# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Zhan Shi' _publ_contact_author_email zshi@mail.jlu.edu.cn loop_ _publ_author_name 'Zhan Shi' 'Baiyan Li' 'Fen Yang' 'Yiming Zhang' 'Gunaghua Li' 'Qi Zhou' 'Jia Hua' 'Shouhua Feng' data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 842364' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C28 H20 Mn N6 O8' _chemical_formula_sum 'C28 H20 Mn N6 O8' _chemical_formula_weight 623.44 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' Mn Mn 0.3368 0.7283 '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 15.259(3) _cell_length_b 13.521(3) _cell_length_c 27.133(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.08(3) _cell_angle_gamma 90.00 _cell_volume 5528.2(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4822 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 0.907 _exptl_absorpt_process_details Process-auto _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21509 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4822 _reflns_number_gt 3525 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0941P)^2^+9.7182P] 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 4822 _refine_ls_number_parameters 406 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1757 _refine_ls_wR_factor_gt 0.1637 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.061 _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 Mn1 Mn 0.97572(4) 0.06059(4) 0.56922(2) 0.0330(2) Uani 1 1 d . . . O1 O 0.9036(2) 0.1392(2) 0.50724(11) 0.0518(8) Uani 1 1 d . A . O2 O 0.99658(18) 0.0831(2) 0.45836(12) 0.0463(8) Uani 1 1 d . . . O3 O 0.48308(19) 0.3090(2) 0.12524(10) 0.0458(8) Uani 1 1 d . . . O4 O 0.52079(19) 0.4595(2) 0.15168(11) 0.0442(7) Uani 1 1 d . . . O5 O 0.9501(6) 0.2276(7) 0.2899(3) 0.0805(12) Uani 0.50 1 d PU A 1 O6 O 0.8242(7) 0.1481(7) 0.2472(4) 0.0805(12) Uani 0.50 1 d PU A 1 O5' O 0.9477(6) 0.1586(7) 0.2861(3) 0.0805(12) Uani 0.50 1 d PU A 2 O6' O 0.8287(7) 0.1929(7) 0.2460(4) 0.0805(12) Uani 0.50 1 d PU A 2 O7 O 0.6187(8) 0.0305(7) 0.2199(4) 0.061(3) Uani 0.40 1 d PU B 1 O7' O 0.5680(11) 0.0371(11) 0.2439(6) 0.089(4) Uani 0.30 1 d PU B 2 O7" O 0.6560(7) 0.0367(7) 0.2138(4) 0.035(2) Uani 0.30 1 d PU B 3 O8 O 0.6865(3) 0.0443(3) 0.29345(16) 0.0845(13) Uani 1 1 d . B . N1 N 0.8711(3) 0.1846(4) 0.28487(16) 0.0724(14) Uani 1 1 d . . . N2 N 0.6494(4) 0.0817(3) 0.25646(17) 0.0749(15) Uani 1 1 d . . . N3 N 1.1229(2) 0.1006(3) 0.56978(13) 0.0407(8) Uani 1 1 d . . . N4 N 1.2618(2) 0.1389(3) 0.60021(13) 0.0395(8) Uani 1 1 d . . . N5 N 1.8454(2) -0.0004(3) 0.58352(14) 0.0467(9) Uani 1 1 d . . . N6 N 1.7074(3) -0.0538(3) 0.57007(18) 0.0595(11) Uani 1 1 d . . . C1 C 0.7485(3) 0.2193(3) 0.33360(14) 0.0377(9) Uani 1 1 d . . . C2 C 0.8348(3) 0.1870(3) 0.33177(15) 0.0406(10) Uani 1 1 d . A . C3 C 0.8917(3) 0.1573(3) 0.37373(16) 0.0385(10) Uani 1 1 d . . . H3 H 0.9483 0.1347 0.3711 0.080 Uiso 1 1 calc . . . C4 C 0.8637(3) 0.1615(3) 0.41985(15) 0.0346(9) Uani 1 1 d . A . C5 C 0.7803(3) 0.1994(3) 0.42312(15) 0.0389(10) Uani 1 1 d . . . H5 H 0.7622 0.2060 0.4541 0.080 Uiso 1 1 calc . . . C6 C 0.7236(3) 0.2274(3) 0.38022(15) 0.0419(10) Uani 1 1 d . A . H6 H 0.6677 0.2522 0.3829 0.080 Uiso 1 1 calc . . . C7 C 0.9258(3) 0.1256(3) 0.46532(16) 0.0384(10) Uani 1 1 d . . . C8 C 0.6851(3) 0.2522(3) 0.28885(14) 0.0403(10) Uani 1 1 d . A . C9 C 0.6380(3) 0.1903(3) 0.25300(16) 0.0456(11) Uani 1 1 d . A . C10 C 0.5823(3) 0.2262(3) 0.21176(16) 0.0463(11) Uani 1 1 d . . . H10 H 0.5517 0.1827 0.1886 0.080 Uiso 1 1 calc . . . C11 C 0.5724(3) 0.3265(3) 0.20515(15) 0.0384(10) Uani 1 1 d . B . C12 C 0.6156(3) 0.3903(3) 0.24112(17) 0.0475(11) Uani 1 1 d . . . H12 H 0.6072 0.4582 0.2375 0.080 Uiso 1 1 calc . . . C13 C 0.6714(3) 0.3533(3) 0.28268(17) 0.0507(12) Uani 1 1 d . A . H13 H 0.6998 0.3968 0.3065 0.080 Uiso 1 1 calc . . . C14 C 0.5196(3) 0.3670(3) 0.15794(15) 0.0391(10) Uani 1 1 d . . . C15 C 1.1883(3) 0.0919(3) 0.60821(16) 0.0412(10) Uani 1 1 d . . . H15 H 1.1835 0.0572 0.6373 0.080 Uiso 1 1 calc . . . C16 C 1.1583(3) 0.1552(3) 0.53560(16) 0.0461(11) Uani 1 1 d . . . H16 H 1.1282 0.1733 0.5044 0.080 Uiso 1 1 calc . . . C17 C 1.2426(3) 0.1789(4) 0.55323(18) 0.0538(12) Uani 1 1 d . . . H17 H 1.2808 0.2155 0.5368 0.080 Uiso 1 1 calc . . . C18 C 1.3484(3) 0.1419(3) 0.63330(18) 0.0463(11) Uani 1 1 d . . . H18A H 1.3424 0.1134 0.6654 0.080 Uiso 1 1 calc . . . H18B H 1.3671 0.2101 0.6387 0.080 Uiso 1 1 calc . . . C19 C 1.4184(3) 0.0854(3) 0.61092(18) 0.0440(11) Uani 1 1 d . . . C20 C 1.4844(4) 0.1360(5) 0.5921(3) 0.0837(18) Uani 1 1 d U . . H20 H 1.4871 0.2045 0.5947 0.080 Uiso 1 1 calc . . . C21 C 1.5473(5) 0.0858(5) 0.5693(3) 0.0878(19) Uani 1 1 d U . . H21 H 1.5885 0.1209 0.5544 0.080 Uiso 1 1 calc . . . C22 C 1.5477(3) -0.0170(4) 0.5690(2) 0.0602(14) Uani 1 1 d . . . C23 C 1.4795(4) -0.0649(4) 0.5847(2) 0.0665(15) Uani 1 1 d . . . H23 H 1.4754 -0.1333 0.5815 0.080 Uiso 1 1 calc . . . C24 C 1.4155(4) -0.0136(4) 0.6056(2) 0.0669(15) Uani 1 1 d . . . H24 H 1.3693 -0.0486 0.6161 0.080 Uiso 1 1 calc . . . C25 C 1.6164(3) -0.0719(5) 0.5452(3) 0.0763(18) Uani 1 1 d . . . H25A H 1.6042 -0.1423 0.5459 0.080 Uiso 1 1 calc . . . H25B H 1.6114 -0.0520 0.5105 0.080 Uiso 1 1 calc . . . C26 C 1.7693(3) -0.0019(4) 0.55205(19) 0.0515(12) Uani 1 1 d . . . H26 H 1.7605 0.0295 0.5212 0.080 Uiso 1 1 calc . . . C27 C 1.8300(3) -0.0556(4) 0.62382(19) 0.0524(12) Uani 1 1 d . . . H27 H 1.8714 -0.0683 0.6522 0.080 Uiso 1 1 calc . . . C28 C 1.7452(4) -0.0886(4) 0.6158(2) 0.0638(14) Uani 1 1 d . . . H28 H 1.7179 -0.1275 0.6372 0.080 Uiso 1 1 calc . . . 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 Mn1 0.0296(3) 0.0415(4) 0.0241(3) -0.0039(3) -0.0072(2) 0.0040(3) O1 0.0539(19) 0.067(2) 0.0286(17) 0.0028(15) -0.0110(14) 0.0166(16) O2 0.0343(16) 0.0458(17) 0.0510(19) -0.0056(14) -0.0166(14) 0.0118(13) O3 0.0441(17) 0.0566(18) 0.0312(16) 0.0074(14) -0.0112(13) -0.0101(14) O4 0.0434(17) 0.0501(19) 0.0349(17) 0.0087(13) -0.0061(13) 0.0067(14) O5 0.0807(13) 0.0816(13) 0.0796(13) 0.0001(5) 0.0135(5) 0.0002(5) O6 0.0807(13) 0.0816(13) 0.0796(13) 0.0001(5) 0.0135(5) 0.0002(5) O5' 0.0807(13) 0.0816(13) 0.0796(13) 0.0001(5) 0.0135(5) 0.0002(5) O6' 0.0807(13) 0.0816(13) 0.0796(13) 0.0001(5) 0.0135(5) 0.0002(5) O7 0.062(3) 0.061(3) 0.061(3) -0.0008(10) 0.0091(11) -0.0002(10) O7' 0.089(4) 0.088(4) 0.089(4) 0.0005(10) 0.0134(12) -0.0005(10) O7" 0.035(3) 0.035(3) 0.035(3) -0.0007(10) 0.0057(11) 0.0001(10) O8 0.115(3) 0.052(2) 0.072(3) 0.0143(19) -0.030(2) 0.004(2) N1 0.054(3) 0.118(4) 0.043(3) 0.008(3) 0.001(2) 0.009(3) N2 0.108(4) 0.045(2) 0.056(3) 0.006(2) -0.035(3) -0.007(2) N3 0.0324(18) 0.048(2) 0.040(2) -0.0011(16) -0.0005(16) -0.0009(16) N4 0.0305(18) 0.046(2) 0.039(2) 0.0054(16) -0.0040(15) 0.0009(15) N5 0.0351(19) 0.057(2) 0.045(2) -0.0100(19) -0.0023(17) 0.0004(17) N6 0.034(2) 0.068(3) 0.075(3) -0.020(2) 0.001(2) 0.0009(19) C1 0.041(2) 0.043(2) 0.025(2) 0.0042(17) -0.0075(17) 0.0046(19) C2 0.045(2) 0.049(2) 0.027(2) 0.0001(18) 0.0035(18) 0.004(2) C3 0.034(2) 0.043(2) 0.037(2) 0.0027(18) 0.0017(19) 0.0055(18) C4 0.037(2) 0.034(2) 0.029(2) -0.0003(16) -0.0088(17) 0.0043(17) C5 0.040(2) 0.049(2) 0.025(2) 0.0000(18) -0.0037(17) 0.0091(19) C6 0.035(2) 0.053(3) 0.035(2) 0.003(2) -0.0014(18) 0.013(2) C7 0.039(2) 0.035(2) 0.035(3) -0.0013(18) -0.0129(19) -0.0012(18) C8 0.044(2) 0.050(3) 0.024(2) 0.0068(18) -0.0049(18) 0.007(2) C9 0.054(3) 0.046(3) 0.031(2) 0.0098(19) -0.009(2) 0.001(2) C10 0.047(3) 0.053(3) 0.034(2) 0.004(2) -0.010(2) -0.007(2) C11 0.034(2) 0.052(3) 0.027(2) 0.0076(19) -0.0033(17) 0.0024(19) C12 0.054(3) 0.048(3) 0.036(2) 0.006(2) -0.008(2) 0.008(2) C13 0.057(3) 0.054(3) 0.035(3) 0.002(2) -0.013(2) 0.001(2) C14 0.030(2) 0.059(3) 0.027(2) 0.012(2) 0.0003(18) 0.004(2) C15 0.032(2) 0.049(2) 0.041(2) 0.000(2) 0.0012(19) -0.0011(19) C16 0.039(2) 0.060(3) 0.036(2) 0.008(2) -0.005(2) -0.006(2) C17 0.044(3) 0.064(3) 0.051(3) 0.015(2) -0.001(2) -0.011(2) C18 0.031(2) 0.055(3) 0.049(3) -0.006(2) -0.007(2) 0.000(2) C19 0.029(2) 0.046(3) 0.053(3) 0.002(2) -0.006(2) -0.0034(18) C20 0.082(2) 0.083(2) 0.087(2) -0.0022(10) 0.0145(10) -0.0010(10) C21 0.086(2) 0.088(2) 0.090(2) -0.0017(10) 0.0164(10) -0.0014(10) C22 0.027(2) 0.059(3) 0.090(4) -0.017(3) -0.004(2) 0.000(2) C23 0.071(4) 0.040(3) 0.092(4) 0.003(3) 0.023(3) -0.002(3) C24 0.067(3) 0.049(3) 0.091(4) 0.000(3) 0.032(3) -0.009(3) C25 0.031(3) 0.088(4) 0.106(5) -0.033(4) -0.003(3) 0.002(3) C26 0.035(2) 0.061(3) 0.056(3) -0.007(2) -0.002(2) 0.004(2) C27 0.042(3) 0.067(3) 0.047(3) -0.006(2) 0.004(2) -0.002(2) C28 0.053(3) 0.064(3) 0.079(4) -0.007(3) 0.024(3) -0.008(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 Mn1 O1 2.142(3) . ? Mn1 O2 2.148(3) 5_756 ? Mn1 N5 2.243(4) 1_455 ? Mn1 O4 2.251(3) 8_556 ? Mn1 N3 2.307(3) . ? Mn1 O3 2.320(3) 8_556 ? Mn1 C14 2.587(4) 8_556 ? O1 C7 1.251(5) . ? O2 C7 1.264(5) . ? O2 Mn1 2.148(3) 5_756 ? O3 C14 1.248(5) . ? O3 Mn1 2.320(3) 8_455 ? O4 C14 1.264(5) . ? O4 Mn1 2.251(3) 8_455 ? O5 N1 1.325(9) . ? O6 N1 1.253(11) . ? O5' N1 1.216(9) . ? O6' N1 1.153(11) . ? O7 N2 1.238(11) . ? O7' N2 1.375(16) . ? O7" N2 1.324(11) . ? O8 N2 1.185(5) . ? N1 C2 1.466(6) . ? N2 C9 1.481(6) . ? N3 C15 1.331(5) . ? N3 C16 1.362(6) . ? N4 C15 1.336(5) . ? N4 C17 1.373(6) . ? N4 C18 1.477(5) . ? N5 C26 1.328(5) . ? N5 C27 1.374(6) . ? N5 Mn1 2.243(4) 1_655 ? N6 C26 1.331(6) . ? N6 C28 1.366(7) . ? N6 C25 1.466(6) . ? C1 C6 1.382(6) . ? C1 C2 1.395(6) . ? C1 C8 1.496(5) . ? C2 C3 1.378(6) . ? C3 C4 1.386(6) . ? C3 H3 0.9300 . ? C4 C5 1.388(6) . ? C4 C7 1.512(5) . ? C5 C6 1.389(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.389(6) . ? C8 C9 1.393(6) . ? C9 C10 1.382(6) . ? C10 C11 1.373(6) . ? C10 H10 0.9300 . ? C11 C12 1.388(6) . ? C11 C14 1.505(5) . ? C12 C13 1.395(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 Mn1 2.587(4) 8_455 ? C15 H15 0.9300 . ? C16 C17 1.339(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.516(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.346(7) . ? C19 C20 1.380(8) . ? C20 C21 1.398(9) . ? C20 H20 0.9300 . ? C21 C22 1.390(8) . ? C21 H21 0.9300 . ? C22 C23 1.350(7) . ? C22 C25 1.512(7) . ? C23 C24 1.390(7) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26 0.9300 . ? C27 C28 1.354(7) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 106.30(12) . 5_756 ? O1 Mn1 N5 87.62(14) . 1_455 ? O2 Mn1 N5 87.48(13) 5_756 1_455 ? O1 Mn1 O4 151.53(12) . 8_556 ? O2 Mn1 O4 101.00(11) 5_756 8_556 ? N5 Mn1 O4 85.63(13) 1_455 8_556 ? O1 Mn1 N3 105.55(13) . . ? O2 Mn1 N3 88.26(12) 5_756 . ? N5 Mn1 N3 166.82(14) 1_455 . ? O4 Mn1 N3 82.96(12) 8_556 . ? O1 Mn1 O3 95.89(12) . 8_556 ? O2 Mn1 O3 157.57(11) 5_756 8_556 ? N5 Mn1 O3 96.84(12) 1_455 8_556 ? O4 Mn1 O3 57.66(11) 8_556 8_556 ? N3 Mn1 O3 82.58(12) . 8_556 ? O1 Mn1 C14 124.62(14) . 8_556 ? O2 Mn1 C14 129.08(13) 5_756 8_556 ? N5 Mn1 C14 94.86(13) 1_455 8_556 ? O4 Mn1 C14 29.24(12) 8_556 8_556 ? N3 Mn1 C14 78.26(13) . 8_556 ? O3 Mn1 C14 28.80(12) 8_556 8_556 ? C7 O1 Mn1 117.5(3) . . ? C7 O2 Mn1 133.1(3) . 5_756 ? C14 O3 Mn1 87.6(2) . 8_455 ? C14 O4 Mn1 90.3(2) . 8_455 ? O6' N1 O5' 116.8(7) . . ? O6' N1 O6 29.1(6) . . ? O5' N1 O6 109.4(7) . . ? O6' N1 O5 115.0(7) . . ? O5' N1 O5 43.1(5) . . ? O6 N1 O5 130.6(7) . . ? O6' N1 C2 123.9(6) . . ? O5' N1 C2 118.5(6) . . ? O6 N1 C2 118.1(6) . . ? O5 N1 C2 111.3(5) . . ? O8 N2 O7 120.6(6) . . ? O8 N2 O7" 116.9(6) . . ? O7 N2 O7" 27.8(6) . . ? O8 N2 O7' 108.3(8) . . ? O7 N2 O7' 49.0(7) . . ? O7" N2 O7' 76.8(8) . . ? O8 N2 C9 120.8(4) . . ? O7 N2 C9 118.5(6) . . ? O7" N2 C9 115.1(6) . . ? O7' N2 C9 109.1(7) . . ? C15 N3 C16 104.6(3) . . ? C15 N3 Mn1 126.4(3) . . ? C16 N3 Mn1 127.8(3) . . ? C15 N4 C17 106.1(3) . . ? C15 N4 C18 127.4(4) . . ? C17 N4 C18 126.4(4) . . ? C26 N5 C27 105.2(4) . . ? C26 N5 Mn1 127.1(3) . 1_655 ? C27 N5 Mn1 127.2(3) . 1_655 ? C26 N6 C28 107.0(4) . . ? C26 N6 C25 126.5(5) . . ? C28 N6 C25 126.5(5) . . ? C6 C1 C2 117.1(3) . . ? C6 C1 C8 118.9(4) . . ? C2 C1 C8 123.9(4) . . ? C3 C2 C1 122.5(4) . . ? C3 C2 N1 115.8(4) . . ? C1 C2 N1 121.7(4) . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.3(3) . . ? C3 C4 C7 118.7(4) . . ? C5 C4 C7 122.0(4) . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 121.4(4) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? O1 C7 O2 124.3(4) . . ? O1 C7 C4 118.0(4) . . ? O2 C7 C4 117.7(4) . . ? C13 C8 C9 117.1(4) . . ? C13 C8 C1 117.1(4) . . ? C9 C8 C1 125.8(4) . . ? C10 C9 C8 122.6(4) . . ? C10 C9 N2 116.8(4) . . ? C8 C9 N2 120.6(4) . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 119.4(4) . . ? C10 C11 C14 120.2(4) . . ? C12 C11 C14 120.2(4) . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C8 C13 C12 120.8(4) . . ? C8 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? O3 C14 O4 122.8(4) . . ? O3 C14 C11 119.7(4) . . ? O4 C14 C11 117.2(4) . . ? O3 C14 Mn1 63.6(2) . 8_455 ? O4 C14 Mn1 60.5(2) . 8_455 ? C11 C14 Mn1 162.7(3) . 8_455 ? N3 C15 N4 112.1(4) . . ? N3 C15 H15 124.0 . . ? N4 C15 H15 124.0 . . ? C17 C16 N3 110.4(4) . . ? C17 C16 H16 124.8 . . ? N3 C16 H16 124.8 . . ? C16 C17 N4 106.8(4) . . ? C16 C17 H17 126.6 . . ? N4 C17 H17 126.6 . . ? N4 C18 C19 111.2(4) . . ? N4 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? N4 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C24 C19 C20 117.8(5) . . ? C24 C19 C18 122.1(4) . . ? C20 C19 C18 120.0(4) . . ? C19 C20 C21 121.1(6) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 119.4(6) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 118.4(5) . . ? C23 C22 C25 121.3(5) . . ? C21 C22 C25 119.8(5) . . ? C22 C23 C24 121.0(5) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C19 C24 C23 121.8(5) . . ? C19 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? N6 C25 C22 113.0(5) . . ? N6 C25 H25A 109.0 . . ? C22 C25 H25A 109.0 . . ? N6 C25 H25B 109.0 . . ? C22 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? N5 C26 N6 111.8(5) . . ? N5 C26 H26 124.1 . . ? N6 C26 H26 124.1 . . ? C28 C27 N5 109.2(5) . . ? C28 C27 H27 125.4 . . ? N5 C27 H27 125.4 . . ? C27 C28 N6 106.8(5) . . ? C27 C28 H28 126.6 . . ? N6 C28 H28 126.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.077 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.073 #=========================END data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 842365' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C28 H20 N6 O8 Zn' _chemical_formula_sum 'C28 H20 N6 O8 Zn' _chemical_formula_weight 633.87 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' Zn Zn 0.2839 1.4301 '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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.549(3) _cell_length_b 12.607(3) _cell_length_c 24.921(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5514(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4852 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 0.954 _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 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 39640 _diffrn_reflns_av_R_equivalents 0.1137 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4852 _reflns_number_gt 3051 _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 SHELXP-97 _computing_publication_material 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^)+(0.1027P)^2^+4.3118P] 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 4852 _refine_ls_number_parameters 388 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1950 _refine_ls_wR_factor_gt 0.1788 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.059 _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 Zn1 Zn 0.23895(4) 0.34541(5) 0.10672(2) 0.0432(3) Uani 1 1 d . . . O1 O 0.2311(2) 0.2505(3) 0.16904(15) 0.0539(10) Uani 1 1 d . . . O2 O 0.2820(3) 0.3826(4) 0.21490(16) 0.0793(15) Uani 1 1 d . . . O3 O 0.2938(3) -0.2656(3) 0.54123(16) 0.0574(11) Uani 1 1 d . . . O4 O 0.1832(3) -0.1932(3) 0.56226(17) 0.0731(14) Uani 1 1 d . . . O5 O 0.3841(3) 0.2978(4) 0.39255(17) 0.0683(12) Uani 1 1 d . . . O6 O 0.3804(3) 0.1379(4) 0.42134(19) 0.0870(17) Uani 1 1 d . . . O7 O 0.3613(3) -0.0649(4) 0.3192(2) 0.0990(17) Uani 1 1 d U . . O8 O 0.4105(5) -0.1683(7) 0.3736(3) 0.147(3) Uani 1 1 d U . . N1 N 0.3605(3) 0.2068(5) 0.39021(18) 0.0546(13) Uani 1 1 d . . . N2 N 0.3634(4) -0.1030(5) 0.3632(2) 0.0786(19) Uani 1 1 d . . . N3 N 0.1477(3) 0.4440(4) 0.11496(17) 0.0479(12) Uani 1 1 d . . . N4 N 0.0769(3) 0.5803(4) 0.13875(19) 0.0534(13) Uani 1 1 d . . . N5 N -0.1702(3) 0.4360(4) 0.40759(17) 0.0460(12) Uani 1 1 d . . . N6 N -0.0906(3) 0.5699(4) 0.40034(18) 0.0477(12) Uani 1 1 d . . . C1 C 0.2626(3) 0.0869(4) 0.3505(2) 0.0455(14) Uani 1 1 d . . . C2 C 0.3071(3) 0.1787(4) 0.3474(2) 0.0419(13) Uani 1 1 d . . . C3 C 0.3037(3) 0.2458(4) 0.3038(2) 0.0464(14) Uani 1 1 d . . . H3 H 0.3334 0.3069 0.3032 0.080 Uiso 1 1 calc . . . C4 C 0.2561(3) 0.2228(4) 0.2609(2) 0.0453(14) Uani 1 1 d . . . C5 C 0.2097(4) 0.1333(5) 0.2643(2) 0.0597(17) Uani 1 1 d . . . H5 H 0.1763 0.1176 0.2365 0.080 Uiso 1 1 calc . . . C6 C 0.2127(4) 0.0681(5) 0.3084(2) 0.0593(17) Uani 1 1 d . . . H6 H 0.1805 0.0096 0.3100 0.080 Uiso 1 1 calc . . . C7 C 0.2570(4) 0.2929(5) 0.2121(2) 0.0499(15) Uani 1 1 d . . . C8 C 0.2622(3) 0.0115(5) 0.3975(2) 0.0470(14) Uani 1 1 d . . . C9 C 0.3078(3) -0.0778(5) 0.4031(2) 0.0478(14) Uani 1 1 d . . . C10 C 0.3032(3) -0.1446(4) 0.4475(2) 0.0508(15) Uani 1 1 d . . . H10 H 0.3364 -0.2017 0.4509 0.080 Uiso 1 1 calc . . . C11 C 0.2495(3) -0.1254(4) 0.4859(2) 0.0450(14) Uani 1 1 d . . . C12 C 0.2028(4) -0.0389(5) 0.4810(2) 0.0626(17) Uani 1 1 d . . . H12 H 0.1670 -0.0252 0.5076 0.080 Uiso 1 1 calc . . . C13 C 0.2077(4) 0.0286(5) 0.4376(2) 0.0563(16) Uani 1 1 d . . . H13 H 0.1746 0.0859 0.4349 0.080 Uiso 1 1 calc . . . C14 C 0.2411(4) -0.2003(5) 0.5341(2) 0.0559(16) Uani 1 1 d . . . C15 C 0.1423(3) 0.5288(5) 0.1461(2) 0.0507(15) Uani 1 1 d . . . H15 H 0.1798 0.5498 0.1703 0.080 Uiso 1 1 calc . . . C16 C 0.0806(4) 0.4424(5) 0.0868(3) 0.0612(17) Uani 1 1 d . . . H16 H 0.0671 0.3915 0.0615 0.080 Uiso 1 1 calc . . . C17 C 0.0367(4) 0.5264(6) 0.1012(3) 0.0695(19) Uani 1 1 d . . . H17 H -0.0113 0.5434 0.0880 0.080 Uiso 1 1 calc . . . C18 C 0.0561(4) 0.6811(5) 0.1639(3) 0.070(2) Uani 1 1 d . . . H18A H 0.0177 0.7153 0.1419 0.080 Uiso 1 1 calc . . . H18B H 0.1006 0.7267 0.1641 0.080 Uiso 1 1 calc . . . C19 C 0.0262(3) 0.6729(4) 0.2203(2) 0.0510(15) Uani 1 1 d . . . C20 C 0.0175(5) 0.5797(5) 0.2476(3) 0.074(2) Uani 1 1 d . . . H20 H 0.0307 0.5162 0.2310 0.080 Uiso 1 1 calc . . . C21 C -0.0107(4) 0.5777(5) 0.2998(3) 0.072(2) Uani 1 1 d . . . H21 H -0.0158 0.5132 0.3175 0.080 Uiso 1 1 calc . . . C22 C -0.0309(3) 0.6680(4) 0.3251(2) 0.0443(13) Uani 1 1 d . . . C23 C -0.0227(4) 0.7623(5) 0.2978(2) 0.0616(18) Uani 1 1 d . . . H23 H -0.0360 0.8257 0.3144 0.080 Uiso 1 1 calc . . . C24 C 0.0050(4) 0.7636(5) 0.2459(3) 0.0681(19) Uani 1 1 d . . . H24 H 0.0093 0.8281 0.2280 0.080 Uiso 1 1 calc . . . C25 C -0.0603(4) 0.6706(5) 0.3819(2) 0.0542(16) Uani 1 1 d . . . H25A H -0.0191 0.6919 0.4055 0.080 Uiso 1 1 calc . . . H25B H -0.1000 0.7239 0.3844 0.080 Uiso 1 1 calc . . . C26 C -0.1585(4) 0.5297(5) 0.3862(2) 0.0505(15) Uani 1 1 d . . . H26 H -0.1931 0.5640 0.3639 0.080 Uiso 1 1 calc . . . C27 C -0.1064(4) 0.4155(6) 0.4368(3) 0.073(2) Uani 1 1 d . . . H27 H -0.0982 0.3543 0.4568 0.080 Uiso 1 1 calc . . . C28 C -0.0568(4) 0.4966(6) 0.4327(3) 0.077(2) Uani 1 1 d . . . H28 H -0.0090 0.5016 0.4487 0.080 Uiso 1 1 calc . . . 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 Zn1 0.0632(5) 0.0350(4) 0.0315(4) -0.0006(3) 0.0013(3) 0.0007(3) O1 0.080(3) 0.049(2) 0.032(2) 0.0054(18) 0.000(2) -0.003(2) O2 0.151(5) 0.043(3) 0.045(3) 0.009(2) -0.002(3) -0.020(3) O3 0.074(3) 0.048(3) 0.050(2) 0.010(2) -0.010(2) -0.001(2) O4 0.112(4) 0.058(3) 0.049(3) 0.010(2) 0.020(3) 0.007(3) O5 0.082(3) 0.061(3) 0.062(3) -0.012(2) -0.011(2) -0.009(3) O6 0.093(4) 0.105(4) 0.063(3) 0.040(3) -0.031(3) -0.032(3) O7 0.1002(19) 0.0989(19) 0.0979(19) 0.0018(10) 0.0041(10) 0.0031(10) O8 0.147(3) 0.148(3) 0.146(3) 0.0024(10) 0.0024(10) 0.0039(10) N1 0.060(3) 0.065(4) 0.039(3) 0.010(3) 0.004(2) -0.006(3) N2 0.090(5) 0.078(4) 0.068(4) 0.028(3) 0.016(3) 0.032(4) N3 0.065(3) 0.041(3) 0.038(3) -0.002(2) 0.003(2) 0.005(2) N4 0.063(4) 0.050(3) 0.047(3) 0.007(2) 0.013(3) 0.009(3) N5 0.067(3) 0.038(3) 0.033(2) 0.002(2) -0.001(2) -0.004(2) N6 0.052(3) 0.045(3) 0.046(3) 0.001(2) -0.002(2) -0.003(2) C1 0.054(4) 0.044(3) 0.038(3) 0.005(3) 0.002(3) 0.002(3) C2 0.059(4) 0.038(3) 0.029(3) -0.002(2) 0.000(3) 0.001(3) C3 0.065(4) 0.036(3) 0.038(3) -0.001(3) 0.009(3) -0.002(3) C4 0.062(4) 0.038(3) 0.036(3) -0.001(2) 0.007(3) 0.005(3) C5 0.091(5) 0.051(4) 0.037(3) 0.006(3) -0.013(3) -0.010(3) C6 0.082(5) 0.049(4) 0.046(3) 0.009(3) -0.002(3) -0.014(3) C7 0.074(4) 0.042(4) 0.034(3) 0.003(3) 0.004(3) 0.005(3) C8 0.062(4) 0.042(3) 0.037(3) 0.004(3) 0.001(3) 0.001(3) C9 0.056(4) 0.049(4) 0.039(3) -0.001(3) 0.003(3) 0.008(3) C10 0.062(4) 0.041(3) 0.050(3) 0.002(3) -0.007(3) 0.003(3) C11 0.061(4) 0.039(3) 0.035(3) -0.003(2) 0.003(3) 0.000(3) C12 0.083(5) 0.060(4) 0.045(4) -0.002(3) 0.017(3) 0.003(4) C13 0.085(5) 0.048(4) 0.035(3) 0.005(3) 0.010(3) 0.008(3) C14 0.081(5) 0.048(4) 0.038(3) -0.006(3) 0.005(3) -0.012(4) C15 0.052(4) 0.053(4) 0.047(3) -0.005(3) 0.001(3) 0.007(3) C16 0.075(5) 0.055(4) 0.054(4) 0.000(3) -0.005(3) 0.002(4) C17 0.061(4) 0.080(5) 0.068(5) 0.017(4) -0.009(4) 0.006(4) C18 0.084(5) 0.053(4) 0.071(4) 0.009(3) 0.026(4) 0.026(3) C19 0.055(4) 0.040(4) 0.059(4) 0.004(3) 0.011(3) 0.008(3) C20 0.109(6) 0.044(4) 0.069(5) -0.002(3) 0.041(4) 0.008(4) C21 0.105(6) 0.035(4) 0.075(5) 0.007(3) 0.034(4) 0.003(4) C22 0.046(3) 0.038(3) 0.049(3) -0.006(3) 0.001(3) 0.001(3) C23 0.096(5) 0.036(3) 0.052(4) -0.010(3) 0.007(4) 0.007(3) C24 0.109(6) 0.039(4) 0.056(4) 0.006(3) 0.007(4) 0.009(4) C25 0.059(4) 0.044(4) 0.060(4) -0.003(3) -0.001(3) -0.007(3) C26 0.060(4) 0.045(4) 0.046(3) 0.006(3) -0.007(3) -0.001(3) C27 0.078(5) 0.065(5) 0.077(5) 0.031(4) -0.027(4) -0.008(4) C28 0.074(5) 0.071(5) 0.085(5) 0.020(4) -0.030(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.965(4) . ? Zn1 N5 1.993(5) 6_656 ? Zn1 O3 2.001(4) 2_554 ? Zn1 N3 2.038(5) . ? Zn1 C14 2.597(7) 2_554 ? O1 C7 1.282(7) . ? O2 C7 1.215(7) . ? O3 C14 1.250(8) . ? O3 Zn1 2.001(4) 2 ? O4 C14 1.239(7) . ? O5 N1 1.221(6) . ? O6 N1 1.216(6) . ? O7 N2 1.198(7) . ? O8 N2 1.195(9) . ? N1 C2 1.464(7) . ? N2 C9 1.428(8) . ? N3 C15 1.324(7) . ? N3 C16 1.371(8) . ? N4 C15 1.332(7) . ? N4 C17 1.354(8) . ? N4 C18 1.463(8) . ? N5 C26 1.312(7) . ? N5 C27 1.361(8) . ? N5 Zn1 1.993(5) 6_556 ? N6 C26 1.342(7) . ? N6 C28 1.362(8) . ? N6 C25 1.451(7) . ? C1 C6 1.388(8) . ? C1 C2 1.399(7) . ? C1 C8 1.508(7) . ? C2 C3 1.378(7) . ? C3 C4 1.387(8) . ? C3 H3 0.9300 . ? C4 C5 1.394(8) . ? C4 C7 1.503(7) . ? C5 C6 1.373(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.388(8) . ? C8 C13 1.399(8) . ? C9 C10 1.392(8) . ? C10 C11 1.367(8) . ? C10 H10 0.9300 . ? C11 C12 1.370(8) . ? C11 C14 1.534(8) . ? C12 C13 1.379(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 Zn1 2.597(7) 2 ? C15 H15 0.9300 . ? C16 C17 1.357(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.505(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.360(8) . ? C19 C20 1.367(8) . ? C20 C21 1.392(8) . ? C20 H20 0.9300 . ? C21 C22 1.347(8) . ? C21 H21 0.9300 . ? C22 C23 1.378(8) . ? C22 C25 1.506(8) . ? C23 C24 1.382(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26 0.9300 . ? C27 C28 1.347(9) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N5 123.10(17) . 6_656 ? O1 Zn1 O3 108.57(17) . 2_554 ? N5 Zn1 O3 111.81(17) 6_656 2_554 ? O1 Zn1 N3 103.70(17) . . ? N5 Zn1 N3 107.3(2) 6_656 . ? O3 Zn1 N3 99.39(18) 2_554 . ? O1 Zn1 C14 97.54(18) . 2_554 ? N5 Zn1 C14 99.85(19) 6_656 2_554 ? O3 Zn1 C14 27.91(18) 2_554 2_554 ? N3 Zn1 C14 127.3(2) . 2_554 ? C7 O1 Zn1 112.5(4) . . ? C14 O3 Zn1 103.6(4) . 2 ? O6 N1 O5 122.9(5) . . ? O6 N1 C2 118.4(5) . . ? O5 N1 C2 118.6(5) . . ? O8 N2 O7 119.6(7) . . ? O8 N2 C9 118.4(6) . . ? O7 N2 C9 121.9(6) . . ? C15 N3 C16 104.5(5) . . ? C15 N3 Zn1 127.4(4) . . ? C16 N3 Zn1 127.9(4) . . ? C15 N4 C17 107.4(5) . . ? C15 N4 C18 125.4(6) . . ? C17 N4 C18 127.0(6) . . ? C26 N5 C27 105.0(5) . . ? C26 N5 Zn1 124.7(4) . 6_556 ? C27 N5 Zn1 130.2(4) . 6_556 ? C26 N6 C28 106.6(5) . . ? C26 N6 C25 125.0(5) . . ? C28 N6 C25 128.4(5) . . ? C6 C1 C2 116.8(5) . . ? C6 C1 C8 118.5(5) . . ? C2 C1 C8 124.5(5) . . ? C3 C2 C1 121.8(5) . . ? C3 C2 N1 117.0(5) . . ? C1 C2 N1 121.1(5) . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 118.3(5) . . ? C3 C4 C7 119.6(5) . . ? C5 C4 C7 122.1(5) . . ? C6 C5 C4 120.8(6) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 121.8(6) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? O2 C7 O1 124.3(5) . . ? O2 C7 C4 120.3(5) . . ? O1 C7 C4 115.4(5) . . ? C9 C8 C13 116.6(5) . . ? C9 C8 C1 125.9(5) . . ? C13 C8 C1 117.4(5) . . ? C8 C9 C10 122.5(5) . . ? C8 C9 N2 120.3(5) . . ? C10 C9 N2 117.2(5) . . ? C11 C10 C9 119.4(5) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.3(5) . . ? C10 C11 C14 120.4(5) . . ? C12 C11 C14 120.3(5) . . ? C11 C12 C13 121.7(6) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C8 120.5(6) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? O4 C14 O3 125.0(6) . . ? O4 C14 C11 118.5(6) . . ? O3 C14 C11 116.5(6) . . ? O4 C14 Zn1 76.5(4) . 2 ? O3 C14 Zn1 48.5(3) . 2 ? C11 C14 Zn1 165.0(5) . 2 ? N3 C15 N4 112.0(5) . . ? N3 C15 H15 124.0 . . ? N4 C15 H15 124.0 . . ? C17 C16 N3 109.8(6) . . ? C17 C16 H16 125.1 . . ? N3 C16 H16 125.1 . . ? N4 C17 C16 106.3(6) . . ? N4 C17 H17 126.9 . . ? C16 C17 H17 126.9 . . ? N4 C18 C19 115.3(5) . . ? N4 C18 H18A 108.5 . . ? C19 C18 H18A 108.5 . . ? N4 C18 H18B 108.5 . . ? C19 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C24 C19 C20 117.4(6) . . ? C24 C19 C18 118.3(5) . . ? C20 C19 C18 124.3(5) . . ? C19 C20 C21 121.3(6) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 121.0(6) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 118.0(5) . . ? C21 C22 C25 123.2(5) . . ? C23 C22 C25 118.7(5) . . ? C22 C23 C24 120.7(5) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C19 C24 C23 121.6(6) . . ? C19 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? N6 C25 C22 113.8(5) . . ? N6 C25 H25A 108.8 . . ? C22 C25 H25A 108.8 . . ? N6 C25 H25B 108.8 . . ? C22 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N5 C26 N6 111.9(5) . . ? N5 C26 H26 124.1 . . ? N6 C26 H26 124.1 . . ? C28 C27 N5 110.3(5) . . ? C28 C27 H27 124.9 . . ? N5 C27 H27 124.9 . . ? C27 C28 N6 106.2(6) . . ? C27 C28 H28 126.9 . . ? N6 C28 H28 126.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.123 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.079 #=========================END data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 842366' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C28 H20 Cd N6 O8' _chemical_formula_sum 'C28 H20 Cd N6 O8' _chemical_formula_weight 680.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.197(3) _cell_length_b 13.474(3) _cell_length_c 27.769(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.51(3) _cell_angle_gamma 90.00 _cell_volume 5607.9(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4887 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details Process-auto _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21551 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4887 _reflns_number_gt 3514 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0569P)^2^+42.6519P] 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 4887 _refine_ls_number_parameters 400 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.02003(3) 0.55992(4) 0.432927(15) 0.03253(17) Uani 1 1 d . . . O1 O -0.0123(3) 0.4059(4) 0.46764(18) 0.0524(14) Uani 1 1 d . A . O2 O -0.1123(4) 0.3484(5) 0.51005(17) 0.0622(16) Uani 1 1 d . . . O3 O -0.5091(3) 0.1874(4) 0.12851(15) 0.0453(12) Uani 1 1 d . . . O4 O -0.4693(3) 0.0345(4) 0.15346(16) 0.0410(11) Uani 1 1 d . . . O5 O -0.0420(8) 0.3252(10) 0.2982(4) 0.055(3) Uani 0.50 1 d PU A 1 O5' O -0.0429(9) 0.2779(11) 0.2989(5) 0.066(4) Uani 0.50 1 d PU A 2 O6 O -0.1679(4) 0.3350(6) 0.2542(2) 0.089(2) Uani 1 1 d . A . O7 O -0.3512(7) 0.4616(7) 0.2178(4) 0.082(3) Uani 0.70 1 d PU B 1 O7' O -0.4092(16) 0.4625(17) 0.2329(9) 0.082(3) Uani 0.30 1 d PU B 2 O8 O -0.3157(4) 0.4519(4) 0.2959(2) 0.0726(18) Uani 1 1 d . B . N1 N -0.1225(5) 0.3158(6) 0.2929(2) 0.0582(18) Uani 1 1 d . . . N2 N -0.3467(6) 0.4132(5) 0.2591(3) 0.080(3) Uani 1 1 d . . . N3 N -0.1307(4) 0.5981(4) 0.4302(2) 0.0382(13) Uani 1 1 d . . . N4 N -0.2684(3) 0.6377(4) 0.3997(2) 0.0379(13) Uani 1 1 d . . . N5 N -0.8508(4) 0.4889(5) 0.4171(2) 0.0483(16) Uani 1 1 d . . . N6 N -0.7115(4) 0.4388(6) 0.4287(3) 0.069(2) Uani 1 1 d . . . C1 C -0.2511(4) 0.2768(5) 0.3358(2) 0.0373(16) Uani 1 1 d . . . C2 C -0.1637(4) 0.3100(5) 0.3373(2) 0.0366(16) Uani 1 1 d . A . C3 C -0.1111(4) 0.3379(5) 0.3805(2) 0.0377(16) Uani 1 1 d . . . H3 H -0.0535 0.3612 0.3802 0.080 Uiso 1 1 calc . . . C4 C -0.1430(4) 0.3314(5) 0.4241(2) 0.0330(15) Uani 1 1 d . A . C5 C -0.2276(4) 0.2934(5) 0.4241(2) 0.0383(17) Uani 1 1 d . . . H5 H -0.2488 0.2853 0.4534 0.080 Uiso 1 1 calc . . . C6 C -0.2813(4) 0.2672(5) 0.3800(2) 0.0389(17) Uani 1 1 d . A . H6 H -0.3385 0.2429 0.3804 0.080 Uiso 1 1 calc . . . C7 C -0.0854(5) 0.3641(5) 0.4703(3) 0.0432(18) Uani 1 1 d . . . C8 C -0.3116(4) 0.2437(5) 0.2906(2) 0.0380(16) Uani 1 1 d . A . C9 C -0.3577(5) 0.3054(5) 0.2546(2) 0.0443(18) Uani 1 1 d . A . C10 C -0.4118(5) 0.2682(5) 0.2136(2) 0.0432(18) Uani 1 1 d . . . H10 H -0.4415 0.3115 0.1903 0.080 Uiso 1 1 calc . . . C11 C -0.4217(4) 0.1671(5) 0.2072(2) 0.0359(16) Uani 1 1 d . B . C12 C -0.3790(5) 0.1037(5) 0.2427(2) 0.0463(18) Uani 1 1 d . . . H12 H -0.3865 0.0355 0.2391 0.080 Uiso 1 1 calc . . . C13 C -0.3244(5) 0.1424(6) 0.2839(3) 0.0489(19) Uani 1 1 d . A . H13 H -0.2959 0.0989 0.3074 0.080 Uiso 1 1 calc . . . C14 C -0.4725(4) 0.1269(6) 0.1601(2) 0.0371(16) Uani 1 1 d . . . C15 C -0.1946(4) 0.5903(6) 0.3925(2) 0.0410(17) Uani 1 1 d . . . H15 H -0.1892 0.5559 0.3641 0.080 Uiso 1 1 calc . . . C16 C -0.1643(5) 0.6533(6) 0.4637(2) 0.0454(18) Uani 1 1 d . . . H16 H -0.1337 0.6716 0.4943 0.080 Uiso 1 1 calc . . . C17 C -0.2497(5) 0.6774(6) 0.4454(3) 0.054(2) Uani 1 1 d . . . H17 H -0.2884 0.7142 0.4611 0.080 Uiso 1 1 calc . . . C18 C -0.3559(4) 0.6398(6) 0.3669(3) 0.0463(18) Uani 1 1 d . . . H18A H -0.3495 0.6119 0.3355 0.080 Uiso 1 1 calc . . . H18B H -0.3757 0.7079 0.3618 0.080 Uiso 1 1 calc . . . C19 C -0.4245(4) 0.5815(5) 0.3883(3) 0.0425(17) Uani 1 1 d . . . C20 C -0.4882(8) 0.6302(9) 0.4082(4) 0.093(3) Uani 1 1 d U . . H20 H -0.4913 0.6990 0.4058 0.080 Uiso 1 1 calc . . . C21 C -0.5498(8) 0.5800(10) 0.4323(4) 0.102(4) Uani 1 1 d U . . H21 H -0.5874 0.6144 0.4497 0.080 Uiso 1 1 calc . . . C22 C -0.5523(5) 0.4751(6) 0.4290(4) 0.071(3) Uani 1 1 d . . . C23 C -0.4844(7) 0.4300(6) 0.4137(4) 0.074(3) Uani 1 1 d . . . H23 H -0.4791 0.3614 0.4165 0.080 Uiso 1 1 calc . . . C24 C -0.4218(7) 0.4822(7) 0.3936(4) 0.079(3) Uani 1 1 d . . . H24 H -0.3755 0.4474 0.3831 0.080 Uiso 1 1 calc . . . C25 C -0.6198(7) 0.4210(8) 0.4536(4) 0.079(3) Uani 1 1 d U . . H25A H -0.6074 0.3504 0.4537 0.080 Uiso 1 1 calc . . . H25B H -0.6141 0.4429 0.4873 0.080 Uiso 1 1 calc . . . C26 C -0.7731(5) 0.4868(7) 0.4476(3) 0.056(2) Uani 1 1 d . . . H26 H -0.7636 0.5157 0.4784 0.080 Uiso 1 1 calc . . . C27 C -0.8365(5) 0.4358(7) 0.3767(3) 0.058(2) Uani 1 1 d . . . H27 H -0.8786 0.4228 0.3491 0.080 Uiso 1 1 calc . . . C28 C -0.7493(6) 0.4054(7) 0.3844(4) 0.073(3) Uani 1 1 d . . . H28 H -0.7214 0.3686 0.3629 0.080 Uiso 1 1 calc . . . 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 0.0268(3) 0.0437(3) 0.0232(2) 0.0050(2) -0.00735(17) -0.0050(2) O1 0.041(3) 0.050(3) 0.055(3) 0.009(3) -0.024(2) -0.016(2) O2 0.060(3) 0.093(5) 0.028(3) -0.004(3) -0.007(2) -0.018(3) O3 0.046(3) 0.054(3) 0.028(2) -0.011(2) -0.016(2) 0.009(3) O4 0.045(3) 0.043(3) 0.031(2) -0.007(2) -0.004(2) -0.006(2) O5 0.055(3) 0.055(3) 0.055(3) -0.0005(10) 0.0099(11) -0.0001(10) O5' 0.065(4) 0.066(4) 0.066(4) 0.0004(10) 0.0116(12) 0.0002(10) O6 0.079(4) 0.153(7) 0.036(3) 0.005(4) 0.012(3) -0.020(4) O7 0.082(3) 0.081(3) 0.081(3) 0.0002(7) 0.0126(8) -0.0001(7) O7' 0.082(3) 0.081(3) 0.081(3) 0.0002(7) 0.0126(8) -0.0001(7) O8 0.103(5) 0.049(4) 0.054(3) -0.017(3) -0.021(3) -0.001(3) N1 0.055(4) 0.088(5) 0.032(3) -0.007(4) 0.009(3) -0.007(4) N2 0.121(7) 0.042(4) 0.057(4) -0.001(4) -0.046(5) 0.007(4) N3 0.031(3) 0.041(3) 0.039(3) 0.002(3) -0.002(3) -0.003(3) N4 0.029(3) 0.041(3) 0.042(3) -0.001(3) -0.001(2) -0.002(3) N5 0.031(3) 0.064(4) 0.048(4) 0.014(3) -0.003(3) 0.004(3) N6 0.028(3) 0.077(5) 0.100(6) 0.034(5) 0.003(4) 0.001(4) C1 0.041(4) 0.043(4) 0.023(3) 0.000(3) -0.008(3) -0.004(3) C2 0.036(4) 0.049(4) 0.025(3) -0.001(3) 0.006(3) -0.003(3) C3 0.031(3) 0.045(4) 0.033(4) 0.002(3) -0.007(3) -0.005(3) C4 0.034(4) 0.036(4) 0.026(3) 0.001(3) -0.003(3) -0.005(3) C5 0.039(4) 0.052(5) 0.023(3) -0.004(3) 0.001(3) -0.011(3) C6 0.029(3) 0.054(5) 0.031(3) -0.001(3) -0.006(3) -0.014(3) C7 0.046(4) 0.039(4) 0.037(4) -0.001(3) -0.015(3) -0.002(4) C8 0.040(4) 0.047(4) 0.024(3) -0.008(3) -0.002(3) -0.003(3) C9 0.056(5) 0.037(4) 0.034(4) -0.006(3) -0.011(3) -0.002(4) C10 0.052(4) 0.042(5) 0.031(4) -0.003(3) -0.006(3) 0.009(3) C11 0.036(4) 0.042(4) 0.026(3) -0.003(3) -0.003(3) -0.001(3) C12 0.059(5) 0.040(4) 0.032(4) -0.006(3) -0.015(3) -0.002(4) C13 0.059(5) 0.045(5) 0.036(4) -0.001(3) -0.015(4) 0.001(4) C14 0.027(3) 0.057(5) 0.027(3) -0.010(3) 0.002(3) -0.001(3) C15 0.028(4) 0.053(5) 0.039(4) -0.003(3) -0.003(3) 0.000(3) C16 0.039(4) 0.057(5) 0.039(4) -0.008(4) 0.002(3) -0.002(4) C17 0.043(4) 0.068(6) 0.049(4) -0.013(4) 0.002(4) 0.009(4) C18 0.028(4) 0.053(5) 0.053(4) 0.001(4) -0.009(3) 0.001(3) C19 0.026(3) 0.040(5) 0.060(5) -0.007(4) 0.002(3) -0.002(3) C20 0.092(3) 0.092(3) 0.094(3) 0.0010(10) 0.0161(11) 0.0002(10) C21 0.101(4) 0.102(4) 0.103(4) 0.0005(10) 0.0179(12) 0.0005(10) C22 0.030(4) 0.049(5) 0.133(9) 0.034(5) 0.014(5) 0.001(4) C23 0.086(7) 0.032(5) 0.113(8) 0.002(5) 0.040(6) -0.002(5) C24 0.084(7) 0.045(5) 0.122(8) 0.006(5) 0.057(7) 0.012(5) C25 0.078(3) 0.079(3) 0.080(3) 0.0014(10) 0.0124(11) -0.0001(10) C26 0.034(4) 0.073(6) 0.058(5) 0.018(4) -0.004(4) -0.008(4) C27 0.047(5) 0.064(6) 0.063(5) 0.012(5) 0.008(4) -0.003(4) C28 0.053(6) 0.065(6) 0.108(8) 0.013(6) 0.035(6) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N5 2.290(6) 1_655 ? Cd1 O2 2.295(5) 5_566 ? Cd1 N3 2.337(5) . ? Cd1 O1 2.374(5) . ? Cd1 O3 2.407(4) 4_455 ? Cd1 O4 2.420(4) 4_455 ? Cd1 C14 2.720(6) 4_455 ? O1 C7 1.258(8) . ? O2 C7 1.256(8) . ? O2 Cd1 2.295(5) 5_566 ? O3 C14 1.258(8) . ? O3 Cd1 2.407(4) 4_445 ? O4 C14 1.260(8) . ? O4 Cd1 2.420(4) 4_445 ? O5 N1 1.215(13) . ? O5' N1 1.298(15) . ? O6 N1 1.206(8) . ? O7 N2 1.311(11) . ? O7' N2 1.28(2) . ? O8 N2 1.175(8) . ? N1 C2 1.475(8) . ? N2 C9 1.465(10) . ? N3 C15 1.308(8) . ? N3 C16 1.356(9) . ? N4 C15 1.334(8) . ? N4 C17 1.363(9) . ? N4 C18 1.483(8) . ? N5 C26 1.336(9) . ? N5 C27 1.378(10) . ? N5 Cd1 2.290(6) 1_455 ? N6 C26 1.315(11) . ? N6 C28 1.348(12) . ? N6 C25 1.469(12) . ? C1 C6 1.387(9) . ? C1 C2 1.396(9) . ? C1 C8 1.495(9) . ? C2 C3 1.378(9) . ? C3 C4 1.380(9) . ? C3 H3 0.9300 . ? C4 C5 1.383(9) . ? C4 C7 1.496(9) . ? C5 C6 1.399(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.387(10) . ? C8 C9 1.396(10) . ? C9 C10 1.385(9) . ? C10 C11 1.379(10) . ? C10 H10 0.9300 . ? C11 C12 1.381(9) . ? C11 C14 1.505(9) . ? C12 C13 1.398(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 Cd1 2.720(6) 4_445 ? C15 H15 0.9300 . ? C16 C17 1.352(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.503(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.345(11) . ? C19 C20 1.361(12) . ? C20 C21 1.410(15) . ? C20 H20 0.9300 . ? C21 C22 1.415(14) . ? C21 H21 0.9300 . ? C22 C23 1.328(12) . ? C22 C25 1.510(12) . ? C23 C24 1.374(12) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26 0.9300 . ? C27 C28 1.369(12) . ? C27 H27 0.9300 . ? C28 H28 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 N5 Cd1 O2 85.0(2) 1_655 5_566 ? N5 Cd1 N3 162.2(2) 1_655 . ? O2 Cd1 N3 112.8(2) 5_566 . ? N5 Cd1 O1 87.4(2) 1_655 . ? O2 Cd1 O1 109.55(18) 5_566 . ? N3 Cd1 O1 86.44(19) . . ? N5 Cd1 O3 97.07(19) 1_655 4_455 ? O2 Cd1 O3 93.87(18) 5_566 4_455 ? N3 Cd1 O3 82.40(18) . 4_455 ? O1 Cd1 O3 156.48(16) . 4_455 ? N5 Cd1 O4 83.90(19) 1_655 4_455 ? O2 Cd1 O4 144.93(18) 5_566 4_455 ? N3 Cd1 O4 81.30(18) . 4_455 ? O1 Cd1 O4 103.03(17) . 4_455 ? O3 Cd1 O4 54.89(16) 4_455 4_455 ? N5 Cd1 C14 93.3(2) 1_655 4_455 ? O2 Cd1 C14 120.9(2) 5_566 4_455 ? N3 Cd1 C14 77.93(19) . 4_455 ? O1 Cd1 C14 129.5(2) . 4_455 ? O3 Cd1 C14 27.56(19) 4_455 4_455 ? O4 Cd1 C14 27.60(19) 4_455 4_455 ? C7 O1 Cd1 131.3(5) . . ? C7 O2 Cd1 105.3(4) . 5_566 ? C14 O3 Cd1 90.2(4) . 4_445 ? C14 O4 Cd1 89.6(4) . 4_445 ? O6 N1 O5 120.2(8) . . ? O6 N1 O5' 125.7(8) . . ? O5 N1 O5' 29.2(7) . . ? O6 N1 C2 119.9(6) . . ? O5 N1 C2 117.5(8) . . ? O5' N1 C2 112.7(8) . . ? O8 N2 O7' 114.6(13) . . ? O8 N2 O7 119.7(8) . . ? O7' N2 O7 47.1(10) . . ? O8 N2 C9 122.5(7) . . ? O7' N2 C9 113.8(12) . . ? O7 N2 C9 115.5(7) . . ? C15 N3 C16 106.2(6) . . ? C15 N3 Cd1 127.0(5) . . ? C16 N3 Cd1 125.2(4) . . ? C15 N4 C17 106.0(6) . . ? C15 N4 C18 127.4(6) . . ? C17 N4 C18 126.4(6) . . ? C26 N5 C27 105.2(7) . . ? C26 N5 Cd1 125.7(6) . 1_455 ? C27 N5 Cd1 128.9(5) . 1_455 ? C26 N6 C28 107.7(7) . . ? C26 N6 C25 125.1(9) . . ? C28 N6 C25 127.1(9) . . ? C6 C1 C2 117.1(6) . . ? C6 C1 C8 117.9(6) . . ? C2 C1 C8 124.9(6) . . ? C3 C2 C1 121.8(6) . . ? C3 C2 N1 116.6(6) . . ? C1 C2 N1 121.6(6) . . ? C2 C3 C4 120.5(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 119.0(6) . . ? C3 C4 C7 119.6(6) . . ? C5 C4 C7 121.4(6) . . ? C4 C5 C6 120.1(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 121.3(6) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? O2 C7 O1 123.1(6) . . ? O2 C7 C4 118.3(6) . . ? O1 C7 C4 118.6(6) . . ? C13 C8 C9 116.6(6) . . ? C13 C8 C1 117.4(6) . . ? C9 C8 C1 126.0(6) . . ? C10 C9 C8 122.2(7) . . ? C10 C9 N2 118.2(6) . . ? C8 C9 N2 119.6(6) . . ? C11 C10 C9 120.0(6) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.4(6) . . ? C10 C11 C14 119.8(6) . . ? C12 C11 C14 120.6(6) . . ? C11 C12 C13 119.9(7) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 121.9(7) . . ? C8 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? O3 C14 O4 124.1(6) . . ? O3 C14 C11 118.5(7) . . ? O4 C14 C11 117.2(6) . . ? O3 C14 Cd1 62.2(3) . 4_445 ? O4 C14 Cd1 62.8(3) . 4_445 ? C11 C14 Cd1 164.2(4) . 4_445 ? N3 C15 N4 111.9(6) . . ? N3 C15 H15 124.0 . . ? N4 C15 H15 124.0 . . ? C17 C16 N3 108.6(6) . . ? C17 C16 H16 125.7 . . ? N3 C16 H16 125.7 . . ? C16 C17 N4 107.2(6) . . ? C16 C17 H17 126.4 . . ? N4 C17 H17 126.4 . . ? N4 C18 C19 110.9(6) . . ? N4 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.0 . . ? C24 C19 C20 116.5(8) . . ? C24 C19 C18 123.4(7) . . ? C20 C19 C18 119.7(8) . . ? C19 C20 C21 122.3(11) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C20 C21 C22 117.5(10) . . ? C20 C21 H21 121.3 . . ? C22 C21 H21 121.3 . . ? C23 C22 C21 117.7(8) . . ? C23 C22 C25 123.1(8) . . ? C21 C22 C25 117.8(9) . . ? C22 C23 C24 121.5(8) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C19 C24 C23 122.9(8) . . ? C19 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? N6 C25 C22 111.8(8) . . ? N6 C25 H25A 109.3 . . ? C22 C25 H25A 109.3 . . ? N6 C25 H25B 109.3 . . ? C22 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? N6 C26 N5 111.8(8) . . ? N6 C26 H26 124.1 . . ? N5 C26 H26 124.1 . . ? C28 C27 N5 107.9(8) . . ? C28 C27 H27 126.0 . . ? N5 C27 H27 126.0 . . ? N6 C28 C27 107.3(8) . . ? N6 C28 H28 126.3 . . ? C27 C28 H28 126.3 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.218 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.107 #=========================END data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 842367' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C42 H28 Mn2 N8 O17' _chemical_formula_sum 'C42 H28 Mn2 N8 O17' _chemical_formula_weight 1026.60 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' Mn Mn 0.3368 0.7283 '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 12.7244(6) _cell_length_b 26.4144(11) _cell_length_c 13.2270(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.738(3) _cell_angle_gamma 90.00 _cell_volume 4336.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4044 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 25.51 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.669 _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 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12762 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.51 _reflns_number_total 4044 _reflns_number_gt 3075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0561P)^2^+10.0820P] 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 4044 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Mn1 Mn 0.92292(4) 0.488884(17) 0.11079(4) 0.02748(16) Uani 1 1 d . . . O1 O 1.0276(2) 0.55041(9) 0.1380(2) 0.0478(7) Uani 1 1 d . A . O2 O 1.1425(2) 0.54471(9) 0.03298(19) 0.0465(6) Uani 1 1 d . . . O3 O 1.3512(2) 0.95144(9) 0.2189(2) 0.0468(6) Uani 1 1 d . . . O4 O 1.4611(2) 0.92827(9) 0.3674(2) 0.0480(7) Uani 1 1 d . . . O5 O 1.1069(13) 0.7508(7) 0.3469(14) 0.0597(7) Uani 0.30 1 d P A 1 O5' O 1.1279(14) 0.7536(7) 0.3621(13) 0.0597(7) Uani 0.30 1 d P A 2 O5" O 1.1784(7) 0.7433(3) 0.3969(7) 0.0597(7) Uani 0.40 1 d P A 3 O6 O 1.1167(17) 0.6704(5) 0.4209(17) 0.0597(7) Uani 0.30 1 d P A 1 O6' O 1.1392(15) 0.6786(6) 0.4318(15) 0.0597(7) Uani 0.30 1 d P A 2 O6" O 1.0919(10) 0.6814(4) 0.4051(9) 0.0597(7) Uani 0.40 1 d P A 3 O7 O 1.5141(8) 0.7513(3) 0.4472(5) 0.0597(7) Uani 0.50 1 d P B 1 O7' O 1.5213(8) 0.7480(3) 0.4104(5) 0.0597(7) Uani 0.50 1 d P B 2 O8 O 1.4182(6) 0.6935(2) 0.3580(5) 0.0597(7) Uani 0.50 1 d P B 1 O8' O 1.3764(6) 0.7012(2) 0.3957(5) 0.0597(7) Uani 0.50 1 d P B 2 N1 N 1.1415(3) 0.70494(11) 0.3582(3) 0.0513(9) Uani 1 1 d . . . N2 N 1.4321(3) 0.73874(11) 0.3761(3) 0.0571(10) Uani 1 1 d . . . N3 N 0.7868(2) 0.54143(10) 0.0917(2) 0.0361(7) Uani 1 1 d . . . N4 N 0.6687(2) 0.59758(11) 0.0143(2) 0.0433(7) Uani 1 1 d . . . C1 C 1.2326(3) 0.71285(13) 0.2110(3) 0.0419(9) Uani 1 1 d . . . C2 C 1.1710(3) 0.68429(12) 0.2647(3) 0.0347(8) Uani 1 1 d . A . C3 C 1.1319(3) 0.63657(12) 0.2325(2) 0.0311(7) Uani 1 1 d . . . H3 H 1.0925 0.6182 0.2714 0.080 Uiso 1 1 calc . . . C4 C 1.1521(3) 0.61654(12) 0.1423(3) 0.0344(8) Uani 1 1 d . A . C5 C 1.2129(4) 0.64438(16) 0.0872(3) 0.0537(11) Uani 1 1 d . . . H5 H 1.2276 0.6310 0.0269 0.080 Uiso 1 1 calc . . . C6 C 1.2520(4) 0.69177(16) 0.1204(3) 0.0571(12) Uani 1 1 d . A . H6 H 1.2918 0.7099 0.0816 0.080 Uiso 1 1 calc . . . C7 C 1.1040(3) 0.56621(12) 0.1013(3) 0.0354(8) Uani 1 1 d . . . C8 C 1.2734(3) 0.76565(13) 0.2385(3) 0.0406(9) Uani 1 1 d . A . C9 C 1.3664(3) 0.77804(12) 0.3139(3) 0.0392(8) Uani 1 1 d . A . C10 C 1.4014(3) 0.82766(12) 0.3322(3) 0.0362(8) Uani 1 1 d . . . H10 H 1.4615 0.8349 0.3843 0.080 Uiso 1 1 calc . . . C11 C 1.3466(3) 0.86614(12) 0.2728(3) 0.0338(7) Uani 1 1 d . B . C12 C 1.2552(3) 0.85498(13) 0.1962(3) 0.0421(9) Uani 1 1 d . . . H12 H 1.2180 0.8809 0.1558 0.080 Uiso 1 1 calc . . . C13 C 1.2199(3) 0.80539(14) 0.1800(3) 0.0455(9) Uani 1 1 d . A . H13 H 1.1587 0.7985 0.1288 0.080 Uiso 1 1 calc . . . C14 C 1.3891(3) 0.91986(12) 0.2877(3) 0.0361(8) Uani 1 1 d . . . C15 C 0.7645(3) 0.57545(14) 0.0182(3) 0.0396(8) Uani 1 1 d . . . H15 H 0.8096 0.5834 -0.0261 0.080 Uiso 1 1 calc . . . C16 C 0.7009(3) 0.54188(15) 0.1385(3) 0.0451(9) Uani 1 1 d . . . H16 H 0.6942 0.5218 0.1944 0.080 Uiso 1 1 calc . . . C17 C 0.6276(3) 0.57601(16) 0.0910(3) 0.0509(10) Uani 1 1 d . . . H17 H 0.5618 0.5834 0.1073 0.080 Uiso 1 1 calc . . . C18 C 0.6127(4) 0.63007(15) -0.0704(3) 0.0551(11) Uani 1 1 d . . . H18A H 0.6647 0.6522 -0.0919 0.080 Uiso 1 1 calc . . . H18B H 0.5613 0.6512 -0.0456 0.080 Uiso 1 1 calc . . . C19 C 0.5000 0.62514(19) -0.2500 0.0396(11) Uani 1 2 d S . . H19 H 0.5000 0.6603 -0.2500 0.080 Uiso 1 2 calc S . . C20 C 0.5541(3) 0.59954(14) -0.1629(3) 0.0417(8) Uani 1 1 d . . . C21 C 0.5536(3) 0.54675(15) -0.1633(3) 0.0502(10) Uani 1 1 d . . . H21 H 0.5894 0.5290 -0.1052 0.080 Uiso 1 1 calc . . . C22 C 0.5000 0.5211(2) -0.2500 0.0534(14) Uani 1 2 d S . . H22 H 0.5000 0.4859 -0.2500 0.080 Uiso 1 2 calc S . . O1W O 0.6316(7) 0.4381(4) -0.0084(8) 0.118(3) Uani 0.50 1 d P . . 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 Mn1 0.0321(3) 0.0158(2) 0.0320(3) -0.0009(2) 0.00148(19) -0.00081(19) O1 0.0436(15) 0.0262(13) 0.0718(18) -0.0137(12) 0.0090(13) -0.0101(11) O2 0.0513(16) 0.0373(14) 0.0453(14) -0.0187(12) -0.0014(12) 0.0000(12) O3 0.0530(16) 0.0301(13) 0.0579(16) 0.0133(12) 0.0137(13) -0.0055(11) O4 0.0566(16) 0.0279(13) 0.0536(16) 0.0008(12) -0.0007(13) -0.0159(12) O5 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O5' 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O5" 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O6 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O6' 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O6" 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O7 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O7' 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O8 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) O8' 0.081(2) 0.0384(13) 0.059(2) -0.0008(14) 0.0137(15) 0.0013(12) N1 0.080(2) 0.0262(16) 0.055(2) -0.0117(15) 0.0295(19) -0.0186(16) N2 0.081(3) 0.0221(16) 0.059(2) 0.0018(15) -0.0040(19) -0.0157(16) N3 0.0370(16) 0.0313(15) 0.0382(15) 0.0018(13) 0.0046(13) 0.0038(12) N4 0.0480(18) 0.0392(17) 0.0380(17) 0.0024(14) -0.0008(14) 0.0125(14) C1 0.055(2) 0.0300(18) 0.040(2) -0.0069(16) 0.0103(17) -0.0168(16) C2 0.0436(19) 0.0267(17) 0.0335(17) -0.0078(14) 0.0078(15) -0.0092(14) C3 0.0330(17) 0.0227(15) 0.0358(18) -0.0009(14) 0.0035(14) -0.0041(13) C4 0.0381(18) 0.0267(17) 0.0358(18) -0.0064(14) 0.0022(15) -0.0057(14) C5 0.074(3) 0.048(2) 0.046(2) -0.0189(19) 0.025(2) -0.023(2) C6 0.080(3) 0.048(2) 0.051(2) -0.012(2) 0.031(2) -0.032(2) C7 0.0346(19) 0.0242(16) 0.0410(19) -0.0068(15) -0.0050(15) 0.0011(14) C8 0.057(2) 0.0276(18) 0.0391(19) -0.0056(15) 0.0143(17) -0.0187(16) C9 0.055(2) 0.0241(17) 0.0369(19) 0.0021(14) 0.0067(16) -0.0083(15) C10 0.045(2) 0.0269(17) 0.0351(18) -0.0012(14) 0.0047(15) -0.0099(15) C11 0.0411(19) 0.0243(16) 0.0362(18) 0.0004(14) 0.0090(15) -0.0095(14) C12 0.048(2) 0.0325(19) 0.042(2) 0.0052(16) 0.0030(17) -0.0075(16) C13 0.052(2) 0.037(2) 0.042(2) -0.0004(17) -0.0006(17) -0.0138(17) C14 0.042(2) 0.0243(17) 0.045(2) 0.0023(16) 0.0163(17) -0.0068(15) C15 0.042(2) 0.0356(19) 0.0400(19) 0.0026(16) 0.0072(16) 0.0057(16) C16 0.045(2) 0.047(2) 0.044(2) 0.0066(18) 0.0121(17) 0.0057(17) C17 0.039(2) 0.057(3) 0.056(2) 0.004(2) 0.0084(18) 0.0121(18) C18 0.068(3) 0.041(2) 0.044(2) -0.0011(18) -0.014(2) 0.018(2) C19 0.037(3) 0.036(3) 0.042(3) 0.000 0.001(2) 0.000 C20 0.040(2) 0.040(2) 0.043(2) -0.0003(17) 0.0028(16) 0.0077(16) C21 0.055(2) 0.038(2) 0.052(2) 0.0050(19) 0.0020(19) 0.0090(18) C22 0.066(4) 0.034(3) 0.058(4) 0.000 0.009(3) 0.000 O1W 0.078(6) 0.103(6) 0.162(9) 0.006(6) 0.004(6) -0.002(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 Mn1 O1 2.082(2) . ? Mn1 O2 2.097(2) 5_765 ? Mn1 O3 2.105(2) 3_445 ? Mn1 O4 2.153(2) 4_745 ? Mn1 N3 2.190(3) . ? O1 C7 1.250(4) . ? O2 C7 1.254(4) . ? O2 Mn1 2.097(2) 5_765 ? O3 C14 1.250(4) . ? O3 Mn1 2.105(2) 3 ? O4 C14 1.255(4) . ? O4 Mn1 2.153(2) 4_755 ? O5 N1 1.287(19) . ? O5' N1 1.30(2) . ? O5" N1 1.184(8) . ? O6 N1 1.316(18) . ? O6' N1 1.202(19) . ? O6" N1 1.158(13) . ? O7 N2 1.285(10) . ? O7' N2 1.152(10) . ? O8 N2 1.225(7) . ? O8' N2 1.277(7) . ? N1 C2 1.474(4) . ? N2 C9 1.466(5) . ? N3 C15 1.308(4) . ? N3 C16 1.370(5) . ? N4 C15 1.342(5) . ? N4 C17 1.364(5) . ? N4 C18 1.465(5) . ? C1 C2 1.390(5) . ? C1 C6 1.392(5) . ? C1 C8 1.505(5) . ? C2 C3 1.387(4) . ? C3 C4 1.380(5) . ? C3 H3 0.9300 . ? C4 C5 1.384(5) . ? C4 C7 1.513(4) . ? C5 C6 1.382(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.390(5) . ? C8 C9 1.408(5) . ? C9 C10 1.388(5) . ? C10 C11 1.376(5) . ? C10 H10 0.9300 . ? C11 C12 1.395(5) . ? C11 C14 1.516(4) . ? C12 C13 1.386(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.349(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C20 1.518(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.381(4) 2_654 ? C19 C20 1.381(4) . ? C19 H19 0.9300 . ? C20 C21 1.394(5) . ? C21 C22 1.377(5) . ? C21 H21 0.9300 . ? C22 C21 1.377(5) 2_654 ? C22 H22 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 126.70(11) . 5_765 ? O1 Mn1 O3 127.32(11) . 3_445 ? O2 Mn1 O3 105.81(11) 5_765 3_445 ? O1 Mn1 O4 99.44(10) . 4_745 ? O2 Mn1 O4 86.00(10) 5_765 4_745 ? O3 Mn1 O4 86.93(10) 3_445 4_745 ? O1 Mn1 N3 89.12(10) . . ? O2 Mn1 N3 91.04(10) 5_765 . ? O3 Mn1 N3 85.74(10) 3_445 . ? O4 Mn1 N3 171.03(11) 4_745 . ? C7 O1 Mn1 135.8(2) . . ? C7 O2 Mn1 134.8(2) . 5_765 ? C14 O3 Mn1 130.7(2) . 3 ? C14 O4 Mn1 126.6(2) . 4_755 ? O6" N1 O5" 116.1(8) . . ? O6" N1 O6' 31.0(7) . . ? O5" N1 O6' 103.0(8) . . ? O6" N1 O5 110.9(11) . . ? O5" N1 O5 48.5(6) . . ? O6' N1 O5 124.9(12) . . ? O6" N1 O5' 114.7(11) . . ? O5" N1 O5' 35.0(6) . . ? O6' N1 O5' 121.0(13) . . ? O5 N1 O5' 13.6(10) . . ? O6" N1 O6 19.4(12) . . ? O5" N1 O6 116.6(10) . . ? O6' N1 O6 15.7(13) . . ? O5 N1 O6 127.1(14) . . ? O5' N1 O6 127.4(12) . . ? O6" N1 C2 121.3(6) . . ? O5" N1 C2 121.9(5) . . ? O6' N1 C2 121.4(9) . . ? O5 N1 C2 113.2(9) . . ? O5' N1 C2 117.4(10) . . ? O6 N1 C2 114.4(9) . . ? O7' N2 O8 111.8(6) . . ? O7' N2 O8' 128.8(6) . . ? O8 N2 O8' 38.7(3) . . ? O7' N2 O7 23.9(4) . . ? O8 N2 O7 117.1(5) . . ? O8' N2 O7 116.7(5) . . ? O7' N2 C9 117.5(5) . . ? O8 N2 C9 122.8(4) . . ? O8' N2 C9 112.9(4) . . ? O7 N2 C9 119.9(4) . . ? C15 N3 C16 105.4(3) . . ? C15 N3 Mn1 123.9(2) . . ? C16 N3 Mn1 130.0(2) . . ? C15 N4 C17 106.5(3) . . ? C15 N4 C18 124.7(3) . . ? C17 N4 C18 127.7(3) . . ? C2 C1 C6 116.7(3) . . ? C2 C1 C8 125.7(3) . . ? C6 C1 C8 117.5(3) . . ? C3 C2 C1 122.7(3) . . ? C3 C2 N1 117.0(3) . . ? C1 C2 N1 120.3(3) . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 C7 120.6(3) . . ? C5 C4 C7 120.5(3) . . ? C6 C5 C4 121.2(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 121.0(3) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? O1 C7 O2 126.1(3) . . ? O1 C7 C4 116.3(3) . . ? O2 C7 C4 117.7(3) . . ? C13 C8 C9 116.8(3) . . ? C13 C8 C1 117.7(3) . . ? C9 C8 C1 125.3(3) . . ? C10 C9 C8 122.0(3) . . ? C10 C9 N2 116.7(3) . . ? C8 C9 N2 121.3(3) . . ? C11 C10 C9 119.7(3) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 119.7(3) . . ? C10 C11 C14 119.7(3) . . ? C12 C11 C14 120.6(3) . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 121.7(3) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? O3 C14 O4 125.9(3) . . ? O3 C14 C11 117.4(3) . . ? O4 C14 C11 116.7(3) . . ? N3 C15 N4 112.0(3) . . ? N3 C15 H15 124.0 . . ? N4 C15 H15 124.0 . . ? C17 C16 N3 109.5(3) . . ? C17 C16 H16 125.2 . . ? N3 C16 H16 125.2 . . ? C16 C17 N4 106.6(3) . . ? C16 C17 H17 126.7 . . ? N4 C17 H17 126.7 . . ? N4 C18 C20 112.0(3) . . ? N4 C18 H18A 109.2 . . ? C20 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C20 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C20 121.4(5) 2_654 . ? C20 C19 H19 119.3 2_654 . ? C20 C19 H19 119.3 . . ? C19 C20 C21 119.0(4) . . ? C19 C20 C18 118.6(3) . . ? C21 C20 C18 122.4(3) . . ? C22 C21 C20 119.8(4) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C21 120.9(5) . 2_654 ? C21 C22 H22 119.5 . . ? C21 C22 H22 119.5 2_654 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.100 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.068 #=========================END data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 842368' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C28 H20 N6 O8 Zn' _chemical_formula_sum 'C28 H20 N6 O8 Zn' _chemical_formula_weight 633.87 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' Zn Zn 0.2839 1.4301 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 10.715(2) _cell_length_b 11.039(2) _cell_length_c 24.188(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.41(3) _cell_angle_gamma 90.00 _cell_volume 2758.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5143 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 25.54 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.953 _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 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15863 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.54 _reflns_number_total 5143 _reflns_number_gt 3945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0428P)^2^+1.7327P] 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 5143 _refine_ls_number_parameters 452 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.073 _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 Zn1 Zn 0.84268(3) -0.57935(3) 0.079687(12) 0.02809(11) Uani 1 1 d . . . O1 O 0.8346(2) -0.65991(19) 0.00635(8) 0.0446(5) Uani 1 1 d . . . O2 O 1.0444(2) -0.7040(2) 0.02496(10) 0.0705(8) Uani 1 1 d . . . O3 O 0.8051(2) -1.2830(2) -0.37559(9) 0.0502(6) Uani 1 1 d . . . O4 O 0.7940(3) -1.4309(2) -0.31491(10) 0.0626(7) Uani 1 1 d . . . O5 O 0.5980(3) -1.0752(2) -0.15710(13) 0.0747(8) Uani 1 1 d . . . O6 O 0.5295(2) -0.9011(3) -0.13828(12) 0.0711(8) Uani 1 1 d . . . O7 O 0.7803(3) -0.8567(2) -0.30451(12) 0.0810(9) Uani 1 1 d . . . O8 O 0.6739(2) -0.8511(2) -0.24089(10) 0.0600(7) Uani 1 1 d . . . N1 N 0.6160(3) -0.9711(3) -0.14007(11) 0.0474(7) Uani 1 1 d . . . N2 N 0.7426(3) -0.9029(2) -0.26640(11) 0.0478(7) Uani 1 1 d . . . N3 N 1.0050(2) -0.4921(2) 0.12090(9) 0.0351(5) Uani 1 1 d . . . N4 N 1.2075(2) -0.4333(2) 0.14941(10) 0.0410(6) Uani 1 1 d . . . N5 N 0.7074(3) -0.4506(2) 0.05546(11) 0.0491(7) Uani 1 1 d . . . C1 C 0.8447(3) -0.9690(3) -0.14462(12) 0.0376(7) Uani 1 1 d . . . C2 C 0.7503(3) -0.9274(2) -0.11981(11) 0.0339(6) Uani 1 1 d . . . C3 C 0.7751(3) -0.8441(3) -0.07543(12) 0.0366(7) Uani 1 1 d . . . H3 H 0.7085 -0.8172 -0.0605 0.080 Uiso 1 1 calc . . . C4 C 0.9006(3) -0.8007(3) -0.05340(11) 0.0364(7) Uani 1 1 d . . . C5 C 0.9952(3) -0.8385(3) -0.07900(14) 0.0504(8) Uani 1 1 d . . . H5 H 1.0787 -0.8079 -0.0658 0.080 Uiso 1 1 calc . . . C6 C 0.9684(3) -0.9208(3) -0.12375(14) 0.0494(8) Uani 1 1 d . . . H6 H 1.0339 -0.9444 -0.1401 0.080 Uiso 1 1 calc . . . C7 C 0.8242(3) -1.0591(3) -0.19258(12) 0.0361(7) Uani 1 1 d . . . C8 C 0.7812(3) -1.0280(3) -0.25029(12) 0.0367(6) Uani 1 1 d . . . C9 C 0.7752(3) -1.1104(3) -0.29406(12) 0.0395(7) Uani 1 1 d . . . H9 H 0.7495 -1.0858 -0.3322 0.080 Uiso 1 1 calc . . . C10 C 0.8081(3) -1.2294(3) -0.28024(12) 0.0369(7) Uani 1 1 d . . . C11 C 0.8512(3) -1.2631(3) -0.22326(12) 0.0424(7) Uani 1 1 d . . . H11 H 0.8734 -1.3434 -0.2139 0.080 Uiso 1 1 calc . . . C12 C 0.8617(3) -1.1790(3) -0.18019(12) 0.0432(7) Uani 1 1 d . . . H12 H 0.8943 -1.2028 -0.1422 0.080 Uiso 1 1 calc . . . C13 C 0.9314(3) -0.7142(3) -0.00311(12) 0.0406(7) Uani 1 1 d . . . C14 C 0.8011(3) -1.3235(3) -0.32612(13) 0.0430(7) Uani 1 1 d . . . C15 C 1.1184(3) -0.4957(3) 0.11011(12) 0.0384(7) Uani 1 1 d . . . H15 H 1.1352 -0.5363 0.0792 0.080 Uiso 1 1 calc . . . C16 C 1.0221(3) -0.4230(3) 0.17003(13) 0.0436(7) Uani 1 1 d . . . H16 H 0.9578 -0.4038 0.1879 0.080 Uiso 1 1 calc . . . C17 C 1.1460(3) -0.3880(3) 0.18785(13) 0.0477(8) Uani 1 1 d . . . H17 H 1.1831 -0.3418 0.2202 0.080 Uiso 1 1 calc . . . C18 C 1.3460(3) -0.4233(3) 0.15197(14) 0.0521(8) Uani 1 1 d . . . H18A H 1.3711 -0.3386 0.1551 0.080 Uiso 1 1 calc . . . H18B H 1.3606 -0.4550 0.1168 0.080 Uiso 1 1 calc . . . C19 C 1.4283(3) -0.4922(3) 0.20246(14) 0.0452(8) Uani 1 1 d . . . C20 C 1.4298(3) -0.6178(3) 0.20245(16) 0.0561(9) Uani 1 1 d . . . H20 H 1.3833 -0.6601 0.1703 0.080 Uiso 1 1 calc . . . C21 C 1.5000 -0.6803(4) 0.2500 0.0629(14) Uani 1 2 d S . . H21 H 1.5000 -0.7645 0.2500 0.080 Uiso 1 2 calc S . . C22 C 1.5000 -0.4302(4) 0.2500 0.0434(10) Uani 1 2 d S . . H22 H 1.5000 -0.3459 0.2500 0.080 Uiso 1 2 calc S . . C23 C 0.7155(7) -0.3661(7) 0.0150(3) 0.0376(18) Uani 0.50 1 d PU A 1 C23' C 0.6766(7) -0.3899(7) 0.0065(3) 0.0380(19) Uani 0.50 1 d PU A 2 N6 N 0.6546(5) -0.2631(5) 0.0200(2) 0.0445(12) Uani 0.50 1 d P A 1 N6' N 0.5665(5) -0.3271(5) -0.0017(2) 0.0470(13) Uani 0.50 1 d P A 2 C24 C 0.6626(9) -0.3770(9) 0.0960(3) 0.064(2) Uani 0.50 1 d P A 1 C24' C 0.5899(9) -0.4463(9) 0.0710(5) 0.077(3) Uani 0.50 1 d P A 2 C25 C 0.6224(10) -0.2679(8) 0.0714(3) 0.079(3) Uani 0.50 1 d P A 1 C25' C 0.5090(9) -0.3638(9) 0.0378(5) 0.087(3) Uani 0.50 1 d P A 2 C26 C 0.6456(10) -0.1593(8) -0.0200(4) 0.079(3) Uani 0.50 1 d P A 1 C26' C 0.5178(8) -0.2309(6) -0.0450(3) 0.063(2) Uani 0.50 1 d P A 2 C27 C 0.5571(7) 0.0352(6) 0.0127(3) 0.0489(16) Uani 0.50 1 d P . . C28 C 0.5386(4) -0.0939(4) -0.01619(14) 0.0578(9) Uani 1 1 d . . . C29 C 0.6718(7) -0.0701(7) 0.0079(3) 0.0568(18) Uani 0.50 1 d P A . C31 C 0.4041(8) -0.1148(7) -0.0412(3) 0.0563(19) Uani 0.50 1 d P . . C30 C 0.6920(7) 0.0414(7) 0.0367(3) 0.0571(19) Uani 0.50 1 d P . . 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 Zn1 0.03353(18) 0.02637(17) 0.02406(16) -0.00022(13) 0.00712(12) 0.00064(13) O1 0.0582(14) 0.0457(12) 0.0292(10) -0.0106(9) 0.0106(10) 0.0032(10) O2 0.0572(16) 0.0841(19) 0.0601(16) -0.0405(14) -0.0024(13) -0.0018(14) O3 0.0676(15) 0.0478(13) 0.0350(11) -0.0092(10) 0.0131(11) 0.0114(11) O4 0.095(2) 0.0394(14) 0.0553(15) -0.0152(11) 0.0229(14) 0.0034(13) O5 0.0717(17) 0.0621(17) 0.097(2) -0.0415(15) 0.0351(16) -0.0278(14) O6 0.0415(14) 0.088(2) 0.0834(19) -0.0294(15) 0.0152(13) 0.0017(13) O7 0.118(2) 0.0569(17) 0.0791(19) 0.0225(15) 0.0456(18) 0.0070(16) O8 0.0768(17) 0.0445(14) 0.0526(14) -0.0087(11) 0.0064(13) 0.0223(12) N1 0.0448(16) 0.0571(18) 0.0425(15) -0.0153(13) 0.0157(12) -0.0064(14) N2 0.0602(17) 0.0382(15) 0.0411(15) -0.0047(12) 0.0067(13) 0.0043(13) N3 0.0392(14) 0.0340(13) 0.0293(12) -0.0029(10) 0.0040(10) -0.0034(11) N4 0.0410(14) 0.0414(15) 0.0348(13) 0.0020(11) -0.0003(11) -0.0079(11) N5 0.0562(17) 0.0515(16) 0.0471(15) 0.0164(13) 0.0271(13) 0.0265(13) C1 0.0434(17) 0.0369(15) 0.0310(15) -0.0078(13) 0.0071(13) 0.0062(13) C2 0.0376(15) 0.0346(15) 0.0290(14) -0.0051(12) 0.0079(12) -0.0009(12) C3 0.0457(17) 0.0345(16) 0.0315(14) -0.0037(12) 0.0136(13) 0.0033(13) C4 0.0449(17) 0.0365(16) 0.0255(14) -0.0062(12) 0.0056(12) 0.0026(13) C5 0.0411(17) 0.059(2) 0.0474(18) -0.0221(16) 0.0049(15) 0.0012(15) C6 0.0392(17) 0.062(2) 0.0464(18) -0.0203(16) 0.0105(14) 0.0052(16) C7 0.0386(16) 0.0382(17) 0.0307(14) -0.0110(12) 0.0082(12) 0.0025(13) C8 0.0428(16) 0.0317(15) 0.0345(15) -0.0058(12) 0.0085(13) 0.0032(13) C9 0.0434(17) 0.0433(17) 0.0314(15) -0.0047(13) 0.0094(13) 0.0012(13) C10 0.0404(16) 0.0371(16) 0.0344(15) -0.0102(13) 0.0120(13) 0.0037(13) C11 0.0497(18) 0.0369(16) 0.0389(16) -0.0043(13) 0.0091(14) 0.0110(14) C12 0.0525(19) 0.0435(18) 0.0308(15) -0.0043(13) 0.0065(14) 0.0104(15) C13 0.0538(19) 0.0393(17) 0.0277(15) -0.0043(13) 0.0090(14) 0.0006(15) C14 0.0440(18) 0.0446(19) 0.0390(17) -0.0117(14) 0.0083(14) 0.0085(14) C15 0.0384(16) 0.0417(17) 0.0314(15) -0.0005(12) 0.0028(13) -0.0073(13) C16 0.0498(19) 0.0397(17) 0.0394(16) -0.0111(14) 0.0086(14) -0.0012(14) C17 0.057(2) 0.0421(18) 0.0373(17) -0.0107(14) 0.0019(15) -0.0073(15) C18 0.0397(17) 0.062(2) 0.0489(19) 0.0059(17) 0.0026(15) -0.0145(16) C19 0.0338(16) 0.0460(19) 0.0532(19) 0.0014(15) 0.0071(14) -0.0064(14) C20 0.0447(19) 0.046(2) 0.072(2) -0.0123(18) 0.0072(17) -0.0075(16) C21 0.051(3) 0.033(3) 0.098(4) 0.000 0.007(3) 0.000 C22 0.039(2) 0.027(2) 0.056(3) 0.000 -0.001(2) 0.000 C23 0.038(2) 0.037(2) 0.038(2) 0.0003(10) 0.0099(11) 0.0008(10) C23' 0.038(2) 0.038(2) 0.038(2) -0.0005(10) 0.0099(11) 0.0007(10) N6 0.052(3) 0.044(3) 0.041(3) 0.006(2) 0.020(3) 0.019(3) N6' 0.047(3) 0.037(3) 0.056(3) 0.008(3) 0.013(3) 0.012(3) C24 0.076(6) 0.083(6) 0.042(4) 0.015(4) 0.029(4) 0.047(5) C24' 0.065(6) 0.081(7) 0.101(7) 0.042(6) 0.052(5) 0.039(5) C25 0.121(7) 0.081(6) 0.046(4) 0.018(4) 0.042(5) 0.065(6) C25' 0.072(6) 0.084(6) 0.121(8) 0.050(6) 0.055(6) 0.041(5) C26 0.121(8) 0.047(5) 0.091(6) 0.043(5) 0.066(6) 0.051(5) C26' 0.082(5) 0.034(4) 0.055(4) 0.003(3) -0.011(4) 0.013(4) C27 0.047(4) 0.048(4) 0.049(4) 0.024(3) 0.008(3) 0.011(3) C28 0.059(2) 0.069(2) 0.0425(19) 0.0121(17) 0.0084(17) -0.002(2) C29 0.052(4) 0.055(5) 0.057(4) 0.020(4) 0.004(3) 0.011(4) C31 0.073(5) 0.042(4) 0.046(4) 0.008(3) 0.001(4) -0.010(4) C30 0.057(4) 0.047(4) 0.059(4) 0.013(3) 0.000(4) -0.006(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 Zn1 O1 1.9656(19) . ? Zn1 O3 1.968(2) 4_536 ? Zn1 N5 2.004(2) . ? Zn1 N3 2.006(2) . ? O1 C13 1.270(4) . ? O2 C13 1.227(4) . ? O3 C14 1.288(4) . ? O3 Zn1 1.968(2) 4_535 ? O4 C14 1.223(4) . ? O5 N1 1.218(3) . ? O6 N1 1.216(3) . ? O7 N2 1.213(4) . ? O8 N2 1.221(3) . ? N1 C2 1.473(4) . ? N2 C8 1.464(4) . ? N3 C15 1.309(4) . ? N3 C16 1.383(4) . ? N4 C15 1.344(3) . ? N4 C17 1.370(4) . ? N4 C18 1.472(4) . ? N5 C23' 1.323(7) . ? N5 C23 1.371(8) . ? N5 C24' 1.408(8) . ? N5 C24 1.449(8) . ? C1 C2 1.384(4) . ? C1 C6 1.392(4) . ? C1 C7 1.499(4) . ? C2 C3 1.385(4) . ? C3 C4 1.393(4) . ? C3 H3 0.9300 . ? C4 C5 1.385(4) . ? C4 C13 1.512(4) . ? C5 C6 1.383(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.392(4) . ? C7 C12 1.393(4) . ? C8 C9 1.385(4) . ? C9 C10 1.379(4) . ? C9 H9 0.9300 . ? C10 C11 1.383(4) . ? C10 C14 1.507(4) . ? C11 C12 1.377(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.339(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.509(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C22 1.383(4) . ? C19 C20 1.387(5) . ? C20 C21 1.380(4) . ? C20 H20 0.9300 . ? C21 C20 1.380(4) 2_855 ? C21 H21 0.9300 . ? C22 C19 1.383(4) 2_855 ? C22 H22 0.9300 . ? C23 N6 1.332(8) . ? C23' N6' 1.337(9) . ? N6 C25 1.376(8) . ? N6 C26 1.487(8) . ? N6' C25' 1.329(10) . ? N6' C26' 1.485(8) . ? C24 C25 1.361(11) . ? C24' C25' 1.363(11) . ? C26 C29 1.184(11) . ? C26 C28 1.379(8) . ? C26' C28 1.655(8) . ? C26' C31 1.787(11) . ? C27 C31 1.127(9) 3_655 ? C27 C28 1.234(8) 3_655 ? C27 C30 1.409(10) . ? C27 C27 1.442(15) 3_655 ? C27 C28 1.576(8) . ? C27 C29 1.718(10) . ? C28 C27 1.234(8) 3_655 ? C28 C29 1.415(8) . ? C28 C31 1.426(8) . ? C29 C30 1.402(11) . ? C31 C27 1.127(9) 3_655 ? C31 C30 1.338(11) 3_655 ? C30 C31 1.338(11) 3_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 100.40(9) . 4_536 ? O1 Zn1 N5 101.66(10) . . ? O3 Zn1 N5 118.08(11) 4_536 . ? O1 Zn1 N3 119.35(10) . . ? O3 Zn1 N3 112.00(9) 4_536 . ? N5 Zn1 N3 105.60(11) . . ? C13 O1 Zn1 122.25(19) . . ? C14 O3 Zn1 107.76(19) . 4_535 ? O6 N1 O5 123.9(3) . . ? O6 N1 C2 117.8(3) . . ? O5 N1 C2 118.3(3) . . ? O7 N2 O8 123.7(3) . . ? O7 N2 C8 118.1(3) . . ? O8 N2 C8 118.2(3) . . ? C15 N3 C16 105.6(2) . . ? C15 N3 Zn1 127.91(19) . . ? C16 N3 Zn1 126.2(2) . . ? C15 N4 C17 106.7(3) . . ? C15 N4 C18 125.9(3) . . ? C17 N4 C18 127.3(3) . . ? C23' N5 C23 20.8(4) . . ? C23' N5 C24' 101.2(5) . . ? C23 N5 C24' 113.5(5) . . ? C23' N5 C24 105.8(5) . . ? C23 N5 C24 101.3(5) . . ? C24' N5 C24 47.1(5) . . ? C23' N5 Zn1 127.6(3) . . ? C23 N5 Zn1 120.9(3) . . ? C24' N5 Zn1 125.1(4) . . ? C24 N5 Zn1 123.0(3) . . ? C2 C1 C6 116.8(3) . . ? C2 C1 C7 125.5(3) . . ? C6 C1 C7 117.6(3) . . ? C1 C2 C3 123.0(3) . . ? C1 C2 N1 120.6(2) . . ? C3 C2 N1 116.4(2) . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 118.2(3) . . ? C5 C4 C13 121.4(3) . . ? C3 C4 C13 120.4(3) . . ? C6 C5 C4 121.5(3) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 120.9(3) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 116.7(2) . . ? C8 C7 C1 123.6(3) . . ? C12 C7 C1 119.3(3) . . ? C9 C8 C7 122.7(3) . . ? C9 C8 N2 117.6(3) . . ? C7 C8 N2 119.6(2) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 119.6(3) . . ? C9 C10 C14 121.3(3) . . ? C11 C10 C14 119.1(3) . . ? C12 C11 C10 120.8(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C7 121.1(3) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? O2 C13 O1 126.2(3) . . ? O2 C13 C4 118.4(3) . . ? O1 C13 C4 115.4(3) . . ? O4 C14 O3 124.2(3) . . ? O4 C14 C10 119.9(3) . . ? O3 C14 C10 116.0(3) . . ? N3 C15 N4 111.5(3) . . ? N3 C15 H15 124.3 . . ? N4 C15 H15 124.3 . . ? C17 C16 N3 109.2(3) . . ? C17 C16 H16 125.4 . . ? N3 C16 H16 125.4 . . ? C16 C17 N4 106.9(3) . . ? C16 C17 H17 126.5 . . ? N4 C17 H17 126.5 . . ? N4 C18 C19 111.2(3) . . ? N4 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? N4 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C22 C19 C20 119.4(3) . . ? C22 C19 C18 120.0(3) . . ? C20 C19 C18 120.5(3) . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C20 120.1(4) . 2_855 ? C20 C21 H21 120.0 . . ? C20 C21 H21 120.0 2_855 . ? C19 C22 C19 120.6(4) . 2_855 ? C19 C22 H22 119.7 . . ? C19 C22 H22 119.7 2_855 . ? N6 C23 N5 113.0(6) . . ? N5 C23' N6' 113.3(6) . . ? C23 N6 C25 107.2(6) . . ? C23 N6 C26 123.2(6) . . ? C25 N6 C26 129.0(6) . . ? C25' N6' C23' 107.1(6) . . ? C25' N6' C26' 125.5(6) . . ? C23' N6' C26' 127.3(6) . . ? C25 C24 N5 108.9(6) . . ? C25' C24' N5 109.8(7) . . ? C24 C25 N6 107.6(6) . . ? N6' C25' C24' 106.5(7) . . ? C29 C26 C28 66.5(5) . . ? C29 C26 N6 107.7(8) . . ? C28 C26 N6 105.7(6) . . ? N6' C26' C28 112.0(5) . . ? N6' C26' C31 126.4(6) . . ? C28 C26' C31 48.8(3) . . ? C31 C27 C28 74.2(7) 3_655 3_655 ? C31 C27 C30 62.5(6) 3_655 . ? C28 C27 C30 136.6(8) 3_655 . ? C31 C27 C27 144.6(10) 3_655 3_655 ? C28 C27 C27 71.7(6) 3_655 3_655 ? C30 C27 C27 149.7(9) . 3_655 ? C31 C27 C28 163.6(7) 3_655 . ? C28 C27 C28 119.7(6) 3_655 . ? C30 C27 C28 102.7(6) . . ? C27 C27 C28 48.0(5) 3_655 . ? C31 C27 C29 114.5(7) 3_655 . ? C28 C27 C29 169.1(7) 3_655 . ? C30 C27 C29 52.2(5) . . ? C27 C27 C29 98.5(7) 3_655 . ? C28 C27 C29 50.7(4) . . ? C27 C28 C26 179.9(9) 3_655 . ? C27 C28 C29 129.7(6) 3_655 . ? C26 C28 C29 50.1(5) . . ? C27 C28 C31 49.5(5) 3_655 . ? C26 C28 C31 130.7(7) . . ? C29 C28 C31 178.5(5) . . ? C27 C28 C27 60.3(6) 3_655 . ? C26 C28 C27 119.6(6) . . ? C29 C28 C27 69.9(4) . . ? C31 C28 C27 109.2(5) . . ? C27 C28 C26' 119.1(5) 3_655 . ? C26 C28 C26' 61.0(6) . . ? C29 C28 C26' 110.6(5) . . ? C31 C28 C26' 70.4(5) . . ? C27 C28 C26' 178.3(5) . . ? C26 C29 C30 174.0(8) . . ? C26 C29 C28 63.3(6) . . ? C30 C29 C28 111.9(6) . . ? C26 C29 C27 122.4(8) . . ? C30 C29 C27 52.5(5) . . ? C28 C29 C27 59.5(4) . . ? C27 C31 C30 69.2(7) 3_655 3_655 ? C27 C31 C28 56.4(5) 3_655 . ? C30 C31 C28 125.5(7) 3_655 . ? C27 C31 C26' 116.4(7) 3_655 . ? C30 C31 C26' 171.4(7) 3_655 . ? C28 C31 C26' 60.8(4) . . ? C31 C30 C29 123.5(7) 3_655 . ? C31 C30 C27 48.3(5) 3_655 . ? C29 C30 C27 75.3(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.54 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.542 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.059 #=========================END data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 842369' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C56 H42 Cd2 N12 O17' _chemical_formula_sum 'C56 H42 Cd2 N12 O17' _chemical_formula_weight 1379.82 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 12.0725(7) _cell_length_b 13.2050(6) _cell_length_c 19.3094(13) _cell_angle_alpha 78.032(4) _cell_angle_beta 78.945(4) _cell_angle_gamma 77.041(3) _cell_volume 2900.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10220 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.815 _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 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16601 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10220 _reflns_number_gt 5805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0531P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10220 _refine_ls_number_parameters 773 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.864 _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 Cd1 Cd -0.19920(4) 0.99139(3) 0.44402(2) 0.03631(14) Uani 1 1 d . . . Cd2 Cd 0.12249(4) -0.13290(3) 0.87570(2) 0.03521(14) Uani 1 1 d . . . O1 O -0.2297(4) 0.8383(3) 0.5248(2) 0.0539(13) Uani 1 1 d . . . O2 O -0.0506(4) 0.8350(3) 0.4728(2) 0.0498(12) Uani 1 1 d . . . O3 O 0.0613(4) -0.0055(3) 0.7841(2) 0.0548(13) Uani 1 1 d . . . O4 O 0.0884(4) 0.0528(3) 0.8759(3) 0.0583(13) Uani 1 1 d . . . O5 O 0.2108(12) 0.4528(10) 0.6614(8) 0.0956(11) Uani 0.50 1 d PU . . O5' O 0.2169(12) 0.4193(10) 0.6366(8) 0.0956(11) Uani 0.50 1 d PU . . O6 O 0.2358(11) 0.5100(9) 0.5352(7) 0.0956(11) Uani 0.50 1 d PU . . O6' O 0.2471(10) 0.5673(9) 0.5788(7) 0.0956(11) Uani 0.50 1 d PU . . O7 O 0.0109(5) 0.5371(5) 0.7751(3) 0.0956(11) Uani 1 1 d U . . O8 O 0.0187(5) 0.4319(5) 0.8696(4) 0.0956(11) Uani 1 1 d U . . O9 O 0.2905(4) -0.2009(3) 0.8002(2) 0.0518(12) Uani 1 1 d . . . O10 O 0.1826(4) -0.3151(4) 0.8546(3) 0.0714(16) Uani 1 1 d . . . O11 O 0.7714(4) -0.9202(3) 0.5380(2) 0.0535(12) Uani 1 1 d . . . O12 O 0.6567(4) -0.8430(3) 0.4589(3) 0.0544(12) Uani 1 1 d . . . O13 O 0.2842(5) -0.6765(4) 0.8106(3) 0.090(2) Uani 1 1 d . . . O14 O 0.4646(4) -0.7320(3) 0.7846(3) 0.0735(16) Uani 1 1 d . . . O15 O 0.6748(4) -0.6178(4) 0.7562(3) 0.0602(13) Uani 1 1 d . . . O16 O 0.7527(5) -0.7786(4) 0.7506(3) 0.0765(16) Uani 1 1 d . . . N1 N 0.1792(6) 0.5026(6) 0.6027(4) 0.088(2) Uani 1 1 d U . . N2 N 0.0134(6) 0.4489(4) 0.8081(4) 0.073(2) Uani 1 1 d . . . N3 N 0.3802(5) -0.6614(4) 0.7850(3) 0.0507(15) Uani 1 1 d . . . N4 N 0.6923(5) -0.6955(4) 0.7282(3) 0.0474(14) Uani 1 1 d . . . N5 N -0.2996(4) 0.9467(4) 0.3738(3) 0.0438(14) Uani 1 1 d . . . N6 N -0.3704(4) 0.9458(4) 0.2764(3) 0.0417(13) Uani 1 1 d . . . N7 N -1.0731(4) 1.0821(3) 0.3732(3) 0.0372(12) Uani 1 1 d . . . N8 N -0.9142(5) 1.1381(4) 0.3230(3) 0.0525(15) Uani 1 1 d . . . N9 N 0.2227(4) -0.1666(4) 0.9685(3) 0.0449(14) Uani 1 1 d . . . N10 N 0.3342(4) -0.2780(4) 1.0397(3) 0.0425(13) Uani 1 1 d . . . N11 N 0.0377(4) -0.8087(4) 1.0640(3) 0.0435(13) Uani 1 1 d . . . N12 N 0.1408(5) -0.6895(4) 1.0153(3) 0.0520(15) Uani 1 1 d . . . C1 C -0.0260(6) 0.4937(4) 0.6499(4) 0.0441(17) Uani 1 1 d . . . C2 C 0.0536(5) 0.5473(5) 0.6055(4) 0.0476(18) Uani 1 1 d . . . C3 C 0.0238(6) 0.6423(5) 0.5606(4) 0.054(2) Uani 1 1 d . . . H3 H 0.0807 0.6750 0.5310 0.080 Uiso 1 1 calc . . . C4 C -0.0900(5) 0.6878(4) 0.5600(3) 0.0377(15) Uani 1 1 d . . . C5 C -0.1724(5) 0.6354(5) 0.6043(4) 0.054(2) Uani 1 1 d . . . H5 H -0.2500 0.6647 0.6045 0.080 Uiso 1 1 calc . . . C6 C -0.1401(6) 0.5402(5) 0.6481(4) 0.056(2) Uani 1 1 d . . . H6 H -0.1967 0.5066 0.6772 0.080 Uiso 1 1 calc . . . C7 C -0.1250(6) 0.7947(4) 0.5159(3) 0.0388(15) Uani 1 1 d . . . C8 C 0.0024(5) 0.3856(4) 0.6958(4) 0.0420(16) Uani 1 1 d . . . C9 C 0.0177(5) 0.3651(4) 0.7673(4) 0.0433(16) Uani 1 1 d . . . C10 C 0.0379(5) 0.2638(4) 0.8057(3) 0.0391(15) Uani 1 1 d . . . H10 H 0.0489 0.2525 0.8533 0.080 Uiso 1 1 calc . . . C11 C 0.0415(5) 0.1797(4) 0.7728(3) 0.0365(15) Uani 1 1 d . . . C12 C 0.0240(5) 0.1974(4) 0.7024(4) 0.0451(17) Uani 1 1 d . . . H12 H 0.0243 0.1409 0.6804 0.080 Uiso 1 1 calc . . . C13 C 0.0058(6) 0.3004(5) 0.6639(4) 0.0474(17) Uani 1 1 d . . . H13 H -0.0043 0.3116 0.6162 0.080 Uiso 1 1 calc . . . C14 C 0.0645(5) 0.0681(4) 0.8147(4) 0.0350(15) Uani 1 1 d . . . C15 C 0.4795(5) -0.5316(4) 0.6960(3) 0.0358(15) Uani 1 1 d . . . C16 C 0.3962(5) -0.5532(4) 0.7546(3) 0.0374(15) Uani 1 1 d . . . C17 C 0.3248(5) -0.4763(5) 0.7898(3) 0.0415(16) Uani 1 1 d . . . H17 H 0.2668 -0.4941 0.8266 0.080 Uiso 1 1 calc . . . C18 C 0.3397(5) -0.3732(4) 0.7705(3) 0.0341(14) Uani 1 1 d . . . C19 C 0.4233(5) -0.3484(4) 0.7122(3) 0.0419(16) Uani 1 1 d . . . H19 H 0.4345 -0.2792 0.6982 0.080 Uiso 1 1 calc . . . C20 C 0.4895(5) -0.4254(4) 0.6752(3) 0.0406(16) Uani 1 1 d . . . H20 H 0.5423 -0.4064 0.6353 0.080 Uiso 1 1 calc . . . C21 C 0.2657(5) -0.2903(5) 0.8110(3) 0.0377(15) Uani 1 1 d . . . C22 C 0.5444(5) -0.6099(4) 0.6489(3) 0.0339(14) Uani 1 1 d . . . C23 C 0.6401(5) -0.6886(4) 0.6647(3) 0.0346(14) Uani 1 1 d . . . C24 C 0.6885(5) -0.7632(4) 0.6217(3) 0.0391(16) Uani 1 1 d . . . H24 H 0.7507 -0.8153 0.6342 0.080 Uiso 1 1 calc . . . C25 C 0.6450(5) -0.7613(4) 0.5600(3) 0.0350(15) Uani 1 1 d . . . C26 C 0.5542(5) -0.6810(4) 0.5418(3) 0.0395(15) Uani 1 1 d . . . H26 H 0.5265 -0.6764 0.4993 0.080 Uiso 1 1 calc . . . C27 C 0.5040(5) -0.6076(4) 0.5858(4) 0.0422(16) Uani 1 1 d . . . H27 H 0.4420 -0.5555 0.5729 0.080 Uiso 1 1 calc . . . C28 C 0.6939(5) -0.8469(5) 0.5158(4) 0.0447(17) Uani 1 1 d . . . C29 C -0.3142(5) 0.9956(4) 0.3084(4) 0.0413(16) Uani 1 1 d . . . H29 H -0.2884 1.0577 0.2868 0.080 Uiso 1 1 calc . . . C30 C -0.3502(7) 0.8613(5) 0.3841(4) 0.067(2) Uani 1 1 d . . . H30 H -0.3543 0.8115 0.4258 0.080 Uiso 1 1 calc . . . C31 C -0.3933(7) 0.8590(6) 0.3257(4) 0.071(2) Uani 1 1 d . . . H31 H -0.4314 0.8083 0.3196 0.080 Uiso 1 1 calc . . . C32 C -0.3984(6) 0.9772(5) 0.2033(4) 0.0508(18) Uani 1 1 d . . . H32A H -0.3645 0.9201 0.1768 0.080 Uiso 1 1 calc . . . H32B H -0.3648 1.0380 0.1795 0.080 Uiso 1 1 calc . . . C33 C -0.5278(5) 1.0046(5) 0.2021(4) 0.0443(16) Uani 1 1 d . . . C34 C -0.6007(6) 1.0573(5) 0.2528(4) 0.0506(18) Uani 1 1 d . . . H34 H -0.5705 1.0762 0.2880 0.080 Uiso 1 1 calc . . . C35 C -0.7192(6) 1.0829(5) 0.2521(4) 0.0478(17) Uani 1 1 d . . . C36 C -0.7637(6) 1.0552(6) 0.1996(4) 0.059(2) Uani 1 1 d . . . H36 H -0.8424 1.0723 0.1985 0.080 Uiso 1 1 calc . . . C37 C -0.6908(7) 1.0019(6) 0.1483(4) 0.070(2) Uani 1 1 d . . . H37 H -0.7209 0.9831 0.1129 0.080 Uiso 1 1 calc . . . C38 C -0.5732(6) 0.9765(5) 0.1496(4) 0.0566(19) Uani 1 1 d . . . H38 H -0.5247 0.9407 0.1152 0.080 Uiso 1 1 calc . . . C39 C -0.7913(6) 1.1443(7) 0.3075(5) 0.079(3) Uani 1 1 d . . . H39A H -0.7591 1.1198 0.3517 0.080 Uiso 1 1 calc . . . H39B H -0.7852 1.2178 0.2919 0.080 Uiso 1 1 calc . . . C40 C -0.9605(5) 1.0616(5) 0.3684(4) 0.0444(17) Uani 1 1 d . . . H40 H -0.9185 1.0020 0.3932 0.080 Uiso 1 1 calc . . . C41 C -1.1002(5) 1.1765(5) 0.3292(4) 0.0450(17) Uani 1 1 d . . . H41 H -1.1743 1.2116 0.3226 0.080 Uiso 1 1 calc . . . C42 C -1.0032(7) 1.2106(5) 0.2968(4) 0.057(2) Uani 1 1 d . . . H42 H -0.9976 1.2716 0.2633 0.080 Uiso 1 1 calc . . . C43 C 0.3208(6) -0.2341(5) 0.9723(4) 0.0476(17) Uani 1 1 d . . . H43 H 0.3745 -0.2493 0.9325 0.080 Uiso 1 1 calc . . . C44 C 0.1702(6) -0.1679(5) 1.0384(4) 0.0527(18) Uani 1 1 d . . . H44 H 0.0990 -0.1280 1.0533 0.080 Uiso 1 1 calc . . . C45 C 0.2392(6) -0.2371(5) 1.0824(4) 0.0558(19) Uani 1 1 d . . . H45 H 0.2240 -0.2530 1.1321 0.080 Uiso 1 1 calc . . . C46 C 0.4224(6) -0.3686(5) 1.0618(4) 0.0516(19) Uani 1 1 d . . . H46A H 0.4451 -0.3599 1.1055 0.080 Uiso 1 1 calc . . . H46B H 0.4897 -0.3707 1.0250 0.080 Uiso 1 1 calc . . . C47 C 0.3810(5) -0.4725(5) 1.0747(4) 0.0446(17) Uani 1 1 d . . . C48 C 0.3043(5) -0.4873(5) 1.0344(4) 0.0452(17) Uani 1 1 d . . . H48 H 0.2776 -0.4326 0.9992 0.080 Uiso 1 1 calc . . . C49 C 0.2664(5) -0.5821(5) 1.0454(4) 0.0448(17) Uani 1 1 d . . . C50 C 0.3103(6) -0.6637(5) 1.0964(4) 0.058(2) Uani 1 1 d . . . H50 H 0.2880 -0.7285 1.1035 0.080 Uiso 1 1 calc . . . C51 C 0.3871(7) -0.6500(6) 1.1370(4) 0.071(2) Uani 1 1 d . . . H51 H 0.4158 -0.7051 1.1714 0.080 Uiso 1 1 calc . . . C52 C 0.4203(6) -0.5543(5) 1.1260(4) 0.062(2) Uani 1 1 d . . . H52 H 0.4706 -0.5447 1.1539 0.080 Uiso 1 1 calc . . . C53 C 0.1805(6) -0.5892(6) 1.0003(4) 0.068(2) Uani 1 1 d . . . H53A H 0.1142 -0.5331 1.0071 0.080 Uiso 1 1 calc . . . H53B H 0.2148 -0.5768 0.9503 0.080 Uiso 1 1 calc . . . C54 C 0.0529(5) -0.7134(5) 1.0638(4) 0.0456(17) Uani 1 1 d . . . H54 H 0.0077 -0.6684 1.0939 0.080 Uiso 1 1 calc . . . C55 C 0.1207(6) -0.8476(5) 1.0131(4) 0.0520(18) Uani 1 1 d . . . H55 H 0.1311 -0.9140 1.0009 0.080 Uiso 1 1 calc . . . C56 C 0.1863(6) -0.7740(7) 0.9826(4) 0.065(2) Uani 1 1 d . . . H56 H 0.2496 -0.7805 0.9467 0.080 Uiso 1 1 calc . . . O1W O 0.4449(6) 0.1877(5) 0.3994(4) 0.101(2) Uiso 1 1 d D . . H1B H 0.480(5) 0.1255(18) 0.404(3) 0.080 Uiso 1 1 d D . . H1A H 0.447(6) 0.220(4) 0.432(2) 0.080 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 Cd1 0.0440(3) 0.0270(2) 0.0351(3) -0.0027(2) -0.0060(2) -0.0034(2) Cd2 0.0397(3) 0.0231(2) 0.0393(3) -0.0007(2) -0.0046(2) -0.00419(19) O1 0.048(3) 0.042(2) 0.056(3) 0.012(2) -0.006(2) 0.003(2) O2 0.052(3) 0.040(2) 0.049(3) 0.010(2) -0.009(2) -0.006(2) O3 0.091(4) 0.024(2) 0.050(3) -0.008(2) -0.020(3) -0.003(2) O4 0.098(4) 0.030(2) 0.047(3) -0.001(2) -0.036(3) 0.004(2) O5 0.0965(12) 0.0948(12) 0.0953(12) -0.0158(4) -0.0152(4) -0.0178(5) O5' 0.0965(12) 0.0948(12) 0.0953(12) -0.0158(4) -0.0152(4) -0.0178(5) O6 0.0965(12) 0.0948(12) 0.0953(12) -0.0158(4) -0.0152(4) -0.0178(5) O6' 0.0965(12) 0.0948(12) 0.0953(12) -0.0158(4) -0.0152(4) -0.0178(5) O7 0.0965(12) 0.0948(12) 0.0953(12) -0.0158(4) -0.0152(4) -0.0178(5) O8 0.0965(12) 0.0948(12) 0.0953(12) -0.0158(4) -0.0152(4) -0.0178(5) O9 0.075(3) 0.026(2) 0.045(3) -0.003(2) -0.002(2) 0.001(2) O10 0.063(3) 0.063(3) 0.090(4) -0.044(3) 0.029(3) -0.020(3) O11 0.060(3) 0.043(3) 0.051(3) -0.015(2) -0.014(3) 0.015(2) O12 0.057(3) 0.057(3) 0.053(3) -0.026(2) -0.016(3) 0.003(2) O13 0.077(4) 0.061(3) 0.117(5) -0.009(3) 0.037(4) -0.035(3) O14 0.075(4) 0.034(3) 0.096(5) -0.001(3) 0.007(3) -0.008(3) O15 0.074(3) 0.058(3) 0.055(3) -0.023(3) -0.021(3) -0.004(3) O16 0.084(4) 0.078(4) 0.063(4) -0.025(3) -0.037(3) 0.029(3) N1 0.087(2) 0.088(2) 0.089(2) -0.0110(10) -0.0127(10) -0.0164(11) N2 0.125(6) 0.014(3) 0.076(5) 0.006(3) -0.026(4) -0.009(3) N3 0.054(4) 0.038(3) 0.054(4) -0.002(3) 0.009(3) -0.014(3) N4 0.050(4) 0.049(3) 0.043(4) -0.011(3) -0.013(3) -0.001(3) N5 0.047(3) 0.036(3) 0.051(4) -0.003(3) -0.012(3) -0.014(3) N6 0.046(3) 0.043(3) 0.039(3) -0.003(3) -0.008(3) -0.016(3) N7 0.043(3) 0.029(3) 0.037(3) 0.001(2) -0.010(3) -0.005(2) N8 0.049(4) 0.058(4) 0.054(4) -0.013(3) -0.004(3) -0.019(3) N9 0.049(3) 0.036(3) 0.047(4) -0.005(3) -0.015(3) 0.001(3) N10 0.048(3) 0.037(3) 0.044(4) -0.003(3) -0.019(3) -0.006(3) N11 0.045(3) 0.041(3) 0.045(4) -0.008(3) 0.000(3) -0.015(3) N12 0.054(4) 0.057(4) 0.051(4) 0.005(3) -0.011(3) -0.031(3) C1 0.054(4) 0.030(3) 0.047(4) 0.011(3) -0.017(4) -0.012(3) C2 0.027(3) 0.041(4) 0.062(5) 0.011(3) -0.012(3) 0.005(3) C3 0.049(4) 0.039(4) 0.061(5) 0.013(3) -0.003(4) -0.007(3) C4 0.047(4) 0.028(3) 0.037(4) 0.000(3) -0.010(3) -0.008(3) C5 0.037(4) 0.036(4) 0.076(6) 0.015(4) -0.009(4) -0.004(3) C6 0.047(4) 0.042(4) 0.067(5) 0.013(4) -0.006(4) -0.008(3) C7 0.048(4) 0.034(3) 0.035(4) -0.001(3) -0.010(3) -0.010(3) C8 0.044(4) 0.032(3) 0.043(4) 0.002(3) -0.009(3) 0.002(3) C9 0.053(4) 0.026(3) 0.049(5) -0.006(3) -0.011(3) -0.003(3) C10 0.041(4) 0.032(3) 0.041(4) 0.000(3) -0.011(3) -0.003(3) C11 0.038(4) 0.029(3) 0.038(4) -0.004(3) -0.006(3) 0.003(3) C12 0.056(4) 0.033(3) 0.041(4) -0.006(3) -0.004(3) -0.002(3) C13 0.058(4) 0.040(4) 0.038(4) -0.006(3) -0.011(3) 0.004(3) C14 0.034(4) 0.025(3) 0.039(4) -0.006(3) 0.003(3) 0.001(3) C15 0.039(4) 0.035(3) 0.033(4) -0.005(3) -0.004(3) -0.008(3) C16 0.037(4) 0.030(3) 0.043(4) -0.006(3) -0.005(3) -0.002(3) C17 0.042(4) 0.043(4) 0.042(4) -0.012(3) 0.002(3) -0.015(3) C18 0.033(3) 0.037(3) 0.030(4) -0.003(3) -0.008(3) -0.001(3) C19 0.057(4) 0.027(3) 0.040(4) -0.003(3) -0.014(3) -0.001(3) C20 0.039(4) 0.034(3) 0.041(4) -0.001(3) 0.002(3) -0.003(3) C21 0.029(4) 0.044(4) 0.037(4) -0.013(3) -0.006(3) 0.006(3) C22 0.038(4) 0.032(3) 0.029(4) -0.003(3) 0.002(3) -0.007(3) C23 0.034(3) 0.040(3) 0.029(4) -0.007(3) -0.004(3) -0.006(3) C24 0.035(4) 0.036(3) 0.048(4) -0.009(3) -0.012(3) -0.002(3) C25 0.035(4) 0.031(3) 0.036(4) -0.009(3) -0.003(3) 0.000(3) C26 0.046(4) 0.034(3) 0.038(4) -0.007(3) -0.008(3) -0.004(3) C27 0.043(4) 0.035(3) 0.042(4) 0.001(3) -0.006(3) -0.001(3) C28 0.038(4) 0.053(4) 0.044(5) -0.013(3) -0.003(3) -0.010(3) C29 0.041(4) 0.035(3) 0.047(5) -0.004(3) -0.004(3) -0.010(3) C30 0.095(6) 0.055(4) 0.062(6) 0.018(4) -0.028(5) -0.047(4) C31 0.105(7) 0.066(5) 0.058(6) 0.012(4) -0.035(5) -0.053(5) C32 0.047(4) 0.062(4) 0.042(5) -0.006(3) -0.003(3) -0.015(3) C33 0.046(4) 0.053(4) 0.034(4) -0.003(3) -0.003(3) -0.018(3) C34 0.053(4) 0.069(5) 0.039(4) -0.009(4) -0.007(4) -0.031(4) C35 0.050(4) 0.051(4) 0.048(5) -0.010(3) -0.009(4) -0.019(3) C36 0.053(5) 0.067(5) 0.062(6) -0.020(4) -0.015(4) -0.009(4) C37 0.071(6) 0.087(6) 0.064(6) -0.025(5) -0.031(5) -0.009(5) C38 0.063(5) 0.059(4) 0.050(5) -0.017(4) -0.016(4) -0.001(4) C39 0.045(5) 0.113(7) 0.100(7) -0.064(6) 0.015(5) -0.033(5) C40 0.040(4) 0.044(4) 0.049(5) -0.006(3) -0.017(3) -0.002(3) C41 0.041(4) 0.037(4) 0.050(5) 0.000(3) -0.011(3) 0.002(3) C42 0.072(5) 0.040(4) 0.053(5) 0.004(3) -0.008(4) -0.011(4) C43 0.045(4) 0.050(4) 0.046(5) -0.005(3) -0.008(4) -0.008(3) C44 0.065(5) 0.045(4) 0.048(5) -0.021(3) -0.020(4) 0.010(3) C45 0.056(5) 0.068(5) 0.042(5) -0.014(4) -0.008(4) -0.004(4) C46 0.058(4) 0.041(4) 0.062(5) -0.006(3) -0.032(4) -0.005(3) C47 0.042(4) 0.047(4) 0.045(4) -0.004(3) -0.012(3) -0.008(3) C48 0.053(4) 0.041(4) 0.044(4) 0.002(3) -0.021(4) -0.012(3) C49 0.043(4) 0.047(4) 0.046(4) 0.003(3) -0.007(3) -0.021(3) C50 0.058(5) 0.047(4) 0.067(6) 0.008(4) -0.014(4) -0.018(4) C51 0.084(6) 0.057(5) 0.070(6) 0.017(4) -0.039(5) -0.014(4) C52 0.066(5) 0.052(4) 0.069(6) 0.017(4) -0.039(4) -0.013(4) C53 0.075(5) 0.066(5) 0.071(6) 0.019(4) -0.030(5) -0.045(4) C54 0.044(4) 0.034(4) 0.062(5) -0.010(3) -0.006(4) -0.016(3) C55 0.052(4) 0.058(4) 0.050(5) -0.019(4) -0.003(4) -0.015(4) C56 0.063(5) 0.087(6) 0.046(5) -0.025(4) 0.012(4) -0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N5 2.223(5) . ? Cd1 N7 2.227(5) 1_655 ? Cd1 O11 2.287(4) 1_475 ? Cd1 O1 2.337(4) . ? Cd1 O2 2.457(4) . ? Cd1 O12 2.501(4) 1_475 ? Cd1 C7 2.722(6) . ? Cd1 C28 2.729(7) 1_475 ? Cd2 N11 2.264(5) 2_547 ? Cd2 N9 2.266(5) . ? Cd2 O3 2.283(4) . ? Cd2 O9 2.374(4) . ? Cd2 O4 2.394(4) . ? Cd2 O10 2.448(4) . ? Cd2 C14 2.667(5) . ? Cd2 C21 2.739(6) . ? O1 C7 1.261(7) . ? O2 C7 1.235(7) . ? O3 C14 1.248(7) . ? O4 C14 1.236(7) . ? O5 O5' 0.701(18) . ? O5 N1 1.269(15) . ? O5' N1 1.200(14) . ? O6 O6' 1.287(15) . ? O6 N1 1.345(14) . ? O6' N1 1.273(12) . ? O7 N2 1.202(7) . ? O8 N2 1.174(8) . ? O9 C21 1.249(7) . ? O10 C21 1.237(7) . ? O11 C28 1.254(7) . ? O11 Cd1 2.287(4) 1_635 ? O12 C28 1.252(7) . ? O12 Cd1 2.501(4) 1_635 ? O13 N3 1.213(6) . ? O14 N3 1.216(6) . ? O15 N4 1.216(6) . ? O16 N4 1.219(6) . ? N1 C2 1.493(8) . ? N2 C9 1.473(8) . ? N3 C16 1.469(7) . ? N4 C23 1.461(8) . ? N5 C29 1.319(7) . ? N5 C30 1.361(7) . ? N6 C29 1.343(7) . ? N6 C31 1.372(8) . ? N6 C32 1.469(8) . ? N7 C40 1.314(7) . ? N7 C41 1.366(7) . ? N7 Cd1 2.227(5) 1_455 ? N8 C40 1.341(8) . ? N8 C42 1.368(8) . ? N8 C39 1.473(8) . ? N9 C43 1.317(7) . ? N9 C44 1.374(8) . ? N10 C43 1.335(8) . ? N10 C45 1.353(8) . ? N10 C46 1.463(7) . ? N11 C54 1.311(7) . ? N11 C55 1.354(8) . ? N11 Cd2 2.264(5) 2_547 ? N12 C54 1.322(8) . ? N12 C56 1.352(9) . ? N12 C53 1.464(8) . ? C1 C2 1.377(8) . ? C1 C6 1.380(8) . ? C1 C8 1.522(8) . ? C2 C3 1.385(8) . ? C3 C4 1.372(8) . ? C3 H3 0.9300 . ? C4 C5 1.392(8) . ? C4 C7 1.506(7) . ? C5 C6 1.383(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.379(9) . ? C8 C9 1.391(9) . ? C9 C10 1.382(7) . ? C10 C11 1.378(8) . ? C10 H10 0.9300 . ? C11 C12 1.380(8) . ? C11 C14 1.520(7) . ? C12 C13 1.399(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.388(8) . ? C15 C20 1.403(7) . ? C15 C22 1.505(8) . ? C16 C17 1.380(8) . ? C17 C18 1.379(8) . ? C17 H17 0.9300 . ? C18 C19 1.397(8) . ? C18 C21 1.503(8) . ? C19 C20 1.379(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.389(8) . ? C22 C23 1.404(7) . ? C23 C24 1.377(8) . ? C24 C25 1.384(8) . ? C24 H24 0.9300 . ? C25 C26 1.386(7) . ? C25 C28 1.505(8) . ? C26 C27 1.382(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 Cd1 2.729(7) 1_635 ? C29 H29 0.9300 . ? C30 C31 1.337(10) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.526(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.376(9) . ? C33 C38 1.388(9) . ? C34 C35 1.396(9) . ? C34 H34 0.9300 . ? C35 C36 1.378(9) . ? C35 C39 1.499(10) . ? C36 C37 1.389(10) . ? C36 H36 0.9300 . ? C37 C38 1.387(9) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40 0.9300 . ? C41 C42 1.343(9) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C45 1.363(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.521(8) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C52 1.371(8) . ? C47 C48 1.386(8) . ? C48 C49 1.389(8) . ? C48 H48 0.9300 . ? C49 C50 1.383(8) . ? C49 C53 1.506(9) . ? C50 C51 1.386(10) . ? C50 H50 0.9300 . ? C51 C52 1.374(9) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54 0.9300 . ? C55 C56 1.359(9) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? O1W H1B 0.833(10) . ? O1W H1A 0.839(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cd1 N7 107.29(18) . 1_655 ? N5 Cd1 O11 139.60(18) . 1_475 ? N7 Cd1 O11 96.53(17) 1_655 1_475 ? N5 Cd1 O1 87.44(17) . . ? N7 Cd1 O1 147.51(16) 1_655 . ? O11 Cd1 O1 89.47(16) 1_475 . ? N5 Cd1 O2 105.59(16) . . ? N7 Cd1 O2 93.26(15) 1_655 . ? O11 Cd1 O2 105.08(15) 1_475 . ? O1 Cd1 O2 54.48(14) . . ? N5 Cd1 O12 92.06(16) . 1_475 ? N7 Cd1 O12 91.55(16) 1_655 1_475 ? O11 Cd1 O12 54.40(14) 1_475 1_475 ? O1 Cd1 O12 117.29(16) . 1_475 ? O2 Cd1 O12 159.37(16) . 1_475 ? N5 Cd1 C7 98.00(18) . . ? N7 Cd1 C7 120.07(18) 1_655 . ? O11 Cd1 C7 97.52(17) 1_475 . ? O1 Cd1 C7 27.53(16) . . ? O2 Cd1 C7 26.96(16) . . ? O12 Cd1 C7 141.50(19) 1_475 . ? N5 Cd1 C28 116.86(19) . 1_475 ? N7 Cd1 C28 94.13(18) 1_655 1_475 ? O11 Cd1 C28 27.16(16) 1_475 1_475 ? O1 Cd1 C28 104.95(18) . 1_475 ? O2 Cd1 C28 132.22(19) . 1_475 ? O12 Cd1 C28 27.25(16) 1_475 1_475 ? C7 Cd1 C28 121.1(2) . 1_475 ? N11 Cd2 N9 97.99(19) 2_547 . ? N11 Cd2 O3 105.14(17) 2_547 . ? N9 Cd2 O3 143.49(16) . . ? N11 Cd2 O9 136.21(17) 2_547 . ? N9 Cd2 O9 90.49(18) . . ? O3 Cd2 O9 91.88(15) . . ? N11 Cd2 O4 107.00(18) 2_547 . ? N9 Cd2 O4 91.11(16) . . ? O3 Cd2 O4 55.44(15) . . ? O9 Cd2 O4 115.74(16) . . ? N11 Cd2 O10 82.81(17) 2_547 . ? N9 Cd2 O10 92.15(18) . . ? O3 Cd2 O10 118.19(17) . . ? O9 Cd2 O10 53.87(14) . . ? O4 Cd2 O10 169.12(17) . . ? N11 Cd2 C14 109.20(17) 2_547 . ? N9 Cd2 C14 117.28(19) . . ? O3 Cd2 C14 27.86(17) . . ? O9 Cd2 C14 104.48(16) . . ? O4 Cd2 C14 27.61(16) . . ? O10 Cd2 C14 145.1(2) . . ? N11 Cd2 C21 109.26(19) 2_547 . ? N9 Cd2 C21 92.87(18) . . ? O3 Cd2 C21 105.32(17) . . ? O9 Cd2 C21 27.09(15) . . ? O4 Cd2 C21 142.55(19) . . ? O10 Cd2 C21 26.85(16) . . ? C14 Cd2 C21 126.10(19) . . ? C7 O1 Cd1 93.5(3) . . ? C7 O2 Cd1 88.6(4) . . ? C14 O3 Cd2 93.4(4) . . ? C14 O4 Cd2 88.6(3) . . ? O5' O5 N1 68.1(19) . . ? O5 O5' N1 79.1(19) . . ? O6' O6 N1 57.8(8) . . ? N1 O6' O6 63.4(8) . . ? C21 O9 Cd2 93.0(4) . . ? C21 O10 Cd2 89.8(4) . . ? C28 O11 Cd1 96.5(4) . 1_635 ? C28 O12 Cd1 86.6(4) . 1_635 ? O5' N1 O5 32.8(8) . . ? O5' N1 O6' 117.3(11) . . ? O5 N1 O6' 104.7(10) . . ? O5' N1 O6 109.0(11) . . ? O5 N1 O6 131.0(11) . . ? O6' N1 O6 58.8(7) . . ? O5' N1 C2 123.5(10) . . ? O5 N1 C2 115.8(9) . . ? O6' N1 C2 116.6(8) . . ? O6 N1 C2 112.4(8) . . ? O8 N2 O7 119.8(7) . . ? O8 N2 C9 122.8(5) . . ? O7 N2 C9 117.3(7) . . ? O13 N3 O14 122.8(5) . . ? O13 N3 C16 118.8(6) . . ? O14 N3 C16 118.4(5) . . ? O15 N4 O16 122.6(6) . . ? O15 N4 C23 118.6(5) . . ? O16 N4 C23 118.8(6) . . ? C29 N5 C30 104.6(5) . . ? C29 N5 Cd1 125.5(4) . . ? C30 N5 Cd1 129.7(4) . . ? C29 N6 C31 105.6(6) . . ? C29 N6 C32 126.7(5) . . ? C31 N6 C32 127.7(5) . . ? C40 N7 C41 105.9(5) . . ? C40 N7 Cd1 128.3(4) . 1_455 ? C41 N7 Cd1 125.5(4) . 1_455 ? C40 N8 C42 106.8(5) . . ? C40 N8 C39 126.1(6) . . ? C42 N8 C39 127.1(6) . . ? C43 N9 C44 105.0(5) . . ? C43 N9 Cd2 124.4(5) . . ? C44 N9 Cd2 122.7(4) . . ? C43 N10 C45 107.1(5) . . ? C43 N10 C46 125.9(6) . . ? C45 N10 C46 125.9(6) . . ? C54 N11 C55 106.0(5) . . ? C54 N11 Cd2 121.7(4) . 2_547 ? C55 N11 Cd2 131.1(4) . 2_547 ? C54 N12 C56 107.7(6) . . ? C54 N12 C53 125.6(7) . . ? C56 N12 C53 126.7(6) . . ? C2 C1 C6 116.3(5) . . ? C2 C1 C8 125.0(6) . . ? C6 C1 C8 118.6(5) . . ? C1 C2 C3 123.2(5) . . ? C1 C2 N1 120.3(5) . . ? C3 C2 N1 116.4(6) . . ? C4 C3 C2 119.7(6) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 118.3(5) . . ? C3 C4 C7 120.9(5) . . ? C5 C4 C7 120.7(5) . . ? C6 C5 C4 120.7(6) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C1 C6 C5 121.7(6) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? O2 C7 O1 123.4(5) . . ? O2 C7 C4 118.9(6) . . ? O1 C7 C4 117.8(5) . . ? O2 C7 Cd1 64.5(3) . . ? O1 C7 Cd1 59.0(3) . . ? C4 C7 Cd1 176.0(5) . . ? C13 C8 C9 117.5(5) . . ? C13 C8 C1 115.9(6) . . ? C9 C8 C1 126.5(6) . . ? C10 C9 C8 122.3(6) . . ? C10 C9 N2 114.8(6) . . ? C8 C9 N2 122.9(5) . . ? C11 C10 C9 119.4(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.8(5) . . ? C10 C11 C14 119.5(6) . . ? C12 C11 C14 120.6(6) . . ? C11 C12 C13 120.0(6) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 121.0(6) . . ? C8 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? O4 C14 O3 122.5(5) . . ? O4 C14 C11 120.0(5) . . ? O3 C14 C11 117.5(6) . . ? O4 C14 Cd2 63.8(3) . . ? O3 C14 Cd2 58.7(3) . . ? C11 C14 Cd2 173.6(4) . . ? C16 C15 C20 115.7(6) . . ? C16 C15 C22 124.5(5) . . ? C20 C15 C22 119.2(5) . . ? C17 C16 C15 123.3(5) . . ? C17 C16 N3 114.9(6) . . ? C15 C16 N3 121.8(5) . . ? C18 C17 C16 120.0(6) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 118.3(6) . . ? C17 C18 C21 120.0(5) . . ? C19 C18 C21 121.6(5) . . ? C20 C19 C18 120.7(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C15 121.8(6) . . ? C19 C20 H20 119.1 . . ? C15 C20 H20 119.1 . . ? O10 C21 O9 123.0(6) . . ? O10 C21 C18 117.5(6) . . ? O9 C21 C18 119.4(6) . . ? O10 C21 Cd2 63.3(3) . . ? O9 C21 Cd2 59.9(3) . . ? C18 C21 Cd2 175.5(4) . . ? C27 C22 C23 116.8(6) . . ? C27 C22 C15 117.7(5) . . ? C23 C22 C15 125.5(5) . . ? C24 C23 C22 121.9(6) . . ? C24 C23 N4 116.8(5) . . ? C22 C23 N4 121.3(5) . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 118.4(6) . . ? C24 C25 C28 120.0(5) . . ? C26 C25 C28 121.6(6) . . ? C27 C26 C25 121.1(6) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C22 121.3(5) . . ? C26 C27 H27 119.3 . . ? C22 C27 H27 119.3 . . ? O12 C28 O11 122.5(6) . . ? O12 C28 C25 119.7(6) . . ? O11 C28 C25 117.8(6) . . ? O12 C28 Cd1 66.2(4) . 1_635 ? O11 C28 Cd1 56.4(3) . 1_635 ? C25 C28 Cd1 174.0(5) . 1_635 ? N5 C29 N6 112.5(5) . . ? N5 C29 H29 123.8 . . ? N6 C29 H29 123.8 . . ? C31 C30 N5 110.5(6) . . ? C31 C30 H30 124.7 . . ? N5 C30 H30 124.7 . . ? C30 C31 N6 106.8(6) . . ? C30 C31 H31 126.6 . . ? N6 C31 H31 126.6 . . ? N6 C32 C33 112.4(5) . . ? N6 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? N6 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C38 119.3(6) . . ? C34 C33 C32 120.6(6) . . ? C38 C33 C32 120.1(7) . . ? C33 C34 C35 121.0(6) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C36 C35 C34 119.4(7) . . ? C36 C35 C39 123.2(7) . . ? C34 C35 C39 117.3(6) . . ? C35 C36 C37 120.0(7) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.2(7) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C33 120.1(7) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? N8 C39 C35 116.0(6) . . ? N8 C39 H39A 108.3 . . ? C35 C39 H39A 108.3 . . ? N8 C39 H39B 108.3 . . ? C35 C39 H39B 108.3 . . ? H39A C39 H39B 107.4 . . ? N7 C40 N8 111.1(5) . . ? N7 C40 H40 124.4 . . ? N8 C40 H40 124.4 . . ? C42 C41 N7 109.5(5) . . ? C42 C41 H41 125.3 . . ? N7 C41 H41 125.3 . . ? C41 C42 N8 106.6(5) . . ? C41 C42 H42 126.7 . . ? N8 C42 H42 126.7 . . ? N9 C43 N10 112.2(6) . . ? N9 C43 H43 123.9 . . ? N10 C43 H43 123.9 . . ? C45 C44 N9 109.2(6) . . ? C45 C44 H44 125.4 . . ? N9 C44 H44 125.4 . . ? N10 C45 C44 106.6(6) . . ? N10 C45 H45 126.7 . . ? C44 C45 H45 126.7 . . ? N10 C46 C47 112.4(5) . . ? N10 C46 H46A 109.1 . . ? C47 C46 H46A 109.1 . . ? N10 C46 H46B 109.1 . . ? C47 C46 H46B 109.1 . . ? H46A C46 H46B 107.9 . . ? C52 C47 C48 118.5(6) . . ? C52 C47 C46 120.4(6) . . ? C48 C47 C46 121.1(5) . . ? C47 C48 C49 121.5(6) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C50 C49 C48 118.3(6) . . ? C50 C49 C53 124.4(6) . . ? C48 C49 C53 117.4(5) . . ? C49 C50 C51 120.8(6) . . ? C49 C50 H50 119.6 . . ? C51 C50 H50 119.6 . . ? C52 C51 C50 119.3(6) . . ? C52 C51 H51 120.3 . . ? C50 C51 H51 120.3 . . ? C47 C52 C51 121.5(6) . . ? C47 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? N12 C53 C49 115.3(5) . . ? N12 C53 H53A 108.4 . . ? C49 C53 H53A 108.4 . . ? N12 C53 H53B 108.4 . . ? C49 C53 H53B 108.4 . . ? H53A C53 H53B 107.5 . . ? N11 C54 N12 111.2(6) . . ? N11 C54 H54 124.4 . . ? N12 C54 H54 124.4 . . ? N11 C55 C56 109.1(6) . . ? N11 C55 H55 125.4 . . ? C56 C55 H55 125.4 . . ? N12 C56 C55 105.9(6) . . ? N12 C56 H56 127.0 . . ? C55 C56 H56 127.0 . . ? H1B O1W H1A 115(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.460 _refine_diff_density_min -1.170 _refine_diff_density_rms 0.100 #=========================END data_compound-7 _database_code_depnum_ccdc_archive 'CCDC 842370' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C34 H24 Mn N6 O8' _chemical_formula_sum 'C34 H24 Mn N6 O8' _chemical_formula_weight 699.53 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' Mn Mn 0.3368 0.7283 '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 9.6753(19) _cell_length_b 14.259(3) _cell_length_c 22.739(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.16(3) _cell_angle_gamma 90.00 _cell_volume 3066.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6957 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 0.496 _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 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 28496 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6957 _reflns_number_gt 5337 _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 SHELXP-97 _computing_publication_material 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^)+(0.0566P)^2^+3.6794P] 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 6957 _refine_ls_number_parameters 445 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.097 _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 Mn1 Mn 0.0000 1.0000 0.5000 0.02345(13) Uani 1 2 d S . . Mn2 Mn -0.5000 1.0000 0.5000 0.02729(14) Uani 1 2 d S . . O1 O -0.3402(2) 1.11246(12) 0.52609(9) 0.0374(4) Uani 1 1 d . . . O2 O -0.1540(2) 1.11457(12) 0.48202(9) 0.0364(4) Uani 1 1 d . . . O3 O -0.14816(19) 1.90850(12) 0.53358(8) 0.0337(4) Uani 1 1 d . . . O4 O -0.35779(19) 1.89904(12) 0.46884(9) 0.0356(4) Uani 1 1 d . . . O5 O -0.4264(3) 1.40611(15) 0.62552(10) 0.0549(6) Uani 1 1 d . . . O6 O -0.4512(2) 1.52756(14) 0.56794(11) 0.0496(6) Uani 1 1 d . . . O7 O -0.1826(6) 1.6212(5) 0.6645(3) 0.0720(8) Uani 0.50 1 d PU A 1 O7' O -0.1175(6) 1.6208(5) 0.6674(3) 0.0720(8) Uani 0.50 1 d PU A 2 O8 O -0.0215(7) 1.5153(5) 0.6222(3) 0.0720(8) Uani 0.50 1 d PU A 1 O8' O -0.0803(7) 1.5109(5) 0.6305(3) 0.0720(8) Uani 0.50 1 d PU A 2 N1 N -0.4031(3) 1.44928(15) 0.58236(11) 0.0371(5) Uani 1 1 d . . . N2 N -0.1245(4) 1.58130(17) 0.62278(12) 0.0543(8) Uani 1 1 d . . . N3 N -0.0849(2) 0.95270(15) 0.40619(10) 0.0332(5) Uani 1 1 d . . . N4 N -0.2173(2) 0.95720(16) 0.31482(10) 0.0354(5) Uani 1 1 d . . . N5 N -1.4365(2) 0.56132(16) 0.09247(11) 0.0379(5) Uani 1 1 d . . . N6 N -1.3033(3) 0.57684(17) 0.18324(11) 0.0423(6) Uani 1 1 d . . . C1 C -0.2296(3) 1.45674(17) 0.51575(12) 0.0317(5) Uani 1 1 d . A . C2 C -0.3148(3) 1.40361(17) 0.54561(11) 0.0302(5) Uani 1 1 d . . . C3 C -0.3225(3) 1.30659(16) 0.54229(11) 0.0291(5) Uani 1 1 d . . . H3 H -0.3829 1.2740 0.5619 0.080 Uiso 1 1 calc . . . C4 C -0.2394(2) 1.25838(16) 0.50947(11) 0.0261(5) Uani 1 1 d . . . C5 C -0.1509(3) 1.30923(17) 0.48050(13) 0.0343(6) Uani 1 1 d . . . H5 H -0.0924 1.2777 0.4594 0.080 Uiso 1 1 calc . . . C6 C -0.1487(3) 1.40657(18) 0.48270(13) 0.0375(6) Uani 1 1 d . . . H6 H -0.0916 1.4391 0.4615 0.080 Uiso 1 1 calc . . . C7 C -0.2453(2) 1.15189(16) 0.50561(11) 0.0262(5) Uani 1 1 d . . . C8 C -0.2253(3) 1.56155(17) 0.51401(12) 0.0320(5) Uani 1 1 d . . . C9 C -0.1831(3) 1.62019(18) 0.56363(12) 0.0338(6) Uani 1 1 d . A . C10 C -0.1895(3) 1.71689(17) 0.55974(12) 0.0328(6) Uani 1 1 d . . . H10 H -0.1599 1.7534 0.5940 0.080 Uiso 1 1 calc . . . C11 C -0.2401(3) 1.75903(17) 0.50481(11) 0.0288(5) Uani 1 1 d . A . C12 C -0.2791(3) 1.70303(18) 0.45440(12) 0.0371(6) Uani 1 1 d . . . H12 H -0.3123 1.7306 0.4170 0.080 Uiso 1 1 calc . . . C13 C -0.2692(3) 1.60590(18) 0.45899(13) 0.0382(6) Uani 1 1 d . A . H13 H -0.2927 1.5698 0.4243 0.080 Uiso 1 1 calc . . . C14 C -0.2498(3) 1.86501(16) 0.50169(11) 0.0272(5) Uani 1 1 d . . . C15 C -0.1985(3) 0.98915(18) 0.37146(12) 0.0334(6) Uani 1 1 d . . . H15 H -0.2583 1.0317 0.3846 0.080 Uiso 1 1 calc . . . C16 C -0.0289(3) 0.8938(2) 0.36935(14) 0.0463(7) Uani 1 1 d . . . H16 H 0.0525 0.8580 0.3813 0.080 Uiso 1 1 calc . . . C17 C -0.1098(4) 0.8958(2) 0.31309(14) 0.0489(8) Uani 1 1 d . . . H17 H -0.0953 0.8621 0.2799 0.080 Uiso 1 1 calc . . . C18 C -0.3349(3) 0.9805(2) 0.26546(13) 0.0421(7) Uani 1 1 d . . . H18A H -0.3009 0.9827 0.2283 0.080 Uiso 1 1 calc . . . H18B H -0.3700 1.0424 0.2723 0.080 Uiso 1 1 calc . . . C19 C -0.4550(3) 0.91091(19) 0.25862(12) 0.0350(6) Uani 1 1 d . . . C20 C -0.4761(3) 0.8568(2) 0.30624(13) 0.0480(8) Uani 1 1 d . . . H20 H -0.4119 0.8600 0.3429 0.080 Uiso 1 1 calc . . . C21 C -0.5917(4) 0.7977(2) 0.30001(14) 0.0488(8) Uani 1 1 d . . . H21 H -0.6027 0.7610 0.3326 0.080 Uiso 1 1 calc . . . C22 C -0.6919(3) 0.79148(18) 0.24646(12) 0.0345(6) Uani 1 1 d . . . C23 C -0.6684(3) 0.8451(2) 0.19853(13) 0.0445(7) Uani 1 1 d . . . H23 H -0.7322 0.8418 0.1618 0.080 Uiso 1 1 calc . . . C24 C -0.5521(3) 0.9033(2) 0.20442(13) 0.0455(7) Uani 1 1 d . . . H24 H -0.5386 0.9380 0.1715 0.080 Uiso 1 1 calc . . . C25 C -0.8192(3) 0.73183(18) 0.24241(12) 0.0336(6) Uani 1 1 d . . . C26 C -0.8882(3) 0.69035(19) 0.18852(12) 0.0369(6) Uani 1 1 d . . . H26 H -0.8536 0.6997 0.1538 0.080 Uiso 1 1 calc . . . C27 C -1.0074(3) 0.63546(19) 0.18612(13) 0.0391(6) Uani 1 1 d . . . H27 H -1.0511 0.6078 0.1499 0.080 Uiso 1 1 calc . . . C28 C -1.0625(3) 0.62119(19) 0.23694(13) 0.0376(6) Uani 1 1 d . . . C29 C -0.9944(3) 0.6624(2) 0.29064(13) 0.0408(6) Uani 1 1 d . . . H29 H -1.0298 0.6536 0.3252 0.080 Uiso 1 1 calc . . . C30 C -0.8748(3) 0.7162(2) 0.29319(12) 0.0403(6) Uani 1 1 d . . . H30 H -0.8304 0.7426 0.3297 0.080 Uiso 1 1 calc . . . C31 C -1.1893(4) 0.5586(2) 0.23554(15) 0.0516(8) Uani 1 1 d . . . H31A H -1.1602 0.4936 0.2348 0.080 Uiso 1 1 calc . . . H31B H -1.2245 0.5683 0.2720 0.080 Uiso 1 1 calc . . . C32 C -1.3352(3) 0.5241(2) 0.13347(14) 0.0414(7) Uani 1 1 d . . . H32 H -1.2907 0.4677 0.1285 0.080 Uiso 1 1 calc . . . C33 C -1.4704(3) 0.6431(2) 0.11781(16) 0.0516(8) Uani 1 1 d . . . H33 H -1.5394 0.6853 0.0993 0.080 Uiso 1 1 calc . . . C34 C -1.3892(4) 0.6537(3) 0.17343(16) 0.0565(9) Uani 1 1 d . . . H34 H -1.3914 0.7033 0.1998 0.080 Uiso 1 1 calc . . . 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 Mn1 0.0242(3) 0.0162(2) 0.0296(3) -0.00315(18) 0.00479(19) -0.00051(18) Mn2 0.0248(3) 0.0176(2) 0.0391(3) 0.0033(2) 0.0060(2) 0.00157(19) O1 0.0353(10) 0.0213(9) 0.0573(12) -0.0010(8) 0.0137(9) -0.0046(7) O2 0.0388(11) 0.0212(9) 0.0513(11) -0.0011(8) 0.0141(9) 0.0083(7) O3 0.0331(10) 0.0233(9) 0.0441(11) 0.0007(7) 0.0070(8) -0.0070(7) O4 0.0312(10) 0.0256(9) 0.0491(11) 0.0002(8) 0.0062(8) 0.0064(7) O5 0.0841(17) 0.0435(12) 0.0471(13) 0.0047(10) 0.0368(12) 0.0109(11) O6 0.0614(14) 0.0256(10) 0.0697(15) -0.0003(9) 0.0312(12) 0.0110(9) O7 0.0731(10) 0.0721(9) 0.0705(9) 0.0022(5) 0.0141(5) 0.0011(5) O7' 0.0731(10) 0.0721(9) 0.0705(9) 0.0022(5) 0.0141(5) 0.0011(5) O8 0.0731(10) 0.0721(9) 0.0705(9) 0.0022(5) 0.0141(5) 0.0011(5) O8' 0.0731(10) 0.0721(9) 0.0705(9) 0.0022(5) 0.0141(5) 0.0011(5) N1 0.0488(14) 0.0245(11) 0.0415(13) -0.0037(9) 0.0175(11) 0.0026(10) N2 0.092(2) 0.0242(12) 0.0411(14) 0.0025(10) 0.0014(14) -0.0057(13) N3 0.0329(12) 0.0328(12) 0.0332(11) -0.0061(9) 0.0051(9) -0.0025(9) N4 0.0313(12) 0.0387(13) 0.0337(12) -0.0020(9) 0.0014(9) -0.0036(9) N5 0.0345(12) 0.0331(12) 0.0457(14) -0.0074(10) 0.0076(10) -0.0058(9) N6 0.0385(13) 0.0412(14) 0.0451(14) -0.0051(10) 0.0037(11) -0.0105(11) C1 0.0389(15) 0.0177(12) 0.0386(14) 0.0002(10) 0.0082(11) 0.0005(10) C2 0.0377(14) 0.0208(11) 0.0335(13) -0.0008(9) 0.0111(11) 0.0044(10) C3 0.0325(13) 0.0211(11) 0.0346(13) 0.0009(9) 0.0093(10) 0.0015(9) C4 0.0243(12) 0.0188(11) 0.0341(13) -0.0012(9) 0.0040(9) 0.0016(9) C5 0.0352(14) 0.0221(12) 0.0493(16) -0.0042(10) 0.0169(12) -0.0009(10) C6 0.0413(16) 0.0243(13) 0.0518(17) -0.0003(11) 0.0207(13) -0.0038(11) C7 0.0249(12) 0.0180(11) 0.0333(13) -0.0012(9) 0.0008(9) 0.0008(9) C8 0.0391(15) 0.0184(11) 0.0392(14) 0.0000(10) 0.0099(11) -0.0002(10) C9 0.0428(15) 0.0236(12) 0.0345(13) 0.0033(10) 0.0070(11) -0.0028(11) C10 0.0417(15) 0.0223(12) 0.0347(13) -0.0028(10) 0.0088(11) -0.0038(10) C11 0.0279(12) 0.0189(11) 0.0402(14) 0.0000(9) 0.0084(10) -0.0004(9) C12 0.0472(17) 0.0246(13) 0.0372(14) 0.0036(10) 0.0034(12) -0.0017(11) C13 0.0527(17) 0.0233(13) 0.0378(14) -0.0038(10) 0.0075(12) -0.0031(11) C14 0.0278(12) 0.0186(11) 0.0374(13) 0.0006(9) 0.0119(10) -0.0005(9) C15 0.0317(13) 0.0331(13) 0.0351(14) -0.0033(10) 0.0062(11) -0.0019(10) C16 0.0433(17) 0.0517(18) 0.0409(16) -0.0121(13) 0.0021(13) 0.0140(14) C17 0.0500(18) 0.058(2) 0.0362(15) -0.0135(13) 0.0034(13) 0.0120(15) C18 0.0394(16) 0.0440(16) 0.0373(15) 0.0069(12) -0.0043(12) -0.0062(12) C19 0.0331(14) 0.0356(14) 0.0337(14) 0.0000(11) 0.0013(11) -0.0008(11) C20 0.0478(18) 0.0528(19) 0.0353(15) 0.0099(13) -0.0098(13) -0.0126(14) C21 0.0485(18) 0.0526(19) 0.0385(16) 0.0150(13) -0.0062(13) -0.0136(14) C22 0.0349(14) 0.0308(13) 0.0347(14) -0.0016(10) 0.0004(11) 0.0006(11) C23 0.0428(16) 0.0562(19) 0.0297(14) 0.0023(12) -0.0034(12) -0.0084(14) C24 0.0444(17) 0.0587(19) 0.0313(14) 0.0078(13) 0.0029(12) -0.0101(14) C25 0.0331(14) 0.0285(13) 0.0361(14) -0.0001(10) 0.0006(11) 0.0029(10) C26 0.0416(16) 0.0339(14) 0.0334(14) -0.0016(11) 0.0039(11) -0.0005(11) C27 0.0443(16) 0.0328(14) 0.0359(14) -0.0041(11) -0.0015(12) -0.0022(12) C28 0.0384(15) 0.0302(13) 0.0405(15) 0.0027(11) -0.0003(12) -0.0003(11) C29 0.0441(16) 0.0407(16) 0.0365(15) -0.0002(12) 0.0057(12) -0.0020(12) C30 0.0425(16) 0.0420(16) 0.0331(14) -0.0061(11) 0.0004(12) -0.0025(12) C31 0.053(2) 0.0514(19) 0.0454(17) 0.0063(14) -0.0013(14) -0.0147(15) C32 0.0427(16) 0.0328(14) 0.0470(17) -0.0060(12) 0.0058(13) -0.0055(12) C33 0.0421(17) 0.0472(18) 0.060(2) -0.0180(15) -0.0013(14) 0.0067(14) C34 0.052(2) 0.054(2) 0.060(2) -0.0246(16) 0.0026(16) 0.0050(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 2.1906(18) . ? Mn1 O2 2.1906(18) 3_576 ? Mn1 O3 2.1912(18) 1_545 ? Mn1 O3 2.1912(18) 3_586 ? Mn1 N3 2.223(2) 3_576 ? Mn1 N3 2.223(2) . ? Mn2 O4 2.2086(18) 3_486 ? Mn2 O4 2.2086(18) 1_545 ? Mn2 O1 2.2196(18) 3_476 ? Mn2 O1 2.2196(18) . ? Mn2 N5 2.240(2) 4_676 ? Mn2 N5 2.240(2) 2_355 ? O1 C7 1.247(3) . ? O2 C7 1.246(3) . ? O3 C14 1.256(3) . ? O3 Mn1 2.1912(18) 1_565 ? O4 C14 1.248(3) . ? O4 Mn2 2.2086(18) 1_565 ? O5 N1 1.219(3) . ? O6 N1 1.227(3) . ? O7 N2 1.329(7) . ? O7' N2 1.149(7) . ? O8 N2 1.372(7) . ? O8' N2 1.090(7) . ? N1 C2 1.467(3) . ? N2 C9 1.455(4) . ? N3 C15 1.318(3) . ? N3 C16 1.375(4) . ? N4 C15 1.342(3) . ? N4 C17 1.366(4) . ? N4 C18 1.458(3) . ? N5 C32 1.314(4) . ? N5 C33 1.371(4) . ? N5 Mn2 2.240(2) 2_345 ? N6 C32 1.340(4) . ? N6 C34 1.365(4) . ? N6 C31 1.465(4) . ? C1 C6 1.392(4) . ? C1 C2 1.397(4) . ? C1 C8 1.496(3) . ? C2 C3 1.387(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9300 . ? C4 C5 1.390(4) . ? C4 C7 1.521(3) . ? C5 C6 1.389(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.386(4) . ? C8 C9 1.395(4) . ? C9 C10 1.382(4) . ? C10 C11 1.380(4) . ? C10 H10 0.9300 . ? C11 C12 1.383(4) . ? C11 C14 1.515(3) . ? C12 C13 1.391(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.352(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.511(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.380(4) . ? C19 C24 1.388(4) . ? C20 C21 1.384(4) . ? C20 H20 0.9300 . ? C21 C22 1.390(4) . ? C21 H21 0.9300 . ? C22 C23 1.389(4) . ? C22 C25 1.484(4) . ? C23 C24 1.382(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.391(4) . ? C25 C26 1.397(4) . ? C26 C27 1.386(4) . ? C26 H26 0.9300 . ? C27 C28 1.386(4) . ? C27 H27 0.9300 . ? C28 C29 1.390(4) . ? C28 C31 1.512(4) . ? C29 C30 1.380(4) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32 0.9300 . ? C33 C34 1.349(5) . ? C33 H33 0.9300 . ? C34 H34 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 O2 Mn1 O2 180.000(1) . 3_576 ? O2 Mn1 O3 92.29(7) . 1_545 ? O2 Mn1 O3 87.71(7) 3_576 1_545 ? O2 Mn1 O3 87.71(7) . 3_586 ? O2 Mn1 O3 92.29(7) 3_576 3_586 ? O3 Mn1 O3 180.0 1_545 3_586 ? O2 Mn1 N3 92.99(8) . 3_576 ? O2 Mn1 N3 87.01(8) 3_576 3_576 ? O3 Mn1 N3 89.01(8) 1_545 3_576 ? O3 Mn1 N3 90.99(8) 3_586 3_576 ? O2 Mn1 N3 87.01(8) . . ? O2 Mn1 N3 92.99(8) 3_576 . ? O3 Mn1 N3 90.99(8) 1_545 . ? O3 Mn1 N3 89.01(8) 3_586 . ? N3 Mn1 N3 180.000(1) 3_576 . ? O4 Mn2 O4 180.00(9) 3_486 1_545 ? O4 Mn2 O1 96.36(7) 3_486 3_476 ? O4 Mn2 O1 83.64(7) 1_545 3_476 ? O4 Mn2 O1 83.64(7) 3_486 . ? O4 Mn2 O1 96.36(7) 1_545 . ? O1 Mn2 O1 180.000(1) 3_476 . ? O4 Mn2 N5 91.12(8) 3_486 4_676 ? O4 Mn2 N5 88.88(8) 1_545 4_676 ? O1 Mn2 N5 90.39(8) 3_476 4_676 ? O1 Mn2 N5 89.61(8) . 4_676 ? O4 Mn2 N5 88.88(8) 3_486 2_355 ? O4 Mn2 N5 91.12(8) 1_545 2_355 ? O1 Mn2 N5 89.61(8) 3_476 2_355 ? O1 Mn2 N5 90.39(8) . 2_355 ? N5 Mn2 N5 180.000(1) 4_676 2_355 ? C7 O1 Mn2 138.74(17) . . ? C7 O2 Mn1 138.98(17) . . ? C14 O3 Mn1 125.65(16) . 1_565 ? C14 O4 Mn2 124.15(17) . 1_565 ? O5 N1 O6 123.4(2) . . ? O5 N1 C2 117.6(2) . . ? O6 N1 C2 119.0(2) . . ? O8' N2 O7' 111.1(5) . . ? O8' N2 O7 119.3(5) . . ? O7' N2 O7 27.8(4) . . ? O8' N2 O8 27.2(4) . . ? O7' N2 O8 115.9(5) . . ? O7 N2 O8 135.9(4) . . ? O8' N2 C9 124.3(4) . . ? O7' N2 C9 124.6(4) . . ? O7 N2 C9 110.9(4) . . ? O8 N2 C9 113.2(4) . . ? C15 N3 C16 105.2(2) . . ? C15 N3 Mn1 123.25(18) . . ? C16 N3 Mn1 131.03(19) . . ? C15 N4 C17 107.2(2) . . ? C15 N4 C18 126.0(2) . . ? C17 N4 C18 126.8(2) . . ? C32 N5 C33 104.7(2) . . ? C32 N5 Mn2 121.61(19) . 2_345 ? C33 N5 Mn2 133.2(2) . 2_345 ? C32 N6 C34 106.8(3) . . ? C32 N6 C31 125.9(3) . . ? C34 N6 C31 127.1(3) . . ? C6 C1 C2 116.1(2) . . ? C6 C1 C8 118.5(2) . . ? C2 C1 C8 125.3(2) . . ? C3 C2 C1 123.0(2) . . ? C3 C2 N1 116.3(2) . . ? C1 C2 N1 120.7(2) . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 C7 120.4(2) . . ? C5 C4 C7 120.9(2) . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 121.8(2) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? O2 C7 O1 127.8(2) . . ? O2 C7 C4 115.4(2) . . ? O1 C7 C4 116.8(2) . . ? C13 C8 C9 116.0(2) . . ? C13 C8 C1 118.3(2) . . ? C9 C8 C1 125.6(2) . . ? C10 C9 C8 123.0(2) . . ? C10 C9 N2 116.3(2) . . ? C8 C9 N2 120.7(2) . . ? C11 C10 C9 119.7(2) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 118.8(2) . . ? C10 C11 C14 118.9(2) . . ? C12 C11 C14 122.3(2) . . ? C11 C12 C13 120.7(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C8 C13 C12 121.7(2) . . ? C8 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? O4 C14 O3 127.5(2) . . ? O4 C14 C11 116.9(2) . . ? O3 C14 C11 115.6(2) . . ? N3 C15 N4 111.6(2) . . ? N3 C15 H15 124.2 . . ? N4 C15 H15 124.2 . . ? C17 C16 N3 109.9(3) . . ? C17 C16 H16 125.1 . . ? N3 C16 H16 125.1 . . ? C16 C17 N4 106.2(3) . . ? C16 C17 H17 126.9 . . ? N4 C17 H17 126.9 . . ? N4 C18 C19 112.8(2) . . ? N4 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? N4 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C24 118.0(3) . . ? C20 C19 C18 121.6(2) . . ? C24 C19 C18 120.3(3) . . ? C19 C20 C21 120.7(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 121.9(3) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C23 C22 C21 117.0(3) . . ? C23 C22 C25 122.5(2) . . ? C21 C22 C25 120.5(3) . . ? C24 C23 C22 121.3(3) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C19 121.2(3) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? C30 C25 C26 117.6(3) . . ? C30 C25 C22 120.1(2) . . ? C26 C25 C22 122.3(3) . . ? C27 C26 C25 120.9(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 120.9(3) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 118.4(3) . . ? C27 C28 C31 121.5(3) . . ? C29 C28 C31 120.0(3) . . ? C30 C29 C28 120.7(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C25 121.5(3) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? N6 C31 C28 112.4(3) . . ? N6 C31 H31A 109.1 . . ? C28 C31 H31A 109.1 . . ? N6 C31 H31B 109.1 . . ? C28 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? N5 C32 N6 112.1(3) . . ? N5 C32 H32 123.9 . . ? N6 C32 H32 123.9 . . ? C34 C33 N5 110.2(3) . . ? C34 C33 H33 124.9 . . ? N5 C33 H33 124.9 . . ? C33 C34 N6 106.1(3) . . ? C33 C34 H34 126.9 . . ? N6 C34 H34 126.9 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.403 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.064 #=========================END data_compound-8 _database_code_depnum_ccdc_archive 'CCDC 842371' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C68 H48 Cd2 N12 O16' _chemical_formula_sum 'C68 H48 Cd2 N12 O16' _chemical_formula_weight 1513.98 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2582(19) _cell_length_b 13.590(3) _cell_length_c 25.513(5) _cell_angle_alpha 86.71(3) _cell_angle_beta 87.74(3) _cell_angle_gamma 85.16(3) _cell_volume 3191.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10782 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.747 _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 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 23953 _diffrn_reflns_av_R_equivalents 0.1097 _diffrn_reflns_av_sigmaI/netI 0.1982 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10782 _reflns_number_gt 5693 _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 SHELXP-97 _computing_publication_material 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^)+(0.1011P)^2^+8.4068P] 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 10782 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1877 _refine_ls_R_factor_gt 0.1066 _refine_ls_wR_factor_ref 0.2526 _refine_ls_wR_factor_gt 0.2143 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Cd1 Cd 0.46658(10) 0.98018(6) 0.24853(3) 0.0588(3) Uani 1 1 d . . . Cd2 Cd 1.10335(10) 0.46334(6) 0.74368(3) 0.0571(3) Uani 1 1 d . . . O1 O 1.0334(10) 0.3238(6) 0.7928(3) 0.078(3) Uani 1 1 d . . . O2 O 1.0351(10) 0.4555(6) 0.8351(3) 0.079(3) Uani 1 1 d . . . O3 O 0.6864(9) 0.0014(6) 1.1999(3) 0.074(2) Uani 1 1 d . . . O4 O 0.4898(9) -0.0019(6) 1.1559(3) 0.075(2) Uani 1 1 d . . . O5 O 0.8657(10) 0.4459(6) 1.0178(3) 0.078(3) Uani 1 1 d . . . O6 O 0.9019(10) 0.3125(6) 1.0661(3) 0.078(3) Uani 1 1 d . . . O7 O 1.1173(11) 0.1168(8) 1.1118(4) 0.114(4) Uani 1 1 d . . . O8 O 1.1391(10) 0.1197(7) 1.0282(4) 0.102(3) Uani 1 1 d . . . O9 O 0.8814(9) 0.4805(6) 0.6956(3) 0.070(2) Uani 1 1 d . . . O10 O 1.0927(10) 0.4856(6) 0.6519(3) 0.070(2) Uani 1 1 d . . . O11 O 0.5508(10) 0.8324(6) 0.2920(3) 0.076(2) Uani 1 1 d . . . O12 O 0.5192(11) 0.9628(6) 0.3390(3) 0.083(3) Uani 1 1 d . . . O13 O 0.4371(10) 0.5793(8) 0.6054(4) 0.101(3) Uani 1 1 d . . . O14 O 0.4385(9) 0.6060(7) 0.5222(4) 0.087(3) Uani 1 1 d . . . O15 O 0.6283(10) 0.9316(6) 0.5232(3) 0.076(3) Uani 1 1 d . . . O16 O 0.6162(10) 0.7934(6) 0.5670(3) 0.073(2) Uani 1 1 d . . . N1 N 0.8978(10) 0.3565(7) 1.0231(4) 0.059(3) Uani 1 1 d . . . N2 N 1.0649(12) 0.1164(8) 1.0694(5) 0.075(3) Uani 1 1 d . . . N3 N 0.5007(12) 0.5916(7) 0.5634(4) 0.066(3) Uani 1 1 d . . . N4 N 0.6238(9) 0.8437(7) 0.5259(4) 0.056(2) Uani 1 1 d . . . N5 N 1.3338(11) 0.4053(8) 0.7482(4) 0.073(3) Uani 1 1 d . . . N6 N 1.5208(12) 0.3275(8) 0.7888(4) 0.071(3) Uani 1 1 d . . . N7 N 1.3910(11) 0.1390(7) 1.2567(4) 0.065(3) Uani 1 1 d . . . N8 N 1.3150(11) 0.2924(7) 1.2340(4) 0.068(3) Uani 1 1 d . . . N9 N 1.1362(12) 0.6223(7) 0.7497(4) 0.077(3) Uani 1 1 d . . . N10 N 1.1809(12) 0.7755(7) 0.7284(4) 0.072(3) Uani 1 1 d . . . N11 N 1.2447(10) 0.9265(7) 0.2487(4) 0.065(3) Uani 1 1 d . . . N12 N 1.0607(11) 0.8467(7) 0.2836(4) 0.058(2) Uani 1 1 d . . . C1 C 0.9014(13) 0.2014(8) 0.9760(4) 0.057(3) Uani 1 1 d . . . C2 C 0.9237(11) 0.2999(8) 0.9758(4) 0.052(3) Uani 1 1 d . . . C3 C 0.9620(13) 0.3554(8) 0.9304(4) 0.058(3) Uani 1 1 d . . . H3 H 0.9721 0.4227 0.9315 0.080 Uiso 1 1 calc . . . C4 C 0.9845(12) 0.3093(8) 0.8844(4) 0.054(3) Uani 1 1 d . . . C5 C 0.9592(14) 0.2105(9) 0.8832(4) 0.067(3) Uani 1 1 d . . . H5 H 0.9727 0.1787 0.8518 0.080 Uiso 1 1 calc . . . C6 C 0.9142(15) 0.1592(8) 0.9282(5) 0.076(4) Uani 1 1 d . . . H6 H 0.8918 0.0941 0.9261 0.080 Uiso 1 1 calc . . . C7 C 1.0156(13) 0.3688(10) 0.8341(4) 0.060(3) Uani 1 1 d . . . C8 C 0.8358(14) 0.1435(7) 1.0223(4) 0.056(3) Uani 1 1 d . . . C9 C 0.9085(14) 0.1057(8) 1.0661(5) 0.064(3) Uani 1 1 d . . . C10 C 0.8453(15) 0.0619(8) 1.1091(4) 0.065(3) Uani 1 1 d . . . H10 H 0.8991 0.0403 1.1381 0.080 Uiso 1 1 calc . . . C11 C 0.6962(13) 0.0502(7) 1.1084(4) 0.054(3) Uani 1 1 d . . . C12 C 0.6202(14) 0.0808(9) 1.0642(5) 0.071(4) Uani 1 1 d . . . H12 H 0.5221 0.0712 1.0631 0.080 Uiso 1 1 calc . . . C13 C 0.6884(13) 0.1253(8) 1.0219(4) 0.061(3) Uani 1 1 d . . . H13 H 0.6362 0.1440 0.9920 0.080 Uiso 1 1 calc . . . C14 C 0.6200(14) 0.0119(8) 1.1582(5) 0.059(3) Uani 1 1 d . . . C15 C 0.7363(13) 0.6303(7) 0.5191(4) 0.054(3) Uani 1 1 d . . . C16 C 0.6614(13) 0.5853(7) 0.5616(4) 0.052(3) Uani 1 1 d . . . C17 C 0.7310(12) 0.5413(7) 0.6043(4) 0.052(3) Uani 1 1 d . . . H17 H 0.6780 0.5150 0.6327 0.080 Uiso 1 1 calc . . . C18 C 0.8811(13) 0.5364(7) 0.6048(4) 0.049(3) Uani 1 1 d . . . C19 C 0.9588(12) 0.5745(8) 0.5622(4) 0.054(3) Uani 1 1 d . . . H19 H 1.0597 0.5689 0.5614 0.080 Uiso 1 1 calc . . . C20 C 0.8844(12) 0.6210(7) 0.5208(4) 0.050(3) Uani 1 1 d . . . H20 H 0.9376 0.6474 0.4925 0.080 Uiso 1 1 calc . . . C21 C 0.9553(15) 0.4965(8) 0.6547(5) 0.058(3) Uani 1 1 d . . . C22 C 0.6685(12) 0.6930(7) 0.4741(4) 0.052(3) Uani 1 1 d . . . C23 C 0.6203(10) 0.7918(7) 0.4767(4) 0.044(3) Uani 1 1 d . . . C24 C 0.5799(11) 0.8501(7) 0.4323(4) 0.051(3) Uani 1 1 d . . . H24 H 0.5498 0.9167 0.4352 0.080 Uiso 1 1 calc . . . C25 C 0.5844(11) 0.8091(8) 0.3842(4) 0.050(3) Uani 1 1 d . . . C26 C 0.6313(13) 0.7099(8) 0.3807(4) 0.060(3) Uani 1 1 d . . . H26 H 0.6345 0.6817 0.3482 0.080 Uiso 1 1 calc . . . C27 C 0.6735(13) 0.6523(7) 0.4248(4) 0.056(3) Uani 1 1 d . . . H27 H 0.7055 0.5861 0.4217 0.080 Uiso 1 1 calc . . . C28 C 0.5502(12) 0.8743(9) 0.3342(5) 0.059(3) Uani 1 1 d . . . C29 C 1.3755(14) 0.3358(9) 0.7854(5) 0.068(3) Uani 1 1 d . . . H29 H 1.3126 0.2986 0.8059 0.080 Uiso 1 1 calc . . . C30 C 1.4638(18) 0.4375(10) 0.7283(5) 0.080(4) Uani 1 1 d . . . H30 H 1.4717 0.4862 0.7015 0.080 Uiso 1 1 calc . . . C31 C 1.5771(15) 0.3898(13) 0.7528(5) 0.089(5) Uani 1 1 d . . . H31 H 1.6748 0.3984 0.7460 0.080 Uiso 1 1 calc . . . C32 C 1.6031(14) 0.2612(10) 0.8288(5) 0.079(4) Uani 1 1 d . . . H32A H 1.5897 0.1925 0.8234 0.080 Uiso 1 1 calc . . . H32B H 1.7059 0.2702 0.8249 0.080 Uiso 1 1 calc . . . C33 C 1.5484(13) 0.2865(9) 0.8828(5) 0.062(3) Uani 1 1 d . . . C34 C 1.4433(17) 0.2344(10) 0.9087(5) 0.082(4) Uani 1 1 d . . . H34 H 1.4033 0.1849 0.8917 0.080 Uiso 1 1 calc . . . C35 C 1.3973(14) 0.2540(10) 0.9582(6) 0.078(4) Uani 1 1 d . . . H35 H 1.3278 0.2163 0.9748 0.080 Uiso 1 1 calc . . . C36 C 1.4496(12) 0.3278(9) 0.9851(5) 0.058(3) Uani 1 1 d . . . C37 C 1.5560(13) 0.3808(9) 0.9586(5) 0.062(3) Uani 1 1 d . . . H37 H 1.5954 0.4307 0.9754 0.080 Uiso 1 1 calc . . . C38 C 1.6031(13) 0.3612(9) 0.9089(5) 0.067(3) Uani 1 1 d . . . H38 H 1.6731 0.3984 0.8922 0.080 Uiso 1 1 calc . . . C39 C 1.4063(13) 0.3472(8) 1.0396(5) 0.060(3) Uani 1 1 d . . . C40 C 1.2654(15) 0.3499(9) 1.0575(5) 0.075(4) Uani 1 1 d . . . H40 H 1.1950 0.3428 1.0333 0.080 Uiso 1 1 calc . . . C41 C 1.2205(14) 0.3624(10) 1.1083(6) 0.081(4) Uani 1 1 d . . . H41 H 1.1226 0.3623 1.1180 0.080 Uiso 1 1 calc . . . C42 C 1.3199(18) 0.3752(9) 1.1450(5) 0.076(4) Uani 1 1 d . . . C43 C 1.4601(18) 0.3764(9) 1.1293(6) 0.081(4) Uani 1 1 d . . . H43 H 1.5283 0.3869 1.1538 0.080 Uiso 1 1 calc . . . C44 C 1.5053(14) 0.3627(10) 1.0783(6) 0.074(4) Uani 1 1 d . . . H44 H 1.6034 0.3636 1.0690 0.080 Uiso 1 1 calc . . . C45 C 1.2715(15) 0.3829(9) 1.2010(5) 0.077(4) Uani 1 1 d . . . H45A H 1.3125 0.4390 1.2149 0.080 Uiso 1 1 calc . . . H45B H 1.1668 0.3950 1.2031 0.080 Uiso 1 1 calc . . . C46 C 1.3621(15) 0.2030(9) 1.2167(4) 0.070(4) Uani 1 1 d . . . H46 H 1.3728 0.1883 1.1815 0.080 Uiso 1 1 calc . . . C47 C 1.3601(17) 0.1887(12) 1.3005(5) 0.091(5) Uani 1 1 d . . . H47 H 1.3696 0.1618 1.3347 0.080 Uiso 1 1 calc . . . C48 C 1.3131(18) 0.2837(11) 1.2873(5) 0.095(5) Uani 1 1 d . . . H48 H 1.2851 0.3332 1.3102 0.080 Uiso 1 1 calc . . . C49 C 1.1570(15) 0.6894(9) 0.7117(5) 0.076(4) Uani 1 1 d . . . H49 H 1.1549 0.6769 0.6763 0.080 Uiso 1 1 calc . . . C50 C 1.1525(17) 0.6728(11) 0.7946(5) 0.087(4) Uani 1 1 d . . . H50 H 1.1459 0.6457 0.8288 0.080 Uiso 1 1 calc . . . C51 C 1.1790(16) 0.7665(10) 0.7811(5) 0.082(4) Uani 1 1 d . . . H51 H 1.1933 0.8156 0.8039 0.080 Uiso 1 1 calc . . . C52 C 1.2074(17) 0.8679(9) 0.6975(5) 0.088(5) Uani 1 1 d . . . H52A H 1.3083 0.8809 0.6998 0.080 Uiso 1 1 calc . . . H52B H 1.1481 0.9226 0.7121 0.080 Uiso 1 1 calc . . . C53 C 1.1722(18) 0.8612(8) 0.6403(5) 0.070(4) Uani 1 1 d . . . C54 C 1.0315(17) 0.8682(10) 0.6247(6) 0.082(4) Uani 1 1 d . . . H54 H 0.9554 0.8808 0.6489 0.080 Uiso 1 1 calc . . . C55 C 1.0035(13) 0.8565(9) 0.5729(6) 0.070(4) Uani 1 1 d . . . H55 H 0.9072 0.8590 0.5634 0.080 Uiso 1 1 calc . . . C56 C 1.1094(13) 0.8414(7) 0.5347(5) 0.054(3) Uani 1 1 d . . . C57 C 1.2477(16) 0.8395(11) 0.5509(6) 0.087(4) Uani 1 1 d . . . H57 H 1.3235 0.8310 0.5262 0.080 Uiso 1 1 calc . . . C58 C 1.2813(16) 0.8496(10) 0.6031(6) 0.086(4) Uani 1 1 d . . . H58 H 1.3775 0.8484 0.6125 0.080 Uiso 1 1 calc . . . C59 C 1.0799(12) 0.8269(8) 0.4797(4) 0.055(3) Uani 1 1 d . . . C60 C 1.1590(14) 0.7556(9) 0.4517(5) 0.066(3) Uani 1 1 d . . . H60 H 1.2357 0.7182 0.4676 0.080 Uiso 1 1 calc . . . C61 C 1.1274(15) 0.7381(8) 0.4005(5) 0.075(4) Uani 1 1 d . . . H61 H 1.1811 0.6888 0.3826 0.080 Uiso 1 1 calc . . . C62 C 1.0143(13) 0.7954(8) 0.3761(5) 0.058(3) Uani 1 1 d . . . C63 C 0.9366(13) 0.8663(9) 0.4028(5) 0.062(3) Uani 1 1 d . . . H63 H 0.8608 0.9040 0.3865 0.080 Uiso 1 1 calc . . . C64 C 0.9674(13) 0.8838(8) 0.4538(5) 0.064(3) Uani 1 1 d . . . H64 H 0.9133 0.9336 0.4712 0.080 Uiso 1 1 calc . . . C65 C 0.9825(13) 0.7802(9) 0.3200(5) 0.068(3) Uani 1 1 d . . . H65A H 1.0108 0.7121 0.3121 0.080 Uiso 1 1 calc . . . H65B H 0.8790 0.7925 0.3151 0.080 Uiso 1 1 calc . . . C66 C 1.2057(15) 0.8566(10) 0.2838(5) 0.080(4) Uani 1 1 d . . . H66 H 1.2696 0.8192 0.3058 0.080 Uiso 1 1 calc . . . C67 C 1.1213(19) 0.9605(9) 0.2260(5) 0.085(4) Uani 1 1 d . . . H67 H 1.1144 1.0092 0.1989 0.080 Uiso 1 1 calc . . . C68 C 1.0108(15) 0.9157(11) 0.2473(5) 0.081(4) Uani 1 1 d . . . H68 H 0.9143 0.9295 0.2386 0.080 Uiso 1 1 calc . . . 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 0.0701(6) 0.0541(5) 0.0498(5) 0.0182(4) 0.0004(4) -0.0058(4) Cd2 0.0736(6) 0.0502(5) 0.0467(5) 0.0116(4) -0.0061(4) -0.0080(4) O1 0.124(8) 0.062(5) 0.045(5) 0.014(4) 0.020(5) -0.019(5) O2 0.122(8) 0.045(5) 0.065(5) 0.020(4) 0.002(5) 0.001(5) O3 0.074(6) 0.095(6) 0.051(5) 0.027(5) 0.004(5) -0.005(5) O4 0.066(6) 0.095(7) 0.065(5) -0.001(5) 0.000(5) -0.021(5) O5 0.120(8) 0.050(5) 0.064(5) 0.000(4) 0.001(5) -0.007(5) O6 0.110(7) 0.071(6) 0.051(5) 0.008(4) 0.001(5) -0.008(5) O7 0.086(7) 0.144(10) 0.108(8) 0.056(7) -0.027(7) -0.023(6) O8 0.064(6) 0.118(8) 0.116(8) 0.039(7) 0.024(6) 0.003(5) O9 0.092(6) 0.066(5) 0.050(5) 0.014(4) -0.005(5) 0.000(5) O10 0.068(6) 0.076(6) 0.063(5) 0.003(4) -0.008(5) 0.005(5) O11 0.110(7) 0.062(5) 0.052(5) 0.005(4) -0.001(5) 0.006(5) O12 0.143(9) 0.048(5) 0.058(5) 0.013(4) -0.025(5) -0.005(5) O13 0.079(7) 0.132(9) 0.085(7) 0.040(6) 0.023(6) -0.012(6) O14 0.078(6) 0.092(7) 0.089(7) 0.030(5) -0.022(6) -0.017(5) O15 0.110(7) 0.045(5) 0.074(6) -0.008(4) -0.007(5) 0.002(5) O16 0.108(7) 0.068(5) 0.041(4) 0.006(4) -0.006(5) 0.009(5) N1 0.067(6) 0.052(6) 0.057(6) 0.016(5) -0.002(5) -0.019(5) N2 0.069(8) 0.071(7) 0.081(8) 0.034(6) 0.003(7) -0.002(6) N3 0.077(8) 0.058(6) 0.061(7) 0.021(5) -0.004(6) -0.009(5) N4 0.051(6) 0.062(7) 0.052(6) -0.008(5) 0.000(5) 0.013(5) N5 0.077(7) 0.097(8) 0.043(6) 0.010(5) -0.006(6) -0.011(6) N6 0.076(8) 0.081(7) 0.054(6) -0.009(5) 0.013(6) 0.000(6) N7 0.089(8) 0.064(6) 0.042(5) 0.007(5) -0.005(5) -0.011(5) N8 0.083(7) 0.052(6) 0.066(7) -0.001(5) 0.012(6) 0.005(5) N9 0.105(9) 0.046(6) 0.079(8) 0.001(6) -0.008(7) -0.003(6) N10 0.107(9) 0.058(7) 0.054(6) 0.000(5) -0.010(6) -0.018(6) N11 0.054(6) 0.090(8) 0.049(6) 0.020(5) -0.003(5) -0.003(5) N12 0.063(7) 0.058(6) 0.053(6) 0.000(5) 0.000(5) -0.014(5) C1 0.076(8) 0.043(7) 0.049(7) 0.010(5) 0.001(6) 0.008(6) C2 0.049(7) 0.054(7) 0.048(7) 0.004(6) 0.005(5) 0.013(5) C3 0.072(8) 0.053(7) 0.050(7) 0.009(6) -0.003(6) -0.006(6) C4 0.061(7) 0.046(7) 0.053(7) 0.013(6) 0.004(6) -0.001(5) C5 0.103(10) 0.061(8) 0.035(6) 0.001(6) 0.005(6) -0.004(7) C6 0.113(11) 0.036(7) 0.074(9) 0.007(6) 0.016(8) -0.001(7) C7 0.065(8) 0.063(8) 0.044(7) 0.019(6) 0.019(6) 0.015(6) C8 0.086(9) 0.039(6) 0.041(6) 0.006(5) 0.007(6) 0.001(6) C9 0.071(9) 0.048(7) 0.072(9) 0.010(6) 0.003(7) -0.004(6) C10 0.105(11) 0.040(6) 0.047(7) 0.013(5) 0.001(7) -0.003(7) C11 0.068(8) 0.039(6) 0.054(7) 0.006(5) 0.007(6) 0.002(6) C12 0.085(9) 0.063(8) 0.065(8) 0.025(7) -0.009(7) -0.015(7) C13 0.067(8) 0.064(8) 0.051(7) 0.014(6) -0.013(6) -0.013(6) C14 0.057(8) 0.053(7) 0.063(8) 0.001(6) 0.018(7) 0.005(6) C15 0.084(9) 0.034(6) 0.045(6) 0.005(5) -0.017(6) 0.004(6) C16 0.070(8) 0.039(6) 0.047(6) 0.008(5) 0.001(6) -0.004(5) C17 0.062(8) 0.045(6) 0.048(6) 0.006(5) 0.009(6) -0.010(5) C18 0.074(8) 0.037(6) 0.034(6) 0.000(5) 0.004(6) 0.004(5) C19 0.056(7) 0.046(6) 0.059(7) 0.002(5) -0.006(6) 0.001(5) C20 0.053(7) 0.048(6) 0.046(6) 0.010(5) 0.005(6) 0.004(5) C21 0.085(10) 0.042(7) 0.048(7) 0.005(5) -0.012(7) -0.015(6) C22 0.062(7) 0.038(6) 0.056(7) 0.012(5) -0.013(6) -0.009(5) C23 0.039(6) 0.044(6) 0.048(6) 0.004(5) 0.004(5) -0.004(5) C24 0.054(7) 0.045(6) 0.053(7) 0.013(5) -0.007(6) -0.004(5) C25 0.055(7) 0.046(7) 0.048(7) 0.013(5) -0.005(6) -0.007(5) C26 0.082(9) 0.054(7) 0.042(6) -0.001(5) -0.005(6) -0.003(6) C27 0.084(8) 0.033(6) 0.053(7) 0.003(5) -0.005(6) -0.007(5) C28 0.061(8) 0.058(8) 0.055(8) 0.018(6) -0.007(6) 0.000(6) C29 0.059(8) 0.084(9) 0.060(8) 0.006(7) -0.003(7) -0.009(7) C30 0.106(12) 0.069(9) 0.064(9) 0.017(7) 0.023(9) -0.025(8) C31 0.068(9) 0.140(14) 0.057(9) 0.001(9) 0.024(8) -0.014(9) C32 0.074(9) 0.083(9) 0.075(9) 0.006(7) -0.019(8) 0.021(7) C33 0.048(7) 0.055(8) 0.080(9) 0.011(7) 0.007(7) 0.009(6) C34 0.107(12) 0.080(10) 0.063(9) -0.002(7) -0.032(9) -0.021(8) C35 0.075(9) 0.078(10) 0.084(10) 0.016(8) -0.023(8) -0.032(7) C36 0.043(7) 0.073(8) 0.055(7) 0.021(6) 0.008(6) -0.005(6) C37 0.056(7) 0.064(8) 0.065(8) -0.006(6) -0.003(7) 0.008(6) C38 0.072(9) 0.055(8) 0.071(9) 0.012(7) -0.005(7) -0.005(6) C39 0.062(8) 0.050(7) 0.066(8) 0.009(6) -0.006(7) 0.002(6) C40 0.073(10) 0.073(9) 0.076(10) -0.007(7) 0.001(8) 0.008(7) C41 0.060(9) 0.099(11) 0.081(10) 0.020(8) 0.006(8) -0.007(7) C42 0.097(11) 0.051(8) 0.073(9) 0.014(7) -0.002(9) 0.019(7) C43 0.103(12) 0.062(9) 0.074(10) -0.002(7) -0.013(9) 0.020(8) C44 0.067(9) 0.078(9) 0.077(10) -0.005(8) 0.008(8) -0.006(7) C45 0.094(10) 0.055(8) 0.079(9) 0.002(7) -0.008(8) 0.006(7) C46 0.112(11) 0.064(8) 0.031(6) 0.005(6) 0.006(7) 0.004(7) C47 0.120(13) 0.098(11) 0.050(8) 0.001(8) -0.019(8) 0.018(9) C48 0.136(14) 0.090(11) 0.055(9) -0.013(8) 0.019(9) 0.003(10) C49 0.112(11) 0.050(8) 0.067(9) -0.002(7) -0.002(8) -0.020(7) C50 0.134(13) 0.076(10) 0.051(8) 0.011(7) -0.001(8) -0.029(9) C51 0.114(12) 0.076(10) 0.061(9) -0.017(7) -0.002(8) -0.028(8) C52 0.147(14) 0.064(8) 0.060(8) 0.010(7) -0.014(9) -0.041(9) C53 0.098(11) 0.044(7) 0.069(9) 0.001(6) -0.005(9) -0.012(7) C54 0.093(11) 0.085(10) 0.069(9) -0.005(8) 0.026(9) -0.021(8) C55 0.048(7) 0.081(9) 0.084(10) -0.015(8) 0.006(7) -0.009(6) C56 0.053(7) 0.035(6) 0.072(8) 0.005(5) 0.000(7) -0.001(5) C57 0.085(11) 0.101(11) 0.075(10) 0.001(8) 0.005(9) -0.013(8) C58 0.079(10) 0.089(11) 0.093(11) -0.003(9) -0.025(9) -0.012(8) C59 0.060(7) 0.052(7) 0.050(7) 0.004(6) 0.011(6) -0.006(6) C60 0.076(9) 0.060(8) 0.061(8) 0.017(6) -0.001(7) -0.019(7) C61 0.101(10) 0.047(7) 0.075(9) 0.011(6) -0.002(8) -0.010(7) C62 0.060(8) 0.051(7) 0.062(8) 0.010(6) -0.008(7) -0.017(6) C63 0.064(8) 0.059(8) 0.062(8) 0.007(6) -0.005(7) -0.010(6) C64 0.067(8) 0.041(7) 0.084(9) 0.001(6) 0.002(7) -0.012(6) C65 0.062(8) 0.064(8) 0.079(9) 0.018(7) -0.005(7) -0.022(6) C66 0.087(10) 0.077(9) 0.073(9) 0.032(7) -0.005(8) -0.013(8) C67 0.128(13) 0.061(8) 0.068(9) 0.020(7) -0.021(9) -0.030(9) C68 0.078(10) 0.107(11) 0.059(8) 0.009(8) -0.036(8) -0.002(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N7 2.231(10) 1_464 ? Cd1 N11 2.236(10) 1_455 ? Cd1 O11 2.328(7) . ? Cd1 O4 2.366(8) 1_564 ? Cd1 O3 2.372(8) 1_564 ? Cd1 O12 2.372(7) . ? Cd1 C28 2.651(10) . ? Cd1 C14 2.692(12) 1_564 ? Cd2 N5 2.216(10) . ? Cd2 N9 2.222(10) . ? Cd2 O1 2.335(7) . ? Cd2 O10 2.349(8) . ? Cd2 O2 2.390(8) . ? Cd2 O9 2.423(8) . ? Cd2 C21 2.694(11) . ? Cd2 C7 2.706(11) . ? O1 C7 1.247(13) . ? O2 C7 1.210(14) . ? O3 C14 1.245(13) . ? O3 Cd1 2.372(8) 1_546 ? O4 C14 1.239(13) . ? O4 Cd1 2.366(8) 1_546 ? O5 N1 1.227(10) . ? O6 N1 1.219(10) . ? O7 N2 1.202(13) . ? O8 N2 1.235(13) . ? O9 C21 1.243(13) . ? O10 C21 1.268(14) . ? O11 C28 1.245(13) . ? O12 C28 1.226(13) . ? O13 N3 1.213(12) . ? O14 N3 1.216(11) . ? O15 N4 1.196(11) . ? O16 N4 1.221(11) . ? N1 C2 1.469(14) . ? N2 C9 1.473(15) . ? N3 C16 1.483(14) . ? N4 C23 1.477(13) . ? N5 C29 1.342(14) . ? N5 C30 1.384(16) . ? N6 C31 1.335(16) . ? N6 C29 1.346(14) . ? N6 C32 1.509(14) . ? N7 C46 1.324(13) . ? N7 C47 1.347(15) . ? N7 Cd1 2.231(10) 1_646 ? N8 C46 1.349(14) . ? N8 C48 1.356(15) . ? N8 C45 1.486(14) . ? N9 C49 1.313(14) . ? N9 C50 1.386(16) . ? N10 C49 1.306(14) . ? N10 C51 1.345(15) . ? N10 C52 1.476(14) . ? N11 C66 1.330(14) . ? N11 C67 1.337(16) . ? N11 Cd1 2.236(10) 1_655 ? N12 C68 1.346(14) . ? N12 C66 1.361(15) . ? N12 C65 1.471(14) . ? C1 C2 1.372(15) . ? C1 C6 1.375(16) . ? C1 C8 1.516(14) . ? C2 C3 1.397(14) . ? C3 C4 1.361(15) . ? C3 H3 0.9300 . ? C4 C5 1.384(15) . ? C4 C7 1.509(14) . ? C5 C6 1.378(15) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.380(15) . ? C8 C13 1.408(15) . ? C9 C10 1.353(15) . ? C10 C11 1.404(16) . ? C10 H10 0.9300 . ? C11 C12 1.380(15) . ? C11 C14 1.515(15) . ? C12 C13 1.365(15) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 Cd1 2.692(11) 1_546 ? C15 C20 1.368(15) . ? C15 C16 1.401(14) . ? C15 C22 1.514(13) . ? C16 C17 1.370(14) . ? C17 C18 1.386(14) . ? C17 H17 0.9300 . ? C18 C19 1.381(14) . ? C18 C21 1.520(14) . ? C19 C20 1.376(13) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C23 1.384(13) . ? C22 C27 1.400(14) . ? C23 C24 1.389(13) . ? C24 C25 1.376(14) . ? C24 H24 0.9300 . ? C25 C26 1.388(14) . ? C25 C28 1.539(13) . ? C26 C27 1.384(14) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.341(18) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.498(17) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.376(17) . ? C33 C38 1.386(17) . ? C34 C35 1.352(18) . ? C34 H34 0.9300 . ? C35 C36 1.377(16) . ? C35 H35 0.9300 . ? C36 C37 1.399(15) . ? C36 C39 1.465(16) . ? C37 C38 1.357(16) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.364(16) . ? C39 C44 1.410(16) . ? C40 C41 1.361(17) . ? C40 H40 0.9300 . ? C41 C42 1.367(18) . ? C41 H41 0.9300 . ? C42 C43 1.345(19) . ? C42 C45 1.486(17) . ? C43 C44 1.369(18) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46 0.9300 . ? C47 C48 1.355(18) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C51 1.340(17) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.517(16) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C58 1.363(18) . ? C53 C54 1.371(18) . ? C54 C55 1.377(17) . ? C54 H54 0.9300 . ? C55 C56 1.365(16) . ? C55 H55 0.9300 . ? C56 C57 1.359(17) . ? C56 C59 1.469(15) . ? C57 C58 1.396(18) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 C60 1.380(16) . ? C59 C64 1.407(15) . ? C60 C61 1.387(16) . ? C60 H60 0.9300 . ? C61 C62 1.396(16) . ? C61 H61 0.9300 . ? C62 C63 1.354(16) . ? C62 C65 1.501(16) . ? C63 C64 1.381(16) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66 0.9300 . ? C67 C68 1.317(18) . ? C67 H67 0.9300 . ? C68 H68 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 N7 Cd1 N11 95.7(4) 1_464 1_455 ? N7 Cd1 O11 145.8(3) 1_464 . ? N11 Cd1 O11 89.6(3) 1_455 . ? N7 Cd1 O4 93.5(3) 1_464 1_564 ? N11 Cd1 O4 94.3(3) 1_455 1_564 ? O11 Cd1 O4 119.8(3) . 1_564 ? N7 Cd1 O3 98.8(3) 1_464 1_564 ? N11 Cd1 O3 146.4(3) 1_455 1_564 ? O11 Cd1 O3 95.0(3) . 1_564 ? O4 Cd1 O3 54.8(3) 1_564 1_564 ? N7 Cd1 O12 90.5(3) 1_464 . ? N11 Cd1 O12 101.8(3) 1_455 . ? O11 Cd1 O12 55.5(3) . . ? O4 Cd1 O12 163.0(3) 1_564 . ? O3 Cd1 O12 108.2(3) 1_564 . ? N7 Cd1 C28 117.9(4) 1_464 . ? N11 Cd1 C28 95.8(3) 1_455 . ? O11 Cd1 C28 28.0(3) . . ? O4 Cd1 C28 145.8(4) 1_564 . ? O3 Cd1 C28 103.8(3) 1_564 . ? O12 Cd1 C28 27.5(3) . . ? N7 Cd1 C14 95.0(3) 1_464 1_564 ? N11 Cd1 C14 121.2(4) 1_455 1_564 ? O11 Cd1 C14 111.0(3) . 1_564 ? O4 Cd1 C14 27.4(3) 1_564 1_564 ? O3 Cd1 C14 27.5(3) 1_564 1_564 ? O12 Cd1 C14 135.7(4) . 1_564 ? C28 Cd1 C14 128.1(4) . 1_564 ? N5 Cd2 N9 97.6(4) . . ? N5 Cd2 O1 90.1(4) . . ? N9 Cd2 O1 142.5(4) . . ? N5 Cd2 O10 98.3(3) . . ? N9 Cd2 O10 90.7(3) . . ? O1 Cd2 O10 124.6(3) . . ? N5 Cd2 O2 99.6(3) . . ? N9 Cd2 O2 88.6(4) . . ? O1 Cd2 O2 53.9(3) . . ? O10 Cd2 O2 162.1(3) . . ? N5 Cd2 O9 148.7(3) . . ? N9 Cd2 O9 99.2(3) . . ? O1 Cd2 O9 92.5(3) . . ? O10 Cd2 O9 55.3(3) . . ? O2 Cd2 O9 107.1(3) . . ? N5 Cd2 C21 125.4(4) . . ? N9 Cd2 C21 93.3(4) . . ? O1 Cd2 C21 111.9(3) . . ? O10 Cd2 C21 28.1(3) . . ? O2 Cd2 C21 134.1(4) . . ? O9 Cd2 C21 27.5(3) . . ? N5 Cd2 C7 95.3(3) . . ? N9 Cd2 C7 115.1(4) . . ? O1 Cd2 C7 27.4(3) . . ? O10 Cd2 C7 148.9(4) . . ? O2 Cd2 C7 26.5(3) . . ? O9 Cd2 C7 101.3(3) . . ? C21 Cd2 C7 127.2(4) . . ? C7 O1 Cd2 93.1(7) . . ? C7 O2 Cd2 91.4(7) . . ? C14 O3 Cd1 90.7(7) . 1_546 ? C14 O4 Cd1 91.1(7) . 1_546 ? C21 O9 Cd2 88.5(7) . . ? C21 O10 Cd2 91.3(7) . . ? C28 O11 Cd1 90.6(6) . . ? C28 O12 Cd1 89.0(7) . . ? O6 N1 O5 122.2(10) . . ? O6 N1 C2 119.0(9) . . ? O5 N1 C2 118.6(9) . . ? O7 N2 O8 122.2(12) . . ? O7 N2 C9 119.6(12) . . ? O8 N2 C9 118.1(12) . . ? O13 N3 O14 122.9(11) . . ? O13 N3 C16 118.9(10) . . ? O14 N3 C16 118.2(10) . . ? O15 N4 O16 124.4(10) . . ? O15 N4 C23 118.7(9) . . ? O16 N4 C23 116.9(9) . . ? C29 N5 C30 103.1(11) . . ? C29 N5 Cd2 120.6(9) . . ? C30 N5 Cd2 134.5(9) . . ? C31 N6 C29 108.8(11) . . ? C31 N6 C32 126.5(12) . . ? C29 N6 C32 124.6(11) . . ? C46 N7 C47 106.2(10) . . ? C46 N7 Cd1 124.2(8) . 1_646 ? C47 N7 Cd1 129.5(8) . 1_646 ? C46 N8 C48 107.0(10) . . ? C46 N8 C45 126.4(10) . . ? C48 N8 C45 126.6(11) . . ? C49 N9 C50 102.9(10) . . ? C49 N9 Cd2 128.5(9) . . ? C50 N9 Cd2 128.4(9) . . ? C49 N10 C51 107.2(11) . . ? C49 N10 C52 128.9(11) . . ? C51 N10 C52 123.9(11) . . ? C66 N11 C67 104.4(11) . . ? C66 N11 Cd1 120.6(8) . 1_655 ? C67 N11 Cd1 133.8(9) . 1_655 ? C68 N12 C66 104.4(10) . . ? C68 N12 C65 130.6(11) . . ? C66 N12 C65 124.8(10) . . ? C2 C1 C6 116.4(10) . . ? C2 C1 C8 124.1(10) . . ? C6 C1 C8 118.3(11) . . ? C1 C2 C3 123.0(11) . . ? C1 C2 N1 121.8(10) . . ? C3 C2 N1 115.0(10) . . ? C4 C3 C2 118.9(10) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.3(10) . . ? C3 C4 C7 120.0(10) . . ? C5 C4 C7 120.2(11) . . ? C6 C5 C4 120.3(11) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C1 C6 C5 121.9(11) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? O2 C7 O1 121.5(10) . . ? O2 C7 C4 120.2(12) . . ? O1 C7 C4 117.9(11) . . ? O2 C7 Cd2 62.0(6) . . ? O1 C7 Cd2 59.5(6) . . ? C4 C7 Cd2 173.1(8) . . ? C9 C8 C13 115.4(10) . . ? C9 C8 C1 125.5(11) . . ? C13 C8 C1 119.1(10) . . ? C10 C9 C8 124.7(12) . . ? C10 C9 N2 115.3(11) . . ? C8 C9 N2 119.9(11) . . ? C9 C10 C11 118.1(11) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C12 C11 C10 119.5(10) . . ? C12 C11 C14 121.4(11) . . ? C10 C11 C14 118.9(10) . . ? C13 C12 C11 120.3(12) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 121.7(10) . . ? C12 C13 H13 119.1 . . ? C8 C13 H13 119.1 . . ? O4 C14 O3 122.8(11) . . ? O4 C14 C11 117.5(12) . . ? O3 C14 C11 119.6(11) . . ? O4 C14 Cd1 61.5(6) . 1_546 ? O3 C14 Cd1 61.7(6) . 1_546 ? C11 C14 Cd1 169.0(8) . 1_546 ? C20 C15 C16 116.1(9) . . ? C20 C15 C22 117.8(10) . . ? C16 C15 C22 126.0(11) . . ? C17 C16 C15 122.2(11) . . ? C17 C16 N3 117.6(10) . . ? C15 C16 N3 120.0(9) . . ? C16 C17 C18 119.4(10) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 119.8(9) . . ? C19 C18 C21 121.5(11) . . ? C17 C18 C21 118.5(10) . . ? C20 C19 C18 118.9(10) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C15 C20 C19 123.4(10) . . ? C15 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? O9 C21 O10 124.0(11) . . ? O9 C21 C18 119.8(12) . . ? O10 C21 C18 116.1(11) . . ? O9 C21 Cd2 64.0(6) . . ? O10 C21 Cd2 60.7(6) . . ? C18 C21 Cd2 168.3(7) . . ? C23 C22 C27 117.5(9) . . ? C23 C22 C15 124.2(10) . . ? C27 C22 C15 117.6(9) . . ? C22 C23 C24 122.0(10) . . ? C22 C23 N4 121.6(9) . . ? C24 C23 N4 116.1(9) . . ? C25 C24 C23 119.8(10) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 119.2(9) . . ? C24 C25 C28 120.4(10) . . ? C26 C25 C28 120.3(10) . . ? C27 C26 C25 120.9(10) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C22 120.5(9) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? O12 C28 O11 124.8(10) . . ? O12 C28 C25 117.7(11) . . ? O11 C28 C25 117.4(11) . . ? O12 C28 Cd1 63.5(6) . . ? O11 C28 Cd1 61.4(6) . . ? C25 C28 Cd1 174.6(8) . . ? N5 C29 N6 110.7(11) . . ? N5 C29 H29 124.6 . . ? N6 C29 H29 124.6 . . ? C31 C30 N5 111.5(11) . . ? C31 C30 H30 124.3 . . ? N5 C30 H30 124.3 . . ? N6 C31 C30 105.9(12) . . ? N6 C31 H31 127.1 . . ? C30 C31 H31 127.1 . . ? C33 C32 N6 109.1(10) . . ? C33 C32 H32A 109.9 . . ? N6 C32 H32A 109.9 . . ? C33 C32 H32B 109.9 . . ? N6 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C34 C33 C38 117.7(12) . . ? C34 C33 C32 120.6(13) . . ? C38 C33 C32 121.6(12) . . ? C35 C34 C33 121.1(12) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 122.4(12) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C35 C36 C37 116.3(11) . . ? C35 C36 C39 123.2(11) . . ? C37 C36 C39 120.3(12) . . ? C38 C37 C36 121.6(12) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C37 C38 C33 120.9(12) . . ? C37 C38 H38 119.6 . . ? C33 C38 H38 119.6 . . ? C40 C39 C44 114.0(12) . . ? C40 C39 C36 122.4(12) . . ? C44 C39 C36 123.5(12) . . ? C41 C40 C39 124.6(13) . . ? C41 C40 H40 117.7 . . ? C39 C40 H40 117.7 . . ? C40 C41 C42 119.7(13) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 118.3(14) . . ? C43 C42 C45 122.1(14) . . ? C41 C42 C45 119.5(14) . . ? C42 C43 C44 121.9(14) . . ? C42 C43 H43 119.1 . . ? C44 C43 H43 119.1 . . ? C43 C44 C39 121.4(13) . . ? C43 C44 H44 119.3 . . ? C39 C44 H44 119.3 . . ? N8 C45 C42 112.8(10) . . ? N8 C45 H45A 109.0 . . ? C42 C45 H45A 109.0 . . ? N8 C45 H45B 109.0 . . ? C42 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? N7 C46 N8 110.5(10) . . ? N7 C46 H46 124.8 . . ? N8 C46 H46 124.8 . . ? N7 C47 C48 109.8(11) . . ? N7 C47 H47 125.1 . . ? C48 C47 H47 125.1 . . ? C47 C48 N8 106.5(12) . . ? C47 C48 H48 126.8 . . ? N8 C48 H48 126.8 . . ? N10 C49 N9 113.6(11) . . ? N10 C49 H49 123.2 . . ? N9 C49 H49 123.2 . . ? C51 C50 N9 109.8(11) . . ? C51 C50 H50 125.1 . . ? N9 C50 H50 125.1 . . ? C50 C51 N10 106.5(11) . . ? C50 C51 H51 126.7 . . ? N10 C51 H51 126.7 . . ? N10 C52 C53 111.3(10) . . ? N10 C52 H52A 109.4 . . ? C53 C52 H52A 109.4 . . ? N10 C52 H52B 109.4 . . ? C53 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C58 C53 C54 118.7(12) . . ? C58 C53 C52 120.1(14) . . ? C54 C53 C52 121.2(14) . . ? C53 C54 C55 119.6(13) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C56 C55 C54 123.6(12) . . ? C56 C55 H55 118.2 . . ? C54 C55 H55 118.2 . . ? C57 C56 C55 115.4(12) . . ? C57 C56 C59 120.9(12) . . ? C55 C56 C59 123.7(11) . . ? C56 C57 C58 123.0(14) . . ? C56 C57 H57 118.5 . . ? C58 C57 H57 118.5 . . ? C53 C58 C57 119.6(13) . . ? C53 C58 H58 120.2 . . ? C57 C58 H58 120.2 . . ? C60 C59 C64 117.4(11) . . ? C60 C59 C56 121.4(10) . . ? C64 C59 C56 121.1(11) . . ? C59 C60 C61 121.9(11) . . ? C59 C60 H60 119.1 . . ? C61 C60 H60 119.1 . . ? C60 C61 C62 119.3(12) . . ? C60 C61 H61 120.3 . . ? C62 C61 H61 120.3 . . ? C63 C62 C61 119.5(11) . . ? C63 C62 C65 120.4(11) . . ? C61 C62 C65 120.0(12) . . ? C62 C63 C64 121.4(11) . . ? C62 C63 H63 119.3 . . ? C64 C63 H63 119.3 . . ? C63 C64 C59 120.5(11) . . ? C63 C64 H64 119.8 . . ? C59 C64 H64 119.8 . . ? N12 C65 C62 111.3(9) . . ? N12 C65 H65A 109.4 . . ? C62 C65 H65A 109.4 . . ? N12 C65 H65B 109.4 . . ? C62 C65 H65B 109.4 . . ? H65A C65 H65B 108.0 . . ? N11 C66 N12 111.6(10) . . ? N11 C66 H66 124.2 . . ? N12 C66 H66 124.2 . . ? C68 C67 N11 110.8(11) . . ? C68 C67 H67 124.6 . . ? N11 C67 H67 124.6 . . ? C67 C68 N12 108.7(12) . . ? C67 C68 H68 125.6 . . ? N12 C68 H68 125.6 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.272 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.111 #=========================END