# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email zhangjp7@mail.sysu.edu.cn _publ_contact_author_name 'Jie-Peng Zhang' loop_ _publ_author_name 'Xiao-Feng Wang' 'Yu Wang' 'Yue-Biao Zhang' 'Wei Xue' 'Jie-Peng Zhang' 'Xiao-Ming Chen' data_1 _database_code_depnum_ccdc_archive 'CCDC 840366' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H48 Cd2 N8 O18' _chemical_formula_weight 1081.60 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 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 11.4413(2) _cell_length_b 14.2690(2) _cell_length_c 14.9766(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.696(2) _cell_angle_gamma 90.00 _cell_volume 2184.39(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6591 _exptl_absorpt_correction_T_max 0.7776 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Germioni S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24650 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4295 _reflns_number_gt 3186 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^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 4295 _refine_ls_number_parameters 265 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.86814(3) 0.100379(19) -0.44048(2) 0.02149(14) Uani 1 1 d . . . O1 O -0.7241(3) 0.2351(2) -0.3833(2) 0.0353(8) Uani 1 1 d . . . O2 O -0.6405(3) 0.09501(19) -0.3357(3) 0.0349(8) Uani 1 1 d . . . O3 O -0.1180(3) 0.4418(2) -0.0751(2) 0.0418(9) Uani 1 1 d . . . O4 O -0.0423(3) 0.3022(2) -0.0152(2) 0.0358(7) Uani 1 1 d . . . O5 O -0.4860(4) 0.0560(3) -0.1335(3) 0.0592(11) Uani 1 1 d . . . O6 O -0.3443(4) 0.0220(3) -0.1878(3) 0.0666(12) Uani 1 1 d . . . O7 O -0.9010(3) 0.1113(2) -0.3007(2) 0.0384(8) Uani 1 1 d . . . O8 O -0.8337(4) 0.0902(2) -0.5763(3) 0.0466(9) Uani 1 1 d . . . N1 N -0.4131(4) 0.0776(3) -0.1704(3) 0.0454(11) Uani 1 1 d . . . N2 N -0.8235(6) 0.1017(3) -0.1329(3) 0.0527(13) Uani 1 1 d . . . N3 N -0.8700(5) 0.1099(3) -0.7355(3) 0.0501(12) Uani 1 1 d . . . C1 C -0.5038(4) 0.2266(3) -0.2620(3) 0.0236(9) Uani 1 1 d . . . C2 C -0.4001(4) 0.1767(3) -0.1896(3) 0.0275(9) Uani 1 1 d . . . C3 C -0.2806(4) 0.2165(3) -0.1279(3) 0.0271(9) Uani 1 1 d . . . H3A H -0.2117 0.1793 -0.0808 0.033 Uiso 1 1 calc R . . C4 C -0.2631(4) 0.3122(3) -0.1361(3) 0.0219(8) Uani 1 1 d . . . C5 C -0.3649(4) 0.3644(3) -0.2052(3) 0.0266(9) Uani 1 1 d . . . H5A H -0.3543 0.4298 -0.2105 0.032 Uiso 1 1 calc R . . C6 C -0.4831(4) 0.3217(3) -0.2674(3) 0.0250(9) Uani 1 1 d . . . H6A H -0.5517 0.3589 -0.3149 0.030 Uiso 1 1 calc R . . C7 C -0.6320(4) 0.1832(3) -0.3319(3) 0.0245(9) Uani 1 1 d . . . C8 C -0.1319(4) 0.3556(3) -0.0707(3) 0.0231(9) Uani 1 1 d . . . C9 C -0.8214(5) 0.0834(3) -0.2177(4) 0.0383(12) Uani 1 1 d . . . H9A H -0.7520 0.0452 -0.2151 0.046 Uiso 1 1 calc R . . C10 C -0.9261(9) 0.1597(5) -0.1290(5) 0.102(3) Uani 1 1 d . . . H10A H -0.9622 0.2013 -0.1872 0.152 Uiso 1 1 calc R . . H10B H -0.8893 0.1973 -0.0677 0.152 Uiso 1 1 calc R . . H10C H -0.9957 0.1194 -0.1294 0.152 Uiso 1 1 calc R . . C11 C -0.7257(7) 0.0631(5) -0.0394(4) 0.084(2) Uani 1 1 d U . . H11A H -0.6795 0.0117 -0.0533 0.126 Uiso 1 1 calc R . . H11B H -0.7685 0.0394 -0.0001 0.126 Uiso 1 1 calc R . . H11C H -0.6630 0.1122 -0.0016 0.126 Uiso 1 1 calc R . . C12 C -0.9083(5) 0.0899(3) -0.6678(4) 0.0395(12) Uani 1 1 d . . . H12A H -0.9977 0.0743 -0.6893 0.047 Uiso 1 1 calc R . . C13 C -0.7365(7) 0.1413(6) -0.7031(6) 0.091(2) Uani 1 1 d U . . H13A H -0.7157 0.1905 -0.6525 0.137 Uiso 1 1 calc R . . H13B H -0.7270 0.1662 -0.7604 0.137 Uiso 1 1 calc R . . H13C H -0.6765 0.0883 -0.6743 0.137 Uiso 1 1 calc R . . C14 C -0.9508(8) 0.1110(5) -0.8394(5) 0.083(2) Uani 1 1 d U . . H14A H -1.0427 0.1101 -0.8525 0.124 Uiso 1 1 calc R . . H14B H -0.9323 0.0558 -0.8698 0.124 Uiso 1 1 calc R . . H14C H -0.9335 0.1679 -0.8682 0.124 Uiso 1 1 calc R . . N4 N -0.3361(7) 0.2927(6) 0.0784(5) 0.1236(15) Uiso 0.601(8) 1 d PD A 1 O9 O -0.2522(6) 0.1463(5) 0.1218(5) 0.1236(15) Uiso 0.601(8) 1 d PD A 1 C16 C -0.4651(11) 0.2563(10) 0.0118(9) 0.1236(15) Uiso 0.601(8) 1 d PD A 1 H16A H -0.4669 0.1885 0.0215 0.185 Uiso 0.601(8) 1 calc PR A 1 H16B H -0.4841 0.2692 -0.0577 0.185 Uiso 0.601(8) 1 calc PR A 1 H16C H -0.5310 0.2867 0.0268 0.185 Uiso 0.601(8) 1 calc PR A 1 C15 C -0.2339(12) 0.2332(10) 0.1310(8) 0.1236(15) Uiso 0.601(8) 1 d PD A 1 H15A H -0.1500 0.2575 0.1741 0.148 Uiso 0.601(8) 1 calc PR A 1 C17 C -0.3286(18) 0.3908(8) 0.0817(11) 0.1236(15) Uiso 0.601(8) 1 d PD A 1 H17A H -0.2396 0.4101 0.1281 0.185 Uiso 0.601(8) 1 calc PR A 1 H17B H -0.3904 0.4158 0.1045 0.185 Uiso 0.601(8) 1 calc PR A 1 H17C H -0.3506 0.4151 0.0148 0.185 Uiso 0.601(8) 1 calc PR A 1 N4' N -0.3361(7) 0.2927(6) 0.0784(5) 0.1236(15) Uiso 0.399(8) 1 d PD A 2 O9' O -0.2522(6) 0.1463(5) 0.1218(5) 0.1236(15) Uiso 0.399(8) 1 d PD A 2 C15' C -0.3487(17) 0.1966(10) 0.0718(10) 0.1236(15) Uiso 0.399(8) 1 d PD A 2 H15B H -0.4305 0.1688 0.0293 0.148 Uiso 0.399(8) 1 calc PR A 2 C16' C -0.2169(16) 0.3398(11) 0.1406(15) 0.1236(15) Uiso 0.399(8) 1 d PD A 2 H16D H -0.2308 0.4077 0.1332 0.185 Uiso 0.399(8) 1 calc PR A 2 H16E H -0.1491 0.3219 0.1209 0.185 Uiso 0.399(8) 1 calc PR A 2 H16F H -0.1891 0.3222 0.2105 0.185 Uiso 0.399(8) 1 calc PR A 2 C17' C -0.4473(17) 0.3492(14) 0.0208(12) 0.1236(15) Uiso 0.399(8) 1 d PD A 2 H17D H -0.4231 0.4156 0.0330 0.185 Uiso 0.399(8) 1 calc PR A 2 H17E H -0.5168 0.3358 0.0401 0.185 Uiso 0.399(8) 1 calc PR A 2 H17F H -0.4785 0.3352 -0.0503 0.185 Uiso 0.399(8) 1 calc PR A 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 Cd1 0.01389(19) 0.01888(19) 0.0239(2) 0.00082(12) 0.00153(13) -0.00065(11) O1 0.0175(15) 0.0289(17) 0.0442(18) -0.0015(14) 0.0003(14) -0.0022(13) O2 0.0228(17) 0.0206(17) 0.043(2) -0.0003(13) -0.0019(14) -0.0045(12) O3 0.0256(18) 0.0241(18) 0.066(2) -0.0120(16) 0.0116(17) -0.0092(14) O4 0.0176(15) 0.0321(17) 0.0401(18) 0.0040(14) -0.0027(13) -0.0027(13) O5 0.051(2) 0.054(2) 0.059(2) 0.018(2) 0.012(2) -0.014(2) O6 0.060(3) 0.032(2) 0.094(3) 0.002(2) 0.022(2) 0.0066(19) O7 0.039(2) 0.046(2) 0.0297(18) 0.0016(14) 0.0148(16) 0.0037(15) O8 0.035(2) 0.073(3) 0.0301(19) -0.0042(16) 0.0132(16) 0.0019(17) N1 0.031(2) 0.038(3) 0.047(3) 0.007(2) 0.000(2) -0.006(2) N2 0.081(4) 0.039(3) 0.030(2) 0.0024(19) 0.018(2) -0.004(2) N3 0.055(3) 0.060(3) 0.043(3) 0.003(2) 0.029(2) -0.003(2) C1 0.020(2) 0.024(2) 0.022(2) -0.0029(17) 0.0050(17) -0.0041(17) C2 0.025(2) 0.021(2) 0.027(2) 0.0020(18) 0.0031(18) -0.0035(18) C3 0.019(2) 0.022(2) 0.030(2) 0.0004(18) 0.0014(17) -0.0030(17) C4 0.0187(19) 0.020(2) 0.024(2) -0.0041(16) 0.0074(16) -0.0022(16) C5 0.024(2) 0.0147(19) 0.036(2) 0.0002(18) 0.0089(19) -0.0069(17) C6 0.020(2) 0.023(2) 0.026(2) 0.0017(17) 0.0056(17) 0.0040(17) C7 0.019(2) 0.028(3) 0.024(2) 0.0015(18) 0.0073(17) -0.0012(18) C8 0.020(2) 0.021(2) 0.028(2) -0.0065(17) 0.0098(18) -0.0055(17) C9 0.041(3) 0.039(3) 0.033(3) -0.003(2) 0.015(2) -0.006(2) C10 0.187(9) 0.068(5) 0.076(5) 0.008(4) 0.083(6) 0.046(5) C11 0.100(5) 0.095(5) 0.039(3) 0.008(3) 0.015(3) -0.022(4) C12 0.035(3) 0.043(3) 0.042(3) 0.000(2) 0.018(2) -0.008(2) C13 0.080(5) 0.122(6) 0.097(5) 0.005(4) 0.063(4) -0.018(4) C14 0.097(5) 0.102(5) 0.054(4) -0.001(3) 0.039(4) -0.012(4) _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 2.243(3) . ? Cd1 O4 2.270(3) 4_465 ? Cd1 O3 2.288(3) 2_444 ? Cd1 O7 2.293(3) . ? Cd1 O2 2.362(3) . ? Cd1 O1 2.424(3) . ? Cd1 C7 2.719(4) . ? O1 C7 1.234(5) . ? O2 C7 1.261(5) . ? O3 C8 1.246(6) . ? O3 Cd1 2.288(3) 2_454 ? O4 C8 1.248(5) . ? O4 Cd1 2.270(3) 4_666 ? O5 N1 1.229(6) . ? O6 N1 1.226(6) . ? O7 C9 1.231(6) . ? O8 C12 1.248(6) . ? N1 C2 1.463(6) . ? N2 C9 1.307(7) . ? N2 C11 1.452(8) . ? N2 C10 1.459(8) . ? N3 C12 1.305(7) . ? N3 C14 1.408(8) . ? N3 C13 1.450(8) . ? C1 C6 1.386(6) . ? C1 C2 1.391(6) . ? C1 C7 1.501(5) . ? C2 C3 1.382(6) . ? C3 C4 1.394(5) . ? C3 H3A 0.9500 . ? C4 C5 1.378(6) . ? C4 C8 1.508(5) . ? C5 C6 1.390(6) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C9 H9A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N4 C15 1.372(11) . ? N4 C17 1.402(11) . ? N4 C16 1.456(11) . ? O9 C15 1.254(13) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 H15A 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C15' H15B 0.9500 . ? C16' H16D 0.9800 . ? C16' H16E 0.9800 . ? C16' H16F 0.9800 . ? C17' H17D 0.9800 . ? C17' H17E 0.9800 . ? C17' H17F 0.9800 . ? 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 O4 93.77(13) . 4_465 ? O8 Cd1 O3 94.39(13) . 2_444 ? O4 Cd1 O3 124.78(11) 4_465 2_444 ? O8 Cd1 O7 179.38(11) . . ? O4 Cd1 O7 86.61(12) 4_465 . ? O3 Cd1 O7 85.79(12) 2_444 . ? O8 Cd1 O2 90.55(13) . . ? O4 Cd1 O2 144.00(10) 4_465 . ? O3 Cd1 O2 90.38(10) 2_444 . ? O7 Cd1 O2 88.85(13) . . ? O8 Cd1 O1 90.20(12) . . ? O4 Cd1 O1 89.72(10) 4_465 . ? O3 Cd1 O1 144.66(10) 2_444 . ? O7 Cd1 O1 89.31(11) . . ? O2 Cd1 O1 54.50(9) . . ? O8 Cd1 C7 92.18(13) . . ? O4 Cd1 C7 116.42(12) 4_465 . ? O3 Cd1 C7 117.69(11) 2_444 . ? O7 Cd1 C7 87.21(12) . . ? O2 Cd1 C7 27.61(11) . . ? O1 Cd1 C7 27.00(11) . . ? C7 O1 Cd1 89.9(2) . . ? C7 O2 Cd1 92.2(2) . . ? C8 O3 Cd1 162.7(3) . 2_454 ? C8 O4 Cd1 103.4(3) . 4_666 ? C9 O7 Cd1 123.3(3) . . ? C12 O8 Cd1 133.1(3) . . ? O6 N1 O5 124.3(5) . . ? O6 N1 C2 116.8(5) . . ? O5 N1 C2 118.8(5) . . ? C9 N2 C11 121.3(6) . . ? C9 N2 C10 121.2(5) . . ? C11 N2 C10 117.5(5) . . ? C12 N3 C14 125.3(6) . . ? C12 N3 C13 118.6(5) . . ? C14 N3 C13 115.9(5) . . ? C6 C1 C2 116.0(4) . . ? C6 C1 C7 120.2(4) . . ? C2 C1 C7 123.8(4) . . ? C3 C2 C1 123.5(4) . . ? C3 C2 N1 115.0(4) . . ? C1 C2 N1 121.4(4) . . ? C2 C3 C4 118.8(4) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 C8 121.7(4) . . ? C3 C4 C8 119.0(4) . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 122.0(4) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? O1 C7 O2 122.9(4) . . ? O1 C7 C1 118.7(4) . . ? O2 C7 C1 118.4(4) . . ? O1 C7 Cd1 63.1(2) . . ? O2 C7 Cd1 60.2(2) . . ? C1 C7 Cd1 173.6(3) . . ? O3 C8 O4 123.4(4) . . ? O3 C8 C4 119.0(4) . . ? O4 C8 C4 117.5(4) . . ? O7 C9 N2 126.0(5) . . ? O7 C9 H9A 117.0 . . ? N2 C9 H9A 117.0 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O8 C12 N3 123.4(5) . . ? O8 C12 H12A 118.3 . . ? N3 C12 H12A 118.3 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 N4 C17 125.1(11) . . ? C15 N4 C16 120.8(10) . . ? C17 N4 C16 114.1(10) . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O9 C15 N4 119.5(11) . . ? O9 C15 H15A 120.3 . . ? N4 C15 H15A 120.3 . . ? N4 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? H16D C16' H16E 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? H17D C17' H17E 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.333 _refine_diff_density_min -1.042 _refine_diff_density_rms 0.112 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 840367' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33.50 H41.50 Cd2 N8.50 O16.50' _chemical_formula_weight 1052.05 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' 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 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 17.3378(3) _cell_length_b 14.2386(2) _cell_length_c 20.9358(6) _cell_angle_alpha 90.00 _cell_angle_beta 121.841(2) _cell_angle_gamma 90.00 _cell_volume 4390.58(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6733 _exptl_absorpt_correction_T_max 0.8839 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Germioni S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29401 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8301 _reflns_number_gt 5510 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1134P)^2^+1.2877P] 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 8301 _refine_ls_number_parameters 505 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.124 _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 Cd2 Cd -0.24858(3) -0.10414(3) 0.16700(2) 0.02307(17) Uani 1 1 d . . . Cd1 Cd -0.24512(4) -0.59996(3) 0.54340(3) 0.02403(17) Uani 1 1 d . . . O1 O -0.2422(4) -0.7342(3) 0.4758(3) 0.0500(14) Uani 1 1 d U . . O2 O -0.2586(5) -0.5971(3) 0.4270(3) 0.0514(15) Uani 1 1 d U . . O3 O -0.2483(4) -0.9419(3) 0.1688(3) 0.0388(13) Uani 1 1 d . . . O4 O -0.2441(4) -0.8008(3) 0.1291(2) 0.0326(12) Uani 1 1 d . . . O6 O -0.2051(13) -0.5336(11) 0.3209(10) 0.217(7) Uiso 1 1 d . . . O5 O -0.3503(12) -0.5429(10) 0.2706(8) 0.193(6) Uiso 1 1 d . . . O7 O -0.2607(4) -0.2420(3) 0.2308(3) 0.0484(14) Uani 1 1 d U . . O8 O -0.2602(4) -0.1013(3) 0.2731(3) 0.0352(12) Uani 1 1 d U . . O9 O -0.2605(3) -0.4378(3) 0.5410(3) 0.0313(11) Uani 1 1 d U . . O10 O -0.2443(4) -0.2941(3) 0.5852(2) 0.0315(11) Uani 1 1 d . . . O11 O -0.1368(7) -0.0600(5) 0.4251(4) 0.093(3) Uani 1 1 d . . . O12 O -0.2634(7) -0.0242(5) 0.4136(5) 0.098(3) Uani 1 1 d . . . O13 O -0.0956(4) -0.1055(3) 0.2394(3) 0.0431(13) Uani 1 1 d . . . O14 O -0.0943(4) -0.5841(4) 0.6103(4) 0.0570(16) Uani 1 1 d . . . N1 N -0.2735(11) -0.5684(9) 0.2894(8) 0.114(4) Uiso 1 1 d . . . N2 N -0.2119(8) -0.0792(5) 0.4152(5) 0.071(3) Uani 1 1 d . . . N3 N -0.5931(4) -0.5984(3) 0.4053(3) 0.0275(13) Uani 1 1 d . . . N4 N -0.4046(4) -0.5976(3) 0.4824(3) 0.0283(13) Uani 1 1 d . . . N5 N 0.0300(6) -0.0983(5) 0.3550(4) 0.062(2) Uani 1 1 d D . . N6 N 0.0427(6) -0.6121(6) 0.7108(6) 0.078(3) Uani 1 1 d . . . C1 C -0.2530(5) -0.7272(4) 0.3583(4) 0.0267(15) Uani 1 1 d . . . C2 C -0.2601(6) -0.6746(4) 0.3004(4) 0.0334(18) Uani 1 1 d . . . C3 C -0.2606(6) -0.7153(4) 0.2403(4) 0.0355(18) Uani 1 1 d . . . H3A H -0.2665 -0.6773 0.2007 0.043 Uiso 1 1 calc R . . C4 C -0.2523(5) -0.8121(4) 0.2381(4) 0.0254(14) Uani 1 1 d . . . C5 C -0.2462(5) -0.8677(4) 0.2949(4) 0.0291(16) Uani 1 1 d . . . H5A H -0.2413 -0.9341 0.2936 0.035 Uiso 1 1 calc R . . C6 C -0.2475(5) -0.8238(4) 0.3540(4) 0.0325(17) Uani 1 1 d . . . H6A H -0.2444 -0.8616 0.3927 0.039 Uiso 1 1 calc R . . C7 C -0.2516(5) -0.6832(4) 0.4251(4) 0.0283(15) Uani 1 1 d . . . C8 C -0.2486(5) -0.8546(4) 0.1743(4) 0.0251(15) Uani 1 1 d . . . C9 C -0.2561(5) -0.2314(4) 0.3449(4) 0.0321(17) Uani 1 1 d . . . C10 C -0.2395(6) -0.1787(4) 0.4065(4) 0.0371(17) Uani 1 1 d U . . C11 C -0.2380(6) -0.2159(4) 0.4684(4) 0.042(2) Uani 1 1 d . . . H11A H -0.2267 -0.1770 0.5093 0.050 Uiso 1 1 calc R . . C12 C -0.2533(5) -0.3116(4) 0.4690(3) 0.0246(14) Uani 1 1 d . . . C13 C -0.2694(5) -0.3672(4) 0.4085(4) 0.0284(16) Uani 1 1 d . . . H13A H -0.2793 -0.4327 0.4090 0.034 Uiso 1 1 calc R . . C14 C -0.2709(5) -0.3272(4) 0.3477(4) 0.0331(17) Uani 1 1 d . . . H14A H -0.2824 -0.3660 0.3067 0.040 Uiso 1 1 calc R . . C15 C -0.2588(5) -0.1891(4) 0.2784(4) 0.0289(16) Uani 1 1 d . . . C16 C -0.2515(5) -0.3515(4) 0.5369(4) 0.0241(15) Uani 1 1 d . . . C17 C -0.5477(5) -0.5346(4) 0.3912(4) 0.0351(18) Uani 1 1 d . . . H17A H -0.5807 -0.4889 0.3532 0.042 Uiso 1 1 calc R . . C18 C -0.4533(5) -0.5332(4) 0.4307(4) 0.0335(17) Uani 1 1 d . . . H18A H -0.4231 -0.4854 0.4205 0.040 Uiso 1 1 calc R . . C19 C -0.4506(5) -0.6617(4) 0.4967(4) 0.0362(17) Uani 1 1 d . . . H19A H -0.4181 -0.7081 0.5341 0.043 Uiso 1 1 calc R . . C20 C -0.5433(6) -0.6613(5) 0.4582(4) 0.0387(19) Uani 1 1 d . . . H20A H -0.5734 -0.7079 0.4697 0.046 Uiso 1 1 calc R . . C21 C -0.0542(6) -0.0789(5) 0.3044(5) 0.0441(19) Uani 1 1 d . A . H21A H -0.0863 -0.0402 0.3197 0.053 Uiso 1 1 calc R . . C24 C -0.0399(7) -0.5938(6) 0.6788(6) 0.055(2) Uani 1 1 d . B . H24A H -0.0637 -0.5865 0.7103 0.066 Uiso 1 1 calc R . . C22 C 0.0869(9) -0.1527(11) 0.3384(10) 0.116(7) Uani 0.925(16) 1 d P A 1 H22A H 0.0507 -0.1767 0.2868 0.173 Uiso 0.925(16) 1 calc PR A 1 H22B H 0.1128 -0.2054 0.3736 0.173 Uiso 0.925(16) 1 calc PR A 1 H22C H 0.1360 -0.1130 0.3433 0.173 Uiso 0.925(16) 1 calc PR A 1 C23 C 0.0782(9) -0.0591(10) 0.4312(6) 0.089(4) Uani 0.925(16) 1 d PD A 1 H23A H 0.0577 -0.0906 0.4613 0.134 Uiso 0.925(16) 1 calc PR A 1 H23B H 0.0655 0.0083 0.4288 0.134 Uiso 0.925(16) 1 calc PR A 1 H23C H 0.1436 -0.0688 0.4544 0.134 Uiso 0.925(16) 1 calc PR A 1 C22' C 0.056(13) -0.194(6) 0.351(15) 0.116(7) Uani 0.075(16) 1 d PD A 2 H22D H 0.0209 -0.2154 0.2984 0.173 Uiso 0.075(16) 1 calc PR A 2 H22E H 0.0430 -0.2349 0.3817 0.173 Uiso 0.075(16) 1 calc PR A 2 H22F H 0.1208 -0.1962 0.3692 0.173 Uiso 0.075(16) 1 calc PR A 2 C23' C 0.090(9) -0.017(7) 0.380(8) 0.089(4) Uani 0.075(16) 1 d PD A 2 H23D H 0.0970 0.0047 0.3388 0.134 Uiso 0.075(16) 1 calc PR A 2 H23E H 0.1490 -0.0338 0.4233 0.134 Uiso 0.075(16) 1 calc PR A 2 H23F H 0.0630 0.0338 0.3937 0.134 Uiso 0.075(16) 1 calc PR A 2 C25 C 0.083(3) -0.565(3) 0.673(2) 0.107(6) Uiso 0.345(16) 1 d P B 3 H25A H 0.0405 -0.5676 0.6187 0.160 Uiso 0.345(16) 1 calc PR B 3 H25B H 0.1397 -0.5963 0.6865 0.160 Uiso 0.345(16) 1 calc PR B 3 H25C H 0.0952 -0.4992 0.6895 0.160 Uiso 0.345(16) 1 calc PR B 3 C26 C 0.086(3) -0.621(2) 0.804(2) 0.078(10) Uiso 0.345(16) 1 d P B 3 H26A H 0.0391 -0.6461 0.8125 0.117 Uiso 0.345(16) 1 calc PR B 3 H26B H 0.1048 -0.5589 0.8274 0.117 Uiso 0.345(16) 1 calc PR B 3 H26C H 0.1381 -0.6635 0.8266 0.117 Uiso 0.345(16) 1 calc PR B 3 C25' C 0.0775(15) -0.6459(16) 0.6595(12) 0.107(6) Uiso 0.655(16) 1 d P B 4 H25D H 0.0365 -0.6232 0.6081 0.160 Uiso 0.655(16) 1 calc PR B 4 H25E H 0.0793 -0.7147 0.6594 0.160 Uiso 0.655(16) 1 calc PR B 4 H25F H 0.1387 -0.6210 0.6787 0.160 Uiso 0.655(16) 1 calc PR B 4 C26' C 0.1100(14) -0.6143(12) 0.7850(11) 0.076(5) Uiso 0.655(16) 1 d P B 4 H26D H 0.1692 -0.6093 0.7897 0.114 Uiso 0.655(16) 1 calc PR B 4 H26E H 0.1069 -0.6735 0.8073 0.114 Uiso 0.655(16) 1 calc PR B 4 H26F H 0.1024 -0.5616 0.8113 0.114 Uiso 0.655(16) 1 calc PR B 4 O16 O -0.4989(7) -0.3319(6) -0.6367(6) 0.119(3) Uiso 0.568(17) 1 d PD C 5 N8 N -0.5070(8) -0.2892(8) -0.7430(6) 0.134(4) Uiso 0.568(17) 1 d PD C 5 C30 C -0.4989(8) -0.2738(8) -0.6785(6) 0.034(4) Uiso 0.568(17) 1 d PD C 5 H30B H -0.4923 -0.2101 -0.6627 0.041 Uiso 0.568(17) 1 calc PR C 5 C31 C -0.5171(16) -0.3901(9) -0.7671(10) 0.097(8) Uiso 0.568(17) 1 d PD C 5 H31A H -0.5174 -0.4301 -0.7292 0.145 Uiso 0.568(17) 1 calc PR C 5 H31B H -0.4662 -0.4079 -0.7725 0.145 Uiso 0.568(17) 1 calc PR C 5 H31C H -0.5743 -0.3981 -0.8154 0.145 Uiso 0.568(17) 1 calc PR C 5 C32 C -0.5063(15) -0.2203(11) -0.7906(10) 0.088(7) Uiso 0.568(17) 1 d PD C 5 H32A H -0.5002 -0.1581 -0.7684 0.132 Uiso 0.568(17) 1 calc PR C 5 H32B H -0.5632 -0.2232 -0.8397 0.132 Uiso 0.568(17) 1 calc PR C 5 H32C H -0.4550 -0.2314 -0.7971 0.132 Uiso 0.568(17) 1 calc PR C 5 O16' O -0.4989(7) -0.3319(6) -0.6367(6) 0.119(3) Uiso 0.432(17) 1 d PD C 6 N8' N -0.5070(8) -0.2892(8) -0.7430(6) 0.134(4) Uiso 0.432(17) 1 d PD C 6 C30' C -0.5080(18) -0.3552(14) -0.6963(12) 0.120(13) Uiso 0.432(17) 1 d PD C 6 H30A H -0.5159 -0.4196 -0.7102 0.144 Uiso 0.432(17) 1 calc PR C 6 C31' C -0.490(3) -0.1897(13) -0.7207(18) 0.19(2) Uiso 0.432(17) 1 d PD C 6 H31D H -0.4933 -0.1800 -0.6760 0.283 Uiso 0.432(17) 1 calc PR C 6 H31E H -0.5353 -0.1506 -0.7619 0.283 Uiso 0.432(17) 1 calc PR C 6 H31F H -0.4290 -0.1723 -0.7093 0.283 Uiso 0.432(17) 1 calc PR C 6 C32' C -0.517(3) -0.317(2) -0.8124(15) 0.23(3) Uiso 0.432(17) 1 d PD C 6 H32D H -0.5221 -0.3851 -0.8173 0.340 Uiso 0.432(17) 1 calc PR C 6 H32E H -0.4636 -0.2960 -0.8135 0.340 Uiso 0.432(17) 1 calc PR C 6 H32F H -0.5716 -0.2876 -0.8542 0.340 Uiso 0.432(17) 1 calc PR C 6 N7 N -0.0029(6) -0.7781(10) -0.0851(8) 0.158(5) Uiso 0.55(2) 1 d PD D 7 O15 O -0.0150(9) -0.6461(12) -0.1444(9) 0.207(6) Uiso 0.55(2) 1 d PD D 7 C27 C -0.0161(9) -0.6815(12) -0.0909(10) 0.082(7) Uiso 0.55(2) 1 d PD D 7 H27A H -0.0251 -0.6459 -0.0570 0.098 Uiso 0.55(2) 1 calc PR D 7 C28 C 0.0116(17) -0.8446(16) -0.1286(13) 0.123(11) Uiso 0.55(2) 1 d PD D 7 H28A H 0.0140 -0.8118 -0.1687 0.184 Uiso 0.55(2) 1 calc PR D 7 H28B H -0.0383 -0.8901 -0.1509 0.184 Uiso 0.55(2) 1 calc PR D 7 H28C H 0.0691 -0.8775 -0.0962 0.184 Uiso 0.55(2) 1 calc PR D 7 C29 C -0.0061(15) -0.807(2) -0.0216(11) 0.139(12) Uiso 0.55(2) 1 d PD D 7 H29A H -0.0180 -0.7524 0.0004 0.208 Uiso 0.55(2) 1 calc PR D 7 H29B H 0.0523 -0.8350 0.0158 0.208 Uiso 0.55(2) 1 calc PR D 7 H29C H -0.0546 -0.8533 -0.0372 0.208 Uiso 0.55(2) 1 calc PR D 7 N7' N -0.0029(6) -0.7781(10) -0.0851(8) 0.158(5) Uiso 0.45(2) 1 d PD D 8 O15' O -0.0150(9) -0.6461(12) -0.1444(9) 0.207(6) Uiso 0.45(2) 1 d PD D 8 C27' C -0.0021(15) -0.7330(17) -0.1445(13) 0.147(16) Uiso 0.45(2) 1 d PD D 8 H27B H 0.0070 -0.7641 -0.1801 0.176 Uiso 0.45(2) 1 calc PR D 8 C28' C -0.010(2) -0.721(2) -0.0323(18) 0.140(15) Uiso 0.45(2) 1 d PD D 8 H28D H -0.0217 -0.6557 -0.0500 0.210 Uiso 0.45(2) 1 calc PR D 8 H28E H 0.0472 -0.7239 0.0167 0.210 Uiso 0.45(2) 1 calc PR D 8 H28F H -0.0597 -0.7436 -0.0272 0.210 Uiso 0.45(2) 1 calc PR D 8 C29' C 0.018(2) -0.8835(19) -0.061(2) 0.138(16) Uiso 0.45(2) 1 d PD D 8 H29D H 0.0212 -0.9188 -0.1000 0.206 Uiso 0.45(2) 1 calc PR D 8 H29E H -0.0302 -0.9096 -0.0553 0.206 Uiso 0.45(2) 1 calc PR D 8 H29F H 0.0763 -0.8883 -0.0134 0.206 Uiso 0.45(2) 1 calc PR D 8 O17 O -0.462(2) -0.6263(19) 0.0670(16) 0.184(7) Uiso 0.50 1 d PD . . N9 N -0.366(2) -0.510(2) 0.0554(16) 0.184(7) Uiso 0.50 1 d PD . . C34 C -0.366(3) -0.568(2) 0.003(2) 0.184(7) Uiso 0.50 1 d PD . . H34A H -0.3752 -0.6328 0.0126 0.277 Uiso 0.50 1 calc PR . . H34B H -0.3073 -0.5624 0.0067 0.277 Uiso 0.50 1 calc PR . . H34C H -0.4147 -0.5491 -0.0474 0.277 Uiso 0.50 1 calc PR . . C35 C -0.341(3) -0.423(2) 0.081(2) 0.184(7) Uiso 0.50 1 d PD . . H35A H -0.3252 -0.4198 0.1337 0.277 Uiso 0.50 1 calc PR . . H35B H -0.3903 -0.3792 0.0507 0.277 Uiso 0.50 1 calc PR . . H35C H -0.2873 -0.4056 0.0793 0.277 Uiso 0.50 1 calc PR . . C33 C -0.4171(19) -0.546(2) 0.0799(19) 0.184(7) Uiso 0.50 1 d PD . . H33A H -0.4224 -0.5053 0.1135 0.221 Uiso 0.50 1 calc PR . . 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 Cd2 0.0372(3) 0.0206(3) 0.0177(3) 0.00070(17) 0.0188(3) 0.00108(19) Cd1 0.0392(4) 0.0205(3) 0.0198(3) 0.00155(17) 0.0206(3) 0.00350(19) O1 0.089(4) 0.037(2) 0.039(3) 0.001(2) 0.043(3) 0.008(2) O2 0.090(4) 0.037(3) 0.039(3) -0.002(2) 0.041(3) 0.006(2) O3 0.068(4) 0.021(2) 0.035(3) -0.007(2) 0.032(3) -0.002(2) O4 0.055(4) 0.029(2) 0.025(3) -0.003(2) 0.029(3) -0.006(2) O7 0.084(4) 0.036(2) 0.038(3) 0.006(2) 0.042(3) 0.004(2) O8 0.053(3) 0.027(2) 0.031(2) 0.0034(17) 0.026(2) 0.002(2) O9 0.048(3) 0.022(2) 0.033(2) 0.0032(18) 0.028(2) 0.0012(19) O10 0.058(4) 0.023(2) 0.023(2) -0.0020(18) 0.028(3) -0.007(2) O11 0.145(9) 0.080(5) 0.062(5) -0.018(4) 0.061(6) -0.059(5) O12 0.180(10) 0.037(4) 0.115(7) 0.005(4) 0.105(7) 0.016(4) O13 0.035(3) 0.053(3) 0.035(3) -0.006(2) 0.014(3) 0.005(2) O14 0.047(4) 0.080(4) 0.051(4) 0.003(3) 0.031(4) -0.001(3) N2 0.147(10) 0.033(4) 0.055(5) -0.003(3) 0.070(7) -0.021(5) N3 0.038(4) 0.021(3) 0.026(3) -0.003(2) 0.018(3) 0.001(2) N4 0.037(4) 0.026(3) 0.026(3) -0.003(2) 0.019(3) -0.002(2) N5 0.046(6) 0.054(4) 0.047(5) 0.006(3) 0.000(4) -0.001(4) N6 0.042(6) 0.099(7) 0.080(7) 0.007(5) 0.022(6) 0.015(5) C1 0.037(4) 0.025(3) 0.026(4) -0.002(3) 0.023(4) 0.002(3) C2 0.062(6) 0.026(3) 0.025(4) 0.005(3) 0.032(4) 0.005(3) C3 0.057(6) 0.028(3) 0.025(4) -0.003(3) 0.024(4) 0.002(3) C4 0.035(4) 0.023(3) 0.023(3) -0.007(3) 0.019(3) -0.005(3) C5 0.047(5) 0.026(3) 0.020(3) 0.001(3) 0.021(4) 0.003(3) C6 0.058(5) 0.023(3) 0.025(4) 0.007(3) 0.028(4) 0.005(3) C7 0.043(5) 0.030(3) 0.022(3) -0.004(3) 0.024(4) -0.002(3) C8 0.033(4) 0.022(3) 0.025(4) -0.005(3) 0.019(4) -0.004(3) C9 0.052(5) 0.027(3) 0.023(4) 0.008(3) 0.023(4) 0.006(3) C10 0.059(4) 0.029(3) 0.025(3) 0.004(2) 0.024(3) -0.008(3) C11 0.089(7) 0.018(3) 0.036(4) -0.006(3) 0.045(5) -0.016(3) C12 0.036(4) 0.025(3) 0.021(3) 0.005(3) 0.020(3) -0.001(3) C13 0.040(5) 0.023(3) 0.025(4) 0.002(3) 0.019(4) -0.003(3) C14 0.047(5) 0.032(3) 0.030(4) -0.007(3) 0.027(4) -0.001(3) C15 0.040(5) 0.034(3) 0.024(4) 0.005(3) 0.025(4) 0.003(3) C16 0.032(4) 0.022(3) 0.025(4) 0.009(3) 0.019(3) 0.002(3) C17 0.049(5) 0.025(3) 0.040(4) 0.009(3) 0.029(4) 0.004(3) C18 0.041(5) 0.031(3) 0.034(4) 0.003(3) 0.023(4) -0.003(3) C19 0.041(5) 0.029(3) 0.036(4) 0.007(3) 0.019(4) -0.001(3) C20 0.055(6) 0.033(4) 0.033(4) 0.008(3) 0.026(4) -0.003(3) C21 0.045(6) 0.051(4) 0.035(5) 0.000(4) 0.020(5) -0.002(4) C24 0.051(7) 0.065(6) 0.050(6) -0.004(4) 0.026(6) 0.013(5) C22 0.045(10) 0.094(10) 0.137(14) -0.045(11) 0.000(9) 0.022(7) C23 0.060(10) 0.120(10) 0.044(7) -0.001(7) -0.003(6) -0.015(7) C22' 0.045(10) 0.094(10) 0.137(14) -0.045(11) 0.000(9) 0.022(7) C23' 0.060(10) 0.120(10) 0.044(7) -0.001(7) -0.003(6) -0.015(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 Cd2 O13 2.256(6) . ? Cd2 O10 2.273(4) 4 ? Cd2 O3 2.310(4) 1_565 ? Cd2 N3 2.334(6) 2_455 ? Cd2 O8 2.335(5) . ? Cd2 O7 2.444(5) . ? Cd2 O9 2.604(4) 4 ? Cd2 C15 2.716(6) . ? Cd1 O14 2.233(7) . ? Cd1 O4 2.276(4) 4_546 ? Cd1 O2 2.322(5) . ? Cd1 O9 2.322(4) . ? Cd1 N4 2.356(6) . ? Cd1 O1 2.395(5) . ? Cd1 C7 2.694(6) . ? O1 C7 1.224(8) . ? O2 C7 1.234(7) . ? O3 C8 1.249(8) . ? O3 Cd2 2.310(4) 1_545 ? O4 C8 1.252(7) . ? O4 Cd1 2.276(4) 4_545 ? O6 N1 1.122(19) . ? O5 N1 1.228(17) . ? O7 C15 1.236(7) . ? O8 C15 1.254(7) . ? O9 C16 1.247(8) . ? O9 Cd2 2.604(4) 4_556 ? O10 C16 1.254(7) . ? O10 Cd2 2.273(4) 4_556 ? O11 N2 1.238(12) . ? O12 N2 1.175(12) . ? O13 C21 1.216(9) . ? O14 C24 1.240(11) . ? N1 C2 1.528(14) . ? N2 C10 1.475(9) . ? N3 C20 1.327(9) . ? N3 C17 1.334(8) . ? N3 Cd2 2.334(6) 2_445 ? N4 C18 1.327(9) . ? N4 C19 1.345(8) . ? N5 C21 1.304(11) . ? N5 C22 1.434(15) . ? N5 C22' 1.45(2) . ? N5 C23' 1.46(2) . ? N5 C23 1.465(11) . ? N6 C24 1.248(12) . ? N6 C26' 1.37(2) . ? N6 C25 1.46(4) . ? N6 C25' 1.56(2) . ? N6 C26 1.69(4) . ? C1 C2 1.376(9) . ? C1 C6 1.384(8) . ? C1 C7 1.520(8) . ? C2 C3 1.381(9) . ? C3 C4 1.389(8) . ? C3 H3A 0.9500 . ? C4 C5 1.386(8) . ? C4 C8 1.496(8) . ? C5 C6 1.398(8) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C9 C10 1.386(9) . ? C9 C14 1.395(9) . ? C9 C15 1.493(8) . ? C10 C11 1.387(9) . ? C11 C12 1.389(8) . ? C11 H11A 0.9500 . ? C12 C13 1.392(9) . ? C12 C16 1.516(8) . ? C13 C14 1.383(9) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C17 C18 1.391(10) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.366(11) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C24 H24A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23' H23D 0.9800 . ? C23' H23E 0.9800 . ? C23' H23F 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C25' H25D 0.9800 . ? C25' H25E 0.9800 . ? C25' H25F 0.9800 . ? C26' H26D 0.9800 . ? C26' H26E 0.9800 . ? C26' H26F 0.9800 . ? O16 C30 1.205(11) . ? N8 C30 1.300(11) . ? N8 C32 1.404(12) . ? N8 C31 1.503(13) . ? C30 H30B 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C30' H30A 0.9500 . ? C31' H31D 0.9800 . ? C31' H31E 0.9800 . ? C31' H31F 0.9800 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? N7 C27 1.389(16) . ? N7 C29 1.420(16) . ? N7 C28 1.425(16) . ? O15 C27 1.237(16) . ? C27 H27A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C27' H27B 0.9500 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 0.9800 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? O17 C33 1.334(19) . ? N9 C35 1.333(18) . ? N9 C33 1.334(19) . ? N9 C34 1.372(18) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C33 H33A 0.9500 . ? 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 Cd2 O10 90.38(18) . 4 ? O13 Cd2 O3 90.37(18) . 1_565 ? O10 Cd2 O3 130.45(15) 4 1_565 ? O13 Cd2 N3 178.00(17) . 2_455 ? O10 Cd2 N3 91.59(18) 4 2_455 ? O3 Cd2 N3 88.12(18) 1_565 2_455 ? O13 Cd2 O8 91.3(2) . . ? O10 Cd2 O8 141.34(14) 4 . ? O3 Cd2 O8 88.16(14) 1_565 . ? N3 Cd2 O8 87.39(19) 2_455 . ? O13 Cd2 O7 92.0(2) . . ? O10 Cd2 O7 86.90(15) 4 . ? O3 Cd2 O7 142.56(16) 1_565 . ? N3 Cd2 O7 88.38(19) 2_455 . ? O8 Cd2 O7 54.45(15) . . ? O13 Cd2 O9 96.86(18) . 4 ? O10 Cd2 O9 53.14(14) 4 4 ? O3 Cd2 O9 77.62(14) 1_565 4 ? N3 Cd2 O9 84.10(17) 2_455 4 ? O8 Cd2 O9 163.62(15) . 4 ? O7 Cd2 O9 138.90(15) . 4 ? O13 Cd2 C15 90.3(2) . . ? O10 Cd2 C15 113.93(17) 4 . ? O3 Cd2 C15 115.60(17) 1_565 . ? N3 Cd2 C15 89.2(2) 2_455 . ? O8 Cd2 C15 27.45(16) . . ? O7 Cd2 C15 27.08(17) . . ? O9 Cd2 C15 165.03(18) 4 . ? O14 Cd1 O4 92.8(2) . 4_546 ? O14 Cd1 O2 95.3(2) . . ? O4 Cd1 O2 142.43(16) 4_546 . ? O14 Cd1 O9 89.8(2) . . ? O4 Cd1 O9 125.95(15) 4_546 . ? O2 Cd1 O9 90.76(15) . . ? O14 Cd1 N4 171.7(2) . . ? O4 Cd1 N4 87.41(18) 4_546 . ? O2 Cd1 N4 89.5(2) . . ? O9 Cd1 N4 83.43(17) . . ? O14 Cd1 O1 94.0(2) . . ? O4 Cd1 O1 88.67(16) 4_546 . ? O2 Cd1 O1 54.24(16) . . ? O9 Cd1 O1 144.99(16) . . ? N4 Cd1 O1 94.33(19) . . ? O14 Cd1 C7 95.1(2) . . ? O4 Cd1 C7 115.54(17) 4_546 . ? O2 Cd1 C7 27.21(17) . . ? O9 Cd1 C7 117.97(17) . . ? N4 Cd1 C7 92.3(2) . . ? O1 Cd1 C7 27.03(17) . . ? C7 O1 Cd1 90.2(4) . . ? C7 O2 Cd1 93.4(4) . . ? C8 O3 Cd2 175.4(4) . 1_545 ? C8 O4 Cd1 103.9(4) . 4_545 ? C15 O7 Cd2 88.8(4) . . ? C15 O8 Cd2 93.4(4) . . ? C16 O9 Cd1 164.6(4) . . ? C16 O9 Cd2 84.1(3) . 4_556 ? Cd1 O9 Cd2 105.03(16) . 4_556 ? C16 O10 Cd2 99.4(3) . 4_556 ? C21 O13 Cd2 122.6(5) . . ? C24 O14 Cd1 129.7(6) . . ? O6 N1 O5 133.5(19) . . ? O6 N1 C2 108.6(16) . . ? O5 N1 C2 113.2(14) . . ? O12 N2 O11 125.1(9) . . ? O12 N2 C10 116.4(10) . . ? O11 N2 C10 118.5(9) . . ? C20 N3 C17 116.4(7) . . ? C20 N3 Cd2 122.9(5) . 2_445 ? C17 N3 Cd2 120.6(5) . 2_445 ? C18 N4 C19 117.0(7) . . ? C18 N4 Cd1 120.8(4) . . ? C19 N4 Cd1 122.2(5) . . ? C21 N5 C22 122.4(10) . . ? C21 N5 C22' 113(8) . . ? C22 N5 C22' 37(10) . . ? C21 N5 C23' 114(6) . . ? C22 N5 C23' 94(7) . . ? C22' N5 C23' 126(10) . . ? C21 N5 C23 123.7(9) . . ? C22 N5 C23 113.6(11) . . ? C22' N5 C23 114(10) . . ? C23' N5 C23 54(6) . . ? C24 N6 C26' 131.7(13) . . ? C24 N6 C25 110.7(19) . . ? C26' N6 C25 105(2) . . ? C24 N6 C25' 116.6(12) . . ? C26' N6 C25' 111.6(14) . . ? C25 N6 C25' 45.9(17) . . ? C24 N6 C26 108.5(16) . . ? C26' N6 C26 24.7(15) . . ? C25 N6 C26 128(2) . . ? C25' N6 C26 132.7(18) . . ? C2 C1 C6 117.4(6) . . ? C2 C1 C7 122.4(5) . . ? C6 C1 C7 120.2(5) . . ? C1 C2 C3 121.9(6) . . ? C1 C2 N1 127.4(7) . . ? C3 C2 N1 110.6(7) . . ? C2 C3 C4 119.8(6) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 120.0(6) . . ? C5 C4 C8 120.9(5) . . ? C3 C4 C8 119.1(5) . . ? C4 C5 C6 118.3(6) . . ? C4 C5 H5A 120.8 . . ? C6 C5 H5A 120.8 . . ? C1 C6 C5 122.5(6) . . ? C1 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? O1 C7 O2 122.1(6) . . ? O1 C7 C1 118.8(6) . . ? O2 C7 C1 119.1(6) . . ? O1 C7 Cd1 62.7(3) . . ? O2 C7 Cd1 59.4(3) . . ? C1 C7 Cd1 177.9(5) . . ? O3 C8 O4 122.2(5) . . ? O3 C8 C4 119.4(5) . . ? O4 C8 C4 118.4(5) . . ? C10 C9 C14 116.3(6) . . ? C10 C9 C15 122.6(6) . . ? C14 C9 C15 121.2(6) . . ? C9 C10 C11 123.7(6) . . ? C9 C10 N2 122.0(6) . . ? C11 C10 N2 114.0(6) . . ? C10 C11 C12 118.3(6) . . ? C10 C11 H11A 120.9 . . ? C12 C11 H11A 120.9 . . ? C11 C12 C13 119.8(5) . . ? C11 C12 C16 117.8(5) . . ? C13 C12 C16 122.3(5) . . ? C14 C13 C12 120.1(6) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C9 121.8(6) . . ? C13 C14 H14A 119.1 . . ? C9 C14 H14A 119.1 . . ? O7 C15 O8 122.9(6) . . ? O7 C15 C9 118.8(6) . . ? O8 C15 C9 118.3(6) . . ? O7 C15 Cd2 64.1(3) . . ? O8 C15 Cd2 59.1(3) . . ? C9 C15 Cd2 174.6(5) . . ? O9 C16 O10 123.3(5) . . ? O9 C16 C12 119.5(5) . . ? O10 C16 C12 117.1(5) . . ? N3 C17 C18 121.6(6) . . ? N3 C17 H17A 119.2 . . ? C18 C17 H17A 119.2 . . ? N4 C18 C17 121.2(6) . . ? N4 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? N4 C19 C20 121.1(7) . . ? N4 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? N3 C20 C19 122.7(6) . . ? N3 C20 H20A 118.6 . . ? C19 C20 H20A 118.6 . . ? O13 C21 N5 126.2(8) . . ? O13 C21 H21A 116.9 . . ? N5 C21 H21A 116.9 . . ? O14 C24 N6 127.0(10) . . ? O14 C24 H24A 116.5 . . ? N6 C24 H24A 116.5 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 H23A 109.5 . . ? N5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C22' H22D 109.5 . . ? N5 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? N5 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? N5 C23' H23D 109.5 . . ? N5 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? N5 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? N6 C25 H25A 109.5 . . ? N6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C25' H25D 109.5 . . ? N6 C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? N6 C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? N6 C26' H26D 109.5 . . ? N6 C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? N6 C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C30 N8 C32 125.7(11) . . ? C30 N8 C31 116.1(10) . . ? C32 N8 C31 118.2(10) . . ? O16 C30 N8 126.6(10) . . ? O16 C30 H30B 116.7 . . ? N8 C30 H30B 116.7 . . ? N8 C31 H31A 109.5 . . ? N8 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N8 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N8 C32 H32A 109.5 . . ? N8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? H31D C31' H31E 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? H32D C32' H32E 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C27 N7 C29 106.4(18) . . ? C27 N7 C28 132.7(18) . . ? C29 N7 C28 120.9(16) . . ? O15 C27 N7 113.7(18) . . ? O15 C27 H27A 123.2 . . ? N7 C27 H27A 123.2 . . ? N7 C28 H28A 109.5 . . ? N7 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N7 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N7 C29 H29A 109.5 . . ? N7 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N7 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? H28D C28' H28E 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? H29D C29' H29E 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C35 N9 C33 110(3) . . ? C35 N9 C34 138(3) . . ? C33 N9 C34 111(3) . . ? N9 C34 H34A 109.5 . . ? N9 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N9 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N9 C35 H35A 109.5 . . ? N9 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N9 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N9 C33 O17 133(4) . . ? N9 C33 H33A 113.3 . . ? O17 C33 H33A 113.3 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.778 _refine_diff_density_min -1.259 _refine_diff_density_rms 0.147 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 840368' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H14 Cd2 N6 O12' _chemical_formula_weight 803.23 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 orthorhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' _cell_length_a 20.914(2) _cell_length_b 14.3821(15) _cell_length_c 7.4466(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2239.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7238 _exptl_absorpt_correction_T_max 0.8699 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Germioni S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10051 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2104 _reflns_number_gt 1823 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1015P)^2^+9.7466P] 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 2104 _refine_ls_number_parameters 119 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1762 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.089 _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 -0.43710(3) 0.39701(4) 0.5000 0.0295(3) Uani 1 2 d S . . C1 C -0.2561(4) 0.2689(7) 0.5000 0.041(2) Uani 1 2 d S . . C2 C -0.2012(5) 0.3225(7) 0.5000 0.050(3) Uani 1 2 d SDU . . C3 C -0.1419(5) 0.2806(7) 0.5000 0.047(2) Uani 1 2 d SU . . H3A H -0.1055 0.3177 0.5000 0.057 Uiso 1 2 d SR . . C4 C -0.1356(4) 0.1853(6) 0.5000 0.0315(19) Uani 1 2 d S . . C5 C -0.1905(4) 0.1320(6) 0.5000 0.038(2) Uani 1 2 d S . . H5A H -0.1874 0.0675 0.5000 0.046 Uiso 1 2 calc SR . . C6 C -0.2502(5) 0.1741(7) 0.5000 0.041(2) Uani 1 2 d SU . . H6A H -0.2867 0.1374 0.5000 0.049 Uiso 1 2 calc SR . . C7 C -0.3219(4) 0.3129(7) 0.5000 0.041(2) Uani 1 2 d S . . C8 C -0.0708(4) 0.1438(7) 0.5000 0.040(2) Uani 1 2 d S . . C9 C -0.4747(4) 0.3423(5) 0.0938(11) 0.058(2) Uani 1 1 d . . . H9A H -0.4986 0.2978 0.1547 0.070 Uiso 1 1 calc R . . C10 C -0.4091(4) 0.4647(5) 0.0926(10) 0.0490(18) Uani 1 1 d . . . H10A H -0.3846 0.5107 0.1553 0.059 Uiso 1 1 d R . . N1 N -0.1969(12) 0.4217(12) 0.5000 0.150(8) Uiso 1 2 d SD . . N2 N -0.4417(2) 0.4036(4) 0.1865(9) 0.0400(14) Uani 1 1 d . . . O1 O -0.3268(4) 0.3971(5) 0.464(2) 0.039(5) Uani 0.50 1 d P . . O2 O -0.3684(4) 0.2642(6) 0.5457(13) 0.043(3) Uani 0.50 1 d PU . . O3 O -0.0638(3) 0.0572(5) 0.5000 0.0429(17) Uani 1 2 d SU . . O4 O -0.0234(3) 0.1980(4) 0.5000 0.0427(17) Uani 1 2 d S . . O5 O -0.2014(8) 0.4570(10) 0.359(2) 0.205(6) 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 Cd1 0.0147(4) 0.0325(4) 0.0414(5) 0.000 0.000 0.0008(2) C1 0.022(5) 0.040(5) 0.062(7) 0.000 0.000 0.006(4) C2 0.041(4) 0.041(4) 0.067(5) 0.000 0.000 0.004(3) C3 0.037(4) 0.041(4) 0.064(5) 0.000 0.000 0.003(3) C4 0.017(4) 0.035(4) 0.043(5) 0.000 0.000 0.005(3) C5 0.026(5) 0.029(4) 0.061(7) 0.000 0.000 0.005(4) C6 0.032(4) 0.039(4) 0.052(4) 0.000 0.000 -0.005(3) C7 0.016(4) 0.042(5) 0.066(7) 0.000 0.000 0.007(4) C8 0.032(5) 0.035(5) 0.052(7) 0.000 0.000 0.010(4) C9 0.065(5) 0.061(5) 0.048(5) 0.005(4) 0.003(4) -0.026(4) C10 0.052(4) 0.054(4) 0.041(4) -0.003(4) 0.001(4) -0.025(3) N2 0.031(3) 0.045(3) 0.044(4) 0.000(3) 0.001(2) 0.002(2) O1 0.025(4) 0.045(4) 0.047(15) 0.005(5) 0.001(4) 0.010(3) O2 0.034(4) 0.047(3) 0.049(6) 0.003(3) 0.002(3) 0.007(3) O3 0.038(3) 0.039(3) 0.052(4) 0.000 0.000 0.005(2) O4 0.017(3) 0.039(3) 0.072(5) 0.000 0.000 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.264(6) 3_456 ? Cd1 O3 2.304(7) 7_565 ? Cd1 O1 2.321(8) . ? Cd1 O1 2.321(8) 6_556 ? Cd1 N2 2.339(7) . ? Cd1 N2 2.339(7) 6_556 ? Cd1 O2 2.414(8) . ? Cd1 O2 2.414(8) 6_556 ? Cd1 C7 2.695(8) . ? Cd1 O3 2.731(6) 3_456 ? Cd1 C8 2.858(9) 3_456 ? C1 C6 1.369(14) . ? C1 C2 1.383(15) . ? C1 C7 1.515(12) . ? C2 C3 1.379(14) . ? C2 N1 1.430(16) . ? C3 C4 1.377(12) . ? C3 H3A 0.9297 . ? C4 C5 1.380(13) . ? C4 C8 1.480(12) . ? C5 C6 1.388(13) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O1 1.244(12) 6_556 ? C7 O1 1.244(12) . ? C7 O2 1.245(12) 6_556 ? C7 O2 1.245(12) . ? C8 O3 1.254(13) . ? C8 O4 1.260(12) . ? C8 Cd1 2.858(9) 3_556 ? C9 N2 1.315(9) . ? C9 C9 1.398(17) 6 ? C9 H9A 0.9300 . ? C10 N2 1.313(9) . ? C10 C10 1.378(16) 6 ? C10 H10A 0.9599 . ? N1 O5 1.167(13) 6_556 ? N1 O5 1.167(13) . ? O1 O1 0.53(3) 6_556 ? O2 O2 0.681(19) 6_556 ? O3 Cd1 2.304(7) 7 ? O3 Cd1 2.731(6) 3_556 ? O4 Cd1 2.264(6) 3_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O3 127.6(2) 3_456 7_565 ? O4 Cd1 O1 142.4(2) 3_456 . ? O3 Cd1 O1 89.5(2) 7_565 . ? O4 Cd1 O1 142.4(2) 3_456 6_556 ? O3 Cd1 O1 89.5(2) 7_565 6_556 ? O1 Cd1 O1 13.1(8) . 6_556 ? O4 Cd1 N2 89.52(13) 3_456 . ? O3 Cd1 N2 87.68(13) 7_565 . ? O1 Cd1 N2 85.8(4) . . ? O1 Cd1 N2 98.9(4) 6_556 . ? O4 Cd1 N2 89.52(13) 3_456 6_556 ? O3 Cd1 N2 87.68(13) 7_565 6_556 ? O1 Cd1 N2 98.9(4) . 6_556 ? O1 Cd1 N2 85.8(4) 6_556 6_556 ? N2 Cd1 N2 173.3(3) . 6_556 ? O4 Cd1 O2 89.9(2) 3_456 . ? O3 Cd1 O2 141.8(2) 7_565 . ? O1 Cd1 O2 54.9(3) . . ? O1 Cd1 O2 52.6(3) 6_556 . ? N2 Cd1 O2 101.4(3) . . ? N2 Cd1 O2 85.2(3) 6_556 . ? O4 Cd1 O2 89.9(2) 3_456 6_556 ? O3 Cd1 O2 141.8(2) 7_565 6_556 ? O1 Cd1 O2 52.6(3) . 6_556 ? O1 Cd1 O2 54.9(3) 6_556 6_556 ? N2 Cd1 O2 85.2(3) . 6_556 ? N2 Cd1 O2 101.4(3) 6_556 6_556 ? O2 Cd1 O2 16.2(5) . 6_556 ? O4 Cd1 C7 116.2(3) 3_456 . ? O3 Cd1 C7 116.2(3) 7_565 . ? O1 Cd1 C7 27.4(3) . . ? O1 Cd1 C7 27.4(3) 6_556 . ? N2 Cd1 C7 93.17(13) . . ? N2 Cd1 C7 93.17(13) 6_556 . ? O2 Cd1 C7 27.5(3) . . ? O2 Cd1 C7 27.5(3) 6_556 . ? O4 Cd1 O3 51.1(2) 3_456 3_456 ? O3 Cd1 O3 76.5(2) 7_565 3_456 ? O1 Cd1 O3 164.6(3) . 3_456 ? O1 Cd1 O3 164.6(3) 6_556 3_456 ? N2 Cd1 O3 87.14(13) . 3_456 ? N2 Cd1 O3 87.14(13) 6_556 3_456 ? O2 Cd1 O3 140.2(3) . 3_456 ? O2 Cd1 O3 140.2(3) 6_556 3_456 ? C7 Cd1 O3 167.3(3) . 3_456 ? O4 Cd1 C8 25.2(3) 3_456 3_456 ? O3 Cd1 C8 102.3(3) 7_565 3_456 ? O1 Cd1 C8 166.5(3) . 3_456 ? O1 Cd1 C8 166.5(3) 6_556 3_456 ? N2 Cd1 C8 88.16(13) . 3_456 ? N2 Cd1 C8 88.16(13) 6_556 3_456 ? O2 Cd1 C8 114.8(3) . 3_456 ? O2 Cd1 C8 114.8(3) 6_556 3_456 ? C7 Cd1 C8 141.5(3) . 3_456 ? O3 Cd1 C8 25.8(3) 3_456 3_456 ? C6 C1 C2 118.7(9) . . ? C6 C1 C7 119.9(9) . . ? C2 C1 C7 121.5(9) . . ? C3 C2 C1 120.2(9) . . ? C3 C2 N1 112.3(13) . . ? C1 C2 N1 127.5(13) . . ? C4 C3 C2 121.4(10) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.1 . . ? C3 C4 C5 118.2(8) . . ? C3 C4 C8 119.3(8) . . ? C5 C4 C8 122.5(8) . . ? C4 C5 C6 120.4(8) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C1 C6 C5 121.1(9) . . ? C1 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? O1 C7 O1 24.6(14) 6_556 . ? O1 C7 O2 122.8(9) 6_556 6_556 ? O1 C7 O2 115.2(8) . 6_556 ? O1 C7 O2 115.2(8) 6_556 . ? O1 C7 O2 122.8(9) . . ? O2 C7 O2 31.7(9) 6_556 . ? O1 C7 C1 118.8(8) 6_556 . ? O1 C7 C1 118.8(8) . . ? O2 C7 C1 118.3(8) 6_556 . ? O2 C7 C1 118.3(8) . . ? O1 C7 Cd1 59.3(5) 6_556 . ? O1 C7 Cd1 59.3(5) . . ? O2 C7 Cd1 63.6(5) 6_556 . ? O2 C7 Cd1 63.6(5) . . ? C1 C7 Cd1 178.0(7) . . ? O3 C8 O4 121.4(8) . . ? O3 C8 C4 120.5(8) . . ? O4 C8 C4 118.1(8) . . ? O3 C8 Cd1 71.4(5) . 3_556 ? O4 C8 Cd1 50.0(4) . 3_556 ? C4 C8 Cd1 168.1(7) . 3_556 ? N2 C9 C9 121.6(5) . 6 ? N2 C9 H9A 119.2 . . ? C9 C9 H9A 119.2 6 . ? N2 C10 C10 122.2(4) . 6 ? N2 C10 H10A 118.7 . . ? C10 C10 H10A 119.1 6 . ? O5 N1 O5 128(2) 6_556 . ? O5 N1 C2 115.4(12) 6_556 . ? O5 N1 C2 115.4(12) . . ? C10 N2 C9 116.2(7) . . ? C10 N2 Cd1 122.5(5) . . ? C9 N2 Cd1 121.2(5) . . ? O1 O1 C7 77.7(7) 6_556 . ? O1 O1 Cd1 83.4(4) 6_556 . ? C7 O1 Cd1 93.3(6) . . ? O2 O2 C7 74.1(5) 6_556 . ? O2 O2 Cd1 81.9(2) 6_556 . ? C7 O2 Cd1 88.9(6) . . ? C8 O3 Cd1 173.7(6) . 7 ? C8 O3 Cd1 82.8(5) . 3_556 ? Cd1 O3 Cd1 103.5(2) 7 3_556 ? C8 O4 Cd1 104.7(6) . 3_556 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.612 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.154 # 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 0.298 -0.023 -0.008 1084 157 ' ' _platon_squeeze_details ; ; #===END data_3' _database_code_depnum_ccdc_archive 'CCDC 840369' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H14 Cd2 N6 O12' _chemical_formula_weight 803.21 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 P21/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 7.4058(3) _cell_length_b 20.7757(7) _cell_length_c 14.2332(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.132(4) _cell_angle_gamma 90.00 _cell_volume 2162.17(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7160 _exptl_absorpt_correction_T_max 0.8657 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Germioni S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10581 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3764 _reflns_number_gt 3194 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+25.2112P] 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 3764 _refine_ls_number_parameters 200 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.073 _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 -0.46179(7) 0.43581(2) -0.39866(3) 0.0177(2) Uani 1 1 d . . . C1 C -0.4651(12) 0.2520(4) -0.2760(5) 0.0292(17) Uani 1 1 d . . . C2 C -0.4810(16) 0.1961(4) -0.3293(6) 0.047(3) Uani 1 1 d . . . C3 C -0.5056(14) 0.1365(4) -0.2909(6) 0.040(2) Uani 1 1 d . . . H3A H -0.5188 0.0993 -0.3300 0.047 Uiso 1 1 calc R . . C4 C -0.5107(11) 0.1317(3) -0.1936(5) 0.0228(16) Uani 1 1 d . . . C5 C -0.4909(11) 0.1864(4) -0.1373(6) 0.0286(17) Uani 1 1 d . . . H5A H -0.4906 0.1834 -0.0707 0.034 Uiso 1 1 calc R . . C6 C -0.4714(12) 0.2466(3) -0.1801(5) 0.0299(18) Uani 1 1 d . . . H6A H -0.4625 0.2843 -0.1420 0.036 Uiso 1 1 calc R . . C7 C -0.4562(10) 0.3182(3) -0.3200(5) 0.0235(16) Uani 1 1 d . . . C8 C -0.5327(9) 0.0662(3) -0.1529(5) 0.0205(15) Uani 1 1 d . . . C9 C -0.8899(10) 0.4121(4) -0.4740(5) 0.0240(16) Uani 1 1 d . . . H9A H -0.8379 0.3923 -0.5236 0.029 Uiso 1 1 calc R . . C10 C -1.0785(10) 0.4122(4) -0.4750(5) 0.0262(16) Uani 1 1 d . . . H10A H -1.1550 0.3929 -0.5273 0.031 Uiso 1 1 calc R . . C11 C -1.0399(10) 0.4689(4) -0.3352(5) 0.0259(17) Uani 1 1 d . . . H11A H -1.0885 0.4905 -0.2859 0.031 Uiso 1 1 calc R . . C12 C -0.8519(10) 0.4690(4) -0.3341(6) 0.0272(17) Uani 1 1 d . . . H12A H -0.7728 0.4897 -0.2841 0.033 Uiso 1 1 calc R . . N1 N -0.4448(18) 0.1946(6) -0.4287(9) 0.081(3) Uani 1 1 d U . . N2 N -0.7863(7) 0.4404(2) -0.4020(3) 0.0074(10) Uani 1 1 d U . . N3 N -1.1563(8) 0.4386(2) -0.4051(4) 0.0177(12) Uani 1 1 d U . . O1 O -0.4983(9) 0.3238(3) -0.4076(4) 0.0371(14) Uani 1 1 d U . . O2 O -0.4059(11) 0.3639(3) -0.2673(4) 0.0526(18) Uani 1 1 d U . . O3 O -0.5147(7) 0.0589(2) -0.0633(4) 0.0261(11) Uani 1 1 d . . . O4 O -0.5643(7) 0.0191(2) -0.2091(4) 0.0219(11) Uani 1 1 d . . . O5 O -0.5737(17) 0.1755(6) -0.4853(8) 0.108(4) Uani 1 1 d U . . O6 O -0.294(2) 0.2148(6) -0.4468(8) 0.127(5) 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 0.0230(3) 0.0100(3) 0.0209(3) 0.0009(2) 0.00562(19) 0.0007(2) C1 0.043(5) 0.019(4) 0.024(4) 0.005(3) 0.000(3) 0.003(3) C2 0.094(8) 0.018(4) 0.030(5) 0.002(4) 0.016(5) -0.012(5) C3 0.081(7) 0.012(4) 0.026(4) -0.003(3) 0.006(4) 0.001(4) C4 0.037(4) 0.011(3) 0.020(4) 0.003(3) 0.006(3) -0.006(3) C5 0.036(4) 0.023(4) 0.031(4) 0.006(3) 0.017(3) 0.002(3) C6 0.054(5) 0.011(3) 0.025(4) -0.006(3) 0.006(4) -0.003(3) C7 0.031(4) 0.010(3) 0.028(4) 0.003(3) 0.001(3) -0.004(3) C8 0.022(3) 0.018(4) 0.023(4) -0.006(3) 0.007(3) 0.001(3) C9 0.025(4) 0.021(4) 0.027(4) -0.010(3) 0.007(3) -0.003(3) C10 0.023(4) 0.026(4) 0.029(4) -0.011(3) 0.001(3) 0.001(3) C11 0.022(4) 0.032(4) 0.025(4) -0.012(3) 0.005(3) 0.006(3) C12 0.020(4) 0.033(4) 0.029(4) -0.008(3) 0.005(3) -0.002(3) N1 0.092(5) 0.072(5) 0.079(5) 0.004(4) 0.016(4) 0.001(4) N2 0.0123(16) 0.0023(16) 0.0068(16) 0.0002(13) -0.0008(13) 0.0013(14) N3 0.037(3) 0.004(2) 0.010(2) -0.0026(19) -0.001(2) -0.004(2) O1 0.069(4) 0.017(3) 0.024(3) 0.006(2) 0.003(3) -0.004(3) O2 0.093(5) 0.025(3) 0.034(3) 0.004(3) -0.009(3) -0.014(3) O3 0.038(3) 0.018(3) 0.022(3) 0.001(2) 0.008(2) 0.004(2) O4 0.031(3) 0.009(2) 0.027(3) 0.003(2) 0.005(2) -0.004(2) O5 0.124(5) 0.104(5) 0.094(5) 0.012(4) 0.009(4) -0.025(4) O6 0.177(13) 0.124(10) 0.101(8) 0.043(7) 0.090(9) 0.063(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.279(6) 1_655 ? Cd1 O4 2.300(5) 2_454 ? Cd1 O3 2.317(5) 4_565 ? Cd1 O1 2.344(5) . ? Cd1 O2 2.378(6) . ? Cd1 N2 2.398(5) . ? Cd1 O3 2.614(5) 2_454 ? Cd1 C7 2.685(7) . ? C1 C6 1.377(11) . ? C1 C2 1.381(12) . ? C1 C7 1.519(10) . ? C2 C3 1.377(12) . ? C2 N1 1.481(15) . ? C3 C4 1.395(11) . ? C3 H3A 0.9500 . ? C4 C5 1.384(11) . ? C4 C8 1.499(10) . ? C5 C6 1.408(11) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 O2 1.231(9) . ? C7 O1 1.241(9) . ? C8 O4 1.263(8) . ? C8 O3 1.270(9) . ? C9 N2 1.318(9) . ? C9 C10 1.394(10) . ? C9 H9A 0.9500 . ? C10 N3 1.344(10) . ? C10 H10A 0.9500 . ? C11 N3 1.363(9) . ? C11 C12 1.389(10) . ? C11 H11A 0.9500 . ? C12 N2 1.293(9) . ? C12 H12A 0.9500 . ? N1 O5 1.214(15) . ? N1 O6 1.257(16) . ? N3 Cd1 2.279(6) 1_455 ? O3 Cd1 2.317(5) 4_566 ? O3 Cd1 2.614(5) 2_444 ? O4 Cd1 2.300(5) 2_444 ? 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 Cd1 O4 91.64(18) 1_655 2_454 ? N3 Cd1 O3 88.14(19) 1_655 4_565 ? O4 Cd1 O3 128.46(18) 2_454 4_565 ? N3 Cd1 O1 97.5(2) 1_655 . ? O4 Cd1 O1 141.23(18) 2_454 . ? O3 Cd1 O1 89.59(18) 4_565 . ? N3 Cd1 O2 89.9(2) 1_655 . ? O4 Cd1 O2 87.8(2) 2_454 . ? O3 Cd1 O2 143.7(2) 4_565 . ? O1 Cd1 O2 54.8(2) . . ? N3 Cd1 N2 174.94(17) 1_655 . ? O4 Cd1 N2 87.76(17) 2_454 . ? O3 Cd1 N2 88.30(17) 4_565 . ? O1 Cd1 N2 86.1(2) . . ? O2 Cd1 N2 95.1(2) . . ? N3 Cd1 O3 90.04(18) 1_655 2_454 ? O4 Cd1 O3 52.98(16) 2_454 2_454 ? O3 Cd1 O3 75.48(19) 4_565 2_454 ? O1 Cd1 O3 163.09(18) . 2_454 ? O2 Cd1 O3 140.79(19) . 2_454 ? N2 Cd1 O3 85.59(16) . 2_454 ? N3 Cd1 C7 95.2(2) 1_655 . ? O4 Cd1 C7 114.3(2) 2_454 . ? O3 Cd1 C7 117.0(2) 4_565 . ? O1 Cd1 C7 27.5(2) . . ? O2 Cd1 C7 27.3(2) . . ? N2 Cd1 C7 89.6(2) . . ? O3 Cd1 C7 166.6(2) 2_454 . ? C6 C1 C2 117.6(7) . . ? C6 C1 C7 119.5(7) . . ? C2 C1 C7 122.7(7) . . ? C3 C2 C1 122.8(8) . . ? C3 C2 N1 114.6(8) . . ? C1 C2 N1 122.0(8) . . ? C2 C3 C4 119.0(7) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 119.9(7) . . ? C5 C4 C8 122.0(6) . . ? C3 C4 C8 118.1(6) . . ? C4 C5 C6 119.1(7) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C1 C6 C5 121.5(7) . . ? C1 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? O2 C7 O1 123.0(7) . . ? O2 C7 C1 118.4(7) . . ? O1 C7 C1 118.6(6) . . ? O2 C7 Cd1 62.3(4) . . ? O1 C7 Cd1 60.8(4) . . ? C1 C7 Cd1 176.7(6) . . ? O4 C8 O3 121.5(7) . . ? O4 C8 C4 118.7(6) . . ? O3 C8 C4 119.7(6) . . ? N2 C9 C10 117.8(6) . . ? N2 C9 H9A 121.1 . . ? C10 C9 H9A 121.1 . . ? N3 C10 C9 122.7(7) . . ? N3 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? N3 C11 C12 121.7(7) . . ? N3 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? N2 C12 C11 119.1(7) . . ? N2 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? O5 N1 O6 127.0(14) . . ? O5 N1 C2 113.5(13) . . ? O6 N1 C2 119.3(12) . . ? C12 N2 C9 123.0(6) . . ? C12 N2 Cd1 119.9(4) . . ? C9 N2 Cd1 117.1(4) . . ? C10 N3 C11 115.7(6) . . ? C10 N3 Cd1 124.4(5) . 1_455 ? C11 N3 Cd1 120.0(5) . 1_455 ? C7 O1 Cd1 91.7(4) . . ? C7 O2 Cd1 90.4(5) . . ? C8 O3 Cd1 169.8(5) . 4_566 ? C8 O3 Cd1 85.2(4) . 2_444 ? Cd1 O3 Cd1 104.52(19) 4_566 2_444 ? C8 O4 Cd1 100.0(4) . 2_444 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.243 _refine_diff_density_min -1.405 _refine_diff_density_rms 0.172 # 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 -0.002 0.387 -0.014 1015 283 ' ' _platon_squeeze_details ; ; #===END data_3'' _database_code_depnum_ccdc_archive 'CCDC 840370' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H14 Cd2 N6 O12' _chemical_formula_weight 803.21 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 P21/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 7.4378(3) _cell_length_b 20.9108(7) _cell_length_c 14.3257(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.650(4) _cell_angle_gamma 90.00 _cell_volume 2225.70(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7224 _exptl_absorpt_correction_T_max 0.8691 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Germioni S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8405 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3864 _reflns_number_gt 3010 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+1.3900P] 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 3864 _refine_ls_number_parameters 200 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.2053 _refine_ls_wR_factor_gt 0.1980 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.098 _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 -0.48840(6) 0.43640(2) -0.39800(3) 0.0302(3) Uani 1 1 d . . . C1 C -0.4898(11) 0.2546(3) -0.2723(5) 0.0430(19) Uani 1 1 d . . . C2 C -0.4951(14) 0.1997(4) -0.3259(5) 0.055(2) Uani 1 1 d DU . . C3 C -0.5021(12) 0.1394(4) -0.2840(6) 0.053(2) Uani 1 1 d U . . H3A H -0.5064 0.1020 -0.3217 0.064 Uiso 1 1 calc R . . C4 C -0.5030(9) 0.1342(3) -0.1891(5) 0.0345(16) Uani 1 1 d . . . C5 C -0.4911(11) 0.1891(3) -0.1336(6) 0.0425(18) Uani 1 1 d . . . H5A H -0.4834 0.1857 -0.0674 0.051 Uiso 1 1 calc R . . C6 C -0.4908(11) 0.2479(3) -0.1760(6) 0.0438(19) Uani 1 1 d . . . H6A H -0.4914 0.2852 -0.1382 0.053 Uiso 1 1 calc R . . C7 C -0.4832(11) 0.3196(3) -0.3167(6) 0.0404(18) Uani 1 1 d . . . C8 C -0.5085(10) 0.0688(3) -0.1463(5) 0.0311(16) Uani 1 1 d . . . C9 C -0.9040(9) 0.4110(4) -0.4686(6) 0.0420(18) Uani 1 1 d . . . H9A H -0.8455 0.3891 -0.5166 0.050 Uiso 1 1 calc R . . C10 C -1.0889(8) 0.4103(4) -0.4695(6) 0.0403(18) Uani 1 1 d . . . H10A H -1.1546 0.3876 -0.5172 0.048 Uiso 1 1 calc R . . C11 C -1.0759(9) 0.4713(4) -0.3402(6) 0.046(2) Uani 1 1 d . . . H11A H -1.1343 0.4943 -0.2931 0.055 Uiso 1 1 calc R . . C12 C -0.8907(9) 0.4710(4) -0.3386(6) 0.047(2) Uani 1 1 d . . . H12A H -0.8249 0.4928 -0.2899 0.057 Uiso 1 1 calc R . . N1 N -0.488(2) 0.1940(6) -0.4355(7) 0.119(4) Uani 1 1 d DU . . N2 N -0.8037(8) 0.4412(2) -0.4032(4) 0.0348(14) Uani 1 1 d U . . N3 N -1.1762(9) 0.4408(3) -0.4051(5) 0.0379(15) Uani 1 1 d U . . O1 O -0.4977(8) 0.3252(3) -0.4012(4) 0.0602(17) Uani 1 1 d U . . O2 O -0.4717(10) 0.3667(4) -0.2659(5) 0.084(2) Uani 1 1 d U . . O3 O -0.5038(9) 0.0616(2) -0.0598(4) 0.0467(14) Uani 1 1 d . . . O4 O -0.5188(7) 0.0212(2) -0.2018(4) 0.0426(13) Uani 1 1 d . . . O5 O -0.645(2) 0.1974(7) -0.4637(10) 0.184(5) Uani 1 1 d U . . O6 O -0.333(2) 0.2033(7) -0.4553(10) 0.191(5) Uani 1 1 d U . . 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 0.0387(4) 0.0178(3) 0.0341(4) 0.00081(19) 0.0035(2) -0.00046(18) C1 0.072(5) 0.025(4) 0.033(4) 0.006(3) 0.001(4) -0.003(3) C2 0.101(6) 0.027(4) 0.035(4) 0.002(3) 0.004(4) -0.006(4) C3 0.097(6) 0.025(4) 0.038(4) 0.008(3) 0.002(4) -0.009(4) C4 0.047(4) 0.019(3) 0.038(4) 0.008(3) 0.002(3) -0.003(3) C5 0.063(5) 0.030(4) 0.035(4) 0.007(3) 0.018(4) 0.006(3) C6 0.075(6) 0.021(3) 0.036(4) -0.002(3) 0.006(4) -0.008(3) C7 0.062(5) 0.015(3) 0.045(5) 0.002(3) 0.012(4) -0.006(3) C8 0.042(4) 0.020(3) 0.032(4) 0.016(3) 0.004(3) 0.000(3) C9 0.022(4) 0.051(4) 0.054(5) -0.020(4) 0.009(3) 0.004(3) C10 0.010(3) 0.047(4) 0.064(5) -0.019(4) 0.002(3) -0.005(3) C11 0.015(3) 0.065(5) 0.058(5) -0.023(4) 0.008(3) 0.000(3) C12 0.021(4) 0.062(5) 0.058(5) -0.017(4) -0.005(3) -0.015(3) N1 0.118(4) 0.117(4) 0.120(4) 0.007(2) 0.006(2) -0.001(2) N2 0.037(2) 0.033(2) 0.035(2) -0.0016(16) 0.0025(17) -0.0007(16) N3 0.040(2) 0.037(2) 0.037(2) -0.0032(16) 0.0029(17) -0.0006(16) O1 0.069(2) 0.054(2) 0.058(2) 0.0031(17) 0.0023(18) -0.0018(17) O2 0.093(3) 0.078(3) 0.081(3) 0.0033(19) 0.0042(19) -0.0018(19) O3 0.067(4) 0.037(3) 0.037(3) 0.012(2) 0.003(3) 0.004(2) O4 0.054(3) 0.027(3) 0.047(3) 0.002(2) 0.005(2) 0.000(2) O5 0.185(7) 0.183(7) 0.181(7) 0.013(5) -0.004(5) -0.023(5) O6 0.199(7) 0.192(7) 0.183(7) 0.010(5) 0.025(5) 0.021(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 Cd1 O4 2.277(5) 2_454 ? Cd1 O3 2.316(6) 4_565 ? Cd1 O1 2.327(7) . ? Cd1 N3 2.331(6) 1_655 ? Cd1 N2 2.345(6) . ? Cd1 O2 2.388(8) . ? Cd1 C7 2.705(7) . ? C1 C2 1.382(11) . ? C1 C6 1.386(11) . ? C1 C7 1.504(9) . ? C2 C3 1.397(10) . ? C2 N1 1.577(9) . ? C3 C4 1.364(10) . ? C3 H3A 0.9500 . ? C4 C5 1.396(10) . ? C4 C8 1.500(8) . ? C5 C6 1.372(10) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 O1 1.216(9) . ? C7 O2 1.224(10) . ? C8 O3 1.246(11) . ? C8 O4 1.275(9) . ? C9 N2 1.330(10) . ? C9 C10 1.375(9) . ? C9 H9A 0.9500 . ? C10 N3 1.317(9) . ? C10 H10A 0.9500 . ? C11 N3 1.327(10) . ? C11 C12 1.377(9) . ? C11 H11A 0.9500 . ? C12 N2 1.311(9) . ? C12 H12A 0.9500 . ? N1 O5 1.215(17) . ? N1 O6 1.217(16) . ? N3 Cd1 2.331(6) 1_455 ? O3 Cd1 2.316(6) 4_566 ? O4 Cd1 2.277(5) 2_444 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O3 127.80(18) 2_454 4_565 ? O4 Cd1 O1 142.2(2) 2_454 . ? O3 Cd1 O1 89.91(19) 4_565 . ? O4 Cd1 N3 90.10(19) 2_454 1_655 ? O3 Cd1 N3 87.7(2) 4_565 1_655 ? O1 Cd1 N3 93.9(2) . 1_655 ? O4 Cd1 N2 88.92(19) 2_454 . ? O3 Cd1 N2 88.0(2) 4_565 . ? O1 Cd1 N2 90.77(19) . . ? N3 Cd1 N2 173.6(2) 1_655 . ? O4 Cd1 O2 88.8(2) 2_454 . ? O3 Cd1 O2 143.4(2) 4_565 . ? O1 Cd1 O2 53.6(2) . . ? N3 Cd1 O2 92.5(2) 1_655 . ? N2 Cd1 O2 93.8(2) . . ? O4 Cd1 C7 115.7(2) 2_454 . ? O3 Cd1 C7 116.5(2) 4_565 . ? O1 Cd1 C7 26.64(19) . . ? N3 Cd1 C7 93.4(2) 1_655 . ? N2 Cd1 C7 92.7(2) . . ? O2 Cd1 C7 26.9(2) . . ? C2 C1 C6 117.9(6) . . ? C2 C1 C7 121.1(7) . . ? C6 C1 C7 121.0(6) . . ? C1 C2 C3 120.7(7) . . ? C1 C2 N1 128.0(7) . . ? C3 C2 N1 111.3(7) . . ? C4 C3 C2 120.2(7) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 119.9(7) . . ? C3 C4 C8 118.8(6) . . ? C5 C4 C8 121.2(7) . . ? C6 C5 C4 119.0(7) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C1 122.1(7) . . ? C5 C6 H6A 118.9 . . ? C1 C6 H6A 118.9 . . ? O1 C7 O2 121.1(7) . . ? O1 C7 C1 120.3(7) . . ? O2 C7 C1 118.5(7) . . ? O1 C7 Cd1 59.1(4) . . ? O2 C7 Cd1 62.0(5) . . ? C1 C7 Cd1 177.3(6) . . ? O3 C8 O4 121.5(6) . . ? O3 C8 C4 121.1(6) . . ? O4 C8 C4 117.3(6) . . ? N2 C9 C10 122.7(6) . . ? N2 C9 H9A 118.6 . . ? C10 C9 H9A 118.6 . . ? N3 C10 C9 120.9(7) . . ? N3 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? N3 C11 C12 122.6(7) . . ? N3 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? N2 C12 C11 121.1(7) . . ? N2 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? O5 N1 O6 144.8(15) . . ? O5 N1 C2 104.7(13) . . ? O6 N1 C2 107.0(13) . . ? C12 N2 C9 116.3(6) . . ? C12 N2 Cd1 121.6(5) . . ? C9 N2 Cd1 122.0(4) . . ? C10 N3 C11 116.3(6) . . ? C10 N3 Cd1 122.4(5) . 1_455 ? C11 N3 Cd1 121.2(5) . 1_455 ? C7 O1 Cd1 94.2(5) . . ? C7 O2 Cd1 91.1(5) . . ? C8 O3 Cd1 171.9(4) . 4_566 ? C8 O4 Cd1 102.6(4) . 2_444 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.698 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.180 # 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 -0.005 0.297 -0.019 1080 316 ' ' _platon_squeeze_details ; ; #===END data_3''' _database_code_depnum_ccdc_archive 'CCDC 840371' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H14 Cd2 N6 O12' _chemical_formula_weight 803.21 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 orthorhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' _cell_length_a 20.993(4) _cell_length_b 14.236(3) _cell_length_c 7.4471(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2225.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7112 _exptl_absorpt_correction_T_max 0.8691 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Germioni S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8407 _diffrn_reflns_av_R_equivalents 0.0844 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2114 _reflns_number_gt 1631 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1322P)^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 2114 _refine_ls_number_parameters 116 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.2027 _refine_ls_wR_factor_gt 0.1951 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.046 _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 -0.43656(3) 0.39829(5) 0.5000 0.0241(3) Uani 1 2 d S . . C1 C -0.2555(5) 0.2745(7) 0.5000 0.029(2) Uani 1 2 d SU . . C2 C -0.2017(6) 0.3271(8) 0.5000 0.053(4) Uani 1 2 d SD . . C3 C -0.1408(6) 0.2868(8) 0.5000 0.041(3) Uani 1 2 d SU . . H3A H -0.1047 0.3247 0.5000 0.050 Uiso 1 2 calc SR . . C4 C -0.1351(5) 0.1902(6) 0.5000 0.020(2) Uani 1 2 d SU . . C5 C -0.1865(8) 0.1400(8) 0.5000 0.059(4) Uani 1 2 d S . . H5A H -0.1823 0.0749 0.5000 0.070 Uiso 1 2 calc SR . . C6 C -0.2473(6) 0.1774(8) 0.5000 0.036(3) Uani 1 2 d SU . . H6A H -0.2826 0.1379 0.5000 0.043 Uiso 1 2 calc SR . . C7 C -0.3205(5) 0.3155(7) 0.5000 0.027(2) Uani 1 2 d SU . . C8 C -0.0683(5) 0.1503(7) 0.5000 0.028(2) Uani 1 2 d SU . . C9 C -0.4123(4) 0.4696(7) 0.9061(12) 0.042(2) Uani 1 1 d . . . H9A H -0.3919 0.5183 0.8459 0.051 Uiso 1 1 calc R . . C10 C -0.4680(5) 0.3367(6) 0.9057(11) 0.046(2) Uani 1 1 d . . . H10A H -0.4884 0.2880 0.8454 0.055 Uiso 1 1 calc R . . N1 N -0.1932(15) 0.4324(17) 0.5000 0.196(12) Uani 1 2 d SDU . . N2 N -0.4401(3) 0.4033(5) 0.8115(10) 0.0346(17) Uani 1 1 d . . . O1 O -0.3257(4) 0.4014(6) 0.5000 0.061(3) Uani 1 2 d S . . O2 O -0.3672(5) 0.2663(6) 0.5000 0.063(3) Uani 1 2 d SU . . O3 O -0.0596(4) 0.0627(7) 0.5000 0.046(2) Uani 1 2 d SU . . O4 O -0.0210(3) 0.2031(5) 0.5000 0.0322(18) Uani 1 2 d SU . . O5 O -0.1995(13) 0.4592(19) 0.342(3) 0.289(12) 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 Cd1 0.0077(4) 0.0370(5) 0.0276(5) 0.000 0.000 0.0009(3) C1 0.023(4) 0.032(4) 0.034(4) 0.000 0.000 -0.001(3) C2 0.024(7) 0.030(6) 0.104(13) 0.000 0.000 0.009(5) C3 0.029(4) 0.043(4) 0.053(5) 0.000 0.000 0.000(4) C4 0.015(4) 0.028(4) 0.016(4) 0.000 0.000 -0.004(3) C5 0.081(12) 0.020(5) 0.075(11) 0.000 0.000 0.009(7) C6 0.030(4) 0.039(4) 0.038(5) 0.000 0.000 -0.006(4) C7 0.012(4) 0.040(4) 0.028(4) 0.000 0.000 0.001(3) C8 0.024(4) 0.030(4) 0.031(4) 0.000 0.000 0.004(3) C9 0.038(5) 0.069(6) 0.020(5) 0.016(4) 0.004(4) -0.006(4) C10 0.059(6) 0.054(5) 0.024(5) -0.008(4) -0.005(4) -0.028(5) N1 0.185(15) 0.209(14) 0.193(15) 0.000 0.000 0.023(9) N2 0.018(3) 0.051(4) 0.035(4) -0.002(3) -0.005(3) -0.003(3) O1 0.022(5) 0.053(5) 0.110(9) 0.000 0.000 0.007(4) O2 0.053(4) 0.055(4) 0.079(5) 0.000 0.000 0.001(4) O3 0.040(4) 0.045(4) 0.054(4) 0.000 0.000 0.006(3) O4 0.017(3) 0.037(3) 0.042(4) 0.000 0.000 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 Cd1 O4 2.286(7) 7_565 ? Cd1 N2 2.322(8) . ? Cd1 N2 2.322(8) 6_556 ? Cd1 O1 2.328(9) . ? Cd1 O3 2.341(9) 3_456 ? Cd1 O2 2.378(10) . ? Cd1 O3 2.643(8) 7_565 ? Cd1 C7 2.706(10) . ? C1 C2 1.354(16) . ? C1 C6 1.393(15) . ? C1 C7 1.485(14) . ? C2 C3 1.402(16) . ? C2 N1 1.51(2) . ? C3 C4 1.381(14) . ? C4 C5 1.294(17) . ? C4 C8 1.513(14) . ? C5 C6 1.384(18) . ? C7 O2 1.204(13) . ? C7 O1 1.228(12) . ? C8 O4 1.246(12) . ? C8 O3 1.261(16) . ? C9 N2 1.315(11) . ? C9 C9 1.399(17) 6_557 ? C10 N2 1.317(11) . ? C10 C10 1.404(17) 6_557 ? N1 O5 1.244(19) 6_556 ? N1 O5 1.244(19) . ? O3 Cd1 2.341(9) 3_446 ? O3 Cd1 2.643(8) 7_665 ? O4 Cd1 2.286(7) 7_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 N2 89.68(15) 7_565 . ? O4 Cd1 N2 89.68(15) 7_565 6_556 ? N2 Cd1 N2 174.9(3) . 6_556 ? O4 Cd1 O1 141.9(3) 7_565 . ? N2 Cd1 O1 91.81(15) . . ? N2 Cd1 O1 91.81(15) 6_556 . ? O4 Cd1 O3 127.2(3) 7_565 3_456 ? N2 Cd1 O3 88.19(16) . 3_456 ? N2 Cd1 O3 88.19(16) 6_556 3_456 ? O1 Cd1 O3 90.9(3) . 3_456 ? O4 Cd1 O2 88.6(3) 7_565 . ? N2 Cd1 O2 92.51(15) . . ? N2 Cd1 O2 92.51(15) 6_556 . ? O1 Cd1 O2 53.3(3) . . ? O3 Cd1 O2 144.2(3) 3_456 . ? O4 Cd1 O3 51.3(3) 7_565 7_565 ? N2 Cd1 O3 87.83(15) . 7_565 ? N2 Cd1 O3 87.83(15) 6_556 7_565 ? O1 Cd1 O3 166.8(3) . 7_565 ? O3 Cd1 O3 75.9(3) 3_456 7_565 ? O2 Cd1 O3 139.9(3) . 7_565 ? O4 Cd1 C7 115.0(3) 7_565 . ? N2 Cd1 C7 92.42(15) . . ? N2 Cd1 C7 92.42(15) 6_556 . ? O1 Cd1 C7 26.9(3) . . ? O3 Cd1 C7 117.8(3) 3_456 . ? O2 Cd1 C7 26.4(3) . . ? O3 Cd1 C7 166.3(3) 7_565 . ? C2 C1 C6 116.5(10) . . ? C2 C1 C7 123.3(10) . . ? C6 C1 C7 120.2(10) . . ? C1 C2 C3 122.3(11) . . ? C1 C2 N1 130.4(16) . . ? C3 C2 N1 107.3(16) . . ? C4 C3 C2 119.1(11) . . ? C5 C4 C3 118.5(11) . . ? C5 C4 C8 124.5(10) . . ? C3 C4 C8 117.0(9) . . ? C4 C5 C6 123.9(11) . . ? C5 C6 C1 119.7(11) . . ? O2 C7 O1 120.6(10) . . ? O2 C7 C1 121.2(10) . . ? O1 C7 C1 118.2(10) . . ? O2 C7 Cd1 61.4(6) . . ? O1 C7 Cd1 59.2(6) . . ? C1 C7 Cd1 177.3(8) . . ? O4 C8 O3 118.9(10) . . ? O4 C8 C4 120.8(9) . . ? O3 C8 C4 120.3(10) . . ? N2 C9 C9 122.4(5) . 6_557 ? N2 C10 C10 122.2(5) . 6_557 ? O5 N1 O5 142(4) 6_556 . ? O5 N1 C2 106.9(19) 6_556 . ? O5 N1 C2 106.9(19) . . ? C9 N2 C10 115.4(8) . . ? C9 N2 Cd1 122.9(6) . . ? C10 N2 Cd1 121.6(5) . . ? C7 O1 Cd1 93.9(7) . . ? C7 O2 Cd1 92.2(7) . . ? C8 O3 Cd1 169.8(8) . 3_446 ? C8 O3 Cd1 86.1(6) . 7_665 ? Cd1 O3 Cd1 104.1(3) 3_446 7_665 ? C8 O4 Cd1 103.7(6) . 7_665 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.817 _refine_diff_density_min -2.123 _refine_diff_density_rms 0.197 # 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 0.291 -0.021 -0.007 1082 489 ' ' _platon_squeeze_details ; ;