# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1964 data_global #======================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Andres E. Goeta, Department of Chemistry University of Durham DURHAM DH1 3LE UK ; _publ_contact_author_phone '+44 191 3744702' _publ_contact_author_fax '+44 191 3844737' _publ_contact_author_email A.E.Goeta@durham.ac.uk _publ_requested_journal 'Dalton Transactions' #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Copper(II) complexes of the isomeric tetraazamacrocyclic ligands 1,11- and 1,8-bis(2'-pyridylmethyl)-cyclam and of the trans-dioxocyclam analogue (trans-dioxocyclam = 1,4,8,11-tetraazacyclotetradecane-5,12-dione) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Goeta, Andres E.' ; Department of Chemistry University of Durham Durham DH1 3LE UK ; 'Howard, Judith A.K.' ; Department of Chemistry University of Durham Durham DH1 3LE UK ; 'Maffeo, Davide' ; Department of Chemistry University of Durham Durham DH1 3LE UK ; 'Williams, J.A. Gareth' ; Department of Chemistry University of Durham Durham DH1 3LE UK ; 'Yufit, Dimitrii S.' ; Department of Chemistry University of Durham Durham DH1 3LE UK ; _publ_section_references ; Blessing R.H. (1995) Acta Cryst. A51, 33-38. Bruker (1998a). SMART-NT V5.0. Data Collection Software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (1998b). SAINT-NT V5.0. Data Reduction Software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (1998c). SHELXTL-NT. Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1990) Acta Cryst. A46, 467-473 Sheldrick, G.M. (1996). SADABS. Empirical Absorption Correction Program. University of G\"ottingen, Germany. Sheldrick, G.M. (1997) SHELXL-97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. ; #================================================================= # A.E. Goeta et al. CIF for additional structure included in the paper, # ref. B000739K data_CuL3 #basic pH _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H32 Cu N6 O4' _chemical_formula_weight 508.08 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7924(3) _cell_length_b 10.3659(3) _cell_length_c 12.6077(3) _cell_angle_alpha 66.602(1) _cell_angle_beta 81.966(1) _cell_angle_gamma 75.804(1) _cell_volume 1137.37(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6089 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 29.0 _exptl_crystal_description triclinic _exptl_crystal_colour clear-purple _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6237 _exptl_absorpt_correction_T_max 0.9064 _exptl_absorpt_process_details none _exptl_special_details ; The data collection nominally covered over a full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 _diffrn_reflns_number 11566 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 29.00 _reflns_number_total 5888 _reflns_number_gt 4674 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.2158P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5888 _refine_ls_number_parameters 342 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.344 _refine_ls_restrained_S_all 1.344 _refine_ls_shift/su_max 0.258 _refine_ls_shift/su_mean 0.010 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 0.5000 0.0000 1.0000 0.01483(16) Uani 1 2 d S . . Cu2 Cu 1.0000 1.0000 0.5000 0.01469(16) Uani 1 2 d S . . N11 N 0.5606(3) 0.1375(4) 0.8399(3) 0.0187(7) Uani 1 1 d . . . N12 N 0.4383(4) 0.1470(4) 1.0675(4) 0.0176(8) Uani 0.90 1 d P . 1 N15 N 0.2626(4) 0.1216(4) 0.8920(3) 0.0226(7) Uani 1 1 d . . . N21 N 0.8777(4) 0.9052(4) 0.4464(3) 0.0220(7) Uani 1 1 d . . . N22 N 1.1756(5) 0.8604(6) 0.4982(4) 0.0179(11) Uani 0.797(14) 1 d P . 1 N25 N 0.9790(4) 1.1592(4) 0.2612(3) 0.0231(8) Uani 1 1 d . . . O12 O 0.3876(6) 0.3700(5) 1.0754(4) 0.0291(11) Uani 0.90 1 d P . 1 O21 O 1.3203(6) 0.6475(6) 0.5028(5) 0.0278(11) Uani 0.797(14) 1 d P . 1 C10 C 0.6155(5) 0.2482(5) 0.8580(4) 0.0242(9) Uani 1 1 d . . . H10A H 0.6571 0.3071 0.7835 0.029 Uiso 1 1 calc R . . H10B H 0.6920 0.1992 0.9130 0.029 Uiso 1 1 calc R . . C11 C 0.5055(5) 0.3479(5) 0.9040(4) 0.0265(9) Uani 1 1 d . . . H11A H 0.5498 0.4250 0.9022 0.034 Uiso 1 1 calc R A 1 H11B H 0.4285 0.3941 0.8493 0.034 Uiso 1 1 calc R A 1 C12 C 0.4393(5) 0.2846(5) 1.0242(4) 0.0196(9) Uani 0.90 1 d P . 1 C18 C 0.6318(5) -0.0948(5) 0.8151(4) 0.0278(9) Uani 1 1 d . . . H18A H 0.5654 -0.0742 0.7552 0.036 Uiso 1 1 calc R . . H18B H 0.7145 -0.1685 0.8078 0.036 Uiso 1 1 calc R . . C19 C 0.6779(4) 0.0412(5) 0.8003(4) 0.0225(8) Uani 1 1 d . . . H19A H 0.7616 0.0160 0.8460 0.027 Uiso 1 1 calc R . . H19B H 0.7042 0.0919 0.7178 0.027 Uiso 1 1 calc R . . C20 C 0.9266(4) 0.7464(4) 0.4992(4) 0.0225(8) Uani 1 1 d . . . H20A H 0.8632 0.7012 0.4769 0.027 Uiso 1 1 calc R . . H20B H 0.9173 0.7161 0.5844 0.027 Uiso 1 1 calc R . . C21 C 1.0804(5) 0.6877(5) 0.4651(4) 0.0331(11) Uani 1 1 d . . . H21A H 1.0975 0.5816 0.5020 0.040 Uiso 1 1 calc R B 1 H21B H 1.0858 0.7128 0.3805 0.040 Uiso 1 1 calc R B 1 C22 C 1.1994(5) 0.7328(5) 0.4921(4) 0.0189(14) Uani 0.797(14) 1 d P . 1 C28 C 0.6938(6) 1.1034(5) 0.4747(4) 0.0355(11) Uani 1 1 d . . . H28A H 0.6118 1.1234 0.5256 0.043 Uiso 1 1 calc R . . H28B H 0.6697 1.1602 0.3931 0.043 Uiso 1 1 calc R . . C29 C 0.7349(5) 0.9450(5) 0.4971(5) 0.0322(10) Uani 1 1 d . . . H29A H 0.7330 0.8895 0.5817 0.039 Uiso 1 1 calc R . . H29B H 0.6650 0.9190 0.4638 0.039 Uiso 1 1 calc R . . C101 C 0.4493(4) 0.2080(4) 0.7519(4) 0.0206(8) Uani 1 1 d . . . H10C H 0.4685 0.3029 0.6993 0.025 Uiso 1 1 calc R . . H10D H 0.4586 0.1490 0.7049 0.025 Uiso 1 1 calc R . . C102 C 0.3000(4) 0.2298(4) 0.7985(3) 0.0188(8) Uani 1 1 d . . . C103 C 0.2041(5) 0.3528(5) 0.7408(4) 0.0267(9) Uani 1 1 d . . . H103 H 0.2349 0.4277 0.6761 0.032 Uiso 1 1 calc R . . C104 C 0.0630(5) 0.3673(5) 0.7771(5) 0.0327(11) Uani 1 1 d . . . H104 H -0.0047 0.4504 0.7373 0.039 Uiso 1 1 calc R . . C105 C 0.0242(5) 0.2568(6) 0.8730(4) 0.0347(11) Uani 1 1 d . . . H105 H -0.0715 0.2625 0.9011 0.042 Uiso 1 1 calc R . . C106 C 0.1268(5) 0.1370(5) 0.9282(4) 0.0293(10) Uani 1 1 d . . . H106 H 0.0990 0.0623 0.9949 0.035 Uiso 1 1 calc R . . C201 C 0.8777(7) 0.9488(5) 0.3188(4) 0.0373(12) Uani 1 1 d . . . H20C H 0.7953 0.9227 0.3010 0.045 Uiso 1 1 calc R . . H20D H 0.9636 0.8923 0.2938 0.045 Uiso 1 1 calc R . . C202 C 0.8728(5) 1.1070(4) 0.2477(3) 0.0213(8) Uani 1 1 d . . . C203 C 0.7674(5) 1.1882(5) 0.1700(4) 0.0272(9) Uani 1 1 d . . . H203 H 0.6951 1.1465 0.1619 0.033 Uiso 1 1 calc R . . C204 C 0.7702(5) 1.3311(5) 0.1046(4) 0.0305(10) Uani 1 1 d . . . H204 H 0.6990 1.3897 0.0516 0.037 Uiso 1 1 calc R . . C205 C 0.8777(5) 1.3867(5) 0.1175(4) 0.0299(10) Uani 1 1 d . . . H205 H 0.8821 1.4843 0.0734 0.036 Uiso 1 1 calc R . . C206 C 0.9799(5) 1.2981(5) 0.1960(4) 0.0284(9) Uani 1 1 d . . . H206 H 1.0540 1.3375 0.2041 0.034 Uiso 1 1 calc R . . O1W O 0.6086(5) 0.5928(5) 0.5521(4) 0.0427(10) Uani 1 1 d . . . H11W H 0.628(7) 0.521(7) 0.547(5) 0.040(18) Uiso 1 1 d . . . H12W H 0.520(8) 0.605(7) 0.547(6) 0.05(2) Uiso 1 1 d . . . O3W O 0.2448(4) 0.4224(4) 0.2633(3) 0.0334(8) Uani 1 1 d . . . H32W H 0.297(6) 0.417(6) 0.308(5) 0.033(15) Uiso 1 1 d . . . H31W H 0.297(7) 0.395(7) 0.216(6) 0.05(2) Uiso 1 1 d . . . C22B C 1.2723(19) 0.7897(19) 0.5132(15) 0.014(5) Uiso 0.203(14) 1 d P . 2 C12B C 0.397(4) 0.219(3) 1.105(3) 0.011(6) Uiso 0.10 1 d PD . 2 N22B N 1.136(2) 0.828(2) 0.4950(16) 0.017(5) Uiso 0.203(14) 1 d P . 2 N12B N 0.465(4) 0.177(4) 1.023(4) 0.019(9) Uiso 0.10 1 d P . 2 O21B O 1.347(2) 0.671(2) 0.5174(18) 0.022(5) Uiso 0.203(14) 1 d P . 2 O12B O 0.367(5) 0.348(3) 1.104(4) 0.016(10) Uiso 0.10 1 d PD C 2 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 0.0187(4) 0.0125(3) 0.0121(3) -0.0025(3) 0.0004(3) -0.0057(3) Cu2 0.0119(3) 0.0170(3) 0.0169(3) -0.0080(3) -0.0023(3) -0.0025(3) N11 0.0167(16) 0.0213(16) 0.0158(15) -0.0019(13) -0.0031(12) -0.0074(13) N12 0.020(2) 0.0180(18) 0.015(2) -0.0042(16) -0.0003(16) -0.0072(16) N15 0.0207(17) 0.0248(17) 0.0208(17) -0.0037(14) -0.0053(13) -0.0086(14) N21 0.0267(19) 0.0189(16) 0.0213(17) -0.0046(14) -0.0042(14) -0.0094(14) N22 0.017(2) 0.021(2) 0.017(2) -0.0077(17) -0.0020(16) -0.0052(19) N25 0.0199(18) 0.0197(17) 0.0297(19) -0.0123(15) -0.0073(14) 0.0042(14) O12 0.047(3) 0.0181(19) 0.022(2) -0.0085(18) 0.006(2) -0.0084(19) O21 0.021(2) 0.023(2) 0.042(3) -0.018(2) -0.0069(19) 0.0027(18) C10 0.024(2) 0.026(2) 0.020(2) -0.0013(16) -0.0013(16) -0.0139(17) C11 0.033(2) 0.031(2) 0.018(2) -0.0060(17) -0.0039(17) -0.0149(19) C12 0.018(2) 0.023(2) 0.020(2) -0.0098(18) -0.0047(17) -0.0016(17) C18 0.024(2) 0.026(2) 0.028(2) -0.0056(18) 0.0033(17) -0.0061(17) C19 0.0150(18) 0.029(2) 0.0194(19) -0.0041(16) 0.0022(14) -0.0077(16) C20 0.024(2) 0.0190(19) 0.023(2) -0.0029(16) -0.0061(16) -0.0077(16) C21 0.031(3) 0.031(2) 0.030(3) -0.003(2) -0.006(2) -0.005(2) C22 0.020(3) 0.024(3) 0.013(2) -0.0050(19) -0.0002(18) -0.008(2) C28 0.048(3) 0.032(2) 0.033(3) -0.019(2) 0.003(2) -0.011(2) C29 0.020(2) 0.033(2) 0.051(3) -0.019(2) -0.005(2) -0.0105(18) C101 0.018(2) 0.0195(19) 0.0193(19) -0.0048(16) -0.0061(15) 0.0027(15) C102 0.023(2) 0.0181(18) 0.0168(18) -0.0059(15) -0.0041(15) -0.0068(15) C103 0.027(2) 0.024(2) 0.029(2) -0.0093(18) -0.0075(18) -0.0042(17) C104 0.027(2) 0.031(2) 0.045(3) -0.022(2) -0.015(2) 0.0053(19) C105 0.019(2) 0.056(3) 0.037(3) -0.027(2) -0.0012(19) -0.005(2) C106 0.022(2) 0.045(3) 0.025(2) -0.011(2) -0.0031(17) -0.017(2) C201 0.071(4) 0.022(2) 0.021(2) -0.0008(18) -0.019(2) -0.015(2) C202 0.030(2) 0.0182(18) 0.0170(18) -0.0065(15) -0.0071(16) -0.0047(16) C203 0.032(2) 0.030(2) 0.022(2) -0.0063(18) -0.0091(17) -0.0109(19) C204 0.042(3) 0.026(2) 0.019(2) -0.0038(17) -0.0124(19) -0.0025(19) C205 0.044(3) 0.026(2) 0.021(2) -0.0068(17) -0.0024(19) -0.011(2) C206 0.026(2) 0.033(2) 0.029(2) -0.0131(19) 0.0023(18) -0.0113(18) O1W 0.036(2) 0.051(3) 0.051(2) -0.031(2) -0.0140(18) -0.0021(19) O3W 0.0223(17) 0.052(2) 0.0296(18) -0.0190(17) 0.0005(15) -0.0087(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N12B 1.91(4) 2_657 ? Cu1 N12B 1.91(4) . ? Cu1 N12 1.961(4) 2_657 ? Cu1 N12 1.961(4) . ? Cu1 N11 2.062(3) . ? Cu1 N11 2.062(3) 2_657 ? Cu2 N22B 1.962(19) . ? Cu2 N22B 1.962(19) 2_776 ? Cu2 N22 1.962(4) . ? Cu2 N22 1.962(4) 2_776 ? Cu2 N21 2.046(3) . ? Cu2 N21 2.046(3) 2_776 ? N11 C10 1.484(5) . ? N11 C19 1.496(5) . ? N11 C101 1.502(5) . ? N12 C12 1.311(6) . ? N12 C18 1.489(6) 2_657 ? N15 C106 1.337(6) . ? N15 C102 1.346(5) . ? N21 C29 1.487(6) . ? N21 C20 1.488(5) . ? N21 C201 1.488(6) . ? N22 C22 1.317(8) . ? N22 C28 1.533(8) 2_776 ? N25 C202 1.341(6) . ? N25 C206 1.347(6) . ? O12 C12 1.266(6) . ? O21 C22 1.280(7) . ? C10 C11 1.523(6) . ? C11 C12 1.513(6) . ? C11 N12B 1.90(4) . ? C18 C12B 1.35(3) 2_657 ? C18 N12 1.489(6) 2_657 ? C18 C19 1.518(6) . ? C20 C21 1.549(7) . ? C21 C22 1.481(7) . ? C21 N22B 1.85(2) . ? C28 C22B 1.300(18) 2_776 ? C28 C29 1.508(6) . ? C28 N22 1.533(8) 2_776 ? C101 C102 1.495(6) . ? C102 C103 1.381(6) . ? C103 C104 1.384(7) . ? C104 C105 1.380(7) . ? C105 C106 1.391(7) . ? C201 C202 1.517(6) . ? C202 C203 1.392(6) . ? C203 C204 1.385(6) . ? C204 C205 1.374(7) . ? C205 C206 1.388(7) . ? C22B O21B 1.26(3) . ? C22B C28 1.300(18) 2_776 ? C22B N22B 1.32(3) . ? C12B O12B 1.29(2) . ? C12B N12B 1.32(5) . ? C12B C18 1.35(3) 2_657 ? 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 N12B Cu1 N12B 180.000(8) 2_657 . ? N12B Cu1 N12 17.4(12) 2_657 2_657 ? N12B Cu1 N12 162.6(12) . 2_657 ? N12B Cu1 N12 162.6(12) 2_657 . ? N12B Cu1 N12 17.4(12) . . ? N12 Cu1 N12 180.000(1) 2_657 . ? N12B Cu1 N11 101.7(13) 2_657 . ? N12B Cu1 N11 78.3(13) . . ? N12 Cu1 N11 84.44(16) 2_657 . ? N12 Cu1 N11 95.56(16) . . ? N12B Cu1 N11 78.3(13) 2_657 2_657 ? N12B Cu1 N11 101.7(13) . 2_657 ? N12 Cu1 N11 95.56(16) 2_657 2_657 ? N12 Cu1 N11 84.44(16) . 2_657 ? N11 Cu1 N11 180.0 . 2_657 ? N22B Cu2 N22B 180.000(5) . 2_776 ? N22B Cu2 N22 17.2(6) . . ? N22B Cu2 N22 162.8(6) 2_776 . ? N22B Cu2 N22 162.8(6) . 2_776 ? N22B Cu2 N22 17.2(6) 2_776 2_776 ? N22 Cu2 N22 180.000(1) . 2_776 ? N22B Cu2 N21 78.6(7) . . ? N22B Cu2 N21 101.4(7) 2_776 . ? N22 Cu2 N21 95.3(2) . . ? N22 Cu2 N21 84.7(2) 2_776 . ? N22B Cu2 N21 101.4(7) . 2_776 ? N22B Cu2 N21 78.6(7) 2_776 2_776 ? N22 Cu2 N21 84.7(2) . 2_776 ? N22 Cu2 N21 95.3(2) 2_776 2_776 ? N21 Cu2 N21 180.000(1) . 2_776 ? C10 N11 C19 110.3(3) . . ? C10 N11 C101 110.2(3) . . ? C19 N11 C101 109.8(3) . . ? C10 N11 Cu1 107.6(2) . . ? C19 N11 Cu1 102.6(2) . . ? C101 N11 Cu1 116.1(2) . . ? C12 N12 C18 114.8(4) . 2_657 ? C12 N12 Cu1 131.2(4) . . ? C18 N12 Cu1 113.8(3) 2_657 . ? C106 N15 C102 117.4(4) . . ? C29 N21 C20 108.7(3) . . ? C29 N21 C201 112.1(4) . . ? C20 N21 C201 108.4(3) . . ? C29 N21 Cu2 103.6(3) . . ? C20 N21 Cu2 108.9(3) . . ? C201 N21 Cu2 115.0(3) . . ? C22 N22 C28 113.8(4) . 2_776 ? C22 N22 Cu2 131.5(5) . . ? C28 N22 Cu2 114.1(4) 2_776 . ? C202 N25 C206 116.9(4) . . ? N11 C10 C11 114.6(3) . . ? C12 C11 C10 118.4(4) . . ? C12 C11 N12B 35.0(12) . . ? C10 C11 N12B 85.6(12) . . ? O12 C12 N12 124.6(5) . . ? O12 C12 C11 116.9(4) . . ? N12 C12 C11 118.5(4) . . ? C12B C18 N12 41.4(14) 2_657 2_657 ? C12B C18 C19 143.3(15) 2_657 . ? N12 C18 C19 107.2(4) 2_657 . ? N11 C19 C18 110.0(3) . . ? N21 C20 C21 115.4(4) . . ? C22 C21 C20 120.5(4) . . ? C22 C21 N22B 34.2(7) . . ? C20 C21 N22B 88.7(7) . . ? O21 C22 N22 124.2(5) . . ? O21 C22 C21 117.7(5) . . ? N22 C22 C21 118.1(5) . . ? C22B C28 C29 145.7(10) 2_776 . ? C22B C28 N22 41.8(8) 2_776 2_776 ? C29 C28 N22 104.9(4) . 2_776 ? N21 C29 C28 112.2(4) . . ? C102 C101 N11 116.2(3) . . ? N15 C102 C103 122.4(4) . . ? N15 C102 C101 117.5(3) . . ? C103 C102 C101 119.9(4) . . ? C102 C103 C104 120.1(4) . . ? C105 C104 C103 117.6(4) . . ? C104 C105 C106 119.2(4) . . ? N15 C106 C105 123.2(4) . . ? N21 C201 C202 115.7(4) . . ? N25 C202 C203 123.4(4) . . ? N25 C202 C201 115.8(4) . . ? C203 C202 C201 120.8(4) . . ? C204 C203 C202 118.5(4) . . ? C205 C204 C203 118.9(4) . . ? C204 C205 C206 119.0(4) . . ? N25 C206 C205 123.2(4) . . ? O21B C22B C28 130.1(18) . 2_776 ? O21B C22B N22B 123.5(19) . . ? C28 C22B N22B 106.4(16) 2_776 . ? O12B C12B N12B 127(4) . . ? O12B C12B C18 131(3) . 2_657 ? N12B C12B C18 102(3) . 2_657 ? C22B N22B C21 109.5(14) . . ? C22B N22B Cu2 129.1(18) . . ? C21 N22B Cu2 121.4(12) . . ? C12B N12B C11 105(3) . . ? C12B N12B Cu1 133(3) . . ? C11 N12B Cu1 122(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.843 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.114 data_L1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H38 Cl2 Cu N6 O9' _chemical_formula_weight 677.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.270(1) _cell_length_b 18.666(2) _cell_length_c 18.717(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.879(3) _cell_angle_gamma 90.00 _cell_volume 2862.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 885 _cell_measurement_theta_min 13.70 _cell_measurement_theta_max 21.88 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'intense blue' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.773 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996 & 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 'Bruker SMART-CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25878 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 30.46 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 30.46 _diffrn_measured_fraction_theta_full 0.922 _reflns_number_total 8036 _reflns_number_gt 6033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998a)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998a)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1 (Bruker, 1998c)' _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. One of the perchlorates found in the lattice is disordered. It was modelled sharing the positions of two of its oxygen atoms while the chloride atom and the other two oxygens are disordered over two positions. A disordered methanol molecule was also found in the lattice. It was modelled as disordered over two positions but sharing the position of the carbon atom. This molecule was refined isotropically and no hydrogens were included in the refinement, although they were included in the final formula. ; _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^)+(0.0480P)^2^+4.9199P] 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 8036 _refine_ls_number_parameters 400 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.914 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.076 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 -0.10787(4) 0.31538(2) 0.26604(2) 0.03504(12) Uani 1 1 d . . . N1 N 0.0982(3) 0.26830(18) 0.2381(2) 0.0495(8) Uani 1 1 d . . . H1N H 0.055(5) 0.237(2) 0.203(2) 0.046(11) Uiso 1 1 d . . . N2 N -0.1463(3) 0.23442(16) 0.33414(18) 0.0402(7) Uani 1 1 d . . . H2N H -0.186(5) 0.202(2) 0.310(2) 0.036(10) Uiso 1 1 d . . . N3 N -0.2234(3) 0.38161(13) 0.33365(15) 0.0327(6) Uani 1 1 d . . . N4 N -0.0629(4) 0.39567(16) 0.19597(19) 0.0477(8) Uani 1 1 d . . . N5 N -0.2982(3) 0.29302(15) 0.17393(16) 0.0362(6) Uani 1 1 d . . . N6 N -0.5821(3) 0.37874(14) 0.39074(16) 0.0344(6) Uani 1 1 d . . . C1 C 0.2089(5) 0.2276(2) 0.2922(3) 0.0632(13) Uani 1 1 d . . . H1A H 0.2638 0.2612 0.3287 0.076 Uiso 1 1 calc R . . H1B H 0.2940 0.2040 0.2682 0.076 Uiso 1 1 calc R . . C2 C 0.1189(5) 0.1719(2) 0.3293(3) 0.0641(13) Uani 1 1 d . . . H2A H 0.1996 0.1413 0.3591 0.077 Uiso 1 1 calc R . . H2B H 0.0568 0.1410 0.2923 0.077 Uiso 1 1 calc R . . C3 C 0.0017(5) 0.2025(2) 0.3773(2) 0.0550(10) Uani 1 1 d . . . H3A H -0.0322 0.1640 0.4084 0.066 Uiso 1 1 calc R . . H3B H 0.0585 0.2398 0.4089 0.066 Uiso 1 1 calc R . . C4 C -0.2598(4) 0.26211(18) 0.3830(2) 0.0409(7) Uani 1 1 d . . . H4A H -0.2506 0.2330 0.4275 0.049 Uiso 1 1 calc R . . H4B H -0.3739 0.2595 0.3588 0.049 Uiso 1 1 calc R . . C5 C -0.2141(4) 0.33881(18) 0.40114(19) 0.0372(7) Uani 1 1 d . . . H5A H -0.2895 0.3590 0.4326 0.045 Uiso 1 1 calc R . . H5B H -0.1019 0.3409 0.4275 0.045 Uiso 1 1 calc R . . C6 C -0.1300(4) 0.44975(18) 0.3502(2) 0.0447(9) Uani 1 1 d . . . H6B H -0.0216 0.4377 0.3769 0.054 Uiso 1 1 calc R . . H6C H -0.1883 0.4792 0.3826 0.054 Uiso 1 1 calc R . . C7 C -0.1053(5) 0.4944(2) 0.2852(3) 0.0569(11) Uani 1 1 d . . . H7A H -0.0580 0.5411 0.3025 0.068 Uiso 1 1 calc R . . H7B H -0.2136 0.5042 0.2573 0.068 Uiso 1 1 calc R . . C8 C 0.0042(5) 0.4617(2) 0.2343(3) 0.0612(12) Uani 1 1 d . . . H8A H 0.0232 0.4981 0.1978 0.073 Uiso 1 1 calc R . . H8B H 0.1112 0.4501 0.2624 0.073 Uiso 1 1 calc R . . C9 C 0.0627(5) 0.3657(2) 0.1533(3) 0.0599(12) Uani 1 1 d . . . H9A H 0.0088 0.3347 0.1142 0.072 Uiso 1 1 calc R . . H9B H 0.1177 0.4054 0.1310 0.072 Uiso 1 1 calc R . . C10 C 0.1862(5) 0.3231(2) 0.2015(3) 0.0625(13) Uani 1 1 d . . . H10A H 0.2633 0.2998 0.1727 0.075 Uiso 1 1 calc R . . H10B H 0.2490 0.3548 0.2375 0.075 Uiso 1 1 calc R . . C11 C -0.2114(5) 0.4114(2) 0.1447(2) 0.0509(10) Uani 1 1 d . . . H11A H -0.1797 0.4340 0.1008 0.061 Uiso 1 1 calc R . . H11B H -0.2806 0.4458 0.1671 0.061 Uiso 1 1 calc R . . C12 C -0.3079(4) 0.3443(2) 0.1240(2) 0.0432(8) Uani 1 1 d . . . C13 C -0.4026(6) 0.3376(3) 0.0578(2) 0.0632(12) Uani 1 1 d . . . H13A H -0.4049 0.3746 0.0229 0.076 Uiso 1 1 calc R . . C14 C -0.4935(6) 0.2765(3) 0.0429(2) 0.0651(12) Uani 1 1 d . . . H14A H -0.5599 0.2709 -0.0024 0.078 Uiso 1 1 calc R . . C15 C -0.4876(4) 0.2234(2) 0.0943(2) 0.0484(9) Uani 1 1 d . . . H15A H -0.5509 0.1810 0.0855 0.058 Uiso 1 1 calc R . . C16 C -0.3885(4) 0.23306(18) 0.1582(2) 0.0391(7) Uani 1 1 d . . . H16A H -0.3825 0.1960 0.1932 0.047 Uiso 1 1 calc R . . C17 C -0.3982(3) 0.39548(17) 0.30250(17) 0.0320(6) Uani 1 1 d . . . H17A H -0.4472 0.3496 0.2838 0.038 Uiso 1 1 calc R . . H17B H -0.3990 0.4283 0.2609 0.038 Uiso 1 1 calc R . . C18 C -0.5056(3) 0.42702(16) 0.35341(17) 0.0299(6) Uani 1 1 d . . . C19 C -0.5283(4) 0.50039(17) 0.3592(2) 0.0405(8) Uani 1 1 d . . . H19A H -0.4722 0.5330 0.3323 0.049 Uiso 1 1 calc R . . C20 C -0.6349(4) 0.52520(18) 0.4050(2) 0.0428(8) Uani 1 1 d . . . H20A H -0.6541 0.5751 0.4092 0.051 Uiso 1 1 calc R . . C21 C -0.7123(4) 0.47669(19) 0.44424(19) 0.0378(7) Uani 1 1 d . . . H21A H -0.7846 0.4923 0.4764 0.045 Uiso 1 1 calc R . . C22 C -0.6817(4) 0.40451(18) 0.43545(19) 0.0367(7) Uani 1 1 d . . . H22A H -0.7346 0.3711 0.4628 0.044 Uiso 1 1 calc R . . Cl1 Cl -0.05716(9) 0.65188(4) 0.41677(4) 0.03581(17) Uani 1 1 d . . . O1 O 0.0724(3) 0.66797(19) 0.3758(2) 0.0730(10) Uani 1 1 d . . . O2 O -0.2020(3) 0.63888(16) 0.36651(16) 0.0570(7) Uani 1 1 d . . . O3 O -0.0891(4) 0.71077(15) 0.46161(16) 0.0600(8) Uani 1 1 d . . . O4 O -0.0154(3) 0.58952(13) 0.45987(14) 0.0441(6) Uani 1 1 d . . . Cl2A Cl -0.3891(13) 0.0621(5) 0.3497(6) 0.074(3) Uani 0.479(12) 1 d P A 1 O5A O -0.2408(12) 0.0687(6) 0.4070(6) 0.100(4) Uani 0.479(12) 1 d P A 1 O6A O -0.5115(13) 0.0905(7) 0.3746(8) 0.137(6) Uani 0.479(12) 1 d P A 1 Cl2B Cl -0.3875(9) 0.0613(3) 0.3337(5) 0.0460(9) Uani 0.521(12) 1 d P A 2 O5B O -0.3615(19) 0.0923(5) 0.4011(4) 0.108(6) Uani 0.521(12) 1 d P A 2 O6B O -0.5638(8) 0.0747(4) 0.3009(5) 0.088(3) Uani 0.521(12) 1 d P A 2 O7 O -0.3034(6) 0.0935(2) 0.2873(2) 0.0955(14) Uani 1 1 d . . . O8 O -0.3867(4) -0.01352(16) 0.33375(19) 0.0713(9) Uani 1 1 d . . . C23 C 0.2488(15) 0.0616(7) 0.4924(7) 0.170(4) Uiso 1 1 d D . . O9A O 0.152(2) 0.0027(9) 0.5067(11) 0.228(6) Uiso 0.558(13) 1 d PD B 1 O9B O 0.0928(18) 0.0451(14) 0.4577(12) 0.228(6) Uiso 0.442(13) 1 d PD B 2 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 0.02335(17) 0.02939(19) 0.0543(3) -0.01333(17) 0.01214(15) -0.00273(14) N1 0.0273(13) 0.0480(17) 0.075(2) -0.0332(17) 0.0125(14) -0.0013(12) N2 0.0350(14) 0.0294(14) 0.0547(19) -0.0110(13) 0.0006(13) 0.0039(11) N3 0.0240(11) 0.0270(12) 0.0479(16) -0.0072(11) 0.0083(11) -0.0009(9) N4 0.0451(16) 0.0348(15) 0.070(2) -0.0149(14) 0.0340(16) -0.0121(12) N5 0.0293(12) 0.0343(13) 0.0469(16) -0.0061(12) 0.0122(11) 0.0010(10) N6 0.0273(12) 0.0302(13) 0.0471(16) -0.0012(11) 0.0106(11) 0.0011(10) C1 0.0317(17) 0.065(3) 0.092(3) -0.040(2) 0.003(2) 0.0128(17) C2 0.049(2) 0.048(2) 0.091(3) -0.026(2) -0.005(2) 0.0240(18) C3 0.049(2) 0.047(2) 0.066(3) -0.0126(19) -0.0056(19) 0.0191(17) C4 0.0352(16) 0.0368(17) 0.051(2) 0.0011(15) 0.0073(15) 0.0026(13) C5 0.0308(15) 0.0384(17) 0.0417(18) -0.0057(14) 0.0020(13) 0.0069(12) C6 0.0358(17) 0.0319(16) 0.069(2) -0.0198(16) 0.0167(16) -0.0082(13) C7 0.062(2) 0.0307(17) 0.086(3) -0.0205(18) 0.037(2) -0.0148(16) C8 0.063(2) 0.0389(19) 0.091(3) -0.025(2) 0.045(2) -0.0224(18) C9 0.049(2) 0.054(2) 0.086(3) -0.028(2) 0.044(2) -0.0198(18) C10 0.0344(18) 0.063(3) 0.097(3) -0.042(2) 0.032(2) -0.0151(17) C11 0.060(2) 0.0402(19) 0.059(2) -0.0006(17) 0.032(2) -0.0029(16) C12 0.0397(17) 0.0464(19) 0.048(2) -0.0023(16) 0.0223(16) 0.0024(14) C13 0.070(3) 0.074(3) 0.048(2) 0.011(2) 0.015(2) 0.002(2) C14 0.053(2) 0.096(4) 0.045(2) -0.008(2) 0.0027(19) -0.006(2) C15 0.0275(15) 0.063(2) 0.056(2) -0.0172(19) 0.0085(15) -0.0053(15) C16 0.0279(14) 0.0378(17) 0.053(2) -0.0087(15) 0.0121(14) -0.0026(12) C17 0.0265(13) 0.0317(15) 0.0391(17) -0.0013(12) 0.0090(12) 0.0050(11) C18 0.0261(13) 0.0287(14) 0.0355(16) -0.0005(12) 0.0063(12) 0.0022(11) C19 0.0438(18) 0.0264(15) 0.054(2) 0.0041(14) 0.0163(16) 0.0063(13) C20 0.0471(19) 0.0289(16) 0.054(2) -0.0031(14) 0.0142(16) 0.0098(13) C21 0.0288(14) 0.0441(18) 0.0422(18) -0.0068(14) 0.0105(13) 0.0057(13) C22 0.0276(14) 0.0372(16) 0.0469(19) 0.0004(14) 0.0110(13) 0.0010(12) Cl1 0.0359(4) 0.0367(4) 0.0362(4) 0.0057(3) 0.0101(3) 0.0040(3) O1 0.0410(15) 0.086(2) 0.099(2) 0.051(2) 0.0328(16) 0.0124(14) O2 0.0409(14) 0.0664(19) 0.0615(18) -0.0141(15) -0.0010(13) 0.0114(13) O3 0.087(2) 0.0354(14) 0.0552(17) -0.0072(12) -0.0008(15) 0.0088(14) O4 0.0569(15) 0.0321(12) 0.0450(14) 0.0068(10) 0.0129(12) 0.0055(11) Cl2A 0.089(3) 0.058(3) 0.087(6) -0.018(2) 0.048(3) -0.012(2) O5A 0.062(5) 0.088(7) 0.138(9) -0.007(6) -0.033(5) -0.008(5) O6A 0.075(7) 0.150(11) 0.188(15) -0.033(10) 0.023(8) 0.060(7) Cl2B 0.0578(17) 0.0275(13) 0.058(3) -0.0007(12) 0.0260(15) 0.0096(11) O5B 0.193(15) 0.094(7) 0.044(4) -0.039(4) 0.043(6) -0.065(8) O6B 0.055(4) 0.097(6) 0.109(7) -0.011(5) 0.006(4) 0.042(4) O7 0.150(4) 0.063(2) 0.073(2) -0.0064(18) 0.014(2) -0.048(2) O8 0.087(2) 0.0423(16) 0.085(2) -0.0050(16) 0.0149(19) -0.0136(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.030(3) . ? Cu1 N1 2.048(3) . ? Cu1 N4 2.059(3) . ? Cu1 N3 2.091(2) . ? Cu1 N5 2.209(3) . ? N1 C10 1.477(5) . ? N1 C1 1.479(6) . ? N1 H1N 0.92(4) . ? N2 C4 1.490(4) . ? N2 C3 1.494(5) . ? N2 H2N 0.80(4) . ? N3 C5 1.488(4) . ? N3 C6 1.498(4) . ? N3 C17 1.506(4) . ? N4 C11 1.480(6) . ? N4 C8 1.495(5) . ? N4 C9 1.502(4) . ? N5 C12 1.333(5) . ? N5 C16 1.355(4) . ? N6 C22 1.341(4) . ? N6 C18 1.350(4) . ? C1 C2 1.503(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.519(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.508(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.512(6) . ? C6 H6B 0.9900 . ? C6 H6C 0.9900 . ? C7 C8 1.529(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.495(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.506(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.378(6) . ? C13 C14 1.373(7) . ? C13 H13A 0.9500 . ? C14 C15 1.377(6) . ? C14 H14A 0.9500 . ? C15 C16 1.366(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.509(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.388(4) . ? C19 C20 1.391(5) . ? C19 H19A 0.9500 . ? C20 C21 1.377(5) . ? C20 H20A 0.9500 . ? C21 C22 1.385(5) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? Cl1 O3 1.429(3) . ? Cl1 O4 1.431(2) . ? Cl1 O1 1.433(3) . ? Cl1 O2 1.439(3) . ? Cl2A O6A 1.285(12) . ? Cl2A O8 1.443(9) . ? Cl2A O5A 1.519(14) . ? Cl2A O7 1.562(11) . ? Cl2B O7 1.328(9) . ? Cl2B O5B 1.379(10) . ? Cl2B O8 1.397(6) . ? Cl2B O6B 1.524(10) . ? C23 O9B 1.397(5) . ? C23 O9A 1.408(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 N2 Cu1 N1 92.77(13) . . ? N2 Cu1 N4 178.18(11) . . ? N1 Cu1 N4 85.42(13) . . ? N2 Cu1 N3 86.35(11) . . ? N1 Cu1 N3 150.86(12) . . ? N4 Cu1 N3 95.32(11) . . ? N2 Cu1 N5 101.14(11) . . ? N1 Cu1 N5 104.37(12) . . ? N4 Cu1 N5 79.17(12) . . ? N3 Cu1 N5 104.37(10) . . ? C10 N1 C1 112.1(3) . . ? C10 N1 Cu1 107.6(2) . . ? C1 N1 Cu1 120.2(3) . . ? C10 N1 H1N 106(3) . . ? C1 N1 H1N 108(3) . . ? Cu1 N1 H1N 102(2) . . ? C4 N2 C3 110.2(3) . . ? C4 N2 Cu1 107.0(2) . . ? C3 N2 Cu1 116.6(3) . . ? C4 N2 H2N 111(3) . . ? C3 N2 H2N 104(3) . . ? Cu1 N2 H2N 108(3) . . ? C5 N3 C6 108.4(3) . . ? C5 N3 C17 110.9(2) . . ? C6 N3 C17 112.0(2) . . ? C5 N3 Cu1 102.81(18) . . ? C6 N3 Cu1 111.22(19) . . ? C17 N3 Cu1 111.18(19) . . ? C11 N4 C8 111.6(3) . . ? C11 N4 C9 107.6(3) . . ? C8 N4 C9 108.9(3) . . ? C11 N4 Cu1 110.5(2) . . ? C8 N4 Cu1 112.5(3) . . ? C9 N4 Cu1 105.4(2) . . ? C12 N5 C16 117.5(3) . . ? C12 N5 Cu1 112.3(2) . . ? C16 N5 Cu1 129.7(2) . . ? C22 N6 C18 117.1(3) . . ? N1 C1 C2 111.9(3) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 C3 114.1(3) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N2 C3 C2 111.9(4) . . ? N2 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N2 C4 C5 108.0(3) . . ? N2 C4 H4A 110.1 . . ? C5 C4 H4A 110.1 . . ? N2 C4 H4B 110.1 . . ? C5 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N3 C5 C4 109.6(3) . . ? N3 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? N3 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N3 C6 C7 115.1(3) . . ? N3 C6 H6B 108.5 . . ? C7 C6 H6B 108.5 . . ? N3 C6 H6C 108.5 . . ? C7 C6 H6C 108.5 . . ? H6B C6 H6C 107.5 . . ? C6 C7 C8 116.0(3) . . ? C6 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? C6 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N4 C8 C7 114.6(3) . . ? N4 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? N4 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10 C9 N4 110.0(4) . . ? C10 C9 H9A 109.7 . . ? N4 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? N4 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? N1 C10 C9 108.0(3) . . ? N1 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? N1 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N4 C11 C12 111.5(3) . . ? N4 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N4 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N5 C12 C13 122.5(4) . . ? N5 C12 C11 115.9(3) . . ? C13 C12 C11 121.6(4) . . ? C14 C13 C12 119.1(4) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C15 119.4(4) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C16 C15 C14 118.4(4) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? N5 C16 C15 123.1(4) . . ? N5 C16 H16A 118.4 . . ? C15 C16 H16A 118.4 . . ? N3 C17 C18 116.1(3) . . ? N3 C17 H17A 108.3 . . ? C18 C17 H17A 108.3 . . ? N3 C17 H17B 108.3 . . ? C18 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? N6 C18 C19 122.7(3) . . ? N6 C18 C17 115.1(3) . . ? C19 C18 C17 122.1(3) . . ? C18 C19 C20 118.7(3) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C22 118.1(3) . . ? C20 C21 H21A 121.0 . . ? C22 C21 H21A 121.0 . . ? N6 C22 C21 124.1(3) . . ? N6 C22 H22A 117.9 . . ? C21 C22 H22A 117.9 . . ? O3 Cl1 O4 110.13(16) . . ? O3 Cl1 O1 111.4(2) . . ? O4 Cl1 O1 109.38(16) . . ? O3 Cl1 O2 108.01(17) . . ? O4 Cl1 O2 110.27(18) . . ? O1 Cl1 O2 107.6(2) . . ? O6A Cl2A O8 120.9(10) . . ? O6A Cl2A O5A 108.1(11) . . ? O8 Cl2A O5A 101.1(7) . . ? O6A Cl2A O7 125.1(9) . . ? O8 Cl2A O7 101.1(6) . . ? O5A Cl2A O7 95.3(8) . . ? O7 Cl2B O5B 112.3(7) . . ? O7 Cl2B O8 116.8(6) . . ? O5B Cl2B O8 114.7(7) . . ? O7 Cl2B O6B 102.7(6) . . ? O5B Cl2B O6B 108.7(8) . . ? O8 Cl2B O6B 99.7(6) . . ? Cl2B O7 Cl2A 7.7(8) . . ? Cl2B O8 Cl2A 12.1(7) . . ? O9B C23 O9A 53.3(11) . . ? 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 N2 Cu1 N1 C10 -165.4(3) . . . . ? N4 Cu1 N1 C10 14.8(3) . . . . ? N3 Cu1 N1 C10 -77.9(4) . . . . ? N5 Cu1 N1 C10 92.3(3) . . . . ? N2 Cu1 N1 C1 -35.6(3) . . . . ? N4 Cu1 N1 C1 144.6(3) . . . . ? N3 Cu1 N1 C1 51.9(4) . . . . ? N5 Cu1 N1 C1 -137.9(3) . . . . ? N1 Cu1 N2 C4 162.0(2) . . . . ? N4 Cu1 N2 C4 168(4) . . . . ? N3 Cu1 N2 C4 11.1(2) . . . . ? N5 Cu1 N2 C4 -92.8(2) . . . . ? N1 Cu1 N2 C3 38.0(3) . . . . ? N4 Cu1 N2 C3 44(4) . . . . ? N3 Cu1 N2 C3 -112.8(3) . . . . ? N5 Cu1 N2 C3 143.3(2) . . . . ? N2 Cu1 N3 C5 18.17(19) . . . . ? N1 Cu1 N3 C5 -71.0(3) . . . . ? N4 Cu1 N3 C5 -161.1(2) . . . . ? N5 Cu1 N3 C5 118.75(19) . . . . ? N2 Cu1 N3 C6 133.9(2) . . . . ? N1 Cu1 N3 C6 44.8(4) . . . . ? N4 Cu1 N3 C6 -45.3(3) . . . . ? N5 Cu1 N3 C6 -125.5(2) . . . . ? N2 Cu1 N3 C17 -100.5(2) . . . . ? N1 Cu1 N3 C17 170.4(3) . . . . ? N4 Cu1 N3 C17 80.2(2) . . . . ? N5 Cu1 N3 C17 0.1(2) . . . . ? N2 Cu1 N4 C11 124(4) . . . . ? N1 Cu1 N4 C11 129.4(2) . . . . ? N3 Cu1 N4 C11 -79.8(2) . . . . ? N5 Cu1 N4 C11 23.8(2) . . . . ? N2 Cu1 N4 C8 -111(4) . . . . ? N1 Cu1 N4 C8 -105.1(3) . . . . ? N3 Cu1 N4 C8 45.6(3) . . . . ? N5 Cu1 N4 C8 149.3(3) . . . . ? N2 Cu1 N4 C9 8(4) . . . . ? N1 Cu1 N4 C9 13.5(3) . . . . ? N3 Cu1 N4 C9 164.2(2) . . . . ? N5 Cu1 N4 C9 -92.1(3) . . . . ? N2 Cu1 N5 C12 173.7(2) . . . . ? N1 Cu1 N5 C12 -90.4(2) . . . . ? N4 Cu1 N5 C12 -8.1(2) . . . . ? N3 Cu1 N5 C12 84.7(2) . . . . ? N2 Cu1 N5 C16 -14.8(3) . . . . ? N1 Cu1 N5 C16 81.1(3) . . . . ? N4 Cu1 N5 C16 163.4(3) . . . . ? N3 Cu1 N5 C16 -103.8(3) . . . . ? C10 N1 C1 C2 -180.0(3) . . . . ? Cu1 N1 C1 C2 52.2(4) . . . . ? N1 C1 C2 C3 -67.4(5) . . . . ? C4 N2 C3 C2 178.6(3) . . . . ? Cu1 N2 C3 C2 -59.2(4) . . . . ? C1 C2 C3 N2 72.4(5) . . . . ? C3 N2 C4 C5 89.3(4) . . . . ? Cu1 N2 C4 C5 -38.5(3) . . . . ? C6 N3 C5 C4 -162.6(2) . . . . ? C17 N3 C5 C4 74.1(3) . . . . ? Cu1 N3 C5 C4 -44.8(3) . . . . ? N2 C4 C5 N3 58.0(3) . . . . ? C5 N3 C6 C7 171.1(3) . . . . ? C17 N3 C6 C7 -66.4(4) . . . . ? Cu1 N3 C6 C7 58.8(3) . . . . ? N3 C6 C7 C8 -66.7(5) . . . . ? C11 N4 C8 C7 66.5(5) . . . . ? C9 N4 C8 C7 -174.9(4) . . . . ? Cu1 N4 C8 C7 -58.4(5) . . . . ? C6 C7 C8 N4 65.9(6) . . . . ? C11 N4 C9 C10 -157.9(3) . . . . ? C8 N4 C9 C10 81.0(4) . . . . ? Cu1 N4 C9 C10 -39.9(3) . . . . ? C1 N1 C10 C9 -174.6(3) . . . . ? Cu1 N1 C10 C9 -40.4(3) . . . . ? N4 C9 C10 N1 54.8(4) . . . . ? C8 N4 C11 C12 -162.1(3) . . . . ? C9 N4 C11 C12 78.5(3) . . . . ? Cu1 N4 C11 C12 -36.1(3) . . . . ? C16 N5 C12 C13 -1.3(5) . . . . ? Cu1 N5 C12 C13 171.4(3) . . . . ? C16 N5 C12 C11 177.5(3) . . . . ? Cu1 N5 C12 C11 -9.9(3) . . . . ? N4 C11 C12 N5 30.5(4) . . . . ? N4 C11 C12 C13 -150.7(4) . . . . ? N5 C12 C13 C14 1.5(6) . . . . ? C11 C12 C13 C14 -177.2(4) . . . . ? C12 C13 C14 C15 -0.2(7) . . . . ? C13 C14 C15 C16 -1.1(6) . . . . ? C12 N5 C16 C15 -0.2(5) . . . . ? Cu1 N5 C16 C15 -171.3(2) . . . . ? C14 C15 C16 N5 1.4(5) . . . . ? C5 N3 C17 C18 52.0(3) . . . . ? C6 N3 C17 C18 -69.2(3) . . . . ? Cu1 N3 C17 C18 165.7(2) . . . . ? C22 N6 C18 C19 -0.9(5) . . . . ? C22 N6 C18 C17 -178.5(3) . . . . ? N3 C17 C18 N6 -89.4(3) . . . . ? N3 C17 C18 C19 92.9(4) . . . . ? N6 C18 C19 C20 -0.3(5) . . . . ? C17 C18 C19 C20 177.2(3) . . . . ? C18 C19 C20 C21 1.2(6) . . . . ? C19 C20 C21 C22 -0.8(5) . . . . ? C18 N6 C22 C21 1.3(5) . . . . ? C20 C21 C22 N6 -0.5(5) . . . . ? O5B Cl2B O7 Cl2A 8(3) . . . . ? O8 Cl2B O7 Cl2A -127(4) . . . . ? O6B Cl2B O7 Cl2A 125(4) . . . . ? O6A Cl2A O7 Cl2B -96(4) . . . . ? O8 Cl2A O7 Cl2B 45(3) . . . . ? O5A Cl2A O7 Cl2B 147(4) . . . . ? O7 Cl2B O8 Cl2A 147(4) . . . . ? O5B Cl2B O8 Cl2A 12(3) . . . . ? O6B Cl2B O8 Cl2A -104(3) . . . . ? O6A Cl2A O8 Cl2B 118(4) . . . . ? O5A Cl2A O8 Cl2B -123(4) . . . . ? O7 Cl2A O8 Cl2B -25(3) . . . . ? #===END data_L2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H26 Cu0.50 N3 O5' _chemical_formula_weight 336.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6790(5) _cell_length_b 15.6748(9) _cell_length_c 11.7179(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.064(3) _cell_angle_gamma 90.00 _cell_volume 1591.84(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 806 _cell_measurement_theta_min 13.66 _cell_measurement_theta_max 23.37 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'intense purple' _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details 'XPREP (Bruker, 1998)' _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 'Bruker SMART-CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19962 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 30.42 _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 30.42 _diffrn_measured_fraction_theta_full 0.923 _reflns_number_total 4454 _reflns_number_gt 3863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998a)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998a)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1 (Bruker, 1998c)' _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. On top of the counterion (an acetate), 3 water molecules were found in the lattice. The hydrogens on these waters were found on difference Fourier maps, but for the refinement the distance O-H was restrained to be 0.901 \%A with an standard deviation of 0.001 \%A. The angle H-O-H was also restrained for each of the water molecules, restraining the distance H...H to be 1.437 \%A with an standard deviation of 0.002 \%A. Each of these water molecules have one of its hydrogens disordered over two positions (occupancies fixed at 0.5 in each position). This disorder allows the water molecules to form an extended hydrogen bond network in combination with the acetate. ; _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^)+(0.0418P)^2^+0.5215P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4454 _refine_ls_number_parameters 312 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.574 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.052 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 0.5000 0.0000 0.5000 0.01508(6) Uani 1 2 d S . . C1 C 0.35323(15) -0.13063(8) 0.61740(11) 0.0237(2) Uani 1 1 d . . . H1A H 0.4066(18) -0.1719(10) 0.5753(13) 0.021(4) Uiso 1 1 d . . . H1B H 0.311(2) -0.1540(11) 0.6829(14) 0.028(4) Uiso 1 1 d . . . C2 C 0.22509(14) -0.09350(8) 0.53926(11) 0.0230(2) Uani 1 1 d . . . H2A H 0.157(2) -0.1395(12) 0.5131(15) 0.035(4) Uiso 1 1 d . . . H2B H 0.1638(19) -0.0503(11) 0.5779(14) 0.024(4) Uiso 1 1 d . . . N1 N 0.29683(11) -0.05046(6) 0.44263(8) 0.01771(18) Uani 1 1 d . . . H1N H 0.3202(19) -0.0892(11) 0.3946(14) 0.025(4) Uiso 1 1 d . . . C3 C 0.18665(15) 0.00734(8) 0.37946(11) 0.0228(2) Uani 1 1 d . . . H3A H 0.092(2) -0.0246(11) 0.3592(14) 0.025(4) Uiso 1 1 d . . . H3B H 0.1622(19) 0.0540(10) 0.4333(14) 0.024(4) Uiso 1 1 d . . . C4 C 0.25467(15) 0.04370(8) 0.27238(11) 0.0251(3) Uani 1 1 d . . . H4A H 0.279(2) -0.0038(10) 0.2236(17) 0.029(5) Uiso 1 1 d . . . H4B H 0.173(2) 0.0767(12) 0.2310(15) 0.035(5) Uiso 1 1 d . . . C5 C 0.39094(15) 0.10394(8) 0.29463(10) 0.0217(2) Uani 1 1 d . . . H5A H 0.4143(19) 0.1306(11) 0.2272(14) 0.025(4) Uiso 1 1 d . . . H5B H 0.3623(19) 0.1499(11) 0.3460(14) 0.028(4) Uiso 1 1 d . . . N2 N 0.53396(12) 0.06238(6) 0.34684(8) 0.01800(19) Uani 1 1 d . . . C6 C 0.59942(17) 0.00630(8) 0.25817(11) 0.0246(3) Uani 1 1 d . . . H6A H 0.513(2) -0.0198(12) 0.2135(16) 0.032(4) Uiso 1 1 d . . . H6B H 0.659(2) 0.0411(12) 0.2074(16) 0.037(5) Uiso 1 1 d . . . C7 C 0.69467(14) -0.06842(8) 0.30253(10) 0.0202(2) Uani 1 1 d . . . C8 C 0.82402(15) -0.09373(9) 0.24494(11) 0.0258(3) Uani 1 1 d . . . H8A H 0.856(2) -0.0598(12) 0.1859(16) 0.037(5) Uiso 1 1 d . . . C9 C 0.90299(16) -0.16693(9) 0.28109(13) 0.0312(3) Uani 1 1 d . . . H9A H 0.991(2) -0.1851(12) 0.2443(16) 0.036(5) Uiso 1 1 d . . . C10 C 0.84861(17) -0.21311(9) 0.37139(12) 0.0314(3) Uani 1 1 d . . . H10A H 0.893(2) -0.2656(13) 0.3987(16) 0.038(5) Uiso 1 1 d . . . C11 C 0.71846(17) -0.18374(8) 0.42328(11) 0.0273(3) Uani 1 1 d . . . H11A H 0.675(2) -0.2154(12) 0.4844(16) 0.038(5) Uiso 1 1 d . . . N3 N 0.64251(12) -0.11166(7) 0.39175(9) 0.0220(2) Uani 1 1 d . . . O1 O 1.19402(13) 0.34657(7) 0.37620(9) 0.0374(2) Uani 1 1 d . . . O2 O 1.21975(11) 0.29954(6) 0.19881(8) 0.0284(2) Uani 1 1 d . . . C13 C 1.15459(14) 0.29959(8) 0.29235(11) 0.0226(2) Uani 1 1 d . . . C12 C 1.01942(16) 0.23953(9) 0.30663(12) 0.0257(3) Uani 1 1 d . . . H12A H 1.050(2) 0.1999(13) 0.3669(18) 0.046(5) Uiso 1 1 d . . . H12B H 0.933(2) 0.2708(13) 0.3300(18) 0.046(5) Uiso 1 1 d . . . H12C H 0.988(2) 0.2083(12) 0.2392(17) 0.038(5) Uiso 1 1 d . . . O3 O 1.44016(18) 0.41858(11) 0.51841(14) 0.0597(4) Uani 1 1 d D . . H31W H 1.3662(18) 0.3950(14) 0.4716(16) 0.074(8) Uiso 1 1 d D . . H32W H 1.5304(14) 0.399(3) 0.495(4) 0.083(19) Uiso 0.50 1 d PD . . H33W H 1.485(5) 0.459(3) 0.477(2) 0.085(19) Uiso 0.50 1 d PD . . O4 O 0.70009(17) 0.31576(8) 0.52196(10) 0.0451(3) Uani 1 1 d D . . H41W H 0.711(3) 0.2834(12) 0.5854(11) 0.075(8) Uiso 1 1 d D . . H42W H 0.781(3) 0.352(2) 0.525(3) 0.062(14) Uiso 0.50 1 d PD . . H43W H 0.616(3) 0.348(2) 0.531(3) 0.065(15) Uiso 0.50 1 d PD . . O5 O 0.97130(15) 0.41170(8) 0.50729(9) 0.0405(3) Uani 1 1 d D . . H51W H 1.0451(16) 0.3859(11) 0.4686(16) 0.057(6) Uiso 1 1 d D . . H52W H 0.990(3) 0.4681(3) 0.503(3) 0.042(12) Uiso 0.50 1 d PD . . H53W H 0.888(2) 0.3772(17) 0.500(4) 0.069(15) Uiso 0.50 1 d PD . . 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 0.01599(10) 0.01480(10) 0.01434(10) 0.00147(6) -0.00011(6) -0.00141(7) C1 0.0274(6) 0.0184(5) 0.0255(6) 0.0038(4) 0.0032(5) -0.0043(5) C2 0.0205(5) 0.0226(6) 0.0263(6) -0.0010(5) 0.0042(4) -0.0054(5) N1 0.0177(4) 0.0164(4) 0.0191(4) -0.0014(4) 0.0008(3) 0.0000(3) C3 0.0187(5) 0.0228(6) 0.0265(6) -0.0021(5) -0.0040(4) 0.0019(4) C4 0.0271(6) 0.0262(6) 0.0213(6) -0.0014(5) -0.0064(5) 0.0046(5) C5 0.0277(6) 0.0185(5) 0.0189(5) 0.0030(4) -0.0002(4) 0.0060(4) N2 0.0219(5) 0.0149(4) 0.0173(4) 0.0004(3) 0.0019(3) 0.0021(4) C6 0.0322(7) 0.0256(6) 0.0163(5) -0.0004(4) 0.0035(5) 0.0082(5) C7 0.0216(5) 0.0199(5) 0.0189(5) -0.0048(4) -0.0003(4) 0.0016(4) C8 0.0232(6) 0.0275(6) 0.0270(6) -0.0078(5) 0.0041(5) -0.0012(5) C9 0.0221(6) 0.0329(7) 0.0384(7) -0.0159(6) -0.0009(5) 0.0065(5) C10 0.0366(7) 0.0251(6) 0.0314(7) -0.0095(5) -0.0098(5) 0.0117(5) C11 0.0386(7) 0.0206(6) 0.0222(6) -0.0030(5) -0.0033(5) 0.0057(5) N3 0.0253(5) 0.0204(5) 0.0201(5) -0.0031(4) 0.0005(4) 0.0035(4) O1 0.0400(6) 0.0360(6) 0.0364(6) -0.0076(4) 0.0030(4) -0.0121(5) O2 0.0288(5) 0.0250(5) 0.0320(5) 0.0039(4) 0.0083(4) -0.0002(4) C13 0.0219(5) 0.0176(5) 0.0284(6) 0.0044(4) 0.0004(4) 0.0018(4) C12 0.0243(6) 0.0224(6) 0.0304(6) 0.0047(5) 0.0017(5) -0.0024(5) O3 0.0445(8) 0.0622(9) 0.0709(10) -0.0063(8) -0.0115(7) -0.0099(7) O4 0.0686(9) 0.0328(6) 0.0335(6) 0.0013(5) -0.0010(5) -0.0056(6) O5 0.0539(7) 0.0377(6) 0.0305(5) -0.0031(4) 0.0071(5) 0.0006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.0149(10) 3_656 ? Cu1 N1 2.0149(10) . ? Cu1 N2 2.0786(10) . ? Cu1 N2 2.0786(10) 3_656 ? Cu1 N3 2.5239(10) . ? C1 N2 1.4949(16) 3_656 ? C1 C2 1.5183(18) . ? C1 H1A 0.949(16) . ? C1 H1B 0.941(17) . ? C2 N1 1.4833(15) . ? C2 H2A 0.973(19) . ? C2 H2B 0.986(17) . ? N1 C3 1.4858(15) . ? N1 H1N 0.860(17) . ? C3 C4 1.5254(19) . ? C3 H3A 0.980(17) . ? C3 H3B 0.996(17) . ? C4 C5 1.5249(18) . ? C4 H4A 0.969(18) . ? C4 H4B 0.986(18) . ? C5 N2 1.5026(15) . ? C5 H5A 0.926(17) . ? C5 H5B 0.980(17) . ? N2 C1 1.4949(16) 3_656 ? N2 C6 1.4960(15) . ? C6 C7 1.5099(17) . ? C6 H6A 0.977(19) . ? C6 H6B 0.974(19) . ? C7 N3 1.3446(16) . ? C7 C8 1.3979(17) . ? C8 C9 1.391(2) . ? C8 H8A 0.926(19) . ? C9 C10 1.385(2) . ? C9 H9A 0.940(19) . ? C10 C11 1.390(2) . ? C10 H10A 0.96(2) . ? C11 N3 1.3496(16) . ? C11 H11A 0.966(19) . ? O1 C13 1.2604(16) . ? O2 C13 1.2600(16) . ? C13 C12 1.5204(18) . ? C12 H12A 0.97(2) . ? C12 H12B 0.95(2) . ? C12 H12C 0.96(2) . ? O3 H31W 0.9008(10) . ? O3 H32W 0.9009(10) . ? O3 H33W 0.9009(11) . ? O4 H41W 0.9009(10) . ? O4 H42W 0.9008(11) . ? O4 H43W 0.9010(10) . ? O5 H51W 0.9006(10) . ? O5 H52W 0.9007(11) . ? O5 H53W 0.9008(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 180.00(6) 3_656 . ? N1 Cu1 N2 86.65(4) 3_656 . ? N1 Cu1 N2 93.35(4) . . ? N1 Cu1 N2 93.35(4) 3_656 3_656 ? N1 Cu1 N2 86.65(4) . 3_656 ? N2 Cu1 N2 180.00(5) . 3_656 ? N1 Cu1 N3 89.79(4) 3_656 . ? N1 Cu1 N3 90.21(4) . . ? N2 Cu1 N3 78.25(4) . . ? N2 Cu1 N3 101.75(4) 3_656 . ? N2 C1 C2 110.02(10) 3_656 . ? N2 C1 H1A 107.6(10) 3_656 . ? C2 C1 H1A 108.0(9) . . ? N2 C1 H1B 109.1(10) 3_656 . ? C2 C1 H1B 109.7(10) . . ? H1A C1 H1B 112.4(14) . . ? N1 C2 C1 108.11(10) . . ? N1 C2 H2A 111.7(11) . . ? C1 C2 H2A 108.7(11) . . ? N1 C2 H2B 107.2(9) . . ? C1 C2 H2B 112.5(9) . . ? H2A C2 H2B 108.6(14) . . ? C2 N1 C3 111.86(10) . . ? C2 N1 Cu1 108.63(7) . . ? C3 N1 Cu1 117.08(8) . . ? C2 N1 H1N 107.5(11) . . ? C3 N1 H1N 105.9(11) . . ? Cu1 N1 H1N 105.2(11) . . ? N1 C3 C4 111.75(10) . . ? N1 C3 H3A 108.5(10) . . ? C4 C3 H3A 110.3(10) . . ? N1 C3 H3B 106.6(9) . . ? C4 C3 H3B 110.6(9) . . ? H3A C3 H3B 109.0(14) . . ? C5 C4 C3 114.92(10) . . ? C5 C4 H4A 112.7(11) . . ? C3 C4 H4A 107.7(11) . . ? C5 C4 H4B 107.0(11) . . ? C3 C4 H4B 107.4(11) . . ? H4A C4 H4B 106.7(15) . . ? N2 C5 C4 114.67(10) . . ? N2 C5 H5A 109.2(10) . . ? C4 C5 H5A 109.7(10) . . ? N2 C5 H5B 107.5(10) . . ? C4 C5 H5B 109.9(10) . . ? H5A C5 H5B 105.4(14) . . ? C1 N2 C6 110.35(10) 3_656 . ? C1 N2 C5 108.56(9) 3_656 . ? C6 N2 C5 107.94(9) . . ? C1 N2 Cu1 102.45(7) 3_656 . ? C6 N2 Cu1 113.57(7) . . ? C5 N2 Cu1 113.78(7) . . ? N2 C6 C7 115.97(10) . . ? N2 C6 H6A 108.1(11) . . ? C7 C6 H6A 104.4(11) . . ? N2 C6 H6B 109.2(11) . . ? C7 C6 H6B 110.3(11) . . ? H6A C6 H6B 108.6(16) . . ? N3 C7 C8 123.01(12) . . ? N3 C7 C6 117.25(11) . . ? C8 C7 C6 119.54(11) . . ? C9 C8 C7 118.84(13) . . ? C9 C8 H8A 122.7(12) . . ? C7 C8 H8A 118.4(12) . . ? C10 C9 C8 118.76(13) . . ? C10 C9 H9A 120.7(12) . . ? C8 C9 H9A 120.6(12) . . ? C9 C10 C11 118.63(13) . . ? C9 C10 H10A 123.9(11) . . ? C11 C10 H10A 117.4(11) . . ? N3 C11 C10 123.64(13) . . ? N3 C11 H11A 115.3(11) . . ? C10 C11 H11A 121.1(11) . . ? C7 N3 C11 117.07(11) . . ? C7 N3 Cu1 103.63(7) . . ? C11 N3 Cu1 133.49(8) . . ? O2 C13 O1 124.24(12) . . ? O2 C13 C12 118.70(12) . . ? O1 C13 C12 117.06(12) . . ? C13 C12 H12A 107.3(12) . . ? C13 C12 H12B 109.8(12) . . ? H12A C12 H12B 108.1(17) . . ? C13 C12 H12C 114.2(11) . . ? H12A C12 H12C 109.2(16) . . ? H12B C12 H12C 108.1(17) . . ? H31W O3 H32W 105.8(3) . . ? H31W O3 H33W 105.8(3) . . ? H32W O3 H33W 71(4) . . ? H41W O4 H42W 105.8(3) . . ? H41W O4 H43W 105.7(3) . . ? H42W O4 H43W 105(4) . . ? H51W O5 H52W 105.9(3) . . ? H51W O5 H53W 105.9(3) . . ? H52W O5 H53W 137(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 N2 C1 C2 N1 54.92(13) 3_656 . . . ? C1 C2 N1 C3 -164.41(10) . . . . ? C1 C2 N1 Cu1 -33.65(11) . . . . ? N1 Cu1 N1 C2 71(90) 3_656 . . . ? N2 Cu1 N1 C2 -173.04(8) . . . . ? N2 Cu1 N1 C2 6.96(8) 3_656 . . . ? N3 Cu1 N1 C2 108.71(8) . . . . ? N1 Cu1 N1 C3 -161(90) 3_656 . . . ? N2 Cu1 N1 C3 -45.18(9) . . . . ? N2 Cu1 N1 C3 134.82(9) 3_656 . . . ? N3 Cu1 N1 C3 -123.43(9) . . . . ? C2 N1 C3 C4 -173.53(10) . . . . ? Cu1 N1 C3 C4 60.18(12) . . . . ? N1 C3 C4 C5 -66.46(14) . . . . ? C3 C4 C5 N2 66.76(14) . . . . ? C4 C5 N2 C1 -170.06(10) . . . 3_656 ? C4 C5 N2 C6 70.31(13) . . . . ? C4 C5 N2 Cu1 -56.71(12) . . . . ? N1 Cu1 N2 C1 -20.98(7) 3_656 . . 3_656 ? N1 Cu1 N2 C1 159.02(7) . . . 3_656 ? N2 Cu1 N2 C1 -135(100) 3_656 . . 3_656 ? N3 Cu1 N2 C1 -111.46(8) . . . 3_656 ? N1 Cu1 N2 C6 98.02(9) 3_656 . . . ? N1 Cu1 N2 C6 -81.98(9) . . . . ? N2 Cu1 N2 C6 -16(100) 3_656 . . . ? N3 Cu1 N2 C6 7.54(8) . . . . ? N1 Cu1 N2 C5 -137.95(8) 3_656 . . . ? N1 Cu1 N2 C5 42.05(8) . . . . ? N2 Cu1 N2 C5 108(100) 3_656 . . . ? N3 Cu1 N2 C5 131.57(8) . . . . ? C1 N2 C6 C7 87.82(13) 3_656 . . . ? C5 N2 C6 C7 -153.69(11) . . . . ? Cu1 N2 C6 C7 -26.55(14) . . . . ? N2 C6 C7 N3 41.30(16) . . . . ? N2 C6 C7 C8 -143.75(12) . . . . ? N3 C7 C8 C9 -0.01(19) . . . . ? C6 C7 C8 C9 -174.66(12) . . . . ? C7 C8 C9 C10 1.35(19) . . . . ? C8 C9 C10 C11 -0.9(2) . . . . ? C9 C10 C11 N3 -1.0(2) . . . . ? C8 C7 N3 C11 -1.77(18) . . . . ? C6 C7 N3 C11 173.00(11) . . . . ? C8 C7 N3 Cu1 155.04(10) . . . . ? C6 C7 N3 Cu1 -30.19(12) . . . . ? C10 C11 N3 C7 2.28(19) . . . . ? C10 C11 N3 Cu1 -145.88(11) . . . . ? N1 Cu1 N3 C7 -74.32(8) 3_656 . . . ? N1 Cu1 N3 C7 105.68(8) . . . . ? N2 Cu1 N3 C7 12.29(7) . . . . ? N2 Cu1 N3 C7 -167.71(7) 3_656 . . . ? N1 Cu1 N3 C11 76.77(13) 3_656 . . . ? N1 Cu1 N3 C11 -103.23(13) . . . . ? N2 Cu1 N3 C11 163.39(13) . . . . ? N2 Cu1 N3 C11 -16.61(13) 3_656 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H31W O1 0.9008(10) 1.970(2) 2.8695(17) 176(2) . O5 H51W O1 0.9006(10) 1.836(4) 2.7306(17) 172(2) . O4 H41W O2 0.9009(10) 1.857(4) 2.7481(16) 169(2) 4_566 N1 H1N O2 0.860(17) 2.078(17) 2.8758(14) 154.0(15) 2_645 O5 H53W O4 0.9008(11) 1.924(7) 2.8063(19) 166(3) . O4 H42W O5 0.9008(11) 1.922(11) 2.8063(19) 167(4) . O4 H43W O3 0.9010(10) 1.882(6) 2.771(2) 169(3) 1_455 O3 H32W O4 0.9009(10) 1.98(4) 2.771(2) 146(6) 1_655 O3 H33W O3 0.9009(11) 2.03(3) 2.798(3) 143(4) 3_866 O5 H52W O5 0.9007(11) 1.919(3) 2.819(3) 179(3) 3_766 #===END data_L3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H58 Cl3 Cu2 N9 O21' _chemical_formula_weight 1155.35 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 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 13.7841(4) _cell_length_b 21.5077(6) _cell_length_c 15.9374(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.544(1) _cell_angle_gamma 90.00 _cell_volume 4684.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular prism' _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2404 _exptl_absorpt_coefficient_mu 1.168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7208 _exptl_absorpt_correction_T_max 0.8174 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996 & Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART-CCD 1K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31888 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 10727 _reflns_number_gt 7383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998a)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998a)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1 (Bruker, 1998c)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The 3 perchlorates in the structure are disordered. For the 6 water molecules, the hydrogen atoms have been located from difference Fourier maps only for one of them. This means that 10 hydrogen atoms could not be located. One of the water molecules has been refined as disordered. The higher than normal maximum shift/su is due to one of the water molecules ; _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^)+(0.0700P)^2^+6.4000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10727 _refine_ls_number_parameters 781 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.094 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.082 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.102 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 1.11380(3) -0.02855(2) 0.13704(3) 0.01686(12) Uani 1 1 d . . . Cu2 Cu 0.78395(3) -0.12584(2) 0.30765(3) 0.01886(12) Uani 1 1 d . . . O1 O 0.7378(2) -0.18286(14) 0.52976(19) 0.0335(7) Uani 1 1 d . . . O2 O 1.02520(19) -0.08431(12) 0.18606(16) 0.0205(6) Uani 1 1 d . . . O3 O 1.00726(18) 0.02838(12) 0.09643(16) 0.0200(5) Uani 1 1 d . . . N1 N 0.8064(2) -0.03706(15) 0.3583(2) 0.0233(7) Uani 1 1 d . . . N2 N 0.8741(3) -0.14065(19) 0.4865(2) 0.0335(9) Uani 1 1 d . . . N3 N 0.8116(2) -0.23205(15) 0.3131(2) 0.0224(7) Uani 1 1 d . . . N4 N 0.9073(2) -0.12447(14) 0.2578(2) 0.0196(7) Uani 1 1 d . . . N5 N 0.6577(2) -0.12013(15) 0.3559(2) 0.0222(7) Uani 1 1 d . . . N6 N 0.7049(2) -0.15583(15) 0.1905(2) 0.0209(7) Uani 1 1 d . . . N7 N 1.2046(2) 0.01736(14) 0.0658(2) 0.0185(6) Uani 1 1 d . . . N8 N 0.9139(2) 0.09599(15) 0.0145(2) 0.0186(7) Uani 1 1 d . . . N9 N 1.2266(2) -0.08653(15) 0.1613(2) 0.0204(7) Uani 1 1 d . . . C1 C 0.8795(3) -0.0337(2) 0.4358(3) 0.0307(10) Uani 1 1 d . . . C2 C 0.8546(4) -0.0755(2) 0.5070(3) 0.0380(11) Uani 1 1 d . . . C3 C 0.8162(3) -0.1894(2) 0.5006(3) 0.0320(10) Uani 1 1 d . . . C4 C 0.8507(3) -0.2515(2) 0.4736(3) 0.0354(11) Uani 1 1 d . . . C5 C 0.7964(3) -0.2721(2) 0.3874(3) 0.0302(10) Uani 1 1 d . . . C6 C 0.9167(3) -0.2329(2) 0.2996(3) 0.0281(9) Uani 1 1 d . . . C7 C 0.9361(3) -0.18710(18) 0.2317(3) 0.0245(9) Uani 1 1 d . . . C8 C 0.9571(3) -0.07743(17) 0.2338(2) 0.0198(8) Uani 1 1 d . . . C9 C 0.9392(3) -0.01243(18) 0.2658(3) 0.0240(8) Uani 1 1 d . . . C10 C 0.8390(3) 0.00286(19) 0.2899(3) 0.0248(8) Uani 1 1 d . . . C11 C 0.7092(3) -0.0124(2) 0.3753(3) 0.0310(10) Uani 1 1 d . . . C12 C 0.6359(3) -0.0636(2) 0.3839(3) 0.0270(9) Uani 1 1 d . . . C13 C 0.5473(4) -0.0517(3) 0.4133(3) 0.0384(11) Uani 1 1 d . . . C14 C 0.4796(4) -0.0995(3) 0.4144(3) 0.0403(12) Uani 1 1 d . . . C15 C 0.5022(3) -0.1572(2) 0.3845(3) 0.0329(10) Uani 1 1 d . . . C16 C 0.5904(3) -0.1659(2) 0.3563(3) 0.0282(9) Uani 1 1 d . . . C17 C 0.7518(3) -0.2608(2) 0.2379(3) 0.0292(9) Uani 1 1 d . . . C18 C 0.7094(3) -0.21578(19) 0.1701(3) 0.0252(9) Uani 1 1 d . . . C19 C 0.6706(3) -0.2372(2) 0.0898(3) 0.0327(10) Uani 1 1 d . . . C20 C 0.6244(3) -0.1960(3) 0.0318(3) 0.0376(12) Uani 1 1 d . . . C21 C 0.6157(3) -0.1340(2) 0.0544(3) 0.0308(10) Uani 1 1 d . . . C22 C 0.6576(3) -0.1154(2) 0.1337(2) 0.0232(8) Uani 1 1 d . . . C25 C 1.0013(3) 0.07533(16) 0.0488(2) 0.0183(7) Uani 1 1 d . . . C24 C 1.0894(3) 0.10932(19) 0.0257(3) 0.0213(8) Uani 1 1 d . . . C23 C 1.1879(3) 0.08638(17) 0.0713(3) 0.0205(8) Uani 1 1 d . . . C28 C 1.3050(3) 0.0035(2) 0.1105(3) 0.0242(8) Uani 1 1 d . . . C29 C 1.3107(3) -0.06259(18) 0.1401(2) 0.0211(8) Uani 1 1 d . . . C30 C 1.3968(3) -0.0975(2) 0.1473(3) 0.0270(9) Uani 1 1 d . . . C31 C 1.3953(3) -0.1579(2) 0.1768(3) 0.0318(10) Uani 1 1 d . . . C32 C 1.3085(3) -0.1818(2) 0.1984(3) 0.0313(10) Uani 1 1 d . . . C33 C 1.2256(3) -0.14518(19) 0.1901(3) 0.0250(8) Uani 1 1 d . . . C26 C 0.8224(3) 0.07302(18) 0.0411(3) 0.0202(8) Uani 1 1 d . . . C27 C 1.1965(3) -0.00344(18) -0.0245(2) 0.0195(8) Uani 1 1 d . . . O1W O 1.1808(2) 0.02424(15) 0.26302(19) 0.0296(7) Uani 1 1 d D . . Cl1 Cl 0.01813(8) 0.16702(4) 0.25581(7) 0.0285(2) Uani 1 1 d . . . O11 O -0.0049(3) 0.21573(17) 0.3101(2) 0.0496(9) Uiso 1 1 d . A . O12 O 0.0852(5) 0.1866(3) 0.2018(4) 0.0687(16) Uiso 0.80 1 d P A 1 O13 O -0.0692(4) 0.1414(2) 0.2070(3) 0.0490(12) Uiso 0.80 1 d P A 1 O14 O 0.0508(4) 0.1144(2) 0.3089(3) 0.0480(11) Uiso 0.80 1 d P A 1 O12' O 0.1261(13) 0.1721(8) 0.2340(12) 0.039(4) Uiso 0.20 1 d P A 2 O13' O -0.0488(11) 0.1642(7) 0.1816(10) 0.028(3) Uiso 0.20 1 d P A 2 O14' O 0.099(2) 0.1310(12) 0.2887(17) 0.078(7) Uiso 0.20 1 d P A 2 Cl2 Cl 0.56501(8) 0.06661(5) 0.14972(8) 0.0363(3) Uani 1 1 d . . . O21 O 0.5524(5) 0.0251(3) 0.0722(4) 0.0403(16) Uiso 0.50 1 d P B 3 O22 O 0.5247(5) 0.0271(3) 0.2154(4) 0.0329(15) Uiso 0.50 1 d P B 3 O23 O 0.4821(5) 0.1087(3) 0.1483(4) 0.0339(16) Uiso 0.50 1 d P B 3 O24 O 0.6431(5) 0.0973(3) 0.2139(4) 0.0391(15) Uiso 0.50 1 d P B 3 O21' O 0.5969(10) 0.0665(6) 0.0739(8) 0.108(4) Uiso 0.50 1 d P B 4 O22' O 0.5410(8) 0.0111(5) 0.1856(7) 0.080(3) Uiso 0.50 1 d P B 4 O23' O 0.5111(5) 0.1202(3) 0.1313(4) 0.0305(15) Uiso 0.50 1 d P B 4 O24' O 0.6670(5) 0.0753(3) 0.1714(4) 0.0392(15) Uiso 0.50 1 d P B 4 Cl3 Cl 0.83719(8) 0.12237(5) 0.56770(7) 0.0345(2) Uani 1 1 d . . . O31 O 0.8526(3) 0.0631(2) 0.6091(3) 0.0748(13) Uiso 1 1 d . C . O32 O 0.9169(4) 0.1292(3) 0.5157(4) 0.0572(14) Uiso 0.70 1 d P C 5 O33 O 0.7499(4) 0.1215(2) 0.5182(3) 0.0500(13) Uiso 0.70 1 d P C 5 O34 O 0.8505(5) 0.1704(3) 0.6304(4) 0.0755(19) Uiso 0.70 1 d P C 5 O32' O 0.9190(10) 0.1547(6) 0.5770(9) 0.058(3) Uiso 0.30 1 d P C 6 O33' O 0.8050(10) 0.1147(6) 0.4724(8) 0.053(3) Uiso 0.30 1 d P C 6 O34' O 0.7558(11) 0.1642(7) 0.5925(9) 0.063(4) Uiso 0.30 1 d P C 6 O2W O 1.0902(2) -0.22103(14) 1.0419(2) 0.0353(7) Uani 1 1 d D . . O3W O 0.5914(3) 0.22149(19) 0.4442(3) 0.0573(11) Uani 1 1 d . . . O4W O 0.4623(4) -0.1109(2) 0.6304(3) 0.0803(14) Uani 1 1 d U . . O5W O 0.6728(8) -0.1103(5) 0.6474(7) 0.059(3) Uiso 0.40 1 d P . . O5'W O 0.6500(5) -0.0868(3) 0.6215(4) 0.0446(15) Uiso 0.60 1 d P . . O6W O 0.7032(8) 0.2569(5) 0.6018(7) 0.119(3) Uiso 0.60 1 d P . . O7W O 0.3480(18) 0.1753(12) 0.2056(17) 0.189(9) Uiso 0.40 1 d P . . H2N H 0.929(4) -0.154(2) 0.473(3) 0.033(14) Uiso 1 1 d . . . H8N H 0.913(3) 0.1273(19) -0.004(3) 0.011(11) Uiso 1 1 d . . . H011 H 0.948(4) -0.051(2) 0.421(3) 0.039(13) Uiso 1 1 d . . . H012 H 0.886(3) 0.010(2) 0.454(3) 0.019(10) Uiso 1 1 d . . . H021 H 0.899(4) -0.063(2) 0.558(3) 0.043(14) Uiso 1 1 d . . . H022 H 0.787(4) -0.069(2) 0.519(3) 0.029(12) Uiso 1 1 d . . . H41 H 0.922(3) -0.255(2) 0.476(3) 0.027(11) Uiso 1 1 d . . . H42 H 0.839(3) -0.281(2) 0.517(3) 0.038(13) Uiso 1 1 d . . . H51 H 0.730(3) -0.2733(19) 0.393(3) 0.024(11) Uiso 1 1 d . . . H52 H 0.814(3) -0.312(2) 0.379(3) 0.037(13) Uiso 1 1 d . . . H61 H 0.936(3) -0.273(2) 0.288(3) 0.028(12) Uiso 1 1 d . . . H62 H 0.955(3) -0.2194(18) 0.353(3) 0.016(10) Uiso 1 1 d . . . H71 H 1.004(3) -0.1911(17) 0.229(2) 0.013(9) Uiso 1 1 d . . . H72 H 0.906(4) -0.198(2) 0.181(3) 0.036(13) Uiso 1 1 d . . . H91 H 0.988(3) -0.0090(17) 0.313(3) 0.011(9) Uiso 1 1 d . . . H92 H 0.948(3) 0.0165(19) 0.221(3) 0.019(10) Uiso 1 1 d . . . H101 H 0.840(3) 0.048(2) 0.305(3) 0.033(12) Uiso 1 1 d . . . H102 H 0.788(3) -0.001(2) 0.242(3) 0.029(12) Uiso 1 1 d . . . H111 H 0.715(3) 0.013(2) 0.425(3) 0.029(12) Uiso 1 1 d . . . H112 H 0.683(4) 0.013(2) 0.330(3) 0.041(14) Uiso 1 1 d . . . H13 H 0.537(4) -0.014(2) 0.431(3) 0.041(14) Uiso 1 1 d . . . H14 H 0.423(4) -0.093(3) 0.431(4) 0.054(16) Uiso 1 1 d . . . H15 H 0.461(4) -0.189(2) 0.386(3) 0.043(14) Uiso 1 1 d . . . H16 H 0.605(3) -0.203(2) 0.334(3) 0.020(11) Uiso 1 1 d . . . H171 H 0.790(4) -0.288(2) 0.213(3) 0.045(15) Uiso 1 1 d . . . H172 H 0.697(3) -0.280(2) 0.254(3) 0.028(12) Uiso 1 1 d . . . H19 H 0.681(4) -0.279(2) 0.082(3) 0.040(14) Uiso 1 1 d . . . H20 H 0.600(4) -0.209(3) -0.014(4) 0.054(17) Uiso 1 1 d . . . H21 H 0.582(3) -0.1041(18) 0.017(3) 0.014(10) Uiso 1 1 d . . . H22 H 0.653(3) -0.068(2) 0.156(3) 0.033(12) Uiso 1 1 d . . . H231 H 1.244(3) 0.1032(19) 0.052(3) 0.019(10) Uiso 1 1 d . . . H232 H 1.197(3) 0.0992(18) 0.133(3) 0.015(10) Uiso 1 1 d . . . H241 H 1.085(3) 0.1088(17) -0.036(3) 0.012(9) Uiso 1 1 d . . . H242 H 1.082(3) 0.145(2) 0.040(3) 0.026(12) Uiso 1 1 d . . . H261 H 0.826(3) 0.0780(16) 0.101(3) 0.010(9) Uiso 1 1 d . . . H262 H 0.769(3) 0.1024(18) 0.012(2) 0.012(9) Uiso 1 1 d . . . H271 H 1.145(3) 0.0168(18) -0.054(3) 0.015(10) Uiso 1 1 d . . . H272 H 1.257(3) 0.0071(17) -0.042(2) 0.009(9) Uiso 1 1 d . . . H281 H 1.317(3) 0.031(2) 0.156(3) 0.030(12) Uiso 1 1 d . . . H282 H 1.354(3) 0.0096(17) 0.076(2) 0.009(9) Uiso 1 1 d . . . H30 H 1.450(3) -0.080(2) 0.130(3) 0.030(12) Uiso 1 1 d . . . H31 H 1.462(3) -0.184(2) 0.180(3) 0.035(12) Uiso 1 1 d . . . H32 H 1.304(3) -0.221(2) 0.213(3) 0.022(11) Uiso 1 1 d . . . H33 H 1.163(3) -0.1579(19) 0.205(3) 0.022(11) Uiso 1 1 d . . . H11W H 1.177(4) -0.0048(15) 0.293(3) 0.037(15) Uiso 1 1 d D . . H12W H 1.147(3) 0.0516(17) 0.276(3) 0.042(16) Uiso 1 1 d D . . H21W H 1.0363(17) -0.234(2) 1.043(4) 0.050 Uiso 1 1 d D . . H22W H 1.132(3) -0.2461(19) 1.038(4) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0166(2) 0.0163(2) 0.0180(2) 0.00208(18) 0.00334(17) 0.00057(17) Cu2 0.0179(2) 0.0203(2) 0.0189(2) -0.00041(18) 0.00417(17) -0.00169(18) O1 0.0328(17) 0.0396(18) 0.0289(16) 0.0054(14) 0.0070(13) -0.0126(14) O2 0.0219(14) 0.0187(13) 0.0220(14) 0.0016(11) 0.0067(11) 0.0001(10) O3 0.0193(13) 0.0197(13) 0.0216(14) 0.0040(11) 0.0057(10) 0.0010(10) N1 0.0239(17) 0.0267(18) 0.0201(17) -0.0031(14) 0.0061(13) -0.0030(14) N2 0.031(2) 0.045(2) 0.0237(19) 0.0056(17) 0.0039(16) -0.0099(18) N3 0.0244(17) 0.0192(16) 0.0241(17) 0.0059(13) 0.0052(13) -0.0005(13) N4 0.0202(16) 0.0185(16) 0.0204(16) 0.0016(13) 0.0043(13) 0.0008(12) N5 0.0205(16) 0.0276(18) 0.0187(16) 0.0023(14) 0.0035(13) -0.0017(13) N6 0.0197(16) 0.0249(17) 0.0185(16) 0.0001(13) 0.0032(13) -0.0034(13) N7 0.0147(15) 0.0186(16) 0.0219(17) -0.0004(13) 0.0012(12) 0.0000(12) N8 0.0226(17) 0.0114(16) 0.0220(17) 0.0032(13) 0.0037(13) 0.0018(13) N9 0.0208(16) 0.0208(16) 0.0196(16) 0.0017(13) 0.0023(13) 0.0015(13) C1 0.034(2) 0.035(2) 0.023(2) -0.0006(19) 0.0012(18) -0.011(2) C2 0.047(3) 0.047(3) 0.021(2) -0.002(2) 0.007(2) -0.020(2) C3 0.030(2) 0.042(3) 0.023(2) 0.0113(19) -0.0013(18) -0.0086(19) C4 0.029(2) 0.042(3) 0.036(3) 0.023(2) 0.0047(19) 0.003(2) C5 0.030(2) 0.022(2) 0.039(3) 0.0121(19) 0.0101(19) 0.0028(18) C6 0.028(2) 0.018(2) 0.039(3) 0.0063(18) 0.0111(19) 0.0054(17) C7 0.024(2) 0.019(2) 0.032(2) 0.0018(17) 0.0083(18) 0.0008(16) C8 0.0224(19) 0.0205(19) 0.0160(18) 0.0054(15) 0.0006(15) 0.0016(15) C9 0.032(2) 0.020(2) 0.022(2) 0.0007(16) 0.0104(18) -0.0026(16) C10 0.032(2) 0.019(2) 0.024(2) -0.0009(17) 0.0070(18) 0.0012(17) C11 0.030(2) 0.029(2) 0.037(3) -0.007(2) 0.014(2) -0.0017(18) C12 0.026(2) 0.035(2) 0.021(2) 0.0001(17) 0.0071(16) 0.0004(18) C13 0.037(3) 0.042(3) 0.040(3) -0.012(2) 0.018(2) -0.001(2) C14 0.026(2) 0.057(3) 0.041(3) -0.003(2) 0.015(2) -0.003(2) C15 0.030(2) 0.045(3) 0.025(2) 0.006(2) 0.0061(18) -0.009(2) C16 0.029(2) 0.031(2) 0.024(2) 0.0050(18) 0.0008(17) -0.0034(18) C17 0.033(2) 0.020(2) 0.037(3) -0.0022(18) 0.011(2) -0.0050(18) C18 0.025(2) 0.026(2) 0.026(2) -0.0015(16) 0.0072(16) -0.0066(16) C19 0.031(2) 0.036(3) 0.033(2) -0.013(2) 0.0105(19) -0.015(2) C20 0.031(2) 0.062(3) 0.020(2) -0.010(2) 0.0042(19) -0.021(2) C21 0.019(2) 0.050(3) 0.023(2) 0.004(2) 0.0018(16) -0.0066(19) C22 0.0166(19) 0.034(2) 0.0196(19) 0.0039(17) 0.0060(15) -0.0021(16) C25 0.0219(19) 0.0153(17) 0.0178(18) -0.0030(14) 0.0035(14) 0.0011(14) C24 0.024(2) 0.0155(19) 0.025(2) 0.0023(16) 0.0064(16) -0.0007(15) C23 0.0160(18) 0.0180(19) 0.028(2) -0.0002(16) 0.0056(16) -0.0022(14) C28 0.0141(19) 0.031(2) 0.028(2) -0.0003(18) 0.0024(16) -0.0001(16) C29 0.0171(18) 0.026(2) 0.0199(19) -0.0017(16) 0.0000(14) 0.0010(15) C30 0.019(2) 0.033(2) 0.029(2) -0.0029(18) 0.0020(17) 0.0033(17) C31 0.026(2) 0.038(3) 0.030(2) -0.0064(19) -0.0024(18) 0.0112(19) C32 0.037(3) 0.023(2) 0.032(2) 0.0034(18) -0.0025(19) 0.0091(18) C33 0.025(2) 0.025(2) 0.025(2) 0.0001(17) 0.0016(17) 0.0020(16) C26 0.022(2) 0.0205(19) 0.019(2) 0.0010(15) 0.0046(15) 0.0019(15) C27 0.019(2) 0.0207(19) 0.0196(19) 0.0015(15) 0.0062(16) -0.0001(15) O1W 0.0367(18) 0.0279(17) 0.0240(16) -0.0001(14) 0.0033(13) 0.0002(14) Cl1 0.0342(6) 0.0219(5) 0.0290(5) -0.0061(4) 0.0027(4) 0.0039(4) Cl2 0.0231(5) 0.0359(6) 0.0482(7) 0.0059(5) -0.0013(5) 0.0018(4) Cl3 0.0373(6) 0.0400(6) 0.0261(5) 0.0049(5) 0.0040(4) -0.0077(5) O2W 0.0335(18) 0.0210(16) 0.052(2) 0.0044(14) 0.0075(16) 0.0059(13) O3W 0.045(2) 0.071(3) 0.062(2) 0.029(2) 0.0256(18) 0.0062(19) O4W 0.081(3) 0.083(3) 0.080(3) -0.023(3) 0.020(3) 0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.947(3) . ? Cu1 O3 1.956(3) . ? Cu1 N9 1.991(3) . ? Cu1 N7 2.050(3) . ? Cu1 O1W 2.385(3) . ? Cu2 N4 1.969(3) . ? Cu2 N5 1.997(3) . ? Cu2 N1 2.080(3) . ? Cu2 N6 2.134(3) . ? Cu2 N3 2.316(3) . ? O1 C3 1.239(5) . ? O2 C8 1.292(4) . ? O3 C25 1.260(4) . ? N1 C1 1.490(5) . ? N1 C11 1.499(5) . ? N1 C10 1.502(5) . ? N2 C3 1.354(6) . ? N2 C2 1.471(7) . ? N3 C6 1.493(5) . ? N3 C17 1.498(5) . ? N3 C5 1.501(5) . ? N4 C8 1.308(5) . ? N4 C7 1.479(5) . ? N5 C12 1.342(5) . ? N5 C16 1.353(5) . ? N6 C18 1.333(5) . ? N6 C22 1.359(5) . ? N7 C27 1.497(5) . ? N7 C28 1.501(5) . ? N7 C23 1.506(5) . ? N8 C25 1.333(5) . ? N8 C26 1.467(5) . ? N9 C33 1.343(5) . ? N9 C29 1.351(5) . ? C1 C2 1.521(6) . ? C3 C4 1.500(7) . ? C4 C5 1.541(7) . ? C6 C7 1.514(6) . ? C8 C9 1.520(5) . ? C9 C10 1.517(6) . ? C11 C12 1.514(6) . ? C12 C13 1.387(6) . ? C13 C14 1.390(7) . ? C14 C15 1.380(7) . ? C15 C16 1.362(6) . ? C17 C18 1.510(6) . ? C18 C19 1.399(6) . ? C19 C20 1.376(7) . ? C20 C21 1.390(7) . ? C21 C22 1.377(6) . ? C25 C24 1.504(5) . ? C24 C23 1.535(5) . ? C28 C29 1.496(6) . ? C29 C30 1.397(5) . ? C30 C31 1.382(6) . ? C31 C32 1.386(7) . ? C32 C33 1.380(6) . ? C26 C27 1.536(5) 3_755 ? Cl1 O14' 1.40(3) . ? Cl1 O13' 1.403(15) . ? Cl1 O12 1.407(6) . ? Cl1 O11 1.421(4) . ? Cl1 O14 1.448(5) . ? Cl1 O13 1.453(5) . ? Cl1 O12' 1.576(17) . ? Cl2 O21' 1.339(13) . ? Cl2 O23' 1.382(7) . ? Cl2 O22' 1.383(11) . ? Cl2 O24' 1.416(7) . ? Cl2 O23 1.457(7) . ? Cl2 O22 1.509(7) . ? Cl2 O21 1.515(7) . ? Cl2 O24 1.533(7) . ? Cl3 O32' 1.317(14) . ? Cl3 O33 1.349(5) . ? Cl3 O34 1.432(7) . ? Cl3 O31 1.439(5) . ? Cl3 O32 1.468(6) . ? Cl3 O34' 1.530(14) . ? Cl3 O33' 1.534(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 O2 Cu1 O3 92.01(11) . . ? O2 Cu1 N9 92.95(12) . . ? O3 Cu1 N9 171.74(12) . . ? O2 Cu1 N7 168.39(12) . . ? O3 Cu1 N7 90.09(11) . . ? N9 Cu1 N7 83.76(12) . . ? O2 Cu1 O1W 98.60(11) . . ? O3 Cu1 O1W 99.87(11) . . ? N9 Cu1 O1W 85.92(12) . . ? N7 Cu1 O1W 92.29(12) . . ? N4 Cu2 N5 175.48(13) . . ? N4 Cu2 N1 92.89(13) . . ? N5 Cu2 N1 83.52(13) . . ? N4 Cu2 N6 91.12(12) . . ? N5 Cu2 N6 89.16(13) . . ? N1 Cu2 N6 130.52(13) . . ? N4 Cu2 N3 83.31(12) . . ? N5 Cu2 N3 101.16(12) . . ? N1 Cu2 N3 151.09(13) . . ? N6 Cu2 N3 78.32(12) . . ? C8 O2 Cu1 135.1(2) . . ? C25 O3 Cu1 133.5(2) . . ? C1 N1 C11 110.8(3) . . ? C1 N1 C10 109.9(3) . . ? C11 N1 C10 106.8(3) . . ? C1 N1 Cu2 114.6(3) . . ? C11 N1 Cu2 107.7(2) . . ? C10 N1 Cu2 106.7(2) . . ? C3 N2 C2 124.8(4) . . ? C6 N3 C17 108.8(3) . . ? C6 N3 C5 110.2(3) . . ? C17 N3 C5 106.0(3) . . ? C6 N3 Cu2 99.5(2) . . ? C17 N3 Cu2 107.9(2) . . ? C5 N3 Cu2 123.8(3) . . ? C8 N4 C7 116.8(3) . . ? C8 N4 Cu2 130.1(3) . . ? C7 N4 Cu2 112.2(2) . . ? C12 N5 C16 118.3(4) . . ? C12 N5 Cu2 115.3(3) . . ? C16 N5 Cu2 126.1(3) . . ? C18 N6 C22 119.4(3) . . ? C18 N6 Cu2 118.1(3) . . ? C22 N6 Cu2 122.3(3) . . ? C27 N7 C28 110.1(3) . . ? C27 N7 C23 111.0(3) . . ? C28 N7 C23 107.8(3) . . ? C27 N7 Cu1 114.5(2) . . ? C28 N7 Cu1 103.5(2) . . ? C23 N7 Cu1 109.5(2) . . ? C25 N8 C26 122.3(3) . . ? C33 N9 C29 119.4(3) . . ? C33 N9 Cu1 127.7(3) . . ? C29 N9 Cu1 112.7(3) . . ? N1 C1 C2 113.3(4) . . ? N2 C2 C1 109.3(4) . . ? O1 C3 N2 122.5(5) . . ? O1 C3 C4 122.2(4) . . ? N2 C3 C4 115.1(4) . . ? C3 C4 C5 112.2(4) . . ? N3 C5 C4 115.8(4) . . ? N3 C6 C7 111.2(3) . . ? N4 C7 C6 108.2(3) . . ? O2 C8 N4 122.3(3) . . ? O2 C8 C9 117.7(3) . . ? N4 C8 C9 119.9(3) . . ? C10 C9 C8 118.5(3) . . ? N1 C10 C9 115.4(3) . . ? N1 C11 C12 112.5(3) . . ? N5 C12 C13 121.6(4) . . ? N5 C12 C11 116.6(4) . . ? C13 C12 C11 121.6(4) . . ? C12 C13 C14 119.3(5) . . ? C15 C14 C13 118.5(4) . . ? C16 C15 C14 119.3(4) . . ? N5 C16 C15 122.9(4) . . ? N3 C17 C18 115.3(3) . . ? N6 C18 C19 121.1(4) . . ? N6 C18 C17 118.2(4) . . ? C19 C18 C17 120.5(4) . . ? C20 C19 C18 119.3(4) . . ? C19 C20 C21 119.4(4) . . ? C22 C21 C20 118.5(4) . . ? N6 C22 C21 122.1(4) . . ? O3 C25 N8 119.9(3) . . ? O3 C25 C24 123.1(3) . . ? N8 C25 C24 117.0(3) . . ? C25 C24 C23 114.9(3) . . ? N7 C23 C24 114.9(3) . . ? C29 C28 N7 110.2(3) . . ? N9 C29 C30 121.5(4) . . ? N9 C29 C28 115.4(3) . . ? C30 C29 C28 123.1(4) . . ? C31 C30 C29 118.9(4) . . ? C30 C31 C32 119.0(4) . . ? C33 C32 C31 119.7(4) . . ? N9 C33 C32 121.6(4) . . ? N8 C26 C27 114.3(3) . 3_755 ? N7 C27 C26 116.5(3) . 3_755 ? #===END