# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global #TrackingRef 'cif.txt' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Zhan Shi' _publ_contact_author_email zshi@mail.jlu.edu.cn _publ_section_title ; Coordination Polymers Constructed by 1,3-Bi(4-pyridyl)propane with Four Different Conformations and 2,2'-Dinitro-4,4' -biphenyldicarboxylate Ligands: The Effects of Metal Ions ; loop_ _publ_author_name 'Baiyan Li.' 'Guanghua Li.' 'Dan Liu.' 'Yu Peng.' 'Xiaojing Zhou.' 'Jia Hua.' ; Zhan Shi ; S.Feng # Attachment 'cif.cif' data_Compound-1 #TrackingRef 'cif.txt' _database_code_depnum_ccdc_archive 'CCDC 778423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C41 H26 Mn2 N6 O16' _chemical_formula_sum 'C41 H26 Mn2 N6 O16' _chemical_formula_weight 968.56 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 14.112(3) _cell_length_b 26.191(5) _cell_length_c 12.785(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.92(3) _cell_angle_gamma 90.00 _cell_volume 4352.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4945 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.659 _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 '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 21081 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.42 _reflns_number_total 4945 _reflns_number_gt 3665 _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. To improve the parameters chemical more reasonable, ultimately restrain instructions EADP (o5, o5', o6, o6', o7, o7', o8, o8'), ISOR (o5, o5', o6, c18, c19, c21, n1), and FLAT (c15, c16, c17, c18, c19, n3) and (c15', c16', c17, c18', c19', n3) were applied in the refinement. ; _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^)+(0.1193P)^2^+29.8153P] 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 4945 _refine_ls_number_parameters 330 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1142 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.2456 _refine_ls_wR_factor_gt 0.2257 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.031 _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 1.07806(5) 0.00687(2) 0.90007(6) 0.0321(2) Uani 1 1 d . . . O1 O 0.9691(3) 0.06819(14) 0.8560(3) 0.0500(9) Uani 1 1 d . . . O2 O 0.8481(3) 0.05052(13) 0.6855(4) 0.0505(10) Uani 1 1 d . . . O3 O 0.6305(3) 0.46516(14) 0.5649(3) 0.0494(9) Uani 1 1 d . . . O4 O 0.5211(3) 0.44484(14) 0.6454(4) 0.0525(10) Uani 1 1 d . . . O5 O 1.0280(9) 0.2433(4) 0.9786(10) 0.075(2) Uani 0.50 1 d PU A 1 O5' O 1.0443(9) 0.2503(4) 0.9262(10) 0.075(2) Uani 0.50 1 d PU A 2 O6 O 0.9232(9) 0.3008(4) 0.9029(9) 0.0683(11) Uani 0.50 1 d PU A 1 O6' O 0.9002(8) 0.2944(4) 0.9344(9) 0.0683(11) Uani 0.50 1 d P A 2 O7 O 0.6153(9) 0.3074(4) 0.9180(9) 0.0683(11) Uani 0.50 1 d P B 1 O7' O 0.5784(8) 0.2949(4) 0.8759(9) 0.0683(11) Uani 0.50 1 d P B 2 O8 O 0.6741(9) 0.2363(4) 0.8670(9) 0.0683(11) Uani 0.50 1 d P B 1 O8' O 0.7041(9) 0.2438(4) 0.9009(9) 0.0683(11) Uani 0.50 1 d P B 2 N1 N 0.9474(5) 0.2581(2) 0.9016(6) 0.0736(16) Uani 1 1 d U . . N2 N 0.6545(5) 0.2826(2) 0.8583(6) 0.0677(16) Uani 1 1 d . . . N3 N 1.2174(3) -0.04272(17) 0.9635(4) 0.0486(11) Uani 1 1 d D . . C1 C 0.8931(4) 0.07959(18) 0.7684(5) 0.0386(11) Uani 1 1 d . . . C2 C 0.8552(4) 0.13388(18) 0.7592(5) 0.0391(11) Uani 1 1 d . A . C3 C 0.9138(4) 0.17049(19) 0.8345(5) 0.0492(14) Uani 1 1 d . . . H3 H 0.9756 0.1615 0.8927 0.100 Uiso 1 1 calc . . . C4 C 0.8802(5) 0.2205(2) 0.8230(5) 0.0549(15) Uani 1 1 d . A . C5 C 0.7862(4) 0.23598(19) 0.7401(5) 0.0486(13) Uani 1 1 d . . . C6 C 0.7296(4) 0.1989(2) 0.6645(5) 0.0499(14) Uani 1 1 d . A . H6 H 0.6674 0.2077 0.6068 0.100 Uiso 1 1 calc . . . C7 C 0.7637(4) 0.14865(19) 0.6731(5) 0.0445(13) Uani 1 1 d . . . H7 H 0.7246 0.1246 0.6203 0.100 Uiso 1 1 calc . . . C8 C 0.5970(4) 0.43599(17) 0.6201(4) 0.0402(11) Uani 1 1 d . . . C9 C 0.6521(4) 0.38586(18) 0.6592(5) 0.0413(11) Uani 1 1 d . A . C10 C 0.6315(4) 0.3563(2) 0.7369(6) 0.0510(14) Uani 1 1 d . . . H10 H 0.5867 0.3682 0.7689 0.100 Uiso 1 1 calc . . . C11 C 0.6773(4) 0.3091(2) 0.7674(6) 0.0515(14) Uani 1 1 d . A . C12 C 0.7444(5) 0.28943(19) 0.7210(5) 0.0497(14) Uani 1 1 d . A . C13 C 0.7620(7) 0.3194(3) 0.6438(7) 0.077(2) Uani 1 1 d . . . H13 H 0.8056 0.3074 0.6104 0.100 Uiso 1 1 calc . . . C14 C 0.7175(6) 0.3676(3) 0.6124(7) 0.070(2) Uani 1 1 d . A . H14 H 0.7323 0.3871 0.5600 0.100 Uiso 1 1 calc . . . C15 C 1.215(4) -0.0878(15) 0.991(2) 0.050(7) Uani 0.50 1 d PD C 1 H15 H 1.1513 -0.1030 0.9719 0.100 Uiso 0.50 1 calc P D 1 C15' C 1.220(4) -0.0858(16) 1.023(2) 0.041(6) Uani 0.50 1 d PD C 2 H15' H 1.1578 -0.0989 1.0208 0.100 Uiso 0.50 1 calc P E 2 C16 C 1.308(3) -0.1191(10) 1.051(2) 0.061(7) Uani 0.50 1 d PD C 1 H16 H 1.3019 -0.1538 1.0633 0.100 Uiso 0.50 1 calc P F 1 C16' C 1.305(3) -0.1100(8) 1.0836(19) 0.045(4) Uani 0.50 1 d PD C 2 H16' H 1.3015 -0.1379 1.1265 0.100 Uiso 0.50 1 calc P G 2 C17 C 1.3992(5) -0.0963(3) 1.0868(5) 0.0602(17) Uani 1 1 d D . . C20 C 1.4992(6) -0.1246(3) 1.1516(7) 0.085(3) Uani 1 1 d . C . H20A H 1.5135 -0.1471 1.0991 0.100 Uiso 1 1 calc . . . H20B H 1.5546 -0.0999 1.1792 0.100 Uiso 1 1 calc . . . C21 C 1.5000 -0.1557(5) 1.2500 0.082(3) Uani 1 2 d SU . . H21A H 1.4398 -0.1776 1.2246 0.100 Uiso 0.50 1 calc P . . H21B H 1.5602 -0.1776 1.2754 0.100 Uiso 0.50 1 calc P . . C19 C 1.3100(15) -0.0200(7) 1.0100(16) 0.076(5) Uani 0.50 1 d PDU C 1 H19 H 1.3139 0.0148 0.9975 0.100 Uiso 0.50 1 calc P H 1 C19' C 1.3054(9) -0.0308(5) 0.9493(15) 0.059(4) Uani 0.50 1 d PD C 2 H19' H 1.3041 -0.0066 0.8955 0.100 Uiso 0.50 1 calc P I 2 C18 C 1.4014(18) -0.0457(9) 1.0766(18) 0.090(7) Uani 0.50 1 d PDU C 1 H18 H 1.4623 -0.0277 1.1128 0.100 Uiso 0.50 1 calc P J 1 C18' C 1.3978(10) -0.0548(7) 1.0155(18) 0.076(5) Uani 0.50 1 d PD C 2 H18' H 1.4591 -0.0433 1.0125 0.100 Uiso 0.50 1 calc P K 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0291(4) 0.0174(3) 0.0446(4) 0.0030(3) 0.0087(3) -0.0004(2) O1 0.046(2) 0.0340(18) 0.061(2) 0.0039(17) 0.0111(19) 0.0154(16) O2 0.041(2) 0.0328(18) 0.074(3) -0.0176(18) 0.0179(19) 0.0018(15) O3 0.052(2) 0.0354(19) 0.052(2) 0.0091(16) 0.0106(18) 0.0012(16) O4 0.041(2) 0.0328(18) 0.078(3) 0.0151(18) 0.017(2) 0.0139(16) O5 0.074(2) 0.074(2) 0.075(2) -0.0005(7) 0.0280(10) -0.0005(7) O5' 0.074(2) 0.074(2) 0.075(2) -0.0005(7) 0.0280(10) -0.0005(7) O6 0.0698(14) 0.0621(13) 0.0692(14) -0.0006(9) 0.0228(10) 0.0015(9) O6' 0.0698(14) 0.0621(13) 0.0692(14) -0.0006(9) 0.0228(10) 0.0015(9) O7 0.0698(14) 0.0621(13) 0.0692(14) -0.0006(9) 0.0228(10) 0.0015(9) O7' 0.0698(14) 0.0621(13) 0.0692(14) -0.0006(9) 0.0228(10) 0.0015(9) O8 0.0698(14) 0.0621(13) 0.0692(14) -0.0006(9) 0.0228(10) 0.0015(9) O8' 0.0698(14) 0.0621(13) 0.0692(14) -0.0006(9) 0.0228(10) 0.0015(9) N1 0.0726(18) 0.0695(18) 0.0743(18) -0.0018(10) 0.0239(11) 0.0016(10) N2 0.069(4) 0.039(3) 0.094(4) 0.018(3) 0.030(3) 0.016(3) N3 0.034(2) 0.036(2) 0.069(3) 0.009(2) 0.014(2) 0.0070(18) C1 0.035(3) 0.027(2) 0.055(3) -0.005(2) 0.020(2) 0.0054(19) C2 0.032(2) 0.028(2) 0.050(3) -0.002(2) 0.008(2) 0.0072(19) C3 0.036(3) 0.033(2) 0.058(3) -0.004(2) -0.004(2) 0.008(2) C4 0.046(3) 0.032(3) 0.066(4) -0.008(2) -0.001(3) 0.005(2) C5 0.046(3) 0.028(2) 0.058(3) -0.001(2) 0.005(3) 0.010(2) C6 0.042(3) 0.042(3) 0.049(3) -0.006(2) -0.001(2) 0.014(2) C7 0.039(3) 0.034(2) 0.047(3) -0.010(2) 0.001(2) 0.008(2) C8 0.039(3) 0.025(2) 0.044(3) 0.0025(19) 0.002(2) 0.0066(19) C9 0.039(3) 0.028(2) 0.049(3) 0.004(2) 0.008(2) 0.008(2) C10 0.039(3) 0.035(3) 0.074(4) 0.014(3) 0.018(3) 0.010(2) C11 0.038(3) 0.033(3) 0.074(4) 0.016(3) 0.012(3) 0.007(2) C12 0.053(3) 0.029(2) 0.052(3) 0.001(2) 0.004(3) 0.016(2) C13 0.099(6) 0.063(4) 0.092(5) 0.022(4) 0.061(5) 0.044(4) C14 0.094(5) 0.053(4) 0.084(5) 0.029(3) 0.057(4) 0.035(4) C15 0.039(10) 0.039(8) 0.048(18) 0.012(12) -0.010(15) 0.007(6) C15' 0.041(15) 0.047(9) 0.032(13) 0.016(9) 0.011(15) 0.006(8) C16 0.059(10) 0.035(8) 0.067(17) -0.011(9) 0.000(12) 0.016(7) C16' 0.056(8) 0.039(11) 0.037(10) 0.002(7) 0.014(9) 0.020(9) C17 0.042(3) 0.057(4) 0.064(4) -0.012(3) 0.002(3) 0.016(3) C20 0.053(4) 0.090(5) 0.079(5) -0.030(4) -0.010(4) 0.026(4) C21 0.082(3) 0.081(3) 0.082(3) 0.000 0.0302(15) 0.000 C19 0.076(5) 0.076(5) 0.077(5) 0.0005(10) 0.029(2) 0.0000(10) C19' 0.039(6) 0.053(7) 0.087(11) 0.028(7) 0.028(7) 0.014(5) C18 0.089(7) 0.090(7) 0.090(7) 0.0002(10) 0.035(3) 0.0000(10) C18' 0.027(6) 0.087(11) 0.116(15) 0.031(11) 0.030(8) 0.013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O4 2.074(3) 4_646 ? Mn1 O3 2.076(4) 8_556 ? Mn1 O2 2.116(4) 2_756 ? Mn1 O1 2.141(3) . ? Mn1 N3 2.229(4) . ? O1 C1 1.248(6) . ? O2 C1 1.258(6) . ? O2 Mn1 2.116(4) 2_756 ? O3 C8 1.251(6) . ? O3 Mn1 2.076(4) 8_455 ? O4 C8 1.255(7) . ? O4 Mn1 2.074(3) 4_656 ? O5 N1 1.241(12) . ? O5' N1 1.294(12) . ? O6 N1 1.171(12) . ? O6' N1 1.319(12) . ? O7 N2 1.279(12) . ? O7' N2 1.224(12) . ? O8 N2 1.239(13) . ? O8' N2 1.234(13) . ? N1 C4 1.463(8) . ? N2 C11 1.492(8) . ? N3 C15 1.23(4) . ? N3 C19 1.35(2) . ? N3 C15' 1.35(4) . ? N3 C19' 1.360(13) . ? C1 C2 1.507(6) . ? C2 C3 1.382(7) . ? C2 C7 1.386(7) . ? C3 C4 1.381(7) . ? C3 H3 0.9300 . ? C4 C5 1.397(8) . ? C5 C6 1.384(8) . ? C5 C12 1.502(7) . ? C6 C7 1.391(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.509(6) . ? C9 C14 1.368(8) . ? C9 C10 1.376(8) . ? C10 C11 1.378(7) . ? C10 H10 0.9300 . ? C11 C12 1.398(9) . ? C12 C13 1.359(9) . ? C13 C14 1.396(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.48(6) . ? C15 H15 0.9300 . ? C15' C16' 1.32(6) . ? C15' H15' 0.9300 . ? C16 C17 1.33(3) . ? C16 H16 0.9300 . ? C16' C17 1.36(3) . ? C16' H16' 0.9300 . ? C17 C18 1.33(2) . ? C17 C18' 1.414(18) . ? C17 C20 1.523(9) . ? C20 C21 1.495(12) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C20 1.495(12) 2_857 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C19 C18 1.41(3) . ? C19 H19 0.9300 . ? C19' C18' 1.397(18) . ? C19' H19' 0.9300 . ? C18 H18 0.9300 . ? C18' H18' 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 O4 Mn1 O3 119.71(17) 4_646 8_556 ? O4 Mn1 O2 133.84(18) 4_646 2_756 ? O3 Mn1 O2 106.35(16) 8_556 2_756 ? O4 Mn1 O1 100.18(16) 4_646 . ? O3 Mn1 O1 86.44(16) 8_556 . ? O2 Mn1 O1 84.63(15) 2_756 . ? O4 Mn1 N3 92.81(16) 4_646 . ? O3 Mn1 N3 85.46(18) 8_556 . ? O2 Mn1 N3 87.76(16) 2_756 . ? O1 Mn1 N3 166.87(17) . . ? C1 O1 Mn1 133.9(3) . . ? C1 O2 Mn1 125.1(3) . 2_756 ? C8 O3 Mn1 136.4(3) . 8_455 ? C8 O4 Mn1 128.5(3) . 4_656 ? O6 N1 O5 118.0(10) . . ? O6 N1 O5' 115.7(9) . . ? O5 N1 O5' 37.2(6) . . ? O6 N1 O6' 28.5(6) . . ? O5 N1 O6' 113.2(9) . . ? O5' N1 O6' 130.8(9) . . ? O6 N1 C4 122.6(8) . . ? O5 N1 C4 118.9(7) . . ? O5' N1 C4 113.6(7) . . ? O6' N1 C4 115.5(7) . . ? O7' N2 O8' 121.6(9) . . ? O7' N2 O8 115.0(9) . . ? O8' N2 O8 23.9(7) . . ? O7' N2 O7 30.9(6) . . ? O8' N2 O7 117.2(9) . . ? O8 N2 O7 125.1(9) . . ? O7' N2 C11 119.4(7) . . ? O8' N2 C11 118.0(8) . . ? O8 N2 C11 114.6(8) . . ? O7 N2 C11 120.2(6) . . ? C15 N3 C19 115(3) . . ? C15 N3 C15' 16.8(17) . . ? C19 N3 C15' 108(2) . . ? C15 N3 C19' 112(2) . . ? C19 N3 C19' 34.6(8) . . ? C15' N3 C19' 116(2) . . ? C15 N3 Mn1 123(3) . . ? C19 N3 Mn1 118.1(9) . . ? C15' N3 Mn1 121(2) . . ? C19' N3 Mn1 122.6(6) . . ? O1 C1 O2 125.9(4) . . ? O1 C1 C2 116.8(4) . . ? O2 C1 C2 117.2(5) . . ? C3 C2 C7 118.6(4) . . ? C3 C2 C1 120.2(4) . . ? C7 C2 C1 121.2(4) . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 122.8(5) . . ? C3 C4 N1 117.5(5) . . ? C5 C4 N1 119.7(5) . . ? C6 C5 C4 116.4(5) . . ? C6 C5 C12 117.2(5) . . ? C4 C5 C12 126.2(5) . . ? C5 C6 C7 121.4(5) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C2 C7 C6 120.9(5) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? O3 C8 O4 125.5(4) . . ? O3 C8 C9 117.4(5) . . ? O4 C8 C9 117.1(5) . . ? C14 C9 C10 119.2(5) . . ? C14 C9 C8 120.5(5) . . ? C10 C9 C8 120.2(5) . . ? C9 C10 C11 120.1(5) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 122.1(6) . . ? C10 C11 N2 114.7(5) . . ? C12 C11 N2 123.1(5) . . ? C13 C12 C11 116.1(5) . . ? C13 C12 C5 119.1(6) . . ? C11 C12 C5 124.3(6) . . ? C12 C13 C14 122.8(6) . . ? C12 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C9 C14 C13 119.7(6) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? N3 C15 C16 124(4) . . ? N3 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C16' C15' N3 123(4) . . ? C16' C15' H15' 118.4 . . ? N3 C15' H15' 118.4 . . ? C17 C16 C15 118(3) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C15' C16' C17 124(3) . . ? C15' C16' H16' 118.2 . . ? C17 C16' H16' 118.2 . . ? C18 C17 C16 118.0(16) . . ? C18 C17 C16' 108.6(14) . . ? C16 C17 C16' 21.1(9) . . ? C18 C17 C18' 33.7(10) . . ? C16 C17 C18' 110.8(14) . . ? C16' C17 C18' 114.6(13) . . ? C18 C17 C20 119.1(12) . . ? C16 C17 C20 122.5(14) . . ? C16' C17 C20 125.1(13) . . ? C18' C17 C20 120.2(8) . . ? C21 C20 C17 115.1(7) . . ? C21 C20 H20A 108.5 . . ? C17 C20 H20A 108.5 . . ? C21 C20 H20B 108.5 . . ? C17 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C20 C21 C20 114.0(10) 2_857 . ? C20 C21 H21A 108.8 2_857 . ? C20 C21 H21A 108.8 . . ? C20 C21 H21B 108.8 2_857 . ? C20 C21 H21B 108.8 . . ? H21A C21 H21B 107.6 . . ? N3 C19 C18 123.9(17) . . ? N3 C19 H19 118.0 . . ? C18 C19 H19 118.0 . . ? N3 C19' C18' 120.1(11) . . ? N3 C19' H19' 120.0 . . ? C18' C19' H19' 120.0 . . ? C17 C18 C19 118.9(19) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C19' C18' C17 120.8(11) . . ? C19' C18' H18' 119.6 . . ? C17 C18' H18' 119.6 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.148 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.110 #=========================END data_Compound-2 #TrackingRef 'cif.txt' _database_code_depnum_ccdc_archive 'CCDC 778424' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C82 H62.50 Co4 N12 O37.25' _chemical_formula_sum 'C82 H62.50 Co4 N12 O37.25' _chemical_formula_weight 2047.66 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' Co Co 0.3494 0.9721 '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 14.381(3) _cell_length_b 16.173(3) _cell_length_c 21.049(4) _cell_angle_alpha 89.88(3) _cell_angle_beta 89.88(3) _cell_angle_gamma 65.10(3) _cell_volume 4440.3(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15290 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2089 _exptl_absorpt_coefficient_mu 0.832 _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 '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 34891 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15290 _reflns_number_gt 12280 _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 ? _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. Standard DFIX restraints were used for the distance of the atoms, such as (o8 and o8'), (o14 and o14'), (o15 and o15'), (o36 and o1w), (H1b and co1), (H1a and co1), (H1a and H1b), (h1a and o35), (h1b and o35), (h1a and o5w). To improve the parameters chemical more reasonable, ultimately restrain instructions EADP (o5, o6, o7, o7', o8, o8', n1, n2, o15, o15', o16, o16', n4, o23, o23', o24, o24', n6, o31, o31', o31", o32, o32', o32"), ISOR (o5, o6, o7, o7', o8, o8', n1, n2, o13, o13', o14, o14', o15, o16, o16', n4, o21, o23, o30, o31, o31', o31", o32, o32', o32", n8, o3w, o4w, o24), and OMIT were applied in the refinement. ; _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^)+(0.0713P)^2^+31.0869P] 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 15290 _refine_ls_number_parameters 1240 _refine_ls_number_restraints 184 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2008 _refine_ls_wR_factor_gt 0.1918 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.038 _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 Co1 Co 0.80012(5) 0.23484(5) 0.43895(4) 0.02086(18) Uani 1 1 d D . . Co2 Co 0.57241(5) 0.44542(5) 0.43668(3) 0.01909(18) Uani 1 1 d . . . Co3 Co 1.06225(6) 0.94164(5) 0.06520(3) 0.02017(18) Uani 1 1 d . . . Co4 Co 1.30188(6) 0.74291(5) 0.06509(4) 0.0254(2) Uani 1 1 d . . . O1 O 0.6818(3) 0.2231(3) 0.3913(2) 0.0357(10) Uani 1 1 d . A . O2 O 0.5464(3) 0.3564(3) 0.3761(2) 0.0297(9) Uani 1 1 d . A . O3 O 0.3331(3) -0.1563(3) 0.1030(2) 0.0310(9) Uani 1 1 d . . . O4 O 0.1793(3) -0.0387(3) 0.1118(2) 0.0302(9) Uani 1 1 d . . . O5 O 0.6304(5) 0.0059(4) 0.1828(3) 0.0666(8) Uani 1 1 d U . . O6 O 0.6370(5) -0.1266(4) 0.1658(3) 0.0666(8) Uani 1 1 d U . . O7' O 0.6843(10) -0.0578(9) 0.3272(7) 0.0666(8) Uani 0.50 1 d PU A 1 O7 O 0.6583(10) -0.0541(9) 0.3575(7) 0.0666(8) Uani 0.50 1 d PU A 2 O8 O 0.5417(11) -0.0647(12) 0.3091(7) 0.0666(8) Uani 0.50 1 d PDU A 1 O8' O 0.5200(11) -0.0546(12) 0.3209(7) 0.0666(8) Uani 0.50 1 d PDU A 2 O9 O 0.7988(3) 0.1300(3) 0.4959(2) 0.0346(10) Uani 1 1 d . B . O10 O 0.6468(3) 0.1991(3) 0.5430(2) 0.0355(10) Uani 1 1 d . B . O11 O 0.5648(3) -0.4617(2) 0.51139(18) 0.0227(8) Uani 1 1 d . . . O12 O 0.7217(3) -0.5358(3) 0.5513(2) 0.0348(10) Uani 1 1 d . C . O13' O 0.8494(11) -0.2614(9) 0.4543(6) 0.066(3) Uani 0.50 1 d PU B 1 O13 O 0.7952(11) -0.2430(9) 0.4315(7) 0.073(4) Uani 0.50 1 d PU B 2 O14 O 0.8727(13) -0.1618(12) 0.4017(7) 0.069(5) Uani 0.50 1 d PDU B 1 O14' O 0.8936(11) -0.1681(11) 0.4165(7) 0.057(4) Uani 0.50 1 d PDU B 2 O15 O 0.9246(13) -0.3625(12) 0.6005(5) 0.0670(9) Uani 0.50 1 d PDU C 1 O15' O 0.9336(13) -0.3641(11) 0.5800(5) 0.0670(9) Uani 0.50 1 d PD C 2 O16' O 0.8591(10) -0.2385(9) 0.6193(7) 0.0670(9) Uani 0.50 1 d PU C 1 O16 O 0.8208(10) -0.2266(9) 0.6446(6) 0.0670(9) Uani 0.50 1 d PU C 2 O17 O 0.6999(3) 0.4636(3) 0.4071(2) 0.0323(10) Uani 1 1 d . . . O18 O 0.8252(3) 0.3284(3) 0.3846(2) 0.0369(11) Uani 1 1 d . . . O19 O 1.1936(3) 0.7410(3) 0.1309(3) 0.0480(13) Uani 1 1 d . D . O20 O 1.0349(3) 0.8453(3) 0.1142(2) 0.0335(10) Uani 1 1 d . D . O21 O 1.0507(6) 0.3212(6) 0.2106(4) 0.094(2) Uani 1 1 d U . . O22 O 1.0303(5) 0.4469(4) 0.1647(3) 0.0702(18) Uani 1 1 d . . . O23' O 1.1535(10) 0.4324(9) 0.2827(6) 0.0670(9) Uani 0.50 1 d P D 1 O23 O 1.1353(10) 0.4656(9) 0.3081(6) 0.0670(9) Uani 0.50 1 d PU D 2 O24' O 1.2537(10) 0.4983(9) 0.2774(7) 0.0670(9) Uani 0.50 1 d P D 1 O24 O 1.2548(10) 0.4723(9) 0.2450(7) 0.0670(9) Uani 0.50 1 d PU D 2 O25 O 1.0669(3) 1.0374(2) -0.00234(19) 0.0237(8) Uani 1 1 d . . . O26 O 1.2301(3) 0.9620(3) -0.0341(2) 0.0331(10) Uani 1 1 d . . . O27 O 1.2884(4) 1.6366(3) 0.0208(3) 0.0520(14) Uani 1 1 d . . . O28 O 1.1490(4) 1.6977(3) -0.0406(2) 0.0398(11) Uani 1 1 d . E . O29 O 1.4561(5) 1.1142(5) -0.0056(5) 0.098(3) Uani 1 1 d . . . O30 O 1.3997(6) 1.2500(5) -0.0415(4) 0.086(2) Uani 1 1 d U . . O31" O 1.3341(16) 1.3757(13) 0.1407(10) 0.0546(17) Uani 0.30 1 d PU E 1 O31' O 1.2758(16) 1.3915(13) 0.1537(9) 0.0546(17) Uani 0.30 1 d PU E 2 O31 O 1.3943(11) 1.3436(9) 0.1114(7) 0.0546(17) Uani 0.40 1 d PU E 3 O32" O 1.2991(15) 1.2711(19) 0.1102(14) 0.0546(17) Uani 0.30 1 d PU E 1 O32' O 1.2673(16) 1.2836(17) 0.1101(12) 0.0546(17) Uani 0.30 1 d PU E 2 O32 O 1.3314(12) 1.2576(11) 0.0946(8) 0.0546(17) Uani 0.40 1 d PU E 3 O33 O 0.6772(3) 0.3362(2) 0.49722(18) 0.0233(8) Uani 1 1 d . . . O34 O 1.1759(3) 0.8368(2) 0.00679(19) 0.0248(8) Uani 1 1 d . . . O35 O 0.9188(4) 0.2322(4) 0.5004(3) 0.0596(15) Uani 1 1 d D . . O36 O 1.4108(5) 0.7367(5) -0.0059(3) 0.077(2) Uani 1 1 d D . . N1 N 0.5838(6) -0.0190(5) 0.3226(4) 0.0666(8) Uani 1 1 d U . . N2 N 0.5902(6) -0.0471(5) 0.1774(4) 0.0666(8) Uani 1 1 d U A . N3 N 0.8295(6) -0.1819(4) 0.4452(4) 0.0584(19) Uani 1 1 d . . . N4 N 0.8501(6) -0.2976(6) 0.5979(4) 0.0670(9) Uani 1 1 d U . . N5 N 1.0158(5) 0.4055(5) 0.2084(3) 0.0550(17) Uani 1 1 d . . . N6 N 1.1664(6) 0.4994(5) 0.2648(4) 0.0670(9) Uani 1 1 d . . . N7 N 1.3871(6) 1.1839(5) -0.0206(4) 0.064(2) Uani 1 1 d . . . N8 N 1.3018(7) 1.3412(6) 0.0964(4) 0.078(2) Uani 1 1 d U . . N9 N 0.9081(4) 0.1348(3) 0.3801(3) 0.0326(12) Uani 1 1 d . . . N10 N 1.4905(4) -0.4458(3) 0.3734(2) 0.0306(11) Uani 1 1 d . . . N11 N 0.9627(4) 1.0430(3) 0.1267(2) 0.0286(11) Uani 1 1 d . . . N12 N 0.4180(5) 1.6462(4) 0.1242(3) 0.0478(16) Uani 1 1 d . . . C1 C 0.4665(5) 0.1180(4) 0.2611(3) 0.0332(14) Uani 1 1 d . . . C2 C 0.5425(5) 0.0781(4) 0.3075(3) 0.0364(15) Uani 1 1 d . A . C3 C 0.5825(5) 0.1277(4) 0.3417(3) 0.0351(14) Uani 1 1 d . . . H3 H 0.6351 0.0981 0.3705 0.080 Uiso 1 1 calc . . . C4 C 0.5454(5) 0.2215(4) 0.3338(3) 0.0266(12) Uani 1 1 d . A . C5 C 0.4660(6) 0.2638(4) 0.2918(3) 0.0415(17) Uani 1 1 d . . . H5 H 0.4370 0.3269 0.2878 0.080 Uiso 1 1 calc . . . C6 C 0.4285(6) 0.2127(5) 0.2552(4) 0.0451(18) Uani 1 1 d . A . H6 H 0.3767 0.2426 0.2259 0.080 Uiso 1 1 calc . . . C7 C 0.5945(4) 0.2723(4) 0.3708(3) 0.0235(12) Uani 1 1 d . . . C8 C 0.4219(5) 0.0682(4) 0.2204(3) 0.0349(15) Uani 1 1 d . A . C9 C 0.4770(5) -0.0088(5) 0.1837(3) 0.0413(17) Uani 1 1 d . . . C10 C 0.4292(5) -0.0538(5) 0.1507(3) 0.0384(16) Uani 1 1 d . A . H10 H 0.4687 -0.1059 0.1277 0.080 Uiso 1 1 calc . . . C11 C 0.3244(5) -0.0231(4) 0.1512(3) 0.0282(13) Uani 1 1 d . . . C12 C 0.2671(5) 0.0566(5) 0.1843(4) 0.0421(17) Uani 1 1 d . A . H12 H 0.1959 0.0807 0.1835 0.080 Uiso 1 1 calc . . . C13 C 0.3155(6) 0.1002(5) 0.2185(4) 0.0449(18) Uani 1 1 d . . . H13 H 0.2756 0.1527 0.2409 0.080 Uiso 1 1 calc . . . C14 C 0.2743(5) -0.0768(4) 0.1183(3) 0.0266(13) Uani 1 1 d . A . C15 C 0.7031(5) -0.1295(4) 0.5343(4) 0.0409(16) Uani 1 1 d . . . C16 C 0.7668(5) -0.1137(4) 0.4919(4) 0.0403(16) Uani 1 1 d . B . C17 C 0.7745(5) -0.0306(4) 0.4892(3) 0.0380(15) Uani 1 1 d . . . H17 H 0.8204 -0.0231 0.4611 0.080 Uiso 1 1 calc . . . C18 C 0.7147(5) 0.0400(4) 0.5279(3) 0.0311(14) Uani 1 1 d . B . C19 C 0.6484(6) 0.0265(5) 0.5701(4) 0.0448(18) Uani 1 1 d . . . H19 H 0.6066 0.0738 0.5964 0.080 Uiso 1 1 calc . . . C20 C 0.6441(6) -0.0585(5) 0.5730(4) 0.055(2) Uani 1 1 d . B . H20 H 0.6001 -0.0669 0.6021 0.080 Uiso 1 1 calc . . . C21 C 0.7195(5) 0.1311(4) 0.5226(3) 0.0276(13) Uani 1 1 d . . . C22 C 0.6884(6) -0.2158(4) 0.5381(4) 0.0409(16) Uani 1 1 d . B . C23 C 0.7579(6) -0.2949(5) 0.5663(4) 0.0495(19) Uani 1 1 d . B . C24 C 0.7467(6) -0.3755(4) 0.5653(4) 0.0434(18) Uani 1 1 d . . . H24 H 0.7969 -0.4284 0.5824 0.080 Uiso 1 1 calc . . . C25 C 0.6592(4) -0.3763(4) 0.5382(3) 0.0284(13) Uani 1 1 d . C . C26 C 0.5859(5) -0.2970(4) 0.5134(3) 0.0346(15) Uani 1 1 d . . . H26 H 0.5259 -0.2964 0.4966 0.080 Uiso 1 1 calc . . . C27 C 0.6010(5) -0.2174(4) 0.5134(4) 0.0422(17) Uani 1 1 d . B . H27 H 0.5508 -0.1643 0.4963 0.080 Uiso 1 1 calc . . . C28 C 0.6488(4) -0.4646(4) 0.5339(3) 0.0242(12) Uani 1 1 d . . . C29 C 0.9378(5) 0.5467(5) 0.2740(3) 0.0383(15) Uani 1 1 d . D . C30 C 0.9518(5) 0.4573(4) 0.2615(3) 0.0347(14) Uani 1 1 d . . . C31 C 0.9064(5) 0.4134(4) 0.2981(3) 0.0327(14) Uani 1 1 d . . . H31 H 0.9209 0.3527 0.2901 0.080 Uiso 1 1 calc . . . C32 C 0.8393(4) 0.4595(4) 0.3466(3) 0.0267(12) Uani 1 1 d . . . C33 C 0.8220(6) 0.5489(4) 0.3581(3) 0.0408(16) Uani 1 1 d . . . H33 H 0.7755 0.5816 0.3895 0.080 Uiso 1 1 calc . . . C34 C 0.8724(6) 0.5902(5) 0.3239(4) 0.0490(19) Uani 1 1 d . . . H34 H 0.8622 0.6492 0.3345 0.080 Uiso 1 1 calc . . . C35 C 0.7839(4) 0.4136(4) 0.3827(3) 0.0232(12) Uani 1 1 d . . . C36 C 0.9843(5) 0.6000(5) 0.2373(3) 0.0372(15) Uani 1 1 d . . . C37 C 1.0896(5) 0.5788(5) 0.2337(3) 0.0377(15) Uani 1 1 d . D . C38 C 1.1245(5) 0.6334(5) 0.2002(3) 0.0425(17) Uani 1 1 d . . . H38 H 1.1947 0.6168 0.1971 0.080 Uiso 1 1 calc . . . C39 C 1.0567(5) 0.7126(4) 0.1713(3) 0.0335(14) Uani 1 1 d . D . C40 C 0.9538(6) 0.7352(5) 0.1749(4) 0.0465(18) Uani 1 1 d . . . H40 H 0.9075 0.7877 0.1550 0.080 Uiso 1 1 calc . . . C41 C 0.9185(6) 0.6799(5) 0.2081(4) 0.0495(19) Uani 1 1 d . D . H41 H 0.8482 0.6971 0.2108 0.080 Uiso 1 1 calc . . . C42 C 1.0987(5) 0.7710(4) 0.1357(3) 0.0304(13) Uani 1 1 d . . . C43 C 1.1986(5) 1.2800(4) -0.0063(3) 0.0373(15) Uani 1 1 d . E . C44 C 1.2800(5) 1.1960(4) -0.0153(4) 0.0390(16) Uani 1 1 d . . . C45 C 1.2672(5) 1.1158(4) -0.0191(3) 0.0370(15) Uani 1 1 d . . . H45 H 1.3235 1.0603 -0.0252 0.080 Uiso 1 1 calc . . . C46 C 1.1702(5) 1.1196(4) -0.0136(3) 0.0276(13) Uani 1 1 d . . . C47 C 1.0877(5) 1.2018(4) -0.0026(3) 0.0352(15) Uani 1 1 d . . . H47 H 1.0225 1.2040 0.0027 0.080 Uiso 1 1 calc . . . C48 C 1.1020(5) 1.2808(4) 0.0004(4) 0.0420(17) Uani 1 1 d . . . H48 H 1.0456 1.3360 0.0070 0.080 Uiso 1 1 calc . . . C49 C 1.1565(4) 1.0327(4) -0.0177(3) 0.0239(12) Uani 1 1 d . . . C50 C 1.2054(5) 1.3701(4) -0.0048(4) 0.0418(17) Uani 1 1 d . . . C51 C 1.2534(7) 1.3986(5) 0.0413(4) 0.051(2) Uani 1 1 d . E . C52 C 1.2574(7) 1.4819(5) 0.0388(4) 0.057(2) Uani 1 1 d . . . H52 H 1.2924 1.4977 0.0702 0.080 Uiso 1 1 calc . . . C53 C 1.2100(5) 1.5426(4) -0.0100(3) 0.0348(15) Uani 1 1 d . E . C54 C 1.1585(6) 1.5175(4) -0.0546(4) 0.0452(18) Uani 1 1 d . . . H54 H 1.1246 1.5579 -0.0872 0.080 Uiso 1 1 calc . . . C55 C 1.1556(7) 1.4329(5) -0.0524(4) 0.054(2) Uani 1 1 d . E . H55 H 1.1195 1.4178 -0.0834 0.080 Uiso 1 1 calc . . . C56 C 1.2147(5) 1.6337(4) -0.0105(3) 0.0317(14) Uani 1 1 d . . . C57 C 0.8934(5) 0.0633(4) 0.3587(3) 0.0388(15) Uani 1 1 d . . . H57 H 0.8326 0.0592 0.3693 0.080 Uiso 1 1 calc . . . C58 C 0.9638(6) -0.0042(5) 0.3221(4) 0.0460(18) Uani 1 1 d . . . H58 H 0.9499 -0.0523 0.3081 0.080 Uiso 1 1 calc . . . C59 C 1.0547(6) -0.0009(5) 0.3060(3) 0.0475(19) Uani 1 1 d . . . C60 C 1.0714(6) 0.0722(5) 0.3283(4) 0.053(2) Uani 1 1 d . . . H60 H 1.1319 0.0773 0.3185 0.080 Uiso 1 1 calc . . . C61 C 0.9974(5) 0.1374(5) 0.3650(4) 0.0448(17) Uani 1 1 d . . . H61 H 1.0100 0.1856 0.3802 0.080 Uiso 1 1 calc . . . C62 C 1.1338(7) -0.0721(6) 0.2656(4) 0.065(3) Uani 1 1 d . . . H62A H 1.1673 -0.0437 0.2391 0.080 Uiso 1 1 calc . . . H62B H 1.1004 -0.0992 0.2380 0.080 Uiso 1 1 calc . . . C63 C 1.2133(7) -0.1460(6) 0.3050(4) 0.062(2) Uani 1 1 d . . . H63A H 1.1827 -0.1827 0.3247 0.080 Uiso 1 1 calc . . . H63B H 1.2368 -0.1183 0.3385 0.080 Uiso 1 1 calc . . . C64 C 1.3052(7) -0.2073(5) 0.2644(4) 0.060(2) Uani 1 1 d . . . H64A H 1.2808 -0.2255 0.2263 0.080 Uiso 1 1 calc . . . H64B H 1.3442 -0.1735 0.2516 0.080 Uiso 1 1 calc . . . C65 C 1.5155(5) -0.3757(4) 0.3676(3) 0.0377(15) Uani 1 1 d . . . H65 H 1.5736 -0.3788 0.3888 0.080 Uiso 1 1 calc . . . C66 C 1.4606(6) -0.2988(4) 0.3319(4) 0.0472(18) Uani 1 1 d . . . H66 H 1.4824 -0.2524 0.3286 0.080 Uiso 1 1 calc . . . C67 C 1.3743(5) -0.2919(5) 0.3015(3) 0.0427(17) Uani 1 1 d . . . C68 C 1.3489(6) -0.3642(5) 0.3064(4) 0.0486(19) Uani 1 1 d . . . H68 H 1.2909 -0.3620 0.2856 0.080 Uiso 1 1 calc . . . C69 C 1.4075(5) -0.4406(5) 0.3418(3) 0.0383(15) Uani 1 1 d . . . H69 H 1.3891 -0.4892 0.3436 0.080 Uiso 1 1 calc . . . C70 C 0.5004(5) 1.6502(5) 0.1448(4) 0.0452(17) Uani 1 1 d . . . H70 H 0.5099 1.7023 0.1353 0.080 Uiso 1 1 calc . . . C71 C 0.5754(6) 1.5830(6) 0.1799(4) 0.0523(19) Uani 1 1 d . . . H71 H 0.6349 1.5891 0.1906 0.080 Uiso 1 1 calc . . . C72 C 0.5627(6) 1.5083(5) 0.1989(4) 0.0514(19) Uani 1 1 d . . . C73 C 0.4707(7) 1.5057(6) 0.1813(4) 0.060(2) Uani 1 1 d . . . H73 H 0.4569 1.4567 0.1934 0.080 Uiso 1 1 calc . . . C74 C 0.4017(6) 1.5741(5) 0.1467(4) 0.0506(19) Uani 1 1 d . . . H74 H 0.3394 1.5721 0.1376 0.080 Uiso 1 1 calc . . . C75 C 0.6394(7) 1.4314(6) 0.2369(4) 0.063(2) Uani 1 1 d . . . H75A H 0.6881 1.4515 0.2555 0.080 Uiso 1 1 calc . . . H75B H 0.6040 1.4170 0.2715 0.080 Uiso 1 1 calc . . . C76 C 0.6960(7) 1.3484(6) 0.2001(4) 0.074(3) Uani 1 1 d . . . H76A H 0.7432 1.3591 0.1718 0.080 Uiso 1 1 calc . . . H76B H 0.6479 1.3359 0.1741 0.080 Uiso 1 1 calc . . . C77 C 0.7561(6) 1.2649(5) 0.2405(4) 0.053(2) Uani 1 1 d . . . H77A H 0.7944 1.2807 0.2725 0.080 Uiso 1 1 calc . . . H77B H 0.7085 1.2463 0.2624 0.080 Uiso 1 1 calc . . . C78 C 0.9763(5) 1.1184(4) 0.1350(3) 0.0350(14) Uani 1 1 d . . . H78 H 1.0317 1.1230 0.1150 0.080 Uiso 1 1 calc . . . C79 C 0.9126(5) 1.1903(4) 0.1716(4) 0.0416(16) Uani 1 1 d . . . H79 H 0.9257 1.2416 0.1761 0.080 Uiso 1 1 calc . . . C80 C 0.8290(5) 1.1865(4) 0.2020(3) 0.0379(15) Uani 1 1 d . . . C81 C 0.8148(5) 1.1080(5) 0.1934(3) 0.0420(16) Uani 1 1 d . . . H81 H 0.7597 1.1023 0.2129 0.080 Uiso 1 1 calc . . . C82 C 0.8815(5) 1.0381(4) 0.1562(3) 0.0357(14) Uani 1 1 d . . . H82 H 0.8704 0.9859 0.1513 0.080 Uiso 1 1 calc . . . O1W O 1.3942(18) 0.826(2) -0.1094(12) 0.083(9) Uani 0.25 1 d PD . . O2W O 1.504(2) 0.5352(16) -0.0103(14) 0.078(8) Uani 0.25 1 d P . . O3W O 0.9157(19) 0.3542(17) 0.5903(12) 0.066(6) Uani 0.25 1 d PU . . O4W O 0.9314(17) 0.3859(15) 0.5407(11) 0.055(5) Uani 0.25 1 d PU . . O5W O 1.0026(14) 0.0391(10) 0.5146(11) 0.050(5) Uani 0.25 1 d PD . . H1A H 0.955(4) 0.1773(13) 0.515(3) 0.080 Uiso 1 1 d D . . H1B H 0.902(3) 0.271(3) 0.528(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 Co1 0.0193(4) 0.0168(4) 0.0283(4) -0.0007(3) 0.0013(3) -0.0093(3) Co2 0.0193(4) 0.0163(3) 0.0230(4) -0.0018(3) 0.0005(3) -0.0088(3) Co3 0.0219(4) 0.0183(4) 0.0236(4) 0.0004(3) -0.0004(3) -0.0116(3) Co4 0.0242(4) 0.0184(4) 0.0372(5) 0.0017(3) -0.0062(3) -0.0125(3) O1 0.027(2) 0.029(2) 0.047(3) -0.015(2) -0.009(2) -0.0087(19) O2 0.033(2) 0.023(2) 0.035(2) -0.0056(17) -0.0051(18) -0.0130(18) O3 0.031(2) 0.024(2) 0.040(2) -0.0090(18) -0.0051(19) -0.0141(18) O4 0.026(2) 0.033(2) 0.033(2) -0.0071(18) -0.0059(18) -0.0136(18) O5 0.0664(8) 0.0666(8) 0.0677(8) -0.0015(4) -0.0007(4) -0.0288(5) O6 0.0664(8) 0.0666(8) 0.0677(8) -0.0015(4) -0.0007(4) -0.0288(5) O7' 0.0664(8) 0.0666(8) 0.0677(8) -0.0015(4) -0.0007(4) -0.0288(5) O7 0.0664(8) 0.0666(8) 0.0677(8) -0.0015(4) -0.0007(4) -0.0288(5) O8 0.0664(8) 0.0666(8) 0.0677(8) -0.0015(4) -0.0007(4) -0.0288(5) O8' 0.0664(8) 0.0666(8) 0.0677(8) -0.0015(4) -0.0007(4) -0.0288(5) O9 0.030(2) 0.023(2) 0.052(3) 0.0090(19) 0.007(2) -0.0132(18) O10 0.040(3) 0.024(2) 0.044(3) -0.0044(19) 0.010(2) -0.015(2) O11 0.0196(19) 0.0242(19) 0.029(2) -0.0075(16) 0.0029(16) -0.0140(16) O12 0.035(2) 0.023(2) 0.050(3) 0.0006(19) -0.012(2) -0.0152(19) O13' 0.066(3) 0.065(3) 0.066(3) -0.0005(10) 0.0005(10) -0.0275(16) O13 0.073(4) 0.072(4) 0.073(4) -0.0009(10) -0.0002(10) -0.0308(18) O14 0.069(5) 0.069(5) 0.069(5) -0.0002(10) 0.0003(10) -0.029(2) O14' 0.057(4) 0.057(4) 0.057(4) -0.0004(10) 0.0005(10) -0.024(2) O15 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) O15' 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) O16' 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) O16 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) O17 0.027(2) 0.023(2) 0.049(3) 0.0039(19) 0.011(2) -0.0119(18) O18 0.038(3) 0.020(2) 0.052(3) 0.0040(19) 0.015(2) -0.0120(19) O19 0.030(3) 0.054(3) 0.064(3) 0.033(3) -0.005(2) -0.023(2) O20 0.034(2) 0.026(2) 0.045(3) 0.0076(19) 0.002(2) -0.0171(19) O21 0.095(2) 0.093(2) 0.094(2) -0.0002(10) 0.0036(10) -0.0398(13) O22 0.095(5) 0.085(4) 0.045(3) -0.003(3) 0.030(3) -0.052(4) O23' 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) O23 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) O24' 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) O24 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) O25 0.024(2) 0.0207(19) 0.032(2) 0.0015(16) -0.0003(17) -0.0153(16) O26 0.029(2) 0.019(2) 0.053(3) -0.0025(19) 0.008(2) -0.0116(18) O27 0.054(3) 0.024(2) 0.082(4) 0.003(2) -0.033(3) -0.020(2) O28 0.044(3) 0.021(2) 0.057(3) 0.006(2) -0.018(2) -0.017(2) O29 0.034(3) 0.068(5) 0.191(9) 0.002(5) -0.003(4) -0.021(3) O30 0.085(2) 0.086(2) 0.089(2) -0.0002(10) 0.0022(10) -0.0385(12) O31" 0.0549(18) 0.0543(17) 0.0548(17) 0.0003(4) -0.0001(4) -0.0231(8) O31' 0.0549(18) 0.0543(17) 0.0548(17) 0.0003(4) -0.0001(4) -0.0231(8) O31 0.0549(18) 0.0543(17) 0.0548(17) 0.0003(4) -0.0001(4) -0.0231(8) O32" 0.0549(18) 0.0543(17) 0.0548(17) 0.0003(4) -0.0001(4) -0.0231(8) O32' 0.0549(18) 0.0543(17) 0.0548(17) 0.0003(4) -0.0001(4) -0.0231(8) O32 0.0549(18) 0.0543(17) 0.0548(17) 0.0003(4) -0.0001(4) -0.0231(8) O33 0.026(2) 0.0199(18) 0.026(2) -0.0012(16) -0.0007(16) -0.0119(16) O34 0.028(2) 0.0184(18) 0.029(2) 0.0002(16) -0.0006(17) -0.0113(16) O35 0.054(3) 0.058(3) 0.068(4) -0.002(3) -0.026(3) -0.025(3) O36 0.066(4) 0.122(6) 0.062(4) -0.035(4) 0.027(3) -0.058(4) N1 0.0664(8) 0.0666(8) 0.0677(8) -0.0015(4) -0.0007(4) -0.0288(5) N2 0.0664(8) 0.0666(8) 0.0677(8) -0.0015(4) -0.0007(4) -0.0288(5) N3 0.082(5) 0.024(3) 0.074(5) -0.005(3) 0.019(4) -0.027(3) N4 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) N5 0.065(4) 0.052(4) 0.059(4) -0.007(3) 0.029(3) -0.036(3) N6 0.0670(10) 0.0673(10) 0.0681(10) 0.0006(4) -0.0006(4) -0.0295(5) N7 0.070(5) 0.054(4) 0.101(6) -0.016(4) 0.026(4) -0.056(4) N8 0.080(2) 0.077(2) 0.078(2) -0.0003(10) -0.0029(10) -0.0340(13) N9 0.031(3) 0.025(3) 0.039(3) -0.001(2) 0.007(2) -0.010(2) N10 0.032(3) 0.029(3) 0.026(3) 0.003(2) 0.001(2) -0.009(2) N11 0.029(3) 0.028(3) 0.031(3) -0.001(2) -0.001(2) -0.013(2) N12 0.041(3) 0.029(3) 0.073(4) 0.008(3) -0.025(3) -0.014(3) C1 0.038(4) 0.036(3) 0.034(3) -0.009(3) -0.004(3) -0.024(3) C2 0.042(4) 0.027(3) 0.044(4) -0.004(3) -0.008(3) -0.018(3) C3 0.037(4) 0.032(3) 0.035(4) -0.007(3) -0.005(3) -0.013(3) C4 0.032(3) 0.027(3) 0.027(3) -0.005(2) 0.000(2) -0.018(3) C5 0.050(4) 0.031(3) 0.047(4) 0.001(3) -0.017(3) -0.020(3) C6 0.057(5) 0.037(4) 0.049(4) 0.003(3) -0.025(4) -0.027(3) C7 0.028(3) 0.028(3) 0.021(3) -0.005(2) 0.003(2) -0.018(3) C8 0.038(4) 0.038(3) 0.038(4) -0.009(3) -0.004(3) -0.025(3) C9 0.036(4) 0.052(4) 0.048(4) -0.018(3) 0.005(3) -0.031(3) C10 0.039(4) 0.042(4) 0.042(4) -0.019(3) 0.005(3) -0.025(3) C11 0.035(3) 0.031(3) 0.026(3) -0.002(2) -0.007(3) -0.021(3) C12 0.040(4) 0.038(4) 0.050(4) -0.015(3) -0.008(3) -0.018(3) C13 0.043(4) 0.036(4) 0.058(5) -0.016(3) -0.010(3) -0.018(3) C14 0.036(3) 0.029(3) 0.020(3) 0.001(2) -0.005(2) -0.019(3) C15 0.046(4) 0.032(3) 0.054(4) 0.003(3) -0.005(3) -0.025(3) C16 0.044(4) 0.025(3) 0.053(4) -0.004(3) 0.003(3) -0.016(3) C17 0.040(4) 0.027(3) 0.050(4) 0.000(3) 0.007(3) -0.017(3) C18 0.032(3) 0.018(3) 0.044(4) 0.005(3) -0.001(3) -0.012(3) C19 0.055(5) 0.034(4) 0.055(5) -0.007(3) 0.020(4) -0.029(3) C20 0.064(5) 0.040(4) 0.078(6) -0.002(4) 0.018(4) -0.038(4) C21 0.032(3) 0.022(3) 0.031(3) 0.004(2) 0.001(3) -0.015(3) C22 0.050(4) 0.031(3) 0.054(4) 0.001(3) -0.004(3) -0.029(3) C23 0.057(5) 0.043(4) 0.066(5) 0.012(4) -0.023(4) -0.039(4) C24 0.047(4) 0.034(3) 0.062(5) 0.016(3) -0.026(4) -0.030(3) C25 0.028(3) 0.023(3) 0.039(3) -0.002(3) -0.002(3) -0.015(3) C26 0.029(3) 0.025(3) 0.053(4) -0.003(3) -0.003(3) -0.014(3) C27 0.040(4) 0.024(3) 0.063(5) -0.001(3) -0.002(3) -0.015(3) C28 0.025(3) 0.023(3) 0.030(3) -0.006(2) 0.003(2) -0.016(2) C29 0.043(4) 0.042(4) 0.041(4) 0.010(3) 0.003(3) -0.028(3) C30 0.037(4) 0.040(4) 0.032(3) 0.001(3) 0.006(3) -0.020(3) C31 0.032(3) 0.027(3) 0.043(4) 0.001(3) 0.007(3) -0.016(3) C32 0.025(3) 0.029(3) 0.029(3) 0.007(2) 0.000(2) -0.014(2) C33 0.049(4) 0.032(3) 0.049(4) -0.005(3) 0.016(3) -0.024(3) C34 0.067(5) 0.028(3) 0.060(5) -0.002(3) 0.020(4) -0.028(3) C35 0.024(3) 0.022(3) 0.026(3) 0.002(2) -0.001(2) -0.012(2) C36 0.044(4) 0.039(4) 0.039(4) 0.009(3) 0.003(3) -0.028(3) C37 0.045(4) 0.040(4) 0.039(4) 0.014(3) -0.002(3) -0.028(3) C38 0.045(4) 0.052(4) 0.045(4) 0.016(3) -0.004(3) -0.033(4) C39 0.039(4) 0.034(3) 0.037(4) 0.009(3) 0.001(3) -0.024(3) C40 0.041(4) 0.042(4) 0.060(5) 0.019(4) -0.005(3) -0.021(3) C41 0.038(4) 0.050(4) 0.068(5) 0.016(4) 0.007(4) -0.025(3) C42 0.037(4) 0.035(3) 0.028(3) 0.008(3) 0.002(3) -0.023(3) C43 0.043(4) 0.025(3) 0.052(4) 0.002(3) -0.007(3) -0.023(3) C44 0.039(4) 0.035(3) 0.054(4) -0.005(3) 0.009(3) -0.026(3) C45 0.031(3) 0.031(3) 0.055(4) -0.006(3) 0.006(3) -0.019(3) C46 0.032(3) 0.023(3) 0.036(3) 0.001(2) 0.000(3) -0.018(3) C47 0.028(3) 0.023(3) 0.059(4) 0.003(3) -0.002(3) -0.015(3) C48 0.036(4) 0.023(3) 0.070(5) -0.002(3) -0.002(3) -0.016(3) C49 0.028(3) 0.021(3) 0.027(3) 0.006(2) -0.005(2) -0.016(3) C50 0.047(4) 0.028(3) 0.060(5) -0.001(3) -0.004(3) -0.025(3) C51 0.078(6) 0.032(4) 0.051(4) 0.014(3) -0.022(4) -0.031(4) C52 0.089(6) 0.038(4) 0.060(5) 0.010(4) -0.031(5) -0.041(4) C53 0.049(4) 0.023(3) 0.041(4) 0.003(3) -0.009(3) -0.023(3) C54 0.068(5) 0.027(3) 0.050(4) 0.010(3) -0.022(4) -0.030(3) C55 0.082(6) 0.044(4) 0.058(5) 0.011(4) -0.030(4) -0.047(4) C56 0.042(4) 0.020(3) 0.040(4) -0.003(3) -0.006(3) -0.019(3) C57 0.039(4) 0.032(3) 0.046(4) -0.005(3) 0.005(3) -0.016(3) C58 0.056(5) 0.029(3) 0.047(4) -0.008(3) 0.003(4) -0.012(3) C59 0.043(4) 0.038(4) 0.040(4) -0.005(3) 0.005(3) 0.004(3) C60 0.034(4) 0.050(4) 0.069(5) -0.008(4) 0.018(4) -0.011(3) C61 0.037(4) 0.038(4) 0.059(5) -0.006(3) 0.010(3) -0.015(3) C62 0.056(5) 0.054(5) 0.045(5) -0.003(4) 0.005(4) 0.015(4) C63 0.066(5) 0.051(5) 0.034(4) -0.001(3) 0.008(4) 0.011(4) C64 0.067(5) 0.035(4) 0.039(4) 0.006(3) 0.005(4) 0.016(4) C65 0.041(4) 0.028(3) 0.040(4) 0.002(3) -0.006(3) -0.010(3) C66 0.056(5) 0.026(3) 0.047(4) 0.002(3) 0.001(4) -0.005(3) C67 0.040(4) 0.037(4) 0.029(3) -0.002(3) 0.003(3) 0.006(3) C68 0.037(4) 0.057(5) 0.039(4) 0.009(3) -0.013(3) -0.008(3) C69 0.038(4) 0.043(4) 0.033(4) 0.003(3) 0.002(3) -0.016(3) C70 0.039(4) 0.039(4) 0.061(5) 0.006(3) -0.007(3) -0.019(3) C71 0.039(4) 0.056(5) 0.063(5) 0.007(4) -0.007(4) -0.022(4) C72 0.040(4) 0.047(4) 0.049(5) -0.005(4) -0.003(3) -0.001(3) C73 0.060(5) 0.047(5) 0.068(6) 0.005(4) -0.004(4) -0.019(4) C74 0.050(5) 0.048(4) 0.057(5) 0.001(4) -0.005(4) -0.025(4) C75 0.057(5) 0.056(5) 0.052(5) -0.002(4) -0.004(4) -0.001(4) C76 0.074(6) 0.050(5) 0.053(5) -0.012(4) -0.018(5) 0.017(4) C77 0.053(5) 0.038(4) 0.042(4) -0.005(3) 0.009(4) 0.004(3) C78 0.037(4) 0.033(3) 0.037(4) -0.002(3) 0.000(3) -0.016(3) C79 0.045(4) 0.024(3) 0.051(4) -0.003(3) -0.003(3) -0.010(3) C80 0.040(4) 0.035(3) 0.025(3) 0.002(3) 0.001(3) -0.003(3) C81 0.036(4) 0.044(4) 0.042(4) 0.001(3) 0.011(3) -0.013(3) C82 0.037(4) 0.037(3) 0.035(4) -0.005(3) 0.007(3) -0.017(3) O1W 0.044(13) 0.11(2) 0.055(15) 0.038(14) 0.010(11) 0.004(13) O2W 0.062(15) 0.058(15) 0.10(2) -0.025(15) 0.027(15) -0.017(13) O3W 0.066(6) 0.066(6) 0.066(6) -0.0009(10) -0.0007(10) -0.027(3) O4W 0.055(5) 0.055(5) 0.056(5) -0.0009(10) -0.0004(10) -0.023(2) O5W 0.027(10) 0.024(9) 0.082(15) 0.012(9) -0.014(10) 0.004(8) _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 Co1 O18 2.044(4) . ? Co1 O1 2.053(4) . ? Co1 O9 2.081(4) . ? Co1 N9 2.110(5) . ? Co1 O35 2.130(5) . ? Co1 O33 2.208(4) . ? Co2 O17 2.069(4) . ? Co2 O2 2.075(4) . ? Co2 N10 2.123(5) 1_465 ? Co2 O11 2.148(4) 1_565 ? Co2 O11 2.171(4) 2_656 ? Co2 O33 2.185(4) . ? Co3 O20 2.039(4) . ? Co3 O4 2.087(4) 1_665 ? Co3 N11 2.106(5) . ? Co3 O25 2.121(4) . ? Co3 O34 2.174(4) . ? Co3 O25 2.190(4) 2_775 ? Co4 O3 2.030(4) 1_665 ? Co4 O27 2.038(4) 1_545 ? Co4 O19 2.092(5) . ? Co4 O36 2.134(6) . ? Co4 N12 2.140(6) 1_645 ? Co4 O34 2.186(4) . ? O1 C7 1.247(7) . ? O2 C7 1.244(7) . ? O3 C14 1.247(7) . ? O3 Co4 2.030(4) 1_445 ? O4 C14 1.248(7) . ? O4 Co3 2.087(4) 1_445 ? O5 N2 1.226(9) . ? O6 N2 1.198(9) . ? O7' N1 1.315(15) . ? O7 N1 1.225(14) . ? O8 N1 1.170(19) . ? O8' N1 1.272(19) . ? O9 C21 1.265(7) . ? O10 C21 1.233(7) . ? O11 C28 1.281(7) . ? O11 Co2 2.148(4) 1_545 ? O11 Co2 2.171(4) 2_656 ? O12 C28 1.242(7) . ? O13' N3 1.210(13) . ? O13 N3 1.311(15) . ? O14 N3 1.223(19) . ? O14' N3 1.197(17) . ? O15 N4 1.143(17) . ? O15' N4 1.286(17) . ? O16' N4 1.114(14) . ? O16 N4 1.433(15) . ? O17 C35 1.246(7) . ? O18 C35 1.250(7) . ? O19 C42 1.244(8) . ? O20 C42 1.250(7) . ? O21 N5 1.239(9) . ? O22 N5 1.206(8) . ? O23' N6 1.233(14) . ? O23 N6 1.238(15) . ? O24' N6 1.277(14) . ? O24 N6 1.230(14) . ? O25 C49 1.300(7) . ? O25 Co3 2.190(4) 2_775 ? O26 C49 1.236(7) . ? O27 C56 1.267(8) . ? O27 Co4 2.038(4) 1_565 ? O28 C56 1.241(7) . ? O29 N7 1.188(10) . ? O30 N7 1.239(9) . ? O31" N8 1.27(2) . ? O31' N8 1.42(2) . ? O31 N8 1.385(16) . ? O32" N8 1.19(3) . ? O32' N8 1.26(3) . ? O32 N8 1.236(18) . ? O35 H1A 0.877(16) . ? O35 H1B 0.824(19) . ? N1 C2 1.460(10) . ? N2 C9 1.483(10) . ? N3 C16 1.469(9) . ? N4 C23 1.468(10) . ? N5 C30 1.466(9) . ? N6 C37 1.450(10) . ? N7 C44 1.472(9) . ? N8 C51 1.465(11) . ? N9 C57 1.339(8) . ? N9 C61 1.339(9) . ? N10 C65 1.331(8) . ? N10 C69 1.339(8) . ? N10 Co2 2.123(5) 1_645 ? N11 C78 1.325(8) . ? N11 C82 1.354(8) . ? N12 C70 1.289(9) . ? N12 C74 1.366(10) . ? N12 Co4 2.140(6) 1_465 ? C1 C6 1.398(9) . ? C1 C2 1.405(9) . ? C1 C8 1.495(8) . ? C2 C3 1.373(9) . ? C3 C4 1.390(8) . ? C3 H3 0.9300 . ? C4 C5 1.378(9) . ? C4 C7 1.507(7) . ? C5 C6 1.395(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.394(10) . ? C8 C9 1.396(9) . ? C9 C10 1.382(8) . ? C10 C11 1.373(9) . ? C10 H10 0.9300 . ? C11 C12 1.390(9) . ? C11 C14 1.512(7) . ? C12 C13 1.384(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C20 1.373(11) . ? C15 C16 1.376(10) . ? C15 C22 1.498(8) . ? C16 C17 1.395(9) . ? C17 C18 1.372(9) . ? C17 H17 0.9300 . ? C18 C19 1.384(9) . ? C18 C21 1.507(8) . ? C19 C20 1.403(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.372(10) . ? C22 C23 1.383(10) . ? C23 C24 1.380(9) . ? C24 C25 1.387(9) . ? C24 H24 0.9300 . ? C25 C26 1.375(9) . ? C25 C28 1.500(7) . ? C26 C27 1.392(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 C34 1.387(10) . ? C29 C30 1.400(9) . ? C29 C36 1.505(8) . ? C30 C31 1.380(9) . ? C31 C32 1.386(9) . ? C31 H31 0.9300 . ? C32 C33 1.381(9) . ? C32 C35 1.503(8) . ? C33 C34 1.377(9) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C36 C41 1.383(10) . ? C36 C37 1.407(9) . ? C37 C38 1.377(9) . ? C38 C39 1.382(9) . ? C38 H38 0.9300 . ? C39 C40 1.368(10) . ? C39 C42 1.515(8) . ? C40 C41 1.388(10) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C43 C44 1.384(9) . ? C43 C48 1.391(9) . ? C43 C50 1.500(8) . ? C44 C45 1.386(8) . ? C45 C46 1.376(8) . ? C45 H45 0.9300 . ? C46 C47 1.378(8) . ? C46 C49 1.501(7) . ? C47 C48 1.379(8) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C50 C51 1.380(10) . ? C50 C55 1.392(10) . ? C51 C52 1.373(9) . ? C52 C53 1.385(10) . ? C52 H52 0.9300 . ? C53 C54 1.362(9) . ? C53 C56 1.502(8) . ? C54 C55 1.387(9) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C57 C58 1.372(10) . ? C57 H57 0.9300 . ? C58 C59 1.372(11) . ? C58 H58 0.9300 . ? C59 C60 1.385(11) . ? C59 C62 1.497(10) . ? C60 C61 1.377(10) . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? C62 C63 1.506(11) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.534(10) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C67 1.524(9) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.381(9) . ? C65 H65 0.9300 . ? C66 C67 1.360(11) . ? C66 H66 0.9300 . ? C67 C68 1.368(11) . ? C68 C69 1.383(10) . ? C68 H68 0.9300 . ? C69 H69 0.9300 . ? C70 C71 1.380(11) . ? C70 H70 0.9300 . ? C71 C72 1.355(11) . ? C71 H71 0.9300 . ? C72 C73 1.392(12) . ? C72 C75 1.499(11) . ? C73 C74 1.347(11) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 C76 1.465(11) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 C77 1.520(11) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C80 1.498(9) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C79 1.375(9) . ? C78 H78 0.9300 . ? C79 C80 1.384(10) . ? C79 H79 0.9300 . ? C80 C81 1.380(10) . ? C81 C82 1.378(9) . ? C81 H81 0.9300 . ? C82 H82 0.9300 . ? O2W O2W 1.27(5) 2_865 ? O3W O4W 1.22(3) . ? O5W O5W 1.44(4) 2_756 ? 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 O18 Co1 O1 101.9(2) . . ? O18 Co1 O9 171.22(17) . . ? O1 Co1 O9 85.10(19) . . ? O18 Co1 N9 86.45(18) . . ? O1 Co1 N9 90.67(19) . . ? O9 Co1 N9 88.19(19) . . ? O18 Co1 O35 88.0(2) . . ? O1 Co1 O35 170.1(2) . . ? O9 Co1 O35 85.2(2) . . ? N9 Co1 O35 91.0(2) . . ? O18 Co1 O33 95.48(15) . . ? O1 Co1 O33 84.59(15) . . ? O9 Co1 O33 90.41(16) . . ? N9 Co1 O33 175.17(18) . . ? O35 Co1 O33 93.49(19) . . ? O17 Co2 O2 110.08(17) . . ? O17 Co2 N10 84.87(19) . 1_465 ? O2 Co2 N10 89.42(18) . 1_465 ? O17 Co2 O11 84.69(16) . 1_565 ? O2 Co2 O11 165.22(16) . 1_565 ? N10 Co2 O11 91.88(17) 1_465 1_565 ? O17 Co2 O11 161.29(15) . 2_656 ? O2 Co2 O11 88.47(15) . 2_656 ? N10 Co2 O11 93.15(18) 1_465 2_656 ? O11 Co2 O11 76.76(15) 1_565 2_656 ? O17 Co2 O33 86.47(16) . . ? O2 Co2 O33 93.60(15) . . ? N10 Co2 O33 171.34(18) 1_465 . ? O11 Co2 O33 87.26(14) 1_565 . ? O11 Co2 O33 95.04(15) 2_656 . ? O20 Co3 O4 107.84(18) . 1_665 ? O20 Co3 N11 89.93(18) . . ? O4 Co3 N11 85.31(18) 1_665 . ? O20 Co3 O25 166.04(16) . . ? O4 Co3 O25 85.94(16) 1_665 . ? N11 Co3 O25 93.58(17) . . ? O20 Co3 O34 90.72(16) . . ? O4 Co3 O34 89.80(15) 1_665 . ? N11 Co3 O34 175.03(17) . . ? O25 Co3 O34 86.95(15) . . ? O20 Co3 O25 89.97(16) . 2_775 ? O4 Co3 O25 161.50(15) 1_665 2_775 ? N11 Co3 O25 89.87(17) . 2_775 ? O25 Co3 O25 76.54(15) . 2_775 ? O34 Co3 O25 95.06(15) . 2_775 ? O3 Co4 O27 172.5(2) 1_665 1_545 ? O3 Co4 O19 99.7(2) 1_665 . ? O27 Co4 O19 87.4(2) 1_545 . ? O3 Co4 O36 84.7(2) 1_665 . ? O27 Co4 O36 88.2(2) 1_545 . ? O19 Co4 O36 175.6(2) . . ? O3 Co4 N12 89.34(19) 1_665 1_645 ? O27 Co4 N12 88.5(2) 1_545 1_645 ? O19 Co4 N12 87.8(2) . 1_645 ? O36 Co4 N12 92.3(3) . 1_645 ? O3 Co4 O34 93.63(15) 1_665 . ? O27 Co4 O34 88.97(17) 1_545 . ? O19 Co4 O34 88.69(17) . . ? O36 Co4 O34 91.0(2) . . ? N12 Co4 O34 175.7(2) 1_645 . ? C7 O1 Co1 139.7(4) . . ? C7 O2 Co2 129.4(4) . . ? C14 O3 Co4 130.3(4) . 1_445 ? C14 O4 Co3 139.7(4) . 1_445 ? C21 O9 Co1 124.1(4) . . ? C28 O11 Co2 118.6(3) . 1_545 ? C28 O11 Co2 127.7(4) . 2_656 ? Co2 O11 Co2 103.24(15) 1_545 2_656 ? C35 O17 Co2 134.9(4) . . ? C35 O18 Co1 133.1(4) . . ? C42 O19 Co4 138.3(4) . . ? C42 O20 Co3 128.0(4) . . ? C49 O25 Co3 117.3(3) . . ? C49 O25 Co3 128.0(4) . 2_775 ? Co3 O25 Co3 103.46(15) . 2_775 ? C56 O27 Co4 130.5(4) . 1_565 ? Co2 O33 Co1 109.90(17) . . ? Co3 O34 Co4 110.79(17) . . ? Co1 O35 H1A 111.8(17) . . ? Co1 O35 H1B 117(2) . . ? H1A O35 H1B 112(3) . . ? O8 N1 O7 116.0(13) . . ? O8 N1 O8' 17.2(6) . . ? O7 N1 O8' 117.7(12) . . ? O8 N1 O7' 118.3(11) . . ? O7 N1 O7' 33.1(7) . . ? O8' N1 O7' 130.1(11) . . ? O8 N1 C2 122.8(11) . . ? O7 N1 C2 120.5(9) . . ? O8' N1 C2 115.9(10) . . ? O7' N1 C2 113.3(8) . . ? O6 N2 O5 123.5(8) . . ? O6 N2 C9 119.2(7) . . ? O5 N2 C9 117.2(7) . . ? O14' N3 O13' 114.9(11) . . ? O14' N3 O14 19.7(5) . . ? O13' N3 O14 118.7(12) . . ? O14' N3 O13 126.3(11) . . ? O13' N3 O13 39.5(7) . . ? O14 N3 O13 115.4(11) . . ? O14' N3 C16 118.3(9) . . ? O13' N3 C16 119.2(8) . . ? O14 N3 C16 121.4(10) . . ? O13 N3 C16 114.1(8) . . ? O16' N4 O15 111.6(13) . . ? O16' N4 O15' 115.7(12) . . ? O15 N4 O15' 20.2(6) . . ? O16' N4 O16 30.2(8) . . ? O15 N4 O16 123.3(11) . . ? O15' N4 O16 136.7(11) . . ? O16' N4 C23 126.1(10) . . ? O15 N4 C23 122.2(11) . . ? O15' N4 C23 113.8(10) . . ? O16 N4 C23 109.3(8) . . ? O22 N5 O21 123.6(7) . . ? O22 N5 C30 118.5(6) . . ? O21 N5 C30 117.8(7) . . ? O24 N6 O23' 107.8(11) . . ? O24 N6 O23 127.0(11) . . ? O23' N6 O23 34.1(7) . . ? O24 N6 O24' 37.0(7) . . ? O23' N6 O24' 115.8(11) . . ? O23 N6 O24' 112.0(11) . . ? O24 N6 C37 116.8(9) . . ? O23' N6 C37 125.1(9) . . ? O23 N6 C37 116.2(9) . . ? O24' N6 C37 119.0(9) . . ? O29 N7 O30 123.1(8) . . ? O29 N7 C44 121.0(6) . . ? O30 N7 C44 115.9(8) . . ? O32" N8 O32 25.4(12) . . ? O32" N8 O32' 19.3(15) . . ? O32 N8 O32' 42.2(11) . . ? O32" N8 O31" 113.8(18) . . ? O32 N8 O31" 118.8(14) . . ? O32' N8 O31" 119.2(17) . . ? O32" N8 O31 112.9(14) . . ? O32 N8 O31 98.4(11) . . ? O32' N8 O31 130.6(14) . . ? O31" N8 O31 44.4(10) . . ? O32" N8 O31' 103.5(17) . . ? O32 N8 O31' 122.7(13) . . ? O32' N8 O31' 98.0(15) . . ? O31" N8 O31' 34.7(10) . . ? O31 N8 O31' 79.1(11) . . ? O32" N8 C51 126.9(16) . . ? O32 N8 C51 121.4(11) . . ? O32' N8 C51 114.7(13) . . ? O31" N8 C51 117.9(11) . . ? O31 N8 C51 111.7(9) . . ? O31' N8 C51 111.8(10) . . ? C57 N9 C61 116.8(6) . . ? C57 N9 Co1 121.8(4) . . ? C61 N9 Co1 121.3(4) . . ? C65 N10 C69 117.0(5) . . ? C65 N10 Co2 120.5(4) . 1_645 ? C69 N10 Co2 122.3(4) . 1_645 ? C78 N11 C82 117.2(5) . . ? C78 N11 Co3 118.9(4) . . ? C82 N11 Co3 123.7(4) . . ? C70 N12 C74 114.6(6) . . ? C70 N12 Co4 127.7(5) . 1_465 ? C74 N12 Co4 117.5(5) . 1_465 ? C6 C1 C2 115.7(5) . . ? C6 C1 C8 118.8(6) . . ? C2 C1 C8 125.4(6) . . ? C3 C2 C1 122.3(6) . . ? C3 C2 N1 115.8(6) . . ? C1 C2 N1 122.0(6) . . ? C2 C3 C4 120.9(6) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 118.2(5) . . ? C5 C4 C7 123.0(5) . . ? C3 C4 C7 118.8(5) . . ? C4 C5 C6 120.6(6) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 122.0(6) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? O2 C7 O1 127.7(5) . . ? O2 C7 C4 118.0(5) . . ? O1 C7 C4 114.2(5) . . ? C13 C8 C9 115.9(5) . . ? C13 C8 C1 118.1(6) . . ? C9 C8 C1 126.1(6) . . ? C10 C9 C8 121.9(6) . . ? C10 C9 N2 116.0(6) . . ? C8 C9 N2 122.1(6) . . ? C11 C10 C9 121.3(6) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 118.0(5) . . ? C10 C11 C14 120.3(5) . . ? C12 C11 C14 121.6(6) . . ? C13 C12 C11 120.4(6) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 122.4(6) . . ? C12 C13 H13 118.8 . . ? C8 C13 H13 118.8 . . ? O3 C14 O4 127.3(5) . . ? O3 C14 C11 115.6(5) . . ? O4 C14 C11 117.0(5) . . ? C20 C15 C16 117.0(6) . . ? C20 C15 C22 118.0(6) . . ? C16 C15 C22 124.9(6) . . ? C15 C16 C17 122.2(6) . . ? C15 C16 N3 122.7(6) . . ? C17 C16 N3 115.1(6) . . ? C18 C17 C16 120.2(6) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 118.7(5) . . ? C17 C18 C21 120.1(6) . . ? C19 C18 C21 121.2(6) . . ? C18 C19 C20 119.9(6) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C15 C20 C19 121.9(7) . . ? C15 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? O10 C21 O9 126.1(5) . . ? O10 C21 C18 118.5(5) . . ? O9 C21 C18 115.4(5) . . ? C27 C22 C23 117.2(6) . . ? C27 C22 C15 119.3(6) . . ? C23 C22 C15 123.5(6) . . ? C24 C23 C22 122.6(6) . . ? C24 C23 N4 116.4(7) . . ? C22 C23 N4 121.0(6) . . ? C23 C24 C25 119.0(6) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 119.3(5) . . ? C26 C25 C28 121.4(5) . . ? C24 C25 C28 119.3(5) . . ? C25 C26 C27 120.4(6) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C22 C27 C26 121.3(6) . . ? C22 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? O12 C28 O11 123.9(5) . . ? O12 C28 C25 118.8(5) . . ? O11 C28 C25 117.3(5) . . ? C34 C29 C30 116.0(6) . . ? C34 C29 C36 117.8(6) . . ? C30 C29 C36 126.1(6) . . ? C31 C30 C29 122.2(6) . . ? C31 C30 N5 116.7(6) . . ? C29 C30 N5 121.2(6) . . ? C30 C31 C32 120.3(6) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 118.1(5) . . ? C33 C32 C35 121.9(5) . . ? C31 C32 C35 119.9(5) . . ? C34 C33 C32 121.0(6) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C29 122.1(6) . . ? C33 C34 H34 118.9 . . ? C29 C34 H34 118.9 . . ? O17 C35 O18 125.7(5) . . ? O17 C35 C32 117.2(5) . . ? O18 C35 C32 117.1(5) . . ? C41 C36 C37 116.5(6) . . ? C41 C36 C29 117.9(6) . . ? C37 C36 C29 125.4(6) . . ? C38 C37 C36 121.1(6) . . ? C38 C37 N6 116.7(7) . . ? C36 C37 N6 122.1(6) . . ? C37 C38 C39 120.8(6) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 119.1(6) . . ? C40 C39 C42 122.0(6) . . ? C38 C39 C42 118.9(6) . . ? C39 C40 C41 120.2(6) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C36 C41 C40 122.2(7) . . ? C36 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? O19 C42 O20 126.0(5) . . ? O19 C42 C39 117.1(6) . . ? O20 C42 C39 116.9(5) . . ? C44 C43 C48 116.8(5) . . ? C44 C43 C50 125.7(6) . . ? C48 C43 C50 117.5(6) . . ? C43 C44 C45 122.5(6) . . ? C43 C44 N7 123.0(6) . . ? C45 C44 N7 114.5(6) . . ? C46 C45 C44 119.0(6) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C45 C46 C47 120.1(5) . . ? C45 C46 C49 118.9(5) . . ? C47 C46 C49 120.9(5) . . ? C46 C47 C48 119.8(6) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C47 C48 C43 121.7(6) . . ? C47 C48 H48 119.1 . . ? C43 C48 H48 119.1 . . ? O26 C49 O25 124.3(5) . . ? O26 C49 C46 119.0(5) . . ? O25 C49 C46 116.7(5) . . ? C51 C50 C55 116.0(6) . . ? C51 C50 C43 126.0(6) . . ? C55 C50 C43 117.9(6) . . ? C52 C51 C50 122.5(7) . . ? C52 C51 N8 116.5(7) . . ? C50 C51 N8 121.1(6) . . ? C51 C52 C53 120.7(7) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C54 C53 C52 117.9(6) . . ? C54 C53 C56 122.9(6) . . ? C52 C53 C56 119.1(6) . . ? C53 C54 C55 121.2(6) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? C54 C55 C50 121.6(6) . . ? C54 C55 H55 119.2 . . ? C50 C55 H55 119.2 . . ? O28 C56 O27 126.1(5) . . ? O28 C56 C53 119.2(5) . . ? O27 C56 C53 114.7(5) . . ? N9 C57 C58 123.0(6) . . ? N9 C57 H57 118.5 . . ? C58 C57 H57 118.5 . . ? C57 C58 C59 120.2(7) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C58 C59 C60 117.5(6) . . ? C58 C59 C62 122.4(8) . . ? C60 C59 C62 120.1(8) . . ? C61 C60 C59 119.2(7) . . ? C61 C60 H60 120.4 . . ? C59 C60 H60 120.4 . . ? N9 C61 C60 123.4(7) . . ? N9 C61 H61 118.3 . . ? C60 C61 H61 118.3 . . ? C59 C62 C63 112.0(7) . . ? C59 C62 H62A 109.2 . . ? C63 C62 H62A 109.2 . . ? C59 C62 H62B 109.2 . . ? C63 C62 H62B 109.2 . . ? H62A C62 H62B 107.9 . . ? C62 C63 C64 111.5(6) . . ? C62 C63 H63A 109.3 . . ? C64 C63 H63A 109.3 . . ? C62 C63 H63B 109.3 . . ? C64 C63 H63B 109.3 . . ? H63A C63 H63B 108.0 . . ? C67 C64 C63 110.7(6) . . ? C67 C64 H64A 109.5 . . ? C63 C64 H64A 109.5 . . ? C67 C64 H64B 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? N10 C65 C66 124.0(7) . . ? N10 C65 H65 118.0 . . ? C66 C65 H65 118.0 . . ? C67 C66 C65 119.1(7) . . ? C67 C66 H66 120.4 . . ? C65 C66 H66 120.4 . . ? C66 C67 C68 117.3(6) . . ? C66 C67 C64 122.9(7) . . ? C68 C67 C64 119.8(7) . . ? C67 C68 C69 121.4(7) . . ? C67 C68 H68 119.3 . . ? C69 C68 H68 119.3 . . ? N10 C69 C68 121.1(6) . . ? N10 C69 H69 119.4 . . ? C68 C69 H69 119.4 . . ? N12 C70 C71 125.0(7) . . ? N12 C70 H70 117.5 . . ? C71 C70 H70 117.5 . . ? C72 C71 C70 120.3(7) . . ? C72 C71 H71 119.8 . . ? C70 C71 H71 119.8 . . ? C71 C72 C73 115.7(7) . . ? C71 C72 C75 124.6(8) . . ? C73 C72 C75 119.7(8) . . ? C74 C73 C72 120.1(8) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C73 C74 N12 123.7(7) . . ? C73 C74 H74 118.1 . . ? N12 C74 H74 118.1 . . ? C76 C75 C72 114.1(7) . . ? C76 C75 H75A 108.7 . . ? C72 C75 H75A 108.7 . . ? C76 C75 H75B 108.7 . . ? C72 C75 H75B 108.7 . . ? H75A C75 H75B 107.6 . . ? C75 C76 C77 114.0(7) . . ? C75 C76 H76A 108.7 . . ? C77 C76 H76A 108.7 . . ? C75 C76 H76B 108.7 . . ? C77 C76 H76B 108.7 . . ? H76A C76 H76B 107.6 . . ? C80 C77 C76 112.5(6) . . ? C80 C77 H77A 109.1 . . ? C76 C77 H77A 109.1 . . ? C80 C77 H77B 109.1 . . ? C76 C77 H77B 109.1 . . ? H77A C77 H77B 107.8 . . ? N11 C78 C79 123.3(6) . . ? N11 C78 H78 118.3 . . ? C79 C78 H78 118.3 . . ? C78 C79 C80 120.2(6) . . ? C78 C79 H79 119.9 . . ? C80 C79 H79 119.9 . . ? C81 C80 C79 116.5(6) . . ? C81 C80 C77 121.9(7) . . ? C79 C80 C77 121.5(7) . . ? C82 C81 C80 120.6(6) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? N11 C82 C81 122.1(6) . . ? N11 C82 H82 119.0 . . ? C81 C82 H82 119.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O35 H1A O5W 0.877(16) 2.044(17) 2.850(16) 152(3) . O35 H1A O14' 0.877(16) 2.56(3) 3.012(14) 113(2) 2_756 O35 H1B O3W 0.824(19) 1.94(3) 2.72(3) 159(5) . O35 H1B O4W 0.824(19) 2.08(6) 2.70(2) 132(7) . _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.239 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.114 #=========================END data_Compound-3 #TrackingRef 'cif.txt' _database_code_depnum_ccdc_archive 'CCDC 778425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C27 H24 N4 Ni O10' _chemical_formula_sum 'C27 H24 N4 Ni O10' _chemical_formula_weight 623.21 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' Ni Ni 0.3393 1.1124 '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 8.1758(16) _cell_length_b 11.792(2) _cell_length_c 14.983(3) _cell_angle_alpha 73.99(3) _cell_angle_beta 77.45(3) _cell_angle_gamma 78.48(3) _cell_volume 1340.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6016 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 0.791 _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 '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 13142 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6016 _reflns_number_gt 3460 _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. Standard DFIX restraints were used for the distance of the atoms, such as (o8 and o8'), (c22' and c21), (c22 and c25), (c22' and c25'). To improve the parameters chemical more reasonable, ultimately restrain instructions EXYZ for (c24 and c25') and EADP for (c24, c25', o5, o5', o6, o6') were applied in the refinement. ; _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^)+(0.1085P)^2^+2.0092P] 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 SHELXL _refine_ls_extinction_coef 0.026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6016 _refine_ls_number_parameters 443 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1471 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2410 _refine_ls_wR_factor_gt 0.2007 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.051 _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 Ni1 Ni -0.50126(9) 1.27600(6) 1.38391(5) 0.0330(3) Uani 1 1 d . . . O1 O -0.3545(5) 1.3016(4) 1.2511(3) 0.0420(10) Uani 1 1 d . . . O2 O -0.1465(5) 1.3873(3) 1.2687(3) 0.0372(9) Uani 1 1 d . . . O3 O 0.3674(5) 1.2562(3) 0.5232(3) 0.0384(10) Uani 1 1 d . . . O4 O 0.5065(6) 1.0842(4) 0.5979(3) 0.0444(11) Uani 1 1 d . B . O5 O 0.358(2) 1.392(3) 1.0498(16) 0.0575(14) Uani 0.50 1 d P A 1 O5' O 0.382(2) 1.386(3) 1.0342(17) 0.0575(14) Uani 0.50 1 d P A 2 O6 O 0.4176(12) 1.2535(10) 0.9590(7) 0.0575(14) Uani 0.50 1 d P A 1 O6' O 0.4047(12) 1.3379(10) 0.9188(7) 0.0575(14) Uani 0.50 1 d P A 2 O7 O 0.258(2) 1.0586(14) 1.0182(10) 0.074(5) Uani 0.50 1 d P B 1 O7' O 0.1618(18) 1.0442(14) 1.0172(12) 0.074(5) Uani 0.50 1 d P B 2 O8 O 0.351(2) 0.942(2) 0.9362(11) 0.043(4) Uani 0.50 1 d PD B 1 O8' O 0.393(3) 0.957(3) 0.9282(18) 0.079(7) Uani 0.50 1 d PD B 2 O1W O -0.3140(6) 1.3306(5) 1.4331(3) 0.0584(13) Uani 1 1 d . . . O2W O -0.3617(5) 1.1043(3) 1.4187(3) 0.0371(9) Uani 1 1 d . . . N1 N 0.3201(6) 1.3379(6) 0.9969(4) 0.0515(15) Uani 1 1 d . . . N2 N 0.2831(8) 1.0391(5) 0.9421(4) 0.0535(15) Uani 1 1 d . . . N3 N -0.6720(6) 1.2047(4) 1.3382(3) 0.0303(10) Uani 1 1 d . . . N4 N -0.6281(8) 0.4478(5) 1.3536(4) 0.0542(15) Uani 1 1 d . . . C1 C -0.2169(7) 1.3421(4) 1.2238(4) 0.0310(12) Uani 1 1 d . . . C2 C -0.1214(7) 1.3283(5) 1.1268(4) 0.0306(12) Uani 1 1 d . A . C3 C 0.0472(7) 1.3487(5) 1.0996(4) 0.0331(12) Uani 1 1 d . . . H3 H 0.0961 1.3795 1.1366 0.080 Uiso 1 1 calc . . . C4 C 0.1402(7) 1.3226(5) 1.0171(4) 0.0334(13) Uani 1 1 d . A . C5 C 0.0746(8) 1.2775(5) 0.9582(4) 0.0414(15) Uani 1 1 d . . . C6 C -0.0969(10) 1.2656(7) 0.9850(4) 0.060(2) Uani 1 1 d . A . H6 H -0.1489 1.2405 0.9460 0.080 Uiso 1 1 calc . . . C7 C -0.1920(8) 1.2901(7) 1.0678(4) 0.0504(17) Uani 1 1 d . . . H7 H -0.3057 1.2803 1.0834 0.080 Uiso 1 1 calc . . . C8 C 0.1674(8) 1.2493(5) 0.8679(4) 0.0402(14) Uani 1 1 d . A . C9 C 0.2615(8) 1.1400(6) 0.8584(4) 0.0432(15) Uani 1 1 d . A . C10 C 0.3384(8) 1.1171(5) 0.7719(4) 0.0418(15) Uani 1 1 d . . . H10 H 0.4000 1.0426 0.7687 0.080 Uiso 1 1 calc . . . C11 C 0.3229(8) 1.2065(5) 0.6897(4) 0.0410(15) Uani 1 1 d . B . C12 C 0.2327(9) 1.3156(6) 0.6974(4) 0.0504(17) Uani 1 1 d . . . H12 H 0.2222 1.3763 0.6432 0.080 Uiso 1 1 calc . . . C13 C 0.1568(9) 1.3370(6) 0.7846(4) 0.0483(17) Uani 1 1 d . A . H13 H 0.0970 1.4121 0.7874 0.080 Uiso 1 1 calc . . . C14 C 0.4048(8) 1.1802(5) 0.5962(4) 0.0378(14) Uani 1 1 d . . . C15 C -0.6314(7) 1.1755(5) 1.2545(4) 0.0356(13) Uani 1 1 d . . . H15 H -0.5316 1.1961 1.2150 0.080 Uiso 1 1 calc . . . C16 C -0.7302(7) 1.1168(5) 1.2249(4) 0.0384(14) Uani 1 1 d . . . H16 H -0.6967 1.0986 1.1664 0.080 Uiso 1 1 calc . . . C17 C -0.8814(6) 1.0842(5) 1.2822(4) 0.0294(12) Uani 1 1 d . . . C18 C -0.9223(7) 1.1140(5) 1.3677(4) 0.0390(14) Uani 1 1 d . . . H18 H -1.0215 1.0942 1.4083 0.080 Uiso 1 1 calc . . . C19 C -0.8171(7) 1.1733(5) 1.3938(4) 0.0373(14) Uani 1 1 d . . . H19 H -0.8480 1.1923 1.4521 0.080 Uiso 1 1 calc . . . C20 C -0.9856(7) 1.0146(5) 1.2511(4) 0.0374(13) Uani 1 1 d . C . H20A H -0.9957 1.0506 1.1857 0.080 Uiso 1 1 calc . . . H20B H -1.0987 1.0197 1.2883 0.080 Uiso 1 1 calc . . . C21 C -0.9097(9) 0.8845(6) 1.2614(6) 0.063(2) Uani 1 1 d D . . C22 C -0.8795(13) 0.8176(8) 1.3475(8) 0.031(2) Uani 0.50 1 d PD C 1 H22A H -0.9858 0.8188 1.3915 0.080 Uiso 0.50 1 calc P D 1 H22B H -0.8048 0.8552 1.3688 0.080 Uiso 0.50 1 calc P E 1 C22' C -0.7439(15) 0.8153(12) 1.2402(10) 0.059(4) Uani 0.50 1 d PD C 2 H22C H -0.6654 0.8556 1.2558 0.080 Uiso 0.50 1 calc P F 2 H22D H -0.7208 0.8291 1.1721 0.080 Uiso 0.50 1 calc P G 2 C23 C -0.5828(14) 0.5411(10) 1.2966(9) 0.038(3) Uani 0.50 1 d P C 1 H23 H -0.4767 0.5303 1.2594 0.080 Uiso 0.50 1 calc P H 1 C23' C -0.6264(18) 0.4963(12) 1.2472(8) 0.048(3) Uani 0.50 1 d P C 2 H23' H -0.5932 0.4456 1.2066 0.080 Uiso 0.50 1 calc P I 2 C24 C -0.6800(12) 0.6765(7) 1.2780(6) 0.077(3) Uani 0.50 1 d P C 1 C24' C -0.6752(16) 0.6171(12) 1.2132(8) 0.043(3) Uani 0.50 1 d P C 2 H24' H -0.7013 0.6523 1.1533 0.080 Uiso 0.50 1 calc P J 2 C25 C -0.8012(13) 0.6885(9) 1.3521(8) 0.025(2) Uani 0.50 1 d PD C 1 C25' C -0.6800(12) 0.6765(7) 1.2780(6) 0.077(3) Uani 0.50 1 d PD C 2 C26 C -0.8626(13) 0.5932(9) 1.4202(7) 0.030(2) Uani 0.50 1 d P C 1 H26 H -0.9603 0.6073 1.4633 0.080 Uiso 0.50 1 calc P K 1 C26' C -0.684(3) 0.6444(14) 1.3620(12) 0.075(6) Uani 0.50 1 d P C 2 H26' H -0.7140 0.6964 1.4015 0.080 Uiso 0.50 1 calc P L 2 C27 C -0.7823(14) 0.4799(10) 1.4249(7) 0.031(2) Uani 0.50 1 d P C 1 H27 H -0.8233 0.4190 1.4739 0.080 Uiso 0.50 1 calc P M 1 C27' C -0.639(3) 0.5180(13) 1.3950(10) 0.074(5) Uani 0.50 1 d P C 2 H27' H -0.6156 0.4904 1.4560 0.080 Uiso 0.50 1 calc P N 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0405(5) 0.0313(4) 0.0273(4) -0.0047(3) -0.0026(3) -0.0123(3) O1 0.033(2) 0.059(3) 0.033(2) -0.0024(19) 0.0012(19) -0.0246(19) O2 0.041(2) 0.033(2) 0.042(2) -0.0184(18) 0.0010(19) -0.0127(18) O3 0.047(2) 0.036(2) 0.029(2) -0.0068(17) 0.0042(19) -0.0108(18) O4 0.059(3) 0.040(3) 0.029(2) -0.0067(18) -0.003(2) -0.004(2) O5 0.039(3) 0.083(4) 0.059(5) -0.039(4) 0.012(3) -0.018(4) O5' 0.039(3) 0.083(4) 0.059(5) -0.039(4) 0.012(3) -0.018(4) O6 0.039(3) 0.083(4) 0.059(5) -0.039(4) 0.012(3) -0.018(4) O6' 0.039(3) 0.083(4) 0.059(5) -0.039(4) 0.012(3) -0.018(4) O7 0.118(13) 0.065(9) 0.022(5) -0.018(5) 0.022(9) 0.001(9) O7' 0.088(10) 0.046(7) 0.053(7) -0.003(5) 0.044(9) -0.008(8) O8 0.062(10) 0.044(8) 0.012(5) 0.004(5) -0.001(6) -0.001(8) O8' 0.052(9) 0.080(15) 0.067(11) 0.006(8) 0.030(7) -0.001(7) O1W 0.075(3) 0.078(4) 0.032(2) -0.007(2) -0.007(2) -0.049(3) O2W 0.0304(19) 0.044(2) 0.0299(19) -0.0010(17) -0.0013(17) -0.0044(17) N1 0.033(3) 0.081(4) 0.046(3) -0.031(3) 0.008(3) -0.012(3) N2 0.081(5) 0.044(4) 0.031(3) -0.006(2) 0.000(3) -0.014(3) N3 0.034(2) 0.022(2) 0.031(2) -0.0016(18) -0.002(2) -0.0059(18) N4 0.071(4) 0.027(3) 0.069(4) -0.005(3) -0.022(3) -0.016(3) C1 0.036(3) 0.019(3) 0.032(3) -0.001(2) -0.006(3) 0.001(2) C2 0.031(3) 0.029(3) 0.030(3) -0.002(2) -0.007(2) -0.007(2) C3 0.040(3) 0.026(3) 0.037(3) -0.005(2) -0.012(3) -0.010(2) C4 0.035(3) 0.027(3) 0.032(3) -0.003(2) 0.001(3) -0.004(2) C5 0.053(4) 0.039(3) 0.033(3) -0.010(3) 0.004(3) -0.020(3) C6 0.075(5) 0.088(6) 0.033(3) -0.020(3) 0.002(3) -0.052(4) C7 0.047(4) 0.077(5) 0.031(3) -0.007(3) -0.004(3) -0.030(3) C8 0.057(4) 0.036(3) 0.031(3) -0.013(2) 0.005(3) -0.024(3) C9 0.060(4) 0.045(4) 0.026(3) -0.007(3) 0.002(3) -0.024(3) C10 0.060(4) 0.040(3) 0.029(3) -0.010(3) 0.001(3) -0.025(3) C11 0.052(4) 0.040(3) 0.032(3) -0.013(3) 0.007(3) -0.020(3) C12 0.071(5) 0.044(4) 0.035(3) -0.009(3) 0.007(3) -0.025(3) C13 0.067(4) 0.040(4) 0.036(3) -0.011(3) 0.009(3) -0.022(3) C14 0.051(4) 0.040(4) 0.026(3) -0.007(2) -0.002(3) -0.024(3) C15 0.039(3) 0.041(3) 0.024(3) 0.002(2) -0.005(3) -0.015(3) C16 0.043(3) 0.045(4) 0.028(3) 0.000(2) -0.011(3) -0.015(3) C17 0.026(3) 0.025(3) 0.033(3) 0.002(2) -0.007(2) -0.005(2) C18 0.032(3) 0.041(3) 0.046(3) -0.019(3) 0.004(3) -0.008(3) C19 0.029(3) 0.034(3) 0.051(4) -0.020(3) 0.001(3) -0.006(2) C20 0.032(3) 0.042(3) 0.040(3) -0.008(3) -0.009(3) -0.010(3) C21 0.068(5) 0.043(4) 0.098(6) -0.040(4) -0.048(5) 0.013(3) C22 0.033(5) 0.017(5) 0.043(6) -0.005(4) -0.010(5) -0.005(4) C22' 0.053(8) 0.082(11) 0.061(9) -0.035(8) -0.007(7) -0.032(8) C23 0.036(6) 0.022(6) 0.044(7) -0.001(5) 0.006(6) 0.003(5) C23' 0.066(9) 0.056(9) 0.027(6) -0.007(6) -0.014(6) -0.017(7) C24 0.107(7) 0.075(6) 0.057(5) -0.029(4) 0.021(5) -0.053(5) C24' 0.043(7) 0.051(8) 0.033(6) -0.008(6) -0.001(6) -0.007(6) C25 0.022(5) 0.031(6) 0.029(6) -0.009(5) -0.014(5) -0.002(4) C25' 0.107(7) 0.075(6) 0.057(5) -0.029(4) 0.021(5) -0.053(5) C26 0.034(6) 0.027(6) 0.029(5) -0.012(4) -0.010(5) 0.010(4) C26' 0.149(19) 0.039(9) 0.056(10) -0.022(8) -0.016(12) -0.041(11) C27 0.032(6) 0.032(6) 0.023(5) -0.004(4) -0.004(5) 0.001(5) C27' 0.141(17) 0.044(9) 0.037(7) -0.014(7) -0.007(9) -0.018(10) _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 Ni1 N4 2.060(6) 1_565 ? Ni1 O1 2.065(4) . ? Ni1 N3 2.080(5) . ? Ni1 O3 2.102(4) 1_456 ? Ni1 O2W 2.104(4) . ? Ni1 O1W 2.109(5) . ? O1 C1 1.252(6) . ? O2 C1 1.249(6) . ? O3 C14 1.260(7) . ? O3 Ni1 2.102(4) 1_654 ? O4 C14 1.261(7) . ? O5 N1 1.27(2) . ? O5' N1 1.14(2) . ? O6 N1 1.321(11) . ? O6' N1 1.223(10) . ? O7 N2 1.191(15) . ? O7' N2 1.335(15) . ? O8 N2 1.19(3) . ? O8' N2 1.22(3) . ? N1 C4 1.473(7) . ? N2 C9 1.486(8) . ? N3 C15 1.347(7) . ? N3 C19 1.347(7) . ? N4 C27' 1.144(14) . ? N4 C23 1.259(12) . ? N4 C27 1.524(12) . ? N4 C23' 1.537(13) . ? N4 Ni1 2.060(6) 1_545 ? C1 C2 1.528(7) . ? C2 C7 1.365(8) . ? C2 C3 1.400(7) . ? C3 C4 1.382(7) . ? C3 H3 0.9300 . ? C4 C5 1.388(8) . ? C5 C6 1.397(9) . ? C5 C8 1.489(8) . ? C6 C7 1.383(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.389(9) . ? C8 C13 1.390(8) . ? C9 C10 1.385(8) . ? C10 C11 1.394(8) . ? C10 H10 0.9300 . ? C11 C12 1.370(9) . ? C11 C14 1.502(7) . ? C12 C13 1.386(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.370(8) . ? C15 H15 0.9300 . ? C16 C17 1.400(8) . ? C16 H16 0.9300 . ? C17 C18 1.375(8) . ? C17 C20 1.510(8) . ? C18 C19 1.386(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.514(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.360(13) . ? C21 C22' 1.455(12) . ? C22 C25 1.518(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C23 C24 1.614(14) . ? C23 H23 0.9300 . ? C23' C24' 1.382(18) . ? C23' H23' 0.9300 . ? C24 C25 1.337(14) . ? C24' H24' 0.9300 . ? C25 C26 1.388(15) . ? C26 C27 1.356(14) . ? C26 H26 0.9300 . ? C26' C27' 1.43(2) . ? C26' H26' 0.9300 . ? C27 H27 0.9300 . ? C27' H27' 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 N4 Ni1 O1 91.7(2) 1_565 . ? N4 Ni1 N3 94.3(2) 1_565 . ? O1 Ni1 N3 90.31(16) . . ? N4 Ni1 O3 88.2(2) 1_565 1_456 ? O1 Ni1 O3 174.42(16) . 1_456 ? N3 Ni1 O3 95.26(17) . 1_456 ? N4 Ni1 O2W 176.5(2) 1_565 . ? O1 Ni1 O2W 88.67(16) . . ? N3 Ni1 O2W 89.20(16) . . ? O3 Ni1 O2W 91.13(15) 1_456 . ? N4 Ni1 O1W 91.6(2) 1_565 . ? O1 Ni1 O1W 89.33(16) . . ? N3 Ni1 O1W 174.13(19) . . ? O3 Ni1 O1W 85.09(17) 1_456 . ? O2W Ni1 O1W 84.93(19) . . ? C1 O1 Ni1 128.3(4) . . ? C14 O3 Ni1 128.2(4) . 1_654 ? O5' N1 O6' 109.0(11) . . ? O5' N1 O5 12.3(13) . . ? O6' N1 O5 120.8(12) . . ? O5' N1 O6 117.7(12) . . ? O6' N1 O6 46.6(6) . . ? O5 N1 O6 127.7(12) . . ? O5' N1 C4 125.8(8) . . ? O6' N1 C4 120.6(6) . . ? O5 N1 C4 113.6(8) . . ? O6 N1 C4 111.8(6) . . ? O8 N2 O7 116.5(12) . . ? O8 N2 O8' 19.0(6) . . ? O7 N2 O8' 116.7(16) . . ? O8 N2 O7' 115.8(11) . . ? O7 N2 O7' 38.3(10) . . ? O8' N2 O7' 129.0(13) . . ? O8 N2 C9 122.9(9) . . ? O7 N2 C9 119.4(9) . . ? O8' N2 C9 115.4(13) . . ? O7' N2 C9 114.6(9) . . ? C15 N3 C19 116.9(5) . . ? C15 N3 Ni1 120.3(4) . . ? C19 N3 Ni1 122.4(4) . . ? C27' N4 C23 71.7(10) . . ? C27' N4 C27 55.4(11) . . ? C23 N4 C27 110.0(8) . . ? C27' N4 C23' 115.5(10) . . ? C23 N4 C23' 48.0(8) . . ? C27 N4 C23' 121.0(8) . . ? C27' N4 Ni1 126.2(10) . 1_545 ? C23 N4 Ni1 130.8(7) . 1_545 ? C27 N4 Ni1 117.2(5) . 1_545 ? C23' N4 Ni1 111.3(6) . 1_545 ? O2 C1 O1 127.1(5) . . ? O2 C1 C2 116.9(5) . . ? O1 C1 C2 115.9(5) . . ? C7 C2 C3 118.7(5) . . ? C7 C2 C1 122.1(5) . . ? C3 C2 C1 119.1(5) . . ? C4 C3 C2 119.2(5) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 123.3(5) . . ? C3 C4 N1 116.0(5) . . ? C5 C4 N1 120.6(5) . . ? C4 C5 C6 115.5(5) . . ? C4 C5 C8 125.8(5) . . ? C6 C5 C8 118.6(6) . . ? C7 C6 C5 122.1(6) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C2 C7 C6 121.0(6) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C9 C8 C13 115.9(5) . . ? C9 C8 C5 125.5(5) . . ? C13 C8 C5 118.6(6) . . ? C10 C9 C8 122.9(6) . . ? C10 C9 N2 115.9(6) . . ? C8 C9 N2 121.2(5) . . ? C9 C10 C11 119.6(6) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 118.4(5) . . ? C12 C11 C14 122.4(6) . . ? C10 C11 C14 119.2(6) . . ? C11 C12 C13 121.1(6) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C12 C13 C8 121.9(6) . . ? C12 C13 H13 119.0 . . ? C8 C13 H13 119.0 . . ? O3 C14 O4 125.8(5) . . ? O3 C14 C11 117.3(6) . . ? O4 C14 C11 116.8(5) . . ? N3 C15 C16 123.0(5) . . ? N3 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C17 120.3(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 116.5(5) . . ? C18 C17 C20 123.4(5) . . ? C16 C17 C20 120.0(5) . . ? C17 C18 C19 120.6(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? N3 C19 C18 122.7(5) . . ? N3 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C17 C20 C21 112.9(5) . . ? C17 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? C17 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C22' 76.7(8) . . ? C22 C21 C20 118.8(7) . . ? C22' C21 C20 137.7(8) . . ? C21 C22 C25 115.8(9) . . ? C21 C22 H22A 108.3 . . ? C25 C22 H22A 108.3 . . ? C21 C22 H22B 108.3 . . ? C25 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C21 C22' H22C 104.9 . . ? C21 C22' H22D 104.9 . . ? H22C C22' H22D 105.8 . . ? N4 C23 C24 130.1(9) . . ? N4 C23 H23 114.9 . . ? C24 C23 H23 114.9 . . ? C24' C23' N4 118.4(10) . . ? C24' C23' H23' 120.8 . . ? N4 C23' H23' 120.8 . . ? C25 C24 C23 109.2(8) . . ? C23' C24' H24' 124.6 . . ? C24 C25 C26 123.9(10) . . ? C24 C25 C22 112.5(9) . . ? C26 C25 C22 123.2(9) . . ? C27 C26 C25 121.0(10) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C27' C26' H26' 123.3 . . ? C26 C27 N4 123.0(9) . . ? C26 C27 H27 118.5 . . ? N4 C27 H27 118.5 . . ? N4 C27' C26' 126.5(14) . . ? N4 C27' H27' 116.8 . . ? C26' C27' H27' 116.8 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.760 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.144 #=========================END data_Compound-4 #TrackingRef 'cif.txt' _database_code_depnum_ccdc_archive 'CCDC 778426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C27 H20 N4 O8 Zn' _chemical_formula_sum 'C27 H20 N4 O8 Zn' _chemical_formula_weight 593.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 cc 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' _cell_length_a 8.2329(16) _cell_length_b 25.653(5) _cell_length_c 12.817(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.72(3) _cell_angle_gamma 90.00 _cell_volume 2650.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5535 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.984 _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 '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 12902 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.43 _reflns_number_total 5535 _reflns_number_gt 4860 _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. To improve the parameters chemical more reasonable, ultimately restrain instructions ISOR for (o6, o6', o5, o5') were applied in the refinement. ; _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^)+(0.0320P)^2^+0.6454P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(9) _refine_ls_number_reflns 5535 _refine_ls_number_parameters 379 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.79556(3) 0.627470(11) 0.20534(3) 0.03804(9) Uani 1 1 d . . . O1 O 0.9203(3) 0.69083(8) 0.25568(17) 0.0500(5) Uani 1 1 d . . . O2 O 1.0078(3) 0.68038(10) 0.10416(17) 0.0573(6) Uani 1 1 d . . . O3 O 2.1231(3) 0.86434(9) 0.58183(18) 0.0583(6) Uani 1 1 d . . . O4 O 2.0183(3) 0.94323(9) 0.5973(2) 0.0623(7) Uani 1 1 d . . . O5 O 1.5670(8) 0.8471(2) 0.1431(5) 0.0569(17) Uani 0.50 1 d PU A 1 O5' O 1.5179(8) 0.8571(2) 0.1288(5) 0.0531(16) Uani 0.50 1 d PU A 2 O6 O 1.4578(8) 0.7905(2) 0.0374(5) 0.0686(14) Uani 0.50 1 d PU A 1 O6' O 1.5389(7) 0.7726(2) 0.0796(4) 0.0688(14) Uani 0.50 1 d PU A 2 O7 O 1.4216(4) 0.96244(11) 0.4408(2) 0.0876(10) Uani 1 1 d . . . O8 O 1.3013(3) 0.91134(10) 0.3180(2) 0.0743(8) Uani 1 1 d . . . N1 N 1.4813(4) 0.80984(12) 0.1272(2) 0.0614(8) Uani 1 1 d . . . N2 N 1.4184(3) 0.92282(11) 0.3885(2) 0.0467(7) Uani 1 1 d . A . N3 N 0.9595(3) 0.56790(9) 0.21890(19) 0.0414(5) Uani 1 1 d . . . N4 N 1.6772(3) 0.38112(9) -0.1676(2) 0.0436(6) Uani 1 1 d . . . C1 C 1.0153(4) 0.70207(11) 0.1903(2) 0.0417(6) Uani 1 1 d . . . C2 C 1.1466(3) 0.74192(11) 0.2294(2) 0.0363(6) Uani 1 1 d . A . C3 C 1.2510(4) 0.75810(12) 0.1634(2) 0.0415(7) Uani 1 1 d . . . H3 H 1.2361 0.7458 0.0939 0.090 Uiso 1 1 calc . . . C4 C 1.3770(4) 0.79264(11) 0.2020(2) 0.0398(6) Uani 1 1 d . A . C5 C 1.4072(3) 0.81160(10) 0.3066(2) 0.0354(6) Uani 1 1 d . . . C6 C 1.3017(4) 0.79507(12) 0.3703(2) 0.0449(7) Uani 1 1 d . A . H6 H 1.3171 0.8073 0.4400 0.090 Uiso 1 1 calc . . . C7 C 1.1728(4) 0.76056(12) 0.3334(2) 0.0420(7) Uani 1 1 d . . . H7 H 1.1037 0.7499 0.3784 0.090 Uiso 1 1 calc . . . C8 C 2.0088(3) 0.89929(12) 0.5609(2) 0.0411(7) Uani 1 1 d . . . C9 C 1.8543(3) 0.88012(11) 0.4867(2) 0.0360(6) Uani 1 1 d . . . C10 C 1.7094(3) 0.90936(10) 0.4694(2) 0.0341(6) Uani 1 1 d . A . H10 H 1.7085 0.9422 0.5002 0.090 Uiso 1 1 calc . . . C11 C 1.5661(4) 0.88956(12) 0.4062(2) 0.0332(6) Uani 1 1 d . . . C12 C 1.5609(3) 0.84020(10) 0.3580(2) 0.0363(6) Uani 1 1 d . A . C13 C 1.7096(4) 0.81281(11) 0.3738(2) 0.0449(7) Uani 1 1 d . . . H13 H 1.7130 0.7807 0.3404 0.090 Uiso 1 1 calc . . . C14 C 1.8520(4) 0.83200(11) 0.4375(2) 0.0423(7) Uani 1 1 d . A . H14 H 1.9486 0.8122 0.4478 0.090 Uiso 1 1 calc . . . C15 C 0.9157(4) 0.52097(12) 0.1788(3) 0.0503(8) Uani 1 1 d . . . H15 H 0.8046 0.5150 0.1488 0.090 Uiso 1 1 calc . . . C16 C 1.0266(4) 0.48076(12) 0.1796(3) 0.0547(8) Uani 1 1 d . . . H16 H 0.9895 0.4488 0.1497 0.090 Uiso 1 1 calc . . . C17 C 1.1926(4) 0.48747(12) 0.2245(2) 0.0419(7) Uani 1 1 d . . . C18 C 1.2366(4) 0.53612(14) 0.2668(3) 0.0614(9) Uani 1 1 d . . . H18 H 1.3466 0.5428 0.2984 0.090 Uiso 1 1 calc . . . C19 C 1.1205(4) 0.57495(13) 0.2629(3) 0.0609(10) Uani 1 1 d . . . H19 H 1.1547 0.6073 0.2918 0.090 Uiso 1 1 calc . . . C20 C 1.3164(4) 0.44470(12) 0.2242(2) 0.0502(8) Uani 1 1 d . . . H20A H 1.2741 0.4128 0.2493 0.090 Uiso 1 1 calc . . . H20B H 1.4187 0.4536 0.2732 0.090 Uiso 1 1 calc . . . C21 C 1.3531(4) 0.43544(13) 0.1136(3) 0.0492(7) Uani 1 1 d . . . H21A H 1.4063 0.4661 0.0915 0.090 Uiso 1 1 calc . . . H21B H 1.2498 0.4299 0.0630 0.090 Uiso 1 1 calc . . . C22 C 1.4659(5) 0.38815(15) 0.1129(3) 0.0595(9) Uani 1 1 d . . . H22A H 1.5564 0.3899 0.1745 0.090 Uiso 1 1 calc . . . H22B H 1.4031 0.3567 0.1192 0.090 Uiso 1 1 calc . . . C23 C 1.5764(5) 0.34390(13) -0.1456(3) 0.0629(10) Uani 1 1 d . . . H23 H 1.5527 0.3158 -0.1920 0.090 Uiso 1 1 calc . . . C24 C 1.5055(5) 0.34528(14) -0.0569(3) 0.0680(11) Uani 1 1 d . . . H24 H 1.4351 0.3184 -0.0457 0.090 Uiso 1 1 calc . . . C25 C 1.5361(5) 0.38482(16) 0.0140(3) 0.0481(9) Uani 1 1 d . . . C26 C 1.6373(5) 0.42419(18) -0.0119(3) 0.0736(14) Uani 1 1 d . . . H26 H 1.6603 0.4531 0.0324 0.090 Uiso 1 1 calc . . . C27 C 1.7036(5) 0.42123(15) -0.1015(3) 0.0679(11) Uani 1 1 d . . . H27 H 1.7699 0.4485 -0.1164 0.090 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 0.02961(15) 0.03964(15) 0.04240(15) 0.00054(17) 0.00147(10) -0.00547(16) O1 0.0449(13) 0.0522(13) 0.0560(12) -0.0101(10) 0.0174(10) -0.0185(10) O2 0.0601(15) 0.0636(14) 0.0471(12) -0.0147(11) 0.0081(11) -0.0212(12) O3 0.0382(13) 0.0654(14) 0.0617(14) -0.0146(11) -0.0121(10) 0.0143(10) O4 0.0446(14) 0.0503(13) 0.0828(16) -0.0179(13) -0.0091(12) -0.0023(11) O5 0.0563(19) 0.0571(19) 0.0579(19) 0.0020(10) 0.0128(10) -0.0033(10) O5' 0.0529(18) 0.0522(18) 0.0546(18) 0.0039(10) 0.0119(10) -0.0025(10) O6 0.0702(16) 0.0707(16) 0.0665(16) -0.0015(10) 0.0175(10) -0.0039(10) O6' 0.0691(16) 0.0701(16) 0.0696(16) -0.0028(10) 0.0199(10) -0.0012(10) O7 0.0672(18) 0.088(2) 0.093(2) -0.0477(17) -0.0163(14) 0.0399(15) O8 0.0426(15) 0.0661(16) 0.0978(19) -0.0112(14) -0.0241(14) 0.0090(12) N1 0.072(2) 0.0640(18) 0.0565(17) -0.0239(14) 0.0329(15) -0.0324(16) N2 0.0344(14) 0.0501(16) 0.0519(15) -0.0017(13) 0.0002(12) 0.0060(12) N3 0.0344(13) 0.0424(13) 0.0454(13) 0.0007(11) 0.0034(10) -0.0016(11) N4 0.0336(13) 0.0461(14) 0.0517(14) -0.0057(11) 0.0100(11) 0.0027(11) C1 0.0373(16) 0.0410(15) 0.0451(15) -0.0021(13) 0.0045(12) -0.0047(13) C2 0.0358(15) 0.0348(14) 0.0384(13) -0.0025(11) 0.0078(11) -0.0046(11) C3 0.0454(17) 0.0436(15) 0.0352(13) -0.0064(12) 0.0076(12) -0.0108(13) C4 0.0390(16) 0.0410(15) 0.0416(14) -0.0046(12) 0.0131(12) -0.0102(12) C5 0.0349(15) 0.0357(14) 0.0348(13) -0.0054(11) 0.0053(11) -0.0044(11) C6 0.0487(18) 0.0509(17) 0.0349(13) -0.0094(13) 0.0077(12) -0.0146(14) C7 0.0404(17) 0.0453(16) 0.0424(15) -0.0064(13) 0.0138(13) -0.0091(13) C8 0.0309(15) 0.0454(17) 0.0437(15) -0.0032(13) 0.0000(12) 0.0036(13) C9 0.0318(15) 0.0379(14) 0.0370(13) 0.0030(11) 0.0040(11) -0.0005(11) C10 0.0333(15) 0.0325(13) 0.0350(13) -0.0013(11) 0.0035(11) -0.0007(11) C11 0.0318(16) 0.0341(14) 0.0334(14) 0.0008(13) 0.0057(12) 0.0011(13) C12 0.0336(14) 0.0384(14) 0.0359(13) -0.0043(12) 0.0049(11) -0.0056(12) C13 0.0454(18) 0.0343(15) 0.0540(17) -0.0080(13) 0.0075(14) -0.0009(13) C14 0.0322(15) 0.0395(15) 0.0531(16) -0.0044(13) 0.0037(12) 0.0082(12) C15 0.0370(17) 0.0463(17) 0.0633(19) -0.0094(15) -0.0002(14) -0.0009(14) C16 0.0454(19) 0.0467(18) 0.067(2) -0.0088(16) 0.0004(15) -0.0005(15) C17 0.0422(16) 0.0491(17) 0.0368(14) 0.0024(13) 0.0141(12) -0.0001(13) C18 0.0343(17) 0.057(2) 0.085(2) -0.0126(19) -0.0043(16) -0.0010(16) C19 0.0407(19) 0.0477(19) 0.086(3) -0.0161(18) -0.0063(18) -0.0017(15) C20 0.047(2) 0.0600(18) 0.0455(19) -0.0006(15) 0.0130(16) 0.0128(16) C21 0.0486(19) 0.0519(18) 0.0507(16) 0.0066(15) 0.0186(14) 0.0064(14) C22 0.065(2) 0.068(2) 0.0500(18) 0.0045(17) 0.0210(17) 0.0168(19) C23 0.081(3) 0.0438(18) 0.072(2) -0.0141(18) 0.034(2) -0.0145(19) C24 0.089(3) 0.048(2) 0.077(2) -0.0046(19) 0.041(2) -0.015(2) C25 0.036(2) 0.058(2) 0.049(2) -0.0030(17) 0.0059(15) 0.0096(17) C26 0.066(3) 0.087(3) 0.075(3) -0.048(2) 0.032(2) -0.030(2) C27 0.055(2) 0.073(2) 0.085(2) -0.035(2) 0.0340(19) -0.0314(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.911(2) 4_364 ? Zn1 O1 1.960(2) . ? Zn1 N3 2.023(2) . ? Zn1 N4 2.072(3) 2_465 ? O1 C1 1.290(4) . ? O2 C1 1.227(4) . ? O3 C8 1.288(4) . ? O3 Zn1 1.911(2) 4_665 ? O4 C8 1.216(4) . ? O5 N1 1.182(6) . ? O5' N1 1.250(7) . ? O6 N1 1.233(6) . ? O6' N1 1.276(6) . ? O7 N2 1.215(3) . ? O8 N2 1.216(3) . ? N1 C4 1.478(4) . ? N2 C11 1.465(4) . ? N3 C15 1.330(4) . ? N3 C19 1.343(4) . ? N4 C27 1.323(4) . ? N4 C23 1.333(4) . ? N4 Zn1 2.072(2) 2_664 ? C1 C2 1.498(4) . ? C2 C3 1.386(4) . ? C2 C7 1.391(4) . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.401(4) . ? C5 C6 1.374(4) . ? C5 C12 1.495(4) . ? C6 C7 1.389(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.507(4) . ? C9 C14 1.384(4) . ? C9 C10 1.389(4) . ? C10 C11 1.385(4) . ? C10 H10 0.9300 . ? C11 C12 1.406(4) . ? C12 C13 1.391(4) . ? C13 C14 1.376(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.376(4) . ? C15 H15 0.9300 . ? C16 C17 1.382(4) . ? C16 H16 0.9300 . ? C17 C18 1.379(4) . ? C17 C20 1.498(4) . ? C18 C19 1.374(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.527(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.529(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C25 1.498(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.380(5) . ? C23 H23 0.9300 . ? C24 C25 1.351(5) . ? C24 H24 0.9300 . ? C25 C26 1.392(6) . ? C26 C27 1.370(5) . ? C26 H26 0.9300 . ? C27 H27 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 O3 Zn1 O1 115.64(10) 4_364 . ? O3 Zn1 N3 121.65(10) 4_364 . ? O1 Zn1 N3 107.59(10) . . ? O3 Zn1 N4 105.88(10) 4_364 2_465 ? O1 Zn1 N4 97.36(9) . 2_465 ? N3 Zn1 N4 105.33(10) . 2_465 ? C1 O1 Zn1 108.54(19) . . ? C8 O3 Zn1 118.99(19) . 4_665 ? O5 N1 O6 117.5(4) . . ? O5 N1 O5' 22.7(4) . . ? O6 N1 O5' 113.4(4) . . ? O5 N1 O6' 115.0(5) . . ? O6 N1 O6' 41.8(3) . . ? O5' N1 O6' 128.5(4) . . ? O5 N1 C4 122.4(4) . . ? O6 N1 C4 119.0(3) . . ? O5' N1 C4 116.7(4) . . ? O6' N1 C4 114.1(3) . . ? O7 N2 O8 122.5(3) . . ? O7 N2 C11 118.5(3) . . ? O8 N2 C11 118.8(3) . . ? C15 N3 C19 116.8(3) . . ? C15 N3 Zn1 121.8(2) . . ? C19 N3 Zn1 121.3(2) . . ? C27 N4 C23 116.8(3) . . ? C27 N4 Zn1 122.9(2) . 2_664 ? C23 N4 Zn1 120.2(2) . 2_664 ? O2 C1 O1 123.8(3) . . ? O2 C1 C2 120.8(3) . . ? O1 C1 C2 115.3(3) . . ? C3 C2 C7 119.1(2) . . ? C3 C2 C1 119.7(2) . . ? C7 C2 C1 121.1(2) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 122.8(3) . . ? C3 C4 N1 117.0(3) . . ? C5 C4 N1 120.2(2) . . ? C6 C5 C4 116.8(2) . . ? C6 C5 C12 118.1(2) . . ? C4 C5 C12 124.2(2) . . ? C5 C6 C7 121.7(2) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C2 120.3(3) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? O4 C8 O3 125.3(3) . . ? O4 C8 C9 121.7(3) . . ? O3 C8 C9 113.1(2) . . ? C14 C9 C10 118.5(3) . . ? C14 C9 C8 120.7(3) . . ? C10 C9 C8 120.8(2) . . ? C11 C10 C9 119.8(3) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 122.3(3) . . ? C10 C11 N2 117.3(3) . . ? C12 C11 N2 120.4(3) . . ? C13 C12 C11 116.3(3) . . ? C13 C12 C5 117.2(2) . . ? C11 C12 C5 125.7(3) . . ? C14 C13 C12 121.6(3) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C9 121.4(3) . . ? C13 C14 H14 119.3 . . ? C9 C14 H14 119.3 . . ? N3 C15 C16 123.2(3) . . ? N3 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 115.8(3) . . ? C18 C17 C20 122.6(3) . . ? C16 C17 C20 121.6(3) . . ? C19 C18 C17 121.1(3) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? N3 C19 C18 122.5(3) . . ? N3 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C17 C20 C21 112.3(2) . . ? C17 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C17 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 111.3(3) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C25 C22 C21 112.9(3) . . ? C25 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C25 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N4 C23 C24 122.8(3) . . ? N4 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C25 C24 C23 121.4(3) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 115.0(3) . . ? C24 C25 C22 124.1(4) . . ? C26 C25 C22 120.9(3) . . ? C27 C26 C25 121.3(3) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? N4 C27 C26 122.6(3) . . ? N4 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.363 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.044 #=========================END data_Compound-5 #TrackingRef 'cif.txt' _database_code_depnum_ccdc_archive 'CCDC 778427' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C41 H26 Cd2 N6 O16' _chemical_formula_sum 'C41 H26 Cd2 N6 O16' _chemical_formula_weight 1083.48 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 28.506(6) _cell_length_b 10.930(2) _cell_length_c 13.220(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.18(3) _cell_angle_gamma 90.00 _cell_volume 3993.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3819 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 1.150 _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 11838 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3819 _reflns_number_gt 2737 _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. Standard DFIX restraints were used for the distance of the atoms, such as (h20a and c20), (h20b and c20), (h20c and c20), (h20d and c20), (h21a and c21), (h21b and c21). ; _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^)+(0.0280P)^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 3819 _refine_ls_number_parameters 316 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.952 _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 0.463237(9) -0.03978(2) 0.59712(2) 0.02904(9) Uani 1 1 d . . . O1 O 0.41642(10) 0.1206(3) 0.5144(2) 0.0511(8) Uani 1 1 d . . . O2 O 0.37809(9) -0.0505(2) 0.5284(2) 0.0422(7) Uani 1 1 d . . . O3 O 0.02979(9) 0.4265(2) 0.08862(19) 0.0333(6) Uani 1 1 d . . . O4 O 0.04761(9) 0.5335(2) 0.2326(2) 0.0436(7) Uani 1 1 d . . . O5 O 0.16747(12) 0.1078(3) 0.3947(3) 0.0812(12) Uani 1 1 d . . . O6 O 0.20024(14) -0.0658(3) 0.3832(3) 0.0903(13) Uani 1 1 d . . . O7 O 0.20727(13) 0.0886(3) 0.1417(3) 0.0753(11) Uani 1 1 d . . . O8 O 0.13210(14) 0.0476(3) 0.1219(3) 0.0880(12) Uani 1 1 d . . . N1 N 0.20101(13) 0.0439(4) 0.3847(3) 0.0515(9) Uani 1 1 d . . . N2 N 0.16733(15) 0.1137(3) 0.1506(3) 0.0514(10) Uani 1 1 d . . . N3 N 0.46964(11) -0.2432(3) 0.6060(2) 0.0299(7) Uani 1 1 d . . . C1 C 0.37862(14) 0.0571(4) 0.4971(3) 0.0380(10) Uani 1 1 d . . . C2 C 0.33191(13) 0.1118(4) 0.4359(3) 0.0346(9) Uani 1 1 d . . . C3 C 0.28888(14) 0.0527(4) 0.4299(3) 0.0383(9) Uani 1 1 d . . . H3 H 0.2886 -0.0239 0.4604 0.080 Uiso 1 1 calc . . . C4 C 0.24584(13) 0.1074(4) 0.3782(3) 0.0349(9) Uani 1 1 d . . . C5 C 0.24367(13) 0.2185(4) 0.3275(3) 0.0364(9) Uani 1 1 d . . . C6 C 0.28789(14) 0.2752(4) 0.3329(3) 0.0456(11) Uani 1 1 d . . . H6 H 0.2885 0.3490 0.2982 0.080 Uiso 1 1 calc . . . C7 C 0.33102(14) 0.2246(4) 0.3885(3) 0.0466(11) Uani 1 1 d . . . H7 H 0.3598 0.2672 0.3940 0.080 Uiso 1 1 calc . . . C8 C 0.05874(13) 0.4570(3) 0.1719(3) 0.0321(8) Uani 1 1 d . . . C9 C 0.10822(13) 0.3997(3) 0.2028(3) 0.0302(8) Uani 1 1 d . . . C10 C 0.11611(13) 0.2875(3) 0.1613(3) 0.0354(9) Uani 1 1 d . . . H10 H 0.0919 0.2506 0.1102 0.080 Uiso 1 1 calc . . . C11 C 0.16032(14) 0.2314(3) 0.1969(3) 0.0383(10) Uani 1 1 d . . . C12 C 0.19783(13) 0.2814(3) 0.2742(3) 0.0339(9) Uani 1 1 d . . . C13 C 0.19012(13) 0.3983(4) 0.3081(3) 0.0368(9) Uani 1 1 d . . . H13 H 0.2150 0.4385 0.3549 0.080 Uiso 1 1 calc . . . C14 C 0.14568(13) 0.4560(3) 0.2728(3) 0.0351(9) Uani 1 1 d . . . H14 H 0.1412 0.5339 0.2970 0.080 Uiso 1 1 calc . . . C15 C 0.43167(15) -0.3135(4) 0.6079(3) 0.0450(10) Uani 1 1 d . . . H15 H 0.4016 -0.2765 0.6007 0.080 Uiso 1 1 calc . . . C16 C 0.43501(18) -0.4380(4) 0.6200(4) 0.0578(13) Uani 1 1 d . . . H16 H 0.4075 -0.4832 0.6208 0.080 Uiso 1 1 calc . . . C17 C 0.47876(19) -0.4969(4) 0.6311(3) 0.0510(12) Uani 1 1 d . . . C18 C 0.51701(18) -0.4244(4) 0.6246(4) 0.0510(12) Uani 1 1 d . . . H18 H 0.5471 -0.4598 0.6285 0.080 Uiso 1 1 calc . . . C19 C 0.51160(15) -0.3000(4) 0.6124(3) 0.0417(10) Uani 1 1 d . . . H19 H 0.5384 -0.2534 0.6084 0.080 Uiso 1 1 calc . . . C20 C 0.4847(4) -0.6318(5) 0.6509(6) 0.0822(18) Uani 1 1 d D . . H20A H 0.480(5) -0.679(10) 0.594(6) 0.080 Uiso 0.50 1 d PD . . H20B H 0.458(3) -0.648(11) 0.674(11) 0.080 Uiso 0.50 1 d PD . . H20C H 0.508(3) -0.661(10) 0.623(10) 0.080 Uiso 0.50 1 d PD . . H20D H 0.460(3) -0.671(10) 0.607(8) 0.080 Uiso 0.50 1 d PD . . C21 C 0.4794(4) -0.6709(8) 0.7438(11) 0.065(4) Uani 0.50 1 d PD . . H21A H 0.475(3) -0.752(2) 0.741(8) 0.080 Uiso 0.50 1 d PD . . H21B H 0.4499(17) -0.654(9) 0.752(9) 0.080 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01951(14) 0.03045(15) 0.03344(15) 0.00197(14) -0.00062(11) 0.00036(13) O1 0.0251(15) 0.0514(18) 0.069(2) 0.0022(16) -0.0042(15) 0.0078(14) O2 0.0321(15) 0.0528(18) 0.0380(15) 0.0063(14) 0.0016(13) 0.0139(14) O3 0.0238(13) 0.0426(16) 0.0299(14) 0.0022(12) -0.0003(12) 0.0065(11) O4 0.0387(16) 0.0562(17) 0.0352(15) 0.0003(15) 0.0079(13) 0.0235(15) O5 0.0376(19) 0.098(3) 0.111(3) 0.033(2) 0.025(2) 0.007(2) O6 0.072(3) 0.067(3) 0.132(4) -0.004(2) 0.025(3) -0.022(2) O7 0.058(2) 0.080(2) 0.083(3) -0.028(2) 0.007(2) 0.030(2) O8 0.061(2) 0.057(2) 0.132(4) -0.035(2) -0.005(2) 0.005(2) N1 0.034(2) 0.066(3) 0.051(2) 0.014(2) 0.0046(18) 0.002(2) N2 0.047(2) 0.047(2) 0.051(2) -0.0067(19) -0.007(2) 0.019(2) N3 0.0287(18) 0.0310(16) 0.0294(16) 0.0001(14) 0.0060(15) -0.0030(14) C1 0.029(2) 0.050(3) 0.033(2) -0.004(2) 0.0047(19) 0.014(2) C2 0.025(2) 0.043(2) 0.033(2) -0.0007(19) 0.0033(18) 0.0075(19) C3 0.033(2) 0.047(2) 0.032(2) 0.005(2) 0.0026(18) 0.004(2) C4 0.022(2) 0.048(2) 0.033(2) 0.0021(19) 0.0024(18) 0.0007(19) C5 0.029(2) 0.047(2) 0.031(2) 0.0033(19) 0.0022(18) 0.0091(19) C6 0.030(2) 0.042(2) 0.060(3) 0.015(2) 0.002(2) 0.006(2) C7 0.026(2) 0.051(3) 0.059(3) 0.008(2) 0.002(2) 0.003(2) C8 0.027(2) 0.037(2) 0.032(2) 0.010(2) 0.0065(18) 0.0036(19) C9 0.0229(19) 0.042(2) 0.0247(19) 0.0045(18) 0.0045(17) 0.0087(18) C10 0.028(2) 0.039(2) 0.036(2) -0.0007(19) 0.0020(19) 0.0064(18) C11 0.036(2) 0.038(2) 0.039(2) -0.0016(19) 0.006(2) 0.0111(19) C12 0.024(2) 0.042(2) 0.034(2) 0.0067(18) 0.0032(18) 0.0079(18) C13 0.028(2) 0.046(2) 0.033(2) -0.0010(19) 0.0007(18) 0.0041(19) C14 0.030(2) 0.042(2) 0.032(2) 0.003(2) 0.0050(18) 0.007(2) C15 0.034(2) 0.046(3) 0.051(3) 0.005(2) 0.004(2) -0.006(2) C16 0.060(3) 0.045(3) 0.062(3) 0.005(2) 0.003(3) -0.023(2) C17 0.074(3) 0.032(2) 0.043(3) -0.0066(19) 0.007(3) -0.001(2) C18 0.061(3) 0.040(3) 0.054(3) -0.001(2) 0.020(3) 0.012(2) C19 0.039(2) 0.041(2) 0.048(3) 0.000(2) 0.015(2) -0.001(2) C20 0.124(6) 0.035(3) 0.078(5) -0.011(3) 0.006(5) -0.004(4) C21 0.122(12) 0.024(4) 0.055(6) 0.004(5) 0.036(11) -0.015(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 N3 2.231(3) . ? Cd1 O3 2.291(2) 8_556 ? Cd1 O1 2.310(3) . ? Cd1 O4 2.347(3) 7_556 ? Cd1 O2 2.377(3) . ? Cd1 O3 2.539(2) 4_545 ? Cd1 O4 2.624(3) 8_556 ? Cd1 C1 2.669(4) . ? O1 C1 1.255(5) . ? O2 C1 1.248(4) . ? O3 C8 1.249(4) . ? O3 Cd1 2.291(2) 8_455 ? O3 Cd1 2.539(2) 4 ? O4 C8 1.253(4) . ? O4 Cd1 2.347(3) 7_556 ? O4 Cd1 2.624(3) 8_455 ? O5 N1 1.217(4) . ? O6 N1 1.199(5) . ? O7 N2 1.205(4) . ? O8 N2 1.219(5) . ? N1 C4 1.475(5) . ? N2 C11 1.459(5) . ? N3 C19 1.332(5) . ? N3 C15 1.333(5) . ? C1 C2 1.502(5) . ? C2 C3 1.371(5) . ? C2 C7 1.381(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9300 . ? C4 C5 1.381(5) . ? C5 C6 1.390(5) . ? C5 C12 1.492(5) . ? C6 C7 1.384(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.505(5) . ? C9 C14 1.375(5) . ? C9 C10 1.385(5) . ? C10 C11 1.377(5) . ? C10 H10 0.9300 . ? C11 C12 1.397(5) . ? C12 C13 1.389(5) . ? C13 C14 1.389(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.371(6) . ? C15 H15 0.9300 . ? C16 C17 1.379(7) . ? C16 H16 0.9300 . ? C17 C18 1.367(6) . ? C17 C20 1.500(7) . ? C18 C19 1.374(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.344(14) . ? C20 C21 1.572(15) 2_656 ? C20 H20A 0.90(2) . ? C20 H20B 0.90(2) . ? C20 H20C 0.90(2) . ? C20 H20D 0.90(2) . ? C21 C21 1.15(2) 2_656 ? C21 C20 1.572(15) 2_656 ? C21 H20B 1.01(14) . ? C21 H21A 0.89(2) . ? C21 H21B 0.89(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 O3 118.88(10) . 8_556 ? N3 Cd1 O1 144.24(11) . . ? O3 Cd1 O1 87.47(10) 8_556 . ? N3 Cd1 O4 90.39(10) . 7_556 ? O3 Cd1 O4 109.66(9) 8_556 7_556 ? O1 Cd1 O4 103.62(10) . 7_556 ? N3 Cd1 O2 91.92(10) . . ? O3 Cd1 O2 142.02(9) 8_556 . ? O1 Cd1 O2 55.89(9) . . ? O4 Cd1 O2 90.35(9) 7_556 . ? N3 Cd1 O3 83.21(9) . 4_545 ? O3 Cd1 O3 76.64(9) 8_556 4_545 ? O1 Cd1 O3 79.92(9) . 4_545 ? O4 Cd1 O3 172.72(9) 7_556 4_545 ? O2 Cd1 O3 86.41(9) . 4_545 ? N3 Cd1 O4 86.59(10) . 8_556 ? O3 Cd1 O4 52.26(8) 8_556 8_556 ? O1 Cd1 O4 129.04(9) . 8_556 ? O4 Cd1 O4 70.03(10) 7_556 8_556 ? O2 Cd1 O4 160.31(8) . 8_556 ? O3 Cd1 O4 112.85(8) 4_545 8_556 ? N3 Cd1 C1 118.28(12) . . ? O3 Cd1 C1 114.83(12) 8_556 . ? O1 Cd1 C1 28.02(10) . . ? O4 Cd1 C1 98.51(10) 7_556 . ? O2 Cd1 C1 27.88(10) . . ? O3 Cd1 C1 81.60(10) 4_545 . ? O4 Cd1 C1 153.32(11) 8_556 . ? C1 O1 Cd1 92.1(2) . . ? C1 O2 Cd1 89.2(2) . . ? C8 O3 Cd1 100.9(2) . 8_455 ? C8 O3 Cd1 128.5(2) . 4 ? Cd1 O3 Cd1 103.36(9) 8_455 4 ? C8 O4 Cd1 138.4(2) . 7_556 ? C8 O4 Cd1 85.1(2) . 8_455 ? Cd1 O4 Cd1 109.87(10) 7_556 8_455 ? O6 N1 O5 124.3(4) . . ? O6 N1 C4 118.8(4) . . ? O5 N1 C4 116.8(4) . . ? O7 N2 O8 124.1(4) . . ? O7 N2 C11 118.1(4) . . ? O8 N2 C11 117.8(4) . . ? C19 N3 C15 116.8(3) . . ? C19 N3 Cd1 121.9(2) . . ? C15 N3 Cd1 121.3(3) . . ? O2 C1 O1 122.7(4) . . ? O2 C1 C2 118.2(4) . . ? O1 C1 C2 119.1(4) . . ? O2 C1 Cd1 62.9(2) . . ? O1 C1 Cd1 59.9(2) . . ? C2 C1 Cd1 177.1(3) . . ? C3 C2 C7 118.5(4) . . ? C3 C2 C1 120.4(4) . . ? C7 C2 C1 121.0(4) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 123.2(4) . . ? C5 C4 N1 120.4(3) . . ? C3 C4 N1 116.3(3) . . ? C4 C5 C6 115.8(4) . . ? C4 C5 C12 124.3(3) . . ? C6 C5 C12 119.8(3) . . ? C7 C6 C5 121.7(4) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C2 C7 C6 120.9(4) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? O3 C8 O4 121.8(3) . . ? O3 C8 C9 120.1(3) . . ? O4 C8 C9 118.1(3) . . ? C14 C9 C10 119.2(3) . . ? C14 C9 C8 121.2(3) . . ? C10 C9 C8 119.6(3) . . ? C11 C10 C9 118.9(4) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 123.3(3) . . ? C10 C11 N2 117.2(4) . . ? C12 C11 N2 119.5(3) . . ? C13 C12 C11 116.3(3) . . ? C13 C12 C5 117.5(4) . . ? C11 C12 C5 126.2(3) . . ? C12 C13 C14 120.8(4) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 121.1(4) . . ? C9 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? N3 C15 C16 122.8(4) . . ? N3 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C15 C16 C17 120.7(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 115.9(4) . . ? C18 C17 C20 121.6(5) . . ? C16 C17 C20 122.5(5) . . ? C17 C18 C19 120.8(4) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? N3 C19 C18 122.9(4) . . ? N3 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? C21 C20 C17 116.1(6) . . ? C21 C20 C21 45.5(9) . 2_656 ? C17 C20 C21 116.3(6) . 2_656 ? C21 C20 H20A 125(8) . . ? C17 C20 H20A 115(8) . . ? C21 C20 H20A 121(9) 2_656 . ? C21 C20 H20B 49(9) . . ? C17 C20 H20B 100(8) . . ? C21 C20 H20B 94(9) 2_656 . ? H20A C20 H20B 103(10) . . ? C21 C20 H20C 122(8) . . ? C17 C20 H20C 110(8) . . ? C21 C20 H20C 83(9) 2_656 . ? H20A C20 H20C 54(8) . . ? H20B C20 H20C 148(10) . . ? C21 C20 H20D 101(9) . . ? C17 C20 H20D 109(8) . . ? C21 C20 H20D 133(8) 2_656 . ? H20A C20 H20D 42(8) . . ? H20B C20 H20D 63(8) . . ? H20C C20 H20D 96(9) . . ? C21 C21 C20 77.9(12) 2_656 . ? C21 C21 C20 56.7(12) 2_656 2_656 ? C20 C21 C20 121.9(8) . 2_656 ? C21 C21 H20B 120(2) 2_656 . ? C20 C21 H20B 42.0(13) . . ? C20 C21 H20B 149(7) 2_656 . ? C21 C21 H21A 98(6) 2_656 . ? C20 C21 H21A 109(7) . . ? C20 C21 H21A 111(7) 2_656 . ? H20B C21 H21A 99(10) . . ? C21 C21 H21B 161(7) 2_656 . ? C20 C21 H21B 111(7) . . ? C20 C21 H21B 105(7) 2_656 . ? H20B C21 H21B 72(7) . . ? H21A C21 H21B 95(8) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.498 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.082 #=========================END