data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C21 H20 O4 Zn' _chemical_formula_sum 'C21 H20 O4 Zn' _chemical_formula_weight 401.74 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' '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 nna' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.429(5) _cell_length_b 11.675(5) _cell_length_c 20.934(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 4015(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4017 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.620 _exptl_absorpt_correction_T_max 0.764 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21154 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.47 _reflns_number_total 4017 _reflns_number_gt 2189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1456P)^2^+19.9961P] 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 4017 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1807 _refine_ls_R_factor_gt 0.1060 _refine_ls_wR_factor_ref 0.3128 _refine_ls_wR_factor_gt 0.2577 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.2500 0.5000 0.67305(5) 0.0370(4) Uani 1 2 d S . . Zn2 Zn 0.23031(13) 0.2500 0.7500 0.0820(8) Uani 1 2 d S . . O1 O 0.2053(5) 0.3932(8) 0.6094(3) 0.0759(12) Uani 1 1 d . . . O2 O 0.2240(5) 0.2257(8) 0.6584(3) 0.0759(12) Uani 1 1 d . . . O3 O -0.1766(5) 0.1093(8) 0.2332(3) 0.0759(12) Uani 1 1 d . . . O4 O -0.1508(4) -0.0795(8) 0.2421(3) 0.0759(12) Uani 1 1 d . . . C1 C 0.1107(5) 0.2937(8) 0.5162(4) 0.043(2) Uani 1 1 d . . . H1 H 0.1059 0.3726 0.5209 1.000 Uiso 1 1 calc . . . C2 C 0.1580(5) 0.2296(8) 0.5582(3) 0.0394(19) Uani 1 1 d . . . C3 C 0.1697(6) 0.1138(9) 0.5509(4) 0.054(2) Uani 1 1 d . . . H3 H 0.2016 0.0748 0.5804 1.000 Uiso 1 1 calc . . . C4 C 0.1347(6) 0.0527(9) 0.4999(5) 0.061(3) Uani 1 1 d . . . H4 H 0.1441 -0.0250 0.4933 1.000 Uiso 1 1 calc . . . C5 C 0.0232(8) -0.0329(11) 0.3808(5) 0.086(4) Uani 1 1 d . . . H5 H 0.0532 -0.0944 0.3965 1.000 Uiso 1 1 calc . . . C6 C -0.0343(8) -0.0453(15) 0.3319(6) 0.095(5) Uani 1 1 d . . . H6 H -0.0429 -0.1174 0.3143 1.000 Uiso 1 1 calc . . . C7 C -0.0796(7) 0.0488(15) 0.3086(5) 0.087(4) Uani 1 1 d . . . C8 C -0.0670(6) 0.1581(14) 0.3326(5) 0.087(4) Uani 1 1 d . . . H8 H -0.0948 0.2205 0.3156 1.000 Uiso 1 1 calc . . . C9 C 0.0114(7) 0.2833(10) 0.4175(5) 0.070(3) Uani 1 1 d . . . C10 C 0.0708(5) 0.2366(8) 0.4670(4) 0.046(2) Uani 1 1 d . . . C11 C 0.0843(6) 0.1186(9) 0.4594(4) 0.059(3) Uani 1 1 d . . . C12 C 0.0327(6) 0.0802(11) 0.4047(4) 0.069(3) Uani 1 1 d . . . C13 C -0.0113(6) 0.1727(11) 0.3832(4) 0.070(3) Uani 1 1 d . . . C14 C 0.1987(5) 0.2862(8) 0.6129(3) 0.040(2) Uani 1 1 d . . . C15 C -0.1421(7) 0.0281(12) 0.2527(7) 0.083(4) Uani 1 1 d . . . C16 C -0.0609(7) 0.3502(11) 0.4493(6) 0.080(3) Uani 1 1 d . . . H16A H -0.0391 0.4130 0.4743 1.000 Uiso 1 1 calc . . . H16B H -0.0950 0.3825 0.4161 1.000 Uiso 1 1 calc . . . C17 C -0.1117(8) 0.2757(12) 0.4915(7) 0.094(4) Uani 1 1 d . . . H17A H -0.0768 0.2318 0.5198 1.000 Uiso 1 1 calc . . . H17B H -0.1428 0.2224 0.4657 1.000 Uiso 1 1 calc . . . C18 C -0.1716(8) 0.3523(13) 0.5324(7) 0.099(4) Uani 1 1 d . . . H18A H -0.2037 0.3042 0.5597 1.000 Uiso 1 1 calc . . . H18B H -0.2068 0.3944 0.5043 1.000 Uiso 1 1 calc . . . H18C H -0.1407 0.4049 0.5579 1.000 Uiso 1 1 calc . . . C19 C 0.0521(11) 0.3708(16) 0.3732(7) 0.127(4) Uani 1 1 d . . . H19A H 0.0122 0.3981 0.3426 1.000 Uiso 1 1 calc . . . H19B H 0.0699 0.4359 0.3983 1.000 Uiso 1 1 calc . . . C20 C 0.1223(11) 0.3237(17) 0.3384(7) 0.127(4) Uani 1 1 d . . . H20A H 0.1070 0.2546 0.3156 1.000 Uiso 1 1 calc . . . H20B H 0.1661 0.3053 0.3677 1.000 Uiso 1 1 calc . . . C21 C 0.1506(10) 0.4226(17) 0.2887(7) 0.127(4) Uani 1 1 d . . . H21A H 0.1954 0.3951 0.2636 1.000 Uiso 1 1 calc . . . H21B H 0.1671 0.4894 0.3121 1.000 Uiso 1 1 calc . . . H21C H 0.1060 0.4417 0.2611 1.000 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0368(7) 0.0512(8) 0.0230(6) 0.000 0.000 0.0101(6) Zn2 0.0954(15) 0.1242(19) 0.0264(8) 0.0126(9) 0.000 0.000 O1 0.074(2) 0.117(3) 0.0367(17) 0.0067(19) -0.0073(16) -0.015(2) O2 0.074(2) 0.117(3) 0.0367(17) 0.0067(19) -0.0073(16) -0.015(2) O3 0.074(2) 0.117(3) 0.0367(17) 0.0067(19) -0.0073(16) -0.015(2) O4 0.074(2) 0.117(3) 0.0367(17) 0.0067(19) -0.0073(16) -0.015(2) C1 0.037(4) 0.059(6) 0.034(4) 0.010(4) -0.008(3) 0.004(4) C2 0.037(4) 0.050(5) 0.031(4) 0.001(4) -0.006(3) -0.005(4) C3 0.054(5) 0.067(7) 0.040(5) 0.006(4) -0.022(4) -0.004(5) C4 0.075(7) 0.053(6) 0.056(5) -0.005(5) -0.026(5) -0.008(5) C5 0.097(9) 0.107(10) 0.054(6) -0.015(6) -0.028(6) -0.033(7) C6 0.082(9) 0.140(12) 0.064(7) -0.018(8) -0.018(7) -0.045(9) C7 0.069(7) 0.156(13) 0.036(5) 0.003(7) -0.011(5) -0.052(8) C8 0.050(6) 0.164(14) 0.046(6) 0.024(7) -0.021(5) -0.028(7) C9 0.066(7) 0.095(8) 0.048(5) 0.024(6) -0.026(5) -0.009(6) C10 0.040(4) 0.057(6) 0.041(4) 0.014(4) -0.015(3) -0.006(4) C11 0.057(6) 0.081(8) 0.039(5) 0.010(5) -0.025(4) -0.019(5) C12 0.066(6) 0.094(9) 0.046(5) -0.003(6) -0.013(5) -0.034(6) C13 0.061(6) 0.112(9) 0.036(5) 0.013(6) -0.021(4) -0.013(6) C14 0.037(4) 0.067(6) 0.017(3) 0.012(4) -0.002(3) -0.005(4) C15 0.061(7) 0.076(9) 0.113(11) 0.007(7) 0.033(7) -0.019(6) C16 0.058(6) 0.090(9) 0.091(8) 0.023(7) -0.026(6) 0.014(6) C17 0.067(7) 0.097(10) 0.117(11) 0.033(9) -0.017(8) 0.003(7) C18 0.071(8) 0.118(12) 0.107(10) -0.018(9) -0.022(7) 0.009(8) C19 0.125(8) 0.175(10) 0.081(6) 0.053(6) -0.017(5) -0.048(8) C20 0.125(8) 0.175(10) 0.081(6) 0.053(6) -0.017(5) -0.048(8) C21 0.125(8) 0.175(10) 0.081(6) 0.053(6) -0.017(5) -0.048(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.967(7) . ? Zn1 O1 1.967(7) 2_565 ? Zn1 O3 2.161(7) 7_566 ? Zn1 O3 2.161(7) 8_666 ? Zn1 O4 2.367(7) 8_666 ? Zn1 O4 2.367(7) 7_566 ? Zn1 C15 2.455(15) 7_566 ? Zn1 C15 2.455(15) 8_666 ? Zn2 O2 1.940(7) 3_556 ? Zn2 O2 1.940(7) . ? Zn2 O3 2.271(10) 8_666 ? Zn2 O3 2.271(10) 6_656 ? Zn2 O4 2.386(9) 5_556 ? Zn2 O4 2.386(9) 7_566 ? O1 C14 1.256(11) . ? O2 C14 1.258(10) . ? O3 C15 1.178(14) . ? O3 Zn1 2.161(7) 7 ? O3 Zn2 2.271(10) 6_556 ? O4 C15 1.283(15) . ? O4 Zn1 2.367(7) 7 ? O4 Zn2 2.386(9) 5_556 ? C1 C10 1.391(12) . ? C1 C2 1.393(11) . ? C1 H1 0.9300 . ? C2 C3 1.373(13) . ? C2 C14 1.480(11) . ? C3 C4 1.407(12) . ? C3 H3 0.9300 . ? C4 C11 1.413(13) . ? C4 H4 0.9300 . ? C5 C6 1.400(15) . ? C5 C12 1.421(16) . ? C5 H5 0.9300 . ? C6 C7 1.41(2) . ? C6 H6 0.9300 . ? C7 C8 1.39(2) . ? C7 C15 1.576(18) . ? C8 C13 1.411(13) . ? C8 H8 0.9300 . ? C9 C13 1.524(16) . ? C9 C10 1.525(11) . ? C9 C19 1.533(17) . ? C9 C16 1.570(16) . ? C10 C11 1.404(13) . ? C11 C12 1.493(12) . ? C12 C13 1.375(16) . ? C15 Zn1 2.455(15) 7 ? C16 C17 1.494(17) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.581(19) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.47(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.62(2) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 94.7(4) . 2_565 ? O1 Zn1 O3 124.1(3) . 7_566 ? O1 Zn1 O3 103.2(3) 2_565 7_566 ? O1 Zn1 O3 103.2(3) . 8_666 ? O1 Zn1 O3 124.1(3) 2_565 8_666 ? O3 Zn1 O3 108.7(4) 7_566 8_666 ? O1 Zn1 O4 156.8(3) . 8_666 ? O1 Zn1 O4 84.7(3) 2_565 8_666 ? O3 Zn1 O4 78.3(3) 7_566 8_666 ? O3 Zn1 O4 59.5(3) 8_666 8_666 ? O1 Zn1 O4 84.7(3) . 7_566 ? O1 Zn1 O4 156.8(3) 2_565 7_566 ? O3 Zn1 O4 59.5(3) 7_566 7_566 ? O3 Zn1 O4 78.3(3) 8_666 7_566 ? O4 Zn1 O4 104.8(4) 8_666 7_566 ? O1 Zn1 C15 106.0(4) . 7_566 ? O1 Zn1 C15 130.2(4) 2_565 7_566 ? O3 Zn1 C15 28.7(3) 7_566 7_566 ? O3 Zn1 C15 94.9(3) 8_666 7_566 ? O4 Zn1 C15 91.7(3) 8_666 7_566 ? O4 Zn1 C15 30.8(4) 7_566 7_566 ? O1 Zn1 C15 130.2(4) . 8_666 ? O1 Zn1 C15 106.0(4) 2_565 8_666 ? O3 Zn1 C15 94.9(3) 7_566 8_666 ? O3 Zn1 C15 28.7(3) 8_666 8_666 ? O4 Zn1 C15 30.8(4) 8_666 8_666 ? O4 Zn1 C15 91.7(3) 7_566 8_666 ? C15 Zn1 C15 94.5(5) 7_566 8_666 ? O2 Zn2 O2 173.9(5) 3_556 . ? O2 Zn2 O3 94.7(3) 3_556 8_666 ? O2 Zn2 O3 89.4(3) . 8_666 ? O2 Zn2 O3 89.4(3) 3_556 6_656 ? O2 Zn2 O3 94.7(3) . 6_656 ? O3 Zn2 O3 95.4(4) 8_666 6_656 ? O2 Zn2 O4 91.4(3) 3_556 5_556 ? O2 Zn2 O4 85.3(3) . 5_556 ? O3 Zn2 O4 169.2(3) 8_666 5_556 ? O3 Zn2 O4 75.8(3) 6_656 5_556 ? O2 Zn2 O4 85.3(3) 3_556 7_566 ? O2 Zn2 O4 91.4(3) . 7_566 ? O3 Zn2 O4 75.8(3) 8_666 7_566 ? O3 Zn2 O4 169.2(3) 6_656 7_566 ? O4 Zn2 O4 113.7(4) 5_556 7_566 ? C14 O1 Zn1 128.6(6) . . ? C14 O2 Zn2 133.2(7) . . ? C15 O3 Zn1 89.7(9) . 7 ? C15 O3 Zn2 148.5(8) . 6_556 ? Zn1 O3 Zn2 98.1(3) 7 6_556 ? C15 O4 Zn1 78.4(8) . 7 ? C15 O4 Zn2 149.9(7) . 5_556 ? Zn1 O4 Zn2 89.6(2) 7 5_556 ? C10 C1 C2 118.2(8) . . ? C10 C1 H1 120.9 . . ? C2 C1 H1 120.9 . . ? C3 C2 C1 122.4(7) . . ? C3 C2 C14 117.6(7) . . ? C1 C2 C14 120.0(8) . . ? C2 C3 C4 121.8(8) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C3 C4 C11 114.7(9) . . ? C3 C4 H4 122.6 . . ? C11 C4 H4 122.6 . . ? C6 C5 C12 115.3(13) . . ? C6 C5 H5 122.4 . . ? C12 C5 H5 122.4 . . ? C5 C6 C7 121.8(14) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C6 120.8(10) . . ? C8 C7 C15 120.5(13) . . ? C6 C7 C15 118.7(13) . . ? C7 C8 C13 118.7(13) . . ? C7 C8 H8 120.7 . . ? C13 C8 H8 120.7 . . ? C13 C9 C10 100.0(8) . . ? C13 C9 C19 112.7(10) . . ? C10 C9 C19 111.8(9) . . ? C13 C9 C16 115.8(9) . . ? C10 C9 C16 112.0(8) . . ? C19 C9 C16 104.8(11) . . ? C1 C10 C11 118.7(7) . . ? C1 C10 C9 129.3(9) . . ? C11 C10 C9 112.0(8) . . ? C10 C11 C4 123.9(8) . . ? C10 C11 C12 107.0(8) . . ? C4 C11 C12 129.0(10) . . ? C13 C12 C5 123.9(9) . . ? C13 C12 C11 108.3(10) . . ? C5 C12 C11 127.7(11) . . ? C12 C13 C8 119.5(12) . . ? C12 C13 C9 112.5(8) . . ? C8 C13 C9 128.0(12) . . ? O1 C14 O2 125.0(8) . . ? O1 C14 C2 116.0(7) . . ? O2 C14 C2 119.0(9) . . ? O3 C15 O4 132.4(14) . . ? O3 C15 C7 116.5(13) . . ? O4 C15 C7 110.6(13) . . ? O3 C15 Zn1 61.6(8) . 7 ? O4 C15 Zn1 70.8(7) . 7 ? C7 C15 Zn1 174.5(8) . 7 ? C17 C16 C9 112.6(10) . . ? C17 C16 H16A 109.1 . . ? C9 C16 H16A 109.1 . . ? C17 C16 H16B 109.1 . . ? C9 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C16 C17 C18 109.8(11) . . ? C16 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C9 113.1(15) . . ? C20 C19 H19A 109.0 . . ? C9 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C9 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 C21 106.0(16) . . ? C19 C20 H20A 110.5 . . ? C21 C20 H20A 110.5 . . ? C19 C20 H20B 110.5 . . ? C21 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 O1 Zn1 O1 C14 146.6(10) 2_565 . . . ? O3 Zn1 O1 C14 -104.0(8) 7_566 . . . ? O3 Zn1 O1 C14 19.9(9) 8_666 . . . ? O4 Zn1 O1 C14 59.0(12) 8_666 . . . ? O4 Zn1 O1 C14 -56.7(8) 7_566 . . . ? C15 Zn1 O1 C14 -79.3(9) 7_566 . . . ? C15 Zn1 O1 C14 31.0(10) 8_666 . . . ? O2 Zn2 O2 C14 66.1(8) 3_556 . . . ? O3 Zn2 O2 C14 -66.4(9) 8_666 . . . ? O3 Zn2 O2 C14 -161.7(8) 6_656 . . . ? O4 Zn2 O2 C14 123.0(9) 5_556 . . . ? O4 Zn2 O2 C14 9.4(9) 7_566 . . . ? C10 C1 C2 C3 3.2(12) . . . . ? C10 C1 C2 C14 -177.4(7) . . . . ? C1 C2 C3 C4 0.4(14) . . . . ? C14 C2 C3 C4 -179.0(9) . . . . ? C2 C3 C4 C11 -2.9(15) . . . . ? C12 C5 C6 C7 -0.2(18) . . . . ? C5 C6 C7 C8 1.6(19) . . . . ? C5 C6 C7 C15 179.0(10) . . . . ? C6 C7 C8 C13 -3.4(17) . . . . ? C15 C7 C8 C13 179.2(9) . . . . ? C2 C1 C10 C11 -4.1(12) . . . . ? C2 C1 C10 C9 175.6(9) . . . . ? C13 C9 C10 C1 -176.2(9) . . . . ? C19 C9 C10 C1 64.3(15) . . . . ? C16 C9 C10 C1 -52.9(13) . . . . ? C13 C9 C10 C11 3.5(11) . . . . ? C19 C9 C10 C11 -116.0(12) . . . . ? C16 C9 C10 C11 126.8(10) . . . . ? C1 C10 C11 C4 1.6(15) . . . . ? C9 C10 C11 C4 -178.1(9) . . . . ? C1 C10 C11 C12 178.6(8) . . . . ? C9 C10 C11 C12 -1.1(11) . . . . ? C3 C4 C11 C10 1.9(15) . . . . ? C3 C4 C11 C12 -174.4(10) . . . . ? C6 C5 C12 C13 0.8(17) . . . . ? C6 C5 C12 C11 175.2(10) . . . . ? C10 C11 C12 C13 -2.1(11) . . . . ? C4 C11 C12 C13 174.7(10) . . . . ? C10 C11 C12 C5 -177.2(11) . . . . ? C4 C11 C12 C5 -0.4(18) . . . . ? C5 C12 C13 C8 -2.7(17) . . . . ? C11 C12 C13 C8 -178.1(9) . . . . ? C5 C12 C13 C9 179.9(10) . . . . ? C11 C12 C13 C9 4.6(12) . . . . ? C7 C8 C13 C12 4.0(16) . . . . ? C7 C8 C13 C9 -179.1(10) . . . . ? C10 C9 C13 C12 -4.9(11) . . . . ? C19 C9 C13 C12 113.9(12) . . . . ? C16 C9 C13 C12 -125.4(10) . . . . ? C10 C9 C13 C8 178.0(10) . . . . ? C19 C9 C13 C8 -63.1(16) . . . . ? C16 C9 C13 C8 57.5(14) . . . . ? Zn1 O1 C14 O2 -3.6(14) . . . . ? Zn1 O1 C14 C2 176.8(5) . . . . ? Zn2 O2 C14 O1 35.6(14) . . . . ? Zn2 O2 C14 C2 -144.7(7) . . . . ? C3 C2 C14 O1 161.9(8) . . . . ? C1 C2 C14 O1 -17.5(11) . . . . ? C3 C2 C14 O2 -17.8(12) . . . . ? C1 C2 C14 O2 162.8(8) . . . . ? Zn1 O3 C15 O4 -2.6(14) 7 . . . ? Zn2 O3 C15 O4 103(2) 6_556 . . . ? Zn1 O3 C15 C7 -174.1(8) 7 . . . ? Zn2 O3 C15 C7 -68.9(18) 6_556 . . . ? Zn2 O3 C15 Zn1 105.2(16) 6_556 . . 7 ? Zn1 O4 C15 O3 2.4(13) 7 . . . ? Zn2 O4 C15 O3 -66(2) 5_556 . . . ? Zn1 O4 C15 C7 174.3(8) 7 . . . ? Zn2 O4 C15 C7 105.9(15) 5_556 . . . ? Zn2 O4 C15 Zn1 -68.4(15) 5_556 . . 7 ? C8 C7 C15 O3 -0.1(16) . . . . ? C6 C7 C15 O3 -177.5(11) . . . . ? C8 C7 C15 O4 -173.4(10) . . . . ? C6 C7 C15 O4 9.2(15) . . . . ? C8 C7 C15 Zn1 -70(11) . . . 7 ? C6 C7 C15 Zn1 113(10) . . . 7 ? C13 C9 C16 C17 51.4(12) . . . . ? C10 C9 C16 C17 -62.4(12) . . . . ? C19 C9 C16 C17 176.2(10) . . . . ? C9 C16 C17 C18 168.7(9) . . . . ? C13 C9 C19 C20 -53.1(15) . . . . ? C10 C9 C19 C20 58.6(16) . . . . ? C16 C9 C19 C20 -179.9(11) . . . . ? C9 C19 C20 C21 173.8(11) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.224 _refine_diff_density_min -1.252 _refine_diff_density_rms 0.135 #===END data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C23 H26 Cd O5' _chemical_formula_sum 'C23 H26 Cd O5' _chemical_formula_weight 494.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.5511(12) _cell_length_b 21.5004(13) _cell_length_c 14.0681(8) _cell_angle_alpha 90.00 _cell_angle_beta 130.5470(10) _cell_angle_gamma 90.00 _cell_volume 4723.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4650 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.660 _exptl_absorpt_correction_T_max 0.750 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean '9.00cm' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13095 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4650 _reflns_number_gt 4222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+53.2208P] 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 4650 _refine_ls_number_parameters 225 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1811 _refine_ls_wR_factor_gt 0.1775 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.0000 0.04131(2) 0.2500 0.01974(18) Uani 1 2 d S . . Cd2 Cd 0.5000 -0.5000 -0.5000 0.02296(19) Uani 1 2 d S . . O1 O 0.8725(3) -0.0222(2) 0.1446(4) 0.0316(9) Uani 1 1 d . . . O2 O 0.9528(3) -0.04031(17) 0.0961(4) 0.0282(8) Uani 1 1 d . . . O3 O 0.5882(3) -0.3824(2) -0.6080(4) 0.0365(10) Uani 1 1 d . . . O4 O 0.4928(2) -0.41085(16) -0.5913(3) 0.0244(8) Uani 1 1 d . . . O5 O 0.3622(3) -0.5199(3) -0.6739(4) 0.0463(11) Uani 1 1 d . . . C1 C 0.8346(4) -0.1279(3) -0.0882(5) 0.0286(12) Uani 1 1 d . . . H1 H 0.8750 -0.1125 -0.0924 0.090 Uiso 1 1 calc . . . C2 C 0.8288(4) -0.1042(3) -0.0013(5) 0.0275(11) Uani 1 1 d . . . C3 C 0.7685(4) -0.1277(3) 0.0050(6) 0.0388(14) Uani 1 1 d . . . H3 H 0.7649 -0.1111 0.0625 0.090 Uiso 1 1 calc . . . C4 C 0.7135(4) -0.1758(3) -0.0737(6) 0.0414(16) Uani 1 1 d . . . H4 H 0.6745 -0.1923 -0.0677 0.090 Uiso 1 1 calc . . . C5 C 0.6020(4) -0.2851(3) -0.2893(6) 0.0340(13) Uani 1 1 d . . . H5 H 0.5821 -0.2819 -0.2461 0.090 Uiso 1 1 calc . . . C6 C 0.5659(4) -0.3273(3) -0.3855(6) 0.0307(12) Uani 1 1 d . . . H6 H 0.5221 -0.3532 -0.4061 0.090 Uiso 1 1 calc . . . C7 C 0.5944(3) -0.3317(3) -0.4527(5) 0.0267(11) Uani 1 1 d . . . C8 C 0.6617(4) -0.2939(3) -0.4201(6) 0.0325(13) Uani 1 1 d . . . H8 H 0.6814 -0.2968 -0.4636 0.090 Uiso 1 1 calc . . . C9 C 0.7744(6) -0.2076(5) -0.2673(10) 0.0729(10) Uani 1 1 d . . . C10 C 0.7785(4) -0.1752(3) -0.1685(5) 0.0305(12) Uani 1 1 d . . . C11 C 0.7184(4) -0.1987(3) -0.1621(5) 0.0315(12) Uani 1 1 d . . . C12 C 0.6687(4) -0.2471(3) -0.2575(5) 0.0301(12) Uani 1 1 d . . . C13 C 0.6988(4) -0.2520(3) -0.3223(6) 0.0321(12) Uani 1 1 d . . . C14 C 0.8875(4) -0.0524(2) 0.0848(5) 0.0256(11) Uani 1 1 d . . . C15 C 0.5567(3) -0.3777(2) -0.5568(5) 0.0257(11) Uani 1 1 d . . . C16 C 0.8601(6) -0.2462(5) -0.2033(10) 0.0729(10) Uani 1 1 d . . . H16A H 0.8538 -0.2693 -0.2681 0.090 Uiso 1 1 calc . . . H16B H 0.9067 -0.2169 -0.1679 0.090 Uiso 1 1 calc . . . C17 C 0.8841(6) -0.2888(5) -0.1075(10) 0.0729(10) Uani 1 1 d . . . H17A H 0.8367 -0.3167 -0.1397 0.090 Uiso 1 1 calc . . . H17B H 0.8965 -0.2659 -0.0379 0.090 Uiso 1 1 calc . . . C18 C 0.9630(6) -0.3270(5) -0.0612(10) 0.0729(10) Uani 1 1 d . . . H18A H 0.9768 -0.3558 0.0018 0.090 Uiso 1 1 calc . . . H18B H 1.0106 -0.2996 -0.0263 0.090 Uiso 1 1 calc . . . H18C H 0.9510 -0.3495 -0.1300 0.090 Uiso 1 1 calc . . . C19 C 0.7611(6) -0.1641(5) -0.3635(10) 0.0729(10) Uani 1 1 d . . . H19A H 0.8098 -0.1362 -0.3211 0.090 Uiso 1 1 calc . . . H19B H 0.7599 -0.1886 -0.4225 0.090 Uiso 1 1 calc . . . C20 C 0.6850(6) -0.1277(5) -0.4314(10) 0.0729(10) Uani 1 1 d . . . H20A H 0.6863 -0.1021 -0.3734 0.090 Uiso 1 1 calc . . . H20B H 0.6358 -0.1551 -0.4737 0.090 Uiso 1 1 calc . . . C21 C 0.6748(6) -0.0843(5) -0.5316(10) 0.0729(10) Uani 1 1 d . . . H21A H 0.6232 -0.0603 -0.5747 0.090 Uiso 1 1 calc . . . H21B H 0.6717 -0.1096 -0.5906 0.090 Uiso 1 1 calc . . . H21C H 0.7231 -0.0569 -0.4900 0.090 Uiso 1 1 calc . . . C22 C 0.2872(9) -0.5317(7) -0.6907(14) 0.100(3) Uani 1 1 d U . . C23 C 0.2001(18) -0.5217(15) -0.783(3) 0.100(3) Uani 0.50 1 d PU . . C23' C 0.2146(18) -0.5620(15) -0.795(3) 0.100(3) Uani 0.50 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 Cd1 0.0234(3) 0.0161(3) 0.0139(3) 0.000 0.0096(2) 0.000 Cd2 0.0247(3) 0.0224(3) 0.0213(3) 0.00118(19) 0.0147(3) -0.00102(19) O1 0.033(2) 0.032(2) 0.027(2) -0.0100(17) 0.0183(18) -0.0062(17) O2 0.030(2) 0.027(2) 0.0237(19) -0.0071(15) 0.0162(18) -0.0100(15) O3 0.041(2) 0.039(2) 0.037(2) -0.0184(19) 0.029(2) -0.0170(19) O4 0.0253(18) 0.0201(17) 0.0208(18) -0.0023(14) 0.0118(16) -0.0043(15) O5 0.034(2) 0.062(3) 0.034(3) -0.005(2) 0.019(2) -0.010(2) C1 0.027(3) 0.029(3) 0.029(3) -0.008(2) 0.017(2) -0.009(2) C2 0.028(3) 0.028(3) 0.024(3) -0.007(2) 0.016(2) -0.006(2) C3 0.044(4) 0.044(4) 0.036(3) -0.020(3) 0.029(3) -0.018(3) C4 0.045(4) 0.050(4) 0.043(4) -0.024(3) 0.035(3) -0.028(3) C5 0.035(3) 0.040(3) 0.033(3) -0.015(3) 0.025(3) -0.016(3) C6 0.031(3) 0.032(3) 0.032(3) -0.010(2) 0.021(3) -0.013(2) C7 0.027(3) 0.025(3) 0.025(3) -0.005(2) 0.015(2) -0.005(2) C8 0.041(3) 0.031(3) 0.035(3) -0.013(2) 0.029(3) -0.013(3) C9 0.071(2) 0.070(2) 0.081(3) -0.0189(19) 0.050(2) -0.0227(19) C10 0.030(3) 0.029(3) 0.029(3) -0.007(2) 0.018(3) -0.008(2) C11 0.031(3) 0.032(3) 0.029(3) -0.010(2) 0.019(3) -0.011(2) C12 0.033(3) 0.029(3) 0.027(3) -0.008(2) 0.019(2) -0.010(2) C13 0.036(3) 0.033(3) 0.032(3) -0.012(2) 0.024(3) -0.011(2) C14 0.030(3) 0.022(2) 0.019(3) 0.000(2) 0.013(2) -0.001(2) C15 0.026(3) 0.021(2) 0.024(3) -0.002(2) 0.014(2) -0.003(2) C16 0.071(2) 0.070(2) 0.081(3) -0.0189(19) 0.050(2) -0.0227(19) C17 0.071(2) 0.070(2) 0.081(3) -0.0189(19) 0.050(2) -0.0227(19) C18 0.071(2) 0.070(2) 0.081(3) -0.0189(19) 0.050(2) -0.0227(19) C19 0.071(2) 0.070(2) 0.081(3) -0.0189(19) 0.050(2) -0.0227(19) C20 0.071(2) 0.070(2) 0.081(3) -0.0189(19) 0.050(2) -0.0227(19) C21 0.071(2) 0.070(2) 0.081(3) -0.0189(19) 0.050(2) -0.0227(19) C22 0.100(3) 0.100(3) 0.100(3) -0.0001(6) 0.065(2) -0.0001(6) C23 0.100(3) 0.100(3) 0.100(3) -0.0001(6) 0.065(2) -0.0001(6) C23' 0.100(3) 0.100(3) 0.100(3) -0.0001(6) 0.065(2) -0.0001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.294(4) 3_556 ? Cd1 O3 2.294(4) 4_654 ? Cd1 O1 2.424(4) . ? Cd1 O1 2.424(4) 2_755 ? Cd1 O2 2.445(4) . ? Cd1 O2 2.445(4) 2_755 ? Cd1 O4 2.548(4) 4_654 ? Cd1 O4 2.548(4) 3_556 ? Cd2 O4 2.258(4) . ? Cd2 O4 2.258(4) 5_644 ? Cd2 O5 2.276(5) . ? Cd2 O5 2.276(5) 5_644 ? Cd2 O2 2.286(4) 4_644 ? Cd2 O2 2.286(4) 8_445 ? O1 C14 1.248(7) . ? O2 C14 1.272(7) . ? O2 Cd2 2.286(4) 4_654 ? O3 C15 1.247(7) . ? O3 Cd1 2.294(4) 3_444 ? O4 C15 1.280(6) . ? O4 Cd1 2.548(4) 3_444 ? O5 C22 1.423(15) . ? C1 C10 1.395(8) . ? C1 C2 1.399(8) . ? C1 H1 0.9300 . ? C2 C3 1.394(8) . ? C2 C14 1.505(7) . ? C3 C4 1.394(8) . ? C3 H3 0.9300 . ? C4 C11 1.400(8) . ? C4 H4 0.9300 . ? C5 C6 1.379(8) . ? C5 C12 1.398(8) . ? C5 H5 0.9300 . ? C6 C7 1.403(8) . ? C6 H6 0.9300 . ? C7 C8 1.400(8) . ? C7 C15 1.498(7) . ? C8 C13 1.386(8) . ? C8 H8 0.9300 . ? C9 C10 1.508(12) . ? C9 C19 1.516(15) . ? C9 C13 1.537(10) . ? C9 C16 1.593(15) . ? C10 C11 1.390(8) . ? C11 C12 1.464(8) . ? C12 C13 1.397(8) . ? C16 C17 1.426(15) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.535(15) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.424(15) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.585(15) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.38(3) . ? C22 C23' 1.40(3) . ? C23 C23' 0.96(4) . ? 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 Cd1 O3 88.7(2) 3_556 4_654 ? O3 Cd1 O1 149.75(14) 3_556 . ? O3 Cd1 O1 86.69(16) 4_654 . ? O3 Cd1 O1 86.69(16) 3_556 2_755 ? O3 Cd1 O1 149.75(14) 4_654 2_755 ? O1 Cd1 O1 111.4(2) . 2_755 ? O3 Cd1 O2 156.73(14) 3_556 . ? O3 Cd1 O2 96.21(15) 4_654 . ? O1 Cd1 O2 53.49(13) . . ? O1 Cd1 O2 77.64(14) 2_755 . ? O3 Cd1 O2 96.21(15) 3_556 2_755 ? O3 Cd1 O2 156.73(14) 4_654 2_755 ? O1 Cd1 O2 77.64(14) . 2_755 ? O1 Cd1 O2 53.50(13) 2_755 2_755 ? O2 Cd1 O2 88.25(18) . 2_755 ? O3 Cd1 O4 90.64(14) 3_556 4_654 ? O3 Cd1 O4 53.94(13) 4_654 4_654 ? O1 Cd1 O4 110.29(13) . 4_654 ? O1 Cd1 O4 96.21(12) 2_755 4_654 ? O2 Cd1 O4 74.31(12) . 4_654 ? O2 Cd1 O4 148.22(12) 2_755 4_654 ? O3 Cd1 O4 53.94(13) 3_556 3_556 ? O3 Cd1 O4 90.64(14) 4_654 3_556 ? O1 Cd1 O4 96.21(12) . 3_556 ? O1 Cd1 O4 110.29(13) 2_755 3_556 ? O2 Cd1 O4 148.22(12) . 3_556 ? O2 Cd1 O4 74.31(12) 2_755 3_556 ? O4 Cd1 O4 132.38(16) 4_654 3_556 ? O4 Cd2 O4 180.0(2) . 5_644 ? O4 Cd2 O5 88.42(16) . . ? O4 Cd2 O5 91.58(17) 5_644 . ? O4 Cd2 O5 91.58(17) . 5_644 ? O4 Cd2 O5 88.42(16) 5_644 5_644 ? O5 Cd2 O5 180.000(1) . 5_644 ? O4 Cd2 O2 83.18(13) . 4_644 ? O4 Cd2 O2 96.82(13) 5_644 4_644 ? O5 Cd2 O2 90.15(17) . 4_644 ? O5 Cd2 O2 89.85(17) 5_644 4_644 ? O4 Cd2 O2 96.82(13) . 8_445 ? O4 Cd2 O2 83.18(13) 5_644 8_445 ? O5 Cd2 O2 89.85(17) . 8_445 ? O5 Cd2 O2 90.15(17) 5_644 8_445 ? O2 Cd2 O2 180.000(1) 4_644 8_445 ? C14 O1 Cd1 93.6(3) . . ? C14 O2 Cd2 145.3(4) . 4_654 ? C14 O2 Cd1 92.1(3) . . ? Cd2 O2 Cd1 100.09(13) 4_654 . ? C15 O3 Cd1 98.5(3) . 3_444 ? C15 O4 Cd2 125.8(3) . . ? C15 O4 Cd1 85.9(3) . 3_444 ? Cd2 O4 Cd1 97.83(13) . 3_444 ? C22 O5 Cd2 131.9(7) . . ? C10 C1 C2 118.5(5) . . ? C10 C1 H1 120.8 . . ? C2 C1 H1 120.8 . . ? C3 C2 C1 120.5(5) . . ? C3 C2 C14 119.8(5) . . ? C1 C2 C14 119.6(5) . . ? C2 C3 C4 120.9(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C11 118.5(5) . . ? C3 C4 H4 120.7 . . ? C11 C4 H4 120.7 . . ? C6 C5 C12 119.2(5) . . ? C6 C5 H5 120.4 . . ? C12 C5 H5 120.4 . . ? C5 C6 C7 120.8(5) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 119.8(5) . . ? C8 C7 C15 118.5(5) . . ? C6 C7 C15 121.7(5) . . ? C13 C8 C7 119.4(5) . . ? C13 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C19 114.0(8) . . ? C10 C9 C13 100.6(7) . . ? C19 C9 C13 113.4(8) . . ? C10 C9 C16 109.9(8) . . ? C19 C9 C16 108.5(8) . . ? C13 C9 C16 110.2(8) . . ? C11 C10 C1 121.0(5) . . ? C11 C10 C9 111.8(6) . . ? C1 C10 C9 127.2(6) . . ? C10 C11 C4 120.6(5) . . ? C10 C11 C12 108.5(5) . . ? C4 C11 C12 130.9(5) . . ? C13 C12 C5 120.3(5) . . ? C13 C12 C11 108.2(5) . . ? C5 C12 C11 131.5(5) . . ? C8 C13 C12 120.4(5) . . ? C8 C13 C9 128.8(6) . . ? C12 C13 C9 110.8(6) . . ? O1 C14 O2 120.8(5) . . ? O1 C14 C2 120.5(5) . . ? O2 C14 C2 118.7(5) . . ? O3 C15 O4 121.7(5) . . ? O3 C15 C7 119.0(5) . . ? O4 C15 C7 119.3(5) . . ? C17 C16 C9 116.4(9) . . ? C17 C16 H16A 108.2 . . ? C9 C16 H16A 108.2 . . ? C17 C16 H16B 108.2 . . ? C9 C16 H16B 108.2 . . ? H16A C16 H16B 107.3 . . ? C16 C17 C18 111.5(9) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C9 114.9(9) . . ? C20 C19 H19A 108.5 . . ? C9 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? C9 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C19 C20 C21 111.9(9) . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C23' 40.5(15) . . ? C23 C22 O5 136.6(17) . . ? C23' C22 O5 124.0(16) . . ? C23' C23 C22 71(3) . . ? C23 C23' C22 69(3) . . ? 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 Cd1 O1 C14 -177.4(3) 3_556 . . . ? O3 Cd1 O1 C14 100.9(3) 4_654 . . . ? O1 Cd1 O1 C14 -54.1(3) 2_755 . . . ? O2 Cd1 O1 C14 0.7(3) . . . . ? O2 Cd1 O1 C14 -96.4(3) 2_755 . . . ? O4 Cd1 O1 C14 51.5(3) 4_654 . . . ? O4 Cd1 O1 C14 -168.8(3) 3_556 . . . ? O3 Cd1 O2 C14 176.9(4) 3_556 . . . ? O3 Cd1 O2 C14 -81.9(3) 4_654 . . . ? O1 Cd1 O2 C14 -0.7(3) . . . . ? O1 Cd1 O2 C14 128.1(3) 2_755 . . . ? O2 Cd1 O2 C14 75.2(3) 2_755 . . . ? O4 Cd1 O2 C14 -131.7(3) 4_654 . . . ? O4 Cd1 O2 C14 19.4(4) 3_556 . . . ? O3 Cd1 O2 Cd2 -35.7(4) 3_556 . . 4_654 ? O3 Cd1 O2 Cd2 65.47(16) 4_654 . . 4_654 ? O1 Cd1 O2 Cd2 146.7(2) . . . 4_654 ? O1 Cd1 O2 Cd2 -84.49(15) 2_755 . . 4_654 ? O2 Cd1 O2 Cd2 -137.4(2) 2_755 . . 4_654 ? O4 Cd1 O2 Cd2 15.69(13) 4_654 . . 4_654 ? O4 Cd1 O2 Cd2 166.83(16) 3_556 . . 4_654 ? O4 Cd2 O4 C15 114(100) 5_644 . . . ? O5 Cd2 O4 C15 -164.5(4) . . . . ? O5 Cd2 O4 C15 15.5(4) 5_644 . . . ? O2 Cd2 O4 C15 -74.2(4) 4_644 . . . ? O2 Cd2 O4 C15 105.8(4) 8_445 . . . ? O4 Cd2 O4 Cd1 -156(100) 5_644 . . 3_444 ? O5 Cd2 O4 Cd1 -73.96(16) . . . 3_444 ? O5 Cd2 O4 Cd1 106.04(16) 5_644 . . 3_444 ? O2 Cd2 O4 Cd1 16.38(13) 4_644 . . 3_444 ? O2 Cd2 O4 Cd1 -163.62(13) 8_445 . . 3_444 ? O4 Cd2 O5 C22 -123.7(9) . . . . ? O4 Cd2 O5 C22 56.3(9) 5_644 . . . ? O5 Cd2 O5 C22 18(100) 5_644 . . . ? O2 Cd2 O5 C22 153.2(9) 4_644 . . . ? O2 Cd2 O5 C22 -26.8(9) 8_445 . . . ? C10 C1 C2 C3 0.3(9) . . . . ? C10 C1 C2 C14 -178.9(5) . . . . ? C1 C2 C3 C4 0.9(10) . . . . ? C14 C2 C3 C4 -179.9(6) . . . . ? C2 C3 C4 C11 -2.0(11) . . . . ? C12 C5 C6 C7 -1.1(10) . . . . ? C5 C6 C7 C8 1.6(9) . . . . ? C5 C6 C7 C15 179.4(6) . . . . ? C6 C7 C8 C13 -0.7(9) . . . . ? C15 C7 C8 C13 -178.6(6) . . . . ? C2 C1 C10 C11 -0.4(9) . . . . ? C2 C1 C10 C9 -179.2(7) . . . . ? C19 C9 C10 C11 124.3(8) . . . . ? C13 C9 C10 C11 2.6(9) . . . . ? C16 C9 C10 C11 -113.6(7) . . . . ? C19 C9 C10 C1 -56.8(11) . . . . ? C13 C9 C10 C1 -178.5(6) . . . . ? C16 C9 C10 C1 65.3(10) . . . . ? C1 C10 C11 C4 -0.7(10) . . . . ? C9 C10 C11 C4 178.3(7) . . . . ? C1 C10 C11 C12 179.6(5) . . . . ? C9 C10 C11 C12 -1.4(8) . . . . ? C3 C4 C11 C10 1.9(11) . . . . ? C3 C4 C11 C12 -178.6(7) . . . . ? C6 C5 C12 C13 -0.2(10) . . . . ? C6 C5 C12 C11 179.7(6) . . . . ? C10 C11 C12 C13 -0.7(7) . . . . ? C4 C11 C12 C13 179.7(7) . . . . ? C10 C11 C12 C5 179.5(7) . . . . ? C4 C11 C12 C5 -0.1(12) . . . . ? C7 C8 C13 C12 -0.6(10) . . . . ? C7 C8 C13 C9 177.9(7) . . . . ? C5 C12 C13 C8 1.1(10) . . . . ? C11 C12 C13 C8 -178.8(6) . . . . ? C5 C12 C13 C9 -177.7(7) . . . . ? C11 C12 C13 C9 2.4(8) . . . . ? C10 C9 C13 C8 178.3(7) . . . . ? C19 C9 C13 C8 56.2(12) . . . . ? C16 C9 C13 C8 -65.7(11) . . . . ? C10 C9 C13 C12 -3.0(9) . . . . ? C19 C9 C13 C12 -125.1(8) . . . . ? C16 C9 C13 C12 113.0(8) . . . . ? Cd1 O1 C14 O2 -1.3(5) . . . . ? Cd1 O1 C14 C2 178.1(4) . . . . ? Cd2 O2 C14 O1 -109.8(6) 4_654 . . . ? Cd1 O2 C14 O1 1.3(5) . . . . ? Cd2 O2 C14 C2 70.8(8) 4_654 . . . ? Cd1 O2 C14 C2 -178.1(4) . . . . ? C3 C2 C14 O1 -13.7(9) . . . . ? C1 C2 C14 O1 165.5(5) . . . . ? C3 C2 C14 O2 165.7(6) . . . . ? C1 C2 C14 O2 -15.1(8) . . . . ? Cd1 O3 C15 O4 -0.5(6) 3_444 . . . ? Cd1 O3 C15 C7 179.8(4) 3_444 . . . ? Cd2 O4 C15 O3 97.1(6) . . . . ? Cd1 O4 C15 O3 0.4(5) 3_444 . . . ? Cd2 O4 C15 C7 -83.2(6) . . . . ? Cd1 O4 C15 C7 -179.9(5) 3_444 . . . ? C8 C7 C15 O3 2.5(8) . . . . ? C6 C7 C15 O3 -175.4(6) . . . . ? C8 C7 C15 O4 -177.2(5) . . . . ? C6 C7 C15 O4 4.9(8) . . . . ? C10 C9 C16 C17 53.3(10) . . . . ? C19 C9 C16 C17 178.6(8) . . . . ? C13 C9 C16 C17 -56.7(11) . . . . ? C9 C16 C17 C18 175.1(7) . . . . ? C10 C9 C19 C20 -58.9(11) . . . . ? C13 C9 C19 C20 55.3(11) . . . . ? C16 C9 C19 C20 178.2(8) . . . . ? C9 C19 C20 C21 -179.0(8) . . . . ? Cd2 O5 C22 C23 150(2) . . . . ? Cd2 O5 C22 C23' -158.6(17) . . . . ? O5 C22 C23 C23' 91(3) . . . . ? O5 C22 C23' C23 -124(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.759 _refine_diff_density_min -2.233 _refine_diff_density_rms 0.189 #===END data_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C140 H142 N16 O19 Zn4' _chemical_formula_sum 'C140 H142 N16 O19 Zn4' _chemical_formula_weight 2614.18 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 triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_Hall p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7354(7) _cell_length_b 13.8485(8) _cell_length_c 22.4233(12) _cell_angle_alpha 88.4380(10) _cell_angle_beta 85.2750(10) _cell_angle_gamma 70.7740(10) _cell_volume 4013.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 15341 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1366 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7712 _exptl_absorpt_correction_T_max 0.8671 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22465 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.03 _reflns_number_total 15341 _reflns_number_gt 11751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1472P)^2^+4.2702P] 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 15341 _refine_ls_number_parameters 820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2336 _refine_ls_wR_factor_gt 0.2153 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 C1 C 0.0855(4) 1.7053(4) 0.2275(4) 0.0657(19) Uani 1 1 d . . . H1 H 0.0518 1.7530 0.2571 0.079 Uiso 1 1 calc R . . C2 C 0.0592(4) 1.7223(5) 0.1678(4) 0.081(2) Uani 1 1 d . . . C3 C 0.1114(5) 1.6543(6) 0.1250(4) 0.098(3) Uani 1 1 d . . . H3 H 0.0935 1.6672 0.0857 0.118 Uiso 1 1 calc R . . C4 C 0.1913(5) 1.5654(6) 0.1374(3) 0.081(2) Uani 1 1 d . . . H4 H 0.2264 1.5194 0.1072 0.097 Uiso 1 1 calc R . . C5 C 0.3683(4) 1.3760(4) 0.1955(2) 0.0543(14) Uani 1 1 d . . . H5 H 0.3715 1.3658 0.1544 0.065 Uiso 1 1 calc R . . C6 C 0.4353(3) 1.3054(3) 0.2309(2) 0.0428(11) Uani 1 1 d . . . H6 H 0.4831 1.2467 0.2136 0.051 Uiso 1 1 calc R . . C7 C 0.4319(3) 1.3215(3) 0.2924(2) 0.0314(9) Uani 1 1 d . . . C8 C 0.3585(3) 1.4074(3) 0.3193(2) 0.0361(9) Uani 1 1 d . . . H8 H 0.3549 1.4170 0.3604 0.043 Uiso 1 1 calc R . . C9 C 0.2014(3) 1.5765(3) 0.3015(3) 0.0486(13) Uani 1 1 d . . . C10 C 0.1637(4) 1.6148(3) 0.2413(3) 0.0528(14) Uani 1 1 d . . . C11 C 0.2166(4) 1.5476(4) 0.1955(3) 0.0568(14) Uani 1 1 d . . . C12 C 0.2961(3) 1.4624(3) 0.2223(2) 0.0436(11) Uani 1 1 d . . . C13 C 0.2909(3) 1.4783(3) 0.2842(2) 0.0387(10) Uani 1 1 d . . . C14 C -0.0262(5) 1.8187(8) 0.1542(6) 0.120(5) Uani 1 1 d . . . C15 C 0.5075(3) 1.2466(3) 0.33003(19) 0.0295(8) Uani 1 1 d . . . C16 C 0.2391(4) 1.6587(4) 0.3296(3) 0.0656(17) Uani 1 1 d . . . H16A H 0.2910 1.6715 0.3015 0.079 Uiso 1 1 calc R . . H16B H 0.1810 1.7218 0.3335 0.079 Uiso 1 1 calc R . . C17 C 0.2830(6) 1.6357(5) 0.3884(4) 0.082(2) Uani 1 1 d . . . H17A H 0.3438 1.5749 0.3851 0.098 Uiso 1 1 calc R . . H17B H 0.2327 1.6221 0.4173 0.098 Uiso 1 1 calc R . . C18 C 0.3133(7) 1.7273(6) 0.4103(5) 0.121(4) Uani 1 1 d . . . H18A H 0.3416 1.7110 0.4485 0.181 Uiso 1 1 calc R . . H18B H 0.2530 1.7872 0.4140 0.181 Uiso 1 1 calc R . . H18C H 0.3640 1.7399 0.3819 0.181 Uiso 1 1 calc R . . C19 C 0.1168(4) 1.5516(4) 0.3420(3) 0.0561(14) Uani 1 1 d . . . H19A H 0.1443 1.5265 0.3800 0.067 Uiso 1 1 calc R . . H19B H 0.0595 1.6144 0.3498 0.067 Uiso 1 1 calc R . . C20 C 0.0756(4) 1.4736(4) 0.3169(3) 0.0649(16) Uani 1 1 d . . . H20A H 0.0532 1.4955 0.2774 0.078 Uiso 1 1 calc R . . H20B H 0.1313 1.4087 0.3125 0.078 Uiso 1 1 calc R . . C21 C -0.0131(6) 1.4575(7) 0.3550(4) 0.100(3) Uani 1 1 d . . . H21A H -0.0354 1.4074 0.3366 0.150 Uiso 1 1 calc R . . H21B H -0.0694 1.5209 0.3589 0.150 Uiso 1 1 calc R . . H21C H 0.0088 1.4339 0.3939 0.150 Uiso 1 1 calc R . . C22 C -0.3031(4) 2.3665(3) 0.2252(2) 0.0396(10) Uani 1 1 d . . . H22 H -0.3646 2.3526 0.2335 0.047 Uiso 1 1 calc R . . C23 C -0.2170(3) 2.2939(3) 0.1965(2) 0.0363(9) Uani 1 1 d . . . C24 C -0.1257(4) 2.3164(3) 0.1841(2) 0.0426(11) Uani 1 1 d . . . H24 H -0.0682 2.2673 0.1657 0.051 Uiso 1 1 calc R . . C25 C -0.1188(4) 2.4102(3) 0.1986(2) 0.0441(11) Uani 1 1 d . . . H25 H -0.0578 2.4249 0.1898 0.053 Uiso 1 1 calc R . . C26 C -0.1576(3) 2.6471(3) 0.2431(2) 0.0429(11) Uani 1 1 d . . . H26 H -0.0918 2.6226 0.2236 0.051 Uiso 1 1 calc R . . C27 C -0.1931(3) 2.7432(3) 0.2686(2) 0.0385(10) Uani 1 1 d . . . H27 H -0.1500 2.7829 0.2669 0.046 Uiso 1 1 calc R . . C28 C -0.2923(3) 2.7820(3) 0.29685(19) 0.0318(9) Uani 1 1 d . . . C29 C -0.3588(3) 2.7238(3) 0.2982(2) 0.0345(9) Uani 1 1 d . . . H29 H -0.4262 2.7502 0.3153 0.041 Uiso 1 1 calc R . . C30 C -0.3806(3) 2.5497(3) 0.2716(2) 0.0433(11) Uani 1 1 d . . . C31 C -0.2958(3) 2.4594(3) 0.2410(2) 0.0408(11) Uani 1 1 d . . . C32 C -0.2054(3) 2.4822(3) 0.2268(2) 0.0391(10) Uani 1 1 d . . . C33 C -0.2224(3) 2.5873(3) 0.2472(2) 0.0368(10) Uani 1 1 d . . . C34 C -0.3230(3) 2.6263(3) 0.2736(2) 0.0365(10) Uani 1 1 d . . . C35 C -0.2263(4) 2.1943(3) 0.1777(2) 0.0366(10) Uani 1 1 d . . . C36 C -0.3313(3) 2.8856(3) 0.32515(18) 0.0300(9) Uani 1 1 d . . . C37 C -0.4748(4) 2.5890(4) 0.2344(3) 0.0561(15) Uani 1 1 d . . . H37A H -0.5106 2.5390 0.2368 0.067 Uiso 1 1 calc R . . H37B H -0.5217 2.6515 0.2526 0.067 Uiso 1 1 calc R . . C38 C -0.4534(5) 2.6104(5) 0.1687(3) 0.0670(16) Uani 1 1 d . . . H38A H -0.4130 2.6563 0.1656 0.080 Uiso 1 1 calc R . . H38B H -0.4120 2.5468 0.1491 0.080 Uiso 1 1 calc R . . C39 C -0.5495(6) 2.6569(6) 0.1362(4) 0.094(2) Uani 1 1 d . . . H39A H -0.5305 2.6685 0.0951 0.141 Uiso 1 1 calc R . . H39B H -0.5901 2.7208 0.1546 0.141 Uiso 1 1 calc R . . H39C H -0.5891 2.6112 0.1381 0.141 Uiso 1 1 calc R . . C40 C -0.4157(4) 2.5226(4) 0.3348(3) 0.0539(14) Uani 1 1 d . . . H40A H -0.4701 2.5821 0.3514 0.065 Uiso 1 1 calc R . . H40B H -0.4456 2.4688 0.3314 0.065 Uiso 1 1 calc R . . C41 C -0.3327(6) 2.4879(5) 0.3788(3) 0.0722(18) Uani 1 1 d . . . H41A H -0.2785 2.4274 0.3633 0.087 Uiso 1 1 calc R . . H41B H -0.3022 2.5412 0.3829 0.087 Uiso 1 1 calc R . . C42 C -0.3756(8) 2.4642(6) 0.4399(4) 0.106(3) Uani 1 1 d . . . H42A H -0.3210 2.4428 0.4665 0.160 Uiso 1 1 calc R . . H42B H -0.4045 2.4104 0.4363 0.160 Uiso 1 1 calc R . . H42C H -0.4285 2.5243 0.4557 0.160 Uiso 1 1 calc R . . C43 C 0.7188(3) 0.9122(3) 0.61966(18) 0.0310(9) Uani 1 1 d . . . C44 C 0.7472(4) 0.8383(4) 0.6636(2) 0.0430(11) Uani 1 1 d . . . H44 H 0.7108 0.7926 0.6706 0.052 Uiso 1 1 calc R . . C45 C 0.8301(4) 0.8317(4) 0.6975(2) 0.0436(11) Uani 1 1 d . . . H45 H 0.8481 0.7816 0.7268 0.052 Uiso 1 1 calc R . . C46 C 0.8853(3) 0.8978(4) 0.6882(2) 0.0414(11) Uani 1 1 d . . . C47 C 0.8555(4) 0.9727(5) 0.6449(3) 0.0601(16) Uani 1 1 d . . . H47 H 0.8913 1.0189 0.6384 0.072 Uiso 1 1 calc R . . C48 C 0.7730(4) 0.9801(4) 0.6107(2) 0.0521(13) Uani 1 1 d . . . H48 H 0.7544 1.0310 0.5818 0.062 Uiso 1 1 calc R . . C49 C 0.9730(3) 0.8930(5) 0.7255(2) 0.0514(13) Uani 1 1 d . . . H49A H 0.9590 0.9584 0.7450 0.062 Uiso 1 1 calc R . . H49B H 0.9784 0.8414 0.7564 0.062 Uiso 1 1 calc R . . C50 C 0.6270(3) 0.9167(3) 0.5847(2) 0.0341(9) Uani 1 1 d . . . H50A H 0.6386 0.8501 0.5674 0.041 Uiso 1 1 calc R . . H50B H 0.5653 0.9323 0.6121 0.041 Uiso 1 1 calc R . . C51 C 0.7942(4) 1.2068(4) 0.3724(3) 0.0632(17) Uani 1 1 d . . . H51 H 0.7483 1.2523 0.3997 0.076 Uiso 1 1 calc R . . C52 C 0.8860(4) 1.2121(4) 0.3509(3) 0.0702(19) Uani 1 1 d . . . H52 H 0.9157 1.2605 0.3606 0.084 Uiso 1 1 calc R . . C53 C 0.8607(3) 1.0813(3) 0.31196(19) 0.0343(9) Uani 1 1 d . . . H53 H 0.8709 1.0229 0.2894 0.041 Uiso 1 1 calc R . . C54 C 0.5680(3) 1.1389(3) 0.48912(19) 0.0334(9) Uani 1 1 d . . . H54 H 0.5415 1.2082 0.4803 0.040 Uiso 1 1 calc R . . C55 C 0.5600(3) 1.0971(3) 0.5436(2) 0.0375(10) Uani 1 1 d . . . H55 H 0.5275 1.1315 0.5785 0.045 Uiso 1 1 calc R . . C56 C 0.6456(3) 0.9762(3) 0.47975(18) 0.0319(9) Uani 1 1 d . . . H56 H 0.6826 0.9121 0.4638 0.038 Uiso 1 1 calc R . . C57 C -0.8114(4) 2.0221(5) 0.1386(2) 0.0493(13) Uani 1 1 d . . . C58 C -0.7784(4) 1.9435(5) 0.1781(2) 0.0519(13) Uani 1 1 d . . . H58 H -0.8137 1.8967 0.1845 0.062 Uiso 1 1 calc R . . C59 C -0.6913(4) 1.9337(4) 0.2088(2) 0.0480(12) Uani 1 1 d . . . H59 H -0.6694 1.8801 0.2357 0.058 Uiso 1 1 calc R . . C60 C -0.6372(3) 2.0010(4) 0.2003(2) 0.0403(10) Uani 1 1 d . . . C61 C -0.6712(4) 2.0804(5) 0.1611(3) 0.0585(14) Uani 1 1 d . . . H61 H -0.6358 2.1271 0.1552 0.070 Uiso 1 1 calc R . . C62 C -0.7584(4) 2.0923(5) 0.1298(3) 0.0606(15) Uani 1 1 d . . . H62 H -0.7808 2.1466 0.1033 0.073 Uiso 1 1 calc R . . C63 C -0.9073(4) 2.0357(6) 0.1054(2) 0.0661(18) Uani 1 1 d . . . H63A H -0.9527 2.0055 0.1286 0.079 Uiso 1 1 calc R . . H63B H -0.9444 2.1080 0.1008 0.079 Uiso 1 1 calc R . . C64 C -0.5446(4) 1.9898(4) 0.2354(2) 0.0469(12) Uani 1 1 d . . . H64A H -0.5537 2.0541 0.2551 0.056 Uiso 1 1 calc R . . H64B H -0.5403 1.9382 0.2662 0.056 Uiso 1 1 calc R . . C65 C -0.4104(4) 1.8778(4) 0.1593(3) 0.0530(13) Uani 1 1 d . . . H65 H -0.4441 1.8318 0.1513 0.064 Uiso 1 1 calc R . . C66 C -0.3146(4) 1.8756(4) 0.1360(2) 0.0479(12) Uani 1 1 d . . . H66 H -0.2709 1.8271 0.1094 0.057 Uiso 1 1 calc R . . C67 C -0.3755(3) 2.0064(3) 0.19538(19) 0.0329(9) Uani 1 1 d . . . H67 H -0.3819 2.0646 0.2173 0.039 Uiso 1 1 calc R . . C68 C -0.8331(5) 1.8760(4) -0.0259(2) 0.0567(14) Uani 1 1 d . . . H68 H -0.8126 1.8146 -0.0468 0.068 Uiso 1 1 calc R . . C69 C -0.8517(5) 1.8853(5) 0.0338(3) 0.0665(16) Uani 1 1 d . . . H69 H -0.8465 1.8327 0.0613 0.080 Uiso 1 1 calc R . . C70 C -0.8775(4) 2.0344(4) -0.0059(2) 0.0458(11) Uani 1 1 d . . . H70 H -0.8943 2.1049 -0.0097 0.055 Uiso 1 1 calc R . . N1 N 0.7780(3) 1.1243(3) 0.34820(17) 0.0334(8) Uani 1 1 d . . . N2 N 0.9277(3) 1.1322(3) 0.31188(18) 0.0422(9) Uani 1 1 d . . . N3 N 0.6097(3) 0.9931(3) 0.53718(15) 0.0313(7) Uani 1 1 d . . . N4 N 0.6216(3) 1.0627(2) 0.44844(15) 0.0301(7) Uani 1 1 d . . . N5 N -0.2939(3) 1.9580(3) 0.15886(16) 0.0335(8) Uani 1 1 d . . . N6 N -0.4471(3) 1.9604(3) 0.19650(17) 0.0376(8) Uani 1 1 d . . . N7 N -0.8797(3) 1.9871(4) 0.04593(17) 0.0487(11) Uani 1 1 d . . . N8 N -0.8489(3) 1.9708(3) -0.05131(16) 0.0392(8) Uani 1 1 d . . . O1 O 0.5264(3) 1.2739(2) 0.37837(15) 0.0488(8) Uani 1 1 d . . . O2 O 0.5501(2) 1.1553(2) 0.30906(13) 0.0330(6) Uani 1 1 d . . . O1W O -0.0752(10) 2.8293(8) 0.3892(6) 0.117(4) Uani 0.50 1 d P . . O3 O -0.0731(4) 1.8103(5) 0.1039(3) 0.113(2) Uani 1 1 d . . . O2W O -0.9586(14) 2.2890(12) 0.0482(6) 0.148(6) Uani 0.50 1 d P . . O4 O -0.0513(3) 1.8915(4) 0.1813(4) 0.152(4) Uani 1 1 d . . . O3W O 0.7995(13) 0.7461(10) 0.4656(9) 0.166(7) Uani 0.50 1 d P . . O5 O -0.3113(3) 2.1906(3) 0.16617(19) 0.0553(9) Uani 1 1 d . . . O6 O -0.1430(2) 2.1177(2) 0.17240(14) 0.0404(7) Uani 1 1 d . . . O7 O -0.4225(2) 2.9216(2) 0.34550(13) 0.0364(7) Uani 1 1 d . . . O8 O -0.2665(2) 2.9347(2) 0.32738(14) 0.0363(7) Uani 1 1 d . . . Zn1 Zn 0.65605(3) 1.07389(3) 0.36072(2) 0.02660(15) Uani 1 1 d . . . Zn2 Zn -0.16662(3) 1.99647(3) 0.13939(2) 0.02942(15) 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 C1 0.024(2) 0.034(3) 0.136(6) 0.015(3) 0.000(3) -0.007(2) C2 0.031(3) 0.059(4) 0.139(7) 0.066(4) -0.007(4) 0.000(3) C3 0.042(3) 0.106(6) 0.118(6) 0.073(5) -0.007(4) 0.008(4) C4 0.049(3) 0.087(5) 0.081(5) 0.038(4) -0.014(3) 0.010(3) C5 0.044(3) 0.052(3) 0.049(3) 0.010(2) -0.010(2) 0.010(2) C6 0.034(2) 0.034(2) 0.048(3) 0.006(2) -0.006(2) 0.0051(19) C7 0.0232(19) 0.0239(19) 0.045(2) 0.0048(17) -0.0073(17) -0.0046(15) C8 0.031(2) 0.027(2) 0.051(3) -0.0010(18) -0.0071(19) -0.0092(17) C9 0.026(2) 0.022(2) 0.092(4) -0.010(2) -0.006(2) -0.0001(17) C10 0.028(2) 0.029(2) 0.101(4) 0.020(3) -0.014(3) -0.0085(19) C11 0.032(3) 0.045(3) 0.081(4) 0.023(3) -0.004(3) 0.002(2) C12 0.032(2) 0.035(2) 0.057(3) 0.012(2) -0.008(2) -0.0017(19) C13 0.024(2) 0.023(2) 0.068(3) 0.002(2) -0.005(2) -0.0062(16) C14 0.024(3) 0.109(7) 0.201(10) 0.121(7) 0.001(5) 0.000(4) C15 0.026(2) 0.0248(19) 0.037(2) 0.0017(16) -0.0033(16) -0.0078(16) C16 0.043(3) 0.034(3) 0.114(5) -0.015(3) -0.008(3) -0.003(2) C17 0.078(5) 0.053(4) 0.114(6) -0.017(4) -0.013(4) -0.020(3) C18 0.102(6) 0.070(5) 0.194(11) -0.060(6) -0.029(6) -0.023(5) C19 0.033(3) 0.041(3) 0.085(4) -0.008(3) 0.005(3) -0.002(2) C20 0.043(3) 0.050(3) 0.103(5) 0.004(3) -0.005(3) -0.016(2) C21 0.069(5) 0.122(7) 0.125(7) 0.028(5) -0.008(4) -0.056(5) C22 0.038(2) 0.030(2) 0.052(3) -0.0097(19) 0.004(2) -0.0148(19) C23 0.040(2) 0.023(2) 0.044(2) -0.0031(17) -0.0022(19) -0.0083(18) C24 0.036(2) 0.029(2) 0.056(3) -0.008(2) 0.002(2) -0.0029(18) C25 0.032(2) 0.030(2) 0.067(3) -0.011(2) 0.009(2) -0.0088(18) C26 0.028(2) 0.029(2) 0.070(3) -0.006(2) 0.005(2) -0.0086(18) C27 0.031(2) 0.030(2) 0.055(3) -0.0032(19) -0.001(2) -0.0114(18) C28 0.029(2) 0.0235(19) 0.041(2) -0.0003(17) -0.0039(17) -0.0063(16) C29 0.029(2) 0.028(2) 0.044(2) -0.0049(18) 0.0008(18) -0.0061(17) C30 0.031(2) 0.026(2) 0.073(3) -0.017(2) 0.011(2) -0.0124(18) C31 0.036(2) 0.027(2) 0.059(3) -0.007(2) 0.006(2) -0.0107(18) C32 0.032(2) 0.029(2) 0.055(3) -0.0056(19) -0.001(2) -0.0085(18) C33 0.030(2) 0.025(2) 0.053(3) -0.0058(18) 0.0036(19) -0.0061(17) C34 0.033(2) 0.027(2) 0.050(3) -0.0069(18) 0.0016(19) -0.0114(18) C35 0.047(3) 0.024(2) 0.037(2) -0.0049(17) 0.0021(19) -0.0096(19) C36 0.037(2) 0.0218(19) 0.031(2) 0.0043(15) -0.0116(17) -0.0079(17) C37 0.034(3) 0.044(3) 0.092(4) -0.030(3) 0.007(3) -0.015(2) C38 0.056(4) 0.054(3) 0.090(5) -0.010(3) -0.012(3) -0.015(3) C39 0.088(5) 0.075(5) 0.114(6) -0.015(4) -0.041(5) -0.009(4) C40 0.048(3) 0.034(2) 0.079(4) -0.017(2) 0.025(3) -0.020(2) C41 0.086(5) 0.055(3) 0.074(4) 0.000(3) 0.016(4) -0.027(3) C42 0.150(8) 0.082(5) 0.086(5) -0.008(4) 0.041(5) -0.046(5) C43 0.026(2) 0.033(2) 0.033(2) 0.0035(17) -0.0014(16) -0.0078(17) C44 0.041(3) 0.045(3) 0.049(3) 0.014(2) -0.010(2) -0.022(2) C45 0.036(2) 0.047(3) 0.045(3) 0.018(2) -0.010(2) -0.010(2) C46 0.024(2) 0.060(3) 0.039(2) 0.010(2) -0.0054(18) -0.014(2) C47 0.053(3) 0.074(4) 0.073(4) 0.032(3) -0.029(3) -0.044(3) C48 0.052(3) 0.065(3) 0.053(3) 0.033(3) -0.026(2) -0.035(3) C49 0.027(2) 0.084(4) 0.044(3) 0.009(3) -0.007(2) -0.019(2) C50 0.031(2) 0.035(2) 0.039(2) 0.0066(18) -0.0092(18) -0.0138(18) C51 0.045(3) 0.040(3) 0.107(5) -0.031(3) 0.012(3) -0.019(2) C52 0.044(3) 0.053(3) 0.124(6) -0.029(3) 0.009(3) -0.032(3) C53 0.025(2) 0.042(2) 0.038(2) 0.0040(19) -0.0090(17) -0.0130(18) C54 0.037(2) 0.029(2) 0.036(2) -0.0016(17) -0.0098(18) -0.0126(18) C55 0.037(2) 0.035(2) 0.042(2) -0.0066(19) -0.0083(19) -0.0111(19) C56 0.034(2) 0.028(2) 0.034(2) -0.0003(16) -0.0083(17) -0.0098(17) C57 0.030(2) 0.086(4) 0.031(2) -0.011(2) 0.0012(19) -0.018(2) C58 0.036(3) 0.074(4) 0.050(3) -0.006(3) -0.003(2) -0.024(3) C59 0.041(3) 0.057(3) 0.047(3) 0.004(2) -0.010(2) -0.017(2) C60 0.032(2) 0.056(3) 0.033(2) -0.001(2) -0.0019(18) -0.015(2) C61 0.053(3) 0.076(4) 0.058(3) 0.017(3) -0.017(3) -0.035(3) C62 0.050(3) 0.077(4) 0.052(3) 0.019(3) -0.015(3) -0.017(3) C63 0.033(3) 0.121(5) 0.037(3) -0.014(3) -0.003(2) -0.014(3) C64 0.035(2) 0.068(3) 0.041(3) -0.001(2) -0.004(2) -0.021(2) C65 0.050(3) 0.050(3) 0.066(3) -0.013(3) -0.005(3) -0.025(2) C66 0.042(3) 0.039(3) 0.062(3) -0.017(2) -0.005(2) -0.010(2) C67 0.031(2) 0.033(2) 0.033(2) 0.0004(17) -0.0067(17) -0.0070(17) C68 0.080(4) 0.047(3) 0.046(3) 0.002(2) 0.000(3) -0.026(3) C69 0.090(5) 0.070(4) 0.047(3) 0.010(3) -0.002(3) -0.038(4) C70 0.039(3) 0.054(3) 0.040(3) -0.004(2) -0.011(2) -0.007(2) N1 0.0304(18) 0.0278(17) 0.045(2) 0.0019(15) -0.0072(15) -0.0128(14) N2 0.0284(19) 0.052(2) 0.048(2) 0.0067(19) -0.0094(16) -0.0152(17) N3 0.0304(18) 0.0344(18) 0.0305(18) 0.0016(14) -0.0082(14) -0.0113(15) N4 0.0308(18) 0.0285(17) 0.0329(18) -0.0012(14) -0.0093(14) -0.0106(14) N5 0.0316(18) 0.0284(17) 0.040(2) -0.0012(15) -0.0093(15) -0.0073(15) N6 0.0316(19) 0.042(2) 0.040(2) -0.0017(16) -0.0080(16) -0.0123(16) N7 0.029(2) 0.080(3) 0.034(2) -0.003(2) -0.0064(16) -0.012(2) N8 0.035(2) 0.047(2) 0.0332(19) -0.0018(16) -0.0037(15) -0.0111(17) O1 0.061(2) 0.0314(16) 0.048(2) -0.0033(14) -0.0206(17) -0.0029(15) O2 0.0307(15) 0.0230(14) 0.0409(16) 0.0013(12) -0.0100(12) -0.0012(11) O1W 0.129(10) 0.064(6) 0.123(10) -0.003(6) -0.032(8) 0.023(6) O3 0.063(3) 0.119(5) 0.111(4) 0.051(4) 0.003(3) 0.027(3) O2W 0.199(15) 0.131(11) 0.108(10) 0.020(9) 0.012(10) -0.053(11) O4 0.027(2) 0.036(2) 0.386(13) 0.075(4) -0.030(4) -0.004(2) O3W 0.162(14) 0.078(8) 0.237(19) 0.038(10) 0.024(13) -0.025(9) O5 0.045(2) 0.0352(18) 0.086(3) -0.0167(18) 0.0014(18) -0.0143(15) O6 0.0498(19) 0.0246(15) 0.0425(17) -0.0048(13) -0.0126(14) -0.0039(13) O7 0.0316(16) 0.0329(15) 0.0420(17) -0.0087(13) -0.0018(13) -0.0065(13) O8 0.0328(16) 0.0234(14) 0.0542(19) -0.0048(13) -0.0083(13) -0.0100(12) Zn1 0.0243(2) 0.0224(2) 0.0328(3) 0.00095(18) -0.00666(18) -0.00615(18) Zn2 0.0263(3) 0.0249(3) 0.0337(3) -0.00169(19) -0.00715(19) -0.00266(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C10 1.402(7) . ? C1 C2 1.408(10) . ? C1 H1 0.9300 . ? C2 C3 1.348(12) . ? C2 C14 1.502(8) . ? C3 C4 1.392(8) . ? C3 H3 0.9300 . ? C4 C11 1.372(9) . ? C4 H4 0.9300 . ? C5 C6 1.386(6) . ? C5 C12 1.391(7) . ? C5 H5 0.9300 . ? C6 C7 1.397(6) . ? C6 H6 0.9300 . ? C7 C8 1.395(6) . ? C7 C15 1.501(5) . ? C8 C13 1.387(6) . ? C8 H8 0.9300 . ? C9 C10 1.506(8) . ? C9 C13 1.537(6) . ? C9 C19 1.538(7) . ? C9 C16 1.563(7) . ? C10 C11 1.390(8) . ? C11 C12 1.472(6) . ? C12 C13 1.404(7) . ? C14 O4 1.128(15) . ? C14 O3 1.371(14) . ? C15 O1 1.232(5) . ? C15 O2 1.290(5) . ? C16 C17 1.477(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.562(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.514(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.503(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C31 1.380(6) . ? C22 C23 1.396(6) . ? C22 H22 0.9300 . ? C23 C24 1.394(6) . ? C23 C35 1.501(6) . ? C24 C25 1.383(6) . ? C24 H24 0.9300 . ? C25 C32 1.392(6) . ? C25 H25 0.9300 . ? C26 C27 1.379(6) . ? C26 C33 1.398(6) . ? C26 H26 0.9300 . ? C27 C28 1.394(6) . ? C27 H27 0.9300 . ? C28 C29 1.401(6) . ? C28 C36 1.496(5) . ? C29 C34 1.387(6) . ? C29 H29 0.9300 . ? C30 C34 1.523(6) . ? C30 C31 1.533(6) . ? C30 C40 1.534(7) . ? C30 C37 1.536(8) . ? C31 C32 1.388(6) . ? C32 C33 1.476(6) . ? C33 C34 1.394(6) . ? C35 O5 1.233(6) . ? C35 O6 1.278(5) . ? C36 O7 1.238(5) . ? C36 O8 1.290(5) . ? C37 C38 1.518(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.504(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.519(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.517(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C48 1.380(6) . ? C43 C44 1.384(6) . ? C43 C50 1.523(6) . ? C44 C45 1.398(6) . ? C44 H44 0.9300 . ? C45 C46 1.369(7) . ? C45 H45 0.9300 . ? C46 C47 1.385(7) . ? C46 C49 1.505(6) . ? C47 C48 1.395(7) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 N2 1.483(6) 2_776 ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 N3 1.458(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.337(8) . ? C51 N1 1.368(6) . ? C51 H51 0.9300 . ? C52 N2 1.368(7) . ? C52 H52 0.9300 . ? C53 N1 1.317(6) . ? C53 N2 1.331(6) . ? C53 H53 0.9300 . ? C54 C55 1.348(6) . ? C54 N4 1.385(5) . ? C54 H54 0.9300 . ? C55 N3 1.382(6) . ? C55 H55 0.9300 . ? C56 N4 1.330(5) . ? C56 N3 1.339(5) . ? C56 H56 0.9300 . ? C57 C58 1.364(8) . ? C57 C62 1.395(8) . ? C57 C63 1.523(7) . ? C58 C59 1.395(7) . ? C58 H58 0.9300 . ? C59 C60 1.371(7) . ? C59 H59 0.9300 . ? C60 C61 1.369(7) . ? C60 C64 1.514(6) . ? C61 C62 1.398(7) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 N7 1.474(6) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 N6 1.479(6) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 N6 1.364(6) . ? C65 C66 1.366(7) . ? C65 H65 0.9300 . ? C66 N5 1.385(6) . ? C66 H66 0.9300 . ? C67 N5 1.327(5) . ? C67 N6 1.336(6) . ? C67 H67 0.9300 . ? C68 C69 1.343(8) . ? C68 N8 1.374(6) . ? C68 H68 0.9300 . ? C69 N7 1.362(8) . ? C69 H69 0.9300 . ? C70 N8 1.313(6) . ? C70 N7 1.321(6) . ? C70 H70 0.9300 . ? N1 Zn1 2.013(3) . ? N2 C49 1.483(6) 2_776 ? N4 Zn1 1.999(3) . ? N5 Zn2 2.001(4) . ? N8 Zn2 2.024(4) 2_495 ? O2 Zn1 1.964(3) . ? O4 Zn2 2.040(5) . ? O6 Zn2 1.984(3) . ? O8 Zn1 2.001(3) 1_475 ? Zn1 O8 2.001(3) 1_635 ? Zn2 N8 2.024(4) 2_495 ? 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 C10 C1 C2 118.6(6) . . ? C10 C1 H1 120.7 . . ? C2 C1 H1 120.7 . . ? C3 C2 C1 120.1(5) . . ? C3 C2 C14 122.2(9) . . ? C1 C2 C14 117.7(9) . . ? C2 C3 C4 122.3(8) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C11 C4 C3 118.0(7) . . ? C11 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C6 C5 C12 118.9(5) . . ? C6 C5 H5 120.5 . . ? C12 C5 H5 120.5 . . ? C5 C6 C7 120.6(4) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 120.3(4) . . ? C8 C7 C15 119.4(4) . . ? C6 C7 C15 120.3(4) . . ? C13 C8 C7 119.4(4) . . ? C13 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C13 101.5(4) . . ? C10 C9 C19 111.1(4) . . ? C13 C9 C19 110.6(4) . . ? C10 C9 C16 108.2(4) . . ? C13 C9 C16 112.4(4) . . ? C19 C9 C16 112.5(5) . . ? C11 C10 C1 119.3(6) . . ? C11 C10 C9 112.0(4) . . ? C1 C10 C9 128.7(6) . . ? C4 C11 C10 121.7(5) . . ? C4 C11 C12 130.7(6) . . ? C10 C11 C12 107.6(5) . . ? C5 C12 C13 120.8(4) . . ? C5 C12 C11 129.9(5) . . ? C13 C12 C11 109.3(4) . . ? C8 C13 C12 119.9(4) . . ? C8 C13 C9 130.6(5) . . ? C12 C13 C9 109.4(4) . . ? O4 C14 O3 121.7(7) . . ? O4 C14 C2 125.7(12) . . ? O3 C14 C2 112.6(11) . . ? O1 C15 O2 123.2(4) . . ? O1 C15 C7 119.9(4) . . ? O2 C15 C7 116.8(4) . . ? C17 C16 C9 117.7(5) . . ? C17 C16 H16A 107.9 . . ? C9 C16 H16A 107.9 . . ? C17 C16 H16B 107.9 . . ? C9 C16 H16B 107.9 . . ? H16A C16 H16B 107.2 . . ? C16 C17 C18 110.7(6) . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C9 115.1(5) . . ? C20 C19 H19A 108.5 . . ? C9 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? C9 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C21 C20 C19 113.8(6) . . ? C21 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C31 C22 C23 119.1(4) . . ? C31 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 119.6(4) . . ? C24 C23 C35 121.4(4) . . ? C22 C23 C35 119.0(4) . . ? C25 C24 C23 121.4(4) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C32 118.3(4) . . ? C24 C25 H25 120.8 . . ? C32 C25 H25 120.8 . . ? C27 C26 C33 118.8(4) . . ? C27 C26 H26 120.6 . . ? C33 C26 H26 120.6 . . ? C26 C27 C28 121.3(4) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C27 C28 C29 119.6(4) . . ? C27 C28 C36 121.8(4) . . ? C29 C28 C36 118.5(4) . . ? C34 C29 C28 119.3(4) . . ? C34 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C34 C30 C31 100.2(3) . . ? C34 C30 C40 111.4(4) . . ? C31 C30 C40 112.2(4) . . ? C34 C30 C37 112.0(4) . . ? C31 C30 C37 111.4(4) . . ? C40 C30 C37 109.3(4) . . ? C22 C31 C32 120.7(4) . . ? C22 C31 C30 127.6(4) . . ? C32 C31 C30 111.6(4) . . ? C31 C32 C25 120.7(4) . . ? C31 C32 C33 108.2(4) . . ? C25 C32 C33 131.1(4) . . ? C34 C33 C26 120.5(4) . . ? C34 C33 C32 108.2(4) . . ? C26 C33 C32 131.3(4) . . ? C29 C34 C33 120.4(4) . . ? C29 C34 C30 127.9(4) . . ? C33 C34 C30 111.7(4) . . ? O5 C35 O6 123.5(4) . . ? O5 C35 C23 119.6(4) . . ? O6 C35 C23 116.9(4) . . ? O7 C36 O8 122.2(4) . . ? O7 C36 C28 120.4(4) . . ? O8 C36 C28 117.4(4) . . ? C38 C37 C30 116.6(4) . . ? C38 C37 H37A 108.1 . . ? C30 C37 H37A 108.1 . . ? C38 C37 H37B 108.1 . . ? C30 C37 H37B 108.1 . . ? H37A C37 H37B 107.3 . . ? C39 C38 C37 113.7(6) . . ? C39 C38 H38A 108.8 . . ? C37 C38 H38A 108.8 . . ? C39 C38 H38B 108.8 . . ? C37 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C30 116.2(4) . . ? C41 C40 H40A 108.2 . . ? C30 C40 H40A 108.2 . . ? C41 C40 H40B 108.2 . . ? C30 C40 H40B 108.2 . . ? H40A C40 H40B 107.4 . . ? C42 C41 C40 112.0(6) . . ? C42 C41 H41A 109.2 . . ? C40 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? C40 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 118.7(4) . . ? C48 C43 C50 123.0(4) . . ? C44 C43 C50 118.3(4) . . ? C43 C44 C45 120.5(4) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 121.2(4) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C45 C46 C47 118.0(4) . . ? C45 C46 C49 121.6(4) . . ? C47 C46 C49 120.3(4) . . ? C46 C47 C48 121.4(4) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C43 C48 C47 120.1(4) . . ? C43 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? N2 C49 C46 111.1(4) 2_776 . ? N2 C49 H49A 109.4 2_776 . ? C46 C49 H49A 109.4 . . ? N2 C49 H49B 109.4 2_776 . ? C46 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? N3 C50 C43 112.7(3) . . ? N3 C50 H50A 109.0 . . ? C43 C50 H50A 109.0 . . ? N3 C50 H50B 109.0 . . ? C43 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? C52 C51 N1 109.7(5) . . ? C52 C51 H51 125.1 . . ? N1 C51 H51 125.1 . . ? C51 C52 N2 106.4(4) . . ? C51 C52 H52 126.8 . . ? N2 C52 H52 126.8 . . ? N1 C53 N2 111.2(4) . . ? N1 C53 H53 124.4 . . ? N2 C53 H53 124.4 . . ? C55 C54 N4 109.5(4) . . ? C55 C54 H54 125.2 . . ? N4 C54 H54 125.2 . . ? C54 C55 N3 106.5(4) . . ? C54 C55 H55 126.7 . . ? N3 C55 H55 126.7 . . ? N4 C56 N3 111.4(4) . . ? N4 C56 H56 124.3 . . ? N3 C56 H56 124.3 . . ? C58 C57 C62 119.8(5) . . ? C58 C57 C63 120.6(5) . . ? C62 C57 C63 119.6(5) . . ? C57 C58 C59 119.5(5) . . ? C57 C58 H58 120.2 . . ? C59 C58 H58 120.2 . . ? C60 C59 C58 121.7(5) . . ? C60 C59 H59 119.1 . . ? C58 C59 H59 119.1 . . ? C61 C60 C59 118.5(4) . . ? C61 C60 C64 121.0(4) . . ? C59 C60 C64 120.4(4) . . ? C60 C61 C62 121.1(5) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C57 C62 C61 119.3(5) . . ? C57 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? N7 C63 C57 111.2(4) . . ? N7 C63 H63A 109.4 . . ? C57 C63 H63A 109.4 . . ? N7 C63 H63B 109.4 . . ? C57 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? N6 C64 C60 111.8(4) . . ? N6 C64 H64A 109.3 . . ? C60 C64 H64A 109.3 . . ? N6 C64 H64B 109.3 . . ? C60 C64 H64B 109.3 . . ? H64A C64 H64B 107.9 . . ? N6 C65 C66 106.8(4) . . ? N6 C65 H65 126.6 . . ? C66 C65 H65 126.6 . . ? C65 C66 N5 108.2(4) . . ? C65 C66 H66 125.9 . . ? N5 C66 H66 125.9 . . ? N5 C67 N6 110.9(4) . . ? N5 C67 H67 124.6 . . ? N6 C67 H67 124.6 . . ? C69 C68 N8 109.8(5) . . ? C69 C68 H68 125.1 . . ? N8 C68 H68 125.1 . . ? C68 C69 N7 106.3(5) . . ? C68 C69 H69 126.8 . . ? N7 C69 H69 126.8 . . ? N8 C70 N7 112.5(5) . . ? N8 C70 H70 123.8 . . ? N7 C70 H70 123.8 . . ? C53 N1 C51 105.5(4) . . ? C53 N1 Zn1 124.4(3) . . ? C51 N1 Zn1 130.0(3) . . ? C53 N2 C52 107.2(4) . . ? C53 N2 C49 125.4(4) . 2_776 ? C52 N2 C49 127.4(4) . 2_776 ? C56 N3 C55 107.1(4) . . ? C56 N3 C50 126.1(4) . . ? C55 N3 C50 126.6(4) . . ? C56 N4 C54 105.4(3) . . ? C56 N4 Zn1 125.4(3) . . ? C54 N4 Zn1 129.2(3) . . ? C67 N5 C66 106.3(4) . . ? C67 N5 Zn2 127.3(3) . . ? C66 N5 Zn2 126.5(3) . . ? C67 N6 C65 107.9(4) . . ? C67 N6 C64 125.3(4) . . ? C65 N6 C64 126.7(4) . . ? C70 N7 C69 107.0(4) . . ? C70 N7 C63 126.3(5) . . ? C69 N7 C63 126.7(5) . . ? C70 N8 C68 104.5(4) . . ? C70 N8 Zn2 128.3(3) . 2_495 ? C68 N8 Zn2 127.2(3) . 2_495 ? C15 O2 Zn1 110.4(3) . . ? C14 O4 Zn2 107.6(8) . . ? C35 O6 Zn2 111.7(3) . . ? C36 O8 Zn1 107.9(3) . 1_475 ? O2 Zn1 N4 120.49(13) . . ? O2 Zn1 O8 112.61(12) . 1_635 ? N4 Zn1 O8 109.38(13) . 1_635 ? O2 Zn1 N1 107.60(13) . . ? N4 Zn1 N1 109.23(14) . . ? O8 Zn1 N1 94.27(13) 1_635 . ? O6 Zn2 N5 124.46(14) . . ? O6 Zn2 N8 98.40(15) . 2_495 ? N5 Zn2 N8 110.94(15) . 2_495 ? O6 Zn2 O4 95.3(2) . . ? N5 Zn2 O4 106.15(16) . . ? N8 Zn2 O4 122.1(3) 2_495 . ? 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 C10 C1 C2 C3 -2.5(9) . . . . ? C10 C1 C2 C14 178.8(5) . . . . ? C1 C2 C3 C4 0.8(11) . . . . ? C14 C2 C3 C4 179.3(7) . . . . ? C2 C3 C4 C11 0.0(11) . . . . ? C12 C5 C6 C7 -1.1(8) . . . . ? C5 C6 C7 C8 2.1(7) . . . . ? C5 C6 C7 C15 -177.6(4) . . . . ? C6 C7 C8 C13 -1.9(6) . . . . ? C15 C7 C8 C13 177.8(4) . . . . ? C2 C1 C10 C11 3.5(7) . . . . ? C2 C1 C10 C9 -176.2(5) . . . . ? C13 C9 C10 C11 3.7(5) . . . . ? C19 C9 C10 C11 -114.0(5) . . . . ? C16 C9 C10 C11 122.1(5) . . . . ? C13 C9 C10 C1 -176.7(5) . . . . ? C19 C9 C10 C1 65.7(6) . . . . ? C16 C9 C10 C1 -58.2(6) . . . . ? C3 C4 C11 C10 1.0(10) . . . . ? C3 C4 C11 C12 -179.7(6) . . . . ? C1 C10 C11 C4 -2.8(8) . . . . ? C9 C10 C11 C4 176.9(5) . . . . ? C1 C10 C11 C12 177.8(4) . . . . ? C9 C10 C11 C12 -2.5(6) . . . . ? C6 C5 C12 C13 0.0(8) . . . . ? C6 C5 C12 C11 -179.5(5) . . . . ? C4 C11 C12 C5 0.3(10) . . . . ? C10 C11 C12 C5 179.7(5) . . . . ? C4 C11 C12 C13 -179.3(6) . . . . ? C10 C11 C12 C13 0.1(6) . . . . ? C7 C8 C13 C12 0.8(6) . . . . ? C7 C8 C13 C9 177.7(4) . . . . ? C5 C12 C13 C8 0.1(7) . . . . ? C11 C12 C13 C8 179.8(4) . . . . ? C5 C12 C13 C9 -177.4(5) . . . . ? C11 C12 C13 C9 2.3(5) . . . . ? C10 C9 C13 C8 179.4(4) . . . . ? C19 C9 C13 C8 -62.6(6) . . . . ? C16 C9 C13 C8 64.0(7) . . . . ? C10 C9 C13 C12 -3.5(5) . . . . ? C19 C9 C13 C12 114.5(5) . . . . ? C16 C9 C13 C12 -118.9(5) . . . . ? C3 C2 C14 O4 -154.1(8) . . . . ? C1 C2 C14 O4 24.5(10) . . . . ? C3 C2 C14 O3 25.7(9) . . . . ? C1 C2 C14 O3 -155.7(6) . . . . ? C8 C7 C15 O1 -21.9(6) . . . . ? C6 C7 C15 O1 157.8(4) . . . . ? C8 C7 C15 O2 158.3(4) . . . . ? C6 C7 C15 O2 -22.1(6) . . . . ? C10 C9 C16 C17 -177.9(5) . . . . ? C13 C9 C16 C17 -66.7(7) . . . . ? C19 C9 C16 C17 58.9(7) . . . . ? C9 C16 C17 C18 -178.3(6) . . . . ? C10 C9 C19 C20 57.6(6) . . . . ? C13 C9 C19 C20 -54.3(6) . . . . ? C16 C9 C19 C20 179.1(5) . . . . ? C9 C19 C20 C21 -175.1(5) . . . . ? C31 C22 C23 C24 -0.4(7) . . . . ? C31 C22 C23 C35 -178.1(4) . . . . ? C22 C23 C24 C25 -1.1(8) . . . . ? C35 C23 C24 C25 176.5(5) . . . . ? C23 C24 C25 C32 0.7(8) . . . . ? C33 C26 C27 C28 -1.4(7) . . . . ? C26 C27 C28 C29 -1.8(7) . . . . ? C26 C27 C28 C36 179.4(4) . . . . ? C27 C28 C29 C34 2.9(7) . . . . ? C36 C28 C29 C34 -178.2(4) . . . . ? C23 C22 C31 C32 2.2(7) . . . . ? C23 C22 C31 C30 179.1(5) . . . . ? C34 C30 C31 C22 -178.0(5) . . . . ? C40 C30 C31 C22 63.6(7) . . . . ? C37 C30 C31 C22 -59.4(7) . . . . ? C34 C30 C31 C32 -1.0(6) . . . . ? C40 C30 C31 C32 -119.3(5) . . . . ? C37 C30 C31 C32 117.7(5) . . . . ? C22 C31 C32 C25 -2.7(8) . . . . ? C30 C31 C32 C25 -180.0(5) . . . . ? C22 C31 C32 C33 177.8(5) . . . . ? C30 C31 C32 C33 0.5(6) . . . . ? C24 C25 C32 C31 1.2(8) . . . . ? C24 C25 C32 C33 -179.4(5) . . . . ? C27 C26 C33 C34 3.4(8) . . . . ? C27 C26 C33 C32 -177.4(5) . . . . ? C31 C32 C33 C34 0.3(5) . . . . ? C25 C32 C33 C34 -179.2(5) . . . . ? C31 C32 C33 C26 -179.0(5) . . . . ? C25 C32 C33 C26 1.6(9) . . . . ? C28 C29 C34 C33 -0.8(7) . . . . ? C28 C29 C34 C30 178.3(5) . . . . ? C26 C33 C34 C29 -2.3(7) . . . . ? C32 C33 C34 C29 178.3(4) . . . . ? C26 C33 C34 C30 178.4(5) . . . . ? C32 C33 C34 C30 -1.0(6) . . . . ? C31 C30 C34 C29 -178.0(5) . . . . ? C40 C30 C34 C29 -59.1(6) . . . . ? C37 C30 C34 C29 63.7(7) . . . . ? C31 C30 C34 C33 1.2(5) . . . . ? C40 C30 C34 C33 120.1(4) . . . . ? C37 C30 C34 C33 -117.1(5) . . . . ? C24 C23 C35 O5 -150.3(5) . . . . ? C22 C23 C35 O5 27.4(7) . . . . ? C24 C23 C35 O6 27.3(6) . . . . ? C22 C23 C35 O6 -155.1(4) . . . . ? C27 C28 C36 O7 173.9(4) . . . . ? C29 C28 C36 O7 -4.9(6) . . . . ? C27 C28 C36 O8 -6.2(6) . . . . ? C29 C28 C36 O8 174.9(4) . . . . ? C34 C30 C37 C38 61.4(6) . . . . ? C31 C30 C37 C38 -49.9(6) . . . . ? C40 C30 C37 C38 -174.6(4) . . . . ? C30 C37 C38 C39 -175.1(5) . . . . ? C34 C30 C40 C41 -52.4(6) . . . . ? C31 C30 C40 C41 59.2(6) . . . . ? C37 C30 C40 C41 -176.7(4) . . . . ? C30 C40 C41 C42 179.4(5) . . . . ? C48 C43 C44 C45 -1.0(7) . . . . ? C50 C43 C44 C45 -179.1(4) . . . . ? C43 C44 C45 C46 0.0(8) . . . . ? C44 C45 C46 C47 1.1(8) . . . . ? C44 C45 C46 C49 178.5(5) . . . . ? C45 C46 C47 C48 -1.1(9) . . . . ? C49 C46 C47 C48 -178.6(5) . . . . ? C44 C43 C48 C47 1.0(8) . . . . ? C50 C43 C48 C47 179.0(5) . . . . ? C46 C47 C48 C43 0.1(10) . . . . ? C45 C46 C49 N2 117.1(5) . . . 2_776 ? C47 C46 C49 N2 -65.5(7) . . . 2_776 ? C48 C43 C50 N3 5.9(6) . . . . ? C44 C43 C50 N3 -176.0(4) . . . . ? N1 C51 C52 N2 0.8(8) . . . . ? N4 C54 C55 N3 0.2(5) . . . . ? C62 C57 C58 C59 -0.6(8) . . . . ? C63 C57 C58 C59 -178.9(5) . . . . ? C57 C58 C59 C60 -0.2(8) . . . . ? C58 C59 C60 C61 0.9(8) . . . . ? C58 C59 C60 C64 178.5(5) . . . . ? C59 C60 C61 C62 -0.7(8) . . . . ? C64 C60 C61 C62 -178.3(5) . . . . ? C58 C57 C62 C61 0.7(8) . . . . ? C63 C57 C62 C61 179.0(5) . . . . ? C60 C61 C62 C57 -0.1(9) . . . . ? C58 C57 C63 N7 -95.0(6) . . . . ? C62 C57 C63 N7 86.7(7) . . . . ? C61 C60 C64 N6 -70.1(6) . . . . ? C59 C60 C64 N6 112.3(5) . . . . ? N6 C65 C66 N5 -0.6(6) . . . . ? N8 C68 C69 N7 0.1(7) . . . . ? N2 C53 N1 C51 -0.2(5) . . . . ? N2 C53 N1 Zn1 178.8(3) . . . . ? C52 C51 N1 C53 -0.4(7) . . . . ? C52 C51 N1 Zn1 -179.3(4) . . . . ? N1 C53 N2 C52 0.7(6) . . . . ? N1 C53 N2 C49 -177.6(4) . . . 2_776 ? C51 C52 N2 C53 -0.9(7) . . . . ? C51 C52 N2 C49 177.3(5) . . . 2_776 ? N4 C56 N3 C55 -0.5(5) . . . . ? N4 C56 N3 C50 -176.2(4) . . . . ? C54 C55 N3 C56 0.1(5) . . . . ? C54 C55 N3 C50 175.8(4) . . . . ? C43 C50 N3 C56 94.5(5) . . . . ? C43 C50 N3 C55 -80.4(5) . . . . ? N3 C56 N4 C54 0.6(4) . . . . ? N3 C56 N4 Zn1 -178.3(3) . . . . ? C55 C54 N4 C56 -0.5(5) . . . . ? C55 C54 N4 Zn1 178.3(3) . . . . ? N6 C67 N5 C66 -0.7(5) . . . . ? N6 C67 N5 Zn2 178.5(3) . . . . ? C65 C66 N5 C67 0.8(5) . . . . ? C65 C66 N5 Zn2 -178.5(3) . . . . ? N5 C67 N6 C65 0.4(5) . . . . ? N5 C67 N6 C64 175.7(4) . . . . ? C66 C65 N6 C67 0.2(6) . . . . ? C66 C65 N6 C64 -175.0(4) . . . . ? C60 C64 N6 C67 130.3(5) . . . . ? C60 C64 N6 C65 -55.3(7) . . . . ? N8 C70 N7 C69 -0.7(6) . . . . ? N8 C70 N7 C63 179.4(4) . . . . ? C68 C69 N7 C70 0.3(7) . . . . ? C68 C69 N7 C63 -179.7(5) . . . . ? C57 C63 N7 C70 -103.1(6) . . . . ? C57 C63 N7 C69 77.0(7) . . . . ? N7 C70 N8 C68 0.7(6) . . . . ? N7 C70 N8 Zn2 179.8(3) . . . 2_495 ? C69 C68 N8 C70 -0.5(6) . . . . ? C69 C68 N8 Zn2 -179.6(4) . . . 2_495 ? O1 C15 O2 Zn1 -5.5(5) . . . . ? C7 C15 O2 Zn1 174.3(3) . . . . ? O3 C14 O4 Zn2 -1.8(8) . . . . ? C2 C14 O4 Zn2 178.0(5) . . . . ? O5 C35 O6 Zn2 3.2(6) . . . . ? C23 C35 O6 Zn2 -174.2(3) . . . . ? O7 C36 O8 Zn1 -5.0(5) . . . 1_475 ? C28 C36 O8 Zn1 175.1(3) . . . 1_475 ? C15 O2 Zn1 N4 53.2(3) . . . . ? C15 O2 Zn1 O8 -175.3(2) . . . 1_635 ? C15 O2 Zn1 N1 -72.8(3) . . . . ? C56 N4 Zn1 O2 132.3(3) . . . . ? C54 N4 Zn1 O2 -46.3(4) . . . . ? C56 N4 Zn1 O8 -0.6(4) . . . 1_635 ? C54 N4 Zn1 O8 -179.1(3) . . . 1_635 ? C56 N4 Zn1 N1 -102.5(3) . . . . ? C54 N4 Zn1 N1 79.0(4) . . . . ? C53 N1 Zn1 O2 -97.1(3) . . . . ? C51 N1 Zn1 O2 81.6(5) . . . . ? C53 N1 Zn1 N4 130.5(3) . . . . ? C51 N1 Zn1 N4 -50.8(5) . . . . ? C53 N1 Zn1 O8 18.2(4) . . . 1_635 ? C51 N1 Zn1 O8 -163.0(5) . . . 1_635 ? C35 O6 Zn2 N5 -37.0(3) . . . . ? C35 O6 Zn2 N8 85.7(3) . . . 2_495 ? C35 O6 Zn2 O4 -150.7(4) . . . . ? C67 N5 Zn2 O6 -0.6(4) . . . . ? C66 N5 Zn2 O6 178.6(3) . . . . ? C67 N5 Zn2 N8 -117.4(4) . . . 2_495 ? C66 N5 Zn2 N8 61.7(4) . . . 2_495 ? C67 N5 Zn2 O4 107.9(4) . . . . ? C66 N5 Zn2 O4 -73.0(5) . . . . ? C14 O4 Zn2 O6 -155.2(5) . . . . ? C14 O4 Zn2 N5 76.6(6) . . . . ? C14 O4 Zn2 N8 -51.8(5) . . . 2_495 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.447 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.135 #====END data_compound4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C70 H68 Cd2 N8 O8' _chemical_formula_sum 'C70 H68 Cd2 N8 O8' _chemical_formula_weight 1374.12 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 _symmetry_space_group_name_Hall p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8420(19) _cell_length_b 13.928(2) _cell_length_c 22.838(3) _cell_angle_alpha 87.372(3) _cell_angle_beta 87.465(3) _cell_angle_gamma 72.708(3) _cell_volume 4197.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15907 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8082 _exptl_absorpt_correction_T_max 0.8950 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23027 _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_sigmaI/netI 0.2830 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.07 _reflns_number_total 15907 _reflns_number_gt 6151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1210P)^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 15907 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2542 _refine_ls_R_factor_gt 0.1071 _refine_ls_wR_factor_ref 0.2990 _refine_ls_wR_factor_gt 0.2196 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _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 C1 C 0.7002(10) 1.1591(10) 0.2996(6) 0.040(3) Uani 1 1 d . . . H1 H 0.7217 1.0946 0.3166 0.048 Uiso 1 1 calc R . . C2 C 0.7635(10) 1.2208(9) 0.2997(6) 0.039(3) Uani 1 1 d . . . C3 C 0.7323(11) 1.3140(9) 0.2736(6) 0.051(4) Uani 1 1 d . . . H3 H 0.7743 1.3552 0.2726 0.061 Uiso 1 1 calc R . . C4 C 0.6381(10) 1.3485(11) 0.2483(7) 0.060(4) Uani 1 1 d . . . H4 H 0.6186 1.4123 0.2304 0.072 Uiso 1 1 calc R . . C5 C 0.4093(11) 1.3885(11) 0.2003(7) 0.057(4) Uani 1 1 d . . . H5 H 0.4310 1.4445 0.1906 0.069 Uiso 1 1 calc R . . C6 C 0.3134(10) 1.3877(11) 0.1849(7) 0.052(4) Uani 1 1 d . . . H6 H 0.2702 1.4430 0.1654 0.062 Uiso 1 1 calc R . . C7 C 0.2830(9) 1.3003(10) 0.1995(6) 0.043(4) Uani 1 1 d . . . C8 C 0.3483(11) 1.2188(10) 0.2284(7) 0.052(4) Uani 1 1 d . . . H8 H 0.3284 1.1615 0.2373 0.062 Uiso 1 1 calc R . . C9 C 0.5253(10) 1.1377(9) 0.2716(6) 0.042(3) Uani 1 1 d . . . C10 C 0.6083(10) 1.1915(9) 0.2754(6) 0.043(4) Uani 1 1 d . . . C11 C 0.5708(11) 1.2886(9) 0.2491(7) 0.050(4) Uani 1 1 d . . . C12 C 0.4708(10) 1.3085(10) 0.2291(7) 0.048(4) Uani 1 1 d . . . C13 C 0.4425(10) 1.2214(10) 0.2441(6) 0.039(3) Uani 1 1 d . . . C14 C 0.8643(10) 1.1846(10) 0.3269(6) 0.038(3) Uani 1 1 d . . . C15 C 0.1784(12) 1.3033(12) 0.1820(6) 0.044(4) Uani 1 1 d . . . C16 C 0.5617(11) 1.0444(10) 0.2331(8) 0.059(4) Uani 1 1 d . . . H16A H 0.6230 0.9996 0.2493 0.071 Uiso 1 1 calc R . . H16B H 0.5107 1.0092 0.2359 0.071 Uiso 1 1 calc R . . C17 C 0.5823(11) 1.0641(11) 0.1701(8) 0.059(4) Uani 1 1 d . . . H17A H 0.6292 1.1040 0.1666 0.071 Uiso 1 1 calc R . . H17B H 0.5198 1.1029 0.1522 0.071 Uiso 1 1 calc R . . C18 C 0.6266(14) 0.9678(15) 0.1375(11) 0.118(8) Uani 1 1 d . . . H18A H 0.6394 0.9838 0.0971 0.177 Uiso 1 1 calc R . . H18B H 0.5796 0.9290 0.1399 0.177 Uiso 1 1 calc R . . H18C H 0.6889 0.9296 0.1548 0.177 Uiso 1 1 calc R . . C19 C 0.4928(11) 1.1071(12) 0.3316(7) 0.059(4) Uani 1 1 d . . . H19A H 0.4335 1.0848 0.3272 0.071 Uiso 1 1 calc R . . H19B H 0.5462 1.0493 0.3456 0.071 Uiso 1 1 calc R . . C20 C 0.4684(12) 1.1828(13) 0.3779(7) 0.071(5) Uani 1 1 d . . . H20A H 0.4147 1.2410 0.3647 0.085 Uiso 1 1 calc R . . H20B H 0.5276 1.2045 0.3837 0.085 Uiso 1 1 calc R . . C21 C 0.4346(15) 1.1421(19) 0.4378(9) 0.123(9) Uani 1 1 d . . . H21A H 0.4207 1.1938 0.4661 0.184 Uiso 1 1 calc R . . H21B H 0.4876 1.0848 0.4514 0.184 Uiso 1 1 calc R . . H21C H 0.3745 1.1226 0.4327 0.184 Uiso 1 1 calc R . . C22 C -0.3078(9) 1.5974(9) 0.2335(6) 0.038(3) Uani 1 1 d . . . H22 H -0.2677 1.5674 0.2648 0.046 Uiso 1 1 calc R . . C23 C -0.2804(10) 1.5645(10) 0.1773(6) 0.043(3) Uani 1 1 d . . . C24 C -0.3412(12) 1.6130(13) 0.1285(7) 0.081(6) Uani 1 1 d . . . H24 H -0.3242 1.5903 0.0906 0.097 Uiso 1 1 calc R . . C25 C -0.4242(14) 1.6930(12) 0.1393(7) 0.082(6) Uani 1 1 d . . . H25 H -0.4615 1.7287 0.1082 0.098 Uiso 1 1 calc R . . C26 C -0.6210(13) 1.8679(10) 0.1892(7) 0.069(5) Uani 1 1 d . . . H26 H -0.6242 1.8666 0.1487 0.083 Uiso 1 1 calc R . . C27 C -0.6955(11) 1.9364(10) 0.2219(6) 0.052(4) Uani 1 1 d . . . H27 H -0.7495 1.9813 0.2029 0.062 Uiso 1 1 calc R . . C28 C -0.6907(9) 1.9388(9) 0.2820(6) 0.035(3) Uani 1 1 d . . . C29 C -0.6093(10) 1.8725(9) 0.3105(6) 0.038(3) Uani 1 1 d . . . H29 H -0.6042 1.8752 0.3508 0.045 Uiso 1 1 calc R . . C30 C -0.4434(9) 1.7212(9) 0.2999(6) 0.038(3) Uani 1 1 d . . . C31 C -0.3951(10) 1.6749(10) 0.2425(6) 0.042(3) Uani 1 1 d . . . C32 C -0.4534(11) 1.7215(11) 0.1962(7) 0.050(4) Uani 1 1 d . . . C33 C -0.5417(10) 1.8018(10) 0.2192(6) 0.049(4) Uani 1 1 d . . . C34 C -0.5354(9) 1.8018(9) 0.2785(6) 0.037(3) Uani 1 1 d . . . C35 C -0.1886(12) 1.4795(11) 0.1636(7) 0.052(4) Uani 1 1 d . . . C36 C -0.7715(10) 2.0122(9) 0.3169(6) 0.033(3) Uani 1 1 d . . . C37 C -0.3644(12) 1.7667(12) 0.3290(7) 0.074(5) Uani 1 1 d . . . H37A H -0.3036 1.7116 0.3361 0.088 Uiso 1 1 calc R . . H37B H -0.3463 1.8121 0.3001 0.088 Uiso 1 1 calc R . . C38 C -0.3940(13) 1.8222(13) 0.3850(8) 0.079(5) Uani 1 1 d . . . H38A H -0.4058 1.7773 0.4164 0.095 Uiso 1 1 calc R . . H38B H -0.4556 1.8774 0.3801 0.095 Uiso 1 1 calc R . . C39 C -0.3043(14) 1.8636(16) 0.4001(10) 0.121(9) Uani 1 1 d . . . H39A H -0.3207 1.8994 0.4359 0.181 Uiso 1 1 calc R . . H39B H -0.2935 1.9081 0.3689 0.181 Uiso 1 1 calc R . . H39C H -0.2438 1.8084 0.4049 0.181 Uiso 1 1 calc R . . C40 C -0.4702(11) 1.6453(11) 0.3399(6) 0.052(4) Uani 1 1 d . . . H40A H -0.5024 1.6776 0.3754 0.063 Uiso 1 1 calc R . . H40B H -0.4087 1.5937 0.3507 0.063 Uiso 1 1 calc R . . C41 C -0.5405(14) 1.5967(13) 0.3125(10) 0.104(8) Uani 1 1 d . . . H41A H -0.5093 1.5666 0.2762 0.125 Uiso 1 1 calc R . . H41B H -0.6028 1.6482 0.3028 0.125 Uiso 1 1 calc R . . C42 C -0.5666(19) 1.5128(19) 0.3542(14) 0.175(13) Uani 1 1 d . . . H42A H -0.6106 1.4837 0.3346 0.263 Uiso 1 1 calc R . . H42B H -0.5998 1.5426 0.3896 0.263 Uiso 1 1 calc R . . H42C H -0.5053 1.4613 0.3637 0.263 Uiso 1 1 calc R . . C43 C 0.0222(11) 1.1367(9) -0.2022(6) 0.041(3) Uani 1 1 d . . . C44 C -0.0654(13) 1.1693(11) -0.1669(8) 0.073(5) Uani 1 1 d . . . H44 H -0.1134 1.1346 -0.1643 0.088 Uiso 1 1 calc R . . C45 C -0.0782(14) 1.2573(13) -0.1352(7) 0.072(5) Uani 1 1 d . . . H45 H -0.1357 1.2807 -0.1112 0.086 Uiso 1 1 calc R . . C46 C -0.0059(15) 1.3101(10) -0.1390(6) 0.059(5) Uani 1 1 d . . . C47 C 0.0728(13) 1.2784(11) -0.1752(7) 0.060(4) Uani 1 1 d . . . H47 H 0.1199 1.3142 -0.1794 0.072 Uiso 1 1 calc R . . C48 C 0.0872(11) 1.1917(10) -0.2075(6) 0.046(4) Uani 1 1 d . . . H48 H 0.1430 1.1718 -0.2331 0.055 Uiso 1 1 calc R . . C49 C 0.0393(11) 1.0448(10) -0.2371(6) 0.050(4) Uani 1 1 d . . . H49A H -0.0213 1.0502 -0.2584 0.061 Uiso 1 1 calc R . . H49B H 0.0939 1.0418 -0.2657 0.061 Uiso 1 1 calc R . . C50 C -0.023(2) 1.4037(11) -0.1042(7) 0.114(9) Uani 1 1 d . . . H50A H 0.0066 1.4504 -0.1257 0.137 Uiso 1 1 calc R . . H50B H -0.0949 1.4361 -0.0989 0.137 Uiso 1 1 calc R . . C51 C 0.1466(14) 0.9168(12) -0.1672(8) 0.073(5) Uani 1 1 d . . . H51 H 0.1963 0.9482 -0.1629 0.088 Uiso 1 1 calc R . . C52 C 0.1439(12) 0.8321(12) -0.1416(8) 0.073(6) Uani 1 1 d . . . H52 H 0.1899 0.7945 -0.1146 0.087 Uiso 1 1 calc R . . C53 C 0.0139(11) 0.8832(9) -0.1970(6) 0.040(3) Uani 1 1 d . . . H53 H -0.0456 0.8882 -0.2160 0.048 Uiso 1 1 calc R . . C54 C 0.1173(17) 1.369(2) -0.0309(9) 0.129(11) Uani 1 1 d . . . H54 H 0.1700 1.3744 -0.0562 0.155 Uiso 1 1 calc R . . C55 C 0.1240(16) 1.3487(18) 0.0266(8) 0.100(7) Uani 1 1 d . . . H55 H 0.1814 1.3404 0.0483 0.119 Uiso 1 1 calc R . . C56 C -0.0303(15) 1.3620(13) 0.0042(8) 0.076(5) Uani 1 1 d . . . H56 H -0.0981 1.3640 0.0067 0.092 Uiso 1 1 calc R . . C57 C 1.0735(11) 1.6276(9) 0.3044(6) 0.046(4) Uani 1 1 d . . . C58 C 0.9952(11) 1.6625(10) 0.3452(6) 0.051(4) Uani 1 1 d . . . H58 H 0.9442 1.6317 0.3503 0.061 Uiso 1 1 calc R . . C59 C 0.9937(11) 1.7440(9) 0.3784(6) 0.051(4) Uani 1 1 d . . . H59 H 0.9441 1.7642 0.4078 0.061 Uiso 1 1 calc R . . C60 C 1.0651(10) 1.7962(9) 0.3686(6) 0.036(3) Uani 1 1 d . . . C61 C 1.1436(11) 1.7574(10) 0.3272(6) 0.048(4) Uani 1 1 d . . . H61 H 1.1946 1.7881 0.3214 0.058 Uiso 1 1 calc R . . C62 C 1.1471(11) 1.6760(9) 0.2954(6) 0.047(4) Uani 1 1 d . . . H62 H 1.1990 1.6530 0.2676 0.057 Uiso 1 1 calc R . . C63 C 1.0791(12) 1.5358(9) 0.2703(7) 0.058(4) Uani 1 1 d . . . H63A H 1.0139 1.5435 0.2536 0.069 Uiso 1 1 calc R . . H63B H 1.1287 1.5300 0.2383 0.069 Uiso 1 1 calc R . . C64 C 0.9372(11) 1.1131(9) 0.5983(6) 0.042(3) Uani 1 1 d . . . H64A H 0.9588 1.0541 0.6243 0.050 Uiso 1 1 calc R . . H64B H 0.8690 1.1190 0.5867 0.050 Uiso 1 1 calc R . . C65 C 1.1914(13) 1.3177(11) 0.3643(7) 0.060(4) Uani 1 1 d . . . H65 H 1.2411 1.2770 0.3882 0.072 Uiso 1 1 calc R . . C66 C 1.1899(11) 1.4122(12) 0.3410(7) 0.061(5) Uani 1 1 d . . . H66 H 1.2365 1.4466 0.3472 0.074 Uiso 1 1 calc R . . C67 C 1.0616(9) 1.3730(9) 0.3113(6) 0.036(3) Uani 1 1 d . . . H67 H 1.0031 1.3768 0.2916 0.043 Uiso 1 1 calc R . . C68 C 1.1391(9) 1.0634(8) 0.4871(5) 0.034(3) Uani 1 1 d . . . H68 H 1.2054 1.0385 0.4726 0.041 Uiso 1 1 calc R . . C69 C 1.1061(10) 1.0504(9) 0.5441(6) 0.036(3) Uani 1 1 d . . . H69 H 1.1449 1.0166 0.5751 0.044 Uiso 1 1 calc R . . C70 C 0.9784(10) 1.1378(8) 0.4926(6) 0.034(3) Uani 1 1 d . . . H70 H 0.9130 1.1746 0.4827 0.041 Uiso 1 1 calc R . . N1 N 0.0608(8) 0.8068(8) -0.1613(5) 0.044(3) Uani 1 1 d . . . N2 N 0.0641(10) 0.9518(8) -0.2016(5) 0.049(3) Uani 1 1 d . . . N3 N 0.0232(15) 1.3791(8) -0.0464(6) 0.075(5) Uani 1 1 d . . . N4 N 0.0334(9) 1.3424(8) 0.0484(5) 0.045(3) Uani 1 1 d . . . N5 N 1.1070(8) 1.4445(8) 0.3072(5) 0.040(3) Uani 1 1 d . . . N6 N 1.1083(8) 1.2940(8) 0.3467(5) 0.037(3) Uani 1 1 d . . . N7 N 1.0594(8) 1.1182(7) 0.4556(4) 0.031(2) Uani 1 1 d . . . N8 N 1.0049(9) 1.0973(8) 0.5452(5) 0.040(3) Uani 1 1 d . . . O1 O 0.1168(7) 1.3860(7) 0.1676(4) 0.048(2) Uani 1 1 d . . . O2 O 0.1559(8) 1.2225(8) 0.1823(5) 0.071(3) Uani 1 1 d . . . O3 O 0.9173(7) 1.2464(6) 0.3256(4) 0.050(3) Uani 1 1 d . . . O4 O 0.8996(7) 1.0983(7) 0.3472(4) 0.046(2) Uani 1 1 d . . . O5 O -0.1759(8) 1.4361(7) 0.1166(5) 0.071(3) Uani 1 1 d . . . O6 O -0.1208(7) 1.4547(7) 0.2017(5) 0.055(3) Uani 1 1 d . . . O7 O -0.8583(6) 2.0434(6) 0.2949(4) 0.039(2) Uani 1 1 d . . . O8 O -0.7527(7) 2.0397(7) 0.3637(4) 0.054(3) Uani 1 1 d . . . Cd1 Cd -0.01215(7) 1.32962(7) 0.14418(4) 0.0361(3) Uani 1 1 d . . . Cd2 Cd 1.06280(7) 1.15567(6) 0.36050(4) 0.0327(3) 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 C1 0.039(9) 0.034(7) 0.046(8) 0.003(6) -0.002(7) -0.009(6) C2 0.041(9) 0.034(8) 0.043(8) 0.008(6) 0.002(7) -0.011(7) C3 0.044(9) 0.028(7) 0.079(11) -0.003(7) -0.028(8) -0.004(6) C4 0.029(9) 0.046(9) 0.094(13) 0.027(8) -0.001(8) 0.000(7) C5 0.046(10) 0.043(9) 0.086(12) 0.020(8) -0.012(9) -0.019(7) C6 0.027(8) 0.049(9) 0.070(10) 0.014(8) -0.007(7) 0.003(7) C7 0.016(7) 0.042(8) 0.071(10) 0.010(7) -0.010(7) -0.007(6) C8 0.049(10) 0.029(8) 0.084(11) 0.011(7) -0.017(8) -0.020(7) C9 0.035(8) 0.033(7) 0.055(9) 0.015(7) -0.007(7) -0.008(6) C10 0.027(8) 0.030(7) 0.077(11) 0.011(7) -0.012(7) -0.015(6) C11 0.047(10) 0.026(7) 0.080(11) 0.002(7) -0.012(8) -0.014(7) C12 0.018(7) 0.037(8) 0.091(12) 0.002(8) -0.022(8) -0.011(6) C13 0.027(8) 0.051(9) 0.046(8) 0.014(7) -0.021(7) -0.019(7) C14 0.029(8) 0.042(8) 0.043(8) -0.012(7) 0.009(6) -0.008(7) C15 0.058(11) 0.051(10) 0.029(8) -0.005(7) 0.001(7) -0.024(9) C16 0.039(9) 0.040(8) 0.101(14) 0.011(8) -0.030(9) -0.014(7) C17 0.036(9) 0.047(9) 0.092(13) -0.008(9) -0.011(9) -0.008(7) C18 0.068(15) 0.099(16) 0.19(3) -0.060(16) 0.010(15) -0.030(12) C19 0.033(9) 0.068(11) 0.084(12) 0.020(9) -0.015(8) -0.026(8) C20 0.045(11) 0.079(12) 0.073(12) 0.021(10) 0.005(9) 0.000(9) C21 0.083(16) 0.19(2) 0.101(17) 0.039(17) 0.014(13) -0.055(16) C22 0.021(7) 0.045(8) 0.047(8) 0.000(6) 0.014(6) -0.011(6) C23 0.036(9) 0.047(8) 0.042(8) 0.005(7) 0.006(7) -0.008(7) C24 0.061(11) 0.096(13) 0.050(10) -0.025(9) 0.016(8) 0.035(10) C25 0.100(15) 0.058(11) 0.056(11) -0.004(9) 0.003(10) 0.023(10) C26 0.092(13) 0.044(9) 0.043(9) -0.011(7) -0.006(9) 0.027(9) C27 0.048(10) 0.050(9) 0.043(9) 0.002(7) 0.002(7) 0.007(7) C28 0.028(8) 0.038(7) 0.039(8) 0.002(6) 0.000(6) -0.009(6) C29 0.051(9) 0.029(7) 0.036(7) -0.007(6) 0.009(7) -0.017(6) C30 0.016(7) 0.031(7) 0.059(9) -0.003(6) 0.005(6) 0.005(6) C31 0.034(8) 0.046(8) 0.039(8) -0.013(7) 0.014(7) -0.002(7) C32 0.036(9) 0.054(9) 0.050(9) 0.002(7) 0.007(7) -0.002(7) C33 0.039(9) 0.041(8) 0.044(9) -0.003(7) 0.004(7) 0.021(7) C34 0.024(7) 0.032(7) 0.055(9) 0.003(6) -0.003(6) -0.006(6) C35 0.042(10) 0.050(9) 0.054(10) 0.009(8) 0.005(8) 0.003(8) C36 0.026(8) 0.029(7) 0.047(9) -0.002(6) 0.005(6) -0.014(6) C37 0.060(11) 0.055(10) 0.079(12) -0.006(9) -0.027(9) 0.027(8) C38 0.075(13) 0.077(12) 0.091(14) -0.030(10) -0.005(10) -0.028(10) C39 0.076(15) 0.115(17) 0.16(2) -0.040(15) -0.077(15) 0.004(13) C40 0.046(10) 0.054(9) 0.053(9) -0.011(7) 0.022(7) -0.012(8) C41 0.068(14) 0.067(12) 0.16(2) 0.030(13) 0.066(13) -0.003(10) C42 0.11(2) 0.14(2) 0.27(4) 0.08(2) 0.06(2) -0.035(17) C43 0.047(10) 0.030(7) 0.046(9) -0.006(6) 0.000(7) -0.009(7) C44 0.081(14) 0.040(9) 0.091(14) 0.008(9) 0.034(10) -0.012(9) C45 0.086(14) 0.063(11) 0.050(10) 0.003(9) 0.023(9) 0.000(10) C46 0.109(15) 0.028(8) 0.030(8) 0.001(6) -0.014(9) -0.004(9) C47 0.081(13) 0.051(10) 0.056(11) 0.004(8) -0.010(10) -0.030(9) C48 0.048(10) 0.055(9) 0.038(8) -0.019(7) 0.007(7) -0.018(7) C49 0.063(11) 0.058(10) 0.035(8) -0.007(7) 0.000(7) -0.024(8) C50 0.26(3) 0.035(9) 0.042(10) 0.003(8) -0.041(14) -0.038(13) C51 0.097(15) 0.037(9) 0.098(14) 0.003(9) -0.028(12) -0.038(10) C52 0.046(11) 0.054(11) 0.120(16) -0.012(10) -0.043(10) -0.010(8) C53 0.047(9) 0.029(7) 0.043(8) -0.001(6) 0.015(7) -0.013(7) C54 0.069(15) 0.28(3) 0.066(15) 0.009(17) 0.010(12) -0.092(19) C55 0.083(15) 0.20(2) 0.038(10) 0.003(12) 0.004(10) -0.076(15) C56 0.081(14) 0.076(12) 0.057(12) 0.001(10) -0.020(11) 0.000(10) C57 0.060(11) 0.020(7) 0.063(10) -0.001(6) 0.009(8) -0.022(7) C58 0.072(11) 0.052(9) 0.047(9) -0.029(7) 0.022(8) -0.047(8) C59 0.062(10) 0.039(8) 0.051(9) -0.014(7) 0.026(7) -0.014(7) C60 0.038(8) 0.031(7) 0.040(8) -0.003(6) 0.004(6) -0.010(6) C61 0.049(10) 0.047(8) 0.054(9) -0.017(7) 0.024(7) -0.025(7) C62 0.057(10) 0.028(7) 0.046(9) -0.008(6) 0.012(7) 0.005(7) C63 0.071(12) 0.027(8) 0.068(11) 0.002(7) -0.002(9) -0.007(7) C64 0.057(10) 0.028(7) 0.040(8) -0.001(6) 0.012(7) -0.014(6) C65 0.074(13) 0.047(9) 0.065(11) 0.007(8) -0.008(9) -0.027(9) C66 0.041(10) 0.074(12) 0.085(12) -0.006(9) -0.018(9) -0.039(9) C67 0.031(8) 0.040(8) 0.040(8) -0.009(6) -0.001(6) -0.013(6) C68 0.031(8) 0.029(7) 0.035(7) -0.003(6) 0.006(6) 0.001(6) C69 0.032(8) 0.030(7) 0.045(8) 0.003(6) -0.009(6) -0.007(6) C70 0.031(8) 0.016(6) 0.054(9) -0.002(6) 0.008(7) -0.007(5) N1 0.042(8) 0.038(7) 0.045(7) -0.002(6) -0.004(6) -0.001(6) N2 0.075(10) 0.029(6) 0.035(7) -0.004(5) -0.007(6) -0.001(6) N3 0.158(17) 0.024(6) 0.037(8) 0.002(5) -0.009(9) -0.017(8) N4 0.060(8) 0.038(6) 0.029(6) -0.015(5) 0.008(6) -0.003(6) N5 0.039(7) 0.034(6) 0.050(7) -0.004(5) -0.004(6) -0.015(5) N6 0.033(7) 0.040(7) 0.042(7) 0.000(5) 0.002(5) -0.019(5) N7 0.038(7) 0.026(5) 0.032(6) -0.002(4) 0.000(5) -0.012(5) N8 0.052(8) 0.032(6) 0.035(7) -0.009(5) 0.001(6) -0.011(5) O1 0.046(6) 0.047(6) 0.042(6) -0.012(5) -0.006(5) 0.005(5) O2 0.043(7) 0.062(7) 0.106(10) 0.015(7) -0.020(6) -0.012(6) O3 0.034(6) 0.037(5) 0.086(8) 0.003(5) -0.013(5) -0.020(5) O4 0.048(6) 0.039(5) 0.045(6) 0.001(4) -0.006(5) -0.001(5) O5 0.071(8) 0.053(6) 0.056(7) -0.009(5) 0.021(6) 0.031(5) O6 0.030(6) 0.040(6) 0.090(8) -0.007(5) 0.013(6) -0.001(5) O7 0.024(5) 0.038(5) 0.049(6) -0.002(4) -0.003(4) 0.001(4) O8 0.036(6) 0.077(7) 0.038(6) -0.018(5) 0.009(5) -0.001(5) Cd1 0.0330(6) 0.0296(6) 0.0412(6) -0.0052(4) -0.0004(5) -0.0021(4) Cd2 0.0319(6) 0.0278(5) 0.0360(6) -0.0043(4) 0.0032(4) -0.0054(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C10 1.351(16) . ? C1 C2 1.397(17) . ? C1 H1 0.9300 . ? C2 C3 1.359(17) . ? C2 C14 1.488(17) . ? C3 C4 1.390(17) . ? C3 H3 0.9300 . ? C4 C11 1.423(18) . ? C4 H4 0.9300 . ? C5 C12 1.349(18) . ? C5 C6 1.391(18) . ? C5 H5 0.9300 . ? C6 C7 1.423(18) . ? C6 H6 0.9300 . ? C7 C8 1.384(17) . ? C7 C15 1.508(18) . ? C8 C13 1.378(16) . ? C8 H8 0.9300 . ? C9 C19 1.505(19) . ? C9 C13 1.506(16) . ? C9 C16 1.547(19) . ? C9 C10 1.554(17) . ? C10 C11 1.412(16) . ? C11 C12 1.421(17) . ? C12 C13 1.405(17) . ? C14 O4 1.232(14) . ? C14 O3 1.286(15) . ? C15 O1 1.252(16) . ? C15 O2 1.254(16) . ? C15 Cd1 2.726(15) . ? C16 C17 1.48(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.51(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.48(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.56(2) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C31 1.376(16) . ? C22 C23 1.380(17) . ? C22 H22 0.9300 . ? C23 C24 1.44(2) . ? C23 C35 1.490(19) . ? C24 C25 1.365(19) . ? C24 H24 0.9300 . ? C25 C32 1.38(2) . ? C25 H25 0.9300 . ? C26 C27 1.395(18) . ? C26 C33 1.389(18) . ? C26 H26 0.9300 . ? C27 C28 1.378(17) . ? C27 H27 0.9300 . ? C28 C29 1.392(16) . ? C28 C36 1.500(17) . ? C29 C34 1.397(17) . ? C29 H29 0.9300 . ? C30 C40 1.484(18) . ? C30 C34 1.508(16) . ? C30 C31 1.525(17) . ? C30 C37 1.60(2) . ? C31 C32 1.376(18) . ? C32 C33 1.486(18) . ? C33 C34 1.360(18) . ? C35 O5 1.236(17) . ? C35 O6 1.267(16) . ? C35 Cd1 2.734(15) . ? C36 O8 1.217(14) . ? C36 O7 1.268(13) . ? C36 Cd2 2.738(13) 1_365 ? C37 C38 1.50(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.57(2) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.51(2) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.59(2) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C48 1.342(18) . ? C43 C44 1.39(2) . ? C43 C49 1.493(17) . ? C44 C45 1.41(2) . ? C44 H44 0.9300 . ? C45 C46 1.41(2) . ? C45 H45 0.9300 . ? C46 C47 1.32(2) . ? C46 C50 1.51(2) . ? C47 C48 1.404(19) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 N2 1.454(16) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 N3 1.472(19) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.30(2) . ? C51 N2 1.368(18) . ? C51 H51 0.9300 . ? C52 N1 1.397(16) . ? C52 H52 0.9300 . ? C53 N2 1.337(16) . ? C53 N1 1.332(15) . ? C53 H53 0.9300 . ? C54 N3 1.33(2) . ? C54 C55 1.33(2) . ? C54 H54 0.9300 . ? C55 N4 1.35(2) . ? C55 H55 0.9300 . ? C56 N4 1.334(18) . ? C56 N3 1.39(2) . ? C56 H56 0.9300 . ? C57 C58 1.385(18) . ? C57 C62 1.383(18) . ? C57 C63 1.508(17) . ? C58 C59 1.388(16) . ? C58 H58 0.9300 . ? C59 C60 1.395(17) . ? C59 H59 0.9300 . ? C60 C61 1.405(17) . ? C60 C64 1.494(16) 2_786 ? C61 C62 1.361(17) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 N5 1.455(16) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 N8 1.482(16) . ? C64 C60 1.494(16) 2_786 ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 N6 1.369(17) . ? C65 C66 1.391(19) . ? C65 H65 0.9300 . ? C66 N5 1.360(16) . ? C66 H66 0.9300 . ? C67 N5 1.324(14) . ? C67 N6 1.349(15) . ? C67 H67 0.9300 . ? C68 N7 1.354(14) . ? C68 C69 1.383(16) . ? C68 H68 0.9300 . ? C69 N8 1.358(15) . ? C69 H69 0.9300 . ? C70 N8 1.322(15) . ? C70 N7 1.342(15) . ? C70 H70 0.9300 . ? N1 Cd1 2.210(11) 2_575 ? N4 Cd1 2.264(11) . ? N6 Cd2 2.204(10) . ? N7 Cd2 2.213(10) . ? O1 Cd1 2.245(9) . ? O2 Cd1 2.528(9) . ? O3 Cd2 2.197(9) . ? O4 Cd2 2.644(9) . ? O5 Cd1 2.403(10) . ? O6 Cd1 2.346(9) . ? O7 Cd2 2.223(8) 1_365 ? O8 Cd2 2.586(9) 1_365 ? Cd1 N1 2.210(11) 2_575 ? Cd2 O7 2.223(8) 1_745 ? Cd2 O8 2.586(9) 1_745 ? Cd2 C36 2.738(13) 1_745 ? 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 C10 C1 C2 121.2(12) . . ? C10 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C3 C2 C1 118.9(13) . . ? C3 C2 C14 120.4(12) . . ? C1 C2 C14 120.7(11) . . ? C2 C3 C4 120.6(13) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C11 121.7(13) . . ? C3 C4 H4 119.1 . . ? C11 C4 H4 119.1 . . ? C12 C5 C6 120.3(13) . . ? C12 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 118.4(12) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C8 C7 C6 119.9(12) . . ? C8 C7 C15 123.7(12) . . ? C6 C7 C15 116.3(12) . . ? C7 C8 C13 120.9(12) . . ? C7 C8 H8 119.5 . . ? C13 C8 H8 119.5 . . ? C19 C9 C13 111.3(11) . . ? C19 C9 C16 109.7(12) . . ? C13 C9 C16 112.7(11) . . ? C19 C9 C10 111.3(11) . . ? C13 C9 C10 100.0(10) . . ? C16 C9 C10 111.5(11) . . ? C1 C10 C11 122.4(12) . . ? C1 C10 C9 130.0(11) . . ? C11 C10 C9 107.6(11) . . ? C10 C11 C4 115.1(12) . . ? C10 C11 C12 112.9(11) . . ? C4 C11 C12 132.0(12) . . ? C5 C12 C13 122.4(12) . . ? C5 C12 C11 132.1(13) . . ? C13 C12 C11 105.5(11) . . ? C8 C13 C12 118.0(12) . . ? C8 C13 C9 127.9(12) . . ? C12 C13 C9 113.9(11) . . ? O4 C14 O3 120.0(12) . . ? O4 C14 C2 123.1(12) . . ? O3 C14 C2 116.8(12) . . ? O1 C15 O2 122.1(14) . . ? O1 C15 C7 119.3(13) . . ? O2 C15 C7 118.7(13) . . ? O1 C15 Cd1 54.6(7) . . ? O2 C15 Cd1 67.5(8) . . ? C7 C15 Cd1 173.4(10) . . ? C17 C16 C9 116.3(12) . . ? C17 C16 H16A 108.2 . . ? C9 C16 H16A 108.2 . . ? C17 C16 H16B 108.2 . . ? C9 C16 H16B 108.2 . . ? H16A C16 H16B 107.4 . . ? C16 C17 C18 112.1(15) . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C9 118.2(13) . . ? C20 C19 H19A 107.8 . . ? C9 C19 H19A 107.8 . . ? C20 C19 H19B 107.8 . . ? C9 C19 H19B 107.8 . . ? H19A C19 H19B 107.1 . . ? C19 C20 C21 113.2(16) . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C31 C22 C23 119.2(13) . . ? C31 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 120.4(13) . . ? C22 C23 C35 122.9(13) . . ? C24 C23 C35 116.7(13) . . ? C25 C24 C23 118.2(15) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? C24 C25 C32 120.5(15) . . ? C24 C25 H25 119.8 . . ? C32 C25 H25 119.8 . . ? C27 C26 C33 117.7(13) . . ? C27 C26 H26 121.2 . . ? C33 C26 H26 121.2 . . ? C26 C27 C28 121.3(13) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 119.5(12) . . ? C29 C28 C36 119.6(11) . . ? C27 C28 C36 120.9(12) . . ? C28 C29 C34 119.9(12) . . ? C28 C29 H29 120.0 . . ? C34 C29 H29 120.0 . . ? C40 C30 C34 112.5(11) . . ? C40 C30 C31 111.2(11) . . ? C34 C30 C31 101.6(11) . . ? C40 C30 C37 111.1(12) . . ? C34 C30 C37 112.5(10) . . ? C31 C30 C37 107.5(11) . . ? C22 C31 C32 120.8(13) . . ? C22 C31 C30 129.1(13) . . ? C32 C31 C30 110.1(11) . . ? C25 C32 C31 120.8(13) . . ? C25 C32 C33 130.6(14) . . ? C31 C32 C33 108.6(13) . . ? C34 C33 C26 122.4(12) . . ? C34 C33 C32 108.2(12) . . ? C26 C33 C32 129.4(13) . . ? C33 C34 C29 119.2(12) . . ? C33 C34 C30 111.5(11) . . ? C29 C34 C30 129.3(12) . . ? O5 C35 O6 120.3(14) . . ? O5 C35 C23 122.5(14) . . ? O6 C35 C23 117.1(15) . . ? O5 C35 Cd1 61.5(8) . . ? O6 C35 Cd1 58.9(7) . . ? C23 C35 Cd1 175.6(12) . . ? O8 C36 O7 122.9(12) . . ? O8 C36 C28 120.5(12) . . ? O7 C36 C28 116.6(11) . . ? O8 C36 Cd2 69.9(7) . 1_365 ? O7 C36 Cd2 53.1(6) . 1_365 ? C28 C36 Cd2 169.0(10) . 1_365 ? C38 C37 C30 119.4(14) . . ? C38 C37 H37A 107.5 . . ? C30 C37 H37A 107.5 . . ? C38 C37 H37B 107.5 . . ? C30 C37 H37B 107.5 . . ? H37A C37 H37B 107.0 . . ? C37 C38 C39 107.3(16) . . ? C37 C38 H38A 110.3 . . ? C39 C38 H38A 110.3 . . ? C37 C38 H38B 110.3 . . ? C39 C38 H38B 110.3 . . ? H38A C38 H38B 108.5 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C30 C40 C41 112.5(13) . . ? C30 C40 H40A 109.1 . . ? C41 C40 H40A 109.1 . . ? C30 C40 H40B 109.1 . . ? C41 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C40 C41 C42 113(2) . . ? C40 C41 H41A 109.0 . . ? C42 C41 H41A 109.0 . . ? C40 C41 H41B 109.0 . . ? C42 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 119.8(13) . . ? C48 C43 C49 120.4(13) . . ? C44 C43 C49 119.7(13) . . ? C43 C44 C45 117.3(15) . . ? C43 C44 H44 121.3 . . ? C45 C44 H44 121.3 . . ? C46 C45 C44 121.5(15) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C47 C46 C45 118.4(14) . . ? C47 C46 C50 122.0(19) . . ? C45 C46 C50 119.6(18) . . ? C46 C47 C48 121.3(15) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C43 C48 C47 121.5(14) . . ? C43 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? N2 C49 C43 113.6(11) . . ? N2 C49 H49A 108.8 . . ? C43 C49 H49A 108.8 . . ? N2 C49 H49B 108.8 . . ? C43 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? N3 C50 C46 111.1(12) . . ? N3 C50 H50A 109.4 . . ? C46 C50 H50A 109.4 . . ? N3 C50 H50B 109.4 . . ? C46 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C52 C51 N2 108.7(14) . . ? C52 C51 H51 125.6 . . ? N2 C51 H51 125.6 . . ? C51 C52 N1 108.8(15) . . ? C51 C52 H52 125.6 . . ? N1 C52 H52 125.6 . . ? N2 C53 N1 110.5(12) . . ? N2 C53 H53 124.7 . . ? N1 C53 H53 124.7 . . ? N3 C54 C55 109.0(18) . . ? N3 C54 H54 125.5 . . ? C55 C54 H54 125.5 . . ? C54 C55 N4 108.7(17) . . ? C54 C55 H55 125.6 . . ? N4 C55 H55 125.6 . . ? N4 C56 N3 107.6(16) . . ? N4 C56 H56 126.2 . . ? N3 C56 H56 126.2 . . ? C58 C57 C62 120.1(12) . . ? C58 C57 C63 119.9(12) . . ? C62 C57 C63 120.0(13) . . ? C57 C58 C59 119.3(12) . . ? C57 C58 H58 120.3 . . ? C59 C58 H58 120.3 . . ? C60 C59 C58 121.4(13) . . ? C60 C59 H59 119.3 . . ? C58 C59 H59 119.3 . . ? C59 C60 C61 117.0(12) . . ? C59 C60 C64 122.7(12) . 2_786 ? C61 C60 C64 120.2(11) . 2_786 ? C62 C61 C60 121.8(13) . . ? C62 C61 H61 119.1 . . ? C60 C61 H61 119.1 . . ? C61 C62 C57 120.1(13) . . ? C61 C62 H62 120.0 . . ? C57 C62 H62 120.0 . . ? N5 C63 C57 111.7(12) . . ? N5 C63 H63A 109.3 . . ? C57 C63 H63A 109.3 . . ? N5 C63 H63B 109.3 . . ? C57 C63 H63B 109.3 . . ? H63A C63 H63B 107.9 . . ? N8 C64 C60 114.4(10) . 2_786 ? N8 C64 H64A 108.7 . . ? C60 C64 H64A 108.7 2_786 . ? N8 C64 H64B 108.7 . . ? C60 C64 H64B 108.7 2_786 . ? H64A C64 H64B 107.6 . . ? N6 C65 C66 109.3(13) . . ? N6 C65 H65 125.3 . . ? C66 C65 H65 125.3 . . ? N5 C66 C65 106.8(12) . . ? N5 C66 H66 126.6 . . ? C65 C66 H66 126.6 . . ? N5 C67 N6 113.7(11) . . ? N5 C67 H67 123.2 . . ? N6 C67 H67 123.2 . . ? N7 C68 C69 109.0(11) . . ? N7 C68 H68 125.5 . . ? C69 C68 H68 125.5 . . ? N8 C69 C68 105.4(11) . . ? N8 C69 H69 127.3 . . ? C68 C69 H69 127.3 . . ? N8 C70 N7 110.3(11) . . ? N8 C70 H70 124.9 . . ? N7 C70 H70 124.9 . . ? C53 N1 C52 105.2(12) . . ? C53 N1 Cd1 124.0(9) . 2_575 ? C52 N1 Cd1 130.7(10) . 2_575 ? C53 N2 C51 106.6(12) . . ? C53 N2 C49 127.7(13) . . ? C51 N2 C49 125.7(13) . . ? C54 N3 C56 106.9(14) . . ? C54 N3 C50 130.0(19) . . ? C56 N3 C50 123.1(19) . . ? C56 N4 C55 107.7(15) . . ? C56 N4 Cd1 124.9(12) . . ? C55 N4 Cd1 126.6(10) . . ? C67 N5 C66 106.5(11) . . ? C67 N5 C63 127.0(12) . . ? C66 N5 C63 126.3(12) . . ? C67 N6 C65 103.7(11) . . ? C67 N6 Cd2 124.9(8) . . ? C65 N6 Cd2 131.0(9) . . ? C68 N7 C70 106.3(10) . . ? C68 N7 Cd2 125.9(8) . . ? C70 N7 Cd2 127.6(9) . . ? C70 N8 C69 109.0(11) . . ? C70 N8 C64 124.9(12) . . ? C69 N8 C64 125.7(11) . . ? C15 O1 Cd1 98.4(9) . . ? C15 O2 Cd1 85.2(9) . . ? C14 O3 Cd2 103.6(8) . . ? C14 O4 Cd2 83.8(8) . . ? C35 O5 Cd1 91.7(9) . . ? C35 O6 Cd1 93.6(9) . . ? C36 O7 Cd2 99.7(7) . 1_365 ? C36 O8 Cd2 83.9(7) . 1_365 ? N1 Cd1 O1 137.6(4) 2_575 . ? N1 Cd1 N4 110.3(4) 2_575 . ? O1 Cd1 N4 88.8(4) . . ? N1 Cd1 O6 106.1(4) 2_575 . ? O1 Cd1 O6 88.7(3) . . ? N4 Cd1 O6 127.7(4) . . ? N1 Cd1 O5 95.4(4) 2_575 . ? O1 Cd1 O5 124.4(4) . . ? N4 Cd1 O5 85.6(4) . . ? O6 Cd1 O5 54.4(4) . . ? N1 Cd1 O2 84.8(4) 2_575 . ? O1 Cd1 O2 54.3(3) . . ? N4 Cd1 O2 99.1(4) . . ? O6 Cd1 O2 120.7(4) . . ? O5 Cd1 O2 174.9(4) . . ? N1 Cd1 C15 111.6(4) 2_575 . ? O1 Cd1 C15 27.0(4) . . ? N4 Cd1 C15 93.8(4) . . ? O6 Cd1 C15 106.3(4) . . ? O5 Cd1 C15 151.3(4) . . ? O2 Cd1 C15 27.3(3) . . ? N1 Cd1 C35 101.9(4) 2_575 . ? O1 Cd1 C35 108.0(4) . . ? N4 Cd1 C35 107.2(4) . . ? O6 Cd1 C35 27.6(4) . . ? O5 Cd1 C35 26.9(4) . . ? O2 Cd1 C35 148.2(5) . . ? C15 Cd1 C35 130.9(5) . . ? O3 Cd2 N6 85.0(4) . . ? O3 Cd2 N7 114.9(4) . . ? N6 Cd2 N7 109.0(4) . . ? O3 Cd2 O7 108.7(3) . 1_745 ? N6 Cd2 O7 110.1(4) . 1_745 ? N7 Cd2 O7 122.6(3) . 1_745 ? O3 Cd2 O8 160.3(3) . 1_745 ? N6 Cd2 O8 93.7(4) . 1_745 ? N7 Cd2 O8 84.1(3) . 1_745 ? O7 Cd2 O8 53.3(3) 1_745 1_745 ? O3 Cd2 O4 52.6(3) . . ? N6 Cd2 O4 137.6(3) . . ? N7 Cd2 O4 90.6(3) . . ? O7 Cd2 O4 87.6(3) 1_745 . ? O8 Cd2 O4 126.3(3) 1_745 . ? O3 Cd2 C36 135.2(4) . 1_745 ? N6 Cd2 C36 102.2(4) . 1_745 ? N7 Cd2 C36 104.4(4) . 1_745 ? O7 Cd2 C36 27.2(3) 1_745 1_745 ? O8 Cd2 C36 26.2(3) 1_745 1_745 ? O4 Cd2 C36 108.9(3) . 1_745 ? 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 C10 C1 C2 C3 -1(2) . . . . ? C10 C1 C2 C14 179.5(12) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C14 C2 C3 C4 -179.7(13) . . . . ? C2 C3 C4 C11 1(2) . . . . ? C12 C5 C6 C7 -1(2) . . . . ? C5 C6 C7 C8 0(2) . . . . ? C5 C6 C7 C15 179.9(13) . . . . ? C6 C7 C8 C13 1(2) . . . . ? C15 C7 C8 C13 -179.0(14) . . . . ? C2 C1 C10 C11 0(2) . . . . ? C2 C1 C10 C9 -178.5(14) . . . . ? C19 C9 C10 C1 58(2) . . . . ? C13 C9 C10 C1 175.3(15) . . . . ? C16 C9 C10 C1 -65.3(19) . . . . ? C19 C9 C10 C11 -121.0(13) . . . . ? C13 C9 C10 C11 -3.2(14) . . . . ? C16 C9 C10 C11 116.2(13) . . . . ? C1 C10 C11 C4 2(2) . . . . ? C9 C10 C11 C4 -179.5(13) . . . . ? C1 C10 C11 C12 -177.0(14) . . . . ? C9 C10 C11 C12 1.6(17) . . . . ? C3 C4 C11 C10 -2(2) . . . . ? C3 C4 C11 C12 176.5(16) . . . . ? C6 C5 C12 C13 1(2) . . . . ? C6 C5 C12 C11 178.9(16) . . . . ? C10 C11 C12 C5 -177.3(17) . . . . ? C4 C11 C12 C5 4(3) . . . . ? C10 C11 C12 C13 0.9(18) . . . . ? C4 C11 C12 C13 -177.7(17) . . . . ? C7 C8 C13 C12 -1(2) . . . . ? C7 C8 C13 C9 -175.3(14) . . . . ? C5 C12 C13 C8 0(2) . . . . ? C11 C12 C13 C8 -178.4(13) . . . . ? C5 C12 C13 C9 175.1(14) . . . . ? C11 C12 C13 C9 -3.3(17) . . . . ? C19 C9 C13 C8 -63.7(19) . . . . ? C16 C9 C13 C8 60.0(19) . . . . ? C10 C9 C13 C8 178.6(14) . . . . ? C19 C9 C13 C12 121.8(14) . . . . ? C16 C9 C13 C12 -114.5(14) . . . . ? C10 C9 C13 C12 4.0(15) . . . . ? C3 C2 C14 O4 -174.4(13) . . . . ? C1 C2 C14 O4 4.6(19) . . . . ? C3 C2 C14 O3 1.8(19) . . . . ? C1 C2 C14 O3 -179.2(12) . . . . ? C8 C7 C15 O1 164.9(14) . . . . ? C6 C7 C15 O1 -15.1(19) . . . . ? C8 C7 C15 O2 -15(2) . . . . ? C6 C7 C15 O2 165.0(14) . . . . ? C8 C7 C15 Cd1 -176(8) . . . . ? C6 C7 C15 Cd1 4(9) . . . . ? C19 C9 C16 C17 171.5(12) . . . . ? C13 C9 C16 C17 46.9(16) . . . . ? C10 C9 C16 C17 -64.7(15) . . . . ? C9 C16 C17 C18 174.7(13) . . . . ? C13 C9 C19 C20 -62.8(16) . . . . ? C16 C9 C19 C20 171.8(12) . . . . ? C10 C9 C19 C20 47.9(17) . . . . ? C9 C19 C20 C21 179.4(13) . . . . ? C31 C22 C23 C24 2(2) . . . . ? C31 C22 C23 C35 -178.5(13) . . . . ? C22 C23 C24 C25 2(3) . . . . ? C35 C23 C24 C25 -178.2(16) . . . . ? C23 C24 C25 C32 -5(3) . . . . ? C33 C26 C27 C28 0(2) . . . . ? C26 C27 C28 C29 1(2) . . . . ? C26 C27 C28 C36 -179.6(14) . . . . ? C27 C28 C29 C34 -2.4(19) . . . . ? C36 C28 C29 C34 178.0(11) . . . . ? C23 C22 C31 C32 -2(2) . . . . ? C23 C22 C31 C30 177.2(13) . . . . ? C40 C30 C31 C22 -60.5(19) . . . . ? C34 C30 C31 C22 179.6(13) . . . . ? C37 C30 C31 C22 61.3(18) . . . . ? C40 C30 C31 C32 118.6(13) . . . . ? C34 C30 C31 C32 -1.3(15) . . . . ? C37 C30 C31 C32 -119.6(13) . . . . ? C24 C25 C32 C31 5(3) . . . . ? C24 C25 C32 C33 -177.2(18) . . . . ? C22 C31 C32 C25 -2(2) . . . . ? C30 C31 C32 C25 179.3(15) . . . . ? C22 C31 C32 C33 -179.7(13) . . . . ? C30 C31 C32 C33 1.1(17) . . . . ? C27 C26 C33 C34 0(2) . . . . ? C27 C26 C33 C32 179.5(16) . . . . ? C25 C32 C33 C34 -178.3(17) . . . . ? C31 C32 C33 C34 -0.3(17) . . . . ? C25 C32 C33 C26 2(3) . . . . ? C31 C32 C33 C26 -179.6(16) . . . . ? C26 C33 C34 C29 -2(2) . . . . ? C32 C33 C34 C29 178.7(12) . . . . ? C26 C33 C34 C30 178.7(14) . . . . ? C32 C33 C34 C30 -0.6(16) . . . . ? C28 C29 C34 C33 3.0(19) . . . . ? C28 C29 C34 C30 -177.9(12) . . . . ? C40 C30 C34 C33 -117.8(14) . . . . ? C31 C30 C34 C33 1.1(15) . . . . ? C37 C30 C34 C33 115.8(14) . . . . ? C40 C30 C34 C29 62.9(18) . . . . ? C31 C30 C34 C29 -178.1(12) . . . . ? C37 C30 C34 C29 -63.4(18) . . . . ? C22 C23 C35 O5 163.7(14) . . . . ? C24 C23 C35 O5 -17(2) . . . . ? C22 C23 C35 O6 -19(2) . . . . ? C24 C23 C35 O6 161.1(14) . . . . ? C22 C23 C35 Cd1 -44(15) . . . . ? C24 C23 C35 Cd1 136(14) . . . . ? C29 C28 C36 O8 25.6(18) . . . . ? C27 C28 C36 O8 -154.0(13) . . . . ? C29 C28 C36 O7 -154.8(11) . . . . ? C27 C28 C36 O7 25.6(18) . . . . ? C29 C28 C36 Cd2 -175(4) . . . 1_365 ? C27 C28 C36 Cd2 5(5) . . . 1_365 ? C40 C30 C37 C38 -61.2(17) . . . . ? C34 C30 C37 C38 65.9(18) . . . . ? C31 C30 C37 C38 176.9(14) . . . . ? C30 C37 C38 C39 -176.3(14) . . . . ? C34 C30 C40 C41 56.0(16) . . . . ? C31 C30 C40 C41 -57.2(16) . . . . ? C37 C30 C40 C41 -176.9(12) . . . . ? C30 C40 C41 C42 178.1(15) . . . . ? C48 C43 C44 C45 -4(2) . . . . ? C49 C43 C44 C45 -179.5(13) . . . . ? C43 C44 C45 C46 0(2) . . . . ? C44 C45 C46 C47 3(2) . . . . ? C44 C45 C46 C50 -179.9(14) . . . . ? C45 C46 C47 C48 -3(2) . . . . ? C50 C46 C47 C48 -179.7(13) . . . . ? C44 C43 C48 C47 4(2) . . . . ? C49 C43 C48 C47 180.0(12) . . . . ? C46 C47 C48 C43 -1(2) . . . . ? C48 C43 C49 N2 112.3(15) . . . . ? C44 C43 C49 N2 -72.0(18) . . . . ? C47 C46 C50 N3 -92(2) . . . . ? C45 C46 C50 N3 91(2) . . . . ? N2 C51 C52 N1 3(2) . . . . ? N3 C54 C55 N4 2(3) . . . . ? C62 C57 C58 C59 -2(2) . . . . ? C63 C57 C58 C59 176.7(13) . . . . ? C57 C58 C59 C60 5(2) . . . . ? C58 C59 C60 C61 -5(2) . . . . ? C58 C59 C60 C64 177.2(13) . . . 2_786 ? C59 C60 C61 C62 4(2) . . . . ? C64 C60 C61 C62 -178.7(13) 2_786 . . . ? C60 C61 C62 C57 -2(2) . . . . ? C58 C57 C62 C61 1(2) . . . . ? C63 C57 C62 C61 -178.3(13) . . . . ? C58 C57 C63 N5 -71.1(18) . . . . ? C62 C57 C63 N5 108.1(15) . . . . ? N6 C65 C66 N5 -2.1(18) . . . . ? N7 C68 C69 N8 1.0(13) . . . . ? N2 C53 N1 C52 1.7(15) . . . . ? N2 C53 N1 Cd1 -175.8(8) . . . 2_575 ? C51 C52 N1 C53 -2.9(18) . . . . ? C51 C52 N1 Cd1 174.4(12) . . . 2_575 ? N1 C53 N2 C51 0.0(16) . . . . ? N1 C53 N2 C49 178.6(12) . . . . ? C52 C51 N2 C53 -1.9(19) . . . . ? C52 C51 N2 C49 179.5(14) . . . . ? C43 C49 N2 C53 120.6(14) . . . . ? C43 C49 N2 C51 -61.0(19) . . . . ? C55 C54 N3 C56 -2(3) . . . . ? C55 C54 N3 C50 178.5(17) . . . . ? N4 C56 N3 C54 0(2) . . . . ? N4 C56 N3 C50 -179.7(12) . . . . ? C46 C50 N3 C54 86(3) . . . . ? C46 C50 N3 C56 -94(2) . . . . ? N3 C56 N4 C55 1.1(19) . . . . ? N3 C56 N4 Cd1 171.0(8) . . . . ? C54 C55 N4 C56 -2(2) . . . . ? C54 C55 N4 Cd1 -171.8(16) . . . . ? N6 C67 N5 C66 0.9(16) . . . . ? N6 C67 N5 C63 176.2(12) . . . . ? C65 C66 N5 C67 0.7(17) . . . . ? C65 C66 N5 C63 -174.6(13) . . . . ? C57 C63 N5 C67 131.2(14) . . . . ? C57 C63 N5 C66 -54.3(19) . . . . ? N5 C67 N6 C65 -2.1(15) . . . . ? N5 C67 N6 Cd2 -175.8(8) . . . . ? C66 C65 N6 C67 2.5(16) . . . . ? C66 C65 N6 Cd2 175.6(10) . . . . ? C69 C68 N7 C70 -0.5(12) . . . . ? C69 C68 N7 Cd2 -176.0(7) . . . . ? N8 C70 N7 C68 -0.2(12) . . . . ? N8 C70 N7 Cd2 175.2(7) . . . . ? N7 C70 N8 C69 0.8(13) . . . . ? N7 C70 N8 C64 173.1(10) . . . . ? C68 C69 N8 C70 -1.1(13) . . . . ? C68 C69 N8 C64 -173.3(11) . . . . ? C60 C64 N8 C70 -86.9(15) 2_786 . . . ? C60 C64 N8 C69 84.2(14) 2_786 . . . ? O2 C15 O1 Cd1 -2.7(15) . . . . ? C7 C15 O1 Cd1 177.4(10) . . . . ? O1 C15 O2 Cd1 2.4(13) . . . . ? C7 C15 O2 Cd1 -177.7(11) . . . . ? O4 C14 O3 Cd2 2.7(14) . . . . ? C2 C14 O3 Cd2 -173.7(9) . . . . ? O3 C14 O4 Cd2 -2.2(11) . . . . ? C2 C14 O4 Cd2 173.9(12) . . . . ? O6 C35 O5 Cd1 0.1(15) . . . . ? C23 C35 O5 Cd1 177.7(13) . . . . ? O5 C35 O6 Cd1 -0.1(16) . . . . ? C23 C35 O6 Cd1 -177.8(11) . . . . ? O8 C36 O7 Cd2 4.4(14) . . . 1_365 ? C28 C36 O7 Cd2 -175.2(9) . . . 1_365 ? O7 C36 O8 Cd2 -3.7(12) . . . 1_365 ? C28 C36 O8 Cd2 175.9(11) . . . 1_365 ? C15 O1 Cd1 N1 18.8(10) . . . 2_575 ? C15 O1 Cd1 N4 -100.7(8) . . . . ? C15 O1 Cd1 O6 131.5(8) . . . . ? C15 O1 Cd1 O5 175.5(7) . . . . ? C15 O1 Cd1 O2 1.4(8) . . . . ? C15 O1 Cd1 C35 151.5(8) . . . . ? C56 N4 Cd1 N1 68.9(12) . . . 2_575 ? C55 N4 Cd1 N1 -123.0(15) . . . 2_575 ? C56 N4 Cd1 O1 -149.8(12) . . . . ? C55 N4 Cd1 O1 18.3(15) . . . . ? C56 N4 Cd1 O6 -62.3(13) . . . . ? C55 N4 Cd1 O6 105.8(15) . . . . ? C56 N4 Cd1 O5 -25.2(12) . . . . ? C55 N4 Cd1 O5 142.9(15) . . . . ? C56 N4 Cd1 O2 156.7(12) . . . . ? C55 N4 Cd1 O2 -35.2(15) . . . . ? C56 N4 Cd1 C15 -176.4(12) . . . . ? C55 N4 Cd1 C15 -8.3(15) . . . . ? C56 N4 Cd1 C35 -41.3(13) . . . . ? C55 N4 Cd1 C35 126.8(15) . . . . ? C35 O6 Cd1 N1 -85.0(9) . . . 2_575 ? C35 O6 Cd1 O1 135.3(9) . . . . ? C35 O6 Cd1 N4 47.8(10) . . . . ? C35 O6 Cd1 O5 0.1(8) . . . . ? C35 O6 Cd1 O2 -178.5(8) . . . . ? C35 O6 Cd1 C15 156.1(9) . . . . ? C35 O5 Cd1 N1 105.9(10) . . . 2_575 ? C35 O5 Cd1 O1 -58.6(10) . . . . ? C35 O5 Cd1 N4 -144.1(10) . . . . ? C35 O5 Cd1 O6 -0.1(9) . . . . ? C35 O5 Cd1 O2 14(5) . . . . ? C35 O5 Cd1 C15 -54.3(13) . . . . ? C15 O2 Cd1 N1 -169.7(9) . . . 2_575 ? C15 O2 Cd1 O1 -1.4(8) . . . . ? C15 O2 Cd1 N4 80.5(9) . . . . ? C15 O2 Cd1 O6 -64.1(9) . . . . ? C15 O2 Cd1 O5 -78(4) . . . . ? C15 O2 Cd1 C35 -65.5(12) . . . . ? O1 C15 Cd1 N1 -166.5(7) . . . 2_575 ? O2 C15 Cd1 N1 11.0(10) . . . 2_575 ? C7 C15 Cd1 N1 173(8) . . . 2_575 ? O2 C15 Cd1 O1 177.5(14) . . . . ? C7 C15 Cd1 O1 -21(8) . . . . ? O1 C15 Cd1 N4 79.9(8) . . . . ? O2 C15 Cd1 N4 -102.6(9) . . . . ? C7 C15 Cd1 N4 59(9) . . . . ? O1 C15 Cd1 O6 -51.3(8) . . . . ? O2 C15 Cd1 O6 126.3(8) . . . . ? C7 C15 Cd1 O6 -72(9) . . . . ? O1 C15 Cd1 O5 -7.8(13) . . . . ? O2 C15 Cd1 O5 169.7(8) . . . . ? C7 C15 Cd1 O5 -28(9) . . . . ? O1 C15 Cd1 O2 -177.5(14) . . . . ? C7 C15 Cd1 O2 162(9) . . . . ? O1 C15 Cd1 C35 -36.9(10) . . . . ? O2 C15 Cd1 C35 140.6(8) . . . . ? C7 C15 Cd1 C35 -57(9) . . . . ? O5 C35 Cd1 N1 -78.2(10) . . . 2_575 ? O6 C35 Cd1 N1 102.0(8) . . . 2_575 ? C23 C35 Cd1 N1 128(14) . . . 2_575 ? O5 C35 Cd1 O1 132.2(9) . . . . ? O6 C35 Cd1 O1 -47.6(9) . . . . ? C23 C35 Cd1 O1 -21(14) . . . . ? O5 C35 Cd1 N4 37.7(10) . . . . ? O6 C35 Cd1 N4 -142.1(8) . . . . ? C23 C35 Cd1 N4 -116(14) . . . . ? O5 C35 Cd1 O6 179.9(15) . . . . ? C23 C35 Cd1 O6 26(14) . . . . ? O6 C35 Cd1 O5 -179.9(15) . . . . ? C23 C35 Cd1 O5 -154(14) . . . . ? O5 C35 Cd1 O2 -177.6(8) . . . . ? O6 C35 Cd1 O2 2.5(13) . . . . ? C23 C35 Cd1 O2 29(14) . . . . ? O5 C35 Cd1 C15 148.9(9) . . . . ? O6 C35 Cd1 C15 -31.0(11) . . . . ? C23 C35 Cd1 C15 -5(14) . . . . ? C14 O3 Cd2 N6 179.9(9) . . . . ? C14 O3 Cd2 N7 -71.4(9) . . . . ? C14 O3 Cd2 O7 70.3(9) . . . 1_745 ? C14 O3 Cd2 O8 92.7(12) . . . 1_745 ? C14 O3 Cd2 O4 -1.4(7) . . . . ? C14 O3 Cd2 C36 77.7(9) . . . 1_745 ? C67 N6 Cd2 O3 -18.7(10) . . . . ? C65 N6 Cd2 O3 169.5(13) . . . . ? C67 N6 Cd2 N7 -133.3(10) . . . . ? C65 N6 Cd2 N7 54.8(13) . . . . ? C67 N6 Cd2 O7 89.5(10) . . . 1_745 ? C65 N6 Cd2 O7 -82.4(13) . . . 1_745 ? C67 N6 Cd2 O8 141.7(10) . . . 1_745 ? C65 N6 Cd2 O8 -30.2(13) . . . 1_745 ? C67 N6 Cd2 O4 -20.2(12) . . . . ? C65 N6 Cd2 O4 168.0(11) . . . . ? C67 N6 Cd2 C36 116.6(10) . . . 1_745 ? C65 N6 Cd2 C36 -55.3(13) . . . 1_745 ? C68 N7 Cd2 O3 180.0(8) . . . . ? C70 N7 Cd2 O3 5.4(10) . . . . ? C68 N7 Cd2 N6 -86.6(9) . . . . ? C70 N7 Cd2 N6 98.8(9) . . . . ? C68 N7 Cd2 O7 44.1(10) . . . 1_745 ? C70 N7 Cd2 O7 -130.5(9) . . . 1_745 ? C68 N7 Cd2 O8 5.3(9) . . . 1_745 ? C70 N7 Cd2 O8 -169.3(9) . . . 1_745 ? C68 N7 Cd2 O4 131.7(9) . . . . ? C70 N7 Cd2 O4 -42.9(9) . . . . ? C68 N7 Cd2 C36 21.9(9) . . . 1_745 ? C70 N7 Cd2 C36 -152.6(9) . . . 1_745 ? C14 O4 Cd2 O3 1.4(7) . . . . ? C14 O4 Cd2 N6 3.3(9) . . . . ? C14 O4 Cd2 N7 122.9(7) . . . . ? C14 O4 Cd2 O7 -114.5(7) . . . 1_745 ? C14 O4 Cd2 O8 -154.0(7) . . . 1_745 ? C14 O4 Cd2 C36 -131.6(7) . . . 1_745 ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.356 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.143 #====END data_compound5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C31 H34 N4 O4 Zn' _chemical_formula_sum 'C31 H34 N4 O4 Zn' _chemical_formula_weight 592.01 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 pbcm _symmetry_space_group_name_Hall -p2c2b loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.783(2) _cell_length_b 24.640(6) _cell_length_c 14.613(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3162.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3248 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7289 _exptl_absorpt_correction_T_max 0.7834 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16860 _diffrn_reflns_av_R_equivalents 0.1422 _diffrn_reflns_av_sigmaI/netI 0.0990 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.06 _reflns_number_total 3248 _reflns_number_gt 2136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0932P)^2^+2.3197P] 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 3248 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1399 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2179 _refine_ls_wR_factor_gt 0.1928 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 C1 C 0.7781(10) -0.1321(3) 0.2500 0.0240(19) Uani 1 2 d S . . H12 H 0.8314 -0.0995 0.2500 0.029 Uiso 1 2 calc SR . . C2 C 0.6180(10) -0.1321(4) 0.2500 0.027(2) Uani 1 2 d S . . C3 C 0.5429(11) -0.1814(4) 0.2500 0.039(2) Uani 1 2 d S . . H10 H 0.4370 -0.1813 0.2500 0.046 Uiso 1 2 calc SR . . C4 C 0.6177(10) -0.2313(4) 0.2500 0.040(3) Uani 1 2 d S . . H9 H 0.5639 -0.2638 0.2500 0.048 Uiso 1 2 calc SR . . C5 C 0.8712(11) -0.3313(3) 0.2500 0.034(2) Uani 1 2 d S . . H3 H 0.7752 -0.3472 0.2500 0.041 Uiso 1 2 calc SR . . C6 C 1.0001(10) -0.3626(3) 0.2500 0.029(2) Uani 1 2 d S . . H2 H 0.9900 -0.4001 0.2500 0.035 Uiso 1 2 calc SR . . C7 C 1.1436(11) -0.3405(3) 0.2500 0.027(2) Uani 1 2 d S . . C8 C 1.1610(10) -0.2849(3) 0.2500 0.026(2) Uani 1 2 d S . . H6 H 1.2579 -0.2696 0.2500 0.032 Uiso 1 2 calc SR . . C9 C 1.0267(10) -0.1898(3) 0.2500 0.0221(18) Uani 1 2 d S . . C10 C 0.8560(9) -0.1808(3) 0.2500 0.0242(19) Uani 1 2 d S . . C11 C 0.7744(11) -0.2305(4) 0.2500 0.031(2) Uani 1 2 d S . . C12 C 0.8875(10) -0.2742(3) 0.2500 0.026(2) Uani 1 2 d S . . C13 C 1.0341(10) -0.2519(3) 0.2500 0.0202(17) Uani 1 2 d S . . C14 C 0.5321(11) -0.0785(3) 0.2500 0.029(2) Uani 1 2 d S . . C15 C 1.2832(11) -0.3757(4) 0.2500 0.026(2) Uani 1 2 d S . . C16 C 1.1026(7) -0.1655(2) 0.3358(4) 0.0297(15) Uani 1 1 d . . . H16A H 1.2099 -0.1749 0.3350 0.036 Uiso 1 1 calc R . . H16B H 1.0952 -0.1263 0.3325 0.036 Uiso 1 1 calc R . . C17 C 1.0355(10) -0.1840(3) 0.4259(4) 0.052(2) Uani 1 1 d . . . H17A H 0.9318 -0.1708 0.4305 0.063 Uiso 1 1 calc R . . H17B H 1.0318 -0.2234 0.4267 0.063 Uiso 1 1 calc R . . C18 C 1.1237(14) -0.1648(4) 0.5074(6) 0.106(5) Uani 1 1 d . . . H18A H 1.0755 -0.1775 0.5623 0.158 Uiso 1 1 calc R . . H18B H 1.1265 -0.1259 0.5077 0.158 Uiso 1 1 calc R . . H18C H 1.2257 -0.1787 0.5044 0.158 Uiso 1 1 calc R . . C19 C 0.3351(8) 0.0800(3) 0.0004(4) 0.0368(16) Uani 1 1 d . . . H23 H 0.3120 0.1032 -0.0479 0.044 Uiso 1 1 calc R . . C20 C 0.4144(8) 0.0924(3) 0.0768(5) 0.0387(18) Uani 1 1 d . . . H24 H 0.4567 0.1261 0.0899 0.046 Uiso 1 1 calc R . . C21 C 0.3506(7) 0.0085(2) 0.0885(4) 0.0286(15) Uani 1 1 d . . . H22 H 0.3395 -0.0267 0.1105 0.034 Uiso 1 1 calc R . . C22 C 0.2025(8) -0.0046(3) -0.0570(4) 0.0350(16) Uani 1 1 d . . . H25A H 0.2211 -0.0431 -0.0487 0.042 Uiso 1 1 calc R . . H25B H 0.2339 0.0049 -0.1186 0.042 Uiso 1 1 calc R . . C23 C 0.0320(8) 0.0063(3) -0.0470(4) 0.0417(17) Uani 1 1 d . . . H26A H 0.0127 0.0442 -0.0608 0.050 Uiso 1 1 calc R . . H26B H -0.0223 -0.0153 -0.0920 0.050 Uiso 1 1 calc R . . N1 N 0.4227(6) 0.0473(2) 0.1322(3) 0.0277(12) Uani 1 1 d . . . N2 N 0.2950(6) 0.0258(2) 0.0085(4) 0.0290(12) Uani 1 1 d . . . O1 O 0.6167(7) -0.0358(2) 0.2500 0.0273(13) Uani 1 2 d S . . O2 O 0.3924(7) -0.0784(2) 0.2500 0.0367(16) Uani 1 2 d S . . O3 O 1.2637(7) -0.4267(2) 0.2500 0.0319(15) Uani 1 2 d S . . O4 O 1.4122(8) -0.3550(3) 0.2500 0.0427(18) Uani 1 2 d S . . Zn1 Zn 0.53557(11) 0.03802(4) 0.2500 0.0223(3) Uani 1 2 d S . . 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 C1 0.029(5) 0.019(4) 0.024(5) 0.000 0.000 -0.001(4) C2 0.026(5) 0.033(5) 0.023(5) 0.000 0.000 0.009(4) C3 0.016(5) 0.033(5) 0.067(7) 0.000 0.000 -0.003(4) C4 0.020(5) 0.024(5) 0.076(8) 0.000 0.000 -0.001(4) C5 0.030(6) 0.023(5) 0.050(6) 0.000 0.000 -0.001(4) C6 0.041(6) 0.017(4) 0.028(5) 0.000 0.000 0.002(4) C7 0.041(6) 0.030(5) 0.012(4) 0.000 0.000 0.007(4) C8 0.024(5) 0.034(5) 0.022(5) 0.000 0.000 -0.002(4) C9 0.024(5) 0.016(4) 0.026(4) 0.000 0.000 0.001(4) C10 0.019(5) 0.022(4) 0.032(5) 0.000 0.000 0.003(4) C11 0.034(6) 0.028(5) 0.031(5) 0.000 0.000 0.000(4) C12 0.030(5) 0.015(4) 0.032(5) 0.000 0.000 0.002(4) C13 0.019(4) 0.023(4) 0.018(4) 0.000 0.000 0.003(4) C14 0.028(5) 0.025(5) 0.034(5) 0.000 0.000 0.002(5) C15 0.032(5) 0.031(5) 0.013(4) 0.000 0.000 0.010(4) C16 0.033(4) 0.029(3) 0.027(3) -0.008(3) -0.007(3) 0.003(3) C17 0.086(6) 0.047(4) 0.025(4) -0.001(3) -0.003(4) 0.010(4) C18 0.213(14) 0.069(6) 0.034(5) -0.003(5) -0.041(7) -0.020(8) C19 0.046(4) 0.037(4) 0.028(4) 0.013(3) -0.006(3) -0.001(3) C20 0.040(4) 0.031(4) 0.045(4) 0.005(3) -0.009(3) -0.002(3) C21 0.029(4) 0.029(3) 0.028(3) 0.002(3) -0.004(3) 0.006(3) C22 0.030(4) 0.051(4) 0.024(3) -0.006(3) 0.001(3) -0.005(3) C23 0.035(4) 0.059(5) 0.031(4) -0.002(3) -0.006(3) -0.003(4) N1 0.024(3) 0.031(3) 0.028(3) 0.002(2) -0.002(2) 0.001(2) N2 0.025(3) 0.035(3) 0.026(3) -0.005(2) 0.000(2) 0.001(2) O1 0.026(3) 0.018(3) 0.038(4) 0.000 0.000 0.002(3) O2 0.026(4) 0.030(3) 0.054(4) 0.000 0.000 0.002(3) O3 0.040(4) 0.023(3) 0.032(4) 0.000 0.000 0.012(3) O4 0.030(4) 0.042(4) 0.057(5) 0.000 0.000 0.015(3) Zn1 0.0209(5) 0.0224(5) 0.0236(5) 0.000 0.000 0.0012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C10 1.380(11) . ? C1 C2 1.407(12) . ? C1 H12 0.9300 . ? C2 C3 1.383(12) . ? C2 C14 1.519(12) . ? C3 C4 1.394(12) . ? C3 H10 0.9300 . ? C4 C11 1.377(12) . ? C4 H9 0.9300 . ? C5 C6 1.370(12) . ? C5 C12 1.414(11) . ? C5 H3 0.9300 . ? C6 C7 1.373(12) . ? C6 H2 0.9300 . ? C7 C8 1.379(11) . ? C7 C15 1.502(12) . ? C8 C13 1.379(11) . ? C8 H6 0.9300 . ? C9 C10 1.516(12) . ? C9 C13 1.531(11) . ? C9 C16 1.542(7) . ? C9 C16 1.542(7) 6_556 ? C10 C11 1.419(12) . ? C11 C12 1.465(12) . ? C12 C13 1.400(12) . ? C14 O2 1.226(10) . ? C14 O1 1.290(10) . ? C15 O4 1.242(11) . ? C15 O3 1.267(10) . ? C16 C17 1.513(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.497(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.350(9) . ? C19 N2 1.386(8) . ? C19 H23 0.9300 . ? C20 N1 1.376(8) . ? C20 H24 0.9300 . ? C21 N1 1.313(8) . ? C21 N2 1.336(8) . ? C21 H22 0.9300 . ? C22 N2 1.463(8) . ? C22 C23 1.529(10) . ? C22 H25A 0.9700 . ? C22 H25B 0.9700 . ? C23 C23 1.517(13) 5 ? C23 H26A 0.9700 . ? C23 H26B 0.9700 . ? N1 Zn1 2.000(5) . ? O1 Zn1 1.953(6) . ? O3 Zn1 1.966(6) 7_755 ? Zn1 O3 1.966(6) 7_765 ? Zn1 N1 2.000(5) 6_556 ? 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 C10 C1 C2 119.7(8) . . ? C10 C1 H12 120.1 . . ? C2 C1 H12 120.1 . . ? C3 C2 C1 118.4(8) . . ? C3 C2 C14 121.7(8) . . ? C1 C2 C14 119.8(8) . . ? C2 C3 C4 123.4(9) . . ? C2 C3 H10 118.3 . . ? C4 C3 H10 118.3 . . ? C11 C4 C3 117.3(9) . . ? C11 C4 H9 121.4 . . ? C3 C4 H9 121.4 . . ? C6 C5 C12 118.5(9) . . ? C6 C5 H3 120.8 . . ? C12 C5 H3 120.8 . . ? C5 C6 C7 122.4(8) . . ? C5 C6 H2 118.8 . . ? C7 C6 H2 118.8 . . ? C6 C7 C8 119.7(8) . . ? C6 C7 C15 121.4(8) . . ? C8 C7 C15 118.9(8) . . ? C13 C8 C7 119.7(8) . . ? C13 C8 H6 120.2 . . ? C7 C8 H6 120.2 . . ? C10 C9 C13 100.9(7) . . ? C10 C9 C16 111.8(5) . . ? C13 C9 C16 111.7(5) . . ? C10 C9 C16 111.8(5) . 6_556 ? C13 C9 C16 111.7(5) . 6_556 ? C16 C9 C16 108.9(7) . 6_556 ? C1 C10 C11 120.0(8) . . ? C1 C10 C9 128.2(8) . . ? C11 C10 C9 111.9(7) . . ? C4 C11 C10 121.2(8) . . ? C4 C11 C12 131.8(8) . . ? C10 C11 C12 107.0(8) . . ? C13 C12 C5 118.9(8) . . ? C13 C12 C11 109.6(7) . . ? C5 C12 C11 131.5(8) . . ? C8 C13 C12 120.9(7) . . ? C8 C13 C9 128.5(8) . . ? C12 C13 C9 110.6(7) . . ? O2 C14 O1 125.0(8) . . ? O2 C14 C2 120.0(8) . . ? O1 C14 C2 115.0(8) . . ? O4 C15 O3 122.0(8) . . ? O4 C15 C7 120.4(8) . . ? O3 C15 C7 117.5(8) . . ? C17 C16 C9 115.0(6) . . ? C17 C16 H16A 108.5 . . ? C9 C16 H16A 108.5 . . ? C17 C16 H16B 108.5 . . ? C9 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C18 C17 C16 113.3(7) . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N2 106.1(6) . . ? C20 C19 H23 126.9 . . ? N2 C19 H23 126.9 . . ? C19 C20 N1 109.4(6) . . ? C19 C20 H24 125.3 . . ? N1 C20 H24 125.3 . . ? N1 C21 N2 111.7(5) . . ? N1 C21 H22 124.2 . . ? N2 C21 H22 124.2 . . ? N2 C22 C23 113.0(5) . . ? N2 C22 H25A 109.0 . . ? C23 C22 H25A 109.0 . . ? N2 C22 H25B 109.0 . . ? C23 C22 H25B 109.0 . . ? H25A C22 H25B 107.8 . . ? C23 C23 C22 114.4(7) 5 . ? C23 C23 H26A 108.7 5 . ? C22 C23 H26A 108.7 . . ? C23 C23 H26B 108.7 5 . ? C22 C23 H26B 108.7 . . ? H26A C23 H26B 107.6 . . ? C21 N1 C20 106.0(5) . . ? C21 N1 Zn1 125.1(4) . . ? C20 N1 Zn1 128.7(4) . . ? C21 N2 C19 106.8(5) . . ? C21 N2 C22 127.8(5) . . ? C19 N2 C22 125.3(5) . . ? C14 O1 Zn1 123.4(6) . . ? C15 O3 Zn1 108.5(6) . 7_755 ? O1 Zn1 O3 94.9(2) . 7_765 ? O1 Zn1 N1 106.72(16) . . ? O3 Zn1 N1 113.20(16) 7_765 . ? O1 Zn1 N1 106.72(16) . 6_556 ? O3 Zn1 N1 113.20(16) 7_765 6_556 ? N1 Zn1 N1 118.8(3) . 6_556 ? 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 C10 C1 C2 C3 0.0 . . . . ? C10 C1 C2 C14 180.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C14 C2 C3 C4 180.0 . . . . ? C2 C3 C4 C11 0.0 . . . . ? C12 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C5 C6 C7 C15 180.0 . . . . ? C6 C7 C8 C13 0.0 . . . . ? C15 C7 C8 C13 180.0 . . . . ? C2 C1 C10 C11 0.0 . . . . ? C2 C1 C10 C9 180.0 . . . . ? C13 C9 C10 C1 180.0 . . . . ? C16 C9 C10 C1 61.2(5) . . . . ? C16 C9 C10 C1 -61.2(5) 6_556 . . . ? C13 C9 C10 C11 0.0 . . . . ? C16 C9 C10 C11 -118.8(5) . . . . ? C16 C9 C10 C11 118.8(5) 6_556 . . . ? C3 C4 C11 C10 0.0 . . . . ? C3 C4 C11 C12 180.0 . . . . ? C1 C10 C11 C4 0.0 . . . . ? C9 C10 C11 C4 180.0 . . . . ? C1 C10 C11 C12 180.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C6 C5 C12 C13 0.0 . . . . ? C6 C5 C12 C11 180.0 . . . . ? C4 C11 C12 C13 180.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C4 C11 C12 C5 0.0 . . . . ? C10 C11 C12 C5 180.0 . . . . ? C7 C8 C13 C12 0.0 . . . . ? C7 C8 C13 C9 180.0 . . . . ? C5 C12 C13 C8 0.0 . . . . ? C11 C12 C13 C8 180.0 . . . . ? C5 C12 C13 C9 180.0 . . . . ? C11 C12 C13 C9 0.0 . . . . ? C10 C9 C13 C8 180.0 . . . . ? C16 C9 C13 C8 -61.1(5) . . . . ? C16 C9 C13 C8 61.1(5) 6_556 . . . ? C10 C9 C13 C12 0.0 . . . . ? C16 C9 C13 C12 118.9(5) . . . . ? C16 C9 C13 C12 -118.9(5) 6_556 . . . ? C3 C2 C14 O2 0.0 . . . . ? C1 C2 C14 O2 180.0 . . . . ? C3 C2 C14 O1 180.0 . . . . ? C1 C2 C14 O1 0.0 . . . . ? C6 C7 C15 O4 180.0 . . . . ? C8 C7 C15 O4 0.0 . . . . ? C6 C7 C15 O3 0.0 . . . . ? C8 C7 C15 O3 180.0 . . . . ? C10 C9 C16 C17 53.8(8) . . . . ? C13 C9 C16 C17 -58.4(8) . . . . ? C16 C9 C16 C17 177.7(4) 6_556 . . . ? C9 C16 C17 C18 173.2(7) . . . . ? N2 C19 C20 N1 -0.7(8) . . . . ? N2 C22 C23 C23 -57.9(10) . . . 5 ? N2 C21 N1 C20 -0.5(7) . . . . ? N2 C21 N1 Zn1 -175.5(4) . . . . ? C19 C20 N1 C21 0.7(8) . . . . ? C19 C20 N1 Zn1 175.5(5) . . . . ? N1 C21 N2 C19 0.1(7) . . . . ? N1 C21 N2 C22 -176.9(5) . . . . ? C20 C19 N2 C21 0.4(7) . . . . ? C20 C19 N2 C22 177.4(6) . . . . ? C23 C22 N2 C21 97.1(8) . . . . ? C23 C22 N2 C19 -79.3(8) . . . . ? O2 C14 O1 Zn1 0.0 . . . . ? C2 C14 O1 Zn1 180.0 . . . . ? O4 C15 O3 Zn1 0.0 . . . 7_755 ? C7 C15 O3 Zn1 180.0 . . . 7_755 ? C14 O1 Zn1 O3 180.0 . . . 7_765 ? C14 O1 Zn1 N1 -64.00(16) . . . . ? C14 O1 Zn1 N1 64.00(16) . . . 6_556 ? C21 N1 Zn1 O1 31.6(6) . . . . ? C20 N1 Zn1 O1 -142.2(6) . . . . ? C21 N1 Zn1 O3 134.7(5) . . . 7_765 ? C20 N1 Zn1 O3 -39.2(6) . . . 7_765 ? C21 N1 Zn1 N1 -88.9(6) . . . 6_556 ? C20 N1 Zn1 N1 97.2(6) . . . 6_556 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.377 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.137 #====END data_compound6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C34 H41 Cd N5 O5' _chemical_formula_sum 'C34 H41 Cd N5 O5' _chemical_formula_weight 712.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1771(9) _cell_length_b 11.5147(8) _cell_length_c 22.2995(15) _cell_angle_alpha 90.00 _cell_angle_beta 95.6420(10) _cell_angle_gamma 90.00 _cell_volume 3367.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6631 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7572 _exptl_absorpt_correction_T_max 0.8460 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18460 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.04 _reflns_number_total 6631 _reflns_number_gt 5012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+5.0316P] 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 6631 _refine_ls_number_parameters 406 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1433 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.080 _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 C1 C 0.7692(4) 0.6093(4) 0.3827(2) 0.0333(11) Uani 1 1 d . . . H6 H 0.8369 0.5924 0.3777 0.040 Uiso 1 1 calc R . . C2 C 0.6905(4) 0.5482(4) 0.3502(2) 0.0297(10) Uani 1 1 d . . . C3 C 0.5886(4) 0.5770(4) 0.3560(2) 0.0357(11) Uani 1 1 d . . . H2 H 0.5367 0.5386 0.3326 0.043 Uiso 1 1 calc R . . C4 C 0.5642(4) 0.6615(5) 0.3961(2) 0.0374(12) Uani 1 1 d . . . H3 H 0.4965 0.6800 0.4001 0.045 Uiso 1 1 calc R . . C5 C 0.5576(4) 0.8488(5) 0.5058(2) 0.0417(13) Uani 1 1 d . . . H8 H 0.4914 0.8256 0.4929 0.050 Uiso 1 1 calc R . . C6 C 0.5756(4) 0.9277(5) 0.5523(2) 0.0413(13) Uani 1 1 d . . . H9 H 0.5211 0.9579 0.5707 0.050 Uiso 1 1 calc R . . C7 C 0.6740(4) 0.9623(4) 0.5717(2) 0.0366(12) Uani 1 1 d . . . C8 C 0.7574(4) 0.9162(4) 0.5445(2) 0.0386(12) Uani 1 1 d . . . H11 H 0.8236 0.9386 0.5576 0.046 Uiso 1 1 calc R . . C9 C 0.7392(4) 0.8376(4) 0.4983(2) 0.0353(11) Uani 1 1 d . . . C10 C 0.6390(4) 0.8048(4) 0.4787(2) 0.0334(11) Uani 1 1 d . . . C11 C 0.6422(4) 0.7181(4) 0.4303(2) 0.0338(11) Uani 1 1 d . . . C12 C 0.7455(4) 0.6956(4) 0.4226(2) 0.0320(11) Uani 1 1 d . . . C13 C 0.8151(4) 0.7779(4) 0.4595(3) 0.0403(13) Uani 1 1 d . . . C14 C 0.6921(5) 1.0509(4) 0.6212(2) 0.0378(12) Uani 1 1 d . . . C15 C 0.7144(4) 0.4516(4) 0.3075(2) 0.0305(10) Uani 1 1 d . . . C16 C 0.9040(5) 0.7172(6) 0.4976(3) 0.0556(17) Uani 1 1 d . . . H14A H 0.9509 0.6875 0.4704 0.067 Uiso 1 1 calc R . . H14B H 0.9403 0.7754 0.5228 0.067 Uiso 1 1 calc R . . C17 C 0.8767(5) 0.6212(6) 0.5365(3) 0.0600(17) Uani 1 1 d . . . H15A H 0.8451 0.5592 0.5119 0.072 Uiso 1 1 calc R . . H15B H 0.8279 0.6483 0.5632 0.072 Uiso 1 1 calc R . . C18 C 0.9729(6) 0.5744(8) 0.5743(3) 0.095(3) Uani 1 1 d . . . H16A H 0.9540 0.5117 0.5994 0.142 Uiso 1 1 calc R . . H16B H 1.0034 0.6355 0.5992 0.142 Uiso 1 1 calc R . . H16C H 1.0208 0.5468 0.5479 0.142 Uiso 1 1 calc R . . C19 C 0.8573(7) 0.8664(6) 0.4163(4) 0.095(3) Uani 1 1 d D . . H19A H 0.9026 0.8211 0.3937 0.114 Uiso 1 1 calc R . . H19B H 0.7992 0.8854 0.3878 0.114 Uiso 1 1 calc R . . C20 C 0.9086(19) 0.9733(10) 0.4267(8) 0.57(4) Uani 1 1 d D . . H20A H 0.9781 0.9587 0.4437 0.684 Uiso 1 1 calc R . . H20B H 0.8748 1.0182 0.4558 0.684 Uiso 1 1 calc R . . C21 C 0.9101(12) 1.0426(9) 0.3689(5) 0.177(7) Uani 1 1 d . . . H21A H 0.8733 1.1138 0.3723 0.266 Uiso 1 1 calc R . . H21B H 0.8786 0.9981 0.3357 0.266 Uiso 1 1 calc R . . H21C H 0.9794 1.0596 0.3621 0.266 Uiso 1 1 calc R . . C22 C 0.6066(4) 0.1136(5) 0.2949(3) 0.0422(13) Uani 1 1 d . . . H29 H 0.5947 0.1714 0.3225 0.051 Uiso 1 1 calc R . . C23 C 0.5802(4) 0.0019(5) 0.2996(3) 0.0478(14) Uani 1 1 d . . . H30 H 0.5459 -0.0311 0.3299 0.057 Uiso 1 1 calc R . . C24 C 0.6565(4) 0.0275(4) 0.2188(2) 0.0373(12) Uani 1 1 d . . . H31 H 0.6849 0.0123 0.1830 0.045 Uiso 1 1 calc R . . C25 C 1.4066(4) 0.3233(4) 0.2646(3) 0.0531(16) Uani 1 1 d . . . H28A H 1.4723 0.3177 0.2882 0.064 Uiso 1 1 calc R . . H28B H 1.4106 0.2791 0.2279 0.064 Uiso 1 1 calc R . . C26 C 1.3262(4) 0.2693(5) 0.3000(3) 0.0474(14) Uani 1 1 d . . . H27A H 1.3223 0.3136 0.3367 0.057 Uiso 1 1 calc R . . H27B H 1.3473 0.1911 0.3115 0.057 Uiso 1 1 calc R . . C27 C 1.2204(4) 0.2642(4) 0.2658(2) 0.0367(12) Uani 1 1 d . . . H26A H 1.1975 0.3426 0.2559 0.044 Uiso 1 1 calc R . . H26B H 1.2243 0.2224 0.2283 0.044 Uiso 1 1 calc R . . C28 C 1.1435(4) 0.2055(5) 0.3014(2) 0.0395(12) Uani 1 1 d . . . H25A H 1.1697 0.1302 0.3150 0.047 Uiso 1 1 calc R . . H25B H 1.1342 0.2518 0.3368 0.047 Uiso 1 1 calc R . . C29 C 0.9236(4) 0.1220(5) 0.2029(3) 0.0495(15) Uani 1 1 d . . . H23 H 0.8872 0.0753 0.1744 0.059 Uiso 1 1 calc R . . C30 C 1.0207(4) 0.1037(5) 0.2261(3) 0.0455(14) Uani 1 1 d . . . H24 H 1.0630 0.0434 0.2164 0.055 Uiso 1 1 calc R . . C31 C 0.9630(4) 0.2582(4) 0.2658(2) 0.0351(11) Uani 1 1 d . . . H22 H 0.9601 0.3246 0.2893 0.042 Uiso 1 1 calc R . . C32 C 0.7491(6) 0.3000(6) 0.5654(3) 0.0583(17) Uani 1 1 d . . . H33 H 0.7979 0.2415 0.5707 0.070 Uiso 1 1 calc R . . C33 C 0.6374(5) 0.4160(7) 0.4985(3) 0.077(2) Uani 1 1 d . . . H32A H 0.6189 0.4233 0.4559 0.115 Uiso 1 1 calc R . . H32B H 0.6653 0.4882 0.5140 0.115 Uiso 1 1 calc R . . H32C H 0.5781 0.3969 0.5182 0.115 Uiso 1 1 calc R . . C34 C 0.7405(9) 0.2630(9) 0.4580(4) 0.122(4) Uani 1 1 d . . . H34A H 0.7054 0.2955 0.4221 0.183 Uiso 1 1 calc R . . H34B H 0.7220 0.1828 0.4613 0.183 Uiso 1 1 calc R . . H34C H 0.8128 0.2691 0.4561 0.183 Uiso 1 1 calc R . . N1 N 0.6132(3) -0.0538(4) 0.2514(2) 0.0400(11) Uani 1 1 d . . . N2 N 0.6539(3) 0.1302(3) 0.24338(19) 0.0346(9) Uani 1 1 d . . . N3 N 0.8869(3) 0.2208(3) 0.2282(2) 0.0367(10) Uani 1 1 d . . . N4 N 1.0449(3) 0.1899(3) 0.26633(19) 0.0352(10) Uani 1 1 d . . . N5 N 0.7127(5) 0.3252(5) 0.5094(2) 0.0610(15) Uani 1 1 d . . . O1 O 0.6188(3) 1.1094(3) 0.63643(17) 0.0479(10) Uani 1 1 d . . . O2 O 0.7814(3) 1.0643(3) 0.64587(17) 0.0468(10) Uani 1 1 d . . . O3 O 0.8045(3) 0.4302(3) 0.30070(19) 0.0506(10) Uani 1 1 d . . . O4 O 0.6414(3) 0.3976(3) 0.28057(18) 0.0500(10) Uani 1 1 d . . . O5 O 0.7242(4) 0.3469(4) 0.6106(2) 0.0647(12) Uani 1 1 d . . . Cd1 Cd 0.72882(3) 0.29621(3) 0.213369(16) 0.02984(13) 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 C1 0.030(3) 0.033(3) 0.038(3) 0.001(2) 0.009(2) 0.001(2) C2 0.030(3) 0.027(2) 0.032(3) 0.002(2) 0.005(2) 0.003(2) C3 0.033(3) 0.035(3) 0.038(3) -0.002(2) -0.003(2) 0.002(2) C4 0.027(3) 0.043(3) 0.042(3) -0.003(2) 0.003(2) 0.008(2) C5 0.041(3) 0.037(3) 0.047(3) -0.002(2) 0.006(3) 0.007(2) C6 0.041(3) 0.037(3) 0.048(3) -0.006(2) 0.012(3) 0.006(2) C7 0.048(3) 0.024(2) 0.038(3) 0.001(2) 0.006(2) 0.007(2) C8 0.043(3) 0.031(3) 0.042(3) -0.001(2) 0.007(2) 0.000(2) C9 0.035(3) 0.028(2) 0.043(3) -0.004(2) 0.008(2) 0.003(2) C10 0.035(3) 0.029(2) 0.036(3) -0.001(2) 0.002(2) 0.004(2) C11 0.039(3) 0.025(2) 0.038(3) 0.001(2) 0.009(2) 0.003(2) C12 0.034(3) 0.029(2) 0.034(3) -0.001(2) 0.004(2) 0.000(2) C13 0.036(3) 0.035(3) 0.052(3) -0.009(2) 0.013(3) -0.003(2) C14 0.057(4) 0.026(3) 0.030(3) 0.004(2) 0.006(3) 0.001(2) C15 0.032(3) 0.025(2) 0.036(3) 0.001(2) 0.007(2) -0.001(2) C16 0.039(3) 0.064(4) 0.062(4) -0.028(3) -0.006(3) 0.006(3) C17 0.050(4) 0.079(5) 0.050(4) -0.009(3) -0.001(3) 0.015(3) C18 0.084(6) 0.140(8) 0.058(5) 0.000(5) -0.005(4) 0.049(6) C19 0.110(7) 0.055(4) 0.138(7) -0.031(5) 0.094(6) -0.035(4) C20 1.20(9) 0.102(11) 0.53(4) 0.143(18) 0.74(5) 0.21(3) C21 0.33(2) 0.089(7) 0.135(9) 0.047(7) 0.138(12) 0.014(10) C22 0.041(3) 0.035(3) 0.052(3) 0.004(2) 0.016(3) 0.003(2) C23 0.041(3) 0.044(3) 0.061(4) 0.012(3) 0.017(3) 0.004(3) C24 0.031(3) 0.033(3) 0.048(3) 0.003(2) 0.004(2) 0.000(2) C25 0.035(3) 0.029(3) 0.096(5) -0.002(3) 0.014(3) 0.005(2) C26 0.036(3) 0.034(3) 0.070(4) 0.010(3) -0.005(3) 0.003(2) C27 0.032(3) 0.035(3) 0.043(3) 0.004(2) 0.003(2) 0.001(2) C28 0.031(3) 0.043(3) 0.044(3) 0.007(2) -0.001(2) 0.008(2) C29 0.041(3) 0.042(3) 0.066(4) -0.020(3) 0.006(3) -0.001(3) C30 0.034(3) 0.034(3) 0.070(4) -0.014(3) 0.012(3) 0.002(2) C31 0.036(3) 0.026(2) 0.044(3) -0.003(2) 0.005(2) 0.004(2) C32 0.075(5) 0.052(4) 0.049(4) 0.004(3) 0.011(3) 0.001(3) C33 0.066(5) 0.079(5) 0.083(5) 0.033(4) 0.000(4) -0.004(4) C34 0.199(13) 0.111(8) 0.063(6) -0.009(5) 0.048(7) 0.015(8) N1 0.026(2) 0.028(2) 0.067(3) 0.010(2) 0.010(2) 0.0012(18) N2 0.031(2) 0.028(2) 0.044(2) 0.0040(18) 0.0039(19) 0.0006(17) N3 0.033(2) 0.030(2) 0.047(3) -0.0052(19) 0.007(2) 0.0006(18) N4 0.032(2) 0.028(2) 0.046(2) 0.0046(18) 0.0032(19) 0.0020(17) N5 0.080(4) 0.060(3) 0.044(3) 0.009(2) 0.009(3) -0.005(3) O1 0.055(2) 0.042(2) 0.048(2) -0.0133(18) 0.0147(19) 0.0034(19) O2 0.056(3) 0.038(2) 0.045(2) -0.0109(17) -0.003(2) 0.0083(18) O3 0.035(2) 0.042(2) 0.077(3) -0.025(2) 0.017(2) -0.0056(17) O4 0.037(2) 0.055(2) 0.057(2) -0.024(2) 0.0001(19) -0.0006(18) O5 0.070(3) 0.072(3) 0.053(3) -0.009(2) 0.007(2) 0.010(3) Cd1 0.0270(2) 0.02576(19) 0.0369(2) 0.00176(15) 0.00391(14) -0.00029(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C12 1.389(7) . ? C1 C2 1.396(7) . ? C1 H6 0.9300 . ? C2 C3 1.401(7) . ? C2 C15 1.517(6) . ? C3 C4 1.381(7) . ? C3 H2 0.9300 . ? C4 C11 1.380(7) . ? C4 H3 0.9300 . ? C5 C10 1.379(7) . ? C5 C6 1.382(7) . ? C5 H8 0.9300 . ? C6 C7 1.385(7) . ? C6 H9 0.9300 . ? C7 C8 1.410(7) . ? C7 C14 1.504(7) . ? C8 C9 1.375(7) . ? C8 H11 0.9300 . ? C9 C10 1.401(7) . ? C9 C13 1.546(7) . ? C10 C11 1.473(7) . ? C11 C12 1.413(7) . ? C12 C13 1.507(7) . ? C13 C19 1.544(9) . ? C13 C16 1.544(8) . ? C14 O1 1.251(6) . ? C14 O2 1.259(6) . ? C14 Cd1 2.714(5) 4_576 ? C15 O3 1.237(6) . ? C15 O4 1.250(6) . ? C16 C17 1.472(9) . ? C16 H14A 0.9700 . ? C16 H14B 0.9700 . ? C17 C18 1.548(9) . ? C17 H15A 0.9700 . ? C17 H15B 0.9700 . ? C18 H16A 0.9600 . ? C18 H16B 0.9600 . ? C18 H16C 0.9600 . ? C19 C20 1.412(17) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.519(17) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.339(8) . ? C22 N2 1.373(7) . ? C22 H29 0.9300 . ? C23 N1 1.359(7) . ? C23 H30 0.9300 . ? C24 N2 1.306(6) . ? C24 N1 1.346(6) . ? C24 H31 0.9300 . ? C25 N1 1.476(7) 2_755 ? C25 C26 1.515(8) . ? C25 H28A 0.9700 . ? C25 H28B 0.9700 . ? C26 C27 1.522(7) . ? C26 H27A 0.9700 . ? C26 H27B 0.9700 . ? C27 C28 1.508(7) . ? C27 H26A 0.9700 . ? C27 H26B 0.9700 . ? C28 N4 1.460(6) . ? C28 H25A 0.9700 . ? C28 H25B 0.9700 . ? C29 C30 1.348(8) . ? C29 N3 1.379(6) . ? C29 H23 0.9300 . ? C30 N4 1.354(6) . ? C30 H24 0.9300 . ? C31 N3 1.314(6) . ? C31 N4 1.335(6) . ? C31 H22 0.9300 . ? C32 O5 1.215(7) . ? C32 N5 1.326(8) . ? C32 H33 0.9300 . ? C33 N5 1.446(9) . ? C33 H32A 0.9600 . ? C33 H32B 0.9600 . ? C33 H32C 0.9600 . ? C34 N5 1.429(9) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N1 C25 1.476(7) 2_745 ? N2 Cd1 2.282(4) . ? N3 Cd1 2.251(4) . ? O1 Cd1 2.395(4) 4_576 ? O2 Cd1 2.352(4) 4_576 ? O3 Cd1 2.605(4) . ? O4 Cd1 2.297(4) . ? Cd1 O2 2.352(4) 4_575 ? Cd1 O1 2.395(4) 4_575 ? Cd1 C14 2.714(5) 4_575 ? 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 C12 C1 C2 119.3(5) . . ? C12 C1 H6 120.3 . . ? C2 C1 H6 120.3 . . ? C1 C2 C3 120.2(4) . . ? C1 C2 C15 120.3(4) . . ? C3 C2 C15 119.5(4) . . ? C4 C3 C2 120.8(5) . . ? C4 C3 H2 119.6 . . ? C2 C3 H2 119.6 . . ? C3 C4 C11 118.9(5) . . ? C3 C4 H3 120.6 . . ? C11 C4 H3 120.6 . . ? C10 C5 C6 119.1(5) . . ? C10 C5 H8 120.4 . . ? C6 C5 H8 120.4 . . ? C5 C6 C7 120.7(5) . . ? C5 C6 H9 119.6 . . ? C7 C6 H9 119.6 . . ? C6 C7 C8 120.1(5) . . ? C6 C7 C14 120.0(5) . . ? C8 C7 C14 119.8(5) . . ? C9 C8 C7 119.1(5) . . ? C9 C8 H11 120.5 . . ? C7 C8 H11 120.5 . . ? C8 C9 C10 120.0(5) . . ? C8 C9 C13 129.6(5) . . ? C10 C9 C13 110.3(4) . . ? C5 C10 C9 121.0(5) . . ? C5 C10 C11 130.4(5) . . ? C9 C10 C11 108.5(4) . . ? C4 C11 C12 121.3(4) . . ? C4 C11 C10 130.6(5) . . ? C12 C11 C10 108.1(4) . . ? C1 C12 C11 119.3(5) . . ? C1 C12 C13 129.5(5) . . ? C11 C12 C13 111.1(4) . . ? C12 C13 C19 108.1(5) . . ? C12 C13 C16 113.9(4) . . ? C19 C13 C16 110.0(6) . . ? C12 C13 C9 101.1(4) . . ? C19 C13 C9 110.4(5) . . ? C16 C13 C9 113.0(5) . . ? O1 C14 O2 121.9(5) . . ? O1 C14 C7 119.6(5) . . ? O2 C14 C7 118.5(5) . . ? O1 C14 Cd1 62.0(3) . 4_576 ? O2 C14 Cd1 60.0(3) . 4_576 ? C7 C14 Cd1 177.6(4) . 4_576 ? O3 C15 O4 123.0(5) . . ? O3 C15 C2 119.0(4) . . ? O4 C15 C2 118.0(4) . . ? C17 C16 C13 116.6(5) . . ? C17 C16 H14A 108.1 . . ? C13 C16 H14A 108.1 . . ? C17 C16 H14B 108.1 . . ? C13 C16 H14B 108.1 . . ? H14A C16 H14B 107.3 . . ? C16 C17 C18 110.4(6) . . ? C16 C17 H15A 109.6 . . ? C18 C17 H15A 109.6 . . ? C16 C17 H15B 109.6 . . ? C18 C17 H15B 109.6 . . ? H15A C17 H15B 108.1 . . ? C17 C18 H16A 109.5 . . ? C17 C18 H16B 109.5 . . ? H16A C18 H16B 109.5 . . ? C17 C18 H16C 109.5 . . ? H16A C18 H16C 109.5 . . ? H16B C18 H16C 109.5 . . ? C20 C19 C13 131.9(10) . . ? C20 C19 H19A 104.3 . . ? C13 C19 H19A 104.3 . . ? C20 C19 H19B 104.3 . . ? C13 C19 H19B 104.3 . . ? H19A C19 H19B 105.6 . . ? C19 C20 C21 111.3(17) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 N2 110.0(5) . . ? C23 C22 H29 125.0 . . ? N2 C22 H29 125.0 . . ? C22 C23 N1 106.6(5) . . ? C22 C23 H30 126.7 . . ? N1 C23 H30 126.7 . . ? N2 C24 N1 111.8(5) . . ? N2 C24 H31 124.1 . . ? N1 C24 H31 124.1 . . ? N1 C25 C26 113.8(4) 2_755 . ? N1 C25 H28A 108.8 2_755 . ? C26 C25 H28A 108.8 . . ? N1 C25 H28B 108.8 2_755 . ? C26 C25 H28B 108.8 . . ? H28A C25 H28B 107.7 . . ? C25 C26 C27 114.1(5) . . ? C25 C26 H27A 108.7 . . ? C27 C26 H27A 108.7 . . ? C25 C26 H27B 108.7 . . ? C27 C26 H27B 108.7 . . ? H27A C26 H27B 107.6 . . ? C28 C27 C26 112.6(5) . . ? C28 C27 H26A 109.1 . . ? C26 C27 H26A 109.1 . . ? C28 C27 H26B 109.1 . . ? C26 C27 H26B 109.1 . . ? H26A C27 H26B 107.8 . . ? N4 C28 C27 112.4(4) . . ? N4 C28 H25A 109.1 . . ? C27 C28 H25A 109.1 . . ? N4 C28 H25B 109.1 . . ? C27 C28 H25B 109.1 . . ? H25A C28 H25B 107.8 . . ? C30 C29 N3 109.2(5) . . ? C30 C29 H23 125.4 . . ? N3 C29 H23 125.4 . . ? C29 C30 N4 107.0(5) . . ? C29 C30 H24 126.5 . . ? N4 C30 H24 126.5 . . ? N3 C31 N4 112.3(4) . . ? N3 C31 H22 123.9 . . ? N4 C31 H22 123.9 . . ? O5 C32 N5 125.5(7) . . ? O5 C32 H33 117.2 . . ? N5 C32 H33 117.2 . . ? N5 C33 H32A 109.5 . . ? N5 C33 H32B 109.5 . . ? H32A C33 H32B 109.5 . . ? N5 C33 H32C 109.5 . . ? H32A C33 H32C 109.5 . . ? H32B C33 H32C 109.5 . . ? N5 C34 H34A 109.5 . . ? N5 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N5 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C24 N1 C23 106.6(4) . . ? C24 N1 C25 127.6(5) . 2_745 ? C23 N1 C25 125.5(5) . 2_745 ? C24 N2 C22 105.0(4) . . ? C24 N2 Cd1 127.2(3) . . ? C22 N2 Cd1 127.4(3) . . ? C31 N3 C29 104.7(4) . . ? C31 N3 Cd1 127.2(3) . . ? C29 N3 Cd1 128.0(4) . . ? C31 N4 C30 106.7(4) . . ? C31 N4 C28 127.5(4) . . ? C30 N4 C28 125.8(4) . . ? C32 N5 C34 123.3(7) . . ? C32 N5 C33 119.7(6) . . ? C34 N5 C33 116.9(7) . . ? C14 O1 Cd1 90.6(3) . 4_576 ? C14 O2 Cd1 92.4(3) . 4_576 ? C15 O3 Cd1 84.8(3) . . ? C15 O4 Cd1 98.9(3) . . ? N3 Cd1 N2 93.13(14) . . ? N3 Cd1 O4 128.06(15) . . ? N2 Cd1 O4 88.57(15) . . ? N3 Cd1 O2 91.78(15) . 4_575 ? N2 Cd1 O2 157.38(14) . 4_575 ? O4 Cd1 O2 105.60(15) . 4_575 ? N3 Cd1 O1 140.04(14) . 4_575 ? N2 Cd1 O1 109.97(14) . 4_575 ? O4 Cd1 O1 85.96(14) . 4_575 ? O2 Cd1 O1 55.05(13) 4_575 4_575 ? N3 Cd1 O3 80.65(13) . . ? N2 Cd1 O3 114.95(14) . . ? O4 Cd1 O3 52.49(12) . . ? O2 Cd1 O3 87.64(13) 4_575 . ? O1 Cd1 O3 115.27(13) 4_575 . ? N3 Cd1 C14 117.09(17) . 4_575 ? N2 Cd1 C14 135.68(16) . 4_575 ? O4 Cd1 C14 95.79(15) . 4_575 ? O2 Cd1 C14 27.62(15) 4_575 4_575 ? O1 Cd1 C14 27.44(15) 4_575 4_575 ? O3 Cd1 C14 102.05(14) . 4_575 ? 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 C12 C1 C2 C3 2.5(7) . . . . ? C12 C1 C2 C15 -178.5(4) . . . . ? C1 C2 C3 C4 -3.5(7) . . . . ? C15 C2 C3 C4 177.6(4) . . . . ? C2 C3 C4 C11 0.4(8) . . . . ? C10 C5 C6 C7 -0.2(8) . . . . ? C5 C6 C7 C8 -0.6(8) . . . . ? C5 C6 C7 C14 178.2(5) . . . . ? C6 C7 C8 C9 0.6(7) . . . . ? C14 C7 C8 C9 -178.3(4) . . . . ? C7 C8 C9 C10 0.3(7) . . . . ? C7 C8 C9 C13 177.5(5) . . . . ? C6 C5 C10 C9 1.0(8) . . . . ? C6 C5 C10 C11 177.8(5) . . . . ? C8 C9 C10 C5 -1.1(8) . . . . ? C13 C9 C10 C5 -178.8(5) . . . . ? C8 C9 C10 C11 -178.4(5) . . . . ? C13 C9 C10 C11 3.8(6) . . . . ? C3 C4 C11 C12 3.6(8) . . . . ? C3 C4 C11 C10 -175.5(5) . . . . ? C5 C10 C11 C4 4.3(9) . . . . ? C9 C10 C11 C4 -178.7(5) . . . . ? C5 C10 C11 C12 -174.8(5) . . . . ? C9 C10 C11 C12 2.2(6) . . . . ? C2 C1 C12 C11 1.4(7) . . . . ? C2 C1 C12 C13 -175.8(5) . . . . ? C4 C11 C12 C1 -4.5(7) . . . . ? C10 C11 C12 C1 174.7(4) . . . . ? C4 C11 C12 C13 173.2(5) . . . . ? C10 C11 C12 C13 -7.6(6) . . . . ? C1 C12 C13 C19 70.7(7) . . . . ? C11 C12 C13 C19 -106.7(5) . . . . ? C1 C12 C13 C16 -51.9(7) . . . . ? C11 C12 C13 C16 130.8(5) . . . . ? C1 C12 C13 C9 -173.4(5) . . . . ? C11 C12 C13 C9 9.3(5) . . . . ? C8 C9 C13 C12 174.7(5) . . . . ? C10 C9 C13 C12 -7.8(5) . . . . ? C8 C9 C13 C19 -71.0(8) . . . . ? C10 C9 C13 C19 106.4(6) . . . . ? C8 C9 C13 C16 52.6(7) . . . . ? C10 C9 C13 C16 -129.9(5) . . . . ? C6 C7 C14 O1 -13.9(7) . . . . ? C8 C7 C14 O1 165.0(5) . . . . ? C6 C7 C14 O2 166.5(5) . . . . ? C8 C7 C14 O2 -14.6(7) . . . . ? C6 C7 C14 Cd1 116(10) . . . 4_576 ? C8 C7 C14 Cd1 -66(10) . . . 4_576 ? C1 C2 C15 O3 -2.1(7) . . . . ? C3 C2 C15 O3 176.9(5) . . . . ? C1 C2 C15 O4 178.3(5) . . . . ? C3 C2 C15 O4 -2.7(7) . . . . ? C12 C13 C16 C17 -52.1(7) . . . . ? C19 C13 C16 C17 -173.6(5) . . . . ? C9 C13 C16 C17 62.5(6) . . . . ? C13 C16 C17 C18 -176.7(5) . . . . ? C12 C13 C19 C20 166.0(15) . . . . ? C16 C13 C19 C20 -69.1(16) . . . . ? C9 C13 C19 C20 56.3(17) . . . . ? C13 C19 C20 C21 -165.2(10) . . . . ? N2 C22 C23 N1 1.5(7) . . . . ? N1 C25 C26 C27 63.0(7) 2_755 . . . ? C25 C26 C27 C28 177.6(5) . . . . ? C26 C27 C28 N4 -174.0(4) . . . . ? N3 C29 C30 N4 0.6(7) . . . . ? N2 C24 N1 C23 0.6(6) . . . . ? N2 C24 N1 C25 173.9(5) . . . 2_745 ? C22 C23 N1 C24 -1.3(6) . . . . ? C22 C23 N1 C25 -174.8(5) . . . 2_745 ? N1 C24 N2 C22 0.4(6) . . . . ? N1 C24 N2 Cd1 173.6(3) . . . . ? C23 C22 N2 C24 -1.2(6) . . . . ? C23 C22 N2 Cd1 -174.4(4) . . . . ? N4 C31 N3 C29 -0.3(6) . . . . ? N4 C31 N3 Cd1 176.2(3) . . . . ? C30 C29 N3 C31 -0.2(7) . . . . ? C30 C29 N3 Cd1 -176.7(4) . . . . ? N3 C31 N4 C30 0.7(6) . . . . ? N3 C31 N4 C28 178.7(5) . . . . ? C29 C30 N4 C31 -0.8(6) . . . . ? C29 C30 N4 C28 -178.8(5) . . . . ? C27 C28 N4 C31 -96.6(6) . . . . ? C27 C28 N4 C30 81.1(6) . . . . ? O5 C32 N5 C34 -176.5(8) . . . . ? O5 C32 N5 C33 0.5(11) . . . . ? O2 C14 O1 Cd1 -2.5(5) . . . 4_576 ? C7 C14 O1 Cd1 177.9(4) . . . 4_576 ? O1 C14 O2 Cd1 2.6(5) . . . 4_576 ? C7 C14 O2 Cd1 -177.8(4) . . . 4_576 ? O4 C15 O3 Cd1 8.8(5) . . . . ? C2 C15 O3 Cd1 -170.7(4) . . . . ? O3 C15 O4 Cd1 -10.1(6) . . . . ? C2 C15 O4 Cd1 169.5(3) . . . . ? C31 N3 Cd1 N2 -118.5(4) . . . . ? C29 N3 Cd1 N2 57.3(5) . . . . ? C31 N3 Cd1 O4 -27.9(5) . . . . ? C29 N3 Cd1 O4 147.9(4) . . . . ? C31 N3 Cd1 O2 83.6(4) . . . 4_575 ? C29 N3 Cd1 O2 -100.6(5) . . . 4_575 ? C31 N3 Cd1 O1 114.8(4) . . . 4_575 ? C29 N3 Cd1 O1 -69.4(5) . . . 4_575 ? C31 N3 Cd1 O3 -3.7(4) . . . . ? C29 N3 Cd1 O3 172.1(5) . . . . ? C31 N3 Cd1 C14 95.1(4) . . . 4_575 ? C29 N3 Cd1 C14 -89.1(5) . . . 4_575 ? C24 N2 Cd1 N3 -61.2(4) . . . . ? C22 N2 Cd1 N3 110.6(4) . . . . ? C24 N2 Cd1 O4 170.8(4) . . . . ? C22 N2 Cd1 O4 -17.4(4) . . . . ? C24 N2 Cd1 O2 41.0(6) . . . 4_575 ? C22 N2 Cd1 O2 -147.2(4) . . . 4_575 ? C24 N2 Cd1 O1 85.6(4) . . . 4_575 ? C22 N2 Cd1 O1 -102.6(4) . . . 4_575 ? C24 N2 Cd1 O3 -142.3(4) . . . . ? C22 N2 Cd1 O3 29.5(5) . . . . ? C24 N2 Cd1 C14 74.0(5) . . . 4_575 ? C22 N2 Cd1 C14 -114.2(4) . . . 4_575 ? C15 O4 Cd1 N3 35.7(4) . . . . ? C15 O4 Cd1 N2 128.5(3) . . . . ? C15 O4 Cd1 O2 -69.4(3) . . . 4_575 ? C15 O4 Cd1 O1 -121.4(3) . . . 4_575 ? C15 O4 Cd1 O3 5.1(3) . . . . ? C15 O4 Cd1 C14 -95.7(3) . . . 4_575 ? C15 O3 Cd1 N3 -161.1(3) . . . . ? C15 O3 Cd1 N2 -72.0(3) . . . . ? C15 O3 Cd1 O4 -5.1(3) . . . . ? C15 O3 Cd1 O2 106.7(3) . . . 4_575 ? C15 O3 Cd1 O1 57.5(3) . . . 4_575 ? C15 O3 Cd1 C14 83.0(3) . . . 4_575 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.744 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.107 #====END data_compound7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C31 H28 N2 O4 Zn' _chemical_formula_sum 'C31 H28 N2 O4 Zn' _chemical_formula_weight 557.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 27.347(5) _cell_length_b 8.637(5) _cell_length_c 10.972(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 103.309(5) _cell_angle_gamma 90.000(5) _cell_volume 2521.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3331 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 25.71 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6913 _exptl_absorpt_correction_T_max 0.7342 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean '9.00cm' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6686 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.71 _reflns_number_total 3331 _reflns_number_gt 2896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+12.3762P] 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 0.000(4) _refine_ls_number_reflns 3331 _refine_ls_number_parameters 313 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1660 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 Zn1 Zn 0.34241(4) 0.37883(8) 0.16607(8) 0.0317(3) Uani 1 1 d . . . O1 O 0.2627(3) 0.3988(7) -0.0324(7) 0.0485(17) Uani 1 1 d . . . O2 O 0.2885(2) 0.5318(7) 0.1431(6) 0.0396(15) Uani 1 1 d . . . O3 O -0.0914(2) 0.9659(7) -0.3610(6) 0.0417(15) Uani 1 1 d . . . O4 O -0.1013(2) 1.0626(8) -0.1838(6) 0.0407(14) Uani 1 1 d . . . N1 N 0.3078(3) 0.1986(9) 0.2440(8) 0.0317(17) Uani 1 1 d . . . N2 N 0.3667(3) 0.1848(10) 0.0859(8) 0.0352(19) Uani 1 1 d . . . C1 C 0.1724(3) 0.5765(9) -0.0906(8) 0.0306(18) Uani 1 1 d . . . H1 H 0.1797 0.5178 -0.1553 0.080 Uiso 1 1 calc . . . C2 C 0.2065(3) 0.5833(11) 0.0266(9) 0.0246(19) Uani 1 1 d . . . C3 C 0.1956(3) 0.6665(9) 0.1250(8) 0.0292(19) Uani 1 1 d . . . H3 H 0.2188 0.6717 0.2016 0.080 Uiso 1 1 calc . . . C4 C 0.1494(3) 0.7425(8) 0.1075(7) 0.0288(16) Uani 1 1 d . . . H4 H 0.1406 0.7932 0.1741 0.080 Uiso 1 1 calc . . . C5 C 0.0374(3) 0.8958(9) 0.0122(8) 0.0327(18) Uani 1 1 d . . . H5 H 0.0487 0.9148 0.0974 0.080 Uiso 1 1 calc . . . C6 C -0.0091(3) 0.9505(9) -0.0508(8) 0.0336(18) Uani 1 1 d . . . H6 H -0.0286 1.0081 -0.0081 0.080 Uiso 1 1 calc . . . C7 C -0.0266(4) 0.9205(13) -0.1757(10) 0.032(2) Uani 1 1 d . . . C8 C 0.0022(3) 0.8333(11) -0.2448(8) 0.0294(19) Uani 1 1 d . . . H8 H -0.0098 0.8135 -0.3297 0.080 Uiso 1 1 calc . . . C9 C 0.0852(4) 0.6737(17) -0.2253(11) 0.0725(19) Uani 1 1 d . . . C10 C 0.1275(3) 0.6597(11) -0.1081(8) 0.0278(19) Uani 1 1 d . . . C11 C 0.1166(3) 0.7418(9) -0.0098(8) 0.0266(18) Uani 1 1 d . . . C12 C 0.0666(3) 0.8145(10) -0.0496(9) 0.029(2) Uani 1 1 d . . . C13 C 0.0495(3) 0.7781(9) -0.1792(8) 0.0287(19) Uani 1 1 d . . . C14 C 0.2559(3) 0.4965(11) 0.0435(10) 0.035(2) Uani 1 1 d . . . C15 C -0.0762(3) 0.9874(11) -0.2467(9) 0.032(2) Uani 1 1 d . . . C16 C 0.1045(4) 0.7619(17) -0.3326(10) 0.0725(19) Uani 1 1 d . . . H16A H 0.0764 0.7601 -0.4050 0.080 Uiso 1 1 calc . . . H16B H 0.1083 0.8691 -0.3056 0.080 Uiso 1 1 calc . . . C17 C 0.1433(4) 0.7321(17) -0.3756(11) 0.0725(19) Uani 1 1 d . . . H17A H 0.1387 0.6306 -0.4144 0.080 Uiso 1 1 calc . . . H17B H 0.1721 0.7253 -0.3051 0.080 Uiso 1 1 calc . . . C18 C 0.1564(4) 0.8442(18) -0.4696(11) 0.0725(19) Uani 1 1 d . . . H18A H 0.1868 0.8113 -0.4913 0.080 Uiso 1 1 calc . . . H18B H 0.1610 0.9459 -0.4335 0.080 Uiso 1 1 calc . . . H18C H 0.1296 0.8463 -0.5435 0.080 Uiso 1 1 calc . . . C19 C 0.0607(4) 0.5179(13) -0.2686(11) 0.0628(17) Uani 1 1 d . . . H19A H 0.0857 0.4497 -0.2898 0.080 Uiso 1 1 calc . . . H19B H 0.0345 0.5336 -0.3438 0.080 Uiso 1 1 calc . . . C20 C 0.0379(5) 0.4391(13) -0.1685(11) 0.0628(17) Uani 1 1 d . . . H20A H 0.0652 0.4080 -0.0997 0.080 Uiso 1 1 calc . . . H20B H 0.0181 0.5155 -0.1362 0.080 Uiso 1 1 calc . . . C21 C 0.0066(5) 0.3063(13) -0.2081(11) 0.0628(17) Uani 1 1 d . . . H21A H -0.0057 0.2674 -0.1389 0.080 Uiso 1 1 calc . . . H21B H 0.0259 0.2273 -0.2370 0.080 Uiso 1 1 calc . . . H21C H -0.0212 0.3353 -0.2748 0.080 Uiso 1 1 calc . . . C22 C 0.2769(4) 0.2181(11) 0.3232(10) 0.042(2) Uani 1 1 d . . . H22 H 0.2694 0.3182 0.3445 0.080 Uiso 1 1 calc . . . C23 C 0.2566(4) 0.0986(12) 0.3721(10) 0.042(2) Uani 1 1 d . . . H23 H 0.2361 0.1163 0.4277 0.080 Uiso 1 1 calc . . . C24 C 0.2663(4) -0.0532(12) 0.3389(11) 0.047(3) Uani 1 1 d . . . H24 H 0.2522 -0.1372 0.3714 0.080 Uiso 1 1 calc . . . C25 C 0.2971(3) -0.0753(10) 0.2574(10) 0.037(2) Uani 1 1 d . . . H25 H 0.3040 -0.1749 0.2338 0.080 Uiso 1 1 calc . . . C26 C 0.3178(3) 0.0522(12) 0.2106(9) 0.034(2) Uani 1 1 d . . . C27 C 0.3530(3) 0.0503(11) 0.1241(9) 0.037(2) Uani 1 1 d . . . C28 C 0.3691(4) -0.0918(13) 0.0860(10) 0.048(3) Uani 1 1 d . . . H28 H 0.3595 -0.1860 0.1143 0.080 Uiso 1 1 calc . . . C29 C 0.4012(4) -0.0823(17) 0.0014(12) 0.063(4) Uani 1 1 d . . . H29 H 0.4136 -0.1727 -0.0265 0.080 Uiso 1 1 calc . . . C30 C 0.4141(4) 0.0562(17) -0.0390(12) 0.060(3) Uani 1 1 d . . . H30 H 0.4344 0.0613 -0.0963 0.080 Uiso 1 1 calc . . . C31 C 0.3967(4) 0.1907(14) 0.0056(10) 0.047(3) Uani 1 1 d . . . H31 H 0.4060 0.2863 -0.0209 0.080 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0174(4) 0.0338(4) 0.0405(5) 0.0030(5) -0.0006(3) -0.0002(5) O1 0.044(4) 0.053(4) 0.049(4) -0.002(3) 0.013(3) 0.018(3) O2 0.016(3) 0.037(3) 0.059(4) 0.005(3) -0.004(3) 0.007(2) O3 0.028(3) 0.057(4) 0.038(4) 0.003(3) 0.005(3) 0.007(3) O4 0.024(3) 0.051(3) 0.043(4) -0.006(3) 0.000(3) 0.012(3) N1 0.024(4) 0.037(4) 0.034(4) 0.002(3) 0.005(3) -0.001(3) N2 0.021(4) 0.050(5) 0.029(4) -0.002(4) -0.006(3) 0.002(3) C1 0.025(4) 0.030(4) 0.038(5) 0.004(3) 0.010(4) 0.003(3) C2 0.016(4) 0.029(4) 0.028(5) 0.009(4) 0.005(3) -0.002(3) C3 0.019(4) 0.024(4) 0.042(5) 0.009(4) 0.001(4) -0.006(3) C4 0.024(4) 0.028(4) 0.030(4) -0.002(3) -0.005(3) -0.006(3) C5 0.027(4) 0.035(4) 0.033(5) -0.007(4) 0.000(4) -0.004(3) C6 0.027(5) 0.035(4) 0.036(5) 0.003(4) 0.002(4) -0.002(4) C7 0.020(5) 0.038(5) 0.037(5) 0.001(4) 0.004(4) -0.003(4) C8 0.016(4) 0.044(4) 0.027(5) 0.010(4) 0.003(3) 0.003(3) C9 0.029(3) 0.137(6) 0.052(3) 0.038(4) 0.011(2) 0.014(3) C10 0.018(4) 0.047(5) 0.019(4) 0.010(4) 0.005(3) -0.001(4) C11 0.022(4) 0.024(4) 0.033(5) 0.014(4) 0.004(3) 0.004(3) C12 0.016(4) 0.028(4) 0.042(5) 0.008(4) 0.003(4) 0.002(3) C13 0.022(4) 0.029(4) 0.029(4) 0.011(3) -0.006(3) 0.007(3) C14 0.020(4) 0.039(5) 0.047(6) 0.013(4) 0.008(4) 0.001(4) C15 0.026(4) 0.032(4) 0.038(5) 0.005(4) 0.009(4) -0.003(4) C16 0.029(3) 0.137(6) 0.052(3) 0.038(4) 0.011(2) 0.014(3) C17 0.029(3) 0.137(6) 0.052(3) 0.038(4) 0.011(2) 0.014(3) C18 0.029(3) 0.137(6) 0.052(3) 0.038(4) 0.011(2) 0.014(3) C19 0.055(4) 0.063(4) 0.064(4) -0.025(3) -0.001(3) -0.008(3) C20 0.055(4) 0.063(4) 0.064(4) -0.025(3) -0.001(3) -0.008(3) C21 0.055(4) 0.063(4) 0.064(4) -0.025(3) -0.001(3) -0.008(3) C22 0.034(5) 0.037(5) 0.052(7) 0.000(4) 0.003(5) -0.001(4) C23 0.036(6) 0.049(5) 0.037(5) 0.004(4) 0.003(4) -0.003(4) C24 0.045(6) 0.044(5) 0.047(6) 0.010(5) -0.001(5) -0.021(5) C25 0.029(5) 0.028(4) 0.048(6) -0.001(4) -0.004(4) -0.004(4) C26 0.024(4) 0.045(5) 0.028(5) -0.002(4) -0.003(3) -0.005(4) C27 0.024(5) 0.036(5) 0.043(6) -0.010(4) -0.010(4) 0.015(4) C28 0.031(6) 0.060(6) 0.044(6) -0.014(5) -0.009(4) 0.013(5) C29 0.033(6) 0.090(9) 0.054(7) -0.033(7) -0.013(5) 0.031(6) C30 0.036(6) 0.081(9) 0.062(8) -0.033(7) 0.011(5) 0.004(6) C31 0.028(5) 0.078(7) 0.035(5) -0.010(5) 0.008(4) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.951(6) . ? Zn1 O4 2.043(6) 4_565 ? Zn1 N2 2.072(9) . ? Zn1 N1 2.103(8) . ? Zn1 O3 2.327(6) 4_565 ? Zn1 C15 2.495(9) 4_565 ? O1 C14 1.230(12) . ? O2 C14 1.279(12) . ? O3 C15 1.241(11) . ? O3 Zn1 2.326(6) 4_464 ? O4 C15 1.261(10) . ? O4 Zn1 2.043(6) 4_464 ? N1 C26 1.362(14) . ? N1 C22 1.356(12) . ? N2 C27 1.319(14) . ? N2 C31 1.335(12) . ? C1 C10 1.399(12) . ? C1 C2 1.404(13) . ? C1 H1 0.9300 . ? C2 C3 1.384(13) . ? C2 C14 1.519(12) . ? C3 C4 1.399(11) . ? C3 H3 0.9300 . ? C4 C11 1.388(11) . ? C4 H4 0.9300 . ? C5 C12 1.357(12) . ? C5 C6 1.383(12) . ? C5 H5 0.9300 . ? C6 C7 1.368(14) . ? C6 H6 0.9300 . ? C7 C8 1.428(13) . ? C7 C15 1.513(13) . ? C8 C13 1.412(11) . ? C8 H8 0.9300 . ? C9 C13 1.500(14) . ? C9 C10 1.523(14) . ? C9 C19 1.529(18) . ? C9 C16 1.591(14) . ? C10 C11 1.379(12) . ? C11 C12 1.477(11) . ? C12 C13 1.426(13) . ? C15 Zn1 2.495(9) 4_464 ? C16 C17 1.284(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.516(16) . ? C17 H17A 0.9699 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.542(16) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.437(15) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9601 . ? C22 C23 1.341(15) . ? C22 H22 0.9300 . ? C23 C24 1.402(15) . ? C23 H23 0.9300 . ? C24 C25 1.376(14) . ? C24 H24 0.9300 . ? C25 C26 1.389(13) . ? C25 H25 0.9300 . ? C26 C27 1.499(11) . ? C27 C28 1.401(14) . ? C28 C29 1.419(17) . ? C28 H28 0.9300 . ? C29 C30 1.35(2) . ? C29 H29 0.9300 . ? C30 C31 1.386(17) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O4 110.1(3) . 4_565 ? O2 Zn1 N2 143.1(3) . . ? O4 Zn1 N2 106.6(3) 4_565 . ? O2 Zn1 N1 99.0(3) . . ? O4 Zn1 N1 100.5(3) 4_565 . ? N2 Zn1 N1 78.0(3) . . ? O2 Zn1 O3 100.3(2) . 4_565 ? O4 Zn1 O3 59.7(2) 4_565 4_565 ? N2 Zn1 O3 94.4(3) . 4_565 ? N1 Zn1 O3 156.2(3) . 4_565 ? O2 Zn1 C15 108.4(3) . 4_565 ? O4 Zn1 C15 30.2(3) 4_565 4_565 ? N2 Zn1 C15 101.1(3) . 4_565 ? N1 Zn1 C15 129.2(3) . 4_565 ? O3 Zn1 C15 29.6(3) 4_565 4_565 ? C14 O2 Zn1 107.9(6) . . ? C15 O3 Zn1 82.8(5) . 4_464 ? C15 O4 Zn1 95.2(6) . 4_464 ? C26 N1 C22 118.8(8) . . ? C26 N1 Zn1 116.1(6) . . ? C22 N1 Zn1 125.0(7) . . ? C27 N2 C31 120.4(10) . . ? C27 N2 Zn1 115.8(7) . . ? C31 N2 Zn1 123.7(8) . . ? C10 C1 C2 118.7(8) . . ? C10 C1 H1 120.6 . . ? C2 C1 H1 120.6 . . ? C3 C2 C1 121.3(8) . . ? C3 C2 C14 120.3(8) . . ? C1 C2 C14 118.4(8) . . ? C2 C3 C4 119.1(8) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C11 C4 C3 119.6(7) . . ? C11 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C12 C5 C6 120.5(8) . . ? C12 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 120.4(8) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 121.5(9) . . ? C6 C7 C15 120.6(9) . . ? C8 C7 C15 117.8(9) . . ? C13 C8 C7 117.5(8) . . ? C13 C8 H8 121.3 . . ? C7 C8 H8 121.3 . . ? C13 C9 C10 100.9(9) . . ? C13 C9 C19 111.2(8) . . ? C10 C9 C19 112.7(10) . . ? C13 C9 C16 108.3(10) . . ? C10 C9 C16 110.2(8) . . ? C19 C9 C16 112.8(11) . . ? C11 C10 C1 119.8(8) . . ? C11 C10 C9 111.2(9) . . ? C1 C10 C9 129.0(9) . . ? C10 C11 C4 121.3(7) . . ? C10 C11 C12 109.8(8) . . ? C4 C11 C12 128.9(8) . . ? C5 C12 C13 121.1(8) . . ? C5 C12 C11 133.2(9) . . ? C13 C12 C11 105.7(8) . . ? C8 C13 C12 119.0(8) . . ? C8 C13 C9 128.5(9) . . ? C12 C13 C9 112.3(8) . . ? O1 C14 O2 123.9(9) . . ? O1 C14 C2 121.6(9) . . ? O2 C14 C2 114.4(8) . . ? O3 C15 O4 122.2(8) . . ? O3 C15 C7 121.0(8) . . ? O4 C15 C7 116.8(9) . . ? O3 C15 Zn1 67.7(5) . 4_464 ? O4 C15 Zn1 54.6(4) . 4_464 ? C7 C15 Zn1 171.1(7) . 4_464 ? C17 C16 C9 128.3(11) . . ? C17 C16 H16A 105.2 . . ? C9 C16 H16A 105.2 . . ? C17 C16 H16B 105.2 . . ? C9 C16 H16B 105.2 . . ? H16A C16 H16B 105.9 . . ? C16 C17 C18 117.8(12) . . ? C16 C17 H17A 107.9 . . ? C18 C17 H17A 107.9 . . ? C16 C17 H17B 107.8 . . ? C18 C17 H17B 107.8 . . ? H17A C17 H17B 107.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C9 C19 C20 112.8(9) . . ? C9 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? C9 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 116.6(10) . . ? C21 C20 H20A 108.1 . . ? C19 C20 H20A 108.1 . . ? C21 C20 H20B 108.1 . . ? C19 C20 H20B 108.1 . . ? H20A C20 H20B 107.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 N1 122.5(9) . . ? C23 C22 H22 118.8 . . ? N1 C22 H22 118.8 . . ? C22 C23 C24 119.7(9) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 118.6(9) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 119.5(9) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N1 C26 C25 120.8(8) . . ? N1 C26 C27 112.2(9) . . ? C25 C26 C27 127.0(10) . . ? N2 C27 C28 123.0(9) . . ? N2 C27 C26 117.6(9) . . ? C28 C27 C26 119.4(11) . . ? C27 C28 C29 115.5(11) . . ? C27 C28 H28 122.3 . . ? C29 C28 H28 122.3 . . ? C30 C29 C28 120.9(11) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.4(11) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? N2 C31 C30 120.9(11) . . ? N2 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? 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 O4 Zn1 O2 C14 175.6(5) 4_565 . . . ? N2 Zn1 O2 C14 2.3(8) . . . . ? N1 Zn1 O2 C14 -79.7(6) . . . . ? O3 Zn1 O2 C14 114.2(6) 4_565 . . . ? C15 Zn1 O2 C14 143.6(6) 4_565 . . . ? O2 Zn1 N1 C26 144.0(6) . . . . ? O4 Zn1 N1 C26 -103.5(6) 4_565 . . . ? N2 Zn1 N1 C26 1.5(7) . . . . ? O3 Zn1 N1 C26 -71.8(10) 4_565 . . . ? C15 Zn1 N1 C26 -93.1(7) 4_565 . . . ? O2 Zn1 N1 C22 -35.9(8) . . . . ? O4 Zn1 N1 C22 76.6(8) 4_565 . . . ? N2 Zn1 N1 C22 -178.4(8) . . . . ? O3 Zn1 N1 C22 108.2(9) 4_565 . . . ? C15 Zn1 N1 C22 87.0(8) 4_565 . . . ? O2 Zn1 N2 C27 -92.9(8) . . . . ? O4 Zn1 N2 C27 93.7(7) 4_565 . . . ? N1 Zn1 N2 C27 -3.8(7) . . . . ? O3 Zn1 N2 C27 153.4(6) 4_565 . . . ? C15 Zn1 N2 C27 124.3(7) 4_565 . . . ? O2 Zn1 N2 C31 90.5(9) . . . . ? O4 Zn1 N2 C31 -82.9(8) 4_565 . . . ? N1 Zn1 N2 C31 179.6(8) . . . . ? O3 Zn1 N2 C31 -23.2(8) 4_565 . . . ? C15 Zn1 N2 C31 -52.3(8) 4_565 . . . ? C10 C1 C2 C3 1.9(13) . . . . ? C10 C1 C2 C14 -178.2(8) . . . . ? C1 C2 C3 C4 1.3(12) . . . . ? C14 C2 C3 C4 -178.6(7) . . . . ? C2 C3 C4 C11 -4.2(11) . . . . ? C12 C5 C6 C7 1.4(13) . . . . ? C5 C6 C7 C8 -0.3(14) . . . . ? C5 C6 C7 C15 -176.6(8) . . . . ? C6 C7 C8 C13 0.3(14) . . . . ? C15 C7 C8 C13 176.8(8) . . . . ? C2 C1 C10 C11 -2.3(12) . . . . ? C2 C1 C10 C9 178.9(10) . . . . ? C13 C9 C10 C11 1.1(11) . . . . ? C19 C9 C10 C11 -117.6(10) . . . . ? C16 C9 C10 C11 115.4(10) . . . . ? C13 C9 C10 C1 -180.0(9) . . . . ? C19 C9 C10 C1 61.3(13) . . . . ? C16 C9 C10 C1 -65.7(16) . . . . ? C1 C10 C11 C4 -0.6(12) . . . . ? C9 C10 C11 C4 178.4(8) . . . . ? C1 C10 C11 C12 -177.8(6) . . . . ? C9 C10 C11 C12 1.2(12) . . . . ? C3 C4 C11 C10 3.9(11) . . . . ? C3 C4 C11 C12 -179.5(7) . . . . ? C6 C5 C12 C13 -2.5(13) . . . . ? C6 C5 C12 C11 -179.7(8) . . . . ? C10 C11 C12 C5 174.3(8) . . . . ? C4 C11 C12 C5 -2.6(15) . . . . ? C10 C11 C12 C13 -3.1(11) . . . . ? C4 C11 C12 C13 180.0(7) . . . . ? C7 C8 C13 C12 -1.4(13) . . . . ? C7 C8 C13 C9 174.4(9) . . . . ? C5 C12 C13 C8 2.5(13) . . . . ? C11 C12 C13 C8 -179.6(7) . . . . ? C5 C12 C13 C9 -173.9(9) . . . . ? C11 C12 C13 C9 3.9(11) . . . . ? C10 C9 C13 C8 -179.1(9) . . . . ? C19 C9 C13 C8 -59.4(13) . . . . ? C16 C9 C13 C8 65.1(14) . . . . ? C10 C9 C13 C12 -3.1(10) . . . . ? C19 C9 C13 C12 116.6(10) . . . . ? C16 C9 C13 C12 -118.9(9) . . . . ? Zn1 O2 C14 O1 -10.9(11) . . . . ? Zn1 O2 C14 C2 167.8(6) . . . . ? C3 C2 C14 O1 165.8(8) . . . . ? C1 C2 C14 O1 -14.0(13) . . . . ? C3 C2 C14 O2 -12.9(12) . . . . ? C1 C2 C14 O2 167.2(8) . . . . ? Zn1 O3 C15 O4 3.3(8) 4_464 . . . ? Zn1 O3 C15 C7 -178.1(8) 4_464 . . . ? Zn1 O4 C15 O3 -3.7(9) 4_464 . . . ? Zn1 O4 C15 C7 177.6(7) 4_464 . . . ? C6 C7 C15 O3 177.1(9) . . . . ? C8 C7 C15 O3 0.6(14) . . . . ? C6 C7 C15 O4 -4.2(13) . . . . ? C8 C7 C15 O4 179.3(8) . . . . ? C6 C7 C15 Zn1 8(5) . . . 4_464 ? C8 C7 C15 Zn1 -168(4) . . . 4_464 ? C13 C9 C16 C17 161.7(14) . . . . ? C10 C9 C16 C17 52(2) . . . . ? C19 C9 C16 C17 -74.7(17) . . . . ? C9 C16 C17 C18 -174.0(13) . . . . ? C13 C9 C19 C20 -53.0(12) . . . . ? C10 C9 C19 C20 59.5(12) . . . . ? C16 C9 C19 C20 -174.9(9) . . . . ? C9 C19 C20 C21 169.5(11) . . . . ? C26 N1 C22 C23 1.4(14) . . . . ? Zn1 N1 C22 C23 -178.7(8) . . . . ? N1 C22 C23 C24 -1.5(16) . . . . ? C22 C23 C24 C25 0.7(16) . . . . ? C23 C24 C25 C26 0.2(15) . . . . ? C22 N1 C26 C25 -0.5(13) . . . . ? Zn1 N1 C26 C25 179.6(7) . . . . ? C22 N1 C26 C27 -179.3(8) . . . . ? Zn1 N1 C26 C27 0.7(9) . . . . ? C24 C25 C26 N1 -0.3(14) . . . . ? C24 C25 C26 C27 178.3(9) . . . . ? C31 N2 C27 C28 1.3(14) . . . . ? Zn1 N2 C27 C28 -175.4(8) . . . . ? C31 N2 C27 C26 -177.8(8) . . . . ? Zn1 N2 C27 C26 5.5(10) . . . . ? N1 C26 C27 N2 -4.1(10) . . . . ? C25 C26 C27 N2 177.1(9) . . . . ? N1 C26 C27 C28 176.7(9) . . . . ? C25 C26 C27 C28 -2.0(13) . . . . ? N2 C27 C28 C29 -0.8(14) . . . . ? C26 C27 C28 C29 178.3(8) . . . . ? C27 C28 C29 C30 -0.8(16) . . . . ? C28 C29 C30 C31 1.8(18) . . . . ? C27 N2 C31 C30 -0.3(14) . . . . ? Zn1 N2 C31 C30 176.1(8) . . . . ? C29 C30 C31 N2 -1.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.302 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.108 #====END