# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr Tong-Bu Lu' _publ_contact_author_email lutongbu@mail.sysu.edu.cn loop_ _publ_author_name 'Hua Xiang' 'Wen-Yang Gao' 'Di-Chang Zhong' 'Long Jiang' 'Tong-Bu Lu' data_1 _database_code_depnum_ccdc_archive 'CCDC 825082' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C54 H30 Cd3 O12), 7(C3 H7 N O)' _chemical_formula_sum 'C75 H79 Cd3 N7 O19' _chemical_formula_weight 1719.65 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.713(11) _cell_length_b 17.135(7) _cell_length_c 15.277(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.121(9) _cell_angle_gamma 90.00 _cell_volume 7718(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3494 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 24.81 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3496 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7058 _exptl_absorpt_correction_T_max 0.7574 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% . _diffrn_reflns_number 17251 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.94 _reflns_number_total 8070 _reflns_number_gt 5529 _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 '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. During the refinement, the restraint command 'dfix' 'isor' 'delu' and 'simu' were ued to restrain the carbon atoms with NPD and ADP problems in the disordered part of BTB ligand and one and a hlaf disordered DMF molecules. Such a refinement led to a relative high restraint value 138. ; _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^)+(0.0722P)^2^+195.8524P] 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 8070 _refine_ls_number_parameters 648 _refine_ls_number_restraints 138 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2191 _refine_ls_wR_factor_gt 0.1924 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8450(3) 0.6851(5) 0.5889(6) 0.0313(13) Uani 1 1 d U . . C2 C 0.8763(3) 0.6161(5) 0.5925(6) 0.0310(15) Uani 1 1 d U . . C3 C 0.9212(3) 0.6219(5) 0.6317(6) 0.0345(19) Uani 1 1 d . . . H3 H 0.9329 0.6706 0.6538 0.041 Uiso 1 1 calc R . . C4 C 0.9481(2) 0.5568(5) 0.6381(6) 0.0360(19) Uani 1 1 d . . . H4 H 0.9786 0.5612 0.6645 0.043 Uiso 1 1 calc R . . C5 C 0.9320(2) 0.4843(5) 0.6072(6) 0.0347(19) Uani 1 1 d . . . C6 C 0.8877(3) 0.4808(5) 0.5663(7) 0.043(2) Uani 1 1 d . . . H6 H 0.8759 0.4326 0.5429 0.052 Uiso 1 1 calc R . . C7 C 0.8606(3) 0.5465(5) 0.5590(6) 0.041(2) Uani 1 1 d . . . H7 H 0.8305 0.5429 0.5301 0.049 Uiso 1 1 calc R . . C8 C 1.2279(3) 0.3419(5) 0.6771(6) 0.0324(18) Uani 1 1 d . . . C9 C 1.1773(2) 0.3415(5) 0.6662(6) 0.0337(19) Uani 1 1 d . . . C10 C 1.1541(3) 0.4046(5) 0.6964(6) 0.037(2) Uani 1 1 d . . . H10 H 1.1706 0.4467 0.7253 0.044 Uiso 1 1 calc R . . C11 C 1.1072(3) 0.4063(5) 0.6843(6) 0.0375(12) Uani 1 1 d U . . H11 H 1.0917 0.4496 0.7053 0.045 Uiso 1 1 calc R . . C12 C 1.0828(3) 0.3462(5) 0.6423(6) 0.0378(11) Uani 1 1 d U . . C13 C 1.1058(3) 0.2838(5) 0.6087(6) 0.0380(11) Uani 1 1 d U . . H13 H 1.0893 0.2433 0.5768 0.046 Uiso 1 1 calc R . . C14 C 1.1529(3) 0.2812(5) 0.6222(6) 0.0377(12) Uani 1 1 d U . . H14 H 1.1685 0.2380 0.6012 0.045 Uiso 1 1 calc R . . C15 C 0.8700(5) -0.0206(8) 0.6625(16) 0.0318(18) Uani 0.528(10) 1 d PDU . 1 C16 C 0.8954(3) 0.0563(4) 0.6666(8) 0.0318(17) Uani 0.528(10) 1 d PGDU . 1 C17 C 0.9368(3) 0.0588(4) 0.6332(7) 0.0319(17) Uani 0.528(10) 1 d PGU . 1 H17A H 0.9496 0.0122 0.6135 0.038 Uiso 0.528(10) 1 calc PR . 1 C18 C 0.9594(3) 0.1294(6) 0.6286(7) 0.0318(18) Uani 0.528(10) 1 d PGU . 1 H18A H 0.9877 0.1311 0.6058 0.038 Uiso 0.528(10) 1 calc PR . 1 C19 C 0.9406(3) 0.1976(4) 0.6574(7) 0.0313(18) Uani 0.528(10) 1 d PGDU . 1 C20 C 0.8991(3) 0.1951(5) 0.6908(7) 0.0317(18) Uani 0.528(10) 1 d PGU . 1 H20A H 0.8863 0.2417 0.7105 0.038 Uiso 0.528(10) 1 calc PR . 1 C21 C 0.8765(3) 0.1245(6) 0.6954(7) 0.0319(17) Uani 0.528(10) 1 d PGU . 1 H21A H 0.8482 0.1228 0.7182 0.038 Uiso 0.528(10) 1 calc PR . 1 O5 O 0.8892(4) -0.0810(7) 0.6496(11) 0.048(3) Uani 0.528(10) 1 d PDU . 1 O6 O 0.8305(4) -0.0201(8) 0.6866(11) 0.042(3) Uani 0.528(10) 1 d PDU . 1 C15' C 0.8699(5) -0.0231(8) 0.6774(16) 0.031(2) Uani 0.472(10) 1 d PDU . 2 C16' C 0.8939(3) 0.0526(5) 0.6599(8) 0.030(4) Uani 0.472(10) 1 d PGDU . 2 C17' C 0.9396(3) 0.0614(5) 0.6910(8) 0.035(4) Uani 0.472(10) 1 d PGU . 2 H17B H 0.9558 0.0197 0.7213 0.042 Uiso 0.472(10) 1 calc PR . 2 C18' C 0.9615(3) 0.1313(6) 0.6778(8) 0.032(2) Uani 0.472(10) 1 d PGU . 2 H18B H 0.9927 0.1374 0.6990 0.038 Uiso 0.472(10) 1 calc PR . 2 C19' C 0.9377(3) 0.1924(5) 0.6334(8) 0.032(2) Uani 0.472(10) 1 d PGDU . 2 C20' C 0.8920(3) 0.1835(5) 0.6024(7) 0.033(2) Uani 0.472(10) 1 d PGU . 2 H20B H 0.8758 0.2252 0.5721 0.039 Uiso 0.472(10) 1 calc PR . 2 C21' C 0.8701(3) 0.1136(6) 0.6156(8) 0.033(2) Uani 0.472(10) 1 d PGU . 2 H21B H 0.8389 0.1075 0.5944 0.040 Uiso 0.472(10) 1 calc PR . 2 O5' O 0.8904(5) -0.0797(8) 0.7086(12) 0.044(4) Uani 0.472(10) 1 d PDU . 2 O6' O 0.8291(5) -0.0277(10) 0.6398(12) 0.041(4) Uani 0.472(10) 1 d PDU . 2 C22 C 0.9596(3) 0.4121(5) 0.6180(7) 0.042(2) Uani 1 1 d . . . C23 C 1.0073(3) 0.4142(5) 0.6205(6) 0.0370(19) Uani 1 1 d U . . H23 H 1.0223 0.4624 0.6132 0.044 Uiso 1 1 calc R . . C24 C 1.0325(3) 0.3453(5) 0.6337(6) 0.040(2) Uani 1 1 d U . . C25 C 1.0103(3) 0.2747(6) 0.6397(6) 0.044(2) Uani 1 1 d U . . H25 H 1.0274 0.2277 0.6456 0.053 Uiso 1 1 calc R . . C26 C 0.9625(3) 0.2713(6) 0.6372(6) 0.041(2) Uani 1 1 d DU . . C27 C 0.9388(3) 0.3411(5) 0.6282(6) 0.039(2) Uani 1 1 d U . . H27 H 0.9069 0.3400 0.6290 0.046 Uiso 1 1 calc R . . C28 C 0.7885(4) 0.9253(6) 0.4715(7) 0.051(2) Uani 1 1 d U . . H28 H 0.7586 0.9450 0.4708 0.062 Uiso 1 1 calc R . . C29 C 0.8082(6) 1.0454(10) 0.4025(11) 0.103(5) Uani 1 1 d U . . H29A H 0.8113 1.0455 0.3393 0.155 Uiso 1 1 calc R . . H29B H 0.8291 1.0839 0.4327 0.155 Uiso 1 1 calc R . . H29C H 0.7770 1.0588 0.4109 0.155 Uiso 1 1 calc R . . C30 C 0.8651(4) 0.9445(8) 0.4358(9) 0.073(3) Uani 1 1 d U . . H30A H 0.8700 0.8938 0.4651 0.109 Uiso 1 1 calc R . . H30B H 0.8858 0.9831 0.4664 0.109 Uiso 1 1 calc R . . H30C H 0.8710 0.9400 0.3743 0.109 Uiso 1 1 calc R . . C31 C 0.8711(9) 0.7425(15) 0.8104(18) 0.080(4) Uani 0.334(11) 1 d PDU A 1 H31A H 0.8797 0.7193 0.7585 0.096 Uiso 0.334(11) 1 calc PR A 1 C32 C 0.9042(13) 0.6317(16) 0.907(2) 0.088(5) Uani 0.334(11) 1 d PDU A 1 H32A H 0.9153 0.6166 0.8514 0.132 Uiso 0.334(11) 1 d PR A 1 H32B H 0.8821 0.5930 0.9219 0.132 Uiso 0.334(11) 1 d PR A 1 H32C H 0.9297 0.6340 0.9540 0.132 Uiso 0.334(11) 1 d PR A 1 C33 C 0.8663(14) 0.743(2) 0.9740(18) 0.083(5) Uani 0.334(11) 1 d PDU A 1 H33A H 0.8566 0.7971 0.9600 0.124 Uiso 0.334(11) 1 d PR A 1 H33B H 0.8933 0.7439 1.0178 0.124 Uiso 0.334(11) 1 d PR A 1 H33C H 0.8418 0.7152 0.9978 0.124 Uiso 0.334(11) 1 d PR A 1 N2 N 0.8804(8) 0.7073(13) 0.8942(16) 0.084(4) Uani 0.334(11) 1 d PDU A 1 O8 O 0.8487(9) 0.8128(15) 0.809(2) 0.075(3) Uani 0.334(11) 1 d PDU A 1 C31' C 0.8850(5) 0.7777(10) 0.8315(10) 0.079(3) Uani 0.666(11) 1 d PDU A 2 H31B H 0.9052 0.8209 0.8363 0.095 Uiso 0.666(11) 1 calc PR A 2 C32' C 0.9476(5) 0.6896(13) 0.8840(13) 0.089(4) Uani 0.666(11) 1 d PDU A 2 H32D H 0.9658 0.7307 0.8609 0.133 Uiso 0.666(11) 1 calc PR A 2 H32E H 0.9569 0.6386 0.8633 0.133 Uiso 0.666(11) 1 calc PR A 2 H32F H 0.9522 0.6907 0.9487 0.133 Uiso 0.666(11) 1 calc PR A 2 C33' C 0.8699(6) 0.6331(12) 0.8427(15) 0.097(4) Uani 0.666(11) 1 d PDU A 2 H33D H 0.8433 0.6444 0.8000 0.146 Uiso 0.666(11) 1 calc PR A 2 H33E H 0.8600 0.6198 0.8998 0.146 Uiso 0.666(11) 1 calc PR A 2 H33F H 0.8866 0.5890 0.8216 0.146 Uiso 0.666(11) 1 calc PR A 2 N2' N 0.8996(5) 0.7024(8) 0.8530(9) 0.083(3) Uani 0.666(11) 1 d PDU A 2 O8' O 0.8396(5) 0.7862(9) 0.8029(10) 0.075(3) Uani 0.666(11) 1 d PDU A 2 C34 C 0.7667(6) 0.4311(10) 0.3976(12) 0.107(2) Uani 1 1 d DU . . H34 H 0.7682 0.4827 0.3753 0.129 Uiso 1 1 calc R . . C35 C 0.7439(6) 0.3949(11) 0.2476(9) 0.110(3) Uani 1 1 d DU . . H35A H 0.7540 0.4488 0.2413 0.164 Uiso 1 1 calc R . . H35B H 0.7113 0.3912 0.2275 0.164 Uiso 1 1 calc R . . H35C H 0.7605 0.3603 0.2120 0.164 Uiso 1 1 calc R . . C36 C 0.7455(6) 0.2906(8) 0.3721(12) 0.108(3) Uani 1 1 d DU . . H36A H 0.7493 0.2889 0.4368 0.162 Uiso 1 1 calc R . . H36B H 0.7676 0.2558 0.3499 0.162 Uiso 1 1 calc R . . H36C H 0.7147 0.2735 0.3495 0.162 Uiso 1 1 calc R . . Cd1 Cd 0.820337(16) 0.84720(3) 0.67035(4) 0.02619(18) Uani 1 1 d U . . Cd2 Cd 0.7500 0.7500 0.5000 0.0267(2) Uani 1 2 d SU . . N1 N 0.8191(4) 0.9690(6) 0.4384(6) 0.064(3) Uani 1 1 d U . . N3 N 0.7527(5) 0.3712(8) 0.3424(8) 0.108(2) Uani 1 1 d DU . . O1 O 0.85904(19) 0.7474(3) 0.6226(4) 0.0375(13) Uani 1 1 d U A . O2 O 0.80504(18) 0.6719(3) 0.5519(4) 0.0329(12) Uani 1 1 d U A . O3 O 1.2495(2) 0.3955(4) 0.7162(5) 0.0486(17) Uani 1 1 d . . . O4 O 1.24859(16) 0.2852(3) 0.6428(4) 0.0342(13) Uani 1 1 d . . . O7 O 0.7974(2) 0.8598(3) 0.5035(4) 0.0399(14) Uani 1 1 d U A . O9 O 0.7774(4) 0.4179(7) 0.4769(8) 0.110(2) Uani 1 1 d U . . C37 C 1.0182(15) 0.804(3) 0.911(3) 0.116(6) Uani 0.22 1 d PDU B 1 H37A H 1.0288 0.7518 0.9200 0.139 Uiso 0.22 1 calc PR B 1 C38 C 0.9616(17) 0.913(3) 0.875(6) 0.115(6) Uani 0.22 1 d PDU B 1 H38A H 0.9359 0.9233 0.9070 0.173 Uiso 0.22 1 d PR B 1 H38B H 0.9531 0.9242 0.8118 0.173 Uiso 0.22 1 d PR B 1 H38C H 0.9874 0.9454 0.8978 0.173 Uiso 0.22 1 d PR B 1 C39 C 0.9359(17) 0.773(3) 0.866(5) 0.116(6) Uani 0.22 1 d PDU B 1 H39A H 0.9207 0.7816 0.8058 0.173 Uiso 0.22 1 d PR B 1 H39B H 0.9142 0.7813 0.9082 0.173 Uiso 0.22 1 d PR B 1 H39C H 0.9479 0.7201 0.8713 0.173 Uiso 0.22 1 d PR B 1 N4 N 0.9741(13) 0.829(2) 0.884(3) 0.116(6) Uani 0.22 1 d PDU B 1 O10 O 1.0407(13) 0.866(3) 0.922(3) 0.116(6) Uani 0.22 1 d PDU B 1 C37' C 1.0354(12) 0.847(2) 0.935(3) 0.117(6) Uani 0.28 1 d PDU C 2 H37B H 1.0557 0.8057 0.9268 0.140 Uiso 0.28 1 calc PR C 2 C38' C 0.9691(16) 0.937(3) 0.898(3) 0.117(6) Uani 0.28 1 d PDU C 2 H38D H 0.9470 0.9212 0.9375 0.175 Uiso 0.28 1 d PR C 2 H38E H 0.9532 0.9580 0.8435 0.175 Uiso 0.28 1 d PR C 2 H38F H 0.9892 0.9770 0.9275 0.175 Uiso 0.28 1 d PR C 2 N4' N 0.9990(11) 0.8715(19) 0.878(2) 0.117(6) Uani 0.28 1 d PDU C 2 C39' C 0.9859(18) 0.834(3) 0.790(2) 0.117(6) Uani 0.28 1 d PDU . 2 H39D H 0.9528 0.8364 0.7766 0.175 Uiso 0.28 1 d PR . 2 H39E H 0.9961 0.7800 0.7910 0.175 Uiso 0.28 1 d PR . 2 H39F H 0.9999 0.8632 0.7500 0.175 Uiso 0.56 2 d SPR . 2 O10' O 1.0360(12) 0.891(2) 1.001(2) 0.117(6) Uani 0.28 1 d PDU C 2 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 C1 0.025(2) 0.029(2) 0.039(2) -0.001(2) 0.0011(19) 0.0058(19) C2 0.025(3) 0.029(3) 0.038(3) -0.001(3) 0.001(2) 0.007(2) C3 0.021(4) 0.024(4) 0.058(6) -0.002(4) 0.001(4) 0.006(3) C4 0.014(3) 0.033(4) 0.060(6) 0.001(4) 0.000(3) 0.004(3) C5 0.015(3) 0.028(4) 0.062(6) 0.004(4) 0.007(3) 0.007(3) C6 0.029(4) 0.028(5) 0.069(6) -0.011(4) -0.008(4) 0.006(4) C7 0.025(4) 0.032(5) 0.061(6) -0.006(4) -0.012(4) 0.014(4) C8 0.022(4) 0.032(4) 0.044(5) 0.000(4) 0.008(3) 0.000(3) C9 0.017(4) 0.032(4) 0.055(5) 0.003(4) 0.014(3) 0.005(3) C10 0.024(4) 0.029(4) 0.060(6) 0.004(4) 0.019(4) 0.000(3) C11 0.0348(17) 0.0364(17) 0.0422(18) 0.0005(13) 0.0083(14) 0.0021(14) C12 0.0348(15) 0.0365(16) 0.0429(16) 0.0011(12) 0.0077(13) 0.0012(12) C13 0.0350(15) 0.0366(15) 0.0429(16) 0.0005(12) 0.0073(13) 0.0010(12) C14 0.0349(16) 0.0365(18) 0.0424(18) 0.0005(14) 0.0074(14) 0.0009(14) C15 0.032(2) 0.031(2) 0.032(2) -0.0004(14) 0.0038(14) -0.0005(12) C16 0.0315(19) 0.0314(19) 0.033(2) -0.0003(11) 0.0040(11) -0.0004(10) C17 0.031(2) 0.032(2) 0.033(2) -0.0005(13) 0.0041(12) 0.0000(11) C18 0.031(2) 0.031(2) 0.033(2) -0.0006(13) 0.0042(12) 0.0001(11) C19 0.030(2) 0.031(2) 0.032(2) -0.0003(12) 0.0041(12) 0.0002(12) C20 0.031(2) 0.031(2) 0.033(2) -0.0002(13) 0.0045(12) 0.0002(12) C21 0.031(2) 0.0315(19) 0.033(2) 0.0001(12) 0.0044(12) -0.0002(11) O5 0.043(6) 0.037(6) 0.066(8) -0.003(6) 0.012(6) -0.002(5) O6 0.030(6) 0.037(6) 0.063(8) 0.002(6) 0.015(6) -0.006(5) C15' 0.031(3) 0.029(3) 0.031(3) -0.001(3) 0.004(3) -0.002(3) C16' 0.026(7) 0.020(7) 0.042(8) -0.002(6) 0.002(6) -0.003(6) C17' 0.029(7) 0.025(7) 0.048(8) 0.010(6) -0.008(6) 0.007(6) C18' 0.031(3) 0.032(3) 0.032(3) 0.0004(15) 0.0038(15) -0.0002(14) C19' 0.031(3) 0.032(3) 0.033(3) 0.0004(13) 0.0041(13) 0.0004(13) C20' 0.032(3) 0.033(3) 0.034(3) 0.0002(13) 0.0037(13) 0.0003(13) C21' 0.032(3) 0.033(3) 0.035(3) -0.0001(15) 0.0037(15) 0.0000(14) O5' 0.039(6) 0.032(6) 0.059(8) 0.010(6) -0.001(6) -0.010(5) O6' 0.031(6) 0.043(7) 0.049(8) 0.001(6) 0.000(6) -0.009(5) C22 0.022(4) 0.027(4) 0.077(7) 0.009(4) 0.015(4) 0.006(3) C23 0.034(2) 0.035(2) 0.043(3) 0.0023(18) 0.0065(18) -0.0001(18) C24 0.036(2) 0.039(3) 0.046(3) 0.0020(18) 0.0070(18) 0.0015(18) C25 0.041(3) 0.042(3) 0.050(3) 0.0019(18) 0.0081(18) 0.0015(18) C26 0.038(3) 0.039(3) 0.046(3) 0.0019(18) 0.0075(18) 0.0014(18) C27 0.034(2) 0.038(3) 0.044(3) 0.0013(18) 0.0070(18) 0.0008(18) C28 0.051(3) 0.050(3) 0.052(3) 0.0017(18) 0.0054(18) -0.0015(18) C29 0.109(6) 0.095(6) 0.104(6) 0.005(5) 0.007(5) -0.006(5) C30 0.070(5) 0.075(5) 0.073(5) 0.002(4) 0.011(4) -0.014(4) C31 0.081(5) 0.080(4) 0.080(4) 0.000(3) 0.010(3) 0.004(3) C32 0.089(6) 0.086(6) 0.088(6) 0.002(4) 0.008(4) 0.006(4) C33 0.084(7) 0.084(6) 0.081(5) 0.002(4) 0.009(4) 0.001(4) N2 0.085(5) 0.083(5) 0.082(5) 0.002(3) 0.009(3) 0.005(3) O8 0.075(4) 0.077(4) 0.074(4) 0.000(3) 0.009(3) 0.003(3) C31' 0.078(4) 0.084(4) 0.076(4) 0.000(3) 0.009(3) 0.004(3) C32' 0.086(4) 0.091(5) 0.089(6) 0.005(4) 0.007(4) 0.008(4) C33' 0.098(5) 0.094(5) 0.099(6) 0.005(4) 0.011(4) -0.003(4) N2' 0.081(4) 0.087(4) 0.081(4) 0.005(3) 0.012(3) 0.007(3) O8' 0.075(3) 0.077(4) 0.072(3) 0.002(3) 0.008(3) 0.004(3) C34 0.107(3) 0.107(3) 0.108(2) -0.0005(14) 0.0127(15) 0.0005(15) C35 0.111(3) 0.109(3) 0.108(3) -0.0001(15) 0.0116(18) 0.0007(18) C36 0.108(3) 0.107(3) 0.109(3) -0.0003(15) 0.0138(18) 0.0008(18) Cd1 0.0124(3) 0.0201(3) 0.0453(4) -0.0042(2) 0.0004(2) 0.0007(2) Cd2 0.0116(3) 0.0193(4) 0.0473(5) -0.0047(3) -0.0044(3) 0.0040(3) N1 0.072(4) 0.057(4) 0.063(4) 0.011(3) 0.005(4) -0.008(4) N3 0.108(3) 0.107(3) 0.108(2) -0.0005(13) 0.0126(14) 0.0007(14) O1 0.029(2) 0.032(2) 0.050(3) -0.005(2) -0.001(2) 0.010(2) O2 0.024(2) 0.029(2) 0.044(3) -0.001(2) -0.003(2) 0.0086(19) O3 0.024(3) 0.039(4) 0.083(5) -0.015(3) 0.009(3) -0.001(3) O4 0.010(2) 0.039(3) 0.054(4) -0.006(3) 0.006(2) 0.004(2) O7 0.031(3) 0.029(3) 0.058(3) 0.004(2) -0.001(2) -0.003(2) O9 0.111(3) 0.110(3) 0.109(3) -0.0014(16) 0.0105(17) 0.0005(18) C37 0.116(6) 0.116(6) 0.116(6) 0.0000(8) 0.0143(11) 0.0001(7) C38 0.115(7) 0.116(6) 0.115(7) 0.0000(9) 0.0143(12) 0.0000(8) C39 0.116(6) 0.116(6) 0.116(7) 0.0000(9) 0.0143(12) 0.0000(8) N4 0.116(6) 0.116(6) 0.116(6) 0.0000(7) 0.0143(11) 0.0000(6) O10 0.116(6) 0.116(6) 0.116(7) 0.0000(9) 0.0143(12) 0.0000(8) C37' 0.117(6) 0.117(6) 0.117(6) 0.0001(7) 0.0145(10) 0.0000(7) C38' 0.117(6) 0.117(6) 0.117(6) 0.0001(8) 0.0146(11) 0.0000(8) N4' 0.117(6) 0.117(6) 0.117(6) 0.0001(6) 0.0145(9) 0.0000(6) C39' 0.117(6) 0.117(6) 0.117(6) 0.0000(7) 0.0145(10) 0.0000(8) O10' 0.117(6) 0.117(6) 0.117(6) 0.0000(8) 0.0144(11) -0.0001(9) _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 C1 O1 1.235(10) . ? C1 O2 1.270(9) . ? C1 C2 1.502(11) . ? C2 C7 1.356(12) . ? C2 C3 1.396(11) . ? C3 C4 1.369(11) . ? C3 H3 0.9500 . ? C4 C5 1.391(12) . ? C4 H4 0.9500 . ? C5 C6 1.387(11) . ? C5 C22 1.481(11) . ? C6 C7 1.381(11) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O3 1.232(10) . ? C8 O4 1.296(10) . ? C8 C9 1.492(10) . ? C9 C14 1.386(12) . ? C9 C10 1.389(11) . ? C10 C11 1.385(11) . ? C10 H10 0.9500 . ? C11 C12 1.372(13) . ? C11 H11 0.9500 . ? C12 C13 1.401(12) . ? C12 C24 1.484(12) . ? C13 C14 1.390(12) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O5 1.208(16) . ? C15 O6 1.275(16) . ? C15 C16 1.515(13) . ? C15 Cd1 2.714(13) 1_545 ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C17 H17A 0.9500 . ? C18 C19 1.3900 . ? C18 H18A 0.9500 . ? C19 C20 1.3900 . ? C19 C26 1.472(11) . ? C20 C21 1.3900 . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? O5 Cd1 2.441(13) 1_545 ? O6 Cd1 2.304(15) 1_545 ? C15' O5' 1.209(16) . ? C15' O6' 1.279(17) . ? C15' C16' 1.519(13) . ? C15' Cd1 2.660(14) 1_545 ? C16' C17' 1.3900 . ? C16' C21' 1.3900 . ? C17' C18' 1.3900 . ? C17' H17B 0.9500 . ? C18' C19' 1.3900 . ? C18' H18B 0.9500 . ? C19' C20' 1.3900 . ? C19' C26 1.538(12) . ? C20' C21' 1.3900 . ? C20' H20B 0.9500 . ? C21' H21B 0.9500 . ? O5' Cd1 2.437(14) 1_545 ? O6' Cd1 2.215(17) 1_545 ? C22 C27 1.382(12) . ? C22 C23 1.416(11) . ? C23 C24 1.399(12) . ? C23 H23 0.9500 . ? C24 C25 1.387(13) . ? C25 C26 1.417(13) . ? C25 H25 0.9500 . ? C26 C27 1.386(13) . ? C27 H27 0.9500 . ? C28 O7 1.240(12) . ? C28 N1 1.325(14) . ? C28 H28 0.9500 . ? C29 N1 1.440(18) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N1 1.437(16) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 O8 1.375(10) . ? C31 N2 1.411(10) . ? C31 H31A 0.9500 . ? C32 N2 1.478(10) . ? C32 H32A 0.9801 . ? C32 H32B 0.9799 . ? C32 H32C 0.9801 . ? C33 N2 1.473(10) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9802 . ? O8 Cd1 2.26(3) . ? C31' O8' 1.372(9) . ? C31' N2' 1.389(9) . ? C31' H31B 0.9500 . ? C31' H39A 1.1784 . ? C31' H39B 1.3707 . ? C32' N2' 1.461(9) . ? C32' H32C 1.5725 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? C32' H39C 0.5589 . ? C33' N2' 1.478(9) . ? C33' H32A 1.3697 . ? C33' H32B 1.3985 . ? C33' H33D 0.9800 . ? C33' H33E 0.9800 . ? C33' H33F 0.9800 . ? N2' H39C 1.4575 . ? O8' Cd1 2.287(15) . ? C34 O9 1.236(19) . ? C34 N3 1.361(9) . ? C34 H34 0.9500 . ? C35 N3 1.495(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N3 1.478(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? Cd1 O6' 2.215(17) 1_565 ? Cd1 O1 2.233(6) . ? Cd1 O6 2.304(15) 1_565 ? Cd1 O4 2.372(5) 3_455 ? Cd1 O5' 2.437(14) 1_565 ? Cd1 O5 2.441(13) 1_565 ? Cd1 O3 2.444(6) 3_455 ? Cd1 O7 2.565(7) . ? Cd1 C15' 2.660(14) 1_565 ? Cd1 C15 2.714(13) 1_565 ? Cd2 O2 2.185(5) . ? Cd2 O2 2.185(5) 7_666 ? Cd2 O4 2.269(6) 3_455 ? Cd2 O4 2.269(6) 5_766 ? Cd2 O7 2.347(6) . ? Cd2 O7 2.347(6) 7_666 ? O3 Cd1 2.444(6) 3_545 ? O4 Cd2 2.269(6) 3_545 ? O4 Cd1 2.372(5) 3_545 ? C37 O10 1.260(7) . ? C37 N4 1.394(7) . ? C37 H37A 0.9500 . ? C38 N4 1.479(10) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C38 H38D 1.1148 . ? C38 H38E 0.9295 . ? C38 H38F 1.5431 . ? C39 N4 1.483(10) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C37' O10' 1.256(10) . ? C37' N4' 1.372(9) . ? C37' H37B 0.9500 . ? C38' N4' 1.490(10) . ? C38' H38A 1.0387 . ? C38' H38B 1.3662 . ? C38' H38C 0.5639 . ? C38' H38D 0.9800 . ? C38' H38E 0.9800 . ? C38' H38F 0.9800 . ? N4' C39' 1.487(10) . ? N4' H38C 1.3580 . ? C39' C39' 1.56(9) 2_756 ? C39' H39D 0.9800 . ? C39' H39E 0.9800 . ? C39' H39F 0.9210 . ? 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 C1 O2 126.1(7) . . ? O1 C1 C2 119.3(7) . . ? O2 C1 C2 114.5(7) . . ? C7 C2 C3 119.3(7) . . ? C7 C2 C1 119.8(7) . . ? C3 C2 C1 120.9(7) . . ? C4 C3 C2 119.4(8) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 122.1(7) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 117.2(7) . . ? C6 C5 C22 119.6(8) . . ? C4 C5 C22 123.2(7) . . ? C7 C6 C5 120.8(8) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C2 C7 C6 121.1(8) . . ? C2 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? O3 C8 O4 120.6(7) . . ? O3 C8 C9 121.0(7) . . ? O4 C8 C9 118.3(7) . . ? C14 C9 C10 119.4(7) . . ? C14 C9 C8 121.0(7) . . ? C10 C9 C8 119.5(8) . . ? C11 C10 C9 120.2(8) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 120.8(8) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 119.4(8) . . ? C11 C12 C24 121.2(8) . . ? C13 C12 C24 119.4(8) . . ? C14 C13 C12 119.9(9) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C9 C14 C13 120.2(8) . . ? C9 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? O5 C15 O6 121.6(14) . . ? O5 C15 C16 120.7(13) . . ? O6 C15 C16 116.9(14) . . ? O5 C15 Cd1 64.1(8) . 1_545 ? O6 C15 Cd1 57.8(8) . 1_545 ? C16 C15 Cd1 173.8(13) . 1_545 ? C17 C16 C21 120.0 . . ? C17 C16 C15 118.0(9) . . ? C21 C16 C15 121.8(9) . . ? C18 C17 C16 120.0 . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 C26 122.6(7) . . ? C18 C19 C26 116.7(7) . . ? C21 C20 C19 120.0 . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? C15 O5 Cd1 89.5(9) . 1_545 ? C15 O6 Cd1 94.2(10) . 1_545 ? O5' C15' O6' 122.0(15) . . ? O5' C15' C16' 122.0(14) . . ? O6' C15' C16' 114.4(14) . . ? O5' C15' Cd1 66.2(9) . 1_545 ? O6' C15' Cd1 56.0(9) . 1_545 ? C16' C15' Cd1 167.2(15) . 1_545 ? C17' C16' C21' 120.0 . . ? C17' C16' C15' 119.5(9) . . ? C21' C16' C15' 120.5(9) . . ? C18' C17' C16' 120.0 . . ? C18' C17' H17B 120.0 . . ? C16' C17' H17B 120.0 . . ? C17' C18' C19' 120.0 . . ? C17' C18' H18B 120.0 . . ? C19' C18' H18B 120.0 . . ? C18' C19' C20' 120.0 . . ? C18' C19' C26 115.5(8) . . ? C20' C19' C26 123.5(8) . . ? C21' C20' C19' 120.0 . . ? C21' C20' H20B 120.0 . . ? C19' C20' H20B 120.0 . . ? C20' C21' C16' 120.0 . . ? C20' C21' H21B 120.0 . . ? C16' C21' H21B 120.0 . . ? C15' O5' Cd1 86.8(10) . 1_545 ? C15' O6' Cd1 95.4(11) . 1_545 ? C27 C22 C23 118.7(8) . . ? C27 C22 C5 120.0(7) . . ? C23 C22 C5 121.3(8) . . ? C24 C23 C22 119.9(8) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 119.7(8) . . ? C25 C24 C12 119.1(8) . . ? C23 C24 C12 121.2(8) . . ? C24 C25 C26 121.2(9) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 117.6(9) . . ? C27 C26 C19 121.9(8) . . ? C25 C26 C19 119.8(9) . . ? C27 C26 C19' 121.3(8) . . ? C25 C26 C19' 120.7(9) . . ? C19 C26 C19' 14.2(6) . . ? C22 C27 C26 122.8(8) . . ? C22 C27 H27 118.6 . . ? C26 C27 H27 118.6 . . ? O7 C28 N1 122.7(10) . . ? O7 C28 H28 118.6 . . ? N1 C28 H28 118.6 . . ? N1 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O8 C31 N2 115(2) . . ? O8 C31 H31A 122.4 . . ? N2 C31 H31A 122.4 . . ? N2 C32 H32A 109.0 . . ? N2 C32 H32B 107.4 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 112.0 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 108.6 . . ? N2 C33 H33B 106.1 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 113.6 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 N2 C33 121.9(11) . . ? C31 N2 C32 122.0(11) . . ? C33 N2 C32 116.1(11) . . ? C31 O8 Cd1 111(2) . . ? O8' C31' N2' 116.2(16) . . ? O8' C31' H31B 121.9 . . ? N2' C31' H31B 121.9 . . ? O8' C31' H39A 141.1 . . ? N2' C31' H39A 82.1 . . ? H31B C31' H39A 52.8 . . ? O8' C31' H39B 139.5 . . ? N2' C31' H39B 72.1 . . ? H31B C31' H39B 64.6 . . ? H39A C31' H39B 77.4 . . ? N2' C32' H32C 85.0 . . ? N2' C32' H32D 109.5 . . ? N2' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? N2' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? N2' C32' H39C 78.6 . . ? H32C C32' H39C 145.6 . . ? H32D C32' H39C 33.7 . . ? H32E C32' H39C 134.7 . . ? H32F C32' H39C 109.0 . . ? N2' C33' H32A 65.5 . . ? N2' C33' H32B 102.4 . . ? H32A C33' H32B 70.6 . . ? N2' C33' H33D 109.5 . . ? N2' C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? N2' C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? C31' N2' C32' 118.8(14) . . ? C31' N2' C33' 123.8(15) . . ? C32' N2' C33' 117.4(10) . . ? C31' N2' H39C 97.1 . . ? C32' N2' H39C 22.1 . . ? C33' N2' H39C 138.5 . . ? C31' O8' Cd1 117.3(9) . . ? O9 C34 N3 119.4(17) . . ? O9 C34 H34 120.3 . . ? N3 C34 H34 120.3 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O6' Cd1 O1 126.4(5) 1_565 . ? O6' Cd1 O8 114.2(8) 1_565 . ? O1 Cd1 O8 87.7(7) . . ? O6' Cd1 O8' 127.2(6) 1_565 . ? O1 Cd1 O8' 81.7(4) . . ? O8 Cd1 O8' 13.4(8) . . ? O6' Cd1 O6 18.3(4) 1_565 1_565 ? O1 Cd1 O6 136.5(3) . 1_565 ? O8 Cd1 O6 97.3(8) . 1_565 ? O8' Cd1 O6 109.9(6) . 1_565 ? O6' Cd1 O4 121.5(4) 1_565 3_455 ? O1 Cd1 O4 95.0(2) . 3_455 ? O8 Cd1 O4 105.8(7) . 3_455 ? O8' Cd1 O4 94.2(4) . 3_455 ? O6 Cd1 O4 124.3(4) 1_565 3_455 ? O6' Cd1 O5' 55.5(4) 1_565 1_565 ? O1 Cd1 O5' 90.7(4) . 1_565 ? O8 Cd1 O5' 72.6(8) . 1_565 ? O8' Cd1 O5' 84.8(5) . 1_565 ? O6 Cd1 O5' 51.0(5) 1_565 1_565 ? O4 Cd1 O5' 174.0(4) 3_455 1_565 ? O6' Cd1 O5 50.4(5) 1_565 1_565 ? O1 Cd1 O5 82.5(3) . 1_565 ? O8 Cd1 O5 91.8(8) . 1_565 ? O8' Cd1 O5 102.9(5) . 1_565 ? O6 Cd1 O5 54.3(4) 1_565 1_565 ? O4 Cd1 O5 162.1(4) 3_455 1_565 ? O5' Cd1 O5 21.2(4) 1_565 1_565 ? O6' Cd1 O3 82.0(4) 1_565 3_455 ? O1 Cd1 O3 148.2(2) . 3_455 ? O8 Cd1 O3 93.1(7) . 3_455 ? O8' Cd1 O3 91.8(4) . 3_455 ? O6 Cd1 O3 75.0(3) 1_565 3_455 ? O4 Cd1 O3 54.2(2) 3_455 3_455 ? O5' Cd1 O3 119.8(4) 1_565 3_455 ? O5 Cd1 O3 129.2(3) 1_565 3_455 ? O6' Cd1 O7 74.5(5) 1_565 . ? O1 Cd1 O7 79.8(2) . . ? O8 Cd1 O7 167.5(7) . . ? O8' Cd1 O7 157.6(4) . . ? O6 Cd1 O7 92.2(4) 1_565 . ? O4 Cd1 O7 74.9(2) 3_455 . ? O5' Cd1 O7 108.0(4) 1_565 . ? O5 Cd1 O7 87.3(4) 1_565 . ? O3 Cd1 O7 97.1(2) 3_455 . ? O6' Cd1 C15' 28.6(4) 1_565 1_565 ? O1 Cd1 C15' 110.3(4) . 1_565 ? O8 Cd1 C15' 92.3(9) . 1_565 ? O8' Cd1 C15' 105.6(6) . 1_565 ? O6 Cd1 C15' 26.7(5) 1_565 1_565 ? O4 Cd1 C15' 149.5(4) 3_455 1_565 ? O5' Cd1 C15' 27.0(4) 1_565 1_565 ? O5 Cd1 C15' 27.8(6) 1_565 1_565 ? O3 Cd1 C15' 101.4(4) 3_455 1_565 ? O7 Cd1 C15' 92.7(5) . 1_565 ? O6' Cd1 C15 26.5(6) 1_565 1_565 ? O1 Cd1 C15 108.6(4) . 1_565 ? O8 Cd1 C15 96.7(9) . 1_565 ? O8' Cd1 C15 110.0(6) . 1_565 ? O6 Cd1 C15 27.9(4) 1_565 1_565 ? O4 Cd1 C15 148.0(4) 3_455 1_565 ? O5' Cd1 C15 29.4(5) 1_565 1_565 ? O5 Cd1 C15 26.4(4) 1_565 1_565 ? O3 Cd1 C15 102.9(4) 3_455 1_565 ? O7 Cd1 C15 88.0(5) . 1_565 ? C15' Cd1 C15 4.8(10) 1_565 1_565 ? O2 Cd2 O2 180.000(1) . 7_666 ? O2 Cd2 O4 85.2(2) . 3_455 ? O2 Cd2 O4 94.8(2) 7_666 3_455 ? O2 Cd2 O4 94.8(2) . 5_766 ? O2 Cd2 O4 85.2(2) 7_666 5_766 ? O4 Cd2 O4 180.000(1) 3_455 5_766 ? O2 Cd2 O7 93.6(2) . . ? O2 Cd2 O7 86.4(2) 7_666 . ? O4 Cd2 O7 81.2(2) 3_455 . ? O4 Cd2 O7 98.8(2) 5_766 . ? O2 Cd2 O7 86.4(2) . 7_666 ? O2 Cd2 O7 93.6(2) 7_666 7_666 ? O4 Cd2 O7 98.8(2) 3_455 7_666 ? O4 Cd2 O7 81.2(2) 5_766 7_666 ? O7 Cd2 O7 180.000(1) . 7_666 ? C28 N1 C30 123.0(10) . . ? C28 N1 C29 121.9(12) . . ? C30 N1 C29 115.1(11) . . ? C34 N3 C36 124.1(15) . . ? C34 N3 C35 113.4(14) . . ? C36 N3 C35 122.5(14) . . ? C1 O1 Cd1 129.6(5) . . ? C1 O2 Cd2 131.9(5) . . ? C8 O3 Cd1 91.4(5) . 3_545 ? C8 O4 Cd2 130.9(5) . 3_545 ? C8 O4 Cd1 93.1(5) . 3_545 ? Cd2 O4 Cd1 99.6(2) 3_545 3_545 ? C28 O7 Cd2 128.2(6) . . ? C28 O7 Cd1 119.0(6) . . ? Cd2 O7 Cd1 92.3(2) . . ? O10 C37 N4 103.8(12) . . ? O10 C37 H37A 128.1 . . ? N4 C37 H37A 128.1 . . ? N4 C38 H38A 109.4 . . ? N4 C38 H38B 109.0 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 110.0 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N4 C38 H38D 99.3 . . ? H38A C38 H38D 28.8 . . ? H38B C38 H38D 137.3 . . ? H38C C38 H38D 89.0 . . ? N4 C38 H38E 155.3 . . ? H38A C38 H38E 85.5 . . ? H38B C38 H38E 46.4 . . ? H38C C38 H38E 81.7 . . ? H38D C38 H38E 102.7 . . ? N4 C38 H38F 121.9 . . ? H38A C38 H38F 89.8 . . ? H38B C38 H38F 115.0 . . ? H38C C38 H38F 19.9 . . ? H38D C38 H38F 72.0 . . ? H38E C38 H38F 76.2 . . ? N4 C39 H39A 109.9 . . ? N4 C39 H39B 109.6 . . ? H39A C39 H39B 109.5 . . ? N4 C39 H39C 109.0 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 N4 C38 123.0(11) . . ? C37 N4 C39 121.6(11) . . ? C38 N4 C39 115.4(10) . . ? O10' C37' N4' 105.4(12) . . ? O10' C37' H37B 127.3 . . ? N4' C37' H37B 127.3 . . ? N4' C38' H38A 117.4 . . ? N4' C38' H38B 79.5 . . ? H38A C38' H38B 82.2 . . ? N4' C38' H38C 65.6 . . ? H38A C38' H38C 173.5 . . ? H38B C38' H38C 104.1 . . ? N4' C38' H38D 112.8 . . ? H38A C38' H38D 30.7 . . ? H38B C38' H38D 111.5 . . ? H38C C38' H38D 143.4 . . ? N4' C38' H38E 109.4 . . ? H38A C38' H38E 79.9 . . ? H38B C38' H38E 32.5 . . ? H38C C38' H38E 104.8 . . ? H38D C38' H38E 109.5 . . ? N4' C38' H38F 106.2 . . ? H38A C38' H38F 129.4 . . ? H38B C38' H38F 132.1 . . ? H38C C38' H38F 45.1 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C37' N4' C39' 122.9(11) . . ? C37' N4' C38' 122.4(11) . . ? C39' N4' C38' 114.6(10) . . ? C37' N4' H38C 110.0 . . ? C39' N4' H38C 123.8 . . ? C38' N4' H38C 22.2 . . ? N4' C39' C39' 127(4) . 2_756 ? N4' C39' H39D 108.5 . . ? C39' C39' H39D 117.2 2_756 . ? N4' C39' H39E 110.2 . . ? C39' C39' H39E 79.6 2_756 . ? H39D C39' H39E 109.5 . . ? N4' C39' H39F 106.2 . . ? C39' C39' H39F 32.2 2_756 . ? H39D C39' H39F 111.5 . . ? H39E C39' H39F 110.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 177.1(8) . . . . ? O2 C1 C2 C7 -1.1(12) . . . . ? O1 C1 C2 C3 -1.3(13) . . . . ? O2 C1 C2 C3 -179.5(8) . . . . ? C7 C2 C3 C4 -1.9(14) . . . . ? C1 C2 C3 C4 176.5(8) . . . . ? C2 C3 C4 C5 -0.5(14) . . . . ? C3 C4 C5 C6 2.2(14) . . . . ? C3 C4 C5 C22 -176.2(9) . . . . ? C4 C5 C6 C7 -1.6(15) . . . . ? C22 C5 C6 C7 176.9(9) . . . . ? C3 C2 C7 C6 2.6(15) . . . . ? C1 C2 C7 C6 -175.9(9) . . . . ? C5 C6 C7 C2 -0.7(16) . . . . ? O3 C8 C9 C14 179.9(9) . . . . ? O4 C8 C9 C14 1.4(13) . . . . ? O3 C8 C9 C10 3.5(13) . . . . ? O4 C8 C9 C10 -175.0(8) . . . . ? C14 C9 C10 C11 1.5(13) . . . . ? C8 C9 C10 C11 178.0(8) . . . . ? C9 C10 C11 C12 -0.2(14) . . . . ? C10 C11 C12 C13 -2.2(14) . . . . ? C10 C11 C12 C24 176.4(8) . . . . ? C11 C12 C13 C14 3.4(13) . . . . ? C24 C12 C13 C14 -175.2(8) . . . . ? C10 C9 C14 C13 -0.3(13) . . . . ? C8 C9 C14 C13 -176.7(8) . . . . ? C12 C13 C14 C9 -2.2(13) . . . . ? O5 C15 C16 C17 16(3) . . . . ? O6 C15 C16 C17 -174.3(16) . . . . ? Cd1 C15 C16 C17 155(11) 1_545 . . . ? O5 C15 C16 C21 -169.3(16) . . . . ? O6 C15 C16 C21 0(2) . . . . ? Cd1 C15 C16 C21 -31(12) 1_545 . . . ? C21 C16 C17 C18 0.0 . . . . ? C15 C16 C17 C18 174.6(13) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C17 C18 C19 C26 -170.2(10) . . . . ? C18 C19 C20 C21 0.0 . . . . ? C26 C19 C20 C21 169.6(10) . . . . ? C19 C20 C21 C16 0.0 . . . . ? C17 C16 C21 C20 0.0 . . . . ? C15 C16 C21 C20 -174.3(14) . . . . ? O6 C15 O5 Cd1 6(2) . . . 1_545 ? C16 C15 O5 Cd1 175.4(18) . . . 1_545 ? O5 C15 O6 Cd1 -7(2) . . . 1_545 ? C16 C15 O6 Cd1 -176.2(15) . . . 1_545 ? O5' C15' C16' C17' -9(3) . . . . ? O6' C15' C16' C17' -174.5(15) . . . . ? Cd1 C15' C16' C17' -135(5) 1_545 . . . ? O5' C15' C16' C21' 173.2(19) . . . . ? O6' C15' C16' C21' 8(2) . . . . ? Cd1 C15' C16' C21' 47(6) 1_545 . . . ? C21' C16' C17' C18' 0.0 . . . . ? C15' C16' C17' C18' -178.0(15) . . . . ? C16' C17' C18' C19' 0.0 . . . . ? C17' C18' C19' C20' 0.0 . . . . ? C17' C18' C19' C26 169.3(10) . . . . ? C18' C19' C20' C21' 0.0 . . . . ? C26 C19' C20' C21' -168.4(11) . . . . ? C19' C20' C21' C16' 0.0 . . . . ? C17' C16' C21' C20' 0.0 . . . . ? C15' C16' C21' C20' 178.0(15) . . . . ? O6' C15' O5' Cd1 -4(2) . . . 1_545 ? C16' C15' O5' Cd1 -169(2) . . . 1_545 ? O5' C15' O6' Cd1 5(3) . . . 1_545 ? C16' C15' O6' Cd1 170.3(15) . . . 1_545 ? C6 C5 C22 C27 -30.7(14) . . . . ? C4 C5 C22 C27 147.7(10) . . . . ? C6 C5 C22 C23 150.9(10) . . . . ? C4 C5 C22 C23 -30.7(15) . . . . ? C27 C22 C23 C24 -0.5(14) . . . . ? C5 C22 C23 C24 177.9(9) . . . . ? C22 C23 C24 C25 3.3(14) . . . . ? C22 C23 C24 C12 -176.0(9) . . . . ? C11 C12 C24 C25 -143.5(10) . . . . ? C13 C12 C24 C25 35.2(13) . . . . ? C11 C12 C24 C23 35.9(14) . . . . ? C13 C12 C24 C23 -145.5(9) . . . . ? C23 C24 C25 C26 -3.2(15) . . . . ? C12 C24 C25 C26 176.2(9) . . . . ? C24 C25 C26 C27 0.2(14) . . . . ? C24 C25 C26 C19 -170.5(9) . . . . ? C24 C25 C26 C19' 173.1(9) . . . . ? C20 C19 C26 C27 -16.9(13) . . . . ? C18 C19 C26 C27 153.0(8) . . . . ? C20 C19 C26 C25 153.3(8) . . . . ? C18 C19 C26 C25 -36.7(12) . . . . ? C20 C19 C26 C19' -109(3) . . . . ? C18 C19 C26 C19' 61(2) . . . . ? C18' C19' C26 C27 -154.3(8) . . . . ? C20' C19' C26 C27 14.6(14) . . . . ? C18' C19' C26 C25 33.0(12) . . . . ? C20' C19' C26 C25 -158.1(8) . . . . ? C18' C19' C26 C19 -58(2) . . . . ? C20' C19' C26 C19 111(3) . . . . ? C23 C22 C27 C26 -2.6(15) . . . . ? C5 C22 C27 C26 178.9(9) . . . . ? C25 C26 C27 C22 2.8(15) . . . . ? C19 C26 C27 C22 173.3(10) . . . . ? C19' C26 C27 C22 -170.1(10) . . . . ? O8 C31 N2 C33 0.8(18) . . . . ? O8 C31 N2 C32 180.0(12) . . . . ? N2 C31 O8 Cd1 -165.4(18) . . . . ? O8' C31' N2' C32' -179.9(10) . . . . ? O8' C31' N2' C33' 3.0(16) . . . . ? N2' C31' O8' Cd1 -126.0(12) . . . . ? C31 O8 Cd1 O6' -138.0(15) . . . 1_565 ? C31 O8 Cd1 O1 -8.8(15) . . . . ? C31 O8 Cd1 O8' 55(4) . . . . ? C31 O8 Cd1 O6 -145.4(15) . . . 1_565 ? C31 O8 Cd1 O4 85.8(16) . . . 3_455 ? C31 O8 Cd1 O5' -100.3(16) . . . 1_565 ? C31 O8 Cd1 O5 -91.2(16) . . . 1_565 ? C31 O8 Cd1 O3 139.4(15) . . . 3_455 ? C31 O8 Cd1 O7 -6(4) . . . . ? C31 O8 Cd1 C15' -119.1(16) . . . 1_565 ? C31 O8 Cd1 C15 -117.3(16) . . . 1_565 ? C31' O8' Cd1 O6' -69.8(13) . . . 1_565 ? C31' O8' Cd1 O1 60.2(11) . . . . ? C31' O8' Cd1 O8 -55(4) . . . . ? C31' O8' Cd1 O6 -76.4(12) . . . 1_565 ? C31' O8' Cd1 O4 154.7(11) . . . 3_455 ? C31' O8' Cd1 O5' -31.3(12) . . . 1_565 ? C31' O8' Cd1 O5 -20.1(12) . . . 1_565 ? C31' O8' Cd1 O3 -151.1(11) . . . 3_455 ? C31' O8' Cd1 O7 95.1(14) . . . . ? C31' O8' Cd1 C15' -48.7(13) . . . 1_565 ? C31' O8' Cd1 C15 -46.7(13) . . . 1_565 ? O7 C28 N1 C30 0.4(17) . . . . ? O7 C28 N1 C29 -179.3(12) . . . . ? O9 C34 N3 C36 6(3) . . . . ? O9 C34 N3 C35 -176.0(16) . . . . ? O2 C1 O1 Cd1 20.5(13) . . . . ? C2 C1 O1 Cd1 -157.5(6) . . . . ? O6' Cd1 O1 C1 -131.6(8) 1_565 . . . ? O8 Cd1 O1 C1 109.7(10) . . . . ? O8' Cd1 O1 C1 97.6(8) . . . . ? O6 Cd1 O1 C1 -152.1(9) 1_565 . . . ? O4 Cd1 O1 C1 4.1(8) 3_455 . . . ? O5' Cd1 O1 C1 -177.7(8) 1_565 . . . ? O5 Cd1 O1 C1 -158.1(8) 1_565 . . . ? O3 Cd1 O1 C1 17.6(10) 3_455 . . . ? O7 Cd1 O1 C1 -69.6(7) . . . . ? C15' Cd1 O1 C1 -158.7(9) 1_565 . . . ? C15 Cd1 O1 C1 -154.0(9) 1_565 . . . ? O1 C1 O2 Cd2 17.9(13) . . . . ? C2 C1 O2 Cd2 -164.0(5) . . . . ? O2 Cd2 O2 C1 -161(100) 7_666 . . . ? O4 Cd2 O2 C1 -66.8(7) 3_455 . . . ? O4 Cd2 O2 C1 113.2(7) 5_766 . . . ? O7 Cd2 O2 C1 14.0(7) . . . . ? O7 Cd2 O2 C1 -166.0(7) 7_666 . . . ? O4 C8 O3 Cd1 7.8(9) . . . 3_545 ? C9 C8 O3 Cd1 -170.7(7) . . . 3_545 ? O3 C8 O4 Cd2 -113.5(8) . . . 3_545 ? C9 C8 O4 Cd2 65.0(10) . . . 3_545 ? O3 C8 O4 Cd1 -8.0(9) . . . 3_545 ? C9 C8 O4 Cd1 170.5(7) . . . 3_545 ? N1 C28 O7 Cd2 -146.0(8) . . . . ? N1 C28 O7 Cd1 94.3(11) . . . . ? O2 Cd2 O7 C28 170.2(8) . . . . ? O2 Cd2 O7 C28 -9.8(8) 7_666 . . . ? O4 Cd2 O7 C28 -105.2(8) 3_455 . . . ? O4 Cd2 O7 C28 74.8(8) 5_766 . . . ? O7 Cd2 O7 C28 151(35) 7_666 . . . ? O2 Cd2 O7 Cd1 -59.3(2) . . . . ? O2 Cd2 O7 Cd1 120.7(2) 7_666 . . . ? O4 Cd2 O7 Cd1 25.28(18) 3_455 . . . ? O4 Cd2 O7 Cd1 -154.72(18) 5_766 . . . ? O7 Cd2 O7 Cd1 -79(35) 7_666 . . . ? O6' Cd1 O7 C28 -17.3(8) 1_565 . . . ? O1 Cd1 O7 C28 -149.7(7) . . . . ? O8 Cd1 O7 C28 -153(3) . . . . ? O8' Cd1 O7 C28 175.1(11) . . . . ? O6 Cd1 O7 C28 -12.8(8) 1_565 . . . ? O4 Cd1 O7 C28 112.2(7) 3_455 . . . ? O5' Cd1 O7 C28 -62.3(8) 1_565 . . . ? O5 Cd1 O7 C28 -66.9(7) 1_565 . . . ? O3 Cd1 O7 C28 62.3(7) 3_455 . . . ? C15' Cd1 O7 C28 -39.6(8) 1_565 . . . ? C15 Cd1 O7 C28 -40.4(8) 1_565 . . . ? O6' Cd1 O7 Cd2 -154.2(5) 1_565 . . . ? O1 Cd1 O7 Cd2 73.3(2) . . . . ? O8 Cd1 O7 Cd2 70(3) . . . . ? O8' Cd1 O7 Cd2 38.2(10) . . . . ? O6 Cd1 O7 Cd2 -149.7(3) 1_565 . . . ? O4 Cd1 O7 Cd2 -24.72(19) 3_455 . . . ? O5' Cd1 O7 Cd2 160.8(4) 1_565 . . . ? O5 Cd1 O7 Cd2 156.2(3) 1_565 . . . ? O3 Cd1 O7 Cd2 -74.6(2) 3_455 . . . ? C15' Cd1 O7 Cd2 -176.5(4) 1_565 . . . ? C15 Cd1 O7 Cd2 -177.3(4) 1_565 . . . ? O10 C37 N4 C38 -1.0(17) . . . . ? O10 C37 N4 C39 -179.1(14) . . . . ? O10' C37' N4' C39' -179.7(14) . . . . ? O10' C37' N4' C38' -0.5(18) . . . . ? C37' N4' C39' C39' -66(4) . . . 2_756 ? C38' N4' C39' C39' 115(4) . . . 2_756 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.94 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.620 _refine_diff_density_min -1.753 _refine_diff_density_rms 0.225 # start Validation Reply Form _vrf_PLAT413_1 ; PROBLEM: Short Inter XH3...XHn RESPONSE: One and a half DMF molecules are disorderd. ; _vrf_PLAT430_1 ; PROBLEM: Short Inter D...A Contact RESPONSE: One and a half DMF molecules are disorderd. ; _vrf_PLAT770_1 ; PROBLEM: Suspect C-H Bond in CIF RESPONSE: One and a half DMF molecules are disorderd. ; _vrf_PLAT771_1 ; PROBLEM: Suspect N-H Bond in CIF RESPONSE: One and a half DMF molecules are disorderd. ; # end Validation Reply Form # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 825083' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C32 H20 Cd N O6), (C5 H6 N), 0.5(C3 H7 N O), 3(H2 O)' _chemical_formula_sum 'C38.50 H35.50 Cd N2.50 O9.50' _chemical_formula_weight 797.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1268(2) _cell_length_b 26.2489(7) _cell_length_c 15.3536(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.4200(10) _cell_angle_gamma 90.00 _cell_volume 3677.11(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1593 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 28.77 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7756 _exptl_absorpt_correction_T_max 0.8282 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% . _diffrn_reflns_number 26445 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8151 _reflns_number_gt 7032 _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. During the refinement, the restraint command 'dfix' 'isor' 'delu' and 'simu' were ued to restrain the C and N atoms with NPD and ADP problems in the disorder of one pyridinium cation, three water molecules and hlaf disordered DMF molecule. Such a refinement led to a relative high restraint value 118. ; _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^)+(0.0984P)^2^+8.3205P] 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 8151 _refine_ls_number_parameters 551 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1797 _refine_ls_wR_factor_gt 0.1731 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6556(5) 0.27126(16) 0.4412(3) 0.0425(9) Uani 1 1 d . . . C2 C 0.5871(5) 0.22153(15) 0.4662(3) 0.0399(9) Uani 1 1 d . . . C3 C 0.6701(4) 0.18355(15) 0.5056(3) 0.0392(8) Uani 1 1 d . . . H3 H 0.7721 0.1887 0.5160 0.047 Uiso 1 1 calc R . . C4 C 0.6067(5) 0.13822(14) 0.5301(3) 0.0384(9) Uani 1 1 d . . . H4 H 0.6650 0.1132 0.5592 0.046 Uiso 1 1 calc R . . C5 C 0.4588(4) 0.12840(14) 0.5128(3) 0.0333(8) Uani 1 1 d . . . C6 C 0.3751(5) 0.16646(17) 0.4717(3) 0.0446(10) Uani 1 1 d . . . H6 H 0.2744 0.1604 0.4584 0.054 Uiso 1 1 calc R . . C7 C 0.4370(5) 0.21292(17) 0.4501(3) 0.0485(10) Uani 1 1 d . . . H7 H 0.3778 0.2389 0.4244 0.058 Uiso 1 1 calc R . . C8 C 0.6053(5) -0.09575(19) 0.9415(3) 0.0493(11) Uani 1 1 d . . . C9 C 0.5428(5) -0.07049(17) 0.8610(3) 0.0434(9) Uani 1 1 d . . . C10 C 0.5208(5) -0.09825(17) 0.7846(3) 0.0451(10) Uani 1 1 d . . . H10 H 0.5429 -0.1336 0.7835 0.054 Uiso 1 1 calc R . . C11 C 0.4664(5) -0.07420(16) 0.7097(3) 0.0420(9) Uani 1 1 d . . . H11 H 0.4518 -0.0934 0.6578 0.050 Uiso 1 1 calc R . . C12 C 0.4328(4) -0.02210(15) 0.7097(2) 0.0350(8) Uani 1 1 d . . . C13 C 0.4532(5) 0.00521(16) 0.7878(3) 0.0407(9) Uani 1 1 d . . . H13 H 0.4298 0.0404 0.7898 0.049 Uiso 1 1 calc R . . C14 C 0.5073(5) -0.01917(18) 0.8621(3) 0.0460(10) Uani 1 1 d . . . H14 H 0.5203 -0.0004 0.9146 0.055 Uiso 1 1 calc R . . C15 C -0.1151(5) -0.09741(18) 0.2265(3) 0.0465(10) Uani 1 1 d . . . C16 C -0.0180(4) -0.07260(17) 0.2950(3) 0.0427(9) Uani 1 1 d . . . C17 C 0.0867(5) -0.03699(19) 0.2705(3) 0.0519(11) Uani 1 1 d . . . H17 H 0.0986 -0.0294 0.2106 0.062 Uiso 1 1 calc R . . C18 C 0.1738(5) -0.01259(18) 0.3332(3) 0.0474(10) Uani 1 1 d . . . H18 H 0.2447 0.0116 0.3156 0.057 Uiso 1 1 calc R . . C19 C 0.1590(4) -0.02297(15) 0.4218(3) 0.0360(8) Uani 1 1 d . . . C20 C 0.0565(4) -0.05959(16) 0.4460(3) 0.0378(8) Uani 1 1 d . . . H20 H 0.0454 -0.0676 0.5058 0.045 Uiso 1 1 calc R . . C21 C -0.0297(4) -0.08453(17) 0.3827(3) 0.0431(9) Uani 1 1 d . . . H21 H -0.0972 -0.1100 0.3999 0.052 Uiso 1 1 calc R . . C22 C 0.3959(4) 0.07798(14) 0.5336(3) 0.0336(8) Uani 1 1 d . . . C23 C 0.4345(4) 0.05318(14) 0.6110(3) 0.0344(8) Uani 1 1 d . . . H23 H 0.4965 0.0699 0.6526 0.041 Uiso 1 1 calc R . . C24 C 0.3839(4) 0.00425(14) 0.6287(3) 0.0337(8) Uani 1 1 d . . . C25 C 0.2930(4) -0.02010(14) 0.5662(2) 0.0339(8) Uani 1 1 d . . . H25 H 0.2588 -0.0536 0.5773 0.041 Uiso 1 1 calc R . . C26 C 0.2523(4) 0.00377(14) 0.4886(2) 0.0329(7) Uani 1 1 d . . . C27 C 0.3035(4) 0.05296(15) 0.4732(3) 0.0349(8) Uani 1 1 d . . . H27 H 0.2751 0.0698 0.4207 0.042 Uiso 1 1 calc R . . O1 O 0.7858(4) 0.27148(13) 0.4169(2) 0.0569(9) Uani 1 1 d . . . O2 O 0.5824(4) 0.31150(12) 0.4457(2) 0.0539(8) Uani 1 1 d . . . O3 O 0.6387(5) -0.06884(14) 1.0064(2) 0.0636(10) Uani 1 1 d . . . O4 O 0.6216(6) -0.14330(15) 0.9432(3) 0.0746(13) Uani 1 1 d . . . O5 O -0.1887(4) -0.13605(14) 0.2469(3) 0.0595(10) Uani 1 1 d . . . O6 O -0.1203(4) -0.07865(13) 0.1513(2) 0.0565(9) Uani 1 1 d . . . N1 N 1.0120(3) 0.35419(13) 0.3493(2) 0.0543(10) Uani 1 1 d G . . C28 C 1.1348(4) 0.37004(17) 0.3973(3) 0.097(3) Uani 1 1 d G . . H28A H 1.1235 0.3896 0.4487 0.116 Uiso 1 1 calc R . . C29 C 1.2742(3) 0.3572(2) 0.3700(4) 0.122(4) Uani 1 1 d G . . H29A H 1.3581 0.3680 0.4029 0.146 Uiso 1 1 calc R . . C30 C 1.2907(4) 0.3285(2) 0.2948(4) 0.099(3) Uani 1 1 d G . . H30A H 1.3860 0.3198 0.2762 0.119 Uiso 1 1 calc R . . C31 C 1.1679(5) 0.3127(2) 0.2468(3) 0.109(3) Uani 1 1 d G . . H31A H 1.1792 0.2931 0.1954 0.131 Uiso 1 1 calc R . . C32 C 1.0285(4) 0.32550(18) 0.2740(2) 0.088(2) Uani 1 1 d G . . H32A H 0.9446 0.3147 0.2412 0.105 Uiso 1 1 calc R . . Cd1 Cd 0.78317(3) 0.362375(10) 0.406133(19) 0.03697(13) Uani 1 1 d . . . N2 N 0.3314(14) 0.3112(5) 0.7050(13) 0.202(5) Uani 0.438(6) 1 d PGU A 1 H2A H 0.2425 0.3074 0.6825 0.243 Uiso 0.438(6) 1 calc PR A 1 C33 C 0.4519(18) 0.3097(5) 0.6514(11) 0.202(5) Uani 0.438(6) 1 d PGU A 1 H33A H 0.4382 0.3045 0.5905 0.243 Uiso 0.438(6) 1 calc PR A 1 C34 C 0.5924(15) 0.3158(5) 0.6869(12) 0.203(4) Uani 0.438(6) 1 d PGU A 1 H34A H 0.6747 0.3148 0.6503 0.244 Uiso 0.438(6) 1 calc PR A 1 C35 C 0.6124(16) 0.3234(6) 0.7760(12) 0.203(4) Uani 0.438(6) 1 d PGU A 1 H35A H 0.7084 0.3276 0.8003 0.243 Uiso 0.438(6) 1 calc PR A 1 C36 C 0.492(2) 0.3249(7) 0.8296(9) 0.204(4) Uani 0.438(6) 1 d PGU A 1 H36A H 0.5056 0.3301 0.8905 0.244 Uiso 0.438(6) 1 calc PR A 1 C37 C 0.3514(18) 0.3189(6) 0.7941(12) 0.203(5) Uani 0.438(6) 1 d PGU A 1 H37A H 0.2691 0.3199 0.8307 0.243 Uiso 0.438(6) 1 calc PR A 1 N2' N 0.4274(18) 0.4210(5) 0.6436(12) 0.203(4) Uani 0.562(6) 1 d PGU A 2 H2'A H 0.3852 0.4435 0.6088 0.243 Uiso 0.562(6) 1 calc PR A 2 C33' C 0.5334(19) 0.3883(6) 0.6119(9) 0.204(4) Uani 0.562(6) 1 d PGU A 2 H33B H 0.5602 0.3903 0.5526 0.245 Uiso 0.562(6) 1 calc PR A 2 C34' C 0.6001(13) 0.3527(6) 0.6669(10) 0.203(4) Uani 0.562(6) 1 d PGU A 2 H34B H 0.6726 0.3304 0.6452 0.244 Uiso 0.562(6) 1 calc PR A 2 C35' C 0.5609(13) 0.3498(5) 0.7537(9) 0.203(4) Uani 0.562(6) 1 d PGU A 2 H35B H 0.6065 0.3255 0.7913 0.244 Uiso 0.562(6) 1 calc PR A 2 C36' C 0.4549(18) 0.3825(5) 0.7854(9) 0.204(4) Uani 0.562(6) 1 d PGU A 2 H36B H 0.4280 0.3805 0.8447 0.244 Uiso 0.562(6) 1 calc PR A 2 C37' C 0.3881(17) 0.4181(4) 0.7304(13) 0.203(4) Uani 0.562(6) 1 d PGU A 2 H37B H 0.3157 0.4404 0.7521 0.243 Uiso 0.562(6) 1 calc PR A 2 C38 C 0.2605(10) 0.2954(12) 0.5817(19) 0.343(7) Uani 0.50 1 d PDU B 2 C39 C 0.337(4) 0.2701(17) 0.723(2) 0.344(7) Uani 0.50 1 d PDU B 2 C40 C 0.124(5) 0.2313(17) 0.657(3) 0.343(7) Uani 0.50 1 d PDU B 2 N3 N 0.240(3) 0.2659(11) 0.652(2) 0.343(7) Uani 0.50 1 d PDU B 2 O7 O 0.359(3) 0.3266(12) 0.572(2) 0.343(7) Uani 0.50 1 d PDU B 2 O1W O 0.069(2) 0.2446(8) 0.4847(14) 0.098(3) Uani 0.30 1 d PU C -1 O2W O 0.8335(12) 0.0216(4) 0.9916(8) 0.075(2) Uani 0.40 1 d PU D -1 O3W O 0.3476(13) 0.2226(4) 0.1685(8) 0.077(3) Uani 0.40 1 d PU E -1 O1'W O 0.0434(8) 0.2187(3) 0.4485(6) 0.094(2) Uani 0.70 1 d PU F -2 O2'W O 0.8885(17) 0.0100(6) 1.0501(11) 0.077(3) Uani 0.30 1 d PU G -2 O3'W O 0.1142(16) 0.2238(5) 0.6471(10) 0.091(3) Uani 0.40 1 d PU H -2 O3A O 0.133(3) 0.2312(10) 0.7216(18) 0.090(4) Uani 0.20 1 d PU I -2 O3B O 0.111(2) 0.2794(7) 0.5635(12) 0.094(3) Uani 0.30 1 d PU J -2 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 C1 0.042(2) 0.042(2) 0.043(2) 0.0069(17) -0.0120(17) -0.0057(16) C2 0.039(2) 0.039(2) 0.041(2) 0.0022(16) -0.0080(17) -0.0047(16) C3 0.0333(19) 0.0374(19) 0.046(2) -0.0009(16) -0.0088(16) -0.0027(15) C4 0.036(2) 0.0351(19) 0.044(2) -0.0023(15) -0.0071(17) -0.0007(14) C5 0.0336(19) 0.0356(18) 0.0305(19) -0.0025(14) -0.0064(14) -0.0022(14) C6 0.033(2) 0.046(2) 0.054(3) 0.0069(19) -0.0134(18) -0.0026(16) C7 0.041(2) 0.046(2) 0.058(3) 0.013(2) -0.015(2) -0.0029(17) C8 0.047(2) 0.059(3) 0.041(2) -0.002(2) -0.0117(19) 0.014(2) C9 0.046(2) 0.051(2) 0.032(2) -0.0024(17) -0.0102(17) 0.0065(18) C10 0.053(3) 0.042(2) 0.040(2) -0.0027(17) -0.0097(18) 0.0065(18) C11 0.049(2) 0.039(2) 0.036(2) -0.0069(16) -0.0122(17) 0.0010(17) C12 0.0333(19) 0.0402(19) 0.0311(19) -0.0022(15) -0.0054(14) -0.0015(14) C13 0.044(2) 0.041(2) 0.037(2) -0.0058(16) -0.0046(17) 0.0037(16) C14 0.053(3) 0.054(2) 0.031(2) -0.0086(17) -0.0109(18) 0.0053(19) C15 0.033(2) 0.051(2) 0.055(3) -0.022(2) -0.0094(18) 0.0032(17) C16 0.031(2) 0.050(2) 0.046(2) -0.0170(18) -0.0153(17) 0.0044(16) C17 0.053(3) 0.061(3) 0.040(2) -0.003(2) -0.015(2) -0.011(2) C18 0.049(2) 0.057(3) 0.035(2) -0.0017(18) -0.0155(18) -0.014(2) C19 0.0279(18) 0.0381(19) 0.041(2) -0.0071(15) -0.0103(15) 0.0006(14) C20 0.0267(18) 0.045(2) 0.041(2) -0.0087(16) -0.0036(15) -0.0029(15) C21 0.0294(19) 0.047(2) 0.052(3) -0.0143(19) -0.0024(17) -0.0055(16) C22 0.0272(17) 0.0357(18) 0.038(2) -0.0036(15) -0.0032(14) -0.0026(13) C23 0.0318(18) 0.0378(18) 0.0331(19) -0.0053(15) -0.0076(14) -0.0030(14) C24 0.0308(18) 0.0368(18) 0.0332(19) -0.0019(14) -0.0057(14) 0.0004(14) C25 0.0338(19) 0.0334(18) 0.0343(19) -0.0046(14) -0.0053(15) -0.0020(14) C26 0.0267(17) 0.0383(18) 0.0332(19) -0.0049(14) -0.0076(14) -0.0014(13) C27 0.0297(18) 0.0408(19) 0.0338(19) -0.0012(15) -0.0061(14) 0.0000(14) O1 0.047(2) 0.0441(18) 0.079(3) 0.0079(16) 0.0045(17) -0.0062(13) O2 0.0438(17) 0.0420(16) 0.075(2) 0.0171(15) -0.0098(16) -0.0031(13) O3 0.086(3) 0.059(2) 0.0440(19) -0.0010(16) -0.0267(18) 0.0018(18) O4 0.111(4) 0.068(2) 0.043(2) -0.0091(17) -0.024(2) 0.044(2) O5 0.0444(19) 0.077(3) 0.057(2) -0.0252(17) -0.0106(16) -0.0141(16) O6 0.060(2) 0.0522(18) 0.055(2) -0.0144(15) -0.0317(16) 0.0025(15) N1 0.040(2) 0.052(2) 0.070(3) 0.018(2) -0.0077(19) 0.0001(16) C28 0.040(3) 0.109(6) 0.140(8) -0.026(5) -0.016(4) -0.003(3) C29 0.039(4) 0.114(7) 0.212(11) -0.035(7) -0.016(5) 0.000(3) C30 0.041(3) 0.091(5) 0.165(8) 0.060(5) 0.018(4) 0.008(3) C31 0.091(6) 0.148(8) 0.091(6) 0.029(5) 0.031(5) 0.030(5) C32 0.064(4) 0.124(6) 0.076(4) 0.025(4) 0.007(3) 0.022(4) Cd1 0.03501(19) 0.03788(18) 0.0373(2) 0.00893(10) -0.01326(12) -0.00399(10) N2 0.201(5) 0.203(5) 0.203(5) 0.000(3) 0.005(3) -0.001(3) C33 0.201(5) 0.204(5) 0.202(5) -0.002(3) 0.006(3) 0.000(3) C34 0.202(5) 0.205(5) 0.203(5) -0.002(3) 0.006(3) -0.001(3) C35 0.202(5) 0.204(5) 0.202(5) -0.002(3) 0.006(3) -0.002(3) C36 0.203(5) 0.205(5) 0.203(5) -0.002(3) 0.006(2) -0.001(3) C37 0.202(5) 0.204(5) 0.202(5) -0.001(3) 0.007(3) 0.000(3) N2' 0.202(5) 0.205(5) 0.202(5) -0.004(3) 0.008(3) -0.001(3) C33' 0.204(5) 0.206(5) 0.204(5) -0.001(3) 0.007(3) 0.002(3) C34' 0.203(5) 0.204(5) 0.203(5) -0.001(3) 0.007(3) 0.000(3) C35' 0.203(5) 0.204(5) 0.203(5) -0.002(2) 0.006(2) -0.001(2) C36' 0.203(5) 0.205(5) 0.203(5) -0.003(3) 0.007(3) 0.000(3) C37' 0.202(5) 0.204(5) 0.202(5) -0.002(3) 0.007(3) -0.001(3) C38 0.343(7) 0.343(7) 0.343(7) 0.0000(7) 0.0086(7) 0.0000(7) C39 0.343(7) 0.344(7) 0.343(7) 0.0001(9) 0.0085(9) -0.0001(9) C40 0.343(7) 0.343(7) 0.343(7) 0.0000(9) 0.0085(9) -0.0001(8) N3 0.343(7) 0.343(7) 0.343(7) 0.0001(7) 0.0086(7) -0.0001(7) O7 0.343(7) 0.343(7) 0.343(7) -0.0001(9) 0.0085(9) 0.0002(8) O1W 0.089(4) 0.099(4) 0.104(4) 0.004(3) 0.000(3) 0.012(3) O2W 0.072(4) 0.074(4) 0.079(4) 0.002(3) -0.003(3) -0.006(3) O3W 0.088(5) 0.066(4) 0.077(5) -0.011(4) -0.003(4) 0.009(4) O1'W 0.078(3) 0.095(3) 0.109(4) -0.002(3) -0.003(3) 0.016(3) O2'W 0.080(4) 0.073(4) 0.078(4) 0.006(4) 0.007(4) -0.003(3) O3'W 0.094(5) 0.085(4) 0.094(5) 0.000(4) -0.010(4) -0.002(3) O3A 0.093(5) 0.086(5) 0.091(5) 0.002(4) 0.000(4) -0.003(4) O3B 0.088(4) 0.094(4) 0.100(5) 0.005(4) 0.002(4) 0.010(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 C1 O2 1.253(5) . ? C1 O1 1.254(6) . ? C1 C2 1.501(6) . ? C1 Cd1 2.720(4) . ? C2 C3 1.383(6) . ? C2 C7 1.404(6) . ? C3 C4 1.379(5) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 H4 0.9500 . ? C5 C6 1.399(6) . ? C5 C22 1.481(5) . ? C6 C7 1.388(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O3 1.253(6) . ? C8 O4 1.257(6) . ? C8 C9 1.503(6) . ? C8 Cd1 2.756(5) 2_646 ? C9 C14 1.386(6) . ? C9 C10 1.392(6) . ? C10 C11 1.392(6) . ? C10 H10 0.9500 . ? C11 C12 1.401(6) . ? C11 H11 0.9500 . ? C12 C13 1.406(5) . ? C12 C24 1.482(5) . ? C13 C14 1.388(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O6 1.255(6) . ? C15 O5 1.260(6) . ? C15 C16 1.506(5) . ? C15 Cd1 2.731(4) 2_545 ? C16 C21 1.389(7) . ? C16 C17 1.395(7) . ? C17 C18 1.390(6) . ? C17 H17 0.9500 . ? C18 C19 1.396(6) . ? C18 H18 0.9500 . ? C19 C20 1.398(6) . ? C19 C26 1.492(5) . ? C20 C21 1.398(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.393(5) . ? C22 C27 1.402(5) . ? C23 C24 1.394(5) . ? C23 H23 0.9500 . ? C24 C25 1.407(5) . ? C25 C26 1.389(5) . ? C25 H25 0.9500 . ? C26 C27 1.395(5) . ? C27 H27 0.9500 . ? O1 Cd1 2.392(3) . ? O2 Cd1 2.359(3) . ? O3 Cd1 2.350(4) 2_646 ? O4 Cd1 2.455(4) 2_646 ? O5 Cd1 2.483(4) 2_545 ? O6 Cd1 2.307(3) 2_545 ? N1 C28 1.3900 . ? N1 C32 1.3900 . ? N1 Cd1 2.294(3) . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 C31 1.3900 . ? C30 H30A 0.9500 . ? C31 C32 1.3900 . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? Cd1 O6 2.307(3) 2 ? Cd1 O3 2.350(4) 2_656 ? Cd1 O4 2.455(4) 2_656 ? Cd1 O5 2.483(4) 2 ? Cd1 C15 2.731(4) 2 ? Cd1 C8 2.756(5) 2_656 ? N2 C33 1.3900 . ? N2 C37 1.3900 . ? N2 H2A 0.8800 . ? C33 C34 1.3900 . ? C33 H33A 0.9500 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C35 H35A 0.9500 . ? C36 C37 1.3900 . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? N2' C33' 1.3900 . ? N2' C37' 1.3900 . ? N2' H2'A 0.8800 . ? C33' C34' 1.3900 . ? C33' H33B 0.9500 . ? C34' C35' 1.3900 . ? C34' H34B 0.9500 . ? C35' C36' 1.3900 . ? C35' H35B 0.9500 . ? C36' C37' 1.3900 . ? C36' H36B 0.9500 . ? C37' H37B 0.9500 . ? C38 O7 1.225(10) . ? C38 N3 1.345(9) . ? C39 N3 1.394(9) . ? C40 N3 1.395(9) . ? 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 O2 C1 O1 121.5(4) . . ? O2 C1 C2 119.5(4) . . ? O1 C1 C2 118.9(4) . . ? O2 C1 Cd1 60.1(2) . . ? O1 C1 Cd1 61.5(2) . . ? C2 C1 Cd1 176.6(3) . . ? C3 C2 C7 118.8(4) . . ? C3 C2 C1 120.8(4) . . ? C7 C2 C1 120.4(4) . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 121.3(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 118.0(4) . . ? C4 C5 C22 120.3(3) . . ? C6 C5 C22 121.7(4) . . ? C7 C6 C5 120.9(4) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C2 120.1(4) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? O3 C8 O4 121.2(4) . . ? O3 C8 C9 119.0(4) . . ? O4 C8 C9 119.8(4) . . ? O3 C8 Cd1 58.2(2) . 2_646 ? O4 C8 Cd1 63.0(3) . 2_646 ? C9 C8 Cd1 177.1(3) . 2_646 ? C14 C9 C10 119.4(4) . . ? C14 C9 C8 120.2(4) . . ? C10 C9 C8 120.4(4) . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 121.1(4) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 118.2(4) . . ? C11 C12 C24 121.1(4) . . ? C13 C12 C24 120.6(4) . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C9 C14 C13 121.1(4) . . ? C9 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? O6 C15 O5 122.5(4) . . ? O6 C15 C16 118.7(4) . . ? O5 C15 C16 118.8(5) . . ? O6 C15 Cd1 57.2(2) . 2_545 ? O5 C15 Cd1 65.3(2) . 2_545 ? C16 C15 Cd1 175.9(4) . 2_545 ? C21 C16 C17 118.8(4) . . ? C21 C16 C15 121.4(4) . . ? C17 C16 C15 119.8(4) . . ? C18 C17 C16 120.4(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 121.2(4) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C20 118.3(4) . . ? C18 C19 C26 120.7(4) . . ? C20 C19 C26 121.0(4) . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C16 C21 C20 120.8(4) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C23 C22 C27 118.8(3) . . ? C23 C22 C5 120.6(3) . . ? C27 C22 C5 120.5(4) . . ? C22 C23 C24 121.3(3) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C25 118.6(4) . . ? C23 C24 C12 120.0(3) . . ? C25 C24 C12 121.4(3) . . ? C26 C25 C24 121.4(3) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 118.7(3) . . ? C25 C26 C19 120.9(3) . . ? C27 C26 C19 120.4(4) . . ? C26 C27 C22 121.3(4) . . ? C26 C27 H27 119.3 . . ? C22 C27 H27 119.3 . . ? C1 O1 Cd1 91.0(3) . . ? C1 O2 Cd1 92.5(3) . . ? C8 O3 Cd1 94.9(3) . 2_646 ? C8 O4 Cd1 89.9(3) . 2_646 ? C15 O5 Cd1 87.3(3) . 2_545 ? C15 O6 Cd1 95.6(3) . 2_545 ? C28 N1 C32 120.0 . . ? C28 N1 Cd1 120.0(2) . . ? C32 N1 Cd1 119.1(2) . . ? C29 C28 N1 120.0 . . ? C29 C28 H28A 120.0 . . ? N1 C28 H28A 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 N1 120.0 . . ? C31 C32 H32A 120.0 . . ? N1 C32 H32A 120.0 . . ? N1 Cd1 O6 120.10(13) . 2 ? N1 Cd1 O3 91.33(14) . 2_656 ? O6 Cd1 O3 83.48(13) 2 2_656 ? N1 Cd1 O2 139.95(12) . . ? O6 Cd1 O2 88.92(12) 2 . ? O3 Cd1 O2 120.94(14) 2_656 . ? N1 Cd1 O1 85.70(12) . . ? O6 Cd1 O1 134.53(12) 2 . ? O3 Cd1 O1 136.43(13) 2_656 . ? O2 Cd1 O1 54.84(11) . . ? N1 Cd1 O4 92.79(16) . 2_656 ? O6 Cd1 O4 127.65(16) 2 2_656 ? O3 Cd1 O4 54.07(12) 2_656 2_656 ? O2 Cd1 O4 88.96(13) . 2_656 ? O1 Cd1 O4 82.63(13) . 2_656 ? N1 Cd1 O5 86.53(13) . 2 ? O6 Cd1 O5 54.65(13) 2 2 ? O3 Cd1 O5 128.40(12) 2_656 2 ? O2 Cd1 O5 89.98(13) . 2 ? O1 Cd1 O5 94.85(13) . 2 ? O4 Cd1 O5 177.43(13) 2_656 2 ? N1 Cd1 C1 113.03(13) . . ? O6 Cd1 C1 113.02(13) 2 . ? O3 Cd1 C1 133.45(14) 2_656 . ? O2 Cd1 C1 27.40(12) . . ? O1 Cd1 C1 27.46(12) . . ? O4 Cd1 C1 84.44(12) 2_656 . ? O5 Cd1 C1 93.54(13) 2 . ? N1 Cd1 C15 104.60(13) . 2 ? O6 Cd1 C15 27.20(14) 2 2 ? O3 Cd1 C15 106.61(14) 2_656 2 ? O2 Cd1 C15 89.17(12) . 2 ? O1 Cd1 C15 116.20(14) . 2 ? O4 Cd1 C15 154.83(17) 2_656 2 ? O5 Cd1 C15 27.45(14) 2 2 ? C1 Cd1 C15 104.62(13) . 2 ? N1 Cd1 C8 92.28(14) . 2_656 ? O6 Cd1 C8 106.14(14) 2 2_656 ? O3 Cd1 C8 26.93(13) 2_656 2_656 ? O2 Cd1 C8 106.26(14) . 2_656 ? O1 Cd1 C8 109.66(14) . 2_656 ? O4 Cd1 C8 27.14(13) 2_656 2_656 ? O5 Cd1 C8 155.32(14) 2 2_656 ? C1 Cd1 C8 109.48(14) . 2_656 ? C15 Cd1 C8 131.87(16) 2 2_656 ? C33 N2 C37 120.0 . . ? C33 N2 H2A 120.0 . . ? C37 N2 H2A 120.0 . . ? N2 C33 C34 120.0 . . ? N2 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 N2 120.0 . . ? C36 C37 H37A 120.0 . . ? N2 C37 H37A 120.0 . . ? C33' N2' C37' 120.0 . . ? C33' N2' H2'A 120.0 . . ? C37' N2' H2'A 120.0 . . ? C34' C33' N2' 120.0 . . ? C34' C33' H33B 120.0 . . ? N2' C33' H33B 120.0 . . ? C33' C34' C35' 120.0 . . ? C33' C34' H34B 120.0 . . ? C35' C34' H34B 120.0 . . ? C36' C35' C34' 120.0 . . ? C36' C35' H35B 120.0 . . ? C34' C35' H35B 120.0 . . ? C35' C36' C37' 120.0 . . ? C35' C36' H36B 120.0 . . ? C37' C36' H36B 120.0 . . ? C36' C37' N2' 120.0 . . ? C36' C37' H37B 120.0 . . ? N2' C37' H37B 120.0 . . ? O7 C38 N3 126.8(17) . . ? C38 N3 C39 118.9(14) . . ? C38 N3 C40 122.9(15) . . ? C39 N3 C40 118.2(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -145.9(4) . . . . ? O1 C1 C2 C3 33.6(6) . . . . ? Cd1 C1 C2 C3 -64(6) . . . . ? O2 C1 C2 C7 33.9(7) . . . . ? O1 C1 C2 C7 -146.7(5) . . . . ? Cd1 C1 C2 C7 116(5) . . . . ? C7 C2 C3 C4 -1.0(7) . . . . ? C1 C2 C3 C4 178.8(4) . . . . ? C2 C3 C4 C5 2.6(7) . . . . ? C3 C4 C5 C6 -1.5(6) . . . . ? C3 C4 C5 C22 175.3(4) . . . . ? C4 C5 C6 C7 -1.1(7) . . . . ? C22 C5 C6 C7 -177.8(4) . . . . ? C5 C6 C7 C2 2.6(8) . . . . ? C3 C2 C7 C6 -1.6(7) . . . . ? C1 C2 C7 C6 178.6(4) . . . . ? O3 C8 C9 C14 -7.3(7) . . . . ? O4 C8 C9 C14 171.9(5) . . . . ? Cd1 C8 C9 C14 8(7) 2_646 . . . ? O3 C8 C9 C10 172.4(5) . . . . ? O4 C8 C9 C10 -8.4(8) . . . . ? Cd1 C8 C9 C10 -172(7) 2_646 . . . ? C14 C9 C10 C11 1.3(7) . . . . ? C8 C9 C10 C11 -178.4(4) . . . . ? C9 C10 C11 C12 -0.1(7) . . . . ? C10 C11 C12 C13 -1.0(6) . . . . ? C10 C11 C12 C24 176.1(4) . . . . ? C11 C12 C13 C14 1.0(6) . . . . ? C24 C12 C13 C14 -176.2(4) . . . . ? C10 C9 C14 C13 -1.4(7) . . . . ? C8 C9 C14 C13 178.3(4) . . . . ? C12 C13 C14 C9 0.2(7) . . . . ? O6 C15 C16 C21 166.5(4) . . . . ? O5 C15 C16 C21 -13.2(6) . . . . ? Cd1 C15 C16 C21 172(4) 2_545 . . . ? O6 C15 C16 C17 -13.8(6) . . . . ? O5 C15 C16 C17 166.5(4) . . . . ? Cd1 C15 C16 C17 -8(4) 2_545 . . . ? C21 C16 C17 C18 -2.3(7) . . . . ? C15 C16 C17 C18 177.9(4) . . . . ? C16 C17 C18 C19 0.0(8) . . . . ? C17 C18 C19 C20 1.6(7) . . . . ? C17 C18 C19 C26 -179.5(4) . . . . ? C18 C19 C20 C21 -0.8(6) . . . . ? C26 C19 C20 C21 -179.7(4) . . . . ? C17 C16 C21 C20 3.1(6) . . . . ? C15 C16 C21 C20 -177.1(4) . . . . ? C19 C20 C21 C16 -1.6(6) . . . . ? C4 C5 C22 C23 41.6(6) . . . . ? C6 C5 C22 C23 -141.8(4) . . . . ? C4 C5 C22 C27 -134.4(4) . . . . ? C6 C5 C22 C27 42.2(6) . . . . ? C27 C22 C23 C24 0.5(6) . . . . ? C5 C22 C23 C24 -175.6(4) . . . . ? C22 C23 C24 C25 0.4(6) . . . . ? C22 C23 C24 C12 177.0(4) . . . . ? C11 C12 C24 C23 -139.9(4) . . . . ? C13 C12 C24 C23 37.1(6) . . . . ? C11 C12 C24 C25 36.5(6) . . . . ? C13 C12 C24 C25 -146.4(4) . . . . ? C23 C24 C25 C26 -0.7(6) . . . . ? C12 C24 C25 C26 -177.2(4) . . . . ? C24 C25 C26 C27 0.0(6) . . . . ? C24 C25 C26 C19 178.4(3) . . . . ? C18 C19 C26 C25 -148.8(4) . . . . ? C20 C19 C26 C25 30.2(6) . . . . ? C18 C19 C26 C27 29.6(6) . . . . ? C20 C19 C26 C27 -151.5(4) . . . . ? C25 C26 C27 C22 0.9(6) . . . . ? C19 C26 C27 C22 -177.5(3) . . . . ? C23 C22 C27 C26 -1.2(6) . . . . ? C5 C22 C27 C26 174.9(4) . . . . ? O2 C1 O1 Cd1 3.3(5) . . . . ? C2 C1 O1 Cd1 -176.2(4) . . . . ? O1 C1 O2 Cd1 -3.3(5) . . . . ? C2 C1 O2 Cd1 176.1(4) . . . . ? O4 C8 O3 Cd1 -0.1(6) . . . 2_646 ? C9 C8 O3 Cd1 179.1(4) . . . 2_646 ? O3 C8 O4 Cd1 0.1(6) . . . 2_646 ? C9 C8 O4 Cd1 -179.1(4) . . . 2_646 ? O6 C15 O5 Cd1 0.8(4) . . . 2_545 ? C16 C15 O5 Cd1 -179.6(3) . . . 2_545 ? O5 C15 O6 Cd1 -0.9(5) . . . 2_545 ? C16 C15 O6 Cd1 179.5(3) . . . 2_545 ? C32 N1 C28 C29 0.0 . . . . ? Cd1 N1 C28 C29 168.8(2) . . . . ? N1 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 N1 0.0 . . . . ? C28 N1 C32 C31 0.0 . . . . ? Cd1 N1 C32 C31 -168.9(2) . . . . ? C28 N1 Cd1 O6 109.9(2) . . . 2 ? C32 N1 Cd1 O6 -81.2(3) . . . 2 ? C28 N1 Cd1 O3 26.6(2) . . . 2_656 ? C32 N1 Cd1 O3 -164.4(2) . . . 2_656 ? C28 N1 Cd1 O2 -119.1(3) . . . . ? C32 N1 Cd1 O2 49.8(3) . . . . ? C28 N1 Cd1 O1 -109.8(2) . . . . ? C32 N1 Cd1 O1 59.1(2) . . . . ? C28 N1 Cd1 O4 -27.4(2) . . . 2_656 ? C32 N1 Cd1 O4 141.5(2) . . . 2_656 ? C28 N1 Cd1 O5 155.0(2) . . . 2 ? C32 N1 Cd1 O5 -36.0(2) . . . 2 ? C28 N1 Cd1 C1 -112.6(3) . . . . ? C32 N1 Cd1 C1 56.3(3) . . . . ? C28 N1 Cd1 C15 134.2(2) . . . 2 ? C32 N1 Cd1 C15 -56.9(3) . . . 2 ? C28 N1 Cd1 C8 -0.3(3) . . . 2_656 ? C32 N1 Cd1 C8 168.6(2) . . . 2_656 ? C1 O2 Cd1 N1 13.2(4) . . . . ? C1 O2 Cd1 O6 152.4(3) . . . 2 ? C1 O2 Cd1 O3 -125.9(3) . . . 2_656 ? C1 O2 Cd1 O1 1.8(3) . . . . ? C1 O2 Cd1 O4 -79.9(3) . . . 2_656 ? C1 O2 Cd1 O5 97.8(3) . . . 2 ? C1 O2 Cd1 C15 125.2(3) . . . 2 ? C1 O2 Cd1 C8 -101.1(3) . . . 2_656 ? C1 O1 Cd1 N1 -174.5(3) . . . . ? C1 O1 Cd1 O6 -45.3(4) . . . 2 ? C1 O1 Cd1 O3 98.1(3) . . . 2_656 ? C1 O1 Cd1 O2 -1.8(3) . . . . ? C1 O1 Cd1 O4 92.1(3) . . . 2_656 ? C1 O1 Cd1 O5 -88.4(3) . . . 2 ? C1 O1 Cd1 C15 -70.3(3) . . . 2 ? C1 O1 Cd1 C8 94.6(3) . . . 2_656 ? O2 C1 Cd1 N1 -170.8(3) . . . . ? O1 C1 Cd1 N1 6.0(3) . . . . ? C2 C1 Cd1 N1 105(5) . . . . ? O2 C1 Cd1 O6 -30.2(3) . . . 2 ? O1 C1 Cd1 O6 146.6(3) . . . 2 ? C2 C1 Cd1 O6 -114(5) . . . 2 ? O2 C1 Cd1 O3 73.2(3) . . . 2_656 ? O1 C1 Cd1 O3 -110.0(3) . . . 2_656 ? C2 C1 Cd1 O3 -11(5) . . . 2_656 ? O1 C1 Cd1 O2 176.8(5) . . . . ? C2 C1 Cd1 O2 -84(5) . . . . ? O2 C1 Cd1 O1 -176.8(5) . . . . ? C2 C1 Cd1 O1 99(5) . . . . ? O2 C1 Cd1 O4 98.5(3) . . . 2_656 ? O1 C1 Cd1 O4 -84.7(3) . . . 2_656 ? C2 C1 Cd1 O4 15(5) . . . 2_656 ? O2 C1 Cd1 O5 -83.1(3) . . . 2 ? O1 C1 Cd1 O5 93.7(3) . . . 2 ? C2 C1 Cd1 O5 -167(5) . . . 2 ? O2 C1 Cd1 C15 -57.6(3) . . . 2 ? O1 C1 Cd1 C15 119.2(3) . . . 2 ? C2 C1 Cd1 C15 -142(5) . . . 2 ? O2 C1 Cd1 C8 87.9(3) . . . 2_656 ? O1 C1 Cd1 C8 -95.3(3) . . . 2_656 ? C2 C1 Cd1 C8 4(5) . . . 2_656 ? C37 N2 C33 C34 0.0 . . . . ? N2 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 N2 0.0 . . . . ? C33 N2 C37 C36 0.0 . . . . ? C37' N2' C33' C34' 0.0 . . . . ? N2' C33' C34' C35' 0.0 . . . . ? C33' C34' C35' C36' 0.0 . . . . ? C34' C35' C36' C37' 0.0 . . . . ? C35' C36' C37' N2' 0.0 . . . . ? C33' N2' C37' C36' 0.0 . . . . ? O7 C38 N3 C39 0.00(3) . . . . ? O7 C38 N3 C40 180.000(16) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.946 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.122 # start Validation Reply Form _vrf_PLAT430_2 ; PROBLEM: Short Inter D...A Contact RESPONSE: Three water molecules, half DMF molecule and one pyridinium cation are disorderd. ; # end Validation Reply Form # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 825084' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C64 H38 N2 O12 Cd2 ) 2(C10 N2 H8) (C3 H7 N O) 19(H2 O) Cd ' _chemical_formula_sum 'C87 H99 N7 O32 Cd3' _chemical_formula_weight 2091.93 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 16.8416(6) _cell_length_b 29.9444(9) _cell_length_c 15.9876(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.0760(10) _cell_angle_gamma 90.00 _cell_volume 7982.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2518 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 31.42 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4280 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7060 _exptl_absorpt_correction_T_max 0.7340 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% . _diffrn_reflns_number 54211 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17712 _reflns_number_gt 13131 _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. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of highly disordered solvent molecules and ions (4,4'-bipy, water molecules, DMF molecules and Cd ions), thereby a final model based only on the ordered part of the crystal structure was obtained. ; _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^)+(0.1081P)^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 17712 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1775 _refine_ls_wR_factor_gt 0.1610 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2915(3) 0.33377(11) -0.1286(2) 0.0346(9) Uani 1 1 d . . . C2 C 0.2543(2) 0.35719(12) -0.2083(2) 0.0334(8) Uani 1 1 d U . . C3 C 0.1775(3) 0.37329(16) -0.2160(2) 0.0519(11) Uani 1 1 d U . . H3 H 0.1461 0.3687 -0.1718 0.062 Uiso 1 1 calc R . . C4 C 0.1456(3) 0.39627(17) -0.2882(3) 0.0561(12) Uani 1 1 d U . . H4 H 0.0934 0.4088 -0.2910 0.067 Uiso 1 1 calc R . . C5 C 0.1866(3) 0.40151(12) -0.3552(2) 0.0341(8) Uani 1 1 d U . . C6 C 0.2602(4) 0.3826(2) -0.3493(3) 0.0767(17) Uani 1 1 d U . . H6 H 0.2885 0.3838 -0.3967 0.092 Uiso 1 1 calc R . . C7 C 0.2959(4) 0.3614(2) -0.2750(3) 0.0805(17) Uani 1 1 d U . . H7 H 0.3490 0.3501 -0.2713 0.097 Uiso 1 1 calc R . . C8 C 0.1117(3) 0.68820(13) -0.5168(2) 0.0372(9) Uani 1 1 d . . . C9 C 0.1183(3) 0.63792(12) -0.5206(2) 0.0341(8) Uani 1 1 d . . . C10 C 0.1781(3) 0.61520(13) -0.4681(2) 0.0391(9) Uani 1 1 d . . . H10 H 0.2183 0.6317 -0.4335 0.047 Uiso 1 1 calc R . . C11 C 0.1799(3) 0.56922(12) -0.4655(2) 0.0357(9) Uani 1 1 d . . . H11 H 0.2206 0.5546 -0.4282 0.043 Uiso 1 1 calc R . . C12 C 0.1229(2) 0.54362(12) -0.5170(2) 0.0305(8) Uani 1 1 d . . . C13 C 0.0637(3) 0.56690(12) -0.5719(2) 0.0397(9) Uani 1 1 d . . . H13 H 0.0251 0.5507 -0.6089 0.048 Uiso 1 1 calc R . . C14 C 0.0615(3) 0.61307(13) -0.5719(2) 0.0409(10) Uani 1 1 d . . . H14 H 0.0203 0.6281 -0.6079 0.049 Uiso 1 1 calc R . . C15 C -0.0391(3) 0.32198(12) -0.8807(2) 0.0374(9) Uani 1 1 d . . . C16 C -0.0046(3) 0.34743(12) -0.8030(2) 0.0353(9) Uani 1 1 d . . . C17 C 0.0592(3) 0.37661(16) -0.8055(2) 0.0558(13) Uani 1 1 d . . . H17 H 0.0819 0.3798 -0.8563 0.067 Uiso 1 1 calc R . . C18 C 0.0905(3) 0.40125(16) -0.7344(3) 0.0535(12) Uani 1 1 d . . . H18 H 0.1330 0.4218 -0.7376 0.064 Uiso 1 1 calc R . . C19 C 0.0595(3) 0.39579(11) -0.6590(2) 0.0332(8) Uani 1 1 d . . . C20 C -0.0010(3) 0.36572(14) -0.6555(2) 0.0490(11) Uani 1 1 d . . . H20 H -0.0202 0.3606 -0.6031 0.059 Uiso 1 1 calc R . . C21 C -0.0353(3) 0.34237(14) -0.7270(2) 0.0475(11) Uani 1 1 d . . . H21 H -0.0795 0.3230 -0.7240 0.057 Uiso 1 1 calc R . . C22 C 0.1522(2) 0.42493(12) -0.4349(2) 0.0314(8) Uani 1 1 d . . . C23 C 0.1522(2) 0.47138(12) -0.4392(2) 0.0326(8) Uani 1 1 d . . . H23 H 0.1723 0.4881 -0.3903 0.039 Uiso 1 1 calc R . . C24 C 0.1232(2) 0.49385(12) -0.5138(2) 0.0318(8) Uani 1 1 d . . . C25 C 0.0948(2) 0.46860(11) -0.5858(2) 0.0308(8) Uani 1 1 d . . . H25 H 0.0763 0.4834 -0.6375 0.037 Uiso 1 1 calc R . . C26 C 0.0932(2) 0.42210(12) -0.5825(2) 0.0326(8) Uani 1 1 d . . . C27 C 0.1214(2) 0.40023(12) -0.5062(2) 0.0331(8) Uani 1 1 d . . . H27 H 0.1194 0.3686 -0.5032 0.040 Uiso 1 1 calc R . . C28 C 0.4391(3) 0.35006(14) 0.1253(2) 0.0417(10) Uani 1 1 d . . . C29 C 0.4807(3) 0.37467(12) 0.2002(2) 0.0388(9) Uani 1 1 d . . . C30 C 0.4432(3) 0.41046(13) 0.2350(2) 0.0397(9) Uani 1 1 d . . . H30 H 0.3920 0.4203 0.2088 0.048 Uiso 1 1 calc R . . C31 C 0.4801(3) 0.43186(13) 0.3077(2) 0.0383(9) Uani 1 1 d . . . H31 H 0.4542 0.4564 0.3302 0.046 Uiso 1 1 calc R . . C32 C 0.5549(3) 0.41753(12) 0.3479(2) 0.0361(9) Uani 1 1 d . . . C33 C 0.5918(3) 0.38186(13) 0.3122(3) 0.0521(12) Uani 1 1 d . . . H33 H 0.6431 0.3719 0.3379 0.063 Uiso 1 1 calc R . . C34 C 0.5550(3) 0.36077(14) 0.2400(3) 0.0518(12) Uani 1 1 d . . . H34 H 0.5810 0.3364 0.2174 0.062 Uiso 1 1 calc R . . C35 C 0.8074(3) 0.33404(15) 0.8615(3) 0.0493(11) Uani 1 1 d . . . C36 C 0.7691(3) 0.36003(14) 0.7871(3) 0.0467(11) Uani 1 1 d . . . C37 C 0.7988(3) 0.40207(15) 0.7694(3) 0.0586(13) Uani 1 1 d . . . H37 H 0.8434 0.4142 0.8052 0.070 Uiso 1 1 calc R . . C38 C 0.7629(3) 0.42672(15) 0.6987(3) 0.0570(13) Uani 1 1 d . . . H38 H 0.7825 0.4556 0.6882 0.068 Uiso 1 1 calc R . . C39 C 0.6990(3) 0.40895(13) 0.6444(2) 0.0412(10) Uani 1 1 d . . . C40 C 0.6776(4) 0.36591(17) 0.6575(4) 0.084(2) Uani 1 1 d . . . H40 H 0.6381 0.3520 0.6176 0.101 Uiso 1 1 calc R . . C41 C 0.7117(4) 0.34204(17) 0.7273(4) 0.087(2) Uani 1 1 d . . . H41 H 0.6948 0.3121 0.7341 0.104 Uiso 1 1 calc R . . C42 C 0.6328(3) 0.70122(13) 0.5232(2) 0.0381(9) Uani 1 1 d . . . C43 C 0.6265(2) 0.65122(12) 0.5230(2) 0.0334(8) Uani 1 1 d . . . C44 C 0.6884(3) 0.62598(12) 0.5694(2) 0.0359(9) Uani 1 1 d . . . H44 H 0.7309 0.6406 0.6041 0.043 Uiso 1 1 calc R . . C45 C 0.6871(2) 0.57991(12) 0.5643(2) 0.0353(8) Uani 1 1 d . . . H45 H 0.7290 0.5631 0.5956 0.042 Uiso 1 1 calc R . . C46 C 0.6251(2) 0.55764(11) 0.5136(2) 0.0302(8) Uani 1 1 d . . . C47 C 0.5636(3) 0.58284(12) 0.4697(2) 0.0366(9) Uani 1 1 d . . . H47 H 0.5205 0.5682 0.4357 0.044 Uiso 1 1 calc R . . C48 C 0.5643(3) 0.62877(12) 0.4750(2) 0.0363(8) Uani 1 1 d . . . H48 H 0.5212 0.6453 0.4450 0.044 Uiso 1 1 calc R . . C49 C 0.5933(3) 0.43959(12) 0.4269(2) 0.0364(9) Uani 1 1 d . . . C50 C 0.6280(2) 0.41474(12) 0.4958(2) 0.0373(9) Uani 1 1 d . . . H50 H 0.6290 0.3831 0.4918 0.045 Uiso 1 1 calc R . . C51 C 0.6615(2) 0.43543(12) 0.5712(2) 0.0349(8) Uani 1 1 d . . . C52 C 0.6587(2) 0.48181(12) 0.5755(2) 0.0330(8) Uani 1 1 d . . . H52 H 0.6799 0.4961 0.6268 0.040 Uiso 1 1 calc R . . C53 C 0.6262(2) 0.50771(12) 0.5081(2) 0.0305(8) Uani 1 1 d . . . C54 C 0.5920(2) 0.48655(12) 0.4338(2) 0.0348(8) Uani 1 1 d . . . H54 H 0.5676 0.5040 0.3875 0.042 Uiso 1 1 calc R . . C55 C 0.2714(4) 0.2929(2) 0.1821(3) 0.0784(17) Uani 1 1 d U . . H55 H 0.3117 0.3147 0.1982 0.094 Uiso 1 1 calc R . . C56 C 0.2145(4) 0.2846(2) 0.2365(3) 0.0718(16) Uani 1 1 d U . . H56 H 0.2162 0.3013 0.2873 0.086 Uiso 1 1 calc R . . C57 C 0.1580(3) 0.25354(12) 0.2175(2) 0.0358(8) Uani 1 1 d U . . C58 C 0.1553(3) 0.23194(17) 0.1420(3) 0.0571(12) Uani 1 1 d U . . H58 H 0.1142 0.2108 0.1245 0.069 Uiso 1 1 calc R . . C59 C 0.2137(3) 0.24148(17) 0.0909(3) 0.0549(12) Uani 1 1 d U . . H59 H 0.2124 0.2253 0.0396 0.066 Uiso 1 1 calc R . . C60 C 0.0526(3) 0.24918(16) 0.4108(2) 0.0469(11) Uani 1 1 d . . . H60 H 0.0640 0.2565 0.4690 0.056 Uiso 1 1 calc R . . C61 C 0.1117(3) 0.25585(15) 0.3602(2) 0.0453(10) Uani 1 1 d . . . H61 H 0.1624 0.2675 0.3839 0.054 Uiso 1 1 calc R . . C62 C 0.0970(3) 0.24545(12) 0.2745(2) 0.0370(9) Uani 1 1 d . . . C63 C 0.0212(3) 0.22789(14) 0.2444(2) 0.0442(10) Uani 1 1 d . . . H63 H 0.0082 0.2199 0.1866 0.053 Uiso 1 1 calc R . . C64 C -0.0343(3) 0.22221(14) 0.2990(2) 0.0448(10) Uani 1 1 d . . . H64 H -0.0853 0.2102 0.2776 0.054 Uiso 1 1 calc R . . Cd1 Cd 0.357057(18) 0.290605(8) 0.011872(15) 0.03153(10) Uani 1 1 d . . . Cd2 Cd 0.107280(18) 0.777445(8) -0.479437(16) 0.03241(10) Uani 1 1 d . . . N1 N 0.2717(2) 0.27200(10) 0.10981(19) 0.0385(8) Uani 1 1 d U . . N2 N -0.0192(2) 0.23297(11) 0.38156(18) 0.0371(7) Uani 1 1 d . . . O1 O 0.24812(17) 0.32493(9) -0.07247(15) 0.0364(6) Uani 1 1 d . . . O2 O 0.36427(18) 0.32293(9) -0.11989(15) 0.0418(7) Uani 1 1 d . . . O3 O 0.1709(2) 0.71022(8) -0.4826(2) 0.0476(8) Uani 1 1 d . . . O4 O 0.0468(2) 0.70650(8) -0.54498(17) 0.0446(8) Uani 1 1 d . . . O5 O 0.00240(19) 0.31627(9) -0.93895(16) 0.0419(7) Uani 1 1 d . . . O6 O -0.1097(2) 0.30703(9) -0.88577(16) 0.0442(7) Uani 1 1 d . . . O7 O 0.3741(2) 0.36469(10) 0.08680(17) 0.0460(7) Uani 1 1 d . . . O8 O 0.4681(2) 0.31355(11) 0.1043(2) 0.0627(10) Uani 1 1 d . . . O9 O 0.7854(2) 0.29448(12) 0.8710(2) 0.0740(12) Uani 1 1 d . . . O10 O 0.8643(2) 0.35123(10) 0.9114(2) 0.0609(9) Uani 1 1 d . . . O11 O 0.6925(2) 0.72030(8) 0.56090(17) 0.0418(7) Uani 1 1 d . . . O12 O 0.5749(2) 0.72315(9) 0.4801(2) 0.0514(8) 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 C1 0.047(3) 0.0286(17) 0.0280(17) 0.0009(14) 0.0030(16) 0.0008(16) C2 0.038(2) 0.0361(17) 0.0253(15) 0.0031(14) 0.0005(14) 0.0039(15) C3 0.048(3) 0.076(3) 0.0324(18) 0.0162(19) 0.0088(17) 0.013(2) C4 0.048(3) 0.080(3) 0.040(2) 0.017(2) 0.0084(19) 0.021(2) C5 0.042(2) 0.0336(17) 0.0258(16) 0.0010(14) 0.0007(15) 0.0037(15) C6 0.071(3) 0.113(4) 0.051(2) 0.036(3) 0.024(2) 0.035(3) C7 0.069(3) 0.113(4) 0.063(3) 0.040(3) 0.024(2) 0.038(3) C8 0.046(3) 0.039(2) 0.0264(17) -0.0035(15) 0.0042(16) -0.0005(18) C9 0.043(3) 0.0310(18) 0.0290(17) 0.0001(14) 0.0064(16) 0.0013(16) C10 0.042(3) 0.0379(19) 0.0369(19) -0.0029(16) 0.0027(17) -0.0029(17) C11 0.038(2) 0.0337(18) 0.0322(18) -0.0016(15) -0.0057(16) 0.0029(16) C12 0.031(2) 0.0317(17) 0.0278(16) -0.0018(14) 0.0013(14) 0.0020(14) C13 0.050(3) 0.0334(19) 0.0325(19) -0.0019(15) -0.0062(17) 0.0048(17) C14 0.046(3) 0.0351(19) 0.039(2) -0.0020(16) -0.0054(18) 0.0093(17) C15 0.048(3) 0.0308(18) 0.0318(18) 0.0001(15) 0.0014(17) -0.0009(17) C16 0.046(3) 0.0305(17) 0.0282(17) -0.0022(14) -0.0004(16) -0.0035(16) C17 0.075(4) 0.067(3) 0.0291(19) -0.013(2) 0.019(2) -0.024(3) C18 0.064(4) 0.060(3) 0.038(2) -0.009(2) 0.012(2) -0.027(2) C19 0.046(3) 0.0288(17) 0.0244(16) -0.0003(14) 0.0039(15) 0.0012(16) C20 0.067(4) 0.052(2) 0.0313(19) -0.0060(18) 0.017(2) -0.015(2) C21 0.064(3) 0.046(2) 0.035(2) -0.0055(17) 0.014(2) -0.021(2) C22 0.037(2) 0.0352(18) 0.0217(15) 0.0042(14) 0.0026(14) 0.0040(15) C23 0.036(2) 0.0351(18) 0.0251(16) -0.0025(14) 0.0000(15) 0.0004(15) C24 0.039(2) 0.0287(17) 0.0274(17) -0.0010(13) 0.0036(15) 0.0020(15) C25 0.035(2) 0.0305(17) 0.0266(16) 0.0029(14) 0.0029(14) 0.0001(15) C26 0.037(2) 0.0349(18) 0.0265(16) -0.0011(14) 0.0047(15) 0.0005(15) C27 0.043(2) 0.0274(17) 0.0284(17) 0.0019(14) 0.0024(16) 0.0013(15) C28 0.043(3) 0.045(2) 0.036(2) -0.0007(17) 0.0009(18) -0.0111(18) C29 0.043(3) 0.0341(19) 0.0364(19) -0.0047(16) -0.0048(17) -0.0066(16) C30 0.038(3) 0.043(2) 0.0359(19) 0.0002(16) -0.0045(17) -0.0021(17) C31 0.043(3) 0.0377(19) 0.0332(18) -0.0007(15) 0.0006(17) 0.0014(17) C32 0.039(2) 0.0313(18) 0.0354(19) -0.0024(15) -0.0032(16) -0.0031(16) C33 0.052(3) 0.040(2) 0.058(3) -0.012(2) -0.016(2) 0.006(2) C34 0.053(3) 0.042(2) 0.054(3) -0.016(2) -0.011(2) 0.008(2) C35 0.045(3) 0.052(2) 0.049(2) 0.010(2) -0.002(2) 0.009(2) C36 0.046(3) 0.045(2) 0.045(2) 0.0080(19) -0.0060(19) 0.0101(19) C37 0.063(4) 0.050(2) 0.056(3) 0.007(2) -0.016(2) -0.009(2) C38 0.060(4) 0.043(2) 0.063(3) 0.010(2) -0.009(2) -0.007(2) C39 0.046(3) 0.0358(19) 0.038(2) 0.0025(16) -0.0052(18) 0.0061(17) C40 0.109(6) 0.051(3) 0.075(4) 0.017(3) -0.049(4) -0.026(3) C41 0.103(5) 0.049(3) 0.091(4) 0.033(3) -0.043(4) -0.030(3) C42 0.045(3) 0.0332(19) 0.0364(19) -0.0003(16) 0.0078(17) -0.0001(17) C43 0.038(2) 0.0291(17) 0.0329(18) 0.0009(14) 0.0046(16) -0.0031(15) C44 0.039(2) 0.0354(19) 0.0318(18) -0.0029(15) -0.0006(16) -0.0075(16) C45 0.034(2) 0.0378(19) 0.0320(18) 0.0024(15) -0.0033(15) -0.0026(16) C46 0.035(2) 0.0293(17) 0.0263(16) -0.0025(13) 0.0043(14) -0.0029(14) C47 0.034(2) 0.0370(19) 0.0367(19) 0.0009(16) -0.0035(16) -0.0045(16) C48 0.033(2) 0.0354(19) 0.0398(19) 0.0014(16) 0.0017(16) 0.0029(15) C49 0.036(2) 0.0345(18) 0.0372(19) -0.0011(15) -0.0011(16) 0.0009(16) C50 0.041(3) 0.0278(17) 0.040(2) -0.0011(15) -0.0060(17) 0.0007(15) C51 0.032(2) 0.0353(18) 0.0357(19) 0.0012(15) -0.0023(16) -0.0031(15) C52 0.032(2) 0.0340(18) 0.0310(17) -0.0030(14) -0.0036(15) 0.0008(15) C53 0.028(2) 0.0299(17) 0.0327(17) -0.0021(14) 0.0012(15) -0.0042(14) C54 0.040(2) 0.0332(18) 0.0304(17) 0.0014(14) 0.0016(16) -0.0012(16) C55 0.095(4) 0.092(3) 0.054(3) -0.023(2) 0.030(3) -0.046(3) C56 0.087(4) 0.087(3) 0.047(2) -0.021(2) 0.027(2) -0.037(3) C57 0.043(2) 0.0379(18) 0.0249(15) -0.0001(14) -0.0001(15) 0.0003(16) C58 0.055(3) 0.077(3) 0.040(2) -0.015(2) 0.0095(19) -0.019(2) C59 0.052(3) 0.075(3) 0.038(2) -0.019(2) 0.0056(19) -0.015(2) C60 0.041(3) 0.073(3) 0.0246(17) -0.0088(18) -0.0020(17) -0.003(2) C61 0.043(3) 0.063(3) 0.0281(18) -0.0026(18) -0.0018(17) -0.003(2) C62 0.052(3) 0.0345(18) 0.0232(16) 0.0012(15) 0.0010(16) 0.0022(17) C63 0.061(3) 0.046(2) 0.0247(18) -0.0031(16) 0.0042(18) -0.010(2) C64 0.053(3) 0.051(2) 0.0298(19) -0.0030(17) 0.0000(18) -0.012(2) Cd1 0.04008(19) 0.02951(15) 0.02323(14) 0.00090(9) -0.00173(11) 0.00068(11) Cd2 0.04050(19) 0.02912(15) 0.02595(15) -0.00009(10) -0.00110(11) 0.00189(11) N1 0.050(2) 0.0378(16) 0.0270(14) -0.0010(13) 0.0031(14) -0.0015(14) N2 0.044(2) 0.0413(17) 0.0261(14) -0.0006(13) 0.0038(14) 0.0014(15) O1 0.0396(18) 0.0429(14) 0.0264(12) 0.0046(11) 0.0032(11) 0.0038(12) O2 0.0415(19) 0.0526(16) 0.0306(13) 0.0080(12) 0.0028(12) 0.0054(13) O3 0.050(2) 0.0294(13) 0.0612(19) -0.0063(13) 0.0006(16) -0.0020(12) O4 0.063(2) 0.0318(14) 0.0353(14) -0.0009(11) -0.0053(14) 0.0113(13) O5 0.0465(19) 0.0484(16) 0.0313(13) -0.0078(12) 0.0066(12) -0.0038(13) O6 0.051(2) 0.0439(15) 0.0368(14) -0.0078(12) 0.0039(13) -0.0073(14) O7 0.046(2) 0.0485(16) 0.0389(14) -0.0048(13) -0.0091(13) -0.0059(14) O8 0.066(3) 0.0504(18) 0.065(2) -0.0265(16) -0.0127(17) 0.0046(16) O9 0.066(3) 0.064(2) 0.082(3) 0.0366(19) -0.025(2) -0.0133(18) O10 0.070(3) 0.0515(18) 0.0536(18) 0.0089(15) -0.0189(17) 0.0096(17) O11 0.052(2) 0.0341(13) 0.0380(15) 0.0000(11) 0.0024(13) -0.0092(13) O12 0.049(2) 0.0335(15) 0.068(2) 0.0050(14) -0.0063(16) 0.0004(13) _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 C1 O2 1.257(5) . ? C1 O1 1.262(5) . ? C1 C2 1.511(5) . ? C1 Cd1 2.691(4) . ? C2 C7 1.362(7) . ? C2 C3 1.369(6) . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 C5 1.364(6) . ? C4 H4 0.9500 . ? C5 C6 1.353(7) . ? C5 C22 1.497(5) . ? C6 C7 1.406(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O4 1.249(5) . ? C8 O3 1.255(5) . ? C8 C9 1.511(5) . ? C8 Cd2 2.742(4) . ? C9 C14 1.386(6) . ? C9 C10 1.395(5) . ? C10 C11 1.378(5) . ? C10 H10 0.9500 . ? C11 C12 1.402(5) . ? C11 H11 0.9500 . ? C12 C13 1.416(5) . ? C12 C24 1.491(5) . ? C13 C14 1.383(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O5 1.251(5) . ? C15 O6 1.263(5) . ? C15 C16 1.504(5) . ? C15 Cd2 2.715(4) 2_543 ? C16 C17 1.391(6) . ? C16 C21 1.392(5) . ? C17 C18 1.394(6) . ? C17 H17 0.9500 . ? C18 C19 1.389(5) . ? C18 H18 0.9500 . ? C19 C20 1.367(6) . ? C19 C26 1.498(5) . ? C20 C21 1.395(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.393(5) . ? C22 C27 1.397(5) . ? C23 C24 1.396(5) . ? C23 H23 0.9500 . ? C24 C25 1.405(5) . ? C25 C26 1.394(5) . ? C25 H25 0.9500 . ? C26 C27 1.406(5) . ? C27 H27 0.9500 . ? C28 O7 1.256(5) . ? C28 O8 1.262(5) . ? C28 C29 1.494(5) . ? C29 C34 1.385(6) . ? C29 C30 1.399(6) . ? C30 C31 1.395(5) . ? C30 H30 0.9500 . ? C31 C32 1.399(6) . ? C31 H31 0.9500 . ? C32 C33 1.398(6) . ? C32 C49 1.490(5) . ? C33 C34 1.383(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 O9 1.257(6) . ? C35 O10 1.268(6) . ? C35 C36 1.490(5) . ? C36 C41 1.371(7) . ? C36 C37 1.398(6) . ? C37 C38 1.414(6) . ? C37 H37 0.9500 . ? C38 C39 1.390(6) . ? C38 H38 0.9500 . ? C39 C40 1.363(6) . ? C39 C51 1.479(5) . ? C40 C41 1.381(6) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 O11 1.236(5) . ? C42 O12 1.292(5) . ? C42 C43 1.501(5) . ? C42 Cd1 2.745(4) 2_655 ? C43 C48 1.384(5) . ? C43 C44 1.410(5) . ? C44 C45 1.382(5) . ? C44 H44 0.9500 . ? C45 C46 1.398(5) . ? C45 H45 0.9500 . ? C46 C47 1.390(5) . ? C46 C53 1.498(5) . ? C47 C48 1.378(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.389(5) . ? C49 C54 1.411(5) . ? C50 C51 1.401(5) . ? C50 H50 0.9500 . ? C51 C52 1.392(5) . ? C52 C53 1.377(5) . ? C52 H52 0.9500 . ? C53 C54 1.396(5) . ? C54 H54 0.9500 . ? C55 N1 1.314(6) . ? C55 C56 1.404(8) . ? C55 H55 0.9500 . ? C56 C57 1.336(7) . ? C56 H56 0.9500 . ? C57 C58 1.365(5) . ? C57 C62 1.484(6) . ? C58 C59 1.394(7) . ? C58 H58 0.9500 . ? C59 N1 1.340(6) . ? C59 H59 0.9500 . ? C60 N2 1.326(5) . ? C60 C61 1.382(6) . ? C60 H60 0.9500 . ? C61 C62 1.394(5) . ? C61 H61 0.9500 . ? C62 C63 1.402(6) . ? C63 C64 1.376(7) . ? C63 H63 0.9500 . ? C64 N2 1.348(5) . ? C64 H64 0.9500 . ? Cd1 O12 2.317(3) 2_645 ? Cd1 O8 2.319(3) . ? Cd1 O2 2.337(2) . ? Cd1 N1 2.337(3) . ? Cd1 O1 2.355(3) . ? Cd1 O11 2.492(3) 2_645 ? Cd1 O7 2.518(3) . ? Cd1 C42 2.745(4) 2_645 ? Cd2 O3 2.285(3) . ? Cd2 N2 2.324(3) 3_565 ? Cd2 O6 2.336(3) 2_553 ? Cd2 O9 2.378(3) 2_655 ? Cd2 O5 2.406(3) 2_553 ? Cd2 O10 2.479(3) 2_655 ? Cd2 O4 2.519(3) . ? Cd2 C15 2.715(4) 2_553 ? N2 Cd2 2.324(3) 3_565 ? O5 Cd2 2.406(3) 2_543 ? O6 Cd2 2.336(3) 2_543 ? O9 Cd2 2.378(3) 2_645 ? O10 Cd2 2.479(3) 2_645 ? O11 Cd1 2.492(3) 2_655 ? O12 Cd1 2.317(3) 2_655 ? 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 O2 C1 O1 121.3(3) . . ? O2 C1 C2 119.7(3) . . ? O1 C1 C2 119.0(4) . . ? O2 C1 Cd1 60.23(18) . . ? O1 C1 Cd1 61.05(19) . . ? C2 C1 Cd1 178.9(3) . . ? C7 C2 C3 118.8(4) . . ? C7 C2 C1 120.3(4) . . ? C3 C2 C1 120.9(4) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 122.1(5) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C6 C5 C4 117.2(4) . . ? C6 C5 C22 119.7(4) . . ? C4 C5 C22 123.0(4) . . ? C5 C6 C7 121.8(5) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C2 C7 C6 119.8(5) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? O4 C8 O3 121.9(4) . . ? O4 C8 C9 119.2(4) . . ? O3 C8 C9 118.9(4) . . ? O4 C8 Cd2 66.5(2) . . ? O3 C8 Cd2 55.8(2) . . ? C9 C8 Cd2 169.8(2) . . ? C14 C9 C10 118.3(3) . . ? C14 C9 C8 120.7(4) . . ? C10 C9 C8 120.8(4) . . ? C11 C10 C9 121.1(4) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 121.3(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C13 117.3(3) . . ? C11 C12 C24 121.9(3) . . ? C13 C12 C24 120.8(3) . . ? C14 C13 C12 120.6(4) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C9 121.4(4) . . ? C13 C14 H14 119.3 . . ? C9 C14 H14 119.3 . . ? O5 C15 O6 121.6(3) . . ? O5 C15 C16 119.6(4) . . ? O6 C15 C16 118.9(4) . . ? O5 C15 Cd2 62.4(2) . 2_543 ? O6 C15 Cd2 59.18(19) . 2_543 ? C16 C15 Cd2 177.6(3) . 2_543 ? C17 C16 C21 118.5(3) . . ? C17 C16 C15 120.3(4) . . ? C21 C16 C15 121.2(4) . . ? C16 C17 C18 120.9(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 119.1(4) . . ? C20 C19 C26 120.8(3) . . ? C18 C19 C26 120.1(4) . . ? C19 C20 C21 121.4(4) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C16 C21 C20 120.0(4) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C27 119.4(3) . . ? C23 C22 C5 120.5(3) . . ? C27 C22 C5 120.1(3) . . ? C22 C23 C24 121.4(3) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C25 118.6(3) . . ? C23 C24 C12 120.7(3) . . ? C25 C24 C12 120.7(3) . . ? C26 C25 C24 120.8(3) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 119.5(3) . . ? C25 C26 C19 120.0(3) . . ? C27 C26 C19 120.4(3) . . ? C22 C27 C26 120.2(3) . . ? C22 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? O7 C28 O8 121.0(4) . . ? O7 C28 C29 119.9(4) . . ? O8 C28 C29 119.0(4) . . ? C34 C29 C30 118.5(4) . . ? C34 C29 C28 120.8(4) . . ? C30 C29 C28 120.6(4) . . ? C31 C30 C29 120.7(4) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 120.6(4) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 118.1(3) . . ? C33 C32 C49 121.3(4) . . ? C31 C32 C49 120.6(4) . . ? C34 C33 C32 121.1(4) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C29 121.1(4) . . ? C33 C34 H34 119.5 . . ? C29 C34 H34 119.5 . . ? O9 C35 O10 121.1(4) . . ? O9 C35 C36 119.1(4) . . ? O10 C35 C36 119.6(4) . . ? C41 C36 C37 116.7(4) . . ? C41 C36 C35 122.3(4) . . ? C37 C36 C35 120.3(4) . . ? C36 C37 C38 120.5(4) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C39 C38 C37 120.4(4) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 117.6(4) . . ? C40 C39 C51 122.4(4) . . ? C38 C39 C51 119.7(4) . . ? C39 C40 C41 121.7(5) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C36 C41 C40 122.2(4) . . ? C36 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? O11 C42 O12 121.7(4) . . ? O11 C42 C43 121.0(4) . . ? O12 C42 C43 117.2(4) . . ? O11 C42 Cd1 65.1(2) . 2_655 ? O12 C42 Cd1 57.3(2) . 2_655 ? C43 C42 Cd1 168.1(3) . 2_655 ? C48 C43 C44 118.5(3) . . ? C48 C43 C42 122.3(4) . . ? C44 C43 C42 119.1(3) . . ? C45 C44 C43 120.0(3) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 121.0(4) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C47 C46 C45 118.5(3) . . ? C47 C46 C53 121.7(3) . . ? C45 C46 C53 119.8(3) . . ? C48 C47 C46 120.8(4) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C43 121.2(4) . . ? C47 C48 H48 119.4 . . ? C43 C48 H48 119.4 . . ? C50 C49 C54 118.8(3) . . ? C50 C49 C32 121.3(3) . . ? C54 C49 C32 119.9(3) . . ? C49 C50 C51 121.3(3) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C52 C51 C50 118.1(3) . . ? C52 C51 C39 120.7(3) . . ? C50 C51 C39 121.2(3) . . ? C53 C52 C51 122.4(3) . . ? C53 C52 H52 118.8 . . ? C51 C52 H52 118.8 . . ? C52 C53 C54 118.7(3) . . ? C52 C53 C46 121.5(3) . . ? C54 C53 C46 119.8(3) . . ? C53 C54 C49 120.6(3) . . ? C53 C54 H54 119.7 . . ? C49 C54 H54 119.7 . . ? N1 C55 C56 123.2(5) . . ? N1 C55 H55 118.4 . . ? C56 C55 H55 118.4 . . ? C57 C56 C55 120.6(5) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C56 C57 C58 117.7(4) . . ? C56 C57 C62 120.4(4) . . ? C58 C57 C62 121.7(4) . . ? C57 C58 C59 118.8(4) . . ? C57 C58 H58 120.6 . . ? C59 C58 H58 120.6 . . ? N1 C59 C58 124.0(4) . . ? N1 C59 H59 118.0 . . ? C58 C59 H59 118.0 . . ? N2 C60 C61 122.9(4) . . ? N2 C60 H60 118.6 . . ? C61 C60 H60 118.6 . . ? C60 C61 C62 120.0(4) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C63 116.6(4) . . ? C61 C62 C57 121.6(4) . . ? C63 C62 C57 121.7(3) . . ? C64 C63 C62 119.8(4) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? N2 C64 C63 122.7(4) . . ? N2 C64 H64 118.7 . . ? C63 C64 H64 118.7 . . ? O12 Cd1 O8 82.81(11) 2_645 . ? O12 Cd1 O2 108.83(12) 2_645 . ? O8 Cd1 O2 108.21(12) . . ? O12 Cd1 N1 95.82(12) 2_645 . ? O8 Cd1 N1 99.23(13) . . ? O2 Cd1 N1 144.83(11) . . ? O12 Cd1 O1 138.73(10) 2_645 . ? O8 Cd1 O1 136.83(11) . . ? O2 Cd1 O1 55.81(10) . . ? N1 Cd1 O1 89.11(11) . . ? O12 Cd1 O11 54.54(10) 2_645 2_645 ? O8 Cd1 O11 137.32(10) . 2_645 ? O2 Cd1 O11 89.16(10) . 2_645 ? N1 Cd1 O11 85.08(11) . 2_645 ? O1 Cd1 O11 85.32(9) . 2_645 ? O12 Cd1 O7 135.97(10) 2_645 . ? O8 Cd1 O7 53.68(10) . . ? O2 Cd1 O7 92.70(9) . . ? N1 Cd1 O7 86.06(11) . . ? O1 Cd1 O7 85.17(9) . . ? O11 Cd1 O7 167.09(11) 2_645 . ? O12 Cd1 C1 127.35(11) 2_645 . ? O8 Cd1 C1 126.13(12) . . ? O2 Cd1 C1 27.84(11) . . ? N1 Cd1 C1 117.05(13) . . ? O1 Cd1 C1 27.97(11) . . ? O11 Cd1 C1 86.83(10) 2_645 . ? O7 Cd1 C1 88.86(10) . . ? O12 Cd1 C42 27.98(12) 2_645 2_645 ? O8 Cd1 C42 110.59(12) . 2_645 ? O2 Cd1 C42 101.94(11) . 2_645 ? N1 Cd1 C42 88.06(12) . 2_645 ? O1 Cd1 C42 111.97(11) . 2_645 ? O11 Cd1 C42 26.75(11) 2_645 2_645 ? O7 Cd1 C42 161.80(11) . 2_645 ? C1 Cd1 C42 109.13(11) . 2_645 ? O3 Cd2 N2 104.03(12) . 3_565 ? O3 Cd2 O6 104.19(11) . 2_553 ? N2 Cd2 O6 140.15(11) 3_565 2_553 ? O3 Cd2 O9 83.90(12) . 2_655 ? N2 Cd2 O9 91.71(14) 3_565 2_655 ? O6 Cd2 O9 118.77(14) 2_553 2_655 ? O3 Cd2 O5 137.80(10) . 2_553 ? N2 Cd2 O5 85.17(11) 3_565 2_553 ? O6 Cd2 O5 55.10(10) 2_553 2_553 ? O9 Cd2 O5 137.64(10) 2_655 2_553 ? O3 Cd2 O10 137.11(12) . 2_655 ? N2 Cd2 O10 85.77(12) 3_565 2_655 ? O6 Cd2 O10 92.26(10) 2_553 2_655 ? O9 Cd2 O10 53.77(11) 2_655 2_655 ? O5 Cd2 O10 83.88(10) 2_553 2_655 ? O3 Cd2 O4 53.94(10) . . ? N2 Cd2 O4 84.72(11) 3_565 . ? O6 Cd2 O4 89.69(10) 2_553 . ? O9 Cd2 O4 134.87(11) 2_655 . ? O5 Cd2 O4 86.98(9) 2_553 . ? O10 Cd2 O4 167.31(13) 2_655 . ? O3 Cd2 C15 124.08(12) . 2_553 ? N2 Cd2 C15 112.58(13) 3_565 2_553 ? O6 Cd2 C15 27.66(12) 2_553 2_553 ? O9 Cd2 C15 133.25(13) 2_655 2_553 ? O5 Cd2 C15 27.44(12) 2_553 2_553 ? O10 Cd2 C15 87.52(11) 2_655 2_553 ? O4 Cd2 C15 88.41(10) . 2_553 ? O3 Cd2 C8 27.01(12) . . ? N2 Cd2 C8 93.17(11) 3_565 . ? O6 Cd2 C8 99.46(10) 2_553 . ? O9 Cd2 C8 109.07(12) 2_655 . ? O5 Cd2 C8 113.28(11) 2_553 . ? O10 Cd2 C8 162.69(12) 2_655 . ? O4 Cd2 C8 27.04(11) . . ? C15 Cd2 C8 108.71(11) 2_553 . ? C55 N1 C59 115.5(4) . . ? C55 N1 Cd1 123.6(3) . . ? C59 N1 Cd1 120.6(3) . . ? C60 N2 C64 118.0(4) . . ? C60 N2 Cd2 116.7(2) . 3_565 ? C64 N2 Cd2 125.2(3) . 3_565 ? C1 O1 Cd1 91.0(2) . . ? C1 O2 Cd1 91.9(2) . . ? C8 O3 Cd2 97.2(3) . . ? C8 O4 Cd2 86.4(2) . . ? C15 O5 Cd2 90.2(3) . 2_543 ? C15 O6 Cd2 93.2(2) . 2_543 ? C28 O7 Cd1 87.7(2) . . ? C28 O8 Cd1 96.8(3) . . ? C35 O9 Cd2 94.8(3) . 2_645 ? C35 O10 Cd2 89.8(3) . 2_645 ? C42 O11 Cd1 88.1(2) . 2_655 ? C42 O12 Cd1 94.7(3) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 8.5(6) . . . . ? O1 C1 C2 C7 -170.5(5) . . . . ? Cd1 C1 C2 C7 -79(17) . . . . ? O2 C1 C2 C3 -173.5(4) . . . . ? O1 C1 C2 C3 7.5(6) . . . . ? Cd1 C1 C2 C3 99(17) . . . . ? C7 C2 C3 C4 -4.7(8) . . . . ? C1 C2 C3 C4 177.3(4) . . . . ? C2 C3 C4 C5 3.8(8) . . . . ? C3 C4 C5 C6 1.0(8) . . . . ? C3 C4 C5 C22 177.9(4) . . . . ? C4 C5 C6 C7 -4.8(9) . . . . ? C22 C5 C6 C7 178.2(5) . . . . ? C3 C2 C7 C6 1.0(9) . . . . ? C1 C2 C7 C6 179.0(5) . . . . ? C5 C6 C7 C2 3.9(10) . . . . ? O4 C8 C9 C14 15.7(6) . . . . ? O3 C8 C9 C14 -166.9(4) . . . . ? Cd2 C8 C9 C14 137.3(16) . . . . ? O4 C8 C9 C10 -159.7(4) . . . . ? O3 C8 C9 C10 17.8(6) . . . . ? Cd2 C8 C9 C10 -38.0(19) . . . . ? C14 C9 C10 C11 -1.6(6) . . . . ? C8 C9 C10 C11 173.9(4) . . . . ? C9 C10 C11 C12 1.5(6) . . . . ? C10 C11 C12 C13 0.3(6) . . . . ? C10 C11 C12 C24 -178.9(4) . . . . ? C11 C12 C13 C14 -2.0(6) . . . . ? C24 C12 C13 C14 177.2(4) . . . . ? C12 C13 C14 C9 2.0(7) . . . . ? C10 C9 C14 C13 -0.2(6) . . . . ? C8 C9 C14 C13 -175.6(4) . . . . ? O5 C15 C16 C17 21.3(6) . . . . ? O6 C15 C16 C17 -158.3(4) . . . . ? Cd2 C15 C16 C17 -125(7) 2_543 . . . ? O5 C15 C16 C21 -158.4(4) . . . . ? O6 C15 C16 C21 21.9(6) . . . . ? Cd2 C15 C16 C21 56(7) 2_543 . . . ? C21 C16 C17 C18 -1.8(8) . . . . ? C15 C16 C17 C18 178.4(5) . . . . ? C16 C17 C18 C19 2.0(8) . . . . ? C17 C18 C19 C20 0.8(7) . . . . ? C17 C18 C19 C26 179.8(4) . . . . ? C18 C19 C20 C21 -3.7(7) . . . . ? C26 C19 C20 C21 177.3(4) . . . . ? C17 C16 C21 C20 -1.1(7) . . . . ? C15 C16 C21 C20 178.7(4) . . . . ? C19 C20 C21 C16 3.9(8) . . . . ? C6 C5 C22 C23 -102.5(5) . . . . ? C4 C5 C22 C23 80.6(6) . . . . ? C6 C5 C22 C27 76.0(6) . . . . ? C4 C5 C22 C27 -100.9(5) . . . . ? C27 C22 C23 C24 -1.1(6) . . . . ? C5 C22 C23 C24 177.5(4) . . . . ? C22 C23 C24 C25 -0.9(6) . . . . ? C22 C23 C24 C12 179.4(4) . . . . ? C11 C12 C24 C23 29.6(6) . . . . ? C13 C12 C24 C23 -149.5(4) . . . . ? C11 C12 C24 C25 -150.0(4) . . . . ? C13 C12 C24 C25 30.8(6) . . . . ? C23 C24 C25 C26 1.8(6) . . . . ? C12 C24 C25 C26 -178.5(4) . . . . ? C24 C25 C26 C27 -0.7(6) . . . . ? C24 C25 C26 C19 177.5(4) . . . . ? C20 C19 C26 C25 -124.5(5) . . . . ? C18 C19 C26 C25 56.6(6) . . . . ? C20 C19 C26 C27 53.7(6) . . . . ? C18 C19 C26 C27 -125.3(5) . . . . ? C23 C22 C27 C26 2.2(6) . . . . ? C5 C22 C27 C26 -176.4(4) . . . . ? C25 C26 C27 C22 -1.4(6) . . . . ? C19 C26 C27 C22 -179.5(4) . . . . ? O7 C28 C29 C34 -175.6(4) . . . . ? O8 C28 C29 C34 7.9(7) . . . . ? O7 C28 C29 C30 8.6(6) . . . . ? O8 C28 C29 C30 -167.9(4) . . . . ? C34 C29 C30 C31 0.5(6) . . . . ? C28 C29 C30 C31 176.4(4) . . . . ? C29 C30 C31 C32 -0.9(6) . . . . ? C30 C31 C32 C33 1.1(6) . . . . ? C30 C31 C32 C49 -178.3(4) . . . . ? C31 C32 C33 C34 -1.1(7) . . . . ? C49 C32 C33 C34 178.4(4) . . . . ? C32 C33 C34 C29 0.8(8) . . . . ? C30 C29 C34 C33 -0.5(7) . . . . ? C28 C29 C34 C33 -176.4(4) . . . . ? O9 C35 C36 C41 -1.4(9) . . . . ? O10 C35 C36 C41 174.7(6) . . . . ? O9 C35 C36 C37 -172.4(5) . . . . ? O10 C35 C36 C37 3.7(8) . . . . ? C41 C36 C37 C38 8.2(9) . . . . ? C35 C36 C37 C38 179.7(5) . . . . ? C36 C37 C38 C39 -1.8(8) . . . . ? C37 C38 C39 C40 -5.8(8) . . . . ? C37 C38 C39 C51 179.3(5) . . . . ? C38 C39 C40 C41 7.0(10) . . . . ? C51 C39 C40 C41 -178.3(6) . . . . ? C37 C36 C41 C40 -7.4(11) . . . . ? C35 C36 C41 C40 -178.6(7) . . . . ? C39 C40 C41 C36 -0.3(13) . . . . ? O11 C42 C43 C48 -173.7(4) . . . . ? O12 C42 C43 C48 4.0(6) . . . . ? Cd1 C42 C43 C48 -55.5(17) 2_655 . . . ? O11 C42 C43 C44 2.5(6) . . . . ? O12 C42 C43 C44 -179.9(4) . . . . ? Cd1 C42 C43 C44 120.7(14) 2_655 . . . ? C48 C43 C44 C45 1.8(6) . . . . ? C42 C43 C44 C45 -174.5(4) . . . . ? C43 C44 C45 C46 0.0(6) . . . . ? C44 C45 C46 C47 -1.4(6) . . . . ? C44 C45 C46 C53 178.9(3) . . . . ? C45 C46 C47 C48 1.0(6) . . . . ? C53 C46 C47 C48 -179.3(4) . . . . ? C46 C47 C48 C43 0.8(6) . . . . ? C44 C43 C48 C47 -2.2(6) . . . . ? C42 C43 C48 C47 174.0(4) . . . . ? C33 C32 C49 C50 -45.0(6) . . . . ? C31 C32 C49 C50 134.5(4) . . . . ? C33 C32 C49 C54 137.7(4) . . . . ? C31 C32 C49 C54 -42.9(6) . . . . ? C54 C49 C50 C51 -0.3(6) . . . . ? C32 C49 C50 C51 -177.6(4) . . . . ? C49 C50 C51 C52 0.5(6) . . . . ? C49 C50 C51 C39 -179.5(4) . . . . ? C40 C39 C51 C52 153.8(5) . . . . ? C38 C39 C51 C52 -31.6(7) . . . . ? C40 C39 C51 C50 -26.2(8) . . . . ? C38 C39 C51 C50 148.4(5) . . . . ? C50 C51 C52 C53 -1.7(6) . . . . ? C39 C51 C52 C53 178.3(4) . . . . ? C51 C52 C53 C54 2.6(6) . . . . ? C51 C52 C53 C46 -178.8(4) . . . . ? C47 C46 C53 C52 -147.6(4) . . . . ? C45 C46 C53 C52 32.1(6) . . . . ? C47 C46 C53 C54 31.0(6) . . . . ? C45 C46 C53 C54 -149.3(4) . . . . ? C52 C53 C54 C49 -2.3(6) . . . . ? C46 C53 C54 C49 179.1(4) . . . . ? C50 C49 C54 C53 1.1(6) . . . . ? C32 C49 C54 C53 178.6(4) . . . . ? N1 C55 C56 C57 1.7(11) . . . . ? C55 C56 C57 C58 -3.2(9) . . . . ? C55 C56 C57 C62 -178.9(6) . . . . ? C56 C57 C58 C59 3.5(8) . . . . ? C62 C57 C58 C59 179.2(5) . . . . ? C57 C58 C59 N1 -2.5(9) . . . . ? N2 C60 C61 C62 0.1(7) . . . . ? C60 C61 C62 C63 -0.7(6) . . . . ? C60 C61 C62 C57 177.9(4) . . . . ? C56 C57 C62 C61 -24.7(7) . . . . ? C58 C57 C62 C61 159.8(4) . . . . ? C56 C57 C62 C63 153.9(5) . . . . ? C58 C57 C62 C63 -21.6(6) . . . . ? C61 C62 C63 C64 0.6(6) . . . . ? C57 C62 C63 C64 -178.0(4) . . . . ? C62 C63 C64 N2 0.1(7) . . . . ? O2 C1 Cd1 O12 -54.8(3) . . . 2_645 ? O1 C1 Cd1 O12 125.4(2) . . . 2_645 ? C2 C1 Cd1 O12 34(17) . . . 2_645 ? O2 C1 Cd1 O8 56.4(3) . . . . ? O1 C1 Cd1 O8 -123.4(2) . . . . ? C2 C1 Cd1 O8 145(17) . . . . ? O1 C1 Cd1 O2 -179.8(4) . . . . ? C2 C1 Cd1 O2 88(17) . . . . ? O2 C1 Cd1 N1 -177.0(2) . . . . ? O1 C1 Cd1 N1 3.2(2) . . . . ? C2 C1 Cd1 N1 -89(17) . . . . ? O2 C1 Cd1 O1 179.8(4) . . . . ? C2 C1 Cd1 O1 -92(17) . . . . ? O2 C1 Cd1 O11 -94.2(2) . . . 2_645 ? O1 C1 Cd1 O11 86.0(2) . . . 2_645 ? C2 C1 Cd1 O11 -6(17) . . . 2_645 ? O2 C1 Cd1 O7 98.0(2) . . . . ? O1 C1 Cd1 O7 -81.8(2) . . . . ? C2 C1 Cd1 O7 -174(100) . . . . ? O2 C1 Cd1 C42 -79.2(2) . . . 2_645 ? O1 C1 Cd1 C42 101.0(2) . . . 2_645 ? C2 C1 Cd1 C42 9(17) . . . 2_645 ? O4 C8 Cd2 O3 -172.9(4) . . . . ? C9 C8 Cd2 O3 61.2(17) . . . . ? O4 C8 Cd2 N2 71.9(2) . . . 3_565 ? O3 C8 Cd2 N2 -115.2(3) . . . 3_565 ? C9 C8 Cd2 N2 -54.0(17) . . . 3_565 ? O4 C8 Cd2 O6 -70.2(2) . . . 2_553 ? O3 C8 Cd2 O6 102.7(3) . . . 2_553 ? C9 C8 Cd2 O6 163.9(17) . . . 2_553 ? O4 C8 Cd2 O9 164.8(2) . . . 2_655 ? O3 C8 Cd2 O9 -22.3(3) . . . 2_655 ? C9 C8 Cd2 O9 38.9(18) . . . 2_655 ? O4 C8 Cd2 O5 -14.3(3) . . . 2_553 ? O3 C8 Cd2 O5 158.7(2) . . . 2_553 ? C9 C8 Cd2 O5 -140.2(17) . . . 2_553 ? O4 C8 Cd2 O10 157.8(4) . . . 2_655 ? O3 C8 Cd2 O10 -29.2(6) . . . 2_655 ? C9 C8 Cd2 O10 32(2) . . . 2_655 ? O3 C8 Cd2 O4 172.9(4) . . . . ? C9 C8 Cd2 O4 -125.9(18) . . . . ? O4 C8 Cd2 C15 -43.3(3) . . . 2_553 ? O3 C8 Cd2 C15 129.7(3) . . . 2_553 ? C9 C8 Cd2 C15 -169.2(17) . . . 2_553 ? C56 C55 N1 C59 -0.5(9) . . . . ? C56 C55 N1 Cd1 173.2(5) . . . . ? C58 C59 N1 C55 0.9(8) . . . . ? C58 C59 N1 Cd1 -173.0(4) . . . . ? O12 Cd1 N1 C55 116.8(5) 2_645 . . . ? O8 Cd1 N1 C55 33.2(5) . . . . ? O2 Cd1 N1 C55 -108.1(5) . . . . ? O1 Cd1 N1 C55 -104.3(5) . . . . ? O11 Cd1 N1 C55 170.4(5) 2_645 . . . ? O7 Cd1 N1 C55 -19.0(5) . . . . ? C1 Cd1 N1 C55 -105.7(5) . . . . ? C42 Cd1 N1 C55 143.7(5) 2_645 . . . ? O12 Cd1 N1 C59 -69.9(4) 2_645 . . . ? O8 Cd1 N1 C59 -153.5(4) . . . . ? O2 Cd1 N1 C59 65.2(4) . . . . ? O1 Cd1 N1 C59 69.1(4) . . . . ? O11 Cd1 N1 C59 -16.3(4) 2_645 . . . ? O7 Cd1 N1 C59 154.3(4) . . . . ? C1 Cd1 N1 C59 67.6(4) . . . . ? C42 Cd1 N1 C59 -43.0(4) 2_645 . . . ? C61 C60 N2 C64 0.7(7) . . . . ? C61 C60 N2 Cd2 178.1(4) . . . 3_565 ? C63 C64 N2 C60 -0.8(6) . . . . ? C63 C64 N2 Cd2 -177.9(3) . . . 3_565 ? O2 C1 O1 Cd1 -0.2(4) . . . . ? C2 C1 O1 Cd1 178.8(3) . . . . ? O12 Cd1 O1 C1 -79.4(3) 2_645 . . . ? O8 Cd1 O1 C1 80.2(3) . . . . ? O2 Cd1 O1 C1 0.1(2) . . . . ? N1 Cd1 O1 C1 -177.2(2) . . . . ? O11 Cd1 O1 C1 -92.1(2) 2_645 . . . ? O7 Cd1 O1 C1 96.7(2) . . . . ? C42 Cd1 O1 C1 -89.6(2) 2_645 . . . ? O1 C1 O2 Cd1 0.2(4) . . . . ? C2 C1 O2 Cd1 -178.8(3) . . . . ? O12 Cd1 O2 C1 136.6(2) 2_645 . . . ? O8 Cd1 O2 C1 -134.9(2) . . . . ? N1 Cd1 O2 C1 4.6(3) . . . . ? O1 Cd1 O2 C1 -0.1(2) . . . . ? O11 Cd1 O2 C1 84.8(2) 2_645 . . . ? O7 Cd1 O2 C1 -82.4(2) . . . . ? C42 Cd1 O2 C1 108.5(2) 2_645 . . . ? O4 C8 O3 Cd2 7.6(4) . . . . ? C9 C8 O3 Cd2 -169.8(3) . . . . ? N2 Cd2 O3 C8 68.6(3) 3_565 . . . ? O6 Cd2 O3 C8 -82.9(3) 2_553 . . . ? O9 Cd2 O3 C8 158.9(3) 2_655 . . . ? O5 Cd2 O3 C8 -29.8(3) 2_553 . . . ? O10 Cd2 O3 C8 167.7(2) 2_655 . . . ? O4 Cd2 O3 C8 -4.0(2) . . . . ? C15 Cd2 O3 C8 -61.7(3) 2_553 . . . ? O3 C8 O4 Cd2 -6.9(4) . . . . ? C9 C8 O4 Cd2 170.5(3) . . . . ? O3 Cd2 O4 C8 4.0(2) . . . . ? N2 Cd2 O4 C8 -107.7(2) 3_565 . . . ? O6 Cd2 O4 C8 111.8(2) 2_553 . . . ? O9 Cd2 O4 C8 -20.5(3) 2_655 . . . ? O5 Cd2 O4 C8 166.9(2) 2_553 . . . ? O10 Cd2 O4 C8 -149.2(4) 2_655 . . . ? C15 Cd2 O4 C8 139.5(2) 2_553 . . . ? O6 C15 O5 Cd2 1.2(4) . . . 2_543 ? C16 C15 O5 Cd2 -178.5(3) . . . 2_543 ? O5 C15 O6 Cd2 -1.2(4) . . . 2_543 ? C16 C15 O6 Cd2 178.5(3) . . . 2_543 ? O8 C28 O7 Cd1 9.0(4) . . . . ? C29 C28 O7 Cd1 -167.5(4) . . . . ? O12 Cd1 O7 C28 5.0(3) 2_645 . . . ? O8 Cd1 O7 C28 -5.2(2) . . . . ? O2 Cd1 O7 C28 -115.9(3) . . . . ? N1 Cd1 O7 C28 99.3(3) . . . . ? O1 Cd1 O7 C28 -171.3(3) . . . . ? O11 Cd1 O7 C28 146.0(4) 2_645 . . . ? C1 Cd1 O7 C28 -143.5(3) . . . . ? C42 Cd1 O7 C28 27.8(5) 2_645 . . . ? O7 C28 O8 Cd1 -9.8(5) . . . . ? C29 C28 O8 Cd1 166.7(3) . . . . ? O12 Cd1 O8 C28 -167.7(3) 2_645 . . . ? O2 Cd1 O8 C28 84.8(3) . . . . ? N1 Cd1 O8 C28 -72.9(3) . . . . ? O1 Cd1 O8 C28 25.7(4) . . . . ? O11 Cd1 O8 C28 -165.7(2) 2_645 . . . ? O7 Cd1 O8 C28 5.2(2) . . . . ? C1 Cd1 O8 C28 60.6(3) . . . . ? C42 Cd1 O8 C28 -164.3(3) 2_645 . . . ? O10 C35 O9 Cd2 -7.6(6) . . . 2_645 ? C36 C35 O9 Cd2 168.4(4) . . . 2_645 ? O9 C35 O10 Cd2 7.3(5) . . . 2_645 ? C36 C35 O10 Cd2 -168.7(4) . . . 2_645 ? O12 C42 O11 Cd1 -9.1(4) . . . 2_655 ? C43 C42 O11 Cd1 168.5(3) . . . 2_655 ? O11 C42 O12 Cd1 9.8(5) . . . 2_655 ? C43 C42 O12 Cd1 -167.8(3) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.850 _refine_diff_density_min -1.195 _refine_diff_density_rms 0.119 # 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 0.581 0.258 -0.003 3339 83 _platon_squeeze_details ; During the refinement of the structure, electron density peaks were located that were believed to be highly disordered solvent molecules and ions (4,4'-bipy, water molecules, DMF molecules and Cd ions). Attempts made to model the disordered solvent molecules and ions were not successful. So the SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of these disordered molecules and ions (Spek, 2003). Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13 ; # start Validation Reply Form _vrf_CHEMW03_3 ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10. RESPONSE: Disordered molecules and ions can not be identified. ; _vrf_PLAT043_3 ; PROBLEM: Check Reported Molecular Weight. RESPONSE: Disordered 4,4'-bipy, solvent molecules and ions can not be identified and removed with the SQUEEZE. ; _vrf_PLAT044_3 ; PROBLEM: Calculated and Reported Dx Differ. RESPONSE: Disordered 4,4'-bipy, solvent molecules and ions can not be identified and removed with the SQUEEZE. ; _vrf_PLAT051_3 ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by. RESPONSE: Disordered 4,4'-bipy, solvent molecules and ions can not be identified and removed with the SQUEEZE. ; # end Validation Reply Form # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 825085' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H84 Cd3 N12 O18' _chemical_formula_weight 1886.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.055(10) _cell_length_b 17.775(6) _cell_length_c 18.682(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.571(9) _cell_angle_gamma 90.00 _cell_volume 8259(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 696 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 19.88 _exptl_crystal_description PRISM _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6881 _exptl_absorpt_correction_T_max 0.8841 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% . _diffrn_reflns_number 28547 _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_sigmaI/netI 0.1191 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7247 _reflns_number_gt 5325 _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 '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^)+(0.0577P)^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 7247 _refine_ls_number_parameters 528 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1894 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.2044 _refine_ls_wR_factor_gt 0.1445 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.969 _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 C1 C 0.1510(4) 0.4068(6) 0.1443(6) 0.021(3) Uani 1 1 d . . . C2 C 0.1258(4) 0.3321(5) 0.1331(6) 0.019(3) Uani 1 1 d . . . C3 C 0.1566(4) 0.2714(5) 0.1768(6) 0.023(3) Uani 1 1 d . . . H3 H 0.1940 0.2772 0.2114 0.028 Uiso 1 1 calc R . . C4 C 0.1314(5) 0.2006(6) 0.1691(7) 0.025(3) Uani 1 1 d . . . H4 H 0.1524 0.1595 0.2003 0.030 Uiso 1 1 calc R . . C5 C 0.0779(4) 0.1895(5) 0.1180(6) 0.023(2) Uani 1 1 d . . . C6 C 0.0482(4) 0.2519(5) 0.0746(6) 0.020(3) Uani 1 1 d . . . H6 H 0.0110 0.2460 0.0383 0.024 Uiso 1 1 calc R . . C7 C 0.0717(4) 0.3228(5) 0.0833(6) 0.021(3) Uani 1 1 d . . . H7 H 0.0503 0.3647 0.0548 0.025 Uiso 1 1 calc R . . C8 C -0.2158(4) 0.0491(5) 0.1440(7) 0.020(2) Uani 1 1 d . . . C9 C -0.1678(4) 0.0434(6) 0.1280(6) 0.017(2) Uani 1 1 d . . . C10 C -0.1655(4) 0.0797(6) 0.0632(6) 0.024(3) Uani 1 1 d U . . H10 H -0.1967 0.1042 0.0238 0.029 Uiso 1 1 calc R . . C11 C -0.1187(4) 0.0804(5) 0.0553(6) 0.014(2) Uani 1 1 d U . . H11 H -0.1174 0.1078 0.0125 0.017 Uiso 1 1 calc R . . C12 C -0.0740(4) 0.0413(5) 0.1099(6) 0.017(2) Uani 1 1 d U . . C13 C -0.0778(4) 0.0002(6) 0.1719(7) 0.027(3) Uani 1 1 d . . . H13 H -0.0483 -0.0295 0.2081 0.032 Uiso 1 1 calc R . . C14 C -0.1227(4) 0.0031(6) 0.1793(7) 0.028(3) Uani 1 1 d . . . H14 H -0.1239 -0.0240 0.2223 0.033 Uiso 1 1 calc R . . C15 C 0.1715(4) -0.3005(5) 0.1589(6) 0.019(3) Uani 1 1 d U . . C16 C 0.1416(4) -0.2274(5) 0.1406(6) 0.020(3) Uani 1 1 d U . . C17 C 0.0855(4) -0.2261(6) 0.1031(6) 0.026(3) Uani 1 1 d U . . H17 H 0.0660 -0.2716 0.0831 0.031 Uiso 1 1 calc R . . C18 C 0.0582(4) -0.1593(5) 0.0949(6) 0.023(3) Uani 1 1 d U . . H18 H 0.0201 -0.1598 0.0718 0.027 Uiso 1 1 calc R . . C19 C 0.0859(4) -0.0913(5) 0.1200(6) 0.020(3) Uani 1 1 d U . . C20 C 0.1417(4) -0.0934(5) 0.1541(6) 0.017(2) Uani 1 1 d . . . H20 H 0.1614 -0.0477 0.1705 0.020 Uiso 1 1 calc R . . C21 C 0.1690(4) -0.1603(5) 0.1646(6) 0.022(3) Uani 1 1 d . . . H21 H 0.2072 -0.1601 0.1887 0.026 Uiso 1 1 calc R . . C22 C 0.0520(4) 0.1158(6) 0.1116(6) 0.018(2) Uani 1 1 d . . . C23 C 0.0013(4) 0.1125(5) 0.1074(6) 0.019(3) Uani 1 1 d . . . H23 H -0.0175 0.1577 0.1043 0.023 Uiso 1 1 calc R . . C24 C -0.0224(4) 0.0430(6) 0.1076(6) 0.019(2) Uani 1 1 d . . . C25 C 0.0060(4) -0.0219(5) 0.1093(6) 0.021(3) Uani 1 1 d . . . H25 H -0.0100 -0.0693 0.1080 0.025 Uiso 1 1 calc R . . C26 C 0.0566(4) -0.0202(6) 0.1130(6) 0.022(3) Uani 1 1 d . . . C27 C 0.0790(4) 0.0501(6) 0.1127(6) 0.022(3) Uani 1 1 d . . . H27 H 0.1130 0.0528 0.1133 0.027 Uiso 1 1 calc R . . C28 C 0.2533(4) 0.5931(6) 0.3595(7) 0.028(3) Uani 1 1 d . . . H28 H 0.2715 0.6309 0.3455 0.034 Uiso 1 1 calc R . . C29 C 0.2244(4) 0.5256(6) 0.4289(7) 0.032(3) Uani 1 1 d . . . H29 H 0.2181 0.5065 0.4713 0.039 Uiso 1 1 calc R . . C30 C 0.2020(4) 0.5016(6) 0.3506(7) 0.027(3) Uani 1 1 d . . . H30 H 0.1772 0.4612 0.3292 0.033 Uiso 1 1 calc R . . C31 C 0.4195(5) 0.8933(6) 0.6308(7) 0.033(3) Uani 1 1 d . . . H31 H 0.4286 0.9057 0.5892 0.039 Uiso 1 1 calc R . . C32 C 0.3849(5) 0.8346(6) 0.6987(8) 0.035(3) Uani 1 1 d . . . H32 H 0.3655 0.8001 0.7144 0.042 Uiso 1 1 calc R . . C33 C 0.4155(5) 0.8926(6) 0.7428(8) 0.041(3) Uani 1 1 d . . . H33 H 0.4215 0.9057 0.7956 0.050 Uiso 1 1 calc R . . C34 C 0.2888(4) 0.6341(6) 0.5023(7) 0.029(3) Uani 1 1 d . . . H34A H 0.2898 0.6113 0.5514 0.035 Uiso 1 1 calc R . . H34B H 0.2703 0.6832 0.4932 0.035 Uiso 1 1 calc R . . C35 C 0.3462(4) 0.6463(6) 0.5156(7) 0.028(3) Uani 1 1 d U . . H35A H 0.3654 0.5974 0.5278 0.033 Uiso 1 1 calc R . . H35B H 0.3452 0.6663 0.4654 0.033 Uiso 1 1 calc R . . C36 C 0.3769(4) 0.7010(6) 0.5847(7) 0.029(3) Uani 1 1 d U . . H36A H 0.3707 0.6875 0.6311 0.035 Uiso 1 1 calc R . . H36B H 0.4159 0.6964 0.6021 0.035 Uiso 1 1 calc R . . C37 C 0.3596(5) 0.7812(6) 0.5605(7) 0.036(3) Uani 1 1 d U . . H37A H 0.3672 0.7952 0.5155 0.044 Uiso 1 1 calc R . . H37B H 0.3202 0.7851 0.5406 0.044 Uiso 1 1 calc R . . C38 C 0.3942(4) 1.1244(6) 0.6164(7) 0.024(3) Uani 1 1 d . . . H38 H 0.3840 1.0855 0.5771 0.029 Uiso 1 1 calc R . . C39 C 0.3937(5) 1.2314(7) 0.6709(7) 0.036(3) Uani 1 1 d . . . H39 H 0.3849 1.2809 0.6799 0.043 Uiso 1 1 calc R . . C40 C 0.4347(5) 1.1875(6) 0.7242(7) 0.029(3) Uani 1 1 d . . . H40 H 0.4596 1.2017 0.7776 0.034 Uiso 1 1 calc R . . C41 C 0.3212(4) 1.2139(6) 0.5275(6) 0.022(3) Uani 1 1 d . . . H41A H 0.3102 1.1721 0.4880 0.027 Uiso 1 1 calc R . . H41B H 0.3317 1.2569 0.5042 0.027 Uiso 1 1 calc R . . C42 C 0.2736(4) 1.2366(6) 0.5398(6) 0.021(3) Uani 1 1 d . . . H42A H 0.2845 1.2776 0.5802 0.025 Uiso 1 1 calc R . . H42B H 0.2620 1.1932 0.5611 0.025 Uiso 1 1 calc R . . Cd1 Cd 0.20192(3) 0.54529(4) 0.17792(5) 0.0190(2) Uani 1 1 d . . . Cd2 Cd 0.5000 1.02645(6) 0.7500 0.0247(3) Uani 1 2 d S . . N1 N 0.2204(3) 0.5441(5) 0.3070(5) 0.024(2) Uani 1 1 d . . . N2 N 0.2588(3) 0.5850(5) 0.4330(5) 0.025(2) Uani 1 1 d . . . N3 N 0.4365(4) 0.9297(5) 0.6992(5) 0.025(2) Uani 1 1 d . . . N4 N 0.3871(4) 0.8352(5) 0.6277(6) 0.025(2) Uani 1 1 d . . . N5 N 0.4346(4) 1.1180(5) 0.6882(6) 0.032(2) Uani 1 1 d . . . N6 N 0.3681(3) 1.1899(5) 0.6021(5) 0.023(2) Uani 1 1 d . . . O1 O 0.1216(3) 0.4659(4) 0.1352(4) 0.031(2) Uani 1 1 d . . . O2 O 0.1997(3) 0.4124(4) 0.1638(5) 0.030(2) Uani 1 1 d . . . O3 O -0.2619(3) 0.0614(4) 0.0848(4) 0.0235(18) Uani 1 1 d . . . O4 O -0.2077(3) 0.0413(4) 0.2136(4) 0.0242(17) Uani 1 1 d . . . O5 O 0.2201(3) -0.3045(4) 0.2125(4) 0.0235(18) Uani 1 1 d . . . O6 O 0.1444(3) -0.3594(4) 0.1175(4) 0.0237(18) Uani 1 1 d . . . O1W O 0.4815(3) 1.0293(4) 0.8607(4) 0.033(2) Uani 1 1 d . . . H1A H 0.5071 1.0129 0.9040 0.050 Uiso 1 1 d R . . H1B H 0.4521 1.0088 0.8514 0.050 Uiso 1 1 d R . . O2W O 0.2617(3) 0.2833(4) 0.1390(4) 0.034(2) Uani 1 1 d . . . H2A H 0.2670 0.2586 0.1810 0.051 Uiso 1 1 d R . . H2B H 0.2596 0.3277 0.1541 0.051 Uiso 1 1 d R . . O3W O 0.0524(3) 0.5685(4) 0.0115(5) 0.055(3) Uani 1 1 d . . . H3A H 0.0733 0.6068 0.0216 0.083 Uiso 1 1 d R . . H3B H 0.0666 0.5381 0.0512 0.083 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(7) 0.016(6) 0.019(6) 0.003(5) -0.002(5) 0.001(5) C2 0.024(7) 0.017(6) 0.013(6) -0.003(5) 0.007(5) -0.003(5) C3 0.014(6) 0.014(6) 0.027(7) -0.002(5) -0.003(5) -0.006(5) C4 0.030(7) 0.014(6) 0.032(7) 0.001(5) 0.014(6) 0.003(5) C5 0.023(6) 0.012(5) 0.027(6) -0.001(4) 0.008(5) 0.009(5) C6 0.029(7) 0.020(6) 0.008(6) -0.005(4) 0.005(5) 0.007(5) C7 0.030(7) 0.004(5) 0.026(7) 0.000(5) 0.011(6) 0.002(5) C8 0.025(7) 0.012(6) 0.019(7) -0.008(5) 0.008(5) 0.000(5) C9 0.008(5) 0.020(6) 0.022(6) -0.003(5) 0.007(5) -0.001(5) C10 0.029(5) 0.018(4) 0.020(4) 0.006(3) 0.007(4) -0.001(4) C11 0.017(4) 0.008(4) 0.014(4) -0.003(3) 0.004(3) 0.002(3) C12 0.020(4) 0.012(4) 0.015(4) 0.000(3) 0.004(3) 0.000(3) C13 0.025(7) 0.019(6) 0.032(7) 0.003(5) 0.009(6) 0.004(5) C14 0.031(7) 0.023(7) 0.026(7) -0.005(5) 0.010(6) -0.003(6) C15 0.019(4) 0.014(4) 0.019(4) 0.008(3) 0.005(3) 0.001(3) C16 0.020(4) 0.014(4) 0.020(4) 0.000(3) 0.005(3) 0.000(3) C17 0.025(5) 0.018(4) 0.027(5) -0.001(4) 0.006(4) 0.000(4) C18 0.017(4) 0.020(4) 0.023(4) -0.001(4) 0.002(3) 0.000(3) C19 0.023(4) 0.015(4) 0.017(4) -0.003(3) 0.007(3) 0.000(3) C20 0.014(6) 0.018(6) 0.014(6) 0.003(5) 0.004(5) 0.003(5) C21 0.021(6) 0.022(6) 0.012(6) -0.001(5) -0.001(5) 0.000(5) C22 0.019(6) 0.018(6) 0.013(6) -0.007(5) 0.005(5) -0.009(5) C23 0.014(6) 0.013(6) 0.026(7) 0.001(5) 0.006(5) 0.007(5) C24 0.020(6) 0.014(6) 0.017(6) -0.001(5) 0.003(5) 0.003(5) C25 0.021(6) 0.012(6) 0.019(6) -0.001(5) 0.000(5) -0.006(5) C26 0.023(7) 0.017(6) 0.015(6) 0.000(5) 0.001(5) 0.002(5) C27 0.017(6) 0.024(6) 0.021(6) 0.000(5) 0.005(5) -0.005(5) C28 0.020(7) 0.023(7) 0.030(8) 0.002(5) 0.002(6) -0.011(5) C29 0.031(7) 0.034(7) 0.024(7) 0.007(6) 0.005(6) -0.016(6) C30 0.024(7) 0.023(7) 0.025(7) 0.007(5) 0.004(6) 0.001(5) C31 0.041(8) 0.028(7) 0.025(7) 0.000(6) 0.011(6) -0.004(6) C32 0.036(8) 0.025(7) 0.056(10) -0.014(6) 0.032(7) -0.013(6) C33 0.047(9) 0.027(7) 0.047(9) 0.000(6) 0.019(7) -0.012(6) C34 0.029(7) 0.026(7) 0.025(7) -0.008(5) 0.006(6) -0.003(5) C35 0.026(5) 0.023(4) 0.027(5) -0.007(4) 0.006(4) 0.006(4) C36 0.023(5) 0.025(4) 0.029(5) -0.008(4) 0.004(4) 0.005(4) C37 0.038(5) 0.033(5) 0.030(5) -0.002(4) 0.008(4) -0.003(4) C38 0.020(7) 0.022(6) 0.023(7) -0.004(5) 0.003(6) 0.004(5) C39 0.045(8) 0.027(7) 0.027(8) -0.009(6) 0.009(7) 0.001(6) C40 0.035(8) 0.013(6) 0.040(8) -0.001(6) 0.019(7) 0.007(5) C41 0.022(7) 0.021(6) 0.014(6) 0.000(5) 0.001(5) -0.002(5) C42 0.019(6) 0.013(6) 0.025(7) 0.004(5) 0.006(5) 0.007(5) Cd1 0.0170(4) 0.0141(4) 0.0201(5) -0.0002(4) 0.0038(3) 0.0000(4) Cd2 0.0189(7) 0.0206(7) 0.0268(7) 0.000 0.0040(6) 0.000 N1 0.020(5) 0.016(5) 0.029(6) 0.000(4) 0.007(4) -0.004(4) N2 0.021(5) 0.034(6) 0.015(5) -0.007(4) 0.004(4) -0.008(4) N3 0.027(6) 0.023(5) 0.018(5) 0.010(4) 0.005(5) 0.007(4) N4 0.027(6) 0.014(5) 0.030(6) 0.002(4) 0.009(5) -0.002(4) N5 0.025(6) 0.020(5) 0.042(7) -0.004(5) 0.009(5) -0.004(4) N6 0.019(5) 0.022(5) 0.026(6) 0.002(4) 0.007(5) 0.008(4) O1 0.036(5) 0.014(4) 0.035(5) 0.004(4) 0.010(4) -0.004(4) O2 0.027(5) 0.023(4) 0.040(5) -0.013(4) 0.016(4) -0.007(4) O3 0.016(4) 0.023(4) 0.024(4) 0.002(3) 0.002(4) 0.003(3) O4 0.027(4) 0.017(4) 0.026(5) 0.004(4) 0.010(4) 0.002(3) O5 0.019(4) 0.017(4) 0.029(5) 0.002(3) 0.006(4) 0.000(3) O6 0.023(4) 0.013(4) 0.028(5) -0.002(3) 0.006(4) 0.002(3) O1W 0.030(5) 0.034(5) 0.030(5) -0.006(4) 0.009(4) -0.011(4) O2W 0.047(5) 0.021(4) 0.036(5) 0.005(4) 0.021(4) 0.010(4) O3W 0.040(6) 0.034(5) 0.055(6) 0.015(5) -0.008(5) -0.012(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 C1 O2 1.246(12) . ? C1 O1 1.297(12) . ? C1 C2 1.472(13) . ? C2 C7 1.374(14) . ? C2 C3 1.386(13) . ? C3 C4 1.416(13) . ? C3 H3 0.9500 . ? C4 C5 1.370(14) . ? C4 H4 0.9500 . ? C5 C6 1.400(13) . ? C5 C22 1.476(13) . ? C6 C7 1.397(13) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O4 1.219(12) . ? C8 O3 1.273(11) . ? C8 C9 1.512(14) . ? C8 Cd1 2.663(11) 3_445 ? C9 C14 1.381(14) . ? C9 C10 1.398(14) . ? C10 C11 1.387(14) . ? C10 H10 0.9500 . ? C11 C12 1.383(12) . ? C11 H11 0.9500 . ? C12 C13 1.415(14) . ? C12 C24 1.468(14) . ? C13 C14 1.332(15) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O5 1.264(12) . ? C15 O6 1.315(11) . ? C15 C16 1.498(13) . ? C16 C21 1.376(13) . ? C16 C17 1.394(14) . ? C17 C18 1.383(14) . ? C17 H17 0.9500 . ? C18 C19 1.395(13) . ? C18 H18 0.9500 . ? C19 C20 1.391(13) . ? C19 C26 1.479(13) . ? C20 C21 1.379(13) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.386(14) . ? C22 C23 1.389(13) . ? C23 C24 1.404(13) . ? C23 H23 0.9500 . ? C24 C25 1.393(13) . ? C25 C26 1.392(14) . ? C25 H25 0.9500 . ? C26 C27 1.399(13) . ? C27 H27 0.9500 . ? C28 N1 1.316(12) . ? C28 N2 1.318(13) . ? C28 H28 0.9500 . ? C29 C30 1.367(15) . ? C29 N2 1.408(13) . ? C29 H29 0.9500 . ? C30 N1 1.374(13) . ? C30 H30 0.9500 . ? C31 N3 1.309(13) . ? C31 N4 1.359(13) . ? C31 H31 0.9500 . ? C32 C33 1.350(15) . ? C32 N4 1.356(14) . ? C32 H32 0.9500 . ? C33 N3 1.375(14) . ? C33 H33 0.9500 . ? C34 N2 1.462(12) . ? C34 C35 1.527(14) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.525(14) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.507(14) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 N4 1.482(13) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N5 1.301(13) . ? C38 N6 1.335(12) . ? C38 H38 0.9500 . ? C39 N6 1.363(13) . ? C39 C40 1.365(15) . ? C39 H39 0.9500 . ? C40 N5 1.405(13) . ? C40 H40 0.9500 . ? C41 N6 1.469(12) . ? C41 C42 1.510(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C42 1.541(18) 7_576 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? Cd1 N1 2.220(9) . ? Cd1 O6 2.249(6) 1_565 ? Cd1 O4 2.306(7) 3 ? Cd1 O2 2.375(7) . ? Cd1 O3 2.403(7) 3 ? Cd1 O1 2.457(7) . ? Cd1 C8 2.663(11) 3 ? Cd2 N5 2.321(9) 2_656 ? Cd2 N5 2.321(9) . ? Cd2 N3 2.339(9) . ? Cd2 N3 2.339(9) 2_656 ? Cd2 O1W 2.353(7) . ? Cd2 O1W 2.353(7) 2_656 ? O3 Cd1 2.403(7) 3_445 ? O4 Cd1 2.306(7) 3_445 ? O6 Cd1 2.250(7) 1_545 ? O1W H1A 0.8457 . ? O1W H1B 0.8434 . ? O2W H2A 0.8493 . ? O2W H2B 0.8497 . ? O3W H3A 0.8614 . ? O3W H3B 0.8525 . ? 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 O2 C1 O1 121.2(9) . . ? O2 C1 C2 120.2(9) . . ? O1 C1 C2 118.6(10) . . ? C7 C2 C3 119.8(9) . . ? C7 C2 C1 120.7(9) . . ? C3 C2 C1 119.4(9) . . ? C2 C3 C4 119.1(10) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 122.1(10) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 117.1(10) . . ? C4 C5 C22 121.6(9) . . ? C6 C5 C22 121.2(10) . . ? C7 C6 C5 121.6(10) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C2 C7 C6 120.1(10) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? O4 C8 O3 124.0(10) . . ? O4 C8 C9 117.4(9) . . ? O3 C8 C9 118.6(9) . . ? O4 C8 Cd1 59.8(6) . 3_445 ? O3 C8 Cd1 64.3(5) . 3_445 ? C9 C8 Cd1 174.3(7) . 3_445 ? C14 C9 C10 116.5(10) . . ? C14 C9 C8 120.7(10) . . ? C10 C9 C8 122.8(9) . . ? C11 C10 C9 121.4(10) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C12 C11 C10 119.8(10) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 118.5(10) . . ? C11 C12 C24 122.6(9) . . ? C13 C12 C24 118.8(9) . . ? C14 C13 C12 119.8(10) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C9 123.7(11) . . ? C13 C14 H14 118.2 . . ? C9 C14 H14 118.2 . . ? O5 C15 O6 122.6(9) . . ? O5 C15 C16 120.9(9) . . ? O6 C15 C16 116.5(9) . . ? C21 C16 C17 118.7(9) . . ? C21 C16 C15 120.5(10) . . ? C17 C16 C15 120.7(9) . . ? C18 C17 C16 120.5(10) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.8(10) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 117.7(9) . . ? C20 C19 C26 121.5(9) . . ? C18 C19 C26 120.8(9) . . ? C21 C20 C19 121.4(10) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C16 C21 C20 120.7(10) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C27 C22 C23 120.1(9) . . ? C27 C22 C5 120.2(9) . . ? C23 C22 C5 119.7(9) . . ? C22 C23 C24 120.8(9) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 117.5(9) . . ? C25 C24 C12 122.9(9) . . ? C23 C24 C12 119.5(9) . . ? C26 C25 C24 122.9(9) . . ? C26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C25 C26 C27 117.9(9) . . ? C25 C26 C19 119.9(9) . . ? C27 C26 C19 122.2(10) . . ? C22 C27 C26 120.8(10) . . ? C22 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? N1 C28 N2 114.0(10) . . ? N1 C28 H28 123.0 . . ? N2 C28 H28 123.0 . . ? C30 C29 N2 104.9(10) . . ? C30 C29 H29 127.6 . . ? N2 C29 H29 127.6 . . ? C29 C30 N1 110.5(10) . . ? C29 C30 H30 124.8 . . ? N1 C30 H30 124.8 . . ? N3 C31 N4 110.6(11) . . ? N3 C31 H31 124.7 . . ? N4 C31 H31 124.7 . . ? C33 C32 N4 106.7(11) . . ? C33 C32 H32 126.6 . . ? N4 C32 H32 126.6 . . ? C32 C33 N3 109.3(12) . . ? C32 C33 H33 125.4 . . ? N3 C33 H33 125.4 . . ? N2 C34 C35 111.1(9) . . ? N2 C34 H34A 109.4 . . ? C35 C34 H34A 109.4 . . ? N2 C34 H34B 109.4 . . ? C35 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 111.5(9) . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C34 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C37 C36 C35 111.9(9) . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N4 C37 C36 112.9(9) . . ? N4 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? N4 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? N5 C38 N6 114.6(10) . . ? N5 C38 H38 122.7 . . ? N6 C38 H38 122.7 . . ? N6 C39 C40 106.1(10) . . ? N6 C39 H39 127.0 . . ? C40 C39 H39 127.0 . . ? C39 C40 N5 109.8(11) . . ? C39 C40 H40 125.1 . . ? N5 C40 H40 125.1 . . ? N6 C41 C42 113.5(9) . . ? N6 C41 H41A 108.9 . . ? C42 C41 H41A 108.9 . . ? N6 C41 H41B 108.9 . . ? C42 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C41 C42 C42 111.2(11) . 7_576 ? C41 C42 H42A 109.4 . . ? C42 C42 H42A 109.4 7_576 . ? C41 C42 H42B 109.4 . . ? C42 C42 H42B 109.4 7_576 . ? H42A C42 H42B 108.0 . . ? N1 Cd1 O6 107.7(3) . 1_565 ? N1 Cd1 O4 90.8(3) . 3 ? O6 Cd1 O4 127.3(2) 1_565 3 ? N1 Cd1 O2 95.3(3) . . ? O6 Cd1 O2 135.9(3) 1_565 . ? O4 Cd1 O2 88.3(2) 3 . ? N1 Cd1 O3 145.4(3) . 3 ? O6 Cd1 O3 89.6(2) 1_565 3 ? O4 Cd1 O3 55.7(2) 3 3 ? O2 Cd1 O3 92.1(2) . 3 ? N1 Cd1 O1 93.7(3) . . ? O6 Cd1 O1 86.2(2) 1_565 . ? O4 Cd1 O1 142.8(2) 3 . ? O2 Cd1 O1 54.5(2) . . ? O3 Cd1 O1 117.7(2) 3 . ? N1 Cd1 C8 117.8(3) . 3 ? O6 Cd1 C8 111.2(3) 1_565 3 ? O4 Cd1 C8 27.2(3) 3 3 ? O2 Cd1 C8 88.9(3) . 3 ? O3 Cd1 C8 28.5(3) 3 3 ? O1 Cd1 C8 134.7(3) . 3 ? N5 Cd2 N5 90.9(4) 2_656 . ? N5 Cd2 N3 174.9(3) 2_656 . ? N5 Cd2 N3 92.0(3) . . ? N5 Cd2 N3 92.0(3) 2_656 2_656 ? N5 Cd2 N3 174.9(3) . 2_656 ? N3 Cd2 N3 85.3(4) . 2_656 ? N5 Cd2 O1W 89.6(3) 2_656 . ? N5 Cd2 O1W 88.7(3) . . ? N3 Cd2 O1W 86.3(3) . . ? N3 Cd2 O1W 95.5(3) 2_656 . ? N5 Cd2 O1W 88.7(3) 2_656 2_656 ? N5 Cd2 O1W 89.6(3) . 2_656 ? N3 Cd2 O1W 95.5(3) . 2_656 ? N3 Cd2 O1W 86.3(3) 2_656 2_656 ? O1W Cd2 O1W 177.6(3) . 2_656 ? C28 N1 C30 104.5(9) . . ? C28 N1 Cd1 122.2(7) . . ? C30 N1 Cd1 133.3(7) . . ? C28 N2 C29 106.1(9) . . ? C28 N2 C34 126.9(9) . . ? C29 N2 C34 126.5(9) . . ? C31 N3 C33 106.2(10) . . ? C31 N3 Cd2 128.7(8) . . ? C33 N3 Cd2 124.5(8) . . ? C32 N4 C31 107.2(9) . . ? C32 N4 C37 125.6(10) . . ? C31 N4 C37 127.1(10) . . ? C38 N5 C40 103.0(9) . . ? C38 N5 Cd2 133.2(8) . . ? C40 N5 Cd2 123.5(7) . . ? C38 N6 C39 106.4(9) . . ? C38 N6 C41 127.5(9) . . ? C39 N6 C41 126.0(9) . . ? C1 O1 Cd1 89.6(6) . . ? C1 O2 Cd1 94.6(6) . . ? C8 O3 Cd1 87.1(6) . 3_445 ? C8 O4 Cd1 93.0(6) . 3_445 ? C15 O6 Cd1 102.7(6) . 1_545 ? Cd2 O1W H1A 113.6 . . ? Cd2 O1W H1B 113.8 . . ? H1A O1W H1B 111.3 . . ? H2A O2W H2B 100.5 . . ? H3A O3W H3B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -154.3(10) . . . . ? O1 C1 C2 C7 27.2(15) . . . . ? O2 C1 C2 C3 29.3(16) . . . . ? O1 C1 C2 C3 -149.2(10) . . . . ? C7 C2 C3 C4 0.1(16) . . . . ? C1 C2 C3 C4 176.5(10) . . . . ? C2 C3 C4 C5 1.9(17) . . . . ? C3 C4 C5 C6 -1.7(16) . . . . ? C3 C4 C5 C22 -178.9(10) . . . . ? C4 C5 C6 C7 -0.5(15) . . . . ? C22 C5 C6 C7 176.7(10) . . . . ? C3 C2 C7 C6 -2.2(16) . . . . ? C1 C2 C7 C6 -178.6(10) . . . . ? C5 C6 C7 C2 2.5(16) . . . . ? O4 C8 C9 C14 25.0(14) . . . . ? O3 C8 C9 C14 -154.7(9) . . . . ? Cd1 C8 C9 C14 -35(8) 3_445 . . . ? O4 C8 C9 C10 -153.1(10) . . . . ? O3 C8 C9 C10 27.2(14) . . . . ? Cd1 C8 C9 C10 147(7) 3_445 . . . ? C14 C9 C10 C11 -5.6(15) . . . . ? C8 C9 C10 C11 172.6(9) . . . . ? C9 C10 C11 C12 3.6(15) . . . . ? C10 C11 C12 C13 1.2(14) . . . . ? C10 C11 C12 C24 -176.7(9) . . . . ? C11 C12 C13 C14 -3.7(15) . . . . ? C24 C12 C13 C14 174.2(10) . . . . ? C12 C13 C14 C9 1.6(17) . . . . ? C10 C9 C14 C13 3.0(16) . . . . ? C8 C9 C14 C13 -175.2(10) . . . . ? O5 C15 C16 C21 17.7(16) . . . . ? O6 C15 C16 C21 -163.4(10) . . . . ? O5 C15 C16 C17 -158.6(10) . . . . ? O6 C15 C16 C17 20.2(15) . . . . ? C21 C16 C17 C18 -4.0(16) . . . . ? C15 C16 C17 C18 172.4(10) . . . . ? C16 C17 C18 C19 3.4(16) . . . . ? C17 C18 C19 C20 -0.6(16) . . . . ? C17 C18 C19 C26 -178.5(10) . . . . ? C18 C19 C20 C21 -1.5(15) . . . . ? C26 C19 C20 C21 176.4(10) . . . . ? C17 C16 C21 C20 2.0(16) . . . . ? C15 C16 C21 C20 -174.5(9) . . . . ? C19 C20 C21 C16 0.8(16) . . . . ? C4 C5 C22 C27 -39.8(15) . . . . ? C6 C5 C22 C27 143.1(10) . . . . ? C4 C5 C22 C23 137.9(11) . . . . ? C6 C5 C22 C23 -39.1(14) . . . . ? C27 C22 C23 C24 2.7(16) . . . . ? C5 C22 C23 C24 -175.0(9) . . . . ? C22 C23 C24 C25 -2.2(15) . . . . ? C22 C23 C24 C12 174.9(9) . . . . ? C11 C12 C24 C25 -129.9(11) . . . . ? C13 C12 C24 C25 52.2(14) . . . . ? C11 C12 C24 C23 53.0(14) . . . . ? C13 C12 C24 C23 -124.8(11) . . . . ? C23 C24 C25 C26 1.8(15) . . . . ? C12 C24 C25 C26 -175.3(9) . . . . ? C24 C25 C26 C27 -1.7(16) . . . . ? C24 C25 C26 C19 176.0(9) . . . . ? C20 C19 C26 C25 -154.8(10) . . . . ? C18 C19 C26 C25 23.0(15) . . . . ? C20 C19 C26 C27 22.8(16) . . . . ? C18 C19 C26 C27 -159.4(10) . . . . ? C23 C22 C27 C26 -2.7(15) . . . . ? C5 C22 C27 C26 175.1(9) . . . . ? C25 C26 C27 C22 2.1(15) . . . . ? C19 C26 C27 C22 -175.5(9) . . . . ? N2 C29 C30 N1 -1.0(12) . . . . ? N4 C32 C33 N3 0.4(14) . . . . ? N2 C34 C35 C36 176.7(9) . . . . ? C34 C35 C36 C37 -75.3(13) . . . . ? C35 C36 C37 N4 177.5(10) . . . . ? N6 C39 C40 N5 0.1(14) . . . . ? N6 C41 C42 C42 178.3(10) . . . 7_576 ? N2 C28 N1 C30 1.5(12) . . . . ? N2 C28 N1 Cd1 178.8(7) . . . . ? C29 C30 N1 C28 -0.2(12) . . . . ? C29 C30 N1 Cd1 -177.0(8) . . . . ? O6 Cd1 N1 C28 -76.1(8) 1_565 . . . ? O4 Cd1 N1 C28 53.7(8) 3 . . . ? O2 Cd1 N1 C28 142.0(8) . . . . ? O3 Cd1 N1 C28 40.6(10) 3 . . . ? O1 Cd1 N1 C28 -163.3(8) . . . . ? C8 Cd1 N1 C28 50.5(9) 3 . . . ? O6 Cd1 N1 C30 100.3(9) 1_565 . . . ? O4 Cd1 N1 C30 -129.9(9) 3 . . . ? O2 Cd1 N1 C30 -41.6(10) . . . . ? O3 Cd1 N1 C30 -143.0(8) 3 . . . ? O1 Cd1 N1 C30 13.1(9) . . . . ? C8 Cd1 N1 C30 -133.1(9) 3 . . . ? N1 C28 N2 C29 -2.2(13) . . . . ? N1 C28 N2 C34 -174.6(10) . . . . ? C30 C29 N2 C28 1.8(12) . . . . ? C30 C29 N2 C34 174.3(10) . . . . ? C35 C34 N2 C28 -52.3(14) . . . . ? C35 C34 N2 C29 136.8(11) . . . . ? N4 C31 N3 C33 1.7(13) . . . . ? N4 C31 N3 Cd2 172.9(6) . . . . ? C32 C33 N3 C31 -1.3(13) . . . . ? C32 C33 N3 Cd2 -173.0(7) . . . . ? N5 Cd2 N3 C31 -145(3) 2_656 . . . ? N5 Cd2 N3 C31 89.5(9) . . . . ? N3 Cd2 N3 C31 -86.2(9) 2_656 . . . ? O1W Cd2 N3 C31 178.0(9) . . . . ? O1W Cd2 N3 C31 -0.3(9) 2_656 . . . ? N5 Cd2 N3 C33 25(4) 2_656 . . . ? N5 Cd2 N3 C33 -100.8(9) . . . . ? N3 Cd2 N3 C33 83.6(9) 2_656 . . . ? O1W Cd2 N3 C33 -12.2(9) . . . . ? O1W Cd2 N3 C33 169.4(9) 2_656 . . . ? C33 C32 N4 C31 0.6(13) . . . . ? C33 C32 N4 C37 179.7(10) . . . . ? N3 C31 N4 C32 -1.5(13) . . . . ? N3 C31 N4 C37 179.4(10) . . . . ? C36 C37 N4 C32 -60.1(15) . . . . ? C36 C37 N4 C31 118.9(12) . . . . ? N6 C38 N5 C40 -0.2(13) . . . . ? N6 C38 N5 Cd2 -174.8(7) . . . . ? C39 C40 N5 C38 0.1(13) . . . . ? C39 C40 N5 Cd2 175.3(8) . . . . ? N5 Cd2 N5 C38 139.4(12) 2_656 . . . ? N3 Cd2 N5 C38 -44.7(11) . . . . ? N3 Cd2 N5 C38 14(4) 2_656 . . . ? O1W Cd2 N5 C38 -131.0(11) . . . . ? O1W Cd2 N5 C38 50.7(11) 2_656 . . . ? N5 Cd2 N5 C40 -34.2(7) 2_656 . . . ? N3 Cd2 N5 C40 141.6(9) . . . . ? N3 Cd2 N5 C40 -160(3) 2_656 . . . ? O1W Cd2 N5 C40 55.3(9) . . . . ? O1W Cd2 N5 C40 -123.0(9) 2_656 . . . ? N5 C38 N6 C39 0.3(14) . . . . ? N5 C38 N6 C41 179.9(10) . . . . ? C40 C39 N6 C38 -0.2(13) . . . . ? C40 C39 N6 C41 -179.9(10) . . . . ? C42 C41 N6 C38 123.5(11) . . . . ? C42 C41 N6 C39 -56.9(14) . . . . ? O2 C1 O1 Cd1 -3.2(11) . . . . ? C2 C1 O1 Cd1 175.3(9) . . . . ? N1 Cd1 O1 C1 -92.1(6) . . . . ? O6 Cd1 O1 C1 160.4(6) 1_565 . . . ? O4 Cd1 O1 C1 4.2(8) 3 . . . ? O2 Cd1 O1 C1 1.8(6) . . . . ? O3 Cd1 O1 C1 72.9(6) 3 . . . ? C8 Cd1 O1 C1 44.1(7) 3 . . . ? O1 C1 O2 Cd1 3.4(11) . . . . ? C2 C1 O2 Cd1 -175.1(9) . . . . ? N1 Cd1 O2 C1 89.0(7) . . . . ? O6 Cd1 O2 C1 -33.4(8) 1_565 . . . ? O4 Cd1 O2 C1 179.6(7) 3 . . . ? O3 Cd1 O2 C1 -124.9(7) 3 . . . ? O1 Cd1 O2 C1 -1.9(6) . . . . ? C8 Cd1 O2 C1 -153.2(7) 3 . . . ? O4 C8 O3 Cd1 -5.1(10) . . . 3_445 ? C9 C8 O3 Cd1 174.5(8) . . . 3_445 ? O3 C8 O4 Cd1 5.4(10) . . . 3_445 ? C9 C8 O4 Cd1 -174.3(8) . . . 3_445 ? O5 C15 O6 Cd1 6.3(12) . . . 1_545 ? C16 C15 O6 Cd1 -172.5(7) . . . 1_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3W H3B O1 0.85 2.06 2.879(10) 160.2 . O3W H3A O6 0.86 2.06 2.739(10) 135.1 1_565 O2W H2B O2 0.85 2.32 3.041(10) 142.2 . O1W H1B O1 0.84 2.24 2.932(11) 139.2 7_566 O1W H1A O3W 0.85 2.07 2.682(11) 129.2 3_556 O2W H2A O5 0.85 2.16 3.013(10) 179.5 4 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.196 _refine_diff_density_min -1.523 _refine_diff_density_rms 0.175 # start Validation Reply Form _vrf_PLAT601_4 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 64.00 A**3 RESPONSE: One and half water molecules can not be detected from different Fourier map due to weak diffraction data and lack of higher angle reflections. ; # end Validation Reply Form