# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jubaraj Bikash Baruah' _publ_contact_author_email juba@iitg.ernet.in loop_ _publ_author_name J.Baruah B.Nath # Attachment '- complex 4.cif' data_bkn _database_code_depnum_ccdc_archive 'CCDC 806671' #TrackingRef '- complex 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H41 Cd N3 O9' _chemical_formula_weight 844.18 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 16.3357(5) _cell_length_b 14.1196(5) _cell_length_c 18.3475(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.841(2) _cell_angle_gamma 90.00 _cell_volume 4090.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5607 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42136 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7341 _reflns_number_gt 4341 _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^)+(0.0450P)^2^+0.5000P] 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 7341 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 0.820 _refine_ls_restrained_S_all 0.820 _refine_ls_shift/su_max 0.005 _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 0.7648(2) 0.5606(3) 0.1851(2) 0.0481(10) Uani 1 1 d . . . C2 C 0.6973(2) 0.4912(3) 0.1959(2) 0.0520(10) Uani 1 1 d . . . H2A H 0.6420 0.5209 0.1801 0.062 Uiso 1 1 calc R . . H2B H 0.6971 0.4359 0.1646 0.062 Uiso 1 1 calc R . . C3 C 0.6413(2) 0.4545(2) 0.30152(18) 0.0386(8) Uani 1 1 d . . . C4 C 0.5988(2) 0.5352(3) 0.31513(19) 0.0440(9) Uani 1 1 d . . . C5 C 0.5312(2) 0.5231(3) 0.34712(19) 0.0524(10) Uani 1 1 d . . . H5 H 0.5025 0.5764 0.3574 0.063 Uiso 1 1 calc R . . C6 C 0.5052(2) 0.4352(3) 0.3642(2) 0.0501(10) Uani 1 1 d . . . C7 C 0.5502(2) 0.3566(3) 0.35079(19) 0.0441(9) Uani 1 1 d . . . H7 H 0.5336 0.2967 0.3625 0.053 Uiso 1 1 calc R . . C8 C 0.6190(2) 0.3647(2) 0.32051(18) 0.0383(8) Uani 1 1 d . . . C9 C 0.6249(2) 0.6334(3) 0.2974(2) 0.0655(12) Uani 1 1 d . . . H9A H 0.6854 0.6363 0.3071 0.098 Uiso 1 1 calc R . . H9B H 0.6060 0.6788 0.3285 0.098 Uiso 1 1 calc R . . H9C H 0.5998 0.6475 0.2453 0.098 Uiso 1 1 calc R . . C10 C 0.4295(3) 0.4252(3) 0.3967(3) 0.0857(15) Uani 1 1 d . . . H10A H 0.3958 0.4818 0.3866 0.129 Uiso 1 1 calc R . . H10B H 0.4485 0.4157 0.4502 0.129 Uiso 1 1 calc R . . H10C H 0.3960 0.3720 0.3740 0.129 Uiso 1 1 calc R . . C11 C 0.6675(2) 0.2788(2) 0.30343(18) 0.0387(8) Uani 1 1 d . . . H11 H 0.7276 0.2961 0.3175 0.046 Uiso 1 1 calc R . . C12 C 0.6582(2) 0.1932(2) 0.3514(2) 0.0435(9) Uani 1 1 d . . . C13 C 0.7063(2) 0.1880(3) 0.4250(2) 0.0580(11) Uani 1 1 d . . . H13 H 0.7468 0.2343 0.4434 0.070 Uiso 1 1 calc R . . C14 C 0.6951(3) 0.1149(3) 0.4719(2) 0.0735(13) Uani 1 1 d . . . H14 H 0.7276 0.1131 0.5215 0.088 Uiso 1 1 calc R . . C15 C 0.6370(3) 0.0458(3) 0.4461(3) 0.0783(14) Uani 1 1 d . . . H15 H 0.6296 -0.0032 0.4777 0.094 Uiso 1 1 calc R . . C16 C 0.5896(3) 0.0493(3) 0.3732(3) 0.0780(14) Uani 1 1 d . . . H16 H 0.5498 0.0022 0.3551 0.094 Uiso 1 1 calc R . . C17 C 0.6000(2) 0.1219(3) 0.3261(2) 0.0588(11) Uani 1 1 d . . . H17 H 0.5674 0.1228 0.2765 0.071 Uiso 1 1 calc R . . C18 C 0.6443(2) 0.2573(2) 0.21893(19) 0.0383(8) Uani 1 1 d . . . C19 C 0.5672(2) 0.2834(2) 0.1722(2) 0.0409(9) Uani 1 1 d . . . H19 H 0.5290 0.3162 0.1928 0.049 Uiso 1 1 calc R . . C20 C 0.5445(2) 0.2626(3) 0.0960(2) 0.0463(9) Uani 1 1 d . . . C21 C 0.5998(2) 0.2118(3) 0.0667(2) 0.0504(10) Uani 1 1 d . . . H21 H 0.5843 0.1954 0.0159 0.061 Uiso 1 1 calc R . . C22 C 0.6783(2) 0.1841(3) 0.1106(2) 0.0467(9) Uani 1 1 d . . . C23 C 0.7003(2) 0.2088(2) 0.1860(2) 0.0410(9) Uani 1 1 d . . . C24 C 0.4612(2) 0.2974(3) 0.0463(2) 0.0747(13) Uani 1 1 d . . . H24A H 0.4713 0.3504 0.0169 0.112 Uiso 1 1 calc R . . H24B H 0.4248 0.3166 0.0772 0.112 Uiso 1 1 calc R . . H24C H 0.4346 0.2474 0.0132 0.112 Uiso 1 1 calc R . . C25 C 0.7378(3) 0.1272(3) 0.0766(2) 0.0749(13) Uani 1 1 d . . . H25A H 0.7875 0.1640 0.0776 0.112 Uiso 1 1 calc R . . H25B H 0.7099 0.1114 0.0253 0.112 Uiso 1 1 calc R . . H25C H 0.7538 0.0701 0.1051 0.112 Uiso 1 1 calc R . . C26 C 0.8424(2) 0.2567(3) 0.2302(2) 0.0650(12) Uani 1 1 d . . . H26A H 0.8295 0.3120 0.2565 0.078 Uiso 1 1 calc R . . H26B H 0.8393 0.2749 0.1786 0.078 Uiso 1 1 calc R . . C27 C 0.9321(2) 0.2227(3) 0.2681(2) 0.0541(10) Uani 1 1 d . . . C28 C 0.8475(3) 0.8824(3) 0.2227(2) 0.0682(12) Uani 1 1 d . . . H28 H 0.8717 0.9006 0.1842 0.082 Uiso 1 1 calc R . . C29 C 0.8111(3) 0.9510(3) 0.2579(3) 0.0837(15) Uani 1 1 d . . . H29 H 0.8101 1.0139 0.2427 0.100 Uiso 1 1 calc R . . C30 C 0.7764(3) 0.9251(4) 0.3159(3) 0.0972(17) Uani 1 1 d . . . H30 H 0.7508 0.9696 0.3401 0.117 Uiso 1 1 calc R . . C31 C 0.7807(3) 0.8323(4) 0.3366(3) 0.0958(18) Uani 1 1 d . . . H31 H 0.7587 0.8122 0.3760 0.115 Uiso 1 1 calc R . . C32 C 0.8179(3) 0.7689(3) 0.2984(2) 0.0715(13) Uani 1 1 d . . . H32 H 0.8213 0.7059 0.3136 0.086 Uiso 1 1 calc R . . C33 C 0.7700(2) 0.8000(3) 0.0416(2) 0.0573(11) Uani 1 1 d . . . H33 H 0.7309 0.7701 0.0628 0.069 Uiso 1 1 calc R . . C34 C 0.7423(3) 0.8714(3) -0.0096(2) 0.0643(11) Uani 1 1 d . . . H34 H 0.6859 0.8904 -0.0221 0.077 Uiso 1 1 calc R . . C35 C 0.8001(3) 0.9141(3) -0.0418(2) 0.0708(13) Uani 1 1 d . . . H35 H 0.7833 0.9628 -0.0765 0.085 Uiso 1 1 calc R . . C36 C 0.8823(3) 0.8844(3) -0.0224(2) 0.0655(12) Uani 1 1 d . . . H36 H 0.9222 0.9114 -0.0443 0.079 Uiso 1 1 calc R . . C37 C 0.9044(2) 0.8145(3) 0.0295(2) 0.0520(10) Uani 1 1 d . . . H37 H 0.9608 0.7954 0.0432 0.062 Uiso 1 1 calc R . . C38 C 0.8951(3) 0.5334(3) 0.0285(3) 0.0703(12) Uani 1 1 d . . . H38 H 0.8698 0.5854 0.0006 0.084 Uiso 1 1 calc R . . C39 C 0.8989(3) 0.4485(4) -0.0092(3) 0.0883(15) Uani 1 1 d . . . H39 H 0.8779 0.4444 -0.0613 0.106 Uiso 1 1 calc R . . C40 C 0.9346(3) 0.3705(4) 0.0325(4) 0.0888(16) Uani 1 1 d . . . H40 H 0.9367 0.3121 0.0096 0.107 Uiso 1 1 calc R . . C41 C 0.9665(3) 0.3815(4) 0.1083(3) 0.0812(14) Uani 1 1 d . . . H41 H 0.9917 0.3307 0.1378 0.097 Uiso 1 1 calc R . . C42 C 0.9613(2) 0.4682(3) 0.1407(3) 0.0665(12) Uani 1 1 d . . . H42 H 0.9839 0.4743 0.1924 0.080 Uiso 1 1 calc R . . Cd1 Cd 0.897101(16) 0.675141(19) 0.168709(15) 0.04626(11) Uani 1 1 d . . . N1 N 0.84942(19) 0.7922(2) 0.24124(18) 0.0540(8) Uani 1 1 d . . . N2 N 0.85025(18) 0.7715(2) 0.06211(16) 0.0476(8) Uani 1 1 d . . . N3 N 0.9257(2) 0.5437(2) 0.1023(2) 0.0577(9) Uani 1 1 d . . . O1 O 0.83535(16) 0.56298(17) 0.23386(14) 0.0553(7) Uani 1 1 d . . . O2 O 0.74703(16) 0.6096(2) 0.12721(16) 0.0664(8) Uani 1 1 d . . . O3 O 0.71264(13) 0.46260(17) 0.27311(13) 0.0507(7) Uani 1 1 d . . . O4 O 0.78113(14) 0.18389(17) 0.23057(13) 0.0492(6) Uani 1 1 d . . . O5 O 0.95774(17) 0.1476(2) 0.25211(17) 0.0780(9) Uani 1 1 d . . . O6 O 0.97775(17) 0.2807(2) 0.30937(18) 0.0839(10) Uani 1 1 d . . . O7 O 0.0591(2) 0.5640(3) 0.38736(19) 0.1374(16) Uani 1 1 d . . . O8 O 0.07987(17) 0.94958(19) 0.14875(14) 0.0701(8) Uani 1 1 d . . . O9 O 0.1171(2) 0.8494(2) 0.0283(2) 0.1012(11) 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(2) 0.041(2) 0.064(3) -0.002(2) 0.029(2) -0.0040(19) C2 0.052(2) 0.055(3) 0.052(3) 0.001(2) 0.018(2) -0.011(2) C3 0.038(2) 0.041(2) 0.036(2) -0.0029(17) 0.0089(17) -0.0062(17) C4 0.049(2) 0.035(2) 0.045(2) 0.0005(18) 0.0065(19) -0.0010(18) C5 0.058(3) 0.051(3) 0.050(2) 0.003(2) 0.015(2) 0.015(2) C6 0.048(2) 0.059(3) 0.050(2) 0.007(2) 0.0248(19) 0.008(2) C7 0.045(2) 0.042(2) 0.049(2) 0.0071(18) 0.0184(19) -0.0007(18) C8 0.037(2) 0.038(2) 0.039(2) -0.0026(17) 0.0083(17) -0.0007(16) C9 0.070(3) 0.043(3) 0.084(3) 0.002(2) 0.020(2) -0.003(2) C10 0.079(3) 0.091(4) 0.108(4) 0.028(3) 0.061(3) 0.024(3) C11 0.034(2) 0.036(2) 0.046(2) -0.0062(18) 0.0098(17) -0.0034(16) C12 0.045(2) 0.039(2) 0.048(2) -0.0001(19) 0.0143(18) 0.0064(18) C13 0.062(3) 0.054(3) 0.053(3) -0.003(2) 0.007(2) -0.007(2) C14 0.093(4) 0.072(3) 0.055(3) 0.016(3) 0.018(3) 0.002(3) C15 0.097(4) 0.063(3) 0.078(4) 0.022(3) 0.031(3) -0.004(3) C16 0.087(3) 0.060(3) 0.082(4) 0.011(3) 0.013(3) -0.021(3) C17 0.060(3) 0.054(3) 0.057(3) 0.002(2) 0.006(2) -0.016(2) C18 0.036(2) 0.034(2) 0.048(2) 0.0030(17) 0.0154(18) -0.0032(16) C19 0.037(2) 0.039(2) 0.047(2) -0.0030(18) 0.0110(18) -0.0001(17) C20 0.041(2) 0.040(2) 0.056(3) 0.001(2) 0.0072(19) -0.0039(18) C21 0.054(3) 0.059(3) 0.040(2) -0.0033(19) 0.015(2) -0.004(2) C22 0.050(2) 0.047(2) 0.048(2) -0.002(2) 0.0207(19) 0.0006(19) C23 0.039(2) 0.036(2) 0.048(2) 0.0018(18) 0.0123(18) -0.0006(17) C24 0.060(3) 0.083(4) 0.067(3) -0.007(3) -0.009(2) 0.005(2) C25 0.075(3) 0.095(4) 0.061(3) -0.010(3) 0.030(2) 0.017(3) C26 0.040(2) 0.053(3) 0.097(3) 0.002(2) 0.010(2) -0.003(2) C27 0.042(2) 0.058(3) 0.061(3) -0.015(2) 0.011(2) 0.000(2) C28 0.078(3) 0.054(3) 0.071(3) 0.001(3) 0.015(2) -0.003(3) C29 0.097(4) 0.050(3) 0.092(4) 0.003(3) 0.002(3) 0.007(3) C30 0.086(4) 0.091(5) 0.119(5) -0.038(4) 0.035(4) -0.003(3) C31 0.118(4) 0.086(4) 0.103(4) -0.034(4) 0.064(4) -0.037(4) C32 0.100(4) 0.053(3) 0.071(3) -0.008(2) 0.040(3) -0.022(3) C33 0.049(3) 0.068(3) 0.055(3) 0.011(2) 0.014(2) -0.003(2) C34 0.056(3) 0.066(3) 0.065(3) 0.009(3) 0.004(2) 0.010(2) C35 0.087(4) 0.056(3) 0.060(3) 0.019(2) 0.002(3) -0.009(3) C36 0.060(3) 0.070(3) 0.066(3) 0.018(3) 0.015(2) -0.013(2) C37 0.048(2) 0.058(3) 0.052(2) 0.008(2) 0.0160(19) -0.002(2) C38 0.073(3) 0.062(3) 0.073(3) -0.002(3) 0.015(3) 0.005(2) C39 0.084(4) 0.095(5) 0.082(4) -0.026(3) 0.015(3) -0.009(3) C40 0.078(4) 0.063(4) 0.132(5) -0.026(4) 0.037(4) -0.005(3) C41 0.077(3) 0.068(4) 0.100(4) 0.011(3) 0.026(3) 0.015(3) C42 0.060(3) 0.068(3) 0.070(3) 0.005(3) 0.014(2) 0.011(2) Cd1 0.04107(17) 0.04476(18) 0.05277(19) 0.00957(15) 0.01167(12) -0.00554(14) N1 0.060(2) 0.042(2) 0.061(2) 0.0022(17) 0.0179(18) -0.0105(16) N2 0.0415(19) 0.051(2) 0.0504(19) 0.0088(16) 0.0120(16) -0.0033(16) N3 0.059(2) 0.057(2) 0.055(2) 0.0041(19) 0.0112(18) 0.0020(18) O1 0.0478(16) 0.0520(18) 0.0685(19) 0.0036(14) 0.0193(15) -0.0140(13) O2 0.0607(18) 0.070(2) 0.0709(19) 0.0260(17) 0.0212(15) -0.0064(15) O3 0.0384(14) 0.0565(17) 0.0587(17) 0.0112(14) 0.0150(13) -0.0050(12) O4 0.0384(14) 0.0458(16) 0.0617(16) 0.0011(13) 0.0099(12) 0.0058(12) O5 0.0641(19) 0.075(2) 0.086(2) -0.0138(18) 0.0034(16) 0.0306(16) O6 0.0530(18) 0.092(3) 0.096(2) -0.028(2) -0.0006(17) 0.0069(17) O7 0.121(3) 0.197(5) 0.086(3) 0.024(3) 0.011(2) -0.073(3) O8 0.083(2) 0.063(2) 0.0617(18) 0.0027(15) 0.0122(15) 0.0021(16) O9 0.111(3) 0.074(2) 0.140(3) -0.005(2) 0.073(2) 0.0058(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.239(4) . ? C1 O1 1.265(4) . ? C1 C2 1.525(5) . ? C2 O3 1.432(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.388(4) . ? C3 C4 1.390(5) . ? C3 O3 1.398(4) . ? C4 C5 1.388(4) . ? C4 C9 1.510(5) . ? C5 C6 1.375(5) . ? C5 H5 0.9300 . ? C6 C7 1.388(5) . ? C6 C10 1.510(5) . ? C7 C8 1.379(4) . ? C7 H7 0.9300 . ? C8 C11 1.524(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.526(5) . ? C11 C18 1.529(5) . ? C11 H11 0.9800 . ? C12 C13 1.380(5) . ? C12 C17 1.380(5) . ? C13 C14 1.386(5) . ? C13 H13 0.9300 . ? C14 C15 1.359(6) . ? C14 H14 0.9300 . ? C15 C16 1.363(6) . ? C15 H15 0.9300 . ? C16 C17 1.380(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.381(4) . ? C18 C23 1.397(4) . ? C19 C20 1.384(5) . ? C19 H19 0.9300 . ? C20 C21 1.368(5) . ? C20 C24 1.513(5) . ? C21 C22 1.384(5) . ? C21 H21 0.9300 . ? C22 C23 1.382(5) . ? C22 C25 1.513(5) . ? C23 O4 1.409(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O4 1.436(4) . ? C26 C27 1.529(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O5 1.204(4) . ? C27 O6 1.228(4) . ? C28 N1 1.316(5) . ? C28 C29 1.381(6) . ? C28 H28 0.9300 . ? C29 C30 1.377(6) . ? C29 H29 0.9300 . ? C30 C31 1.361(7) . ? C30 H30 0.9300 . ? C31 C32 1.372(6) . ? C31 H31 0.9300 . ? C32 N1 1.322(5) . ? C32 H32 0.9300 . ? C33 N2 1.330(4) . ? C33 C34 1.373(5) . ? C33 H33 0.9300 . ? C34 C35 1.376(5) . ? C34 H34 0.9300 . ? C35 C36 1.364(5) . ? C35 H35 0.9300 . ? C36 C37 1.354(5) . ? C36 H36 0.9300 . ? C37 N2 1.335(4) . ? C37 H37 0.9300 . ? C38 N3 1.324(5) . ? C38 C39 1.394(6) . ? C38 H38 0.9300 . ? C39 C40 1.382(6) . ? C39 H39 0.9300 . ? C40 C41 1.363(6) . ? C40 H40 0.9300 . ? C41 C42 1.372(6) . ? C41 H41 0.9300 . ? C42 N3 1.328(5) . ? C42 H42 0.9300 . ? Cd1 N3 2.333(3) . ? Cd1 N2 2.344(3) . ? Cd1 O1 2.360(2) . ? Cd1 N1 2.375(3) . ? Cd1 O5 2.474(3) 2_755 ? Cd1 O6 2.478(3) 2_755 ? Cd1 O2 2.548(3) . ? O5 Cd1 2.474(3) 2_745 ? O6 Cd1 2.478(3) 2_745 ? 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 124.2(3) . . ? O2 C1 C2 116.9(4) . . ? O1 C1 C2 118.9(4) . . ? O3 C2 C1 111.1(3) . . ? O3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? O3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C8 C3 C4 121.9(3) . . ? C8 C3 O3 117.8(3) . . ? C4 C3 O3 120.1(3) . . ? C5 C4 C3 117.6(3) . . ? C5 C4 C9 120.2(3) . . ? C3 C4 C9 122.2(3) . . ? C6 C5 C4 122.3(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 118.2(3) . . ? C5 C6 C10 120.4(3) . . ? C7 C6 C10 121.4(4) . . ? C8 C7 C6 121.9(3) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C3 118.0(3) . . ? C7 C8 C11 122.5(3) . . ? C3 C8 C11 119.4(3) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 C12 112.2(3) . . ? C8 C11 C18 111.1(3) . . ? C12 C11 C18 113.0(3) . . ? C8 C11 H11 106.7 . . ? C12 C11 H11 106.7 . . ? C18 C11 H11 106.7 . . ? C13 C12 C17 117.4(4) . . ? C13 C12 C11 119.4(3) . . ? C17 C12 C11 123.1(3) . . ? C12 C13 C14 121.0(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.1(4) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.4 . . ? C15 C16 C17 120.7(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 121.1(4) . . ? C16 C17 H17 119.4 . . ? C12 C17 H17 119.4 . . ? C19 C18 C23 117.2(3) . . ? C19 C18 C11 121.7(3) . . ? C23 C18 C11 121.1(3) . . ? C18 C19 C20 122.4(3) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C21 C20 C19 118.4(3) . . ? C21 C20 C24 121.1(4) . . ? C19 C20 C24 120.5(3) . . ? C20 C21 C22 121.8(3) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C23 C22 C21 118.4(3) . . ? C23 C22 C25 121.2(3) . . ? C21 C22 C25 120.5(3) . . ? C22 C23 C18 121.8(3) . . ? C22 C23 O4 118.8(3) . . ? C18 C23 O4 119.4(3) . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O4 C26 C27 111.2(3) . . ? O4 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? O4 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? O5 C27 O6 122.9(4) . . ? O5 C27 C26 121.2(4) . . ? O6 C27 C26 115.5(4) . . ? N1 C28 C29 122.8(4) . . ? N1 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C30 C29 C28 119.1(5) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C31 C30 C29 118.0(5) . . ? C31 C30 H30 121.0 . . ? C29 C30 H30 121.0 . . ? C30 C31 C32 118.8(5) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N1 C32 C31 123.9(4) . . ? N1 C32 H32 118.1 . . ? C31 C32 H32 118.1 . . ? N2 C33 C34 123.0(4) . . ? N2 C33 H33 118.5 . . ? C34 C33 H33 118.5 . . ? C33 C34 C35 118.2(4) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C36 C35 C34 119.5(4) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C37 C36 C35 118.3(4) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? N2 C37 C36 124.0(4) . . ? N2 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? N3 C38 C39 123.2(5) . . ? N3 C38 H38 118.4 . . ? C39 C38 H38 118.4 . . ? C40 C39 C38 118.5(5) . . ? C40 C39 H39 120.8 . . ? C38 C39 H39 120.8 . . ? C41 C40 C39 118.1(5) . . ? C41 C40 H40 121.0 . . ? C39 C40 H40 121.0 . . ? C40 C41 C42 119.6(5) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? N3 C42 C41 123.6(4) . . ? N3 C42 H42 118.2 . . ? C41 C42 H42 118.2 . . ? N3 Cd1 N2 95.27(11) . . ? N3 Cd1 O1 84.24(10) . . ? N2 Cd1 O1 136.16(10) . . ? N3 Cd1 N1 170.04(10) . . ? N2 Cd1 N1 88.85(11) . . ? O1 Cd1 N1 86.51(10) . . ? N3 Cd1 O5 83.78(11) . 2_755 ? N2 Cd1 O5 129.82(10) . 2_755 ? O1 Cd1 O5 93.83(9) . 2_755 ? N1 Cd1 O5 100.54(11) . 2_755 ? N3 Cd1 O6 107.21(11) . 2_755 ? N2 Cd1 O6 82.30(10) . 2_755 ? O1 Cd1 O6 139.73(10) . 2_755 ? N1 Cd1 O6 82.30(11) . 2_755 ? O5 Cd1 O6 51.12(9) 2_755 2_755 ? N3 Cd1 O2 82.01(10) . . ? N2 Cd1 O2 82.98(9) . . ? O1 Cd1 O2 53.44(8) . . ? N1 Cd1 O2 89.52(10) . . ? O5 Cd1 O2 145.35(9) 2_755 . ? O6 Cd1 O2 163.28(10) 2_755 . ? C28 N1 C32 117.2(4) . . ? C28 N1 Cd1 121.2(3) . . ? C32 N1 Cd1 121.4(3) . . ? C33 N2 C37 117.0(3) . . ? C33 N2 Cd1 120.0(2) . . ? C37 N2 Cd1 121.7(2) . . ? C38 N3 C42 117.0(4) . . ? C38 N3 Cd1 123.2(3) . . ? C42 N3 Cd1 118.7(3) . . ? C1 O1 Cd1 95.2(2) . . ? C1 O2 Cd1 87.2(2) . . ? C3 O3 C2 116.1(2) . . ? C23 O4 C26 111.7(3) . . ? C27 O5 Cd1 93.4(3) . 2_745 ? C27 O6 Cd1 92.6(3) . 2_745 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.438 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.074 # Attachment '- complex 8.cif' data_hgabp3no2_0m _database_code_depnum_ccdc_archive 'CCDC 837718' #TrackingRef '- complex 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H96 Hg2 N10 O20' _chemical_formula_weight 1990.91 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' Hg Hg -2.3894 9.2266 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7843(3) _cell_length_b 12.7257(4) _cell_length_c 19.1614(6) _cell_angle_alpha 90.829(2) _cell_angle_beta 97.845(2) _cell_angle_gamma 111.982(2) _cell_volume 2186.08(12) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.81 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1002 _exptl_absorpt_coefficient_mu 3.582 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3003 _exptl_absorpt_correction_T_max 0.5951 _exptl_absorpt_process_details 'North et al., 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29447 _diffrn_reflns_av_R_equivalents 0.0928 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7501 _reflns_number_gt 5716 _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^)+(0.0300P)^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 7501 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 Hg1 Hg 0.052942(19) 0.135551(16) -0.056490(9) 0.05891(9) Uani 1 1 d . . . O3 O -0.0095(3) 0.2813(2) 0.18856(14) 0.0458(7) Uani 1 1 d . . . O6 O 0.2266(3) 0.0933(2) 0.28925(15) 0.0511(7) Uani 1 1 d . . . O1 O -0.0632(4) 0.1010(3) 0.03817(17) 0.0752(10) Uani 1 1 d . . . O2 O 0.1325(4) 0.2479(3) 0.08456(19) 0.0784(10) Uani 1 1 d . . . O8 O 0.1779(4) -0.0527(3) 0.12343(18) 0.0871(11) Uani 1 1 d . . . O7 O 0.0149(4) -0.0468(3) 0.19033(19) 0.0747(10) Uani 1 1 d . . . O4 O 0.4511(4) 0.4298(3) 0.0938(2) 0.0906(12) Uani 1 1 d . . . O5 O 0.4467(4) 0.3200(3) 0.17893(18) 0.0721(10) Uani 1 1 d . . . N2 N 0.0728(5) 0.3246(4) -0.0765(2) 0.0695(12) Uani 1 1 d . . . N1 N 0.4319(4) 0.4034(4) 0.1542(2) 0.0639(11) Uani 1 1 d . . . N3 N 0.2870(4) 0.1458(3) -0.04818(19) 0.0520(9) Uani 1 1 d . . . C23 C 0.3408(4) 0.1738(4) 0.3358(2) 0.0462(11) Uani 1 1 d . . . C18 C 0.3653(4) 0.2879(4) 0.3301(2) 0.0453(11) Uani 1 1 d . . . C19 C 0.4728(4) 0.3666(4) 0.3788(2) 0.0552(12) Uani 1 1 d . . . H19 H 0.4937 0.4435 0.3742 0.066 Uiso 1 1 calc R . . C20 C 0.5504(5) 0.3340(5) 0.4343(2) 0.0584(13) Uani 1 1 d . . . C21 C 0.5202(5) 0.2200(5) 0.4400(2) 0.0635(14) Uani 1 1 d . . . H21 H 0.5704 0.1974 0.4779 0.076 Uiso 1 1 calc R . . C22 C 0.4167(5) 0.1380(4) 0.3907(2) 0.0530(12) Uani 1 1 d . . . C25 C 0.3864(6) 0.0143(5) 0.3986(3) 0.0854(17) Uani 1 1 d . . . H25A H 0.2818 -0.0294 0.3848 0.128 Uiso 1 1 calc R . . H25B H 0.4156 0.0034 0.4470 0.128 Uiso 1 1 calc R . . H25C H 0.4423 -0.0101 0.3691 0.128 Uiso 1 1 calc R . . C24 C 0.6668(6) 0.4245(5) 0.4892(3) 0.097(2) Uani 1 1 d . . . H24A H 0.7072 0.4949 0.4675 0.146 Uiso 1 1 calc R . . H24B H 0.7457 0.3994 0.5061 0.146 Uiso 1 1 calc R . . H24C H 0.6199 0.4355 0.5280 0.146 Uiso 1 1 calc R . . C11 C 0.2576(4) 0.3207(3) 0.2767(2) 0.0423(10) Uani 1 1 d . . . H11 H 0.2348 0.2713 0.2335 0.051 Uiso 1 1 calc R . . C7 C 0.1034(5) 0.2922(4) 0.3780(2) 0.0536(12) Uani 1 1 d . . . H7 H 0.1900 0.3051 0.4096 0.064 Uiso 1 1 calc R . . C8 C 0.1119(4) 0.2945(3) 0.3065(2) 0.0418(10) Uani 1 1 d . . . C6 C -0.0265(5) 0.2720(4) 0.4043(2) 0.0580(12) Uani 1 1 d . . . C5 C -0.1539(5) 0.2524(4) 0.3562(3) 0.0616(13) Uani 1 1 d . . . H5 H -0.2433 0.2382 0.3731 0.074 Uiso 1 1 calc R . . C4 C -0.1540(5) 0.2531(4) 0.2839(2) 0.0504(11) Uani 1 1 d . . . C9 C -0.2963(5) 0.2336(5) 0.2346(3) 0.0741(15) Uani 1 1 d . . . H9A H -0.2745 0.2809 0.1958 0.111 Uiso 1 1 calc R . . H9B H -0.3639 0.2521 0.2596 0.111 Uiso 1 1 calc R . . H9C H -0.3412 0.1553 0.2170 0.111 Uiso 1 1 calc R . . C12 C 0.3216(5) 0.4422(4) 0.2569(2) 0.0501(11) Uani 1 1 d . . . C13 C 0.3012(5) 0.5267(4) 0.2967(3) 0.0648(13) Uani 1 1 d . . . H13 H 0.2495 0.5060 0.3348 0.078 Uiso 1 1 calc R . . C17 C 0.3954(5) 0.4797(4) 0.1993(3) 0.0563(12) Uani 1 1 d . . . C1 C 0.0084(5) 0.1775(4) 0.0869(2) 0.0501(11) Uani 1 1 d . . . C2 C -0.0683(5) 0.1742(4) 0.1493(2) 0.0544(11) Uani 1 1 d . . . H2A H -0.1741 0.1535 0.1335 0.065 Uiso 1 1 calc R . . H2B H -0.0561 0.1167 0.1794 0.065 Uiso 1 1 calc R . . C3 C -0.0190(4) 0.2745(3) 0.2604(2) 0.0412(10) Uani 1 1 d . . . C14 C 0.3544(7) 0.6391(5) 0.2819(4) 0.0876(17) Uani 1 1 d . . . H14 H 0.3411 0.6927 0.3108 0.105 Uiso 1 1 calc R . . C15 C 0.4257(7) 0.6719(5) 0.2259(4) 0.0956(19) Uani 1 1 d . . . H15 H 0.4626 0.7481 0.2165 0.115 Uiso 1 1 calc R . . C16 C 0.4441(6) 0.5919(5) 0.1825(3) 0.0842(17) Uani 1 1 d . . . H16 H 0.4887 0.6133 0.1423 0.101 Uiso 1 1 calc R . . C26 C 0.2760(5) 0.0535(4) 0.2312(2) 0.0599(13) Uani 1 1 d . . . H26A H 0.3364 0.0111 0.2484 0.072 Uiso 1 1 calc R . . H26B H 0.3372 0.1179 0.2081 0.072 Uiso 1 1 calc R . . C27 C 0.1439(6) -0.0216(4) 0.1788(3) 0.0583(13) Uani 1 1 d . . . C37 C 0.3365(6) 0.1146(4) -0.1032(3) 0.0628(13) Uani 1 1 d . . . H37 H 0.2763 0.0968 -0.1471 0.075 Uiso 1 1 calc R . . C36 C 0.4750(6) 0.1081(4) -0.0964(3) 0.0682(14) Uani 1 1 d . . . H36 H 0.5078 0.0868 -0.1355 0.082 Uiso 1 1 calc R . . C35 C 0.5640(6) 0.1330(4) -0.0323(3) 0.0749(15) Uani 1 1 d . . . H35 H 0.6575 0.1286 -0.0270 0.090 Uiso 1 1 calc R . . C34 C 0.5126(6) 0.1645(4) 0.0235(3) 0.0761(16) Uani 1 1 d . . . H34 H 0.5719 0.1829 0.0676 0.091 Uiso 1 1 calc R . . C33 C 0.3725(5) 0.1693(4) 0.0149(2) 0.0627(13) Uani 1 1 d . . . H33 H 0.3374 0.1891 0.0537 0.075 Uiso 1 1 calc R . . C32 C -0.0360(7) 0.3486(6) -0.1128(3) 0.100(2) Uani 1 1 d . . . H32 H -0.1203 0.2895 -0.1357 0.120 Uiso 1 1 calc R . . C28 C 0.1924(6) 0.4113(5) -0.0447(3) 0.0826(17) Uani 1 1 d . . . H28 H 0.2691 0.3949 -0.0193 0.099 Uiso 1 1 calc R . . C31 C -0.0275(9) 0.4594(8) -0.1175(4) 0.120(3) Uani 1 1 d . . . H31 H -0.1038 0.4748 -0.1441 0.145 Uiso 1 1 calc R . . C29 C 0.2092(8) 0.5215(5) -0.0468(4) 0.103(2) Uani 1 1 d . . . H29 H 0.2957 0.5795 -0.0249 0.124 Uiso 1 1 calc R . . C30 C 0.0935(10) 0.5444(7) -0.0828(4) 0.122(3) Uani 1 1 d . . . H30 H 0.0984 0.6188 -0.0832 0.147 Uiso 1 1 calc R . . O9 O 0.3734(8) 0.0591(5) 0.7239(3) 0.160(3) Uani 1 1 d . . . N5 N 0.1959(7) 0.0599(4) 0.6341(3) 0.0929(15) Uani 1 1 d . . . C38 C 0.3017(8) 0.1228(8) 0.5905(4) 0.160(4) Uani 1 1 d . . . H38A H 0.4007 0.1360 0.6136 0.239 Uiso 1 1 calc R . . H38B H 0.2922 0.1942 0.5825 0.239 Uiso 1 1 calc R . . H38C H 0.2832 0.0802 0.5461 0.239 Uiso 1 1 calc R . . C39 C 0.0384(9) 0.0233(7) 0.6053(4) 0.127(3) Uani 1 1 d . . . H39A H -0.0207 -0.0118 0.6409 0.191 Uiso 1 1 calc R . . H39B H 0.0152 -0.0303 0.5655 0.191 Uiso 1 1 calc R . . H39C H 0.0167 0.0879 0.5906 0.191 Uiso 1 1 calc R . . C40 C 0.2468(12) 0.0358(6) 0.6971(4) 0.116(3) Uani 1 1 d . . . H40 H 0.1745 -0.0046 0.7239 0.139 Uiso 1 1 calc R . . N4 N 0.0726(8) 0.3562(7) 0.6972(4) 0.121(2) Uani 1 1 d . . . O10 O -0.1436(14) 0.2855(13) 0.6343(5) 0.267(7) Uani 1 1 d . . . C42 C 0.0936(18) 0.4552(9) 0.6766(8) 0.285(9) Uani 1 1 d . . . H42A H 0.1849 0.5148 0.6906 0.342 Uiso 1 1 calc R . . H42B H 0.0177 0.4678 0.6476 0.342 Uiso 1 1 calc R . . C41 C 0.1865(15) 0.3378(15) 0.7406(7) 0.299(9) Uani 1 1 d . . . H41A H 0.2796 0.3770 0.7240 0.449 Uiso 1 1 calc R . . H41B H 0.1663 0.2579 0.7395 0.449 Uiso 1 1 calc R . . H41C H 0.1922 0.3659 0.7881 0.449 Uiso 1 1 calc R . . C10 C -0.0309(6) 0.2705(6) 0.4827(3) 0.095(2) Uani 1 1 d . . . H10A H 0.0565 0.2612 0.5065 0.142 Uiso 1 1 calc R . . H10B H -0.1183 0.2084 0.4916 0.142 Uiso 1 1 calc R . . H10C H -0.0336 0.3407 0.5000 0.142 Uiso 1 1 calc R . . C43 C -0.060(2) 0.2542(9) 0.6790(9) 0.245(10) Uani 1 1 d . . . H43 H -0.0789 0.1826 0.6958 0.294 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.05698(13) 0.06467(14) 0.04613(13) -0.00454(9) 0.00078(9) 0.01571(10) O3 0.0484(17) 0.0469(18) 0.0396(17) 0.0032(14) 0.0037(14) 0.0162(14) O6 0.0392(16) 0.0553(19) 0.0509(18) -0.0081(15) -0.0002(14) 0.0121(14) O1 0.089(3) 0.068(2) 0.046(2) -0.0053(18) 0.0076(18) 0.006(2) O2 0.059(2) 0.095(3) 0.068(2) -0.019(2) 0.0176(18) 0.013(2) O8 0.084(3) 0.101(3) 0.054(2) -0.024(2) 0.005(2) 0.012(2) O7 0.056(2) 0.079(3) 0.074(3) -0.0066(19) -0.0106(19) 0.016(2) O4 0.095(3) 0.108(3) 0.056(2) 0.012(2) 0.027(2) 0.018(2) O5 0.066(2) 0.101(3) 0.065(2) 0.012(2) 0.0163(18) 0.047(2) N2 0.075(3) 0.069(3) 0.065(3) 0.009(2) -0.006(2) 0.034(3) N1 0.042(2) 0.087(3) 0.050(3) 0.001(3) 0.005(2) 0.011(2) N3 0.053(2) 0.049(2) 0.048(2) -0.0041(18) 0.0051(19) 0.0132(18) C23 0.038(2) 0.062(3) 0.039(2) -0.003(2) 0.004(2) 0.021(2) C18 0.036(2) 0.062(3) 0.035(2) -0.005(2) 0.0028(19) 0.017(2) C19 0.044(3) 0.067(3) 0.050(3) -0.010(2) -0.001(2) 0.019(2) C20 0.039(3) 0.086(4) 0.045(3) -0.015(3) -0.001(2) 0.022(3) C21 0.049(3) 0.104(5) 0.039(3) 0.000(3) -0.001(2) 0.034(3) C22 0.046(3) 0.075(3) 0.042(3) 0.004(2) 0.008(2) 0.027(2) C25 0.092(4) 0.097(5) 0.073(4) 0.018(3) -0.001(3) 0.047(4) C24 0.076(4) 0.124(5) 0.072(4) -0.034(3) -0.023(3) 0.031(4) C11 0.037(2) 0.051(3) 0.037(2) -0.005(2) 0.0041(19) 0.016(2) C7 0.049(3) 0.066(3) 0.046(3) 0.000(2) 0.004(2) 0.024(2) C8 0.042(2) 0.044(2) 0.038(2) -0.0027(19) 0.0035(19) 0.016(2) C6 0.062(3) 0.071(3) 0.048(3) 0.007(2) 0.019(3) 0.030(3) C5 0.050(3) 0.070(3) 0.069(4) 0.004(3) 0.020(3) 0.025(3) C4 0.045(3) 0.053(3) 0.055(3) 0.003(2) 0.005(2) 0.021(2) C9 0.049(3) 0.097(4) 0.080(4) 0.001(3) 0.004(3) 0.033(3) C12 0.040(2) 0.057(3) 0.048(3) 0.000(2) 0.004(2) 0.013(2) C13 0.066(3) 0.058(3) 0.067(3) 0.000(3) 0.014(3) 0.019(3) C17 0.040(3) 0.063(3) 0.056(3) 0.004(3) 0.004(2) 0.010(2) C1 0.054(3) 0.046(3) 0.043(3) 0.002(2) -0.004(2) 0.015(2) C2 0.054(3) 0.053(3) 0.046(3) -0.002(2) 0.008(2) 0.008(2) C3 0.040(2) 0.042(2) 0.043(3) 0.002(2) 0.006(2) 0.017(2) C14 0.090(4) 0.062(4) 0.104(5) -0.003(4) 0.026(4) 0.018(3) C15 0.107(5) 0.057(4) 0.115(6) 0.014(4) 0.030(4) 0.018(4) C16 0.079(4) 0.077(4) 0.084(4) 0.020(4) 0.018(3) 0.014(3) C26 0.056(3) 0.067(3) 0.048(3) -0.011(2) 0.002(2) 0.016(3) C27 0.064(4) 0.048(3) 0.051(3) 0.003(2) -0.005(3) 0.013(3) C37 0.071(4) 0.060(3) 0.051(3) 0.007(2) 0.011(3) 0.016(3) C36 0.076(4) 0.059(3) 0.079(4) 0.016(3) 0.034(3) 0.028(3) C35 0.061(3) 0.070(4) 0.093(4) 0.008(3) 0.008(3) 0.026(3) C34 0.070(4) 0.082(4) 0.071(4) -0.002(3) -0.012(3) 0.032(3) C33 0.069(3) 0.066(3) 0.051(3) -0.006(2) -0.001(3) 0.027(3) C32 0.086(4) 0.114(6) 0.096(5) 0.025(4) -0.010(4) 0.042(4) C28 0.085(4) 0.061(4) 0.094(4) 0.014(3) -0.006(3) 0.025(3) C31 0.105(6) 0.131(7) 0.146(7) 0.053(6) 0.005(5) 0.072(6) C29 0.106(5) 0.064(4) 0.127(6) 0.023(4) 0.008(4) 0.021(4) C30 0.150(7) 0.095(6) 0.143(7) 0.040(5) 0.028(6) 0.068(6) O9 0.222(7) 0.116(5) 0.106(4) -0.007(3) -0.034(5) 0.045(5) N5 0.124(5) 0.097(4) 0.065(3) 0.019(3) 0.037(3) 0.042(4) C38 0.130(7) 0.232(11) 0.126(7) 0.083(7) 0.065(6) 0.062(7) C39 0.127(7) 0.133(7) 0.140(7) 0.021(5) 0.052(6) 0.059(6) C40 0.205(10) 0.065(5) 0.073(6) 0.005(4) 0.040(6) 0.039(6) N4 0.130(5) 0.115(6) 0.121(5) -0.001(4) 0.035(4) 0.046(5) O10 0.284(11) 0.43(2) 0.153(8) -0.016(9) 0.065(7) 0.196(13) C42 0.45(2) 0.098(8) 0.38(2) 0.084(11) 0.226(19) 0.124(12) C41 0.219(14) 0.48(3) 0.235(16) -0.030(16) -0.017(12) 0.195(18) C10 0.089(4) 0.149(6) 0.054(3) 0.011(4) 0.027(3) 0.049(4) C43 0.42(3) 0.075(7) 0.269(19) 0.015(10) 0.241(19) 0.062(12) _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 Hg1 N3 2.227(3) . ? Hg1 O1 2.233(3) . ? Hg1 O8 2.291(3) 2 ? Hg1 N2 2.381(4) . ? O3 C3 1.395(5) . ? O3 C2 1.422(5) . ? O6 C23 1.393(5) . ? O6 C26 1.428(5) . ? O1 C1 1.263(5) . ? O2 C1 1.217(5) . ? O8 C27 1.255(6) . ? O8 Hg1 2.291(3) 2 ? O7 C27 1.233(6) . ? O4 N1 1.229(5) . ? O5 N1 1.218(5) . ? N2 C32 1.326(6) . ? N2 C28 1.334(6) . ? N1 C17 1.462(6) . ? N3 C37 1.333(6) . ? N3 C33 1.333(5) . ? C23 C22 1.386(5) . ? C23 C18 1.389(6) . ? C18 C19 1.377(5) . ? C18 C11 1.541(5) . ? C19 C20 1.382(6) . ? C19 H19 0.9300 . ? C20 C21 1.377(7) . ? C20 C24 1.544(6) . ? C21 C22 1.388(6) . ? C21 H21 0.9300 . ? C22 C25 1.502(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C11 C12 1.511(6) . ? C11 C8 1.530(6) . ? C11 H11 0.9800 . ? C7 C6 1.367(6) . ? C7 C8 1.384(6) . ? C7 H7 0.9300 . ? C8 C3 1.387(5) . ? C6 C5 1.383(6) . ? C6 C10 1.510(6) . ? C5 C4 1.385(6) . ? C5 H5 0.9300 . ? C4 C3 1.385(6) . ? C4 C9 1.506(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C12 C17 1.394(6) . ? C12 C13 1.398(6) . ? C13 C14 1.376(7) . ? C13 H13 0.9300 . ? C17 C16 1.384(7) . ? C1 C2 1.488(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C14 C15 1.345(8) . ? C14 H14 0.9300 . ? C15 C16 1.384(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C26 C27 1.512(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C37 C36 1.376(6) . ? C37 H37 0.9300 . ? C36 C35 1.362(7) . ? C36 H36 0.9300 . ? C35 C34 1.356(7) . ? C35 H35 0.9300 . ? C34 C33 1.383(6) . ? C34 H34 0.9300 . ? C33 H33 0.9300 . ? C32 C31 1.385(9) . ? C32 H32 0.9300 . ? C28 C29 1.352(8) . ? C28 H28 0.9300 . ? C31 C30 1.349(9) . ? C31 H31 0.9300 . ? C29 C30 1.370(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? O9 C40 1.197(9) . ? N5 C40 1.327(8) . ? N5 C38 1.429(8) . ? N5 C39 1.456(8) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40 0.9300 . ? N4 C42 1.276(10) . ? N4 C41 1.391(12) . ? N4 C43 1.445(16) . ? O10 C43 1.276(19) . ? C42 H42A 0.9300 . ? C42 H42B 0.9300 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C43 H43 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Hg1 O1 119.95(13) . . ? N3 Hg1 O8 142.46(13) . 2 ? O1 Hg1 O8 87.03(13) . 2 ? N3 Hg1 N2 103.76(13) . . ? O1 Hg1 N2 101.88(13) . . ? O8 Hg1 N2 94.40(14) 2 . ? C3 O3 C2 114.0(3) . . ? C23 O6 C26 114.1(3) . . ? C1 O1 Hg1 109.7(3) . . ? C27 O8 Hg1 100.6(3) . 2 ? C32 N2 C28 117.6(5) . . ? C32 N2 Hg1 123.0(4) . . ? C28 N2 Hg1 119.1(3) . . ? O5 N1 O4 123.7(4) . . ? O5 N1 C17 118.7(4) . . ? O4 N1 C17 117.6(5) . . ? C37 N3 C33 119.1(4) . . ? C37 N3 Hg1 121.0(3) . . ? C33 N3 Hg1 119.3(3) . . ? C22 C23 C18 121.6(4) . . ? C22 C23 O6 119.3(4) . . ? C18 C23 O6 118.7(3) . . ? C19 C18 C23 118.3(4) . . ? C19 C18 C11 122.0(4) . . ? C23 C18 C11 119.0(4) . . ? C18 C19 C20 121.6(5) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 118.7(4) . . ? C21 C20 C24 121.2(4) . . ? C19 C20 C24 120.1(5) . . ? C20 C21 C22 121.7(4) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 117.9(4) . . ? C23 C22 C25 121.8(4) . . ? C21 C22 C25 120.3(4) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 C11 C8 111.7(3) . . ? C12 C11 C18 113.9(3) . . ? C8 C11 C18 108.5(3) . . ? C12 C11 H11 107.5 . . ? C8 C11 H11 107.5 . . ? C18 C11 H11 107.5 . . ? C6 C7 C8 123.0(4) . . ? C6 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? C7 C8 C3 117.4(4) . . ? C7 C8 C11 123.3(3) . . ? C3 C8 C11 119.3(4) . . ? C7 C6 C5 117.4(4) . . ? C7 C6 C10 121.3(4) . . ? C5 C6 C10 121.3(4) . . ? C6 C5 C4 122.8(4) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C4 C3 117.1(4) . . ? C5 C4 C9 120.1(4) . . ? C3 C4 C9 122.8(4) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C17 C12 C13 114.9(4) . . ? C17 C12 C11 126.0(4) . . ? C13 C12 C11 119.0(4) . . ? C14 C13 C12 122.8(5) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C16 C17 C12 122.6(5) . . ? C16 C17 N1 115.4(5) . . ? C12 C17 N1 121.9(4) . . ? O2 C1 O1 123.2(5) . . ? O2 C1 C2 121.6(4) . . ? O1 C1 C2 115.2(4) . . ? O3 C2 C1 111.2(4) . . ? O3 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? O3 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C8 122.3(4) . . ? C4 C3 O3 120.3(3) . . ? C8 C3 O3 117.4(4) . . ? C15 C14 C13 120.4(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.8(6) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 119.3(6) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? O6 C26 C27 110.4(4) . . ? O6 C26 H26A 109.6 . . ? C27 C26 H26A 109.6 . . ? O6 C26 H26B 109.6 . . ? C27 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? O7 C27 O8 124.3(5) . . ? O7 C27 C26 121.4(5) . . ? O8 C27 C26 114.3(5) . . ? N3 C37 C36 121.3(5) . . ? N3 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C35 C36 C37 120.1(5) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C34 C35 C36 118.3(5) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C35 C34 C33 120.2(5) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? N3 C33 C34 121.0(5) . . ? N3 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? N2 C32 C31 121.7(6) . . ? N2 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? N2 C28 C29 124.2(5) . . ? N2 C28 H28 117.9 . . ? C29 C28 H28 117.9 . . ? C30 C31 C32 118.8(6) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C28 C29 C30 117.3(7) . . ? C28 C29 H29 121.4 . . ? C30 C29 H29 121.4 . . ? C31 C30 C29 120.3(7) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C40 N5 C38 118.3(7) . . ? C40 N5 C39 124.1(7) . . ? C38 N5 C39 117.6(6) . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O9 C40 N5 128.6(9) . . ? O9 C40 H40 115.7 . . ? N5 C40 H40 115.7 . . ? C42 N4 C41 119.8(12) . . ? C42 N4 C43 127.2(11) . . ? C41 N4 C43 113.0(12) . . ? N4 C42 H42A 120.0 . . ? N4 C42 H42B 120.0 . . ? H42A C42 H42B 120.0 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O10 C43 N4 103.6(12) . . ? O10 C43 H43 128.2 . . ? N4 C43 H43 128.2 . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.537 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.123 # Attachment '- complex 5.cif' data_mon _database_code_depnum_ccdc_archive 'CCDC 837719' #TrackingRef '- complex 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H74 Cd2 N4 O22' _chemical_formula_weight 1524.11 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.4571(11) _cell_length_b 21.0538(12) _cell_length_c 9.2040(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.921(4) _cell_angle_gamma 90.00 _cell_volume 3374.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.86 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1564 _exptl_absorpt_coefficient_mu 0.710 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28782 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5843 _reflns_number_gt 3876 _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^)+(0.1000P)^2^+0.0389P] 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 5843 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1799 _refine_ls_goodness_of_fit_ref 1.259 _refine_ls_restrained_S_all 1.259 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.03925(3) 0.51397(3) 1.20503(6) 0.0292(2) Uani 1 1 d . . . C11 C 0.3117(4) 0.4277(3) 0.7861(7) 0.0268(17) Uani 1 1 d . . . H11 H 0.2581 0.4301 0.8108 0.032 Uiso 1 1 calc R . . C3 C 0.3058(4) 0.5476(3) 0.7792(8) 0.0293(17) Uani 1 1 d . . . C18 C 0.3171(4) 0.3719(3) 0.6789(8) 0.0269(17) Uani 1 1 d . . . C8 C 0.3307(4) 0.4916(3) 0.7159(8) 0.0279(17) Uani 1 1 d . . . C23 C 0.2538(4) 0.3564(3) 0.5860(8) 0.0263(17) Uani 1 1 d . . . C12 C 0.3599(4) 0.4191(3) 0.9281(8) 0.0283(18) Uani 1 1 d . . . C22 C 0.2579(4) 0.3089(3) 0.4795(8) 0.0303(18) Uani 1 1 d . . . C21 C 0.3265(5) 0.2773(3) 0.4709(8) 0.036(2) Uani 1 1 d . . . H21 H 0.3297 0.2455 0.4013 0.043 Uiso 1 1 calc R . . C20 C 0.3906(5) 0.2910(3) 0.5615(9) 0.036(2) Uani 1 1 d . . . C7 C 0.3696(5) 0.4969(3) 0.5918(9) 0.034(2) Uani 1 1 d . . . H7 H 0.3856 0.4599 0.5476 0.040 Uiso 1 1 calc R . . C24 C 0.4656(5) 0.2570(4) 0.5451(10) 0.051(2) Uani 1 1 d . . . H24A H 0.4845 0.2401 0.6376 0.076 Uiso 1 1 calc R . . H24B H 0.5024 0.2863 0.5108 0.076 Uiso 1 1 calc R . . H24C H 0.4577 0.2229 0.4764 0.076 Uiso 1 1 calc R . . C17 C 0.3297(5) 0.4022(3) 1.0599(8) 0.0353(19) Uani 1 1 d . . . C4 C 0.3222(4) 0.6079(3) 0.7207(9) 0.0330(19) Uani 1 1 d . . . C16 C 0.3740(6) 0.3955(4) 1.1900(10) 0.055(3) Uani 1 1 d . . . H16 H 0.3516 0.3854 1.2758 0.066 Uiso 1 1 calc R . . C5 C 0.3621(5) 0.6088(4) 0.5981(9) 0.043(2) Uani 1 1 d . . . H5 H 0.3737 0.6479 0.5585 0.051 Uiso 1 1 calc R . . C13 C 0.4397(5) 0.4295(3) 0.9357(9) 0.039(2) Uani 1 1 d . . . H13 H 0.4626 0.4426 0.8524 0.047 Uiso 1 1 calc R . . C6 C 0.3862(5) 0.5542(4) 0.5297(9) 0.040(2) Uani 1 1 d . . . C10 C 0.4258(6) 0.5587(4) 0.3901(11) 0.069(3) Uani 1 1 d . . . H10A H 0.4643 0.5261 0.3883 0.104 Uiso 1 1 calc R . . H10B H 0.4497 0.5996 0.3839 0.104 Uiso 1 1 calc R . . H10C H 0.3889 0.5532 0.3089 0.104 Uiso 1 1 calc R . . C14 C 0.4850(5) 0.4209(4) 1.0627(11) 0.051(2) Uani 1 1 d . . . H14 H 0.5379 0.4265 1.0628 0.061 Uiso 1 1 calc R . . C9 C 0.2966(5) 0.6684(4) 0.7900(10) 0.053(2) Uani 1 1 d . . . H9A H 0.3388 0.6976 0.7994 0.080 Uiso 1 1 calc R . . H9B H 0.2794 0.6592 0.8846 0.080 Uiso 1 1 calc R . . H9C H 0.2553 0.6869 0.7302 0.080 Uiso 1 1 calc R . . C15 C 0.4527(6) 0.4043(4) 1.1889(11) 0.059(3) Uani 1 1 d . . . H15 H 0.4837 0.3988 1.2742 0.070 Uiso 1 1 calc R . . O5 O 0.2134(3) 0.3585(3) 0.9774(6) 0.0466(15) Uani 1 1 d . . . O4 O 0.2176(4) 0.4164(3) 1.1715(7) 0.0652(19) Uani 1 1 d . . . N1 N 0.2474(4) 0.3914(3) 1.0687(8) 0.0423(18) Uani 1 1 d . . . O3 O 0.2631(3) 0.5434(2) 0.9002(5) 0.0266(11) Uani 1 1 d . . . O6 O 0.1866(3) 0.3922(2) 0.5933(5) 0.0287(12) Uani 1 1 d . . . C2 C 0.1822(4) 0.5447(3) 0.8572(8) 0.0309(18) Uani 1 1 d . . . H2A H 0.1704 0.5118 0.7854 0.037 Uiso 1 1 calc R . . H2B H 0.1690 0.5854 0.8128 0.037 Uiso 1 1 calc R . . C26 C 0.1256(4) 0.3592(3) 0.6584(8) 0.0306(18) Uani 1 1 d . . . H26A H 0.1455 0.3387 0.7475 0.037 Uiso 1 1 calc R . . H26B H 0.1050 0.3267 0.5924 0.037 Uiso 1 1 calc R . . C1 C 0.1355(5) 0.5344(4) 0.9860(8) 0.0331(19) Uani 1 1 d . . . O2 O 0.0789(3) 0.4966(2) 0.9743(5) 0.0318(13) Uani 1 1 d . . . O1 O 0.1507(3) 0.5642(3) 1.0992(6) 0.0543(17) Uani 1 1 d . . . C32 C -0.0246(4) 0.3855(3) 1.3445(8) 0.0314(18) Uani 1 1 d . . . H32 H -0.0367 0.4140 1.4166 0.038 Uiso 1 1 calc R . . C28 C 0.0282(4) 0.3661(3) 1.1279(7) 0.0276(17) Uani 1 1 d . . . H28 H 0.0524 0.3807 1.0475 0.033 Uiso 1 1 calc R . . C31 C -0.0461(5) 0.3226(4) 1.3597(9) 0.039(2) Uani 1 1 d . . . H31 H -0.0713 0.3092 1.4399 0.046 Uiso 1 1 calc R . . C30 C -0.0287(5) 0.2806(4) 1.2512(10) 0.052(2) Uani 1 1 d . . . H30 H -0.0425 0.2380 1.2563 0.062 Uiso 1 1 calc R . . C29 C 0.0100(5) 0.3033(4) 1.1342(9) 0.043(2) Uani 1 1 d . . . H29 H 0.0232 0.2758 1.0610 0.052 Uiso 1 1 calc R . . C25 C 0.1905(5) 0.2937(4) 0.3749(9) 0.044(2) Uani 1 1 d . . . H25A H 0.2081 0.2722 0.2914 0.066 Uiso 1 1 calc R . . H25B H 0.1649 0.3323 0.3446 0.066 Uiso 1 1 calc R . . H25C H 0.1553 0.2667 0.4219 0.066 Uiso 1 1 calc R . . N2 N 0.0128(3) 0.4079(3) 1.2321(6) 0.0277(14) Uani 1 1 d . . . O9 O 0.1200(3) 0.5137(2) 1.4076(6) 0.0370(13) Uani 1 1 d . . . O8 O -0.0125(3) 0.6153(2) 1.2308(5) 0.0292(12) Uani 1 1 d . . . O7 O -0.0640(3) 0.5390(2) 1.3600(5) 0.0263(11) Uani 1 1 d . . . C27 C -0.0633(4) 0.5953(3) 1.3083(7) 0.0236(16) Uani 1 1 d . . . C19 C 0.3842(4) 0.3384(3) 0.6647(8) 0.0291(18) Uani 1 1 d . . . H19 H 0.4268 0.3480 0.7269 0.035 Uiso 1 1 calc R . . O11 O 0.2224(8) 0.6802(5) 0.1510(11) 0.144(5) Uani 1 1 d . . . H11A H 0.1967 0.6765 0.2219 0.216 Uiso 1 1 calc R . . C33 C 0.1962(7) 0.5330(6) 1.4208(11) 0.081(4) Uani 1 1 d . . . H33A H 0.2137 0.5409 1.3258 0.122 Uiso 1 1 calc R . . H33B H 0.2270 0.5002 1.4679 0.122 Uiso 1 1 calc R . . H33C H 0.2006 0.5712 1.4777 0.122 Uiso 1 1 calc R . . O10 O 0.8037(10) 0.2928(10) 0.573(3) 0.349(15) Uani 1 1 d . . . C34 C 0.300(2) 0.6592(11) 0.189(3) 0.34(2) Uani 1 1 d . . . H34A H 0.3350 0.6918 0.1650 0.506 Uiso 1 1 calc R . . H34B H 0.3096 0.6213 0.1351 0.506 Uiso 1 1 calc R . . H34C H 0.3055 0.6504 0.2912 0.506 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0418(4) 0.0232(3) 0.0234(4) -0.0013(2) 0.0085(2) 0.0014(3) C11 0.033(4) 0.018(4) 0.031(5) -0.001(3) 0.016(3) -0.002(3) C3 0.032(4) 0.029(4) 0.026(5) 0.002(3) -0.002(3) -0.003(3) C18 0.038(5) 0.018(4) 0.025(4) 0.001(3) 0.006(4) -0.003(3) C8 0.029(4) 0.017(4) 0.038(5) 0.000(3) 0.006(3) 0.001(3) C23 0.032(5) 0.017(4) 0.031(5) 0.006(3) 0.008(3) 0.005(3) C12 0.041(5) 0.016(4) 0.028(5) 0.000(3) -0.001(4) 0.002(3) C22 0.038(5) 0.029(4) 0.025(5) 0.003(3) 0.008(4) 0.000(4) C21 0.053(6) 0.030(4) 0.026(5) -0.002(3) 0.012(4) 0.002(4) C20 0.042(5) 0.026(4) 0.041(5) 0.001(4) 0.013(4) 0.001(4) C7 0.041(5) 0.021(4) 0.041(5) -0.004(3) 0.023(4) 0.003(3) C24 0.049(6) 0.031(5) 0.075(7) -0.008(4) 0.019(5) 0.009(4) C17 0.041(5) 0.031(4) 0.033(5) -0.004(3) -0.001(4) 0.000(4) C4 0.036(5) 0.022(4) 0.043(5) 0.001(3) 0.012(4) 0.000(3) C16 0.080(8) 0.039(5) 0.045(6) -0.003(4) -0.015(5) -0.001(5) C5 0.048(6) 0.030(5) 0.052(6) 0.014(4) 0.017(4) -0.004(4) C13 0.050(6) 0.021(4) 0.044(6) 0.000(3) -0.002(4) -0.008(4) C6 0.044(5) 0.027(5) 0.052(6) 0.006(4) 0.023(4) 0.003(4) C10 0.086(8) 0.049(6) 0.081(8) 0.012(5) 0.061(6) 0.009(5) C14 0.049(6) 0.027(5) 0.075(7) 0.000(5) -0.015(5) -0.008(4) C9 0.067(7) 0.027(5) 0.067(7) -0.006(4) 0.024(5) -0.005(4) C15 0.074(8) 0.042(6) 0.055(7) -0.004(5) -0.026(6) -0.006(5) O5 0.050(4) 0.048(4) 0.042(4) 0.000(3) 0.011(3) -0.015(3) O4 0.079(5) 0.078(5) 0.042(4) 0.000(3) 0.026(3) 0.008(4) N1 0.055(5) 0.039(4) 0.034(5) 0.011(3) 0.013(4) 0.001(4) O3 0.031(3) 0.028(3) 0.022(3) -0.005(2) 0.006(2) -0.006(2) O6 0.032(3) 0.017(2) 0.037(3) 0.005(2) 0.002(2) -0.001(2) C2 0.038(5) 0.027(4) 0.027(5) -0.001(3) 0.001(3) 0.000(3) C26 0.030(5) 0.023(4) 0.038(5) 0.002(3) -0.001(3) 0.000(3) C1 0.056(6) 0.027(4) 0.018(5) -0.004(3) 0.007(4) 0.010(4) O2 0.030(3) 0.033(3) 0.033(3) 0.009(2) 0.008(2) -0.003(2) O1 0.076(5) 0.057(4) 0.032(4) -0.016(3) 0.017(3) -0.022(3) C32 0.042(5) 0.029(4) 0.023(4) -0.001(3) -0.001(4) 0.008(4) C28 0.040(5) 0.032(4) 0.010(4) 0.000(3) -0.003(3) 0.003(3) C31 0.046(5) 0.036(5) 0.034(5) 0.005(4) 0.005(4) -0.001(4) C30 0.076(7) 0.024(5) 0.055(6) 0.003(4) 0.004(5) -0.008(4) C29 0.062(6) 0.036(5) 0.031(5) -0.008(4) -0.006(4) 0.006(4) C25 0.059(6) 0.044(5) 0.030(5) -0.004(4) 0.007(4) 0.004(4) N2 0.027(4) 0.032(4) 0.024(4) 0.001(3) 0.003(3) 0.001(3) O9 0.036(3) 0.043(3) 0.031(3) 0.005(2) -0.006(2) -0.007(3) O8 0.035(3) 0.025(3) 0.029(3) 0.003(2) 0.009(2) -0.001(2) O7 0.037(3) 0.017(2) 0.026(3) 0.001(2) 0.007(2) 0.003(2) C27 0.029(4) 0.024(4) 0.017(4) -0.002(3) -0.003(3) 0.002(3) C19 0.028(5) 0.027(4) 0.033(5) 0.002(3) 0.008(3) -0.002(3) O11 0.250(14) 0.082(7) 0.100(8) -0.009(6) 0.015(8) -0.078(8) C33 0.084(9) 0.117(10) 0.041(7) 0.016(6) -0.005(6) -0.020(7) O10 0.186(15) 0.31(2) 0.56(4) 0.24(3) 0.040(19) -0.036(14) C34 0.56(6) 0.20(3) 0.21(3) -0.08(2) -0.25(3) 0.18(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O9 2.259(5) . ? Cd1 N2 2.297(6) . ? Cd1 O2 2.307(5) . ? Cd1 O8 2.335(5) . ? Cd1 O7 2.432(5) . ? Cd1 O1 2.473(6) . ? Cd1 O2 2.562(5) 3_567 ? Cd1 C27 2.697(7) . ? C11 C12 1.516(10) . ? C11 C8 1.539(9) . ? C11 C18 1.540(9) . ? C3 O3 1.385(8) . ? C3 C8 1.399(10) . ? C3 C4 1.415(10) . ? C18 C19 1.382(10) . ? C18 C23 1.389(10) . ? C8 C7 1.373(10) . ? C23 O6 1.400(8) . ? C23 C22 1.406(10) . ? C12 C17 1.401(10) . ? C12 C13 1.407(10) . ? C22 C21 1.377(10) . ? C22 C25 1.503(11) . ? C21 C20 1.380(11) . ? C20 C19 1.388(10) . ? C20 C24 1.509(10) . ? C7 C6 1.375(10) . ? C17 C16 1.388(11) . ? C17 N1 1.462(10) . ? C4 C5 1.366(10) . ? C4 C9 1.506(10) . ? C16 C15 1.386(13) . ? C5 C6 1.389(11) . ? C13 C14 1.377(11) . ? C6 C10 1.504(11) . ? C14 C15 1.371(13) . ? O5 N1 1.212(8) . ? O4 N1 1.230(8) . ? O3 C2 1.440(8) . ? O6 C26 1.436(8) . ? C2 C1 1.500(10) . ? C26 C27 1.496(10) 3_567 ? C1 O1 1.230(9) . ? C1 O2 1.267(9) . ? O2 Cd1 2.562(5) 3_567 ? C32 N2 1.346(9) . ? C32 C31 1.385(10) . ? C28 N2 1.342(9) . ? C28 C29 1.363(10) . ? C31 C30 1.383(12) . ? C30 C29 1.394(12) . ? O9 C33 1.387(12) . ? O8 C27 1.248(8) . ? O7 C27 1.278(8) . ? C27 C26 1.496(10) 3_567 ? O11 C34 1.44(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Cd1 N2 91.54(19) . . ? O9 Cd1 O2 123.32(19) . . ? N2 Cd1 O2 91.20(19) . . ? O9 Cd1 O8 98.20(18) . . ? N2 Cd1 O8 142.6(2) . . ? O2 Cd1 O8 112.39(17) . . ? O9 Cd1 O7 87.85(18) . . ? N2 Cd1 O7 89.14(18) . . ? O2 Cd1 O7 148.80(18) . . ? O8 Cd1 O7 55.56(16) . . ? O9 Cd1 O1 82.1(2) . . ? N2 Cd1 O1 128.9(2) . . ? O2 Cd1 O1 53.94(18) . . ? O8 Cd1 O1 88.27(18) . . ? O7 Cd1 O1 140.63(17) . . ? O9 Cd1 O2 163.95(18) . 3_567 ? N2 Cd1 O2 80.01(18) . 3_567 ? O2 Cd1 O2 70.9(2) . 3_567 ? O8 Cd1 O2 81.05(16) . 3_567 ? O7 Cd1 O2 78.47(16) . 3_567 ? O1 Cd1 O2 113.83(18) . 3_567 ? O9 Cd1 C27 95.89(19) . . ? N2 Cd1 C27 115.9(2) . . ? O2 Cd1 C27 132.31(19) . . ? O8 Cd1 C27 27.52(18) . . ? O7 Cd1 C27 28.24(18) . . ? O1 Cd1 C27 115.2(2) . . ? O2 Cd1 C27 75.97(18) 3_567 . ? C12 C11 C8 110.1(6) . . ? C12 C11 C18 114.1(6) . . ? C8 C11 C18 111.9(6) . . ? O3 C3 C8 118.7(6) . . ? O3 C3 C4 119.9(6) . . ? C8 C3 C4 121.4(7) . . ? C19 C18 C23 117.7(7) . . ? C19 C18 C11 122.6(7) . . ? C23 C18 C11 119.6(6) . . ? C7 C8 C3 117.7(6) . . ? C7 C8 C11 123.6(6) . . ? C3 C8 C11 118.7(6) . . ? C18 C23 O6 118.5(6) . . ? C18 C23 C22 121.4(6) . . ? O6 C23 C22 120.0(7) . . ? C17 C12 C13 115.2(7) . . ? C17 C12 C11 123.8(7) . . ? C13 C12 C11 120.9(6) . . ? C21 C22 C23 118.0(7) . . ? C21 C22 C25 120.4(7) . . ? C23 C22 C25 121.6(7) . . ? C22 C21 C20 122.5(7) . . ? C21 C20 C19 117.6(7) . . ? C21 C20 C24 120.9(7) . . ? C19 C20 C24 121.4(7) . . ? C8 C7 C6 123.2(7) . . ? C16 C17 C12 123.5(8) . . ? C16 C17 N1 115.4(8) . . ? C12 C17 N1 121.1(7) . . ? C5 C4 C3 117.0(7) . . ? C5 C4 C9 121.4(7) . . ? C3 C4 C9 121.6(7) . . ? C15 C16 C17 118.3(9) . . ? C4 C5 C6 123.4(7) . . ? C14 C13 C12 122.1(8) . . ? C7 C6 C5 117.3(7) . . ? C7 C6 C10 122.1(7) . . ? C5 C6 C10 120.5(7) . . ? C15 C14 C13 120.4(9) . . ? C14 C15 C16 120.4(9) . . ? O5 N1 O4 124.4(7) . . ? O5 N1 C17 119.2(7) . . ? O4 N1 C17 116.5(7) . . ? C3 O3 C2 110.4(5) . . ? C23 O6 C26 114.0(5) . . ? O3 C2 C1 110.8(6) . . ? O6 C26 C27 110.3(5) . 3_567 ? O1 C1 O2 121.0(7) . . ? O1 C1 C2 119.9(8) . . ? O2 C1 C2 119.1(7) . . ? C1 O2 Cd1 96.0(4) . . ? C1 O2 Cd1 134.3(5) . 3_567 ? Cd1 O2 Cd1 109.1(2) . 3_567 ? C1 O1 Cd1 89.1(5) . . ? N2 C32 C31 124.1(7) . . ? N2 C28 C29 123.2(7) . . ? C30 C31 C32 117.7(8) . . ? C31 C30 C29 118.7(8) . . ? C28 C29 C30 119.5(8) . . ? C28 N2 C32 116.8(6) . . ? C28 N2 Cd1 120.6(5) . . ? C32 N2 Cd1 122.4(5) . . ? C33 O9 Cd1 127.7(5) . . ? C27 O8 Cd1 92.6(4) . . ? C27 O7 Cd1 87.5(4) . . ? O8 C27 O7 123.4(6) . . ? O8 C27 C26 117.2(6) . 3_567 ? O7 C27 C26 119.4(6) . 3_567 ? O8 C27 Cd1 59.8(3) . . ? O7 C27 Cd1 64.3(3) . . ? C26 C27 Cd1 171.0(5) 3_567 . ? C18 C19 C20 122.7(7) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.812 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.250 # Attachment '- complex 7.cif' data_p1 _database_code_depnum_ccdc_archive 'CCDC 837720' #TrackingRef '- complex 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H70 Cd2 N6 O26' _chemical_formula_weight 1684.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7715(8) _cell_length_b 12.4713(9) _cell_length_c 15.3045(11) _cell_angle_alpha 80.416(3) _cell_angle_beta 80.098(3) _cell_angle_gamma 67.749(3) _cell_volume 2035.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28951 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7252 _reflns_number_gt 6287 _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^)+(0.0914P)^2^+0.2940P] 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 7252 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1299 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.189942(18) 0.353208(18) 0.393644(14) 0.04731(12) Uani 1 1 d . . . O4 O 1.1362(3) 0.7534(2) 0.8620(2) 0.0894(9) Uani 1 1 d . . . O5 O 1.0198(3) 0.7706(2) 0.9879(2) 0.0930(9) Uani 1 1 d . . . O3 O 1.40654(19) 0.35748(19) 0.63881(13) 0.0489(5) Uani 1 1 d . . . O6 O 1.07906(16) 0.29588(16) 0.80242(12) 0.0383(4) Uani 1 1 d . . . O8 O 0.9440(3) 0.5152(2) 0.73632(17) 0.0668(7) Uani 1 1 d . . . O7 O 0.9274(2) 0.4546(2) 0.61516(16) 0.0601(6) Uani 1 1 d . . . O2 O 1.2633(2) 0.3870(2) 0.51577(16) 0.0659(6) Uani 1 1 d . . . O1 O 1.3440(3) 0.2042(3) 0.4900(2) 0.0809(8) Uani 1 1 d . . . O9 O 1.0159(3) 0.3243(2) 0.47777(17) 0.0668(6) Uani 1 1 d . . . N2 N 1.3617(3) 0.3702(3) 0.2951(2) 0.0563(7) Uani 1 1 d . . . N3 N 1.2011(2) 0.1976(2) 0.32226(18) 0.0521(6) Uani 1 1 d . . . C14 C 1.1512(3) 0.4166(3) 1.0504(2) 0.0501(7) Uani 1 1 d . . . H14 H 1.1381 0.3807 1.1075 0.060 Uiso 1 1 calc R . . N1 N 1.0927(3) 0.7116(3) 0.9319(2) 0.0588(7) Uani 1 1 d . . . C11 C 1.2963(2) 0.3291(2) 0.81759(17) 0.0323(5) Uani 1 1 d . . . H11 H 1.2533 0.3706 0.7656 0.039 Uiso 1 1 calc R . . C12 C 1.2298(2) 0.3993(2) 0.89520(18) 0.0339(6) Uani 1 1 d . . . C13 C 1.2101(3) 0.3485(3) 0.98207(19) 0.0413(6) Uani 1 1 d . . . H13 H 1.2370 0.2678 0.9940 0.050 Uiso 1 1 calc R . . C15 C 1.1112(3) 0.5362(3) 1.0366(2) 0.0479(7) Uani 1 1 d . . . H15 H 1.0714 0.5819 1.0829 0.058 Uiso 1 1 calc R . . C16 C 1.1333(2) 0.5848(2) 0.9504(2) 0.0426(7) Uani 1 1 d . . . C17 C 1.1903(2) 0.5191(2) 0.87986(19) 0.0388(6) Uani 1 1 d . . . H17 H 1.2018 0.5554 0.8226 0.047 Uiso 1 1 calc R . . C18 C 1.2886(2) 0.2074(2) 0.83217(18) 0.0346(6) Uani 1 1 d . . . C19 C 1.3860(3) 0.1087(2) 0.8585(2) 0.0471(7) Uani 1 1 d . . . H19 H 1.4597 0.1160 0.8650 0.057 Uiso 1 1 calc R . . C20 C 1.3771(3) -0.0010(3) 0.8755(3) 0.0578(9) Uani 1 1 d . . . C24 C 1.4864(4) -0.1061(3) 0.9041(4) 0.1009(17) Uani 1 1 d . . . H24A H 1.4684 -0.1330 0.9656 0.151 Uiso 1 1 calc R . . H24B H 1.5580 -0.0848 0.8972 0.151 Uiso 1 1 calc R . . H24C H 1.5020 -0.1671 0.8678 0.151 Uiso 1 1 calc R . . C21 C 1.2658(4) -0.0083(3) 0.8666(3) 0.0598(9) Uani 1 1 d . . . H21 H 1.2580 -0.0810 0.8781 0.072 Uiso 1 1 calc R . . C22 C 1.1649(3) 0.0879(3) 0.8413(2) 0.0490(7) Uani 1 1 d . . . C25 C 1.0438(3) 0.0752(3) 0.8353(3) 0.0707(11) Uani 1 1 d . . . H25A H 0.9776 0.1317 0.8681 0.106 Uiso 1 1 calc R . . H25B H 1.0473 -0.0018 0.8600 0.106 Uiso 1 1 calc R . . H25C H 1.0294 0.0878 0.7739 0.106 Uiso 1 1 calc R . . C23 C 1.1786(2) 0.1958(2) 0.82355(18) 0.0359(6) Uani 1 1 d . . . C8 C 1.4294(2) 0.3256(2) 0.79472(18) 0.0344(6) Uani 1 1 d . . . C7 C 1.5027(3) 0.3109(2) 0.8605(2) 0.0407(6) Uani 1 1 d . . . H7 H 1.4698 0.3040 0.9200 0.049 Uiso 1 1 calc R . . C6 C 1.6243(3) 0.3061(3) 0.8404(2) 0.0471(7) Uani 1 1 d . . . C10 C 1.7024(3) 0.2875(4) 0.9143(3) 0.0759(11) Uani 1 1 d . . . H10A H 1.7392 0.2055 0.9326 0.114 Uiso 1 1 calc R . . H10B H 1.6512 0.3261 0.9642 0.114 Uiso 1 1 calc R . . H10C H 1.7662 0.3190 0.8931 0.114 Uiso 1 1 calc R . . C5 C 1.6702(3) 0.3203(3) 0.7525(2) 0.0555(8) Uani 1 1 d . . . H5 H 1.7509 0.3187 0.7384 0.067 Uiso 1 1 calc R . . C4 C 1.6000(3) 0.3371(3) 0.6835(2) 0.0518(8) Uani 1 1 d . . . C9 C 1.6530(4) 0.3578(5) 0.5871(3) 0.0833(12) Uani 1 1 d . . . H9A H 1.7254 0.3763 0.5856 0.125 Uiso 1 1 calc R . . H9B H 1.5925 0.4215 0.5564 0.125 Uiso 1 1 calc R . . H9C H 1.6746 0.2887 0.5583 0.125 Uiso 1 1 calc R . . C33 C 1.1138(4) 0.2034(3) 0.2773(3) 0.0796(12) Uani 1 1 d . . . H33 H 1.0462 0.2726 0.2721 0.096 Uiso 1 1 calc R . . C34 C 1.1184(6) 0.1108(4) 0.2376(5) 0.125(2) Uani 1 1 d . . . H34 H 1.0546 0.1190 0.2057 0.150 Uiso 1 1 calc R . . C35 C 1.2123(6) 0.0100(4) 0.2440(4) 0.1104(19) Uani 1 1 d . . . H35 H 1.2154 -0.0531 0.2174 0.132 Uiso 1 1 calc R . . C36 C 1.3029(6) 0.0024(4) 0.2904(4) 0.112(2) Uani 1 1 d . . . H36 H 1.3698 -0.0671 0.2976 0.134 Uiso 1 1 calc R . . C37 C 1.2949(4) 0.0988(4) 0.3269(3) 0.0885(14) Uani 1 1 d . . . H37 H 1.3598 0.0934 0.3565 0.106 Uiso 1 1 calc R . . C28 C 1.3486(3) 0.3962(3) 0.2090(2) 0.0640(9) Uani 1 1 d . . . H28 H 1.2719 0.4099 0.1916 0.077 Uiso 1 1 calc R . . C29 C 1.4429(4) 0.4038(4) 0.1437(3) 0.0762(11) Uani 1 1 d . . . H29 H 1.4299 0.4210 0.0839 0.091 Uiso 1 1 calc R . . C30 C 1.5534(4) 0.3860(4) 0.1678(4) 0.0840(13) Uani 1 1 d . . . H30 H 1.6182 0.3902 0.1248 0.101 Uiso 1 1 calc R . . C32 C 1.4691(4) 0.3543(5) 0.3183(3) 0.0874(14) Uani 1 1 d . . . H32 H 1.4796 0.3372 0.3785 0.105 Uiso 1 1 calc R . . C31 C 1.5699(4) 0.3619(5) 0.2559(4) 0.1025(17) Uani 1 1 d . . . H31 H 1.6452 0.3507 0.2743 0.123 Uiso 1 1 calc R . . C1 C 1.3346(3) 0.2853(3) 0.5313(2) 0.0559(8) Uani 1 1 d . . . C2 C 1.4192(3) 0.2550(3) 0.6033(2) 0.0545(8) Uani 1 1 d . . . H2A H 1.3983 0.2009 0.6505 0.065 Uiso 1 1 calc R . . H2B H 1.5043 0.2176 0.5783 0.065 Uiso 1 1 calc R . . C26 C 1.0608(3) 0.3165(3) 0.7107(2) 0.0467(7) Uani 1 1 d . . . H26A H 1.0293 0.2604 0.6974 0.056 Uiso 1 1 calc R . . H26B H 1.1394 0.3060 0.6741 0.056 Uiso 1 1 calc R . . C3 C 1.4805(3) 0.3376(2) 0.70613(19) 0.0411(6) Uani 1 1 d . . . C27 C 0.9710(3) 0.4382(3) 0.6883(2) 0.0439(7) Uani 1 1 d . . . O13 O 0.1938(3) 0.5890(3) 0.6300(2) 0.1012(10) Uani 1 1 d . . . O10 O 0.0323(16) 0.1009(8) 0.5516(7) 0.390(9) Uani 1 1 d . . . O11 O 0.6198(17) 0.0381(8) 0.4364(11) 0.435(10) Uani 1 1 d . . . O12 O 0.8052(13) 0.1394(14) 0.4121(10) 0.394(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04584(16) 0.04872(17) 0.04295(16) -0.01023(11) -0.01460(10) -0.00602(11) O4 0.103(2) 0.0430(14) 0.109(2) -0.0095(14) 0.0092(19) -0.0206(15) O5 0.096(2) 0.0593(16) 0.109(2) -0.0453(17) 0.0030(18) -0.0032(15) O3 0.0526(12) 0.0538(12) 0.0353(11) -0.0038(9) -0.0148(9) -0.0099(10) O6 0.0342(9) 0.0385(10) 0.0407(10) -0.0077(8) -0.0101(8) -0.0078(8) O8 0.0847(17) 0.0432(13) 0.0586(15) -0.0133(11) -0.0186(13) -0.0002(12) O7 0.0549(13) 0.0584(14) 0.0532(13) -0.0083(11) -0.0215(11) 0.0024(10) O2 0.0616(14) 0.0758(17) 0.0527(14) -0.0048(12) -0.0270(11) -0.0087(13) O1 0.095(2) 0.0831(19) 0.0693(18) -0.0201(15) -0.0378(16) -0.0209(16) O9 0.0699(15) 0.0741(16) 0.0582(15) -0.0181(12) -0.0009(12) -0.0263(13) N2 0.0481(15) 0.0599(17) 0.0600(18) -0.0119(14) -0.0070(13) -0.0162(13) N3 0.0519(15) 0.0491(15) 0.0517(16) -0.0122(12) -0.0130(12) -0.0087(12) C14 0.0493(16) 0.068(2) 0.0388(16) -0.0068(14) -0.0086(13) -0.0256(15) N1 0.0491(15) 0.0467(15) 0.083(2) -0.0239(16) -0.0132(15) -0.0110(13) C11 0.0332(12) 0.0310(13) 0.0343(13) -0.0030(10) -0.0108(10) -0.0105(10) C12 0.0288(12) 0.0367(14) 0.0394(14) -0.0058(11) -0.0081(10) -0.0130(11) C13 0.0433(15) 0.0460(15) 0.0378(15) -0.0021(12) -0.0106(12) -0.0183(13) C15 0.0387(15) 0.066(2) 0.0472(17) -0.0263(15) -0.0050(13) -0.0199(14) C16 0.0315(13) 0.0388(15) 0.0611(19) -0.0156(13) -0.0084(13) -0.0114(12) C17 0.0352(13) 0.0395(15) 0.0444(16) -0.0057(12) -0.0057(11) -0.0154(12) C18 0.0394(14) 0.0305(13) 0.0354(14) -0.0047(10) -0.0111(11) -0.0111(11) C19 0.0455(16) 0.0361(15) 0.0587(19) -0.0009(13) -0.0213(14) -0.0090(13) C20 0.063(2) 0.0334(16) 0.075(2) 0.0032(15) -0.0269(18) -0.0109(15) C24 0.086(3) 0.037(2) 0.170(5) 0.021(2) -0.056(3) -0.006(2) C21 0.073(2) 0.0339(16) 0.077(2) 0.0020(15) -0.0231(19) -0.0222(16) C22 0.0485(16) 0.0419(16) 0.062(2) -0.0088(14) -0.0101(14) -0.0203(14) C25 0.062(2) 0.057(2) 0.108(3) -0.007(2) -0.022(2) -0.0338(18) C23 0.0366(13) 0.0322(13) 0.0386(15) -0.0078(11) -0.0085(11) -0.0089(11) C8 0.0346(13) 0.0307(13) 0.0377(14) -0.0060(10) -0.0088(11) -0.0087(11) C7 0.0389(14) 0.0460(15) 0.0401(15) -0.0099(12) -0.0079(12) -0.0150(12) C6 0.0372(14) 0.0506(17) 0.0568(19) -0.0155(14) -0.0120(13) -0.0128(13) C10 0.0479(19) 0.109(3) 0.080(3) -0.022(2) -0.0253(18) -0.026(2) C5 0.0360(15) 0.062(2) 0.072(2) -0.0197(17) 0.0000(15) -0.0188(14) C4 0.0461(17) 0.0550(19) 0.0522(19) -0.0092(15) 0.0031(14) -0.0183(15) C9 0.074(3) 0.116(3) 0.057(2) -0.013(2) 0.016(2) -0.040(2) C33 0.079(3) 0.055(2) 0.113(4) -0.014(2) -0.051(3) -0.0136(19) C34 0.145(5) 0.066(3) 0.192(7) -0.020(3) -0.106(5) -0.028(3) C35 0.135(4) 0.058(3) 0.146(5) -0.038(3) -0.062(4) -0.013(3) C36 0.117(4) 0.063(3) 0.140(5) -0.034(3) -0.059(4) 0.013(3) C37 0.080(3) 0.073(3) 0.097(3) -0.039(2) -0.041(2) 0.015(2) C28 0.060(2) 0.079(2) 0.058(2) -0.0137(18) -0.0078(17) -0.0277(19) C29 0.083(3) 0.082(3) 0.070(3) -0.021(2) 0.003(2) -0.037(2) C30 0.069(3) 0.096(3) 0.093(3) -0.017(3) 0.009(2) -0.041(2) C32 0.065(2) 0.121(4) 0.079(3) 0.003(3) -0.022(2) -0.037(3) C31 0.060(3) 0.147(5) 0.109(4) 0.006(3) -0.016(2) -0.053(3) C1 0.0512(18) 0.078(2) 0.0385(17) -0.0112(17) -0.0105(14) -0.0193(18) C2 0.0527(17) 0.062(2) 0.0430(17) -0.0081(15) -0.0166(14) -0.0089(15) C26 0.0469(16) 0.0456(16) 0.0428(16) -0.0121(13) -0.0141(13) -0.0045(13) C3 0.0419(15) 0.0411(15) 0.0393(15) -0.0064(12) -0.0086(12) -0.0116(12) C27 0.0351(14) 0.0474(17) 0.0432(16) -0.0011(13) -0.0058(12) -0.0093(12) O13 0.092(2) 0.108(2) 0.086(2) -0.0264(19) -0.0133(18) -0.0087(19) O10 0.74(3) 0.183(7) 0.234(10) 0.014(7) 0.012(13) -0.197(12) O11 0.64(3) 0.169(8) 0.51(2) -0.002(10) -0.27(2) -0.085(12) O12 0.332(15) 0.45(2) 0.361(17) -0.117(14) 0.000(13) -0.081(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O7 2.263(2) 2_766 ? Cd1 N3 2.332(3) . ? Cd1 O9 2.342(3) . ? Cd1 O2 2.347(2) . ? Cd1 N2 2.362(3) . ? Cd1 O1 2.525(3) . ? O4 N1 1.227(4) . ? O5 N1 1.221(4) . ? O3 C3 1.393(3) . ? O3 C2 1.418(4) . ? O6 C23 1.387(3) . ? O6 C26 1.423(3) . ? O8 C27 1.219(4) . ? O7 C27 1.265(4) . ? O7 Cd1 2.263(2) 2_766 ? O2 C1 1.237(4) . ? O1 C1 1.240(5) . ? N2 C32 1.305(5) . ? N2 C28 1.326(5) . ? N3 C33 1.306(4) . ? N3 C37 1.308(5) . ? C14 C15 1.373(5) . ? C14 C13 1.377(4) . ? C14 H14 0.9300 . ? N1 C16 1.460(4) . ? C11 C12 1.516(4) . ? C11 C8 1.530(3) . ? C11 C18 1.532(3) . ? C11 H11 0.9800 . ? C12 C17 1.377(4) . ? C12 C13 1.395(4) . ? C13 H13 0.9300 . ? C15 C16 1.383(4) . ? C15 H15 0.9300 . ? C16 C17 1.385(4) . ? C17 H17 0.9300 . ? C18 C19 1.384(4) . ? C18 C23 1.386(4) . ? C19 C20 1.390(4) . ? C19 H19 0.9300 . ? C20 C21 1.378(5) . ? C20 C24 1.513(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C21 C22 1.387(5) . ? C21 H21 0.9300 . ? C22 C23 1.393(4) . ? C22 C25 1.512(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C8 C7 1.382(4) . ? C8 C3 1.394(4) . ? C7 C6 1.392(4) . ? C7 H7 0.9300 . ? C6 C5 1.370(5) . ? C6 C10 1.512(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C5 C4 1.392(5) . ? C5 H5 0.9300 . ? C4 C3 1.387(4) . ? C4 C9 1.521(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C33 C34 1.371(6) . ? C33 H33 0.9300 . ? C34 C35 1.325(7) . ? C34 H34 0.9300 . ? C35 C36 1.346(7) . ? C35 H35 0.9300 . ? C36 C37 1.374(7) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C28 C29 1.380(5) . ? C28 H28 0.9300 . ? C29 C30 1.341(6) . ? C29 H29 0.9300 . ? C30 C31 1.362(7) . ? C30 H30 0.9300 . ? C32 C31 1.413(7) . ? C32 H32 0.9300 . ? C31 H31 0.9300 . ? C1 C2 1.517(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C26 C27 1.508(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? 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 O7 Cd1 N3 134.33(9) 2_766 . ? O7 Cd1 O9 85.85(9) 2_766 . ? N3 Cd1 O9 83.96(9) . . ? O7 Cd1 O2 85.66(9) 2_766 . ? N3 Cd1 O2 139.45(9) . . ? O9 Cd1 O2 94.69(9) . . ? O7 Cd1 N2 97.00(10) 2_766 . ? N3 Cd1 N2 89.37(10) . . ? O9 Cd1 N2 172.82(9) . . ? O2 Cd1 N2 92.11(10) . . ? O7 Cd1 O1 138.84(9) 2_766 . ? N3 Cd1 O1 86.50(9) . . ? O9 Cd1 O1 95.42(10) . . ? O2 Cd1 O1 53.19(9) . . ? N2 Cd1 O1 86.79(11) . . ? C3 O3 C2 113.9(2) . . ? C23 O6 C26 113.9(2) . . ? C27 O7 Cd1 102.1(2) . 2_766 ? C1 O2 Cd1 95.6(2) . . ? C1 O1 Cd1 87.2(2) . . ? C32 N2 C28 117.3(3) . . ? C32 N2 Cd1 125.4(3) . . ? C28 N2 Cd1 117.2(2) . . ? C33 N3 C37 116.5(3) . . ? C33 N3 Cd1 122.2(2) . . ? C37 N3 Cd1 121.3(3) . . ? C15 C14 C13 122.0(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? O5 N1 O4 123.3(3) . . ? O5 N1 C16 118.3(3) . . ? O4 N1 C16 118.4(3) . . ? C12 C11 C8 111.3(2) . . ? C12 C11 C18 112.5(2) . . ? C8 C11 C18 112.6(2) . . ? C12 C11 H11 106.7 . . ? C8 C11 H11 106.7 . . ? C18 C11 H11 106.7 . . ? C17 C12 C13 118.3(3) . . ? C17 C12 C11 118.4(2) . . ? C13 C12 C11 123.2(2) . . ? C14 C13 C12 120.7(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C14 C15 C16 116.5(3) . . ? C14 C15 H15 121.8 . . ? C16 C15 H15 121.8 . . ? C15 C16 C17 123.1(3) . . ? C15 C16 N1 118.9(3) . . ? C17 C16 N1 118.0(3) . . ? C12 C17 C16 119.4(3) . . ? C12 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C23 118.5(2) . . ? C19 C18 C11 122.2(2) . . ? C23 C18 C11 119.2(2) . . ? C18 C19 C20 122.2(3) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C21 C20 C19 117.3(3) . . ? C21 C20 C24 122.7(3) . . ? C19 C20 C24 120.0(3) . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C21 C22 122.9(3) . . ? C20 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C21 C22 C23 117.8(3) . . ? C21 C22 C25 120.7(3) . . ? C23 C22 C25 121.6(3) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C18 C23 O6 118.3(2) . . ? C18 C23 C22 121.3(2) . . ? O6 C23 C22 120.3(2) . . ? C7 C8 C3 117.7(2) . . ? C7 C8 C11 121.6(2) . . ? C3 C8 C11 120.7(2) . . ? C8 C7 C6 122.0(3) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C5 C6 C7 118.3(3) . . ? C5 C6 C10 121.3(3) . . ? C7 C6 C10 120.4(3) . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C5 C4 122.1(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C3 C4 C5 117.8(3) . . ? C3 C4 C9 122.0(3) . . ? C5 C4 C9 120.2(3) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C33 C34 122.3(4) . . ? N3 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C35 C34 C33 121.1(5) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 117.4(4) . . ? C34 C35 H35 121.3 . . ? C36 C35 H35 121.3 . . ? C35 C36 C37 119.0(4) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? N3 C37 C36 123.7(4) . . ? N3 C37 H37 118.2 . . ? C36 C37 H37 118.2 . . ? N2 C28 C29 123.3(4) . . ? N2 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C30 C29 C28 119.0(4) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 119.5(4) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? N2 C32 C31 122.9(4) . . ? N2 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? C30 C31 C32 117.9(4) . . ? C30 C31 H31 121.0 . . ? C32 C31 H31 121.0 . . ? O2 C1 O1 123.9(3) . . ? O2 C1 C2 119.8(3) . . ? O1 C1 C2 116.3(3) . . ? O3 C2 C1 110.0(3) . . ? O3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O6 C26 C27 111.0(2) . . ? O6 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? O6 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C4 C3 O3 119.3(3) . . ? C4 C3 C8 121.9(3) . . ? O3 C3 C8 118.7(2) . . ? O8 C27 O7 122.7(3) . . ? O8 C27 C26 122.6(3) . . ? O7 C27 C26 114.7(3) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.635 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.073 # Attachment '- lignad 2.cif' data_bn _database_code_depnum_ccdc_archive 'CCDC 840829' #TrackingRef '- lignad 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 N O8' _chemical_formula_weight 493.50 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' _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 16.297(3) _cell_length_b 9.222(2) _cell_length_c 16.374(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.019(15) _cell_angle_gamma 90.00 _cell_volume 2454.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11872 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.1260 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4427 _reflns_number_gt 2439 _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^)+(0.0515P)^2^+0.3757P] 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 4427 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.2006 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 O3 O 0.77869(13) 0.6918(3) 0.05538(12) 0.0515(6) Uani 1 1 d . . . O6 O 0.77806(15) 0.9606(3) -0.14976(13) 0.0607(7) Uani 1 1 d . . . O4 O 0.81461(16) 1.0799(3) 0.10372(14) 0.0723(8) Uani 1 1 d . . . O2 O 0.90254(15) 0.5667(3) -0.01820(16) 0.0784(9) Uani 1 1 d . . . O1 O 0.99293(16) 0.6352(4) 0.08216(16) 0.0902(10) Uani 1 1 d . . . H1 H 1.0238 0.5837 0.0573 0.135 Uiso 1 1 calc R . . O5 O 0.8637(2) 1.2752(4) 0.0559(2) 0.1201(13) Uani 1 1 d . . . O8 O 0.9898(2) 0.8988(7) -0.1140(3) 0.1494(17) Uani 1 1 d . . . H8 H 1.0160 0.8672 -0.0732 0.224 Uiso 1 1 calc R . . O7 O 0.9049(2) 1.0027(5) -0.0353(2) 0.1274(15) Uani 1 1 d . . . C10 C 0.67434(18) 0.8710(3) 0.07315(15) 0.0388(7) Uani 1 1 d . . . C3 C 0.71625(19) 0.7464(3) 0.10111(17) 0.0439(8) Uani 1 1 d . . . C12 C 0.67739(19) 1.1050(4) -0.01133(16) 0.0429(8) Uani 1 1 d . . . C11 C 0.69949(18) 0.9435(3) -0.00494(16) 0.0410(8) Uani 1 1 d . . . H11 H 0.7596 0.9370 -0.0042 0.049 Uiso 1 1 calc R . . C9 C 0.61199(19) 0.9241(4) 0.11853(16) 0.0438(8) Uani 1 1 d . . . H9 H 0.5843 1.0080 0.1012 0.053 Uiso 1 1 calc R . . C18 C 0.66483(19) 0.8651(3) -0.08271(16) 0.0429(8) Uani 1 1 d . . . C7 C 0.58980(19) 0.8542(4) 0.18974(16) 0.0466(8) Uani 1 1 d . . . C4 C 0.6945(2) 0.6708(4) 0.17118(17) 0.0493(9) Uani 1 1 d . . . C25 C 0.7060(2) 0.8777(4) -0.15389(18) 0.0502(8) Uani 1 1 d . . . C17 C 0.7298(2) 1.2180(4) 0.01458(17) 0.0480(8) Uani 1 1 d . . . C13 C 0.6025(2) 1.1490(4) -0.04989(18) 0.0500(8) Uani 1 1 d . . . H13 H 0.5646 1.0785 -0.0677 0.060 Uiso 1 1 calc R . . C19 C 0.5913(2) 0.7890(4) -0.08634(17) 0.0462(8) Uani 1 1 d . . . H19 H 0.5634 0.7795 -0.0390 0.055 Uiso 1 1 calc R . . C14 C 0.5825(2) 1.2933(4) -0.0627(2) 0.0619(10) Uani 1 1 d . . . H14 H 0.5313 1.3179 -0.0874 0.074 Uiso 1 1 calc R . . C20 C 0.5580(2) 0.7263(4) -0.1586(2) 0.0546(9) Uani 1 1 d . . . C2 C 0.8593(2) 0.7186(4) 0.0903(2) 0.0601(10) Uani 1 1 d . . . H2A H 0.8631 0.6909 0.1476 0.072 Uiso 1 1 calc R . . H2B H 0.8718 0.8211 0.0869 0.072 Uiso 1 1 calc R . . C6 C 0.6310(2) 0.7283(4) 0.21303(18) 0.0515(9) Uani 1 1 d . . . H6 H 0.6153 0.6796 0.2592 0.062 Uiso 1 1 calc R . . C23 C 0.6751(3) 0.8191(4) -0.22753(19) 0.0614(10) Uani 1 1 d . . . C16 C 0.7113(3) 1.3619(4) -0.0009(2) 0.0604(10) Uani 1 1 d . . . H16 H 0.7495 1.4330 0.0150 0.072 Uiso 1 1 calc R . . C15 C 0.6378(3) 1.4009(4) -0.0391(2) 0.0650(10) Uani 1 1 d . . . H15 H 0.6253 1.4980 -0.0491 0.078 Uiso 1 1 calc R . . C22 C 0.6019(2) 0.7449(4) -0.2281(2) 0.0645(11) Uani 1 1 d . . . H22 H 0.5805 0.7051 -0.2773 0.077 Uiso 1 1 calc R . . C8 C 0.5236(2) 0.9143(5) 0.2398(2) 0.0693(11) Uani 1 1 d . . . H8A H 0.4732 0.8626 0.2270 0.104 Uiso 1 1 calc R . . H8B H 0.5155 1.0152 0.2273 0.104 Uiso 1 1 calc R . . H8C H 0.5398 0.9033 0.2970 0.104 Uiso 1 1 calc R . . C5 C 0.7366(3) 0.5331(4) 0.2007(2) 0.0688(11) Uani 1 1 d . . . H5A H 0.7791 0.5558 0.2422 0.103 Uiso 1 1 calc R . . H5B H 0.7603 0.4861 0.1556 0.103 Uiso 1 1 calc R . . H5C H 0.6971 0.4696 0.2229 0.103 Uiso 1 1 calc R . . C1 C 0.9199(2) 0.6327(4) 0.0452(2) 0.0593(10) Uani 1 1 d . . . C27 C 0.9171(3) 0.9375(6) -0.0950(3) 0.0804(13) Uani 1 1 d . . . C21 C 0.4765(2) 0.6487(5) -0.1629(2) 0.0783(12) Uani 1 1 d . . . H21A H 0.4698 0.6003 -0.1119 0.117 Uiso 1 1 calc R . . H21B H 0.4748 0.5786 -0.2064 0.117 Uiso 1 1 calc R . . H21C H 0.4329 0.7176 -0.1733 0.117 Uiso 1 1 calc R . . C24 C 0.7175(3) 0.8437(6) -0.3061(2) 0.0929(15) Uani 1 1 d . . . H24A H 0.7623 0.7766 -0.3087 0.139 Uiso 1 1 calc R . . H24B H 0.7382 0.9411 -0.3070 0.139 Uiso 1 1 calc R . . H24C H 0.6788 0.8289 -0.3523 0.139 Uiso 1 1 calc R . . C26 C 0.8528(3) 0.8845(6) -0.1574(3) 0.0821(13) Uani 1 1 d . . . H26A H 0.8713 0.8989 -0.2119 0.099 Uiso 1 1 calc R . . H26B H 0.8439 0.7815 -0.1498 0.099 Uiso 1 1 calc R . . N1 N 0.8082(2) 1.1887(4) 0.06018(19) 0.0658(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3 0.0451(13) 0.0603(16) 0.0486(11) -0.0043(10) -0.0001(10) 0.0053(12) O6 0.0559(16) 0.0644(17) 0.0634(14) 0.0020(12) 0.0161(11) -0.0034(14) O4 0.0796(19) 0.079(2) 0.0551(14) 0.0049(13) -0.0180(12) -0.0148(16) O2 0.0613(17) 0.099(2) 0.0754(17) -0.0204(15) 0.0057(13) 0.0029(16) O1 0.0528(17) 0.139(3) 0.0784(18) -0.0207(17) 0.0014(14) 0.0163(19) O5 0.078(2) 0.104(3) 0.173(3) 0.036(2) -0.035(2) -0.049(2) O8 0.058(2) 0.203(5) 0.188(4) -0.039(4) 0.021(2) 0.016(3) O7 0.069(2) 0.205(5) 0.108(3) -0.038(3) 0.0032(18) -0.008(2) C10 0.0422(18) 0.0374(18) 0.0360(14) 0.0020(13) -0.0017(12) -0.0049(16) C3 0.0455(19) 0.047(2) 0.0387(15) -0.0038(13) -0.0031(13) 0.0033(16) C12 0.0473(19) 0.045(2) 0.0366(14) 0.0021(13) 0.0049(13) -0.0006(17) C11 0.0389(18) 0.045(2) 0.0393(15) 0.0011(13) 0.0003(12) -0.0030(15) C9 0.0462(19) 0.044(2) 0.0398(15) 0.0030(13) -0.0029(13) 0.0019(16) C18 0.0462(19) 0.0394(19) 0.0429(15) 0.0025(13) 0.0010(13) 0.0052(16) C7 0.0453(19) 0.056(2) 0.0379(15) -0.0007(14) -0.0021(13) -0.0004(17) C4 0.057(2) 0.048(2) 0.0420(16) 0.0053(14) -0.0050(14) 0.0005(18) C25 0.053(2) 0.052(2) 0.0454(17) 0.0012(15) 0.0062(14) 0.0018(19) C17 0.055(2) 0.049(2) 0.0396(16) 0.0020(14) 0.0003(14) -0.0070(19) C13 0.054(2) 0.043(2) 0.0524(18) -0.0002(15) -0.0014(15) 0.0003(18) C19 0.052(2) 0.0427(19) 0.0432(16) -0.0009(14) 0.0007(14) 0.0026(17) C14 0.065(3) 0.053(2) 0.067(2) 0.0045(18) -0.0032(18) 0.011(2) C20 0.054(2) 0.050(2) 0.057(2) -0.0026(16) -0.0105(16) 0.0003(18) C2 0.054(2) 0.063(2) 0.062(2) -0.0052(18) -0.0032(17) 0.003(2) C6 0.060(2) 0.056(2) 0.0380(16) 0.0065(15) 0.0001(15) -0.0020(19) C23 0.073(3) 0.067(3) 0.0450(18) -0.0047(16) 0.0045(16) 0.002(2) C16 0.083(3) 0.044(2) 0.0538(19) -0.0011(16) 0.0068(18) -0.017(2) C15 0.088(3) 0.041(2) 0.066(2) 0.0041(17) 0.004(2) 0.007(2) C22 0.074(3) 0.068(3) 0.0502(19) -0.0140(17) -0.0088(18) 0.010(2) C8 0.070(3) 0.088(3) 0.0520(19) 0.0123(19) 0.0146(17) 0.015(2) C5 0.089(3) 0.059(3) 0.058(2) 0.0162(18) 0.0042(18) 0.019(2) C1 0.044(2) 0.076(3) 0.058(2) 0.0072(19) 0.0011(16) 0.001(2) C27 0.057(3) 0.097(4) 0.089(3) 0.005(3) 0.015(2) 0.000(3) C21 0.074(3) 0.082(3) 0.076(2) -0.013(2) -0.014(2) -0.014(3) C24 0.108(4) 0.124(4) 0.049(2) -0.007(2) 0.022(2) 0.003(3) C26 0.066(3) 0.100(4) 0.084(3) -0.012(2) 0.023(2) 0.011(3) N1 0.067(2) 0.064(2) 0.0658(18) 0.0029(17) -0.0058(16) -0.0175(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O3 C3 1.399(4) . ? O3 C2 1.418(4) . ? O6 C25 1.398(4) . ? O6 C26 1.419(4) . ? O4 N1 1.231(4) . ? O2 C1 1.219(4) . ? O1 C1 1.297(4) . ? O5 N1 1.212(4) . ? O8 C27 1.296(5) . ? O7 C27 1.176(5) . ? C10 C9 1.389(4) . ? C10 C3 1.397(4) . ? C10 C11 1.524(4) . ? C3 C4 1.409(4) . ? C12 C13 1.394(4) . ? C12 C17 1.395(4) . ? C12 C11 1.534(4) . ? C11 C18 1.537(4) . ? C9 C7 1.402(4) . ? C18 C19 1.386(4) . ? C18 C25 1.390(4) . ? C7 C6 1.381(5) . ? C7 C8 1.506(4) . ? C4 C6 1.386(5) . ? C4 C5 1.506(5) . ? C25 C23 1.384(5) . ? C17 C16 1.380(5) . ? C17 N1 1.459(5) . ? C13 C14 1.383(5) . ? C19 C20 1.393(4) . ? C14 C15 1.377(5) . ? C20 C22 1.397(5) . ? C20 C21 1.506(5) . ? C2 C1 1.500(5) . ? C23 C22 1.375(5) . ? C23 C24 1.520(5) . ? C16 C15 1.359(5) . ? C27 C26 1.494(6) . ? 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 C3 O3 C2 114.2(2) . . ? C25 O6 C26 116.6(3) . . ? C9 C10 C3 118.3(3) . . ? C9 C10 C11 122.9(3) . . ? C3 C10 C11 118.8(3) . . ? C10 C3 O3 118.5(3) . . ? C10 C3 C4 121.9(3) . . ? O3 C3 C4 119.5(3) . . ? C13 C12 C17 114.7(3) . . ? C13 C12 C11 120.5(3) . . ? C17 C12 C11 124.7(3) . . ? C10 C11 C12 114.0(2) . . ? C10 C11 C18 112.6(2) . . ? C12 C11 C18 109.2(2) . . ? C10 C9 C7 121.6(3) . . ? C19 C18 C25 118.3(3) . . ? C19 C18 C11 122.7(3) . . ? C25 C18 C11 118.9(3) . . ? C6 C7 C9 117.9(3) . . ? C6 C7 C8 120.8(3) . . ? C9 C7 C8 121.3(3) . . ? C6 C4 C3 116.9(3) . . ? C6 C4 C5 120.2(3) . . ? C3 C4 C5 122.9(3) . . ? C23 C25 C18 122.0(3) . . ? C23 C25 O6 120.6(3) . . ? C18 C25 O6 117.3(3) . . ? C16 C17 C12 122.8(3) . . ? C16 C17 N1 116.4(3) . . ? C12 C17 N1 120.8(3) . . ? C14 C13 C12 122.6(3) . . ? C18 C19 C20 122.1(3) . . ? C15 C14 C13 120.6(3) . . ? C19 C20 C22 116.8(3) . . ? C19 C20 C21 121.8(3) . . ? C22 C20 C21 121.3(3) . . ? O3 C2 C1 109.4(3) . . ? C7 C6 C4 123.4(3) . . ? C22 C23 C25 117.6(3) . . ? C22 C23 C24 120.9(3) . . ? C25 C23 C24 121.3(4) . . ? C15 C16 C17 120.9(4) . . ? C16 C15 C14 118.4(4) . . ? C23 C22 C20 123.3(3) . . ? O2 C1 O1 123.8(3) . . ? O2 C1 C2 124.2(3) . . ? O1 C1 C2 112.0(3) . . ? O7 C27 O8 123.5(5) . . ? O7 C27 C26 125.7(4) . . ? O8 C27 C26 110.8(4) . . ? O6 C26 C27 110.1(4) . . ? O5 N1 O4 122.4(3) . . ? O5 N1 C17 118.6(3) . . ? O4 N1 C17 118.9(3) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.197 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.048 # Attachment '- complex 6.cif' data_vskr_6 _database_code_depnum_ccdc_archive 'CCDC 844623' #TrackingRef '- complex 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H74 Cd2 N6 O20' _chemical_formula_weight 1592.19 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 P21/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 12.5560(10) _cell_length_b 25.231(2) _cell_length_c 12.2248(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.953(4) _cell_angle_gamma 90.00 _cell_volume 3788.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9947 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 26.90 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2249 _exptl_absorpt_correction_T_max 0.3831 _exptl_absorpt_process_details 'North et al., 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53316 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.48 _reflns_number_total 9492 _reflns_number_gt 6870 _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^)+(0.0634P)^2^+11.5704P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9492 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2383 _refine_ls_wR_factor_gt 0.2310 _refine_ls_goodness_of_fit_ref 1.294 _refine_ls_restrained_S_all 1.294 _refine_ls_shift/su_max 0.017 _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 N2 N 0.8153(5) 0.1127(3) 0.5278(6) 0.086(2) Uani 1 1 d G . . C33 C 0.8889(9) 0.1356(6) 0.6158(7) 0.36(2) Uani 1 1 d G . . H33 H 0.8732 0.1368 0.6868 0.430 Uiso 1 1 calc R . . C34 C 0.9860(9) 0.1567(7) 0.5975(12) 0.44(3) Uani 1 1 d G . . H34 H 1.0353 0.1720 0.6564 0.529 Uiso 1 1 calc R . . C35 C 1.0095(8) 0.1549(7) 0.4914(14) 0.31(2) Uani 1 1 d G . . H35 H 1.0745 0.1690 0.4792 0.369 Uiso 1 1 calc R . . C36 C 0.9359(11) 0.1320(8) 0.4034(10) 0.35(2) Uani 1 1 d G . . H36 H 0.9516 0.1308 0.3324 0.423 Uiso 1 1 calc R . . C37 C 0.8388(9) 0.1109(6) 0.4217(7) 0.36(2) Uani 1 1 d G . . H37 H 0.7896 0.0956 0.3629 0.427 Uiso 1 1 calc R . . C26 C 0.8124(6) -0.0067(3) 0.8411(6) 0.0551(16) Uani 1 1 d . . . H26A H 0.8770 0.0119 0.8794 0.066 Uiso 1 1 calc R . . H26B H 0.7670 -0.0136 0.8948 0.066 Uiso 1 1 calc R . . Cd1 Cd 0.64818(4) 0.087370(18) 0.56661(4) 0.05149(18) Uani 1 1 d . . . C23 C 0.0859(5) 0.0863(3) 0.1258(6) 0.0495(14) Uani 1 1 d . . . C8 C 0.3050(5) 0.1119(2) 0.0186(5) 0.0391(12) Uani 1 1 d . . . C1 C 0.5483(5) 0.0814(3) 0.3423(5) 0.0459(14) Uani 1 1 d . . . C4 C 0.4747(5) 0.0809(3) -0.0269(6) 0.0504(15) Uani 1 1 d . . . C3 C 0.4164(5) 0.1019(2) 0.0493(5) 0.0397(12) Uani 1 1 d . . . C7 C 0.2509(5) 0.0985(3) -0.0883(5) 0.0476(14) Uani 1 1 d . . . H7 H 0.1768 0.1053 -0.1097 0.057 Uiso 1 1 calc R . . C6 C 0.3051(6) 0.0747(3) -0.1652(5) 0.0525(16) Uani 1 1 d . . . C5 C 0.4179(6) 0.0686(3) -0.1324(6) 0.0537(16) Uani 1 1 d . . . H5 H 0.4562 0.0556 -0.1842 0.064 Uiso 1 1 calc R . . C18 C 0.1265(5) 0.1297(3) 0.0784(5) 0.0435(13) Uani 1 1 d . . . C2 C 0.4854(5) 0.0694(3) 0.2278(5) 0.0492(15) Uani 1 1 d . . . H2A H 0.5233 0.0424 0.1944 0.059 Uiso 1 1 calc R . . H2B H 0.4147 0.0554 0.2330 0.059 Uiso 1 1 calc R . . C22 C -0.0246(7) 0.0751(3) 0.1049(8) 0.072(2) Uani 1 1 d . . . C19 C 0.0544(5) 0.1627(3) 0.0072(6) 0.0610(18) Uani 1 1 d . . . H19 H 0.0808 0.1919 -0.0252 0.073 Uiso 1 1 calc R . . C10 C 0.2440(7) 0.0574(3) -0.2788(6) 0.069(2) Uani 1 1 d . . . H10A H 0.2652 0.0791 -0.3352 0.103 Uiso 1 1 calc R . . H10B H 0.1672 0.0610 -0.2828 0.103 Uiso 1 1 calc R . . H10C H 0.2608 0.0210 -0.2909 0.103 Uiso 1 1 calc R . . C9 C 0.5963(6) 0.0733(3) 0.0056(7) 0.067(2) Uani 1 1 d . . . H9A H 0.6123 0.0365 0.0209 0.100 Uiso 1 1 calc R . . H9B H 0.6248 0.0939 0.0711 0.100 Uiso 1 1 calc R . . H9C H 0.6292 0.0846 -0.0547 0.100 Uiso 1 1 calc R . . C20 C -0.0568(6) 0.1522(4) -0.0157(8) 0.073(2) Uani 1 1 d . . . C21 C -0.0938(6) 0.1093(4) 0.0316(8) 0.077(2) Uani 1 1 d . . . H21 H -0.1681 0.1021 0.0149 0.093 Uiso 1 1 calc R . . C12 C 0.2715(5) 0.2002(2) 0.1056(5) 0.0439(13) Uani 1 1 d . . . C17 C 0.2389(6) 0.2355(3) 0.1816(6) 0.0615(18) Uani 1 1 d . . . C16 C 0.2619(8) 0.2900(3) 0.1837(9) 0.083(3) Uani 1 1 d . . . H16 H 0.2394 0.3118 0.2359 0.099 Uiso 1 1 calc R . . C14 C 0.3480(7) 0.2783(3) 0.0348(8) 0.076(2) Uani 1 1 d . . . H14 H 0.3858 0.2926 -0.0161 0.091 Uiso 1 1 calc R . . C15 C 0.3164(9) 0.3104(4) 0.1105(10) 0.095(3) Uani 1 1 d . . . H15 H 0.3325 0.3464 0.1118 0.114 Uiso 1 1 calc R . . N1 N 0.1801(7) 0.2184(3) 0.2658(6) 0.0760(19) Uani 1 1 d . . . O4 O 0.1979(6) 0.1748(3) 0.3088(5) 0.0899(19) Uani 1 1 d . . . O5 O 0.1089(7) 0.2496(3) 0.2892(7) 0.127(3) Uani 1 1 d . . . O1 O 0.5850(4) 0.04175(18) 0.4023(4) 0.0554(11) Uani 1 1 d . . . O2 O 0.5589(5) 0.1275(2) 0.3779(4) 0.0706(15) Uani 1 1 d . . . O3 O 0.4705(3) 0.11500(16) 0.1572(3) 0.0413(9) Uani 1 1 d . . . O7 O 0.7257(5) 0.0724(2) 0.7698(5) 0.0797(17) Uani 1 1 d . . . O8 O 0.7280(5) 0.0100(2) 0.6494(4) 0.0698(14) Uani 1 1 d . . . N3 N 0.6220(6) 0.1704(2) 0.6365(6) 0.0659(17) Uani 1 1 d . . . O6 O 0.1570(4) 0.05531(17) 0.2006(4) 0.0541(11) Uani 1 1 d . . . O9 O 0.4789(5) 0.0640(2) 0.6000(5) 0.0593(12) Uani 1 1 d . . . C11 C 0.2489(4) 0.1402(2) 0.1018(5) 0.0398(12) Uani 1 1 d . . . H11 H 0.2797 0.1260 0.1762 0.048 Uiso 1 1 calc R . . C13 C 0.3253(6) 0.2243(3) 0.0312(6) 0.0561(16) Uani 1 1 d . . . H13 H 0.3471 0.2036 -0.0233 0.067 Uiso 1 1 calc R . . C28 C 0.5841(8) 0.1753(4) 0.7289(8) 0.086(3) Uani 1 1 d . . . H28 H 0.5656 0.1446 0.7630 0.103 Uiso 1 1 calc R . . C29 C 0.5705(11) 0.2235(5) 0.7776(12) 0.131(6) Uani 1 1 d . . . H29 H 0.5475 0.2245 0.8452 0.157 Uiso 1 1 calc R . . C32 C 0.6378(11) 0.2144(4) 0.5918(12) 0.117(4) Uani 1 1 d . . . H32 H 0.6598 0.2131 0.5237 0.140 Uiso 1 1 calc R . . C30 C 0.5900(15) 0.2678(7) 0.7294(15) 0.166(9) Uani 1 1 d . . . H30 H 0.5791 0.3005 0.7606 0.199 Uiso 1 1 calc R . . C31 C 0.6249(15) 0.2649(5) 0.6365(18) 0.158(7) Uani 1 1 d . . . H31 H 0.6410 0.2954 0.6005 0.189 Uiso 1 1 calc R . . C25 C -0.0692(9) 0.0284(5) 0.1596(10) 0.110(4) Uani 1 1 d . . . H25A H -0.0585 -0.0036 0.1208 0.165 Uiso 1 1 calc R . . H25B H -0.1455 0.0335 0.1564 0.165 Uiso 1 1 calc R . . H25C H -0.0316 0.0257 0.2362 0.165 Uiso 1 1 calc R . . C24 C -0.1345(7) 0.1888(5) -0.0906(12) 0.123(5) Uani 1 1 d . . . H24A H -0.1782 0.1688 -0.1502 0.184 Uiso 1 1 calc R . . H24B H -0.0940 0.2152 -0.1215 0.184 Uiso 1 1 calc R . . H24C H -0.1808 0.2059 -0.0480 0.184 Uiso 1 1 calc R . . O10 O 0.2990(6) 0.0874(3) 0.4406(6) 0.102(2) Uani 1 1 d . . . C27 C 0.7504(5) 0.0279(3) 0.7469(6) 0.0508(15) Uani 1 1 d . . . H9M H 0.475(7) 0.030(4) 0.597(8) 0.08(3) Uiso 1 1 d . . . H9N H 0.427(8) 0.070(4) 0.537(8) 0.08(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N2 0.068(5) 0.115(6) 0.072(5) 0.015(4) 0.008(4) -0.023(4) C33 0.097(13) 0.30(3) 0.70(7) -0.08(4) 0.13(3) -0.092(17) C34 0.34(4) 0.20(2) 0.92(10) 0.06(4) 0.44(6) -0.03(2) C35 0.113(14) 0.50(5) 0.31(3) 0.18(3) 0.033(17) -0.10(2) C36 0.22(2) 0.62(6) 0.28(3) -0.29(4) 0.19(2) -0.27(3) C37 0.159(17) 0.65(6) 0.30(3) -0.34(4) 0.142(19) -0.22(3) C26 0.065(4) 0.049(4) 0.046(4) 0.004(3) 0.001(3) -0.001(3) Cd1 0.0588(3) 0.0414(3) 0.0510(3) 0.0011(2) 0.0035(2) -0.0015(2) C23 0.046(3) 0.051(3) 0.052(3) 0.006(3) 0.013(3) 0.005(3) C8 0.034(3) 0.046(3) 0.037(3) 0.006(2) 0.006(2) -0.003(2) C1 0.038(3) 0.054(4) 0.044(3) 0.008(3) 0.004(2) -0.002(3) C4 0.046(4) 0.050(4) 0.059(4) 0.010(3) 0.019(3) 0.002(3) C3 0.039(3) 0.038(3) 0.040(3) 0.002(2) 0.004(2) -0.002(2) C7 0.044(3) 0.053(4) 0.044(3) 0.005(3) 0.003(3) -0.006(3) C6 0.063(4) 0.050(4) 0.044(3) 0.008(3) 0.008(3) -0.013(3) C5 0.058(4) 0.052(4) 0.054(4) 0.001(3) 0.020(3) 0.000(3) C18 0.033(3) 0.052(3) 0.046(3) 0.004(3) 0.008(2) 0.000(2) C2 0.047(4) 0.048(3) 0.046(3) 0.010(3) -0.005(3) -0.004(3) C22 0.063(5) 0.070(5) 0.093(6) -0.004(4) 0.037(5) -0.020(4) C19 0.041(4) 0.065(4) 0.071(5) 0.018(4) 0.001(3) 0.006(3) C10 0.076(5) 0.080(5) 0.049(4) -0.011(4) 0.012(4) -0.025(4) C9 0.046(4) 0.083(5) 0.075(5) 0.000(4) 0.022(4) 0.008(4) C20 0.044(4) 0.078(5) 0.091(6) 0.009(5) 0.000(4) 0.009(4) C21 0.036(4) 0.085(6) 0.109(7) 0.010(5) 0.010(4) -0.003(4) C12 0.039(3) 0.049(3) 0.039(3) 0.001(2) -0.001(2) 0.007(3) C17 0.066(5) 0.072(5) 0.045(4) 0.007(3) 0.010(3) 0.014(4) C16 0.106(7) 0.047(4) 0.096(7) -0.009(4) 0.024(6) 0.010(4) C14 0.082(6) 0.055(4) 0.089(6) 0.016(4) 0.016(5) 0.000(4) C15 0.122(9) 0.046(4) 0.114(8) 0.011(5) 0.021(7) 0.009(5) N1 0.096(5) 0.070(4) 0.065(4) -0.004(4) 0.025(4) 0.005(4) O4 0.135(6) 0.074(4) 0.065(4) 0.007(3) 0.030(4) 0.011(4) O5 0.149(7) 0.123(6) 0.131(7) 0.022(5) 0.083(6) 0.051(6) O1 0.059(3) 0.057(3) 0.042(2) 0.008(2) -0.010(2) 0.005(2) O2 0.095(4) 0.061(3) 0.043(3) 0.003(2) -0.014(3) -0.010(3) O3 0.037(2) 0.042(2) 0.041(2) 0.0047(17) -0.0014(16) -0.0015(17) O7 0.105(5) 0.064(3) 0.063(3) 0.005(3) 0.002(3) 0.019(3) O8 0.087(4) 0.059(3) 0.051(3) 0.009(2) -0.014(3) 0.008(3) N3 0.080(4) 0.042(3) 0.063(4) 0.000(3) -0.014(3) 0.009(3) O6 0.071(3) 0.046(2) 0.042(2) 0.0073(19) 0.004(2) 0.000(2) O9 0.065(3) 0.055(3) 0.059(3) -0.001(2) 0.015(3) 0.001(3) C11 0.035(3) 0.047(3) 0.036(3) 0.011(2) 0.006(2) 0.005(2) C13 0.054(4) 0.051(4) 0.063(4) 0.009(3) 0.011(3) 0.004(3) C28 0.087(6) 0.078(6) 0.076(6) -0.024(5) -0.020(5) 0.019(5) C29 0.127(10) 0.081(7) 0.146(12) -0.036(8) -0.059(8) 0.046(7) C32 0.140(11) 0.071(7) 0.126(10) 0.006(6) -0.003(8) 0.005(6) C30 0.190(16) 0.121(12) 0.140(13) -0.082(11) -0.070(12) 0.063(11) C31 0.205(17) 0.049(6) 0.201(18) -0.005(9) 0.000(14) 0.012(8) C25 0.089(7) 0.125(9) 0.126(9) 0.027(7) 0.044(7) -0.037(7) C24 0.047(5) 0.113(9) 0.185(13) 0.036(8) -0.028(6) 0.015(5) O10 0.111(5) 0.083(4) 0.097(5) -0.026(4) -0.016(4) 0.013(4) C27 0.050(4) 0.052(4) 0.047(4) 0.014(3) 0.003(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N2 C33 1.3900 . ? N2 C37 1.3900 . ? N2 Cd1 2.334(6) . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C26 O6 1.411(8) 3_656 ? C26 C27 1.525(9) . ? Cd1 O1 2.308(5) . ? Cd1 N3 2.312(6) . ? Cd1 O9 2.322(5) . ? Cd1 O8 2.327(5) . ? Cd1 O7 2.501(6) . ? Cd1 O2 2.555(5) . ? C23 O6 1.381(8) . ? C23 C18 1.383(9) . ? C23 C22 1.388(10) . ? C8 C7 1.385(8) . ? C8 C3 1.395(8) . ? C8 C11 1.529(8) . ? C1 O2 1.238(8) . ? C1 O1 1.270(7) . ? C1 C2 1.489(9) . ? C4 C5 1.373(10) . ? C4 C3 1.402(9) . ? C4 C9 1.508(10) . ? C3 O3 1.393(7) . ? C7 C6 1.404(10) . ? C6 C5 1.399(10) . ? C6 C10 1.505(10) . ? C18 C19 1.395(9) . ? C18 C11 1.527(8) . ? C2 O3 1.427(7) . ? C22 C21 1.407(13) . ? C22 C25 1.517(12) . ? C19 C20 1.391(10) . ? C20 C21 1.355(12) . ? C20 C24 1.508(12) . ? C12 C13 1.381(9) . ? C12 C17 1.408(9) . ? C12 C11 1.539(8) . ? C17 C16 1.403(11) . ? C17 N1 1.451(10) . ? C16 C15 1.337(14) . ? C14 C15 1.350(13) . ? C14 C13 1.392(10) . ? N1 O4 1.219(9) . ? N1 O5 1.267(9) . ? O7 C27 1.212(9) . ? O8 C27 1.251(8) . ? N3 C32 1.270(13) . ? N3 C28 1.319(12) . ? O6 C26 1.411(8) 3_656 ? C28 C29 1.381(14) . ? C29 C30 1.31(2) . ? C32 C31 1.409(17) . ? C30 C31 1.30(2) . ? 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 C33 N2 C37 120.0 . . ? C33 N2 Cd1 116.0(5) . . ? C37 N2 Cd1 123.6(5) . . ? N2 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C37 120.0 . . ? C36 C37 N2 120.0 . . ? O6 C26 C27 111.1(6) 3_656 . ? O1 Cd1 N3 136.38(19) . . ? O1 Cd1 O9 82.17(19) . . ? N3 Cd1 O9 87.7(2) . . ? O1 Cd1 O8 89.98(17) . . ? N3 Cd1 O8 132.9(2) . . ? O9 Cd1 O8 92.2(2) . . ? O1 Cd1 N2 97.0(2) . . ? N3 Cd1 N2 91.7(3) . . ? O9 Cd1 N2 178.0(2) . . ? O8 Cd1 N2 89.6(3) . . ? O1 Cd1 O7 141.39(17) . . ? N3 Cd1 O7 80.0(2) . . ? O9 Cd1 O7 88.2(2) . . ? O8 Cd1 O7 52.96(19) . . ? N2 Cd1 O7 93.5(2) . . ? O1 Cd1 O2 53.46(16) . . ? N3 Cd1 O2 84.6(2) . . ? O9 Cd1 O2 90.7(2) . . ? O8 Cd1 O2 142.51(18) . . ? N2 Cd1 O2 87.3(2) . . ? O7 Cd1 O2 164.53(18) . . ? O6 C23 C18 118.8(6) . . ? O6 C23 C22 119.4(6) . . ? C18 C23 C22 121.7(7) . . ? C7 C8 C3 118.5(6) . . ? C7 C8 C11 122.7(5) . . ? C3 C8 C11 118.8(5) . . ? O2 C1 O1 122.4(6) . . ? O2 C1 C2 121.3(6) . . ? O1 C1 C2 116.2(6) . . ? C5 C4 C3 117.9(6) . . ? C5 C4 C9 121.3(6) . . ? C3 C4 C9 120.8(6) . . ? O3 C3 C8 118.5(5) . . ? O3 C3 C4 120.0(5) . . ? C8 C3 C4 121.5(6) . . ? C8 C7 C6 121.8(6) . . ? C5 C6 C7 117.2(6) . . ? C5 C6 C10 121.7(7) . . ? C7 C6 C10 121.1(7) . . ? C4 C5 C6 122.9(6) . . ? C23 C18 C19 119.1(6) . . ? C23 C18 C11 120.2(5) . . ? C19 C18 C11 120.7(6) . . ? O3 C2 C1 112.5(5) . . ? C23 C22 C21 117.0(7) . . ? C23 C22 C25 121.6(9) . . ? C21 C22 C25 121.4(8) . . ? C20 C19 C18 120.5(7) . . ? C21 C20 C19 119.0(7) . . ? C21 C20 C24 120.9(8) . . ? C19 C20 C24 120.1(8) . . ? C20 C21 C22 122.8(7) . . ? C13 C12 C17 113.9(6) . . ? C13 C12 C11 121.7(6) . . ? C17 C12 C11 124.4(6) . . ? C16 C17 C12 123.0(7) . . ? C16 C17 N1 114.3(7) . . ? C12 C17 N1 122.7(7) . . ? C15 C16 C17 119.8(8) . . ? C15 C14 C13 121.4(9) . . ? C16 C15 C14 119.5(9) . . ? O4 N1 O5 122.5(8) . . ? O4 N1 C17 120.0(7) . . ? O5 N1 C17 117.5(7) . . ? C1 O1 Cd1 97.4(4) . . ? C1 O2 Cd1 86.6(4) . . ? C3 O3 C2 111.0(4) . . ? C27 O7 Cd1 88.7(4) . . ? C27 O8 Cd1 95.9(4) . . ? C32 N3 C28 113.8(9) . . ? C32 N3 Cd1 125.8(8) . . ? C28 N3 Cd1 120.3(6) . . ? C23 O6 C26 116.1(5) . 3_656 ? C18 C11 C8 112.2(5) . . ? C18 C11 C12 110.4(5) . . ? C8 C11 C12 111.8(5) . . ? C12 C13 C14 122.3(7) . . ? N3 C28 C29 123.4(12) . . ? C30 C29 C28 120.4(16) . . ? N3 C32 C31 125.6(15) . . ? C31 C30 C29 118.2(14) . . ? C30 C31 C32 118.5(15) . . ? O7 C27 O8 122.4(6) . . ? O7 C27 C26 118.2(6) . . ? O8 C27 C26 119.4(6) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.973 _refine_diff_density_min -0.918 _refine_diff_density_rms 0.104 # Attachment '- complex 12.cif' data_ommm _database_code_depnum_ccdc_archive 'CCDC 851819' #TrackingRef '- complex 12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H30 K2 O11' _chemical_formula_weight 608.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.4531(15) _cell_length_b 14.4853(13) _cell_length_c 11.8689(10) _cell_angle_alpha 90.00 _cell_angle_beta 78.186(4) _cell_angle_gamma 90.00 _cell_volume 2937.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9979 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 27.67 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.380 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8478 _exptl_absorpt_correction_T_max 0.9111 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37122 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7250 _reflns_number_gt 5475 _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^)+(0.0150P)^2^+25.4323P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7250 _refine_ls_number_parameters 381 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.2258 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C18 C 1.3231(3) 0.0065(3) 0.7166(4) 0.0269(9) Uani 1 1 d . . . C24 C 1.5114(3) 0.0118(4) 0.8301(5) 0.0446(13) Uani 1 1 d . . . H24A H 1.5137 -0.0274 0.8945 0.067 Uiso 1 1 calc R . . H24B H 1.5348 0.0704 0.8404 0.067 Uiso 1 1 calc R . . H24C H 1.5393 -0.0165 0.7607 0.067 Uiso 1 1 calc R . . K1 K 0.92203(7) 0.25205(9) 0.79873(10) 0.0413(3) Uani 1 1 d . . . K2 K 1.06960(12) 0.02597(15) 0.88469(18) 0.0824(6) Uani 1 1 d . . . C19 C 1.2742(3) 0.0592(3) 0.7998(4) 0.0273(9) Uani 1 1 d . . . C20 C 1.2987(3) 0.0918(3) 0.8971(4) 0.0327(10) Uani 1 1 d . . . C11 C 0.7060(3) 0.4690(3) 0.8879(4) 0.0285(9) Uani 1 1 d . . . H11 H 0.7630 0.4625 0.8644 0.034 Uiso 1 1 calc R . . C8 C 0.6734(3) 0.3728(3) 0.9215(4) 0.0276(9) Uani 1 1 d . . . C3 C 0.7045(3) 0.2957(3) 0.8591(4) 0.0281(9) Uani 1 1 d . . . C21 C 1.3759(3) 0.0755(4) 0.9056(4) 0.0350(11) Uani 1 1 d . . . H21 H 1.3935 0.0983 0.9690 0.042 Uiso 1 1 calc R . . C4 C 0.6761(3) 0.2072(4) 0.8861(4) 0.0323(10) Uani 1 1 d . . . C7 C 0.6112(3) 0.3592(4) 1.0147(4) 0.0352(11) Uani 1 1 d . . . H7 H 0.5892 0.4099 1.0574 0.042 Uiso 1 1 calc R . . C22 C 1.4277(3) 0.0259(4) 0.8220(4) 0.0329(10) Uani 1 1 d . . . C5 C 0.6139(3) 0.1974(4) 0.9807(4) 0.0358(11) Uani 1 1 d . . . H5 H 0.5939 0.1387 1.0005 0.043 Uiso 1 1 calc R . . C12 C 0.6908(3) 0.5373(3) 0.9881(4) 0.0321(10) Uani 1 1 d . . . C6 C 0.5814(3) 0.2720(4) 1.0452(4) 0.0371(11) Uani 1 1 d . . . C23 C 1.3993(3) -0.0090(4) 0.7295(4) 0.0321(10) Uani 1 1 d . . . H23 H 1.4325 -0.0440 0.6744 0.038 Uiso 1 1 calc R . . C13 C 0.6280(3) 0.5984(4) 1.0069(5) 0.0418(12) Uani 1 1 d . . . H13 H 0.5932 0.5986 0.9570 0.050 Uiso 1 1 calc R . . C25 C 1.2440(4) 0.1427(5) 0.9922(5) 0.0489(14) Uani 1 1 d . . . H25A H 1.2705 0.1556 1.0537 0.073 Uiso 1 1 calc R . . H25B H 1.1988 0.1053 1.0205 0.073 Uiso 1 1 calc R . . H25C H 1.2279 0.1997 0.9627 0.073 Uiso 1 1 calc R . . C17 C 0.7406(3) 0.5393(4) 1.0656(5) 0.0457(13) Uani 1 1 d . . . H17 H 0.7829 0.4990 1.0557 0.055 Uiso 1 1 calc R . . C9 C 0.7105(3) 0.1236(4) 0.8196(5) 0.0443(13) Uani 1 1 d . . . H9A H 0.6986 0.0697 0.8670 0.066 Uiso 1 1 calc R . . H9B H 0.7663 0.1306 0.7972 0.066 Uiso 1 1 calc R . . H9C H 0.6886 0.1170 0.7522 0.066 Uiso 1 1 calc R . . C15 C 0.6673(4) 0.6601(5) 1.1737(6) 0.0558(17) Uani 1 1 d . . . H15 H 0.6596 0.7016 1.2348 0.067 Uiso 1 1 calc R . . C14 C 0.6167(4) 0.6590(4) 1.0990(6) 0.0522(15) Uani 1 1 d . . . H14 H 0.5743 0.6993 1.1105 0.063 Uiso 1 1 calc R . . C16 C 0.7279(4) 0.6011(5) 1.1584(6) 0.0579(17) Uani 1 1 d . . . H16 H 0.7617 0.6013 1.2097 0.069 Uiso 1 1 calc R . . C10 C 0.5177(4) 0.2582(5) 1.1509(6) 0.0616(19) Uani 1 1 d . . . H10A H 0.4866 0.2055 1.1400 0.092 Uiso 1 1 calc R . . H10B H 0.4850 0.3121 1.1634 0.092 Uiso 1 1 calc R . . H10C H 0.5409 0.2482 1.2166 0.092 Uiso 1 1 calc R . . C2 C 0.7632(3) 0.3098(4) 0.6578(4) 0.0351(11) Uani 1 1 d . . . H2A H 0.7211 0.3518 0.6506 0.042 Uiso 1 1 calc R . . H2B H 0.7497 0.2488 0.6343 0.042 Uiso 1 1 calc R . . C1 C 0.8388(3) 0.3418(3) 0.5811(4) 0.0322(10) Uani 1 1 d . . . C26 C 1.1088(3) 0.1591(4) 0.6890(4) 0.0316(10) Uani 1 1 d . . . C27 C 1.1870(3) 0.1605(3) 0.7289(5) 0.0330(10) Uani 1 1 d . . . H27A H 1.2296 0.1678 0.6629 0.040 Uiso 1 1 calc R . . H27B H 1.1880 0.2124 0.7802 0.040 Uiso 1 1 calc R . . O4 O 1.19719(18) 0.0759(2) 0.7879(3) 0.0303(7) Uani 1 1 d . . . O6 O 1.0719(2) 0.0849(3) 0.6939(3) 0.0400(9) Uani 1 1 d . . . O3 O 0.77251(18) 0.3074(3) 0.7745(3) 0.0335(8) Uani 1 1 d . . . O1 O 0.8955(2) 0.3643(3) 0.6256(3) 0.0362(8) Uani 1 1 d . . . O2 O 0.8385(2) 0.1550(3) 0.9755(3) 0.0474(10) Uani 1 1 d . . . O7 O 0.9380(3) 0.4110(3) 0.9113(4) 0.0625(13) Uani 1 1 d . . . O8 O 0.9230(3) 0.0955(3) 0.6510(4) 0.0559(11) Uani 1 1 d . . . O9 O 1.0293(2) 0.1895(3) 0.9579(3) 0.0453(9) Uani 1 1 d . . . O10 O 1.0665(2) -0.0045(3) 1.0824(3) 0.0394(8) Uani 1 1 d D . . O11 O 0.9097(3) 0.8993(4) 0.7318(5) 0.0604(12) Uani 1 1 d D . . O5 O 1.0883(2) 0.2350(3) 0.6547(4) 0.0472(10) Uani 1 1 d . . . H11M H 0.954(2) 0.903(6) 0.693(6) 0.09(3) Uiso 1 1 d D . . H11N H 0.908(4) 0.845(2) 0.753(6) 0.06(2) Uiso 1 1 d D . . H10M H 1.092(3) -0.051(3) 1.082(5) 0.042(18) Uiso 1 1 d D . . H10N H 1.077(3) 0.037(3) 1.130(4) 0.029(14) Uiso 1 1 d 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 C18 0.026(2) 0.028(2) 0.026(2) 0.0000(18) -0.0037(17) 0.0005(17) C24 0.034(3) 0.055(4) 0.047(3) 0.000(3) -0.016(2) 0.001(2) K1 0.0418(6) 0.0466(7) 0.0354(6) 0.0057(5) -0.0076(5) 0.0002(5) K2 0.0744(12) 0.0909(14) 0.0801(13) 0.0108(11) -0.0115(10) 0.0003(10) C19 0.026(2) 0.027(2) 0.028(2) 0.0009(18) -0.0032(17) 0.0006(17) C20 0.035(2) 0.032(2) 0.029(2) -0.0030(19) -0.0016(19) 0.000(2) C11 0.024(2) 0.033(2) 0.028(2) 0.0046(18) -0.0026(17) -0.0005(18) C8 0.026(2) 0.030(2) 0.026(2) 0.0042(18) -0.0059(17) -0.0005(18) C3 0.023(2) 0.040(3) 0.021(2) 0.0022(18) -0.0034(16) -0.0017(18) C21 0.040(3) 0.038(3) 0.029(2) -0.005(2) -0.011(2) -0.001(2) C4 0.030(2) 0.037(3) 0.031(2) -0.003(2) -0.0071(19) 0.000(2) C7 0.033(2) 0.034(3) 0.034(3) 0.003(2) 0.002(2) 0.003(2) C22 0.031(2) 0.034(3) 0.035(3) 0.002(2) -0.010(2) -0.002(2) C5 0.035(3) 0.033(3) 0.038(3) 0.004(2) -0.004(2) -0.007(2) C12 0.033(2) 0.033(2) 0.029(2) 0.0050(19) -0.0031(19) -0.007(2) C6 0.034(3) 0.040(3) 0.033(3) 0.004(2) 0.004(2) -0.005(2) C23 0.029(2) 0.036(3) 0.030(2) -0.004(2) -0.0031(19) 0.0029(19) C13 0.041(3) 0.045(3) 0.039(3) 0.000(2) -0.007(2) 0.002(2) C25 0.047(3) 0.058(4) 0.038(3) -0.015(3) -0.002(2) 0.004(3) C17 0.039(3) 0.056(4) 0.044(3) 0.002(3) -0.014(2) -0.003(3) C9 0.045(3) 0.038(3) 0.047(3) -0.009(2) -0.002(2) -0.001(2) C15 0.065(4) 0.052(4) 0.045(3) -0.014(3) 0.001(3) -0.014(3) C14 0.052(4) 0.044(3) 0.054(4) -0.008(3) 0.002(3) 0.003(3) C16 0.057(4) 0.073(5) 0.046(4) -0.008(3) -0.017(3) -0.017(4) C10 0.064(4) 0.048(4) 0.057(4) 0.004(3) 0.024(3) -0.008(3) C2 0.031(2) 0.048(3) 0.026(2) -0.003(2) -0.0042(19) -0.007(2) C1 0.032(2) 0.033(2) 0.029(2) -0.0024(19) -0.0016(19) -0.0012(19) C26 0.031(2) 0.036(3) 0.026(2) 0.0005(19) -0.0028(18) 0.003(2) C27 0.030(2) 0.025(2) 0.043(3) 0.004(2) -0.006(2) 0.0010(18) O4 0.0233(15) 0.0283(17) 0.0377(18) 0.0040(14) -0.0024(13) 0.0013(13) O6 0.039(2) 0.044(2) 0.040(2) 0.0013(17) -0.0161(16) -0.0079(17) O3 0.0233(15) 0.053(2) 0.0232(16) -0.0010(15) -0.0010(12) -0.0032(15) O1 0.0306(17) 0.046(2) 0.0326(18) 0.0063(16) -0.0070(14) -0.0047(15) O2 0.047(2) 0.070(3) 0.0244(17) 0.0006(18) -0.0049(16) 0.013(2) O7 0.081(3) 0.052(3) 0.053(3) -0.003(2) -0.010(2) 0.006(2) O8 0.054(3) 0.064(3) 0.053(3) -0.002(2) -0.016(2) 0.005(2) O9 0.045(2) 0.051(2) 0.037(2) -0.0040(18) -0.0019(17) -0.0027(18) O10 0.039(2) 0.043(2) 0.036(2) -0.0044(17) -0.0074(16) 0.0012(18) O11 0.062(3) 0.049(3) 0.072(3) -0.007(3) -0.016(3) 0.001(2) O5 0.048(2) 0.045(2) 0.051(2) 0.0135(19) -0.0151(19) 0.0054(18) _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 C18 C23 1.387(6) . ? C18 C19 1.394(6) . ? C18 C11 1.533(6) 2_746 ? C24 C22 1.498(7) . ? K1 O2 2.693(4) . ? K1 O7 2.705(5) . ? K1 O1 2.732(4) . ? K1 O3 2.801(4) . ? K1 O8 2.864(5) . ? K1 O9 3.057(4) . ? K1 O5 3.061(4) . ? K1 K2 4.514(3) 2_756 ? K2 O10 2.348(4) 3_757 ? K2 O10 2.377(4) . ? K2 O4 2.399(4) . ? K2 O6 2.413(4) . ? K2 O1 2.417(4) 2_746 ? K2 O9 2.571(5) . ? K2 C1 3.179(5) 2_746 ? K2 K2 3.352(4) 3_757 ? K2 K1 4.514(3) 2_746 ? C19 C20 1.393(7) . ? C19 O4 1.401(5) . ? C20 C21 1.391(7) . ? C20 C25 1.513(7) . ? C11 C12 1.527(7) . ? C11 C8 1.528(6) . ? C11 C18 1.533(6) 2_756 ? C8 C3 1.388(7) . ? C8 C7 1.396(6) . ? C3 C4 1.387(7) . ? C3 O3 1.399(5) . ? C21 C22 1.397(7) . ? C4 C5 1.400(7) . ? C4 C9 1.502(7) . ? C7 C6 1.385(7) . ? C22 C23 1.389(7) . ? C5 C6 1.379(7) . ? C12 C17 1.389(7) . ? C12 C13 1.391(7) . ? C6 C10 1.510(7) . ? C13 C14 1.384(8) . ? C17 C16 1.402(9) . ? C15 C16 1.343(10) . ? C15 C14 1.374(9) . ? C2 O3 1.429(6) . ? C2 C1 1.513(7) . ? C1 O2 1.256(6) 4_565 ? C1 O1 1.257(6) . ? C1 K2 3.179(5) 2_756 ? C26 O6 1.247(6) . ? C26 O5 1.251(6) . ? C26 C27 1.533(7) . ? C27 O4 1.440(6) . ? O1 K2 2.417(4) 2_756 ? O2 C1 1.256(6) 4_566 ? O10 K2 2.348(4) 3_757 ? 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 C23 C18 C19 118.2(4) . . ? C23 C18 C11 121.1(4) . 2_746 ? C19 C18 C11 120.7(4) . 2_746 ? O2 K1 O7 98.85(14) . . ? O2 K1 O1 138.47(12) . . ? O7 K1 O1 85.13(14) . . ? O2 K1 O3 82.09(11) . . ? O7 K1 O3 89.95(14) . . ? O1 K1 O3 56.48(10) . . ? O2 K1 O8 89.87(14) . . ? O7 K1 O8 171.10(15) . . ? O1 K1 O8 89.51(13) . . ? O3 K1 O8 93.02(12) . . ? O2 K1 O9 70.47(11) . . ? O7 K1 O9 78.99(13) . . ? O1 K1 O9 149.37(12) . . ? O3 K1 O9 148.17(11) . . ? O8 K1 O9 102.49(12) . . ? O2 K1 O5 133.86(12) . . ? O7 K1 O5 99.37(14) . . ? O1 K1 O5 85.13(11) . . ? O3 K1 O5 139.68(11) . . ? O8 K1 O5 73.04(13) . . ? O9 K1 O5 72.01(11) . . ? O2 K1 K2 142.53(10) . 2_756 ? O7 K1 K2 59.56(11) . 2_756 ? O1 K1 K2 26.89(8) . 2_756 ? O3 K1 K2 68.75(8) . 2_756 ? O8 K1 K2 113.90(10) . 2_756 ? O9 K1 K2 126.53(9) . 2_756 ? O5 K1 K2 82.43(8) . 2_756 ? O10 K2 O10 89.61(15) 3_757 . ? O10 K2 O4 158.13(16) 3_757 . ? O10 K2 O4 111.11(15) . . ? O10 K2 O6 91.45(15) 3_757 . ? O10 K2 O6 169.99(17) . . ? O4 K2 O6 66.92(13) . . ? O10 K2 O1 96.66(15) 3_757 2_746 ? O10 K2 O1 79.89(15) . 2_746 ? O4 K2 O1 93.93(13) . 2_746 ? O6 K2 O1 109.86(15) . 2_746 ? O10 K2 O9 82.40(15) 3_757 . ? O10 K2 O9 83.58(15) . . ? O4 K2 O9 92.71(14) . . ? O6 K2 O9 86.69(15) . . ? O1 K2 O9 163.46(15) 2_746 . ? O10 K2 C1 112.71(16) 3_757 2_746 ? O10 K2 C1 68.18(14) . 2_746 ? O4 K2 C1 82.67(13) . 2_746 ? O6 K2 C1 120.30(15) . 2_746 ? O1 K2 C1 20.78(12) 2_746 2_746 ? O9 K2 C1 147.14(15) . 2_746 ? O10 K2 K2 45.16(11) 3_757 3_757 ? O10 K2 K2 44.45(11) . 3_757 ? O4 K2 K2 154.86(15) . 3_757 ? O6 K2 K2 135.73(14) . 3_757 ? O1 K2 K2 87.52(12) 2_746 3_757 ? O9 K2 K2 80.11(12) . 3_757 ? C1 K2 K2 90.39(12) 2_746 3_757 ? O10 K2 K1 84.02(12) 3_757 2_746 ? O10 K2 K1 107.73(12) . 2_746 ? O4 K2 K1 95.67(10) . 2_746 ? O6 K2 K1 82.28(11) . 2_746 ? O1 K2 K1 30.76(9) 2_746 2_746 ? O9 K2 K1 162.26(12) . 2_746 ? C1 K2 K1 49.93(10) 2_746 2_746 ? K2 K2 K1 98.22(9) 3_757 2_746 ? C20 C19 C18 121.7(4) . . ? C20 C19 O4 119.2(4) . . ? C18 C19 O4 119.0(4) . . ? C21 C20 C19 117.9(4) . . ? C21 C20 C25 120.1(5) . . ? C19 C20 C25 122.0(5) . . ? C12 C11 C8 113.1(4) . . ? C12 C11 C18 111.5(4) . 2_756 ? C8 C11 C18 111.5(4) . 2_756 ? C3 C8 C7 117.7(4) . . ? C3 C8 C11 120.7(4) . . ? C7 C8 C11 121.5(4) . . ? C4 C3 C8 122.5(4) . . ? C4 C3 O3 119.2(4) . . ? C8 C3 O3 117.8(4) . . ? C20 C21 C22 122.1(5) . . ? C3 C4 C5 117.5(5) . . ? C3 C4 C9 122.6(5) . . ? C5 C4 C9 120.0(5) . . ? C6 C7 C8 121.7(5) . . ? C23 C22 C21 117.7(5) . . ? C23 C22 C24 120.8(5) . . ? C21 C22 C24 121.5(5) . . ? C6 C5 C4 121.9(5) . . ? C17 C12 C13 117.4(5) . . ? C17 C12 C11 119.7(5) . . ? C13 C12 C11 122.9(5) . . ? C5 C6 C7 118.7(5) . . ? C5 C6 C10 120.5(5) . . ? C7 C6 C10 120.8(5) . . ? C18 C23 C22 122.2(5) . . ? C14 C13 C12 120.7(6) . . ? C12 C17 C16 121.0(6) . . ? C16 C15 C14 119.9(6) . . ? C15 C14 C13 120.7(6) . . ? C15 C16 C17 120.4(6) . . ? O3 C2 C1 109.4(4) . . ? O2 C1 O1 125.0(5) 4_565 . ? O2 C1 C2 115.5(4) 4_565 . ? O1 C1 C2 119.4(4) . . ? O2 C1 K2 101.6(3) 4_565 2_756 ? O1 C1 K2 43.0(3) . 2_756 ? C2 C1 K2 125.4(3) . 2_756 ? O6 C26 O5 126.3(5) . . ? O6 C26 C27 118.7(4) . . ? O5 C26 C27 114.9(4) . . ? O4 C27 C26 110.2(4) . . ? C19 O4 C27 114.3(3) . . ? C19 O4 K2 135.7(3) . . ? C27 O4 K2 107.1(3) . . ? C26 O6 K2 104.9(3) . . ? C3 O3 C2 116.8(3) . . ? C3 O3 K1 124.3(3) . . ? C2 O3 K1 113.6(3) . . ? C1 O1 K2 116.2(3) . 2_756 ? C1 O1 K1 115.5(3) . . ? K2 O1 K1 122.36(15) 2_756 . ? C1 O2 K1 130.3(4) 4_566 . ? K2 O9 K1 102.94(14) . . ? K2 O10 K2 90.39(15) 3_757 . ? C26 O5 K1 101.0(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.659 _refine_diff_density_min -2.022 _refine_diff_density_rms 0.130 # Attachment '- complex 13.cif' data_vskr _database_code_depnum_ccdc_archive 'CCDC 851820' #TrackingRef '- complex 13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 K2 N O11' _chemical_formula_weight 619.70 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.8855(4) _cell_length_b 12.4867(3) _cell_length_c 33.5892(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5823.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9164 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 0.385 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77996 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.34 _reflns_number_total 7251 _reflns_number_gt 5245 _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^)+(0.0879P)^2^+4.9827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7251 _refine_ls_number_parameters 382 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1967 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 K1 K 0.17566(7) 0.53868(6) 0.21126(2) 0.0637(2) Uani 1 1 d . . . K2 K -0.00123(5) 0.77110(6) 0.23694(2) 0.0584(2) Uani 1 1 d . . . C3 C -0.05612(17) 0.7358(2) 0.11340(7) 0.0350(5) Uani 1 1 d . . . C5 C -0.0713(2) 0.8668(2) 0.06200(9) 0.0448(6) Uani 1 1 d . . . H5 H -0.0911 0.9343 0.0536 0.054 Uiso 1 1 calc R . . C7 C 0.00183(18) 0.6991(2) 0.04774(8) 0.0385(6) Uani 1 1 d . . . H7 H 0.0329 0.6538 0.0299 0.046 Uiso 1 1 calc R . . C4 C -0.08433(19) 0.8385(2) 0.10147(8) 0.0405(6) Uani 1 1 d . . . C8 C -0.01149(17) 0.6654(2) 0.08701(7) 0.0333(5) Uani 1 1 d . . . C6 C -0.02978(19) 0.7979(2) 0.03453(8) 0.0412(6) Uani 1 1 d . . . C10 C -0.0192(2) 0.8304(3) -0.00856(10) 0.0582(8) Uani 1 1 d . . . H10A H 0.0138 0.7750 -0.0229 0.087 Uiso 1 1 calc R . . H10B H 0.0171 0.8957 -0.0102 0.087 Uiso 1 1 calc R . . H10C H -0.0818 0.8413 -0.0200 0.087 Uiso 1 1 calc R . . C9 C -0.1263(3) 0.9162(3) 0.13112(11) 0.0577(8) Uani 1 1 d . . . H9A H -0.1315 0.9857 0.1191 0.087 Uiso 1 1 calc R . . H9B H -0.0851 0.9204 0.1540 0.087 Uiso 1 1 calc R . . H9C H -0.1890 0.8921 0.1391 0.087 Uiso 1 1 calc R . . C11 C 0.02458(18) 0.5570(2) 0.10170(8) 0.0347(5) Uani 1 1 d . . . H11 H 0.0310 0.5631 0.1307 0.042 Uiso 1 1 calc R . . C23 C 0.20476(18) 0.57910(19) 0.10358(7) 0.0338(5) Uani 1 1 d . . . C22 C 0.29840(19) 0.5555(2) 0.09132(8) 0.0387(6) Uani 1 1 d . . . C21 C 0.31004(19) 0.4832(2) 0.06035(9) 0.0433(6) Uani 1 1 d . . . H21 H 0.3720 0.4672 0.0517 0.052 Uiso 1 1 calc R . . C18 C 0.12491(18) 0.53152(19) 0.08569(7) 0.0334(5) Uani 1 1 d . . . C19 C 0.14037(19) 0.4597(2) 0.05456(8) 0.0422(6) Uani 1 1 d . . . H19 H 0.0878 0.4282 0.0420 0.051 Uiso 1 1 calc R . . C20 C 0.2328(2) 0.4343(2) 0.04194(9) 0.0453(6) Uani 1 1 d . . . C25 C 0.3853(2) 0.6010(3) 0.11244(10) 0.0546(8) Uani 1 1 d . . . H25A H 0.4397 0.5550 0.1082 0.082 Uiso 1 1 calc R . . H25B H 0.3722 0.6060 0.1404 0.082 Uiso 1 1 calc R . . H25C H 0.3991 0.6710 0.1021 0.082 Uiso 1 1 calc R . . C24 C 0.2490(3) 0.3528(3) 0.00942(12) 0.0777(13) Uani 1 1 d . . . H24A H 0.1888 0.3365 -0.0032 0.116 Uiso 1 1 calc R . . H24B H 0.2756 0.2886 0.0207 0.116 Uiso 1 1 calc R . . H24C H 0.2930 0.3814 -0.0099 0.116 Uiso 1 1 calc R . . C13 C -0.1047(2) 0.4634(3) 0.06041(9) 0.0508(7) Uani 1 1 d . . . H13 H -0.1016 0.5198 0.0424 0.061 Uiso 1 1 calc R . . C12 C -0.04618(19) 0.4655(2) 0.09409(8) 0.0407(6) Uani 1 1 d . . . C17 C -0.0567(2) 0.3783(2) 0.11990(10) 0.0490(7) Uani 1 1 d . . . C16 C -0.1192(3) 0.2939(3) 0.11321(12) 0.0622(9) Uani 1 1 d . . . H16 H -0.1238 0.2375 0.1312 0.075 Uiso 1 1 calc R . . C15 C -0.1742(3) 0.2954(3) 0.07938(12) 0.0671(10) Uani 1 1 d . . . H15 H -0.2164 0.2392 0.0742 0.081 Uiso 1 1 calc R . . C14 C -0.1679(2) 0.3788(3) 0.05301(11) 0.0621(9) Uani 1 1 d . . . H14 H -0.2058 0.3790 0.0302 0.074 Uiso 1 1 calc R . . C27 C 0.1938(2) 0.8089(2) 0.17275(8) 0.0401(6) Uani 1 1 d . . . C26 C 0.1989(2) 0.7546(2) 0.13255(8) 0.0397(6) Uani 1 1 d . . . H26A H 0.1476 0.7812 0.1156 0.048 Uiso 1 1 calc R . . H26B H 0.2599 0.7711 0.1199 0.048 Uiso 1 1 calc R . . C1 C -0.1460(3) 0.5831(3) 0.19841(10) 0.0560(8) Uani 1 1 d . . . C2 C -0.1554(2) 0.6518(2) 0.16147(8) 0.0445(6) Uani 1 1 d . . . H2A H -0.1732 0.6072 0.1390 0.053 Uiso 1 1 calc R . . H2B H -0.2060 0.7043 0.1654 0.053 Uiso 1 1 calc R . . O3 O -0.06679(13) 0.70584(15) 0.15283(5) 0.0398(4) Uani 1 1 d . . . O1 O -0.0645(2) 0.5752(3) 0.21357(9) 0.0878(10) Uani 1 1 d . . . O4 O 0.0815(3) 0.3948(3) 0.15733(10) 0.0958(10) Uani 1 1 d . . . O6 O 0.18957(14) 0.64107(14) 0.13720(5) 0.0396(4) Uani 1 1 d . . . O7 O 0.18391(17) 0.75237(16) 0.20318(6) 0.0507(5) Uani 1 1 d . . . O9 O 0.19508(17) 0.3434(2) 0.26220(7) 0.0609(6) Uani 1 1 d . . . O2 O 0.2783(2) 0.5408(2) 0.29000(9) 0.0810(8) Uani 1 1 d . . . O11 O 0.0441(2) 0.9764(2) 0.21554(9) 0.0705(7) Uani 1 1 d D . . O8 O 0.30217(19) 0.40861(16) 0.17208(7) 0.0590(6) Uani 1 1 d . . . N1 N -0.0025(3) 0.3716(2) 0.15732(10) 0.0642(8) Uani 1 1 d . . . O5 O -0.0462(4) 0.3461(4) 0.18691(11) 0.1465(19) Uani 1 1 d . . . O10 O 0.0981(2) 0.6258(3) 0.28783(12) 0.1027(11) Uani 1 1 d . . . H11M H 0.060(4) 1.003(4) 0.2388(9) 0.115(19) Uiso 1 1 d D . . H11N H 0.094(3) 0.968(4) 0.2004(14) 0.111(19) Uiso 1 1 d 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 K1 0.1071(7) 0.0372(4) 0.0469(4) 0.0012(3) 0.0036(4) 0.0072(4) K2 0.0541(4) 0.0566(4) 0.0645(5) -0.0022(3) 0.0025(3) 0.0034(3) C3 0.0313(12) 0.0404(13) 0.0335(12) -0.0032(10) 0.0014(9) -0.0028(10) C5 0.0401(14) 0.0396(14) 0.0549(16) 0.0079(12) -0.0010(12) 0.0035(11) C7 0.0360(13) 0.0450(15) 0.0346(13) -0.0014(10) 0.0027(10) 0.0014(11) C4 0.0351(13) 0.0390(14) 0.0475(15) -0.0049(11) 0.0031(11) 0.0005(11) C8 0.0304(12) 0.0362(13) 0.0334(12) -0.0025(9) -0.0011(9) -0.0009(9) C6 0.0338(12) 0.0483(15) 0.0416(14) 0.0057(11) -0.0017(11) -0.0025(11) C10 0.0562(19) 0.070(2) 0.0484(18) 0.0187(15) 0.0008(14) 0.0040(16) C9 0.066(2) 0.0431(16) 0.064(2) -0.0131(14) 0.0084(16) 0.0091(15) C11 0.0360(12) 0.0355(13) 0.0327(12) -0.0017(9) 0.0010(10) 0.0011(10) C23 0.0429(13) 0.0283(11) 0.0302(11) 0.0010(9) -0.0015(10) -0.0001(10) C22 0.0368(13) 0.0392(14) 0.0399(13) 0.0024(10) -0.0022(10) -0.0040(10) C21 0.0347(13) 0.0481(16) 0.0472(15) -0.0050(12) 0.0054(11) 0.0047(11) C18 0.0345(12) 0.0331(12) 0.0327(12) -0.0019(9) -0.0002(9) 0.0025(10) C19 0.0359(13) 0.0467(15) 0.0439(15) -0.0151(12) -0.0039(11) 0.0009(11) C20 0.0421(15) 0.0480(16) 0.0459(15) -0.0139(12) 0.0034(12) 0.0055(12) C25 0.0419(16) 0.064(2) 0.0577(18) -0.0075(15) -0.0062(13) -0.0081(14) C24 0.0523(19) 0.094(3) 0.087(3) -0.055(2) 0.0030(19) 0.0085(19) C13 0.0418(15) 0.0580(18) 0.0528(17) -0.0077(14) -0.0002(13) -0.0052(13) C12 0.0351(13) 0.0410(14) 0.0459(15) -0.0068(11) 0.0075(11) -0.0001(11) C17 0.0475(16) 0.0438(16) 0.0555(17) -0.0040(13) 0.0064(13) 0.0004(12) C16 0.062(2) 0.0491(18) 0.076(2) -0.0071(16) 0.0173(18) -0.0107(15) C15 0.060(2) 0.062(2) 0.079(3) -0.0199(19) 0.0149(18) -0.0177(17) C14 0.0460(17) 0.077(2) 0.063(2) -0.0169(18) -0.0028(15) -0.0025(16) C27 0.0444(14) 0.0352(13) 0.0407(14) -0.0045(11) -0.0002(11) -0.0003(11) C26 0.0494(15) 0.0312(13) 0.0384(13) -0.0003(10) -0.0015(11) -0.0064(11) C1 0.067(2) 0.0459(17) 0.0555(18) 0.0068(14) 0.0014(16) -0.0094(15) C2 0.0392(14) 0.0522(17) 0.0421(15) -0.0003(12) 0.0042(11) -0.0037(12) O3 0.0365(9) 0.0491(11) 0.0338(9) -0.0031(8) 0.0038(7) -0.0039(8) O1 0.092(2) 0.085(2) 0.086(2) 0.0410(16) -0.0300(16) -0.0236(17) O4 0.088(2) 0.111(3) 0.088(2) 0.0196(18) -0.0295(18) 0.0051(19) O6 0.0555(11) 0.0309(9) 0.0322(9) -0.0033(7) 0.0027(8) -0.0061(8) O7 0.0768(15) 0.0374(11) 0.0378(10) -0.0036(8) 0.0031(10) -0.0039(10) O9 0.0617(14) 0.0589(14) 0.0620(14) -0.0054(11) 0.0136(11) -0.0055(11) O2 0.0816(18) 0.0759(18) 0.0854(19) -0.0272(15) -0.0171(15) -0.0184(15) O11 0.0744(18) 0.0669(17) 0.0703(18) -0.0210(13) -0.0019(15) 0.0045(13) O8 0.0902(17) 0.0318(11) 0.0549(13) -0.0055(9) -0.0075(11) 0.0041(10) N1 0.084(2) 0.0493(16) 0.0597(18) 0.0140(13) -0.0060(15) -0.0082(15) O5 0.211(5) 0.165(4) 0.064(2) 0.034(2) 0.000(3) -0.073(4) O10 0.092(2) 0.083(2) 0.133(3) 0.035(2) -0.019(2) -0.0131(18) _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 K1 O7 2.684(2) . ? K1 O8 2.730(2) . ? K1 O6 2.8037(19) . ? K1 O4 2.867(4) . ? K1 O9 2.991(3) . ? K1 O10 2.993(4) . ? K1 O2 3.005(3) . ? K1 O1 3.367(3) . ? K1 K2 3.8986(11) . ? K1 K2 4.4786(11) 3_545 ? K2 O1 2.716(3) . ? K2 O11 2.736(3) . ? K2 O5 2.802(4) 3 ? K2 O7 2.819(2) . ? K2 O9 2.839(2) 3 ? K2 O10 2.849(3) . ? K2 O3 3.0779(19) . ? K2 K1 4.4786(11) 3 ? C3 O3 1.384(3) . ? C3 C8 1.393(3) . ? C3 C4 1.400(4) . ? C5 C4 1.384(4) . ? C5 C6 1.387(4) . ? C7 C6 1.382(4) . ? C7 C8 1.397(4) . ? C4 C9 1.508(4) . ? C8 C11 1.525(4) . ? C6 C10 1.510(4) . ? C11 C18 1.527(3) . ? C11 C12 1.529(4) . ? C23 O6 1.385(3) . ? C23 C18 1.394(3) . ? C23 C22 1.395(4) . ? C22 C21 1.386(4) . ? C22 C25 1.511(4) . ? C21 C20 1.381(4) . ? C18 C19 1.394(3) . ? C19 C20 1.388(4) . ? C20 C24 1.510(4) . ? C13 C12 1.393(4) . ? C13 C14 1.395(5) . ? C12 C17 1.399(4) . ? C17 C16 1.384(5) . ? C17 N1 1.468(5) . ? C16 C15 1.369(6) . ? C15 C14 1.369(6) . ? C27 O8 1.247(3) 8_665 ? C27 O7 1.250(3) . ? C27 C26 1.513(4) . ? C26 O6 1.432(3) . ? C1 O2 1.239(4) 6_556 ? C1 O1 1.244(4) . ? C1 C2 1.514(4) . ? C2 O3 1.432(3) . ? O4 N1 1.202(4) . ? O9 K2 2.839(2) 3_545 ? O2 C1 1.239(4) 6_656 ? O8 C27 1.247(3) 8_655 ? N1 O5 1.207(5) . ? O5 K2 2.802(4) 3_545 ? 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 O7 K1 O8 121.00(8) . . ? O7 K1 O6 56.92(6) . . ? O8 K1 O6 78.42(6) . . ? O7 K1 O4 125.35(8) . . ? O8 K1 O4 67.42(9) . . ? O6 K1 O4 75.91(8) . . ? O7 K1 O9 149.80(7) . . ? O8 K1 O9 74.50(7) . . ? O6 K1 O9 150.83(6) . . ? O4 K1 O9 83.78(8) . . ? O7 K1 O10 74.99(8) . . ? O8 K1 O10 149.53(8) . . ? O6 K1 O10 128.43(8) . . ? O4 K1 O10 127.34(11) . . ? O9 K1 O10 80.62(8) . . ? O7 K1 O2 93.44(8) . . ? O8 K1 O2 97.13(8) . . ? O6 K1 O2 138.10(8) . . ? O4 K1 O2 141.08(9) . . ? O9 K1 O2 57.37(7) . . ? O10 K1 O2 53.93(9) . . ? O7 K1 O1 84.85(8) . . ? O8 K1 O1 136.79(8) . . ? O6 K1 O1 91.55(6) . . ? O4 K1 O1 69.37(10) . . ? O9 K1 O1 100.74(7) . . ? O10 K1 O1 64.81(9) . . ? O2 K1 O1 116.65(8) . . ? O7 K1 K2 46.32(5) . . ? O8 K1 K2 162.70(5) . . ? O6 K1 K2 84.27(4) . . ? O4 K1 K2 108.61(8) . . ? O9 K1 K2 122.48(5) . . ? O10 K1 K2 46.57(6) . . ? O2 K1 K2 95.60(6) . . ? O1 K1 K2 43.12(6) . . ? O7 K1 K2 143.50(6) . 3_545 ? O8 K1 K2 95.25(5) . 3_545 ? O6 K1 K2 136.24(5) . 3_545 ? O4 K1 K2 62.05(7) . 3_545 ? O9 K1 K2 38.58(5) . 3_545 ? O10 K1 K2 75.08(7) . 3_545 ? O2 K1 K2 85.48(6) . 3_545 ? O1 K1 K2 63.66(5) . 3_545 ? K2 K1 K2 97.394(19) . 3_545 ? O1 K2 O11 147.44(9) . . ? O1 K2 O5 129.86(13) . 3 ? O11 K2 O5 82.68(13) . 3 ? O1 K2 O7 95.98(9) . . ? O11 K2 O7 76.24(8) . . ? O5 K2 O7 100.41(12) 3 . ? O1 K2 O9 89.00(9) . 3 ? O11 K2 O9 85.58(8) . 3 ? O5 K2 O9 96.14(11) 3 3 ? O7 K2 O9 153.50(7) . 3 ? O1 K2 O10 75.89(9) . . ? O11 K2 O10 130.01(10) . . ? O5 K2 O10 63.35(12) 3 . ? O7 K2 O10 75.35(9) . . ? O9 K2 O10 130.94(9) 3 . ? O1 K2 O3 53.16(7) . . ? O11 K2 O3 94.31(7) . . ? O5 K2 O3 174.70(10) 3 . ? O7 K2 O3 83.03(6) . . ? O9 K2 O3 79.24(6) 3 . ? O10 K2 O3 121.69(9) . . ? O1 K2 K1 57.95(7) . . ? O11 K2 K1 119.62(7) . . ? O5 K2 K1 107.62(10) 3 . ? O7 K2 K1 43.52(4) . . ? O9 K2 K1 146.75(6) 3 . ? O10 K2 K1 49.74(9) . . ? O3 K2 K1 77.65(4) . . ? O1 K2 K1 127.54(8) . 3 ? O11 K2 K1 61.81(6) . 3 ? O5 K2 K1 61.51(9) 3 3 ? O7 K2 K1 135.34(5) . 3 ? O9 K2 K1 41.07(5) 3 3 ? O10 K2 K1 120.25(9) . 3 ? O3 K2 K1 113.22(4) . 3 ? K1 K2 K1 169.12(2) . 3 ? O3 C3 C8 119.1(2) . . ? O3 C3 C4 119.4(2) . . ? C8 C3 C4 121.3(2) . . ? C4 C5 C6 122.2(3) . . ? C6 C7 C8 122.0(3) . . ? C5 C4 C3 118.1(2) . . ? C5 C4 C9 121.3(3) . . ? C3 C4 C9 120.6(3) . . ? C3 C8 C7 118.0(2) . . ? C3 C8 C11 120.0(2) . . ? C7 C8 C11 122.0(2) . . ? C7 C6 C5 118.1(3) . . ? C7 C6 C10 121.1(3) . . ? C5 C6 C10 120.8(3) . . ? C8 C11 C18 111.8(2) . . ? C8 C11 C12 113.5(2) . . ? C18 C11 C12 111.8(2) . . ? O6 C23 C18 117.9(2) . . ? O6 C23 C22 120.0(2) . . ? C18 C23 C22 121.6(2) . . ? C21 C22 C23 117.9(2) . . ? C21 C22 C25 120.3(3) . . ? C23 C22 C25 121.7(3) . . ? C20 C21 C22 122.2(2) . . ? C23 C18 C19 118.4(2) . . ? C23 C18 C11 119.0(2) . . ? C19 C18 C11 122.6(2) . . ? C20 C19 C18 121.2(2) . . ? C21 C20 C19 118.7(2) . . ? C21 C20 C24 120.4(3) . . ? C19 C20 C24 120.8(3) . . ? C12 C13 C14 121.7(3) . . ? C13 C12 C17 115.3(3) . . ? C13 C12 C11 121.7(3) . . ? C17 C12 C11 123.0(3) . . ? C16 C17 C12 123.9(3) . . ? C16 C17 N1 114.7(3) . . ? C12 C17 N1 121.4(3) . . ? C15 C16 C17 118.3(4) . . ? C16 C15 C14 120.8(3) . . ? C15 C14 C13 120.0(3) . . ? O8 C27 O7 125.7(3) 8_665 . ? O8 C27 C26 115.4(2) 8_665 . ? O7 C27 C26 118.9(2) . . ? O6 C26 C27 110.0(2) . . ? O2 C1 O1 127.5(3) 6_556 . ? O2 C1 C2 115.2(3) 6_556 . ? O1 C1 C2 117.3(3) . . ? O3 C2 C1 111.0(2) . . ? C3 O3 C2 114.4(2) . . ? C3 O3 K2 140.82(15) . . ? C2 O3 K2 101.11(14) . . ? C1 O1 K2 109.9(3) . . ? C1 O1 K1 154.4(3) . . ? K2 O1 K1 78.92(7) . . ? N1 O4 K1 126.4(3) . . ? C23 O6 C26 116.77(19) . . ? C23 O6 K1 118.63(14) . . ? C26 O6 K1 123.67(14) . . ? C27 O7 K1 130.44(17) . . ? C27 O7 K2 112.44(19) . . ? K1 O7 K2 90.16(7) . . ? K2 O9 K1 100.35(8) 3_545 . ? C1 O2 K1 133.1(3) 6_656 . ? C27 O8 K1 127.9(2) 8_655 . ? O4 N1 O5 123.4(4) . . ? O4 N1 C17 119.0(3) . . ? O5 N1 C17 117.5(4) . . ? N1 O5 K2 136.2(4) . 3_545 ? K2 O10 K1 83.69(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.522 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.065 # Attachment '- complex 10.cif' data_hg4pic_0m _database_code_depnum_ccdc_archive 'CCDC 859335' #TrackingRef '- complex 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H78 Hg2 N6 O16' _chemical_formula_weight 1756.64 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0283(5) _cell_length_b 13.0271(6) _cell_length_c 14.9975(6) _cell_angle_alpha 71.685(2) _cell_angle_beta 88.736(3) _cell_angle_gamma 85.118(3) _cell_volume 2038.05(15) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 3.826 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2334 _exptl_absorpt_correction_T_max 0.5613 _exptl_absorpt_process_details 'North et al.,1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23302 _diffrn_reflns_av_R_equivalents 0.0998 _diffrn_reflns_av_sigmaI/netI 0.1305 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7000 _reflns_number_gt 3425 _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^)+(0.0330P)^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 7000 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1136 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.43209(3) 1.01040(2) 0.383010(19) 0.07781(17) Uani 1 1 d . . . C18 C 0.1900(6) 0.5609(6) 0.8131(4) 0.0522(19) Uani 1 1 d . . . C19 C 0.0984(6) 0.4905(6) 0.8301(4) 0.065(2) Uani 1 1 d . . . H19 H 0.1165 0.4218 0.8244 0.078 Uiso 1 1 calc R . . C23 C 0.1604(7) 0.6650(7) 0.8191(4) 0.058(2) Uani 1 1 d . . . C22 C 0.0453(8) 0.6955(7) 0.8423(5) 0.075(2) Uani 1 1 d . . . C20 C -0.0180(7) 0.5177(8) 0.8550(5) 0.078(3) Uani 1 1 d . . . C21 C -0.0414(7) 0.6191(9) 0.8612(5) 0.086(3) Uani 1 1 d . . . H21 H -0.1190 0.6388 0.8789 0.103 Uiso 1 1 calc R . . C24 C -0.1149(6) 0.4367(7) 0.8750(5) 0.119(3) Uani 1 1 d . . . H24A H -0.0960 0.3856 0.8415 0.179 Uiso 1 1 calc R . . H24B H -0.1929 0.4746 0.8550 0.179 Uiso 1 1 calc R . . H24C H -0.1167 0.3988 0.9412 0.179 Uiso 1 1 calc R . . C25 C 0.0131(6) 0.8065(8) 0.8517(6) 0.117(3) Uani 1 1 d . . . H25A H 0.0839 0.8325 0.8707 0.176 Uiso 1 1 calc R . . H25B H -0.0494 0.8021 0.8980 0.176 Uiso 1 1 calc R . . H25C H -0.0157 0.8556 0.7924 0.176 Uiso 1 1 calc R . . C26 C 0.2481(6) 0.8174(5) 0.7168(4) 0.068(2) Uani 1 1 d . . . H26A H 0.1871 0.8755 0.7170 0.081 Uiso 1 1 calc R . . H26B H 0.2265 0.7872 0.6685 0.081 Uiso 1 1 calc R . . C32 C 0.2763(7) 1.2261(7) 0.3541(5) 0.074(2) Uani 1 1 d . . . H32 H 0.3414 1.2514 0.3152 0.088 Uiso 1 1 calc R . . C30 C 0.0880(7) 1.2649(8) 0.4186(6) 0.087(3) Uani 1 1 d . . . C28 C 0.1844(8) 1.0863(7) 0.4508(6) 0.096(3) Uani 1 1 d . . . H28 H 0.1827 1.0121 0.4806 0.115 Uiso 1 1 calc R . . C31 C 0.1857(8) 1.2990(7) 0.3631(5) 0.084(2) Uani 1 1 d . . . H31 H 0.1900 1.3724 0.3314 0.101 Uiso 1 1 calc R . . C29 C 0.0908(8) 1.1545(9) 0.4639(6) 0.103(3) Uani 1 1 d . . . H29 H 0.0277 1.1267 0.5039 0.123 Uiso 1 1 calc R . . C12 C 0.3886(7) 0.4556(5) 0.8814(4) 0.0516(18) Uani 1 1 d . . . C17 C 0.5066(7) 0.4178(6) 0.8804(4) 0.057(2) Uani 1 1 d . . . C16 C 0.5703(6) 0.3533(6) 0.9596(5) 0.075(2) Uani 1 1 d . . . H16 H 0.6503 0.3266 0.9551 0.089 Uiso 1 1 calc R . . C13 C 0.3333(6) 0.4278(6) 0.9690(4) 0.065(2) Uani 1 1 d . . . H13 H 0.2520 0.4513 0.9734 0.078 Uiso 1 1 calc R . . C14 C 0.3949(7) 0.3665(6) 1.0494(5) 0.073(2) Uani 1 1 d . . . H14 H 0.3551 0.3508 1.1069 0.088 Uiso 1 1 calc R . . C15 C 0.5117(8) 0.3292(6) 1.0461(5) 0.077(2) Uani 1 1 d . . . H15 H 0.5529 0.2879 1.1008 0.093 Uiso 1 1 calc R . . C11 C 0.3201(5) 0.5243(5) 0.7923(4) 0.0494(17) Uani 1 1 d . . . H11 H 0.3634 0.5897 0.7649 0.059 Uiso 1 1 calc R . . C3 C 0.3137(5) 0.5212(6) 0.6241(5) 0.0541(19) Uani 1 1 d . . . C8 C 0.3195(5) 0.4646(6) 0.7194(4) 0.0468(17) Uani 1 1 d . . . C7 C 0.3180(5) 0.3532(6) 0.7448(4) 0.059(2) Uani 1 1 d . . . H7 H 0.3214 0.3132 0.8082 0.071 Uiso 1 1 calc R . . C6 C 0.3117(6) 0.2989(6) 0.6794(5) 0.064(2) Uani 1 1 d . . . C5 C 0.3054(6) 0.3593(6) 0.5857(5) 0.072(2) Uani 1 1 d . . . H5 H 0.3006 0.3241 0.5409 0.086 Uiso 1 1 calc R . . C4 C 0.3059(6) 0.4713(7) 0.5567(4) 0.059(2) Uani 1 1 d . . . C9 C 0.2969(7) 0.5362(6) 0.4520(4) 0.096(3) Uani 1 1 d . . . H9A H 0.2586 0.6074 0.4445 0.144 Uiso 1 1 calc R . . H9B H 0.2496 0.4996 0.4202 0.144 Uiso 1 1 calc R . . H9C H 0.3771 0.5422 0.4256 0.144 Uiso 1 1 calc R . . C10 C 0.3092(7) 0.1769(6) 0.7096(5) 0.100(3) Uani 1 1 d . . . H10A H 0.3708 0.1440 0.7564 0.149 Uiso 1 1 calc R . . H10B H 0.3243 0.1520 0.6562 0.149 Uiso 1 1 calc R . . H10C H 0.2308 0.1573 0.7352 0.149 Uiso 1 1 calc R . . O6 O 0.2508(4) 0.7358(3) 0.8055(3) 0.0620(12) Uani 1 1 d . . . O5 O 0.5783(4) 0.5398(5) 0.7458(3) 0.0933(19) Uani 1 1 d . . . O4 O 0.6411(6) 0.3710(6) 0.7756(4) 0.111(2) Uani 1 1 d . . . O3 O 0.3087(3) 0.6343(4) 0.5980(2) 0.0595(12) Uani 1 1 d . . . O1 O 0.4909(4) 0.8447(4) 0.4715(3) 0.0784(15) Uani 1 1 d . . . O2 O 0.2933(5) 0.8345(4) 0.4697(3) 0.0833(16) Uani 1 1 d . . . N2 N 0.2768(5) 1.1216(5) 0.3976(4) 0.0674(17) Uani 1 1 d . . . N1 N 0.5793(6) 0.4435(7) 0.7938(4) 0.074(2) Uani 1 1 d . . . N3 N 0.3729(6) 0.9913(7) 0.2363(5) 0.097(2) Uani 1 1 d . . . C2 C 0.4201(5) 0.6822(5) 0.5611(4) 0.067(2) Uani 1 1 d . . . H2A H 0.4640 0.6383 0.5273 0.080 Uiso 1 1 calc R . . H2B H 0.4712 0.6829 0.6127 0.080 Uiso 1 1 calc R . . C1 C 0.3956(8) 0.7950(6) 0.4968(4) 0.068(2) Uani 1 1 d . . . C27 C 0.6280(8) 1.1380(6) 0.3043(5) 0.064(2) Uani 1 1 d . . . O8 O 0.5364(4) 1.1868(5) 0.2650(3) 0.0821(17) Uani 1 1 d . . . O7 O 0.6309(4) 1.0473(4) 0.3699(3) 0.0857(15) Uani 1 1 d . . . C36 C 0.3021(12) 0.9685(11) 0.0692(7) 0.153(4) Uani 1 1 d . . . C34 C 0.3800(9) 1.0631(8) 0.1589(7) 0.131(4) Uani 1 1 d . . . H34 H 0.4133 1.1263 0.1591 0.157 Uiso 1 1 calc R . . C35 C 0.3445(11) 1.0583(10) 0.0751(8) 0.157(5) Uani 1 1 d . . . H35 H 0.3496 1.1179 0.0215 0.189 Uiso 1 1 calc R . . C38 C 0.3242(13) 0.9077(10) 0.2335(7) 0.194(6) Uani 1 1 d . . . H38 H 0.3117 0.8545 0.2902 0.233 Uiso 1 1 calc R . . C37 C 0.2873(15) 0.8893(10) 0.1499(10) 0.271(10) Uani 1 1 d . . . H37 H 0.2545 0.8254 0.1512 0.326 Uiso 1 1 calc R . . C39 C 0.2631(14) 0.9570(10) -0.0277(7) 0.270(8) Uani 1 1 d . . . H39A H 0.2027 1.0145 -0.0574 0.405 Uiso 1 1 calc R . . H39B H 0.2299 0.8883 -0.0170 0.405 Uiso 1 1 calc R . . H39C H 0.3329 0.9611 -0.0677 0.405 Uiso 1 1 calc R . . C33 C -0.0147(7) 1.3418(8) 0.4335(6) 0.134(4) Uani 1 1 d . . . H33A H 0.0039 1.3646 0.4862 0.200 Uiso 1 1 calc R . . H33B H -0.0885 1.3056 0.4455 0.200 Uiso 1 1 calc R . . H33C H -0.0249 1.4039 0.3783 0.200 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0819(3) 0.0582(2) 0.0789(2) 0.00086(17) 0.00351(16) -0.01400(17) C18 0.055(5) 0.063(6) 0.039(4) -0.012(4) 0.007(3) -0.025(4) C19 0.061(5) 0.070(6) 0.062(4) -0.013(4) 0.013(4) -0.025(4) C23 0.053(5) 0.077(6) 0.048(4) -0.019(4) 0.014(4) -0.028(5) C22 0.073(6) 0.082(7) 0.079(5) -0.037(5) 0.024(5) -0.017(5) C20 0.062(6) 0.099(8) 0.072(5) -0.018(5) 0.016(4) -0.033(6) C21 0.056(6) 0.135(9) 0.066(5) -0.031(6) 0.018(4) -0.008(6) C24 0.067(5) 0.145(9) 0.140(7) -0.027(6) 0.032(5) -0.054(6) C25 0.085(6) 0.142(10) 0.137(8) -0.065(7) 0.043(5) -0.003(6) C26 0.068(5) 0.054(5) 0.076(5) -0.012(4) -0.001(4) -0.005(4) C32 0.078(6) 0.067(7) 0.070(5) -0.012(5) 0.005(4) -0.012(5) C30 0.058(6) 0.096(8) 0.105(7) -0.029(6) -0.016(5) 0.009(6) C28 0.070(6) 0.072(7) 0.124(7) -0.002(5) 0.017(5) 0.000(5) C31 0.075(6) 0.080(7) 0.092(6) -0.019(5) -0.005(5) -0.010(6) C29 0.075(7) 0.100(9) 0.122(7) -0.019(7) 0.027(5) -0.018(6) C12 0.067(5) 0.046(5) 0.043(4) -0.010(4) 0.006(4) -0.023(4) C17 0.062(5) 0.066(6) 0.039(4) -0.005(4) 0.007(4) -0.022(4) C16 0.069(5) 0.083(6) 0.062(5) -0.004(5) -0.007(5) -0.022(4) C13 0.078(5) 0.069(6) 0.045(4) -0.012(4) 0.010(4) -0.017(4) C14 0.083(6) 0.083(6) 0.048(5) -0.012(4) 0.008(5) -0.013(5) C15 0.100(7) 0.072(6) 0.049(5) 0.004(4) -0.012(5) -0.028(5) C11 0.058(5) 0.048(5) 0.036(4) 0.000(4) 0.008(3) -0.020(4) C3 0.063(5) 0.044(5) 0.044(4) 0.002(4) 0.009(3) -0.011(4) C8 0.050(4) 0.049(5) 0.037(4) -0.005(4) 0.009(3) -0.013(3) C7 0.088(5) 0.051(5) 0.036(4) -0.008(4) 0.010(4) -0.017(4) C6 0.077(5) 0.051(5) 0.059(5) -0.009(5) 0.004(4) -0.016(4) C5 0.099(6) 0.060(6) 0.059(5) -0.021(5) 0.008(4) -0.012(5) C4 0.073(5) 0.071(6) 0.034(4) -0.019(4) 0.008(3) -0.001(4) C9 0.140(7) 0.099(7) 0.044(4) -0.018(5) -0.002(4) -0.007(5) C10 0.147(8) 0.062(6) 0.092(6) -0.024(5) 0.011(5) -0.022(5) O6 0.067(3) 0.057(3) 0.058(3) -0.010(3) 0.004(2) -0.016(3) O5 0.085(4) 0.088(5) 0.079(4) 0.015(3) 0.017(3) -0.020(3) O4 0.121(5) 0.117(6) 0.083(4) -0.019(4) 0.027(4) 0.010(4) O3 0.062(3) 0.057(3) 0.047(3) -0.001(2) 0.016(2) -0.003(3) O1 0.080(3) 0.053(3) 0.088(3) -0.001(3) 0.023(3) -0.013(3) O2 0.079(4) 0.067(4) 0.081(4) 0.008(3) -0.008(3) -0.002(3) N2 0.060(4) 0.064(5) 0.073(4) -0.011(4) 0.004(3) -0.015(4) N1 0.057(5) 0.099(7) 0.060(5) -0.016(5) -0.002(4) -0.011(4) N3 0.139(6) 0.059(5) 0.082(6) 0.004(5) -0.025(4) -0.036(5) C2 0.071(5) 0.059(5) 0.053(4) 0.008(4) 0.013(4) -0.013(4) C1 0.090(7) 0.056(6) 0.044(4) 0.003(4) -0.006(5) -0.007(5) C27 0.084(6) 0.051(6) 0.060(5) -0.019(5) 0.018(5) -0.025(5) O8 0.053(3) 0.104(5) 0.074(3) -0.003(3) -0.002(3) -0.012(3) O7 0.100(4) 0.060(4) 0.092(4) -0.012(3) 0.005(3) -0.020(3) C36 0.268(14) 0.097(10) 0.090(9) -0.019(8) -0.068(8) -0.014(10) C34 0.221(11) 0.098(9) 0.056(6) 0.006(7) -0.020(7) -0.032(7) C35 0.262(14) 0.110(11) 0.090(9) -0.001(8) -0.007(8) -0.073(9) C38 0.384(19) 0.104(10) 0.082(8) 0.005(7) -0.083(9) -0.073(12) C37 0.57(3) 0.097(10) 0.129(11) 0.018(9) -0.139(14) -0.122(14) C39 0.51(3) 0.165(14) 0.133(10) -0.025(9) -0.121(13) -0.064(15) C33 0.081(6) 0.132(10) 0.174(9) -0.035(7) 0.008(6) 0.013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 O1 2.200(4) . ? Hg1 N2 2.200(6) . ? Hg1 O7 2.276(4) . ? Hg1 N3 2.401(7) . ? C18 C19 1.388(8) . ? C18 C23 1.397(9) . ? C18 C11 1.530(8) . ? C19 C20 1.378(9) . ? C23 C22 1.368(9) . ? C23 O6 1.384(7) . ? C22 C21 1.400(10) . ? C22 C25 1.508(9) . ? C20 C21 1.356(10) . ? C20 C24 1.524(10) . ? C26 O6 1.417(6) . ? C26 C27 1.518(8) 2_676 ? C32 N2 1.312(8) . ? C32 C31 1.353(9) . ? C30 C31 1.363(9) . ? C30 C29 1.381(10) . ? C30 C33 1.508(10) . ? C28 N2 1.303(8) . ? C28 C29 1.356(10) . ? C12 C17 1.353(8) . ? C12 C13 1.389(7) . ? C12 C11 1.528(8) . ? C17 C16 1.385(8) . ? C17 N1 1.473(8) . ? C16 C15 1.393(8) . ? C13 C14 1.376(8) . ? C14 C15 1.343(8) . ? C11 C8 1.529(8) . ? C3 C4 1.371(8) . ? C3 C8 1.386(8) . ? C3 O3 1.396(7) . ? C8 C7 1.381(8) . ? C7 C6 1.383(8) . ? C6 C5 1.378(8) . ? C6 C10 1.512(9) . ? C5 C4 1.385(8) . ? C4 C9 1.533(8) . ? O5 N1 1.233(7) . ? O4 N1 1.214(7) . ? O3 C2 1.445(6) . ? O1 C1 1.270(8) . ? O2 C1 1.221(8) . ? N3 C34 1.247(9) . ? N3 C38 1.267(11) . ? C2 C1 1.488(9) . ? C27 O8 1.207(8) . ? C27 O7 1.276(7) . ? C27 C26 1.518(8) 2_676 ? C36 C35 1.324(12) . ? C36 C37 1.338(13) . ? C36 C39 1.580(13) . ? C34 C35 1.347(11) . ? C38 C37 1.422(13) . ? 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 Hg1 N2 130.5(2) . . ? O1 Hg1 O7 88.38(18) . . ? N2 Hg1 O7 126.0(2) . . ? O1 Hg1 N3 105.0(2) . . ? N2 Hg1 N3 97.7(2) . . ? O7 Hg1 N3 107.2(2) . . ? C19 C18 C23 117.7(6) . . ? C19 C18 C11 121.1(7) . . ? C23 C18 C11 121.1(6) . . ? C20 C19 C18 123.1(7) . . ? C22 C23 O6 119.9(8) . . ? C22 C23 C18 120.9(7) . . ? O6 C23 C18 119.0(7) . . ? C23 C22 C21 118.1(8) . . ? C23 C22 C25 121.5(8) . . ? C21 C22 C25 120.4(8) . . ? C21 C20 C19 116.8(7) . . ? C21 C20 C24 122.1(9) . . ? C19 C20 C24 121.1(9) . . ? C20 C21 C22 123.4(8) . . ? O6 C26 C27 109.9(6) . 2_676 ? N2 C32 C31 123.1(7) . . ? C31 C30 C29 115.6(8) . . ? C31 C30 C33 122.9(10) . . ? C29 C30 C33 121.4(9) . . ? N2 C28 C29 121.9(8) . . ? C32 C31 C30 120.1(8) . . ? C28 C29 C30 120.9(8) . . ? C17 C12 C13 115.6(6) . . ? C17 C12 C11 122.4(6) . . ? C13 C12 C11 122.0(6) . . ? C12 C17 C16 123.8(6) . . ? C12 C17 N1 122.2(6) . . ? C16 C17 N1 114.0(7) . . ? C17 C16 C15 118.5(7) . . ? C14 C13 C12 122.2(6) . . ? C15 C14 C13 120.9(6) . . ? C14 C15 C16 119.0(7) . . ? C12 C11 C8 111.5(5) . . ? C12 C11 C18 112.1(5) . . ? C8 C11 C18 110.3(5) . . ? C4 C3 C8 122.8(7) . . ? C4 C3 O3 119.8(6) . . ? C8 C3 O3 117.4(7) . . ? C7 C8 C3 117.0(6) . . ? C7 C8 C11 122.1(5) . . ? C3 C8 C11 120.9(6) . . ? C8 C7 C6 122.5(6) . . ? C5 C6 C7 118.1(7) . . ? C5 C6 C10 120.7(7) . . ? C7 C6 C10 121.2(6) . . ? C6 C5 C4 121.6(7) . . ? C3 C4 C5 118.1(6) . . ? C3 C4 C9 121.7(7) . . ? C5 C4 C9 120.2(7) . . ? C23 O6 C26 114.9(5) . . ? C3 O3 C2 115.8(5) . . ? C1 O1 Hg1 107.1(5) . . ? C28 N2 C32 118.3(7) . . ? C28 N2 Hg1 121.3(6) . . ? C32 N2 Hg1 120.4(5) . . ? O4 N1 O5 123.5(7) . . ? O4 N1 C17 119.2(8) . . ? O5 N1 C17 117.2(7) . . ? C34 N3 C38 114.8(9) . . ? C34 N3 Hg1 124.0(7) . . ? C38 N3 Hg1 121.1(7) . . ? O3 C2 C1 111.6(6) . . ? O2 C1 O1 123.7(7) . . ? O2 C1 C2 122.7(7) . . ? O1 C1 C2 113.6(7) . . ? O8 C27 O7 124.3(7) . . ? O8 C27 C26 122.4(7) . 2_676 ? O7 C27 C26 113.2(7) . 2_676 ? C27 O7 Hg1 102.8(5) . . ? C35 C36 C37 117.0(11) . . ? C35 C36 C39 122.0(12) . . ? C37 C36 C39 120.9(13) . . ? N3 C34 C35 126.5(10) . . ? C36 C35 C34 119.8(11) . . ? N3 C38 C37 124.8(10) . . ? C36 C37 C38 116.7(11) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.690 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.100 # Attachment '- complex 9.cif' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated directly or indirectly from an entry in the # Cambridge Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting from # the CCDC's data processing and validation procedures. Files generated from # CSD entries are Copyright 2011 Cambridge Crystallographic Data Centre. They # may be used in bona fide research applications only, and may not be copied or # further disseminated in any form, whether machine-readable or not, except for # the purposes of generating routine backup copies on your local computer # system. # # Files arising from any other source may also contain material that is the # copyright of third parties, including the originator, and you should check # with the originator concerning the permitted uses of the information # contained in this CIF. # # For further information on the CCDC and the free tools enCIFer and Mercury # for validating and visualising CIF files, please visit www.ccdc.cam.ac.uk # ####################################################################### data_cdabp14picmeoh_0m _database_code_depnum_ccdc_archive 'CCDC 859336' #TrackingRef '- complex 9.cif' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 12.0700(7) _cell_length_b 15.6708(10) _cell_length_c 26.0946(16) _cell_angle_alpha 90.00 _cell_angle_beta 101.023(3) _cell_angle_gamma 90.00 _cell_volume 4844.64 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z N1 N 0.1450(5) 0.1158(4) 0.2164(2) C28 C 0.0558(6) 0.1649(5) 0.2265(3) H28 H 0.0639 0.2237 0.2304 C29 C -0.0457(6) 0.1262(5) 0.2308(3) H29 H -0.1054 0.1591 0.2376 C30 C -0.0578(6) 0.0383(5) 0.2250(3) C31 C 0.0315(5) -0.0108(5) 0.2149(3) H31 H 0.0234 -0.0696 0.2111 C32 C 0.1329(5) 0.0279(4) 0.2106(2) H32 H 0.1926 -0.0050 0.2039 C12 C 0.3236(6) -0.3341(4) 0.0790(3) C17 C 0.2739(7) -0.3833(4) 0.0365(3) H17 H 0.2354 -0.3571 0.0063 C16 C 0.2818(8) -0.4718(4) 0.0390(4) H16 H 0.2485 -0.5047 0.0106 C15 C 0.3393(8) -0.5110(4) 0.0841(4) H15 H 0.3446 -0.5702 0.0858 C14 C 0.3890(8) -0.4618(4) 0.1266(4) H14 H 0.4275 -0.4880 0.1568 C13 C 0.3812(7) -0.3733(4) 0.1241(3) H13 H 0.4144 -0.3404 0.1525 C40 C 0.4841(8) 0.3261(4) 0.1689(4) H40 H 0.4257 0.3631 0.1722 C41 C 0.5846(9) 0.3581(4) 0.1581(5) H41 H 0.5935 0.4166 0.1544 C42 C 0.6719(8) 0.3028(5) 0.1531(6) C43 C 0.6587(7) 0.2154(5) 0.1587(5) H43 H 0.7172 0.1784 0.1554 C44 C 0.5583(6) 0.1833(4) 0.1695(4) H44 H 0.5494 0.1249 0.1732 N3 N 0.4709(7) 0.2386(4) 0.1745(4) Cd1 Cd 0.30351(10) 0.18404(8) 0.19350(5) N2 N 0.1948(11) 0.2978(7) 0.1518(5) C36 C 0.0572(15) 0.4308(12) 0.1042(8) C38 C 0.1343(13) 0.2919(10) 0.1060(8) H38 H 0.1364 0.2406 0.0883 C34 C 0.1871(17) 0.3732(12) 0.1727(7) H34 H 0.2349 0.3820 0.2047 C35 C 0.1206(17) 0.4393(12) 0.1549(7) H35 H 0.1167 0.4879 0.1749 C37 C 0.0665(14) 0.3557(13) 0.0809(8) H37 H 0.0264 0.3466 0.0473 C23 C 0.1284(14) -0.1808(9) 0.0728(6) C19 C 0.1969(17) -0.1783(10) -0.0064(7) H19 H 0.2547 -0.1897 -0.0244 C18 C 0.2193(14) -0.1993(9) 0.0475(6) C20 C 0.1025(19) -0.1441(12) -0.0347(7) C22 C 0.0294(15) -0.1415(11) 0.0447(7) C21 C 0.0203(19) -0.1260(11) -0.0074(8) H21 H -0.0462 -0.1016 -0.0253 O2 O 0.3629(10) 0.0491(8) 0.1661(5) O1 O 0.2579(12) 0.1204(8) 0.1022(6) C8 C 0.4292(13) -0.2029(8) 0.0615(7) C3 C 0.4645(12) -0.1201(9) 0.0747(6) C11 C 0.3263(12) -0.2385(10) 0.0772(5) H11 H 0.3307 -0.2201 0.1135 C4 C 0.5609(13) -0.0843(12) 0.0623(8) C7 C 0.500(2) -0.2489(14) 0.0349(10) H7 H 0.4812 -0.3054 0.0265 C2 C 0.3306(14) -0.0072(9) 0.0785(7) H2A H 0.2573 -0.0300 0.0626 H2B H 0.3645 0.0178 0.0512 C1 C 0.3172(14) 0.0597(11) 0.1182(8) O4 O 0.1453(9) -0.1929(7) 0.1270(4) O3 O 0.4027(9) -0.0759(6) 0.1045(3) C26 C 0.1027(15) -0.2728(10) 0.1419(6) H26A H 0.1355 -0.3192 0.1252 H26B H 0.0215 -0.2747 0.1303 C27 C 0.3689(14) 0.2164(12) 0.3001(8) O5 O 0.3121(11) 0.2699(9) 0.2727(4) O6 O 0.4013(11) 0.1501(9) 0.2816(5) C39 C -0.0157(17) 0.5017(15) 0.0784(9) H39A H -0.0453 0.5333 0.1043 H39B H -0.0770 0.4784 0.0534 H39C H 0.0283 0.5389 0.0610 C33 C -0.168(3) 0.001(3) 0.2371(16) H33A H -0.2201 -0.0101 0.2049 H33B H -0.2013 0.0405 0.2577 H33C H -0.1520 -0.0518 0.2560 C24 C 0.0860(19) -0.1248(15) -0.0894(7) H24A H 0.0354 -0.1657 -0.1087 H24B H 0.1573 -0.1271 -0.1006 H24C H 0.0545 -0.0686 -0.0955 C25 C -0.0639(17) -0.1180(16) 0.0762(9) H25A H -0.1106 -0.0734 0.0585 H25B H -0.0292 -0.0990 0.1105 H25C H -0.1095 -0.1674 0.0791 C5 C 0.624(2) -0.1362(15) 0.0342(11) H5 H 0.6887 -0.1131 0.0251 C9 C 0.5979(16) 0.0027(13) 0.0759(9) H9A H 0.5410 0.0421 0.0595 H9B H 0.6670 0.0137 0.0640 H9C H 0.6099 0.0098 0.1131 C6 C 0.597(2) -0.2156(15) 0.0199(13) C45 C 0.774(2) 0.3481(18) 0.1355(14) H45A H 0.7841 0.3251 0.1026 H45B H 0.8412 0.3389 0.1613 H45C H 0.7593 0.4083 0.1319 C10 C 0.688(4) -0.272(2) 0.006(3) H10A H 0.7342 -0.2938 0.0376 H10B H 0.7340 -0.2401 -0.0131 H10C H 0.6540 -0.3192 -0.0147 C26' C 0.3973 0.2272 0.3581 C27' C 0.1311 -0.2836 0.1999 O7 O 0.1239(18) 0.3634(15) 0.2949(7) #END # Attachment '- complex11.cif' data_hg4pic_0m_11 _database_code_depnum_ccdc_archive 'CCDC 859337' #TrackingRef '- complex11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H92 Hg2 N8 O18' _chemical_formula_weight 1902.84 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' Hg Hg -2.3894 9.2266 '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 37.3419(10) _cell_length_b 9.7381(2) _cell_length_c 23.5545(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.128(2) _cell_angle_gamma 90.00 _cell_volume 8374.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9890 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 21.66 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3824 _exptl_absorpt_coefficient_mu 3.734 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2511 _exptl_absorpt_correction_T_max 0.3467 _exptl_absorpt_process_details 'North et al.,1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48101 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7537 _reflns_number_gt 5174 _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^)+(0.0438P)^2^+5.0000P] 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 7537 _refine_ls_number_parameters 513 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.898 _refine_ls_shift/su_max 1.080 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.213929(5) 0.264120(17) 0.433207(8) 0.06224(9) Uani 1 1 d . . . C8 C 0.39898(13) 0.2881(4) 0.36065(19) 0.0523(11) Uani 1 1 d . . . C3 C 0.36277(14) 0.3207(5) 0.3351(2) 0.0605(12) Uani 1 1 d . . . C7 C 0.42624(13) 0.3393(4) 0.3345(2) 0.0605(12) Uani 1 1 d . . . H7 H 0.4505 0.3220 0.3521 0.073 Uiso 1 1 calc R . . C6 C 0.41903(15) 0.4148(5) 0.2837(2) 0.0659(13) Uani 1 1 d . . . C4 C 0.35398(15) 0.3974(5) 0.2842(2) 0.0726(14) Uani 1 1 d . . . C5 C 0.38281(17) 0.4420(5) 0.2596(2) 0.0758(15) Uani 1 1 d . . . H5 H 0.3773 0.4925 0.2254 0.091 Uiso 1 1 calc R . . C10 C 0.44889(16) 0.4594(6) 0.2546(3) 0.0975(19) Uani 1 1 d . . . H10A H 0.4384 0.4953 0.2168 0.146 Uiso 1 1 calc R . . H10B H 0.4642 0.3823 0.2508 0.146 Uiso 1 1 calc R . . H10C H 0.4633 0.5294 0.2774 0.146 Uiso 1 1 calc R . . C18 C 0.40733(12) 0.0419(4) 0.3921(2) 0.0566(12) Uani 1 1 d . . . C23 C 0.39551(12) -0.0611(4) 0.4242(2) 0.0576(12) Uani 1 1 d . . . C21 C 0.40691(16) -0.2296(5) 0.3572(3) 0.0835(18) Uani 1 1 d . . . H21 H 0.4069 -0.3210 0.3458 0.100 Uiso 1 1 calc R . . C22 C 0.39543(13) -0.1982(5) 0.4079(2) 0.0684(14) Uani 1 1 d . . . C19 C 0.41851(14) 0.0045(5) 0.3422(2) 0.0790(16) Uani 1 1 d . . . H19 H 0.4266 0.0726 0.3203 0.095 Uiso 1 1 calc R . . C20 C 0.41825(16) -0.1313(5) 0.3231(3) 0.0869(17) Uani 1 1 d . . . C11 C 0.40699(12) 0.1911(4) 0.41251(19) 0.0536(11) Uani 1 1 d . . . H11 H 0.3864 0.1995 0.4322 0.064 Uiso 1 1 calc R . . C12 C 0.44110(13) 0.2307(4) 0.4562(2) 0.0578(12) Uani 1 1 d . . . C17 C 0.43854(13) 0.3314(5) 0.4965(2) 0.0615(12) Uani 1 1 d . . . H17 H 0.4160 0.3713 0.4970 0.074 Uiso 1 1 calc R . . C37 C 0.15139(19) -0.1185(7) 0.4141(3) 0.107(2) Uani 1 1 d . . . H37 H 0.1268 -0.1413 0.4103 0.128 Uiso 1 1 calc R . . C38 C 0.16260(16) 0.0148(5) 0.4200(2) 0.0817(16) Uani 1 1 d . . . H38 H 0.1455 0.0836 0.4209 0.098 Uiso 1 1 calc R . . C34 C 0.22281(15) -0.0482(5) 0.42429(19) 0.0663(13) Uani 1 1 d . . . H34 H 0.2472 -0.0229 0.4274 0.080 Uiso 1 1 calc R . . C26 C 0.34604(14) -0.0230(5) 0.4699(2) 0.0724(14) Uani 1 1 d . . . H26A H 0.3382 -0.1133 0.4796 0.087 Uiso 1 1 calc R . . H26B H 0.3342 -0.0035 0.4300 0.087 Uiso 1 1 calc R . . O6 O 0.38463(9) -0.0239(3) 0.47491(14) 0.0652(8) Uani 1 1 d . . . O1 O 0.27029(8) 0.3586(3) 0.44244(14) 0.0709(9) Uani 1 1 d . . . O2 O 0.27141(9) 0.1857(3) 0.38080(15) 0.0738(10) Uani 1 1 d . . . O3 O 0.33485(9) 0.2620(3) 0.35824(15) 0.0661(9) Uani 1 1 d . . . C1 C 0.28462(13) 0.2895(5) 0.4065(2) 0.0578(12) Uani 1 1 d . . . C2 C 0.31996(12) 0.3493(4) 0.3963(2) 0.0633(12) Uani 1 1 d . . . H2A H 0.3155 0.4399 0.3792 0.076 Uiso 1 1 calc R . . H2B H 0.3373 0.3584 0.4330 0.076 Uiso 1 1 calc R . . N3 N 0.19806(12) 0.0489(4) 0.42460(15) 0.0615(10) Uani 1 1 d . . . C16 C 0.46904(16) 0.3725(5) 0.5358(2) 0.0723(14) Uani 1 1 d . . . C15 C 0.50282(17) 0.3184(7) 0.5372(3) 0.0911(18) Uani 1 1 d . . . H15 H 0.5233 0.3488 0.5640 0.109 Uiso 1 1 calc R . . C14 C 0.50565(18) 0.2177(7) 0.4979(3) 0.108(2) Uani 1 1 d . . . H14 H 0.5283 0.1774 0.4984 0.129 Uiso 1 1 calc R . . C13 C 0.47530(15) 0.1750(6) 0.4575(3) 0.0865(17) Uani 1 1 d . . . H13 H 0.4779 0.1077 0.4307 0.104 Uiso 1 1 calc R . . C25 C 0.38366(17) -0.3117(5) 0.4444(3) 0.101(2) Uani 1 1 d . . . H25A H 0.3574 -0.3175 0.4361 0.152 Uiso 1 1 calc R . . H25B H 0.3924 -0.2917 0.4848 0.152 Uiso 1 1 calc R . . H25C H 0.3937 -0.3976 0.4351 0.152 Uiso 1 1 calc R . . C27 C 0.33399(15) 0.0822(5) 0.5091(2) 0.0595(12) Uani 1 1 d . . . C28 C 0.20456(17) 0.3244(7) 0.2922(3) 0.0927(18) Uani 1 1 d . . . H28 H 0.2211 0.2519 0.2960 0.111 Uiso 1 1 calc R . . C32 C 0.1661(2) 0.4558(7) 0.3297(3) 0.115(2) Uani 1 1 d . . . H32 H 0.1545 0.4778 0.3598 0.139 Uiso 1 1 calc R . . N2 N 0.18972(12) 0.3558(4) 0.33756(19) 0.0760(12) Uani 1 1 d . . . C35 C 0.21375(17) -0.1862(5) 0.4195(2) 0.0766(15) Uani 1 1 d . . . C36 C 0.1774(2) -0.2185(6) 0.4138(3) 0.103(2) Uani 1 1 d . . . H36 H 0.1702 -0.3100 0.4096 0.123 Uiso 1 1 calc R . . C39 C 0.2433(2) -0.2924(6) 0.4199(3) 0.116(2) Uani 1 1 d . . . H39A H 0.2415 -0.3626 0.4477 0.174 Uiso 1 1 calc R . . H39B H 0.2669 -0.2493 0.4301 0.174 Uiso 1 1 calc R . . H39C H 0.2404 -0.3327 0.3820 0.174 Uiso 1 1 calc R . . O7 O 0.35343(10) 0.1804(4) 0.52814(16) 0.0832(10) Uani 1 1 d . . . O4 O 0.43491(18) 0.5227(7) 0.5785(3) 0.176(3) Uani 1 1 d . . . N1 N 0.4651(2) 0.4774(6) 0.5790(3) 0.1100(18) Uani 1 1 d . . . C29 C 0.19670(19) 0.3934(8) 0.2403(3) 0.102(2) Uani 1 1 d . . . C31 C 0.1574(3) 0.5318(8) 0.2783(4) 0.158(4) Uani 1 1 d . . . H31 H 0.1407 0.6039 0.2744 0.190 Uiso 1 1 calc R . . C30 C 0.1739(3) 0.4971(9) 0.2344(4) 0.141(3) Uani 1 1 d . . . H30 H 0.1690 0.5470 0.1999 0.169 Uiso 1 1 calc R . . C33 C 0.2135(2) 0.3529(11) 0.1900(3) 0.165(4) Uani 1 1 d . . . H33A H 0.1951 0.3109 0.1604 0.248 Uiso 1 1 calc R . . H33B H 0.2330 0.2888 0.2030 0.248 Uiso 1 1 calc R . . H33C H 0.2229 0.4330 0.1745 0.248 Uiso 1 1 calc R . . C9 C 0.31459(16) 0.4244(7) 0.2554(3) 0.118(2) Uani 1 1 d . . . H9A H 0.3005 0.3422 0.2561 0.177 Uiso 1 1 calc R . . H9B H 0.3132 0.4519 0.2158 0.177 Uiso 1 1 calc R . . H9C H 0.3050 0.4962 0.2758 0.177 Uiso 1 1 calc R . . O8 O 0.30208(9) 0.0596(3) 0.51807(14) 0.0703(9) Uani 1 1 d . . . C24 C 0.4287(2) -0.1670(7) 0.2667(3) 0.141(3) Uani 1 1 d . . . H24A H 0.4283 -0.0855 0.2437 0.211 Uiso 1 1 calc R . . H24B H 0.4116 -0.2324 0.2461 0.211 Uiso 1 1 calc R . . H24C H 0.4529 -0.2059 0.2744 0.211 Uiso 1 1 calc R . . O5 O 0.49162(15) 0.5139(6) 0.6135(2) 0.163(2) Uani 1 1 d . . . N4 N 0.4510(2) 0.0316(7) 0.1382(3) 0.1150(18) Uani 1 1 d . . . C41 C 0.4779(4) 0.1260(12) 0.1790(5) 0.257(7) Uani 1 1 d . . . H41A H 0.4803 0.2112 0.1597 0.385 Uiso 1 1 calc R . . H41B H 0.5014 0.0822 0.1893 0.385 Uiso 1 1 calc R . . H41C H 0.4687 0.1435 0.2135 0.385 Uiso 1 1 calc R . . C42 C 0.4716(4) -0.0894(17) 0.1406(7) 0.318(9) Uani 1 1 d . . . H42A H 0.4558 -0.1673 0.1405 0.477 Uiso 1 1 calc R . . H42B H 0.4903 -0.0898 0.1754 0.477 Uiso 1 1 calc R . . H42C H 0.4827 -0.0938 0.1074 0.477 Uiso 1 1 calc R . . O9 O 0.4084(7) 0.1242(15) 0.1284(9) 0.450(12) Uani 1 1 d D . . C43 C 0.4184(6) 0.009(2) 0.1084(7) 0.51(3) Uani 1 1 d D . . H43 H 0.4070 -0.0588 0.0834 0.613 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.06550(15) 0.05577(12) 0.06732(15) 0.00208(9) 0.01820(10) 0.00000(9) C8 0.051(3) 0.048(2) 0.059(3) -0.017(2) 0.014(2) -0.004(2) C3 0.056(3) 0.059(3) 0.068(3) -0.018(2) 0.016(3) -0.006(2) C7 0.054(3) 0.054(3) 0.077(4) -0.014(2) 0.021(3) -0.004(2) C6 0.072(4) 0.060(3) 0.070(4) -0.013(2) 0.025(3) -0.003(2) C4 0.068(4) 0.080(3) 0.065(4) -0.012(3) 0.002(3) 0.007(3) C5 0.096(5) 0.076(3) 0.056(3) -0.001(2) 0.019(3) 0.001(3) C10 0.118(5) 0.078(4) 0.115(5) 0.001(3) 0.067(4) -0.005(3) C18 0.045(3) 0.052(3) 0.075(3) -0.013(2) 0.019(3) -0.002(2) C23 0.047(3) 0.056(3) 0.069(3) -0.007(2) 0.011(3) 0.005(2) C21 0.079(4) 0.054(3) 0.120(5) -0.025(3) 0.028(4) 0.006(3) C22 0.059(3) 0.052(3) 0.096(4) -0.004(3) 0.020(3) 0.001(2) C19 0.086(4) 0.057(3) 0.106(5) -0.013(3) 0.049(4) -0.005(3) C20 0.098(5) 0.068(4) 0.109(5) -0.023(3) 0.055(4) -0.001(3) C11 0.046(3) 0.052(2) 0.066(3) -0.010(2) 0.019(2) -0.005(2) C12 0.053(3) 0.057(3) 0.064(3) 0.000(2) 0.014(2) -0.003(2) C17 0.055(3) 0.063(3) 0.064(3) 0.000(2) 0.007(3) -0.004(2) C37 0.095(5) 0.087(5) 0.150(6) -0.013(4) 0.053(5) -0.030(4) C38 0.085(4) 0.075(4) 0.090(4) -0.011(3) 0.028(3) -0.010(3) C34 0.079(4) 0.055(3) 0.066(3) 0.008(2) 0.018(3) -0.004(2) C26 0.070(4) 0.070(3) 0.084(4) -0.013(3) 0.033(3) -0.010(3) O6 0.060(2) 0.069(2) 0.066(2) 0.0005(16) 0.0108(18) 0.0053(16) O1 0.060(2) 0.075(2) 0.082(2) -0.0092(18) 0.0251(19) 0.0047(16) O2 0.075(2) 0.066(2) 0.086(3) -0.0046(19) 0.030(2) -0.0144(18) O3 0.049(2) 0.067(2) 0.084(2) -0.0215(16) 0.0172(18) -0.0047(15) C1 0.049(3) 0.062(3) 0.060(3) 0.011(2) 0.006(3) 0.009(2) C2 0.054(3) 0.059(3) 0.079(3) -0.013(2) 0.020(3) -0.002(2) N3 0.077(3) 0.057(2) 0.052(2) 0.0011(17) 0.017(2) -0.014(2) C16 0.070(4) 0.075(3) 0.069(4) -0.001(3) 0.008(3) -0.013(3) C15 0.062(4) 0.109(5) 0.093(5) 0.006(4) -0.005(4) -0.018(3) C14 0.058(4) 0.132(6) 0.129(6) -0.002(5) 0.009(4) 0.015(4) C13 0.050(4) 0.102(4) 0.105(5) -0.020(3) 0.010(3) 0.005(3) C25 0.115(5) 0.055(3) 0.140(6) 0.011(3) 0.041(4) 0.007(3) C27 0.069(4) 0.057(3) 0.055(3) 0.007(2) 0.017(3) 0.001(2) C28 0.096(5) 0.105(4) 0.071(4) 0.009(3) 0.003(4) 0.011(4) C32 0.137(6) 0.115(5) 0.088(5) 0.001(4) 0.010(4) 0.038(5) N2 0.081(3) 0.077(3) 0.066(3) 0.009(2) 0.006(3) 0.013(2) C35 0.102(5) 0.056(3) 0.076(4) 0.007(2) 0.030(3) -0.006(3) C36 0.123(6) 0.067(4) 0.129(6) -0.010(3) 0.050(5) -0.034(4) C39 0.150(7) 0.066(4) 0.140(6) 0.015(4) 0.049(5) 0.010(4) O7 0.072(3) 0.077(2) 0.103(3) -0.026(2) 0.025(2) -0.007(2) O4 0.137(5) 0.202(6) 0.167(5) -0.123(5) -0.013(4) 0.015(5) N1 0.111(5) 0.114(4) 0.094(4) -0.029(3) -0.005(4) -0.019(4) C29 0.092(5) 0.129(6) 0.073(5) 0.031(4) -0.009(4) -0.003(4) C31 0.224(10) 0.132(7) 0.102(6) 0.024(5) -0.006(7) 0.085(6) C30 0.189(9) 0.138(7) 0.088(6) 0.039(5) 0.008(6) 0.021(6) C33 0.138(7) 0.286(12) 0.070(5) 0.024(6) 0.021(5) 0.008(8) C9 0.086(5) 0.165(7) 0.091(5) 0.014(4) -0.008(4) 0.022(4) O8 0.078(3) 0.0595(19) 0.083(2) -0.0028(16) 0.039(2) -0.0030(16) C24 0.205(8) 0.092(5) 0.163(7) -0.044(5) 0.121(6) -0.003(5) O5 0.143(5) 0.193(5) 0.133(4) -0.070(4) -0.019(4) -0.053(4) N4 0.126(6) 0.125(5) 0.103(5) -0.005(4) 0.043(4) -0.004(4) C41 0.351(18) 0.195(12) 0.265(14) -0.076(11) 0.158(13) -0.101(13) C42 0.40(2) 0.282(19) 0.35(2) -0.031(16) 0.26(2) 0.036(18) O9 0.62(3) 0.253(13) 0.53(3) 0.136(15) 0.24(2) 0.139(17) C43 0.40(4) 0.93(8) 0.150(13) -0.01(3) -0.058(19) -0.40(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N3 2.176(4) . ? Hg1 O8 2.215(3) 7_556 ? Hg1 O1 2.265(3) . ? Hg1 N2 2.415(4) . ? C8 C7 1.388(6) . ? C8 C3 1.396(6) . ? C8 C11 1.523(6) . ? C3 C4 1.393(7) . ? C3 O3 1.396(5) . ? C7 C6 1.382(6) . ? C6 C5 1.378(7) . ? C6 C10 1.492(7) . ? C4 C5 1.394(7) . ? C4 C9 1.508(7) . ? C18 C19 1.375(6) . ? C18 C23 1.384(6) . ? C18 C11 1.531(5) . ? C23 O6 1.387(5) . ? C23 C22 1.389(6) . ? C21 C20 1.373(7) . ? C21 C22 1.385(8) . ? C22 C25 1.520(7) . ? C19 C20 1.396(6) . ? C20 C24 1.501(7) . ? C11 C12 1.510(6) . ? C12 C17 1.382(6) . ? C12 C13 1.382(7) . ? C17 C16 1.367(6) . ? C37 C38 1.362(7) . ? C37 C36 1.377(8) . ? C38 N3 1.347(6) . ? C34 N3 1.323(6) . ? C34 C35 1.384(7) . ? C26 O6 1.421(5) . ? C26 C27 1.509(6) . ? O1 C1 1.283(5) . ? O2 C1 1.227(6) . ? O3 C2 1.430(5) . ? C1 C2 1.507(6) . ? C16 C15 1.361(7) . ? C16 N1 1.472(7) . ? C15 C14 1.367(9) . ? C14 C13 1.383(8) . ? C27 O7 1.227(5) . ? C27 O8 1.272(5) . ? C28 N2 1.339(6) . ? C28 C29 1.371(7) . ? C32 N2 1.301(7) . ? C32 C31 1.399(9) . ? C35 C36 1.372(8) . ? C35 C39 1.512(8) . ? O4 N1 1.209(7) . ? N1 O5 1.195(6) . ? C29 C30 1.309(9) . ? C29 C33 1.505(9) . ? C31 C30 1.355(10) . ? O8 Hg1 2.215(3) 7_556 ? N4 C43 1.290(17) . ? N4 C42 1.401(14) . ? N4 C41 1.540(12) . ? O9 C43 1.298(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Hg1 O8 134.16(13) . 7_556 ? N3 Hg1 O1 129.02(14) . . ? O8 Hg1 O1 88.96(12) 7_556 . ? N3 Hg1 N2 103.16(14) . . ? O8 Hg1 N2 96.20(14) 7_556 . ? O1 Hg1 N2 95.60(13) . . ? C7 C8 C3 117.5(5) . . ? C7 C8 C11 122.7(4) . . ? C3 C8 C11 119.7(4) . . ? C4 C3 C8 121.7(5) . . ? C4 C3 O3 119.7(5) . . ? C8 C3 O3 118.3(4) . . ? C6 C7 C8 123.2(5) . . ? C5 C6 C7 117.1(5) . . ? C5 C6 C10 121.2(5) . . ? C7 C6 C10 121.7(5) . . ? C3 C4 C5 117.5(5) . . ? C3 C4 C9 120.8(5) . . ? C5 C4 C9 121.6(5) . . ? C6 C5 C4 123.1(5) . . ? C19 C18 C23 117.6(4) . . ? C19 C18 C11 123.0(4) . . ? C23 C18 C11 119.4(4) . . ? C18 C23 O6 117.8(4) . . ? C18 C23 C22 121.9(5) . . ? O6 C23 C22 120.3(4) . . ? C20 C21 C22 122.7(5) . . ? C21 C22 C23 117.9(5) . . ? C21 C22 C25 120.3(5) . . ? C23 C22 C25 121.8(5) . . ? C18 C19 C20 122.9(5) . . ? C21 C20 C19 117.0(5) . . ? C21 C20 C24 121.7(5) . . ? C19 C20 C24 121.3(5) . . ? C12 C11 C8 112.6(3) . . ? C12 C11 C18 113.3(4) . . ? C8 C11 C18 110.4(4) . . ? C17 C12 C13 117.4(5) . . ? C17 C12 C11 118.7(4) . . ? C13 C12 C11 123.9(4) . . ? C16 C17 C12 120.3(5) . . ? C38 C37 C36 118.2(6) . . ? N3 C38 C37 121.3(5) . . ? N3 C34 C35 122.4(5) . . ? O6 C26 C27 112.4(4) . . ? C23 O6 C26 113.9(3) . . ? C1 O1 Hg1 103.4(3) . . ? C3 O3 C2 114.9(3) . . ? O2 C1 O1 125.3(5) . . ? O2 C1 C2 120.9(4) . . ? O1 C1 C2 113.8(4) . . ? O3 C2 C1 109.9(4) . . ? C34 N3 C38 119.9(4) . . ? C34 N3 Hg1 120.8(3) . . ? C38 N3 Hg1 119.2(3) . . ? C15 C16 C17 122.7(5) . . ? C15 C16 N1 118.6(6) . . ? C17 C16 N1 118.8(5) . . ? C16 C15 C14 117.6(6) . . ? C15 C14 C13 120.9(6) . . ? C12 C13 C14 121.1(5) . . ? O7 C27 O8 125.2(5) . . ? O7 C27 C26 121.5(5) . . ? O8 C27 C26 113.3(4) . . ? N2 C28 C29 123.6(6) . . ? N2 C32 C31 123.1(7) . . ? C32 N2 C28 116.1(5) . . ? C32 N2 Hg1 121.2(4) . . ? C28 N2 Hg1 121.6(4) . . ? C36 C35 C34 116.8(5) . . ? C36 C35 C39 123.4(5) . . ? C34 C35 C39 119.8(6) . . ? C35 C36 C37 121.4(5) . . ? O5 N1 O4 122.4(7) . . ? O5 N1 C16 119.3(7) . . ? O4 N1 C16 118.3(6) . . ? C30 C29 C28 119.1(8) . . ? C30 C29 C33 119.2(7) . . ? C28 C29 C33 121.8(7) . . ? C30 C31 C32 118.0(7) . . ? C29 C30 C31 120.1(7) . . ? C27 O8 Hg1 108.5(3) . 7_556 ? C43 N4 C42 109.2(11) . . ? C43 N4 C41 148.9(12) . . ? C42 N4 C41 101.4(10) . . ? N4 C43 O9 88.1(17) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.609 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.190