# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Maji, Tapas' 'Chakraborty, Anindita' 'L. Gurunatha' 'A. Muthulakshmi' 'Dutta, Sudipta' 'Pati, Swapan' _publ_contact_author_name 'Maji, Tapas' _publ_contact_author_email tmaji@jncasr.ac.in _publ_section_title ; Assembly of trinuclear and tetranuclear building units of Cu2+ towards two 1D magnetic systems: Synthesis and magneto-structural correlations ; # Attachment '- mcif.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 861308' #TrackingRef '- mcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H31 Cu3 N9 O6' _chemical_formula_sum 'C40 H31 Cu3 N9 O6' _chemical_formula_weight 924.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 8.4798(3) _cell_length_b 20.8033(7) _cell_length_c 21.2503(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.601(2) _cell_angle_gamma 90.00 _cell_volume 3744.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Parallelepiped _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 1.751 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7209 _exptl_absorpt_correction_T_max 0.8726 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 24643 _diffrn_reflns_av_R_equivalents 0.1056 _diffrn_reflns_av_sigmaI/netI 0.1548 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8515 _reflns_number_gt 4036 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker,2000)' _computing_cell_refinement SMART _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 1.4.1' _computing_publication_material 'PLATON (Spek, 2003)' _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^ > 2\s(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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8515 _refine_ls_number_parameters 523 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1653 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.971 _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 0.3246(8) 0.2346(3) -0.1766(3) 0.0477(17) Uani 1 1 d . . . H1 H 0.3703 0.2740 -0.1856 0.057 Uiso 1 1 calc R . . C2 C 0.2297(8) 0.2054(3) -0.2231(3) 0.0545(19) Uani 1 1 d . . . H2 H 0.2117 0.2244 -0.2623 0.065 Uiso 1 1 calc R . . C3 C 0.1637(9) 0.1477(3) -0.2092(3) 0.060(2) Uani 1 1 d . . . H3 H 0.0992 0.1268 -0.2393 0.072 Uiso 1 1 calc R . . C4 C 0.1924(8) 0.1202(3) -0.1503(3) 0.0550(19) Uani 1 1 d . . . H4 H 0.1475 0.0808 -0.1406 0.066 Uiso 1 1 calc R . . C5 C 0.2887(7) 0.1520(3) -0.1061(3) 0.0367(15) Uani 1 1 d . . . C6 C 0.3204(7) 0.1294(3) -0.0407(3) 0.0360(15) Uani 1 1 d . . . C7 C 0.2772(7) 0.0643(3) -0.0193(3) 0.0395(16) Uani 1 1 d . . . C8 C 0.1913(8) 0.0559(3) 0.0338(3) 0.0535(19) Uani 1 1 d . . . H8 H 0.1606 0.0917 0.0565 0.064 Uiso 1 1 calc R . . C9 C 0.1505(9) -0.0045(4) 0.0536(4) 0.073(2) Uani 1 1 d . . . H9 H 0.0912 -0.0095 0.0891 0.088 Uiso 1 1 calc R . . C10 C 0.1983(10) -0.0582(3) 0.0204(4) 0.074(2) Uani 1 1 d . . . H10 H 0.1698 -0.0992 0.0333 0.089 Uiso 1 1 calc R . . C11 C 0.2867(9) -0.0511(3) -0.0309(4) 0.068(2) Uani 1 1 d . . . H11 H 0.3213 -0.0870 -0.0524 0.082 Uiso 1 1 calc R . . C12 C 0.3251(8) 0.0102(3) -0.0510(4) 0.0570(19) Uani 1 1 d . . . H12 H 0.3842 0.0150 -0.0866 0.068 Uiso 1 1 calc R . . C13 C 0.2143(7) 0.4960(3) 0.0608(3) 0.0439(17) Uani 1 1 d . . . H13 H 0.2024 0.4801 0.1012 0.053 Uiso 1 1 calc R . . C14 C 0.1544(8) 0.5567(3) 0.0458(3) 0.0501(18) Uani 1 1 d . . . H14 H 0.1036 0.5809 0.0757 0.060 Uiso 1 1 calc R . . C15 C 0.1717(8) 0.5799(3) -0.0132(4) 0.0525(19) Uani 1 1 d . . . H15 H 0.1326 0.6204 -0.0241 0.063 Uiso 1 1 calc R . . C16 C 0.2477(7) 0.5433(3) -0.0574(3) 0.0449(17) Uani 1 1 d . . . H16 H 0.2623 0.5592 -0.0976 0.054 Uiso 1 1 calc R . . C17 C 0.3014(7) 0.4823(3) -0.0401(3) 0.0353(15) Uani 1 1 d . . . C18 C 0.3709(7) 0.4358(3) -0.0839(3) 0.0340(14) Uani 1 1 d . . . C19 C 0.3727(7) 0.4453(3) -0.1526(3) 0.0366(15) Uani 1 1 d . . . C20 C 0.4688(7) 0.4895(3) -0.1806(3) 0.0461(17) Uani 1 1 d . . . H20 H 0.5294 0.5175 -0.1555 0.055 Uiso 1 1 calc R . . C21 C 0.4766(9) 0.4930(3) -0.2454(4) 0.058(2) Uani 1 1 d . . . H21 H 0.5415 0.5232 -0.2634 0.070 Uiso 1 1 calc R . . C22 C 0.3883(10) 0.4517(4) -0.2832(3) 0.063(2) Uani 1 1 d . . . H22 H 0.3956 0.4534 -0.3267 0.076 Uiso 1 1 calc R . . C23 C 0.2899(8) 0.4084(3) -0.2571(4) 0.059(2) Uani 1 1 d . . . H23 H 0.2287 0.3808 -0.2826 0.071 Uiso 1 1 calc R . . C24 C 0.2823(7) 0.4058(3) -0.1925(3) 0.0454(17) Uani 1 1 d . . . H24 H 0.2141 0.3764 -0.1750 0.054 Uiso 1 1 calc R . . C25 C 0.3669(7) 0.1363(3) 0.1985(3) 0.0495(18) Uani 1 1 d . . . H25 H 0.4151 0.1081 0.1713 0.059 Uiso 1 1 calc R . . C26 C 0.3075(8) 0.1128(3) 0.2522(4) 0.062(2) Uani 1 1 d . . . H26 H 0.3153 0.0693 0.2616 0.075 Uiso 1 1 calc R . . C27 C 0.2354(8) 0.1543(3) 0.2925(3) 0.057(2) Uani 1 1 d . . . H27 H 0.1937 0.1390 0.3294 0.068 Uiso 1 1 calc R . . C28 C 0.2257(7) 0.2183(3) 0.2779(3) 0.0448(17) Uani 1 1 d . . . H28 H 0.1762 0.2468 0.3044 0.054 Uiso 1 1 calc R . . C29 C 0.2906(7) 0.2399(3) 0.2232(3) 0.0371(15) Uani 1 1 d . . . C30 C 0.2820(7) 0.3073(3) 0.2000(3) 0.0340(14) Uani 1 1 d . . . C31 C 0.1879(7) 0.3582(3) 0.2299(3) 0.0335(14) Uani 1 1 d . . . C32 C 0.2149(8) 0.3752(3) 0.2927(3) 0.0501(18) Uani 1 1 d . . . H32 H 0.2931 0.3546 0.3173 0.060 Uiso 1 1 calc R . . C33 C 0.1242(9) 0.4233(3) 0.3187(3) 0.058(2) Uani 1 1 d . . . H33 H 0.1407 0.4344 0.3609 0.069 Uiso 1 1 calc R . . C34 C 0.0114(9) 0.4542(3) 0.2825(4) 0.063(2) Uani 1 1 d . . . H34 H -0.0478 0.4867 0.3001 0.075 Uiso 1 1 calc R . . C35 C -0.0156(9) 0.4381(3) 0.2211(4) 0.066(2) Uani 1 1 d . . . H35 H -0.0932 0.4595 0.1969 0.079 Uiso 1 1 calc R . . C36 C 0.0722(8) 0.3896(3) 0.1940(3) 0.0496(18) Uani 1 1 d . . . H36 H 0.0529 0.3785 0.1519 0.060 Uiso 1 1 calc R . . C37 C 0.8006(8) 0.2409(3) 0.1126(3) 0.0430(16) Uani 1 1 d . . . C38 C 0.9576(8) 0.2100(4) 0.1239(4) 0.078(3) Uani 1 1 d . . . H38A H 0.9464 0.1724 0.1496 0.117 Uiso 1 1 calc R . . H38B H 1.0285 0.2397 0.1450 0.117 Uiso 1 1 calc R . . H38C H 0.9990 0.1978 0.0843 0.117 Uiso 1 1 calc R . . C39 C 0.8394(10) 0.2389(5) -0.0604(5) 0.100(3) Uani 1 1 d U . . C40 C 1.0743(9) 0.2831(4) -0.0257(4) 0.069(3) Uani 1 1 d . . . N1 N 0.3538(5) 0.2092(2) -0.1200(2) 0.0362(12) Uani 1 1 d . . . N2 N 0.3892(5) 0.1728(2) -0.0043(2) 0.0347(12) Uani 1 1 d . . . N3 N 0.2880(5) 0.4600(2) 0.0193(2) 0.0337(12) Uani 1 1 d . . . N4 N 0.4178(5) 0.3827(2) -0.0564(2) 0.0338(12) Uani 1 1 d . . . N5 N 0.3580(6) 0.1984(2) 0.1838(2) 0.0392(13) Uani 1 1 d . . . N6 N 0.3547(6) 0.3161(2) 0.1481(2) 0.0361(12) Uani 1 1 d . . . N7 N 0.7133(7) 0.2271(2) -0.0647(3) 0.0489(15) Uani 1 1 d . . . N8 N 0.9867(8) 0.2488(4) -0.0633(4) 0.119(3) Uani 1 1 d U . . N9 N 1.1628(7) 0.3111(3) 0.0040(3) 0.0610(18) Uani 1 1 d . . . O1 O 0.4140(5) 0.16051(18) 0.0563(2) 0.0436(11) Uani 1 1 d . . . O2 O 0.4755(5) 0.33566(17) -0.09062(18) 0.0387(10) Uani 1 1 d . . . O3 O 0.3527(5) 0.37477(17) 0.12245(19) 0.0460(12) Uani 1 1 d . . . O4 O 0.5008(4) 0.29236(16) 0.03559(17) 0.0324(9) Uani 1 1 d . . . H37 H 0.5800 0.2989 0.0452 0.039 Uiso 1 1 d R . . O5 O 0.6839(5) 0.2149(2) 0.1372(2) 0.0484(12) Uani 1 1 d . . . O6 O 0.7929(5) 0.2906(2) 0.0802(2) 0.0621(14) Uani 1 1 d . . . Cu1 Cu 0.46569(8) 0.25177(3) -0.04651(3) 0.0331(2) Uani 1 1 d . . . Cu2 Cu 0.37557(9) 0.37164(3) 0.03264(3) 0.0347(2) Uani 1 1 d . . . Cu3 Cu 0.44595(8) 0.23920(3) 0.10765(3) 0.0350(2) 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 0.047(4) 0.051(4) 0.045(5) 0.005(4) 0.003(4) -0.004(3) C2 0.062(5) 0.059(5) 0.043(5) 0.014(4) -0.005(4) -0.001(4) C3 0.075(6) 0.059(5) 0.043(5) -0.008(4) -0.017(4) -0.011(4) C4 0.060(5) 0.048(4) 0.056(5) 0.001(4) -0.009(4) -0.012(4) C5 0.033(4) 0.038(4) 0.039(4) -0.006(3) 0.003(3) 0.002(3) C6 0.040(4) 0.029(3) 0.039(4) 0.000(3) 0.001(3) 0.002(3) C7 0.036(4) 0.035(4) 0.047(4) 0.005(3) -0.001(3) 0.001(3) C8 0.058(5) 0.041(4) 0.063(5) -0.005(3) 0.008(4) -0.004(3) C9 0.082(6) 0.057(5) 0.080(6) 0.023(5) 0.014(5) -0.018(4) C10 0.104(7) 0.029(4) 0.086(7) 0.016(4) -0.015(5) -0.016(4) C11 0.068(6) 0.038(5) 0.097(7) -0.002(4) -0.015(5) -0.001(4) C12 0.056(5) 0.048(5) 0.067(5) -0.008(4) 0.005(4) -0.005(4) C13 0.055(4) 0.034(4) 0.043(4) -0.002(3) 0.009(3) 0.005(3) C14 0.055(5) 0.038(4) 0.057(5) -0.007(3) 0.001(4) 0.012(3) C15 0.060(5) 0.028(4) 0.070(6) 0.004(4) 0.006(4) 0.005(3) C16 0.056(4) 0.033(4) 0.046(4) 0.003(3) 0.004(3) 0.003(3) C17 0.041(4) 0.031(3) 0.033(4) 0.003(3) -0.007(3) -0.004(3) C18 0.034(4) 0.035(4) 0.033(4) -0.002(3) -0.003(3) -0.004(3) C19 0.037(4) 0.032(3) 0.040(4) 0.005(3) 0.000(3) -0.001(3) C20 0.046(4) 0.045(4) 0.047(5) 0.007(3) 0.001(3) 0.005(3) C21 0.071(6) 0.051(5) 0.055(5) 0.021(4) 0.016(4) 0.011(4) C22 0.094(7) 0.061(5) 0.035(5) 0.007(4) 0.003(4) 0.019(5) C23 0.066(5) 0.057(5) 0.053(5) -0.007(4) -0.013(4) 0.009(4) C24 0.053(4) 0.032(4) 0.051(5) 0.004(3) -0.004(4) 0.001(3) C25 0.052(4) 0.039(4) 0.059(5) 0.006(3) 0.011(4) 0.010(3) C26 0.080(6) 0.041(4) 0.068(6) 0.022(4) 0.028(4) 0.005(4) C27 0.064(5) 0.058(5) 0.049(5) 0.019(4) 0.016(4) 0.000(4) C28 0.044(4) 0.047(4) 0.043(4) 0.012(3) 0.008(3) 0.007(3) C29 0.035(4) 0.040(4) 0.036(4) 0.002(3) 0.003(3) 0.001(3) C30 0.033(4) 0.042(4) 0.027(4) -0.001(3) 0.000(3) 0.004(3) C31 0.042(4) 0.030(3) 0.029(4) -0.005(3) 0.004(3) -0.003(3) C32 0.050(4) 0.056(4) 0.044(5) -0.007(3) 0.003(3) 0.005(3) C33 0.067(5) 0.066(5) 0.042(5) -0.014(4) 0.011(4) -0.001(4) C34 0.070(6) 0.053(5) 0.067(6) -0.008(4) 0.019(5) 0.004(4) C35 0.068(6) 0.062(5) 0.067(6) 0.009(4) 0.002(5) 0.015(4) C36 0.063(5) 0.048(4) 0.038(4) 0.002(3) 0.004(4) 0.010(4) C37 0.044(4) 0.048(4) 0.035(4) -0.001(3) -0.013(3) 0.004(4) C38 0.037(4) 0.095(6) 0.101(7) 0.040(5) -0.009(4) -0.003(4) C39 0.034(4) 0.151(6) 0.118(6) -0.096(5) 0.024(4) -0.019(4) C40 0.039(5) 0.081(6) 0.089(7) -0.037(5) 0.014(5) -0.010(4) N1 0.040(3) 0.029(3) 0.040(3) 0.002(2) 0.005(3) 0.002(2) N2 0.040(3) 0.029(3) 0.035(3) -0.004(2) 0.000(3) -0.002(2) N3 0.033(3) 0.031(3) 0.037(3) -0.003(2) 0.001(2) 0.000(2) N4 0.038(3) 0.031(3) 0.032(3) 0.001(2) 0.000(2) 0.004(2) N5 0.044(3) 0.039(3) 0.035(3) 0.005(2) 0.005(3) -0.001(3) N6 0.040(3) 0.035(3) 0.033(3) 0.003(2) 0.001(2) -0.003(2) N7 0.048(4) 0.046(3) 0.052(4) -0.004(3) 0.000(3) 0.010(3) N8 0.048(4) 0.174(6) 0.137(6) -0.101(5) 0.023(4) -0.019(4) N9 0.042(4) 0.055(4) 0.086(5) -0.004(3) 0.005(4) -0.005(3) O1 0.065(3) 0.032(2) 0.033(3) 0.002(2) -0.007(2) -0.002(2) O2 0.049(3) 0.030(2) 0.038(3) 0.0031(19) 0.011(2) 0.0075(19) O3 0.077(3) 0.025(2) 0.037(3) 0.0010(19) 0.017(2) 0.000(2) O4 0.026(2) 0.032(2) 0.039(3) 0.0004(18) 0.0000(18) -0.0013(17) O5 0.036(3) 0.060(3) 0.050(3) 0.019(2) 0.003(2) 0.000(2) O6 0.045(3) 0.055(3) 0.086(4) 0.029(3) -0.003(3) -0.006(2) Cu1 0.0360(4) 0.0303(4) 0.0331(4) 0.0007(3) 0.0016(3) -0.0011(3) Cu2 0.0419(5) 0.0290(4) 0.0334(4) 0.0011(3) 0.0048(3) 0.0018(3) Cu3 0.0411(5) 0.0315(4) 0.0330(5) 0.0028(3) 0.0069(3) 0.0016(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.327(8) . ? C1 C2 1.386(9) . ? C1 H1 0.9300 . ? C2 C3 1.361(9) . ? C2 H2 0.9300 . ? C3 C4 1.389(9) . ? C3 H3 0.9300 . ? C4 C5 1.385(8) . ? C4 H4 0.9300 . ? C5 N1 1.350(7) . ? C5 C6 1.479(8) . ? C6 N2 1.309(7) . ? C6 C7 1.480(8) . ? C7 C12 1.382(8) . ? C7 C8 1.383(8) . ? C8 C9 1.376(8) . ? C8 H8 0.9300 . ? C9 C10 1.393(10) . ? C9 H9 0.9300 . ? C10 C11 1.359(10) . ? C10 H10 0.9300 . ? C11 C12 1.389(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N3 1.334(6) . ? C13 C14 1.392(8) . ? C13 H13 0.9300 . ? C14 C15 1.358(9) . ? C14 H14 0.9300 . ? C15 C16 1.390(8) . ? C15 H15 0.9300 . ? C16 C17 1.392(7) . ? C16 H16 0.9300 . ? C17 N3 1.356(7) . ? C17 C18 1.482(7) . ? C18 N4 1.303(7) . ? C18 C19 1.475(8) . ? C19 C20 1.381(7) . ? C19 C24 1.387(8) . ? C20 C21 1.384(9) . ? C20 H20 0.9300 . ? C21 C22 1.373(9) . ? C21 H21 0.9300 . ? C22 C23 1.363(9) . ? C22 H22 0.9300 . ? C23 C24 1.378(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N5 1.331(7) . ? C25 C26 1.358(8) . ? C25 H25 0.9300 . ? C26 C27 1.379(9) . ? C26 H26 0.9300 . ? C27 C28 1.367(8) . ? C27 H27 0.9300 . ? C28 C29 1.385(7) . ? C28 H28 0.9300 . ? C29 N5 1.348(7) . ? C29 C30 1.487(8) . ? C30 N6 1.301(6) . ? C30 C31 1.486(7) . ? C31 C36 1.380(8) . ? C31 C32 1.390(8) . ? C32 C33 1.391(8) . ? C32 H32 0.9300 . ? C33 C34 1.361(10) . ? C33 H33 0.9300 . ? C34 C35 1.358(10) . ? C34 H34 0.9300 . ? C35 C36 1.393(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 O6 1.242(7) . ? C37 O5 1.262(7) . ? C37 C38 1.488(8) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N7 1.097(8) . ? C39 N8 1.270(9) . ? C40 N9 1.121(9) . ? C40 N8 1.283(10) . ? N1 Cu1 1.997(5) . ? N2 O1 1.322(6) . ? N2 Cu1 1.993(4) . ? N3 Cu2 1.997(4) . ? N4 O2 1.327(5) . ? N4 Cu2 1.954(5) . ? N5 Cu3 2.000(4) . ? N6 O3 1.337(5) . ? N6 Cu3 1.989(5) . ? N7 Cu1 2.212(5) . ? N9 Cu2 2.261(6) 1_655 ? O1 Cu3 1.979(4) . ? O2 Cu1 1.984(4) . ? O3 Cu2 1.928(4) . ? O4 Cu1 1.949(4) . ? O4 Cu2 1.961(3) . ? O4 Cu3 1.962(3) . ? O4 H37 0.7064 . ? O5 Cu3 2.146(4) . ? Cu2 N9 2.261(6) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.3(6) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 117.6(7) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 120.1(7) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.2(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 120.5(6) . . ? N1 C5 C6 115.3(5) . . ? C4 C5 C6 124.1(6) . . ? N2 C6 C5 113.1(5) . . ? N2 C6 C7 124.0(6) . . ? C5 C6 C7 122.8(6) . . ? C12 C7 C8 118.2(6) . . ? C12 C7 C6 120.8(6) . . ? C8 C7 C6 120.9(5) . . ? C9 C8 C7 121.0(6) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.7(7) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.2(7) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.6(7) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C7 C12 C11 121.3(7) . . ? C7 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? N3 C13 C14 122.4(6) . . ? N3 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 118.7(6) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 120.1(6) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 118.6(6) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? N3 C17 C16 121.1(5) . . ? N3 C17 C18 114.4(5) . . ? C16 C17 C18 124.4(5) . . ? N4 C18 C19 122.8(5) . . ? N4 C18 C17 113.2(5) . . ? C19 C18 C17 123.8(5) . . ? C20 C19 C24 116.9(6) . . ? C20 C19 C18 123.3(6) . . ? C24 C19 C18 119.7(5) . . ? C19 C20 C21 121.3(7) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 119.9(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.3(7) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.2(7) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C23 C24 C19 122.4(6) . . ? C23 C24 H24 118.8 . . ? C19 C24 H24 118.8 . . ? N5 C25 C26 121.8(6) . . ? N5 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C27 119.3(6) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C28 C27 C26 119.5(6) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 119.0(6) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? N5 C29 C28 120.7(5) . . ? N5 C29 C30 114.5(5) . . ? C28 C29 C30 124.7(5) . . ? N6 C30 C29 113.3(5) . . ? N6 C30 C31 123.1(5) . . ? C29 C30 C31 123.4(5) . . ? C36 C31 C32 119.5(6) . . ? C36 C31 C30 118.9(6) . . ? C32 C31 C30 121.6(6) . . ? C31 C32 C33 119.6(7) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 120.3(7) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 120.6(7) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.5(7) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 119.5(7) . . ? C31 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? O6 C37 O5 124.3(6) . . ? O6 C37 C38 118.3(6) . . ? O5 C37 C38 117.4(6) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C39 N8 171.7(9) . . ? N9 C40 N8 173.3(8) . . ? C1 N1 C5 119.2(6) . . ? C1 N1 Cu1 126.5(4) . . ? C5 N1 Cu1 113.8(4) . . ? C6 N2 O1 119.3(5) . . ? C6 N2 Cu1 116.6(4) . . ? O1 N2 Cu1 123.9(4) . . ? C13 N3 C17 119.0(5) . . ? C13 N3 Cu2 127.3(4) . . ? C17 N3 Cu2 113.6(4) . . ? C18 N4 O2 119.5(5) . . ? C18 N4 Cu2 117.9(4) . . ? O2 N4 Cu2 122.2(3) . . ? C25 N5 C29 119.8(5) . . ? C25 N5 Cu3 125.7(4) . . ? C29 N5 Cu3 114.5(4) . . ? C30 N6 O3 118.5(5) . . ? C30 N6 Cu3 117.5(4) . . ? O3 N6 Cu3 123.8(3) . . ? C39 N7 Cu1 149.7(6) . . ? C39 N8 C40 127.1(7) . . ? C40 N9 Cu2 161.1(7) . 1_655 ? N2 O1 Cu3 112.9(3) . . ? N4 O2 Cu1 111.4(3) . . ? N6 O3 Cu2 111.9(3) . . ? Cu1 O4 Cu2 105.98(17) . . ? Cu1 O4 Cu3 114.99(17) . . ? Cu2 O4 Cu3 110.59(16) . . ? Cu1 O4 H37 116.5 . . ? Cu2 O4 H37 110.7 . . ? Cu3 O4 H37 98.0 . . ? C37 O5 Cu3 121.5(4) . . ? O4 Cu1 O2 91.94(15) . . ? O4 Cu1 N2 89.67(18) . . ? O2 Cu1 N2 163.40(18) . . ? O4 Cu1 N1 160.03(16) . . ? O2 Cu1 N1 92.80(18) . . ? N2 Cu1 N1 80.4(2) . . ? O4 Cu1 N7 98.57(18) . . ? O2 Cu1 N7 93.48(17) . . ? N2 Cu1 N7 102.62(19) . . ? N1 Cu1 N7 100.49(19) . . ? O3 Cu2 N4 170.04(18) . . ? O3 Cu2 O4 94.32(16) . . ? N4 Cu2 O4 90.42(17) . . ? O3 Cu2 N3 93.18(18) . . ? N4 Cu2 N3 80.67(19) . . ? O4 Cu2 N3 167.32(16) . . ? O3 Cu2 N9 99.8(2) . 1_455 ? N4 Cu2 N9 89.1(2) . 1_455 ? O4 Cu2 N9 87.95(18) . 1_455 ? N3 Cu2 N9 100.8(2) . 1_455 ? O4 Cu3 O1 93.86(16) . . ? O4 Cu3 N6 89.69(17) . . ? O1 Cu3 N6 149.00(19) . . ? O4 Cu3 N5 168.67(17) . . ? O1 Cu3 N5 92.76(18) . . ? N6 Cu3 N5 79.93(19) . . ? O4 Cu3 O5 96.19(15) . . ? O1 Cu3 O5 94.01(17) . . ? N6 Cu3 O5 116.23(19) . . ? N5 Cu3 O5 92.51(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.932 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.105 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 861309' #TrackingRef '- mcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H35 Cl Cu4 N4 O15' _chemical_formula_sum 'C28 H35 Cl Cu4 N4 O15' _chemical_formula_weight 957.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbn21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 7.9039(2) _cell_length_b 15.7253(4) _cell_length_c 27.7552(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3449.73(16) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 2.587 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7820 _exptl_absorpt_correction_T_max 0.8603 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 35361 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.45 _reflns_number_total 6150 _reflns_number_gt 5295 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker,2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 1.4.1' _computing_publication_material 'PLATON (Spek, 2003)' _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^ > 2\s(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^)+(0.1210P)^2^+4.0368P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.52(3) _refine_ls_number_reflns 6150 _refine_ls_number_parameters 470 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1762 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6655(10) 0.2293(5) 0.2195(3) 0.0360(19) Uani 1 1 d . . . C2 C 0.6348(12) 0.2178(9) 0.2682(3) 0.056(3) Uani 1 1 d U . . H2 H 0.7212 0.2035 0.2894 0.067 Uiso 1 1 calc R . . C3 C 0.4697(14) 0.2285(10) 0.2838(3) 0.069(3) Uani 1 1 d U . . H3 H 0.4463 0.2228 0.3165 0.083 Uiso 1 1 calc R . . C4 C 0.3369(13) 0.2477(7) 0.2524(3) 0.050(2) Uani 1 1 d . . . H4 H 0.2270 0.2559 0.2634 0.060 Uiso 1 1 calc R . . C5 C 0.3770(10) 0.2537(5) 0.2043(3) 0.0317(17) Uani 1 1 d . . . C6 C 0.8327(10) 0.2266(6) 0.1962(3) 0.038(2) Uani 1 1 d . . . H6A H 0.9071 0.2664 0.2125 0.046 Uiso 1 1 calc R . . H6B H 0.8799 0.1702 0.2003 0.046 Uiso 1 1 calc R . . C7 C 0.2540(10) 0.2749(6) 0.1649(3) 0.0335(19) Uani 1 1 d . . . H7A H 0.1855 0.2256 0.1572 0.040 Uiso 1 1 calc R . . H7B H 0.1795 0.3205 0.1751 0.040 Uiso 1 1 calc R . . C8 C 0.3129(9) 0.5106(5) 0.2212(3) 0.0351(19) Uani 1 1 d . . . C9 C 0.3461(13) 0.5227(8) 0.2705(3) 0.057(3) Uani 1 1 d . . . H9 H 0.2595 0.5372 0.2917 0.068 Uiso 1 1 calc R . . C10 C 0.5066(14) 0.5128(10) 0.2865(4) 0.071(4) Uani 1 1 d . . . H10 H 0.5294 0.5182 0.3192 0.085 Uiso 1 1 calc R . . C11 C 0.1461(11) 0.5129(6) 0.1973(3) 0.039(2) Uani 1 1 d . . . H11A H 0.0946 0.5677 0.2038 0.046 Uiso 1 1 calc R . . H11B H 0.0748 0.4699 0.2120 0.046 Uiso 1 1 calc R . . C12 C 0.6011(10) 0.4871(5) 0.2062(3) 0.0322(18) Uani 1 1 d . . . C13 C 0.7230(10) 0.4685(6) 0.1664(3) 0.0308(18) Uani 1 1 d . . . H13A H 0.7921 0.5181 0.1599 0.037 Uiso 1 1 calc R . . H13B H 0.7971 0.4220 0.1756 0.037 Uiso 1 1 calc R . . C14 C 0.3069(12) 0.4915(5) 0.0213(3) 0.0365(19) Uani 1 1 d . . . H14A H 0.4051 0.5239 0.0112 0.044 Uiso 1 1 calc R . . H14B H 0.2173 0.5312 0.0292 0.044 Uiso 1 1 calc R . . C15 C 0.2512(10) 0.4353(5) -0.0183(3) 0.0278(18) Uani 1 1 d . . . C16 C 0.1765(15) 0.2954(6) -0.0377(4) 0.051(2) Uani 1 1 d . . . C17 C 0.150(2) 0.2092(7) -0.0149(5) 0.075(4) Uani 1 1 d . . . H17A H 0.2180 0.1672 -0.0317 0.089 Uiso 1 1 calc R . . H17B H 0.0322 0.1929 -0.0180 0.089 Uiso 1 1 calc R . . C18 C 0.7876(16) 0.5450(6) -0.0114(4) 0.052(3) Uani 1 1 d . . . H18A H 0.9041 0.5618 -0.0169 0.063 Uiso 1 1 calc R . . H18B H 0.7148 0.5883 -0.0250 0.063 Uiso 1 1 calc R . . C19 C 0.7545(14) 0.4616(6) -0.0360(3) 0.043(2) Uani 1 1 d . . . C20 C 0.6937(12) 0.3193(5) -0.0206(3) 0.0331(19) Uani 1 1 d . . . C21 C 0.6526(12) 0.2579(5) 0.0186(3) 0.0354(19) Uani 1 1 d . . . H21A H 0.5487 0.2279 0.0110 0.042 Uiso 1 1 calc R . . H21B H 0.7428 0.2165 0.0218 0.042 Uiso 1 1 calc R . . C22 C 0.6833(17) 0.3000(6) -0.0699(3) 0.056(3) Uani 1 1 d . . . H22 H 0.6593 0.2453 -0.0807 0.068 Uiso 1 1 calc R . . C23 C 0.7110(19) 0.3677(7) -0.1025(3) 0.062(3) Uani 1 1 d . . . H23 H 0.7069 0.3574 -0.1354 0.074 Uiso 1 1 calc R . . C24 C 0.7434(14) 0.4475(6) -0.0864(3) 0.047(2) Uani 1 1 d . . . H24 H 0.7582 0.4921 -0.1080 0.056 Uiso 1 1 calc R . . C25 C 0.2364(15) 0.4602(6) -0.0670(3) 0.051(3) Uani 1 1 d . . . H25 H 0.2506 0.5164 -0.0765 0.062 Uiso 1 1 calc R . . C26 C 0.199(2) 0.3958(8) -0.1005(4) 0.072(4) Uani 1 1 d . . . H26 H 0.1877 0.4094 -0.1329 0.086 Uiso 1 1 calc R . . C27 C 0.180(2) 0.3152(8) -0.0863(4) 0.079(4) Uani 1 1 d . . . H27 H 0.1685 0.2723 -0.1091 0.095 Uiso 1 1 calc R . . C28 C 0.6393(14) 0.4944(7) 0.2545(3) 0.053(3) Uani 1 1 d . . . H28 H 0.7496 0.4875 0.2655 0.064 Uiso 1 1 calc R . . N1 N 0.5351(9) 0.2444(4) 0.1905(2) 0.0298(14) Uani 1 1 d . . . N2 N 0.4399(8) 0.4955(4) 0.1917(2) 0.0287(13) Uani 1 1 d . . . N3 N 0.2247(8) 0.3546(4) -0.0063(3) 0.0264(13) Uani 1 1 d . . . N4 N 0.7322(8) 0.3977(4) -0.0065(3) 0.0235(13) Uani 1 1 d . . . O1 O 0.8307(8) 0.2472(4) 0.1447(2) 0.0439(15) Uani 1 1 d U . . H1O H 0.8991 0.2828 0.1245 0.053 Uiso 1 1 d R . . O2 O 0.3504(6) 0.3009(3) 0.1234(2) 0.0350(12) Uani 1 1 d . . . O1W O 0.5118(7) 0.1221(3) 0.0964(3) 0.0425(16) Uani 1 1 d . . . H1O1 H 0.4528 0.0752 0.1135 0.051 Uiso 1 1 d R . . H2O1 H 0.5973 0.0902 0.0746 0.051 Uiso 1 1 d R . . O3 O 0.1454(7) 0.4989(3) 0.1438(2) 0.0367(13) Uani 1 1 d U . . O2W O 0.5178(7) 0.6284(3) 0.0910(3) 0.0445(16) Uani 1 1 d . . . H1O2 H 0.4598 0.6576 0.0655 0.053 Uiso 1 1 d R . . H2O2 H 0.5854 0.6784 0.0959 0.053 Uiso 1 1 d R . . O4 O 0.6272(6) 0.4458(3) 0.1243(2) 0.0318(11) Uani 1 1 d . . . O5 O 0.3477(7) 0.4426(3) 0.0620(2) 0.0333(11) Uani 1 1 d . . . O6 O 0.1990(11) 0.2104(4) 0.0382(3) 0.060(2) Uani 1 1 d . . . O7 O 0.7578(8) 0.5389(4) 0.0386(2) 0.0365(14) Uani 1 1 d . . . H7O H 0.6658 0.5714 0.0590 0.044 Uiso 1 1 d R . . O8 O 0.6337(8) 0.3031(3) 0.0617(2) 0.0378(13) Uani 1 1 d . . . O9 O 0.483(2) 0.069(2) -0.1874(10) 0.36(3) Uani 1 1 d . . . O10 O 0.490(3) 0.206(2) -0.1790(11) 0.273(12) Uani 1 1 d U . . O11 O 0.597(4) 0.1272(11) -0.1299(15) 0.35(2) Uani 1 1 d . . . O12 O 0.325(5) 0.1337(14) -0.1355(18) 0.48(4) Uani 1 1 d . . . O13 O -0.0097(6) 0.3728(3) 0.0944(3) 0.0378(14) Uani 1 1 d . . . H13O H 0.0486 0.4199 0.1130 0.045 Uiso 1 1 d R . . Cu1 Cu 0.71338(11) 0.42305(5) 0.06086(3) 0.0247(2) Uani 1 1 d . . . Cu2 Cu 0.25847(11) 0.32626(5) 0.06116(3) 0.0234(2) Uani 1 1 d . . . Cu3 Cu 0.38810(11) 0.47727(5) 0.12636(4) 0.0278(2) Uani 1 1 d . . . Cu4 Cu 0.58938(11) 0.26244(5) 0.12431(4) 0.0286(2) Uani 1 1 d . . . Cl1 Cl 0.4714(6) 0.1322(2) -0.16024(19) 0.0951(12) 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 0.026(4) 0.035(4) 0.047(5) 0.001(4) -0.009(4) -0.003(3) C2 0.036(4) 0.109(8) 0.022(4) 0.012(5) -0.002(3) 0.002(5) C3 0.047(5) 0.134(9) 0.025(4) 0.004(5) 0.006(4) -0.005(6) C4 0.041(5) 0.074(7) 0.035(5) 0.013(5) 0.009(4) 0.008(5) C5 0.029(4) 0.034(4) 0.033(5) 0.003(3) 0.000(3) -0.001(3) C6 0.020(4) 0.062(5) 0.033(5) 0.019(4) 0.002(3) 0.003(4) C7 0.020(4) 0.042(5) 0.038(5) 0.016(4) -0.002(3) -0.009(3) C8 0.015(4) 0.040(5) 0.050(5) -0.003(4) -0.004(4) 0.005(3) C9 0.039(5) 0.108(9) 0.023(4) -0.015(5) -0.004(4) 0.015(5) C10 0.048(6) 0.141(11) 0.023(5) -0.011(6) -0.017(4) 0.015(7) C11 0.033(4) 0.051(5) 0.032(5) -0.012(4) -0.003(4) 0.012(4) C12 0.030(4) 0.045(5) 0.021(4) 0.005(3) -0.002(3) 0.004(3) C13 0.021(4) 0.036(4) 0.036(5) -0.010(4) 0.001(3) 0.002(3) C14 0.052(5) 0.024(4) 0.034(5) 0.000(3) -0.008(4) -0.001(3) C15 0.043(5) 0.015(3) 0.025(4) 0.009(3) -0.007(3) -0.003(3) C16 0.073(7) 0.042(5) 0.037(5) -0.015(4) -0.005(5) -0.011(5) C17 0.103(11) 0.041(6) 0.079(9) -0.003(5) 0.011(8) -0.017(6) C18 0.079(8) 0.035(5) 0.042(6) 0.004(4) 0.001(5) -0.005(5) C19 0.067(6) 0.038(5) 0.025(4) 0.004(4) 0.010(4) -0.002(4) C20 0.055(5) 0.021(4) 0.023(4) -0.007(3) 0.014(4) -0.006(3) C21 0.055(5) 0.027(4) 0.024(4) 0.000(3) 0.005(4) 0.006(4) C22 0.105(9) 0.037(5) 0.028(5) -0.011(4) 0.012(5) -0.026(5) C23 0.122(11) 0.044(6) 0.019(5) -0.006(4) 0.012(5) -0.015(6) C24 0.076(7) 0.038(5) 0.027(5) 0.005(4) 0.013(4) -0.004(4) C25 0.094(8) 0.033(5) 0.027(5) 0.012(4) -0.018(5) -0.014(5) C26 0.122(11) 0.074(8) 0.021(5) 0.002(5) -0.019(6) -0.015(8) C27 0.147(13) 0.056(7) 0.034(6) -0.015(5) 0.000(7) -0.040(8) C28 0.051(6) 0.077(7) 0.032(5) -0.011(5) -0.008(4) 0.021(5) N1 0.035(4) 0.026(3) 0.029(4) -0.001(3) -0.001(3) 0.005(3) N2 0.026(3) 0.028(3) 0.032(4) -0.001(3) 0.007(3) 0.009(3) N3 0.036(3) 0.017(3) 0.026(3) 0.003(3) -0.003(3) -0.005(2) N4 0.032(3) 0.010(3) 0.028(3) -0.004(3) 0.002(3) -0.002(2) O1 0.041(3) 0.049(3) 0.042(3) -0.019(2) -0.019(2) 0.020(2) O2 0.035(3) 0.039(3) 0.031(3) 0.010(3) 0.003(3) -0.003(2) O1W 0.055(4) 0.015(2) 0.058(4) 0.006(2) 0.022(3) -0.004(3) O3 0.040(3) 0.022(2) 0.048(3) 0.005(2) 0.031(2) 0.009(2) O2W 0.041(3) 0.034(3) 0.058(5) -0.007(2) -0.017(3) 0.008(3) O4 0.025(3) 0.044(3) 0.025(3) -0.003(3) -0.001(2) -0.001(2) O5 0.044(3) 0.031(3) 0.025(3) 0.002(3) -0.009(3) 0.004(2) O6 0.109(6) 0.027(3) 0.045(4) -0.015(3) 0.024(4) -0.022(4) O7 0.063(4) 0.025(3) 0.021(3) -0.004(2) -0.006(3) -0.006(2) O8 0.065(4) 0.028(3) 0.020(3) 0.003(2) 0.011(3) -0.003(2) O9 0.103(13) 0.56(5) 0.41(4) -0.41(4) 0.030(16) -0.022(19) O10 0.149(16) 0.36(2) 0.31(2) 0.231(19) 0.003(15) -0.012(16) O11 0.37(4) 0.096(12) 0.58(5) -0.026(19) -0.37(4) 0.039(16) O12 0.56(6) 0.121(14) 0.75(7) 0.10(3) 0.58(6) 0.09(2) O13 0.030(3) 0.036(3) 0.047(4) -0.004(2) 0.000(2) 0.002(3) Cu1 0.0444(5) 0.0131(4) 0.0165(4) -0.0015(3) 0.0069(5) -0.0014(3) Cu2 0.0369(5) 0.0160(4) 0.0174(4) 0.0027(4) -0.0044(4) -0.0052(3) Cu3 0.0247(4) 0.0356(5) 0.0231(5) -0.0047(4) -0.0052(4) 0.0043(3) Cu4 0.0262(4) 0.0335(5) 0.0262(5) 0.0071(5) 0.0056(4) 0.0039(3) Cl1 0.105(3) 0.083(2) 0.097(3) -0.0021(19) -0.034(2) -0.005(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.330(10) . ? C1 C2 1.383(13) . ? C1 C6 1.472(12) . ? C2 C3 1.386(15) . ? C3 C4 1.397(14) . ? C4 C5 1.374(12) . ? C5 N1 1.316(11) . ? C5 C7 1.500(11) . ? C6 O1 1.465(10) . ? C7 O2 1.441(10) . ? C8 N2 1.318(10) . ? C8 C9 1.407(13) . ? C8 C11 1.477(11) . ? C9 C10 1.353(14) . ? C10 C28 1.405(15) . ? C11 O3 1.502(10) . ? C12 N2 1.343(10) . ? C12 C28 1.378(12) . ? C12 C13 1.494(11) . ? C13 O4 1.438(10) . ? C14 O5 1.404(10) . ? C14 C15 1.478(11) . ? C15 N3 1.329(9) . ? C15 C25 1.412(12) . ? C16 N3 1.332(11) . ? C16 C27 1.382(15) . ? C16 C17 1.511(15) . ? C17 O6 1.524(15) . ? C18 O7 1.410(12) . ? C18 C19 1.502(13) . ? C19 N4 1.308(12) . ? C19 C24 1.419(13) . ? C20 N4 1.328(10) . ? C20 C22 1.404(12) . ? C20 C21 1.491(11) . ? C21 O8 1.400(9) . ? C22 C23 1.413(14) . ? C23 C24 1.355(14) . ? C25 C26 1.405(15) . ? C26 C27 1.335(17) . ? N1 Cu4 1.907(7) . ? N2 Cu3 1.880(7) . ? N3 Cu2 1.942(7) . ? N4 Cu1 1.918(7) . ? O1 Cu4 2.005(6) . ? O2 Cu2 1.916(6) . ? O2 Cu4 1.983(5) . ? O1W Cu4 2.418(5) . ? O3 Cu3 2.008(5) . ? O2W Cu3 2.768(6) . ? O4 Cu1 1.921(6) . ? O4 Cu3 1.955(5) . ? O5 Cu3 1.895(6) . ? O5 Cu2 1.961(5) . ? O6 Cu2 1.986(6) . ? O7 Cu1 1.955(6) . ? O8 Cu4 1.885(6) . ? O8 Cu1 1.988(5) . ? O9 Cl1 1.247(17) . ? O10 Cl1 1.29(2) . ? O11 Cl1 1.303(18) . ? O12 Cl1 1.35(2) . ? O13 Cu2 2.424(5) . ? 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 118.6(8) . . ? N1 C1 C6 115.7(8) . . ? C2 C1 C6 125.6(8) . . ? C1 C2 C3 117.0(9) . . ? C2 C3 C4 122.6(9) . . ? C5 C4 C3 116.6(9) . . ? N1 C5 C4 119.6(8) . . ? N1 C5 C7 115.3(7) . . ? C4 C5 C7 125.0(8) . . ? O1 C6 C1 114.4(7) . . ? O2 C7 C5 107.7(6) . . ? N2 C8 C9 119.2(7) . . ? N2 C8 C11 113.9(8) . . ? C9 C8 C11 126.9(8) . . ? C10 C9 C8 118.5(9) . . ? C9 C10 C28 121.1(9) . . ? C8 C11 O3 116.4(7) . . ? N2 C12 C28 119.5(8) . . ? N2 C12 C13 114.1(7) . . ? C28 C12 C13 126.4(8) . . ? O4 C13 C12 108.1(6) . . ? O5 C14 C15 109.9(6) . . ? N3 C15 C25 119.5(8) . . ? N3 C15 C14 115.5(7) . . ? C25 C15 C14 124.8(7) . . ? N3 C16 C27 118.4(9) . . ? N3 C16 C17 113.0(9) . . ? C27 C16 C17 127.9(9) . . ? C16 C17 O6 111.1(8) . . ? O7 C18 C19 111.1(7) . . ? N4 C19 C24 119.2(9) . . ? N4 C19 C18 114.1(8) . . ? C24 C19 C18 126.6(8) . . ? N4 C20 C22 120.1(8) . . ? N4 C20 C21 115.8(7) . . ? C22 C20 C21 124.0(7) . . ? O8 C21 C20 108.5(6) . . ? C20 C22 C23 116.8(8) . . ? C24 C23 C22 121.1(9) . . ? C23 C24 C19 118.7(9) . . ? C26 C25 C15 116.7(9) . . ? C27 C26 C25 120.9(10) . . ? C26 C27 C16 120.2(10) . . ? C12 C28 C10 117.9(9) . . ? C5 N1 C1 125.4(8) . . ? C5 N1 Cu4 118.6(6) . . ? C1 N1 Cu4 115.8(6) . . ? C8 N2 C12 123.6(7) . . ? C8 N2 Cu3 117.5(5) . . ? C12 N2 Cu3 118.8(5) . . ? C16 N3 C15 123.1(8) . . ? C16 N3 Cu2 120.8(6) . . ? C15 N3 Cu2 116.1(6) . . ? C19 N4 C20 124.0(8) . . ? C19 N4 Cu1 117.4(6) . . ? C20 N4 Cu1 117.6(5) . . ? C6 O1 Cu4 108.2(5) . . ? C7 O2 Cu2 125.4(5) . . ? C7 O2 Cu4 114.0(5) . . ? Cu2 O2 Cu4 115.9(3) . . ? C11 O3 Cu3 105.0(5) . . ? C13 O4 Cu1 127.2(4) . . ? C13 O4 Cu3 115.0(5) . . ? Cu1 O4 Cu3 114.6(3) . . ? C14 O5 Cu3 129.8(5) . . ? C14 O5 Cu2 114.7(5) . . ? Cu3 O5 Cu2 109.9(3) . . ? C17 O6 Cu2 112.4(6) . . ? C18 O7 Cu1 113.8(5) . . ? C21 O8 Cu4 129.4(4) . . ? C21 O8 Cu1 116.0(5) . . ? Cu4 O8 Cu1 113.0(3) . . ? N4 Cu1 O4 163.7(3) . . ? N4 Cu1 O7 82.7(3) . . ? O4 Cu1 O7 100.4(2) . . ? N4 Cu1 O8 80.7(2) . . ? O4 Cu1 O8 93.1(2) . . ? O7 Cu1 O8 160.7(3) . . ? O2 Cu2 N3 165.6(2) . . ? O2 Cu2 O5 92.7(2) . . ? N3 Cu2 O5 81.2(2) . . ? O2 Cu2 O6 100.8(3) . . ? N3 Cu2 O6 82.5(3) . . ? O5 Cu2 O6 160.9(3) . . ? O2 Cu2 O13 93.0(2) . . ? N3 Cu2 O13 100.2(3) . . ? O5 Cu2 O13 91.6(2) . . ? O6 Cu2 O13 101.1(3) . . ? N2 Cu3 O5 171.7(2) . . ? N2 Cu3 O4 81.7(3) . . ? O5 Cu3 O4 93.6(2) . . ? N2 Cu3 O3 87.2(3) . . ? O5 Cu3 O3 96.6(2) . . ? O4 Cu3 O3 166.9(3) . . ? N2 Cu3 O2W 97.5(3) . . ? O5 Cu3 O2W 88.6(2) . . ? O4 Cu3 O2W 81.3(2) . . ? O3 Cu3 O2W 107.08(19) . . ? O8 Cu4 N1 168.6(2) . . ? O8 Cu4 O2 93.5(3) . . ? N1 Cu4 O2 81.0(3) . . ? O8 Cu4 O1 97.2(3) . . ? N1 Cu4 O1 85.6(3) . . ? O2 Cu4 O1 161.2(2) . . ? O8 Cu4 O1W 93.5(2) . . ? N1 Cu4 O1W 96.6(3) . . ? O2 Cu4 O1W 91.9(2) . . ? O1 Cu4 O1W 102.9(2) . . ? O9 Cl1 O10 118(3) . . ? O9 Cl1 O11 106.6(18) . . ? O10 Cl1 O11 103.1(18) . . ? O9 Cl1 O12 113(2) . . ? O10 Cl1 O12 107.0(17) . . ? O11 Cl1 O12 109(4) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.713 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.300