# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_update_record ; 2013-10-10 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H52 Cd3 N8 O14 S2, O4 S, 2(H O0.50), H O0.50' _chemical_formula_sum 'C48 H56 Cd3 N8 O20 S3' _chemical_formula_weight 1498.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.070(3) _cell_length_b 22.001(4) _cell_length_c 20.966(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.07(3) _cell_angle_gamma 90.00 _cell_volume 6370(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25406 _cell_measurement_theta_min 2.4541 _cell_measurement_theta_max 34.7606 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4964 _exptl_absorpt_correction_T_max 0.7216 _exptl_absorpt_process_details 'SADABS, (Sheldrick 2008)' _exptl_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Rigaku _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method dtprofit.ref _diffrn_reflns_number 11150 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11150 _reflns_number_gt 10051 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0454P)^2^+19.0285P] 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 11150 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.002 _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 0.51501(2) 0.744167(17) 0.262178(16) 0.02480(10) Uani 1 1 d . . . Cd2 Cd 0.64014(3) 0.988824(17) 0.19028(2) 0.03163(11) Uani 1 1 d . . . Cd3 Cd 0.32061(3) 0.502884(17) 0.302553(19) 0.03089(11) Uani 1 1 d . . . S1 S 0.51480(9) 0.91389(6) 0.28282(7) 0.0322(3) Uani 1 1 d . . . S2 S 0.51008(9) 0.57758(6) 0.24546(6) 0.0290(3) Uani 1 1 d . . . S3 S 0.20568(10) 0.41736(6) 0.48838(7) 0.0351(3) Uani 1 1 d . . . O1 O 0.4984(3) 0.84829(17) 0.2780(2) 0.0455(10) Uani 1 1 d . . . O2 O 0.4386(4) 0.9422(2) 0.3086(3) 0.0771(16) Uani 1 1 d . . . O3 O 0.6074(4) 0.9289(2) 0.3209(4) 0.106(3) Uani 1 1 d . . . O4 O 0.5092(4) 0.9392(2) 0.2163(2) 0.0631(13) Uani 1 1 d . . . O5 O 0.5404(3) 0.64097(18) 0.2527(2) 0.0469(10) Uani 1 1 d . . . O6 O 0.4180(3) 0.5709(2) 0.2648(3) 0.0741(16) Uani 1 1 d . . . O7 O 0.5791(4) 0.5377(3) 0.2846(3) 0.102(2) Uani 1 1 d . . . O8 O 0.4995(6) 0.5594(3) 0.1790(3) 0.125(3) Uani 1 1 d . . . O9 O 0.2199(3) 0.37892(19) 0.5467(2) 0.0537(11) Uani 1 1 d . . . O10 O 0.1938(3) 0.3786(2) 0.4301(2) 0.0548(12) Uani 1 1 d . . . O11 O 0.1201(3) 0.4552(2) 0.4867(2) 0.0611(13) Uani 1 1 d . . . O12 O 0.2903(3) 0.4561(2) 0.4897(2) 0.0517(11) Uani 1 1 d . . . O13 O 0.7809(4) 0.9726(2) 0.2753(2) 0.0695(14) Uani 1 1 d . . . H13A H 0.8263 0.9959 0.2935 0.083 Uiso 1 1 d R . . H13B H 0.7635 0.9512 0.3048 0.083 Uiso 1 1 d R . . O14 O 0.7387(3) 1.05839(19) 0.1559(2) 0.0485(10) Uani 1 1 d . . . H14A H 0.7510 1.0943 0.1449 0.058 Uiso 1 1 d R . . H14B H 0.7886 1.0368 0.1552 0.058 Uiso 1 1 d R . . O15 O 0.5386(3) 1.0120(2) 0.0933(2) 0.0522(11) Uani 1 1 d . . . H15A H 0.4893 1.0340 0.0795 0.063 Uiso 1 1 d R . . H15B H 0.5700 1.0082 0.0627 0.063 Uiso 1 1 d R . . O16 O 0.4002(3) 0.45190(19) 0.39326(19) 0.0457(10) Uani 1 1 d . . . H16A H 0.3943 0.4475 0.4326 0.055 Uiso 1 1 d R . . H16B H 0.4551 0.4377 0.3897 0.055 Uiso 1 1 d R . . O17 O 0.1972(3) 0.4445(2) 0.3246(2) 0.0524(11) Uani 1 1 d . . . H17A H 0.1854 0.4191 0.3527 0.063 Uiso 1 1 d R . . H17B H 0.1572 0.4378 0.2894 0.063 Uiso 1 1 d R . . O18 O 0.2011(3) 0.5340(2) 0.2140(2) 0.0523(11) Uani 1 1 d . . . H18A H 0.1405 0.5284 0.2027 0.063 Uiso 1 1 d R . . H18B H 0.2221 0.5459 0.1807 0.063 Uiso 1 1 d R . . O19 O 0.2349(5) 0.2571(3) 0.4870(3) 0.0907(19) Uani 1 1 d . . . H19A H 0.2293 0.2774 0.5206 0.109 Uiso 1 1 d R . . H19B H 0.1782 0.2493 0.4662 0.109 Uiso 1 1 d R . . O20 O 0.4450(4) 0.4802(3) 0.5819(3) 0.0325(18) Uani 0.50 1 d P . . H20A H 0.3910 0.4865 0.5567 0.039 Uiso 0.50 1 d PR . . H20B H 0.4334 0.4675 0.6180 0.039 Uiso 0.50 1 d PR . . O21 O 0.2990(7) 0.5397(4) 0.1107(4) 0.051(2) Uani 0.50 1 d P . . H21A H 0.3568 0.5484 0.1285 0.062 Uiso 0.50 1 d PR . . H21B H 0.2947 0.5421 0.0698 0.062 Uiso 0.50 1 d PR . . N1 N 0.3491(3) 0.7434(2) 0.2114(2) 0.0298(10) Uani 1 1 d . . . N2 N -0.0089(3) 0.7701(2) -0.1316(2) 0.0310(10) Uani 1 1 d . . . N3 N -0.2838(3) 0.90870(19) 0.1489(2) 0.0336(10) Uani 1 1 d . . . N4 N -0.0990(3) 0.56963(19) 0.2496(2) 0.0322(10) Uani 1 1 d . . . N5 N 0.6803(3) 0.75166(19) 0.3120(2) 0.0282(9) Uani 1 1 d . . . N6 N 1.0408(3) 0.7430(2) 0.6563(2) 0.0289(9) Uani 1 1 d . . . N7 N 1.2728(3) 0.58423(19) 0.3587(2) 0.0336(10) Uani 1 1 d . . . N8 N 1.1330(3) 0.92773(19) 0.2628(2) 0.0329(10) Uani 1 1 d . . . C1 C 0.2913(4) 0.7919(2) 0.2070(3) 0.0329(12) Uani 1 1 d . . . H1 H 0.3168 0.8281 0.2258 0.039 Uiso 1 1 calc R . . C2 C 0.1952(4) 0.7909(2) 0.1760(3) 0.0342(12) Uani 1 1 d . . . H2 H 0.1576 0.8258 0.1749 0.041 Uiso 1 1 calc R . . C3 C 0.1549(3) 0.7384(2) 0.1468(2) 0.0239(10) Uani 1 1 d . . . C4 C 0.2154(4) 0.6889(2) 0.1504(3) 0.0345(12) Uani 1 1 d . . . H4 H 0.1919 0.6522 0.1315 0.041 Uiso 1 1 calc R . . C5 C 0.3103(4) 0.6931(2) 0.1817(3) 0.0380(13) Uani 1 1 d . . . H5 H 0.3497 0.6591 0.1823 0.046 Uiso 1 1 calc R . . C6 C 0.0506(3) 0.7324(2) 0.1153(2) 0.0220(10) Uani 1 1 d . . . H6 H 0.0420 0.6946 0.0902 0.026 Uiso 1 1 calc R . . C7 C 0.0263(4) 0.8184(3) -0.0982(3) 0.0417(14) Uani 1 1 d . . . H7 H 0.0523 0.8494 -0.1196 0.050 Uiso 1 1 calc R . . C8 C 0.0264(4) 0.8250(3) -0.0322(3) 0.0370(13) Uani 1 1 d . . . H8 H 0.0521 0.8600 -0.0106 0.044 Uiso 1 1 calc R . . C9 C -0.0109(3) 0.7806(2) 0.0010(2) 0.0259(10) Uani 1 1 d . . . C10 C -0.0488(4) 0.7302(3) -0.0344(3) 0.0373(13) Uani 1 1 d . . . H10 H -0.0762 0.6989 -0.0141 0.045 Uiso 1 1 calc R . . C11 C -0.0463(4) 0.7261(3) -0.0995(3) 0.0380(13) Uani 1 1 d . . . H11 H -0.0714 0.6915 -0.1222 0.046 Uiso 1 1 calc R . . C12 C -0.0062(3) 0.7841(2) 0.0734(2) 0.0245(10) Uani 1 1 d . . . H12 H 0.0191 0.8238 0.0897 0.029 Uiso 1 1 calc R . . C13 C -0.2402(4) 0.9133(2) 0.0982(3) 0.0403(14) Uani 1 1 d . . . H13 H -0.2514 0.9479 0.0724 0.048 Uiso 1 1 calc R . . C14 C -0.1790(4) 0.8693(3) 0.0818(3) 0.0377(13) Uani 1 1 d . . . H14 H -0.1491 0.8752 0.0464 0.045 Uiso 1 1 calc R . . C15 C -0.1620(3) 0.8161(2) 0.1181(2) 0.0242(10) Uani 1 1 d . . . C16 C -0.2092(4) 0.8114(2) 0.1704(2) 0.0306(11) Uani 1 1 d . . . H16 H -0.2008 0.7768 0.1964 0.037 Uiso 1 1 calc R . . C17 C -0.2685(4) 0.8578(2) 0.1839(3) 0.0329(12) Uani 1 1 d . . . H17 H -0.2992 0.8533 0.2192 0.039 Uiso 1 1 calc R . . C18 C -0.0962(3) 0.7673(2) 0.1029(2) 0.0229(10) Uani 1 1 d . . . H18 H -0.1345 0.7366 0.0754 0.027 Uiso 1 1 calc R . . C19 C -0.1659(4) 0.5999(2) 0.2076(3) 0.0350(12) Uani 1 1 d . . . H19 H -0.2289 0.5849 0.1989 0.042 Uiso 1 1 calc R . . C20 C -0.1460(4) 0.6524(2) 0.1765(3) 0.0328(12) Uani 1 1 d . . . H20 H -0.1949 0.6715 0.1472 0.039 Uiso 1 1 calc R . . C21 C -0.0534(3) 0.6768(2) 0.1888(2) 0.0239(10) Uani 1 1 d . . . C22 C 0.0160(4) 0.6443(2) 0.2319(2) 0.0298(11) Uani 1 1 d . . . H22 H 0.0795 0.6582 0.2416 0.036 Uiso 1 1 calc R . . C23 C -0.0088(4) 0.5918(2) 0.2601(3) 0.0331(12) Uani 1 1 d . . . H23 H 0.0395 0.5706 0.2878 0.040 Uiso 1 1 calc R . . C24 C -0.0276(3) 0.7352(2) 0.1594(2) 0.0234(10) Uani 1 1 d . . . H24 H -0.0067 0.7647 0.1943 0.028 Uiso 1 1 calc R . . C25 C 0.7112(4) 0.8022(3) 0.3443(3) 0.0406(14) Uani 1 1 d . . . H25 H 0.6665 0.8329 0.3466 0.049 Uiso 1 1 calc R . . C26 C 0.8066(4) 0.8116(2) 0.3748(3) 0.0372(13) Uani 1 1 d . . . H26 H 0.8253 0.8485 0.3950 0.045 Uiso 1 1 calc R . . C27 C 0.8739(3) 0.7657(2) 0.3749(2) 0.0241(10) Uani 1 1 d . . . C28 C 0.8413(4) 0.7124(2) 0.3427(3) 0.0318(12) Uani 1 1 d . . . H28 H 0.8837 0.6801 0.3415 0.038 Uiso 1 1 calc R . . C29 C 0.7451(4) 0.7076(2) 0.3122(3) 0.0329(12) Uani 1 1 d . . . H29 H 0.7247 0.6715 0.2907 0.039 Uiso 1 1 calc R . . C30 C 0.9779(3) 0.7756(2) 0.4070(2) 0.0229(10) Uani 1 1 d . . . H30 H 0.9848 0.8146 0.4298 0.027 Uiso 1 1 calc R . . C31 C 1.0107(4) 0.6920(3) 0.6245(3) 0.0337(12) Uani 1 1 d . . . H31 H 0.9893 0.6600 0.6471 0.040 Uiso 1 1 calc R . . C32 C 1.0102(4) 0.6849(2) 0.5589(2) 0.0308(11) Uani 1 1 d . . . H32 H 0.9893 0.6483 0.5386 0.037 Uiso 1 1 calc R . . C33 C 1.0398(3) 0.7308(2) 0.5233(2) 0.0241(10) Uani 1 1 d . . . C34 C 1.0735(4) 0.7832(2) 0.5573(3) 0.0354(12) Uani 1 1 d . . . H34 H 1.0969 0.8153 0.5359 0.043 Uiso 1 1 calc R . . C35 C 1.0723(4) 0.7876(3) 0.6226(3) 0.0362(13) Uani 1 1 d . . . H35 H 1.0943 0.8233 0.6442 0.043 Uiso 1 1 calc R . . C36 C 1.0327(3) 0.7250(2) 0.4514(2) 0.0222(10) Uani 1 1 d . . . H36 H 1.0054 0.6852 0.4370 0.027 Uiso 1 1 calc R . . C37 C 1.2838(4) 0.6402(2) 0.3370(3) 0.0381(13) Uani 1 1 d . . . H37 H 1.3238 0.6457 0.3069 0.046 Uiso 1 1 calc R . . C38 C 1.2386(4) 0.6903(2) 0.3570(3) 0.0339(12) Uani 1 1 d . . . H38 H 1.2484 0.7284 0.3403 0.041 Uiso 1 1 calc R . . C39 C 1.1786(3) 0.6842(2) 0.4019(2) 0.0247(10) Uani 1 1 d . . . C40 C 1.1712(4) 0.6267(2) 0.4258(3) 0.0371(13) Uani 1 1 d . . . H40 H 1.1342 0.6202 0.4575 0.044 Uiso 1 1 calc R . . C41 C 1.2180(5) 0.5782(3) 0.4033(3) 0.0436(15) Uani 1 1 d . . . H41 H 1.2107 0.5398 0.4201 0.052 Uiso 1 1 calc R . . C42 C 1.1233(3) 0.7376(2) 0.4203(2) 0.0210(10) Uani 1 1 d . . . H42 H 1.1670 0.7668 0.4464 0.025 Uiso 1 1 calc R . . C43 C 1.1987(4) 0.8990(2) 0.3069(3) 0.0355(12) Uani 1 1 d . . . H43 H 1.2623 0.9130 0.3142 0.043 Uiso 1 1 calc R . . C44 C 1.1772(3) 0.8496(2) 0.3422(2) 0.0291(11) Uani 1 1 d . . . H44 H 1.2254 0.8317 0.3730 0.035 Uiso 1 1 calc R . . C45 C 1.0836(3) 0.8267(2) 0.3315(2) 0.0237(10) Uani 1 1 d . . . C46 C 1.0152(4) 0.8584(2) 0.2872(3) 0.0326(12) Uani 1 1 d . . . H46 H 0.9508 0.8461 0.2797 0.039 Uiso 1 1 calc R . . C47 C 1.0416(4) 0.9076(2) 0.2545(3) 0.0333(12) Uani 1 1 d . . . H47 H 0.9940 0.9280 0.2254 0.040 Uiso 1 1 calc R . . C48 C 1.0550(3) 0.7701(2) 0.3627(2) 0.0225(10) Uani 1 1 d . . . H48 H 1.0324 0.7401 0.3286 0.027 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 0.02210(18) 0.0345(2) 0.01836(18) 0.00140(15) 0.00522(13) -0.00285(14) Cd2 0.0336(2) 0.0243(2) 0.0400(2) -0.00551(16) 0.01468(17) 0.00102(15) Cd3 0.0362(2) 0.0238(2) 0.0344(2) -0.00509(16) 0.01110(16) 0.00312(15) S1 0.0253(6) 0.0292(7) 0.0418(8) -0.0025(6) 0.0059(5) 0.0011(5) S2 0.0271(6) 0.0279(7) 0.0336(7) -0.0046(5) 0.0098(5) 0.0010(5) S3 0.0395(7) 0.0354(7) 0.0318(7) -0.0003(6) 0.0107(6) -0.0033(6) O1 0.054(3) 0.029(2) 0.050(3) 0.0004(19) 0.003(2) -0.0048(18) O2 0.075(4) 0.073(4) 0.092(4) -0.012(3) 0.039(3) 0.023(3) O3 0.062(3) 0.045(3) 0.179(7) -0.009(4) -0.060(4) -0.002(3) O4 0.081(3) 0.058(3) 0.056(3) 0.002(2) 0.028(3) -0.024(3) O5 0.058(3) 0.034(2) 0.049(3) -0.0024(19) 0.013(2) -0.0102(19) O6 0.055(3) 0.044(3) 0.137(5) 0.009(3) 0.054(3) -0.003(2) O7 0.062(3) 0.056(3) 0.164(6) 0.022(4) -0.036(4) 0.001(3) O8 0.227(9) 0.094(5) 0.073(4) -0.041(4) 0.074(5) -0.055(5) O9 0.087(3) 0.039(2) 0.038(2) 0.0086(19) 0.021(2) 0.003(2) O10 0.078(3) 0.051(3) 0.040(2) -0.011(2) 0.024(2) -0.019(2) O11 0.052(3) 0.081(4) 0.053(3) 0.007(2) 0.015(2) 0.023(2) O12 0.046(2) 0.053(3) 0.055(3) 0.003(2) 0.007(2) -0.016(2) O13 0.080(4) 0.065(3) 0.058(3) -0.001(3) -0.001(3) 0.009(3) O14 0.045(2) 0.043(2) 0.058(3) 0.010(2) 0.014(2) -0.0094(19) O15 0.037(2) 0.077(3) 0.042(3) 0.001(2) 0.0046(18) -0.003(2) O16 0.039(2) 0.056(3) 0.040(2) 0.007(2) 0.0024(17) 0.0034(19) O17 0.047(2) 0.069(3) 0.038(2) 0.007(2) 0.0011(18) -0.023(2) O18 0.050(3) 0.055(3) 0.048(3) 0.004(2) 0.002(2) 0.010(2) O19 0.132(6) 0.064(4) 0.083(4) -0.009(3) 0.037(4) 0.008(3) O20 0.010(3) 0.062(5) 0.021(3) 0.011(3) -0.008(2) -0.028(3) O21 0.076(6) 0.057(6) 0.023(4) 0.007(4) 0.012(4) -0.014(5) N1 0.024(2) 0.038(3) 0.029(2) -0.0002(19) 0.0066(17) 0.0002(18) N2 0.031(2) 0.040(3) 0.023(2) -0.0017(19) 0.0067(17) -0.0003(19) N3 0.035(2) 0.027(2) 0.040(3) 0.001(2) 0.012(2) 0.0073(19) N4 0.034(2) 0.028(2) 0.036(3) 0.009(2) 0.0109(19) 0.0015(19) N5 0.022(2) 0.035(2) 0.026(2) 0.0009(19) 0.0016(16) 0.0000(18) N6 0.029(2) 0.037(3) 0.022(2) -0.0033(19) 0.0080(17) 0.0012(18) N7 0.040(3) 0.027(2) 0.036(3) -0.001(2) 0.012(2) 0.0051(19) N8 0.036(2) 0.023(2) 0.040(3) 0.004(2) 0.010(2) -0.0009(18) C1 0.028(3) 0.029(3) 0.040(3) -0.006(2) 0.004(2) -0.004(2) C2 0.025(3) 0.030(3) 0.047(3) -0.003(2) 0.007(2) 0.002(2) C3 0.023(2) 0.027(3) 0.022(2) 0.000(2) 0.0053(18) -0.0016(19) C4 0.032(3) 0.031(3) 0.038(3) -0.006(2) 0.000(2) 0.004(2) C5 0.028(3) 0.031(3) 0.052(4) -0.006(3) 0.002(2) 0.008(2) C6 0.022(2) 0.022(2) 0.021(2) -0.0014(19) 0.0024(18) 0.0002(19) C7 0.060(4) 0.039(3) 0.029(3) 0.004(3) 0.014(3) -0.011(3) C8 0.053(4) 0.031(3) 0.028(3) -0.004(2) 0.012(2) -0.007(2) C9 0.025(2) 0.029(3) 0.025(3) 0.001(2) 0.0074(19) 0.004(2) C10 0.044(3) 0.040(3) 0.030(3) -0.003(2) 0.014(2) -0.010(3) C11 0.043(3) 0.044(3) 0.028(3) -0.008(2) 0.010(2) -0.005(3) C12 0.025(2) 0.026(3) 0.022(3) 0.001(2) 0.0047(19) 0.002(2) C13 0.052(4) 0.027(3) 0.046(4) 0.013(3) 0.017(3) 0.013(3) C14 0.045(3) 0.037(3) 0.036(3) 0.009(2) 0.022(3) 0.010(2) C15 0.021(2) 0.026(3) 0.025(3) 0.001(2) 0.0003(18) 0.0043(19) C16 0.036(3) 0.027(3) 0.032(3) 0.009(2) 0.014(2) 0.005(2) C17 0.035(3) 0.034(3) 0.035(3) 0.004(2) 0.019(2) 0.006(2) C18 0.022(2) 0.026(2) 0.021(2) 0.000(2) 0.0046(18) -0.0001(19) C19 0.029(3) 0.033(3) 0.043(3) 0.002(2) 0.008(2) -0.006(2) C20 0.029(3) 0.031(3) 0.036(3) 0.009(2) 0.001(2) 0.004(2) C21 0.027(2) 0.026(3) 0.021(2) 0.002(2) 0.0111(19) 0.001(2) C22 0.029(3) 0.034(3) 0.026(3) 0.005(2) 0.004(2) 0.000(2) C23 0.027(3) 0.034(3) 0.038(3) 0.013(2) 0.005(2) 0.008(2) C24 0.026(2) 0.025(3) 0.020(2) 0.005(2) 0.0064(18) 0.0016(19) C25 0.033(3) 0.036(3) 0.050(4) -0.006(3) 0.000(2) 0.011(2) C26 0.036(3) 0.028(3) 0.044(3) -0.009(2) 0.000(2) 0.005(2) C27 0.022(2) 0.028(3) 0.025(3) 0.006(2) 0.0090(19) -0.0010(19) C28 0.025(3) 0.028(3) 0.042(3) -0.003(2) 0.006(2) 0.002(2) C29 0.031(3) 0.028(3) 0.039(3) -0.005(2) 0.006(2) -0.002(2) C30 0.028(2) 0.022(2) 0.019(2) -0.0026(19) 0.0049(18) 0.0018(19) C31 0.036(3) 0.037(3) 0.030(3) 0.002(2) 0.010(2) -0.007(2) C32 0.042(3) 0.029(3) 0.024(3) -0.002(2) 0.012(2) -0.005(2) C33 0.022(2) 0.028(3) 0.023(2) -0.002(2) 0.0069(18) 0.0012(19) C34 0.047(3) 0.032(3) 0.030(3) 0.001(2) 0.013(2) -0.011(2) C35 0.045(3) 0.038(3) 0.027(3) -0.010(2) 0.011(2) -0.012(3) C36 0.025(2) 0.023(2) 0.019(2) 0.0008(19) 0.0050(18) -0.0009(19) C37 0.044(3) 0.031(3) 0.045(3) -0.003(3) 0.024(3) 0.001(2) C38 0.040(3) 0.021(3) 0.044(3) 0.004(2) 0.017(2) 0.001(2) C39 0.025(2) 0.027(3) 0.020(2) 0.000(2) 0.0004(18) 0.002(2) C40 0.052(3) 0.028(3) 0.037(3) 0.007(2) 0.024(3) 0.010(2) C41 0.069(4) 0.024(3) 0.046(4) 0.009(3) 0.030(3) 0.007(3) C42 0.026(2) 0.020(2) 0.017(2) -0.0002(18) 0.0045(18) -0.0034(19) C43 0.030(3) 0.031(3) 0.045(3) 0.006(2) 0.007(2) -0.003(2) C44 0.026(3) 0.026(3) 0.034(3) 0.005(2) 0.004(2) 0.000(2) C45 0.029(3) 0.021(2) 0.023(2) -0.001(2) 0.0095(19) 0.0002(19) C46 0.025(3) 0.032(3) 0.040(3) 0.005(2) 0.005(2) -0.002(2) C47 0.035(3) 0.027(3) 0.038(3) 0.006(2) 0.007(2) 0.002(2) C48 0.022(2) 0.025(2) 0.021(2) 0.0000(19) 0.0066(18) -0.0026(19) _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 O5 2.313(4) . ? Cd1 O1 2.333(4) . ? Cd1 N6 2.334(4) 4_575 ? Cd1 N2 2.336(4) 4_676 ? Cd1 N5 2.365(4) . ? Cd1 N1 2.373(4) . ? Cd2 O14 2.274(4) . ? Cd2 O4 2.297(4) . ? Cd2 O15 2.306(4) . ? Cd2 N3 2.316(4) 1_655 ? Cd2 N4 2.316(4) 2 ? Cd2 O13 2.423(5) . ? Cd3 O6 2.272(4) . ? Cd3 O17 2.278(4) . ? Cd3 O16 2.305(4) . ? Cd3 N7 2.313(4) 1_455 ? Cd3 N8 2.320(4) 2_645 ? Cd3 O18 2.354(4) . ? S1 O3 1.430(5) . ? S1 O2 1.432(5) . ? S1 O1 1.462(4) . ? S1 O4 1.489(5) . ? S2 O8 1.429(6) . ? S2 O6 1.437(4) . ? S2 O7 1.443(5) . ? S2 O5 1.458(4) . ? S3 O12 1.459(4) . ? S3 O11 1.459(4) . ? S3 O9 1.468(4) . ? S3 O10 1.474(4) . ? O13 H13A 0.8501 . ? O13 H13B 0.8501 . ? O14 H14A 0.8501 . ? O14 H14B 0.8500 . ? O15 H15A 0.8500 . ? O15 H15B 0.8499 . ? O16 H16A 0.8501 . ? O16 H16B 0.8500 . ? O17 H17A 0.8501 . ? O17 H17B 0.8500 . ? O18 H18A 0.8500 . ? O18 H18B 0.8499 . ? O19 H19A 0.8499 . ? O19 H19B 0.8500 . ? O20 H20A 0.8501 . ? O20 H20B 0.8499 . ? O21 H21A 0.8500 . ? O21 H21B 0.8498 . ? N1 C5 1.333(7) . ? N1 C1 1.334(6) . ? N2 C7 1.316(7) . ? N2 C11 1.343(7) . ? N2 Cd1 2.336(4) 4_575 ? N3 C13 1.330(7) . ? N3 C17 1.334(7) . ? N3 Cd2 2.316(4) 1_455 ? N4 C19 1.337(7) . ? N4 C23 1.338(7) . ? N4 Cd2 2.316(4) 2_545 ? N5 C29 1.331(6) . ? N5 C25 1.332(7) . ? N6 C31 1.333(7) . ? N6 C35 1.335(7) . ? N6 Cd1 2.334(4) 4_676 ? N7 C41 1.327(7) . ? N7 C37 1.333(7) . ? N7 Cd3 2.313(4) 1_655 ? N8 C43 1.334(7) . ? N8 C47 1.339(7) . ? N8 Cd3 2.320(4) 2_655 ? C1 C2 1.383(7) . ? C1 H1 0.9300 . ? C2 C3 1.378(7) . ? C2 H2 0.9300 . ? C3 C4 1.376(7) . ? C3 C6 1.496(6) . ? C4 C5 1.373(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C12 1.559(6) . ? C6 C24 1.569(6) . ? C6 H6 0.9800 . ? C7 C8 1.391(7) . ? C7 H7 0.9300 . ? C8 C9 1.364(7) . ? C8 H8 0.9300 . ? C9 C10 1.383(7) . ? C9 C12 1.508(7) . ? C10 C11 1.376(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C18 1.557(6) . ? C12 H12 0.9800 . ? C13 C14 1.382(7) . ? C13 H13 0.9300 . ? C14 C15 1.392(7) . ? C14 H14 0.9300 . ? C15 C16 1.389(7) . ? C15 C18 1.491(6) . ? C16 C17 1.382(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C24 1.548(6) . ? C18 H18 0.9800 . ? C19 C20 1.382(7) . ? C19 H19 0.9300 . ? C20 C21 1.387(7) . ? C20 H20 0.9300 . ? C21 C22 1.393(7) . ? C21 C24 1.500(6) . ? C22 C23 1.373(7) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24 0.9800 . ? C25 C26 1.387(7) . ? C25 H25 0.9300 . ? C26 C27 1.384(7) . ? C26 H26 0.9300 . ? C27 C28 1.387(7) . ? C27 C30 1.504(6) . ? C28 C29 1.386(7) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C36 1.557(6) . ? C30 C48 1.562(6) . ? C30 H30 0.9800 . ? C31 C32 1.383(7) . ? C31 H31 0.9300 . ? C32 C33 1.368(7) . ? C32 H32 0.9300 . ? C33 C34 1.390(7) . ? C33 C36 1.496(6) . ? C34 C35 1.376(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C42 1.564(6) . ? C36 H36 0.9800 . ? C37 C38 1.376(7) . ? C37 H37 0.9300 . ? C38 C39 1.386(7) . ? C38 H38 0.9300 . ? C39 C40 1.373(7) . ? C39 C42 1.499(6) . ? C40 C41 1.382(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C48 1.565(6) . ? C42 H42 0.9800 . ? C43 C44 1.381(7) . ? C43 H43 0.9300 . ? C44 C45 1.387(7) . ? C44 H44 0.9300 . ? C45 C46 1.389(7) . ? C45 C48 1.497(6) . ? C46 C47 1.371(7) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 H48 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 O5 Cd1 O1 175.99(14) . . ? O5 Cd1 N6 89.00(15) . 4_575 ? O1 Cd1 N6 93.08(15) . 4_575 ? O5 Cd1 N2 90.17(15) . 4_676 ? O1 Cd1 N2 87.72(15) . 4_676 ? N6 Cd1 N2 179.01(15) 4_575 4_676 ? O5 Cd1 N5 87.22(15) . . ? O1 Cd1 N5 89.18(14) . . ? N6 Cd1 N5 95.27(14) 4_575 . ? N2 Cd1 N5 84.15(14) 4_676 . ? O5 Cd1 N1 96.28(15) . . ? O1 Cd1 N1 87.36(14) . . ? N6 Cd1 N1 83.88(14) 4_575 . ? N2 Cd1 N1 96.75(15) 4_676 . ? N5 Cd1 N1 176.38(15) . . ? O14 Cd2 O4 164.10(17) . . ? O14 Cd2 O15 83.35(15) . . ? O4 Cd2 O15 85.70(16) . . ? O14 Cd2 N3 92.28(16) . 1_655 ? O4 Cd2 N3 100.18(17) . 1_655 ? O15 Cd2 N3 95.19(16) . 1_655 ? O14 Cd2 N4 83.52(16) . 2 ? O4 Cd2 N4 86.55(16) . 2 ? O15 Cd2 N4 97.64(16) . 2 ? N3 Cd2 N4 165.93(16) 1_655 2 ? O14 Cd2 O13 82.54(17) . . ? O4 Cd2 O13 109.58(19) . . ? O15 Cd2 O13 164.05(17) . . ? N3 Cd2 O13 78.00(16) 1_655 . ? N4 Cd2 O13 88.12(16) 2 . ? O6 Cd3 O17 167.61(18) . . ? O6 Cd3 O16 112.23(18) . . ? O17 Cd3 O16 80.00(15) . . ? O6 Cd3 N7 85.50(17) . 1_455 ? O17 Cd3 N7 91.44(16) . 1_455 ? O16 Cd3 N7 95.69(15) . 1_455 ? O6 Cd3 N8 90.39(17) . 2_645 ? O17 Cd3 N8 91.73(16) . 2_645 ? O16 Cd3 N8 89.62(15) . 2_645 ? N7 Cd3 N8 174.22(16) 1_455 2_645 ? O6 Cd3 O18 85.44(19) . . ? O17 Cd3 O18 82.40(16) . . ? O16 Cd3 O18 162.29(15) . . ? N7 Cd3 O18 86.73(15) 1_455 . ? N8 Cd3 O18 88.90(15) 2_645 . ? O3 S1 O2 110.9(4) . . ? O3 S1 O1 112.4(3) . . ? O2 S1 O1 109.6(3) . . ? O3 S1 O4 108.4(4) . . ? O2 S1 O4 106.4(3) . . ? O1 S1 O4 108.9(3) . . ? O8 S2 O6 108.4(4) . . ? O8 S2 O7 108.5(5) . . ? O6 S2 O7 108.8(4) . . ? O8 S2 O5 110.0(3) . . ? O6 S2 O5 109.2(3) . . ? O7 S2 O5 111.8(3) . . ? O12 S3 O11 109.5(3) . . ? O12 S3 O9 109.9(3) . . ? O11 S3 O9 109.2(3) . . ? O12 S3 O10 108.4(3) . . ? O11 S3 O10 110.4(3) . . ? O9 S3 O10 109.4(3) . . ? S1 O1 Cd1 163.9(3) . . ? S1 O4 Cd2 120.0(3) . . ? S2 O5 Cd1 154.3(3) . . ? S2 O6 Cd3 143.3(3) . . ? Cd2 O13 H13A 132.7 . . ? Cd2 O13 H13B 107.9 . . ? H13A O13 H13B 107.7 . . ? Cd2 O14 H14A 151.6 . . ? Cd2 O14 H14B 100.6 . . ? H14A O14 H14B 107.7 . . ? Cd2 O15 H15A 139.0 . . ? Cd2 O15 H15B 108.7 . . ? H15A O15 H15B 107.7 . . ? Cd3 O16 H16A 137.2 . . ? Cd3 O16 H16B 114.3 . . ? H16A O16 H16B 107.7 . . ? Cd3 O17 H17A 140.2 . . ? Cd3 O17 H17B 108.9 . . ? H17A O17 H17B 107.7 . . ? Cd3 O18 H18A 134.7 . . ? Cd3 O18 H18B 115.5 . . ? H18A O18 H18B 107.7 . . ? H19A O19 H19B 107.7 . . ? H20A O20 H20B 107.7 . . ? H21A O21 H21B 107.7 . . ? C5 N1 C1 116.3(4) . . ? C5 N1 Cd1 119.6(3) . . ? C1 N1 Cd1 124.0(3) . . ? C7 N2 C11 117.3(5) . . ? C7 N2 Cd1 120.5(4) . 4_575 ? C11 N2 Cd1 121.5(4) . 4_575 ? C13 N3 C17 117.0(4) . . ? C13 N3 Cd2 124.0(4) . 1_455 ? C17 N3 Cd2 118.1(3) . 1_455 ? C19 N4 C23 116.9(4) . . ? C19 N4 Cd2 121.6(3) . 2_545 ? C23 N4 Cd2 121.2(3) . 2_545 ? C29 N5 C25 116.7(4) . . ? C29 N5 Cd1 124.5(3) . . ? C25 N5 Cd1 118.7(3) . . ? C31 N6 C35 117.4(4) . . ? C31 N6 Cd1 119.1(3) . 4_676 ? C35 N6 Cd1 122.8(3) . 4_676 ? C41 N7 C37 117.0(5) . . ? C41 N7 Cd3 123.2(4) . 1_655 ? C37 N7 Cd3 118.4(3) . 1_655 ? C43 N8 C47 117.0(5) . . ? C43 N8 Cd3 120.7(3) . 2_655 ? C47 N8 Cd3 122.1(3) . 2_655 ? N1 C1 C2 123.2(5) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 120.2(5) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 116.3(4) . . ? C4 C3 C6 119.9(4) . . ? C2 C3 C6 123.7(4) . . ? C5 C4 C3 120.4(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? N1 C5 C4 123.6(5) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C3 C6 C12 122.6(4) . . ? C3 C6 C24 118.4(4) . . ? C12 C6 C24 87.8(3) . . ? C3 C6 H6 108.7 . . ? C12 C6 H6 108.7 . . ? C24 C6 H6 108.7 . . ? N2 C7 C8 122.9(5) . . ? N2 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C9 C8 C7 120.4(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 116.5(5) . . ? C8 C9 C12 122.1(5) . . ? C10 C9 C12 121.3(5) . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? N2 C11 C10 122.5(5) . . ? N2 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C9 C12 C18 120.4(4) . . ? C9 C12 C6 116.6(4) . . ? C18 C12 C6 88.4(3) . . ? C9 C12 H12 109.9 . . ? C18 C12 H12 109.9 . . ? C6 C12 H12 109.9 . . ? N3 C13 C14 123.4(5) . . ? N3 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 115.8(4) . . ? C16 C15 C18 121.7(4) . . ? C14 C15 C18 122.4(4) . . ? C17 C16 C15 120.4(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? N3 C17 C16 123.2(5) . . ? N3 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C15 C18 C24 119.0(4) . . ? C15 C18 C12 120.0(4) . . ? C24 C18 C12 88.7(3) . . ? C15 C18 H18 109.2 . . ? C24 C18 H18 109.2 . . ? C12 C18 H18 109.2 . . ? N4 C19 C20 123.2(5) . . ? N4 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C19 C20 C21 120.2(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 116.0(5) . . ? C20 C21 C24 123.2(4) . . ? C22 C21 C24 120.8(4) . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? N4 C23 C22 123.2(5) . . ? N4 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? C21 C24 C18 122.7(4) . . ? C21 C24 C6 117.4(4) . . ? C18 C24 C6 88.3(3) . . ? C21 C24 H24 108.9 . . ? C18 C24 H24 108.9 . . ? C6 C24 H24 108.9 . . ? N5 C25 C26 123.5(5) . . ? N5 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C27 C26 C25 119.6(5) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 117.0(4) . . ? C26 C27 C30 120.1(4) . . ? C28 C27 C30 122.8(4) . . ? C29 C28 C27 119.4(5) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? N5 C29 C28 123.7(5) . . ? N5 C29 H29 118.2 . . ? C28 C29 H29 118.2 . . ? C27 C30 C36 119.5(4) . . ? C27 C30 C48 116.8(4) . . ? C36 C30 C48 88.8(3) . . ? C27 C30 H30 110.0 . . ? C36 C30 H30 110.0 . . ? C48 C30 H30 110.0 . . ? N6 C31 C32 122.3(5) . . ? N6 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C33 C32 C31 121.0(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 116.2(5) . . ? C32 C33 C36 121.3(4) . . ? C34 C33 C36 122.5(4) . . ? C35 C34 C33 120.1(5) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? N6 C35 C34 122.9(5) . . ? N6 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? C33 C36 C30 118.1(4) . . ? C33 C36 C42 120.2(4) . . ? C30 C36 C42 88.5(3) . . ? C33 C36 H36 109.4 . . ? C30 C36 H36 109.4 . . ? C42 C36 H36 109.4 . . ? N7 C37 C38 122.9(5) . . ? N7 C37 H37 118.5 . . ? C38 C37 H37 118.5 . . ? C37 C38 C39 120.5(5) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 115.8(5) . . ? C40 C39 C42 123.3(4) . . ? C38 C39 C42 120.9(4) . . ? C39 C40 C41 120.8(5) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? N7 C41 C40 122.9(5) . . ? N7 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? C39 C42 C36 118.3(4) . . ? C39 C42 C48 115.6(4) . . ? C36 C42 C48 88.5(3) . . ? C39 C42 H42 110.9 . . ? C36 C42 H42 110.9 . . ? C48 C42 H42 110.9 . . ? N8 C43 C44 123.3(5) . . ? N8 C43 H43 118.3 . . ? C44 C43 H43 118.3 . . ? C43 C44 C45 119.9(5) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C44 C45 C46 116.1(5) . . ? C44 C45 C48 123.9(4) . . ? C46 C45 C48 119.9(4) . . ? C47 C46 C45 120.7(5) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? N8 C47 C46 122.8(5) . . ? N8 C47 H47 118.6 . . ? C46 C47 H47 118.6 . . ? C45 C48 C30 118.1(4) . . ? C45 C48 C42 122.7(4) . . ? C30 C48 C42 88.3(3) . . ? C45 C48 H48 108.6 . . ? C30 C48 H48 108.6 . . ? C42 C48 H48 108.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.038 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.099 # 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 -0.003 0.500 0.000 505 69 ' ' 2 -0.005 1.000 0.500 505 69 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 966028' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_update_record ; 2013-10-10 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H15 Cd N3 O3, N O3' _chemical_formula_sum 'C18 H15 Cd N4 O6' _chemical_formula_weight 495.74 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 cubic _symmetry_space_group_name_H-M 'I -4 3 m' _symmetry_space_group_name_Hall 'I -4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 15.6677(5) _cell_length_b 15.6677(5) _cell_length_c 15.6677(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3846.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 439 _cell_measurement_theta_min 4.1020 _cell_measurement_theta_max 22.2140 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_T_min 0.7983 _exptl_absorpt_correction_T_max 0.7983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_detector_area_resol_mean 10.3818 _diffrn_reflns_number 1867 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.64 _reflns_number_total 679 _reflns_number_gt 578 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0678P)^2^+11.2291P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.41(14) _refine_ls_number_reflns 679 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 0.68353(5) 0.31647(5) 0.31647(5) 0.0292(4) Uani 1 6 d S . . N1 N 0.7808(4) 0.2192(4) 0.3792(7) 0.037(2) Uani 1 2 d S . . C3 C 0.8923(5) 0.1077(5) 0.4638(7) 0.028(3) Uani 1 2 d S . . C1 C 0.8319(6) 0.1681(6) 0.3381(8) 0.048(4) Uani 1 2 d S . . H1 H 0.8308 0.1692 0.2774 0.058 Uiso 1 2 calc SR . . C5 C 0.7837(6) 0.2163(6) 0.4635(10) 0.060(4) Uani 1 2 d S . . H5 H 0.7473 0.2527 0.4956 0.072 Uiso 1 2 calc SR . . C2 C 0.8885(6) 0.1115(6) 0.3782(8) 0.049(4) Uani 1 2 d S . . H2 H 0.9243 0.0757 0.3447 0.059 Uiso 1 2 calc SR . . C4 C 0.8386(7) 0.1614(7) 0.5066(10) 0.060(5) Uani 1 2 d S . . H4 H 0.8388 0.1612 0.5672 0.071 Uiso 1 2 calc SR . . C6 C 0.9513(5) 0.0487(5) 0.5108(7) 0.027(2) Uani 1 2 d S . . H6 H 0.9435 0.0565 0.5736 0.033 Uiso 1 2 calc SR . . O1 O 0.5792(4) 0.2662(6) 0.4208(4) 0.0362(19) Uani 1 2 d S . . N2 N 0.8948(14) 0.1052(14) 0.1052(14) 0.115(12) Uani 1 6 d S . . O2 O 0.9109(13) 0.0891(13) 0.1755(17) 0.32(2) Uani 1 2 d S . . 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 0.0292(4) 0.0292(4) 0.0292(4) 0.0030(4) -0.0030(4) -0.0030(4) N1 0.034(4) 0.034(4) 0.043(7) 0.000(3) 0.000(3) 0.018(5) C3 0.027(4) 0.027(4) 0.030(7) 0.003(4) -0.003(4) -0.007(5) C1 0.047(5) 0.047(5) 0.049(8) 0.009(4) -0.009(4) 0.005(7) C5 0.064(7) 0.064(7) 0.053(10) 0.002(5) -0.002(5) 0.029(8) C2 0.059(6) 0.059(6) 0.030(8) -0.003(4) 0.003(4) 0.024(8) C4 0.070(8) 0.070(8) 0.038(8) -0.001(4) 0.001(4) 0.029(8) C6 0.026(3) 0.026(3) 0.030(6) 0.004(4) -0.004(4) 0.003(5) O1 0.031(3) 0.046(6) 0.031(3) -0.002(3) -0.003(4) 0.002(3) N2 0.115(12) 0.115(12) 0.115(12) -0.015(12) 0.015(12) 0.015(12) O2 0.43(3) 0.43(3) 0.107(18) 0.031(14) -0.031(14) 0.23(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 N1 2.369(10) . ? Cd1 N1 2.369(10) 7_665 ? Cd1 N1 2.369(10) 10_656 ? Cd1 O1 2.443(8) 10_656 ? Cd1 O1 2.443(8) 7_665 ? Cd1 O1 2.443(8) . ? N1 C1 1.304(16) . ? N1 C5 1.323(18) . ? C3 C2 1.343(17) . ? C3 C4 1.365(19) . ? C3 C6 1.500(15) . ? C1 C2 1.402(18) . ? C1 H1 0.9500 . ? C5 C4 1.392(19) . ? C5 H5 0.9500 . ? C2 H2 0.9500 . ? C4 H4 0.9500 . ? C6 C6 1.563(15) 4_556 ? C6 C6 1.563(15) 3_756 ? C6 H6 1.0000 . ? N2 O2 1.16(3) 7_665 ? N2 O2 1.16(3) 10_656 ? N2 O2 1.16(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 96.9(3) . 7_665 ? N1 Cd1 N1 96.9(3) . 10_656 ? N1 Cd1 N1 96.9(3) 7_665 10_656 ? N1 Cd1 O1 86.9(2) . 10_656 ? N1 Cd1 O1 174.3(4) 7_665 10_656 ? N1 Cd1 O1 86.9(2) 10_656 10_656 ? N1 Cd1 O1 174.3(4) . 7_665 ? N1 Cd1 O1 86.9(2) 7_665 7_665 ? N1 Cd1 O1 86.9(2) 10_656 7_665 ? O1 Cd1 O1 89.1(3) 10_656 7_665 ? N1 Cd1 O1 86.9(2) . . ? N1 Cd1 O1 86.9(2) 7_665 . ? N1 Cd1 O1 174.3(4) 10_656 . ? O1 Cd1 O1 89.1(3) 10_656 . ? O1 Cd1 O1 89.1(3) 7_665 . ? C1 N1 C5 116.9(11) . . ? C1 N1 Cd1 125.8(9) . . ? C5 N1 Cd1 117.3(8) . . ? C2 C3 C4 115.8(12) . . ? C2 C3 C6 123.0(11) . . ? C4 C3 C6 121.2(10) . . ? N1 C1 C2 123.7(12) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? N1 C5 C4 121.8(14) . . ? N1 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C3 C2 C1 120.2(12) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C3 C4 C5 121.6(14) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C3 C6 C6 119.7(8) . 4_556 ? C3 C6 C6 119.7(8) . 3_756 ? C6 C6 C6 87.3(3) 4_556 3_756 ? C3 C6 H6 109.4 . . ? C6 C6 H6 109.4 4_556 . ? C6 C6 H6 109.4 3_756 . ? O2 N2 O2 111(2) 7_665 10_656 ? O2 N2 O2 111(2) 7_665 . ? O2 N2 O2 111(2) 10_656 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.595 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 966029' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_update_record ; 2013-10-10 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Cd2 N4 O14 S2, 2(C H4 O), 3(H2 O)' _chemical_formula_sum 'C26 H46 Cd2 N4 O19 S2' _chemical_formula_weight 1007.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 17.9901(15) _cell_length_b 13.5567(12) _cell_length_c 15.6762(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.684(9) _cell_angle_gamma 90.00 _cell_volume 3821.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3326 _cell_measurement_theta_min 3.2560 _cell_measurement_theta_max 26.9400 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6959 _exptl_absorpt_correction_T_max 0.6959 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 200(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 'Xcalibur, Atlas, Gemini' _diffrn_detector_area_resol_mean 10.4692 _diffrn_measurement_method '\w scans' _diffrn_reflns_number 21880 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1156 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 22077 _reflns_number_gt 14756 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1087P)^2^+48.2089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22077 _refine_ls_number_parameters 475 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1405 _refine_ls_R_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.2610 _refine_ls_wR_factor_gt 0.2354 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.998 _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 0.97026(3) 1.56443(5) 0.80275(4) 0.03258(19) Uani 1 1 d . . . S1 S 1.08452(11) 1.38066(18) 0.89893(15) 0.0374(6) Uani 1 1 d . . . O1 O 1.0250(3) 1.4178(4) 0.8420(4) 0.0431(16) Uani 1 1 d . . . N1 N 0.9330(4) 1.3988(6) 0.2881(5) 0.0394(19) Uani 1 1 d . . . C1 C 0.9448(5) 1.3367(7) 0.3546(7) 0.051(3) Uani 1 1 d . . . H1 H 0.9936 1.3121 0.3649 0.061 Uiso 1 1 calc R . . Cd2 Cd 0.54335(3) 0.94156(5) 0.80342(4) 0.03284(19) Uani 1 1 d . . . S2 S 0.41693(12) 1.11193(18) 0.88984(15) 0.0377(6) Uani 1 1 d . . . O2 O 1.0523(3) 1.3133(5) 0.9616(4) 0.0477(16) Uani 1 1 d . . . N2 N 0.9013(3) 1.4856(5) 0.6976(5) 0.0366(18) Uani 1 1 d . . . C2 C 0.8896(5) 1.3073(10) 0.4081(7) 0.059(3) Uani 1 1 d . . . H2 H 0.9000 1.2637 0.4544 0.071 Uiso 1 1 calc R . . O3 O 1.1211(3) 1.4635(5) 0.9439(4) 0.0403(15) Uani 1 1 d . . . N3 N 0.6094(4) 1.0292(5) 0.7053(5) 0.0370(18) Uani 1 1 d . . . C3 C 0.8168(5) 1.3439(8) 0.3920(7) 0.051(3) Uani 1 1 d U . . O4 O 1.1381(3) 1.3230(6) 0.8494(5) 0.064(2) Uani 1 1 d . . . N4 N 0.5520(3) 1.1030(5) 0.2903(5) 0.0357(18) Uani 1 1 d . . . C4 C 0.8061(5) 1.4089(9) 0.3268(7) 0.053(3) Uani 1 1 d . . . H4 H 0.7584 1.4368 0.3153 0.063 Uiso 1 1 calc R . . O5 O 0.4830(3) 1.0841(5) 0.8418(4) 0.0481(17) Uani 1 1 d . . . C5 C 0.8642(4) 1.4333(8) 0.2786(7) 0.052(3) Uani 1 1 d . . . H5 H 0.8551 1.4793 0.2338 0.062 Uiso 1 1 calc R . . O6 O 0.4369(3) 1.1842(5) 0.9555(4) 0.0472(16) Uani 1 1 d . . . C6 C 0.7473(5) 1.3103(8) 0.4393(7) 0.052(3) Uani 1 1 d . . . H6 H 0.7009 1.3391 0.4130 0.063 Uiso 1 1 calc R . . O7 O 0.3592(3) 1.1532(5) 0.8318(4) 0.0574(19) Uani 1 1 d . . . C7 C 0.9045(6) 1.3855(8) 0.6970(8) 0.067(3) Uani 1 1 d . . . H7 H 0.9409 1.3540 0.7327 0.080 Uiso 1 1 calc R . . O8 O 0.3861(3) 1.0227(5) 0.9316(4) 0.0429(16) Uani 1 1 d . . . C8 C 0.8572(6) 1.3267(9) 0.6468(8) 0.067(3) Uani 1 1 d . . . H8 H 0.8616 1.2569 0.6488 0.081 Uiso 1 1 calc R . . O9 O 1.0376(3) 1.6249(4) 0.9175(4) 0.0484(17) Uani 1 1 d . . . H1W1 H 1.0601 1.5869 0.9529 0.058 Uiso 1 1 d R . . H2W1 H 1.0606 1.6797 0.9178 0.058 Uiso 1 1 d R . . C9 C 0.8053(5) 1.3694(8) 0.5956(6) 0.049(3) Uani 1 1 d . . . O10 O 0.9227(4) 1.7195(5) 0.7824(5) 0.073(2) Uani 1 1 d . . . H1W2 H 0.9084 1.7740 0.7607 0.087 Uiso 1 1 d R . . H2W2 H 0.9252 1.7267 0.8363 0.087 Uiso 1 1 d R . . C10 C 0.8006(6) 1.4698(9) 0.5965(8) 0.068(4) Uani 1 1 d . . . H10 H 0.7650 1.5027 0.5608 0.082 Uiso 1 1 calc R . . O11 O 0.8659(3) 1.5347(5) 0.8828(4) 0.0470(17) Uani 1 1 d . . . H1W3 H 0.8429 1.4958 0.9153 0.056 Uiso 1 1 d R . . H2W3 H 0.8336 1.5694 0.8558 0.056 Uiso 1 1 d R . . C11 C 0.8466(6) 1.5219(9) 0.6483(8) 0.066(3) Uani 1 1 d . . . H11 H 0.8393 1.5913 0.6497 0.079 Uiso 1 1 calc R . . O12 O 0.6407(3) 0.9720(5) 0.8988(4) 0.0460(17) Uani 1 1 d . . . H1W4 H 0.6810 1.0023 0.8892 0.055 Uiso 1 1 d R . . H2W4 H 0.6390 0.9627 0.9523 0.055 Uiso 1 1 d R . . C12 C 0.7445(5) 1.3093(9) 0.5414(7) 0.055(3) Uani 1 1 d . . . H12 H 0.6936 1.3285 0.5595 0.066 Uiso 1 1 calc R . . O13 O 0.4766(3) 0.8690(4) 0.9091(4) 0.0402(15) Uani 1 1 d . . . H1W5 H 0.4350 0.8882 0.9275 0.048 Uiso 1 1 d R . . H2W5 H 0.4948 0.8278 0.9449 0.048 Uiso 1 1 d R . . C13 C 0.6020(6) 1.1269(8) 0.7020(7) 0.055(3) Uani 1 1 d . . . H13 H 0.5680 1.1585 0.7383 0.066 Uiso 1 1 calc R . . O14 O 0.6020(5) 0.7924(6) 0.7848(5) 0.092(3) Uani 1 1 d . . . H1W6 H 0.6194 0.8009 0.8353 0.110 Uiso 1 1 d R . . H2W6 H 0.6224 0.7412 0.7647 0.110 Uiso 1 1 d R . . C14 C 0.6433(6) 1.1839(8) 0.6462(8) 0.062(3) Uani 1 1 d . . . H14 H 0.6347 1.2530 0.6434 0.074 Uiso 1 1 calc R . . C15 C 0.6954(5) 1.1436(9) 0.5958(6) 0.049(3) Uani 1 1 d . . . O15 O 0.6186(8) 0.6607(11) 0.9308(8) 0.166(5) Uani 1 1 d . . . H15O H 0.6144 0.7139 0.9589 0.199 Uiso 1 1 d R . . C16 C 0.7047(6) 1.0426(9) 0.6022(8) 0.066(3) Uani 1 1 d . . . H16 H 0.7422 1.0104 0.5711 0.080 Uiso 1 1 calc R . . O16 O 1.1015(5) 1.1733(7) 1.0676(5) 0.084(3) Uani 1 1 d U . . H16O H 1.0923 1.2244 1.0378 0.101 Uiso 1 1 d R . . C17 C 0.6599(5) 0.9898(8) 0.6534(7) 0.049(3) Uani 1 1 d . . . H17 H 0.6646 0.9200 0.6525 0.059 Uiso 1 1 calc R . . O17 O 0.7473(5) 0.8274(8) 0.9153(6) 0.109(3) Uani 1 1 d . . . H1W7 H 0.7305 0.8779 0.8890 0.131 Uiso 1 1 d R . . H2W7 H 0.7941 0.8260 0.9094 0.131 Uiso 1 1 d R . . C18 C 0.7521(5) 1.1994(9) 0.5435(6) 0.053(3) Uani 1 1 d . . . H18 H 0.8039 1.1801 0.5616 0.064 Uiso 1 1 calc R . . O18 O 0.7486(4) 1.6352(8) 0.8140(7) 0.112(4) Uani 1 1 d . . . H1W8 H 0.7493 1.6426 0.7602 0.134 Uiso 1 1 d R . . H2W8 H 0.7089 1.6044 0.8254 0.134 Uiso 1 1 d R . . C19 C 0.6230(6) 1.0793(10) 0.2771(7) 0.065(3) Uani 1 1 d . . . H19 H 0.6315 1.0412 0.2274 0.079 Uiso 1 1 calc R . . O19 O 0.2702(4) 1.2697(7) 0.9333(5) 0.084(3) Uani 1 1 d . . . H1W9 H 0.2289 1.2696 0.9055 0.101 Uiso 1 1 d R . . H2W9 H 0.3044 1.2598 0.8981 0.101 Uiso 1 1 d R . . C20 C 0.6828(6) 1.1020(10) 0.3240(7) 0.065(3) Uani 1 1 d . . . H20 H 0.7302 1.0771 0.3098 0.078 Uiso 1 1 calc R . . C21 C 0.6749(6) 1.1635(9) 0.3952(7) 0.057(3) Uani 1 1 d . . . C22 C 0.6018(6) 1.1891(8) 0.4111(7) 0.053(3) Uani 1 1 d . . . H22 H 0.5923 1.2292 0.4592 0.063 Uiso 1 1 calc R . . C23 C 0.5423(5) 1.1588(7) 0.3598(6) 0.046(2) Uani 1 1 d . . . H23 H 0.4934 1.1779 0.3741 0.055 Uiso 1 1 calc R . . C24 C 0.7431(5) 1.1987(9) 0.4435(7) 0.051(3) Uani 1 1 d . . . H24 H 0.7884 1.1694 0.4181 0.061 Uiso 1 1 calc R . . C25 C 0.5652(12) 0.5998(17) 0.9416(13) 0.166(5) Uani 1 1 d . . . H25A H 0.5693 0.5720 0.9992 0.249 Uiso 1 1 calc R . . H25B H 0.5679 0.5466 0.8995 0.249 Uiso 1 1 calc R . . H25C H 0.5175 0.6343 0.9343 0.249 Uiso 1 1 calc R . . C26 C 1.0550(8) 1.0922(13) 1.0524(12) 0.117(6) Uani 1 1 d U . . H26A H 1.0161 1.0911 1.0948 0.175 Uiso 1 1 calc R . . H26B H 1.0843 1.0313 1.0567 0.175 Uiso 1 1 calc R . . H26C H 1.0321 1.0974 0.9951 0.175 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 0.0354(3) 0.0264(4) 0.0361(4) -0.0008(3) 0.0027(3) -0.0006(3) S1 0.0414(11) 0.0347(14) 0.0361(13) -0.0045(12) -0.0015(10) 0.0125(11) O1 0.057(3) 0.026(4) 0.046(4) -0.001(3) -0.014(3) -0.006(3) N1 0.037(4) 0.044(5) 0.037(5) 0.000(4) 0.005(3) -0.003(4) C1 0.037(5) 0.033(6) 0.083(8) 0.012(6) -0.005(5) -0.011(4) Cd2 0.0366(3) 0.0276(4) 0.0343(4) -0.0003(3) 0.0016(3) -0.0009(3) S2 0.0440(12) 0.0297(13) 0.0394(14) 0.0037(11) 0.0045(10) 0.0076(10) O2 0.061(4) 0.028(4) 0.054(4) 0.003(3) 0.002(3) 0.011(3) N2 0.036(4) 0.029(4) 0.044(5) -0.006(4) -0.005(3) -0.007(3) C2 0.066(6) 0.079(9) 0.031(6) 0.005(6) 0.003(5) -0.015(6) O3 0.039(3) 0.040(4) 0.041(4) -0.003(3) 0.000(3) 0.001(3) N3 0.041(4) 0.023(4) 0.048(5) 0.003(4) 0.017(3) -0.007(3) C3 0.033(4) 0.066(6) 0.053(6) -0.016(5) -0.012(4) -0.032(4) O4 0.057(4) 0.077(6) 0.059(5) -0.022(4) 0.013(3) 0.026(4) N4 0.026(3) 0.034(4) 0.046(5) -0.003(4) -0.009(3) -0.008(3) C4 0.036(5) 0.076(8) 0.046(7) 0.003(6) -0.007(4) -0.006(5) O5 0.046(3) 0.032(4) 0.068(5) 0.000(3) 0.022(3) 0.010(3) C5 0.036(5) 0.061(7) 0.058(7) 0.009(6) 0.007(4) -0.003(5) O6 0.068(4) 0.036(4) 0.038(4) -0.004(3) 0.003(3) 0.011(3) C6 0.058(6) 0.041(7) 0.057(7) -0.003(6) -0.010(5) 0.005(5) O7 0.056(4) 0.059(5) 0.057(5) 0.016(4) -0.001(3) -0.007(4) C7 0.086(8) 0.042(7) 0.070(8) -0.002(7) -0.042(6) 0.014(6) O8 0.042(3) 0.036(4) 0.051(4) 0.009(3) 0.007(3) 0.007(3) C8 0.096(8) 0.038(7) 0.067(8) -0.009(6) -0.011(7) -0.018(6) O9 0.067(4) 0.019(3) 0.058(4) -0.003(3) -0.015(3) -0.013(3) C9 0.072(6) 0.047(7) 0.029(5) -0.002(5) -0.011(5) -0.020(6) O10 0.126(6) 0.045(5) 0.047(5) 0.015(4) 0.012(4) 0.045(4) C10 0.066(7) 0.052(8) 0.086(9) 0.009(7) -0.030(6) -0.017(6) O11 0.032(3) 0.050(4) 0.060(5) 0.012(4) 0.008(3) -0.005(3) C11 0.075(7) 0.053(8) 0.068(8) -0.003(7) -0.014(6) -0.008(6) O12 0.038(3) 0.069(5) 0.031(3) 0.011(3) 0.003(2) -0.012(3) C12 0.059(6) 0.054(8) 0.051(7) -0.010(6) -0.001(5) 0.026(5) O13 0.043(3) 0.034(4) 0.044(4) 0.009(3) 0.004(3) -0.006(3) C13 0.078(7) 0.043(7) 0.045(6) 0.014(6) 0.030(5) 0.020(6) O14 0.163(8) 0.067(6) 0.045(5) -0.012(4) -0.009(5) 0.067(6) C14 0.079(7) 0.028(6) 0.079(9) 0.017(6) 0.002(6) -0.003(6) C15 0.044(5) 0.065(8) 0.038(6) -0.010(6) 0.012(4) -0.026(5) O15 0.227(13) 0.159(13) 0.113(8) -0.062(8) 0.041(8) -0.093(9) C16 0.068(7) 0.058(9) 0.075(9) -0.014(7) 0.031(6) -0.007(6) O16 0.131(7) 0.058(6) 0.064(6) 0.011(5) 0.000(5) 0.008(5) C17 0.054(5) 0.039(6) 0.054(7) 0.002(5) 0.013(5) 0.001(5) O17 0.115(7) 0.105(9) 0.106(8) 0.004(7) -0.012(6) 0.028(6) C18 0.062(6) 0.056(7) 0.041(6) 0.000(6) 0.007(5) 0.008(6) O18 0.080(5) 0.132(9) 0.122(8) -0.026(7) -0.033(5) 0.050(6) C19 0.074(7) 0.090(10) 0.031(6) -0.004(6) -0.016(5) -0.024(7) O19 0.056(4) 0.109(8) 0.087(6) -0.021(6) 0.001(4) 0.034(5) C20 0.060(6) 0.087(10) 0.049(7) 0.000(7) -0.002(5) -0.010(6) C21 0.064(6) 0.057(8) 0.050(7) 0.005(6) 0.006(5) -0.032(6) C22 0.077(7) 0.035(6) 0.046(6) -0.015(5) 0.004(5) -0.001(5) C23 0.063(6) 0.040(6) 0.034(6) -0.002(5) 0.006(5) -0.008(5) C24 0.055(5) 0.050(7) 0.049(6) -0.001(6) 0.010(4) 0.004(5) C25 0.227(13) 0.159(13) 0.113(8) -0.062(8) 0.041(8) -0.093(9) C26 0.118(11) 0.084(12) 0.149(16) 0.053(11) -0.004(10) -0.013(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O10 2.288(7) . ? Cd1 O9 2.291(6) . ? Cd1 O1 2.295(6) . ? Cd1 N2 2.298(7) . ? Cd1 O11 2.324(6) . ? Cd1 N1 2.335(7) 3_786 ? S1 O1 1.462(6) . ? S1 O3 1.472(6) . ? S1 O2 1.472(7) . ? S1 O4 1.479(7) . ? N1 C5 1.327(11) . ? N1 C1 1.352(12) . ? N1 Cd1 2.335(7) 3_786 ? C1 C2 1.378(13) . ? C1 H1 0.9500 . ? Cd2 O13 2.297(6) . ? Cd2 N3 2.300(7) . ? Cd2 O14 2.304(7) . ? Cd2 O5 2.306(6) . ? Cd2 N4 2.307(6) 3_676 ? Cd2 O12 2.307(5) . ? S2 O6 1.458(7) . ? S2 O7 1.471(7) . ? S2 O5 1.474(6) . ? S2 O8 1.490(7) . ? N2 C11 1.328(12) . ? N2 C7 1.359(13) . ? C2 C3 1.416(14) . ? C2 H2 0.9500 . ? N3 C13 1.332(12) . ? N3 C17 1.349(12) . ? C3 C4 1.360(15) . ? C3 C6 1.541(14) . ? N4 C19 1.339(13) . ? N4 C23 1.342(12) . ? N4 Cd2 2.307(6) 3_676 ? C4 C5 1.348(13) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C24 1.516(13) . ? C6 C12 1.603(14) . ? C6 H6 1.0000 . ? C7 C8 1.392(15) . ? C7 H7 0.9500 . ? C8 C9 1.345(14) . ? C8 H8 0.9500 . ? O9 H1W1 0.8501 . ? O9 H2W1 0.8500 . ? C9 C10 1.364(15) . ? C9 C12 1.589(14) . ? O10 H1W2 0.8499 . ? O10 H2W2 0.8500 . ? C10 C11 1.343(15) . ? C10 H10 0.9500 . ? O11 H1W3 0.8499 . ? O11 H2W3 0.8501 . ? C11 H11 0.9500 . ? O12 H1W4 0.8503 . ? O12 H2W4 0.8500 . ? C12 C18 1.497(14) . ? C12 H12 1.0000 . ? O13 H1W5 0.8501 . ? O13 H2W5 0.8500 . ? C13 C14 1.397(14) . ? C13 H13 0.9500 . ? O14 H1W6 0.8499 . ? O14 H2W6 0.8499 . ? C14 C15 1.359(15) . ? C14 H14 0.9500 . ? C15 C16 1.382(16) . ? C15 C18 1.527(14) . ? O15 C25 1.282(19) . ? O15 H15O 0.8500 . ? C16 C17 1.357(15) . ? C16 H16 0.9500 . ? O16 C26 1.397(17) . ? O16 H16O 0.8500 . ? C17 H17 0.9500 . ? O17 H1W7 0.8501 . ? O17 H2W7 0.8500 . ? C18 C24 1.572(14) . ? C18 H18 1.0000 . ? O18 H1W8 0.8500 . ? O18 H2W8 0.8499 . ? C19 C20 1.321(13) . ? C19 H19 0.9500 . ? O19 H1W9 0.8501 . ? O19 H2W9 0.8501 . ? C20 C21 1.404(16) . ? C20 H20 0.9500 . ? C21 C22 1.391(14) . ? C21 C24 1.499(14) . ? C22 C23 1.381(13) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 O10 Cd1 O9 88.2(3) . . ? O10 Cd1 O1 171.5(3) . . ? O9 Cd1 O1 83.5(2) . . ? O10 Cd1 N2 97.8(3) . . ? O9 Cd1 N2 172.7(3) . . ? O1 Cd1 N2 90.5(2) . . ? O10 Cd1 O11 86.0(3) . . ? O9 Cd1 O11 93.2(2) . . ? O1 Cd1 O11 93.0(2) . . ? N2 Cd1 O11 83.0(2) . . ? O10 Cd1 N1 90.0(3) . 3_786 ? O9 Cd1 N1 90.9(2) . 3_786 ? O1 Cd1 N1 91.5(3) . 3_786 ? N2 Cd1 N1 93.4(3) . 3_786 ? O11 Cd1 N1 174.2(2) . 3_786 ? O1 S1 O3 109.8(4) . . ? O1 S1 O2 108.9(4) . . ? O3 S1 O2 109.5(4) . . ? O1 S1 O4 109.8(4) . . ? O3 S1 O4 111.4(4) . . ? O2 S1 O4 107.4(4) . . ? S1 O1 Cd1 139.7(4) . . ? C5 N1 C1 115.5(8) . . ? C5 N1 Cd1 124.5(7) . 3_786 ? C1 N1 Cd1 120.0(6) . 3_786 ? N1 C1 C2 123.4(9) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? O13 Cd2 N3 174.1(2) . . ? O13 Cd2 O14 88.1(3) . . ? N3 Cd2 O14 97.0(3) . . ? O13 Cd2 O5 84.9(2) . . ? N3 Cd2 O5 89.9(2) . . ? O14 Cd2 O5 171.9(3) . . ? O13 Cd2 N4 87.3(2) . 3_676 ? N3 Cd2 N4 95.7(3) . 3_676 ? O14 Cd2 N4 91.4(3) . 3_676 ? O5 Cd2 N4 92.2(3) . 3_676 ? O13 Cd2 O12 90.7(2) . . ? N3 Cd2 O12 86.8(2) . . ? O14 Cd2 O12 84.1(3) . . ? O5 Cd2 O12 92.0(2) . . ? N4 Cd2 O12 175.1(3) 3_676 . ? O6 S2 O7 109.6(4) . . ? O6 S2 O5 110.3(4) . . ? O7 S2 O5 110.3(4) . . ? O6 S2 O8 108.8(4) . . ? O7 S2 O8 108.4(4) . . ? O5 S2 O8 109.4(4) . . ? C11 N2 C7 113.4(8) . . ? C11 N2 Cd1 128.4(7) . . ? C7 N2 Cd1 116.5(6) . . ? C1 C2 C3 118.0(10) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C13 N3 C17 115.9(8) . . ? C13 N3 Cd2 119.2(6) . . ? C17 N3 Cd2 124.8(6) . . ? C4 C3 C2 118.1(9) . . ? C4 C3 C6 117.1(8) . . ? C2 C3 C6 124.7(10) . . ? C19 N4 C23 114.1(8) . . ? C19 N4 Cd2 122.2(6) . 3_676 ? C23 N4 Cd2 123.5(6) . 3_676 ? C5 C4 C3 119.0(9) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? S2 O5 Cd2 137.8(4) . . ? N1 C5 C4 125.9(10) . . ? N1 C5 H5 117.0 . . ? C4 C5 H5 117.0 . . ? C24 C6 C3 111.0(9) . . ? C24 C6 C12 86.9(9) . . ? C3 C6 C12 122.2(8) . . ? C24 C6 H6 111.4 . . ? C3 C6 H6 111.4 . . ? C12 C6 H6 111.4 . . ? N2 C7 C8 123.4(9) . . ? N2 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C9 C8 C7 119.6(11) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? Cd1 O9 H1W1 121.7 . . ? Cd1 O9 H2W1 124.2 . . ? H1W1 O9 H2W1 107.7 . . ? C8 C9 C10 117.7(9) . . ? C8 C9 C12 123.7(10) . . ? C10 C9 C12 118.4(9) . . ? Cd1 O10 H1W2 164.1 . . ? Cd1 O10 H2W2 87.6 . . ? H1W2 O10 H2W2 107.7 . . ? C11 C10 C9 119.6(10) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? Cd1 O11 H1W3 147.9 . . ? Cd1 O11 H2W3 100.8 . . ? H1W3 O11 H2W3 107.7 . . ? N2 C11 C10 126.2(12) . . ? N2 C11 H11 116.9 . . ? C10 C11 H11 116.9 . . ? Cd2 O12 H1W4 127.3 . . ? Cd2 O12 H2W4 124.3 . . ? H1W4 O12 H2W4 107.7 . . ? C18 C12 C9 115.9(8) . . ? C18 C12 C6 91.4(8) . . ? C9 C12 C6 119.2(9) . . ? C18 C12 H12 109.7 . . ? C9 C12 H12 109.7 . . ? C6 C12 H12 109.7 . . ? Cd2 O13 H1W5 126.7 . . ? Cd2 O13 H2W5 123.9 . . ? H1W5 O13 H2W5 107.7 . . ? N3 C13 C14 121.4(9) . . ? N3 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? Cd2 O14 H1W6 85.5 . . ? Cd2 O14 H2W6 165.5 . . ? H1W6 O14 H2W6 107.7 . . ? C15 C14 C13 122.0(10) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 116.1(10) . . ? C14 C15 C18 126.6(11) . . ? C16 C15 C18 116.6(10) . . ? C25 O15 H15O 113.6 . . ? C17 C16 C15 119.5(10) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C26 O16 H16O 116.2 . . ? N3 C17 C16 124.8(10) . . ? N3 C17 H17 117.6 . . ? C16 C17 H17 117.6 . . ? H1W7 O17 H2W7 107.7 . . ? C12 C18 C15 116.3(10) . . ? C12 C18 C24 88.7(9) . . ? C15 C18 C24 118.8(9) . . ? C12 C18 H18 110.5 . . ? C15 C18 H18 110.5 . . ? C24 C18 H18 110.5 . . ? H1W8 O18 H2W8 107.7 . . ? C20 C19 N4 128.5(11) . . ? C20 C19 H19 115.8 . . ? N4 C19 H19 115.8 . . ? H1W9 O19 H2W9 107.7 . . ? C19 C20 C21 118.8(11) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C22 C21 C20 114.1(9) . . ? C22 C21 C24 126.5(10) . . ? C20 C21 C24 119.3(10) . . ? C23 C22 C21 122.9(10) . . ? C23 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? N4 C23 C22 121.5(9) . . ? N4 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C21 C24 C6 109.7(9) . . ? C21 C24 C18 124.3(9) . . ? C6 C24 C18 91.9(9) . . ? C21 C24 H24 109.7 . . ? C6 C24 H24 109.7 . . ? C18 C24 H24 109.7 . . ? O15 C25 H25A 109.5 . . ? O15 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O15 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O16 C26 H26A 109.5 . . ? O16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.889 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.204 _database_code_depnum_ccdc_archive 'CCDC 966030' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Cd N5 O5, N O3' _chemical_formula_sum 'C24 H24 Cd N6 O8' _chemical_formula_weight 636.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.3104(9) _cell_length_b 13.9294(5) _cell_length_c 19.6913(7) _cell_angle_alpha 90.00 _cell_angle_beta 128.8180(10) _cell_angle_gamma 90.00 _cell_volume 5409.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 30.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7283 _exptl_absorpt_correction_T_max 0.8490 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33763 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7816 _reflns_number_gt 6785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+11.1798P] 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 7816 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _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 0.295410(7) 0.210760(10) 0.305957(8) 0.01725(5) Uani 1 1 d . . . O1 O 0.31067(9) 0.04164(13) 0.30300(12) 0.0417(4) Uani 1 1 d . . . O2 O 0.40732(12) 0.07790(15) 0.33694(15) 0.0557(6) Uani 1 1 d . . . O3 O 0.37167(10) -0.06694(13) 0.30324(16) 0.0569(6) Uani 1 1 d . . . O5 O 0.25831(9) 0.35862(12) 0.31702(12) 0.0415(4) Uani 1 1 d . . . O4 O 0.23547(9) 0.20112(12) 0.15840(10) 0.0343(4) Uani 1 1 d . . . O6 O 0.15368(12) 0.07243(18) -0.01634(13) 0.0645(7) Uani 1 1 d . . . O7 O 0.17172(12) 0.02757(14) 0.10157(12) 0.0569(6) Uani 1 1 d . . . O8 O 0.11509(12) -0.06327(14) -0.01095(12) 0.0576(6) Uani 1 1 d . . . N1 N 0.19557(8) 0.16248(13) 0.27965(12) 0.0237(3) Uani 1 1 d . . . N2 N 0.12412(10) -0.20633(13) 0.18905(12) 0.0270(4) Uani 1 1 d . . . N3 N 0.36304(9) 0.19588(12) 0.45718(10) 0.0219(3) Uani 1 1 d . . . N4 N 0.32436(11) -0.17960(16) 0.48702(13) 0.0395(5) Uani 1 1 d . . . N5 N 0.36344(10) 0.01745(14) 0.31473(13) 0.0331(4) Uani 1 1 d . . . N6 N 0.14694(11) 0.01196(16) 0.02376(13) 0.0387(5) Uani 1 1 d . . . C1 C 0.13638(11) 0.19650(16) 0.20835(15) 0.0296(5) Uani 1 1 d . . . H1 H 0.1372 0.2383 0.1709 0.035 Uiso 1 1 calc R . . C2 C 0.07446(11) 0.17378(16) 0.18679(15) 0.0285(4) Uani 1 1 d . . . H2 H 0.0339 0.1983 0.1348 0.034 Uiso 1 1 calc R . . C3 C 0.07170(10) 0.11522(14) 0.24104(13) 0.0219(4) Uani 1 1 d . . . C4 C 0.13345(11) 0.08218(16) 0.31693(14) 0.0268(4) Uani 1 1 d . . . H4 H 0.1342 0.0437 0.3574 0.032 Uiso 1 1 calc R . . C5 C 0.19351(10) 0.10587(15) 0.33274(14) 0.0254(4) Uani 1 1 d . . . H5 H 0.2349 0.0808 0.3834 0.031 Uiso 1 1 calc R . . C6 C 0.00397(10) 0.08331(14) 0.21359(13) 0.0213(4) Uani 1 1 d . . . H6 H -0.0346 0.1167 0.1595 0.026 Uiso 1 1 calc R . . C7 C -0.00574(10) -0.02915(14) 0.20675(13) 0.0210(4) Uani 1 1 d . . . H7 H -0.0544 -0.0445 0.1581 0.025 Uiso 1 1 calc R . . C8 C 0.03842(10) -0.09200(15) 0.19914(13) 0.0221(4) Uani 1 1 d . . . C9 C 0.07852(12) -0.16294(17) 0.26037(15) 0.0295(5) Uani 1 1 d . . . H9 H 0.0777 -0.1731 0.3074 0.035 Uiso 1 1 calc R . . C10 C 0.11975(13) -0.21872(17) 0.25269(16) 0.0314(5) Uani 1 1 d . . . H10 H 0.1461 -0.2679 0.2944 0.038 Uiso 1 1 calc R . . C11 C 0.08441(11) -0.13852(16) 0.12877(15) 0.0283(4) Uani 1 1 d . . . H11 H 0.0863 -0.1297 0.0825 0.034 Uiso 1 1 calc R . . C12 C 0.04100(11) -0.08116(16) 0.13114(14) 0.0271(4) Uani 1 1 d . . . H12 H 0.0133 -0.0349 0.0868 0.032 Uiso 1 1 calc R . . C13 C 0.33983(11) 0.21967(15) 0.49993(13) 0.0242(4) Uani 1 1 d . . . H13 H 0.3005 0.2589 0.4712 0.029 Uiso 1 1 calc R . . C14 C 0.37068(11) 0.18961(15) 0.58449(13) 0.0236(4) Uani 1 1 d . . . H14 H 0.3521 0.2074 0.6123 0.028 Uiso 1 1 calc R . . C15 C 0.42870(10) 0.13350(14) 0.62823(12) 0.0199(4) Uani 1 1 d . . . C16 C 0.45440(10) 0.11260(15) 0.58493(12) 0.0246(4) Uani 1 1 d . . . H16 H 0.4951 0.0767 0.6132 0.029 Uiso 1 1 calc R . . C17 C 0.42028(10) 0.14438(16) 0.50034(12) 0.0245(4) Uani 1 1 d . . . H17 H 0.4383 0.1289 0.4715 0.029 Uiso 1 1 calc R . . C18 C 0.46035(10) 0.09480(14) 0.71738(11) 0.0203(4) Uani 1 1 d . . . H18 H 0.4411 0.1261 0.7433 0.024 Uiso 1 1 calc R . . C19 C 0.46134(10) -0.01822(14) 0.72532(12) 0.0213(4) Uani 1 1 d . . . H19 H 0.4528 -0.0356 0.7669 0.026 Uiso 1 1 calc R . . C20 C 0.41483(11) -0.07646(15) 0.64319(12) 0.0237(4) Uani 1 1 d . . . C21 C 0.34493(12) -0.07188(17) 0.59638(15) 0.0325(5) Uani 1 1 d . . . H21 H 0.3265 -0.0332 0.6168 0.039 Uiso 1 1 calc R . . C22 C 0.30213(12) -0.12416(19) 0.51968(16) 0.0379(5) Uani 1 1 d . . . H22 H 0.2546 -0.1202 0.4890 0.046 Uiso 1 1 calc R . . C23 C 0.39120(14) -0.1853(2) 0.53320(17) 0.0447(6) Uani 1 1 d . . . H23 H 0.4082 -0.2259 0.5120 0.054 Uiso 1 1 calc R . . C24 C 0.43802(12) -0.13574(18) 0.61067(15) 0.0361(5) Uani 1 1 d . . . H24 H 0.4853 -0.1426 0.6407 0.043 Uiso 1 1 calc R . . H1W H 0.2158 0.1477 0.1358 0.043(8) Uiso 1 1 d R . . H2W H 0.2193 0.2411 0.1172 0.057(10) Uiso 1 1 d R . . H3W H 0.2190 0.3770 0.2734 0.073(12) Uiso 1 1 d R . . H4W H 0.2843 0.4070 0.3409 0.081(13) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01548(7) 0.01957(7) 0.01430(7) 0.00288(5) 0.00818(5) -0.00241(5) O1 0.0322(9) 0.0346(9) 0.0443(10) -0.0033(8) 0.0172(8) 0.0100(7) O2 0.0869(16) 0.0452(11) 0.0706(14) -0.0300(10) 0.0666(14) -0.0351(11) O3 0.0333(10) 0.0280(9) 0.0953(17) -0.0167(10) 0.0335(11) -0.0003(8) O5 0.0299(9) 0.0248(8) 0.0457(10) -0.0023(8) 0.0120(8) 0.0057(7) O4 0.0414(9) 0.0329(9) 0.0167(7) 0.0015(6) 0.0123(7) -0.0101(7) O6 0.0679(15) 0.0745(16) 0.0361(10) -0.0023(11) 0.0252(11) -0.0318(13) O7 0.0849(16) 0.0359(10) 0.0283(9) -0.0047(8) 0.0250(10) -0.0123(10) O8 0.0781(15) 0.0361(10) 0.0305(9) -0.0074(8) 0.0203(10) -0.0157(10) N1 0.0179(8) 0.0231(8) 0.0303(9) 0.0029(7) 0.0152(7) -0.0012(6) N2 0.0321(10) 0.0275(9) 0.0326(9) 0.0010(7) 0.0256(9) 0.0047(8) N3 0.0207(8) 0.0248(8) 0.0149(7) 0.0026(6) 0.0087(7) -0.0002(6) N4 0.0345(11) 0.0378(11) 0.0278(10) -0.0093(9) 0.0107(9) -0.0053(9) N5 0.0328(10) 0.0266(10) 0.0308(10) -0.0051(8) 0.0155(9) -0.0011(8) N6 0.0407(11) 0.0348(11) 0.0238(9) 0.0002(8) 0.0121(9) -0.0019(9) C1 0.0222(10) 0.0305(11) 0.0342(11) 0.0098(9) 0.0168(9) 0.0014(8) C2 0.0190(9) 0.0295(11) 0.0321(11) 0.0062(9) 0.0137(9) 0.0026(8) C3 0.0190(9) 0.0216(9) 0.0279(10) -0.0022(8) 0.0159(8) 0.0001(7) C4 0.0247(10) 0.0287(11) 0.0292(10) 0.0035(8) 0.0179(9) -0.0034(8) C5 0.0204(9) 0.0268(10) 0.0291(10) 0.0038(8) 0.0155(9) -0.0009(8) C6 0.0176(8) 0.0233(9) 0.0240(9) 0.0017(8) 0.0135(8) 0.0014(7) C7 0.0188(9) 0.0227(9) 0.0238(9) 0.0000(7) 0.0145(8) 0.0000(7) C8 0.0210(9) 0.0230(9) 0.0244(9) -0.0012(8) 0.0152(8) -0.0012(7) C9 0.0325(11) 0.0366(12) 0.0304(11) 0.0068(9) 0.0251(10) 0.0071(9) C10 0.0388(12) 0.0311(11) 0.0360(12) 0.0080(9) 0.0292(11) 0.0085(10) C11 0.0315(11) 0.0305(11) 0.0312(11) 0.0029(9) 0.0238(10) 0.0064(9) C12 0.0284(10) 0.0300(11) 0.0271(10) 0.0051(8) 0.0194(9) 0.0072(9) C13 0.0223(9) 0.0246(10) 0.0191(9) 0.0029(8) 0.0098(8) 0.0049(8) C14 0.0270(10) 0.0251(10) 0.0193(9) -0.0002(7) 0.0148(8) 0.0027(8) C15 0.0225(9) 0.0180(9) 0.0133(8) -0.0014(7) 0.0084(7) -0.0018(7) C16 0.0211(9) 0.0305(11) 0.0159(8) 0.0032(8) 0.0086(8) 0.0056(8) C17 0.0229(9) 0.0326(11) 0.0164(8) 0.0021(8) 0.0116(8) 0.0024(8) C18 0.0222(9) 0.0222(9) 0.0123(8) -0.0005(7) 0.0087(7) 0.0010(7) C19 0.0232(9) 0.0224(9) 0.0127(8) 0.0002(7) 0.0086(8) -0.0009(7) C20 0.0268(10) 0.0205(9) 0.0168(9) 0.0010(7) 0.0103(8) -0.0020(8) C21 0.0277(11) 0.0346(12) 0.0275(11) -0.0053(9) 0.0136(9) -0.0029(9) C22 0.0266(11) 0.0383(13) 0.0305(11) -0.0075(10) 0.0089(10) -0.0037(10) C23 0.0417(14) 0.0474(15) 0.0360(13) -0.0197(12) 0.0200(12) -0.0041(12) C24 0.0283(11) 0.0385(13) 0.0320(12) -0.0120(10) 0.0144(10) -0.0040(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.2882(15) . ? Cd1 N2 2.2891(17) 4 ? Cd1 O5 2.3296(17) . ? Cd1 N3 2.3345(16) . ? Cd1 N1 2.3377(16) . ? Cd1 O1 2.3937(18) . ? O1 N5 1.251(3) . ? O2 N5 1.235(3) . ? O3 N5 1.239(3) . ? O5 H3W 0.8501 . ? O5 H4W 0.8489 . ? O4 H1W 0.8497 . ? O4 H2W 0.8489 . ? O6 N6 1.237(3) . ? O7 N6 1.258(3) . ? O8 N6 1.235(3) . ? N1 C5 1.336(3) . ? N1 C1 1.343(3) . ? N2 C10 1.337(3) . ? N2 C11 1.348(3) . ? N2 Cd1 2.2891(17) 4_545 ? N3 C13 1.336(3) . ? N3 C17 1.339(3) . ? N4 C23 1.329(4) . ? N4 C22 1.334(3) . ? C1 C2 1.379(3) . ? C1 H1 0.9500 . ? C2 C3 1.380(3) . ? C2 H2 0.9500 . ? C3 C4 1.400(3) . ? C3 C6 1.506(3) . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C6 1.568(4) 2 ? C6 C7 1.578(3) . ? C6 H6 1.0000 . ? C7 C8 1.499(3) . ? C7 C7 1.538(4) 2 ? C7 H7 1.0000 . ? C8 C9 1.388(3) . ? C8 C12 1.389(3) . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 C15 1.387(3) . ? C14 H14 0.9500 . ? C15 C16 1.389(3) . ? C15 C18 1.500(2) . ? C16 C17 1.383(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C18 1.564(4) 2_656 ? C18 C19 1.581(3) . ? C18 H18 1.0000 . ? C19 C20 1.508(3) . ? C19 C19 1.546(4) 2_656 ? C19 H19 1.0000 . ? C20 C24 1.381(3) . ? C20 C21 1.393(3) . ? C21 C22 1.391(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.394(3) . ? C23 H23 0.9500 . ? C24 H24 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 O4 Cd1 N2 87.02(6) . 4 ? O4 Cd1 O5 100.68(6) . . ? N2 Cd1 O5 87.13(7) 4 . ? O4 Cd1 N3 170.71(6) . . ? N2 Cd1 N3 93.94(6) 4 . ? O5 Cd1 N3 88.59(6) . . ? O4 Cd1 N1 86.42(6) . . ? N2 Cd1 N1 164.51(6) 4 . ? O5 Cd1 N1 80.33(6) . . ? N3 Cd1 N1 94.79(6) . . ? O4 Cd1 O1 84.26(6) . . ? N2 Cd1 O1 110.17(7) 4 . ? O5 Cd1 O1 162.35(7) . . ? N3 Cd1 O1 86.74(6) . . ? N1 Cd1 O1 83.11(6) . . ? N5 O1 Cd1 115.50(15) . . ? Cd1 O5 H3W 117.3 . . ? Cd1 O5 H4W 122.4 . . ? H3W O5 H4W 109.3 . . ? Cd1 O4 H1W 114.8 . . ? Cd1 O4 H2W 135.6 . . ? H1W O4 H2W 107.6 . . ? C5 N1 C1 117.45(18) . . ? C5 N1 Cd1 124.28(13) . . ? C1 N1 Cd1 118.21(14) . . ? C10 N2 C11 117.51(18) . . ? C10 N2 Cd1 119.27(15) . 4_545 ? C11 N2 Cd1 122.94(14) . 4_545 ? C13 N3 C17 117.47(17) . . ? C13 N3 Cd1 121.43(13) . . ? C17 N3 Cd1 119.59(13) . . ? C23 N4 C22 116.5(2) . . ? O2 N5 O3 119.6(2) . . ? O2 N5 O1 120.1(2) . . ? O3 N5 O1 120.3(2) . . ? O8 N6 O6 121.9(2) . . ? O8 N6 O7 118.3(2) . . ? O6 N6 O7 119.8(2) . . ? N1 C1 C2 123.3(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 119.8(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 117.15(18) . . ? C2 C3 C6 119.69(18) . . ? C4 C3 C6 122.97(18) . . ? C5 C4 C3 119.64(19) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 122.66(19) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C3 C6 C6 116.2(2) . 2 ? C3 C6 C7 113.88(16) . . ? C6 C6 C7 88.61(10) 2 . ? C3 C6 H6 112.1 . . ? C6 C6 H6 112.1 2 . ? C7 C6 H6 112.1 . . ? C8 C7 C7 118.40(17) . 2 ? C8 C7 C6 120.15(16) . . ? C7 C7 C6 89.67(10) 2 . ? C8 C7 H7 109.0 . . ? C7 C7 H7 109.0 2 . ? C6 C7 H7 109.0 . . ? C9 C8 C12 117.67(19) . . ? C9 C8 C7 120.92(18) . . ? C12 C8 C7 121.41(18) . . ? C10 C9 C8 119.73(19) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 122.8(2) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C12 123.03(19) . . ? N2 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C11 C12 C8 119.2(2) . . ? C11 C12 H12 120.4 . . ? C8 C12 H12 120.4 . . ? N3 C13 C14 122.83(19) . . ? N3 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 119.70(18) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 117.24(17) . . ? C14 C15 C18 120.67(17) . . ? C16 C15 C18 122.06(18) . . ? C17 C16 C15 119.52(19) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? N3 C17 C16 123.13(19) . . ? N3 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C15 C18 C18 115.48(19) . 2_656 ? C15 C18 C19 115.94(15) . . ? C18 C18 C19 89.20(10) 2_656 . ? C15 C18 H18 111.5 . . ? C18 C18 H18 111.5 2_656 . ? C19 C18 H18 111.5 . . ? C20 C19 C19 120.26(18) . 2_656 ? C20 C19 C18 118.45(16) . . ? C19 C19 C18 89.86(10) 2_656 . ? C20 C19 H19 108.9 . . ? C19 C19 H19 108.9 2_656 . ? C18 C19 H19 108.9 . . ? C24 C20 C21 117.0(2) . . ? C24 C20 C19 123.1(2) . . ? C21 C20 C19 119.95(19) . . ? C22 C21 C20 119.8(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? N4 C22 C21 123.4(2) . . ? N4 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N4 C23 C24 124.3(2) . . ? N4 C23 H23 117.9 . . ? C24 C23 H23 117.9 . . ? C20 C24 C23 119.1(2) . . ? C20 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H2W N4 0.85 1.95 2.796(3) 173.1 4 O5 H3W O1 0.85 2.58 3.156(3) 125.8 4 O5 H3W O3 0.85 1.95 2.782(3) 165.2 4 O5 H4W O7 0.85 1.94 2.772(3) 166.7 4 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.872 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 966031'