# Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Socety of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'ProfD Daofeng Sun' _publ_contact_author_email DFSUN@SDU.EDU.CN _publ_section_title ; Three Novel 3D Metal-organic Frameworks with 1D Ladder, Tube or Chain as Assembly Units ; loop_ _publ_author_name 'Daofeng Sun.' 'Fangna Dai.' 'Haiyan He.' 'Xin Tong.' 'Aiping Xie.' # Attachment '1.cif' data_080418c _database_code_depnum_ccdc_archive 'CCDC 675166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H26 Cu4 N4 O18 S' _chemical_formula_weight 1112.85 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' S S 0.1246 0.1234 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.5656(8) _cell_length_b 6.6676(2) _cell_length_c 21.2236(5) _cell_angle_alpha 90.00 _cell_angle_beta 126.7420(10) _cell_angle_gamma 90.00 _cell_volume 3806.26(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3264 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 22.65 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 2.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7989 _exptl_absorpt_correction_T_max 0.8915 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12823 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 23.29 _reflns_number_total 2738 _reflns_number_gt 2108 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1023P)^2^+23.1305P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2738 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 S S 1.0000 0.9738(4) 0.7500 0.0271(7) Uani 1 2 d S . . Cu1 Cu 0.89735(3) 0.65965(14) 0.64687(5) 0.0232(3) Uani 1 1 d . . . Cu2 Cu 1.00132(3) 0.51301(14) 0.81957(5) 0.0200(3) Uani 1 1 d . . . O1 O 0.8841(2) 0.6532(9) 0.7244(3) 0.0351(16) Uani 1 1 d . . . O2 O 0.95322(19) 0.5546(10) 0.8394(3) 0.0358(16) Uani 1 1 d . . . O3 O 0.95108(19) 0.5176(8) 1.0688(3) 0.0267(14) Uani 1 1 d . . . O4 O 0.87856(19) 0.4384(9) 1.0458(3) 0.0288(14) Uani 1 1 d . . . O5 O 0.7224(2) 0.5927(12) 0.7855(3) 0.0512(19) Uani 1 1 d . . . O6 O 0.7249(2) 0.5857(10) 0.6827(3) 0.0358(15) Uani 1 1 d . . . O7 O 0.95150(17) 0.4680(7) 0.7054(3) 0.0162(12) Uani 1 1 d . . . O8 O 0.9664(2) 0.8439(8) 0.6805(3) 0.0375(15) Uani 1 1 d . . . O9 O 0.9707(3) 1.0966(9) 0.7647(4) 0.0454(17) Uani 1 1 d . . . C1 C 0.8793(3) 0.5857(12) 0.8282(4) 0.0193(17) Uani 1 1 d . . . C2 C 0.9046(3) 0.5530(11) 0.9090(4) 0.0181(17) Uani 1 1 d . . . H2 H 0.9391 0.5430 0.9422 0.022 Uiso 1 1 calc R . . C3 C 0.8776(3) 0.5356(11) 0.9389(4) 0.0203(18) Uani 1 1 d . . . C4 C 0.8261(3) 0.5542(12) 0.8890(4) 0.0218(18) Uani 1 1 d . . . H4 H 0.8083 0.5464 0.9095 0.026 Uiso 1 1 calc R . . C5 C 0.8015(3) 0.5836(12) 0.8101(4) 0.0230(18) Uani 1 1 d . . . C6 C 0.8278(3) 0.6004(12) 0.7796(4) 0.0232(18) Uani 1 1 d . . . H6 H 0.8110 0.6219 0.7260 0.028 Uiso 1 1 calc R . . C7 C 0.9087(3) 0.6000(12) 0.7958(4) 0.0259(19) Uani 1 1 d . . . C8 C 0.9045(3) 0.4976(11) 1.0246(4) 0.0182(18) Uani 1 1 d . . . C9 C 0.7452(3) 0.5902(13) 0.7582(5) 0.032(2) Uani 1 1 d . . . C10 C 0.8433(4) 1.0244(15) 0.6325(5) 0.056(3) Uani 1 1 d . . . H10 H 0.8678 1.0280 0.6865 0.067 Uiso 1 1 calc R . . C11 C 0.8077(4) 1.1693(16) 0.5994(5) 0.063(4) Uani 1 1 d . . . H11 H 0.8086 1.2680 0.6312 0.075 Uiso 1 1 calc R . . C12 C 0.7699(3) 1.1729(13) 0.5190(5) 0.035(2) Uani 1 1 d . . . C13 C 0.7721(4) 1.0225(16) 0.4761(5) 0.058(3) Uani 1 1 d . . . H13 H 0.7486 1.0189 0.4217 0.070 Uiso 1 1 calc R . . C14 C 0.8083(4) 0.8799(16) 0.5131(5) 0.052(3) Uani 1 1 d . . . H14 H 0.8076 0.7788 0.4823 0.062 Uiso 1 1 calc R . . C15 C 0.8905(3) 0.0709(14) 0.8605(5) 0.037(2) Uani 1 1 d . . . H15 H 0.8697 0.0959 0.8067 0.045 Uiso 1 1 calc R . . C16 C 0.9415(3) 0.0508(14) 0.8976(5) 0.039(2) Uani 1 1 d . . . H16 H 0.9543 0.0626 0.8693 0.047 Uiso 1 1 calc R . . C17 C 0.9727(3) 0.0125(11) 0.9785(4) 0.0225(18) Uani 1 1 d . . . C18 C 0.9510(3) 0.0026(13) 1.0171(5) 0.032(2) Uani 1 1 d . . . H18 H 0.9708 -0.0165 1.0713 0.039 Uiso 1 1 calc R . . C19 C 0.9003(3) 0.0207(13) 0.9758(5) 0.036(2) Uani 1 1 d . . . H19 H 0.8864 0.0080 1.0027 0.044 Uiso 1 1 calc R . . N1 N 0.8448(3) 0.8747(11) 0.5906(4) 0.0342(18) Uani 1 1 d . . . N2 N 0.8702(2) 0.0559(11) 0.8984(4) 0.0333(17) 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 S 0.0383(18) 0.0187(16) 0.0333(17) 0.000 0.0262(15) 0.000 Cu1 0.0226(6) 0.0337(6) 0.0161(5) 0.0067(4) 0.0131(4) 0.0126(4) Cu2 0.0107(5) 0.0391(7) 0.0110(5) 0.0049(4) 0.0069(4) 0.0038(4) O1 0.028(3) 0.063(4) 0.018(3) 0.019(3) 0.016(3) 0.027(3) O2 0.012(3) 0.084(5) 0.011(3) 0.011(3) 0.007(3) 0.012(3) O3 0.012(3) 0.055(4) 0.010(3) 0.006(2) 0.005(2) 0.001(2) O4 0.018(3) 0.052(4) 0.017(3) -0.001(2) 0.011(3) -0.015(3) O5 0.021(3) 0.109(6) 0.032(3) 0.001(4) 0.021(3) 0.001(4) O6 0.020(3) 0.063(4) 0.016(3) 0.001(3) 0.005(3) 0.000(3) O7 0.009(3) 0.027(3) 0.012(3) 0.002(2) 0.005(2) 0.003(2) O8 0.041(4) 0.029(4) 0.033(3) 0.001(3) 0.017(3) -0.004(3) O9 0.071(5) 0.028(3) 0.067(4) 0.009(3) 0.057(4) 0.013(3) C1 0.016(4) 0.026(4) 0.018(4) -0.004(3) 0.011(3) -0.001(3) C2 0.013(4) 0.031(5) 0.012(4) 0.004(3) 0.008(3) 0.003(3) C3 0.015(4) 0.030(5) 0.015(4) 0.000(3) 0.009(3) 0.000(3) C4 0.021(4) 0.031(5) 0.023(4) 0.002(3) 0.019(4) -0.001(4) C5 0.012(4) 0.030(5) 0.022(4) 0.000(4) 0.007(4) -0.001(3) C6 0.023(5) 0.030(5) 0.011(4) -0.001(3) 0.008(3) 0.000(4) C7 0.029(5) 0.028(5) 0.026(5) 0.000(4) 0.020(4) 0.005(4) C8 0.026(5) 0.020(4) 0.014(4) 0.005(3) 0.014(4) 0.009(3) C9 0.017(4) 0.038(5) 0.031(5) 0.008(4) 0.008(4) 0.001(4) C10 0.073(8) 0.060(7) 0.021(5) 0.005(5) 0.021(5) 0.031(6) C11 0.087(8) 0.057(7) 0.028(5) 0.010(5) 0.026(6) 0.049(6) C12 0.038(5) 0.042(6) 0.035(5) 0.013(4) 0.027(4) 0.016(4) C13 0.049(7) 0.069(8) 0.024(5) 0.005(5) 0.005(5) 0.041(6) C14 0.049(6) 0.057(7) 0.040(6) -0.006(5) 0.022(5) 0.025(5) C15 0.029(5) 0.039(6) 0.029(5) -0.001(4) 0.009(4) 0.003(4) C16 0.023(5) 0.051(6) 0.038(5) -0.004(4) 0.015(4) -0.004(4) C17 0.016(4) 0.023(5) 0.022(4) -0.006(3) 0.008(4) -0.002(3) C18 0.017(5) 0.047(6) 0.022(4) -0.003(4) 0.006(4) 0.003(4) C19 0.030(5) 0.051(6) 0.035(5) -0.009(4) 0.023(5) 0.000(4) N1 0.037(4) 0.044(5) 0.024(4) 0.010(3) 0.019(4) 0.017(4) N2 0.017(4) 0.043(5) 0.035(4) -0.008(3) 0.013(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S O9 1.449(6) 2_756 ? S O9 1.449(6) . ? S O8 1.486(6) . ? S O8 1.486(6) 2_756 ? Cu1 O7 1.944(5) . ? Cu1 O1 1.944(5) . ? Cu1 O4 1.952(5) 6_565 ? Cu1 N1 2.018(7) . ? Cu1 O8 2.325(6) . ? Cu2 O2 1.916(5) . ? Cu2 O3 1.919(5) 5_767 ? Cu2 O7 1.970(5) 2_756 ? Cu2 O7 1.978(5) . ? Cu2 Cu2 2.9012(17) 2_756 ? O1 C7 1.268(9) . ? O2 C7 1.236(9) . ? O3 C8 1.260(9) . ? O3 Cu2 1.919(5) 5_767 ? O4 C8 1.259(9) . ? O4 Cu1 1.952(5) 6_566 ? O5 C9 1.203(10) . ? O6 C9 1.314(10) . ? O7 Cu2 1.970(5) 2_756 ? C1 C6 1.389(10) . ? C1 C2 1.402(10) . ? C1 C7 1.506(11) . ? C2 C3 1.387(10) . ? C3 C4 1.391(11) . ? C3 C8 1.492(10) . ? C4 C5 1.368(10) . ? C5 C6 1.376(11) . ? C5 C9 1.514(11) . ? C10 N1 1.358(11) . ? C10 C11 1.361(13) . ? C11 C12 1.389(12) . ? C12 C13 1.385(12) . ? C12 C12 1.486(16) 7_676 ? C13 C14 1.363(13) . ? C14 N1 1.340(11) . ? C15 N2 1.333(11) . ? C15 C16 1.397(12) . ? C16 C17 1.399(12) . ? C17 C18 1.388(12) . ? C17 C17 1.487(15) 5_757 ? C18 C19 1.376(12) . ? C19 N2 1.337(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 S O9 111.2(5) 2_756 . ? O9 S O8 109.0(3) 2_756 . ? O9 S O8 109.4(4) . . ? O9 S O8 109.4(4) 2_756 2_756 ? O9 S O8 109.0(3) . 2_756 ? O8 S O8 108.7(5) . 2_756 ? O7 Cu1 O1 92.6(2) . . ? O7 Cu1 O4 92.6(2) . 6_565 ? O1 Cu1 O4 146.7(3) . 6_565 ? O7 Cu1 N1 175.8(3) . . ? O1 Cu1 N1 87.4(2) . . ? O4 Cu1 N1 89.7(2) 6_565 . ? O7 Cu1 O8 76.8(2) . . ? O1 Cu1 O8 116.3(2) . . ? O4 Cu1 O8 97.0(2) 6_565 . ? N1 Cu1 O8 99.4(3) . . ? O2 Cu2 O3 86.2(2) . 5_767 ? O2 Cu2 O7 177.6(2) . 2_756 ? O3 Cu2 O7 96.1(2) 5_767 2_756 ? O2 Cu2 O7 94.9(2) . . ? O3 Cu2 O7 165.1(2) 5_767 . ? O7 Cu2 O7 82.7(2) 2_756 . ? O2 Cu2 Cu2 134.96(16) . 2_756 ? O3 Cu2 Cu2 138.87(16) 5_767 2_756 ? O7 Cu2 Cu2 42.80(13) 2_756 2_756 ? O7 Cu2 Cu2 42.61(14) . 2_756 ? C7 O1 Cu1 134.6(5) . . ? C7 O2 Cu2 132.2(5) . . ? C8 O3 Cu2 130.8(5) . 5_767 ? C8 O4 Cu1 131.3(5) . 6_566 ? Cu1 O7 Cu2 108.8(2) . 2_756 ? Cu1 O7 Cu2 117.7(2) . . ? Cu2 O7 Cu2 94.6(2) 2_756 . ? S O8 Cu1 129.7(3) . . ? C6 C1 C2 119.5(7) . . ? C6 C1 C7 121.4(7) . . ? C2 C1 C7 119.1(7) . . ? C3 C2 C1 119.2(7) . . ? C2 C3 C4 119.9(7) . . ? C2 C3 C8 119.2(7) . . ? C4 C3 C8 120.9(7) . . ? C5 C4 C3 120.7(7) . . ? C4 C5 C6 119.9(7) . . ? C4 C5 C9 118.1(7) . . ? C6 C5 C9 121.9(7) . . ? C5 C6 C1 120.6(7) . . ? O2 C7 O1 126.5(7) . . ? O2 C7 C1 118.1(7) . . ? O1 C7 C1 115.3(7) . . ? O4 C8 O3 125.7(6) . . ? O4 C8 C3 116.5(7) . . ? O3 C8 C3 117.7(7) . . ? O5 C9 O6 124.8(7) . . ? O5 C9 C5 121.8(8) . . ? O6 C9 C5 113.4(7) . . ? N1 C10 C11 123.4(9) . . ? C10 C11 C12 121.3(9) . . ? C13 C12 C11 115.3(8) . . ? C13 C12 C12 121.9(10) . 7_676 ? C11 C12 C12 122.8(10) . 7_676 ? C14 C13 C12 120.3(9) . . ? N1 C14 C13 124.9(9) . . ? N2 C15 C16 123.2(8) . . ? C15 C16 C17 118.5(8) . . ? C18 C17 C16 117.3(8) . . ? C18 C17 C17 121.4(9) . 5_757 ? C16 C17 C17 121.2(9) . 5_757 ? C19 C18 C17 120.4(8) . . ? N2 C19 C18 122.4(8) . . ? C14 N1 C10 114.8(7) . . ? C14 N1 Cu1 125.4(6) . . ? C10 N1 Cu1 119.8(6) . . ? C15 N2 C19 118.1(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.295 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.169 # Attachment '2.cif' data_071204a _database_code_depnum_ccdc_archive 'CCDC 675167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common none _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 Cu1.50 N2 O7.50' _chemical_formula_weight 525.69 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 monoclinic _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 18.8020(17) _cell_length_b 8.5577(8) _cell_length_c 16.0542(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.469(7) _cell_angle_gamma 90.00 _cell_volume 2548.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 695 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 14.47 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1070 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7446 _exptl_absorpt_correction_T_max 0.9027 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20774 _diffrn_reflns_av_R_equivalents 0.2301 _diffrn_reflns_av_sigmaI/netI 0.2380 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4349 _reflns_number_gt 1786 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1316P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4349 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2326 _refine_ls_R_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.2842 _refine_ls_wR_factor_gt 0.2151 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.5000 0.4452(2) 0.2500 0.0329(7) Uani 1 2 d S . . O1 O 0.2798(5) 1.2283(12) 0.1645(7) 0.063(3) Uani 1 1 d . . . N1 N 0.4963(5) 0.2853(11) 0.1598(6) 0.030(3) Uani 1 1 d . . . C1 C 0.2488(7) 1.108(2) 0.1740(8) 0.051(4) Uani 1 1 d . . . N2 N 0.1313(6) 1.3878(14) 0.1747(7) 0.045(3) Uani 1 1 d . . . C2 C 0.3536(7) 0.8933(16) 0.2685(8) 0.054(4) Uani 1 1 d . . . H2A H 0.3461 1.0019 0.2795 0.081 Uiso 1 1 calc R . . H2B H 0.4044 0.8724 0.2749 0.081 Uiso 1 1 calc R . . H2C H 0.3326 0.8305 0.3077 0.081 Uiso 1 1 calc R . . C3 C 0.3917(7) 0.6118(14) 0.1887(8) 0.032(3) Uani 1 1 d . . . C4 C 0.3253(6) 0.5313(15) 0.0185(8) 0.047(4) Uani 1 1 d . . . H4A H 0.3762 0.5278 0.0171 0.070 Uiso 1 1 calc R . . H4B H 0.2992 0.5246 -0.0380 0.070 Uiso 1 1 calc R . . H4C H 0.3123 0.4451 0.0512 0.070 Uiso 1 1 calc R . . C5 C 0.2248(7) 0.7526(14) -0.0779(8) 0.032(3) Uani 1 1 d . . . C6 C 0.1827(8) 1.0324(18) 0.0016(9) 0.076(5) Uani 1 1 d . . . H6A H 0.1934 1.0476 -0.0543 0.115 Uiso 1 1 calc R . . H6B H 0.1852 1.1309 0.0306 0.115 Uiso 1 1 calc R . . H6C H 0.1351 0.9896 -0.0019 0.115 Uiso 1 1 calc R . . C7 C 0.2675(6) 0.9514(14) 0.1327(7) 0.029(3) Uani 1 1 d . . . C8 C 0.3169(6) 0.8527(15) 0.1756(7) 0.032(3) Uani 1 1 d . . . C9 C 0.3363(6) 0.7184(14) 0.1386(7) 0.026(3) Uani 1 1 d . . . C10 C 0.3070(6) 0.6834(14) 0.0583(7) 0.029(3) Uani 1 1 d . . . C11 C 0.2566(6) 0.7870(14) 0.0128(7) 0.028(3) Uani 1 1 d . . . C12 C 0.2374(6) 0.9200(15) 0.0498(8) 0.036(3) Uani 1 1 d . . . C13 C 0.4421(8) 0.1948(18) 0.1370(10) 0.068(5) Uani 1 1 d . . . H13 H 0.4014 0.2058 0.1625 0.082 Uiso 1 1 calc R . . C14 C 0.5531(8) 0.2644(17) 0.1225(9) 0.065(5) Uani 1 1 d . . . H14 H 0.5932 0.3277 0.1387 0.078 Uiso 1 1 calc R . . C15 C 0.4425(8) 0.0813(19) 0.0754(10) 0.068(5) Uani 1 1 d . . . H15 H 0.4022 0.0175 0.0618 0.082 Uiso 1 1 calc R . . C16 C 0.5562(7) 0.1532(17) 0.0604(10) 0.062(5) Uani 1 1 d . . . H16 H 0.5981 0.1437 0.0369 0.074 Uiso 1 1 calc R . . C17 C 0.4998(6) 0.0587(13) 0.0335(7) 0.028(3) Uani 1 1 d . . . C18 C 0.1461(7) 1.485(2) 0.1158(10) 0.067(5) Uani 1 1 d . . . H18 H 0.1929 1.5229 0.1212 0.080 Uiso 1 1 calc R . . C19 C 0.0651(7) 1.3302(18) 0.1632(9) 0.064(5) Uani 1 1 d . . . H19 H 0.0537 1.2594 0.2030 0.077 Uiso 1 1 calc R . . C20 C 0.0966(6) 1.5341(17) 0.0458(8) 0.054(4) Uani 1 1 d . . . H20 H 0.1106 1.6025 0.0065 0.065 Uiso 1 1 calc R . . C21 C 0.0128(7) 1.3672(19) 0.0978(9) 0.065(5) Uani 1 1 d . . . H21 H -0.0321 1.3195 0.0930 0.078 Uiso 1 1 calc R . . C22 C 0.0261(6) 1.4787(17) 0.0363(8) 0.046(4) Uani 1 1 d . . . Cu2 Cu 0.20825(7) 1.31522(19) 0.26578(10) 0.0379(6) Uani 1 1 d . . . O2 O 0.1974(5) 1.0943(10) 0.2197(5) 0.047(2) Uani 1 1 d . . . O3 O 0.3745(4) 0.5281(10) 0.2469(6) 0.047(2) Uani 1 1 d . . . O4 O 0.4544(5) 0.6043(10) 0.1679(5) 0.044(2) Uani 1 1 d . . . O5 O 0.2684(4) 0.7572(10) -0.1311(5) 0.038(2) Uani 1 1 d . . . O6 O 0.1603(4) 0.7183(11) -0.1006(5) 0.053(3) Uani 1 1 d . . . O7 O 0.2456(5) 1.5324(10) 0.2894(6) 0.053(3) Uani 1 1 d . . . O8 O 0.1581(10) 0.7926(17) 0.2673(13) 0.056(5) Uani 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 0.0289(12) 0.0310(14) 0.0356(14) 0.000 -0.0046(10) 0.000 O1 0.052(6) 0.041(7) 0.099(9) -0.012(6) 0.017(6) -0.013(5) N1 0.034(6) 0.036(7) 0.019(6) -0.010(5) 0.005(5) -0.010(5) C1 0.031(8) 0.089(14) 0.029(9) 0.010(9) -0.008(7) 0.015(8) N2 0.037(7) 0.055(8) 0.042(7) 0.013(6) 0.000(6) 0.018(6) C2 0.049(8) 0.049(9) 0.057(10) -0.007(8) -0.011(7) 0.013(7) C3 0.036(8) 0.017(7) 0.040(9) -0.011(6) -0.006(6) 0.003(6) C4 0.038(7) 0.054(10) 0.044(9) 0.007(8) -0.009(6) 0.011(7) C5 0.045(8) 0.033(8) 0.019(7) 0.008(6) 0.004(6) 0.008(6) C6 0.098(12) 0.077(13) 0.042(10) 0.003(9) -0.023(8) 0.049(10) C7 0.031(6) 0.028(8) 0.028(7) -0.009(6) 0.001(6) -0.002(6) C8 0.031(7) 0.042(9) 0.021(7) -0.003(6) 0.002(5) -0.006(6) C9 0.028(6) 0.032(8) 0.021(7) -0.005(6) 0.008(5) 0.003(6) C10 0.029(6) 0.028(7) 0.027(7) 0.003(6) 0.002(5) -0.005(6) C11 0.025(6) 0.036(8) 0.022(7) 0.000(6) 0.006(5) -0.007(6) C12 0.027(7) 0.037(9) 0.043(9) 0.000(7) 0.001(6) 0.005(6) C13 0.072(11) 0.068(12) 0.070(12) -0.041(10) 0.030(9) -0.026(10) C14 0.071(11) 0.059(11) 0.066(11) -0.036(9) 0.014(9) -0.044(9) C15 0.048(9) 0.077(13) 0.084(13) -0.031(10) 0.024(9) -0.036(9) C16 0.045(8) 0.062(11) 0.083(12) -0.030(10) 0.027(8) -0.004(8) C17 0.033(6) 0.022(7) 0.027(8) 0.001(6) 0.002(6) -0.010(6) C18 0.026(7) 0.099(14) 0.074(12) 0.026(11) 0.004(7) -0.004(8) C19 0.040(8) 0.076(12) 0.068(11) 0.030(10) -0.017(8) -0.003(8) C20 0.038(7) 0.078(11) 0.042(9) 0.033(8) -0.010(6) -0.023(8) C21 0.035(8) 0.092(13) 0.062(11) 0.032(10) -0.010(7) -0.004(8) C22 0.028(7) 0.064(10) 0.045(10) 0.007(8) 0.004(6) -0.001(7) Cu2 0.0306(9) 0.0431(11) 0.0370(10) 0.0014(9) -0.0032(7) 0.0064(8) O2 0.053(6) 0.041(6) 0.045(6) -0.006(5) -0.004(5) 0.002(5) O3 0.040(5) 0.042(6) 0.055(6) 0.019(5) -0.003(5) 0.000(5) O4 0.042(5) 0.046(6) 0.039(6) 0.010(5) -0.007(4) 0.011(5) O5 0.037(5) 0.051(6) 0.023(5) 0.000(4) -0.004(4) -0.011(4) O6 0.028(5) 0.079(8) 0.048(6) 0.004(5) -0.002(4) -0.018(5) O7 0.055(6) 0.046(6) 0.055(6) -0.006(5) 0.000(5) -0.012(5) O8 0.072(13) 0.004(9) 0.096(16) 0.008(10) 0.029(11) -0.002(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.986(9) 2_655 ? Cu1 N1 1.986(9) . ? Cu1 O4 1.988(8) 2_655 ? Cu1 O4 1.988(8) . ? Cu1 C3 2.547(12) 2_655 ? Cu1 C3 2.547(12) . ? O1 C1 1.204(17) . ? O1 Cu2 2.392(10) . ? N1 C13 1.285(15) . ? N1 C14 1.320(16) . ? C1 O2 1.311(15) . ? C1 C7 1.561(19) . ? C1 Cu2 2.503(16) . ? N2 C18 1.320(16) . ? N2 C19 1.324(16) . ? N2 Cu2 1.980(10) . ? C2 C8 1.576(15) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O3 1.261(14) . ? C3 O4 1.280(14) . ? C3 C9 1.512(15) . ? C4 C10 1.515(16) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O6 1.242(14) . ? C5 O5 1.278(14) . ? C5 C11 1.509(16) . ? C5 Cu2 2.545(12) 4_575 ? C6 C12 1.523(16) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.357(15) . ? C7 C12 1.384(15) . ? C8 C9 1.370(15) . ? C9 C10 1.350(15) . ? C10 C11 1.410(15) . ? C11 C12 1.360(15) . ? C13 C15 1.387(18) . ? C13 H13 0.9300 . ? C14 C16 1.386(18) . ? C14 H14 0.9300 . ? C15 C17 1.375(17) . ? C15 H15 0.9300 . ? C16 C17 1.347(16) . ? C16 H16 0.9300 . ? C17 C17 1.47(2) 3_655 ? C18 C20 1.401(17) . ? C18 H18 0.9300 . ? C19 C21 1.352(17) . ? C19 H19 0.9300 . ? C20 C22 1.393(16) . ? C20 H20 0.9300 . ? C21 C22 1.424(18) . ? C21 H21 0.9300 . ? C22 C22 1.44(2) 3_585 ? Cu2 O5 1.947(8) 4_576 ? Cu2 O7 2.001(9) . ? Cu2 O2 2.028(9) . ? Cu2 C5 2.545(12) 4_576 ? O5 Cu2 1.947(8) 4_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 92.8(6) 2_655 . ? N1 Cu1 O4 91.7(4) 2_655 2_655 ? N1 Cu1 O4 156.2(4) . 2_655 ? N1 Cu1 O4 156.2(4) 2_655 . ? N1 Cu1 O4 91.7(4) . . ? O4 Cu1 O4 93.6(5) 2_655 . ? N1 Cu1 C3 100.1(4) 2_655 2_655 ? N1 Cu1 C3 126.7(4) . 2_655 ? O4 Cu1 C3 29.7(4) 2_655 2_655 ? O4 Cu1 C3 95.9(3) . 2_655 ? N1 Cu1 C3 126.7(4) 2_655 . ? N1 Cu1 C3 100.1(4) . . ? O4 Cu1 C3 95.9(3) 2_655 . ? O4 Cu1 C3 29.7(4) . . ? C3 Cu1 C3 111.9(5) 2_655 . ? C1 O1 Cu2 80.9(9) . . ? C13 N1 C14 116.9(12) . . ? C13 N1 Cu1 123.6(10) . . ? C14 N1 Cu1 119.4(8) . . ? O1 C1 O2 124.3(16) . . ? O1 C1 C7 122.2(13) . . ? O2 C1 C7 113.5(14) . . ? O1 C1 Cu2 70.7(10) . . ? O2 C1 Cu2 53.9(7) . . ? C7 C1 Cu2 165.9(11) . . ? C18 N2 C19 116.0(11) . . ? C18 N2 Cu2 120.8(9) . . ? C19 N2 Cu2 122.8(10) . . ? C8 C2 H2A 109.5 . . ? C8 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C8 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O3 C3 O4 121.7(11) . . ? O3 C3 C9 119.9(11) . . ? O4 C3 C9 118.4(12) . . ? O3 C3 Cu1 71.5(7) . . ? O4 C3 Cu1 50.2(6) . . ? C9 C3 Cu1 168.4(10) . . ? C10 C4 H4A 109.5 . . ? C10 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C10 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O6 C5 O5 120.9(11) . . ? O6 C5 C11 122.9(12) . . ? O5 C5 C11 116.2(11) . . ? O6 C5 Cu2 72.6(7) . 4_575 ? O5 C5 Cu2 48.4(5) . 4_575 ? C11 C5 Cu2 163.9(9) . 4_575 ? C12 C6 H6A 109.5 . . ? C12 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C12 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 120.3(11) . . ? C8 C7 C1 120.1(10) . . ? C12 C7 C1 119.4(11) . . ? C7 C8 C9 120.8(11) . . ? C7 C8 C2 120.0(11) . . ? C9 C8 C2 119.2(11) . . ? C10 C9 C8 120.2(11) . . ? C10 C9 C3 120.7(11) . . ? C8 C9 C3 119.0(10) . . ? C9 C10 C11 119.3(11) . . ? C9 C10 C4 120.6(11) . . ? C11 C10 C4 120.1(10) . . ? C12 C11 C10 120.3(11) . . ? C12 C11 C5 119.5(11) . . ? C10 C11 C5 120.2(11) . . ? C11 C12 C7 119.1(11) . . ? C11 C12 C6 120.8(11) . . ? C7 C12 C6 120.1(12) . . ? N1 C13 C15 121.9(14) . . ? N1 C13 H13 119.1 . . ? C15 C13 H13 119.1 . . ? N1 C14 C16 123.5(13) . . ? N1 C14 H14 118.3 . . ? C16 C14 H14 118.3 . . ? C17 C15 C13 122.9(13) . . ? C17 C15 H15 118.5 . . ? C13 C15 H15 118.5 . . ? C17 C16 C14 121.3(13) . . ? C17 C16 H16 119.4 . . ? C14 C16 H16 119.4 . . ? C16 C17 C15 113.5(12) . . ? C16 C17 C17 123.1(14) . 3_655 ? C15 C17 C17 123.4(13) . 3_655 ? N2 C18 C20 125.1(13) . . ? N2 C18 H18 117.5 . . ? C20 C18 H18 117.5 . . ? N2 C19 C21 124.5(14) . . ? N2 C19 H19 117.7 . . ? C21 C19 H19 117.7 . . ? C22 C20 C18 118.6(12) . . ? C22 C20 H20 120.7 . . ? C18 C20 H20 120.7 . . ? C19 C21 C22 120.5(13) . . ? C19 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C20 C22 C21 115.1(11) . . ? C20 C22 C22 120.8(16) . 3_585 ? C21 C22 C22 123.8(15) . 3_585 ? O5 Cu2 N2 168.5(4) 4_576 . ? O5 Cu2 O7 89.9(4) 4_576 . ? N2 Cu2 O7 92.3(4) . . ? O5 Cu2 O2 91.3(3) 4_576 . ? N2 Cu2 O2 90.3(4) . . ? O7 Cu2 O2 161.1(4) . . ? O5 Cu2 O1 99.6(4) 4_576 . ? N2 Cu2 O1 91.1(4) . . ? O7 Cu2 O1 101.4(4) . . ? O2 Cu2 O1 59.7(3) . . ? O5 Cu2 C1 94.9(4) 4_576 . ? N2 Cu2 C1 92.5(4) . . ? O7 Cu2 C1 129.6(5) . . ? O2 Cu2 C1 31.5(4) . . ? O1 Cu2 C1 28.4(4) . . ? O5 Cu2 C5 29.4(3) 4_576 4_576 ? N2 Cu2 C5 139.1(5) . 4_576 ? O7 Cu2 C5 92.5(4) . 4_576 ? O2 Cu2 C5 97.8(4) . 4_576 ? O1 Cu2 C5 127.5(4) . 4_576 ? C1 Cu2 C5 114.8(4) . 4_576 ? C1 O2 Cu2 94.7(9) . . ? C3 O4 Cu1 100.1(8) . . ? C5 O5 Cu2 102.2(7) . 4_575 ? 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 Cu1 N1 C13 68.6(11) 2_655 . . . ? O4 Cu1 N1 C13 169.1(11) 2_655 . . . ? O4 Cu1 N1 C13 -88.1(12) . . . . ? C3 Cu1 N1 C13 173.3(11) 2_655 . . . ? C3 Cu1 N1 C13 -59.5(12) . . . . ? N1 Cu1 N1 C14 -108.8(11) 2_655 . . . ? O4 Cu1 N1 C14 -8.2(16) 2_655 . . . ? O4 Cu1 N1 C14 94.6(11) . . . . ? C3 Cu1 N1 C14 -4.0(12) 2_655 . . . ? C3 Cu1 N1 C14 123.2(11) . . . . ? Cu2 O1 C1 O2 5.7(12) . . . . ? Cu2 O1 C1 C7 -173.8(11) . . . . ? N1 Cu1 C3 O3 2.5(9) 2_655 . . . ? N1 Cu1 C3 O3 103.8(7) . . . . ? O4 Cu1 C3 O3 -93.9(7) 2_655 . . . ? O4 Cu1 C3 O3 179.2(11) . . . . ? C3 Cu1 C3 O3 -119.8(7) 2_655 . . . ? N1 Cu1 C3 O4 -176.6(7) 2_655 . . . ? N1 Cu1 C3 O4 -75.4(7) . . . . ? O4 Cu1 C3 O4 86.9(8) 2_655 . . . ? C3 Cu1 C3 O4 61.1(6) 2_655 . . . ? N1 Cu1 C3 C9 -167(4) 2_655 . . . ? N1 Cu1 C3 C9 -66(4) . . . . ? O4 Cu1 C3 C9 96(4) 2_655 . . . ? O4 Cu1 C3 C9 10(4) . . . . ? C3 Cu1 C3 C9 71(4) 2_655 . . . ? O1 C1 C7 C8 91.9(16) . . . . ? O2 C1 C7 C8 -87.6(14) . . . . ? Cu2 C1 C7 C8 -63(4) . . . . ? O1 C1 C7 C12 -83.2(16) . . . . ? O2 C1 C7 C12 97.3(13) . . . . ? Cu2 C1 C7 C12 122(3) . . . . ? C12 C7 C8 C9 -1.8(18) . . . . ? C1 C7 C8 C9 -176.9(12) . . . . ? C12 C7 C8 C2 177.2(11) . . . . ? C1 C7 C8 C2 2.1(18) . . . . ? C7 C8 C9 C10 0.7(18) . . . . ? C2 C8 C9 C10 -178.2(11) . . . . ? C7 C8 C9 C3 179.9(11) . . . . ? C2 C8 C9 C3 0.9(17) . . . . ? O3 C3 C9 C10 -106.6(13) . . . . ? O4 C3 C9 C10 70.4(15) . . . . ? Cu1 C3 C9 C10 62(4) . . . . ? O3 C3 C9 C8 74.2(15) . . . . ? O4 C3 C9 C8 -108.8(13) . . . . ? Cu1 C3 C9 C8 -117(4) . . . . ? C8 C9 C10 C11 0.5(17) . . . . ? C3 C9 C10 C11 -178.7(11) . . . . ? C8 C9 C10 C4 -176.9(11) . . . . ? C3 C9 C10 C4 3.9(17) . . . . ? C9 C10 C11 C12 -0.6(17) . . . . ? C4 C10 C11 C12 176.8(11) . . . . ? C9 C10 C11 C5 178.2(11) . . . . ? C4 C10 C11 C5 -4.4(16) . . . . ? O6 C5 C11 C12 -69.3(16) . . . . ? O5 C5 C11 C12 112.2(13) . . . . ? Cu2 C5 C11 C12 128(3) 4_575 . . . ? O6 C5 C11 C10 111.9(14) . . . . ? O5 C5 C11 C10 -66.7(15) . . . . ? Cu2 C5 C11 C10 -51(4) 4_575 . . . ? C10 C11 C12 C7 -0.4(17) . . . . ? C5 C11 C12 C7 -179.3(11) . . . . ? C10 C11 C12 C6 -179.6(12) . . . . ? C5 C11 C12 C6 1.5(18) . . . . ? C8 C7 C12 C11 1.6(18) . . . . ? C1 C7 C12 C11 176.7(12) . . . . ? C8 C7 C12 C6 -179.2(12) . . . . ? C1 C7 C12 C6 -4.1(19) . . . . ? C14 N1 C13 C15 -1(2) . . . . ? Cu1 N1 C13 C15 -178.0(12) . . . . ? C13 N1 C14 C16 1(2) . . . . ? Cu1 N1 C14 C16 178.4(12) . . . . ? N1 C13 C15 C17 -1(3) . . . . ? N1 C14 C16 C17 1(3) . . . . ? C14 C16 C17 C15 -2(2) . . . . ? C14 C16 C17 C17 178.6(15) . . . 3_655 ? C13 C15 C17 C16 2(2) . . . . ? C13 C15 C17 C17 -178.4(15) . . . 3_655 ? C19 N2 C18 C20 3(2) . . . . ? Cu2 N2 C18 C20 175.4(12) . . . . ? C18 N2 C19 C21 -2(2) . . . . ? Cu2 N2 C19 C21 -174.3(13) . . . . ? N2 C18 C20 C22 0(3) . . . . ? N2 C19 C21 C22 -2(3) . . . . ? C18 C20 C22 C21 -4(2) . . . . ? C18 C20 C22 C22 -177.6(17) . . . 3_585 ? C19 C21 C22 C20 5(2) . . . . ? C19 C21 C22 C22 178.3(18) . . . 3_585 ? C18 N2 Cu2 O5 148.3(19) . . . 4_576 ? C19 N2 Cu2 O5 -39(3) . . . 4_576 ? C18 N2 Cu2 O7 47.8(12) . . . . ? C19 N2 Cu2 O7 -140.0(12) . . . . ? C18 N2 Cu2 O2 -113.4(12) . . . . ? C19 N2 Cu2 O2 58.8(12) . . . . ? C18 N2 Cu2 O1 -53.7(12) . . . . ? C19 N2 Cu2 O1 118.5(12) . . . . ? C18 N2 Cu2 C1 -82.0(12) . . . . ? C19 N2 Cu2 C1 90.2(13) . . . . ? C18 N2 Cu2 C5 144.2(11) . . . 4_576 ? C19 N2 Cu2 C5 -43.6(15) . . . 4_576 ? C1 O1 Cu2 O5 82.4(8) . . . 4_576 ? C1 O1 Cu2 N2 -93.2(8) . . . . ? C1 O1 Cu2 O7 174.2(8) . . . . ? C1 O1 Cu2 O2 -3.5(7) . . . . ? C1 O1 Cu2 C5 72.1(9) . . . 4_576 ? O1 C1 Cu2 O5 -101.2(8) . . . 4_576 ? O2 C1 Cu2 O5 84.6(7) . . . 4_576 ? C7 C1 Cu2 O5 57(4) . . . 4_576 ? O1 C1 Cu2 N2 87.7(8) . . . . ? O2 C1 Cu2 N2 -86.5(7) . . . . ? C7 C1 Cu2 N2 -115(3) . . . . ? O1 C1 Cu2 O7 -7.3(10) . . . . ? O2 C1 Cu2 O7 178.4(6) . . . . ? C7 C1 Cu2 O7 150(3) . . . . ? O1 C1 Cu2 O2 174.2(12) . . . . ? C7 C1 Cu2 O2 -28(3) . . . . ? O2 C1 Cu2 O1 -174.2(12) . . . . ? C7 C1 Cu2 O1 158(4) . . . . ? O1 C1 Cu2 C5 -123.7(8) . . . 4_576 ? O2 C1 Cu2 C5 62.1(7) . . . 4_576 ? C7 C1 Cu2 C5 34(4) . . . 4_576 ? O1 C1 O2 Cu2 -6.6(14) . . . . ? C7 C1 O2 Cu2 172.8(8) . . . . ? O5 Cu2 O2 C1 -97.1(7) 4_576 . . . ? N2 Cu2 O2 C1 94.3(7) . . . . ? O7 Cu2 O2 C1 -3.7(14) . . . . ? O1 Cu2 O2 C1 3.2(7) . . . . ? C5 Cu2 O2 C1 -125.9(7) 4_576 . . . ? O3 C3 O4 Cu1 -0.9(13) . . . . ? C9 C3 O4 Cu1 -177.8(8) . . . . ? N1 Cu1 O4 C3 6.8(13) 2_655 . . . ? N1 Cu1 O4 C3 107.6(7) . . . . ? O4 Cu1 O4 C3 -95.6(7) 2_655 . . . ? C3 Cu1 O4 C3 -125.3(7) 2_655 . . . ? O6 C5 O5 Cu2 -4.5(14) . . . 4_575 ? C11 C5 O5 Cu2 174.1(8) . . . 4_575 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.530 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.151 # Attachment '3.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 687867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H41 Cd2 N5 O17' _chemical_formula_weight 992.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.500(5) _cell_length_b 18.577(5) _cell_length_c 15.394(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.97(3) _cell_angle_gamma 90.00 _cell_volume 4024(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5534 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 24.74 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7273 _exptl_absorpt_correction_T_max 0.8951 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13780 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.74 _reflns_number_total 6452 _reflns_number_gt 5200 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+55.6045P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(5) _refine_ls_number_reflns 6452 _refine_ls_number_parameters 490 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1871 _refine_ls_wR_factor_gt 0.1270 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.005 _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 Cd1 Cd 0.61146(6) 0.20923(4) 0.11651(6) 0.0336(2) Uani 1 1 d . . . Cd2 Cd 0.41301(6) 0.30600(4) 0.32715(6) 0.0352(3) Uani 1 1 d . . . O1 O 0.4395(8) 0.2704(5) 0.1917(6) 0.051(3) Uani 1 1 d . . . O2 O 0.4805(9) 0.2784(5) 0.0635(7) 0.050(3) Uani 1 1 d . . . O3 O 0.0282(8) 0.2649(7) 0.0342(7) 0.063(3) Uani 1 1 d . . . O4 O 0.0446(7) 0.2617(5) -0.1056(6) 0.040(2) Uani 1 1 d . . . O5 O 0.2522(10) 0.5637(5) 0.0034(8) 0.074(4) Uani 1 1 d . . . O6 O 0.2619(7) 0.5106(5) -0.1206(7) 0.050(2) Uani 1 1 d . . . O7 O 0.6260(9) 0.1787(5) -0.0321(7) 0.054(3) Uani 1 1 d . . . O8 O 0.7470(7) 0.1384(6) 0.1455(8) 0.049(3) Uani 1 1 d . . . O9 O 0.6421(7) 0.2063(5) 0.2699(7) 0.047(2) Uani 1 1 d . . . O10 O 0.4005(10) 0.3429(7) 0.4686(8) 0.072(4) Uani 1 1 d . . . O11 O 0.2813(8) 0.3753(5) 0.2775(8) 0.053(3) Uani 1 1 d . . . O12 O 0.4603(12) 0.6809(8) 0.3942(10) 0.086(4) Uani 1 1 d . . . O13 O 0.3037(11) 0.6155(8) 0.3147(9) 0.087(4) Uani 1 1 d . . . O14 O 0.1080(11) 0.6862(8) 0.7077(8) 0.083(4) Uani 1 1 d . . . O15 O 0.3350(14) 0.8213(10) 0.3341(13) 0.108(5) Uani 1 1 d . . . O16 O 0.4113(15) 0.9177(9) 0.3217(13) 0.114(5) Uani 1 1 d . . . O17 O 0.4736(12) 0.8129(11) 0.3183(9) 0.110(6) Uani 1 1 d . . . N1 N 0.7116(11) 0.3082(6) 0.1048(9) 0.045(3) Uani 1 1 d . . . N2 N 1.0149(10) 0.6055(6) 0.1052(9) 0.047(3) Uani 1 1 d . . . N3 N 0.3230(10) 0.2028(5) 0.3285(9) 0.041(3) Uani 1 1 d . . . N4 N 0.0146(10) -0.0976(6) 0.3244(9) 0.045(3) Uani 1 1 d . . . N5 N 0.4080(15) 0.8537(10) 0.3260(10) 0.074(4) Uani 1 1 d . . . C1 C 0.4261(10) 0.2909(5) 0.1129(9) 0.032(3) Uani 1 1 d . . . C2 C 0.3312(10) 0.3290(6) 0.0686(8) 0.038(3) Uani 1 1 d . . . C3 C 0.2482(10) 0.2902(6) 0.0475(8) 0.037(3) Uani 1 1 d . . . C4 C 0.2409(10) 0.2106(7) 0.0726(11) 0.047(4) Uani 1 1 d . . . H4A H 0.1765 0.1945 0.0516 0.071 Uiso 1 1 calc R . . H4B H 0.2602 0.2054 0.1365 0.071 Uiso 1 1 calc R . . H4C H 0.2817 0.1821 0.0455 0.071 Uiso 1 1 calc R . . C5 C 0.1613(10) 0.3247(7) 0.0016(8) 0.035(3) Uani 1 1 d . . . C6 C 0.0670(10) 0.2817(7) -0.0242(8) 0.039(3) Uani 1 1 d . . . C7 C 0.1610(10) 0.3968(6) -0.0234(8) 0.037(3) Uani 1 1 d . . . C8 C 0.0703(13) 0.4344(8) -0.0701(11) 0.058(4) Uani 1 1 d . . . H8A H 0.0840 0.4835 -0.0818 0.087 Uiso 1 1 calc R . . H8B H 0.0262 0.4332 -0.0325 0.087 Uiso 1 1 calc R . . H8C H 0.0430 0.4104 -0.1255 0.087 Uiso 1 1 calc R . . C9 C 0.2476(10) 0.4340(6) -0.0032(8) 0.037(3) Uani 1 1 d . . . C10 C 0.2548(12) 0.5081(7) -0.0422(10) 0.047(4) Uani 1 1 d . . . C11 C 0.3332(9) 0.4009(7) 0.0447(8) 0.036(3) Uani 1 1 d . . . C12 C 0.4268(11) 0.4440(7) 0.0687(12) 0.058(4) Uani 1 1 d . . . H12A H 0.4152 0.4925 0.0473 0.088 Uiso 1 1 calc R . . H12B H 0.4726 0.4219 0.0414 0.088 Uiso 1 1 calc R . . H12C H 0.4510 0.4446 0.1325 0.088 Uiso 1 1 calc R . . C13 C 0.6781(10) 0.3761(7) 0.0950(9) 0.040(3) Uiso 1 1 d . . . H13 H 0.6138 0.3839 0.0907 0.048 Uiso 1 1 calc R . . C14 C 0.7361(11) 0.4345(7) 0.0911(12) 0.057(4) Uani 1 1 d . . . H14 H 0.7105 0.4807 0.0848 0.069 Uiso 1 1 calc R . . C15 C 0.8300(10) 0.4249(7) 0.0964(10) 0.040(3) Uani 1 1 d . . . C16 C 0.8616(11) 0.3553(7) 0.1027(11) 0.046(4) Uani 1 1 d . . . H16 H 0.9252 0.3464 0.1046 0.055 Uiso 1 1 calc R . . C17 C 0.8039(12) 0.2996(7) 0.1062(10) 0.038(4) Uiso 1 1 d . . . H17 H 0.8287 0.2532 0.1097 0.045 Uiso 1 1 calc R . . C18 C 0.8938(10) 0.4869(7) 0.0974(9) 0.038(3) Uani 1 1 d . . . C19 C 0.8720(11) 0.5451(7) 0.0400(9) 0.046(3) Uani 1 1 d . . . H19 H 0.8145 0.5459 -0.0029 0.055 Uiso 1 1 calc R . . C20 C 0.9347(10) 0.6025(7) 0.0454(9) 0.041(3) Uani 1 1 d . . . H20 H 0.9185 0.6402 0.0048 0.049 Uiso 1 1 calc R . . C21 C 1.0414(9) 0.5492(7) 0.1602(11) 0.045(4) Uani 1 1 d . . . H21 H 1.0997 0.5507 0.2019 0.054 Uiso 1 1 calc R . . C22 C 0.9842(12) 0.4889(8) 0.1567(11) 0.056(4) Uani 1 1 d . . . H22 H 1.0057 0.4498 0.1936 0.068 Uiso 1 1 calc R . . C23 C 0.3379(9) 0.1393(7) 0.2984(9) 0.038(3) Uani 1 1 d . . . H23 H 0.3922 0.1357 0.2765 0.046 Uiso 1 1 calc R . . C24 C 0.2875(12) 0.0788(7) 0.2941(10) 0.051(4) Uani 1 1 d . . . H24 H 0.3063 0.0362 0.2716 0.061 Uiso 1 1 calc R . . C25 C 0.2010(11) 0.0832(7) 0.3269(9) 0.040(3) Uani 1 1 d . . . C26 C 0.1833(12) 0.1494(7) 0.3614(10) 0.047(4) Uani 1 1 d . . . H26 H 0.1300 0.1540 0.3846 0.057 Uiso 1 1 calc R . . C27 C 0.2397(8) 0.2075(6) 0.3628(11) 0.035(3) Uani 1 1 d . . . H27 H 0.2244 0.2508 0.3862 0.042 Uiso 1 1 calc R . . C28 C 0.1397(10) 0.0206(7) 0.3242(10) 0.037(3) Uani 1 1 d . . . C29 C 0.1696(11) -0.0496(7) 0.3194(10) 0.044(3) Uani 1 1 d . . . H29 H 0.2318 -0.0589 0.3164 0.053 Uiso 1 1 calc R . . C30 C 0.1073(9) -0.1064(7) 0.3190(8) 0.035(3) Uiso 1 1 d . . . H30 H 0.1294 -0.1530 0.3149 0.041 Uiso 1 1 calc R . . C31 C -0.0132(10) -0.0308(7) 0.3277(13) 0.057(4) Uani 1 1 d . . . H31 H -0.0761 -0.0226 0.3291 0.068 Uiso 1 1 calc R . . C32 C 0.0452(11) 0.0288(7) 0.3293(12) 0.055(4) Uani 1 1 d . . . H32 H 0.0212 0.0747 0.3339 0.067 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 Cd1 0.0334(5) 0.0237(4) 0.0414(5) 0.0021(4) 0.0044(4) -0.0038(4) Cd2 0.0343(5) 0.0219(4) 0.0475(6) -0.0007(4) 0.0064(4) -0.0058(4) O1 0.066(7) 0.040(5) 0.042(6) -0.001(4) 0.006(5) 0.025(5) O2 0.070(8) 0.032(5) 0.046(6) 0.002(4) 0.010(5) 0.018(5) O3 0.053(7) 0.095(9) 0.037(5) -0.014(5) 0.005(5) -0.025(6) O4 0.041(6) 0.039(5) 0.034(5) -0.005(4) -0.003(4) -0.011(4) O5 0.118(11) 0.032(5) 0.072(8) -0.007(5) 0.023(7) 0.030(6) O6 0.041(6) 0.048(6) 0.069(7) 0.007(5) 0.025(5) 0.014(5) O7 0.087(9) 0.036(5) 0.041(5) -0.004(4) 0.022(5) -0.003(5) O8 0.032(6) 0.050(6) 0.069(7) 0.002(5) 0.016(5) 0.013(5) O9 0.027(5) 0.066(7) 0.057(6) 0.007(5) 0.030(5) 0.018(4) O10 0.071(9) 0.089(10) 0.055(7) -0.004(6) 0.016(6) -0.006(7) O11 0.036(6) 0.033(5) 0.081(8) -0.008(5) -0.003(5) 0.001(4) O12 0.096(12) 0.075(9) 0.088(10) -0.008(7) 0.024(8) -0.009(8) O13 0.104(11) 0.094(10) 0.066(8) 0.026(7) 0.027(7) 0.034(8) O14 0.081(10) 0.110(11) 0.050(6) 0.020(7) -0.002(6) 0.014(8) O15 0.084(13) 0.102(12) 0.137(15) 0.004(10) 0.026(11) 0.006(10) O16 0.131(15) 0.095(11) 0.127(14) 0.014(12) 0.056(11) 0.001(13) O17 0.086(12) 0.184(18) 0.059(8) 0.006(9) 0.013(8) 0.066(12) N1 0.062(10) 0.026(6) 0.045(7) 0.003(5) 0.012(7) -0.003(5) N2 0.059(9) 0.029(6) 0.049(7) 0.001(5) 0.006(7) -0.018(5) N3 0.045(8) 0.022(5) 0.044(7) 0.001(4) -0.010(6) -0.007(5) N4 0.049(8) 0.020(5) 0.064(8) -0.002(5) 0.012(6) -0.001(5) N5 0.075(11) 0.098(12) 0.049(8) -0.006(9) 0.018(7) 0.021(12) C1 0.037(8) 0.011(5) 0.044(8) -0.005(5) 0.002(6) 0.004(5) C2 0.048(8) 0.029(6) 0.030(6) -0.004(5) 0.000(6) -0.008(6) C3 0.052(9) 0.028(6) 0.028(6) -0.004(5) 0.004(6) 0.005(5) C4 0.026(7) 0.032(7) 0.081(11) 0.005(6) 0.009(7) 0.001(5) C5 0.043(8) 0.037(6) 0.026(6) -0.008(5) 0.007(5) 0.004(6) C6 0.046(9) 0.044(7) 0.028(7) 0.001(5) 0.013(6) -0.002(6) C7 0.048(8) 0.030(6) 0.031(6) -0.005(5) 0.006(6) 0.002(6) C8 0.066(12) 0.043(8) 0.055(9) 0.004(7) -0.006(8) 0.010(8) C9 0.048(9) 0.028(6) 0.034(7) -0.003(5) 0.006(6) -0.001(6) C10 0.054(9) 0.031(7) 0.052(10) 0.002(6) 0.003(7) 0.016(6) C11 0.027(7) 0.034(6) 0.043(7) -0.001(5) -0.001(5) 0.009(5) C12 0.035(8) 0.031(7) 0.096(13) 0.000(7) -0.009(8) -0.004(6) C14 0.043(9) 0.024(7) 0.095(12) -0.004(7) -0.004(8) -0.004(6) C15 0.029(8) 0.033(7) 0.055(8) -0.004(6) 0.005(6) -0.008(6) C16 0.034(8) 0.031(7) 0.077(10) 0.004(6) 0.021(7) -0.005(6) C18 0.045(8) 0.029(6) 0.042(7) -0.001(5) 0.018(6) -0.003(6) C19 0.047(9) 0.035(7) 0.048(8) -0.004(6) -0.005(7) -0.005(6) C20 0.048(9) 0.035(7) 0.038(7) 0.001(5) 0.006(6) 0.007(6) C21 0.014(6) 0.045(8) 0.074(10) 0.007(7) 0.006(6) -0.004(6) C22 0.066(11) 0.034(7) 0.062(10) 0.015(7) 0.002(9) -0.002(7) C23 0.025(7) 0.040(7) 0.051(8) -0.002(6) 0.011(6) 0.003(5) C24 0.073(12) 0.020(6) 0.055(9) -0.004(6) 0.009(8) -0.002(6) C25 0.047(9) 0.028(6) 0.041(7) -0.001(5) 0.001(7) -0.001(6) C26 0.052(10) 0.030(7) 0.061(9) -0.007(6) 0.016(8) 0.000(6) C27 0.001(6) 0.033(6) 0.070(10) -0.005(6) 0.007(6) -0.001(4) C28 0.035(7) 0.028(6) 0.050(8) 0.000(5) 0.013(6) -0.007(5) C29 0.040(8) 0.030(7) 0.065(9) -0.004(6) 0.014(7) -0.011(6) C31 0.023(7) 0.036(7) 0.116(14) -0.011(8) 0.025(8) -0.015(6) C32 0.044(9) 0.026(7) 0.097(12) -0.015(7) 0.019(9) 0.008(6) _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 Cd1 O2 2.274(11) . ? Cd1 O9 2.295(10) . ? Cd1 O8 2.317(10) . ? Cd1 N2 2.364(11) 3_445 ? Cd1 N1 2.376(13) . ? Cd1 O7 2.416(10) . ? Cd2 O11 2.277(10) . ? Cd2 O1 2.306(9) . ? Cd2 O4 2.311(9) 4 ? Cd2 N4 2.325(12) 3 ? Cd2 N3 2.322(11) . ? Cd2 O10 2.331(12) . ? O1 C1 1.242(16) . ? O2 C1 1.242(18) . ? O3 C6 1.211(17) . ? O4 C6 1.271(15) . ? O4 Cd2 2.311(9) 4_454 ? O5 C10 1.254(16) . ? O6 C10 1.238(18) . ? O15 N5 1.25(2) . ? O16 N5 1.19(2) . ? O17 N5 1.24(2) . ? N1 C13 1.347(17) . ? N1 C17 1.34(2) . ? N2 C20 1.299(19) . ? N2 C21 1.341(18) . ? N2 Cd1 2.364(11) 3 ? N3 C23 1.305(17) . ? N3 C27 1.43(2) . ? N4 C31 1.310(18) . ? N4 C30 1.377(18) . ? N4 Cd2 2.325(12) 3_445 ? C1 C2 1.551(19) . ? C2 C3 1.373(19) . ? C2 C11 1.388(17) . ? C3 C5 1.437(19) . ? C3 C4 1.539(17) . ? C5 C7 1.394(18) . ? C5 C6 1.550(19) . ? C7 C9 1.401(19) . ? C7 C8 1.51(2) . ? C9 C11 1.421(18) . ? C9 C10 1.516(18) . ? C11 C12 1.543(19) . ? C13 C14 1.38(2) . ? C14 C15 1.36(2) . ? C15 C16 1.367(19) . ? C15 C18 1.475(18) . ? C16 C17 1.34(2) . ? C18 C19 1.383(19) . ? C18 C22 1.41(2) . ? C19 C20 1.39(2) . ? C21 C22 1.39(2) . ? C23 C24 1.334(19) . ? C24 C25 1.46(2) . ? C25 C26 1.389(19) . ? C25 C28 1.457(17) . ? C26 C27 1.352(19) . ? C28 C29 1.382(19) . ? C28 C32 1.40(2) . ? C29 C30 1.388(18) . ? C31 C32 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O9 108.7(3) . . ? O2 Cd1 O8 170.3(4) . . ? O9 Cd1 O8 81.0(4) . . ? O2 Cd1 N2 90.4(4) . 3_445 ? O9 Cd1 N2 91.2(4) . 3_445 ? O8 Cd1 N2 90.6(5) . 3_445 ? O2 Cd1 N1 90.5(5) . . ? O9 Cd1 N1 97.2(4) . . ? O8 Cd1 N1 87.0(4) . . ? N2 Cd1 N1 170.8(5) 3_445 . ? O2 Cd1 O7 92.8(4) . . ? O9 Cd1 O7 158.3(4) . . ? O8 Cd1 O7 77.6(4) . . ? N2 Cd1 O7 85.7(4) 3_445 . ? N1 Cd1 O7 85.1(4) . . ? O11 Cd2 O1 99.7(4) . . ? O11 Cd2 O4 173.2(4) . 4 ? O1 Cd2 O4 87.1(3) . 4 ? O11 Cd2 N4 92.4(4) . 3 ? O1 Cd2 N4 87.7(4) . 3 ? O4 Cd2 N4 88.3(4) 4 3 ? O11 Cd2 N3 92.4(4) . . ? O1 Cd2 N3 89.3(5) . . ? O4 Cd2 N3 87.2(4) 4 . ? N4 Cd2 N3 174.7(5) 3 . ? O11 Cd2 O10 84.2(5) . . ? O1 Cd2 O10 175.0(4) . . ? O4 Cd2 O10 89.0(4) 4 . ? N4 Cd2 O10 89.0(5) 3 . ? N3 Cd2 O10 93.6(5) . . ? C1 O1 Cd2 140.8(8) . . ? C1 O2 Cd1 119.0(8) . . ? C6 O4 Cd2 126.0(9) . 4_454 ? C13 N1 C17 116.3(13) . . ? C13 N1 Cd1 121.5(12) . . ? C17 N1 Cd1 122.1(9) . . ? C20 N2 C21 119.1(12) . . ? C20 N2 Cd1 120.0(9) . 3 ? C21 N2 Cd1 121.0(10) . 3 ? C23 N3 C27 114.4(12) . . ? C23 N3 Cd2 126.9(12) . . ? C27 N3 Cd2 118.6(8) . . ? C31 N4 C30 115.4(12) . . ? C31 N4 Cd2 121.8(10) . 3_445 ? C30 N4 Cd2 122.8(8) . 3_445 ? O16 N5 O15 122(2) . . ? O16 N5 O17 124(2) . . ? O15 N5 O17 113.7(19) . . ? O2 C1 O1 124.6(12) . . ? O2 C1 C2 116.4(12) . . ? O1 C1 C2 118.8(13) . . ? C3 C2 C11 121.0(12) . . ? C3 C2 C1 120.0(10) . . ? C11 C2 C1 118.8(11) . . ? C2 C3 C5 119.8(11) . . ? C2 C3 C4 123.6(12) . . ? C5 C3 C4 116.5(12) . . ? C7 C5 C3 120.5(12) . . ? C7 C5 C6 118.7(12) . . ? C3 C5 C6 120.7(11) . . ? O3 C6 O4 127.1(13) . . ? O3 C6 C5 118.7(11) . . ? O4 C6 C5 113.8(11) . . ? C5 C7 C9 118.0(12) . . ? C5 C7 C8 121.4(13) . . ? C9 C7 C8 120.7(12) . . ? C7 C9 C11 121.7(11) . . ? C7 C9 C10 120.2(12) . . ? C11 C9 C10 117.6(12) . . ? O6 C10 O5 122.4(14) . . ? O6 C10 C9 116.7(11) . . ? O5 C10 C9 120.8(14) . . ? C2 C11 C9 118.9(12) . . ? C2 C11 C12 120.7(11) . . ? C9 C11 C12 120.5(11) . . ? N1 C13 C14 122.3(15) . . ? C15 C14 C13 120.4(13) . . ? C14 C15 C16 116.3(13) . . ? C14 C15 C18 121.0(12) . . ? C16 C15 C18 122.7(14) . . ? C17 C16 C15 122.1(15) . . ? C16 C17 N1 122.5(14) . . ? C19 C18 C22 115.3(12) . . ? C19 C18 C15 123.9(13) . . ? C22 C18 C15 120.8(12) . . ? C18 C19 C20 121.1(13) . . ? N2 C20 C19 122.4(12) . . ? N2 C21 C22 121.8(13) . . ? C21 C22 C18 120.2(13) . . ? N3 C23 C24 130.0(15) . . ? C23 C24 C25 116.2(13) . . ? C26 C25 C28 123.3(15) . . ? C26 C25 C24 115.8(13) . . ? C28 C25 C24 120.9(12) . . ? C27 C26 C25 123.1(15) . . ? C26 C27 N3 120.4(12) . . ? C29 C28 C32 115.4(12) . . ? C29 C28 C25 123.9(13) . . ? C32 C28 C25 120.7(12) . . ? C28 C29 C30 120.4(14) . . ? N4 C30 C29 123.6(13) . . ? N4 C31 C32 124.3(14) . . ? C31 C32 C28 120.9(12) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 24.74 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.327 _refine_diff_density_min -1.997 _refine_diff_density_rms 0.204