# Electronic Supplementary Material (ESI) for CrystEngComm # 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_1 #TrackingRef '1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H68 Cd2 Cl2 Cu4 N14 O18' _chemical_formula_weight 1967.29 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5726(19) _cell_length_b 13.341(2) _cell_length_c 13.473(4) _cell_angle_alpha 102.989(2) _cell_angle_beta 109.678(2) _cell_angle_gamma 108.726(2) _cell_volume 1869.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12763 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 25.2 _exptl_crystal_description Rectangular _exptl_crystal_colour Brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.827 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7116 _exptl_absorpt_correction_T_max 0.7588 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 12763 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.23 _reflns_number_total 6497 _reflns_number_gt 5196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.03' _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^)+(0.0440P)^2^+1.2898P] 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 6497 _refine_ls_number_parameters 521 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.32923(3) 0.12339(2) 0.82559(2) 0.04275(10) Uani 1 1 d . . . Cu1 Cu 0.34236(5) 0.37920(4) 0.93225(4) 0.04369(14) Uani 1 1 d . . . Cu2 Cu 0.13518(4) 0.14059(4) 0.60518(4) 0.04289(14) Uani 1 1 d . . . Cl7 Cl -0.11972(19) 0.51438(17) 0.67787(18) 0.1018(6) Uani 1 1 d . . . O11 O 0.3737(3) 0.2650(2) 0.9876(2) 0.0475(7) Uani 1 1 d . . . O61 O 0.2379(3) 0.0595(2) 0.6322(2) 0.0463(6) Uani 1 1 d . . . O41 O 0.1325(3) 0.1205(2) 0.7422(2) 0.0500(7) Uani 1 1 d . . . O31 O 0.3932(3) 0.3097(2) 0.8263(2) 0.0502(7) Uani 1 1 d . . . N1 N 0.5200(4) 0.1226(3) 0.8709(3) 0.0615(10) Uani 1 1 d . . . N53 N 0.1409(3) 0.1336(3) 0.4589(3) 0.0517(9) Uani 1 1 d . . . N19 N 0.2826(3) 0.4253(3) 1.0445(3) 0.0519(9) Uani 1 1 d . . . C17 C 0.3346(4) 0.3057(4) 1.1494(3) 0.0488(10) Uani 1 1 d . . . C25 C 0.3895(4) 0.4261(3) 0.7145(3) 0.0437(9) Uani 1 1 d . . . C55 C 0.2540(4) 0.0144(3) 0.4579(3) 0.0464(10) Uani 1 1 d . . . N23 N 0.3274(4) 0.4910(3) 0.8614(3) 0.0589(10) Uani 1 1 d . . . N5 N 0.2632(4) -0.0327(3) 0.8661(3) 0.0669(11) Uani 1 1 d . . . C42 C 0.0715(4) 0.1490(4) 0.7987(3) 0.0478(10) Uani 1 1 d . . . C30 C 0.4181(4) 0.3407(3) 0.7462(3) 0.0402(9) Uani 1 1 d . . . N49 N 0.0463(3) 0.2367(3) 0.6092(3) 0.0509(8) Uani 1 1 d . . . C13 C 0.4341(4) 0.1827(4) 1.1218(3) 0.0546(11) Uani 1 1 d . . . H13 H 0.4677 0.1484 1.0806 0.066 Uiso 1 1 calc R . . C18 C 0.2855(4) 0.3847(4) 1.1231(4) 0.0560(11) Uani 1 1 d . . . C59 C 0.3228(4) -0.0701(4) 0.5917(3) 0.0587(12) Uani 1 1 d . . . H59 H 0.3339 -0.0794 0.6603 0.070 Uiso 1 1 calc R . . C12 C 0.3800(4) 0.2513(3) 1.0837(3) 0.0449(9) Uani 1 1 d . . . C29 C 0.4739(4) 0.2884(4) 0.6922(3) 0.0491(10) Uani 1 1 d . . . H29 H 0.4949 0.2330 0.7133 0.059 Uiso 1 1 calc R . . C51 C -0.0148(5) 0.2122(4) 0.4076(4) 0.0648(13) Uani 1 1 d . . . H51A H -0.0799 0.1390 0.3914 0.078 Uiso 1 1 calc R . . H51B H -0.0502 0.2432 0.3532 0.078 Uiso 1 1 calc R . . C48 C 0.0038(4) 0.2576(4) 0.6817(4) 0.0559(11) Uani 1 1 d . . . C47 C 0.0108(4) 0.2177(4) 0.7729(3) 0.0492(10) Uani 1 1 d . . . C16 C 0.3395(5) 0.2840(4) 1.2480(4) 0.0623(12) Uani 1 1 d . . . H16 H 0.3073 0.3183 1.2910 0.075 Uiso 1 1 calc R . . C26 C 0.4116(5) 0.4505(4) 0.6257(4) 0.0622(12) Uani 1 1 d . . . H26 H 0.3895 0.5043 0.6021 0.075 Uiso 1 1 calc R . . C24 C 0.3451(4) 0.4934(4) 0.7735(4) 0.0542(11) Uani 1 1 d . . . C56 C 0.2936(4) -0.0445(4) 0.3888(4) 0.0615(12) Uani 1 1 d . . . H56 H 0.2858 -0.0345 0.3210 0.074 Uiso 1 1 calc R . . C60 C 0.2720(4) 0.0034(3) 0.5628(3) 0.0439(9) Uani 1 1 d . . . C54 C 0.1925(4) 0.0792(4) 0.4155(3) 0.0508(11) Uani 1 1 d . . . C28 C 0.4984(5) 0.3178(4) 0.6082(4) 0.0604(12) Uani 1 1 d . . . H28 H 0.5381 0.2838 0.5746 0.072 Uiso 1 1 calc R . . C43 C 0.0679(4) 0.1097(4) 0.8866(4) 0.0594(12) Uani 1 1 d . . . H43 H 0.1060 0.0622 0.9029 0.071 Uiso 1 1 calc R . . C46 C -0.0488(4) 0.2485(4) 0.8390(4) 0.0657(13) Uani 1 1 d . . . H46 H -0.0888 0.2946 0.8228 0.079 Uiso 1 1 calc R . . C50 C 0.0225(5) 0.2899(4) 0.5233(4) 0.0683(13) Uani 1 1 d . . . H50A H -0.0433 0.3134 0.5220 0.082 Uiso 1 1 calc R . . H50B H 0.0978 0.3578 0.5457 0.082 Uiso 1 1 calc R . . C15 C 0.3895(5) 0.2151(4) 1.2820(4) 0.0667(13) Uani 1 1 d . . . H15 H 0.3910 0.2014 1.3471 0.080 Uiso 1 1 calc R . . O71 O -0.1449(7) 0.4399(6) 0.7286(6) 0.166(3) Uani 1 1 d . . . C4 C 0.2807(4) -0.0838(4) 0.9223(4) 0.0556(11) Uani 1 1 d . . . C58 C 0.3568(5) -0.1288(5) 0.5208(4) 0.0731(15) Uani 1 1 d . . . H58 H 0.3897 -0.1783 0.5413 0.088 Uiso 1 1 calc R . . C14 C 0.4383(5) 0.1651(4) 1.2191(4) 0.0637(13) Uani 1 1 d . . . H14 H 0.4746 0.1188 1.2429 0.076 Uiso 1 1 calc R . . C45 C -0.0488(5) 0.2120(5) 0.9260(4) 0.0729(14) Uani 1 1 d . . . H45 H -0.0869 0.2343 0.9695 0.088 Uiso 1 1 calc R . . C52 C 0.0876(5) 0.1936(5) 0.3910(4) 0.0734(15) Uani 1 1 d . . . H52A H 0.1541 0.2670 0.4099 0.088 Uiso 1 1 calc R . . H52B H 0.0572 0.1498 0.3112 0.088 Uiso 1 1 calc R . . C27 C 0.4647(5) 0.3972(4) 0.5730(4) 0.0691(14) Uani 1 1 d . . . H27 H 0.4783 0.4142 0.5137 0.083 Uiso 1 1 calc R . . C22 C 0.2909(8) 0.5779(6) 0.9075(6) 0.106(2) Uani 1 1 d . . . H22A H 0.3666 0.6446 0.9640 0.127 Uiso 1 1 calc R . . H22B H 0.2515 0.6002 0.8464 0.127 Uiso 1 1 calc R . . C44 C 0.0087(5) 0.1410(5) 0.9485(4) 0.0705(14) Uani 1 1 d . . . H44 H 0.0071 0.1144 1.0064 0.085 Uiso 1 1 calc R . . C2 C 0.6064(4) 0.1292(4) 0.9409(4) 0.0512(10) Uani 1 1 d . . . C20 C 0.2300(6) 0.5095(5) 1.0460(4) 0.0739(15) Uani 1 1 d . . . H20A H 0.1494 0.4759 1.0463 0.089 Uiso 1 1 calc R . . H20B H 0.2846 0.5748 1.1168 0.089 Uiso 1 1 calc R . . C57 C 0.3431(5) -0.1156(5) 0.4192(4) 0.0739(15) Uani 1 1 d . . . H57 H 0.3675 -0.1552 0.3719 0.089 Uiso 1 1 calc R . . O72 O -0.0264(6) 0.5175(6) 0.6479(6) 0.166(3) Uani 1 1 d . . . C21 C 0.2133(9) 0.5495(7) 0.9553(8) 0.135(3) Uani 1 1 d . . . H21A H 0.1340 0.4920 0.8931 0.162 Uiso 1 1 calc R . . H21B H 0.1996 0.6165 0.9795 0.162 Uiso 1 1 calc R . . O73 O -0.2186(9) 0.4928(13) 0.5891(10) 0.342(9) Uani 1 1 d . . . N3 N 0.7117(4) 0.1477(4) 1.0188(4) 0.0792(14) Uani 1 1 d . . . O74 O -0.0960(14) 0.6169(8) 0.7408(11) 0.310(8) Uani 1 1 d . . . O1W O 0.2095(7) 0.6321(7) 0.6388(7) 0.194(3) Uani 1 1 d . . . H18 H 0.251(4) 0.414(4) 1.169(3) 0.054(12) Uiso 1 1 d . . . H54 H 0.191(4) 0.081(3) 0.349(4) 0.051(12) Uiso 1 1 d . . . H24 H 0.336(4) 0.552(4) 0.742(4) 0.069(14) Uiso 1 1 d . . . H48 H -0.035(4) 0.299(4) 0.675(4) 0.066(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0560(2) 0.04596(19) 0.03494(15) 0.01934(13) 0.01845(13) 0.03096(15) Cu1 0.0561(3) 0.0436(3) 0.0401(3) 0.0172(2) 0.0230(2) 0.0290(2) Cu2 0.0453(3) 0.0471(3) 0.0382(2) 0.0195(2) 0.0147(2) 0.0238(2) Cl7 0.1419(15) 0.1270(14) 0.1463(15) 0.0984(13) 0.1095(14) 0.1055(13) O11 0.0676(19) 0.0530(17) 0.0380(14) 0.0231(13) 0.0264(13) 0.0373(15) O61 0.0579(17) 0.0530(17) 0.0347(13) 0.0179(12) 0.0184(13) 0.0329(14) O41 0.0556(17) 0.0671(19) 0.0470(15) 0.0303(14) 0.0269(14) 0.0389(16) O31 0.078(2) 0.0502(17) 0.0502(15) 0.0289(13) 0.0402(15) 0.0413(16) N1 0.069(3) 0.068(3) 0.064(2) 0.033(2) 0.028(2) 0.044(2) N53 0.061(2) 0.057(2) 0.0462(18) 0.0300(17) 0.0224(17) 0.0307(19) N19 0.058(2) 0.058(2) 0.0470(19) 0.0175(17) 0.0248(17) 0.0343(19) C17 0.056(3) 0.053(3) 0.041(2) 0.0184(19) 0.0229(19) 0.026(2) C25 0.048(2) 0.037(2) 0.046(2) 0.0184(18) 0.0198(18) 0.0170(19) C55 0.043(2) 0.048(2) 0.039(2) 0.0111(18) 0.0164(18) 0.015(2) N23 0.090(3) 0.052(2) 0.060(2) 0.0275(18) 0.040(2) 0.048(2) N5 0.078(3) 0.059(2) 0.064(2) 0.038(2) 0.020(2) 0.033(2) C42 0.041(2) 0.051(3) 0.047(2) 0.0163(19) 0.0189(19) 0.018(2) C30 0.046(2) 0.035(2) 0.0370(19) 0.0139(16) 0.0182(17) 0.0148(18) N49 0.056(2) 0.055(2) 0.0496(19) 0.0253(17) 0.0189(17) 0.0338(19) C13 0.070(3) 0.064(3) 0.041(2) 0.024(2) 0.025(2) 0.039(2) C18 0.063(3) 0.067(3) 0.045(2) 0.015(2) 0.031(2) 0.033(2) C59 0.068(3) 0.074(3) 0.042(2) 0.021(2) 0.021(2) 0.044(3) C12 0.050(2) 0.050(2) 0.0333(19) 0.0162(18) 0.0179(18) 0.022(2) C29 0.063(3) 0.049(2) 0.049(2) 0.025(2) 0.029(2) 0.031(2) C51 0.071(3) 0.074(3) 0.054(3) 0.038(2) 0.019(2) 0.037(3) C48 0.051(3) 0.056(3) 0.056(3) 0.017(2) 0.015(2) 0.031(2) C47 0.043(2) 0.051(3) 0.051(2) 0.016(2) 0.0183(19) 0.022(2) C16 0.075(3) 0.081(3) 0.045(2) 0.025(2) 0.037(2) 0.038(3) C26 0.088(4) 0.055(3) 0.057(3) 0.035(2) 0.035(3) 0.033(3) C24 0.068(3) 0.044(3) 0.060(3) 0.027(2) 0.029(2) 0.029(2) C56 0.068(3) 0.074(3) 0.043(2) 0.019(2) 0.028(2) 0.031(3) C60 0.040(2) 0.049(2) 0.0353(19) 0.0102(17) 0.0129(17) 0.0189(19) C54 0.056(3) 0.057(3) 0.037(2) 0.020(2) 0.020(2) 0.019(2) C28 0.082(3) 0.058(3) 0.060(3) 0.027(2) 0.046(3) 0.034(3) C43 0.062(3) 0.070(3) 0.060(3) 0.034(2) 0.032(2) 0.033(3) C46 0.053(3) 0.074(3) 0.073(3) 0.021(3) 0.030(2) 0.033(3) C50 0.092(4) 0.066(3) 0.067(3) 0.040(3) 0.031(3) 0.052(3) C15 0.089(4) 0.081(3) 0.043(2) 0.034(2) 0.033(2) 0.039(3) O71 0.239(7) 0.192(6) 0.234(7) 0.169(6) 0.170(6) 0.159(6) C4 0.048(3) 0.053(3) 0.063(3) 0.025(2) 0.019(2) 0.022(2) C58 0.087(4) 0.093(4) 0.055(3) 0.021(3) 0.028(3) 0.066(3) C14 0.087(4) 0.074(3) 0.049(2) 0.036(2) 0.031(2) 0.046(3) C45 0.068(3) 0.088(4) 0.072(3) 0.023(3) 0.044(3) 0.035(3) C52 0.100(4) 0.091(4) 0.067(3) 0.053(3) 0.045(3) 0.061(3) C27 0.107(4) 0.065(3) 0.068(3) 0.042(3) 0.058(3) 0.042(3) C22 0.191(7) 0.098(5) 0.125(5) 0.070(4) 0.112(6) 0.112(5) C44 0.071(3) 0.085(4) 0.069(3) 0.034(3) 0.045(3) 0.030(3) C2 0.060(3) 0.055(3) 0.059(3) 0.035(2) 0.032(2) 0.035(2) C20 0.098(4) 0.090(4) 0.068(3) 0.032(3) 0.044(3) 0.071(3) C57 0.085(4) 0.091(4) 0.059(3) 0.018(3) 0.036(3) 0.055(3) O72 0.200(6) 0.173(6) 0.249(7) 0.105(5) 0.186(6) 0.116(5) C21 0.226(9) 0.138(6) 0.225(9) 0.134(7) 0.184(8) 0.157(7) O73 0.162(8) 0.55(2) 0.336(14) 0.343(16) 0.052(8) 0.120(11) N3 0.054(3) 0.086(3) 0.107(3) 0.073(3) 0.025(2) 0.027(2) O74 0.62(2) 0.233(9) 0.485(17) 0.255(11) 0.487(18) 0.316(13) O1W 0.176(6) 0.240(8) 0.223(8) 0.138(7) 0.074(6) 0.136(6) _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 N5 2.242(4) . ? Cd1 N1 2.272(4) . ? Cd1 O61 2.279(2) . ? Cd1 O11 2.300(3) . ? Cd1 O41 2.330(3) . ? Cd1 O31 2.350(3) . ? Cd1 Cu2 3.2572(7) . ? Cu1 O31 1.925(3) . ? Cu1 O11 1.932(3) . ? Cu1 N23 1.967(3) . ? Cu1 N19 1.968(3) . ? Cu2 O61 1.931(3) . ? Cu2 O41 1.934(3) . ? Cu2 N49 1.956(3) . ? Cu2 N53 1.979(3) . ? Cl7 O73 1.293(8) . ? Cl7 O74 1.314(9) . ? Cl7 O71 1.343(5) . ? Cl7 O72 1.355(5) . ? O11 C12 1.328(4) . ? O61 C60 1.334(4) . ? O41 C42 1.327(5) . ? O31 C30 1.334(4) . ? N1 C2 1.135(5) . ? N53 C54 1.287(5) . ? N53 C52 1.478(5) . ? N19 C18 1.288(5) . ? N19 C20 1.475(5) . ? C17 C12 1.398(5) . ? C17 C16 1.407(6) . ? C17 C18 1.434(6) . ? C25 C26 1.400(6) . ? C25 C30 1.409(5) . ? C25 C24 1.432(6) . ? C55 C56 1.401(6) . ? C55 C60 1.403(5) . ? C55 C54 1.424(6) . ? N23 C24 1.282(5) . ? N23 C22 1.466(6) . ? N5 C4 1.142(5) . ? C42 C47 1.398(6) . ? C42 C43 1.407(6) . ? C30 C29 1.392(5) . ? N49 C48 1.282(6) . ? N49 C50 1.485(5) . ? C13 C14 1.369(6) . ? C13 C12 1.392(6) . ? C59 C58 1.365(6) . ? C59 C60 1.389(6) . ? C29 C28 1.374(5) . ? C51 C52 1.464(7) . ? C51 C50 1.482(6) . ? C48 C47 1.432(6) . ? C47 C46 1.416(6) . ? C16 C15 1.348(6) . ? C26 C27 1.361(7) . ? C56 C57 1.355(7) . ? C28 C27 1.380(6) . ? C43 C44 1.374(6) . ? C46 C45 1.366(7) . ? C15 C14 1.379(7) . ? C4 N3 1.293(6) 2_657 ? C58 C57 1.380(7) . ? C45 C44 1.390(7) . ? C22 C21 1.343(8) . ? C2 N3 1.284(6) . ? C20 C21 1.420(8) . ? N3 C4 1.293(6) 2_657 ? 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 N5 Cd1 N1 90.19(15) . . ? N5 Cd1 O61 104.97(13) . . ? N1 Cd1 O61 103.78(12) . . ? N5 Cd1 O11 101.54(12) . . ? N1 Cd1 O11 100.25(12) . . ? O61 Cd1 O11 143.83(9) . . ? N5 Cd1 O41 95.76(13) . . ? N1 Cd1 O41 168.10(12) . . ? O61 Cd1 O41 64.74(9) . . ? O11 Cd1 O41 88.66(10) . . ? N5 Cd1 O31 164.68(12) . . ? N1 Cd1 O31 95.55(12) . . ? O61 Cd1 O31 87.47(9) . . ? O11 Cd1 O31 63.48(9) . . ? O41 Cd1 O31 81.31(10) . . ? N5 Cd1 Cu2 118.12(10) . . ? N1 Cd1 Cu2 132.43(10) . . ? O61 Cd1 Cu2 35.58(6) . . ? O11 Cd1 Cu2 109.28(7) . . ? O41 Cd1 Cu2 35.88(6) . . ? O31 Cd1 Cu2 67.44(7) . . ? O31 Cu1 O11 78.74(11) . . ? O31 Cu1 N23 91.64(13) . . ? O11 Cu1 N23 169.98(13) . . ? O31 Cu1 N19 170.16(13) . . ? O11 Cu1 N19 92.22(13) . . ? N23 Cu1 N19 97.56(15) . . ? O61 Cu2 O41 79.36(11) . . ? O61 Cu2 N49 169.14(12) . . ? O41 Cu2 N49 91.84(13) . . ? O61 Cu2 N53 91.27(13) . . ? O41 Cu2 N53 169.16(13) . . ? N49 Cu2 N53 98.04(14) . . ? O61 Cu2 Cd1 43.37(7) . . ? O41 Cu2 Cd1 44.92(8) . . ? N49 Cu2 Cd1 125.80(10) . . ? N53 Cu2 Cd1 129.18(10) . . ? O73 Cl7 O74 100.4(8) . . ? O73 Cl7 O71 111.2(6) . . ? O74 Cl7 O71 111.2(5) . . ? O73 Cl7 O72 109.1(7) . . ? O74 Cl7 O72 110.8(6) . . ? O71 Cl7 O72 113.3(4) . . ? C12 O11 Cu1 129.1(2) . . ? C12 O11 Cd1 125.0(2) . . ? Cu1 O11 Cd1 102.93(10) . . ? C60 O61 Cu2 130.4(2) . . ? C60 O61 Cd1 126.8(2) . . ? Cu2 O61 Cd1 101.05(10) . . ? C42 O41 Cu2 129.7(3) . . ? C42 O41 Cd1 124.8(2) . . ? Cu2 O41 Cd1 99.20(11) . . ? C30 O31 Cu1 130.2(2) . . ? C30 O31 Cd1 125.2(2) . . ? Cu1 O31 Cd1 101.35(11) . . ? C2 N1 Cd1 145.4(4) . . ? C54 N53 C52 114.2(4) . . ? C54 N53 Cu2 123.7(3) . . ? C52 N53 Cu2 122.1(3) . . ? C18 N19 C20 113.9(4) . . ? C18 N19 Cu1 123.2(3) . . ? C20 N19 Cu1 122.9(3) . . ? C12 C17 C16 118.6(4) . . ? C12 C17 C18 123.4(4) . . ? C16 C17 C18 118.0(4) . . ? C26 C25 C30 118.8(4) . . ? C26 C25 C24 118.3(4) . . ? C30 C25 C24 122.8(4) . . ? C56 C55 C60 119.1(4) . . ? C56 C55 C54 117.9(4) . . ? C60 C55 C54 123.0(4) . . ? C24 N23 C22 115.3(4) . . ? C24 N23 Cu1 124.6(3) . . ? C22 N23 Cu1 120.1(3) . . ? C4 N5 Cd1 150.4(4) . . ? O41 C42 C47 121.4(4) . . ? O41 C42 C43 119.5(4) . . ? C47 C42 C43 119.1(4) . . ? O31 C30 C29 119.8(3) . . ? O31 C30 C25 121.5(3) . . ? C29 C30 C25 118.7(3) . . ? C48 N49 C50 115.5(4) . . ? C48 N49 Cu2 124.5(3) . . ? C50 N49 Cu2 120.1(3) . . ? C14 C13 C12 120.9(4) . . ? N19 C18 C17 128.9(4) . . ? C58 C59 C60 120.8(4) . . ? O11 C12 C13 120.0(4) . . ? O11 C12 C17 121.4(4) . . ? C13 C12 C17 118.5(4) . . ? C28 C29 C30 120.6(4) . . ? C52 C51 C50 114.4(4) . . ? N49 C48 C47 128.3(4) . . ? C42 C47 C46 118.7(4) . . ? C42 C47 C48 123.5(4) . . ? C46 C47 C48 117.8(4) . . ? C15 C16 C17 121.9(4) . . ? C27 C26 C25 121.5(4) . . ? N23 C24 C25 128.6(4) . . ? C57 C56 C55 121.1(4) . . ? O61 C60 C59 120.3(3) . . ? O61 C60 C55 121.1(4) . . ? C59 C60 C55 118.5(4) . . ? N53 C54 C55 129.4(4) . . ? C29 C28 C27 120.9(4) . . ? C44 C43 C42 120.5(5) . . ? C45 C46 C47 121.5(5) . . ? C51 C50 N49 112.8(4) . . ? C16 C15 C14 119.1(4) . . ? N5 C4 N3 174.2(5) . 2_657 ? C59 C58 C57 120.9(5) . . ? C13 C14 C15 120.8(4) . . ? C46 C45 C44 119.2(4) . . ? C51 C52 N53 114.7(4) . . ? C26 C27 C28 119.4(4) . . ? C21 C22 N23 117.4(5) . . ? C43 C44 C45 120.9(5) . . ? N1 C2 N3 173.0(5) . . ? C21 C20 N19 116.6(4) . . ? C56 C57 C58 119.5(4) . . ? C22 C21 C20 128.2(7) . . ? C2 N3 C4 121.7(4) . 2_657 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.638 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 926329' ####################################################################### # # 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 #TrackingRef '1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H64 Cd2 Cl2 Cu4 N14 O16' _chemical_formula_weight 1931.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.890(5) _cell_length_b 13.226(5) _cell_length_c 17.248(5) _cell_angle_alpha 101.448(5) _cell_angle_beta 98.822(5) _cell_angle_gamma 107.349(5) _cell_volume 1847.6(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13027 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 25.00 _exptl_crystal_description Rectangular _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.846 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5144 _exptl_absorpt_correction_T_max 0.7005 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 13027 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6283 _reflns_number_gt 5631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.03' _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^)+(0.0553P)^2^+104.0178P] 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 6283 _refine_ls_number_parameters 524 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.1133 _refine_ls_wR_factor_ref 0.3255 _refine_ls_wR_factor_gt 0.3239 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.093 _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 0.19801(15) 0.35503(10) 0.86697(7) 0.0362(4) Uani 1 1 d . . . Cu1 Cu 0.1461(3) 0.3429(2) 0.67317(13) 0.0485(6) Uani 1 1 d . A . Cu2 Cu 0.4624(3) 0.23808(19) 0.81714(13) 0.0443(6) Uani 1 1 d . A . O11 O 0.1048(16) 0.4302(10) 0.7662(7) 0.046(3) Uani 1 1 d . . . C12 C 0.093(2) 0.5300(16) 0.7779(11) 0.047(4) Uani 1 1 d . . . C13 C 0.045(3) 0.5734(17) 0.8480(13) 0.055(5) Uani 1 1 d . . . H13 H 0.0142 0.5303 0.8832 0.066 Uiso 1 1 calc R . . C14 C 0.045(3) 0.680(2) 0.8641(13) 0.068(7) Uani 1 1 d . . . H14 H 0.0195 0.7092 0.9120 0.082 Uiso 1 1 calc R . . C15 C 0.082(3) 0.7449(18) 0.8119(14) 0.068(6) Uani 1 1 d . . . H15 H 0.0725 0.8142 0.8214 0.082 Uiso 1 1 calc R . . C16 C 0.134(3) 0.704(2) 0.7443(16) 0.075(7) Uani 1 1 d . . . H16 H 0.1710 0.7492 0.7114 0.090 Uiso 1 1 calc R . . C17 C 0.131(3) 0.5934(17) 0.7247(14) 0.059(5) Uani 1 1 d . . . C18 C 0.183(3) 0.558(2) 0.6528(14) 0.076(7) Uani 1 1 d . A . H18 H 0.2131 0.6111 0.6245 0.091 Uiso 1 1 calc R . . N19 N 0.195(3) 0.4645(16) 0.6209(10) 0.072(6) Uani 1 1 d D . . C20A C 0.245(6) 0.462(4) 0.5458(19) 0.17(2) Uani 0.40(7) 1 d PD A 1 H20A H 0.3064 0.5359 0.5461 0.201 Uiso 0.40(7) 1 calc PR A 1 H20B H 0.1492 0.4365 0.5021 0.201 Uiso 0.40(7) 1 calc PR A 1 C21A C 0.348(7) 0.390(3) 0.526(4) 0.07(2) Uiso 0.40(7) 1 d PD A 1 H21A H 0.4539 0.4257 0.5617 0.081 Uiso 0.40(7) 1 calc PR A 1 H21B H 0.3614 0.3890 0.4709 0.081 Uiso 0.40(7) 1 calc PR A 1 C22A C 0.289(3) 0.270(3) 0.5307(13) 0.094(10) Uani 0.40(7) 1 d PD A 1 H22A H 0.2179 0.2267 0.4788 0.113 Uiso 0.40(7) 1 calc PR A 1 H22B H 0.3833 0.2470 0.5362 0.113 Uiso 0.40(7) 1 calc PR A 1 C20B C 0.245(6) 0.462(4) 0.5458(19) 0.17(2) Uani 0.60(7) 1 d PD A 2 H20C H 0.3565 0.5102 0.5570 0.201 Uiso 0.60(7) 1 calc PR A 2 H20D H 0.1793 0.4897 0.5117 0.201 Uiso 0.60(7) 1 calc PR A 2 C21B C 0.234(6) 0.348(4) 0.499(3) 0.072(15) Uiso 0.60(7) 1 d P A 2 H21C H 0.1205 0.3104 0.4731 0.087 Uiso 0.60(7) 1 calc PR A 2 H21D H 0.2886 0.3603 0.4549 0.087 Uiso 0.60(7) 1 calc PR A 2 C22B C 0.289(3) 0.270(3) 0.5307(13) 0.094(10) Uani 0.60(7) 1 d PD A 2 H22C H 0.4052 0.3015 0.5532 0.113 Uiso 0.60(7) 1 calc PR A 2 H22D H 0.2686 0.2052 0.4874 0.113 Uiso 0.60(7) 1 calc PR A 2 N23 N 0.207(2) 0.2412(16) 0.5928(10) 0.060(5) Uani 1 1 d D . . C24 C 0.169(3) 0.138(2) 0.5917(12) 0.059(6) Uani 1 1 d . A . H24 H 0.1961 0.0952 0.5502 0.071 Uiso 1 1 calc R . . C25 C 0.090(3) 0.0785(18) 0.6448(13) 0.062(6) Uani 1 1 d . . . C26 C 0.052(4) -0.036(2) 0.6232(17) 0.085(8) Uani 1 1 d . A . H26 H 0.0805 -0.0704 0.5781 0.102 Uiso 1 1 calc R . . C27 C -0.027(4) -0.0954(19) 0.6699(14) 0.076(8) Uani 1 1 d . . . H27 H -0.0601 -0.1715 0.6538 0.092 Uiso 1 1 calc R A . C28 C -0.060(3) -0.0442(17) 0.7424(13) 0.071(7) Uani 1 1 d . A . H28 H -0.1129 -0.0853 0.7743 0.086 Uiso 1 1 calc R . . C29 C -0.011(3) 0.0693(17) 0.7641(13) 0.055(5) Uani 1 1 d . . . H29 H -0.0251 0.1053 0.8131 0.066 Uiso 1 1 calc R A . C30 C 0.058(2) 0.1292(15) 0.7148(12) 0.045(4) Uani 1 1 d . A . O31 O 0.0985(17) 0.2395(11) 0.7387(8) 0.055(3) Uani 1 1 d . . . O41 O 0.4365(15) 0.3784(11) 0.8230(9) 0.052(3) Uani 1 1 d . . . C42 C 0.512(2) 0.4615(19) 0.7928(13) 0.053(5) Uani 1 1 d . A . C43 C 0.500(3) 0.5603(17) 0.8156(14) 0.068(7) Uani 1 1 d . . . H43 H 0.4477 0.5737 0.8574 0.082 Uiso 1 1 calc R A . C44 C 0.563(3) 0.646(2) 0.7794(17) 0.082(8) Uani 1 1 d . A . H44 H 0.5400 0.7107 0.7911 0.098 Uiso 1 1 calc R . . C45 C 0.658(4) 0.630(2) 0.7267(18) 0.092(9) Uani 1 1 d . . . H45 H 0.7027 0.6853 0.7027 0.110 Uiso 1 1 calc R A . C46 C 0.689(3) 0.533(2) 0.7084(16) 0.078(7) Uani 1 1 d . A . H46 H 0.7615 0.5265 0.6758 0.093 Uiso 1 1 calc R . . C47 C 0.613(2) 0.4448(18) 0.7382(11) 0.053(5) Uani 1 1 d . . . C48 C 0.654(3) 0.351(2) 0.7185(13) 0.068(7) Uani 1 1 d . A . H48 H 0.7259 0.3526 0.6845 0.082 Uiso 1 1 calc R . . N49 N 0.606(2) 0.2612(17) 0.7410(10) 0.057(4) Uani 1 1 d . . . C50 C 0.677(3) 0.178(2) 0.7129(15) 0.078(8) Uani 1 1 d . A . H50A H 0.7524 0.1734 0.7580 0.094 Uiso 1 1 calc R . . H50B H 0.7346 0.1970 0.6718 0.094 Uiso 1 1 calc R . . C51 C 0.545(4) 0.071(2) 0.6788(17) 0.094(9) Uani 1 1 d . . . H51A H 0.5831 0.0230 0.6425 0.112 Uiso 1 1 calc R A . H51B H 0.4549 0.0822 0.6465 0.112 Uiso 1 1 calc R . . C52 C 0.485(4) 0.014(2) 0.7410(17) 0.095(10) Uani 1 1 d . A . H52A H 0.3912 -0.0506 0.7133 0.113 Uiso 1 1 calc R . . H52B H 0.5683 -0.0111 0.7653 0.113 Uiso 1 1 calc R . . N53 N 0.439(2) 0.0803(15) 0.8067(12) 0.068(5) Uani 1 1 d . . . C54 C 0.390(3) 0.0296(18) 0.8599(15) 0.064(6) Uani 1 1 d . A . H54 H 0.3951 -0.0407 0.8541 0.076 Uiso 1 1 calc R . . C55 C 0.327(2) 0.0729(17) 0.9290(13) 0.055(5) Uani 1 1 d . . . C56 C 0.292(3) 0.0028(19) 0.9805(16) 0.071(6) Uani 1 1 d . A . H56 H 0.3112 -0.0634 0.9698 0.085 Uiso 1 1 calc R . . C57 C 0.230(3) 0.032(2) 1.0462(17) 0.081(8) Uani 1 1 d . . . H57 H 0.2075 -0.0143 1.0805 0.097 Uiso 1 1 calc R A . C58 C 0.202(3) 0.134(2) 1.0605(14) 0.074(7) Uani 1 1 d . A . H58 H 0.1603 0.1547 1.1049 0.089 Uiso 1 1 calc R . . C59 C 0.234(3) 0.1998(18) 1.0114(12) 0.058(5) Uani 1 1 d . . . H59 H 0.2143 0.2659 1.0221 0.069 Uiso 1 1 calc R A . C60 C 0.298(2) 0.1699(16) 0.9418(12) 0.048(4) Uani 1 1 d . A . O61 O 0.3236(15) 0.2345(10) 0.8956(8) 0.046(3) Uani 1 1 d . . . N1 N -0.037(2) 0.2988(15) 0.9103(11) 0.059(4) Uani 1 1 d . . . C2 C -0.153(2) 0.3185(15) 0.9233(11) 0.043(4) Uani 1 1 d . A . N3 N -0.2826(19) 0.3309(15) 0.9367(12) 0.062(5) Uani 1 1 d . . . C4 C -0.283(2) 0.4211(17) 0.9840(11) 0.047(5) Uani 1 1 d . A . N5 N -0.290(2) 0.4977(16) 1.0226(12) 0.065(5) Uani 1 1 d . . . Cl7 Cl 0.7397(11) 0.2272(6) 0.5016(4) 0.094(2) Uani 1 1 d D . . O71 O 0.781(4) 0.2252(17) 0.4222(10) 0.172(14) Uani 1 1 d D . . O72 O 0.592(5) 0.136(4) 0.494(2) 0.15(4) Uani 0.46(9) 1 d PD . . O73 O 0.871(4) 0.224(7) 0.560(2) 0.22(7) Uani 0.46(9) 1 d PD . . O74 O 0.707(10) 0.330(3) 0.530(3) 0.12(4) Uani 0.46(9) 1 d PD . . O75 O 0.839(6) 0.330(3) 0.5600(18) 0.14(3) Uani 0.54(9) 1 d PD . . O76 O 0.775(8) 0.136(4) 0.529(3) 0.17(4) Uani 0.54(9) 1 d PD . . O77 O 0.569(3) 0.210(6) 0.494(3) 0.22(4) Uani 0.54(9) 1 d PD . . 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 0.0368(7) 0.0418(7) 0.0342(7) 0.0055(5) 0.0117(5) 0.0203(5) Cu1 0.0536(14) 0.0525(14) 0.0344(12) 0.0054(10) 0.0152(10) 0.0120(11) Cu2 0.0407(12) 0.0567(14) 0.0392(12) 0.0042(10) 0.0119(9) 0.0257(10) O11 0.057(8) 0.046(7) 0.033(6) 0.006(5) 0.010(6) 0.018(6) C12 0.050(11) 0.058(12) 0.035(10) 0.013(9) 0.004(8) 0.022(9) C13 0.071(14) 0.056(12) 0.053(12) 0.020(10) 0.032(11) 0.031(11) C14 0.102(18) 0.082(16) 0.044(12) 0.017(11) 0.012(12) 0.067(15) C15 0.099(18) 0.052(12) 0.055(13) 0.018(11) 0.007(12) 0.031(12) C16 0.090(18) 0.073(16) 0.075(17) 0.037(14) 0.030(14) 0.028(14) C17 0.066(13) 0.051(12) 0.061(13) 0.017(10) 0.015(11) 0.019(10) C18 0.083(17) 0.10(2) 0.052(14) 0.032(14) 0.031(12) 0.029(15) N19 0.113(17) 0.062(12) 0.043(10) 0.019(9) 0.030(11) 0.023(11) C20A 0.28(6) 0.16(4) 0.10(3) 0.04(3) 0.12(4) 0.08(4) C22A 0.076(17) 0.16(3) 0.046(14) 0.018(16) 0.019(12) 0.041(19) C20B 0.28(6) 0.16(4) 0.10(3) 0.04(3) 0.12(4) 0.08(4) C22B 0.076(17) 0.16(3) 0.046(14) 0.018(16) 0.019(12) 0.041(19) N23 0.048(10) 0.078(13) 0.053(10) 0.006(9) 0.024(8) 0.021(9) C24 0.066(14) 0.083(16) 0.032(10) 0.002(10) 0.008(9) 0.041(12) C25 0.061(13) 0.063(13) 0.053(12) -0.017(10) -0.016(10) 0.044(11) C26 0.11(2) 0.073(17) 0.080(18) 0.003(14) 0.010(16) 0.060(16) C27 0.12(2) 0.050(13) 0.049(13) 0.010(11) -0.005(14) 0.036(14) C28 0.12(2) 0.045(12) 0.046(12) 0.009(10) 0.001(13) 0.034(13) C29 0.061(12) 0.053(12) 0.048(11) 0.002(9) 0.007(10) 0.026(10) C30 0.033(9) 0.044(10) 0.053(11) 0.001(9) -0.002(8) 0.019(8) O31 0.068(9) 0.050(8) 0.041(7) 0.009(6) 0.017(7) 0.013(7) O41 0.045(7) 0.053(8) 0.069(9) 0.017(7) 0.025(7) 0.024(6) C42 0.028(9) 0.078(14) 0.057(12) 0.029(11) 0.016(8) 0.012(9) C43 0.074(15) 0.046(12) 0.067(14) 0.000(10) 0.033(12) -0.004(11) C44 0.087(18) 0.056(14) 0.085(19) 0.014(13) 0.009(15) 0.008(13) C45 0.09(2) 0.083(19) 0.083(19) 0.010(15) 0.038(16) -0.003(16) C46 0.063(15) 0.085(18) 0.076(17) 0.020(14) 0.035(13) 0.004(13) C47 0.053(11) 0.068(13) 0.036(10) 0.011(9) 0.012(9) 0.020(10) C48 0.046(12) 0.102(19) 0.047(12) 0.003(13) 0.014(10) 0.020(12) N49 0.052(10) 0.086(13) 0.037(9) 0.011(9) 0.017(8) 0.030(9) C50 0.063(14) 0.12(2) 0.052(13) 0.001(14) 0.019(11) 0.049(15) C51 0.088(19) 0.11(2) 0.077(18) -0.017(17) 0.034(16) 0.046(18) C52 0.16(3) 0.066(16) 0.083(19) 0.003(14) 0.06(2) 0.069(18) N53 0.068(12) 0.055(11) 0.075(13) -0.013(10) 0.019(10) 0.033(9) C54 0.058(13) 0.053(12) 0.082(17) 0.017(12) 0.017(12) 0.021(10) C55 0.051(11) 0.055(12) 0.060(13) 0.015(10) 0.005(10) 0.022(10) C56 0.067(15) 0.056(13) 0.087(18) 0.018(12) 0.014(13) 0.020(11) C57 0.10(2) 0.088(18) 0.089(19) 0.054(16) 0.042(16) 0.053(16) C58 0.086(17) 0.096(19) 0.049(13) 0.025(13) 0.010(12) 0.044(15) C59 0.073(14) 0.066(13) 0.046(11) 0.016(10) 0.032(10) 0.032(11) C60 0.039(10) 0.054(11) 0.047(11) 0.011(9) 0.007(8) 0.012(8) O61 0.044(7) 0.056(8) 0.050(7) 0.018(6) 0.018(6) 0.028(6) N1 0.050(10) 0.066(11) 0.063(11) 0.012(9) 0.021(9) 0.021(9) C2 0.038(10) 0.048(10) 0.039(10) 0.003(8) 0.015(8) 0.011(8) N3 0.036(9) 0.065(11) 0.081(13) -0.008(10) 0.019(8) 0.027(8) C4 0.027(8) 0.059(12) 0.044(10) -0.004(9) 0.006(7) 0.013(8) N5 0.053(10) 0.064(11) 0.070(12) -0.010(10) 0.005(9) 0.028(9) Cl7 0.123(6) 0.094(5) 0.072(4) 0.021(4) 0.055(4) 0.033(5) O71 0.34(4) 0.115(19) 0.13(2) 0.053(17) 0.15(3) 0.11(2) O72 0.08(4) 0.18(7) 0.16(6) 0.10(5) 0.02(3) -0.01(4) O73 0.08(4) 0.6(2) 0.18(7) 0.26(10) 0.09(4) 0.18(8) O74 0.17(9) 0.15(6) 0.11(5) 0.04(4) 0.10(5) 0.10(6) O75 0.11(5) 0.21(6) 0.06(3) -0.02(3) 0.03(3) 0.03(4) O76 0.14(7) 0.27(8) 0.15(5) 0.03(6) 0.09(5) 0.10(6) O77 0.12(5) 0.21(10) 0.28(10) -0.01(7) -0.02(5) 0.08(6) _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 N5 2.278(18) 2_567 ? Cd1 O61 2.288(12) . ? Cd1 N1 2.294(17) . ? Cd1 O31 2.295(13) . ? Cd1 O41 2.315(12) . ? Cd1 O11 2.330(13) . ? Cd1 Cu1 3.268(3) . ? Cu1 O31 1.935(13) . ? Cu1 O11 1.935(12) . ? Cu1 N19 1.967(18) . ? Cu1 N23 1.989(17) . ? Cu2 O41 1.923(13) . ? Cu2 O61 1.964(12) . ? Cu2 N49 1.969(17) . ? Cu2 N53 2.004(19) . ? O11 C12 1.33(2) . ? C12 C17 1.37(3) . ? C12 C13 1.41(3) . ? C13 C14 1.39(3) . ? C14 C15 1.37(3) . ? C15 C16 1.39(3) . ? C16 C17 1.42(3) . ? C17 C18 1.43(3) . ? C18 N19 1.29(3) . ? N19 C20B 1.431(14) . ? N19 C20A 1.431(14) . ? C20A C21A 1.53(2) . ? C21A C22A 1.53(2) . ? C22A N23 1.436(13) . ? C20B C21B 1.52(5) . ? C21B C22B 1.43(5) . ? C22B N23 1.436(13) . ? N23 C24 1.30(3) . ? C24 C25 1.45(3) . ? C25 C30 1.37(3) . ? C25 C26 1.41(3) . ? C26 C27 1.36(4) . ? C27 C28 1.41(3) . ? C28 C29 1.39(3) . ? C29 C30 1.37(3) . ? C30 O31 1.35(2) . ? O41 C42 1.35(2) . ? C42 C43 1.33(3) . ? C42 C47 1.43(3) . ? C43 C44 1.41(3) . ? C44 C45 1.36(4) . ? C45 C46 1.37(4) . ? C46 C47 1.40(3) . ? C47 C48 1.39(3) . ? C48 N49 1.29(3) . ? N49 C50 1.47(3) . ? C50 C51 1.48(4) . ? C51 C52 1.51(4) . ? C52 N53 1.47(3) . ? N53 C54 1.29(3) . ? C54 C55 1.48(3) . ? C55 C60 1.36(3) . ? C55 C56 1.41(3) . ? C56 C57 1.37(3) . ? C57 C58 1.43(3) . ? C58 C59 1.33(3) . ? C59 C60 1.44(3) . ? C60 O61 1.28(2) . ? N1 C2 1.18(2) . ? C2 N3 1.26(2) . ? N3 C4 1.31(2) . ? C4 N5 1.12(2) . ? N5 Cd1 2.278(18) 2_567 ? Cl7 O73 1.442(16) . ? Cl7 O77 1.445(16) . ? Cl7 O75 1.449(16) . ? Cl7 O72 1.458(16) . ? Cl7 O71 1.468(12) . ? Cl7 O74 1.480(17) . ? Cl7 O76 1.483(17) . ? 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 N5 Cd1 O61 106.5(6) 2_567 . ? N5 Cd1 N1 88.2(7) 2_567 . ? O61 Cd1 N1 103.1(6) . . ? N5 Cd1 O31 165.5(6) 2_567 . ? O61 Cd1 O31 86.3(5) . . ? N1 Cd1 O31 95.7(6) . . ? N5 Cd1 O41 98.2(6) 2_567 . ? O61 Cd1 O41 66.6(5) . . ? N1 Cd1 O41 169.0(6) . . ? O31 Cd1 O41 80.3(5) . . ? N5 Cd1 O11 101.5(6) 2_567 . ? O61 Cd1 O11 145.2(4) . . ? N1 Cd1 O11 97.9(6) . . ? O31 Cd1 O11 64.1(5) . . ? O41 Cd1 O11 89.6(5) . . ? N5 Cd1 Cu1 130.6(6) 2_567 . ? O61 Cd1 Cu1 109.6(3) . . ? N1 Cd1 Cu1 114.5(5) . . ? O31 Cd1 Cu1 35.5(3) . . ? O41 Cd1 Cu1 67.7(4) . . ? O11 Cd1 Cu1 35.7(3) . . ? O31 Cu1 O11 78.7(5) . . ? O31 Cu1 N19 171.4(7) . . ? O11 Cu1 N19 92.8(7) . . ? O31 Cu1 N23 92.5(7) . . ? O11 Cu1 N23 169.2(7) . . ? N19 Cu1 N23 95.8(8) . . ? O31 Cu1 Cd1 43.6(4) . . ? O11 Cu1 Cd1 44.7(4) . . ? N19 Cu1 Cd1 128.4(5) . . ? N23 Cu1 Cd1 124.5(6) . . ? O41 Cu2 O61 81.1(5) . . ? O41 Cu2 N49 92.0(7) . . ? O61 Cu2 N49 172.9(7) . . ? O41 Cu2 N53 168.2(7) . . ? O61 Cu2 N53 91.4(7) . . ? N49 Cu2 N53 95.7(8) . . ? C12 O11 Cu1 129.4(11) . . ? C12 O11 Cd1 125.9(11) . . ? Cu1 O11 Cd1 99.6(5) . . ? O11 C12 C17 121.6(18) . . ? O11 C12 C13 119.3(17) . . ? C17 C12 C13 119.0(19) . . ? C14 C13 C12 119.8(19) . . ? C15 C14 C13 122(2) . . ? C14 C15 C16 118(2) . . ? C15 C16 C17 121(2) . . ? C12 C17 C16 120(2) . . ? C12 C17 C18 124(2) . . ? C16 C17 C18 117(2) . . ? N19 C18 C17 130(2) . . ? C18 N19 C20B 113(2) . . ? C18 N19 C20A 113(2) . . ? C20B N19 C20A 0.0(9) . . ? C18 N19 Cu1 121.6(15) . . ? C20B N19 Cu1 126(2) . . ? C20A N19 Cu1 126(2) . . ? N19 C20A C21A 117(4) . . ? C20A C21A C22A 119(4) . . ? N23 C22A C21A 120(3) . . ? N19 C20B C21B 115(3) . . ? C22B C21B C20B 127(3) . . ? C21B C22B N23 110(3) . . ? C24 N23 C22B 114(2) . . ? C24 N23 C22A 114(2) . . ? C22B N23 C22A 0.0(9) . . ? C24 N23 Cu1 120.3(13) . . ? C22B N23 Cu1 125.5(18) . . ? C22A N23 Cu1 125.5(18) . . ? N23 C24 C25 130.4(18) . . ? C30 C25 C26 120(3) . . ? C30 C25 C24 123(2) . . ? C26 C25 C24 116(2) . . ? C27 C26 C25 118(2) . . ? C26 C27 C28 122(2) . . ? C29 C28 C27 118(2) . . ? C30 C29 C28 121(2) . . ? O31 C30 C29 117.8(17) . . ? O31 C30 C25 122(2) . . ? C29 C30 C25 120.6(19) . . ? C30 O31 Cu1 127.7(12) . . ? C30 O31 Cd1 129.4(12) . . ? Cu1 O31 Cd1 100.9(6) . . ? C42 O41 Cu2 130.3(12) . . ? C42 O41 Cd1 126.1(12) . . ? Cu2 O41 Cd1 102.0(6) . . ? C43 C42 O41 121.4(18) . . ? C43 C42 C47 119.0(19) . . ? O41 C42 C47 119(2) . . ? C42 C43 C44 123(2) . . ? C45 C44 C43 118(3) . . ? C44 C45 C46 121(3) . . ? C45 C46 C47 121(2) . . ? C48 C47 C46 118(2) . . ? C48 C47 C42 125(2) . . ? C46 C47 C42 117(2) . . ? N49 C48 C47 129(2) . . ? C48 N49 C50 116.0(19) . . ? C48 N49 Cu2 124.1(15) . . ? C50 N49 Cu2 119.6(16) . . ? N49 C50 C51 109(2) . . ? C50 C51 C52 115(2) . . ? N53 C52 C51 116(2) . . ? C54 N53 C52 114(2) . . ? C54 N53 Cu2 122.2(15) . . ? C52 N53 Cu2 123.4(18) . . ? N53 C54 C55 126(2) . . ? C60 C55 C56 121(2) . . ? C60 C55 C54 124(2) . . ? C56 C55 C54 114(2) . . ? C57 C56 C55 121(2) . . ? C56 C57 C58 118(2) . . ? C59 C58 C57 121(2) . . ? C58 C59 C60 121(2) . . ? O61 C60 C55 123.8(19) . . ? O61 C60 C59 118.6(18) . . ? C55 C60 C59 117.7(19) . . ? C60 O61 Cu2 127.2(12) . . ? C60 O61 Cd1 130.6(12) . . ? Cu2 O61 Cd1 101.7(5) . . ? C2 N1 Cd1 146.3(16) . . ? N1 C2 N3 175(2) . . ? C2 N3 C4 121.6(18) . . ? N5 C4 N3 177(2) . . ? C4 N5 Cd1 152.8(17) . 2_567 ? O77 Cl7 O75 111.6(15) . . ? O73 Cl7 O72 110.7(15) . . ? O75 Cl7 O72 138.5(19) . . ? O73 Cl7 O71 111.0(14) . . ? O77 Cl7 O71 110.1(15) . . ? O75 Cl7 O71 110.1(13) . . ? O72 Cl7 O71 110.1(14) . . ? O73 Cl7 O74 109.3(16) . . ? O72 Cl7 O74 107.8(14) . . ? O71 Cl7 O74 107.9(13) . . ? O77 Cl7 O76 108.7(15) . . ? O75 Cl7 O76 108.8(15) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 3.623 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.231 _database_code_depnum_ccdc_archive 'CCDC 926330' ####################################################################### # # 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 #TrackingRef '1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 Cd Cl Cu2 N7 O8' _chemical_formula_weight 965.65 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' Cu Cu 0.3201 1.2651 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall 'C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, 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' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 8.090(5) _cell_length_b 27.992(5) _cell_length_c 17.987(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 4073(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27251 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 29.8 _exptl_crystal_description Hexagonal _exptl_crystal_colour Brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.674 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7835 _exptl_absorpt_correction_T_max 0.8309 _exptl_absorpt_process_details SADBAS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 27251 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 29.77 _reflns_number_total 5585 _reflns_number_gt 4501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.03' _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^)+(0.0572P)^2^+2.4722P] 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 0.02(2) _refine_ls_number_reflns 5585 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.0000 0.228665(10) 0.7500 0.04063(9) Uani 1 2 d S . . Cu1 Cu 1.00345(9) 0.160567(13) 0.902550(19) 0.04547(11) Uani 1 1 d . . . Cl7 Cl 0.5726(3) 0.0000 1.0000 0.0954(7) Uani 1 2 d S . . O11 O 1.0489(3) 0.22677(8) 0.87716(13) 0.0501(6) Uani 1 1 d . . . O31 O 0.8768(3) 0.16548(8) 0.81194(13) 0.0427(5) Uani 1 1 d . . . C17 C 1.1174(5) 0.25581(15) 0.9974(2) 0.0543(9) Uani 1 1 d . . . C2 C 0.6392(4) 0.28813(13) 0.7555(4) 0.0623(9) Uani 1 1 d . . . N23 N 0.9785(6) 0.09138(11) 0.90657(17) 0.0567(9) Uani 1 1 d . . . C25 C 0.8147(5) 0.08277(15) 0.7937(2) 0.0584(10) Uani 1 1 d . . . C28 C 0.6378(6) 0.1075(2) 0.6665(3) 0.0763(14) Uani 1 1 d . . . H28 H 0.5776 0.1159 0.6245 0.092 Uiso 1 1 calc R . . C29 C 0.7113(5) 0.14260(18) 0.7093(2) 0.0631(11) Uani 1 1 d . . . H29 H 0.7000 0.1745 0.6958 0.076 Uiso 1 1 calc R . . C26 C 0.7384(6) 0.04807(16) 0.7450(5) 0.0803(14) Uani 1 1 d . . . H26 H 0.7500 0.0158 0.7562 0.096 Uiso 1 1 calc R . . C12 C 1.0776(5) 0.26295(14) 0.9223(2) 0.0497(8) Uani 1 1 d . . . C13 C 1.0686(6) 0.30995(14) 0.8949(3) 0.0590(10) Uani 1 1 d . . . H13 H 1.0419 0.3152 0.8453 0.071 Uiso 1 1 calc R . . C27 C 0.6531(7) 0.0602(3) 0.6857(3) 0.0921(19) Uani 1 1 d . . . H27 H 0.6031 0.0368 0.6567 0.110 Uiso 1 1 calc R . . C24 C 0.9010(6) 0.06628(15) 0.8584(3) 0.0644(11) Uani 1 1 d . . . H24 H 0.9007 0.0335 0.8663 0.077 Uiso 1 1 calc R . . C22 C 1.0509(8) 0.06180(18) 0.9666(3) 0.0889(19) Uani 1 1 d . . . H22A H 0.9907 0.0319 0.9696 0.107 Uiso 1 1 calc R . . H22B H 1.1646 0.0544 0.9539 0.107 Uiso 1 1 calc R . . C21 C 1.0472(11) 0.0851(2) 1.0389(4) 0.110(3) Uani 1 1 d . . . H21A H 0.9341 0.0945 1.0494 0.132 Uiso 1 1 calc R . . H21B H 1.0792 0.0619 1.0763 0.132 Uiso 1 1 calc R . . C15 C 1.1401(7) 0.34078(18) 1.0156(3) 0.0751(14) Uani 1 1 d . . . H15 H 1.1625 0.3666 1.0465 0.090 Uiso 1 1 calc R . . N3 N 0.5000 0.3100(2) 0.7500 0.139(4) Uani 1 2 d S . . C14 C 1.0995(6) 0.34872(17) 0.9414(3) 0.0702(12) Uani 1 1 d . . . H14 H 1.0930 0.3797 0.9230 0.084 Uiso 1 1 calc R . . C16 C 1.1470(6) 0.2970(2) 1.0425(3) 0.0736(14) Uani 1 1 d . . . H16 H 1.1720 0.2927 1.0926 0.088 Uiso 1 1 calc R . . C30 C 0.8036(4) 0.13041(14) 0.77341(19) 0.0478(8) Uani 1 1 d . . . C18 C 1.1318(7) 0.2105(2) 1.0298(2) 0.0753(14) Uani 1 1 d . . . H18 H 1.1676 0.2104 1.0789 0.090 Uiso 1 1 calc R . . C20 C 1.1461(12) 0.1245(3) 1.0468(4) 0.139(4) Uani 1 1 d . . . H20A H 1.2581 0.1153 1.0339 0.167 Uiso 1 1 calc R . . H20B H 1.1465 0.1333 1.0989 0.167 Uiso 1 1 calc R . . N19 N 1.1030(6) 0.16910(14) 1.0018(2) 0.0730(11) Uani 1 1 d . . . N1 N 0.7691(4) 0.27379(12) 0.7637(2) 0.0618(10) Uani 1 1 d . . . O71 O 0.6219(17) 0.0252(7) 0.9523(6) 0.443(13) Uani 1 1 d . . . O72 O 0.4222(15) -0.0274(3) 0.9769(10) 0.299(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03992(15) 0.05192(17) 0.03005(15) 0.000 -0.00097(18) 0.000 Cu1 0.0502(2) 0.0494(2) 0.0368(2) 0.00523(13) -0.0072(3) -0.0059(3) Cl7 0.0683(10) 0.0873(13) 0.1306(18) 0.0634(13) 0.000 0.000 O11 0.0700(18) 0.0443(11) 0.0360(13) -0.0025(10) -0.0058(10) -0.0084(11) O31 0.0426(12) 0.0527(13) 0.0328(12) 0.0001(10) -0.0020(9) -0.0066(10) C17 0.059(2) 0.064(2) 0.0401(19) -0.0127(17) -0.0070(17) -0.0075(17) C2 0.0449(17) 0.0604(19) 0.082(3) -0.006(3) 0.001(3) -0.0014(14) N23 0.063(3) 0.0541(16) 0.0533(17) 0.0104(13) 0.0044(17) -0.0029(18) C25 0.052(2) 0.073(3) 0.050(2) -0.0064(19) 0.0082(17) -0.0171(19) C28 0.051(2) 0.115(4) 0.063(3) -0.019(3) -0.008(2) -0.028(3) C29 0.044(2) 0.100(3) 0.046(2) -0.007(2) -0.0005(16) -0.015(2) C26 0.085(3) 0.076(3) 0.079(3) -0.016(3) 0.020(4) -0.038(2) C12 0.0502(18) 0.062(2) 0.0368(18) -0.0040(16) -0.0023(15) -0.0060(16) C13 0.067(2) 0.054(2) 0.057(2) -0.0085(18) -0.0006(19) -0.0037(18) C27 0.078(3) 0.127(5) 0.071(3) -0.031(3) 0.002(3) -0.056(3) C24 0.073(3) 0.053(2) 0.067(3) 0.002(2) 0.015(2) -0.012(2) C22 0.117(6) 0.069(3) 0.081(3) 0.023(3) -0.026(3) 0.002(3) C21 0.142(8) 0.098(4) 0.090(4) 0.034(3) -0.018(4) 0.001(4) C15 0.071(3) 0.078(3) 0.076(3) -0.036(3) -0.006(2) -0.012(2) N3 0.049(3) 0.063(3) 0.304(12) 0.000 -0.003(8) 0.000 C14 0.072(3) 0.059(2) 0.080(3) -0.021(2) 0.001(2) -0.006(2) C16 0.065(3) 0.106(4) 0.050(3) -0.023(3) -0.007(2) -0.022(3) C30 0.0323(16) 0.069(2) 0.042(2) -0.0085(15) 0.0079(12) -0.0099(15) C18 0.086(3) 0.102(4) 0.038(2) 0.006(2) -0.022(2) -0.021(3) C20 0.196(9) 0.128(5) 0.094(5) 0.062(4) -0.086(5) -0.060(6) N19 0.091(3) 0.075(2) 0.052(2) 0.0176(18) -0.030(2) -0.021(2) N1 0.0496(16) 0.074(2) 0.061(3) 0.0014(18) 0.0009(15) 0.0097(15) O71 0.258(13) 0.81(3) 0.259(11) 0.331(16) -0.088(10) -0.304(18) O72 0.199(12) 0.174(8) 0.53(2) -0.073(10) 0.053(14) -0.033(6) _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 2.268(3) 4_756 ? Cd1 N1 2.268(3) . ? Cd1 O31 2.316(2) 4_756 ? Cd1 O31 2.316(2) . ? Cd1 O11 2.322(2) . ? Cd1 O11 2.322(2) 4_756 ? Cu1 O31 1.930(2) . ? Cu1 O11 1.944(2) . ? Cu1 N23 1.948(3) . ? Cu1 N19 1.974(4) . ? Cl7 O71 1.181(8) 3_557 ? Cl7 O71 1.181(8) . ? Cl7 O72 1.497(12) . ? Cl7 O72 1.497(12) 3_557 ? O11 C12 1.319(4) . ? O31 C30 1.340(4) . ? C17 C18 1.401(7) . ? C17 C12 1.402(6) . ? C17 C16 1.430(6) . ? C2 N1 1.135(5) . ? C2 N3 1.286(5) . ? N23 C24 1.279(6) . ? N23 C22 1.481(6) . ? C25 C30 1.385(6) . ? C25 C24 1.434(7) . ? C25 C26 1.446(7) . ? C28 C27 1.372(9) . ? C28 C29 1.383(6) . ? C29 C30 1.416(5) . ? C26 C27 1.317(10) . ? C12 C13 1.407(6) . ? C13 C14 1.393(6) . ? C22 C21 1.456(9) . ? C21 C20 1.371(9) . ? C15 C16 1.319(7) . ? C15 C14 1.393(8) . ? N3 C2 1.286(5) 4_656 ? C18 N19 1.284(6) . ? C20 N19 1.526(7) . ? O72 O72 1.74(2) 3_557 ? 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 112.32(18) 4_756 . ? N1 Cd1 O31 91.06(11) 4_756 4_756 ? N1 Cd1 O31 146.31(11) . 4_756 ? N1 Cd1 O31 146.31(11) 4_756 . ? N1 Cd1 O31 91.06(11) . . ? O31 Cd1 O31 80.41(12) 4_756 . ? N1 Cd1 O11 88.83(12) 4_756 . ? N1 Cd1 O11 92.63(12) . . ? O31 Cd1 O11 112.53(8) 4_756 . ? O31 Cd1 O11 65.29(8) . . ? N1 Cd1 O11 92.63(12) 4_756 4_756 ? N1 Cd1 O11 88.83(12) . 4_756 ? O31 Cd1 O11 65.29(8) 4_756 4_756 ? O31 Cd1 O11 112.53(9) . 4_756 ? O11 Cd1 O11 177.38(11) . 4_756 ? O31 Cu1 O11 80.44(10) . . ? O31 Cu1 N23 92.70(13) . . ? O11 Cu1 N23 167.41(13) . . ? O31 Cu1 N19 166.45(16) . . ? O11 Cu1 N19 91.15(13) . . ? N23 Cu1 N19 97.42(15) . . ? O71 Cl7 O71 140.5(15) 3_557 . ? O71 Cl7 O72 99.8(10) 3_557 . ? O71 Cl7 O72 112.3(8) . . ? O71 Cl7 O72 112.3(8) 3_557 3_557 ? O71 Cl7 O72 99.8(10) . 3_557 ? O72 Cl7 O72 71.2(8) . 3_557 ? C12 O11 Cu1 128.4(2) . . ? C12 O11 Cd1 128.3(2) . . ? Cu1 O11 Cd1 102.77(10) . . ? C30 O31 Cu1 128.3(2) . . ? C30 O31 Cd1 120.1(2) . . ? Cu1 O31 Cd1 103.43(10) . . ? C18 C17 C12 123.3(4) . . ? C18 C17 C16 118.6(4) . . ? C12 C17 C16 118.1(4) . . ? N1 C2 N3 171.8(5) . . ? C24 N23 C22 112.3(4) . . ? C24 N23 Cu1 124.9(3) . . ? C22 N23 Cu1 122.8(3) . . ? C30 C25 C24 123.7(4) . . ? C30 C25 C26 117.4(5) . . ? C24 C25 C26 118.9(5) . . ? C27 C28 C29 120.4(5) . . ? C28 C29 C30 120.6(5) . . ? C27 C26 C25 122.7(5) . . ? O11 C12 C17 121.6(4) . . ? O11 C12 C13 119.5(3) . . ? C17 C12 C13 118.9(4) . . ? C14 C13 C12 120.6(4) . . ? C26 C27 C28 120.0(5) . . ? N23 C24 C25 127.7(4) . . ? C21 C22 N23 113.1(5) . . ? C20 C21 C22 116.1(7) . . ? C16 C15 C14 120.7(4) . . ? C2 N3 C2 123.2(5) 4_656 . ? C13 C14 C15 119.6(5) . . ? C15 C16 C17 122.2(4) . . ? O31 C30 C25 122.7(3) . . ? O31 C30 C29 118.6(4) . . ? C25 C30 C29 118.7(4) . . ? N19 C18 C17 129.7(4) . . ? C21 C20 N19 118.1(5) . . ? C18 N19 C20 119.3(4) . . ? C18 N19 Cu1 122.5(3) . . ? C20 N19 Cu1 118.2(4) . . ? C2 N1 Cd1 161.0(4) . . ? Cl7 O72 O72 54.4(4) . 3_557 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 29.77 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.628 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.080 _database_code_depnum_ccdc_archive 'CCDC 926331' ####################################################################### # # 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 #TrackingRef '1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 Cd Cu2 N10 O4' _chemical_formula_weight 932.25 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' Cu Cu 0.3201 1.2651 '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 Trigonal _symmetry_space_group_name_H-M 'P 32 2 1' _symmetry_space_group_name_Hall 'P 32 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' 'y, x, -z' _cell_length_a 11.377(5) _cell_length_b 11.377(5) _cell_length_c 25.411(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 2848.4(19) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 44436 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.5 _exptl_crystal_description Hexagonal _exptl_crystal_colour Green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 1.719 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.6446 _exptl_absorpt_correction_T_max 0.7249 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 44436 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.54 _reflns_number_total 4847 _reflns_number_gt 4542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.03' _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^)+(0.0432P)^2^+0.9100P] 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 0.007(16) _refine_ls_number_reflns 4847 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.50426(2) 0.50426(2) 1.0000 0.04012(7) Uani 1 2 d S . . Cu1 Cu 0.31136(4) 0.25130(4) 0.922434(15) 0.05966(12) Uani 1 1 d . . . O11 O 0.5015(2) 0.3838(2) 0.92989(7) 0.0512(5) Uani 1 1 d . . . O31 O 0.2932(2) 0.3939(3) 0.95625(9) 0.0639(6) Uani 1 1 d . . . C13 C 0.7177(4) 0.5182(4) 0.89284(13) 0.0615(8) Uani 1 1 d . . . H13 H 0.7283 0.5929 0.9118 0.074 Uiso 1 1 calc R . . C17 C 0.5867(4) 0.2839(4) 0.86955(11) 0.0606(8) Uani 1 1 d . . . C29 C 0.1980(4) 0.5301(5) 0.97691(14) 0.0733(10) Uani 1 1 d . . . H29 H 0.2824 0.6005 0.9873 0.088 Uiso 1 1 calc R . . C12 C 0.5992(3) 0.3952(4) 0.89822(10) 0.0490(6) Uani 1 1 d . . . N19 N 0.3638(4) 0.1145(3) 0.90053(11) 0.0695(8) Uani 1 1 d . . . N5 N 0.3031(5) 0.2999(5) 0.83067(14) 0.0978(14) Uani 1 1 d . . . N1 N 0.7109(3) 0.5677(4) 1.03299(13) 0.0808(10) Uani 1 1 d . . . C16 C 0.6945(5) 0.3031(5) 0.83607(13) 0.0787(12) Uani 1 1 d . . . H16 H 0.6871 0.2295 0.8172 0.094 Uiso 1 1 calc R . . N3 N 0.3326(7) 0.2617(7) 0.74056(16) 0.142(3) Uani 1 1 d . . . C4 C 0.3234(4) 0.2798(4) 0.78989(14) 0.0622(8) Uani 1 1 d . . . C30 C 0.1867(3) 0.4095(5) 0.95830(11) 0.0632(9) Uani 1 1 d . . . C28 C 0.0865(5) 0.5469(7) 0.98014(17) 0.0983(17) Uani 1 1 d . . . H28 H 0.0966 0.6280 0.9930 0.118 Uiso 1 1 calc R . . C25 C 0.0567(4) 0.3049(6) 0.94323(15) 0.0860(15) Uani 1 1 d . . . C18 C 0.4751(4) 0.1493(4) 0.87675(13) 0.0669(10) Uani 1 1 d . . . H18 H 0.4849 0.0794 0.8625 0.080 Uiso 1 1 calc R . . N23 N 0.1152(4) 0.1257(5) 0.9259(2) 0.123(2) Uani 1 1 d . . . C20 C 0.2691(6) -0.0320(5) 0.9077(2) 0.1057(18) Uani 1 1 d . . . H20A H 0.2959 -0.0821 0.8845 0.127 Uiso 1 1 calc R . . H20B H 0.2765 -0.0566 0.9436 0.127 Uiso 1 1 calc R . . C24 C 0.0312(4) 0.1688(7) 0.9302(2) 0.116(2) Uani 1 1 d . . . H24 H -0.0592 0.1043 0.9242 0.139 Uiso 1 1 calc R . . C14 C 0.8209(4) 0.5326(5) 0.85994(15) 0.0780(11) Uani 1 1 d . . . H14 H 0.9002 0.6163 0.8577 0.094 Uiso 1 1 calc R . . C15 C 0.8089(5) 0.4267(6) 0.83079(16) 0.0859(13) Uani 1 1 d . . . H15 H 0.8774 0.4384 0.8077 0.103 Uiso 1 1 calc R . . C27 C -0.0419(6) 0.4435(10) 0.9643(2) 0.127(3) Uani 1 1 d . . . H27 H -0.1171 0.4551 0.9664 0.152 Uiso 1 1 calc R . . C26 C -0.0538(5) 0.3275(9) 0.9462(2) 0.121(2) Uani 1 1 d . . . H26 H -0.1386 0.2591 0.9352 0.145 Uiso 1 1 calc R . . C21 C 0.1300(8) -0.0720(7) 0.8973(4) 0.160(3) Uani 1 1 d . . . H21A H 0.1256 -0.0549 0.8602 0.192 Uiso 1 1 calc R . . H21B H 0.0790 -0.1698 0.9017 0.192 Uiso 1 1 calc R . . C22 C 0.0610(7) -0.0259(8) 0.9213(5) 0.207(6) Uani 1 1 d . . . H22A H 0.0444 -0.0622 0.9568 0.249 Uiso 1 1 calc R . . H22B H -0.0265 -0.0648 0.9040 0.249 Uiso 1 1 calc R . . C2 C 0.8099(3) 0.6123(4) 1.05525(14) 0.0680(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03903(10) 0.03903(10) 0.03630(11) -0.00302(5) 0.00302(5) 0.01501(11) Cu1 0.0465(2) 0.0681(3) 0.0545(2) -0.02593(17) -0.00533(15) 0.02123(19) O11 0.0460(11) 0.0637(13) 0.0435(9) -0.0126(9) 0.0032(8) 0.0271(10) O31 0.0455(10) 0.0842(17) 0.0650(12) -0.0330(12) -0.0120(9) 0.0347(12) C13 0.0584(18) 0.073(2) 0.0606(17) 0.0110(15) 0.0149(14) 0.0384(17) C17 0.077(2) 0.085(2) 0.0445(13) -0.0084(14) -0.0041(13) 0.059(2) C29 0.076(2) 0.110(3) 0.0603(18) 0.002(2) 0.0010(17) 0.067(2) C12 0.0526(15) 0.076(2) 0.0349(11) 0.0011(12) 0.0015(11) 0.0446(15) N19 0.082(2) 0.0598(17) 0.0600(15) -0.0201(14) -0.0144(15) 0.0307(15) N5 0.138(4) 0.142(4) 0.0648(19) -0.034(2) -0.027(2) 0.109(3) N1 0.0586(18) 0.095(3) 0.081(2) -0.0142(18) -0.0155(15) 0.0325(17) C16 0.104(3) 0.117(4) 0.0562(17) -0.014(2) 0.002(2) 0.086(3) N3 0.231(7) 0.232(7) 0.078(2) 0.019(3) 0.028(3) 0.202(6) C4 0.065(2) 0.073(2) 0.0679(19) -0.0069(16) -0.0057(15) 0.0483(18) C30 0.0519(16) 0.108(3) 0.0396(13) -0.0071(14) -0.0043(12) 0.0478(19) C28 0.111(4) 0.164(5) 0.075(2) 0.029(3) 0.019(2) 0.110(4) C25 0.0448(17) 0.141(5) 0.064(2) -0.019(2) -0.0090(15) 0.041(2) C18 0.087(3) 0.085(3) 0.0532(16) -0.0205(16) -0.0109(17) 0.061(2) N23 0.0508(19) 0.118(3) 0.157(4) -0.086(3) -0.004(2) 0.010(2) C20 0.113(4) 0.069(3) 0.114(4) -0.035(3) -0.018(3) 0.030(3) C24 0.043(2) 0.145(5) 0.114(4) -0.061(4) -0.014(2) 0.013(3) C14 0.068(2) 0.103(3) 0.073(2) 0.022(2) 0.0267(18) 0.050(2) C15 0.073(3) 0.131(4) 0.069(2) 0.009(2) 0.0215(19) 0.062(3) C27 0.084(3) 0.248(9) 0.096(3) 0.038(4) 0.010(3) 0.119(5) C26 0.060(3) 0.222(8) 0.088(3) -0.009(4) -0.012(2) 0.077(4) C21 0.102(5) 0.091(4) 0.241(10) -0.038(5) -0.030(6) 0.015(4) C22 0.072(4) 0.116(5) 0.364(14) -0.145(8) 0.010(6) -0.006(4) C2 0.0476(17) 0.079(2) 0.0631(17) -0.0145(16) -0.0058(14) 0.0214(16) _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 O11 2.2385(19) . ? Cd1 O11 2.2385(19) 6_557 ? Cd1 N1 2.247(3) . ? Cd1 N1 2.247(3) 6_557 ? Cd1 O31 2.358(2) . ? Cd1 O31 2.358(2) 6_557 ? Cd1 Cu1 3.2662(10) . ? Cd1 Cu1 3.2662(10) 6_557 ? Cu1 O11 1.930(2) . ? Cu1 O31 1.936(3) . ? Cu1 N23 1.960(4) . ? Cu1 N19 2.004(3) . ? Cu1 N5 2.409(4) . ? O11 C12 1.325(3) . ? O31 C30 1.311(4) . ? C13 C12 1.381(5) . ? C13 C14 1.383(5) . ? C17 C12 1.405(5) . ? C17 C16 1.418(5) . ? C17 C18 1.430(6) . ? C29 C28 1.376(6) . ? C29 C30 1.396(6) . ? N19 C18 1.274(5) . ? N19 C20 1.476(6) . ? N5 C4 1.110(5) . ? N1 C2 1.130(4) . ? C16 C15 1.363(7) . ? N3 C2 1.267(5) 2_654 ? N3 C4 1.283(5) . ? C30 C25 1.411(6) . ? C28 C27 1.401(10) . ? C25 C26 1.406(7) . ? C25 C24 1.463(9) . ? N23 C24 1.279(8) . ? N23 C22 1.518(9) . ? C20 C21 1.435(10) . ? C14 C15 1.362(7) . ? C27 C26 1.339(10) . ? C21 C22 1.294(11) . ? C2 N3 1.267(5) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Cd1 O11 143.48(11) . 6_557 ? O11 Cd1 N1 100.71(11) . . ? O11 Cd1 N1 104.03(11) 6_557 . ? O11 Cd1 N1 104.03(11) . 6_557 ? O11 Cd1 N1 100.71(11) 6_557 6_557 ? N1 Cd1 N1 93.8(2) . 6_557 ? O11 Cd1 O31 66.41(8) . . ? O11 Cd1 O31 85.09(8) 6_557 . ? N1 Cd1 O31 165.82(11) . . ? N1 Cd1 O31 95.18(12) 6_557 . ? O11 Cd1 O31 85.09(8) . 6_557 ? O11 Cd1 O31 66.41(8) 6_557 6_557 ? N1 Cd1 O31 95.18(12) . 6_557 ? N1 Cd1 O31 165.82(11) 6_557 6_557 ? O31 Cd1 O31 78.35(15) . 6_557 ? O11 Cd1 Cu1 35.17(5) . . ? O11 Cd1 Cu1 109.32(6) 6_557 . ? N1 Cd1 Cu1 129.96(10) . . ? N1 Cd1 Cu1 114.80(10) 6_557 . ? O31 Cd1 Cu1 35.88(6) . . ? O31 Cd1 Cu1 66.81(7) 6_557 . ? O11 Cd1 Cu1 109.32(6) . 6_557 ? O11 Cd1 Cu1 35.17(5) 6_557 6_557 ? N1 Cd1 Cu1 114.80(10) . 6_557 ? N1 Cd1 Cu1 129.96(10) 6_557 6_557 ? O31 Cd1 Cu1 66.81(7) . 6_557 ? O31 Cd1 Cu1 35.88(6) 6_557 6_557 ? Cu1 Cd1 Cu1 78.11(3) . 6_557 ? O11 Cu1 O31 81.34(9) . . ? O11 Cu1 N23 171.03(14) . . ? O31 Cu1 N23 91.81(15) . . ? O11 Cu1 N19 88.91(12) . . ? O31 Cu1 N19 166.39(11) . . ? N23 Cu1 N19 96.82(18) . . ? O11 Cu1 N5 94.19(14) . . ? O31 Cu1 N5 101.81(12) . . ? N23 Cu1 N5 92.9(2) . . ? N19 Cu1 N5 88.29(12) . . ? O11 Cu1 Cd1 41.91(5) . . ? O31 Cu1 Cd1 45.57(6) . . ? N23 Cu1 Cd1 129.33(12) . . ? N19 Cu1 Cd1 121.47(9) . . ? N5 Cu1 Cd1 117.91(12) . . ? C12 O11 Cu1 125.08(19) . . ? C12 O11 Cd1 132.0(2) . . ? Cu1 O11 Cd1 102.91(8) . . ? C30 O31 Cu1 128.6(2) . . ? C30 O31 Cd1 132.3(2) . . ? Cu1 O31 Cd1 98.55(9) . . ? C12 C13 C14 121.4(4) . . ? C12 C17 C16 118.9(4) . . ? C12 C17 C18 122.3(3) . . ? C16 C17 C18 118.5(4) . . ? C28 C29 C30 121.2(5) . . ? O11 C12 C13 120.4(3) . . ? O11 C12 C17 121.6(3) . . ? C13 C12 C17 118.0(3) . . ? C18 N19 C20 117.4(4) . . ? C18 N19 Cu1 121.7(3) . . ? C20 N19 Cu1 120.7(3) . . ? C4 N5 Cu1 145.1(3) . . ? C2 N1 Cd1 168.4(4) . . ? C15 C16 C17 121.6(4) . . ? C2 N3 C4 124.1(4) 2_654 . ? N5 C4 N3 170.8(4) . . ? O31 C30 C29 120.6(4) . . ? O31 C30 C25 121.7(4) . . ? C29 C30 C25 117.6(4) . . ? C29 C28 C27 120.9(6) . . ? C26 C25 C30 119.1(6) . . ? C26 C25 C24 118.9(5) . . ? C30 C25 C24 121.6(4) . . ? N19 C18 C17 127.2(3) . . ? C24 N23 C22 119.0(5) . . ? C24 N23 Cu1 121.4(4) . . ? C22 N23 Cu1 119.5(4) . . ? C21 C20 N19 113.7(5) . . ? N23 C24 C25 129.3(4) . . ? C15 C14 C13 121.3(4) . . ? C14 C15 C16 118.8(4) . . ? C26 C27 C28 118.4(4) . . ? C27 C26 C25 122.7(6) . . ? C22 C21 C20 125.5(8) . . ? C21 C22 N23 120.8(7) . . ? N1 C2 N3 171.9(5) . 3_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.440 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 926332'