858(2) -0.06143(7) 0.0446(8) Uani 1 1 d . . . Cl2 Cl 0.81493(14) -0.23687(8) 0.23820(2) 0.0312(3) Uani 1 1 d . . . O7 O 0.8412(4) -0.1218(2) 0.24598(7) 0.0507(8) Uani 1 1 d . . . O8 O 0.8455(4) -0.3045(3) 0.26823(8) 0.0580(10) Uani 1 1 d . . . O9 O 0.6101(4) -0.2479(2) 0.22697(7) 0.0443(8) Uani 1 1 d . . . O10 O 0.9236(4) -0.2705(2) 0.20944(8) 0.0508(8) Uani 1 1 d . . . O11 O 0.0958(4) 0.2248(2) 0.03614(7) 0.0383(7) Uani 1 1 d . . . H11 H 0.1919 0.2128 0.0565 0.050 Uiso 1 1 d . . . C31 C 0.1370(5) 0.3356(3) 0.02749(11) 0.0421(12) Uani 1 1 d . . . H31A H 0.0951 0.3845 0.0461 0.063 Uiso 1 1 calc R . . H31B H 0.0682 0.3551 0.0054 0.063 Uiso 1 1 calc R . . H31C H 0.2763 0.3442 0.0249 0.063 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 0.0201(2) 0.0162(3) 0.0165(3) 0.0002(2) 0.00366(18) 0.0006(2) O1 0.0377(15) 0.0211(15) 0.0135(14) -0.0019(12) 0.0060(11) 0.0073(12) O2 0.0258(14) 0.0188(15) 0.0329(16) -0.0043(12) 0.0172(12) 0.0033(12) N1 0.0221(16) 0.0199(19) 0.0222(18) -0.0006(15) 0.0045(13) 0.0022(15) N2 0.0180(15) 0.0160(17) 0.0120(16) -0.0010(13) 0.0022(12) -0.0022(14) N3 0.0228(16) 0.0142(17) 0.0176(17) 0.0018(14) 0.0061(13) -0.0031(14) N4 0.0216(16) 0.0176(18) 0.0207(17) -0.0023(15) 0.0032(13) 0.0008(15) N5 0.0147(14) 0.0156(17) 0.0140(16) 0.0002(13) 0.0024(12) 0.0007(13) N6 0.0267(16) 0.0194(18) 0.0170(17) 0.0031(15) 0.0056(13) -0.0021(14) C1 0.023(2) 0.019(2) 0.025(2) 0.0078(18) 0.0024(16) 0.0015(18) C2 0.0201(19) 0.017(2) 0.035(2) -0.0007(19) 0.0031(17) 0.0032(17) C3 0.025(2) 0.025(2) 0.027(2) -0.0084(19) 0.0058(17) 0.0035(19) C4 0.0209(19) 0.024(2) 0.019(2) 0.0013(18) 0.0066(16) 0.0044(18) C5 0.0157(18) 0.016(2) 0.022(2) 0.0003(17) 0.0067(15) 0.0019(16) C6 0.0207(19) 0.017(2) 0.015(2) 0.0000(17) 0.0023(15) -0.0014(17) C7 0.0207(19) 0.019(2) 0.021(2) -0.0018(18) 0.0091(16) 0.0016(18) C8 0.031(2) 0.029(3) 0.025(2) 0.0056(19) 0.0091(17) -0.005(2) C9 0.025(2) 0.018(2) 0.022(2) 0.0054(18) 0.0055(16) 0.0058(18) C10 0.0180(18) 0.017(2) 0.015(2) -0.0022(16) 0.0014(15) 0.0029(17) C11 0.0205(19) 0.017(2) 0.015(2) -0.0023(17) 0.0033(15) -0.0033(17) C12 0.026(2) 0.017(2) 0.021(2) -0.0001(17) 0.0038(16) -0.0001(18) C13 0.030(2) 0.023(2) 0.025(2) -0.0019(19) 0.0013(18) 0.0072(19) C14 0.0176(19) 0.034(3) 0.022(2) -0.002(2) 0.0058(16) 0.0038(19) C15 0.025(2) 0.023(2) 0.020(2) 0.0014(18) 0.0041(17) -0.0059(18) C16 0.025(2) 0.017(2) 0.029(2) 0.0011(19) 0.0063(17) -0.0027(18) C17 0.030(2) 0.016(2) 0.036(3) -0.0027(19) -0.0036(19) 0.0016(19) C18 0.025(2) 0.026(2) 0.023(2) -0.0051(19) 0.0000(17) 0.0022(19) C19 0.0191(19) 0.027(2) 0.018(2) -0.0025(18) 0.0050(15) 0.0006(18) C20 0.0185(18) 0.019(2) 0.014(2) 0.0017(17) 0.0008(15) -0.0037(17) C21 0.0130(17) 0.016(2) 0.019(2) -0.0022(17) 0.0019(14) 0.0049(16) C22 0.0219(19) 0.024(2) 0.013(2) 0.0012(17) 0.0018(15) 0.0006(18) C23 0.0202(19) 0.024(2) 0.019(2) 0.0056(18) 0.0047(16) 0.0015(18) C24 0.0195(19) 0.018(2) 0.024(2) 0.0035(18) 0.0049(16) -0.0016(17) C25 0.0104(17) 0.017(2) 0.024(2) 0.0043(17) 0.0021(15) 0.0001(16) C26 0.0144(18) 0.016(2) 0.019(2) -0.0007(17) 0.0016(15) -0.0010(16) C27 0.0236(19) 0.017(2) 0.023(2) 0.0006(18) 0.0011(16) -0.0024(18) C28 0.021(2) 0.019(2) 0.041(3) -0.011(2) 0.0033(18) -0.0015(18) C29 0.028(2) 0.032(3) 0.019(2) -0.0056(19) 0.0009(17) -0.004(2) C30 0.027(2) 0.027(2) 0.023(2) 0.0023(19) 0.0013(17) -0.0011(19) Cl1 0.0298(5) 0.0238(6) 0.0207(5) 0.0021(4) 0.0051(4) 0.0018(5) O3 0.0447(16) 0.0298(18) 0.0332(17) 0.0143(14) 0.0061(13) 0.0085(14) O4 0.0415(16) 0.0387(19) 0.0265(16) -0.0070(14) -0.0057(12) 0.0082(14) O5 0.0383(17) 0.055(2) 0.063(2) 0.0033(17) 0.0165(15) -0.0210(16) O6 0.074(2) 0.0312(18) 0.0288(17) -0.0050(14) 0.0084(14) 0.0241(16) Cl2 0.0485(6) 0.0259(6) 0.0196(5) 0.0016(5) 0.0039(5) -0.0081(5) O7 0.083(2) 0.036(2) 0.0345(19) -0.0036(15) 0.0137(16) -0.0125(17) O8 0.064(2) 0.065(2) 0.044(2) 0.0361(18) -0.0016(16) 0.0078(18) O9 0.0369(16) 0.056(2) 0.0395(19) -0.0007(16) -0.0014(14) 0.0004(15) O10 0.0582(19) 0.041(2) 0.055(2) 0.0037(16) 0.0297(16) 0.0203(16) O11 0.0436(17) 0.0303(18) 0.0396(18) -0.0014(14) -0.0131(14) -0.0038(14) C31 0.031(2) 0.044(3) 0.051(3) 0.002(2) -0.009(2) 0.003(2) _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 N2 1.987(3) . ? Cu1 N5 2.034(3) . ? Cu1 N3 2.054(3) . ? Cu1 O1 2.085(2) . ? Cu1 N6 2.141(3) . ? Cu1 O2 2.227(2) . ? O1 N1 1.336(3) . ? O2 N4 1.331(3) . ? N1 C1 1.360(4) . ? N1 C5 1.371(4) . ? N2 C10 1.351(4) . ? N2 C6 1.357(4) . ? N3 C15 1.347(4) . ? N3 C11 1.349(4) . ? N4 C16 1.356(4) . ? N4 C20 1.370(4) . ? N5 C21 1.352(4) . ? N5 C25 1.363(4) . ? N6 C30 1.334(4) . ? N6 C26 1.355(4) . ? C1 C2 1.364(5) . ? C2 C3 1.394(5) . ? C3 C4 1.383(5) . ? C4 C5 1.377(5) . ? C5 C6 1.479(5) . ? C6 C7 1.383(5) . ? C7 C8 1.391(5) . ? C8 C9 1.379(5) . ? C9 C10 1.391(5) . ? C10 C11 1.491(4) . ? C11 C12 1.380(5) . ? C12 C13 1.388(5) . ? C13 C14 1.382(5) . ? C14 C15 1.370(5) . ? C16 C17 1.363(5) . ? C17 C18 1.378(5) . ? C18 C19 1.379(5) . ? C19 C20 1.384(5) . ? C20 C21 1.481(5) . ? C21 C22 1.391(5) . ? C22 C23 1.387(5) . ? C23 C24 1.376(4) . ? C24 C25 1.386(4) . ? C25 C26 1.488(4) . ? C26 C27 1.386(5) . ? C27 C28 1.392(5) . ? C28 C29 1.377(5) . ? C29 C30 1.379(5) . ? Cl1 O4 1.433(2) . ? Cl1 O5 1.434(3) . ? Cl1 O3 1.436(3) . ? Cl1 O6 1.445(3) . ? Cl2 O8 1.419(3) . ? Cl2 O10 1.419(3) . ? Cl2 O7 1.433(3) . ? Cl2 O9 1.472(3) . ? O11 C31 1.413(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 N2 Cu1 N5 175.98(10) . . ? N2 Cu1 N3 80.77(11) . . ? N5 Cu1 N3 101.12(11) . . ? N2 Cu1 O1 84.58(10) . . ? N5 Cu1 O1 92.64(10) . . ? N3 Cu1 O1 158.92(10) . . ? N2 Cu1 N6 103.69(11) . . ? N5 Cu1 N6 79.10(11) . . ? N3 Cu1 N6 109.50(10) . . ? O1 Cu1 N6 88.61(10) . . ? N2 Cu1 O2 95.19(10) . . ? N5 Cu1 O2 81.35(10) . . ? N3 Cu1 O2 88.85(10) . . ? O1 Cu1 O2 77.42(9) . . ? N6 Cu1 O2 155.35(10) . . ? N1 O1 Cu1 112.83(18) . . ? N4 O2 Cu1 111.08(17) . . ? O1 N1 C1 117.9(3) . . ? O1 N1 C5 121.2(3) . . ? C1 N1 C5 120.8(3) . . ? C10 N2 C6 119.4(3) . . ? C10 N2 Cu1 114.1(2) . . ? C6 N2 Cu1 125.6(2) . . ? C15 N3 C11 118.4(3) . . ? C15 N3 Cu1 128.2(2) . . ? C11 N3 Cu1 111.9(2) . . ? O2 N4 C16 118.1(3) . . ? O2 N4 C20 121.1(3) . . ? C16 N4 C20 120.8(3) . . ? C21 N5 C25 119.4(3) . . ? C21 N5 Cu1 126.2(2) . . ? C25 N5 Cu1 114.1(2) . . ? C30 N6 C26 118.0(3) . . ? C30 N6 Cu1 126.9(2) . . ? C26 N6 Cu1 110.0(2) . . ? N1 C1 C2 121.3(3) . . ? C1 C2 C3 119.3(4) . . ? C4 C3 C2 118.6(3) . . ? C5 C4 C3 121.5(3) . . ? N1 C5 C4 118.4(3) . . ? N1 C5 C6 120.2(3) . . ? C4 C5 C6 121.3(3) . . ? N2 C6 C7 121.4(3) . . ? N2 C6 C5 118.6(3) . . ? C7 C6 C5 119.8(3) . . ? C6 C7 C8 119.1(3) . . ? C9 C8 C7 119.5(4) . . ? C8 C9 C10 119.1(3) . . ? N2 C10 C9 121.5(3) . . ? N2 C10 C11 114.7(3) . . ? C9 C10 C11 123.8(3) . . ? N3 C11 C12 122.4(3) . . ? N3 C11 C10 114.7(3) . . ? C12 C11 C10 122.9(3) . . ? C11 C12 C13 118.5(3) . . ? C14 C13 C12 119.1(3) . . ? C15 C14 C13 119.4(3) . . ? N3 C15 C14 122.2(3) . . ? N4 C16 C17 120.8(3) . . ? C16 C17 C18 120.4(4) . . ? C17 C18 C19 118.1(4) . . ? C18 C19 C20 121.7(4) . . ? N4 C20 C19 118.1(3) . . ? N4 C20 C21 120.6(3) . . ? C19 C20 C21 121.3(3) . . ? N5 C21 C22 120.8(3) . . ? N5 C21 C20 120.3(3) . . ? C22 C21 C20 118.6(3) . . ? C23 C22 C21 119.7(3) . . ? C24 C23 C22 119.2(3) . . ? C23 C24 C25 119.5(3) . . ? N5 C25 C24 121.3(3) . . ? N5 C25 C26 115.9(3) . . ? C24 C25 C26 122.8(3) . . ? N6 C26 C27 122.3(3) . . ? N6 C26 C25 114.6(3) . . ? C27 C26 C25 123.1(3) . . ? C26 C27 C28 118.2(3) . . ? C29 C28 C27 119.8(4) . . ? C28 C29 C30 118.2(4) . . ? N6 C30 C29 123.5(4) . . ? O4 Cl1 O5 109.67(17) . . ? O4 Cl1 O3 109.03(17) . . ? O5 Cl1 O3 109.98(16) . . ? O4 Cl1 O6 109.37(16) . . ? O5 Cl1 O6 109.54(18) . . ? O3 Cl1 O6 109.23(17) . . ? O8 Cl2 O10 113.34(19) . . ? O8 Cl2 O7 112.25(18) . . ? O10 Cl2 O7 111.87(18) . . ? O8 Cl2 O9 107.05(18) . . ? O10 Cl2 O9 106.55(18) . . ? O7 Cl2 O9 105.14(18) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.773 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.149 # Attachment '2.cif.cif' data_aja0301 _database_code_depnum_ccdc_archive 'CCDC 659291' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 Cl2 Cu1 N6 O12' _chemical_formula_sum 'C30 H22 Cl2 Cu N6 O12' _chemical_formula_weight 792.98 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 11.9300(3) _cell_length_b 11.9300(3) _cell_length_c 22.5540(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3210.00(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8884 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Irregular Block' _exptl_crystal_colour Green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.763 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 13174 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1808 _reflns_number_gt 1480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0360P)^2^+4.9118P] 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 1808 _refine_ls_number_parameters 117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 C1 C -0.16777(19) -0.02510(18) 0.12045(10) 0.0250(5) Uani 1 1 d . . . H1 H -0.1414 -0.0582 0.1561 0.030 Uiso 1 1 calc R . . C2 C -0.27280(19) -0.05215(19) 0.09933(11) 0.0288(5) Uani 1 1 d . . . H2 H -0.3179 -0.1052 0.1198 0.035 Uiso 1 1 calc R . . C3 C -0.31195(19) -0.00166(19) 0.04827(10) 0.0290(5) Uani 1 1 d . . . H3 H -0.3853 -0.0172 0.0340 0.035 Uiso 1 1 calc R . . C4 C -0.24281(18) 0.07187(18) 0.01817(10) 0.0243(5) Uani 1 1 d . . . H4 H -0.2686 0.1062 -0.0173 0.029 Uiso 1 1 calc R . . C5 C -0.13626(16) 0.09604(16) 0.03914(9) 0.0178(4) Uani 1 1 d . . . C6 C -0.06197(16) 0.17465(16) 0.00637(9) 0.0177(4) Uani 1 1 d . . . C7 C -0.06195(18) 0.17173(18) -0.05527(9) 0.0240(5) Uani 1 1 d . . . H7 H -0.1041 0.1165 -0.0758 0.029 Uiso 1 1 calc R . . C8 C 0.0000 0.2500 -0.08639(13) 0.0249(7) Uani 1 2 d S . . H8 H 0.0000 0.2500 -0.1285 0.030 Uiso 1 2 calc SR . . O1 O -0.00193(12) 0.07284(13) 0.11353(6) 0.0253(4) Uani 1 1 d . . . Cu1 Cu 0.0000 0.2500 0.1250 0.01486(15) Uani 1 4 d S . . N1 N -0.10207(14) 0.04814(14) 0.09079(7) 0.0196(4) Uani 1 1 d . . . N2 N 0.0000 0.2500 0.03658(10) 0.0160(5) Uani 1 2 d S . . Cl1S Cl -0.5000 0.2500 -0.01588(3) 0.02150(19) Uani 1 2 d S . . O1S O -0.53656(14) 0.34180(14) -0.05241(7) 0.0326(4) Uani 1 1 d . . . O2S O -0.40864(14) 0.28638(15) 0.02117(7) 0.0367(4) 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 C1 0.0291(12) 0.0204(11) 0.0256(11) 0.0046(9) 0.0031(9) -0.0021(9) C2 0.0290(12) 0.0229(12) 0.0344(12) -0.0023(9) 0.0054(10) -0.0076(9) C3 0.0219(11) 0.0276(12) 0.0375(13) -0.0060(10) -0.0033(9) -0.0061(9) C4 0.0235(11) 0.0242(11) 0.0252(11) -0.0021(9) -0.0043(9) -0.0010(9) C5 0.0203(10) 0.0139(10) 0.0194(10) -0.0038(8) -0.0017(8) 0.0012(8) C6 0.0176(10) 0.0174(10) 0.0181(9) -0.0016(8) -0.0017(8) 0.0037(8) C7 0.0262(12) 0.0252(11) 0.0205(10) -0.0041(9) -0.0043(9) 0.0013(9) C8 0.0328(17) 0.0287(17) 0.0132(13) 0.000 0.000 0.0029(13) O1 0.0193(8) 0.0300(8) 0.0266(8) 0.0064(6) -0.0078(6) -0.0033(6) Cu1 0.01520(18) 0.01520(18) 0.0142(2) 0.000 0.000 0.000 N1 0.0197(9) 0.0168(9) 0.0222(9) -0.0007(7) -0.0019(7) -0.0009(7) N2 0.0146(12) 0.0128(11) 0.0205(12) 0.000 0.000 0.0010(9) Cl1S 0.0216(4) 0.0247(4) 0.0182(4) 0.000 0.000 -0.0030(3) O1S 0.0298(9) 0.0372(10) 0.0307(9) 0.0102(7) -0.0027(7) 0.0022(7) O2S 0.0393(10) 0.0388(10) 0.0322(9) -0.0005(8) -0.0157(7) -0.0100(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 C1 N1 1.351(3) . ? C1 C2 1.379(3) . ? C2 C3 1.381(3) . ? C3 C4 1.382(3) . ? C4 C5 1.386(3) . ? C5 N1 1.360(3) . ? C5 C6 1.487(3) . ? C6 N2 1.349(2) . ? C6 C7 1.391(3) . ? C7 C8 1.382(3) . ? C8 C7 1.382(3) 2 ? O1 N1 1.333(2) . ? O1 Cu1 2.1294(15) . ? Cu1 N2 1.994(2) 15 ? Cu1 N2 1.994(2) . ? Cu1 O1 2.1294(15) 15 ? Cu1 O1 2.1294(15) 16 ? Cu1 O1 2.1294(15) 2 ? N2 C6 1.349(2) 2 ? Cl1S O1S 1.4382(16) 2_455 ? Cl1S O1S 1.4382(16) . ? Cl1S O2S 1.4403(16) 2_455 ? Cl1S O2S 1.4403(16) . ? 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 C1 C2 120.5(2) . . ? C1 C2 C3 119.6(2) . . ? C2 C3 C4 119.0(2) . . ? C3 C4 C5 120.8(2) . . ? N1 C5 C4 118.66(19) . . ? N1 C5 C6 120.79(17) . . ? C4 C5 C6 120.54(18) . . ? N2 C6 C7 121.44(19) . . ? N2 C6 C5 119.74(18) . . ? C7 C6 C5 118.76(18) . . ? C8 C7 C6 119.4(2) . . ? C7 C8 C7 119.0(3) 2 . ? N1 O1 Cu1 106.01(11) . . ? N2 Cu1 N2 180.0 15 . ? N2 Cu1 O1 83.03(4) 15 15 ? N2 Cu1 O1 96.97(4) . 15 ? N2 Cu1 O1 83.03(4) 15 16 ? N2 Cu1 O1 96.97(4) . 16 ? O1 Cu1 O1 166.06(8) 15 16 ? N2 Cu1 O1 96.98(4) 15 . ? N2 Cu1 O1 83.02(4) . . ? O1 Cu1 O1 90.845(9) 15 . ? O1 Cu1 O1 90.845(9) 16 . ? N2 Cu1 O1 96.98(4) 15 2 ? N2 Cu1 O1 83.02(4) . 2 ? O1 Cu1 O1 90.845(9) 15 2 ? O1 Cu1 O1 90.845(9) 16 2 ? O1 Cu1 O1 166.04(8) . 2 ? O1 N1 C1 118.18(17) . . ? O1 N1 C5 120.36(16) . . ? C1 N1 C5 121.46(18) . . ? C6 N2 C6 119.3(2) . 2 ? C6 N2 Cu1 120.35(12) . . ? C6 N2 Cu1 120.35(12) 2 . ? O1S Cl1S O1S 110.11(14) 2_455 . ? O1S Cl1S O2S 109.41(9) 2_455 2_455 ? O1S Cl1S O2S 109.41(10) . 2_455 ? O1S Cl1S O2S 109.41(10) 2_455 . ? O1S Cl1S O2S 109.41(9) . . ? O2S Cl1S O2S 109.07(15) 2_455 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.310 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.068 # Attachment '3.cif.cif' data_01src109 _database_code_depnum_ccdc_archive 'CCDC 659292' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H29 Cl2 Cu N8 O14.50' _chemical_formula_weight 916.09 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' 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.189(3) _cell_length_b 23.155(5) _cell_length_c 24.749(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7558(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23248 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9241 _exptl_absorpt_correction_T_max 0.9686 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32866 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.1426 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16055 _reflns_number_gt 9573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The H atoms on the water solvate are restrained to idealised geometry. ; _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^)+(0.0708P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(13) _refine_ls_number_reflns 16055 _refine_ls_number_parameters 1092 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.027 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 C61 C 0.1059(8) 0.0736(4) 0.9984(3) 0.083(3) Uani 1 1 d . . . H61A H 0.0813 0.0363 1.0117 0.125 Uiso 1 1 calc R . . H61B H 0.1768 0.0697 0.9871 0.125 Uiso 1 1 calc R . . H61C H 0.0646 0.0858 0.9675 0.125 Uiso 1 1 calc R . . C62 C 0.0983(7) 0.1175(4) 1.0422(4) 0.063(2) Uani 1 1 d . . . C63 C 0.6287(8) 0.0151(5) 0.7824(4) 0.086(3) Uani 1 1 d . . . H63A H 0.6977 0.0210 0.7689 0.129 Uiso 1 1 calc R . . H63B H 0.5954 -0.0151 0.7611 0.129 Uiso 1 1 calc R . . H63C H 0.6313 0.0034 0.8204 0.129 Uiso 1 1 calc R . . C64 C 0.5726(7) 0.0678(7) 0.7776(3) 0.090(4) Uani 1 1 d . . . C65 C 0.4733(7) 0.6674(4) 0.8502(3) 0.074(3) Uani 1 1 d . . . H65A H 0.4758 0.6260 0.8583 0.111 Uiso 1 1 calc R . . H65B H 0.5363 0.6790 0.8322 0.111 Uiso 1 1 calc R . . H65C H 0.4156 0.6754 0.8265 0.111 Uiso 1 1 calc R . . C66 C 0.4621(6) 0.6996(3) 0.9000(3) 0.0482(19) Uani 1 1 d . . . C67 C 0.3866(14) 0.7701(6) 0.7226(7) 0.164(7) Uani 1 1 d . . . H67A H 0.3993 0.7667 0.7614 0.246 Uiso 1 1 calc R . . H67B H 0.4363 0.7965 0.7065 0.246 Uiso 1 1 calc R . . H67C H 0.3927 0.7320 0.7057 0.246 Uiso 1 1 calc R . . C68 C 0.2856(18) 0.7923(5) 0.7138(5) 0.117(5) Uani 1 1 d . . . N13 N 0.0890(8) 0.1478(4) 1.0768(3) 0.099(3) Uani 1 1 d . . . N14 N 0.5320(8) 0.1095(7) 0.7724(4) 0.166(7) Uani 1 1 d . . . N15 N 0.4494(6) 0.7247(3) 0.9371(3) 0.067(2) Uani 1 1 d . . . N16 N 0.1960(12) 0.8081(5) 0.7074(6) 0.143(5) Uani 1 1 d . . . O29 O 0.7605(6) 0.7438(4) 0.8946(5) 0.128(3) Uani 1 1 d D . . H29A H 0.772(9) 0.7021(12) 0.886(6) 0.192 Uiso 1 1 d D . . H29B H 0.698(6) 0.743(5) 0.917(6) 0.192 Uiso 1 1 d D . . C1 C 0.8012(5) 0.9311(3) 0.9064(3) 0.0349(15) Uani 1 1 d . . . H1 H 0.8028 0.9570 0.8766 0.042 Uiso 1 1 calc R . . C2 C 0.8874(5) 0.9012(3) 0.9207(2) 0.0323(14) Uani 1 1 d . . . H2 H 0.9489 0.9073 0.9015 0.039 Uiso 1 1 calc R . . C3 C 0.8844(5) 0.8628(3) 0.9625(2) 0.0352(14) Uani 1 1 d . . . H3 H 0.9438 0.8423 0.9725 0.042 Uiso 1 1 calc R . . C4 C 0.7939(4) 0.8538(3) 0.9906(2) 0.0310(14) Uani 1 1 d . . . H4 H 0.7907 0.8260 1.0187 0.037 Uiso 1 1 calc R . . C5 C 0.7098(4) 0.8854(3) 0.9771(2) 0.0291(14) Uani 1 1 d . . . C6 C 0.6113(5) 0.8788(3) 1.0040(2) 0.0298(13) Uani 1 1 d . . . C7 C 0.5599(5) 0.8267(3) 1.0054(2) 0.0391(16) Uani 1 1 d . . . H7 H 0.5873 0.7937 0.9879 0.047 Uiso 1 1 calc R . . C8 C 0.4679(5) 0.8230(3) 1.0325(3) 0.0394(16) Uani 1 1 d . . . H8 H 0.4340 0.7869 1.0357 0.047 Uiso 1 1 calc R . . C9 C 0.4263(5) 0.8722(3) 1.0548(2) 0.0378(17) Uani 1 1 d . . . H9 H 0.3620 0.8701 1.0720 0.045 Uiso 1 1 calc R . . C10 C 0.4761(4) 0.9237(3) 1.0524(2) 0.0311(15) Uani 1 1 d . . . C11 C 0.4360(4) 0.9779(3) 1.0732(2) 0.0307(14) Uani 1 1 d . . . C12 C 0.4079(5) 0.9856(3) 1.1282(2) 0.0413(17) Uani 1 1 d . . . H12 H 0.4147 0.9547 1.1532 0.050 Uiso 1 1 calc R . . C13 C 0.3715(5) 1.0372(3) 1.1447(3) 0.0472(19) Uani 1 1 d . . . H13 H 0.3511 1.0422 1.1812 0.057 Uiso 1 1 calc R . . C14 C 0.3639(5) 1.0825(3) 1.1091(2) 0.0453(18) Uani 1 1 d . . . H14 H 0.3421 1.1193 1.1216 0.054 Uiso 1 1 calc R . . C15 C 0.3878(5) 1.0748(3) 1.0551(3) 0.0408(16) Uani 1 1 d . . . H15 H 0.3798 1.1057 1.0302 0.049 Uiso 1 1 calc R . . C16 C 0.4125(5) 1.0885(3) 0.8881(2) 0.0349(16) Uani 1 1 d . . . H16 H 0.4034 1.0509 0.8736 0.042 Uiso 1 1 calc R . . C17 C 0.3318(5) 1.1261(3) 0.8902(2) 0.0418(17) Uani 1 1 d . . . H17 H 0.2666 1.1144 0.8782 0.050 Uiso 1 1 calc R . . C18 C 0.3477(5) 1.1822(4) 0.9105(3) 0.056(2) Uani 1 1 d . . . H18 H 0.2935 1.2092 0.9118 0.067 Uiso 1 1 calc R . . C19 C 0.4421(5) 1.1971(3) 0.9284(3) 0.0460(19) Uani 1 1 d . . . H19 H 0.4539 1.2352 0.9413 0.055 Uiso 1 1 calc R . . C20 C 0.5208(5) 1.1578(3) 0.9282(2) 0.0315(15) Uani 1 1 d . . . C21 C 0.6248(5) 1.1711(3) 0.9464(2) 0.0347(15) Uani 1 1 d . . . C22 C 0.6776(5) 1.2187(3) 0.9275(2) 0.0377(16) Uani 1 1 d . . . H22 H 0.6472 1.2437 0.9017 0.045 Uiso 1 1 calc R . . C23 C 0.7754(5) 1.2300(3) 0.9464(3) 0.0419(17) Uani 1 1 d . . . H23 H 0.8121 1.2628 0.9343 0.050 Uiso 1 1 calc R . . C24 C 0.8174(5) 1.1915(3) 0.9835(2) 0.0347(15) Uani 1 1 d . . . H24 H 0.8849 1.1971 0.9958 0.042 Uiso 1 1 calc R . . C25 C 0.7621(4) 1.1456(3) 1.0025(2) 0.0308(15) Uani 1 1 d . . . C26 C 0.8022(4) 1.1038(3) 1.0430(2) 0.0283(14) Uani 1 1 d . . . C27 C 0.8306(4) 1.1172(3) 1.0943(2) 0.0358(16) Uani 1 1 d . . . H27 H 0.8244 1.1559 1.1065 0.043 Uiso 1 1 calc R . . C28 C 0.8681(5) 1.0759(3) 1.1288(3) 0.0449(18) Uani 1 1 d . . . H28 H 0.8889 1.0858 1.1644 0.054 Uiso 1 1 calc R . . C29 C 0.8747(5) 1.0206(3) 1.1108(2) 0.0410(17) Uani 1 1 d . . . H29 H 0.8982 0.9912 1.1345 0.049 Uiso 1 1 calc R . . C30 C 0.8474(4) 1.0061(3) 1.0577(3) 0.0368(15) Uani 1 1 d . . . H30 H 0.8538 0.9675 1.0451 0.044 Uiso 1 1 calc R . . C31 C 0.3563(5) 0.9520(3) 0.7484(3) 0.0371(16) Uani 1 1 d . . . H31 H 0.3625 0.9213 0.7737 0.045 Uiso 1 1 calc R . . C32 C 0.3916(5) 0.9445(3) 0.6975(3) 0.0423(16) Uani 1 1 d . . . H32 H 0.4241 0.9094 0.6876 0.051 Uiso 1 1 calc R . . C33 C 0.3799(5) 0.9890(3) 0.6593(3) 0.0427(17) Uani 1 1 d . . . H33 H 0.4023 0.9839 0.6231 0.051 Uiso 1 1 calc R . . C34 C 0.3362(4) 1.0392(3) 0.6749(3) 0.0338(15) Uani 1 1 d . . . H34 H 0.3310 1.0704 0.6501 0.041 Uiso 1 1 calc R . . C35 C 0.2992(5) 1.0452(3) 0.7265(2) 0.0330(15) Uani 1 1 d . . . C36 C 0.2483(5) 1.0973(3) 0.7467(2) 0.0335(15) Uani 1 1 d . . . C37 C 0.2950(5) 1.1521(3) 0.7457(3) 0.0427(17) Uani 1 1 d . . . H37 H 0.3622 1.1565 0.7325 0.051 Uiso 1 1 calc R . . C38 C 0.2408(6) 1.1992(3) 0.7644(3) 0.0472(18) Uani 1 1 d . . . H38 H 0.2704 1.2366 0.7632 0.057 Uiso 1 1 calc R . . C39 C 0.1452(5) 1.1925(3) 0.7846(3) 0.0388(16) Uani 1 1 d . . . H39 H 0.1092 1.2250 0.7979 0.047 Uiso 1 1 calc R . . C40 C 0.1000(5) 1.1376(3) 0.7857(2) 0.0296(14) Uani 1 1 d . . . C41 C -0.0001(4) 1.1270(3) 0.8088(2) 0.0276(14) Uani 1 1 d . . . C42 C -0.0861(5) 1.1566(3) 0.7925(2) 0.0363(16) Uani 1 1 d . . . H42 H -0.0821 1.1850 0.7648 0.044 Uiso 1 1 calc R . . C43 C -0.1795(5) 1.1442(3) 0.8176(3) 0.0429(17) Uani 1 1 d . . . H43 H -0.2403 1.1621 0.8057 0.052 Uiso 1 1 calc R . . C44 C -0.1807(5) 1.1046(3) 0.8605(2) 0.0356(16) Uani 1 1 d . . . H44 H -0.2424 1.0959 0.8786 0.043 Uiso 1 1 calc R . . C45 C -0.0933(5) 1.0792(3) 0.8757(2) 0.0308(15) Uani 1 1 d . . . H45 H -0.0943 1.0533 0.9055 0.037 Uiso 1 1 calc R . . C46 C -0.1133(4) 0.9957(3) 0.7206(2) 0.0325(14) Uani 1 1 d . . . H46 H -0.1262 1.0344 0.7316 0.039 Uiso 1 1 calc R . . C47 C -0.1317(4) 0.9796(3) 0.6678(2) 0.0390(16) Uani 1 1 d . . . H47 H -0.1570 1.0069 0.6425 0.047 Uiso 1 1 calc R . . C48 C -0.1127(5) 0.9229(3) 0.6518(2) 0.0443(17) Uani 1 1 d . . . H48 H -0.1252 0.9110 0.6157 0.053 Uiso 1 1 calc R . . C49 C -0.0747(4) 0.8834(3) 0.6901(2) 0.0371(16) Uani 1 1 d . . . H49 H -0.0620 0.8444 0.6801 0.044 Uiso 1 1 calc R . . C50 C -0.0563(4) 0.9017(3) 0.7419(2) 0.0294(14) Uani 1 1 d . . . C51 C -0.0145(4) 0.8633(3) 0.7836(2) 0.0296(14) Uani 1 1 d . . . C52 C -0.0634(5) 0.8137(3) 0.8011(2) 0.0366(15) Uani 1 1 d . . . H52 H -0.1271 0.8033 0.7860 0.044 Uiso 1 1 calc R . . C53 C -0.0201(5) 0.7795(3) 0.8400(3) 0.0425(17) Uani 1 1 d . . . H53 H -0.0534 0.7456 0.8521 0.051 Uiso 1 1 calc R . . C54 C 0.0724(5) 0.7952(3) 0.8612(3) 0.0421(17) Uani 1 1 d . . . H54 H 0.1036 0.7713 0.8876 0.051 Uiso 1 1 calc R . . C55 C 0.1199(5) 0.8445(2) 0.8449(2) 0.0285(14) Uani 1 1 d . . . C56 C 0.2173(4) 0.8644(3) 0.8660(2) 0.0302(15) Uani 1 1 d . . . C57 C 0.3030(5) 0.8312(3) 0.8655(3) 0.0400(17) Uani 1 1 d . . . H57 H 0.3005 0.7931 0.8511 0.048 Uiso 1 1 calc R . . C58 C 0.3941(5) 0.8526(3) 0.8857(3) 0.0424(16) Uani 1 1 d . . . H58 H 0.4549 0.8307 0.8836 0.051 Uiso 1 1 calc R . . C59 C 0.3930(5) 0.9072(3) 0.9092(2) 0.0380(15) Uani 1 1 d . . . H59 H 0.4535 0.9223 0.9244 0.046 Uiso 1 1 calc R . . C60 C 0.3069(5) 0.9391(3) 0.9107(2) 0.0307(15) Uani 1 1 d . . . H60 H 0.3078 0.9764 0.9265 0.037 Uiso 1 1 calc R . . N1 N 0.7141(4) 0.9238(2) 0.93470(18) 0.0277(11) Uani 1 1 d . . . N2 N 0.5701(4) 0.9264(2) 1.02860(19) 0.0317(12) Uani 1 1 d . . . N3 N 0.4223(3) 1.0233(2) 1.03851(19) 0.0325(12) Uani 1 1 d . . . N4 N 0.5056(3) 1.1049(2) 0.90661(18) 0.0289(12) Uani 1 1 d . . . N5 N 0.6660(4) 1.1376(2) 0.98579(18) 0.0282(12) Uani 1 1 d . . . N6 N 0.8119(4) 1.0478(2) 1.02478(19) 0.0318(12) Uani 1 1 d . . . N7 N 0.3128(3) 1.0017(2) 0.7638(2) 0.0315(12) Uani 1 1 d . . . N8 N 0.1506(4) 1.0921(2) 0.76376(18) 0.0282(12) Uani 1 1 d . . . N9 N -0.0054(4) 1.0889(2) 0.85064(18) 0.0280(12) Uani 1 1 d . . . N10 N -0.0772(3) 0.9571(2) 0.75668(18) 0.0264(11) Uani 1 1 d . . . N11 N 0.0760(4) 0.8767(2) 0.80441(19) 0.0288(12) Uani 1 1 d . . . N12 N 0.2200(4) 0.9181(2) 0.88996(18) 0.0273(11) Uani 1 1 d . . . O1 O 0.6324(3) 0.95456(17) 0.92067(15) 0.0298(9) Uani 1 1 d . . . O2 O 0.6236(3) 0.97408(17) 1.03082(14) 0.0283(9) Uani 1 1 d . . . O3 O 0.4419(3) 1.01494(18) 0.98639(14) 0.0304(10) Uani 1 1 d . . . O4 O 0.5816(3) 1.06777(16) 0.90080(14) 0.0275(9) Uani 1 1 d . . . O5 O 0.6100(3) 1.09571(16) 1.00826(14) 0.0289(9) Uani 1 1 d . . . O6 O 0.7881(3) 1.03565(16) 0.97476(15) 0.0298(9) Uani 1 1 d . . . O7 O 0.2832(3) 1.00922(18) 0.81370(15) 0.0311(10) Uani 1 1 d . . . O8 O 0.1047(3) 1.04164(16) 0.75923(14) 0.0271(9) Uani 1 1 d . . . O9 O 0.0784(3) 1.06262(17) 0.86793(14) 0.0277(9) Uani 1 1 d . . . O10 O -0.0604(3) 0.97371(17) 0.80739(14) 0.0281(9) Uani 1 1 d . . . O11 O 0.1280(3) 0.92204(16) 0.78420(14) 0.0250(9) Uani 1 1 d . . . O12 O 0.1358(3) 0.95000(17) 0.89135(15) 0.0291(10) Uani 1 1 d . . . Cu1 Cu 0.61102(5) 1.02237(3) 0.96607(3) 0.02746(18) Uani 1 1 d . . . Cu2 Cu 0.10988(5) 0.99328(3) 0.82561(2) 0.02532(17) Uani 1 1 d . . . O21 O 0.6355(4) 0.6375(2) 0.01210(18) 0.0539(13) Uani 1 1 d . . . O22 O 0.7184(3) 0.5563(2) -0.0244(2) 0.0519(13) Uani 1 1 d . . . O23 O 0.6758(3) 0.6345(2) -0.08116(17) 0.0462(12) Uani 1 1 d . . . O24 O 0.5467(4) 0.5737(2) -0.0458(2) 0.0583(14) Uani 1 1 d . . . Cl3 Cl 0.64357(12) 0.60020(8) -0.03393(6) 0.0432(4) Uani 1 1 d . . . O13 O 0.0120(5) 0.2753(3) 0.9625(3) 0.108(3) Uani 1 1 d . . . O14 O 0.1539(3) 0.2822(2) 0.90572(19) 0.0495(12) Uani 1 1 d . . . O15 O 0.0809(5) 0.1931(2) 0.9183(3) 0.098(2) Uani 1 1 d . . . O16 O -0.0040(4) 0.2616(3) 0.8709(2) 0.0647(15) Uani 1 1 d . . . Cl1 Cl 0.06069(12) 0.25270(7) 0.91645(6) 0.0384(4) Uani 1 1 d . . . O17 O 0.2280(7) 0.6434(8) 0.8910(3) 0.265(9) Uani 1 1 d . . . O18 O 0.2494(5) 0.6020(3) 0.8085(3) 0.107(3) Uani 1 1 d . . . O19 O 0.2201(5) 0.6964(3) 0.8137(3) 0.100(2) Uani 1 1 d . . . O20 O 0.0908(4) 0.6316(3) 0.8375(2) 0.0712(16) Uani 1 1 d . . . Cl2 Cl 0.19677(15) 0.64330(9) 0.84138(7) 0.0561(5) Uani 1 1 d . . . O25 O 0.6096(9) 0.7926(6) 0.8057(4) 0.206(7) Uani 1 1 d . . . O26 O 0.6812(8) 0.8326(3) 0.7350(4) 0.159(4) Uani 1 1 d . . . O27 O 0.5425(4) 0.8774(3) 0.7771(3) 0.086(2) Uani 1 1 d . . . O28 O 0.6579(18) 0.8492(10) 0.8446(9) 0.107(11) Uani 0.38(2) 1 d P A 1 O28' O 0.7140(8) 0.8884(7) 0.7959(6) 0.115(8) Uani 0.62(2) 1 d P A 2 Cl4 Cl 0.63177(18) 0.84508(12) 0.78229(10) 0.0800(8) Uani 1 1 d . A . 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 C61 0.102(8) 0.101(7) 0.047(5) 0.007(5) -0.008(5) 0.021(7) C62 0.057(5) 0.063(6) 0.070(6) 0.013(5) 0.006(5) -0.002(5) C63 0.085(7) 0.106(8) 0.068(5) -0.036(6) 0.033(6) -0.049(7) C64 0.046(6) 0.191(14) 0.032(4) 0.022(6) -0.001(4) 0.012(7) C65 0.063(6) 0.119(8) 0.041(5) 0.002(5) 0.001(4) 0.027(6) C66 0.052(5) 0.046(5) 0.046(5) 0.007(4) 0.005(4) -0.002(4) C67 0.210(18) 0.117(12) 0.165(14) 0.023(10) -0.061(14) -0.041(14) C68 0.227(19) 0.052(8) 0.072(7) -0.007(6) -0.012(12) -0.032(10) N13 0.141(9) 0.079(6) 0.077(6) -0.006(5) 0.016(6) -0.029(6) N14 0.104(8) 0.293(17) 0.101(8) 0.112(10) 0.037(7) 0.090(10) N15 0.092(6) 0.041(4) 0.068(5) 0.002(4) 0.005(4) -0.019(4) N16 0.193(14) 0.100(9) 0.134(10) -0.017(7) -0.006(10) 0.034(10) O29 0.093(6) 0.092(5) 0.200(10) 0.044(6) -0.013(6) -0.011(5) C1 0.031(4) 0.033(4) 0.041(4) -0.005(3) 0.007(3) -0.002(3) C2 0.028(3) 0.039(4) 0.030(3) -0.005(3) 0.008(3) 0.002(3) C3 0.026(3) 0.043(4) 0.037(3) -0.005(3) 0.000(3) 0.005(3) C4 0.023(3) 0.041(4) 0.029(3) 0.001(3) 0.002(3) 0.004(3) C5 0.023(3) 0.032(4) 0.032(3) -0.004(3) -0.001(3) -0.002(3) C6 0.024(3) 0.034(4) 0.032(3) 0.007(3) -0.008(3) -0.002(3) C7 0.034(4) 0.049(5) 0.033(3) 0.007(3) 0.000(3) -0.004(3) C8 0.028(4) 0.051(5) 0.040(4) 0.018(3) 0.000(3) -0.006(3) C9 0.022(3) 0.065(5) 0.026(3) 0.019(3) -0.001(3) -0.005(3) C10 0.017(3) 0.051(4) 0.025(3) 0.003(3) 0.001(3) -0.002(3) C11 0.019(3) 0.047(4) 0.026(3) 0.006(3) -0.001(3) 0.002(3) C12 0.028(4) 0.068(5) 0.028(3) -0.002(3) 0.000(3) -0.006(4) C13 0.033(4) 0.079(6) 0.029(3) -0.006(4) -0.004(3) 0.000(4) C14 0.035(4) 0.072(5) 0.029(3) -0.005(3) 0.006(3) 0.011(4) C15 0.034(4) 0.051(4) 0.037(3) 0.003(3) -0.007(3) 0.009(4) C16 0.035(4) 0.046(4) 0.023(3) -0.002(3) -0.006(3) -0.001(3) C17 0.034(4) 0.064(5) 0.028(3) -0.001(3) 0.001(3) 0.002(4) C18 0.039(4) 0.079(6) 0.048(4) -0.021(4) -0.014(4) 0.022(4) C19 0.032(4) 0.059(5) 0.047(4) -0.021(4) -0.009(3) 0.021(4) C20 0.027(3) 0.039(4) 0.029(3) -0.009(3) 0.005(3) 0.002(3) C21 0.034(4) 0.033(4) 0.037(3) -0.010(3) -0.008(3) 0.006(3) C22 0.040(4) 0.043(4) 0.030(3) 0.003(3) 0.000(3) 0.000(3) C23 0.043(4) 0.040(4) 0.042(4) -0.006(3) -0.006(3) -0.009(3) C24 0.024(3) 0.040(4) 0.040(4) -0.013(3) -0.003(3) -0.006(3) C25 0.016(3) 0.042(4) 0.034(3) -0.008(3) -0.001(3) 0.000(3) C26 0.016(3) 0.036(4) 0.033(3) -0.009(3) -0.002(3) 0.000(3) C27 0.012(3) 0.059(5) 0.037(3) -0.004(3) -0.005(3) -0.007(3) C28 0.029(4) 0.073(6) 0.032(3) -0.004(4) -0.017(3) 0.001(4) C29 0.024(3) 0.063(5) 0.035(3) 0.006(3) -0.005(3) 0.000(4) C30 0.026(3) 0.037(4) 0.048(4) 0.009(3) -0.005(3) 0.000(3) C31 0.026(3) 0.037(4) 0.048(4) 0.008(3) 0.004(3) 0.002(3) C32 0.026(3) 0.048(4) 0.053(4) -0.002(3) 0.008(4) 0.004(4) C33 0.025(3) 0.068(5) 0.034(3) 0.003(3) 0.006(3) -0.001(4) C34 0.025(3) 0.037(4) 0.039(3) 0.008(3) 0.015(3) 0.004(3) C35 0.025(3) 0.042(4) 0.032(3) 0.009(3) -0.003(3) 0.001(3) C36 0.029(3) 0.039(4) 0.033(3) 0.001(3) 0.010(3) 0.009(3) C37 0.039(4) 0.037(4) 0.052(4) 0.011(3) 0.012(3) -0.008(3) C38 0.051(5) 0.031(4) 0.059(5) 0.012(3) 0.002(4) -0.012(4) C39 0.044(4) 0.026(4) 0.046(4) 0.009(3) 0.005(3) 0.005(3) C40 0.035(3) 0.032(4) 0.023(3) 0.006(2) 0.001(3) 0.002(3) C41 0.025(3) 0.030(4) 0.027(3) 0.001(3) 0.008(3) 0.001(3) C42 0.044(4) 0.031(4) 0.034(3) 0.001(3) -0.007(3) 0.008(3) C43 0.031(4) 0.060(5) 0.038(4) -0.012(3) -0.003(3) 0.007(3) C44 0.035(4) 0.035(4) 0.037(4) -0.008(3) 0.012(3) 0.001(3) C45 0.034(4) 0.030(3) 0.028(3) -0.004(3) 0.014(3) -0.001(3) C46 0.022(3) 0.047(4) 0.028(3) 0.000(3) 0.000(3) -0.001(3) C47 0.023(3) 0.058(5) 0.036(3) 0.007(3) -0.003(3) -0.004(3) C48 0.033(4) 0.066(5) 0.034(3) -0.020(3) 0.002(3) -0.010(4) C49 0.023(3) 0.052(4) 0.036(3) -0.003(3) -0.007(3) 0.003(3) C50 0.022(3) 0.034(4) 0.032(3) -0.007(3) 0.003(3) -0.009(3) C51 0.021(3) 0.034(4) 0.034(3) -0.005(3) -0.004(3) 0.001(3) C52 0.033(4) 0.037(4) 0.039(4) -0.005(3) 0.001(3) -0.005(3) C53 0.039(4) 0.037(4) 0.051(4) -0.002(3) -0.005(3) -0.007(3) C54 0.038(4) 0.037(4) 0.051(4) 0.007(3) 0.008(3) 0.000(3) C55 0.030(3) 0.021(3) 0.034(3) -0.001(2) -0.002(3) 0.005(3) C56 0.026(3) 0.036(4) 0.029(3) 0.008(3) -0.004(3) 0.005(3) C57 0.040(4) 0.040(4) 0.040(4) -0.005(3) -0.002(3) -0.008(3) C58 0.024(3) 0.048(4) 0.055(4) 0.004(3) -0.007(3) 0.006(4) C59 0.023(3) 0.053(4) 0.038(3) 0.007(3) -0.013(3) 0.001(3) C60 0.034(4) 0.042(4) 0.016(3) 0.001(3) -0.002(3) -0.001(3) N1 0.024(3) 0.034(3) 0.025(3) -0.001(2) -0.003(2) -0.004(2) N2 0.023(3) 0.050(4) 0.022(2) 0.004(2) -0.005(2) -0.001(3) N3 0.014(2) 0.058(4) 0.025(3) -0.012(3) 0.001(2) -0.003(2) N4 0.021(3) 0.043(3) 0.023(3) 0.001(2) 0.000(2) 0.002(2) N5 0.025(3) 0.033(3) 0.027(3) -0.005(2) 0.004(2) -0.005(2) N6 0.024(3) 0.043(3) 0.028(3) 0.000(2) 0.003(2) -0.004(2) N7 0.019(2) 0.037(3) 0.038(3) 0.010(2) 0.002(2) 0.001(2) N8 0.029(3) 0.033(3) 0.023(2) 0.002(2) 0.001(2) 0.000(2) N9 0.028(3) 0.031(3) 0.025(3) -0.007(2) -0.004(2) 0.005(2) N10 0.016(2) 0.036(3) 0.027(2) 0.000(2) -0.001(2) -0.001(2) N11 0.030(3) 0.028(3) 0.029(3) -0.002(2) 0.004(2) -0.005(2) N12 0.031(3) 0.032(3) 0.019(2) -0.002(2) 0.000(2) -0.002(2) O1 0.022(2) 0.036(2) 0.031(2) 0.0002(18) -0.0034(18) 0.0067(18) O2 0.025(2) 0.035(2) 0.0243(19) 0.0000(17) -0.0002(18) -0.011(2) O3 0.023(2) 0.047(3) 0.0212(19) 0.0001(18) 0.0041(17) -0.007(2) O4 0.026(2) 0.034(2) 0.0232(19) -0.0032(17) 0.0023(18) 0.0068(19) O5 0.020(2) 0.037(2) 0.030(2) -0.0102(17) 0.0018(19) -0.005(2) O6 0.029(2) 0.036(2) 0.025(2) -0.0032(18) 0.0018(18) 0.0030(19) O7 0.023(2) 0.045(3) 0.025(2) -0.0025(19) 0.0027(17) -0.003(2) O8 0.026(2) 0.031(2) 0.0251(19) -0.0060(16) 0.0032(19) -0.003(2) O9 0.027(2) 0.036(2) 0.0192(19) -0.0008(17) -0.0006(17) 0.0037(19) O10 0.025(2) 0.039(2) 0.0201(19) -0.0046(17) 0.0032(17) 0.0001(19) O11 0.021(2) 0.031(2) 0.0231(18) -0.0046(16) 0.0017(17) -0.0013(18) O12 0.026(2) 0.034(2) 0.027(2) 0.0003(17) 0.0055(18) 0.0040(19) Cu1 0.0235(4) 0.0365(4) 0.0224(3) -0.0016(3) -0.0002(3) -0.0008(3) Cu2 0.0250(4) 0.0301(4) 0.0209(3) -0.0007(3) -0.0005(3) 0.0000(3) O21 0.047(3) 0.077(4) 0.038(2) -0.012(2) 0.005(2) 0.003(3) O22 0.036(3) 0.065(3) 0.055(3) 0.007(3) 0.004(2) 0.017(2) O23 0.047(3) 0.056(3) 0.036(2) 0.002(2) 0.003(2) -0.002(2) O24 0.039(3) 0.075(4) 0.060(3) -0.009(3) -0.002(3) -0.015(3) Cl3 0.0328(9) 0.0634(12) 0.0335(8) 0.0008(8) -0.0008(8) 0.0001(8) O13 0.076(4) 0.150(6) 0.097(5) -0.087(5) 0.048(4) -0.062(4) O14 0.036(3) 0.055(3) 0.057(3) 0.003(2) 0.008(2) -0.006(2) O15 0.113(6) 0.046(4) 0.134(6) 0.023(4) -0.017(5) -0.012(4) O16 0.049(3) 0.096(4) 0.049(3) -0.001(3) -0.008(3) -0.005(3) Cl1 0.0341(9) 0.0411(10) 0.0400(9) 0.0011(7) -0.0028(8) -0.0083(8) O17 0.104(7) 0.65(3) 0.041(4) 0.019(9) -0.018(4) -0.154(12) O18 0.078(5) 0.074(4) 0.169(7) -0.048(5) 0.038(5) -0.006(4) O19 0.090(5) 0.050(4) 0.162(7) 0.012(4) -0.007(5) -0.016(4) O20 0.052(3) 0.097(4) 0.065(4) -0.002(3) 0.008(3) -0.022(3) Cl2 0.0560(12) 0.0701(14) 0.0423(10) 0.0017(9) 0.0055(9) -0.0023(11) O25 0.188(10) 0.243(12) 0.186(10) 0.166(10) 0.119(9) 0.138(10) O26 0.196(9) 0.072(5) 0.209(10) 0.043(6) 0.120(8) 0.067(6) O27 0.047(3) 0.064(4) 0.147(6) -0.010(4) -0.019(4) 0.025(3) O28 0.115(19) 0.096(16) 0.112(19) -0.032(13) -0.058(15) 0.026(14) O28' 0.040(7) 0.165(14) 0.140(14) -0.066(12) -0.020(7) 0.021(7) Cl4 0.0668(16) 0.0932(19) 0.0799(15) -0.0247(14) -0.0145(13) 0.0441(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C61 C62 1.490(12) . ? C62 N13 1.114(10) . ? C63 C64 1.432(15) . ? C64 N14 1.111(16) . ? C65 C66 1.448(11) . ? C66 N15 1.099(9) . ? C67 C68 1.44(2) . ? C68 N16 1.25(2) . ? C1 N1 1.357(7) . ? C1 C2 1.377(9) . ? C2 C3 1.365(8) . ? C3 C4 1.397(8) . ? C4 C5 1.370(8) . ? C5 N1 1.377(7) . ? C5 C6 1.469(8) . ? C6 N2 1.371(8) . ? C6 C7 1.384(9) . ? C7 C8 1.390(9) . ? C8 C9 1.380(9) . ? C9 C10 1.364(9) . ? C10 N2 1.375(7) . ? C10 C11 1.455(9) . ? C11 N3 1.368(8) . ? C11 C12 1.423(8) . ? C12 C13 1.352(10) . ? C13 C14 1.373(10) . ? C14 C15 1.385(9) . ? C15 N3 1.342(8) . ? C16 N4 1.365(7) . ? C16 C17 1.376(9) . ? C17 C18 1.409(10) . ? C18 C19 1.367(9) . ? C19 C20 1.380(9) . ? C20 N4 1.350(8) . ? C20 C21 1.477(9) . ? C21 N5 1.359(8) . ? C21 C22 1.384(9) . ? C22 C23 1.397(9) . ? C23 C24 1.395(9) . ? C24 C25 1.371(9) . ? C25 N5 1.345(7) . ? C25 C26 1.491(9) . ? C26 C27 1.361(8) . ? C26 N6 1.378(8) . ? C27 C28 1.375(9) . ? C28 C29 1.360(10) . ? C29 C30 1.403(9) . ? C30 N6 1.347(8) . ? C31 N7 1.342(8) . ? C31 C32 1.355(9) . ? C32 C33 1.406(9) . ? C33 C34 1.356(9) . ? C34 C35 1.374(9) . ? C35 N7 1.378(7) . ? C35 C36 1.467(9) . ? C36 N8 1.362(7) . ? C36 C37 1.410(9) . ? C37 C38 1.384(10) . ? C38 C39 1.365(9) . ? C39 C40 1.404(9) . ? C40 N8 1.361(7) . ? C40 C41 1.460(8) . ? C41 N9 1.361(7) . ? C41 C42 1.386(8) . ? C42 C43 1.410(9) . ? C43 C44 1.402(9) . ? C44 C45 1.349(9) . ? C45 N9 1.334(7) . ? C46 N10 1.352(7) . ? C46 C47 1.380(8) . ? C47 C48 1.394(9) . ? C48 C49 1.408(9) . ? C49 C50 1.372(8) . ? C50 N10 1.361(8) . ? C50 C51 1.469(8) . ? C51 N11 1.336(7) . ? C51 C52 1.387(9) . ? C52 C53 1.370(9) . ? C53 C54 1.377(9) . ? C54 C55 1.365(9) . ? C55 N11 1.376(7) . ? C55 C56 1.461(8) . ? C56 C57 1.368(9) . ? C56 N12 1.379(8) . ? C57 C58 1.393(9) . ? C58 C59 1.391(9) . ? C59 C60 1.355(9) . ? C60 N12 1.345(7) . ? N1 O1 1.337(6) . ? N2 O2 1.312(6) . ? N3 O3 1.330(6) . ? N4 O4 1.328(6) . ? N5 O5 1.341(6) . ? N6 O6 1.307(6) . ? N7 O7 1.307(6) . ? N8 O8 1.320(6) . ? N9 O9 1.332(6) . ? N10 O10 1.332(6) . ? N11 O11 1.350(6) . ? N12 O12 1.334(6) . ? O1 Cu1 1.951(4) . ? O2 Cu1 1.961(4) . ? O3 Cu1 2.292(4) . ? O4 Cu1 1.966(4) . ? O5 Cu1 1.994(4) . ? O6 Cu1 2.366(4) . ? O7 Cu2 2.334(4) . ? O8 Cu2 1.989(4) . ? O9 Cu2 1.961(4) . ? O10 Cu2 2.335(4) . ? O11 Cu2 1.957(4) . ? O12 Cu2 1.941(4) . ? O21 Cl3 1.433(5) . ? O22 Cl3 1.436(5) . ? O23 Cl3 1.475(5) . ? O24 Cl3 1.449(5) . ? O13 Cl1 1.410(6) . ? O14 Cl1 1.432(5) . ? O15 Cl1 1.407(6) . ? O16 Cl1 1.428(5) . ? O17 Cl2 1.296(7) . ? O18 Cl2 1.436(6) . ? O19 Cl2 1.441(6) . ? O20 Cl2 1.427(5) . ? O25 Cl4 1.377(10) . ? O25 O28 1.75(2) . ? O26 Cl4 1.370(9) . ? O27 Cl4 1.402(5) . ? O28 Cl4 1.58(2) . ? O28' Cl4 1.516(13) . ? 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 N13 C62 C61 175.5(10) . . ? N14 C64 C63 177.1(12) . . ? N15 C66 C65 176.8(9) . . ? N16 C68 C67 175.9(15) . . ? N1 C1 C2 120.3(6) . . ? C3 C2 C1 119.8(6) . . ? C2 C3 C4 120.0(6) . . ? C5 C4 C3 119.4(6) . . ? C4 C5 N1 119.9(5) . . ? C4 C5 C6 123.4(5) . . ? N1 C5 C6 116.7(5) . . ? N2 C6 C7 119.7(6) . . ? N2 C6 C5 117.9(5) . . ? C7 C6 C5 122.4(6) . . ? C6 C7 C8 119.6(7) . . ? C9 C8 C7 119.2(6) . . ? C10 C9 C8 121.0(6) . . ? C9 C10 N2 119.5(6) . . ? C9 C10 C11 124.4(5) . . ? N2 C10 C11 116.1(6) . . ? N3 C11 C12 118.1(6) . . ? N3 C11 C10 119.2(5) . . ? C12 C11 C10 122.7(6) . . ? C13 C12 C11 119.5(6) . . ? C12 C13 C14 120.5(6) . . ? C13 C14 C15 120.3(7) . . ? N3 C15 C14 119.2(6) . . ? N4 C16 C17 120.4(6) . . ? C16 C17 C18 118.9(6) . . ? C19 C18 C17 118.9(7) . . ? C18 C19 C20 121.1(7) . . ? N4 C20 C19 119.2(6) . . ? N4 C20 C21 116.7(5) . . ? C19 C20 C21 123.9(6) . . ? N5 C21 C22 119.7(6) . . ? N5 C21 C20 118.1(6) . . ? C22 C21 C20 122.0(6) . . ? C21 C22 C23 120.0(6) . . ? C22 C23 C24 117.9(6) . . ? C25 C24 C23 120.6(6) . . ? N5 C25 C24 120.1(6) . . ? N5 C25 C26 116.9(5) . . ? C24 C25 C26 123.0(5) . . ? C27 C26 N6 119.7(6) . . ? C27 C26 C25 125.2(6) . . ? N6 C26 C25 115.1(5) . . ? C26 C27 C28 121.3(6) . . ? C29 C28 C27 118.3(6) . . ? C28 C29 C30 121.1(6) . . ? N6 C30 C29 118.9(6) . . ? N7 C31 C32 121.4(6) . . ? C31 C32 C33 119.6(6) . . ? C34 C33 C32 118.9(6) . . ? C33 C34 C35 120.2(6) . . ? C34 C35 N7 120.1(6) . . ? C34 C35 C36 124.1(6) . . ? N7 C35 C36 115.7(5) . . ? N8 C36 C37 119.8(6) . . ? N8 C36 C35 117.8(6) . . ? C37 C36 C35 122.2(6) . . ? C38 C37 C36 118.6(6) . . ? C39 C38 C37 120.6(6) . . ? C38 C39 C40 120.2(6) . . ? N8 C40 C39 119.0(6) . . ? N8 C40 C41 118.0(5) . . ? C39 C40 C41 123.0(6) . . ? N9 C41 C42 120.1(5) . . ? N9 C41 C40 117.0(5) . . ? C42 C41 C40 122.7(5) . . ? C41 C42 C43 118.9(6) . . ? C44 C43 C42 118.6(6) . . ? C45 C44 C43 119.2(6) . . ? N9 C45 C44 122.6(6) . . ? N10 C46 C47 120.5(6) . . ? C46 C47 C48 119.4(6) . . ? C47 C48 C49 119.0(6) . . ? C50 C49 C48 119.4(6) . . ? N10 C50 C49 120.4(6) . . ? N10 C50 C51 117.2(5) . . ? C49 C50 C51 122.4(6) . . ? N11 C51 C52 119.1(6) . . ? N11 C51 C50 117.8(5) . . ? C52 C51 C50 123.1(5) . . ? C53 C52 C51 120.3(6) . . ? C52 C53 C54 119.1(7) . . ? C55 C54 C53 120.9(7) . . ? C54 C55 N11 118.4(6) . . ? C54 C55 C56 124.1(6) . . ? N11 C55 C56 117.4(5) . . ? C57 C56 N12 119.4(5) . . ? C57 C56 C55 123.1(6) . . ? N12 C56 C55 117.4(5) . . ? C56 C57 C58 120.6(6) . . ? C59 C58 C57 117.7(6) . . ? C60 C59 C58 121.0(6) . . ? N12 C60 C59 120.4(6) . . ? O1 N1 C1 118.8(5) . . ? O1 N1 C5 120.6(5) . . ? C1 N1 C5 120.6(5) . . ? O2 N2 C6 118.9(5) . . ? O2 N2 C10 120.3(5) . . ? C6 N2 C10 120.8(5) . . ? O3 N3 C15 119.5(5) . . ? O3 N3 C11 118.1(5) . . ? C15 N3 C11 122.4(5) . . ? O4 N4 C20 121.2(5) . . ? O4 N4 C16 117.5(5) . . ? C20 N4 C16 121.3(5) . . ? O5 N5 C25 119.4(5) . . ? O5 N5 C21 119.3(5) . . ? C25 N5 C21 121.3(5) . . ? O6 N6 C30 120.1(5) . . ? O6 N6 C26 119.3(5) . . ? C30 N6 C26 120.6(5) . . ? O7 N7 C31 120.7(5) . . ? O7 N7 C35 119.7(5) . . ? C31 N7 C35 119.6(5) . . ? O8 N8 C40 119.6(5) . . ? O8 N8 C36 119.1(5) . . ? C40 N8 C36 121.3(5) . . ? O9 N9 C45 119.6(5) . . ? O9 N9 C41 119.8(5) . . ? C45 N9 C41 120.5(5) . . ? O10 N10 C46 119.4(5) . . ? O10 N10 C50 119.5(5) . . ? C46 N10 C50 121.2(5) . . ? C51 N11 O11 119.4(5) . . ? C51 N11 C55 122.1(5) . . ? O11 N11 C55 118.5(5) . . ? O12 N12 C60 120.0(5) . . ? O12 N12 C56 119.2(5) . . ? C60 N12 C56 120.7(5) . . ? N1 O1 Cu1 113.3(3) . . ? N2 O2 Cu1 113.6(3) . . ? N3 O3 Cu1 113.0(3) . . ? N4 O4 Cu1 114.0(3) . . ? N5 O5 Cu1 113.3(3) . . ? N6 O6 Cu1 110.5(3) . . ? N7 O7 Cu2 113.0(3) . . ? N8 O8 Cu2 114.3(3) . . ? N9 O9 Cu2 112.2(3) . . ? N10 O10 Cu2 113.5(3) . . ? N11 O11 Cu2 113.5(3) . . ? N12 O12 Cu2 114.2(3) . . ? O1 Cu1 O2 89.97(16) . . ? O1 Cu1 O4 89.18(16) . . ? O2 Cu1 O4 173.21(16) . . ? O1 Cu1 O5 171.16(17) . . ? O2 Cu1 O5 93.34(16) . . ? O4 Cu1 O5 88.48(16) . . ? O1 Cu1 O3 101.91(15) . . ? O2 Cu1 O3 81.96(15) . . ? O4 Cu1 O3 91.62(15) . . ? O5 Cu1 O3 86.68(16) . . ? O1 Cu1 O6 90.83(14) . . ? O2 Cu1 O6 85.20(15) . . ? O4 Cu1 O6 101.55(15) . . ? O5 Cu1 O6 81.29(15) . . ? O3 Cu1 O6 161.84(13) . . ? O12 Cu2 O11 88.98(16) . . ? O12 Cu2 O9 90.70(16) . . ? O11 Cu2 O9 174.66(16) . . ? O12 Cu2 O8 171.42(17) . . ? O11 Cu2 O8 92.65(15) . . ? O9 Cu2 O8 88.45(15) . . ? O12 Cu2 O7 90.86(15) . . ? O11 Cu2 O7 86.99(15) . . ? O9 Cu2 O7 98.35(15) . . ? O8 Cu2 O7 80.82(15) . . ? O12 Cu2 O10 103.36(15) . . ? O11 Cu2 O10 81.54(15) . . ? O9 Cu2 O10 93.35(15) . . ? O8 Cu2 O10 85.22(15) . . ? O7 Cu2 O10 161.48(13) . . ? O21 Cl3 O22 110.2(3) . . ? O21 Cl3 O24 110.6(3) . . ? O22 Cl3 O24 109.9(3) . . ? O21 Cl3 O23 109.1(3) . . ? O22 Cl3 O23 108.3(3) . . ? O24 Cl3 O23 108.7(3) . . ? O15 Cl1 O13 115.1(5) . . ? O15 Cl1 O16 106.3(4) . . ? O13 Cl1 O16 108.2(4) . . ? O15 Cl1 O14 108.2(4) . . ? O13 Cl1 O14 111.3(3) . . ? O16 Cl1 O14 107.4(3) . . ? O17 Cl2 O20 112.0(4) . . ? O17 Cl2 O18 112.7(8) . . ? O20 Cl2 O18 108.0(4) . . ? O17 Cl2 O19 112.5(8) . . ? O20 Cl2 O19 109.8(4) . . ? O18 Cl2 O19 101.3(4) . . ? Cl4 O25 O28 59.6(11) . . ? Cl4 O28 O25 48.6(6) . . ? O26 Cl4 O25 105.9(6) . . ? O26 Cl4 O27 115.7(6) . . ? O25 Cl4 O27 109.4(5) . . ? O26 Cl4 O28' 89.4(7) . . ? O25 Cl4 O28' 129.9(9) . . ? O27 Cl4 O28' 105.5(6) . . ? O26 Cl4 O28 137.8(10) . . ? O25 Cl4 O28 71.9(10) . . ? O27 Cl4 O28 103.9(9) . . ? O28' Cl4 O28 65.7(9) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.669 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.086 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 659293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H33 Cl4 Cu2 N6 O24' _chemical_formula_weight 1130.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.359(4) _cell_length_b 13.832(6) _cell_length_c 15.251(4) _cell_angle_alpha 74.14(3) _cell_angle_beta 80.58(2) _cell_angle_gamma 78.99(2) _cell_volume 2049.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1146 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5218 _exptl_absorpt_correction_T_max 0.8206 _exptl_absorpt_process_details ; DIFABS: Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8616 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.29 _reflns_number_total 8289 _reflns_number_gt 7036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _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. ; _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^)+(0.0581P)^2^+3.3765P] 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 8289 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.007 _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 O1 O 0.35341(18) 0.93415(14) 0.28483(13) 0.0175(4) Uani 1 1 d . . . O2 O 0.5697(2) 0.8268(2) 0.18804(16) 0.0256(5) Uani 1 1 d . . . O3 O 0.6067(2) 0.90659(16) 0.34684(16) 0.0197(4) Uani 1 1 d . . . H03A H 0.618(5) 0.920(4) 0.400(4) 0.062(15) Uiso 1 1 d . . . H03B H 0.607(4) 0.956(4) 0.314(3) 0.045(13) Uiso 1 1 d . . . O4 O 0.3542(2) 0.86719(16) 0.48032(14) 0.0275(5) Uani 1 1 d . . . O5 O 0.4418(3) 0.71966(18) 0.58466(19) 0.0406(6) Uani 1 1 d . . . O6 O 0.2131(3) 0.7555(2) 0.57276(19) 0.0425(6) Uani 1 1 d . . . O7 O 0.3128(2) 0.85579(17) 0.63780(14) 0.0315(5) Uani 1 1 d . . . O8 O 0.63633(18) 1.07427(14) 0.20448(13) 0.0186(4) Uani 1 1 d . . . O9 O 0.4201(2) 1.17721(19) 0.29628(17) 0.0264(5) Uani 1 1 d . . . H09A H 0.379(5) 1.229(4) 0.305(3) 0.047(13) Uiso 1 1 d . . . H09B H 0.464(5) 1.156(4) 0.335(4) 0.068(18) Uiso 1 1 d . . . O10 O 0.3857(2) 1.09791(16) 0.13956(15) 0.0197(4) Uani 1 1 d . . . H010 H 0.382(4) 1.046(3) 0.177(3) 0.032(11) Uiso 1 1 d . . . O11 O 0.6250(3) 1.14985(18) 0.00710(16) 0.0379(6) Uani 1 1 d . . . O12 O 0.7290(3) 1.1400(2) -0.13631(17) 0.0507(8) Uani 1 1 d . . . O13 O 0.7886(3) 1.2507(2) -0.0624(2) 0.0472(7) Uani 1 1 d . . . O14 O 0.5869(3) 1.28708(19) -0.1212(2) 0.0534(8) Uani 1 1 d . . . O15 O -0.0414(3) 0.6113(2) 0.5955(3) 0.0726(11) Uani 1 1 d . . . O16 O -0.1493(3) 0.7777(2) 0.55997(18) 0.0461(7) Uani 1 1 d . . . O17 O -0.2553(2) 0.65077(18) 0.6645(2) 0.0377(6) Uani 1 1 d . . . O18 O -0.0812(3) 0.7097(3) 0.7039(2) 0.0597(9) Uani 1 1 d . . . O19 O 0.8860(3) 0.7505(2) 0.2006(2) 0.0480(7) Uani 1 1 d . . . O20 O 0.9636(3) 0.5824(2) 0.1996(2) 0.0520(7) Uani 1 1 d . . . O21 O 0.9281(3) 0.7024(3) 0.0621(2) 0.0725(11) Uani 1 1 d . . . O22 O 0.7464(2) 0.65419(18) 0.1665(2) 0.0411(6) Uani 1 1 d . . . O23 O -0.3440(2) 0.9401(2) 1.01172(17) 0.0277(5) Uani 1 1 d . . . O24 O 0.6359(3) 0.9328(2) 0.50421(18) 0.0345(6) Uani 1 1 d . . . H024 H 0.679(4) 0.894(3) 0.540(3) 0.038(12) Uiso 1 1 d . . . H024' H 0.625(4) 0.978(3) 0.516(3) 0.031(12) Uiso 1 1 d . . . N1 N 0.2245(2) 0.94173(17) 0.31846(15) 0.0161(4) Uani 1 1 d . . . N2 N 0.3524(2) 0.72815(17) 0.35068(15) 0.0154(4) Uani 1 1 d . . . N3 N 0.5964(2) 0.68858(17) 0.38589(16) 0.0180(5) Uani 1 1 d . . . N4 N 0.7656(2) 1.07184(18) 0.17276(16) 0.0173(5) Uani 1 1 d . . . N5 N 0.6276(2) 1.28250(17) 0.14581(15) 0.0168(5) Uani 1 1 d . . . N6 N 0.3873(2) 1.31748(18) 0.10366(17) 0.0204(5) Uani 1 1 d . . . Cu1 Cu 0.47798(3) 0.81995(2) 0.34680(2) 0.01481(10) Uani 1 1 d . . . Cu2 Cu 0.50806(3) 1.18779(2) 0.14514(2) 0.01520(10) Uani 1 1 d . . . Cl1 Cl 0.32928(7) 0.79753(5) 0.57020(4) 0.02051(15) Uani 1 1 d . . . Cl2 Cl -0.12918(7) 0.68567(6) 0.63191(6) 0.02798(17) Uani 1 1 d . . . Cl3 Cl 0.68374(7) 1.20844(5) -0.07862(5) 0.02131(15) Uani 1 1 d . . . Cl4 Cl 0.88171(8) 0.67329(6) 0.15522(6) 0.02891(18) Uani 1 1 d . . . C1 C 0.1643(3) 1.0349(2) 0.3270(2) 0.0207(6) Uani 1 1 d . . . H1 H 0.216(4) 1.080(3) 0.311(2) 0.025 Uiso 1 1 d . . . C2 C 0.0326(3) 1.0513(2) 0.3589(2) 0.0258(6) Uani 1 1 d . . . H2 H -0.002(4) 1.117(3) 0.365(2) 0.031 Uiso 1 1 d . . . C3 C -0.0383(3) 0.9704(3) 0.3844(2) 0.0297(7) Uani 1 1 d . . . H3 H -0.120(4) 0.982(3) 0.407(3) 0.036 Uiso 1 1 d . . . C4 C 0.0259(3) 0.8759(2) 0.3758(2) 0.0253(6) Uani 1 1 d . . . H4 H -0.021(4) 0.821(3) 0.395(3) 0.030 Uiso 1 1 d . . . C5 C 0.1587(3) 0.8604(2) 0.34195(18) 0.0177(5) Uani 1 1 d . . . C6 C 0.2247(3) 0.7579(2) 0.33446(18) 0.0174(5) Uani 1 1 d . . . C7 C 0.1529(3) 0.6912(2) 0.3174(2) 0.0230(6) Uani 1 1 d . . . H7 H 0.064(4) 0.715(3) 0.305(2) 0.028 Uiso 1 1 d . . . C8 C 0.2118(3) 0.5922(2) 0.3205(2) 0.0267(7) Uani 1 1 d . . . H8 H 0.169(4) 0.550(3) 0.310(3) 0.032 Uiso 1 1 d . . . C9 C 0.3412(3) 0.5604(2) 0.3418(2) 0.0239(6) Uani 1 1 d . . . H9 H 0.376(3) 0.492(3) 0.345(2) 0.029 Uiso 1 1 d . . . C10 C 0.4094(3) 0.6308(2) 0.35594(18) 0.0176(5) Uani 1 1 d . . . C11 C 0.5471(3) 0.6078(2) 0.37926(18) 0.0189(6) Uani 1 1 d . . . C12 C 0.6206(3) 0.5118(2) 0.3949(2) 0.0250(6) Uani 1 1 d . . . H12 H 0.592(4) 0.462(3) 0.394(3) 0.030 Uiso 1 1 d . . . C13 C 0.7481(3) 0.4980(2) 0.4181(2) 0.0303(7) Uani 1 1 d . . . H13 H 0.801(4) 0.435(3) 0.433(3) 0.036 Uiso 1 1 d . . . C14 C 0.7977(3) 0.5805(3) 0.4259(2) 0.0309(7) Uani 1 1 d . . . H14 H 0.885(4) 0.576(3) 0.449(3) 0.037 Uiso 1 1 d . . . C15 C 0.7192(3) 0.6749(2) 0.4096(2) 0.0252(6) Uani 1 1 d . . . H15 H 0.750(4) 0.735(3) 0.413(2) 0.030 Uiso 1 1 d . . . C16 C 0.8322(3) 0.9810(2) 0.1622(2) 0.0233(6) Uani 1 1 d . . . H16 H 0.785(4) 0.932(3) 0.178(2) 0.028 Uiso 1 1 d . . . C17 C 0.9645(3) 0.9704(3) 0.1304(2) 0.0284(7) Uani 1 1 d . . . H17 H 1.007(4) 0.909(3) 0.124(3) 0.034 Uiso 1 1 d . . . C18 C 1.0293(3) 1.0542(3) 0.1083(2) 0.0319(7) Uani 1 1 d . . . H18 H 1.111(4) 1.047(3) 0.084(3) 0.038 Uiso 1 1 d . . . C19 C 0.9595(3) 1.1455(3) 0.1203(2) 0.0263(7) Uani 1 1 d . . . H19 H 1.000(4) 1.202(3) 0.107(3) 0.032 Uiso 1 1 d . . . C20 C 0.8260(3) 1.1553(2) 0.15389(18) 0.0196(6) Uani 1 1 d . . . C21 C 0.7535(3) 1.2553(2) 0.16489(18) 0.0200(6) Uani 1 1 d . . . C22 C 0.8182(3) 1.3222(2) 0.1885(2) 0.0267(7) Uani 1 1 d . . . H22 H 0.900(4) 1.300(3) 0.203(3) 0.032 Uiso 1 1 d . . . C23 C 0.7533(4) 1.4182(3) 0.1895(2) 0.0315(7) Uani 1 1 d . . . H23 H 0.797(4) 1.461(3) 0.202(3) 0.038 Uiso 1 1 d . . . C24 C 0.6253(3) 1.4483(2) 0.1652(2) 0.0274(7) Uani 1 1 d . . . H24 H 0.585(4) 1.514(3) 0.167(3) 0.033 Uiso 1 1 d . . . C25 C 0.5644(3) 1.3777(2) 0.14413(18) 0.0201(6) Uani 1 1 d . . . C26 C 0.4288(3) 1.3987(2) 0.11638(19) 0.0205(6) Uani 1 1 d . . . C27 C 0.3503(4) 1.4928(2) 0.1026(2) 0.0294(7) Uani 1 1 d . . . H27 H 0.381(4) 1.543(3) 0.110(3) 0.035 Uiso 1 1 d . . . C28 C 0.2261(3) 1.5040(2) 0.0741(2) 0.0331(8) Uani 1 1 d . . . H28 H 0.175(4) 1.567(3) 0.060(3) 0.040 Uiso 1 1 d . . . C29 C 0.1849(3) 1.4214(3) 0.0595(3) 0.0344(8) Uani 1 1 d . . . H29 H 0.094(4) 1.424(3) 0.035(3) 0.041 Uiso 1 1 d . . . C30 C 0.2680(3) 1.3285(2) 0.0752(2) 0.0282(7) Uani 1 1 d . . . H30 H 0.245(4) 1.272(3) 0.064(3) 0.034 Uiso 1 1 d . . . H23D H -0.364(4) 0.991(4) 1.013(3) 0.039(13) Uiso 1 1 d . . . H10D H 0.379(4) 1.081(3) 0.088(3) 0.044(12) Uiso 1 1 d . . . H23E H -0.363(4) 0.904(4) 1.061(3) 0.046(13) Uiso 1 1 d . . . H02A H 0.606(5) 0.791(4) 0.184(4) 0.044(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0132(9) 0.0174(9) 0.0197(10) -0.0008(8) 0.0003(7) -0.0042(7) O2 0.0223(12) 0.0299(13) 0.0238(12) -0.0065(10) -0.0005(9) -0.0044(11) O3 0.0213(10) 0.0163(10) 0.0216(11) -0.0017(9) -0.0027(8) -0.0077(8) O4 0.0408(13) 0.0259(11) 0.0172(10) -0.0045(9) -0.0007(9) -0.0124(10) O5 0.0420(14) 0.0239(12) 0.0544(16) -0.0090(11) -0.0141(12) 0.0047(10) O6 0.0373(14) 0.0460(15) 0.0488(16) -0.0104(12) 0.0000(12) -0.0241(12) O7 0.0480(14) 0.0293(12) 0.0173(10) -0.0097(9) -0.0013(10) -0.0028(10) O8 0.0158(9) 0.0176(9) 0.0216(10) -0.0028(8) 0.0006(7) -0.0061(7) O9 0.0234(11) 0.0254(12) 0.0294(12) -0.0087(10) 0.0020(10) -0.0033(9) O10 0.0241(10) 0.0178(10) 0.0188(10) -0.0024(9) -0.0037(8) -0.0088(8) O11 0.0593(16) 0.0265(12) 0.0267(12) -0.0102(10) 0.0173(11) -0.0178(11) O12 0.092(2) 0.0382(15) 0.0200(12) -0.0131(11) 0.0118(13) -0.0132(15) O13 0.0427(15) 0.0480(16) 0.0572(17) -0.0032(13) -0.0208(13) -0.0245(13) O14 0.0506(17) 0.0246(13) 0.086(2) 0.0026(13) -0.0422(16) -0.0042(11) O15 0.0319(15) 0.0508(19) 0.140(3) -0.048(2) 0.0079(18) 0.0022(13) O16 0.0430(15) 0.0479(16) 0.0395(15) 0.0022(12) -0.0042(12) -0.0074(12) O17 0.0247(12) 0.0259(12) 0.0656(17) -0.0168(12) 0.0018(11) -0.0100(9) O18 0.067(2) 0.072(2) 0.0492(17) 0.0016(15) -0.0310(15) -0.0363(17) O19 0.0461(16) 0.0385(15) 0.071(2) -0.0283(14) -0.0135(14) -0.0062(12) O20 0.0417(15) 0.0339(14) 0.074(2) -0.0091(14) -0.0084(14) 0.0044(12) O21 0.073(2) 0.116(3) 0.0335(16) -0.0008(17) -0.0079(15) -0.053(2) O22 0.0281(12) 0.0287(13) 0.0694(18) -0.0133(12) -0.0046(12) -0.0112(10) O23 0.0390(13) 0.0219(12) 0.0241(13) -0.0049(10) -0.0041(10) -0.0098(11) O24 0.0519(16) 0.0236(13) 0.0302(13) -0.0056(11) -0.0168(12) -0.0021(12) N1 0.0142(11) 0.0183(11) 0.0159(11) -0.0040(9) -0.0012(8) -0.0036(9) N2 0.0206(11) 0.0150(11) 0.0114(10) -0.0030(8) -0.0004(8) -0.0065(9) N3 0.0201(11) 0.0148(11) 0.0188(11) -0.0044(9) -0.0017(9) -0.0022(9) N4 0.0163(11) 0.0195(11) 0.0167(11) -0.0036(9) -0.0013(9) -0.0057(9) N5 0.0236(12) 0.0159(11) 0.0120(10) -0.0019(9) -0.0003(9) -0.0095(9) N6 0.0233(12) 0.0148(11) 0.0220(12) -0.0037(9) -0.0011(10) -0.0027(9) Cu1 0.01559(17) 0.01222(17) 0.01743(18) -0.00299(13) -0.00266(12) -0.00449(12) Cu2 0.01743(17) 0.01234(17) 0.01690(18) -0.00354(13) -0.00200(13) -0.00512(12) Cl1 0.0246(3) 0.0203(3) 0.0172(3) -0.0042(3) -0.0018(3) -0.0063(3) Cl2 0.0206(3) 0.0220(4) 0.0434(4) -0.0106(3) -0.0049(3) -0.0038(3) Cl3 0.0261(3) 0.0218(3) 0.0170(3) -0.0024(3) -0.0046(3) -0.0080(3) Cl4 0.0285(4) 0.0243(4) 0.0356(4) -0.0078(3) -0.0004(3) -0.0103(3) C1 0.0220(14) 0.0189(14) 0.0222(14) -0.0063(11) -0.0030(11) -0.0036(11) C2 0.0242(15) 0.0239(15) 0.0287(16) -0.0095(13) -0.0031(12) 0.0021(12) C3 0.0170(14) 0.0367(18) 0.0336(18) -0.0098(14) 0.0014(13) -0.0022(13) C4 0.0196(14) 0.0267(16) 0.0289(16) -0.0033(13) 0.0002(12) -0.0095(12) C5 0.0184(13) 0.0189(13) 0.0155(13) -0.0008(10) -0.0030(10) -0.0062(10) C6 0.0214(13) 0.0171(13) 0.0129(12) 0.0002(10) -0.0005(10) -0.0080(11) C7 0.0242(15) 0.0235(15) 0.0230(15) -0.0025(12) -0.0049(12) -0.0107(12) C8 0.0356(17) 0.0240(15) 0.0272(16) -0.0080(12) -0.0062(13) -0.0165(13) C9 0.0350(17) 0.0163(14) 0.0227(15) -0.0048(11) -0.0036(12) -0.0093(12) C10 0.0237(14) 0.0144(13) 0.0142(12) -0.0018(10) -0.0005(10) -0.0057(10) C11 0.0234(14) 0.0183(13) 0.0145(13) -0.0035(10) 0.0000(10) -0.0046(11) C12 0.0332(17) 0.0158(14) 0.0232(15) -0.0030(12) 0.0020(12) -0.0045(12) C13 0.0307(17) 0.0201(15) 0.0320(17) -0.0006(13) -0.0003(13) 0.0043(13) C14 0.0247(16) 0.0297(17) 0.0343(18) -0.0031(14) -0.0068(13) 0.0013(13) C15 0.0232(15) 0.0245(15) 0.0269(16) -0.0034(12) -0.0049(12) -0.0038(12) C16 0.0237(15) 0.0232(15) 0.0243(15) -0.0074(12) -0.0034(12) -0.0041(12) C17 0.0245(15) 0.0317(17) 0.0288(16) -0.0110(13) -0.0033(13) 0.0013(13) C18 0.0181(15) 0.045(2) 0.0299(17) -0.0073(15) 0.0014(13) -0.0053(14) C19 0.0221(15) 0.0312(17) 0.0255(16) 0.0000(13) -0.0038(12) -0.0133(13) C20 0.0219(14) 0.0229(14) 0.0143(13) -0.0004(11) -0.0046(10) -0.0085(11) C21 0.0259(14) 0.0207(14) 0.0138(13) -0.0003(11) -0.0001(11) -0.0121(11) C22 0.0322(17) 0.0280(16) 0.0227(15) -0.0013(12) -0.0085(13) -0.0146(13) C23 0.050(2) 0.0263(16) 0.0260(16) -0.0069(13) -0.0071(14) -0.0232(15) C24 0.0432(19) 0.0176(14) 0.0245(15) -0.0067(12) -0.0032(13) -0.0110(13) C25 0.0315(15) 0.0157(13) 0.0136(13) -0.0031(10) 0.0003(11) -0.0080(11) C26 0.0282(15) 0.0169(13) 0.0158(13) -0.0029(11) 0.0012(11) -0.0070(11) C27 0.0435(19) 0.0182(15) 0.0248(16) -0.0064(12) 0.0019(14) -0.0037(13) C28 0.0345(18) 0.0203(15) 0.0344(18) -0.0005(13) 0.0010(14) 0.0070(13) C29 0.0260(16) 0.0289(17) 0.043(2) -0.0036(15) -0.0058(14) 0.0033(13) C30 0.0271(16) 0.0218(15) 0.0343(17) -0.0030(13) -0.0077(13) -0.0024(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 O1 N1 1.345(3) . ? O1 Cu1 1.9642(19) . ? O2 Cu1 2.435(2) . ? O3 Cu1 1.956(2) . ? O4 Cl1 1.460(2) . ? O4 Cu1 2.402(2) . ? O5 Cl1 1.429(2) . ? O6 Cl1 1.423(2) . ? O7 Cl1 1.444(2) . ? O8 N4 1.345(3) . ? O8 Cu2 1.9674(19) . ? O9 Cu2 2.312(2) . ? O10 Cu2 1.963(2) . ? O11 Cl3 1.444(2) . ? O11 Cu2 2.388(2) . ? O12 Cl3 1.429(3) . ? O13 Cl3 1.412(2) . ? O14 Cl3 1.422(3) . ? O15 Cl2 1.408(3) . ? O16 Cl2 1.442(3) . ? O17 Cl2 1.444(2) . ? O18 Cl2 1.416(3) . ? O19 Cl4 1.433(3) . ? O20 Cl4 1.440(3) . ? O21 Cl4 1.396(3) . ? O22 Cl4 1.450(2) . ? N1 C1 1.351(4) . ? N1 C5 1.360(3) . ? N2 C10 1.349(3) . ? N2 C6 1.350(4) . ? N2 Cu1 1.968(2) . ? N3 C15 1.344(4) . ? N3 C11 1.347(4) . ? N3 Cu1 1.989(2) . ? N4 C16 1.350(4) . ? N4 C20 1.357(4) . ? N5 C21 1.343(4) . ? N5 C25 1.349(4) . ? N5 Cu2 1.970(2) . ? N6 C30 1.344(4) . ? N6 C26 1.348(4) . ? N6 Cu2 1.991(2) . ? C1 C2 1.369(4) . ? C2 C3 1.388(5) . ? C3 C4 1.378(5) . ? C4 C5 1.385(4) . ? C5 C6 1.479(4) . ? C6 C7 1.389(4) . ? C7 C8 1.380(4) . ? C8 C9 1.391(5) . ? C9 C10 1.386(4) . ? C10 C11 1.481(4) . ? C11 C12 1.379(4) . ? C12 C13 1.389(5) . ? C13 C14 1.378(5) . ? C14 C15 1.383(4) . ? C16 C17 1.371(4) . ? C17 C18 1.384(5) . ? C18 C19 1.374(5) . ? C19 C20 1.388(4) . ? C20 C21 1.481(4) . ? C21 C22 1.389(4) . ? C22 C23 1.373(5) . ? C23 C24 1.392(5) . ? C24 C25 1.388(4) . ? C25 C26 1.485(4) . ? C26 C27 1.378(4) . ? C27 C28 1.392(5) . ? C28 C29 1.377(5) . ? C29 C30 1.388(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 N1 O1 Cu1 118.68(15) . . ? Cl1 O4 Cu1 125.40(13) . . ? N4 O8 Cu2 118.86(15) . . ? Cl3 O11 Cu2 135.11(14) . . ? O1 N1 C1 116.1(2) . . ? O1 N1 C5 121.9(2) . . ? C1 N1 C5 122.0(2) . . ? C10 N2 C6 119.9(2) . . ? C10 N2 Cu1 113.91(18) . . ? C6 N2 Cu1 125.29(18) . . ? C15 N3 C11 119.2(2) . . ? C15 N3 Cu1 127.3(2) . . ? C11 N3 Cu1 113.22(19) . . ? O8 N4 C16 116.0(2) . . ? O8 N4 C20 122.0(2) . . ? C16 N4 C20 122.0(3) . . ? C21 N5 C25 120.2(2) . . ? C21 N5 Cu2 125.25(19) . . ? C25 N5 Cu2 113.26(19) . . ? C30 N6 C26 119.5(3) . . ? C30 N6 Cu2 127.0(2) . . ? C26 N6 Cu2 113.06(19) . . ? O3 Cu1 O1 93.54(9) . . ? O3 Cu1 N2 177.55(9) . . ? O1 Cu1 N2 88.82(9) . . ? O3 Cu1 N3 95.87(9) . . ? O1 Cu1 N3 165.77(9) . . ? N2 Cu1 N3 81.93(9) . . ? O3 Cu1 O4 89.27(8) . . ? O1 Cu1 O4 81.56(8) . . ? N2 Cu1 O4 90.43(8) . . ? N3 Cu1 O4 109.16(9) . . ? O3 Cu1 O2 86.40(9) . . ? O1 Cu1 O2 80.74(9) . . ? N2 Cu1 O2 94.63(9) . . ? N3 Cu1 O2 89.21(9) . . ? O4 Cu1 O2 161.47(9) . . ? O10 Cu2 O8 93.29(8) . . ? O10 Cu2 N5 177.37(9) . . ? O8 Cu2 N5 89.05(9) . . ? O10 Cu2 N6 95.97(9) . . ? O8 Cu2 N6 167.81(9) . . ? N5 Cu2 N6 81.87(10) . . ? O10 Cu2 O9 88.13(9) . . ? O8 Cu2 O9 81.38(9) . . ? N5 Cu2 O9 93.38(9) . . ? N6 Cu2 O9 91.00(10) . . ? O10 Cu2 O11 86.54(9) . . ? O8 Cu2 O11 83.55(9) . . ? N5 Cu2 O11 92.56(9) . . ? N6 Cu2 O11 104.88(10) . . ? O9 Cu2 O11 163.69(9) . . ? O6 Cl1 O5 111.12(16) . . ? O6 Cl1 O7 111.32(16) . . ? O5 Cl1 O7 109.53(15) . . ? O6 Cl1 O4 108.95(15) . . ? O5 Cl1 O4 108.67(15) . . ? O7 Cl1 O4 107.13(13) . . ? O15 Cl2 O18 113.0(2) . . ? O15 Cl2 O16 108.9(2) . . ? O18 Cl2 O16 107.75(18) . . ? O15 Cl2 O17 109.21(17) . . ? O18 Cl2 O17 109.62(18) . . ? O16 Cl2 O17 108.20(16) . . ? O13 Cl3 O14 110.03(16) . . ? O13 Cl3 O12 111.75(19) . . ? O14 Cl3 O12 108.62(19) . . ? O13 Cl3 O11 109.66(17) . . ? O14 Cl3 O11 110.20(18) . . ? O12 Cl3 O11 106.51(15) . . ? O21 Cl4 O19 111.2(2) . . ? O21 Cl4 O20 110.1(2) . . ? O19 Cl4 O20 107.29(18) . . ? O21 Cl4 O22 110.14(18) . . ? O19 Cl4 O22 108.82(16) . . ? O20 Cl4 O22 109.18(16) . . ? N1 C1 C2 120.7(3) . . ? C1 C2 C3 119.2(3) . . ? C4 C3 C2 118.9(3) . . ? C3 C4 C5 121.5(3) . . ? N1 C5 C4 117.6(3) . . ? N1 C5 C6 122.3(2) . . ? C4 C5 C6 120.1(3) . . ? N2 C6 C7 120.9(3) . . ? N2 C6 C5 119.0(2) . . ? C7 C6 C5 119.9(3) . . ? C8 C7 C6 119.3(3) . . ? C7 C8 C9 119.6(3) . . ? C10 C9 C8 118.7(3) . . ? N2 C10 C9 121.5(3) . . ? N2 C10 C11 114.0(2) . . ? C9 C10 C11 124.6(3) . . ? N3 C11 C12 121.5(3) . . ? N3 C11 C10 114.8(2) . . ? C12 C11 C10 123.8(3) . . ? C11 C12 C13 119.2(3) . . ? C14 C13 C12 119.2(3) . . ? C13 C14 C15 118.9(3) . . ? N3 C15 C14 122.0(3) . . ? N4 C16 C17 120.6(3) . . ? C16 C17 C18 119.3(3) . . ? C19 C18 C17 118.9(3) . . ? C18 C19 C20 121.5(3) . . ? N4 C20 C19 117.6(3) . . ? N4 C20 C21 122.4(3) . . ? C19 C20 C21 120.0(3) . . ? N5 C21 C22 120.9(3) . . ? N5 C21 C20 118.8(2) . . ? C22 C21 C20 120.1(3) . . ? C23 C22 C21 119.3(3) . . ? C22 C23 C24 119.9(3) . . ? C25 C24 C23 118.4(3) . . ? N5 C25 C24 121.3(3) . . ? N5 C25 C26 114.2(2) . . ? C24 C25 C26 124.6(3) . . ? N6 C26 C27 121.4(3) . . ? N6 C26 C25 114.3(2) . . ? C27 C26 C25 124.3(3) . . ? C26 C27 C28 119.2(3) . . ? C29 C28 C27 119.4(3) . . ? C28 C29 C30 118.7(3) . . ? N6 C30 C29 121.8(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 Cu1 O1 N1 C1 133.7(2) . . . . ? Cu1 O1 N1 C5 -46.7(3) . . . . ? Cu2 O8 N4 C16 -135.1(2) . . . . ? Cu2 O8 N4 C20 45.9(3) . . . . ? N1 O1 Cu1 O3 -133.16(18) . . . . ? N1 O1 Cu1 N2 46.19(18) . . . . ? N1 O1 Cu1 N3 95.5(4) . . . . ? N1 O1 Cu1 O4 -44.42(17) . . . . ? N1 O1 Cu1 O2 141.07(18) . . . . ? C10 N2 Cu1 O3 -40(2) . . . . ? C6 N2 Cu1 O3 151(2) . . . . ? C10 N2 Cu1 O1 155.41(19) . . . . ? C6 N2 Cu1 O1 -13.8(2) . . . . ? C10 N2 Cu1 N3 -13.74(18) . . . . ? C6 N2 Cu1 N3 177.0(2) . . . . ? C10 N2 Cu1 O4 -123.04(19) . . . . ? C6 N2 Cu1 O4 67.7(2) . . . . ? C10 N2 Cu1 O2 74.80(19) . . . . ? C6 N2 Cu1 O2 -94.4(2) . . . . ? C15 N3 Cu1 O3 4.5(3) . . . . ? C11 N3 Cu1 O3 -169.68(19) . . . . ? C15 N3 Cu1 O1 135.6(3) . . . . ? C11 N3 Cu1 O1 -38.5(5) . . . . ? C15 N3 Cu1 N2 -174.4(3) . . . . ? C11 N3 Cu1 N2 11.41(19) . . . . ? C15 N3 Cu1 O4 -86.8(3) . . . . ? C11 N3 Cu1 O4 99.04(19) . . . . ? C15 N3 Cu1 O2 90.8(3) . . . . ? C11 N3 Cu1 O2 -83.4(2) . . . . ? Cl1 O4 Cu1 O3 -117.53(16) . . . . ? Cl1 O4 Cu1 O1 148.77(17) . . . . ? Cl1 O4 Cu1 N2 60.03(16) . . . . ? Cl1 O4 Cu1 N3 -21.57(18) . . . . ? Cl1 O4 Cu1 O2 166.06(19) . . . . ? N4 O8 Cu2 O10 134.03(18) . . . . ? N4 O8 Cu2 N5 -44.79(18) . . . . ? N4 O8 Cu2 N6 -86.6(5) . . . . ? N4 O8 Cu2 O9 -138.36(18) . . . . ? N4 O8 Cu2 O11 47.89(18) . . . . ? C21 N5 Cu2 O10 -142(2) . . . . ? C25 N5 Cu2 O10 51(2) . . . . ? C21 N5 Cu2 O8 11.6(2) . . . . ? C25 N5 Cu2 O8 -155.19(19) . . . . ? C21 N5 Cu2 N6 -176.6(2) . . . . ? C25 N5 Cu2 N6 16.64(19) . . . . ? C21 N5 Cu2 O9 92.9(2) . . . . ? C25 N5 Cu2 O9 -73.88(19) . . . . ? C21 N5 Cu2 O11 -71.9(2) . . . . ? C25 N5 Cu2 O11 121.31(19) . . . . ? C30 N6 Cu2 O10 -5.1(3) . . . . ? C26 N6 Cu2 O10 167.4(2) . . . . ? C30 N6 Cu2 O8 -144.3(4) . . . . ? C26 N6 Cu2 O8 28.2(5) . . . . ? C30 N6 Cu2 N5 173.4(3) . . . . ? C26 N6 Cu2 N5 -14.1(2) . . . . ? C30 N6 Cu2 O9 -93.3(3) . . . . ? C26 N6 Cu2 O9 79.2(2) . . . . ? C30 N6 Cu2 O11 82.9(3) . . . . ? C26 N6 Cu2 O11 -104.6(2) . . . . ? Cl3 O11 Cu2 O10 136.2(2) . . . . ? Cl3 O11 Cu2 O8 -130.1(2) . . . . ? Cl3 O11 Cu2 N5 -41.3(2) . . . . ? Cl3 O11 Cu2 N6 40.9(3) . . . . ? Cl3 O11 Cu2 O9 -152.6(2) . . . . ? Cu1 O4 Cl1 O6 -87.07(19) . . . . ? Cu1 O4 Cl1 O5 34.1(2) . . . . ? Cu1 O4 Cl1 O7 152.39(15) . . . . ? Cu2 O11 Cl3 O13 63.9(3) . . . . ? Cu2 O11 Cl3 O14 -57.4(3) . . . . ? Cu2 O11 Cl3 O12 -175.0(2) . . . . ? O1 N1 C1 C2 178.7(3) . . . . ? C5 N1 C1 C2 -0.9(4) . . . . ? N1 C1 C2 C3 1.4(5) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? O1 N1 C5 C4 -179.9(2) . . . . ? C1 N1 C5 C4 -0.3(4) . . . . ? O1 N1 C5 C6 1.6(4) . . . . ? C1 N1 C5 C6 -178.8(3) . . . . ? C3 C4 C5 N1 0.9(4) . . . . ? C3 C4 C5 C6 179.5(3) . . . . ? C10 N2 C6 C7 -4.0(4) . . . . ? Cu1 N2 C6 C7 164.6(2) . . . . ? C10 N2 C6 C5 171.4(2) . . . . ? Cu1 N2 C6 C5 -19.9(3) . . . . ? N1 C5 C6 N2 34.2(4) . . . . ? C4 C5 C6 N2 -144.3(3) . . . . ? N1 C5 C6 C7 -150.3(3) . . . . ? C4 C5 C6 C7 31.2(4) . . . . ? N2 C6 C7 C8 2.4(4) . . . . ? C5 C6 C7 C8 -173.0(3) . . . . ? C6 C7 C8 C9 0.8(5) . . . . ? C7 C8 C9 C10 -2.5(5) . . . . ? C6 N2 C10 C9 2.3(4) . . . . ? Cu1 N2 C10 C9 -167.6(2) . . . . ? C6 N2 C10 C11 -176.7(2) . . . . ? Cu1 N2 C10 C11 13.4(3) . . . . ? C8 C9 C10 N2 1.0(4) . . . . ? C8 C9 C10 C11 179.8(3) . . . . ? C15 N3 C11 C12 -1.0(4) . . . . ? Cu1 N3 C11 C12 173.7(2) . . . . ? C15 N3 C11 C10 178.0(3) . . . . ? Cu1 N3 C11 C10 -7.4(3) . . . . ? N2 C10 C11 N3 -3.9(3) . . . . ? C9 C10 C11 N3 177.1(3) . . . . ? N2 C10 C11 C12 175.0(3) . . . . ? C9 C10 C11 C12 -3.9(4) . . . . ? N3 C11 C12 C13 0.1(4) . . . . ? C10 C11 C12 C13 -178.7(3) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? C12 C13 C14 C15 -0.5(5) . . . . ? C11 N3 C15 C14 1.1(5) . . . . ? Cu1 N3 C15 C14 -172.8(2) . . . . ? C13 C14 C15 N3 -0.3(5) . . . . ? O8 N4 C16 C17 -179.9(3) . . . . ? C20 N4 C16 C17 -1.0(4) . . . . ? N4 C16 C17 C18 -0.5(5) . . . . ? C16 C17 C18 C19 1.0(5) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? O8 N4 C20 C19 -179.2(2) . . . . ? C16 N4 C20 C19 1.9(4) . . . . ? O8 N4 C20 C21 -1.4(4) . . . . ? C16 N4 C20 C21 179.7(3) . . . . ? C18 C19 C20 N4 -1.4(4) . . . . ? C18 C19 C20 C21 -179.3(3) . . . . ? C25 N5 C21 C22 3.8(4) . . . . ? Cu2 N5 C21 C22 -162.1(2) . . . . ? C25 N5 C21 C20 -171.8(2) . . . . ? Cu2 N5 C21 C20 22.3(3) . . . . ? N4 C20 C21 N5 -35.4(4) . . . . ? C19 C20 C21 N5 142.4(3) . . . . ? N4 C20 C21 C22 149.0(3) . . . . ? C19 C20 C21 C22 -33.2(4) . . . . ? N5 C21 C22 C23 -1.9(4) . . . . ? C20 C21 C22 C23 173.7(3) . . . . ? C21 C22 C23 C24 -1.4(5) . . . . ? C22 C23 C24 C25 2.8(5) . . . . ? C21 N5 C25 C24 -2.4(4) . . . . ? Cu2 N5 C25 C24 165.1(2) . . . . ? C21 N5 C25 C26 176.3(2) . . . . ? Cu2 N5 C25 C26 -16.1(3) . . . . ? C23 C24 C25 N5 -0.9(4) . . . . ? C23 C24 C25 C26 -179.5(3) . . . . ? C30 N6 C26 C27 1.3(4) . . . . ? Cu2 N6 C26 C27 -171.8(2) . . . . ? C30 N6 C26 C25 -177.6(3) . . . . ? Cu2 N6 C26 C25 9.3(3) . . . . ? N5 C25 C26 N6 4.4(3) . . . . ? C24 C25 C26 N6 -176.8(3) . . . . ? N5 C25 C26 C27 -174.4(3) . . . . ? C24 C25 C26 C27 4.3(5) . . . . ? N6 C26 C27 C28 -0.6(5) . . . . ? C25 C26 C27 C28 178.2(3) . . . . ? C26 C27 C28 C29 -0.7(5) . . . . ? C27 C28 C29 C30 1.2(5) . . . . ? C26 N6 C30 C29 -0.7(5) . . . . ? Cu2 N6 C30 C29 171.3(3) . . . . ? C28 C29 C30 N6 -0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.116 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.144 # Attachment '5.cif.cif' data_01src122 _database_code_depnum_ccdc_archive 'CCDC 659294' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 Cl2 Cu N3 O11' _chemical_formula_weight 545.72 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 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 10.354(2) _cell_length_b 16.323(3) _cell_length_c 11.593(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.57(3) _cell_angle_gamma 90.00 _cell_volume 1867.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9205 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 1.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8622 _exptl_absorpt_correction_T_max 0.9849 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 13783 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4213 _reflns_number_gt 2935 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4213 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.006 _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 C1 C 0.7369(3) 0.1778(2) 0.2897(3) 0.0240(7) Uani 1 1 d . . . H1 H 0.7161 0.2315 0.3103 0.029 Uiso 1 1 calc R . . C2 C 0.7508(3) 0.1632(2) 0.1772(3) 0.0284(8) Uani 1 1 d . . . H2 H 0.7432 0.2068 0.1212 0.034 Uiso 1 1 calc R . . C3 C 0.7758(3) 0.0848(2) 0.1469(3) 0.0297(8) Uani 1 1 d . . . H3 H 0.7825 0.0732 0.0686 0.036 Uiso 1 1 calc R . . C4 C 0.7911(3) 0.0228(2) 0.2316(3) 0.0240(7) Uani 1 1 d . . . H4 H 0.8075 -0.0316 0.2104 0.029 Uiso 1 1 calc R . . C5 C 0.7831(3) 0.0385(2) 0.3471(3) 0.0188(7) Uani 1 1 d . . . C6 C 0.8145(3) -0.02649(19) 0.4415(2) 0.0171(7) Uani 1 1 d . . . C7 C 0.8983(3) -0.0899(2) 0.4294(3) 0.0210(7) Uani 1 1 d . . . H7 H 0.9371 -0.0894 0.3648 0.025 Uiso 1 1 calc R . . C8 C 0.9254(3) -0.1534(2) 0.5111(3) 0.0241(7) Uani 1 1 d . . . H8 H 0.9800 -0.1983 0.5018 0.029 Uiso 1 1 calc R . . C9 C 0.8722(3) -0.1511(2) 0.6065(3) 0.0221(7) Uani 1 1 d . . . H9 H 0.8905 -0.1941 0.6643 0.027 Uiso 1 1 calc R . . C10 C 0.7917(3) -0.08538(19) 0.6175(3) 0.0172(7) Uani 1 1 d . . . C11 C 0.7427(3) -0.08243(18) 0.7259(3) 0.0162(7) Uani 1 1 d . . . C12 C 0.8186(3) -0.1167(2) 0.8349(3) 0.0240(8) Uani 1 1 d . . . H12 H 0.9044 -0.1402 0.8410 0.029 Uiso 1 1 calc R . . C13 C 0.7719(3) -0.1174(2) 0.9341(3) 0.0274(8) Uani 1 1 d . . . H13 H 0.8236 -0.1424 1.0075 0.033 Uiso 1 1 calc R . . C14 C 0.6483(3) -0.0809(2) 0.9254(3) 0.0248(8) Uani 1 1 d . . . H14 H 0.6136 -0.0813 0.9925 0.030 Uiso 1 1 calc R . . C15 C 0.5769(3) -0.04439(19) 0.8188(3) 0.0202(7) Uani 1 1 d . . . H15 H 0.4936 -0.0177 0.8129 0.024 Uiso 1 1 calc R . . N1 N 0.7526(2) 0.11669(16) 0.3711(2) 0.0175(6) Uani 1 1 d . . . N2 N 0.7620(2) -0.02350(15) 0.5354(2) 0.0144(5) Uani 1 1 d . . . N3 N 0.6239(2) -0.04601(15) 0.7220(2) 0.0150(5) Uani 1 1 d . . . O1 O 0.7440(2) 0.13809(13) 0.48083(17) 0.0202(5) Uani 1 1 d . . . O2 O 0.54427(18) -0.00921(12) 0.62148(16) 0.0157(5) Uani 1 1 d . . . O3 O 0.7543(2) 0.11907(14) 0.74810(18) 0.0275(6) Uani 1 1 d . . . O4 O 0.9619(3) 0.04987(15) 0.8231(3) 0.0491(8) Uani 1 1 d . . . O5 O 0.9605(3) 0.18543(16) 0.7600(2) 0.0410(7) Uani 1 1 d . . . O6 O 0.9032(2) 0.15652(16) 0.93610(18) 0.0357(6) Uani 1 1 d . . . O7 O 0.5177(2) 0.30406(16) 0.4328(2) 0.0408(7) Uani 1 1 d . . . O8 O 0.4433(2) 0.23479(15) 0.2472(2) 0.0412(7) Uani 1 1 d . . . O9 O 0.4277(2) 0.37678(15) 0.2523(2) 0.0385(6) Uani 1 1 d . . . O10 O 0.2851(2) 0.29732(17) 0.3289(2) 0.0405(7) Uani 1 1 d . . . O11 O 0.5050(2) 0.15189(17) 0.5445(2) 0.0240(6) Uani 1 1 d . . . Cl1 Cl 0.89596(7) 0.12720(5) 0.81795(7) 0.0226(2) Uani 1 1 d . . . Cl2 Cl 0.41738(7) 0.30265(5) 0.31532(6) 0.0216(2) Uani 1 1 d . . . Cu1 Cu 0.63980(3) 0.06657(2) 0.54802(3) 0.01581(13) Uani 1 1 d . . . H11A H 0.477(4) 0.151(3) 0.609(4) 0.051(13) Uiso 1 1 d . . . H11B H 0.506(3) 0.188(2) 0.518(3) 0.004(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0211(17) 0.0208(19) 0.0279(17) 0.0085(15) 0.0041(14) -0.0006(14) C2 0.0241(17) 0.035(2) 0.0238(17) 0.0076(16) 0.0040(14) -0.0074(16) C3 0.0291(19) 0.040(2) 0.0215(17) -0.0021(16) 0.0097(15) -0.0102(17) C4 0.0248(17) 0.025(2) 0.0233(17) -0.0053(15) 0.0092(14) -0.0031(15) C5 0.0149(15) 0.0211(17) 0.0214(16) -0.0019(14) 0.0071(13) -0.0036(13) C6 0.0153(14) 0.0166(17) 0.0190(15) -0.0025(13) 0.0046(12) -0.0020(14) C7 0.0174(15) 0.0221(18) 0.0250(16) -0.0064(14) 0.0085(13) -0.0023(14) C8 0.0150(15) 0.0182(18) 0.0380(19) -0.0046(16) 0.0064(14) 0.0015(14) C9 0.0164(15) 0.0161(17) 0.0302(17) 0.0020(15) 0.0017(13) 0.0018(13) C10 0.0125(14) 0.0169(17) 0.0204(15) -0.0011(13) 0.0020(12) -0.0020(13) C11 0.0165(15) 0.0109(16) 0.0194(15) 0.0020(12) 0.0028(12) -0.0023(13) C12 0.0178(16) 0.0224(19) 0.0278(17) 0.0075(15) 0.0009(14) -0.0020(14) C13 0.0280(18) 0.031(2) 0.0179(16) 0.0064(15) -0.0017(14) -0.0051(16) C14 0.0291(18) 0.025(2) 0.0186(16) 0.0034(14) 0.0050(14) -0.0055(15) C15 0.0223(16) 0.0183(17) 0.0212(16) -0.0011(14) 0.0082(13) -0.0012(14) N1 0.0136(13) 0.0205(15) 0.0187(13) 0.0017(11) 0.0052(10) -0.0019(11) N2 0.0116(12) 0.0126(14) 0.0178(12) -0.0011(11) 0.0025(10) -0.0025(10) N3 0.0169(13) 0.0113(13) 0.0136(12) 0.0006(10) -0.0003(10) -0.0019(10) O1 0.0271(12) 0.0180(12) 0.0185(10) -0.0017(9) 0.0113(9) -0.0015(10) O2 0.0145(10) 0.0167(11) 0.0141(10) 0.0035(9) 0.0015(8) 0.0017(9) O3 0.0173(11) 0.0344(15) 0.0275(12) -0.0095(11) 0.0018(10) -0.0039(10) O4 0.0336(15) 0.0246(15) 0.083(2) -0.0130(14) 0.0087(14) 0.0083(12) O5 0.0411(15) 0.0385(16) 0.0522(16) -0.0087(13) 0.0273(13) -0.0180(13) O6 0.0347(14) 0.0486(17) 0.0207(12) -0.0072(11) 0.0037(10) -0.0012(13) O7 0.0431(15) 0.0403(16) 0.0300(13) 0.0001(12) -0.0027(12) 0.0021(13) O8 0.0437(15) 0.0319(16) 0.0502(16) -0.0181(13) 0.0175(13) -0.0014(12) O9 0.0408(15) 0.0274(15) 0.0484(15) 0.0171(12) 0.0153(13) 0.0019(12) O10 0.0319(14) 0.0492(17) 0.0489(15) -0.0063(13) 0.0249(12) -0.0107(13) O11 0.0295(14) 0.0192(15) 0.0253(14) 0.0060(12) 0.0114(11) 0.0065(12) Cl1 0.0184(4) 0.0195(4) 0.0288(4) -0.0063(3) 0.0057(3) -0.0010(3) Cl2 0.0245(4) 0.0183(4) 0.0228(4) 0.0001(3) 0.0082(3) -0.0023(3) Cu1 0.0172(2) 0.0130(2) 0.0180(2) 0.00148(16) 0.00651(15) 0.00111(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.349(4) . ? C1 C2 1.376(4) . ? C2 C3 1.372(5) . ? C3 C4 1.386(5) . ? C4 C5 1.391(4) . ? C5 N1 1.363(4) . ? C5 C6 1.488(4) . ? C6 N2 1.357(4) . ? C6 C7 1.384(4) . ? C7 C8 1.376(4) . ? C8 C9 1.376(4) . ? C9 C10 1.387(4) . ? C10 N2 1.358(4) . ? C10 C11 1.491(4) . ? C11 N3 1.355(4) . ? C11 C12 1.389(4) . ? C12 C13 1.376(4) . ? C13 C14 1.387(5) . ? C14 C15 1.370(4) . ? C15 N3 1.351(4) . ? N1 O1 1.348(3) . ? N2 Cu1 1.974(2) . ? N3 O2 1.349(3) . ? O1 Cu1 1.908(2) . ? O2 Cu1 1.935(2) . ? O3 Cl1 1.451(2) . ? O3 Cu1 2.421(2) . ? O4 Cl1 1.428(3) . ? O5 Cl1 1.440(2) . ? O6 Cl1 1.431(2) . ? O7 Cl2 1.442(2) . ? O8 Cl2 1.432(2) . ? O9 Cl2 1.434(2) . ? O10 Cl2 1.428(2) . ? O11 Cu1 1.964(2) . ? 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 C1 C2 120.6(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 119.3(3) . . ? C3 C4 C5 121.3(3) . . ? N1 C5 C4 117.0(3) . . ? N1 C5 C6 122.1(3) . . ? C4 C5 C6 120.8(3) . . ? N2 C6 C7 121.6(3) . . ? N2 C6 C5 120.8(3) . . ? C7 C6 C5 117.6(3) . . ? C8 C7 C6 119.9(3) . . ? C9 C8 C7 118.9(3) . . ? C8 C9 C10 119.5(3) . . ? N2 C10 C9 121.7(3) . . ? N2 C10 C11 120.2(3) . . ? C9 C10 C11 118.0(3) . . ? N3 C11 C12 117.8(3) . . ? N3 C11 C10 121.5(2) . . ? C12 C11 C10 120.7(3) . . ? C13 C12 C11 121.2(3) . . ? C12 C13 C14 119.0(3) . . ? C15 C14 C13 119.1(3) . . ? N3 C15 C14 120.6(3) . . ? O1 N1 C1 116.1(3) . . ? O1 N1 C5 121.4(2) . . ? C1 N1 C5 122.4(3) . . ? C6 N2 C10 118.4(3) . . ? C6 N2 Cu1 120.5(2) . . ? C10 N2 Cu1 121.11(19) . . ? O2 N3 C15 115.4(2) . . ? O2 N3 C11 122.4(2) . . ? C15 N3 C11 122.2(3) . . ? N1 O1 Cu1 115.69(17) . . ? N3 O2 Cu1 113.88(16) . . ? Cl1 O3 Cu1 133.41(13) . . ? O4 Cl1 O6 111.68(17) . . ? O4 Cl1 O5 108.63(17) . . ? O6 Cl1 O5 109.14(15) . . ? O4 Cl1 O3 109.42(15) . . ? O6 Cl1 O3 108.47(14) . . ? O5 Cl1 O3 109.48(15) . . ? O10 Cl2 O8 111.08(15) . . ? O10 Cl2 O9 109.21(15) . . ? O8 Cl2 O9 108.47(15) . . ? O10 Cl2 O7 109.78(15) . . ? O8 Cl2 O7 109.34(16) . . ? O9 Cl2 O7 108.92(15) . . ? O1 Cu1 O2 176.54(8) . . ? O1 Cu1 O11 92.49(11) . . ? O2 Cu1 O11 90.45(11) . . ? O1 Cu1 N2 88.36(9) . . ? O2 Cu1 N2 88.90(9) . . ? O11 Cu1 N2 173.94(10) . . ? O1 Cu1 O3 90.04(8) . . ? O2 Cu1 O3 88.41(8) . . ? O11 Cu1 O3 84.75(9) . . ? N2 Cu1 O3 101.25(9) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.543 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.106