# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Gan Li,' _publ_contact_author_email gangli@zzu.edu.cn _publ_section_title ; 2-Phenyl-4,5-imidazole dicarboxylate-based metal-organic frameworks assembled under hydro(solvo)thermal conditions ; loop_ _publ_author_name 'wenyue wang' 'Zeli Yang' 'Chengjie Wang' 'huijie lu' 'Shuangquan Zang' ; Gang Li ; data_a _database_code_depnum_ccdc_archive 'CCDC 809968' #TrackingRef '- complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H28 Cd2 N8 O8' _chemical_formula_weight 1045.56 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 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 10.5015(3) _cell_length_b 19.8003(4) _cell_length_c 21.2490(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.696(2) _cell_angle_gamma 90.00 _cell_volume 4292.73(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5338 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7289 _exptl_absorpt_correction_T_max 0.8328 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18448 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7677 _reflns_number_gt 5775 _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. 71 restrains were used to restrain the Uij of atoms C6, C7, C8, C9, C10, C11, C24, C25, C26, C27, C30, and C37. To do these restrains, these atoms may have reasonable displacement parameters. ; _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^)+(0.0568P)^2^+7.3778P] 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 7677 _refine_ls_number_parameters 566 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.044 _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 Cd1 Cd 1.08955(4) 0.36325(2) 0.182935(19) 0.04894(14) Uani 1 1 d . . . Cd2 Cd 0.77311(4) 0.070072(19) 0.176875(18) 0.04435(13) Uani 1 1 d . . . O1 O 0.9351(4) 0.0612(2) 0.27948(18) 0.0603(11) Uani 1 1 d . . . O2 O 1.1007(4) 0.1159(2) 0.34310(17) 0.0598(11) Uani 1 1 d . . . H2 H 1.1395 0.1518 0.3425 0.090 Uiso 1 1 calc R . . O3 O 1.2369(4) 0.2160(2) 0.33508(18) 0.0654(11) Uani 1 1 d . . . O4 O 1.2284(4) 0.3061(2) 0.2712(2) 0.0664(12) Uani 1 1 d . . . O5 O 1.2298(4) 0.4574(2) 0.20938(19) 0.0571(10) Uani 1 1 d . . . O6 O 1.2421(4) 0.5610(2) 0.2486(2) 0.0625(11) Uani 1 1 d . . . H6 H 1.1894 0.5898 0.2539 0.094 Uiso 1 1 calc R . . O7 O 1.1036(4) 0.64091(19) 0.2907(2) 0.0607(11) Uani 1 1 d . . . O8 O 0.9174(4) 0.63904(19) 0.3219(2) 0.0596(11) Uani 1 1 d . . . N1 N 1.0013(4) 0.2596(2) 0.1883(2) 0.0455(10) Uani 1 1 d . . . N2 N 0.8930(4) 0.1635(2) 0.18933(19) 0.0414(10) Uani 1 1 d . . . N3 N 0.9916(4) 0.4350(2) 0.2419(2) 0.0438(10) Uani 1 1 d . . . N4 N 0.8679(4) 0.5077(2) 0.28196(19) 0.0407(10) Uani 1 1 d . . . N5 N 1.1856(6) 0.3204(3) 0.1026(3) 0.0639(14) Uani 1 1 d . . . N6 N 0.9800(5) 0.4082(3) 0.0820(3) 0.0655(14) Uani 1 1 d . . . N7 N 0.8997(4) -0.0043(2) 0.1303(2) 0.0447(10) Uani 1 1 d . . . N8 N 0.6863(4) 0.0637(2) 0.0636(2) 0.0492(11) Uani 1 1 d . . . C1 C 0.9007(5) 0.2222(2) 0.1585(2) 0.0386(11) Uani 1 1 d . . . C2 C 0.9963(5) 0.1646(3) 0.2428(2) 0.0399(11) Uani 1 1 d . . . C3 C 1.0634(5) 0.2237(3) 0.2417(2) 0.0420(12) Uani 1 1 d . . . C4 C 1.0106(6) 0.1099(3) 0.2904(3) 0.0493(13) Uani 1 1 d . . . C5 C 1.1844(6) 0.2510(3) 0.2851(3) 0.0562(15) Uani 1 1 d . . . C6 C 0.8096(4) 0.2439(2) 0.09869(14) 0.0480(12) Uani 1 1 d GU . . C7 C 0.7032(5) 0.2850(3) 0.10029(18) 0.092(2) Uani 1 1 d GU . . H7 H 0.6870 0.2977 0.1398 0.111 Uiso 1 1 calc R . . C8 C 0.6210(4) 0.3073(3) 0.0428(2) 0.106(2) Uani 1 1 d GU . . H8 H 0.5499 0.3349 0.0439 0.128 Uiso 1 1 calc R . . C9 C 0.6453(5) 0.2884(3) -0.01628(18) 0.091(2) Uani 1 1 d GU . . H9 H 0.5903 0.3033 -0.0547 0.109 Uiso 1 1 calc R . . C10 C 0.7517(6) 0.2473(3) -0.01788(14) 0.105(2) Uani 1 1 d GU . . H10 H 0.7679 0.2346 -0.0574 0.126 Uiso 1 1 calc R . . C11 C 0.8338(5) 0.2250(3) 0.03960(18) 0.091(2) Uani 1 1 d GU . . H11 H 0.9050 0.1974 0.0385 0.109 Uiso 1 1 calc R . . C12 C 0.8806(5) 0.4438(3) 0.2615(2) 0.0418(12) Uani 1 1 d . . . C13 C 1.0542(5) 0.4961(3) 0.2507(2) 0.0430(12) Uani 1 1 d . . . C14 C 0.9776(5) 0.5405(2) 0.2754(2) 0.0392(11) Uani 1 1 d . . . C15 C 1.1828(5) 0.5045(3) 0.2345(3) 0.0472(13) Uani 1 1 d . . . C16 C 0.9992(6) 0.6118(3) 0.2971(3) 0.0481(13) Uani 1 1 d . . . C17 C 0.7874(6) 0.3886(3) 0.2630(3) 0.0509(14) Uani 1 1 d . . . C18 C 0.8300(7) 0.3265(3) 0.2880(3) 0.0611(16) Uani 1 1 d . . . H18 H 0.9191 0.3189 0.3045 0.073 Uiso 1 1 calc R . . C19 C 0.7410(9) 0.2753(4) 0.2888(4) 0.081(2) Uani 1 1 d . . . H19 H 0.7709 0.2332 0.3054 0.097 Uiso 1 1 calc R . . C20 C 0.6094(9) 0.2856(4) 0.2654(4) 0.086(3) Uani 1 1 d . . . H20 H 0.5500 0.2511 0.2666 0.104 Uiso 1 1 calc R . . C21 C 0.5663(7) 0.3472(4) 0.2405(4) 0.081(2) Uani 1 1 d . . . H21 H 0.4769 0.3542 0.2244 0.097 Uiso 1 1 calc R . . C22 C 0.6527(6) 0.3994(3) 0.2385(3) 0.0667(17) Uani 1 1 d . . . H22 H 0.6220 0.4411 0.2212 0.080 Uiso 1 1 calc R . . C23 C 1.2812(8) 0.2741(4) 0.1130(5) 0.091(2) Uani 1 1 d . . . H23 H 1.3230 0.2626 0.1552 0.109 Uiso 1 1 calc R . . C24 C 1.3185(13) 0.2435(6) 0.0627(6) 0.143(4) Uani 1 1 d U . . H24 H 1.3859 0.2119 0.0708 0.171 Uiso 1 1 calc R . . C25 C 1.2570(14) 0.2593(7) 0.0009(6) 0.147(3) Uani 1 1 d U . . H25 H 1.2835 0.2384 -0.0331 0.176 Uiso 1 1 calc R . . C26 C 1.1556(13) 0.3057(6) -0.0130(5) 0.131(3) Uani 1 1 d U . . C27 C 1.0847(16) 0.3237(7) -0.0759(6) 0.153(4) Uani 1 1 d U . . H27 H 1.1056 0.3029 -0.1114 0.183 Uiso 1 1 calc R . . C28 C 0.9907(14) 0.3685(7) -0.0859(4) 0.144(5) Uani 1 1 d . . . H28 H 0.9496 0.3806 -0.1281 0.173 Uiso 1 1 calc R . . C29 C 0.9501(12) 0.3992(6) -0.0333(4) 0.108(3) Uani 1 1 d . . . C30 C 0.8501(13) 0.4445(7) -0.0410(6) 0.137(6) Uani 1 1 d . . . H30 H 0.8065 0.4570 -0.0828 0.164 Uiso 1 1 calc R . . C31 C 0.8110(10) 0.4727(5) 0.0110(6) 0.122(4) Uani 1 1 d . . . H31 H 0.7426 0.5037 0.0057 0.147 Uiso 1 1 calc R . . C32 C 0.8814(8) 0.4515(4) 0.0722(4) 0.090(2) Uani 1 1 d . . . H32 H 0.8573 0.4689 0.1084 0.108 Uiso 1 1 calc R . . C33 C 1.0174(8) 0.3821(4) 0.0304(3) 0.073(2) Uani 1 1 d . . . C34 C 1.1225(8) 0.3356(4) 0.0413(3) 0.073(2) Uani 1 1 d . . . C35 C 1.0055(6) -0.0380(3) 0.1626(3) 0.0556(15) Uani 1 1 d . . . H35 H 1.0390 -0.0277 0.2061 0.067 Uiso 1 1 calc R . . C36 C 1.0675(7) -0.0873(4) 0.1347(3) 0.0708(19) Uani 1 1 d . . . H36 H 1.1396 -0.1102 0.1592 0.085 Uiso 1 1 calc R . . C37 C 1.0218(8) -0.1016(4) 0.0712(4) 0.083(2) Uani 1 1 d . . . H37 H 1.0615 -0.1353 0.0520 0.099 Uiso 1 1 calc R . . C38 C 0.9143(7) -0.0659(3) 0.0338(3) 0.0647(17) Uani 1 1 d . . . C39 C 0.8634(8) -0.0768(4) -0.0337(3) 0.080(2) Uani 1 1 d . . . H39 H 0.9002 -0.1100 -0.0548 0.095 Uiso 1 1 calc R . . C40 C 0.7634(8) -0.0400(4) -0.0670(3) 0.078(2) Uani 1 1 d . . . H40 H 0.7344 -0.0469 -0.1114 0.094 Uiso 1 1 calc R . . C41 C 0.7001(6) 0.0092(3) -0.0367(3) 0.0599(16) Uani 1 1 d . . . C42 C 0.5940(7) 0.0486(4) -0.0691(3) 0.075(2) Uani 1 1 d . . . H42 H 0.5635 0.0443 -0.1138 0.090 Uiso 1 1 calc R . . C43 C 0.5359(7) 0.0921(4) -0.0369(3) 0.077(2) Uani 1 1 d . . . H43 H 0.4647 0.1177 -0.0586 0.092 Uiso 1 1 calc R . . C44 C 0.5844(7) 0.0988(4) 0.0306(3) 0.0689(18) Uani 1 1 d . . . H44 H 0.5433 0.1289 0.0529 0.083 Uiso 1 1 calc R . . C45 C 0.7429(5) 0.0196(3) 0.0304(2) 0.0451(12) Uani 1 1 d . . . C46 C 0.8553(5) -0.0179(3) 0.0664(3) 0.0460(13) 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 Cd1 0.0557(3) 0.0416(2) 0.0477(2) -0.00434(17) 0.00854(19) -0.00346(19) Cd2 0.0465(2) 0.0400(2) 0.0447(2) -0.00233(16) 0.00713(18) -0.00293(18) O1 0.073(3) 0.050(2) 0.052(2) 0.0092(18) 0.003(2) -0.008(2) O2 0.071(3) 0.062(3) 0.037(2) 0.0023(18) -0.006(2) 0.000(2) O3 0.069(3) 0.065(3) 0.048(2) -0.001(2) -0.015(2) -0.006(2) O4 0.065(3) 0.053(3) 0.067(3) -0.005(2) -0.013(2) -0.014(2) O5 0.052(2) 0.054(2) 0.068(3) -0.011(2) 0.022(2) -0.010(2) O6 0.054(2) 0.052(2) 0.089(3) -0.012(2) 0.030(2) -0.012(2) O7 0.064(3) 0.039(2) 0.084(3) -0.0052(19) 0.027(2) -0.013(2) O8 0.061(3) 0.039(2) 0.082(3) -0.0059(19) 0.025(2) -0.003(2) N1 0.047(3) 0.044(2) 0.041(2) -0.0034(19) 0.001(2) -0.008(2) N2 0.046(3) 0.038(2) 0.037(2) -0.0014(18) 0.003(2) -0.003(2) N3 0.050(3) 0.036(2) 0.046(2) -0.0065(19) 0.015(2) -0.008(2) N4 0.042(2) 0.036(2) 0.044(2) 0.0004(18) 0.010(2) -0.0017(19) N5 0.079(4) 0.049(3) 0.067(3) -0.008(2) 0.023(3) -0.011(3) N6 0.065(4) 0.049(3) 0.073(4) 0.015(3) -0.003(3) -0.009(3) N7 0.040(2) 0.048(3) 0.042(2) -0.001(2) 0.003(2) 0.003(2) N8 0.046(3) 0.049(3) 0.048(3) 0.000(2) 0.000(2) 0.006(2) C1 0.039(3) 0.039(3) 0.033(2) -0.006(2) 0.000(2) -0.003(2) C2 0.042(3) 0.043(3) 0.031(2) -0.004(2) 0.002(2) 0.001(2) C3 0.047(3) 0.039(3) 0.035(3) -0.008(2) -0.001(2) -0.002(2) C4 0.061(4) 0.043(3) 0.042(3) -0.004(2) 0.008(3) 0.002(3) C5 0.057(4) 0.057(4) 0.048(3) -0.011(3) 0.000(3) -0.005(3) C6 0.055(3) 0.043(3) 0.041(3) 0.007(2) 0.004(2) -0.002(2) C7 0.083(4) 0.121(5) 0.065(3) 0.008(4) 0.002(3) 0.044(4) C8 0.090(5) 0.133(6) 0.084(4) 0.024(4) -0.004(4) 0.042(4) C9 0.089(5) 0.111(5) 0.059(3) 0.036(4) -0.011(3) -0.002(4) C10 0.127(6) 0.131(6) 0.045(3) 0.009(4) -0.003(4) 0.026(5) C11 0.112(5) 0.110(5) 0.043(3) -0.001(3) 0.002(3) 0.040(4) C12 0.046(3) 0.037(3) 0.042(3) -0.001(2) 0.010(2) -0.004(2) C13 0.044(3) 0.047(3) 0.036(3) 0.000(2) 0.008(2) -0.006(3) C14 0.044(3) 0.033(3) 0.039(3) 0.001(2) 0.005(2) -0.006(2) C15 0.050(3) 0.047(3) 0.044(3) 0.004(2) 0.009(3) -0.010(3) C16 0.053(4) 0.037(3) 0.052(3) 0.004(2) 0.009(3) -0.001(3) C17 0.060(4) 0.043(3) 0.054(3) -0.013(3) 0.022(3) -0.015(3) C18 0.080(4) 0.039(3) 0.073(4) -0.007(3) 0.036(4) -0.013(3) C19 0.120(7) 0.049(4) 0.091(5) -0.010(3) 0.058(5) -0.013(4) C20 0.110(7) 0.052(4) 0.117(6) -0.033(4) 0.067(5) -0.038(4) C21 0.062(4) 0.069(5) 0.119(6) -0.030(4) 0.038(4) -0.027(4) C22 0.056(4) 0.061(4) 0.083(5) -0.020(3) 0.016(4) -0.017(3) C23 0.092(6) 0.067(5) 0.122(7) -0.016(5) 0.042(5) 0.007(4) C24 0.179(9) 0.114(7) 0.160(7) -0.043(7) 0.091(7) 0.013(6) C25 0.198(9) 0.133(7) 0.135(6) -0.055(6) 0.090(7) -0.010(6) C26 0.190(9) 0.130(7) 0.092(5) -0.043(5) 0.068(6) -0.035(6) C27 0.220(11) 0.162(9) 0.087(6) -0.046(6) 0.059(7) -0.044(8) C28 0.208(14) 0.169(12) 0.042(5) -0.012(6) 0.004(7) -0.082(10) C29 0.128(9) 0.110(8) 0.067(6) 0.022(5) -0.017(6) -0.052(7) C30 0.135(11) 0.140(11) 0.096(8) 0.055(8) -0.050(8) -0.077(9) C31 0.101(7) 0.095(7) 0.140(9) 0.054(7) -0.033(7) -0.011(6) C32 0.085(6) 0.077(5) 0.097(6) 0.016(4) 0.000(5) -0.006(5) C33 0.098(6) 0.072(5) 0.041(3) 0.001(3) 0.003(4) -0.045(4) C34 0.096(6) 0.062(4) 0.065(4) -0.019(3) 0.027(4) -0.025(4) C35 0.055(4) 0.062(4) 0.047(3) 0.006(3) 0.005(3) 0.010(3) C36 0.065(4) 0.076(5) 0.070(4) 0.012(4) 0.013(4) 0.032(4) C37 0.102(6) 0.068(5) 0.079(5) -0.012(4) 0.022(4) 0.039(4) C38 0.075(4) 0.058(4) 0.059(4) -0.008(3) 0.012(3) 0.016(3) C39 0.103(6) 0.074(5) 0.059(4) -0.021(3) 0.014(4) 0.021(4) C40 0.099(6) 0.087(5) 0.044(3) -0.021(3) 0.006(4) 0.004(5) C41 0.063(4) 0.066(4) 0.042(3) -0.007(3) -0.005(3) -0.006(3) C42 0.071(5) 0.096(6) 0.046(3) -0.002(4) -0.011(3) -0.005(4) C43 0.067(5) 0.090(5) 0.060(4) 0.011(4) -0.013(4) 0.018(4) C44 0.064(4) 0.073(4) 0.063(4) -0.001(3) 0.001(3) 0.017(4) C45 0.045(3) 0.043(3) 0.043(3) -0.002(2) 0.001(2) -0.007(2) C46 0.051(3) 0.039(3) 0.047(3) -0.003(2) 0.009(3) -0.001(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 Cd1 N1 2.265(4) . ? Cd1 N3 2.293(4) . ? Cd1 N5 2.339(5) . ? Cd1 N6 2.356(5) . ? Cd1 O5 2.359(4) . ? Cd1 O4 2.372(4) . ? Cd2 N2 2.219(4) . ? Cd2 N4 2.257(4) 2_645 ? Cd2 N7 2.354(4) . ? Cd2 N8 2.367(4) . ? Cd2 O8 2.427(4) 2_645 ? Cd2 O1 2.433(4) . ? O1 C4 1.236(7) . ? O2 C4 1.289(7) . ? O2 H2 0.8200 . ? O3 C5 1.279(7) . ? O4 C5 1.248(7) . ? O5 C15 1.234(7) . ? O6 C15 1.282(6) . ? O6 H6 0.8200 . ? O7 C16 1.275(6) . ? O8 C16 1.234(6) . ? O8 Cd2 2.427(4) 2_655 ? N1 C1 1.324(6) . ? N1 C3 1.366(6) . ? N2 C1 1.345(6) . ? N2 C2 1.372(6) . ? N3 C12 1.339(6) . ? N3 C13 1.367(6) . ? N4 C14 1.358(6) . ? N4 C12 1.355(6) . ? N4 Cd2 2.257(4) 2_655 ? N5 C34 1.347(9) . ? N5 C23 1.339(9) . ? N6 C32 1.321(9) . ? N6 C33 1.352(9) . ? N7 C35 1.338(7) . ? N7 C46 1.355(6) . ? N8 C44 1.327(7) . ? N8 C45 1.347(7) . ? C1 C6 1.462(6) . ? C2 C3 1.369(7) . ? C2 C4 1.466(7) . ? C3 C5 1.483(8) . ? C6 C7 1.3900 . ? C6 C11 1.3900 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.472(7) . ? C13 C14 1.377(7) . ? C13 C15 1.480(7) . ? C14 C16 1.485(7) . ? C17 C18 1.372(8) . ? C17 C22 1.403(9) . ? C18 C19 1.382(9) . ? C18 H18 0.9300 . ? C19 C20 1.369(11) . ? C19 H19 0.9300 . ? C20 C21 1.363(11) . ? C20 H20 0.9300 . ? C21 C22 1.384(9) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.364(12) . ? C23 H23 0.9300 . ? C24 C25 1.356(16) . ? C24 H24 0.9300 . ? C25 C26 1.385(16) . ? C25 H25 0.9300 . ? C26 C27 1.412(17) . ? C26 C34 1.413(11) . ? C27 C28 1.307(17) . ? C27 H27 0.9300 . ? C28 C29 1.422(16) . ? C28 H28 0.9300 . ? C29 C30 1.362(16) . ? C29 C33 1.413(10) . ? C30 C31 1.386(16) . ? C30 H30 0.9300 . ? C31 C32 1.400(12) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.413(11) . ? C35 C36 1.383(8) . ? C35 H35 0.9300 . ? C36 C37 1.351(9) . ? C36 H36 0.9300 . ? C37 C38 1.407(9) . ? C37 H37 0.9300 . ? C38 C46 1.402(8) . ? C38 C39 1.424(9) . ? C39 C40 1.335(10) . ? C39 H39 0.9300 . ? C40 C41 1.417(9) . ? C40 H40 0.9300 . ? C41 C42 1.400(9) . ? C41 C45 1.405(7) . ? C42 C43 1.336(10) . ? C42 H42 0.9300 . ? C43 C44 1.409(9) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.449(7) . ? 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 Cd1 N3 106.99(15) . . ? N1 Cd1 N5 87.71(16) . . ? N3 Cd1 N5 161.95(17) . . ? N1 Cd1 N6 105.73(16) . . ? N3 Cd1 N6 94.44(19) . . ? N5 Cd1 N6 71.0(2) . . ? N1 Cd1 O5 160.59(15) . . ? N3 Cd1 O5 73.47(14) . . ? N5 Cd1 O5 96.21(15) . . ? N6 Cd1 O5 93.50(16) . . ? N1 Cd1 O4 73.16(15) . . ? N3 Cd1 O4 97.75(16) . . ? N5 Cd1 O4 96.51(19) . . ? N6 Cd1 O4 167.53(19) . . ? O5 Cd1 O4 87.49(14) . . ? N2 Cd2 N4 144.68(14) . 2_645 ? N2 Cd2 N7 102.18(15) . . ? N4 Cd2 N7 107.95(15) 2_645 . ? N2 Cd2 N8 103.68(15) . . ? N4 Cd2 N8 103.61(15) 2_645 . ? N7 Cd2 N8 70.05(15) . . ? N2 Cd2 O8 88.59(14) . 2_645 ? N4 Cd2 O8 71.69(14) 2_645 2_645 ? N7 Cd2 O8 154.90(14) . 2_645 ? N8 Cd2 O8 85.46(15) . 2_645 ? N2 Cd2 O1 72.37(14) . . ? N4 Cd2 O1 89.80(14) 2_645 . ? N7 Cd2 O1 89.25(14) . . ? N8 Cd2 O1 157.90(15) . . ? O8 Cd2 O1 115.73(14) 2_645 . ? C4 O1 Cd2 113.2(3) . . ? C4 O2 H2 109.5 . . ? C5 O4 Cd1 114.3(4) . . ? C15 O5 Cd1 114.1(3) . . ? C15 O6 H6 109.5 . . ? C16 O8 Cd2 114.7(3) . 2_655 ? C1 N1 C3 106.0(4) . . ? C1 N1 Cd1 140.6(4) . . ? C3 N1 Cd1 113.1(3) . . ? C1 N2 C2 105.2(4) . . ? C1 N2 Cd2 139.4(3) . . ? C2 N2 Cd2 115.3(3) . . ? C12 N3 C13 105.6(4) . . ? C12 N3 Cd1 141.8(3) . . ? C13 N3 Cd1 111.1(3) . . ? C14 N4 C12 105.3(4) . . ? C14 N4 Cd2 115.3(3) . 2_655 ? C12 N4 Cd2 139.4(3) . 2_655 ? C34 N5 C23 119.4(6) . . ? C34 N5 Cd1 115.2(5) . . ? C23 N5 Cd1 124.4(5) . . ? C32 N6 C33 119.2(7) . . ? C32 N6 Cd1 125.7(5) . . ? C33 N6 Cd1 114.8(5) . . ? C35 N7 C46 117.6(5) . . ? C35 N7 Cd2 125.4(4) . . ? C46 N7 Cd2 116.8(3) . . ? C44 N8 C45 117.6(5) . . ? C44 N8 Cd2 125.3(4) . . ? C45 N8 Cd2 117.1(3) . . ? N1 C1 N2 112.5(4) . . ? N1 C1 C6 122.4(4) . . ? N2 C1 C6 125.1(4) . . ? C3 C2 N2 108.0(4) . . ? C3 C2 C4 132.4(5) . . ? N2 C2 C4 119.4(5) . . ? C2 C3 N1 108.2(4) . . ? C2 C3 C5 132.0(5) . . ? N1 C3 C5 119.8(5) . . ? O1 C4 O2 122.8(5) . . ? O1 C4 C2 119.4(5) . . ? O2 C4 C2 117.7(5) . . ? O4 C5 O3 124.0(5) . . ? O4 C5 C3 118.8(5) . . ? O3 C5 C3 117.2(5) . . ? C7 C6 C11 120.0 . . ? C7 C6 C1 121.0(3) . . ? C11 C6 C1 118.9(3) . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C6 120.0 . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? N3 C12 N4 112.3(4) . . ? N3 C12 C17 122.9(4) . . ? N4 C12 C17 124.7(5) . . ? N3 C13 C14 108.2(4) . . ? N3 C13 C15 120.2(5) . . ? C14 C13 C15 131.7(5) . . ? N4 C14 C13 108.6(4) . . ? N4 C14 C16 119.6(5) . . ? C13 C14 C16 131.7(5) . . ? O5 C15 O6 122.7(5) . . ? O5 C15 C13 119.8(5) . . ? O6 C15 C13 117.6(5) . . ? O8 C16 O7 123.5(5) . . ? O8 C16 C14 118.5(5) . . ? O7 C16 C14 117.9(5) . . ? C18 C17 C22 119.2(6) . . ? C18 C17 C12 121.0(6) . . ? C22 C17 C12 119.7(5) . . ? C17 C18 C19 120.2(7) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.9(7) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 119.3(7) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 121.4(7) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C21 C22 C17 119.1(7) . . ? C21 C22 H22 120.5 . . ? C17 C22 H22 120.5 . . ? C24 C23 N5 121.2(10) . . ? C24 C23 H23 119.4 . . ? N5 C23 H23 119.4 . . ? C23 C24 C25 119.8(12) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 121.8(10) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C27 125.1(11) . . ? C25 C26 C34 115.4(11) . . ? C27 C26 C34 119.5(12) . . ? C28 C27 C26 122.2(12) . . ? C28 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? C27 C28 C29 121.2(11) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C33 118.0(11) . . ? C30 C29 C28 123.6(11) . . ? C33 C29 C28 118.4(12) . . ? C29 C30 C31 122.4(10) . . ? C29 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C30 C31 C32 115.4(11) . . ? C30 C31 H31 122.3 . . ? C32 C31 H31 122.3 . . ? N6 C32 C31 124.3(10) . . ? N6 C32 H32 117.9 . . ? C31 C32 H32 117.9 . . ? N6 C33 C34 118.8(6) . . ? N6 C33 C29 120.7(9) . . ? C34 C33 C29 120.5(8) . . ? N5 C34 C33 119.4(6) . . ? N5 C34 C26 122.4(9) . . ? C33 C34 C26 118.2(9) . . ? N7 C35 C36 123.3(6) . . ? N7 C35 H35 118.4 . . ? C36 C35 H35 118.4 . . ? C37 C36 C35 119.0(6) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C38 120.4(6) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C46 C38 C37 116.8(6) . . ? C46 C38 C39 119.7(6) . . ? C37 C38 C39 123.4(6) . . ? C40 C39 C38 120.8(6) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C41 121.9(6) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C42 C41 C45 116.3(6) . . ? C42 C41 C40 124.3(6) . . ? C45 C41 C40 119.4(6) . . ? C43 C42 C41 121.0(6) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 118.9(6) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.6 . . ? N8 C44 C43 122.7(6) . . ? N8 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? N8 C45 C41 123.5(5) . . ? N8 C45 C46 117.5(4) . . ? C41 C45 C46 119.0(5) . . ? N7 C46 C38 122.8(5) . . ? N7 C46 C45 118.1(5) . . ? C38 C46 C45 119.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cd2 O1 C4 -2.3(4) . . . . ? N4 Cd2 O1 C4 -151.3(4) 2_645 . . . ? N7 Cd2 O1 C4 100.7(4) . . . . ? N8 Cd2 O1 C4 80.6(6) . . . . ? O8 Cd2 O1 C4 -81.8(4) 2_645 . . . ? N1 Cd1 O4 C5 -7.9(4) . . . . ? N3 Cd1 O4 C5 97.6(4) . . . . ? N5 Cd1 O4 C5 -93.5(4) . . . . ? N6 Cd1 O4 C5 -94.6(9) . . . . ? O5 Cd1 O4 C5 170.5(4) . . . . ? N1 Cd1 O5 C15 -102.7(6) . . . . ? N3 Cd1 O5 C15 -8.4(4) . . . . ? N5 Cd1 O5 C15 156.5(4) . . . . ? N6 Cd1 O5 C15 85.2(4) . . . . ? O4 Cd1 O5 C15 -107.3(4) . . . . ? N3 Cd1 N1 C1 87.5(6) . . . . ? N5 Cd1 N1 C1 -81.9(6) . . . . ? N6 Cd1 N1 C1 -12.3(6) . . . . ? O5 Cd1 N1 C1 175.9(4) . . . . ? O4 Cd1 N1 C1 -179.4(6) . . . . ? N3 Cd1 N1 C3 -86.2(4) . . . . ? N5 Cd1 N1 C3 104.5(4) . . . . ? N6 Cd1 N1 C3 174.0(4) . . . . ? O5 Cd1 N1 C3 2.2(7) . . . . ? O4 Cd1 N1 C3 6.9(3) . . . . ? N4 Cd2 N2 C1 -115.5(5) 2_645 . . . ? N7 Cd2 N2 C1 96.3(5) . . . . ? N8 Cd2 N2 C1 24.2(5) . . . . ? O8 Cd2 N2 C1 -60.8(5) 2_645 . . . ? O1 Cd2 N2 C1 -178.4(6) . . . . ? N4 Cd2 N2 C2 67.8(4) 2_645 . . . ? N7 Cd2 N2 C2 -80.4(3) . . . . ? N8 Cd2 N2 C2 -152.6(3) . . . . ? O8 Cd2 N2 C2 122.4(3) 2_645 . . . ? O1 Cd2 N2 C2 4.8(3) . . . . ? N1 Cd1 N3 C12 -27.3(6) . . . . ? N5 Cd1 N3 C12 116.1(7) . . . . ? N6 Cd1 N3 C12 80.6(6) . . . . ? O5 Cd1 N3 C12 173.0(6) . . . . ? O4 Cd1 N3 C12 -102.0(6) . . . . ? N1 Cd1 N3 C13 169.6(3) . . . . ? N5 Cd1 N3 C13 -46.9(7) . . . . ? N6 Cd1 N3 C13 -82.4(4) . . . . ? O5 Cd1 N3 C13 9.9(3) . . . . ? O4 Cd1 N3 C13 95.0(4) . . . . ? N1 Cd1 N5 C34 99.9(4) . . . . ? N3 Cd1 N5 C34 -45.3(8) . . . . ? N6 Cd1 N5 C34 -7.6(4) . . . . ? O5 Cd1 N5 C34 -99.2(4) . . . . ? O4 Cd1 N5 C34 172.7(4) . . . . ? N1 Cd1 N5 C23 -68.2(5) . . . . ? N3 Cd1 N5 C23 146.6(6) . . . . ? N6 Cd1 N5 C23 -175.7(6) . . . . ? O5 Cd1 N5 C23 92.7(5) . . . . ? O4 Cd1 N5 C23 4.5(6) . . . . ? N1 Cd1 N6 C32 99.0(6) . . . . ? N3 Cd1 N6 C32 -10.1(6) . . . . ? N5 Cd1 N6 C32 -179.1(6) . . . . ? O5 Cd1 N6 C32 -83.7(6) . . . . ? O4 Cd1 N6 C32 -177.9(7) . . . . ? N1 Cd1 N6 C33 -75.5(4) . . . . ? N3 Cd1 N6 C33 175.5(4) . . . . ? N5 Cd1 N6 C33 6.4(4) . . . . ? O5 Cd1 N6 C33 101.8(4) . . . . ? O4 Cd1 N6 C33 7.6(10) . . . . ? N2 Cd2 N7 C35 79.4(5) . . . . ? N4 Cd2 N7 C35 -81.9(5) 2_645 . . . ? N8 Cd2 N7 C35 179.7(5) . . . . ? O8 Cd2 N7 C35 -166.9(4) 2_645 . . . ? O1 Cd2 N7 C35 7.6(5) . . . . ? N2 Cd2 N7 C46 -106.0(4) . . . . ? N4 Cd2 N7 C46 92.6(4) 2_645 . . . ? N8 Cd2 N7 C46 -5.7(4) . . . . ? O8 Cd2 N7 C46 7.6(6) 2_645 . . . ? O1 Cd2 N7 C46 -177.8(4) . . . . ? N2 Cd2 N8 C44 -79.4(5) . . . . ? N4 Cd2 N8 C44 77.9(5) 2_645 . . . ? N7 Cd2 N8 C44 -177.7(5) . . . . ? O8 Cd2 N8 C44 8.0(5) 2_645 . . . ? O1 Cd2 N8 C44 -156.2(5) . . . . ? N2 Cd2 N8 C45 102.6(4) . . . . ? N4 Cd2 N8 C45 -100.1(4) 2_645 . . . ? N7 Cd2 N8 C45 4.4(4) . . . . ? O8 Cd2 N8 C45 -170.0(4) 2_645 . . . ? O1 Cd2 N8 C45 25.8(6) . . . . ? C3 N1 C1 N2 0.1(6) . . . . ? Cd1 N1 C1 N2 -173.9(4) . . . . ? C3 N1 C1 C6 179.9(4) . . . . ? Cd1 N1 C1 C6 5.9(8) . . . . ? C2 N2 C1 N1 0.4(6) . . . . ? Cd2 N2 C1 N1 -176.6(4) . . . . ? C2 N2 C1 C6 -179.4(4) . . . . ? Cd2 N2 C1 C6 3.6(8) . . . . ? C1 N2 C2 C3 -0.7(5) . . . . ? Cd2 N2 C2 C3 177.1(3) . . . . ? C1 N2 C2 C4 175.0(5) . . . . ? Cd2 N2 C2 C4 -7.1(6) . . . . ? N2 C2 C3 N1 0.7(6) . . . . ? C4 C2 C3 N1 -174.2(5) . . . . ? N2 C2 C3 C5 -177.5(5) . . . . ? C4 C2 C3 C5 7.6(10) . . . . ? C1 N1 C3 C2 -0.5(6) . . . . ? Cd1 N1 C3 C2 175.3(3) . . . . ? C1 N1 C3 C5 178.0(5) . . . . ? Cd1 N1 C3 C5 -6.2(6) . . . . ? Cd2 O1 C4 O2 177.6(4) . . . . ? Cd2 O1 C4 C2 -0.5(6) . . . . ? C3 C2 C4 O1 179.6(5) . . . . ? N2 C2 C4 O1 5.1(8) . . . . ? C3 C2 C4 O2 1.4(9) . . . . ? N2 C2 C4 O2 -173.1(5) . . . . ? Cd1 O4 C5 O3 -172.1(5) . . . . ? Cd1 O4 C5 C3 7.5(7) . . . . ? C2 C3 C5 O4 177.0(6) . . . . ? N1 C3 C5 O4 -1.1(8) . . . . ? C2 C3 C5 O3 -3.4(9) . . . . ? N1 C3 C5 O3 178.5(5) . . . . ? N1 C1 C6 C7 -85.1(6) . . . . ? N2 C1 C6 C7 94.6(5) . . . . ? N1 C1 C6 C11 92.2(5) . . . . ? N2 C1 C6 C11 -88.0(6) . . . . ? C11 C6 C7 C8 0.0 . . . . ? C1 C6 C7 C8 177.3(4) . . . . ? C6 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C10 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C6 0.0 . . . . ? C7 C6 C11 C10 0.0 . . . . ? C1 C6 C11 C10 -177.4(4) . . . . ? C13 N3 C12 N4 0.6(6) . . . . ? Cd1 N3 C12 N4 -163.0(4) . . . . ? C13 N3 C12 C17 -176.8(5) . . . . ? Cd1 N3 C12 C17 19.6(9) . . . . ? C14 N4 C12 N3 -0.6(6) . . . . ? Cd2 N4 C12 N3 -179.0(4) 2_655 . . . ? C14 N4 C12 C17 176.7(5) . . . . ? Cd2 N4 C12 C17 -1.7(9) 2_655 . . . ? C12 N3 C13 C14 -0.3(6) . . . . ? Cd1 N3 C13 C14 169.0(3) . . . . ? C12 N3 C13 C15 179.2(5) . . . . ? Cd1 N3 C13 C15 -11.6(6) . . . . ? C12 N4 C14 C13 0.4(5) . . . . ? Cd2 N4 C14 C13 179.3(3) 2_655 . . . ? C12 N4 C14 C16 -176.6(4) . . . . ? Cd2 N4 C14 C16 2.2(6) 2_655 . . . ? N3 C13 C14 N4 -0.1(6) . . . . ? C15 C13 C14 N4 -179.5(5) . . . . ? N3 C13 C14 C16 176.5(5) . . . . ? C15 C13 C14 C16 -2.9(10) . . . . ? Cd1 O5 C15 O6 -175.9(4) . . . . ? Cd1 O5 C15 C13 5.4(6) . . . . ? N3 C13 C15 O5 4.4(8) . . . . ? C14 C13 C15 O5 -176.3(5) . . . . ? N3 C13 C15 O6 -174.4(5) . . . . ? C14 C13 C15 O6 5.0(9) . . . . ? Cd2 O8 C16 O7 178.0(4) 2_655 . . . ? Cd2 O8 C16 C14 -3.9(6) 2_655 . . . ? N4 C14 C16 O8 1.3(7) . . . . ? C13 C14 C16 O8 -174.9(5) . . . . ? N4 C14 C16 O7 179.5(5) . . . . ? C13 C14 C16 O7 3.3(9) . . . . ? N3 C12 C17 C18 45.5(8) . . . . ? N4 C12 C17 C18 -131.6(6) . . . . ? N3 C12 C17 C22 -134.4(6) . . . . ? N4 C12 C17 C22 48.5(8) . . . . ? C22 C17 C18 C19 0.2(9) . . . . ? C12 C17 C18 C19 -179.7(5) . . . . ? C17 C18 C19 C20 -0.7(10) . . . . ? C18 C19 C20 C21 0.8(11) . . . . ? C19 C20 C21 C22 -0.3(11) . . . . ? C20 C21 C22 C17 -0.3(10) . . . . ? C18 C17 C22 C21 0.3(9) . . . . ? C12 C17 C22 C21 -179.8(6) . . . . ? C34 N5 C23 C24 1.9(12) . . . . ? Cd1 N5 C23 C24 169.5(7) . . . . ? N5 C23 C24 C25 -0.8(16) . . . . ? C23 C24 C25 C26 0(2) . . . . ? C24 C25 C26 C27 -178.4(12) . . . . ? C24 C25 C26 C34 0.7(18) . . . . ? C25 C26 C27 C28 -179.3(13) . . . . ? C34 C26 C27 C28 2(2) . . . . ? C26 C27 C28 C29 -3(2) . . . . ? C27 C28 C29 C30 -177.9(12) . . . . ? C27 C28 C29 C33 2.6(17) . . . . ? C33 C29 C30 C31 -1.6(15) . . . . ? C28 C29 C30 C31 178.8(10) . . . . ? C29 C30 C31 C32 0.1(15) . . . . ? C33 N6 C32 C31 0.1(11) . . . . ? Cd1 N6 C32 C31 -174.2(6) . . . . ? C30 C31 C32 N6 0.7(13) . . . . ? C32 N6 C33 C34 -179.7(6) . . . . ? Cd1 N6 C33 C34 -4.8(7) . . . . ? C32 N6 C33 C29 -1.7(10) . . . . ? Cd1 N6 C33 C29 173.1(5) . . . . ? C30 C29 C33 N6 2.5(11) . . . . ? C28 C29 C33 N6 -178.0(8) . . . . ? C30 C29 C33 C34 -179.6(8) . . . . ? C28 C29 C33 C34 -0.1(11) . . . . ? C23 N5 C34 C33 177.0(6) . . . . ? Cd1 N5 C34 C33 8.3(8) . . . . ? C23 N5 C34 C26 -1.7(11) . . . . ? Cd1 N5 C34 C26 -170.4(6) . . . . ? N6 C33 C34 N5 -2.4(9) . . . . ? C29 C33 C34 N5 179.7(6) . . . . ? N6 C33 C34 C26 176.4(7) . . . . ? C29 C33 C34 C26 -1.5(11) . . . . ? C25 C26 C34 N5 0.4(14) . . . . ? C27 C26 C34 N5 179.5(9) . . . . ? C25 C26 C34 C33 -178.3(9) . . . . ? C27 C26 C34 C33 0.8(14) . . . . ? C46 N7 C35 C36 -2.6(9) . . . . ? Cd2 N7 C35 C36 171.9(5) . . . . ? N7 C35 C36 C37 1.5(11) . . . . ? C35 C36 C37 C38 1.3(12) . . . . ? C36 C37 C38 C46 -2.8(11) . . . . ? C36 C37 C38 C39 178.1(8) . . . . ? C46 C38 C39 C40 2.8(12) . . . . ? C37 C38 C39 C40 -178.1(8) . . . . ? C38 C39 C40 C41 -2.7(12) . . . . ? C39 C40 C41 C42 -179.2(7) . . . . ? C39 C40 C41 C45 -0.3(11) . . . . ? C45 C41 C42 C43 -1.6(10) . . . . ? C40 C41 C42 C43 177.3(7) . . . . ? C41 C42 C43 C44 0.9(12) . . . . ? C45 N8 C44 C43 -1.1(10) . . . . ? Cd2 N8 C44 C43 -179.1(5) . . . . ? C42 C43 C44 N8 0.5(12) . . . . ? C44 N8 C45 C41 0.3(8) . . . . ? Cd2 N8 C45 C41 178.5(4) . . . . ? C44 N8 C45 C46 179.2(5) . . . . ? Cd2 N8 C45 C46 -2.7(6) . . . . ? C42 C41 C45 N8 1.0(9) . . . . ? C40 C41 C45 N8 -178.0(6) . . . . ? C42 C41 C45 C46 -177.8(6) . . . . ? C40 C41 C45 C46 3.2(9) . . . . ? C35 N7 C46 C38 0.9(8) . . . . ? Cd2 N7 C46 C38 -174.1(5) . . . . ? C35 N7 C46 C45 -178.3(5) . . . . ? Cd2 N7 C46 C45 6.7(6) . . . . ? C37 C38 C46 N7 1.8(10) . . . . ? C39 C38 C46 N7 -179.1(6) . . . . ? C37 C38 C46 C45 -179.0(6) . . . . ? C39 C38 C46 C45 0.1(9) . . . . ? N8 C45 C46 N7 -2.7(7) . . . . ? C41 C45 C46 N7 176.2(5) . . . . ? N8 C45 C46 C38 178.1(5) . . . . ? C41 C45 C46 C38 -3.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.575 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.084 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 181 35 ' ' 2 0.500 0.500 1.000 181 35 ' ' _platon_squeeze_details ; ; # Attachment '- complex 2.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 809969' #TrackingRef '- complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H28 Cd2 N8 O8' _chemical_formula_weight 997.52 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 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 9.3505(4) _cell_length_b 20.6898(9) _cell_length_c 20.1672(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.284(2) _cell_angle_gamma 90.00 _cell_volume 3826.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9935 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.40 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6831 _exptl_absorpt_correction_T_max 0.8070 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28872 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7089 _reflns_number_gt 5951 _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^)+(0.0407P)^2^+3.1732P] 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 7089 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Cd1 Cd 0.25809(2) 0.289223(11) 0.050783(12) 0.03134(8) Uani 1 1 d . . . Cd2 Cd 0.62899(2) 0.507477(12) 0.269599(12) 0.03070(8) Uani 1 1 d . . . O1 O 0.5360(3) 0.57207(11) 0.17517(12) 0.0435(6) Uani 1 1 d . . . O2 O 0.4128(3) 0.57046(12) 0.06929(13) 0.0502(7) Uani 1 1 d . . . O3 O 0.2963(4) 0.49016(13) -0.01403(13) 0.0570(8) Uani 1 1 d . . . H3 H 0.3332 0.5165 0.0147 0.086 Uiso 1 1 calc R . . O4 O 0.2491(3) 0.38525(12) -0.01821(12) 0.0499(7) Uani 1 1 d . . . O5 O 0.4462(3) 0.24023(11) 0.00760(11) 0.0375(5) Uani 1 1 d . . . O6 O 0.5905(3) 0.15421(13) 0.01386(12) 0.0466(6) Uani 1 1 d . . . O7 O 0.6352(3) 0.05278(13) 0.07835(14) 0.0487(7) Uani 1 1 d . . . H7 H 0.6124 0.0839 0.0534 0.073 Uiso 1 1 calc R . . O8 O 0.5512(3) 0.00290(11) 0.15949(13) 0.0424(6) Uani 1 1 d . . . N1 N 0.4923(3) 0.44194(12) 0.19111(12) 0.0268(6) Uani 1 1 d . . . N2 N 0.3810(3) 0.36884(12) 0.11607(12) 0.0279(6) Uani 1 1 d . . . N3 N 0.2904(3) 0.18549(12) 0.09716(12) 0.0284(6) Uani 1 1 d . . . N4 N 0.3397(3) 0.09556(13) 0.16020(13) 0.0303(6) Uani 1 1 d . . . N5 N 0.0786(3) 0.25762(14) -0.03966(14) 0.0390(7) Uani 1 1 d . . . N6 N 0.0292(3) 0.31138(15) 0.07574(16) 0.0425(7) Uani 1 1 d . . . N7 N 0.8513(3) 0.49784(14) 0.23365(14) 0.0364(7) Uani 1 1 d . . . N8 N 0.8039(3) 0.45453(14) 0.35361(14) 0.0355(7) Uani 1 1 d . . . C1 C 0.4464(3) 0.47250(15) 0.13017(15) 0.0273(7) Uani 1 1 d . . . C2 C 0.3774(3) 0.42751(15) 0.08421(15) 0.0283(7) Uani 1 1 d . . . C3 C 0.4502(3) 0.38027(15) 0.18020(14) 0.0252(6) Uani 1 1 d . . . C4 C 0.4674(4) 0.54307(16) 0.12473(17) 0.0349(8) Uani 1 1 d . . . C5 C 0.3028(4) 0.43322(18) 0.01254(17) 0.0388(8) Uani 1 1 d . . . C6 C 0.4690(3) 0.33047(15) 0.23315(15) 0.0293(7) Uani 1 1 d . . . C7 C 0.4970(4) 0.26678(16) 0.21972(17) 0.0342(8) Uani 1 1 d . . . H7A H 0.5138 0.2555 0.1773 0.041 Uiso 1 1 calc R . . C8 C 0.5006(4) 0.21944(17) 0.2687(2) 0.0449(9) Uani 1 1 d . . . H8 H 0.5177 0.1765 0.2589 0.054 Uiso 1 1 calc R . . C9 C 0.4786(4) 0.2364(2) 0.33197(19) 0.0465(10) Uani 1 1 d . . . H9 H 0.4790 0.2047 0.3648 0.056 Uiso 1 1 calc R . . C10 C 0.4562(4) 0.29939(19) 0.34663(18) 0.0441(9) Uani 1 1 d . . . H10 H 0.4451 0.3105 0.3900 0.053 Uiso 1 1 calc R . . C11 C 0.4496(4) 0.34695(17) 0.29820(16) 0.0346(8) Uani 1 1 d . . . H11 H 0.4325 0.3897 0.3087 0.042 Uiso 1 1 calc R . . C12 C 0.4093(3) 0.15606(15) 0.08062(15) 0.0283(7) Uani 1 1 d . . . C13 C 0.4396(3) 0.10058(16) 0.11907(15) 0.0296(7) Uani 1 1 d . . . C14 C 0.2518(3) 0.14737(15) 0.14487(15) 0.0279(7) Uani 1 1 d . . . C15 C 0.4853(4) 0.18596(17) 0.03062(16) 0.0334(7) Uani 1 1 d . . . C16 C 0.5482(4) 0.04865(17) 0.12020(17) 0.0361(8) Uani 1 1 d . . . C17 C 0.1229(4) 0.15744(15) 0.17545(17) 0.0320(7) Uani 1 1 d . . . C18 C 0.1330(4) 0.15182(17) 0.24458(18) 0.0390(8) Uani 1 1 d . . . H18 H 0.2229 0.1440 0.2725 0.047 Uiso 1 1 calc R . . C19 C 0.0090(5) 0.15778(19) 0.2721(2) 0.0536(11) Uani 1 1 d . . . H19 H 0.0154 0.1537 0.3185 0.064 Uiso 1 1 calc R . . C20 C -0.1231(5) 0.1698(2) 0.2308(3) 0.0629(13) Uani 1 1 d . . . H20 H -0.2063 0.1735 0.2494 0.076 Uiso 1 1 calc R . . C21 C -0.1337(4) 0.1764(2) 0.1623(3) 0.0574(11) Uani 1 1 d . . . H21 H -0.2236 0.1850 0.1347 0.069 Uiso 1 1 calc R . . C22 C -0.0112(4) 0.17019(17) 0.13454(19) 0.0412(8) Uani 1 1 d . . . H22 H -0.0185 0.1746 0.0881 0.049 Uiso 1 1 calc R . . C23 C 0.1069(5) 0.2285(2) -0.0946(2) 0.0511(10) Uani 1 1 d . . . H23 H 0.2036 0.2225 -0.0984 0.061 Uiso 1 1 calc R . . C24 C -0.0026(6) 0.2068(2) -0.1464(2) 0.0612(12) Uani 1 1 d . . . H24 H 0.0199 0.1869 -0.1844 0.073 Uiso 1 1 calc R . . C25 C -0.1428(5) 0.2153(2) -0.1404(2) 0.0673(14) Uani 1 1 d . . . H25 H -0.2184 0.2004 -0.1740 0.081 Uiso 1 1 calc R . . C26 C -0.1731(5) 0.2460(2) -0.0843(2) 0.0652(13) Uani 1 1 d . . . H26 H -0.2692 0.2523 -0.0798 0.078 Uiso 1 1 calc R . . C27 C -0.0602(4) 0.26748(18) -0.03492(19) 0.0422(9) Uani 1 1 d . . . C28 C -0.0882(4) 0.30024(18) 0.0270(2) 0.0431(9) Uani 1 1 d . . . C29 C -0.2266(4) 0.3178(2) 0.0360(3) 0.0639(12) Uani 1 1 d . . . H29 H -0.3073 0.3118 0.0014 0.077 Uiso 1 1 calc R . . C30 C -0.2424(6) 0.3441(3) 0.0965(3) 0.0779(15) Uani 1 1 d . . . H30 H -0.3344 0.3563 0.1030 0.094 Uiso 1 1 calc R . . C31 C -0.1249(6) 0.3524(2) 0.1470(3) 0.0733(14) Uani 1 1 d . . . H31 H -0.1353 0.3684 0.1888 0.088 Uiso 1 1 calc R . . C32 C 0.0099(5) 0.3366(2) 0.1347(2) 0.0588(11) Uani 1 1 d . . . H32 H 0.0914 0.3437 0.1686 0.071 Uiso 1 1 calc R . . C33 C 0.8678(4) 0.51263(19) 0.17045(19) 0.0478(10) Uani 1 1 d . . . H33 H 0.7858 0.5239 0.1384 0.057 Uiso 1 1 calc R . . C34 C 1.0003(5) 0.5117(2) 0.1517(2) 0.0603(12) Uani 1 1 d . . . H34 H 1.0081 0.5213 0.1075 0.072 Uiso 1 1 calc R . . C35 C 1.1202(5) 0.4966(2) 0.1987(3) 0.0659(13) Uani 1 1 d . . . H35 H 1.2118 0.4967 0.1872 0.079 Uiso 1 1 calc R . . C36 C 1.1060(4) 0.4809(2) 0.2639(2) 0.0533(11) Uani 1 1 d . . . H36 H 1.1874 0.4699 0.2964 0.064 Uiso 1 1 calc R . . C37 C 0.9689(4) 0.48175(16) 0.27985(17) 0.0349(8) Uani 1 1 d . . . C38 C 0.9432(4) 0.46267(17) 0.34791(17) 0.0358(8) Uani 1 1 d . . . C39 C 1.0562(4) 0.4519(2) 0.4023(2) 0.0500(10) Uani 1 1 d . . . H39 H 1.1522 0.4592 0.3981 0.060 Uiso 1 1 calc R . . C40 C 1.0254(5) 0.4302(2) 0.4627(2) 0.0555(11) Uani 1 1 d . . . H40 H 1.1004 0.4217 0.4994 0.067 Uiso 1 1 calc R . . C41 C 0.8829(5) 0.4213(2) 0.4680(2) 0.0529(10) Uani 1 1 d . . . H41 H 0.8594 0.4067 0.5081 0.063 Uiso 1 1 calc R . . C42 C 0.7758(4) 0.43430(19) 0.41299(18) 0.0463(9) Uani 1 1 d . . . H42 H 0.6791 0.4289 0.4169 0.056 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 0.02819(14) 0.03116(15) 0.03400(14) -0.00122(10) 0.00442(10) -0.00114(10) Cd2 0.02765(14) 0.03304(15) 0.03202(14) -0.00524(10) 0.00733(10) -0.00116(10) O1 0.0560(16) 0.0279(13) 0.0430(14) -0.0009(11) 0.0011(12) -0.0041(12) O2 0.0646(18) 0.0340(14) 0.0459(15) 0.0121(12) -0.0044(13) -0.0030(13) O3 0.084(2) 0.0431(16) 0.0355(14) 0.0099(12) -0.0092(14) -0.0100(15) O4 0.0680(18) 0.0458(16) 0.0301(13) 0.0013(12) -0.0048(12) -0.0160(14) O5 0.0419(14) 0.0383(14) 0.0364(13) 0.0095(11) 0.0177(10) 0.0045(11) O6 0.0462(15) 0.0546(16) 0.0473(15) 0.0109(12) 0.0293(12) 0.0125(13) O7 0.0470(15) 0.0481(17) 0.0598(17) 0.0133(13) 0.0325(13) 0.0189(13) O8 0.0398(14) 0.0381(14) 0.0531(16) 0.0161(12) 0.0185(12) 0.0109(11) N1 0.0253(13) 0.0291(15) 0.0265(13) 0.0008(11) 0.0064(10) -0.0013(11) N2 0.0281(14) 0.0299(15) 0.0263(13) -0.0003(11) 0.0065(10) -0.0011(11) N3 0.0287(14) 0.0292(14) 0.0288(14) 0.0011(11) 0.0093(11) 0.0004(12) N4 0.0311(14) 0.0301(15) 0.0320(14) 0.0005(11) 0.0120(11) 0.0029(12) N5 0.0344(16) 0.0412(18) 0.0405(17) 0.0012(13) 0.0051(12) -0.0015(13) N6 0.0352(17) 0.0390(17) 0.0542(19) -0.0034(15) 0.0113(14) 0.0023(14) N7 0.0348(16) 0.0431(18) 0.0337(16) -0.0042(12) 0.0127(12) 0.0011(13) N8 0.0308(15) 0.0377(17) 0.0391(16) 0.0021(13) 0.0092(12) 0.0003(13) C1 0.0251(16) 0.0282(17) 0.0299(16) 0.0001(13) 0.0087(12) 0.0002(13) C2 0.0285(16) 0.0291(17) 0.0283(16) 0.0034(13) 0.0079(12) -0.0022(13) C3 0.0222(15) 0.0279(17) 0.0268(16) 0.0012(13) 0.0079(12) -0.0002(13) C4 0.0343(18) 0.0307(19) 0.041(2) 0.0028(15) 0.0096(15) 0.0006(15) C5 0.043(2) 0.043(2) 0.0300(17) 0.0073(16) 0.0046(15) -0.0061(17) C6 0.0263(16) 0.0317(18) 0.0290(17) 0.0010(14) 0.0033(12) -0.0053(14) C7 0.0354(18) 0.0349(19) 0.0310(17) -0.0030(15) 0.0032(14) -0.0007(15) C8 0.043(2) 0.0293(19) 0.055(2) 0.0058(17) -0.0078(17) -0.0068(16) C9 0.041(2) 0.051(2) 0.043(2) 0.0176(18) -0.0018(16) -0.0149(18) C10 0.048(2) 0.054(3) 0.0319(19) 0.0047(17) 0.0118(16) -0.0107(18) C11 0.0373(19) 0.038(2) 0.0307(17) -0.0019(15) 0.0115(14) -0.0059(15) C12 0.0283(16) 0.0317(18) 0.0263(16) 0.0001(13) 0.0090(12) 0.0025(14) C13 0.0286(16) 0.0329(18) 0.0289(16) 0.0001(14) 0.0093(13) 0.0057(14) C14 0.0270(16) 0.0283(17) 0.0298(16) -0.0024(13) 0.0094(12) -0.0002(13) C15 0.0320(18) 0.042(2) 0.0277(17) 0.0014(15) 0.0101(13) -0.0006(16) C16 0.0310(18) 0.039(2) 0.0409(19) -0.0013(16) 0.0121(14) 0.0033(15) C17 0.0316(17) 0.0257(17) 0.0418(19) -0.0014(14) 0.0152(14) 0.0003(14) C18 0.042(2) 0.036(2) 0.043(2) -0.0013(16) 0.0191(16) 0.0005(16) C19 0.063(3) 0.048(2) 0.061(3) -0.007(2) 0.038(2) 0.000(2) C20 0.046(3) 0.057(3) 0.099(4) -0.014(3) 0.047(3) 0.000(2) C21 0.029(2) 0.053(3) 0.092(3) -0.009(2) 0.015(2) 0.0028(18) C22 0.0358(19) 0.039(2) 0.049(2) -0.0026(17) 0.0103(16) 0.0013(16) C23 0.053(2) 0.054(3) 0.045(2) -0.0013(19) 0.0083(18) -0.003(2) C24 0.089(4) 0.052(3) 0.038(2) -0.0017(18) 0.001(2) -0.008(2) C25 0.062(3) 0.067(3) 0.060(3) 0.006(2) -0.019(2) -0.018(2) C26 0.044(2) 0.079(3) 0.064(3) 0.004(3) -0.010(2) -0.011(2) C27 0.0322(19) 0.040(2) 0.051(2) 0.0127(17) -0.0006(16) -0.0079(16) C28 0.0325(19) 0.035(2) 0.063(2) 0.0091(18) 0.0127(17) 0.0018(16) C29 0.034(2) 0.067(3) 0.090(3) 0.011(3) 0.011(2) 0.006(2) C30 0.060(3) 0.074(3) 0.114(4) 0.001(3) 0.050(3) 0.018(3) C31 0.072(3) 0.064(3) 0.096(4) -0.018(3) 0.046(3) 0.005(3) C32 0.057(3) 0.053(3) 0.072(3) -0.020(2) 0.026(2) 0.001(2) C33 0.048(2) 0.060(3) 0.039(2) -0.0016(18) 0.0159(17) 0.0010(19) C34 0.065(3) 0.074(3) 0.051(3) -0.002(2) 0.034(2) 0.002(2) C35 0.044(3) 0.087(4) 0.077(3) 0.003(3) 0.037(2) 0.003(2) C36 0.031(2) 0.068(3) 0.063(3) 0.001(2) 0.0149(18) 0.0021(19) C37 0.0286(17) 0.0358(19) 0.0416(19) -0.0061(15) 0.0105(14) -0.0027(15) C38 0.0346(19) 0.0341(19) 0.0387(19) -0.0031(15) 0.0072(14) 0.0000(15) C39 0.034(2) 0.057(3) 0.055(2) -0.003(2) 0.0002(17) -0.0036(18) C40 0.055(3) 0.064(3) 0.042(2) 0.003(2) -0.0037(18) 0.005(2) C41 0.060(3) 0.059(3) 0.041(2) 0.0083(19) 0.0111(18) 0.005(2) C42 0.044(2) 0.053(2) 0.044(2) 0.0069(18) 0.0133(17) 0.0043(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.275(2) . ? Cd1 N5 2.318(3) . ? Cd1 N3 2.337(3) . ? Cd1 N6 2.338(3) . ? Cd1 O5 2.340(2) . ? Cd1 O4 2.418(2) . ? Cd2 N1 2.277(2) . ? Cd2 N4 2.291(3) 2_655 ? Cd2 N7 2.340(3) . ? Cd2 O1 2.350(2) . ? Cd2 N8 2.379(3) . ? Cd2 O8 2.415(2) 2_655 ? O1 C4 1.245(4) . ? O2 C4 1.268(4) . ? O3 C5 1.291(4) . ? O3 H3 0.8200 . ? O4 C5 1.225(4) . ? O5 C15 1.242(4) . ? O6 C15 1.282(4) . ? O7 C16 1.285(4) . ? O7 H7 0.8200 . ? O8 C16 1.231(4) . ? O8 Cd2 2.415(2) 2_645 ? N1 C3 1.340(4) . ? N1 C1 1.374(4) . ? N2 C3 1.349(4) . ? N2 C2 1.371(4) . ? N3 C14 1.347(4) . ? N3 C12 1.365(4) . ? N4 C14 1.349(4) . ? N4 C13 1.369(4) . ? N4 Cd2 2.291(3) 2_645 ? N5 C23 1.333(5) . ? N5 C27 1.336(5) . ? N6 C32 1.342(5) . ? N6 C28 1.342(5) . ? N7 C37 1.337(4) . ? N7 C33 1.349(4) . ? N8 C38 1.340(4) . ? N8 C42 1.342(4) . ? C1 C2 1.381(4) . ? C1 C4 1.480(5) . ? C2 C5 1.482(4) . ? C3 C6 1.470(4) . ? C6 C7 1.381(5) . ? C6 C11 1.401(4) . ? C7 C8 1.387(5) . ? C7 H7A 0.9300 . ? C8 C9 1.377(6) . ? C8 H8 0.9300 . ? C9 C10 1.362(6) . ? C9 H9 0.9300 . ? C10 C11 1.379(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.383(4) . ? C12 C15 1.478(4) . ? C13 C16 1.476(5) . ? C14 C17 1.472(4) . ? C17 C18 1.384(5) . ? C17 C22 1.385(5) . ? C18 C19 1.385(5) . ? C18 H18 0.9300 . ? C19 C20 1.370(6) . ? C19 H19 0.9300 . ? C20 C21 1.372(6) . ? C20 H20 0.9300 . ? C21 C22 1.376(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.387(6) . ? C23 H23 0.9300 . ? C24 C25 1.352(7) . ? C24 H24 0.9300 . ? C25 C26 1.375(7) . ? C25 H25 0.9300 . ? C26 C27 1.375(5) . ? C26 H26 0.9300 . ? C27 C28 1.488(6) . ? C28 C29 1.390(5) . ? C29 C30 1.371(7) . ? C29 H29 0.9300 . ? C30 C31 1.354(7) . ? C30 H30 0.9300 . ? C31 C32 1.371(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.364(6) . ? C33 H33 0.9300 . ? C34 C35 1.355(7) . ? C34 H34 0.9300 . ? C35 C36 1.386(6) . ? C35 H35 0.9300 . ? C36 C37 1.381(5) . ? C36 H36 0.9300 . ? C37 C38 1.492(5) . ? C38 C39 1.384(5) . ? C39 C40 1.382(6) . ? C39 H39 0.9300 . ? C40 C41 1.369(6) . ? C40 H40 0.9300 . ? C41 C42 1.368(5) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N5 149.96(10) . . ? N2 Cd1 N3 114.98(9) . . ? N5 Cd1 N3 94.18(10) . . ? N2 Cd1 N6 96.53(10) . . ? N5 Cd1 N6 70.88(11) . . ? N3 Cd1 N6 98.39(10) . . ? N2 Cd1 O5 101.39(9) . . ? N5 Cd1 O5 93.78(10) . . ? N3 Cd1 O5 72.76(8) . . ? N6 Cd1 O5 162.02(10) . . ? N2 Cd1 O4 72.22(8) . . ? N5 Cd1 O4 80.84(9) . . ? N3 Cd1 O4 166.47(9) . . ? N6 Cd1 O4 91.88(10) . . ? O5 Cd1 O4 94.91(9) . . ? N1 Cd2 N4 152.82(9) . 2_655 ? N1 Cd2 N7 98.38(9) . . ? N4 Cd2 N7 104.20(10) 2_655 . ? N1 Cd2 O1 72.95(9) . . ? N4 Cd2 O1 91.76(9) 2_655 . ? N7 Cd2 O1 90.44(10) . . ? N1 Cd2 N8 115.79(9) . . ? N4 Cd2 N8 86.51(10) 2_655 . ? N7 Cd2 N8 69.69(10) . . ? O1 Cd2 N8 158.88(9) . . ? N1 Cd2 O8 91.52(8) . 2_655 ? N4 Cd2 O8 71.64(8) 2_655 2_655 ? N7 Cd2 O8 160.87(10) . 2_655 ? O1 Cd2 O8 108.17(9) . 2_655 ? N8 Cd2 O8 91.27(9) . 2_655 ? C4 O1 Cd2 116.0(2) . . ? C5 O3 H3 109.5 . . ? C5 O4 Cd1 114.2(2) . . ? C15 O5 Cd1 116.1(2) . . ? C16 O7 H7 109.5 . . ? C16 O8 Cd2 114.9(2) . 2_645 ? C3 N1 C1 105.1(2) . . ? C3 N1 Cd2 141.9(2) . . ? C1 N1 Cd2 112.48(19) . . ? C3 N2 C2 104.9(2) . . ? C3 N2 Cd1 140.8(2) . . ? C2 N2 Cd1 114.00(19) . . ? C14 N3 C12 104.9(3) . . ? C14 N3 Cd1 142.4(2) . . ? C12 N3 Cd1 111.07(19) . . ? C14 N4 C13 105.0(3) . . ? C14 N4 Cd2 140.5(2) . 2_645 ? C13 N4 Cd2 114.5(2) . 2_645 ? C23 N5 C27 118.8(3) . . ? C23 N5 Cd1 123.4(3) . . ? C27 N5 Cd1 117.7(2) . . ? C32 N6 C28 118.9(3) . . ? C32 N6 Cd1 123.6(3) . . ? C28 N6 Cd1 117.4(2) . . ? C37 N7 C33 118.9(3) . . ? C37 N7 Cd2 117.7(2) . . ? C33 N7 Cd2 123.1(2) . . ? C38 N8 C42 118.6(3) . . ? C38 N8 Cd2 115.2(2) . . ? C42 N8 Cd2 123.5(2) . . ? N1 C1 C2 108.3(3) . . ? N1 C1 C4 119.8(3) . . ? C2 C1 C4 131.8(3) . . ? N2 C2 C1 108.5(3) . . ? N2 C2 C5 119.4(3) . . ? C1 C2 C5 132.1(3) . . ? N1 C3 N2 113.2(3) . . ? N1 C3 C6 124.0(3) . . ? N2 C3 C6 122.7(3) . . ? O1 C4 O2 124.0(3) . . ? O1 C4 C1 118.0(3) . . ? O2 C4 C1 118.0(3) . . ? O4 C5 O3 123.2(3) . . ? O4 C5 C2 119.8(3) . . ? O3 C5 C2 116.9(3) . . ? C7 C6 C11 118.7(3) . . ? C7 C6 C3 121.8(3) . . ? C11 C6 C3 119.4(3) . . ? C6 C7 C8 120.9(3) . . ? C6 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C9 C8 C7 119.6(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 121.1(3) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 119.6(3) . . ? C10 C11 H11 120.2 . . ? C6 C11 H11 120.2 . . ? N3 C12 C13 108.7(3) . . ? N3 C12 C15 120.2(3) . . ? C13 C12 C15 131.0(3) . . ? N4 C13 C12 108.3(3) . . ? N4 C13 C16 119.0(3) . . ? C12 C13 C16 132.7(3) . . ? N3 C14 N4 113.1(3) . . ? N3 C14 C17 124.9(3) . . ? N4 C14 C17 121.9(3) . . ? O5 C15 O6 123.3(3) . . ? O5 C15 C12 119.2(3) . . ? O6 C15 C12 117.5(3) . . ? O8 C16 O7 122.5(3) . . ? O8 C16 C13 119.9(3) . . ? O7 C16 C13 117.6(3) . . ? C18 C17 C22 119.4(3) . . ? C18 C17 C14 120.7(3) . . ? C22 C17 C14 119.8(3) . . ? C17 C18 C19 119.9(4) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 119.9(4) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.5(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 119.9(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C17 120.3(4) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? N5 C23 C24 122.4(4) . . ? N5 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C25 C24 C23 118.5(4) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C24 C25 C26 119.6(4) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 119.5(4) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? N5 C27 C26 121.2(4) . . ? N5 C27 C28 117.5(3) . . ? C26 C27 C28 121.2(4) . . ? N6 C28 C29 120.6(4) . . ? N6 C28 C27 116.1(3) . . ? C29 C28 C27 123.3(4) . . ? C30 C29 C28 119.0(4) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C31 C30 C29 120.4(4) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 118.3(5) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? N6 C32 C31 122.7(4) . . ? N6 C32 H32 118.7 . . ? C31 C32 H32 118.7 . . ? N7 C33 C34 122.5(4) . . ? N7 C33 H33 118.7 . . ? C34 C33 H33 118.7 . . ? C35 C34 C33 118.8(4) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 119.8(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C36 C35 118.9(4) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? N7 C37 C36 121.0(3) . . ? N7 C37 C38 116.6(3) . . ? C36 C37 C38 122.3(3) . . ? N8 C38 C39 121.1(3) . . ? N8 C38 C37 116.5(3) . . ? C39 C38 C37 122.4(3) . . ? C40 C39 C38 119.5(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C39 119.1(4) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C42 C41 C40 118.7(4) . . ? C42 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? N8 C42 C41 123.0(4) . . ? N8 C42 H42 118.5 . . ? C41 C42 H42 118.5 . . ? 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 Cd2 O1 C4 -5.5(2) . . . . ? N4 Cd2 O1 C4 -162.6(3) 2_655 . . . ? N7 Cd2 O1 C4 93.1(3) . . . . ? N8 Cd2 O1 C4 112.5(3) . . . . ? O8 Cd2 O1 C4 -91.4(3) 2_655 . . . ? N2 Cd1 O4 C5 -5.0(3) . . . . ? N5 Cd1 O4 C5 161.5(3) . . . . ? N3 Cd1 O4 C5 -129.3(4) . . . . ? N6 Cd1 O4 C5 91.3(3) . . . . ? O5 Cd1 O4 C5 -105.4(3) . . . . ? N2 Cd1 O5 C15 108.0(2) . . . . ? N5 Cd1 O5 C15 -98.0(2) . . . . ? N3 Cd1 O5 C15 -4.8(2) . . . . ? N6 Cd1 O5 C15 -67.3(4) . . . . ? O4 Cd1 O5 C15 -179.1(2) . . . . ? N4 Cd2 N1 C3 -123.6(3) 2_655 . . . ? N7 Cd2 N1 C3 90.3(3) . . . . ? O1 Cd2 N1 C3 178.2(3) . . . . ? N8 Cd2 N1 C3 18.8(4) . . . . ? O8 Cd2 N1 C3 -73.3(3) 2_655 . . . ? N4 Cd2 N1 C1 65.7(3) 2_655 . . . ? N7 Cd2 N1 C1 -80.4(2) . . . . ? O1 Cd2 N1 C1 7.50(19) . . . . ? N8 Cd2 N1 C1 -151.8(2) . . . . ? O8 Cd2 N1 C1 116.0(2) 2_655 . . . ? N5 Cd1 N2 C3 148.8(3) . . . . ? N3 Cd1 N2 C3 -16.2(4) . . . . ? N6 Cd1 N2 C3 86.2(3) . . . . ? O5 Cd1 N2 C3 -92.3(3) . . . . ? O4 Cd1 N2 C3 176.1(3) . . . . ? N5 Cd1 N2 C2 -23.7(3) . . . . ? N3 Cd1 N2 C2 171.3(2) . . . . ? N6 Cd1 N2 C2 -86.3(2) . . . . ? O5 Cd1 N2 C2 95.1(2) . . . . ? O4 Cd1 N2 C2 3.6(2) . . . . ? N2 Cd1 N3 C14 74.5(3) . . . . ? N5 Cd1 N3 C14 -98.1(3) . . . . ? N6 Cd1 N3 C14 -26.8(3) . . . . ? O5 Cd1 N3 C14 169.3(3) . . . . ? O4 Cd1 N3 C14 -165.8(3) . . . . ? N2 Cd1 N3 C12 -87.9(2) . . . . ? N5 Cd1 N3 C12 99.6(2) . . . . ? N6 Cd1 N3 C12 170.8(2) . . . . ? O5 Cd1 N3 C12 6.89(19) . . . . ? O4 Cd1 N3 C12 31.8(5) . . . . ? N2 Cd1 N5 C23 114.3(3) . . . . ? N3 Cd1 N5 C23 -79.4(3) . . . . ? N6 Cd1 N5 C23 -176.8(3) . . . . ? O5 Cd1 N5 C23 -6.4(3) . . . . ? O4 Cd1 N5 C23 88.0(3) . . . . ? N2 Cd1 N5 C27 -68.0(3) . . . . ? N3 Cd1 N5 C27 98.4(3) . . . . ? N6 Cd1 N5 C27 1.0(2) . . . . ? O5 Cd1 N5 C27 171.4(3) . . . . ? O4 Cd1 N5 C27 -94.3(3) . . . . ? N2 Cd1 N6 C32 -29.9(3) . . . . ? N5 Cd1 N6 C32 178.1(3) . . . . ? N3 Cd1 N6 C32 86.6(3) . . . . ? O5 Cd1 N6 C32 145.5(3) . . . . ? O4 Cd1 N6 C32 -102.2(3) . . . . ? N2 Cd1 N6 C28 147.5(3) . . . . ? N5 Cd1 N6 C28 -4.4(3) . . . . ? N3 Cd1 N6 C28 -96.0(3) . . . . ? O5 Cd1 N6 C28 -37.1(5) . . . . ? O4 Cd1 N6 C28 75.2(3) . . . . ? N1 Cd2 N7 C37 -128.2(2) . . . . ? N4 Cd2 N7 C37 67.0(3) 2_655 . . . ? O1 Cd2 N7 C37 159.0(2) . . . . ? N8 Cd2 N7 C37 -13.7(2) . . . . ? O8 Cd2 N7 C37 -7.8(4) 2_655 . . . ? N1 Cd2 N7 C33 57.2(3) . . . . ? N4 Cd2 N7 C33 -107.6(3) 2_655 . . . ? O1 Cd2 N7 C33 -15.6(3) . . . . ? N8 Cd2 N7 C33 171.7(3) . . . . ? O8 Cd2 N7 C33 177.6(3) 2_655 . . . ? N1 Cd2 N8 C38 108.1(2) . . . . ? N4 Cd2 N8 C38 -88.1(2) 2_655 . . . ? N7 Cd2 N8 C38 18.4(2) . . . . ? O1 Cd2 N8 C38 -2.2(4) . . . . ? O8 Cd2 N8 C38 -159.6(2) 2_655 . . . ? N1 Cd2 N8 C42 -91.0(3) . . . . ? N4 Cd2 N8 C42 72.8(3) 2_655 . . . ? N7 Cd2 N8 C42 179.3(3) . . . . ? O1 Cd2 N8 C42 158.7(3) . . . . ? O8 Cd2 N8 C42 1.3(3) 2_655 . . . ? C3 N1 C1 C2 0.0(3) . . . . ? Cd2 N1 C1 C2 174.1(2) . . . . ? C3 N1 C1 C4 176.4(3) . . . . ? Cd2 N1 C1 C4 -9.5(3) . . . . ? C3 N2 C2 C1 0.7(3) . . . . ? Cd1 N2 C2 C1 175.8(2) . . . . ? C3 N2 C2 C5 -177.6(3) . . . . ? Cd1 N2 C2 C5 -2.5(4) . . . . ? N1 C1 C2 N2 -0.5(3) . . . . ? C4 C1 C2 N2 -176.3(3) . . . . ? N1 C1 C2 C5 177.5(3) . . . . ? C4 C1 C2 C5 1.7(6) . . . . ? C1 N1 C3 N2 0.4(3) . . . . ? Cd2 N1 C3 N2 -170.6(2) . . . . ? C1 N1 C3 C6 -176.1(3) . . . . ? Cd2 N1 C3 C6 12.8(5) . . . . ? C2 N2 C3 N1 -0.7(3) . . . . ? Cd1 N2 C3 N1 -173.6(2) . . . . ? C2 N2 C3 C6 175.9(3) . . . . ? Cd1 N2 C3 C6 2.9(5) . . . . ? Cd2 O1 C4 O2 -178.5(3) . . . . ? Cd2 O1 C4 C1 2.5(4) . . . . ? N1 C1 C4 O1 4.9(5) . . . . ? C2 C1 C4 O1 -179.6(3) . . . . ? N1 C1 C4 O2 -174.2(3) . . . . ? C2 C1 C4 O2 1.2(5) . . . . ? Cd1 O4 C5 O3 -173.4(3) . . . . ? Cd1 O4 C5 C2 5.5(4) . . . . ? N2 C2 C5 O4 -2.3(5) . . . . ? C1 C2 C5 O4 179.9(3) . . . . ? N2 C2 C5 O3 176.7(3) . . . . ? C1 C2 C5 O3 -1.1(6) . . . . ? N1 C3 C6 C7 -146.1(3) . . . . ? N2 C3 C6 C7 37.7(5) . . . . ? N1 C3 C6 C11 37.6(4) . . . . ? N2 C3 C6 C11 -138.6(3) . . . . ? C11 C6 C7 C8 2.4(5) . . . . ? C3 C6 C7 C8 -173.8(3) . . . . ? C6 C7 C8 C9 -1.2(5) . . . . ? C7 C8 C9 C10 -1.2(5) . . . . ? C8 C9 C10 C11 2.4(6) . . . . ? C9 C10 C11 C6 -1.2(5) . . . . ? C7 C6 C11 C10 -1.2(5) . . . . ? C3 C6 C11 C10 175.1(3) . . . . ? C14 N3 C12 C13 0.0(3) . . . . ? Cd1 N3 C12 C13 168.9(2) . . . . ? C14 N3 C12 C15 -177.9(3) . . . . ? Cd1 N3 C12 C15 -8.9(3) . . . . ? C14 N4 C13 C12 0.7(3) . . . . ? Cd2 N4 C13 C12 -179.0(2) 2_645 . . . ? C14 N4 C13 C16 -176.4(3) . . . . ? Cd2 N4 C13 C16 3.9(4) 2_645 . . . ? N3 C12 C13 N4 -0.4(4) . . . . ? C15 C12 C13 N4 177.1(3) . . . . ? N3 C12 C13 C16 176.1(3) . . . . ? C15 C12 C13 C16 -6.3(6) . . . . ? C12 N3 C14 N4 0.5(3) . . . . ? Cd1 N3 C14 N4 -162.5(2) . . . . ? C12 N3 C14 C17 -176.1(3) . . . . ? Cd1 N3 C14 C17 20.9(5) . . . . ? C13 N4 C14 N3 -0.7(3) . . . . ? Cd2 N4 C14 N3 178.8(2) 2_645 . . . ? C13 N4 C14 C17 176.0(3) . . . . ? Cd2 N4 C14 C17 -4.5(5) 2_645 . . . ? Cd1 O5 C15 O6 -177.2(2) . . . . ? Cd1 O5 C15 C12 1.9(4) . . . . ? N3 C12 C15 O5 5.1(5) . . . . ? C13 C12 C15 O5 -172.2(3) . . . . ? N3 C12 C15 O6 -175.7(3) . . . . ? C13 C12 C15 O6 7.0(5) . . . . ? Cd2 O8 C16 O7 -178.8(3) 2_645 . . . ? Cd2 O8 C16 C13 -0.2(4) 2_645 . . . ? N4 C13 C16 O8 -2.5(5) . . . . ? C12 C13 C16 O8 -178.8(3) . . . . ? N4 C13 C16 O7 176.1(3) . . . . ? C12 C13 C16 O7 -0.1(6) . . . . ? N3 C14 C17 C18 -135.4(3) . . . . ? N4 C14 C17 C18 48.3(4) . . . . ? N3 C14 C17 C22 47.2(5) . . . . ? N4 C14 C17 C22 -129.1(3) . . . . ? C22 C17 C18 C19 1.2(5) . . . . ? C14 C17 C18 C19 -176.3(3) . . . . ? C17 C18 C19 C20 -0.5(6) . . . . ? C18 C19 C20 C21 -0.4(6) . . . . ? C19 C20 C21 C22 0.7(7) . . . . ? C20 C21 C22 C17 -0.1(6) . . . . ? C18 C17 C22 C21 -0.8(5) . . . . ? C14 C17 C22 C21 176.6(3) . . . . ? C27 N5 C23 C24 -1.4(6) . . . . ? Cd1 N5 C23 C24 176.3(3) . . . . ? N5 C23 C24 C25 -0.4(6) . . . . ? C23 C24 C25 C26 1.3(7) . . . . ? C24 C25 C26 C27 -0.3(7) . . . . ? C23 N5 C27 C26 2.4(6) . . . . ? Cd1 N5 C27 C26 -175.4(3) . . . . ? C23 N5 C27 C28 -179.9(3) . . . . ? Cd1 N5 C27 C28 2.3(4) . . . . ? C25 C26 C27 N5 -1.6(6) . . . . ? C25 C26 C27 C28 -179.2(4) . . . . ? C32 N6 C28 C29 3.5(6) . . . . ? Cd1 N6 C28 C29 -174.1(3) . . . . ? C32 N6 C28 C27 -175.4(3) . . . . ? Cd1 N6 C28 C27 7.1(4) . . . . ? N5 C27 C28 N6 -6.2(5) . . . . ? C26 C27 C28 N6 171.4(4) . . . . ? N5 C27 C28 C29 174.9(4) . . . . ? C26 C27 C28 C29 -7.4(6) . . . . ? N6 C28 C29 C30 -2.8(7) . . . . ? C27 C28 C29 C30 175.9(4) . . . . ? C28 C29 C30 C31 -0.5(8) . . . . ? C29 C30 C31 C32 2.9(8) . . . . ? C28 N6 C32 C31 -0.9(6) . . . . ? Cd1 N6 C32 C31 176.5(3) . . . . ? C30 C31 C32 N6 -2.3(8) . . . . ? C37 N7 C33 C34 0.1(6) . . . . ? Cd2 N7 C33 C34 174.6(3) . . . . ? N7 C33 C34 C35 -1.3(7) . . . . ? C33 C34 C35 C36 1.6(7) . . . . ? C34 C35 C36 C37 -0.7(7) . . . . ? C33 N7 C37 C36 0.8(5) . . . . ? Cd2 N7 C37 C36 -174.1(3) . . . . ? C33 N7 C37 C38 -177.0(3) . . . . ? Cd2 N7 C37 C38 8.1(4) . . . . ? C35 C36 C37 N7 -0.4(6) . . . . ? C35 C36 C37 C38 177.2(4) . . . . ? C42 N8 C38 C39 -1.4(5) . . . . ? Cd2 N8 C38 C39 160.5(3) . . . . ? C42 N8 C38 C37 176.8(3) . . . . ? Cd2 N8 C38 C37 -21.3(4) . . . . ? N7 C37 C38 N8 9.2(5) . . . . ? C36 C37 C38 N8 -168.6(4) . . . . ? N7 C37 C38 C39 -172.7(3) . . . . ? C36 C37 C38 C39 9.6(6) . . . . ? N8 C38 C39 C40 2.3(6) . . . . ? C37 C38 C39 C40 -175.7(4) . . . . ? C38 C39 C40 C41 -1.6(6) . . . . ? C39 C40 C41 C42 0.0(6) . . . . ? C38 N8 C42 C41 -0.3(6) . . . . ? Cd2 N8 C42 C41 -160.6(3) . . . . ? C40 C41 C42 N8 1.0(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O6 0.82 1.65 2.461(3) 168.8 . O3 H3 O2 0.82 1.64 2.461(4) 176.8 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.687 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.082 # Attachment '- complex 3.cif' data_c _database_code_depnum_ccdc_archive 'CCDC 809970' #TrackingRef '- complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H12 N4 O9 Pb3' _chemical_formula_weight 1097.93 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' Pb Pb -3.3944 10.1111 '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 20.0411(3) _cell_length_b 8.38050(10) _cell_length_c 13.2718(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.9050(10) _cell_angle_gamma 90.00 _cell_volume 2223.88(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9652 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 22.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1318 _exptl_absorpt_correction_T_max 0.1889 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19418 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4119 _reflns_number_gt 3557 _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. 310 restrains were used to restrain the Uij of atoms C2, C4, N2, C3, N1, C1, C6, C7, C8, C9, C10, C11, C13, C14, C12, N3, N4, C17, C18, C19, C20, C21, O9, H1W, O9, H2W and C22. To do these restrains, these atoms have reasonable displacement parameters, and the structure has reasonable O CH bond length. ; _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^)+(0.1510P)^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 4119 _refine_ls_number_parameters 343 _refine_ls_number_restraints 210 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1905 _refine_ls_wR_factor_gt 0.1827 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.055 _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 Pb1 Pb 0.09890(3) 1.10153(6) 0.04574(4) 0.0240(2) Uani 1 1 d . . . Pb2 Pb 0.24862(3) 0.68457(6) 0.10607(4) 0.0286(2) Uani 1 1 d . . . Pb3 Pb 0.02882(3) 0.51267(6) 0.17493(4) 0.0263(2) Uani 1 1 d . . . O1 O 0.1689(5) 0.8971(10) 0.1464(7) 0.021(2) Uani 1 1 d . . . O2 O 0.0768(5) 0.9490(11) 0.2165(7) 0.0216(19) Uani 1 1 d . . . O3 O 0.0077(5) 0.7465(11) 0.3491(7) 0.026(2) Uani 1 1 d . . . O4 O 0.0396(4) 0.6298(11) 0.4914(7) 0.022(2) Uani 1 1 d . . . O5 O 0.1277(6) 0.1727(11) -0.2865(7) 0.028(2) Uani 1 1 d . . . O6 O 0.0708(6) 0.1760(12) -0.1480(7) 0.034(3) Uani 1 1 d . . . O7 O 0.0650(5) 0.4410(12) -0.0046(7) 0.026(2) Uani 1 1 d . . . O8 O 0.1445(4) 0.5823(10) 0.0756(7) 0.020(2) Uani 1 1 d . . . N1 N 0.2131(6) 0.6895(13) 0.2881(8) 0.021(2) Uani 1 1 d U . . N2 N 0.1688(6) 0.5898(12) 0.4264(8) 0.020(2) Uani 1 1 d U . . N3 N 0.2356(6) 0.5009(12) -0.0527(8) 0.024(2) Uani 1 1 d U . . N4 N 0.2320(6) 0.3392(13) -0.1896(8) 0.023(2) Uani 1 1 d U . . C1 C 0.2235(8) 0.5985(15) 0.3715(10) 0.023(2) Uani 1 1 d U . . C2 C 0.1497(7) 0.7469(15) 0.2899(9) 0.020(2) Uani 1 1 d U . . C3 C 0.1223(7) 0.6829(14) 0.3737(9) 0.018(2) Uani 1 1 d U . . C4 C 0.1290(8) 0.8715(15) 0.2138(9) 0.022(3) Uani 1 1 d U . . C5 C 0.0544(7) 0.6929(14) 0.4072(10) 0.019(3) Uani 1 1 d . . . C6 C 0.2874(8) 0.5243(17) 0.4008(10) 0.027(2) Uani 1 1 d U . . C7 C 0.2951(9) 0.4105(18) 0.4784(12) 0.036(3) Uani 1 1 d U . . H7 H 0.2574 0.3778 0.5099 0.043 Uiso 1 1 calc R . . C8 C 0.3545(9) 0.346(2) 0.5094(13) 0.043(3) Uani 1 1 d U . . H8 H 0.3576 0.2786 0.5649 0.052 Uiso 1 1 calc R . . C9 C 0.4141(10) 0.382(2) 0.4568(15) 0.050(3) Uani 1 1 d U . . H9 H 0.4545 0.3306 0.4727 0.060 Uiso 1 1 calc R . . C10 C 0.4077(9) 0.499(2) 0.3812(14) 0.047(3) Uani 1 1 d U . . H10 H 0.4451 0.5294 0.3483 0.056 Uiso 1 1 calc R . . C11 C 0.3476(9) 0.567(2) 0.3551(13) 0.039(3) Uani 1 1 d U . . H11 H 0.3454 0.6454 0.3053 0.047 Uiso 1 1 calc R . . C12 C 0.2695(7) 0.4452(17) -0.1316(10) 0.025(2) Uani 1 1 d U . . C13 C 0.1724(7) 0.3289(15) -0.1498(9) 0.019(2) Uani 1 1 d U . . C14 C 0.1746(7) 0.4296(15) -0.0639(10) 0.022(2) Uani 1 1 d U . . C15 C 0.1191(7) 0.2194(15) -0.1981(10) 0.022(3) Uani 1 1 d . . . C16 C 0.1245(7) 0.4852(14) 0.0039(9) 0.018(3) Uani 1 1 d . . . C17 C 0.3378(9) 0.4928(19) -0.1515(13) 0.036(2) Uani 1 1 d U . . C18 C 0.3847(9) 0.542(2) -0.0735(15) 0.048(3) Uani 1 1 d U . . H18 H 0.3724 0.5385 -0.0072 0.057 Uiso 1 1 calc R . . C19 C 0.4450(10) 0.594(2) -0.0904(17) 0.058(3) Uani 1 1 d U . . H19 H 0.4756 0.6238 -0.0381 0.069 Uiso 1 1 calc R . . C20 C 0.4606(10) 0.600(3) -0.1936(18) 0.063(4) Uani 1 1 d U . . H20 H 0.5020 0.6417 -0.2073 0.076 Uiso 1 1 calc R . . C21 C 0.4223(10) 0.554(3) -0.2683(17) 0.060(3) Uani 1 1 d U . . H21 H 0.4368 0.5555 -0.3334 0.073 Uiso 1 1 calc R . . C22 C 0.3560(10) 0.500(2) -0.2500(14) 0.046(3) Uani 1 1 d U . . H22 H 0.3262 0.4695 -0.3033 0.055 Uiso 1 1 calc R . . O9 O 0.2620(8) 0.3932(13) 0.1616(9) 0.057(4) Uani 1 1 d D . . H1W H 0.3017 0.4146 0.1530 0.085 Uiso 1 1 d RD . . H2W H 0.2590 0.3340 0.2112 0.085 Uiso 1 1 d RD . . 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 Pb1 0.0382(4) 0.0164(3) 0.0174(3) -0.00021(18) 0.0024(2) -0.0037(2) Pb2 0.0335(4) 0.0281(4) 0.0249(4) -0.0023(2) 0.0069(3) -0.0057(2) Pb3 0.0331(4) 0.0226(3) 0.0236(3) -0.0075(2) 0.0049(3) -0.0035(2) O1 0.024(5) 0.022(5) 0.016(4) 0.005(4) 0.000(4) 0.002(4) O2 0.023(5) 0.024(5) 0.018(4) 0.004(4) 0.004(4) 0.004(4) O3 0.031(6) 0.025(5) 0.021(5) 0.006(4) -0.003(4) 0.007(4) O4 0.011(5) 0.024(5) 0.031(5) 0.011(4) 0.010(4) 0.006(4) O5 0.043(7) 0.021(5) 0.020(5) -0.006(4) -0.005(4) -0.002(4) O6 0.056(8) 0.026(5) 0.018(5) -0.002(4) -0.006(5) -0.010(5) O7 0.025(6) 0.026(5) 0.027(5) -0.006(4) 0.007(4) 0.002(4) O8 0.015(5) 0.021(5) 0.025(5) -0.003(4) 0.007(4) -0.003(4) N1 0.028(5) 0.021(4) 0.014(4) 0.002(3) 0.003(4) -0.003(4) N2 0.029(5) 0.017(4) 0.015(4) 0.001(3) 0.001(4) 0.002(4) N3 0.034(5) 0.017(4) 0.020(5) -0.001(4) 0.000(4) -0.002(4) N4 0.029(5) 0.019(4) 0.021(4) -0.002(4) 0.005(4) -0.002(4) C1 0.032(4) 0.019(4) 0.018(4) -0.003(4) 0.001(4) 0.000(4) C2 0.033(5) 0.019(4) 0.007(4) 0.002(4) 0.004(4) 0.001(4) C3 0.030(5) 0.015(5) 0.009(4) 0.002(4) 0.003(4) -0.002(4) C4 0.042(7) 0.018(5) 0.005(5) 0.002(4) -0.007(5) -0.004(5) C5 0.020(7) 0.014(6) 0.023(7) -0.007(5) 0.006(6) -0.006(5) C6 0.031(5) 0.026(5) 0.022(5) -0.007(4) 0.000(4) 0.002(4) C7 0.042(6) 0.030(6) 0.034(6) 0.001(5) -0.003(5) 0.001(5) C8 0.047(6) 0.040(6) 0.042(6) 0.005(5) -0.003(5) 0.006(5) C9 0.041(6) 0.052(7) 0.056(7) 0.002(6) -0.006(6) 0.006(6) C10 0.030(6) 0.056(7) 0.055(7) 0.004(6) 0.010(6) 0.006(6) C11 0.031(5) 0.044(6) 0.044(6) 0.000(5) 0.006(5) 0.000(5) C12 0.031(5) 0.023(5) 0.023(5) -0.004(4) 0.003(4) -0.002(4) C13 0.026(5) 0.015(5) 0.017(5) 0.000(4) 0.004(4) 0.003(4) C14 0.034(5) 0.014(5) 0.020(5) 0.003(4) 0.004(4) -0.003(4) C15 0.030(8) 0.015(6) 0.021(7) 0.001(5) 0.002(6) -0.003(6) C16 0.027(8) 0.010(6) 0.018(6) 0.004(5) -0.002(6) 0.006(5) C17 0.033(5) 0.037(5) 0.037(5) -0.009(5) 0.003(4) -0.006(5) C18 0.036(6) 0.047(7) 0.059(6) -0.011(6) -0.004(5) -0.006(6) C19 0.035(6) 0.061(8) 0.076(7) -0.014(7) -0.003(6) -0.010(6) C20 0.037(7) 0.071(8) 0.083(8) -0.020(7) 0.017(6) -0.006(6) C21 0.044(7) 0.071(8) 0.069(7) -0.016(7) 0.025(6) -0.009(7) C22 0.036(6) 0.055(7) 0.050(6) -0.012(6) 0.019(5) -0.006(6) O9 0.110(12) 0.029(6) 0.032(6) 0.003(5) 0.013(7) -0.004(7) _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 Pb1 O4 2.361(9) 4_575 ? Pb1 O1 2.537(8) . ? Pb1 O2 2.665(9) . ? Pb1 O6 2.668(10) 1_565 ? Pb1 N2 2.710(11) 4_575 ? Pb2 O8 2.267(9) . ? Pb2 O1 2.475(9) . ? Pb2 O9 2.559(11) . ? Pb2 N1 2.565(10) . ? Pb2 N3 2.608(11) . ? Pb3 O3 2.362(9) 2_545 ? Pb3 O5 2.543(10) 4_566 ? Pb3 O7 2.607(9) . ? Pb3 O2 2.695(9) 2_545 ? O1 C4 1.258(17) . ? O2 C4 1.234(17) . ? O2 Pb3 2.695(9) 2 ? O3 C5 1.255(17) . ? O3 Pb3 2.362(9) 2 ? O4 C5 1.290(16) . ? O4 Pb1 2.361(9) 4_576 ? O5 C15 1.260(16) . ? O5 Pb3 2.543(10) 4_565 ? O6 C15 1.264(17) . ? O6 Pb1 2.668(10) 1_545 ? O7 C16 1.246(16) . ? O8 C16 1.295(15) . ? N1 C1 1.348(17) . ? N1 C2 1.360(18) . ? N2 C1 1.360(18) . ? N2 C3 1.371(17) . ? N2 Pb1 2.710(11) 4_576 ? N3 C14 1.360(18) . ? N3 C12 1.368(18) . ? N4 C13 1.342(17) . ? N4 C12 1.367(18) . ? C1 C6 1.45(2) . ? C2 C3 1.382(17) . ? C2 C4 1.492(17) . ? C3 C5 1.461(18) . ? C6 C7 1.41(2) . ? C6 C11 1.43(2) . ? C7 C8 1.34(2) . ? C7 H7 0.9300 . ? C8 C9 1.46(3) . ? C8 H8 0.9300 . ? C9 C10 1.40(3) . ? C9 H9 0.9300 . ? C10 C11 1.36(2) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.47(2) . ? C13 C14 1.417(18) . ? C13 C15 1.516(19) . ? C14 C16 1.470(19) . ? C17 C22 1.38(2) . ? C17 C18 1.41(2) . ? C18 C19 1.32(3) . ? C18 H18 0.9300 . ? C19 C20 1.43(3) . ? C19 H19 0.9300 . ? C20 C21 1.27(3) . ? C20 H20 0.9300 . ? C21 C22 1.44(3) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? O9 H1W 0.8311 . ? O9 H2W 0.8296 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Pb1 O1 81.7(3) 4_575 . ? O4 Pb1 O2 75.9(3) 4_575 . ? O1 Pb1 O2 49.2(3) . . ? O4 Pb1 O6 80.1(3) 4_575 1_565 ? O1 Pb1 O6 137.6(3) . 1_565 ? O2 Pb1 O6 153.5(3) . 1_565 ? O4 Pb1 N2 66.7(3) 4_575 4_575 ? O1 Pb1 N2 67.6(3) . 4_575 ? O2 Pb1 N2 109.6(3) . 4_575 ? O6 Pb1 N2 70.1(3) 1_565 4_575 ? O8 Pb2 O1 73.2(3) . . ? O8 Pb2 O9 76.6(4) . . ? O1 Pb2 O9 132.9(4) . . ? O8 Pb2 N1 82.1(3) . . ? O1 Pb2 N1 63.9(3) . . ? O9 Pb2 N1 77.0(4) . . ? O8 Pb2 N3 66.0(4) . . ? O1 Pb2 N3 124.7(3) . . ? O9 Pb2 N3 70.9(4) . . ? N1 Pb2 N3 138.7(3) . . ? O3 Pb3 O5 71.4(3) 2_545 4_566 ? O3 Pb3 O7 76.3(3) 2_545 . ? O5 Pb3 O7 77.4(3) 4_566 . ? O3 Pb3 O2 68.7(3) 2_545 2_545 ? O5 Pb3 O2 113.7(3) 4_566 2_545 ? O7 Pb3 O2 136.1(3) . 2_545 ? C4 O1 Pb2 118.8(8) . . ? C4 O1 Pb1 97.7(8) . . ? Pb2 O1 Pb1 135.6(4) . . ? C4 O2 Pb1 92.2(7) . . ? C4 O2 Pb3 144.9(8) . 2 ? Pb1 O2 Pb3 122.8(3) . 2 ? C5 O3 Pb3 129.2(8) . 2 ? C5 O4 Pb1 117.4(8) . 4_576 ? C15 O5 Pb3 102.9(9) . 4_565 ? C15 O6 Pb1 117.1(9) . 1_545 ? C16 O7 Pb3 100.0(8) . . ? C16 O8 Pb2 127.2(8) . . ? C1 N1 C2 106.2(11) . . ? C1 N1 Pb2 136.6(9) . . ? C2 N1 Pb2 110.0(8) . . ? C1 N2 C3 103.9(11) . . ? C1 N2 Pb1 144.4(8) . 4_576 ? C3 N2 Pb1 105.9(8) . 4_576 ? C14 N3 C12 104.8(11) . . ? C14 N3 Pb2 112.8(8) . . ? C12 N3 Pb2 142.4(10) . . ? C13 N4 C12 106.9(11) . . ? N1 C1 N2 112.7(12) . . ? N1 C1 C6 123.1(13) . . ? N2 C1 C6 124.2(12) . . ? N1 C2 C3 107.5(11) . . ? N1 C2 C4 116.9(11) . . ? C3 C2 C4 135.2(13) . . ? N2 C3 C2 109.7(12) . . ? N2 C3 C5 119.5(11) . . ? C2 C3 C5 130.7(12) . . ? O2 C4 O1 120.8(11) . . ? O2 C4 C2 123.1(12) . . ? O1 C4 C2 116.1(13) . . ? O3 C5 O4 118.2(12) . . ? O3 C5 C3 120.3(12) . . ? O4 C5 C3 120.9(12) . . ? C7 C6 C11 115.2(15) . . ? C7 C6 C1 122.6(14) . . ? C11 C6 C1 122.1(13) . . ? C8 C7 C6 123.1(17) . . ? C8 C7 H7 118.4 . . ? C6 C7 H7 118.4 . . ? C7 C8 C9 120.7(17) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 116.7(17) . . ? C10 C9 H9 121.7 . . ? C8 C9 H9 121.7 . . ? C11 C10 C9 121.0(18) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C6 123.0(16) . . ? C10 C11 H11 118.5 . . ? C6 C11 H11 118.5 . . ? N4 C12 N3 111.8(13) . . ? N4 C12 C17 124.0(13) . . ? N3 C12 C17 124.2(13) . . ? N4 C13 C14 107.3(12) . . ? N4 C13 C15 119.6(11) . . ? C14 C13 C15 133.1(13) . . ? N3 C14 C13 109.2(12) . . ? N3 C14 C16 116.1(11) . . ? C13 C14 C16 134.1(13) . . ? O5 C15 O6 124.0(13) . . ? O5 C15 C13 116.3(12) . . ? O6 C15 C13 119.6(12) . . ? O7 C16 O8 120.0(12) . . ? O7 C16 C14 122.7(12) . . ? O8 C16 C14 117.3(12) . . ? C22 C17 C18 118.3(17) . . ? C22 C17 C12 119.4(15) . . ? C18 C17 C12 122.1(15) . . ? C19 C18 C17 123(2) . . ? C19 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C18 C19 C20 116.1(19) . . ? C18 C19 H19 122.0 . . ? C20 C19 H19 122.0 . . ? C21 C20 C19 125(2) . . ? C21 C20 H20 117.4 . . ? C19 C20 H20 117.4 . . ? C20 C21 C22 119(2) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C17 C22 C21 118.6(18) . . ? C17 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? Pb2 O9 H1W 80.7 . . ? Pb2 O9 H2W 142.0 . . ? H1W O9 H2W 111.1 . . ? 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 O8 Pb2 O1 C4 59.9(9) . . . . ? O9 Pb2 O1 C4 7.7(11) . . . . ? N1 Pb2 O1 C4 -29.4(9) . . . . ? N3 Pb2 O1 C4 103.3(9) . . . . ? O8 Pb2 O1 Pb1 -81.3(5) . . . . ? O9 Pb2 O1 Pb1 -133.6(6) . . . . ? N1 Pb2 O1 Pb1 -170.6(7) . . . . ? N3 Pb2 O1 Pb1 -37.9(7) . . . . ? O4 Pb1 O1 C4 -76.2(8) 4_575 . . . ? O2 Pb1 O1 C4 2.4(7) . . . . ? O6 Pb1 O1 C4 -141.5(8) 1_565 . . . ? N2 Pb1 O1 C4 -144.4(8) 4_575 . . . ? O4 Pb1 O1 Pb2 70.2(5) 4_575 . . . ? O2 Pb1 O1 Pb2 148.7(7) . . . . ? O6 Pb1 O1 Pb2 4.8(8) 1_565 . . . ? N2 Pb1 O1 Pb2 2.0(5) 4_575 . . . ? O4 Pb1 O2 C4 88.7(8) 4_575 . . . ? O1 Pb1 O2 C4 -2.4(7) . . . . ? O6 Pb1 O2 C4 114.6(9) 1_565 . . . ? N2 Pb1 O2 C4 30.2(9) 4_575 . . . ? O4 Pb1 O2 Pb3 -94.3(5) 4_575 . . 2 ? O1 Pb1 O2 Pb3 174.6(6) . . . 2 ? O6 Pb1 O2 Pb3 -68.4(9) 1_565 . . 2 ? N2 Pb1 O2 Pb3 -152.8(4) 4_575 . . 2 ? O3 Pb3 O7 C16 -130.4(8) 2_545 . . . ? O5 Pb3 O7 C16 -56.8(8) 4_566 . . . ? O2 Pb3 O7 C16 -167.9(7) 2_545 . . . ? O1 Pb2 O8 C16 143.5(10) . . . . ? O9 Pb2 O8 C16 -73.0(10) . . . . ? N1 Pb2 O8 C16 -151.4(10) . . . . ? N3 Pb2 O8 C16 1.8(9) . . . . ? O8 Pb2 N1 C1 100.3(13) . . . . ? O1 Pb2 N1 C1 175.3(14) . . . . ? O9 Pb2 N1 C1 22.3(13) . . . . ? N3 Pb2 N1 C1 61.6(15) . . . . ? O8 Pb2 N1 C2 -44.3(8) . . . . ? O1 Pb2 N1 C2 30.8(8) . . . . ? O9 Pb2 N1 C2 -122.3(9) . . . . ? N3 Pb2 N1 C2 -83.0(10) . . . . ? O8 Pb2 N3 C14 -5.7(8) . . . . ? O1 Pb2 N3 C14 -51.8(9) . . . . ? O9 Pb2 N3 C14 77.7(9) . . . . ? N1 Pb2 N3 C14 36.9(11) . . . . ? O8 Pb2 N3 C12 175.9(16) . . . . ? O1 Pb2 N3 C12 129.8(15) . . . . ? O9 Pb2 N3 C12 -100.7(16) . . . . ? N1 Pb2 N3 C12 -141.5(14) . . . . ? C2 N1 C1 N2 1.8(15) . . . . ? Pb2 N1 C1 N2 -143.6(10) . . . . ? C2 N1 C1 C6 -175.6(12) . . . . ? Pb2 N1 C1 C6 39(2) . . . . ? C3 N2 C1 N1 -0.6(14) . . . . ? Pb1 N2 C1 N1 145.7(11) 4_576 . . . ? C3 N2 C1 C6 176.8(12) . . . . ? Pb1 N2 C1 C6 -37(2) 4_576 . . . ? C1 N1 C2 C3 -2.3(14) . . . . ? Pb2 N1 C2 C3 153.2(8) . . . . ? C1 N1 C2 C4 171.0(11) . . . . ? Pb2 N1 C2 C4 -33.5(13) . . . . ? C1 N2 C3 C2 -0.8(14) . . . . ? Pb1 N2 C3 C2 -161.2(9) 4_576 . . . ? C1 N2 C3 C5 175.6(11) . . . . ? Pb1 N2 C3 C5 15.3(13) 4_576 . . . ? N1 C2 C3 N2 2.0(14) . . . . ? C4 C2 C3 N2 -169.5(14) . . . . ? N1 C2 C3 C5 -174.0(12) . . . . ? C4 C2 C3 C5 15(3) . . . . ? Pb1 O2 C4 O1 4.2(13) . . . . ? Pb3 O2 C4 O1 -171.4(9) 2 . . . ? Pb1 O2 C4 C2 -177.3(11) . . . . ? Pb3 O2 C4 C2 7(2) 2 . . . ? Pb2 O1 C4 O2 -158.2(10) . . . . ? Pb1 O1 C4 O2 -4.5(14) . . . . ? Pb2 O1 C4 C2 23.3(14) . . . . ? Pb1 O1 C4 C2 177.0(9) . . . . ? N1 C2 C4 O2 -169.4(12) . . . . ? C3 C2 C4 O2 1(2) . . . . ? N1 C2 C4 O1 9.1(17) . . . . ? C3 C2 C4 O1 179.9(14) . . . . ? Pb3 O3 C5 O4 99.9(13) 2 . . . ? Pb3 O3 C5 C3 -88.3(14) 2 . . . ? Pb1 O4 C5 O3 140.4(9) 4_576 . . . ? Pb1 O4 C5 C3 -31.3(15) 4_576 . . . ? N2 C3 C5 O3 -164.0(11) . . . . ? C2 C3 C5 O3 12(2) . . . . ? N2 C3 C5 O4 7.7(18) . . . . ? C2 C3 C5 O4 -176.7(13) . . . . ? N1 C1 C6 C7 -169.9(13) . . . . ? N2 C1 C6 C7 13(2) . . . . ? N1 C1 C6 C11 13(2) . . . . ? N2 C1 C6 C11 -164.5(13) . . . . ? C11 C6 C7 C8 1(2) . . . . ? C1 C6 C7 C8 -176.8(15) . . . . ? C6 C7 C8 C9 -6(3) . . . . ? C7 C8 C9 C10 7(3) . . . . ? C8 C9 C10 C11 -4(3) . . . . ? C9 C10 C11 C6 -1(3) . . . . ? C7 C6 C11 C10 3(2) . . . . ? C1 C6 C11 C10 -179.7(16) . . . . ? C13 N4 C12 N3 1.7(16) . . . . ? C13 N4 C12 C17 -178.5(14) . . . . ? C14 N3 C12 N4 -1.5(16) . . . . ? Pb2 N3 C12 N4 177.0(10) . . . . ? C14 N3 C12 C17 178.8(14) . . . . ? Pb2 N3 C12 C17 -3(2) . . . . ? C12 N4 C13 C14 -1.2(15) . . . . ? C12 N4 C13 C15 179.9(12) . . . . ? C12 N3 C14 C13 0.7(14) . . . . ? Pb2 N3 C14 C13 -178.4(8) . . . . ? C12 N3 C14 C16 -172.1(11) . . . . ? Pb2 N3 C14 C16 8.9(14) . . . . ? N4 C13 C14 N3 0.4(15) . . . . ? C15 C13 C14 N3 179.0(13) . . . . ? N4 C13 C14 C16 171.3(13) . . . . ? C15 C13 C14 C16 -10(3) . . . . ? Pb3 O5 C15 O6 0.1(16) 4_565 . . . ? Pb3 O5 C15 C13 177.5(9) 4_565 . . . ? Pb1 O6 C15 O5 136.6(12) 1_545 . . . ? Pb1 O6 C15 C13 -40.7(15) 1_545 . . . ? N4 C13 C15 O5 -16.4(19) . . . . ? C14 C13 C15 O5 165.1(14) . . . . ? N4 C13 C15 O6 161.2(13) . . . . ? C14 C13 C15 O6 -17(2) . . . . ? Pb3 O7 C16 O8 -18.0(12) . . . . ? Pb3 O7 C16 C14 160.9(10) . . . . ? Pb2 O8 C16 O7 -178.7(8) . . . . ? Pb2 O8 C16 C14 2.3(15) . . . . ? N3 C14 C16 O7 173.1(12) . . . . ? C13 C14 C16 O7 3(2) . . . . ? N3 C14 C16 O8 -8.0(16) . . . . ? C13 C14 C16 O8 -178.4(13) . . . . ? N4 C12 C17 C22 32(2) . . . . ? N3 C12 C17 C22 -148.0(16) . . . . ? N4 C12 C17 C18 -151.9(16) . . . . ? N3 C12 C17 C18 28(2) . . . . ? C22 C17 C18 C19 0(3) . . . . ? C12 C17 C18 C19 -176.2(18) . . . . ? C17 C18 C19 C20 1(3) . . . . ? C18 C19 C20 C21 -3(4) . . . . ? C19 C20 C21 C22 4(4) . . . . ? C18 C17 C22 C21 1(3) . . . . ? C12 C17 C22 C21 177.0(17) . . . . ? C20 C21 C22 C17 -3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H2W N4 0.83 2.06 2.866(16) 165.2 4_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.863 _refine_diff_density_min -2.498 _refine_diff_density_rms 0.545 # Attachment '- complex 4.cif' data_f _database_code_depnum_ccdc_archive 'CCDC 809971' #TrackingRef '- complex 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 N4 O14 Sr' _chemical_formula_weight 658.09 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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 27.280(3) _cell_length_b 31.413(4) _cell_length_c 6.6156(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5669.2(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5023 _cell_measurement_theta_min 2.5936 _cell_measurement_theta_max 27.3504 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 1.976 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6817 _exptl_absorpt_correction_T_max 0.7428 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10814 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3182 _reflns_number_gt 2869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0133P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(5) _refine_ls_number_reflns 3182 _refine_ls_number_parameters 187 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Sr1 Sr 0.7500 0.7500 0.12585(6) 0.02019(7) Uani 1 2 d S . . O1 O 0.57704(6) 0.54118(5) -0.0070(3) 0.0399(5) Uani 1 1 d . . . O2 O 0.58069(7) 0.60161(5) -0.1794(3) 0.0450(5) Uani 1 1 d . . . O3 O 0.62396(8) 0.66954(5) -0.1543(3) 0.0540(6) Uani 1 1 d . . . H3 H 0.6092 0.6468 -0.1550 0.081 Uiso 1 1 calc R . . O4 O 0.68262(7) 0.69950(5) 0.0227(3) 0.0449(5) Uani 1 1 d . . . O5 O 0.78382(7) 0.70767(5) -0.1994(3) 0.0367(5) Uani 1 1 d . . . H5B H 0.8087 0.7215 -0.2400 0.055 Uiso 1 1 d R . . H5A H 0.7933 0.6835 -0.1568 0.055 Uiso 1 1 d R . . O6 O 0.72497(7) 0.70464(5) 0.4383(3) 0.0342(4) Uani 1 1 d . . . H6A H 0.7373 0.7032 0.5562 0.051 Uiso 1 1 d R . . H6B H 0.7175 0.6795 0.4018 0.051 Uiso 1 1 d R . . O7 O 0.60740(6) 0.49165(4) 0.3642(4) 0.0444(5) Uani 1 1 d . . . H7A H 0.6212 0.4717 0.4299 0.067 Uiso 1 1 d R . . H7B H 0.5897 0.4819 0.2693 0.067 Uiso 1 1 d R . . N1 N 0.68999(7) 0.62882(5) 0.2778(3) 0.0332(4) Uani 1 1 d . . . N2 N 0.64867(7) 0.56866(5) 0.2625(3) 0.0290(4) Uani 1 1 d . . . H2A H 0.6388 0.5434 0.2919 0.035 Uiso 1 1 calc R . . C1 C 0.59398(10) 0.57729(7) -0.0331(4) 0.0304(6) Uani 1 1 d . . . C2 C 0.63170(8) 0.59315(6) 0.1077(4) 0.0266(5) Uani 1 1 d . . . C3 C 0.65816(8) 0.63043(6) 0.1206(4) 0.0301(5) Uani 1 1 d . . . C4 C 0.65577(10) 0.66953(7) -0.0096(4) 0.0348(6) Uani 1 1 d . . . C5 C 0.68347(8) 0.59067(6) 0.3614(4) 0.0302(5) Uani 1 1 d . . . C6 C 0.71063(10) 0.57486(7) 0.5366(4) 0.0365(6) Uani 1 1 d . . . C7 C 0.75810(12) 0.59035(9) 0.5676(5) 0.0595(10) Uani 1 1 d . . . H7 H 0.7716 0.6099 0.4779 0.071 Uiso 1 1 calc R . . C8 C 0.78480(15) 0.57634(11) 0.7331(7) 0.0798(14) Uani 1 1 d . . . H8 H 0.8163 0.5866 0.7548 0.096 Uiso 1 1 calc R . . C9 C 0.76511(16) 0.54751(11) 0.8646(6) 0.0793(11) Uani 1 1 d . . . H9 H 0.7832 0.5387 0.9762 0.095 Uiso 1 1 calc R . . C10 C 0.71852(14) 0.53133(9) 0.8334(4) 0.0604(9) Uani 1 1 d . . . H10 H 0.7053 0.5115 0.9223 0.072 Uiso 1 1 calc R . . C11 C 0.69196(10) 0.54514(7) 0.6680(4) 0.0432(6) Uani 1 1 d . . . H11 H 0.6608 0.5341 0.6452 0.052 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 Sr1 0.02011(12) 0.01612(10) 0.02434(11) 0.000 0.000 -0.00004(13) O1 0.0425(11) 0.0333(8) 0.0440(11) 0.0109(8) -0.0138(9) -0.0198(8) O2 0.0543(12) 0.0362(9) 0.0446(11) 0.0141(8) -0.0276(9) -0.0178(8) O3 0.0704(14) 0.0341(8) 0.0575(13) 0.0232(9) -0.0377(12) -0.0270(9) O4 0.0518(12) 0.0323(9) 0.0507(12) 0.0135(8) -0.0215(10) -0.0209(8) O5 0.0399(11) 0.0348(8) 0.0354(11) -0.0018(8) -0.0079(8) 0.0059(7) O6 0.0464(11) 0.0252(8) 0.0309(11) 0.0040(7) -0.0068(8) -0.0055(7) O7 0.0502(10) 0.0354(9) 0.0475(11) 0.0189(11) -0.0154(12) -0.0095(7) N1 0.0381(11) 0.0256(8) 0.0361(11) 0.0071(8) -0.0170(10) -0.0078(8) N2 0.0354(11) 0.0231(8) 0.0284(10) 0.0081(7) -0.0097(9) -0.0077(8) C1 0.0271(14) 0.0327(12) 0.0314(13) 0.0041(10) -0.0076(11) -0.0093(10) C2 0.0277(11) 0.0229(9) 0.0293(12) 0.0065(10) -0.0086(10) -0.0069(8) C3 0.0329(12) 0.0254(9) 0.0320(11) 0.0047(10) -0.0099(12) -0.0075(9) C4 0.0394(16) 0.0308(12) 0.0343(14) 0.0144(11) -0.0108(12) -0.0070(11) C5 0.0348(12) 0.0249(9) 0.0309(12) 0.0031(9) -0.0079(11) -0.0031(9) C6 0.0463(18) 0.0280(12) 0.0353(15) -0.0001(11) -0.0165(13) 0.0020(11) C7 0.069(2) 0.0493(15) 0.060(2) 0.0145(13) -0.0369(18) -0.0090(14) C8 0.082(3) 0.067(2) 0.091(3) 0.011(2) -0.059(3) -0.0048(19) C9 0.113(3) 0.066(2) 0.058(2) 0.0052(18) -0.051(2) 0.021(2) C10 0.088(3) 0.0556(16) 0.0371(17) 0.0125(13) -0.0094(16) 0.0140(16) C11 0.0545(17) 0.0423(13) 0.0327(14) 0.0054(10) -0.0080(12) 0.0052(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O4 2.5221(17) . ? Sr1 O4 2.5221(17) 14_665 ? Sr1 O1 2.5867(16) 4_655 ? Sr1 O1 2.5867(16) 3_565 ? Sr1 O6 2.6017(17) 14_665 ? Sr1 O6 2.6017(17) . ? Sr1 O5 2.6926(19) 14_665 ? Sr1 O5 2.6926(19) . ? O1 C1 1.237(3) . ? O1 Sr1 2.5867(16) 11_464 ? O2 C1 1.285(3) . ? O3 C4 1.292(3) . ? O3 H3 0.8200 . ? O4 C4 1.212(3) . ? O5 H5B 0.8504 . ? O5 H5A 0.8500 . ? O6 H6A 0.8501 . ? O6 H6B 0.8497 . ? O7 H7A 0.8499 . ? O7 H7B 0.8500 . ? N1 C5 1.332(3) . ? N1 C3 1.356(3) . ? N2 C5 1.345(3) . ? N2 C2 1.362(3) . ? N2 H2A 0.8600 . ? C1 C2 1.475(3) . ? C2 C3 1.378(3) . ? C3 C4 1.501(3) . ? C5 C6 1.462(3) . ? C6 C11 1.374(4) . ? C6 C7 1.398(4) . ? C7 C8 1.387(5) . ? C7 H7 0.9300 . ? C8 C9 1.365(6) . ? C8 H8 0.9300 . ? C9 C10 1.384(5) . ? C9 H9 0.9300 . ? C10 C11 1.382(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Sr1 O4 148.61(9) . 14_665 ? O4 Sr1 O1 78.67(6) . 4_655 ? O4 Sr1 O1 111.01(6) 14_665 4_655 ? O4 Sr1 O1 111.01(6) . 3_565 ? O4 Sr1 O1 78.67(6) 14_665 3_565 ? O1 Sr1 O1 145.14(9) 4_655 3_565 ? O4 Sr1 O6 138.65(6) . 14_665 ? O4 Sr1 O6 71.29(6) 14_665 14_665 ? O1 Sr1 O6 72.62(6) 4_655 14_665 ? O1 Sr1 O6 79.79(5) 3_565 14_665 ? O4 Sr1 O6 71.29(6) . . ? O4 Sr1 O6 138.65(6) 14_665 . ? O1 Sr1 O6 79.79(5) 4_655 . ? O1 Sr1 O6 72.62(6) 3_565 . ? O6 Sr1 O6 74.79(8) 14_665 . ? O4 Sr1 O5 81.06(6) . 14_665 ? O4 Sr1 O5 73.91(6) 14_665 14_665 ? O1 Sr1 O5 73.38(6) 4_655 14_665 ? O1 Sr1 O5 139.89(6) 3_565 14_665 ? O6 Sr1 O5 117.03(4) 14_665 14_665 ? O6 Sr1 O5 144.63(5) . 14_665 ? O4 Sr1 O5 73.91(6) . . ? O4 Sr1 O5 81.06(6) 14_665 . ? O1 Sr1 O5 139.89(6) 4_655 . ? O1 Sr1 O5 73.38(6) 3_565 . ? O6 Sr1 O5 144.63(5) 14_665 . ? O6 Sr1 O5 117.03(5) . . ? O5 Sr1 O5 73.89(8) 14_665 . ? C1 O1 Sr1 136.09(16) . 11_464 ? C4 O3 H3 109.5 . . ? C4 O4 Sr1 167.65(17) . . ? Sr1 O5 H5B 105.9 . . ? Sr1 O5 H5A 106.3 . . ? H5B O5 H5A 108.6 . . ? Sr1 O6 H6A 130.9 . . ? Sr1 O6 H6B 110.2 . . ? H6A O6 H6B 107.8 . . ? H7A O7 H7B 111.3 . . ? C5 N1 C3 105.47(17) . . ? C5 N2 C2 108.40(16) . . ? C5 N2 H2A 125.8 . . ? C2 N2 H2A 125.8 . . ? O1 C1 O2 123.0(2) . . ? O1 C1 C2 118.8(2) . . ? O2 C1 C2 118.15(19) . . ? N2 C2 C3 104.79(19) . . ? N2 C2 C1 121.43(17) . . ? C3 C2 C1 133.8(2) . . ? N1 C3 C2 110.56(19) . . ? N1 C3 C4 119.89(19) . . ? C2 C3 C4 129.5(2) . . ? O4 C4 O3 122.4(2) . . ? O4 C4 C3 120.5(2) . . ? O3 C4 C3 117.0(2) . . ? N1 C5 N2 110.8(2) . . ? N1 C5 C6 124.5(2) . . ? N2 C5 C6 124.68(19) . . ? C11 C6 C7 119.2(3) . . ? C11 C6 C5 123.0(2) . . ? C7 C6 C5 117.8(2) . . ? C8 C7 C6 119.4(3) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.6(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 119.0(3) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C6 C11 C10 121.3(3) . . ? C6 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Sr1 O4 C4 115.4(10) 14_665 . . . ? O1 Sr1 O4 C4 -132.7(10) 4_655 . . . ? O1 Sr1 O4 C4 12.3(10) 3_565 . . . ? O6 Sr1 O4 C4 -86.2(10) 14_665 . . . ? O6 Sr1 O4 C4 -49.8(10) . . . . ? O5 Sr1 O4 C4 152.6(10) 14_665 . . . ? O5 Sr1 O4 C4 76.9(10) . . . . ? Sr1 O1 C1 O2 -19.0(4) 11_464 . . . ? Sr1 O1 C1 C2 161.93(17) 11_464 . . . ? C5 N2 C2 C3 0.0(3) . . . . ? C5 N2 C2 C1 178.3(2) . . . . ? O1 C1 C2 N2 1.2(4) . . . . ? O2 C1 C2 N2 -178.0(2) . . . . ? O1 C1 C2 C3 178.8(3) . . . . ? O2 C1 C2 C3 -0.3(4) . . . . ? C5 N1 C3 C2 0.3(3) . . . . ? C5 N1 C3 C4 -179.8(2) . . . . ? N2 C2 C3 N1 -0.2(3) . . . . ? C1 C2 C3 N1 -178.1(3) . . . . ? N2 C2 C3 C4 179.9(3) . . . . ? C1 C2 C3 C4 2.0(5) . . . . ? Sr1 O4 C4 O3 -156.8(8) . . . . ? Sr1 O4 C4 C3 23.6(12) . . . . ? N1 C3 C4 O4 1.1(4) . . . . ? C2 C3 C4 O4 -179.0(3) . . . . ? N1 C3 C4 O3 -178.5(2) . . . . ? C2 C3 C4 O3 1.4(5) . . . . ? C3 N1 C5 N2 -0.3(3) . . . . ? C3 N1 C5 C6 179.6(2) . . . . ? C2 N2 C5 N1 0.2(3) . . . . ? C2 N2 C5 C6 -179.7(2) . . . . ? N1 C5 C6 C11 152.9(3) . . . . ? N2 C5 C6 C11 -27.3(4) . . . . ? N1 C5 C6 C7 -28.4(4) . . . . ? N2 C5 C6 C7 151.4(3) . . . . ? C11 C6 C7 C8 -1.8(5) . . . . ? C5 C6 C7 C8 179.5(3) . . . . ? C6 C7 C8 C9 0.3(6) . . . . ? C7 C8 C9 C10 0.9(6) . . . . ? C8 C9 C10 C11 -0.7(5) . . . . ? C7 C6 C11 C10 2.1(4) . . . . ? C5 C6 C11 C10 -179.2(2) . . . . ? C9 C10 C11 C6 -0.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.63 2.444(2) 174.6 . O6 H6B N1 0.85 1.94 2.777(2) 166.8 . N2 H2A O7 0.86 1.90 2.752(2) 171.1 . O5 H5A O2 0.85 2.13 2.880(2) 147.6 3_565 O5 H5B O7 0.85 2.01 2.843(3) 167.2 3_564 O6 H6A O5 0.85 2.06 2.886(2) 163.6 1_556 O7 H7A O3 0.85 1.98 2.781(2) 157.4 8_645 O7 H7B O6 0.85 2.03 2.785(3) 147.2 8_644 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.367 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.050