# 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 wxt@fjirsm.ac.cn _publ_contact_author_name 'Xin-Tao Wu' loop_ _publ_author_name 'Xintao Wu' 'Qilong Zhu' 'Chaojun Shen' 'Chunhong Tan' 'Tianlu Sheng' 'Shengmin Hu' data_1 _database_code_depnum_ccdc_archive 'CCDC 838864' #TrackingRef 'CCDC 838864.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H33 Cd N7 O8' _chemical_formula_weight 719.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 -0.8080 1.2020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 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 12.943(4) _cell_length_b 12.329(3) _cell_length_c 23.867(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.881(12) _cell_angle_gamma 90.00 _cell_volume 3603.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8690 _cell_measurement_theta_min 3.1473 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5871 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27237 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7817 _reflns_number_gt 6911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. Although there are large solvent accessible voids in the structure; the network is strongly bonded and can maintain its long-range ordering. SQUEEZE is not used here. ; _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^)+(0.1117P)^2^+4.6836P] 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 7817 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1723 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.012 _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 0.25767(2) 0.48046(2) -0.236148(12) 0.03760(13) Uani 1 1 d . . . O1 O 0.1838(2) 0.3169(2) -0.21732(15) 0.0522(7) Uani 1 1 d . . . O2 O 0.2854(2) 0.3050(2) -0.27600(14) 0.0504(7) Uani 1 1 d . . . O3 O 0.1003(3) 0.0140(2) 0.17176(15) 0.0514(8) Uani 1 1 d . . . O4 O 0.2496(2) -0.0768(3) 0.17902(13) 0.0510(7) Uani 1 1 d . . . O5 O 0.5691(3) -0.5807(4) 0.18904(16) 0.0730(11) Uani 1 1 d . . . O6 O 0.6011(3) -0.4309(3) 0.15020(18) 0.0759(11) Uani 1 1 d . . . N1 N 0.1523(3) -0.2685(2) -0.25765(15) 0.0449(8) Uani 1 1 d . . . H1A H 0.2077 -0.2941 -0.2656 0.054 Uiso 1 1 d R . . N2 N 0.1716(2) -0.4056(2) -0.18775(14) 0.0366(6) Uani 1 1 d . . . N3 N 0.0693(3) -0.2446(2) -0.18734(15) 0.0428(7) Uani 1 1 d . . . N4 N 0.0841(3) -0.3812(2) -0.11410(14) 0.0396(7) Uani 1 1 d . . . N5 N -0.0205(3) -0.2266(3) -0.12075(15) 0.0486(8) Uani 1 1 d . . . H5C H -0.0383 -0.1637 -0.1365 0.058 Uiso 1 1 d R . . N6 N 0.1840(3) -0.5339(3) -0.11548(17) 0.0483(8) Uani 1 1 d . . . H6C H 0.2220 -0.5713 -0.1321 0.058 Uiso 1 1 d R . . C1 C 0.1306(3) -0.3066(3) -0.20942(17) 0.0372(7) Uani 1 1 d . . . C2 C 0.0468(3) -0.2867(3) -0.14116(16) 0.0373(7) Uani 1 1 d . . . C3 C 0.1455(3) -0.4375(3) -0.13936(16) 0.0356(7) Uani 1 1 d . . . C4 C 0.0838(4) -0.1851(3) -0.29692(19) 0.0469(9) Uani 1 1 d . . . H4A H 0.0106 -0.1897 -0.2945 0.056 Uiso 1 1 calc R . . H4B H 0.0794 -0.2013 -0.3374 0.056 Uiso 1 1 calc R . . C5 C -0.0644(4) -0.2592(4) -0.0751(2) 0.0546(11) Uani 1 1 d . . . H5A H -0.0569 -0.3372 -0.0699 0.066 Uiso 1 1 calc R . . H5B H -0.1417 -0.2421 -0.0877 0.066 Uiso 1 1 calc R . . C6 C 0.1686(4) -0.5787(4) -0.06314(18) 0.0503(10) Uani 1 1 d . . . H6A H 0.1550 -0.6559 -0.0689 0.060 Uiso 1 1 calc R . . H6B H 0.1045 -0.5459 -0.0576 0.060 Uiso 1 1 calc R . . C7 C 0.2234(3) 0.2624(3) -0.2500(2) 0.0448(9) Uani 1 1 d . . . C8 C 0.1529(3) -0.0504(3) 0.15079(17) 0.0407(8) Uani 1 1 d . . . C9 C 0.5438(4) -0.5129(4) 0.1480(2) 0.0534(11) Uani 1 1 d . . . C10 C 0.1248(3) -0.0700(3) -0.28273(17) 0.0407(8) Uani 1 1 d . . . C11 C 0.1877(4) -0.0218(3) -0.3131(2) 0.0458(9) Uani 1 1 d . . . H11A H 0.2070 -0.0614 -0.3414 0.055 Uiso 1 1 calc R . . C12 C 0.2222(3) 0.0851(3) -0.3016(2) 0.0473(9) Uani 1 1 d . . . H12A H 0.2647 0.1164 -0.3221 0.057 Uiso 1 1 calc R . . C13 C 0.1939(3) 0.1451(3) -0.26004(19) 0.0415(8) Uani 1 1 d . . . C14 C 0.1305(4) 0.0970(3) -0.2295(2) 0.0496(10) Uani 1 1 d . . . H14A H 0.1114 0.1366 -0.2012 0.059 Uiso 1 1 calc R . . C15 C 0.0957(4) -0.0096(3) -0.2412(2) 0.0495(10) Uani 1 1 d . . . H15A H 0.0526 -0.0407 -0.2210 0.059 Uiso 1 1 calc R . . C16 C -0.0085(3) -0.2046(4) -0.01620(19) 0.0471(9) Uani 1 1 d . . . C17 C -0.0649(3) -0.1355(3) 0.0092(2) 0.0485(9) Uani 1 1 d . . . H17A H -0.1387 -0.1224 -0.0100 0.058 Uiso 1 1 calc R . . C18 C -0.0133(3) -0.0859(3) 0.06227(19) 0.0474(9) Uani 1 1 d . . . H18A H -0.0527 -0.0405 0.0789 0.057 Uiso 1 1 calc R . . C19 C 0.0974(3) -0.1027(3) 0.09161(17) 0.0403(8) Uani 1 1 d . . . C20 C 0.1543(4) -0.1706(5) 0.0663(2) 0.0647(14) Uani 1 1 d . . . H20A H 0.2283 -0.1828 0.0854 0.078 Uiso 1 1 calc R . . C21 C 0.1022(4) -0.2207(5) 0.0127(2) 0.0736(17) Uani 1 1 d . . . H21A H 0.1417 -0.2656 -0.0042 0.088 Uiso 1 1 calc R . . C22 C 0.2653(3) -0.5613(3) -0.00782(19) 0.0484(9) Uani 1 1 d . . . C23 C 0.3202(6) -0.4646(5) 0.0047(3) 0.096(3) Uani 1 1 d . . . H23A H 0.2961 -0.4069 -0.0213 0.116 Uiso 1 1 calc R . . C24 C 0.4088(6) -0.4497(5) 0.0540(3) 0.095(2) Uani 1 1 d . . . H24A H 0.4449 -0.3834 0.0600 0.115 Uiso 1 1 calc R . . C25 C 0.4450(4) -0.5302(4) 0.0943(2) 0.0514(10) Uani 1 1 d . . . C26 C 0.3903(4) -0.6282(4) 0.0840(2) 0.0611(12) Uani 1 1 d . . . H26A H 0.4127 -0.6843 0.1113 0.073 Uiso 1 1 calc R . . C27 C 0.3022(4) -0.6426(4) 0.0332(2) 0.0595(12) Uani 1 1 d . . . H27A H 0.2668 -0.7093 0.0265 0.071 Uiso 1 1 calc R . . N7 N 0.4939(3) 0.2289(4) -0.2469(2) 0.0766(14) Uani 1 1 d . . . H7A H 0.4253 0.2530 -0.2643 0.092 Uiso 1 1 calc R . . H7B H 0.5088 0.1805 -0.2715 0.092 Uiso 1 1 calc R . . C29 C 0.5007(6) 0.1746(9) -0.1908(4) 0.121(3) Uani 1 1 d . . . H29A H 0.4495 0.1157 -0.1985 0.181 Uiso 1 1 calc R . . H29B H 0.4839 0.2257 -0.1646 0.181 Uiso 1 1 calc R . . H29C H 0.5733 0.1471 -0.1726 0.181 Uiso 1 1 calc R . . O1W O 0.3657(8) -0.8920(7) 0.1228(5) 0.194(4) Uani 1 1 d . . . O2W O 0.3698(10) -0.1060(12) -0.0362(11) 0.448(14) Uani 1 1 d . . . C28 C 0.5693(6) 0.3198(7) -0.2383(5) 0.134(4) Uani 1 1 d . . . H28A H 0.5621 0.3525 -0.2758 0.201 Uiso 1 1 calc R . . H28B H 0.6428 0.2943 -0.2205 0.201 Uiso 1 1 calc R . . H28C H 0.5527 0.3725 -0.2128 0.201 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04302(18) 0.02680(17) 0.0400(2) 0.00197(9) 0.00930(13) 0.00081(9) O1 0.0609(17) 0.0285(12) 0.072(2) -0.0079(13) 0.0274(16) -0.0047(12) O2 0.0522(16) 0.0324(13) 0.068(2) 0.0043(13) 0.0217(14) -0.0005(12) O3 0.0593(18) 0.0448(16) 0.0453(19) -0.0087(13) 0.0102(15) 0.0094(13) O4 0.0487(15) 0.0593(18) 0.0408(16) -0.0066(13) 0.0086(12) 0.0043(13) O5 0.0555(18) 0.104(3) 0.049(2) 0.020(2) 0.0025(15) -0.0129(19) O6 0.064(2) 0.0529(19) 0.082(3) -0.0022(19) -0.0159(18) -0.0005(16) N1 0.066(2) 0.0257(14) 0.049(2) 0.0031(13) 0.0264(17) 0.0026(13) N2 0.0422(15) 0.0292(14) 0.0374(17) 0.0005(12) 0.0112(13) 0.0017(11) N3 0.0575(19) 0.0286(14) 0.0414(18) 0.0002(13) 0.0150(15) 0.0075(13) N4 0.0483(16) 0.0364(15) 0.0314(16) 0.0009(12) 0.0091(13) 0.0028(13) N5 0.062(2) 0.0470(18) 0.0369(19) -0.0048(14) 0.0154(16) 0.0142(16) N6 0.064(2) 0.0380(17) 0.041(2) 0.0099(14) 0.0147(17) 0.0106(15) C1 0.0465(18) 0.0245(15) 0.039(2) -0.0004(13) 0.0111(15) -0.0018(13) C2 0.0425(18) 0.0339(17) 0.0319(19) -0.0056(14) 0.0071(14) 0.0014(14) C3 0.0389(16) 0.0308(16) 0.0305(18) 0.0022(13) 0.0022(14) 0.0004(13) C4 0.065(2) 0.0294(17) 0.042(2) 0.0026(15) 0.0119(19) 0.0001(16) C5 0.051(2) 0.066(3) 0.045(3) -0.014(2) 0.0144(19) -0.003(2) C6 0.057(2) 0.045(2) 0.041(2) 0.0111(17) 0.0040(18) -0.0048(18) C7 0.0418(18) 0.0306(18) 0.054(2) 0.0048(17) 0.0051(17) -0.0008(15) C8 0.052(2) 0.0338(17) 0.035(2) 0.0018(15) 0.0135(16) -0.0003(15) C9 0.043(2) 0.064(3) 0.046(3) -0.003(2) 0.0060(19) 0.0068(19) C10 0.0484(19) 0.0281(16) 0.042(2) 0.0055(14) 0.0103(16) 0.0038(14) C11 0.059(2) 0.0342(19) 0.048(3) 0.0013(15) 0.024(2) 0.0051(16) C12 0.055(2) 0.0364(19) 0.054(3) 0.0053(17) 0.0224(19) 0.0009(16) C13 0.0452(19) 0.0249(15) 0.054(2) 0.0047(15) 0.0145(17) 0.0040(14) C14 0.063(2) 0.0311(17) 0.061(3) 0.0001(18) 0.030(2) 0.0019(17) C15 0.063(3) 0.0318(18) 0.061(3) 0.0043(18) 0.030(2) 0.0004(17) C16 0.055(2) 0.051(2) 0.039(2) -0.0057(17) 0.0198(17) -0.0019(18) C17 0.0413(19) 0.051(2) 0.053(3) -0.0094(19) 0.0146(17) 0.0001(16) C18 0.049(2) 0.046(2) 0.049(2) -0.0094(18) 0.0183(18) 0.0033(17) C19 0.0461(19) 0.0400(18) 0.036(2) 0.0012(15) 0.0142(15) 0.0017(15) C20 0.045(2) 0.095(4) 0.049(3) -0.019(3) 0.0078(19) 0.018(2) C21 0.057(3) 0.109(4) 0.050(3) -0.030(3) 0.009(2) 0.024(3) C22 0.052(2) 0.043(2) 0.045(2) 0.0064(18) 0.0083(18) -0.0005(17) C23 0.104(5) 0.056(3) 0.083(4) 0.028(3) -0.032(4) -0.019(3) C24 0.102(5) 0.055(3) 0.086(5) 0.017(3) -0.028(4) -0.021(3) C25 0.045(2) 0.057(3) 0.046(3) -0.0002(19) 0.0057(18) 0.0011(17) C26 0.061(3) 0.063(3) 0.048(3) 0.018(2) 0.002(2) -0.008(2) C27 0.067(3) 0.054(2) 0.050(3) 0.013(2) 0.009(2) -0.017(2) N7 0.053(2) 0.088(3) 0.086(4) -0.027(3) 0.019(2) 0.009(2) C29 0.091(5) 0.164(9) 0.100(6) 0.006(6) 0.020(4) 0.048(5) O1W 0.223(9) 0.160(7) 0.250(10) 0.042(7) 0.147(9) -0.028(6) O2W 0.179(10) 0.296(16) 0.93(4) 0.12(2) 0.268(19) -0.070(10) C28 0.086(5) 0.116(6) 0.217(11) -0.067(7) 0.073(6) -0.022(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 N2 2.320(3) 1_565 ? Cd1 O4 2.320(3) 4_565 ? Cd1 O1 2.336(3) . ? Cd1 O6 2.345(3) 3_655 ? Cd1 O2 2.436(3) . ? Cd1 O3 2.467(3) 4_565 ? Cd1 O5 2.488(4) 3_655 ? Cd1 C7 2.727(4) . ? Cd1 C8 2.738(4) 4_565 ? Cd1 C9 2.773(5) 3_655 ? O1 C7 1.258(5) . ? O2 C7 1.275(5) . ? O3 C8 1.250(5) . ? O3 Cd1 2.467(3) 4_566 ? O4 C8 1.257(5) . ? O4 Cd1 2.320(3) 4_566 ? O5 C9 1.247(6) . ? O5 Cd1 2.488(4) 3_655 ? O6 C9 1.245(6) . ? O6 Cd1 2.345(3) 3_655 ? N1 C1 1.354(5) . ? N1 C4 1.477(5) . ? N1 H1A 0.8601 . ? N2 C1 1.364(4) . ? N2 C3 1.362(5) . ? N2 Cd1 2.320(3) 1_545 ? N3 C1 1.328(5) . ? N3 C2 1.333(5) . ? N4 C3 1.338(5) . ? N4 C2 1.343(5) . ? N5 C2 1.349(5) . ? N5 C5 1.441(6) . ? N5 H5C 0.8600 . ? N6 C3 1.342(5) . ? N6 C6 1.437(6) . ? N6 H6C 0.8600 . ? C4 C10 1.515(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C16 1.514(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C22 1.512(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C13 1.496(5) . ? C8 C19 1.507(6) . ? C8 Cd1 2.738(4) 4_566 ? C9 C25 1.505(7) . ? C9 Cd1 2.773(5) 3_655 ? C10 C15 1.384(6) . ? C10 C11 1.387(6) . ? C11 C12 1.391(6) . ? C11 H11A 0.9300 . ? C12 C13 1.378(6) . ? C12 H12A 0.9300 . ? C13 C14 1.393(6) . ? C14 C15 1.389(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.382(6) . ? C16 C21 1.389(6) . ? C17 C18 1.370(6) . ? C17 H17A 0.9300 . ? C18 C19 1.391(6) . ? C18 H18A 0.9300 . ? C19 C20 1.377(6) . ? C20 C21 1.384(7) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.371(7) . ? C22 C27 1.374(6) . ? C23 C24 1.363(8) . ? C23 H23A 0.9300 . ? C24 C25 1.355(7) . ? C24 H24A 0.9300 . ? C25 C26 1.382(7) . ? C26 C27 1.382(7) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? N7 C29 1.475(9) . ? N7 C28 1.456(9) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 O4 103.37(11) 1_565 4_565 ? N2 Cd1 O1 97.73(10) 1_565 . ? O4 Cd1 O1 134.74(11) 4_565 . ? N2 Cd1 O6 94.96(13) 1_565 3_655 ? O4 Cd1 O6 134.36(13) 4_565 3_655 ? O1 Cd1 O6 81.86(13) . 3_655 ? N2 Cd1 O2 152.54(10) 1_565 . ? O4 Cd1 O2 94.85(11) 4_565 . ? O1 Cd1 O2 55.24(10) . . ? O6 Cd1 O2 86.47(12) 3_655 . ? N2 Cd1 O3 92.04(11) 1_565 4_565 ? O4 Cd1 O3 54.36(10) 4_565 4_565 ? O1 Cd1 O3 85.65(11) . 4_565 ? O6 Cd1 O3 166.39(11) 3_655 4_565 ? O2 Cd1 O3 81.97(11) . 4_565 ? N2 Cd1 O5 88.97(13) 1_565 3_655 ? O4 Cd1 O5 85.39(11) 4_565 3_655 ? O1 Cd1 O5 134.97(12) . 3_655 ? O6 Cd1 O5 53.16(13) 3_655 3_655 ? O2 Cd1 O5 113.11(13) . 3_655 ? O3 Cd1 O5 138.81(11) 4_565 3_655 ? N2 Cd1 C7 124.89(12) 1_565 . ? O4 Cd1 C7 116.04(12) 4_565 . ? O1 Cd1 C7 27.40(12) . . ? O6 Cd1 C7 84.21(12) 3_655 . ? O2 Cd1 C7 27.86(11) . . ? O3 Cd1 C7 82.21(11) 4_565 . ? O5 Cd1 C7 129.18(13) 3_655 . ? N2 Cd1 C8 97.79(11) 1_565 4_565 ? O4 Cd1 C8 27.22(11) 4_565 4_565 ? O1 Cd1 C8 110.99(12) . 4_565 ? O6 Cd1 C8 160.36(14) 3_655 4_565 ? O2 Cd1 C8 89.04(11) . 4_565 ? O3 Cd1 C8 27.17(11) 4_565 4_565 ? O5 Cd1 C8 112.07(12) 3_655 4_565 ? C7 Cd1 C8 100.46(12) . 4_565 ? N2 Cd1 C9 90.65(13) 1_565 3_655 ? O4 Cd1 C9 110.91(13) 4_565 3_655 ? O1 Cd1 C9 108.37(14) . 3_655 ? O6 Cd1 C9 26.52(14) 3_655 3_655 ? O2 Cd1 C9 101.95(12) . 3_655 ? O3 Cd1 C9 165.23(13) 4_565 3_655 ? O5 Cd1 C9 26.73(13) 3_655 3_655 ? C7 Cd1 C9 107.98(13) . 3_655 ? C8 Cd1 C9 138.08(14) 4_565 3_655 ? C7 O1 Cd1 93.9(2) . . ? C7 O2 Cd1 88.9(2) . . ? C8 O3 Cd1 88.5(2) . 4_566 ? C8 O4 Cd1 95.2(2) . 4_566 ? C9 O5 Cd1 89.5(3) . 3_655 ? C9 O6 Cd1 96.3(3) . 3_655 ? C1 N1 C4 122.3(3) . . ? C1 N1 H1A 118.5 . . ? C4 N1 H1A 119.1 . . ? C1 N2 C3 114.0(3) . . ? C1 N2 Cd1 122.9(2) . 1_545 ? C3 N2 Cd1 122.6(2) . 1_545 ? C1 N3 C2 114.9(3) . . ? C3 N4 C2 114.0(3) . . ? C2 N5 C5 125.4(4) . . ? C2 N5 H5C 116.8 . . ? C5 N5 H5C 117.9 . . ? C3 N6 C6 124.9(4) . . ? C3 N6 H6C 117.8 . . ? C6 N6 H6C 117.2 . . ? N3 C1 N1 116.8(3) . . ? N3 C1 N2 125.0(3) . . ? N1 C1 N2 118.1(3) . . ? N3 C2 N4 126.5(3) . . ? N3 C2 N5 115.0(3) . . ? N4 C2 N5 118.4(3) . . ? N4 C3 N6 117.5(3) . . ? N4 C3 N2 125.4(3) . . ? N6 C3 N2 117.1(3) . . ? N1 C4 C10 114.6(3) . . ? N1 C4 H4A 108.6 . . ? C10 C4 H4A 108.6 . . ? N1 C4 H4B 108.6 . . ? C10 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N5 C5 C16 113.0(4) . . ? N5 C5 H5A 109.0 . . ? C16 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? C16 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N6 C6 C22 113.3(4) . . ? N6 C6 H6A 108.9 . . ? C22 C6 H6A 108.9 . . ? N6 C6 H6B 108.9 . . ? C22 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O1 C7 O2 121.9(4) . . ? O1 C7 C13 118.8(4) . . ? O2 C7 C13 119.3(4) . . ? O1 C7 Cd1 58.72(19) . . ? O2 C7 Cd1 63.2(2) . . ? C13 C7 Cd1 174.8(3) . . ? O3 C8 O4 121.8(4) . . ? O3 C8 C19 119.4(4) . . ? O4 C8 C19 118.8(3) . . ? O3 C8 Cd1 64.3(2) . 4_566 ? O4 C8 Cd1 57.6(2) . 4_566 ? C19 C8 Cd1 173.0(3) . 4_566 ? O6 C9 O5 120.7(4) . . ? O6 C9 C25 118.7(5) . . ? O5 C9 C25 120.6(4) . . ? O6 C9 Cd1 57.2(2) . 3_655 ? O5 C9 Cd1 63.8(3) . 3_655 ? C25 C9 Cd1 172.0(4) . 3_655 ? C15 C10 C11 119.1(3) . . ? C15 C10 C4 120.5(4) . . ? C11 C10 C4 120.4(4) . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 120.5(4) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 119.1(3) . . ? C12 C13 C7 121.3(4) . . ? C14 C13 C7 119.4(4) . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C10 C15 C14 120.4(4) . . ? C10 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C17 C16 C21 118.5(4) . . ? C17 C16 C5 121.3(4) . . ? C21 C16 C5 120.2(4) . . ? C18 C17 C16 120.7(4) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 120.9(4) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C20 C19 C18 118.6(4) . . ? C20 C19 C8 120.7(4) . . ? C18 C19 C8 120.6(3) . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C16 120.7(4) . . ? C20 C21 H21A 119.6 . . ? C16 C21 H21A 119.6 . . ? C23 C22 C27 116.3(4) . . ? C23 C22 C6 122.6(4) . . ? C27 C22 C6 121.2(4) . . ? C24 C23 C22 122.5(5) . . ? C24 C23 H23A 118.7 . . ? C22 C23 H23A 118.7 . . ? C23 C24 C25 121.0(5) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? C24 C25 C26 118.3(5) . . ? C24 C25 C9 120.3(4) . . ? C26 C25 C9 121.3(4) . . ? C25 C26 C27 119.9(4) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C22 C27 C26 122.0(4) . . ? C22 C27 H27A 119.0 . . ? C26 C27 H27A 119.0 . . ? C29 N7 C28 112.3(7) . . ? C29 N7 H7A 109.1 . . ? C28 N7 H7A 109.1 . . ? C29 N7 H7B 109.1 . . ? C28 N7 H7B 109.1 . . ? H7A N7 H7B 107.9 . . ? 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 . . ? 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 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cd1 O1 C7 172.9(2) 1_565 . . . ? O4 Cd1 O1 C7 55.4(3) 4_565 . . . ? O6 Cd1 O1 C7 -93.1(3) 3_655 . . . ? O2 Cd1 O1 C7 -1.8(2) . . . . ? O3 Cd1 O1 C7 81.5(3) 4_565 . . . ? O5 Cd1 O1 C7 -90.8(3) 3_655 . . . ? C8 Cd1 O1 C7 71.5(3) 4_565 . . . ? C9 Cd1 O1 C7 -93.8(3) 3_655 . . . ? N2 Cd1 O2 C7 -9.7(4) 1_565 . . . ? O4 Cd1 O2 C7 -141.5(2) 4_565 . . . ? O1 Cd1 O2 C7 1.8(2) . . . . ? O6 Cd1 O2 C7 84.3(3) 3_655 . . . ? O3 Cd1 O2 C7 -88.5(2) 4_565 . . . ? O5 Cd1 O2 C7 131.5(2) 3_655 . . . ? C8 Cd1 O2 C7 -114.8(2) 4_565 . . . ? C9 Cd1 O2 C7 105.9(3) 3_655 . . . ? C2 N3 C1 N1 177.8(3) . . . . ? C2 N3 C1 N2 -1.2(5) . . . . ? C4 N1 C1 N3 -21.1(5) . . . . ? C4 N1 C1 N2 157.9(3) . . . . ? C3 N2 C1 N3 -0.8(5) . . . . ? Cd1 N2 C1 N3 171.3(3) 1_545 . . . ? C3 N2 C1 N1 -179.8(3) . . . . ? Cd1 N2 C1 N1 -7.7(5) 1_545 . . . ? C1 N3 C2 N4 3.4(6) . . . . ? C1 N3 C2 N5 -176.4(3) . . . . ? C3 N4 C2 N3 -3.1(5) . . . . ? C3 N4 C2 N5 176.7(3) . . . . ? C5 N5 C2 N3 174.1(4) . . . . ? C5 N5 C2 N4 -5.8(6) . . . . ? C2 N4 C3 N6 -178.7(3) . . . . ? C2 N4 C3 N2 0.7(5) . . . . ? C6 N6 C3 N4 -3.2(6) . . . . ? C6 N6 C3 N2 177.4(4) . . . . ? C1 N2 C3 N4 1.1(5) . . . . ? Cd1 N2 C3 N4 -171.0(3) 1_545 . . . ? C1 N2 C3 N6 -179.5(3) . . . . ? Cd1 N2 C3 N6 8.4(4) 1_545 . . . ? C1 N1 C4 C10 95.0(5) . . . . ? C2 N5 C5 C16 104.1(5) . . . . ? C3 N6 C6 C22 -98.2(5) . . . . ? Cd1 O1 C7 O2 3.3(4) . . . . ? Cd1 O1 C7 C13 -174.7(3) . . . . ? Cd1 O2 C7 O1 -3.1(4) . . . . ? Cd1 O2 C7 C13 174.9(3) . . . . ? N2 Cd1 C7 O1 -8.5(3) 1_565 . . . ? O4 Cd1 C7 O1 -139.4(2) 4_565 . . . ? O6 Cd1 C7 O1 83.5(3) 3_655 . . . ? O2 Cd1 C7 O1 176.9(4) . . . . ? O3 Cd1 C7 O1 -95.6(3) 4_565 . . . ? O5 Cd1 C7 O1 114.1(3) 3_655 . . . ? C8 Cd1 C7 O1 -115.8(3) 4_565 . . . ? C9 Cd1 C7 O1 95.4(3) 3_655 . . . ? N2 Cd1 C7 O2 174.6(2) 1_565 . . . ? O4 Cd1 C7 O2 43.7(3) 4_565 . . . ? O1 Cd1 C7 O2 -176.9(4) . . . . ? O6 Cd1 C7 O2 -93.4(3) 3_655 . . . ? O3 Cd1 C7 O2 87.5(2) 4_565 . . . ? O5 Cd1 C7 O2 -62.7(3) 3_655 . . . ? C8 Cd1 C7 O2 67.3(2) 4_565 . . . ? C9 Cd1 C7 O2 -81.5(3) 3_655 . . . ? Cd1 O3 C8 O4 -3.3(4) 4_566 . . . ? Cd1 O3 C8 C19 173.3(3) 4_566 . . . ? Cd1 O4 C8 O3 3.5(4) 4_566 . . . ? Cd1 O4 C8 C19 -173.1(3) 4_566 . . . ? Cd1 O6 C9 O5 6.5(5) 3_655 . . . ? Cd1 O6 C9 C25 -172.0(4) 3_655 . . . ? Cd1 O5 C9 O6 -6.1(5) 3_655 . . . ? Cd1 O5 C9 C25 172.4(4) 3_655 . . . ? N1 C4 C10 C15 -86.7(5) . . . . ? N1 C4 C10 C11 96.3(5) . . . . ? C15 C10 C11 C12 0.7(7) . . . . ? C4 C10 C11 C12 177.8(4) . . . . ? C10 C11 C12 C13 -0.3(7) . . . . ? C11 C12 C13 C14 0.2(6) . . . . ? C11 C12 C13 C7 -175.7(4) . . . . ? O1 C7 C13 C12 170.9(4) . . . . ? O2 C7 C13 C12 -7.2(6) . . . . ? O1 C7 C13 C14 -5.0(6) . . . . ? O2 C7 C13 C14 177.0(4) . . . . ? C12 C13 C14 C15 -0.5(6) . . . . ? C7 C13 C14 C15 175.5(4) . . . . ? C11 C10 C15 C14 -1.0(7) . . . . ? C4 C10 C15 C14 -178.0(4) . . . . ? C13 C14 C15 C10 0.9(7) . . . . ? N5 C5 C16 C17 116.4(5) . . . . ? N5 C5 C16 C21 -61.6(6) . . . . ? C21 C16 C17 C18 -1.5(7) . . . . ? C5 C16 C17 C18 -179.6(4) . . . . ? C16 C17 C18 C19 0.9(7) . . . . ? C17 C18 C19 C20 -0.2(7) . . . . ? C17 C18 C19 C8 -178.3(4) . . . . ? O3 C8 C19 C20 177.4(4) . . . . ? O4 C8 C19 C20 -5.9(6) . . . . ? O3 C8 C19 C18 -4.5(6) . . . . ? O4 C8 C19 C18 172.2(4) . . . . ? C18 C19 C20 C21 0.1(8) . . . . ? C8 C19 C20 C21 178.3(5) . . . . ? C19 C20 C21 C16 -0.8(10) . . . . ? C17 C16 C21 C20 1.5(9) . . . . ? C5 C16 C21 C20 179.5(5) . . . . ? N6 C6 C22 C23 43.1(7) . . . . ? N6 C6 C22 C27 -137.6(5) . . . . ? C27 C22 C23 C24 2.1(12) . . . . ? C6 C22 C23 C24 -178.6(7) . . . . ? C22 C23 C24 C25 -2.1(14) . . . . ? C23 C24 C25 C26 0.4(12) . . . . ? C23 C24 C25 C9 179.2(7) . . . . ? O6 C9 C25 C24 -11.1(8) . . . . ? O5 C9 C25 C24 170.4(6) . . . . ? O6 C9 C25 C26 167.7(5) . . . . ? O5 C9 C25 C26 -10.8(8) . . . . ? C24 C25 C26 C27 1.1(9) . . . . ? C9 C25 C26 C27 -177.7(5) . . . . ? C23 C22 C27 C26 -0.6(9) . . . . ? C6 C22 C27 C26 -179.9(5) . . . . ? C25 C26 C27 C22 -1.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.296 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.115 # Attachment 'CCDC 838865.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 838865' #TrackingRef 'CCDC 838865.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H31 Cd N7 O7' _chemical_formula_weight 702.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.28(2) _cell_length_b 14.524(10) _cell_length_c 20.084(15) _cell_angle_alpha 90.00 _cell_angle_beta 115.414(11) _cell_angle_gamma 90.00 _cell_volume 7714(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12311 _cell_measurement_theta_min 2.1085 _cell_measurement_theta_max 27.4855 _exptl_crystal_description octahedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2400 _exptl_crystal_size_mid 0.2400 _exptl_crystal_size_min 0.2400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7019 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25354 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.1139 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8737 _reflns_number_gt 5749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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. There are very large solvent accessible voids in the structure because bipy molecules should play crucial template roles under solvothermal condition. The network is strongly bonded, so the porous structure can maintain its long-range ordering. SQUEEZE is not used here. ; _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^)+(0.1893P)^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 8737 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.3054 _refine_ls_wR_factor_gt 0.2071 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.134426(16) 0.48068(3) 0.28729(2) 0.0425(2) Uani 1 1 d . . . N1 N 0.2262(2) 0.6658(4) 0.2118(3) 0.0502(13) Uani 1 1 d . . . N2 N 0.20083(18) 0.5431(4) 0.2684(3) 0.0431(11) Uani 1 1 d . . . N3 N 0.28367(19) 0.6105(4) 0.3299(3) 0.0485(13) Uani 1 1 d . . . N4 N 0.1474(2) 0.5990(4) 0.1530(3) 0.0550(15) Uani 1 1 d . . . H4A H 0.1258 0.5581 0.1519 0.066 Uiso 1 1 calc R . . N5 N 0.3057(2) 0.7267(4) 0.2739(3) 0.0536(15) Uani 1 1 d . . . H5A H 0.2984 0.7633 0.2371 0.064 Uiso 1 1 calc R . . N6 N 0.2604(2) 0.4889(5) 0.3811(3) 0.0639(19) Uani 1 1 d . . . H6A H 0.2420 0.4408 0.3758 0.077 Uiso 1 1 calc R . . N7 N 0.5000 0.2222(9) 0.7500 0.104(4) Uani 1 2 d S . . H7A H 0.4739 0.1855 0.7226 0.125 Uiso 1 1 d R . . N8 N 0.0000 0.3537(10) -0.2500 0.144(7) Uani 1 2 d S . . H8A H 0.0273 0.3906 -0.2323 0.173 Uiso 1 1 d R . . C1 C 0.1927(2) 0.6044(4) 0.2122(3) 0.0428(13) Uani 1 1 d . . . C2 C 0.2701(2) 0.6662(4) 0.2720(3) 0.0409(13) Uani 1 1 d . . . C3 C 0.2477(2) 0.5510(5) 0.3252(3) 0.0484(15) Uani 1 1 d . . . C4 C 0.1349(3) 0.6616(6) 0.0914(3) 0.073(3) Uani 1 1 d . . . H4B H 0.1619 0.6615 0.0755 0.087 Uiso 1 1 calc R . . H4C H 0.1315 0.7237 0.1066 0.087 Uiso 1 1 calc R . . C5 C 0.3557(2) 0.7331(5) 0.3350(3) 0.0541(17) Uani 1 1 d . . . H5B H 0.3774 0.7698 0.3200 0.065 Uiso 1 1 calc R . . H5C H 0.3702 0.6720 0.3473 0.065 Uiso 1 1 calc R . . C6 C 0.3051(4) 0.5040(8) 0.4497(5) 0.113(5) Uani 1 1 d . . . H6B H 0.3004 0.5589 0.4737 0.136 Uiso 1 1 calc R . . H6C H 0.3341 0.5140 0.4392 0.136 Uiso 1 1 calc R . . C7 C -0.0482(2) 0.5440(5) -0.1605(3) 0.0469(14) Uani 1 1 d . . . C8 C 0.3569(3) 0.9074(7) 0.5967(4) 0.066(2) Uani 1 1 d . . . C9 C 0.3501(2) 0.1917(4) 0.6482(3) 0.0462(14) Uani 1 1 d . . . C10 C 0.0853(2) 0.6322(5) 0.0273(3) 0.0552(18) Uani 1 1 d . . . C11 C 0.0383(3) 0.6447(6) 0.0246(3) 0.068(2) Uani 1 1 d . . . H11A H 0.0358 0.6732 0.0644 0.082 Uiso 1 1 calc R . . C12 C -0.0056(3) 0.6175(6) -0.0341(3) 0.0581(18) Uani 1 1 d . . . H12A H -0.0371 0.6281 -0.0346 0.070 Uiso 1 1 calc R . . C13 C -0.0008(2) 0.5728(5) -0.0935(3) 0.0438(14) Uani 1 1 d . . . C14 C 0.0455(3) 0.5566(6) -0.0908(4) 0.0632(19) Uani 1 1 d . . . H14A H 0.0482 0.5249 -0.1292 0.076 Uiso 1 1 calc R . . C15 C 0.0889(3) 0.5866(6) -0.0318(4) 0.063(2) Uani 1 1 d . . . H15A H 0.1204 0.5765 -0.0313 0.076 Uiso 1 1 calc R . . C16 C 0.3538(2) 0.7764(5) 0.4029(3) 0.0503(16) Uani 1 1 d . . . C17 C 0.3289(3) 0.8594(6) 0.3987(4) 0.0594(18) Uani 1 1 d . . . H17A H 0.3115 0.8878 0.3532 0.071 Uiso 1 1 calc R . . C18 C 0.3297(3) 0.8994(6) 0.4604(4) 0.067(2) Uani 1 1 d . . . H18A H 0.3128 0.9549 0.4559 0.080 Uiso 1 1 calc R . . C19 C 0.3546(3) 0.8607(6) 0.5292(4) 0.0581(18) Uani 1 1 d . . . C20 C 0.3789(3) 0.7762(7) 0.5344(4) 0.077(2) Uani 1 1 d . . . H20A H 0.3965 0.7487 0.5802 0.092 Uiso 1 1 calc R . . C21 C 0.3766(3) 0.7334(5) 0.4715(4) 0.064(2) Uani 1 1 d . . . H21A H 0.3906 0.6750 0.4751 0.077 Uiso 1 1 calc R . . C22 C 0.3152(3) 0.4230(6) 0.5009(4) 0.076(3) Uani 1 1 d . . . C23 C 0.3603(3) 0.3790(7) 0.5245(4) 0.081(3) Uani 1 1 d . . . H23A H 0.3843 0.3989 0.5088 0.098 Uiso 1 1 calc R . . C24 C 0.3710(3) 0.3029(6) 0.5728(4) 0.067(2) Uani 1 1 d . . . H24A H 0.4017 0.2723 0.5874 0.080 Uiso 1 1 calc R . . C25 C 0.3380(3) 0.2741(5) 0.5980(3) 0.0496(15) Uani 1 1 d . . . C26 C 0.2909(3) 0.3212(6) 0.5747(4) 0.0609(19) Uani 1 1 d . . . H26A H 0.2674 0.3035 0.5919 0.073 Uiso 1 1 calc R . . C27 C 0.2814(3) 0.3927(6) 0.5267(4) 0.074(2) Uani 1 1 d . . . H27A H 0.2504 0.4225 0.5105 0.088 Uiso 1 1 calc R . . C28 C 0.4825(6) 0.2821(13) 0.8004(11) 0.188(9) Uani 1 1 d . . . H28A H 0.4737 0.2424 0.8312 0.283 Uiso 1 1 calc R . . H28B H 0.4537 0.3184 0.7700 0.283 Uiso 1 1 calc R . . H28C H 0.5096 0.3221 0.8307 0.283 Uiso 1 1 calc R . . C29 C -0.0004(6) 0.3080(12) -0.1894(9) 0.157(6) Uani 1 1 d . . . H29A H -0.0008 0.3523 -0.1541 0.236 Uiso 1 1 calc R . . H29B H 0.0294 0.2704 -0.1671 0.236 Uiso 1 1 calc R . . H29C H -0.0299 0.2699 -0.2050 0.236 Uiso 1 1 calc R . . O1 O -0.09078(17) 0.5636(4) -0.1629(2) 0.0590(13) Uani 1 1 d . . . O1W O 0.3524(7) 0.5983(15) 0.7140(10) 0.288(9) Uiso 1 1 d . . . O2 O -0.0440(2) 0.5048(5) -0.2133(3) 0.0808(19) Uani 1 1 d . . . O3 O 0.3842(3) 0.8790(5) 0.6588(3) 0.086(2) Uani 1 1 d . . . O4 O 0.3345(3) 0.9777(5) 0.5893(4) 0.090(2) Uani 1 1 d . . . O5 O 0.3931(2) 0.1599(4) 0.6747(3) 0.0695(15) Uani 1 1 d . . . O6 O 0.31472(18) 0.1580(3) 0.6624(2) 0.0514(11) 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 0.0439(3) 0.0547(4) 0.0249(3) 0.00211(15) 0.0109(2) -0.00357(18) N1 0.057(3) 0.055(3) 0.031(2) 0.008(2) 0.012(2) -0.011(3) N2 0.036(2) 0.057(3) 0.031(2) 0.009(2) 0.0094(19) -0.004(2) N3 0.045(3) 0.059(3) 0.034(2) 0.008(2) 0.009(2) -0.011(2) N4 0.048(3) 0.069(4) 0.030(2) 0.012(2) 0.000(2) -0.017(3) N5 0.057(3) 0.069(4) 0.028(2) 0.001(2) 0.012(2) -0.021(3) N6 0.054(3) 0.076(4) 0.040(3) 0.025(3) 0.000(3) -0.025(3) N7 0.109(10) 0.081(8) 0.121(11) 0.000 0.048(9) 0.000 N8 0.212(18) 0.085(9) 0.24(2) 0.000 0.199(17) 0.000 C1 0.041(3) 0.054(4) 0.028(2) 0.003(2) 0.009(2) -0.004(3) C2 0.048(3) 0.045(3) 0.029(2) 0.002(2) 0.016(2) -0.008(3) C3 0.050(3) 0.057(4) 0.028(3) 0.008(3) 0.006(2) -0.007(3) C4 0.070(5) 0.084(6) 0.032(3) 0.017(3) -0.008(3) -0.029(4) C5 0.051(4) 0.073(5) 0.036(3) -0.012(3) 0.016(3) -0.016(3) C6 0.096(8) 0.111(7) 0.061(6) 0.052(5) -0.034(5) -0.047(6) C7 0.048(3) 0.052(3) 0.033(3) 0.007(3) 0.009(3) 0.005(3) C8 0.074(5) 0.075(5) 0.047(4) -0.020(4) 0.024(4) -0.017(4) C9 0.057(4) 0.052(4) 0.028(2) 0.003(2) 0.016(2) 0.000(3) C10 0.048(3) 0.073(5) 0.028(3) 0.015(3) 0.000(2) -0.017(3) C11 0.074(5) 0.091(6) 0.026(3) -0.004(3) 0.010(3) -0.005(4) C12 0.048(3) 0.085(5) 0.036(3) 0.000(3) 0.012(3) 0.006(3) C13 0.037(3) 0.060(4) 0.027(2) 0.006(2) 0.007(2) 0.006(3) C14 0.051(4) 0.090(5) 0.044(3) -0.012(4) 0.016(3) 0.002(4) C15 0.035(3) 0.090(6) 0.054(4) 0.004(4) 0.008(3) 0.000(3) C16 0.046(3) 0.064(4) 0.037(3) -0.008(3) 0.014(3) -0.013(3) C17 0.063(4) 0.068(5) 0.037(3) 0.001(3) 0.012(3) 0.005(4) C18 0.068(5) 0.078(5) 0.044(4) -0.010(4) 0.015(3) -0.001(4) C19 0.052(4) 0.074(5) 0.043(3) -0.011(3) 0.016(3) -0.012(4) C20 0.081(6) 0.109(7) 0.029(3) 0.006(4) 0.012(3) -0.003(5) C21 0.079(5) 0.059(4) 0.044(3) -0.002(3) 0.015(3) 0.011(4) C22 0.065(5) 0.090(6) 0.037(3) 0.023(4) -0.013(3) -0.017(4) C23 0.066(5) 0.110(8) 0.062(5) 0.026(5) 0.021(4) -0.016(5) C24 0.057(4) 0.074(5) 0.061(4) 0.022(4) 0.018(4) -0.001(4) C25 0.056(4) 0.054(4) 0.029(3) 0.007(2) 0.009(2) -0.003(3) C26 0.049(4) 0.073(5) 0.053(4) 0.020(3) 0.015(3) 0.001(3) C27 0.049(4) 0.087(6) 0.067(5) 0.030(4) 0.008(4) 0.005(4) C28 0.132(12) 0.188(18) 0.29(3) 0.054(18) 0.138(15) 0.003(13) C29 0.165(14) 0.159(15) 0.156(14) 0.064(12) 0.076(12) 0.028(12) O1 0.044(2) 0.085(4) 0.035(2) 0.008(2) 0.0045(18) -0.008(2) O2 0.056(3) 0.123(5) 0.044(3) -0.026(3) 0.003(3) 0.023(3) O3 0.102(5) 0.103(5) 0.045(3) -0.022(3) 0.023(3) -0.005(4) O4 0.127(6) 0.093(5) 0.054(4) -0.026(3) 0.043(4) -0.006(4) O5 0.066(3) 0.079(4) 0.062(3) 0.026(3) 0.026(3) 0.018(3) O6 0.065(3) 0.053(3) 0.033(2) 0.0007(18) 0.018(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.319(5) . ? Cd1 O4 2.324(6) 7_566 ? Cd1 O1 2.355(5) 5_565 ? Cd1 O2 2.426(6) 5_565 ? Cd1 O5 2.435(6) 7_556 ? Cd1 O6 2.450(5) 7_556 ? Cd1 O3 2.476(7) 7_566 ? Cd1 C7 2.733(6) 5_565 ? Cd1 C8 2.762(8) 7_566 ? N1 C1 1.328(8) . ? N1 C2 1.334(7) . ? N2 C3 1.361(7) . ? N2 C1 1.376(7) . ? N3 C2 1.330(7) . ? N3 C3 1.334(8) . ? N4 C1 1.350(7) . ? N4 C4 1.451(8) . ? N5 C2 1.352(8) . ? N5 C5 1.454(8) . ? N6 C3 1.361(8) . ? N6 C6 1.455(9) . ? N7 C28 1.58(2) . ? N7 C28 1.58(2) 2_656 ? N8 C29 1.391(15) . ? N8 C29 1.391(15) 2_554 ? C4 C10 1.531(8) . ? C5 C16 1.525(9) . ? C6 C22 1.506(11) . ? C7 O2 1.257(9) . ? C7 O1 1.258(8) . ? C7 C13 1.519(8) . ? C7 Cd1 2.733(6) 5_565 ? C8 O4 1.189(11) . ? C8 O3 1.228(10) . ? C8 C19 1.491(10) . ? C8 Cd1 2.762(8) 7_566 ? C9 O5 1.228(8) . ? C9 O6 1.284(8) . ? C9 C25 1.507(8) . ? C10 C11 1.366(11) . ? C10 C15 1.401(11) . ? C11 C12 1.377(9) . ? C12 C13 1.418(9) . ? C13 C14 1.356(9) . ? C14 C15 1.384(9) . ? C16 C17 1.393(11) . ? C16 C21 1.395(9) . ? C17 C18 1.359(10) . ? C18 C19 1.377(11) . ? C19 C20 1.398(13) . ? C20 C21 1.384(11) . ? C22 C23 1.358(13) . ? C22 C27 1.372(12) . ? C23 C24 1.414(11) . ? C24 C25 1.336(10) . ? C25 C26 1.427(10) . ? C26 C27 1.363(10) . ? O1 Cd1 2.355(5) 5_565 ? O2 Cd1 2.426(6) 5_565 ? O3 Cd1 2.476(7) 7_566 ? O4 Cd1 2.324(6) 7_566 ? O5 Cd1 2.435(6) 7_556 ? O6 Cd1 2.450(5) 7_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 N2 Cd1 O4 95.8(2) . 7_566 ? N2 Cd1 O1 92.56(18) . 5_565 ? O4 Cd1 O1 171.2(2) 7_566 5_565 ? N2 Cd1 O2 129.6(2) . 5_565 ? O4 Cd1 O2 117.1(3) 7_566 5_565 ? O1 Cd1 O2 54.65(18) 5_565 5_565 ? N2 Cd1 O5 142.43(19) . 7_556 ? O4 Cd1 O5 85.1(2) 7_566 7_556 ? O1 Cd1 O5 90.06(19) 5_565 7_556 ? O2 Cd1 O5 81.0(2) 5_565 7_556 ? N2 Cd1 O6 89.13(18) . 7_556 ? O4 Cd1 O6 83.3(2) 7_566 7_556 ? O1 Cd1 O6 99.77(17) 5_565 7_556 ? O2 Cd1 O6 129.4(2) 5_565 7_556 ? O5 Cd1 O6 53.56(17) 7_556 7_556 ? N2 Cd1 O3 96.2(2) . 7_566 ? O4 Cd1 O3 51.6(2) 7_566 7_566 ? O1 Cd1 O3 124.6(2) 5_565 7_566 ? O2 Cd1 O3 79.0(2) 5_565 7_566 ? O5 Cd1 O3 112.8(2) 7_556 7_566 ? O6 Cd1 O3 134.86(17) 7_556 7_566 ? N2 Cd1 C7 113.72(19) . 5_565 ? O4 Cd1 C7 144.2(3) 7_566 5_565 ? O1 Cd1 C7 27.36(19) 5_565 5_565 ? O2 Cd1 C7 27.4(2) 5_565 5_565 ? O5 Cd1 C7 83.37(19) 7_556 5_565 ? O6 Cd1 C7 115.55(18) 7_556 5_565 ? O3 Cd1 C7 103.1(2) 7_566 5_565 ? N2 Cd1 C8 97.4(2) . 7_566 ? O4 Cd1 C8 25.2(2) 7_566 7_566 ? O1 Cd1 C8 150.1(2) 5_565 7_566 ? O2 Cd1 C8 98.4(2) 5_565 7_566 ? O5 Cd1 C8 98.7(2) 7_556 7_566 ? O6 Cd1 C8 108.5(2) 7_556 7_566 ? O3 Cd1 C8 26.4(2) 7_566 7_566 ? C7 Cd1 C8 125.2(2) 5_565 7_566 ? C1 N1 C2 115.1(5) . . ? C3 N2 C1 113.0(5) . . ? C3 N2 Cd1 120.7(4) . . ? C1 N2 Cd1 121.6(4) . . ? C2 N3 C3 113.7(5) . . ? C1 N4 C4 120.5(6) . . ? C2 N5 C5 123.4(5) . . ? C3 N6 C6 119.8(6) . . ? C28 N7 C28 113.0(15) . 2_656 ? C29 N8 C29 123.0(19) . 2_554 ? N1 C1 N4 118.8(5) . . ? N1 C1 N2 124.8(5) . . ? N4 C1 N2 116.3(5) . . ? N3 C2 N1 126.9(6) . . ? N3 C2 N5 115.6(5) . . ? N1 C2 N5 117.4(5) . . ? N3 C3 N6 116.3(5) . . ? N3 C3 N2 126.5(5) . . ? N6 C3 N2 117.0(6) . . ? N4 C4 C10 110.1(6) . . ? N5 C5 C16 111.9(6) . . ? N6 C6 C22 111.2(7) . . ? O2 C7 O1 121.6(6) . . ? O2 C7 C13 119.3(6) . . ? O1 C7 C13 119.0(6) . . ? O2 C7 Cd1 62.6(4) . 5_565 ? O1 C7 Cd1 59.4(3) . 5_565 ? C13 C7 Cd1 171.4(5) . 5_565 ? O4 C8 O3 120.0(8) . . ? O4 C8 C19 118.1(8) . . ? O3 C8 C19 121.7(9) . . ? O4 C8 Cd1 56.3(4) . 7_566 ? O3 C8 Cd1 63.7(5) . 7_566 ? C19 C8 Cd1 170.6(6) . 7_566 ? O5 C9 O6 122.4(6) . . ? O5 C9 C25 119.5(6) . . ? O6 C9 C25 118.2(6) . . ? C11 C10 C15 118.0(6) . . ? C11 C10 C4 124.9(7) . . ? C15 C10 C4 117.0(7) . . ? C10 C11 C12 123.4(7) . . ? C11 C12 C13 117.3(6) . . ? C14 C13 C12 120.3(6) . . ? C14 C13 C7 120.4(6) . . ? C12 C13 C7 119.3(6) . . ? C13 C14 C15 121.0(7) . . ? C14 C15 C10 119.9(7) . . ? C17 C16 C21 117.7(6) . . ? C17 C16 C5 121.4(6) . . ? C21 C16 C5 120.9(7) . . ? C18 C17 C16 120.7(7) . . ? C17 C18 C19 122.4(8) . . ? C18 C19 C20 117.8(7) . . ? C18 C19 C8 121.6(8) . . ? C20 C19 C8 120.6(7) . . ? C21 C20 C19 120.2(7) . . ? C20 C21 C16 121.0(8) . . ? C23 C22 C27 118.0(7) . . ? C23 C22 C6 118.9(9) . . ? C27 C22 C6 123.1(9) . . ? C22 C23 C24 120.2(8) . . ? C25 C24 C23 121.4(8) . . ? C24 C25 C26 118.8(6) . . ? C24 C25 C9 120.1(7) . . ? C26 C25 C9 121.1(6) . . ? C27 C26 C25 118.2(7) . . ? C26 C27 C22 123.4(8) . . ? C7 O1 Cd1 93.3(4) . 5_565 ? C7 O2 Cd1 90.0(4) . 5_565 ? C8 O3 Cd1 89.9(6) . 7_566 ? C8 O4 Cd1 98.5(6) . 7_566 ? C9 O5 Cd1 92.0(4) . 7_556 ? C9 O6 Cd1 90.0(4) . 7_556 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.891 _refine_diff_density_min -3.172 _refine_diff_density_rms 0.284