# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jhy-Der Chen' _publ_contact_author_email jdchen@cycu.edu.tw loop_ _publ_author_name 'Ming-Jhe Sie' 'Yin-Jui Chang' 'Po-Wen Cheng' 'Po-Ting Kuo' 'Chun-Wei Yeh' 'Chi-Feng Cheng' 'Jhy-Der Chen' 'Ju-Chun Wang' data_1 _database_code_depnum_ccdc_archive 'CCDC 866971' #TrackingRef '- all-2nd-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 Cd N4 O6' _chemical_formula_weight 650.95 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.5232(6) _cell_length_b 21.1310(9) _cell_length_c 16.0399(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.615(2) _cell_angle_gamma 90.00 _cell_volume 4784.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8543 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.904 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5909 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _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 'Bruker AXS APEX2' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40267 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9400 _reflns_number_gt 5247 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0403P)^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 9400 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1112 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Cd Cd 0.447397(18) 0.325686(14) 0.629317(17) 0.04623(11) Uani 1 1 d . . . O1 O 0.3655(5) 0.6687(3) 0.6797(4) 0.0725(19) Uiso 0.50 1 d P A 1 O2 O 0.5228(6) 0.9783(4) 0.6556(6) 0.103(3) Uiso 0.50 1 d P A 1 O1' O 0.3322(6) 0.6679(3) 0.6350(5) 0.091(2) Uiso 0.50 1 d P B 2 O2' O 0.5152(8) 0.9796(4) 0.6022(7) 0.135(3) Uiso 0.50 1 d P B 2 O3 O 0.60052(16) 0.32663(13) 0.73792(16) 0.0570(7) Uani 1 1 d . . . O4 O 0.59880(17) 0.31265(13) 0.60209(16) 0.0599(8) Uani 1 1 d . . . O5 O 0.29131(18) 0.33588(15) 0.55863(18) 0.0766(9) Uani 1 1 d . . . O6 O 0.37983(18) 0.33256(13) 0.46624(16) 0.0654(8) Uani 1 1 d . . . N1 N 0.4588(3) 0.43452(16) 0.6347(2) 0.0570(9) Uani 1 1 d . . . N2 N 0.4780(3) 0.63040(17) 0.6187(2) 0.0672(10) Uani 1 1 d . . . H2A H 0.5210 0.6420 0.5931 0.081 Uiso 1 1 calc R C 1 N3 N 0.3804(9) 1.0252(6) 0.6521(7) 0.100(4) Uiso 0.50 1 d P A 1 H3A H 0.3279 1.0172 0.6662 0.120 Uiso 0.50 1 calc PR A 1 N3' N 0.3748(9) 1.0251(6) 0.6160(8) 0.115(5) Uiso 0.50 1 d P B 2 H3'A H 0.3167 1.0145 0.6114 0.138 Uiso 0.50 1 calc PR B 2 N4 N 0.4308(3) 1.21831(18) 0.6321(2) 0.0706(11) Uani 1 1 d . . . C1 C 0.3951(3) 0.4724(2) 0.6539(3) 0.0759(14) Uani 1 1 d . . . H1A H 0.3446 0.4534 0.6706 0.091 Uiso 1 1 calc R . . C2 C 0.3960(3) 0.5363(2) 0.6515(3) 0.0791(15) Uani 1 1 d . . . H2B H 0.3481 0.5597 0.6666 0.095 Uiso 1 1 calc R A . C3 C 0.4688(3) 0.5661(2) 0.6265(3) 0.0552(11) Uani 1 1 d . . . C4 C 0.5387(3) 0.5271(2) 0.6077(3) 0.0755(14) Uani 1 1 d . . . H4B H 0.5909 0.5448 0.5923 0.091 Uiso 1 1 calc R A . C5 C 0.5306(3) 0.4628(2) 0.6119(3) 0.0729(14) Uani 1 1 d . . . H5A H 0.5776 0.4377 0.5982 0.087 Uiso 1 1 calc R . . C6 C 0.4324(9) 0.6757(6) 0.6436(7) 0.064(3) Uiso 0.50 1 d P A 1 C7 C 0.4688(10) 0.7420(7) 0.6262(10) 0.098(5) Uiso 0.50 1 d P A 1 H7A H 0.5321 0.7480 0.6618 0.117 Uiso 0.50 1 calc PR A 1 H7B H 0.4726 0.7445 0.5667 0.117 Uiso 0.50 1 calc PR A 1 C8 C 0.4044(9) 0.7948(6) 0.6446(8) 0.080(4) Uiso 0.50 1 d P A 1 H8A H 0.3965 0.7919 0.7029 0.120 Uiso 0.50 1 calc PR A 1 H8B H 0.3426 0.7928 0.6051 0.120 Uiso 0.50 1 calc PR A 1 C9 C 0.4606(13) 0.8609(9) 0.6305(12) 0.134(7) Uiso 0.50 1 d P A 1 H9A H 0.5246 0.8618 0.6660 0.161 Uiso 0.50 1 calc PR A 1 H9B H 0.4622 0.8669 0.5709 0.161 Uiso 0.50 1 calc PR A 1 C10 C 0.3951(10) 0.9117(7) 0.6607(10) 0.112(5) Uiso 0.50 1 d P A 1 H10A H 0.3308 0.9093 0.6257 0.135 Uiso 0.50 1 calc PR A 1 H10B H 0.3937 0.9048 0.7202 0.135 Uiso 0.50 1 calc PR A 1 C11 C 0.4390(10) 0.9758(6) 0.6499(8) 0.082(4) Uiso 0.50 1 d P A 1 C6' C 0.4042(11) 0.6792(6) 0.6184(8) 0.079(4) Uiso 0.50 1 d P B 2 C7' C 0.4392(9) 0.7421(6) 0.6005(9) 0.074(4) Uiso 0.50 1 d P B 2 H7'A H 0.4999 0.7490 0.6403 0.089 Uiso 0.50 1 calc PR B 2 H7'B H 0.4506 0.7411 0.5433 0.089 Uiso 0.50 1 calc PR B 2 C8' C 0.3824(12) 0.7936(8) 0.6052(10) 0.136(6) Uiso 0.50 1 d P B 2 H8'A H 0.3596 0.7900 0.6572 0.163 Uiso 0.50 1 calc PR B 2 H8'B H 0.3276 0.7919 0.5571 0.163 Uiso 0.50 1 calc PR B 2 C9' C 0.4288(10) 0.8579(7) 0.6050(9) 0.083(4) Uiso 0.50 1 d P B 2 H9'A H 0.4861 0.8576 0.6506 0.100 Uiso 0.50 1 calc PR B 2 H9'B H 0.4484 0.8615 0.5514 0.100 Uiso 0.50 1 calc PR B 2 C10' C 0.3801(12) 0.9121(8) 0.6143(10) 0.138(6) Uiso 0.50 1 d P B 2 H10C H 0.3648 0.9111 0.6700 0.166 Uiso 0.50 1 calc PR B 2 H10D H 0.3208 0.9121 0.5711 0.166 Uiso 0.50 1 calc PR B 2 C11' C 0.4359(12) 0.9783(8) 0.6062(10) 0.113(5) Uiso 0.50 1 d P B 2 C12 C 0.3984(5) 1.0894(2) 0.6331(4) 0.109(2) Uani 1 1 d . . . C13 C 0.3337(9) 1.1305(6) 0.6647(8) 0.088(4) Uiso 0.50 1 d P A 1 H13A H 0.2846 1.1149 0.6870 0.106 Uiso 0.50 1 calc PR A 1 C13' C 0.3251(9) 1.1323(6) 0.6250(8) 0.085(4) Uiso 0.50 1 d P A 2 H13B H 0.2633 1.1190 0.6216 0.101 Uiso 0.50 1 calc PR A 2 C14 C 0.3507(7) 1.1939(5) 0.6591(6) 0.059(3) Uiso 0.50 1 d P A 1 H14A H 0.3081 1.2224 0.6736 0.088 Uiso 0.50 1 calc PR A 1 C14' C 0.3469(10) 1.1953(6) 0.6224(8) 0.088(4) Uiso 0.50 1 d P A 2 H14B H 0.2968 1.2238 0.6127 0.106 Uiso 0.50 1 calc PR A 2 C15 C 0.4954(4) 1.1777(3) 0.6250(4) 0.0935(17) Uani 1 1 d . A . H15A H 0.5533 1.1936 0.6194 0.112 Uiso 1 1 calc R . . C16 C 0.4852(4) 1.1125(3) 0.6250(4) 0.108(2) Uani 1 1 d . A . H16A H 0.5342 1.0856 0.6199 0.130 Uiso 1 1 calc R . . C17 C 0.6425(2) 0.31752(17) 0.6789(3) 0.0455(9) Uani 1 1 d . . . C18 C 0.7488(2) 0.31342(18) 0.7013(2) 0.0498(10) Uani 1 1 d . . . C19 C 0.8015(3) 0.3276(2) 0.7821(2) 0.0667(12) Uani 1 1 d . . . H19A H 0.7709 0.3388 0.8247 0.080 Uiso 1 1 calc R . . C20 C 0.8988(3) 0.3254(2) 0.8007(3) 0.0719(13) Uani 1 1 d . . . H20A H 0.9327 0.3354 0.8559 0.086 Uiso 1 1 calc R D . C21 C 0.9472(2) 0.30900(19) 0.7404(3) 0.0575(11) Uani 1 1 d . . . C22 C 0.8945(6) 0.3070(4) 0.6523(5) 0.042(2) Uiso 0.50 1 d P D 1 H22A H 0.9259 0.3035 0.6083 0.051 Uiso 0.50 1 calc PR D 1 C23 C 0.7956(6) 0.3104(4) 0.6339(5) 0.041(2) Uiso 0.50 1 d P D 1 H23A H 0.7608 0.3106 0.5772 0.050 Uiso 0.50 1 calc PR D 1 C22' C 0.8948(6) 0.2800(4) 0.6674(6) 0.055(3) Uiso 0.50 1 d P D 2 H22B H 0.9257 0.2576 0.6322 0.066 Uiso 0.50 1 calc PR D 2 C23' C 0.7957(6) 0.2838(4) 0.6455(6) 0.047(3) Uiso 0.50 1 d P D 2 H23B H 0.7614 0.2667 0.5941 0.056 Uiso 0.50 1 calc PR D 2 C24 C 0.3009(3) 0.3358(2) 0.4838(3) 0.0566(11) Uani 1 1 d . . . C25 C 0.2129(3) 0.3409(2) 0.4127(2) 0.0630(13) Uani 1 1 d . . . C26 C 0.2139(3) 0.3382(2) 0.3287(3) 0.0788(15) Uani 1 1 d . . . H26A H 0.2718 0.3350 0.3135 0.095 Uiso 1 1 calc R . . C27 C 0.1319(3) 0.3400(3) 0.2650(3) 0.0910(17) Uani 1 1 d . . . H27A H 0.1354 0.3379 0.2079 0.109 Uiso 1 1 calc R E . C28 C 0.0453(3) 0.3447(2) 0.2839(3) 0.0809(15) Uani 1 1 d . . . C29 C 0.0440(6) 0.3671(4) 0.3699(5) 0.049(2) Uiso 0.50 1 d P E 1 H29A H -0.0111 0.3832 0.3818 0.059 Uiso 0.50 1 calc PR E 1 C29' C 0.0425(7) 0.3303(4) 0.3689(6) 0.069(3) Uiso 0.50 1 d P F 2 H29B H -0.0151 0.3224 0.3828 0.083 Uiso 0.50 1 calc PR F 2 C30 C 0.1265(5) 0.3636(4) 0.4323(5) 0.041(2) Uiso 0.50 1 d P E 1 H30A H 0.1269 0.3759 0.4880 0.062 Uiso 0.50 1 calc PR E 1 C30' C 0.1280(6) 0.3280(4) 0.4329(6) 0.062(2) Uiso 0.50 1 d P F 2 H30B H 0.1268 0.3176 0.4890 0.074 Uiso 0.50 1 calc PR F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.02230(14) 0.0650(2) 0.04603(17) 0.00135(17) -0.00277(10) -0.00171(15) O3 0.0244(14) 0.093(2) 0.0547(16) -0.0032(16) 0.0109(13) 0.0022(14) O4 0.0274(15) 0.099(2) 0.0489(17) -0.0081(15) -0.0007(13) 0.0003(14) O5 0.0319(17) 0.147(3) 0.0452(18) 0.0061(19) -0.0034(14) -0.0048(17) O6 0.0295(16) 0.106(2) 0.0552(18) 0.0040(16) -0.0021(13) -0.0049(16) N1 0.043(2) 0.066(2) 0.059(2) 0.0085(19) 0.0057(18) -0.0003(19) N2 0.075(3) 0.062(3) 0.072(3) 0.006(2) 0.032(2) 0.001(2) N4 0.053(3) 0.067(3) 0.090(3) -0.006(2) 0.013(2) -0.008(2) C1 0.057(3) 0.076(4) 0.104(4) 0.011(3) 0.037(3) -0.005(3) C2 0.067(4) 0.064(4) 0.119(4) -0.006(3) 0.048(3) 0.000(3) C3 0.054(3) 0.057(3) 0.056(3) 0.001(2) 0.016(2) -0.003(2) C4 0.059(3) 0.074(3) 0.099(4) 0.017(3) 0.030(3) -0.003(3) C5 0.054(3) 0.073(4) 0.095(4) 0.015(3) 0.026(3) 0.007(2) C12 0.111(5) 0.046(3) 0.166(6) -0.003(4) 0.029(4) -0.028(3) C15 0.077(4) 0.065(4) 0.141(5) -0.004(4) 0.029(3) -0.011(3) C16 0.100(5) 0.071(4) 0.156(6) 0.001(4) 0.038(4) -0.002(3) C17 0.022(2) 0.058(3) 0.055(3) 0.001(2) 0.0069(19) -0.0021(18) C18 0.027(2) 0.070(3) 0.051(2) -0.007(2) 0.0074(18) -0.0038(18) C19 0.028(2) 0.126(4) 0.047(2) -0.006(3) 0.0108(19) -0.006(3) C20 0.025(2) 0.141(4) 0.048(2) -0.003(3) 0.0054(19) -0.008(3) C21 0.022(2) 0.093(3) 0.056(3) 0.000(2) 0.004(2) 0.0015(19) C24 0.029(2) 0.083(3) 0.051(3) 0.006(2) -0.0029(19) -0.008(2) C25 0.030(2) 0.114(4) 0.038(2) 0.005(2) -0.0068(18) -0.009(2) C26 0.034(2) 0.144(5) 0.052(3) 0.004(3) -0.003(2) -0.001(3) C27 0.043(3) 0.178(6) 0.043(3) 0.004(3) -0.008(2) -0.004(3) C28 0.041(3) 0.146(5) 0.045(3) 0.002(3) -0.010(2) -0.006(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 Cd N4 2.283(4) 1_545 ? Cd O5 2.294(3) . ? Cd N1 2.306(3) . ? Cd O4 2.357(2) . ? Cd O3 2.391(3) 2_656 ? Cd O3 2.481(2) . ? Cd O6 2.572(2) . ? O1 C6 1.251(12) . ? O2 C11 1.200(13) . ? O1' C6' 1.163(14) . ? O2' C11' 1.167(15) . ? O3 C17 1.255(4) . ? O3 Cd 2.391(3) 2_656 ? O4 C17 1.251(4) . ? O5 C24 1.240(5) . ? O6 C24 1.245(4) . ? N1 C1 1.313(5) . ? N1 C5 1.324(5) . ? N2 C6 1.281(12) . ? N2 C3 1.374(5) . ? N2 C6' 1.486(14) . ? N2 H2A 0.8600 . ? N3 C11 1.352(15) . ? N3 C12 1.428(12) . ? N3 H3A 0.8600 . ? N3' C11' 1.362(17) . ? N3' C12 1.411(13) . ? N3' H3'A 0.8600 . ? N4 C14' 1.286(13) . ? N4 C15 1.297(6) . ? N4 C14 1.430(11) . ? N4 Cd 2.283(4) 1_565 ? C1 C2 1.353(6) . ? C1 H1A 0.9300 . ? C2 C3 1.369(6) . ? C2 H2B 0.9300 . ? C3 C4 1.395(5) . ? C4 C5 1.367(6) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.545(18) . ? C7 C8 1.528(18) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.66(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.58(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.524(16) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C6' C7' 1.475(17) . ? C7' C8' 1.379(18) . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C8' C9' 1.516(18) . ? C8' H8'A 0.9700 . ? C8' H8'B 0.9700 . ? C9' C10' 1.373(18) . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? C10' C11' 1.64(2) . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C12 C13' 1.381(13) . ? C12 C16 1.387(7) . ? C12 C13 1.456(13) . ? C13 C14 1.368(14) . ? C13 H13A 0.9300 . ? C13' C14' 1.371(15) . ? C13' H13B 0.9300 . ? C14 H14A 0.9300 . ? C14' H14B 0.9300 . ? C15 C16 1.385(6) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.503(5) . ? C18 C19 1.374(5) . ? C18 C23' 1.393(9) . ? C18 C23 1.407(9) . ? C19 C20 1.375(5) . ? C19 H19A 0.9300 . ? C20 C21 1.367(5) . ? C20 H20A 0.9300 . ? C21 C22' 1.381(9) . ? C21 C22 1.440(9) . ? C21 C21 1.493(7) 2_756 ? C22 C23 1.398(10) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C22' C23' 1.402(11) . ? C22' H22B 0.9300 . ? C23' H23B 0.9300 . ? C24 C25 1.503(5) . ? C25 C26 1.353(5) . ? C25 C30' 1.374(9) . ? C25 C30 1.445(8) . ? C26 C27 1.376(5) . ? C26 H26A 0.9300 . ? C27 C28 1.365(6) . ? C27 H27A 0.9300 . ? C28 C29' 1.406(10) . ? C28 C29 1.461(9) . ? C28 C28 1.497(8) 2 ? C29 C30 1.371(10) . ? C29 H29A 0.9300 . ? C29' C30' 1.414(11) . ? C29' H29B 0.9300 . ? C30 H30A 0.9300 . ? C30' H30B 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 N4 Cd O5 90.35(13) 1_545 . ? N4 Cd N1 175.84(14) 1_545 . ? O5 Cd N1 88.79(12) . . ? N4 Cd O4 89.72(12) 1_545 . ? O5 Cd O4 140.90(10) . . ? N1 Cd O4 93.52(12) . . ? N4 Cd O3 86.37(12) 1_545 2_656 ? O5 Cd O3 88.77(9) . 2_656 ? N1 Cd O3 89.54(11) . 2_656 ? O4 Cd O3 130.23(8) . 2_656 ? N4 Cd O3 94.35(11) 1_545 . ? O5 Cd O3 164.68(9) . . ? N1 Cd O3 85.47(10) . . ? O4 Cd O3 53.83(8) . . ? O3 Cd O3 77.02(9) 2_656 . ? N4 Cd O6 93.38(11) 1_545 . ? O5 Cd O6 52.85(9) . . ? N1 Cd O6 89.34(10) . . ? O4 Cd O6 88.13(9) . . ? O3 Cd O6 141.61(8) 2_656 . ? O3 Cd O6 141.05(9) . . ? C17 O3 Cd 164.8(2) . 2_656 ? C17 O3 Cd 89.1(2) . . ? Cd O3 Cd 102.98(9) 2_656 . ? C17 O4 Cd 95.0(2) . . ? C24 O5 Cd 98.9(2) . . ? C24 O6 Cd 85.6(2) . . ? C1 N1 C5 115.7(4) . . ? C1 N1 Cd 124.6(3) . . ? C5 N1 Cd 119.6(3) . . ? C6 N2 C3 130.0(7) . . ? C3 N2 C6' 127.0(7) . . ? C6 N2 H2A 115.0 . . ? C3 N2 H2A 115.0 . . ? C6' N2 H2A 113.9 . . ? C11 N3 C12 125.4(11) . . ? C11 N3 H3A 117.3 . . ? C12 N3 H3A 117.3 . . ? C11' N3' C12 125.9(13) . . ? C11' N3' H3'A 117.1 . . ? C12 N3' H3'A 117.1 . . ? C14' N4 C15 115.0(7) . . ? C15 N4 C14 116.4(5) . . ? C14' N4 Cd 118.4(6) . 1_565 ? C15 N4 Cd 125.0(3) . 1_565 ? C14 N4 Cd 117.5(5) . 1_565 ? N1 C1 C2 126.2(4) . . ? N1 C1 H1A 116.9 . . ? C2 C1 H1A 116.9 . . ? C1 C2 C3 118.7(4) . . ? C1 C2 H2B 120.7 . . ? C3 C2 H2B 120.7 . . ? C2 C3 N2 125.4(4) . . ? C2 C3 C4 116.4(4) . . ? N2 C3 C4 118.3(4) . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4B 120.0 . . ? C3 C4 H4B 120.0 . . ? N1 C5 C4 123.0(4) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? O1 C6 N2 124.7(11) . . ? O1 C6 C7 121.8(12) . . ? N2 C6 C7 113.4(11) . . ? C8 C7 C6 112.0(12) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 104.2(12) . . ? C7 C8 H8A 110.9 . . ? C9 C8 H8A 110.9 . . ? C7 C8 H8B 110.9 . . ? C9 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? C10 C9 C8 100.3(13) . . ? C10 C9 H9A 111.7 . . ? C8 C9 H9A 111.7 . . ? C10 C9 H9B 111.7 . . ? C8 C9 H9B 111.7 . . ? H9A C9 H9B 109.5 . . ? C11 C10 C9 105.6(12) . . ? C11 C10 H10A 110.6 . . ? C9 C10 H10A 110.6 . . ? C11 C10 H10B 110.6 . . ? C9 C10 H10B 110.6 . . ? H10A C10 H10B 108.7 . . ? O2 C11 N3 126.6(13) . . ? O2 C11 C10 118.4(12) . . ? N3 C11 C10 113.5(12) . . ? O1' C6' C7' 126.8(13) . . ? O1' C6' N2 122.9(12) . . ? C7' C6' N2 110.2(11) . . ? C8' C7' C6' 117.6(13) . . ? C8' C7' H7'A 107.9 . . ? C6' C7' H7'A 107.9 . . ? C8' C7' H7'B 107.9 . . ? C6' C7' H7'B 107.9 . . ? H7'A C7' H7'B 107.2 . . ? C7' C8' C9' 115.8(14) . . ? C7' C8' H8'A 108.3 . . ? C9' C8' H8'A 108.3 . . ? C7' C8' H8'B 108.3 . . ? C9' C8' H8'B 108.3 . . ? H8'A C8' H8'B 107.4 . . ? C10' C9' C8' 120.4(14) . . ? C10' C9' H9'A 107.2 . . ? C8' C9' H9'A 107.2 . . ? C10' C9' H9'B 107.2 . . ? C8' C9' H9'B 107.2 . . ? H9'A C9' H9'B 106.9 . . ? C9' C10' C11' 115.3(14) . . ? C9' C10' H10C 108.4 . . ? C11' C10' H10C 108.4 . . ? C9' C10' H10D 108.4 . . ? C11' C10' H10D 108.4 . . ? H10C C10' H10D 107.5 . . ? O2' C11' N3' 131.8(17) . . ? O2' C11' C10' 122.5(16) . . ? N3' C11' C10' 105.2(14) . . ? C13' C12 C16 117.2(7) . . ? C13' C12 N3' 117.9(9) . . ? C16 C12 N3' 120.4(8) . . ? C13' C12 N3 117.9(9) . . ? C16 C12 N3 124.8(7) . . ? C16 C12 C13 119.8(7) . . ? N3' C12 C13 119.7(9) . . ? N3 C12 C13 109.1(8) . . ? C14 C13 C12 114.9(10) . . ? C14 C13 H13A 122.6 . . ? C12 C13 H13A 122.6 . . ? C14' C13' C12 117.5(11) . . ? C14' C13' H13B 121.2 . . ? C12 C13' H13B 121.2 . . ? C13 C14 N4 123.0(9) . . ? C13 C14 H14A 118.5 . . ? N4 C14 H14A 118.5 . . ? N4 C14' C13' 125.6(12) . . ? N4 C14' H14B 117.2 . . ? C13' C14' H14B 117.2 . . ? N4 C15 C16 125.3(5) . . ? N4 C15 H15A 117.3 . . ? C16 C15 H15A 117.3 . . ? C15 C16 C12 116.8(5) . . ? C15 C16 H16A 121.6 . . ? C12 C16 H16A 121.6 . . ? O4 C17 O3 122.1(3) . . ? O4 C17 C18 119.0(3) . . ? O3 C17 C18 118.9(3) . . ? C19 C18 C23' 117.1(5) . . ? C19 C18 C23 118.1(5) . . ? C19 C18 C17 121.7(4) . . ? C23' C18 C17 120.2(5) . . ? C23 C18 C17 118.3(5) . . ? C18 C19 C20 120.9(4) . . ? C18 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? C21 C20 C19 121.8(4) . . ? C21 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C20 C21 C22' 116.1(5) . . ? C20 C21 C22 117.3(4) . . ? C20 C21 C21 121.9(4) . 2_756 ? C22' C21 C21 120.6(5) . 2_756 ? C22 C21 C21 119.0(5) . 2_756 ? C23 C22 C21 119.2(7) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C22 C23 C18 119.8(7) . . ? C22 C23 H23A 120.1 . . ? C18 C23 H23A 120.1 . . ? C21 C22' C23' 121.0(8) . . ? C21 C22' H22B 119.5 . . ? C23' C22' H22B 119.5 . . ? C18 C23' C22' 119.6(8) . . ? C18 C23' H23B 120.2 . . ? C22' C23' H23B 120.2 . . ? O5 C24 O6 122.6(4) . . ? O5 C24 C25 117.7(4) . . ? O6 C24 C25 119.7(4) . . ? C26 C25 C30' 116.6(5) . . ? C26 C25 C30 116.4(4) . . ? C26 C25 C24 123.1(4) . . ? C30' C25 C24 117.2(5) . . ? C30 C25 C24 119.1(4) . . ? C25 C26 C27 121.9(4) . . ? C25 C26 H26A 119.1 . . ? C27 C26 H26A 119.1 . . ? C28 C27 C26 121.3(4) . . ? C28 C27 H27A 119.4 . . ? C26 C27 H27A 119.4 . . ? C27 C28 C29' 116.0(5) . . ? C27 C28 C29 116.8(5) . . ? C27 C28 C28 122.4(5) . 2 ? C29' C28 C28 118.9(6) . 2 ? C29 C28 C28 118.8(6) . 2 ? C30 C29 C28 117.9(7) . . ? C30 C29 H29A 121.0 . . ? C28 C29 H29A 121.0 . . ? C28 C29' C30' 119.4(8) . . ? C28 C29' H29B 120.3 . . ? C30' C29' H29B 120.3 . . ? C29 C30 C25 120.9(7) . . ? C29 C30 H30A 119.5 . . ? C25 C30 H30A 119.5 . . ? C25 C30' C29' 120.3(8) . . ? C25 C30' H30B 119.8 . . ? C29' C30' H30B 119.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.459 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.066 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.013 0.000 2282 481 'co-crystallized THF and DMF solvent molecules' _platon_squeeze_details ; ? ; # End of data1 data_2 _database_code_depnum_ccdc_archive 'CCDC 866972' #TrackingRef '- all-2nd-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H66 Cd2 N10 O16' _chemical_formula_weight 1432.05 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 10.7477(2) _cell_length_b 36.4644(7) _cell_length_c 15.9903(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.9960(10) _cell_angle_gamma 90.00 _cell_volume 6251.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9912 _cell_measurement_theta_min 2.203 _cell_measurement_theta_max 28.266 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8999 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _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 'Bruker AXS APEX2' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55694 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13645 _reflns_number_gt 9675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0593P)^2^+23.0795P] 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 13645 _refine_ls_number_parameters 790 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.004 _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 0.32105(4) 0.711883(11) 0.91714(2) 0.02388(12) Uani 1 1 d . . . Cd2 Cd 0.38819(3) 1.023235(11) 0.92192(2) 0.02181(11) Uani 1 1 d . . . N1 N 0.4453(4) 0.69705(13) 0.8086(3) 0.0295(11) Uani 1 1 d . . . N2 N 0.6761(4) 0.67375(15) 0.6150(3) 0.0315(12) Uani 1 1 d . . . H2A H 0.6825 0.6510 0.6020 0.038 Uiso 1 1 calc R . . N3 N 0.9964(4) 0.74872(14) 0.2340(3) 0.0298(11) Uani 1 1 d . . . H3A H 1.0289 0.7663 0.2641 0.036 Uiso 1 1 calc R . . N4 N 1.2034(4) 0.71996(13) 0.0309(3) 0.0266(10) Uani 1 1 d . . . N5 N 0.5120(4) 1.03561(13) 0.8145(3) 0.0262(10) Uani 1 1 d . . . N6 N 0.6913(5) 1.07084(14) 0.6043(3) 0.0317(12) Uani 1 1 d . . . H6A H 0.7372 1.0899 0.6139 0.038 Uiso 1 1 calc R . . N7 N 1.0186(5) 0.99856(15) 0.2219(3) 0.0342(12) Uani 1 1 d . . . H7A H 0.9560 0.9848 0.2070 0.041 Uiso 1 1 calc R . . N8 N 1.2631(4) 1.01566(13) 0.0322(3) 0.0276(11) Uani 1 1 d . . . O1 O 0.7485(4) 0.73026(14) 0.5876(3) 0.0472(12) Uani 1 1 d . . . O2 O 0.8340(4) 0.70866(14) 0.2255(3) 0.0424(11) Uani 1 1 d . . . O3 O 0.6245(4) 1.03142(14) 0.5008(3) 0.0480(12) Uani 1 1 d . . . O4 O 1.1020(5) 1.03294(16) 0.3297(3) 0.0539(14) Uani 1 1 d . . . O5 O 0.1396(4) 0.69643(11) 0.8332(2) 0.0302(9) Uani 1 1 d . . . O6 O 0.2284(3) 0.64647(11) 0.8879(2) 0.0290(9) Uani 1 1 d . . . O7 O -0.3043(4) 0.58779(11) 0.6041(2) 0.0296(9) Uani 1 1 d . . . O8 O -0.2086(4) 0.53902(11) 0.6618(3) 0.0338(10) Uani 1 1 d . . . O9 O 0.2764(4) 0.76874(11) 0.8529(3) 0.0372(10) Uani 1 1 d . . . O10 O 0.4232(4) 0.76949(11) 0.9550(3) 0.0354(10) Uani 1 1 d . . . O11 O 0.3578(4) 0.96645(12) 0.8655(3) 0.0416(11) Uani 1 1 d . . . O12 O 0.4580(4) 0.95575(11) 0.9869(3) 0.0366(10) Uani 1 1 d . . . O13 O 0.4639(5) 0.68253(16) 1.0066(3) 0.0625(15) Uani 1 1 d . . . H13A H 0.5447 0.6878 1.0108 0.075 Uiso 1 1 d R . . H13C H 0.4590 0.6581 1.0140 0.075 Uiso 1 1 d R . . C1 C 0.4857(6) 0.66324(17) 0.7945(4) 0.0338(14) Uani 1 1 d . . . H1A H 0.4618 0.6444 0.8291 0.041 Uiso 1 1 calc R . . C2 C 0.5610(6) 0.65481(16) 0.7314(4) 0.0339(14) Uani 1 1 d . . . H2B H 0.5868 0.6308 0.7238 0.041 Uiso 1 1 calc R . . C3 C 0.5986(5) 0.68239(17) 0.6789(3) 0.0276(13) Uani 1 1 d . . . C4 C 0.5561(6) 0.71733(19) 0.6931(4) 0.0457(18) Uani 1 1 d . . . H4B H 0.5786 0.7367 0.6595 0.055 Uiso 1 1 calc R . . C5 C 0.4800(6) 0.72323(19) 0.7573(5) 0.0463(18) Uani 1 1 d . . . H5A H 0.4511 0.7469 0.7654 0.056 Uiso 1 1 calc R . . C6 C 0.7428(6) 0.6983(2) 0.5713(4) 0.0390(16) Uani 1 1 d . . . C7 C 0.8089(8) 0.6805(2) 0.5007(5) 0.058(2) Uani 1 1 d . . . H7B H 0.7496 0.6657 0.4671 0.069 Uiso 1 1 calc R . . H7C H 0.8736 0.6643 0.5247 0.069 Uiso 1 1 calc R . . C8 C 0.8675(6) 0.7085(2) 0.4441(4) 0.0473(18) Uani 1 1 d . . . H8B H 0.9179 0.7255 0.4788 0.057 Uiso 1 1 calc R . . H8C H 0.9223 0.6958 0.4081 0.057 Uiso 1 1 calc R . . C9 C 0.7723(6) 0.7299(2) 0.3904(4) 0.0467(18) Uani 1 1 d . . . H9A H 0.7211 0.7441 0.4262 0.056 Uiso 1 1 calc R . . H9B H 0.7182 0.7130 0.3582 0.056 Uiso 1 1 calc R . . C10 C 0.8346(7) 0.7559(2) 0.3301(4) 0.0472(18) Uani 1 1 d . . . H10A H 0.7742 0.7738 0.3081 0.057 Uiso 1 1 calc R . . H10B H 0.9021 0.7690 0.3605 0.057 Uiso 1 1 calc R . . C11 C 0.8858(6) 0.73488(19) 0.2577(4) 0.0345(14) Uani 1 1 d . . . C12 C 1.0624(5) 0.73740(16) 0.1660(3) 0.0253(12) Uani 1 1 d . . . C13 C 1.0188(6) 0.7131(2) 0.1044(4) 0.0468(19) Uani 1 1 d . . . H13B H 0.9409 0.7022 0.1067 0.056 Uiso 1 1 calc R . . C14 C 1.0920(6) 0.7053(2) 0.0396(4) 0.0442(18) Uani 1 1 d . . . H14A H 1.0614 0.6887 -0.0009 0.053 Uiso 1 1 calc R . . C15 C 1.2469(6) 0.74241(18) 0.0918(4) 0.0368(15) Uani 1 1 d . . . H15A H 1.3260 0.7524 0.0886 0.044 Uiso 1 1 calc R . . C16 C 1.1809(6) 0.75149(18) 0.1590(4) 0.0385(15) Uani 1 1 d . . . H16A H 1.2157 0.7672 0.2001 0.046 Uiso 1 1 calc R . . C17 C 0.4907(5) 1.01898(16) 0.7402(4) 0.0320(14) Uani 1 1 d . . . H17A H 0.4349 0.9995 0.7374 0.038 Uiso 1 1 calc R . . C18 C 0.5449(6) 1.02848(16) 0.6674(4) 0.0317(14) Uani 1 1 d . . . H18A H 0.5254 1.0160 0.6174 0.038 Uiso 1 1 calc R . . C19 C 0.6306(5) 1.05767(16) 0.6718(4) 0.0294(13) Uani 1 1 d . . . C20 C 0.6557(5) 1.07436(17) 0.7494(4) 0.0326(14) Uani 1 1 d . . . H20A H 0.7131 1.0934 0.7551 0.039 Uiso 1 1 calc R . . C21 C 0.5956(5) 1.06273(16) 0.8175(4) 0.0300(13) Uani 1 1 d . . . H21A H 0.6142 1.0744 0.8686 0.036 Uiso 1 1 calc R . . C22 C 0.6874(6) 1.05719(19) 0.5236(4) 0.0364(15) Uani 1 1 d . . . C23 C 0.7715(7) 1.0778(2) 0.4666(4) 0.0450(17) Uani 1 1 d . . . H23A H 0.7277 1.0992 0.4436 0.054 Uiso 1 1 calc R . . H23B H 0.8455 1.0862 0.4993 0.054 Uiso 1 1 calc R . . C24 C 0.8093(6) 1.0537(2) 0.3960(4) 0.0413(16) Uani 1 1 d . . . H24A H 0.8537 1.0685 0.3574 0.050 Uiso 1 1 calc R . . H24B H 0.7348 1.0443 0.3657 0.050 Uiso 1 1 calc R . . C25 C 0.8910(6) 1.0218(2) 0.4250(4) 0.0427(17) Uani 1 1 d . . . H25A H 0.8487 1.0079 0.4663 0.051 Uiso 1 1 calc R . . H25B H 0.9678 1.0313 0.4523 0.051 Uiso 1 1 calc R . . C26 C 0.9229(6) 0.9962(2) 0.3545(4) 0.0460(18) Uani 1 1 d . . . H26A H 0.9512 0.9730 0.3783 0.055 Uiso 1 1 calc R . . H26B H 0.8482 0.9916 0.3184 0.055 Uiso 1 1 calc R . . C27 C 1.0233(6) 1.0118(2) 0.3023(4) 0.0393(16) Uani 1 1 d . . . C28 C 1.1043(5) 1.00494(17) 0.1613(4) 0.0306(14) Uani 1 1 d . . . C29 C 1.0927(6) 0.98499(19) 0.0889(4) 0.0423(17) Uani 1 1 d . . . H29A H 1.0303 0.9674 0.0814 0.051 Uiso 1 1 calc R . . C30 C 1.1732(6) 0.99094(19) 0.0272(4) 0.0415(16) Uani 1 1 d . . . H30A H 1.1638 0.9766 -0.0210 0.050 Uiso 1 1 calc R . . C31 C 1.2754(6) 1.0345(2) 0.1036(4) 0.0449(17) Uani 1 1 d . . . H31A H 1.3394 1.0517 0.1097 0.054 Uiso 1 1 calc R . . C32 C 1.1995(6) 1.0303(2) 0.1691(4) 0.0461(18) Uani 1 1 d . . . H32A H 1.2124 1.0442 0.2176 0.055 Uiso 1 1 calc R . . C33 C 0.1465(5) 0.66183(16) 0.8409(3) 0.0232(12) Uani 1 1 d . . . C34 C 0.0533(5) 0.63904(15) 0.7914(3) 0.0236(12) Uani 1 1 d . . . C35 C -0.0418(6) 0.62269(17) 0.8299(4) 0.0345(15) Uani 1 1 d . . . H35A H -0.0476 0.6256 0.8873 0.041 Uiso 1 1 calc R . . C36 C -0.1306(6) 0.60158(18) 0.7833(4) 0.0364(15) Uani 1 1 d . . . H36A H -0.1944 0.5905 0.8105 0.044 Uiso 1 1 calc R . . C37 C -0.1258(5) 0.59686(16) 0.6995(4) 0.0273(13) Uani 1 1 d . . . C38 C -0.2203(5) 0.57317(17) 0.6514(3) 0.0266(13) Uani 1 1 d . . . C39 C -0.0263(5) 0.61276(16) 0.6575(3) 0.0249(12) Uani 1 1 d . . . C40 C -0.0129(5) 0.60726(17) 0.5706(4) 0.0295(13) Uani 1 1 d . . . H40A H -0.0718 0.5933 0.5395 0.035 Uiso 1 1 calc R . . C41 C 0.0844(5) 0.62201(19) 0.5317(4) 0.0355(15) Uani 1 1 d . . . H41A H 0.0926 0.6177 0.4751 0.043 Uiso 1 1 calc R . . C42 C 0.1718(6) 0.64366(19) 0.5780(4) 0.0378(15) Uani 1 1 d . . . H42A H 0.2375 0.6540 0.5513 0.045 Uiso 1 1 calc R . . C43 C 0.1625(5) 0.64988(17) 0.6617(4) 0.0302(13) Uani 1 1 d . . . H43A H 0.2218 0.6643 0.6913 0.036 Uiso 1 1 calc R . . C44 C 0.0630(5) 0.63451(15) 0.7036(3) 0.0232(12) Uani 1 1 d . . . C45 C 0.3509(5) 0.78635(15) 0.9026(3) 0.0228(12) Uani 1 1 d . . . C46 C 0.3539(5) 0.82715(15) 0.9015(3) 0.0221(11) Uani 1 1 d . . . C47 C 0.4540(5) 0.84349(15) 0.9454(3) 0.0259(12) Uani 1 1 d . . . H47A H 0.5151 0.8287 0.9720 0.031 Uiso 1 1 calc R . . C48 C 0.4663(5) 0.88148(16) 0.9510(4) 0.0269(12) Uani 1 1 d . . . H48A H 0.5348 0.8916 0.9814 0.032 Uiso 1 1 calc R . . C49 C 0.3781(5) 0.90415(15) 0.9118(3) 0.0229(12) Uani 1 1 d . . . C50 C 0.4002(5) 0.94513(15) 0.9231(4) 0.0276(13) Uani 1 1 d . . . C51 C 0.2719(5) 0.88912(15) 0.8656(3) 0.0216(11) Uani 1 1 d . . . C52 C 0.1744(5) 0.91111(17) 0.8285(4) 0.0315(14) Uani 1 1 d . . . H52A H 0.1816 0.9365 0.8308 0.038 Uiso 1 1 calc R . . C53 C 0.0696(6) 0.89561(19) 0.7892(4) 0.0358(15) Uani 1 1 d . . . H53A H 0.0066 0.9106 0.7653 0.043 Uiso 1 1 calc R . . C54 C 0.0570(6) 0.85766(19) 0.7848(4) 0.0372(15) Uani 1 1 d . . . H54A H -0.0146 0.8474 0.7583 0.045 Uiso 1 1 calc R . . C55 C 0.1486(5) 0.83543(18) 0.8189(4) 0.0332(14) Uani 1 1 d . . . H55A H 0.1393 0.8101 0.8145 0.040 Uiso 1 1 calc R . . C56 C 0.2590(5) 0.85016(15) 0.8614(3) 0.0223(11) Uani 1 1 d . . . N9 N 0.7196(8) 0.5885(3) 0.0062(6) 0.084(2) Uani 1 1 d . . . O14 O 0.8563(9) 0.6345(3) 0.0378(6) 0.132(3) Uani 1 1 d . . . C57 C 0.8179(12) 0.6042(3) 0.0492(8) 0.111(5) Uani 1 1 d . . . H57A H 0.8595 0.5903 0.0912 0.134 Uiso 1 1 calc R . . C58 C 0.6360(10) 0.6095(3) -0.0525(7) 0.099(4) Uani 1 1 d . . . C59 C 0.6869(12) 0.5514(4) 0.0173(8) 0.113(4) Uani 1 1 d . . . N10 N 0.5828(9) 0.6215(3) 0.2211(5) 0.223(7) Uiso 1 1 d D A . C60 C 0.6987(9) 0.6258(3) 0.2732(7) 0.117(4) Uiso 1 1 d D . . C61 C 0.5451(13) 0.5840(3) 0.2010(10) 0.190(8) Uiso 1 1 d D . . C62 C 0.5122(11) 0.6513(3) 0.1922(7) 0.371(19) Uiso 1 1 d D . . O15 O 0.5463(16) 0.6822(3) 0.2105(11) 0.171(9) Uiso 0.50 1 d PD A 1 O15' O 0.4162(13) 0.6466(6) 0.1490(10) 0.262(15) Uiso 0.50 1 d PD A 2 O16 O 0.7054(9) 0.6979(3) 0.0197(8) 0.190(5) Uani 1 1 d . . . H16B H 0.7403 0.7126 0.0553 0.285 Uiso 1 1 d R . . H16C H 0.7368 0.6766 0.0268 0.285 Uiso 1 1 d 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 0.0283(2) 0.0218(2) 0.0223(2) -0.00677(17) 0.00745(16) -0.00260(17) Cd2 0.01963(19) 0.0191(2) 0.0274(2) 0.00686(17) 0.00686(15) 0.00258(16) N1 0.028(2) 0.028(3) 0.034(3) -0.007(2) 0.013(2) -0.004(2) N2 0.027(2) 0.040(3) 0.029(3) -0.008(2) 0.011(2) 0.001(2) N3 0.036(3) 0.033(3) 0.020(2) -0.004(2) 0.000(2) 0.007(2) N4 0.032(3) 0.027(3) 0.021(2) -0.003(2) 0.005(2) -0.003(2) N5 0.028(2) 0.019(2) 0.033(3) 0.005(2) 0.008(2) 0.0008(19) N6 0.040(3) 0.029(3) 0.028(3) 0.002(2) 0.015(2) -0.002(2) N7 0.029(3) 0.041(3) 0.035(3) 0.010(2) 0.016(2) -0.001(2) N8 0.024(2) 0.024(3) 0.035(3) 0.005(2) 0.006(2) 0.005(2) O1 0.052(3) 0.045(3) 0.047(3) -0.005(2) 0.027(2) -0.006(2) O2 0.035(2) 0.055(3) 0.038(3) 0.000(2) 0.009(2) -0.003(2) O3 0.051(3) 0.055(3) 0.041(3) -0.008(2) 0.021(2) -0.013(2) O4 0.042(3) 0.077(4) 0.045(3) -0.008(3) 0.018(2) -0.007(3) O5 0.043(2) 0.025(2) 0.024(2) -0.0030(17) 0.0047(18) -0.0115(18) O6 0.027(2) 0.026(2) 0.034(2) -0.0066(18) 0.0050(18) -0.0042(17) O7 0.027(2) 0.032(2) 0.030(2) -0.0081(18) 0.0044(18) -0.0051(17) O8 0.025(2) 0.030(2) 0.047(3) -0.013(2) 0.0052(18) -0.0035(18) O9 0.046(3) 0.023(2) 0.041(3) -0.0089(19) -0.002(2) -0.0062(19) O10 0.036(2) 0.025(2) 0.044(3) 0.002(2) 0.001(2) -0.0007(18) O11 0.064(3) 0.024(2) 0.039(3) 0.007(2) 0.020(2) -0.002(2) O12 0.026(2) 0.029(2) 0.056(3) -0.015(2) 0.011(2) -0.0023(18) O13 0.053(3) 0.066(4) 0.068(4) 0.000(3) -0.003(3) 0.012(3) C1 0.040(3) 0.027(3) 0.037(3) -0.003(3) 0.017(3) 0.000(3) C2 0.037(3) 0.022(3) 0.045(4) -0.008(3) 0.017(3) 0.000(3) C3 0.023(3) 0.038(3) 0.022(3) -0.005(3) 0.005(2) -0.003(2) C4 0.053(4) 0.037(4) 0.051(4) 0.011(3) 0.031(3) 0.003(3) C5 0.052(4) 0.030(4) 0.060(5) -0.001(3) 0.030(4) 0.004(3) C6 0.029(3) 0.053(5) 0.036(4) 0.005(3) 0.012(3) 0.005(3) C7 0.071(5) 0.052(5) 0.055(5) 0.005(4) 0.044(4) 0.016(4) C8 0.045(4) 0.058(5) 0.042(4) 0.005(4) 0.022(3) 0.010(3) C9 0.037(4) 0.069(5) 0.036(4) 0.000(4) 0.017(3) 0.004(3) C10 0.049(4) 0.057(5) 0.038(4) 0.000(3) 0.015(3) 0.022(4) C11 0.034(3) 0.041(4) 0.028(3) 0.007(3) 0.006(3) 0.012(3) C12 0.031(3) 0.032(3) 0.013(3) 0.003(2) 0.002(2) 0.006(2) C13 0.034(3) 0.077(5) 0.030(3) -0.025(4) 0.006(3) -0.012(3) C14 0.040(4) 0.061(5) 0.032(4) -0.024(3) 0.006(3) -0.017(3) C15 0.037(3) 0.045(4) 0.029(3) -0.009(3) 0.009(3) -0.012(3) C16 0.048(4) 0.041(4) 0.027(3) -0.014(3) 0.007(3) -0.009(3) C17 0.035(3) 0.024(3) 0.038(4) 0.004(3) 0.006(3) -0.008(3) C18 0.038(3) 0.026(3) 0.032(3) 0.002(3) 0.010(3) -0.005(3) C19 0.027(3) 0.026(3) 0.036(3) 0.005(3) 0.010(3) 0.004(2) C20 0.033(3) 0.027(3) 0.040(4) -0.001(3) 0.015(3) -0.007(3) C21 0.037(3) 0.025(3) 0.029(3) 0.001(3) 0.005(3) -0.002(3) C22 0.037(3) 0.039(4) 0.034(4) 0.005(3) 0.015(3) -0.004(3) C23 0.048(4) 0.055(5) 0.034(4) 0.006(3) 0.017(3) -0.008(3) C24 0.041(4) 0.057(5) 0.026(3) 0.012(3) 0.006(3) 0.003(3) C25 0.039(3) 0.066(5) 0.025(3) 0.014(3) 0.012(3) 0.008(3) C26 0.044(4) 0.057(5) 0.040(4) 0.015(3) 0.024(3) 0.008(3) C27 0.030(3) 0.051(4) 0.038(4) 0.007(3) 0.014(3) 0.006(3) C28 0.024(3) 0.036(3) 0.032(3) 0.013(3) 0.008(2) 0.006(3) C29 0.038(4) 0.043(4) 0.048(4) -0.003(3) 0.017(3) -0.012(3) C30 0.047(4) 0.040(4) 0.039(4) -0.004(3) 0.017(3) -0.014(3) C31 0.037(4) 0.050(4) 0.050(4) -0.012(3) 0.021(3) -0.013(3) C32 0.043(4) 0.059(5) 0.038(4) -0.012(3) 0.018(3) -0.011(3) C33 0.026(3) 0.028(3) 0.016(3) -0.002(2) 0.008(2) -0.005(2) C34 0.027(3) 0.026(3) 0.018(3) -0.004(2) 0.004(2) -0.005(2) C35 0.042(3) 0.041(4) 0.023(3) -0.013(3) 0.017(3) -0.018(3) C36 0.039(3) 0.040(4) 0.032(3) -0.010(3) 0.016(3) -0.015(3) C37 0.026(3) 0.026(3) 0.030(3) -0.010(3) 0.010(2) -0.005(2) C38 0.027(3) 0.035(3) 0.020(3) -0.011(3) 0.014(2) -0.008(3) C39 0.028(3) 0.028(3) 0.019(3) -0.008(2) 0.006(2) -0.004(2) C40 0.028(3) 0.037(3) 0.024(3) -0.009(3) 0.004(2) 0.000(3) C41 0.034(3) 0.053(4) 0.020(3) -0.006(3) 0.011(3) -0.003(3) C42 0.031(3) 0.055(4) 0.029(3) -0.002(3) 0.012(3) -0.010(3) C43 0.031(3) 0.036(3) 0.024(3) -0.005(3) 0.007(2) -0.012(3) C44 0.023(3) 0.029(3) 0.019(3) -0.005(2) 0.008(2) -0.003(2) C45 0.022(3) 0.025(3) 0.023(3) -0.004(2) 0.013(2) 0.001(2) C46 0.025(3) 0.019(3) 0.023(3) -0.003(2) 0.011(2) -0.001(2) C47 0.027(3) 0.022(3) 0.029(3) -0.005(2) 0.005(2) 0.003(2) C48 0.025(3) 0.028(3) 0.028(3) -0.004(3) 0.004(2) -0.009(2) C49 0.031(3) 0.022(3) 0.017(3) -0.002(2) 0.010(2) -0.004(2) C50 0.027(3) 0.020(3) 0.038(3) -0.001(3) 0.021(3) -0.002(2) C51 0.023(3) 0.026(3) 0.017(3) 0.002(2) 0.007(2) -0.001(2) C52 0.037(3) 0.032(3) 0.027(3) 0.010(3) 0.013(3) 0.005(3) C53 0.034(3) 0.045(4) 0.027(3) 0.013(3) -0.001(3) 0.005(3) C54 0.028(3) 0.049(4) 0.034(4) 0.001(3) -0.003(3) -0.004(3) C55 0.033(3) 0.033(3) 0.033(3) -0.007(3) 0.002(3) -0.003(3) C56 0.026(3) 0.021(3) 0.020(3) -0.002(2) 0.007(2) 0.001(2) N9 0.069(5) 0.082(6) 0.100(6) 0.000(5) -0.002(5) -0.001(5) O14 0.128(7) 0.115(8) 0.154(9) -0.031(6) 0.018(6) -0.013(6) C57 0.126(10) 0.079(8) 0.126(10) 0.035(7) -0.017(8) -0.061(8) C58 0.084(7) 0.104(9) 0.106(9) 0.040(7) -0.010(6) 0.002(6) C59 0.128(11) 0.087(9) 0.122(10) 0.010(8) -0.017(8) -0.014(8) O16 0.125(8) 0.133(9) 0.299(15) -0.018(10) -0.071(9) -0.018(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 Cd1 O13 2.290(5) . ? Cd1 N4 2.305(4) 1_456 ? Cd1 N1 2.325(4) . ? Cd1 O9 2.348(4) . ? Cd1 O5 2.357(4) . ? Cd1 O10 2.427(4) . ? Cd1 O6 2.614(4) . ? Cd1 C45 2.746(6) . ? Cd2 O12 2.261(4) 3_677 ? Cd2 O11 2.273(4) . ? Cd2 N5 2.290(4) . ? Cd2 N8 2.307(5) 1_456 ? Cd2 O8 2.343(4) 2_556 ? Cd2 O7 2.545(4) 2_556 ? N1 C5 1.329(8) . ? N1 C1 1.332(8) . ? N2 C6 1.367(8) . ? N2 C3 1.399(7) . ? N2 H2A 0.8600 . ? N3 C11 1.370(8) . ? N3 C12 1.401(7) . ? N3 H3A 0.8600 . ? N4 C14 1.327(8) . ? N4 C15 1.333(7) . ? N4 Cd1 2.305(4) 1_654 ? N5 C21 1.335(7) . ? N5 C17 1.338(8) . ? N6 C22 1.381(8) . ? N6 C19 1.386(7) . ? N6 H6A 0.8600 . ? N7 C27 1.371(8) . ? N7 C28 1.402(7) . ? N7 H7A 0.8600 . ? N8 C30 1.320(8) . ? N8 C31 1.332(8) . ? N8 Cd2 2.307(5) 1_654 ? O1 C6 1.196(8) . ? O2 C11 1.204(8) . ? O3 C22 1.199(8) . ? O4 C27 1.204(8) . ? O5 C33 1.269(7) . ? O6 C33 1.249(7) . ? O7 C38 1.256(7) . ? O7 Cd2 2.545(4) 2_546 ? O8 C38 1.261(7) . ? O8 Cd2 2.343(4) 2_546 ? O9 C45 1.264(7) . ? O10 C45 1.262(7) . ? O11 C50 1.265(7) . ? O12 C50 1.220(7) . ? O12 Cd2 2.261(4) 3_677 ? O13 H13A 0.8873 . ? O13 H13C 0.9012 . ? C1 C2 1.372(8) . ? C1 H1A 0.9300 . ? C2 C3 1.387(8) . ? C2 H2B 0.9300 . ? C3 C4 1.377(9) . ? C4 C5 1.374(9) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.520(9) . ? C7 C8 1.529(10) . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.508(10) . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.538(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.522(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 C13 1.383(8) . ? C12 C16 1.385(8) . ? C13 C14 1.373(9) . ? C13 H13B 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.369(8) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.382(8) . ? C17 H17A 0.9300 . ? C18 C19 1.406(8) . ? C18 H18A 0.9300 . ? C19 C20 1.391(8) . ? C20 C21 1.371(8) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.525(8) . ? C23 C24 1.508(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.510(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.522(9) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.520(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C28 C29 1.366(9) . ? C28 C32 1.377(9) . ? C29 C30 1.374(8) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.381(9) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.487(7) . ? C34 C35 1.367(7) . ? C34 C44 1.424(7) . ? C35 C36 1.399(8) . ? C35 H35A 0.9300 . ? C36 C37 1.356(8) . ? C36 H36A 0.9300 . ? C37 C39 1.425(7) . ? C37 C38 1.503(8) . ? C39 C44 1.413(8) . ? C39 C40 1.420(7) . ? C40 C41 1.364(8) . ? C40 H40A 0.9300 . ? C41 C42 1.398(9) . ? C41 H41A 0.9300 . ? C42 C43 1.369(8) . ? C42 H42A 0.9300 . ? C43 C44 1.416(7) . ? C43 H43A 0.9300 . ? C45 C46 1.488(8) . ? C46 C47 1.378(8) . ? C46 C56 1.436(8) . ? C47 C48 1.394(8) . ? C47 H47A 0.9300 . ? C48 C49 1.375(8) . ? C48 H48A 0.9300 . ? C49 C51 1.426(8) . ? C49 C50 1.522(8) . ? C51 C52 1.416(8) . ? C51 C56 1.428(7) . ? C52 C53 1.373(9) . ? C52 H52A 0.9300 . ? C53 C54 1.392(9) . ? C53 H53A 0.9300 . ? C54 C55 1.360(9) . ? C54 H54A 0.9300 . ? C55 C56 1.430(8) . ? C55 H55A 0.9300 . ? N9 C57 1.346(13) . ? N9 C59 1.414(14) . ? N9 C58 1.468(13) . ? O14 C57 1.199(12) . ? C57 H57A 0.9300 . ? N10 C62 1.386(4) . ? N10 C61 1.456(4) . ? N10 C60 1.458(4) . ? C62 O15 1.212(5) . ? C62 O15' 1.214(5) . ? O16 H16B 0.8500 . ? O16 H16C 0.8506 . ? 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 O13 Cd1 N4 87.00(18) . 1_456 ? O13 Cd1 N1 87.86(19) . . ? N4 Cd1 N1 173.39(17) 1_456 . ? O13 Cd1 O9 142.52(18) . . ? N4 Cd1 O9 97.21(16) 1_456 . ? N1 Cd1 O9 89.40(16) . . ? O13 Cd1 O5 137.40(18) . . ? N4 Cd1 O5 90.12(15) 1_456 . ? N1 Cd1 O5 90.84(15) . . ? O9 Cd1 O5 79.99(14) . . ? O13 Cd1 O10 88.68(18) . . ? N4 Cd1 O10 87.50(15) 1_456 . ? N1 Cd1 O10 96.55(16) . . ? O9 Cd1 O10 54.55(14) . . ? O5 Cd1 O10 133.67(14) . . ? O13 Cd1 O6 85.17(17) . . ? N4 Cd1 O6 91.97(14) 1_456 . ? N1 Cd1 O6 83.44(14) . . ? O9 Cd1 O6 131.57(14) . . ? O5 Cd1 O6 52.43(13) . . ? O10 Cd1 O6 173.85(14) . . ? O13 Cd1 C45 115.97(19) . . ? N4 Cd1 C45 90.81(15) 1_456 . ? N1 Cd1 C45 95.19(16) . . ? O9 Cd1 C45 27.32(15) . . ? O5 Cd1 C45 106.56(15) . . ? O10 Cd1 C45 27.35(15) . . ? O6 Cd1 C45 158.80(15) . . ? O12 Cd2 O11 130.03(16) 3_677 . ? O12 Cd2 N5 88.88(16) 3_677 . ? O11 Cd2 N5 87.53(16) . . ? O12 Cd2 N8 89.23(16) 3_677 1_456 ? O11 Cd2 N8 96.81(16) . 1_456 ? N5 Cd2 N8 175.50(17) . 1_456 ? O12 Cd2 O8 145.24(15) 3_677 2_556 ? O11 Cd2 O8 84.68(16) . 2_556 ? N5 Cd2 O8 91.24(15) . 2_556 ? N8 Cd2 O8 88.00(15) 1_456 2_556 ? O12 Cd2 O7 91.54(14) 3_677 2_556 ? O11 Cd2 O7 137.59(16) . 2_556 ? N5 Cd2 O7 85.00(14) . 2_556 ? N8 Cd2 O7 90.97(14) 1_456 2_556 ? O8 Cd2 O7 53.90(14) 2_556 2_556 ? C5 N1 C1 116.8(5) . . ? C5 N1 Cd1 119.6(4) . . ? C1 N1 Cd1 123.6(4) . . ? C6 N2 C3 125.9(6) . . ? C6 N2 H2A 117.1 . . ? C3 N2 H2A 117.1 . . ? C11 N3 C12 127.1(5) . . ? C11 N3 H3A 116.5 . . ? C12 N3 H3A 116.5 . . ? C14 N4 C15 116.3(5) . . ? C14 N4 Cd1 125.5(4) . 1_654 ? C15 N4 Cd1 118.1(4) . 1_654 ? C21 N5 C17 116.2(5) . . ? C21 N5 Cd2 122.9(4) . . ? C17 N5 Cd2 120.2(4) . . ? C22 N6 C19 128.1(5) . . ? C22 N6 H6A 115.9 . . ? C19 N6 H6A 115.9 . . ? C27 N7 C28 127.3(6) . . ? C27 N7 H7A 116.3 . . ? C28 N7 H7A 116.3 . . ? C30 N8 C31 115.7(5) . . ? C30 N8 Cd2 120.0(4) . 1_654 ? C31 N8 Cd2 124.4(4) . 1_654 ? C33 O5 Cd1 98.2(3) . . ? C33 O6 Cd1 86.7(3) . . ? C38 O7 Cd2 86.4(3) . 2_546 ? C38 O8 Cd2 95.6(4) . 2_546 ? C45 O9 Cd1 94.1(3) . . ? C45 O10 Cd1 90.5(3) . . ? C50 O11 Cd2 103.7(4) . . ? C50 O12 Cd2 162.5(4) . 3_677 ? Cd1 O13 H13A 123.8 . . ? Cd1 O13 H13C 120.1 . . ? H13A O13 H13C 105.6 . . ? N1 C1 C2 123.3(6) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C1 C2 C3 119.6(6) . . ? C1 C2 H2B 120.2 . . ? C3 C2 H2B 120.2 . . ? C4 C3 C2 117.2(5) . . ? C4 C3 N2 123.3(6) . . ? C2 C3 N2 119.4(5) . . ? C5 C4 C3 119.3(6) . . ? C5 C4 H4B 120.4 . . ? C3 C4 H4B 120.4 . . ? N1 C5 C4 123.8(6) . . ? N1 C5 H5A 118.1 . . ? C4 C5 H5A 118.1 . . ? O1 C6 N2 123.2(6) . . ? O1 C6 C7 123.9(6) . . ? N2 C6 C7 112.9(6) . . ? C6 C7 C8 112.8(6) . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? C6 C7 H7C 109.0 . . ? C8 C7 H7C 109.0 . . ? H7B C7 H7C 107.8 . . ? C9 C8 C7 113.1(6) . . ? C9 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? C9 C8 H8C 109.0 . . ? C7 C8 H8C 109.0 . . ? H8B C8 H8C 107.8 . . ? C8 C9 C10 111.6(6) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.2(6) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? O2 C11 N3 123.9(6) . . ? O2 C11 C10 123.0(6) . . ? N3 C11 C10 113.0(6) . . ? C13 C12 C16 116.6(5) . . ? C13 C12 N3 125.2(5) . . ? C16 C12 N3 118.1(5) . . ? C14 C13 C12 119.1(6) . . ? C14 C13 H13B 120.5 . . ? C12 C13 H13B 120.5 . . ? N4 C14 C13 124.4(6) . . ? N4 C14 H14A 117.8 . . ? C13 C14 H14A 117.8 . . ? N4 C15 C16 123.2(6) . . ? N4 C15 H15A 118.4 . . ? C16 C15 H15A 118.4 . . ? C15 C16 C12 120.2(6) . . ? C15 C16 H16A 119.9 . . ? C12 C16 H16A 119.9 . . ? N5 C17 C18 125.3(5) . . ? N5 C17 H17A 117.4 . . ? C18 C17 H17A 117.4 . . ? C17 C18 C19 117.4(6) . . ? C17 C18 H18A 121.3 . . ? C19 C18 H18A 121.3 . . ? N6 C19 C20 118.1(5) . . ? N6 C19 C18 124.5(6) . . ? C20 C19 C18 117.5(5) . . ? C21 C20 C19 120.0(6) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? N5 C21 C20 123.6(6) . . ? N5 C21 H21A 118.2 . . ? C20 C21 H21A 118.2 . . ? O3 C22 N6 123.1(6) . . ? O3 C22 C23 123.3(6) . . ? N6 C22 C23 113.6(6) . . ? C24 C23 C22 111.3(6) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 113.6(5) . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C24 C25 C26 113.7(5) . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 112.5(6) . . ? C27 C26 H26A 109.1 . . ? C25 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? C25 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? O4 C27 N7 123.1(6) . . ? O4 C27 C26 123.1(6) . . ? N7 C27 C26 113.7(6) . . ? C29 C28 C32 117.2(5) . . ? C29 C28 N7 118.1(6) . . ? C32 C28 N7 124.7(6) . . ? C28 C29 C30 119.9(6) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? N8 C30 C29 124.1(6) . . ? N8 C30 H30A 118.0 . . ? C29 C30 H30A 118.0 . . ? N8 C31 C32 124.2(6) . . ? N8 C31 H31A 117.9 . . ? C32 C31 H31A 117.9 . . ? C28 C32 C31 118.8(6) . . ? C28 C32 H32A 120.6 . . ? C31 C32 H32A 120.6 . . ? O6 C33 O5 122.5(5) . . ? O6 C33 C34 119.3(5) . . ? O5 C33 C34 118.1(5) . . ? C35 C34 C44 120.1(5) . . ? C35 C34 C33 120.1(5) . . ? C44 C34 C33 119.8(5) . . ? C34 C35 C36 120.3(5) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C37 C36 C35 121.6(5) . . ? C37 C36 H36A 119.2 . . ? C35 C36 H36A 119.2 . . ? C36 C37 C39 119.7(5) . . ? C36 C37 C38 120.5(5) . . ? C39 C37 C38 119.7(5) . . ? O7 C38 O8 124.0(5) . . ? O7 C38 C37 119.7(5) . . ? O8 C38 C37 116.3(5) . . ? C44 C39 C40 118.6(5) . . ? C44 C39 C37 119.1(5) . . ? C40 C39 C37 122.3(5) . . ? C41 C40 C39 121.6(5) . . ? C41 C40 H40A 119.2 . . ? C39 C40 H40A 119.2 . . ? C40 C41 C42 119.3(5) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? C43 C42 C41 121.2(5) . . ? C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 120.4(5) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C39 C44 C43 118.9(5) . . ? C39 C44 C34 119.1(5) . . ? C43 C44 C34 122.0(5) . . ? O10 C45 O9 120.2(5) . . ? O10 C45 C46 118.8(5) . . ? O9 C45 C46 120.9(5) . . ? O10 C45 Cd1 62.1(3) . . ? O9 C45 Cd1 58.5(3) . . ? C46 C45 Cd1 172.9(3) . . ? C47 C46 C56 118.6(5) . . ? C47 C46 C45 116.3(5) . . ? C56 C46 C45 125.0(5) . . ? C46 C47 C48 122.0(5) . . ? C46 C47 H47A 119.0 . . ? C48 C47 H47A 119.0 . . ? C49 C48 C47 120.6(5) . . ? C49 C48 H48A 119.7 . . ? C47 C48 H48A 119.7 . . ? C48 C49 C51 120.4(5) . . ? C48 C49 C50 116.1(5) . . ? C51 C49 C50 123.5(5) . . ? O12 C50 O11 123.3(6) . . ? O12 C50 C49 118.5(5) . . ? O11 C50 C49 118.2(6) . . ? C52 C51 C49 122.8(5) . . ? C52 C51 C56 118.5(5) . . ? C49 C51 C56 118.5(5) . . ? C53 C52 C51 121.2(6) . . ? C53 C52 H52A 119.4 . . ? C51 C52 H52A 119.4 . . ? C52 C53 C54 120.4(6) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C55 C54 C53 120.5(6) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C54 C55 C56 121.4(6) . . ? C54 C55 H55A 119.3 . . ? C56 C55 H55A 119.3 . . ? C51 C56 C55 118.0(5) . . ? C51 C56 C46 119.8(5) . . ? C55 C56 C46 122.2(5) . . ? C57 N9 C59 122.3(10) . . ? C57 N9 C58 122.0(10) . . ? C59 N9 C58 115.6(9) . . ? O14 C57 N9 125.3(13) . . ? O14 C57 H57A 117.3 . . ? N9 C57 H57A 117.3 . . ? C62 N10 C61 121.7(4) . . ? C62 N10 C60 122.1(4) . . ? C61 N10 C60 116.2(4) . . ? O15 C62 O15' 120.0(10) . . ? O15 C62 N10 119.9(6) . . ? O15' C62 N10 120.1(7) . . ? H16B O16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.830 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.118 # End of data2 data_3 _database_code_depnum_ccdc_archive 'CCDC 866973' #TrackingRef '- all-2nd-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Cd N4 O9' _chemical_formula_weight 702.98 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 12.230(2) _cell_length_b 14.6964(15) _cell_length_c 18.117(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.946(14) _cell_angle_gamma 90.00 _cell_volume 3244.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 16.88 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9385 _exptl_absorpt_correction_T_max 0.9754 _exptl_absorpt_process_details '(XSCANS; Siemens, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7130 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5712 _reflns_number_gt 3155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens, 1995)' _computing_cell_refinement XSCANS _computing_data_reduction 'SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (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^)+(0.0501P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5712 _refine_ls_number_parameters 413 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Cd Cd 0.37774(3) 0.49788(3) 0.24069(2) 0.05229(15) Uani 1 1 d . . . O1 O 0.7735(4) 0.2579(3) 0.0308(2) 0.0875(14) Uani 1 1 d . . . O2 O 0.7536(3) 0.7463(3) 0.5039(2) 0.0730(11) Uani 1 1 d . . . O3 O 0.3554(4) 0.3474(2) 0.2820(2) 0.0723(11) Uani 1 1 d . . . O4 O 0.2487(3) 0.3963(2) 0.1881(2) 0.0691(11) Uani 1 1 d . . . O5 O 0.0589(3) -0.0020(3) 0.2171(3) 0.0802(12) Uani 1 1 d . . . O6 O 0.3508(4) -0.3552(2) 0.1927(2) 0.0757(12) Uani 1 1 d . . . O7 O 0.2497(3) -0.3991(2) 0.2795(2) 0.0700(11) Uani 1 1 d . . . N1 N 0.5012(4) 0.4673(3) 0.1557(3) 0.0579(12) Uani 1 1 d . . . N2 N 0.7509(4) 0.4100(3) 0.0191(2) 0.0577(12) Uani 1 1 d . . . H2A H 0.7748 0.4574 -0.0023 0.069 Uiso 1 1 calc R . . N3 N 0.4951(4) 0.5304(3) 0.3417(3) 0.0587(12) Uani 1 1 d . . . N4 N 0.7369(3) 0.5935(3) 0.5122(2) 0.0555(12) Uani 1 1 d . . . H4A H 0.7610 0.5468 0.5372 0.067 Uiso 1 1 calc R . . C1 C 0.5445(5) 0.3845(4) 0.1534(4) 0.0800(19) Uani 1 1 d . . . H1A H 0.5194 0.3404 0.1846 0.096 Uiso 1 1 calc R . . C2 C 0.6226(5) 0.3598(4) 0.1086(3) 0.0715(17) Uani 1 1 d . . . H2B H 0.6476 0.3001 0.1081 0.086 Uiso 1 1 calc R . . C3 C 0.6649(4) 0.4250(4) 0.0634(3) 0.0532(14) Uani 1 1 d . . . C4 C 0.6198(5) 0.5116(3) 0.0656(3) 0.0584(14) Uani 1 1 d . . . H4B H 0.6446 0.5575 0.0360 0.070 Uiso 1 1 calc R . . C5 C 0.5398(5) 0.5293(4) 0.1107(3) 0.0581(15) Uani 1 1 d . . . H5A H 0.5103 0.5877 0.1104 0.070 Uiso 1 1 calc R . . C6 C 0.8027(5) 0.3293(4) 0.0053(3) 0.0596(15) Uani 1 1 d . . . C7 C 0.8956(5) 0.3381(4) -0.0423(3) 0.0620(15) Uani 1 1 d . . . H7A H 0.9393 0.3908 -0.0265 0.074 Uiso 1 1 calc R . . H7B H 0.8665 0.3481 -0.0931 0.074 Uiso 1 1 calc R . . C8 C 0.9700(4) 0.2531(4) -0.0390(3) 0.0598(14) Uani 1 1 d . . . H8A H 1.0108 0.2503 0.0093 0.072 Uiso 1 1 calc R . . H8B H 0.9243 0.1991 -0.0446 0.072 Uiso 1 1 calc R . . C9 C 0.5355(5) 0.4697(3) 0.3915(3) 0.0560(14) Uani 1 1 d . . . H9A H 0.5086 0.4105 0.3876 0.067 Uiso 1 1 calc R . . C10 C 0.6139(4) 0.4885(3) 0.4479(3) 0.0542(13) Uani 1 1 d . . . H10A H 0.6400 0.4428 0.4802 0.065 Uiso 1 1 calc R . . C11 C 0.6542(4) 0.5767(3) 0.4566(3) 0.0488(13) Uani 1 1 d . . . C12 C 0.6094(5) 0.6415(4) 0.4074(3) 0.0718(17) Uani 1 1 d . . . H12A H 0.6305 0.7022 0.4121 0.086 Uiso 1 1 calc R . . C13 C 0.5337(5) 0.6147(4) 0.3517(3) 0.0771(19) Uani 1 1 d . . . H13A H 0.5069 0.6589 0.3181 0.092 Uiso 1 1 calc R . . C14 C 0.7850(5) 0.6746(4) 0.5324(3) 0.0571(14) Uani 1 1 d . . . C15 C 0.8747(5) 0.6692(4) 0.5937(3) 0.0656(16) Uani 1 1 d . . . H15A H 0.9185 0.6153 0.5868 0.079 Uiso 1 1 calc R . . H15B H 0.8422 0.6627 0.6404 0.079 Uiso 1 1 calc R . . C16 C 0.9499(4) 0.7525(4) 0.5981(3) 0.0632(15) Uani 1 1 d . . . H16A H 0.9052 0.8071 0.5932 0.076 Uiso 1 1 calc R . . H16B H 0.9907 0.7541 0.6464 0.076 Uiso 1 1 calc R . . C17 C 0.2792(5) 0.3342(3) 0.2329(3) 0.0505(14) Uani 1 1 d . . . C18 C 0.2235(4) 0.2438(3) 0.2264(3) 0.0481(13) Uani 1 1 d . . . C19 C 0.2554(5) 0.1756(4) 0.2766(3) 0.0661(16) Uani 1 1 d . . . H19A H 0.3127 0.1862 0.3127 0.079 Uiso 1 1 calc R . . C20 C 0.2030(5) 0.0918(4) 0.2739(3) 0.0749(19) Uani 1 1 d . . . H20A H 0.2240 0.0463 0.3079 0.090 Uiso 1 1 calc R . . C21 C 0.1190(5) 0.0780(3) 0.2194(3) 0.0580(15) Uani 1 1 d . . . C22 C 0.0884(4) 0.1434(4) 0.1679(3) 0.0607(15) Uani 1 1 d . . . H22A H 0.0330 0.1317 0.1306 0.073 Uiso 1 1 calc R . . C23 C 0.1406(4) 0.2271(3) 0.1718(3) 0.0553(14) Uani 1 1 d . . . H23A H 0.1195 0.2722 0.1374 0.066 Uiso 1 1 calc R . . C24 C 0.1177(5) -0.0831(3) 0.2241(3) 0.0599(16) Uani 1 1 d . . . C25 C 0.2025(5) -0.0996(4) 0.1804(4) 0.0733(18) Uani 1 1 d . . . H25A H 0.2246 -0.0548 0.1486 0.088 Uiso 1 1 calc R . . C26 C 0.2538(5) -0.1824(3) 0.1842(3) 0.0676(17) Uani 1 1 d . . . H26A H 0.3098 -0.1941 0.1540 0.081 Uiso 1 1 calc R . . C27 C 0.2234(4) -0.2486(3) 0.2324(3) 0.0517(14) Uani 1 1 d . . . C28 C 0.1384(5) -0.2305(4) 0.2760(3) 0.0617(15) Uani 1 1 d . . . H28A H 0.1166 -0.2747 0.3084 0.074 Uiso 1 1 calc R . . C29 C 0.0861(5) -0.1475(4) 0.2717(3) 0.0653(16) Uani 1 1 d . . . H29A H 0.0293 -0.1356 0.3012 0.078 Uiso 1 1 calc R . . C30 C 0.2771(4) -0.3392(4) 0.2349(3) 0.0515(14) Uani 1 1 d . . . O8 O 0.1710(5) 0.4229(3) 0.0419(3) 0.0827(14) Uani 1 1 d . . . O9 O 0.1814(5) -0.4250(3) 0.4200(3) 0.0823(15) Uani 1 1 d . . . H8C H 0.197(8) 0.416(6) 0.088(5) 0.18(5) Uiso 1 1 d . . . H8D H 0.190(5) 0.377(4) 0.020(3) 0.07(2) Uiso 1 1 d . . . H9B H 0.178(6) -0.378(5) 0.439(4) 0.11(3) Uiso 1 1 d . . . H9C H 0.211(8) -0.437(6) 0.371(5) 0.19(4) Uiso 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 Cd 0.0528(2) 0.0350(2) 0.0686(3) -0.0038(2) 0.00262(17) -0.0006(2) O1 0.109(4) 0.046(3) 0.115(3) 0.007(2) 0.052(3) 0.014(3) O2 0.076(3) 0.050(3) 0.089(3) 0.001(2) -0.013(2) -0.018(2) O3 0.084(3) 0.049(2) 0.080(3) 0.006(2) -0.015(2) -0.017(2) O4 0.082(3) 0.041(2) 0.081(3) 0.005(2) -0.010(2) -0.010(2) O5 0.056(2) 0.0332(19) 0.151(4) 0.009(2) 0.010(2) -0.001(2) O6 0.088(3) 0.049(2) 0.094(3) 0.007(2) 0.030(3) 0.018(2) O7 0.079(3) 0.041(2) 0.092(3) 0.014(2) 0.021(2) 0.007(2) N1 0.055(3) 0.040(2) 0.079(3) -0.003(2) 0.013(2) 0.007(2) N2 0.064(3) 0.044(3) 0.067(3) 0.005(2) 0.014(2) 0.011(2) N3 0.056(3) 0.045(3) 0.074(3) -0.005(2) 0.002(2) -0.008(2) N4 0.061(3) 0.043(3) 0.062(3) 0.006(2) 0.000(2) -0.010(2) C1 0.084(5) 0.050(4) 0.111(5) 0.011(3) 0.040(4) 0.014(3) C2 0.082(4) 0.034(3) 0.102(5) 0.007(3) 0.030(4) 0.018(3) C3 0.056(4) 0.049(3) 0.054(3) -0.006(3) 0.003(3) 0.011(3) C4 0.066(3) 0.038(3) 0.072(3) -0.001(3) 0.005(3) 0.014(3) C5 0.061(4) 0.038(3) 0.075(4) -0.006(3) 0.007(3) 0.009(3) C6 0.067(4) 0.047(4) 0.065(4) 0.003(3) 0.006(3) 0.014(3) C7 0.073(4) 0.050(3) 0.064(4) 0.006(3) 0.007(3) 0.017(3) C8 0.063(4) 0.059(3) 0.056(3) 0.001(3) 0.000(3) 0.011(3) C9 0.055(4) 0.034(3) 0.079(4) -0.006(3) 0.010(3) -0.005(3) C10 0.052(3) 0.045(4) 0.065(3) -0.002(3) 0.001(3) -0.006(3) C11 0.047(3) 0.047(3) 0.053(3) -0.006(3) 0.006(3) -0.004(3) C12 0.077(4) 0.042(3) 0.092(4) 0.006(3) -0.020(4) -0.013(3) C13 0.081(5) 0.050(4) 0.094(5) 0.014(3) -0.024(4) -0.017(3) C14 0.062(4) 0.051(4) 0.058(4) 0.001(3) 0.008(3) -0.013(3) C15 0.080(4) 0.066(4) 0.050(3) 0.002(3) 0.000(3) -0.027(3) C16 0.068(4) 0.066(4) 0.054(3) 0.001(3) 0.002(3) -0.024(3) C17 0.055(4) 0.036(3) 0.061(4) -0.010(3) 0.013(3) 0.001(3) C18 0.051(4) 0.034(3) 0.061(3) -0.004(3) 0.009(3) -0.001(3) C19 0.068(4) 0.046(3) 0.081(4) 0.009(3) -0.011(3) -0.003(3) C20 0.078(4) 0.042(3) 0.099(5) 0.020(3) -0.023(4) -0.007(3) C21 0.051(4) 0.031(3) 0.094(5) -0.002(3) 0.017(3) -0.002(3) C22 0.052(3) 0.043(3) 0.085(4) -0.004(3) -0.001(3) 0.003(3) C23 0.057(4) 0.037(3) 0.071(4) 0.001(3) 0.004(3) 0.003(3) C24 0.045(4) 0.031(3) 0.104(5) -0.003(3) 0.006(3) -0.005(3) C25 0.073(4) 0.039(3) 0.112(5) 0.026(3) 0.029(4) 0.003(3) C26 0.073(4) 0.040(3) 0.095(4) 0.009(3) 0.033(4) 0.001(3) C27 0.046(4) 0.039(3) 0.069(4) 0.001(3) 0.005(3) -0.003(3) C28 0.062(4) 0.041(3) 0.083(4) 0.008(3) 0.008(3) -0.003(3) C29 0.057(4) 0.045(3) 0.097(5) 0.004(3) 0.021(3) 0.003(3) C30 0.043(4) 0.044(3) 0.066(4) -0.007(3) -0.004(3) 0.001(3) O8 0.123(4) 0.043(3) 0.082(4) 0.008(3) 0.007(3) 0.008(3) O9 0.117(4) 0.048(3) 0.081(3) 0.007(3) -0.001(3) 0.000(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 Cd N3 2.277(4) . ? Cd N1 2.292(4) . ? Cd O4 2.317(4) . ? Cd O7 2.330(4) 1_565 ? Cd O6 2.340(4) 1_565 ? Cd O3 2.358(4) . ? Cd C17 2.689(5) . ? Cd C30 2.690(5) 1_565 ? O1 C6 1.212(6) . ? O2 C14 1.221(6) . ? O3 C17 1.247(6) . ? O4 C17 1.256(6) . ? O5 C21 1.385(6) . ? O5 C24 1.392(6) . ? O6 C30 1.254(6) . ? O6 Cd 2.340(4) 1_545 ? O7 C30 1.260(6) . ? O7 Cd 2.330(4) 1_545 ? N1 C1 1.330(6) . ? N1 C5 1.336(7) . ? N2 C6 1.379(6) . ? N2 C3 1.395(6) . ? N2 H2A 0.8600 . ? N3 C13 1.332(6) . ? N3 C9 1.334(7) . ? N4 C14 1.365(6) . ? N4 C11 1.387(6) . ? N4 H4A 0.8600 . ? C1 C2 1.355(7) . ? C1 H1A 0.9300 . ? C2 C3 1.388(7) . ? C2 H2B 0.9300 . ? C3 C4 1.389(6) . ? C4 C5 1.353(7) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.489(7) . ? C7 C8 1.544(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C16 1.511(7) 2_745 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.369(7) . ? C9 H9A 0.9300 . ? C10 C11 1.390(6) . ? C10 H10A 0.9300 . ? C11 C12 1.385(7) . ? C12 C13 1.368(7) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.495(7) . ? C15 C16 1.530(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C8 1.511(7) 2_755 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.492(7) . ? C18 C23 1.377(7) . ? C18 C19 1.388(7) . ? C19 C20 1.386(7) . ? C19 H19A 0.9300 . ? C20 C21 1.378(8) . ? C20 H20A 0.9300 . ? C21 C22 1.369(7) . ? C22 C23 1.385(7) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C29 1.359(7) . ? C24 C25 1.379(7) . ? C25 C26 1.368(7) . ? C25 H25A 0.9300 . ? C26 C27 1.379(7) . ? C26 H26A 0.9300 . ? C27 C28 1.385(7) . ? C27 C30 1.483(7) . ? C28 C29 1.376(7) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 Cd 2.690(5) 1_545 ? O8 H8C 0.87(8) . ? O8 H8D 0.82(6) . ? O9 H9B 0.77(7) . ? O9 H9C 1.01(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd N1 100.06(16) . . ? N3 Cd O4 145.66(15) . . ? N1 Cd O4 93.57(15) . . ? N3 Cd O7 90.84(15) . 1_565 ? N1 Cd O7 146.01(15) . 1_565 ? O4 Cd O7 95.22(14) . 1_565 ? N3 Cd O6 99.42(16) . 1_565 ? N1 Cd O6 90.64(15) . 1_565 ? O4 Cd O6 111.88(14) . 1_565 ? O7 Cd O6 55.67(13) 1_565 1_565 ? N3 Cd O3 91.39(15) . . ? N1 Cd O3 97.48(15) . . ? O4 Cd O3 55.43(13) . . ? O7 Cd O3 114.47(14) 1_565 . ? O6 Cd O3 165.16(15) 1_565 . ? N3 Cd C17 118.62(17) . . ? N1 Cd C17 96.16(15) . . ? O4 Cd C17 27.81(14) . . ? O7 Cd C17 106.69(14) 1_565 . ? O6 Cd C17 139.26(18) 1_565 . ? O3 Cd C17 27.63(14) . . ? N3 Cd C30 95.69(16) . 1_565 ? N1 Cd C30 118.31(18) . 1_565 ? O4 Cd C30 105.33(14) . 1_565 ? O7 Cd C30 27.91(14) 1_565 1_565 ? O6 Cd C30 27.76(14) 1_565 1_565 ? O3 Cd C30 141.44(17) . 1_565 ? C17 Cd C30 126.35(15) . 1_565 ? C17 O3 Cd 91.1(3) . . ? C17 O4 Cd 92.8(3) . . ? C21 O5 C24 117.1(4) . . ? C30 O6 Cd 91.9(3) . 1_545 ? C30 O7 Cd 92.1(3) . 1_545 ? C1 N1 C5 116.3(5) . . ? C1 N1 Cd 119.2(4) . . ? C5 N1 Cd 124.3(4) . . ? C6 N2 C3 128.5(5) . . ? C6 N2 H2A 115.8 . . ? C3 N2 H2A 115.8 . . ? C13 N3 C9 115.1(5) . . ? C13 N3 Cd 119.7(4) . . ? C9 N3 Cd 125.0(4) . . ? C14 N4 C11 128.4(5) . . ? C14 N4 H4A 115.8 . . ? C11 N4 H4A 115.8 . . ? N1 C1 C2 124.5(6) . . ? N1 C1 H1A 117.7 . . ? C2 C1 H1A 117.7 . . ? C1 C2 C3 119.1(5) . . ? C1 C2 H2B 120.5 . . ? C3 C2 H2B 120.5 . . ? C2 C3 C4 116.5(5) . . ? C2 C3 N2 124.6(5) . . ? C4 C3 N2 118.8(5) . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4B 119.9 . . ? C3 C4 H4B 119.9 . . ? N1 C5 C4 123.3(5) . . ? N1 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? O1 C6 N2 121.3(5) . . ? O1 C6 C7 124.1(5) . . ? N2 C6 C7 114.6(5) . . ? C6 C7 C8 112.6(4) . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C16 C8 C7 113.2(4) 2_745 . ? C16 C8 H8A 108.9 2_745 . ? C7 C8 H8A 108.9 . . ? C16 C8 H8B 108.9 2_745 . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.8 . . ? N3 C9 C10 124.4(5) . . ? N3 C9 H9A 117.8 . . ? C10 C9 H9A 117.8 . . ? C9 C10 C11 119.5(5) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C12 C11 N4 124.6(5) . . ? C12 C11 C10 116.9(5) . . ? N4 C11 C10 118.5(5) . . ? C13 C12 C11 118.8(5) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? N3 C13 C12 125.3(5) . . ? N3 C13 H13A 117.4 . . ? C12 C13 H13A 117.4 . . ? O2 C14 N4 121.9(5) . . ? O2 C14 C15 122.9(5) . . ? N4 C14 C15 115.1(5) . . ? C14 C15 C16 113.3(5) . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C8 C16 C15 113.1(5) 2_755 . ? C8 C16 H16A 109.0 2_755 . ? C15 C16 H16A 109.0 . . ? C8 C16 H16B 109.0 2_755 . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? O3 C17 O4 120.6(5) . . ? O3 C17 C18 120.2(5) . . ? O4 C17 C18 119.2(5) . . ? O3 C17 Cd 61.3(3) . . ? O4 C17 Cd 59.4(3) . . ? C18 C17 Cd 178.5(4) . . ? C23 C18 C19 119.4(5) . . ? C23 C18 C17 121.2(5) . . ? C19 C18 C17 119.4(5) . . ? C20 C19 C18 121.0(5) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C21 C20 C19 118.1(5) . . ? C21 C20 H20A 121.0 . . ? C19 C20 H20A 121.0 . . ? C22 C21 C20 121.9(5) . . ? C22 C21 O5 117.5(5) . . ? C20 C21 O5 120.5(5) . . ? C21 C22 C23 119.4(5) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C18 C23 C22 120.2(5) . . ? C18 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C29 C24 C25 120.7(5) . . ? C29 C24 O5 118.8(5) . . ? C25 C24 O5 120.4(5) . . ? C26 C25 C24 119.4(5) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C25 C26 C27 120.8(5) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C26 C27 C28 118.8(5) . . ? C26 C27 C30 120.7(5) . . ? C28 C27 C30 120.4(5) . . ? C29 C28 C27 120.4(5) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C24 C29 C28 119.8(5) . . ? C24 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? O6 C30 O7 120.3(5) . . ? O6 C30 C27 119.3(5) . . ? O7 C30 C27 120.4(5) . . ? O6 C30 Cd 60.4(3) . 1_545 ? O7 C30 Cd 59.9(3) . 1_545 ? C27 C30 Cd 178.9(4) . 1_545 ? H8C O8 H8D 105(7) . . ? H9B O9 H9C 126(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.659 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.066 # End of data3 data_4 _database_code_depnum_ccdc_archive 'CCDC 866974' #TrackingRef '- all-2nd-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 Cd N4 O9.50 S' _chemical_formula_weight 742.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9666(2) _cell_length_b 13.4111(4) _cell_length_c 14.7643(4) _cell_angle_alpha 78.5410(10) _cell_angle_beta 82.9790(10) _cell_angle_gamma 89.2230(10) _cell_volume 1534.30(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 754 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7111 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _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_reflns_number 23651 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6345 _reflns_number_gt 5607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0373P)^2^+1.2354P] 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 6345 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Cd Cd 0.65367(2) 0.653711(15) 0.836747(13) 0.04040(8) Uani 1 1 d . . . S S 1.51481(11) 0.86009(7) 0.42397(6) 0.0599(2) Uani 1 1 d . . . O1 O 0.9366(3) 0.6827(2) 1.28699(18) 0.0689(7) Uani 1 1 d . B . O2 O -0.0956(15) 0.8834(11) 1.0582(6) 0.062(2) Uani 0.50 1 d P A 1 O3 O 0.7767(6) 0.7853(4) 0.7066(3) 0.0480(12) Uiso 0.50 1 d P B 1 O2' O -0.1071(16) 0.8915(11) 1.0151(9) 0.057(4) Uani 0.50 1 d P B 2 O3' O 0.8054(6) 0.8019(4) 0.7304(3) 0.0478(12) Uiso 0.50 1 d P B 2 O4 O 0.9287(3) 0.65764(17) 0.76911(15) 0.0547(5) Uani 1 1 d . B . O5 O 1.6709(3) 0.8460(2) 0.4639(2) 0.0809(8) Uani 1 1 d . . . O6 O 1.4839(4) 0.95391(19) 0.3631(2) 0.0841(9) Uani 1 1 d . . . O7 O 1.4603(3) 0.42569(18) 0.26648(17) 0.0622(6) Uani 1 1 d . . . O8 O 1.377(2) 0.5364(19) 0.1527(19) 0.051(3) Uani 0.50 1 d P . 1 O8' O 1.333(2) 0.525(2) 0.1568(19) 0.057(3) Uani 0.50 1 d P . 2 N1 N 0.7182(3) 0.61238(17) 0.98591(16) 0.0427(5) Uani 1 1 d . B . N2 N 0.9253(3) 0.53432(19) 1.23682(16) 0.0467(6) Uani 1 1 d . B . H2A H 0.9499 0.4709 1.2507 0.056 Uiso 1 1 calc R . . N3 N 0.4478(3) 0.76528(17) 0.86721(17) 0.0431(5) Uani 1 1 d . B . N4 N -0.0205(14) 0.9115(8) 0.9014(7) 0.060(2) Uani 0.50 1 d P A 1 H4C H -0.0648 0.9367 0.8517 0.072 Uiso 0.50 1 calc PR A 1 N4' N 0.0102(12) 0.9380(8) 0.8638(6) 0.0489(19) Uani 0.50 1 d P B 2 H4'A H 0.0041 0.9755 0.8099 0.059 Uiso 0.50 1 calc PR B 2 C1 C 0.7740(4) 0.5188(2) 1.0178(2) 0.0495(7) Uani 1 1 d . . . H1A H 0.7673 0.4696 0.9820 0.059 Uiso 1 1 calc R B . C2 C 0.8403(4) 0.4921(2) 1.1002(2) 0.0481(7) Uani 1 1 d . B . H2B H 0.8753 0.4258 1.1202 0.058 Uiso 1 1 calc R . . C3 C 0.8551(3) 0.5649(2) 1.15404(18) 0.0406(6) Uani 1 1 d . . . C4 C 0.7957(4) 0.6614(2) 1.1222(2) 0.0459(6) Uani 1 1 d . B . H4A H 0.8008 0.7124 1.1564 0.055 Uiso 1 1 calc R . . C5 C 0.7292(4) 0.6803(2) 1.0391(2) 0.0458(7) Uani 1 1 d . . . H5A H 0.6890 0.7453 1.0187 0.055 Uiso 1 1 calc R B . C6 C 0.9598(4) 0.5921(3) 1.2986(2) 0.0511(7) Uani 1 1 d . . . C7 C 1.0229(5) 0.5306(3) 1.3854(2) 0.0674(10) Uani 1 1 d . B . H7A H 1.1021 0.4821 1.3661 0.081 Uiso 0.50 1 d PR C 1 H7B H 1.0845 0.5760 1.4124 0.081 Uiso 0.50 1 d PR C 1 H7C H 0.9442 0.4765 1.4136 0.081 Uiso 0.50 1 d PR C 2 H7D H 1.1294 0.5008 1.3683 0.081 Uiso 0.50 1 d PR C 2 C8 C 0.9029(9) 0.4769(7) 1.4591(4) 0.079(3) Uani 0.50 1 d P B 1 H8A H 0.8277 0.5268 1.4795 0.095 Uiso 0.50 1 d PR B 1 H8B H 0.8373 0.4355 1.4302 0.095 Uiso 0.50 1 d PR B 1 C8' C 1.0439(10) 0.5928(6) 1.4540(5) 0.069(2) Uani 0.50 1 d P B 2 H8'A H 1.1292 0.6439 1.4282 0.083 Uiso 0.50 1 d PR B 2 H8'B H 0.9396 0.6261 1.4688 0.083 Uiso 0.50 1 d PR B 2 C9 C 0.3329(4) 0.7435(2) 0.9422(2) 0.0517(7) Uani 1 1 d . . . H9A H 0.3555 0.6908 0.9903 0.062 Uiso 1 1 calc R B . C10 C 0.1831(4) 0.7945(3) 0.9524(3) 0.0646(10) Uani 1 1 d . B . H10A H 0.1068 0.7766 1.0061 0.078 Uiso 1 1 calc R . . C11 C 0.1479(4) 0.8735(3) 0.8811(3) 0.0650(10) Uani 1 1 d . . . C12 C 0.2693(5) 0.8989(3) 0.8053(3) 0.0668(10) Uani 1 1 d . B . H12A H 0.2524 0.9535 0.7576 0.080 Uiso 1 1 calc R . . C13 C 0.4148(4) 0.8437(2) 0.8002(2) 0.0528(7) Uani 1 1 d . . . H13A H 0.4942 0.8614 0.7479 0.063 Uiso 1 1 calc R B . C14 C -0.128(2) 0.9172(9) 0.9819(14) 0.050(6) Uani 0.50 1 d P A 1 C15 C -0.2903(12) 0.9766(7) 0.9580(7) 0.064(2) Uani 0.50 1 d P A 1 H15A H -0.2656 1.0490 0.9442 0.077 Uiso 0.50 1 calc PR A 1 H15B H -0.3268 0.9584 0.9030 0.077 Uiso 0.50 1 calc PR A 1 C16 C -0.4307(10) 0.9528(6) 1.0381(8) 0.062(2) Uani 0.50 1 d P . 1 H16A H -0.4637 0.8824 1.0493 0.074 Uiso 0.50 1 d PR . 1 H16B H -0.3925 0.9666 1.0936 0.074 Uiso 0.50 1 d PR . 1 C14' C -0.1153(17) 0.9387(10) 0.9373(8) 0.043(3) Uani 0.50 1 d P B 2 C15' C -0.2654(12) 1.0024(7) 0.9069(7) 0.058(2) Uani 0.50 1 d P B 2 H15C H -0.2350 1.0740 0.8949 0.070 Uiso 0.50 1 calc PR B 2 H15D H -0.2952 0.9863 0.8496 0.070 Uiso 0.50 1 calc PR B 2 C16' C -0.4158(11) 0.9815(7) 0.9815(7) 0.061(2) Uani 0.50 1 d P . 2 H16C H -0.4493 0.9114 0.9908 0.074 Uiso 0.50 1 d PR . 2 H16D H -0.3825 0.9934 1.0388 0.074 Uiso 0.50 1 d PR . 2 C17 C 0.9202(4) 0.7420(2) 0.7154(2) 0.0454(6) Uani 1 1 d . B . C18 C 1.0712(4) 0.7777(2) 0.6456(2) 0.0444(6) Uani 1 1 d . . . C19 C 1.0546(5) 0.8523(3) 0.5685(3) 0.0688(10) Uani 1 1 d . B . H19A H 0.9510 0.8837 0.5612 0.083 Uiso 1 1 calc R . . C20 C 1.1923(5) 0.8804(3) 0.5019(3) 0.0716(11) Uani 1 1 d . . . H20A H 1.1816 0.9299 0.4491 0.086 Uiso 1 1 calc R B . C21 C 1.3453(4) 0.8344(2) 0.5146(2) 0.0502(7) Uani 1 1 d . B . C22 C 1.3645(4) 0.7622(3) 0.5920(2) 0.0523(7) Uani 1 1 d . . . H22A H 1.4695 0.7332 0.6005 0.063 Uiso 1 1 calc R B . C23 C 1.2262(4) 0.7329(2) 0.6573(2) 0.0491(7) Uani 1 1 d . B . H23A H 1.2373 0.6827 0.7095 0.059 Uiso 1 1 calc R . . C24 C 1.4915(4) 0.7596(2) 0.3642(2) 0.0479(7) Uani 1 1 d . . . C25 C 1.4125(5) 0.7765(3) 0.2852(2) 0.0586(8) Uani 1 1 d . . . H25A H 1.3744 0.8411 0.2615 0.070 Uiso 1 1 calc R . . C26 C 1.3898(4) 0.6972(3) 0.2411(2) 0.0578(8) Uani 1 1 d . . . H26A H 1.3365 0.7086 0.1873 0.069 Uiso 1 1 calc R . . C27 C 1.4456(3) 0.6004(2) 0.27592(19) 0.0442(6) Uani 1 1 d . . . C28 C 1.5245(4) 0.5845(2) 0.3561(2) 0.0494(7) Uani 1 1 d . . . H28A H 1.5617 0.5199 0.3804 0.059 Uiso 1 1 calc R . . C29 C 1.5484(4) 0.6641(3) 0.4001(2) 0.0529(7) Uani 1 1 d . . . H29A H 1.6025 0.6533 0.4535 0.063 Uiso 1 1 calc R . . C30 C 1.4187(4) 0.5134(3) 0.2289(2) 0.0487(7) Uani 1 1 d . . . O9 O 0.9664(5) 0.8894(3) 0.3064(4) 0.1511(18) Uani 1 1 d . . . H9B H 0.8870 0.9211 0.3322 0.181 Uiso 1 1 d R . . H9D H 0.9305 0.8210 0.3079 0.181 Uiso 1 1 d R . . O10 O 0.8504(12) 0.9932(7) 0.7423(6) 0.137(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.03746(12) 0.04176(12) 0.03934(12) -0.00379(8) -0.00235(8) 0.01033(8) S 0.0592(5) 0.0531(5) 0.0634(5) -0.0164(4) 0.0178(4) -0.0148(4) O1 0.0828(18) 0.0645(16) 0.0677(15) -0.0251(13) -0.0226(13) 0.0077(13) O2 0.047(3) 0.052(4) 0.083(6) -0.012(6) 0.005(5) 0.007(3) O2' 0.041(6) 0.051(6) 0.068(11) 0.007(8) 0.011(6) 0.015(4) O4 0.0464(12) 0.0570(13) 0.0512(12) 0.0060(10) 0.0033(9) 0.0101(10) O5 0.0504(14) 0.103(2) 0.097(2) -0.0468(17) 0.0091(13) -0.0246(14) O6 0.106(2) 0.0501(14) 0.0818(18) -0.0037(13) 0.0326(16) -0.0150(14) O7 0.0688(15) 0.0559(13) 0.0677(15) -0.0198(12) -0.0208(12) 0.0145(12) O8 0.041(7) 0.061(6) 0.053(4) -0.016(4) -0.010(5) -0.014(5) O8' 0.051(8) 0.068(6) 0.051(5) -0.007(4) -0.018(6) -0.021(6) N1 0.0439(13) 0.0401(12) 0.0410(12) -0.0013(10) -0.0050(10) 0.0056(10) N2 0.0503(14) 0.0516(14) 0.0372(12) -0.0072(10) -0.0054(10) 0.0101(11) N3 0.0381(12) 0.0395(12) 0.0523(14) -0.0100(10) -0.0067(10) 0.0084(10) N4 0.050(5) 0.067(7) 0.069(7) -0.025(5) -0.014(5) 0.027(5) N4' 0.037(4) 0.051(5) 0.055(5) -0.005(3) -0.001(4) 0.016(3) C1 0.0647(19) 0.0422(15) 0.0414(15) -0.0063(12) -0.0095(13) 0.0083(14) C2 0.0624(19) 0.0387(15) 0.0417(15) -0.0034(12) -0.0098(13) 0.0130(13) C3 0.0362(13) 0.0478(15) 0.0350(13) -0.0056(11) 0.0022(10) 0.0035(12) C4 0.0467(16) 0.0435(15) 0.0478(16) -0.0108(13) -0.0043(12) 0.0057(13) C5 0.0454(16) 0.0374(14) 0.0519(16) -0.0020(12) -0.0069(13) 0.0084(12) C6 0.0451(16) 0.066(2) 0.0432(16) -0.0141(14) -0.0025(13) 0.0031(15) C7 0.080(2) 0.077(2) 0.0498(19) -0.0176(17) -0.0200(17) 0.009(2) C8 0.065(4) 0.141(7) 0.027(3) -0.013(4) -0.003(3) 0.052(5) C8' 0.074(5) 0.089(5) 0.047(4) -0.018(4) -0.014(3) 0.017(4) C9 0.0384(15) 0.0400(15) 0.073(2) -0.0076(14) 0.0006(14) 0.0056(12) C10 0.0372(16) 0.0527(19) 0.104(3) -0.0257(19) 0.0076(17) 0.0040(14) C11 0.0465(18) 0.057(2) 0.108(3) -0.045(2) -0.0316(19) 0.0245(16) C12 0.076(2) 0.057(2) 0.075(2) -0.0206(18) -0.032(2) 0.0352(18) C13 0.0596(19) 0.0471(16) 0.0554(18) -0.0139(14) -0.0163(15) 0.0166(14) C14 0.034(5) 0.032(9) 0.08(2) -0.012(11) -0.004(9) 0.010(6) C15 0.035(5) 0.060(6) 0.103(8) -0.035(6) -0.004(5) 0.016(4) C16 0.029(3) 0.051(5) 0.112(7) -0.036(5) -0.003(5) 0.012(3) C14' 0.035(4) 0.030(5) 0.062(7) -0.008(5) 0.001(6) -0.003(3) C15' 0.036(4) 0.053(5) 0.085(6) -0.018(5) 0.001(5) 0.014(3) C16' 0.037(5) 0.057(5) 0.091(6) -0.023(5) 0.000(5) 0.010(3) C17 0.0415(15) 0.0467(16) 0.0468(15) -0.0098(13) -0.0004(12) 0.0075(12) C18 0.0438(15) 0.0416(14) 0.0455(15) -0.0080(12) 0.0023(12) 0.0033(12) C19 0.058(2) 0.0560(19) 0.076(2) 0.0116(17) 0.0099(17) 0.0226(16) C20 0.071(2) 0.054(2) 0.072(2) 0.0165(17) 0.0143(18) 0.0125(17) C21 0.0491(17) 0.0448(16) 0.0542(17) -0.0135(14) 0.0102(14) -0.0048(13) C22 0.0414(16) 0.0642(19) 0.0506(17) -0.0120(15) -0.0025(13) 0.0045(14) C23 0.0442(16) 0.0584(18) 0.0427(15) -0.0053(13) -0.0049(12) 0.0060(14) C24 0.0429(15) 0.0498(16) 0.0478(16) -0.0114(13) 0.0103(12) -0.0050(13) C25 0.070(2) 0.0490(17) 0.0500(18) -0.0016(14) 0.0037(16) 0.0077(16) C26 0.064(2) 0.064(2) 0.0420(16) -0.0037(15) -0.0057(14) 0.0093(16) C27 0.0355(14) 0.0534(17) 0.0425(14) -0.0106(13) 0.0020(11) 0.0012(12) C28 0.0434(16) 0.0531(17) 0.0526(17) -0.0119(14) -0.0079(13) 0.0090(13) C29 0.0472(17) 0.0606(19) 0.0534(17) -0.0167(15) -0.0083(14) 0.0048(14) C30 0.0359(14) 0.065(2) 0.0456(17) -0.0160(14) 0.0026(12) -0.0012(14) O9 0.108(3) 0.117(3) 0.246(6) -0.083(4) -0.015(3) 0.007(2) O10 0.152(8) 0.134(7) 0.129(6) -0.019(5) -0.045(6) 0.027(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N3 2.270(2) . ? Cd N1 2.281(2) . ? Cd O4 2.291(2) . ? Cd O7 2.300(2) 2_766 ? Cd O8' 2.38(3) 2_766 ? Cd O3 2.451(5) . ? Cd O3' 2.497(5) . ? Cd O8 2.54(2) 2_766 ? S O6 1.431(3) . ? S O5 1.435(3) . ? S C21 1.766(3) . ? S C24 1.775(3) . ? O1 C6 1.208(4) . ? O2 C14 1.19(2) . ? O3 C17 1.284(5) . ? O2' C14' 1.205(16) . ? O3' C17 1.238(5) . ? O4 C17 1.252(3) . ? O7 C30 1.256(4) . ? O7 Cd 2.300(2) 2_766 ? O8 C30 1.19(3) . ? O8 Cd 2.54(2) 2_766 ? O8' C30 1.31(3) . ? O8' Cd 2.38(3) 2_766 ? N1 C5 1.326(4) . ? N1 C1 1.339(4) . ? N2 C6 1.362(4) . ? N2 C3 1.391(4) . ? N2 H2A 0.8600 . ? N3 C9 1.334(4) . ? N3 C13 1.341(4) . ? N4 C14 1.39(2) . ? N4 C11 1.447(11) . ? N4 H4C 0.8600 . ? N4' C14' 1.384(12) . ? N4' C11 1.405(11) . ? N4' H4'A 0.8600 . ? C1 C2 1.367(4) . ? C1 H1A 0.9300 . ? C2 C3 1.391(4) . ? C2 H2B 0.9300 . ? C3 C4 1.384(4) . ? C4 C5 1.372(4) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.517(5) . ? C7 C8 1.438(9) . ? C7 C8' 1.459(8) . ? C7 H7A 0.9598 . ? C7 H7B 0.9600 . ? C7 H7C 0.9601 . ? C7 H7D 0.9601 . ? C8 H8A 0.9600 . ? C8 H8B 0.9599 . ? C8' H8'A 0.9600 . ? C8' H8'B 0.9600 . ? C9 C10 1.376(4) . ? C9 H9A 0.9300 . ? C10 C11 1.388(6) . ? C10 H10A 0.9300 . ? C11 C12 1.378(6) . ? C12 C13 1.369(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.548(17) . ? C15 C16 1.514(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C16' 1.52(2) 2_477 ? C16 H16A 0.9600 . ? C16 H16B 0.9599 . ? C14' C15' 1.521(18) . ? C15' C16' 1.513(11) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16' H16C 0.9599 . ? C16' H16D 0.9600 . ? C17 C18 1.502(4) . ? C18 C19 1.376(4) . ? C18 C23 1.380(4) . ? C19 C20 1.383(5) . ? C19 H19A 0.9300 . ? C20 C21 1.375(5) . ? C20 H20A 0.9300 . ? C21 C22 1.366(4) . ? C22 C23 1.378(4) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C25 1.370(5) . ? C24 C29 1.379(4) . ? C25 C26 1.378(5) . ? C25 H25A 0.9300 . ? C26 C27 1.386(4) . ? C26 H26A 0.9300 . ? C27 C28 1.385(4) . ? C27 C30 1.502(4) . ? C28 C29 1.381(4) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? O9 H9B 0.8499 . ? O9 H9D 0.9601 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd N1 95.18(8) . . ? N3 Cd O4 138.46(8) . . ? N1 Cd O4 95.04(8) . . ? N3 Cd O7 101.90(8) . 2_766 ? N1 Cd O7 137.54(9) . 2_766 ? O4 Cd O7 97.17(9) . 2_766 ? N3 Cd O8' 135.5(4) . 2_766 ? N1 Cd O8' 84.2(7) . 2_766 ? O4 Cd O8' 85.5(4) . 2_766 ? O7 Cd O8' 56.6(6) 2_766 2_766 ? N3 Cd O3 88.18(12) . . ? N1 Cd O3 129.72(14) . . ? O4 Cd O3 55.16(12) . . ? O7 Cd O3 89.75(14) 2_766 . ? O8' Cd O3 125.7(6) 2_766 . ? N3 Cd O3' 86.38(12) . . ? N1 Cd O3' 117.87(14) . . ? O4 Cd O3' 53.52(12) . . ? O7 Cd O3' 101.89(14) 2_766 . ? O8' Cd O3' 132.9(6) 2_766 . ? N3 Cd O8 127.7(4) . 2_766 ? N1 Cd O8 85.7(6) . 2_766 ? O4 Cd O8 93.1(4) . 2_766 ? O7 Cd O8 53.2(6) 2_766 2_766 ? O3 Cd O8 129.7(6) . 2_766 ? O3' Cd O8 138.3(5) . 2_766 ? O6 S O5 119.94(19) . . ? O6 S C21 108.96(16) . . ? O5 S C21 108.67(17) . . ? O6 S C24 108.12(17) . . ? O5 S C24 108.13(16) . . ? C21 S C24 101.43(14) . . ? C17 O3 Cd 87.8(3) . . ? C17 O3' Cd 86.7(3) . . ? C17 O4 Cd 95.99(17) . . ? C30 O7 Cd 94.59(19) . 2_766 ? C30 O8 Cd 85.0(14) . 2_766 ? C30 O8' Cd 89.3(14) . 2_766 ? C5 N1 C1 116.5(2) . . ? C5 N1 Cd 123.31(18) . . ? C1 N1 Cd 119.31(19) . . ? C6 N2 C3 128.2(3) . . ? C6 N2 H2A 115.9 . . ? C3 N2 H2A 115.9 . . ? C9 N3 C13 116.9(3) . . ? C9 N3 Cd 121.46(19) . . ? C13 N3 Cd 119.9(2) . . ? C14 N4 C11 135.5(9) . . ? C14 N4 H4C 112.2 . . ? C11 N4 H4C 112.2 . . ? C14' N4' C11 117.2(8) . . ? C14' N4' H4'A 121.4 . . ? C11 N4' H4'A 121.4 . . ? N1 C1 C2 123.3(3) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C1 C2 C3 119.4(3) . . ? C1 C2 H2B 120.3 . . ? C3 C2 H2B 120.3 . . ? C4 C3 C2 117.6(3) . . ? C4 C3 N2 125.1(3) . . ? C2 C3 N2 117.3(2) . . ? C5 C4 C3 118.5(3) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N1 C5 C4 124.6(3) . . ? N1 C5 H5A 117.7 . . ? C4 C5 H5A 117.7 . . ? O1 C6 N2 123.3(3) . . ? O1 C6 C7 123.3(3) . . ? N2 C6 C7 113.3(3) . . ? C8 C7 C8' 82.7(5) . . ? C8 C7 C6 119.3(4) . . ? C8' C7 C6 112.1(4) . . ? C8 C7 H7A 107.9 . . ? C8' C7 H7A 126.2 . . ? C6 C7 H7A 107.6 . . ? C8 C7 H7B 106.6 . . ? C6 C7 H7B 107.8 . . ? H7A C7 H7B 107.2 . . ? C8' C7 H7C 108.5 . . ? C6 C7 H7C 109.7 . . ? C8' C7 H7D 109.2 . . ? C6 C7 H7D 109.1 . . ? H7C C7 H7D 108.1 . . ? C7 C8 H8A 107.0 . . ? C7 C8 H8B 105.6 . . ? H8A C8 H8B 106.7 . . ? C7 C8' H8'A 109.2 . . ? C7 C8' H8'B 109.8 . . ? H8'A C8' H8'B 108.5 . . ? N3 C9 C10 123.8(3) . . ? N3 C9 H9A 118.1 . . ? C10 C9 H9A 118.1 . . ? C9 C10 C11 118.7(3) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C12 C11 C10 117.7(3) . . ? C12 C11 N4' 106.9(4) . . ? C10 C11 N4' 135.4(5) . . ? C12 C11 N4 131.9(5) . . ? C10 C11 N4 110.3(5) . . ? N4' C11 N4 25.1(4) . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? N3 C13 C12 122.9(3) . . ? N3 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? O2 C14 N4 123.6(15) . . ? O2 C14 C15 125.4(18) . . ? N4 C14 C15 110.9(12) . . ? C16 C15 C14 110.9(11) . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C16' 110.7(8) . 2_477 ? C15 C16 H16A 110.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.5 . . ? O2' C14' N4' 123.4(13) . . ? O2' C14' C15' 124.7(12) . . ? N4' C14' C15' 111.9(9) . . ? C16' C15' C14' 110.5(8) . . ? C16' C15' H15C 109.6 . . ? C14' C15' H15C 109.6 . . ? C16' C15' H15D 109.6 . . ? C14' C15' H15D 109.6 . . ? H15C C15' H15D 108.1 . . ? C15' C16' H16C 109.3 . . ? C15' C16' H16D 108.7 . . ? H16C C16' H16D 108.1 . . ? O3' C17 O4 120.7(3) . . ? O4 C17 O3 120.3(3) . . ? O3' C17 C18 120.1(3) . . ? O4 C17 C18 117.9(2) . . ? O3 C17 C18 120.1(3) . . ? C19 C18 C23 119.9(3) . . ? C19 C18 C17 120.4(3) . . ? C23 C18 C17 119.7(3) . . ? C18 C19 C20 119.9(3) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C22 C21 C20 121.4(3) . . ? C22 C21 S 119.1(2) . . ? C20 C21 S 119.2(3) . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22A 120.4 . . ? C23 C22 H22A 120.4 . . ? C22 C23 C18 120.4(3) . . ? C22 C23 H23A 119.8 . . ? C18 C23 H23A 119.8 . . ? C25 C24 C29 120.7(3) . . ? C25 C24 S 120.1(2) . . ? C29 C24 S 119.2(3) . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C28 C27 C26 119.0(3) . . ? C28 C27 C30 120.2(3) . . ? C26 C27 C30 120.8(3) . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C24 C29 C28 119.5(3) . . ? C24 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? O8 C30 O7 125.1(12) . . ? O7 C30 O8' 119.5(12) . . ? O8 C30 C27 115.6(12) . . ? O7 C30 C27 118.7(3) . . ? O8' C30 C27 121.2(12) . . ? H9B O9 H9D 109.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.070 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.063 # End of data4 data_5 _database_code_depnum_ccdc_archive 'CCDC 866975' #TrackingRef '- all-2nd-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 Cd N4 O9' _chemical_formula_weight 678.96 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 11.29900(10) _cell_length_b 15.7788(2) _cell_length_c 16.5709(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.1390(10) _cell_angle_gamma 90.00 _cell_volume 2791.04(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9942 _cell_measurement_theta_min 2.303 _cell_measurement_theta_max 28.296 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8851 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _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 'Bruker AXS APEX2' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24807 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6097 _reflns_number_gt 4725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0325P)^2^+1.2125P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6097 _refine_ls_number_parameters 403 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Cd Cd 0.580011(19) 0.447281(12) 0.182768(13) 0.02963(7) Uani 1 1 d D . . N1 N 0.7123(2) 0.53132(14) 0.13321(15) 0.0323(5) Uani 1 1 d . . . N2 N 0.8109(2) 0.54916(15) -0.05382(14) 0.0357(5) Uani 1 1 d . . . H2A H 0.7459 0.5234 -0.0867 0.043 Uiso 1 1 calc R . . N3 N 0.8933(3) 0.40593(16) -0.47603(15) 0.0423(6) Uani 1 1 d . . . H3A H 0.9359 0.3718 -0.4368 0.051 Uiso 1 1 calc R . . N4 N 0.7377(2) 0.38369(14) -0.70866(15) 0.0354(5) Uani 1 1 d . . . O1 O 0.9957(2) 0.60649(14) -0.05035(14) 0.0476(6) Uani 1 1 d . . . O2 O 0.8169(3) 0.53779(15) -0.49854(16) 0.0861(11) Uani 1 1 d . . . O3 O 0.40845(18) 0.54123(12) 0.15396(13) 0.0367(5) Uani 1 1 d . . . O4 O 0.5630(2) 0.56134(13) 0.27278(13) 0.0445(5) Uani 1 1 d . . . O5 O 0.0662(2) 0.85749(13) 0.29064(15) 0.0458(6) Uani 1 1 d . . . O6 O 0.0451(2) 0.74612(13) 0.36703(15) 0.0495(6) Uani 1 1 d . . . O7 O 0.5655(2) 0.36324(15) 0.06959(15) 0.0518(6) Uani 1 1 d D . . C1 C 0.7947(3) 0.58154(19) 0.18926(19) 0.0365(7) Uani 1 1 d . . . H1A H 0.7886 0.5886 0.2435 0.044 Uiso 1 1 calc R . . C2 C 0.8880(3) 0.62302(18) 0.16891(18) 0.0392(7) Uani 1 1 d . . . H2B H 0.9437 0.6577 0.2091 0.047 Uiso 1 1 calc R . . C3 C 0.8993(3) 0.61340(18) 0.08944(18) 0.0369(7) Uani 1 1 d . . . H3B H 0.9631 0.6405 0.0755 0.044 Uiso 1 1 calc R . . C4 C 0.8136(3) 0.56253(16) 0.03038(17) 0.0298(6) Uani 1 1 d . . . C5 C 0.7216(3) 0.52316(17) 0.05541(17) 0.0312(6) Uani 1 1 d . . . H5A H 0.6633 0.4893 0.0159 0.037 Uiso 1 1 calc R . . C6 C 0.8980(3) 0.57177(17) -0.08985(19) 0.0331(6) Uani 1 1 d . . . C7 C 0.8611(3) 0.54854(19) -0.18322(18) 0.0389(7) Uani 1 1 d . . . H7A H 0.7727 0.5606 -0.2103 0.047 Uiso 1 1 calc R . . H7B H 0.8730 0.4881 -0.1880 0.047 Uiso 1 1 calc R . . C8 C 0.9346(3) 0.5952(2) -0.2309(2) 0.0438(8) Uani 1 1 d . . . H8A H 1.0213 0.5769 -0.2095 0.053 Uiso 1 1 calc R . . H8B H 0.9326 0.6554 -0.2197 0.053 Uiso 1 1 calc R . . C9 C 0.8833(4) 0.5801(2) -0.3267(2) 0.0490(8) Uani 1 1 d . . . H9A H 0.7936 0.5897 -0.3461 0.059 Uiso 1 1 calc R . . H9B H 0.9202 0.6214 -0.3548 0.059 Uiso 1 1 calc R . . C10 C 0.9080(3) 0.4930(2) -0.35393(19) 0.0479(8) Uani 1 1 d . . . H10A H 0.8645 0.4519 -0.3303 0.057 Uiso 1 1 calc R . . H10B H 0.9970 0.4812 -0.3302 0.057 Uiso 1 1 calc R . . C11 C 0.8671(3) 0.4816(2) -0.4497(2) 0.0433(7) Uani 1 1 d . . . C12 C 0.8592(3) 0.37573(18) -0.56049(18) 0.0369(7) Uani 1 1 d . . . C13 C 0.9113(3) 0.3005(2) -0.5755(2) 0.0487(8) Uani 1 1 d . . . H13A H 0.9708 0.2725 -0.5311 0.058 Uiso 1 1 calc R . . C14 C 0.8742(4) 0.2676(2) -0.6570(2) 0.0543(9) Uani 1 1 d . . . H14A H 0.9072 0.2165 -0.6679 0.065 Uiso 1 1 calc R . . C15 C 0.7885(3) 0.3105(2) -0.7218(2) 0.0467(8) Uani 1 1 d . . . H15A H 0.7647 0.2882 -0.7768 0.056 Uiso 1 1 calc R . . C16 C 0.7726(3) 0.41534(19) -0.62897(19) 0.0375(7) Uani 1 1 d . . . H16A H 0.7369 0.4659 -0.6196 0.045 Uiso 1 1 calc R . . C17 C 0.4530(3) 0.57596(17) 0.22613(18) 0.0309(6) Uani 1 1 d . . . C18 C 0.3708(3) 0.63509(16) 0.25555(18) 0.0301(6) Uani 1 1 d . . . C19 C 0.2790(3) 0.67860(18) 0.19435(19) 0.0368(7) Uani 1 1 d . . . H19A H 0.2729 0.6732 0.1372 0.044 Uiso 1 1 calc R . . C20 C 0.1941(3) 0.73121(18) 0.21666(19) 0.0367(7) Uani 1 1 d . . . H20A H 0.1327 0.7603 0.1743 0.044 Uiso 1 1 calc R . . C21 C 0.2014(2) 0.73982(16) 0.30085(18) 0.0306(6) Uani 1 1 d . . . C22 C 0.0966(3) 0.78573(18) 0.32159(19) 0.0340(6) Uani 1 1 d . . . C23 C 0.2991(3) 0.70008(16) 0.36615(17) 0.0296(6) Uani 1 1 d . . . C24 C 0.3173(3) 0.7137(2) 0.4540(2) 0.0436(7) Uani 1 1 d . . . H24A H 0.2639 0.7507 0.4690 0.052 Uiso 1 1 calc R . . C25 C 0.4099(3) 0.6747(2) 0.5171(2) 0.0494(8) Uani 1 1 d . . . H25A H 0.4204 0.6861 0.5740 0.059 Uiso 1 1 calc R . . C26 C 0.4890(3) 0.6177(2) 0.4958(2) 0.0537(9) Uani 1 1 d . . . H26A H 0.5506 0.5895 0.5387 0.064 Uiso 1 1 calc R . . C27 C 0.4764(3) 0.6030(2) 0.4117(2) 0.0477(8) Uani 1 1 d . . . H27A H 0.5293 0.5641 0.3988 0.057 Uiso 1 1 calc R . . C28 C 0.3846(3) 0.64567(16) 0.34371(18) 0.0314(6) Uani 1 1 d . . . O8 O 0.7497(3) 0.16580(17) 0.1170(2) 0.0656(7) Uani 1 1 d D . . O9 O 0.7754(3) 0.3165(2) 0.0386(2) 0.0786(9) Uani 1 1 d D . . H7C H 0.6375(13) 0.349(2) 0.0695(17) 0.088(15) Uiso 1 1 d D . . H7D H 0.538(4) 0.3148(10) 0.0789(16) 0.096(16) Uiso 1 1 d D . . H8C H 0.718(4) 0.133(2) 0.0747(18) 0.083(15) Uiso 1 1 d D . . H8D H 0.817(3) 0.142(3) 0.149(3) 0.12(2) Uiso 1 1 d D . . H9C H 0.843(3) 0.344(3) 0.059(4) 0.15(3) Uiso 1 1 d D . . H9D H 0.784(5) 0.2655(13) 0.057(3) 0.11(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.03010(11) 0.03016(11) 0.03243(11) -0.00674(9) 0.01543(8) -0.00358(9) N1 0.0327(13) 0.0360(13) 0.0298(13) -0.0005(10) 0.0125(11) -0.0026(10) N2 0.0318(13) 0.0485(14) 0.0275(12) -0.0039(11) 0.0105(10) -0.0115(11) N3 0.0532(17) 0.0431(15) 0.0288(14) 0.0054(11) 0.0110(13) 0.0095(13) N4 0.0410(15) 0.0349(13) 0.0314(13) -0.0020(10) 0.0132(11) -0.0027(11) O1 0.0381(13) 0.0646(15) 0.0436(13) -0.0089(11) 0.0180(11) -0.0166(11) O2 0.158(3) 0.0419(15) 0.0357(14) 0.0006(11) 0.0006(16) 0.0250(16) O3 0.0332(11) 0.0393(12) 0.0385(12) -0.0123(9) 0.0132(9) -0.0013(9) O4 0.0357(12) 0.0544(14) 0.0419(12) -0.0143(10) 0.0104(10) 0.0108(10) O5 0.0430(13) 0.0360(12) 0.0667(15) 0.0099(10) 0.0292(12) 0.0123(10) O6 0.0502(14) 0.0419(12) 0.0712(16) 0.0137(11) 0.0399(13) 0.0125(10) O7 0.0603(17) 0.0511(15) 0.0558(15) -0.0232(11) 0.0350(13) -0.0250(12) C1 0.0391(17) 0.0427(16) 0.0284(15) -0.0018(12) 0.0118(14) -0.0032(13) C2 0.0404(18) 0.0422(17) 0.0316(16) -0.0076(13) 0.0072(14) -0.0138(13) C3 0.0334(16) 0.0411(17) 0.0365(17) 0.0021(13) 0.0119(14) -0.0114(13) C4 0.0312(14) 0.0326(15) 0.0256(14) 0.0020(11) 0.0090(12) -0.0015(11) C5 0.0297(15) 0.0335(14) 0.0295(15) -0.0021(11) 0.0085(12) -0.0069(11) C6 0.0294(15) 0.0368(16) 0.0354(16) 0.0017(12) 0.0137(13) 0.0009(12) C7 0.0360(16) 0.0482(18) 0.0353(16) -0.0029(13) 0.0155(13) -0.0023(14) C8 0.053(2) 0.0450(18) 0.0389(18) -0.0026(14) 0.0232(16) -0.0079(15) C9 0.068(2) 0.0446(18) 0.0407(19) 0.0020(14) 0.0260(18) -0.0002(16) C10 0.060(2) 0.0476(19) 0.0316(17) 0.0002(14) 0.0092(16) 0.0025(16) C11 0.055(2) 0.0395(17) 0.0325(17) 0.0032(14) 0.0108(15) 0.0006(15) C12 0.0448(18) 0.0366(16) 0.0331(16) 0.0034(12) 0.0176(14) -0.0002(13) C13 0.060(2) 0.0442(19) 0.0428(19) 0.0083(14) 0.0187(17) 0.0154(16) C14 0.071(3) 0.0402(19) 0.056(2) -0.0022(16) 0.027(2) 0.0139(17) C15 0.058(2) 0.0442(19) 0.0404(18) -0.0094(14) 0.0188(17) 0.0007(16) C16 0.0459(18) 0.0348(15) 0.0349(17) 0.0007(12) 0.0177(15) 0.0036(13) C17 0.0305(15) 0.0290(14) 0.0371(16) -0.0036(11) 0.0161(13) -0.0019(11) C18 0.0291(15) 0.0289(14) 0.0355(16) -0.0052(11) 0.0149(13) -0.0015(11) C19 0.0378(17) 0.0400(17) 0.0351(16) -0.0049(12) 0.0155(14) -0.0019(13) C20 0.0312(16) 0.0403(17) 0.0382(17) 0.0043(13) 0.0108(13) 0.0045(13) C21 0.0272(14) 0.0261(14) 0.0413(16) -0.0031(11) 0.0150(13) -0.0016(11) C22 0.0284(15) 0.0333(16) 0.0409(17) -0.0022(12) 0.0121(13) 0.0027(12) C23 0.0299(15) 0.0276(14) 0.0350(16) -0.0040(11) 0.0156(13) -0.0032(11) C24 0.0427(19) 0.0470(18) 0.0465(19) -0.0091(14) 0.0220(16) -0.0028(14) C25 0.050(2) 0.063(2) 0.0370(18) -0.0034(16) 0.0158(17) -0.0009(17) C26 0.048(2) 0.069(2) 0.042(2) 0.0108(17) 0.0115(17) 0.0096(18) C27 0.049(2) 0.054(2) 0.044(2) 0.0059(15) 0.0197(17) 0.0138(16) C28 0.0295(15) 0.0284(14) 0.0388(16) -0.0023(11) 0.0145(13) -0.0018(11) O8 0.082(2) 0.0494(16) 0.0594(18) -0.0063(14) 0.0153(17) 0.0091(15) O9 0.060(2) 0.067(2) 0.117(3) 0.0152(19) 0.040(2) -0.0018(16) _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 Cd O7 2.259(2) . ? Cd N4 2.306(2) 1_556 ? Cd O5 2.3252(19) 2_545 ? Cd N1 2.339(2) . ? Cd O3 2.3614(19) . ? Cd O4 2.3852(19) . ? Cd C17 2.716(3) . ? N1 C5 1.334(3) . ? N1 C1 1.338(4) . ? N2 C6 1.355(3) . ? N2 C4 1.402(3) . ? N2 H2A 0.8600 . ? N3 C11 1.337(4) . ? N3 C12 1.407(4) . ? N3 H3A 0.8600 . ? N4 C15 1.338(4) . ? N4 C16 1.344(4) . ? N4 Cd 2.306(2) 1_554 ? O1 C6 1.214(3) . ? O2 C11 1.209(4) . ? O3 C17 1.261(3) . ? O4 C17 1.251(3) . ? O5 C22 1.244(3) . ? O5 Cd 2.3252(19) 2 ? O6 C22 1.258(3) . ? O7 H7C 0.843(10) . ? O7 H7D 0.858(10) . ? C1 C2 1.373(4) . ? C1 H1A 0.9300 . ? C2 C3 1.373(4) . ? C2 H2B 0.9300 . ? C3 C4 1.385(4) . ? C3 H3B 0.9300 . ? C4 C5 1.386(4) . ? C5 H5A 0.9300 . ? C6 C7 1.510(4) . ? C7 C8 1.511(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.521(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.502(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.511(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 C16 1.381(4) . ? C12 C13 1.383(4) . ? C13 C14 1.378(5) . ? C13 H13A 0.9300 . ? C14 C15 1.367(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.505(3) . ? C18 C19 1.374(4) . ? C18 C28 1.427(4) . ? C19 C20 1.407(4) . ? C19 H19A 0.9300 . ? C20 C21 1.377(4) . ? C20 H20A 0.9300 . ? C21 C23 1.414(4) . ? C21 C22 1.521(3) . ? C23 C24 1.418(4) . ? C23 C28 1.429(3) . ? C24 C25 1.359(5) . ? C24 H24A 0.9300 . ? C25 C26 1.392(4) . ? C25 H25A 0.9300 . ? C26 C27 1.373(4) . ? C26 H26A 0.9300 . ? C27 C28 1.426(4) . ? C27 H27A 0.9300 . ? O8 H8C 0.850(10) . ? O8 H8D 0.857(10) . ? O9 H9C 0.851(10) . ? O9 H9D 0.855(10) . ? 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 O7 Cd N4 102.68(9) . 1_556 ? O7 Cd O5 86.39(8) . 2_545 ? N4 Cd O5 90.13(8) 1_556 2_545 ? O7 Cd N1 85.53(8) . . ? N4 Cd N1 95.81(8) 1_556 . ? O5 Cd N1 170.85(8) 2_545 . ? O7 Cd O3 111.68(9) . . ? N4 Cd O3 143.53(7) 1_556 . ? O5 Cd O3 80.43(7) 2_545 . ? N1 Cd O3 98.61(7) . . ? O7 Cd O4 164.48(9) . . ? N4 Cd O4 92.33(8) 1_556 . ? O5 Cd O4 97.66(7) 2_545 . ? N1 Cd O4 89.07(8) . . ? O3 Cd O4 54.80(7) . . ? O7 Cd C17 139.28(10) . . ? N4 Cd C17 117.34(8) 1_556 . ? O5 Cd C17 86.30(7) 2_545 . ? N1 Cd C17 97.07(8) . . ? O3 Cd C17 27.64(8) . . ? O4 Cd C17 27.43(8) . . ? C5 N1 C1 118.1(2) . . ? C5 N1 Cd 123.13(18) . . ? C1 N1 Cd 118.12(17) . . ? C6 N2 C4 128.1(2) . . ? C6 N2 H2A 115.9 . . ? C4 N2 H2A 115.9 . . ? C11 N3 C12 127.5(3) . . ? C11 N3 H3A 116.2 . . ? C12 N3 H3A 116.2 . . ? C15 N4 C16 118.5(3) . . ? C15 N4 Cd 120.7(2) . 1_554 ? C16 N4 Cd 120.48(19) . 1_554 ? C17 O3 Cd 92.03(17) . . ? C17 O4 Cd 91.17(16) . . ? C22 O5 Cd 126.43(18) . 2 ? Cd O7 H7C 110.2(10) . . ? Cd O7 H7D 107.8(10) . . ? H7C O7 H7D 100(4) . . ? N1 C1 C2 121.8(3) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2B 119.9 . . ? C1 C2 H2B 119.9 . . ? C2 C3 C4 118.6(2) . . ? C2 C3 H3B 120.7 . . ? C4 C3 H3B 120.7 . . ? C3 C4 C5 117.9(2) . . ? C3 C4 N2 124.9(2) . . ? C5 C4 N2 117.2(2) . . ? N1 C5 C4 123.4(3) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? O1 C6 N2 123.0(3) . . ? O1 C6 C7 124.0(2) . . ? N2 C6 C7 113.0(2) . . ? C6 C7 C8 113.7(2) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C9 112.6(3) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C8 114.3(3) . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C9 C10 C11 113.6(3) . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? O2 C11 N3 122.8(3) . . ? O2 C11 C10 122.1(3) . . ? N3 C11 C10 115.1(3) . . ? C16 C12 C13 118.0(3) . . ? C16 C12 N3 123.6(3) . . ? C13 C12 N3 118.4(3) . . ? C14 C13 C12 119.3(3) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? N4 C15 C14 122.1(3) . . ? N4 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? N4 C16 C12 122.6(3) . . ? N4 C16 H16A 118.7 . . ? C12 C16 H16A 118.7 . . ? O4 C17 O3 120.8(2) . . ? O4 C17 C18 120.5(2) . . ? O3 C17 C18 118.7(3) . . ? O4 C17 Cd 61.41(14) . . ? O3 C17 Cd 60.33(14) . . ? C18 C17 Cd 169.90(18) . . ? C19 C18 C28 120.0(2) . . ? C19 C18 C17 117.9(2) . . ? C28 C18 C17 122.2(3) . . ? C18 C19 C20 121.1(3) . . ? C18 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C23 120.3(2) . . ? C20 C21 C22 118.9(3) . . ? C23 C21 C22 120.6(2) . . ? O5 C22 O6 125.4(2) . . ? O5 C22 C21 118.1(2) . . ? O6 C22 C21 116.5(2) . . ? C21 C23 C24 122.2(2) . . ? C21 C23 C28 119.5(2) . . ? C24 C23 C28 118.4(3) . . ? C25 C24 C23 122.5(3) . . ? C25 C24 H24A 118.8 . . ? C23 C24 H24A 118.8 . . ? C24 C25 C26 119.6(3) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C26 C27 C28 121.9(3) . . ? C26 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 . . ? C27 C28 C18 124.1(2) . . ? C27 C28 C23 117.1(3) . . ? C18 C28 C23 118.7(3) . . ? H8C O8 H8D 107(4) . . ? H9C O9 H9D 112(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.694 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.068 # End of data5 and End of all