# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Lang, Jian-Ping' _publ_contact_author_email jplang@suda.edu.cn _publ_section_title ; Novel Zn and Cd Coordination Polymers of 1,1'-(1,6-hexanediyl) bis-1H-benzimidazole: Solvothermal synthesis, crystal structures and photoluminescence properties ; loop_ _publ_author_name 'Jing Wang' 'Zhi-Gang Ren' 'Ming Dai' 'Yang Chen' 'Jian-Ping Lang' # Attachment '- JPLangCIF (revised).CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 811023' #TrackingRef '- JPLangCIF (revised).CIF' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 Cl2 N4 Zn' _chemical_formula_sum 'C20 H22 Cl2 N4 Zn' _chemical_formula_weight 454.69 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1700(18) _cell_length_b 9.949(2) _cell_length_c 12.068(2) _cell_angle_alpha 102.98(3) _cell_angle_beta 104.75(3) _cell_angle_gamma 98.51(3) _cell_volume 1012.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4186 _cell_measurement_theta_min 3.1740 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 1.489 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5873 _exptl_absorpt_correction_T_max 0.8654 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9659 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4540 _reflns_number_gt 3384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4540 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.18167(4) 0.27740(3) 0.76578(3) 0.03558(13) Uani 1 1 d . . . Cl1 Cl 0.28031(12) 0.21329(9) 0.92989(7) 0.0543(2) Uani 1 1 d . . . Cl2 Cl -0.05158(9) 0.15188(8) 0.64540(7) 0.0437(2) Uani 1 1 d . . . N1 N 0.1737(3) 0.4829(2) 0.8295(2) 0.0352(6) Uani 1 1 d . A . N2 N 0.1445(3) 0.6683(3) 0.9573(2) 0.0465(7) Uani 1 1 d . . . N3 N 0.4000(4) 1.2195(3) 1.5017(3) 0.0686(11) Uani 1 1 d . . . N4 N 0.3167(3) 1.2774(2) 1.6576(2) 0.0354(6) Uani 1 1 d . . . C1 C 0.1725(4) 0.5385(3) 0.9394(3) 0.0421(8) Uani 1 1 d . A . H1 H 0.1897 0.4912 0.9992 0.051 Uiso 1 1 calc R . . C2 C 0.1438(3) 0.5860(3) 0.7707(3) 0.0327(7) Uani 1 1 d . . . C3 C 0.1312(3) 0.5844(3) 0.6533(3) 0.0373(7) Uani 1 1 d . A . H3 H 0.1453 0.5064 0.5996 0.045 Uiso 1 1 calc R . . C4 C 0.0972(4) 0.7022(4) 0.6188(3) 0.0490(9) Uani 1 1 d . . . H4 H 0.0878 0.7050 0.5400 0.059 Uiso 1 1 calc R A . C5 C 0.0763(4) 0.8177(4) 0.6995(4) 0.0599(11) Uani 1 1 d . A . H5 H 0.0517 0.8956 0.6728 0.072 Uiso 1 1 calc R . . C6 C 0.0904(4) 0.8210(3) 0.8151(4) 0.0544(10) Uani 1 1 d . . . H6 H 0.0772 0.8995 0.8687 0.065 Uiso 1 1 calc R A . C7 C 0.1251(4) 0.7028(3) 0.8500(3) 0.0392(8) Uani 1 1 d . A . C8 C 0.1468(16) 0.7400(13) 1.0824(11) 0.045(3) Uani 0.595(7) 1 d P A 1 H8A H 0.1124 0.6676 1.1190 0.054 Uiso 0.595(7) 1 calc PR A 1 H8B H 0.0727 0.8016 1.0780 0.054 Uiso 0.595(7) 1 calc PR A 1 C9 C 0.3057(8) 0.8282(7) 1.1628(5) 0.0438(17) Uani 0.595(7) 1 d P A 1 H9A H 0.3026 0.8519 1.2454 0.053 Uiso 0.595(7) 1 calc PR A 1 H9B H 0.3822 0.7698 1.1579 0.053 Uiso 0.595(7) 1 calc PR A 1 C10 C 0.3596(10) 0.9635(8) 1.1336(6) 0.044(2) Uani 0.595(7) 1 d P A 1 H10A H 0.2814 1.0210 1.1323 0.053 Uiso 0.595(7) 1 calc PR A 1 H10B H 0.3760 0.9420 1.0549 0.053 Uiso 0.595(7) 1 calc PR A 1 C11 C 0.509(3) 1.043(4) 1.228(2) 0.057(6) Uani 0.595(7) 1 d P A 1 H11A H 0.5857 0.9845 1.2250 0.068 Uiso 0.595(7) 1 calc PR A 1 H11B H 0.5466 1.1286 1.2068 0.068 Uiso 0.595(7) 1 calc PR A 1 C12 C 0.5071(8) 1.0878(8) 1.3550(6) 0.0442(17) Uani 0.595(7) 1 d P A 1 H12A H 0.6077 1.1476 1.4047 0.053 Uiso 0.595(7) 1 calc PR A 1 H12B H 0.4905 1.0037 1.3835 0.053 Uiso 0.595(7) 1 calc PR A 1 C13 C 0.3801(7) 1.1693(6) 1.3688(5) 0.0357(14) Uani 0.595(7) 1 d P A 1 H13A H 0.3905 1.2502 1.3355 0.043 Uiso 0.595(7) 1 calc PR A 1 H13B H 0.2778 1.1077 1.3268 0.043 Uiso 0.595(7) 1 calc PR A 1 C8A C 0.108(2) 0.7713(18) 1.0514(16) 0.043(4) Uani 0.405(7) 1 d P A 2 H8A1 H 0.0053 0.7875 1.0169 0.052 Uiso 0.405(7) 1 calc PR A 2 H8A2 H 0.1009 0.7269 1.1152 0.052 Uiso 0.405(7) 1 calc PR A 2 C9A C 0.2164(9) 0.9110(7) 1.1064(7) 0.037(2) Uani 0.405(7) 1 d P A 2 H9A1 H 0.1799 0.9661 1.1678 0.044 Uiso 0.405(7) 1 calc PR A 2 H9A2 H 0.2142 0.9615 1.0452 0.044 Uiso 0.405(7) 1 calc PR A 2 C10A C 0.3790(14) 0.9041(13) 1.1611(10) 0.045(3) Uani 0.405(7) 1 d P A 2 H10C H 0.4156 0.8465 1.1011 0.054 Uiso 0.405(7) 1 calc PR A 2 H10D H 0.3834 0.8585 1.2256 0.054 Uiso 0.405(7) 1 calc PR A 2 C11A C 0.490(4) 1.059(5) 1.213(3) 0.042(6) Uani 0.405(7) 1 d P A 2 H11C H 0.5978 1.0505 1.2417 0.051 Uiso 0.405(7) 1 calc PR A 2 H11D H 0.4823 1.1066 1.1499 0.051 Uiso 0.405(7) 1 calc PR A 2 C12A C 0.4467(15) 1.1488(12) 1.3168(10) 0.061(3) Uani 0.405(7) 1 d P A 2 H12C H 0.5167 1.2421 1.3449 0.074 Uiso 0.405(7) 1 calc PR A 2 H12D H 0.3421 1.1625 1.2851 0.074 Uiso 0.405(7) 1 calc PR A 2 C13A C 0.4506(12) 1.0949(10) 1.4167(9) 0.057(3) Uani 0.405(7) 1 d P A 2 H13C H 0.5544 1.0838 1.4548 0.068 Uiso 0.405(7) 1 calc PR A 2 H13D H 0.3770 1.0043 1.3948 0.068 Uiso 0.405(7) 1 calc PR A 2 C14 C 0.2895(4) 1.1905(3) 1.5526(3) 0.0443(8) Uani 1 1 d . A . H14 H 0.2022 1.1158 1.5165 0.053 Uiso 1 1 calc R . . C15 C 0.5102(4) 1.3335(4) 1.5817(3) 0.0497(9) Uani 1 1 d . A . C16 C 0.6462(5) 1.4103(5) 1.5759(4) 0.0804(16) Uani 1 1 d . . . H16 H 0.6797 1.3880 1.5079 0.097 Uiso 1 1 calc R A . C17 C 0.7293(4) 1.5199(4) 1.6733(3) 0.0594(11) Uani 1 1 d . A . H17 H 0.8241 1.5713 1.6735 0.071 Uiso 1 1 calc R . . C18 C 0.6769(4) 1.5565(3) 1.7714(3) 0.0462(8) Uani 1 1 d . . . H18 H 0.7362 1.6327 1.8367 0.055 Uiso 1 1 calc R A . C19 C 0.5404(4) 1.4837(3) 1.7751(3) 0.0432(8) Uani 1 1 d . A . H19 H 0.5043 1.5100 1.8414 0.052 Uiso 1 1 calc R . . C20 C 0.4570(3) 1.3707(3) 1.6792(3) 0.0340(7) Uani 1 1 d . A . 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 0.0440(2) 0.0321(2) 0.0346(2) 0.00896(15) 0.01922(17) 0.00775(15) Cl1 0.0786(7) 0.0553(5) 0.0400(5) 0.0185(4) 0.0225(5) 0.0313(5) Cl2 0.0448(5) 0.0389(4) 0.0448(4) 0.0089(3) 0.0149(4) 0.0024(3) N1 0.0423(16) 0.0314(12) 0.0315(13) 0.0065(11) 0.0138(12) 0.0055(11) N2 0.0469(17) 0.0394(15) 0.0438(16) -0.0100(13) 0.0248(14) -0.0063(13) N3 0.063(2) 0.066(2) 0.0530(18) -0.0287(16) 0.0372(17) -0.0253(17) N4 0.0409(15) 0.0322(12) 0.0311(13) 0.0031(11) 0.0145(12) 0.0034(11) C1 0.050(2) 0.0393(17) 0.0308(16) 0.0017(14) 0.0168(15) -0.0042(15) C2 0.0328(17) 0.0285(14) 0.0353(16) 0.0059(12) 0.0133(14) 0.0008(12) C3 0.0357(18) 0.0366(16) 0.0399(17) 0.0111(14) 0.0134(15) 0.0041(13) C4 0.043(2) 0.048(2) 0.057(2) 0.0263(18) 0.0105(17) 0.0040(16) C5 0.042(2) 0.0388(19) 0.101(3) 0.031(2) 0.015(2) 0.0086(16) C6 0.045(2) 0.0307(17) 0.084(3) 0.0051(18) 0.024(2) 0.0059(15) C7 0.0329(18) 0.0293(15) 0.0476(19) -0.0027(14) 0.0158(15) -0.0028(13) C8 0.060(8) 0.035(5) 0.037(6) -0.006(3) 0.029(5) -0.004(4) C9 0.062(5) 0.040(3) 0.028(3) 0.002(3) 0.018(3) 0.011(3) C10 0.067(6) 0.038(4) 0.032(4) 0.007(3) 0.025(4) 0.011(4) C11 0.052(8) 0.057(10) 0.050(10) -0.012(7) 0.021(6) 0.006(6) C12 0.035(4) 0.052(4) 0.037(4) -0.007(3) 0.012(3) 0.011(3) C13 0.047(4) 0.038(3) 0.024(3) 0.002(2) 0.014(3) 0.014(3) C8A 0.052(9) 0.040(8) 0.038(9) -0.001(5) 0.028(7) 0.004(6) C9A 0.038(5) 0.030(4) 0.037(4) -0.003(3) 0.015(4) 0.002(3) C10A 0.053(7) 0.043(7) 0.038(6) -0.007(5) 0.025(5) 0.014(6) C11A 0.048(13) 0.048(9) 0.031(7) 0.002(7) 0.026(9) 0.000(9) C12A 0.056(8) 0.051(6) 0.056(7) -0.011(5) 0.022(6) -0.020(6) C13A 0.061(7) 0.044(5) 0.071(7) 0.007(5) 0.038(6) 0.010(5) C14 0.0371(19) 0.0471(18) 0.0387(18) -0.0041(15) 0.0165(15) -0.0057(15) C15 0.044(2) 0.0475(19) 0.048(2) -0.0112(16) 0.0255(17) -0.0046(16) C16 0.066(3) 0.077(3) 0.079(3) -0.027(2) 0.051(2) -0.021(2) C17 0.040(2) 0.053(2) 0.072(3) -0.0082(19) 0.026(2) -0.0089(17) C18 0.045(2) 0.0434(18) 0.0372(18) 0.0002(15) 0.0051(16) -0.0013(15) C19 0.052(2) 0.0437(17) 0.0291(16) 0.0001(14) 0.0159(15) 0.0038(16) C20 0.0336(17) 0.0363(15) 0.0330(16) 0.0091(13) 0.0117(14) 0.0078(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N4 2.015(2) 1_544 ? Zn1 N1 2.035(2) . ? Zn1 Cl1 2.2301(11) . ? Zn1 Cl2 2.2488(14) . ? N1 C1 1.321(4) . ? N1 C2 1.394(4) . ? N2 C1 1.335(4) . ? N2 C7 1.388(4) . ? N2 C8A 1.492(19) . ? N2 C8 1.510(13) . ? N3 C14 1.340(4) . ? N3 C15 1.383(4) . ? N3 C13 1.523(6) . ? N3 C13A 1.627(10) . ? N4 C14 1.303(4) . ? N4 C20 1.397(4) . ? N4 Zn1 2.015(2) 1_566 ? C1 H1 0.9400 . ? C2 C3 1.388(4) . ? C2 C7 1.393(4) . ? C3 C4 1.381(4) . ? C3 H3 0.9400 . ? C4 C5 1.400(5) . ? C4 H4 0.9400 . ? C5 C6 1.360(5) . ? C5 H5 0.9400 . ? C6 C7 1.388(5) . ? C6 H6 0.9400 . ? C8 C9 1.534(15) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.513(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.51(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.50(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.536(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C8A C9A 1.48(2) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C9A C10A 1.488(15) . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C10A C11A 1.61(5) . ? C10A H10C 0.9800 . ? C10A H10D 0.9800 . ? C11A C12A 1.54(4) . ? C11A H11C 0.9800 . ? C11A H11D 0.9800 . ? C12A C13A 1.420(17) . ? C12A H12C 0.9800 . ? C12A H12D 0.9800 . ? C13A H13C 0.9800 . ? C13A H13D 0.9800 . ? C14 H14 0.9400 . ? C15 C20 1.382(4) . ? C15 C16 1.389(5) . ? C16 C17 1.368(5) . ? C16 H16 0.9400 . ? C17 C18 1.384(4) . ? C17 H17 0.9400 . ? C18 C19 1.367(4) . ? C18 H18 0.9400 . ? C19 C20 1.378(4) . ? C19 H19 0.9400 . ? 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 Zn1 N1 106.07(10) 1_544 . ? N4 Zn1 Cl1 114.45(8) 1_544 . ? N1 Zn1 Cl1 103.60(8) . . ? N4 Zn1 Cl2 104.59(8) 1_544 . ? N1 Zn1 Cl2 110.54(8) . . ? Cl1 Zn1 Cl2 117.17(4) . . ? C1 N1 C2 104.9(3) . . ? C1 N1 Zn1 123.5(2) . . ? C2 N1 Zn1 130.84(19) . . ? C1 N2 C7 106.9(2) . . ? C1 N2 C8A 137.7(6) . . ? C7 N2 C8A 114.6(6) . . ? C1 N2 C8 116.2(5) . . ? C7 N2 C8 136.8(5) . . ? C8A N2 C8 23.7(6) . . ? C14 N3 C15 107.2(2) . . ? C14 N3 C13 124.6(3) . . ? C15 N3 C13 125.4(3) . . ? C14 N3 C13A 121.5(4) . . ? C15 N3 C13A 120.4(4) . . ? C13 N3 C13A 44.7(4) . . ? C14 N4 C20 106.2(2) . . ? C14 N4 Zn1 126.7(2) . 1_566 ? C20 N4 Zn1 127.13(19) . 1_566 ? N1 C1 N2 113.5(3) . . ? N1 C1 H1 123.2 . . ? N2 C1 H1 123.2 . . ? C3 C2 C7 121.1(3) . . ? C3 C2 N1 129.9(3) . . ? C7 C2 N1 109.0(3) . . ? C4 C3 C2 117.1(3) . . ? C4 C3 H3 121.5 . . ? C2 C3 H3 121.5 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 122.4(3) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C7 116.7(3) . . ? C5 C6 H6 121.6 . . ? C7 C6 H6 121.6 . . ? N2 C7 C6 132.6(3) . . ? N2 C7 C2 105.6(3) . . ? C6 C7 C2 121.8(3) . . ? N2 C8 C9 114.1(9) . . ? N2 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N2 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 115.3(6) . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? C8 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 C10 C11 108.1(13) . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C12 C11 C10 118.0(18) . . ? C12 C11 H11A 107.8 . . ? C10 C11 H11A 107.8 . . ? C12 C11 H11B 107.8 . . ? C10 C11 H11B 107.8 . . ? H11A C11 H11B 107.1 . . ? C11 C12 C13 112.3(13) . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N3 C13 C12 106.9(5) . . ? N3 C13 H13A 110.3 . . ? C12 C13 H13A 110.3 . . ? N3 C13 H13B 110.3 . . ? C12 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? C9A C8A N2 117.5(14) . . ? C9A C8A H8A1 107.9 . . ? N2 C8A H8A1 107.9 . . ? C9A C8A H8A2 107.9 . . ? N2 C8A H8A2 107.9 . . ? H8A1 C8A H8A2 107.2 . . ? C8A C9A C10A 114.5(10) . . ? C8A C9A H9A1 108.6 . . ? C10A C9A H9A1 108.6 . . ? C8A C9A H9A2 108.6 . . ? C10A C9A H9A2 108.6 . . ? H9A1 C9A H9A2 107.6 . . ? C9A C10A C11A 111.4(18) . . ? C9A C10A H10C 109.3 . . ? C11A C10A H10C 109.3 . . ? C9A C10A H10D 109.3 . . ? C11A C10A H10D 109.3 . . ? H10C C10A H10D 108.0 . . ? C12A C11A C10A 111(2) . . ? C12A C11A H11C 109.4 . . ? C10A C11A H11C 109.4 . . ? C12A C11A H11D 109.4 . . ? C10A C11A H11D 109.4 . . ? H11C C11A H11D 108.0 . . ? C13A C12A C11A 117.1(19) . . ? C13A C12A H12C 108.0 . . ? C11A C12A H12C 108.0 . . ? C13A C12A H12D 108.0 . . ? C11A C12A H12D 108.0 . . ? H12C C12A H12D 107.3 . . ? C12A C13A N3 100.8(9) . . ? C12A C13A H13C 111.6 . . ? N3 C13A H13C 111.6 . . ? C12A C13A H13D 111.6 . . ? N3 C13A H13D 111.6 . . ? H13C C13A H13D 109.4 . . ? N4 C14 N3 112.5(3) . . ? N4 C14 H14 123.8 . . ? N3 C14 H14 123.8 . . ? C20 C15 N3 105.9(3) . . ? C20 C15 C16 121.4(3) . . ? N3 C15 C16 132.6(3) . . ? C17 C16 C15 117.2(3) . . ? C17 C16 H16 121.4 . . ? C15 C16 H16 121.4 . . ? C16 C17 C18 121.4(3) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 118.3(3) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C19 C20 C15 120.4(3) . . ? C19 C20 N4 131.4(3) . . ? C15 C20 N4 108.2(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.464 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.075 #===END #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 811024' #TrackingRef '- JPLangCIF (revised).CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 Br2 N4 Zn' _chemical_formula_sum 'C20 H22 Br2 N4 Zn' _chemical_formula_weight 543.61 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2071(18) _cell_length_b 10.196(2) _cell_length_c 12.285(3) _cell_angle_alpha 102.64(3) _cell_angle_beta 105.75(3) _cell_angle_gamma 98.64(3) _cell_volume 1055.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4420 _cell_measurement_theta_min 3.1100 _cell_measurement_theta_max 27.4391 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 4.960 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2416 _exptl_absorpt_correction_T_max 0.6369 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8151 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3657 _reflns_number_gt 2015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1125P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3657 _refine_ls_number_parameters 299 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.1564 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.2452 _refine_ls_wR_factor_gt 0.2023 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.80820(15) 0.71560(15) 0.73267(12) 0.0688(5) Uani 1 1 d . . . Br1 Br 1.05626(13) 0.84844(14) 0.85865(11) 0.0773(5) Uani 1 1 d . . . Br2 Br 0.70124(19) 0.78592(17) 0.56199(12) 0.0928(5) Uani 1 1 d . . . N1 N 0.8182(11) 0.5167(11) 0.6668(9) 0.074(3) Uani 1 1 d . A . N2 N 0.8455(11) 0.3392(12) 0.5426(9) 0.078(3) Uani 1 1 d . . . N3 N 0.6024(13) -0.2284(13) -0.0020(11) 0.099(4) Uani 1 1 d . . . N4 N 0.6786(10) -0.2847(10) -0.1587(8) 0.065(2) Uani 1 1 d . . . C1 C 0.8169(13) 0.4633(15) 0.5585(11) 0.075(3) Uani 1 1 d . A . H1 H 0.7975 0.5089 0.4992 0.090 Uiso 1 1 calc R . . C2 C 0.8664(12) 0.3056(13) 0.6485(13) 0.074(3) Uani 1 1 d U A . C3 C 0.9035(15) 0.1895(15) 0.6811(15) 0.095(4) Uani 1 1 d U . . H3 H 0.9205 0.1153 0.6290 0.114 Uiso 1 1 calc R A . C4 C 0.9138(15) 0.1913(16) 0.7971(16) 0.095(4) Uani 1 1 d U A . H4 H 0.9344 0.1135 0.8225 0.114 Uiso 1 1 calc R . . C5 C 0.8956(14) 0.2995(16) 0.8750(14) 0.089(3) Uani 1 1 d U . . H5 H 0.9054 0.2962 0.9525 0.106 Uiso 1 1 calc R A . C6 C 0.8622(14) 0.4161(15) 0.8399(12) 0.081(3) Uani 1 1 d U A . H6 H 0.8498 0.4919 0.8931 0.098 Uiso 1 1 calc R . . C7 C 0.8482(12) 0.4172(13) 0.7274(11) 0.067(3) Uani 1 1 d U . . C8 C 0.858(3) 0.270(3) 0.424(2) 0.103(8) Uani 0.74(2) 1 d PU A 1 H8A H 0.9337 0.2126 0.4339 0.123 Uiso 0.74(2) 1 calc PR A 1 H8B H 0.8944 0.3413 0.3886 0.123 Uiso 0.74(2) 1 calc PR A 1 C9 C 0.692(2) 0.177(2) 0.3361(18) 0.085(6) Uani 0.74(2) 1 d PU A 1 H9A H 0.6128 0.2295 0.3424 0.102 Uiso 0.74(2) 1 calc PR A 1 H9B H 0.6955 0.1605 0.2553 0.102 Uiso 0.74(2) 1 calc PR A 1 C10 C 0.6438(19) 0.043(2) 0.3563(15) 0.071(5) Uani 0.74(2) 1 d PU A 1 H10A H 0.6296 0.0576 0.4339 0.085 Uiso 0.74(2) 1 calc PR A 1 H10B H 0.7245 -0.0091 0.3548 0.085 Uiso 0.74(2) 1 calc PR A 1 C11 C 0.493(3) -0.038(3) 0.262(3) 0.082(7) Uani 0.74(2) 1 d PU A 1 H11A H 0.4158 0.0183 0.2636 0.099 Uiso 0.74(2) 1 calc PR A 1 H11B H 0.4578 -0.1207 0.2841 0.099 Uiso 0.74(2) 1 calc PR A 1 C12 C 0.497(2) -0.083(2) 0.1327(18) 0.080(5) Uani 0.74(2) 1 d PU A 1 H12A H 0.3964 -0.1394 0.0809 0.096 Uiso 0.74(2) 1 calc PR A 1 H12B H 0.5206 -0.0014 0.1052 0.096 Uiso 0.74(2) 1 calc PR A 1 C13 C 0.6242(19) -0.1671(17) 0.1295(16) 0.064(4) Uani 0.74(2) 1 d PU A 1 H13A H 0.7276 -0.1073 0.1696 0.077 Uiso 0.74(2) 1 calc PR A 1 H13B H 0.6113 -0.2407 0.1681 0.077 Uiso 0.74(2) 1 calc PR A 1 C8A C 0.846(8) 0.219(8) 0.449(5) 0.083(15) Uani 0.26(2) 1 d PU A 2 H8A1 H 0.8309 0.2604 0.3826 0.100 Uiso 0.26(2) 1 calc PR A 2 H8A2 H 0.9572 0.2204 0.4728 0.100 Uiso 0.26(2) 1 calc PR A 2 C9A C 0.789(5) 0.082(6) 0.387(4) 0.080(13) Uani 0.26(2) 1 d PU A 2 H9A1 H 0.7889 0.0199 0.4379 0.097 Uiso 0.26(2) 1 calc PR A 2 H9A2 H 0.8379 0.0505 0.3278 0.097 Uiso 0.26(2) 1 calc PR A 2 C10A C 0.616(7) 0.114(7) 0.332(6) 0.087(14) Uani 0.26(2) 1 d PU A 2 H10C H 0.6118 0.1599 0.2692 0.105 Uiso 0.26(2) 1 calc PR A 2 H10D H 0.5785 0.1651 0.3919 0.105 Uiso 0.26(2) 1 calc PR A 2 C11A C 0.520(9) -0.069(9) 0.277(8) 0.066(13) Uani 0.26(2) 1 d PU A 2 H11C H 0.5545 -0.1146 0.3381 0.079 Uiso 0.26(2) 1 calc PR A 2 H11D H 0.4078 -0.0773 0.2596 0.079 Uiso 0.26(2) 1 calc PR A 2 C12A C 0.548(6) -0.137(6) 0.175(5) 0.079(12) Uani 0.26(2) 1 d PU A 2 H12C H 0.6505 -0.1547 0.2073 0.094 Uiso 0.26(2) 1 calc PR A 2 H12D H 0.4764 -0.2265 0.1519 0.094 Uiso 0.26(2) 1 calc PR A 2 C13A C 0.553(6) -0.121(7) 0.068(5) 0.082(14) Uani 0.26(2) 1 d PU A 2 H13C H 0.6231 -0.0322 0.0816 0.099 Uiso 0.26(2) 1 calc PR A 2 H13D H 0.4494 -0.1155 0.0231 0.099 Uiso 0.26(2) 1 calc PR A 2 C14 C 0.7113(14) -0.2008(15) -0.0498(12) 0.085(4) Uani 1 1 d . A . H14 H 0.8015 -0.1307 -0.0122 0.102 Uiso 1 1 calc R . . C15 C 0.4883(14) -0.3399(13) -0.0796(11) 0.075(3) Uani 1 1 d . A . C16 C 0.3543(15) -0.4125(15) -0.0729(14) 0.097(5) Uani 1 1 d . . . H16 H 0.3231 -0.3898 -0.0056 0.116 Uiso 1 1 calc R A . C17 C 0.2683(14) -0.5189(15) -0.1684(12) 0.086(4) Uani 1 1 d . A . H17 H 0.1737 -0.5681 -0.1677 0.103 Uiso 1 1 calc R . . C18 C 0.3158(13) -0.5570(14) -0.2664(10) 0.078(4) Uani 1 1 d . . . H18 H 0.2540 -0.6319 -0.3300 0.094 Uiso 1 1 calc R A . C19 C 0.4533(13) -0.4859(14) -0.2718(11) 0.075(3) Uani 1 1 d . A . H19 H 0.4877 -0.5124 -0.3369 0.089 Uiso 1 1 calc R . . C20 C 0.5373(13) -0.3747(13) -0.1774(10) 0.066(3) Uani 1 1 d . A . 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 0.0740(9) 0.0608(10) 0.0824(9) 0.0245(7) 0.0371(7) 0.0168(7) Br1 0.0740(8) 0.0711(10) 0.0939(9) 0.0250(7) 0.0381(7) 0.0123(6) Br2 0.1222(12) 0.0846(11) 0.0860(9) 0.0333(8) 0.0389(8) 0.0398(9) N1 0.072(6) 0.071(8) 0.082(7) 0.032(6) 0.025(5) 0.011(5) N2 0.065(6) 0.078(9) 0.083(7) 0.005(6) 0.031(5) 0.000(5) N3 0.094(8) 0.086(9) 0.130(10) 0.012(7) 0.080(8) -0.001(7) N4 0.060(5) 0.067(7) 0.065(5) 0.019(5) 0.021(4) 0.004(5) C1 0.080(8) 0.066(10) 0.083(9) 0.025(7) 0.033(7) 0.008(7) C2 0.056(6) 0.058(7) 0.115(8) 0.020(6) 0.037(6) 0.014(5) C3 0.079(8) 0.067(8) 0.149(9) 0.031(8) 0.047(8) 0.020(7) C4 0.079(8) 0.065(8) 0.170(11) 0.058(8) 0.064(8) 0.019(7) C5 0.077(7) 0.095(9) 0.124(9) 0.063(7) 0.049(7) 0.026(7) C6 0.088(8) 0.074(8) 0.105(7) 0.038(6) 0.055(7) 0.020(6) C7 0.056(6) 0.067(7) 0.090(7) 0.029(6) 0.034(6) 0.018(5) C8 0.103(11) 0.082(15) 0.126(16) 0.012(11) 0.075(10) -0.018(10) C9 0.089(10) 0.074(11) 0.111(12) 0.022(9) 0.065(9) 0.013(8) C10 0.068(10) 0.073(11) 0.078(8) 0.034(8) 0.027(7) 0.006(7) C11 0.082(12) 0.076(15) 0.078(11) 0.002(11) 0.027(9) 0.009(9) C12 0.092(12) 0.062(11) 0.077(8) 0.000(8) 0.023(9) 0.028(8) C13 0.064(9) 0.060(10) 0.079(10) 0.030(8) 0.030(8) 0.019(7) C8A 0.10(2) 0.09(3) 0.06(2) 0.01(2) 0.041(19) -0.01(2) C9A 0.070(18) 0.08(2) 0.08(2) 0.020(17) 0.019(16) 0.000(16) C10A 0.09(2) 0.067(18) 0.10(3) 0.042(17) 0.01(2) 0.010(18) C11A 0.063(15) 0.066(15) 0.069(14) 0.019(9) 0.023(10) 0.012(9) C12A 0.06(2) 0.09(2) 0.096(19) 0.026(15) 0.060(17) -0.001(18) C13A 0.08(2) 0.09(3) 0.08(2) 0.02(2) 0.04(2) 0.01(2) C14 0.070(8) 0.083(11) 0.100(10) 0.021(8) 0.029(7) 0.012(7) C15 0.070(7) 0.068(9) 0.089(8) 0.002(7) 0.045(6) 0.013(7) C16 0.081(9) 0.074(10) 0.130(12) 0.006(9) 0.055(9) -0.003(7) C17 0.061(7) 0.084(11) 0.113(10) 0.034(9) 0.029(7) 0.006(7) C18 0.067(7) 0.086(10) 0.067(7) -0.001(6) 0.025(6) 0.001(6) C19 0.064(7) 0.088(10) 0.074(7) 0.019(7) 0.030(6) 0.014(7) C20 0.069(7) 0.062(8) 0.071(7) 0.023(6) 0.022(6) 0.018(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 Zn1 N4 2.018(8) 1_566 ? Zn1 N1 2.038(11) . ? Zn1 Br2 2.373(2) . ? Zn1 Br1 2.383(2) . ? N1 C1 1.318(15) . ? N1 C7 1.401(15) . ? N2 C1 1.315(16) . ? N2 C2 1.389(17) . ? N2 C8A 1.49(7) . ? N2 C8 1.52(3) . ? N3 C14 1.318(15) . ? N3 C15 1.389(16) . ? N3 C13A 1.45(6) . ? N3 C13 1.54(2) . ? N4 C14 1.347(15) . ? N4 C20 1.404(14) . ? N4 Zn1 2.018(8) 1_544 ? C1 H1 0.9400 . ? C2 C7 1.388(17) . ? C2 C3 1.390(18) . ? C3 C4 1.40(2) . ? C3 H3 0.9400 . ? C4 C5 1.358(19) . ? C4 H4 0.9400 . ? C5 C6 1.398(18) . ? C5 H5 0.9400 . ? C6 C7 1.356(16) . ? C6 H6 0.9400 . ? C8 C9 1.62(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.46(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.52(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.57(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.55(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C8A C9A 1.38(8) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C9A C10A 1.66(9) . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C10A C11A 1.83(11) . ? C10A H10C 0.9800 . ? C10A H10D 0.9800 . ? C11A C12A 1.40(9) . ? C11A H11C 0.9800 . ? C11A H11D 0.9800 . ? C12A C13A 1.36(8) . ? C12A H12C 0.9800 . ? C12A H12D 0.9800 . ? C13A H13C 0.9800 . ? C13A H13D 0.9800 . ? C14 H14 0.9400 . ? C15 C16 1.373(16) . ? C15 C20 1.389(15) . ? C16 C17 1.364(18) . ? C16 H16 0.9400 . ? C17 C18 1.388(16) . ? C17 H17 0.9400 . ? C18 C19 1.387(15) . ? C18 H18 0.9400 . ? C19 C20 1.379(16) . ? C19 H19 0.9400 . ? 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 Zn1 N1 107.7(4) 1_566 . ? N4 Zn1 Br2 115.1(3) 1_566 . ? N1 Zn1 Br2 103.4(3) . . ? N4 Zn1 Br1 103.7(3) 1_566 . ? N1 Zn1 Br1 110.8(3) . . ? Br2 Zn1 Br1 115.97(8) . . ? C1 N1 C7 106.5(11) . . ? C1 N1 Zn1 124.7(9) . . ? C7 N1 Zn1 128.3(8) . . ? C1 N2 C2 107.3(10) . . ? C1 N2 C8A 142(3) . . ? C2 N2 C8A 111(3) . . ? C1 N2 C8 117.7(15) . . ? C2 N2 C8 134.9(16) . . ? C8A N2 C8 26(2) . . ? C14 N3 C15 108.9(11) . . ? C14 N3 C13A 122(2) . . ? C15 N3 C13A 117(2) . . ? C14 N3 C13 122.8(12) . . ? C15 N3 C13 126.8(10) . . ? C13A N3 C13 43(2) . . ? C14 N4 C20 104.5(9) . . ? C14 N4 Zn1 127.4(8) . 1_544 ? C20 N4 Zn1 128.0(8) . 1_544 ? N2 C1 N1 112.7(12) . . ? N2 C1 H1 123.6 . . ? N1 C1 H1 123.6 . . ? C7 C2 N2 106.7(11) . . ? C7 C2 C3 122.1(14) . . ? N2 C2 C3 131.1(13) . . ? C2 C3 C4 115.0(14) . . ? C2 C3 H3 122.5 . . ? C4 C3 H3 122.5 . . ? C5 C4 C3 123.4(14) . . ? C5 C4 H4 118.3 . . ? C3 C4 H4 118.3 . . ? C4 C5 C6 119.9(14) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 118.5(13) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C2 121.0(13) . . ? C6 C7 N1 132.2(12) . . ? C2 C7 N1 106.8(11) . . ? N2 C8 C9 111.0(16) . . ? N2 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N2 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 116.2(19) . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9B 108.2 . . ? C8 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 110(2) . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C10 C11 C12 117(2) . . ? C10 C11 H11A 108.0 . . ? C12 C11 H11A 108.0 . . ? C10 C11 H11B 108.0 . . ? C12 C11 H11B 108.0 . . ? H11A C11 H11B 107.3 . . ? C13 C12 C11 108.9(18) . . ? C13 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? C13 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N3 C13 C12 105.7(15) . . ? N3 C13 H13A 110.6 . . ? C12 C13 H13A 110.6 . . ? N3 C13 H13B 110.6 . . ? C12 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? C9A C8A N2 149(5) . . ? C9A C8A H8A1 99.4 . . ? N2 C8A H8A1 99.4 . . ? C9A C8A H8A2 99.4 . . ? N2 C8A H8A2 99.4 . . ? H8A1 C8A H8A2 104.0 . . ? C8A C9A C10A 90(5) . . ? C8A C9A H9A1 113.6 . . ? C10A C9A H9A1 113.6 . . ? C8A C9A H9A2 113.6 . . ? C10A C9A H9A2 113.6 . . ? H9A1 C9A H9A2 110.9 . . ? C9A C10A C11A 93(5) . . ? C9A C10A H10C 113.0 . . ? C11A C10A H10C 113.0 . . ? C9A C10A H10D 113.0 . . ? C11A C10A H10D 113.0 . . ? H10C C10A H10D 110.4 . . ? C12A C11A C10A 113(6) . . ? C12A C11A H11C 108.9 . . ? C10A C11A H11C 108.9 . . ? C12A C11A H11D 108.9 . . ? C10A C11A H11D 108.9 . . ? H11C C11A H11D 107.7 . . ? C13A C12A C11A 141(8) . . ? C13A C12A H12C 101.8 . . ? C11A C12A H12C 101.8 . . ? C13A C12A H12D 101.8 . . ? C11A C12A H12D 101.8 . . ? H12C C12A H12D 104.7 . . ? C12A C13A N3 115(6) . . ? C12A C13A H13C 108.4 . . ? N3 C13A H13C 108.4 . . ? C12A C13A H13D 108.4 . . ? N3 C13A H13D 108.4 . . ? H13C C13A H13D 107.5 . . ? N3 C14 N4 112.3(12) . . ? N3 C14 H14 123.8 . . ? N4 C14 H14 123.8 . . ? C16 C15 N3 133.0(12) . . ? C16 C15 C20 122.0(13) . . ? N3 C15 C20 105.0(10) . . ? C17 C16 C15 116.9(13) . . ? C17 C16 H16 121.5 . . ? C15 C16 H16 121.5 . . ? C16 C17 C18 122.2(12) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C19 C18 C17 120.8(12) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 117.2(11) . . ? C20 C19 H19 121.4 . . ? C18 C19 H19 121.4 . . ? C19 C20 C15 120.9(11) . . ? C19 C20 N4 129.7(11) . . ? C15 C20 N4 109.4(11) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.058 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.117 #===END #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 811025' #TrackingRef '- JPLangCIF (revised).CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H23 Cd I2 N4 O0.50' _chemical_formula_sum 'C20 H23 Cd I2 N4 O0.50' _chemical_formula_weight 693.62 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5750(17) _cell_length_b 11.228(2) _cell_length_c 14.062(3) _cell_angle_alpha 92.39(3) _cell_angle_beta 106.67(3) _cell_angle_gamma 107.85(3) _cell_volume 1222.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5291 _cell_measurement_theta_min 3.0554 _cell_measurement_theta_max 27.5010 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 658 _exptl_absorpt_coefficient_mu 3.434 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5467 _exptl_absorpt_correction_T_max 0.7252 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9818 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4249 _reflns_number_gt 2974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC,2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4249 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1696 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.48221(10) 0.67665(7) 0.27406(6) 0.0341(3) Uani 1 1 d . . . I1 I 0.80021(11) 0.80443(10) 0.26673(7) 0.0643(3) Uani 1 1 d . . . I2 I 0.41423(10) 0.43470(7) 0.32067(6) 0.0423(3) Uani 1 1 d . . . N1 N 0.2755(12) 0.6768(9) 0.1326(7) 0.038(2) Uani 1 1 d . . . N2 N 0.0264(10) 0.6791(8) 0.0253(7) 0.031(2) Uani 1 1 d . . . N3 N 0.3814(12) 0.7645(9) 0.3776(7) 0.041(2) Uani 1 1 d . . . N4 N 0.2805(12) 0.7847(9) 0.5036(7) 0.039(2) Uani 1 1 d . . . C1 C 0.1244(14) 0.6936(10) 0.1206(9) 0.035(3) Uani 1 1 d . . . H1A H 0.0896 0.7141 0.1749 0.041 Uiso 1 1 calc R . . C2 C 0.1163(13) 0.6492(10) -0.0346(8) 0.031(2) Uani 1 1 d . . . C3 C 0.0775(16) 0.6203(9) -0.1365(9) 0.042(3) Uani 1 1 d . . . H3A H -0.0282 0.6191 -0.1814 0.050 Uiso 1 1 calc R . . C4 C 0.2006(16) 0.5931(12) -0.1699(9) 0.050(3) Uani 1 1 d . . . H4A H 0.1781 0.5738 -0.2392 0.059 Uiso 1 1 calc R . . C5 C 0.3594(16) 0.5933(12) -0.1037(10) 0.049(3) Uani 1 1 d . . . H5A H 0.4390 0.5722 -0.1293 0.059 Uiso 1 1 calc R . . C6 C 0.3984(15) 0.6243(12) -0.0012(9) 0.043(3) Uani 1 1 d . . . H6A H 0.5053 0.6269 0.0432 0.051 Uiso 1 1 calc R . . C7 C 0.2772(13) 0.6511(9) 0.0341(9) 0.032(3) Uani 1 1 d . . . C8 C -0.1391(13) 0.6989(10) -0.0112(9) 0.039(3) Uani 1 1 d . . . H8A H -0.1874 0.6985 0.0440 0.047 Uiso 1 1 calc R . . H8B H -0.2186 0.6284 -0.0632 0.047 Uiso 1 1 calc R . . C9 C -0.1272(15) 0.8197(10) -0.0534(9) 0.043(3) Uani 1 1 d . . . H9A H -0.2432 0.8256 -0.0784 0.051 Uiso 1 1 calc R . . H9B H -0.0835 0.8184 -0.1105 0.051 Uiso 1 1 calc R . . C10 C -0.0080(17) 0.9391(11) 0.0237(10) 0.049(3) Uani 1 1 d . . . H10A H -0.0547 0.9435 0.0792 0.059 Uiso 1 1 calc R . . H10B H 0.1070 0.9320 0.0512 0.059 Uiso 1 1 calc R . . C11 C 0.3408(14) 0.7138(10) 0.4541(9) 0.037(3) Uani 1 1 d . . . H11A H 0.3528 0.6366 0.4719 0.044 Uiso 1 1 calc R . . C12 C 0.2769(14) 0.8900(10) 0.4540(9) 0.040(3) Uani 1 1 d . . . C13 C 0.2292(15) 0.9922(11) 0.4734(10) 0.047(3) Uani 1 1 d . . . H13A H 0.1874 1.0004 0.5274 0.056 Uiso 1 1 calc R . . C14 C 0.2457(18) 1.0814(13) 0.4103(12) 0.061(4) Uani 1 1 d . . . H14A H 0.2145 1.1530 0.4206 0.074 Uiso 1 1 calc R . . C15 C 0.3077(18) 1.0670(12) 0.3315(12) 0.060(4) Uani 1 1 d . . . H15A H 0.3140 1.1288 0.2883 0.072 Uiso 1 1 calc R . . C16 C 0.3602(17) 0.9679(11) 0.3134(10) 0.048(3) Uani 1 1 d . . . H16A H 0.4070 0.9615 0.2613 0.058 Uiso 1 1 calc R . . C17 C 0.3399(13) 0.8762(9) 0.3775(9) 0.034(3) Uani 1 1 d . . . C18 C 0.2073(15) 0.7462(13) 0.5852(10) 0.048(3) Uani 1 1 d . . . H18A H 0.2268 0.8216 0.6307 0.058 Uiso 1 1 calc R . . H18B H 0.2669 0.6934 0.6237 0.058 Uiso 1 1 calc R . . C19 C 0.0160(17) 0.6735(12) 0.5451(10) 0.055(3) Uani 1 1 d . . . H19A H -0.0428 0.7287 0.5095 0.066 Uiso 1 1 calc R . . H19B H -0.0267 0.6528 0.6020 0.066 Uiso 1 1 calc R . . C20 C -0.0337(15) 0.5517(12) 0.4746(11) 0.052(3) Uani 1 1 d . . . H20A H 0.0118 0.5716 0.4186 0.062 Uiso 1 1 calc R . . H20B H -0.1599 0.5171 0.4469 0.062 Uiso 1 1 calc R . . O1 O 0.524(3) 1.029(2) 0.060(2) 0.105(8) Uiso 0.50 1 d P . . H2O1 H 0.5625 1.0645 0.1201 0.126 Uiso 0.50 1 d PR . . H1O1 H 0.5000 1.0000 0.0000 0.126 Uiso 1 2 d SR . . 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 0.0357(5) 0.0383(5) 0.0287(5) 0.0053(3) 0.0092(3) 0.0137(4) I1 0.0404(5) 0.0845(7) 0.0528(6) -0.0011(5) 0.0179(4) -0.0016(5) I2 0.0476(5) 0.0375(4) 0.0409(5) 0.0086(3) 0.0080(4) 0.0181(4) N1 0.039(5) 0.043(5) 0.034(6) 0.012(4) 0.011(4) 0.016(4) N2 0.027(5) 0.029(5) 0.037(6) 0.005(4) 0.008(4) 0.012(4) N3 0.050(6) 0.053(6) 0.024(5) 0.006(4) 0.013(4) 0.023(5) N4 0.038(5) 0.048(6) 0.028(5) -0.003(4) 0.005(4) 0.016(5) C1 0.041(6) 0.033(6) 0.030(7) 0.004(5) 0.011(5) 0.012(5) C2 0.029(5) 0.033(6) 0.029(7) 0.006(5) 0.005(5) 0.010(5) C3 0.053(7) 0.024(5) 0.037(7) 0.005(5) 0.002(6) 0.007(5) C4 0.060(8) 0.062(8) 0.022(7) -0.007(6) -0.003(6) 0.030(7) C5 0.045(7) 0.071(9) 0.047(9) 0.001(7) 0.021(6) 0.034(7) C6 0.034(6) 0.065(8) 0.036(7) 0.011(6) 0.014(5) 0.023(6) C7 0.029(6) 0.024(5) 0.046(7) 0.008(5) 0.017(5) 0.010(5) C8 0.030(6) 0.034(6) 0.047(8) 0.009(5) 0.004(5) 0.007(5) C9 0.044(7) 0.043(7) 0.039(7) 0.008(5) 0.003(5) 0.021(6) C10 0.054(8) 0.045(7) 0.050(8) 0.009(6) 0.009(6) 0.027(6) C11 0.044(7) 0.038(6) 0.032(7) 0.008(5) 0.011(5) 0.020(5) C12 0.036(6) 0.027(6) 0.043(8) -0.012(5) 0.003(5) 0.004(5) C13 0.045(7) 0.040(7) 0.048(8) -0.009(6) 0.009(6) 0.010(6) C14 0.057(9) 0.046(8) 0.069(11) -0.008(7) -0.003(8) 0.024(7) C15 0.062(9) 0.039(7) 0.065(10) 0.005(7) 0.006(8) 0.011(7) C16 0.062(8) 0.036(7) 0.039(8) 0.005(6) 0.011(6) 0.012(6) C17 0.030(6) 0.024(5) 0.038(7) -0.007(5) -0.001(5) 0.008(5) C18 0.043(7) 0.068(8) 0.040(8) 0.002(6) 0.020(6) 0.023(6) C19 0.058(8) 0.064(9) 0.048(9) 0.014(7) 0.024(7) 0.021(7) C20 0.036(7) 0.052(7) 0.064(9) 0.020(7) 0.016(6) 0.009(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 Cd1 N3 2.228(9) . ? Cd1 N1 2.254(9) . ? Cd1 I1 2.6980(14) . ? Cd1 I2 2.7469(13) . ? N1 C1 1.330(13) . ? N1 C7 1.408(15) . ? N2 C1 1.335(14) . ? N2 C2 1.388(14) . ? N2 C8 1.453(13) . ? N3 C11 1.321(14) . ? N3 C17 1.405(13) . ? N4 C11 1.341(14) . ? N4 C12 1.401(15) . ? N4 C18 1.479(15) . ? C1 H1A 0.9400 . ? C2 C3 1.375(16) . ? C2 C7 1.433(14) . ? C3 C4 1.377(17) . ? C3 H3A 0.9400 . ? C4 C5 1.411(16) . ? C4 H4A 0.9400 . ? C5 C6 1.386(17) . ? C5 H5A 0.9400 . ? C6 C7 1.376(15) . ? C6 H6A 0.9400 . ? C8 C9 1.490(15) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.556(17) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C10 1.53(2) 2_575 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 H11A 0.9400 . ? C12 C17 1.358(16) . ? C12 C13 1.372(16) . ? C13 C14 1.37(2) . ? C13 H13A 0.9400 . ? C14 C15 1.38(2) . ? C14 H14A 0.9400 . ? C15 C16 1.363(18) . ? C15 H15A 0.9400 . ? C16 C17 1.400(16) . ? C16 H16A 0.9400 . ? C18 C19 1.511(17) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.524(18) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C20 1.56(2) 2_566 ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? O1 O1 1.66(5) 2_675 ? O1 H2O1 0.8500 . ? O1 H1O1 0.8298 . ? 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 N1 95.7(3) . . ? N3 Cd1 I1 117.6(3) . . ? N1 Cd1 I1 111.5(2) . . ? N3 Cd1 I2 101.5(2) . . ? N1 Cd1 I2 108.6(2) . . ? I1 Cd1 I2 119.13(5) . . ? C1 N1 C7 104.3(9) . . ? C1 N1 Cd1 130.0(8) . . ? C7 N1 Cd1 125.7(7) . . ? C1 N2 C2 107.5(8) . . ? C1 N2 C8 127.2(10) . . ? C2 N2 C8 125.2(9) . . ? C11 N3 C17 104.5(9) . . ? C11 N3 Cd1 124.4(8) . . ? C17 N3 Cd1 131.0(8) . . ? C11 N4 C12 107.3(10) . . ? C11 N4 C18 124.8(10) . . ? C12 N4 C18 127.2(10) . . ? N1 C1 N2 114.6(10) . . ? N1 C1 H1A 122.7 . . ? N2 C1 H1A 122.7 . . ? C3 C2 N2 133.3(10) . . ? C3 C2 C7 121.8(11) . . ? N2 C2 C7 104.9(9) . . ? C2 C3 C4 117.0(11) . . ? C2 C3 H3A 121.5 . . ? C4 C3 H3A 121.5 . . ? C3 C4 C5 122.4(12) . . ? C3 C4 H4A 118.8 . . ? C5 C4 H4A 118.8 . . ? C6 C5 C4 120.2(11) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C7 C6 C5 118.5(11) . . ? C7 C6 H6A 120.7 . . ? C5 C6 H6A 120.7 . . ? C6 C7 N1 131.2(10) . . ? C6 C7 C2 120.1(11) . . ? N1 C7 C2 108.6(9) . . ? N2 C8 C9 113.2(9) . . ? N2 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N2 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 113.6(10) . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C10 C10 C9 112.1(13) 2_575 . ? C10 C10 H10A 109.2 2_575 . ? C9 C10 H10A 109.2 . . ? C10 C10 H10B 109.2 2_575 . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N3 C11 N4 112.6(10) . . ? N3 C11 H11A 123.7 . . ? N4 C11 H11A 123.7 . . ? C17 C12 C13 123.1(12) . . ? C17 C12 N4 105.2(9) . . ? C13 C12 N4 131.6(12) . . ? C14 C13 C12 116.6(13) . . ? C14 C13 H13A 121.7 . . ? C12 C13 H13A 121.7 . . ? C13 C14 C15 120.6(12) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 123.3(13) . . ? C16 C15 H15A 118.4 . . ? C14 C15 H15A 118.4 . . ? C15 C16 C17 115.5(13) . . ? C15 C16 H16A 122.2 . . ? C17 C16 H16A 122.2 . . ? C12 C17 C16 120.9(10) . . ? C12 C17 N3 110.3(10) . . ? C16 C17 N3 128.8(11) . . ? N4 C18 C19 111.7(11) . . ? N4 C18 H18A 109.3 . . ? C19 C18 H18A 109.3 . . ? N4 C18 H18B 109.3 . . ? C19 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 115.1(11) . . ? C18 C19 H19A 108.5 . . ? C20 C19 H19A 108.5 . . ? C18 C19 H19B 108.5 . . ? C20 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C19 C20 C20 114.0(15) . 2_566 ? C19 C20 H20A 108.7 . . ? C20 C20 H20A 108.7 2_566 . ? C19 C20 H20B 108.7 . . ? C20 C20 H20B 108.7 2_566 . ? H20A C20 H20B 107.6 . . ? O1 O1 H2O1 172.1 2_675 . ? O1 O1 H1O1 0.0 2_675 . ? H2O1 O1 H1O1 172.1 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.776 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.213 #===END #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 811026' #TrackingRef '- JPLangCIF (revised).CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H44 Cd Cl2 N8' _chemical_formula_sum 'C40 H44 Cd Cl2 N8' _chemical_formula_weight 820.13 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' Cl Cl 0.1484 0.1585 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.056(2) _cell_length_b 12.055(2) _cell_length_c 12.710(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.09(3) _cell_angle_gamma 90.00 _cell_volume 1844.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5216 _cell_measurement_theta_min 3.3800 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8000 _exptl_absorpt_correction_T_max 0.9262 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11461 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0775 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4198 _reflns_number_gt 3270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4198 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.5000 0.0000 0.02777(12) Uani 1 2 d S . . Cl1 Cl 0.29806(7) 0.57704(7) -0.00395(8) 0.0387(2) Uani 1 1 d . . . N1 N 0.5605(2) 0.6236(2) 0.1317(2) 0.0325(7) Uani 1 1 d . . . N2 N 0.6192(2) 0.6671(2) 0.2957(2) 0.0345(7) Uani 1 1 d . . . N3 N 0.8227(2) 0.2243(2) 0.7257(2) 0.0315(7) Uani 1 1 d . . . N4 N 0.9519(2) 0.1359(2) 0.6364(2) 0.0327(7) Uani 1 1 d . . . C1 C 0.4958(3) 0.8159(3) 0.0789(3) 0.0373(9) Uani 1 1 d . . . H1A H 0.4696 0.7978 0.0101 0.045 Uiso 1 1 calc R . . C2 C 0.4894(3) 0.9224(3) 0.1174(4) 0.0477(11) Uani 1 1 d . . . H2A H 0.4570 0.9781 0.0741 0.057 Uiso 1 1 calc R . . C3 C 0.5296(4) 0.9494(3) 0.2187(4) 0.0513(11) Uani 1 1 d . . . H3A H 0.5246 1.0235 0.2409 0.062 Uiso 1 1 calc R . . C4 C 0.5764(3) 0.8724(3) 0.2881(3) 0.0437(10) Uani 1 1 d . . . H4A H 0.6036 0.8917 0.3563 0.052 Uiso 1 1 calc R . . C5 C 0.5807(3) 0.7645(3) 0.2501(3) 0.0314(8) Uani 1 1 d . . . C6 C 0.5429(3) 0.7361(3) 0.1470(3) 0.0308(8) Uani 1 1 d . . . C7 C 0.6051(3) 0.5872(3) 0.2212(3) 0.0358(9) Uani 1 1 d . . . H7A H 0.6253 0.5127 0.2328 0.043 Uiso 1 1 calc R . . C8 C 0.6566(4) 0.6539(3) 0.4066(3) 0.0468(10) Uani 1 1 d . . . H8A H 0.6041 0.6917 0.4506 0.056 Uiso 1 1 calc R . . H8B H 0.7291 0.6899 0.4184 0.056 Uiso 1 1 calc R . . C9 C 0.6662(3) 0.5342(3) 0.4402(3) 0.0435(10) Uani 1 1 d . . . H9A H 0.7296 0.5002 0.4074 0.052 Uiso 1 1 calc R . . H9B H 0.5990 0.4942 0.4154 0.052 Uiso 1 1 calc R . . C10 C 0.6816(3) 0.5226(3) 0.5595(3) 0.0382(9) Uani 1 1 d . . . H10A H 0.7470 0.5654 0.5844 0.046 Uiso 1 1 calc R . . H10B H 0.6168 0.5541 0.5919 0.046 Uiso 1 1 calc R . . C11 C 0.6962(3) 0.4033(3) 0.5950(3) 0.0419(10) Uani 1 1 d . . . H11A H 0.7648 0.3739 0.5676 0.050 Uiso 1 1 calc R . . H11B H 0.6342 0.3592 0.5645 0.050 Uiso 1 1 calc R . . C12 C 0.7013(3) 0.3897(3) 0.7136(3) 0.0389(9) Uani 1 1 d . . . H12A H 0.7635 0.4336 0.7439 0.047 Uiso 1 1 calc R . . H12B H 0.6329 0.4195 0.7408 0.047 Uiso 1 1 calc R . . C13 C 0.7153(3) 0.2705(3) 0.7499(3) 0.0362(9) Uani 1 1 d . . . H13A H 0.7075 0.2670 0.8262 0.043 Uiso 1 1 calc R . . H13B H 0.6562 0.2252 0.7158 0.043 Uiso 1 1 calc R . . C14 C 0.8452(3) 0.1563(3) 0.6438(3) 0.0344(9) Uani 1 1 d . . . H14A H 0.7898 0.1268 0.5970 0.041 Uiso 1 1 calc R . . C15 C 0.9242(3) 0.2505(3) 0.7757(3) 0.0296(8) Uani 1 1 d . . . C16 C 0.9508(3) 0.3131(3) 0.8649(3) 0.0368(9) Uani 1 1 d . . . H16A H 0.8957 0.3486 0.9022 0.044 Uiso 1 1 calc R . . C17 C 1.0615(3) 0.3208(3) 0.8963(3) 0.0391(9) Uani 1 1 d . . . H17A H 1.0827 0.3617 0.9571 0.047 Uiso 1 1 calc R . . C18 C 1.1431(3) 0.2690(3) 0.8395(3) 0.0428(10) Uani 1 1 d . . . H18A H 1.2180 0.2763 0.8628 0.051 Uiso 1 1 calc R . . C19 C 1.1164(3) 0.2076(3) 0.7502(3) 0.0361(9) Uani 1 1 d . . . H19A H 1.1722 0.1749 0.7117 0.043 Uiso 1 1 calc R . . C20 C 1.0039(3) 0.1952(3) 0.7184(3) 0.0295(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02681(19) 0.0312(2) 0.0252(2) -0.00404(17) 0.00108(14) -0.00026(16) Cl1 0.0324(5) 0.0489(6) 0.0350(6) 0.0026(4) 0.0026(4) 0.0111(4) N1 0.0341(16) 0.0306(16) 0.0325(19) -0.0029(14) -0.0020(14) -0.0013(13) N2 0.0408(18) 0.0326(17) 0.0291(19) -0.0055(14) -0.0076(14) -0.0018(14) N3 0.0292(15) 0.0344(16) 0.0313(19) -0.0015(14) 0.0048(14) 0.0037(13) N4 0.0312(16) 0.0321(16) 0.035(2) -0.0012(14) 0.0048(14) 0.0029(13) C1 0.044(2) 0.039(2) 0.029(2) 0.0004(18) -0.0002(18) 0.0045(17) C2 0.050(2) 0.038(2) 0.055(3) 0.006(2) -0.001(2) 0.0103(19) C3 0.064(3) 0.031(2) 0.059(3) -0.012(2) 0.003(2) 0.004(2) C4 0.048(2) 0.041(2) 0.042(3) -0.012(2) -0.002(2) 0.0019(19) C5 0.0278(18) 0.034(2) 0.033(2) -0.0040(17) 0.0014(16) -0.0001(15) C6 0.0267(18) 0.033(2) 0.033(2) -0.0017(17) 0.0010(16) 0.0021(15) C7 0.041(2) 0.028(2) 0.038(2) -0.0029(18) -0.0044(18) 0.0025(16) C8 0.066(3) 0.040(2) 0.032(2) 0.0000(19) -0.014(2) -0.004(2) C9 0.051(2) 0.040(2) 0.039(3) -0.0016(18) -0.008(2) 0.0017(18) C10 0.044(2) 0.040(2) 0.030(2) -0.0023(17) -0.0063(17) 0.0045(17) C11 0.052(2) 0.038(2) 0.035(2) 0.0006(18) -0.0008(19) 0.0082(18) C12 0.041(2) 0.042(2) 0.033(2) 0.0001(18) 0.0018(18) 0.0075(18) C13 0.0304(19) 0.043(2) 0.036(2) 0.0006(18) 0.0082(18) 0.0048(17) C14 0.035(2) 0.035(2) 0.033(2) 0.0020(17) 0.0024(17) -0.0028(16) C15 0.0313(19) 0.0283(18) 0.030(2) 0.0054(16) 0.0058(16) 0.0009(15) C16 0.041(2) 0.040(2) 0.031(2) 0.0054(18) 0.0100(18) 0.0045(18) C17 0.043(2) 0.044(2) 0.030(2) -0.0011(18) -0.0015(18) -0.0014(18) C18 0.035(2) 0.048(2) 0.045(3) 0.002(2) -0.0020(19) -0.0067(18) C19 0.031(2) 0.035(2) 0.042(3) 0.0039(19) 0.0064(18) 0.0015(16) C20 0.0344(19) 0.0256(18) 0.029(2) 0.0061(16) 0.0045(16) 0.0019(15) _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 N1 2.329(3) . ? Cd1 N1 2.329(3) 3_665 ? Cd1 N4 2.477(3) 2_655 ? Cd1 N4 2.477(3) 4_565 ? Cd1 Cl1 2.6036(10) . ? Cd1 Cl1 2.6036(9) 3_665 ? N1 C7 1.307(5) . ? N1 C6 1.389(4) . ? N2 C7 1.355(4) . ? N2 C5 1.379(4) . ? N2 C8 1.465(5) . ? N3 C14 1.363(4) . ? N3 C15 1.385(4) . ? N3 C13 1.458(4) . ? N4 C14 1.318(4) . ? N4 C20 1.386(5) . ? N4 Cd1 2.477(3) 2_645 ? C1 C2 1.378(5) . ? C1 C6 1.394(5) . ? C1 H1A 0.9400 . ? C2 C3 1.389(6) . ? C2 H2A 0.9400 . ? C3 C4 1.380(6) . ? C3 H3A 0.9400 . ? C4 C5 1.389(5) . ? C4 H4A 0.9400 . ? C5 C6 1.406(5) . ? C7 H7A 0.9400 . ? C8 C9 1.508(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.523(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.515(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.514(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.515(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9400 . ? C15 C16 1.385(5) . ? C15 C20 1.405(4) . ? C16 C17 1.375(5) . ? C16 H16A 0.9400 . ? C17 C18 1.399(5) . ? C17 H17A 0.9400 . ? C18 C19 1.378(5) . ? C18 H18A 0.9400 . ? C19 C20 1.402(5) . ? C19 H19A 0.9400 . ? 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 N1 Cd1 N1 180.0 . 3_665 ? N1 Cd1 N4 90.24(10) . 2_655 ? N1 Cd1 N4 89.76(10) 3_665 2_655 ? N1 Cd1 N4 89.76(10) . 4_565 ? N1 Cd1 N4 90.24(10) 3_665 4_565 ? N4 Cd1 N4 180.0 2_655 4_565 ? N1 Cd1 Cl1 92.42(8) . . ? N1 Cd1 Cl1 87.58(8) 3_665 . ? N4 Cd1 Cl1 90.27(7) 2_655 . ? N4 Cd1 Cl1 89.73(7) 4_565 . ? N1 Cd1 Cl1 87.58(8) . 3_665 ? N1 Cd1 Cl1 92.41(8) 3_665 3_665 ? N4 Cd1 Cl1 89.73(7) 2_655 3_665 ? N4 Cd1 Cl1 90.27(7) 4_565 3_665 ? Cl1 Cd1 Cl1 180.0 . 3_665 ? C7 N1 C6 105.4(3) . . ? C7 N1 Cd1 120.6(2) . . ? C6 N1 Cd1 132.9(3) . . ? C7 N2 C5 106.6(3) . . ? C7 N2 C8 128.0(3) . . ? C5 N2 C8 125.2(3) . . ? C14 N3 C15 106.3(3) . . ? C14 N3 C13 127.3(3) . . ? C15 N3 C13 126.1(3) . . ? C14 N4 C20 104.7(3) . . ? C14 N4 Cd1 116.1(2) . 2_645 ? C20 N4 Cd1 138.9(2) . 2_645 ? C2 C1 C6 116.9(4) . . ? C2 C1 H1A 121.6 . . ? C6 C1 H1A 121.6 . . ? C1 C2 C3 121.6(4) . . ? C1 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 . . ? C4 C3 C2 123.0(4) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C3 C4 C5 115.4(4) . . ? C3 C4 H4A 122.3 . . ? C5 C4 H4A 122.3 . . ? N2 C5 C4 132.0(4) . . ? N2 C5 C6 105.6(3) . . ? C4 C5 C6 122.4(4) . . ? N1 C6 C1 130.4(4) . . ? N1 C6 C5 108.9(3) . . ? C1 C6 C5 120.7(3) . . ? N1 C7 N2 113.6(3) . . ? N1 C7 H7A 123.2 . . ? N2 C7 H7A 123.2 . . ? N2 C8 C9 113.1(3) . . ? N2 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N2 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 112.0(3) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 112.9(3) . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 C11 C12 113.4(3) . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C11 113.8(3) . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? N3 C13 C12 112.6(3) . . ? N3 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? N3 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N4 C14 N3 113.7(3) . . ? N4 C14 H14A 123.2 . . ? N3 C14 H14A 123.2 . . ? C16 C15 N3 131.3(3) . . ? C16 C15 C20 123.2(3) . . ? N3 C15 C20 105.4(3) . . ? C17 C16 C15 116.9(3) . . ? C17 C16 H16A 121.5 . . ? C15 C16 H16A 121.5 . . ? C16 C17 C18 121.2(4) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C19 C18 C17 121.7(4) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C20 118.3(3) . . ? C18 C19 H19A 120.9 . . ? C20 C19 H19A 120.9 . . ? N4 C20 C19 131.6(3) . . ? N4 C20 C15 109.9(3) . . ? C19 C20 C15 118.5(3) . . ? 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 C14 H14A Cl1 0.94 2.78 3.413(4) 125.8 4_666 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.436 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.084 #===END #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 811027' #TrackingRef '- JPLangCIF (revised).CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H62 Cd3 N8 O12' _chemical_formula_sum 'C52 H62 Cd3 N8 O12' _chemical_formula_weight 1328.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7552(18) _cell_length_b 9.4860(19) _cell_length_c 16.064(3) _cell_angle_alpha 93.72(3) _cell_angle_beta 94.91(3) _cell_angle_gamma 98.88(3) _cell_volume 1309.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5412 _cell_measurement_theta_min 3.1906 _cell_measurement_theta_max 27.4816 _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 670 _exptl_absorpt_coefficient_mu 1.277 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6634 _exptl_absorpt_correction_T_max 0.8829 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12623 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5888 _reflns_number_gt 4661 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5888 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.038 _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 Cd1 Cd 0.67333(3) 0.56871(2) 0.256747(14) 0.03180(8) Uani 1 1 d . . . Cd2 Cd 0.5000 0.5000 0.0000 0.02205(8) Uani 1 2 d S . . N1 N 0.7877(3) 0.4147(3) 0.33546(17) 0.0366(6) Uani 1 1 d . . . N2 N 0.9937(3) 0.3485(3) 0.40526(17) 0.0330(6) Uani 1 1 d . . . N3 N 1.4151(3) -0.2866(3) 0.01997(16) 0.0275(5) Uani 1 1 d . . . N4 N 1.3911(3) -0.0847(3) 0.09285(15) 0.0266(5) Uani 1 1 d . . . O1 O 0.7680(4) 0.7486(3) 0.36829(17) 0.0618(8) Uani 1 1 d . . . O2 O 0.6112(4) 0.7971(3) 0.26876(18) 0.0688(9) Uani 1 1 d . . . O3 O 0.4098(3) 0.4652(3) 0.27101(15) 0.0491(6) Uani 1 1 d . . . O4 O 0.4825(2) 0.4733(2) 0.14474(13) 0.0335(5) Uani 1 1 d . . . O5 O 0.7440(2) 0.6149(2) 0.05200(15) 0.0400(6) Uani 1 1 d . . . O6 O 0.8687(3) 0.5943(3) 0.17640(15) 0.0445(6) Uani 1 1 d . . . C1 C 0.8733(3) 0.3303(3) 0.45673(19) 0.0263(6) Uani 1 1 d . . . C2 C 0.8688(4) 0.2869(4) 0.5379(2) 0.0392(8) Uani 1 1 d . . . H2 H 0.9559 0.2612 0.5680 0.047 Uiso 1 1 calc R . . C3 C 0.7270(4) 0.2838(4) 0.5718(2) 0.0451(9) Uani 1 1 d . . . H3 H 0.7178 0.2561 0.6265 0.054 Uiso 1 1 calc R . . C4 C 0.5994(4) 0.3208(4) 0.5263(2) 0.0435(9) Uani 1 1 d . . . H4 H 0.5052 0.3160 0.5508 0.052 Uiso 1 1 calc R . . C5 C 0.6056(4) 0.3648(3) 0.4457(2) 0.0375(8) Uani 1 1 d . . . H5 H 0.5182 0.3895 0.4154 0.045 Uiso 1 1 calc R . . C6 C 0.7457(4) 0.3704(3) 0.4123(2) 0.0326(7) Uani 1 1 d . . . C7 C 0.9378(4) 0.4004(3) 0.3351(2) 0.0349(7) Uani 1 1 d . . . H7 H 0.9974 0.4242 0.2906 0.042 Uiso 1 1 calc R . . C8 C 1.1499(4) 0.3182(4) 0.4251(2) 0.0378(8) Uani 1 1 d . . . H8A H 1.1917 0.3663 0.4800 0.045 Uiso 1 1 calc R . . H8B H 1.2164 0.3576 0.3834 0.045 Uiso 1 1 calc R . . C9 C 1.1555(4) 0.1596(4) 0.4267(2) 0.0389(8) Uani 1 1 d . . . H9A H 1.0750 0.1180 0.4608 0.047 Uiso 1 1 calc R . . H9B H 1.2561 0.1480 0.4548 0.047 Uiso 1 1 calc R . . C10 C 1.1329(4) 0.0745(4) 0.3415(2) 0.0382(8) Uani 1 1 d . . . H10A H 1.0974 -0.0265 0.3492 0.046 Uiso 1 1 calc R . . H10B H 1.0513 0.1084 0.3062 0.046 Uiso 1 1 calc R . . C11 C 1.2785(4) 0.0861(4) 0.2964(2) 0.0374(8) Uani 1 1 d . . . H11A H 1.3613 0.0557 0.3325 0.045 Uiso 1 1 calc R . . H11B H 1.3118 0.1867 0.2866 0.045 Uiso 1 1 calc R . . C12 C 1.2569(4) -0.0034(3) 0.2129(2) 0.0354(7) Uani 1 1 d . . . H12A H 1.2309 -0.1048 0.2229 0.042 Uiso 1 1 calc R . . H12B H 1.1696 0.0224 0.1780 0.042 Uiso 1 1 calc R . . C13 C 1.4012(4) 0.0179(3) 0.1663(2) 0.0320(7) Uani 1 1 d . . . H13A H 1.4169 0.1153 0.1481 0.038 Uiso 1 1 calc R . . H13B H 1.4916 0.0081 0.2045 0.038 Uiso 1 1 calc R . . C14 C 1.3147(3) -0.0789(3) 0.01415(18) 0.0242(6) Uani 1 1 d . . . C15 C 1.2382(4) 0.0238(3) -0.0206(2) 0.0339(7) Uani 1 1 d . . . H15 H 1.2287 0.1092 0.0102 0.041 Uiso 1 1 calc R . . C16 C 1.1766(4) -0.0057(4) -0.1028(2) 0.0404(8) Uani 1 1 d . . . H16 H 1.1258 0.0620 -0.1292 0.048 Uiso 1 1 calc R . . C17 C 1.1879(4) -0.1341(4) -0.1477(2) 0.0380(8) Uani 1 1 d . . . H17 H 1.1423 -0.1513 -0.2033 0.046 Uiso 1 1 calc R . . C18 C 1.2637(4) -0.2362(3) -0.1132(2) 0.0313(7) Uani 1 1 d . . . H18 H 1.2704 -0.3223 -0.1440 0.038 Uiso 1 1 calc R . . C19 C 1.3299(3) -0.2070(3) -0.03107(18) 0.0247(6) Uani 1 1 d . . . C20 C 1.4473(3) -0.2096(3) 0.0912(2) 0.0297(7) Uani 1 1 d . . . H20 H 1.5047 -0.2383 0.1374 0.036 Uiso 1 1 calc R . . C21 C 0.7050(5) 0.9829(4) 0.3741(2) 0.0498(9) Uani 1 1 d . . . H21A H 0.6945 1.0485 0.3309 0.075 Uiso 1 1 calc R . . H21B H 0.8042 1.0115 0.4073 0.075 Uiso 1 1 calc R . . H21C H 0.6217 0.9846 0.4100 0.075 Uiso 1 1 calc R . . C22 C 0.6969(4) 0.8342(4) 0.3340(2) 0.0344(7) Uani 1 1 d . . . C23 C 0.2157(4) 0.3855(4) 0.1570(2) 0.0454(9) Uani 1 1 d . . . H23A H 0.1797 0.2979 0.1824 0.068 Uiso 1 1 calc R . . H23B H 0.2147 0.3652 0.0970 0.068 Uiso 1 1 calc R . . H23C H 0.1477 0.4548 0.1679 0.068 Uiso 1 1 calc R . . C24 C 0.3773(4) 0.4450(3) 0.1935(2) 0.0298(7) Uani 1 1 d . . . C25 C 1.0154(4) 0.6792(4) 0.0685(2) 0.0410(8) Uani 1 1 d . . . H25A H 1.0513 0.6013 0.0377 0.061 Uiso 1 1 calc R . . H25B H 1.0916 0.7173 0.1151 0.061 Uiso 1 1 calc R . . H25C H 1.0015 0.7541 0.0316 0.061 Uiso 1 1 calc R . . C26 C 0.8628(3) 0.6247(3) 0.1014(2) 0.0292(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04036(15) 0.02999(13) 0.02441(14) 0.00143(9) -0.00263(10) 0.00715(10) Cd2 0.02471(16) 0.02149(15) 0.02069(16) 0.00112(11) 0.00243(11) 0.00610(11) N1 0.0473(17) 0.0338(15) 0.0295(15) 0.0038(12) 0.0021(12) 0.0097(12) N2 0.0345(15) 0.0328(14) 0.0319(15) -0.0023(12) 0.0025(12) 0.0090(11) N3 0.0324(14) 0.0253(13) 0.0250(14) 0.0010(10) 0.0010(11) 0.0071(10) N4 0.0293(13) 0.0262(13) 0.0248(13) -0.0020(10) 0.0015(10) 0.0082(10) O1 0.084(2) 0.0516(17) 0.0486(17) -0.0116(13) -0.0250(15) 0.0309(15) O2 0.107(2) 0.0429(16) 0.0510(18) -0.0123(13) -0.0365(17) 0.0267(15) O3 0.0517(15) 0.0691(18) 0.0242(13) 0.0025(12) 0.0054(11) 0.0016(13) O4 0.0318(12) 0.0437(13) 0.0247(12) 0.0035(10) 0.0043(9) 0.0041(10) O5 0.0298(12) 0.0444(14) 0.0428(14) 0.0095(11) -0.0018(10) -0.0028(10) O6 0.0448(14) 0.0561(16) 0.0324(14) 0.0102(12) 0.0019(11) 0.0055(12) C1 0.0326(16) 0.0201(14) 0.0265(16) -0.0012(12) 0.0049(13) 0.0054(11) C2 0.047(2) 0.0403(19) 0.0327(19) 0.0047(15) 0.0038(16) 0.0130(15) C3 0.058(2) 0.048(2) 0.033(2) 0.0091(17) 0.0143(17) 0.0124(17) C4 0.0383(19) 0.050(2) 0.045(2) 0.0057(17) 0.0151(16) 0.0089(16) C5 0.0335(18) 0.0354(17) 0.044(2) 0.0005(15) 0.0034(15) 0.0084(13) C6 0.0401(18) 0.0271(16) 0.0304(18) -0.0005(13) 0.0003(14) 0.0078(13) C7 0.049(2) 0.0314(17) 0.0267(17) 0.0028(13) 0.0067(15) 0.0122(14) C8 0.0283(16) 0.0419(19) 0.042(2) -0.0078(15) -0.0021(14) 0.0094(14) C9 0.0385(19) 0.050(2) 0.0308(19) 0.0017(16) 0.0022(15) 0.0168(16) C10 0.0405(19) 0.0425(19) 0.0330(19) -0.0003(15) 0.0027(15) 0.0132(15) C11 0.0370(18) 0.0422(19) 0.0325(19) -0.0032(15) 0.0017(15) 0.0087(14) C12 0.0354(18) 0.0354(17) 0.0350(19) -0.0024(14) 0.0072(14) 0.0046(13) C13 0.0341(17) 0.0320(16) 0.0291(17) -0.0064(13) 0.0032(13) 0.0062(13) C14 0.0224(14) 0.0251(14) 0.0250(15) 0.0019(12) 0.0033(12) 0.0035(11) C15 0.0350(17) 0.0250(15) 0.043(2) 0.0026(14) 0.0023(15) 0.0094(13) C16 0.0418(19) 0.0372(19) 0.043(2) 0.0091(16) -0.0078(16) 0.0120(15) C17 0.0397(19) 0.0401(19) 0.0322(19) 0.0051(15) -0.0079(14) 0.0055(14) C18 0.0338(17) 0.0324(17) 0.0280(17) -0.0005(13) 0.0028(13) 0.0078(13) C19 0.0233(14) 0.0244(14) 0.0273(16) 0.0043(12) 0.0056(12) 0.0041(11) C20 0.0316(16) 0.0304(16) 0.0288(17) 0.0042(13) 0.0020(13) 0.0101(13) C21 0.063(3) 0.037(2) 0.046(2) -0.0043(17) -0.0081(19) 0.0072(17) C22 0.0417(19) 0.0350(17) 0.0249(17) 0.0013(14) -0.0029(14) 0.0047(14) C23 0.040(2) 0.058(2) 0.038(2) 0.0073(18) 0.0042(16) 0.0054(17) C24 0.0369(17) 0.0261(15) 0.0285(17) 0.0063(13) 0.0069(14) 0.0078(13) C25 0.0319(18) 0.0419(19) 0.048(2) 0.0052(16) 0.0029(15) 0.0011(14) C26 0.0289(16) 0.0217(14) 0.0352(18) -0.0029(13) 0.0002(13) 0.0018(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O6 2.223(2) . ? Cd1 N1 2.283(3) . ? Cd1 O2 2.314(3) . ? Cd1 O4 2.378(2) . ? Cd1 O1 2.392(3) . ? Cd1 O3 2.400(3) . ? Cd1 C22 2.705(3) . ? Cd1 C24 2.753(3) . ? Cd2 N3 2.275(2) 2_755 ? Cd2 N3 2.275(2) 1_465 ? Cd2 O5 2.304(2) . ? Cd2 O5 2.304(2) 2_665 ? Cd2 O4 2.370(2) . ? Cd2 O4 2.370(2) 2_665 ? N1 C7 1.342(4) . ? N1 C6 1.390(4) . ? N2 C7 1.343(4) . ? N2 C1 1.391(4) . ? N2 C8 1.453(4) . ? N3 C20 1.302(4) . ? N3 C19 1.395(4) . ? N3 Cd2 2.275(2) 1_645 ? N4 C20 1.350(4) . ? N4 C14 1.387(4) . ? N4 C13 1.467(4) . ? O1 C22 1.227(4) . ? O2 C22 1.233(4) . ? O3 C24 1.248(4) . ? O4 C24 1.268(4) . ? O5 C26 1.240(4) . ? O6 C26 1.256(4) . ? C1 C6 1.390(4) . ? C1 C2 1.395(4) . ? C2 C3 1.394(5) . ? C2 H2 0.9400 . ? C3 C4 1.386(5) . ? C3 H3 0.9400 . ? C4 C5 1.388(5) . ? C4 H4 0.9400 . ? C5 C6 1.376(5) . ? C5 H5 0.9400 . ? C7 H7 0.9400 . ? C8 C9 1.514(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.526(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.512(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.521(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.517(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.386(4) . ? C14 C19 1.405(4) . ? C15 C16 1.376(5) . ? C15 H15 0.9400 . ? C16 C17 1.395(5) . ? C16 H16 0.9400 . ? C17 C18 1.375(4) . ? C17 H17 0.9400 . ? C18 C19 1.387(4) . ? C18 H18 0.9400 . ? C20 H20 0.9400 . ? C21 C22 1.500(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C23 C24 1.495(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C25 C26 1.508(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Cd1 N1 91.60(9) . . ? O6 Cd1 O2 102.52(11) . . ? N1 Cd1 O2 139.90(10) . . ? O6 Cd1 O4 94.58(8) . . ? N1 Cd1 O4 118.93(9) . . ? O2 Cd1 O4 97.39(9) . . ? O6 Cd1 O1 101.06(11) . . ? N1 Cd1 O1 86.72(9) . . ? O2 Cd1 O1 53.97(9) . . ? O4 Cd1 O1 149.63(8) . . ? O6 Cd1 O3 147.69(9) . . ? N1 Cd1 O3 96.54(10) . . ? O2 Cd1 O3 91.14(11) . . ? O4 Cd1 O3 54.28(8) . . ? O1 Cd1 O3 110.57(10) . . ? O6 Cd1 C22 102.29(10) . . ? N1 Cd1 C22 113.51(10) . . ? O2 Cd1 C22 27.04(9) . . ? O4 Cd1 C22 124.05(9) . . ? O1 Cd1 C22 26.96(8) . . ? O3 Cd1 C22 102.93(10) . . ? O6 Cd1 C24 121.73(9) . . ? N1 Cd1 C24 110.51(10) . . ? O2 Cd1 C24 93.67(10) . . ? O4 Cd1 C24 27.39(8) . . ? O1 Cd1 C24 132.13(10) . . ? O3 Cd1 C24 26.94(8) . . ? C22 Cd1 C24 115.03(10) . . ? N3 Cd2 N3 180.0 2_755 1_465 ? N3 Cd2 O5 92.25(9) 2_755 . ? N3 Cd2 O5 87.75(9) 1_465 . ? N3 Cd2 O5 87.75(9) 2_755 2_665 ? N3 Cd2 O5 92.25(9) 1_465 2_665 ? O5 Cd2 O5 180.0 . 2_665 ? N3 Cd2 O4 92.33(9) 2_755 . ? N3 Cd2 O4 87.67(9) 1_465 . ? O5 Cd2 O4 80.69(8) . . ? O5 Cd2 O4 99.31(8) 2_665 . ? N3 Cd2 O4 87.67(9) 2_755 2_665 ? N3 Cd2 O4 92.33(9) 1_465 2_665 ? O5 Cd2 O4 99.31(8) . 2_665 ? O5 Cd2 O4 80.69(8) 2_665 2_665 ? O4 Cd2 O4 180.0 . 2_665 ? C7 N1 C6 105.0(3) . . ? C7 N1 Cd1 123.6(2) . . ? C6 N1 Cd1 126.2(2) . . ? C7 N2 C1 106.8(3) . . ? C7 N2 C8 127.3(3) . . ? C1 N2 C8 125.9(3) . . ? C20 N3 C19 105.0(2) . . ? C20 N3 Cd2 121.17(19) . 1_645 ? C19 N3 Cd2 133.9(2) . 1_645 ? C20 N4 C14 106.5(3) . . ? C20 N4 C13 125.7(3) . . ? C14 N4 C13 127.7(2) . . ? C22 O1 Cd1 90.9(2) . . ? C22 O2 Cd1 94.4(2) . . ? C24 O3 Cd1 92.5(2) . . ? C24 O4 Cd2 138.0(2) . . ? C24 O4 Cd1 93.01(18) . . ? Cd2 O4 Cd1 126.71(9) . . ? C26 O5 Cd2 151.0(2) . . ? C26 O6 Cd1 126.9(2) . . ? C6 C1 N2 106.2(3) . . ? C6 C1 C2 122.5(3) . . ? N2 C1 C2 131.3(3) . . ? C3 C2 C1 115.9(3) . . ? C3 C2 H2 122.0 . . ? C1 C2 H2 122.0 . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 122.3(3) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 116.8(3) . . ? C6 C5 H5 121.6 . . ? C4 C5 H5 121.6 . . ? C5 C6 C1 121.2(3) . . ? C5 C6 N1 129.6(3) . . ? C1 C6 N1 109.2(3) . . ? N1 C7 N2 112.8(3) . . ? N1 C7 H7 123.6 . . ? N2 C7 H7 123.6 . . ? N2 C8 C9 112.9(3) . . ? N2 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N2 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 115.8(3) . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C11 C10 C9 113.6(3) . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C10 C11 C12 113.3(3) . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C11 112.3(3) . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N4 C13 C12 112.7(3) . . ? N4 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? N4 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 N4 132.2(3) . . ? C15 C14 C19 122.6(3) . . ? N4 C14 C19 105.2(2) . . ? C16 C15 C14 116.4(3) . . ? C16 C15 H15 121.8 . . ? C14 C15 H15 121.8 . . ? C15 C16 C17 121.5(3) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 122.1(3) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 117.4(3) . . ? C17 C18 H18 121.3 . . ? C19 C18 H18 121.3 . . ? C18 C19 N3 130.8(3) . . ? C18 C19 C14 120.0(3) . . ? N3 C19 C14 109.1(3) . . ? N3 C20 N4 114.2(3) . . ? N3 C20 H20 122.9 . . ? N4 C20 H20 122.9 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 O2 120.6(3) . . ? O1 C22 C21 120.2(3) . . ? O2 C22 C21 119.1(3) . . ? O1 C22 Cd1 62.16(18) . . ? O2 C22 Cd1 58.52(18) . . ? C21 C22 Cd1 177.6(2) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 O4 120.0(3) . . ? O3 C24 C23 120.8(3) . . ? O4 C24 C23 119.1(3) . . ? O3 C24 Cd1 60.58(18) . . ? O4 C24 Cd1 59.60(16) . . ? C23 C24 Cd1 176.8(2) . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O5 C26 O6 126.5(3) . . ? O5 C26 C25 117.0(3) . . ? O6 C26 C25 116.5(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.747 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.134 #===END #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 811028' #TrackingRef '- JPLangCIF (revised).CIF' #============================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 N4 O8 Zn2' _chemical_formula_sum 'C28 H34 N4 O8 Zn2' _chemical_formula_weight 685.38 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 Tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 22.382(3) _cell_length_b 22.382(3) _cell_length_c 11.243(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5632(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5551 _cell_measurement_theta_min 3.2772 _cell_measurement_theta_max 27.4816 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 1.762 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6729 _exptl_absorpt_correction_T_max 0.7580 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8339 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3207 _reflns_number_gt 2655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+7.9510P] 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 3207 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.771687(15) 0.753144(16) 0.12496(3) 0.02830(13) Uani 1 1 d . . . N1 N 0.80317(11) 0.75461(11) -0.0430(2) 0.0266(5) Uani 1 1 d . . . N2 N 0.83927(11) 0.72327(11) -0.2164(2) 0.0272(5) Uani 1 1 d . . . O1 O 0.73980(12) 0.66775(11) 0.1278(2) 0.0456(6) Uani 1 1 d . . . O2 O 0.70927(12) 0.66239(11) 0.31506(19) 0.0464(6) Uani 1 1 d . . . O3 O 0.68619(10) 0.78266(12) 0.09591(19) 0.0430(6) Uani 1 1 d . . . O4 O 0.65591(10) 0.77844(12) 0.28294(19) 0.0452(6) Uani 1 1 d . . . C1 C 0.82666(13) 0.70964(14) -0.1019(2) 0.0280(6) Uani 1 1 d . . . H1 H 0.8339 0.6719 -0.0681 0.034 Uiso 1 1 calc R . . C2 C 0.80022(12) 0.80161(13) -0.1238(2) 0.0252(6) Uani 1 1 d . . . C3 C 0.78081(15) 0.86001(15) -0.1095(3) 0.0365(8) Uani 1 1 d . . . H3 H 0.7667 0.8740 -0.0359 0.044 Uiso 1 1 calc R . . C4 C 0.78309(17) 0.89658(16) -0.2081(3) 0.0469(9) Uani 1 1 d . . . H4 H 0.7705 0.9365 -0.2009 0.056 Uiso 1 1 calc R . . C5 C 0.80344(17) 0.87632(17) -0.3177(3) 0.0471(9) Uani 1 1 d . . . H5 H 0.8036 0.9026 -0.3830 0.056 Uiso 1 1 calc R . . C6 C 0.82312(15) 0.81916(16) -0.3327(3) 0.0387(8) Uani 1 1 d . . . H6 H 0.8367 0.8054 -0.4069 0.046 Uiso 1 1 calc R . . C7 C 0.82222(12) 0.78219(14) -0.2333(2) 0.0265(6) Uani 1 1 d . . . C8 C 0.87081(14) 0.68519(15) -0.3028(3) 0.0332(7) Uani 1 1 d . . . H8A H 0.8595 0.6974 -0.3835 0.040 Uiso 1 1 calc R . . H8B H 0.8581 0.6437 -0.2918 0.040 Uiso 1 1 calc R . . C9 C 0.93829(14) 0.68864(14) -0.2906(3) 0.0317(7) Uani 1 1 d . . . H9A H 0.9562 0.6630 -0.3517 0.038 Uiso 1 1 calc R . . H9B H 0.9494 0.6720 -0.2130 0.038 Uiso 1 1 calc R . . C10 C 0.96587(13) 0.75057(14) -0.3011(3) 0.0331(7) Uani 1 1 d . . . H10A H 0.9520 0.7752 -0.2345 0.040 Uiso 1 1 calc R . . H10B H 0.9519 0.7693 -0.3749 0.040 Uiso 1 1 calc R . . C11 C 0.70283(17) 0.57571(15) 0.1968(3) 0.0465(9) Uani 1 1 d . . . H11A H 0.6607 0.5723 0.1779 0.070 Uiso 1 1 calc R . . H11B H 0.7113 0.5536 0.2691 0.070 Uiso 1 1 calc R . . H11C H 0.7263 0.5595 0.1319 0.070 Uiso 1 1 calc R . . C12 C 0.71865(14) 0.64032(14) 0.2146(3) 0.0316(7) Uani 1 1 d . . . C13 C 0.58904(14) 0.81741(16) 0.1412(3) 0.0381(8) Uani 1 1 d . . . H13A H 0.5570 0.7947 0.1777 0.057 Uiso 1 1 calc R . . H13B H 0.5847 0.8162 0.0554 0.057 Uiso 1 1 calc R . . H13C H 0.5872 0.8585 0.1681 0.057 Uiso 1 1 calc R . . C14 C 0.64849(14) 0.79061(14) 0.1760(3) 0.0296(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0295(2) 0.0362(2) 0.01925(19) 0.00125(14) 0.00468(14) -0.00069(15) N1 0.0251(12) 0.0344(14) 0.0202(11) 0.0009(10) 0.0044(10) 0.0010(11) N2 0.0297(13) 0.0314(13) 0.0204(11) -0.0008(10) 0.0053(10) 0.0020(11) O1 0.0627(17) 0.0367(13) 0.0374(13) 0.0003(11) 0.0075(12) -0.0116(12) O2 0.0622(17) 0.0430(14) 0.0339(12) -0.0070(11) 0.0092(12) -0.0124(12) O3 0.0323(13) 0.0644(17) 0.0322(11) 0.0010(11) 0.0041(10) 0.0113(12) O4 0.0379(13) 0.0693(18) 0.0283(12) 0.0098(11) 0.0014(10) 0.0059(12) C1 0.0300(16) 0.0313(16) 0.0227(13) 0.0032(12) 0.0024(12) -0.0008(13) C2 0.0220(14) 0.0320(15) 0.0216(13) 0.0008(12) 0.0014(11) 0.0002(12) C3 0.0387(18) 0.0383(18) 0.0324(16) -0.0034(14) 0.0054(14) 0.0073(15) C4 0.054(2) 0.0354(19) 0.051(2) 0.0066(17) 0.0031(18) 0.0109(17) C5 0.055(2) 0.047(2) 0.0393(19) 0.0192(17) 0.0054(17) 0.0118(18) C6 0.0401(19) 0.050(2) 0.0255(15) 0.0075(15) 0.0081(14) 0.0037(16) C7 0.0224(14) 0.0345(16) 0.0226(13) 0.0034(12) 0.0029(11) 0.0001(12) C8 0.0360(17) 0.0370(17) 0.0266(15) -0.0100(13) 0.0047(13) 0.0036(14) C9 0.0337(17) 0.0368(17) 0.0247(14) -0.0020(13) 0.0015(13) 0.0088(14) C10 0.0334(17) 0.0395(18) 0.0265(15) 0.0033(13) 0.0004(13) 0.0072(15) C11 0.053(2) 0.0319(18) 0.054(2) -0.0010(16) -0.0020(18) -0.0079(16) C12 0.0291(16) 0.0297(16) 0.0359(16) 0.0001(14) -0.0050(14) -0.0021(13) C13 0.0344(18) 0.045(2) 0.0351(17) -0.0002(15) 0.0020(14) 0.0063(15) C14 0.0297(16) 0.0300(16) 0.0292(15) -0.0012(13) -0.0001(13) -0.0016(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.016(2) . ? Zn1 O1 2.041(2) . ? Zn1 O4 2.049(2) 13_665 ? Zn1 O3 2.051(2) . ? Zn1 O2 2.052(2) 13_665 ? Zn1 Zn1 2.9778(8) 13_665 ? N1 C1 1.315(4) . ? N1 C2 1.391(4) . ? N2 C1 1.352(3) . ? N2 C7 1.386(4) . ? N2 C8 1.473(4) . ? O1 C12 1.246(4) . ? O2 C12 1.250(4) . ? O2 Zn1 2.052(2) 13_665 ? O3 C14 1.247(4) . ? O4 C14 1.244(4) . ? O4 Zn1 2.049(2) 13_665 ? C1 H1 0.9400 . ? C2 C3 1.387(4) . ? C2 C7 1.395(4) . ? C3 C4 1.378(5) . ? C3 H3 0.9400 . ? C4 C5 1.390(5) . ? C4 H4 0.9400 . ? C5 C6 1.364(5) . ? C5 H5 0.9400 . ? C6 C7 1.391(4) . ? C6 H6 0.9400 . ? C8 C9 1.519(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.522(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C10 1.528(6) 6_664 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.502(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C13 C14 1.511(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 O1 98.76(9) . . ? N1 Zn1 O4 101.68(9) . 13_665 ? O1 Zn1 O4 86.88(11) . 13_665 ? N1 Zn1 O3 99.89(9) . . ? O1 Zn1 O3 88.73(11) . . ? O4 Zn1 O3 158.40(9) 13_665 . ? N1 Zn1 O2 102.72(9) . 13_665 ? O1 Zn1 O2 158.51(9) . 13_665 ? O4 Zn1 O2 89.28(11) 13_665 13_665 ? O3 Zn1 O2 87.10(10) . 13_665 ? N1 Zn1 Zn1 177.73(7) . 13_665 ? O1 Zn1 Zn1 80.03(6) . 13_665 ? O4 Zn1 Zn1 76.37(6) 13_665 13_665 ? O3 Zn1 Zn1 82.03(6) . 13_665 ? O2 Zn1 Zn1 78.52(6) 13_665 13_665 ? C1 N1 C2 105.6(2) . . ? C1 N1 Zn1 126.8(2) . . ? C2 N1 Zn1 127.39(19) . . ? C1 N2 C7 106.7(2) . . ? C1 N2 C8 126.7(3) . . ? C7 N2 C8 126.3(2) . . ? C12 O1 Zn1 127.3(2) . . ? C12 O2 Zn1 128.7(2) . 13_665 ? C14 O3 Zn1 124.2(2) . . ? C14 O4 Zn1 132.0(2) . 13_665 ? N1 C1 N2 113.0(3) . . ? N1 C1 H1 123.5 . . ? N2 C1 H1 123.5 . . ? C3 C2 N1 130.7(3) . . ? C3 C2 C7 120.4(3) . . ? N1 C2 C7 108.9(2) . . ? C4 C3 C2 117.1(3) . . ? C4 C3 H3 121.5 . . ? C2 C3 H3 121.5 . . ? C3 C4 C5 122.1(3) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 117.0(3) . . ? C5 C6 H6 121.5 . . ? C7 C6 H6 121.5 . . ? N2 C7 C6 132.2(3) . . ? N2 C7 C2 105.8(2) . . ? C6 C7 C2 121.9(3) . . ? N2 C8 C9 112.8(2) . . ? N2 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N2 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 116.3(3) . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9B 108.2 . . ? C10 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C10 113.0(3) . 6_664 ? C9 C10 H10A 109.0 . . ? C10 C10 H10A 109.0 6_664 . ? C9 C10 H10B 109.0 . . ? C10 C10 H10B 109.0 6_664 . ? H10A C10 H10B 107.8 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O1 C12 O2 125.2(3) . . ? O1 C12 C11 117.3(3) . . ? O2 C12 C11 117.5(3) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 C14 O3 125.2(3) . . ? O4 C14 C13 117.0(3) . . ? O3 C14 C13 117.8(3) . . ? 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 C9 H9A O4 0.98 2.58 3.533(4) 163.0 8_453 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.377 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.066 #===END