# 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 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #========================================================= data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 843914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H32 Cd N4 O7, 5(H2 O)' _chemical_formula_sum 'C25 H32 Cd N4 O12' _chemical_formula_weight 692.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.185(5) _cell_length_b 10.983(5) _cell_length_c 14.243(5) _cell_angle_alpha 88.775(5) _cell_angle_beta 72.634(5) _cell_angle_gamma 75.770(5) _cell_volume 1471.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1573 _cell_measurement_theta_min 2.9781 _cell_measurement_theta_max 29.1454 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58739 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9349 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.1786 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5373 _reflns_number_gt 2816 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0362P)^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 5373 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1532 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.004 _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 -0.09498(6) 0.36482(7) 0.74156(5) 0.0446(2) Uani 1 1 d . . . O5 O 0.5740(5) 0.3035(5) 0.3560(4) 0.0558(16) Uani 1 1 d . . . O7 O 0.1829(5) 0.4066(6) 0.2649(4) 0.0545(15) Uani 1 1 d . . . O3 O 0.6707(5) 0.3625(6) 0.7440(4) 0.0551(16) Uani 1 1 d . . . C7 C 0.5287(7) 0.3266(7) 0.4559(6) 0.044(2) Uani 1 1 d . . . C3 C 0.5956(6) 0.3472(7) 0.6016(6) 0.0383(19) Uani 1 1 d . . . N1 N -0.1557(6) 0.3947(7) 0.9052(5) 0.0559(19) Uani 1 1 d . . . C8 C 0.6318(7) 0.3303(7) 0.5019(6) 0.042(2) Uani 1 1 d . . . H8 H 0.7258 0.3210 0.4640 0.051 Uiso 1 1 calc R . . C5 C 0.3528(7) 0.3569(7) 0.6142(6) 0.043(2) Uani 1 1 d . . . N4 N 0.0061(7) -0.1522(8) 1.2635(6) 0.060(2) Uani 1 1 d . . . O6 O 0.0309(7) 0.3775(8) 0.4151(5) 0.107(3) Uani 1 1 d . . . H6' H -0.0154 0.4470 0.4068 0.160 Uiso 1 1 calc R . . C16 C 0.1507(9) 0.3446(10) 0.3404(7) 0.057(3) Uani 1 1 d . . . C6 C 0.3888(7) 0.3415(7) 0.5136(6) 0.043(2) Uani 1 1 d . . . H6 H 0.3191 0.3410 0.4839 0.052 Uiso 1 1 calc R . . C15 C 0.2454(9) 0.2179(10) 0.3468(7) 0.065(3) Uani 1 1 d . . . C4 C 0.4541(7) 0.3591(7) 0.6596(6) 0.042(2) Uani 1 1 d . . . H4 H 0.4292 0.3684 0.7279 0.050 Uiso 1 1 calc R . . O1 O 0.1095(5) 0.3814(6) 0.6289(5) 0.0661(18) Uani 1 1 d . . . O2 O 0.1725(5) 0.3575(7) 0.7646(5) 0.080(2) Uani 1 1 d . . . N2 N -0.1174(10) 0.3835(8) 1.0507(6) 0.070(2) Uani 1 1 d . . . C2 C 0.7047(7) 0.3514(7) 0.6533(7) 0.044(2) Uani 1 1 d . . . C10 C 0.3927(9) 0.2013(10) 0.3316(7) 0.065(3) Uani 1 1 d . . . N3 N -0.0455(11) 0.0397(12) 1.2151(11) 0.118(4) Uani 1 1 d . . . C11 C 0.4712(11) 0.0802(11) 0.3409(8) 0.088(4) Uani 1 1 d . . . H11 H 0.5681 0.0668 0.3313 0.105 Uiso 1 1 calc R . . C9 C 0.4618(9) 0.3095(9) 0.3094(7) 0.071(3) Uani 1 1 d . . . H9A H 0.5023 0.3108 0.2386 0.085 Uiso 1 1 calc R . . H9B H 0.3894 0.3876 0.3318 0.085 Uiso 1 1 calc R . . C24 C -0.1020(11) -0.0814(12) 1.3359(9) 0.091(3) Uani 1 1 d . . . H24 H -0.1490 -0.1107 1.3950 0.109 Uiso 1 1 calc R . . C1 C 0.2013(7) 0.3660(8) 0.6755(8) 0.053(2) Uani 1 1 d . . . C14 C 0.1848(11) 0.1164(11) 0.3723(8) 0.082(3) Uani 1 1 d . . . H14 H 0.0873 0.1281 0.3858 0.098 Uiso 1 1 calc R . . C17 C -0.0640(9) 0.3557(9) 0.9564(7) 0.065(3) Uani 1 1 d . . . H17 H 0.0301 0.3124 0.9271 0.078 Uiso 1 1 calc R . . C21 C -0.0624(18) 0.2582(19) 1.1922(12) 0.176(9) Uani 1 1 d . . . H21A H 0.0089 0.2420 1.2264 0.211 Uiso 1 1 calc R . . H21B H -0.1552 0.2837 1.2410 0.211 Uiso 1 1 calc R . . C18 C -0.2805(10) 0.4463(11) 0.9773(9) 0.093(4) Uani 1 1 d . . . H18 H -0.3674 0.4806 0.9665 0.112 Uiso 1 1 calc R . . C25 C -0.1307(12) 0.0355(13) 1.3100(12) 0.110(5) Uani 1 1 d . . . H25 H -0.1968 0.1035 1.3489 0.132 Uiso 1 1 calc R . . C23 C 0.0352(11) -0.0746(14) 1.1952(10) 0.094(4) Uani 1 1 d . . . H23 H 0.1082 -0.0986 1.1364 0.113 Uiso 1 1 calc R . . C20 C -0.0403(18) 0.3620(13) 1.1231(10) 0.122(5) Uani 1 1 d . . . H20A H -0.0651 0.4398 1.1627 0.147 Uiso 1 1 calc R . . H20B H 0.0604 0.3450 1.0878 0.147 Uiso 1 1 calc R . . C12 C 0.4113(13) -0.0180(12) 0.3631(10) 0.111(4) Uani 1 1 d . . . H12 H 0.4667 -0.0973 0.3687 0.133 Uiso 1 1 calc R . . C13 C 0.2676(13) 0.0002(12) 0.3775(9) 0.101(4) Uani 1 1 d . . . H13 H 0.2269 -0.0678 0.3909 0.122 Uiso 1 1 calc R . . C22 C -0.0535(16) 0.1581(18) 1.1441(10) 0.148(7) Uani 1 1 d . . . H22A H 0.0309 0.1417 1.0873 0.178 Uiso 1 1 calc R . . H22B H -0.1357 0.1688 1.1209 0.178 Uiso 1 1 calc R . . C19 C -0.2584(15) 0.4399(12) 1.0651(9) 0.114(5) Uani 1 1 d . . . H19 H -0.3264 0.4686 1.1253 0.136 Uiso 1 1 calc R . . O4 O 0.8282(5) 0.3474(6) 0.5993(4) 0.0599(17) Uani 1 1 d . . . O1W O 0.5284(9) 0.2258(10) 0.8892(6) 0.141(3) Uani 1 1 d . . . O2W O 0.4007(10) 0.2499(10) 0.0968(6) 0.157(4) Uani 1 1 d . . . O3W O 0.2864(9) 0.1646(11) 0.8704(9) 0.183(5) Uani 1 1 d . . . O4W O -0.3100(13) 0.0776(14) 1.0671(10) 0.221(6) Uani 1 1 d . . . O5W O 0.3281(12) 0.0257(13) 0.0984(10) 0.213(5) 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 0.0404(3) 0.0490(4) 0.0495(4) 0.0138(3) -0.0193(2) -0.0145(2) O5 0.047(3) 0.071(5) 0.050(4) 0.003(3) -0.020(3) -0.011(3) O7 0.061(3) 0.050(4) 0.055(4) 0.023(3) -0.020(3) -0.019(3) O3 0.054(3) 0.073(5) 0.048(4) 0.004(3) -0.023(3) -0.023(3) C7 0.053(5) 0.037(6) 0.042(5) 0.002(4) -0.015(4) -0.010(4) C3 0.032(4) 0.030(5) 0.060(6) 0.015(4) -0.023(4) -0.012(3) N1 0.055(4) 0.064(6) 0.052(5) 0.015(4) -0.020(4) -0.018(4) C8 0.037(4) 0.047(6) 0.046(5) 0.013(4) -0.012(4) -0.017(4) C5 0.036(4) 0.033(5) 0.065(6) 0.006(4) -0.019(4) -0.011(3) N4 0.059(4) 0.046(6) 0.073(6) 0.009(5) -0.021(4) -0.008(4) O6 0.099(5) 0.119(8) 0.089(6) 0.007(5) -0.010(4) -0.025(5) C16 0.055(5) 0.059(8) 0.063(7) 0.003(6) -0.016(5) -0.026(5) C6 0.040(4) 0.034(5) 0.063(6) 0.010(4) -0.028(4) -0.010(3) C15 0.068(6) 0.048(7) 0.087(8) 0.006(6) -0.033(5) -0.016(5) C4 0.040(4) 0.035(5) 0.048(5) 0.009(4) -0.008(3) -0.013(3) O1 0.035(3) 0.063(5) 0.099(5) 0.031(4) -0.021(3) -0.012(3) O2 0.047(3) 0.112(7) 0.074(5) -0.003(5) 0.000(3) -0.028(3) N2 0.112(7) 0.047(6) 0.058(6) 0.016(5) -0.032(5) -0.026(5) C2 0.040(4) 0.031(5) 0.064(6) 0.006(5) -0.020(4) -0.010(3) C10 0.068(6) 0.057(8) 0.073(7) 0.010(5) -0.028(5) -0.014(5) N3 0.089(7) 0.073(9) 0.183(14) 0.045(9) -0.029(7) -0.020(6) C11 0.076(6) 0.058(9) 0.128(11) 0.002(7) -0.040(6) -0.006(6) C9 0.074(6) 0.067(8) 0.076(7) 0.001(6) -0.027(5) -0.019(5) C24 0.081(7) 0.064(9) 0.114(11) 0.014(8) -0.022(7) -0.005(6) C1 0.033(5) 0.040(6) 0.082(8) 0.000(6) -0.011(5) -0.007(4) C14 0.096(7) 0.053(8) 0.110(9) 0.016(7) -0.042(6) -0.031(6) C17 0.074(6) 0.059(7) 0.056(7) 0.016(6) -0.017(5) -0.012(5) C21 0.219(16) 0.19(2) 0.143(17) -0.058(16) -0.018(12) -0.140(15) C18 0.072(6) 0.104(10) 0.068(8) 0.006(7) 0.003(6) 0.015(6) C25 0.083(8) 0.049(10) 0.169(15) -0.006(9) -0.011(8) 0.007(7) C23 0.074(7) 0.067(10) 0.136(12) 0.041(9) -0.023(7) -0.021(7) C20 0.251(16) 0.073(10) 0.082(10) 0.036(8) -0.091(10) -0.067(10) C12 0.107(9) 0.061(10) 0.176(14) 0.017(8) -0.055(8) -0.027(7) C13 0.116(9) 0.051(9) 0.150(12) 0.016(8) -0.049(8) -0.034(7) C22 0.213(15) 0.20(2) 0.103(12) 0.097(12) -0.105(11) -0.129(14) C19 0.153(12) 0.098(11) 0.053(8) -0.005(8) 0.000(8) -0.003(9) O4 0.032(3) 0.090(5) 0.064(4) 0.013(3) -0.015(3) -0.027(3) O1W 0.176(8) 0.159(10) 0.096(7) 0.044(6) -0.033(6) -0.069(7) O2W 0.230(10) 0.144(10) 0.085(7) 0.016(6) -0.034(6) -0.047(7) O3W 0.120(7) 0.195(12) 0.225(12) 0.083(9) -0.040(7) -0.042(7) O4W 0.217(11) 0.250(17) 0.230(14) 0.033(12) -0.071(10) -0.119(10) O5W 0.191(10) 0.209(14) 0.207(13) 0.037(11) -0.009(8) -0.057(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.235(7) . ? Cd1 O1 2.264(5) . ? Cd1 N4 2.282(8) 2_557 ? Cd1 O3 2.383(4) 1_455 ? Cd1 O4 2.407(5) 1_455 ? Cd1 O7 2.459(6) 2_566 ? Cd1 C2 2.729(7) 1_455 ? O5 C7 1.367(8) . ? O5 C9 1.471(9) . ? O7 C16 1.264(11) . ? O7 Cd1 2.459(6) 2_566 ? O3 C2 1.234(9) . ? O3 Cd1 2.383(4) 1_655 ? C7 C6 1.387(9) . ? C7 C8 1.403(9) . ? C3 C8 1.361(9) . ? C3 C4 1.407(9) . ? C3 C2 1.514(9) . ? N1 C17 1.336(10) . ? N1 C18 1.372(10) . ? C8 H8 0.9300 . ? C5 C6 1.372(10) . ? C5 C4 1.376(9) . ? C5 C1 1.509(10) . ? N4 C23 1.295(13) . ? N4 C24 1.347(12) . ? N4 Cd1 2.282(8) 2_557 ? O6 C16 1.332(10) . ? O6 H6' 0.8200 . ? C16 C15 1.504(13) . ? C6 H6 0.9300 . ? C15 C14 1.394(13) . ? C15 C10 1.416(11) . ? C4 H4 0.9300 . ? O1 C1 1.277(9) . ? O2 C1 1.222(10) . ? N2 C17 1.301(10) . ? N2 C19 1.371(13) . ? N2 C20 1.456(13) . ? C2 O4 1.253(8) . ? C2 Cd1 2.729(7) 1_655 ? C10 C11 1.399(14) . ? C10 C9 1.507(13) . ? N3 C23 1.304(14) . ? N3 C25 1.378(16) . ? N3 C22 1.631(17) . ? C11 C12 1.352(14) . ? C11 H11 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C24 C25 1.316(15) . ? C24 H24 0.9300 . ? C14 C13 1.359(14) . ? C14 H14 0.9300 . ? C17 H17 0.9300 . ? C21 C22 1.277(18) . ? C21 C20 1.51(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C18 C19 1.332(14) . ? C18 H18 0.9300 . ? C25 H25 0.9300 . ? C23 H23 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C12 C13 1.379(13) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C19 H19 0.9300 . ? O4 Cd1 2.407(5) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 O1 127.6(2) . . ? N1 Cd1 N4 96.1(3) . 2_557 ? O1 Cd1 N4 89.8(3) . 2_557 ? N1 Cd1 O3 93.3(2) . 1_455 ? O1 Cd1 O3 137.6(2) . 1_455 ? N4 Cd1 O3 97.2(2) 2_557 1_455 ? N1 Cd1 O4 147.36(19) . 1_455 ? O1 Cd1 O4 84.02(19) . 1_455 ? N4 Cd1 O4 91.4(2) 2_557 1_455 ? O3 Cd1 O4 54.18(17) 1_455 1_455 ? N1 Cd1 O7 87.6(2) . 2_566 ? O1 Cd1 O7 87.2(2) . 2_566 ? N4 Cd1 O7 176.2(3) 2_557 2_566 ? O3 Cd1 O7 83.51(18) 1_455 2_566 ? O4 Cd1 O7 85.92(19) 1_455 2_566 ? N1 Cd1 C2 120.1(2) . 1_455 ? O1 Cd1 C2 111.1(2) . 1_455 ? N4 Cd1 C2 94.7(2) 2_557 1_455 ? O3 Cd1 C2 26.85(19) 1_455 1_455 ? O4 Cd1 C2 27.3(2) 1_455 1_455 ? O7 Cd1 C2 84.3(2) 2_566 1_455 ? C7 O5 C9 115.7(6) . . ? C16 O7 Cd1 125.1(6) . 2_566 ? C2 O3 Cd1 92.4(4) . 1_655 ? O5 C7 C6 123.7(6) . . ? O5 C7 C8 117.3(6) . . ? C6 C7 C8 118.9(7) . . ? C8 C3 C4 120.0(6) . . ? C8 C3 C2 121.8(6) . . ? C4 C3 C2 118.3(7) . . ? C17 N1 C18 102.9(8) . . ? C17 N1 Cd1 122.9(6) . . ? C18 N1 Cd1 134.2(7) . . ? C3 C8 C7 120.6(6) . . ? C3 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C6 C5 C4 120.8(6) . . ? C6 C5 C1 119.2(7) . . ? C4 C5 C1 119.9(8) . . ? C23 N4 C24 104.2(10) . . ? C23 N4 Cd1 128.8(9) . 2_557 ? C24 N4 Cd1 126.5(8) . 2_557 ? C16 O6 H6' 109.5 . . ? O7 C16 O6 125.2(10) . . ? O7 C16 C15 119.9(8) . . ? O6 C16 C15 114.7(9) . . ? C5 C6 C7 120.4(6) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C14 C15 C10 119.7(10) . . ? C14 C15 C16 118.8(8) . . ? C10 C15 C16 121.4(9) . . ? C5 C4 C3 119.3(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C1 O1 Cd1 105.6(6) . . ? C17 N2 C19 105.1(9) . . ? C17 N2 C20 126.4(11) . . ? C19 N2 C20 128.5(11) . . ? O3 C2 O4 122.6(6) . . ? O3 C2 C3 120.8(6) . . ? O4 C2 C3 116.6(8) . . ? O3 C2 Cd1 60.7(3) . 1_655 ? O4 C2 Cd1 61.8(4) . 1_655 ? C3 C2 Cd1 177.9(6) . 1_655 ? C11 C10 C15 117.0(9) . . ? C11 C10 C9 121.2(8) . . ? C15 C10 C9 121.7(9) . . ? C23 N3 C25 103.3(12) . . ? C23 N3 C22 129.3(14) . . ? C25 N3 C22 127.4(13) . . ? C12 C11 C10 122.5(10) . . ? C12 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? O5 C9 C10 113.6(8) . . ? O5 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? O5 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C25 C24 N4 109.4(12) . . ? C25 C24 H24 125.3 . . ? N4 C24 H24 125.3 . . ? O2 C1 O1 123.7(7) . . ? O2 C1 C5 119.9(8) . . ? O1 C1 C5 116.4(9) . . ? C13 C14 C15 120.3(10) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? N2 C17 N1 114.3(8) . . ? N2 C17 H17 122.8 . . ? N1 C17 H17 122.8 . . ? C22 C21 C20 110.1(15) . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.2 . . ? C19 C18 N1 109.8(10) . . ? C19 C18 H18 125.1 . . ? N1 C18 H18 125.1 . . ? C24 C25 N3 108.0(10) . . ? C24 C25 H25 126.0 . . ? N3 C25 H25 126.0 . . ? N4 C23 N3 114.9(12) . . ? N4 C23 H23 122.5 . . ? N3 C23 H23 122.5 . . ? N2 C20 C21 118.0(12) . . ? N2 C20 H20A 107.8 . . ? C21 C20 H20A 107.8 . . ? N2 C20 H20B 107.8 . . ? C21 C20 H20B 107.8 . . ? H20A C20 H20B 107.1 . . ? C11 C12 C13 119.5(12) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 120.8(11) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C21 C22 N3 109.6(14) . . ? C21 C22 H22A 109.7 . . ? N3 C22 H22A 109.7 . . ? C21 C22 H22B 109.7 . . ? N3 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C18 C19 N2 107.8(10) . . ? C18 C19 H19 126.1 . . ? N2 C19 H19 126.1 . . ? C2 O4 Cd1 90.8(5) . 1_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 O5 C7 C6 6.9(11) . . . . ? C9 O5 C7 C8 -175.7(7) . . . . ? O1 Cd1 N1 C17 -39.9(8) . . . . ? N4 Cd1 N1 C17 54.5(7) 2_557 . . . ? O3 Cd1 N1 C17 152.1(7) 1_455 . . . ? O4 Cd1 N1 C17 156.8(6) 1_455 . . . ? O7 Cd1 N1 C17 -124.5(7) 2_566 . . . ? C2 Cd1 N1 C17 153.5(6) 1_455 . . . ? O1 Cd1 N1 C18 142.8(9) . . . . ? N4 Cd1 N1 C18 -122.8(9) 2_557 . . . ? O3 Cd1 N1 C18 -25.2(9) 1_455 . . . ? O4 Cd1 N1 C18 -20.5(12) 1_455 . . . ? O7 Cd1 N1 C18 58.2(9) 2_566 . . . ? C2 Cd1 N1 C18 -23.8(10) 1_455 . . . ? C4 C3 C8 C7 1.1(12) . . . . ? C2 C3 C8 C7 180.0(7) . . . . ? O5 C7 C8 C3 -177.0(7) . . . . ? C6 C7 C8 C3 0.5(12) . . . . ? Cd1 O7 C16 O6 26.4(11) 2_566 . . . ? Cd1 O7 C16 C15 -158.9(5) 2_566 . . . ? C4 C5 C6 C7 0.6(12) . . . . ? C1 C5 C6 C7 -176.8(7) . . . . ? O5 C7 C6 C5 176.0(7) . . . . ? C8 C7 C6 C5 -1.3(12) . . . . ? O7 C16 C15 C14 -129.9(10) . . . . ? O6 C16 C15 C14 45.3(12) . . . . ? O7 C16 C15 C10 52.8(12) . . . . ? O6 C16 C15 C10 -132.0(9) . . . . ? C6 C5 C4 C3 0.9(12) . . . . ? C1 C5 C4 C3 178.3(7) . . . . ? C8 C3 C4 C5 -1.8(11) . . . . ? C2 C3 C4 C5 179.3(7) . . . . ? N1 Cd1 O1 C1 22.9(6) . . . . ? N4 Cd1 O1 C1 -74.6(5) 2_557 . . . ? O3 Cd1 O1 C1 -175.1(5) 1_455 . . . ? O4 Cd1 O1 C1 -166.1(5) 1_455 . . . ? O7 Cd1 O1 C1 107.7(5) 2_566 . . . ? C2 Cd1 O1 C1 -169.6(5) 1_455 . . . ? Cd1 O3 C2 O4 -0.8(8) 1_655 . . . ? Cd1 O3 C2 C3 -178.4(6) 1_655 . . . ? C8 C3 C2 O3 -177.5(8) . . . . ? C4 C3 C2 O3 1.4(11) . . . . ? C8 C3 C2 O4 4.8(11) . . . . ? C4 C3 C2 O4 -176.3(7) . . . . ? C8 C3 C2 Cd1 46(16) . . . 1_655 ? C4 C3 C2 Cd1 -135(15) . . . 1_655 ? C14 C15 C10 C11 1.6(14) . . . . ? C16 C15 C10 C11 178.9(9) . . . . ? C14 C15 C10 C9 -176.6(9) . . . . ? C16 C15 C10 C9 0.7(13) . . . . ? C15 C10 C11 C12 0.1(16) . . . . ? C9 C10 C11 C12 178.4(10) . . . . ? C7 O5 C9 C10 -71.3(9) . . . . ? C11 C10 C9 O5 -35.5(12) . . . . ? C15 C10 C9 O5 142.6(8) . . . . ? C23 N4 C24 C25 -1.8(13) . . . . ? Cd1 N4 C24 C25 -175.2(8) 2_557 . . . ? Cd1 O1 C1 O2 -6.6(11) . . . . ? Cd1 O1 C1 C5 172.8(6) . . . . ? C6 C5 C1 O2 167.2(9) . . . . ? C4 C5 C1 O2 -10.2(13) . . . . ? C6 C5 C1 O1 -12.3(11) . . . . ? C4 C5 C1 O1 170.3(7) . . . . ? C10 C15 C14 C13 -3.5(16) . . . . ? C16 C15 C14 C13 179.1(10) . . . . ? C19 N2 C17 N1 3.3(12) . . . . ? C20 N2 C17 N1 -174.7(9) . . . . ? C18 N1 C17 N2 -3.2(11) . . . . ? Cd1 N1 C17 N2 178.7(6) . . . . ? C17 N1 C18 C19 1.8(13) . . . . ? Cd1 N1 C18 C19 179.5(8) . . . . ? N4 C24 C25 N3 4.2(14) . . . . ? C23 N3 C25 C24 -4.8(14) . . . . ? C22 N3 C25 C24 171.7(11) . . . . ? C24 N4 C23 N3 -1.4(14) . . . . ? Cd1 N4 C23 N3 171.7(7) 2_557 . . . ? C25 N3 C23 N4 3.9(15) . . . . ? C22 N3 C23 N4 -172.5(10) . . . . ? C17 N2 C20 C21 -107.1(17) . . . . ? C19 N2 C20 C21 75.3(18) . . . . ? C22 C21 C20 N2 47(2) . . . . ? C10 C11 C12 C13 0.0(19) . . . . ? C15 C14 C13 C12 3.6(18) . . . . ? C11 C12 C13 C14 -1.9(19) . . . . ? C20 C21 C22 N3 168.7(13) . . . . ? C23 N3 C22 C21 -137.3(16) . . . . ? C25 N3 C22 C21 47.1(19) . . . . ? N1 C18 C19 N2 0.0(15) . . . . ? C17 N2 C19 C18 -1.9(14) . . . . ? C20 N2 C19 C18 176.1(11) . . . . ? O3 C2 O4 Cd1 0.8(8) . . . 1_655 ? C3 C2 O4 Cd1 178.5(6) . . . 1_655 ? 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 O6 H6' O1 0.82 2.02 2.837(10) 172.9 2_566 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.597 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.102 #========================================================= data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 843915' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H50 N8 O17 Zn2' _chemical_formula_sum 'C50 H50 N8 O17 Zn2' _chemical_formula_weight 1165.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.518(5) _cell_length_b 17.907(5) _cell_length_c 18.204(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 111.876(5) _cell_angle_gamma 90.000(5) _cell_volume 5299(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3941 _cell_measurement_theta_min 2.9751 _cell_measurement_theta_max 29.2263 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98094 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25438 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.1487 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 29.29 _reflns_number_total 12342 _reflns_number_gt 5027 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0361P)^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 12342 _refine_ls_number_parameters 713 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2063 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.1749 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.012 _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 0.25501(5) 0.32884(3) 0.33249(4) 0.0588(2) Uani 1 1 d . . . Zn2 Zn 0.72675(4) 0.19676(3) 0.89091(4) 0.0528(2) Uani 1 1 d . . . O10 O 0.7169(3) 0.2749(2) 0.5305(2) 0.0707(12) Uani 1 1 d . . . C8 C 0.3314(4) 0.2025(3) 0.6126(3) 0.0518(14) Uani 1 1 d . . . H8 H 0.2844 0.2247 0.6150 0.062 Uiso 1 1 calc R . . C33 C 0.8033(4) 0.1942(3) 0.6694(3) 0.0516(14) Uani 1 1 d . . . H33 H 0.7632 0.2275 0.6711 0.062 Uiso 1 1 calc R . . O8 O 0.7641(3) 0.1980(2) 0.8023(2) 0.0600(10) Uani 1 1 d . . . C3 C 0.3814(4) 0.1592(3) 0.6752(3) 0.0546(15) Uani 1 1 d . . . N6 N 0.5236(3) 0.3211(3) 0.7548(3) 0.0647(14) Uani 1 1 d . . . C28 C 0.8442(4) 0.1493(3) 0.7343(3) 0.0555(15) Uani 1 1 d . . . O11 O 0.8067(3) 0.24449(19) 0.4782(2) 0.0642(11) Uani 1 1 d . . . O2 O 0.2399(3) 0.2956(3) 0.4837(3) 0.0987(16) Uani 1 1 d . . . N7 N 0.3890(4) 0.5033(3) 0.5901(3) 0.0605(13) Uani 1 1 d . . . C27 C 0.7787(4) 0.2389(3) 0.5328(3) 0.0563(16) Uani 1 1 d . . . C32 C 0.8221(4) 0.1893(3) 0.6024(3) 0.0518(15) Uani 1 1 d . . . C5 C 0.4685(4) 0.1351(3) 0.6041(4) 0.0706(18) Uani 1 1 d . . . O3 O 0.2953(3) 0.1824(2) 0.7473(2) 0.0655(11) Uani 1 1 d . . . C4 C 0.4513(4) 0.1245(3) 0.6713(4) 0.0652(17) Uani 1 1 d . . . H4 H 0.4851 0.0952 0.7128 0.078 Uiso 1 1 calc R . . C7 C 0.3514(4) 0.2126(3) 0.5472(3) 0.0540(15) Uani 1 1 d . . . O9 O 0.8641(3) 0.1215(2) 0.8679(2) 0.0822(14) Uani 1 1 d . . . C30 C 0.9217(5) 0.0943(3) 0.6638(4) 0.074(2) Uani 1 1 d . . . O4 O 0.4060(3) 0.1115(2) 0.8048(3) 0.0847(14) Uani 1 1 d . . . C29 C 0.9033(4) 0.1000(3) 0.7305(4) 0.0698(18) Uani 1 1 d . . . H29 H 0.9312 0.0702 0.7740 0.084 Uiso 1 1 calc R . . O1 O 0.3220(3) 0.2676(2) 0.4217(2) 0.0706(12) Uani 1 1 d . . . O12 O 0.9807(4) 0.0427(3) 0.6679(3) 0.117(2) Uani 1 1 d . . . N2 N 0.1835(4) 0.5322(3) 0.3876(3) 0.0764(16) Uani 1 1 d . . . C26 C 0.8240(4) 0.1563(3) 0.8077(3) 0.0576(16) Uani 1 1 d . . . N5 N 0.6224(3) 0.2568(2) 0.8419(3) 0.0584(13) Uani 1 1 d . . . N3 N -0.0383(3) 0.7172(3) 0.2901(4) 0.0759(16) Uani 1 1 d . . . N8 N 0.3073(3) 0.5927(2) 0.5984(3) 0.0567(13) Uani 1 1 d . . . C42 C 0.5906(4) 0.2802(3) 0.7687(4) 0.0604(16) Uani 1 1 d . . . H42 H 0.6125 0.2693 0.7307 0.072 Uiso 1 1 calc R . . N1 N 0.2405(3) 0.4332(3) 0.3597(3) 0.0613(13) Uani 1 1 d . . . C23 C -0.1118(4) 0.7482(3) 0.2808(4) 0.0702(18) Uani 1 1 d . . . H23 H -0.1363 0.7448 0.3180 0.084 Uiso 1 1 calc R . . C6 C 0.4191(4) 0.1781(3) 0.5425(4) 0.0678(18) Uani 1 1 d . . . H6 H 0.4316 0.1838 0.4974 0.081 Uiso 1 1 calc R . . C45 C 0.4735(4) 0.3571(3) 0.6810(4) 0.0707(18) Uani 1 1 d . . . H45A H 0.4194 0.3677 0.6815 0.085 Uiso 1 1 calc R . . H45B H 0.4669 0.3236 0.6371 0.085 Uiso 1 1 calc R . . C2 C 0.3594(4) 0.1501(3) 0.7476(4) 0.0596(16) Uani 1 1 d . . . O5 O 0.5355(4) 0.1067(3) 0.5926(3) 0.124(2) Uani 1 1 d . . . C1 C 0.2995(5) 0.2615(3) 0.4807(4) 0.0675(18) Uani 1 1 d . . . C47 C 0.4643(5) 0.4676(4) 0.5903(4) 0.088(2) Uani 1 1 d . . . H47A H 0.4990 0.5050 0.5800 0.106 Uiso 1 1 calc R . . H47B H 0.4500 0.4310 0.5480 0.106 Uiso 1 1 calc R . . C31 C 0.8806(4) 0.1386(3) 0.5988(3) 0.0687(19) Uani 1 1 d . . . H31 H 0.8920 0.1344 0.5530 0.082 Uiso 1 1 calc R . . C35 C 1.0764(8) -0.0134(5) 0.6226(5) 0.101(3) Uani 1 1 d . . . N4 N -0.1435(3) 0.7827(3) 0.2151(3) 0.0699(15) Uani 1 1 d . . . C49 C 0.2653(4) 0.5274(3) 0.5827(4) 0.0677(17) Uani 1 1 d . . . H49 H 0.2104 0.5218 0.5765 0.081 Uiso 1 1 calc R . . C34 C 1.0016(5) 0.0361(4) 0.6000(4) 0.111(3) Uani 1 1 d . . . H34A H 1.0136 0.0848 0.5836 0.133 Uiso 1 1 calc R . . H34B H 0.9563 0.0142 0.5565 0.133 Uiso 1 1 calc R . . C46 C 0.5129(4) 0.4285(3) 0.6699(4) 0.079(2) Uani 1 1 d . . . H46A H 0.5681 0.4178 0.6724 0.095 Uiso 1 1 calc R . . H46B H 0.5175 0.4623 0.7130 0.095 Uiso 1 1 calc R . . C11 C 0.6984(6) -0.0361(4) 0.6362(6) 0.096(3) Uani 1 1 d . . . C18 C 0.2588(5) 0.5532(4) 0.3912(4) 0.080(2) Uani 1 1 d . . . H18 H 0.2821 0.6005 0.4029 0.096 Uiso 1 1 calc R . . C10 C 0.6383(5) 0.0199(4) 0.5993(5) 0.088(2) Uani 1 1 d . . . C19 C 0.1747(4) 0.4598(3) 0.3685(4) 0.0749(19) Uani 1 1 d . . . H19 H 0.1280 0.4318 0.3621 0.090 Uiso 1 1 calc R . . C48 C 0.3144(5) 0.4719(3) 0.5775(4) 0.0748(19) Uani 1 1 d . . . H48 H 0.3002 0.4218 0.5674 0.090 Uiso 1 1 calc R . . C50 C 0.3816(5) 0.5759(3) 0.6024(3) 0.0666(18) Uani 1 1 d . . . H50 H 0.4240 0.6104 0.6126 0.080 Uiso 1 1 calc R . . C9 C 0.5804(5) 0.0499(4) 0.6387(5) 0.099(2) Uani 1 1 d . . . H9A H 0.5442 0.0105 0.6429 0.119 Uiso 1 1 calc R . . H9B H 0.6121 0.0680 0.6915 0.119 Uiso 1 1 calc R . . C20 C 0.1209(5) 0.5773(4) 0.4058(4) 0.088(2) Uani 1 1 d . . . H20A H 0.0856 0.5444 0.4215 0.105 Uiso 1 1 calc R . . H20B H 0.1484 0.6109 0.4496 0.105 Uiso 1 1 calc R . . C22 C 0.0138(4) 0.6738(4) 0.3585(4) 0.089(2) Uani 1 1 d . . . H22A H -0.0206 0.6447 0.3790 0.107 Uiso 1 1 calc R . . H22B H 0.0469 0.7074 0.3999 0.107 Uiso 1 1 calc R . . O6 O 0.6576(5) -0.0719(4) 0.7384(4) 0.154(3) Uani 1 1 d . . . C41 C 0.9995(15) -0.1298(7) 0.5760(9) 0.180(8) Uani 1 1 d . . . O13 O 0.9349(6) -0.1112(5) 0.5766(7) 0.221(5) Uani 1 1 d . . . C17 C 0.2933(5) 0.4918(4) 0.3746(4) 0.0750(19) Uani 1 1 d . . . H17 H 0.3459 0.4897 0.3735 0.090 Uiso 1 1 calc R . . C43 C 0.5721(5) 0.2850(4) 0.8772(4) 0.097(2) Uani 1 1 d . . . H43 H 0.5793 0.2787 0.9301 0.116 Uiso 1 1 calc R . . C16 C 0.7074(8) -0.0674(5) 0.7126(8) 0.140(5) Uani 1 1 d . . . C21 C 0.0704(5) 0.6212(4) 0.3352(4) 0.091(2) Uani 1 1 d . . . H21A H 0.0376 0.5878 0.2933 0.109 Uiso 1 1 calc R . . H21B H 0.1058 0.6501 0.3158 0.109 Uiso 1 1 calc R . . C14 C 0.6820(7) 0.0245(6) 0.4878(6) 0.132(4) Uani 1 1 d . . . H14 H 0.6764 0.0442 0.4388 0.158 Uiso 1 1 calc R . . C13 C 0.7393(7) -0.0288(5) 0.5242(7) 0.119(3) Uani 1 1 d . . . H13 H 0.7737 -0.0457 0.4993 0.143 Uiso 1 1 calc R . . C44 C 0.5103(5) 0.3237(4) 0.8231(5) 0.100(3) Uani 1 1 d . . . H44 H 0.4669 0.3474 0.8314 0.120 Uiso 1 1 calc R . . C25 C -0.0889(5) 0.7762(5) 0.1800(5) 0.110(3) Uani 1 1 d . . . H25 H -0.0959 0.7958 0.1306 0.132 Uiso 1 1 calc R . . C15 C 0.6333(6) 0.0474(5) 0.5273(6) 0.119(3) Uani 1 1 d . . . H15 H 0.5943 0.0841 0.5039 0.143 Uiso 1 1 calc R . . C40 C 1.0763(8) -0.0879(7) 0.6153(6) 0.111(3) Uani 1 1 d . . . O14 O 1.0002(6) -0.1973(5) 0.5380(5) 0.211(4) Uani 1 1 d . . . H14A H 1.0473 -0.2071 0.5421 0.316 Uiso 1 1 calc R . . C24 C -0.0234(6) 0.7381(5) 0.2253(5) 0.115(3) Uani 1 1 d . . . H24 H 0.0234 0.7277 0.2146 0.138 Uiso 1 1 calc R . . C12 C 0.7479(6) -0.0585(4) 0.5970(6) 0.117(3) Uani 1 1 d . . . H12 H 0.7881 -0.0944 0.6199 0.141 Uiso 1 1 calc R . . C39 C 1.1502(10) -0.1292(6) 0.6391(7) 0.142(5) Uani 1 1 d . . . H39 H 1.1491 -0.1806 0.6315 0.171 Uiso 1 1 calc R . . C36 C 1.1499(9) 0.0195(6) 0.6539(6) 0.127(4) Uani 1 1 d . . . H36 H 1.1522 0.0711 0.6597 0.152 Uiso 1 1 calc R . . C37 C 1.2210(9) -0.0195(8) 0.6774(7) 0.167(5) Uani 1 1 d . . . H37 H 1.2707 0.0060 0.6977 0.200 Uiso 1 1 calc R . . C38 C 1.2212(9) -0.0938(10) 0.6723(7) 0.163(6) Uani 1 1 d . . . H38 H 1.2704 -0.1203 0.6916 0.196 Uiso 1 1 calc R . . O1W O 1.0145(3) 0.0648(3) 0.9609(4) 0.1253(19) Uani 1 1 d . . . O2W O 0.1353(4) 0.3347(4) 0.5568(4) 0.164(3) Uani 1 1 d . . . O3W O 0.5996(4) 0.2793(6) 0.5917(4) 0.084(3) Uani 0.50 1 d P . . O4W O 0.4785(5) 0.1529(4) 0.9648(5) 0.068(2) Uani 0.50 1 d P . . O7 O 0.7967(8) -0.0729(6) 0.7765(9) 0.218(6) Uani 0.70 1 d P . . O7' O 0.6895(16) -0.1553(13) 0.6979(15) 0.171(9) Uani 0.30 1 d PU . . 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 0.0706(5) 0.0614(4) 0.0501(5) -0.0004(3) 0.0292(4) -0.0028(4) Zn2 0.0683(5) 0.0533(4) 0.0375(4) 0.0014(3) 0.0207(3) 0.0027(3) O10 0.086(3) 0.080(3) 0.048(3) 0.013(2) 0.027(2) 0.014(3) C8 0.062(4) 0.051(3) 0.050(4) 0.002(3) 0.029(3) 0.001(3) C33 0.066(4) 0.048(3) 0.041(3) -0.003(3) 0.019(3) 0.006(3) O8 0.080(3) 0.067(2) 0.040(2) 0.0059(18) 0.030(2) 0.021(2) C3 0.069(4) 0.056(3) 0.044(4) 0.002(3) 0.026(3) -0.009(3) N6 0.066(4) 0.069(3) 0.056(4) 0.011(3) 0.019(3) 0.015(3) C28 0.079(5) 0.054(3) 0.042(4) 0.002(3) 0.033(3) 0.010(3) O11 0.096(3) 0.064(2) 0.040(2) 0.0071(18) 0.035(2) 0.006(2) O2 0.110(4) 0.125(4) 0.083(4) 0.036(3) 0.062(3) 0.043(3) N7 0.072(4) 0.055(3) 0.054(3) 0.008(2) 0.023(3) 0.012(3) C27 0.073(5) 0.053(3) 0.046(4) -0.005(3) 0.025(4) -0.007(3) C32 0.070(4) 0.054(3) 0.034(3) 0.002(2) 0.022(3) 0.003(3) C5 0.068(5) 0.079(4) 0.085(5) 0.009(4) 0.052(4) 0.012(4) O3 0.075(3) 0.082(3) 0.051(3) 0.007(2) 0.037(2) 0.012(2) C4 0.070(5) 0.071(4) 0.059(4) 0.015(3) 0.030(4) 0.008(4) C7 0.067(4) 0.056(3) 0.044(4) 0.010(3) 0.027(3) 0.005(3) O9 0.090(4) 0.118(3) 0.042(3) 0.021(2) 0.028(3) 0.027(3) C30 0.120(6) 0.071(4) 0.047(4) 0.011(3) 0.050(4) 0.033(4) O4 0.099(4) 0.104(3) 0.056(3) 0.024(3) 0.034(3) 0.012(3) C29 0.098(5) 0.063(4) 0.052(4) 0.017(3) 0.033(4) 0.026(4) O1 0.090(3) 0.075(3) 0.053(3) 0.014(2) 0.035(3) 0.012(2) O12 0.191(6) 0.116(4) 0.082(4) 0.044(3) 0.095(4) 0.093(4) N2 0.072(4) 0.063(3) 0.093(5) -0.008(3) 0.030(4) 0.019(3) C26 0.078(5) 0.061(4) 0.038(4) 0.005(3) 0.027(4) 0.006(3) N5 0.064(3) 0.067(3) 0.047(3) 0.007(2) 0.023(3) 0.016(3) N3 0.065(4) 0.084(4) 0.085(5) 0.018(3) 0.035(4) 0.016(3) N8 0.067(4) 0.053(3) 0.048(3) 0.000(2) 0.020(3) 0.000(3) C42 0.068(5) 0.069(4) 0.046(4) 0.003(3) 0.025(3) 0.006(4) N1 0.063(4) 0.065(3) 0.058(3) -0.004(2) 0.025(3) 0.005(3) C23 0.062(5) 0.073(4) 0.085(6) 0.008(4) 0.037(4) 0.011(4) C6 0.082(5) 0.080(4) 0.055(4) 0.016(3) 0.041(4) 0.011(4) C45 0.072(5) 0.070(4) 0.062(5) 0.007(3) 0.015(4) 0.007(4) C2 0.071(5) 0.069(4) 0.042(4) 0.003(3) 0.025(4) -0.007(4) O5 0.128(5) 0.146(5) 0.134(5) 0.072(4) 0.091(4) 0.069(4) C1 0.086(5) 0.069(4) 0.058(4) 0.009(3) 0.039(4) 0.001(4) C47 0.098(6) 0.081(5) 0.098(6) 0.025(4) 0.051(5) 0.018(4) C31 0.111(6) 0.066(4) 0.047(4) 0.007(3) 0.050(4) 0.020(4) C35 0.162(10) 0.089(7) 0.051(5) -0.006(4) 0.037(6) 0.047(7) N4 0.068(4) 0.076(3) 0.072(4) 0.013(3) 0.033(3) 0.014(3) C49 0.075(5) 0.055(4) 0.069(5) 0.004(3) 0.023(4) 0.004(4) C34 0.169(9) 0.103(5) 0.081(6) 0.021(4) 0.070(6) 0.066(6) C46 0.076(5) 0.070(4) 0.088(6) 0.008(4) 0.027(4) 0.013(4) C11 0.108(7) 0.073(5) 0.132(8) -0.024(5) 0.074(6) -0.014(5) C18 0.089(6) 0.065(4) 0.098(6) -0.005(4) 0.050(5) -0.007(4) C10 0.091(6) 0.079(5) 0.105(7) -0.011(5) 0.047(5) -0.008(5) C19 0.076(5) 0.067(4) 0.078(5) -0.005(3) 0.025(4) -0.004(4) C48 0.087(6) 0.051(4) 0.074(5) 0.003(3) 0.016(4) -0.008(4) C50 0.089(6) 0.052(4) 0.052(4) 0.003(3) 0.018(4) -0.002(4) C9 0.122(7) 0.106(6) 0.089(6) 0.018(5) 0.063(6) 0.021(5) C20 0.093(6) 0.082(5) 0.083(6) 0.001(4) 0.027(5) 0.010(4) C22 0.077(5) 0.104(5) 0.091(6) 0.018(4) 0.036(5) 0.026(4) O6 0.162(7) 0.200(7) 0.111(6) 0.039(5) 0.063(5) 0.036(5) C41 0.34(3) 0.098(9) 0.164(13) 0.055(8) 0.167(17) 0.106(13) O13 0.186(9) 0.154(7) 0.337(14) 0.046(7) 0.114(9) 0.053(6) C17 0.090(6) 0.073(4) 0.076(5) 0.001(4) 0.047(4) -0.012(4) C43 0.098(6) 0.128(6) 0.067(5) 0.034(4) 0.035(5) 0.056(5) C16 0.195(13) 0.107(7) 0.192(12) 0.056(7) 0.158(11) 0.069(7) C21 0.100(6) 0.088(5) 0.081(6) 0.010(4) 0.029(5) 0.023(5) C14 0.148(10) 0.138(8) 0.141(10) -0.003(7) 0.092(9) 0.004(7) C13 0.139(9) 0.119(7) 0.144(10) -0.037(7) 0.103(8) -0.017(7) C44 0.110(7) 0.124(6) 0.081(6) 0.009(5) 0.052(6) 0.047(5) C25 0.080(6) 0.159(7) 0.098(7) 0.048(6) 0.040(5) 0.054(6) C15 0.126(8) 0.131(7) 0.131(9) 0.013(6) 0.084(7) 0.029(6) C40 0.153(11) 0.110(8) 0.077(7) 0.001(6) 0.051(7) 0.001(8) O14 0.318(12) 0.172(7) 0.192(9) 0.009(6) 0.152(9) -0.028(8) C24 0.109(7) 0.159(8) 0.109(7) 0.039(6) 0.078(6) 0.040(6) C12 0.133(8) 0.109(6) 0.142(9) -0.019(6) 0.088(8) -0.001(6) C39 0.216(14) 0.129(9) 0.093(8) 0.023(7) 0.071(9) 0.111(11) C36 0.170(11) 0.120(8) 0.080(7) -0.032(6) 0.034(7) 0.049(9) C37 0.197(15) 0.158(11) 0.134(10) -0.050(8) 0.048(9) 0.041(11) C38 0.137(11) 0.233(17) 0.104(10) -0.018(10) 0.028(8) 0.083(12) O1W 0.101(4) 0.133(4) 0.136(5) 0.015(4) 0.037(4) 0.017(4) O2W 0.144(6) 0.242(7) 0.139(6) 0.046(5) 0.092(5) 0.050(5) O3W 0.019(4) 0.222(10) 0.017(4) 0.000(5) 0.012(3) -0.005(5) O4W 0.092(7) 0.070(5) 0.062(6) -0.009(4) 0.053(5) -0.021(5) O7 0.170(11) 0.164(9) 0.357(19) 0.080(10) 0.142(12) 0.084(9) O7' 0.183(12) 0.158(11) 0.179(12) 0.000(9) 0.075(9) 0.013(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.940(4) 4_565 ? Zn1 O1 1.948(4) . ? Zn1 N1 1.974(5) . ? Zn1 N4 1.997(5) 2_545 ? Zn2 O8 1.954(4) . ? Zn2 O11 1.984(4) 4_566 ? Zn2 N8 1.989(5) 2_646 ? Zn2 N5 2.019(5) . ? O10 C27 1.246(6) . ? C8 C7 1.373(7) . ? C8 C3 1.387(7) . ? C8 H8 0.9300 . ? C33 C32 1.382(7) . ? C33 C28 1.387(7) . ? C33 H33 0.9300 . ? O8 C26 1.262(6) . ? C3 C4 1.398(7) . ? C3 C2 1.513(7) . ? N6 C42 1.326(7) . ? N6 C44 1.349(8) . ? N6 C45 1.452(7) . ? C28 C29 1.381(7) . ? C28 C26 1.510(7) . ? O11 C27 1.265(6) . ? O11 Zn2 1.984(4) 4_565 ? O2 C1 1.230(7) . ? N7 C50 1.333(6) . ? N7 C48 1.362(7) . ? N7 C47 1.465(7) . ? C27 C32 1.501(8) . ? C32 C31 1.388(7) . ? C5 C6 1.370(8) . ? C5 O5 1.365(7) . ? C5 C4 1.376(8) . ? O3 C2 1.261(7) . ? O3 Zn1 1.940(4) 4_566 ? C4 H4 0.9300 . ? C7 C6 1.369(8) . ? C7 C1 1.496(8) . ? O9 C26 1.229(6) . ? C30 O12 1.367(7) . ? C30 C29 1.371(7) . ? C30 C31 1.383(8) . ? O4 C2 1.263(7) . ? C29 H29 0.9300 . ? O1 C1 1.279(7) . ? O12 C34 1.419(7) . ? N2 C19 1.337(7) . ? N2 C18 1.350(8) . ? N2 C20 1.496(8) . ? N5 C42 1.306(6) . ? N5 C43 1.367(7) . ? N3 C24 1.353(8) . ? N3 C23 1.353(7) . ? N3 C22 1.463(8) . ? N8 C50 1.311(7) . ? N8 C49 1.355(7) . ? N8 Zn2 1.989(5) 2_656 ? C42 H42 0.9300 . ? N1 C19 1.310(7) . ? N1 C17 1.358(7) . ? C23 N4 1.274(7) . ? C23 H23 0.9300 . ? C6 H6 0.9300 . ? C45 C46 1.502(7) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? O5 C9 1.366(8) . ? C47 C46 1.548(9) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C31 H31 0.9300 . ? C35 C36 1.335(12) . ? C35 C40 1.341(12) . ? C35 C34 1.507(10) . ? N4 C25 1.339(8) . ? N4 Zn1 1.997(5) 2 ? C49 C48 1.340(8) . ? C49 H49 0.9300 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C11 C12 1.372(9) . ? C11 C10 1.428(10) . ? C11 C16 1.454(12) . ? C18 C17 1.341(8) . ? C18 H18 0.9300 . ? C10 C15 1.371(10) . ? C10 C9 1.541(9) . ? C19 H19 0.9300 . ? C48 H48 0.9300 . ? C50 H50 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C20 C21 1.486(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C22 C21 1.537(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? O6 C16 1.136(9) . ? C41 O13 1.185(16) . ? C41 O14 1.395(13) . ? C41 C40 1.47(2) . ? C17 H17 0.9300 . ? C43 C44 1.352(9) . ? C43 H43 0.9300 . ? C16 O7 1.567(17) . ? C16 O7' 1.61(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C14 C15 1.367(10) . ? C14 C13 1.365(12) . ? C14 H14 0.9300 . ? C13 C12 1.382(12) . ? C13 H13 0.9300 . ? C44 H44 0.9300 . ? C25 C24 1.325(10) . ? C25 H25 0.9300 . ? C15 H15 0.9300 . ? C40 C39 1.412(14) . ? O14 H14A 0.8200 . ? C24 H24 0.9300 . ? C12 H12 0.9300 . ? C39 C38 1.324(15) . ? C39 H39 0.9300 . ? C36 C37 1.350(14) . ? C36 H36 0.9300 . ? C37 C38 1.334(15) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 108.80(17) 4_565 . ? O3 Zn1 N1 114.73(19) 4_565 . ? O1 Zn1 N1 114.65(19) . . ? O3 Zn1 N4 101.5(2) 4_565 2_545 ? O1 Zn1 N4 108.5(2) . 2_545 ? N1 Zn1 N4 107.7(2) . 2_545 ? O8 Zn2 O11 107.61(17) . 4_566 ? O8 Zn2 N8 107.23(17) . 2_646 ? O11 Zn2 N8 124.53(17) 4_566 2_646 ? O8 Zn2 N5 98.92(18) . . ? O11 Zn2 N5 108.91(18) 4_566 . ? N8 Zn2 N5 106.7(2) 2_646 . ? C7 C8 C3 120.0(5) . . ? C7 C8 H8 120.0 . . ? C3 C8 H8 120.0 . . ? C32 C33 C28 119.8(5) . . ? C32 C33 H33 120.1 . . ? C28 C33 H33 120.1 . . ? C26 O8 Zn2 117.0(3) . . ? C4 C3 C8 120.2(5) . . ? C4 C3 C2 120.6(6) . . ? C8 C3 C2 119.2(6) . . ? C42 N6 C44 106.7(6) . . ? C42 N6 C45 127.5(5) . . ? C44 N6 C45 125.8(6) . . ? C29 C28 C33 119.2(5) . . ? C29 C28 C26 121.7(5) . . ? C33 C28 C26 119.1(5) . . ? C27 O11 Zn2 107.9(4) . 4_565 ? C50 N7 C48 106.5(6) . . ? C50 N7 C47 124.7(6) . . ? C48 N7 C47 128.8(5) . . ? O10 C27 O11 121.2(6) . . ? O10 C27 C32 119.7(5) . . ? O11 C27 C32 119.1(6) . . ? C33 C32 C31 120.5(5) . . ? C33 C32 C27 119.6(5) . . ? C31 C32 C27 119.9(5) . . ? C6 C5 O5 113.6(6) . . ? C6 C5 C4 121.6(6) . . ? O5 C5 C4 124.8(7) . . ? C2 O3 Zn1 122.5(4) . 4_566 ? C5 C4 C3 118.1(6) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C6 C7 C8 120.2(5) . . ? C6 C7 C1 119.5(5) . . ? C8 C7 C1 120.4(6) . . ? O12 C30 C29 115.1(5) . . ? O12 C30 C31 125.2(5) . . ? C29 C30 C31 119.7(6) . . ? C30 C29 C28 121.3(6) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C1 O1 Zn1 118.0(4) . . ? C30 O12 C34 116.3(5) . . ? C19 N2 C18 107.3(5) . . ? C19 N2 C20 124.1(6) . . ? C18 N2 C20 128.5(6) . . ? O9 C26 O8 123.5(5) . . ? O9 C26 C28 120.2(6) . . ? O8 C26 C28 116.3(5) . . ? C42 N5 C43 104.8(5) . . ? C42 N5 Zn2 126.4(4) . . ? C43 N5 Zn2 128.7(4) . . ? C24 N3 C23 105.1(6) . . ? C24 N3 C22 128.8(6) . . ? C23 N3 C22 126.0(6) . . ? C50 N8 C49 105.3(5) . . ? C50 N8 Zn2 122.5(4) . 2_656 ? C49 N8 Zn2 132.1(5) . 2_656 ? N5 C42 N6 112.5(5) . . ? N5 C42 H42 123.7 . . ? N6 C42 H42 123.7 . . ? C19 N1 C17 105.1(5) . . ? C19 N1 Zn1 125.1(5) . . ? C17 N1 Zn1 129.8(5) . . ? N4 C23 N3 112.3(6) . . ? N4 C23 H23 123.9 . . ? N3 C23 H23 123.9 . . ? C5 C6 C7 120.0(6) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? N6 C45 C46 110.6(5) . . ? N6 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? N6 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? O4 C2 O3 123.8(5) . . ? O4 C2 C3 118.7(6) . . ? O3 C2 C3 117.5(6) . . ? C9 O5 C5 121.0(5) . . ? O2 C1 O1 121.8(6) . . ? O2 C1 C7 121.6(6) . . ? O1 C1 C7 116.5(6) . . ? N7 C47 C46 112.5(5) . . ? N7 C47 H47A 109.1 . . ? C46 C47 H47A 109.1 . . ? N7 C47 H47B 109.1 . . ? C46 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C30 C31 C32 119.6(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C36 C35 C40 116.5(10) . . ? C36 C35 C34 117.4(9) . . ? C40 C35 C34 126.1(12) . . ? C23 N4 C25 105.4(6) . . ? C23 N4 Zn1 128.5(5) . 2 ? C25 N4 Zn1 125.9(5) . 2 ? C48 C49 N8 110.0(6) . . ? C48 C49 H49 125.0 . . ? N8 C49 H49 125.0 . . ? O12 C34 C35 106.9(6) . . ? O12 C34 H34A 110.3 . . ? C35 C34 H34A 110.3 . . ? O12 C34 H34B 110.3 . . ? C35 C34 H34B 110.3 . . ? H34A C34 H34B 108.6 . . ? C45 C46 C47 113.0(6) . . ? C45 C46 H46A 109.0 . . ? C47 C46 H46A 109.0 . . ? C45 C46 H46B 109.0 . . ? C47 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C12 C11 C10 117.4(9) . . ? C12 C11 C16 121.4(9) . . ? C10 C11 C16 121.2(8) . . ? C17 C18 N2 106.0(6) . . ? C17 C18 H18 127.0 . . ? N2 C18 H18 127.0 . . ? C15 C10 C11 118.3(7) . . ? C15 C10 C9 120.1(8) . . ? C11 C10 C9 121.6(8) . . ? N1 C19 N2 111.3(6) . . ? N1 C19 H19 124.4 . . ? N2 C19 H19 124.4 . . ? C49 C48 N7 106.4(5) . . ? C49 C48 H48 126.8 . . ? N7 C48 H48 126.8 . . ? N8 C50 N7 111.8(6) . . ? N8 C50 H50 124.1 . . ? N7 C50 H50 124.1 . . ? O5 C9 C10 107.5(6) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C21 C20 N2 110.1(6) . . ? C21 C20 H20A 109.6 . . ? N2 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? N2 C20 H20B 109.6 . . ? H20A C20 H20B 108.2 . . ? N3 C22 C21 110.6(6) . . ? N3 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? O13 C41 O14 116(2) . . ? O13 C41 C40 123.8(14) . . ? O14 C41 C40 120.5(15) . . ? C18 C17 N1 110.3(6) . . ? C18 C17 H17 124.8 . . ? N1 C17 H17 124.8 . . ? C44 C43 N5 109.2(6) . . ? C44 C43 H43 125.4 . . ? N5 C43 H43 125.4 . . ? O6 C16 C11 126.6(12) . . ? O6 C16 O7 113.4(12) . . ? C11 C16 O7 117.2(10) . . ? O6 C16 O7' 82.4(11) . . ? C11 C16 O7' 105.8(12) . . ? O7 C16 O7' 98.1(12) . . ? C20 C21 C22 108.8(6) . . ? C20 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? C20 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? C15 C14 C13 116.3(10) . . ? C15 C14 H14 121.8 . . ? C13 C14 H14 121.8 . . ? C14 C13 C12 122.2(9) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C43 C44 N6 106.7(6) . . ? C43 C44 H44 126.7 . . ? N6 C44 H44 126.7 . . ? C24 C25 N4 110.8(7) . . ? C24 C25 H25 124.6 . . ? N4 C25 H25 124.6 . . ? C10 C15 C14 124.4(9) . . ? C10 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? C35 C40 C39 121.6(11) . . ? C35 C40 C41 121.5(12) . . ? C39 C40 C41 116.7(12) . . ? C41 O14 H14A 109.5 . . ? C25 C24 N3 106.3(7) . . ? C25 C24 H24 126.8 . . ? N3 C24 H24 126.8 . . ? C11 C12 C13 121.4(9) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C38 C39 C40 119.2(12) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C35 C36 C37 122.5(11) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C38 C37 C36 121.3(14) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C39 C38 C37 118.8(14) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Zn2 O8 C26 76.1(4) 4_566 . . . ? N8 Zn2 O8 C26 -60.0(4) 2_646 . . . ? N5 Zn2 O8 C26 -170.7(4) . . . . ? C7 C8 C3 C4 -1.3(8) . . . . ? C7 C8 C3 C2 178.7(5) . . . . ? C32 C33 C28 C29 -0.1(9) . . . . ? C32 C33 C28 C26 178.9(5) . . . . ? Zn2 O11 C27 O10 -8.6(6) 4_565 . . . ? Zn2 O11 C27 C32 172.8(4) 4_565 . . . ? C28 C33 C32 C31 1.3(9) . . . . ? C28 C33 C32 C27 -179.0(5) . . . . ? O10 C27 C32 C33 -12.0(8) . . . . ? O11 C27 C32 C33 166.6(5) . . . . ? O10 C27 C32 C31 167.7(6) . . . . ? O11 C27 C32 C31 -13.6(8) . . . . ? C6 C5 C4 C3 -0.1(10) . . . . ? O5 C5 C4 C3 178.1(6) . . . . ? C8 C3 C4 C5 0.3(8) . . . . ? C2 C3 C4 C5 -179.7(5) . . . . ? C3 C8 C7 C6 2.1(8) . . . . ? C3 C8 C7 C1 -177.8(5) . . . . ? O12 C30 C29 C28 -179.2(6) . . . . ? C31 C30 C29 C28 0.0(11) . . . . ? C33 C28 C29 C30 -0.5(10) . . . . ? C26 C28 C29 C30 -179.6(6) . . . . ? O3 Zn1 O1 C1 -172.7(4) 4_565 . . . ? N1 Zn1 O1 C1 57.3(5) . . . . ? N4 Zn1 O1 C1 -63.1(5) 2_545 . . . ? C29 C30 O12 C34 -179.4(7) . . . . ? C31 C30 O12 C34 1.4(11) . . . . ? Zn2 O8 C26 O9 -7.4(8) . . . . ? Zn2 O8 C26 C28 171.4(4) . . . . ? C29 C28 C26 O9 5.0(9) . . . . ? C33 C28 C26 O9 -174.1(5) . . . . ? C29 C28 C26 O8 -173.9(5) . . . . ? C33 C28 C26 O8 7.1(8) . . . . ? O8 Zn2 N5 C42 6.1(5) . . . . ? O11 Zn2 N5 C42 118.2(5) 4_566 . . . ? N8 Zn2 N5 C42 -105.0(5) 2_646 . . . ? O8 Zn2 N5 C43 -170.3(6) . . . . ? O11 Zn2 N5 C43 -58.2(6) 4_566 . . . ? N8 Zn2 N5 C43 78.6(6) 2_646 . . . ? C43 N5 C42 N6 -0.2(7) . . . . ? Zn2 N5 C42 N6 -177.2(4) . . . . ? C44 N6 C42 N5 -0.9(7) . . . . ? C45 N6 C42 N5 178.9(5) . . . . ? O3 Zn1 N1 C19 131.6(5) 4_565 . . . ? O1 Zn1 N1 C19 -101.4(5) . . . . ? N4 Zn1 N1 C19 19.4(6) 2_545 . . . ? O3 Zn1 N1 C17 -49.6(6) 4_565 . . . ? O1 Zn1 N1 C17 77.3(5) . . . . ? N4 Zn1 N1 C17 -161.8(5) 2_545 . . . ? C24 N3 C23 N4 2.9(8) . . . . ? C22 N3 C23 N4 -179.7(6) . . . . ? O5 C5 C6 C7 -177.4(6) . . . . ? C4 C5 C6 C7 0.9(10) . . . . ? C8 C7 C6 C5 -2.0(9) . . . . ? C1 C7 C6 C5 178.0(6) . . . . ? C42 N6 C45 C46 -79.4(7) . . . . ? C44 N6 C45 C46 100.3(7) . . . . ? Zn1 O3 C2 O4 -4.6(8) 4_566 . . . ? Zn1 O3 C2 C3 176.1(3) 4_566 . . . ? C4 C3 C2 O4 1.1(8) . . . . ? C8 C3 C2 O4 -178.9(5) . . . . ? C4 C3 C2 O3 -179.6(5) . . . . ? C8 C3 C2 O3 0.5(8) . . . . ? C6 C5 O5 C9 -165.0(7) . . . . ? C4 C5 O5 C9 16.7(11) . . . . ? Zn1 O1 C1 O2 -3.5(9) . . . . ? Zn1 O1 C1 C7 178.7(4) . . . . ? C6 C7 C1 O2 -177.4(6) . . . . ? C8 C7 C1 O2 2.6(9) . . . . ? C6 C7 C1 O1 0.4(8) . . . . ? C8 C7 C1 O1 -179.6(5) . . . . ? C50 N7 C47 C46 99.1(7) . . . . ? C48 N7 C47 C46 -81.2(8) . . . . ? O12 C30 C31 C32 -179.7(6) . . . . ? C29 C30 C31 C32 1.2(10) . . . . ? C33 C32 C31 C30 -1.9(9) . . . . ? C27 C32 C31 C30 178.4(6) . . . . ? N3 C23 N4 C25 -1.5(8) . . . . ? N3 C23 N4 Zn1 173.2(4) . . . 2 ? C50 N8 C49 C48 0.1(7) . . . . ? Zn2 N8 C49 C48 176.9(4) 2_656 . . . ? C30 O12 C34 C35 170.6(7) . . . . ? C36 C35 C34 O12 -88.5(10) . . . . ? C40 C35 C34 O12 90.5(9) . . . . ? N6 C45 C46 C47 177.4(5) . . . . ? N7 C47 C46 C45 73.9(7) . . . . ? C19 N2 C18 C17 -0.5(8) . . . . ? C20 N2 C18 C17 175.9(6) . . . . ? C12 C11 C10 C15 0.3(11) . . . . ? C16 C11 C10 C15 179.6(9) . . . . ? C12 C11 C10 C9 -179.1(7) . . . . ? C16 C11 C10 C9 0.3(12) . . . . ? C17 N1 C19 N2 0.4(7) . . . . ? Zn1 N1 C19 N2 179.4(4) . . . . ? C18 N2 C19 N1 0.0(8) . . . . ? C20 N2 C19 N1 -176.5(6) . . . . ? N8 C49 C48 N7 -0.2(7) . . . . ? C50 N7 C48 C49 0.2(7) . . . . ? C47 N7 C48 C49 -179.6(6) . . . . ? C49 N8 C50 N7 0.0(6) . . . . ? Zn2 N8 C50 N7 -177.1(3) 2_656 . . . ? C48 N7 C50 N8 -0.1(7) . . . . ? C47 N7 C50 N8 179.7(5) . . . . ? C5 O5 C9 C10 167.7(6) . . . . ? C15 C10 C9 O5 -4.5(10) . . . . ? C11 C10 C9 O5 174.9(7) . . . . ? C19 N2 C20 C21 -99.0(7) . . . . ? C18 N2 C20 C21 85.2(8) . . . . ? C24 N3 C22 C21 -27.5(10) . . . . ? C23 N3 C22 C21 155.8(6) . . . . ? N2 C18 C17 N1 0.7(8) . . . . ? C19 N1 C17 C18 -0.7(7) . . . . ? Zn1 N1 C17 C18 -179.7(5) . . . . ? C42 N5 C43 C44 1.1(8) . . . . ? Zn2 N5 C43 C44 178.1(5) . . . . ? C12 C11 C16 O6 -153.6(11) . . . . ? C10 C11 C16 O6 27.1(17) . . . . ? C12 C11 C16 O7 46.7(13) . . . . ? C10 C11 C16 O7 -132.6(9) . . . . ? C12 C11 C16 O7' -61.4(15) . . . . ? C10 C11 C16 O7' 119.3(12) . . . . ? N2 C20 C21 C22 -173.4(6) . . . . ? N3 C22 C21 C20 -179.0(6) . . . . ? C15 C14 C13 C12 0.1(15) . . . . ? N5 C43 C44 N6 -1.7(9) . . . . ? C42 N6 C44 C43 1.6(8) . . . . ? C45 N6 C44 C43 -178.2(6) . . . . ? C23 N4 C25 C24 -0.5(10) . . . . ? Zn1 N4 C25 C24 -175.4(6) 2 . . . ? C11 C10 C15 C14 0.5(14) . . . . ? C9 C10 C15 C14 179.8(8) . . . . ? C13 C14 C15 C10 -0.7(15) . . . . ? C36 C35 C40 C39 -0.4(13) . . . . ? C34 C35 C40 C39 -179.4(8) . . . . ? C36 C35 C40 C41 -175.2(10) . . . . ? C34 C35 C40 C41 5.8(14) . . . . ? O13 C41 C40 C35 -31.3(17) . . . . ? O14 C41 C40 C35 151.6(9) . . . . ? O13 C41 C40 C39 153.7(12) . . . . ? O14 C41 C40 C39 -23.4(15) . . . . ? N4 C25 C24 N3 2.3(11) . . . . ? C23 N3 C24 C25 -3.0(9) . . . . ? C22 N3 C24 C25 179.7(7) . . . . ? C10 C11 C12 C13 -0.8(12) . . . . ? C16 C11 C12 C13 179.9(10) . . . . ? C14 C13 C12 C11 0.6(15) . . . . ? C35 C40 C39 C38 2.7(16) . . . . ? C41 C40 C39 C38 177.7(11) . . . . ? C40 C35 C36 C37 -0.2(15) . . . . ? C34 C35 C36 C37 179.0(8) . . . . ? C35 C36 C37 C38 -1.6(18) . . . . ? C40 C39 C38 C37 -4.4(19) . . . . ? C36 C37 C38 C39 4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.644 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.076 #========================================================= data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 843916' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 N4 O7 Zn' _chemical_formula_sum 'C26 H24 N4 O7 Zn' _chemical_formula_weight 569.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 20.322(5) _cell_length_b 7.679(5) _cell_length_c 16.703(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 2607(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3530 _cell_measurement_theta_min 2.9138 _cell_measurement_theta_max 29.0988 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98086 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11792 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 29.16 _reflns_number_total 4844 _reflns_number_gt 3842 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0670P)^2^+1.2338P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(18) _refine_ls_number_reflns 4844 _refine_ls_number_parameters 344 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.31237(2) 0.86361(6) 1.31864(4) 0.03802(16) Uani 1 1 d . . . C3 C 0.3353(2) 1.2879(6) 1.4753(3) 0.0365(10) Uani 1 1 d . . . N1 N 0.40568(19) 0.7883(5) 1.3041(2) 0.0425(10) Uani 1 1 d . . . O2 O 0.37061(19) 1.2244(4) 1.3429(2) 0.0526(9) Uani 1 1 d . . . O4 O 0.23583(16) 1.4413(4) 1.7241(2) 0.0460(8) Uani 1 1 d . . . C8 C 0.3771(3) 1.4299(7) 1.4832(3) 0.0443(12) Uani 1 1 d . . . H8 H 0.4066 1.4552 1.4423 0.053 Uiso 1 1 calc R . . O5 O 0.4173(2) 1.6702(6) 1.5645(3) 0.0762(14) Uani 1 1 d . . . O3 O 0.2138(2) 1.1792(5) 1.6752(2) 0.0544(9) Uani 1 1 d . . . N4 N 0.7547(2) -0.1744(5) 1.3630(3) 0.0474(10) Uani 1 1 d . . . C15 C 0.5647(3) 1.8409(6) 1.5830(3) 0.0475(12) Uani 1 1 d . . . C1 C 0.3385(2) 1.1754(6) 1.4017(3) 0.0375(10) Uani 1 1 d . . . C4 C 0.2919(2) 1.2506(6) 1.5375(3) 0.0403(10) Uani 1 1 d . . . H4 H 0.2647 1.1535 1.5344 0.048 Uiso 1 1 calc R . . C5 C 0.2893(2) 1.3598(6) 1.6047(3) 0.0385(10) Uani 1 1 d . . . O1 O 0.30704(16) 1.0337(4) 1.4057(2) 0.0470(8) Uani 1 1 d . . . C6 C 0.3300(3) 1.5004(7) 1.6097(3) 0.0472(12) Uani 1 1 d . . . H6 H 0.3270 1.5749 1.6534 0.057 Uiso 1 1 calc R . . C7 C 0.3759(3) 1.5335(7) 1.5499(3) 0.0490(12) Uani 1 1 d . . . C10 C 0.5067(3) 1.8570(7) 1.5414(4) 0.0540(15) Uani 1 1 d . . . N3 N 0.6954(2) 0.0618(6) 1.3762(3) 0.0572(13) Uani 1 1 d . . . N2 N 0.4884(2) 0.6147(6) 1.2837(3) 0.0584(12) Uani 1 1 d . . . C2 C 0.2428(2) 1.3217(7) 1.6719(3) 0.0413(11) Uani 1 1 d . . . C17 C 0.4239(3) 0.6277(7) 1.2931(3) 0.0497(13) Uani 1 1 d . . . H17 H 0.3951 0.5335 1.2921 0.060 Uiso 1 1 calc R . . C22 C 0.6061(3) 0.2445(7) 1.3237(6) 0.0740(16) Uani 1 1 d . . . H22A H 0.5753 0.1676 1.3506 0.089 Uiso 1 1 calc R . . H22B H 0.6110 0.2047 1.2689 0.089 Uiso 1 1 calc R . . C18 C 0.4619(2) 0.8845(7) 1.3009(4) 0.0600(19) Uani 1 1 d . . . H18 H 0.4640 1.0049 1.3064 0.072 Uiso 1 1 calc R . . O6 O 0.5999(3) 1.5608(7) 1.5329(4) 0.0999(16) Uani 1 1 d . . . C14 C 0.5964(3) 1.9887(8) 1.6129(4) 0.0617(16) Uani 1 1 d . . . H14 H 0.6352 1.9769 1.6420 0.074 Uiso 1 1 calc R . . C13 C 0.5706(4) 2.1504(7) 1.5995(4) 0.0657(17) Uani 1 1 d . . . H13 H 0.5921 2.2493 1.6181 0.079 Uiso 1 1 calc R . . C19 C 0.5137(3) 0.7795(9) 1.2888(4) 0.073(2) Uani 1 1 d . . . H19 H 0.5577 0.8120 1.2848 0.088 Uiso 1 1 calc R . . C9 C 0.4669(3) 1.7059(8) 1.5094(4) 0.0648(16) Uani 1 1 d . . . H9A H 0.4480 1.7358 1.4579 0.078 Uiso 1 1 calc R . . H9B H 0.4949 1.6046 1.5025 0.078 Uiso 1 1 calc R . . C20 C 0.5246(4) 0.4500(9) 1.2718(4) 0.0748(18) Uani 1 1 d . . . H20A H 0.4944 0.3536 1.2796 0.090 Uiso 1 1 calc R . . H20B H 0.5400 0.4451 1.2169 0.090 Uiso 1 1 calc R . . C26 C 0.7410(3) -0.0162(6) 1.3354(3) 0.0523(14) Uani 1 1 d . . . H26 H 0.7619 0.0333 1.2915 0.063 Uiso 1 1 calc R . . C12 C 0.5134(4) 2.1649(8) 1.5591(6) 0.088(3) Uani 1 1 d . . . H12 H 0.4960 2.2751 1.5499 0.106 Uiso 1 1 calc R . . C23 C 0.6700(3) 0.2374(8) 1.3643(5) 0.079(2) Uani 1 1 d . . . H23A H 0.7016 0.3033 1.3332 0.095 Uiso 1 1 calc R . . H23B H 0.6659 0.2936 1.4161 0.095 Uiso 1 1 calc R . . C11 C 0.4801(3) 2.0213(8) 1.5309(5) 0.0733(18) Uani 1 1 d . . . H11 H 0.4399 2.0347 1.5049 0.088 Uiso 1 1 calc R . . C16 C 0.5997(4) 1.6696(8) 1.5903(4) 0.0682(18) Uani 1 1 d . . . C21 C 0.5793(3) 0.4282(8) 1.3240(6) 0.0817(19) Uani 1 1 d . . . H21A H 0.5660 0.4583 1.3781 0.098 Uiso 1 1 calc R . . H21B H 0.6139 0.5079 1.3081 0.098 Uiso 1 1 calc R . . C24 C 0.6781(4) -0.0465(11) 1.4347(5) 0.100(3) Uani 1 1 d . . . H24 H 0.6467 -0.0257 1.4740 0.120 Uiso 1 1 calc R . . O7 O 0.6399(4) 1.6491(8) 1.6509(4) 0.123(3) Uani 1 1 d . . . H7 H 0.6562 1.5516 1.6491 0.184 Uiso 1 1 calc R . . C25 C 0.7148(4) -0.1931(10) 1.4261(5) 0.089(2) Uani 1 1 d . . . H25 H 0.7126 -0.2909 1.4588 0.107 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 0.0399(3) 0.0366(2) 0.0376(3) -0.0072(3) -0.0019(3) -0.0029(2) C3 0.038(2) 0.033(2) 0.038(3) -0.003(2) -0.002(2) 0.000(2) N1 0.042(2) 0.0410(19) 0.045(3) -0.0033(18) 0.0002(18) 0.0030(16) O2 0.068(2) 0.0436(18) 0.046(2) -0.0134(15) 0.0137(17) -0.0037(17) O4 0.053(2) 0.0431(18) 0.0413(17) -0.0064(16) 0.0091(16) -0.0039(16) C8 0.050(3) 0.049(3) 0.034(3) -0.007(2) 0.006(2) 0.001(2) O5 0.084(3) 0.078(3) 0.067(3) -0.033(2) 0.027(2) -0.048(2) O3 0.061(2) 0.055(2) 0.047(2) -0.0072(18) 0.0061(18) -0.0181(19) N4 0.047(2) 0.042(2) 0.053(2) 0.0057(19) 0.000(2) 0.0087(19) C15 0.050(3) 0.045(3) 0.047(3) 0.003(2) -0.003(2) -0.009(2) C1 0.036(2) 0.040(2) 0.037(3) -0.011(2) -0.003(2) -0.002(2) C4 0.044(3) 0.037(2) 0.040(3) -0.007(2) -0.003(2) -0.001(2) C5 0.039(2) 0.044(3) 0.033(2) -0.005(2) -0.003(2) -0.002(2) O1 0.056(2) 0.0446(19) 0.0405(19) -0.0161(16) 0.0025(16) -0.0130(16) C6 0.053(3) 0.044(3) 0.045(3) -0.016(2) 0.000(2) -0.004(2) C7 0.055(3) 0.046(3) 0.046(3) -0.009(2) -0.001(2) -0.014(2) C10 0.056(3) 0.052(3) 0.054(4) -0.003(3) -0.002(3) -0.012(3) N3 0.047(3) 0.048(2) 0.077(4) -0.002(3) -0.001(2) 0.015(2) N2 0.055(3) 0.046(2) 0.074(3) -0.002(2) 0.001(2) 0.015(2) C2 0.040(3) 0.048(3) 0.036(3) -0.006(2) -0.006(2) 0.002(2) C17 0.056(3) 0.047(3) 0.046(3) -0.006(2) -0.007(2) 0.001(2) C22 0.062(3) 0.063(3) 0.097(5) -0.007(4) -0.011(4) 0.018(3) C18 0.046(3) 0.045(3) 0.090(6) -0.005(3) -0.002(3) -0.001(2) O6 0.129(5) 0.067(3) 0.104(4) -0.012(3) -0.016(4) 0.003(3) C14 0.064(4) 0.054(3) 0.067(4) 0.000(3) -0.018(3) -0.013(3) C13 0.082(5) 0.044(3) 0.072(4) -0.004(3) -0.016(4) -0.011(3) C19 0.039(3) 0.068(4) 0.112(6) 0.001(4) 0.006(3) 0.001(3) C9 0.070(4) 0.063(3) 0.062(4) -0.015(3) -0.007(3) -0.021(3) C20 0.079(5) 0.069(4) 0.076(4) -0.012(4) 0.005(4) 0.021(3) C26 0.052(3) 0.043(2) 0.062(4) 0.006(2) -0.002(2) 0.006(2) C12 0.101(6) 0.047(3) 0.116(7) -0.007(4) -0.036(5) 0.015(4) C23 0.064(4) 0.051(3) 0.123(6) -0.021(4) -0.018(4) 0.016(3) C11 0.070(4) 0.053(3) 0.097(5) -0.007(3) -0.031(4) 0.003(3) C16 0.080(5) 0.050(3) 0.075(4) -0.007(3) -0.015(4) 0.002(3) C21 0.069(4) 0.069(3) 0.108(5) -0.020(5) -0.017(5) 0.022(3) C24 0.095(6) 0.090(5) 0.116(7) 0.027(5) 0.067(5) 0.028(5) O7 0.154(7) 0.110(5) 0.105(5) 0.001(4) -0.051(5) 0.042(4) C25 0.112(6) 0.071(4) 0.085(5) 0.029(4) 0.052(5) 0.031(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 1.952(3) 3_544 ? Zn1 O1 1.958(3) . ? Zn1 N1 1.998(4) . ? Zn1 N4 2.009(4) 4_455 ? C3 C8 1.388(7) . ? C3 C4 1.392(7) . ? C3 C1 1.505(7) . ? N1 C17 1.300(6) . ? N1 C18 1.361(6) . ? O2 C1 1.237(6) . ? O4 C2 1.275(6) . ? O4 Zn1 1.952(3) 3 ? C8 C7 1.369(7) . ? C8 H8 0.9300 . ? O5 C7 1.368(6) . ? O5 C9 1.391(7) . ? O3 C2 1.244(6) . ? N4 C26 1.328(6) . ? N4 C25 1.336(8) . ? N4 Zn1 2.009(4) 4 ? C15 C10 1.374(9) . ? C15 C14 1.398(7) . ? C15 C16 1.501(8) . ? C1 O1 1.264(6) . ? C4 C5 1.403(6) . ? C4 H4 0.9300 . ? C5 C6 1.362(7) . ? C5 C2 1.495(7) . ? C6 C7 1.390(7) . ? C6 H6 0.9300 . ? C10 C11 1.384(8) . ? C10 C9 1.511(8) . ? N3 C26 1.296(7) . ? N3 C24 1.330(9) . ? N3 C23 1.458(8) . ? N2 C17 1.326(7) . ? N2 C19 1.369(8) . ? N2 C20 1.476(7) . ? C17 H17 0.9300 . ? C22 C23 1.466(9) . ? C22 C21 1.513(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C18 C19 1.342(8) . ? C18 H18 0.9300 . ? O6 C16 1.272(8) . ? C14 C13 1.367(8) . ? C14 H14 0.9300 . ? C13 C12 1.349(10) . ? C13 H13 0.9300 . ? C19 H19 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C20 C21 1.423(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C26 H26 0.9300 . ? C12 C11 1.377(9) . ? C12 H12 0.9300 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C11 H11 0.9300 . ? C16 O7 1.310(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C24 C25 1.358(10) . ? C24 H24 0.9300 . ? O7 H7 0.8200 . ? C25 H25 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O1 111.68(15) 3_544 . ? O4 Zn1 N1 117.79(16) 3_544 . ? O1 Zn1 N1 109.65(15) . . ? O4 Zn1 N4 103.10(17) 3_544 4_455 ? O1 Zn1 N4 100.15(17) . 4_455 ? N1 Zn1 N4 112.94(17) . 4_455 ? C8 C3 C4 118.6(4) . . ? C8 C3 C1 120.2(4) . . ? C4 C3 C1 121.3(4) . . ? C17 N1 C18 105.7(4) . . ? C17 N1 Zn1 124.2(3) . . ? C18 N1 Zn1 130.1(3) . . ? C2 O4 Zn1 112.9(3) . 3 ? C7 C8 C3 121.5(5) . . ? C7 C8 H8 119.2 . . ? C3 C8 H8 119.2 . . ? C7 O5 C9 118.7(4) . . ? C26 N4 C25 104.2(5) . . ? C26 N4 Zn1 130.9(4) . 4 ? C25 N4 Zn1 124.5(4) . 4 ? C10 C15 C14 120.3(5) . . ? C10 C15 C16 121.8(5) . . ? C14 C15 C16 117.6(5) . . ? O2 C1 O1 124.8(4) . . ? O2 C1 C3 119.8(4) . . ? O1 C1 C3 115.4(4) . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.9(5) . . ? C6 C5 C2 119.5(4) . . ? C4 C5 C2 120.5(4) . . ? C1 O1 Zn1 120.4(3) . . ? C5 C6 C7 120.6(5) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? O5 C7 C8 125.4(5) . . ? O5 C7 C6 115.2(4) . . ? C8 C7 C6 119.4(5) . . ? C15 C10 C11 118.8(5) . . ? C15 C10 C9 124.6(5) . . ? C11 C10 C9 116.5(6) . . ? C26 N3 C24 106.6(5) . . ? C26 N3 C23 127.6(6) . . ? C24 N3 C23 125.8(6) . . ? C17 N2 C19 107.1(4) . . ? C17 N2 C20 125.0(5) . . ? C19 N2 C20 127.9(5) . . ? O3 C2 O4 123.4(5) . . ? O3 C2 C5 120.3(4) . . ? O4 C2 C5 116.3(4) . . ? N1 C17 N2 111.7(5) . . ? N1 C17 H17 124.2 . . ? N2 C17 H17 124.2 . . ? C23 C22 C21 110.6(5) . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C19 C18 N1 109.8(5) . . ? C19 C18 H18 125.1 . . ? N1 C18 H18 125.1 . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C12 C13 C14 119.2(6) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C18 C19 N2 105.7(5) . . ? C18 C19 H19 127.1 . . ? N2 C19 H19 127.1 . . ? O5 C9 C10 107.7(5) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C21 C20 N2 114.0(6) . . ? C21 C20 H20A 108.7 . . ? N2 C20 H20A 108.7 . . ? C21 C20 H20B 108.7 . . ? N2 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? N3 C26 N4 112.9(5) . . ? N3 C26 H26 123.5 . . ? N4 C26 H26 123.5 . . ? C13 C12 C11 122.0(6) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? N3 C23 C22 114.3(5) . . ? N3 C23 H23A 108.7 . . ? C22 C23 H23A 108.7 . . ? N3 C23 H23B 108.7 . . ? C22 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C12 C11 C10 119.6(6) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? O6 C16 O7 120.1(6) . . ? O6 C16 C15 121.1(6) . . ? O7 C16 C15 117.7(6) . . ? C20 C21 C22 112.9(6) . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? N3 C24 C25 107.2(6) . . ? N3 C24 H24 126.4 . . ? C25 C24 H24 126.4 . . ? C16 O7 H7 109.5 . . ? N4 C25 C24 109.1(6) . . ? N4 C25 H25 125.5 . . ? C24 C25 H25 125.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Zn1 N1 C17 -94.5(4) 3_544 . . . ? O1 Zn1 N1 C17 136.4(4) . . . . ? N4 Zn1 N1 C17 25.6(5) 4_455 . . . ? O4 Zn1 N1 C18 83.5(5) 3_544 . . . ? O1 Zn1 N1 C18 -45.6(5) . . . . ? N4 Zn1 N1 C18 -156.4(5) 4_455 . . . ? C4 C3 C8 C7 -0.7(8) . . . . ? C1 C3 C8 C7 -179.3(5) . . . . ? C8 C3 C1 O2 -11.4(7) . . . . ? C4 C3 C1 O2 170.0(5) . . . . ? C8 C3 C1 O1 168.3(5) . . . . ? C4 C3 C1 O1 -10.2(7) . . . . ? C8 C3 C4 C5 2.6(7) . . . . ? C1 C3 C4 C5 -178.8(4) . . . . ? C3 C4 C5 C6 -1.1(7) . . . . ? C3 C4 C5 C2 179.8(4) . . . . ? O2 C1 O1 Zn1 5.0(7) . . . . ? C3 C1 O1 Zn1 -174.7(3) . . . . ? O4 Zn1 O1 C1 -72.6(4) 3_544 . . . ? N1 Zn1 O1 C1 59.9(4) . . . . ? N4 Zn1 O1 C1 178.8(4) 4_455 . . . ? C4 C5 C6 C7 -2.4(8) . . . . ? C2 C5 C6 C7 176.7(5) . . . . ? C9 O5 C7 C8 -2.6(9) . . . . ? C9 O5 C7 C6 176.7(6) . . . . ? C3 C8 C7 O5 176.6(6) . . . . ? C3 C8 C7 C6 -2.7(8) . . . . ? C5 C6 C7 O5 -175.1(5) . . . . ? C5 C6 C7 C8 4.3(8) . . . . ? C14 C15 C10 C11 -0.9(9) . . . . ? C16 C15 C10 C11 -174.2(6) . . . . ? C14 C15 C10 C9 -177.4(6) . . . . ? C16 C15 C10 C9 9.2(9) . . . . ? Zn1 O4 C2 O3 10.1(6) 3 . . . ? Zn1 O4 C2 C5 -169.2(3) 3 . . . ? C6 C5 C2 O3 -167.4(5) . . . . ? C4 C5 C2 O3 11.7(7) . . . . ? C6 C5 C2 O4 12.0(7) . . . . ? C4 C5 C2 O4 -169.0(4) . . . . ? C18 N1 C17 N2 0.4(6) . . . . ? Zn1 N1 C17 N2 178.8(4) . . . . ? C19 N2 C17 N1 -0.1(7) . . . . ? C20 N2 C17 N1 178.7(5) . . . . ? C17 N1 C18 C19 -0.6(7) . . . . ? Zn1 N1 C18 C19 -178.9(4) . . . . ? C10 C15 C14 C13 -1.4(9) . . . . ? C16 C15 C14 C13 172.3(6) . . . . ? C15 C14 C13 C12 1.7(11) . . . . ? N1 C18 C19 N2 0.6(8) . . . . ? C17 N2 C19 C18 -0.3(7) . . . . ? C20 N2 C19 C18 -179.0(6) . . . . ? C7 O5 C9 C10 -177.8(5) . . . . ? C15 C10 C9 O5 97.1(8) . . . . ? C11 C10 C9 O5 -79.5(8) . . . . ? C17 N2 C20 C21 -129.5(7) . . . . ? C19 N2 C20 C21 49.0(10) . . . . ? C24 N3 C26 N4 1.0(8) . . . . ? C23 N3 C26 N4 177.8(5) . . . . ? C25 N4 C26 N3 -0.8(7) . . . . ? Zn1 N4 C26 N3 172.6(4) 4 . . . ? C14 C13 C12 C11 0.1(13) . . . . ? C26 N3 C23 C22 102.4(9) . . . . ? C24 N3 C23 C22 -81.3(10) . . . . ? C21 C22 C23 N3 172.3(7) . . . . ? C13 C12 C11 C10 -2.4(13) . . . . ? C15 C10 C11 C12 2.7(10) . . . . ? C9 C10 C11 C12 179.5(8) . . . . ? C10 C15 C16 O6 35.7(9) . . . . ? C14 C15 C16 O6 -137.8(7) . . . . ? C10 C15 C16 O7 -156.7(8) . . . . ? C14 C15 C16 O7 29.8(10) . . . . ? N2 C20 C21 C22 167.3(7) . . . . ? C23 C22 C21 C20 167.9(8) . . . . ? C26 N3 C24 C25 -0.8(9) . . . . ? C23 N3 C24 C25 -177.7(7) . . . . ? C26 N4 C25 C24 0.2(9) . . . . ? Zn1 N4 C25 C24 -173.7(6) 4 . . . ? N3 C24 C25 N4 0.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.704 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.068 #========================================================= data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 843917' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Co N4 O7' _chemical_formula_sum 'C26 H24 Co N4 O7' _chemical_formula_weight 563.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6973(6) _cell_length_b 11.1543(7) _cell_length_c 11.5573(7) _cell_angle_alpha 92.228(5) _cell_angle_beta 94.339(5) _cell_angle_gamma 95.885(5) _cell_volume 1238.59(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2478 _cell_measurement_theta_min 2.9420 _cell_measurement_theta_max 29.1661 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 582 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96889 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8841 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 29.23 _reflns_number_total 5626 _reflns_number_gt 4123 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0393P)^2^+1.2340P] 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 5626 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.30655(4) 0.11116(4) 0.29146(4) 0.02752(14) Uani 1 1 d . . . O5 O -0.1049(2) 0.2558(2) 0.7354(2) 0.0380(6) Uani 1 1 d . . . O4 O -0.5311(2) 0.2185(2) 0.4587(2) 0.0405(6) Uani 1 1 d . . . O1 O 0.1710(2) 0.1101(2) 0.4102(2) 0.0329(5) Uani 1 1 d . . . O2 O 0.0184(3) 0.0919(3) 0.2575(2) 0.0643(9) Uani 1 1 d . . . O3 O -0.4960(2) 0.0743(2) 0.3329(2) 0.0338(5) Uani 1 1 d . . . N2 N 0.3215(3) -0.1118(3) -0.0044(2) 0.0329(6) Uani 1 1 d . . . O7 O 0.3376(3) 0.2101(3) 0.8615(3) 0.0609(8) Uani 1 1 d . . . C7 C -0.0643(3) 0.1339(3) 0.4404(3) 0.0249(7) Uani 1 1 d . . . O6 O 0.3683(4) 0.1557(3) 0.6771(3) 0.0763(10) Uani 1 1 d . . . H6A H 0.3575 0.1846 0.6133 0.114 Uiso 1 1 calc R . . N1 N 0.2792(3) 0.0027(3) 0.1443(2) 0.0326(6) Uani 1 1 d . . . C10 C 0.1303(3) 0.3583(3) 0.7286(3) 0.0357(8) Uani 1 1 d . . . C18 C 0.1710(4) -0.0026(4) 0.0613(3) 0.0484(10) Uani 1 1 d . . . H18 H 0.0914 0.0364 0.0675 0.058 Uiso 1 1 calc R . . C3 C -0.3050(3) 0.1547(3) 0.4654(3) 0.0255(7) Uani 1 1 d . . . C11 C 0.2683(3) 0.3403(3) 0.7136(3) 0.0349(8) Uani 1 1 d . . . C5 C -0.1304(3) 0.2093(3) 0.6235(3) 0.0285(7) Uani 1 1 d . . . C9 C 0.0361(3) 0.2652(4) 0.7850(3) 0.0402(9) Uani 1 1 d . . . H9A H 0.0713 0.1873 0.7769 0.048 Uiso 1 1 calc R . . H9B H 0.0380 0.2865 0.8674 0.048 Uiso 1 1 calc R . . C2 C -0.4533(3) 0.1494(3) 0.4175(3) 0.0275(7) Uani 1 1 d . . . C8 C -0.2023(3) 0.1220(3) 0.3958(3) 0.0276(7) Uani 1 1 d . . . H8 H -0.2261 0.0924 0.3198 0.033 Uiso 1 1 calc R . . C20 C 0.3925(4) -0.1921(3) -0.0777(3) 0.0425(9) Uani 1 1 d . . . H20A H 0.4871 -0.1942 -0.0445 0.051 Uiso 1 1 calc R . . H20B H 0.3969 -0.1600 -0.1543 0.051 Uiso 1 1 calc R . . C16 C 0.3282(3) 0.2304(3) 0.7586(3) 0.0368(8) Uani 1 1 d . . . C14 C 0.1631(5) 0.5437(4) 0.6280(5) 0.0620(13) Uani 1 1 d . . . H14 H 0.1268 0.6115 0.5989 0.074 Uiso 1 1 calc R . . C21 C 0.3202(5) -0.3186(4) -0.0892(4) 0.0602(12) Uani 1 1 d . . . H21A H 0.3620 -0.3650 -0.1473 0.072 Uiso 1 1 calc R . . H21B H 0.2231 -0.3161 -0.1150 0.072 Uiso 1 1 calc R . . C4 C -0.2681(3) 0.1992(3) 0.5782(3) 0.0292(7) Uani 1 1 d . . . H4 H -0.3363 0.2227 0.6241 0.035 Uiso 1 1 calc R . . C15 C 0.0806(4) 0.4606(4) 0.6847(4) 0.0518(11) Uani 1 1 d . . . H15 H -0.0113 0.4738 0.6937 0.062 Uiso 1 1 calc R . . C6 C -0.0286(3) 0.1752(3) 0.5541(3) 0.0283(7) Uani 1 1 d . . . H6 H 0.0636 0.1803 0.5842 0.034 Uiso 1 1 calc R . . C13 C 0.3000(5) 0.5256(4) 0.6145(4) 0.0590(12) Uani 1 1 d . . . H13 H 0.3568 0.5817 0.5774 0.071 Uiso 1 1 calc R . . C19 C 0.1958(4) -0.0723(4) -0.0308(3) 0.0481(10) Uani 1 1 d . . . H19 H 0.1384 -0.0899 -0.0988 0.058 Uiso 1 1 calc R . . C17 C 0.3682(3) -0.0648(3) 0.1002(3) 0.0327(8) Uani 1 1 d . . . H17 H 0.4532 -0.0778 0.1378 0.039 Uiso 1 1 calc R . . C1 C 0.0480(3) 0.1091(3) 0.3619(3) 0.0312(7) Uani 1 1 d . . . C12 C 0.3512(4) 0.4241(4) 0.6563(4) 0.0470(10) Uani 1 1 d . . . H12 H 0.4429 0.4112 0.6461 0.056 Uiso 1 1 calc R . . N3 N 0.2702(3) -0.5671(3) 0.1238(3) 0.0465(8) Uani 1 1 d . . . C22 C 0.3307(5) -0.3810(4) 0.0274(4) 0.0666(13) Uani 1 1 d . . . H22A H 0.4273 -0.3909 0.0494 0.080 Uiso 1 1 calc R . . H22B H 0.2975 -0.3305 0.0874 0.080 Uiso 1 1 calc R . . C23 C 0.2482(5) -0.4999(4) 0.0195(4) 0.0667(13) Uani 1 1 d . . . H23A H 0.1503 -0.4889 0.0070 0.080 Uiso 1 1 calc R . . H23B H 0.2732 -0.5464 -0.0470 0.080 Uiso 1 1 calc R . . C24 C 0.2866(4) -0.6848(3) 0.1252(3) 0.0397(9) Uani 1 1 d . . . H24 H 0.2880 -0.7349 0.0592 0.048 Uiso 1 1 calc R . . C26 C 0.2921(4) -0.6187(4) 0.3025(4) 0.0473(10) Uani 1 1 d . . . H26 H 0.2979 -0.6164 0.3833 0.057 Uiso 1 1 calc R . . C25 C 0.2746(4) -0.5249(4) 0.2365(4) 0.0512(10) Uani 1 1 d . . . H25 H 0.2669 -0.4460 0.2624 0.061 Uiso 1 1 calc R . . N4 N 0.3002(3) -0.7195(3) 0.2311(3) 0.0351(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 Co1 0.0192(2) 0.0357(3) 0.0279(3) -0.00306(19) 0.00148(16) 0.00611(16) O5 0.0212(11) 0.0609(17) 0.0303(14) -0.0150(12) -0.0013(9) 0.0045(10) O4 0.0237(12) 0.0567(17) 0.0428(16) -0.0024(13) 0.0034(10) 0.0133(11) O1 0.0170(11) 0.0469(15) 0.0350(14) -0.0004(11) 0.0044(9) 0.0030(9) O2 0.0349(15) 0.129(3) 0.0302(17) -0.0171(17) 0.0016(11) 0.0224(16) O3 0.0212(11) 0.0419(14) 0.0366(14) -0.0046(11) -0.0041(9) 0.0030(9) N2 0.0334(15) 0.0371(17) 0.0281(16) -0.0048(13) 0.0018(12) 0.0065(12) O7 0.071(2) 0.083(2) 0.0319(17) 0.0021(15) -0.0036(14) 0.0283(16) C7 0.0186(14) 0.0266(17) 0.0291(18) -0.0022(13) 0.0022(12) 0.0022(11) O6 0.097(3) 0.078(3) 0.061(2) 0.0080(19) 0.019(2) 0.032(2) N1 0.0263(14) 0.0435(17) 0.0277(16) -0.0059(13) -0.0027(11) 0.0080(12) C10 0.0332(18) 0.037(2) 0.035(2) -0.0097(16) -0.0057(14) 0.0039(14) C18 0.0290(18) 0.075(3) 0.040(2) -0.020(2) -0.0117(15) 0.0192(17) C3 0.0191(15) 0.0297(17) 0.0271(18) -0.0005(14) 0.0003(12) 0.0010(12) C11 0.0352(18) 0.035(2) 0.032(2) -0.0095(15) -0.0054(14) 0.0021(14) C5 0.0242(16) 0.0332(18) 0.0272(18) -0.0039(14) 0.0002(12) 0.0015(12) C9 0.0298(18) 0.055(2) 0.034(2) -0.0076(18) -0.0056(14) 0.0032(15) C2 0.0167(14) 0.0372(19) 0.0286(18) 0.0046(15) 0.0007(12) 0.0030(12) C8 0.0218(15) 0.0352(19) 0.0248(18) -0.0033(14) -0.0007(12) 0.0024(12) C20 0.054(2) 0.043(2) 0.033(2) -0.0018(17) 0.0090(17) 0.0131(17) C16 0.0279(17) 0.049(2) 0.032(2) -0.0039(17) 0.0024(14) 0.0027(15) C14 0.069(3) 0.033(2) 0.083(4) 0.003(2) -0.005(3) 0.011(2) C21 0.096(4) 0.045(3) 0.041(3) -0.006(2) 0.014(2) 0.010(2) C4 0.0198(15) 0.0344(19) 0.034(2) -0.0028(15) 0.0061(13) 0.0043(12) C15 0.042(2) 0.043(2) 0.070(3) -0.011(2) -0.0036(19) 0.0089(17) C6 0.0166(14) 0.0285(18) 0.038(2) -0.0034(15) -0.0019(12) 0.0001(12) C13 0.067(3) 0.036(2) 0.072(3) -0.001(2) 0.008(2) -0.006(2) C19 0.037(2) 0.073(3) 0.033(2) -0.014(2) -0.0092(16) 0.0149(18) C17 0.0284(17) 0.038(2) 0.030(2) -0.0044(15) -0.0037(13) 0.0044(14) C1 0.0216(16) 0.0366(19) 0.035(2) -0.0025(16) 0.0040(13) 0.0035(13) C12 0.042(2) 0.041(2) 0.056(3) -0.004(2) 0.0053(18) -0.0016(16) N3 0.067(2) 0.0358(19) 0.039(2) 0.0023(15) 0.0014(16) 0.0168(15) C22 0.094(4) 0.054(3) 0.050(3) 0.003(2) 0.003(3) 0.003(2) C23 0.095(4) 0.048(3) 0.055(3) 0.006(2) -0.011(3) 0.009(2) C24 0.048(2) 0.037(2) 0.036(2) -0.0044(17) 0.0064(16) 0.0132(16) C26 0.058(2) 0.047(2) 0.037(2) -0.0079(19) 0.0041(18) 0.0113(18) C25 0.069(3) 0.038(2) 0.048(3) -0.005(2) 0.005(2) 0.0144(19) N4 0.0366(16) 0.0354(17) 0.0341(18) -0.0010(14) 0.0037(12) 0.0085(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.970(2) . ? Co1 O3 2.025(2) 1_655 ? Co1 N1 2.033(3) . ? Co1 N4 2.044(3) 1_565 ? O5 C5 1.369(4) . ? O5 C9 1.434(4) . ? O4 C2 1.238(4) . ? O1 C1 1.277(4) . ? O2 C1 1.221(4) . ? O3 C2 1.279(4) . ? O3 Co1 2.025(2) 1_455 ? N2 C17 1.327(4) . ? N2 C19 1.355(4) . ? N2 C20 1.466(4) . ? O7 C16 1.218(4) . ? C7 C6 1.383(4) . ? C7 C8 1.388(4) . ? C7 C1 1.509(4) . ? O6 C16 1.339(5) . ? O6 H6A 0.8200 . ? N1 C17 1.320(4) . ? N1 C18 1.362(4) . ? C10 C15 1.383(5) . ? C10 C11 1.396(5) . ? C10 C9 1.512(5) . ? C18 C19 1.346(5) . ? C18 H18 0.9300 . ? C3 C4 1.384(4) . ? C3 C8 1.395(4) . ? C3 C2 1.497(4) . ? C11 C12 1.391(5) . ? C11 C16 1.504(5) . ? C5 C4 1.389(4) . ? C5 C6 1.391(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8 H8 0.9300 . ? C20 C21 1.506(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C14 C15 1.380(6) . ? C14 C13 1.382(6) . ? C14 H14 0.9300 . ? C21 C22 1.542(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C4 H4 0.9300 . ? C15 H15 0.9300 . ? C6 H6 0.9300 . ? C13 C12 1.372(6) . ? C13 H13 0.9300 . ? C19 H19 0.9300 . ? C17 H17 0.9300 . ? C12 H12 0.9300 . ? N3 C24 1.338(5) . ? N3 C25 1.364(5) . ? N3 C23 1.459(5) . ? C22 C23 1.473(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N4 1.299(5) . ? C24 H24 0.9300 . ? C26 C25 1.335(6) . ? C26 N4 1.382(5) . ? C26 H26 0.9300 . ? C25 H25 0.9300 . ? N4 Co1 2.044(3) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O3 120.70(10) . 1_655 ? O1 Co1 N1 123.51(10) . . ? O3 Co1 N1 94.84(10) 1_655 . ? O1 Co1 N4 101.57(10) . 1_565 ? O3 Co1 N4 111.93(10) 1_655 1_565 ? N1 Co1 N4 103.47(12) . 1_565 ? C5 O5 C9 117.2(2) . . ? C1 O1 Co1 110.2(2) . . ? C2 O3 Co1 103.66(18) . 1_455 ? C17 N2 C19 107.4(3) . . ? C17 N2 C20 126.3(3) . . ? C19 N2 C20 126.3(3) . . ? C6 C7 C8 120.4(3) . . ? C6 C7 C1 119.8(3) . . ? C8 C7 C1 119.6(3) . . ? C16 O6 H6A 109.5 . . ? C17 N1 C18 104.7(3) . . ? C17 N1 Co1 128.3(2) . . ? C18 N1 Co1 126.5(2) . . ? C15 C10 C11 117.9(3) . . ? C15 C10 C9 121.1(3) . . ? C11 C10 C9 120.9(3) . . ? C19 C18 N1 110.2(3) . . ? C19 C18 H18 124.9 . . ? N1 C18 H18 124.9 . . ? C4 C3 C8 119.6(3) . . ? C4 C3 C2 119.5(3) . . ? C8 C3 C2 120.8(3) . . ? C12 C11 C10 120.0(3) . . ? C12 C11 C16 119.5(3) . . ? C10 C11 C16 120.5(3) . . ? O5 C5 C4 116.0(3) . . ? O5 C5 C6 124.5(3) . . ? C4 C5 C6 119.4(3) . . ? O5 C9 C10 112.7(3) . . ? O5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? O5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? O4 C2 O3 121.5(3) . . ? O4 C2 C3 119.9(3) . . ? O3 C2 C3 118.6(3) . . ? C7 C8 C3 119.7(3) . . ? C7 C8 H8 120.2 . . ? C3 C8 H8 120.2 . . ? N2 C20 C21 112.3(3) . . ? N2 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? N2 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? O7 C16 O6 122.6(4) . . ? O7 C16 C11 122.3(3) . . ? O6 C16 C11 115.1(3) . . ? C15 C14 C13 119.6(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C20 C21 C22 111.2(4) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C14 C15 C10 122.0(4) . . ? C14 C15 H15 119.0 . . ? C10 C15 H15 119.0 . . ? C7 C6 C5 120.1(3) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C12 C13 C14 119.4(4) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C18 C19 N2 106.0(3) . . ? C18 C19 H19 127.0 . . ? N2 C19 H19 127.0 . . ? N1 C17 N2 111.7(3) . . ? N1 C17 H17 124.1 . . ? N2 C17 H17 124.1 . . ? O2 C1 O1 123.8(3) . . ? O2 C1 C7 119.5(3) . . ? O1 C1 C7 116.6(3) . . ? C13 C12 C11 121.0(4) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C24 N3 C25 107.3(3) . . ? C24 N3 C23 125.2(4) . . ? C25 N3 C23 127.5(4) . . ? C23 C22 C21 111.3(4) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N3 C23 C22 112.3(4) . . ? N3 C23 H23A 109.1 . . ? C22 C23 H23A 109.1 . . ? N3 C23 H23B 109.1 . . ? C22 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? N4 C24 N3 110.9(3) . . ? N4 C24 H24 124.5 . . ? N3 C24 H24 124.5 . . ? C25 C26 N4 108.8(4) . . ? C25 C26 H26 125.6 . . ? N4 C26 H26 125.6 . . ? C26 C25 N3 106.7(4) . . ? C26 C25 H25 126.6 . . ? N3 C25 H25 126.6 . . ? C24 N4 C26 106.3(3) . . ? C24 N4 Co1 130.1(3) . 1_545 ? C26 N4 Co1 123.2(3) . 1_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Co1 O1 C1 -165.8(2) 1_655 . . . ? N1 Co1 O1 C1 -45.1(3) . . . . ? N4 Co1 O1 C1 69.8(2) 1_565 . . . ? O1 Co1 N1 C17 -131.9(3) . . . . ? O3 Co1 N1 C17 0.2(3) 1_655 . . . ? N4 Co1 N1 C17 114.1(3) 1_565 . . . ? O1 Co1 N1 C18 58.0(4) . . . . ? O3 Co1 N1 C18 -169.8(3) 1_655 . . . ? N4 Co1 N1 C18 -55.9(3) 1_565 . . . ? C17 N1 C18 C19 0.0(5) . . . . ? Co1 N1 C18 C19 171.9(3) . . . . ? C15 C10 C11 C12 0.1(5) . . . . ? C9 C10 C11 C12 176.8(4) . . . . ? C15 C10 C11 C16 -179.5(3) . . . . ? C9 C10 C11 C16 -2.9(5) . . . . ? C9 O5 C5 C4 179.0(3) . . . . ? C9 O5 C5 C6 -2.6(5) . . . . ? C5 O5 C9 C10 68.1(4) . . . . ? C15 C10 C9 O5 31.9(5) . . . . ? C11 C10 C9 O5 -144.6(3) . . . . ? Co1 O3 C2 O4 3.4(4) 1_455 . . . ? Co1 O3 C2 C3 -175.3(2) 1_455 . . . ? C4 C3 C2 O4 24.6(5) . . . . ? C8 C3 C2 O4 -151.6(3) . . . . ? C4 C3 C2 O3 -156.7(3) . . . . ? C8 C3 C2 O3 27.2(4) . . . . ? C6 C7 C8 C3 1.5(5) . . . . ? C1 C7 C8 C3 -174.6(3) . . . . ? C4 C3 C8 C7 0.3(5) . . . . ? C2 C3 C8 C7 176.5(3) . . . . ? C17 N2 C20 C21 110.7(4) . . . . ? C19 N2 C20 C21 -68.9(5) . . . . ? C12 C11 C16 O7 118.1(4) . . . . ? C10 C11 C16 O7 -62.2(5) . . . . ? C12 C11 C16 O6 -62.9(5) . . . . ? C10 C11 C16 O6 116.8(4) . . . . ? N2 C20 C21 C22 -67.7(5) . . . . ? C8 C3 C4 C5 -1.4(5) . . . . ? C2 C3 C4 C5 -177.6(3) . . . . ? O5 C5 C4 C3 179.2(3) . . . . ? C6 C5 C4 C3 0.7(5) . . . . ? C13 C14 C15 C10 -0.4(7) . . . . ? C11 C10 C15 C14 -0.2(6) . . . . ? C9 C10 C15 C14 -176.8(4) . . . . ? C8 C7 C6 C5 -2.2(5) . . . . ? C1 C7 C6 C5 173.8(3) . . . . ? O5 C5 C6 C7 -177.2(3) . . . . ? C4 C5 C6 C7 1.1(5) . . . . ? C15 C14 C13 C12 1.0(7) . . . . ? N1 C18 C19 N2 0.3(5) . . . . ? C17 N2 C19 C18 -0.5(4) . . . . ? C20 N2 C19 C18 179.2(3) . . . . ? C18 N1 C17 N2 -0.3(4) . . . . ? Co1 N1 C17 N2 -172.0(2) . . . . ? C19 N2 C17 N1 0.5(4) . . . . ? C20 N2 C17 N1 -179.2(3) . . . . ? Co1 O1 C1 O2 10.7(4) . . . . ? Co1 O1 C1 C7 -167.8(2) . . . . ? C6 C7 C1 O2 -168.1(3) . . . . ? C8 C7 C1 O2 8.0(5) . . . . ? C6 C7 C1 O1 10.5(4) . . . . ? C8 C7 C1 O1 -173.4(3) . . . . ? C14 C13 C12 C11 -1.1(7) . . . . ? C10 C11 C12 C13 0.5(6) . . . . ? C16 C11 C12 C13 -179.8(4) . . . . ? C20 C21 C22 C23 174.2(4) . . . . ? C24 N3 C23 C22 -137.2(4) . . . . ? C25 N3 C23 C22 44.6(6) . . . . ? C21 C22 C23 N3 172.8(4) . . . . ? C25 N3 C24 N4 0.4(4) . . . . ? C23 N3 C24 N4 -178.2(4) . . . . ? N4 C26 C25 N3 0.7(5) . . . . ? C24 N3 C25 C26 -0.6(5) . . . . ? C23 N3 C25 C26 177.9(4) . . . . ? N3 C24 N4 C26 0.0(4) . . . . ? N3 C24 N4 Co1 172.3(2) . . . 1_545 ? C25 C26 N4 C24 -0.4(4) . . . . ? C25 C26 N4 Co1 -173.4(3) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.837 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.834 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.079 #========================================================= data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 843918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H55.50 Co N8 O7, 6.75(H2 O)' _chemical_formula_sum 'C38 H55.50 Co N8 O13.75' _chemical_formula_weight 903.33 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.846(5) _cell_length_b 12.858(5) _cell_length_c 13.629(5) _cell_angle_alpha 89.363(5) _cell_angle_beta 84.024(5) _cell_angle_gamma 76.580(5) _cell_volume 2177.6(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1660 _cell_measurement_theta_min 3.0630 _cell_measurement_theta_max 29.2152 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 953 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99359 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13782 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.1197 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7975 _reflns_number_gt 4181 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0640P)^2^+0.0375P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7975 _refine_ls_number_parameters 589 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1560 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1380 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.49653(5) 0.23737(5) 0.75024(4) 0.0415(2) Uani 1 1 d . . . O5 O 0.1657(3) 0.4549(3) 0.3253(2) 0.0603(10) Uani 1 1 d . . . O3 O 0.2872(3) 0.1428(3) -0.0064(2) 0.0505(9) Uani 1 1 d . . . O6 O 0.2950(3) 0.6524(3) 0.4954(2) 0.0641(11) Uani 1 1 d . . . O2 O 0.5911(3) 0.1574(3) 0.1841(3) 0.0677(11) Uani 1 1 d . . . N2 N 0.1591(3) 0.3523(4) 0.7989(3) 0.0514(11) Uani 1 1 d . . . N1 N 0.3334(3) 0.3287(3) 0.7699(3) 0.0455(10) Uani 1 1 d . . . O7 O 0.2137(3) 0.6972(3) 0.6485(3) 0.0789(12) Uani 1 1 d . . . H7 H 0.2752 0.6980 0.6588 0.118 Uiso 1 1 calc R . . C8 C 0.3753(4) 0.2220(4) 0.1500(3) 0.0419(12) Uani 1 1 d . . . H8 H 0.4208 0.1698 0.1088 0.050 Uiso 1 1 calc R . . C15 C 0.1080(4) 0.6641(4) 0.5207(3) 0.0393(12) Uani 1 1 d . . . C2 C 0.2221(5) 0.1977(4) 0.0587(3) 0.0449(13) Uani 1 1 d . . . C5 C 0.2411(4) 0.3773(4) 0.2708(3) 0.0439(12) Uani 1 1 d . . . N3 N -0.3608(3) 0.3954(4) 0.9580(3) 0.0481(11) Uani 1 1 d . . . O4 O 0.1230(3) 0.2117(3) 0.0615(3) 0.0717(12) Uani 1 1 d . . . C10 C 0.1038(4) 0.5951(4) 0.4431(3) 0.0460(13) Uani 1 1 d . . . C3 C 0.2670(4) 0.2506(4) 0.1377(3) 0.0396(12) Uani 1 1 d . . . N5 N 0.6563(3) 0.1359(3) 0.7286(3) 0.0455(10) Uani 1 1 d . . . O1 O 0.5759(3) 0.2907(3) 0.2876(3) 0.0766(13) Uani 1 1 d . . . N4 N -0.4470(3) 0.3401(3) 0.8455(3) 0.0463(11) Uani 1 1 d . . . C19 C 0.1772(4) 0.4459(5) 0.7610(4) 0.0545(14) Uani 1 1 d . . . H19 H 0.1260 0.5078 0.7498 0.065 Uiso 1 1 calc R . . N6 N 0.8318(3) 0.0836(4) 0.7261(3) 0.0585(12) Uani 1 1 d . . . C4 C 0.2000(4) 0.3289(4) 0.1999(3) 0.0451(13) Uani 1 1 d . . . H4 H 0.1268 0.3484 0.1932 0.054 Uiso 1 1 calc R . . C7 C 0.4173(4) 0.2692(4) 0.2224(3) 0.0407(12) Uani 1 1 d . . . C6 C 0.3489(4) 0.3476(4) 0.2834(3) 0.0445(13) Uani 1 1 d . . . H6 H 0.3760 0.3800 0.3326 0.053 Uiso 1 1 calc R . . C24 C -0.2946(4) 0.3921(5) 1.0398(4) 0.0625(16) Uani 1 1 d . . . H24A H -0.2763 0.3197 1.0641 0.075 Uiso 1 1 calc R . . H24B H -0.3357 0.4378 1.0932 0.075 Uiso 1 1 calc R . . C28 C 0.7474(4) 0.1661(4) 0.7195(4) 0.0530(14) Uani 1 1 d . . . H28 H 0.7528 0.2364 0.7096 0.064 Uiso 1 1 calc R . . C9 C 0.2014(4) 0.5188(4) 0.3937(3) 0.0511(14) Uani 1 1 d . . . H9A H 0.2499 0.5580 0.3595 0.061 Uiso 1 1 calc R . . H9B H 0.2393 0.4738 0.4424 0.061 Uiso 1 1 calc R . . C16 C 0.2126(4) 0.6699(4) 0.5538(3) 0.0427(12) Uani 1 1 d . . . C1 C 0.5369(4) 0.2368(4) 0.2325(4) 0.0511(14) Uani 1 1 d . . . C27 C -0.4536(4) 0.4465(4) 0.8358(4) 0.0527(14) Uani 1 1 d . . . H27 H -0.4892 0.4891 0.7883 0.063 Uiso 1 1 calc R . . C11 C 0.0022(5) 0.5962(4) 0.4135(4) 0.0560(15) Uani 1 1 d . . . H11 H -0.0029 0.5501 0.3630 0.067 Uiso 1 1 calc R . . C21 C -0.0132(5) 0.3943(5) 0.9029(4) 0.0675(17) Uani 1 1 d . . . H21A H -0.0273 0.4675 0.8802 0.081 Uiso 1 1 calc R . . H21B H 0.0239 0.3910 0.9618 0.081 Uiso 1 1 calc R . . C25 C -0.3899(4) 0.3118(4) 0.9202(4) 0.0513(14) Uani 1 1 d . . . H25 H -0.3719 0.2425 0.9438 0.062 Uiso 1 1 calc R . . C18 C 0.2849(4) 0.4299(4) 0.7431(3) 0.0498(13) Uani 1 1 d . . . H18 H 0.3211 0.4802 0.7165 0.060 Uiso 1 1 calc R . . C34 C 1.1997(4) -0.0304(4) 0.5533(4) 0.0575(14) Uani 1 1 d . . . H34A H 1.1895 0.0149 0.4960 0.069 Uiso 1 1 calc R . . H34B H 1.1747 -0.0941 0.5407 0.069 Uiso 1 1 calc R . . C29 C 0.6841(4) 0.0274(4) 0.7399(3) 0.0530(14) Uani 1 1 d . . . H29 H 0.6362 -0.0171 0.7469 0.064 Uiso 1 1 calc R . . C14 C 0.0121(4) 0.7285(4) 0.5655(3) 0.0484(13) Uani 1 1 d . . . H14 H 0.0150 0.7722 0.6186 0.058 Uiso 1 1 calc R . . C13 C -0.0844(5) 0.7295(4) 0.5341(4) 0.0564(15) Uani 1 1 d . . . H13 H -0.1465 0.7745 0.5645 0.068 Uiso 1 1 calc R . . C33 C 1.1326(4) 0.0276(5) 0.6407(4) 0.0628(16) Uani 1 1 d . . . H33A H 1.1469 0.0981 0.6454 0.075 Uiso 1 1 calc R . . H33B H 1.1530 -0.0108 0.7000 0.075 Uiso 1 1 calc R . . C20 C 0.0548(5) 0.3242(5) 0.8269(4) 0.0651(16) Uani 1 1 d . . . H20A H 0.0166 0.3272 0.7687 0.078 Uiso 1 1 calc R . . H20B H 0.0682 0.2513 0.8502 0.078 Uiso 1 1 calc R . . C26 C -0.4019(4) 0.4818(4) 0.9040(4) 0.0549(14) Uani 1 1 d . . . H26 H -0.3954 0.5515 0.9127 0.066 Uiso 1 1 calc R . . C32 C 1.0132(4) 0.0392(5) 0.6353(4) 0.0598(15) Uani 1 1 d . . . H32A H 0.9920 0.0827 0.5789 0.072 Uiso 1 1 calc R . . H32B H 1.0003 -0.0310 0.6242 0.072 Uiso 1 1 calc R . . C30 C 0.7912(5) -0.0047(5) 0.7392(4) 0.0614(16) Uani 1 1 d . . . H30 H 0.8303 -0.0744 0.7464 0.074 Uiso 1 1 calc R . . C17 C 0.2538(4) 0.2858(4) 0.8033(4) 0.0540(14) Uani 1 1 d . . . H17 H 0.2629 0.2166 0.8273 0.065 Uiso 1 1 calc R . . C23 C -0.1921(5) 0.4284(5) 1.0086(4) 0.0747(18) Uani 1 1 d . . . H23A H -0.2109 0.5016 0.9863 0.090 Uiso 1 1 calc R . . H23B H -0.1523 0.4273 1.0655 0.090 Uiso 1 1 calc R . . C12 C -0.0904(4) 0.6637(4) 0.4570(4) 0.0589(15) Uani 1 1 d . . . H12 H -0.1565 0.6647 0.4343 0.071 Uiso 1 1 calc R . . C35 C 1.3184(4) -0.0626(5) 0.5652(4) 0.0618(15) Uani 1 1 d . . . H35A H 1.3291 -0.1082 0.6222 0.074 Uiso 1 1 calc R . . H35B H 1.3559 -0.1037 0.5075 0.074 Uiso 1 1 calc R . . C31 C 0.9446(5) 0.0876(6) 0.7243(5) 0.084(2) Uani 1 1 d . . . H31A H 0.9732 0.0512 0.7818 0.101 Uiso 1 1 calc R . . H31B H 0.9486 0.1618 0.7293 0.101 Uiso 1 1 calc R . . C22 C -0.1213(5) 0.3605(5) 0.9282(4) 0.0746(18) Uani 1 1 d . . . H22A H -0.1589 0.3659 0.8695 0.089 Uiso 1 1 calc R . . H22B H -0.1065 0.2864 0.9484 0.089 Uiso 1 1 calc R . . N7 N 1.3646(3) 0.0295(3) 0.5777(3) 0.0482(11) Uani 1 1 d . . . N8 N 1.4396(3) 0.1438(3) 0.6465(3) 0.0455(11) Uani 1 1 d . . . C38 C 1.4184(4) 0.1764(5) 0.5526(4) 0.0532(14) Uani 1 1 d . . . H38 H 1.4335 0.2374 0.5228 0.064 Uiso 1 1 calc R . . C37 C 1.4062(4) 0.0545(4) 0.6574(4) 0.0489(13) Uani 1 1 d . . . H37 H 1.4111 0.0137 0.7142 0.059 Uiso 1 1 calc R . . C36 C 1.3725(4) 0.1065(5) 0.5104(4) 0.0570(15) Uani 1 1 d . . . H36 H 1.3505 0.1103 0.4473 0.068 Uiso 1 1 calc R . . O5W O 0.8080(4) 0.1294(4) 0.1400(4) 0.1040(16) Uani 1 1 d . . . O7W O 0.0670(7) 0.0684(7) -0.0586(6) 0.074(2) Uani 0.50 1 d P . . O8W O 0.1156(15) -0.0022(15) 0.0149(13) 0.086(5) Uani 0.25 1 d PU . . O1W O 0.4671(3) 0.1353(3) 0.8682(2) 0.0508(9) Uani 1 1 d . . . H1A H 0.406(4) 0.152(4) 0.912(4) 0.076 Uiso 1 1 d D . . H1B H 0.521(4) 0.114(5) 0.903(4) 0.076 Uiso 1 1 d D . . O2W O 0.5336(3) 0.3333(3) 0.6316(2) 0.0570(10) Uani 1 1 d D . . H2B H 0.5961(19) 0.316(4) 0.598(3) 0.086 Uiso 1 1 d D . . H2A H 0.493(3) 0.390(3) 0.610(3) 0.086 Uiso 1 1 d D . . O3W O 0.4746(4) 0.5410(3) 0.5978(3) 0.0661(11) Uani 1 1 d D . . H3A H 0.462(5) 0.595(3) 0.637(4) 0.099 Uiso 1 1 d D . . H3B H 0.450(5) 0.561(5) 0.543(2) 0.099 Uiso 1 1 d D . . O4W O 0.6198(4) 0.0707(3) 0.9944(3) 0.0678(13) Uani 1 1 d . . . H4B H 0.607(6) 0.091(5) 1.052(4) 0.102 Uiso 1 1 d . . . H4A H 0.639(6) 0.013(6) 0.992(5) 0.102 Uiso 1 1 d . . . O6W O -0.0488(4) 0.2317(6) 0.1982(4) 0.1204(19) Uani 1 1 d DU . . H6A H -0.050(7) 0.295(2) 0.181(7) 0.181 Uiso 1 1 d D . . H6B H 0.012(3) 0.190(5) 0.201(7) 0.181 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0301(4) 0.0457(5) 0.0484(4) 0.0007(3) 0.0017(3) -0.0103(3) O5 0.038(2) 0.069(3) 0.069(2) -0.0407(19) 0.0026(17) -0.0041(19) O3 0.047(2) 0.059(2) 0.0437(19) -0.0122(16) 0.0058(16) -0.0110(18) O6 0.042(2) 0.089(3) 0.059(2) -0.0253(19) 0.0139(18) -0.019(2) O2 0.046(3) 0.069(3) 0.080(2) -0.031(2) -0.0131(19) 0.007(2) N2 0.033(3) 0.065(3) 0.060(3) 0.005(2) -0.002(2) -0.020(2) N1 0.030(3) 0.054(3) 0.053(2) 0.0040(19) 0.0002(19) -0.012(2) O7 0.072(3) 0.084(3) 0.080(3) -0.017(2) -0.004(2) -0.017(2) C8 0.040(3) 0.038(3) 0.047(3) -0.004(2) 0.003(2) -0.008(2) C15 0.039(3) 0.033(3) 0.045(3) -0.007(2) 0.000(2) -0.008(2) C2 0.044(4) 0.049(3) 0.042(3) -0.004(2) -0.001(2) -0.012(3) C5 0.036(3) 0.047(3) 0.049(3) -0.015(2) -0.001(2) -0.011(3) N3 0.033(3) 0.059(3) 0.054(3) -0.006(2) -0.0030(19) -0.014(2) O4 0.034(3) 0.105(3) 0.077(3) -0.040(2) 0.0025(19) -0.019(2) C10 0.038(3) 0.043(3) 0.055(3) -0.005(2) 0.000(2) -0.007(3) C3 0.034(3) 0.041(3) 0.042(3) -0.004(2) 0.001(2) -0.007(2) N5 0.031(3) 0.051(3) 0.055(2) -0.0021(19) 0.0009(19) -0.012(2) O1 0.049(3) 0.082(3) 0.096(3) -0.046(2) -0.024(2) 0.001(2) N4 0.039(3) 0.043(3) 0.058(3) -0.001(2) -0.001(2) -0.013(2) C19 0.038(4) 0.055(4) 0.070(3) 0.005(3) -0.010(3) -0.009(3) N6 0.027(3) 0.070(4) 0.074(3) -0.012(2) 0.000(2) -0.005(3) C4 0.032(3) 0.047(3) 0.056(3) -0.007(2) -0.004(2) -0.008(2) C7 0.036(3) 0.041(3) 0.047(3) 0.000(2) -0.005(2) -0.011(2) C6 0.049(4) 0.041(3) 0.043(3) -0.011(2) -0.002(2) -0.012(3) C24 0.044(4) 0.089(5) 0.057(3) -0.004(3) -0.005(3) -0.021(3) C28 0.037(4) 0.051(4) 0.072(3) -0.008(3) -0.003(3) -0.013(3) C9 0.047(4) 0.049(3) 0.055(3) -0.015(2) 0.002(2) -0.010(3) C16 0.044(3) 0.039(3) 0.043(3) -0.011(2) 0.003(2) -0.009(2) C1 0.042(3) 0.057(4) 0.051(3) -0.010(3) -0.007(2) -0.005(3) C27 0.050(4) 0.050(4) 0.060(3) 0.001(3) -0.012(3) -0.013(3) C11 0.051(4) 0.058(4) 0.056(3) -0.012(2) -0.008(3) -0.005(3) C21 0.047(4) 0.077(4) 0.077(4) -0.006(3) -0.005(3) -0.012(3) C25 0.041(3) 0.048(3) 0.062(3) 0.004(3) -0.001(3) -0.006(3) C18 0.038(3) 0.050(4) 0.062(3) 0.000(2) -0.001(2) -0.014(3) C34 0.039(3) 0.060(4) 0.077(4) -0.010(3) -0.007(3) -0.017(3) C29 0.041(4) 0.051(4) 0.066(3) -0.002(3) 0.006(3) -0.014(3) C14 0.041(4) 0.049(3) 0.050(3) -0.011(2) -0.001(2) -0.001(3) C13 0.043(4) 0.059(4) 0.060(3) -0.007(3) 0.004(3) 0.001(3) C33 0.041(4) 0.074(4) 0.074(4) 0.000(3) -0.009(3) -0.013(3) C20 0.050(4) 0.075(4) 0.075(4) 0.001(3) -0.007(3) -0.023(3) C26 0.054(4) 0.040(3) 0.071(4) -0.001(3) -0.004(3) -0.013(3) C32 0.043(4) 0.062(4) 0.076(4) -0.005(3) -0.003(3) -0.014(3) C30 0.054(4) 0.052(4) 0.071(4) 0.004(3) 0.004(3) -0.001(3) C17 0.034(3) 0.056(4) 0.068(3) 0.020(3) -0.003(3) -0.005(3) C23 0.048(4) 0.104(5) 0.075(4) -0.017(3) -0.003(3) -0.023(4) C12 0.036(3) 0.067(4) 0.070(4) -0.002(3) -0.008(3) -0.002(3) C35 0.038(4) 0.060(4) 0.089(4) -0.019(3) -0.007(3) -0.013(3) C31 0.041(4) 0.109(6) 0.100(5) -0.041(4) -0.008(3) -0.009(4) C22 0.043(4) 0.103(5) 0.082(4) -0.005(3) -0.003(3) -0.026(4) N7 0.028(3) 0.055(3) 0.061(3) -0.009(2) -0.008(2) -0.008(2) N8 0.034(3) 0.052(3) 0.051(3) 0.0004(19) -0.0025(18) -0.011(2) C38 0.042(4) 0.063(4) 0.057(3) 0.002(3) -0.003(3) -0.018(3) C37 0.035(3) 0.057(4) 0.053(3) -0.002(2) 0.000(2) -0.008(3) C36 0.040(4) 0.076(4) 0.051(3) 0.000(3) -0.006(2) -0.007(3) O5W 0.067(3) 0.113(4) 0.134(4) -0.017(3) -0.007(3) -0.025(3) O7W 0.069(6) 0.076(6) 0.086(6) -0.036(4) -0.025(4) -0.025(5) O8W 0.083(9) 0.090(9) 0.091(8) -0.041(7) 0.021(7) -0.043(7) O1W 0.042(2) 0.061(2) 0.048(2) 0.0074(16) 0.0053(15) -0.0111(19) O2W 0.044(2) 0.057(3) 0.064(2) 0.0116(17) 0.0126(18) -0.0083(19) O3W 0.082(3) 0.053(3) 0.060(2) -0.0089(18) -0.013(2) -0.005(2) O4W 0.081(3) 0.059(3) 0.056(2) -0.002(2) -0.010(2) -0.001(3) O6W 0.083(4) 0.192(5) 0.090(3) -0.056(4) 0.027(3) -0.051(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O2W 2.105(3) . ? Co1 O1W 2.123(3) . ? Co1 N1 2.143(4) . ? Co1 N4 2.152(4) 1_655 ? Co1 N8 2.154(4) 1_455 ? Co1 N5 2.154(4) . ? O5 C5 1.380(5) . ? O5 C9 1.428(6) . ? O3 C2 1.253(5) . ? O6 C16 1.234(5) . ? O2 C1 1.246(5) . ? N2 C17 1.322(6) . ? N2 C19 1.364(7) . ? N2 C20 1.479(7) . ? N1 C17 1.310(6) . ? N1 C18 1.368(6) . ? O7 C16 1.343(5) . ? O7 H7 0.8200 . ? C8 C3 1.381(6) . ? C8 C7 1.382(6) . ? C8 H8 0.9300 . ? C15 C14 1.398(6) . ? C15 C10 1.401(6) . ? C15 C16 1.480(7) . ? C2 O4 1.241(6) . ? C2 C3 1.509(7) . ? C5 C4 1.369(6) . ? C5 C6 1.377(7) . ? N3 C25 1.342(6) . ? N3 C26 1.358(6) . ? N3 C24 1.466(6) . ? C10 C11 1.403(7) . ? C10 C9 1.502(6) . ? C3 C4 1.391(6) . ? N5 C28 1.309(6) . ? N5 C29 1.369(6) . ? O1 C1 1.243(6) . ? N4 C25 1.316(6) . ? N4 C27 1.358(6) . ? N4 Co1 2.152(4) 1_455 ? C19 C18 1.347(7) . ? C19 H19 0.9300 . ? N6 C28 1.339(6) . ? N6 C30 1.358(7) . ? N6 C31 1.460(7) . ? C4 H4 0.9300 . ? C7 C6 1.391(6) . ? C7 C1 1.517(7) . ? C6 H6 0.9300 . ? C24 C23 1.514(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C28 H28 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C27 C26 1.337(7) . ? C27 H27 0.9300 . ? C11 C12 1.381(7) . ? C11 H11 0.9300 . ? C21 C20 1.455(7) . ? C21 C22 1.554(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C25 H25 0.9300 . ? C18 H18 0.9300 . ? C34 C33 1.492(7) . ? C34 C35 1.509(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C29 C30 1.340(7) . ? C29 H29 0.9300 . ? C14 C13 1.350(7) . ? C14 H14 0.9300 . ? C13 C12 1.377(7) . ? C13 H13 0.9300 . ? C33 C32 1.515(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C26 H26 0.9300 . ? C32 C31 1.476(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C30 H30 0.9300 . ? C17 H17 0.9300 . ? C23 C22 1.496(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C12 H12 0.9300 . ? C35 N7 1.461(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? N7 C37 1.334(6) . ? N7 C36 1.356(6) . ? N8 C37 1.318(6) . ? N8 C38 1.377(6) . ? N8 Co1 2.154(4) 1_655 ? C38 C36 1.348(7) . ? C38 H38 0.9300 . ? C37 H37 0.9300 . ? C36 H36 0.9300 . ? O7W O8W 1.44(2) . ? O1W H1A 0.92(5) . ? O1W H1B 0.87(5) . ? O2W H2B 0.861(10) . ? O2W H2A 0.855(10) . ? O3W H3A 0.855(10) . ? O3W H3B 0.854(10) . ? O4W H4B 0.81(6) . ? O4W H4A 0.73(7) . ? O6W H6A 0.846(10) . ? O6W H6B 0.844(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W Co1 O1W 177.06(15) . . ? O2W Co1 N1 91.31(15) . . ? O1W Co1 N1 91.60(15) . . ? O2W Co1 N4 87.88(16) . 1_655 ? O1W Co1 N4 92.28(15) . 1_655 ? N1 Co1 N4 93.83(16) . 1_655 ? O2W Co1 N8 87.90(16) . 1_455 ? O1W Co1 N8 91.98(15) . 1_455 ? N1 Co1 N8 85.12(15) . 1_455 ? N4 Co1 N8 175.64(16) 1_655 1_455 ? O2W Co1 N5 90.65(15) . . ? O1W Co1 N5 86.42(15) . . ? N1 Co1 N5 176.02(17) . . ? N4 Co1 N5 89.70(16) 1_655 . ? N8 Co1 N5 91.49(15) 1_455 . ? C5 O5 C9 118.8(4) . . ? C17 N2 C19 107.5(4) . . ? C17 N2 C20 124.2(5) . . ? C19 N2 C20 128.3(5) . . ? C17 N1 C18 104.8(4) . . ? C17 N1 Co1 121.9(3) . . ? C18 N1 Co1 132.8(3) . . ? C16 O7 H7 109.5 . . ? C3 C8 C7 121.3(4) . . ? C3 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C14 C15 C10 119.1(5) . . ? C14 C15 C16 120.4(4) . . ? C10 C15 C16 120.4(4) . . ? O4 C2 O3 123.6(5) . . ? O4 C2 C3 118.3(4) . . ? O3 C2 C3 118.1(5) . . ? C4 C5 C6 120.6(4) . . ? C4 C5 O5 114.0(5) . . ? C6 C5 O5 125.4(4) . . ? C25 N3 C26 106.7(4) . . ? C25 N3 C24 126.0(5) . . ? C26 N3 C24 127.3(5) . . ? C15 C10 C11 117.4(4) . . ? C15 C10 C9 123.2(5) . . ? C11 C10 C9 119.4(5) . . ? C8 C3 C4 118.6(4) . . ? C8 C3 C2 120.7(4) . . ? C4 C3 C2 120.7(5) . . ? C28 N5 C29 105.3(4) . . ? C28 N5 Co1 127.1(4) . . ? C29 N5 Co1 126.6(4) . . ? C25 N4 C27 104.8(4) . . ? C25 N4 Co1 127.5(4) . 1_455 ? C27 N4 Co1 127.4(3) . 1_455 ? C18 C19 N2 105.6(5) . . ? C18 C19 H19 127.2 . . ? N2 C19 H19 127.2 . . ? C28 N6 C30 106.3(5) . . ? C28 N6 C31 127.2(6) . . ? C30 N6 C31 126.5(5) . . ? C5 C4 C3 120.6(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C8 C7 C6 119.1(5) . . ? C8 C7 C1 119.7(4) . . ? C6 C7 C1 121.1(4) . . ? C5 C6 C7 119.8(4) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? N3 C24 C23 111.9(4) . . ? N3 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? N3 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N5 C28 N6 111.9(5) . . ? N5 C28 H28 124.0 . . ? N6 C28 H28 124.0 . . ? O5 C9 C10 107.7(4) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? O6 C16 O7 121.8(5) . . ? O6 C16 C15 120.6(4) . . ? O7 C16 C15 117.6(4) . . ? O1 C1 O2 123.5(5) . . ? O1 C1 C7 118.8(4) . . ? O2 C1 C7 117.7(5) . . ? C26 C27 N4 110.6(5) . . ? C26 C27 H27 124.7 . . ? N4 C27 H27 124.7 . . ? C12 C11 C10 121.9(5) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C20 C21 C22 110.5(5) . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? N4 C25 N3 111.6(5) . . ? N4 C25 H25 124.2 . . ? N3 C25 H25 124.2 . . ? C19 C18 N1 110.1(5) . . ? C19 C18 H18 125.0 . . ? N1 C18 H18 125.0 . . ? C33 C34 C35 113.9(4) . . ? C33 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? C33 C34 H34B 108.8 . . ? C35 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C30 C29 N5 109.3(5) . . ? C30 C29 H29 125.3 . . ? N5 C29 H29 125.3 . . ? C13 C14 C15 122.2(5) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C13 C12 119.7(5) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C34 C33 C32 112.6(5) . . ? C34 C33 H33A 109.1 . . ? C32 C33 H33A 109.1 . . ? C34 C33 H33B 109.1 . . ? C32 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C21 C20 N2 113.3(5) . . ? C21 C20 H20A 108.9 . . ? N2 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? N2 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C27 C26 N3 106.3(5) . . ? C27 C26 H26 126.8 . . ? N3 C26 H26 126.8 . . ? C31 C32 C33 114.2(5) . . ? C31 C32 H32A 108.7 . . ? C33 C32 H32A 108.7 . . ? C31 C32 H32B 108.7 . . ? C33 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C29 C30 N6 107.2(5) . . ? C29 C30 H30 126.4 . . ? N6 C30 H30 126.4 . . ? N1 C17 N2 112.1(5) . . ? N1 C17 H17 124.0 . . ? N2 C17 H17 124.0 . . ? C22 C23 C24 113.3(5) . . ? C22 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? C22 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C13 C12 C11 119.6(5) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? N7 C35 C34 112.5(4) . . ? N7 C35 H35A 109.1 . . ? C34 C35 H35A 109.1 . . ? N7 C35 H35B 109.1 . . ? C34 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? N6 C31 C32 114.4(5) . . ? N6 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? N6 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C23 C22 C21 112.2(5) . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C37 N7 C36 106.8(5) . . ? C37 N7 C35 126.8(5) . . ? C36 N7 C35 126.4(5) . . ? C37 N8 C38 104.5(4) . . ? C37 N8 Co1 131.1(3) . 1_655 ? C38 N8 Co1 124.0(4) . 1_655 ? C36 C38 N8 109.7(5) . . ? C36 C38 H38 125.2 . . ? N8 C38 H38 125.2 . . ? N8 C37 N7 112.3(5) . . ? N8 C37 H37 123.9 . . ? N7 C37 H37 123.9 . . ? C38 C36 N7 106.7(5) . . ? C38 C36 H36 126.6 . . ? N7 C36 H36 126.6 . . ? Co1 O1W H1A 122(3) . . ? Co1 O1W H1B 114(4) . . ? H1A O1W H1B 107(4) . . ? Co1 O2W H2B 119(3) . . ? Co1 O2W H2A 128(3) . . ? H2B O2W H2A 113.0(18) . . ? H3A O3W H3B 109(6) . . ? H4B O4W H4A 110(7) . . ? H6A O6W H6B 117(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2W Co1 N1 C17 149.3(4) . . . . ? O1W Co1 N1 C17 -30.3(4) . . . . ? N4 Co1 N1 C17 -122.7(4) 1_655 . . . ? N8 Co1 N1 C17 61.5(4) 1_455 . . . ? N5 Co1 N1 C17 30(2) . . . . ? O2W Co1 N1 C18 -21.4(4) . . . . ? O1W Co1 N1 C18 159.0(4) . . . . ? N4 Co1 N1 C18 66.6(4) 1_655 . . . ? N8 Co1 N1 C18 -109.1(4) 1_455 . . . ? N5 Co1 N1 C18 -140.9(19) . . . . ? C9 O5 C5 C4 -173.0(4) . . . . ? C9 O5 C5 C6 7.1(7) . . . . ? C14 C15 C10 C11 0.9(7) . . . . ? C16 C15 C10 C11 -178.0(4) . . . . ? C14 C15 C10 C9 -176.8(5) . . . . ? C16 C15 C10 C9 4.3(7) . . . . ? C7 C8 C3 C4 0.1(7) . . . . ? C7 C8 C3 C2 -179.5(4) . . . . ? O4 C2 C3 C8 167.4(5) . . . . ? O3 C2 C3 C8 -13.2(7) . . . . ? O4 C2 C3 C4 -12.3(7) . . . . ? O3 C2 C3 C4 167.2(4) . . . . ? O2W Co1 N5 C28 49.7(4) . . . . ? O1W Co1 N5 C28 -130.5(4) . . . . ? N1 Co1 N5 C28 169.3(18) . . . . ? N4 Co1 N5 C28 -38.2(4) 1_655 . . . ? N8 Co1 N5 C28 137.6(4) 1_455 . . . ? O2W Co1 N5 C29 -143.5(4) . . . . ? O1W Co1 N5 C29 36.3(4) . . . . ? N1 Co1 N5 C29 -24(2) . . . . ? N4 Co1 N5 C29 128.6(4) 1_655 . . . ? N8 Co1 N5 C29 -55.6(4) 1_455 . . . ? C17 N2 C19 C18 0.6(6) . . . . ? C20 N2 C19 C18 -176.8(5) . . . . ? C6 C5 C4 C3 -1.5(7) . . . . ? O5 C5 C4 C3 178.6(4) . . . . ? C8 C3 C4 C5 0.9(7) . . . . ? C2 C3 C4 C5 -179.5(4) . . . . ? C3 C8 C7 C6 -0.4(7) . . . . ? C3 C8 C7 C1 -179.0(4) . . . . ? C4 C5 C6 C7 1.2(7) . . . . ? O5 C5 C6 C7 -178.9(4) . . . . ? C8 C7 C6 C5 -0.2(7) . . . . ? C1 C7 C6 C5 178.3(5) . . . . ? C25 N3 C24 C23 119.5(6) . . . . ? C26 N3 C24 C23 -58.4(7) . . . . ? C29 N5 C28 N6 -1.2(5) . . . . ? Co1 N5 C28 N6 167.9(3) . . . . ? C30 N6 C28 N5 0.7(6) . . . . ? C31 N6 C28 N5 -176.7(5) . . . . ? C5 O5 C9 C10 -179.5(4) . . . . ? C15 C10 C9 O5 174.5(4) . . . . ? C11 C10 C9 O5 -3.2(7) . . . . ? C14 C15 C16 O6 -149.3(5) . . . . ? C10 C15 C16 O6 29.6(7) . . . . ? C14 C15 C16 O7 29.2(7) . . . . ? C10 C15 C16 O7 -151.9(4) . . . . ? C8 C7 C1 O1 169.4(5) . . . . ? C6 C7 C1 O1 -9.1(7) . . . . ? C8 C7 C1 O2 -10.1(7) . . . . ? C6 C7 C1 O2 171.3(5) . . . . ? C25 N4 C27 C26 -0.4(6) . . . . ? Co1 N4 C27 C26 -174.7(3) 1_455 . . . ? C15 C10 C11 C12 1.4(8) . . . . ? C9 C10 C11 C12 179.2(5) . . . . ? C27 N4 C25 N3 0.2(5) . . . . ? Co1 N4 C25 N3 174.6(3) 1_455 . . . ? C26 N3 C25 N4 0.0(6) . . . . ? C24 N3 C25 N4 -178.3(4) . . . . ? N2 C19 C18 N1 -0.4(6) . . . . ? C17 N1 C18 C19 0.0(6) . . . . ? Co1 N1 C18 C19 171.9(3) . . . . ? C28 N5 C29 C30 1.2(5) . . . . ? Co1 N5 C29 C30 -167.9(3) . . . . ? C10 C15 C14 C13 -2.4(8) . . . . ? C16 C15 C14 C13 176.6(5) . . . . ? C15 C14 C13 C12 1.4(8) . . . . ? C35 C34 C33 C32 -168.5(5) . . . . ? C22 C21 C20 N2 179.7(5) . . . . ? C17 N2 C20 C21 123.1(6) . . . . ? C19 N2 C20 C21 -59.9(7) . . . . ? N4 C27 C26 N3 0.4(6) . . . . ? C25 N3 C26 C27 -0.2(6) . . . . ? C24 N3 C26 C27 178.0(5) . . . . ? C34 C33 C32 C31 174.9(5) . . . . ? N5 C29 C30 N6 -0.8(6) . . . . ? C28 N6 C30 C29 0.1(6) . . . . ? C31 N6 C30 C29 177.5(5) . . . . ? C18 N1 C17 N2 0.4(6) . . . . ? Co1 N1 C17 N2 -172.6(3) . . . . ? C19 N2 C17 N1 -0.6(6) . . . . ? C20 N2 C17 N1 176.9(4) . . . . ? N3 C24 C23 C22 -60.6(7) . . . . ? C14 C13 C12 C11 0.9(8) . . . . ? C10 C11 C12 C13 -2.4(8) . . . . ? C33 C34 C35 N7 -62.5(6) . . . . ? C28 N6 C31 C32 -111.5(6) . . . . ? C30 N6 C31 C32 71.6(8) . . . . ? C33 C32 C31 N6 -170.8(5) . . . . ? C24 C23 C22 C21 -175.8(5) . . . . ? C20 C21 C22 C23 178.1(5) . . . . ? C34 C35 N7 C37 115.3(5) . . . . ? C34 C35 N7 C36 -64.1(6) . . . . ? C37 N8 C38 C36 0.4(6) . . . . ? Co1 N8 C38 C36 -172.9(3) 1_655 . . . ? C38 N8 C37 N7 -0.7(5) . . . . ? Co1 N8 C37 N7 172.0(3) 1_655 . . . ? C36 N7 C37 N8 0.7(5) . . . . ? C35 N7 C37 N8 -178.8(4) . . . . ? N8 C38 C36 N7 0.0(6) . . . . ? C37 N7 C36 C38 -0.4(6) . . . . ? C35 N7 C36 C38 179.1(5) . . . . ? 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 O1W H1A O3 0.92(5) 1.82(5) 2.711(5) 163(5) 1_556 O1W H1B O4W 0.87(5) 1.86(5) 2.722(6) 171(5) . O2W H2B O6 0.861(10) 1.91(3) 2.695(5) 152(4) 2_666 O2W H2A O3W 0.855(10) 1.92(4) 2.650(5) 143(6) . O3W H3B O6 0.854(10) 2.23(4) 2.901(6) 136(5) . O3W H3B O3W 0.854(10) 2.33(5) 2.833(7) 118(5) 2_666 O4W H4A O3 0.73(7) 2.03(7) 2.739(5) 167(8) 2_656 O4W H4B O2 0.81(6) 1.98(6) 2.782(5) 170(7) 1_556 O6W H6B O4 0.844(10) 2.31(9) 2.702(6) 109(7) . O7 H7 O1 0.82 2.15 2.963(6) 169.7 2_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.428 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.063 #========================================================= data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 843919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cu N4 O7' _chemical_formula_sum 'C26 H24 Cu N4 O7' _chemical_formula_weight 568.03 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9508(4) _cell_length_b 9.0335(3) _cell_length_c 18.2518(7) _cell_angle_alpha 76.907(3) _cell_angle_beta 79.085(4) _cell_angle_gamma 65.248(4) _cell_volume 1297.89(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1999 _cell_measurement_theta_min 2.8754 _cell_measurement_theta_max 29.0882 _exptl_crystal_description block _exptl_crystal_colour blue _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 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 586 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93466 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8475 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4732 _reflns_number_gt 2804 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0301P)^2^+1.2767P] 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 4732 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1229 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.1602 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.195 _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 Cu1 Cu 1.0000 0.0000 0.5000 0.0478(3) Uani 1 2 d S . . Cu2 Cu 1.0000 0.0000 1.0000 0.0682(4) Uani 1 2 d S . . O5 O 1.0385(5) -0.6591(4) 0.80544(19) 0.0517(9) Uani 1 1 d . . . O2 O 1.0296(5) 0.0025(5) 0.6396(2) 0.0609(11) Uani 1 1 d . . . O1 O 1.0381(4) -0.1936(4) 0.58244(18) 0.0486(9) Uani 1 1 d . . . O4 O 1.0326(7) -0.2980(6) 0.9819(2) 0.0985(18) Uani 1 1 d . . . C6 C 1.0302(6) -0.4029(6) 0.7226(3) 0.0369(11) Uani 1 1 d . . . H6 H 1.0340 -0.4426 0.6792 0.044 Uiso 1 1 calc R . . C8 C 1.0193(6) -0.1872(6) 0.7810(3) 0.0401(12) Uani 1 1 d . . . H8 H 1.0165 -0.0816 0.7770 0.048 Uiso 1 1 calc R . . C7 C 1.0278(6) -0.2463(6) 0.7170(2) 0.0349(11) Uani 1 1 d . . . O3 O 0.9687(5) -0.0550(5) 0.9085(2) 0.0643(12) Uani 1 1 d . . . C5 C 1.0270(6) -0.5001(6) 0.7933(3) 0.0394(12) Uani 1 1 d . . . O7 O 0.8067(6) -0.3949(5) 0.5591(3) 0.0865(14) Uani 1 1 d . . . O6 O 0.9638(7) -0.6691(6) 0.5762(3) 0.1115(19) Uani 1 1 d . . . H6A H 1.0088 -0.6441 0.5346 0.167 Uiso 1 1 calc R . . C3 C 1.0148(6) -0.2819(6) 0.8514(3) 0.0425(13) Uani 1 1 d . . . N2 N 0.5268(6) 0.0646(7) 0.5903(3) 0.0688(14) Uani 1 1 d . . . N1 N 0.7601(5) 0.0711(6) 0.5293(2) 0.0515(12) Uani 1 1 d . . . C4 C 1.0210(6) -0.4386(6) 0.8575(3) 0.0446(13) Uani 1 1 d . . . H4 H 1.0212 -0.5040 0.9049 0.053 Uiso 1 1 calc R . . C10 C 0.8131(7) -0.6331(7) 0.7405(3) 0.0557(15) Uani 1 1 d . . . N3 N 0.4560(8) -0.0463(9) 0.8897(3) 0.089(2) Uani 1 1 d . . . C9 C 0.9947(7) -0.7124(6) 0.7475(3) 0.0530(15) Uani 1 1 d . . . H9A H 1.0288 -0.8315 0.7587 0.064 Uiso 1 1 calc R . . H9B H 1.0539 -0.6859 0.6995 0.064 Uiso 1 1 calc R . . C15 C 0.7444(8) -0.5544(7) 0.6727(4) 0.0600(16) Uani 1 1 d . . . C1 C 1.0334(6) -0.1375(7) 0.6418(3) 0.0425(12) Uani 1 1 d . . . C2 C 1.0050(8) -0.2091(8) 0.9205(3) 0.0603(17) Uani 1 1 d . . . C16 C 0.8406(8) -0.5324(8) 0.5981(4) 0.0636(17) Uani 1 1 d . . . N4 N 0.2393(7) -0.0611(9) 0.9626(3) 0.0800(18) Uani 1 1 d . . . C18 C 0.6401(8) 0.2260(8) 0.5203(4) 0.076(2) Uani 1 1 d . . . H18 H 0.6551 0.3196 0.4927 0.091 Uiso 1 1 calc R . . C17 C 0.6871(7) -0.0243(7) 0.5721(3) 0.0583(16) Uani 1 1 d . . . H17 H 0.7400 -0.1376 0.5874 0.070 Uiso 1 1 calc R . . C13 C 0.4737(10) -0.4850(11) 0.7423(7) 0.108(3) Uani 1 1 d . . . H13 H 0.3592 -0.4360 0.7426 0.129 Uiso 1 1 calc R . . C14 C 0.5721(10) -0.4801(9) 0.6747(5) 0.089(2) Uani 1 1 d . . . H14 H 0.5236 -0.4268 0.6301 0.107 Uiso 1 1 calc R . . C12 C 0.5403(11) -0.5597(11) 0.8082(6) 0.105(3) Uani 1 1 d . . . H12 H 0.4721 -0.5613 0.8534 0.127 Uiso 1 1 calc R . . C19 C 0.4954(9) 0.2232(9) 0.5576(4) 0.088(2) Uani 1 1 d . . . H19 H 0.3942 0.3128 0.5603 0.105 Uiso 1 1 calc R . . C23 C 0.5615(10) 0.0123(13) 0.8340(5) 0.135(4) Uani 1 1 d . . . H23A H 0.6730 -0.0395 0.8487 0.162 Uiso 1 1 calc R . . H23B H 0.5243 0.1306 0.8313 0.162 Uiso 1 1 calc R . . C20 C 0.4169(8) -0.0004(10) 0.6469(5) 0.093(2) Uani 1 1 d . . . H20A H 0.3048 0.0548 0.6329 0.112 Uiso 1 1 calc R . . H20B H 0.4527 -0.1175 0.6464 0.112 Uiso 1 1 calc R . . C26 C 0.3699(13) -0.2255(13) 0.9693(6) 0.133(4) Uani 1 1 d . . . H26 H 0.3655 -0.3234 0.9976 0.160 Uiso 1 1 calc R . . C11 C 0.7105(9) -0.6340(9) 0.8080(4) 0.080(2) Uani 1 1 d . . . H11 H 0.7566 -0.6848 0.8534 0.097 Uiso 1 1 calc R . . C25 C 0.5032(12) -0.2014(16) 0.9234(6) 0.147(4) Uani 1 1 d . . . H25 H 0.6094 -0.2823 0.9175 0.177 Uiso 1 1 calc R . . C22 C 0.5640(13) -0.0237(16) 0.7566(5) 0.159(5) Uani 1 1 d . . . H22A H 0.6324 0.0262 0.7215 0.190 Uiso 1 1 calc R . . H22B H 0.6211 -0.1424 0.7587 0.190 Uiso 1 1 calc R . . C24 C 0.3030(10) 0.0260(11) 0.9192(5) 0.106(3) Uani 1 1 d . . . H24 H 0.2451 0.1396 0.9074 0.127 Uiso 1 1 calc R . . C21 C 0.4177(11) 0.0243(15) 0.7243(5) 0.158(5) Uani 1 1 d . . . H21A H 0.3574 0.1415 0.7255 0.190 Uiso 1 1 calc R . . H21B H 0.3527 -0.0314 0.7581 0.190 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 0.0565(6) 0.0610(6) 0.0268(5) -0.0018(4) -0.0017(4) -0.0280(5) Cu2 0.0790(8) 0.1085(9) 0.0469(6) -0.0479(6) 0.0218(5) -0.0600(7) O5 0.077(3) 0.044(2) 0.046(2) -0.0007(17) -0.0165(19) -0.0341(19) O2 0.089(3) 0.052(2) 0.046(2) 0.0021(18) -0.007(2) -0.037(2) O1 0.064(2) 0.056(2) 0.0282(18) -0.0003(16) -0.0060(17) -0.0281(19) O4 0.192(5) 0.120(4) 0.028(2) -0.006(2) -0.012(3) -0.107(4) C6 0.044(3) 0.045(3) 0.029(3) -0.010(2) -0.004(2) -0.021(2) C8 0.054(3) 0.042(3) 0.032(3) -0.009(2) 0.001(2) -0.028(3) C7 0.036(3) 0.043(3) 0.027(2) -0.005(2) -0.005(2) -0.016(2) O3 0.094(3) 0.075(3) 0.043(2) -0.034(2) 0.007(2) -0.046(2) C5 0.050(3) 0.039(3) 0.038(3) -0.006(2) -0.007(2) -0.024(2) O7 0.104(4) 0.059(3) 0.089(3) 0.007(3) -0.027(3) -0.027(3) O6 0.160(5) 0.095(4) 0.080(4) -0.020(3) -0.008(3) -0.050(4) C3 0.061(4) 0.050(3) 0.028(3) -0.009(2) 0.001(2) -0.034(3) N2 0.049(3) 0.078(4) 0.075(4) -0.016(3) 0.003(3) -0.023(3) N1 0.053(3) 0.062(3) 0.037(3) -0.004(2) -0.003(2) -0.023(3) C4 0.061(4) 0.055(3) 0.025(3) 0.001(2) -0.008(2) -0.033(3) C10 0.058(4) 0.051(3) 0.065(4) -0.012(3) -0.004(3) -0.027(3) N3 0.060(4) 0.098(5) 0.080(4) 0.023(4) 0.007(3) -0.028(3) C9 0.066(4) 0.040(3) 0.060(4) -0.012(3) -0.014(3) -0.023(3) C15 0.054(4) 0.059(4) 0.078(5) -0.017(3) -0.012(3) -0.028(3) C1 0.046(3) 0.051(3) 0.033(3) -0.003(2) -0.006(2) -0.022(3) C2 0.085(5) 0.087(5) 0.034(3) -0.018(3) 0.005(3) -0.059(4) C16 0.074(5) 0.053(4) 0.072(4) -0.017(4) -0.024(4) -0.023(3) N4 0.075(4) 0.127(5) 0.058(4) -0.049(4) 0.019(3) -0.053(4) C18 0.070(5) 0.073(5) 0.064(4) 0.019(3) -0.010(4) -0.022(4) C17 0.057(4) 0.060(4) 0.057(4) -0.008(3) 0.001(3) -0.026(3) C13 0.053(5) 0.106(7) 0.169(10) -0.035(7) -0.007(6) -0.030(5) C14 0.082(6) 0.082(5) 0.112(7) -0.008(5) -0.036(5) -0.034(4) C12 0.070(6) 0.117(7) 0.126(8) -0.026(6) 0.008(5) -0.038(5) C19 0.057(5) 0.087(5) 0.087(5) 0.010(4) -0.008(4) -0.009(4) C23 0.080(6) 0.196(10) 0.115(8) 0.029(7) -0.006(6) -0.072(6) C20 0.052(4) 0.109(6) 0.115(7) -0.010(5) 0.016(4) -0.043(4) C26 0.117(8) 0.124(8) 0.136(9) -0.012(6) 0.025(7) -0.046(7) C11 0.078(5) 0.089(5) 0.079(5) -0.015(4) 0.007(4) -0.044(4) C25 0.075(7) 0.200(12) 0.142(10) -0.044(9) 0.034(6) -0.041(7) C22 0.092(7) 0.278(14) 0.084(7) 0.002(8) 0.023(6) -0.081(8) C24 0.067(5) 0.115(7) 0.097(6) 0.021(5) 0.012(5) -0.027(5) C21 0.068(6) 0.269(14) 0.092(7) 0.060(8) -0.002(6) -0.070(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu1 N1 1.968(4) 2_756 ? Cu1 N1 1.968(4) . ? Cu1 O1 1.985(3) . ? Cu1 O1 1.985(3) 2_756 ? Cu2 O3 1.945(3) . ? Cu2 O3 1.945(3) 2_757 ? Cu2 N4 1.996(5) 1_655 ? Cu2 N4 1.996(5) 2_657 ? O5 C5 1.366(5) . ? O5 C9 1.431(6) . ? O2 C1 1.242(6) . ? O1 C1 1.284(6) . ? O4 C2 1.221(7) . ? C6 C7 1.386(6) . ? C6 C5 1.390(6) . ? C6 H6 0.9300 . ? C8 C7 1.368(6) . ? C8 C3 1.377(6) . ? C8 H8 0.9300 . ? C7 C1 1.502(6) . ? O3 C2 1.266(7) . ? C5 C4 1.391(6) . ? O7 C16 1.227(7) . ? O6 C16 1.348(7) . ? O6 H6A 0.8200 . ? C3 C4 1.372(6) . ? C3 C2 1.522(7) . ? N2 C17 1.338(7) . ? N2 C19 1.352(8) . ? N2 C20 1.484(8) . ? N1 C17 1.324(7) . ? N1 C18 1.358(7) . ? C4 H4 0.9300 . ? C10 C11 1.391(8) . ? C10 C15 1.392(8) . ? C10 C9 1.495(8) . ? N3 C24 1.312(8) . ? N3 C25 1.316(12) . ? N3 C23 1.421(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C15 C14 1.397(9) . ? C15 C16 1.488(9) . ? N4 C24 1.223(8) . ? N4 C26 1.451(10) . ? N4 Cu2 1.996(5) 1_455 ? C18 C19 1.352(8) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? C13 C12 1.350(11) . ? C13 C14 1.378(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C12 C11 1.384(10) . ? C12 H12 0.9300 . ? C19 H19 0.9300 . ? C23 C22 1.513(12) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C20 C21 1.481(12) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C26 C25 1.389(11) . ? C26 H26 0.9300 . ? C11 H11 0.9300 . ? C25 H25 0.9300 . ? C22 C21 1.397(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 H24 0.9300 . ? C21 H21A 0.9700 . ? C21 H21B 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 Cu1 N1 180.0(2) 2_756 . ? N1 Cu1 O1 90.62(16) 2_756 . ? N1 Cu1 O1 89.38(17) . . ? N1 Cu1 O1 89.38(16) 2_756 2_756 ? N1 Cu1 O1 90.62(16) . 2_756 ? O1 Cu1 O1 180.00(15) . 2_756 ? O3 Cu2 O3 180.000(1) . 2_757 ? O3 Cu2 N4 88.86(18) . 1_655 ? O3 Cu2 N4 91.14(18) 2_757 1_655 ? O3 Cu2 N4 91.14(18) . 2_657 ? O3 Cu2 N4 88.86(18) 2_757 2_657 ? N4 Cu2 N4 180.000(1) 1_655 2_657 ? C5 O5 C9 117.9(4) . . ? C1 O1 Cu1 104.4(3) . . ? C7 C6 C5 119.7(4) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C7 C8 C3 120.9(4) . . ? C7 C8 H8 119.5 . . ? C3 C8 H8 119.5 . . ? C8 C7 C6 119.9(4) . . ? C8 C7 C1 118.4(4) . . ? C6 C7 C1 121.7(4) . . ? C2 O3 Cu2 106.9(4) . . ? O5 C5 C4 115.6(4) . . ? O5 C5 C6 124.9(4) . . ? C4 C5 C6 119.4(4) . . ? C16 O6 H6A 109.5 . . ? C4 C3 C8 119.6(4) . . ? C4 C3 C2 121.9(5) . . ? C8 C3 C2 118.4(4) . . ? C17 N2 C19 107.5(5) . . ? C17 N2 C20 123.9(6) . . ? C19 N2 C20 127.9(6) . . ? C17 N1 C18 105.7(5) . . ? C17 N1 Cu1 124.9(4) . . ? C18 N1 Cu1 128.8(4) . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C11 C10 C15 119.8(6) . . ? C11 C10 C9 115.8(6) . . ? C15 C10 C9 124.3(5) . . ? C24 N3 C25 104.8(7) . . ? C24 N3 C23 132.7(8) . . ? C25 N3 C23 122.5(8) . . ? O5 C9 C10 112.4(4) . . ? O5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? O5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C10 C15 C14 118.4(6) . . ? C10 C15 C16 124.9(6) . . ? C14 C15 C16 116.6(7) . . ? O2 C1 O1 123.0(5) . . ? O2 C1 C7 119.4(4) . . ? O1 C1 C7 117.6(4) . . ? O4 C2 O3 124.5(5) . . ? O4 C2 C3 120.3(6) . . ? O3 C2 C3 115.1(5) . . ? O7 C16 O6 122.6(6) . . ? O7 C16 C15 120.4(6) . . ? O6 C16 C15 117.0(6) . . ? C24 N4 C26 104.4(6) . . ? C24 N4 Cu2 127.5(6) . 1_455 ? C26 N4 Cu2 127.2(6) . 1_455 ? C19 C18 N1 109.6(6) . . ? C19 C18 H18 125.2 . . ? N1 C18 H18 125.2 . . ? N1 C17 N2 110.8(5) . . ? N1 C17 H17 124.6 . . ? N2 C17 H17 124.6 . . ? C12 C13 C14 121.2(8) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 120.4(8) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C13 C12 C11 119.6(8) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C18 C19 N2 106.5(6) . . ? C18 C19 H19 126.8 . . ? N2 C19 H19 126.8 . . ? N3 C23 C22 112.1(8) . . ? N3 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? N3 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C21 C20 N2 112.2(7) . . ? C21 C20 H20A 109.2 . . ? N2 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? N2 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C25 C26 N4 103.3(9) . . ? C25 C26 H26 128.3 . . ? N4 C26 H26 128.3 . . ? C12 C11 C10 120.5(8) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? N3 C25 C26 109.5(9) . . ? N3 C25 H25 125.3 . . ? C26 C25 H25 125.3 . . ? C21 C22 C23 121.3(9) . . ? C21 C22 H22A 107.0 . . ? C23 C22 H22A 107.0 . . ? C21 C22 H22B 107.0 . . ? C23 C22 H22B 107.0 . . ? H22A C22 H22B 106.8 . . ? N4 C24 N3 117.7(8) . . ? N4 C24 H24 121.1 . . ? N3 C24 H24 121.1 . . ? C22 C21 C20 122.4(8) . . ? C22 C21 H21A 106.7 . . ? C20 C21 H21A 106.7 . . ? C22 C21 H21B 106.7 . . ? C20 C21 H21B 106.7 . . ? H21A C21 H21B 106.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 O1 C1 96.9(3) 2_756 . . . ? N1 Cu1 O1 C1 -83.1(3) . . . . ? O1 Cu1 O1 C1 -21(100) 2_756 . . . ? C3 C8 C7 C6 0.7(7) . . . . ? C3 C8 C7 C1 -179.6(4) . . . . ? C5 C6 C7 C8 -1.1(7) . . . . ? C5 C6 C7 C1 179.2(4) . . . . ? O3 Cu2 O3 C2 -167(100) 2_757 . . . ? N4 Cu2 O3 C2 85.0(4) 1_655 . . . ? N4 Cu2 O3 C2 -95.0(4) 2_657 . . . ? C9 O5 C5 C4 161.2(5) . . . . ? C9 O5 C5 C6 -22.5(7) . . . . ? C7 C6 C5 O5 -176.0(4) . . . . ? C7 C6 C5 C4 0.1(7) . . . . ? C7 C8 C3 C4 0.8(8) . . . . ? C7 C8 C3 C2 -179.9(5) . . . . ? N1 Cu1 N1 C17 132(100) 2_756 . . . ? O1 Cu1 N1 C17 -17.1(5) . . . . ? O1 Cu1 N1 C17 162.9(5) 2_756 . . . ? N1 Cu1 N1 C18 -58(100) 2_756 . . . ? O1 Cu1 N1 C18 152.7(5) . . . . ? O1 Cu1 N1 C18 -27.3(5) 2_756 . . . ? C8 C3 C4 C5 -1.8(8) . . . . ? C2 C3 C4 C5 178.9(5) . . . . ? O5 C5 C4 C3 177.9(5) . . . . ? C6 C5 C4 C3 1.4(8) . . . . ? C5 O5 C9 C10 -70.0(6) . . . . ? C11 C10 C9 O5 -47.4(7) . . . . ? C15 C10 C9 O5 129.5(5) . . . . ? C11 C10 C15 C14 -0.9(9) . . . . ? C9 C10 C15 C14 -177.7(5) . . . . ? C11 C10 C15 C16 174.4(6) . . . . ? C9 C10 C15 C16 -2.3(9) . . . . ? Cu1 O1 C1 O2 -9.1(6) . . . . ? Cu1 O1 C1 C7 169.3(3) . . . . ? C8 C7 C1 O2 -0.2(7) . . . . ? C6 C7 C1 O2 179.4(5) . . . . ? C8 C7 C1 O1 -178.7(5) . . . . ? C6 C7 C1 O1 1.0(7) . . . . ? Cu2 O3 C2 O4 8.6(8) . . . . ? Cu2 O3 C2 C3 -170.8(4) . . . . ? C4 C3 C2 O4 13.4(9) . . . . ? C8 C3 C2 O4 -165.9(6) . . . . ? C4 C3 C2 O3 -167.2(5) . . . . ? C8 C3 C2 O3 13.5(8) . . . . ? C10 C15 C16 O7 -127.5(7) . . . . ? C14 C15 C16 O7 48.0(8) . . . . ? C10 C15 C16 O6 52.6(8) . . . . ? C14 C15 C16 O6 -131.9(6) . . . . ? C17 N1 C18 C19 -0.1(8) . . . . ? Cu1 N1 C18 C19 -171.4(5) . . . . ? C18 N1 C17 N2 -0.2(7) . . . . ? Cu1 N1 C17 N2 171.6(4) . . . . ? C19 N2 C17 N1 0.3(7) . . . . ? C20 N2 C17 N1 -170.4(6) . . . . ? C12 C13 C14 C15 0.7(12) . . . . ? C10 C15 C14 C13 0.0(10) . . . . ? C16 C15 C14 C13 -175.8(6) . . . . ? C14 C13 C12 C11 -0.5(14) . . . . ? N1 C18 C19 N2 0.2(9) . . . . ? C17 N2 C19 C18 -0.3(8) . . . . ? C20 N2 C19 C18 169.8(7) . . . . ? C24 N3 C23 C22 -97.8(13) . . . . ? C25 N3 C23 C22 81.9(12) . . . . ? C17 N2 C20 C21 89.3(9) . . . . ? C19 N2 C20 C21 -79.4(10) . . . . ? C24 N4 C26 C25 0.5(11) . . . . ? Cu2 N4 C26 C25 170.2(6) 1_455 . . . ? C13 C12 C11 C10 -0.4(12) . . . . ? C15 C10 C11 C12 1.2(10) . . . . ? C9 C10 C11 C12 178.2(6) . . . . ? C24 N3 C25 C26 5.5(12) . . . . ? C23 N3 C25 C26 -174.3(9) . . . . ? N4 C26 C25 N3 -3.8(12) . . . . ? N3 C23 C22 C21 53.4(15) . . . . ? C26 N4 C24 N3 3.1(11) . . . . ? Cu2 N4 C24 N3 -166.5(5) 1_455 . . . ? C25 N3 C24 N4 -5.6(12) . . . . ? C23 N3 C24 N4 174.1(9) . . . . ? C23 C22 C21 C20 176.3(9) . . . . ? N2 C20 C21 C22 -51.0(14) . . . . ? 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 O6 H6A O7 0.82 2.22 3.013(7) 163.3 2_746 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.738 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.077 #========================================================= data_compound-7 _database_code_depnum_ccdc_archive 'CCDC 843920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H26 Cu N4 O7' _chemical_formula_sum 'C27 H26 Cu N4 O7' _chemical_formula_weight 582.06 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 15.9321(7) _cell_length_b 17.2033(6) _cell_length_c 9.9871(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2737.31(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2353 _cell_measurement_theta_min 3.1193 _cell_measurement_theta_max 29.1183 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99069 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12106 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 29.18 _reflns_number_total 6274 _reflns_number_gt 4183 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0667P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.470(18) _refine_ls_number_reflns 6274 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.02349(4) 0.67875(3) 0.94733(6) 0.03418(18) Uani 1 1 d . . . O5 O 0.1047(3) 0.95372(19) 0.5021(3) 0.0465(10) Uani 1 1 d . . . O3 O 0.0285(2) 0.68135(18) 0.1476(3) 0.0302(7) Uani 1 1 d . . . O2 O 0.0086(3) 0.63097(19) 0.6378(4) 0.0464(10) Uani 1 1 d . . . O4 O 0.0332(3) 0.80282(18) 0.0756(3) 0.0491(10) Uani 1 1 d . . . O1 O 0.0194(3) 0.73200(19) 0.7768(3) 0.0410(8) Uani 1 1 d . . . N3 N -0.2766(3) 0.3563(2) 1.0053(6) 0.0459(13) Uani 1 1 d . . . N2 N -0.2241(3) 0.6444(2) 1.0448(6) 0.0433(11) Uani 1 1 d . . . N1 N -0.0987(2) 0.6592(2) 0.9571(5) 0.0364(10) Uani 1 1 d . . . C7 C 0.0380(3) 0.7812(3) 0.3108(5) 0.0279(11) Uani 1 1 d . . . C4 C 0.0589(3) 0.8312(3) 0.5713(5) 0.0356(12) Uani 1 1 d . . . H4 H 0.0652 0.8482 0.6591 0.043 Uiso 1 1 calc R . . N4 N -0.1466(3) 0.3403(2) 0.9359(5) 0.0391(10) Uani 1 1 d . . . C11 C 0.2717(3) 1.0565(3) 0.5168(6) 0.0407(14) Uani 1 1 d . . . C10 C 0.1915(3) 1.0642(3) 0.4651(6) 0.0366(12) Uani 1 1 d . . . C2 C 0.0326(3) 0.7546(3) 0.1675(5) 0.0304(11) Uani 1 1 d . . . C24 C -0.3484(4) 0.3693(3) 1.0969(7) 0.0537(17) Uani 1 1 d . . . H24A H -0.3271 0.3782 1.1866 0.064 Uiso 1 1 calc R . . H24B H -0.3827 0.3227 1.0993 0.064 Uiso 1 1 calc R . . C9 C 0.1459(4) 0.9988(3) 0.3978(5) 0.0455(15) Uani 1 1 d . . . H9A H 0.1047 1.0192 0.3355 0.055 Uiso 1 1 calc R . . H9B H 0.1850 0.9665 0.3486 0.055 Uiso 1 1 calc R . . C27 C -0.2003(4) 0.3334(4) 0.8300(7) 0.0515(16) Uani 1 1 d . . . H27 H -0.1844 0.3234 0.7421 0.062 Uiso 1 1 calc R . . C15 C 0.1534(3) 1.1367(3) 0.4711(6) 0.0429(14) Uani 1 1 d . . . H15 H 0.0997 1.1428 0.4361 0.052 Uiso 1 1 calc R . . C14 C 0.1932(3) 1.2000(3) 0.5279(6) 0.0439(14) Uani 1 1 d . . . H14 H 0.1668 1.2482 0.5303 0.053 Uiso 1 1 calc R . . C6 C 0.0662(3) 0.8571(3) 0.3355(5) 0.0327(12) Uani 1 1 d . . . H6 H 0.0770 0.8908 0.2647 0.039 Uiso 1 1 calc R . . C8 C 0.0200(3) 0.7316(2) 0.4153(4) 0.0267(10) Uani 1 1 d . . . H8 H 0.0004 0.6816 0.3983 0.032 Uiso 1 1 calc R . . C1 C 0.0183(3) 0.7009(3) 0.6614(5) 0.0317(10) Uani 1 1 d . . . C3 C 0.0314(3) 0.7568(2) 0.5460(5) 0.0276(9) Uani 1 1 d . . . C5 C 0.0775(3) 0.8811(2) 0.4647(6) 0.0331(11) Uani 1 1 d . . . C17 C -0.1422(3) 0.6467(3) 1.0677(6) 0.0411(13) Uani 1 1 d . . . H17 H -0.1181 0.6402 1.1518 0.049 Uiso 1 1 calc R . . C12 C 0.3108(3) 1.1206(3) 0.5745(7) 0.0507(16) Uani 1 1 d . . . H12 H 0.3646 1.1154 0.6097 0.061 Uiso 1 1 calc R . . C22 C -0.3557(4) 0.5143(3) 1.0324(8) 0.0602(18) Uani 1 1 d . . . H22A H -0.3136 0.5068 0.9634 0.072 Uiso 1 1 calc R . . H22B H -0.3953 0.5528 1.0005 0.072 Uiso 1 1 calc R . . O6 O 0.2902(4) 0.9180(3) 0.5290(8) 0.119(3) Uani 1 1 d . . . C21 C -0.3141(5) 0.5439(4) 1.1569(8) 0.0654(19) Uani 1 1 d . . . H21A H -0.2640 0.5134 1.1742 0.078 Uiso 1 1 calc R . . H21B H -0.3519 0.5370 1.2322 0.078 Uiso 1 1 calc R . . C20 C -0.2900(4) 0.6297(4) 1.1461(7) 0.0589(18) Uani 1 1 d . . . H20A H -0.3395 0.6597 1.1232 0.071 Uiso 1 1 calc R . . H20B H -0.2702 0.6476 1.2327 0.071 Uiso 1 1 calc R . . C25 C -0.1955(3) 0.3542(3) 1.0409(8) 0.0445(14) Uani 1 1 d . . . H25 H -0.1760 0.3615 1.1278 0.053 Uiso 1 1 calc R . . O7 O 0.3956(4) 0.9887(3) 0.4534(8) 0.132(3) Uani 1 1 d . . . H7 H 0.4177 0.9457 0.4490 0.198 Uiso 1 1 calc R . . C19 C -0.2352(4) 0.6551(4) 0.9113(7) 0.0554(18) Uani 1 1 d . . . H19 H -0.2862 0.6562 0.8658 0.067 Uiso 1 1 calc R . . C13 C 0.2715(3) 1.1910(3) 0.5802(7) 0.0505(16) Uani 1 1 d . . . H13 H 0.2984 1.2331 0.6200 0.061 Uiso 1 1 calc R . . C26 C -0.2801(4) 0.3433(4) 0.8724(7) 0.0567(17) Uani 1 1 d . . . H26 H -0.3282 0.3415 0.8199 0.068 Uiso 1 1 calc R . . C18 C -0.1583(4) 0.6639(3) 0.8574(6) 0.0490(15) Uani 1 1 d . . . H18 H -0.1472 0.6719 0.7670 0.059 Uiso 1 1 calc R . . C16 C 0.3193(4) 0.9815(3) 0.5034(8) 0.062(2) Uani 1 1 d . . . C23 C -0.4022(3) 0.4370(3) 1.0563(9) 0.0650(19) Uani 1 1 d . . . H23A H -0.4441 0.4452 1.1254 0.078 Uiso 1 1 calc R . . H23B H -0.4317 0.4232 0.9748 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 0.0408(3) 0.0442(3) 0.0175(3) -0.0003(3) -0.0002(3) -0.0026(3) O5 0.067(3) 0.0442(19) 0.029(2) -0.0090(15) 0.0096(19) -0.0183(19) O3 0.0442(19) 0.0337(16) 0.0129(14) -0.0013(13) -0.0002(15) -0.008(2) O2 0.065(3) 0.0375(18) 0.036(2) 0.0033(15) 0.003(2) -0.0069(19) O4 0.087(3) 0.0410(18) 0.0188(19) 0.0027(14) -0.007(2) 0.0015(19) O1 0.059(2) 0.0466(19) 0.0171(17) 0.0022(14) 0.000(2) -0.003(2) N3 0.037(2) 0.047(3) 0.053(4) 0.008(2) 0.003(2) 0.004(2) N2 0.045(2) 0.041(2) 0.044(3) -0.003(2) 0.011(3) -0.005(2) N1 0.040(2) 0.042(2) 0.027(2) -0.001(2) -0.003(2) -0.0035(18) C7 0.024(2) 0.035(2) 0.025(3) -0.0024(19) -0.004(2) 0.004(2) C4 0.039(3) 0.044(3) 0.023(3) -0.004(2) -0.004(2) 0.000(2) N4 0.043(2) 0.046(2) 0.028(3) 0.004(2) 0.000(2) 0.0050(19) C11 0.034(3) 0.037(3) 0.050(4) 0.005(2) 0.011(3) -0.002(2) C10 0.042(3) 0.036(2) 0.032(3) 0.002(2) 0.004(3) -0.007(2) C2 0.030(3) 0.038(3) 0.023(3) 0.0027(19) 0.001(2) -0.009(2) C24 0.042(3) 0.054(3) 0.065(5) 0.007(3) 0.013(3) 0.000(3) C9 0.066(4) 0.037(3) 0.034(3) 0.004(2) 0.003(3) -0.006(3) C27 0.051(3) 0.068(4) 0.035(4) 0.001(3) -0.005(3) 0.008(3) C15 0.033(3) 0.042(3) 0.053(4) -0.009(3) 0.001(3) 0.000(2) C14 0.038(3) 0.038(3) 0.056(4) -0.009(2) 0.000(3) 0.001(2) C6 0.039(3) 0.034(3) 0.025(3) 0.001(2) 0.000(2) 0.003(2) C8 0.029(2) 0.029(2) 0.022(2) -0.0028(16) 0.000(2) -0.002(2) C1 0.030(2) 0.044(3) 0.022(2) -0.0014(19) -0.001(2) -0.001(2) C3 0.031(2) 0.031(2) 0.020(2) 0.0041(19) -0.004(3) -0.001(2) C5 0.036(3) 0.028(2) 0.035(3) -0.006(2) 0.006(3) -0.006(2) C17 0.044(3) 0.050(3) 0.029(3) -0.004(3) 0.003(3) -0.007(3) C12 0.033(3) 0.059(3) 0.060(5) 0.000(3) -0.005(3) -0.008(3) C22 0.051(4) 0.051(3) 0.079(5) 0.010(3) 0.000(4) -0.001(3) O6 0.100(4) 0.055(3) 0.202(8) 0.016(4) 0.046(5) 0.000(3) C21 0.062(4) 0.069(4) 0.065(5) 0.001(4) 0.019(4) -0.018(4) C20 0.056(4) 0.062(4) 0.058(5) -0.013(3) 0.025(3) -0.004(3) C25 0.042(3) 0.053(3) 0.039(4) 0.001(3) -0.001(3) 0.002(3) O7 0.097(4) 0.087(4) 0.212(8) 0.015(5) 0.035(6) 0.028(3) C19 0.046(3) 0.068(4) 0.052(5) 0.009(3) -0.012(3) -0.008(3) C13 0.036(3) 0.048(3) 0.067(5) -0.013(3) 0.006(3) -0.014(3) C26 0.052(4) 0.078(5) 0.041(4) 0.001(3) -0.015(3) 0.003(4) C18 0.061(4) 0.059(4) 0.027(3) 0.007(3) -0.006(3) -0.007(3) C16 0.047(4) 0.044(3) 0.096(6) 0.010(3) 0.006(4) -0.005(3) C23 0.038(3) 0.049(3) 0.108(6) -0.015(4) 0.010(4) -0.002(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu1 O1 1.935(3) . ? Cu1 N1 1.978(4) . ? Cu1 N4 1.991(4) 2_565 ? Cu1 O3 2.002(3) 1_556 ? O5 C5 1.373(5) . ? O5 C9 1.455(6) . ? O3 C2 1.277(5) . ? O3 Cu1 2.002(3) 1_554 ? O2 C1 1.236(5) . ? O4 C2 1.238(5) . ? O1 C1 1.271(5) . ? N3 C25 1.341(7) . ? N3 C26 1.346(8) . ? N3 C24 1.482(7) . ? N2 C17 1.326(7) . ? N2 C19 1.357(8) . ? N2 C20 1.479(8) . ? N1 C17 1.322(7) . ? N1 C18 1.379(7) . ? C7 C8 1.379(6) . ? C7 C6 1.403(6) . ? C7 C2 1.505(7) . ? C4 C3 1.377(6) . ? C4 C5 1.400(7) . ? C4 H4 0.9300 . ? N4 C25 1.328(8) . ? N4 C27 1.366(7) . ? N4 Cu1 1.991(4) 2_565 ? C11 C10 1.384(7) . ? C11 C12 1.392(7) . ? C11 C16 1.502(8) . ? C10 C15 1.390(7) . ? C10 C9 1.498(7) . ? C24 C23 1.502(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C27 C26 1.350(9) . ? C27 H27 0.9300 . ? C15 C14 1.381(7) . ? C15 H15 0.9300 . ? C14 C13 1.362(8) . ? C14 H14 0.9300 . ? C6 C5 1.367(7) . ? C6 H6 0.9300 . ? C8 C3 1.387(7) . ? C8 H8 0.9300 . ? C1 C3 1.515(6) . ? C17 H17 0.9300 . ? C12 C13 1.364(8) . ? C12 H12 0.9300 . ? C22 C21 1.498(10) . ? C22 C23 1.541(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? O6 C16 1.215(7) . ? C21 C20 1.530(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C25 H25 0.9300 . ? O7 C16 1.319(8) . ? O7 H7 0.8200 . ? C19 C18 1.347(9) . ? C19 H19 0.9300 . ? C13 H13 0.9300 . ? C26 H26 0.9300 . ? C18 H18 0.9300 . ? C23 H23A 0.9700 . ? C23 H23B 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 O1 Cu1 N1 95.20(18) . . ? O1 Cu1 N4 93.48(19) . 2_565 ? N1 Cu1 N4 160.77(15) . 2_565 ? O1 Cu1 O3 150.46(14) . 1_556 ? N1 Cu1 O3 89.64(18) . 1_556 ? N4 Cu1 O3 91.24(18) 2_565 1_556 ? C5 O5 C9 115.7(4) . . ? C2 O3 Cu1 100.4(3) . 1_554 ? C1 O1 Cu1 126.9(3) . . ? C25 N3 C26 107.3(6) . . ? C25 N3 C24 125.7(6) . . ? C26 N3 C24 127.0(6) . . ? C17 N2 C19 107.1(5) . . ? C17 N2 C20 125.8(6) . . ? C19 N2 C20 127.1(5) . . ? C17 N1 C18 104.6(4) . . ? C17 N1 Cu1 125.8(4) . . ? C18 N1 Cu1 129.3(4) . . ? C8 C7 C6 120.7(5) . . ? C8 C7 C2 121.3(4) . . ? C6 C7 C2 118.0(4) . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C25 N4 C27 105.0(5) . . ? C25 N4 Cu1 124.2(4) . 2_565 ? C27 N4 Cu1 130.3(4) . 2_565 ? C10 C11 C12 119.4(4) . . ? C10 C11 C16 121.0(5) . . ? C12 C11 C16 119.5(5) . . ? C11 C10 C15 118.3(4) . . ? C11 C10 C9 122.9(4) . . ? C15 C10 C9 118.7(5) . . ? O4 C2 O3 123.1(4) . . ? O4 C2 C7 120.0(4) . . ? O3 C2 C7 116.8(4) . . ? N3 C24 C23 113.0(5) . . ? N3 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? N3 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O5 C9 C10 107.4(4) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C26 C27 N4 109.7(6) . . ? C26 C27 H27 125.2 . . ? N4 C27 H27 125.2 . . ? C14 C15 C10 121.6(5) . . ? C14 C15 H15 119.2 . . ? C10 C15 H15 119.2 . . ? C13 C14 C15 119.3(4) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C5 C6 C7 119.4(5) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C7 C8 C3 119.4(4) . . ? C7 C8 H8 120.3 . . ? C3 C8 H8 120.3 . . ? O2 C1 O1 125.7(4) . . ? O2 C1 C3 119.3(4) . . ? O1 C1 C3 115.0(4) . . ? C4 C3 C8 120.3(4) . . ? C4 C3 C1 119.6(4) . . ? C8 C3 C1 120.0(4) . . ? C6 C5 O5 125.0(5) . . ? C6 C5 C4 120.3(4) . . ? O5 C5 C4 114.7(5) . . ? N1 C17 N2 112.1(6) . . ? N1 C17 H17 123.9 . . ? N2 C17 H17 123.9 . . ? C13 C12 C11 121.0(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C21 C22 C23 112.2(6) . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C22 C21 C20 112.4(6) . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? N2 C20 C21 113.0(5) . . ? N2 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? N2 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? N4 C25 N3 111.1(6) . . ? N4 C25 H25 124.4 . . ? N3 C25 H25 124.4 . . ? C16 O7 H7 109.5 . . ? C18 C19 N2 106.8(6) . . ? C18 C19 H19 126.6 . . ? N2 C19 H19 126.6 . . ? C14 C13 C12 120.3(5) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? N3 C26 C27 106.9(6) . . ? N3 C26 H26 126.5 . . ? C27 C26 H26 126.5 . . ? C19 C18 N1 109.3(6) . . ? C19 C18 H18 125.3 . . ? N1 C18 H18 125.3 . . ? O6 C16 O7 121.0(6) . . ? O6 C16 C11 124.1(6) . . ? O7 C16 C11 114.8(5) . . ? C24 C23 C22 115.9(5) . . ? C24 C23 H23A 108.3 . . ? C22 C23 H23A 108.3 . . ? C24 C23 H23B 108.3 . . ? C22 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 O1 C1 -83.2(5) . . . . ? N4 Cu1 O1 C1 79.6(5) 2_565 . . . ? O3 Cu1 O1 C1 178.3(4) 1_556 . . . ? O1 Cu1 N1 C17 -156.8(4) . . . . ? N4 Cu1 N1 C17 86.8(7) 2_565 . . . ? O3 Cu1 N1 C17 -6.0(4) 1_556 . . . ? O1 Cu1 N1 C18 15.3(5) . . . . ? N4 Cu1 N1 C18 -101.1(7) 2_565 . . . ? O3 Cu1 N1 C18 166.1(5) 1_556 . . . ? C12 C11 C10 C15 0.9(8) . . . . ? C16 C11 C10 C15 -174.9(6) . . . . ? C12 C11 C10 C9 178.2(5) . . . . ? C16 C11 C10 C9 2.4(8) . . . . ? Cu1 O3 C2 O4 -0.3(6) 1_554 . . . ? Cu1 O3 C2 C7 -179.6(3) 1_554 . . . ? C8 C7 C2 O4 166.2(5) . . . . ? C6 C7 C2 O4 -17.0(7) . . . . ? C8 C7 C2 O3 -14.6(7) . . . . ? C6 C7 C2 O3 162.3(4) . . . . ? C25 N3 C24 C23 123.7(6) . . . . ? C26 N3 C24 C23 -57.4(8) . . . . ? C5 O5 C9 C10 -164.2(4) . . . . ? C11 C10 C9 O5 85.4(6) . . . . ? C15 C10 C9 O5 -97.4(6) . . . . ? C25 N4 C27 C26 0.1(7) . . . . ? Cu1 N4 C27 C26 172.7(4) 2_565 . . . ? C11 C10 C15 C14 -0.5(9) . . . . ? C9 C10 C15 C14 -177.9(5) . . . . ? C10 C15 C14 C13 -0.5(10) . . . . ? C8 C7 C6 C5 1.5(7) . . . . ? C2 C7 C6 C5 -175.4(4) . . . . ? C6 C7 C8 C3 -1.2(7) . . . . ? C2 C7 C8 C3 175.5(4) . . . . ? Cu1 O1 C1 O2 10.1(9) . . . . ? Cu1 O1 C1 C3 -169.0(3) . . . . ? C5 C4 C3 C8 -1.6(7) . . . . ? C5 C4 C3 C1 175.0(4) . . . . ? C7 C8 C3 C4 1.3(7) . . . . ? C7 C8 C3 C1 -175.3(5) . . . . ? O2 C1 C3 C4 -166.9(5) . . . . ? O1 C1 C3 C4 12.3(7) . . . . ? O2 C1 C3 C8 9.7(7) . . . . ? O1 C1 C3 C8 -171.1(5) . . . . ? C7 C6 C5 O5 180.0(5) . . . . ? C7 C6 C5 C4 -1.8(7) . . . . ? C9 O5 C5 C6 -18.0(7) . . . . ? C9 O5 C5 C4 163.7(4) . . . . ? C3 C4 C5 C6 1.8(7) . . . . ? C3 C4 C5 O5 -179.8(4) . . . . ? C18 N1 C17 N2 -1.0(6) . . . . ? Cu1 N1 C17 N2 172.7(3) . . . . ? C19 N2 C17 N1 0.8(6) . . . . ? C20 N2 C17 N1 178.6(4) . . . . ? C10 C11 C12 C13 -0.3(9) . . . . ? C16 C11 C12 C13 175.5(6) . . . . ? C23 C22 C21 C20 -163.5(5) . . . . ? C17 N2 C20 C21 -92.7(7) . . . . ? C19 N2 C20 C21 84.7(8) . . . . ? C22 C21 C20 N2 -66.1(8) . . . . ? C27 N4 C25 N3 0.0(6) . . . . ? Cu1 N4 C25 N3 -173.2(3) 2_565 . . . ? C26 N3 C25 N4 -0.1(6) . . . . ? C24 N3 C25 N4 179.1(4) . . . . ? C17 N2 C19 C18 -0.2(6) . . . . ? C20 N2 C19 C18 -178.0(5) . . . . ? C15 C14 C13 C12 1.2(10) . . . . ? C11 C12 C13 C14 -0.7(10) . . . . ? C25 N3 C26 C27 0.1(7) . . . . ? C24 N3 C26 C27 -179.0(5) . . . . ? N4 C27 C26 N3 -0.1(8) . . . . ? N2 C19 C18 N1 -0.4(7) . . . . ? C17 N1 C18 C19 0.8(6) . . . . ? Cu1 N1 C18 C19 -172.5(4) . . . . ? C10 C11 C16 O6 -47.9(11) . . . . ? C12 C11 C16 O6 136.3(8) . . . . ? C10 C11 C16 O7 128.5(7) . . . . ? C12 C11 C16 O7 -47.3(9) . . . . ? N3 C24 C23 C22 -52.3(9) . . . . ? C21 C22 C23 C24 -63.0(8) . . . . ? 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 O7 H7 O2 0.82 2.14 2.882(7) 150.2 3_566 _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.874 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.088 #========================================================end