# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Jianhua Lin' _publ_contact_author_address ; Department of Chemistry College of Chemistry and Chemical Engineering Chongqing University Chongqing, 400030 P. R. China ; #======================================================================== _publ_contact_author_email jhlin@cqu.edu.cn _publ_contact_author_fax +86-023-65102316 _publ_contact_author_phone +86-023-65102316 _publ_contact_letter ; Dear Sir, Please consider this CIF submission for publication in CrystEngComm. All authors have seen and approved this submission. Best wishes Jianhua Lin ; loop_ _publ_author_name 'Yun Gong' 'Jian LiLi' 'Jianbo Qin' 'Jian Lin' #======================================================================= data_10030302 _database_code_depnum_ccdc_archive 'CCDC 787900' #TrackingRef '- 10030302.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H20 N4 Ni2 O14' _chemical_formula_weight 849.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P41212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 11.2689(5) _cell_length_b 11.2689(5) _cell_length_c 29.897(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3796.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6789 _cell_measurement_theta_min 3.2705 _cell_measurement_theta_max 27.4372 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5457 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29760 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4362 _reflns_number_gt 3840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.1153P)^2^+15.7396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(5) _refine_ls_number_reflns 4362 _refine_ls_number_parameters 270 _refine_ls_number_restraints 109 _refine_ls_R_factor_all 0.0990 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2490 _refine_ls_wR_factor_gt 0.2414 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.69418(7) -0.06817(8) 0.09390(3) 0.0308(3) Uani 1 1 d . . . N1 N 0.5073(5) -0.0749(8) 0.0960(2) 0.0498(18) Uani 1 1 d . . . N2 N -0.1216(5) -0.0649(7) 0.0929(2) 0.0424(16) Uani 1 1 d . . . O1 O 0.6944(6) 0.1175(5) 0.09338(18) 0.0462(13) Uani 1 1 d . . . O2A O 0.8025(10) 0.2203(8) 0.0407(3) 0.0575(17) Uani 0.70 1 d PU . . O2B O 0.702(2) 0.2594(16) 0.0414(7) 0.055(5) Uani 0.30 1 d P . . O3 O 0.6913(5) -0.0662(6) 0.02544(16) 0.0440(12) Uani 1 1 d . . . O4 O 0.5901(7) -0.1097(7) -0.0347(2) 0.071(2) Uani 1 1 d . . . O5A O 0.4031(17) 0.4031(17) 0.0000 0.075(6) Uani 0.40 2 d SP . . O5B O 0.281(2) 0.224(2) -0.0376(10) 0.075(6) Uani 0.30 1 d P . . O6 O 0.7049(6) -0.2506(5) 0.0917(2) 0.0523(15) Uani 1 1 d . . . O7 O 0.6988(5) -0.0747(5) 0.16277(16) 0.0417(12) Uani 1 1 d . . . O8 O 0.6578(13) 0.6578(13) 0.0000 0.087(7) Uani 0.50 2 d SP . . O9 O 0.595(3) 0.420(3) 0.9781(13) 0.087(7) Uani 0.25 1 d P . . C1 C 0.4460(7) -0.1581(9) 0.0765(4) 0.059(2) Uani 1 1 d U . . H1 H 0.4873 -0.2208 0.0636 0.071 Uiso 1 1 calc R . . C2 C 0.3221(8) -0.1597(10) 0.0737(4) 0.061(2) Uani 1 1 d U . . H2 H 0.2822 -0.2207 0.0592 0.074 Uiso 1 1 calc R . . C3 C 0.2608(7) -0.0662(10) 0.0937(3) 0.061(2) Uani 1 1 d U . . C4 C 0.3272(8) 0.0214(12) 0.1143(4) 0.075(3) Uani 1 1 d U . . H4 H 0.2893 0.0847 0.1283 0.089 Uiso 1 1 calc R . . C5 C 0.4511(8) 0.0149(11) 0.1142(4) 0.072(3) Uani 1 1 d U . . H5 H 0.4947 0.0756 0.1274 0.086 Uiso 1 1 calc R . . C6 C 0.1299(7) -0.0611(10) 0.0930(3) 0.060(2) Uani 1 1 d U . . C7 C 0.0649(9) -0.1171(11) 0.0578(4) 0.072(3) Uani 1 1 d U . . H7 H 0.1037 -0.1531 0.0339 0.087 Uiso 1 1 calc R . . C8 C -0.0573(8) -0.1161(11) 0.0604(4) 0.073(3) Uani 1 1 d U . . H8 H -0.0988 -0.1544 0.0377 0.087 Uiso 1 1 calc R . . C9 C -0.0580(7) -0.0109(9) 0.1260(3) 0.049(2) Uani 1 1 d U . . H9 H -0.0990 0.0284 0.1486 0.059 Uiso 1 1 calc R . . C10 C 0.0665(7) -0.0118(9) 0.1275(3) 0.054(2) Uani 1 1 d U . . H10 H 0.1060 0.0208 0.1519 0.065 Uiso 1 1 calc R . . C11 C 0.5431(11) 0.0687(11) 0.0029(4) 0.072(2) Uani 1 1 d U . . C12 C 0.4387(13) 0.0867(13) -0.0197(4) 0.090(3) Uani 1 1 d U . . H12 H 0.4061 0.0263 -0.0370 0.108 Uiso 1 1 calc R . . C13 C 0.3806(13) 0.1991(14) -0.0164(5) 0.096(3) Uani 1 1 d U . . C14 C 0.4350(13) 0.2960(13) 0.0056(5) 0.098(3) Uani 1 1 d U . . C15 C 0.5427(12) 0.2775(12) 0.0280(5) 0.089(3) Uani 1 1 d U . . H15 H 0.5759 0.3401 0.0439 0.107 Uiso 1 1 calc R . . C16 C 0.6037(11) 0.1660(10) 0.0272(4) 0.072(2) Uani 1 1 d U . . C17 C 0.7079(10) 0.1662(9) 0.0546(3) 0.0580(16) Uani 1 1 d U . . C18 C 0.6103(9) -0.0425(9) -0.0020(3) 0.058(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0211(4) 0.0383(5) 0.0330(4) -0.0039(4) -0.0036(3) 0.0055(4) N1 0.023(3) 0.074(5) 0.052(4) -0.021(5) 0.005(3) -0.002(3) N2 0.013(2) 0.071(4) 0.042(3) -0.012(4) -0.006(2) -0.004(3) O1 0.065(4) 0.041(3) 0.034(3) -0.002(2) -0.017(3) -0.004(3) O2A 0.066(4) 0.057(4) 0.050(3) -0.005(3) 0.001(3) -0.011(3) O2B 0.075(15) 0.022(8) 0.066(13) 0.018(8) -0.017(12) -0.007(10) O3 0.038(3) 0.061(4) 0.033(2) -0.009(3) -0.008(2) -0.011(3) O4 0.077(5) 0.074(5) 0.064(4) -0.024(4) -0.040(4) 0.004(4) O5A 0.060(7) 0.060(7) 0.106(15) 0.029(7) -0.029(7) 0.001(8) O5B 0.060(7) 0.060(7) 0.106(15) 0.029(7) -0.029(7) 0.001(8) O6 0.055(4) 0.044(3) 0.058(4) 0.003(3) -0.015(4) 0.006(3) O7 0.041(3) 0.051(3) 0.033(2) -0.004(2) 0.004(2) 0.011(2) O8 0.056(6) 0.056(6) 0.148(19) -0.037(9) 0.037(9) -0.005(8) O9 0.056(6) 0.056(6) 0.148(19) -0.037(9) 0.037(9) -0.005(8) C1 0.027(4) 0.071(6) 0.078(5) -0.023(5) -0.001(4) 0.006(4) C2 0.028(4) 0.078(5) 0.078(5) -0.036(4) 0.000(4) 0.004(4) C3 0.026(3) 0.090(5) 0.067(4) -0.042(4) -0.004(3) 0.002(4) C4 0.030(4) 0.113(6) 0.081(5) -0.058(5) -0.005(4) 0.008(4) C5 0.026(4) 0.107(7) 0.082(6) -0.062(5) -0.005(4) 0.017(4) C6 0.018(3) 0.096(5) 0.067(4) -0.040(4) -0.001(3) 0.005(3) C7 0.033(4) 0.112(6) 0.071(5) -0.051(5) -0.001(4) 0.006(4) C8 0.032(4) 0.120(8) 0.066(5) -0.056(5) -0.011(4) -0.003(5) C9 0.022(3) 0.074(5) 0.052(4) -0.028(4) -0.001(3) 0.006(4) C10 0.023(3) 0.081(5) 0.058(4) -0.033(4) -0.005(3) 0.007(4) C11 0.088(5) 0.069(5) 0.059(4) -0.008(4) -0.031(4) 0.016(4) C12 0.100(6) 0.091(6) 0.079(5) -0.009(5) -0.045(5) 0.018(6) C13 0.094(7) 0.098(7) 0.096(6) -0.004(6) -0.049(6) 0.019(6) C14 0.095(7) 0.090(7) 0.109(7) 0.003(6) -0.043(6) 0.024(6) C15 0.089(6) 0.077(6) 0.100(6) -0.003(5) -0.036(6) 0.010(5) C16 0.084(5) 0.062(5) 0.069(5) -0.003(4) -0.016(4) 0.010(4) C17 0.067(4) 0.057(4) 0.050(3) -0.006(3) 0.001(3) -0.010(3) C18 0.068(6) 0.058(5) 0.048(4) -0.001(4) -0.020(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 N2 1.365(10) . ? C9 C10 1.403(10) . ? C9 H9 0.9300 . ? C1 N1 1.303(11) . ? C1 C2 1.398(11) . ? C1 H1 0.9300 . ? Ni1 O3 2.047(5) . ? Ni1 O7 2.061(5) . ? Ni1 O6 2.060(6) . ? Ni1 N2 2.077(5) 1_655 ? Ni1 O1 2.093(6) . ? Ni1 N1 2.108(6) . ? O3 C18 1.255(11) . ? O1 C17 1.292(11) . ? N2 C8 1.342(11) . ? N2 Ni1 2.077(5) 1_455 ? N1 C5 1.313(11) . ? C3 C4 1.384(13) . ? C3 C2 1.394(13) . ? C3 C6 1.477(10) . ? C6 C10 1.373(11) . ? C6 C7 1.429(12) . ? O2A C17 1.297(14) . ? C4 C5 1.398(12) . ? C4 H4 0.9300 . ? C17 O2B 1.12(2) . ? C17 C16 1.432(15) . ? C2 H2 0.9300 . ? C10 H10 0.9300 . ? C18 O4 1.258(11) . ? C18 C11 1.471(15) . ? C5 H5 0.9300 . ? C8 C7 1.379(13) . ? C8 H8 0.9300 . ? C11 C12 1.371(15) . ? C11 C16 1.482(16) . ? C7 H7 0.9300 . ? C16 C15 1.432(17) . ? C12 C13 1.429(19) . ? C12 H12 0.9300 . ? C15 C14 1.402(17) . ? C15 H15 0.9300 . ? O5A C14 1.271(19) 7 ? O5A C14 1.271(19) . ? O5B C13 1.32(3) . ? C14 C13 1.415(19) . ? 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 N2 C9 C10 123.0(7) . . ? N2 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? N1 C1 C2 124.5(9) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? O3 Ni1 O7 178.5(2) . . ? O3 Ni1 O6 88.9(3) . . ? O7 Ni1 O6 89.7(2) . . ? O3 Ni1 N2 90.1(2) . 1_655 ? O7 Ni1 N2 89.4(2) . 1_655 ? O6 Ni1 N2 87.6(3) . 1_655 ? O3 Ni1 O1 88.9(2) . . ? O7 Ni1 O1 92.5(2) . . ? O6 Ni1 O1 175.9(3) . . ? N2 Ni1 O1 88.9(3) 1_655 . ? O3 Ni1 N1 90.8(3) . . ? O7 Ni1 N1 89.7(3) . . ? O6 Ni1 N1 91.4(3) . . ? N2 Ni1 N1 178.7(3) 1_655 . ? O1 Ni1 N1 92.1(3) . . ? C18 O3 Ni1 131.8(6) . . ? C17 O1 Ni1 115.6(6) . . ? C8 N2 C9 115.6(6) . . ? C8 N2 Ni1 122.9(5) . 1_455 ? C9 N2 Ni1 121.5(5) . 1_455 ? C1 N1 C5 119.0(7) . . ? C1 N1 Ni1 122.9(6) . . ? C5 N1 Ni1 117.8(6) . . ? C4 C3 C2 117.5(8) . . ? C4 C3 C6 121.3(8) . . ? C2 C3 C6 121.2(8) . . ? C10 C6 C7 117.8(8) . . ? C10 C6 C3 121.6(8) . . ? C7 C6 C3 120.4(8) . . ? C3 C4 C5 120.1(9) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? O2B C17 O1 134.9(15) . . ? O2B C17 O2A 59.8(14) . . ? O1 C17 O2A 125.8(10) . . ? O2B C17 C16 75.5(14) . . ? O1 C17 C16 114.7(10) . . ? O2A C17 C16 119.4(10) . . ? C3 C2 C1 117.3(9) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? C6 C10 C9 119.9(7) . . ? C6 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? O3 C18 O4 120.7(10) . . ? O3 C18 C11 119.4(9) . . ? O4 C18 C11 119.8(9) . . ? N1 C5 C4 121.6(9) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? N2 C8 C7 125.8(8) . . ? N2 C8 H8 117.1 . . ? C7 C8 H8 117.1 . . ? C12 C11 C18 121.3(11) . . ? C12 C11 C16 121.8(11) . . ? C18 C11 C16 116.1(9) . . ? C8 C7 C6 117.7(8) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C15 C16 C17 112.5(10) . . ? C15 C16 C11 115.8(11) . . ? C17 C16 C11 131.3(10) . . ? C11 C12 C13 119.4(12) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C15 C16 122.6(13) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C14 O5A C14 124(3) 7 . ? O5A C14 C13 123.3(14) . . ? O5A C14 C15 116.7(16) . . ? C13 C14 C15 118.9(13) . . ? O5B C13 C14 115.3(17) . . ? O5B C13 C12 123.1(17) . . ? C14 C13 C12 121.1(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.239 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.132 #===END data_10030401 _database_code_depnum_ccdc_archive 'CCDC 787901' #TrackingRef '- 10030302.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H64 Cu4 N8 O40' _chemical_formula_weight 2319.83 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.412(13) _cell_length_b 9.512(5) _cell_length_c 29.262(13) _cell_angle_alpha 90.00 _cell_angle_beta 126.59(3) _cell_angle_gamma 90.00 _cell_volume 4785(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11211 _cell_measurement_theta_min 3.0113 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6040 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrysAlis RED(Oxford Diffraction 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur/Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29275 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8413 _reflns_number_gt 7202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD(Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED(Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED(Oxford Diffraction, 2009)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'publCIF (Westrip, 2010)' _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^)+(0.1271P)^2^+12.5805P] 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 8413 _refine_ls_number_parameters 694 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.2385 _refine_ls_wR_factor_gt 0.2270 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.107 _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 Cu1 Cu 0.20531(4) 0.10602(7) 0.21167(3) 0.0510(2) Uani 1 1 d U . . Cu2 Cu 0.22519(4) 0.41823(7) 0.26156(3) 0.0472(2) Uani 1 1 d . . . N1 N 0.3011(3) 0.5780(5) 0.3016(3) 0.0633(13) Uani 1 1 d U . . N2 N 0.2462(3) 0.4077(5) 0.3375(2) 0.0524(12) Uani 1 1 d . . . N3 N 0.1199(3) -0.0241(5) 0.1557(2) 0.0535(12) Uani 1 1 d . . . N4 N 0.2046(3) -0.0208(5) 0.2656(2) 0.0503(11) Uani 1 1 d . . . O1 O 0.2956(4) 0.8750(6) 0.1068(2) 0.0943(19) Uani 1 1 d . . . O2 O 0.2918(3) 0.8263(6) 0.0326(2) 0.0863(16) Uani 1 1 d . . . O3 O 0.3039(4) 0.6219(9) -0.0076(2) 0.116(2) Uani 1 1 d . . . H3 H 0.3017 0.6925 0.0076 0.174 Uiso 1 1 calc R . . O4 O 0.3520(5) 0.4110(8) 0.0166(3) 0.127(3) Uani 1 1 d . . . O5 O 0.4831(3) 0.5898(5) 0.26418(19) 0.0752(15) Uani 1 1 d . . . O6 O 0.2919(2) 0.2241(4) 0.26976(17) 0.0535(10) Uani 1 1 d . . . O7 O 0.3778(4) 0.0797(5) 0.2784(3) 0.099(2) Uani 1 1 d . . . O8 O 0.4191(3) 0.1529(6) 0.3956(2) 0.0862(7) Uani 1 1 d U . . H8 H 0.4246 0.1122 0.4225 0.129 Uiso 1 1 calc R . . O9 O 0.5225(3) 0.2577(6) 0.4657(2) 0.0862(7) Uani 1 1 d . . . O10 O -0.3139(3) 0.7969(6) -0.1450(2) 0.0862(7) Uani 1 1 d . . . O11 O -0.2283(3) 0.8905(6) -0.0624(2) 0.0862(7) Uani 1 1 d U . . H11 H -0.2556 0.9605 -0.0775 0.129 Uiso 1 1 calc R . . O12 O -0.1867(2) 0.7657(4) -0.15246(17) 0.0539(10) Uani 1 1 d . . . O13 O -0.2060(3) 0.5465(4) -0.18834(18) 0.0569(10) Uani 1 1 d . . . O14 O -0.0975(3) 0.2762(4) -0.00693(15) 0.0564(11) Uani 1 1 d . . . O15 O 0.0564(3) 0.4547(4) 0.20787(18) 0.0571(10) Uani 1 1 d . . . O16 O 0.13782(19) 0.2850(4) 0.22518(14) 0.0471(8) Uani 1 1 d U . . O17 O -0.0482(3) -0.0126(5) 0.2045(2) 0.0787(15) Uani 1 1 d . . . H17 H -0.0356 -0.0312 0.2363 0.118 Uiso 1 1 calc R . . O18 O 0.0333(3) 0.1634(5) 0.25062(16) 0.0608(11) Uani 1 1 d . . . O19 O 0.2762(4) -0.0735(8) 0.1920(3) 0.114(2) Uani 1 1 d . . . O20 O 0.9021(8) 0.5846(16) 0.1307(5) 0.107(4) Uani 0.50 1 d P . . O21 O 0.4176(6) 0.0192(12) 0.4696(4) 0.081(3) Uani 0.50 1 d P . . C1 C 0.3613(3) 0.6704(6) 0.1138(2) 0.0462(12) Uani 1 1 d . . . C2 C 0.3973(3) 0.6735(6) 0.1714(2) 0.0493(13) Uani 1 1 d . . . H2 H 0.3899 0.7510 0.1870 0.059 Uiso 1 1 calc R . . C3 C 0.4434(3) 0.5672(6) 0.2062(2) 0.0513(14) Uani 1 1 d . . . C4 C 0.4537(4) 0.4494(7) 0.1846(3) 0.0695(19) Uani 1 1 d . . . H4 H 0.4840 0.3750 0.2081 0.083 Uiso 1 1 calc R . . C5 C 0.4188(4) 0.4443(7) 0.1281(4) 0.0695(19) Uani 1 1 d . . . H5 H 0.4258 0.3642 0.1134 0.083 Uiso 1 1 calc R . . C6 C 0.3730(4) 0.5521(7) 0.0907(3) 0.0566(14) Uani 1 1 d . . . C7 C 0.3119(4) 0.7993(7) 0.0820(3) 0.0610(16) Uani 1 1 d . . . C8 C 0.3419(6) 0.5253(11) 0.0300(4) 0.089(3) Uani 1 1 d . . . C9 C 0.4781(3) 0.4951(6) 0.2974(2) 0.0512(13) Uani 1 1 d . . . C10 C 0.5309(4) 0.5183(7) 0.3549(3) 0.0589(15) Uani 1 1 d . . . H10 H 0.5683 0.5884 0.3686 0.071 Uiso 1 1 calc R . . C11 C 0.5271(4) 0.4358(7) 0.3915(3) 0.0586(15) Uani 1 1 d . . . H11A H 0.5626 0.4508 0.4305 0.070 Uiso 1 1 calc R . . C12 C 0.4717(3) 0.3301(6) 0.3721(2) 0.0498(13) Uani 1 1 d . . . C13 C 0.4195(3) 0.3071(5) 0.3135(2) 0.0419(11) Uani 1 1 d . . . C14 C 0.4234(3) 0.3898(5) 0.2759(2) 0.0462(12) Uani 1 1 d . . . H14 H 0.3896 0.3739 0.2369 0.055 Uiso 1 1 calc R . . C15 C 0.4714(4) 0.2460(7) 0.4142(3) 0.0614(16) Uani 1 1 d U . . C16 C 0.3603(3) 0.1924(6) 0.2867(2) 0.0466(12) Uani 1 1 d . . . C17 C -0.2561(4) 0.7890(8) -0.0985(3) 0.0725(9) Uani 1 1 d U . . C18 C -0.2085(4) 0.6583(8) -0.0729(3) 0.0644(10) Uani 1 1 d U . . C19 C -0.1952(3) 0.6074(6) -0.0226(2) 0.0502(13) Uani 1 1 d . . . H19 H -0.2116 0.6597 -0.0047 0.060 Uiso 1 1 calc R . . C20 C -0.1580(3) 0.4807(6) 0.0003(2) 0.0478(13) Uani 1 1 d . . . H20 H -0.1493 0.4471 0.0335 0.057 Uiso 1 1 calc R . . C21 C -0.1340(3) 0.4047(5) -0.0265(2) 0.0435(12) Uani 1 1 d . . . C22 C -0.1483(3) 0.4521(6) -0.0771(2) 0.0483(13) Uani 1 1 d . . . H22 H -0.1335 0.3980 -0.0957 0.058 Uiso 1 1 calc R . . C23 C -0.1847(3) 0.5804(6) -0.0995(2) 0.0439(12) Uani 1 1 d . . . C24 C -0.1937(3) 0.6341(6) -0.1516(2) 0.0465(13) Uani 1 1 d . . . C25 C -0.0746(3) 0.2319(6) 0.0460(2) 0.0444(12) Uani 1 1 d . . . C26 C -0.1094(3) 0.1163(6) 0.0490(2) 0.0538(14) Uani 1 1 d . . . H26 H -0.1476 0.0683 0.0162 0.065 Uiso 1 1 calc R . . C27 C -0.0870(3) 0.0715(6) 0.1017(2) 0.0509(13) Uani 1 1 d . . . H27 H -0.1110 -0.0069 0.1040 0.061 Uiso 1 1 calc R . . C28 C -0.0298(3) 0.1408(5) 0.1510(2) 0.0389(11) Uani 1 1 d . . . C29 C 0.0070(3) 0.2557(5) 0.14781(19) 0.0357(10) Uani 1 1 d . . . C30 C -0.0155(3) 0.3013(5) 0.0946(2) 0.0414(11) Uani 1 1 d . . . H30 H 0.0090 0.3780 0.0919 0.050 Uiso 1 1 calc R . . C31 C 0.0708(3) 0.3376(5) 0.1983(2) 0.0386(11) Uani 1 1 d . . . C32 C -0.0102(3) 0.0988(6) 0.2072(2) 0.0444(12) Uani 1 1 d . . . C33 C 0.3230(5) 0.6625(7) 0.2773(5) 0.089(3) Uani 1 1 d . . . H33 H 0.3018 0.6552 0.2390 0.107 Uiso 1 1 calc R . . C34 C 0.3830(5) 0.7692(9) 0.3148(4) 0.088(2) Uani 1 1 d . . . H34 H 0.3972 0.8350 0.2990 0.106 Uiso 1 1 calc R . . C35 C 0.4166(6) 0.7727(10) 0.3698(5) 0.100(3) Uani 1 1 d . . . H35 H 0.4573 0.8349 0.3931 0.120 Uiso 1 1 calc R . . C36 C 0.3921(5) 0.6867(9) 0.3919(4) 0.095(3) Uani 1 1 d . . . H36 H 0.4143 0.6915 0.4305 0.113 Uiso 1 1 calc R . . C37 C 0.3335(4) 0.5896(7) 0.3575(3) 0.0679(17) Uani 1 1 d U . . C38 C 0.3015(4) 0.4958(7) 0.3775(3) 0.0674(17) Uani 1 1 d . . . C39 C 0.3236(5) 0.4918(11) 0.4334(3) 0.098(3) Uani 1 1 d . . . H39 H 0.3615 0.5533 0.4606 0.117 Uiso 1 1 calc R . . C40 C 0.2905(7) 0.4006(12) 0.4477(3) 0.111(4) Uani 1 1 d . . . H40 H 0.3046 0.3991 0.4846 0.133 Uiso 1 1 calc R . . C41 C 0.2356(5) 0.3091(10) 0.4073(3) 0.087(2) Uani 1 1 d . . . H41 H 0.2130 0.2422 0.4165 0.104 Uiso 1 1 calc R . . C42 C 0.2145(4) 0.3188(7) 0.3529(3) 0.0628(16) Uani 1 1 d . . . H42 H 0.1757 0.2592 0.3253 0.075 Uiso 1 1 calc R . . C43 C 0.0819(4) -0.0223(7) 0.0990(3) 0.0635(16) Uani 1 1 d . . . H43 H 0.0932 0.0483 0.0830 0.076 Uiso 1 1 calc R . . C44 C 0.0269(5) -0.1213(9) 0.0639(3) 0.078(2) Uani 1 1 d . . . H44 H 0.0017 -0.1176 0.0248 0.093 Uiso 1 1 calc R . . C45 C 0.0094(5) -0.2255(8) 0.0870(4) 0.079(2) Uani 1 1 d . . . H45 H -0.0283 -0.2924 0.0637 0.095 Uiso 1 1 calc R . . C46 C 0.0485(4) -0.2295(7) 0.1448(4) 0.0726(19) Uani 1 1 d . . . H46 H 0.0379 -0.2999 0.1613 0.087 Uiso 1 1 calc R . . C47 C 0.1043(3) -0.1269(6) 0.1787(3) 0.0526(14) Uani 1 1 d . . . C48 C 0.1494(3) -0.1195(6) 0.2412(3) 0.0524(14) Uani 1 1 d . . . C49 C 0.1360(4) -0.2025(8) 0.2727(3) 0.075(2) Uani 1 1 d . . . H49 H 0.0966 -0.2695 0.2552 0.090 Uiso 1 1 calc R . . C50 C 0.1816(5) -0.1851(9) 0.3306(4) 0.083(2) Uani 1 1 d . . . H50 H 0.1735 -0.2413 0.3527 0.100 Uiso 1 1 calc R . . C51 C 0.2382(4) -0.0867(9) 0.3558(3) 0.075(2) Uani 1 1 d . . . H51 H 0.2696 -0.0741 0.3950 0.090 Uiso 1 1 calc R . . C52 C 0.2483(4) -0.0055(8) 0.3216(3) 0.0646(17) Uani 1 1 d . . . H52 H 0.2872 0.0625 0.3384 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0410(4) 0.0490(4) 0.0572(4) 0.0202(3) 0.0261(3) 0.0006(3) Cu2 0.0484(4) 0.0461(4) 0.0477(4) 0.0097(3) 0.0289(3) -0.0004(3) N1 0.062(3) 0.038(2) 0.105(4) 0.006(3) 0.058(3) 0.004(2) N2 0.045(3) 0.054(3) 0.045(3) -0.002(2) 0.020(2) -0.003(2) N3 0.061(3) 0.046(3) 0.069(3) 0.002(2) 0.047(3) 0.004(2) N4 0.041(2) 0.049(3) 0.063(3) 0.022(2) 0.032(2) 0.007(2) O1 0.126(5) 0.059(3) 0.077(3) 0.012(3) 0.049(3) 0.043(3) O2 0.085(4) 0.092(4) 0.057(3) 0.029(3) 0.029(3) 0.018(3) O3 0.145(6) 0.147(6) 0.059(3) -0.007(4) 0.062(4) 0.010(5) O4 0.185(8) 0.109(5) 0.134(6) -0.058(5) 0.120(6) -0.025(5) O5 0.070(3) 0.060(3) 0.052(2) 0.014(2) 0.012(2) -0.029(2) O6 0.0336(19) 0.049(2) 0.067(2) 0.0163(19) 0.0240(18) 0.0031(16) O7 0.113(5) 0.046(3) 0.177(7) -0.021(3) 0.107(5) -0.016(3) O8 0.0862(16) 0.0814(16) 0.0539(12) 0.0050(11) 0.0217(11) -0.0065(13) O9 0.0862(16) 0.0814(16) 0.0539(12) 0.0050(11) 0.0217(11) -0.0065(13) O10 0.0862(16) 0.0814(16) 0.0539(12) 0.0050(11) 0.0217(11) -0.0065(13) O11 0.0862(16) 0.0814(16) 0.0539(12) 0.0050(11) 0.0217(11) -0.0065(13) O12 0.062(2) 0.050(2) 0.060(2) 0.0135(19) 0.041(2) 0.0045(19) O13 0.079(3) 0.049(2) 0.056(2) 0.0152(19) 0.048(2) 0.009(2) O14 0.080(3) 0.050(2) 0.0375(19) 0.0142(17) 0.034(2) 0.027(2) O15 0.065(3) 0.047(2) 0.057(2) -0.0046(19) 0.035(2) 0.007(2) O16 0.0365(18) 0.062(2) 0.0367(17) 0.0082(16) 0.0187(15) -0.0032(15) O17 0.113(4) 0.072(3) 0.060(3) -0.002(2) 0.056(3) -0.035(3) O18 0.069(3) 0.077(3) 0.040(2) 0.001(2) 0.034(2) -0.017(2) O19 0.107(5) 0.129(6) 0.118(5) 0.031(4) 0.072(4) 0.031(4) O20 0.091(8) 0.156(13) 0.077(7) -0.006(7) 0.052(7) 0.017(8) O21 0.081(6) 0.097(8) 0.096(7) 0.055(6) 0.070(6) 0.021(6) C1 0.049(3) 0.039(3) 0.048(3) 0.001(2) 0.027(2) -0.001(2) C2 0.053(3) 0.039(3) 0.049(3) 0.002(2) 0.027(3) -0.002(2) C3 0.042(3) 0.042(3) 0.054(3) 0.009(2) 0.020(3) -0.009(2) C4 0.058(4) 0.048(4) 0.092(5) 0.019(4) 0.039(4) 0.008(3) C5 0.076(4) 0.042(3) 0.105(6) -0.007(4) 0.062(5) 0.003(3) C6 0.059(3) 0.054(3) 0.066(4) -0.009(3) 0.042(3) -0.007(3) C7 0.062(4) 0.053(4) 0.054(3) 0.007(3) 0.027(3) 0.006(3) C8 0.108(7) 0.095(6) 0.090(6) -0.032(5) 0.074(6) -0.024(5) C9 0.045(3) 0.040(3) 0.053(3) 0.012(2) 0.021(3) 0.000(2) C10 0.050(3) 0.050(3) 0.051(3) 0.000(3) 0.016(3) -0.009(3) C11 0.054(3) 0.058(4) 0.046(3) -0.005(3) 0.020(3) -0.009(3) C12 0.043(3) 0.054(3) 0.047(3) 0.002(3) 0.023(2) 0.000(2) C13 0.032(2) 0.038(3) 0.047(3) 0.007(2) 0.019(2) 0.004(2) C14 0.034(3) 0.040(3) 0.045(3) 0.002(2) 0.012(2) -0.003(2) C15 0.063(4) 0.068(4) 0.045(3) -0.001(3) 0.029(3) -0.005(3) C16 0.045(3) 0.040(3) 0.053(3) 0.012(2) 0.028(2) 0.002(2) C17 0.0790(17) 0.0756(18) 0.0473(13) 0.0038(13) 0.0292(13) -0.0047(14) C18 0.0746(19) 0.0721(19) 0.0437(15) 0.0040(15) 0.0336(14) -0.0041(16) C19 0.058(3) 0.049(3) 0.039(3) 0.003(2) 0.027(3) 0.014(3) C20 0.058(3) 0.048(3) 0.034(2) 0.007(2) 0.025(2) 0.008(3) C21 0.046(3) 0.043(3) 0.037(3) 0.013(2) 0.022(2) 0.014(2) C22 0.054(3) 0.050(3) 0.048(3) 0.010(2) 0.034(3) 0.012(3) C23 0.043(3) 0.042(3) 0.042(3) 0.012(2) 0.023(2) 0.004(2) C24 0.037(3) 0.051(3) 0.053(3) 0.021(3) 0.027(2) 0.009(2) C25 0.057(3) 0.039(3) 0.032(2) 0.010(2) 0.024(2) 0.016(2) C26 0.052(3) 0.054(3) 0.038(3) 0.001(2) 0.018(3) 0.005(3) C27 0.051(3) 0.050(3) 0.047(3) 0.003(2) 0.027(3) -0.006(3) C28 0.041(3) 0.039(3) 0.036(2) 0.007(2) 0.023(2) 0.005(2) C29 0.035(2) 0.038(3) 0.036(2) 0.008(2) 0.022(2) 0.012(2) C30 0.048(3) 0.038(3) 0.038(3) 0.010(2) 0.026(2) 0.009(2) C31 0.043(3) 0.043(3) 0.037(2) 0.010(2) 0.028(2) 0.007(2) C32 0.047(3) 0.046(3) 0.046(3) 0.008(2) 0.031(3) 0.004(2) C33 0.112(6) 0.041(4) 0.152(8) 0.008(4) 0.099(7) 0.005(4) C34 0.086(5) 0.066(5) 0.115(7) 0.011(5) 0.061(5) -0.021(4) C35 0.117(8) 0.078(6) 0.114(8) -0.021(5) 0.073(7) -0.022(5) C36 0.098(6) 0.082(6) 0.120(7) -0.039(5) 0.074(6) -0.033(5) C37 0.065(4) 0.051(3) 0.088(4) -0.014(3) 0.045(3) 0.001(3) C38 0.055(4) 0.058(4) 0.074(4) -0.013(3) 0.030(3) -0.004(3) C39 0.089(6) 0.118(8) 0.049(4) -0.031(5) 0.020(4) -0.012(5) C40 0.141(9) 0.122(8) 0.046(4) -0.003(5) 0.042(5) -0.020(7) C41 0.103(6) 0.093(6) 0.047(4) 0.005(4) 0.035(4) -0.008(5) C42 0.071(4) 0.065(4) 0.043(3) 0.002(3) 0.029(3) -0.009(3) C43 0.078(4) 0.061(4) 0.065(4) -0.003(3) 0.051(4) -0.003(3) C44 0.090(5) 0.076(5) 0.069(4) -0.018(4) 0.049(4) 0.003(4) C45 0.087(5) 0.060(4) 0.089(5) -0.020(4) 0.051(5) -0.012(4) C46 0.075(4) 0.044(3) 0.110(6) 0.003(4) 0.062(4) -0.006(3) C47 0.055(3) 0.038(3) 0.076(4) 0.004(3) 0.045(3) 0.002(3) C48 0.052(3) 0.041(3) 0.078(4) 0.016(3) 0.046(3) 0.007(2) C49 0.075(4) 0.074(5) 0.089(5) 0.022(4) 0.056(4) -0.006(4) C50 0.083(5) 0.090(6) 0.098(6) 0.038(5) 0.066(5) 0.007(4) C51 0.065(4) 0.092(6) 0.067(4) 0.032(4) 0.040(4) 0.009(4) C52 0.051(3) 0.072(4) 0.068(4) 0.029(3) 0.034(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu2 O13 1.955(4) 3_565 ? Cu2 O16 1.966(4) . ? Cu2 N2 1.989(5) . ? Cu2 N1 2.013(6) . ? Cu2 O6 2.258(4) . ? Cu2 Cu1 3.2235(18) . ? Cu1 O12 1.956(4) 3_565 ? Cu1 O6 1.957(4) . ? Cu1 N4 1.994(4) . ? Cu1 N3 1.997(5) . ? Cu1 O16 2.414(4) . ? Cu1 O19 2.566(7) . ? O1 C7 1.214(8) . ? O2 C7 1.264(8) . ? O5 C9 1.376(7) . ? O5 C3 1.389(8) . ? O9 C15 1.232(7) . ? O8 C15 1.269(8) . ? O8 H8 0.8200 . ? O7 C16 1.206(7) . ? O6 C16 1.273(6) . ? O12 C24 1.263(7) . ? O12 Cu1 1.956(4) 3_565 ? O13 C24 1.257(7) . ? O13 Cu2 1.955(4) 3_565 ? O10 C17 1.174(8) . ? O11 C17 1.286(9) . ? O11 H11 0.8200 . ? O15 C31 1.231(6) . ? O16 C31 1.259(6) . ? O14 C21 1.378(6) . ? O14 C25 1.382(6) . ? O17 C32 1.309(7) . ? O17 H17 0.8200 . ? O18 C32 1.203(7) . ? O4 C8 1.219(10) . ? O3 C8 1.285(12) . ? O3 H3 0.8200 . ? N3 C47 1.338(8) . ? N3 C43 1.343(8) . ? N4 C52 1.324(8) . ? N4 C48 1.334(8) . ? N2 C42 1.320(8) . ? N2 C38 1.351(8) . ? N1 C33 1.329(9) . ? N1 C37 1.347(10) . ? C1 C2 1.375(8) . ? C1 C6 1.411(8) . ? C1 C7 1.521(8) . ? C2 C3 1.354(8) . ? C2 H2 0.9300 . ? C3 C4 1.368(10) . ? C4 C5 1.348(11) . ? C4 H4 0.9300 . ? C5 C6 1.390(10) . ? C5 H5 0.9300 . ? C6 C8 1.499(10) . ? C9 C10 1.376(8) . ? C9 C14 1.374(8) . ? C10 C11 1.369(9) . ? C10 H10 0.9300 . ? C11 C12 1.393(8) . ? C11 H11A 0.9300 . ? C12 C13 1.397(7) . ? C12 C15 1.470(8) . ? C13 C14 1.397(8) . ? C13 C16 1.492(7) . ? C14 H14 0.9300 . ? C37 C36 1.391(11) . ? C37 C38 1.445(11) . ? C36 C35 1.329(13) . ? C36 H36 0.9300 . ? C35 C34 1.316(12) . ? C35 H35 0.9300 . ? C34 C33 1.485(12) . ? C34 H34 0.9300 . ? C33 H33 0.9300 . ? C38 C39 1.406(11) . ? C39 C40 1.336(14) . ? C39 H39 0.9300 . ? C40 C41 1.372(13) . ? C40 H40 0.9300 . ? C41 C42 1.376(9) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C52 C51 1.379(9) . ? C52 H52 0.9300 . ? C51 C50 1.351(11) . ? C51 H51 0.9300 . ? C50 C49 1.370(11) . ? C50 H50 0.9300 . ? C49 C48 1.369(8) . ? C49 H49 0.9300 . ? C48 C47 1.474(9) . ? C47 C46 1.397(9) . ? C46 C45 1.370(11) . ? C46 H46 0.9300 . ? C45 C44 1.371(11) . ? C45 H45 0.9300 . ? C44 C43 1.374(10) . ? C44 H44 0.9300 . ? C43 H43 0.9300 . ? C29 C28 1.384(7) . ? C29 C30 1.395(6) . ? C29 C31 1.500(7) . ? C28 C27 1.383(8) . ? C28 C32 1.489(7) . ? C27 C26 1.381(8) . ? C27 H27 0.9300 . ? C26 C25 1.361(8) . ? C26 H26 0.9300 . ? C25 C30 1.383(8) . ? C30 H30 0.9300 . ? C21 C20 1.373(8) . ? C21 C22 1.396(7) . ? C20 C19 1.378(8) . ? C20 H20 0.9300 . ? C19 C18 1.408(8) . ? C19 H19 0.9300 . ? C18 C23 1.374(9) . ? C18 C17 1.495(10) . ? C23 C22 1.385(7) . ? C23 C24 1.508(7) . ? C22 H22 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Cu2 O16 90.40(17) 3_565 . ? O13 Cu2 N2 172.97(19) 3_565 . ? O16 Cu2 N2 94.63(17) . . ? O13 Cu2 N1 94.4(2) 3_565 . ? O16 Cu2 N1 168.28(19) . . ? N2 Cu2 N1 79.7(2) . . ? O13 Cu2 O6 87.90(16) 3_565 . ? O16 Cu2 O6 82.41(15) . . ? N2 Cu2 O6 97.63(18) . . ? N1 Cu2 O6 108.40(18) . . ? O13 Cu2 Cu1 77.12(13) 3_565 . ? O16 Cu2 Cu1 48.31(12) . . ? N2 Cu2 Cu1 109.90(14) . . ? N1 Cu2 Cu1 143.31(15) . . ? O6 Cu2 Cu1 36.78(10) . . ? O12 Cu1 O6 89.94(17) 3_565 . ? O12 Cu1 N4 170.00(17) 3_565 . ? O6 Cu1 N4 96.32(19) . . ? O12 Cu1 N3 93.2(2) 3_565 . ? O6 Cu1 N3 176.55(19) . . ? N4 Cu1 N3 80.7(2) . . ? O12 Cu1 O16 83.06(15) 3_565 . ? O6 Cu1 O16 78.61(15) . . ? N4 Cu1 O16 90.51(17) . . ? N3 Cu1 O16 103.09(17) . . ? O12 Cu1 O19 93.0(2) 3_565 . ? O6 Cu1 O19 101.3(2) . . ? N4 Cu1 O19 93.4(2) . . ? N3 Cu1 O19 77.2(2) . . ? O16 Cu1 O19 176.08(17) . . ? O12 Cu1 Cu2 74.26(13) 3_565 . ? O6 Cu1 Cu2 43.70(11) . . ? N4 Cu1 Cu2 105.07(16) . . ? N3 Cu1 Cu2 138.72(14) . . ? O16 Cu1 Cu2 37.46(9) . . ? O19 Cu1 Cu2 141.12(18) . . ? C9 O5 C3 120.9(4) . . ? C15 O8 H8 109.5 . . ? C16 O6 Cu1 118.5(4) . . ? C16 O6 Cu2 138.1(4) . . ? Cu1 O6 Cu2 99.52(15) . . ? C24 O12 Cu1 132.2(4) . 3_565 ? C24 O13 Cu2 128.5(4) . 3_565 ? C17 O11 H11 109.5 . . ? C31 O16 Cu2 116.4(4) . . ? C31 O16 Cu1 138.6(3) . . ? Cu2 O16 Cu1 94.24(14) . . ? C21 O14 C25 118.1(4) . . ? C32 O17 H17 109.5 . . ? C8 O3 H3 109.5 . . ? C47 N3 C43 118.9(6) . . ? C47 N3 Cu1 114.9(4) . . ? C43 N3 Cu1 126.1(4) . . ? C52 N4 C48 119.2(5) . . ? C52 N4 Cu1 125.4(4) . . ? C48 N4 Cu1 115.1(4) . . ? C42 N2 C38 117.7(6) . . ? C42 N2 Cu2 126.4(4) . . ? C38 N2 Cu2 115.8(5) . . ? C33 N1 C37 120.5(7) . . ? C33 N1 Cu2 124.4(6) . . ? C37 N1 Cu2 115.0(4) . . ? C2 C1 C6 118.4(5) . . ? C2 C1 C7 114.2(5) . . ? C6 C1 C7 127.4(5) . . ? C3 C2 C1 122.0(6) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 C4 120.7(6) . . ? C2 C3 O5 116.3(6) . . ? C4 C3 O5 122.8(6) . . ? C5 C4 C3 118.1(6) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 C6 123.7(6) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C5 C6 C1 117.0(6) . . ? C5 C6 C8 114.5(7) . . ? C1 C6 C8 128.5(7) . . ? O1 C7 O2 122.8(6) . . ? O1 C7 C1 117.1(6) . . ? O2 C7 C1 120.1(6) . . ? O5 C9 C10 113.9(5) . . ? O5 C9 C14 123.9(5) . . ? C10 C9 C14 122.1(5) . . ? C11 C10 C9 118.5(6) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 121.9(6) . . ? C10 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C11 C12 C13 118.5(5) . . ? C11 C12 C15 118.6(5) . . ? C13 C12 C15 122.9(5) . . ? C12 C13 C14 120.0(5) . . ? C12 C13 C16 124.6(5) . . ? C14 C13 C16 115.3(5) . . ? C9 C14 C13 119.0(5) . . ? C9 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? O9 C15 O8 120.1(6) . . ? O9 C15 C12 122.1(6) . . ? O8 C15 C12 117.6(5) . . ? O7 C16 O6 123.7(6) . . ? O7 C16 C13 119.2(5) . . ? O6 C16 C13 116.8(5) . . ? N1 C37 C36 121.6(8) . . ? N1 C37 C38 114.5(6) . . ? C36 C37 C38 123.9(8) . . ? C35 C36 C37 120.2(9) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C34 C35 C36 119.6(9) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C34 C33 121.4(8) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? N1 C33 C34 116.5(9) . . ? N1 C33 H33 121.8 . . ? C34 C33 H33 121.8 . . ? N2 C38 C39 120.3(7) . . ? N2 C38 C37 114.5(7) . . ? C39 C38 C37 125.2(7) . . ? C40 C39 C38 120.6(8) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 118.9(8) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C40 C41 C42 118.4(8) . . ? C40 C41 H41 120.8 . . ? C42 C41 H41 120.8 . . ? N2 C42 C41 123.9(7) . . ? N2 C42 H42 118.0 . . ? C41 C42 H42 118.0 . . ? N4 C52 C51 122.4(7) . . ? N4 C52 H52 118.8 . . ? C51 C52 H52 118.8 . . ? C50 C51 C52 118.1(7) . . ? C50 C51 H51 121.0 . . ? C52 C51 H51 121.0 . . ? C51 C50 C49 120.3(6) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C48 C49 C50 118.8(7) . . ? C48 C49 H49 120.6 . . ? C50 C49 H49 120.6 . . ? N4 C48 C49 121.3(6) . . ? N4 C48 C47 114.4(5) . . ? C49 C48 C47 124.2(6) . . ? N3 C47 C46 121.1(6) . . ? N3 C47 C48 114.5(5) . . ? C46 C47 C48 124.4(6) . . ? C45 C46 C47 119.5(7) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C46 C45 C44 118.9(7) . . ? C46 C45 H45 120.6 . . ? C44 C45 H45 120.6 . . ? C43 C44 C45 119.5(7) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? N3 C43 C44 122.2(7) . . ? N3 C43 H43 118.9 . . ? C44 C43 H43 118.9 . . ? C28 C29 C30 119.3(5) . . ? C28 C29 C31 124.3(4) . . ? C30 C29 C31 116.4(4) . . ? C27 C28 C29 119.5(5) . . ? C27 C28 C32 121.1(5) . . ? C29 C28 C32 119.4(5) . . ? C26 C27 C28 121.4(5) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C25 C26 C27 118.9(5) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C26 C25 O14 118.5(5) . . ? C26 C25 C30 121.2(5) . . ? O14 C25 C30 120.3(5) . . ? C25 C30 C29 119.7(5) . . ? C25 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? O15 C31 O16 124.3(5) . . ? O15 C31 C29 119.4(4) . . ? O16 C31 C29 116.0(4) . . ? O18 C32 O17 122.8(5) . . ? O18 C32 C28 124.0(5) . . ? O17 C32 C28 113.1(5) . . ? C20 C21 O14 122.8(5) . . ? C20 C21 C22 121.0(5) . . ? O14 C21 C22 116.1(5) . . ? C21 C20 C19 119.2(5) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C19 C18 120.5(6) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C23 C18 C19 119.7(6) . . ? C23 C18 C17 122.4(5) . . ? C19 C18 C17 117.6(6) . . ? C18 C23 C22 120.1(5) . . ? C18 C23 C24 121.6(5) . . ? C22 C23 C24 118.2(5) . . ? C23 C22 C21 119.6(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? O10 C17 O11 123.7(8) . . ? O10 C17 C18 124.5(7) . . ? O11 C17 C18 111.6(6) . . ? O13 C24 O12 127.4(5) . . ? O13 C24 C23 118.4(5) . . ? O12 C24 C23 114.2(5) . . ? O4 C8 O3 120.4(9) . . ? O4 C8 C6 119.6(10) . . ? O3 C8 C6 120.0(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.702 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.104 #===END data_1002 _database_code_depnum_ccdc_archive 'CCDC 870432' #TrackingRef '- 10030302.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H38 Co3 N6 O30' _chemical_formula_weight 1523.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.6634(5) _cell_length_b 9.0656(2) _cell_length_c 24.3568(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.831(2) _cell_angle_gamma 90.00 _cell_volume 6433.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8112 _cell_measurement_theta_min 2.3481 _cell_measurement_theta_max 28.8584 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3092 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84677 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis RED(Oxford Diffraction 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur/Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14025 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5669 _reflns_number_gt 4326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD(Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED(Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED(Oxford Diffraction, 2009)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'publCIF (Westrip, 2010)' _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^)+(0.0745P)^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 5669 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Co1 Co 0.0000 0.94038(5) 0.2500 0.02494(15) Uani 1 2 d S . . Co2 Co 0.260014(11) 0.54555(4) 0.142120(14) 0.02598(13) Uani 1 1 d . . . N1 N 0.26715(8) 0.4688(3) 0.06097(11) 0.0362(6) Uani 1 1 d . . . N2 N 0.21100(7) 0.6715(3) 0.08600(9) 0.0317(5) Uani 1 1 d . . . N3 N 0.03732(7) 0.7569(2) 0.22702(9) 0.0293(5) Uani 1 1 d . . . O1 O 0.38605(7) 1.2891(3) -0.11168(10) 0.0582(7) Uani 1 1 d . . . O2 O 0.36628(8) 1.0883(3) -0.07321(10) 0.0635(7) Uani 1 1 d . . . O3 O 0.45400(8) 1.4232(3) -0.11404(10) 0.0590(7) Uani 1 1 d . . . H3 H 0.4299 1.3874 -0.1085 0.089 Uiso 1 1 calc R . . O4 O 0.52684(7) 1.4185(3) -0.07562(9) 0.0484(6) Uani 1 1 d . . . O5 O 0.47197(6) 0.9791(2) 0.09907(8) 0.0383(5) Uani 1 1 d . . . O6 O 0.29899(8) 1.1062(3) 0.20971(11) 0.0592(7) Uani 1 1 d . . . O7 O 0.31619(6) 0.8795(2) 0.24112(8) 0.0321(4) Uani 1 1 d . . . O8 O 0.31353(6) 0.6921(2) 0.14020(7) 0.0279(4) Uani 1 1 d . . . O9 O 0.37683(6) 0.5985(2) 0.19305(10) 0.0438(5) Uani 1 1 d . . . O10 O 0.30687(7) 0.3980(2) 0.18787(11) 0.0559(7) Uani 1 1 d . . . O11 O 0.25233(8) 0.6596(3) 0.21440(9) 0.0543(6) Uani 1 1 d . . . O12 O 0.20881(6) 0.3995(2) 0.15568(8) 0.0364(5) Uani 1 1 d . . . O13 O 0.04356(7) 1.1019(2) 0.22586(9) 0.0441(5) Uani 1 1 d . . . O14 O 0.04384(6) 0.9556(2) 0.33037(8) 0.0338(5) Uani 1 1 d . . . O15 O 0.33655(15) 0.4855(4) 0.80792(15) 0.1189(14) Uani 1 1 d . . . C1 C 0.35380(8) 0.7016(3) 0.16650(11) 0.0254(6) Uani 1 1 d . . . C2 C 0.32072(9) 0.9878(3) 0.21086(11) 0.0301(6) Uani 1 1 d . . . C3 C 0.37664(8) 0.8481(3) 0.16168(10) 0.0241(6) Uani 1 1 d . . . C4 C 0.35809(8) 0.9809(3) 0.17624(11) 0.0260(6) Uani 1 1 d . . . C5 C 0.37791(9) 1.1122(3) 0.16270(11) 0.0328(6) Uani 1 1 d . . . H5 H 0.3656 1.2013 0.1719 0.039 Uiso 1 1 calc R . . C6 C 0.41505(10) 1.1143(3) 0.13621(12) 0.0350(7) Uani 1 1 d . . . H6 H 0.4275 1.2033 0.1272 0.042 Uiso 1 1 calc R . . C7 C 0.43324(9) 0.9823(3) 0.12333(11) 0.0292(6) Uani 1 1 d . . . C8 C 0.41488(8) 0.8497(3) 0.13572(11) 0.0266(6) Uani 1 1 d . . . H8 H 0.4279 0.7615 0.1269 0.032 Uiso 1 1 calc R . . C9 C 0.47298(9) 1.0807(3) 0.05658(11) 0.0315(6) Uani 1 1 d . . . C10 C 0.43658(9) 1.0946(3) 0.01299(12) 0.0342(7) Uani 1 1 d . . . H10 H 0.4104 1.0381 0.0130 0.041 Uiso 1 1 calc R . . C11 C 0.43764(9) 1.1908(3) -0.03110(11) 0.0308(6) Uani 1 1 d . . . C12 C 0.47782(8) 1.2746(3) -0.03101(11) 0.0294(6) Uani 1 1 d . . . C13 C 0.51370(9) 1.2572(3) 0.01359(12) 0.0400(7) Uani 1 1 d . . . H13 H 0.5403 1.3120 0.0141 0.048 Uiso 1 1 calc R . . C14 C 0.51203(9) 1.1626(4) 0.05723(12) 0.0407(8) Uani 1 1 d . . . H14 H 0.5369 1.1541 0.0867 0.049 Uiso 1 1 calc R . . C15 C 0.39358(10) 1.1875(4) -0.07475(12) 0.0368(7) Uani 1 1 d . . . C16 C 0.48742(10) 1.3781(3) -0.07615(12) 0.0367(7) Uani 1 1 d . . . C17 C 0.29930(12) 0.3725(4) 0.05123(16) 0.0541(9) Uani 1 1 d . . . H17 H 0.3185 0.3293 0.0815 0.065 Uiso 1 1 calc R . . C18 C 0.30478(15) 0.3357(5) -0.00178(19) 0.0701(12) Uani 1 1 d . . . H18 H 0.3272 0.2683 -0.0072 0.084 Uiso 1 1 calc R . . C19 C 0.27692(16) 0.3995(5) -0.04656(19) 0.0739(13) Uani 1 1 d . . . H19 H 0.2801 0.3753 -0.0827 0.089 Uiso 1 1 calc R . . C20 C 0.24417(14) 0.4993(5) -0.03797(14) 0.0598(10) Uani 1 1 d . . . H20 H 0.2251 0.5440 -0.0680 0.072 Uiso 1 1 calc R . . C21 C 0.24020(10) 0.5323(3) 0.01708(12) 0.0374(7) Uani 1 1 d . . . C22 C 0.20638(9) 0.6394(3) 0.03103(12) 0.0356(7) Uani 1 1 d . . . C23 C 0.17227(11) 0.7031(4) -0.00854(15) 0.0560(10) Uani 1 1 d . . . H23 H 0.1698 0.6806 -0.0462 0.067 Uiso 1 1 calc R . . C24 C 0.14207(12) 0.7999(5) 0.00865(18) 0.0664(12) Uani 1 1 d . . . H24 H 0.1187 0.8425 -0.0174 0.080 Uiso 1 1 calc R . . C25 C 0.14641(11) 0.8331(4) 0.06370(18) 0.0602(10) Uani 1 1 d . . . H25 H 0.1263 0.8985 0.0760 0.072 Uiso 1 1 calc R . . C26 C 0.18181(10) 0.7666(3) 0.10146(14) 0.0453(8) Uani 1 1 d . . . H26 H 0.1851 0.7901 0.1392 0.054 Uiso 1 1 calc R . . C27 C 0.07513(9) 0.7632(4) 0.20416(12) 0.0401(7) Uani 1 1 d . . . H27 H 0.0871 0.8549 0.1976 0.048 Uiso 1 1 calc R . . C28 C 0.09664(11) 0.6374(4) 0.19019(13) 0.0490(9) Uani 1 1 d . . . H28 H 0.1231 0.6449 0.1751 0.059 Uiso 1 1 calc R . . C29 C 0.07909(12) 0.5027(4) 0.19853(13) 0.0459(8) Uani 1 1 d . . . H29 H 0.0929 0.4170 0.1887 0.055 Uiso 1 1 calc R . . C30 C 0.04045(10) 0.4961(3) 0.22184(13) 0.0393(7) Uani 1 1 d . . . H30 H 0.0277 0.4051 0.2278 0.047 Uiso 1 1 calc R . . C31 C 0.02054(9) 0.6234(3) 0.23634(11) 0.0287(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 Co1 0.0248(3) 0.0215(3) 0.0278(3) 0.000 0.0031(2) 0.000 Co2 0.02414(19) 0.0297(2) 0.0238(2) 0.00192(16) 0.00372(15) -0.00434(15) N1 0.0394(13) 0.0354(14) 0.0358(14) -0.0057(12) 0.0118(11) -0.0080(12) N2 0.0282(11) 0.0347(14) 0.0324(14) 0.0042(11) 0.0062(10) -0.0037(11) N3 0.0285(11) 0.0330(13) 0.0262(12) 0.0027(10) 0.0047(10) 0.0036(10) O1 0.0433(12) 0.0701(17) 0.0550(15) 0.0250(14) -0.0065(11) -0.0032(12) O2 0.0471(13) 0.0772(17) 0.0560(15) 0.0189(14) -0.0164(12) -0.0288(14) O3 0.0497(14) 0.0719(17) 0.0541(15) 0.0312(13) 0.0064(12) -0.0056(13) O4 0.0431(12) 0.0557(14) 0.0502(14) 0.0177(11) 0.0187(11) -0.0072(11) O5 0.0293(10) 0.0513(13) 0.0367(12) 0.0141(10) 0.0126(9) -0.0009(10) O6 0.0650(15) 0.0465(14) 0.0797(18) 0.0204(13) 0.0487(14) 0.0222(12) O7 0.0404(10) 0.0307(11) 0.0290(10) -0.0009(9) 0.0164(9) -0.0061(9) O8 0.0241(9) 0.0310(10) 0.0280(10) 0.0016(8) 0.0037(8) -0.0067(8) O9 0.0285(10) 0.0368(11) 0.0652(15) 0.0219(12) 0.0065(10) 0.0027(10) O10 0.0385(11) 0.0408(13) 0.0803(18) 0.0219(13) -0.0098(12) -0.0013(11) O11 0.0667(14) 0.0616(15) 0.0417(13) -0.0203(11) 0.0278(11) -0.0323(12) O12 0.0313(10) 0.0447(12) 0.0329(11) 0.0055(10) 0.0055(9) -0.0126(9) O13 0.0401(11) 0.0396(12) 0.0500(13) 0.0086(11) 0.0017(10) -0.0107(10) O14 0.0340(10) 0.0336(11) 0.0324(11) -0.0048(9) 0.0027(9) 0.0028(9) O15 0.167(4) 0.090(2) 0.082(2) 0.000(2) -0.024(2) -0.005(2) C1 0.0234(13) 0.0284(15) 0.0267(14) 0.0024(12) 0.0106(11) -0.0002(12) C2 0.0318(14) 0.0325(16) 0.0283(15) -0.0022(13) 0.0113(12) 0.0006(13) C3 0.0226(12) 0.0291(14) 0.0194(13) 0.0013(11) 0.0012(10) -0.0017(11) C4 0.0247(13) 0.0324(15) 0.0210(13) 0.0013(12) 0.0046(11) -0.0015(12) C5 0.0429(16) 0.0265(15) 0.0305(15) 0.0002(13) 0.0104(13) -0.0024(13) C6 0.0428(16) 0.0313(16) 0.0317(16) 0.0051(13) 0.0092(13) -0.0117(14) C7 0.0234(13) 0.0433(17) 0.0211(14) 0.0037(13) 0.0044(11) -0.0079(13) C8 0.0256(12) 0.0298(15) 0.0248(14) 0.0001(12) 0.0060(11) -0.0011(12) C9 0.0305(14) 0.0408(17) 0.0252(14) 0.0028(13) 0.0104(12) -0.0032(13) C10 0.0286(14) 0.0440(17) 0.0307(16) 0.0030(14) 0.0073(12) -0.0108(13) C11 0.0295(13) 0.0395(16) 0.0240(14) -0.0026(13) 0.0065(11) -0.0035(13) C12 0.0279(13) 0.0364(16) 0.0258(14) 0.0010(12) 0.0102(11) -0.0013(12) C13 0.0305(14) 0.055(2) 0.0352(17) 0.0071(15) 0.0071(13) -0.0157(14) C14 0.0300(14) 0.057(2) 0.0323(16) 0.0071(15) -0.0003(13) -0.0104(15) C15 0.0321(15) 0.053(2) 0.0257(15) -0.0005(15) 0.0059(12) -0.0018(15) C16 0.0403(16) 0.0404(18) 0.0315(16) 0.0059(14) 0.0126(14) 0.0004(15) C17 0.056(2) 0.043(2) 0.070(2) -0.0113(18) 0.0294(19) -0.0023(17) C18 0.081(3) 0.058(3) 0.087(3) -0.024(2) 0.055(3) -0.012(2) C19 0.101(3) 0.073(3) 0.062(3) -0.029(2) 0.052(3) -0.035(3) C20 0.080(3) 0.070(2) 0.0342(18) -0.0104(18) 0.0226(18) -0.033(2) C21 0.0442(17) 0.0417(18) 0.0268(15) -0.0004(14) 0.0082(13) -0.0170(15) C22 0.0366(15) 0.0407(17) 0.0282(16) 0.0102(14) 0.0029(13) -0.0125(14) C23 0.0477(19) 0.076(3) 0.0397(19) 0.0176(19) -0.0047(16) -0.013(2) C24 0.046(2) 0.083(3) 0.063(3) 0.034(2) -0.0083(19) 0.000(2) C25 0.0386(18) 0.053(2) 0.088(3) 0.020(2) 0.0096(19) 0.0117(17) C26 0.0400(16) 0.0443(19) 0.053(2) 0.0056(16) 0.0121(15) -0.0016(16) C27 0.0384(15) 0.0486(19) 0.0350(17) 0.0060(15) 0.0111(13) 0.0057(15) C28 0.0404(17) 0.074(3) 0.0341(17) 0.0070(17) 0.0113(14) 0.0212(18) C29 0.0508(19) 0.049(2) 0.0358(18) -0.0069(16) 0.0020(15) 0.0183(17) C30 0.0449(17) 0.0310(16) 0.0382(17) -0.0051(14) -0.0018(14) 0.0094(14) C31 0.0321(14) 0.0285(15) 0.0223(14) 0.0001(12) -0.0036(11) 0.0036(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 Co1 O13 2.108(2) . ? Co1 O13 2.108(2) 2 ? Co1 N3 2.131(2) 2 ? Co1 N3 2.131(2) . ? Co1 O14 2.1414(18) 2 ? Co1 O14 2.1414(18) . ? Co2 O8 2.0774(17) . ? Co2 O12 2.0872(18) . ? Co2 O11 2.091(2) . ? Co2 O10 2.093(2) . ? Co2 N2 2.131(2) . ? Co2 N1 2.143(3) . ? C9 C10 1.370(4) . ? C9 C14 1.373(4) . ? C9 O5 1.390(3) . ? O8 C1 1.248(3) . ? O9 C1 1.262(3) . ? C11 C10 1.388(4) . ? C11 C12 1.413(4) . ? C11 C15 1.522(4) . ? O5 C7 1.387(3) . ? N2 C26 1.326(4) . ? N2 C22 1.352(4) . ? O7 C2 1.251(3) . ? O2 C15 1.215(4) . ? N3 C31 1.343(3) . ? N3 C27 1.344(3) . ? O3 C16 1.288(4) . ? O3 H3 0.8200 . ? N1 C21 1.338(4) . ? N1 C17 1.347(4) . ? O4 C16 1.223(3) . ? C12 C13 1.380(4) . ? C12 C16 1.512(4) . ? O1 C15 1.278(4) . ? C1 C3 1.505(4) . ? C3 C4 1.398(4) . ? C3 C8 1.399(3) . ? C7 C6 1.373(4) . ? C7 C8 1.377(4) . ? C2 O6 1.249(3) . ? C2 C4 1.515(4) . ? C4 C5 1.394(4) . ? C8 H8 0.9300 . ? C31 C30 1.373(4) . ? C31 C31 1.494(5) 2 ? C22 C23 1.385(4) . ? C22 C21 1.481(4) . ? C30 C29 1.373(5) . ? C30 H30 0.9300 . ? C6 C5 1.378(4) . ? C6 H6 0.9300 . ? C5 H5 0.9300 . ? C21 C20 1.400(4) . ? C29 C28 1.358(5) . ? C29 H29 0.9300 . ? C28 C27 1.381(4) . ? C28 H28 0.9300 . ? C10 H10 0.9300 . ? C26 C25 1.396(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C17 C18 1.372(5) . ? C17 H17 0.9300 . ? C13 C14 1.374(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C23 C24 1.374(5) . ? C23 H23 0.9300 . ? C20 C19 1.372(6) . ? C20 H20 0.9300 . ? C25 C24 1.356(6) . ? C25 H25 0.9300 . ? C24 H24 0.9300 . ? C19 C18 1.367(6) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Co1 O13 92.03(12) . 2 ? O13 Co1 N3 172.53(9) . 2 ? O13 Co1 N3 95.34(8) 2 2 ? O13 Co1 N3 95.34(8) . . ? O13 Co1 N3 172.53(9) 2 . ? N3 Co1 N3 77.33(12) 2 . ? O13 Co1 O14 89.95(7) . 2 ? O13 Co1 O14 84.93(8) 2 2 ? N3 Co1 O14 91.95(8) 2 2 ? N3 Co1 O14 93.80(8) . 2 ? O13 Co1 O14 84.93(8) . . ? O13 Co1 O14 89.95(7) 2 . ? N3 Co1 O14 93.80(8) 2 . ? N3 Co1 O14 91.95(8) . . ? O14 Co1 O14 172.63(10) 2 . ? O8 Co2 O12 172.32(7) . . ? O8 Co2 O11 84.68(8) . . ? O12 Co2 O11 89.01(8) . . ? O8 Co2 O10 89.25(8) . . ? O12 Co2 O10 86.60(8) . . ? O11 Co2 O10 91.97(10) . . ? O8 Co2 N2 94.30(8) . . ? O12 Co2 N2 90.70(8) . . ? O11 Co2 N2 96.08(10) . . ? O10 Co2 N2 171.47(10) . . ? O8 Co2 N1 88.77(8) . . ? O12 Co2 N1 98.11(8) . . ? O11 Co2 N1 169.24(9) . . ? O10 Co2 N1 96.48(10) . . ? N2 Co2 N1 75.88(9) . . ? C10 C9 C14 119.9(3) . . ? C10 C9 O5 120.9(2) . . ? C14 C9 O5 119.0(2) . . ? C1 O8 Co2 133.98(17) . . ? C10 C11 C12 118.6(2) . . ? C10 C11 C15 112.8(2) . . ? C12 C11 C15 128.7(3) . . ? C7 O5 C9 116.0(2) . . ? C26 N2 C22 118.1(3) . . ? C26 N2 Co2 124.7(2) . . ? C22 N2 Co2 116.74(19) . . ? C31 N3 C27 118.3(2) . . ? C31 N3 Co1 115.54(17) . . ? C27 N3 Co1 126.2(2) . . ? C16 O3 H3 109.5 . . ? C21 N1 C17 118.3(3) . . ? C21 N1 Co2 116.7(2) . . ? C17 N1 Co2 124.7(2) . . ? C13 C12 C11 117.7(3) . . ? C13 C12 C16 114.9(2) . . ? C11 C12 C16 127.3(2) . . ? O8 C1 O9 125.9(2) . . ? O8 C1 C3 115.0(2) . . ? O9 C1 C3 119.0(2) . . ? C4 C3 C8 119.8(2) . . ? C4 C3 C1 122.4(2) . . ? C8 C3 C1 117.4(2) . . ? C6 C7 C8 121.5(2) . . ? C6 C7 O5 120.5(3) . . ? C8 C7 O5 117.9(3) . . ? O6 C2 O7 125.2(3) . . ? O6 C2 C4 116.8(3) . . ? O7 C2 C4 117.8(2) . . ? C5 C4 C3 118.2(2) . . ? C5 C4 C2 118.8(3) . . ? C3 C4 C2 122.7(2) . . ? C7 C8 C3 119.7(3) . . ? C7 C8 H8 120.1 . . ? C3 C8 H8 120.1 . . ? N3 C31 C30 121.5(3) . . ? N3 C31 C31 115.75(14) . 2 ? C30 C31 C31 122.74(18) . 2 ? N2 C22 C23 121.6(3) . . ? N2 C22 C21 114.9(2) . . ? C23 C22 C21 123.5(3) . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C7 C6 C5 118.5(3) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C5 C4 122.2(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N1 C21 C20 121.9(3) . . ? N1 C21 C22 115.3(3) . . ? C20 C21 C22 122.8(3) . . ? C28 C29 C30 118.3(3) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C29 C28 C27 119.9(3) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C9 C10 C11 121.9(3) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? O4 C16 O3 121.2(3) . . ? O4 C16 C12 119.2(3) . . ? O3 C16 C12 119.5(3) . . ? N2 C26 C25 123.0(3) . . ? N2 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? N3 C27 C28 121.8(3) . . ? N3 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? O2 C15 O1 121.7(3) . . ? O2 C15 C11 118.9(3) . . ? O1 C15 C11 119.4(3) . . ? N1 C17 C18 122.4(4) . . ? N1 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C14 C13 C12 123.1(3) . . ? C14 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? C9 C14 C13 118.8(3) . . ? C9 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C24 C23 C22 119.1(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C19 C20 C21 118.4(4) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C24 C25 C26 118.4(4) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C25 C24 C23 119.8(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C18 C19 C20 119.8(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C18 C17 119.2(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.542 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.063 #===END data_120406g _database_code_depnum_ccdc_archive 'CCDC 787896' #TrackingRef '- 10030302.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H62 F2 N6 O23 Zn2' _chemical_formula_weight 1331.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.4400(12) _cell_length_b 20.3899(18) _cell_length_c 19.5001(17) _cell_angle_alpha 90.00 _cell_angle_beta 108.521(2) _cell_angle_gamma 90.00 _cell_volume 5444.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 0.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6578 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12867 _diffrn_reflns_av_R_equivalents 0.1413 _diffrn_reflns_av_sigmaI/netI 0.1721 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4772 _reflns_number_gt 2188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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. Due to a large number of lattice water molecules in the structure, the quality of the crystal is not good enough, so we have used a relatively low number of reflections for this structure (2188 from 4772 unique). We have tried to recollect the crystal data with better crystal, but failed to improve the data. ; _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^)+(0.1245P)^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 4772 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1680 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2534 _refine_ls_wR_factor_gt 0.2055 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.15630(7) 0.52757(5) 0.46184(5) 0.0399(4) Uani 1 1 d . . . F1 F 0.5607(4) 0.4146(3) 0.6942(3) 0.0758(18) Uani 1 1 d . . . N1 N 0.5107(5) 0.6319(4) 0.5267(4) 0.050(2) Uani 1 1 d . . . N2 N 0.7044(5) 0.5052(4) 0.7337(4) 0.056(2) Uani 1 1 d . . . N3 N 0.8667(6) 0.4589(5) 0.8444(5) 0.079(3) Uani 1 1 d . . . H3 H 0.8887 0.4934 0.8739 0.094 Uiso 1 1 d R . . O1 O 0.1133(5) 0.5609(4) 0.5389(3) 0.0577(18) Uani 1 1 d . . . O2 O 0.1942(7) 0.6473(4) 0.5304(5) 0.103(3) Uani 1 1 d . . . H2 H 0.2126 0.6229 0.5039 0.155 Uiso 1 1 calc R . . O3 O -0.0596(5) 0.5286(3) 0.6023(4) 0.0613(18) Uani 1 1 d . . . O4 O -0.1014(6) 0.5903(4) 0.5082(4) 0.081(2) Uani 1 1 d . . . O5 O 0.0000 0.7496(4) 0.7500 0.050(2) Uani 1 2 d S . . O6 O 0.1831(4) 0.5827(3) 0.3915(3) 0.0571(18) Uani 1 1 d . . . O7 O 0.2677(5) 0.6565(4) 0.3580(4) 0.071(2) Uani 1 1 d . . . O8 O 0.2928(4) 0.5015(3) 0.5018(3) 0.0496(16) Uani 1 1 d . . . O9 O 0.6723(5) 0.6226(4) 0.6571(4) 0.075(2) Uani 1 1 d . . . O10 O 0.0946(9) 0.7158(6) 0.2915(7) 0.197(6) Uani 1 1 d . . . H10C H 0.1518 0.6999 0.3088 0.236 Uiso 1 1 d R . . H10D H 0.0587 0.6983 0.3136 0.236 Uiso 1 1 d R . . O11 O 0.9886(8) 0.6500(6) 0.3771(8) 0.217(7) Uani 1 1 d . . . H11C H 1.0448 0.6341 0.3820 0.260 Uiso 1 1 d R . . H11D H 0.9475 0.6187 0.3671 0.260 Uiso 1 1 d R . . O12 O 0.3645(11) 0.7341(8) 0.5644(9) 0.100(7) Uani 0.529(16) 1 d P A 1 H12C H 0.3154 0.7086 0.5543 0.120 Uiso 0.529(16) 1 d PR A 1 H12D H 0.3490 0.7678 0.5375 0.120 Uiso 0.265(8) 1 d PR A 1 H12B H 0.3809 0.7453 0.6086 0.120 Uiso 0.265(8) 1 d PR A 1 O13 O 0.3947(13) 0.6759(9) 0.6344(9) 0.100(8) Uani 0.471(16) 1 d P A 2 H13C H 0.3371 0.6693 0.6061 0.120 Uiso 0.471(16) 1 d PR A 2 H13D H 0.3953 0.7117 0.6569 0.120 Uiso 0.471(16) 1 d PR A 2 C1 C 0.1348(7) 0.6177(5) 0.5538(5) 0.053(3) Uani 1 1 d . . . C2 C -0.0557(7) 0.5787(5) 0.5718(5) 0.048(2) Uani 1 1 d . . . C3 C 0.0929(6) 0.6531(4) 0.6025(4) 0.039(2) Uani 1 1 d . . . C4 C 0.0092(6) 0.6319(4) 0.6151(4) 0.038(2) Uani 1 1 d . . . C5 C -0.0201(6) 0.6633(4) 0.6664(4) 0.039(2) Uani 1 1 d . . . H5 H -0.0746 0.6486 0.6776 0.047 Uiso 1 1 calc R . . C6 C 0.0299(6) 0.7155(4) 0.7007(4) 0.039(2) Uani 1 1 d . . . C7 C 0.1096(6) 0.7375(4) 0.6868(4) 0.043(2) Uani 1 1 d . . . H7 H 0.1428 0.7741 0.7109 0.051 Uiso 1 1 calc R . . C8 C 0.1407(6) 0.7061(4) 0.6380(4) 0.044(2) Uani 1 1 d . . . H8 H 0.1962 0.7210 0.6285 0.053 Uiso 1 1 calc R . . C9 C 0.2604(7) 0.6138(5) 0.3995(5) 0.050(2) Uani 1 1 d . . . C10 C 0.4251(6) 0.6387(5) 0.4737(5) 0.052(2) Uani 1 1 d . . . H10 H 0.4178 0.6746 0.4431 0.062 Uiso 1 1 calc R . . C11 C 0.3495(6) 0.5974(4) 0.4618(5) 0.043(2) Uani 1 1 d . . . C12 C 0.3595(6) 0.5427(4) 0.5058(5) 0.043(2) Uani 1 1 d . . . C13 C 0.4513(5) 0.5339(4) 0.5594(5) 0.040(2) Uani 1 1 d . . . C14 C 0.5247(6) 0.5795(5) 0.5735(5) 0.046(2) Uani 1 1 d . . . C15 C 0.6073(7) 0.5728(5) 0.6343(5) 0.053(3) Uani 1 1 d . . . C16 C 0.6214(6) 0.5167(5) 0.6752(5) 0.050(2) Uani 1 1 d . . . C17 C 0.5488(6) 0.4708(5) 0.6560(5) 0.048(2) Uani 1 1 d . . . C18 C 0.4650(6) 0.4792(5) 0.6027(5) 0.044(2) Uani 1 1 d . . . H18 H 0.4158 0.4479 0.5947 0.053 Uiso 1 1 calc R . . C19 C 0.5826(7) 0.6837(6) 0.5330(6) 0.068(3) Uani 1 1 d . . . H19 H 0.5855 0.7179 0.5689 0.082 Uiso 1 1 calc R . . C20 C 0.6740(8) 0.6666(6) 0.5218(6) 0.073(3) Uani 1 1 d . . . H20A H 0.6839 0.6212 0.5110 0.087 Uiso 1 1 calc R . . H20B H 0.7324 0.6895 0.5504 0.087 Uiso 1 1 calc R . . C21 C 0.5992(7) 0.7049(6) 0.4661(6) 0.076(3) Uani 1 1 d . . . H21A H 0.6118 0.7511 0.4610 0.092 Uiso 1 1 calc R . . H21B H 0.5633 0.6828 0.4216 0.092 Uiso 1 1 calc R . . C22 C 0.6966(7) 0.4916(6) 0.8036(5) 0.066(3) Uani 1 1 d . . . H22A H 0.7068 0.5320 0.8313 0.080 Uiso 1 1 calc R . . H22B H 0.6309 0.4765 0.7979 0.080 Uiso 1 1 calc R . . C23 C 0.7645(8) 0.4437(7) 0.8435(7) 0.085(4) Uani 1 1 d . . . H23 H 0.7651 0.4478 0.8938 0.102 Uiso 1 1 calc R . . C24 C 0.7423(10) 0.3784(7) 0.8247(8) 0.117(5) Uani 1 1 d . . . H24A H 0.6735 0.3714 0.8143 0.175 Uiso 1 1 calc R . . H24B H 0.7777 0.3507 0.8641 0.175 Uiso 1 1 calc R . . H24C H 0.7606 0.3681 0.7827 0.175 Uiso 1 1 calc R . . C25 C 0.8722(7) 0.4753(6) 0.7744(6) 0.074(3) Uani 1 1 d . . . H25A H 0.8613 0.4361 0.7447 0.088 Uiso 1 1 calc R . . H25B H 0.9372 0.4915 0.7794 0.088 Uiso 1 1 calc R . . C26 C 0.7998(7) 0.5255(6) 0.7378(6) 0.066(3) Uani 1 1 d . . . H26A H 0.8150 0.5665 0.7643 0.079 Uiso 1 1 calc R . . H26B H 0.8029 0.5330 0.6895 0.079 Uiso 1 1 calc R . . C27 C 0.6486(10) 0.6644(6) 0.7074(7) 0.105(5) Uani 1 1 d . . . H27A H 0.5843 0.6822 0.6857 0.158 Uiso 1 1 calc R . . H27B H 0.6951 0.6995 0.7208 0.158 Uiso 1 1 calc R . . H27C H 0.6502 0.6397 0.7497 0.158 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0327(6) 0.0491(7) 0.0374(6) -0.0065(5) 0.0102(4) -0.0093(5) F1 0.055(3) 0.072(4) 0.084(4) 0.028(4) -0.001(3) -0.007(3) N1 0.038(4) 0.052(5) 0.054(5) -0.002(4) 0.007(4) -0.017(4) N2 0.036(4) 0.080(6) 0.051(5) 0.002(4) 0.010(4) -0.012(4) N3 0.045(5) 0.109(9) 0.073(6) 0.003(6) 0.007(5) -0.009(5) O1 0.053(4) 0.060(5) 0.062(4) -0.016(4) 0.021(3) -0.023(4) O2 0.118(7) 0.093(7) 0.128(7) -0.031(6) 0.082(6) -0.029(6) O3 0.065(4) 0.052(5) 0.057(4) -0.007(4) 0.006(4) -0.026(4) O4 0.076(5) 0.084(6) 0.060(5) -0.014(4) -0.010(4) -0.010(5) O5 0.073(6) 0.037(5) 0.050(5) 0.000 0.034(5) 0.000 O6 0.043(4) 0.068(5) 0.056(4) 0.001(4) 0.010(3) -0.016(4) O7 0.059(4) 0.075(5) 0.068(5) 0.026(4) 0.003(4) -0.028(4) O8 0.042(4) 0.045(4) 0.061(4) 0.002(3) 0.016(3) -0.013(3) O9 0.062(5) 0.074(6) 0.068(5) -0.003(4) -0.008(4) -0.031(4) O10 0.142(10) 0.152(11) 0.217(13) 0.013(10) -0.057(9) 0.010(9) O11 0.097(8) 0.159(12) 0.319(18) 0.011(12) -0.041(10) -0.043(9) O12 0.089(12) 0.093(14) 0.104(14) -0.017(11) 0.010(10) -0.004(10) O13 0.088(13) 0.094(15) 0.104(16) -0.017(12) 0.010(11) -0.004(11) C1 0.050(6) 0.060(7) 0.056(6) -0.007(5) 0.028(5) -0.010(6) C2 0.048(6) 0.044(6) 0.045(6) -0.013(5) 0.007(5) 0.002(5) C3 0.045(5) 0.043(6) 0.034(5) 0.000(4) 0.018(4) 0.001(5) C4 0.045(5) 0.036(5) 0.032(4) -0.003(4) 0.009(4) -0.005(4) C5 0.040(5) 0.035(5) 0.045(5) 0.006(4) 0.017(4) -0.002(4) C6 0.054(6) 0.033(5) 0.033(5) 0.002(4) 0.017(4) 0.004(5) C7 0.050(6) 0.040(5) 0.040(5) -0.003(4) 0.016(4) -0.013(5) C8 0.045(5) 0.045(6) 0.046(5) 0.002(4) 0.019(4) -0.004(5) C9 0.037(5) 0.053(6) 0.057(6) -0.002(5) 0.012(5) -0.010(5) C10 0.041(5) 0.055(6) 0.055(6) 0.005(5) 0.008(5) -0.013(5) C11 0.030(5) 0.050(6) 0.046(5) -0.009(5) 0.008(4) -0.008(5) C12 0.043(5) 0.043(6) 0.047(5) -0.005(4) 0.018(4) -0.007(5) C13 0.022(4) 0.051(6) 0.048(5) -0.008(5) 0.012(4) -0.008(4) C14 0.035(5) 0.054(6) 0.047(5) -0.005(5) 0.009(4) -0.011(5) C15 0.039(5) 0.060(7) 0.054(6) -0.003(5) 0.009(5) -0.018(5) C16 0.032(5) 0.069(7) 0.048(6) -0.008(5) 0.011(4) -0.008(5) C17 0.033(5) 0.058(6) 0.048(5) 0.001(5) 0.005(4) -0.009(5) C18 0.031(5) 0.053(6) 0.051(5) -0.002(5) 0.016(4) -0.011(5) C19 0.048(6) 0.067(8) 0.077(8) 0.005(6) 0.004(6) -0.024(6) C20 0.049(6) 0.073(8) 0.083(8) 0.017(6) 0.003(6) -0.016(6) C21 0.051(6) 0.074(8) 0.088(8) 0.028(7) -0.001(6) -0.026(6) C22 0.044(6) 0.097(9) 0.055(6) 0.007(6) 0.011(5) -0.005(6) C23 0.057(7) 0.101(11) 0.085(9) 0.012(8) 0.005(7) -0.016(8) C24 0.073(9) 0.098(12) 0.151(14) -0.016(10) -0.005(9) 0.010(9) C25 0.042(6) 0.105(10) 0.073(8) -0.010(7) 0.016(5) -0.006(7) C26 0.041(6) 0.092(9) 0.059(6) -0.006(6) 0.009(5) -0.018(6) C27 0.101(11) 0.084(10) 0.096(10) -0.030(8) -0.017(8) -0.015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O6 1.905(6) . ? Zn1 O1 1.924(6) . ? Zn1 O3 1.927(6) 5_566 ? Zn1 O8 1.949(6) . ? Zn1 C2 2.575(10) 5_566 ? F1 C17 1.348(10) . ? N1 C10 1.343(11) . ? N1 C14 1.380(11) . ? N1 C19 1.457(11) . ? N2 C16 1.387(11) . ? N2 C26 1.415(11) . ? N2 C22 1.432(11) . ? N3 C25 1.431(13) . ? N3 C23 1.504(13) . ? N3 H3 0.8999 . ? O1 C1 1.209(11) . ? O2 C1 1.249(11) . ? O2 H2 0.8200 . ? O3 C2 1.193(11) . ? O3 Zn1 1.927(6) 5_566 ? O4 C2 1.228(11) . ? O5 C6 1.362(9) 2_556 ? O5 C6 1.362(9) . ? O6 C9 1.251(10) . ? O7 C9 1.216(10) . ? O8 C12 1.261(10) . ? O9 C15 1.358(11) . ? O9 C27 1.421(13) . ? O10 H10C 0.8501 . ? O10 H10D 0.8500 . ? O11 H11C 0.8500 . ? O11 H11D 0.8500 . ? O12 H12C 0.8500 . ? O12 H12D 0.8500 . ? O12 H12B 0.8501 . ? O13 H13C 0.8500 . ? O13 H13D 0.8500 . ? C1 C3 1.467(11) . ? C2 C4 1.505(12) . ? C2 Zn1 2.575(10) 5_566 ? C3 C8 1.348(11) . ? C3 C4 1.377(11) . ? C4 C5 1.365(10) . ? C5 C6 1.340(11) . ? C5 H5 0.9300 . ? C6 C7 1.340(11) . ? C7 C8 1.338(11) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C11 1.499(12) . ? C10 C11 1.339(11) . ? C10 H10 0.9300 . ? C11 C12 1.387(12) . ? C12 C13 1.414(11) . ? C13 C14 1.370(11) . ? C13 C18 1.375(12) . ? C14 C15 1.396(12) . ? C15 C16 1.373(13) . ? C16 C17 1.365(12) . ? C17 C18 1.332(11) . ? C18 H18 0.9300 . ? C19 C20 1.447(14) . ? C19 C21 1.464(14) . ? C19 H19 0.9800 . ? C20 C21 1.486(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.426(15) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.391(17) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.475(14) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? 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 Zn1 O1 122.9(3) . . ? O6 Zn1 O3 98.9(3) . 5_566 ? O1 Zn1 O3 111.7(3) . 5_566 ? O6 Zn1 O8 92.2(3) . . ? O1 Zn1 O8 108.7(3) . . ? O3 Zn1 O8 122.0(3) 5_566 . ? O6 Zn1 C2 122.7(3) . 5_566 ? O1 Zn1 C2 101.6(3) . 5_566 ? O3 Zn1 C2 26.0(3) 5_566 5_566 ? O8 Zn1 C2 106.8(3) . 5_566 ? C10 N1 C14 119.6(8) . . ? C10 N1 C19 116.6(8) . . ? C14 N1 C19 123.7(8) . . ? C16 N2 C26 124.7(8) . . ? C16 N2 C22 120.4(7) . . ? C26 N2 C22 111.8(8) . . ? C25 N3 C23 112.9(9) . . ? C25 N3 H3 108.1 . . ? C23 N3 H3 108.3 . . ? C1 O1 Zn1 113.8(6) . . ? C1 O2 H2 109.5 . . ? C2 O3 Zn1 109.0(6) . 5_566 ? C6 O5 C6 118.8(9) 2_556 . ? C9 O6 Zn1 125.9(6) . . ? C12 O8 Zn1 119.9(6) . . ? C15 O9 C27 112.3(9) . . ? H10C O10 H10D 108.2 . . ? H11C O11 H11D 108.2 . . ? H12C O12 H12D 108.4 . . ? H12C O12 H12B 110.0 . . ? H12D O12 H12B 110.0 . . ? H13C O13 H13D 108.5 . . ? O1 C1 O2 121.9(9) . . ? O1 C1 C3 120.0(8) . . ? O2 C1 C3 118.1(10) . . ? O3 C2 O4 124.9(10) . . ? O3 C2 C4 117.3(9) . . ? O4 C2 C4 117.8(9) . . ? O3 C2 Zn1 45.0(5) . 5_566 ? O4 C2 Zn1 80.0(6) . 5_566 ? C4 C2 Zn1 161.8(7) . 5_566 ? C8 C3 C4 119.7(8) . . ? C8 C3 C1 118.6(8) . . ? C4 C3 C1 121.7(8) . . ? C5 C4 C3 118.5(8) . . ? C5 C4 C2 117.8(8) . . ? C3 C4 C2 123.5(8) . . ? C6 C5 C4 119.7(8) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C7 C6 C5 121.8(8) . . ? C7 C6 O5 117.2(8) . . ? C5 C6 O5 121.0(8) . . ? C8 C7 C6 119.2(8) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C3 121.1(8) . . ? C7 C8 H8 119.4 . . ? C3 C8 H8 119.4 . . ? O7 C9 O6 122.9(9) . . ? O7 C9 C11 117.7(8) . . ? O6 C9 C11 119.4(9) . . ? C11 C10 N1 124.7(9) . . ? C11 C10 H10 117.6 . . ? N1 C10 H10 117.6 . . ? C10 C11 C12 118.7(8) . . ? C10 C11 C9 116.3(9) . . ? C12 C11 C9 125.0(8) . . ? O8 C12 C11 124.7(8) . . ? O8 C12 C13 118.7(8) . . ? C11 C12 C13 116.6(8) . . ? C14 C13 C18 118.4(8) . . ? C14 C13 C12 123.1(9) . . ? C18 C13 C12 118.3(8) . . ? C13 C14 N1 116.9(8) . . ? C13 C14 C15 120.2(9) . . ? N1 C14 C15 122.9(8) . . ? O9 C15 C16 118.3(8) . . ? O9 C15 C14 121.4(9) . . ? C16 C15 C14 120.2(9) . . ? C17 C16 C15 116.9(9) . . ? C17 C16 N2 119.8(9) . . ? C15 C16 N2 123.2(9) . . ? C18 C17 F1 117.7(8) . . ? C18 C17 C16 123.6(9) . . ? F1 C17 C16 118.6(8) . . ? C17 C18 C13 120.1(8) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 N1 118.3(10) . . ? C20 C19 C21 61.4(7) . . ? N1 C19 C21 116.9(9) . . ? C20 C19 H19 116.3 . . ? N1 C19 H19 116.3 . . ? C21 C19 H19 116.3 . . ? C19 C20 C21 59.9(7) . . ? C19 C20 H20A 117.8 . . ? C21 C20 H20A 117.8 . . ? C19 C20 H20B 117.8 . . ? C21 C20 H20B 117.8 . . ? H20A C20 H20B 114.9 . . ? C19 C21 C20 58.7(7) . . ? C19 C21 H21A 117.9 . . ? C20 C21 H21A 117.9 . . ? C19 C21 H21B 117.9 . . ? C20 C21 H21B 117.9 . . ? H21A C21 H21B 115.1 . . ? C23 C22 N2 113.8(9) . . ? C23 C22 H22A 108.8 . . ? N2 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? N2 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 116.8(11) . . ? C24 C23 N3 110.0(12) . . ? C22 C23 N3 111.5(10) . . ? C24 C23 H23 105.9 . . ? C22 C23 H23 105.9 . . ? N3 C23 H23 105.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 112.2(9) . . ? N3 C25 H25A 109.2 . . ? C26 C25 H25A 109.2 . . ? N3 C25 H25B 109.2 . . ? C26 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? N2 C26 C25 110.6(9) . . ? N2 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? O9 C27 H27A 109.5 . . ? O9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.701 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.118 #===END