# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1686 data_ifn20m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 Cd Cl2 N6 O10' _chemical_formula_weight 783.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.7260(5) _cell_length_b 10.5384(6) _cell_length_c 34.657(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3187.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.917 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.7456 _exptl_absorpt_correction_T_max 0.8167 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21043 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 28.91 _reflns_number_total 7601 _reflns_number_gt 6621 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.040(19) _refine_ls_number_reflns 7601 _refine_ls_number_parameters 445 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.42974(2) 0.40822(2) 0.370097(6) 0.03826(7) Uani 1 1 d . . . N1 N 0.2648(3) 0.2606(2) 0.34218(8) 0.0357(5) Uani 1 1 d . . . N2 N 0.5176(3) 0.3591(2) 0.30547(8) 0.0403(6) Uani 1 1 d . . . H2 H 0.4656 0.4125 0.2895 0.048 Uiso 1 1 calc R . . N3 N 0.5012(3) 0.5564(3) 0.41821(8) 0.0449(6) Uani 1 1 d . . . H3 H 0.4115 0.5912 0.4265 0.054 Uiso 1 1 calc R . . N4 N 0.2083(3) 0.3500(3) 0.41629(8) 0.0403(6) Uani 1 1 d . . . H4 H 0.1805 0.4208 0.4296 0.048 Uiso 1 1 calc R . . N5 N 0.6034(4) 0.2444(3) 0.39368(10) 0.0563(8) Uani 1 1 d . . . N6 N 0.2855(4) 0.5822(3) 0.34306(10) 0.0586(8) Uani 1 1 d . . . C1 C 0.3089(4) 0.2043(3) 0.30918(9) 0.0390(7) Uani 1 1 d . . . C2 C 0.2122(4) 0.1217(3) 0.29026(10) 0.0459(8) Uani 1 1 d . . . H2A H 0.2433 0.0833 0.2674 0.055 Uiso 1 1 calc R . . C3 C 0.0701(4) 0.0961(3) 0.30520(9) 0.0480(7) Uani 1 1 d . . . H3A H 0.0042 0.0401 0.2927 0.058 Uiso 1 1 calc R . . C4 C 0.0261(4) 0.1546(3) 0.33907(10) 0.0451(8) Uani 1 1 d . . . H4A H -0.0697 0.1384 0.3498 0.054 Uiso 1 1 calc R . . C5 C 0.1252(3) 0.2371(3) 0.35674(9) 0.0376(7) Uani 1 1 d . . . C6 C 0.0793(4) 0.3096(3) 0.39260(9) 0.0431(7) Uani 1 1 d . . . H6A H 0.0212 0.3839 0.3850 0.052 Uiso 1 1 calc R . . H6B H 0.0125 0.2564 0.4081 0.052 Uiso 1 1 calc R . . C7 C 0.2709(4) 0.2602(3) 0.44288(9) 0.0399(7) Uani 1 1 d . . . C8 C 0.2680(4) 0.1307(3) 0.43737(12) 0.0497(8) Uani 1 1 d . . . H8 H 0.2181 0.0964 0.4161 0.060 Uiso 1 1 calc R . . C9 C 0.3405(5) 0.0518(4) 0.46388(14) 0.0622(11) Uani 1 1 d . . . H9 H 0.3361 -0.0357 0.4605 0.075 Uiso 1 1 calc R . . C10 C 0.4167(5) 0.0996(4) 0.49426(12) 0.0677(10) Uani 1 1 d . . . H10 H 0.4688 0.0457 0.5110 0.081 Uiso 1 1 calc R . . C11 C 0.4176(5) 0.2291(4) 0.50060(11) 0.0610(9) Uani 1 1 d . . . H11 H 0.4672 0.2623 0.5221 0.073 Uiso 1 1 calc R . . C12 C 0.3448(4) 0.3089(3) 0.47505(10) 0.0460(8) Uani 1 1 d . . . C13 C 0.4707(5) 0.5079(4) 0.48773(12) 0.0613(11) Uani 1 1 d . . . H13A H 0.5226 0.4713 0.5098 0.074 Uiso 1 1 calc R . . H13B H 0.4454 0.5951 0.4940 0.074 Uiso 1 1 calc R . . C14 C 0.5761(5) 0.5059(4) 0.45377(10) 0.0538(8) Uani 1 1 d . . . H14A H 0.6661 0.5565 0.4595 0.065 Uiso 1 1 calc R . . H14B H 0.6095 0.4195 0.4491 0.065 Uiso 1 1 calc R . . C15 C 0.5874(5) 0.6627(3) 0.40083(11) 0.0540(9) Uani 1 1 d . . . H15A H 0.6254 0.7178 0.4211 0.065 Uiso 1 1 calc R . . H15B H 0.5195 0.7121 0.3845 0.065 Uiso 1 1 calc R . . C16 C 0.7201(4) 0.6150(3) 0.37719(12) 0.0570(10) Uani 1 1 d . . . H16A H 0.7753 0.6852 0.3656 0.068 Uiso 1 1 calc R . . H16B H 0.7905 0.5667 0.3931 0.068 Uiso 1 1 calc R . . C17 C 0.7471(4) 0.4778(3) 0.32107(11) 0.0468(8) Uani 1 1 d . . . C18 C 0.9016(4) 0.5098(4) 0.31623(12) 0.0590(10) Uani 1 1 d . . . H18 H 0.9470 0.5725 0.3312 0.071 Uiso 1 1 calc R . . C19 C 0.9851(4) 0.4451(5) 0.28837(13) 0.0643(12) Uani 1 1 d . . . H19 H 1.0875 0.4659 0.2846 0.077 Uiso 1 1 calc R . . C20 C 0.9208(5) 0.3519(4) 0.26650(12) 0.0608(10) Uani 1 1 d . . . H20 H 0.9792 0.3092 0.2482 0.073 Uiso 1 1 calc R . . C21 C 0.7652(4) 0.3204(4) 0.27172(11) 0.0554(9) Uani 1 1 d . . . H21 H 0.7208 0.2565 0.2570 0.066 Uiso 1 1 calc R . . C22 C 0.6789(4) 0.3849(3) 0.29880(10) 0.0432(7) Uani 1 1 d . . . C23 C 0.4671(4) 0.2308(3) 0.29505(11) 0.0464(8) Uani 1 1 d . . . H23A H 0.5372 0.1692 0.3060 0.056 Uiso 1 1 calc R . . H23B H 0.4698 0.2215 0.2672 0.056 Uiso 1 1 calc R . . C24 C 0.6503(4) 0.1521(4) 0.40502(12) 0.0534(9) Uani 1 1 d . . . C25 C 0.7121(6) 0.0353(4) 0.42065(15) 0.0767(13) Uani 1 1 d . . . H25A H 0.8171 0.0481 0.4279 0.115 Uiso 1 1 calc R . . H25B H 0.7064 -0.0303 0.4015 0.115 Uiso 1 1 calc R . . H25C H 0.6538 0.0106 0.4429 0.115 Uiso 1 1 calc R . . C26 C 0.2446(4) 0.6835(4) 0.34114(12) 0.0529(9) Uani 1 1 d . . . C27 C 0.1890(6) 0.8131(4) 0.33965(16) 0.0811(14) Uani 1 1 d . . . H27A H 0.0911 0.8150 0.3270 0.122 Uiso 1 1 calc R . . H27B H 0.2604 0.8646 0.3255 0.122 Uiso 1 1 calc R . . H27C H 0.1788 0.8455 0.3654 0.122 Uiso 1 1 calc R . . O1 O 0.3314(3) 0.4382(2) 0.48046(7) 0.0535(6) Uani 1 1 d . . . O2 O 0.6530(3) 0.5353(2) 0.34784(8) 0.0522(6) Uani 1 1 d . . . O3A O 0.7833(16) 0.8073(11) 0.2968(4) 0.123(5) Uani 0.601(16) 1 d PU A 1 O5A O 0.5275(11) 0.8448(19) 0.3047(4) 0.163(6) Uani 0.601(16) 1 d PU A 1 O6A O 0.7034(16) 0.9796(9) 0.3302(3) 0.113(4) Uani 0.601(16) 1 d PU A 1 O3B O 0.8056(15) 0.878(2) 0.3177(6) 0.133(7) Uani 0.399(16) 1 d PU A 2 O5B O 0.586(3) 0.7733(12) 0.2983(4) 0.128(7) Uani 0.399(16) 1 d PU A 2 O6B O 0.576(3) 0.9553(14) 0.3323(3) 0.122(7) Uani 0.399(16) 1 d PU A 2 O4 O 0.6633(5) 0.9663(3) 0.26589(10) 0.0940(12) Uani 1 1 d . A . O7 O -0.0078(5) 0.8114(4) 0.42872(13) 0.1147(15) Uani 1 1 d . . . O8 O 0.2394(5) 0.7407(4) 0.43578(16) 0.1175(16) Uani 1 1 d . . . O9 O 0.0738(8) 0.7082(4) 0.48430(11) 0.1353(19) Uani 1 1 d . . . O10 O 0.0522(4) 0.5954(3) 0.42657(11) 0.0929(10) Uani 1 1 d . . . Cl1 Cl 0.66444(11) 0.89504(10) 0.30045(3) 0.0586(2) Uani 1 1 d . . . Cl2 Cl 0.08275(13) 0.71438(8) 0.44384(3) 0.0595(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03881(10) 0.03520(10) 0.04077(11) -0.00110(9) -0.00246(10) -0.00313(10) N1 0.0381(13) 0.0339(12) 0.0350(13) -0.0009(10) -0.0036(10) -0.0016(10) N2 0.0397(14) 0.0385(13) 0.0426(15) 0.0067(11) 0.0025(11) 0.0023(11) N3 0.0469(14) 0.0410(15) 0.0467(16) -0.0007(11) -0.0078(12) -0.0040(12) N4 0.0452(15) 0.0424(14) 0.0333(14) -0.0051(11) -0.0038(11) 0.0016(12) N5 0.057(2) 0.0518(18) 0.060(2) 0.0034(14) -0.0021(15) 0.0080(14) N6 0.0525(17) 0.0509(19) 0.072(2) 0.0068(17) -0.0118(15) 0.0028(16) C1 0.0443(16) 0.0330(15) 0.0397(17) -0.0029(12) 0.0002(13) 0.0017(13) C2 0.0572(19) 0.0393(18) 0.0412(18) -0.0080(13) -0.0007(15) -0.0014(14) C3 0.0575(17) 0.0400(14) 0.0464(17) -0.0066(14) -0.0071(16) -0.011(2) C4 0.0442(18) 0.0489(18) 0.0420(18) 0.0027(14) -0.0034(13) -0.0114(14) C5 0.0388(15) 0.0391(16) 0.0348(15) 0.0025(12) -0.0038(12) -0.0021(12) C6 0.0366(15) 0.0500(16) 0.0428(17) -0.0053(13) -0.0027(15) -0.0035(15) C7 0.0405(16) 0.0449(17) 0.0343(16) 0.0002(13) 0.0036(13) 0.0008(13) C8 0.0500(19) 0.0480(19) 0.051(2) 0.0038(15) 0.0077(16) -0.0054(15) C9 0.064(2) 0.048(2) 0.075(3) 0.0152(19) 0.007(2) -0.0010(17) C10 0.062(2) 0.075(3) 0.065(2) 0.028(2) -0.009(2) -0.008(3) C11 0.064(2) 0.074(2) 0.0444(19) 0.0082(17) -0.011(2) -0.004(2) C12 0.0427(18) 0.054(2) 0.0412(18) -0.0001(15) 0.0004(14) -0.0036(15) C13 0.075(3) 0.064(2) 0.044(2) -0.0117(18) -0.0164(18) -0.011(2) C14 0.054(2) 0.0572(19) 0.050(2) -0.0004(15) -0.0120(19) -0.0050(19) C15 0.065(2) 0.0369(16) 0.060(2) -0.0052(14) -0.008(2) -0.0088(17) C16 0.0538(19) 0.048(2) 0.069(3) 0.0013(17) -0.0075(17) -0.0185(16) C17 0.0374(16) 0.0510(19) 0.052(2) 0.0132(16) 0.0014(15) 0.0010(14) C18 0.041(2) 0.072(2) 0.064(2) 0.023(2) -0.0049(17) -0.0075(18) C19 0.0368(17) 0.088(3) 0.068(3) 0.035(2) 0.0053(18) 0.0063(19) C20 0.0479(19) 0.075(2) 0.059(2) 0.0239(19) 0.0122(19) 0.015(2) C21 0.050(2) 0.065(2) 0.052(2) 0.0119(18) 0.0066(17) 0.0094(18) C22 0.0371(15) 0.048(2) 0.0442(18) 0.0134(14) 0.0021(13) 0.0012(13) C23 0.0464(19) 0.0473(17) 0.0455(18) -0.0080(15) 0.0055(14) 0.0013(14) C24 0.053(2) 0.052(2) 0.054(2) -0.0009(17) -0.0016(17) 0.0089(17) C25 0.091(3) 0.058(2) 0.081(3) 0.013(2) 0.003(3) 0.025(2) C26 0.050(2) 0.053(2) 0.056(2) 0.0070(17) -0.0044(17) -0.0019(17) C27 0.095(4) 0.057(3) 0.091(4) 0.021(2) 0.003(3) 0.022(3) O1 0.0602(15) 0.0560(15) 0.0442(14) -0.0113(11) -0.0091(11) -0.0031(12) O2 0.0443(13) 0.0547(14) 0.0577(16) -0.0056(12) 0.0012(11) -0.0142(11) O3A 0.141(9) 0.105(7) 0.123(8) 0.040(5) 0.057(7) 0.068(6) O5A 0.079(6) 0.259(16) 0.151(9) 0.007(11) 0.017(5) -0.099(8) O6A 0.144(9) 0.108(6) 0.087(5) -0.039(4) -0.036(6) -0.013(6) O3B 0.059(6) 0.175(17) 0.166(15) 0.066(13) -0.028(8) -0.025(9) O5B 0.22(2) 0.075(7) 0.085(8) 0.015(6) -0.030(11) -0.056(9) O6B 0.193(17) 0.110(9) 0.062(6) -0.004(5) 0.027(9) 0.031(11) O4 0.141(3) 0.076(2) 0.065(2) 0.0074(17) -0.006(2) -0.001(2) O7 0.141(4) 0.085(3) 0.118(3) -0.006(2) -0.022(3) 0.060(3) O8 0.082(3) 0.098(3) 0.172(5) -0.023(3) 0.002(3) -0.010(2) O9 0.230(5) 0.106(3) 0.070(2) -0.012(2) 0.024(3) 0.052(4) O10 0.110(3) 0.0632(17) 0.106(3) -0.0271(18) -0.023(2) 0.010(2) Cl1 0.0591(5) 0.0574(5) 0.0592(5) -0.0039(5) -0.0002(4) 0.0002(4) Cl2 0.0672(6) 0.0452(4) 0.0661(6) -0.0097(4) 0.0034(5) 0.0089(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.330(3) . ? Cd1 N3 2.368(3) . ? Cd1 N6 2.413(3) . ? Cd1 N2 2.423(3) . ? Cd1 N5 2.438(3) . ? Cd1 O2 2.486(2) . ? Cd1 N4 2.583(3) . ? N1 C5 1.341(4) . ? N1 C1 1.345(4) . ? N2 C22 1.452(4) . ? N2 C23 1.467(4) . ? N3 C15 1.478(4) . ? N3 C14 1.493(4) . ? N4 C7 1.429(4) . ? N4 C6 1.457(4) . ? N5 C24 1.126(5) . ? N6 C26 1.127(5) . ? C1 C2 1.379(4) . ? C1 C23 1.491(5) . ? C2 C3 1.371(5) . ? C3 C4 1.381(5) . ? C4 C5 1.371(4) . ? C5 C6 1.513(4) . ? C7 C8 1.378(5) . ? C7 C12 1.386(5) . ? C8 C9 1.392(6) . ? C9 C10 1.344(6) . ? C10 C11 1.383(6) . ? C11 C12 1.376(5) . ? C12 O1 1.381(5) . ? C13 O1 1.442(5) . ? C13 C14 1.494(6) . ? C15 C16 1.505(6) . ? C16 O2 1.443(4) . ? C17 O2 1.379(4) . ? C17 C22 1.381(5) . ? C17 C18 1.400(5) . ? C18 C19 1.389(6) . ? C19 C20 1.362(7) . ? C20 C21 1.409(6) . ? C21 C22 1.382(5) . ? C24 C25 1.449(5) . ? C26 C27 1.450(6) . ? O3A Cl1 1.395(8) . ? O5A Cl1 1.316(8) . ? O6A Cl1 1.404(7) . ? O3B Cl1 1.381(12) . ? O5B Cl1 1.455(13) . ? O6B Cl1 1.489(12) . ? O4 Cl1 1.414(4) . ? O7 Cl2 1.395(4) . ? O8 Cl2 1.423(4) . ? O9 Cl2 1.406(4) . ? O10 Cl2 1.415(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N3 153.55(10) . . ? N1 Cd1 N6 91.35(10) . . ? N3 Cd1 N6 84.82(11) . . ? N1 Cd1 N2 70.67(9) . . ? N3 Cd1 N2 135.11(10) . . ? N6 Cd1 N2 88.20(11) . . ? N1 Cd1 N5 92.89(10) . . ? N3 Cd1 N5 93.87(10) . . ? N6 Cd1 N5 172.88(12) . . ? N2 Cd1 N5 87.81(10) . . ? N1 Cd1 O2 135.63(9) . . ? N3 Cd1 O2 69.95(9) . . ? N6 Cd1 O2 83.05(10) . . ? N2 Cd1 O2 65.20(9) . . ? N5 Cd1 O2 89.92(10) . . ? N1 Cd1 N4 68.69(9) . . ? N3 Cd1 N4 85.25(9) . . ? N6 Cd1 N4 91.77(11) . . ? N2 Cd1 N4 139.34(9) . . ? N5 Cd1 N4 95.09(10) . . ? O2 Cd1 N4 154.99(8) . . ? C5 N1 C1 119.9(3) . . ? C5 N1 Cd1 121.9(2) . . ? C1 N1 Cd1 118.1(2) . . ? C22 N2 C23 115.2(3) . . ? C22 N2 Cd1 114.4(2) . . ? C23 N2 Cd1 109.2(2) . . ? C15 N3 C14 112.5(3) . . ? C15 N3 Cd1 110.3(2) . . ? C14 N3 Cd1 117.5(2) . . ? C7 N4 C6 117.7(3) . . ? C7 N4 Cd1 105.73(19) . . ? C6 N4 Cd1 107.36(19) . . ? C24 N5 Cd1 162.7(3) . . ? C26 N6 Cd1 155.1(3) . . ? N1 C1 C2 120.5(3) . . ? N1 C1 C23 117.5(3) . . ? C2 C1 C23 121.9(3) . . ? C3 C2 C1 119.9(3) . . ? C2 C3 C4 119.0(3) . . ? C5 C4 C3 119.2(3) . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 117.2(3) . . ? C4 C5 C6 121.3(3) . . ? N4 C6 C5 113.9(3) . . ? C8 C7 C12 119.1(3) . . ? C8 C7 N4 124.0(3) . . ? C12 C7 N4 116.9(3) . . ? C7 C8 C9 119.5(4) . . ? C10 C9 C8 121.2(4) . . ? C9 C10 C11 119.8(4) . . ? C12 C11 C10 119.9(4) . . ? C11 C12 O1 123.7(3) . . ? C11 C12 C7 120.4(3) . . ? O1 C12 C7 115.8(3) . . ? O1 C13 C14 112.0(3) . . ? N3 C14 C13 112.1(3) . . ? N3 C15 C16 111.1(3) . . ? O2 C16 C15 105.4(3) . . ? O2 C17 C22 115.5(3) . . ? O2 C17 C18 123.3(4) . . ? C22 C17 C18 121.2(4) . . ? C19 C18 C17 118.1(4) . . ? C20 C19 C18 121.7(4) . . ? C19 C20 C21 119.7(4) . . ? C22 C21 C20 119.8(4) . . ? C17 C22 C21 119.6(3) . . ? C17 C22 N2 117.5(3) . . ? C21 C22 N2 122.9(3) . . ? N2 C23 C1 111.7(3) . . ? N5 C24 C25 178.3(5) . . ? N6 C26 C27 178.3(5) . . ? C12 O1 C13 117.0(3) . . ? C17 O2 C16 119.2(3) . . ? C17 O2 Cd1 116.0(2) . . ? C16 O2 Cd1 114.4(2) . . ? O5A Cl1 O3B 135.2(9) . . ? O5A Cl1 O3A 114.7(8) . . ? O3B Cl1 O3A 44.6(8) . . ? O5A Cl1 O6A 113.2(8) . . ? O3B Cl1 O6A 63.3(10) . . ? O3A Cl1 O6A 107.9(7) . . ? O5A Cl1 O4 107.6(7) . . ? O3B Cl1 O4 116.3(7) . . ? O3A Cl1 O4 106.3(4) . . ? O6A Cl1 O4 106.6(5) . . ? O5A Cl1 O5B 39.1(9) . . ? O3B Cl1 O5B 108.8(10) . . ? O3A Cl1 O5B 76.1(9) . . ? O6A Cl1 O5B 135.2(7) . . ? O4 Cl1 O5B 115.0(6) . . ? O5A Cl1 O6B 67.5(9) . . ? O3B Cl1 O6B 101.5(10) . . ? O3A Cl1 O6B 137.4(7) . . ? O6A Cl1 O6B 46.5(7) . . ? O4 Cl1 O6B 113.4(5) . . ? O5B Cl1 O6B 99.8(10) . . ? O7 Cl2 O9 112.2(3) . . ? O7 Cl2 O10 112.6(2) . . ? O9 Cl2 O10 111.7(3) . . ? O7 Cl2 O8 109.1(3) . . ? O9 Cl2 O8 105.0(4) . . ? O10 Cl2 O8 105.7(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 N3 Cd1 N1 C5 4.7(4) . . . . ? N6 Cd1 N1 C5 -76.4(2) . . . . ? N2 Cd1 N1 C5 -164.0(2) . . . . ? N5 Cd1 N1 C5 109.3(2) . . . . ? O2 Cd1 N1 C5 -157.8(2) . . . . ? N4 Cd1 N1 C5 15.0(2) . . . . ? N3 Cd1 N1 C1 -179.6(2) . . . . ? N6 Cd1 N1 C1 99.3(2) . . . . ? N2 Cd1 N1 C1 11.7(2) . . . . ? N5 Cd1 N1 C1 -74.9(2) . . . . ? O2 Cd1 N1 C1 17.9(3) . . . . ? N4 Cd1 N1 C1 -169.3(2) . . . . ? N1 Cd1 N2 C22 -157.7(2) . . . . ? N3 Cd1 N2 C22 29.4(3) . . . . ? N6 Cd1 N2 C22 110.2(2) . . . . ? N5 Cd1 N2 C22 -63.9(2) . . . . ? O2 Cd1 N2 C22 27.02(19) . . . . ? N4 Cd1 N2 C22 -159.18(19) . . . . ? N1 Cd1 N2 C23 -27.0(2) . . . . ? N3 Cd1 N2 C23 160.14(19) . . . . ? N6 Cd1 N2 C23 -119.0(2) . . . . ? N5 Cd1 N2 C23 66.9(2) . . . . ? O2 Cd1 N2 C23 157.8(2) . . . . ? N4 Cd1 N2 C23 -28.4(3) . . . . ? N1 Cd1 N3 C15 -144.7(2) . . . . ? N6 Cd1 N3 C15 -62.1(2) . . . . ? N2 Cd1 N3 C15 20.1(3) . . . . ? N5 Cd1 N3 C15 110.9(2) . . . . ? O2 Cd1 N3 C15 22.4(2) . . . . ? N4 Cd1 N3 C15 -154.3(2) . . . . ? N1 Cd1 N3 C14 84.5(3) . . . . ? N6 Cd1 N3 C14 167.1(3) . . . . ? N2 Cd1 N3 C14 -110.7(3) . . . . ? N5 Cd1 N3 C14 -19.9(3) . . . . ? O2 Cd1 N3 C14 -108.4(3) . . . . ? N4 Cd1 N3 C14 74.9(3) . . . . ? N1 Cd1 N4 C7 100.3(2) . . . . ? N3 Cd1 N4 C7 -84.3(2) . . . . ? N6 Cd1 N4 C7 -168.9(2) . . . . ? N2 Cd1 N4 C7 101.8(2) . . . . ? N5 Cd1 N4 C7 9.2(2) . . . . ? O2 Cd1 N4 C7 -91.6(3) . . . . ? N1 Cd1 N4 C6 -26.15(19) . . . . ? N3 Cd1 N4 C6 149.3(2) . . . . ? N6 Cd1 N4 C6 64.6(2) . . . . ? N2 Cd1 N4 C6 -24.7(3) . . . . ? N5 Cd1 N4 C6 -117.3(2) . . . . ? O2 Cd1 N4 C6 141.9(2) . . . . ? N1 Cd1 N5 C24 -31.0(11) . . . . ? N3 Cd1 N5 C24 123.5(11) . . . . ? N6 Cd1 N5 C24 -157.4(11) . . . . ? N2 Cd1 N5 C24 -101.5(11) . . . . ? O2 Cd1 N5 C24 -166.7(11) . . . . ? N4 Cd1 N5 C24 37.9(11) . . . . ? N1 Cd1 N6 C26 158.3(8) . . . . ? N3 Cd1 N6 C26 4.5(8) . . . . ? N2 Cd1 N6 C26 -131.1(8) . . . . ? N5 Cd1 N6 C26 -75.2(14) . . . . ? O2 Cd1 N6 C26 -65.9(8) . . . . ? N4 Cd1 N6 C26 89.6(8) . . . . ? C5 N1 C1 C2 -0.5(5) . . . . ? Cd1 N1 C1 C2 -176.3(2) . . . . ? C5 N1 C1 C23 -178.0(3) . . . . ? Cd1 N1 C1 C23 6.1(4) . . . . ? N1 C1 C2 C3 -0.2(5) . . . . ? C23 C1 C2 C3 177.2(3) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C1 N1 C5 C4 1.1(5) . . . . ? Cd1 N1 C5 C4 176.8(2) . . . . ? C1 N1 C5 C6 -176.4(3) . . . . ? Cd1 N1 C5 C6 -0.7(4) . . . . ? C3 C4 C5 N1 -1.0(5) . . . . ? C3 C4 C5 C6 176.4(3) . . . . ? C7 N4 C6 C5 -83.3(4) . . . . ? Cd1 N4 C6 C5 35.7(3) . . . . ? N1 C5 C6 N4 -26.4(4) . . . . ? C4 C5 C6 N4 156.1(3) . . . . ? C6 N4 C7 C8 29.1(5) . . . . ? Cd1 N4 C7 C8 -90.8(3) . . . . ? C6 N4 C7 C12 -154.1(3) . . . . ? Cd1 N4 C7 C12 86.0(3) . . . . ? C12 C7 C8 C9 -0.7(5) . . . . ? N4 C7 C8 C9 176.1(3) . . . . ? C7 C8 C9 C10 -1.7(6) . . . . ? C8 C9 C10 C11 3.2(7) . . . . ? C9 C10 C11 C12 -2.2(7) . . . . ? C10 C11 C12 O1 175.6(4) . . . . ? C10 C11 C12 C7 -0.1(6) . . . . ? C8 C7 C12 C11 1.6(5) . . . . ? N4 C7 C12 C11 -175.4(3) . . . . ? C8 C7 C12 O1 -174.5(3) . . . . ? N4 C7 C12 O1 8.5(4) . . . . ? C15 N3 C14 C13 124.1(3) . . . . ? Cd1 N3 C14 C13 -106.1(3) . . . . ? O1 C13 C14 N3 56.6(4) . . . . ? C14 N3 C15 C16 80.3(4) . . . . ? Cd1 N3 C15 C16 -53.0(4) . . . . ? N3 C15 C16 O2 59.5(4) . . . . ? O2 C17 C18 C19 179.8(3) . . . . ? C22 C17 C18 C19 -0.2(5) . . . . ? C17 C18 C19 C20 -0.8(6) . . . . ? C18 C19 C20 C21 0.7(6) . . . . ? C19 C20 C21 C22 0.4(5) . . . . ? O2 C17 C22 C21 -178.7(3) . . . . ? C18 C17 C22 C21 1.2(5) . . . . ? O2 C17 C22 N2 0.7(4) . . . . ? C18 C17 C22 N2 -179.3(3) . . . . ? C20 C21 C22 C17 -1.4(5) . . . . ? C20 C21 C22 N2 179.2(3) . . . . ? C23 N2 C22 C17 -154.3(3) . . . . ? Cd1 N2 C22 C17 -26.6(4) . . . . ? C23 N2 C22 C21 25.1(5) . . . . ? Cd1 N2 C22 C21 152.9(3) . . . . ? C22 N2 C23 C1 169.7(3) . . . . ? Cd1 N2 C23 C1 39.4(3) . . . . ? N1 C1 C23 N2 -31.8(4) . . . . ? C2 C1 C23 N2 150.7(3) . . . . ? Cd1 N5 C24 C25 -116(17) . . . . ? Cd1 N6 C26 C27 -76(18) . . . . ? C11 C12 O1 C13 53.3(5) . . . . ? C7 C12 O1 C13 -130.7(3) . . . . ? C14 C13 O1 C12 65.5(4) . . . . ? C22 C17 O2 C16 168.1(3) . . . . ? C18 C17 O2 C16 -11.9(5) . . . . ? C22 C17 O2 Cd1 25.0(4) . . . . ? C18 C17 O2 Cd1 -154.9(3) . . . . ? C15 C16 O2 C17 179.4(3) . . . . ? C15 C16 O2 Cd1 -37.0(3) . . . . ? N1 Cd1 O2 C17 -34.5(3) . . . . ? N3 Cd1 O2 C17 153.7(3) . . . . ? N6 Cd1 O2 C17 -119.3(2) . . . . ? N2 Cd1 O2 C17 -28.0(2) . . . . ? N5 Cd1 O2 C17 59.6(2) . . . . ? N4 Cd1 O2 C17 161.5(2) . . . . ? N1 Cd1 O2 C16 -179.3(2) . . . . ? N3 Cd1 O2 C16 8.9(2) . . . . ? N6 Cd1 O2 C16 95.9(2) . . . . ? N2 Cd1 O2 C16 -172.9(3) . . . . ? N5 Cd1 O2 C16 -85.2(2) . . . . ? N4 Cd1 O2 C16 16.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.91 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.658 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.075 data_ifn14a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H22 Cd N6 O8' _chemical_formula_weight 622.87 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.9479(13) _cell_length_b 12.605(2) _cell_length_c 23.682(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.467(18) _cell_angle_gamma 90.00 _cell_volume 2361.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.988 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.6378 _exptl_absorpt_correction_T_max 0.9076 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15442 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.34 _reflns_number_total 5685 _reflns_number_gt 4627 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0629P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5685 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.20056(2) 0.269165(14) 0.097747(7) 0.02751(8) Uani 1 1 d . . . O1 O -0.0704(2) 0.37974(13) 0.14715(7) 0.0303(4) Uani 1 1 d . . . O2 O 0.3231(2) 0.08068(14) 0.14603(8) 0.0370(4) Uani 1 1 d . . . O3 O 0.4505(3) 0.33413(18) 0.14933(9) 0.0494(5) Uani 1 1 d . . . O4 O 0.5037(2) 0.40469(17) 0.23233(9) 0.0446(5) Uani 1 1 d . . . O5 O 0.2574(3) 0.33925(18) 0.20667(10) 0.0516(6) Uani 1 1 d . . . O6 O -0.1348(3) 0.17026(18) -0.04110(8) 0.0467(5) Uani 1 1 d . . . O7 O 0.0792(3) 0.13684(16) 0.02037(8) 0.0420(5) Uani 1 1 d . . . O8 O -0.0630(3) 0.27955(15) 0.02802(9) 0.0443(5) Uani 1 1 d . . . N1 N 0.3164(2) 0.34858(16) 0.01842(8) 0.0266(4) Uani 1 1 d . . . N2 N 0.1463(3) 0.46864(16) 0.08889(9) 0.0273(4) Uani 1 1 d . . . N3 N 0.0093(3) 0.16056(16) 0.14477(9) 0.0310(4) Uani 1 1 d . . . H3B H -0.0155 0.1058 0.1204 0.037 Uiso 1 1 calc R . . N4 N 0.4487(3) 0.16048(16) 0.05686(9) 0.0273(4) Uani 1 1 d . . . N5 N 0.4047(3) 0.36015(16) 0.19671(10) 0.0347(5) Uani 1 1 d . . . N6 N -0.0414(3) 0.19451(18) 0.00158(9) 0.0322(5) Uani 1 1 d . . . C1 C 0.4146(3) 0.2942(2) -0.01405(10) 0.0275(5) Uani 1 1 d . . . C2 C 0.4616(3) 0.3335(2) -0.06518(11) 0.0327(5) Uani 1 1 d . . . H2 H 0.5291 0.2935 -0.0871 0.039 Uiso 1 1 calc R . . C3 C 0.4057(3) 0.4339(2) -0.08300(11) 0.0335(5) Uani 1 1 d . . . H3A H 0.4325 0.4613 -0.1175 0.040 Uiso 1 1 calc R . . C4 C 0.3099(3) 0.4920(2) -0.04846(10) 0.0305(5) Uani 1 1 d . . . H4 H 0.2741 0.5601 -0.0587 0.037 Uiso 1 1 calc R . . C5 C 0.2680(3) 0.44705(19) 0.00165(10) 0.0270(5) Uani 1 1 d . . . C6 C 0.1774(3) 0.50913(19) 0.04184(10) 0.0278(5) Uani 1 1 d . . . H6 H 0.1428 0.5781 0.0328 0.033 Uiso 1 1 calc R . . C7 C 0.0740(3) 0.53252(19) 0.12913(10) 0.0285(5) Uani 1 1 d . . . C8 C 0.1115(3) 0.6394(2) 0.13822(12) 0.0357(6) Uani 1 1 d . . . H8 H 0.1829 0.6742 0.1154 0.043 Uiso 1 1 calc R . . C9 C 0.0420(4) 0.6938(2) 0.18136(13) 0.0410(6) Uani 1 1 d . . . H9 H 0.0687 0.7648 0.1880 0.049 Uiso 1 1 calc R . . C10 C -0.0662(4) 0.6427(2) 0.21421(12) 0.0396(6) Uani 1 1 d . . . H10 H -0.1131 0.6799 0.2428 0.048 Uiso 1 1 calc R . . C11 C -0.1067(3) 0.5364(2) 0.20555(11) 0.0327(5) Uani 1 1 d . . . H11 H -0.1802 0.5024 0.2279 0.039 Uiso 1 1 calc R . . C12 C -0.0355(3) 0.48194(19) 0.16291(10) 0.0279(5) Uani 1 1 d . . . C13 C -0.1395(3) 0.3094(2) 0.18600(11) 0.0305(5) Uani 1 1 d . . . H13A H -0.2486 0.3345 0.1957 0.037 Uiso 1 1 calc R . . H13B H -0.0642 0.3021 0.2205 0.037 Uiso 1 1 calc R . . C14 C -0.1568(3) 0.2061(2) 0.15424(12) 0.0326(5) Uani 1 1 d . . . H14A H -0.2184 0.1560 0.1756 0.039 Uiso 1 1 calc R . . H14B H -0.2215 0.2175 0.1179 0.039 Uiso 1 1 calc R . . C15 C 0.0877(4) 0.1095(2) 0.19679(12) 0.0375(6) Uani 1 1 d . . . H15A H 0.0011 0.0749 0.2164 0.045 Uiso 1 1 calc R . . H15B H 0.1413 0.1630 0.2219 0.045 Uiso 1 1 calc R . . C16 C 0.2178(4) 0.0286(2) 0.18279(13) 0.0403(6) Uani 1 1 d . . . H16A H 0.2838 0.0050 0.2170 0.048 Uiso 1 1 calc R . . H16B H 0.1632 -0.0325 0.1641 0.048 Uiso 1 1 calc R . . C17 C 0.4568(3) 0.0263(2) 0.12863(11) 0.0319(5) Uani 1 1 d . . . C18 C 0.5270(4) -0.0634(2) 0.15611(12) 0.0388(6) Uani 1 1 d . . . H18 H 0.4757 -0.0936 0.1860 0.047 Uiso 1 1 calc R . . C19 C 0.6730(4) -0.1074(2) 0.13881(12) 0.0428(7) Uani 1 1 d . . . H19 H 0.7226 -0.1652 0.1583 0.051 Uiso 1 1 calc R . . C20 C 0.7461(4) -0.0660(2) 0.09276(12) 0.0397(6) Uani 1 1 d . . . H20 H 0.8446 -0.0959 0.0815 0.048 Uiso 1 1 calc R . . C21 C 0.6723(3) 0.0199(2) 0.06361(11) 0.0331(5) Uani 1 1 d . . . H21 H 0.7197 0.0463 0.0321 0.040 Uiso 1 1 calc R . . C22 C 0.5271(3) 0.06719(19) 0.08115(11) 0.0293(5) Uani 1 1 d . . . C23 C 0.4826(3) 0.19164(19) 0.00829(10) 0.0275(5) Uani 1 1 d . . . H23 H 0.5498 0.1503 -0.0131 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02751(11) 0.02823(12) 0.02742(12) 0.00377(6) 0.00594(7) -0.00221(6) O1 0.0369(10) 0.0257(8) 0.0292(9) -0.0005(7) 0.0080(7) -0.0033(7) O2 0.0378(10) 0.0326(10) 0.0430(11) 0.0137(8) 0.0151(8) 0.0060(8) O3 0.0505(12) 0.0560(13) 0.0402(11) -0.0167(10) -0.0040(9) 0.0157(10) O4 0.0365(11) 0.0476(12) 0.0503(12) -0.0228(10) 0.0065(9) -0.0053(9) O5 0.0310(10) 0.0498(12) 0.0724(15) 0.0158(11) -0.0028(10) -0.0071(9) O6 0.0421(11) 0.0630(14) 0.0336(11) 0.0022(9) -0.0035(9) -0.0087(10) O7 0.0404(11) 0.0456(11) 0.0401(11) -0.0005(9) 0.0047(8) 0.0098(9) O8 0.0605(14) 0.0333(11) 0.0400(12) 0.0040(8) 0.0087(10) 0.0074(9) N1 0.0267(10) 0.0268(10) 0.0266(10) 0.0009(8) 0.0047(8) -0.0015(8) N2 0.0264(10) 0.0260(10) 0.0301(11) 0.0006(8) 0.0056(8) -0.0006(8) N3 0.0369(11) 0.0255(10) 0.0321(11) 0.0001(8) 0.0106(9) -0.0014(8) N4 0.0282(10) 0.0223(9) 0.0314(11) -0.0014(8) 0.0030(8) -0.0021(8) N5 0.0341(12) 0.0259(10) 0.0433(13) -0.0032(9) -0.0010(10) 0.0047(9) N6 0.0320(11) 0.0353(11) 0.0304(11) 0.0034(9) 0.0090(9) -0.0035(9) C1 0.0261(11) 0.0292(12) 0.0279(12) -0.0008(9) 0.0061(9) -0.0045(9) C2 0.0302(13) 0.0384(14) 0.0303(13) -0.0026(10) 0.0074(10) -0.0036(10) C3 0.0361(13) 0.0393(14) 0.0252(12) 0.0045(10) 0.0037(10) -0.0079(11) C4 0.0321(13) 0.0302(12) 0.0286(13) 0.0049(9) -0.0002(10) -0.0051(10) C5 0.0259(11) 0.0286(12) 0.0264(12) 0.0033(9) 0.0029(9) -0.0012(9) C6 0.0266(12) 0.0263(12) 0.0304(13) 0.0035(9) 0.0023(9) 0.0012(9) C7 0.0268(12) 0.0285(12) 0.0307(13) 0.0011(9) 0.0047(9) 0.0023(9) C8 0.0373(14) 0.0301(13) 0.0414(15) 0.0013(11) 0.0122(11) -0.0014(10) C9 0.0514(17) 0.0270(12) 0.0463(16) -0.0043(12) 0.0135(13) 0.0009(12) C10 0.0499(17) 0.0340(14) 0.0368(15) -0.0050(11) 0.0139(12) 0.0052(12) C11 0.0363(13) 0.0323(13) 0.0306(13) 0.0023(10) 0.0090(10) 0.0018(10) C12 0.0278(12) 0.0276(12) 0.0286(12) 0.0021(9) 0.0035(9) 0.0023(9) C13 0.0305(12) 0.0287(12) 0.0333(13) 0.0037(10) 0.0086(10) -0.0008(10) C14 0.0293(12) 0.0333(13) 0.0363(14) -0.0007(10) 0.0083(10) -0.0073(10) C15 0.0409(15) 0.0363(14) 0.0364(14) 0.0107(11) 0.0093(11) 0.0005(11) C16 0.0393(15) 0.0369(14) 0.0464(16) 0.0157(12) 0.0124(12) 0.0020(11) C17 0.0321(13) 0.0296(12) 0.0337(13) -0.0010(10) 0.0012(10) 0.0008(10) C18 0.0491(16) 0.0327(13) 0.0344(14) 0.0042(11) 0.0025(12) 0.0056(12) C19 0.0545(18) 0.0321(14) 0.0401(16) -0.0017(12) -0.0047(13) 0.0124(12) C20 0.0414(15) 0.0337(14) 0.0433(16) -0.0106(12) -0.0002(12) 0.0102(12) C21 0.0341(13) 0.0329(13) 0.0323(13) -0.0076(10) 0.0027(10) 0.0017(10) C22 0.0321(13) 0.0243(11) 0.0308(12) -0.0029(9) -0.0001(10) 0.0000(9) C23 0.0299(12) 0.0228(11) 0.0310(12) -0.0004(9) 0.0082(9) -0.0012(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.376(2) . ? Cd1 N1 2.389(2) . ? Cd1 N3 2.397(2) . ? Cd1 O8 2.544(2) . ? Cd1 N2 2.556(2) . ? Cd1 O7 2.595(2) . ? Cd1 N4 2.658(2) . ? O1 C12 1.362(3) . ? O1 C13 1.425(3) . ? O2 C17 1.361(3) . ? O2 C16 1.424(3) . ? O3 N5 1.256(3) . ? O4 N5 1.232(3) . ? O5 N5 1.245(3) . ? O6 N6 1.234(3) . ? O7 N6 1.250(3) . ? O8 N6 1.261(3) . ? N1 C1 1.336(3) . ? N1 C5 1.348(3) . ? N2 C6 1.271(3) . ? N2 C7 1.411(3) . ? N3 C15 1.474(3) . ? N3 C14 1.476(3) . ? N4 C23 1.268(3) . ? N4 C22 1.426(3) . ? C1 C2 1.392(3) . ? C1 C23 1.480(3) . ? C2 C3 1.393(4) . ? C3 C4 1.379(4) . ? C4 C5 1.384(3) . ? C5 C6 1.472(3) . ? C7 C8 1.391(4) . ? C7 C12 1.392(3) . ? C8 C9 1.388(4) . ? C9 C10 1.374(4) . ? C10 C11 1.389(4) . ? C11 C12 1.385(3) . ? C13 C14 1.505(4) . ? C15 C16 1.511(4) . ? C17 C18 1.395(4) . ? C17 C22 1.401(4) . ? C18 C19 1.383(4) . ? C19 C20 1.385(4) . ? C20 C21 1.384(4) . ? C21 C22 1.397(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 N1 83.90(8) . . ? O3 Cd1 N3 119.60(8) . . ? N1 Cd1 N3 155.98(7) . . ? O3 Cd1 O8 155.82(7) . . ? N1 Cd1 O8 79.82(7) . . ? N3 Cd1 O8 79.14(7) . . ? O3 Cd1 N2 80.18(7) . . ? N1 Cd1 N2 66.30(7) . . ? N3 Cd1 N2 119.37(7) . . ? O8 Cd1 N2 76.95(6) . . ? O3 Cd1 O7 145.17(7) . . ? N1 Cd1 O7 81.91(7) . . ? N3 Cd1 O7 75.61(7) . . ? O8 Cd1 O7 49.23(6) . . ? N2 Cd1 O7 121.73(6) . . ? O3 Cd1 N4 75.64(7) . . ? N1 Cd1 N4 64.83(7) . . ? N3 Cd1 N4 113.58(7) . . ? O8 Cd1 N4 112.55(7) . . ? N2 Cd1 N4 127.02(6) . . ? O7 Cd1 N4 69.53(6) . . ? C12 O1 C13 119.47(19) . . ? C17 O2 C16 118.3(2) . . ? N5 O3 Cd1 104.48(17) . . ? N6 O7 Cd1 95.65(15) . . ? N6 O8 Cd1 97.83(15) . . ? C1 N1 C5 118.0(2) . . ? C1 N1 Cd1 121.84(16) . . ? C5 N1 Cd1 119.78(16) . . ? C6 N2 C7 119.2(2) . . ? C6 N2 Cd1 114.94(16) . . ? C7 N2 Cd1 125.61(15) . . ? C15 N3 C14 110.8(2) . . ? C15 N3 Cd1 113.67(17) . . ? C14 N3 Cd1 117.69(15) . . ? C23 N4 C22 119.9(2) . . ? C23 N4 Cd1 113.58(16) . . ? C22 N4 Cd1 126.08(16) . . ? O4 N5 O5 121.2(2) . . ? O4 N5 O3 120.7(2) . . ? O5 N5 O3 118.2(2) . . ? O6 N6 O7 121.9(2) . . ? O6 N6 O8 121.2(2) . . ? O7 N6 O8 116.9(2) . . ? N1 C1 C2 122.5(2) . . ? N1 C1 C23 117.1(2) . . ? C2 C1 C23 120.2(2) . . ? C1 C2 C3 118.9(2) . . ? C4 C3 C2 118.7(2) . . ? C3 C4 C5 118.9(2) . . ? N1 C5 C4 122.9(2) . . ? N1 C5 C6 116.3(2) . . ? C4 C5 C6 120.6(2) . . ? N2 C6 C5 120.1(2) . . ? C8 C7 C12 119.4(2) . . ? C8 C7 N2 124.2(2) . . ? C12 C7 N2 116.4(2) . . ? C9 C8 C7 119.8(3) . . ? C10 C9 C8 120.0(3) . . ? C9 C10 C11 121.2(3) . . ? C12 C11 C10 118.7(2) . . ? O1 C12 C11 125.6(2) . . ? O1 C12 C7 113.4(2) . . ? C11 C12 C7 120.9(2) . . ? O1 C13 C14 103.8(2) . . ? N3 C14 C13 111.8(2) . . ? N3 C15 C16 110.8(2) . . ? O2 C16 C15 106.1(2) . . ? O2 C17 C18 123.8(2) . . ? O2 C17 C22 116.1(2) . . ? C18 C17 C22 120.0(2) . . ? C19 C18 C17 119.8(3) . . ? C20 C19 C18 120.6(3) . . ? C21 C20 C19 119.8(3) . . ? C20 C21 C22 120.6(3) . . ? C21 C22 C17 119.1(2) . . ? C21 C22 N4 125.0(2) . . ? C17 C22 N4 115.8(2) . . ? N4 C23 C1 119.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1 O3 N5 144.71(17) . . . . ? N3 Cd1 O3 N5 -40.52(19) . . . . ? O8 Cd1 O3 N5 96.9(2) . . . . ? N2 Cd1 O3 N5 77.78(16) . . . . ? O7 Cd1 O3 N5 -148.94(14) . . . . ? N4 Cd1 O3 N5 -149.76(18) . . . . ? O3 Cd1 O7 N6 -147.00(15) . . . . ? N1 Cd1 O7 N6 -80.08(15) . . . . ? N3 Cd1 O7 N6 91.40(15) . . . . ? O8 Cd1 O7 N6 3.43(13) . . . . ? N2 Cd1 O7 N6 -24.49(17) . . . . ? N4 Cd1 O7 N6 -146.15(16) . . . . ? O3 Cd1 O8 N6 133.11(18) . . . . ? N1 Cd1 O8 N6 84.64(16) . . . . ? N3 Cd1 O8 N6 -83.69(15) . . . . ? N2 Cd1 O8 N6 152.45(16) . . . . ? O7 Cd1 O8 N6 -3.41(13) . . . . ? N4 Cd1 O8 N6 27.50(17) . . . . ? O3 Cd1 N1 C1 91.58(18) . . . . ? N3 Cd1 N1 C1 -77.2(3) . . . . ? O8 Cd1 N1 C1 -106.39(18) . . . . ? N2 Cd1 N1 C1 173.5(2) . . . . ? O7 Cd1 N1 C1 -56.52(18) . . . . ? N4 Cd1 N1 C1 14.60(17) . . . . ? O3 Cd1 N1 C5 -95.87(18) . . . . ? N3 Cd1 N1 C5 95.4(2) . . . . ? O8 Cd1 N1 C5 66.17(18) . . . . ? N2 Cd1 N1 C5 -13.95(16) . . . . ? O7 Cd1 N1 C5 116.03(18) . . . . ? N4 Cd1 N1 C5 -172.84(19) . . . . ? O3 Cd1 N2 C6 100.42(18) . . . . ? N1 Cd1 N2 C6 12.81(16) . . . . ? N3 Cd1 N2 C6 -141.04(17) . . . . ? O8 Cd1 N2 C6 -71.66(17) . . . . ? O7 Cd1 N2 C6 -50.31(19) . . . . ? N4 Cd1 N2 C6 36.9(2) . . . . ? O3 Cd1 N2 C7 -84.99(18) . . . . ? N1 Cd1 N2 C7 -172.6(2) . . . . ? N3 Cd1 N2 C7 33.6(2) . . . . ? O8 Cd1 N2 C7 102.93(18) . . . . ? O7 Cd1 N2 C7 124.27(17) . . . . ? N4 Cd1 N2 C7 -148.51(17) . . . . ? O3 Cd1 N3 C15 -21.03(19) . . . . ? N1 Cd1 N3 C15 146.10(18) . . . . ? O8 Cd1 N3 C15 175.37(18) . . . . ? N2 Cd1 N3 C15 -116.46(17) . . . . ? O7 Cd1 N3 C15 124.95(18) . . . . ? N4 Cd1 N3 C15 65.34(18) . . . . ? O3 Cd1 N3 C14 110.90(18) . . . . ? N1 Cd1 N3 C14 -82.0(2) . . . . ? O8 Cd1 N3 C14 -52.70(18) . . . . ? N2 Cd1 N3 C14 15.5(2) . . . . ? O7 Cd1 N3 C14 -103.11(18) . . . . ? N4 Cd1 N3 C14 -162.72(17) . . . . ? O3 Cd1 N4 C23 -104.27(18) . . . . ? N1 Cd1 N4 C23 -14.31(16) . . . . ? N3 Cd1 N4 C23 139.34(17) . . . . ? O8 Cd1 N4 C23 51.70(18) . . . . ? N2 Cd1 N4 C23 -38.7(2) . . . . ? O7 Cd1 N4 C23 76.23(17) . . . . ? O3 Cd1 N4 C22 83.46(18) . . . . ? N1 Cd1 N4 C22 173.4(2) . . . . ? N3 Cd1 N4 C22 -32.9(2) . . . . ? O8 Cd1 N4 C22 -120.58(18) . . . . ? N2 Cd1 N4 C22 149.02(17) . . . . ? O7 Cd1 N4 C22 -96.04(18) . . . . ? Cd1 O3 N5 O4 -174.55(19) . . . . ? Cd1 O3 N5 O5 5.8(3) . . . . ? Cd1 O7 N6 O6 173.6(2) . . . . ? Cd1 O7 N6 O8 -5.9(2) . . . . ? Cd1 O8 N6 O6 -173.44(19) . . . . ? Cd1 O8 N6 O7 6.0(2) . . . . ? C5 N1 C1 C2 -2.9(3) . . . . ? Cd1 N1 C1 C2 169.80(18) . . . . ? C5 N1 C1 C23 173.1(2) . . . . ? Cd1 N1 C1 C23 -14.2(3) . . . . ? N1 C1 C2 C3 0.7(4) . . . . ? C23 C1 C2 C3 -175.2(2) . . . . ? C1 C2 C3 C4 1.9(4) . . . . ? C2 C3 C4 C5 -2.1(4) . . . . ? C1 N1 C5 C4 2.6(3) . . . . ? Cd1 N1 C5 C4 -170.24(18) . . . . ? C1 N1 C5 C6 -172.9(2) . . . . ? Cd1 N1 C5 C6 14.3(3) . . . . ? C3 C4 C5 N1 -0.1(4) . . . . ? C3 C4 C5 C6 175.2(2) . . . . ? C7 N2 C6 C5 174.0(2) . . . . ? Cd1 N2 C6 C5 -11.1(3) . . . . ? N1 C5 C6 N2 -1.2(3) . . . . ? C4 C5 C6 N2 -176.8(2) . . . . ? C6 N2 C7 C8 -36.0(3) . . . . ? Cd1 N2 C7 C8 149.6(2) . . . . ? C6 N2 C7 C12 146.9(2) . . . . ? Cd1 N2 C7 C12 -27.4(3) . . . . ? C12 C7 C8 C9 1.2(4) . . . . ? N2 C7 C8 C9 -175.8(2) . . . . ? C7 C8 C9 C10 -1.3(4) . . . . ? C8 C9 C10 C11 0.7(5) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C13 O1 C12 C11 -21.7(4) . . . . ? C13 O1 C12 C7 162.4(2) . . . . ? C10 C11 C12 O1 -176.0(2) . . . . ? C10 C11 C12 C7 -0.2(4) . . . . ? C8 C7 C12 O1 175.8(2) . . . . ? N2 C7 C12 O1 -7.0(3) . . . . ? C8 C7 C12 C11 -0.4(4) . . . . ? N2 C7 C12 C11 176.8(2) . . . . ? C12 O1 C13 C14 -179.0(2) . . . . ? C15 N3 C14 C13 77.8(3) . . . . ? Cd1 N3 C14 C13 -55.4(3) . . . . ? O1 C13 C14 N3 67.1(3) . . . . ? C14 N3 C15 C16 157.9(2) . . . . ? Cd1 N3 C15 C16 -66.9(2) . . . . ? C17 O2 C16 C15 177.3(2) . . . . ? N3 C15 C16 O2 49.4(3) . . . . ? C16 O2 C17 C18 -19.2(4) . . . . ? C16 O2 C17 C22 162.6(2) . . . . ? O2 C17 C18 C19 -173.6(3) . . . . ? C22 C17 C18 C19 4.5(4) . . . . ? C17 C18 C19 C20 -2.9(4) . . . . ? C18 C19 C20 C21 -0.2(4) . . . . ? C19 C20 C21 C22 1.8(4) . . . . ? C20 C21 C22 C17 -0.2(4) . . . . ? C20 C21 C22 N4 175.0(2) . . . . ? O2 C17 C22 C21 175.3(2) . . . . ? C18 C17 C22 C21 -3.0(4) . . . . ? O2 C17 C22 N4 -0.3(3) . . . . ? C18 C17 C22 N4 -178.6(2) . . . . ? C23 N4 C22 C21 17.6(4) . . . . ? Cd1 N4 C22 C21 -170.55(18) . . . . ? C23 N4 C22 C17 -167.0(2) . . . . ? Cd1 N4 C22 C17 4.8(3) . . . . ? C22 N4 C23 C1 -173.7(2) . . . . ? Cd1 N4 C23 C1 13.5(3) . . . . ? N1 C1 C23 N4 -1.2(3) . . . . ? C2 C1 C23 N4 174.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.306 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.126 data_ifn15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H26 Cd Cl2 N4 O12' _chemical_formula_weight 733.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.382(7) _cell_length_b 10.683(2) _cell_length_c 18.127(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.983(6) _cell_angle_gamma 90.00 _cell_volume 5415.2(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.7747 _exptl_absorpt_correction_T_max 0.8552 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17448 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.66 _reflns_number_total 6471 _reflns_number_gt 4866 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6471 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.369915(8) 0.619662(19) 0.749469(14) 0.02410(9) Uani 1 1 d . . . Cl1 Cl 0.74492(3) 0.71617(7) 0.62389(5) 0.03099(18) Uani 1 1 d . . . Cl2 Cl 0.46138(3) 0.89455(7) 0.59300(5) 0.03061(18) Uani 1 1 d . . . O1 O 0.43112(8) 0.74737(19) 0.90853(13) 0.0281(5) Uani 1 1 d . . . O2 O 0.31350(9) 0.7751(2) 0.62447(14) 0.0344(5) Uani 1 1 d . . . O3 O 0.69346(12) 0.7134(4) 0.5916(2) 0.0810(12) Uani 1 1 d . . . O4 O 0.76562(13) 0.6585(3) 0.70370(18) 0.0666(10) Uani 1 1 d . . . O5 O 0.75806(14) 0.8439(3) 0.6313(2) 0.0644(9) Uani 1 1 d . . . O6 O 0.75772(10) 0.6533(2) 0.56796(16) 0.0413(6) Uani 1 1 d . . . O7 O 0.50241(10) 0.9746(3) 0.6351(2) 0.0543(8) Uani 1 1 d . . . O8 O 0.41986(9) 0.9548(3) 0.58792(19) 0.0505(7) Uani 1 1 d . . . O9 O 0.47002(9) 0.7786(2) 0.64013(15) 0.0361(6) Uani 1 1 d . . . O10 O 0.45580(12) 0.8652(2) 0.51227(17) 0.0495(7) Uani 1 1 d . . . O11 O 0.43500(8) 0.7086(2) 0.74899(15) 0.0397(6) Uani 1 1 d . . . H1W H 0.4476 0.7338 0.7095 0.048 Uiso 1 1 d R . . H2W H 0.4685 0.7330 0.7881 0.048 Uiso 1 1 d R . . O12 O 0.30378(8) 0.5243(2) 0.75552(16) 0.0359(6) Uani 1 1 d . . . H3W H 0.2876 0.4601 0.7114 0.043 Uiso 1 1 d R . . H4W H 0.2805 0.5695 0.7695 0.043 Uiso 1 1 d R . . N1 N 0.38445(9) 0.4089(2) 0.72845(16) 0.0249(5) Uani 1 1 d . . . N2 N 0.41862(9) 0.5013(2) 0.88690(16) 0.0225(5) Uani 1 1 d . . . N3 N 0.34227(9) 0.8013(2) 0.78959(16) 0.0264(6) Uani 1 1 d . . . H3B H 0.3376 0.7777 0.8336 0.032 Uiso 1 1 calc R . . N4 N 0.34807(9) 0.5699(3) 0.59950(16) 0.0275(6) Uani 1 1 d . . . C1 C 0.36920(11) 0.3635(3) 0.6519(2) 0.0273(7) Uani 1 1 d . . . C2 C 0.37452(12) 0.2384(3) 0.6368(2) 0.0322(7) Uani 1 1 d . . . H2 H 0.3627 0.2089 0.5829 0.039 Uiso 1 1 calc R . . C3 C 0.39777(13) 0.1579(3) 0.7038(2) 0.0349(8) Uani 1 1 d . . . H3A H 0.4024 0.0741 0.6955 0.042 Uiso 1 1 calc R . . C4 C 0.41373(12) 0.2053(3) 0.7826(2) 0.0315(7) Uani 1 1 d . . . H4 H 0.4293 0.1535 0.8284 0.038 Uiso 1 1 calc R . . C5 C 0.40640(11) 0.3318(3) 0.7934(2) 0.0254(6) Uani 1 1 d . . . C6 C 0.42439(11) 0.3854(3) 0.8764(2) 0.0262(6) Uani 1 1 d . . . H6 H 0.4403 0.3343 0.9223 0.031 Uiso 1 1 calc R . . C7 C 0.43786(10) 0.5490(3) 0.96923(19) 0.0240(6) Uani 1 1 d . . . C8 C 0.44967(11) 0.4757(3) 1.0393(2) 0.0295(7) Uani 1 1 d . . . H8 H 0.4458 0.3893 1.0335 0.035 Uiso 1 1 calc R . . C9 C 0.46703(11) 0.5281(3) 1.1176(2) 0.0318(7) Uani 1 1 d . . . H9 H 0.4753 0.4778 1.1640 0.038 Uiso 1 1 calc R . . C10 C 0.47182(12) 0.6568(3) 1.1252(2) 0.0342(7) Uani 1 1 d . . . H10 H 0.4828 0.6929 1.1773 0.041 Uiso 1 1 calc R . . C11 C 0.46068(12) 0.7332(3) 1.0572(2) 0.0307(7) Uani 1 1 d . . . H11 H 0.4647 0.8194 1.0638 0.037 Uiso 1 1 calc R . . C12 C 0.44336(11) 0.6797(3) 0.97883(19) 0.0252(6) Uani 1 1 d . . . C13 C 0.41482(13) 0.8733(3) 0.9099(2) 0.0306(7) Uani 1 1 d . . . H13A H 0.4413 0.9319 0.9288 0.037 Uiso 1 1 calc R . . H13B H 0.3999 0.8789 0.9463 0.037 Uiso 1 1 calc R . . C14 C 0.37878(12) 0.9014(3) 0.8209(2) 0.0284(7) Uani 1 1 d . . . H14A H 0.3635 0.9813 0.8184 0.034 Uiso 1 1 calc R . . H14B H 0.3951 0.9067 0.7866 0.034 Uiso 1 1 calc R . . C15 C 0.29546(12) 0.8484(3) 0.7270(2) 0.0331(7) Uani 1 1 d . . . H15A H 0.2863 0.9206 0.7490 0.040 Uiso 1 1 calc R . . H15B H 0.2714 0.7841 0.7152 0.040 Uiso 1 1 calc R . . C16 C 0.29697(12) 0.8847(3) 0.6482(2) 0.0315(7) Uani 1 1 d . . . H16A H 0.2654 0.9083 0.6060 0.038 Uiso 1 1 calc R . . H16B H 0.3187 0.9542 0.6574 0.038 Uiso 1 1 calc R . . C17 C 0.31645(12) 0.7744(3) 0.5518(2) 0.0315(7) Uani 1 1 d . . . C18 C 0.30313(12) 0.8730(3) 0.4954(2) 0.0353(8) Uani 1 1 d . . . H18 H 0.2915 0.9474 0.5060 0.042 Uiso 1 1 calc R . . C19 C 0.30757(12) 0.8579(4) 0.4233(2) 0.0383(8) Uani 1 1 d . . . H19 H 0.2991 0.9235 0.3855 0.046 Uiso 1 1 calc R . . C20 C 0.32438(13) 0.7467(4) 0.4061(2) 0.0438(9) Uani 1 1 d . . . H20 H 0.3272 0.7382 0.3575 0.053 Uiso 1 1 calc R . . C21 C 0.33699(12) 0.6479(4) 0.4625(2) 0.0360(8) Uani 1 1 d . . . H21 H 0.3477 0.5728 0.4510 0.043 Uiso 1 1 calc R . . C22 C 0.33349(11) 0.6615(3) 0.5360(2) 0.0302(7) Uani 1 1 d . . . C23 C 0.34915(11) 0.4550(3) 0.5840(2) 0.0294(7) Uani 1 1 d . . . H23 H 0.3373 0.4282 0.5294 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02430(13) 0.02138(13) 0.02837(14) -0.00066(9) 0.01348(10) -0.00087(8) Cl1 0.0374(4) 0.0287(4) 0.0302(4) -0.0046(3) 0.0183(3) -0.0034(3) Cl2 0.0355(4) 0.0240(4) 0.0336(4) 0.0017(3) 0.0168(3) 0.0022(3) O1 0.0349(12) 0.0218(10) 0.0281(12) -0.0015(9) 0.0147(10) -0.0010(9) O2 0.0448(14) 0.0301(12) 0.0310(13) 0.0035(10) 0.0195(11) 0.0079(10) O3 0.0461(18) 0.131(3) 0.076(2) -0.059(2) 0.0361(17) -0.0297(19) O4 0.103(3) 0.0589(18) 0.0358(16) 0.0086(15) 0.0300(17) 0.0250(18) O5 0.110(3) 0.0322(14) 0.057(2) -0.0100(14) 0.0430(19) -0.0172(16) O6 0.0535(16) 0.0414(13) 0.0375(14) -0.0035(12) 0.0282(12) 0.0063(12) O7 0.0468(16) 0.0429(15) 0.073(2) -0.0075(14) 0.0265(15) -0.0137(13) O8 0.0379(15) 0.0509(16) 0.0575(18) -0.0037(14) 0.0171(13) 0.0136(12) O9 0.0464(14) 0.0307(12) 0.0331(13) 0.0083(10) 0.0195(11) 0.0021(11) O10 0.077(2) 0.0433(15) 0.0331(14) 0.0090(12) 0.0294(14) 0.0128(13) O11 0.0303(12) 0.0596(16) 0.0311(13) -0.0064(12) 0.0156(10) -0.0181(11) O12 0.0311(13) 0.0327(12) 0.0496(15) -0.0089(11) 0.0233(11) -0.0090(10) N1 0.0228(13) 0.0269(13) 0.0255(14) -0.0041(10) 0.0114(11) -0.0019(10) N2 0.0208(12) 0.0223(12) 0.0249(13) 0.0005(10) 0.0108(10) -0.0011(9) N3 0.0274(13) 0.0237(12) 0.0297(14) -0.0008(11) 0.0143(11) -0.0030(10) N4 0.0228(13) 0.0337(14) 0.0241(13) 0.0012(11) 0.0091(11) 0.0009(11) C1 0.0244(15) 0.0317(16) 0.0274(16) -0.0039(13) 0.0131(13) -0.0040(12) C2 0.0352(18) 0.0319(17) 0.0352(18) -0.0113(14) 0.0210(15) -0.0096(14) C3 0.0406(19) 0.0234(15) 0.048(2) -0.0071(15) 0.0265(17) -0.0063(14) C4 0.0354(18) 0.0242(15) 0.0391(19) 0.0012(14) 0.0204(15) -0.0007(13) C5 0.0251(15) 0.0229(14) 0.0300(16) -0.0027(13) 0.0140(13) -0.0017(12) C6 0.0259(15) 0.0262(15) 0.0265(16) 0.0028(12) 0.0121(13) 0.0018(12) C7 0.0177(14) 0.0291(16) 0.0248(15) -0.0008(12) 0.0094(12) 0.0005(11) C8 0.0286(16) 0.0309(16) 0.0293(17) 0.0034(13) 0.0134(13) 0.0002(13) C9 0.0269(16) 0.0409(19) 0.0249(16) 0.0074(14) 0.0094(13) 0.0036(14) C10 0.0316(17) 0.0437(19) 0.0276(17) -0.0088(15) 0.0137(14) 0.0004(15) C11 0.0319(17) 0.0298(17) 0.0290(17) -0.0063(14) 0.0126(14) -0.0034(13) C12 0.0214(15) 0.0281(16) 0.0260(16) -0.0015(12) 0.0106(12) -0.0011(12) C13 0.0376(18) 0.0238(16) 0.0307(17) -0.0014(13) 0.0158(14) -0.0012(13) C14 0.0348(17) 0.0184(14) 0.0327(18) -0.0007(12) 0.0159(14) -0.0006(12) C15 0.0277(16) 0.0346(17) 0.040(2) 0.0027(15) 0.0178(15) 0.0041(13) C16 0.0283(16) 0.0262(16) 0.0374(19) 0.0025(14) 0.0128(14) 0.0043(12) C17 0.0323(17) 0.0346(17) 0.0218(16) 0.0016(14) 0.0073(13) -0.0018(14) C18 0.0313(18) 0.0378(19) 0.0339(19) 0.0082(15) 0.0122(14) 0.0025(14) C19 0.0278(17) 0.050(2) 0.0312(19) 0.0147(16) 0.0080(14) 0.0004(15) C20 0.0284(18) 0.073(3) 0.0305(18) 0.0107(19) 0.0139(15) 0.0067(18) C21 0.0250(16) 0.053(2) 0.0271(17) 0.0039(16) 0.0096(13) 0.0065(15) C22 0.0229(15) 0.0415(18) 0.0232(16) 0.0034(14) 0.0077(12) 0.0015(13) C23 0.0288(16) 0.0352(18) 0.0226(16) -0.0059(13) 0.0102(13) -0.0039(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O11 2.256(2) . ? Cd1 O12 2.359(2) . ? Cd1 N1 2.363(3) . ? Cd1 N3 2.371(3) . ? Cd1 N4 2.540(3) . ? Cd1 N2 2.585(3) . ? Cl1 O5 1.414(3) . ? Cl1 O6 1.418(3) . ? Cl1 O4 1.429(3) . ? Cl1 O3 1.447(3) . ? Cl2 O8 1.418(3) . ? Cl2 O10 1.427(3) . ? Cl2 O7 1.442(3) . ? Cl2 O9 1.459(2) . ? O1 C12 1.360(4) . ? O1 C13 1.444(4) . ? O2 C17 1.362(4) . ? O2 C16 1.424(4) . ? N1 C1 1.336(4) . ? N1 C5 1.343(4) . ? N2 C6 1.278(4) . ? N2 C7 1.426(4) . ? N3 C15 1.479(4) . ? N3 C14 1.479(4) . ? N4 C23 1.263(4) . ? N4 C22 1.419(4) . ? C1 C2 1.389(4) . ? C1 C23 1.472(5) . ? C2 C3 1.394(5) . ? C3 C4 1.378(5) . ? C4 C5 1.400(4) . ? C5 C6 1.462(4) . ? C7 C8 1.392(4) . ? C7 C12 1.409(4) . ? C8 C9 1.386(5) . ? C9 C10 1.383(5) . ? C10 C11 1.384(5) . ? C11 C12 1.392(4) . ? C13 C14 1.521(5) . ? C15 C16 1.501(5) . ? C17 C18 1.393(5) . ? C17 C22 1.401(5) . ? C18 C19 1.386(5) . ? C19 C20 1.392(5) . ? C20 C21 1.396(5) . ? C21 C22 1.392(5) . ? 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 O11 Cd1 O12 177.71(9) . . ? O11 Cd1 N1 99.17(9) . . ? O12 Cd1 N1 80.46(9) . . ? O11 Cd1 N3 96.56(9) . . ? O12 Cd1 N3 83.52(8) . . ? N1 Cd1 N3 162.56(9) . . ? O11 Cd1 N4 83.64(9) . . ? O12 Cd1 N4 98.25(9) . . ? N1 Cd1 N4 66.80(9) . . ? N3 Cd1 N4 122.75(9) . . ? O11 Cd1 N2 93.97(8) . . ? O12 Cd1 N2 83.80(8) . . ? N1 Cd1 N2 67.45(8) . . ? N3 Cd1 N2 104.08(9) . . ? N4 Cd1 N2 133.12(8) . . ? O5 Cl1 O6 111.11(19) . . ? O5 Cl1 O4 109.9(2) . . ? O6 Cl1 O4 111.93(17) . . ? O5 Cl1 O3 106.4(2) . . ? O6 Cl1 O3 109.12(18) . . ? O4 Cl1 O3 108.2(2) . . ? O8 Cl2 O10 110.57(18) . . ? O8 Cl2 O7 109.79(17) . . ? O10 Cl2 O7 109.7(2) . . ? O8 Cl2 O9 110.15(17) . . ? O10 Cl2 O9 108.53(15) . . ? O7 Cl2 O9 108.00(17) . . ? C12 O1 C13 115.5(2) . . ? C17 O2 C16 119.4(3) . . ? C1 N1 C5 119.2(3) . . ? C1 N1 Cd1 120.6(2) . . ? C5 N1 Cd1 120.2(2) . . ? C6 N2 C7 118.7(3) . . ? C6 N2 Cd1 113.1(2) . . ? C7 N2 Cd1 128.22(18) . . ? C15 N3 C14 112.1(2) . . ? C15 N3 Cd1 114.7(2) . . ? C14 N3 Cd1 112.46(19) . . ? C23 N4 C22 121.4(3) . . ? C23 N4 Cd1 114.9(2) . . ? C22 N4 Cd1 123.7(2) . . ? N1 C1 C2 122.3(3) . . ? N1 C1 C23 116.3(3) . . ? C2 C1 C23 121.2(3) . . ? C1 C2 C3 119.0(3) . . ? C4 C3 C2 118.5(3) . . ? C3 C4 C5 119.6(3) . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 117.8(3) . . ? C4 C5 C6 120.7(3) . . ? N2 C6 C5 121.2(3) . . ? C8 C7 C12 118.5(3) . . ? C8 C7 N2 124.5(3) . . ? C12 C7 N2 116.9(3) . . ? C9 C8 C7 121.7(3) . . ? C10 C9 C8 118.5(3) . . ? C9 C10 C11 121.7(3) . . ? C10 C11 C12 119.4(3) . . ? O1 C12 C11 123.5(3) . . ? O1 C12 C7 116.4(3) . . ? C11 C12 C7 120.1(3) . . ? O1 C13 C14 105.3(2) . . ? N3 C14 C13 109.8(3) . . ? N3 C15 C16 111.7(3) . . ? O2 C16 C15 104.3(3) . . ? O2 C17 C18 125.2(3) . . ? O2 C17 C22 113.7(3) . . ? C18 C17 C22 121.1(3) . . ? C19 C18 C17 118.6(3) . . ? C18 C19 C20 121.4(3) . . ? C19 C20 C21 119.5(3) . . ? C22 C21 C20 120.2(3) . . ? C21 C22 C17 119.2(3) . . ? C21 C22 N4 124.6(3) . . ? C17 C22 N4 116.1(3) . . ? N4 C23 C1 120.2(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 O11 Cd1 N1 C1 -87.7(2) . . . . ? O12 Cd1 N1 C1 94.6(2) . . . . ? N3 Cd1 N1 C1 118.1(3) . . . . ? N4 Cd1 N1 C1 -8.7(2) . . . . ? N2 Cd1 N1 C1 -178.2(3) . . . . ? O11 Cd1 N1 C5 95.1(2) . . . . ? O12 Cd1 N1 C5 -82.6(2) . . . . ? N3 Cd1 N1 C5 -59.1(4) . . . . ? N4 Cd1 N1 C5 174.1(2) . . . . ? N2 Cd1 N1 C5 4.6(2) . . . . ? O11 Cd1 N2 C6 -102.0(2) . . . . ? O12 Cd1 N2 C6 78.5(2) . . . . ? N1 Cd1 N2 C6 -3.7(2) . . . . ? N3 Cd1 N2 C6 160.2(2) . . . . ? N4 Cd1 N2 C6 -17.0(3) . . . . ? O11 Cd1 N2 C7 79.5(2) . . . . ? O12 Cd1 N2 C7 -100.0(2) . . . . ? N1 Cd1 N2 C7 177.8(2) . . . . ? N3 Cd1 N2 C7 -18.3(2) . . . . ? N4 Cd1 N2 C7 164.5(2) . . . . ? O11 Cd1 N3 C15 115.7(2) . . . . ? O12 Cd1 N3 C15 -66.6(2) . . . . ? N1 Cd1 N3 C15 -89.9(4) . . . . ? N4 Cd1 N3 C15 29.1(2) . . . . ? N2 Cd1 N3 C15 -148.5(2) . . . . ? O11 Cd1 N3 C14 -13.9(2) . . . . ? O12 Cd1 N3 C14 163.8(2) . . . . ? N1 Cd1 N3 C14 140.5(3) . . . . ? N4 Cd1 N3 C14 -100.5(2) . . . . ? N2 Cd1 N3 C14 81.9(2) . . . . ? O11 Cd1 N4 C23 112.1(2) . . . . ? O12 Cd1 N4 C23 -66.6(2) . . . . ? N1 Cd1 N4 C23 9.2(2) . . . . ? N3 Cd1 N4 C23 -154.2(2) . . . . ? N2 Cd1 N4 C23 22.6(3) . . . . ? O11 Cd1 N4 C22 -70.7(2) . . . . ? O12 Cd1 N4 C22 110.6(2) . . . . ? N1 Cd1 N4 C22 -173.6(3) . . . . ? N3 Cd1 N4 C22 23.0(3) . . . . ? N2 Cd1 N4 C22 -160.2(2) . . . . ? C5 N1 C1 C2 1.1(5) . . . . ? Cd1 N1 C1 C2 -176.1(2) . . . . ? C5 N1 C1 C23 -175.0(3) . . . . ? Cd1 N1 C1 C23 7.8(4) . . . . ? N1 C1 C2 C3 -1.8(5) . . . . ? C23 C1 C2 C3 174.0(3) . . . . ? C1 C2 C3 C4 1.4(5) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C1 N1 C5 C4 0.2(4) . . . . ? Cd1 N1 C5 C4 177.4(2) . . . . ? C1 N1 C5 C6 177.6(3) . . . . ? Cd1 N1 C5 C6 -5.3(4) . . . . ? C3 C4 C5 N1 -0.6(5) . . . . ? C3 C4 C5 C6 -177.9(3) . . . . ? C7 N2 C6 C5 -178.6(3) . . . . ? Cd1 N2 C6 C5 2.7(4) . . . . ? N1 C5 C6 N2 1.4(5) . . . . ? C4 C5 C6 N2 178.8(3) . . . . ? C6 N2 C7 C8 -20.5(4) . . . . ? Cd1 N2 C7 C8 158.0(2) . . . . ? C6 N2 C7 C12 162.0(3) . . . . ? Cd1 N2 C7 C12 -19.5(4) . . . . ? C12 C7 C8 C9 -0.7(5) . . . . ? N2 C7 C8 C9 -178.2(3) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C8 C9 C10 C11 -1.3(5) . . . . ? C9 C10 C11 C12 1.2(5) . . . . ? C13 O1 C12 C11 -28.7(4) . . . . ? C13 O1 C12 C7 151.5(3) . . . . ? C10 C11 C12 O1 179.5(3) . . . . ? C10 C11 C12 C7 -0.8(5) . . . . ? C8 C7 C12 O1 -179.7(3) . . . . ? N2 C7 C12 O1 -2.0(4) . . . . ? C8 C7 C12 C11 0.6(4) . . . . ? N2 C7 C12 C11 178.2(3) . . . . ? C12 O1 C13 C14 -148.5(3) . . . . ? C15 N3 C14 C13 150.0(3) . . . . ? Cd1 N3 C14 C13 -79.1(3) . . . . ? O1 C13 C14 N3 52.6(3) . . . . ? C14 N3 C15 C16 68.7(4) . . . . ? Cd1 N3 C15 C16 -61.1(3) . . . . ? C17 O2 C16 C15 176.4(3) . . . . ? N3 C15 C16 O2 55.4(3) . . . . ? C16 O2 C17 C18 -1.9(5) . . . . ? C16 O2 C17 C22 179.6(3) . . . . ? O2 C17 C18 C19 -179.1(3) . . . . ? C22 C17 C18 C19 -0.7(5) . . . . ? C17 C18 C19 C20 0.8(5) . . . . ? C18 C19 C20 C21 0.1(5) . . . . ? C19 C20 C21 C22 -1.1(5) . . . . ? C20 C21 C22 C17 1.1(5) . . . . ? C20 C21 C22 N4 -176.0(3) . . . . ? O2 C17 C22 C21 178.4(3) . . . . ? C18 C17 C22 C21 -0.2(5) . . . . ? O2 C17 C22 N4 -4.3(4) . . . . ? C18 C17 C22 N4 177.2(3) . . . . ? C23 N4 C22 C21 -26.0(5) . . . . ? Cd1 N4 C22 C21 157.0(3) . . . . ? C23 N4 C22 C17 156.8(3) . . . . ? Cd1 N4 C22 C17 -20.2(4) . . . . ? C22 N4 C23 C1 173.5(3) . . . . ? Cd1 N4 C23 C1 -9.2(4) . . . . ? N1 C1 C23 N4 1.7(5) . . . . ? C2 C1 C23 N4 -174.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 28.66 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.870 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.139 data_60 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 10,16-dioxa-3,13,,23,29-tetraazatetraciclo[23.3.1.0^4,9^.0^17,22^] nonacosa-1(29),4(9),5,7,17,19,21,25,27-nonaene ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H28 N4 O3' _chemical_formula_weight 408.49 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 21.7074(3) _cell_length_b 12.1388(2) _cell_length_c 7.9913(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2105.72(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 1.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8461 _exptl_absorpt_correction_T_max 1.0000 _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 'SIEMENS CCD SMART ' _diffrn_measurement_method ' \w scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7640 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2338 _reflns_number_gt 1965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SIEMENS SMART' _computing_cell_refinement 'SIEMENS SMART' _computing_data_reduction 'SIEMENS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1998)' _computing_publication_material CIFTAB _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 w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.3349P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(14) _refine_ls_number_reflns 2338 _refine_ls_number_parameters 142 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.007 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.38531(6) 0.34437(11) 0.49397(17) 0.0602(3) Uani 1 d . . . OW O 0.5000 0.64322(14) 0.2560(3) 0.0644(5) Uani 1 d S . . N1 N 0.5000 0.13435(14) 0.8967(3) 0.0421(4) Uani 1 d S . . N2 N 0.38091(6) 0.20211(12) 0.7434(2) 0.0505(3) Uani 1 d . . . N3 N 0.5000 0.41459(16) 0.3426(3) 0.0510(5) Uani 1 d S . . C1 C 0.44696(6) 0.07796(12) 0.9040(2) 0.0428(3) Uani 1 d . . . C2 C 0.44544(8) -0.03545(14) 0.9219(3) 0.0577(4) Uani 1 d . . . H2 H 0.4080 -0.0726 0.9266 0.069 Uiso 1 calc R . . C3 C 0.5000 -0.0924(2) 0.9327(4) 0.0676(8) Uani 1 d S . . H3 H 0.5000 -0.1684 0.9471 0.081 Uiso 1 calc SR . . C4 C 0.38821(7) 0.14472(14) 0.9005(2) 0.0508(4) Uani 1 d . . . H4A H 0.3533 0.0961 0.9177 0.061 Uiso 1 calc R . . H4B H 0.3888 0.1978 0.9912 0.061 Uiso 1 calc R . . C5 C 0.33289(6) 0.27857(12) 0.7290(2) 0.0470(4) Uani 1 d . . . C6 C 0.33502(7) 0.35430(13) 0.5966(2) 0.0497(4) Uani 1 d . . . C7 C 0.28860(8) 0.43149(14) 0.5773(3) 0.0600(5) Uani 1 d . . . H7 H 0.2910 0.4833 0.4919 0.072 Uiso 1 calc R . . C8 C 0.23832(9) 0.43166(17) 0.6857(3) 0.0652(6) Uani 1 d . . . H8 H 0.2071 0.4833 0.6724 0.078 Uiso 1 calc R . . C9 C 0.23504(8) 0.35566(17) 0.8115(3) 0.0621(5) Uani 1 d . . . H9 H 0.2009 0.3544 0.8817 0.075 Uiso 1 calc R . . C10 C 0.28238(7) 0.28019(15) 0.8354(3) 0.0560(4) Uani 1 d . . . H10 H 0.2802 0.2303 0.9236 0.067 Uiso 1 calc R . . C11 C 0.38703(9) 0.41093(16) 0.3466(3) 0.0629(5) Uani 1 d . . . H11A H 0.3875 0.4884 0.3763 0.076 Uiso 1 calc R . . H11B H 0.3511 0.3968 0.2777 0.076 Uiso 1 calc R . . C12 C 0.44425(8) 0.38134(16) 0.2540(2) 0.0620(5) Uani 1 d . . . H12A H 0.4452 0.3023 0.2366 0.074 Uiso 1 calc R . . H12B H 0.4436 0.4165 0.1450 0.074 Uiso 1 calc R . . H2N H 0.4176 0.2325 0.7026 0.074 Uiso 1 d R . . H3N H 0.4999 0.3860 0.4530 0.074 Uiso 1 d SR . . H1W H 0.4999 0.6981 0.3521 0.093 Uiso 1 d SR . . H2W H 0.4999 0.5682 0.3085 0.093 Uiso 1 d SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0497(6) 0.0675(8) 0.0635(8) 0.0239(7) -0.0058(5) 0.0055(6) OW 0.0767(11) 0.0471(9) 0.0694(12) -0.0031(9) 0.000 0.000 N1 0.0371(7) 0.0381(8) 0.0511(11) 0.0104(8) 0.000 0.000 N2 0.0387(6) 0.0538(7) 0.0589(9) 0.0146(7) 0.0041(6) 0.0069(6) N3 0.0645(12) 0.0465(10) 0.0421(11) 0.0059(8) 0.000 0.000 C1 0.0391(6) 0.0460(7) 0.0434(8) 0.0097(7) 0.0006(6) -0.0017(6) C2 0.0500(8) 0.0454(8) 0.0777(12) 0.0128(8) -0.0005(8) -0.0117(7) C3 0.0694(15) 0.0332(11) 0.100(2) 0.0121(13) 0.000 0.000 C4 0.0381(6) 0.0568(9) 0.0575(10) 0.0122(8) 0.0039(7) 0.0012(6) C5 0.0372(7) 0.0423(8) 0.0614(10) -0.0005(7) -0.0079(7) -0.0001(6) C6 0.0423(7) 0.0477(8) 0.0590(10) 0.0012(8) -0.0154(7) -0.0005(6) C7 0.0583(9) 0.0510(9) 0.0706(12) -0.0010(9) -0.0271(9) 0.0067(8) C8 0.0537(9) 0.0606(11) 0.0814(14) -0.0202(10) -0.0247(10) 0.0173(8) C9 0.0433(8) 0.0662(11) 0.0768(13) -0.0151(10) -0.0038(8) 0.0081(8) C10 0.0430(8) 0.0544(9) 0.0706(12) -0.0006(8) -0.0015(8) 0.0021(7) C11 0.0657(10) 0.0612(11) 0.0618(12) 0.0206(9) -0.0216(9) -0.0034(9) C12 0.0811(12) 0.0601(10) 0.0447(10) 0.0060(9) -0.0140(9) -0.0054(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C6 1.371(2) . ? O1 C11 1.429(2) . ? N1 C1 1.3407(16) . ? N1 C1 1.3407(16) 4_655 ? N2 C5 1.4005(19) . ? N2 C4 1.444(2) . ? N3 C12 1.459(2) . ? N3 C12 1.459(2) 4_655 ? C1 C2 1.384(2) . ? C1 C4 1.511(2) . ? C2 C3 1.374(2) . ? C3 C2 1.374(2) 4_655 ? C5 C10 1.388(2) . ? C5 C6 1.402(2) . ? C6 C7 1.385(2) . ? C7 C8 1.393(3) . ? C8 C9 1.366(3) . ? C9 C10 1.390(2) . ? C11 C12 1.489(3) . ? 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 C6 O1 C11 117.67(14) . . ? C1 N1 C1 118.35(17) . 4_655 ? C5 N2 C4 118.24(14) . . ? C12 N3 C12 112.1(2) . 4_655 ? N1 C1 C2 122.19(14) . . ? N1 C1 C4 116.75(14) . . ? C2 C1 C4 121.00(14) . . ? C3 C2 C1 119.10(16) . . ? C2 C3 C2 119.1(2) . 4_655 ? N2 C4 C1 111.57(14) . . ? C10 C5 N2 123.14(16) . . ? C10 C5 C6 118.63(14) . . ? N2 C5 C6 118.18(14) . . ? O1 C6 C7 124.93(17) . . ? O1 C6 C5 114.83(13) . . ? C7 C6 C5 120.23(17) . . ? C6 C7 C8 120.13(19) . . ? C9 C8 C7 119.82(17) . . ? C8 C9 C10 120.50(19) . . ? C9 C10 C5 120.61(18) . . ? O1 C11 C12 107.14(15) . . ? N3 C12 C11 112.58(17) . . ? 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 C1 N1 C1 C2 1.3(3) 4_655 . . . ? C1 N1 C1 C4 178.28(13) 4_655 . . . ? N1 C1 C2 C3 0.0(3) . . . . ? C4 C1 C2 C3 -176.9(2) . . . . ? C1 C2 C3 C2 -1.3(5) . . . 4_655 ? C5 N2 C4 C1 -171.88(14) . . . . ? N1 C1 C4 N2 64.7(2) . . . . ? C2 C1 C4 N2 -118.28(19) . . . . ? C4 N2 C5 C10 -18.9(2) . . . . ? C4 N2 C5 C6 163.56(15) . . . . ? C11 O1 C6 C7 -6.7(3) . . . . ? C11 O1 C6 C5 173.41(16) . . . . ? C10 C5 C6 O1 -177.68(15) . . . . ? N2 C5 C6 O1 0.0(2) . . . . ? C10 C5 C6 C7 2.4(2) . . . . ? N2 C5 C6 C7 -179.95(16) . . . . ? O1 C6 C7 C8 177.66(16) . . . . ? C5 C6 C7 C8 -2.4(3) . . . . ? C6 C7 C8 C9 0.2(3) . . . . ? C7 C8 C9 C10 1.9(3) . . . . ? C8 C9 C10 C5 -1.9(3) . . . . ? N2 C5 C10 C9 -177.77(18) . . . . ? C6 C5 C10 C9 -0.2(3) . . . . ? C6 O1 C11 C12 -177.52(15) . . . . ? C12 N3 C12 C11 177.74(11) 4_655 . . . ? O1 C11 C12 N3 -67.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.498 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.498 _refine_diff_density_max 0.117 _refine_diff_density_min -0.152 _refine_diff_density_rms 0.036 data_ifn17a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H26 Cd N6 O8' _chemical_formula_weight 626.90 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.891(5) _cell_length_b 12.824(6) _cell_length_c 16.724(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.48(3) _cell_angle_gamma 90.00 _cell_volume 2457.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.5994 _exptl_absorpt_correction_T_max 0.7636 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5413 _diffrn_reflns_av_R_equivalents 0.0957 _diffrn_reflns_av_sigmaI/netI 0.0963 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4296 _reflns_number_gt 2736 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4296 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.2119 _refine_ls_wR_factor_gt 0.1715 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.28856(5) -0.22186(5) 1.04591(4) 0.0405(3) Uani 1 1 d . . . O1 O 0.5451(6) -0.2203(5) 1.2014(4) 0.0591(18) Uani 1 1 d . . . O2 O 0.2948(5) -0.2062(5) 0.8875(4) 0.0477(15) Uani 1 1 d . . . O3 O 0.3398(8) -0.0339(8) 1.0259(6) 0.104(3) Uani 1 1 d . . . O4 O 0.2476(10) -0.0496(8) 1.1164(6) 0.110(4) Uani 1 1 d . . . O5 O 0.3096(8) 0.1018(6) 1.0937(5) 0.079(2) Uani 1 1 d . . . O6 O 0.2486(6) -0.3935(6) 0.9908(5) 0.068(2) Uani 1 1 d . . . O7 O 0.3947(7) -0.4723(6) 1.0731(5) 0.074(2) Uani 1 1 d . . . O8 O 0.2861(8) -0.5534(6) 0.9682(5) 0.088(3) Uani 1 1 d . . . N1 N 0.1191(6) -0.2568(6) 1.0913(4) 0.0390(17) Uani 1 1 d . . . N2 N 0.1090(6) -0.1786(6) 0.9377(4) 0.0391(16) Uani 1 1 d . . . H2 H 0.0840 -0.2412 0.9139 0.047 Uiso 1 1 calc R . . N3 N 0.4783(7) -0.2576(7) 1.0328(5) 0.057(2) Uani 1 1 d . . . H3 H 0.4951 -0.3201 1.0590 0.069 Uiso 1 1 calc R . . N4 N 0.3401(6) -0.3032(6) 1.1908(4) 0.0433(18) Uani 1 1 d . . . H4 H 0.3999 -0.3483 1.1929 0.052 Uiso 1 1 calc R . . N5 N 0.2982(7) 0.0089(7) 1.0815(6) 0.059(2) Uani 1 1 d . . . N6 N 0.3095(7) -0.4750(6) 1.0100(5) 0.050(2) Uani 1 1 d . . . C1 C 0.0166(7) -0.2138(6) 1.0500(5) 0.0369(18) Uani 1 1 d . . . C2 C -0.0834(8) -0.2275(9) 1.0755(6) 0.058(3) Uani 1 1 d . . . H2A H -0.1536 -0.1976 1.0463 0.070 Uiso 1 1 calc R . . C3 C -0.0770(9) -0.2862(10) 1.1452(6) 0.064(3) Uani 1 1 d . . . H3A H -0.1431 -0.2965 1.1639 0.077 Uiso 1 1 calc R . . C4 C 0.0259(9) -0.3289(8) 1.1863(6) 0.052(2) Uani 1 1 d . . . H4A H 0.0305 -0.3681 1.2338 0.062 Uiso 1 1 calc R . . C5 C 0.1251(7) -0.3151(7) 1.1584(5) 0.041(2) Uani 1 1 d . . . C6 C 0.2388(8) -0.3676(7) 1.1961(5) 0.047(2) Uani 1 1 d . . . H6A H 0.2447 -0.3828 1.2539 0.057 Uiso 1 1 calc R . . H6B H 0.2411 -0.4334 1.1679 0.057 Uiso 1 1 calc R . . C7 C 0.3816(8) -0.2295(7) 1.2553(6) 0.046(2) Uani 1 1 d . . . C8 C 0.3244(9) -0.1994(8) 1.3129(6) 0.053(2) Uani 1 1 d . . . H8 H 0.2526 -0.2289 1.3117 0.063 Uiso 1 1 calc R . . C9 C 0.3726(11) -0.1252(9) 1.3729(6) 0.067(3) Uani 1 1 d . . . H9 H 0.3327 -0.1052 1.4113 0.080 Uiso 1 1 calc R . . C10 C 0.4797(11) -0.0810(9) 1.3757(6) 0.070(3) Uani 1 1 d . . . H10 H 0.5133 -0.0327 1.4166 0.084 Uiso 1 1 calc R . . C11 C 0.5364(10) -0.1102(8) 1.3162(7) 0.064(3) Uani 1 1 d . . . H11 H 0.6077 -0.0801 1.3165 0.077 Uiso 1 1 calc R . . C12 C 0.4886(9) -0.1814(8) 1.2584(5) 0.049(2) Uani 1 1 d . . . C13 C 0.5759(10) -0.1482(9) 1.1492(6) 0.068(3) Uani 1 1 d . . . H13A H 0.6516 -0.1186 1.1764 0.081 Uiso 1 1 calc R . . H13B H 0.5194 -0.0919 1.1379 0.081 Uiso 1 1 calc R . . C14 C 0.5809(9) -0.1960(10) 1.0711(7) 0.069(3) Uani 1 1 d . . . H14A H 0.6493 -0.2404 1.0811 0.083 Uiso 1 1 calc R . . H14B H 0.5895 -0.1417 1.0328 0.083 Uiso 1 1 calc R . . C15 C 0.4764(9) -0.2842(8) 0.9448(6) 0.057(3) Uani 1 1 d . . . H15A H 0.5561 -0.2900 0.9409 0.068 Uiso 1 1 calc R . . H15B H 0.4395 -0.3517 0.9310 0.068 Uiso 1 1 calc R . . C16 C 0.4141(8) -0.2068(8) 0.8836(6) 0.054(3) Uani 1 1 d . . . H16A H 0.4486 -0.1383 0.8969 0.064 Uiso 1 1 calc R . . H16B H 0.4183 -0.2257 0.8283 0.064 Uiso 1 1 calc R . . C17 C 0.2212(8) -0.1314(7) 0.8436(5) 0.042(2) Uani 1 1 d . . . C18 C 0.2373(10) -0.0768(8) 0.7762(6) 0.059(3) Uani 1 1 d . . . H18 H 0.3034 -0.0889 0.7578 0.070 Uiso 1 1 calc R . . C19 C 0.1569(9) -0.0055(9) 0.7367(6) 0.059(3) Uani 1 1 d . . . H19 H 0.1685 0.0309 0.6914 0.071 Uiso 1 1 calc R . . C20 C 0.0578(9) 0.0136(8) 0.7633(6) 0.061(3) Uani 1 1 d . . . H20 H 0.0038 0.0632 0.7365 0.073 Uiso 1 1 calc R . . C21 C 0.0397(8) -0.0413(8) 0.8296(5) 0.049(2) Uani 1 1 d . . . H21 H -0.0265 -0.0284 0.8476 0.059 Uiso 1 1 calc R . . C22 C 0.1195(7) -0.1152(7) 0.8695(5) 0.0361(19) Uani 1 1 d . . . C23 C 0.0159(7) -0.1464(7) 0.9757(5) 0.044(2) Uani 1 1 d . . . H23A H -0.0592 -0.1522 0.9351 0.053 Uiso 1 1 calc R . . H23B H 0.0273 -0.0741 0.9929 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0408(4) 0.0442(4) 0.0411(4) -0.0006(3) 0.0186(3) -0.0024(3) O1 0.077(5) 0.047(4) 0.061(4) 0.003(3) 0.032(4) 0.007(4) O2 0.049(4) 0.047(4) 0.053(4) 0.006(3) 0.023(3) 0.010(3) O3 0.101(7) 0.092(7) 0.128(8) -0.054(6) 0.047(6) 0.004(6) O4 0.161(9) 0.086(7) 0.084(6) 0.008(5) 0.034(6) -0.061(7) O5 0.122(7) 0.034(4) 0.095(6) -0.015(4) 0.054(5) -0.008(4) O6 0.051(4) 0.061(5) 0.081(5) -0.003(4) -0.001(4) 0.010(4) O7 0.077(5) 0.070(5) 0.063(5) -0.001(4) 0.000(4) 0.017(4) O8 0.117(7) 0.050(5) 0.087(6) -0.024(4) 0.011(5) -0.001(5) N1 0.038(4) 0.046(4) 0.035(4) 0.007(3) 0.013(3) -0.005(3) N2 0.047(4) 0.037(4) 0.036(4) -0.004(3) 0.017(3) -0.003(3) N3 0.044(4) 0.080(6) 0.052(5) -0.001(4) 0.019(4) 0.009(4) N4 0.041(4) 0.047(5) 0.037(4) 0.005(3) 0.001(3) 0.002(3) N5 0.058(5) 0.053(6) 0.062(5) -0.006(5) 0.008(4) 0.000(4) N6 0.064(5) 0.042(5) 0.050(5) 0.001(4) 0.027(4) -0.003(4) C1 0.034(4) 0.039(5) 0.038(4) 0.003(4) 0.010(3) 0.000(4) C2 0.042(5) 0.086(8) 0.053(5) 0.008(6) 0.025(4) 0.010(5) C3 0.048(5) 0.101(9) 0.051(6) 0.006(6) 0.025(5) -0.002(6) C4 0.070(6) 0.053(6) 0.044(5) 0.007(5) 0.034(5) 0.001(5) C5 0.037(4) 0.049(5) 0.040(5) -0.001(4) 0.016(4) -0.001(4) C6 0.058(6) 0.041(5) 0.044(5) 0.009(4) 0.015(4) -0.004(4) C7 0.054(5) 0.038(5) 0.046(5) 0.006(4) 0.011(4) 0.008(5) C8 0.063(6) 0.054(6) 0.047(5) 0.004(4) 0.026(5) 0.006(5) C9 0.087(8) 0.073(8) 0.041(5) 0.001(5) 0.019(5) 0.023(7) C10 0.096(9) 0.051(7) 0.048(6) -0.002(5) -0.009(6) 0.013(7) C11 0.078(7) 0.056(6) 0.058(6) 0.006(5) 0.016(6) -0.010(6) C12 0.063(6) 0.044(5) 0.037(5) 0.002(4) 0.010(4) 0.005(5) C13 0.067(7) 0.072(8) 0.064(7) -0.010(6) 0.018(5) -0.035(6) C14 0.049(6) 0.103(10) 0.061(6) -0.007(6) 0.023(5) -0.025(6) C15 0.052(5) 0.069(7) 0.055(6) 0.000(5) 0.022(5) 0.012(5) C16 0.056(5) 0.068(7) 0.048(5) 0.010(5) 0.032(5) 0.009(5) C17 0.051(5) 0.044(5) 0.029(4) -0.002(4) 0.006(4) -0.007(4) C18 0.076(7) 0.054(6) 0.053(6) 0.002(5) 0.029(5) -0.016(6) C19 0.069(7) 0.068(7) 0.040(5) 0.011(5) 0.012(5) -0.009(6) C20 0.065(7) 0.051(6) 0.055(6) 0.017(5) -0.005(5) -0.007(5) C21 0.049(5) 0.053(6) 0.040(5) 0.006(4) 0.004(4) 0.002(5) C22 0.042(4) 0.039(5) 0.027(4) -0.004(3) 0.008(3) -0.009(4) C23 0.045(5) 0.047(5) 0.043(5) 0.005(4) 0.015(4) 0.000(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 Cd1 N3 2.370(7) . ? Cd1 N1 2.378(6) . ? Cd1 O6 2.385(8) . ? Cd1 N2 2.466(7) . ? Cd1 O3 2.530(11) . ? Cd1 N4 2.558(7) . ? Cd1 O4 2.610(11) . ? O1 C13 1.388(12) . ? O1 C12 1.396(11) . ? O2 C17 1.371(10) . ? O2 C16 1.438(10) . ? O3 N5 1.287(11) . ? O4 N5 1.204(11) . ? O5 N5 1.211(11) . ? O6 N6 1.263(10) . ? O7 N6 1.253(10) . ? O8 N6 1.215(11) . ? N1 C5 1.335(11) . ? N1 C1 1.349(11) . ? N2 C22 1.434(10) . ? N2 C23 1.475(10) . ? N3 C14 1.450(13) . ? N3 C15 1.505(12) . ? N4 C7 1.420(12) . ? N4 C6 1.482(11) . ? C1 C2 1.378(12) . ? C1 C23 1.512(11) . ? C2 C3 1.371(14) . ? C3 C4 1.350(14) . ? C4 C5 1.391(12) . ? C5 C6 1.491(12) . ? C7 C8 1.375(13) . ? C7 C12 1.403(13) . ? C8 C9 1.391(15) . ? C9 C10 1.382(16) . ? C10 C11 1.396(15) . ? C11 C12 1.341(14) . ? C13 C14 1.458(14) . ? C15 C16 1.476(14) . ? C17 C18 1.382(12) . ? C17 C22 1.405(11) . ? C18 C19 1.361(15) . ? C19 C20 1.388(14) . ? C20 C21 1.378(13) . ? C21 C22 1.381(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 N1 154.4(3) . . ? N3 Cd1 O6 83.2(3) . . ? N1 Cd1 O6 81.4(3) . . ? N3 Cd1 N2 129.4(2) . . ? N1 Cd1 N2 68.6(2) . . ? O6 Cd1 N2 83.1(2) . . ? N3 Cd1 O3 84.4(3) . . ? N1 Cd1 O3 118.5(3) . . ? O6 Cd1 O3 149.1(3) . . ? N2 Cd1 O3 83.1(3) . . ? N3 Cd1 N4 90.9(3) . . ? N1 Cd1 N4 68.3(2) . . ? O6 Cd1 N4 87.8(3) . . ? N2 Cd1 N4 136.8(2) . . ? O3 Cd1 N4 120.6(3) . . ? N3 Cd1 O4 120.2(3) . . ? N1 Cd1 O4 74.9(3) . . ? O6 Cd1 O4 156.0(3) . . ? N2 Cd1 O4 84.9(3) . . ? O3 Cd1 O4 48.2(3) . . ? N4 Cd1 O4 86.8(3) . . ? C13 O1 C12 116.6(8) . . ? C17 O2 C16 118.4(7) . . ? N5 O3 Cd1 99.1(7) . . ? N5 O4 Cd1 97.5(7) . . ? N6 O6 Cd1 128.6(6) . . ? C5 N1 C1 119.9(7) . . ? C5 N1 Cd1 121.0(5) . . ? C1 N1 Cd1 119.1(5) . . ? C22 N2 C23 114.8(7) . . ? C22 N2 Cd1 118.0(5) . . ? C23 N2 Cd1 110.4(5) . . ? C14 N3 C15 110.3(8) . . ? C14 N3 Cd1 124.3(7) . . ? C15 N3 Cd1 111.6(6) . . ? C7 N4 C6 116.7(7) . . ? C7 N4 Cd1 113.2(5) . . ? C6 N4 Cd1 106.9(5) . . ? O4 N5 O5 125.4(10) . . ? O4 N5 O3 115.0(10) . . ? O5 N5 O3 119.6(10) . . ? O8 N6 O7 121.2(9) . . ? O8 N6 O6 120.7(9) . . ? O7 N6 O6 118.1(8) . . ? N1 C1 C2 121.8(8) . . ? N1 C1 C23 117.4(7) . . ? C2 C1 C23 120.8(8) . . ? C1 C2 C3 118.4(9) . . ? C4 C3 C2 119.5(9) . . ? C3 C4 C5 120.8(9) . . ? N1 C5 C4 119.5(8) . . ? N1 C5 C6 116.6(7) . . ? C4 C5 C6 123.8(8) . . ? N4 C6 C5 112.5(7) . . ? C8 C7 C12 117.6(9) . . ? C8 C7 N4 125.7(9) . . ? C12 C7 N4 116.7(8) . . ? C7 C8 C9 120.9(10) . . ? C10 C9 C8 120.2(10) . . ? C9 C10 C11 118.8(10) . . ? C12 C11 C10 120.3(11) . . ? C11 C12 O1 123.1(10) . . ? C11 C12 C7 122.2(9) . . ? O1 C12 C7 114.5(8) . . ? O1 C13 C14 111.4(9) . . ? C13 C14 N3 113.2(8) . . ? C16 C15 N3 113.5(8) . . ? O2 C16 C15 106.9(7) . . ? O2 C17 C18 125.7(9) . . ? O2 C17 C22 114.6(7) . . ? C18 C17 C22 119.6(9) . . ? C19 C18 C17 120.3(10) . . ? C18 C19 C20 120.6(9) . . ? C21 C20 C19 119.8(10) . . ? C20 C21 C22 120.3(9) . . ? C21 C22 C17 119.3(8) . . ? C21 C22 N2 125.4(8) . . ? C17 C22 N2 115.3(7) . . ? N2 C23 C1 110.8(7) . . ? 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 N3 Cd1 O3 N5 -137.4(7) . . . . ? N1 Cd1 O3 N5 30.6(8) . . . . ? O6 Cd1 O3 N5 155.8(6) . . . . ? N2 Cd1 O3 N5 91.7(6) . . . . ? N4 Cd1 O3 N5 -49.7(7) . . . . ? O4 Cd1 O3 N5 2.4(6) . . . . ? N3 Cd1 O4 N5 45.5(8) . . . . ? N1 Cd1 O4 N5 -157.0(8) . . . . ? O6 Cd1 O4 N5 -148.1(7) . . . . ? N2 Cd1 O4 N5 -87.9(7) . . . . ? O3 Cd1 O4 N5 -2.5(6) . . . . ? N4 Cd1 O4 N5 134.6(7) . . . . ? N3 Cd1 O6 N6 44.0(8) . . . . ? N1 Cd1 O6 N6 -115.5(8) . . . . ? N2 Cd1 O6 N6 175.2(8) . . . . ? O3 Cd1 O6 N6 111.1(9) . . . . ? N4 Cd1 O6 N6 -47.2(8) . . . . ? O4 Cd1 O6 N6 -124.3(8) . . . . ? N3 Cd1 N1 C5 25.8(10) . . . . ? O6 Cd1 N1 C5 79.5(7) . . . . ? N2 Cd1 N1 C5 165.4(7) . . . . ? O3 Cd1 N1 C5 -125.6(7) . . . . ? N4 Cd1 N1 C5 -11.6(6) . . . . ? O4 Cd1 N1 C5 -104.2(7) . . . . ? N3 Cd1 N1 C1 -156.6(6) . . . . ? O6 Cd1 N1 C1 -102.9(6) . . . . ? N2 Cd1 N1 C1 -17.0(6) . . . . ? O3 Cd1 N1 C1 52.0(7) . . . . ? N4 Cd1 N1 C1 166.0(7) . . . . ? O4 Cd1 N1 C1 73.5(6) . . . . ? N3 Cd1 N2 C22 -36.3(7) . . . . ? N1 Cd1 N2 C22 164.9(6) . . . . ? O6 Cd1 N2 C22 -111.6(6) . . . . ? O3 Cd1 N2 C22 40.7(6) . . . . ? N4 Cd1 N2 C22 169.0(5) . . . . ? O4 Cd1 N2 C22 89.2(6) . . . . ? N3 Cd1 N2 C23 -171.1(5) . . . . ? N1 Cd1 N2 C23 30.1(5) . . . . ? O6 Cd1 N2 C23 113.6(6) . . . . ? O3 Cd1 N2 C23 -94.1(6) . . . . ? N4 Cd1 N2 C23 34.2(7) . . . . ? O4 Cd1 N2 C23 -45.7(6) . . . . ? N1 Cd1 N3 C14 -112.8(10) . . . . ? O6 Cd1 N3 C14 -166.1(9) . . . . ? N2 Cd1 N3 C14 118.6(8) . . . . ? O3 Cd1 N3 C14 42.2(8) . . . . ? N4 Cd1 N3 C14 -78.4(8) . . . . ? O4 Cd1 N3 C14 8.4(9) . . . . ? N1 Cd1 N3 C15 111.1(8) . . . . ? O6 Cd1 N3 C15 57.7(7) . . . . ? N2 Cd1 N3 C15 -17.6(8) . . . . ? O3 Cd1 N3 C15 -94.0(7) . . . . ? N4 Cd1 N3 C15 145.4(7) . . . . ? O4 Cd1 N3 C15 -127.8(7) . . . . ? N3 Cd1 N4 C7 92.9(6) . . . . ? N1 Cd1 N4 C7 -102.3(6) . . . . ? O6 Cd1 N4 C7 176.1(6) . . . . ? N2 Cd1 N4 C7 -106.4(6) . . . . ? O3 Cd1 N4 C7 8.8(7) . . . . ? O4 Cd1 N4 C7 -27.3(6) . . . . ? N3 Cd1 N4 C6 -137.2(6) . . . . ? N1 Cd1 N4 C6 27.6(5) . . . . ? O6 Cd1 N4 C6 -54.0(6) . . . . ? N2 Cd1 N4 C6 23.5(7) . . . . ? O3 Cd1 N4 C6 138.7(5) . . . . ? O4 Cd1 N4 C6 102.6(6) . . . . ? Cd1 O4 N5 O5 -177.6(10) . . . . ? Cd1 O4 N5 O3 4.1(10) . . . . ? Cd1 O3 N5 O4 -4.3(10) . . . . ? Cd1 O3 N5 O5 177.4(8) . . . . ? Cd1 O6 N6 O8 -169.2(7) . . . . ? Cd1 O6 N6 O7 10.6(12) . . . . ? C5 N1 C1 C2 0.6(13) . . . . ? Cd1 N1 C1 C2 -177.1(7) . . . . ? C5 N1 C1 C23 178.5(8) . . . . ? Cd1 N1 C1 C23 0.9(10) . . . . ? N1 C1 C2 C3 0.3(16) . . . . ? C23 C1 C2 C3 -177.6(9) . . . . ? C1 C2 C3 C4 -0.2(17) . . . . ? C2 C3 C4 C5 -0.7(17) . . . . ? C1 N1 C5 C4 -1.5(13) . . . . ? Cd1 N1 C5 C4 176.1(7) . . . . ? C1 N1 C5 C6 174.7(8) . . . . ? Cd1 N1 C5 C6 -7.7(11) . . . . ? C3 C4 C5 N1 1.6(15) . . . . ? C3 C4 C5 C6 -174.3(10) . . . . ? C7 N4 C6 C5 85.9(9) . . . . ? Cd1 N4 C6 C5 -42.0(8) . . . . ? N1 C5 C6 N4 35.7(11) . . . . ? C4 C5 C6 N4 -148.3(9) . . . . ? C6 N4 C7 C8 -12.7(13) . . . . ? Cd1 N4 C7 C8 112.1(9) . . . . ? C6 N4 C7 C12 169.4(8) . . . . ? Cd1 N4 C7 C12 -65.8(9) . . . . ? C12 C7 C8 C9 -1.2(14) . . . . ? N4 C7 C8 C9 -179.1(9) . . . . ? C7 C8 C9 C10 -0.4(16) . . . . ? C8 C9 C10 C11 1.7(16) . . . . ? C9 C10 C11 C12 -1.4(16) . . . . ? C10 C11 C12 O1 -174.6(9) . . . . ? C10 C11 C12 C7 -0.3(15) . . . . ? C13 O1 C12 C11 -59.7(13) . . . . ? C13 O1 C12 C7 125.6(9) . . . . ? C8 C7 C12 C11 1.6(14) . . . . ? N4 C7 C12 C11 179.7(9) . . . . ? C8 C7 C12 O1 176.3(8) . . . . ? N4 C7 C12 O1 -5.6(12) . . . . ? C12 O1 C13 C14 -152.7(9) . . . . ? O1 C13 C14 N3 49.1(14) . . . . ? C15 N3 C14 C13 167.3(10) . . . . ? Cd1 N3 C14 C13 30.6(14) . . . . ? C14 N3 C15 C16 -90.6(11) . . . . ? Cd1 N3 C15 C16 51.8(10) . . . . ? C17 O2 C16 C15 172.2(8) . . . . ? N3 C15 C16 O2 -62.6(11) . . . . ? C16 O2 C17 C18 21.6(13) . . . . ? C16 O2 C17 C22 -161.4(8) . . . . ? O2 C17 C18 C19 178.8(9) . . . . ? C22 C17 C18 C19 2.0(14) . . . . ? C17 C18 C19 C20 0.0(16) . . . . ? C18 C19 C20 C21 -1.0(16) . . . . ? C19 C20 C21 C22 -0.2(15) . . . . ? C20 C21 C22 C17 2.2(13) . . . . ? C20 C21 C22 N2 -178.6(9) . . . . ? O2 C17 C22 C21 179.7(8) . . . . ? C18 C17 C22 C21 -3.1(13) . . . . ? O2 C17 C22 N2 0.4(10) . . . . ? C18 C17 C22 N2 177.6(8) . . . . ? C23 N2 C22 C21 -11.5(12) . . . . ? Cd1 N2 C22 C21 -144.5(7) . . . . ? C23 N2 C22 C17 167.7(7) . . . . ? Cd1 N2 C22 C17 34.8(9) . . . . ? C22 N2 C23 C1 -176.6(7) . . . . ? Cd1 N2 C23 C1 -40.2(8) . . . . ? N1 C1 C23 N2 27.4(11) . . . . ? C2 C1 C23 N2 -154.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.832 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.135 data_ifn21 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Cl3 N9 O17 Zn2' _chemical_formula_weight 1260.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/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 19.5154(10) _cell_length_b 12.2075(6) _cell_length_c 22.3744(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.8220(10) _cell_angle_gamma 90.00 _cell_volume 5292.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6402 _exptl_absorpt_correction_T_max 0.8478 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34249 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 28.37 _reflns_number_total 12571 _reflns_number_gt 7455 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0980P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12571 _refine_ls_number_parameters 760 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1337 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.875 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.733710(19) 0.98489(3) 0.190147(17) 0.04271(12) Uani 1 1 d . . . Zn2 Zn 0.697348(19) 0.95156(3) 0.343133(16) 0.04322(12) Uani 1 1 d . . . O1 O 0.59194(13) 1.0311(2) 0.15507(12) 0.0600(7) Uani 1 1 d . . . O2 O 0.75088(11) 1.20219(19) 0.22984(11) 0.0509(6) Uani 1 1 d . . . O3 O 0.65230(12) 0.73809(19) 0.30296(11) 0.0549(6) Uani 1 1 d . . . O4 O 0.55868(13) 1.0395(2) 0.31891(11) 0.0570(6) Uani 1 1 d . . . O5 O 0.68376(11) 0.96786(17) 0.25766(9) 0.0433(5) Uani 1 1 d . . . H5A H 0.6367 0.9673 0.2445 0.052 Uiso 1 1 calc R . . O6A O 0.7064(6) 0.9954(14) 0.5479(7) 0.458(11) Uani 1 1 d U A 1 O7A O 0.5791(4) 0.9985(7) 0.5228(3) 0.102(3) Uani 0.536(9) 1 d P A 1 O7B O 0.6692(9) 0.9453(5) 0.5249(3) 0.162(8) Uani 0.464(9) 1 d PU A 2 O8A O 0.6293(5) 1.0704(9) 0.6063(4) 0.125(3) Uiso 0.536(9) 1 d PU A 1 O8B O 0.6494(5) 1.0120(8) 0.6123(4) 0.097(3) Uiso 0.464(9) 1 d PU A 2 O9 O 0.6551(3) 1.1305(3) 0.5187(3) 0.1512(19) Uani 1 1 d . A . O10 O 1.0376(4) 0.7332(7) 0.3056(4) 0.234(3) Uani 1 1 d . B . O11A O 1.0756(18) 0.935(2) 0.3600(8) 0.227(16) Uani 0.300(14) 1 d PU B 1 O11B O 1.0899(3) 0.8186(9) 0.3739(3) 0.149(5) Uani 0.700(14) 1 d PU B 2 O12A O 0.9698(9) 0.837(2) 0.3352(15) 0.112(10) Uani 0.300(14) 1 d PU B 1 O12B O 0.9807(6) 0.8651(13) 0.3565(8) 0.175(6) Uani 0.700(14) 1 d PU B 2 O13 O 1.0470(2) 0.9042(5) 0.2794(3) 0.159(2) Uani 1 1 d . B . O14 O 0.7343(5) 1.0314(8) -0.0746(5) 0.305(6) Uani 1 1 d . C . O15 O 0.8125(4) 0.9231(7) -0.0636(4) 0.251(4) Uani 1 1 d . C . O16A O 0.8188(10) 1.032(3) 0.0151(13) 0.220(12) Uani 0.46(2) 1 d PU C 1 O16B O 0.7958(12) 1.0879(9) -0.0129(8) 0.177(8) Uani 0.54(2) 1 d PU C 2 O17A O 0.7149(11) 0.9461(13) -0.0079(8) 0.146(9) Uani 0.46(2) 1 d PU C 1 O17B O 0.7700(13) 0.9226(10) 0.0131(7) 0.187(7) Uani 0.54(2) 1 d PU C 2 N1 N 0.80085(13) 0.8635(2) 0.16560(12) 0.0438(6) Uani 1 1 d . . . N2 N 0.83708(14) 1.0258(2) 0.24067(12) 0.0457(6) Uani 1 1 d . . . N3 N 0.73025(15) 1.0898(2) 0.11739(13) 0.0500(7) Uani 1 1 d . . . H3 H 0.7481 1.0493 0.0888 0.060 Uiso 1 1 calc R . . N4 N 0.66662(13) 0.8560(2) 0.12455(12) 0.0433(6) Uani 1 1 d . . . N5 N 0.77981(14) 1.0038(2) 0.40605(12) 0.0468(6) Uani 1 1 d . . . N6 N 0.67943(14) 1.1352(2) 0.36358(13) 0.0476(6) Uani 1 1 d . . . N7 N 0.63195(14) 0.8784(2) 0.40019(13) 0.0486(7) Uani 1 1 d . . . H7 H 0.6445 0.9105 0.4366 0.058 Uiso 1 1 calc R . . N8 N 0.77849(14) 0.8166(2) 0.34796(13) 0.0473(6) Uani 1 1 d . . . C1 C 0.86765(17) 0.8717(3) 0.18624(16) 0.0501(8) Uani 1 1 d . . . C2 C 0.9164(2) 0.7988(3) 0.16822(19) 0.0653(10) Uani 1 1 d . . . H2 H 0.9630 0.8057 0.1824 0.078 Uiso 1 1 calc R . . C3 C 0.8936(2) 0.7163(4) 0.1288(2) 0.0744(12) Uani 1 1 d . . . H3A H 0.9250 0.6663 0.1164 0.089 Uiso 1 1 calc R . . C4 C 0.8249(2) 0.7075(3) 0.10783(19) 0.0673(11) Uani 1 1 d . . . H4 H 0.8091 0.6520 0.0812 0.081 Uiso 1 1 calc R . . C5 C 0.77926(17) 0.7835(3) 0.12717(16) 0.0475(8) Uani 1 1 d . . . C6 C 0.70485(18) 0.7836(3) 0.10650(16) 0.0524(8) Uani 1 1 d . . . H6 H 0.6861 0.7299 0.0800 0.063 Uiso 1 1 calc R . . C7 C 0.59531(16) 0.8614(3) 0.10255(15) 0.0474(8) Uani 1 1 d . . . C8 C 0.5598(2) 0.7790(3) 0.06766(17) 0.0604(9) Uani 1 1 d . . . H8 H 0.5827 0.7149 0.0594 0.073 Uiso 1 1 calc R . . C9 C 0.4914(2) 0.7925(4) 0.04569(19) 0.0693(11) Uani 1 1 d . . . H9 H 0.4682 0.7374 0.0228 0.083 Uiso 1 1 calc R . . C10 C 0.4574(2) 0.8875(5) 0.05748(19) 0.0777(13) Uani 1 1 d . . . H10 H 0.4114 0.8969 0.0418 0.093 Uiso 1 1 calc R . . C11 C 0.4908(2) 0.9682(4) 0.09211(19) 0.0691(11) Uani 1 1 d . . . H11 H 0.4675 1.0321 0.1000 0.083 Uiso 1 1 calc R . . C12 C 0.55959(18) 0.9547(3) 0.11546(16) 0.0524(8) Uani 1 1 d . . . C13 C 0.6072(2) 1.1356(3) 0.1285(2) 0.0768(13) Uani 1 1 d . . . H13A H 0.6232 1.1870 0.1601 0.092 Uiso 1 1 calc R . . H13B H 0.5655 1.1650 0.1064 0.092 Uiso 1 1 calc R . . C14 C 0.6603(2) 1.1230(3) 0.08757(19) 0.0661(11) Uani 1 1 d . . . H14A H 0.6648 1.1920 0.0669 0.079 Uiso 1 1 calc R . . H14B H 0.6447 1.0686 0.0574 0.079 Uiso 1 1 calc R . . C15 C 0.7791(2) 1.1844(3) 0.12774(17) 0.0590(9) Uani 1 1 d . . . H15A H 0.7801 1.2241 0.0903 0.071 Uiso 1 1 calc R . . H15B H 0.8252 1.1569 0.1402 0.071 Uiso 1 1 calc R . . C16 C 0.7585(2) 1.2611(3) 0.17490(18) 0.0628(10) Uani 1 1 d . . . H16A H 0.7934 1.3176 0.1830 0.075 Uiso 1 1 calc R . . H16B H 0.7153 1.2965 0.1602 0.075 Uiso 1 1 calc R . . C17 C 0.80726(17) 1.2060(3) 0.27261(15) 0.0480(8) Uani 1 1 d . . . C18 C 0.8201(2) 1.2973(3) 0.30887(18) 0.0588(9) Uani 1 1 d . . . H18 H 0.7920 1.3587 0.3024 0.071 Uiso 1 1 calc R . . C19 C 0.8741(2) 1.2981(4) 0.35430(18) 0.0673(11) Uani 1 1 d . . . H19 H 0.8821 1.3595 0.3788 0.081 Uiso 1 1 calc R . . C20 C 0.9165(2) 1.2075(4) 0.36352(18) 0.0657(11) Uani 1 1 d . . . H20 H 0.9526 1.2078 0.3946 0.079 Uiso 1 1 calc R . . C21 C 0.90566(18) 1.1171(3) 0.32716(17) 0.0576(9) Uani 1 1 d . . . H21 H 0.9346 1.0566 0.3336 0.069 Uiso 1 1 calc R . . C22 C 0.85129(17) 1.1157(3) 0.28042(15) 0.0470(8) Uani 1 1 d . . . C23 C 0.88563(17) 0.9634(3) 0.22779(16) 0.0507(8) Uani 1 1 d . . . H23 H 0.9311 0.9754 0.2442 0.061 Uiso 1 1 calc R . . C24 C 0.77833(18) 1.1027(3) 0.43107(16) 0.0519(8) Uani 1 1 d . . . C25 C 0.8289(2) 1.1342(4) 0.47719(18) 0.0670(11) Uani 1 1 d . . . H25 H 0.8280 1.2035 0.4943 0.080 Uiso 1 1 calc R . . C26 C 0.8809(2) 1.0598(4) 0.49709(19) 0.0751(12) Uani 1 1 d . . . H26 H 0.9142 1.0782 0.5288 0.090 Uiso 1 1 calc R . . C27 C 0.8828(2) 0.9596(4) 0.46981(18) 0.0672(11) Uani 1 1 d . . . H27 H 0.9183 0.9106 0.4815 0.081 Uiso 1 1 calc R . . C28 C 0.83049(17) 0.9324(3) 0.42417(16) 0.0526(8) Uani 1 1 d . . . C29 C 0.82859(18) 0.8308(3) 0.38938(17) 0.0546(9) Uani 1 1 d . . . H29 H 0.8629 0.7780 0.3972 0.066 Uiso 1 1 calc R . . C30 C 0.77532(19) 0.7254(3) 0.30873(16) 0.0534(9) Uani 1 1 d . . . C31 C 0.8333(2) 0.6747(3) 0.29101(19) 0.0668(11) Uani 1 1 d . . . H31 H 0.8771 0.6974 0.3072 0.080 Uiso 1 1 calc R . . C32 C 0.8261(3) 0.5908(4) 0.2494(2) 0.0837(14) Uani 1 1 d . . . H32 H 0.8647 0.5556 0.2379 0.100 Uiso 1 1 calc R . . C33 C 0.7600(3) 0.5594(4) 0.2249(2) 0.0874(15) Uani 1 1 d . . . H33 H 0.7549 0.5038 0.1964 0.105 Uiso 1 1 calc R . . C34 C 0.7032(2) 0.6081(3) 0.24183(19) 0.0677(11) Uani 1 1 d . . . H34 H 0.6595 0.5866 0.2247 0.081 Uiso 1 1 calc R . . C35 C 0.7104(2) 0.6898(3) 0.28469(17) 0.0535(8) Uani 1 1 d . . . C36 C 0.6290(2) 0.6906(3) 0.35515(18) 0.0643(10) Uani 1 1 d . . . H36A H 0.6493 0.6183 0.3616 0.077 Uiso 1 1 calc R . . H36B H 0.5793 0.6820 0.3485 0.077 Uiso 1 1 calc R . . C37 C 0.6481(2) 0.7601(3) 0.41105(18) 0.0618(10) Uani 1 1 d . . . H37A H 0.6232 0.7337 0.4432 0.074 Uiso 1 1 calc R . . H37B H 0.6971 0.7522 0.4241 0.074 Uiso 1 1 calc R . . C38 C 0.55593(19) 0.8954(3) 0.38950(19) 0.0613(10) Uani 1 1 d . . . H38A H 0.5369 0.8510 0.3556 0.074 Uiso 1 1 calc R . . H38B H 0.5353 0.8713 0.4246 0.074 Uiso 1 1 calc R . . C39 C 0.5376(2) 1.0121(3) 0.37704(19) 0.0618(10) Uani 1 1 d . . . H39A H 0.4883 1.0226 0.3765 0.074 Uiso 1 1 calc R . . H39B H 0.5611 1.0588 0.4080 0.074 Uiso 1 1 calc R . . C40 C 0.56559(19) 1.1515(3) 0.31019(16) 0.0541(8) Uani 1 1 d . . . C41 C 0.5116(2) 1.2092(4) 0.28011(19) 0.0724(12) Uani 1 1 d . . . H41 H 0.4703 1.1743 0.2667 0.087 Uiso 1 1 calc R . . C42 C 0.5198(3) 1.3207(5) 0.2701(2) 0.0884(15) Uani 1 1 d . . . H42 H 0.4837 1.3612 0.2501 0.106 Uiso 1 1 calc R . . C43 C 0.5815(3) 1.3707(4) 0.2898(2) 0.0855(15) Uani 1 1 d . . . H43 H 0.5872 1.4447 0.2819 0.103 Uiso 1 1 calc R . . C44 C 0.6349(2) 1.3135(4) 0.3211(2) 0.0749(12) Uani 1 1 d . . . H44 H 0.6761 1.3488 0.3344 0.090 Uiso 1 1 calc R . . C45 C 0.62691(19) 1.2017(3) 0.33296(16) 0.0531(8) Uani 1 1 d . . . C46 C 0.72278(18) 1.1745(3) 0.40468(16) 0.0538(9) Uani 1 1 d . . . H46 H 0.7194 1.2464 0.4176 0.065 Uiso 1 1 calc R . . Cl1 Cl 0.64834(6) 1.03551(8) 0.55037(5) 0.0682(3) Uani 1 1 d . . . Cl2 Cl 1.03871(6) 0.84461(13) 0.33132(6) 0.0904(4) Uani 1 1 d . . . Cl3 Cl 0.77674(7) 0.98623(9) -0.03130(5) 0.0770(3) Uani 1 1 d . . . C1S C 0.9912(5) 1.4328(6) 0.5783(4) 0.157(3) Uani 1 1 d . . . H1S1 H 1.0282 1.4850 0.5808 0.236 Uiso 1 1 calc R . . H1S2 H 0.9891 1.4006 0.6172 0.236 Uiso 1 1 calc R . . H1S3 H 0.9483 1.4690 0.5653 0.236 Uiso 1 1 calc R . . C2S C 1.0034(4) 1.3461(6) 0.5347(3) 0.113(2) Uani 1 1 d . . . N1S N 1.0121(3) 1.2821(6) 0.5010(3) 0.139(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0463(2) 0.0445(2) 0.0387(2) 0.00251(16) 0.01067(16) 0.00537(15) Zn2 0.0453(2) 0.0498(2) 0.0348(2) -0.00083(15) 0.00593(15) -0.00531(15) O1 0.0581(15) 0.0652(17) 0.0540(15) -0.0139(13) -0.0039(12) 0.0136(12) O2 0.0509(13) 0.0488(13) 0.0532(14) -0.0013(11) 0.0071(11) -0.0037(10) O3 0.0616(15) 0.0501(14) 0.0532(14) 0.0025(11) 0.0071(12) -0.0061(11) O4 0.0575(14) 0.0637(16) 0.0501(15) -0.0061(12) 0.0075(12) -0.0030(11) O5 0.0410(11) 0.0551(13) 0.0339(11) 0.0011(9) 0.0054(9) -0.0015(9) O6A 0.258(10) 0.65(2) 0.52(2) 0.400(18) 0.250(12) 0.282(13) O7A 0.089(5) 0.157(7) 0.055(4) -0.010(4) -0.006(3) -0.046(5) O7B 0.41(2) 0.015(3) 0.046(4) -0.015(3) -0.047(7) 0.036(6) O9 0.212(5) 0.075(3) 0.178(5) 0.030(3) 0.074(4) 0.011(3) O10 0.312(10) 0.173(6) 0.235(8) -0.019(6) 0.099(7) 0.016(6) O11A 0.37(3) 0.21(2) 0.086(11) -0.005(12) -0.036(16) -0.21(2) O11B 0.088(4) 0.254(12) 0.096(5) -0.036(6) -0.030(3) 0.083(6) O12A 0.037(7) 0.129(14) 0.17(2) 0.050(13) 0.007(9) -0.035(9) O12B 0.143(10) 0.215(12) 0.188(13) 0.098(10) 0.103(9) 0.113(8) O13 0.101(3) 0.219(6) 0.163(5) 0.075(4) 0.035(3) -0.019(3) O14 0.282(10) 0.227(9) 0.373(14) 0.122(10) -0.099(10) 0.035(7) O15 0.235(7) 0.286(9) 0.238(8) -0.138(7) 0.052(6) 0.087(7) O16A 0.141(11) 0.32(3) 0.20(2) -0.179(19) 0.009(13) -0.052(17) O16B 0.31(2) 0.079(7) 0.144(12) -0.016(6) 0.021(12) -0.082(9) O17A 0.192(15) 0.115(10) 0.154(12) -0.069(9) 0.115(12) -0.079(9) O17B 0.254(18) 0.125(8) 0.201(12) 0.109(9) 0.101(12) 0.034(10) N1 0.0425(14) 0.0441(15) 0.0452(16) -0.0018(12) 0.0069(12) 0.0029(11) N2 0.0448(15) 0.0496(16) 0.0427(15) -0.0003(12) 0.0047(12) -0.0029(12) N3 0.0653(18) 0.0438(15) 0.0406(15) 0.0005(12) 0.0055(13) -0.0035(13) N4 0.0448(14) 0.0438(15) 0.0416(15) -0.0008(11) 0.0063(12) -0.0016(11) N5 0.0464(15) 0.0559(17) 0.0388(15) -0.0049(12) 0.0077(12) -0.0070(12) N6 0.0487(15) 0.0497(16) 0.0461(16) -0.0040(13) 0.0131(13) -0.0033(12) N7 0.0536(16) 0.0548(17) 0.0384(15) 0.0012(12) 0.0096(12) -0.0050(13) N8 0.0495(16) 0.0461(16) 0.0464(16) 0.0035(12) 0.0060(13) 0.0012(12) C1 0.0484(19) 0.0509(19) 0.052(2) -0.0016(15) 0.0091(16) 0.0065(15) C2 0.046(2) 0.073(3) 0.077(3) -0.013(2) 0.0086(19) 0.0088(17) C3 0.061(2) 0.068(3) 0.097(3) -0.021(2) 0.021(2) 0.018(2) C4 0.070(3) 0.061(2) 0.072(3) -0.023(2) 0.014(2) 0.0081(19) C5 0.0501(18) 0.0422(18) 0.0504(19) -0.0038(15) 0.0064(15) 0.0020(14) C6 0.056(2) 0.0452(19) 0.056(2) -0.0101(16) 0.0052(17) -0.0031(15) C7 0.0417(17) 0.057(2) 0.0429(18) 0.0009(15) 0.0043(14) -0.0037(14) C8 0.060(2) 0.062(2) 0.059(2) -0.0051(18) 0.0072(18) -0.0110(17) C9 0.059(2) 0.085(3) 0.062(3) -0.005(2) -0.002(2) -0.022(2) C10 0.049(2) 0.127(4) 0.054(2) 0.003(3) -0.0056(19) -0.006(2) C11 0.056(2) 0.093(3) 0.058(2) 0.000(2) 0.0023(19) 0.014(2) C12 0.0474(19) 0.069(2) 0.0400(18) -0.0019(16) 0.0036(15) 0.0022(16) C13 0.069(3) 0.057(3) 0.098(3) -0.011(2) -0.020(3) 0.020(2) C14 0.080(3) 0.053(2) 0.059(2) 0.0131(18) -0.017(2) -0.0012(19) C15 0.076(2) 0.050(2) 0.052(2) 0.0113(17) 0.0072(19) -0.0135(17) C16 0.083(3) 0.0398(19) 0.063(2) 0.0060(17) -0.003(2) -0.0058(18) C17 0.0515(19) 0.0498(19) 0.0442(18) -0.0028(15) 0.0117(15) -0.0083(15) C18 0.066(2) 0.052(2) 0.062(2) -0.0114(18) 0.0198(19) -0.0081(17) C19 0.074(3) 0.071(3) 0.059(2) -0.024(2) 0.017(2) -0.024(2) C20 0.055(2) 0.089(3) 0.052(2) -0.012(2) 0.0035(18) -0.022(2) C21 0.051(2) 0.070(2) 0.052(2) -0.0073(18) 0.0076(17) -0.0073(17) C22 0.0468(18) 0.054(2) 0.0412(18) -0.0032(15) 0.0077(14) -0.0068(14) C23 0.0394(17) 0.062(2) 0.051(2) -0.0023(16) 0.0047(15) 0.0016(15) C24 0.0500(19) 0.062(2) 0.0457(19) -0.0095(17) 0.0139(16) -0.0152(16) C25 0.062(2) 0.085(3) 0.055(2) -0.019(2) 0.0091(19) -0.021(2) C26 0.064(3) 0.108(4) 0.052(2) -0.011(2) -0.002(2) -0.022(2) C27 0.056(2) 0.090(3) 0.053(2) 0.004(2) -0.0055(18) -0.007(2) C28 0.0445(18) 0.072(2) 0.0412(19) 0.0047(17) 0.0034(15) -0.0054(16) C29 0.051(2) 0.059(2) 0.055(2) 0.0066(17) 0.0076(17) 0.0057(16) C30 0.071(2) 0.0403(18) 0.050(2) 0.0048(15) 0.0096(18) 0.0076(16) C31 0.075(3) 0.062(2) 0.066(3) 0.010(2) 0.019(2) 0.019(2) C32 0.114(4) 0.060(3) 0.083(3) 0.007(2) 0.035(3) 0.033(3) C33 0.135(5) 0.051(2) 0.077(3) -0.013(2) 0.016(3) 0.002(3) C34 0.091(3) 0.052(2) 0.061(2) -0.0078(19) 0.014(2) -0.007(2) C35 0.071(2) 0.0402(18) 0.051(2) 0.0013(15) 0.0130(18) -0.0015(16) C36 0.073(2) 0.051(2) 0.073(3) 0.0028(19) 0.022(2) -0.0124(18) C37 0.074(3) 0.057(2) 0.057(2) 0.0144(18) 0.0171(19) -0.0030(18) C38 0.054(2) 0.067(2) 0.065(2) -0.0033(19) 0.0178(18) -0.0129(18) C39 0.056(2) 0.067(2) 0.066(2) 0.0001(19) 0.0252(19) -0.0010(18) C40 0.059(2) 0.060(2) 0.0448(19) -0.0018(16) 0.0131(16) 0.0093(17) C41 0.070(3) 0.089(3) 0.058(2) 0.000(2) 0.005(2) 0.019(2) C42 0.110(4) 0.091(4) 0.065(3) 0.010(3) 0.012(3) 0.037(3) C43 0.124(4) 0.057(3) 0.082(3) 0.012(2) 0.038(3) 0.022(3) C44 0.083(3) 0.061(3) 0.085(3) 0.003(2) 0.032(3) 0.008(2) C45 0.060(2) 0.050(2) 0.052(2) -0.0021(16) 0.0206(17) 0.0066(16) C46 0.057(2) 0.051(2) 0.057(2) -0.0145(17) 0.0178(18) -0.0084(16) Cl1 0.0930(8) 0.0590(6) 0.0548(6) 0.0020(4) 0.0179(5) -0.0018(5) Cl2 0.0626(7) 0.1238(11) 0.0837(8) 0.0172(8) 0.0036(6) 0.0163(7) Cl3 0.1055(9) 0.0655(7) 0.0622(6) -0.0056(5) 0.0188(6) 0.0019(6) C1S 0.226(9) 0.111(5) 0.135(7) 0.012(5) 0.021(6) -0.014(6) C2S 0.136(5) 0.098(5) 0.097(5) 0.016(4) -0.017(4) -0.010(4) N1S 0.152(5) 0.145(6) 0.115(5) -0.018(4) -0.009(4) -0.008(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 Zn1 O5 1.904(2) . ? Zn1 N3 2.066(3) . ? Zn1 N1 2.094(3) . ? Zn1 N2 2.248(3) . ? Zn1 N4 2.426(3) . ? Zn2 O5 1.910(2) . ? Zn2 N5 2.107(3) . ? Zn2 N7 2.108(3) . ? Zn2 N8 2.279(3) . ? Zn2 N6 2.323(3) . ? O1 C12 1.386(4) . ? O1 C13 1.453(5) . ? O2 C17 1.371(4) . ? O2 C16 1.447(4) . ? O3 C35 1.383(4) . ? O3 C36 1.426(4) . ? O4 C40 1.389(4) . ? O4 C39 1.449(4) . ? O6A Cl1 1.241(8) . ? O7A Cl1 1.488(6) . ? O7B Cl1 1.326(8) . ? O8A Cl1 1.412(10) . ? O8B Cl1 1.412(9) . ? O9 Cl1 1.373(4) . ? O10 Cl2 1.477(8) . ? O11A Cl2 1.424(14) . ? O11B Cl2 1.334(5) . ? O12A Cl2 1.362(18) . ? O12B Cl2 1.346(12) . ? O13 Cl2 1.397(5) . ? O14 Cl3 1.318(8) . ? O15 Cl3 1.313(5) . ? O16A Cl3 1.366(17) . ? O16B Cl3 1.346(12) . ? O17A Cl3 1.456(11) . ? O17B Cl3 1.279(9) . ? N1 C5 1.336(4) . ? N1 C1 1.334(4) . ? N2 C23 1.276(4) . ? N2 C22 1.419(4) . ? N3 C15 1.498(4) . ? N3 C14 1.502(5) . ? N4 C6 1.254(4) . ? N4 C7 1.421(4) . ? N5 C24 1.332(4) . ? N5 C28 1.345(5) . ? N6 C46 1.267(4) . ? N6 C45 1.418(4) . ? N7 C38 1.489(4) . ? N7 C37 1.492(5) . ? N8 C29 1.277(4) . ? N8 C30 1.415(4) . ? C1 C2 1.397(5) . ? C1 C23 1.471(5) . ? C2 C3 1.376(6) . ? C3 C4 1.373(6) . ? C4 C5 1.389(5) . ? C5 C6 1.471(5) . ? C7 C12 1.384(5) . ? C7 C8 1.405(5) . ? C8 C9 1.376(6) . ? C9 C10 1.378(6) . ? C10 C11 1.370(6) . ? C11 C12 1.391(5) . ? C13 C14 1.469(6) . ? C15 C16 1.501(5) . ? C17 C18 1.384(5) . ? C17 C22 1.396(5) . ? C18 C19 1.374(6) . ? C19 C20 1.382(6) . ? C20 C21 1.372(5) . ? C21 C22 1.399(5) . ? C24 C25 1.395(5) . ? C24 C46 1.463(5) . ? C25 C26 1.395(6) . ? C26 C27 1.369(6) . ? C27 C28 1.396(5) . ? C28 C29 1.463(5) . ? C30 C35 1.385(5) . ? C30 C31 1.388(5) . ? C31 C32 1.381(6) . ? C32 C33 1.393(7) . ? C33 C34 1.350(7) . ? C34 C35 1.379(5) . ? C36 C37 1.521(6) . ? C38 C39 1.487(6) . ? C40 C41 1.375(5) . ? C40 C45 1.386(5) . ? C41 C42 1.392(7) . ? C42 C43 1.375(7) . ? C43 C44 1.376(6) . ? C44 C45 1.403(5) . ? C1S C2S 1.478(10) . ? C2S N1S 1.112(8) . ? 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 O5 Zn1 N3 136.14(11) . . ? O5 Zn1 N1 121.73(10) . . ? N3 Zn1 N1 101.24(11) . . ? O5 Zn1 N2 97.98(10) . . ? N3 Zn1 N2 101.65(11) . . ? N1 Zn1 N2 74.77(10) . . ? O5 Zn1 N4 96.82(9) . . ? N3 Zn1 N4 87.73(10) . . ? N1 Zn1 N4 72.06(9) . . ? N2 Zn1 N4 146.69(9) . . ? O5 Zn2 N5 129.92(10) . . ? O5 Zn2 N7 128.95(10) . . ? N5 Zn2 N7 101.12(11) . . ? O5 Zn2 N8 97.81(10) . . ? N5 Zn2 N8 73.50(11) . . ? N7 Zn2 N8 97.60(10) . . ? O5 Zn2 N6 95.19(10) . . ? N5 Zn2 N6 72.37(11) . . ? N7 Zn2 N6 99.99(10) . . ? N8 Zn2 N6 143.95(10) . . ? C12 O1 C13 115.4(3) . . ? C17 O2 C16 114.9(3) . . ? C35 O3 C36 114.9(3) . . ? C40 O4 C39 113.3(3) . . ? Zn1 O5 Zn2 141.50(12) . . ? C5 N1 C1 119.9(3) . . ? C5 N1 Zn1 121.8(2) . . ? C1 N1 Zn1 118.2(2) . . ? C23 N2 C22 120.6(3) . . ? C23 N2 Zn1 113.6(2) . . ? C22 N2 Zn1 125.7(2) . . ? C15 N3 C14 112.8(3) . . ? C15 N3 Zn1 113.3(2) . . ? C14 N3 Zn1 117.4(2) . . ? C6 N4 C7 121.1(3) . . ? C6 N4 Zn1 110.7(2) . . ? C7 N4 Zn1 128.0(2) . . ? C24 N5 C28 120.8(3) . . ? C24 N5 Zn2 120.1(2) . . ? C28 N5 Zn2 118.8(2) . . ? C46 N6 C45 121.1(3) . . ? C46 N6 Zn2 113.9(2) . . ? C45 N6 Zn2 125.0(2) . . ? C38 N7 C37 110.4(3) . . ? C38 N7 Zn2 120.5(2) . . ? C37 N7 Zn2 112.2(2) . . ? C29 N8 C30 122.0(3) . . ? C29 N8 Zn2 113.9(2) . . ? C30 N8 Zn2 124.1(2) . . ? N1 C1 C2 121.6(3) . . ? N1 C1 C23 115.2(3) . . ? C2 C1 C23 123.2(3) . . ? C3 C2 C1 118.1(4) . . ? C2 C3 C4 120.3(4) . . ? C3 C4 C5 118.5(4) . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 115.2(3) . . ? C4 C5 C6 123.2(3) . . ? N4 C6 C5 120.2(3) . . ? C12 C7 C8 118.6(3) . . ? C12 C7 N4 117.5(3) . . ? C8 C7 N4 123.9(3) . . ? C9 C8 C7 120.4(4) . . ? C8 C9 C10 120.2(4) . . ? C11 C10 C9 120.3(4) . . ? C10 C11 C12 120.1(4) . . ? C7 C12 O1 119.0(3) . . ? C7 C12 C11 120.4(4) . . ? O1 C12 C11 120.4(3) . . ? O1 C13 C14 111.0(3) . . ? C13 C14 N3 115.0(3) . . ? N3 C15 C16 111.8(3) . . ? O2 C16 C15 110.5(3) . . ? O2 C17 C18 120.8(3) . . ? O2 C17 C22 119.4(3) . . ? C18 C17 C22 119.8(3) . . ? C19 C18 C17 120.6(4) . . ? C18 C19 C20 119.8(4) . . ? C21 C20 C19 120.5(4) . . ? C20 C21 C22 120.2(4) . . ? C17 C22 C21 119.0(3) . . ? C17 C22 N2 117.4(3) . . ? C21 C22 N2 123.5(3) . . ? N2 C23 C1 118.0(3) . . ? N5 C24 C25 120.8(4) . . ? N5 C24 C46 115.2(3) . . ? C25 C24 C46 124.0(4) . . ? C24 C25 C26 118.7(4) . . ? C27 C26 C25 119.8(4) . . ? C26 C27 C28 118.9(4) . . ? N5 C28 C27 120.9(4) . . ? N5 C28 C29 114.7(3) . . ? C27 C28 C29 124.2(4) . . ? N8 C29 C28 118.0(3) . . ? C35 C30 C31 119.2(4) . . ? C35 C30 N8 117.3(3) . . ? C31 C30 N8 123.4(4) . . ? C32 C31 C30 120.1(4) . . ? C31 C32 C33 119.0(4) . . ? C34 C33 C32 121.4(4) . . ? C33 C34 C35 119.5(4) . . ? C34 C35 O3 119.6(4) . . ? C34 C35 C30 120.7(4) . . ? O3 C35 C30 119.7(3) . . ? O3 C36 C37 112.0(3) . . ? N7 C37 C36 112.3(3) . . ? C39 C38 N7 112.1(3) . . ? O4 C39 C38 107.5(3) . . ? C41 C40 O4 119.4(4) . . ? C41 C40 C45 122.1(4) . . ? O4 C40 C45 118.5(3) . . ? C40 C41 C42 119.0(5) . . ? C43 C42 C41 119.7(4) . . ? C44 C43 C42 121.3(5) . . ? C43 C44 C45 119.7(5) . . ? C40 C45 C44 118.1(4) . . ? C40 C45 N6 117.9(3) . . ? C44 C45 N6 123.9(4) . . ? N6 C46 C24 117.7(3) . . ? O6A Cl1 O7B 47.5(11) . . ? O6A Cl1 O9 99.5(6) . . ? O7B Cl1 O9 115.2(5) . . ? O6A Cl1 O8B 93.3(7) . . ? O7B Cl1 O8B 106.5(6) . . ? O9 Cl1 O8B 133.3(5) . . ? O6A Cl1 O8A 119.7(9) . . ? O7B Cl1 O8A 139.3(6) . . ? O9 Cl1 O8A 104.7(5) . . ? O8B Cl1 O8A 33.6(4) . . ? O6A Cl1 O7A 130.6(11) . . ? O7B Cl1 O7A 83.1(7) . . ? O9 Cl1 O7A 100.4(4) . . ? O8B Cl1 O7A 104.6(4) . . ? O8A Cl1 O7A 97.9(5) . . ? O11B Cl2 O12B 109.9(8) . . ? O11B Cl2 O12A 126.8(14) . . ? O12B Cl2 O12A 25.8(17) . . ? O11B Cl2 O13 124.6(5) . . ? O12B Cl2 O13 115.9(7) . . ? O12A Cl2 O13 107.6(13) . . ? O11B Cl2 O11A 64.3(13) . . ? O12B Cl2 O11A 94.2(15) . . ? O12A Cl2 O11A 118.4(19) . . ? O13 Cl2 O11A 82.6(8) . . ? O11B Cl2 O10 91.9(5) . . ? O12B Cl2 O10 111.1(8) . . ? O12A Cl2 O10 89.5(13) . . ? O13 Cl2 O10 98.8(4) . . ? O11A Cl2 O10 150.5(18) . . ? O17B Cl3 O15 100.4(8) . . ? O17B Cl3 O14 135.3(13) . . ? O15 Cl3 O14 99.8(7) . . ? O17B Cl3 O16B 111.8(9) . . ? O15 Cl3 O16B 124.3(10) . . ? O14 Cl3 O16B 88.1(9) . . ? O17B Cl3 O16A 76.6(14) . . ? O15 Cl3 O16A 110.5(10) . . ? O14 Cl3 O16A 130.9(17) . . ? O16B Cl3 O16A 42.9(14) . . ? O17B Cl3 O17A 49.6(7) . . ? O15 Cl3 O17A 121.2(6) . . ? O14 Cl3 O17A 85.9(12) . . ? O16B Cl3 O17A 114.2(9) . . ? O16A Cl3 O17A 108.3(11) . . ? N1S C2S C1S 178.7(8) . . ? 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 N3 Zn1 O5 Zn2 -129.98(19) . . . . ? N1 Zn1 O5 Zn2 63.1(2) . . . . ? N2 Zn1 O5 Zn2 -13.9(2) . . . . ? N4 Zn1 O5 Zn2 136.19(19) . . . . ? N5 Zn2 O5 Zn1 26.4(3) . . . . ? N7 Zn2 O5 Zn1 -154.98(17) . . . . ? N8 Zn2 O5 Zn1 -48.6(2) . . . . ? N6 Zn2 O5 Zn1 97.7(2) . . . . ? O5 Zn1 N1 C5 90.1(3) . . . . ? N3 Zn1 N1 C5 -80.7(3) . . . . ? N2 Zn1 N1 C5 -179.8(3) . . . . ? N4 Zn1 N1 C5 3.2(2) . . . . ? O5 Zn1 N1 C1 -94.3(3) . . . . ? N3 Zn1 N1 C1 94.9(3) . . . . ? N2 Zn1 N1 C1 -4.3(2) . . . . ? N4 Zn1 N1 C1 178.7(3) . . . . ? O5 Zn1 N2 C23 125.1(2) . . . . ? N3 Zn1 N2 C23 -94.3(3) . . . . ? N1 Zn1 N2 C23 4.3(2) . . . . ? N4 Zn1 N2 C23 9.6(3) . . . . ? O5 Zn1 N2 C22 -59.0(3) . . . . ? N3 Zn1 N2 C22 81.5(3) . . . . ? N1 Zn1 N2 C22 -179.9(3) . . . . ? N4 Zn1 N2 C22 -174.6(2) . . . . ? O5 Zn1 N3 C15 94.8(3) . . . . ? N1 Zn1 N3 C15 -96.5(2) . . . . ? N2 Zn1 N3 C15 -20.0(3) . . . . ? N4 Zn1 N3 C15 -167.7(2) . . . . ? O5 Zn1 N3 C14 -39.6(3) . . . . ? N1 Zn1 N3 C14 129.1(3) . . . . ? N2 Zn1 N3 C14 -154.4(2) . . . . ? N4 Zn1 N3 C14 57.9(3) . . . . ? O5 Zn1 N4 C6 -123.8(2) . . . . ? N3 Zn1 N4 C6 100.0(2) . . . . ? N1 Zn1 N4 C6 -2.6(2) . . . . ? N2 Zn1 N4 C6 -7.9(3) . . . . ? O5 Zn1 N4 C7 62.1(3) . . . . ? N3 Zn1 N4 C7 -74.1(3) . . . . ? N1 Zn1 N4 C7 -176.7(3) . . . . ? N2 Zn1 N4 C7 178.0(2) . . . . ? O5 Zn2 N5 C24 89.7(3) . . . . ? N7 Zn2 N5 C24 -89.1(3) . . . . ? N8 Zn2 N5 C24 176.1(3) . . . . ? N6 Zn2 N5 C24 7.9(2) . . . . ? O5 Zn2 N5 C28 -96.0(3) . . . . ? N7 Zn2 N5 C28 85.1(3) . . . . ? N8 Zn2 N5 C28 -9.6(2) . . . . ? N6 Zn2 N5 C28 -177.8(3) . . . . ? O5 Zn2 N6 C46 -135.7(2) . . . . ? N5 Zn2 N6 C46 -5.4(2) . . . . ? N7 Zn2 N6 C46 93.2(2) . . . . ? N8 Zn2 N6 C46 -24.8(3) . . . . ? O5 Zn2 N6 C45 42.5(3) . . . . ? N5 Zn2 N6 C45 172.8(3) . . . . ? N7 Zn2 N6 C45 -88.6(3) . . . . ? N8 Zn2 N6 C45 153.3(2) . . . . ? O5 Zn2 N7 C38 -40.3(3) . . . . ? N5 Zn2 N7 C38 138.6(3) . . . . ? N8 Zn2 N7 C38 -146.8(3) . . . . ? N6 Zn2 N7 C38 64.8(3) . . . . ? O5 Zn2 N7 C37 92.3(3) . . . . ? N5 Zn2 N7 C37 -88.8(2) . . . . ? N8 Zn2 N7 C37 -14.2(2) . . . . ? N6 Zn2 N7 C37 -162.6(2) . . . . ? O5 Zn2 N8 C29 136.9(2) . . . . ? N5 Zn2 N8 C29 7.5(2) . . . . ? N7 Zn2 N8 C29 -92.0(3) . . . . ? N6 Zn2 N8 C29 26.8(3) . . . . ? O5 Zn2 N8 C30 -42.3(3) . . . . ? N5 Zn2 N8 C30 -171.8(3) . . . . ? N7 Zn2 N8 C30 88.8(3) . . . . ? N6 Zn2 N8 C30 -152.4(2) . . . . ? C5 N1 C1 C2 0.6(5) . . . . ? Zn1 N1 C1 C2 -175.0(3) . . . . ? C5 N1 C1 C23 179.4(3) . . . . ? Zn1 N1 C1 C23 3.8(4) . . . . ? N1 C1 C2 C3 -0.9(6) . . . . ? C23 C1 C2 C3 -179.6(4) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? C1 N1 C5 C4 0.0(5) . . . . ? Zn1 N1 C5 C4 175.5(3) . . . . ? C1 N1 C5 C6 -178.9(3) . . . . ? Zn1 N1 C5 C6 -3.4(4) . . . . ? C3 C4 C5 N1 -0.4(6) . . . . ? C3 C4 C5 C6 178.5(4) . . . . ? C7 N4 C6 C5 176.4(3) . . . . ? Zn1 N4 C6 C5 1.9(4) . . . . ? N1 C5 C6 N4 0.6(5) . . . . ? C4 C5 C6 N4 -178.3(4) . . . . ? C6 N4 C7 C12 -167.9(3) . . . . ? Zn1 N4 C7 C12 5.6(4) . . . . ? C6 N4 C7 C8 10.7(5) . . . . ? Zn1 N4 C7 C8 -175.8(3) . . . . ? C12 C7 C8 C9 1.6(6) . . . . ? N4 C7 C8 C9 -177.0(3) . . . . ? C7 C8 C9 C10 0.4(6) . . . . ? C8 C9 C10 C11 -1.3(7) . . . . ? C9 C10 C11 C12 0.2(7) . . . . ? C8 C7 C12 O1 173.1(3) . . . . ? N4 C7 C12 O1 -8.2(5) . . . . ? C8 C7 C12 C11 -2.7(5) . . . . ? N4 C7 C12 C11 175.9(3) . . . . ? C13 O1 C12 C7 112.0(4) . . . . ? C13 O1 C12 C11 -72.1(4) . . . . ? C10 C11 C12 C7 1.9(6) . . . . ? C10 C11 C12 O1 -173.9(4) . . . . ? C12 O1 C13 C14 -67.7(4) . . . . ? O1 C13 C14 N3 -65.5(4) . . . . ? C15 N3 C14 C13 -99.8(4) . . . . ? Zn1 N3 C14 C13 34.8(4) . . . . ? C14 N3 C15 C16 69.1(4) . . . . ? Zn1 N3 C15 C16 -67.4(3) . . . . ? C17 O2 C16 C15 97.1(4) . . . . ? N3 C15 C16 O2 54.1(4) . . . . ? C16 O2 C17 C18 79.1(4) . . . . ? C16 O2 C17 C22 -102.3(4) . . . . ? O2 C17 C18 C19 175.7(3) . . . . ? C22 C17 C18 C19 -2.9(5) . . . . ? C17 C18 C19 C20 0.8(6) . . . . ? C18 C19 C20 C21 0.8(6) . . . . ? C19 C20 C21 C22 -0.2(6) . . . . ? O2 C17 C22 C21 -175.2(3) . . . . ? C18 C17 C22 C21 3.4(5) . . . . ? O2 C17 C22 N2 3.5(4) . . . . ? C18 C17 C22 N2 -177.9(3) . . . . ? C20 C21 C22 C17 -1.9(5) . . . . ? C20 C21 C22 N2 179.5(3) . . . . ? C23 N2 C22 C17 151.6(3) . . . . ? Zn1 N2 C22 C17 -23.9(4) . . . . ? C23 N2 C22 C21 -29.8(5) . . . . ? Zn1 N2 C22 C21 154.7(3) . . . . ? C22 N2 C23 C1 -179.9(3) . . . . ? Zn1 N2 C23 C1 -3.9(4) . . . . ? N1 C1 C23 N2 0.3(5) . . . . ? C2 C1 C23 N2 179.1(4) . . . . ? C28 N5 C24 C25 -0.7(5) . . . . ? Zn2 N5 C24 C25 173.4(3) . . . . ? C28 N5 C24 C46 176.5(3) . . . . ? Zn2 N5 C24 C46 -9.4(4) . . . . ? N5 C24 C25 C26 -0.6(6) . . . . ? C46 C24 C25 C26 -177.5(4) . . . . ? C24 C25 C26 C27 2.4(6) . . . . ? C25 C26 C27 C28 -2.8(6) . . . . ? C24 N5 C28 C27 0.2(5) . . . . ? Zn2 N5 C28 C27 -174.0(3) . . . . ? C24 N5 C28 C29 -175.2(3) . . . . ? Zn2 N5 C28 C29 10.6(4) . . . . ? C26 C27 C28 N5 1.5(6) . . . . ? C26 C27 C28 C29 176.5(4) . . . . ? C30 N8 C29 C28 174.6(3) . . . . ? Zn2 N8 C29 C28 -4.6(4) . . . . ? N5 C28 C29 N8 -3.4(5) . . . . ? C27 C28 C29 N8 -178.6(4) . . . . ? C29 N8 C30 C35 152.3(3) . . . . ? Zn2 N8 C30 C35 -28.6(4) . . . . ? C29 N8 C30 C31 -31.3(5) . . . . ? Zn2 N8 C30 C31 147.9(3) . . . . ? C35 C30 C31 C32 0.7(6) . . . . ? N8 C30 C31 C32 -175.6(4) . . . . ? C30 C31 C32 C33 1.1(7) . . . . ? C31 C32 C33 C34 -1.1(7) . . . . ? C32 C33 C34 C35 -0.7(7) . . . . ? C33 C34 C35 O3 -178.6(4) . . . . ? C33 C34 C35 C30 2.6(6) . . . . ? C36 O3 C35 C34 93.7(4) . . . . ? C36 O3 C35 C30 -87.6(4) . . . . ? C31 C30 C35 C34 -2.6(5) . . . . ? N8 C30 C35 C34 173.9(3) . . . . ? C31 C30 C35 O3 178.6(3) . . . . ? N8 C30 C35 O3 -4.8(5) . . . . ? C35 O3 C36 C37 103.3(4) . . . . ? C38 N7 C37 C36 67.7(4) . . . . ? Zn2 N7 C37 C36 -69.6(3) . . . . ? O3 C36 C37 N7 46.7(4) . . . . ? C37 N7 C38 C39 -178.7(3) . . . . ? Zn2 N7 C38 C39 -45.4(4) . . . . ? C40 O4 C39 C38 -160.2(3) . . . . ? N7 C38 C39 O4 68.7(4) . . . . ? C39 O4 C40 C41 -95.8(4) . . . . ? C39 O4 C40 C45 83.5(4) . . . . ? O4 C40 C41 C42 -178.1(4) . . . . ? C45 C40 C41 C42 2.6(6) . . . . ? C40 C41 C42 C43 0.5(7) . . . . ? C41 C42 C43 C44 -2.1(7) . . . . ? C42 C43 C44 C45 0.5(7) . . . . ? C41 C40 C45 C44 -4.2(5) . . . . ? O4 C40 C45 C44 176.6(3) . . . . ? C41 C40 C45 N6 179.7(3) . . . . ? O4 C40 C45 N6 0.4(5) . . . . ? C43 C44 C45 C40 2.6(6) . . . . ? C43 C44 C45 N6 178.5(4) . . . . ? C46 N6 C45 C40 -151.4(3) . . . . ? Zn2 N6 C45 C40 30.5(4) . . . . ? C46 N6 C45 C44 32.7(5) . . . . ? Zn2 N6 C45 C44 -145.4(3) . . . . ? C45 N6 C46 C24 -175.7(3) . . . . ? Zn2 N6 C46 C24 2.6(4) . . . . ? N5 C24 C46 N6 3.9(5) . . . . ? C25 C24 C46 N6 -179.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.694 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.105