# 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H40 Cd2 N4 O12' _chemical_formula_sum 'C64 H40 Cd2 N4 O12' _chemical_formula_weight 1281.80 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 P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.1902(10) _cell_length_b 29.7214(18) _cell_length_c 16.0823(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.722(5) _cell_angle_gamma 90.00 _cell_volume 8121.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8545 _cell_measurement_theta_min 2.3241 _cell_measurement_theta_max 29.2348 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.898 0.272 0.028 3422.1 220.9 _platon_squeeze_details ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 28028 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14303 _reflns_number_gt 9072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1371P)^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 14007 _refine_ls_number_parameters 739 _refine_ls_number_restraints 1472 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2501 _refine_ls_wR_factor_gt 0.2213 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.004 _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 0.40134(3) 0.781545(15) 0.48035(3) 0.04752(19) Uani 1 1 d . . . Cd2 Cd 0.85294(3) 0.710048(16) 0.01422(3) 0.04746(19) Uani 1 1 d . . . C29 C 0.8689(3) 0.8501(2) -0.0149(4) 0.0480(13) Uani 1 1 d U . . C9 C 0.6130(4) 1.1413(2) 0.9877(4) 0.0462(13) Uani 1 1 d U . . O3 O 0.5460(3) 1.20997(14) 0.9551(3) 0.0596(13) Uani 1 1 d . . . O7 O 0.8038(3) 0.78082(15) -0.0520(3) 0.0606(13) Uani 1 1 d . . . C5 C 0.5618(4) 0.8989(2) 0.8443(4) 0.0448(12) Uani 1 1 d U . . C1 C 0.4652(4) 0.8269(2) 0.6207(4) 0.0490(14) Uani 1 1 d U . . O5 O 0.7479(3) 0.82761(18) 1.4303(3) 0.0648(14) Uani 1 1 d . . . C19 C 0.6887(4) 0.9024(2) 1.1469(4) 0.0456(12) Uani 1 1 d U . . C2 C 0.4993(4) 0.8511(2) 0.6978(4) 0.0484(13) Uani 1 1 d U . . C27 C 0.5952(3) 0.9715(2) 0.9190(4) 0.0433(11) Uani 1 1 d U . . H27A H 0.5761 0.9862 0.8690 0.052 Uiso 1 1 calc R . . C16 C 0.7538(4) 0.8573(2) 1.2947(4) 0.0474(13) Uani 1 1 d U . . C22 C 0.5953(3) 0.9239(2) 0.9204(3) 0.0428(12) Uani 1 1 d U . . O1 O 0.5060(3) 0.82063(18) 0.5640(3) 0.0645(13) Uani 1 1 d . . . C24 C 0.6555(3) 0.9262(2) 1.0666(3) 0.0408(11) Uani 1 1 d U . . O4 O 0.6639(3) 1.21385(15) 1.0282(4) 0.0736(17) Uani 1 1 d . . . N2 N 0.7704(4) 0.7281(2) 0.1132(3) 0.0559(15) Uani 1 1 d . . . C25 C 0.6531(3) 0.9734(2) 1.0640(4) 0.0432(11) Uani 1 1 d U . . H25A H 0.6720 0.9895 1.1125 0.052 Uiso 1 1 calc R . . C15 C 0.7877(4) 0.8346(2) 1.3738(4) 0.0517(14) Uani 1 1 d U . . O6 O 0.8578(3) 0.82105(18) 1.3814(3) 0.0650(13) Uani 1 1 d . . . C13 C 0.5590(3) 1.0699(2) 0.9417(4) 0.0444(12) Uani 1 1 d U . . H13A H 0.5179 1.0538 0.9110 0.053 Uiso 1 1 calc R . . C62 C 0.6589(4) 0.7460(3) 0.2192(4) 0.0598(14) Uani 1 1 d U . . O8 O 0.9209(3) 0.77801(16) 0.0264(4) 0.0691(15) Uani 1 1 d . . . O2 O 0.3949(3) 0.81256(18) 0.6136(3) 0.0684(14) Uani 1 1 d . . . C8 C 0.6086(4) 1.1912(2) 0.9887(4) 0.0501(14) Uani 1 1 d U . . C12 C 0.6215(3) 1.0469(2) 0.9887(3) 0.0392(11) Uani 1 1 d U . . C57 C 0.5995(4) 0.7543(3) 0.2757(4) 0.0614(14) Uani 1 1 d U . . C28 C 0.8651(4) 0.7992(2) -0.0150(4) 0.0528(14) Uani 1 1 d U . . N1 N 0.4867(4) 0.76856(19) 0.3814(3) 0.0558(14) Uani 1 1 d . . . C53 C 0.9060(4) 1.0636(2) 0.0718(4) 0.0575(13) Uani 1 1 d U . . C14 C 0.5574(4) 1.1163(2) 0.9403(4) 0.0463(13) Uani 1 1 d U . . H14A H 0.5168 1.1308 0.9056 0.056 Uiso 1 1 calc R . . C54 C 0.9042(4) 1.0167(2) 0.0662(4) 0.0532(13) Uani 1 1 d U . . H54A H 0.9241 0.9997 0.1132 0.064 Uiso 1 1 calc R . . C50 C 0.8441(3) 1.0195(2) -0.0774(4) 0.0514(12) Uani 1 1 d U . . H50A H 0.8238 1.0046 -0.1268 0.062 Uiso 1 1 calc R . . C32 C 0.8733(3) 0.9444(2) -0.0107(4) 0.0470(12) Uani 1 1 d U . . C49 C 0.8740(3) 0.9951(2) -0.0069(4) 0.0492(13) Uani 1 1 d U . . C10 C 0.6776(4) 1.1192(2) 1.0323(4) 0.0474(13) Uani 1 1 d U . . H10A H 0.7190 1.1359 1.0612 0.057 Uiso 1 1 calc R . . C23 C 0.6258(3) 0.9024(2) 0.9945(3) 0.0437(12) Uani 1 1 d U . . C34 C 0.8125(4) 0.8747(2) -0.0635(4) 0.0482(13) Uani 1 1 d U . . H34A H 0.7732 0.8598 -0.0993 0.058 Uiso 1 1 calc R . . C26 C 0.6230(3) 0.9972(2) 0.9905(3) 0.0416(12) Uani 1 1 d U . . C46 C 0.8090(4) 1.0912(3) -0.1517(4) 0.0631(15) Uani 1 1 d U . . C39 C 0.9399(4) 1.0854(3) 0.1516(4) 0.0638(15) Uani 1 1 d U . . C30 C 0.9309(4) 0.8725(2) 0.0323(4) 0.0499(14) Uani 1 1 d U . . H30A H 0.9715 0.8559 0.0626 0.060 Uiso 1 1 calc R . . C33 C 0.8121(4) 0.9208(2) -0.0611(4) 0.0481(12) Uani 1 1 d U . . H33A H 0.7713 0.9366 -0.0928 0.058 Uiso 1 1 calc R . . C11 C 0.6810(4) 1.0725(2) 1.0343(4) 0.0471(12) Uani 1 1 d U . . H11A H 0.7235 1.0582 1.0663 0.056 Uiso 1 1 calc R . . C31 C 0.9342(3) 0.9187(2) 0.0355(4) 0.0488(13) Uani 1 1 d U . . H31A H 0.9764 0.9330 0.0679 0.059 Uiso 1 1 calc R . . C51 C 0.8439(4) 1.0665(2) -0.0752(4) 0.0547(13) Uani 1 1 d U . . C52 C 0.8746(4) 1.0890(3) -0.0004(4) 0.0590(14) Uani 1 1 d U . . C36 C 1.0102(5) 1.1287(3) 0.2995(5) 0.0828(18) Uani 1 1 d U . . O9 O 1.1186(4) 1.1441(3) 0.4045(4) 0.129(3) Uani 1 1 d U . . C17 C 0.6793(4) 0.8752(3) 1.2865(4) 0.0669(16) Uani 1 1 d U . . H17A H 0.6494 0.8721 1.3296 0.080 Uiso 1 1 calc R . . N3 N 0.6259(4) 0.8554(3) 0.9987(4) 0.095(3) Uani 1 1 d . . . H3B H 0.6071 0.8399 0.9552 0.114 Uiso 1 1 calc R . . H3C H 0.6449 0.8421 1.0448 0.114 Uiso 1 1 calc R . . C18 C 0.6486(4) 0.8983(3) 1.2124(4) 0.0600(14) Uani 1 1 d U . . H18A H 0.5989 0.9113 1.2084 0.072 Uiso 1 1 calc R . . C58 C 0.6131(4) 0.7420(3) 0.3583(4) 0.0694(16) Uani 1 1 d U . . H58A H 0.6611 0.7295 0.3815 0.083 Uiso 1 1 calc R . . O11 O 0.6320(4) 1.1520(3) -0.4032(4) 0.125(3) Uani 1 1 d U . . C21 C 0.7937(4) 0.8596(3) 1.2275(4) 0.0670(16) Uani 1 1 d U . . H21A H 0.8431 0.8463 1.2312 0.080 Uiso 1 1 calc R . . C60 C 0.7834(5) 0.7178(3) 0.1923(5) 0.0841(19) Uani 1 1 d U . . H60A H 0.8311 0.7042 0.2133 0.101 Uiso 1 1 calc R . . C3 C 0.5719(4) 0.8699(3) 0.7060(4) 0.0659(15) Uani 1 1 d U . . H3A H 0.6014 0.8672 0.6623 0.079 Uiso 1 1 calc R . . O10 O 1.0248(7) 1.1828(3) 0.4018(6) 0.187(5) Uani 1 1 d . . . C6 C 0.4899(4) 0.8790(3) 0.8361(4) 0.0648(14) Uani 1 1 d U . . H6A H 0.4605 0.8818 0.8798 0.078 Uiso 1 1 calc R . . N4 N 0.8736(3) 1.1359(2) 0.0038(4) 0.076(2) Uani 1 1 d . . . H4B H 0.8541 1.1513 -0.0396 0.091 Uiso 1 1 calc R . . H4C H 0.8925 1.1493 0.0498 0.091 Uiso 1 1 calc R . . C43 C 0.7405(5) 1.1379(3) -0.2957(5) 0.0822(18) Uani 1 1 d U . . C63 C 0.6471(4) 0.7585(3) 0.1385(4) 0.0730(16) Uani 1 1 d U . . H63A H 0.6004 0.7727 0.1161 0.088 Uiso 1 1 calc R . . C55 C 0.4728(5) 0.7806(3) 0.3027(5) 0.0763(19) Uani 1 1 d U . . H55A H 0.4245 0.7937 0.2824 0.092 Uiso 1 1 calc R . . C7 C 0.4581(5) 0.8543(3) 0.7641(4) 0.0714(16) Uani 1 1 d U . . H7A H 0.4095 0.8402 0.7617 0.086 Uiso 1 1 calc R . . C59 C 0.5539(4) 0.7484(3) 0.4074(4) 0.0690(17) Uani 1 1 d U . . H59A H 0.5626 0.7377 0.4624 0.083 Uiso 1 1 calc R . . C56 C 0.5269(5) 0.7745(3) 0.2477(4) 0.0707(17) Uani 1 1 d U . . H56A H 0.5148 0.7840 0.1921 0.085 Uiso 1 1 calc R . . C64 C 0.7043(5) 0.7504(3) 0.0881(4) 0.0760(17) Uani 1 1 d U . . H64A H 0.6956 0.7612 0.0333 0.091 Uiso 1 1 calc R . . C4 C 0.6030(4) 0.8931(3) 0.7784(4) 0.0639(14) Uani 1 1 d U . . H4A H 0.6534 0.9050 0.7824 0.077 Uiso 1 1 calc R . . C20 C 0.7617(4) 0.8817(3) 1.1532(4) 0.0632(14) Uani 1 1 d U . . H20A H 0.7895 0.8826 1.1079 0.076 Uiso 1 1 calc R . . C40 C 1.0182(5) 1.0770(3) 0.1829(5) 0.0810(17) Uani 1 1 d U . . H40A H 1.0471 1.0567 0.1559 0.097 Uiso 1 1 calc R . . C61 C 0.7307(5) 0.7259(3) 0.2472(5) 0.0830(18) Uani 1 1 d U . . H61A H 0.7435 0.7179 0.3035 0.100 Uiso 1 1 calc R . . C45 C 0.7296(5) 1.0832(3) -0.1829(5) 0.0809(17) Uani 1 1 d U . . H45A H 0.7006 1.0627 -0.1565 0.097 Uiso 1 1 calc R . . C41 C 1.0535(5) 1.0995(3) 0.2565(5) 0.0890(18) Uani 1 1 d U . . H41A H 1.1064 1.0947 0.2766 0.107 Uiso 1 1 calc R . . C44 C 0.6945(5) 1.1066(3) -0.2548(6) 0.0921(19) Uani 1 1 d U . . H44A H 0.6418 1.1019 -0.2759 0.110 Uiso 1 1 calc R . . C38 C 0.8998(5) 1.1143(3) 0.1937(5) 0.0885(17) Uani 1 1 d U . . H38A H 0.8473 1.1202 0.1728 0.106 Uiso 1 1 calc R . . C47 C 0.8502(5) 1.1198(3) -0.1940(5) 0.0894(17) Uani 1 1 d U . . H47A H 0.9032 1.1250 -0.1744 0.107 Uiso 1 1 calc R . . C48 C 0.8143(5) 1.1416(3) -0.2666(6) 0.0945(19) Uani 1 1 d U . . H48A H 0.8452 1.1598 -0.2954 0.113 Uiso 1 1 calc R . . C37 C 0.9344(6) 1.1361(3) 0.2689(6) 0.097(2) Uani 1 1 d U . . H37A H 0.9045 1.1553 0.2969 0.117 Uiso 1 1 calc R . . C42 C 0.6984(7) 1.1627(4) -0.3720(6) 0.096(2) Uani 1 1 d U . . O12 O 0.7205(7) 1.1919(3) -0.3947(6) 0.203(6) Uani 1 1 d . . . C35 C 1.0514(7) 1.1542(4) 0.3758(6) 0.095(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0694(4) 0.0376(3) 0.0320(3) -0.00121(19) -0.0036(2) -0.0004(2) Cd2 0.0640(3) 0.0435(3) 0.0313(3) -0.00268(19) -0.0042(2) -0.0004(2) C29 0.048(3) 0.041(3) 0.050(3) 0.007(3) -0.009(2) -0.006(2) C9 0.055(3) 0.034(3) 0.045(3) 0.000(2) -0.009(2) 0.008(2) O3 0.084(4) 0.037(3) 0.052(3) -0.003(2) -0.007(3) 0.005(2) O7 0.079(3) 0.048(3) 0.048(3) -0.003(2) -0.013(2) -0.019(2) C5 0.055(2) 0.045(3) 0.032(2) 0.000(2) -0.002(2) -0.005(2) C1 0.063(3) 0.052(3) 0.031(3) -0.007(3) 0.002(3) -0.007(3) O5 0.071(3) 0.088(4) 0.036(2) 0.017(2) 0.008(2) 0.013(3) C19 0.053(3) 0.049(3) 0.032(2) 0.004(2) -0.001(2) 0.005(2) C2 0.061(3) 0.051(3) 0.033(2) -0.012(2) 0.006(2) -0.006(3) C27 0.050(2) 0.044(2) 0.035(2) -0.001(2) 0.002(2) -0.001(2) C16 0.056(3) 0.053(3) 0.031(2) 0.008(2) 0.003(2) 0.009(3) C22 0.049(2) 0.046(3) 0.032(2) -0.003(2) 0.002(2) 0.001(2) O1 0.081(3) 0.073(4) 0.038(2) -0.019(2) 0.004(2) -0.007(3) C24 0.044(2) 0.048(3) 0.031(2) 0.005(2) 0.007(2) 0.001(2) O4 0.066(3) 0.035(3) 0.109(5) -0.010(3) -0.023(3) -0.005(2) N2 0.080(4) 0.054(3) 0.031(3) 0.000(3) -0.002(3) 0.008(3) C25 0.050(2) 0.043(2) 0.034(2) 0.002(2) -0.001(2) 0.003(2) C15 0.067(3) 0.052(3) 0.035(3) 0.007(3) 0.004(3) 0.007(3) O6 0.068(3) 0.078(4) 0.044(3) 0.023(3) -0.008(2) 0.015(3) C13 0.049(2) 0.038(2) 0.043(2) 0.002(2) -0.005(2) 0.000(2) C62 0.072(3) 0.079(3) 0.028(2) 0.012(3) 0.004(2) 0.026(3) O8 0.061(3) 0.042(3) 0.095(4) 0.006(3) -0.018(3) 0.002(2) O2 0.077(3) 0.073(4) 0.050(3) -0.023(3) -0.006(2) -0.014(3) C8 0.061(3) 0.040(3) 0.046(3) 0.000(3) 0.001(3) 0.008(3) C12 0.044(2) 0.035(2) 0.037(2) 0.000(2) 0.000(2) 0.002(2) C57 0.072(3) 0.078(3) 0.034(2) 0.012(3) 0.007(2) 0.023(3) C28 0.062(3) 0.050(3) 0.046(3) 0.006(3) 0.006(3) -0.001(3) N1 0.085(4) 0.048(3) 0.031(3) -0.007(3) -0.001(3) 0.005(3) C53 0.057(3) 0.057(3) 0.054(3) -0.006(2) -0.005(2) -0.006(2) C14 0.053(3) 0.038(3) 0.045(3) 0.003(2) -0.002(2) 0.006(2) C54 0.054(2) 0.051(3) 0.050(2) 0.002(2) -0.005(2) -0.006(2) C50 0.047(2) 0.052(3) 0.050(2) 0.001(2) -0.009(2) 0.000(2) C32 0.044(2) 0.047(3) 0.047(2) 0.000(2) -0.002(2) -0.004(2) C49 0.051(2) 0.046(3) 0.046(2) 0.004(2) -0.006(2) -0.004(2) C10 0.052(3) 0.037(3) 0.051(3) 0.000(2) -0.003(2) -0.004(2) C23 0.050(2) 0.045(2) 0.035(2) -0.001(2) 0.002(2) 0.001(2) C34 0.051(3) 0.045(3) 0.045(3) 0.002(3) -0.004(2) -0.006(2) C26 0.048(2) 0.040(2) 0.034(2) 0.000(2) -0.003(2) 0.001(2) C46 0.067(3) 0.058(3) 0.060(3) 0.013(3) -0.008(3) -0.004(3) C39 0.072(3) 0.058(3) 0.055(3) -0.010(3) -0.011(3) -0.005(3) C30 0.047(3) 0.047(3) 0.054(3) 0.005(3) -0.002(2) 0.002(2) C33 0.051(2) 0.043(3) 0.046(2) 0.001(2) -0.006(2) -0.003(2) C11 0.051(2) 0.039(2) 0.047(3) 0.000(2) -0.004(2) 0.004(2) C31 0.046(2) 0.045(3) 0.050(3) 0.006(2) -0.010(2) -0.003(2) C51 0.052(2) 0.055(3) 0.052(2) 0.010(2) -0.007(2) -0.004(2) C52 0.060(3) 0.053(3) 0.058(3) 0.002(2) -0.012(2) -0.001(2) C36 0.097(4) 0.072(4) 0.071(3) -0.017(3) -0.014(3) -0.014(3) O9 0.095(4) 0.207(9) 0.078(4) -0.030(5) -0.014(3) -0.057(5) C17 0.078(3) 0.081(4) 0.041(3) 0.013(3) 0.010(3) 0.019(3) N3 0.123(6) 0.063(5) 0.087(5) -0.005(4) -0.024(5) 0.002(4) C18 0.062(3) 0.074(3) 0.044(3) 0.012(3) 0.007(2) 0.021(3) C58 0.082(3) 0.091(4) 0.034(3) 0.016(3) 0.005(3) 0.031(3) O11 0.094(4) 0.192(9) 0.082(4) 0.030(5) -0.006(3) 0.052(4) C21 0.073(3) 0.081(3) 0.047(3) 0.021(3) 0.009(3) 0.025(3) C60 0.090(4) 0.110(4) 0.054(3) 0.021(3) 0.015(3) 0.046(3) C3 0.076(3) 0.076(3) 0.045(3) -0.021(3) 0.007(3) -0.014(3) O10 0.286(13) 0.107(7) 0.131(7) -0.068(6) -0.095(7) 0.045(8) C6 0.076(3) 0.073(3) 0.047(3) -0.018(3) 0.011(2) -0.016(3) N4 0.086(5) 0.056(4) 0.076(5) 0.009(3) -0.013(4) -0.004(3) C43 0.091(4) 0.072(4) 0.075(4) 0.018(3) -0.015(3) 0.004(3) C63 0.079(3) 0.101(4) 0.039(3) 0.021(3) 0.012(3) 0.032(3) C55 0.088(4) 0.095(4) 0.046(3) 0.016(3) 0.009(3) 0.036(4) C7 0.078(3) 0.082(4) 0.053(3) -0.018(3) 0.006(3) -0.024(3) C59 0.081(4) 0.092(4) 0.032(3) 0.018(3) 0.003(3) 0.018(3) C56 0.087(3) 0.088(4) 0.037(3) 0.018(3) 0.010(3) 0.033(3) C64 0.086(3) 0.099(4) 0.043(3) 0.020(3) 0.009(3) 0.026(3) C4 0.067(3) 0.074(3) 0.049(3) -0.016(3) 0.005(2) -0.018(3) C20 0.072(3) 0.076(3) 0.043(2) 0.016(3) 0.013(2) 0.016(3) C40 0.077(3) 0.089(3) 0.069(3) -0.018(3) -0.012(3) -0.001(3) C61 0.097(4) 0.109(4) 0.044(3) 0.019(3) 0.017(3) 0.040(3) C45 0.078(3) 0.086(3) 0.074(3) 0.021(3) -0.002(3) 0.002(3) C41 0.085(3) 0.097(4) 0.078(3) -0.017(3) -0.008(3) -0.008(3) C44 0.091(4) 0.094(4) 0.084(3) 0.022(3) -0.012(3) 0.005(3) C38 0.089(3) 0.087(3) 0.080(3) -0.022(3) -0.017(3) 0.001(3) C47 0.088(3) 0.087(3) 0.085(3) 0.026(3) -0.016(3) -0.003(3) C48 0.098(4) 0.090(4) 0.088(4) 0.032(3) -0.010(3) -0.009(3) C37 0.106(4) 0.094(4) 0.084(4) -0.032(3) -0.013(3) 0.009(4) C42 0.128(4) 0.079(4) 0.076(4) 0.022(4) -0.003(4) 0.008(4) O12 0.297(14) 0.120(8) 0.146(8) 0.071(7) -0.115(8) -0.045(8) C35 0.127(4) 0.084(4) 0.067(4) -0.008(4) -0.008(4) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.297(5) 2_646 ? Cd1 O2 2.350(5) . ? Cd1 O11 2.357(8) 3_675 ? Cd1 N1 2.354(6) . ? Cd1 O1 2.379(5) . ? Cd1 O3 2.477(4) 2_646 ? Cd1 O12 2.457(10) 3_675 ? Cd1 C1 2.715(6) . ? Cd1 C8 2.742(7) 2_646 ? Cd2 O8 2.327(5) . ? Cd2 O6 2.341(4) 4_574 ? Cd2 N2 2.349(6) . ? Cd2 O9 2.366(8) 2_745 ? Cd2 O5 2.366(4) 4_574 ? Cd2 O7 2.450(5) . ? Cd2 O10 2.456(10) 2_745 ? Cd2 C28 2.705(7) . ? Cd2 C15 2.711(6) 4_574 ? C29 C34 1.361(8) . ? C29 C30 1.382(8) . ? C29 C28 1.515(9) . ? C9 C14 1.353(8) . ? C9 C10 1.393(8) . ? C9 C8 1.483(9) . ? O3 C8 1.259(8) . ? O3 Cd1 2.477(4) 2_656 ? O7 C28 1.254(8) . ? C5 C6 1.359(9) . ? C5 C4 1.372(9) . ? C5 C22 1.473(8) . ? C1 O1 1.246(7) . ? C1 O2 1.270(8) . ? C1 C2 1.475(8) . ? O5 C15 1.234(8) . ? O5 Cd2 2.366(4) 4_577 ? C19 C18 1.348(9) . ? C19 C20 1.387(9) . ? C19 C24 1.508(8) . ? C2 C7 1.369(9) . ? C2 C3 1.355(9) . ? C27 C26 1.403(8) . ? C27 C22 1.413(8) . ? C27 H27A 0.9300 . ? C16 C21 1.367(9) . ? C16 C17 1.373(9) . ? C16 C15 1.480(8) . ? C22 C23 1.384(8) . ? C24 C23 1.389(8) . ? C24 C25 1.405(8) . ? O4 C8 1.256(8) . ? O4 Cd1 2.297(5) 2_656 ? N2 C60 1.294(9) . ? N2 C64 1.324(9) . ? C25 C26 1.407(7) . ? C25 H25A 0.9300 . ? C15 O6 1.259(8) . ? C15 Cd2 2.711(6) 4_577 ? O6 Cd2 2.341(4) 4_577 ? C13 C14 1.379(8) . ? C13 C12 1.395(7) . ? C13 H13A 0.9300 . ? C62 C63 1.335(8) . ? C62 C61 1.383(10) . ? C62 C57 1.486(10) . ? O8 C28 1.253(8) . ? C8 Cd1 2.742(7) 2_656 ? C12 C11 1.392(8) . ? C12 C26 1.477(8) . ? C57 C58 1.364(8) . ? C57 C56 1.398(9) . ? N1 C55 1.302(9) . ? N1 C59 1.312(8) . ? C53 C54 1.397(9) . ? C53 C52 1.421(9) . ? C53 C39 1.477(9) . ? C14 H14A 0.9300 . ? C54 C49 1.370(8) . ? C54 H54A 0.9300 . ? C50 C49 1.378(8) . ? C50 C51 1.398(9) . ? C50 H50A 0.9300 . ? C32 C31 1.412(8) . ? C32 C33 1.414(8) . ? C32 C49 1.509(9) . ? C10 C11 1.390(8) . ? C10 H10A 0.9300 . ? C23 N3 1.396(9) . ? C34 C33 1.371(8) . ? C34 H34A 0.9300 . ? C46 C47 1.355(11) . ? C46 C45 1.401(10) . ? C46 C51 1.479(9) . ? C39 C38 1.348(11) . ? C39 C40 1.386(10) . ? C30 C31 1.376(9) . ? C30 H30A 0.9300 . ? C33 H33A 0.9300 . ? C11 H11A 0.9300 . ? C31 H31A 0.9300 . ? C51 C52 1.407(9) . ? C52 N4 1.394(9) . ? C36 C37 1.339(12) . ? C36 C41 1.393(12) . ? C36 C35 1.521(12) . ? O9 C35 1.215(12) . ? O9 Cd2 2.366(8) 2_755 ? C17 C18 1.407(9) . ? C17 H17A 0.9300 . ? N3 H3B 0.8600 . ? N3 H3C 0.8600 . ? C18 H18A 0.9300 . ? C58 C59 1.393(10) . ? C58 H58A 0.9300 . ? O11 C42 1.217(13) . ? O11 Cd1 2.357(8) 3_675 ? C21 C20 1.402(9) . ? C21 H21A 0.9300 . ? C60 C61 1.379(11) . ? C60 H60A 0.9300 . ? C3 C4 1.388(9) . ? C3 H3A 0.9300 . ? O10 C35 1.079(13) . ? O10 Cd2 2.456(10) 2_755 ? C6 C7 1.410(9) . ? C6 H6A 0.9300 . ? N4 H4B 0.8600 . ? N4 H4C 0.8600 . ? C43 C48 1.289(11) . ? C43 C44 1.442(12) . ? C43 C42 1.519(12) . ? C63 C64 1.387(10) . ? C63 H63A 0.9300 . ? C55 C56 1.388(11) . ? C55 H55A 0.9300 . ? C7 H7A 0.9300 . ? C59 H59A 0.9300 . ? C56 H56A 0.9300 . ? C64 H64A 0.9300 . ? C4 H4A 0.9300 . ? C20 H20A 0.9300 . ? C40 C41 1.414(10) . ? C40 H40A 0.9300 . ? C61 H61A 0.9300 . ? C45 C44 1.403(10) . ? C45 H45A 0.9300 . ? C41 H41A 0.9300 . ? C44 H44A 0.9300 . ? C38 C37 1.419(11) . ? C38 H38A 0.9300 . ? C47 C48 1.394(11) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C37 H37A 0.9300 . ? C42 O12 1.035(12) . ? O12 Cd1 2.457(10) 3_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 O2 108.0(2) 2_646 . ? O4 Cd1 O11 128.7(2) 2_646 3_675 ? O2 Cd1 O11 96.3(2) . 3_675 ? O4 Cd1 N1 99.5(2) 2_646 . ? O2 Cd1 N1 143.21(18) . . ? O11 Cd1 N1 84.7(2) 3_675 . ? O4 Cd1 O1 141.43(19) 2_646 . ? O2 Cd1 O1 55.18(16) . . ? O11 Cd1 O1 89.5(2) 3_675 . ? N1 Cd1 O1 88.12(18) . . ? O4 Cd1 O3 54.34(17) 2_646 2_646 ? O2 Cd1 O3 91.12(18) . 2_646 ? O11 Cd1 O3 169.9(2) 3_675 2_646 ? N1 Cd1 O3 85.24(19) . 2_646 ? O1 Cd1 O3 89.17(17) . 2_646 ? O4 Cd1 O12 83.2(3) 2_646 3_675 ? O2 Cd1 O12 103.3(3) . 3_675 ? O11 Cd1 O12 46.9(3) 3_675 3_675 ? N1 Cd1 O12 103.9(3) . 3_675 ? O1 Cd1 O12 131.8(3) . 3_675 ? O3 Cd1 O12 137.5(3) 2_646 3_675 ? O4 Cd1 C1 128.1(2) 2_646 . ? O2 Cd1 C1 27.87(18) . . ? O11 Cd1 C1 93.2(2) 3_675 . ? N1 Cd1 C1 115.4(2) . . ? O1 Cd1 C1 27.31(17) . . ? O3 Cd1 C1 90.14(18) 2_646 . ? O12 Cd1 C1 120.6(3) 3_675 . ? O4 Cd1 C8 27.07(18) 2_646 2_646 ? O2 Cd1 C8 101.89(19) . 2_646 ? O11 Cd1 C8 154.1(2) 3_675 2_646 ? N1 Cd1 C8 91.40(19) . 2_646 ? O1 Cd1 C8 116.00(19) . 2_646 ? O3 Cd1 C8 27.32(16) 2_646 2_646 ? O12 Cd1 C8 110.2(3) 3_675 2_646 ? C1 Cd1 C8 111.38(19) . 2_646 ? O8 Cd2 O6 109.4(2) . 4_574 ? O8 Cd2 N2 95.3(2) . . ? O6 Cd2 N2 144.81(18) 4_574 . ? O8 Cd2 O9 127.9(2) . 2_745 ? O6 Cd2 O9 98.3(2) 4_574 2_745 ? N2 Cd2 O9 84.8(2) . 2_745 ? O8 Cd2 O5 142.07(18) . 4_574 ? O6 Cd2 O5 54.70(16) 4_574 4_574 ? N2 Cd2 O5 90.42(18) . 4_574 ? O9 Cd2 O5 90.0(2) 2_745 4_574 ? O8 Cd2 O7 55.03(16) . . ? O6 Cd2 O7 89.99(18) 4_574 . ? N2 Cd2 O7 83.97(19) . . ? O9 Cd2 O7 168.7(2) 2_745 . ? O5 Cd2 O7 88.57(17) 4_574 . ? O8 Cd2 O10 82.2(2) . 2_745 ? O6 Cd2 O10 103.0(3) 4_574 2_745 ? N2 Cd2 O10 104.9(3) . 2_745 ? O9 Cd2 O10 48.3(3) 2_745 2_745 ? O5 Cd2 O10 132.3(3) 4_574 2_745 ? O7 Cd2 O10 137.1(2) . 2_745 ? O8 Cd2 C28 27.54(18) . . ? O6 Cd2 C28 102.3(2) 4_574 . ? N2 Cd2 C28 88.0(2) . . ? O9 Cd2 C28 153.2(2) 2_745 . ? O5 Cd2 C28 115.9(2) 4_574 . ? O7 Cd2 C28 27.58(17) . . ? O10 Cd2 C28 109.7(3) 2_745 . ? O8 Cd2 C15 129.3(2) . 4_574 ? O6 Cd2 C15 27.64(18) 4_574 4_574 ? N2 Cd2 C15 117.4(2) . 4_574 ? O9 Cd2 C15 94.6(2) 2_745 4_574 ? O5 Cd2 C15 27.06(17) 4_574 4_574 ? O7 Cd2 C15 89.18(18) . 4_574 ? O10 Cd2 C15 120.5(3) 2_745 4_574 ? C28 Cd2 C15 111.5(2) . 4_574 ? C34 C29 C30 118.7(6) . . ? C34 C29 C28 120.5(6) . . ? C30 C29 C28 120.7(6) . . ? C14 C9 C10 118.1(6) . . ? C14 C9 C8 121.5(6) . . ? C10 C9 C8 120.2(6) . . ? C8 O3 Cd1 88.1(4) . 2_656 ? C28 O7 Cd2 87.6(4) . . ? C6 C5 C4 115.9(6) . . ? C6 C5 C22 122.4(6) . . ? C4 C5 C22 121.6(6) . . ? O1 C1 O2 121.0(6) . . ? O1 C1 C2 119.5(6) . . ? O2 C1 C2 119.5(6) . . ? O1 C1 Cd1 61.2(3) . . ? O2 C1 Cd1 59.9(3) . . ? C2 C1 Cd1 179.1(5) . . ? C15 O5 Cd2 92.2(4) . 4_577 ? C18 C19 C20 118.0(6) . . ? C18 C19 C24 122.6(6) . . ? C20 C19 C24 119.4(5) . . ? C7 C2 C3 118.3(6) . . ? C7 C2 C1 120.1(6) . . ? C3 C2 C1 121.6(6) . . ? C26 C27 C22 122.1(6) . . ? C26 C27 H27A 119.0 . . ? C22 C27 H27A 119.0 . . ? C21 C16 C17 118.5(6) . . ? C21 C16 C15 121.5(6) . . ? C17 C16 C15 120.0(6) . . ? C23 C22 C27 118.5(5) . . ? C23 C22 C5 122.0(6) . . ? C27 C22 C5 119.4(5) . . ? C1 O1 Cd1 91.5(4) . . ? C23 C24 C25 118.7(5) . . ? C23 C24 C19 121.3(6) . . ? C25 C24 C19 120.0(5) . . ? C8 O4 Cd1 96.6(4) . 2_656 ? C60 N2 C64 115.5(6) . . ? C60 N2 Cd2 125.4(5) . . ? C64 N2 Cd2 119.1(4) . . ? C26 C25 C24 122.1(5) . . ? C26 C25 H25A 119.0 . . ? C24 C25 H25A 119.0 . . ? O5 C15 O6 120.3(6) . . ? O5 C15 C16 121.2(6) . . ? O6 C15 C16 118.4(6) . . ? O5 C15 Cd2 60.7(3) . 4_577 ? O6 C15 Cd2 59.6(3) . 4_577 ? C16 C15 Cd2 177.3(5) . 4_577 ? C15 O6 Cd2 92.7(4) . 4_577 ? C14 C13 C12 120.8(6) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C63 C62 C61 115.7(7) . . ? C63 C62 C57 122.1(6) . . ? C61 C62 C57 122.2(6) . . ? C28 O8 Cd2 93.3(4) . . ? C1 O2 Cd1 92.3(4) . . ? O3 C8 O4 120.7(6) . . ? O3 C8 C9 118.7(6) . . ? O4 C8 C9 120.4(6) . . ? O3 C8 Cd1 64.6(3) . 2_656 ? O4 C8 Cd1 56.3(3) . 2_656 ? C9 C8 Cd1 170.1(5) . 2_656 ? C11 C12 C13 117.5(6) . . ? C11 C12 C26 121.8(5) . . ? C13 C12 C26 120.7(5) . . ? C58 C57 C56 116.2(6) . . ? C58 C57 C62 121.3(6) . . ? C56 C57 C62 122.5(6) . . ? O7 C28 O8 123.6(7) . . ? O7 C28 C29 118.0(6) . . ? O8 C28 C29 118.2(6) . . ? O7 C28 Cd2 64.8(4) . . ? O8 C28 Cd2 59.2(4) . . ? C29 C28 Cd2 169.5(5) . . ? C55 N1 C59 117.3(6) . . ? C55 N1 Cd1 124.8(5) . . ? C59 N1 Cd1 117.9(4) . . ? C54 C53 C52 118.5(6) . . ? C54 C53 C39 119.8(6) . . ? C52 C53 C39 121.8(7) . . ? C9 C14 C13 122.0(6) . . ? C9 C14 H14A 119.0 . . ? C13 C14 H14A 119.0 . . ? C49 C54 C53 121.6(6) . . ? C49 C54 H54A 119.2 . . ? C53 C54 H54A 119.2 . . ? C49 C50 C51 120.4(6) . . ? C49 C50 H50A 119.8 . . ? C51 C50 H50A 119.8 . . ? C31 C32 C33 117.4(6) . . ? C31 C32 C49 121.2(5) . . ? C33 C32 C49 121.4(5) . . ? C54 C49 C50 120.4(7) . . ? C54 C49 C32 120.1(6) . . ? C50 C49 C32 119.5(6) . . ? C9 C10 C11 120.7(6) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C22 C23 C24 121.7(6) . . ? C22 C23 N3 120.1(6) . . ? C24 C23 N3 118.1(5) . . ? C29 C34 C33 121.7(6) . . ? C29 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? C27 C26 C25 116.9(6) . . ? C27 C26 C12 121.7(5) . . ? C25 C26 C12 121.4(5) . . ? C47 C46 C45 118.8(7) . . ? C47 C46 C51 123.5(7) . . ? C45 C46 C51 117.7(6) . . ? C38 C39 C40 118.4(7) . . ? C38 C39 C53 123.5(7) . . ? C40 C39 C53 118.0(7) . . ? C29 C30 C31 121.6(6) . . ? C29 C30 H30A 119.2 . . ? C31 C30 H30A 119.2 . . ? C34 C33 C32 120.4(6) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C12 C11 C10 120.6(6) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C30 C31 C32 119.9(6) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C52 C51 C50 119.7(6) . . ? C52 C51 C46 121.9(6) . . ? C50 C51 C46 118.4(6) . . ? C51 C52 N4 120.7(6) . . ? C51 C52 C53 119.4(7) . . ? N4 C52 C53 119.9(6) . . ? C37 C36 C41 118.8(8) . . ? C37 C36 C35 121.5(9) . . ? C41 C36 C35 119.5(9) . . ? C35 O9 Cd2 96.3(7) . 2_755 ? C16 C17 C18 119.7(7) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C23 N3 H3B 120.0 . . ? C23 N3 H3C 120.0 . . ? H3B N3 H3C 120.0 . . ? C19 C18 C17 122.2(6) . . ? C19 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? C57 C58 C59 119.0(6) . . ? C57 C58 H58A 120.5 . . ? C59 C58 H58A 120.5 . . ? C42 O11 Cd1 97.8(7) . 3_675 ? C16 C21 C20 121.2(7) . . ? C16 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? N2 C60 C61 123.8(8) . . ? N2 C60 H60A 118.1 . . ? C61 C60 H60A 118.1 . . ? C2 C3 C4 121.1(7) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C35 O10 Cd2 95.5(10) . 2_755 ? C5 C6 C7 122.7(7) . . ? C5 C6 H6A 118.6 . . ? C7 C6 H6A 118.6 . . ? C52 N4 H4B 120.0 . . ? C52 N4 H4C 120.0 . . ? H4B N4 H4C 120.0 . . ? C48 C43 C44 117.8(8) . . ? C48 C43 C42 125.0(9) . . ? C44 C43 C42 117.1(8) . . ? C62 C63 C64 120.2(7) . . ? C62 C63 H63A 119.9 . . ? C64 C63 H63A 119.9 . . ? N1 C55 C56 122.8(7) . . ? N1 C55 H55A 118.6 . . ? C56 C55 H55A 118.6 . . ? C2 C7 C6 119.6(7) . . ? C2 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? N1 C59 C58 124.4(6) . . ? N1 C59 H59A 117.8 . . ? C58 C59 H59A 117.8 . . ? C55 C56 C57 120.2(6) . . ? C55 C56 H56A 119.9 . . ? C57 C56 H56A 119.9 . . ? N2 C64 C63 124.1(6) . . ? N2 C64 H64A 118.0 . . ? C63 C64 H64A 118.0 . . ? C5 C4 C3 122.3(7) . . ? C5 C4 H4A 118.9 . . ? C3 C4 H4A 118.9 . . ? C19 C20 C21 120.2(6) . . ? C19 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 . . ? C39 C40 C41 119.2(8) . . ? C39 C40 H40A 120.4 . . ? C41 C40 H40A 120.4 . . ? C60 C61 C62 120.4(7) . . ? C60 C61 H61A 119.8 . . ? C62 C61 H61A 119.8 . . ? C44 C45 C46 119.0(8) . . ? C44 C45 H45A 120.5 . . ? C46 C45 H45A 120.5 . . ? C36 C41 C40 121.1(8) . . ? C36 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? C45 C44 C43 119.9(8) . . ? C45 C44 H44A 120.1 . . ? C43 C44 H44A 120.1 . . ? C39 C38 C37 122.5(8) . . ? C39 C38 H38A 118.7 . . ? C37 C38 H38A 118.7 . . ? C46 C47 C48 120.9(8) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? C43 C48 C47 123.4(9) . . ? C43 C48 H48A 118.3 . . ? C47 C48 H48A 118.3 . . ? C36 C37 C38 119.9(9) . . ? C36 C37 H37A 120.1 . . ? C38 C37 H37A 120.1 . . ? O12 C42 O11 116.4(12) . . ? O12 C42 C43 122.5(13) . . ? O11 C42 C43 120.5(10) . . ? C42 O12 Cd1 98.0(11) . 3_675 ? O10 C35 O9 118.7(11) . . ? O10 C35 C36 122.2(12) . . ? O9 C35 C36 118.9(10) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.329 _refine_diff_density_min -1.265 _refine_diff_density_rms 0.114 _database_code_depnum_ccdc_archive 'CCDC 966925' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H28 Cd2 N2 O14' _chemical_formula_sum 'C64 H28 Cd2 N2 O14' _chemical_formula_weight 1273.71 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 P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0229(8) _cell_length_b 29.8118(10) _cell_length_c 16.1301(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.179(4) _cell_angle_gamma 90.00 _cell_volume 8080.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8169 _cell_measurement_theta_min 2.3781 _cell_measurement_theta_max 28.4057 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536.0 _exptl_absorpt_coefficient_mu 0.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.933 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_process_details ? _exptl_special_details ; # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.898 0.272 0.028 3422.1 220.9 _platon_squeeze_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 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 31346 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14244 _reflns_number_gt 9337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1142P)^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 13933 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.2037 _refine_ls_wR_factor_gt 0.1870 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 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 0.40365(3) 0.720989(13) 0.47796(3) 0.04537(16) Uani 1 1 d . . . Cd2 Cd 0.14299(3) 1.210588(14) -0.01303(3) 0.04519(15) Uani 1 1 d . . . C1 C 0.3044(7) 0.6653(4) 0.3679(6) 0.101(3) Uani 1 1 d . . . C2 C 0.2614(6) 0.6391(2) 0.2946(5) 0.085(2) Uani 1 1 d . . . C3 C 0.1887(6) 0.6448(4) 0.2605(8) 0.168(6) Uani 1 1 d . . . C4 C 0.1526(6) 0.6227(4) 0.1884(7) 0.139(5) Uani 1 1 d . . . C5 C 0.1911(4) 0.5925(2) 0.1516(4) 0.0576(16) Uani 1 1 d . . . C6 C 0.2730(5) 0.5814(3) 0.1876(6) 0.104(3) Uani 1 1 d . . . C7 C 0.3104(6) 0.6040(4) 0.2596(6) 0.125(4) Uani 1 1 d . . . C8 C 0.1306(4) 0.3006(2) 0.0179(4) 0.0506(15) Uani 1 1 d . . . C9 C 0.1278(4) 0.3502(2) 0.0196(4) 0.0556(16) Uani 1 1 d . . . C10 C 0.1860(4) 0.37536(18) 0.0666(4) 0.0517(15) Uani 1 1 d . . . H10 H 0.2268 0.3608 0.1017 0.062 Uiso 1 1 calc R . . C11 C 0.1860(3) 0.42088(18) 0.0633(4) 0.0505(14) Uani 1 1 d . . . H11 H 0.2274 0.4366 0.0953 0.061 Uiso 1 1 calc R . . C12 C 0.1255(3) 0.44479(18) 0.0132(4) 0.0457(13) Uani 1 1 d . . . C13 C 0.0645(3) 0.41918(19) -0.0327(4) 0.0517(15) Uani 1 1 d . . . H13A H 0.0227 0.4337 -0.0664 0.062 Uiso 1 1 calc R . . C14 C 0.0651(3) 0.37341(19) -0.0291(4) 0.0550(16) Uani 1 1 d . . . H14 H 0.0232 0.3574 -0.0595 0.066 Uiso 1 1 calc R . . C15 C -0.0488(6) 0.6534(3) -0.3754(5) 0.081(2) Uani 1 1 d . . . C16 C -0.0067(5) 0.6288(2) -0.3013(5) 0.071(2) Uani 1 1 d . . . C17 C -0.0493(5) 0.5961(3) -0.2606(5) 0.095(3) Uani 1 1 d . . . H17 H -0.1015 0.5891 -0.2834 0.114 Uiso 1 1 calc R . . C18 C -0.0147(4) 0.5752(3) -0.1894(5) 0.085(2) Uani 1 1 d . . . H18 H -0.0427 0.5533 -0.1652 0.102 Uiso 1 1 calc R . . C19 C 0.0629(4) 0.58637(19) -0.1521(4) 0.0548(15) Uani 1 1 d . . . C20 C 0.1010(5) 0.6169(3) -0.1909(6) 0.108(3) Uani 1 1 d . . . H20 H 0.1526 0.6249 -0.1675 0.129 Uiso 1 1 calc R . . C21 C 0.0668(6) 0.6368(3) -0.2638(6) 0.126(4) Uani 1 1 d . . . H21 H 0.0970 0.6573 -0.2887 0.151 Uiso 1 1 calc R . . C22 C 0.1562(3) 0.56685(18) 0.0750(4) 0.0463(14) Uani 1 1 d . . . C23 C 0.1556(3) 0.51935(18) 0.0790(4) 0.0493(14) Uani 1 1 d . . . C24 C 0.1258(3) 0.49387(18) 0.0084(4) 0.0445(13) Uani 1 1 d . . . C25 C 0.0962(3) 0.51603(18) -0.0646(4) 0.0505(14) Uani 1 1 d . . . C26 C 0.0969(3) 0.56372(18) -0.0706(4) 0.0485(14) Uani 1 1 d . . . C27 C 0.1276(3) 0.58852(19) 0.0006(4) 0.0489(14) Uani 1 1 d . . . C28 C 0.3953(4) 0.8108(2) 0.5106(4) 0.0507(14) Uani 1 1 d . . . C29 C 0.3884(3) 0.86077(18) 0.5140(3) 0.0449(14) Uani 1 1 d . . . C30 C 0.4466(3) 0.88584(18) 0.5606(4) 0.0481(14) Uani 1 1 d . . . H30 H 0.4893 0.8715 0.5929 0.058 Uiso 1 1 calc R . . C31 C 0.4431(3) 0.93243(18) 0.5606(4) 0.0480(14) Uani 1 1 d . . . H31 H 0.4838 0.9486 0.5926 0.058 Uiso 1 1 calc R . . C32 C 0.3795(3) 0.95538(18) 0.5133(3) 0.0419(13) Uani 1 1 d . . . C33 C 0.3190(3) 0.92908(18) 0.4678(4) 0.0499(14) Uani 1 1 d . . . H33 H 0.2754 0.9431 0.4361 0.060 Uiso 1 1 calc R . . C34 C 0.3229(3) 0.88318(18) 0.4691(4) 0.0470(14) Uani 1 1 d . . . H34 H 0.2813 0.8666 0.4396 0.056 Uiso 1 1 calc R . . C35 C 0.5349(4) 1.17631(19) 0.8809(4) 0.0498(14) Uani 1 1 d . . . C36 C 0.5015(3) 1.15079(18) 0.8036(4) 0.0458(13) Uani 1 1 d . . . C37 C 0.4297(5) 1.1279(3) 0.7984(5) 0.087(3) Uani 1 1 d . . . H37 H 0.4025 1.1283 0.8441 0.105 Uiso 1 1 calc R . . C38 C 0.3975(4) 1.1042(3) 0.7261(4) 0.080(2) Uani 1 1 d . . . H38 H 0.3495 1.0890 0.7243 0.096 Uiso 1 1 calc R . . C39 C 0.4358(3) 1.10316(17) 0.6583(4) 0.0457(13) Uani 1 1 d . . . C40 C 0.5042(5) 1.1284(3) 0.6625(4) 0.085(2) Uani 1 1 d . . . H40 H 0.5293 1.1298 0.6154 0.101 Uiso 1 1 calc R . . C41 C 0.5375(4) 1.1518(2) 0.7350(4) 0.077(2) Uani 1 1 d . . . H41 H 0.5842 1.1680 0.7357 0.092 Uiso 1 1 calc R . . C42 C 0.2079(4) 1.16648(19) 0.1279(4) 0.0502(14) Uani 1 1 d . . . C43 C 0.2424(3) 1.14294(18) 0.2061(4) 0.0468(14) Uani 1 1 d . . . C44 C 0.2057(4) 1.1431(3) 0.2760(4) 0.085(3) Uani 1 1 d . . . H44 H 0.1575 1.1581 0.2741 0.102 Uiso 1 1 calc R . . C45 C 0.2390(4) 1.1215(3) 0.3496(4) 0.088(3) Uani 1 1 d . . . H45 H 0.2126 1.1225 0.3958 0.106 Uiso 1 1 calc R . . C46 C 0.3090(3) 1.09886(17) 0.3560(4) 0.0448(13) Uani 1 1 d . . . C47 C 0.3478(4) 1.0994(3) 0.2869(4) 0.078(2) Uani 1 1 d . . . H47 H 0.3967 1.0850 0.2898 0.094 Uiso 1 1 calc R . . C48 C 0.3148(4) 1.1211(3) 0.2132(4) 0.077(2) Uani 1 1 d . . . H48 H 0.3420 1.1209 0.1676 0.092 Uiso 1 1 calc R . . C49 C 0.3766(3) 1.00516(17) 0.5113(3) 0.0418(13) Uani 1 1 d . . . C50 C 0.3447(3) 1.02769(17) 0.4371(4) 0.0462(14) Uani 1 1 d . . . C51 C 0.3429(3) 1.07476(18) 0.4353(3) 0.0438(13) Uani 1 1 d . . . C52 C 0.3729(3) 1.09894(17) 0.5077(3) 0.0447(14) Uani 1 1 d . . . C53 C 0.4035(3) 1.07731(17) 0.5817(3) 0.0431(13) Uani 1 1 d . . . C54 C 0.4053(3) 1.03004(18) 0.5834(4) 0.0466(14) Uani 1 1 d . . . C55 C 0.4437(4) 1.2465(3) -0.4054(4) 0.076(2) Uani 1 1 d . . . H55 H 0.4345 1.2352 -0.4599 0.091 Uiso 1 1 calc R . . C56 C 0.3854(4) 1.2401(3) -0.3552(4) 0.074(2) Uani 1 1 d . . . H56 H 0.3381 1.2257 -0.3769 0.088 Uiso 1 1 calc R . . C57 C 0.3975(3) 1.25500(18) -0.2739(3) 0.0461(13) Uani 1 1 d . . . C58 C 0.4682(4) 1.2755(2) -0.2477(4) 0.068(2) Uani 1 1 d . . . H58 H 0.4804 1.2856 -0.1926 0.081 Uiso 1 1 calc R . . C59 C 0.5223(5) 1.2815(2) -0.3019(4) 0.073(2) Uani 1 1 d . . . H59 H 0.5697 1.2963 -0.2821 0.088 Uiso 1 1 calc R . . C60 C 0.2898(4) 1.2531(3) -0.0873(4) 0.090(3) Uani 1 1 d . . . H60 H 0.2981 1.2647 -0.0330 0.108 Uiso 1 1 calc R . . C61 C 0.3463(4) 1.2629(3) -0.1400(4) 0.092(3) Uani 1 1 d . . . H61 H 0.3898 1.2811 -0.1203 0.111 Uiso 1 1 calc R . . C62 C 0.3377(3) 1.24644(18) -0.2177(3) 0.0444(13) Uani 1 1 d . . . C63 C 0.2684(6) 1.2240(3) -0.2436(5) 0.126(4) Uani 1 1 d . . . H63 H 0.2557 1.2145 -0.2991 0.151 Uiso 1 1 calc R . . C64 C 0.2173(6) 1.2153(3) -0.1878(6) 0.122(4) Uani 1 1 d . . . H64 H 0.1721 1.1984 -0.2070 0.147 Uiso 1 1 calc R . . O1 O 0.3697(5) 0.6524(3) 0.4060(4) 0.136(3) Uani 1 1 d . . . O2 O 0.2836(6) 0.6986(3) 0.3869(6) 0.193(5) Uani 1 1 d . . . O3 O 0.1918(3) 0.28094(13) 0.0547(3) 0.0619(12) Uani 1 1 d . . . O4 O 0.0739(3) 0.27860(14) -0.0232(4) 0.0736(14) Uani 1 1 d . . . O5 O -0.1153(4) 0.6422(2) -0.4080(4) 0.118(2) Uani 1 1 d . . . O6 O -0.0228(5) 0.6859(2) -0.3981(5) 0.157(4) Uani 1 1 d . . . O7 O 0.4577(3) 0.79240(13) 0.5419(3) 0.0607(11) Uani 1 1 d . . . O8 O 0.3374(3) 0.78856(13) 0.4728(4) 0.0723(14) Uani 1 1 d . . . O9 O 0.6041(3) 1.19162(15) 0.8880(3) 0.0657(12) Uani 1 1 d . . . O10 O 0.4929(3) 1.18114(15) 0.9385(3) 0.0667(12) Uani 1 1 d . . . O11 O 0.1365(3) 1.18021(16) 0.1200(3) 0.0692(13) Uani 1 1 d . . . O12 O 0.2491(3) 1.17182(15) 0.0708(3) 0.0649(12) Uani 1 1 d . . . O13 O 0.3721(4) 1.1447(2) 0.5028(4) 0.122(2) Uani 1 1 d . . . O14 O 0.1285(3) 0.63538(18) -0.0041(3) 0.0931(18) Uani 1 1 d . . . N1 N 0.2272(3) 1.22882(17) -0.1103(3) 0.0574(13) Uani 1 1 d . . . N2 N 0.5104(3) 1.26738(17) -0.3804(3) 0.0530(12) 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 0.0570(3) 0.0433(3) 0.0333(3) 0.00066(17) -0.0005(2) 0.00044(18) Cd2 0.0540(3) 0.0478(3) 0.0322(3) 0.00157(17) 0.0018(2) 0.00061(18) C1 0.131(9) 0.102(7) 0.058(6) -0.004(5) -0.019(6) -0.010(7) C2 0.116(7) 0.067(5) 0.066(5) -0.023(4) -0.007(5) -0.024(5) C3 0.099(7) 0.229(13) 0.151(11) -0.137(10) -0.059(7) 0.064(8) C4 0.103(7) 0.175(10) 0.122(9) -0.093(8) -0.038(6) 0.053(7) C5 0.060(4) 0.052(4) 0.053(4) -0.001(3) -0.012(3) -0.006(3) C6 0.076(6) 0.145(8) 0.082(7) -0.031(6) -0.018(5) -0.011(5) C7 0.102(7) 0.175(10) 0.094(8) -0.052(7) 0.003(6) -0.031(7) C8 0.063(4) 0.051(4) 0.040(4) 0.000(3) 0.014(3) 0.001(3) C9 0.056(4) 0.050(4) 0.052(4) 0.008(3) -0.020(3) 0.005(3) C10 0.057(4) 0.048(3) 0.048(4) 0.001(3) 0.001(3) 0.005(3) C11 0.049(3) 0.051(4) 0.048(4) -0.003(3) -0.003(3) -0.004(3) C12 0.047(3) 0.046(3) 0.041(3) -0.002(2) -0.002(3) 0.004(3) C13 0.039(3) 0.054(4) 0.058(4) -0.004(3) -0.004(3) 0.004(3) C14 0.044(3) 0.052(4) 0.070(5) -0.014(3) 0.013(3) -0.006(3) C15 0.109(7) 0.068(5) 0.055(5) -0.004(4) -0.024(5) 0.021(5) C16 0.087(5) 0.057(4) 0.060(5) 0.000(3) -0.016(4) 0.011(4) C17 0.066(5) 0.151(8) 0.059(5) 0.018(5) -0.015(4) -0.001(5) C18 0.062(5) 0.120(7) 0.066(5) 0.029(4) -0.012(4) -0.006(4) C19 0.054(4) 0.053(4) 0.052(4) -0.002(3) -0.009(3) 0.005(3) C20 0.071(5) 0.121(7) 0.117(8) 0.069(6) -0.032(5) -0.029(5) C21 0.124(8) 0.125(8) 0.112(9) 0.067(7) -0.033(7) -0.045(6) C22 0.042(3) 0.044(3) 0.050(4) -0.010(3) -0.002(3) -0.003(2) C23 0.037(3) 0.050(3) 0.057(4) -0.001(3) -0.003(3) 0.003(3) C24 0.041(3) 0.041(3) 0.048(4) 0.002(3) -0.002(3) 0.002(2) C25 0.047(3) 0.049(3) 0.054(4) 0.001(3) 0.002(3) 0.001(3) C26 0.046(3) 0.044(3) 0.053(4) 0.001(3) -0.001(3) -0.003(3) C27 0.046(3) 0.041(3) 0.054(4) 0.000(3) -0.007(3) -0.004(2) C28 0.059(4) 0.047(3) 0.047(4) 0.005(3) 0.008(3) 0.008(3) C29 0.047(3) 0.045(3) 0.043(4) 0.004(2) 0.004(3) 0.000(3) C30 0.048(3) 0.047(3) 0.045(4) 0.004(3) -0.005(3) 0.006(3) C31 0.046(3) 0.043(3) 0.050(4) 0.002(3) -0.007(3) -0.001(3) C32 0.039(3) 0.046(3) 0.040(3) 0.001(2) 0.004(3) 0.002(2) C33 0.049(3) 0.049(3) 0.048(4) 0.001(3) -0.004(3) 0.002(3) C34 0.037(3) 0.045(3) 0.056(4) -0.001(3) -0.002(3) 0.005(2) C35 0.061(4) 0.051(3) 0.037(4) -0.002(3) 0.006(3) 0.000(3) C36 0.050(3) 0.049(3) 0.038(3) -0.007(2) 0.007(3) 0.000(3) C37 0.095(6) 0.120(7) 0.051(5) -0.028(4) 0.025(4) -0.038(5) C38 0.073(5) 0.113(6) 0.055(5) -0.020(4) 0.015(4) -0.037(4) C39 0.051(3) 0.038(3) 0.045(4) 0.000(2) -0.001(3) 0.002(3) C40 0.095(6) 0.123(7) 0.038(4) -0.022(4) 0.017(4) -0.038(5) C41 0.088(5) 0.092(5) 0.054(5) -0.027(4) 0.019(4) -0.045(4) C42 0.062(4) 0.050(3) 0.036(3) 0.000(3) 0.001(3) -0.008(3) C43 0.050(3) 0.053(3) 0.038(3) 0.008(3) 0.006(3) 0.001(3) C44 0.080(5) 0.126(7) 0.056(5) 0.038(4) 0.029(4) 0.046(5) C45 0.084(5) 0.134(7) 0.054(5) 0.044(4) 0.034(4) 0.058(5) C46 0.055(3) 0.035(3) 0.042(3) 0.004(2) -0.003(3) 0.002(2) C47 0.069(5) 0.119(6) 0.045(4) 0.009(4) 0.008(4) 0.039(4) C48 0.083(5) 0.111(6) 0.038(4) 0.012(4) 0.015(4) 0.029(4) C49 0.045(3) 0.040(3) 0.041(3) 0.002(2) 0.008(3) -0.001(2) C50 0.049(3) 0.043(3) 0.046(4) -0.002(3) 0.008(3) 0.003(3) C51 0.048(3) 0.049(3) 0.032(3) 0.000(2) -0.001(3) 0.003(3) C52 0.056(3) 0.033(3) 0.044(4) -0.001(2) 0.003(3) 0.004(2) C53 0.052(3) 0.046(3) 0.029(3) 0.000(2) -0.001(3) 0.006(3) C54 0.053(3) 0.046(3) 0.042(3) 0.002(3) 0.011(3) 0.001(3) C55 0.062(4) 0.129(7) 0.038(4) -0.025(4) 0.012(3) -0.016(4) C56 0.061(4) 0.121(6) 0.036(4) -0.018(4) 0.003(3) -0.026(4) C57 0.056(3) 0.049(3) 0.032(3) 0.004(2) 0.002(3) 0.009(3) C58 0.088(5) 0.085(5) 0.032(4) -0.017(3) 0.014(4) -0.034(4) C59 0.088(5) 0.084(5) 0.052(5) -0.022(3) 0.023(4) -0.037(4) C60 0.074(5) 0.164(8) 0.031(4) -0.033(4) 0.008(4) -0.047(5) C61 0.077(5) 0.161(8) 0.042(4) -0.035(5) 0.019(4) -0.048(5) C62 0.051(3) 0.051(3) 0.030(3) 0.004(2) 0.002(3) 0.000(3) C63 0.134(8) 0.194(10) 0.060(6) -0.060(6) 0.048(6) -0.101(7) C64 0.121(8) 0.176(9) 0.081(7) -0.060(6) 0.051(6) -0.101(7) O1 0.154(7) 0.165(7) 0.083(5) -0.023(5) 0.002(5) -0.054(6) O2 0.238(11) 0.125(6) 0.180(9) -0.096(7) -0.077(7) 0.026(7) O3 0.077(3) 0.054(3) 0.050(3) 0.0017(19) -0.004(2) 0.017(2) O4 0.064(3) 0.052(3) 0.096(4) -0.004(2) -0.015(3) -0.001(2) O5 0.113(5) 0.163(6) 0.069(4) 0.028(4) -0.009(4) 0.048(4) O6 0.210(9) 0.106(5) 0.123(7) 0.055(5) -0.068(6) -0.033(6) O7 0.068(3) 0.051(2) 0.057(3) -0.003(2) -0.009(2) 0.015(2) O8 0.062(3) 0.044(2) 0.103(4) -0.007(2) -0.010(3) -0.002(2) O9 0.067(3) 0.076(3) 0.051(3) -0.018(2) -0.002(2) -0.004(2) O10 0.075(3) 0.081(3) 0.043(3) -0.022(2) 0.004(2) -0.008(2) O11 0.065(3) 0.091(3) 0.050(3) 0.023(2) 0.004(2) 0.010(2) O12 0.064(3) 0.087(3) 0.042(3) 0.017(2) 0.006(2) 0.008(2) O13 0.145(6) 0.094(5) 0.114(6) -0.001(4) -0.016(5) 0.008(4) O14 0.105(4) 0.069(3) 0.100(5) 0.000(3) 0.001(4) 0.004(3) N1 0.068(4) 0.069(3) 0.037(3) -0.003(2) 0.015(3) -0.010(3) N2 0.059(3) 0.066(3) 0.028(3) 0.005(2) -0.009(2) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O8 2.304(4) . ? Cd1 N2 2.339(5) 3_675 ? Cd1 O9 2.355(4) 2_646 ? Cd1 O10 2.360(4) 2_646 ? Cd1 O1 2.377(7) . ? Cd1 O2 2.412(8) . ? Cd1 O7 2.478(4) . ? Cd1 C35 2.700(6) 2_646 ? Cd1 C28 2.737(6) . ? Cd2 O4 2.337(4) 1_565 ? Cd2 O11 2.348(4) . ? Cd2 N1 2.352(5) . ? Cd2 O12 2.377(4) . ? Cd2 O5 2.410(6) 2_554 ? Cd2 O6 2.418(7) 2_554 ? Cd2 O3 2.448(4) 1_565 ? Cd2 C42 2.705(6) . ? Cd2 C8 2.744(6) 1_565 ? C1 O2 1.111(11) . ? C1 O1 1.243(11) . ? C1 C2 1.508(11) . ? C2 C3 1.282(11) . ? C2 C7 1.503(12) . ? C3 C4 1.392(11) . ? C4 C5 1.309(10) . ? C5 C6 1.461(10) . ? C5 C22 1.494(8) . ? C6 C7 1.404(11) . ? C8 O3 1.259(7) . ? C8 O4 1.264(7) . ? C8 C9 1.480(8) . ? C8 Cd2 2.744(6) 1_545 ? C9 C10 1.371(8) . ? C9 C14 1.403(8) . ? C10 C11 1.358(7) . ? C10 H10 0.9300 . ? C11 C12 1.399(7) . ? C11 H11 0.9300 . ? C12 C13 1.401(7) . ? C12 C24 1.465(7) . ? C13 C14 1.366(8) . ? C13 H13A 0.9300 . ? C14 H14 0.9300 . ? C15 O6 1.149(10) . ? C15 O5 1.217(10) . ? C15 C16 1.487(10) . ? C16 C21 1.322(10) . ? C16 C17 1.435(11) . ? C17 C18 1.354(9) . ? C17 H17 0.9300 . ? C18 C19 1.403(9) . ? C18 H18 0.9300 . ? C19 C20 1.330(9) . ? C19 C26 1.508(8) . ? C20 C21 1.362(10) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.382(8) . ? C22 C23 1.418(7) . ? C23 C24 1.395(8) . ? C24 C25 1.374(8) . ? C25 C26 1.425(7) . ? C26 C27 1.395(8) . ? C27 O14 1.399(7) . ? C28 O7 1.230(7) . ? C28 O8 1.262(8) . ? C28 C29 1.495(8) . ? C29 C30 1.366(8) . ? C29 C34 1.399(7) . ? C30 C31 1.390(7) . ? C30 H30 0.9300 . ? C31 C32 1.400(7) . ? C31 H31 0.9300 . ? C32 C33 1.406(7) . ? C32 C49 1.485(7) . ? C33 C34 1.370(7) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 O9 1.251(7) . ? C35 O10 1.267(7) . ? C35 C36 1.494(8) . ? C35 Cd1 2.700(6) 2_656 ? C36 C41 1.348(8) . ? C36 C37 1.391(9) . ? C37 C38 1.399(9) . ? C37 H37 0.9300 . ? C38 C39 1.359(9) . ? C38 H38 0.9300 . ? C39 C40 1.379(9) . ? C39 C53 1.485(7) . ? C40 C41 1.401(9) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 O12 1.254(7) . ? C42 O11 1.270(7) . ? C42 C43 1.481(8) . ? C43 C44 1.374(8) . ? C43 C48 1.382(9) . ? C44 C45 1.389(9) . ? C44 H44 0.9300 . ? C45 C46 1.358(8) . ? C45 H45 0.9300 . ? C46 C47 1.384(9) . ? C46 C51 1.500(7) . ? C47 C48 1.391(9) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.400(7) . ? C49 C50 1.404(7) . ? C50 C51 1.404(7) . ? C51 C52 1.397(7) . ? C52 O13 1.368(8) . ? C52 C53 1.384(7) . ? C53 C54 1.410(7) . ? C55 N2 1.301(8) . ? C55 C56 1.391(9) . ? C55 H55 0.9300 . ? C56 C57 1.368(8) . ? C56 H56 0.9300 . ? C57 C58 1.356(8) . ? C57 C62 1.489(8) . ? C58 C59 1.379(9) . ? C58 H58 0.9300 . ? C59 N2 1.319(8) . ? C59 H59 0.9300 . ? C60 N1 1.293(8) . ? C60 C61 1.413(9) . ? C60 H60 0.9300 . ? C61 C62 1.333(8) . ? C61 H61 0.9300 . ? C62 C63 1.364(9) . ? C63 C64 1.372(11) . ? C63 H63 0.9300 . ? C64 N1 1.299(9) . ? C64 H64 0.9300 . ? O3 Cd2 2.448(4) 1_545 ? O4 Cd2 2.337(4) 1_545 ? O5 Cd2 2.410(6) 2_544 ? O6 Cd2 2.418(7) 2_544 ? O9 Cd1 2.355(4) 2_656 ? O10 Cd1 2.360(4) 2_656 ? N2 Cd1 2.339(5) 3_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Cd1 N2 101.61(18) . 3_675 ? O8 Cd1 O9 105.04(19) . 2_646 ? N2 Cd1 O9 143.62(16) 3_675 2_646 ? O8 Cd1 O10 140.99(18) . 2_646 ? N2 Cd1 O10 88.23(16) 3_675 2_646 ? O9 Cd1 O10 55.58(15) 2_646 2_646 ? O8 Cd1 O1 130.9(3) . . ? N2 Cd1 O1 85.9(2) 3_675 . ? O9 Cd1 O1 94.8(2) 2_646 . ? O10 Cd1 O1 87.0(2) 2_646 . ? O8 Cd1 O2 81.8(2) . . ? N2 Cd1 O2 101.0(3) 3_675 . ? O9 Cd1 O2 106.8(3) 2_646 . ? O10 Cd1 O2 133.7(2) 2_646 . ? O1 Cd1 O2 49.3(3) . . ? O8 Cd1 O7 53.91(15) . . ? N2 Cd1 O7 85.52(17) 3_675 . ? O9 Cd1 O7 90.51(16) 2_646 . ? O10 Cd1 O7 90.06(15) 2_646 . ? O1 Cd1 O7 171.0(2) . . ? O2 Cd1 O7 135.5(2) . . ? O8 Cd1 C35 125.69(19) . 2_646 ? N2 Cd1 C35 116.13(18) 3_675 2_646 ? O9 Cd1 C35 27.60(15) 2_646 2_646 ? O10 Cd1 C35 27.98(16) 2_646 2_646 ? O1 Cd1 C35 91.1(2) . 2_646 ? O2 Cd1 C35 123.6(3) . 2_646 ? O7 Cd1 C35 90.27(16) . 2_646 ? O8 Cd1 C28 27.31(17) . . ? N2 Cd1 C28 92.36(17) 3_675 . ? O9 Cd1 C28 100.10(17) 2_646 . ? O10 Cd1 C28 116.06(18) 2_646 . ? O1 Cd1 C28 156.9(3) . . ? O2 Cd1 C28 108.9(2) . . ? O7 Cd1 C28 26.69(15) . . ? C35 Cd1 C28 110.22(18) 2_646 . ? O4 Cd2 O11 107.59(19) 1_565 . ? O4 Cd2 N1 96.10(19) 1_565 . ? O11 Cd2 N1 145.25(18) . . ? O4 Cd2 O12 142.23(17) 1_565 . ? O11 Cd2 O12 55.59(15) . . ? N1 Cd2 O12 90.17(17) . . ? O4 Cd2 O5 130.0(2) 1_565 2_554 ? O11 Cd2 O5 97.1(2) . 2_554 ? N1 Cd2 O5 86.1(2) . 2_554 ? O12 Cd2 O5 87.5(2) . 2_554 ? O4 Cd2 O6 81.6(2) 1_565 2_554 ? O11 Cd2 O6 105.4(3) . 2_554 ? N1 Cd2 O6 102.9(3) . 2_554 ? O12 Cd2 O6 133.2(2) . 2_554 ? O5 Cd2 O6 49.7(2) 2_554 2_554 ? O4 Cd2 O3 54.51(16) 1_565 1_565 ? O11 Cd2 O3 89.13(16) . 1_565 ? N1 Cd2 O3 84.26(17) . 1_565 ? O12 Cd2 O3 89.40(15) . 1_565 ? O5 Cd2 O3 169.8(2) 2_554 1_565 ? O6 Cd2 O3 136.1(2) 2_554 1_565 ? O4 Cd2 C42 127.91(19) 1_565 . ? O11 Cd2 C42 27.98(16) . . ? N1 Cd2 C42 117.54(19) . . ? O12 Cd2 C42 27.61(16) . . ? O5 Cd2 C42 93.0(2) 2_554 . ? O6 Cd2 C42 123.0(2) 2_554 . ? O3 Cd2 C42 88.70(16) 1_565 . ? O4 Cd2 C8 27.35(17) 1_565 1_565 ? O11 Cd2 C8 101.22(17) . 1_565 ? N1 Cd2 C8 88.18(17) . 1_565 ? O12 Cd2 C8 116.46(18) . 1_565 ? O5 Cd2 C8 155.4(2) 2_554 1_565 ? O6 Cd2 C8 108.8(2) 2_554 1_565 ? O3 Cd2 C8 27.31(16) 1_565 1_565 ? C42 Cd2 C8 110.82(18) . 1_565 ? O2 C1 O1 116.1(10) . . ? O2 C1 C2 122.9(11) . . ? O1 C1 C2 120.7(10) . . ? C3 C2 C7 119.1(7) . . ? C3 C2 C1 125.6(9) . . ? C7 C2 C1 115.3(9) . . ? C2 C3 C4 124.3(9) . . ? C5 C4 C3 121.2(8) . . ? C4 C5 C6 119.4(7) . . ? C4 C5 C22 124.4(6) . . ? C6 C5 C22 116.1(6) . . ? C7 C6 C5 119.8(8) . . ? C6 C7 C2 116.1(9) . . ? O3 C8 O4 120.8(5) . . ? O3 C8 C9 118.9(6) . . ? O4 C8 C9 120.2(6) . . ? O3 C8 Cd2 63.2(3) . 1_545 ? O4 C8 Cd2 58.1(3) . 1_545 ? C9 C8 Cd2 169.8(4) . 1_545 ? C10 C9 C14 117.3(5) . . ? C10 C9 C8 122.3(5) . . ? C14 C9 C8 120.4(5) . . ? C11 C10 C9 122.0(5) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C10 C11 C12 121.8(5) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C13 116.3(5) . . ? C11 C12 C24 122.0(5) . . ? C13 C12 C24 121.7(5) . . ? C14 C13 C12 121.5(5) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C9 121.1(5) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? O6 C15 O5 118.3(8) . . ? O6 C15 C16 120.8(9) . . ? O5 C15 C16 120.5(9) . . ? C21 C16 C17 115.1(7) . . ? C21 C16 C15 125.3(8) . . ? C17 C16 C15 119.4(7) . . ? C18 C17 C16 121.1(7) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.5(7) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 117.1(6) . . ? C20 C19 C26 124.7(6) . . ? C18 C19 C26 118.2(6) . . ? C19 C20 C21 122.2(8) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 123.9(8) . . ? C16 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? C27 C22 C23 120.1(5) . . ? C27 C22 C5 121.1(5) . . ? C23 C22 C5 118.7(5) . . ? C24 C23 C22 120.8(5) . . ? C25 C24 C23 118.3(5) . . ? C25 C24 C12 121.4(5) . . ? C23 C24 C12 120.3(5) . . ? C24 C25 C26 122.1(5) . . ? C27 C26 C25 118.6(5) . . ? C27 C26 C19 121.4(5) . . ? C25 C26 C19 120.0(5) . . ? C22 C27 C26 120.1(5) . . ? C22 C27 O14 120.6(5) . . ? C26 C27 O14 119.4(5) . . ? O7 C28 O8 121.3(5) . . ? O7 C28 C29 119.8(6) . . ? O8 C28 C29 118.8(5) . . ? O7 C28 Cd1 64.8(3) . . ? O8 C28 Cd1 56.8(3) . . ? C29 C28 Cd1 171.2(4) . . ? C30 C29 C34 118.1(5) . . ? C30 C29 C28 120.7(5) . . ? C34 C29 C28 121.1(5) . . ? C29 C30 C31 121.3(5) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C30 C31 C32 121.1(5) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C31 C32 C33 116.8(5) . . ? C31 C32 C49 121.4(5) . . ? C33 C32 C49 121.8(5) . . ? C34 C33 C32 121.2(5) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C29 121.2(5) . . ? C33 C34 H34 119.4 . . ? C29 C34 H34 119.4 . . ? O9 C35 O10 121.6(6) . . ? O9 C35 C36 119.3(5) . . ? O10 C35 C36 119.0(5) . . ? O9 C35 Cd1 60.7(3) . 2_656 ? O10 C35 Cd1 60.9(3) . 2_656 ? C36 C35 Cd1 178.9(4) . 2_656 ? C41 C36 C37 118.1(6) . . ? C41 C36 C35 120.8(5) . . ? C37 C36 C35 121.0(5) . . ? C36 C37 C38 121.5(6) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C39 C38 C37 120.5(6) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 117.3(6) . . ? C38 C39 C53 121.2(5) . . ? C40 C39 C53 121.4(5) . . ? C39 C40 C41 122.5(6) . . ? C39 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C36 C41 C40 119.9(6) . . ? C36 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? O12 C42 O11 121.6(6) . . ? O12 C42 C43 119.6(6) . . ? O11 C42 C43 118.8(5) . . ? O12 C42 Cd2 61.5(3) . . ? O11 C42 Cd2 60.2(3) . . ? C43 C42 Cd2 178.7(5) . . ? C44 C43 C48 116.8(6) . . ? C44 C43 C42 121.8(6) . . ? C48 C43 C42 121.4(5) . . ? C43 C44 C45 121.4(6) . . ? C43 C44 H44 119.3 . . ? C45 C44 H44 119.3 . . ? C46 C45 C44 122.0(6) . . ? C46 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? C45 C46 C47 117.3(6) . . ? C45 C46 C51 121.1(5) . . ? C47 C46 C51 121.5(5) . . ? C46 C47 C48 120.9(6) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C43 C48 C47 121.6(6) . . ? C43 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? C54 C49 C50 119.4(5) . . ? C54 C49 C32 120.4(5) . . ? C50 C49 C32 120.2(5) . . ? C51 C50 C49 120.0(5) . . ? C52 C51 C50 119.6(5) . . ? C52 C51 C46 120.3(5) . . ? C50 C51 C46 120.0(5) . . ? O13 C52 C53 120.9(5) . . ? O13 C52 C51 117.9(5) . . ? C53 C52 C51 121.2(5) . . ? C52 C53 C54 119.1(5) . . ? C52 C53 C39 121.0(5) . . ? C54 C53 C39 119.9(5) . . ? C49 C54 C53 120.7(5) . . ? N2 C55 C56 123.6(6) . . ? N2 C55 H55 118.2 . . ? C56 C55 H55 118.2 . . ? C57 C56 C55 120.1(6) . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C58 C57 C56 115.8(6) . . ? C58 C57 C62 123.1(6) . . ? C56 C57 C62 121.0(6) . . ? C57 C58 C59 120.7(6) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? N2 C59 C58 123.5(7) . . ? N2 C59 H59 118.3 . . ? C58 C59 H59 118.3 . . ? N1 C60 C61 123.6(6) . . ? N1 C60 H60 118.2 . . ? C61 C60 H60 118.2 . . ? C62 C61 C60 120.4(6) . . ? C62 C61 H61 119.8 . . ? C60 C61 H61 119.8 . . ? C61 C62 C63 115.4(6) . . ? C61 C62 C57 121.8(6) . . ? C63 C62 C57 122.7(6) . . ? C62 C63 C64 120.0(7) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? N1 C64 C63 125.1(7) . . ? N1 C64 H64 117.5 . . ? C63 C64 H64 117.5 . . ? C1 O1 Cd1 95.9(7) . . ? C1 O2 Cd1 98.0(8) . . ? C8 O3 Cd2 89.5(4) . 1_545 ? C8 O4 Cd2 94.5(4) . 1_545 ? C15 O5 Cd2 94.9(6) . 2_544 ? C15 O6 Cd2 96.4(6) . 2_544 ? C28 O7 Cd1 88.5(4) . . ? C28 O8 Cd1 95.8(4) . . ? C35 O9 Cd1 91.7(4) . 2_656 ? C35 O10 Cd1 91.1(4) . 2_656 ? C42 O11 Cd2 91.8(4) . . ? C42 O12 Cd2 90.9(4) . . ? C60 N1 C64 115.1(6) . . ? C60 N1 Cd2 120.0(4) . . ? C64 N1 Cd2 124.9(5) . . ? C55 N2 C59 116.3(6) . . ? C55 N2 Cd1 118.1(4) . 3_675 ? C59 N2 Cd1 125.6(4) . 3_675 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.834 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 966926' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H32 Cd3 N2 O14' _chemical_formula_sum 'C54 H32 Cd3 N2 O14' _chemical_formula_weight 1270.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3028(5) _cell_length_b 14.9043(7) _cell_length_c 15.2092(7) _cell_angle_alpha 70.594(4) _cell_angle_beta 83.472(4) _cell_angle_gamma 84.978(4) _cell_volume 1973.29(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7287 _cell_measurement_theta_min 3.1455 _cell_measurement_theta_max 74.1977 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 626.0 _exptl_absorpt_coefficient_mu 6.780 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.258 _exptl_absorpt_correction_T_max 0.322 _exptl_absorpt_process_details ? _exptl_special_details ; # SQUEEZE RESULTS (APPEND TO CIF) 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 1 -0.007 0.000 -0.018 981.4 266.4 _platon_squeeze_details ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 8068 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 74.36 _reflns_number_total 8068 _reflns_number_gt 6790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0893P)^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 7798 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 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 0.5000 0.5000 0.0000 0.01476(10) Uani 1 2 d S . . Cd2 Cd 0.65692(3) -0.278677(16) 1.034721(14) 0.01834(10) Uani 1 1 d . . . O3 O 0.4692(3) -0.18015(19) 0.9624(2) 0.0316(6) Uani 1 1 d . . . O4 O 0.6742(3) -0.11386(18) 0.95700(19) 0.0285(6) Uani 1 1 d . . . O5 O -0.3258(3) 0.61568(19) 0.94734(17) 0.0219(5) Uani 1 1 d . . . O6 O -0.1322(3) 0.6886(2) 0.9464(2) 0.0278(6) Uani 1 1 d . . . O1 O 0.5235(3) 0.49959(17) 0.14368(15) 0.0181(5) Uani 1 1 d . . . O2 O 0.5094(3) 0.64498(19) 0.15702(17) 0.0273(6) Uani 1 1 d . . . O7 O 0.6730(4) 0.3812(2) 0.0316(2) 0.0394(8) Uani 1 1 d . . . N1 N 0.1625(4) 0.2756(2) 0.8704(2) 0.0230(6) Uani 1 1 d . . . H1A H 0.1972 0.2205 0.9024 0.028 Uiso 1 1 calc R . . H1B H 0.1049 0.3085 0.8978 0.028 Uiso 1 1 calc R . . C12 C 0.3559(4) 0.1643(3) 0.7811(2) 0.0188(7) Uani 1 1 d . . . C9 C 0.4787(4) -0.0123(2) 0.8833(2) 0.0180(7) Uani 1 1 d . . . C2 C 0.4451(4) 0.5144(2) 0.2911(2) 0.0152(6) Uani 1 1 d . . . C15 C -0.1909(4) 0.6278(2) 0.9242(2) 0.0178(7) Uani 1 1 d . . . C8 C 0.5467(4) -0.1068(2) 0.9367(2) 0.0171(7) Uani 1 1 d . . . C19 C 0.0595(4) 0.4644(2) 0.7708(2) 0.0161(6) Uani 1 1 d . . . C27 C 0.1927(4) 0.4420(2) 0.6263(2) 0.0166(6) Uani 1 1 d . . . H27A H 0.1559 0.5020 0.5922 0.020 Uiso 1 1 calc R . . C6 C 0.3426(4) 0.5328(2) 0.4374(2) 0.0166(6) Uani 1 1 d . . . H6A H 0.3089 0.5724 0.4722 0.020 Uiso 1 1 calc R . . C22 C 0.2888(4) 0.3915(2) 0.5801(2) 0.0173(7) Uani 1 1 d . . . C14 C 0.5612(4) 0.0664(3) 0.8519(3) 0.0256(8) Uani 1 1 d . . . H14A H 0.6577 0.0606 0.8647 0.031 Uiso 1 1 calc R . . C7 C 0.3938(4) 0.5723(2) 0.3444(2) 0.0168(6) Uani 1 1 d . . . H7A H 0.3940 0.6382 0.3173 0.020 Uiso 1 1 calc R . . C16 C -0.1052(4) 0.5724(3) 0.8696(2) 0.0188(7) Uani 1 1 d . . . C24 C 0.2940(4) 0.2593(3) 0.7273(2) 0.0193(7) Uani 1 1 d . . . C5 C 0.3410(4) 0.4338(2) 0.4797(2) 0.0172(7) Uani 1 1 d . . . C13 C 0.5004(5) 0.1548(3) 0.8011(3) 0.0277(8) Uani 1 1 d . . . H13A H 0.5564 0.2078 0.7804 0.033 Uiso 1 1 calc R . . C1 C 0.4963(4) 0.5561(2) 0.1894(2) 0.0151(6) Uani 1 1 d . . . C23 C 0.3384(4) 0.3002(3) 0.6321(2) 0.0195(7) Uani 1 1 d . . . H23A H 0.4029 0.2656 0.6027 0.023 Uiso 1 1 calc R . . C25 C 0.2007(4) 0.3126(2) 0.7716(2) 0.0180(7) Uani 1 1 d . . . C3 C 0.4470(4) 0.4166(3) 0.3327(2) 0.0203(7) Uani 1 1 d . . . H3A H 0.4828 0.3772 0.2980 0.024 Uiso 1 1 calc R . . C10 C 0.3336(4) -0.0030(3) 0.8644(3) 0.0267(8) Uani 1 1 d . . . H10A H 0.2771 -0.0558 0.8858 0.032 Uiso 1 1 calc R . . C4 C 0.3957(4) 0.3768(3) 0.4257(2) 0.0238(8) Uani 1 1 d . . . H4A H 0.3979 0.3109 0.4527 0.029 Uiso 1 1 calc R . . C26 C 0.1504(4) 0.4056(2) 0.7213(2) 0.0162(6) Uani 1 1 d . . . C17 C 0.0423(4) 0.5581(3) 0.8760(3) 0.0273(8) Uani 1 1 d . . . H17A H 0.0875 0.5851 0.9119 0.033 Uiso 1 1 calc R . . C11 C 0.2742(4) 0.0845(3) 0.8141(3) 0.0267(8) Uani 1 1 d . . . H11A H 0.1774 0.0901 0.8021 0.032 Uiso 1 1 calc R . . C21 C -0.1701(5) 0.5384(4) 0.8116(3) 0.0373(11) Uani 1 1 d . . . H21A H -0.2691 0.5501 0.8060 0.045 Uiso 1 1 calc R . . C20 C -0.0880(4) 0.4861(4) 0.7611(3) 0.0361(10) Uani 1 1 d . . . H20A H -0.1324 0.4653 0.7201 0.043 Uiso 1 1 calc R . . C18 C 0.1227(4) 0.5028(3) 0.8281(3) 0.0302(9) Uani 1 1 d . . . H18A H 0.2215 0.4913 0.8344 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01928(18) 0.01878(18) 0.00987(16) -0.00923(13) -0.00066(12) -0.00297(13) Cd2 0.03009(16) 0.01404(14) 0.00924(14) -0.00294(10) 0.00394(10) -0.00315(10) O3 0.0358(16) 0.0132(13) 0.0441(17) -0.0068(12) -0.0025(13) -0.0032(11) O4 0.0383(16) 0.0119(12) 0.0308(14) 0.0024(10) -0.0096(12) -0.0065(11) O5 0.0229(13) 0.0269(14) 0.0211(12) -0.0159(10) 0.0093(10) -0.0111(10) O6 0.0263(14) 0.0291(15) 0.0363(15) -0.0230(12) 0.0062(11) -0.0084(11) O1 0.0271(13) 0.0224(13) 0.0073(10) -0.0082(9) 0.0006(9) -0.0030(10) O2 0.0473(17) 0.0201(14) 0.0121(11) -0.0041(10) 0.0109(11) -0.0115(12) O7 0.0469(19) 0.0450(19) 0.0330(16) -0.0247(14) -0.0110(13) 0.0194(15) N1 0.0336(17) 0.0236(16) 0.0104(13) -0.0043(11) 0.0035(11) -0.0051(13) C12 0.0299(19) 0.0175(17) 0.0093(14) -0.0056(13) 0.0020(13) -0.0029(14) C9 0.0258(18) 0.0158(17) 0.0117(14) -0.0039(13) 0.0011(12) -0.0027(13) C2 0.0211(16) 0.0200(17) 0.0050(13) -0.0041(12) -0.0006(11) -0.0046(13) C15 0.0273(18) 0.0172(16) 0.0096(14) -0.0044(12) -0.0025(12) -0.0026(13) C8 0.0287(18) 0.0084(15) 0.0112(14) 0.0000(12) 0.0035(12) -0.0049(13) C19 0.0224(17) 0.0167(16) 0.0077(13) -0.0019(12) 0.0005(12) -0.0036(13) C27 0.0234(17) 0.0154(16) 0.0117(14) -0.0047(12) -0.0012(12) -0.0041(13) C6 0.0272(17) 0.0137(16) 0.0121(14) -0.0077(12) -0.0017(12) -0.0043(13) C22 0.0285(17) 0.0163(16) 0.0076(14) -0.0050(12) -0.0005(12) -0.0011(13) C14 0.030(2) 0.0160(18) 0.0280(18) -0.0011(15) -0.0064(15) -0.0072(15) C7 0.0241(17) 0.0148(16) 0.0117(14) -0.0034(12) 0.0005(12) -0.0085(13) C16 0.0207(17) 0.0236(18) 0.0122(14) -0.0047(13) 0.0019(12) -0.0108(14) C24 0.0259(18) 0.0192(17) 0.0127(15) -0.0042(13) -0.0009(13) -0.0067(14) C5 0.0268(18) 0.0169(17) 0.0089(14) -0.0058(13) -0.0011(12) -0.0009(13) C13 0.034(2) 0.0200(19) 0.0263(19) -0.0025(15) -0.0029(16) -0.0066(16) C1 0.0204(16) 0.0159(16) 0.0077(14) -0.0013(12) -0.0003(11) -0.0047(12) C23 0.0287(18) 0.0181(17) 0.0121(15) -0.0051(13) -0.0007(13) -0.0042(14) C25 0.0262(18) 0.0199(17) 0.0078(14) -0.0038(12) 0.0013(12) -0.0070(14) C3 0.035(2) 0.0164(17) 0.0104(15) -0.0065(13) 0.0005(13) 0.0000(14) C10 0.029(2) 0.0165(18) 0.0306(19) -0.0029(15) 0.0017(15) -0.0075(15) C4 0.042(2) 0.0160(17) 0.0137(16) -0.0064(13) 0.0019(14) 0.0003(15) C26 0.0207(16) 0.0165(16) 0.0130(14) -0.0064(12) -0.0004(12) -0.0037(13) C17 0.0247(19) 0.034(2) 0.033(2) -0.0227(17) -0.0032(15) -0.0051(16) C11 0.027(2) 0.025(2) 0.0274(19) -0.0057(16) -0.0054(15) -0.0042(16) C21 0.0219(19) 0.069(3) 0.040(2) -0.044(2) 0.0021(17) -0.007(2) C20 0.021(2) 0.065(3) 0.040(2) -0.040(2) 0.0023(16) -0.0090(19) C18 0.0223(19) 0.039(2) 0.041(2) -0.0275(19) -0.0068(16) -0.0011(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 O1 2.219(2) . ? Cd1 O1 2.219(2) 2_665 ? Cd1 O7 2.251(3) 2_665 ? Cd1 O7 2.251(3) . ? Cd1 O5 2.349(2) 1_654 ? Cd1 O5 2.349(2) 2_566 ? Cd2 O2 2.219(3) 1_546 ? Cd2 O3 2.309(3) . ? Cd2 N1 2.348(3) 2_657 ? Cd2 O6 2.358(3) 1_645 ? Cd2 O5 2.360(2) 1_645 ? Cd2 O4 2.357(2) . ? Cd2 C8 2.681(3) . ? Cd2 C15 2.728(3) 1_645 ? O3 C8 1.288(4) . ? O4 C8 1.246(5) . ? O5 C15 1.276(4) . ? O5 Cd1 2.349(2) 1_456 ? O5 Cd2 2.360(2) 1_465 ? O6 C15 1.251(4) . ? O6 Cd2 2.358(3) 1_465 ? O1 C1 1.253(4) . ? O2 C1 1.263(4) . ? O2 Cd2 2.219(2) 1_564 ? N1 C25 1.433(4) . ? N1 Cd2 2.348(3) 2_657 ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? C12 C11 1.386(5) . ? C12 C13 1.396(5) . ? C12 C24 1.484(5) . ? C9 C14 1.376(5) . ? C9 C10 1.398(5) . ? C9 C8 1.498(5) . ? C2 C3 1.383(5) . ? C2 C7 1.391(5) . ? C2 C1 1.500(4) . ? C15 C16 1.482(5) . ? C15 Cd2 2.728(3) 1_465 ? C19 C20 1.395(5) . ? C19 C18 1.392(5) . ? C19 C26 1.488(5) . ? C27 C26 1.387(4) . ? C27 C22 1.397(5) . ? C27 H27A 0.9300 . ? C6 C7 1.385(4) . ? C6 C5 1.401(5) . ? C6 H6A 0.9300 . ? C22 C23 1.395(5) . ? C22 C5 1.486(4) . ? C14 C13 1.395(5) . ? C14 H14A 0.9300 . ? C7 H7A 0.9300 . ? C16 C21 1.367(5) . ? C16 C17 1.380(5) . ? C24 C25 1.393(5) . ? C24 C23 1.400(5) . ? C5 C4 1.395(5) . ? C13 H13A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.411(5) . ? C3 C4 1.386(5) . ? C3 H3A 0.9300 . ? C10 C11 1.377(5) . ? C10 H10A 0.9300 . ? C4 H4A 0.9300 . ? C17 C18 1.391(6) . ? C17 H17A 0.9300 . ? C11 H11A 0.9300 . ? C21 C20 1.393(6) . ? C21 H21A 0.9300 . ? C20 H20A 0.9300 . ? C18 H18A 0.9300 . ? 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 O1 Cd1 O1 180.0 . 2_665 ? O1 Cd1 O7 95.76(10) . 2_665 ? O1 Cd1 O7 84.24(10) 2_665 2_665 ? O1 Cd1 O7 84.24(10) . . ? O1 Cd1 O7 95.76(10) 2_665 . ? O7 Cd1 O7 180.0 2_665 . ? O1 Cd1 O5 87.12(8) . 1_654 ? O1 Cd1 O5 92.88(8) 2_665 1_654 ? O7 Cd1 O5 88.37(12) 2_665 1_654 ? O7 Cd1 O5 91.63(12) . 1_654 ? O1 Cd1 O5 92.88(8) . 2_566 ? O1 Cd1 O5 87.12(8) 2_665 2_566 ? O7 Cd1 O5 91.63(12) 2_665 2_566 ? O7 Cd1 O5 88.37(12) . 2_566 ? O5 Cd1 O5 180.0 1_654 2_566 ? O2 Cd2 O3 92.21(11) 1_546 . ? O2 Cd2 N1 92.57(11) 1_546 2_657 ? O3 Cd2 N1 138.38(11) . 2_657 ? O2 Cd2 O6 138.86(10) 1_546 1_645 ? O3 Cd2 O6 120.89(11) . 1_645 ? N1 Cd2 O6 78.73(10) 2_657 1_645 ? O2 Cd2 O5 100.54(9) 1_546 1_645 ? O3 Cd2 O5 97.38(10) . 1_645 ? N1 Cd2 O5 122.20(10) 2_657 1_645 ? O6 Cd2 O5 55.03(8) 1_645 1_645 ? O2 Cd2 O4 129.72(10) 1_546 . ? O3 Cd2 O4 56.38(10) . . ? N1 Cd2 O4 90.01(10) 2_657 . ? O6 Cd2 O4 90.77(10) 1_645 . ? O5 Cd2 O4 119.88(9) 1_645 . ? O2 Cd2 C8 112.99(11) 1_546 . ? O3 Cd2 C8 28.69(10) . . ? N1 Cd2 C8 114.69(11) 2_657 . ? O6 Cd2 C8 107.06(10) 1_645 . ? O5 Cd2 C8 110.97(10) 1_645 . ? O4 Cd2 C8 27.69(10) . . ? O2 Cd2 C15 121.03(10) 1_546 1_645 ? O3 Cd2 C15 112.69(10) . 1_645 ? N1 Cd2 C15 99.83(11) 2_657 1_645 ? O6 Cd2 C15 27.25(10) 1_645 1_645 ? O5 Cd2 C15 27.86(10) 1_645 1_645 ? O4 Cd2 C15 107.85(10) . 1_645 ? C8 Cd2 C15 113.01(10) . 1_645 ? C8 O3 Cd2 91.9(2) . . ? C8 O4 Cd2 90.8(2) . . ? C15 O5 Cd1 143.6(2) . 1_456 ? C15 O5 Cd2 92.35(19) . 1_465 ? Cd1 O5 Cd2 113.28(9) 1_456 1_465 ? C15 O6 Cd2 93.1(2) . 1_465 ? C1 O1 Cd1 137.2(2) . . ? C1 O2 Cd2 126.2(2) . 1_564 ? C25 N1 Cd2 115.6(2) . 2_657 ? C25 N1 H1A 120.0 . . ? Cd2 N1 H1A 65.2 2_657 . ? C25 N1 H1B 120.0 . . ? Cd2 N1 H1B 89.3 2_657 . ? H1A N1 H1B 120.0 . . ? C11 C12 C13 118.6(3) . . ? C11 C12 C24 122.1(3) . . ? C13 C12 C24 119.3(3) . . ? C14 C9 C10 119.6(3) . . ? C14 C9 C8 119.3(3) . . ? C10 C9 C8 121.1(3) . . ? C3 C2 C7 119.1(3) . . ? C3 C2 C1 119.6(3) . . ? C7 C2 C1 121.3(3) . . ? O6 C15 O5 119.2(3) . . ? O6 C15 C16 120.2(3) . . ? O5 C15 C16 120.6(3) . . ? O6 C15 Cd2 59.66(18) . 1_465 ? O5 C15 Cd2 59.79(17) . 1_465 ? C16 C15 Cd2 176.4(2) . 1_465 ? O4 C8 O3 120.9(3) . . ? O4 C8 C9 120.8(3) . . ? O3 C8 C9 118.3(3) . . ? O4 C8 Cd2 61.51(17) . . ? O3 C8 Cd2 59.38(18) . . ? C9 C8 Cd2 177.5(3) . . ? C20 C19 C18 117.0(3) . . ? C20 C19 C26 123.3(3) . . ? C18 C19 C26 119.7(3) . . ? C26 C27 C22 122.2(3) . . ? C26 C27 H27A 118.9 . . ? C22 C27 H27A 118.9 . . ? C7 C6 C5 120.8(3) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C23 C22 C27 117.7(3) . . ? C23 C22 C5 120.6(3) . . ? C27 C22 C5 121.7(3) . . ? C9 C14 C13 120.1(4) . . ? C9 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C6 C7 C2 120.6(3) . . ? C6 C7 H7A 119.7 . . ? C2 C7 H7A 119.7 . . ? C21 C16 C17 120.4(4) . . ? C21 C16 C15 120.8(3) . . ? C17 C16 C15 118.8(3) . . ? C25 C24 C23 118.8(3) . . ? C25 C24 C12 120.9(3) . . ? C23 C24 C12 120.1(3) . . ? C6 C5 C4 117.8(3) . . ? C6 C5 C22 120.7(3) . . ? C4 C5 C22 121.4(3) . . ? C14 C13 C12 120.5(4) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? O1 C1 O2 125.3(3) . . ? O1 C1 C2 117.2(3) . . ? O2 C1 C2 117.5(3) . . ? C22 C23 C24 121.9(3) . . ? C22 C23 H23A 119.0 . . ? C24 C23 H23A 119.0 . . ? C24 C25 C26 120.6(3) . . ? C24 C25 N1 120.0(3) . . ? C26 C25 N1 119.2(3) . . ? C2 C3 C4 120.4(3) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C11 C10 C9 119.9(3) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C3 C4 C5 121.3(3) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C27 C26 C25 118.7(3) . . ? C27 C26 C19 121.2(3) . . ? C25 C26 C19 120.1(3) . . ? C18 C17 C16 119.2(3) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C10 C11 C12 121.2(4) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C16 C21 C20 120.0(4) . . ? C16 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C20 C19 121.3(4) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C17 C18 C19 121.9(4) . . ? C17 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 74.36 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.885 _refine_diff_density_min -2.822 _refine_diff_density_rms 0.140 #end _database_code_depnum_ccdc_archive 'CCDC 966927'