Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'L. Thompson' 'Julie L. Collins' 'Loiuse N. Dawe' 'Victoria A. Milway' 'Santokh Tandon' _publ_contact_author_name L.Thompson _publ_contact_author_address ; Department of Chemistry Memorial University of St John's Newfoundland A1B 3X7 CANADA ; _publ_contact_author_email LTHOMP@MUN.CA _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Linear Copper 'chain' complexes with bulky tritopic hydrazone ligands - structural and magnetic studies. ; data_shelxl_(3) _database_code_depnum_ccdc_archive 'CCDC 630952' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H31 Cl2 Cu3 N10 O18.50 ' _chemical_formula_weight 1185.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.241(2) _cell_length_b 10.3565(19) _cell_length_c 10.819(2) _cell_angle_alpha 89.755(4) _cell_angle_beta 90.118(6) _cell_angle_gamma 98.288(5) _cell_volume 1135.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5210 _cell_measurement_theta_min 2.6148 _cell_measurement_theta_max 30.5746 _exptl_crystal_description Prism _exptl_crystal_colour Blue/Brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 1.597 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6149 _exptl_absorpt_correction_T_max 0.8159 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 14929 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4795 _reflns_number_gt 4663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0732P)^2^+1.9195P] 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 4795 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.85442(3) 0.43375(3) 0.71809(3) 0.01873(12) Uani 1 1 d . . . Cu2 Cu 0.5000 0.5000 1.0000 0.02124(14) Uani 1 2 d S . . Cl1 Cl 1.11648(7) 0.87285(6) 1.06987(6) 0.02663(17) Uani 1 1 d . . . O1 O 1.22154(19) 0.5488(2) 0.67454(18) 0.0269(4) Uani 1 1 d . . . O2 O 1.03320(19) 0.44052(19) 0.65247(18) 0.0253(4) Uani 1 1 d . . . O3 O 0.67808(18) 0.57217(18) 1.01298(18) 0.0238(4) Uani 1 1 d . . . O4 O 0.43293(19) 0.6136(2) 0.85494(19) 0.0262(4) Uani 1 1 d . . . O5 O 0.8896(3) 0.7828(2) 0.5958(2) 0.0459(6) Uani 1 1 d . . . O6 O 0.8024(3) 0.8550(3) 0.7608(3) 0.0534(7) Uani 1 1 d . . . O7 O 0.9833(3) 0.9298(3) 0.7144(3) 0.0492(7) Uani 1 1 d . . . O8 O 0.7589(2) 0.5610(2) 0.56204(18) 0.0249(4) Uani 1 1 d . . . O9 O 0.5096(8) 0.4081(9) 1.4918(10) 0.040(2) Uani 0.25 1 d P . . O10 O 0.5849(5) 0.7157(5) 0.6993(5) 0.0688(13) Uiso 0.70 1 d P . . O11 O 0.5317(13) 0.7761(13) 0.7085(11) 0.068(3) Uiso 0.30 1 d P . . N1 N 0.9417(2) 0.5581(2) 0.8320(2) 0.0187(4) Uani 1 1 d . . . N2 N 0.7291(2) 0.4474(2) 0.8430(2) 0.0199(4) Uani 1 1 d . . . N3 N 0.6140(2) 0.3825(2) 0.8478(2) 0.0205(4) Uani 1 1 d . . . N4 N 0.7746(2) 0.2827(2) 0.6414(2) 0.0216(5) Uani 1 1 d . . . N5 N 0.8914(3) 0.8560(3) 0.6903(2) 0.0323(6) Uani 1 1 d . . . C1 C 1.1099(3) 0.5247(3) 0.7035(2) 0.0217(5) Uani 1 1 d . . . C2 C 1.0588(2) 0.5998(3) 0.8104(2) 0.0200(5) Uani 1 1 d . . . C3 C 1.1182(3) 0.6980(3) 0.8828(2) 0.0215(5) Uani 1 1 d . . . H1 H 1.2076 0.7333 0.8674 0.026 Uiso 1 1 calc R . . C4 C 1.0514(3) 0.7479(2) 0.9787(2) 0.0202(5) Uani 1 1 d . . . C5 C 0.9306(3) 0.6998(2) 1.0036(2) 0.0202(5) Uani 1 1 d . . . H2 H 0.8830 0.7287 1.0709 0.024 Uiso 1 1 calc R . . C6 C 0.8779(2) 0.6040(2) 0.9249(2) 0.0184(5) Uani 1 1 d . . . C7 C 0.7498(2) 0.5389(2) 0.9307(2) 0.0194(5) Uani 1 1 d . . . C8 C 0.5882(2) 0.2865(2) 0.7738(2) 0.0197(5) Uani 1 1 d . . . C9 C 0.4636(3) 0.2216(2) 0.7940(2) 0.0212(5) Uani 1 1 d . . . C10 C 0.4584(3) 0.1623(3) 0.9124(3) 0.0269(6) Uani 1 1 d . . . H3 H 0.5295 0.1704 0.9697 0.032 Uiso 1 1 calc R . . C11 C 0.3458(3) 0.0968(3) 0.9313(3) 0.0318(7) Uani 1 1 d . . . H4 H 0.3283 0.0508 1.0071 0.038 Uiso 1 1 calc R . . C12 C 0.2385(3) 0.0915(3) 0.8333(3) 0.0313(7) Uani 1 1 d . . . H5 H 0.1578 0.0380 0.8532 0.038 Uiso 1 1 calc R . . C13 C 0.2410(3) 0.1543(3) 0.7173(3) 0.0284(6) Uani 1 1 d . . . H6 H 0.1682 0.1491 0.6621 0.034 Uiso 1 1 calc R . . C14 C 0.3539(3) 0.2188(3) 0.6967(3) 0.0253(6) Uani 1 1 d . . . H7 H 0.3705 0.2653 0.6211 0.030 Uiso 1 1 calc R . . C15 C 0.6665(3) 0.2278(3) 0.6779(2) 0.0215(5) Uani 1 1 d . . . C16 C 0.6281(3) 0.1106(3) 0.6295(3) 0.0291(6) Uani 1 1 d . . . H8 H 0.5476 0.0628 0.6583 0.035 Uiso 1 1 calc R . . C17 C 0.6972(3) 0.0532(3) 0.5400(3) 0.0370(7) Uani 1 1 d . . . H9 H 0.6633 -0.0304 0.5085 0.044 Uiso 1 1 calc R . . C18 C 0.8041(3) 0.1120(3) 0.5010(3) 0.0378(8) Uani 1 1 d . . . H10 H 0.8546 0.0780 0.4385 0.045 Uiso 1 1 calc R . . C19 C 0.8408(3) 0.2258(3) 0.5545(3) 0.0285(6) Uani 1 1 d . . . H11 H 0.9229 0.2728 0.5289 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01565(18) 0.01741(18) 0.02041(18) -0.00462(12) 0.00887(12) -0.00711(12) Cu2 0.0144(2) 0.0220(2) 0.0241(2) -0.00554(17) 0.00961(17) -0.00883(17) Cl1 0.0242(3) 0.0209(3) 0.0311(3) -0.0064(2) 0.0056(3) -0.0100(3) O1 0.0170(9) 0.0319(10) 0.0276(10) -0.0050(8) 0.0120(7) -0.0104(8) O2 0.0188(9) 0.0249(9) 0.0288(10) -0.0085(8) 0.0124(7) -0.0085(8) O3 0.0176(9) 0.0224(9) 0.0279(9) -0.0099(7) 0.0120(7) -0.0096(7) O4 0.0209(9) 0.0243(9) 0.0300(10) -0.0041(8) 0.0075(8) -0.0087(8) O5 0.0568(16) 0.0307(12) 0.0431(13) -0.0079(10) 0.0128(12) -0.0183(11) O6 0.0458(15) 0.0598(18) 0.0518(16) 0.0097(13) 0.0251(13) -0.0021(13) O7 0.0440(14) 0.0397(14) 0.0572(16) -0.0146(12) 0.0119(12) -0.0177(12) O8 0.0250(10) 0.0254(10) 0.0223(9) -0.0017(7) 0.0078(7) -0.0029(8) O9 0.012(4) 0.037(5) 0.067(6) 0.013(4) 0.008(4) -0.008(3) N1 0.0151(10) 0.0177(10) 0.0209(10) -0.0017(8) 0.0070(8) -0.0057(8) N2 0.0154(10) 0.0179(10) 0.0232(10) -0.0032(8) 0.0096(8) -0.0084(8) N3 0.0161(10) 0.0176(10) 0.0247(11) -0.0033(8) 0.0082(8) -0.0086(8) N4 0.0187(10) 0.0192(10) 0.0245(11) -0.0038(8) 0.0094(8) -0.0054(9) N5 0.0316(13) 0.0304(13) 0.0323(13) 0.0025(10) 0.0070(11) -0.0044(11) C1 0.0182(12) 0.0232(12) 0.0216(12) -0.0019(9) 0.0070(9) -0.0043(10) C2 0.0157(11) 0.0207(12) 0.0216(12) 0.0007(9) 0.0062(9) -0.0039(10) C3 0.0168(11) 0.0206(12) 0.0245(12) -0.0001(10) 0.0068(9) -0.0063(10) C4 0.0188(12) 0.0160(11) 0.0233(12) -0.0003(9) 0.0019(9) -0.0059(9) C5 0.0168(12) 0.0180(11) 0.0243(12) -0.0036(9) 0.0076(9) -0.0033(10) C6 0.0148(11) 0.0168(11) 0.0217(12) -0.0007(9) 0.0061(9) -0.0042(9) C7 0.0153(11) 0.0177(11) 0.0230(12) -0.0025(9) 0.0071(9) -0.0055(9) C8 0.0157(11) 0.0173(11) 0.0241(12) -0.0022(9) 0.0064(9) -0.0043(9) C9 0.0182(12) 0.0160(11) 0.0268(13) -0.0053(9) 0.0087(10) -0.0064(10) C10 0.0230(13) 0.0242(13) 0.0308(14) -0.0011(11) 0.0062(11) -0.0061(11) C11 0.0321(15) 0.0230(13) 0.0370(16) 0.0014(11) 0.0149(12) -0.0074(12) C12 0.0234(14) 0.0204(13) 0.0466(17) -0.0099(12) 0.0155(12) -0.0095(11) C13 0.0201(13) 0.0245(13) 0.0381(15) -0.0124(11) 0.0046(11) -0.0053(11) C14 0.0213(13) 0.0235(13) 0.0291(13) -0.0041(10) 0.0069(11) -0.0040(11) C15 0.0196(12) 0.0185(12) 0.0245(12) -0.0045(9) 0.0058(9) -0.0039(10) C16 0.0228(13) 0.0202(13) 0.0418(16) -0.0093(11) 0.0115(12) -0.0059(11) C17 0.0329(16) 0.0236(14) 0.0509(19) -0.0177(13) 0.0145(14) -0.0086(13) C18 0.0320(16) 0.0315(16) 0.0472(19) -0.0180(14) 0.0193(14) -0.0052(13) C19 0.0261(14) 0.0241(13) 0.0327(14) -0.0071(11) 0.0135(11) -0.0055(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.855(2) . ? Cu1 N2 1.886(2) . ? Cu1 N1 1.911(2) . ? Cu1 O2 1.9568(19) . ? Cu1 O8 2.427(2) . ? Cu2 O3 1.8738(18) 2_667 ? Cu2 O3 1.8739(18) . ? Cu2 O4 2.129(2) 2_667 ? Cu2 O4 2.129(2) . ? Cu2 N3 2.448(2) 2_667 ? Cu2 N3 2.448(2) . ? Cl1 C4 1.688(3) . ? O1 C1 1.178(3) . ? O2 C1 1.219(3) . ? O3 C7 1.237(3) . ? O5 N5 1.274(4) . ? O6 N5 1.188(4) . ? O7 N5 1.154(4) . ? O10 O11 0.893(12) . ? N1 C2 1.237(3) . ? N1 C6 1.327(3) . ? N2 N3 1.271(3) . ? N2 C7 1.338(3) . ? N3 C8 1.276(3) . ? N4 C15 1.235(3) . ? N4 C19 1.346(4) . ? C1 C2 1.530(4) . ? C2 C3 1.359(4) . ? C3 C4 1.386(4) . ? C4 C5 1.294(3) . ? C5 C6 1.361(4) . ? C6 C7 1.387(3) . ? C8 C9 1.372(3) . ? C8 C15 1.496(4) . ? C9 C10 1.416(4) . ? C9 C14 1.535(4) . ? C10 C11 1.267(4) . ? C11 C12 1.521(5) . ? C12 C13 1.410(5) . ? C13 C14 1.268(4) . ? C15 C16 1.331(4) . ? C16 C17 1.386(4) . ? C17 C18 1.247(4) . ? C18 C19 1.321(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N2 99.48(9) . . ? N4 Cu1 N1 164.87(10) . . ? N2 Cu1 N1 75.07(9) . . ? N4 Cu1 O2 99.33(9) . . ? N2 Cu1 O2 154.53(9) . . ? N1 Cu1 O2 82.38(9) . . ? N4 Cu1 O8 89.03(9) . . ? N2 Cu1 O8 97.18(9) . . ? N1 Cu1 O8 105.53(8) . . ? O2 Cu1 O8 100.15(8) . . ? O3 Cu2 O3 179.999(1) 2_667 . ? O3 Cu2 O4 101.97(8) 2_667 2_667 ? O3 Cu2 O4 78.03(8) . 2_667 ? O3 Cu2 O4 78.03(8) 2_667 . ? O3 Cu2 O4 101.97(8) . . ? O4 Cu2 O4 179.999(2) 2_667 . ? O3 Cu2 N3 75.06(8) 2_667 2_667 ? O3 Cu2 N3 104.94(8) . 2_667 ? O4 Cu2 N3 89.63(8) 2_667 2_667 ? O4 Cu2 N3 90.37(8) . 2_667 ? O3 Cu2 N3 104.94(8) 2_667 . ? O3 Cu2 N3 75.06(8) . . ? O4 Cu2 N3 90.37(8) 2_667 . ? O4 Cu2 N3 89.63(8) . . ? N3 Cu2 N3 179.999(1) 2_667 . ? C1 O2 Cu1 111.26(17) . . ? C7 O3 Cu2 114.71(17) . . ? C2 N1 C6 121.4(2) . . ? C2 N1 Cu1 116.65(19) . . ? C6 N1 Cu1 121.79(17) . . ? N3 N2 C7 112.8(2) . . ? N3 N2 Cu1 125.35(18) . . ? C7 N2 Cu1 121.56(17) . . ? N2 N3 C8 117.3(2) . . ? N2 N3 Cu2 103.68(16) . . ? C8 N3 Cu2 138.84(18) . . ? C15 N4 C19 119.8(2) . . ? C15 N4 Cu1 120.07(19) . . ? C19 N4 Cu1 119.76(19) . . ? O7 N5 O6 114.2(3) . . ? O7 N5 O5 121.2(3) . . ? O6 N5 O5 124.6(3) . . ? O1 C1 O2 122.4(3) . . ? O1 C1 C2 119.2(2) . . ? O2 C1 C2 118.4(2) . . ? N1 C2 C3 117.3(2) . . ? N1 C2 C1 110.6(2) . . ? C3 C2 C1 132.1(2) . . ? C2 C3 C4 121.5(2) . . ? C5 C4 C3 120.6(2) . . ? C5 C4 Cl1 115.0(2) . . ? C3 C4 Cl1 124.4(2) . . ? C4 C5 C6 114.0(2) . . ? N1 C6 C5 125.1(2) . . ? N1 C6 C7 109.9(2) . . ? C5 C6 C7 125.0(2) . . ? O3 C7 N2 132.1(2) . . ? O3 C7 C6 117.1(2) . . ? N2 C7 C6 110.8(2) . . ? N3 C8 C9 110.8(2) . . ? N3 C8 C15 133.8(2) . . ? C9 C8 C15 115.3(2) . . ? C8 C9 C10 109.3(2) . . ? C8 C9 C14 121.8(2) . . ? C10 C9 C14 128.9(2) . . ? C11 C10 C9 110.6(3) . . ? C10 C11 C12 120.3(3) . . ? C13 C12 C11 129.5(2) . . ? C14 C13 C12 110.7(3) . . ? C13 C14 C9 119.9(3) . . ? N4 C15 C16 114.9(3) . . ? N4 C15 C8 122.2(2) . . ? C16 C15 C8 122.8(2) . . ? C15 C16 C17 124.6(3) . . ? C18 C17 C16 119.7(3) . . ? C17 C18 C19 113.7(3) . . ? C18 C19 N4 127.2(3) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.955 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.100 #===END data_shelxl_(4) _database_code_depnum_ccdc_archive 'CCDC 630953' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.50 H31.50 Cl2 Cu2 N8.50 O11.50' _chemical_formula_weight 959.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.310(3) _cell_length_b 16.369(3) _cell_length_c 18.756(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.994(4) _cell_angle_gamma 90.00 _cell_volume 3908.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15150 _cell_measurement_theta_min 2.0266 _cell_measurement_theta_max 30.7845 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.7380 _exptl_absorpt_correction_T_max 0.9090 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 36349 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8934 _reflns_number_gt 8239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0990P)^2^+10.1671P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8934 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.2046 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.99968(4) 0.30742(3) 0.37169(3) 0.02988(17) Uani 1 1 d . . . Cu2 Cu 1.00134(4) 0.32824(4) 0.11415(3) 0.03385(17) Uani 1 1 d . . . Cl1 Cl 0.93795(11) 0.03366(8) 0.32406(7) 0.0483(3) Uani 1 1 d . . . Cl2 Cl 0.48290(14) 0.10251(13) 0.29194(15) 0.0872(7) Uani 1 1 d . . . O1 O 1.0910(3) 0.1571(2) 0.54919(17) 0.0368(7) Uani 1 1 d . . . O2 O 1.1007(3) 0.2564(2) 0.18955(16) 0.0359(7) Uani 1 1 d . . . O3 O 1.0080(4) 0.0375(4) 0.3992(3) 0.0766(14) Uani 1 1 d . . . O4 O 0.9937(6) 0.0553(4) 0.2743(3) 0.100(2) Uani 1 1 d . . . O5 O 0.8567(5) 0.0895(4) 0.3204(3) 0.099(2) Uani 1 1 d . . . O6 O 0.9012(5) -0.0472(3) 0.3125(4) 0.0900(18) Uani 1 1 d . . . O7 O 0.5736(4) 0.0812(4) 0.2698(4) 0.0932(19) Uani 1 1 d . . . O8 O 0.3907(5) 0.1054(5) 0.2295(4) 0.109(2) Uani 1 1 d . . . O9 O 0.4638(5) 0.0406(4) 0.3421(4) 0.101(2) Uani 1 1 d . . . O10 O 0.4993(6) 0.1777(4) 0.3327(6) 0.141(4) Uani 1 1 d . . . O11 O 1.4559(8) 0.3678(10) 0.0722(10) 0.111(6) Uani 0.50 1 d P . . O12 O 1.1616(4) 0.3883(3) 0.4025(3) 0.0638(12) Uani 1 1 d . . . N1 N 0.9282(3) 0.4037(2) 0.39324(19) 0.0303(7) Uani 1 1 d . . . N2 N 0.9465(3) 0.2757(2) 0.51427(19) 0.0308(7) Uani 1 1 d . . . N3 N 1.0133(3) 0.2644(2) 0.47131(19) 0.0315(8) Uani 1 1 d . . . N4 N 1.0993(3) 0.2212(2) 0.37406(19) 0.0316(7) Uani 1 1 d . . . N5 N 0.9927(3) 0.2970(2) 0.26043(17) 0.0291(7) Uani 1 1 d . . . N6 N 0.9345(3) 0.3298(2) 0.19300(19) 0.0309(7) Uani 1 1 d . . . N7 N 0.8681(3) 0.3854(2) 0.0617(2) 0.0335(8) Uani 1 1 d . . . N8 N 1.3781(9) 0.3239(7) 0.1406(7) 0.064(3) Uani 0.50 1 d P . . N9 N 1.3108(13) 0.3885(10) 0.3669(9) 0.089(4) Uiso 0.50 1 d P . . N10 N 1.3403(15) 0.4206(11) 0.4200(11) 0.100(5) Uiso 0.50 1 d P . . C1 C 0.9334(4) 0.4710(3) 0.3529(2) 0.0355(9) Uani 1 1 d . . . H1 H 0.9635 0.4665 0.3129 0.043 Uiso 1 1 calc R . . C2 C 0.8969(4) 0.5456(3) 0.3674(3) 0.0421(11) Uani 1 1 d . . . H2 H 0.9018 0.5919 0.3381 0.050 Uiso 1 1 calc R . . C3 C 0.8529(5) 0.5526(3) 0.4251(3) 0.0455(12) Uani 1 1 d . . . H3 H 0.8276 0.6038 0.4363 0.055 Uiso 1 1 calc R . . C4 C 0.8461(4) 0.4840(3) 0.4664(3) 0.0392(10) Uani 1 1 d . . . H4 H 0.8142 0.4877 0.5054 0.047 Uiso 1 1 calc R . . C5 C 0.8857(3) 0.4097(3) 0.4510(2) 0.0312(8) Uani 1 1 d . . . C6 C 0.8856(3) 0.3386(3) 0.5011(2) 0.0310(8) Uani 1 1 d . . . C7 C 0.8047(4) 0.3384(3) 0.5429(2) 0.0338(9) Uani 1 1 d . . . C8 C 0.8141(4) 0.3833(4) 0.6072(3) 0.0438(11) Uani 1 1 d . . . H5 H 0.8753 0.4151 0.6283 0.053 Uiso 1 1 calc R . . C9 C 0.7333(4) 0.3818(4) 0.6412(3) 0.0500(13) Uani 1 1 d . . . H6 H 0.7399 0.4126 0.6852 0.060 Uiso 1 1 calc R . . C10 C 0.6447(4) 0.3360(4) 0.6111(3) 0.0522(14) Uani 1 1 d . . . H7 H 0.5894 0.3363 0.6336 0.063 Uiso 1 1 calc R . . C11 C 0.6358(4) 0.2897(4) 0.5484(3) 0.0509(13) Uani 1 1 d . . . H8 H 0.5755 0.2565 0.5287 0.061 Uiso 1 1 calc R . . C12 C 0.7148(4) 0.2914(3) 0.5138(3) 0.0434(11) Uani 1 1 d . . . H9 H 0.7075 0.2602 0.4698 0.052 Uiso 1 1 calc R . . C13 C 1.0784(4) 0.2008(3) 0.4925(2) 0.0332(9) Uani 1 1 d . . . C14 C 1.1395(4) 0.1830(3) 0.4383(2) 0.0340(9) Uani 1 1 d . . . C15 C 1.2271(4) 0.1352(4) 0.4501(3) 0.0477(13) Uani 1 1 d . . . H10 H 1.2561 0.1077 0.4961 0.057 Uiso 1 1 calc R . . C16 C 1.2725(4) 0.1283(4) 0.3919(3) 0.0496(13) Uani 1 1 d . . . H11 H 1.3346 0.0969 0.3989 0.060 Uiso 1 1 calc R . . C17 C 1.2275(4) 0.1670(3) 0.3237(3) 0.0412(11) Uani 1 1 d . . . H12 H 1.2570 0.1615 0.2835 0.049 Uiso 1 1 calc R . . C18 C 1.1395(4) 0.2133(3) 0.3167(2) 0.0329(9) Uani 1 1 d . . . C19 C 1.0756(3) 0.2587(3) 0.2498(2) 0.0319(9) Uani 1 1 d . . . C20 C 0.8394(4) 0.3553(3) 0.1788(2) 0.0316(9) Uani 1 1 d . . . C21 C 0.7755(3) 0.3491(3) 0.2311(2) 0.0317(8) Uani 1 1 d . . . C22 C 0.7725(4) 0.2744(3) 0.2665(2) 0.0350(9) Uani 1 1 d . . . H13 H 0.8146 0.2300 0.2594 0.042 Uiso 1 1 calc R . . C23 C 0.7077(4) 0.2651(3) 0.3121(3) 0.0428(11) Uani 1 1 d . . . H14 H 0.7036 0.2138 0.3349 0.051 Uiso 1 1 calc R . . C24 C 0.6496(4) 0.3303(4) 0.3243(3) 0.0505(13) Uani 1 1 d . . . H15 H 0.6059 0.3237 0.3559 0.061 Uiso 1 1 calc R . . C25 C 0.6538(4) 0.4049(4) 0.2915(3) 0.0482(12) Uani 1 1 d . . . H16 H 0.6143 0.4495 0.3014 0.058 Uiso 1 1 calc R . . C26 C 0.7159(4) 0.4153(3) 0.2437(3) 0.0377(10) Uani 1 1 d . . . H17 H 0.7177 0.4663 0.2200 0.045 Uiso 1 1 calc R . . C27 C 0.7979(4) 0.3871(3) 0.1020(2) 0.0336(9) Uani 1 1 d . . . C28 C 0.6953(4) 0.4115(3) 0.0703(3) 0.0412(10) Uani 1 1 d . . . H18 H 0.6468 0.4114 0.0987 0.049 Uiso 1 1 calc R . . C29 C 0.6640(5) 0.4362(4) -0.0037(3) 0.0478(12) Uani 1 1 d . . . H19 H 0.5936 0.4531 -0.0264 0.057 Uiso 1 1 calc R . . C30 C 0.7352(5) 0.4363(4) -0.0439(3) 0.0490(13) Uani 1 1 d . . . H20 H 0.7151 0.4536 -0.0944 0.059 Uiso 1 1 calc R . . C31 C 0.8383(4) 0.4102(3) -0.0089(3) 0.0420(11) Uani 1 1 d . . . H21 H 0.8881 0.4104 -0.0363 0.050 Uiso 1 1 calc R . . C32 C 1.4327(10) 0.3685(15) 0.1111(9) 0.078(5) Uani 0.50 1 d P . . H22 H 1.4547 0.4168 0.1396 0.093 Uiso 0.50 1 calc PR . . C33 C 1.3393(17) 0.2501(11) 0.1118(10) 0.100(6) Uani 0.50 1 d P . . H23 H 1.3866 0.2256 0.0863 0.120 Uiso 0.50 1 calc PR . . H24 H 1.2696 0.2576 0.0761 0.120 Uiso 0.50 1 calc PR . . H25 H 1.3339 0.2140 0.1521 0.120 Uiso 0.50 1 calc PR . . C34 C 1.3521(12) 0.3508(13) 0.2041(13) 0.107(8) Uani 0.50 1 d P . . H26 H 1.2848 0.3268 0.2045 0.128 Uiso 0.50 1 calc PR . . H27 H 1.3464 0.4105 0.2030 0.128 Uiso 0.50 1 calc PR . . H28 H 1.4070 0.3339 0.2490 0.128 Uiso 0.50 1 calc PR . . C35 C 1.2216(8) 0.4048(5) 0.3658(6) 0.087(3) Uani 1 1 d . . . C36 C 1.377(2) 0.3486(18) 0.4355(16) 0.129(8) Uiso 0.50 1 d P . . C37 C 1.355(2) 0.4035(19) 0.4868(17) 0.137(9) Uiso 0.50 1 d P . . C38 C 1.357(2) 0.4074(16) 0.3039(15) 0.122(7) Uiso 0.50 1 d P . . C39 C 1.414(2) 0.4444(16) 0.3835(16) 0.129(8) Uiso 0.50 1 d P . . 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 0.0356(3) 0.0377(3) 0.0204(3) 0.00193(19) 0.0145(2) 0.0045(2) Cu2 0.0405(3) 0.0446(3) 0.0208(3) 0.0001(2) 0.0157(2) 0.0003(2) Cl1 0.0630(8) 0.0432(7) 0.0441(7) 0.0024(5) 0.0242(6) 0.0108(6) Cl2 0.0472(8) 0.0884(13) 0.1369(19) -0.0468(13) 0.0438(11) -0.0132(8) O1 0.0423(17) 0.0497(19) 0.0236(14) 0.0075(13) 0.0179(13) 0.0117(14) O2 0.0428(17) 0.0463(18) 0.0249(14) 0.0005(13) 0.0196(13) 0.0042(14) O3 0.092(4) 0.079(3) 0.055(3) -0.005(3) 0.016(3) 0.011(3) O4 0.145(6) 0.107(4) 0.077(4) -0.021(3) 0.078(4) -0.035(4) O5 0.144(5) 0.107(4) 0.049(3) 0.015(3) 0.032(3) 0.088(4) O6 0.080(4) 0.054(3) 0.121(5) 0.010(3) 0.006(3) -0.005(2) O7 0.062(3) 0.124(5) 0.112(5) -0.007(4) 0.054(3) 0.011(3) O8 0.076(4) 0.112(5) 0.135(6) -0.006(5) 0.026(4) 0.019(4) O9 0.078(4) 0.128(5) 0.112(5) -0.059(4) 0.052(4) -0.053(4) O10 0.112(5) 0.104(5) 0.243(10) -0.095(6) 0.109(6) -0.051(4) O11 0.022(5) 0.119(10) 0.170(16) 0.061(11) -0.005(7) -0.004(5) O12 0.062(3) 0.064(3) 0.081(3) -0.026(2) 0.044(2) -0.020(2) N1 0.0357(18) 0.0345(18) 0.0229(15) 0.0003(14) 0.0123(14) -0.0007(14) N2 0.0363(18) 0.0384(19) 0.0231(16) 0.0021(14) 0.0171(14) 0.0044(15) N3 0.0370(18) 0.042(2) 0.0225(16) 0.0058(14) 0.0193(14) 0.0082(15) N4 0.0371(18) 0.041(2) 0.0207(15) 0.0010(14) 0.0154(14) 0.0035(15) N5 0.0366(18) 0.0398(19) 0.0138(14) 0.0022(13) 0.0119(13) 0.0033(14) N6 0.0363(18) 0.0383(19) 0.0211(16) 0.0006(14) 0.0131(14) 0.0040(15) N7 0.043(2) 0.038(2) 0.0224(16) 0.0008(14) 0.0128(15) -0.0034(15) N8 0.055(6) 0.068(7) 0.058(6) 0.027(6) -0.001(5) -0.004(5) C1 0.038(2) 0.041(2) 0.029(2) 0.0028(18) 0.0111(17) -0.0014(18) C2 0.054(3) 0.038(2) 0.034(2) 0.006(2) 0.013(2) 0.000(2) C3 0.061(3) 0.039(2) 0.041(3) 0.003(2) 0.022(2) 0.007(2) C4 0.049(3) 0.039(2) 0.033(2) 0.0018(19) 0.019(2) 0.008(2) C5 0.033(2) 0.040(2) 0.0236(18) -0.0002(17) 0.0131(16) 0.0030(17) C6 0.035(2) 0.038(2) 0.0246(19) 0.0010(16) 0.0145(16) 0.0024(17) C7 0.040(2) 0.038(2) 0.029(2) 0.0076(17) 0.0205(18) 0.0076(18) C8 0.045(3) 0.058(3) 0.033(2) 0.001(2) 0.019(2) 0.007(2) C9 0.054(3) 0.069(4) 0.037(2) 0.005(2) 0.028(2) 0.014(3) C10 0.045(3) 0.072(4) 0.050(3) 0.016(3) 0.029(2) 0.015(3) C11 0.041(3) 0.064(3) 0.054(3) 0.015(3) 0.022(2) 0.006(2) C12 0.042(3) 0.053(3) 0.040(3) 0.004(2) 0.020(2) 0.000(2) C13 0.036(2) 0.044(2) 0.0230(19) 0.0016(17) 0.0141(16) 0.0056(18) C14 0.036(2) 0.045(2) 0.025(2) 0.0036(18) 0.0158(17) 0.0088(18) C15 0.041(3) 0.074(4) 0.032(2) 0.011(2) 0.016(2) 0.025(2) C16 0.045(3) 0.071(4) 0.040(3) 0.012(2) 0.023(2) 0.027(3) C17 0.041(2) 0.059(3) 0.030(2) 0.002(2) 0.0204(19) 0.010(2) C18 0.037(2) 0.045(2) 0.0215(18) -0.0003(17) 0.0149(16) 0.0036(18) C19 0.036(2) 0.042(2) 0.0210(18) -0.0022(17) 0.0140(16) -0.0010(17) C20 0.038(2) 0.037(2) 0.0220(18) -0.0025(16) 0.0119(16) -0.0011(17) C21 0.032(2) 0.038(2) 0.0265(19) 0.0005(17) 0.0107(16) -0.0007(17) C22 0.037(2) 0.038(2) 0.030(2) -0.0006(18) 0.0104(17) -0.0026(18) C23 0.043(3) 0.053(3) 0.036(2) 0.007(2) 0.017(2) -0.003(2) C24 0.043(3) 0.073(4) 0.044(3) 0.011(3) 0.025(2) 0.002(2) C25 0.040(3) 0.068(3) 0.043(3) 0.003(3) 0.022(2) 0.010(2) C26 0.038(2) 0.044(2) 0.034(2) 0.0059(19) 0.0141(19) 0.0067(19) C27 0.040(2) 0.039(2) 0.0226(19) -0.0006(17) 0.0105(17) -0.0001(18) C28 0.043(3) 0.050(3) 0.030(2) 0.006(2) 0.0094(19) 0.004(2) C29 0.050(3) 0.058(3) 0.032(2) 0.007(2) 0.007(2) 0.010(2) C30 0.060(3) 0.057(3) 0.028(2) 0.009(2) 0.010(2) 0.004(2) C31 0.053(3) 0.049(3) 0.026(2) 0.005(2) 0.0137(19) 0.002(2) C32 0.020(6) 0.141(16) 0.066(9) 0.000(10) 0.004(5) -0.016(7) C33 0.127(16) 0.072(11) 0.091(12) 0.038(10) 0.016(11) 0.024(10) C34 0.046(8) 0.113(14) 0.143(19) 0.048(14) -0.001(10) -0.016(9) C35 0.096(6) 0.074(5) 0.117(7) 0.012(5) 0.071(6) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.928(4) . ? Cu1 N1 1.944(4) . ? Cu1 N3 1.955(3) . ? Cu1 N5 2.069(3) . ? Cu2 N6 1.936(3) . ? Cu2 O1 1.954(3) 4_565 ? Cu2 N7 1.992(4) . ? Cu2 O2 2.009(3) . ? Cu2 N2 2.478(4) 4_565 ? Cl1 O4 1.397(5) . ? Cl1 O5 1.402(5) . ? Cl1 O6 1.406(5) . ? Cl1 O3 1.446(5) . ? Cl2 O8 1.428(7) . ? Cl2 O7 1.429(5) . ? Cl2 O10 1.431(6) . ? Cl2 O9 1.455(8) . ? O1 C13 1.251(5) . ? O1 Cu2 1.954(3) 4_566 ? O2 C19 1.269(5) . ? O11 C32 0.87(2) . ? O12 C35 1.227(8) . ? N1 C1 1.350(6) . ? N1 C5 1.364(5) . ? N2 C6 1.288(6) . ? N2 N3 1.375(4) . ? N2 Cu2 2.478(4) 4_566 ? N3 C13 1.339(6) . ? N4 C14 1.324(5) . ? N4 C18 1.340(5) . ? N5 C19 1.334(5) . ? N5 N6 1.384(5) . ? N6 C20 1.285(6) . ? N7 C31 1.330(6) . ? N7 C27 1.362(5) . ? N8 C32 1.27(2) . ? N8 C33 1.36(2) . ? N8 C34 1.40(3) . ? N9 N10 1.09(2) . ? N9 C35 1.212(16) . ? N9 C36 1.48(3) . ? N9 C38 1.51(3) . ? N9 C39 1.60(3) . ? N10 C37 1.24(3) . ? N10 C36 1.28(3) . ? N10 C39 1.40(3) . ? N10 C35 1.63(2) . ? C1 C2 1.372(7) . ? C2 C3 1.376(7) . ? C3 C4 1.381(7) . ? C4 C5 1.389(6) . ? C5 C6 1.497(6) . ? C6 C7 1.505(6) . ? C7 C8 1.388(7) . ? C7 C12 1.394(7) . ? C8 C9 1.401(6) . ? C9 C10 1.372(9) . ? C10 C11 1.375(9) . ? C11 C12 1.388(7) . ? C13 C14 1.504(6) . ? C14 C15 1.368(6) . ? C15 C16 1.396(6) . ? C16 C17 1.397(7) . ? C17 C18 1.369(6) . ? C18 C19 1.492(6) . ? C20 C21 1.477(6) . ? C20 C27 1.479(6) . ? C21 C22 1.399(6) . ? C21 C26 1.402(6) . ? C22 C23 1.389(6) . ? C23 C24 1.375(8) . ? C24 C25 1.376(8) . ? C25 C26 1.396(6) . ? C27 C28 1.379(7) . ? C28 C29 1.387(7) . ? C29 C30 1.373(8) . ? C30 C31 1.403(8) . ? C36 C37 1.41(4) . ? C36 C39 1.99(4) . ? C38 C39 1.58(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 164.58(16) . . ? N4 Cu1 N3 80.99(14) . . ? N1 Cu1 N3 90.43(15) . . ? N4 Cu1 N5 77.90(14) . . ? N1 Cu1 N5 113.36(15) . . ? N3 Cu1 N5 153.99(16) . . ? N6 Cu2 O1 167.33(15) . 4_565 ? N6 Cu2 N7 80.17(15) . . ? O1 Cu2 N7 104.63(15) 4_565 . ? N6 Cu2 O2 79.92(14) . . ? O1 Cu2 O2 96.55(14) 4_565 . ? N7 Cu2 O2 158.45(14) . . ? N6 Cu2 N2 119.17(14) . 4_565 ? O1 Cu2 N2 73.21(12) 4_565 4_565 ? N7 Cu2 N2 85.80(14) . 4_565 ? O2 Cu2 N2 96.77(13) . 4_565 ? O4 Cl1 O5 110.8(4) . . ? O4 Cl1 O6 111.3(4) . . ? O5 Cl1 O6 112.2(4) . . ? O4 Cl1 O3 108.9(4) . . ? O5 Cl1 O3 106.8(3) . . ? O6 Cl1 O3 106.7(4) . . ? O8 Cl2 O7 111.5(4) . . ? O8 Cl2 O10 111.8(5) . . ? O7 Cl2 O10 110.8(4) . . ? O8 Cl2 O9 106.4(4) . . ? O7 Cl2 O9 109.9(4) . . ? O10 Cl2 O9 106.3(5) . . ? C13 O1 Cu2 120.4(3) . 4_566 ? C19 O2 Cu2 108.6(3) . . ? C1 N1 C5 119.2(4) . . ? C1 N1 Cu1 115.9(3) . . ? C5 N1 Cu1 124.4(3) . . ? C6 N2 N3 118.3(3) . . ? C6 N2 Cu2 136.3(3) . 4_566 ? N3 N2 Cu2 104.6(2) . 4_566 ? C13 N3 N2 113.8(3) . . ? C13 N3 Cu1 115.8(3) . . ? N2 N3 Cu1 128.0(3) . . ? C14 N4 C18 122.3(4) . . ? C14 N4 Cu1 117.3(3) . . ? C18 N4 Cu1 119.1(3) . . ? C19 N5 N6 108.2(3) . . ? C19 N5 Cu1 113.2(3) . . ? N6 N5 Cu1 137.5(3) . . ? C20 N6 N5 124.7(4) . . ? C20 N6 Cu2 119.4(3) . . ? N5 N6 Cu2 115.7(3) . . ? C31 N7 C27 119.5(4) . . ? C31 N7 Cu2 126.8(3) . . ? C27 N7 Cu2 113.1(3) . . ? C32 N8 C33 122.5(17) . . ? C32 N8 C34 120.3(16) . . ? C33 N8 C34 117.2(14) . . ? N10 N9 C35 89.8(16) . . ? N10 N9 C36 57.1(15) . . ? C35 N9 C36 116.0(17) . . ? N10 N9 C38 120(2) . . ? C35 N9 C38 124.1(17) . . ? C36 N9 C38 119.8(18) . . ? N10 N9 C39 59.2(15) . . ? C35 N9 C39 131.0(16) . . ? C36 N9 C39 80.1(16) . . ? C38 N9 C39 61.1(15) . . ? N9 N10 C37 136(2) . . ? N9 N10 C36 76.9(19) . . ? C37 N10 C36 68(2) . . ? N9 N10 C39 78.7(19) . . ? C37 N10 C39 129(2) . . ? C36 N10 C39 96(2) . . ? N9 N10 C35 48.0(12) . . ? C37 N10 C35 115(2) . . ? C36 N10 C35 103.2(18) . . ? C39 N10 C35 115.3(18) . . ? N1 C1 C2 122.4(4) . . ? C1 C2 C3 119.2(5) . . ? C2 C3 C4 119.1(5) . . ? C3 C4 C5 120.2(4) . . ? N1 C5 C4 119.9(4) . . ? N1 C5 C6 121.3(4) . . ? C4 C5 C6 118.7(4) . . ? N2 C6 C5 128.7(4) . . ? N2 C6 C7 113.9(4) . . ? C5 C6 C7 117.4(4) . . ? C8 C7 C12 118.8(4) . . ? C8 C7 C6 123.8(4) . . ? C12 C7 C6 117.4(4) . . ? C7 C8 C9 120.0(5) . . ? C10 C9 C8 120.3(5) . . ? C9 C10 C11 120.1(5) . . ? C10 C11 C12 120.1(6) . . ? C11 C12 C7 120.6(5) . . ? O1 C13 N3 127.7(4) . . ? O1 C13 C14 119.9(4) . . ? N3 C13 C14 112.4(4) . . ? N4 C14 C15 121.0(4) . . ? N4 C14 C13 111.7(4) . . ? C15 C14 C13 127.3(4) . . ? C14 C15 C16 117.6(5) . . ? C15 C16 C17 120.9(4) . . ? C18 C17 C16 117.6(4) . . ? N4 C18 C17 120.6(4) . . ? N4 C18 C19 111.3(4) . . ? C17 C18 C19 128.1(4) . . ? O2 C19 N5 126.2(4) . . ? O2 C19 C18 120.1(4) . . ? N5 C19 C18 113.7(3) . . ? N6 C20 C21 124.3(4) . . ? N6 C20 C27 112.4(4) . . ? C21 C20 C27 123.2(4) . . ? C22 C21 C26 119.9(4) . . ? C22 C21 C20 118.5(4) . . ? C26 C21 C20 121.5(4) . . ? C23 C22 C21 119.8(5) . . ? C24 C23 C22 119.8(5) . . ? C23 C24 C25 121.1(5) . . ? C24 C25 C26 120.3(5) . . ? C25 C26 C21 119.0(5) . . ? N7 C27 C28 121.3(4) . . ? N7 C27 C20 114.3(4) . . ? C28 C27 C20 124.2(4) . . ? C27 C28 C29 119.1(5) . . ? C30 C29 C28 119.7(5) . . ? C29 C30 C31 118.7(5) . . ? N7 C31 C30 121.7(5) . . ? O11 C32 N8 138(3) . . ? N9 C35 O12 137.6(12) . . ? N9 C35 N10 42.1(10) . . ? O12 C35 N10 110.9(10) . . ? N10 C36 C37 54.9(18) . . ? N10 C36 N9 46.0(14) . . ? C37 C36 N9 97(2) . . ? N10 C36 C39 44.7(14) . . ? C37 C36 C39 88(2) . . ? N9 C36 C39 52.7(13) . . ? N10 C37 C36 57.1(18) . . ? N9 C38 C39 62.3(15) . . ? N10 C39 C38 98(2) . . ? N10 C39 N9 42.0(12) . . ? C38 C39 N9 56.7(14) . . ? N10 C39 C36 39.8(13) . . ? C38 C39 C36 92.3(19) . . ? N9 C39 C36 47.2(12) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.062 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.125 #===END data_shelxl(5) _database_code_depnum_ccdc_archive 'CCDC 630954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H58 Cu5 N20 O30' _chemical_formula_weight 1905.00 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2559(15) _cell_length_b 10.671(2) _cell_length_c 21.686(4) _cell_angle_alpha 85.018(5) _cell_angle_beta 81.688(5) _cell_angle_gamma 82.852(5) _cell_volume 1871.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5962 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 31.2 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 967 _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8311 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15481 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7283 _reflns_number_gt 6831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 3.7.0' _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0580P)^2^+4.2295P] 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 7283 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.45440(5) 0.46161(3) 0.351361(17) 0.01833(11) Uani 1 1 d . . . Cu2 Cu 0.82337(5) 0.19839(3) 0.203457(17) 0.01729(11) Uani 1 1 d . . . Cu3 Cu 1.0000 0.0000 0.0000 0.02165(14) Uani 1 2 d S . . O1 O 0.9461(3) 0.1785(2) 0.01722(10) 0.0227(5) Uani 1 1 d . . . O2 O 0.5483(3) 0.5243(2) 0.26460(10) 0.0206(5) Uani 1 1 d . . . O3 O 0.7668(3) -0.0363(3) 0.02175(14) 0.0361(6) Uani 1 1 d . . . O4 O 0.3392(3) 0.6232(2) 0.37638(11) 0.0241(5) Uani 1 1 d . . . H24 H 0.2294 0.6342 0.3772 0.022 Uiso 1 1 d . . . H25 H 0.3387 0.6468 0.4120 0.022 Uiso 1 1 d . . . O5 O 0.6534(3) 0.5012(2) 0.40033(11) 0.0255(5) Uani 1 1 d . . . H22 H 0.7529 0.5180 0.3690 0.022 Uiso 1 1 d . . . H23 H 0.6957 0.4403 0.4323 0.022 Uiso 1 1 d . . . O6 O 1.0295(4) 0.3062(3) 0.22451(14) 0.0373(6) Uani 1 1 d . . . H29 H 1.0060 0.3641 0.2587 0.022 Uiso 1 1 d . . . O7 O 0.7624(4) 0.1814(3) 0.43793(13) 0.0431(7) Uani 1 1 d . . . O8 O 0.8035(3) 0.1497(2) 0.53470(12) 0.0302(6) Uani 1 1 d . . . O9 O 0.6846(4) 0.3300(2) 0.50126(12) 0.0402(7) Uani 1 1 d . . . O10 O 0.1813(3) 0.4728(3) 0.30115(14) 0.0440(8) Uani 1 1 d . . . O11 O 0.0274(4) 0.6106(3) 0.35890(16) 0.0497(8) Uani 1 1 d . . . O12 O -0.0834(4) 0.4921(4) 0.30454(16) 0.0560(9) Uani 1 1 d . . . O13 O 0.5083(5) 0.2396(5) 0.1025(2) 0.0948(17) Uani 1 1 d . . . O14 O 0.3071(6) 0.2385(5) 0.0520(2) 0.0924(16) Uani 1 1 d . . . O15 O 0.4586(17) 0.0972(13) 0.0390(7) 0.051(3) Uiso 0.25 1 d P . . O16 O 0.3547(19) 0.0805(14) 0.1010(7) 0.057(4) Uiso 0.25 1 d P . . O17 O 0.4745(9) 0.0684(7) 0.0793(4) 0.0588(18) Uiso 0.50 1 d P . . N1 N 0.9289(3) 0.0563(2) 0.25210(12) 0.0176(5) Uani 1 1 d . . . N2 N 0.9973(3) 0.0095(2) 0.11291(13) 0.0198(6) Uani 1 1 d . . . N3 N 0.9281(3) 0.1304(2) 0.12465(12) 0.0181(5) Uani 1 1 d . . . N4 N 0.7750(3) 0.3442(2) 0.14705(12) 0.0188(5) Uani 1 1 d . . . N5 N 0.6405(3) 0.3105(2) 0.25824(12) 0.0174(5) Uani 1 1 d . . . N6 N 0.5431(3) 0.3014(2) 0.31557(12) 0.0177(5) Uani 1 1 d . . . N7 N 0.3523(3) 0.3396(3) 0.41719(13) 0.0208(6) Uani 1 1 d . . . N8 N 0.7512(4) 0.2181(3) 0.49122(13) 0.0243(6) Uani 1 1 d . . . N9 N 0.0439(4) 0.5251(4) 0.32189(16) 0.0391(8) Uani 1 1 d . . . N10 N 0.4219(4) 0.1884(3) 0.07594(16) 0.0334(7) Uani 1 1 d . . . C1 C 0.9330(4) 0.0765(3) 0.31230(15) 0.0203(6) Uani 1 1 d . . . H9 H 0.8610 0.1445 0.3300 0.024 Uiso 1 1 calc R . . C2 C 1.0357(4) 0.0039(3) 0.34973(15) 0.0224(7) Uani 1 1 d . . . H8 H 1.0336 0.0211 0.3921 0.027 Uiso 1 1 calc R . . C3 C 1.1412(4) -0.0939(3) 0.32409(16) 0.0242(7) Uani 1 1 d . . . H7 H 1.2156 -0.1444 0.3482 0.029 Uiso 1 1 calc R . . C4 C 1.1370(4) -0.1177(3) 0.26225(16) 0.0226(7) Uani 1 1 d . . . H6 H 1.2074 -0.1862 0.2442 0.027 Uiso 1 1 calc R . . C5 C 1.0302(4) -0.0416(3) 0.22657(15) 0.0189(6) Uani 1 1 d . . . C6 C 1.1179(4) -0.1943(3) 0.14046(16) 0.0233(7) Uani 1 1 d . . . C7 C 1.0537(5) -0.3042(3) 0.16646(18) 0.0282(8) Uani 1 1 d . . . H5 H 0.9594 -0.2995 0.1973 0.034 Uiso 1 1 calc R . . C8 C 1.1284(5) -0.4214(4) 0.1471(2) 0.0364(9) Uani 1 1 d . . . H4 H 1.0825 -0.4966 0.1637 0.044 Uiso 1 1 calc R . . C9 C 1.2692(5) -0.4284(4) 0.10378(19) 0.0393(10) Uani 1 1 d . . . H3 H 1.3224 -0.5086 0.0919 0.047 Uiso 1 1 calc R . . C10 C 1.3322(5) -0.3196(4) 0.07787(18) 0.0359(9) Uani 1 1 d . . . H2 H 1.4268 -0.3247 0.0471 0.043 Uiso 1 1 calc R . . C11 C 1.2585(5) -0.2019(3) 0.09635(16) 0.0275(8) Uani 1 1 d . . . H1 H 1.3039 -0.1271 0.0789 0.033 Uiso 1 1 calc R . . C12 C 1.0388(4) -0.0671(3) 0.15926(15) 0.0203(6) Uani 1 1 d . . . C13 C 0.9104(4) 0.2061(3) 0.07294(14) 0.0182(6) Uani 1 1 d . . . C14 C 0.8369(4) 0.3370(3) 0.08730(14) 0.0180(6) Uani 1 1 d . . . C15 C 0.8293(4) 0.4430(3) 0.04574(15) 0.0214(7) Uani 1 1 d . . . H10 H 0.8724 0.4381 0.0029 0.026 Uiso 1 1 calc R . . C16 C 0.7563(4) 0.5573(3) 0.06907(16) 0.0259(7) Uani 1 1 d . . . H11 H 0.7524 0.6323 0.0421 0.031 Uiso 1 1 calc R . . C17 C 0.6890(4) 0.5625(3) 0.13154(16) 0.0228(7) Uani 1 1 d . . . H12 H 0.6372 0.6397 0.1476 0.027 Uiso 1 1 calc R . . C18 C 0.7000(4) 0.4515(3) 0.16946(14) 0.0187(6) Uani 1 1 d . . . C19 C 0.6250(4) 0.4327(3) 0.23607(14) 0.0184(6) Uani 1 1 d . . . C20 C 0.4986(4) 0.1966(3) 0.34307(14) 0.0182(6) Uani 1 1 d . . . C21 C 0.5422(4) 0.0688(3) 0.31889(15) 0.0202(6) Uani 1 1 d . . . C22 C 0.5265(4) 0.0510(3) 0.25691(16) 0.0248(7) Uani 1 1 d . . . H17 H 0.4908 0.1206 0.2298 0.030 Uiso 1 1 calc R . . C23 C 0.5636(5) -0.0696(4) 0.23538(19) 0.0333(8) Uani 1 1 d . . . H18 H 0.5524 -0.0824 0.1935 0.040 Uiso 1 1 calc R . . C24 C 0.6167(5) -0.1712(3) 0.2744(2) 0.0352(9) Uani 1 1 d . . . H19 H 0.6402 -0.2535 0.2595 0.042 Uiso 1 1 calc R . . C25 C 0.6356(5) -0.1530(3) 0.33514(19) 0.0314(8) Uani 1 1 d . . . H20 H 0.6742 -0.2226 0.3616 0.038 Uiso 1 1 calc R . . C26 C 0.5988(4) -0.0339(3) 0.35763(17) 0.0252(7) Uani 1 1 d . . . H21 H 0.6120 -0.0219 0.3994 0.030 Uiso 1 1 calc R . . C27 C 0.3854(4) 0.2168(3) 0.40229(15) 0.0195(6) Uani 1 1 d . . . C28 C 0.3125(4) 0.1215(3) 0.43920(16) 0.0238(7) Uani 1 1 d . . . H16 H 0.3350 0.0363 0.4280 0.029 Uiso 1 1 calc R . . C29 C 0.2055(5) 0.1517(3) 0.49311(17) 0.0287(8) Uani 1 1 d . . . H15 H 0.1536 0.0874 0.5188 0.034 Uiso 1 1 calc R . . C30 C 0.1758(5) 0.2757(4) 0.50887(17) 0.0304(8) Uani 1 1 d . . . H14 H 0.1051 0.2979 0.5458 0.036 Uiso 1 1 calc R . . C31 C 0.2511(4) 0.3671(3) 0.46963(16) 0.0260(7) Uani 1 1 d . . . H13 H 0.2304 0.4526 0.4803 0.031 Uiso 1 1 calc R . . C32 C 1.1905(5) 0.2524(4) 0.2206(2) 0.0426(10) Uani 1 1 d . . . H26 H 1.2233 0.2158 0.1801 0.051 Uiso 1 1 calc R . . H27 H 1.2013 0.1856 0.2543 0.051 Uiso 1 1 calc R . . H28 H 1.2617 0.3173 0.2247 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0254(2) 0.0143(2) 0.0147(2) -0.00451(14) -0.00127(15) 0.00118(15) Cu2 0.0253(2) 0.01385(19) 0.01186(19) -0.00272(14) -0.00212(15) 0.00199(15) Cu3 0.0247(3) 0.0220(3) 0.0187(3) -0.0104(2) -0.0042(2) 0.0032(2) O1 0.0323(13) 0.0220(12) 0.0132(11) -0.0049(9) -0.0041(9) 0.0030(10) O2 0.0281(12) 0.0162(11) 0.0165(11) -0.0041(9) -0.0029(9) 0.0029(9) O3 0.0267(13) 0.0389(15) 0.0446(16) -0.0168(13) -0.0057(12) -0.0006(11) O4 0.0325(13) 0.0192(11) 0.0198(12) -0.0072(9) -0.0041(10) 0.0040(10) O5 0.0292(12) 0.0250(12) 0.0234(12) -0.0023(10) -0.0075(10) -0.0023(10) O6 0.0422(16) 0.0324(14) 0.0415(16) -0.0048(12) -0.0157(13) -0.0075(12) O7 0.063(2) 0.0450(17) 0.0215(14) -0.0160(12) -0.0099(13) 0.0067(15) O8 0.0427(15) 0.0238(12) 0.0231(13) 0.0014(10) -0.0068(11) 0.0013(11) O9 0.069(2) 0.0239(13) 0.0248(14) -0.0076(11) -0.0113(13) 0.0171(13) O10 0.0278(14) 0.069(2) 0.0375(16) -0.0261(15) -0.0046(12) 0.0033(14) O11 0.0328(15) 0.067(2) 0.0520(19) -0.0340(17) -0.0041(14) 0.0009(15) O12 0.0300(15) 0.092(3) 0.052(2) -0.0330(19) -0.0023(14) -0.0154(16) O13 0.052(2) 0.142(4) 0.106(4) -0.075(3) -0.011(2) -0.026(3) O14 0.081(3) 0.100(4) 0.098(4) 0.041(3) -0.051(3) -0.005(3) N1 0.0226(13) 0.0171(13) 0.0131(12) -0.0036(10) -0.0019(10) -0.0010(10) N2 0.0223(13) 0.0176(13) 0.0196(14) -0.0057(10) -0.0041(11) 0.0024(11) N3 0.0228(13) 0.0153(13) 0.0160(13) -0.0046(10) -0.0019(10) 0.0012(10) N4 0.0241(13) 0.0169(13) 0.0153(13) -0.0049(10) -0.0027(10) 0.0004(11) N5 0.0229(13) 0.0159(13) 0.0123(12) -0.0030(10) 0.0004(10) 0.0008(10) N6 0.0217(13) 0.0175(13) 0.0145(12) -0.0043(10) -0.0044(10) -0.0001(10) N7 0.0261(14) 0.0192(13) 0.0175(13) -0.0061(10) -0.0016(11) -0.0025(11) N8 0.0301(15) 0.0248(15) 0.0182(14) -0.0065(11) -0.0039(11) -0.0002(12) N9 0.0301(17) 0.059(2) 0.0286(17) -0.0063(16) -0.0030(14) -0.0069(16) N10 0.0373(18) 0.0256(16) 0.0411(19) -0.0073(14) -0.0152(15) -0.0037(14) C1 0.0234(16) 0.0201(15) 0.0171(15) -0.0030(12) -0.0001(12) -0.0034(13) C2 0.0277(17) 0.0259(17) 0.0147(15) -0.0009(13) -0.0054(13) -0.0047(14) C3 0.0308(18) 0.0229(16) 0.0195(16) -0.0002(13) -0.0097(14) 0.0010(14) C4 0.0259(17) 0.0187(16) 0.0231(17) -0.0043(13) -0.0062(13) 0.0033(13) C5 0.0235(16) 0.0159(15) 0.0181(15) -0.0012(12) -0.0050(12) -0.0028(12) C6 0.0282(17) 0.0204(16) 0.0221(16) -0.0067(13) -0.0105(13) 0.0054(13) C7 0.0342(19) 0.0205(17) 0.0310(19) -0.0036(14) -0.0103(15) 0.0013(14) C8 0.050(2) 0.0204(18) 0.043(2) -0.0035(16) -0.0246(19) 0.0014(17) C9 0.054(3) 0.027(2) 0.038(2) -0.0160(17) -0.0245(19) 0.0225(18) C10 0.042(2) 0.037(2) 0.0247(19) -0.0105(16) -0.0102(16) 0.0229(18) C11 0.0361(19) 0.0265(18) 0.0183(16) -0.0027(13) -0.0083(14) 0.0091(15) C12 0.0214(15) 0.0190(16) 0.0212(16) -0.0055(12) -0.0046(12) -0.0005(12) C13 0.0205(15) 0.0194(15) 0.0150(15) -0.0056(12) -0.0025(12) -0.0003(12) C14 0.0200(15) 0.0194(15) 0.0159(15) -0.0033(12) -0.0048(12) -0.0029(12) C15 0.0269(16) 0.0224(16) 0.0149(15) -0.0014(12) -0.0024(12) -0.0037(13) C16 0.0365(19) 0.0205(16) 0.0191(16) 0.0019(13) -0.0028(14) -0.0004(14) C17 0.0307(17) 0.0164(15) 0.0204(16) -0.0029(12) -0.0031(13) 0.0017(13) C18 0.0214(15) 0.0196(15) 0.0155(15) -0.0039(12) -0.0040(12) -0.0002(12) C19 0.0230(15) 0.0171(15) 0.0157(15) -0.0042(12) -0.0045(12) -0.0001(12) C20 0.0214(15) 0.0186(15) 0.0152(15) -0.0026(12) -0.0055(12) 0.0000(12) C21 0.0236(16) 0.0152(15) 0.0213(16) -0.0053(12) 0.0009(12) -0.0022(12) C22 0.0288(17) 0.0215(17) 0.0253(17) -0.0069(13) -0.0048(14) -0.0030(14) C23 0.038(2) 0.030(2) 0.034(2) -0.0163(16) -0.0040(16) -0.0051(16) C24 0.041(2) 0.0161(17) 0.049(2) -0.0133(16) -0.0014(18) -0.0032(15) C25 0.035(2) 0.0156(16) 0.041(2) 0.0003(15) 0.0018(16) 0.0001(14) C26 0.0296(18) 0.0197(16) 0.0251(17) -0.0021(13) -0.0003(14) -0.0013(14) C27 0.0227(16) 0.0196(15) 0.0166(15) -0.0038(12) -0.0033(12) -0.0011(13) C28 0.0263(17) 0.0208(16) 0.0242(17) -0.0037(13) -0.0017(13) -0.0037(13) C29 0.0323(19) 0.0283(18) 0.0243(18) -0.0008(14) 0.0028(14) -0.0067(15) C30 0.0345(19) 0.034(2) 0.0221(17) -0.0090(15) 0.0063(15) -0.0074(16) C31 0.0326(18) 0.0251(17) 0.0193(16) -0.0089(13) 0.0036(14) -0.0020(14) C32 0.043(2) 0.033(2) 0.050(3) -0.0066(19) 0.003(2) -0.0062(18) _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 O4 1.944(2) . ? Cu1 N6 1.954(3) . ? Cu1 N7 2.012(3) . ? Cu1 O2 2.019(2) . ? Cu1 O5 2.182(2) . ? Cu2 N4 1.932(3) . ? Cu2 N3 1.956(3) . ? Cu2 N1 1.957(3) . ? Cu2 N5 2.098(3) . ? Cu2 O6 2.287(3) . ? Cu3 O1 1.957(2) 2_755 ? Cu3 O1 1.957(2) . ? Cu3 O3 1.993(3) 2_755 ? Cu3 O3 1.993(3) . ? Cu3 N2 2.456(3) 2_755 ? Cu3 N2 2.456(3) . ? O1 C13 1.254(4) . ? O2 C19 1.256(4) . ? O6 C32 1.375(5) . ? O7 N8 1.239(4) . ? O8 N8 1.236(4) . ? O9 N8 1.274(4) . ? O10 N9 1.240(4) . ? O11 N9 1.250(5) . ? O12 N9 1.264(4) . ? O13 N10 1.187(5) . ? O14 N10 1.192(5) . ? O15 O17 0.924(14) . ? O15 N10 1.294(14) . ? O15 O16 1.50(2) . ? O16 O17 1.030(15) . ? O16 N10 1.376(15) . ? O17 N10 1.299(8) . ? N1 C1 1.347(4) . ? N1 C5 1.359(4) . ? N2 C12 1.297(4) . ? N2 N3 1.374(4) . ? N3 C13 1.339(4) . ? N4 C14 1.327(4) . ? N4 C18 1.328(4) . ? N5 C19 1.348(4) . ? N5 N6 1.382(4) . ? N6 C20 1.290(4) . ? N7 C31 1.341(4) . ? N7 C27 1.362(4) . ? C1 C2 1.379(5) . ? C2 C3 1.376(5) . ? C3 C4 1.392(5) . ? C4 C5 1.395(4) . ? C5 C12 1.498(4) . ? C6 C7 1.388(5) . ? C6 C11 1.392(5) . ? C6 C12 1.494(4) . ? C7 C8 1.395(5) . ? C8 C9 1.383(6) . ? C9 C10 1.374(6) . ? C10 C11 1.391(5) . ? C13 C14 1.492(4) . ? C14 C15 1.385(4) . ? C15 C16 1.394(5) . ? C16 C17 1.391(5) . ? C17 C18 1.383(5) . ? C18 C19 1.494(4) . ? C20 C21 1.487(4) . ? C20 C27 1.490(4) . ? C21 C26 1.397(5) . ? C21 C22 1.400(5) . ? C22 C23 1.390(5) . ? C23 C24 1.384(6) . ? C24 C25 1.381(6) . ? C25 C26 1.384(5) . ? C27 C28 1.381(5) . ? C28 C29 1.395(5) . ? C29 C30 1.379(5) . ? C30 C31 1.384(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 O4 Cu1 N6 169.97(10) . . ? O4 Cu1 N7 101.88(11) . . ? N6 Cu1 N7 80.00(11) . . ? O4 Cu1 O2 96.55(9) . . ? N6 Cu1 O2 79.36(10) . . ? N7 Cu1 O2 156.39(10) . . ? O4 Cu1 O5 87.21(10) . . ? N6 Cu1 O5 102.36(10) . . ? N7 Cu1 O5 97.70(10) . . ? O2 Cu1 O5 97.81(9) . . ? N4 Cu2 N3 80.69(11) . . ? N4 Cu2 N1 165.75(11) . . ? N3 Cu2 N1 91.73(11) . . ? N4 Cu2 N5 77.31(11) . . ? N3 Cu2 N5 153.41(11) . . ? N1 Cu2 N5 112.77(10) . . ? N4 Cu2 O6 84.34(11) . . ? N3 Cu2 O6 99.48(11) . . ? N1 Cu2 O6 85.05(11) . . ? N5 Cu2 O6 93.05(11) . . ? O1 Cu3 O1 180.00(13) 2_755 . ? O1 Cu3 O3 93.07(11) 2_755 2_755 ? O1 Cu3 O3 86.93(11) . 2_755 ? O1 Cu3 O3 86.93(11) 2_755 . ? O1 Cu3 O3 93.07(11) . . ? O3 Cu3 O3 180.0 2_755 . ? O1 Cu3 N2 73.62(9) 2_755 2_755 ? O1 Cu3 N2 106.38(9) . 2_755 ? O3 Cu3 N2 85.62(10) 2_755 2_755 ? O3 Cu3 N2 94.38(10) . 2_755 ? O1 Cu3 N2 106.38(9) 2_755 . ? O1 Cu3 N2 73.62(9) . . ? O3 Cu3 N2 94.38(10) 2_755 . ? O3 Cu3 N2 85.62(10) . . ? N2 Cu3 N2 180.0 2_755 . ? C13 O1 Cu3 118.6(2) . . ? C19 O2 Cu1 109.4(2) . . ? C32 O6 Cu2 122.0(2) . . ? O17 O15 N10 69.4(11) . . ? O17 O15 O16 42.7(9) . . ? N10 O15 O16 58.5(8) . . ? O17 O16 N10 63.5(9) . . ? O17 O16 O15 37.5(8) . . ? N10 O16 O15 53.3(8) . . ? O15 O17 O16 99.8(14) . . ? O15 O17 N10 68.8(10) . . ? O16 O17 N10 71.3(10) . . ? C1 N1 C5 118.5(3) . . ? C1 N1 Cu2 115.0(2) . . ? C5 N1 Cu2 124.2(2) . . ? C12 N2 N3 118.8(3) . . ? C12 N2 Cu3 137.0(2) . . ? N3 N2 Cu3 104.23(18) . . ? C13 N3 N2 113.7(3) . . ? C13 N3 Cu2 116.0(2) . . ? N2 N3 Cu2 129.5(2) . . ? C14 N4 C18 122.1(3) . . ? C14 N4 Cu2 117.4(2) . . ? C18 N4 Cu2 120.0(2) . . ? C19 N5 N6 107.9(2) . . ? C19 N5 Cu2 112.6(2) . . ? N6 N5 Cu2 138.8(2) . . ? C20 N6 N5 124.1(3) . . ? C20 N6 Cu1 119.6(2) . . ? N5 N6 Cu1 115.95(19) . . ? C31 N7 C27 119.1(3) . . ? C31 N7 Cu1 127.6(2) . . ? C27 N7 Cu1 113.1(2) . . ? O8 N8 O7 122.0(3) . . ? O8 N8 O9 119.1(3) . . ? O7 N8 O9 118.8(3) . . ? O10 N9 O11 122.0(3) . . ? O10 N9 O12 119.2(4) . . ? O11 N9 O12 118.9(3) . . ? O13 N10 O14 125.9(5) . . ? O13 N10 O15 130.1(7) . . ? O14 N10 O15 96.1(7) . . ? O13 N10 O17 106.9(5) . . ? O14 N10 O17 127.2(5) . . ? O15 N10 O17 41.8(6) . . ? O13 N10 O16 122.3(7) . . ? O14 N10 O16 98.0(7) . . ? O15 N10 O16 68.1(9) . . ? O17 N10 O16 45.2(6) . . ? N1 C1 C2 123.8(3) . . ? C3 C2 C1 118.3(3) . . ? C2 C3 C4 118.9(3) . . ? C3 C4 C5 120.4(3) . . ? N1 C5 C4 120.1(3) . . ? N1 C5 C12 121.9(3) . . ? C4 C5 C12 117.9(3) . . ? C7 C6 C11 119.8(3) . . ? C7 C6 C12 121.0(3) . . ? C11 C6 C12 119.2(3) . . ? C6 C7 C8 119.7(4) . . ? C9 C8 C7 120.1(4) . . ? C10 C9 C8 120.1(3) . . ? C9 C10 C11 120.4(4) . . ? C10 C11 C6 119.8(4) . . ? N2 C12 C6 113.9(3) . . ? N2 C12 C5 128.9(3) . . ? C6 C12 C5 117.0(3) . . ? O1 C13 N3 127.8(3) . . ? O1 C13 C14 119.8(3) . . ? N3 C13 C14 112.4(3) . . ? N4 C14 C15 120.9(3) . . ? N4 C14 C13 112.2(3) . . ? C15 C14 C13 126.8(3) . . ? C14 C15 C16 117.6(3) . . ? C17 C16 C15 120.6(3) . . ? C18 C17 C16 117.8(3) . . ? N4 C18 C17 120.9(3) . . ? N4 C18 C19 112.1(3) . . ? C17 C18 C19 126.9(3) . . ? O2 C19 N5 126.3(3) . . ? O2 C19 C18 120.6(3) . . ? N5 C19 C18 113.0(3) . . ? N6 C20 C21 126.1(3) . . ? N6 C20 C27 112.2(3) . . ? C21 C20 C27 121.6(3) . . ? C26 C21 C22 119.6(3) . . ? C26 C21 C20 120.4(3) . . ? C22 C21 C20 119.9(3) . . ? C23 C22 C21 119.3(3) . . ? C24 C23 C22 120.6(4) . . ? C25 C24 C23 120.0(3) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 120.0(3) . . ? N7 C27 C28 121.0(3) . . ? N7 C27 C20 114.8(3) . . ? C28 C27 C20 124.1(3) . . ? C27 C28 C29 119.3(3) . . ? C30 C29 C28 119.5(3) . . ? C29 C30 C31 118.5(3) . . ? N7 C31 C30 122.6(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.449 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.099