Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal SOciety of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_section_title ;Supramolecular frameworks assembled via intermolecular lone pair-aromatic interaction between carbonyl and pyridyl groups ; _publ_contact_author_name 'Prof. Thomas Mak' _publ_contact_author_email TCWMAK@CUHK.EDU.HK loop_ _publ_author_name 'Thomas C. W. Mak' 'Xu-Dong Chen.' 'Chong-Qing Wan.' # Attachment 'cqw2-cif.txt' data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 663086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H22 B2 Cu F8 N6 O4' _chemical_formula_weight 815.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2844(11) _cell_length_b 17.7865(18) _cell_length_c 9.3905(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.380(2) _cell_angle_gamma 90.00 _cell_volume 1712.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776600 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11867 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0914 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4263 _reflns_number_gt 2469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4263 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.0000 0.5000 0.02588(18) Uani 1 2 d S . . C1 C 0.6933(4) 0.0315(2) 0.2874(4) 0.0362(9) Uani 1 1 d . . . H1A H 0.6256 0.0167 0.2221 0.043 Uiso 1 1 calc R . . C2 C 0.8076(4) 0.0558(2) 0.2373(4) 0.0459(10) Uani 1 1 d . . . H2A H 0.8178 0.0557 0.1398 0.055 Uiso 1 1 calc R . . C3 C 0.9082(4) 0.0806(2) 0.3327(4) 0.0404(9) Uani 1 1 d . . . H3A H 0.9859 0.0979 0.3001 0.049 Uiso 1 1 calc R . . C4 C 0.8906(3) 0.07912(18) 0.4761(4) 0.0299(8) Uani 1 1 d . . . C5 C 0.7750(3) 0.05041(18) 0.5195(4) 0.0283(7) Uani 1 1 d . . . H5A H 0.7657 0.0462 0.6169 0.034 Uiso 1 1 calc R . . N1 N 0.6757(3) 0.02838(15) 0.4282(3) 0.0267(6) Uani 1 1 d . . . C6 C 0.9951(3) 0.10760(19) 0.5814(4) 0.0333(8) Uani 1 1 d . . . O1 O 1.1090(3) 0.10721(17) 0.5553(3) 0.0545(8) Uani 1 1 d . . . C7 C 0.9569(3) 0.13934(19) 0.7213(4) 0.0314(8) Uani 1 1 d . . . C8 C 1.0453(4) 0.1435(2) 0.8396(5) 0.0471(11) Uani 1 1 d . . . H8A H 1.1290 0.1240 0.8363 0.057 Uiso 1 1 calc R . . C9 C 1.0078(4) 0.1768(3) 0.9624(5) 0.0564(13) Uani 1 1 d . . . H9A H 1.0651 0.1794 1.0438 0.068 Uiso 1 1 calc R . . C10 C 0.8841(4) 0.2063(2) 0.9627(4) 0.0465(10) Uani 1 1 d . . . H10A H 0.8566 0.2300 1.0433 0.056 Uiso 1 1 calc R . . C11 C 0.8014(3) 0.19969(18) 0.8393(4) 0.0299(8) Uani 1 1 d . . . N2 N 0.8365(3) 0.16672(15) 0.7212(3) 0.0274(6) Uani 1 1 d . . . C12 C 0.6684(4) 0.2364(2) 0.8308(4) 0.0343(8) Uani 1 1 d . . . O2 O 0.6504(3) 0.29102(16) 0.9022(3) 0.0566(8) Uani 1 1 d . . . C13 C 0.5623(3) 0.13144(18) 0.6844(4) 0.0288(8) Uani 1 1 d . . . H13A H 0.6224 0.0986 0.7299 0.035 Uiso 1 1 calc R . . C14 C 0.5645(3) 0.20642(19) 0.7265(4) 0.0318(8) Uani 1 1 d . . . C15 C 0.4696(4) 0.2539(2) 0.6652(5) 0.0441(10) Uani 1 1 d . . . H15A H 0.4667 0.3042 0.6923 0.053 Uiso 1 1 calc R . . C16 C 0.3792(4) 0.2254(2) 0.5633(5) 0.0453(10) Uani 1 1 d . . . H16A H 0.3129 0.2559 0.5228 0.054 Uiso 1 1 calc R . . C17 C 0.3880(3) 0.1511(2) 0.5216(4) 0.0363(9) Uani 1 1 d . . . H17A H 0.3293 0.1330 0.4494 0.044 Uiso 1 1 calc R . . N3 N 0.4784(3) 0.10426(15) 0.5820(3) 0.0270(6) Uani 1 1 d . . . B B 0.7046(5) -0.0537(3) 0.8528(5) 0.0501(13) Uani 1 1 d . . . F1 F 0.6083(2) -0.04141(12) 0.7423(2) 0.0499(6) Uani 1 1 d . . . F2 F 0.7753(4) 0.00851(18) 0.8752(3) 0.1121(15) Uani 1 1 d . . . F3 F 0.7800(3) -0.1125(2) 0.8045(4) 0.1100(13) Uani 1 1 d . . . F4 F 0.6568(4) -0.0802(2) 0.9711(3) 0.1045(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0218(3) 0.0235(3) 0.0324(3) -0.0053(3) 0.0024(2) -0.0037(2) C1 0.039(2) 0.038(2) 0.032(2) -0.0059(17) 0.0028(16) -0.0042(17) C2 0.044(2) 0.062(3) 0.032(2) -0.0036(19) 0.0100(17) -0.012(2) C3 0.033(2) 0.046(2) 0.044(2) -0.0020(19) 0.0126(17) -0.0076(18) C4 0.0245(18) 0.0268(17) 0.039(2) -0.0037(16) 0.0032(15) -0.0002(14) C5 0.0258(18) 0.0291(18) 0.0301(18) -0.0037(15) 0.0038(14) -0.0006(14) N1 0.0238(15) 0.0224(13) 0.0345(16) -0.0032(12) 0.0066(12) -0.0021(11) C6 0.0238(19) 0.0301(18) 0.046(2) -0.0056(16) 0.0001(16) -0.0004(14) O1 0.0264(15) 0.068(2) 0.070(2) -0.0181(16) 0.0087(14) -0.0065(13) C7 0.0257(18) 0.0295(18) 0.038(2) -0.0012(16) -0.0027(15) -0.0006(14) C8 0.034(2) 0.048(2) 0.057(3) -0.004(2) -0.015(2) 0.0040(18) C9 0.057(3) 0.066(3) 0.042(3) -0.009(2) -0.024(2) 0.006(2) C10 0.053(3) 0.052(3) 0.033(2) -0.0124(19) -0.0033(19) 0.001(2) C11 0.0310(19) 0.0270(18) 0.0316(19) -0.0040(15) 0.0025(15) -0.0026(14) N2 0.0274(15) 0.0238(14) 0.0305(16) -0.0014(12) -0.0003(12) -0.0014(11) C12 0.038(2) 0.0307(19) 0.035(2) -0.0081(16) 0.0078(16) -0.0049(16) O2 0.0462(18) 0.0539(18) 0.070(2) -0.0391(16) 0.0069(15) 0.0010(14) C13 0.0277(18) 0.0282(18) 0.0307(19) -0.0037(15) 0.0042(14) -0.0011(14) C14 0.0285(18) 0.0284(18) 0.039(2) -0.0076(15) 0.0057(15) -0.0004(14) C15 0.036(2) 0.031(2) 0.065(3) -0.0128(19) 0.0018(19) 0.0092(16) C16 0.030(2) 0.037(2) 0.068(3) -0.011(2) -0.0075(19) 0.0114(17) C17 0.0227(18) 0.037(2) 0.049(2) -0.0061(17) 0.0002(16) 0.0012(15) N3 0.0201(14) 0.0256(14) 0.0355(16) -0.0049(12) 0.0038(12) -0.0045(11) B 0.055(3) 0.050(3) 0.043(3) 0.008(2) -0.008(2) -0.008(2) F1 0.0465(14) 0.0496(14) 0.0510(14) 0.0021(12) -0.0133(11) 0.0025(11) F2 0.149(3) 0.092(2) 0.084(2) 0.0351(18) -0.064(2) -0.075(2) F3 0.087(3) 0.131(3) 0.107(3) -0.005(2) -0.026(2) 0.045(2) F4 0.140(3) 0.121(3) 0.0531(18) 0.0206(19) 0.0073(19) -0.042(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.027(3) 3_656 ? Cu1 N3 2.027(3) . ? Cu1 N1 2.040(3) . ? Cu1 N1 2.040(3) 3_656 ? C1 N1 1.350(4) . ? C1 C2 1.368(5) . ? C1 H1A 0.9300 . ? C2 C3 1.387(5) . ? C2 H2A 0.9300 . ? C3 C4 1.373(5) . ? C3 H3A 0.9300 . ? C4 C5 1.384(5) . ? C4 C6 1.492(4) . ? C5 N1 1.341(4) . ? C5 H5A 0.9300 . ? C6 O1 1.215(4) . ? C6 C7 1.509(5) . ? C7 N2 1.331(4) . ? C7 C8 1.383(5) . ? C8 C9 1.378(6) . ? C8 H8A 0.9300 . ? C9 C10 1.376(6) . ? C9 H9A 0.9300 . ? C10 C11 1.389(5) . ? C10 H10A 0.9300 . ? C11 N2 1.328(4) . ? C11 C12 1.513(5) . ? C12 O2 1.202(4) . ? C12 C14 1.491(5) . ? C13 N3 1.333(4) . ? C13 C14 1.391(4) . ? C13 H13A 0.9300 . ? C14 C15 1.383(5) . ? C15 C16 1.379(5) . ? C15 H15A 0.9300 . ? C16 C17 1.383(5) . ? C16 H16A 0.9300 . ? C17 N3 1.342(4) . ? C17 H17A 0.9300 . ? B F2 1.333(5) . ? B F4 1.335(6) . ? B F1 1.396(5) . ? B F3 1.397(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N3 180.0 3_656 . ? N3 Cu1 N1 88.59(11) 3_656 . ? N3 Cu1 N1 91.41(11) . . ? N3 Cu1 N1 91.41(11) 3_656 3_656 ? N3 Cu1 N1 88.59(11) . 3_656 ? N1 Cu1 N1 180.00(15) . 3_656 ? N1 C1 C2 122.2(3) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C1 C2 C3 119.8(4) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C4 C3 C2 118.7(4) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C3 C4 C5 118.4(3) . . ? C3 C4 C6 120.1(3) . . ? C5 C4 C6 121.5(3) . . ? N1 C5 C4 123.3(3) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? C5 N1 C1 117.5(3) . . ? C5 N1 Cu1 120.8(2) . . ? C1 N1 Cu1 121.5(2) . . ? O1 C6 C4 121.4(4) . . ? O1 C6 C7 119.8(3) . . ? C4 C6 C7 118.8(3) . . ? N2 C7 C8 122.5(4) . . ? N2 C7 C6 116.1(3) . . ? C8 C7 C6 121.3(3) . . ? C9 C8 C7 119.1(4) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C9 C10 C11 118.2(4) . . ? C9 C10 H10A 120.9 . . ? C11 C10 H10A 120.9 . . ? N2 C11 C10 123.1(3) . . ? N2 C11 C12 116.6(3) . . ? C10 C11 C12 120.1(3) . . ? C11 N2 C7 118.2(3) . . ? O2 C12 C14 121.5(3) . . ? O2 C12 C11 119.7(3) . . ? C14 C12 C11 118.7(3) . . ? N3 C13 C14 123.3(3) . . ? N3 C13 H13A 118.4 . . ? C14 C13 H13A 118.4 . . ? C15 C14 C13 118.1(3) . . ? C15 C14 C12 120.1(3) . . ? C13 C14 C12 121.7(3) . . ? C16 C15 C14 118.8(3) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C15 C16 C17 119.5(3) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? N3 C17 C16 122.1(3) . . ? N3 C17 H17A 118.9 . . ? C16 C17 H17A 118.9 . . ? C13 N3 C17 118.0(3) . . ? C13 N3 Cu1 121.5(2) . . ? C17 N3 Cu1 120.0(2) . . ? F2 B F4 113.1(4) . . ? F2 B F1 109.6(4) . . ? F4 B F1 112.9(4) . . ? F2 B F3 111.3(5) . . ? F4 B F3 104.8(4) . . ? F1 B F3 104.9(4) . . ? 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 N1 C1 C2 C3 -2.2(6) . . . . ? C1 C2 C3 C4 0.8(6) . . . . ? C2 C3 C4 C5 2.3(5) . . . . ? C2 C3 C4 C6 -178.1(3) . . . . ? C3 C4 C5 N1 -4.4(5) . . . . ? C6 C4 C5 N1 175.9(3) . . . . ? C4 C5 N1 C1 3.1(5) . . . . ? C4 C5 N1 Cu1 -171.7(2) . . . . ? C2 C1 N1 C5 0.3(5) . . . . ? C2 C1 N1 Cu1 175.1(3) . . . . ? N3 Cu1 N1 C5 -119.5(2) 3_656 . . . ? N3 Cu1 N1 C5 60.5(2) . . . . ? N1 Cu1 N1 C5 -148(100) 3_656 . . . ? N3 Cu1 N1 C1 65.9(3) 3_656 . . . ? N3 Cu1 N1 C1 -114.1(3) . . . . ? N1 Cu1 N1 C1 37(100) 3_656 . . . ? C3 C4 C6 O1 -26.6(5) . . . . ? C5 C4 C6 O1 153.0(4) . . . . ? C3 C4 C6 C7 151.7(3) . . . . ? C5 C4 C6 C7 -28.6(5) . . . . ? O1 C6 C7 N2 153.1(3) . . . . ? C4 C6 C7 N2 -25.3(5) . . . . ? O1 C6 C7 C8 -23.2(6) . . . . ? C4 C6 C7 C8 158.4(3) . . . . ? N2 C7 C8 C9 0.3(6) . . . . ? C6 C7 C8 C9 176.3(4) . . . . ? C7 C8 C9 C10 -1.2(7) . . . . ? C8 C9 C10 C11 1.3(6) . . . . ? C9 C10 C11 N2 -0.4(6) . . . . ? C9 C10 C11 C12 -175.3(4) . . . . ? C10 C11 N2 C7 -0.5(5) . . . . ? C12 C11 N2 C7 174.5(3) . . . . ? C8 C7 N2 C11 0.6(5) . . . . ? C6 C7 N2 C11 -175.6(3) . . . . ? N2 C11 C12 O2 -148.6(4) . . . . ? C10 C11 C12 O2 26.6(5) . . . . ? N2 C11 C12 C14 27.6(5) . . . . ? C10 C11 C12 C14 -157.2(3) . . . . ? N3 C13 C14 C15 4.2(6) . . . . ? N3 C13 C14 C12 -173.6(3) . . . . ? O2 C12 C14 C15 26.9(6) . . . . ? C11 C12 C14 C15 -149.2(4) . . . . ? O2 C12 C14 C13 -155.3(4) . . . . ? C11 C12 C14 C13 28.6(5) . . . . ? C13 C14 C15 C16 -1.5(6) . . . . ? C12 C14 C15 C16 176.4(4) . . . . ? C14 C15 C16 C17 -2.0(7) . . . . ? C15 C16 C17 N3 3.2(6) . . . . ? C14 C13 N3 C17 -3.2(5) . . . . ? C14 C13 N3 Cu1 168.7(3) . . . . ? C16 C17 N3 C13 -0.6(6) . . . . ? C16 C17 N3 Cu1 -172.5(3) . . . . ? N3 Cu1 N3 C13 -150(100) 3_656 . . . ? N1 Cu1 N3 C13 -61.6(3) . . . . ? N1 Cu1 N3 C13 118.4(3) 3_656 . . . ? N3 Cu1 N3 C17 22(100) 3_656 . . . ? N1 Cu1 N3 C17 110.1(3) . . . . ? N1 Cu1 N3 C17 -69.9(3) 3_656 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.605 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.082 #===End data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 663087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H27 Cu N9 O11' _chemical_formula_weight 825.19 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' 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 9.154(5) _cell_length_b 21.374(11) _cell_length_c 18.717(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.286(11) _cell_angle_gamma 90.00 _cell_volume 3662(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1684 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.732525 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25386 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.43 _reflns_number_total 9108 _reflns_number_gt 5394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.1248P)^2^+1.9743P] 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 9108 _refine_ls_number_parameters 530 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.2226 _refine_ls_wR_factor_gt 0.1782 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.5000 0.0000 0.03923(18) Uani 1 2 d S . . Cu2 Cu 0.5000 0.5000 0.5000 0.04364(19) Uani 1 2 d S . . N1 N 0.5542(3) 0.54257(13) 0.09606(15) 0.0396(6) Uani 1 1 d . . . N3 N 0.2909(3) 0.49215(12) 0.03446(16) 0.0369(6) Uani 1 1 d . . . N2 N 0.2223(3) 0.64993(13) 0.14507(15) 0.0408(6) Uani 1 1 d . . . N4 N 0.5453(3) 0.59067(14) 0.47421(16) 0.0452(7) Uani 1 1 d . . . N6 N 0.4007(3) 0.48470(14) 0.40237(16) 0.0434(7) Uani 1 1 d . . . N5 N 0.2222(3) 0.64451(14) 0.34145(17) 0.0489(7) Uani 1 1 d . . . N7 N 0.3632(4) 0.64281(16) -0.0683(2) 0.0603(9) Uani 1 1 d . . . N8 N 0.1619(8) 0.5273(4) 0.5818(3) 0.119(2) Uani 1 1 d . . . N9 N 0.3027(7) 0.6625(4) -0.3076(5) 0.156(3) Uani 1 1 d . . . O1 O 0.5011(3) 0.72176(15) 0.24188(17) 0.0711(9) Uani 1 1 d . . . O2 O -0.1311(2) 0.60608(13) 0.09685(15) 0.0534(7) Uani 1 1 d . . . O3 O 0.3665(4) 0.78715(14) 0.4027(2) 0.0960(13) Uani 1 1 d . . . O4 O 0.0202(3) 0.53581(16) 0.24098(15) 0.0624(8) Uani 1 1 d . . . O5 O 0.3308(6) 0.6821(2) -0.0220(3) 0.1250(18) Uani 1 1 d . . . O6 O 0.2918(9) 0.6428(3) -0.1194(4) 0.199(4) Uani 1 1 d . . . O7 O 0.4582(3) 0.60491(13) -0.05453(17) 0.0596(7) Uani 1 1 d . . . O8 O 0.1908(13) 0.4864(4) 0.6297(4) 0.225(5) Uani 1 1 d . . . O9 O 0.0455(7) 0.5517(6) 0.5805(5) 0.237(6) Uani 1 1 d . . . O10 O 0.2598(3) 0.53863(16) 0.54211(17) 0.0683(8) Uani 1 1 d . . . C1 C 0.5063(3) 0.59944(16) 0.11323(19) 0.0406(7) Uani 1 1 d . . . H1A H 0.4625 0.6234 0.0776 0.049 Uiso 1 1 calc R . . C2 C 0.5178(4) 0.62505(17) 0.18116(19) 0.0432(8) Uani 1 1 d . . . C3 C 0.5956(4) 0.5919(2) 0.2322(2) 0.0511(9) Uani 1 1 d . . . H3A H 0.6093 0.6082 0.2778 0.061 Uiso 1 1 calc R . . C4 C 0.6521(4) 0.5345(2) 0.2142(2) 0.0551(10) Uani 1 1 d . . . H4A H 0.7074 0.5119 0.2471 0.066 Uiso 1 1 calc R . . C5 C 0.6263(4) 0.51081(18) 0.1476(2) 0.0467(9) Uani 1 1 d . . . H5A H 0.6601 0.4708 0.1373 0.056 Uiso 1 1 calc R . . C6 C 0.4466(4) 0.68556(17) 0.1994(2) 0.0500(9) Uani 1 1 d . . . C7 C 0.3005(4) 0.69927(16) 0.1664(2) 0.0460(8) Uani 1 1 d . . . C8 C 0.2493(5) 0.76040(19) 0.1594(3) 0.0682(12) Uani 1 1 d . . . H8A H 0.3063 0.7942 0.1739 0.082 Uiso 1 1 calc R . . C9 C 0.1112(6) 0.7697(2) 0.1303(3) 0.0764(14) Uani 1 1 d . . . H9A H 0.0743 0.8100 0.1249 0.092 Uiso 1 1 calc R . . C10 C 0.0298(5) 0.71918(18) 0.1096(3) 0.0596(11) Uani 1 1 d . . . H10A H -0.0635 0.7246 0.0907 0.072 Uiso 1 1 calc R . . C11 C 0.0883(4) 0.65993(16) 0.11745(19) 0.0415(8) Uani 1 1 d . . . C12 C 0.0016(3) 0.60338(15) 0.09795(18) 0.0382(7) Uani 1 1 d . . . C13 C 0.0793(3) 0.54402(15) 0.08059(17) 0.0347(7) Uani 1 1 d . . . C14 C 0.2158(3) 0.54406(15) 0.05000(17) 0.0361(7) Uani 1 1 d . . . H14A H 0.2583 0.5825 0.0395 0.043 Uiso 1 1 calc R . . C15 C 0.2279(3) 0.43745(16) 0.04863(19) 0.0400(7) Uani 1 1 d . . . H15A H 0.2789 0.4009 0.0385 0.048 Uiso 1 1 calc R . . C16 C 0.0905(4) 0.43265(16) 0.07754(19) 0.0417(7) Uani 1 1 d . . . H16A H 0.0492 0.3936 0.0858 0.050 Uiso 1 1 calc R . . C17 C 0.0146(3) 0.48661(16) 0.09425(19) 0.0392(7) Uani 1 1 d . . . H17A H -0.0781 0.4844 0.1143 0.047 Uiso 1 1 calc R . . C18 C 0.6855(4) 0.61029(19) 0.4720(2) 0.0547(10) Uani 1 1 d . . . H18A H 0.7593 0.5833 0.4868 0.066 Uiso 1 1 calc R . . C19 C 0.7220(5) 0.6693(2) 0.4481(3) 0.0649(12) Uani 1 1 d . . . H19A H 0.8187 0.6825 0.4494 0.078 Uiso 1 1 calc R . . C20 C 0.6152(5) 0.70829(19) 0.4226(2) 0.0602(11) Uani 1 1 d . . . H20A H 0.6392 0.7476 0.4048 0.072 Uiso 1 1 calc R . . C21 C 0.4710(4) 0.68870(16) 0.4236(2) 0.0495(9) Uani 1 1 d . . . C22 C 0.4413(4) 0.63005(16) 0.4519(2) 0.0469(8) Uani 1 1 d . . . H22A H 0.3443 0.6176 0.4556 0.056 Uiso 1 1 calc R . . C23 C 0.3530(5) 0.73050(18) 0.3964(2) 0.0618(11) Uani 1 1 d . . . C24 C 0.4638(4) 0.44478(18) 0.3563(2) 0.0505(9) Uani 1 1 d . . . H24A H 0.5459 0.4224 0.3709 0.061 Uiso 1 1 calc R . . C25 C 0.4099(5) 0.4361(2) 0.2879(2) 0.0571(10) Uani 1 1 d . . . H25A H 0.4522 0.4065 0.2579 0.069 Uiso 1 1 calc R . . C26 C 0.2933(5) 0.47133(19) 0.2643(2) 0.0528(9) Uani 1 1 d . . . H26A H 0.2577 0.4667 0.2180 0.063 Uiso 1 1 calc R . . C27 C 0.2300(4) 0.51365(17) 0.31048(19) 0.0451(8) Uani 1 1 d . . . C28 C 0.2833(4) 0.51721(17) 0.38009(19) 0.0435(8) Uani 1 1 d . . . H28A H 0.2358 0.5431 0.4125 0.052 Uiso 1 1 calc R . . C29 C 0.1089(4) 0.55464(19) 0.2844(2) 0.0491(9) Uani 1 1 d . . . C30 C 0.1033(4) 0.62161(19) 0.3093(2) 0.0514(9) Uani 1 1 d . . . C31 C -0.0201(5) 0.6576(2) 0.2928(2) 0.0668(12) Uani 1 1 d . . . H31A H -0.0999 0.6400 0.2694 0.080 Uiso 1 1 calc R . . C32 C -0.0203(6) 0.7193(3) 0.3121(3) 0.0758(14) Uani 1 1 d . . . H32A H -0.1011 0.7444 0.3026 0.091 Uiso 1 1 calc R . . C33 C 0.1018(6) 0.7438(2) 0.3459(3) 0.0730(13) Uani 1 1 d . . . H33A H 0.1045 0.7858 0.3589 0.088 Uiso 1 1 calc R . . C34 C 0.2203(5) 0.70509(19) 0.3604(2) 0.0566(10) Uani 1 1 d . . . C35 C 0.1978(7) 0.6451(3) -0.2816(3) 0.0905(16) Uani 1 1 d . . . C36 C 0.0692(7) 0.6238(3) -0.2527(4) 0.0982(18) Uiso 1 1 d . . . H36A H 0.0764 0.6243 -0.2016 0.147 Uiso 1 1 calc R . . H36B H 0.0512 0.5818 -0.2687 0.147 Uiso 1 1 calc R . . H36C H -0.0098 0.6504 -0.2678 0.147 Uiso 1 1 calc R . . O1W O 0.199(2) 0.6943(7) 0.5309(11) 0.105(6) Uani 0.25 1 d P . . O1W' O 0.0812(13) 0.6679(9) 0.5036(7) 0.197(8) Uani 0.50 1 d P . . O1W" O 0.1028(16) 0.7310(9) 0.5490(7) 0.096(6) Uani 0.25 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 0.0267(3) 0.0442(3) 0.0469(4) -0.0149(3) 0.0064(2) 0.0001(2) Cu2 0.0581(4) 0.0359(3) 0.0369(3) 0.0033(2) -0.0075(3) -0.0125(3) N1 0.0284(12) 0.0445(15) 0.0460(16) -0.0086(13) 0.0060(11) -0.0018(11) N3 0.0283(12) 0.0408(15) 0.0415(15) -0.0100(12) 0.0029(11) 0.0004(10) N2 0.0418(15) 0.0365(14) 0.0441(16) -0.0104(12) 0.0074(12) 0.0018(12) N4 0.0551(17) 0.0409(15) 0.0396(16) 0.0012(13) -0.0022(13) -0.0150(14) N6 0.0544(18) 0.0404(15) 0.0354(15) 0.0010(12) -0.0040(13) -0.0134(13) N5 0.0539(18) 0.0469(17) 0.0459(17) 0.0027(14) -0.0004(14) -0.0048(14) N7 0.067(2) 0.0460(19) 0.068(2) 0.0153(17) -0.0140(19) -0.0037(17) N8 0.118(5) 0.147(5) 0.092(4) -0.045(4) 0.047(4) -0.062(4) N9 0.109(5) 0.149(6) 0.209(8) -0.017(6) 0.053(5) -0.019(4) O1 0.071(2) 0.0641(19) 0.078(2) -0.0347(16) -0.0072(17) -0.0127(15) O2 0.0326(12) 0.0592(16) 0.0684(18) -0.0066(13) 0.0025(11) 0.0093(11) O3 0.107(3) 0.0359(16) 0.145(4) -0.0060(19) -0.023(3) -0.0032(17) O4 0.0588(17) 0.079(2) 0.0490(17) -0.0037(14) -0.0114(13) -0.0135(15) O5 0.171(5) 0.087(3) 0.117(4) -0.017(3) -0.014(3) 0.062(3) O6 0.286(8) 0.128(4) 0.183(6) -0.046(4) -0.160(6) 0.097(5) O7 0.0459(14) 0.0533(16) 0.080(2) 0.0016(15) -0.0012(14) 0.0077(13) O8 0.389(14) 0.167(6) 0.120(5) 0.010(5) 0.119(7) -0.083(7) O9 0.078(4) 0.429(16) 0.204(8) -0.120(9) 0.030(4) -0.016(6) O10 0.0627(18) 0.083(2) 0.0594(18) 0.0049(16) 0.0116(15) -0.0127(16) C1 0.0337(16) 0.0428(18) 0.0454(19) -0.0082(15) 0.0039(14) -0.0029(13) C2 0.0367(16) 0.0485(19) 0.045(2) -0.0094(15) 0.0067(14) -0.0091(14) C3 0.0432(19) 0.065(2) 0.045(2) -0.0084(18) -0.0005(16) -0.0070(17) C4 0.0420(19) 0.069(3) 0.054(2) 0.003(2) -0.0017(17) 0.0008(18) C5 0.0322(16) 0.049(2) 0.059(2) -0.0032(17) 0.0049(16) 0.0011(14) C6 0.053(2) 0.046(2) 0.051(2) -0.0132(17) 0.0092(17) -0.0106(16) C7 0.0463(19) 0.0386(18) 0.053(2) -0.0148(15) 0.0117(16) -0.0026(15) C8 0.075(3) 0.038(2) 0.092(3) -0.016(2) 0.013(3) -0.004(2) C9 0.085(3) 0.038(2) 0.107(4) -0.003(2) 0.004(3) 0.012(2) C10 0.055(2) 0.044(2) 0.080(3) -0.002(2) -0.002(2) 0.0110(18) C11 0.0402(17) 0.0396(17) 0.0448(19) -0.0040(14) 0.0070(14) 0.0075(14) C12 0.0347(16) 0.0434(18) 0.0366(17) -0.0023(14) 0.0050(13) 0.0054(13) C13 0.0314(15) 0.0378(16) 0.0349(16) -0.0053(13) 0.0020(12) 0.0000(13) C14 0.0302(14) 0.0372(16) 0.0409(18) -0.0073(13) 0.0034(13) 0.0003(12) C15 0.0337(15) 0.0391(17) 0.0473(19) -0.0083(15) -0.0002(14) 0.0031(13) C16 0.0406(17) 0.0376(17) 0.0469(19) -0.0018(15) 0.0025(14) -0.0045(14) C17 0.0277(15) 0.0467(18) 0.0431(19) -0.0043(14) 0.0052(13) -0.0020(13) C18 0.058(2) 0.052(2) 0.054(2) 0.0028(18) -0.0039(18) -0.0129(18) C19 0.058(2) 0.060(3) 0.077(3) 0.007(2) -0.003(2) -0.025(2) C20 0.075(3) 0.043(2) 0.063(3) 0.0045(18) 0.002(2) -0.024(2) C21 0.068(2) 0.0352(17) 0.045(2) -0.0034(15) -0.0006(17) -0.0086(16) C22 0.056(2) 0.0401(18) 0.044(2) -0.0016(15) -0.0010(16) -0.0149(16) C23 0.080(3) 0.0349(19) 0.070(3) 0.0012(18) 0.001(2) -0.0065(19) C24 0.058(2) 0.044(2) 0.049(2) -0.0026(16) -0.0011(18) -0.0086(17) C25 0.073(3) 0.053(2) 0.045(2) -0.0138(18) 0.0028(19) -0.007(2) C26 0.062(2) 0.058(2) 0.038(2) -0.0084(17) -0.0024(17) -0.0108(19) C27 0.0486(19) 0.0488(19) 0.0380(19) -0.0005(15) -0.0003(15) -0.0145(16) C28 0.0492(19) 0.0434(18) 0.0379(19) 0.0001(15) 0.0000(15) -0.0117(15) C29 0.051(2) 0.059(2) 0.0374(19) 0.0018(16) 0.0025(16) -0.0097(17) C30 0.052(2) 0.063(2) 0.039(2) 0.0047(17) 0.0035(16) -0.0046(18) C31 0.053(2) 0.083(3) 0.065(3) 0.006(2) 0.003(2) 0.004(2) C32 0.069(3) 0.080(3) 0.078(3) 0.008(3) 0.003(3) 0.021(3) C33 0.085(3) 0.059(3) 0.075(3) 0.006(2) 0.007(3) 0.014(2) C34 0.070(3) 0.046(2) 0.053(2) 0.0063(18) 0.002(2) 0.0032(19) C35 0.089(4) 0.083(4) 0.099(4) -0.009(3) 0.013(3) 0.004(3) O1W 0.118(14) 0.071(10) 0.126(15) 0.016(9) 0.037(12) 0.037(10) O1W' 0.095(7) 0.35(2) 0.151(11) 0.146(13) 0.027(7) 0.098(11) O1W" 0.072(8) 0.170(16) 0.046(7) -0.016(9) 0.004(6) 0.066(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.030(3) . ? Cu1 N3 2.030(3) 3_665 ? Cu1 N1 2.073(3) 3_665 ? Cu1 N1 2.073(3) . ? Cu2 N4 2.040(3) 3_666 ? Cu2 N4 2.040(3) . ? Cu2 N6 2.063(3) . ? Cu2 N6 2.063(3) 3_666 ? N1 C1 1.332(4) . ? N1 C5 1.349(5) . ? N3 C15 1.331(4) . ? N3 C14 1.338(4) . ? N2 C7 1.335(4) . ? N2 C11 1.345(4) . ? N4 C22 1.336(5) . ? N4 C18 1.351(5) . ? N6 C28 1.344(5) . ? N6 C24 1.345(5) . ? N5 C30 1.335(5) . ? N5 C34 1.343(5) . ? N7 O6 1.155(6) . ? N7 O7 1.215(4) . ? N7 O5 1.245(5) . ? N8 O9 1.186(10) . ? N8 O10 1.192(6) . ? N8 O8 1.279(11) . ? N9 C35 1.141(8) . ? O1 C6 1.216(4) . ? O2 C12 1.216(4) . ? O3 C23 1.223(5) . ? O4 C29 1.215(4) . ? C1 C2 1.388(5) . ? C1 H1A 0.9300 . ? C2 C3 1.384(5) . ? C2 C6 1.488(5) . ? C3 C4 1.375(6) . ? C3 H3A 0.9300 . ? C4 C5 1.364(6) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.498(6) . ? C7 C8 1.394(6) . ? C8 C9 1.389(7) . ? C8 H8A 0.9300 . ? C9 C10 1.366(6) . ? C9 H9A 0.9300 . ? C10 C11 1.383(5) . ? C10 H10A 0.9300 . ? C11 C12 1.491(5) . ? C12 C13 1.491(4) . ? C13 C14 1.377(4) . ? C13 C17 1.387(5) . ? C14 H14A 0.9300 . ? C15 C16 1.375(5) . ? C15 H15A 0.9300 . ? C16 C17 1.383(5) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.379(6) . ? C18 H18A 0.9300 . ? C19 C20 1.369(6) . ? C19 H19A 0.9300 . ? C20 C21 1.385(6) . ? C20 H20A 0.9300 . ? C21 C22 1.389(5) . ? C21 C23 1.490(6) . ? C22 H22A 0.9300 . ? C23 C34 1.488(6) . ? C24 C25 1.383(6) . ? C24 H24A 0.9300 . ? C25 C26 1.378(6) . ? C25 H25A 0.9300 . ? C26 C27 1.381(5) . ? C26 H26A 0.9300 . ? C27 C28 1.391(5) . ? C27 C29 1.492(6) . ? C28 H28A 0.9300 . ? C29 C30 1.506(6) . ? C30 C31 1.399(6) . ? C31 C32 1.368(7) . ? C31 H31A 0.9300 . ? C32 C33 1.384(7) . ? C32 H32A 0.9300 . ? C33 C34 1.390(6) . ? C33 H33A 0.9300 . ? C35 C36 1.375(8) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? O1W O1W" 1.229(19) . ? O1W O1W' 1.32(2) . ? O1W' O1W" 1.60(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N3 180.0(2) . 3_665 ? N3 Cu1 N1 90.99(11) . 3_665 ? N3 Cu1 N1 89.01(11) 3_665 3_665 ? N3 Cu1 N1 89.01(11) . . ? N3 Cu1 N1 90.99(11) 3_665 . ? N1 Cu1 N1 180.00(15) 3_665 . ? N4 Cu2 N4 180.000(1) 3_666 . ? N4 Cu2 N6 88.27(11) 3_666 . ? N4 Cu2 N6 91.73(11) . . ? N4 Cu2 N6 91.73(11) 3_666 3_666 ? N4 Cu2 N6 88.27(11) . 3_666 ? N6 Cu2 N6 180.000(1) . 3_666 ? C1 N1 C5 116.5(3) . . ? C1 N1 Cu1 122.1(2) . . ? C5 N1 Cu1 120.9(2) . . ? C15 N3 C14 117.5(3) . . ? C15 N3 Cu1 123.1(2) . . ? C14 N3 Cu1 119.1(2) . . ? C7 N2 C11 118.4(3) . . ? C22 N4 C18 118.0(3) . . ? C22 N4 Cu2 121.8(2) . . ? C18 N4 Cu2 119.8(3) . . ? C28 N6 C24 118.3(3) . . ? C28 N6 Cu2 122.7(2) . . ? C24 N6 Cu2 118.7(3) . . ? C30 N5 C34 117.5(4) . . ? O6 N7 O7 125.3(5) . . ? O6 N7 O5 116.1(5) . . ? O7 N7 O5 118.4(4) . . ? O9 N8 O10 125.2(10) . . ? O9 N8 O8 119.8(8) . . ? O10 N8 O8 114.9(9) . . ? N1 C1 C2 123.9(4) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C3 C2 C1 117.8(3) . . ? C3 C2 C6 120.8(3) . . ? C1 C2 C6 121.4(3) . . ? C4 C3 C2 118.7(4) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N1 C5 C4 123.2(4) . . ? N1 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? O1 C6 C2 121.6(4) . . ? O1 C6 C7 120.5(3) . . ? C2 C6 C7 117.8(3) . . ? N2 C7 C8 122.2(4) . . ? N2 C7 C6 116.4(3) . . ? C8 C7 C6 121.4(4) . . ? C9 C8 C7 118.4(4) . . ? C9 C8 H8A 120.8 . . ? C7 C8 H8A 120.8 . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C9 C10 C11 118.9(4) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? N2 C11 C10 122.6(3) . . ? N2 C11 C12 116.7(3) . . ? C10 C11 C12 120.7(3) . . ? O2 C12 C11 119.8(3) . . ? O2 C12 C13 120.9(3) . . ? C11 C12 C13 119.3(3) . . ? C14 C13 C17 117.8(3) . . ? C14 C13 C12 121.7(3) . . ? C17 C13 C12 120.5(3) . . ? N3 C14 C13 123.9(3) . . ? N3 C14 H14A 118.0 . . ? C13 C14 H14A 118.0 . . ? N3 C15 C16 122.8(3) . . ? N3 C15 H15A 118.6 . . ? C16 C15 H15A 118.6 . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C16 C17 C13 118.7(3) . . ? C16 C17 H17A 120.7 . . ? C13 C17 H17A 120.7 . . ? N4 C18 C19 121.7(4) . . ? N4 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? C20 C19 C18 119.7(4) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 119.3(4) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C20 C21 C22 117.8(4) . . ? C20 C21 C23 120.2(3) . . ? C22 C21 C23 121.9(4) . . ? N4 C22 C21 123.2(4) . . ? N4 C22 H22A 118.4 . . ? C21 C22 H22A 118.4 . . ? O3 C23 C34 119.1(4) . . ? O3 C23 C21 119.2(4) . . ? C34 C23 C21 121.6(3) . . ? N6 C24 C25 121.8(4) . . ? N6 C24 H24A 119.1 . . ? C25 C24 H24A 119.1 . . ? C26 C25 C24 119.7(4) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C27 119.0(4) . . ? C25 C26 H26A 120.5 . . ? C27 C26 H26A 120.5 . . ? C26 C27 C28 118.4(4) . . ? C26 C27 C29 119.5(3) . . ? C28 C27 C29 122.0(3) . . ? N6 C28 C27 122.6(4) . . ? N6 C28 H28A 118.7 . . ? C27 C28 H28A 118.7 . . ? O4 C29 C27 121.1(4) . . ? O4 C29 C30 119.8(4) . . ? C27 C29 C30 118.9(3) . . ? N5 C30 C31 123.6(4) . . ? N5 C30 C29 117.3(3) . . ? C31 C30 C29 118.9(4) . . ? C32 C31 C30 118.4(5) . . ? C32 C31 H31A 120.8 . . ? C30 C31 H31A 120.8 . . ? C31 C32 C33 118.8(5) . . ? C31 C32 H32A 120.6 . . ? C33 C32 H32A 120.6 . . ? C32 C33 C34 119.5(5) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? N5 C34 C33 122.2(4) . . ? N5 C34 C23 117.4(4) . . ? C33 C34 C23 120.4(4) . . ? N9 C35 C36 177.9(9) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1W" O1W O1W' 78.0(16) . . ? O1W O1W' O1W" 48.5(12) . . ? O1W O1W" O1W' 53.5(12) . . ? 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 N3 Cu1 N1 C1 -68.9(3) . . . . ? N3 Cu1 N1 C1 111.1(3) 3_665 . . . ? N1 Cu1 N1 C1 45(100) 3_665 . . . ? N3 Cu1 N1 C5 103.4(3) . . . . ? N3 Cu1 N1 C5 -76.6(3) 3_665 . . . ? N1 Cu1 N1 C5 -143(100) 3_665 . . . ? N3 Cu1 N3 C15 91.0(3) 3_665 . . . ? N1 Cu1 N3 C15 67.2(3) 3_665 . . . ? N1 Cu1 N3 C15 -112.8(3) . . . . ? N3 Cu1 N3 C14 -95.2(2) 3_665 . . . ? N1 Cu1 N3 C14 -119.0(3) 3_665 . . . ? N1 Cu1 N3 C14 61.0(3) . . . . ? N4 Cu2 N4 C22 0(100) 3_666 . . . ? N6 Cu2 N4 C22 53.7(3) . . . . ? N6 Cu2 N4 C22 -126.3(3) 3_666 . . . ? N4 Cu2 N4 C18 0(100) 3_666 . . . ? N6 Cu2 N4 C18 -119.0(3) . . . . ? N6 Cu2 N4 C18 61.0(3) 3_666 . . . ? N4 Cu2 N6 C28 119.8(3) 3_666 . . . ? N4 Cu2 N6 C28 -60.2(3) . . . . ? N6 Cu2 N6 C28 -13(100) 3_666 . . . ? N4 Cu2 N6 C24 -66.6(3) 3_666 . . . ? N4 Cu2 N6 C24 113.4(3) . . . . ? N6 Cu2 N6 C24 161(100) 3_666 . . . ? C5 N1 C1 C2 -4.5(5) . . . . ? Cu1 N1 C1 C2 168.1(2) . . . . ? N1 C1 C2 C3 6.2(5) . . . . ? N1 C1 C2 C6 -172.5(3) . . . . ? C1 C2 C3 C4 -2.6(5) . . . . ? C6 C2 C3 C4 176.1(3) . . . . ? C2 C3 C4 C5 -2.1(6) . . . . ? C1 N1 C5 C4 -0.7(5) . . . . ? Cu1 N1 C5 C4 -173.4(3) . . . . ? C3 C4 C5 N1 4.0(6) . . . . ? C3 C2 C6 O1 34.6(5) . . . . ? C1 C2 C6 O1 -146.6(4) . . . . ? C3 C2 C6 C7 -142.2(4) . . . . ? C1 C2 C6 C7 36.5(5) . . . . ? C11 N2 C7 C8 -1.5(5) . . . . ? C11 N2 C7 C6 177.7(3) . . . . ? O1 C6 C7 N2 -153.6(4) . . . . ? C2 C6 C7 N2 23.3(5) . . . . ? O1 C6 C7 C8 25.7(6) . . . . ? C2 C6 C7 C8 -157.4(4) . . . . ? N2 C7 C8 C9 1.1(7) . . . . ? C6 C7 C8 C9 -178.1(4) . . . . ? C7 C8 C9 C10 0.2(8) . . . . ? C8 C9 C10 C11 -0.9(8) . . . . ? C7 N2 C11 C10 0.8(5) . . . . ? C7 N2 C11 C12 -176.8(3) . . . . ? C9 C10 C11 N2 0.5(7) . . . . ? C9 C10 C11 C12 177.9(4) . . . . ? N2 C11 C12 O2 154.4(3) . . . . ? C10 C11 C12 O2 -23.2(5) . . . . ? N2 C11 C12 C13 -25.1(5) . . . . ? C10 C11 C12 C13 157.3(4) . . . . ? O2 C12 C13 C14 149.9(3) . . . . ? C11 C12 C13 C14 -30.6(5) . . . . ? O2 C12 C13 C17 -29.4(5) . . . . ? C11 C12 C13 C17 150.1(3) . . . . ? C15 N3 C14 C13 1.1(5) . . . . ? Cu1 N3 C14 C13 -173.1(3) . . . . ? C17 C13 C14 N3 -1.8(5) . . . . ? C12 C13 C14 N3 178.9(3) . . . . ? C14 N3 C15 C16 0.5(5) . . . . ? Cu1 N3 C15 C16 174.5(3) . . . . ? N3 C15 C16 C17 -1.4(5) . . . . ? C15 C16 C17 C13 0.6(5) . . . . ? C14 C13 C17 C16 0.9(5) . . . . ? C12 C13 C17 C16 -179.8(3) . . . . ? C22 N4 C18 C19 0.6(6) . . . . ? Cu2 N4 C18 C19 173.6(3) . . . . ? N4 C18 C19 C20 -3.3(7) . . . . ? C18 C19 C20 C21 2.4(7) . . . . ? C19 C20 C21 C22 1.1(6) . . . . ? C19 C20 C21 C23 179.8(4) . . . . ? C18 N4 C22 C21 3.1(5) . . . . ? Cu2 N4 C22 C21 -169.7(3) . . . . ? C20 C21 C22 N4 -4.0(6) . . . . ? C23 C21 C22 N4 177.4(4) . . . . ? C20 C21 C23 O3 -31.9(6) . . . . ? C22 C21 C23 O3 146.7(5) . . . . ? C20 C21 C23 C34 146.9(4) . . . . ? C22 C21 C23 C34 -34.5(6) . . . . ? C28 N6 C24 C25 -0.8(5) . . . . ? Cu2 N6 C24 C25 -174.7(3) . . . . ? N6 C24 C25 C26 3.5(6) . . . . ? C24 C25 C26 C27 -1.7(6) . . . . ? C25 C26 C27 C28 -2.4(6) . . . . ? C25 C26 C27 C29 176.6(3) . . . . ? C24 N6 C28 C27 -3.6(5) . . . . ? Cu2 N6 C28 C27 170.0(3) . . . . ? C26 C27 C28 N6 5.3(5) . . . . ? C29 C27 C28 N6 -173.8(3) . . . . ? C26 C27 C29 O4 35.0(5) . . . . ? C28 C27 C29 O4 -145.9(4) . . . . ? C26 C27 C29 C30 -141.1(4) . . . . ? C28 C27 C29 C30 37.9(5) . . . . ? C34 N5 C30 C31 1.8(6) . . . . ? C34 N5 C30 C29 176.7(3) . . . . ? O4 C29 C30 N5 -162.8(3) . . . . ? C27 C29 C30 N5 13.4(5) . . . . ? O4 C29 C30 C31 12.4(5) . . . . ? C27 C29 C30 C31 -171.4(3) . . . . ? N5 C30 C31 C32 -1.4(6) . . . . ? C29 C30 C31 C32 -176.3(4) . . . . ? C30 C31 C32 C33 0.9(7) . . . . ? C31 C32 C33 C34 -0.9(7) . . . . ? C30 N5 C34 C33 -1.7(6) . . . . ? C30 N5 C34 C23 179.9(3) . . . . ? C32 C33 C34 N5 1.4(7) . . . . ? C32 C33 C34 C23 179.6(4) . . . . ? O3 C23 C34 N5 166.8(4) . . . . ? C21 C23 C34 N5 -12.1(6) . . . . ? O3 C23 C34 C33 -11.6(7) . . . . ? C21 C23 C34 C33 169.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.729 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.089 #===END