# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_cc _database_code_depnum_ccdc_archive 'CCDC 912551' #TrackingRef 'cc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.50 H14 Cd3 N3 O15' _chemical_formula_weight 1143.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 35.7480(18) _cell_length_b 18.5200(9) _cell_length_c 24.4110(13) _cell_angle_alpha 90.00 _cell_angle_beta 118.6200(10) _cell_angle_gamma 90.00 _cell_volume 14186.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.563 _exptl_crystal_size_mid 0.340 _exptl_crystal_size_min 0.315 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4432 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.573 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63139 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.47 _reflns_number_total 15805 _reflns_number_gt 9412 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. In order to get a better geometry configuration, delu, isor, dfix and dang instructions were used to constrain these disordered C, N atoms on the coordinated DMF molecules. ; _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^)+(0.0712P)^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 15805 _refine_ls_number_parameters 560 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1337 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.126 _refine_ls_shift/su_mean 0.004 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 0.209786(9) 0.62229(2) 0.810035(16) 0.04860(11) Uani 1 1 d . . . Cd2 Cd 0.315612(10) 0.64121(2) 0.819473(17) 0.05126(11) Uani 1 1 d . . . Cd3 Cd 0.322414(11) 0.56859(2) 0.955275(18) 0.05820(13) Uani 1 1 d . . . O1 O 0.37623(13) 0.5689(3) 0.9295(2) 0.0911(16) Uani 1 1 d . . . O2 O 0.37657(13) 0.6066(3) 1.0497(2) 0.0944(16) Uani 1 1 d . . . O3 O 0.3266(2) 0.4510(3) 0.9747(3) 0.120(2) Uani 1 1 d . . . O4 O 0.28153(10) 0.6007(2) 0.99654(16) 0.0648(10) Uani 1 1 d . . . O5 O 0.22772(12) 0.5669(2) 0.90587(17) 0.0630(10) Uani 1 1 d . . . O6 O 0.28199(10) 0.55073(18) 0.84394(15) 0.0521(8) Uani 1 1 d . . . O7 O 0.21927(10) 0.5091(2) 0.77558(17) 0.0647(11) Uani 1 1 d . . . O8 O 0.24198(9) 0.7194(2) 0.87422(16) 0.0580(9) Uani 1 1 d . . . O9 O 0.30825(10) 0.6812(2) 0.90561(15) 0.0545(9) Uani 1 1 d . . . O10 O 0.38413(14) 0.6602(4) 0.8776(2) 0.1115(19) Uani 1 1 d . . . O11 O 0.3123(2) 0.5671(3) 0.7457(2) 0.1047(18) Uani 1 1 d . . . O12 O 0.29499(10) 0.7496(2) 0.7755(2) 0.0787(13) Uani 1 1 d . . . O13 O 0.23936(10) 0.6807(2) 0.75182(15) 0.0554(9) Uani 1 1 d . . . O14 O 0.1413(4) 0.6081(7) 0.7991(5) 0.098(3) Uiso 0.50 1 d P . . O14' O 0.1394(3) 0.5695(5) 0.7808(4) 0.068(2) Uiso 0.50 1 d P . . O15 O 0.1461(2) 0.6756(5) 0.7461(3) 0.0595(18) Uiso 0.50 1 d P . . O15' O 0.1459(3) 0.6518(5) 0.7176(4) 0.080(2) Uiso 0.50 1 d P . . C1 C 0.17763(14) 0.9245(3) 0.6621(2) 0.0574(14) Uani 1 1 d . . . H1 H 0.1607 0.9642 0.6417 0.069 Uiso 1 1 calc R . . C2 C 0.3022(7) 0.4509(11) 0.6718(8) 0.263(9) Uani 1 1 d U . . N3 N 0.3571(9) 0.3399(10) 0.9993(11) 0.316(9) Uiso 1 1 d DU . . C5 C 0.3615(9) 0.4208(10) 1.0025(10) 0.140(9) Uani 0.50 1 d PD . . C6 C 0.39790(18) 0.6158(5) 0.9238(3) 0.082(2) Uani 1 1 d . . . C7 C -0.01219(19) 0.6861(6) 0.8699(4) 0.141(4) Uani 1 1 d . . . H7 H 0.0002 0.7217 0.9002 0.169 Uiso 1 1 calc R . . C8 C -0.05657(19) 0.6816(6) 0.8360(4) 0.134(4) Uani 1 1 d . . . H8 H -0.0728 0.7137 0.8452 0.161 Uiso 1 1 calc R . . C9 C -0.0068(2) 0.5916(6) 0.8154(4) 0.132(3) Uani 1 1 d U . . H9 H 0.0099 0.5600 0.8067 0.159 Uiso 1 1 calc R . . C10 C 0.22215(13) 0.9306(3) 0.6927(2) 0.0502(12) Uani 1 1 d . . . C11 C 0.24650(14) 0.8706(3) 0.7216(2) 0.0541(13) Uani 1 1 d . . . H11 H 0.2761 0.8742 0.7419 0.065 Uiso 1 1 calc R . . C12 C 0.11249(16) 0.8555(3) 0.6289(3) 0.0746(19) Uani 1 1 d . . . C13 C 0.07523(16) 0.8589(3) 0.5976(3) 0.084(2) Uani 1 1 d . . . C14 C 0.03015(16) 0.8639(4) 0.5555(3) 0.082(2) Uani 1 1 d . . . C15 C 0.0102(2) 0.8127(5) 0.5110(5) 0.143(4) Uani 1 1 d . . . H15 H 0.0254 0.7734 0.5084 0.172 Uiso 1 1 calc R . . C16 C 0.0071(2) 0.9161(6) 0.5577(4) 0.143(4) Uani 1 1 d . . . H16 H 0.0199 0.9509 0.5886 0.171 Uiso 1 1 calc R . . C17 C 0.28094(14) 0.7229(3) 0.9082(2) 0.0480(11) Uani 1 1 d . . . C18 C 0.25793(14) 0.5008(3) 0.8083(2) 0.0488(12) Uani 1 1 d . . . C19 C 0.24234(15) 0.5976(3) 0.9575(2) 0.0532(12) Uani 1 1 d . . . C20 C 0.21228(14) 0.6353(3) 0.9752(2) 0.0452(11) Uani 1 1 d . . . C21 C 0.22886(13) 0.6826(3) 1.0257(2) 0.0461(11) Uani 1 1 d . . . H21 H 0.2582 0.6888 1.0492 0.055 Uiso 1 1 calc R . . C22 C 0.20185(13) 0.7207(3) 1.0412(2) 0.0438(11) Uani 1 1 d . . . C23 C 0.15773(14) 0.7103(3) 1.0062(2) 0.0520(12) Uani 1 1 d . . . H23 H 0.1394 0.7364 1.0158 0.062 Uiso 1 1 calc R . . C24 C 0.16867(14) 0.6245(3) 0.9411(2) 0.0525(13) Uani 1 1 d . . . H24 H 0.1577 0.5929 0.9074 0.063 Uiso 1 1 calc R . . C25 C 0.14131(13) 0.6610(3) 0.9572(2) 0.0540(13) Uani 1 1 d . . . C26 C 0.09570(15) 0.6517(4) 0.9220(3) 0.0670(16) Uani 1 1 d . . . C27 C 0.05833(15) 0.6471(4) 0.8946(3) 0.0740(19) Uani 1 1 d . . . C28 C 0.01235(15) 0.6420(4) 0.8603(3) 0.0736(18) Uani 1 1 d . . . C29 C -0.0514(2) 0.5859(6) 0.7814(4) 0.132(3) Uani 1 1 d U . . H29 H -0.0638 0.5493 0.7520 0.159 Uiso 1 1 calc R . . C30 C 0.4633(2) 0.5772(5) 1.0157(4) 0.126(4) Uani 1 1 d . . . H30 H 0.4480 0.5393 1.0203 0.152 Uiso 1 1 calc R . . C31 C -0.07642(15) 0.6328(3) 0.7910(3) 0.0633(15) Uani 1 1 d . . . C32 C 0.12395(17) 0.6283(4) 0.7459(3) 0.0666(16) Uani 1 1 d . . . C33 C 0.44407(16) 0.6231(4) 0.9706(3) 0.0715(17) Uani 1 1 d . . . C34 C 0.4669(2) 0.6808(6) 0.9693(4) 0.138(4) Uani 1 1 d . . . H34 H 0.4533 0.7170 0.9399 0.166 Uiso 1 1 calc R . . C35 C 0.25536(16) 0.7403(3) 0.7508(2) 0.0564(13) Uani 1 1 d . . . C36 C 0.22750(14) 0.8046(3) 0.7208(2) 0.0496(12) Uani 1 1 d . . . C37 C 0.18354(14) 0.7985(3) 0.6911(2) 0.0567(14) Uani 1 1 d . . . H37 H 0.1708 0.7545 0.6904 0.068 Uiso 1 1 calc R . . C38 C 0.15880(14) 0.8586(3) 0.6623(3) 0.0601(15) Uani 1 1 d . . . C39 C 0.3073(6) 0.5829(10) 0.6968(8) 0.210(5) Uani 1 1 d U . . C40 C 0.3703(3) 0.6431(5) 1.0866(3) 0.103(3) Uani 1 1 d . . . C41 C 0.4460(3) 0.6558(8) 1.1584(6) 0.215(7) Uani 1 1 d . . . C42 C 0.3913(5) 0.7125(8) 1.1830(5) 0.210(7) Uani 1 1 d . . . C44 C 0.2853(7) 0.5667(12) 0.5816(8) 0.286(7) Uani 1 1 d DU . . N1 N 0.2983(5) 0.5314(9) 0.6489(6) 0.240(5) Uani 1 1 d DU . . N2 N 0.4013(3) 0.6679(5) 1.1419(3) 0.136(3) Uani 1 1 d . . . C3 C 0.3127(8) 0.3138(14) 0.9649(11) 0.330(12) Uiso 1 1 d D . . C43 C 0.4005(10) 0.315(2) 1.0353(19) 0.55(3) Uiso 1 1 d DU . . 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 0.02420(14) 0.0464(2) 0.0621(2) -0.00625(16) 0.01009(14) 0.00281(13) Cd2 0.03380(17) 0.0471(2) 0.0622(2) 0.00225(16) 0.01439(15) 0.00788(14) Cd3 0.04015(19) 0.0617(3) 0.0648(2) -0.00130(18) 0.01875(16) 0.01048(17) O1 0.041(2) 0.091(4) 0.135(4) -0.047(3) 0.037(2) -0.013(2) O2 0.049(2) 0.125(5) 0.083(3) -0.017(3) 0.010(2) 0.009(3) O3 0.175(6) 0.079(4) 0.122(4) 0.026(3) 0.084(4) 0.053(4) O4 0.0329(16) 0.083(3) 0.071(2) -0.009(2) 0.0193(16) 0.0090(17) O5 0.059(2) 0.063(3) 0.068(2) -0.0108(18) 0.0314(18) 0.0078(18) O6 0.0443(17) 0.040(2) 0.064(2) -0.0106(15) 0.0198(15) -0.0054(14) O7 0.0365(17) 0.050(2) 0.082(2) -0.0123(18) 0.0086(16) 0.0093(15) O8 0.0331(15) 0.056(2) 0.067(2) -0.0155(17) 0.0101(15) -0.0033(15) O9 0.0462(18) 0.047(2) 0.061(2) -0.0128(16) 0.0190(15) 0.0028(15) O10 0.045(2) 0.168(6) 0.096(4) 0.004(4) 0.013(2) 0.004(3) O11 0.162(5) 0.078(4) 0.092(3) -0.001(3) 0.075(4) 0.022(3) O12 0.0309(16) 0.057(3) 0.119(3) 0.027(2) 0.0131(19) 0.0070(16) O13 0.0475(18) 0.042(2) 0.070(2) 0.0077(16) 0.0223(16) 0.0032(15) C1 0.028(2) 0.048(3) 0.079(3) 0.016(2) 0.013(2) 0.004(2) C2 0.40(3) 0.205(7) 0.214(13) -0.051(8) 0.174(18) 0.015(18) C5 0.25(3) 0.066(13) 0.177(18) 0.050(12) 0.15(2) 0.066(15) C6 0.039(3) 0.119(7) 0.079(4) -0.021(4) 0.022(3) 0.004(4) C7 0.033(3) 0.193(10) 0.155(7) -0.109(7) 0.011(4) -0.005(4) C8 0.037(3) 0.169(9) 0.167(8) -0.095(7) 0.024(4) -0.005(4) C9 0.056(4) 0.178(7) 0.154(6) -0.084(6) 0.044(4) -0.008(4) C10 0.028(2) 0.045(3) 0.064(3) 0.009(2) 0.0098(19) 0.0014(19) C11 0.034(2) 0.045(3) 0.063(3) 0.008(2) 0.006(2) -0.002(2) C12 0.039(3) 0.055(4) 0.100(4) 0.023(3) 0.010(3) -0.005(2) C13 0.031(2) 0.062(4) 0.118(5) 0.028(3) 0.002(3) -0.004(2) C14 0.027(2) 0.069(5) 0.114(5) 0.022(4) 0.004(3) -0.009(3) C15 0.036(3) 0.127(8) 0.198(9) -0.041(7) 0.001(4) 0.013(4) C16 0.044(4) 0.159(9) 0.150(8) -0.058(7) -0.014(4) 0.021(5) C17 0.035(2) 0.040(3) 0.059(3) -0.006(2) 0.014(2) -0.0015(19) C18 0.040(2) 0.042(3) 0.053(3) -0.003(2) 0.013(2) 0.004(2) C19 0.040(2) 0.050(3) 0.067(3) 0.006(2) 0.023(2) 0.006(2) C20 0.034(2) 0.044(3) 0.052(3) -0.002(2) 0.0167(19) 0.0006(19) C21 0.0281(19) 0.042(3) 0.056(3) 0.001(2) 0.0109(18) -0.0004(18) C22 0.030(2) 0.036(3) 0.055(3) -0.0043(19) 0.0123(18) -0.0012(18) C23 0.032(2) 0.050(3) 0.065(3) -0.009(2) 0.016(2) -0.001(2) C24 0.033(2) 0.059(4) 0.056(3) -0.011(2) 0.014(2) -0.001(2) C25 0.027(2) 0.054(4) 0.066(3) -0.010(2) 0.011(2) -0.002(2) C26 0.034(2) 0.084(5) 0.074(3) -0.025(3) 0.017(2) -0.004(3) C27 0.028(2) 0.101(5) 0.080(4) -0.026(3) 0.015(2) -0.009(3) C28 0.025(2) 0.100(5) 0.077(4) -0.026(3) 0.009(2) -0.012(3) C29 0.053(4) 0.185(8) 0.137(6) -0.083(6) 0.029(4) -0.016(4) C30 0.044(3) 0.130(8) 0.164(8) 0.045(6) 0.017(4) -0.017(4) C31 0.032(2) 0.070(4) 0.073(3) -0.004(3) 0.013(2) -0.003(2) C32 0.040(3) 0.072(5) 0.080(4) 0.004(3) 0.023(3) 0.004(3) C33 0.032(2) 0.085(5) 0.080(4) -0.011(3) 0.012(3) -0.001(3) C34 0.059(4) 0.131(9) 0.147(8) 0.043(6) -0.013(4) -0.009(5) C35 0.045(3) 0.047(4) 0.065(3) 0.010(2) 0.017(2) 0.007(2) C36 0.034(2) 0.036(3) 0.065(3) 0.010(2) 0.013(2) -0.0010(19) C37 0.033(2) 0.038(3) 0.081(3) 0.017(2) 0.014(2) -0.0030(19) C38 0.029(2) 0.054(4) 0.075(3) 0.014(3) 0.007(2) -0.001(2) C39 0.225(10) 0.196(8) 0.213(7) -0.032(7) 0.108(8) 0.020(8) C40 0.099(6) 0.105(7) 0.072(5) -0.010(4) 0.015(4) -0.006(5) C41 0.075(6) 0.237(16) 0.203(12) -0.012(11) -0.037(7) -0.022(8) C42 0.300(18) 0.202(15) 0.118(8) -0.076(9) 0.092(10) -0.002(12) C44 0.348(13) 0.323(12) 0.222(6) 0.005(7) 0.163(9) -0.012(9) N1 0.307(10) 0.223(7) 0.185(6) -0.029(5) 0.113(7) 0.015(8) N2 0.136(7) 0.121(7) 0.095(5) -0.022(4) 0.010(4) -0.023(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 O15 2.278(8) . ? Cd1 O8 2.299(3) . ? Cd1 O7 2.343(4) . ? Cd1 O5 2.345(4) . ? Cd1 O14 2.347(11) . ? Cd1 O15' 2.380(9) . ? Cd1 O13 2.397(4) . ? Cd1 O14' 2.465(9) . ? Cd1 C32 2.697(5) . ? Cd2 O10 2.192(4) . ? Cd2 O11 2.223(5) . ? Cd2 O12 2.230(4) . ? Cd2 O6 2.301(4) . ? Cd2 O9 2.360(3) . ? Cd2 O13 2.526(3) . ? Cd2 C35 2.713(5) . ? Cd2 Cd3 3.4764(6) . ? Cd3 O4 2.217(4) . ? Cd3 O3 2.219(6) . ? Cd3 O1 2.292(5) . ? Cd3 O2 2.298(4) . ? Cd3 O9 2.342(4) . ? Cd3 O6 2.413(3) . ? O1 C6 1.216(9) . ? O2 C40 1.230(9) . ? O3 C5 1.23(2) . ? O4 C19 1.263(5) . ? O5 C19 1.246(6) . ? O6 C18 1.278(5) . ? O7 C18 1.231(5) . ? O8 C17 1.235(5) . ? O9 C17 1.271(6) . ? O10 C6 1.287(9) . ? O11 C39 1.157(17) . ? O12 C35 1.258(6) . ? O13 C35 1.249(6) . ? O14 O14' 0.827(12) . ? O14 C32 1.199(11) . ? O14' C32 1.329(10) . ? O15 O15' 0.821(10) . ? O15 C32 1.180(9) . ? O15' C32 1.344(11) . ? C1 C38 1.396(7) . ? C1 C10 1.402(6) . ? C2 N1 1.58(2) . ? N3 C43 1.445(18) . ? N3 C3 1.477(16) . ? N3 C5 1.505(16) . ? C6 C33 1.498(7) . ? C7 C28 1.299(9) . ? C7 C8 1.397(8) . ? C8 C31 1.335(9) . ? C9 C28 1.350(9) . ? C9 C29 1.406(9) . ? C10 C11 1.379(6) . ? C10 C18 1.488(7) 4_556 ? C11 C36 1.393(7) . ? C12 C13 1.178(7) . ? C12 C38 1.455(6) . ? C13 C14 1.441(6) . ? C14 C16 1.290(11) . ? C14 C15 1.357(11) . ? C15 C34 1.391(9) 8_465 ? C16 C30 1.405(8) 8_465 ? C17 C22 1.506(6) 7_567 ? C18 C10 1.488(7) 4_546 ? C19 C20 1.508(7) . ? C20 C24 1.386(6) . ? C20 C21 1.393(6) . ? C21 C22 1.386(6) . ? C22 C23 1.401(6) . ? C22 C17 1.506(6) 7_567 ? C23 C25 1.392(7) . ? C24 C25 1.391(7) . ? C25 C26 1.444(6) . ? C26 C27 1.176(7) . ? C27 C28 1.447(6) . ? C29 C31 1.345(10) . ? C30 C33 1.296(10) . ? C30 C16 1.405(8) 8_566 ? C31 C32 1.497(7) 2_556 ? C32 C31 1.497(7) 2_556 ? C33 C34 1.354(11) . ? C34 C15 1.391(9) 8_566 ? C35 C36 1.499(7) . ? C36 C37 1.384(6) . ? C37 C38 1.386(7) . ? C39 N1 1.421(18) . ? C40 N2 1.353(9) . ? C41 N2 1.465(15) . ? C42 N2 1.468(13) . ? C44 N1 1.617(14) . ? 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 O15 Cd1 O8 97.9(2) . . ? O15 Cd1 O7 114.2(2) . . ? O8 Cd1 O7 146.43(11) . . ? O15 Cd1 O5 125.4(2) . . ? O8 Cd1 O5 81.60(14) . . ? O7 Cd1 O5 87.11(14) . . ? O15 Cd1 O14 47.5(3) . . ? O8 Cd1 O14 108.6(3) . . ? O7 Cd1 O14 100.4(3) . . ? O5 Cd1 O14 80.6(3) . . ? O15 Cd1 O15' 20.2(2) . . ? O8 Cd1 O15' 114.0(3) . . ? O7 Cd1 O15' 95.9(3) . . ? O5 Cd1 O15' 136.6(3) . . ? O14 Cd1 O15' 56.2(4) . . ? O15 Cd1 O13 88.7(2) . . ? O8 Cd1 O13 80.33(13) . . ? O7 Cd1 O13 90.58(14) . . ? O5 Cd1 O13 143.25(12) . . ? O14 Cd1 O13 135.7(3) . . ? O15' Cd1 O13 80.2(2) . . ? O15 Cd1 O14' 55.1(3) . . ? O8 Cd1 O14' 128.0(2) . . ? O7 Cd1 O14' 81.1(2) . . ? O5 Cd1 O14' 82.4(2) . . ? O14 Cd1 O14' 19.6(3) . . ? O15' Cd1 O14' 55.6(3) . . ? O13 Cd1 O14' 133.4(2) . . ? O15 Cd1 C32 25.7(2) . . ? O8 Cd1 C32 114.98(16) . . ? O7 Cd1 C32 98.53(16) . . ? O5 Cd1 C32 106.76(17) . . ? O14 Cd1 C32 26.3(3) . . ? O15' Cd1 C32 29.9(3) . . ? O13 Cd1 C32 109.85(16) . . ? O14' Cd1 C32 29.4(2) . . ? O10 Cd2 O11 103.4(2) . . ? O10 Cd2 O12 100.2(2) . . ? O11 Cd2 O12 106.79(19) . . ? O10 Cd2 O6 120.62(19) . . ? O11 Cd2 O6 85.94(18) . . ? O12 Cd2 O6 133.43(13) . . ? O10 Cd2 O9 86.57(17) . . ? O11 Cd2 O9 158.54(18) . . ? O12 Cd2 O9 89.69(16) . . ? O6 Cd2 O9 72.67(12) . . ? O10 Cd2 O13 153.9(2) . . ? O11 Cd2 O13 91.55(18) . . ? O12 Cd2 O13 54.54(12) . . ? O6 Cd2 O13 81.16(12) . . ? O9 Cd2 O13 86.89(11) . . ? O10 Cd2 C35 127.0(2) . . ? O11 Cd2 C35 101.47(19) . . ? O12 Cd2 C35 27.31(15) . . ? O6 Cd2 C35 107.11(15) . . ? O9 Cd2 C35 86.78(15) . . ? O13 Cd2 C35 27.29(13) . . ? O10 Cd2 Cd3 84.20(16) . . ? O11 Cd2 Cd3 119.10(14) . . ? O12 Cd2 Cd3 131.59(13) . . ? O6 Cd2 Cd3 43.74(8) . . ? O9 Cd2 Cd3 42.13(9) . . ? O13 Cd2 Cd3 107.23(8) . . ? C35 Cd2 Cd3 121.54(12) . . ? O4 Cd3 O3 99.1(2) . . ? O4 Cd3 O1 161.15(16) . . ? O3 Cd3 O1 94.6(2) . . ? O4 Cd3 O2 83.34(15) . . ? O3 Cd3 O2 98.5(2) . . ? O1 Cd3 O2 81.93(17) . . ? O4 Cd3 O9 88.29(14) . . ? O3 Cd3 O9 163.79(17) . . ? O1 Cd3 O9 81.81(16) . . ? O2 Cd3 O9 96.65(17) . . ? O4 Cd3 O6 112.27(12) . . ? O3 Cd3 O6 92.81(18) . . ? O1 Cd3 O6 79.64(14) . . ? O2 Cd3 O6 159.07(17) . . ? O9 Cd3 O6 71.01(11) . . ? O4 Cd3 Cd2 124.69(10) . . ? O3 Cd3 Cd2 123.37(15) . . ? O1 Cd3 Cd2 54.70(13) . . ? O2 Cd3 Cd2 118.59(15) . . ? O9 Cd3 Cd2 42.52(8) . . ? O6 Cd3 Cd2 41.26(8) . . ? C6 O1 Cd3 134.3(5) . . ? C40 O2 Cd3 122.8(5) . . ? C5 O3 Cd3 120.8(12) . . ? C19 O4 Cd3 112.3(3) . . ? C19 O5 Cd1 126.2(4) . . ? C18 O6 Cd2 128.0(3) . . ? C18 O6 Cd3 135.2(3) . . ? Cd2 O6 Cd3 94.99(11) . . ? C18 O7 Cd1 100.9(3) . . ? C17 O8 Cd1 122.3(3) . . ? C17 O9 Cd3 119.8(3) . . ? C17 O9 Cd2 130.7(3) . . ? Cd3 O9 Cd2 95.35(13) . . ? C6 O10 Cd2 107.7(5) . . ? C39 O11 Cd2 127.0(10) . . ? C35 O12 Cd2 98.3(3) . . ? C35 O13 Cd1 138.3(4) . . ? C35 O13 Cd2 84.7(3) . . ? Cd1 O13 Cd2 97.23(12) . . ? O14' O14 C32 79.7(12) . . ? O14' O14 Cd1 88.3(12) . . ? C32 O14 Cd1 93.3(7) . . ? O14 O14' C32 62.6(11) . . ? O14 O14' Cd1 72.1(11) . . ? C32 O14' Cd1 85.0(5) . . ? O15' O15 C32 82.3(11) . . ? O15' O15 Cd1 86.9(10) . . ? C32 O15 Cd1 97.4(5) . . ? O15 O15' C32 60.4(9) . . ? O15 O15' Cd1 72.9(9) . . ? C32 O15' Cd1 88.2(5) . . ? C38 C1 C10 119.7(4) . . ? C43 N3 C3 142(3) . . ? C43 N3 C5 104(2) . . ? C3 N3 C5 114(2) . . ? O3 C5 N3 112(2) . . ? O1 C6 O10 124.1(6) . . ? O1 C6 C33 120.4(7) . . ? O10 C6 C33 115.5(7) . . ? C28 C7 C8 122.0(7) . . ? C31 C8 C7 122.1(7) . . ? C28 C9 C29 121.5(7) . . ? C11 C10 C1 119.0(5) . . ? C11 C10 C18 121.5(4) . 4_556 ? C1 C10 C18 119.4(4) . 4_556 ? C10 C11 C36 121.0(4) . . ? C13 C12 C38 172.5(7) . . ? C12 C13 C14 175.8(9) . . ? C16 C14 C15 117.0(6) . . ? C16 C14 C13 122.5(7) . . ? C15 C14 C13 120.5(7) . . ? C14 C15 C34 120.0(8) . 8_465 ? C14 C16 C30 123.1(8) . 8_465 ? O8 C17 O9 125.5(4) . . ? O8 C17 C22 118.3(4) . 7_567 ? O9 C17 C22 116.2(4) . 7_567 ? O7 C18 O6 122.1(5) . . ? O7 C18 C10 119.7(4) . 4_546 ? O6 C18 C10 118.2(4) . 4_546 ? O5 C19 O4 124.1(5) . . ? O5 C19 C20 119.3(4) . . ? O4 C19 C20 116.6(5) . . ? C24 C20 C21 120.1(4) . . ? C24 C20 C19 120.8(4) . . ? C21 C20 C19 119.0(4) . . ? C22 C21 C20 120.3(4) . . ? C21 C22 C23 119.5(4) . . ? C21 C22 C17 120.8(4) . 7_567 ? C23 C22 C17 119.5(4) . 7_567 ? C25 C23 C22 120.1(5) . . ? C20 C24 C25 120.1(4) . . ? C24 C25 C23 119.8(4) . . ? C24 C25 C26 121.3(5) . . ? C23 C25 C26 118.8(5) . . ? C27 C26 C25 176.8(7) . . ? C26 C27 C28 179.3(9) . . ? C7 C28 C9 117.2(5) . . ? C7 C28 C27 122.2(6) . . ? C9 C28 C27 120.6(6) . . ? C31 C29 C9 120.6(7) . . ? C33 C30 C16 121.0(8) . 8_566 ? C8 C31 C29 116.5(6) . . ? C8 C31 C32 122.4(6) . 2_556 ? C29 C31 C32 121.1(6) . 2_556 ? O15 C32 O14 103.3(8) . . ? O15 C32 O14' 122.3(7) . . ? O14 C32 O14' 37.8(6) . . ? O15 C32 O15' 37.3(5) . . ? O14 C32 O15' 122.1(8) . . ? O14' C32 O15' 115.5(7) . . ? O15 C32 C31 121.8(7) . 2_556 ? O14 C32 C31 121.2(8) . 2_556 ? O14' C32 C31 115.8(6) . 2_556 ? O15' C32 C31 116.6(6) . 2_556 ? O15 C32 Cd1 56.9(4) . . ? O14 C32 Cd1 60.3(6) . . ? O14' C32 Cd1 65.6(4) . . ? O15' C32 Cd1 61.9(4) . . ? C31 C32 Cd1 178.5(5) 2_556 . ? C30 C33 C34 117.1(6) . . ? C30 C33 C6 122.2(7) . . ? C34 C33 C6 120.6(7) . . ? C33 C34 C15 121.4(8) . 8_566 ? O13 C35 O12 122.2(5) . . ? O13 C35 C36 120.6(4) . . ? O12 C35 C36 117.2(5) . . ? O13 C35 Cd2 68.0(3) . . ? O12 C35 Cd2 54.4(3) . . ? C36 C35 Cd2 169.8(4) . . ? C37 C36 C11 120.2(4) . . ? C37 C36 C35 120.8(5) . . ? C11 C36 C35 119.0(4) . . ? C36 C37 C38 119.2(5) . . ? C37 C38 C1 120.9(4) . . ? C37 C38 C12 122.1(5) . . ? C1 C38 C12 117.0(5) . . ? O11 C39 N1 122.7(17) . . ? O2 C40 N2 124.6(9) . . ? C39 N1 C2 113.4(14) . . ? C39 N1 C44 114.0(17) . . ? C2 N1 C44 132.6(14) . . ? C40 N2 C41 119.1(10) . . ? C40 N2 C42 121.4(10) . . ? C41 N2 C42 119.2(10) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.853 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.094 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 -0.325 0.193 6509 845 ' ' 2 0.500 0.222 0.750 13 3 ' ' 3 0.000 0.278 0.250 13 1 ' ' 4 0.000 0.722 0.750 13 3 ' ' 5 0.500 0.778 0.250 13 1 ' ' _platon_squeeze_details ; The remaining solvent molecules were disordered and assigned as 8 DMF molecules, 8 ethanol molecules and 16 water molecules per unit cell, which were determined by TGA, elemental analysis and SQUEEZE results. The contributions of these disordered solvents to the scattering values have been removed by using the PLATON SQUEEZE program. We can see from the SQUEEZE that there are about 853e in the unit cell, as about 107e per asymmetric unit, which include 21e of H of coordinated DMF molecules and 86e of free solvent. From the calculation and related information (The CHN and TGA), the asymmetric unit should include one DMF, one C2H5OH and two H2O (40e+26e+10e*2=86e). Anal. Cald. for C47.5H52Cd3N4O19: C, 43.21; H, 3.97; N, 4.24; found: C, 42.97; H, 4.23; N, 4.34. Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. ;