# 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_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Jianhua Lin' _publ_contact_author_address ; Department of Chemistry College of Chemistry and Chemical Engineering Chongqing University Chongqing, 400044 P. R. China ; #======================================================================== _publ_contact_author_email jhlin@cqu.edu.cn _publ_contact_author_fax +86-023-65102348 _publ_contact_author_phone +86-023-65102348 _publ_contact_letter ; Dear Sir, Please consider this CIF submission for publication in CrystEngComm. All authors have seen and approved this submission. Best wishes Jianhua Lin ; loop_ _publ_author_name 'Yun Gong' 'Tao Wu' 'Jian Lin' #===END data_0922 _database_code_depnum_ccdc_archive 'CCDC 800774' #TrackingRef '- 0923.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H17 Mn N O7' _chemical_formula_weight 402.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.8267(3) _cell_length_b 28.9972(8) _cell_length_c 9.5316(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.186(2) _cell_angle_gamma 90.00 _cell_volume 3542.59(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4706 _cell_measurement_theta_min 2.5534 _cell_measurement_theta_max 28.7414 _exptl_crystal_description Block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68443 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford XCaliburE' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7408 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3131 _reflns_number_gt 2459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0723P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3131 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1042 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 Mn1 Mn 1.0000 0.5000 0.5000 0.02142(16) Uani 1 2 d S . . Mn2 Mn 1.0000 0.406197(17) 0.2500 0.02586(17) Uani 1 2 d S . . O1 O 0.95620(15) 0.56311(6) 0.40781(18) 0.0396(5) Uani 1 1 d . . . O3 O 0.86120(13) 0.50201(6) 0.62811(17) 0.0291(4) Uani 1 1 d . . . O4 O 0.66728(13) 0.48167(7) 0.71805(18) 0.0377(5) Uani 1 1 d . . . C14 C 0.7409(2) 0.50272(10) 0.8131(3) 0.0357(7) Uani 1 1 d . . . H14A H 0.7541 0.4821 0.8920 0.043 Uiso 1 1 calc R . . H14B H 0.7107 0.5308 0.8492 0.043 Uiso 1 1 calc R . . O5 O 0.90594(12) 0.46287(6) 0.33097(15) 0.0249(4) Uani 1 1 d . . . O7 O 1.11008(14) 0.39393(6) 0.42265(18) 0.0361(4) Uani 1 1 d . . . O2 O 0.77637(18) 0.65682(7) 0.3762(2) 0.0557(6) Uani 1 1 d . . . O6 O 0.89842(17) 0.35642(7) 0.3587(2) 0.0522(6) Uani 1 1 d . . . C8 C 0.61125(18) 0.50975(9) 0.6290(3) 0.0295(6) Uani 1 1 d . . . C7 C 0.9020(2) 0.59523(8) 0.4518(3) 0.0332(6) Uani 1 1 d . . . C11 C 0.53120(18) 0.48682(9) 0.5479(3) 0.0281(6) Uani 1 1 d . . . C13 C 0.84414(17) 0.51448(8) 0.7488(2) 0.0230(5) Uani 1 1 d . . . C9 C 0.6284(2) 0.55586(10) 0.6117(3) 0.0379(7) Uani 1 1 d . . . H9 H 0.6817 0.5705 0.6634 0.045 Uiso 1 1 calc R . . C12 C 0.5126(2) 0.43927(10) 0.5622(3) 0.0386(6) Uani 1 1 d . . . H12 H 0.5534 0.4218 0.6248 0.046 Uiso 1 1 calc R . . C10 C 0.5660(2) 0.58098(10) 0.5168(3) 0.0454(7) Uani 1 1 d . . . H10 H 0.5781 0.6124 0.5067 0.055 Uiso 1 1 calc R . . C2 C 0.7349(2) 0.72963(9) 0.4658(3) 0.0420(7) Uani 1 1 d . . . C6 C 0.8474(3) 0.62237(11) 0.3364(3) 0.0567(9) Uani 1 1 d . . . H6A H 0.9003 0.6370 0.2814 0.068 Uiso 1 1 calc R . . H6B H 0.8101 0.6008 0.2752 0.068 Uiso 1 1 calc R . . C1 C 0.8141(2) 0.69633(10) 0.4368(3) 0.0436(7) Uani 1 1 d . . . C5 C 0.9161(2) 0.70481(10) 0.4728(4) 0.0534(9) Uani 1 1 d . . . H5 H 0.9673 0.6835 0.4510 0.064 Uiso 1 1 calc R . . C15 C 0.8156(3) 0.34069(12) 0.3108(4) 0.0603(9) Uani 1 1 d . . . H15 H 0.8100 0.3371 0.2138 0.072 Uiso 1 1 calc R . . C3 C 0.6285(2) 0.72171(10) 0.4255(4) 0.0537(8) Uani 1 1 d . . . H3 H 0.6086 0.6948 0.3785 0.064 Uiso 1 1 calc R . . C4 C 0.5565(2) 0.75398(11) 0.4568(4) 0.0594(9) Uani 1 1 d . . . H4 H 0.4868 0.7487 0.4310 0.071 Uiso 1 1 calc R . . N1 N 0.7357(2) 0.32866(14) 0.3796(3) 0.0814(11) Uani 1 1 d . . . C17 C 0.6388(4) 0.3129(2) 0.3153(5) 0.141(3) Uani 1 1 d . . . H17A H 0.5907 0.3059 0.3870 0.211 Uiso 1 1 calc R . . H17B H 0.6511 0.2858 0.2608 0.211 Uiso 1 1 calc R . . H17C H 0.6100 0.3367 0.2553 0.211 Uiso 1 1 calc R . . C16 C 0.7368(6) 0.3356(5) 0.5254(6) 0.289(8) Uani 1 1 d . . . H16A H 0.6722 0.3249 0.5615 0.434 Uiso 1 1 calc R . . H16B H 0.7451 0.3678 0.5455 0.434 Uiso 1 1 calc R . . H16C H 0.7937 0.3187 0.5689 0.434 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0176(3) 0.0268(3) 0.0194(3) -0.0026(2) -0.0048(2) 0.0048(2) Mn2 0.0254(3) 0.0261(3) 0.0259(3) 0.000 -0.0021(2) 0.000 O1 0.0504(12) 0.0358(10) 0.0325(10) 0.0035(8) 0.0003(9) 0.0184(9) O3 0.0203(9) 0.0447(11) 0.0223(10) -0.0054(7) 0.0000(7) -0.0002(7) O4 0.0202(9) 0.0543(12) 0.0380(11) 0.0034(9) -0.0086(8) -0.0103(9) C14 0.0197(13) 0.0618(18) 0.0252(14) -0.0012(12) -0.0028(11) -0.0093(12) O5 0.0208(8) 0.0331(9) 0.0203(8) -0.0026(7) -0.0058(7) 0.0040(7) O7 0.0438(11) 0.0359(10) 0.0280(10) -0.0005(8) -0.0059(8) 0.0080(9) O2 0.0596(15) 0.0394(12) 0.0665(14) 0.0012(10) -0.0178(11) 0.0223(11) O6 0.0477(13) 0.0554(13) 0.0528(13) 0.0186(10) -0.0093(10) -0.0163(11) C8 0.0152(12) 0.0484(16) 0.0248(14) -0.0008(11) -0.0013(10) -0.0028(11) C7 0.0367(15) 0.0303(14) 0.0321(15) 0.0038(11) -0.0074(12) 0.0041(12) C11 0.0160(12) 0.0424(15) 0.0260(13) -0.0031(10) 0.0010(10) -0.0042(10) C13 0.0155(11) 0.0299(13) 0.0231(13) 0.0062(10) -0.0040(10) 0.0009(10) C9 0.0261(14) 0.0475(17) 0.0393(16) -0.0082(13) -0.0086(12) -0.0107(12) C12 0.0285(15) 0.0435(16) 0.0431(16) 0.0022(13) -0.0064(12) -0.0016(12) C10 0.0389(17) 0.0367(16) 0.060(2) -0.0019(14) -0.0101(14) -0.0101(13) C2 0.0386(16) 0.0344(14) 0.0528(18) 0.0176(13) -0.0025(13) 0.0092(13) C6 0.080(2) 0.0500(19) 0.0393(17) 0.0004(14) -0.0152(16) 0.0306(18) C1 0.0448(18) 0.0371(16) 0.0484(18) 0.0141(13) -0.0054(14) 0.0134(14) C5 0.0412(18) 0.0411(18) 0.078(2) 0.0191(16) 0.0094(16) 0.0167(15) C15 0.065(2) 0.070(2) 0.0462(19) 0.0056(17) 0.0008(17) -0.0224(19) C3 0.0443(19) 0.0375(17) 0.078(2) 0.0149(15) -0.0105(16) 0.0038(15) C4 0.0331(17) 0.0439(19) 0.101(3) 0.0223(18) -0.0038(17) 0.0038(14) N1 0.0480(18) 0.152(3) 0.0445(18) -0.0071(19) 0.0073(14) -0.027(2) C17 0.077(3) 0.263(8) 0.082(3) -0.004(4) 0.001(3) -0.078(4) C16 0.126(6) 0.67(2) 0.074(4) -0.085(8) 0.019(4) -0.143(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.0975(17) . ? Mn1 O1 2.0975(17) 5_766 ? Mn1 O3 2.1976(16) 5_766 ? Mn1 O3 2.1976(16) . ? Mn1 O5 2.2500(15) 5_766 ? Mn1 O5 2.2500(15) . ? Mn2 O7 2.1566(17) 2_755 ? Mn2 O7 2.1566(17) . ? Mn2 O5 2.1960(16) 2_755 ? Mn2 O5 2.1960(16) . ? Mn2 O6 2.227(2) . ? Mn2 O6 2.227(2) 2_755 ? O1 C7 1.245(3) . ? O3 C13 1.234(3) . ? O4 C8 1.361(3) . ? O4 C14 1.421(3) . ? C14 C13 1.519(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? O5 C13 1.275(3) 6_565 ? O7 C7 1.252(3) 5_766 ? O2 C1 1.363(4) . ? O2 C6 1.414(4) . ? O6 C15 1.228(4) . ? C8 C9 1.366(4) . ? C8 C11 1.426(3) . ? C7 O7 1.252(3) 5_766 ? C7 C6 1.503(4) . ? C11 C12 1.407(4) . ? C11 C11 1.415(5) 5_666 ? C13 O5 1.275(3) 6_566 ? C9 C10 1.390(4) . ? C9 H9 0.9300 . ? C12 C10 1.367(4) 5_666 ? C12 H12 0.9300 . ? C10 C12 1.367(4) 5_666 ? C10 H10 0.9300 . ? C2 C2 1.396(6) 7_666 ? C2 C3 1.423(4) . ? C2 C1 1.436(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C1 C5 1.362(4) . ? C5 C4 1.409(5) 7_666 ? C5 H5 0.9300 . ? C15 N1 1.286(4) . ? C15 H15 0.9300 . ? C3 C4 1.356(4) . ? C3 H3 0.9300 . ? C4 C5 1.409(5) 7_666 ? C4 H4 0.9300 . ? N1 C16 1.403(6) . ? N1 C17 1.439(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 O1 Mn1 O1 180.00(5) . 5_766 ? O1 Mn1 O3 90.00(7) . 5_766 ? O1 Mn1 O3 90.00(7) 5_766 5_766 ? O1 Mn1 O3 90.00(7) . . ? O1 Mn1 O3 90.00(7) 5_766 . ? O3 Mn1 O3 180.0 5_766 . ? O1 Mn1 O5 90.58(6) . 5_766 ? O1 Mn1 O5 89.42(7) 5_766 5_766 ? O3 Mn1 O5 89.25(6) 5_766 5_766 ? O3 Mn1 O5 90.75(6) . 5_766 ? O1 Mn1 O5 89.42(7) . . ? O1 Mn1 O5 90.58(7) 5_766 . ? O3 Mn1 O5 90.75(6) 5_766 . ? O3 Mn1 O5 89.25(6) . . ? O5 Mn1 O5 180.00(7) 5_766 . ? O7 Mn2 O7 161.02(10) 2_755 . ? O7 Mn2 O5 101.99(6) 2_755 2_755 ? O7 Mn2 O5 92.24(6) . 2_755 ? O7 Mn2 O5 92.24(6) 2_755 . ? O7 Mn2 O5 101.99(6) . . ? O5 Mn2 O5 83.11(8) 2_755 . ? O7 Mn2 O6 82.56(7) 2_755 . ? O7 Mn2 O6 85.16(7) . . ? O5 Mn2 O6 171.01(7) 2_755 . ? O5 Mn2 O6 89.00(7) . . ? O7 Mn2 O6 85.16(7) 2_755 2_755 ? O7 Mn2 O6 82.56(7) . 2_755 ? O5 Mn2 O6 89.00(7) 2_755 2_755 ? O5 Mn2 O6 171.01(7) . 2_755 ? O6 Mn2 O6 99.18(12) . 2_755 ? C7 O1 Mn1 130.98(16) . . ? C13 O3 Mn1 134.61(16) . . ? C8 O4 C14 117.6(2) . . ? O4 C14 C13 114.0(2) . . ? O4 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? O4 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C13 O5 Mn2 120.46(14) 6_565 . ? C13 O5 Mn1 119.79(14) 6_565 . ? Mn2 O5 Mn1 108.84(6) . . ? C7 O7 Mn2 125.91(17) 5_766 . ? C1 O2 C6 119.0(3) . . ? C15 O6 Mn2 125.5(2) . . ? O4 C8 C9 125.3(2) . . ? O4 C8 C11 114.3(2) . . ? C9 C8 C11 120.4(2) . . ? O1 C7 O7 126.9(2) . 5_766 ? O1 C7 C6 113.3(2) . . ? O7 C7 C6 119.8(2) 5_766 . ? C12 C11 C11 119.9(3) . 5_666 ? C12 C11 C8 121.7(2) . . ? C11 C11 C8 118.4(3) 5_666 . ? O3 C13 O5 126.5(2) . 6_566 ? O3 C13 C14 119.9(2) . . ? O5 C13 C14 113.5(2) 6_566 . ? C8 C9 C10 120.0(3) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C10 C12 C11 119.5(3) 5_666 . ? C10 C12 H12 120.3 5_666 . ? C11 C12 H12 120.3 . . ? C12 C10 C9 121.8(3) 5_666 . ? C12 C10 H10 119.1 5_666 . ? C9 C10 H10 119.1 . . ? C2 C2 C3 120.5(3) 7_666 . ? C2 C2 C1 118.3(3) 7_666 . ? C3 C2 C1 121.2(3) . . ? O2 C6 C7 117.4(2) . . ? O2 C6 H6A 108.0 . . ? C7 C6 H6A 108.0 . . ? O2 C6 H6B 108.0 . . ? C7 C6 H6B 108.0 . . ? H6A C6 H6B 107.2 . . ? C5 C1 O2 125.5(3) . . ? C5 C1 C2 120.6(3) . . ? O2 C1 C2 113.9(3) . . ? C1 C5 C4 119.5(3) . 7_666 ? C1 C5 H5 120.2 . . ? C4 C5 H5 120.2 7_666 . ? O6 C15 N1 127.3(3) . . ? O6 C15 H15 116.4 . . ? N1 C15 H15 116.4 . . ? C4 C3 C2 118.9(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 122.0(3) . 7_666 ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 7_666 . ? C15 N1 C16 119.3(4) . . ? C15 N1 C17 124.1(3) . . ? C16 N1 C17 116.3(4) . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.515 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.075 #======================================================================= data_0923 _database_code_depnum_ccdc_archive 'CCDC 800775' #TrackingRef '- 0923.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Cd O8' _chemical_formula_weight 418.62 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' 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 11.6576(3) _cell_length_b 7.97420(10) _cell_length_c 15.6452(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.303(2) _cell_angle_gamma 90.00 _cell_volume 1420.98(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4720 _cell_measurement_theta_min 2.5490 _cell_measurement_theta_max 28.7894 _exptl_crystal_description cubic _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92630 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6193 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2513 _reflns_number_gt 2182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0447P)^2^+0.7718P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2513 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.48713(2) 0.46566(3) 0.802829(17) 0.01944(12) Uani 1 1 d . . . O2 O 0.6181(2) 0.4693(3) 0.96157(19) 0.0295(6) Uani 1 1 d . . . O3 O 0.8722(2) 0.6967(3) 0.93723(17) 0.0272(6) Uani 1 1 d . . . O6 O 1.5107(2) 1.1835(3) 0.81381(16) 0.0212(6) Uani 1 1 d . . . O1 O 0.6675(2) 0.5879(4) 0.84729(17) 0.0295(6) Uani 1 1 d . . . O7 O 0.3004(2) 0.3771(3) 0.73086(18) 0.0316(7) Uani 1 1 d . . . O8 O 0.3727(2) 0.6228(3) 0.87038(18) 0.0284(6) Uani 1 1 d . . . C14 C 0.6888(3) 0.5515(4) 0.9270(3) 0.0218(8) Uani 1 1 d . . . C13 C 0.8033(3) 0.6043(5) 0.9859(2) 0.0215(8) Uani 1 1 d . . . H13B H 0.7874 0.6731 1.0332 0.026 Uiso 1 1 calc R . . H13A H 0.8463 0.5058 1.0113 0.026 Uiso 1 1 calc R . . C3 C 1.0247(3) 0.7200(5) 1.0690(2) 0.0239(8) Uani 1 1 d . . . H3 H 0.9788 0.6663 1.1025 0.029 Uiso 1 1 calc R . . C5 C 1.0489(3) 0.8330(4) 0.9293(2) 0.0195(8) Uani 1 1 d . . . C10 C 1.0059(3) 0.8685(5) 0.8402(3) 0.0248(8) Uani 1 1 d . . . H10 H 0.9324 0.8292 0.8121 0.030 Uiso 1 1 calc R . . C2 C 1.1390(3) 0.7729(5) 1.1078(2) 0.0250(8) Uani 1 1 d . . . H2 H 1.1683 0.7530 1.1670 0.030 Uiso 1 1 calc R . . C4 C 0.9812(3) 0.7479(4) 0.9815(2) 0.0205(8) Uani 1 1 d . . . O4 O 1.3409(2) 1.0222(3) 0.96445(18) 0.0264(6) Uani 1 1 d . . . O5 O 1.4539(2) 0.9253(3) 0.83324(18) 0.0280(6) Uani 1 1 d . . . C7 C 1.2301(3) 0.9780(4) 0.9196(3) 0.0212(8) Uani 1 1 d . . . C8 C 1.1845(4) 1.0165(5) 0.8340(3) 0.0270(9) Uani 1 1 d . . . H8 H 1.2279 1.0793 0.8020 0.032 Uiso 1 1 calc R . . C9 C 1.0712(3) 0.9600(5) 0.7949(3) 0.0272(9) Uani 1 1 d . . . H9 H 1.0402 0.9860 0.7365 0.033 Uiso 1 1 calc R . . C12 C 1.4600(3) 1.0774(4) 0.8537(2) 0.0178(7) Uani 1 1 d . . . C11 C 1.4046(3) 1.1434(5) 0.9262(2) 0.0236(8) Uani 1 1 d . . . H11A H 1.4660 1.1896 0.9719 0.028 Uiso 1 1 calc R . . H11B H 1.3517 1.2343 0.9031 0.028 Uiso 1 1 calc R . . C1 C 1.2070(3) 0.8523(5) 1.0603(2) 0.0235(8) Uani 1 1 d . . . H1 H 1.2829 0.8842 1.0871 0.028 Uiso 1 1 calc R . . C6 C 1.1644(3) 0.8874(4) 0.9708(2) 0.0185(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01727(17) 0.01865(17) 0.02344(18) -0.00096(12) 0.00667(11) -0.00416(10) O2 0.0204(14) 0.0345(15) 0.0352(16) -0.0003(13) 0.0096(12) -0.0104(12) O3 0.0165(13) 0.0353(15) 0.0281(15) 0.0074(13) 0.0010(11) -0.0102(11) O6 0.0193(13) 0.0190(13) 0.0269(14) 0.0024(11) 0.0085(11) -0.0011(10) O1 0.0244(14) 0.0351(15) 0.0255(15) 0.0059(13) -0.0023(11) -0.0078(12) O7 0.0194(14) 0.0290(15) 0.0435(17) -0.0049(14) 0.0002(12) -0.0010(12) O8 0.0299(15) 0.0234(14) 0.0340(15) -0.0050(13) 0.0117(12) 0.0029(12) C14 0.0160(18) 0.0180(18) 0.031(2) -0.0026(16) 0.0037(16) 0.0032(15) C13 0.0159(18) 0.0221(18) 0.027(2) -0.0009(17) 0.0068(15) -0.0021(16) C3 0.0194(19) 0.025(2) 0.028(2) 0.0012(17) 0.0076(16) -0.0035(15) C5 0.0169(18) 0.0171(17) 0.0245(19) -0.0025(16) 0.0046(15) 0.0011(14) C10 0.0196(19) 0.028(2) 0.0250(19) -0.0027(18) 0.0007(16) -0.0027(16) C2 0.0216(19) 0.031(2) 0.0220(19) 0.0004(17) 0.0030(16) -0.0030(17) C4 0.0142(17) 0.0212(17) 0.026(2) -0.0009(16) 0.0027(15) -0.0018(15) O4 0.0170(13) 0.0369(15) 0.0261(15) 0.0024(12) 0.0065(11) -0.0105(11) O5 0.0346(15) 0.0174(12) 0.0361(16) -0.0040(12) 0.0170(13) -0.0014(12) C7 0.0160(19) 0.0198(18) 0.028(2) -0.0036(16) 0.0061(16) -0.0008(15) C8 0.025(2) 0.032(2) 0.027(2) 0.0006(18) 0.0111(17) -0.0027(17) C9 0.026(2) 0.035(2) 0.0196(19) 0.0009(18) 0.0022(16) 0.0010(17) C12 0.0108(16) 0.0208(18) 0.0208(18) -0.0011(15) 0.0010(14) -0.0005(14) C11 0.023(2) 0.0240(19) 0.027(2) -0.0038(17) 0.0121(16) -0.0063(16) C1 0.0164(18) 0.0262(19) 0.027(2) -0.0015(17) 0.0016(15) -0.0027(16) C6 0.0164(17) 0.0171(17) 0.0222(18) -0.0043(16) 0.0050(15) 0.0024(15) _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 O8 2.251(2) . ? Cd1 O6 2.268(2) 1_445 ? Cd1 O1 2.287(3) . ? Cd1 O7 2.337(2) . ? Cd1 O5 2.394(3) 2_746 ? Cd1 O6 2.524(2) 2_746 ? Cd1 O2 2.624(3) . ? O2 C14 1.262(5) . ? O3 C4 1.373(4) . ? O3 C13 1.425(4) . ? O6 C12 1.269(4) . ? O6 Cd1 2.268(2) 1_665 ? O6 Cd1 2.524(2) 2_756 ? O1 C14 1.253(5) . ? C14 C13 1.511(5) . ? C13 H13B 0.9700 . ? C13 H13A 0.9700 . ? C3 C4 1.372(5) . ? C3 C2 1.406(5) . ? C3 H3 0.9300 . ? C5 C10 1.407(5) . ? C5 C4 1.423(5) . ? C5 C6 1.431(5) . ? C10 C9 1.358(5) . ? C10 H10 0.9300 . ? C2 C1 1.354(5) . ? C2 H2 0.9300 . ? O4 C7 1.378(4) . ? O4 C11 1.425(4) . ? O5 C12 1.252(4) . ? O5 Cd1 2.394(3) 2_756 ? C7 C8 1.367(6) . ? C7 C6 1.418(5) . ? C8 C9 1.407(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C12 C11 1.515(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C1 C6 1.411(5) . ? C1 H1 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 O8 Cd1 O6 126.20(9) . 1_445 ? O8 Cd1 O1 102.62(10) . . ? O6 Cd1 O1 108.13(10) 1_445 . ? O8 Cd1 O7 79.05(10) . . ? O6 Cd1 O7 79.74(9) 1_445 . ? O1 Cd1 O7 167.67(10) . . ? O8 Cd1 O5 143.46(9) . 2_746 ? O6 Cd1 O5 83.16(8) 1_445 2_746 ? O1 Cd1 O5 84.74(10) . 2_746 ? O7 Cd1 O5 86.87(10) . 2_746 ? O8 Cd1 O6 93.14(9) . 2_746 ? O6 Cd1 O6 135.87(5) 1_445 2_746 ? O1 Cd1 O6 77.06(9) . 2_746 ? O7 Cd1 O6 90.67(9) . 2_746 ? O5 Cd1 O6 53.17(8) 2_746 2_746 ? O8 Cd1 O2 80.38(9) . . ? O6 Cd1 O2 84.41(8) 1_445 . ? O1 Cd1 O2 52.83(9) . . ? O7 Cd1 O2 138.91(9) . . ? O5 Cd1 O2 128.61(9) 2_746 . ? O6 Cd1 O2 125.69(8) 2_746 . ? C14 O2 Cd1 84.4(2) . . ? C4 O3 C13 116.8(3) . . ? C12 O6 Cd1 129.6(2) . 1_665 ? C12 O6 Cd1 88.5(2) . 2_756 ? Cd1 O6 Cd1 130.37(10) 1_665 2_756 ? C14 O1 Cd1 100.3(2) . . ? O1 C14 O2 122.6(3) . . ? O1 C14 C13 120.3(3) . . ? O2 C14 C13 117.1(3) . . ? O3 C13 C14 110.1(3) . . ? O3 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? O3 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? H13B C13 H13A 108.2 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C10 C5 C4 122.7(3) . . ? C10 C5 C6 119.4(3) . . ? C4 C5 C6 117.9(3) . . ? C9 C10 C5 120.3(3) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? C1 C2 C3 121.0(4) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C3 C4 O3 124.1(3) . . ? C3 C4 C5 121.1(3) . . ? O3 C4 C5 114.8(3) . . ? C7 O4 C11 118.4(3) . . ? C12 O5 Cd1 94.9(2) . 2_756 ? C8 C7 O4 124.6(3) . . ? C8 C7 C6 121.6(3) . . ? O4 C7 C6 113.8(3) . . ? C7 C8 C9 119.2(4) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 121.6(4) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? O5 C12 O6 121.8(3) . . ? O5 C12 C11 121.2(3) . . ? O6 C12 C11 117.0(3) . . ? O4 C11 C12 115.0(3) . . ? O4 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? O4 C11 H11B 108.5 . . ? C12 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C2 C1 C6 120.9(3) . . ? C2 C1 H1 119.5 . . ? C6 C1 H1 119.5 . . ? C1 C6 C7 122.9(3) . . ? C1 C6 C5 119.2(3) . . ? C7 C6 C5 117.9(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.701 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.142 #===END data_1112-1 _database_code_depnum_ccdc_archive 'CCDC 807896' #TrackingRef '- 0923.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H17 N O7 Pb' _chemical_formula_weight 554.51 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 11.9066(2) _cell_length_b 20.4425(4) _cell_length_c 7.46310(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.596(2) _cell_angle_gamma 90.00 _cell_volume 1796.12(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4625 _cell_measurement_theta_min 2.6337 _cell_measurement_theta_max 28.8437 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 9.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.50600 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku XCaliburE' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7539 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3110 _reflns_number_gt 2402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0180P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3110 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0397 _refine_ls_wR_factor_gt 0.0388 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.839861(14) 0.794752(8) 0.04988(2) 0.03212(6) Uani 1 1 d . . . O1 O 0.6166(3) 0.78709(15) 0.0813(4) 0.0501(9) Uani 1 1 d . . . O3 O 0.5398(2) 0.62555(14) 0.2052(3) 0.0398(8) Uani 1 1 d . . . O4 O 0.9638(3) 0.69506(14) 0.1595(4) 0.0470(8) Uani 1 1 d . . . C1 C 0.5763(3) 0.6067(2) -0.1018(5) 0.0355(11) Uani 1 1 d . . . H1 H 0.6015 0.6494 -0.1127 0.043 Uiso 1 1 calc R . . O6 O 1.0246(2) 0.56397(14) 0.1488(4) 0.0427(8) Uani 1 1 d . . . O2 O 0.7278(2) 0.70717(14) 0.1953(4) 0.0385(7) Uani 1 1 d . . . C2 C 0.5739(3) 0.5628(2) -0.2459(5) 0.0379(11) Uani 1 1 d . . . H2 H 0.5984 0.5767 -0.3522 0.045 Uiso 1 1 calc R . . O5 O 0.8627(3) 0.68966(16) -0.1115(4) 0.0509(9) Uani 1 1 d . . . C4 C 0.5012(3) 0.5216(2) 0.0752(5) 0.0268(9) Uani 1 1 d . . . C7 C 0.6314(4) 0.7321(2) 0.1467(5) 0.0290(10) Uani 1 1 d . . . C6 C 0.5269(3) 0.69346(19) 0.1715(6) 0.0349(11) Uani 1 1 d . . . H6A H 0.4949 0.7128 0.2714 0.042 Uiso 1 1 calc R . . H6B H 0.4715 0.6991 0.0633 0.042 Uiso 1 1 calc R . . C13 C 1.1447(3) 0.4963(2) 0.4328(5) 0.0337(11) Uani 1 1 d . . . H13 H 1.1819 0.5097 0.3381 0.040 Uiso 1 1 calc R . . C5 C 0.5414(3) 0.58628(19) 0.0555(5) 0.0286(10) Uani 1 1 d . . . O7 O 1.0502(3) 0.83497(19) 0.1460(4) 0.0636(10) Uani 1 1 d . . . C3 C 0.5366(3) 0.5001(2) -0.2344(5) 0.0327(10) Uani 1 1 d . . . H3 H 0.5361 0.4718 -0.3319 0.039 Uiso 1 1 calc R . . C12 C 1.0279(3) 0.51011(19) 0.4281(5) 0.0275(10) Uani 1 1 d . . . C10 C 0.8507(4) 0.5576(2) 0.2805(5) 0.0380(11) Uani 1 1 d . . . H10 H 0.8093 0.5799 0.1839 0.046 Uiso 1 1 calc R . . C8 C 0.9299(4) 0.6636(2) 0.0188(6) 0.0397(12) Uani 1 1 d . . . C11 C 0.9633(4) 0.54536(19) 0.2818(5) 0.0318(10) Uani 1 1 d . . . C9 C 0.9637(4) 0.5942(2) -0.0089(5) 0.0483(13) Uani 1 1 d . . . H9A H 0.8958 0.5688 -0.0491 0.058 Uiso 1 1 calc R . . H9B H 1.0105 0.5930 -0.1048 0.058 Uiso 1 1 calc R . . C15 C 1.1222(4) 0.8323(3) 0.0427(7) 0.0578(14) Uani 1 1 d . . . H15 H 1.0984 0.8198 -0.0768 0.069 Uiso 1 1 calc R . . N1 N 1.2295(4) 0.8460(2) 0.0911(7) 0.0739(14) Uani 1 1 d . . . C14 C 1.2022(4) 0.4636(2) 0.5748(6) 0.0424(12) Uani 1 1 d . . . H14 H 1.2790 0.4550 0.5765 0.051 Uiso 1 1 calc R . . C16 C 1.2674(5) 0.8693(4) 0.2719(10) 0.142(3) Uani 1 1 d . . . H16A H 1.3478 0.8771 0.2873 0.213 Uiso 1 1 calc R . . H16B H 1.2508 0.8371 0.3580 0.213 Uiso 1 1 calc R . . H16C H 1.2287 0.9094 0.2912 0.213 Uiso 1 1 calc R . . C17 C 1.3092(5) 0.8463(5) -0.0368(11) 0.157(4) Uani 1 1 d . . . H17A H 1.3833 0.8576 0.0246 0.236 Uiso 1 1 calc R . . H17B H 1.2856 0.8779 -0.1302 0.236 Uiso 1 1 calc R . . H17C H 1.3117 0.8037 -0.0900 0.236 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.03540(10) 0.03257(10) 0.02804(9) -0.00168(9) 0.00357(7) -0.00755(9) O1 0.068(2) 0.033(2) 0.0498(19) 0.0129(16) 0.0109(17) -0.0028(17) O3 0.059(2) 0.031(2) 0.0305(16) -0.0067(13) 0.0125(15) -0.0122(15) O4 0.0453(19) 0.032(2) 0.058(2) 0.0018(16) -0.0094(17) 0.0055(15) C1 0.047(3) 0.025(3) 0.036(2) -0.002(2) 0.010(2) -0.013(2) O6 0.0537(19) 0.043(2) 0.0337(16) 0.0218(14) 0.0149(15) 0.0213(16) O2 0.0290(17) 0.047(2) 0.0390(17) -0.0096(15) 0.0019(14) -0.0025(16) C2 0.047(3) 0.045(3) 0.025(2) -0.001(2) 0.018(2) -0.009(2) O5 0.068(2) 0.061(3) 0.0254(16) 0.0191(14) 0.0122(16) 0.0344(17) C4 0.025(2) 0.029(3) 0.027(2) 0.0006(17) 0.0067(19) -0.0019(19) C7 0.039(3) 0.030(3) 0.018(2) -0.0075(18) 0.005(2) -0.005(2) C6 0.032(2) 0.033(3) 0.039(2) -0.008(2) 0.004(2) 0.000(2) C13 0.034(3) 0.031(3) 0.036(2) 0.008(2) 0.008(2) 0.008(2) C5 0.026(2) 0.029(3) 0.029(2) -0.0047(18) 0.0001(19) -0.0046(19) O7 0.049(2) 0.081(3) 0.063(2) -0.011(2) 0.016(2) -0.024(2) C3 0.039(3) 0.036(3) 0.024(2) -0.0046(19) 0.009(2) -0.007(2) C12 0.038(3) 0.019(2) 0.025(2) 0.0038(17) 0.0023(19) 0.0080(19) C10 0.045(3) 0.037(3) 0.030(2) 0.012(2) -0.001(2) 0.015(2) C8 0.039(3) 0.042(3) 0.042(3) 0.023(2) 0.020(2) 0.011(2) C11 0.043(3) 0.026(3) 0.027(2) 0.0050(18) 0.007(2) 0.008(2) C9 0.074(4) 0.045(3) 0.027(2) 0.015(2) 0.015(2) 0.024(3) C15 0.050(4) 0.058(4) 0.063(4) -0.004(3) 0.001(3) -0.011(3) N1 0.040(3) 0.070(4) 0.110(4) 0.018(3) 0.007(3) 0.002(3) C14 0.031(3) 0.048(3) 0.047(3) 0.005(2) 0.001(2) 0.008(2) C16 0.076(5) 0.172(10) 0.156(8) 0.019(7) -0.053(5) -0.019(5) C17 0.086(5) 0.165(9) 0.246(10) 0.059(7) 0.105(6) 0.043(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O5 2.498(3) . ? Pb1 O5 2.521(3) 4_576 ? Pb1 O2 2.568(3) . ? Pb1 O4 2.577(3) . ? Pb1 O7 2.632(3) . ? Pb1 O1 2.707(3) . ? O1 C7 1.228(5) . ? O3 C5 1.378(4) . ? O3 C6 1.415(4) . ? O4 C8 1.247(5) . ? C1 C5 1.368(5) . ? C1 C2 1.397(5) . ? C1 H1 0.9300 . ? O6 C11 1.371(4) . ? O6 C9 1.428(5) . ? O2 C7 1.259(5) . ? C2 C3 1.363(6) . ? C2 H2 0.9300 . ? O5 C8 1.280(5) . ? O5 Pb1 2.521(3) 4_575 ? C4 C3 1.403(5) 3_665 ? C4 C5 1.421(5) . ? C4 C4 1.426(7) 3_665 ? C7 C6 1.508(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C13 C14 1.349(5) . ? C13 C12 1.415(5) . ? C13 H13 0.9300 . ? O7 C15 1.236(5) . ? C3 C4 1.403(5) 3_665 ? C3 H3 0.9300 . ? C12 C12 1.406(7) 3_766 ? C12 C11 1.433(5) . ? C10 C11 1.362(5) . ? C10 C14 1.398(5) 3_766 ? C10 H10 0.9300 . ? C8 C9 1.497(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C15 N1 1.306(6) . ? C15 H15 0.9300 . ? N1 C16 1.439(8) . ? N1 C17 1.443(7) . ? C14 C10 1.398(5) 3_766 ? C14 H14 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? 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 O5 Pb1 O5 126.09(8) . 4_576 ? O5 Pb1 O2 72.83(9) . . ? O5 Pb1 O2 69.48(9) 4_576 . ? O5 Pb1 O4 51.29(9) . . ? O5 Pb1 O4 79.10(11) 4_576 . ? O2 Pb1 O4 67.89(10) . . ? O5 Pb1 O7 103.44(11) . . ? O5 Pb1 O7 74.45(10) 4_576 . ? O2 Pb1 O7 129.48(10) . . ? O4 Pb1 O7 71.57(11) . . ? O5 Pb1 O1 99.84(10) . . ? O5 Pb1 O1 83.13(10) 4_576 . ? O2 Pb1 O1 49.03(9) . . ? O4 Pb1 O1 116.74(9) . . ? O7 Pb1 O1 154.29(10) . . ? C7 O1 Pb1 90.2(3) . . ? C5 O3 C6 116.2(3) . . ? C8 O4 Pb1 92.4(3) . . ? C5 C1 C2 119.4(4) . . ? C5 C1 H1 120.3 . . ? C2 C1 H1 120.3 . . ? C11 O6 C9 117.2(3) . . ? C7 O2 Pb1 96.1(3) . . ? C3 C2 C1 121.6(4) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C8 O5 Pb1 95.3(3) . . ? C8 O5 Pb1 140.9(3) . 4_575 ? Pb1 O5 Pb1 111.81(11) . 4_575 ? C3 C4 C5 122.5(3) 3_665 . ? C3 C4 C4 119.9(5) 3_665 3_665 ? C5 C4 C4 117.5(4) . 3_665 ? O1 C7 O2 123.7(4) . . ? O1 C7 C6 117.2(4) . . ? O2 C7 C6 119.1(4) . . ? O3 C6 C7 117.7(4) . . ? O3 C6 H6A 107.9 . . ? C7 C6 H6A 107.9 . . ? O3 C6 H6B 107.9 . . ? C7 C6 H6B 107.9 . . ? H6A C6 H6B 107.2 . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C1 C5 O3 124.1(4) . . ? C1 C5 C4 121.6(4) . . ? O3 C5 C4 114.3(3) . . ? C15 O7 Pb1 122.4(3) . . ? C2 C3 C4 120.0(4) . 3_665 ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 3_665 . ? C12 C12 C13 119.8(4) 3_766 . ? C12 C12 C11 117.9(4) 3_766 . ? C13 C12 C11 122.3(3) . . ? C11 C10 C14 119.7(4) . 3_766 ? C11 C10 H10 120.2 . . ? C14 C10 H10 120.2 3_766 . ? O4 C8 O5 120.8(4) . . ? O4 C8 C9 123.0(4) . . ? O5 C8 C9 116.1(5) . . ? C10 C11 O6 125.1(4) . . ? C10 C11 C12 120.9(4) . . ? O6 C11 C12 114.0(3) . . ? O6 C9 C8 114.2(4) . . ? O6 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? O6 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? O7 C15 N1 124.0(5) . . ? O7 C15 H15 118.0 . . ? N1 C15 H15 118.0 . . ? C15 N1 C16 119.1(5) . . ? C15 N1 C17 122.1(6) . . ? C16 N1 C17 118.3(6) . . ? C13 C14 C10 121.7(4) . 3_766 ? C13 C14 H14 119.1 . . ? C10 C14 H14 119.1 3_766 . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.919 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.094 #===END #===END data_1224-2 _database_code_depnum_ccdc_archive 'CCDC 807897' #TrackingRef '- 0923.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 Cd N2 O6' _chemical_formula_weight 566.83 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.8352(9) _cell_length_b 11.4382(3) _cell_length_c 7.3069(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.104(4) _cell_angle_gamma 90.00 _cell_volume 2137.69(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3645 _cell_measurement_theta_min 2.8101 _cell_measurement_theta_max 28.6508 _exptl_crystal_description rectangular _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76744 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4506 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1880 _reflns_number_gt 1691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0281P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1880 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.0000 0.600158(16) 0.7500 0.02404(9) Uani 1 2 d S . . O2 O 0.97031(6) 0.61540(13) 0.4347(2) 0.0320(4) Uani 1 1 d . . . O3 O 1.07755(6) 0.51200(12) 0.7445(2) 0.0364(4) Uani 1 1 d . . . O1 O 0.84055(6) 0.63218(12) 0.2221(2) 0.0343(4) Uani 1 1 d . . . N1 N 0.95049(7) 0.77445(14) 0.7951(2) 0.0280(4) Uani 1 1 d . . . C1 C 0.90238(10) 0.7749(2) 0.8369(3) 0.0383(6) Uani 1 1 d . . . H1 H 0.8868 0.7035 0.8562 0.046 Uiso 1 1 calc R . . C2 C 0.87384(11) 0.8765(2) 0.8535(4) 0.0497(7) Uani 1 1 d . . . H2 H 0.8397 0.8729 0.8802 0.060 Uiso 1 1 calc R . . C3 C 0.89684(10) 0.9809(2) 0.8300(4) 0.0490(7) Uani 1 1 d . . . H3 H 0.8783 1.0499 0.8394 0.059 Uiso 1 1 calc R . . C4 C 0.94824(10) 0.98531(18) 0.7916(3) 0.0362(6) Uani 1 1 d . . . C5 C 0.97362(9) 0.87860(16) 0.7716(3) 0.0272(5) Uani 1 1 d . . . C6 C 0.97544(11) 1.09238(17) 0.7695(4) 0.0459(7) Uani 1 1 d . . . H6 H 0.9587 1.1632 0.7825 0.055 Uiso 1 1 calc R . . C13 C 0.92799(9) 0.57810(16) 0.3534(3) 0.0253(5) Uani 1 1 d . . . C12 C 0.87970(8) 0.64687(18) 0.3786(3) 0.0281(5) Uani 1 1 d . . . H12A H 0.8664 0.6203 0.4891 0.034 Uiso 1 1 calc R . . H12B H 0.8885 0.7291 0.3941 0.034 Uiso 1 1 calc R . . C10 C 0.80090(8) 0.71206(16) 0.1979(3) 0.0255(5) Uani 1 1 d . . . C11 C 0.79027(9) 0.79085(18) 0.3285(3) 0.0313(5) Uani 1 1 d . . . H11 H 0.8101 0.7913 0.4450 0.038 Uiso 1 1 calc R . . C9 C 0.77052(8) 0.70858(16) 0.0201(3) 0.0239(5) Uani 1 1 d . . . C8 C 0.78043(9) 0.62739(17) -0.1173(3) 0.0290(5) Uani 1 1 d . . . H8 H 0.8073 0.5731 -0.0917 0.035 Uiso 1 1 calc R . . C7 C 0.75098(9) 0.62864(19) -0.2854(3) 0.0330(5) Uani 1 1 d . . . H7 H 0.7581 0.5753 -0.3746 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01861(14) 0.02128(12) 0.02943(14) 0.000 -0.00632(10) 0.000 O2 0.0210(9) 0.0434(8) 0.0293(8) 0.0015(7) -0.0044(7) -0.0009(7) O3 0.0330(10) 0.0293(8) 0.0439(10) -0.0110(7) -0.0056(8) 0.0095(7) O1 0.0266(9) 0.0341(7) 0.0374(9) -0.0043(7) -0.0117(8) 0.0149(7) N1 0.0263(11) 0.0244(8) 0.0330(10) 0.0006(8) 0.0030(9) -0.0029(8) C1 0.0292(14) 0.0349(12) 0.0522(16) -0.0003(11) 0.0110(13) -0.0035(10) C2 0.0315(15) 0.0479(14) 0.074(2) -0.0030(14) 0.0214(15) 0.0035(12) C3 0.0428(17) 0.0361(13) 0.0717(19) -0.0016(13) 0.0210(16) 0.0121(12) C4 0.0413(15) 0.0281(11) 0.0409(14) 0.0001(10) 0.0116(13) 0.0076(10) C5 0.0309(13) 0.0237(10) 0.0265(11) -0.0003(9) 0.0025(10) 0.0010(9) C6 0.0588(19) 0.0224(11) 0.0596(17) 0.0003(11) 0.0191(15) 0.0048(10) C13 0.0263(13) 0.0246(10) 0.0232(11) 0.0064(9) -0.0025(10) 0.0048(9) C12 0.0231(12) 0.0266(10) 0.0317(12) -0.0017(9) -0.0058(10) 0.0052(9) C10 0.0175(11) 0.0245(10) 0.0333(12) 0.0063(9) 0.0002(10) 0.0053(9) C11 0.0244(13) 0.0379(12) 0.0303(12) 0.0021(10) -0.0014(10) 0.0052(10) C9 0.0147(10) 0.0244(10) 0.0324(12) 0.0071(9) 0.0030(9) 0.0017(8) C8 0.0202(12) 0.0262(10) 0.0402(13) 0.0020(10) 0.0026(11) 0.0083(9) C7 0.0306(14) 0.0341(11) 0.0344(13) -0.0053(10) 0.0051(12) 0.0091(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.2484(15) 2_756 ? Cd1 O3 2.2484(15) . ? Cd1 O2 2.3300(15) 2_756 ? Cd1 O2 2.3300(15) . ? Cd1 N1 2.4161(17) 2_756 ? Cd1 N1 2.4161(17) . ? O2 C13 1.244(3) . ? O3 C13 1.251(2) 5_766 ? O1 C10 1.365(2) . ? O1 C12 1.426(2) . ? N1 C1 1.321(3) . ? N1 C5 1.354(3) . ? C1 C2 1.391(3) . ? C1 H1 0.9300 . ? C2 C3 1.356(3) . ? C2 H2 0.9300 . ? C3 C4 1.396(3) . ? C3 H3 0.9300 . ? C4 C5 1.403(3) . ? C4 C6 1.432(3) . ? C5 C5 1.442(5) 2_756 ? C6 C6 1.339(5) 2_756 ? C6 H6 0.9300 . ? C13 O3 1.251(2) 5_766 ? C13 C12 1.508(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C10 C11 1.368(3) . ? C10 C9 1.420(3) . ? C11 C7 1.410(3) 7_665 ? C11 H11 0.9300 . ? C9 C8 1.418(3) . ? C9 C9 1.422(4) 7_665 ? C8 C7 1.351(3) . ? C8 H8 0.9300 . ? C7 C11 1.410(3) 7_665 ? C7 H7 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 O3 Cd1 O3 126.71(8) 2_756 . ? O3 Cd1 O2 100.70(5) 2_756 2_756 ? O3 Cd1 O2 83.19(5) . 2_756 ? O3 Cd1 O2 83.19(5) 2_756 . ? O3 Cd1 O2 100.70(5) . . ? O2 Cd1 O2 171.42(7) 2_756 . ? O3 Cd1 N1 149.62(6) 2_756 2_756 ? O3 Cd1 N1 82.96(5) . 2_756 ? O2 Cd1 N1 88.06(6) 2_756 2_756 ? O2 Cd1 N1 84.86(5) . 2_756 ? O3 Cd1 N1 82.96(5) 2_756 . ? O3 Cd1 N1 149.62(6) . . ? O2 Cd1 N1 84.86(5) 2_756 . ? O2 Cd1 N1 88.06(6) . . ? N1 Cd1 N1 68.80(8) 2_756 . ? C13 O2 Cd1 126.25(14) . . ? C13 O3 Cd1 110.44(14) 5_766 . ? C10 O1 C12 117.34(16) . . ? C1 N1 C5 118.18(18) . . ? C1 N1 Cd1 124.61(14) . . ? C5 N1 Cd1 117.20(14) . . ? N1 C1 C2 123.4(2) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.6(2) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.2(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 117.5(2) . . ? C3 C4 C6 123.3(2) . . ? C5 C4 C6 119.2(2) . . ? N1 C5 C4 122.1(2) . . ? N1 C5 C5 118.38(12) . 2_756 ? C4 C5 C5 119.53(14) . 2_756 ? C6 C6 C4 121.25(14) 2_756 . ? C6 C6 H6 119.4 2_756 . ? C4 C6 H6 119.4 . . ? O2 C13 O3 125.3(2) . 5_766 ? O2 C13 C12 116.70(18) . . ? O3 C13 C12 118.0(2) 5_766 . ? O1 C12 C13 110.24(16) . . ? O1 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? O1 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? O1 C10 C11 124.8(2) . . ? O1 C10 C9 114.03(17) . . ? C11 C10 C9 121.12(18) . . ? C10 C11 C7 119.6(2) . 7_665 ? C10 C11 H11 120.2 . . ? C7 C11 H11 120.2 7_665 . ? C8 C9 C10 122.32(18) . . ? C8 C9 C9 119.6(2) . 7_665 ? C10 C9 C9 118.1(2) . 7_665 ? C7 C8 C9 120.17(19) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C7 C11 121.4(2) . 7_665 ? C8 C7 H7 119.3 . . ? C11 C7 H7 119.3 7_665 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.291 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.062 #===END data_1224-3 _database_code_depnum_ccdc_archive 'CCDC 807898' #TrackingRef '- 0923.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H66 Cd5 N4 O30' _chemical_formula_weight 2245.47 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7493(11) _cell_length_b 12.9213(13) _cell_length_c 14.2679(17) _cell_angle_alpha 107.940(10) _cell_angle_beta 97.377(9) _cell_angle_gamma 97.394(8) _cell_volume 2011.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5991 _cell_measurement_theta_min 2.5337 _cell_measurement_theta_max 29.1752 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1114 _exptl_absorpt_coefficient_mu 1.394 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64156 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford XCaliburE' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13863 _diffrn_reflns_av_R_equivalents 0.1025 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7049 _reflns_number_gt 5087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.1981P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7049 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.2678 _refine_ls_wR_factor_gt 0.2079 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.5000 0.5000 0.0264(3) Uani 1 2 d S . . Cd2 Cd 0.53895(6) -0.55775(6) 0.23443(5) 0.0372(3) Uani 1 1 d . . . Cd3 Cd 0.28331(5) 0.44636(5) 0.49350(5) 0.0285(3) Uani 1 1 d . . . O14 O 0.1811(6) 0.2981(5) 0.5091(6) 0.0414(17) Uani 1 1 d . . . O13 O 0.5763(6) -0.4373(6) 0.3956(5) 0.0392(16) Uani 1 1 d . . . O15 O 0.6585(6) -0.6567(6) 0.2889(6) 0.0446(17) Uani 1 1 d . . . O5 O 0.1105(6) 0.4766(6) 0.3748(5) 0.0445(18) Uani 1 1 d . . . O12 O -0.0029(6) 0.3260(5) 0.4999(6) 0.0396(16) Uani 1 1 d . . . O1 O 0.4549(6) -0.1925(6) 0.4416(5) 0.0432(17) Uani 1 1 d . . . O11 O 0.1832(5) 0.5536(5) 0.6044(5) 0.0329(14) Uani 1 1 d . . . O10 O 0.2225(6) 0.8051(6) 0.8025(5) 0.0500(19) Uani 1 1 d . . . O2 O 0.4675(6) -0.3760(7) 0.2949(5) 0.0458(18) Uani 1 1 d . . . O9 O 0.3592(6) -0.6418(7) 0.3617(5) 0.0475(18) Uani 1 1 d . . . C19 C 0.5202(7) -0.3632(7) 0.3786(7) 0.0292(19) Uani 1 1 d . . . O8 O 0.3594(7) -0.6525(7) 0.2040(6) 0.056(2) Uani 1 1 d . . . N2 N 0.5233(7) -0.6517(7) 0.0648(6) 0.043(2) Uani 1 1 d . . . C33 C 0.2385(8) 0.6409(8) 0.6754(7) 0.035(2) Uani 1 1 d . . . C18 C 0.5202(9) -0.2649(8) 0.4702(8) 0.040(2) Uani 1 1 d . . . H18A H 0.4863 -0.2898 0.5197 0.048 Uiso 1 1 calc R . . H18B H 0.5996 -0.2270 0.4997 0.048 Uiso 1 1 calc R . . C25 C 0.1739(9) -1.1051(9) -0.1560(8) 0.041(2) Uani 1 1 d . . . O6 O 0.1280(6) 0.1188(6) 0.5679(6) 0.0427(17) Uani 1 1 d . . . O7 O 0.1597(6) -0.8074(6) 0.1367(6) 0.053(2) Uani 1 1 d . . . C45 C 0.0778(7) 0.2739(8) 0.5125(7) 0.032(2) Uani 1 1 d . . . C6 C 0.5892(8) -0.6020(9) 0.0142(7) 0.038(2) Uani 1 1 d . . . O4 O 0.2837(7) 0.5869(7) 0.4330(7) 0.058(2) Uani 1 1 d . . . N1 N 0.6733(7) -0.4585(8) 0.1708(7) 0.050(2) Uani 1 1 d . . . C24 C 0.3143(9) -0.6733(9) 0.2725(9) 0.046(3) Uani 1 1 d . . . C15 C 0.2651(7) 0.0010(8) 0.5392(8) 0.037(2) Uani 1 1 d . . . C40 C 0.1877(8) 0.5534(8) 0.3720(9) 0.041(2) Uani 1 1 d . . . C11 C 0.4039(8) -0.1267(8) 0.5121(7) 0.034(2) Uani 1 1 d . . . C30 C 0.2206(8) -1.0426(8) -0.0532(8) 0.037(2) Uani 1 1 d . . . C16 C 0.3256(7) -0.0685(8) 0.4752(8) 0.034(2) Uani 1 1 d . . . C22 C 0.2145(9) -0.8910(8) 0.0977(8) 0.040(2) Uani 1 1 d . . . C43 C 0.1837(7) 0.0556(7) 0.4989(8) 0.033(2) Uani 1 1 d . . . C5 C 0.6680(8) -0.4948(8) 0.0703(7) 0.036(2) Uani 1 1 d . . . C12 C 0.4230(9) -0.1131(9) 0.6117(9) 0.046(3) Uani 1 1 d . . . H12 H 0.4759 -0.1498 0.6370 0.055 Uiso 1 1 calc R . . C7 C 0.5790(10) -0.6533(10) -0.0900(8) 0.048(3) Uani 1 1 d . . . H7 H 0.6250 -0.6207 -0.1253 0.058 Uiso 1 1 calc R . . C44 C 0.0371(8) 0.1670(8) 0.5347(9) 0.040(2) Uani 1 1 d . . . H44A H -0.0119 0.1832 0.5853 0.048 Uiso 1 1 calc R . . H44B H -0.0104 0.1135 0.4743 0.048 Uiso 1 1 calc R . . C14 C 0.2868(9) 0.0133(8) 0.6417(8) 0.040(2) Uani 1 1 d . . . H14 H 0.2497 0.0601 0.6865 0.048 Uiso 1 1 calc R . . C17 C 0.3027(9) -0.0832(9) 0.3695(8) 0.044(2) Uani 1 1 d . . . H17 H 0.3413 -0.1288 0.3252 0.053 Uiso 1 1 calc R . . C42 C 0.1658(9) 0.0403(9) 0.3999(8) 0.046(3) Uani 1 1 d . . . H42 H 0.1135 0.0773 0.3743 0.055 Uiso 1 1 calc R . . C29 C 0.1698(8) -0.9502(8) -0.0050(8) 0.040(2) Uani 1 1 d . . . O3 O 0.0827(9) 0.5508(9) 0.2195(8) 0.088(4) Uani 1 1 d . . . C28 C 0.0769(8) -0.9230(9) -0.0593(8) 0.043(2) Uani 1 1 d . . . H28 H 0.0409 -0.8650 -0.0279 0.051 Uiso 1 1 calc R . . C13 C 0.3642(10) -0.0454(10) 0.6748(8) 0.049(3) Uani 1 1 d . . . H13 H 0.3769 -0.0387 0.7423 0.059 Uiso 1 1 calc R . . C41 C 0.2232(10) -0.0285(9) 0.3362(8) 0.047(3) Uani 1 1 d . . . H41 H 0.2073 -0.0381 0.2682 0.056 Uiso 1 1 calc R . . C39 C 0.1701(9) 0.6127(10) 0.2981(8) 0.046(3) Uani 1 1 d . . . H39A H 0.1495 0.6839 0.3303 0.055 Uiso 1 1 calc R . . H39B H 0.2419 0.6255 0.2734 0.055 Uiso 1 1 calc R . . C9 C 0.4361(11) -0.8000(12) -0.0840(10) 0.061(3) Uani 1 1 d . . . H9 H 0.3833 -0.8659 -0.1147 0.073 Uiso 1 1 calc R . . C21 C 0.3042(11) -0.9219(11) 0.1472(10) 0.056(3) Uani 1 1 d . . . H21 H 0.3322 -0.8823 0.2145 0.067 Uiso 1 1 calc R . . C1 C 0.7449(10) -0.3663(10) 0.2255(10) 0.057(3) Uani 1 1 d . . . H1 H 0.7494 -0.3440 0.2946 0.068 Uiso 1 1 calc R . . C26 C 0.0821(9) -1.0751(10) -0.2074(9) 0.051(3) Uani 1 1 d . . . H26 H 0.0495 -1.1163 -0.2735 0.061 Uiso 1 1 calc R . . C8 C 0.5011(11) -0.7522(11) -0.1414(9) 0.060(3) Uani 1 1 d . . . H8 H 0.4926 -0.7850 -0.2104 0.072 Uiso 1 1 calc R . . C23 C 0.1956(10) -0.7468(10) 0.2427(8) 0.055(3) Uani 1 1 d . . . H23A H 0.1954 -0.7995 0.2786 0.066 Uiso 1 1 calc R . . H23B H 0.1381 -0.7014 0.2643 0.066 Uiso 1 1 calc R . . C10 C 0.4512(10) -0.7489(10) 0.0168(9) 0.054(3) Uani 1 1 d . . . H10 H 0.4098 -0.7827 0.0541 0.065 Uiso 1 1 calc R . . C4 C 0.7302(10) -0.4343(11) 0.0256(10) 0.056(3) Uani 1 1 d . . . H4 H 0.7237 -0.4583 -0.0437 0.068 Uiso 1 1 calc R . . C31 C 0.3125(10) -1.0714(10) 0.0002(9) 0.050(3) Uani 1 1 d . . . H31 H 0.3456 -1.1316 -0.0311 0.060 Uiso 1 1 calc R . . C32 C 0.1664(9) 0.7301(9) 0.7057(8) 0.046(3) Uani 1 1 d . . . H32A H 0.1611 0.7690 0.6575 0.055 Uiso 1 1 calc R . . H32B H 0.0882 0.6979 0.7085 0.055 Uiso 1 1 calc R . . C27 C 0.0405(9) -0.9806(11) -0.1561(10) 0.055(3) Uani 1 1 d . . . H27 H -0.0162 -0.9564 -0.1918 0.067 Uiso 1 1 calc R . . C2 C 0.8131(11) -0.3013(11) 0.1867(12) 0.068(4) Uani 1 1 d . . . H2 H 0.8631 -0.2370 0.2278 0.082 Uiso 1 1 calc R . . C36 C 0.0068(10) 0.4921(13) 0.0456(11) 0.062(3) Uani 1 1 d . . . C20 C 0.3542(11) -1.0097(11) 0.1004(11) 0.062(3) Uani 1 1 d . . . H20 H 0.4161 -1.0281 0.1358 0.074 Uiso 1 1 calc R . . C37 C 0.0730(12) 0.5687(12) 0.1304(10) 0.067(4) Uani 1 1 d . . . C35 C -0.0510(12) 0.3862(12) 0.0550(13) 0.070(4) Uani 1 1 d . . . H35 H -0.0445 0.3729 0.1157 0.084 Uiso 1 1 calc R . . C38 C 0.1270(12) 0.6719(13) 0.1226(13) 0.076(4) Uani 1 1 d . . . H38 H 0.1712 0.7279 0.1782 0.092 Uiso 1 1 calc R . . C3 C 0.8042(12) -0.3355(12) 0.0842(14) 0.082(5) Uani 1 1 d . . . H3 H 0.8472 -0.2933 0.0542 0.098 Uiso 1 1 calc R . . C34 C -0.1101(13) 0.3153(13) -0.0266(13) 0.078(4) Uani 1 1 d . . . H34 H -0.1456 0.2486 -0.0224 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0229(5) 0.0261(5) 0.0366(6) 0.0148(4) 0.0090(4) 0.0127(4) Cd2 0.0347(4) 0.0454(5) 0.0317(4) 0.0127(4) 0.0049(3) 0.0091(3) Cd3 0.0267(4) 0.0301(4) 0.0328(4) 0.0132(3) 0.0066(3) 0.0114(3) O14 0.042(4) 0.021(3) 0.064(5) 0.014(3) 0.019(3) 0.008(3) O13 0.042(4) 0.036(4) 0.037(4) 0.007(3) -0.003(3) 0.021(3) O15 0.035(4) 0.035(4) 0.055(5) 0.006(4) -0.004(3) 0.011(3) O5 0.054(4) 0.040(4) 0.044(4) 0.020(4) 0.016(3) 0.005(3) O12 0.036(4) 0.029(3) 0.056(5) 0.020(3) 0.000(3) 0.012(3) O1 0.053(4) 0.043(4) 0.047(4) 0.022(4) 0.018(3) 0.032(3) O11 0.034(3) 0.025(3) 0.028(3) -0.009(3) 0.001(3) 0.013(3) O10 0.054(4) 0.047(4) 0.036(4) -0.007(3) -0.002(3) 0.023(4) O2 0.051(4) 0.061(5) 0.034(4) 0.022(4) 0.009(3) 0.024(4) O9 0.043(4) 0.065(5) 0.035(4) 0.011(4) 0.012(3) 0.017(4) C19 0.027(4) 0.023(4) 0.033(5) 0.005(4) 0.003(4) 0.005(3) O8 0.053(5) 0.066(5) 0.043(4) 0.011(4) 0.021(4) -0.007(4) N2 0.049(5) 0.050(5) 0.028(4) 0.010(4) 0.009(4) 0.005(4) C33 0.037(5) 0.037(5) 0.037(5) 0.016(5) 0.011(4) 0.017(4) C18 0.040(5) 0.035(6) 0.047(6) 0.014(5) 0.003(5) 0.017(4) C25 0.037(5) 0.037(6) 0.050(6) 0.010(5) 0.012(5) 0.014(4) O6 0.046(4) 0.041(4) 0.058(5) 0.031(4) 0.018(3) 0.022(3) O7 0.044(4) 0.046(4) 0.059(5) -0.002(4) 0.014(4) 0.012(3) C45 0.023(4) 0.035(5) 0.046(6) 0.021(5) 0.005(4) 0.010(4) C6 0.038(5) 0.049(6) 0.024(5) 0.010(5) 0.000(4) 0.014(4) O4 0.048(5) 0.072(6) 0.069(6) 0.045(5) 0.011(4) 0.012(4) N1 0.040(5) 0.068(7) 0.053(6) 0.032(5) 0.012(4) 0.010(4) C24 0.042(6) 0.041(6) 0.063(8) 0.019(6) 0.028(6) 0.016(5) C15 0.025(4) 0.036(5) 0.066(7) 0.036(5) 0.013(4) 0.012(4) C40 0.036(5) 0.036(6) 0.059(7) 0.025(5) 0.014(5) 0.010(4) C11 0.036(5) 0.036(5) 0.037(5) 0.015(4) 0.009(4) 0.015(4) C30 0.034(5) 0.036(5) 0.041(6) 0.013(5) 0.007(4) 0.007(4) C16 0.024(4) 0.034(5) 0.049(6) 0.021(5) 0.005(4) 0.008(4) C22 0.041(5) 0.035(5) 0.038(6) 0.004(5) 0.009(4) 0.000(4) C43 0.020(4) 0.030(5) 0.060(7) 0.024(5) 0.014(4) 0.011(3) C5 0.031(5) 0.042(6) 0.040(6) 0.016(5) 0.009(4) 0.019(4) C12 0.048(6) 0.046(6) 0.052(7) 0.024(6) 0.006(5) 0.024(5) C7 0.053(6) 0.062(7) 0.028(5) 0.009(5) 0.012(5) 0.014(5) C44 0.032(5) 0.032(5) 0.068(7) 0.028(5) 0.017(5) 0.014(4) C14 0.050(6) 0.038(5) 0.037(6) 0.011(5) 0.011(5) 0.023(5) C17 0.048(6) 0.042(6) 0.055(7) 0.023(5) 0.021(5) 0.027(5) C42 0.046(6) 0.045(6) 0.055(7) 0.027(6) 0.008(5) 0.017(5) C29 0.036(5) 0.041(6) 0.048(6) 0.017(5) 0.018(4) 0.006(4) O3 0.091(7) 0.106(8) 0.063(6) 0.057(6) -0.021(5) -0.032(6) C28 0.035(5) 0.039(6) 0.055(7) 0.014(5) 0.010(5) 0.011(4) C13 0.054(6) 0.064(7) 0.035(6) 0.020(6) 0.003(5) 0.026(6) C41 0.061(7) 0.052(7) 0.037(6) 0.021(5) 0.008(5) 0.027(5) C39 0.044(6) 0.048(6) 0.047(7) 0.026(6) -0.004(5) -0.001(5) C9 0.058(7) 0.071(9) 0.060(8) 0.025(7) 0.017(6) 0.017(6) C21 0.062(7) 0.058(8) 0.051(7) 0.020(6) 0.013(6) 0.013(6) C1 0.053(7) 0.049(7) 0.060(8) 0.006(6) 0.014(6) 0.010(6) C26 0.043(6) 0.060(7) 0.042(6) 0.003(6) 0.000(5) 0.022(5) C8 0.076(8) 0.068(8) 0.027(6) 0.001(6) 0.005(6) 0.023(7) C23 0.052(6) 0.057(7) 0.039(6) -0.008(5) 0.020(5) -0.006(5) C10 0.059(7) 0.059(8) 0.038(6) 0.005(6) 0.017(5) 0.003(6) C4 0.058(7) 0.059(8) 0.066(8) 0.028(7) 0.033(6) 0.020(6) C31 0.051(6) 0.047(6) 0.047(7) 0.011(5) -0.003(5) 0.014(5) C32 0.040(5) 0.050(6) 0.040(6) 0.002(5) 0.000(5) 0.019(5) C27 0.038(6) 0.067(8) 0.065(8) 0.024(7) 0.004(5) 0.024(6) C2 0.057(8) 0.054(8) 0.098(12) 0.019(8) 0.040(8) 0.013(6) C36 0.031(6) 0.089(10) 0.073(9) 0.034(8) 0.004(6) 0.019(6) C20 0.062(8) 0.057(8) 0.070(9) 0.022(7) 0.002(6) 0.023(6) C37 0.075(9) 0.069(9) 0.063(9) 0.028(8) 0.013(7) 0.021(7) C35 0.065(8) 0.057(8) 0.089(11) 0.037(8) -0.009(8) 0.008(7) C38 0.066(8) 0.083(10) 0.099(12) 0.061(10) 0.011(8) 0.007(7) C3 0.077(10) 0.066(9) 0.134(15) 0.054(10) 0.066(10) 0.021(8) C34 0.077(10) 0.069(10) 0.098(12) 0.045(10) 0.007(9) 0.013(8) _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 O12 2.244(6) . ? Cd1 O12 2.244(6) 2_566 ? Cd1 O5 2.309(7) 2_566 ? Cd1 O5 2.309(7) . ? Cd1 O11 2.343(6) . ? Cd1 O11 2.343(6) 2_566 ? Cd2 O8 2.215(7) . ? Cd2 O15 2.238(7) . ? Cd2 O13 2.294(7) . ? Cd2 N2 2.320(8) . ? Cd2 N1 2.351(8) . ? Cd2 O2 2.531(7) . ? Cd3 O13 2.176(6) 2_656 ? Cd3 O14 2.214(6) . ? Cd3 O9 2.236(7) 1_565 ? Cd3 O4 2.239(7) . ? Cd3 O11 2.314(6) . ? Cd3 O5 2.621(7) . ? Cd3 C40 2.749(10) . ? O14 C45 1.224(10) . ? O13 C19 1.294(10) . ? O13 Cd3 2.176(6) 2_656 ? O15 C33 1.216(11) 2_656 ? O5 C40 1.268(11) . ? O12 C45 1.257(10) . ? O1 C11 1.361(11) . ? O1 C18 1.404(11) . ? O11 C33 1.289(12) . ? O10 C25 1.362(12) 1_576 ? O10 C32 1.434(12) . ? O2 C19 1.224(11) . ? O9 C24 1.232(13) . ? O9 Cd3 2.236(7) 1_545 ? C19 C18 1.517(14) . ? O8 C24 1.251(12) . ? N2 C10 1.346(14) . ? N2 C6 1.355(12) . ? C33 O15 1.216(11) 2_656 ? C33 C32 1.507(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C25 O10 1.362(12) 1_534 ? C25 C26 1.390(14) . ? C25 C30 1.433(15) . ? O6 C43 1.368(12) . ? O6 C44 1.405(11) . ? O7 C22 1.339(12) . ? O7 C23 1.449(13) . ? C45 C44 1.542(12) . ? C6 C7 1.412(14) . ? C6 C5 1.487(15) . ? O4 C40 1.268(13) . ? N1 C1 1.318(15) . ? N1 C5 1.354(14) . ? C24 C23 1.512(15) . ? C15 C16 1.404(14) . ? C15 C14 1.407(14) . ? C15 C43 1.423(12) . ? C40 C39 1.492(13) . ? C11 C12 1.362(14) . ? C11 C16 1.410(12) . ? C30 C31 1.397(14) . ? C30 C29 1.427(14) . ? C16 C17 1.447(14) . ? C22 C21 1.363(15) . ? C22 C29 1.420(15) . ? C43 C42 1.349(14) . ? C5 C4 1.354(14) . ? C12 C13 1.372(15) . ? C12 H12 0.9300 . ? C7 C8 1.399(17) . ? C7 H7 0.9300 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C14 C13 1.383(13) . ? C14 H14 0.9300 . ? C17 C41 1.365(14) . ? C17 H17 0.9300 . ? C42 C41 1.373(15) . ? C42 H42 0.9300 . ? C29 C28 1.401(14) . ? O3 C37 1.355(15) . ? O3 C39 1.376(14) . ? C28 C27 1.333(16) . ? C28 H28 0.9300 . ? C13 H13 0.9300 . ? C41 H41 0.9300 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C9 C10 1.362(17) . ? C9 C8 1.409(17) . ? C9 H9 0.9300 . ? C21 C20 1.373(17) . ? C21 H21 0.9300 . ? C1 C2 1.372(17) . ? C1 H1 0.9300 . ? C26 C27 1.401(16) . ? C26 H26 0.9300 . ? C8 H8 0.9300 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C10 H10 0.9300 . ? C4 C3 1.40(2) . ? C4 H4 0.9300 . ? C31 C20 1.392(17) . ? C31 H31 0.9300 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C27 H27 0.9300 . ? C2 C3 1.38(2) . ? C2 H2 0.9300 . ? C36 C37 1.37(2) . ? C36 C36 1.37(3) 2_565 ? C36 C35 1.500(19) . ? C20 H20 0.9300 . ? C37 C38 1.445(19) . ? C35 C34 1.28(2) . ? C35 H35 0.9300 . ? C38 C34 1.42(2) 2_565 ? C38 H38 0.9300 . ? C3 H3 0.9300 . ? C34 C38 1.42(2) 2_565 ? C34 H34 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 O12 Cd1 O12 180.000(1) . 2_566 ? O12 Cd1 O5 87.4(3) . 2_566 ? O12 Cd1 O5 92.6(3) 2_566 2_566 ? O12 Cd1 O5 92.6(3) . . ? O12 Cd1 O5 87.4(3) 2_566 . ? O5 Cd1 O5 180.000(1) 2_566 . ? O12 Cd1 O11 89.6(2) . . ? O12 Cd1 O11 90.4(2) 2_566 . ? O5 Cd1 O11 97.0(2) 2_566 . ? O5 Cd1 O11 83.0(2) . . ? O12 Cd1 O11 90.4(2) . 2_566 ? O12 Cd1 O11 89.6(2) 2_566 2_566 ? O5 Cd1 O11 83.0(2) 2_566 2_566 ? O5 Cd1 O11 97.0(2) . 2_566 ? O11 Cd1 O11 180.000(1) . 2_566 ? O8 Cd2 O15 107.0(3) . . ? O8 Cd2 O13 108.5(3) . . ? O15 Cd2 O13 86.9(2) . . ? O8 Cd2 N2 80.8(3) . . ? O15 Cd2 N2 96.7(3) . . ? O13 Cd2 N2 168.7(3) . . ? O8 Cd2 N1 144.4(3) . . ? O15 Cd2 N1 98.3(3) . . ? O13 Cd2 N1 97.2(3) . . ? N2 Cd2 N1 71.7(3) . . ? O8 Cd2 O2 91.5(3) . . ? O15 Cd2 O2 140.5(2) . . ? O13 Cd2 O2 53.8(2) . . ? N2 Cd2 O2 121.0(3) . . ? N1 Cd2 O2 84.1(3) . . ? O13 Cd3 O14 88.5(3) 2_656 . ? O13 Cd3 O9 94.8(3) 2_656 1_565 ? O14 Cd3 O9 97.1(3) . 1_565 ? O13 Cd3 O4 123.6(3) 2_656 . ? O14 Cd3 O4 147.1(3) . . ? O9 Cd3 O4 87.7(3) 1_565 . ? O13 Cd3 O11 97.1(2) 2_656 . ? O14 Cd3 O11 88.3(2) . . ? O9 Cd3 O11 167.0(3) 1_565 . ? O4 Cd3 O11 81.5(3) . . ? O13 Cd3 O5 173.7(2) 2_656 . ? O14 Cd3 O5 93.5(2) . . ? O9 Cd3 O5 90.8(2) 1_565 . ? O4 Cd3 O5 53.8(3) . . ? O11 Cd3 O5 77.0(2) . . ? O13 Cd3 C40 150.6(3) 2_656 . ? O14 Cd3 C40 120.6(3) . . ? O9 Cd3 C40 85.6(3) 1_565 . ? O4 Cd3 C40 27.1(3) . . ? O11 Cd3 C40 81.5(3) . . ? O5 Cd3 C40 27.2(2) . . ? C45 O14 Cd3 132.0(6) . . ? C19 O13 Cd3 137.8(6) . 2_656 ? C19 O13 Cd2 97.1(5) . . ? Cd3 O13 Cd2 121.4(3) 2_656 . ? C33 O15 Cd2 135.4(7) 2_656 . ? C40 O5 Cd1 122.5(7) . . ? C40 O5 Cd3 82.0(6) . . ? Cd1 O5 Cd3 90.0(2) . . ? C45 O12 Cd1 131.7(6) . . ? C11 O1 C18 117.5(8) . . ? C33 O11 Cd3 120.1(6) . . ? C33 O11 Cd1 136.2(6) . . ? Cd3 O11 Cd1 97.2(2) . . ? C25 O10 C32 118.1(8) 1_576 . ? C19 O2 Cd2 87.8(5) . . ? C24 O9 Cd3 127.9(6) . 1_545 ? O2 C19 O13 121.2(9) . . ? O2 C19 C18 123.8(8) . . ? O13 C19 C18 114.9(8) . . ? C24 O8 Cd2 121.1(8) . . ? C10 N2 C6 120.6(9) . . ? C10 N2 Cd2 123.1(7) . . ? C6 N2 Cd2 116.3(7) . . ? O15 C33 O11 125.0(9) 2_656 . ? O15 C33 C32 121.1(9) 2_656 . ? O11 C33 C32 113.7(8) . . ? O1 C18 C19 109.0(8) . . ? O1 C18 H18A 109.9 . . ? C19 C18 H18A 109.9 . . ? O1 C18 H18B 109.9 . . ? C19 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? O10 C25 C26 123.4(10) 1_534 . ? O10 C25 C30 116.3(9) 1_534 . ? C26 C25 C30 120.3(9) . . ? C43 O6 C44 119.0(8) . . ? C22 O7 C23 117.0(9) . . ? O14 C45 O12 128.1(8) . . ? O14 C45 C44 118.3(7) . . ? O12 C45 C44 113.6(7) . . ? N2 C6 C7 118.5(10) . . ? N2 C6 C5 118.8(9) . . ? C7 C6 C5 122.7(9) . . ? C40 O4 Cd3 99.5(6) . . ? C1 N1 C5 119.3(10) . . ? C1 N1 Cd2 123.9(8) . . ? C5 N1 Cd2 116.6(7) . . ? O9 C24 O8 125.9(10) . . ? O9 C24 C23 116.9(9) . . ? O8 C24 C23 117.2(11) . . ? C16 C15 C14 118.2(8) . . ? C16 C15 C43 119.5(9) . . ? C14 C15 C43 122.2(9) . . ? O4 C40 O5 122.7(9) . . ? O4 C40 C39 115.2(8) . . ? O5 C40 C39 122.1(10) . . ? O4 C40 Cd3 53.5(5) . . ? O5 C40 Cd3 70.8(6) . . ? C39 C40 Cd3 163.3(7) . . ? O1 C11 C12 126.0(8) . . ? O1 C11 C16 114.7(8) . . ? C12 C11 C16 119.3(9) . . ? C31 C30 C29 120.0(10) . . ? C31 C30 C25 121.4(9) . . ? C29 C30 C25 118.5(9) . . ? C15 C16 C11 121.0(9) . . ? C15 C16 C17 118.8(8) . . ? C11 C16 C17 120.2(9) . . ? O7 C22 C21 126.2(10) . . ? O7 C22 C29 113.5(9) . . ? C21 C22 C29 120.2(10) . . ? C42 C43 O6 126.0(8) . . ? C42 C43 C15 119.7(9) . . ? O6 C43 C15 114.3(9) . . ? N1 C5 C4 120.6(11) . . ? N1 C5 C6 116.1(9) . . ? C4 C5 C6 123.3(10) . . ? C11 C12 C13 120.1(9) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C7 C6 121.4(11) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? O6 C44 C45 114.5(7) . . ? O6 C44 H44A 108.6 . . ? C45 C44 H44A 108.6 . . ? O6 C44 H44B 108.6 . . ? C45 C44 H44B 108.6 . . ? H44A C44 H44B 107.6 . . ? C13 C14 C15 118.9(9) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C41 C17 C16 118.4(9) . . ? C41 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C43 C42 C41 121.5(9) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C28 C29 C22 122.7(10) . . ? C28 C29 C30 119.4(10) . . ? C22 C29 C30 118.0(9) . . ? C37 O3 C39 121.0(10) . . ? C27 C28 C29 119.7(10) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C12 C13 C14 122.4(10) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C17 C41 C42 122.1(10) . . ? C17 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? O3 C39 C40 109.9(9) . . ? O3 C39 H39A 109.7 . . ? C40 C39 H39A 109.7 . . ? O3 C39 H39B 109.7 . . ? C40 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C10 C9 C8 119.4(13) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C22 C21 C20 121.8(12) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? N1 C1 C2 123.9(13) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C25 C26 C27 117.6(11) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C7 C8 C9 117.1(11) . . ? C7 C8 H8 121.5 . . ? C9 C8 H8 121.5 . . ? O7 C23 C24 115.5(9) . . ? O7 C23 H23A 108.4 . . ? C24 C23 H23A 108.4 . . ? O7 C23 H23B 108.4 . . ? C24 C23 H23B 108.4 . . ? H23A C23 H23B 107.5 . . ? N2 C10 C9 122.9(11) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C5 C4 C3 119.6(13) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C20 C31 C30 119.8(11) . . ? C20 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? O10 C32 C33 107.7(8) . . ? O10 C32 H32A 110.2 . . ? C33 C32 H32A 110.2 . . ? O10 C32 H32B 110.2 . . ? C33 C32 H32B 110.2 . . ? H32A C32 H32B 108.5 . . ? C28 C27 C26 124.2(10) . . ? C28 C27 H27 117.9 . . ? C26 C27 H27 117.9 . . ? C1 C2 C3 117.0(14) . . ? C1 C2 H2 121.5 . . ? C3 C2 H2 121.5 . . ? C37 C36 C36 123.0(17) . 2_565 ? C37 C36 C35 117.1(12) . . ? C36 C36 C35 119.8(18) 2_565 . ? C21 C20 C31 120.2(12) . . ? C21 C20 H20 119.9 . . ? C31 C20 H20 119.9 . . ? O3 C37 C36 121.2(12) . . ? O3 C37 C38 121.1(13) . . ? C36 C37 C38 117.6(13) . . ? C34 C35 C36 115.4(14) . . ? C34 C35 H35 122.3 . . ? C36 C35 H35 122.3 . . ? C34 C38 C37 117.4(15) 2_565 . ? C34 C38 H38 121.3 2_565 . ? C37 C38 H38 121.3 . . ? C2 C3 C4 119.5(12) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C35 C34 C38 126.7(14) . 2_565 ? C35 C34 H34 116.6 . . ? C38 C34 H34 116.6 2_565 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.143 _refine_diff_density_min -2.165 _refine_diff_density_rms 0.279